data_publication_text _publ_contact_author_name 'Stuart Krasnoff' _publ_contact_author_address ;USDA-ARS Biological IPM Research Unit Robt. W. Holley Ctr. for Ag. and Health Tower Rd. Ithaca, NY 14853 ; _publ_contact_author_email sbk1@cornell.edu _publ_contact_author_phone '(607) 255-2026' loop_ _publ_author_name _publ_author_address 'Krasnoff, Stuart B.' ;USDA-ARS Biological IPM Research Unit Robert Holley Center for Agriculture and Health Tower Rd. Ithaca, NY 14853 ; 'Englich, Ulrich' ;Cornell High Energy Synchrotron Source Cornell University 200L Wilson Lab Rt. 366 & Pine Tree Road Ithaca, New York 14853 ; 'Miller, Paula G.' ;Department of Biomedical Engineering Cornell University Ithaca NY 14853 ; 'Shuler, Michael L.' ;Department of Biomedical Engineering Cornell University Ithaca NY 14853 ; 'Glahn, Raymond P.' ;USDA-ARS Robert Holley Center for Agriculture and Health Tower Rd. Ithaca, NY 14853 ; 'Donzelli, Bruno G. G.' ;Dept. of Plant Pathology and Plant-Microbe Biology Cornell University Ithaca, NY 14853 ; 'Gibson, Donna M.' ;USDA-ARS Robert Holley Center for Agriculture and Health Tower Rd. Ithaca, NY 14853 ; data_MetaA_45_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Metacridamide A' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H55 N O6' _chemical_formula_weight 609.82 _chemical_absolute_configuration rm 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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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 12.480(3) _cell_length_b 13.140(3) _cell_length_c 21.920(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3594.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'thin plate' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9925 _exptl_absorpt_correction_T_max 0.9996 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.91770 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'CHESS F1' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ADSC Q270 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15222 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 30.64 _reflns_number_total 4991 _reflns_number_gt 4692 _reflns_threshold_expression >2sigma(I) _computing_data_collection ADX _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _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^)+(0.0716P)^2^+1.6966P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.034(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(12) _refine_ls_number_reflns 4991 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 O1 O 0.12864(15) 0.83560(13) 0.84854(9) 0.0324(5) Uani 1 1 d . . . C2 C 0.1009(2) 0.7633(2) 0.80873(14) 0.0329(7) Uani 1 1 d . . . O2 O 0.04122(18) 0.77443(16) 0.76694(11) 0.0474(6) Uani 1 1 d . . . C3 C 0.1581(2) 0.6651(2) 0.82632(13) 0.0305(6) Uani 1 1 d . . . H3A H 0.2336 0.6825 0.8330 0.037 Uiso 1 1 calc R . . C25 C 0.1551(2) 0.5866(2) 0.77460(14) 0.0362(7) Uani 1 1 d . . . H25A H 0.1729 0.5198 0.7905 0.043 Uiso 1 1 calc R . . H25B H 0.0836 0.5836 0.7574 0.043 Uiso 1 1 calc R . . C26 C 0.2349(2) 0.6165(2) 0.72556(13) 0.0339(7) Uani 1 1 d . . . C27 C 0.2044(2) 0.6693(2) 0.67407(14) 0.0377(7) Uani 1 1 d . . . H27A H 0.1321 0.6812 0.6668 0.045 Uiso 1 1 calc R . . C28 C 0.2795(3) 0.7045(2) 0.63321(15) 0.0445(8) Uani 1 1 d . . . H28A H 0.2575 0.7403 0.5988 0.053 Uiso 1 1 calc R . . C29 C 0.3867(3) 0.6872(3) 0.64290(16) 0.0483(8) Uani 1 1 d . . . H29A H 0.4372 0.7115 0.6154 0.058 Uiso 1 1 calc R . . C28' C 0.4188(3) 0.6332(3) 0.69402(16) 0.0530(9) Uani 1 1 d . . . H28B H 0.4912 0.6203 0.7007 0.064 Uiso 1 1 calc R . . C27' C 0.3427(3) 0.5986(3) 0.73504(15) 0.0460(8) Uani 1 1 d . . . H27B H 0.3645 0.5628 0.7695 0.055 Uiso 1 1 calc R . . N4 N 0.11705(18) 0.62681(16) 0.88391(11) 0.0301(5) Uani 1 1 d . . . H4A H 0.0491 0.6246 0.8904 0.036 Uiso 1 1 calc R . . C5 C 0.1861(2) 0.59465(19) 0.92725(14) 0.0323(7) Uani 1 1 d . . . O3 O 0.28349(15) 0.59324(15) 0.91900(10) 0.0381(5) Uani 1 1 d . . . C6 C 0.1395(2) 0.5595(2) 0.98665(13) 0.0318(6) Uani 1 1 d . . . C30 C 0.1973(3) 0.4716(2) 1.01576(16) 0.0446(8) Uani 1 1 d . . . H30A H 0.1627 0.4540 1.0534 0.067 Uiso 1 1 calc R . . H30B H 0.2703 0.4905 1.0237 0.067 Uiso 1 1 calc R . . H30C H 0.1959 0.4141 0.9887 0.067 Uiso 1 1 calc R . . C7 C 0.0570(2) 0.6070(2) 1.01220(14) 0.0352(7) Uani 1 1 d . . . H7A H 0.0289 0.6627 0.9915 0.042 Uiso 1 1 calc R . . C8 C 0.0050(2) 0.5783(2) 1.07167(14) 0.0353(7) Uani 1 1 d . . . H8A H 0.0612 0.5518 1.0986 0.042 Uiso 1 1 calc R . . C31 C -0.0768(2) 0.4933(2) 1.06191(15) 0.0406(7) Uani 1 1 d . . . H31A H -0.0427 0.4367 1.0422 0.061 Uiso 1 1 calc R . . H31B H -0.1342 0.5179 1.0368 0.061 Uiso 1 1 calc R . . H31C H -0.1049 0.4720 1.1006 0.061 Uiso 1 1 calc R . . C9 C -0.0458(2) 0.6705(2) 1.10338(14) 0.0378(7) Uani 1 1 d . . . H9A H -0.0843 0.6459 1.1394 0.045 Uiso 1 1 calc R . . O4 O -0.12207(15) 0.71046(16) 1.06216(10) 0.0401(5) Uani 1 1 d . . . H4B H -0.1413 0.7669 1.0738 0.060 Uiso 1 1 calc R . . C10 C 0.0382(2) 0.7466(2) 1.12459(14) 0.0374(7) Uani 1 1 d . . . C32 C 0.1089(3) 0.7082(3) 1.17575(18) 0.0588(10) Uani 1 1 d . . . H32A H 0.1602 0.7597 1.1864 0.088 Uiso 1 1 calc R . . H32B H 0.1459 0.6480 1.1626 0.088 Uiso 1 1 calc R . . H32C H 0.0655 0.6926 1.2107 0.088 Uiso 1 1 calc R . . C11 C 0.0466(2) 0.8382(2) 1.10085(14) 0.0374(7) Uani 1 1 d . . . H11A H -0.0022 0.8538 1.0702 0.045 Uiso 1 1 calc R . . C12 C 0.1251(2) 0.9210(2) 1.11682(13) 0.0363(7) Uani 1 1 d . . . H12A H 0.1787 0.8913 1.1442 0.044 Uiso 1 1 calc R . . C33 C 0.0679(3) 1.0061(3) 1.15219(15) 0.0448(8) Uani 1 1 d . . . H33A H 0.0344 0.9780 1.1878 0.067 Uiso 1 1 calc R . . H33B H 0.0145 1.0367 1.1266 0.067 Uiso 1 1 calc R . . H33C H 0.1192 1.0567 1.1642 0.067 Uiso 1 1 calc R . . C13 C 0.1838(2) 0.9553(2) 1.05882(13) 0.0325(7) Uani 1 1 d . . . H13A H 0.2245 0.8970 1.0432 0.039 Uiso 1 1 calc R . . O5 O 0.26062(14) 1.03604(14) 1.07443(9) 0.0333(5) Uani 1 1 d . . . C131 C 0.3563(2) 1.0069(2) 1.09615(13) 0.0346(7) Uani 1 1 d . . . O132 O 0.38123(15) 0.92017(15) 1.10591(9) 0.0387(5) Uani 1 1 d . . . C132 C 0.4283(2) 1.0968(2) 1.10737(16) 0.0468(8) Uani 1 1 d . . . H13B H 0.4961 1.0736 1.1226 0.070 Uiso 1 1 calc R . . H13C H 0.3957 1.1412 1.1368 0.070 Uiso 1 1 calc R . . H13D H 0.4391 1.1331 1.0698 0.070 Uiso 1 1 calc R . . C14 C 0.1146(2) 0.9948(2) 1.00785(13) 0.0324(7) Uani 1 1 d . . . C34 C 0.0575(3) 1.0943(3) 1.01591(16) 0.0504(9) Uani 1 1 d . . . H34A H 0.0167 1.1093 0.9799 0.076 Uiso 1 1 calc R . . H34B H 0.1091 1.1474 1.0226 0.076 Uiso 1 1 calc R . . H34C H 0.0103 1.0900 1.0504 0.076 Uiso 1 1 calc R . . C15 C 0.1000(2) 0.9362(2) 0.95898(13) 0.0341(7) Uani 1 1 d . . . H15A H 0.1422 0.8780 0.9571 0.041 Uiso 1 1 calc R . . C16 C 0.0243(2) 0.9518(2) 0.90642(13) 0.0338(7) Uani 1 1 d . . . H16A H -0.0023 1.0219 0.9082 0.041 Uiso 1 1 calc R . . C35 C -0.0715(2) 0.8802(3) 0.91240(15) 0.0449(8) Uani 1 1 d . . . H35A H -0.1055 0.8908 0.9512 0.067 Uiso 1 1 calc R . . H35B H -0.0474 0.8110 0.9096 0.067 Uiso 1 1 calc R . . H35C H -0.1217 0.8939 0.8803 0.067 Uiso 1 1 calc R . . C17 C 0.0808(2) 0.9370(2) 0.84504(13) 0.0317(7) Uani 1 1 d . . . H17A H 0.0278 0.9386 0.8121 0.038 Uiso 1 1 calc R . . C18 C 0.1717(2) 1.0103(2) 0.83054(13) 0.0334(7) Uani 1 1 d . . . H18A H 0.2202 1.0113 0.8657 0.040 Uiso 1 1 calc R . . C19 C 0.1310(2) 1.1193(2) 0.82029(16) 0.0386(7) Uani 1 1 d . . . H19A H 0.0694 1.1313 0.8463 0.046 Uiso 1 1 calc R . . H19B H 0.1077 1.1264 0.7783 0.046 Uiso 1 1 calc R . . C20 C 0.2172(2) 1.2004(2) 0.83390(17) 0.0464(9) Uani 1 1 d . . . H20A H 0.2858 1.1748 0.8184 0.056 Uiso 1 1 calc R . . C21 C 0.2293(3) 1.2178(2) 0.90221(19) 0.0549(10) Uani 1 1 d . . . H21A H 0.1650 1.2511 0.9171 0.066 Uiso 1 1 calc R . . H21B H 0.2340 1.1520 0.9222 0.066 Uiso 1 1 calc R . . C22 C 0.3255(3) 1.2809(3) 0.9212(3) 0.0791(14) Uani 1 1 d . . . H22A H 0.3252 1.2893 0.9647 0.119 Uiso 1 1 calc R . . H22B H 0.3220 1.3464 0.9019 0.119 Uiso 1 1 calc R . . H22C H 0.3901 1.2468 0.9090 0.119 Uiso 1 1 calc R . . C23 C 0.2357(3) 0.9761(2) 0.77522(15) 0.0439(8) Uani 1 1 d . . . H23A H 0.2622 0.9084 0.7819 0.066 Uiso 1 1 calc R . . H23B H 0.2949 1.0216 0.7690 0.066 Uiso 1 1 calc R . . H23C H 0.1904 0.9766 0.7398 0.066 Uiso 1 1 calc R . . C24 C 0.1920(3) 1.2992(2) 0.8003(2) 0.0628(11) Uani 1 1 d . . . H24A H 0.2468 1.3485 0.8088 0.094 Uiso 1 1 calc R . . H24B H 0.1239 1.3249 0.8137 0.094 Uiso 1 1 calc R . . H24C H 0.1894 1.2864 0.7572 0.094 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 0.0350(11) 0.0242(9) 0.0381(11) -0.0026(8) -0.0087(9) 0.0017(8) C2 0.0283(16) 0.0283(15) 0.0420(18) -0.0036(12) -0.0003(14) -0.0052(12) O2 0.0477(13) 0.0387(12) 0.0558(14) -0.0131(10) -0.0224(12) 0.0123(10) C3 0.0236(14) 0.0266(14) 0.0412(16) 0.0014(12) 0.0017(12) -0.0038(12) C25 0.0361(16) 0.0249(14) 0.0475(17) -0.0019(13) 0.0029(14) -0.0024(12) C26 0.0358(16) 0.0246(13) 0.0412(17) -0.0056(12) 0.0029(14) 0.0023(12) C27 0.0351(17) 0.0334(15) 0.0447(18) -0.0028(13) -0.0011(14) 0.0049(13) C28 0.049(2) 0.0392(16) 0.0452(19) 0.0021(14) 0.0043(16) 0.0049(15) C29 0.044(2) 0.0517(19) 0.049(2) 0.0020(16) 0.0133(16) 0.0019(15) C28' 0.0295(17) 0.074(2) 0.055(2) 0.0075(18) 0.0028(16) 0.0121(16) C27' 0.0401(19) 0.0530(19) 0.0450(18) 0.0055(15) 0.0029(15) 0.0121(15) N4 0.0211(12) 0.0292(11) 0.0400(14) 0.0025(10) 0.0029(10) -0.0015(9) C5 0.0274(16) 0.0206(13) 0.0489(18) -0.0038(12) 0.0009(13) -0.0009(11) O3 0.0222(11) 0.0400(11) 0.0520(13) 0.0030(9) 0.0048(9) 0.0026(8) C6 0.0246(14) 0.0278(14) 0.0430(16) 0.0030(12) 0.0052(13) -0.0019(12) C30 0.0354(17) 0.0410(17) 0.057(2) 0.0085(15) 0.0073(15) 0.0072(14) C7 0.0244(15) 0.0327(15) 0.0485(18) 0.0039(13) -0.0023(14) -0.0029(13) C8 0.0293(15) 0.0360(16) 0.0408(17) 0.0083(13) 0.0010(13) -0.0021(12) C31 0.0296(15) 0.0444(17) 0.0478(19) 0.0105(14) 0.0034(14) -0.0044(14) C9 0.0263(15) 0.0427(16) 0.0445(18) 0.0101(14) 0.0070(13) 0.0005(13) O4 0.0247(10) 0.0412(11) 0.0543(13) 0.0022(9) -0.0001(10) 0.0045(9) C10 0.0335(16) 0.0448(17) 0.0340(16) 0.0017(14) 0.0018(13) 0.0042(14) C32 0.070(3) 0.046(2) 0.061(2) 0.0032(17) -0.024(2) -0.0035(18) C11 0.0233(14) 0.0500(18) 0.0387(17) 0.0026(14) -0.0011(12) 0.0030(13) C12 0.0239(15) 0.0486(17) 0.0365(16) 0.0039(14) -0.0007(13) 0.0039(13) C33 0.0350(17) 0.058(2) 0.0411(18) -0.0022(15) 0.0057(14) -0.0019(15) C13 0.0246(14) 0.0340(15) 0.0389(16) -0.0032(12) -0.0005(12) 0.0001(12) O5 0.0219(10) 0.0365(10) 0.0415(11) -0.0039(8) -0.0003(8) 0.0002(8) C131 0.0196(14) 0.0435(18) 0.0406(17) -0.0067(14) 0.0034(12) 0.0014(13) O132 0.0252(10) 0.0382(12) 0.0528(13) 0.0005(9) -0.0016(9) 0.0042(9) C132 0.0256(15) 0.0469(18) 0.068(2) -0.0090(16) -0.0017(15) -0.0007(14) C14 0.0233(14) 0.0375(15) 0.0364(16) -0.0027(13) 0.0049(12) -0.0007(12) C34 0.054(2) 0.052(2) 0.0450(19) -0.0074(15) -0.0101(16) 0.0198(17) C15 0.0273(15) 0.0318(15) 0.0433(17) 0.0020(14) 0.0005(13) 0.0012(12) C16 0.0312(15) 0.0289(14) 0.0414(17) -0.0003(13) -0.0045(13) 0.0028(12) C35 0.0321(16) 0.0525(18) 0.050(2) 0.0037(16) 0.0011(15) -0.0030(14) C17 0.0305(15) 0.0245(13) 0.0400(16) -0.0018(12) -0.0101(13) 0.0016(11) C18 0.0303(15) 0.0332(15) 0.0367(16) -0.0009(12) -0.0055(12) 0.0001(13) C19 0.0302(16) 0.0275(15) 0.0582(19) 0.0062(13) -0.0057(14) 0.0022(12) C20 0.0287(16) 0.0276(15) 0.083(3) 0.0018(15) 0.0043(16) 0.0038(13) C21 0.0364(17) 0.0332(16) 0.095(3) -0.0182(17) -0.0075(18) 0.0038(14) C22 0.039(2) 0.061(2) 0.137(4) -0.041(3) -0.008(2) 0.0054(18) C23 0.0442(18) 0.0385(16) 0.0491(19) 0.0003(14) 0.0034(15) 0.0002(15) C24 0.0410(19) 0.0320(17) 0.115(3) 0.0108(19) 0.012(2) 0.0030(15) _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 C2 1.335(3) . ? O1 C17 1.462(3) . ? C2 O2 1.190(3) . ? C2 C3 1.524(4) . ? C3 N4 1.452(4) . ? C3 C25 1.533(4) . ? C25 C26 1.517(4) . ? C26 C27 1.378(4) . ? C26 C27' 1.382(5) . ? C27 C28 1.377(4) . ? C28 C29 1.373(5) . ? C29 C28' 1.386(5) . ? C28' C27' 1.385(5) . ? N4 C5 1.350(4) . ? C5 O3 1.229(3) . ? C5 C6 1.499(4) . ? C6 C7 1.329(4) . ? C6 C30 1.503(4) . ? C7 C8 1.504(4) . ? C8 C31 1.528(4) . ? C8 C9 1.533(4) . ? C9 O4 1.414(4) . ? C9 C10 1.521(4) . ? C10 C11 1.316(4) . ? C10 C32 1.513(5) . ? C11 C12 1.505(4) . ? C12 C13 1.535(4) . ? C12 C33 1.536(4) . ? C13 O5 1.470(3) . ? C13 C14 1.505(4) . ? O5 C131 1.342(3) . ? C131 O132 1.200(4) . ? C131 C132 1.505(4) . ? C14 C15 1.332(4) . ? C14 C34 1.499(4) . ? C15 C16 1.504(4) . ? C16 C35 1.527(4) . ? C16 C17 1.531(4) . ? C17 C18 1.522(4) . ? C18 C23 1.520(4) . ? C18 C19 1.537(4) . ? C19 C20 1.543(4) . ? C20 C21 1.522(5) . ? C20 C24 1.526(5) . ? C21 C22 1.517(5) . ? 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 C2 O1 C17 120.5(2) . . ? O2 C2 O1 125.3(3) . . ? O2 C2 C3 126.3(3) . . ? O1 C2 C3 108.4(2) . . ? N4 C3 C2 110.4(2) . . ? N4 C3 C25 113.6(2) . . ? C2 C3 C25 111.8(2) . . ? C26 C25 C3 109.5(2) . . ? C27 C26 C27' 118.5(3) . . ? C27 C26 C25 122.0(3) . . ? C27' C26 C25 119.2(3) . . ? C28 C27 C26 121.0(3) . . ? C29 C28 C27 120.4(3) . . ? C28 C29 C28' 119.5(3) . . ? C27' C28' C29 119.6(3) . . ? C26 C27' C28' 121.0(3) . . ? C5 N4 C3 119.7(2) . . ? O3 C5 N4 122.1(3) . . ? O3 C5 C6 120.4(3) . . ? N4 C5 C6 117.4(2) . . ? C7 C6 C5 121.4(3) . . ? C7 C6 C30 123.6(3) . . ? C5 C6 C30 114.8(2) . . ? C6 C7 C8 125.6(3) . . ? C7 C8 C31 110.5(2) . . ? C7 C8 C9 111.9(2) . . ? C31 C8 C9 111.4(2) . . ? O4 C9 C10 114.5(2) . . ? O4 C9 C8 106.4(2) . . ? C10 C9 C8 111.9(2) . . ? C11 C10 C32 123.5(3) . . ? C11 C10 C9 122.4(3) . . ? C32 C10 C9 114.1(3) . . ? C10 C11 C12 128.4(3) . . ? C11 C12 C13 109.3(2) . . ? C11 C12 C33 109.9(2) . . ? C13 C12 C33 115.2(3) . . ? O5 C13 C14 107.3(2) . . ? O5 C13 C12 109.3(2) . . ? C14 C13 C12 116.2(2) . . ? C131 O5 C13 117.2(2) . . ? O132 C131 O5 124.4(3) . . ? O132 C131 C132 124.2(3) . . ? O5 C131 C132 111.4(3) . . ? C15 C14 C34 122.3(3) . . ? C15 C14 C13 118.4(3) . . ? C34 C14 C13 119.1(3) . . ? C14 C15 C16 128.6(3) . . ? C15 C16 C35 110.0(2) . . ? C15 C16 C17 111.5(2) . . ? C35 C16 C17 110.9(2) . . ? O1 C17 C18 106.5(2) . . ? O1 C17 C16 105.0(2) . . ? C18 C17 C16 116.5(2) . . ? C23 C18 C17 111.8(2) . . ? C23 C18 C19 109.4(2) . . ? C17 C18 C19 112.0(2) . . ? C18 C19 C20 112.6(2) . . ? C21 C20 C24 111.6(3) . . ? C21 C20 C19 111.3(3) . . ? C24 C20 C19 110.5(3) . . ? C22 C21 C20 115.5(4) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 30.64 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.236 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.045