# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email bioduneseola@hotmail.com _publ_contact_author_name 'A. O. Eseola' loop_ _publ_author_name A.Eseola O.Adepitan H.Gorls data_a _database_code_depnum_ccdc_archive 'CCDC 839336' #TrackingRef 'C-dp.2THF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H44 N4 O3' _chemical_formula_weight 688.84 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6376(4) _cell_length_b 13.6428(6) _cell_length_c 29.0057(9) _cell_angle_alpha 101.577(2) _cell_angle_beta 91.754(2) _cell_angle_gamma 104.734(2) _cell_volume 3599.9(2) _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 Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9960 _exptl_absorpt_correction_T_max 0.9968 _exptl_special_details ; ? ; _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 ? _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 17185 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13787 _reflns_number_gt 10451 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+8.1975P] 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_number_reflns 13787 _refine_ls_number_parameters 963 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.1773 _refine_ls_wR_factor_gt 0.1584 _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_restrained_S_all 1.202 _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 O1A O -0.0825(3) 0.53997(19) -0.22857(8) 0.0216(5) Uani 1 1 d . . . N1A N 0.0603(3) 0.4578(2) -0.17673(9) 0.0177(6) Uani 1 1 d . . . H1NA H 0.062(4) 0.519(3) -0.1868(11) 0.013(8) Uiso 1 1 d . . . C1A C -0.1656(3) 0.4443(3) -0.25019(10) 0.0159(6) Uani 1 1 d . . . O1B O 0.7968(3) 0.82431(18) 0.27698(8) 0.0207(5) Uani 1 1 d . . . H1OB H 0.761(6) 0.877(4) 0.2645(18) 0.069(16) Uiso 1 1 d . . . N1B N 0.6510(3) 0.9029(2) 0.22579(9) 0.0165(5) Uani 1 1 d . . . C1B C 0.7142(3) 0.7281(3) 0.25500(10) 0.0170(6) Uani 1 1 d . . . O1TA O -0.5322(3) 0.36153(19) -0.40809(8) 0.0239(5) Uani 1 1 d . . . C1TA C -0.6784(4) 0.2969(3) -0.41713(13) 0.0345(9) Uani 1 1 d . . . H1TA H -0.7449 0.3327 -0.3999 0.041 Uiso 1 1 calc R . . H1TB H -0.6864 0.2307 -0.4070 0.041 Uiso 1 1 calc R . . O1TB O 0.3551(3) 0.6311(2) 0.09647(8) 0.0242(5) Uani 1 1 d . . . C1TB C 0.2140(4) 0.5676(3) 0.10093(12) 0.0299(8) Uani 1 1 d . . . H1TC H 0.1560 0.6102 0.1188 0.036 Uiso 1 1 calc R . . H1TD H 0.2211 0.5122 0.1176 0.036 Uiso 1 1 calc R . . O1TC O -0.0998(3) 0.1614(3) 0.10607(10) 0.0419(7) Uani 1 1 d . . . C1TC C -0.0019(5) 0.1646(4) 0.07047(16) 0.0489(12) Uani 1 1 d . . . H1TE H -0.0214 0.2086 0.0491 0.059 Uiso 1 1 calc R . . H1TF H -0.0117 0.0939 0.0515 0.059 Uiso 1 1 calc R . . O1TD O 1.0098(3) 1.1233(2) 0.42591(11) 0.0437(7) Uani 1 1 d . . . C1TD C 0.9199(5) 1.1027(4) 0.46273(15) 0.0440(11) Uani 1 1 d . . . H1TG H 0.8876 1.1646 0.4768 0.053 Uiso 1 1 calc R . . H1TH H 0.9719 1.0829 0.4878 0.053 Uiso 1 1 calc R . . N2A N -0.0117(3) 0.2887(2) -0.18004(9) 0.0179(6) Uani 1 1 d . . . C2A C -0.2771(3) 0.4325(3) -0.28527(11) 0.0173(6) Uani 1 1 d . . . N2B N 0.5001(3) 0.8068(2) 0.16583(9) 0.0165(5) Uani 1 1 d . . . H2NB H 0.452(5) 0.749(4) 0.1435(15) 0.042(12) Uiso 1 1 d . . . C2B C 0.7349(3) 0.6408(3) 0.27006(10) 0.0170(6) Uani 1 1 d . . . C2TA C -0.7135(5) 0.2774(3) -0.46984(14) 0.0398(10) Uani 1 1 d . . . H2TA H -0.8171 0.2692 -0.4776 0.048 Uiso 1 1 calc R . . H2TB H -0.6872 0.2146 -0.4864 0.048 Uiso 1 1 calc R . . C2TB C 0.1465(4) 0.5214(3) 0.05122(12) 0.0313(9) Uani 1 1 d . . . H2TC H 0.0404 0.5074 0.0498 0.038 Uiso 1 1 calc R . . H2TD H 0.1724 0.4563 0.0380 0.038 Uiso 1 1 calc R . . C2TC C 0.1475(5) 0.2093(4) 0.09509(16) 0.0506(12) Uani 1 1 d . . . H2TE H 0.1772 0.2859 0.1000 0.061 Uiso 1 1 calc R . . H2TF H 0.2190 0.1803 0.0771 0.061 Uiso 1 1 calc R . . C2TD C 0.7940(6) 1.0147(5) 0.43979(16) 0.0600(15) Uani 1 1 d . . . H2TG H 0.7043 1.0234 0.4537 0.072 Uiso 1 1 calc R . . H2TH H 0.8088 0.9477 0.4439 0.072 Uiso 1 1 calc R . . N3A N -0.2321(3) 0.6200(2) -0.27521(9) 0.0170(6) Uani 1 1 d . . . C3A C -0.3608(3) 0.3326(3) -0.30622(10) 0.0173(6) Uani 1 1 d . . . H3AA H -0.4361 0.3247 -0.3297 0.021 Uiso 1 1 calc R . . N3B N 0.9371(3) 0.7396(2) 0.33124(9) 0.0183(6) Uani 1 1 d . . . H3NB H 0.940(4) 0.798(3) 0.3227(12) 0.019(10) Uiso 1 1 d . . . C3B C 0.6471(3) 0.5428(3) 0.24829(10) 0.0174(6) Uani 1 1 d . . . H3BA H 0.6608 0.4837 0.2585 0.021 Uiso 1 1 calc R . . C3TA C -0.6214(4) 0.3743(3) -0.48265(13) 0.0332(9) Uani 1 1 d . . . H3TA H -0.6016 0.3613 -0.5163 0.040 Uiso 1 1 calc R . . H3TB H -0.6675 0.4322 -0.4760 0.040 Uiso 1 1 calc R . . C3TB C 0.2121(4) 0.6063(3) 0.02557(13) 0.0330(9) Uani 1 1 d . . . H3TC H 0.1603 0.6612 0.0303 0.040 Uiso 1 1 calc R . . H3TD H 0.2111 0.5780 -0.0087 0.040 Uiso 1 1 calc R . . C3TC C 0.1289(5) 0.1749(4) 0.14152(15) 0.0420(10) Uani 1 1 d . . . H3TE H 0.1353 0.1026 0.1384 0.050 Uiso 1 1 calc R . . H3TF H 0.2016 0.2211 0.1667 0.050 Uiso 1 1 calc R . . C3TD C 0.7856(5) 1.0183(3) 0.38802(14) 0.0382(10) Uani 1 1 d . . . H3TG H 0.6948 1.0326 0.3783 0.046 Uiso 1 1 calc R . . H3TH H 0.7927 0.9521 0.3680 0.046 Uiso 1 1 calc R . . N4A N -0.4030(3) 0.5278(2) -0.33083(9) 0.0181(6) Uani 1 1 d . . . H4NA H -0.461(5) 0.469(3) -0.3539(15) 0.041(12) Uiso 1 1 d . . . C4A C -0.3371(3) 0.2443(3) -0.29373(10) 0.0166(6) Uani 1 1 d . . . N4B N 0.8666(3) 0.5691(2) 0.32362(9) 0.0183(6) Uani 1 1 d . . . C4B C 0.5414(3) 0.5286(3) 0.21258(10) 0.0173(6) Uani 1 1 d . . . C4TA C -0.4864(4) 0.3962(3) -0.45054(12) 0.0260(8) Uani 1 1 d . . . H4TA H -0.4193 0.3579 -0.4657 0.031 Uiso 1 1 calc R . . H4TB H -0.4372 0.4713 -0.4431 0.031 Uiso 1 1 calc R . . C4TB C 0.3649(4) 0.6474(3) 0.04878(12) 0.0300(8) Uani 1 1 d . . . H4TC H 0.4292 0.6091 0.0318 0.036 Uiso 1 1 calc R . . H4TD H 0.4026 0.7221 0.0490 0.036 Uiso 1 1 calc R . . C4TC C -0.0207(5) 0.1838(4) 0.15132(14) 0.0396(10) Uani 1 1 d . . . H4TE H -0.0663 0.1336 0.1703 0.048 Uiso 1 1 calc R . . H4TF H -0.0173 0.2547 0.1688 0.048 Uiso 1 1 calc R . . C4TD C 0.9157(5) 1.1073(4) 0.38498(17) 0.0499(12) Uani 1 1 d . . . H4TG H 0.9642 1.0892 0.3561 0.060 Uiso 1 1 calc R . . H4TH H 0.8852 1.1710 0.3840 0.060 Uiso 1 1 calc R . . C5A C -0.2267(3) 0.2582(3) -0.25900(11) 0.0186(7) Uani 1 1 d . . . H5AA H -0.2090 0.1988 -0.2502 0.022 Uiso 1 1 calc R . . C5B C 0.5231(3) 0.6160(3) 0.19776(10) 0.0167(6) Uani 1 1 d . . . H5BA H 0.4511 0.6075 0.1731 0.020 Uiso 1 1 calc R . . C6A C -0.1411(3) 0.3563(3) -0.23669(10) 0.0146(6) Uani 1 1 d . . . C6B C 0.6079(3) 0.7155(3) 0.21821(10) 0.0156(6) Uani 1 1 d . . . C7A C -0.4285(4) 0.1381(3) -0.31708(11) 0.0214(7) Uani 1 1 d . . . H7AA H -0.5021 0.1443 -0.3396 0.032 Uiso 1 1 calc R . . H7AB H -0.4752 0.1031 -0.2930 0.032 Uiso 1 1 calc R . . H7AC H -0.3677 0.0975 -0.3339 0.032 Uiso 1 1 calc R . . C7B C 0.4473(4) 0.4214(3) 0.18970(11) 0.0221(7) Uani 1 1 d . . . H7BA H 0.4446 0.3747 0.2115 0.033 Uiso 1 1 calc R . . H7BB H 0.4869 0.3945 0.1606 0.033 Uiso 1 1 calc R . . H7BC H 0.3494 0.4257 0.1822 0.033 Uiso 1 1 calc R . . C8A C -0.0306(3) 0.3659(3) -0.19901(10) 0.0165(6) Uani 1 1 d . . . C8B C 0.5860(3) 0.8069(3) 0.20344(11) 0.0179(7) Uani 1 1 d . . . C9A C 0.0966(3) 0.3348(3) -0.14383(11) 0.0174(6) Uani 1 1 d . . . C9B C 0.5112(3) 0.9086(3) 0.16337(10) 0.0161(6) Uani 1 1 d . . . C10A C 0.1443(3) 0.4403(3) -0.14144(11) 0.0181(7) Uani 1 1 d . . . C10B C 0.6052(3) 0.9691(3) 0.20154(10) 0.0167(6) Uani 1 1 d . . . C11A C 0.1382(3) 0.2713(3) -0.11285(11) 0.0177(6) Uani 1 1 d . . . C11B C 0.4265(4) 0.9292(3) 0.12493(11) 0.0183(7) Uani 1 1 d . . . C12A C 0.1452(4) 0.1708(3) -0.13220(12) 0.0224(7) Uani 1 1 d . . . H12A H 0.1255 0.1442 -0.1653 0.027 Uiso 1 1 calc R . . C12B C 0.2782(4) 0.8839(3) 0.11766(12) 0.0228(7) Uani 1 1 d . . . H12B H 0.2319 0.8433 0.1387 0.027 Uiso 1 1 calc R . . C13A C 0.1810(4) 0.1089(3) -0.10336(13) 0.0262(8) Uani 1 1 d . . . H13A H 0.1849 0.0403 -0.1168 0.031 Uiso 1 1 calc R . . C13B C 0.1977(4) 0.8974(3) 0.08007(13) 0.0290(8) Uani 1 1 d . . . H13B H 0.0970 0.8656 0.0752 0.035 Uiso 1 1 calc R . . C14A C 0.2109(4) 0.1474(3) -0.05493(13) 0.0294(8) Uani 1 1 d . . . H14A H 0.2368 0.1057 -0.0353 0.035 Uiso 1 1 calc R . . C14B C 0.2645(4) 0.9574(3) 0.04964(12) 0.0299(8) Uani 1 1 d . . . H14B H 0.2096 0.9666 0.0239 0.036 Uiso 1 1 calc R . . C15A C 0.2029(4) 0.2468(3) -0.03553(12) 0.0271(8) Uani 1 1 d . . . H15A H 0.2223 0.2731 -0.0024 0.032 Uiso 1 1 calc R . . C15B C 0.4108(4) 1.0037(3) 0.05669(12) 0.0254(8) Uani 1 1 d . . . H15B H 0.4558 1.0458 0.0361 0.031 Uiso 1 1 calc R . . C16A C 0.1663(4) 0.3088(3) -0.06419(12) 0.0230(7) Uani 1 1 d . . . H16A H 0.1605 0.3768 -0.0505 0.028 Uiso 1 1 calc R . . C16B C 0.4925(4) 0.9891(3) 0.09372(11) 0.0210(7) Uani 1 1 d . . . H16B H 0.5935 1.0198 0.0979 0.025 Uiso 1 1 calc R . . C17A C 0.2540(3) 0.5266(3) -0.11192(10) 0.0176(7) Uani 1 1 d . . . C17B C 0.6485(3) 1.0809(3) 0.22216(11) 0.0169(6) Uani 1 1 d . . . C18A C 0.3785(3) 0.5109(3) -0.09171(11) 0.0197(7) Uani 1 1 d . . . H18A H 0.3918 0.4430 -0.0965 0.024 Uiso 1 1 calc R . . C18B C 0.6450(4) 1.1576(3) 0.19671(12) 0.0250(8) Uani 1 1 d . . . H18B H 0.6128 1.1378 0.1641 0.030 Uiso 1 1 calc R . . C19A C 0.4824(4) 0.5948(3) -0.06471(11) 0.0240(7) Uani 1 1 d . . . H19A H 0.5659 0.5836 -0.0507 0.029 Uiso 1 1 calc R . . C19B C 0.6879(4) 1.2618(3) 0.21855(12) 0.0259(8) Uani 1 1 d . . . H19B H 0.6850 1.3123 0.2005 0.031 Uiso 1 1 calc R . . C20A C 0.4661(4) 0.6944(3) -0.05790(12) 0.0262(8) Uani 1 1 d . . . H20A H 0.5382 0.7511 -0.0396 0.031 Uiso 1 1 calc R . . C20B C 0.7349(4) 1.2940(3) 0.26612(12) 0.0230(7) Uani 1 1 d . . . H20B H 0.7652 1.3657 0.2807 0.028 Uiso 1 1 calc R . . C21A C 0.3445(4) 0.7111(3) -0.07789(12) 0.0260(8) Uani 1 1 d . . . H21A H 0.3331 0.7794 -0.0736 0.031 Uiso 1 1 calc R . . C21B C 0.7365(3) 1.2182(3) 0.29204(12) 0.0218(7) Uani 1 1 d . . . H21B H 0.7668 1.2384 0.3248 0.026 Uiso 1 1 calc R . . C22A C 0.2388(4) 0.6276(3) -0.10437(11) 0.0217(7) Uani 1 1 d . . . H22A H 0.1547 0.6395 -0.1176 0.026 Uiso 1 1 calc R . . C22B C 0.6946(3) 1.1141(3) 0.27038(11) 0.0200(7) Uani 1 1 d . . . H22B H 0.6970 1.0638 0.2886 0.024 Uiso 1 1 calc R . . C23A C -0.3036(3) 0.5245(3) -0.29743(10) 0.0167(6) Uani 1 1 d . . . C23B C 0.8452(3) 0.6492(3) 0.30760(10) 0.0159(6) Uani 1 1 d . . . C24A C -0.3944(3) 0.6308(3) -0.33002(11) 0.0173(6) Uani 1 1 d . . . C24B C 0.9784(3) 0.6108(3) 0.35882(11) 0.0174(6) Uani 1 1 d . . . C25A C -0.2872(3) 0.6882(3) -0.29481(11) 0.0171(6) Uani 1 1 d . . . C25B C 1.0250(3) 0.7174(3) 0.36389(11) 0.0173(6) Uani 1 1 d . . . C26A C -0.4811(3) 0.6618(3) -0.36438(10) 0.0166(6) Uani 1 1 d . . . C26B C 1.0276(3) 0.5408(3) 0.38414(11) 0.0193(7) Uani 1 1 d . . . C27A C -0.4265(4) 0.7506(3) -0.38154(12) 0.0249(7) Uani 1 1 d . . . H27A H -0.3315 0.7924 -0.3711 0.030 Uiso 1 1 calc R . . C27B C 1.0659(4) 0.5667(3) 0.43271(11) 0.0214(7) Uani 1 1 d . . . H27B H 1.0623 0.6322 0.4507 0.026 Uiso 1 1 calc R . . C28A C -0.5099(4) 0.7786(3) -0.41381(13) 0.0313(9) Uani 1 1 d . . . H28A H -0.4720 0.8400 -0.4250 0.038 Uiso 1 1 calc R . . C28B C 1.1094(4) 0.4966(3) 0.45495(12) 0.0237(7) Uani 1 1 d . . . H28B H 1.1374 0.5153 0.4879 0.028 Uiso 1 1 calc R . . C29A C -0.6479(4) 0.7179(3) -0.42985(12) 0.0251(8) Uani 1 1 d . . . H29A H -0.7044 0.7371 -0.4521 0.030 Uiso 1 1 calc R . . C29B C 1.1122(4) 0.3997(3) 0.42935(12) 0.0251(8) Uani 1 1 d . . . H29B H 1.1406 0.3518 0.4447 0.030 Uiso 1 1 calc R . . C30A C -0.7023(4) 0.6291(3) -0.41308(11) 0.0220(7) Uani 1 1 d . . . H30A H -0.7966 0.5869 -0.4242 0.026 Uiso 1 1 calc R . . C30B C 1.0732(3) 0.3735(3) 0.38126(12) 0.0215(7) Uani 1 1 d . . . H30B H 1.0758 0.3076 0.3635 0.026 Uiso 1 1 calc R . . C31A C -0.6215(3) 0.6007(3) -0.38034(11) 0.0184(7) Uani 1 1 d . . . H31A H -0.6609 0.5401 -0.3687 0.022 Uiso 1 1 calc R . . C31B C 1.0302(3) 0.4433(3) 0.35886(11) 0.0198(7) Uani 1 1 d . . . H31B H 1.0023 0.4241 0.3259 0.024 Uiso 1 1 calc R . . C32A C -0.2325(3) 0.8001(3) -0.27643(11) 0.0180(6) Uani 1 1 d . . . C32B C 1.1394(3) 0.8005(3) 0.39402(10) 0.0179(7) Uani 1 1 d . . . C33A C -0.0847(3) 0.8445(3) -0.26564(11) 0.0204(7) Uani 1 1 d . . . H33A H -0.0200 0.8021 -0.2713 0.024 Uiso 1 1 calc R . . C33B C 1.1283(4) 0.9024(3) 0.40383(12) 0.0233(7) Uani 1 1 d . . . H33B H 1.0451 0.9176 0.3919 0.028 Uiso 1 1 calc R . . C34A C -0.0317(4) 0.9498(3) -0.24681(12) 0.0233(7) Uani 1 1 d . . . H34A H 0.0691 0.9791 -0.2398 0.028 Uiso 1 1 calc R . . C34B C 1.2378(4) 0.9822(3) 0.43090(12) 0.0255(8) Uani 1 1 d . . . H34B H 1.2294 1.0514 0.4371 0.031 Uiso 1 1 calc R . . C35A C -0.1248(4) 1.0127(3) -0.23806(12) 0.0252(8) Uani 1 1 d . . . H35A H -0.0882 1.0849 -0.2252 0.030 Uiso 1 1 calc R . . C35B C 1.3587(4) 0.9610(3) 0.44878(12) 0.0244(7) Uani 1 1 d . . . H35B H 1.4333 1.0153 0.4674 0.029 Uiso 1 1 calc R . . C36A C -0.2718(4) 0.9691(3) -0.24821(13) 0.0254(8) Uani 1 1 d . . . H36A H -0.3361 1.0118 -0.2420 0.031 Uiso 1 1 calc R . . C36B C 1.3706(4) 0.8602(3) 0.43933(11) 0.0220(7) Uani 1 1 d . . . H36B H 1.4536 0.8455 0.4518 0.026 Uiso 1 1 calc R . . C37A C -0.3260(4) 0.8636(3) -0.26741(12) 0.0230(7) Uani 1 1 d . . . H37A H -0.4269 0.8347 -0.2744 0.028 Uiso 1 1 calc R . . C37B C 1.2627(4) 0.7800(3) 0.41192(11) 0.0216(7) Uani 1 1 d . . . H37B H 1.2729 0.7112 0.4054 0.026 Uiso 1 1 calc R . . H1OA H -0.124(6) 0.592(4) -0.2398(18) 0.074(17) Uiso 1 1 d . . . 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 O1A 0.0231(12) 0.0133(13) 0.0254(12) 0.0034(9) -0.0085(9) 0.0012(10) N1A 0.0190(13) 0.0163(16) 0.0168(13) 0.0042(11) -0.0026(10) 0.0028(12) C1A 0.0168(15) 0.0144(17) 0.0139(14) 0.0017(12) -0.0006(11) 0.0009(13) O1B 0.0236(12) 0.0109(13) 0.0247(12) 0.0040(9) -0.0063(9) 0.0002(10) N1B 0.0195(13) 0.0122(15) 0.0173(13) 0.0021(10) -0.0015(10) 0.0046(11) C1B 0.0181(15) 0.0129(17) 0.0175(15) 0.0021(12) 0.0028(12) 0.0004(13) O1TA 0.0246(13) 0.0216(14) 0.0211(12) 0.0028(10) -0.0034(9) 0.0002(11) C1TA 0.027(2) 0.031(2) 0.036(2) 0.0004(17) 0.0061(16) -0.0041(17) O1TB 0.0225(12) 0.0248(15) 0.0188(11) 0.0007(10) -0.0039(9) -0.0013(11) C1TB 0.0261(19) 0.033(2) 0.0266(18) 0.0082(15) 0.0032(15) -0.0006(16) O1TC 0.0370(16) 0.051(2) 0.0406(16) 0.0148(14) 0.0018(13) 0.0136(15) C1TC 0.049(3) 0.054(3) 0.039(2) 0.009(2) 0.003(2) 0.007(2) O1TD 0.0290(15) 0.038(2) 0.064(2) 0.0174(15) -0.0019(14) 0.0032(14) C1TD 0.042(2) 0.047(3) 0.038(2) 0.002(2) -0.0088(19) 0.010(2) N2A 0.0170(13) 0.0184(16) 0.0171(13) 0.0023(11) -0.0009(10) 0.0041(11) C2A 0.0157(15) 0.0195(18) 0.0172(15) 0.0048(12) 0.0028(12) 0.0048(13) N2B 0.0213(14) 0.0128(15) 0.0155(13) 0.0028(10) -0.0003(10) 0.0053(12) C2B 0.0171(15) 0.0178(18) 0.0168(15) 0.0040(12) -0.0007(12) 0.0061(13) C2TA 0.032(2) 0.038(3) 0.037(2) -0.0024(18) -0.0115(17) -0.0011(19) C2TB 0.0255(19) 0.035(2) 0.0273(19) -0.0006(16) -0.0047(15) 0.0039(17) C2TC 0.041(3) 0.057(4) 0.048(3) 0.016(2) 0.003(2) 0.000(2) C2TD 0.054(3) 0.068(4) 0.037(2) 0.011(2) 0.006(2) -0.021(3) N3A 0.0165(13) 0.0150(15) 0.0185(13) 0.0034(10) 0.0002(10) 0.0027(11) C3A 0.0159(15) 0.0191(18) 0.0151(14) 0.0019(12) -0.0040(11) 0.0033(13) N3B 0.0185(14) 0.0159(16) 0.0195(13) 0.0051(11) -0.0031(10) 0.0022(12) C3B 0.0228(16) 0.0139(17) 0.0171(15) 0.0051(12) 0.0035(12) 0.0060(13) C3TA 0.041(2) 0.034(2) 0.0262(19) 0.0049(16) -0.0058(16) 0.0147(19) C3TB 0.030(2) 0.044(3) 0.0250(18) 0.0091(17) -0.0056(15) 0.0098(19) C3TC 0.035(2) 0.044(3) 0.043(2) 0.013(2) -0.0021(18) 0.003(2) C3TD 0.036(2) 0.032(3) 0.038(2) 0.0020(18) -0.0051(17) 0.0002(19) N4A 0.0171(13) 0.0149(15) 0.0209(14) 0.0037(11) 0.0000(11) 0.0021(11) C4A 0.0188(15) 0.0132(17) 0.0163(14) 0.0033(12) 0.0026(12) 0.0014(13) N4B 0.0210(14) 0.0196(16) 0.0156(13) 0.0044(11) -0.0015(10) 0.0075(12) C4B 0.0173(15) 0.0153(18) 0.0169(15) 0.0015(12) 0.0015(12) 0.0018(13) C4TA 0.0273(18) 0.029(2) 0.0227(17) 0.0105(15) 0.0020(14) 0.0049(16) C4TB 0.032(2) 0.037(2) 0.0176(16) 0.0063(15) 0.0025(14) 0.0028(17) C4TC 0.044(2) 0.038(3) 0.035(2) 0.0042(18) -0.0011(18) 0.011(2) C4TD 0.047(3) 0.052(3) 0.050(3) 0.025(2) 0.000(2) 0.003(2) C5A 0.0185(16) 0.0181(18) 0.0196(15) 0.0055(12) 0.0041(12) 0.0041(14) C5B 0.0159(15) 0.0172(18) 0.0156(14) 0.0029(12) -0.0015(11) 0.0029(13) C6A 0.0137(14) 0.0137(17) 0.0149(14) 0.0026(11) 0.0005(11) 0.0013(12) C6B 0.0161(15) 0.0164(17) 0.0150(14) 0.0043(12) 0.0020(11) 0.0049(13) C7A 0.0224(17) 0.0172(19) 0.0220(16) 0.0042(13) -0.0031(13) 0.0010(14) C7B 0.0219(17) 0.0188(19) 0.0223(16) 0.0040(13) -0.0015(13) 0.0005(14) C8A 0.0166(15) 0.0153(17) 0.0175(15) 0.0032(12) 0.0008(12) 0.0044(13) C8B 0.0177(15) 0.0195(18) 0.0171(15) 0.0031(12) -0.0002(12) 0.0068(14) C9A 0.0163(15) 0.0186(18) 0.0181(15) 0.0034(12) 0.0010(12) 0.0064(13) C9B 0.0178(15) 0.0136(17) 0.0176(15) 0.0053(12) 0.0027(12) 0.0038(13) C10A 0.0203(16) 0.0177(18) 0.0170(15) 0.0054(12) 0.0003(12) 0.0051(14) C10B 0.0170(15) 0.0165(18) 0.0168(15) 0.0042(12) 0.0022(12) 0.0043(13) C11A 0.0151(15) 0.0189(19) 0.0196(15) 0.0069(13) -0.0001(12) 0.0037(13) C11B 0.0225(16) 0.0144(18) 0.0173(15) 0.0019(12) -0.0022(12) 0.0051(14) C12A 0.0218(17) 0.021(2) 0.0253(17) 0.0060(14) 0.0017(13) 0.0063(15) C12B 0.0250(17) 0.0195(19) 0.0250(17) 0.0071(13) 0.0017(13) 0.0062(15) C13A 0.0206(17) 0.018(2) 0.042(2) 0.0093(15) 0.0019(15) 0.0053(15) C13B 0.0196(17) 0.033(2) 0.0331(19) 0.0093(16) -0.0053(14) 0.0048(16) C14A 0.0266(19) 0.029(2) 0.038(2) 0.0183(16) -0.0022(15) 0.0081(17) C14B 0.032(2) 0.033(2) 0.0252(18) 0.0104(15) -0.0109(15) 0.0074(17) C15A 0.0268(18) 0.029(2) 0.0240(17) 0.0113(15) -0.0059(14) 0.0010(16) C15B 0.034(2) 0.023(2) 0.0212(16) 0.0089(14) 0.0006(14) 0.0069(16) C16A 0.0268(18) 0.0175(19) 0.0234(17) 0.0051(13) -0.0021(13) 0.0034(15) C16B 0.0216(16) 0.0206(19) 0.0207(16) 0.0035(13) 0.0017(13) 0.0066(14) C17A 0.0184(15) 0.0195(18) 0.0137(14) 0.0043(12) 0.0014(12) 0.0022(13) C17B 0.0157(15) 0.0129(17) 0.0220(15) 0.0044(12) 0.0014(12) 0.0031(13) C18A 0.0179(16) 0.0196(19) 0.0202(15) 0.0048(13) -0.0004(12) 0.0026(14) C18B 0.0287(18) 0.022(2) 0.0213(16) 0.0022(14) -0.0026(14) 0.0040(16) C19A 0.0214(17) 0.027(2) 0.0222(17) 0.0048(14) -0.0004(13) 0.0044(15) C19B 0.0313(19) 0.020(2) 0.0286(18) 0.0079(14) 0.0019(15) 0.0077(16) C20A 0.0234(17) 0.024(2) 0.0258(17) 0.0044(14) -0.0017(14) -0.0030(15) C20B 0.0215(17) 0.0149(18) 0.0314(18) 0.0030(14) -0.0025(14) 0.0049(14) C21A 0.0277(18) 0.019(2) 0.0285(18) 0.0035(14) -0.0019(14) 0.0035(15) C21B 0.0188(16) 0.0206(19) 0.0225(16) -0.0029(13) -0.0056(13) 0.0057(14) C22A 0.0217(16) 0.0192(19) 0.0229(16) 0.0066(13) -0.0045(13) 0.0021(14) C22B 0.0196(16) 0.0178(19) 0.0240(16) 0.0035(13) -0.0003(13) 0.0082(14) C23A 0.0168(15) 0.0166(18) 0.0167(15) 0.0040(12) 0.0003(12) 0.0040(13) C23B 0.0138(14) 0.0145(17) 0.0183(15) 0.0033(12) -0.0004(11) 0.0024(13) C24A 0.0155(15) 0.0134(17) 0.0235(16) 0.0063(12) 0.0013(12) 0.0029(13) C24B 0.0129(14) 0.0214(18) 0.0173(15) 0.0031(12) -0.0004(11) 0.0043(13) C25A 0.0133(14) 0.0172(18) 0.0202(15) 0.0048(12) 0.0023(12) 0.0024(13) C25B 0.0150(15) 0.0200(18) 0.0170(15) 0.0051(12) 0.0005(12) 0.0039(13) C26A 0.0153(15) 0.0172(18) 0.0161(14) 0.0017(12) -0.0025(11) 0.0040(13) C26B 0.0159(15) 0.021(2) 0.0205(16) 0.0070(13) 0.0006(12) 0.0027(14) C27A 0.0198(17) 0.020(2) 0.0316(18) 0.0089(14) -0.0022(14) -0.0019(14) C27B 0.0221(17) 0.022(2) 0.0192(16) 0.0056(13) 0.0036(13) 0.0027(14) C28A 0.033(2) 0.025(2) 0.038(2) 0.0183(16) -0.0016(16) 0.0039(17) C28B 0.0181(16) 0.032(2) 0.0199(16) 0.0093(14) -0.0024(12) 0.0015(15) C29A 0.0243(18) 0.029(2) 0.0255(17) 0.0095(15) -0.0012(14) 0.0110(16) C29B 0.0198(17) 0.026(2) 0.0333(19) 0.0167(15) 0.0006(14) 0.0051(15) C30A 0.0174(16) 0.025(2) 0.0219(16) 0.0023(13) -0.0037(12) 0.0045(14) C30B 0.0193(16) 0.0201(19) 0.0270(17) 0.0074(14) 0.0052(13) 0.0063(14) C31A 0.0205(16) 0.0134(17) 0.0206(15) 0.0037(12) 0.0013(12) 0.0030(13) C31B 0.0167(15) 0.022(2) 0.0186(15) 0.0044(13) 0.0002(12) 0.0018(14) C32A 0.0204(16) 0.0114(17) 0.0205(15) 0.0038(12) 0.0014(12) 0.0009(13) C32B 0.0183(15) 0.0185(18) 0.0157(15) 0.0046(12) 0.0028(12) 0.0018(13) C33A 0.0181(16) 0.0196(19) 0.0244(16) 0.0036(13) 0.0014(13) 0.0078(14) C33B 0.0218(17) 0.020(2) 0.0289(18) 0.0061(14) -0.0010(14) 0.0060(15) C34A 0.0172(16) 0.0186(19) 0.0303(18) 0.0035(14) -0.0024(13) 0.0000(14) C34B 0.0252(18) 0.0178(19) 0.0289(18) -0.0007(14) -0.0041(14) 0.0026(15) C35A 0.0258(18) 0.0121(18) 0.0342(19) -0.0003(14) -0.0059(14) 0.0039(15) C35B 0.0253(18) 0.019(2) 0.0237(17) 0.0042(13) -0.0046(14) -0.0028(15) C36A 0.0219(17) 0.019(2) 0.0361(19) 0.0019(15) 0.0011(14) 0.0090(15) C36B 0.0182(16) 0.025(2) 0.0227(16) 0.0086(14) -0.0030(13) 0.0026(15) C37A 0.0155(15) 0.0196(19) 0.0323(18) 0.0038(14) -0.0016(13) 0.0036(14) C37B 0.0233(17) 0.0205(19) 0.0199(16) 0.0045(13) 0.0001(13) 0.0038(14) _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 O1A C1A 1.359(4) . ? O1A H1OA 1.00(5) . ? N1A C8A 1.355(4) . ? N1A C10A 1.380(4) . ? N1A H1NA 0.93(3) . ? C1A C6A 1.406(4) . ? C1A C2A 1.412(4) . ? O1B C1B 1.366(4) . ? O1B H1OB 1.00(5) . ? N1B C8B 1.321(4) . ? N1B C10B 1.394(4) . ? C1B C2B 1.405(4) . ? C1B C6B 1.409(4) . ? O1TA C1TA 1.444(4) . ? O1TA C4TA 1.447(4) . ? C1TA C2TA 1.511(5) . ? C1TA H1TA 0.9900 . ? C1TA H1TB 0.9900 . ? O1TB C1TB 1.440(4) . ? O1TB C4TB 1.447(4) . ? C1TB C2TB 1.506(5) . ? C1TB H1TC 0.9900 . ? C1TB H1TD 0.9900 . ? O1TC C1TC 1.420(5) . ? O1TC C4TC 1.434(5) . ? C1TC C2TC 1.507(6) . ? C1TC H1TE 0.9900 . ? C1TC H1TF 0.9900 . ? O1TD C4TD 1.418(5) . ? O1TD C1TD 1.423(5) . ? C1TD C2TD 1.498(6) . ? C1TD H1TG 0.9900 . ? C1TD H1TH 0.9900 . ? N2A C8A 1.331(4) . ? N2A C9A 1.387(4) . ? C2A C3A 1.398(4) . ? C2A C23A 1.450(4) . ? N2B C8B 1.349(4) . ? N2B C9B 1.382(4) . ? N2B H2NB 0.92(4) . ? C2B C3B 1.399(5) . ? C2B C23B 1.465(4) . ? C2TA C3TA 1.515(6) . ? C2TA H2TA 0.9900 . ? C2TA H2TB 0.9900 . ? C2TB C3TB 1.516(5) . ? C2TB H2TC 0.9900 . ? C2TB H2TD 0.9900 . ? C2TC C3TC 1.514(6) . ? C2TC H2TE 0.9900 . ? C2TC H2TF 0.9900 . ? C2TD C3TD 1.512(6) . ? C2TD H2TG 0.9900 . ? C2TD H2TH 0.9900 . ? N3A C23A 1.329(4) . ? N3A C25A 1.384(4) . ? C3A C4A 1.394(4) . ? C3A H3AA 0.9500 . ? N3B C23B 1.358(4) . ? N3B C25B 1.380(4) . ? N3B H3NB 0.87(4) . ? C3B C4B 1.379(4) . ? C3B H3BA 0.9500 . ? C3TA C4TA 1.506(5) . ? C3TA H3TA 0.9900 . ? C3TA H3TB 0.9900 . ? C3TB C4TB 1.518(5) . ? C3TB H3TC 0.9900 . ? C3TB H3TD 0.9900 . ? C3TC C4TC 1.508(6) . ? C3TC H3TE 0.9900 . ? C3TC H3TF 0.9900 . ? C3TD C4TD 1.526(6) . ? C3TD H3TG 0.9900 . ? C3TD H3TH 0.9900 . ? N4A C23A 1.357(4) . ? N4A C24A 1.382(4) . ? N4A H4NA 0.97(4) . ? C4A C5A 1.392(4) . ? C4A C7A 1.502(4) . ? N4B C23B 1.329(4) . ? N4B C24B 1.384(4) . ? C4B C5B 1.395(5) . ? C4B C7B 1.516(4) . ? C4TA H4TA 0.9900 . ? C4TA H4TB 0.9900 . ? C4TB H4TC 0.9900 . ? C4TB H4TD 0.9900 . ? C4TC H4TE 0.9900 . ? C4TC H4TF 0.9900 . ? C4TD H4TG 0.9900 . ? C4TD H4TH 0.9900 . ? C5A C6A 1.396(4) . ? C5A H5AA 0.9500 . ? C5B C6B 1.395(4) . ? C5B H5BA 0.9500 . ? C6A C8A 1.465(4) . ? C6B C8B 1.458(4) . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? C7B H7BA 0.9800 . ? C7B H7BB 0.9800 . ? C7B H7BC 0.9800 . ? C9A C10A 1.383(5) . ? C9A C11A 1.478(4) . ? C9B C10B 1.386(4) . ? C9B C11B 1.475(4) . ? C10A C17A 1.464(4) . ? C10B C17B 1.467(4) . ? C11A C12A 1.393(5) . ? C11A C16A 1.394(4) . ? C11B C12B 1.396(5) . ? C11B C16B 1.400(4) . ? C12A C13A 1.395(5) . ? C12A H12A 0.9500 . ? C12B C13B 1.388(5) . ? C12B H12B 0.9500 . ? C13A C14A 1.391(5) . ? C13A H13A 0.9500 . ? C13B C14B 1.386(5) . ? C13B H13B 0.9500 . ? C14A C15A 1.383(5) . ? C14A H14A 0.9500 . ? C14B C15B 1.380(5) . ? C14B H14B 0.9500 . ? C15A C16A 1.394(5) . ? C15A H15A 0.9500 . ? C15B C16B 1.389(5) . ? C15B H15B 0.9500 . ? C16A H16A 0.9500 . ? C16B H16B 0.9500 . ? C17A C22A 1.396(5) . ? C17A C18A 1.403(4) . ? C17B C22B 1.401(4) . ? C17B C18B 1.403(5) . ? C18A C19A 1.392(5) . ? C18A H18A 0.9500 . ? C18B C19B 1.385(5) . ? C18B H18B 0.9500 . ? C19A C20A 1.383(5) . ? C19A H19A 0.9500 . ? C19B C20B 1.385(5) . ? C19B H19B 0.9500 . ? C20A C21A 1.381(5) . ? C20A H20A 0.9500 . ? C20B C21B 1.399(5) . ? C20B H20B 0.9500 . ? C21A C22A 1.391(5) . ? C21A H21A 0.9500 . ? C21B C22B 1.382(5) . ? C21B H21B 0.9500 . ? C22A H22A 0.9500 . ? C22B H22B 0.9500 . ? C24A C25A 1.388(4) . ? C24A C26A 1.472(4) . ? C24B C25B 1.384(5) . ? C24B C26B 1.472(4) . ? C25A C32A 1.462(4) . ? C25B C32B 1.474(4) . ? C26A C27A 1.388(5) . ? C26A C31A 1.405(4) . ? C26B C31B 1.391(5) . ? C26B C27B 1.396(4) . ? C27A C28A 1.386(5) . ? C27A H27A 0.9500 . ? C27B C28B 1.393(5) . ? C27B H27B 0.9500 . ? C28A C29A 1.385(5) . ? C28A H28A 0.9500 . ? C28B C29B 1.387(5) . ? C28B H28B 0.9500 . ? C29A C30A 1.382(5) . ? C29A H29A 0.9500 . ? C29B C30B 1.384(5) . ? C29B H29B 0.9500 . ? C30A C31A 1.383(4) . ? C30A H30A 0.9500 . ? C30B C31B 1.390(5) . ? C30B H30B 0.9500 . ? C31A H31A 0.9500 . ? C31B H31B 0.9500 . ? C32A C33A 1.396(4) . ? C32A C37A 1.398(4) . ? C32B C33B 1.394(5) . ? C32B C37B 1.397(4) . ? C33A C34A 1.385(5) . ? C33A H33A 0.9500 . ? C33B C34B 1.391(5) . ? C33B H33B 0.9500 . ? C34A C35A 1.388(5) . ? C34A H34A 0.9500 . ? C34B C35B 1.380(5) . ? C34B H34B 0.9500 . ? C35A C36A 1.387(5) . ? C35A H35A 0.9500 . ? C35B C36B 1.382(5) . ? C35B H35B 0.9500 . ? C36A C37A 1.390(5) . ? C36A H36A 0.9500 . ? C36B C37B 1.390(5) . ? C36B H36B 0.9500 . ? C37A H37A 0.9500 . ? C37B H37B 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 C1A O1A H1OA 107(3) . . ? C8A N1A C10A 108.7(3) . . ? C8A N1A H1NA 121(2) . . ? C10A N1A H1NA 130(2) . . ? O1A C1A C6A 119.2(3) . . ? O1A C1A C2A 120.9(3) . . ? C6A C1A C2A 119.9(3) . . ? C1B O1B H1OB 108(3) . . ? C8B N1B C10B 107.2(3) . . ? O1B C1B C2B 118.9(3) . . ? O1B C1B C6B 121.2(3) . . ? C2B C1B C6B 119.9(3) . . ? C1TA O1TA C4TA 109.3(3) . . ? O1TA C1TA C2TA 105.6(3) . . ? O1TA C1TA H1TA 110.6 . . ? C2TA C1TA H1TA 110.6 . . ? O1TA C1TA H1TB 110.6 . . ? C2TA C1TA H1TB 110.6 . . ? H1TA C1TA H1TB 108.8 . . ? C1TB O1TB C4TB 109.8(3) . . ? O1TB C1TB C2TB 105.8(3) . . ? O1TB C1TB H1TC 110.6 . . ? C2TB C1TB H1TC 110.6 . . ? O1TB C1TB H1TD 110.6 . . ? C2TB C1TB H1TD 110.6 . . ? H1TC C1TB H1TD 108.7 . . ? C1TC O1TC C4TC 109.1(3) . . ? O1TC C1TC C2TC 107.2(4) . . ? O1TC C1TC H1TE 110.3 . . ? C2TC C1TC H1TE 110.3 . . ? O1TC C1TC H1TF 110.3 . . ? C2TC C1TC H1TF 110.3 . . ? H1TE C1TC H1TF 108.5 . . ? C4TD O1TD C1TD 106.0(3) . . ? O1TD C1TD C2TD 105.5(3) . . ? O1TD C1TD H1TG 110.6 . . ? C2TD C1TD H1TG 110.6 . . ? O1TD C1TD H1TH 110.6 . . ? C2TD C1TD H1TH 110.6 . . ? H1TG C1TD H1TH 108.8 . . ? C8A N2A C9A 105.2(3) . . ? C3A C2A C1A 119.0(3) . . ? C3A C2A C23A 122.1(3) . . ? C1A C2A C23A 118.9(3) . . ? C8B N2B C9B 108.3(3) . . ? C8B N2B H2NB 126(3) . . ? C9B N2B H2NB 126(3) . . ? C3B C2B C1B 118.6(3) . . ? C3B C2B C23B 119.2(3) . . ? C1B C2B C23B 122.2(3) . . ? C1TA C2TA C3TA 103.0(3) . . ? C1TA C2TA H2TA 111.2 . . ? C3TA C2TA H2TA 111.2 . . ? C1TA C2TA H2TB 111.2 . . ? C3TA C2TA H2TB 111.2 . . ? H2TA C2TA H2TB 109.1 . . ? C1TB C2TB C3TB 102.1(3) . . ? C1TB C2TB H2TC 111.3 . . ? C3TB C2TB H2TC 111.3 . . ? C1TB C2TB H2TD 111.3 . . ? C3TB C2TB H2TD 111.3 . . ? H2TC C2TB H2TD 109.2 . . ? C1TC C2TC C3TC 101.7(4) . . ? C1TC C2TC H2TE 111.4 . . ? C3TC C2TC H2TE 111.4 . . ? C1TC C2TC H2TF 111.4 . . ? C3TC C2TC H2TF 111.4 . . ? H2TE C2TC H2TF 109.3 . . ? C1TD C2TD C3TD 105.8(4) . . ? C1TD C2TD H2TG 110.6 . . ? C3TD C2TD H2TG 110.6 . . ? C1TD C2TD H2TH 110.6 . . ? C3TD C2TD H2TH 110.6 . . ? H2TG C2TD H2TH 108.7 . . ? C23A N3A C25A 107.2(3) . . ? C4A C3A C2A 122.0(3) . . ? C4A C3A H3AA 119.0 . . ? C2A C3A H3AA 119.0 . . ? C23B N3B C25B 108.4(3) . . ? C23B N3B H3NB 121(2) . . ? C25B N3B H3NB 130(3) . . ? C4B C3B C2B 122.5(3) . . ? C4B C3B H3BA 118.7 . . ? C2B C3B H3BA 118.7 . . ? C4TA C3TA C2TA 101.7(3) . . ? C4TA C3TA H3TA 111.4 . . ? C2TA C3TA H3TA 111.4 . . ? C4TA C3TA H3TB 111.4 . . ? C2TA C3TA H3TB 111.4 . . ? H3TA C3TA H3TB 109.3 . . ? C2TB C3TB C4TB 102.6(3) . . ? C2TB C3TB H3TC 111.2 . . ? C4TB C3TB H3TC 111.2 . . ? C2TB C3TB H3TD 111.2 . . ? C4TB C3TB H3TD 111.2 . . ? H3TC C3TB H3TD 109.2 . . ? C4TC C3TC C2TC 101.9(4) . . ? C4TC C3TC H3TE 111.4 . . ? C2TC C3TC H3TE 111.4 . . ? C4TC C3TC H3TF 111.4 . . ? C2TC C3TC H3TF 111.4 . . ? H3TE C3TC H3TF 109.2 . . ? C2TD C3TD C4TD 103.1(3) . . ? C2TD C3TD H3TG 111.1 . . ? C4TD C3TD H3TG 111.1 . . ? C2TD C3TD H3TH 111.1 . . ? C4TD C3TD H3TH 111.1 . . ? H3TG C3TD H3TH 109.1 . . ? C23A N4A C24A 108.0(3) . . ? C23A N4A H4NA 126(3) . . ? C24A N4A H4NA 126(3) . . ? C5A C4A C3A 117.8(3) . . ? C5A C4A C7A 121.4(3) . . ? C3A C4A C7A 120.7(3) . . ? C23B N4B C24B 105.5(3) . . ? C3B C4B C5B 118.1(3) . . ? C3B C4B C7B 121.5(3) . . ? C5B C4B C7B 120.4(3) . . ? O1TA C4TA C3TA 106.0(3) . . ? O1TA C4TA H4TA 110.5 . . ? C3TA C4TA H4TA 110.5 . . ? O1TA C4TA H4TB 110.5 . . ? C3TA C4TA H4TB 110.5 . . ? H4TA C4TA H4TB 108.7 . . ? O1TB C4TB C3TB 105.3(3) . . ? O1TB C4TB H4TC 110.7 . . ? C3TB C4TB H4TC 110.7 . . ? O1TB C4TB H4TD 110.7 . . ? C3TB C4TB H4TD 110.7 . . ? H4TC C4TB H4TD 108.8 . . ? O1TC C4TC C3TC 106.1(3) . . ? O1TC C4TC H4TE 110.5 . . ? C3TC C4TC H4TE 110.5 . . ? O1TC C4TC H4TF 110.5 . . ? C3TC C4TC H4TF 110.5 . . ? H4TE C4TC H4TF 108.7 . . ? O1TD C4TD C3TD 106.6(3) . . ? O1TD C4TD H4TG 110.4 . . ? C3TD C4TD H4TG 110.4 . . ? O1TD C4TD H4TH 110.4 . . ? C3TD C4TD H4TH 110.4 . . ? H4TG C4TD H4TH 108.6 . . ? C4A C5A C6A 122.3(3) . . ? C4A C5A H5AA 118.8 . . ? C6A C5A H5AA 118.9 . . ? C6B C5B C4B 121.7(3) . . ? C6B C5B H5BA 119.2 . . ? C4B C5B H5BA 119.2 . . ? C5A C6A C1A 119.0(3) . . ? C5A C6A C8A 119.7(3) . . ? C1A C6A C8A 121.3(3) . . ? C5B C6B C1B 119.2(3) . . ? C5B C6B C8B 121.5(3) . . ? C1B C6B C8B 119.3(3) . . ? C4A C7A H7AA 109.5 . . ? C4A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C4A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? C4B C7B H7BA 109.5 . . ? C4B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C4B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? N2A C8A N1A 111.1(3) . . ? N2A C8A C6A 125.4(3) . . ? N1A C8A C6A 123.4(3) . . ? N1B C8B N2B 110.6(3) . . ? N1B C8B C6B 123.3(3) . . ? N2B C8B C6B 126.1(3) . . ? C10A C9A N2A 110.6(3) . . ? C10A C9A C11A 129.8(3) . . ? N2A C9A C11A 119.6(3) . . ? N2B C9B C10B 105.9(3) . . ? N2B C9B C11B 118.8(3) . . ? C10B C9B C11B 135.4(3) . . ? N1A C10A C9A 104.5(3) . . ? N1A C10A C17A 120.3(3) . . ? C9A C10A C17A 135.3(3) . . ? C9B C10B N1B 108.0(3) . . ? C9B C10B C17B 133.2(3) . . ? N1B C10B C17B 118.4(3) . . ? C12A C11A C16A 119.0(3) . . ? C12A C11A C9A 119.7(3) . . ? C16A C11A C9A 121.3(3) . . ? C12B C11B C16B 118.8(3) . . ? C12B C11B C9B 119.7(3) . . ? C16B C11B C9B 121.5(3) . . ? C11A C12A C13A 120.5(3) . . ? C11A C12A H12A 119.8 . . ? C13A C12A H12A 119.8 . . ? C13B C12B C11B 120.7(3) . . ? C13B C12B H12B 119.6 . . ? C11B C12B H12B 119.6 . . ? C14A C13A C12A 120.1(3) . . ? C14A C13A H13A 119.9 . . ? C12A C13A H13A 119.9 . . ? C14B C13B C12B 119.8(3) . . ? C14B C13B H13B 120.1 . . ? C12B C13B H13B 120.1 . . ? C15A C14A C13A 119.5(3) . . ? C15A C14A H14A 120.2 . . ? C13A C14A H14A 120.2 . . ? C15B C14B C13B 120.1(3) . . ? C15B C14B H14B 119.9 . . ? C13B C14B H14B 119.9 . . ? C14A C15A C16A 120.5(3) . . ? C14A C15A H15A 119.7 . . ? C16A C15A H15A 119.7 . . ? C14B C15B C16B 120.4(3) . . ? C14B C15B H15B 119.8 . . ? C16B C15B H15B 119.8 . . ? C11A C16A C15A 120.3(3) . . ? C11A C16A H16A 119.8 . . ? C15A C16A H16A 119.8 . . ? C15B C16B C11B 120.2(3) . . ? C15B C16B H16B 119.9 . . ? C11B C16B H16B 119.9 . . ? C22A C17A C18A 118.3(3) . . ? C22A C17A C10A 120.5(3) . . ? C18A C17A C10A 121.2(3) . . ? C22B C17B C18B 117.4(3) . . ? C22B C17B C10B 118.6(3) . . ? C18B C17B C10B 124.1(3) . . ? C19A C18A C17A 119.9(3) . . ? C19A C18A H18A 120.1 . . ? C17A C18A H18A 120.1 . . ? C19B C18B C17B 120.9(3) . . ? C19B C18B H18B 119.6 . . ? C17B C18B H18B 119.6 . . ? C20A C19A C18A 121.0(3) . . ? C20A C19A H19A 119.5 . . ? C18A C19A H19A 119.5 . . ? C18B C19B C20B 121.4(3) . . ? C18B C19B H19B 119.3 . . ? C20B C19B H19B 119.3 . . ? C21A C20A C19A 119.7(3) . . ? C21A C20A H20A 120.2 . . ? C19A C20A H20A 120.2 . . ? C19B C20B C21B 118.2(3) . . ? C19B C20B H20B 120.9 . . ? C21B C20B H20B 120.9 . . ? C20A C21A C22A 119.9(3) . . ? C20A C21A H21A 120.1 . . ? C22A C21A H21A 120.1 . . ? C22B C21B C20B 120.6(3) . . ? C22B C21B H21B 119.7 . . ? C20B C21B H21B 119.7 . . ? C21A C22A C17A 121.2(3) . . ? C21A C22A H22A 119.4 . . ? C17A C22A H22A 119.4 . . ? C21B C22B C17B 121.5(3) . . ? C21B C22B H22B 119.2 . . ? C17B C22B H22B 119.2 . . ? N3A C23A N4A 110.4(3) . . ? N3A C23A C2A 122.6(3) . . ? N4A C23A C2A 126.9(3) . . ? N4B C23B N3B 111.0(3) . . ? N4B C23B C2B 124.2(3) . . ? N3B C23B C2B 124.7(3) . . ? N4A C24A C25A 106.0(3) . . ? N4A C24A C26A 121.8(3) . . ? C25A C24A C26A 132.0(3) . . ? N4B C24B C25B 110.3(3) . . ? N4B C24B C26B 118.8(3) . . ? C25B C24B C26B 130.9(3) . . ? N3A C25A C24A 108.4(3) . . ? N3A C25A C32A 119.9(3) . . ? C24A C25A C32A 131.6(3) . . ? N3B C25B C24B 104.7(3) . . ? N3B C25B C32B 120.8(3) . . ? C24B C25B C32B 134.5(3) . . ? C27A C26A C31A 119.0(3) . . ? C27A C26A C24A 121.2(3) . . ? C31A C26A C24A 119.8(3) . . ? C31B C26B C27B 118.8(3) . . ? C31B C26B C24B 118.5(3) . . ? C27B C26B C24B 122.7(3) . . ? C28A C27A C26A 120.3(3) . . ? C28A C27A H27A 119.8 . . ? C26A C27A H27A 119.8 . . ? C28B C27B C26B 120.2(3) . . ? C28B C27B H27B 119.9 . . ? C26B C27B H27B 119.9 . . ? C29A C28A C27A 120.6(3) . . ? C29A C28A H28A 119.7 . . ? C27A C28A H28A 119.7 . . ? C29B C28B C27B 120.5(3) . . ? C29B C28B H28B 119.8 . . ? C27B C28B H28B 119.8 . . ? C30A C29A C28A 119.2(3) . . ? C30A C29A H29A 120.4 . . ? C28A C29A H29A 120.4 . . ? C30B C29B C28B 119.5(3) . . ? C30B C29B H29B 120.3 . . ? C28B C29B H29B 120.3 . . ? C29A C30A C31A 120.9(3) . . ? C29A C30A H30A 119.5 . . ? C31A C30A H30A 119.5 . . ? C29B C30B C31B 120.3(3) . . ? C29B C30B H30B 119.9 . . ? C31B C30B H30B 119.9 . . ? C30A C31A C26A 119.8(3) . . ? C30A C31A H31A 120.1 . . ? C26A C31A H31A 120.1 . . ? C30B C31B C26B 120.8(3) . . ? C30B C31B H31B 119.6 . . ? C26B C31B H31B 119.6 . . ? C33A C32A C37A 118.8(3) . . ? C33A C32A C25A 120.0(3) . . ? C37A C32A C25A 121.2(3) . . ? C33B C32B C37B 118.7(3) . . ? C33B C32B C25B 120.2(3) . . ? C37B C32B C25B 121.1(3) . . ? C34A C33A C32A 120.6(3) . . ? C34A C33A H33A 119.7 . . ? C32A C33A H33A 119.7 . . ? C34B C33B C32B 120.7(3) . . ? C34B C33B H33B 119.6 . . ? C32B C33B H33B 119.6 . . ? C33A C34A C35A 120.4(3) . . ? C33A C34A H34A 119.8 . . ? C35A C34A H34A 119.8 . . ? C35B C34B C33B 120.2(3) . . ? C35B C34B H34B 119.9 . . ? C33B C34B H34B 119.9 . . ? C36A C35A C34A 119.4(3) . . ? C36A C35A H35A 120.3 . . ? C34A C35A H35A 120.3 . . ? C34B C35B C36B 119.5(3) . . ? C34B C35B H35B 120.3 . . ? C36B C35B H35B 120.3 . . ? C35A C36A C37A 120.6(3) . . ? C35A C36A H36A 119.7 . . ? C37A C36A H36A 119.7 . . ? C35B C36B C37B 120.9(3) . . ? C35B C36B H36B 119.5 . . ? C37B C36B H36B 119.5 . . ? C36A C37A C32A 120.2(3) . . ? C36A C37A H37A 119.9 . . ? C32A C37A H37A 119.9 . . ? C36B C37B C32B 120.0(3) . . ? C36B C37B H37B 120.0 . . ? C32B C37B H37B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.833 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.833 _refine_diff_density_max 0.277 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.063 # Attachment 'C-dp.cif' data_C-dp _database_code_depnum_ccdc_archive 'CCDC 839337' #TrackingRef 'C-dp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H28 N4 O' _chemical_formula_weight 544.63 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.181(3) _cell_length_b 12.540(3) _cell_length_c 16.598(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.48(3) _cell_angle_gamma 90.00 _cell_volume 2815.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Pale-yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _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 17473 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0747 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6444 _reflns_number_gt 4495 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0540P)^2^+3.1044P] 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_number_reflns 6444 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1759 _refine_ls_wR_factor_gt 0.1472 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _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 0.17754(13) 0.02830(14) 0.42208(11) 0.0191(4) Uani 1 1 d . . . N1 N 0.22431(16) 0.27964(17) 0.27369(14) 0.0181(5) Uani 1 1 d . . . C1 C 0.09917(17) 0.0592(2) 0.35544(15) 0.0156(5) Uani 1 1 d . . . N2 N 0.28642(15) 0.15972(17) 0.37321(14) 0.0195(5) Uani 1 1 d . . . C2 C 0.11003(18) 0.13736(19) 0.29832(16) 0.0163(5) Uani 1 1 d . . . N3 N -0.08885(15) -0.13324(16) 0.38524(13) 0.0172(5) Uani 1 1 d . . . C3 C 0.02921(18) 0.1635(2) 0.22939(16) 0.0171(5) Uani 1 1 d . . . N4 N 0.06113(16) -0.10565(17) 0.47180(13) 0.0166(4) Uani 1 1 d . . . C4 C -0.06279(17) 0.1153(2) 0.21615(16) 0.0165(5) Uani 1 1 d . . . C5 C -0.07251(18) 0.0407(2) 0.27498(16) 0.0170(5) Uani 1 1 d . . . C6 C 0.00640(18) 0.01093(19) 0.34418(16) 0.0159(5) Uani 1 1 d . . . C7 C -0.1480(2) 0.1421(3) 0.13989(19) 0.0249(6) Uani 1 1 d . . . C8 C 0.20557(18) 0.1902(2) 0.31305(16) 0.0172(5) Uani 1 1 d . . . C9 C 0.32178(18) 0.3078(2) 0.31209(17) 0.0189(5) Uani 1 1 d . . . C10 C 0.35970(18) 0.2321(2) 0.37309(16) 0.0180(5) Uani 1 1 d . . . C11 C 0.36437(18) 0.4081(2) 0.29062(17) 0.0199(6) Uani 1 1 d . . . C12 C 0.3859(3) 0.4213(3) 0.2152(2) 0.0354(7) Uani 1 1 d . . . C13 C 0.4292(3) 0.5153(3) 0.1991(2) 0.0395(8) Uani 1 1 d . . . C14 C 0.4516(2) 0.5959(2) 0.2588(2) 0.0333(7) Uani 1 1 d . . . C15 C 0.4296(2) 0.5842(2) 0.3339(2) 0.0292(7) Uani 1 1 d . . . C16 C 0.3855(2) 0.4908(2) 0.3494(2) 0.0262(6) Uani 1 1 d . . . C17 C 0.46031(18) 0.2193(2) 0.43217(17) 0.0188(5) Uani 1 1 d . . . C18 C 0.54102(18) 0.2772(2) 0.42437(18) 0.0219(6) Uani 1 1 d . . . C19 C 0.6347(2) 0.2610(2) 0.48013(19) 0.0241(6) Uani 1 1 d . . . C20 C 0.6501(2) 0.1850(2) 0.54297(19) 0.0265(6) Uani 1 1 d . . . C21 C 0.5710(2) 0.1273(2) 0.5526(2) 0.0295(7) Uani 1 1 d . . . C22 C 0.4766(2) 0.1445(2) 0.49750(19) 0.0257(6) Uani 1 1 d . . . C23 C -0.00786(17) -0.07356(19) 0.39990(16) 0.0152(5) Uani 1 1 d . . . C24 C 0.02412(18) -0.1904(2) 0.50624(16) 0.0169(5) Uani 1 1 d . . . C25 C -0.06951(18) -0.2067(2) 0.45051(16) 0.0166(5) Uani 1 1 d . . . C26 C 0.08195(18) -0.2442(2) 0.58357(16) 0.0176(5) Uani 1 1 d . . . C27 C 0.1827(2) -0.2241(2) 0.61929(17) 0.0222(6) Uani 1 1 d . . . C28 C 0.2376(2) -0.2789(2) 0.69082(18) 0.0263(6) Uani 1 1 d . . . C29 C 0.1934(2) -0.3551(2) 0.72747(18) 0.0261(6) Uani 1 1 d . . . C30 C 0.0926(2) -0.3733(2) 0.69404(18) 0.0245(6) Uani 1 1 d . . . C31 C 0.0370(2) -0.3186(2) 0.62373(17) 0.0210(6) Uani 1 1 d . . . C32 C -0.14379(18) -0.2904(2) 0.44902(16) 0.0182(5) Uani 1 1 d . . . C33 C -0.1225(2) -0.3983(2) 0.44310(18) 0.0219(6) Uani 1 1 d . . . C34 C -0.1945(2) -0.4746(2) 0.43832(18) 0.0260(6) Uani 1 1 d . . . C35 C -0.2881(2) -0.4450(2) 0.4388(2) 0.0288(7) Uani 1 1 d . . . C36 C -0.3098(2) -0.3380(3) 0.4455(2) 0.0311(7) Uani 1 1 d . . . C37 C -0.2381(2) -0.2611(2) 0.45067(18) 0.0237(6) Uani 1 1 d . . . HN4 H 0.122(2) -0.076(3) 0.492(2) 0.031(9) Uiso 1 1 d . . . H29 H 0.231(2) -0.401(2) 0.7735(19) 0.022(7) Uiso 1 1 d . . . H5 H -0.136(2) 0.007(2) 0.2662(18) 0.023(8) Uiso 1 1 d . . . H34 H -0.179(2) -0.550(3) 0.433(2) 0.036(9) Uiso 1 1 d . . . H31 H -0.035(2) -0.335(2) 0.5992(19) 0.025(8) Uiso 1 1 d . . . H28 H 0.307(2) -0.263(2) 0.7149(19) 0.023(8) Uiso 1 1 d . . . H27 H 0.217(2) -0.174(2) 0.5948(19) 0.023(8) Uiso 1 1 d . . . H7B H -0.164(3) 0.083(3) 0.099(2) 0.052(11) Uiso 1 1 d . . . H18 H 0.532(2) 0.329(3) 0.375(2) 0.030(8) Uiso 1 1 d . . . H15 H 0.445(2) 0.642(3) 0.378(2) 0.034(9) Uiso 1 1 d . . . H7A H -0.208(3) 0.154(3) 0.157(2) 0.042(10) Uiso 1 1 d . . . H3 H 0.037(2) 0.218(2) 0.1909(19) 0.022(8) Uiso 1 1 d . . . H33 H -0.057(2) -0.421(3) 0.441(2) 0.035(9) Uiso 1 1 d . . . H35 H -0.340(2) -0.500(3) 0.4359(19) 0.030(8) Uiso 1 1 d . . . H14 H 0.484(2) 0.663(3) 0.2500(19) 0.026(8) Uiso 1 1 d . . . H19 H 0.692(2) 0.306(3) 0.475(2) 0.036(9) Uiso 1 1 d . . . H36 H -0.377(2) -0.317(3) 0.443(2) 0.036(9) Uiso 1 1 d . . . H30 H 0.062(2) -0.427(3) 0.719(2) 0.031(9) Uiso 1 1 d . . . H16 H 0.368(2) 0.480(3) 0.405(2) 0.038(9) Uiso 1 1 d . . . H37 H -0.254(2) -0.186(3) 0.4581(19) 0.028(8) Uiso 1 1 d . . . H20 H 0.713(2) 0.175(3) 0.583(2) 0.038(9) Uiso 1 1 d . . . HN1 H 0.182(2) 0.314(3) 0.230(2) 0.035(9) Uiso 1 1 d . . . H22 H 0.417(2) 0.106(3) 0.504(2) 0.036(9) Uiso 1 1 d . . . H13 H 0.447(3) 0.526(3) 0.147(3) 0.064(12) Uiso 1 1 d . . . H1O H 0.238(3) 0.070(4) 0.415(3) 0.075(14) Uiso 1 1 d . . . H7C H -0.134(3) 0.205(3) 0.112(2) 0.055(11) Uiso 1 1 d . . . H21 H 0.584(2) 0.074(3) 0.602(2) 0.037(9) Uiso 1 1 d . . . H12 H 0.372(2) 0.361(3) 0.175(2) 0.041(10) Uiso 1 1 d . . . 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 0.0170(8) 0.0186(9) 0.0189(9) 0.0055(8) 0.0011(7) -0.0029(8) N1 0.0166(10) 0.0164(11) 0.0198(11) 0.0031(9) 0.0034(9) -0.0011(9) C1 0.0148(11) 0.0166(12) 0.0133(12) -0.0009(10) 0.0012(9) 0.0031(10) N2 0.0165(10) 0.0194(11) 0.0214(12) 0.0016(9) 0.0039(9) -0.0028(9) C2 0.0166(12) 0.0142(12) 0.0182(13) -0.0016(10) 0.0052(10) -0.0009(10) N3 0.0186(10) 0.0148(10) 0.0186(11) -0.0004(9) 0.0063(9) -0.0008(9) C3 0.0191(12) 0.0155(12) 0.0171(13) 0.0012(10) 0.0058(10) 0.0014(10) N4 0.0160(10) 0.0157(10) 0.0170(11) -0.0001(9) 0.0031(9) -0.0008(9) C4 0.0144(11) 0.0162(12) 0.0173(12) -0.0011(10) 0.0023(10) 0.0031(10) C5 0.0163(12) 0.0163(12) 0.0180(13) -0.0037(10) 0.0043(10) 0.0004(10) C6 0.0183(12) 0.0137(12) 0.0162(12) -0.0032(10) 0.0059(10) -0.0016(10) C7 0.0184(13) 0.0289(15) 0.0224(15) 0.0038(13) -0.0014(11) -0.0009(12) C8 0.0180(12) 0.0166(12) 0.0164(13) 0.0018(10) 0.0043(10) -0.0005(10) C9 0.0174(12) 0.0192(13) 0.0200(13) 0.0014(11) 0.0058(10) -0.0028(11) C10 0.0175(12) 0.0159(12) 0.0207(13) 0.0009(10) 0.0058(10) -0.0014(10) C11 0.0133(11) 0.0191(13) 0.0247(14) 0.0068(11) 0.0016(10) 0.0000(10) C12 0.050(2) 0.0294(16) 0.0280(16) 0.0007(14) 0.0129(15) -0.0099(15) C13 0.050(2) 0.0364(18) 0.0371(19) 0.0076(15) 0.0199(16) -0.0099(16) C14 0.0287(15) 0.0186(14) 0.052(2) 0.0081(14) 0.0118(14) -0.0037(13) C15 0.0271(15) 0.0211(14) 0.0398(18) -0.0011(13) 0.0104(13) -0.0031(12) C16 0.0237(13) 0.0221(14) 0.0342(17) -0.0009(12) 0.0109(12) -0.0017(12) C17 0.0181(12) 0.0162(12) 0.0215(13) -0.0024(11) 0.0049(10) 0.0011(10) C18 0.0152(12) 0.0245(14) 0.0245(14) 0.0016(12) 0.0037(10) -0.0009(11) C19 0.0207(13) 0.0208(13) 0.0294(15) -0.0019(12) 0.0055(11) -0.0038(12) C20 0.0178(13) 0.0269(15) 0.0293(16) -0.0015(12) -0.0014(12) -0.0016(12) C21 0.0247(14) 0.0254(15) 0.0316(17) 0.0072(13) -0.0019(12) -0.0003(12) C22 0.0216(13) 0.0226(14) 0.0295(15) 0.0052(12) 0.0026(12) -0.0029(12) C23 0.0156(11) 0.0157(12) 0.0152(12) -0.0027(10) 0.0059(10) 0.0000(10) C24 0.0182(12) 0.0157(12) 0.0177(13) -0.0008(10) 0.0068(10) -0.0014(10) C25 0.0207(12) 0.0153(12) 0.0147(12) -0.0009(10) 0.0067(10) -0.0001(10) C26 0.0209(12) 0.0171(12) 0.0138(12) -0.0009(10) 0.0040(10) 0.0018(10) C27 0.0236(13) 0.0217(13) 0.0202(14) -0.0010(11) 0.0051(11) -0.0022(12) C28 0.0218(13) 0.0276(15) 0.0244(15) -0.0008(12) -0.0009(11) -0.0026(12) C29 0.0299(15) 0.0245(14) 0.0197(14) 0.0048(12) 0.0009(12) 0.0042(13) C30 0.0347(15) 0.0211(14) 0.0188(14) 0.0027(11) 0.0098(12) -0.0012(12) C31 0.0230(13) 0.0237(13) 0.0175(13) -0.0013(11) 0.0080(11) -0.0025(11) C32 0.0186(12) 0.0197(13) 0.0161(13) -0.0015(10) 0.0051(10) -0.0053(11) C33 0.0222(13) 0.0185(13) 0.0257(14) -0.0013(11) 0.0082(11) -0.0023(11) C34 0.0379(16) 0.0167(13) 0.0250(15) -0.0031(11) 0.0119(13) -0.0047(13) C35 0.0282(15) 0.0256(15) 0.0334(17) -0.0025(13) 0.0107(13) -0.0133(13) C36 0.0218(14) 0.0299(16) 0.0426(19) -0.0045(14) 0.0111(13) -0.0048(13) C37 0.0229(13) 0.0215(14) 0.0273(15) -0.0017(12) 0.0084(11) -0.0008(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 O1 C1 1.368(3) . ? O1 H1O 1.04(5) . ? N1 C8 1.364(3) . ? N1 C9 1.383(3) . ? N1 HN1 0.90(3) . ? C1 C2 1.404(4) . ? C1 C6 1.409(3) . ? N2 C8 1.330(3) . ? N2 C10 1.380(3) . ? C2 C3 1.393(4) . ? C2 C8 1.461(3) . ? N3 C23 1.331(3) . ? N3 C25 1.385(3) . ? C3 C4 1.394(3) . ? C3 H3 0.96(3) . ? N4 C23 1.357(3) . ? N4 C24 1.383(3) . ? N4 HN4 0.91(3) . ? C4 C5 1.389(4) . ? C4 C7 1.502(4) . ? C5 C6 1.392(3) . ? C5 H5 0.97(3) . ? C6 C23 1.460(3) . ? C7 H7B 0.98(4) . ? C7 H7A 0.99(4) . ? C7 H7C 0.96(4) . ? C9 C10 1.374(4) . ? C9 C11 1.484(4) . ? C10 C17 1.477(4) . ? C11 C12 1.386(4) . ? C11 C16 1.394(4) . ? C12 C13 1.391(4) . ? C12 H12 0.99(4) . ? C13 C14 1.383(5) . ? C13 H13 0.99(4) . ? C14 C15 1.381(5) . ? C14 H14 0.99(3) . ? C15 C16 1.388(4) . ? C15 H15 1.01(3) . ? C16 H16 1.04(3) . ? C17 C18 1.394(4) . ? C17 C22 1.399(4) . ? C18 C19 1.387(4) . ? C18 H18 1.02(3) . ? C19 C20 1.381(4) . ? C19 H19 1.01(3) . ? C20 C21 1.384(4) . ? C20 H20 0.94(3) . ? C21 C22 1.392(4) . ? C21 H21 1.03(3) . ? C22 H22 1.01(3) . ? C24 C25 1.386(3) . ? C24 C26 1.464(4) . ? C25 C32 1.482(3) . ? C26 C27 1.395(4) . ? C26 C31 1.406(4) . ? C27 C28 1.390(4) . ? C27 H27 0.95(3) . ? C28 C29 1.381(4) . ? C28 H28 0.96(3) . ? C29 C30 1.388(4) . ? C29 H29 0.98(3) . ? C30 C31 1.379(4) . ? C30 H30 0.96(3) . ? C31 H31 1.01(3) . ? C32 C37 1.395(4) . ? C32 C33 1.396(4) . ? C33 C34 1.384(4) . ? C33 H33 0.99(3) . ? C34 C35 1.380(4) . ? C34 H34 0.98(3) . ? C35 C36 1.389(4) . ? C35 H35 0.99(3) . ? C36 C37 1.385(4) . ? C36 H36 0.98(3) . ? C37 H37 0.98(3) . ? 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 C1 O1 H1O 105(2) . . ? C8 N1 C9 107.5(2) . . ? C8 N1 HN1 127(2) . . ? C9 N1 HN1 125(2) . . ? O1 C1 C2 121.1(2) . . ? O1 C1 C6 119.0(2) . . ? C2 C1 C6 119.9(2) . . ? C8 N2 C10 106.8(2) . . ? C3 C2 C1 119.2(2) . . ? C3 C2 C8 121.6(2) . . ? C1 C2 C8 119.2(2) . . ? C23 N3 C25 105.9(2) . . ? C2 C3 C4 121.9(2) . . ? C2 C3 H3 118.9(17) . . ? C4 C3 H3 119.2(17) . . ? C23 N4 C24 109.2(2) . . ? C23 N4 HN4 124(2) . . ? C24 N4 HN4 127(2) . . ? C5 C4 C3 117.8(2) . . ? C5 C4 C7 121.3(2) . . ? C3 C4 C7 120.9(2) . . ? C4 C5 C6 122.4(2) . . ? C4 C5 H5 118.1(17) . . ? C6 C5 H5 119.5(18) . . ? C5 C6 C1 118.8(2) . . ? C5 C6 C23 119.1(2) . . ? C1 C6 C23 122.0(2) . . ? C4 C7 H7B 112(2) . . ? C4 C7 H7A 110(2) . . ? H7B C7 H7A 105(3) . . ? C4 C7 H7C 111(2) . . ? H7B C7 H7C 109(3) . . ? H7A C7 H7C 110(3) . . ? N2 C8 N1 110.3(2) . . ? N2 C8 C2 122.9(2) . . ? N1 C8 C2 126.6(2) . . ? C10 C9 N1 106.2(2) . . ? C10 C9 C11 131.7(2) . . ? N1 C9 C11 121.9(2) . . ? C9 C10 N2 109.1(2) . . ? C9 C10 C17 130.6(2) . . ? N2 C10 C17 120.3(2) . . ? C12 C11 C16 118.9(3) . . ? C12 C11 C9 122.3(3) . . ? C16 C11 C9 118.7(3) . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12 117(2) . . ? C13 C12 H12 122(2) . . ? C14 C13 C12 120.2(3) . . ? C14 C13 H13 118(2) . . ? C12 C13 H13 122(2) . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 117.4(18) . . ? C13 C14 H14 122.4(18) . . ? C14 C15 C16 119.6(3) . . ? C14 C15 H15 121.9(19) . . ? C16 C15 H15 118.5(19) . . ? C15 C16 C11 120.8(3) . . ? C15 C16 H16 120.9(19) . . ? C11 C16 H16 118.3(19) . . ? C18 C17 C22 118.1(2) . . ? C18 C17 C10 122.5(2) . . ? C22 C17 C10 119.3(2) . . ? C19 C18 C17 120.7(3) . . ? C19 C18 H18 119.2(17) . . ? C17 C18 H18 120.0(17) . . ? C20 C19 C18 120.4(3) . . ? C20 C19 H19 119.8(19) . . ? C18 C19 H19 119.8(19) . . ? C19 C20 C21 119.9(3) . . ? C19 C20 H20 122(2) . . ? C21 C20 H20 118(2) . . ? C20 C21 C22 119.7(3) . . ? C20 C21 H21 118.1(18) . . ? C22 C21 H21 122.2(18) . . ? C21 C22 C17 121.0(3) . . ? C21 C22 H22 121.7(19) . . ? C17 C22 H22 117.2(19) . . ? N3 C23 N4 110.4(2) . . ? N3 C23 C6 124.6(2) . . ? N4 C23 C6 124.9(2) . . ? N4 C24 C25 104.1(2) . . ? N4 C24 C26 122.3(2) . . ? C25 C24 C26 133.6(2) . . ? N3 C25 C24 110.4(2) . . ? N3 C25 C32 119.0(2) . . ? C24 C25 C32 130.5(2) . . ? C27 C26 C31 118.1(2) . . ? C27 C26 C24 121.5(2) . . ? C31 C26 C24 120.4(2) . . ? C28 C27 C26 120.9(3) . . ? C28 C27 H27 117.5(18) . . ? C26 C27 H27 121.6(18) . . ? C29 C28 C27 120.4(3) . . ? C29 C28 H28 119.9(18) . . ? C27 C28 H28 119.7(18) . . ? C28 C29 C30 119.1(3) . . ? C28 C29 H29 122.4(17) . . ? C30 C29 H29 118.3(17) . . ? C31 C30 C29 121.1(3) . . ? C31 C30 H30 119.7(19) . . ? C29 C30 H30 119.2(19) . . ? C30 C31 C26 120.3(3) . . ? C30 C31 H31 119.7(18) . . ? C26 C31 H31 119.9(18) . . ? C37 C32 C33 119.1(2) . . ? C37 C32 C25 119.6(2) . . ? C33 C32 C25 121.3(2) . . ? C34 C33 C32 120.2(3) . . ? C34 C33 H33 119.5(19) . . ? C32 C33 H33 120.4(19) . . ? C35 C34 C33 120.5(3) . . ? C35 C34 H34 120.3(19) . . ? C33 C34 H34 119.1(19) . . ? C34 C35 C36 119.8(3) . . ? C34 C35 H35 120.5(18) . . ? C36 C35 H35 119.7(18) . . ? C37 C36 C35 120.1(3) . . ? C37 C36 H36 121(2) . . ? C35 C36 H36 119(2) . . ? C36 C37 C32 120.4(3) . . ? C36 C37 H37 118.9(18) . . ? C32 C37 H37 120.6(18) . . ? 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 O1 C1 C2 C3 177.5(2) . . . . ? C6 C1 C2 C3 -2.2(4) . . . . ? O1 C1 C2 C8 -3.1(4) . . . . ? C6 C1 C2 C8 177.2(2) . . . . ? C1 C2 C3 C4 1.0(4) . . . . ? C8 C2 C3 C4 -178.4(2) . . . . ? C2 C3 C4 C5 1.0(4) . . . . ? C2 C3 C4 C7 -178.0(3) . . . . ? C3 C4 C5 C6 -1.9(4) . . . . ? C7 C4 C5 C6 177.1(3) . . . . ? C4 C5 C6 C1 0.7(4) . . . . ? C4 C5 C6 C23 -175.7(2) . . . . ? O1 C1 C6 C5 -178.3(2) . . . . ? C2 C1 C6 C5 1.3(4) . . . . ? O1 C1 C6 C23 -2.0(4) . . . . ? C2 C1 C6 C23 177.6(2) . . . . ? C10 N2 C8 N1 0.3(3) . . . . ? C10 N2 C8 C2 -175.2(2) . . . . ? C9 N1 C8 N2 -0.9(3) . . . . ? C9 N1 C8 C2 174.4(2) . . . . ? C3 C2 C8 N2 -173.1(2) . . . . ? C1 C2 C8 N2 7.5(4) . . . . ? C3 C2 C8 N1 12.1(4) . . . . ? C1 C2 C8 N1 -167.3(2) . . . . ? C8 N1 C9 C10 1.2(3) . . . . ? C8 N1 C9 C11 -173.8(2) . . . . ? N1 C9 C10 N2 -1.0(3) . . . . ? C11 C9 C10 N2 173.2(3) . . . . ? N1 C9 C10 C17 178.1(3) . . . . ? C11 C9 C10 C17 -7.7(5) . . . . ? C8 N2 C10 C9 0.4(3) . . . . ? C8 N2 C10 C17 -178.8(2) . . . . ? C10 C9 C11 C12 113.3(4) . . . . ? N1 C9 C11 C12 -73.2(4) . . . . ? C10 C9 C11 C16 -65.2(4) . . . . ? N1 C9 C11 C16 108.3(3) . . . . ? C16 C11 C12 C13 0.9(5) . . . . ? C9 C11 C12 C13 -177.6(3) . . . . ? C11 C12 C13 C14 0.4(5) . . . . ? C12 C13 C14 C15 -1.1(5) . . . . ? C13 C14 C15 C16 0.5(5) . . . . ? C14 C15 C16 C11 0.8(4) . . . . ? C12 C11 C16 C15 -1.5(4) . . . . ? C9 C11 C16 C15 177.0(3) . . . . ? C9 C10 C17 C18 -11.4(4) . . . . ? N2 C10 C17 C18 167.6(3) . . . . ? C9 C10 C17 C22 170.2(3) . . . . ? N2 C10 C17 C22 -10.8(4) . . . . ? C22 C17 C18 C19 -0.2(4) . . . . ? C10 C17 C18 C19 -178.6(3) . . . . ? C17 C18 C19 C20 1.8(4) . . . . ? C18 C19 C20 C21 -2.5(5) . . . . ? C19 C20 C21 C22 1.5(5) . . . . ? C20 C21 C22 C17 0.1(5) . . . . ? C18 C17 C22 C21 -0.8(4) . . . . ? C10 C17 C22 C21 177.7(3) . . . . ? C25 N3 C23 N4 -0.5(3) . . . . ? C25 N3 C23 C6 176.7(2) . . . . ? C24 N4 C23 N3 0.0(3) . . . . ? C24 N4 C23 C6 -177.1(2) . . . . ? C5 C6 C23 N3 7.2(4) . . . . ? C1 C6 C23 N3 -169.1(2) . . . . ? C5 C6 C23 N4 -176.1(2) . . . . ? C1 C6 C23 N4 7.6(4) . . . . ? C23 N4 C24 C25 0.5(3) . . . . ? C23 N4 C24 C26 178.9(2) . . . . ? C23 N3 C25 C24 0.8(3) . . . . ? C23 N3 C25 C32 -175.8(2) . . . . ? N4 C24 C25 N3 -0.8(3) . . . . ? C26 C24 C25 N3 -178.9(3) . . . . ? N4 C24 C25 C32 175.3(2) . . . . ? C26 C24 C25 C32 -2.8(5) . . . . ? N4 C24 C26 C27 -10.4(4) . . . . ? C25 C24 C26 C27 167.5(3) . . . . ? N4 C24 C26 C31 170.0(2) . . . . ? C25 C24 C26 C31 -12.1(4) . . . . ? C31 C26 C27 C28 2.2(4) . . . . ? C24 C26 C27 C28 -177.4(3) . . . . ? C26 C27 C28 C29 0.6(4) . . . . ? C27 C28 C29 C30 -2.7(4) . . . . ? C28 C29 C30 C31 1.8(4) . . . . ? C29 C30 C31 C26 1.1(4) . . . . ? C27 C26 C31 C30 -3.1(4) . . . . ? C24 C26 C31 C30 176.6(2) . . . . ? N3 C25 C32 C37 -61.3(3) . . . . ? C24 C25 C32 C37 122.9(3) . . . . ? N3 C25 C32 C33 116.5(3) . . . . ? C24 C25 C32 C33 -59.3(4) . . . . ? C37 C32 C33 C34 0.5(4) . . . . ? C25 C32 C33 C34 -177.3(3) . . . . ? C32 C33 C34 C35 0.4(4) . . . . ? C33 C34 C35 C36 -1.0(5) . . . . ? C34 C35 C36 C37 0.7(5) . . . . ? C35 C36 C37 C32 0.2(5) . . . . ? C33 C32 C37 C36 -0.8(4) . . . . ? C25 C32 C37 C36 177.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.288 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.074