# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_cambridge 0440 _publ_section_title ;Anion recognition by N-confused calix[4]pyrrole-?-carbaldehyde and its Knoevenagel reaction derivatives ; _publ_contact_author_name 'Philip Gale' _publ_contact_author_email PHILIP.GALE@SOTON.AC.UK loop_ _publ_author_name P.Gale W.Dahaen S.E.Garcia-Garrido M.Kostermans M.E.Light # Attachment 'Crystal structure data_revised.cif' data_2006sot0648 _database_code_depnum_ccdc_archive 'CCDC 624049' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H37.80 N4 O1.90' _chemical_formula_weight 472.83 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 10.1714(3) _cell_length_b 10.1756(3) _cell_length_c 13.1069(4) _cell_angle_alpha 107.535(2) _cell_angle_beta 92.714(2) _cell_angle_gamma 91.380(2) _cell_volume 1291.03(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5845 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour 'Dark Yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 510 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9598 _exptl_absorpt_correction_T_max 0.9848 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 17460 reflections reduced R(int) from 0.0653 to 0.0385 Ratio of minimum to maximum apparent transmission: 0.803911 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29203 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5888 _reflns_number_gt 3951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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. The isolated hydrogen atom reported by CIFCHECK is an erroneous alert, probably due to it possessing less than unit occupancy. There a re a couple of residual peaks and troughs in the difference map around the site of the disorder. The substituent on the pyrrole shows a 10% disorder - this is mirrored in the 10% vacancy at the water site. ; _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^)+(0.0979P)^2^+1.6184P] 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 5888 _refine_ls_number_parameters 336 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.2009 _refine_ls_wR_factor_gt 0.1779 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 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 O2 O 0.71001(4) 0.31185(4) 0.46614(3) 0.04577(12) Uani 0.90 1 d PD . . H99 H 0.72871(18) 0.22509(13) 0.4620(3) 0.050 Uiso 0.90 1 d PD . . H98 H 0.62128(12) 0.3061(2) 0.4557(2) 0.050 Uiso 0.90 1 d PD . . C1 C 0.32505(3) 0.21712(4) 0.17128(3) 0.02298(10) Uani 1 1 d . . . C2 C 0.30311(4) 0.12898(4) 0.06904(3) 0.03054(12) Uani 1 1 d . . . H2 H 0.2676 0.1526 0.0088 0.037 Uiso 1 1 calc R . . C3 C 0.34293(4) -0.00366(4) 0.06939(3) 0.03105(12) Uani 1 1 d . . . H3 H 0.3380 -0.0848 0.0096 0.037 Uiso 1 1 calc R . . C4 C 0.38957(3) 0.00603(4) 0.17104(3) 0.02212(10) Uani 1 1 d . . . C5 C 0.43954(4) -0.10178(4) 0.21974(3) 0.02527(11) Uani 1 1 d . . . C6 C 0.34151(4) -0.12400(4) 0.29967(3) 0.03501(12) Uani 1 1 d . . . H6A H 0.3338 -0.0374 0.3573 0.053 Uiso 1 1 calc R . . H6B H 0.3733 -0.1950 0.3302 0.053 Uiso 1 1 calc R . . H6C H 0.2551 -0.1537 0.2624 0.053 Uiso 1 1 calc R . . C7 C 0.45238(4) -0.23836(4) 0.13055(4) 0.03554(13) Uani 1 1 d . . . H7A H 0.3662 -0.2687 0.0929 0.053 Uiso 1 1 calc R . . H7B H 0.4839 -0.3086 0.1621 0.053 Uiso 1 1 calc R . . H7C H 0.5152 -0.2250 0.0798 0.053 Uiso 1 1 calc R . . C8 C 0.57321(4) -0.05650(3) 0.27878(3) 0.02269(10) Uani 1 1 d . . . C9 C 0.61867(4) -0.05412(4) 0.37897(3) 0.02915(11) Uani 1 1 d . . . H9 H 0.5687 -0.0766 0.4312 0.035 Uiso 1 1 calc R . . C10 C 0.75469(4) -0.01181(4) 0.39119(3) 0.02923(11) Uani 1 1 d . . . H10 H 0.8113 -0.0015 0.4531 0.035 Uiso 1 1 calc R . . C11 C 0.78934(3) 0.01126(3) 0.29860(3) 0.02177(10) Uani 1 1 d . . . C12 C 0.91996(3) 0.05469(4) 0.26388(3) 0.02279(10) Uani 1 1 d . . . C13 C 0.97895(4) -0.07000(4) 0.18358(3) 0.02961(12) Uani 1 1 d . . . H13A H 0.9946 -0.1420 0.2178 0.044 Uiso 1 1 calc R . . H13B H 1.0624 -0.0412 0.1609 0.044 Uiso 1 1 calc R . . H13C H 0.9173 -0.1062 0.1210 0.044 Uiso 1 1 calc R . . C14 C 1.01757(4) 0.10501(4) 0.36265(3) 0.03191(12) Uani 1 1 d . . . H14A H 0.9844 0.1873 0.4137 0.048 Uiso 1 1 calc R . . H14B H 1.1035 0.1277 0.3401 0.048 Uiso 1 1 calc R . . H14C H 1.0269 0.0321 0.3968 0.048 Uiso 1 1 calc R . . C15 C 0.90006(3) 0.16733(4) 0.21246(3) 0.02129(10) Uani 1 1 d . . . C16 C 0.92895(4) 0.17629(4) 0.11381(3) 0.02543(11) Uani 1 1 d . . . H16 H 0.9664 0.1065 0.0586 0.031 Uiso 1 1 calc R . . C17 C 0.89310(4) 0.30842(4) 0.10829(3) 0.02539(11) Uani 1 1 d . . . H17 H 0.9017 0.3424 0.0488 0.030 Uiso 1 1 calc R . . C18 C 0.84399(3) 0.37765(3) 0.20437(3) 0.02090(10) Uani 1 1 d . . . C19 C 0.79416(4) 0.52225(4) 0.24634(3) 0.02451(10) Uani 1 1 d . A . C20 C 0.79081(4) 0.59106(4) 0.15663(4) 0.03720(12) Uani 1 1 d . . . H20A H 0.7563 0.6835 0.1835 0.056 Uiso 1 1 calc R . . H20B H 0.7338 0.5354 0.0958 0.056 Uiso 1 1 calc R . . H20C H 0.8802 0.5981 0.1334 0.056 Uiso 1 1 calc R . . C21 C 0.88969(4) 0.60834(4) 0.33843(4) 0.03652(14) Uani 1 1 d . . . H21A H 0.8618 0.7038 0.3624 0.055 Uiso 1 1 calc R . . H21B H 0.9789 0.6065 0.3131 0.055 Uiso 1 1 calc R . . H21C H 0.8890 0.5694 0.3983 0.055 Uiso 1 1 calc R . . C22 C 0.65297(4) 0.51291(3) 0.28134(3) 0.02225(10) Uani 1 1 d D . . C23A C 0.59247(3) 0.58333(3) 0.36980(3) 0.02500(12) Uani 0.90 1 d PD A 1 C26A C 0.63102(4) 0.67908(5) 0.46393(3) 0.03625(14) Uani 0.90 1 d PD A 1 H26A H 0.7201 0.7127 0.4725 0.044 Uiso 0.90 1 calc PR A 1 O1A O 0.55714(4) 0.72877(4) 0.54313(3) 0.04665(12) Uani 0.90 1 d PD A 1 N4A N 0.45966(3) 0.53782(3) 0.35557(2) 0.02915(10) Uani 0.90 1 d PD A 1 H4A H 0.3995 0.5695 0.4019 0.035 Uiso 0.90 1 calc PR A 1 C23B C 0.45966(3) 0.53782(3) 0.35557(2) 0.02500(12) Uani 0.10 1 d PD A 2 C26B C 0.39521(7) 0.56610(10) 0.44767(4) 0.03625(14) Uani 0.10 1 d PD . 2 H26B H 0.3203 0.5142 0.4569 0.044 Uiso 0.10 1 calc PRD . 2 O1B O 0.44683(19) 0.66993(13) 0.51997(12) 0.04665(12) Uani 0.10 1 d PD . 2 N4B N 0.59247(3) 0.58333(3) 0.36980(3) 0.02915(10) Uani 0.10 1 d PD A 2 H4B H 0.6296 0.6463 0.4261 0.035 Uiso 0.10 1 calc PR A 2 C24 C 0.43769(4) 0.44105(4) 0.26318(3) 0.02454(10) Uani 1 1 d D . . C25 C 0.55625(4) 0.42078(4) 0.21219(3) 0.02426(10) Uani 1 1 d . A . H25 H 0.5699 0.3573 0.1440 0.029 Uiso 1 1 calc R . . C27 C 0.30552(4) 0.36984(4) 0.21764(3) 0.02643(11) Uani 1 1 d . A . C28 C 0.25482(4) 0.42766(4) 0.12768(4) 0.03824(13) Uani 1 1 d . . . H28A H 0.3196 0.4129 0.0727 0.057 Uiso 1 1 calc R A . H28B H 0.2416 0.5267 0.1576 0.057 Uiso 1 1 calc R . . H28C H 0.1710 0.3802 0.0955 0.057 Uiso 1 1 calc R . . C29 C 0.20317(4) 0.39677(4) 0.30319(3) 0.03280(12) Uani 1 1 d . . . H29A H 0.1173 0.3564 0.2698 0.049 Uiso 1 1 calc R A . H29B H 0.1964 0.4964 0.3358 0.049 Uiso 1 1 calc RD . . H29C H 0.2304 0.3547 0.3586 0.049 Uiso 1 1 calc RD . . N1 N 0.37778(3) 0.14052(3) 0.23259(2) 0.02182(8) Uani 1 1 d . . . H1 H 0.4007 0.1731 0.3014 0.026 Uiso 1 1 calc R . . N2 N 0.67799(3) -0.01675(3) 0.23032(2) 0.02220(9) Uani 1 1 d . . . H2A H 0.6743 -0.0102 0.1648 0.027 Uiso 1 1 calc R . . N3 N 0.84866(3) 0.29187(3) 0.26742(2) 0.02173(8) Uani 1 1 d . . . H3A H 0.8227 0.3129 0.3333 0.026 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 O2 0.04553(19) 0.04312(18) 0.04877(18) 0.01240(14) 0.01241(16) 0.00438(16) C1 0.01551(15) 0.02444(15) 0.03206(17) 0.01318(12) 0.00166(14) -0.00006(13) C2 0.02911(19) 0.03628(19) 0.02608(17) 0.01045(14) -0.00629(15) 0.00045(16) C3 0.0318(2) 0.02583(18) 0.02962(19) 0.00012(15) -0.00322(16) 0.00211(16) C4 0.01641(15) 0.02064(15) 0.02779(16) 0.00503(13) 0.00221(14) -0.00089(13) C5 0.01899(16) 0.02055(15) 0.03706(18) 0.00998(13) 0.00178(15) -0.00046(13) C6 0.02162(18) 0.03604(18) 0.0559(2) 0.02636(14) 0.00555(16) 0.00033(15) C7 0.02734(19) 0.01997(17) 0.0539(2) 0.00383(17) -0.00177(19) -0.00154(16) C8 0.01957(16) 0.01635(14) 0.03450(17) 0.01053(12) 0.00546(14) 0.00233(13) C9 0.02718(18) 0.03233(17) 0.03314(17) 0.01676(13) 0.00686(15) 0.00375(15) C10 0.02571(18) 0.03484(18) 0.02952(17) 0.01376(13) -0.00210(15) 0.00295(15) C11 0.01881(16) 0.01806(15) 0.02849(16) 0.00736(12) -0.00124(14) 0.00250(13) C12 0.01609(15) 0.02053(15) 0.03171(17) 0.00826(13) -0.00111(14) 0.00025(13) C13 0.02252(18) 0.02184(16) 0.0448(2) 0.00974(14) 0.00630(16) 0.00379(14) C14 0.02547(19) 0.03082(18) 0.0405(2) 0.01414(14) -0.00801(16) -0.00197(15) C15 0.01413(15) 0.01902(15) 0.02895(17) 0.00513(12) -0.00165(14) -0.00065(13) C16 0.02691(18) 0.02232(16) 0.02514(17) 0.00419(13) 0.00260(15) 0.00001(15) C17 0.02450(18) 0.02658(16) 0.02616(16) 0.00989(13) 0.00013(14) -0.00056(14) C18 0.01526(15) 0.02041(14) 0.02851(16) 0.01017(12) -0.00128(13) -0.00165(13) C19 0.01800(16) 0.01819(15) 0.03725(18) 0.00859(13) 0.00019(15) -0.00113(13) C20 0.02842(19) 0.03093(17) 0.0615(2) 0.02649(14) 0.01084(18) 0.00419(15) C21 0.02066(18) 0.02226(18) 0.0571(3) -0.00105(18) -0.00459(18) -0.00151(15) C22 0.01985(16) 0.01598(14) 0.03246(17) 0.00997(12) -0.00125(14) 0.00192(13) C23A 0.0289(2) 0.01763(16) 0.02860(19) 0.00772(14) -0.00176(16) 0.00058(16) C26A 0.0346(2) 0.0373(2) 0.0369(2) 0.01175(17) -0.0015(2) 0.0026(2) O1A 0.0632(2) 0.04290(18) 0.02889(16) 0.00390(14) -0.00275(16) 0.00744(17) N4A 0.02615(17) 0.02582(15) 0.04058(17) 0.01575(12) 0.01144(14) 0.00829(14) C23B 0.0289(2) 0.01763(16) 0.02860(19) 0.00772(14) -0.00176(16) 0.00058(16) C26B 0.0346(2) 0.0373(2) 0.0369(2) 0.01175(17) -0.0015(2) 0.0026(2) O1B 0.0632(2) 0.04290(18) 0.02889(16) 0.00390(14) -0.00275(16) 0.00744(17) N4B 0.02615(17) 0.02582(15) 0.04058(17) 0.01575(12) 0.01144(14) 0.00829(14) C24 0.02107(17) 0.01792(14) 0.03616(18) 0.01050(12) 0.00108(15) 0.00153(13) C25 0.02043(17) 0.01886(15) 0.03166(18) 0.00504(13) 0.00075(14) 0.00031(14) C27 0.01725(16) 0.02361(16) 0.04142(19) 0.01436(13) 0.00111(15) 0.00177(14) C28 0.0266(2) 0.03405(18) 0.0611(2) 0.02665(15) -0.00773(18) -0.00053(16) C29 0.02080(17) 0.02407(17) 0.0503(2) 0.00575(16) 0.00676(17) 0.00055(15) N1 0.02269(14) 0.01894(13) 0.02343(13) 0.00630(10) -0.00091(12) -0.00102(12) N2 0.01940(14) 0.02363(13) 0.02480(13) 0.00940(10) 0.00057(12) -0.00051(12) N3 0.02139(14) 0.01982(13) 0.02384(13) 0.00600(10) 0.00307(12) 0.00262(11) _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 O2 O1B 1.623(2) 2_666 ? O2 C26B 1.8158(8) 2_666 ? C1 C2 1.3739(5) . ? C1 N1 1.3776(5) . ? C1 C27 1.5103(5) . ? C2 C3 1.4197(6) . ? C3 C4 1.3669(6) . ? C4 N1 1.3747(4) . ? C4 C5 1.5124(6) . ? C5 C8 1.5215(5) . ? C5 C7 1.5360(5) . ? C5 C6 1.5406(6) . ? C8 C9 1.3644(6) . ? C8 N2 1.3787(5) . ? C9 C10 1.4262(6) . ? C10 C11 1.3639(6) . ? C11 N2 1.3783(5) . ? C11 C12 1.5223(5) . ? C12 C15 1.5075(6) . ? C12 C13 1.5393(5) . ? C12 C14 1.5422(5) . ? C15 C16 1.3683(6) . ? C15 N3 1.3841(4) . ? C16 C17 1.4233(6) . ? C17 C18 1.3688(5) . ? C18 N3 1.3711(5) . ? C18 C19 1.5163(5) . ? C19 C22 1.5375(5) . ? C19 C20 1.5386(7) . ? C19 C21 1.5424(5) . ? C22 C23A 1.3507(5) . ? C22 C25 1.4239(5) . ? C23A C26A 1.3553(5) . ? C23A N4A 1.4029(5) . ? C26A O1A 1.2937(5) . ? N4A C24 1.3158(4) . ? C26B O1B 1.2699(14) . ? C26B O2 1.8158(8) 2_666 ? O1B O2 1.623(2) 2_666 ? C24 C25 1.3960(5) . ? C24 C27 1.5182(5) . ? C27 C29 1.5346(6) . ? C27 C28 1.5418(7) . ? 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 O1B O2 C26B 42.89(5) 2_666 2_666 ? C2 C1 N1 106.74(3) . . ? C2 C1 C27 131.47(4) . . ? N1 C1 C27 121.75(3) . . ? C1 C2 C3 107.84(4) . . ? C4 C3 C2 107.87(3) . . ? C3 C4 N1 107.14(3) . . ? C3 C4 C5 131.50(3) . . ? N1 C4 C5 121.28(3) . . ? C4 C5 C8 110.80(3) . . ? C4 C5 C7 109.36(3) . . ? C8 C5 C7 109.15(3) . . ? C4 C5 C6 109.58(3) . . ? C8 C5 C6 108.78(3) . . ? C7 C5 C6 109.14(3) . . ? C9 C8 N2 106.82(3) . . ? C9 C8 C5 130.95(4) . . ? N2 C8 C5 122.10(3) . . ? C8 C9 C10 107.77(4) . . ? C11 C10 C9 108.14(3) . . ? C10 C11 N2 106.62(3) . . ? C10 C11 C12 132.05(3) . . ? N2 C11 C12 121.31(3) . . ? C15 C12 C11 110.26(3) . . ? C15 C12 C13 109.50(3) . . ? C11 C12 C13 109.83(3) . . ? C15 C12 C14 110.40(3) . . ? C11 C12 C14 109.07(3) . . ? C13 C12 C14 107.74(3) . . ? C16 C15 N3 106.74(3) . . ? C16 C15 C12 131.65(3) . . ? N3 C15 C12 121.57(3) . . ? C15 C16 C17 108.09(3) . . ? C18 C17 C16 107.50(4) . . ? C17 C18 N3 107.46(3) . . ? C17 C18 C19 131.56(4) . . ? N3 C18 C19 120.95(3) . . ? C18 C19 C22 108.79(3) . . ? C18 C19 C20 109.74(3) . . ? C22 C19 C20 108.30(3) . . ? C18 C19 C21 108.96(3) . . ? C22 C19 C21 112.77(3) . . ? C20 C19 C21 108.24(3) . . ? C23A C22 C25 107.04(3) . . ? C23A C22 C19 132.28(3) . . ? C25 C22 C19 120.61(3) . . ? C22 C23A C26A 135.37(4) . . ? C22 C23A N4A 107.52(3) . . ? C26A C23A N4A 117.08(3) . . ? O1A C26A C23A 125.72(4) . . ? C24 N4A C23A 110.47(3) . . ? O1B C26B O2 60.43(9) . 2_666 ? C26B O1B O2 76.69(10) . 2_666 ? N4A C24 C25 107.72(3) . . ? N4A C24 C27 126.07(3) . . ? C25 C24 C27 126.14(3) . . ? C24 C25 C22 107.25(3) . . ? C1 C27 C24 108.55(3) . . ? C1 C27 C29 110.71(3) . . ? C24 C27 C29 111.62(3) . . ? C1 C27 C28 109.32(3) . . ? C24 C27 C28 108.42(3) . . ? C29 C27 C28 108.17(3) . . ? C4 N1 C1 110.41(3) . . ? C11 N2 C8 110.65(3) . . ? C18 N3 C15 110.20(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.048 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.061 #===END data_2006sot0639 _database_code_depnum_ccdc_archive 'CCDC 624050' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H40 N6 O, 0.5(C2 H3 N)' _chemical_formula_sum 'C42 H41.50 N6.50 O' _chemical_formula_weight 653.32 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 19.7663(15) _cell_length_b 11.8837(8) _cell_length_c 15.7559(14) _cell_angle_alpha 90.00 _cell_angle_beta 106.807(4) _cell_angle_gamma 90.00 _cell_volume 3542.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7046 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.02 _exptl_crystal_description Slab _exptl_crystal_colour Red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9751 _exptl_absorpt_correction_T_max 0.9970 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 11975 reflections reduced R(int) from 0.0726 to 0.0541 Ratio of minimum to maximum apparent transmission: 0.611566 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35967 _diffrn_reflns_av_R_equivalents 0.1582 _diffrn_reflns_av_sigmaI/netI 0.1726 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.11 _reflns_number_total 7024 _reflns_number_gt 3104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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. The MeCN is disordered over 2 positions, and is responsible for the high residual peak. ; _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^)+(0.1456P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7024 _refine_ls_number_parameters 465 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.2209 _refine_ls_R_factor_gt 0.0907 _refine_ls_wR_factor_ref 0.2756 _refine_ls_wR_factor_gt 0.2159 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.003 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 C1 C 0.3181(2) 0.9778(4) 0.0719(3) 0.0302(11) Uani 1 1 d . . . C2 C 0.2851(2) 1.0678(4) 0.0238(3) 0.0371(12) Uani 1 1 d . . . H2 H 0.2964 1.1006 -0.0253 0.044 Uiso 1 1 calc R . . C3 C 0.2305(3) 1.1040(4) 0.0601(3) 0.0388(12) Uani 1 1 d . . . H3 H 0.1990 1.1649 0.0392 0.047 Uiso 1 1 calc R . . C4 C 0.2316(2) 1.0362(4) 0.1300(3) 0.0334(12) Uani 1 1 d . . . C5 C 0.1900(2) 1.0337(4) 0.1980(3) 0.0364(12) Uani 1 1 d . . . C6 C 0.2391(3) 1.0655(4) 0.2891(3) 0.0435(13) Uani 1 1 d . . . H6A H 0.2126 1.0637 0.3329 0.065 Uiso 1 1 calc R . . H6B H 0.2578 1.1414 0.2865 0.065 Uiso 1 1 calc R . . H6C H 0.2783 1.0117 0.3061 0.065 Uiso 1 1 calc R . . C7 C 0.1298(3) 1.1201(4) 0.1706(4) 0.0476(14) Uani 1 1 d . . . H7A H 0.0966 1.0974 0.1140 0.071 Uiso 1 1 calc R . . H7B H 0.1494 1.1942 0.1641 0.071 Uiso 1 1 calc R . . H7C H 0.1051 1.1237 0.2162 0.071 Uiso 1 1 calc R . . C8 C 0.1611(2) 0.9165(4) 0.2030(3) 0.0331(12) Uani 1 1 d . . . C9 C 0.1704(3) 0.8423(4) 0.2705(3) 0.0404(13) Uani 1 1 d . . . H9 H 0.1998 0.8532 0.3294 0.048 Uiso 1 1 calc R . . C10 C 0.1290(3) 0.7458(4) 0.2387(4) 0.0424(13) Uani 1 1 d . . . H10 H 0.1259 0.6809 0.2726 0.051 Uiso 1 1 calc R . . C11 C 0.0942(2) 0.7616(4) 0.1511(3) 0.0347(12) Uani 1 1 d . . . C12 C 0.0428(2) 0.6909(4) 0.0836(3) 0.0401(13) Uani 1 1 d . . . C13 C -0.0304(3) 0.7461(6) 0.0552(4) 0.0663(18) Uani 1 1 d . . . H13A H -0.0469 0.7585 0.1074 0.099 Uiso 1 1 calc R . . H13B H -0.0637 0.6967 0.0134 0.099 Uiso 1 1 calc R . . H13C H -0.0275 0.8184 0.0265 0.099 Uiso 1 1 calc R . . C14 C 0.0364(3) 0.5751(5) 0.1241(4) 0.0660(18) Uani 1 1 d . . . H14A H 0.0829 0.5389 0.1426 0.099 Uiso 1 1 calc R . . H14B H 0.0035 0.5280 0.0798 0.099 Uiso 1 1 calc R . . H14C H 0.0187 0.5846 0.1757 0.099 Uiso 1 1 calc R . . C15 C 0.0695(2) 0.6761(4) 0.0036(3) 0.0366(12) Uani 1 1 d . . . C16 C 0.0393(3) 0.6983(4) -0.0845(3) 0.0426(13) Uani 1 1 d . . . H16 H -0.0065 0.7290 -0.1102 0.051 Uiso 1 1 calc R . . C17 C 0.0889(3) 0.6671(4) -0.1311(3) 0.0418(13) Uani 1 1 d . . . H17 H 0.0822 0.6736 -0.1931 0.050 Uiso 1 1 calc R . . C18 C 0.1473(2) 0.6265(4) -0.0698(3) 0.0346(12) Uani 1 1 d . . . C19 C 0.2147(2) 0.5772(4) -0.0804(3) 0.0380(12) Uani 1 1 d . . . C20 C 0.2147(3) 0.5837(5) -0.1766(3) 0.0515(15) Uani 1 1 d . . . H20A H 0.1739 0.5426 -0.2138 0.077 Uiso 1 1 calc R . . H20B H 0.2583 0.5501 -0.1829 0.077 Uiso 1 1 calc R . . H20C H 0.2120 0.6627 -0.1953 0.077 Uiso 1 1 calc R . . C21 C 0.2215(3) 0.4524(4) -0.0479(4) 0.0539(15) Uani 1 1 d . . . H21A H 0.2279 0.4504 0.0161 0.081 Uiso 1 1 calc R . . H21B H 0.2624 0.4174 -0.0608 0.081 Uiso 1 1 calc R . . H21C H 0.1786 0.4111 -0.0788 0.081 Uiso 1 1 calc R . . C22 C 0.2775(2) 0.6448(4) -0.0265(3) 0.0332(12) Uani 1 1 d . . . C23 C 0.2830(2) 0.7599(4) -0.0064(3) 0.0301(11) Uani 1 1 d . . . H23 H 0.2451 0.8123 -0.0221 0.036 Uiso 1 1 calc R . . C24 C 0.3523(2) 0.7857(4) 0.0401(3) 0.0322(12) Uani 1 1 d . . . C25 C 0.3901(2) 0.6806(4) 0.0502(3) 0.0321(11) Uani 1 1 d . . . C26 C 0.3789(2) 0.9045(4) 0.0650(3) 0.0308(11) Uani 1 1 d . . . C27 C 0.4383(2) 0.9151(4) 0.1537(3) 0.0375(12) Uani 1 1 d . . . H27A H 0.4448 0.9945 0.1710 0.056 Uiso 1 1 calc R . . H27B H 0.4825 0.8852 0.1464 0.056 Uiso 1 1 calc R . . H27C H 0.4253 0.8724 0.1998 0.056 Uiso 1 1 calc R . . C28 C 0.4076(3) 0.9504(4) -0.0092(3) 0.0402(13) Uani 1 1 d . . . H28A H 0.3712 0.9436 -0.0663 0.060 Uiso 1 1 calc R . . H28B H 0.4494 0.9071 -0.0109 0.060 Uiso 1 1 calc R . . H28C H 0.4205 1.0297 0.0024 0.060 Uiso 1 1 calc R . . C29 C 0.4595(2) 0.6534(4) 0.0983(3) 0.0342(12) Uani 1 1 d . . . H29 H 0.4879 0.7171 0.1217 0.041 Uiso 1 1 calc R . . C30 C 0.4951(2) 0.5514(4) 0.1184(3) 0.0298(11) Uani 1 1 d . . . C31 C 0.4686(3) 0.4381(4) 0.0907(3) 0.0339(12) Uani 1 1 d . . . C32 C 0.5203(2) 0.3574(4) 0.1436(3) 0.0327(12) Uani 1 1 d . . . C33 C 0.5181(3) 0.2407(4) 0.1434(3) 0.0380(12) Uani 1 1 d . . . H33 H 0.4805 0.2018 0.1027 0.046 Uiso 1 1 calc R . . C34 C 0.5706(3) 0.1828(4) 0.2022(4) 0.0425(13) Uani 1 1 d . . . H34 H 0.5702 0.1028 0.2021 0.051 Uiso 1 1 calc R . . C35 C 0.6247(3) 0.2406(4) 0.2623(4) 0.0457(14) Uani 1 1 d . . . H35 H 0.6598 0.1989 0.3046 0.055 Uiso 1 1 calc R . . C36 C 0.6294(3) 0.3577(4) 0.2629(3) 0.0395(13) Uani 1 1 d . . . H36 H 0.6675 0.3958 0.3035 0.047 Uiso 1 1 calc R . . C37 C 0.5764(2) 0.4163(4) 0.2019(3) 0.0327(12) Uani 1 1 d . . . C38 C 0.5648(2) 0.5388(4) 0.1797(3) 0.0345(12) Uani 1 1 d . . . C39 C 0.6162(2) 0.6198(4) 0.2102(3) 0.0340(12) Uani 1 1 d . . . C40 C 0.6127(2) 0.7318(5) 0.1760(4) 0.0397(13) Uani 1 1 d . . . C41 C 0.6820(3) 0.5985(4) 0.2759(4) 0.0362(12) Uani 1 1 d . . . N1 N 0.28533(19) 0.9594(3) 0.1367(3) 0.0336(10) Uani 1 1 d . . . H1 H 0.2970 0.9059 0.1769 0.040 Uiso 1 1 calc R . . N2 N 0.11464(19) 0.8675(3) 0.1303(3) 0.0362(10) Uani 1 1 d . . . H2A H 0.0998 0.8989 0.0776 0.043 Uiso 1 1 calc R . . N3 N 0.13514(19) 0.6326(3) 0.0109(3) 0.0341(10) Uani 1 1 d . . . H3A H 0.1655 0.6115 0.0611 0.041 Uiso 1 1 calc R . . N4 N 0.34112(19) 0.5994(3) 0.0069(3) 0.0347(10) Uani 1 1 d . . . H4 H 0.3511 0.5279 0.0023 0.042 Uiso 1 1 calc R . . N5 N 0.6140(2) 0.8237(4) 0.1526(3) 0.0569(13) Uani 1 1 d . . . N6 N 0.7352(2) 0.5866(4) 0.3304(3) 0.0479(12) Uani 1 1 d . . . O1 O 0.41237(18) 0.4085(3) 0.0359(2) 0.0407(9) Uani 1 1 d . . . N7 N 0.0683(4) 0.9702(7) -0.0723(5) 0.052(2) Uani 0.50 1 d PDU . . C44 C 0.0000 1.0308(9) -0.2500 0.099(3) Uani 1 2 d SDU . . H44A H -0.0404 1.0795 -0.2515 0.149 Uiso 0.50 1 calc PR . . H44B H -0.0167 0.9628 -0.2850 0.149 Uiso 0.50 1 calc PR . . H44C H 0.0331 1.0712 -0.2749 0.149 Uiso 0.50 1 calc PR . . C43 C 0.0395(5) 0.9960(9) -0.1488(5) 0.049(3) Uani 0.50 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(3) 0.032(3) 0.026(3) -0.001(2) 0.003(2) -0.003(2) C2 0.037(3) 0.039(3) 0.035(3) -0.002(2) 0.010(2) -0.001(2) C3 0.041(3) 0.034(3) 0.034(3) 0.004(2) 0.000(2) 0.010(2) C4 0.026(3) 0.032(3) 0.039(3) -0.007(2) 0.005(2) -0.001(2) C5 0.033(3) 0.037(3) 0.037(3) -0.005(2) 0.007(2) 0.004(2) C6 0.044(3) 0.048(3) 0.038(3) -0.011(3) 0.012(3) -0.005(2) C7 0.041(3) 0.041(3) 0.062(4) -0.004(3) 0.017(3) 0.007(2) C8 0.027(3) 0.040(3) 0.030(3) -0.005(2) 0.005(2) 0.001(2) C9 0.045(3) 0.040(3) 0.030(3) -0.001(3) 0.001(3) 0.007(2) C10 0.050(3) 0.036(3) 0.039(4) 0.003(3) 0.011(3) 0.000(2) C11 0.032(3) 0.040(3) 0.033(3) 0.000(2) 0.012(3) 0.000(2) C12 0.035(3) 0.046(3) 0.040(3) -0.006(3) 0.014(3) -0.011(2) C13 0.031(3) 0.111(5) 0.057(4) -0.021(4) 0.011(3) -0.012(3) C14 0.094(5) 0.058(4) 0.054(4) -0.003(3) 0.034(4) -0.039(3) C15 0.033(3) 0.040(3) 0.033(3) 0.000(2) 0.003(2) -0.009(2) C16 0.034(3) 0.047(3) 0.042(4) 0.004(3) 0.003(3) -0.001(2) C17 0.040(3) 0.052(3) 0.031(3) 0.004(3) 0.007(3) -0.004(3) C18 0.035(3) 0.036(3) 0.031(3) -0.004(2) 0.007(2) -0.007(2) C19 0.036(3) 0.032(3) 0.044(3) -0.006(2) 0.008(3) -0.004(2) C20 0.047(3) 0.067(4) 0.041(4) -0.017(3) 0.014(3) -0.012(3) C21 0.045(3) 0.040(3) 0.074(4) -0.003(3) 0.012(3) -0.004(2) C22 0.029(3) 0.036(3) 0.034(3) -0.001(2) 0.008(2) 0.005(2) C23 0.029(3) 0.027(3) 0.035(3) 0.001(2) 0.009(2) 0.004(2) C24 0.031(3) 0.038(3) 0.028(3) 0.001(2) 0.010(2) -0.002(2) C25 0.028(3) 0.038(3) 0.030(3) 0.004(2) 0.006(2) 0.004(2) C26 0.024(3) 0.035(3) 0.031(3) -0.004(2) 0.005(2) -0.004(2) C27 0.030(3) 0.041(3) 0.035(3) -0.005(2) -0.001(2) 0.002(2) C28 0.040(3) 0.039(3) 0.045(3) -0.005(2) 0.019(3) -0.007(2) C29 0.039(3) 0.032(3) 0.035(3) -0.002(2) 0.016(3) -0.003(2) C30 0.032(3) 0.032(3) 0.024(3) 0.001(2) 0.007(2) 0.006(2) C31 0.033(3) 0.037(3) 0.035(3) -0.001(2) 0.016(3) -0.001(2) C32 0.035(3) 0.033(3) 0.034(3) 0.003(2) 0.016(2) 0.006(2) C33 0.045(3) 0.035(3) 0.038(3) 0.001(2) 0.019(3) -0.001(2) C34 0.048(3) 0.036(3) 0.047(4) 0.004(3) 0.021(3) 0.007(3) C35 0.044(3) 0.050(3) 0.049(4) 0.019(3) 0.022(3) 0.016(3) C36 0.034(3) 0.046(3) 0.040(3) 0.010(3) 0.012(3) 0.007(2) C37 0.035(3) 0.036(3) 0.033(3) 0.001(2) 0.018(2) 0.005(2) C38 0.039(3) 0.038(3) 0.031(3) 0.003(2) 0.018(3) 0.001(2) C39 0.030(3) 0.040(3) 0.030(3) -0.008(2) 0.007(2) 0.003(2) C40 0.030(3) 0.041(3) 0.047(3) -0.006(3) 0.008(3) -0.002(2) C41 0.040(3) 0.036(3) 0.035(3) -0.013(2) 0.015(3) -0.002(2) N1 0.036(2) 0.031(2) 0.034(2) 0.0076(18) 0.010(2) 0.0038(18) N2 0.032(2) 0.044(2) 0.029(2) 0.003(2) 0.005(2) -0.0015(19) N3 0.028(2) 0.043(2) 0.028(2) 0.0000(18) 0.0037(19) -0.0037(18) N4 0.034(2) 0.029(2) 0.039(3) -0.0034(19) 0.007(2) -0.0024(19) N5 0.048(3) 0.047(3) 0.077(4) 0.000(3) 0.019(3) -0.004(2) N6 0.041(3) 0.056(3) 0.042(3) -0.011(2) 0.005(2) 0.003(2) O1 0.045(2) 0.0330(19) 0.042(2) -0.0039(16) 0.0097(18) -0.0035(16) N7 0.053(3) 0.052(3) 0.053(3) -0.0006(11) 0.0161(12) -0.0032(11) C44 0.099(4) 0.100(4) 0.100(4) 0.000 0.0301(14) 0.000 C43 0.048(3) 0.049(3) 0.049(3) 0.0012(11) 0.0137(13) -0.0011(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.363(6) . ? C1 N1 1.375(5) . ? C1 C26 1.513(6) . ? C2 C3 1.426(7) . ? C3 C4 1.359(6) . ? C4 N1 1.381(5) . ? C4 C5 1.528(6) . ? C5 C8 1.517(6) . ? C5 C6 1.529(7) . ? C5 C7 1.535(6) . ? C8 C9 1.352(6) . ? C8 N2 1.373(6) . ? C9 C10 1.414(7) . ? C10 C11 1.365(7) . ? C11 N2 1.389(6) . ? C11 C12 1.499(7) . ? C12 C15 1.511(7) . ? C12 C13 1.532(7) . ? C12 C14 1.538(7) . ? C15 C16 1.369(7) . ? C15 N3 1.370(6) . ? C16 C17 1.433(7) . ? C17 C18 1.362(7) . ? C18 N3 1.362(6) . ? C18 C19 1.508(7) . ? C19 C22 1.515(6) . ? C19 C20 1.519(7) . ? C19 C21 1.561(7) . ? C22 N4 1.329(5) . ? C22 C23 1.402(6) . ? C23 C24 1.389(6) . ? C24 C25 1.440(6) . ? C24 C26 1.518(6) . ? C25 N4 1.397(6) . ? C25 C29 1.401(6) . ? C26 C28 1.539(6) . ? C26 C27 1.549(6) . ? C29 C30 1.392(6) . ? C30 C38 1.443(6) . ? C30 C31 1.464(6) . ? C31 O1 1.245(5) . ? C31 C32 1.472(6) . ? C32 C33 1.387(6) . ? C32 C37 1.405(6) . ? C33 C34 1.361(7) . ? C34 C35 1.389(7) . ? C35 C36 1.394(7) . ? C36 C37 1.388(6) . ? C37 C38 1.500(6) . ? C38 C39 1.381(6) . ? C39 C41 1.432(7) . ? C39 C40 1.430(7) . ? C40 N5 1.156(6) . ? C41 N6 1.158(6) . ? N7 C43 1.213(7) . ? C44 C43 1.614(7) . ? 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 C1 N1 106.6(4) . . ? C2 C1 C26 132.4(4) . . ? N1 C1 C26 121.1(4) . . ? C1 C2 C3 108.0(4) . . ? C4 C3 C2 108.0(4) . . ? C3 C4 N1 106.6(4) . . ? C3 C4 C5 133.9(4) . . ? N1 C4 C5 119.4(4) . . ? C8 C5 C6 108.9(4) . . ? C8 C5 C4 109.9(4) . . ? C6 C5 C4 109.2(4) . . ? C8 C5 C7 110.8(4) . . ? C6 C5 C7 109.2(4) . . ? C4 C5 C7 108.7(4) . . ? C9 C8 N2 106.6(4) . . ? C9 C8 C5 132.2(5) . . ? N2 C8 C5 121.2(4) . . ? C8 C9 C10 108.5(5) . . ? C11 C10 C9 108.5(4) . . ? C10 C11 N2 105.5(4) . . ? C10 C11 C12 132.9(5) . . ? N2 C11 C12 121.6(4) . . ? C11 C12 C15 109.2(4) . . ? C11 C12 C13 110.9(4) . . ? C15 C12 C13 109.5(4) . . ? C11 C12 C14 109.1(4) . . ? C15 C12 C14 109.4(4) . . ? C13 C12 C14 108.7(4) . . ? C16 C15 N3 106.4(4) . . ? C16 C15 C12 131.9(5) . . ? N3 C15 C12 121.7(4) . . ? C15 C16 C17 107.9(4) . . ? C18 C17 C16 107.1(4) . . ? C17 C18 N3 107.5(4) . . ? C17 C18 C19 130.9(5) . . ? N3 C18 C19 121.6(4) . . ? C18 C19 C22 109.8(4) . . ? C18 C19 C20 110.2(4) . . ? C22 C19 C20 107.2(4) . . ? C18 C19 C21 109.1(4) . . ? C22 C19 C21 109.9(4) . . ? C20 C19 C21 110.5(4) . . ? N4 C22 C23 107.7(4) . . ? N4 C22 C19 122.3(4) . . ? C23 C22 C19 129.9(4) . . ? C24 C23 C22 109.5(4) . . ? C23 C24 C25 105.6(4) . . ? C23 C24 C26 123.8(4) . . ? C25 C24 C26 130.5(4) . . ? N4 C25 C29 122.5(4) . . ? N4 C25 C24 106.3(4) . . ? C29 C25 C24 130.9(4) . . ? C1 C26 C24 109.4(3) . . ? C1 C26 C28 109.0(4) . . ? C24 C26 C28 108.0(4) . . ? C1 C26 C27 107.4(4) . . ? C24 C26 C27 115.1(4) . . ? C28 C26 C27 107.8(4) . . ? C30 C29 C25 132.5(4) . . ? C29 C30 C38 124.3(4) . . ? C29 C30 C31 128.3(4) . . ? C38 C30 C31 107.1(4) . . ? O1 C31 C30 129.6(4) . . ? O1 C31 C32 122.9(4) . . ? C30 C31 C32 107.5(4) . . ? C33 C32 C37 121.1(4) . . ? C33 C32 C31 129.4(5) . . ? C37 C32 C31 109.5(4) . . ? C34 C33 C32 119.2(5) . . ? C33 C34 C35 119.9(5) . . ? C34 C35 C36 122.4(5) . . ? C37 C36 C35 117.4(5) . . ? C36 C37 C32 119.9(4) . . ? C36 C37 C38 133.1(5) . . ? C32 C37 C38 107.0(4) . . ? C39 C38 C30 128.7(4) . . ? C39 C38 C37 123.2(4) . . ? C30 C38 C37 108.0(4) . . ? C38 C39 C41 123.5(4) . . ? C38 C39 C40 124.6(4) . . ? C41 C39 C40 111.8(4) . . ? N5 C40 C39 175.6(6) . . ? N6 C41 C39 176.7(5) . . ? C1 N1 C4 110.8(4) . . ? C8 N2 C11 110.9(4) . . ? C18 N3 C15 111.1(4) . . ? C22 N4 C25 110.8(4) . . ? N7 C43 C44 179.0(10) . . ? 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 N2 H2A N7 0.88 2.42 3.291(8) 173.3 . N3 H3A N6 0.88 2.22 3.068(6) 162.1 2_655 N4 H4 O1 0.88 1.84 2.639(5) 149.8 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.529 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.090 #===END data_2006sot0682 _database_code_depnum_ccdc_archive 'CCDC 624051' _database_code_CSD 6SOT0682 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H48 N4 O5 S' _chemical_formula_weight 660.85 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' S S 0.1246 0.1234 '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 10.1460(2) _cell_length_b 26.3142(9) _cell_length_c 26.8959(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.040(2) _cell_angle_gamma 90.00 _cell_volume 7110.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13690 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 26.02 _exptl_crystal_description Needle _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9497 _exptl_absorpt_correction_T_max 0.9959 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 31824 reflections reduced R(int) from 0.0991 to 0.0760 Ratio of minimum to maximum apparent transmission: 0.725392 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76382 _diffrn_reflns_av_R_equivalents 0.1523 _diffrn_reflns_av_sigmaI/netI 0.1431 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 26.10 _reflns_number_total 13971 _reflns_number_gt 7770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.1387P)^2^+40.7798P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13971 _refine_ls_number_parameters 828 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.1950 _refine_ls_R_factor_gt 0.1076 _refine_ls_wR_factor_ref 0.3182 _refine_ls_wR_factor_gt 0.2649 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.004 _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 -0.0473(5) 0.40317(19) 0.82092(18) 0.0296(11) Uani 1 1 d . . . H1 H -0.0136 0.3755 0.8360 0.036 Uiso 1 1 calc R . . N2 N 0.2558(5) 0.4419(2) 0.93647(19) 0.0342(12) Uani 1 1 d . . . H2 H 0.2299 0.4384 0.9662 0.041 Uiso 1 1 calc R . . N3 N 0.4049(5) 0.4048(2) 0.76604(18) 0.0337(12) Uani 1 1 d . . . H3 H 0.3973 0.3753 0.7808 0.040 Uiso 1 1 calc R . . N4 N 0.0933(5) 0.3711(2) 0.71260(19) 0.0364(13) Uani 1 1 d . . . H4 H 0.0830 0.4042 0.7094 0.044 Uiso 1 1 calc R . . C1 C -0.1124(5) 0.4051(2) 0.7726(2) 0.0297(14) Uani 1 1 d . . . C2 C -0.1494(6) 0.4551(2) 0.7629(2) 0.0323(14) Uani 1 1 d . . . H2A H -0.1954 0.4682 0.7324 0.039 Uiso 1 1 calc R . . C3 C -0.1058(6) 0.4831(2) 0.8073(2) 0.0326(14) Uani 1 1 d . . . H3A H -0.1188 0.5185 0.8116 0.039 Uiso 1 1 calc R . . C4 C -0.0424(6) 0.4513(2) 0.8426(2) 0.0308(14) Uani 1 1 d . . . C5 C 0.0287(6) 0.4604(2) 0.8946(2) 0.0317(14) Uani 1 1 d . . . C6 C 0.0115(7) 0.5167(2) 0.9081(3) 0.0430(17) Uani 1 1 d . . . H6A H 0.0600 0.5236 0.9415 0.065 Uiso 1 1 calc R . . H6B H -0.0833 0.5241 0.9079 0.065 Uiso 1 1 calc R . . H6C H 0.0466 0.5383 0.8833 0.065 Uiso 1 1 calc R . . C7 C -0.0277(6) 0.4267(3) 0.9335(2) 0.0381(15) Uani 1 1 d . . . H7A H -0.0184 0.3908 0.9247 0.057 Uiso 1 1 calc R . . H7B H -0.1220 0.4346 0.9335 0.057 Uiso 1 1 calc R . . H7C H 0.0214 0.4331 0.9669 0.057 Uiso 1 1 calc R . . C8 C 0.1750(6) 0.4508(2) 0.8946(2) 0.0276(13) Uani 1 1 d . . . C9 C 0.2529(5) 0.4539(2) 0.8557(2) 0.0272(13) Uani 1 1 d . . . H9 H 0.2201 0.4597 0.8213 0.033 Uiso 1 1 calc R . . C10 C 0.3860(6) 0.4472(2) 0.8754(2) 0.0312(14) Uani 1 1 d . . . C11 C 0.3870(6) 0.4389(2) 0.9277(2) 0.0337(15) Uani 1 1 d . . . C12 C 0.5033(5) 0.4495(2) 0.8458(2) 0.0320(14) Uani 1 1 d . . . C13 C 0.6009(6) 0.4042(3) 0.8568(2) 0.0408(16) Uani 1 1 d . . . H13A H 0.5512 0.3722 0.8525 0.061 Uiso 1 1 calc R . . H13B H 0.6463 0.4066 0.8913 0.061 Uiso 1 1 calc R . . H13C H 0.6668 0.4052 0.8334 0.061 Uiso 1 1 calc R . . C14 C 0.5778(7) 0.4994(3) 0.8596(3) 0.0476(18) Uani 1 1 d . . . H14A H 0.6509 0.5030 0.8395 0.071 Uiso 1 1 calc R . . H14B H 0.6139 0.4992 0.8953 0.071 Uiso 1 1 calc R . . H14C H 0.5163 0.5281 0.8526 0.071 Uiso 1 1 calc R . . C15 C 0.4542(5) 0.4487(2) 0.7904(2) 0.0313(14) Uani 1 1 d . . . C16 C 0.4483(7) 0.4853(3) 0.7543(3) 0.0501(19) Uani 1 1 d . . . H16 H 0.4762 0.5196 0.7596 0.060 Uiso 1 1 calc R . . C17 C 0.3943(8) 0.4639(3) 0.7081(3) 0.055(2) Uani 1 1 d . . . H17 H 0.3781 0.4816 0.6771 0.066 Uiso 1 1 calc R . . C18 C 0.3689(6) 0.4138(3) 0.7149(2) 0.0398(16) Uani 1 1 d . . . C19 C 0.3128(7) 0.3724(3) 0.6799(3) 0.0457(18) Uani 1 1 d . . . C20 C 0.4237(7) 0.3339(3) 0.6725(3) 0.065(2) Uani 1 1 d . . . H20A H 0.4954 0.3514 0.6585 0.098 Uiso 1 1 calc R . . H20B H 0.3868 0.3071 0.6494 0.098 Uiso 1 1 calc R . . H20C H 0.4590 0.3188 0.7050 0.098 Uiso 1 1 calc R . . C21 C 0.2581(8) 0.3958(4) 0.6283(3) 0.061(2) Uani 1 1 d . . . H21A H 0.1844 0.4189 0.6323 0.091 Uiso 1 1 calc R . . H21B H 0.2261 0.3687 0.6048 0.091 Uiso 1 1 calc R . . H21C H 0.3290 0.4148 0.6153 0.091 Uiso 1 1 calc R . . C22 C 0.2024(6) 0.3444(3) 0.7011(2) 0.0381(16) Uani 1 1 d . . . C23 C 0.1802(7) 0.2950(3) 0.7112(2) 0.0406(16) Uani 1 1 d . . . H23 H 0.2386 0.2676 0.7070 0.049 Uiso 1 1 calc R . . C24 C 0.0554(6) 0.2907(3) 0.7292(2) 0.0397(16) Uani 1 1 d . . . H24 H 0.0156 0.2603 0.7391 0.048 Uiso 1 1 calc R . . C25 C 0.0033(6) 0.3389(2) 0.7296(2) 0.0335(14) Uani 1 1 d . . . C26 C -0.1305(6) 0.3588(3) 0.7394(2) 0.0348(15) Uani 1 1 d . . . C27 C -0.2062(7) 0.3176(3) 0.7643(3) 0.0450(18) Uani 1 1 d . . . H27A H -0.1560 0.3085 0.7969 0.068 Uiso 1 1 calc R . . H27B H -0.2169 0.2875 0.7427 0.068 Uiso 1 1 calc R . . H27C H -0.2941 0.3305 0.7692 0.068 Uiso 1 1 calc R . . C28 C -0.2118(6) 0.3737(3) 0.6890(3) 0.0484(19) Uani 1 1 d . . . H28A H -0.2946 0.3902 0.6950 0.073 Uiso 1 1 calc R . . H28B H -0.2327 0.3431 0.6686 0.073 Uiso 1 1 calc R . . H28C H -0.1599 0.3971 0.6711 0.073 Uiso 1 1 calc R . . C29 C 0.4926(7) 0.4288(3) 0.9654(2) 0.0475(18) Uani 1 1 d D . . H29 H 0.5766 0.4333 0.9542 0.057 Uiso 1 1 calc R . . C30 C 0.5049(6) 0.4143(3) 1.0139(2) 0.0498(19) Uani 1 1 d D . . C31 C 0.6400(7) 0.4056(3) 1.0403(3) 0.063(2) Uani 1 1 d D . . C32 C 0.5453(7) 0.3523(3) 1.0975(2) 0.059(2) Uani 1 1 d D . . C33 C 0.3968(6) 0.4071(3) 1.0440(2) 0.0469(18) Uani 1 1 d D . . C34 C 0.5699(10) 0.3411(4) 1.1530(3) 0.082(3) Uani 1 1 d D . . H34A H 0.5810 0.3731 1.1718 0.123 Uiso 1 1 calc R . . H34B H 0.6507 0.3206 1.1607 0.123 Uiso 1 1 calc R . . H34C H 0.4939 0.3224 1.1627 0.123 Uiso 1 1 calc R . . C35 C 0.5321(9) 0.3050(3) 1.0657(3) 0.083(3) Uani 1 1 d D . . H35A H 0.4549 0.2854 1.0729 0.125 Uiso 1 1 calc R . . H35B H 0.6128 0.2844 1.0734 0.125 Uiso 1 1 calc R . . H35C H 0.5201 0.3145 1.0301 0.125 Uiso 1 1 calc R . . O1 O 0.7393(5) 0.4191(3) 1.0232(2) 0.0747(18) Uani 1 1 d D . . O2 O 0.2813(5) 0.4219(2) 1.03420(18) 0.0595(15) Uani 1 1 d D . . O3 O 0.6544(5) 0.3825(2) 1.08544(18) 0.0666(16) Uani 1 1 d D . . O4 O 0.4256(5) 0.3819(2) 1.08851(17) 0.0562(14) Uani 1 1 d D . . N5 N 0.0206(5) 0.60374(19) 0.62999(18) 0.0302(12) Uani 1 1 d . . . H5 H 0.0291 0.6367 0.6261 0.036 Uiso 1 1 calc R . . N6 N 0.3467(5) 0.61017(19) 0.69059(17) 0.0292(11) Uani 1 1 d . . . H6 H 0.3412 0.5794 0.6776 0.035 Uiso 1 1 calc R . . N7 N 0.4764(4) 0.62992(18) 0.57751(17) 0.0244(11) Uani 1 1 d . . . H7 H 0.4619 0.6629 0.5777 0.029 Uiso 1 1 calc R . . C36 C -0.0366(6) 0.5716(2) 0.5929(2) 0.0316(14) Uani 1 1 d . . . C37 C -0.0312(7) 0.5249(3) 0.6138(3) 0.0504(19) Uani 1 1 d . . . H37 H -0.0636 0.4944 0.5974 0.061 Uiso 1 1 calc R . . C38 C 0.0312(7) 0.5289(3) 0.6644(3) 0.053(2) Uani 1 1 d . . . H38 H 0.0477 0.5017 0.6877 0.064 Uiso 1 1 calc R . . C39 C 0.0629(6) 0.5782(3) 0.6737(2) 0.0349(15) Uani 1 1 d . . . C40 C 0.1218(6) 0.6054(3) 0.7207(2) 0.0453(18) Uani 1 1 d . . . C41 C 0.1524(8) 0.5681(4) 0.7643(3) 0.069(3) Uani 1 1 d . . . H41A H 0.0694 0.5525 0.7715 0.104 Uiso 1 1 calc R . . H41B H 0.1950 0.5862 0.7941 0.104 Uiso 1 1 calc R . . H41C H 0.2124 0.5415 0.7552 0.104 Uiso 1 1 calc R . . C42 C 0.0212(7) 0.6456(4) 0.7343(3) 0.062(2) Uani 1 1 d . . . H42A H 0.0109 0.6724 0.7087 0.094 Uiso 1 1 calc R . . H42B H 0.0541 0.6605 0.7671 0.094 Uiso 1 1 calc R . . H42C H -0.0651 0.6294 0.7357 0.094 Uiso 1 1 calc R . . C43 C 0.2486(6) 0.6334(3) 0.7135(2) 0.0343(15) Uani 1 1 d . . . C44 C 0.2975(7) 0.6801(3) 0.7289(2) 0.0409(16) Uani 1 1 d . . . H44 H 0.2527 0.7047 0.7462 0.049 Uiso 1 1 calc R . . C45 C 0.4245(6) 0.6858(3) 0.7148(2) 0.0368(15) Uani 1 1 d . . . H45 H 0.4805 0.7147 0.7207 0.044 Uiso 1 1 calc R . . C46 C 0.4532(6) 0.6420(2) 0.6911(2) 0.0275(13) Uani 1 1 d . . . C47 C 0.5766(6) 0.6256(2) 0.6688(2) 0.0308(14) Uani 1 1 d . . . C48 C 0.6578(6) 0.5864(3) 0.7032(2) 0.0371(15) Uani 1 1 d . . . H48A H 0.6037 0.5559 0.7059 0.056 Uiso 1 1 calc R . . H48B H 0.6829 0.6011 0.7366 0.056 Uiso 1 1 calc R . . H48C H 0.7383 0.5772 0.6889 0.056 Uiso 1 1 calc R . . C49 C 0.6659(6) 0.6720(2) 0.6645(2) 0.0346(15) Uani 1 1 d . . . H49A H 0.7442 0.6617 0.6494 0.052 Uiso 1 1 calc R . . H49B H 0.6945 0.6860 0.6981 0.052 Uiso 1 1 calc R . . H49C H 0.6161 0.6978 0.6435 0.052 Uiso 1 1 calc R . . C50 C 0.5342(5) 0.6022(2) 0.6180(2) 0.0269(13) Uani 1 1 d . . . C51 C 0.5355(6) 0.5528(2) 0.6023(2) 0.0297(13) Uani 1 1 d . . . H51 H 0.5688 0.5246 0.6222 0.036 Uiso 1 1 calc R . . C52 C 0.4780(6) 0.5508(2) 0.5505(2) 0.0344(15) Uani 1 1 d . . . H52 H 0.4659 0.5213 0.5299 0.041 Uiso 1 1 calc R . . C53 C 0.4444(6) 0.5990(2) 0.5367(2) 0.0291(13) Uani 1 1 d . A . C54 C 0.3711(6) 0.6190(2) 0.4875(2) 0.0310(14) Uani 1 1 d . . . C55 C 0.3797(7) 0.5793(3) 0.4453(2) 0.0370(15) Uani 1 1 d . A . H55A H 0.3284 0.5491 0.4517 0.055 Uiso 1 1 calc R . . H55B H 0.4730 0.5699 0.4449 0.055 Uiso 1 1 calc R . . H55C H 0.3432 0.5940 0.4128 0.055 Uiso 1 1 calc R . . C56 C 0.4395(6) 0.6683(2) 0.4729(2) 0.0332(14) Uani 1 1 d . A . H56A H 0.4005 0.6787 0.4390 0.050 Uiso 1 1 calc R . . H56B H 0.5350 0.6621 0.4736 0.050 Uiso 1 1 calc R . . H56C H 0.4264 0.6952 0.4968 0.050 Uiso 1 1 calc R . . C61 C -0.0893(6) 0.5921(2) 0.5416(2) 0.0322(14) Uani 1 1 d . . . C62 C -0.1560(7) 0.5481(3) 0.5089(3) 0.0477(18) Uani 1 1 d . . . H62A H -0.0899 0.5216 0.5055 0.072 Uiso 1 1 calc R . . H62B H -0.1917 0.5611 0.4756 0.072 Uiso 1 1 calc R . . H62C H -0.2286 0.5337 0.5249 0.072 Uiso 1 1 calc R . . C63 C -0.1963(6) 0.6321(3) 0.5470(2) 0.0360(15) Uani 1 1 d . . . H63A H -0.2646 0.6173 0.5650 0.054 Uiso 1 1 calc R . . H63B H -0.2374 0.6432 0.5136 0.054 Uiso 1 1 calc R . . H63C H -0.1555 0.6613 0.5658 0.054 Uiso 1 1 calc R . . C57A C 0.2259(6) 0.6261(2) 0.4930(2) 0.0336(6) Uani 0.65 1 d P A 1 C58A C 0.1567(6) 0.5975(2) 0.5236(2) 0.0336(6) Uani 0.65 1 d P A 1 H58A H 0.1937 0.5713 0.5456 0.040 Uiso 0.65 1 calc PR A 1 C59A C 0.0231(6) 0.6129(2) 0.5171(2) 0.0336(6) Uani 0.65 1 d P A 1 C60A C 0.1329(6) 0.6605(2) 0.46692(19) 0.0336(6) Uani 0.65 1 d PD A 1 N8A N 0.0111(5) 0.65162(19) 0.48355(19) 0.0336(6) Uani 0.65 1 d P A 1 H8A H -0.0627 0.6686 0.4737 0.040 Uiso 0.65 1 calc PR A 1 C64A C 0.1284(8) 0.6974(3) 0.4308(3) 0.0301(7) Uani 0.65 1 d PD A 1 H64A H 0.2105 0.6984 0.4176 0.036 Uiso 0.65 1 calc PR A 1 C65A C 0.0441(7) 0.7329(3) 0.4078(3) 0.0301(7) Uani 0.65 1 d PD A 1 C68A C 0.0979(8) 0.7649(3) 0.3702(3) 0.0301(7) Uani 0.65 1 d PD A 1 C67A C -0.0710(7) 0.8258(3) 0.3801(3) 0.0301(7) Uani 0.65 1 d PD A 1 C66A C -0.0926(8) 0.7435(3) 0.4157(4) 0.0301(7) Uani 0.65 1 d PD A 1 C69A C -0.0037(9) 0.8520(3) 0.4265(3) 0.0301(7) Uani 0.65 1 d PD A 1 H69A H -0.0697 0.8715 0.4419 0.045 Uiso 0.65 1 calc PR A 1 H69B H 0.0650 0.8750 0.4174 0.045 Uiso 0.65 1 calc PR A 1 H69C H 0.0373 0.8265 0.4504 0.045 Uiso 0.65 1 calc PR A 1 C70A C -0.1596(8) 0.8597(3) 0.3440(4) 0.0301(7) Uani 0.65 1 d PD A 1 H70A H -0.2032 0.8392 0.3160 0.045 Uiso 0.65 1 calc PR A 1 H70B H -0.1056 0.8862 0.3312 0.045 Uiso 0.65 1 calc PR A 1 H70C H -0.2274 0.8755 0.3616 0.045 Uiso 0.65 1 calc PR A 1 O5A O 0.2012(5) 0.7551(2) 0.3537(2) 0.0318(7) Uani 0.65 1 d PD A 1 O6A O -0.1621(6) 0.7174(2) 0.4395(2) 0.0318(7) Uani 0.65 1 d PD A 1 O8A O 0.0274(5) 0.8060(2) 0.3519(2) 0.0318(7) Uani 0.65 1 d PD A 1 O7A O -0.1550(6) 0.7854(2) 0.3933(2) 0.0318(7) Uani 0.65 1 d PD A 1 C57B C 0.2259(6) 0.6261(2) 0.4930(2) 0.0336(6) Uani 0.35 1 d P A 2 C58B C 0.1567(6) 0.5975(2) 0.5236(2) 0.0336(6) Uani 0.35 1 d P A 2 H58B H 0.1937 0.5713 0.5456 0.040 Uiso 0.35 1 calc PR A 2 C59B C 0.0231(6) 0.6129(2) 0.5171(2) 0.0336(6) Uani 0.35 1 d P A 2 N8B N 0.1329(6) 0.6605(2) 0.46692(19) 0.0336(6) Uani 0.35 1 d P A 2 H8B H 0.1492 0.6831 0.4445 0.040 Uiso 0.35 1 calc PR A 2 C60B C 0.0111(5) 0.65162(19) 0.48355(19) 0.0336(6) Uani 0.35 1 d PD A 2 C64B C -0.0595(13) 0.6896(5) 0.4590(5) 0.0301(7) Uani 0.35 1 d PD A 2 H64B H -0.1453 0.6863 0.4689 0.036 Uiso 0.35 1 calc PR A 2 C65B C -0.0715(10) 0.7297(5) 0.4278(6) 0.0301(7) Uani 0.35 1 d PD A 2 C68B C 0.0313(12) 0.7516(5) 0.4011(6) 0.0301(7) Uani 0.35 1 d PD A 2 C67B C -0.0987(10) 0.8275(4) 0.3894(4) 0.0301(7) Uani 0.35 1 d PD A 2 C66B C -0.2044(10) 0.7540(5) 0.4170(6) 0.0301(7) Uani 0.35 1 d PD A 2 C69B C -0.0510(16) 0.8496(6) 0.4402(5) 0.0301(7) Uani 0.35 1 d PD A 2 H69D H -0.1247 0.8673 0.4527 0.045 Uiso 0.35 1 calc PR A 2 H69E H 0.0214 0.8737 0.4375 0.045 Uiso 0.35 1 calc PR A 2 H69F H -0.0185 0.8223 0.4635 0.045 Uiso 0.35 1 calc PR A 2 C70B C -0.1283(15) 0.8673(5) 0.3487(6) 0.0301(7) Uani 0.35 1 d PD A 2 H70D H -0.1537 0.8506 0.3162 0.045 Uiso 0.35 1 calc PR A 2 H70E H -0.0489 0.8882 0.3473 0.045 Uiso 0.35 1 calc PR A 2 H70F H -0.2016 0.8890 0.3562 0.045 Uiso 0.35 1 calc PR A 2 O5B O 0.1424(9) 0.7342(4) 0.3996(4) 0.0318(7) Uani 0.35 1 d PD A 2 O6B O -0.3067(9) 0.7346(4) 0.4281(4) 0.0318(7) Uani 0.35 1 d PD A 2 O8B O 0.0023(10) 0.7950(3) 0.3740(4) 0.0318(7) Uani 0.35 1 d PD A 2 O7B O -0.2179(9) 0.7983(4) 0.3910(4) 0.0318(7) Uani 0.35 1 d PD A 2 S1 S 0.16174(16) 0.27853(6) 0.88650(6) 0.0347(4) Uani 1 1 d . . . O9 O 0.0386(4) 0.31020(17) 0.88292(17) 0.0408(11) Uani 1 1 d . . . C71 C 0.2529(8) 0.2890(3) 0.9472(3) 0.057(2) Uani 1 1 d . . . H71A H 0.2659 0.3255 0.9528 0.086 Uiso 1 1 calc R . . H71B H 0.3396 0.2721 0.9495 0.086 Uiso 1 1 calc R . . H71C H 0.2031 0.2750 0.9728 0.086 Uiso 1 1 calc R . . C72 C 0.2733(7) 0.3107(3) 0.8514(3) 0.0440(17) Uani 1 1 d . . . H72A H 0.2380 0.3096 0.8156 0.066 Uiso 1 1 calc R . . H72B H 0.3605 0.2941 0.8569 0.066 Uiso 1 1 calc R . . H72C H 0.2827 0.3462 0.8625 0.066 Uiso 1 1 calc R . . S2 S -0.32065(16) 0.26635(6) 0.90059(6) 0.0325(4) Uani 1 1 d . . . O10 O -0.4371(4) 0.24251(16) 0.92074(17) 0.0390(11) Uani 1 1 d . . . C73 C -0.2310(8) 0.3006(3) 0.9521(3) 0.0502(19) Uani 1 1 d . . . H73A H -0.2864 0.3284 0.9617 0.075 Uiso 1 1 calc R . . H73B H -0.1492 0.3146 0.9420 0.075 Uiso 1 1 calc R . . H73C H -0.2084 0.2776 0.9806 0.075 Uiso 1 1 calc R . . C74 C -0.2006(6) 0.2174(2) 0.8982(2) 0.0359(15) Uani 1 1 d . . . H74A H -0.1762 0.2029 0.9318 0.054 Uiso 1 1 calc R . . H74B H -0.1212 0.2316 0.8864 0.054 Uiso 1 1 calc R . . H74C H -0.2383 0.1907 0.8751 0.054 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 N1 0.025(3) 0.029(3) 0.035(3) 0.000(2) 0.004(2) -0.001(2) N2 0.030(3) 0.046(3) 0.027(3) -0.003(2) 0.007(2) 0.002(2) N3 0.037(3) 0.034(3) 0.030(3) 0.005(2) 0.006(2) -0.003(2) N4 0.031(3) 0.040(3) 0.039(3) -0.003(3) 0.007(2) -0.006(2) C1 0.020(3) 0.041(4) 0.029(3) 0.000(3) 0.005(2) -0.005(3) C2 0.027(3) 0.030(3) 0.040(4) 0.013(3) 0.007(3) 0.002(3) C3 0.029(3) 0.025(3) 0.045(4) -0.001(3) 0.010(3) -0.001(3) C4 0.025(3) 0.031(4) 0.037(4) -0.004(3) 0.007(3) -0.003(3) C5 0.024(3) 0.036(4) 0.035(4) -0.003(3) 0.004(3) -0.006(3) C6 0.043(4) 0.034(4) 0.052(4) -0.017(3) 0.007(3) 0.001(3) C7 0.033(4) 0.048(4) 0.034(4) -0.008(3) 0.008(3) -0.004(3) C8 0.029(3) 0.021(3) 0.031(3) -0.002(3) -0.001(3) 0.004(2) C9 0.024(3) 0.029(3) 0.028(3) 0.000(3) 0.004(2) -0.002(2) C10 0.033(3) 0.026(3) 0.035(4) -0.007(3) 0.007(3) -0.001(3) C11 0.032(4) 0.033(4) 0.033(4) -0.012(3) -0.004(3) 0.003(3) C12 0.016(3) 0.040(4) 0.039(4) -0.004(3) 0.000(2) 0.000(2) C13 0.029(4) 0.054(4) 0.038(4) 0.003(3) -0.001(3) 0.006(3) C14 0.030(4) 0.057(5) 0.057(5) -0.015(4) 0.011(3) -0.019(3) C15 0.018(3) 0.038(4) 0.039(4) -0.004(3) 0.009(2) -0.008(3) C16 0.063(5) 0.043(4) 0.046(4) -0.001(4) 0.013(4) -0.024(4) C17 0.068(5) 0.059(5) 0.037(4) 0.013(4) 0.009(4) -0.020(4) C18 0.029(4) 0.056(5) 0.035(4) -0.001(3) 0.007(3) -0.014(3) C19 0.038(4) 0.064(5) 0.037(4) -0.011(4) 0.011(3) -0.013(3) C20 0.041(4) 0.084(6) 0.075(6) -0.038(5) 0.026(4) -0.013(4) C21 0.048(5) 0.099(7) 0.037(4) -0.006(4) 0.010(3) -0.034(4) C22 0.028(3) 0.056(5) 0.029(3) -0.006(3) -0.002(3) -0.005(3) C23 0.041(4) 0.049(5) 0.032(4) -0.008(3) 0.003(3) 0.000(3) C24 0.038(4) 0.040(4) 0.041(4) -0.001(3) 0.005(3) -0.003(3) C25 0.034(4) 0.037(4) 0.028(3) -0.002(3) 0.001(3) -0.009(3) C26 0.024(3) 0.046(4) 0.035(4) 0.001(3) 0.005(3) -0.007(3) C27 0.033(4) 0.050(4) 0.054(5) -0.011(4) 0.016(3) -0.015(3) C28 0.026(4) 0.067(5) 0.050(4) -0.007(4) -0.002(3) 0.001(3) C29 0.041(4) 0.064(5) 0.035(4) -0.006(4) -0.002(3) 0.012(3) C30 0.045(4) 0.073(5) 0.030(4) -0.013(4) 0.000(3) 0.006(4) C31 0.048(5) 0.091(7) 0.049(5) -0.017(5) 0.002(4) 0.014(5) C32 0.069(6) 0.067(6) 0.037(4) -0.004(4) -0.012(4) 0.018(4) C33 0.056(5) 0.056(5) 0.026(4) -0.009(3) -0.005(3) 0.009(4) C34 0.100(7) 0.092(7) 0.048(5) -0.002(5) -0.009(5) 0.017(6) C35 0.097(7) 0.092(7) 0.054(5) -0.011(5) -0.016(5) 0.049(6) O1 0.047(4) 0.115(5) 0.056(4) -0.004(3) -0.012(3) 0.011(3) O2 0.049(3) 0.092(4) 0.037(3) -0.002(3) 0.005(2) 0.022(3) O3 0.064(4) 0.094(5) 0.037(3) 0.000(3) -0.010(3) 0.018(3) O4 0.064(3) 0.067(4) 0.035(3) -0.002(3) 0.000(2) 0.014(3) N5 0.030(3) 0.031(3) 0.030(3) 0.007(2) 0.004(2) -0.002(2) N6 0.030(3) 0.032(3) 0.026(3) 0.000(2) 0.006(2) -0.005(2) N7 0.024(3) 0.024(3) 0.027(3) -0.001(2) 0.011(2) -0.0019(19) C36 0.021(3) 0.035(4) 0.038(4) -0.004(3) 0.000(3) 0.001(3) C37 0.045(4) 0.035(4) 0.069(5) 0.009(4) -0.003(4) -0.003(3) C38 0.050(5) 0.050(5) 0.059(5) 0.026(4) 0.002(4) 0.009(4) C39 0.024(3) 0.049(4) 0.032(4) 0.015(3) 0.007(3) 0.003(3) C40 0.027(4) 0.080(6) 0.029(4) 0.011(4) 0.003(3) -0.003(3) C41 0.044(5) 0.123(8) 0.038(4) 0.038(5) -0.006(3) -0.027(5) C42 0.039(4) 0.113(7) 0.036(4) -0.018(4) 0.011(3) 0.007(4) C43 0.026(3) 0.053(4) 0.024(3) 0.008(3) 0.004(2) 0.008(3) C44 0.049(4) 0.044(4) 0.030(4) -0.008(3) 0.009(3) 0.013(3) C45 0.036(4) 0.038(4) 0.037(4) -0.002(3) 0.007(3) 0.002(3) C46 0.026(3) 0.033(3) 0.024(3) 0.005(3) 0.004(2) -0.003(2) C47 0.024(3) 0.039(4) 0.030(3) 0.004(3) 0.004(2) 0.000(3) C48 0.031(3) 0.048(4) 0.032(4) 0.005(3) 0.003(3) 0.001(3) C49 0.029(3) 0.042(4) 0.033(4) -0.002(3) 0.004(3) -0.014(3) C50 0.021(3) 0.030(3) 0.031(3) 0.003(3) 0.010(2) 0.000(2) C51 0.033(3) 0.033(4) 0.024(3) 0.004(3) 0.008(2) 0.006(3) C52 0.044(4) 0.028(4) 0.033(4) -0.004(3) 0.012(3) 0.002(3) C53 0.029(3) 0.029(3) 0.031(3) -0.004(3) 0.012(3) -0.002(2) C54 0.033(3) 0.034(4) 0.028(3) 0.003(3) 0.011(3) 0.000(3) C55 0.044(4) 0.047(4) 0.022(3) 0.001(3) 0.014(3) 0.007(3) C56 0.026(3) 0.042(4) 0.032(3) 0.010(3) 0.006(3) 0.000(3) C61 0.027(3) 0.041(4) 0.028(3) -0.008(3) 0.000(2) 0.003(3) C62 0.031(4) 0.061(5) 0.052(4) -0.018(4) 0.010(3) -0.010(3) C63 0.025(3) 0.048(4) 0.037(4) 0.006(3) 0.013(3) 0.007(3) C57A 0.0456(16) 0.0293(15) 0.0249(14) -0.0021(11) 0.0017(11) 0.0024(12) C58A 0.0456(16) 0.0293(15) 0.0249(14) -0.0021(11) 0.0017(11) 0.0024(12) C59A 0.0456(16) 0.0293(15) 0.0249(14) -0.0021(11) 0.0017(11) 0.0024(12) C60A 0.0456(16) 0.0293(15) 0.0249(14) -0.0021(11) 0.0017(11) 0.0024(12) N8A 0.0456(16) 0.0293(15) 0.0249(14) -0.0021(11) 0.0017(11) 0.0024(12) C64A 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C65A 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C68A 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C67A 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C66A 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C69A 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C70A 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) O5A 0.0261(16) 0.0359(17) 0.0347(17) 0.0071(13) 0.0087(13) -0.0003(12) O6A 0.0261(16) 0.0359(17) 0.0347(17) 0.0071(13) 0.0087(13) -0.0003(12) O8A 0.0261(16) 0.0359(17) 0.0347(17) 0.0071(13) 0.0087(13) -0.0003(12) O7A 0.0261(16) 0.0359(17) 0.0347(17) 0.0071(13) 0.0087(13) -0.0003(12) C57B 0.0456(16) 0.0293(15) 0.0249(14) -0.0021(11) 0.0017(11) 0.0024(12) C58B 0.0456(16) 0.0293(15) 0.0249(14) -0.0021(11) 0.0017(11) 0.0024(12) C59B 0.0456(16) 0.0293(15) 0.0249(14) -0.0021(11) 0.0017(11) 0.0024(12) N8B 0.0456(16) 0.0293(15) 0.0249(14) -0.0021(11) 0.0017(11) 0.0024(12) C60B 0.0456(16) 0.0293(15) 0.0249(14) -0.0021(11) 0.0017(11) 0.0024(12) C64B 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C65B 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C68B 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C67B 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C66B 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C69B 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) C70B 0.0303(17) 0.0308(18) 0.0298(17) 0.0061(13) 0.0058(12) -0.0006(13) O5B 0.0261(16) 0.0359(17) 0.0347(17) 0.0071(13) 0.0087(13) -0.0003(12) O6B 0.0261(16) 0.0359(17) 0.0347(17) 0.0071(13) 0.0087(13) -0.0003(12) O8B 0.0261(16) 0.0359(17) 0.0347(17) 0.0071(13) 0.0087(13) -0.0003(12) O7B 0.0261(16) 0.0359(17) 0.0347(17) 0.0071(13) 0.0087(13) -0.0003(12) S1 0.0356(9) 0.0293(9) 0.0400(9) 0.0023(7) 0.0079(7) 0.0000(7) O9 0.024(2) 0.045(3) 0.055(3) 0.009(2) 0.010(2) 0.0054(19) C71 0.059(5) 0.072(6) 0.040(4) 0.008(4) 0.005(4) 0.014(4) C72 0.044(4) 0.041(4) 0.049(4) 0.001(3) 0.015(3) -0.004(3) S2 0.0358(9) 0.0277(8) 0.0344(9) 0.0010(7) 0.0068(7) 0.0001(6) O10 0.033(2) 0.036(3) 0.049(3) -0.004(2) 0.010(2) -0.0019(19) C73 0.058(5) 0.043(4) 0.053(5) -0.012(4) 0.019(4) -0.012(3) C74 0.034(4) 0.035(4) 0.040(4) -0.005(3) 0.009(3) 0.000(3) _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 C1 1.373(8) . ? N1 C4 1.392(8) . ? N2 C8 1.317(7) . ? N2 C11 1.387(8) . ? N3 C15 1.387(8) . ? N3 C18 1.393(8) . ? N4 C25 1.369(8) . ? N4 C22 1.382(8) . ? C1 C2 1.382(9) . ? C1 C26 1.506(9) . ? C2 C3 1.419(9) . ? C3 C4 1.359(9) . ? C4 C5 1.502(9) . ? C5 C8 1.506(8) . ? C5 C6 1.540(9) . ? C5 C7 1.541(9) . ? C8 C9 1.400(8) . ? C9 C10 1.391(8) . ? C10 C11 1.421(9) . ? C10 C12 1.523(8) . ? C11 C29 1.394(9) . ? C12 C15 1.504(9) . ? C12 C14 1.536(9) . ? C12 C13 1.550(9) . ? C15 C16 1.363(9) . ? C16 C17 1.404(10) . ? C17 C18 1.360(10) . ? C18 C19 1.500(9) . ? C19 C22 1.519(9) . ? C19 C20 1.547(11) . ? C19 C21 1.547(10) . ? C22 C23 1.353(10) . ? C23 C24 1.421(9) . ? C24 C25 1.377(9) . ? C25 C26 1.512(9) . ? C26 C28 1.536(9) . ? C26 C27 1.537(9) . ? C29 C30 1.347(7) . ? C30 C33 1.464(8) . ? C30 C31 1.471(9) . ? C31 O1 1.217(8) . ? C31 O3 1.348(8) . ? C32 O4 1.434(7) . ? C32 O3 1.437(8) . ? C32 C35 1.505(9) . ? C32 C34 1.508(8) . ? C33 O2 1.228(7) . ? C33 O4 1.365(7) . ? N5 C39 1.371(7) . ? N5 C36 1.373(8) . ? N6 C46 1.365(7) . ? N6 C43 1.385(8) . ? N7 C53 1.370(7) . ? N7 C50 1.373(7) . ? C36 C37 1.350(9) . ? C36 C61 1.509(9) . ? C37 C38 1.423(11) . ? C38 C39 1.351(10) . ? C39 C40 1.501(10) . ? C40 C43 1.519(9) . ? C40 C41 1.529(10) . ? C40 C42 1.549(11) . ? C43 C44 1.366(9) . ? C44 C45 1.400(9) . ? C45 C46 1.368(9) . ? C46 C47 1.525(8) . ? C47 C50 1.503(8) . ? C47 C49 1.534(8) . ? C47 C48 1.546(9) . ? C50 C51 1.370(8) . ? C51 C52 1.433(9) . ? C52 C53 1.351(9) . ? C53 C54 1.520(9) . ? C54 C57A 1.513(9) . ? C54 C56 1.546(8) . ? C54 C55 1.552(8) . ? C61 C59A 1.499(9) . ? C61 C63 1.533(8) . ? C61 C62 1.551(9) . ? C57A C58A 1.379(9) . ? C57A C60A 1.420(8) . ? C58A C59A 1.403(9) . ? C59A N8A 1.354(8) . ? C60A C64A 1.369(7) . ? C60A N8A 1.391(8) . ? C64A C65A 1.357(6) . ? C65A C66A 1.460(9) . ? C65A C68A 1.478(9) . ? C68A O5A 1.222(8) . ? C68A O8A 1.351(8) . ? C67A O8A 1.434(8) . ? C67A O7A 1.438(8) . ? C67A C69A 1.503(9) . ? C67A C70A 1.517(8) . ? C66A O6A 1.225(8) . ? C66A O7A 1.368(8) . ? C64B C65B 1.343(6) . ? C65B C68B 1.465(10) . ? C65B C66B 1.484(10) . ? C68B O5B 1.222(10) . ? C68B O8B 1.365(10) . ? C67B O8B 1.438(10) . ? C67B O7B 1.438(9) . ? C67B C69B 1.503(10) . ? C67B C70B 1.515(10) . ? C66B O6B 1.230(9) . ? C66B O7B 1.358(9) . ? S1 O9 1.494(4) . ? S1 C71 1.782(8) . ? S1 C72 1.786(7) . ? S2 O10 1.504(4) . ? S2 C74 1.781(6) . ? S2 C73 1.790(7) . ? 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 N1 C4 110.3(5) . . ? C8 N2 C11 111.2(5) . . ? C15 N3 C18 110.6(5) . . ? C25 N4 C22 110.7(6) . . ? N1 C1 C2 107.2(5) . . ? N1 C1 C26 122.2(5) . . ? C2 C1 C26 130.5(6) . . ? C1 C2 C3 106.9(5) . . ? C4 C3 C2 109.2(5) . . ? C3 C4 N1 106.4(5) . . ? C3 C4 C5 132.2(6) . . ? N1 C4 C5 121.4(5) . . ? C4 C5 C8 108.5(5) . . ? C4 C5 C6 108.5(5) . . ? C8 C5 C6 107.8(5) . . ? C4 C5 C7 111.4(5) . . ? C8 C5 C7 111.3(5) . . ? C6 C5 C7 109.3(5) . . ? N2 C8 C9 107.5(5) . . ? N2 C8 C5 121.7(5) . . ? C9 C8 C5 130.5(5) . . ? C10 C9 C8 109.0(5) . . ? C9 C10 C11 105.7(5) . . ? C9 C10 C12 125.7(5) . . ? C11 C10 C12 128.6(5) . . ? N2 C11 C29 123.0(6) . . ? N2 C11 C10 106.6(5) . . ? C29 C11 C10 130.4(6) . . ? C15 C12 C10 110.0(5) . . ? C15 C12 C14 109.5(5) . . ? C10 C12 C14 107.6(5) . . ? C15 C12 C13 107.0(5) . . ? C10 C12 C13 113.3(5) . . ? C14 C12 C13 109.4(5) . . ? C16 C15 N3 106.0(6) . . ? C16 C15 C12 132.2(6) . . ? N3 C15 C12 121.9(5) . . ? C15 C16 C17 108.7(6) . . ? C18 C17 C16 109.0(6) . . ? C17 C18 N3 105.7(6) . . ? C17 C18 C19 133.0(7) . . ? N3 C18 C19 121.3(6) . . ? C18 C19 C22 110.6(5) . . ? C18 C19 C20 109.7(6) . . ? C22 C19 C20 108.5(6) . . ? C18 C19 C21 109.3(6) . . ? C22 C19 C21 109.8(5) . . ? C20 C19 C21 108.8(6) . . ? C23 C22 N4 106.4(6) . . ? C23 C22 C19 134.0(6) . . ? N4 C22 C19 119.6(6) . . ? C22 C23 C24 109.1(6) . . ? C25 C24 C23 106.9(6) . . ? N4 C25 C24 107.0(6) . . ? N4 C25 C26 120.1(6) . . ? C24 C25 C26 132.6(6) . . ? C1 C26 C25 110.2(5) . . ? C1 C26 C28 108.9(5) . . ? C25 C26 C28 108.6(5) . . ? C1 C26 C27 109.8(5) . . ? C25 C26 C27 110.3(6) . . ? C28 C26 C27 108.9(5) . . ? C30 C29 C11 135.8(7) . . ? C29 C30 C33 126.6(6) . . ? C29 C30 C31 117.7(6) . . ? C33 C30 C31 115.7(5) . . ? O1 C31 O3 118.8(6) . . ? O1 C31 C30 122.5(7) . . ? O3 C31 C30 118.7(6) . . ? O4 C32 O3 108.8(5) . . ? O4 C32 C35 110.3(6) . . ? O3 C32 C35 109.8(6) . . ? O4 C32 C34 107.0(6) . . ? O3 C32 C34 107.8(6) . . ? C35 C32 C34 113.0(7) . . ? O2 C33 O4 115.0(6) . . ? O2 C33 C30 127.4(6) . . ? O4 C33 C30 117.6(5) . . ? C31 O3 C32 117.6(5) . . ? C33 O4 C32 119.0(5) . . ? C39 N5 C36 111.7(5) . . ? C46 N6 C43 110.0(5) . . ? C53 N7 C50 110.4(5) . . ? C37 C36 N5 105.7(6) . . ? C37 C36 C61 134.0(6) . . ? N5 C36 C61 120.3(5) . . ? C36 C37 C38 108.5(7) . . ? C39 C38 C37 108.1(6) . . ? C38 C39 N5 105.9(6) . . ? C38 C39 C40 132.1(6) . . ? N5 C39 C40 121.8(6) . . ? C39 C40 C43 111.7(5) . . ? C39 C40 C41 110.6(7) . . ? C43 C40 C41 108.9(5) . . ? C39 C40 C42 109.1(5) . . ? C43 C40 C42 107.2(6) . . ? C41 C40 C42 109.1(6) . . ? C44 C43 N6 106.2(5) . . ? C44 C43 C40 132.6(6) . . ? N6 C43 C40 121.1(6) . . ? C43 C44 C45 108.9(6) . . ? C46 C45 C44 107.4(6) . . ? N6 C46 C45 107.6(5) . . ? N6 C46 C47 121.0(5) . . ? C45 C46 C47 131.5(6) . . ? C50 C47 C46 109.1(5) . . ? C50 C47 C49 110.8(5) . . ? C46 C47 C49 109.3(5) . . ? C50 C47 C48 109.4(5) . . ? C46 C47 C48 110.6(5) . . ? C49 C47 C48 107.7(5) . . ? C51 C50 N7 106.2(5) . . ? C51 C50 C47 131.0(5) . . ? N7 C50 C47 122.7(5) . . ? C50 C51 C52 108.4(5) . . ? C53 C52 C51 106.6(5) . . ? C52 C53 N7 108.4(5) . . ? C52 C53 C54 129.8(6) . . ? N7 C53 C54 121.6(5) . . ? C57A C54 C53 108.8(5) . . ? C57A C54 C56 113.5(5) . . ? C53 C54 C56 109.3(5) . . ? C57A C54 C55 108.1(5) . . ? C53 C54 C55 109.3(5) . . ? C56 C54 C55 107.8(5) . . ? C59A C61 C36 109.8(5) . . ? C59A C61 C63 112.5(5) . . ? C36 C61 C63 108.9(5) . . ? C59A C61 C62 108.8(5) . . ? C36 C61 C62 108.9(6) . . ? C63 C61 C62 107.9(5) . . ? C58A C57A C60A 106.5(6) . . ? C58A C57A C54 125.1(6) . . ? C60A C57A C54 128.3(6) . . ? C57A C58A C59A 109.3(6) . . ? N8A C59A C58A 107.2(5) . . ? N8A C59A C61 124.4(6) . . ? C58A C59A C61 128.4(6) . . ? C64A C60A N8A 113.9(5) . . ? C64A C60A C57A 139.1(6) . . ? N8A C60A C57A 107.0(5) . . ? C59A N8A C60A 109.8(5) . . ? C65A C64A C60A 140.1(7) . . ? C64A C65A C66A 128.1(6) . . ? C64A C65A C68A 115.8(6) . . ? C66A C65A C68A 116.1(5) . . ? O5A C68A O8A 118.2(6) . . ? O5A C68A C65A 123.2(6) . . ? O8A C68A C65A 118.5(6) . . ? O8A C67A O7A 110.1(6) . . ? O8A C67A C69A 109.7(6) . . ? O7A C67A C69A 110.5(6) . . ? O8A C67A C70A 105.6(6) . . ? O7A C67A C70A 105.9(6) . . ? C69A C67A C70A 114.9(6) . . ? O6A C66A O7A 114.6(6) . . ? O6A C66A C65A 126.6(6) . . ? O7A C66A C65A 118.7(6) . . ? C68A O8A C67A 118.0(6) . . ? C66A O7A C67A 116.8(6) . . ? C64B C65B C68B 127.3(9) . . ? C64B C65B C66B 117.5(8) . . ? C68B C65B C66B 115.1(7) . . ? O5B C68B O8B 115.2(9) . . ? O5B C68B C65B 126.3(9) . . ? O8B C68B C65B 118.4(8) . . ? O8B C67B O7B 109.2(8) . . ? O8B C67B C69B 109.9(9) . . ? O7B C67B C69B 110.1(9) . . ? O8B C67B C70B 106.3(9) . . ? O7B C67B C70B 107.9(9) . . ? C69B C67B C70B 113.3(9) . . ? O6B C66B O7B 117.0(9) . . ? O6B C66B C65B 123.3(9) . . ? O7B C66B C65B 119.6(8) . . ? C68B O8B C67B 116.9(8) . . ? C66B O7B C67B 116.7(8) . . ? O9 S1 C71 107.2(3) . . ? O9 S1 C72 106.7(3) . . ? C71 S1 C72 97.2(4) . . ? O10 S2 C74 106.7(3) . . ? O10 S2 C73 105.7(3) . . ? C74 S2 C73 96.7(3) . . ? 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 H1 O9 0.88 2.15 3.020(7) 168.2 . N2 H2 O2 0.88 1.88 2.658(7) 146.0 . N7 H7 O10 0.88 2.11 2.991(6) 177.2 2_556 N8A H8A O6A 0.88 1.80 2.628(8) 154.9 . N8B H8B O5B 0.88 1.80 2.664(11) 166.3 . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.10 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.617 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.069 #===END