data_dt0985rm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H92 N4 O8' _chemical_formula_weight 1333.66 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' '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'MONOCLINIC' _symmetry_space_group_name_H-M 'P 2(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 11.2369(9) _cell_length_b 8.9082(7) _cell_length_c 19.2612(17) _cell_angle_alpha 90.00 _cell_angle_beta 106.6240(10) _cell_angle_gamma 90.00 _cell_volume 1847.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'BRUKER SMART CCD AREA DETECTOR' _diffrn_measurement_method 'PHI-OMEGA' _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <10 _diffrn_reflns_number 6990 _diffrn_reflns_av_R_equivalents 0.0155 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2420 _reflns_number_gt 2205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SMART 3' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON; 'MERCURY 1.2' _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^)+(0.0538P)^2^+0.3028P] 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 2420 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 N1 N 0.07026(9) 0.43639(12) 0.22516(5) 0.0237(3) Uani 1 1 d . . . O1 O 0.05824(8) 0.95237(9) 0.18169(4) 0.0300(2) Uani 1 1 d . . . O2 O 0.14243(8) 0.73210(10) 0.22535(5) 0.0321(3) Uani 1 1 d . . . C1 C 0.12212(11) 0.83625(13) 0.17953(6) 0.0248(3) Uani 1 1 d . . . C2 C 0.17857(11) 0.82801(13) 0.11776(6) 0.0246(3) Uani 1 1 d . . . C3 C 0.27164(12) 0.72611(17) 0.11801(8) 0.0357(3) Uani 1 1 d . . . C4 C 0.32591(13) 0.72606(18) 0.06208(8) 0.0413(4) Uani 1 1 d . . . C5 C 0.28876(12) 0.82635(16) 0.00509(7) 0.0340(4) Uani 1 1 d . . . C6 C 0.19208(13) 0.92423(15) 0.00369(7) 0.0330(3) Uani 1 1 d . . . C7 C 0.13894(12) 0.92622(14) 0.05973(7) 0.0290(3) Uani 1 1 d . . . C8 C 0.35226(16) 0.8333(2) -0.05355(9) 0.0478(4) Uani 1 1 d . . . C9 C 0.28114(12) 0.21522(14) 0.18443(7) 0.0268(3) Uani 1 1 d . . . C10 C 0.38033(12) 0.20607(15) 0.15578(7) 0.0305(3) Uani 1 1 d . . . C11 C 0.47973(12) 0.30303(16) 0.17927(7) 0.0323(3) Uani 1 1 d . . . C12 C 0.48007(13) 0.41010(16) 0.23083(7) 0.0351(4) Uani 1 1 d . . . C13 C 0.38073(12) 0.42041(15) 0.25919(7) 0.0309(3) Uani 1 1 d . . . C14 C 0.28005(11) 0.32330(13) 0.23622(6) 0.0237(3) Uani 1 1 d . . . C15 C 0.17200(12) 0.33384(15) 0.26693(7) 0.0269(3) Uani 1 1 d . . . C16 C 0.00137(12) 0.37986(16) 0.15141(7) 0.0288(3) Uani 1 1 d . . . C17 C -0.10271(11) 0.48476(14) 0.11414(6) 0.0266(3) Uani 1 1 d . . . C18 C -0.21325(11) 0.48648(15) 0.13278(7) 0.0304(3) Uani 1 1 d . . . C19 C -0.30903(13) 0.58231(16) 0.09762(8) 0.0379(4) Uani 1 1 d . . . C20 C -0.29569(14) 0.67603(17) 0.04332(8) 0.0416(4) Uani 1 1 d . . . C21 C -0.18614(14) 0.67570(16) 0.02469(8) 0.0388(4) Uani 1 1 d . . . C22 C -0.09003(13) 0.58155(15) 0.06041(7) 0.0319(3) Uani 1 1 d . . . H1N1 H 0.1022(12) 0.5332(17) 0.2216(7) 0.030(3) Uiso 1 1 d . . . H1N2 H 0.0116(13) 0.4461(15) 0.2567(8) 0.038(4) Uiso 1 1 d . . . H3 H 0.2988(13) 0.6543(18) 0.1573(8) 0.044(4) Uiso 1 1 d . . . H4 H 0.3901(14) 0.6580(19) 0.0641(8) 0.052(5) Uiso 1 1 d . . . H6 H 0.1610(13) 0.9927(17) -0.0373(8) 0.044(4) Uiso 1 1 d . . . H7 H 0.0750(12) 0.9970(16) 0.0597(7) 0.032(4) Uiso 1 1 d . . . H8A H 0.2924(15) 0.8348(18) -0.1032(10) 0.058(5) Uiso 1 1 d . . . H8C H 0.4066(16) 0.741(2) -0.0516(9) 0.063(5) Uiso 1 1 d . . . H9 H 0.2143(12) 0.1467(16) 0.1697(7) 0.027(3) Uiso 1 1 d . . . H10 H 0.3798(11) 0.1315(16) 0.1202(7) 0.032(3) Uiso 1 1 d . . . H11 H 0.5498(13) 0.2932(16) 0.1605(8) 0.039(4) Uiso 1 1 d . . . H12 H 0.5518(14) 0.4774(18) 0.2485(8) 0.043(4) Uiso 1 1 d . . . H13 H 0.3814(12) 0.4973(16) 0.2950(8) 0.035(4) Uiso 1 1 d . . . H15A H 0.1988(11) 0.3751(15) 0.3166(8) 0.028(3) Uiso 1 1 d . . . H15B H 0.1322(12) 0.2372(16) 0.2671(7) 0.028(3) Uiso 1 1 d . . . H16A H 0.0620(12) 0.3717(14) 0.1244(7) 0.027(3) Uiso 1 1 d . . . H16B H -0.0303(12) 0.2807(17) 0.1583(7) 0.032(4) Uiso 1 1 d . . . H18 H -0.2218(12) 0.4173(16) 0.1712(8) 0.033(4) Uiso 1 1 d . . . H19 H -0.3854(14) 0.5851(16) 0.1110(8) 0.044(4) Uiso 1 1 d . . . H20 H -0.3606(14) 0.7405(18) 0.0191(8) 0.044(4) Uiso 1 1 d . . . H21 H -0.1761(13) 0.7422(18) -0.0125(9) 0.045(4) Uiso 1 1 d . . . H22 H -0.0133(13) 0.5818(15) 0.0490(7) 0.036(4) Uiso 1 1 d . . . H8B H 0.4039(17) 0.925(2) -0.0486(10) 0.070(5) 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 N1 0.0249(6) 0.0233(6) 0.0258(6) 0.0001(4) 0.0119(5) 0.0003(5) O1 0.0344(5) 0.0278(5) 0.0342(5) 0.0022(4) 0.0200(4) 0.0022(4) O2 0.0426(6) 0.0259(5) 0.0301(5) 0.0012(4) 0.0142(4) -0.0033(4) C1 0.0261(7) 0.0217(7) 0.0271(7) -0.0017(6) 0.0085(5) -0.0057(5) C2 0.0232(7) 0.0244(7) 0.0270(7) -0.0056(5) 0.0085(5) -0.0055(5) C3 0.0352(8) 0.0400(8) 0.0329(7) 0.0006(7) 0.0114(6) 0.0074(7) C4 0.0313(8) 0.0542(10) 0.0412(8) -0.0091(7) 0.0151(6) 0.0103(7) C5 0.0313(7) 0.0431(9) 0.0312(7) -0.0140(6) 0.0144(6) -0.0107(6) C6 0.0426(8) 0.0325(8) 0.0276(7) -0.0032(6) 0.0160(6) -0.0041(6) C7 0.0317(8) 0.0274(7) 0.0308(7) -0.0026(6) 0.0134(6) 0.0013(6) C8 0.0468(10) 0.0633(12) 0.0428(10) -0.0177(8) 0.0282(8) -0.0138(9) C9 0.0268(7) 0.0234(7) 0.0300(7) 0.0013(6) 0.0081(6) 0.0017(6) C10 0.0354(8) 0.0313(8) 0.0260(7) -0.0022(6) 0.0108(6) 0.0073(6) C11 0.0285(7) 0.0416(8) 0.0314(7) 0.0025(6) 0.0159(6) 0.0052(6) C12 0.0276(7) 0.0417(9) 0.0380(8) -0.0060(7) 0.0126(6) -0.0056(7) C13 0.0313(8) 0.0341(8) 0.0288(7) -0.0071(6) 0.0110(6) -0.0009(6) C14 0.0253(7) 0.0251(7) 0.0213(6) 0.0055(5) 0.0078(5) 0.0046(5) C15 0.0288(7) 0.0280(8) 0.0264(7) 0.0042(6) 0.0120(6) 0.0026(6) C16 0.0295(7) 0.0290(8) 0.0289(7) -0.0040(6) 0.0099(6) 0.0010(6) C17 0.0290(7) 0.0255(7) 0.0243(6) -0.0061(5) 0.0062(5) -0.0011(5) C18 0.0300(7) 0.0311(7) 0.0293(7) -0.0018(6) 0.0072(6) -0.0016(6) C19 0.0271(8) 0.0451(9) 0.0393(8) -0.0032(7) 0.0060(6) 0.0038(6) C20 0.0390(9) 0.0381(9) 0.0394(8) 0.0014(7) -0.0018(7) 0.0100(7) C21 0.0496(9) 0.0334(8) 0.0311(8) 0.0033(7) 0.0080(7) 0.0010(7) C22 0.0351(8) 0.0328(8) 0.0286(7) -0.0044(6) 0.0104(6) -0.0025(6) _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 N1 C16 1.4972(16) . ? N1 C15 1.5042(16) . ? N1 H1N1 0.944(15) . ? N1 H1N2 1.019(15) . ? O1 C1 1.2665(15) . ? O2 O2 0.000(2) 1 ? O2 C1 1.2557(15) . ? C1 O2 1.2557(15) 1 ? C1 C2 1.5017(17) . ? C2 C3 1.3839(19) . ? C2 C7 1.3886(18) . ? C3 C4 1.381(2) . ? C3 H3 0.971(16) . ? C4 C5 1.384(2) . ? C4 H4 0.935(17) . ? C5 C6 1.387(2) . ? C5 C8 1.4999(19) . ? C6 C7 1.3751(19) . ? C6 H6 0.980(16) . ? C7 H7 0.955(14) . ? C8 H8A 0.999(18) . ? C8 H8C 1.021(19) . ? C8 H8B 0.991(19) . ? C9 C10 1.3803(18) . ? C9 C14 1.3890(18) . ? C9 H9 0.947(14) . ? C10 C11 1.382(2) . ? C10 H10 0.953(14) . ? C11 C12 1.3763(19) . ? C11 H11 0.961(15) . ? C12 C13 1.3790(19) . ? C12 H12 0.984(16) . ? C13 C14 1.3920(18) . ? C13 H13 0.971(15) . ? C14 C15 1.4979(17) . ? C15 H15A 0.987(14) . ? C15 H15B 0.970(14) . ? C16 C17 1.5086(18) . ? C16 H16A 0.972(13) . ? C16 H16B 0.976(15) . ? C17 C22 1.3854(19) . ? C17 C18 1.3882(18) . ? C18 C19 1.3887(19) . ? C18 H18 0.989(15) . ? C19 C20 1.380(2) . ? C19 H19 0.963(15) . ? C20 C21 1.377(2) . ? C20 H20 0.940(16) . ? C21 C22 1.385(2) . ? C21 H21 0.961(16) . ? C22 H22 0.949(14) . ? 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 C16 N1 C15 114.25(10) . . ? C16 N1 H1N1 110.0(8) . . ? C15 N1 H1N1 110.3(8) . . ? C16 N1 H1N2 110.3(8) . . ? C15 N1 H1N2 104.8(8) . . ? H1N1 N1 H1N2 106.9(11) . . ? O2 O2 C1 0(10) 1 . ? O2 C1 O2 0.00(10) 1 . ? O2 C1 O1 124.83(11) 1 . ? O2 C1 O1 124.83(11) . . ? O2 C1 C2 119.19(11) 1 . ? O2 C1 C2 119.19(11) . . ? O1 C1 C2 115.96(10) . . ? C3 C2 C7 118.95(12) . . ? C3 C2 C1 121.30(12) . . ? C7 C2 C1 119.73(11) . . ? C4 C3 C2 119.96(14) . . ? C4 C3 H3 119.8(9) . . ? C2 C3 H3 120.3(9) . . ? C3 C4 C5 121.21(13) . . ? C3 C4 H4 118.4(10) . . ? C5 C4 H4 120.3(10) . . ? C4 C5 C6 118.55(12) . . ? C4 C5 C8 121.56(14) . . ? C6 C5 C8 119.88(14) . . ? C7 C6 C5 120.43(13) . . ? C7 C6 H6 119.4(8) . . ? C5 C6 H6 120.2(8) . . ? C6 C7 C2 120.82(12) . . ? C6 C7 H7 120.2(8) . . ? C2 C7 H7 119.0(8) . . ? C5 C8 H8A 112.7(9) . . ? C5 C8 H8C 110.4(10) . . ? H8A C8 H8C 106.1(14) . . ? C5 C8 H8B 110.7(10) . . ? H8A C8 H8B 107.3(15) . . ? H8C C8 H8B 109.6(14) . . ? C10 C9 C14 120.14(12) . . ? C10 C9 H9 120.3(8) . . ? C14 C9 H9 119.5(8) . . ? C9 C10 C11 120.12(13) . . ? C9 C10 H10 119.3(8) . . ? C11 C10 H10 120.6(8) . . ? C12 C11 C10 120.30(12) . . ? C12 C11 H11 120.2(8) . . ? C10 C11 H11 119.5(8) . . ? C11 C12 C13 119.78(13) . . ? C11 C12 H12 120.3(8) . . ? C13 C12 H12 119.9(8) . . ? C12 C13 C14 120.60(12) . . ? C12 C13 H13 119.1(8) . . ? C14 C13 H13 120.3(8) . . ? C9 C14 C13 119.06(11) . . ? C9 C14 C15 120.12(11) . . ? C13 C14 C15 120.82(11) . . ? C14 C15 N1 113.88(10) . . ? C14 C15 H15A 110.4(7) . . ? N1 C15 H15A 105.5(7) . . ? C14 C15 H15B 111.8(7) . . ? N1 C15 H15B 105.1(7) . . ? H15A C15 H15B 109.8(11) . . ? N1 C16 C17 111.29(10) . . ? N1 C16 H16A 106.4(7) . . ? C17 C16 H16A 111.0(7) . . ? N1 C16 H16B 106.5(8) . . ? C17 C16 H16B 111.3(8) . . ? H16A C16 H16B 110.1(11) . . ? C22 C17 C18 118.50(12) . . ? C22 C17 C16 120.63(11) . . ? C18 C17 C16 120.87(12) . . ? C17 C18 C19 120.45(13) . . ? C17 C18 H18 118.2(8) . . ? C19 C18 H18 121.3(8) . . ? C20 C19 C18 120.30(14) . . ? C20 C19 H19 119.0(9) . . ? C18 C19 H19 120.7(9) . . ? C21 C20 C19 119.69(14) . . ? C21 C20 H20 119.8(9) . . ? C19 C20 H20 120.5(9) . . ? C20 C21 C22 120.00(14) . . ? C20 C21 H21 119.9(9) . . ? C22 C21 H21 120.1(9) . . ? C21 C22 C17 121.05(13) . . ? C21 C22 H22 121.0(8) . . ? C17 C22 H22 118.0(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N1 O2 0.944(15) 1.825(16) 2.7559(14) 168.2(12) 1 N1 H1N2 O1 1.019(15) 1.601(15) 2.6090(13) 169.2(12) 2_545 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.142 _refine_diff_density_min -0.173 _refine_diff_density_rms 0.028