# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Linda Shimizu' 'Mahender B. Dewal' 'Jacob Hiller' 'Mark D. Smith' 'David Sobransingh' _publ_contact_author_name 'Linda Shimizu' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of South Carolina Columbia SC 29208 UNITED STATES OF AMERICA ; _publ_contact_author_email SHIMIZUL@MAIL.CHEM.SC.EDU _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Inclusion of electrochemically active guests by novel oxacalixarene hosts ; data_ds1 _database_code_depnum_ccdc_archive 'CCDC 659154' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H18 N4 O14, unknown solvate' _chemical_formula_sum 'C32 H18 N4 O14' _chemical_formula_weight 682.50 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 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' 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 8.8759(8) _cell_length_b 12.7053(12) _cell_length_c 16.6618(15) _cell_angle_alpha 90.00 _cell_angle_beta 103.925(2) _cell_angle_gamma 90.00 _cell_volume 1823.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 3703 _cell_measurement_theta_min 2.364 _cell_measurement_theta_max 23.402 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; No scattering observed above 2-theta ca. 45 degrees. ; _diffrn_ambient_temperature 150(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 15369 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 22.54 _reflns_number_total 2533 _reflns_number_gt 1861 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.625 (Bruker, 1998)' _computing_cell_refinement 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0701P)^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 2533 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1269 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.4182(3) 0.05717(19) 0.13310(17) 0.0334(7) Uani 1 1 d . . . C2 C 0.3570(3) 0.0716(2) 0.20119(17) 0.0365(7) Uani 1 1 d . . . H2 H 0.2512 0.0897 0.1957 0.044 Uiso 1 1 calc R . . C3 C 0.4577(3) 0.0582(2) 0.27735(17) 0.0386(7) Uani 1 1 d . . . C4 C 0.6120(3) 0.0318(2) 0.28747(18) 0.0389(7) Uani 1 1 d . . . H4 H 0.6781 0.0234 0.3411 0.047 Uiso 1 1 calc R . . C5 C 0.6677(3) 0.0181(2) 0.21767(17) 0.0358(7) Uani 1 1 d . . . C6 C 0.5704(3) 0.0311(2) 0.13919(17) 0.0350(7) Uani 1 1 d . . . H6 H 0.6086 0.0222 0.0910 0.042 Uiso 1 1 calc R . . C7 C 0.2533(3) 0.1546(2) 0.02447(15) 0.0295(6) Uani 1 1 d . . . C8 C 0.1245(3) 0.1555(2) -0.04380(15) 0.0284(6) Uani 1 1 d . . . C9 C 0.0630(4) 0.2500 -0.0762(2) 0.0291(9) Uani 1 2 d S . . H9 H -0.0243 0.2500 -0.1222 0.035 Uiso 1 2 calc SR . . C10 C 0.3145(4) 0.2500 0.0569(2) 0.0300(9) Uani 1 2 d S . . H10 H 0.4015 0.2500 0.1031 0.036 Uiso 1 2 calc SR . . C11 C 0.3774(3) 0.1550(3) 0.38243(17) 0.0438(8) Uani 1 1 d . . . C12 C 0.3140(4) 0.1555(3) 0.45133(18) 0.0565(10) Uani 1 1 d . . . C13 C 0.2828(5) 0.2500 0.4845(3) 0.0660(16) Uani 1 2 d S . . H13 H 0.2388 0.2500 0.5311 0.079 Uiso 1 2 calc SR . . C14 C 0.4111(4) 0.2500 0.3497(2) 0.0442(11) Uani 1 2 d S . . H14 H 0.4579 0.2500 0.3041 0.053 Uiso 1 2 calc SR . . C15 C 0.9353(3) 0.0218(2) 0.29092(18) 0.0449(8) Uani 1 1 d . . . H15A H 1.0371 -0.0067 0.2870 0.054 Uiso 1 1 calc R . . H15B H 0.9124 -0.0055 0.3424 0.054 Uiso 1 1 calc R . . C16 C 0.9428(3) 0.1397(2) 0.29427(17) 0.0377(7) Uani 1 1 d . . . C17 C 0.9278(3) 0.1957(2) 0.36392(17) 0.0464(8) Uani 1 1 d . . . H17 H 0.9175 0.1587 0.4119 0.056 Uiso 1 1 calc R . . C18 C 0.9576(3) 0.1957(2) 0.22483(17) 0.0375(7) Uani 1 1 d . . . H18 H 0.9678 0.1587 0.1769 0.045 Uiso 1 1 calc R . . O1 O 0.3181(2) 0.06148(13) 0.05358(11) 0.0386(5) Uani 1 1 d . . . O2 O 0.3999(2) 0.06095(17) 0.34923(12) 0.0487(6) Uani 1 1 d . . . O3 O 0.8163(2) -0.01313(15) 0.22040(11) 0.0411(5) Uani 1 1 d . . . N1 N 0.0457(3) 0.06025(18) -0.08149(13) 0.0333(6) Uani 1 1 d . . . O4 O -0.0718(2) 0.07158(15) -0.13693(12) 0.0436(5) Uani 1 1 d . . . O5 O 0.0998(2) -0.02573(15) -0.05622(11) 0.0394(5) Uani 1 1 d . . . N2 N 0.2685(4) 0.0595(4) 0.4879(2) 0.0742(10) Uani 1 1 d . . . O6 O 0.3297(5) -0.0257(3) 0.4769(2) 0.1242(14) Uani 1 1 d . . . O7 O 0.1818(3) 0.0663(3) 0.53237(18) 0.1116(13) Uani 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 C1 0.0382(17) 0.0197(14) 0.0384(17) 0.0019(12) 0.0013(14) -0.0016(12) C2 0.0319(16) 0.0323(16) 0.0434(17) 0.0051(13) 0.0052(14) -0.0027(13) C3 0.0390(18) 0.0404(18) 0.0381(18) 0.0109(13) 0.0124(14) -0.0059(14) C4 0.0341(18) 0.0432(18) 0.0370(17) 0.0141(13) 0.0041(14) -0.0019(13) C5 0.0310(17) 0.0320(16) 0.0432(18) 0.0116(13) 0.0068(14) 0.0003(13) C6 0.0398(18) 0.0259(16) 0.0385(17) 0.0014(12) 0.0077(14) 0.0011(13) C7 0.0303(16) 0.0257(15) 0.0333(15) 0.0003(12) 0.0097(13) 0.0021(12) C8 0.0291(15) 0.0281(15) 0.0280(15) -0.0031(12) 0.0070(12) -0.0018(12) C9 0.024(2) 0.037(2) 0.026(2) 0.000 0.0051(16) 0.000 C10 0.027(2) 0.030(2) 0.031(2) 0.000 0.0016(17) 0.000 C11 0.0254(16) 0.070(2) 0.0345(17) 0.0075(16) 0.0048(13) 0.0012(15) C12 0.0359(19) 0.102(3) 0.0327(18) 0.0099(19) 0.0097(15) -0.0081(19) C13 0.032(3) 0.135(6) 0.030(3) 0.000 0.008(2) 0.000 C14 0.031(2) 0.068(3) 0.035(2) 0.000 0.0131(19) 0.000 C15 0.0351(18) 0.053(2) 0.0444(18) 0.0092(15) 0.0055(15) 0.0050(15) C16 0.0241(15) 0.0508(19) 0.0358(17) 0.0067(15) 0.0025(12) 0.0026(13) C17 0.0382(17) 0.0638(19) 0.0358(17) 0.0088(14) 0.0058(13) -0.0026(14) C18 0.0312(16) 0.0468(16) 0.0355(16) 0.0002(13) 0.0102(12) 0.0024(13) O1 0.0449(12) 0.0235(10) 0.0405(12) -0.0014(8) -0.0032(9) 0.0048(9) O2 0.0445(13) 0.0626(15) 0.0416(12) 0.0155(11) 0.0154(10) -0.0049(11) O3 0.0310(12) 0.0452(12) 0.0460(12) 0.0058(9) 0.0070(9) 0.0054(9) N1 0.0338(14) 0.0335(15) 0.0335(14) -0.0025(11) 0.0097(12) -0.0025(11) O4 0.0339(12) 0.0422(12) 0.0485(13) -0.0067(10) -0.0025(10) -0.0080(9) O5 0.0465(12) 0.0274(11) 0.0445(12) -0.0020(9) 0.0113(9) -0.0027(9) N2 0.050(2) 0.125(3) 0.0510(19) 0.032(2) 0.0188(16) -0.002(2) O6 0.189(4) 0.115(3) 0.092(2) 0.017(2) 0.080(3) -0.036(3) O7 0.0716(18) 0.187(3) 0.090(2) 0.087(2) 0.0478(17) 0.032(2) _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 C6 1.371(4) . ? C1 C2 1.383(4) . ? C1 O1 1.407(3) . ? C2 C3 1.375(4) . ? C2 H2 0.9500 . ? C3 C4 1.380(4) . ? C3 O2 1.412(3) . ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? C5 O3 1.367(3) . ? C5 C6 1.393(4) . ? C6 H6 0.9500 . ? C7 O1 1.353(3) . ? C7 C10 1.384(3) . ? C7 C8 1.406(4) . ? C8 C9 1.375(3) . ? C8 N1 1.461(3) . ? C9 C8 1.375(3) 4_565 ? C9 H9 0.9500 . ? C10 C7 1.384(3) 4_565 ? C10 H10 0.9500 . ? C11 O2 1.352(4) . ? C11 C14 1.386(4) . ? C11 C12 1.395(4) . ? C12 C13 1.377(4) . ? C12 N2 1.463(5) . ? C13 C12 1.377(4) 4_565 ? C13 H13 0.9500 . ? C14 C11 1.386(4) 4_565 ? C14 H14 0.9500 . ? C15 O3 1.447(3) . ? C15 C16 1.501(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.391(4) . ? C16 C17 1.395(4) . ? C17 C17 1.379(6) 4_565 ? C17 H17 0.9500 . ? C18 C18 1.381(6) 4_565 ? C18 H18 0.9500 . ? N1 O4 1.224(3) . ? N1 O5 1.226(3) . ? N2 O7 1.193(4) . ? N2 O6 1.244(5) . ? 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 C6 C1 C2 123.1(3) . . ? C6 C1 O1 117.8(2) . . ? C2 C1 O1 118.9(2) . . ? C3 C2 C1 116.4(3) . . ? C3 C2 H2 121.8 . . ? C1 C2 H2 121.8 . . ? C2 C3 C4 123.2(3) . . ? C2 C3 O2 119.5(3) . . ? C4 C3 O2 117.0(2) . . ? C5 C4 C3 118.3(3) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? O3 C5 C4 123.2(2) . . ? O3 C5 C6 116.2(2) . . ? C4 C5 C6 120.6(3) . . ? C1 C6 C5 118.4(3) . . ? C1 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? O1 C7 C10 122.2(2) . . ? O1 C7 C8 119.3(2) . . ? C10 C7 C8 118.4(2) . . ? C9 C8 C7 119.6(2) . . ? C9 C8 N1 116.8(2) . . ? C7 C8 N1 123.6(2) . . ? C8 C9 C8 121.8(3) 4_565 . ? C8 C9 H9 119.1 4_565 . ? C8 C9 H9 119.1 . . ? C7 C10 C7 122.3(3) . 4_565 ? C7 C10 H10 118.8 . . ? C7 C10 H10 118.8 4_565 . ? O2 C11 C14 122.8(3) . . ? O2 C11 C12 118.0(3) . . ? C14 C11 C12 119.2(3) . . ? C13 C12 C11 119.6(4) . . ? C13 C12 N2 117.2(3) . . ? C11 C12 N2 123.1(4) . . ? C12 C13 C12 121.3(4) 4_565 . ? C12 C13 H13 119.3 4_565 . ? C12 C13 H13 119.3 . . ? C11 C14 C11 121.0(4) 4_565 . ? C11 C14 H14 119.5 4_565 . ? C11 C14 H14 119.5 . . ? O3 C15 C16 110.7(2) . . ? O3 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C18 C16 C17 118.6(3) . . ? C18 C16 C15 119.4(3) . . ? C17 C16 C15 121.9(3) . . ? C17 C17 C16 120.68(17) 4_565 . ? C17 C17 H17 119.7 4_565 . ? C16 C17 H17 119.7 . . ? C18 C18 C16 120.72(17) 4_565 . ? C18 C18 H18 119.6 4_565 . ? C16 C18 H18 119.6 . . ? C7 O1 C1 119.27(19) . . ? C11 O2 C3 119.2(2) . . ? C5 O3 C15 116.6(2) . . ? O4 N1 O5 123.8(2) . . ? O4 N1 C8 117.4(2) . . ? O5 N1 C8 118.9(2) . . ? O7 N2 O6 121.6(4) . . ? O7 N2 C12 118.8(4) . . ? O6 N2 C12 119.4(3) . . ? 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 -0.1(4) . . . . ? O1 C1 C2 C3 175.0(2) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? C1 C2 C3 O2 -173.5(2) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? O2 C3 C4 C5 173.5(2) . . . . ? C3 C4 C5 O3 -176.7(2) . . . . ? C3 C4 C5 C6 0.3(4) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? O1 C1 C6 C5 -174.8(2) . . . . ? O3 C5 C6 C1 176.8(2) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? O1 C7 C8 C9 -176.8(2) . . . . ? C10 C7 C8 C9 -0.1(4) . . . . ? O1 C7 C8 N1 5.8(4) . . . . ? C10 C7 C8 N1 -177.5(3) . . . . ? C7 C8 C9 C8 0.2(5) . . . 4_565 ? N1 C8 C9 C8 177.8(2) . . . 4_565 ? O1 C7 C10 C7 176.5(2) . . . 4_565 ? C8 C7 C10 C7 -0.1(5) . . . 4_565 ? O2 C11 C12 C13 -177.0(3) . . . . ? C14 C11 C12 C13 1.4(5) . . . . ? O2 C11 C12 N2 -1.1(4) . . . . ? C14 C11 C12 N2 177.3(3) . . . . ? C11 C12 C13 C12 -0.5(6) . . . 4_565 ? N2 C12 C13 C12 -176.6(3) . . . 4_565 ? O2 C11 C14 C11 176.0(2) . . . 4_565 ? C12 C11 C14 C11 -2.4(6) . . . 4_565 ? O3 C15 C16 C18 -52.5(3) . . . . ? O3 C15 C16 C17 124.4(3) . . . . ? C18 C16 C17 C17 0.0(3) . . . 4_565 ? C15 C16 C17 C17 -176.93(18) . . . 4_565 ? C17 C16 C18 C18 0.0(3) . . . 4_565 ? C15 C16 C18 C18 177.01(17) . . . 4_565 ? C10 C7 O1 C1 20.0(4) . . . . ? C8 C7 O1 C1 -163.4(2) . . . . ? C6 C1 O1 C7 -115.8(3) . . . . ? C2 C1 O1 C7 68.9(3) . . . . ? C14 C11 O2 C3 -1.1(4) . . . . ? C12 C11 O2 C3 177.3(2) . . . . ? C2 C3 O2 C11 -82.6(3) . . . . ? C4 C3 O2 C11 103.6(3) . . . . ? C4 C5 O3 C15 -32.9(4) . . . . ? C6 C5 O3 C15 150.0(2) . . . . ? C16 C15 O3 C5 -60.4(3) . . . . ? C9 C8 N1 O4 -2.5(3) . . . . ? C7 C8 N1 O4 175.0(2) . . . . ? C9 C8 N1 O5 177.6(2) . . . . ? C7 C8 N1 O5 -4.9(4) . . . . ? C13 C12 N2 O7 14.3(5) . . . . ? C11 C12 N2 O7 -161.6(3) . . . . ? C13 C12 N2 O6 -160.4(4) . . . . ? C11 C12 N2 O6 23.6(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.54 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.519 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.043 # Attachment 'host3.cif' data_sqz _database_code_depnum_ccdc_archive 'CCDC 659155' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H24 N4 O12, unknown solvate' _chemical_formula_sum 'C38 H24 N4 O12' _chemical_formula_weight 728.61 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1115(4) _cell_length_b 14.0678(4) _cell_length_c 17.4915(5) _cell_angle_alpha 79.9180(10) _cell_angle_beta 86.4530(10) _cell_angle_gamma 74.7700(10) _cell_volume 2830.77(15) _cell_formula_units_Z 3 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8678 _cell_measurement_theta_min 2.365 _cell_measurement_theta_max 25.984 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 30721 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10008 _reflns_number_gt 7259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; Squeeze used for disordered solvent species: Squeeze output: Summary and Remarks : N = NOTE, W = WARNING, E = ERROR #=============================================================================== N: No S.U.'s (esd) on observed/calculated parameters. #------------------------------------------------------------------------------- N: Number of moved primary input atoms: .................................. 4 N: Total Potential Solvent Accessible Void Vol .................. 503.4 Ang^3 N: Electron Count / Cell = 143 - To be included in D(calc), F000 & Mol.Wght. #=============================================================================== 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^)+(0.0375P)^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 10008 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _refine_ls_shift/su_max 0.001 _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 1.02093(12) -0.22135(11) 0.24816(9) 0.0248(3) Uani 1 1 d . . . C2 C 0.99485(12) -0.15590(11) 0.30188(9) 0.0261(4) Uani 1 1 d . . . C3 C 0.93990(13) -0.05634(11) 0.27664(9) 0.0282(4) Uani 1 1 d . . . H3 H 0.9243 -0.0106 0.3124 0.034 Uiso 1 1 calc R . . C4 C 0.90762(13) -0.02305(11) 0.20011(9) 0.0274(4) Uani 1 1 d . . . C5 C 0.92952(13) -0.09199(11) 0.14899(9) 0.0275(4) Uani 1 1 d . . . C6 C 0.98697(13) -0.18981(11) 0.17213(9) 0.0275(4) Uani 1 1 d . . . H6 H 1.0032 -0.2353 0.1362 0.033 Uiso 1 1 calc R . . C7 C 0.94784(13) -0.15467(11) 0.43592(9) 0.0277(4) Uani 1 1 d . . . C8 C 0.83407(14) -0.15321(12) 0.43510(9) 0.0359(4) Uani 1 1 d . . . H8 H 0.8039 -0.1718 0.3927 0.043 Uiso 1 1 calc R . . C9 C 0.76449(14) -0.12437(12) 0.49665(9) 0.0357(4) Uani 1 1 d . . . H9 H 0.6856 -0.1227 0.4960 0.043 Uiso 1 1 calc R . . C10 C 0.80612(14) -0.09771(11) 0.55954(9) 0.0299(4) Uani 1 1 d . . . C11 C 0.92105(15) -0.10016(12) 0.55834(9) 0.0341(4) Uani 1 1 d . . . H11 H 0.9518 -0.0822 0.6008 0.041 Uiso 1 1 calc R . . C12 C 0.99258(14) -0.12818(12) 0.49663(9) 0.0329(4) Uani 1 1 d . . . H12 H 1.0713 -0.1290 0.4965 0.040 Uiso 1 1 calc R . . C13 C 0.72700(15) -0.06656(11) 0.62674(9) 0.0360(4) Uani 1 1 d . . . H13A H 0.6666 -0.1031 0.6327 0.043 Uiso 1 1 calc R . . H13B H 0.7714 -0.0862 0.6752 0.043 Uiso 1 1 calc R . . C14 C 0.67112(14) 0.04415(11) 0.61615(9) 0.0301(4) Uani 1 1 d . . . C15 C 0.56148(14) 0.08423(12) 0.58694(10) 0.0359(4) Uani 1 1 d . . . H15 H 0.5194 0.0407 0.5748 0.043 Uiso 1 1 calc R . . C16 C 0.51224(14) 0.18601(12) 0.57516(10) 0.0356(4) Uani 1 1 d . . . H16 H 0.4372 0.2120 0.5551 0.043 Uiso 1 1 calc R . . C17 C 0.57275(13) 0.24918(11) 0.59278(9) 0.0287(4) Uani 1 1 d . . . C18 C 0.68099(13) 0.21232(12) 0.62307(9) 0.0320(4) Uani 1 1 d . . . H18 H 0.7220 0.2561 0.6362 0.038 Uiso 1 1 calc R . . C19 C 0.72866(14) 0.11015(12) 0.63388(9) 0.0326(4) Uani 1 1 d . . . H19 H 0.8036 0.0845 0.6542 0.039 Uiso 1 1 calc R . . C20 C 0.56961(13) 0.41711(11) 0.60032(9) 0.0281(4) Uani 1 1 d . . . C21 C 0.53744(13) 0.45325(11) 0.66966(9) 0.0285(4) Uani 1 1 d . . . C22 C 0.58358(13) 0.52511(11) 0.68980(9) 0.0307(4) Uani 1 1 d . . . H22 H 0.5603 0.5506 0.7367 0.037 Uiso 1 1 calc R . . C23 C 0.66318(14) 0.55939(11) 0.64167(9) 0.0299(4) Uani 1 1 d . . . C24 C 0.69814(14) 0.52399(11) 0.57193(9) 0.0309(4) Uani 1 1 d . . . C25 C 0.64839(13) 0.45365(11) 0.55154(9) 0.0301(4) Uani 1 1 d . . . H25 H 0.6688 0.4304 0.5035 0.036 Uiso 1 1 calc R . . C26 C 0.82402(14) 0.51657(12) 0.46258(9) 0.0332(4) Uani 1 1 d . . . C27 C 0.78941(14) 0.57215(12) 0.39170(10) 0.0366(4) Uani 1 1 d . . . H27 H 0.7338 0.6345 0.3882 0.044 Uiso 1 1 calc R . . C28 C 0.83712(14) 0.53568(12) 0.32511(10) 0.0352(4) Uani 1 1 d . . . H28 H 0.8141 0.5739 0.2757 0.042 Uiso 1 1 calc R . . C29 C 0.91757(13) 0.44474(11) 0.32918(9) 0.0293(4) Uani 1 1 d . . . C30 C 0.95095(15) 0.39073(12) 0.40175(10) 0.0376(4) Uani 1 1 d . . . H30 H 1.0065 0.3283 0.4056 0.045 Uiso 1 1 calc R . . C31 C 0.90452(15) 0.42627(12) 0.46902(10) 0.0396(4) Uani 1 1 d . . . H31 H 0.9280 0.3889 0.5186 0.048 Uiso 1 1 calc R . . C32 C 0.97151(14) 0.40756(12) 0.25576(9) 0.0340(4) Uani 1 1 d . . . H32A H 0.9488 0.4624 0.2113 0.041 Uiso 1 1 calc R . . H32B H 1.0557 0.3921 0.2599 0.041 Uiso 1 1 calc R . . C33 C 0.94069(13) 0.31614(11) 0.23789(8) 0.0275(4) Uani 1 1 d . . . C34 C 1.02433(14) 0.22914(11) 0.23151(9) 0.0309(4) Uani 1 1 d . . . H34 H 1.1017 0.2259 0.2412 0.037 Uiso 1 1 calc R . . C35 C 0.99813(14) 0.14659(11) 0.21134(9) 0.0313(4) Uani 1 1 d . . . H35 H 1.0568 0.0880 0.2062 0.038 Uiso 1 1 calc R . . C36 C 0.88611(13) 0.15118(11) 0.19894(8) 0.0269(4) Uani 1 1 d . . . C37 C 0.80028(14) 0.23632(11) 0.20480(9) 0.0304(4) Uani 1 1 d . . . H37 H 0.7230 0.2386 0.1959 0.036 Uiso 1 1 calc R . . C38 C 0.82821(14) 0.31800(12) 0.22376(9) 0.0318(4) Uani 1 1 d . . . H38 H 0.7694 0.3770 0.2273 0.038 Uiso 1 1 calc R . . C39 C 0.59680(13) 0.85844(12) 0.18685(9) 0.0296(4) Uani 1 1 d . . . C40 C 0.62946(13) 0.80419(11) 0.12588(9) 0.0287(4) Uani 1 1 d . . . C41 C 0.54502(13) 0.79547(11) 0.07967(9) 0.0311(4) Uani 1 1 d . . . H41 H 0.5657 0.7584 0.0382 0.037 Uiso 1 1 calc R . . C42 C 0.43143(13) 0.83983(11) 0.09308(9) 0.0298(4) Uani 1 1 d . . . C43 C 0.40182(13) 0.89671(12) 0.15243(9) 0.0323(4) Uani 1 1 d . . . C44 C 0.48446(13) 0.90648(12) 0.19881(9) 0.0335(4) Uani 1 1 d . . . H44 H 0.4640 0.9461 0.2387 0.040 Uiso 1 1 calc R . . C45 C 0.77506(13) 0.69348(12) 0.06427(9) 0.0299(4) Uani 1 1 d . . . C46 C 0.76334(14) 0.59909(12) 0.09171(9) 0.0345(4) Uani 1 1 d . . . H46 H 0.7318 0.5840 0.1421 0.041 Uiso 1 1 calc R . . C47 C 0.79784(14) 0.52606(12) 0.04527(9) 0.0328(4) Uani 1 1 d . . . H47 H 0.7894 0.4607 0.0641 0.039 Uiso 1 1 calc R . . C48 C 0.84451(13) 0.54644(11) -0.02822(9) 0.0279(4) Uani 1 1 d . . . C49 C 0.85614(14) 0.64251(12) -0.05349(9) 0.0360(4) Uani 1 1 d . . . H49 H 0.8888 0.6578 -0.1034 0.043 Uiso 1 1 calc R . . C50 C 0.82143(14) 0.71710(12) -0.00803(10) 0.0372(4) Uani 1 1 d . . . H50 H 0.8295 0.7826 -0.0264 0.045 Uiso 1 1 calc R . . C51 C 0.88552(14) 0.46772(12) -0.08006(9) 0.0328(4) Uani 1 1 d . . . H51A H 0.8801 0.5016 -0.1348 0.039 Uiso 1 1 calc R . . H51B H 0.9673 0.4351 -0.0696 0.039 Uiso 1 1 calc R . . C52 C 0.82100(13) 0.38751(12) -0.07062(9) 0.0286(4) Uani 1 1 d . . . C53 C 0.84414(13) 0.30649(11) -0.01084(9) 0.0310(4) Uani 1 1 d . . . H53 H 0.9017 0.3012 0.0253 0.037 Uiso 1 1 calc R . . C54 C 0.78535(13) 0.23321(12) -0.00259(9) 0.0304(4) Uani 1 1 d . . . H54 H 0.8017 0.1785 0.0390 0.037 Uiso 1 1 calc R . . C55 C 0.70287(13) 0.24058(11) -0.05539(9) 0.0282(4) Uani 1 1 d . . . C56 C 0.67811(14) 0.31923(12) -0.11598(9) 0.0352(4) Uani 1 1 d . . . H56 H 0.6214 0.3234 -0.1524 0.042 Uiso 1 1 calc R . . C57 C 0.73748(14) 0.39230(12) -0.12287(9) 0.0339(4) Uani 1 1 d . . . H57 H 0.7205 0.4470 -0.1644 0.041 Uiso 1 1 calc R . . N1 N 1.07791(11) -0.32709(9) 0.27107(7) 0.0300(3) Uani 1 1 d . . . N2 N 0.45489(11) 0.41850(11) 0.72387(8) 0.0365(3) Uani 1 1 d . . . N3 N 0.71289(13) 0.63235(11) 0.66778(10) 0.0434(4) Uani 1 1 d . . . N4 N 0.88585(14) -0.06405(10) 0.06958(8) 0.0387(4) Uani 1 1 d . . . N5 N 0.67891(12) 0.86248(11) 0.24320(8) 0.0346(3) Uani 1 1 d . . . N6 N 0.28351(12) 0.94933(12) 0.16692(8) 0.0428(4) Uani 1 1 d . . . O1 O 1.02441(9) -0.19158(7) 0.37755(6) 0.0322(3) Uani 1 1 d . . . O2 O 0.51850(9) 0.35114(8) 0.57605(6) 0.0335(3) Uani 1 1 d . . . O3 O 0.78051(10) 0.55830(8) 0.52937(6) 0.0418(3) Uani 1 1 d . . . O4 O 0.85300(9) 0.07367(7) 0.17305(6) 0.0337(3) Uani 1 1 d . . . O5 O 1.04812(10) -0.38754(8) 0.23992(6) 0.0373(3) Uani 1 1 d . . . O6 O 1.15330(11) -0.34975(8) 0.31951(7) 0.0466(3) Uani 1 1 d . . . O7 O 0.44189(10) 0.33506(9) 0.72461(7) 0.0495(3) Uani 1 1 d . . . O8 O 0.40328(11) 0.47477(10) 0.76750(8) 0.0589(4) Uani 1 1 d . . . O9 O 0.73221(11) 0.62158(10) 0.73684(8) 0.0532(3) Uani 1 1 d . . . O10 O 0.73018(17) 0.70002(11) 0.62021(9) 0.0914(6) Uani 1 1 d . . . O11 O 0.78741(12) -0.01303(9) 0.06095(7) 0.0561(4) Uani 1 1 d . . . O12 O 0.94766(12) -0.09769(9) 0.01765(7) 0.0542(4) Uani 1 1 d . . . O13 O 0.74317(9) 0.76660(8) 0.11279(6) 0.0354(3) Uani 1 1 d . . . O14 O 0.64863(9) 0.16269(8) -0.04220(6) 0.0352(3) Uani 1 1 d . . . O15 O 0.66036(11) 0.93916(10) 0.27139(8) 0.0568(4) Uani 1 1 d . . . O16 O 0.75758(10) 0.78906(9) 0.26154(7) 0.0418(3) Uani 1 1 d . . . O17 O 0.20782(11) 0.90898(10) 0.16109(8) 0.0580(4) Uani 1 1 d . . . O18 O 0.26781(11) 1.03235(10) 0.18551(8) 0.0594(4) Uani 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 C1 0.0226(8) 0.0210(8) 0.0311(9) -0.0056(7) 0.0017(7) -0.0056(7) C2 0.0249(8) 0.0286(9) 0.0257(9) -0.0042(7) 0.0002(7) -0.0089(7) C3 0.0308(9) 0.0254(9) 0.0297(9) -0.0099(7) 0.0000(7) -0.0061(7) C4 0.0275(9) 0.0224(9) 0.0319(9) -0.0043(7) -0.0031(7) -0.0050(7) C5 0.0324(9) 0.0271(9) 0.0247(9) -0.0044(7) -0.0025(7) -0.0098(7) C6 0.0288(9) 0.0270(9) 0.0293(9) -0.0102(7) 0.0041(7) -0.0093(7) C7 0.0342(9) 0.0214(8) 0.0257(9) -0.0054(7) 0.0003(7) -0.0034(7) C8 0.0403(10) 0.0420(10) 0.0291(9) -0.0120(8) -0.0038(8) -0.0122(8) C9 0.0333(10) 0.0397(10) 0.0354(10) -0.0091(8) -0.0002(8) -0.0099(8) C10 0.0402(10) 0.0192(8) 0.0292(9) -0.0035(7) 0.0020(8) -0.0065(7) C11 0.0443(11) 0.0316(9) 0.0294(9) -0.0102(7) -0.0055(8) -0.0105(8) C12 0.0326(9) 0.0332(9) 0.0344(10) -0.0088(8) -0.0029(8) -0.0083(8) C13 0.0467(11) 0.0301(9) 0.0323(10) -0.0078(7) 0.0040(8) -0.0110(8) C14 0.0369(10) 0.0278(9) 0.0260(9) -0.0080(7) 0.0062(7) -0.0086(8) C15 0.0385(10) 0.0321(10) 0.0436(11) -0.0143(8) 0.0019(8) -0.0156(8) C16 0.0289(9) 0.0377(10) 0.0428(10) -0.0128(8) -0.0021(8) -0.0085(8) C17 0.0303(9) 0.0256(9) 0.0302(9) -0.0068(7) 0.0040(7) -0.0067(7) C18 0.0308(9) 0.0278(9) 0.0402(10) -0.0097(7) -0.0017(8) -0.0095(8) C19 0.0275(9) 0.0327(10) 0.0371(10) -0.0088(7) -0.0016(8) -0.0046(8) C20 0.0273(9) 0.0221(8) 0.0322(9) -0.0036(7) -0.0035(7) -0.0015(7) C21 0.0249(9) 0.0240(9) 0.0325(9) -0.0006(7) 0.0017(7) -0.0023(7) C22 0.0342(9) 0.0269(9) 0.0272(9) -0.0053(7) 0.0028(7) -0.0012(8) C23 0.0363(9) 0.0201(8) 0.0323(9) -0.0060(7) 0.0027(8) -0.0053(7) C24 0.0351(9) 0.0230(9) 0.0324(9) -0.0033(7) 0.0060(8) -0.0061(8) C25 0.0339(9) 0.0272(9) 0.0277(9) -0.0063(7) 0.0026(7) -0.0049(8) C26 0.0391(10) 0.0352(10) 0.0317(10) -0.0125(8) 0.0105(8) -0.0186(8) C27 0.0359(10) 0.0315(10) 0.0423(11) -0.0106(8) 0.0039(8) -0.0063(8) C28 0.0393(10) 0.0350(10) 0.0319(10) -0.0059(8) 0.0003(8) -0.0108(8) C29 0.0330(9) 0.0282(9) 0.0315(9) -0.0072(7) 0.0054(7) -0.0158(8) C30 0.0443(11) 0.0260(9) 0.0402(11) -0.0064(8) 0.0052(9) -0.0060(8) C31 0.0553(12) 0.0330(10) 0.0302(10) -0.0022(8) 0.0034(9) -0.0135(9) C32 0.0356(10) 0.0352(10) 0.0343(10) -0.0097(8) 0.0072(8) -0.0137(8) C33 0.0330(9) 0.0283(9) 0.0214(8) -0.0045(7) 0.0058(7) -0.0091(7) C34 0.0274(9) 0.0316(9) 0.0322(9) -0.0005(7) 0.0004(7) -0.0082(8) C35 0.0295(9) 0.0230(9) 0.0368(10) -0.0046(7) 0.0023(8) 0.0003(7) C36 0.0345(9) 0.0232(8) 0.0226(8) -0.0051(6) -0.0001(7) -0.0061(7) C37 0.0289(9) 0.0294(9) 0.0330(9) -0.0065(7) -0.0008(7) -0.0067(7) C38 0.0321(9) 0.0259(9) 0.0354(10) -0.0091(7) 0.0045(8) -0.0026(7) C39 0.0275(9) 0.0333(9) 0.0317(9) -0.0118(7) 0.0002(7) -0.0105(8) C40 0.0258(9) 0.0270(9) 0.0341(9) -0.0073(7) 0.0025(7) -0.0073(7) C41 0.0336(10) 0.0304(9) 0.0320(9) -0.0112(7) 0.0014(8) -0.0094(8) C42 0.0295(9) 0.0307(9) 0.0310(9) -0.0037(7) -0.0049(7) -0.0108(8) C43 0.0229(9) 0.0358(10) 0.0371(10) -0.0083(8) 0.0028(8) -0.0050(8) C44 0.0300(9) 0.0384(10) 0.0340(10) -0.0152(8) 0.0044(8) -0.0070(8) C45 0.0270(9) 0.0335(9) 0.0324(9) -0.0155(7) 0.0016(7) -0.0072(7) C46 0.0371(10) 0.0414(10) 0.0264(9) -0.0088(8) 0.0084(8) -0.0123(8) C47 0.0398(10) 0.0298(9) 0.0311(10) -0.0073(7) 0.0046(8) -0.0126(8) C48 0.0261(9) 0.0321(9) 0.0273(9) -0.0089(7) 0.0015(7) -0.0085(7) C49 0.0429(10) 0.0386(10) 0.0292(9) -0.0089(8) 0.0102(8) -0.0154(8) C50 0.0441(11) 0.0297(9) 0.0408(11) -0.0084(8) 0.0053(9) -0.0144(8) C51 0.0344(9) 0.0368(10) 0.0308(9) -0.0124(7) 0.0086(8) -0.0131(8) C52 0.0269(9) 0.0322(9) 0.0288(9) -0.0151(7) 0.0055(7) -0.0061(7) C53 0.0285(9) 0.0337(9) 0.0319(9) -0.0114(8) -0.0048(7) -0.0051(8) C54 0.0335(9) 0.0279(9) 0.0291(9) -0.0063(7) -0.0063(7) -0.0042(8) C55 0.0256(9) 0.0289(9) 0.0314(9) -0.0083(7) 0.0004(7) -0.0071(7) C56 0.0336(10) 0.0411(10) 0.0322(10) -0.0027(8) -0.0106(8) -0.0118(8) C57 0.0377(10) 0.0321(9) 0.0310(9) -0.0031(7) -0.0020(8) -0.0082(8) N1 0.0325(8) 0.0274(8) 0.0301(8) -0.0081(6) 0.0032(7) -0.0063(6) N2 0.0308(8) 0.0373(9) 0.0383(9) -0.0027(7) 0.0035(7) -0.0065(7) N3 0.0547(10) 0.0341(9) 0.0451(10) -0.0169(8) 0.0205(8) -0.0159(8) N4 0.0538(10) 0.0261(8) 0.0353(9) -0.0069(7) -0.0112(8) -0.0052(8) N5 0.0273(8) 0.0430(9) 0.0367(8) -0.0172(7) 0.0008(7) -0.0078(7) N6 0.0289(8) 0.0538(10) 0.0464(10) -0.0168(8) -0.0003(7) -0.0061(8) O1 0.0350(6) 0.0312(6) 0.0261(6) -0.0074(5) -0.0022(5) 0.0010(5) O2 0.0294(6) 0.0271(6) 0.0436(7) -0.0064(5) -0.0040(5) -0.0055(5) O3 0.0554(8) 0.0412(7) 0.0386(7) -0.0184(5) 0.0201(6) -0.0268(6) O4 0.0433(7) 0.0212(6) 0.0360(7) -0.0065(5) -0.0127(5) -0.0031(5) O5 0.0496(7) 0.0258(6) 0.0407(7) -0.0121(5) 0.0020(6) -0.0132(6) O6 0.0499(8) 0.0332(7) 0.0518(8) -0.0120(6) -0.0210(7) 0.0058(6) O7 0.0535(8) 0.0367(8) 0.0578(9) -0.0019(6) 0.0139(7) -0.0176(6) O8 0.0586(9) 0.0627(9) 0.0612(9) -0.0265(7) 0.0337(7) -0.0226(7) O9 0.0538(8) 0.0616(9) 0.0533(9) -0.0248(7) -0.0002(7) -0.0207(7) O10 0.1833(19) 0.0558(10) 0.0603(10) -0.0253(8) 0.0450(11) -0.0752(12) O11 0.0629(9) 0.0422(8) 0.0568(9) -0.0144(6) -0.0297(7) 0.0079(7) O12 0.0755(10) 0.0526(8) 0.0328(7) -0.0146(6) 0.0002(7) -0.0086(7) O13 0.0254(6) 0.0410(7) 0.0458(7) -0.0252(6) 0.0039(5) -0.0080(5) O14 0.0361(7) 0.0352(7) 0.0361(7) 0.0003(5) -0.0110(5) -0.0141(5) O15 0.0469(8) 0.0615(9) 0.0712(9) -0.0453(8) -0.0084(7) -0.0057(7) O16 0.0321(7) 0.0483(8) 0.0443(7) -0.0127(6) -0.0050(6) -0.0050(6) O17 0.0295(7) 0.0723(10) 0.0790(10) -0.0267(8) 0.0042(7) -0.0172(7) O18 0.0380(8) 0.0613(9) 0.0810(10) -0.0395(8) -0.0001(7) 0.0016(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 C1 C6 1.378(2) . ? C1 C2 1.394(2) . ? C1 N1 1.4614(19) . ? C2 O1 1.3651(17) . ? C2 C3 1.389(2) . ? C3 C4 1.383(2) . ? C3 H3 0.9500 . ? C4 O4 1.3613(17) . ? C4 C5 1.396(2) . ? C5 C6 1.371(2) . ? C5 N4 1.468(2) . ? C6 H6 0.9500 . ? C7 C12 1.370(2) . ? C7 C8 1.374(2) . ? C7 O1 1.4099(17) . ? C8 C9 1.377(2) . ? C8 H8 0.9500 . ? C9 C10 1.385(2) . ? C9 H9 0.9500 . ? C10 C11 1.382(2) . ? C10 C13 1.521(2) . ? C11 C12 1.387(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.510(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.382(2) . ? C14 C15 1.390(2) . ? C15 C16 1.383(2) . ? C15 H15 0.9500 . ? C16 C17 1.374(2) . ? C16 H16 0.9500 . ? C17 C18 1.379(2) . ? C17 O2 1.3987(17) . ? C18 C19 1.385(2) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 O2 1.3774(18) . ? C20 C25 1.381(2) . ? C20 C21 1.391(2) . ? C21 C22 1.380(2) . ? C21 N2 1.454(2) . ? C22 C23 1.368(2) . ? C22 H22 0.9500 . ? C23 C24 1.398(2) . ? C23 N3 1.465(2) . ? C24 O3 1.3483(18) . ? C24 C25 1.390(2) . ? C25 H25 0.9500 . ? C26 C27 1.370(2) . ? C26 C31 1.375(2) . ? C26 O3 1.4101(18) . ? C27 C28 1.387(2) . ? C27 H27 0.9500 . ? C28 C29 1.383(2) . ? C28 H28 0.9500 . ? C29 C30 1.384(2) . ? C29 C32 1.517(2) . ? C30 C31 1.388(2) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.516(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.385(2) . ? C33 C38 1.392(2) . ? C34 C35 1.387(2) . ? C34 H34 0.9500 . ? C35 C36 1.370(2) . ? C35 H35 0.9500 . ? C36 C37 1.379(2) . ? C36 O4 1.4072(17) . ? C37 C38 1.377(2) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.372(2) . ? C39 C40 1.397(2) . ? C39 N5 1.461(2) . ? C40 O13 1.3600(17) . ? C40 C41 1.385(2) . ? C41 C42 1.377(2) . ? C41 H41 0.9500 . ? C42 O14 1.3674(18) 2_665 ? C42 C43 1.393(2) . ? C43 C44 1.375(2) . ? C43 N6 1.459(2) . ? C44 H44 0.9500 . ? C45 C46 1.372(2) . ? C45 C50 1.374(2) . ? C45 O13 1.4086(17) . ? C46 C47 1.384(2) . ? C46 H46 0.9500 . ? C47 C48 1.386(2) . ? C47 H47 0.9500 . ? C48 C49 1.387(2) . ? C48 C51 1.517(2) . ? C49 C50 1.389(2) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.514(2) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C57 1.386(2) . ? C52 C53 1.386(2) . ? C53 C54 1.383(2) . ? C53 H53 0.9500 . ? C54 C55 1.374(2) . ? C54 H54 0.9500 . ? C55 C56 1.375(2) . ? C55 O14 1.3987(18) . ? C56 C57 1.387(2) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? N1 O5 1.2240(15) . ? N1 O6 1.2254(16) . ? N2 O8 1.2216(17) . ? N2 O7 1.2224(17) . ? N3 O10 1.2035(18) . ? N3 O9 1.2204(18) . ? N4 O12 1.2206(17) . ? N4 O11 1.2223(17) . ? N5 O16 1.2175(16) . ? N5 O15 1.2257(16) . ? N6 O17 1.2159(18) . ? N6 O18 1.2306(18) . ? O14 C42 1.3674(18) 2_665 ? 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 C6 C1 C2 120.90(14) . . ? C6 C1 N1 117.34(13) . . ? C2 C1 N1 121.62(13) . . ? O1 C2 C3 122.09(13) . . ? O1 C2 C1 118.99(13) . . ? C3 C2 C1 118.93(14) . . ? C4 C3 C2 120.77(14) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? O4 C4 C3 122.69(13) . . ? O4 C4 C5 118.68(14) . . ? C3 C4 C5 118.61(14) . . ? C6 C5 C4 121.47(14) . . ? C6 C5 N4 117.17(13) . . ? C4 C5 N4 121.25(14) . . ? C5 C6 C1 119.17(14) . . ? C5 C6 H6 120.4 . . ? C1 C6 H6 120.4 . . ? C12 C7 C8 121.19(15) . . ? C12 C7 O1 117.61(14) . . ? C8 C7 O1 120.99(14) . . ? C7 C8 C9 118.92(15) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C8 C9 C10 121.90(16) . . ? C8 C9 H9 119.0 . . ? C10 C9 H9 119.0 . . ? C11 C10 C9 117.52(15) . . ? C11 C10 C13 121.91(14) . . ? C9 C10 C13 120.56(15) . . ? C10 C11 C12 121.57(15) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C7 C12 C11 118.89(15) . . ? C7 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C14 C13 C10 113.40(13) . . ? C14 C13 H13A 108.9 . . ? C10 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? C10 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C19 C14 C15 117.28(14) . . ? C19 C14 C13 120.87(15) . . ? C15 C14 C13 121.83(14) . . ? C16 C15 C14 121.50(15) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C15 119.41(15) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.91(15) . . ? C16 C17 O2 115.65(14) . . ? C18 C17 O2 123.42(14) . . ? C17 C18 C19 118.55(15) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C14 C19 C18 122.34(15) . . ? C14 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? O2 C20 C25 118.71(14) . . ? O2 C20 C21 121.62(14) . . ? C25 C20 C21 119.49(14) . . ? C22 C21 C20 120.50(14) . . ? C22 C21 N2 116.89(14) . . ? C20 C21 N2 122.62(14) . . ? C23 C22 C21 119.48(14) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 121.46(15) . . ? C22 C23 N3 117.00(14) . . ? C24 C23 N3 121.51(14) . . ? O3 C24 C25 123.86(14) . . ? O3 C24 C23 117.85(14) . . ? C25 C24 C23 118.27(14) . . ? C20 C25 C24 120.77(14) . . ? C20 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C27 C26 C31 121.64(15) . . ? C27 C26 O3 117.73(15) . . ? C31 C26 O3 120.47(15) . . ? C26 C27 C28 118.74(16) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C29 C28 C27 121.34(16) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C30 118.39(15) . . ? C28 C29 C32 120.58(14) . . ? C30 C29 C32 120.97(15) . . ? C29 C30 C31 121.06(16) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C26 C31 C30 118.82(16) . . ? C26 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? C33 C32 C29 115.65(13) . . ? C33 C32 H32A 108.4 . . ? C29 C32 H32A 108.4 . . ? C33 C32 H32B 108.4 . . ? C29 C32 H32B 108.4 . . ? H32A C32 H32B 107.4 . . ? C34 C33 C38 117.59(14) . . ? C34 C33 C32 121.06(14) . . ? C38 C33 C32 121.28(14) . . ? C33 C34 C35 121.72(15) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? C36 C35 C34 118.76(15) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C35 C36 C37 121.32(14) . . ? C35 C36 O4 122.41(14) . . ? C37 C36 O4 116.04(13) . . ? C38 C37 C36 119.05(15) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? C37 C38 C33 121.54(15) . . ? C37 C38 H38 119.2 . . ? C33 C38 H38 119.2 . . ? C44 C39 C40 121.22(14) . . ? C44 C39 N5 116.80(13) . . ? C40 C39 N5 121.91(14) . . ? O13 C40 C41 123.36(14) . . ? O13 C40 C39 118.09(14) . . ? C41 C40 C39 118.48(14) . . ? C42 C41 C40 120.85(14) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? O14 C42 C41 119.23(14) 2_665 . ? O14 C42 C43 120.92(14) 2_665 . ? C41 C42 C43 119.37(14) . . ? C44 C43 C42 120.61(14) . . ? C44 C43 N6 117.59(14) . . ? C42 C43 N6 121.79(14) . . ? C39 C44 C43 119.36(14) . . ? C39 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C46 C45 C50 121.58(14) . . ? C46 C45 O13 119.01(14) . . ? C50 C45 O13 119.36(14) . . ? C45 C46 C47 119.32(15) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? C46 C47 C48 121.21(15) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C47 C48 C49 117.70(14) . . ? C47 C48 C51 122.65(14) . . ? C49 C48 C51 119.63(14) . . ? C48 C49 C50 122.04(15) . . ? C48 C49 H49 119.0 . . ? C50 C49 H49 119.0 . . ? C45 C50 C49 118.15(15) . . ? C45 C50 H50 120.9 . . ? C49 C50 H50 120.9 . . ? C52 C51 C48 115.46(13) . . ? C52 C51 H51A 108.4 . . ? C48 C51 H51A 108.4 . . ? C52 C51 H51B 108.4 . . ? C48 C51 H51B 108.4 . . ? H51A C51 H51B 107.5 . . ? C57 C52 C53 117.76(14) . . ? C57 C52 C51 120.52(14) . . ? C53 C52 C51 121.71(14) . . ? C54 C53 C52 121.54(14) . . ? C54 C53 H53 119.2 . . ? C52 C53 H53 119.2 . . ? C55 C54 C53 119.08(15) . . ? C55 C54 H54 120.5 . . ? C53 C54 H54 120.5 . . ? C54 C55 C56 121.21(15) . . ? C54 C55 O14 114.72(13) . . ? C56 C55 O14 124.07(14) . . ? C55 C56 C57 118.79(15) . . ? C55 C56 H56 120.6 . . ? C57 C56 H56 120.6 . . ? C52 C57 C56 121.62(15) . . ? C52 C57 H57 119.2 . . ? C56 C57 H57 119.2 . . ? O5 N1 O6 124.02(13) . . ? O5 N1 C1 117.81(13) . . ? O6 N1 C1 118.17(13) . . ? O8 N2 O7 123.48(14) . . ? O8 N2 C21 117.35(14) . . ? O7 N2 C21 119.15(14) . . ? O10 N3 O9 124.09(16) . . ? O10 N3 C23 118.14(16) . . ? O9 N3 C23 117.76(14) . . ? O12 N4 O11 124.61(15) . . ? O12 N4 C5 117.99(15) . . ? O11 N4 C5 117.27(14) . . ? O16 N5 O15 124.40(14) . . ? O16 N5 C39 118.63(13) . . ? O15 N5 C39 116.90(14) . . ? O17 N6 O18 124.38(15) . . ? O17 N6 C43 118.97(15) . . ? O18 N6 C43 116.64(14) . . ? C2 O1 C7 118.12(11) . . ? C20 O2 C17 117.98(11) . . ? C24 O3 C26 118.48(12) . . ? C4 O4 C36 119.56(11) . . ? C40 O13 C45 117.57(12) . . ? C42 O14 C55 119.69(12) 2_665 . ? 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 O1 176.33(13) . . . . ? N1 C1 C2 O1 0.6(2) . . . . ? C6 C1 C2 C3 -3.9(2) . . . . ? N1 C1 C2 C3 -179.56(13) . . . . ? O1 C2 C3 C4 -177.85(14) . . . . ? C1 C2 C3 C4 2.4(2) . . . . ? C2 C3 C4 O4 179.58(14) . . . . ? C2 C3 C4 C5 1.2(2) . . . . ? O4 C4 C5 C6 178.17(14) . . . . ? C3 C4 C5 C6 -3.4(2) . . . . ? O4 C4 C5 N4 -5.6(2) . . . . ? C3 C4 C5 N4 172.89(14) . . . . ? C4 C5 C6 C1 1.9(2) . . . . ? N4 C5 C6 C1 -174.50(14) . . . . ? C2 C1 C6 C5 1.8(2) . . . . ? N1 C1 C6 C5 177.64(13) . . . . ? C12 C7 C8 C9 0.1(2) . . . . ? O1 C7 C8 C9 174.62(14) . . . . ? C7 C8 C9 C10 -0.6(2) . . . . ? C8 C9 C10 C11 0.5(2) . . . . ? C8 C9 C10 C13 -179.78(15) . . . . ? C9 C10 C11 C12 0.0(2) . . . . ? C13 C10 C11 C12 -179.67(14) . . . . ? C8 C7 C12 C11 0.5(2) . . . . ? O1 C7 C12 C11 -174.27(13) . . . . ? C10 C11 C12 C7 -0.5(2) . . . . ? C11 C10 C13 C14 89.92(19) . . . . ? C9 C10 C13 C14 -89.75(18) . . . . ? C10 C13 C14 C19 -81.97(19) . . . . ? C10 C13 C14 C15 96.69(18) . . . . ? C19 C14 C15 C16 0.7(2) . . . . ? C13 C14 C15 C16 -177.98(15) . . . . ? C14 C15 C16 C17 -0.1(2) . . . . ? C15 C16 C17 C18 -1.0(2) . . . . ? C15 C16 C17 O2 177.41(14) . . . . ? C16 C17 C18 C19 1.4(2) . . . . ? O2 C17 C18 C19 -176.90(14) . . . . ? C15 C14 C19 C18 -0.3(2) . . . . ? C13 C14 C19 C18 178.39(14) . . . . ? C17 C18 C19 C14 -0.7(2) . . . . ? O2 C20 C21 C22 -174.96(13) . . . . ? C25 C20 C21 C22 0.0(2) . . . . ? O2 C20 C21 N2 4.9(2) . . . . ? C25 C20 C21 N2 179.90(14) . . . . ? C20 C21 C22 C23 -1.2(2) . . . . ? N2 C21 C22 C23 178.88(13) . . . . ? C21 C22 C23 C24 0.7(2) . . . . ? C21 C22 C23 N3 -177.33(14) . . . . ? C22 C23 C24 O3 -177.19(14) . . . . ? N3 C23 C24 O3 0.7(2) . . . . ? C22 C23 C24 C25 1.1(2) . . . . ? N3 C23 C24 C25 179.01(14) . . . . ? O2 C20 C25 C24 176.92(13) . . . . ? C21 C20 C25 C24 1.8(2) . . . . ? O3 C24 C25 C20 175.85(14) . . . . ? C23 C24 C25 C20 -2.3(2) . . . . ? C31 C26 C27 C28 0.1(2) . . . . ? O3 C26 C27 C28 175.59(14) . . . . ? C26 C27 C28 C29 0.5(2) . . . . ? C27 C28 C29 C30 -0.7(2) . . . . ? C27 C28 C29 C32 -178.09(14) . . . . ? C28 C29 C30 C31 0.4(2) . . . . ? C32 C29 C30 C31 177.77(15) . . . . ? C27 C26 C31 C30 -0.4(2) . . . . ? O3 C26 C31 C30 -175.76(14) . . . . ? C29 C30 C31 C26 0.1(3) . . . . ? C28 C29 C32 C33 -112.67(17) . . . . ? C30 C29 C32 C33 70.0(2) . . . . ? C29 C32 C33 C34 -120.64(16) . . . . ? C29 C32 C33 C38 62.4(2) . . . . ? C38 C33 C34 C35 0.4(2) . . . . ? C32 C33 C34 C35 -176.71(14) . . . . ? C33 C34 C35 C36 -1.3(2) . . . . ? C34 C35 C36 C37 1.2(2) . . . . ? C34 C35 C36 O4 175.43(13) . . . . ? C35 C36 C37 C38 -0.2(2) . . . . ? O4 C36 C37 C38 -174.84(13) . . . . ? C36 C37 C38 C33 -0.7(2) . . . . ? C34 C33 C38 C37 0.6(2) . . . . ? C32 C33 C38 C37 177.67(14) . . . . ? C44 C39 C40 O13 173.74(14) . . . . ? N5 C39 C40 O13 -9.6(2) . . . . ? C44 C39 C40 C41 -3.2(2) . . . . ? N5 C39 C40 C41 173.44(14) . . . . ? O13 C40 C41 C42 -176.34(14) . . . . ? C39 C40 C41 C42 0.5(2) . . . . ? C40 C41 C42 O14 174.16(14) . . . 2_665 ? C40 C41 C42 C43 2.0(2) . . . . ? O14 C42 C43 C44 -173.84(14) 2_665 . . . ? C41 C42 C43 C44 -1.8(2) . . . . ? O14 C42 C43 N6 5.0(2) 2_665 . . . ? C41 C42 C43 N6 177.02(15) . . . . ? C40 C39 C44 C43 3.4(2) . . . . ? N5 C39 C44 C43 -173.39(15) . . . . ? C42 C43 C44 C39 -0.9(2) . . . . ? N6 C43 C44 C39 -179.77(15) . . . . ? C50 C45 C46 C47 -0.7(2) . . . . ? O13 C45 C46 C47 -177.99(14) . . . . ? C45 C46 C47 C48 0.3(2) . . . . ? C46 C47 C48 C49 0.4(2) . . . . ? C46 C47 C48 C51 178.71(15) . . . . ? C47 C48 C49 C50 -0.8(2) . . . . ? C51 C48 C49 C50 -179.16(15) . . . . ? C46 C45 C50 C49 0.3(2) . . . . ? O13 C45 C50 C49 177.59(14) . . . . ? C48 C49 C50 C45 0.5(3) . . . . ? C47 C48 C51 C52 31.5(2) . . . . ? C49 C48 C51 C52 -150.24(15) . . . . ? C48 C51 C52 C57 100.25(17) . . . . ? C48 C51 C52 C53 -80.82(19) . . . . ? C57 C52 C53 C54 -0.8(2) . . . . ? C51 C52 C53 C54 -179.74(14) . . . . ? C52 C53 C54 C55 0.6(2) . . . . ? C53 C54 C55 C56 0.0(2) . . . . ? C53 C54 C55 O14 179.79(13) . . . . ? C54 C55 C56 C57 -0.5(2) . . . . ? O14 C55 C56 C57 179.77(14) . . . . ? C53 C52 C57 C56 0.3(2) . . . . ? C51 C52 C57 C56 179.27(14) . . . . ? C55 C56 C57 C52 0.3(2) . . . . ? C6 C1 N1 O5 -33.43(19) . . . . ? C2 C1 N1 O5 142.41(14) . . . . ? C6 C1 N1 O6 145.76(14) . . . . ? C2 C1 N1 O6 -38.4(2) . . . . ? C22 C21 N2 O8 24.3(2) . . . . ? C20 C21 N2 O8 -155.53(15) . . . . ? C22 C21 N2 O7 -154.47(14) . . . . ? C20 C21 N2 O7 25.7(2) . . . . ? C22 C23 N3 O10 -140.99(17) . . . . ? C24 C23 N3 O10 41.0(2) . . . . ? C22 C23 N3 O9 37.7(2) . . . . ? C24 C23 N3 O9 -140.32(16) . . . . ? C6 C5 N4 O12 -42.4(2) . . . . ? C4 C5 N4 O12 141.23(15) . . . . ? C6 C5 N4 O11 133.67(15) . . . . ? C4 C5 N4 O11 -42.7(2) . . . . ? C44 C39 N5 O16 142.81(15) . . . . ? C40 C39 N5 O16 -34.0(2) . . . . ? C44 C39 N5 O15 -34.1(2) . . . . ? C40 C39 N5 O15 149.09(16) . . . . ? C44 C43 N6 O17 -141.97(16) . . . . ? C42 C43 N6 O17 39.2(2) . . . . ? C44 C43 N6 O18 37.1(2) . . . . ? C42 C43 N6 O18 -141.81(17) . . . . ? C3 C2 O1 C7 38.50(19) . . . . ? C1 C2 O1 C7 -141.71(14) . . . . ? C12 C7 O1 C2 -134.74(14) . . . . ? C8 C7 O1 C2 50.53(19) . . . . ? C25 C20 O2 C17 88.94(17) . . . . ? C21 C20 O2 C17 -96.02(17) . . . . ? C16 C17 O2 C20 172.99(13) . . . . ? C18 C17 O2 C20 -8.7(2) . . . . ? C25 C24 O3 C26 -3.9(2) . . . . ? C23 C24 O3 C26 174.30(14) . . . . ? C27 C26 O3 C24 104.51(17) . . . . ? C31 C26 O3 C24 -80.0(2) . . . . ? C3 C4 O4 C36 39.7(2) . . . . ? C5 C4 O4 C36 -141.88(14) . . . . ? C35 C36 O4 C4 38.2(2) . . . . ? C37 C36 O4 C4 -147.27(14) . . . . ? C41 C40 O13 C45 -17.7(2) . . . . ? C39 C40 O13 C45 165.46(14) . . . . ? C46 C45 O13 C40 -72.66(19) . . . . ? C50 C45 O13 C40 109.99(17) . . . . ? C54 C55 O14 C42 -177.20(14) . . . 2_665 ? C56 C55 O14 C42 2.5(2) . . . 2_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.189 _refine_diff_density_min -0.166 _refine_diff_density_rms 0.034