# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Prof Sergey Gromov' _publ_contact_author_address ; Photochemistry Center Russian Academy of Sciences 7A Novatorov str Moscow 119421 RUSSIAN FEDERATION ; _publ_contact_author_email GROMOV@PHOTONICS.RU _publ_section_title ; Novel supramolecular charge-transfer systems based on bis(18-crown-6)stilbene and viologen analogues bearing two ammonioalkyl groups ; loop_ _publ_author_name 'Sergey Gromov' 'Michael V. Alfimov' 'Asya A. Botsmanova' 'Andrei V. Churakov' 'Ulf G. Edlund' ; J.Howard ; 'Dan Johnels' L.G.Kuz'mina 'Natalia A. Lobova' 'Yuri A. Strelenko' 'Evgeny N. Ushakov' ; A.I.Vedernikov ; data_a _database_code_depnum_ccdc_archive 'CCDC 232849' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 O4' _chemical_formula_weight 300.34 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9484(5) _cell_length_b 6.7152(3) _cell_length_c 12.4323(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.500(3) _cell_angle_gamma 90.00 _cell_volume 746.35(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 320 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9671 _exptl_absorpt_correction_T_max 0.9907 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2775 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1064 _reflns_number_gt 872 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^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 refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.007(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1064 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.15564(11) 0.03871(16) 0.06730(8) 0.0222(3) Uani 1 1 d . . . O2 O 0.03142(10) 0.08495(16) 0.25000(8) 0.0235(4) Uani 1 1 d . . . C1 C 0.51799(17) -0.0234(2) 0.44987(13) 0.0197(4) Uani 1 1 d . . . C2 C 0.42267(16) -0.0118(2) 0.35103(12) 0.0180(4) Uani 1 1 d . . . C3 C 0.48470(17) -0.0423(2) 0.25215(13) 0.0192(4) Uani 1 1 d . . . C4 C 0.39955(17) -0.0267(2) 0.15578(13) 0.0198(4) Uani 1 1 d . . . C5 C 0.24907(17) 0.0198(2) 0.15699(12) 0.0185(4) Uani 1 1 d . . . C6 C 0.18225(16) 0.0469(2) 0.25691(13) 0.0184(4) Uani 1 1 d . . . C7 C 0.26804(17) 0.0319(2) 0.35168(13) 0.0191(4) Uani 1 1 d . . . C8 C 0.2141(2) -0.0228(3) -0.03325(13) 0.0244(4) Uani 1 1 d . . . C9 C -0.04740(19) 0.0730(3) 0.34763(14) 0.0247(4) Uani 1 1 d . . . H4A H 0.4453(17) -0.050(2) 0.0894(13) 0.018(4) Uiso 1 1 d . . . H3A H 0.591(2) -0.076(2) 0.2513(13) 0.027(4) Uiso 1 1 d . . . H7A H 0.2216(17) 0.051(2) 0.4183(14) 0.024(4) Uiso 1 1 d . . . H8A H 0.128(2) -0.023(2) -0.0834(15) 0.029(5) Uiso 1 1 d . . . H8B H 0.2586(16) -0.164(3) -0.0275(12) 0.026(4) Uiso 1 1 d . . . H8C H 0.2928(19) 0.075(3) -0.0568(14) 0.033(5) Uiso 1 1 d . . . H9A H -0.1529(19) 0.092(2) 0.3247(12) 0.025(4) Uiso 1 1 d . . . H9B H -0.0152(16) 0.173(3) 0.4004(13) 0.028(4) Uiso 1 1 d . . . H9C H -0.0363(18) -0.060(3) 0.3830(15) 0.037(5) Uiso 1 1 d . . . H1A H 0.6176(19) -0.069(2) 0.4362(12) 0.021(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0185(6) 0.0328(7) 0.0150(6) -0.0013(5) -0.0017(5) 0.0033(4) O2 0.0158(6) 0.0362(7) 0.0186(7) 0.0007(5) 0.0021(4) 0.0039(4) C1 0.0162(9) 0.0202(9) 0.0227(10) 0.0012(7) 0.0009(7) 0.0002(6) C2 0.0181(8) 0.0164(8) 0.0194(10) 0.0007(6) -0.0019(7) -0.0017(6) C3 0.0163(9) 0.0218(9) 0.0193(9) -0.0010(7) -0.0018(7) 0.0007(6) C4 0.0199(9) 0.0220(9) 0.0178(10) -0.0013(7) 0.0046(7) -0.0004(6) C5 0.0190(8) 0.0191(9) 0.0168(10) 0.0011(7) -0.0040(7) -0.0024(6) C6 0.0142(8) 0.0188(8) 0.0223(10) -0.0011(7) 0.0001(7) 0.0009(6) C7 0.0210(9) 0.0188(9) 0.0176(10) -0.0014(7) 0.0025(8) -0.0010(6) C8 0.0222(9) 0.0348(11) 0.0161(10) -0.0037(7) 0.0000(8) 0.0034(8) C9 0.0190(9) 0.0360(11) 0.0192(10) -0.0008(9) 0.0034(7) 0.0021(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C5 1.3701(18) . ? O1 C8 1.4365(19) . ? O2 C6 1.3726(17) . ? O2 C9 1.4324(19) . ? C1 C1 1.338(3) 3_656 ? C1 C2 1.467(2) . ? C2 C3 1.386(2) . ? C2 C7 1.415(2) . ? C3 C4 1.396(2) . ? C4 C5 1.383(2) . ? C5 C6 1.414(2) . ? C6 C7 1.382(2) . ? 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 C5 O1 C8 116.70(12) . . ? C6 O2 C9 117.11(12) . . ? C1 C1 C2 127.80(19) 3_656 . ? C3 C2 C7 117.73(14) . . ? C3 C2 C1 119.63(14) . . ? C7 C2 C1 122.64(15) . . ? C2 C3 C4 121.72(15) . . ? C5 C4 C3 120.19(16) . . ? O1 C5 C4 124.88(14) . . ? O1 C5 C6 115.90(13) . . ? C4 C5 C6 119.21(14) . . ? O2 C6 C7 125.12(14) . . ? O2 C6 C5 114.92(13) . . ? C7 C6 C5 119.96(14) . . ? C6 C7 C2 121.16(15) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.168 _refine_diff_density_min -0.149 _refine_diff_density_rms 0.036 data_f _database_code_depnum_ccdc_archive 'CCDC 238954' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H48 O12' _chemical_formula_weight 648.72 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.7776(15) _cell_length_b 9.0073(3) _cell_length_c 8.6096(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.988(2) _cell_angle_gamma 90.00 _cell_volume 3299.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9434 _exptl_absorpt_correction_T_max 0.9980 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9016 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3184 _reflns_number_gt 2135 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.4130P] 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 refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3184 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.17466(3) 0.27084(12) 1.06377(13) 0.0215(3) Uani 1 1 d . . . O2 O 0.15260(3) 0.09040(12) 0.84488(13) 0.0217(3) Uani 1 1 d . . . O3 O 0.08469(3) 0.05560(12) 0.80211(14) 0.0247(3) Uani 1 1 d . . . O4 O 0.04712(3) 0.20369(13) 1.01577(14) 0.0241(3) Uani 1 1 d . . . O5 O 0.06622(3) 0.50069(13) 1.10629(15) 0.0277(3) Uani 1 1 d . . . O6 O 0.13387(3) 0.46365(15) 1.21263(15) 0.0299(4) Uani 1 1 d . . . C1 C 0.23768(5) 0.21300(19) 0.5209(2) 0.0204(4) Uani 1 1 d . . . C2 C 0.22235(5) 0.23231(17) 0.6652(2) 0.0196(4) Uani 1 1 d . . . C3 C 0.23406(5) 0.32701(18) 0.7859(2) 0.0196(4) Uani 1 1 d . . . C4 C 0.21888(5) 0.34127(18) 0.9209(2) 0.0196(4) Uani 1 1 d . . . C5 C 0.19170(5) 0.26233(17) 0.9377(2) 0.0174(4) Uani 1 1 d . . . C6 C 0.17928(5) 0.16533(17) 0.8171(2) 0.0179(4) Uani 1 1 d . . . C7 C 0.19477(5) 0.15117(18) 0.6835(2) 0.0201(4) Uani 1 1 d . . . C8 C 0.18513(5) 0.37663(19) 1.1842(2) 0.0202(4) Uani 1 1 d . . . C9 C 0.15979(5) 0.3889(2) 1.2921(2) 0.0250(5) Uani 1 1 d . . . C10 C 0.11080(6) 0.5037(2) 1.3139(2) 0.0307(5) Uani 1 1 d . . . C11 C 0.08511(6) 0.5881(2) 1.2209(3) 0.0324(5) Uani 1 1 d . . . C12 C 0.04262(5) 0.4192(2) 1.1719(2) 0.0254(5) Uani 1 1 d . . . C13 C 0.02630(5) 0.3193(2) 1.0492(2) 0.0242(5) Uani 1 1 d . . . C14 C 0.03494(5) 0.1130(2) 0.8886(2) 0.0243(4) Uani 1 1 d . . . C15 C 0.05809(5) -0.00779(19) 0.8633(2) 0.0254(5) Uani 1 1 d . . . C16 C 0.10694(5) -0.05445(18) 0.7667(2) 0.0215(4) Uani 1 1 d . . . C17 C 0.13530(5) 0.01912(19) 0.7126(2) 0.0203(4) Uani 1 1 d . . . H1 H 0.2277(5) 0.136(2) 0.449(2) 0.026(5) Uiso 1 1 d . . . H3 H 0.2520(5) 0.3813(19) 0.777(2) 0.017(5) Uiso 1 1 d . . . H4 H 0.2285(5) 0.4090(19) 1.003(2) 0.019(5) Uiso 1 1 d . . . H7 H 0.1861(5) 0.0849(18) 0.602(2) 0.020(5) Uiso 1 1 d . . . H8B H 0.2055(5) 0.3420(19) 1.242(2) 0.022(5) Uiso 1 1 d . . . H8A H 0.1888(4) 0.4738(18) 1.140(2) 0.017(5) Uiso 1 1 d . . . H9B H 0.1682(5) 0.4457(19) 1.384(2) 0.025(5) Uiso 1 1 d . . . H9A H 0.1542(5) 0.2898(19) 1.331(2) 0.021(5) Uiso 1 1 d . . . H10B H 0.1026(5) 0.412(2) 1.363(2) 0.030(5) Uiso 1 1 d . . . H10A H 0.1213(5) 0.566(2) 1.398(2) 0.037(6) Uiso 1 1 d . . . H11B H 0.0949(5) 0.664(2) 1.159(2) 0.040(6) Uiso 1 1 d . . . H11A H 0.0703(5) 0.6312(18) 1.291(2) 0.018(5) Uiso 1 1 d . . . H12B H 0.0514(5) 0.362(2) 1.260(2) 0.026(5) Uiso 1 1 d . . . H12A H 0.0261(5) 0.488(2) 1.209(2) 0.029(5) Uiso 1 1 d . . . H13B H 0.0206(5) 0.379(2) 0.957(2) 0.034(6) Uiso 1 1 d . . . H13A H 0.0065(5) 0.2740(19) 1.084(2) 0.027(5) Uiso 1 1 d . . . H14B H 0.0146(5) 0.0706(18) 0.908(2) 0.022(5) Uiso 1 1 d . . . H14A H 0.0308(5) 0.1767(18) 0.791(2) 0.021(5) Uiso 1 1 d . . . H15B H 0.0475(5) -0.0831(19) 0.791(2) 0.028(5) Uiso 1 1 d . . . H15A H 0.0645(5) -0.063(2) 0.966(3) 0.036(6) Uiso 1 1 d . . . H16B H 0.0966(5) -0.1195(19) 0.688(2) 0.023(5) Uiso 1 1 d . . . H16A H 0.1130(5) -0.121(2) 0.860(2) 0.028(5) Uiso 1 1 d . . . H17B H 0.1285(5) 0.0940(18) 0.632(2) 0.023(5) Uiso 1 1 d . . . H17A H 0.1481(4) -0.0570(18) 0.670(2) 0.018(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0242(8) 0.0264(6) 0.0148(6) -0.0059(5) 0.0064(6) -0.0057(6) O2 0.0240(8) 0.0277(6) 0.0145(6) -0.0045(5) 0.0065(6) -0.0078(6) O3 0.0233(8) 0.0214(6) 0.0311(7) -0.0024(5) 0.0112(6) -0.0023(6) O4 0.0239(8) 0.0279(6) 0.0202(7) -0.0034(5) 0.0013(6) 0.0051(6) O5 0.0290(9) 0.0288(6) 0.0262(7) -0.0015(5) 0.0076(7) -0.0019(6) O6 0.0238(9) 0.0461(8) 0.0203(7) -0.0058(6) 0.0051(6) 0.0057(7) C1 0.0217(11) 0.0230(8) 0.0167(10) 0.0029(7) 0.0022(9) 0.0048(8) C2 0.0206(11) 0.0195(7) 0.0192(10) 0.0042(7) 0.0044(9) 0.0066(8) C3 0.0158(11) 0.0233(8) 0.0201(10) 0.0059(7) 0.0032(9) -0.0004(8) C4 0.0212(12) 0.0205(8) 0.0171(9) 0.0014(7) 0.0013(9) 0.0001(8) C5 0.0178(11) 0.0201(7) 0.0150(9) 0.0032(6) 0.0045(8) 0.0035(8) C6 0.0175(11) 0.0186(7) 0.0180(9) 0.0011(7) 0.0032(8) -0.0013(7) C7 0.0237(12) 0.0214(8) 0.0157(9) -0.0001(7) 0.0045(9) 0.0014(8) C8 0.0232(12) 0.0232(8) 0.0138(9) -0.0028(7) 0.0005(9) -0.0028(8) C9 0.0298(13) 0.0292(9) 0.0161(10) -0.0052(8) 0.0034(9) -0.0056(9) C10 0.0276(13) 0.0420(11) 0.0237(10) -0.0131(9) 0.0088(10) -0.0015(10) C11 0.0343(15) 0.0278(9) 0.0373(12) -0.0100(9) 0.0140(11) -0.0025(10) C12 0.0253(13) 0.0283(9) 0.0239(10) -0.0005(8) 0.0082(10) 0.0048(9) C13 0.0206(12) 0.0280(9) 0.0246(10) 0.0016(8) 0.0049(9) 0.0063(9) C14 0.0209(12) 0.0306(9) 0.0215(10) -0.0024(8) 0.0024(9) -0.0068(9) C15 0.0268(13) 0.0249(8) 0.0260(10) -0.0045(8) 0.0099(10) -0.0080(9) C16 0.0234(12) 0.0205(8) 0.0209(10) -0.0056(8) 0.0044(9) -0.0008(8) C17 0.0242(12) 0.0215(8) 0.0154(9) -0.0045(7) 0.0036(9) -0.0021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C5 1.372(2) . ? O1 C8 1.445(2) . ? O2 C6 1.369(2) . ? O2 C17 1.443(2) . ? O3 C15 1.422(2) . ? O3 C16 1.429(2) . ? O4 C13 1.419(2) . ? O4 C14 1.421(2) . ? O5 C12 1.413(2) . ? O5 C11 1.442(3) . ? O6 C9 1.412(3) . ? O6 C10 1.430(2) . ? C1 C1 1.328(4) 7_556 ? C1 C2 1.475(2) . ? C2 C3 1.396(2) . ? C2 C7 1.410(3) . ? C3 C4 1.395(2) . ? C4 C5 1.383(3) . ? C5 C6 1.417(2) . ? C6 C7 1.392(2) . ? C8 C9 1.504(3) . ? C10 C11 1.497(3) . ? C12 C13 1.504(3) . ? C14 C15 1.503(3) . ? C16 C17 1.499(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 C5 O1 C8 117.03(14) . . ? C6 O2 C17 116.73(13) . . ? C15 O3 C16 112.14(13) . . ? C13 O4 C14 112.99(15) . . ? C12 O5 C11 112.48(15) . . ? C9 O6 C10 112.47(15) . . ? C1 C1 C2 127.2(2) 7_556 . ? C3 C2 C7 118.22(16) . . ? C3 C2 C1 122.85(17) . . ? C7 C2 C1 118.93(16) . . ? C4 C3 C2 120.93(18) . . ? C5 C4 C3 120.61(17) . . ? O1 C5 C4 125.17(16) . . ? O1 C5 C6 115.14(16) . . ? C4 C5 C6 119.68(16) . . ? O2 C6 C7 125.24(16) . . ? O2 C6 C5 115.58(14) . . ? C7 C6 C5 119.18(17) . . ? C6 C7 C2 121.38(17) . . ? O1 C8 C9 107.60(16) . . ? O6 C9 C8 108.41(15) . . ? O6 C10 C11 108.51(17) . . ? O5 C11 C10 114.60(16) . . ? O5 C12 C13 109.17(15) . . ? O4 C13 C12 109.07(17) . . ? O4 C14 C15 109.50(17) . . ? O3 C15 C14 109.12(15) . . ? O3 C16 C17 109.78(14) . . ? O2 C17 C16 108.44(14) . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 0.210 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.044