# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 207/381 data_global # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Martina Walker EMBL Hamburg c/o DESY Building 25A Notkestrasse 85 D-22603 Hamburg Germany ; _publ_contact_author_phone '049 40 89902193' _publ_contact_author_fax '049 40 89902149' _publ_contact_author_email Mwalker@embl-hamburg.de _publ_requested_journal 'J. Chem. Soc.,Perkin Trans. I' _publ_section_title ; 'Structure and Biosynthesis of Kendomycin, a new Carbocyclic ansa-Compound from Streptomyces' ; #=========================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=========================================================================== # 3. TITLE AND AUTHOR LIST loop_ _publ_author_name _publ_author_address 'Bode, Helge B.' ; Institut f\"ur Organische Chemie Universit\"at G\"ottingen Tammannstr. 2 D-37077 G\"ottingen Germany ; 'Zeeck, Axel' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 2 D-37077 G\"ottingen Germany ; #============================================================================== data_makro _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Kendomycin _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H42 O6' _chemical_formula_weight 486.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_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' _cell_length_a 10.032(2) _cell_length_b 10.900(2) _cell_length_c 24.779(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2709.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type 'semi empirical' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; 'Intensities were measured with a Bruker CCD area detector' ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe-Siemens-Huber four circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6219 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6219 _reflns_number_gt 4797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.050 (Bruker, 1997-98)' _computing_cell_refinement 'SAINT 5.00 (Bruker, 1997)' _computing_data_reduction 'SAINT 5.00 (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Sheldrick,1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.0167P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.2(11) _refine_ls_number_reflns 6219 _refine_ls_number_parameters 332 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.541 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O5 O 0.57524(18) 0.38044(15) 0.07010(7) 0.0219(4) Uani 1 1 d . . . O3 O 0.65564(18) 0.71425(16) -0.11106(7) 0.0256(4) Uani 1 1 d . . . O1 O 0.91904(18) 0.68960(15) 0.04720(7) 0.0226(4) Uani 1 1 d . . . O19 O 1.03999(17) 0.55653(16) 0.10167(7) 0.0232(4) Uani 1 1 d D . . H19 H 1.095(3) 0.612(2) 0.1089(12) 0.035 Uiso 1 1 d D . . O4 O 0.5237(2) 0.51976(18) -0.08359(7) 0.0293(5) Uani 1 1 d D . . H4 H 0.525(3) 0.572(3) -0.1087(11) 0.044 Uiso 1 1 d D . . C4A C 0.6547(3) 0.4895(2) -0.00543(10) 0.0208(6) Uani 1 1 d . . . C6 C 0.6369(3) 0.2556(2) -0.00884(10) 0.0228(6) Uani 1 1 d . . . H6 H 0.7334 0.2525 0.0011 0.027 Uiso 1 1 calc RD . . C5 C 0.5778(3) 0.3773(2) 0.01235(10) 0.0202(6) Uani 1 1 d . . . H5 H 0.4842 0.3847 -0.0012 0.024 Uiso 1 1 calc R . . C3 C 0.6946(3) 0.6671(2) -0.06776(11) 0.0229(6) Uani 1 1 d . . . C20A C 0.7612(3) 0.5406(2) 0.02735(11) 0.0208(6) Uani 1 1 d . . . O7 O 0.6286(2) 0.03488(17) 0.00408(8) 0.0359(5) Uani 1 1 d D . . H7 H 0.604(4) 0.013(3) -0.0259(15) 0.054 Uiso 1 1 d . . . C7 C 0.5666(3) 0.1486(2) 0.01801(11) 0.0250(6) Uani 1 1 d . . . H7A H 0.4723 0.1466 0.0050 0.030 Uiso 1 1 calc R . . C2 C 0.8001(3) 0.7174(2) -0.03517(10) 0.0220(6) Uani 1 1 d . . . C4 C 0.6250(3) 0.5534(2) -0.05031(10) 0.0222(6) Uani 1 1 d . . . C27 C 0.7368(3) 0.7533(3) 0.12977(12) 0.0333(7) Uani 1 1 d . . . H27A H 0.7527 0.8019 0.0972 0.050 Uiso 1 1 calc R . . H27B H 0.7166 0.8082 0.1600 0.050 Uiso 1 1 calc R . . H27C H 0.6613 0.6979 0.1237 0.050 Uiso 1 1 calc R . . C22 C 0.6255(3) 0.2496(2) -0.07031(11) 0.0287(6) Uani 1 1 d . . . H22A H 0.6600 0.1706 -0.0831 0.043 Uiso 1 1 calc R . . H22B H 0.6775 0.3164 -0.0864 0.043 Uiso 1 1 calc R . . H22C H 0.5318 0.2578 -0.0809 0.043 Uiso 1 1 calc R . . C20 C 0.8168(3) 0.5087(2) 0.07475(10) 0.0212(6) Uani 1 1 d . . . H20 H 0.7983 0.4348 0.0937 0.025 Uiso 1 1 calc R . . C21 C 0.8716(3) 0.8324(2) -0.05143(12) 0.0321(7) Uani 1 1 d . . . H21A H 0.8258 0.9036 -0.0360 0.048 Uiso 1 1 calc R . . H21B H 0.8721 0.8391 -0.0909 0.048 Uiso 1 1 calc R . . H21C H 0.9635 0.8296 -0.0381 0.048 Uiso 1 1 calc R . . C18 C 0.8615(3) 0.6778(2) 0.14296(10) 0.0227(6) Uani 1 1 d . . . H18 H 0.9335 0.7364 0.1538 0.027 Uiso 1 1 calc R . . C1 C 0.8269(3) 0.6544(2) 0.01037(10) 0.0204(6) Uani 1 1 d . . . C19 C 0.9116(3) 0.6054(2) 0.09352(10) 0.0212(6) Uani 1 1 d . . . C8 C 0.5654(3) 0.1587(2) 0.07959(11) 0.0295(6) Uani 1 1 d . . . H8 H 0.5069 0.0919 0.0938 0.035 Uiso 1 1 calc R . . C17 C 0.8383(3) 0.5895(2) 0.19041(11) 0.0258(6) Uani 1 1 d . . . H17A H 0.9205 0.5407 0.1959 0.031 Uiso 1 1 calc R . . H17B H 0.7664 0.5317 0.1803 0.031 Uiso 1 1 calc R . . C13 C 0.5320(3) 0.5242(3) 0.23690(11) 0.0264(6) Uani 1 1 d . . . H13 H 0.5570 0.5930 0.2156 0.032 Uiso 1 1 calc R . . C10 C 0.4913(3) 0.3107(2) 0.15378(11) 0.0272(6) Uani 1 1 d . . . H10A H 0.5816 0.3292 0.1677 0.033 Uiso 1 1 calc R . . H10B H 0.4573 0.2379 0.1733 0.033 Uiso 1 1 calc R . . C14 C 0.6188(3) 0.4916(2) 0.27499(11) 0.0260(6) Uani 1 1 d . . . C9 C 0.5001(3) 0.2815(2) 0.09378(10) 0.0242(6) Uani 1 1 d . . . H9 H 0.4081 0.2827 0.0783 0.029 Uiso 1 1 calc R . . C11 C 0.3997(3) 0.4198(3) 0.16470(11) 0.0283(6) Uani 1 1 d . . . H11A H 0.3074 0.3961 0.1550 0.034 Uiso 1 1 calc R . . H11B H 0.4261 0.4880 0.1406 0.034 Uiso 1 1 calc R . . C16 C 0.8008(3) 0.6504(3) 0.24442(11) 0.0284(6) Uani 1 1 d . . . H16 H 0.7269 0.7100 0.2378 0.034 Uiso 1 1 calc R . . C12 C 0.3997(3) 0.4670(3) 0.22295(11) 0.0281(6) Uani 1 1 d . . . H12A H 0.3848 0.3957 0.2476 0.034 Uiso 1 1 calc R . . C15 C 0.7522(3) 0.5534(3) 0.28492(11) 0.0306(7) Uani 1 1 d . . . H15A H 0.8209 0.4883 0.2868 0.037 Uiso 1 1 calc R . . H15B H 0.7484 0.5926 0.3209 0.037 Uiso 1 1 calc R . . C23 C 0.7044(3) 0.1417(3) 0.10442(12) 0.0402(8) Uani 1 1 d . . . H23A H 0.7597 0.2133 0.0961 0.060 Uiso 1 1 calc R . . H23B H 0.7459 0.0678 0.0894 0.060 Uiso 1 1 calc R . . H23C H 0.6962 0.1331 0.1436 0.060 Uiso 1 1 calc R . . C26 C 0.9199(3) 0.7201(3) 0.26853(13) 0.0466(9) Uani 1 1 d . . . H26A H 0.8922 0.7614 0.3018 0.070 Uiso 1 1 calc R . . H26B H 0.9517 0.7812 0.2425 0.070 Uiso 1 1 calc R . . H26C H 0.9919 0.6621 0.2766 0.070 Uiso 1 1 calc R . . C24 C 0.2845(3) 0.5576(3) 0.23045(14) 0.0441(8) Uani 1 1 d . . . H24A H 0.2840 0.5876 0.2677 0.066 Uiso 1 1 calc R . . H24B H 0.1999 0.5163 0.2227 0.066 Uiso 1 1 calc R . . H24C H 0.2959 0.6270 0.2057 0.066 Uiso 1 1 calc R . . C25 C 0.5918(4) 0.3885(3) 0.31413(14) 0.0455(9) Uani 1 1 d . . . H25A H 0.5786 0.4224 0.3504 0.068 Uiso 1 1 calc R . . H25B H 0.6679 0.3322 0.3145 0.068 Uiso 1 1 calc R . . H25C H 0.5115 0.3441 0.3029 0.068 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 O5 0.0256(10) 0.0208(9) 0.0191(9) -0.0014(7) 0.0025(8) -0.0051(8) O3 0.0258(10) 0.0287(10) 0.0222(10) 0.0043(8) 0.0012(8) 0.0043(8) O1 0.0242(9) 0.0224(9) 0.0210(10) 0.0004(8) -0.0014(8) -0.0062(8) O19 0.0207(10) 0.0222(10) 0.0267(10) -0.0029(8) -0.0008(8) -0.0004(8) O4 0.0292(11) 0.0315(11) 0.0273(11) 0.0045(9) -0.0091(9) -0.0041(9) C4A 0.0202(13) 0.0192(12) 0.0231(14) -0.0024(11) 0.0034(11) 0.0017(11) C6 0.0201(13) 0.0236(13) 0.0246(14) -0.0051(11) -0.0011(11) -0.0012(11) C5 0.0194(13) 0.0226(13) 0.0187(13) -0.0025(11) -0.0007(11) -0.0027(11) C3 0.0225(14) 0.0242(13) 0.0220(15) -0.0013(11) 0.0058(12) 0.0058(11) C20A 0.0186(13) 0.0196(13) 0.0244(14) -0.0017(11) 0.0048(11) 0.0006(11) O7 0.0520(14) 0.0222(10) 0.0335(12) -0.0086(9) -0.0045(11) 0.0052(10) C7 0.0280(15) 0.0202(13) 0.0267(15) -0.0049(11) -0.0014(12) -0.0020(12) C2 0.0221(14) 0.0217(13) 0.0223(15) 0.0003(11) 0.0027(11) 0.0014(11) C4 0.0210(13) 0.0257(13) 0.0198(13) -0.0048(11) 0.0007(11) 0.0010(11) C27 0.0351(17) 0.0355(16) 0.0293(16) -0.0006(14) 0.0044(13) 0.0106(14) C22 0.0318(16) 0.0297(15) 0.0248(15) -0.0054(13) 0.0022(12) -0.0017(13) C20 0.0220(14) 0.0198(12) 0.0219(14) -0.0011(11) 0.0015(11) -0.0015(11) C21 0.0308(16) 0.0289(15) 0.0367(17) 0.0081(13) -0.0010(13) -0.0062(13) C18 0.0211(14) 0.0228(13) 0.0242(14) -0.0050(11) 0.0006(11) -0.0014(11) C1 0.0185(13) 0.0200(13) 0.0226(14) -0.0039(11) 0.0023(11) 0.0017(11) C19 0.0216(13) 0.0191(12) 0.0230(14) 0.0027(11) -0.0001(11) -0.0007(11) C8 0.0372(16) 0.0206(13) 0.0306(16) 0.0008(12) 0.0009(14) -0.0048(12) C17 0.0267(15) 0.0265(14) 0.0242(15) -0.0038(11) 0.0029(12) -0.0020(12) C13 0.0314(16) 0.0273(14) 0.0206(15) 0.0005(12) 0.0038(12) -0.0024(12) C10 0.0315(15) 0.0270(14) 0.0230(15) 0.0027(12) 0.0030(12) -0.0045(12) C14 0.0281(15) 0.0289(14) 0.0211(14) -0.0013(12) 0.0032(12) 0.0023(12) C9 0.0239(14) 0.0253(14) 0.0233(14) 0.0000(11) 0.0044(11) -0.0065(12) C11 0.0265(15) 0.0345(15) 0.0238(15) -0.0022(12) 0.0012(12) -0.0014(12) C16 0.0284(15) 0.0322(15) 0.0246(15) -0.0056(12) 0.0021(12) -0.0031(13) C12 0.0271(15) 0.0354(16) 0.0218(14) -0.0007(12) 0.0026(12) -0.0041(13) C15 0.0310(16) 0.0401(17) 0.0207(15) -0.0027(13) -0.0004(13) 0.0008(14) C23 0.058(2) 0.0323(16) 0.0302(18) 0.0005(14) -0.0064(16) 0.0151(16) C26 0.047(2) 0.059(2) 0.0328(18) -0.0157(16) 0.0025(16) -0.0190(18) C24 0.0313(17) 0.059(2) 0.042(2) -0.0171(17) 0.0058(15) 0.0024(16) C25 0.044(2) 0.047(2) 0.046(2) 0.0180(16) -0.0058(16) -0.0001(17) _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 O5 C5 1.432(3) . ? O5 C9 1.440(3) . ? O3 C3 1.252(3) . ? O1 C1 1.355(3) . ? O1 C19 1.471(3) . ? O19 C19 1.408(3) . ? O4 C4 1.359(3) . ? C4A C4 1.346(4) . ? C4A C20A 1.453(4) . ? C4A C5 1.512(3) . ? C6 C7 1.516(4) . ? C6 C22 1.529(4) . ? C6 C5 1.545(4) . ? C3 C2 1.439(4) . ? C3 C4 1.488(4) . ? C20A C20 1.346(4) . ? C20A C1 1.466(4) . ? O7 C7 1.429(3) . ? C7 C8 1.530(4) . ? C2 C1 1.348(4) . ? C2 C21 1.499(4) . ? C27 C18 1.532(4) . ? C20 C19 1.494(4) . ? C18 C17 1.537(4) . ? C18 C19 1.541(4) . ? C8 C9 1.532(4) . ? C8 C23 1.535(4) . ? C17 C16 1.541(4) . ? C13 C14 1.332(4) . ? C13 C12 1.506(4) . ? C10 C9 1.523(4) . ? C10 C11 1.528(4) . ? C14 C25 1.508(4) . ? C14 C15 1.518(4) . ? C11 C12 1.532(4) . ? C16 C26 1.537(4) . ? C16 C15 1.537(4) . ? C12 C24 1.532(4) . ? 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 C5 O5 C9 113.49(18) . . ? C1 O1 C19 108.31(19) . . ? C4 C4A C20A 115.2(2) . . ? C4 C4A C5 123.1(2) . . ? C20A C4A C5 121.5(2) . . ? C7 C6 C22 111.7(2) . . ? C7 C6 C5 109.4(2) . . ? C22 C6 C5 110.3(2) . . ? O5 C5 C4A 106.3(2) . . ? O5 C5 C6 111.6(2) . . ? C4A C5 C6 113.6(2) . . ? O3 C3 C2 123.7(2) . . ? O3 C3 C4 116.4(2) . . ? C2 C3 C4 120.0(2) . . ? C20 C20A C4A 133.9(2) . . ? C20 C20A C1 106.4(2) . . ? C4A C20A C1 119.6(2) . . ? O7 C7 C6 111.0(2) . . ? O7 C7 C8 107.9(2) . . ? C6 C7 C8 112.7(2) . . ? C1 C2 C3 115.0(2) . . ? C1 C2 C21 123.8(2) . . ? C3 C2 C21 121.2(2) . . ? C4A C4 O4 121.9(2) . . ? C4A C4 C3 124.6(2) . . ? O4 C4 C3 113.6(2) . . ? C20A C20 C19 110.7(2) . . ? C27 C18 C17 112.1(2) . . ? C27 C18 C19 111.8(2) . . ? C17 C18 C19 109.7(2) . . ? C2 C1 O1 123.7(2) . . ? C2 C1 C20A 125.6(2) . . ? O1 C1 C20A 110.7(2) . . ? O19 C19 O1 107.6(2) . . ? O19 C19 C20 111.1(2) . . ? O1 C19 C20 103.27(19) . . ? O19 C19 C18 112.2(2) . . ? O1 C19 C18 108.49(19) . . ? C20 C19 C18 113.6(2) . . ? C7 C8 C9 107.2(2) . . ? C7 C8 C23 112.6(2) . . ? C9 C8 C23 113.7(2) . . ? C18 C17 C16 115.6(2) . . ? C14 C13 C12 128.9(3) . . ? C9 C10 C11 111.7(2) . . ? C13 C14 C25 122.5(3) . . ? C13 C14 C15 124.9(3) . . ? C25 C14 C15 112.6(2) . . ? O5 C9 C10 105.8(2) . . ? O5 C9 C8 109.7(2) . . ? C10 C9 C8 115.6(2) . . ? C10 C11 C12 115.3(2) . . ? C26 C16 C15 109.5(2) . . ? C26 C16 C17 111.2(2) . . ? C15 C16 C17 110.4(2) . . ? C13 C12 C24 111.7(2) . . ? C13 C12 C11 110.8(2) . . ? C24 C12 C11 109.3(2) . . ? C14 C15 C16 118.6(2) . . ? _diffrn_measured_fraction_theta_max .997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full .997 _refine_diff_density_max .160 _refine_diff_density_min -.203 _refine_diff_density_rms .043