# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics # This journal is © The Owner Societies 2012 data_global _journal_name_full Phys.Chem.Chem.Phys.(PCCP) _journal_coden_cambridge 1326 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name A.Benniston 'Helge Lemmetyinen' 'Jerry Hagon' 'Xiaoyan He' 'Nikolai Tkachenko' 'William Clegg' 'Ross Harrington' _publ_contact_author_email a.c.benniston@ncl.ac.uk data_acb24 _database_code_depnum_ccdc_archive 'CCDC 861599' #TrackingRef '- ACB24.CIF' # start Validation Reply Form _vrf_PLAT411_acb24 ; PROBLEM: Short Inter H...H Contact H38A .. H38B .. 1.60 Ang. RESPONSE: Incorrect alert - this is an intramolecular contact within an appropriately calculated ideal methyl group. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; 7-(Methylsulfinyl)-14-phenylbenzo[5,6]tetraceno[1,12,11,10-jklmna]acridin-14-ium hexafluorophosphate(V), acetonitrile solvate ; _chemical_name_common ; 7-(Methylsulfinyl)-14-phenylbenzo(5,6)tetraceno(1,12,11,10- jklmna)acridin-14-ium hexafluorophosphate(V), acetonitrile solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C34 H20 N O S +,P F6 -,C2 H3 N' _chemical_formula_sum 'C36 H23 F6 N2 O P S' _chemical_formula_weight 676.59 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0930 0.0842 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1137 0.1104 '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 'P 21/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 13.773(4) _cell_length_b 6.7999(18) _cell_length_c 15.291(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.715(3) _cell_angle_gamma 90.00 _cell_volume 1422.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2863 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 28.57 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.948 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6709 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX2 CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10624 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 23.54 _reflns_number_total 2705 _reflns_number_gt 2070 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.1474P)^2^+0.7861P] 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 2705 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.2342 _refine_ls_wR_factor_gt 0.2157 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 C1 C 0.4626(3) 0.2500 0.5291(3) 0.0345(8) Uani 1 2 d S . . C2 C 0.3872(3) 0.2500 0.5842(3) 0.0387(9) Uani 1 2 d S . . C3 C 0.4130(3) 0.2500 0.6770(3) 0.0429(10) Uani 1 2 d S . . H3 H 0.3625 0.2500 0.7143 0.051 Uiso 1 2 calc SR . . C4 C 0.5073(3) 0.2500 0.7138(3) 0.0449(10) Uani 1 2 d S . . H4 H 0.5224 0.2500 0.7761 0.054 Uiso 1 2 calc SR . . C5 C 0.5840(3) 0.2500 0.6587(2) 0.0387(9) Uani 1 2 d S . . C6 C 0.5621(3) 0.2500 0.5670(2) 0.0346(9) Uani 1 2 d S . . N7 N 0.6798(2) 0.2500 0.6957(2) 0.0423(8) Uani 1 2 d S . . C8 C 0.7559(3) 0.2500 0.6453(3) 0.0405(9) Uani 1 2 d S . . C9 C 0.7362(3) 0.2500 0.5531(2) 0.0359(9) Uani 1 2 d S . . C10 C 0.6383(3) 0.2500 0.5128(2) 0.0325(8) Uani 1 2 d S . . C11 C 0.8542(3) 0.2500 0.6856(3) 0.0528(12) Uani 1 2 d S . . H11 H 0.8677 0.2500 0.7480 0.063 Uiso 1 2 calc SR . . C12 C 0.9280(3) 0.2500 0.6352(3) 0.0556(12) Uani 1 2 d S . . H12 H 0.9934 0.2500 0.6631 0.067 Uiso 1 2 calc SR . . C13 C 0.9116(3) 0.2500 0.5416(3) 0.0492(11) Uani 1 2 d S . . C14 C 0.8147(3) 0.2500 0.4994(3) 0.0377(9) Uani 1 2 d S . . C15 C 0.7960(3) 0.2500 0.4076(2) 0.0383(9) Uani 1 2 d S . . C16 C 0.6952(3) 0.2500 0.3658(2) 0.0365(9) Uani 1 2 d S . . C17 C 0.6175(3) 0.2500 0.4196(2) 0.0347(8) Uani 1 2 d S . . C18 C 0.5186(3) 0.2500 0.3806(2) 0.0376(9) Uani 1 2 d S . . C19 C 0.4393(3) 0.2500 0.4368(2) 0.0369(9) Uani 1 2 d S . . C20 C 0.9882(3) 0.2500 0.4910(3) 0.0594(13) Uani 1 2 d S . . H20 H 1.0537 0.2500 0.5186 0.071 Uiso 1 2 calc SR . . C21 C 0.9698(3) 0.2500 0.4003(3) 0.0586(13) Uani 1 2 d S . . H21 H 1.0230 0.2500 0.3660 0.070 Uiso 1 2 calc SR . . C22 C 0.8758(3) 0.2500 0.3588(3) 0.0459(10) Uani 1 2 d S . . H22 H 0.8648 0.2500 0.2963 0.055 Uiso 1 2 calc SR . . C23 C 0.3417(3) 0.2500 0.4027(3) 0.0419(10) Uani 1 2 d S . . H23 H 0.3249 0.2500 0.3406 0.050 Uiso 1 2 calc SR . . C24 C 0.2674(3) 0.2500 0.4572(3) 0.0440(10) Uani 1 2 d S . . H24 H 0.2010 0.2500 0.4319 0.053 Uiso 1 2 calc SR . . C25 C 0.2891(3) 0.2500 0.5468(3) 0.0426(10) Uani 1 2 d S . . H25 H 0.2381 0.2500 0.5836 0.051 Uiso 1 2 calc SR . . C26 C 0.6724(3) 0.2500 0.2755(3) 0.0479(10) Uani 1 2 d S . . H26 H 0.7233 0.2500 0.2386 0.057 Uiso 1 2 calc SR . . C27 C 0.5769(3) 0.2500 0.2389(3) 0.0572(13) Uani 1 2 d S . . C28 C 0.5009(3) 0.2500 0.2897(3) 0.0568(13) Uani 1 2 d S . . H28 H 0.4355 0.2500 0.2621 0.068 Uiso 1 2 calc SR . . C29 C 0.7021(3) 0.2500 0.7915(3) 0.0510(11) Uani 1 2 d S . . C30 C 0.7136(3) 0.4233(7) 0.8354(2) 0.0781(12) Uani 1 1 d . . . H30 H 0.7050 0.5442 0.8043 0.094 Uiso 1 1 calc R . . C31 C 0.7377(4) 0.4228(9) 0.9253(2) 0.1005(17) Uani 1 1 d . . . H31 H 0.7459 0.5435 0.9566 0.121 Uiso 1 1 calc R . . C32 C 0.7496(4) 0.2500 0.9689(3) 0.093(2) Uani 1 2 d S . . H32 H 0.7666 0.2500 1.0309 0.112 Uiso 1 2 calc SR . . S33 S 0.54917(13) 0.1866(3) 0.12237(10) 0.0669(9) Uani 0.50 1 d P A -1 O34 O 0.4447(4) 0.1512(12) 0.1068(3) 0.126(4) Uani 0.50 1 d P A -1 C35 C 0.5694(7) 0.4378(14) 0.0892(5) 0.083(3) Uani 0.50 1 d P A -1 H35A H 0.5590 0.4473 0.0249 0.124 Uiso 0.50 1 calc PR A -1 H35B H 0.6365 0.4769 0.1103 0.124 Uiso 0.50 1 calc PR A -1 H35C H 0.5235 0.5252 0.1146 0.124 Uiso 0.50 1 calc PR A -1 N36 N 0.1347(4) 0.2500 1.2438(3) 0.0719(13) Uani 1 2 d S . . C37 C 0.0834(4) 0.2500 1.1806(3) 0.0650(14) Uani 1 2 d S . . C38 C 0.0173(5) 0.2500 1.0984(4) 0.088(2) Uani 1 2 d S . . H38A H -0.0506 0.2500 1.1118 0.106 Uiso 1 2 calc SR . . H38B H 0.0291 0.1323 1.0641 0.106 Uiso 0.50 1 calc PR . . H38C H 0.0291 0.3677 1.0641 0.106 Uiso 0.50 1 calc PR . . P P 0.16112(9) 0.2500 0.83155(7) 0.0548(5) Uani 1 2 d S . . F1 F 0.1651(3) 0.4785(5) 0.8338(2) 0.1368(14) Uani 1 1 d . . . F2 F 0.0481(2) 0.2500 0.8182(2) 0.137(2) Uani 1 2 d S . . F3 F 0.2760(3) 0.2500 0.8455(2) 0.1230(18) Uani 1 2 d S . . F4 F 0.1672(2) 0.2500 0.72902(17) 0.1063(15) Uani 1 2 d S . . F5 F 0.1565(2) 0.2500 0.93415(16) 0.0827(11) Uani 1 2 d S . . 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 0.035(2) 0.0305(19) 0.040(2) 0.000 0.0116(16) 0.000 C2 0.043(2) 0.036(2) 0.040(2) 0.000 0.0176(17) 0.000 C3 0.041(2) 0.048(2) 0.043(2) 0.000 0.0227(17) 0.000 C4 0.052(2) 0.058(3) 0.0279(19) 0.000 0.0197(17) 0.000 C5 0.040(2) 0.044(2) 0.034(2) 0.000 0.0111(16) 0.000 C6 0.042(2) 0.036(2) 0.0283(19) 0.000 0.0149(15) 0.000 N7 0.0439(19) 0.061(2) 0.0235(16) 0.000 0.0110(13) 0.000 C8 0.039(2) 0.053(2) 0.031(2) 0.000 0.0108(16) 0.000 C9 0.040(2) 0.042(2) 0.0282(19) 0.000 0.0131(15) 0.000 C10 0.0337(19) 0.0326(19) 0.0327(19) 0.000 0.0106(15) 0.000 C11 0.049(2) 0.084(3) 0.026(2) 0.000 0.0074(17) 0.000 C12 0.036(2) 0.094(4) 0.037(2) 0.000 0.0076(17) 0.000 C13 0.044(2) 0.068(3) 0.038(2) 0.000 0.0149(18) 0.000 C14 0.039(2) 0.043(2) 0.034(2) 0.000 0.0149(16) 0.000 C15 0.042(2) 0.042(2) 0.033(2) 0.000 0.0144(16) 0.000 C16 0.041(2) 0.039(2) 0.0313(19) 0.000 0.0129(16) 0.000 C17 0.043(2) 0.035(2) 0.0279(18) 0.000 0.0127(15) 0.000 C18 0.037(2) 0.041(2) 0.036(2) 0.000 0.0082(16) 0.000 C19 0.042(2) 0.035(2) 0.035(2) 0.000 0.0103(16) 0.000 C20 0.034(2) 0.099(4) 0.048(3) 0.000 0.0166(19) 0.000 C21 0.041(2) 0.099(4) 0.039(2) 0.000 0.0207(18) 0.000 C22 0.044(2) 0.061(3) 0.036(2) 0.000 0.0184(17) 0.000 C23 0.040(2) 0.045(2) 0.042(2) 0.000 0.0085(17) 0.000 C24 0.037(2) 0.048(2) 0.049(2) 0.000 0.0095(17) 0.000 C25 0.038(2) 0.040(2) 0.053(2) 0.000 0.0208(18) 0.000 C26 0.048(2) 0.067(3) 0.031(2) 0.000 0.0159(17) 0.000 C27 0.046(2) 0.098(4) 0.030(2) 0.000 0.0098(18) 0.000 C28 0.042(2) 0.096(4) 0.033(2) 0.000 0.0058(18) 0.000 C29 0.043(2) 0.084(3) 0.028(2) 0.000 0.0109(17) 0.000 C30 0.092(3) 0.109(3) 0.0347(17) -0.0159(19) 0.0155(17) -0.033(2) C31 0.115(4) 0.154(5) 0.035(2) -0.022(2) 0.016(2) -0.050(3) C32 0.063(3) 0.190(8) 0.029(3) 0.000 0.012(2) 0.000 S33 0.0615(10) 0.115(3) 0.0247(7) -0.0071(8) 0.0070(6) -0.0108(9) O34 0.083(4) 0.260(13) 0.036(2) -0.020(4) 0.011(2) -0.042(5) C35 0.114(7) 0.105(7) 0.034(3) 0.029(4) 0.029(4) 0.021(5) N36 0.069(3) 0.100(4) 0.051(3) 0.000 0.024(2) 0.000 C37 0.059(3) 0.093(4) 0.049(3) 0.000 0.030(2) 0.000 C38 0.078(4) 0.141(6) 0.048(3) 0.000 0.021(3) 0.000 P 0.0539(8) 0.0898(10) 0.0226(6) 0.000 0.0131(5) 0.000 F1 0.212(4) 0.095(2) 0.120(3) 0.0253(17) 0.092(3) 0.012(2) F2 0.0494(19) 0.322(7) 0.0421(18) 0.000 0.0083(14) 0.000 F3 0.063(2) 0.253(6) 0.054(2) 0.000 0.0112(16) 0.000 F4 0.070(2) 0.229(5) 0.0229(14) 0.000 0.0194(13) 0.000 F5 0.095(2) 0.131(3) 0.0252(14) 0.000 0.0183(13) 0.000 _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 1.413(5) . ? C1 C6 1.423(5) . ? C1 C19 1.410(5) . ? C2 C3 1.421(6) . ? C2 C25 1.404(6) . ? C3 H3 0.950 . ? C3 C4 1.355(6) . ? C4 H4 0.950 . ? C4 C5 1.426(5) . ? C5 C6 1.399(5) . ? C5 N7 1.374(5) . ? C6 C10 1.412(5) . ? N7 C8 1.373(5) . ? N7 C29 1.461(5) . ? C8 C9 1.403(5) . ? C8 C11 1.420(6) . ? C9 C10 1.416(5) . ? C9 C14 1.432(5) . ? C10 C17 1.421(5) . ? C11 H11 0.950 . ? C11 C12 1.347(6) . ? C12 H12 0.950 . ? C12 C13 1.422(6) . ? C13 C14 1.413(6) . ? C13 C20 1.379(6) . ? C14 C15 1.397(5) . ? C15 C16 1.460(6) . ? C15 C22 1.398(5) . ? C16 C17 1.424(5) . ? C16 C26 1.380(5) . ? C17 C18 1.421(5) . ? C18 C19 1.467(5) . ? C18 C28 1.383(6) . ? C19 C23 1.384(5) . ? C20 H20 0.950 . ? C20 C21 1.381(6) . ? C21 H21 0.950 . ? C21 C22 1.374(6) . ? C22 H22 0.950 . ? C23 H23 0.950 . ? C23 C24 1.393(6) . ? C24 H24 0.950 . ? C24 C25 1.368(6) . ? C25 H25 0.950 . ? C26 H26 0.950 . ? C26 C27 1.367(6) . ? C27 C28 1.375(6) . ? C27 S33 1.829(4) . ? C28 H28 0.950 . ? C29 C30 1.356(5) . ? C29 C30 1.356(5) 4_565 ? C30 H30 0.950 . ? C30 C31 1.375(5) . ? C31 H31 0.950 . ? C31 C32 1.352(6) . ? C32 C31 1.352(6) 4_565 ? C32 H32 0.950 . ? S33 O34 1.450(6) . ? S33 C35 1.813(10) . ? C35 H35A 0.980 . ? C35 H35B 0.980 . ? C35 H35C 0.980 . ? N36 C37 1.129(7) . ? C37 C38 1.463(8) . ? C38 H38A 0.980 . ? C38 H38B 0.980 . ? C38 H38C 0.980 . ? P F1 1.555(3) . ? P F1 1.555(3) 4_565 ? P F2 1.546(3) . ? P F3 1.571(4) . ? P F4 1.580(3) . ? P F5 1.578(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 C2 C1 C6 119.7(4) . . ? C2 C1 C19 120.0(4) . . ? C6 C1 C19 120.3(3) . . ? C1 C2 C3 118.7(4) . . ? C1 C2 C25 119.8(4) . . ? C3 C2 C25 121.5(4) . . ? C2 C3 H3 119.0 . . ? C2 C3 C4 122.1(4) . . ? H3 C3 C4 119.0 . . ? C3 C4 H4 120.2 . . ? C3 C4 C5 119.6(4) . . ? H4 C4 C5 120.2 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 N7 119.8(4) . . ? C6 C5 N7 119.8(3) . . ? C1 C6 C5 119.5(3) . . ? C1 C6 C10 120.5(3) . . ? C5 C6 C10 120.0(4) . . ? C5 N7 C8 121.9(3) . . ? C5 N7 C29 119.5(3) . . ? C8 N7 C29 118.6(3) . . ? N7 C8 C9 119.6(4) . . ? N7 C8 C11 120.5(4) . . ? C9 C8 C11 119.9(4) . . ? C8 C9 C10 120.0(3) . . ? C8 C9 C14 120.3(4) . . ? C10 C9 C14 119.6(4) . . ? C6 C10 C9 118.7(3) . . ? C6 C10 C17 120.8(3) . . ? C9 C10 C17 120.5(3) . . ? C8 C11 H11 120.1 . . ? C8 C11 C12 119.7(4) . . ? H11 C11 C12 120.1 . . ? C11 C12 H12 118.8 . . ? C11 C12 C13 122.3(4) . . ? H12 C12 C13 118.8 . . ? C12 C13 C14 119.3(4) . . ? C12 C13 C20 121.5(4) . . ? C14 C13 C20 119.2(4) . . ? C9 C14 C13 118.3(4) . . ? C9 C14 C15 120.9(4) . . ? C13 C14 C15 120.8(4) . . ? C14 C15 C16 119.6(3) . . ? C14 C15 C22 118.2(4) . . ? C16 C15 C22 122.2(4) . . ? C15 C16 C17 119.2(3) . . ? C15 C16 C26 122.1(3) . . ? C17 C16 C26 118.7(4) . . ? C10 C17 C16 120.2(4) . . ? C10 C17 C18 119.4(3) . . ? C16 C17 C18 120.4(3) . . ? C17 C18 C19 119.9(3) . . ? C17 C18 C28 117.9(4) . . ? C19 C18 C28 122.2(4) . . ? C1 C19 C18 119.2(3) . . ? C1 C19 C23 118.4(3) . . ? C18 C19 C23 122.4(4) . . ? C13 C20 H20 120.0 . . ? C13 C20 C21 120.1(4) . . ? H20 C20 C21 120.0 . . ? C20 C21 H21 119.5 . . ? C20 C21 C22 121.0(4) . . ? H21 C21 C22 119.5 . . ? C15 C22 C21 120.7(4) . . ? C15 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C19 C23 H23 119.2 . . ? C19 C23 C24 121.5(4) . . ? H23 C23 C24 119.2 . . ? C23 C24 H24 119.7 . . ? C23 C24 C25 120.6(4) . . ? H24 C24 C25 119.7 . . ? C2 C25 C24 119.7(4) . . ? C2 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C16 C26 H26 119.8 . . ? C16 C26 C27 120.4(4) . . ? H26 C26 C27 119.8 . . ? C26 C27 C28 121.8(4) . . ? C26 C27 S33 118.7(3) . . ? C28 C27 S33 117.7(3) . . ? C18 C28 C27 120.8(4) . . ? C18 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? N7 C29 C30 119.7(2) . . ? N7 C29 C30 119.7(2) . 4_565 ? C30 C29 C30 120.7(5) . 4_565 ? C29 C30 H30 120.2 . . ? C29 C30 C31 119.5(5) . . ? H30 C30 C31 120.2 . . ? C30 C31 H31 120.1 . . ? C30 C31 C32 119.8(5) . . ? H31 C31 C32 120.1 . . ? C31 C32 C31 120.8(5) . 4_565 ? C31 C32 H32 119.6 . . ? C31 C32 H32 119.6 4_565 . ? C27 S33 O34 106.8(3) . . ? C27 S33 C35 91.6(3) . . ? O34 S33 C35 107.0(5) . . ? S33 C35 H35A 109.5 . . ? S33 C35 H35B 109.5 . . ? S33 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N36 C37 C38 179.7(5) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? F1 P F1 175.5(3) . 4_565 ? F1 P F2 92.00(15) . . ? F1 P F2 92.00(15) 4_565 . ? F1 P F3 88.00(15) . . ? F1 P F3 87.99(15) 4_565 . ? F1 P F4 90.93(11) . . ? F1 P F4 90.93(11) 4_565 . ? F1 P F5 89.05(12) . . ? F1 P F5 89.05(12) 4_565 . ? F2 P F3 179.81(18) . . ? F2 P F4 92.17(17) . . ? F2 P F5 88.55(18) . . ? F3 P F4 88.02(18) . . ? F3 P F5 91.26(18) . . ? F4 P F5 179.28(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 C6 C1 C2 C3 0.0 . . . . ? C6 C1 C2 C25 180.0 . . . . ? C19 C1 C2 C3 180.0 . . . . ? C19 C1 C2 C25 0.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? C25 C2 C3 C4 180.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C3 C4 C5 N7 180.0 . . . . ? C4 C5 C6 C1 0.0 . . . . ? C4 C5 C6 C10 180.0 . . . . ? N7 C5 C6 C1 180.0 . . . . ? N7 C5 C6 C10 0.0 . . . . ? C2 C1 C6 C5 0.0 . . . . ? C2 C1 C6 C10 180.0 . . . . ? C19 C1 C6 C5 180.0 . . . . ? C19 C1 C6 C10 0.0 . . . . ? C4 C5 N7 C8 180.0 . . . . ? C4 C5 N7 C29 0.0 . . . . ? C6 C5 N7 C8 0.0 . . . . ? C6 C5 N7 C29 180.0 . . . . ? C5 N7 C8 C9 0.0 . . . . ? C5 N7 C8 C11 180.0 . . . . ? C29 N7 C8 C9 180.0 . . . . ? C29 N7 C8 C11 0.0 . . . . ? N7 C8 C9 C10 0.0 . . . . ? N7 C8 C9 C14 180.0 . . . . ? C11 C8 C9 C10 180.0 . . . . ? C11 C8 C9 C14 0.0 . . . . ? C1 C6 C10 C9 180.0 . . . . ? C1 C6 C10 C17 0.0 . . . . ? C5 C6 C10 C9 0.0 . . . . ? C5 C6 C10 C17 180.0 . . . . ? C8 C9 C10 C6 0.0 . . . . ? C8 C9 C10 C17 180.0 . . . . ? C14 C9 C10 C6 180.0 . . . . ? C14 C9 C10 C17 0.0 . . . . ? N7 C8 C11 C12 180.0 . . . . ? C9 C8 C11 C12 0.0 . . . . ? C8 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C11 C12 C13 C20 180.0 . . . . ? C12 C13 C14 C9 0.0 . . . . ? C12 C13 C14 C15 180.0 . . . . ? C20 C13 C14 C9 180.0 . . . . ? C20 C13 C14 C15 0.0 . . . . ? C8 C9 C14 C13 0.0 . . . . ? C8 C9 C14 C15 180.0 . . . . ? C10 C9 C14 C13 180.0 . . . . ? C10 C9 C14 C15 0.0 . . . . ? C9 C14 C15 C16 0.0 . . . . ? C9 C14 C15 C22 180.0 . . . . ? C13 C14 C15 C16 180.0 . . . . ? C13 C14 C15 C22 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C14 C15 C16 C26 180.0 . . . . ? C22 C15 C16 C17 180.0 . . . . ? C22 C15 C16 C26 0.0 . . . . ? C6 C10 C17 C16 180.0 . . . . ? C6 C10 C17 C18 0.0 . . . . ? C9 C10 C17 C16 0.0 . . . . ? C9 C10 C17 C18 180.0 . . . . ? C15 C16 C17 C10 0.0 . . . . ? C15 C16 C17 C18 180.0 . . . . ? C26 C16 C17 C10 180.0 . . . . ? C26 C16 C17 C18 0.0 . . . . ? C10 C17 C18 C19 0.0 . . . . ? C10 C17 C18 C28 180.0 . . . . ? C16 C17 C18 C19 180.0 . . . . ? C16 C17 C18 C28 0.0 . . . . ? C2 C1 C19 C18 180.0 . . . . ? C2 C1 C19 C23 0.0 . . . . ? C6 C1 C19 C18 0.0 . . . . ? C6 C1 C19 C23 180.0 . . . . ? C17 C18 C19 C1 0.0 . . . . ? C17 C18 C19 C23 180.0 . . . . ? C28 C18 C19 C1 180.0 . . . . ? C28 C18 C19 C23 0.0 . . . . ? C12 C13 C20 C21 180.0 . . . . ? C14 C13 C20 C21 0.0 . . . . ? C13 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C15 0.0 . . . . ? C14 C15 C22 C21 0.0 . . . . ? C16 C15 C22 C21 180.0 . . . . ? C1 C19 C23 C24 0.0 . . . . ? C18 C19 C23 C24 180.0 . . . . ? C19 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C2 0.0 . . . . ? C1 C2 C25 C24 0.0 . . . . ? C3 C2 C25 C24 180.0 . . . . ? C15 C16 C26 C27 180.0 . . . . ? C17 C16 C26 C27 0.0 . . . . ? C16 C26 C27 C28 0.0 . . . . ? C16 C26 C27 S33 -164.40(10) . . . . ? C26 C27 C28 C18 0.0 . . . . ? S33 C27 C28 C18 164.56(10) . . . . ? C17 C18 C28 C27 0.0 . . . . ? C19 C18 C28 C27 180.0 . . . . ? C5 N7 C29 C30 -90.8(4) . . . . ? C5 N7 C29 C30 90.8(4) . . . 4_565 ? C8 N7 C29 C30 89.2(4) . . . . ? C8 N7 C29 C30 -89.2(4) . . . 4_565 ? N7 C29 C30 C31 -177.9(4) . . . . ? C30 C29 C30 C31 0.4(8) 4_565 . . . ? C29 C30 C31 C32 -0.1(7) . . . . ? C30 C31 C32 C31 -0.3(10) . . . 4_565 ? C26 C27 S33 O34 166.3(4) . . . . ? C26 C27 S33 C35 -85.4(3) . . . . ? C28 C27 S33 O34 1.3(4) . . . . ? C28 C27 S33 C35 109.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.54 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.609 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.066 # Contents of RES file _computing_special_details ; TITL acb24 in P2(1)/m CELL 0.6709 13.773 6.7999 15.291 90.000 96.715 90.000 ZERR 2.00 0.004 0.0018 0.004 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, -Z SFAC C H N F P S O DISP P 0.09297 0.08419 318.32 DISP S 0.11369 0.11037 417.30 UNIT 72 46 4 12 2 2 2 REM orange needle SIZE 0.25 0.03 0.02 TEMP -153 SHEL 5.8 0.84 L.S. 8 ACTA BOND $H CONF FMAP 2 PLAN 10 rem EXTI 0.010559 insignificant WGHT 0.147400 0.786100 FVAR 0.40280 C1 1 0.462633 0.250000 0.529066 10.50000 0.03451 0.03045 = 0.04016 0.00000 0.01160 0.00000 C2 1 0.387230 0.250000 0.584243 10.50000 0.04302 0.03604 = 0.04007 0.00000 0.01758 0.00000 C3 1 0.412992 0.250000 0.676960 10.50000 0.04111 0.04834 = 0.04332 0.00000 0.02265 0.00000 AFIX 43 H3 2 0.362474 0.250000 0.714273 10.50000 -1.20000 AFIX 0 C4 1 0.507337 0.250000 0.713825 10.50000 0.05249 0.05787 = 0.02786 0.00000 0.01971 0.00000 AFIX 43 H4 2 0.522363 0.250000 0.776064 10.50000 -1.20000 AFIX 0 C5 1 0.583982 0.250000 0.658662 10.50000 0.03988 0.04404 = 0.03371 0.00000 0.01107 0.00000 C6 1 0.562058 0.250000 0.566995 10.50000 0.04208 0.03591 = 0.02828 0.00000 0.01489 0.00000 N7 3 0.679792 0.250000 0.695729 10.50000 0.04388 0.06115 = 0.02346 0.00000 0.01101 0.00000 C8 1 0.755925 0.250000 0.645276 10.50000 0.03868 0.05331 = 0.03110 0.00000 0.01082 0.00000 C9 1 0.736198 0.250000 0.553127 10.50000 0.03973 0.04185 = 0.02822 0.00000 0.01309 0.00000 C10 1 0.638288 0.250000 0.512784 10.50000 0.03371 0.03256 = 0.03266 0.00000 0.01055 0.00000 C11 1 0.854157 0.250000 0.685645 10.50000 0.04939 0.08375 = 0.02601 0.00000 0.00738 0.00000 AFIX 43 H11 2 0.867733 0.250000 0.748004 10.50000 -1.20000 AFIX 0 C12 1 0.927997 0.250000 0.635170 10.50000 0.03639 0.09390 = 0.03716 0.00000 0.00763 0.00000 AFIX 43 H12 2 0.993362 0.250000 0.663053 10.50000 -1.20000 AFIX 0 C13 1 0.911587 0.250000 0.541611 10.50000 0.04368 0.06833 = 0.03798 0.00000 0.01492 0.00000 C14 1 0.814676 0.250000 0.499427 10.50000 0.03892 0.04274 = 0.03411 0.00000 0.01491 0.00000 C15 1 0.796037 0.250000 0.407605 10.50000 0.04244 0.04171 = 0.03313 0.00000 0.01443 0.00000 C16 1 0.695184 0.250000 0.365790 10.50000 0.04114 0.03897 = 0.03131 0.00000 0.01291 0.00000 C17 1 0.617509 0.250000 0.419566 10.50000 0.04312 0.03508 = 0.02788 0.00000 0.01270 0.00000 C18 1 0.518606 0.250000 0.380634 10.50000 0.03743 0.04091 = 0.03551 0.00000 0.00818 0.00000 C19 1 0.439269 0.250000 0.436798 10.50000 0.04161 0.03544 = 0.03489 0.00000 0.01026 0.00000 C20 1 0.988201 0.250000 0.491035 10.50000 0.03379 0.09927 = 0.04793 0.00000 0.01662 0.00000 AFIX 43 H20 2 1.053678 0.250000 0.518647 10.50000 -1.20000 AFIX 0 C21 1 0.969816 0.250000 0.400272 10.50000 0.04142 0.09935 = 0.03880 0.00000 0.02073 0.00000 AFIX 43 H21 2 1.023041 0.250000 0.365965 10.50000 -1.20000 AFIX 0 C22 1 0.875751 0.250000 0.358829 10.50000 0.04365 0.06133 = 0.03588 0.00000 0.01843 0.00000 AFIX 43 H22 2 0.864780 0.250000 0.296325 10.50000 -1.20000 AFIX 0 C23 1 0.341653 0.250000 0.402658 10.50000 0.04040 0.04472 = 0.04158 0.00000 0.00850 0.00000 AFIX 43 H23 2 0.324903 0.250000 0.340600 10.50000 -1.20000 AFIX 0 C24 1 0.267395 0.250000 0.457204 10.50000 0.03679 0.04769 = 0.04867 0.00000 0.00954 0.00000 AFIX 43 H24 2 0.201022 0.250000 0.431921 10.50000 -1.20000 AFIX 0 C25 1 0.289145 0.250000 0.546835 10.50000 0.03833 0.03988 = 0.05330 0.00000 0.02075 0.00000 AFIX 43 H25 2 0.238107 0.250000 0.583596 10.50000 -1.20000 AFIX 0 C26 1 0.672383 0.250000 0.275491 10.50000 0.04804 0.06689 = 0.03146 0.00000 0.01595 0.00000 AFIX 43 H26 2 0.723271 0.250000 0.238570 10.50000 -1.20000 AFIX 0 C27 1 0.576950 0.250000 0.238862 10.50000 0.04573 0.09755 = 0.02960 0.00000 0.00985 0.00000 C28 1 0.500936 0.250000 0.289731 10.50000 0.04213 0.09568 = 0.03284 0.00000 0.00580 0.00000 AFIX 43 H28 2 0.435477 0.250000 0.262075 10.50000 -1.20000 AFIX 0 C29 1 0.702107 0.250000 0.791505 10.50000 0.04271 0.08446 = 0.02752 0.00000 0.01091 0.00000 C30 1 0.713560 0.423321 0.835412 11.00000 0.09244 0.10916 = 0.03469 -0.01591 0.01551 -0.03268 AFIX 43 H30 2 0.704983 0.544194 0.804314 11.00000 -1.20000 AFIX 0 C31 1 0.737675 0.422832 0.925256 11.00000 0.11474 0.15390 = 0.03463 -0.02165 0.01575 -0.04957 AFIX 43 H31 2 0.745912 0.543501 0.956554 11.00000 -1.20000 AFIX 0 C32 1 0.749615 0.250000 0.968876 10.50000 0.06259 0.18996 = 0.02857 0.00000 0.01184 0.00000 AFIX 43 H32 2 0.766596 0.250002 1.030907 10.50000 -1.20000 AFIX 0 PART -1 S33 6 0.549165 0.186551 0.122373 10.50000 0.06154 0.11500 = 0.02471 -0.00712 0.00698 -0.01075 O34 7 0.444736 0.151206 0.106839 10.50000 0.08337 0.26035 = 0.03582 -0.02005 0.01058 -0.04231 C35 1 0.569351 0.437824 0.089222 10.50000 0.11380 0.10543 = 0.03424 0.02932 0.02888 0.02052 AFIX 33 H35A 2 0.558963 0.447254 0.024854 10.50000 -1.50000 H35B 2 0.636527 0.476873 0.110261 10.50000 -1.50000 H35C 2 0.523476 0.525177 0.114631 10.50000 -1.50000 AFIX 0 PART 0 N36 3 0.134681 0.250000 1.243817 10.50000 0.06919 0.09957 = 0.05088 0.00000 0.02383 0.00000 C37 1 0.083377 0.250000 1.180555 10.50000 0.05859 0.09290 = 0.04914 0.00000 0.03045 0.00000 C38 1 0.017268 0.250000 1.098361 10.50000 0.07751 0.14096 = 0.04844 0.00000 0.02062 0.00000 AFIX 33 H38A 2 -0.050596 0.250000 1.111761 10.50000 -1.20000 H38B 2 0.029061 0.132327 1.064137 10.50000 -1.20000 H38C 2 0.029061 0.367673 1.064137 10.50000 -1.20000 AFIX 0 P 5 0.161122 0.250000 0.831546 10.50000 0.05392 0.08979 = 0.02261 0.00000 0.01309 0.00000 F1 4 0.165061 0.478498 0.833790 11.00000 0.21236 0.09527 = 0.11973 0.02534 0.09153 0.01152 F2 4 0.048111 0.250000 0.818163 10.50000 0.04938 0.32157 = 0.04212 0.00000 0.00825 0.00000 F3 4 0.275952 0.250000 0.845492 10.50000 0.06279 0.25283 = 0.05434 0.00000 0.01115 0.00000 F4 4 0.167192 0.250000 0.729017 10.50000 0.06979 0.22949 = 0.02289 0.00000 0.01943 0.00000 F5 4 0.156515 0.250000 0.934150 10.50000 0.09514 0.13060 = 0.02517 0.00000 0.01833 0.00000 HKLF 4 REM acb24 in P2(1)/m REM R1 = 0.0755 for 2070 Fo > 4sig(Fo) and 0.0909 for all 2705 data REM 283 parameters refined using 0 restraints END ; #===END