# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Coppens, Philip' 'Ma, Bao-Qing' _publ_contact_author_name 'Dr Philip Coppens' _publ_contact_author_address ; Department of Chemistry State University of New York at Buffalo Buffalo New York 14260-3000 USA ; _publ_contact_author_email 'COPPENS@ACSU.BUFFALO.EDU' _publ_section_title ; A novel scoop-shaped conformation of C-methylcalix[4]resorcinarene in a bilayer structure ; data_p-1 _database_code_CSD 173809 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 O9' _chemical_formula_weight 562.59 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9289(4) _cell_length_b 12.4936(6) _cell_length_c 12.6547(7) _cell_angle_alpha 104.290(2) _cell_angle_beta 106.652(2) _cell_angle_gamma 108.593(2) _cell_volume 1322.91(11) _cell_formula_units_Z 2 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(1) _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 'SMART CCD 1000' _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 21607 _diffrn_reflns_av_R_equivalents 0.1171 _diffrn_reflns_av_sigmaI/netI 0.1436 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 31.09 _reflns_number_total 7549 _reflns_number_gt 3856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART CCD 1000' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP' _computing_publication_material 'XCIF' _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^)+(0.0522P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7549 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1312 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.903 _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 0.48276(19) 0.55200(15) 0.71308(13) 0.0165(4) Uani 1 1 d . . . O2 O 0.18514(19) 0.46426(15) 0.30274(13) 0.0149(3) Uani 1 1 d . . . O3 O 0.07468(19) 0.32609(15) 0.06688(14) 0.0172(4) Uani 1 1 d . . . O4 O 0.45019(18) 0.19819(15) -0.01564(13) 0.0152(3) Uani 1 1 d . . . O5 O 0.73091(19) 0.28883(15) 0.17088(14) 0.0163(4) Uani 1 1 d . . . O6 O 1.00920(19) 0.38184(15) 0.57826(13) 0.0160(4) Uani 1 1 d . . . O7 O 0.95622(18) 0.29697(15) 0.83798(14) 0.0164(4) Uani 1 1 d . . . O8 O 0.56137(18) 0.39554(14) 0.92562(13) 0.0135(3) Uani 1 1 d . . . O9 O 0.7738(2) 0.51801(17) 1.14438(14) 0.0191(4) Uani 1 1 d . . . C1 C 0.3250(2) 0.34877(19) 0.58187(18) 0.0103(4) Uani 1 1 d . . . C2 C 0.3821(2) 0.47214(19) 0.59986(18) 0.0117(4) Uani 1 1 d . . . C3 C 0.3368(2) 0.5123(2) 0.50814(19) 0.0128(4) Uani 1 1 d . . . C4 C 0.2363(2) 0.42765(19) 0.39547(18) 0.0120(4) Uani 1 1 d . . . C5 C 0.1775(2) 0.30271(19) 0.37133(18) 0.0110(4) Uani 1 1 d . . . C6 C 0.2235(2) 0.26687(19) 0.46649(18) 0.0103(4) Uani 1 1 d . . . C7 C 0.0700(2) 0.21369(19) 0.24535(18) 0.0110(4) Uani 1 1 d . . . C8 C -0.0312(3) 0.0876(2) 0.2370(2) 0.0149(5) Uani 1 1 d . . . C9 C 0.1653(2) 0.20665(19) 0.17034(17) 0.0112(4) Uani 1 1 d . . . C10 C 0.1651(2) 0.26223(19) 0.08729(18) 0.0125(4) Uani 1 1 d . . . C11 C 0.2572(3) 0.2585(2) 0.02360(18) 0.0135(4) Uani 1 1 d . . . C12 C 0.3527(2) 0.19929(19) 0.04316(18) 0.0124(4) Uani 1 1 d . . . C13 C 0.3591(2) 0.14294(19) 0.12596(18) 0.0114(4) Uani 1 1 d . . . C14 C 0.2639(2) 0.14897(19) 0.18800(18) 0.0105(4) Uani 1 1 d . . . C15 C 0.4684(3) 0.08154(19) 0.15194(18) 0.0119(4) Uani 1 1 d . . . C16 C 0.3843(3) -0.0466(2) 0.1474(2) 0.0138(5) Uani 1 1 d . . . C17 C 0.6097(2) 0.16368(19) 0.26778(18) 0.0109(4) Uani 1 1 d . . . C18 C 0.7310(3) 0.2604(2) 0.26968(18) 0.0124(4) Uani 1 1 d . . . C19 C 0.8629(3) 0.3340(2) 0.37215(19) 0.0122(4) Uani 1 1 d . . . C20 C 0.8776(2) 0.31224(19) 0.47589(18) 0.0122(4) Uani 1 1 d . . . C21 C 0.7592(2) 0.21853(19) 0.48048(18) 0.0112(4) Uani 1 1 d . . . C22 C 0.6281(3) 0.1460(2) 0.37507(18) 0.0116(4) Uani 1 1 d . . . C23 C 0.7869(3) 0.1948(2) 0.59517(18) 0.0120(4) Uani 1 1 d . . . C24 C 0.7357(3) 0.0600(2) 0.5753(2) 0.0189(5) Uani 1 1 d . . . C25 C 0.7255(2) 0.25494(19) 0.67914(18) 0.0103(4) Uani 1 1 d . . . C26 C 0.8152(2) 0.30260(19) 0.80107(18) 0.0125(4) Uani 1 1 d . . . C27 C 0.7639(3) 0.3530(2) 0.88371(19) 0.0125(4) Uani 1 1 d . . . C28 C 0.6191(2) 0.35410(19) 0.84516(18) 0.0114(4) Uani 1 1 d . . . C29 C 0.5246(2) 0.30933(19) 0.72434(18) 0.0101(4) Uani 1 1 d . . . C30 C 0.5811(2) 0.26042(19) 0.64373(18) 0.0105(4) Uani 1 1 d . . . C31 C 0.3664(2) 0.3121(2) 0.68813(18) 0.0109(4) Uani 1 1 d . . . C32 C 0.2413(3) 0.1929(2) 0.6748(2) 0.0157(5) Uani 1 1 d . . . H19A H 0.939(3) 0.398(2) 0.3695(18) 0.009(6) Uiso 1 1 d . . . H16C H 0.298(3) -0.099(2) 0.067(2) 0.019(6) Uiso 1 1 d . . . H11A H 0.254(3) 0.300(2) -0.0324(19) 0.010(6) Uiso 1 1 d . . . H22A H 0.546(2) 0.0776(19) 0.3740(18) 0.006(5) Uiso 1 1 d . . . H10 H 0.860(4) 0.574(3) 1.167(3) 0.058(11) Uiso 1 1 d . . . H8B H 0.027(3) 0.042(2) 0.264(2) 0.019(7) Uiso 1 1 d . . . H24C H 0.618(3) 0.011(2) 0.527(2) 0.031(8) Uiso 1 1 d . . . H15A H 0.505(2) 0.0680(18) 0.0888(18) 0.004(5) Uiso 1 1 d . . . H32C H 0.138(3) 0.197(2) 0.654(2) 0.026(7) Uiso 1 1 d . . . H14A H 0.272(3) 0.112(2) 0.2506(19) 0.014(6) Uiso 1 1 d . . . H8A H -0.106(3) 0.034(2) 0.154(2) 0.014(6) Uiso 1 1 d . . . H27A H 0.830(3) 0.384(2) 0.971(2) 0.017(6) Uiso 1 1 d . . . H24B H 0.783(3) 0.022(2) 0.526(2) 0.029(7) Uiso 1 1 d . . . H7 H 0.990(3) 0.312(2) 0.913(2) 0.035(8) Uiso 1 1 d . . . H24A H 0.770(3) 0.048(2) 0.654(2) 0.017(6) Uiso 1 1 d . . . H2 H 0.242(4) 0.540(3) 0.325(3) 0.050(10) Uiso 1 1 d . . . H6 H 1.075(3) 0.417(3) 0.561(2) 0.039(10) Uiso 1 1 d . . . H7A H 0.001(3) 0.248(2) 0.2108(19) 0.012(6) Uiso 1 1 d . . . H6A H 0.177(2) 0.180(2) 0.4500(18) 0.007(6) Uiso 1 1 d . . . H3A H 0.375(2) 0.601(2) 0.5235(19) 0.012(6) Uiso 1 1 d . . . H4 H 0.466(3) 0.257(3) -0.040(2) 0.038(9) Uiso 1 1 d . . . H30A H 0.513(3) 0.2260(19) 0.5568(19) 0.012(6) Uiso 1 1 d . . . H1 H 0.516(4) 0.623(3) 0.718(3) 0.057(11) Uiso 1 1 d . . . H31A H 0.373(2) 0.3743(19) 0.7527(18) 0.003(5) Uiso 1 1 d . . . H9 H 0.797(4) 0.463(4) 1.175(3) 0.083(13) Uiso 1 1 d . . . H16B H 0.457(3) -0.085(2) 0.167(2) 0.033(8) Uiso 1 1 d . . . H32B H 0.265(3) 0.179(2) 0.748(2) 0.028(7) Uiso 1 1 d . . . H32A H 0.228(3) 0.121(2) 0.612(2) 0.027(7) Uiso 1 1 d . . . H8 H 0.638(4) 0.444(3) 1.000(3) 0.068(11) Uiso 1 1 d . . . H16A H 0.326(3) -0.051(2) 0.203(2) 0.028(7) Uiso 1 1 d . . . H23A H 0.897(3) 0.2339(19) 0.6393(19) 0.008(6) Uiso 1 1 d . . . H8C H -0.092(3) 0.088(2) 0.285(2) 0.022(7) Uiso 1 1 d . . . H3 H 0.091(3) 0.376(3) 0.139(2) 0.042(9) Uiso 1 1 d . . . H5 H 0.643(3) 0.251(3) 0.113(2) 0.042(9) 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 0.0171(9) 0.0128(8) 0.0130(8) 0.0023(6) 0.0025(7) 0.0033(7) O2 0.0183(9) 0.0141(8) 0.0131(8) 0.0077(6) 0.0052(7) 0.0068(7) O3 0.0226(9) 0.0247(9) 0.0119(8) 0.0081(7) 0.0071(7) 0.0176(8) O4 0.0181(9) 0.0204(9) 0.0156(8) 0.0107(7) 0.0118(7) 0.0105(7) O5 0.0138(9) 0.0230(9) 0.0139(8) 0.0102(7) 0.0069(7) 0.0063(7) O6 0.0122(8) 0.0185(9) 0.0137(8) 0.0052(7) 0.0041(7) 0.0036(7) O7 0.0138(8) 0.0275(9) 0.0113(8) 0.0092(7) 0.0047(7) 0.0116(7) O8 0.0153(8) 0.0183(8) 0.0083(7) 0.0037(6) 0.0065(7) 0.0082(7) O9 0.0179(9) 0.0205(9) 0.0143(8) 0.0058(7) 0.0035(7) 0.0054(8) C1 0.0088(10) 0.0154(11) 0.0107(10) 0.0054(8) 0.0056(8) 0.0079(8) C2 0.0088(10) 0.0142(11) 0.0101(10) 0.0016(8) 0.0036(8) 0.0048(8) C3 0.0120(11) 0.0120(11) 0.0149(11) 0.0050(9) 0.0067(9) 0.0046(9) C4 0.0132(11) 0.0171(11) 0.0132(10) 0.0094(9) 0.0089(9) 0.0093(9) C5 0.0088(10) 0.0154(11) 0.0105(10) 0.0042(8) 0.0057(8) 0.0062(9) C6 0.0099(10) 0.0109(10) 0.0120(10) 0.0042(8) 0.0056(8) 0.0056(8) C7 0.0096(10) 0.0145(11) 0.0089(10) 0.0044(8) 0.0026(8) 0.0062(9) C8 0.0129(11) 0.0164(11) 0.0129(11) 0.0036(9) 0.0045(9) 0.0051(9) C9 0.0102(10) 0.0148(11) 0.0062(9) 0.0013(8) 0.0022(8) 0.0054(8) C10 0.0119(11) 0.0135(11) 0.0097(10) 0.0035(8) 0.0008(8) 0.0061(9) C11 0.0171(11) 0.0149(11) 0.0092(10) 0.0064(9) 0.0044(9) 0.0069(9) C12 0.0126(11) 0.0134(11) 0.0094(10) 0.0016(8) 0.0056(8) 0.0041(9) C13 0.0103(10) 0.0104(10) 0.0111(10) 0.0021(8) 0.0037(8) 0.0036(8) C14 0.0103(10) 0.0094(10) 0.0077(10) 0.0020(8) 0.0018(8) 0.0017(8) C15 0.0138(11) 0.0140(11) 0.0106(10) 0.0047(8) 0.0074(9) 0.0070(9) C16 0.0160(12) 0.0118(11) 0.0132(11) 0.0036(9) 0.0058(9) 0.0065(9) C17 0.0105(10) 0.0111(10) 0.0128(10) 0.0039(8) 0.0052(8) 0.0064(8) C18 0.0148(11) 0.0165(11) 0.0143(11) 0.0087(9) 0.0098(9) 0.0107(9) C19 0.0115(11) 0.0124(11) 0.0162(11) 0.0061(9) 0.0083(9) 0.0062(9) C20 0.0097(10) 0.0132(11) 0.0134(10) 0.0027(8) 0.0046(9) 0.0064(8) C21 0.0141(11) 0.0137(11) 0.0113(10) 0.0055(8) 0.0080(9) 0.0094(9) C22 0.0122(11) 0.0138(11) 0.0142(10) 0.0067(8) 0.0090(9) 0.0076(9) C23 0.0138(11) 0.0144(11) 0.0103(10) 0.0052(8) 0.0060(9) 0.0075(9) C24 0.0299(15) 0.0202(13) 0.0147(12) 0.0089(10) 0.0117(11) 0.0158(11) C25 0.0108(10) 0.0111(10) 0.0112(10) 0.0056(8) 0.0056(8) 0.0051(8) C26 0.0105(11) 0.0161(11) 0.0143(11) 0.0081(9) 0.0053(9) 0.0075(9) C27 0.0147(11) 0.0147(11) 0.0089(10) 0.0053(8) 0.0038(9) 0.0072(9) C28 0.0154(11) 0.0119(10) 0.0112(10) 0.0049(8) 0.0080(9) 0.0078(9) C29 0.0090(10) 0.0116(10) 0.0117(10) 0.0060(8) 0.0050(8) 0.0046(8) C30 0.0105(10) 0.0111(10) 0.0081(10) 0.0033(8) 0.0023(8) 0.0038(8) C31 0.0100(10) 0.0137(11) 0.0096(10) 0.0038(8) 0.0044(8) 0.0059(8) C32 0.0145(12) 0.0187(12) 0.0141(11) 0.0070(10) 0.0064(9) 0.0060(10) _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 C2 1.373(2) . ? O2 C4 1.384(2) . ? O3 C10 1.391(3) . ? O4 C12 1.381(2) . ? O5 C18 1.381(2) . ? O6 C20 1.375(2) . ? O7 C26 1.374(3) . ? O8 C28 1.378(2) . ? C1 C2 1.394(3) . ? C1 C6 1.399(3) . ? C1 C31 1.515(3) . ? C2 C3 1.391(3) . ? C3 C4 1.384(3) . ? C4 C5 1.397(3) . ? C5 C6 1.393(3) . ? C5 C7 1.520(3) . ? C7 C9 1.526(3) . ? C7 C8 1.533(3) . ? C9 C14 1.390(3) . ? C9 C10 1.395(3) . ? C10 C11 1.385(3) . ? C11 C12 1.383(3) . ? C12 C13 1.397(3) . ? C13 C14 1.399(3) . ? C13 C15 1.525(3) . ? C15 C17 1.527(3) . ? C15 C16 1.530(3) . ? C17 C18 1.398(3) . ? C17 C22 1.399(3) . ? C18 C19 1.383(3) . ? C19 C20 1.382(3) . ? C20 C21 1.397(3) . ? C21 C22 1.397(3) . ? C21 C23 1.518(3) . ? C23 C24 1.527(3) . ? C23 C25 1.528(3) . ? C25 C26 1.396(3) . ? C25 C30 1.403(3) . ? C26 C27 1.391(3) . ? C27 C28 1.384(3) . ? C28 C29 1.397(3) . ? C29 C30 1.403(3) . ? C29 C31 1.519(3) . ? C31 C32 1.538(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 116.98(19) . . ? C2 C1 C31 118.79(18) . . ? C6 C1 C31 124.1(2) . . ? O1 C2 C3 121.7(2) . . ? O1 C2 C1 116.70(19) . . ? C3 C2 C1 121.6(2) . . ? C4 C3 C2 119.2(2) . . ? C3 C4 O2 120.8(2) . . ? C3 C4 C5 121.9(2) . . ? O2 C4 C5 117.23(19) . . ? C6 C5 C4 116.87(19) . . ? C6 C5 C7 123.5(2) . . ? C4 C5 C7 119.64(19) . . ? C5 C6 C1 123.4(2) . . ? C5 C7 C9 108.97(17) . . ? C5 C7 C8 114.33(17) . . ? C9 C7 C8 112.10(18) . . ? C14 C9 C10 117.14(19) . . ? C14 C9 C7 120.10(19) . . ? C10 C9 C7 122.66(19) . . ? C11 C10 O3 117.15(19) . . ? C11 C10 C9 121.6(2) . . ? O3 C10 C9 121.26(19) . . ? C12 C11 C10 119.4(2) . . ? O4 C12 C11 120.70(19) . . ? O4 C12 C13 117.6(2) . . ? C11 C12 C13 121.7(2) . . ? C12 C13 C14 116.8(2) . . ? C12 C13 C15 122.25(19) . . ? C14 C13 C15 120.88(19) . . ? C9 C14 C13 123.4(2) . . ? C13 C15 C17 110.40(17) . . ? C13 C15 C16 111.87(18) . . ? C17 C15 C16 113.78(18) . . ? C18 C17 C22 116.54(19) . . ? C18 C17 C15 120.15(18) . . ? C22 C17 C15 123.29(19) . . ? O5 C18 C19 114.93(19) . . ? O5 C18 C17 123.5(2) . . ? C19 C18 C17 121.61(19) . . ? C20 C19 C18 120.0(2) . . ? O6 C20 C19 121.3(2) . . ? O6 C20 C21 117.56(19) . . ? C19 C20 C21 121.1(2) . . ? C22 C21 C20 117.08(19) . . ? C22 C21 C23 124.3(2) . . ? C20 C21 C23 118.34(19) . . ? C21 C22 C17 123.6(2) . . ? C21 C23 C24 113.12(18) . . ? C21 C23 C25 115.72(18) . . ? C24 C23 C25 110.81(18) . . ? C26 C25 C30 116.89(19) . . ? C26 C25 C23 118.04(19) . . ? C30 C25 C23 124.97(19) . . ? O7 C26 C27 120.42(19) . . ? O7 C26 C25 117.96(19) . . ? C27 C26 C25 121.6(2) . . ? C28 C27 C26 119.7(2) . . ? O8 C28 C27 120.65(19) . . ? O8 C28 C29 117.76(19) . . ? C27 C28 C29 121.54(19) . . ? C28 C29 C30 117.1(2) . . ? C28 C29 C31 118.85(19) . . ? C30 C29 C31 124.05(18) . . ? C29 C30 C25 123.20(19) . . ? C1 C31 C29 113.46(17) . . ? C1 C31 C32 113.58(18) . . ? C29 C31 C32 111.03(18) . . ? 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 O3 H3 O2 0.90(3) 1.87(3) 2.732(2) 159(3) . O4 H4 O8 0.86(3) 1.90(3) 2.737(2) 163(3) 1_554 O5 H5 O4 0.85(3) 1.91(3) 2.742(2) 168(3) . O7 H7 O3 0.86(3) 1.82(3) 2.676(2) 170(3) 1_656 O8 H8 O9 0.92(3) 1.73(3) 2.638(2) 172(3) . O9 H9 O5 0.93(4) 2.04(4) 2.876(2) 149(3) 1_556 O9 H10 O7 0.82(3) 2.04(3) 2.834(2) 160(3) 2_767 _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 31.09 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 0.509 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.102