# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'David Bardelang' _publ_contact_author_email DAVID.BARDELANG@NRC-CNRC.GC.CA _publ_section_title ; Single-crystal to single-crystal phase transition of cucurbit[5]uril hydrochloride hydrates : large water-filled channels transforming to layers of unusual stability. ; loop_ _publ_author_name 'David Bardelang' 'Roberto Anedda' 'Donald M Leek' 'Igor Moudrakovski' 'Christopher I Ratcliffe' ; J.Ripmeester ; 'Konstantin A Udachin' # Attachment 'dav6revised.cif' data_dav6 _database_code_depnum_ccdc_archive 'CCDC 687155' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common cucurbit(5)uril _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H45 Cl2 N20 O17.50' _chemical_formula_weight 1036.76 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pmn2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _cell_length_a 14.280(4) _cell_length_b 11.560(3) _cell_length_c 13.183(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2176.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(1)K _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1078 _exptl_absorpt_coefficient_mu 0.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8864 _exptl_absorpt_correction_T_max 0.9805 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1)K _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEXII CCD' _diffrn_measurement_method ' \f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15278 _diffrn_reflns_av_R_equivalents 0.1190 _diffrn_reflns_av_sigmaI/netI 0.0865 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 23.42 _reflns_number_total 3289 _reflns_number_gt 2378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS V.5.0' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1580P)^2^+20.7790P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.4(3) _refine_ls_number_reflns 3289 _refine_ls_number_parameters 343 _refine_ls_number_restraints 172 _refine_ls_R_factor_all 0.1535 _refine_ls_R_factor_gt 0.1102 _refine_ls_wR_factor_ref 0.3116 _refine_ls_wR_factor_gt 0.2653 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 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 0.8907(2) -0.0772(3) 0.4072(2) 0.0359(10) Uani 1 1 d . . . O2 O 0.8871(2) 0.1538(3) -0.0078(2) 0.0306(9) Uani 1 1 d U . . O3 O 0.8201(2) 0.1741(3) 0.5076(3) 0.0320(8) Uani 1 1 d U . . O4 O 0.8185(2) 0.3868(3) 0.0845(3) 0.0380(10) Uani 1 1 d . . . O5 O 1.0000 0.3196(4) 0.5609(4) 0.0351(12) Uani 1 2 d SU . . O6 O 1.0000 0.5311(4) 0.1430(4) 0.0439(17) Uani 1 2 d S . . N1 N 0.9152(2) -0.1153(3) 0.2365(3) 0.0213(9) Uani 1 1 d U . . N2 N 0.9141(3) -0.0200(3) 0.0717(3) 0.0255(11) Uani 1 1 d . . . N3 N 0.7963(3) -0.0024(3) 0.2801(3) 0.0265(9) Uani 1 1 d U . . N4 N 0.7845(3) 0.0768(3) 0.1109(3) 0.0268(9) Uani 1 1 d U . . N5 N 0.7360(3) 0.1734(4) 0.3580(3) 0.0322(10) Uani 1 1 d U . . N6 N 0.7392(3) 0.2589(4) 0.1872(3) 0.0333(10) Uani 1 1 d U . . N7 N 0.7859(3) 0.3414(4) 0.4227(3) 0.0336(10) Uani 1 1 d U . . N8 N 0.7870(3) 0.4259(3) 0.2510(3) 0.0372(13) Uani 1 1 d . . . N9 N 0.9234(3) 0.4574(4) 0.4663(3) 0.0320(11) Uani 1 1 d U . . N10 N 0.9208(3) 0.5422(4) 0.2977(3) 0.0369(12) Uani 1 1 d U . . C1 C 1.0000 -0.1842(6) 0.2508(7) 0.042(2) Uani 1 2 d S . . H1B H 1.0000 -0.2172 0.3201 0.050 Uiso 1 2 calc SR . . H1A H 1.0000 -0.2492 0.2019 0.050 Uiso 1 2 calc SR . . C2 C 0.8686(3) -0.0937(4) 0.1442(3) 0.0264(12) Uani 1 1 d U . . H2 H 0.8487 -0.1679 0.1117 0.032 Uiso 1 1 calc R . . C3 C 1.0000 -0.0517(6) 0.0151(5) 0.0288(19) Uani 1 2 d S . . H3B H 1.0000 -0.0119 -0.0513 0.035 Uiso 1 2 calc SR . . H3A H 1.0000 -0.1361 0.0024 0.035 Uiso 1 2 calc SR . . C4 C 0.8715(3) -0.0673(4) 0.3186(3) 0.0266(12) Uani 1 1 d U . . C5 C 0.7802(3) -0.0198(4) 0.1763(4) 0.0235(10) Uani 1 1 d U . . H5 H 0.7211 -0.0644 0.1652 0.028 Uiso 1 1 calc R . . C6 C 0.8680(3) 0.0785(4) 0.0532(3) 0.0242(10) Uani 1 1 d U . . C7 C 0.7278(3) 0.0523(4) 0.3494(4) 0.0268(11) Uani 1 1 d U . . H7B H 0.6639 0.0337 0.3254 0.032 Uiso 1 1 calc R . . H7A H 0.7352 0.0178 0.4177 0.032 Uiso 1 1 calc R . . C8 C 0.7206(4) 0.1746(4) 0.1116(4) 0.0354(11) Uani 1 1 d U . . H8B H 0.7230 0.2126 0.0443 0.042 Uiso 1 1 calc R . . H8A H 0.6561 0.1452 0.1214 0.042 Uiso 1 1 calc R . . C9 C 0.7013(4) 0.2588(4) 0.2897(4) 0.0369(9) Uani 1 1 d U . . H9 H 0.6314 0.2546 0.2868 0.044 Uiso 1 1 calc R . . C10 C 0.7861(3) 0.2249(5) 0.4343(4) 0.0299(10) Uani 1 1 d U . . C11 C 0.7306(4) 0.3728(5) 0.3336(4) 0.0392(10) Uani 1 1 d U . . H11 H 0.6754 0.4217 0.3520 0.047 Uiso 1 1 calc R . . C12 C 0.7855(4) 0.3584(4) 0.1664(4) 0.0332(11) Uani 1 1 d U . . C13 C 0.8273(4) 0.4212(4) 0.4941(4) 0.0339(11) Uani 1 1 d U . . H13B H 0.8288 0.3845 0.5619 0.041 Uiso 1 1 calc R . . H13A H 0.7871 0.4908 0.4988 0.041 Uiso 1 1 calc R . . C14 C 0.8273(4) 0.5399(5) 0.2529(4) 0.0439(17) Uani 1 1 d . . . H14B H 0.7858 0.5919 0.2921 0.053 Uiso 1 1 calc R . . H14A H 0.8309 0.5699 0.1827 0.053 Uiso 1 1 calc R . . C15 C 1.0000 0.4006(6) 0.5048(6) 0.0278(15) Uani 1 2 d SU . . C16 C 0.9426(3) 0.5558(4) 0.4037(4) 0.0331(15) Uani 1 1 d U . . H16 H 0.9161 0.6288 0.4325 0.040 Uiso 1 1 calc R . . C17 C 1.0000 0.5372(5) 0.2358(6) 0.035(2) Uani 1 2 d S . . Cl1 Cl 1.0000 -0.06069(15) -0.26490(13) 0.0289(4) Uani 1 2 d SU A 1 Cl2 Cl 1.0000 0.53032(17) -0.21170(15) 0.0398(5) Uani 1 2 d SU B 2 O1W O 1.0000 0.3605(5) -0.0211(5) 0.0558(19) Uani 1 2 d S C 3 H1Y H 1.0000 0.2760 -0.0036 0.084 Uiso 1 2 d S D 3 H1W H 1.0000 0.4056 0.0394 0.084 Uiso 1 2 d S E 3 O2W O 1.0000 0.0758(5) 0.5278(4) 0.0526(19) Uani 1 2 d S F 4 H2Y H 1.0000 0.0274 0.4698 0.079 Uiso 1 2 d S G 4 H2W H 1.0000 0.0325 0.5918 0.079 Uiso 1 2 d S H 4 O3W O 1.0000 -0.3042(5) 0.5952(4) 0.0460(17) Uani 1 2 d S I 5 H3Y H 1.0000 -0.3593 0.6436 0.069 Uiso 1 2 d S J 5 H3W H 1.0000 -0.2237 0.6187 0.069 Uiso 1 2 d S K 5 O4W O 0.5000 0.7707(6) 0.2601(5) 0.074(2) Uani 1 2 d S L 6 H4Y H 0.5000 0.7391 0.3273 0.112 Uiso 1 2 d S M 6 H4W H 0.5000 0.7142 0.2011 0.112 Uiso 1 2 d S N 6 O5W O 0.6965(4) 0.7510(5) 0.3142(4) 0.0844(18) Uani 1 1 d . O 7 H5Y H 0.6543 0.7863 0.2705 0.127 Uiso 1 1 d . P 7 H5W H 0.6829 0.7760 0.3889 0.127 Uiso 1 1 d . Q 7 O6W O 0.9519(7) -0.3213(7) -0.0149(6) 0.064(3) Uani 0.50 1 d P . 8 H6W H 0.9566 -0.3661 0.0527 0.095 Uiso 0.50 1 d P R 8 H6Y H 1.0000 -0.3535 -0.0584 0.095 Uiso 1 2 d S S 8 O7W O 1.0137(7) 0.2150(8) 0.2868(9) 0.123(3) Uani 0.25 1 d PDU T -11 H7W H 1.0113 0.1508 0.3359 0.184 Uiso 0.25 1 d PD U -11 H7Y H 1.0749 0.2540 0.2932 0.184 Uiso 0.25 1 d PD V -11 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 0.0098(15) 0.066(2) 0.0317(17) 0.0073(17) 0.0028(15) -0.0161(16) O2 0.0043(13) 0.0503(18) 0.0372(17) 0.0050(15) -0.0040(14) 0.0011(13) O3 0.0101(13) 0.0568(16) 0.0292(14) 0.0054(13) 0.0038(12) -0.0045(12) O4 0.0197(17) 0.056(2) 0.0384(18) 0.0122(17) -0.0040(16) 0.0182(16) O5 0.0110(19) 0.047(2) 0.047(2) -0.0010(19) 0.000 0.000 O6 0.061(4) 0.033(3) 0.038(3) 0.007(2) 0.000 0.000 N1 0.0079(16) 0.0363(18) 0.0195(16) 0.0003(16) 0.0023(16) -0.0084(15) N2 0.0115(19) 0.042(2) 0.023(2) 0.0027(17) 0.0019(18) -0.0044(17) N3 0.0113(15) 0.0399(16) 0.0282(16) -0.0012(14) 0.0023(14) -0.0110(13) N4 0.0135(16) 0.0408(17) 0.0262(16) 0.0002(14) 0.0024(14) 0.0021(14) N5 0.0116(15) 0.0547(18) 0.0302(17) -0.0047(15) 0.0079(14) 0.0023(15) N6 0.0164(16) 0.0460(17) 0.0373(17) -0.0039(15) -0.0074(15) 0.0096(15) N7 0.0110(17) 0.064(2) 0.0264(17) -0.0047(17) -0.0033(15) 0.0033(17) N8 0.031(2) 0.043(2) 0.037(2) -0.0069(19) -0.010(2) 0.013(2) N9 0.0062(16) 0.050(2) 0.039(2) -0.0032(18) 0.0011(17) 0.0043(17) N10 0.048(3) 0.044(2) 0.019(2) 0.0000(19) -0.004(2) 0.014(2) C1 0.036(4) 0.020(3) 0.070(5) 0.020(3) 0.000 0.000 C2 0.012(2) 0.038(2) 0.030(2) -0.0036(19) -0.0011(19) -0.0088(19) C3 0.019(3) 0.042(4) 0.026(3) -0.002(3) 0.000 0.000 C4 0.012(2) 0.053(2) 0.015(2) 0.0067(19) -0.0017(18) -0.0172(19) C5 0.0058(17) 0.0373(18) 0.0274(18) -0.0059(16) 0.0005(15) -0.0086(15) C6 0.0132(18) 0.0336(18) 0.0257(17) -0.0003(15) -0.0032(15) -0.0053(15) C7 0.0107(17) 0.0437(19) 0.0259(18) 0.0014(15) 0.0041(15) -0.0041(15) C8 0.0213(19) 0.049(2) 0.036(2) -0.0017(17) -0.0042(16) 0.0020(17) C9 0.0203(15) 0.0521(15) 0.0384(15) 0.0015(14) 0.0048(14) 0.0093(13) C10 0.0160(17) 0.0481(18) 0.0254(17) 0.0003(15) 0.0052(15) 0.0001(15) C11 0.0195(16) 0.0589(18) 0.0393(17) 0.0048(16) 0.0046(16) 0.0169(16) C12 0.0264(19) 0.0437(19) 0.0296(19) 0.0017(16) -0.0071(16) 0.0176(16) C13 0.0242(19) 0.0432(19) 0.0344(19) -0.0008(16) 0.0053(16) 0.0079(16) C14 0.046(3) 0.053(3) 0.032(3) -0.003(2) -0.012(3) 0.029(3) C15 0.013(3) 0.039(3) 0.032(3) 0.008(3) 0.000 0.000 C16 0.018(3) 0.038(3) 0.043(3) 0.001(2) 0.002(2) 0.008(2) C17 0.055(5) 0.012(3) 0.038(4) -0.002(3) 0.000 0.000 Cl1 0.0032(6) 0.0539(8) 0.0295(7) 0.0066(7) 0.000 0.000 Cl2 0.0077(7) 0.0654(10) 0.0462(9) 0.0100(9) 0.000 0.000 O1W 0.043(3) 0.057(3) 0.068(4) -0.003(3) 0.000 0.000 O2W 0.034(3) 0.083(4) 0.041(3) 0.006(3) 0.000 0.000 O3W 0.035(3) 0.066(3) 0.038(3) -0.005(3) 0.000 0.000 O4W 0.092(5) 0.078(4) 0.054(4) -0.010(3) 0.000 0.000 O5W 0.042(3) 0.109(4) 0.102(4) -0.029(3) 0.024(3) 0.016(3) O6W 0.084(6) 0.050(4) 0.056(5) 0.002(4) -0.019(5) 0.011(4) O7W 0.120(5) 0.121(5) 0.127(5) -0.002(4) 0.002(5) 0.000(4) _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 C4 1.204(5) . ? O2 C6 1.216(5) . ? O3 C10 1.232(6) . ? O4 C12 1.223(6) . ? O5 C15 1.194(8) . ? O6 C17 1.225(9) . ? N1 C4 1.368(6) . ? N1 C2 1.410(6) . ? N1 C1 1.461(5) . ? N2 C6 1.337(6) . ? N2 C2 1.436(6) . ? N2 C3 1.482(5) . ? N3 C5 1.402(6) . ? N3 C4 1.405(6) . ? N3 C7 1.481(6) . ? N4 C5 1.412(6) . ? N4 C6 1.415(6) . ? N4 C8 1.454(7) . ? N5 C10 1.370(6) . ? N5 C7 1.409(6) . ? N5 C9 1.425(7) . ? N6 C12 1.356(7) . ? N6 C8 1.419(7) . ? N6 C9 1.455(7) . ? N7 C10 1.355(7) . ? N7 C13 1.444(7) . ? N7 C11 1.461(7) . ? N8 C12 1.361(7) . ? N8 C14 1.439(7) . ? N8 C11 1.487(7) . ? N9 C15 1.373(6) . ? N9 C16 1.433(7) . ? N9 C13 1.480(6) . ? N10 C17 1.396(6) . ? N10 C16 1.440(7) . ? N10 C14 1.459(7) . ? C1 N1 1.461(5) 4_755 ? C2 C5 1.581(7) . ? C3 N2 1.482(5) 4_755 ? C9 C11 1.498(8) . ? C15 N9 1.373(6) 4_755 ? C16 C16 1.638(10) 4_755 ? C17 N10 1.396(6) 4_755 ? O6W O6W 1.374(19) 4_755 ? 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 C4 N1 C2 113.3(4) . . ? C4 N1 C1 119.8(5) . . ? C2 N1 C1 126.8(5) . . ? C6 N2 C2 113.8(4) . . ? C6 N2 C3 121.8(4) . . ? C2 N2 C3 124.2(4) . . ? C5 N3 C4 113.7(4) . . ? C5 N3 C7 123.8(4) . . ? C4 N3 C7 120.7(4) . . ? C5 N4 C6 112.1(4) . . ? C5 N4 C8 125.7(4) . . ? C6 N4 C8 121.5(4) . . ? C10 N5 C7 122.3(4) . . ? C10 N5 C9 110.1(4) . . ? C7 N5 C9 127.5(4) . . ? C12 N6 C8 122.1(4) . . ? C12 N6 C9 111.7(4) . . ? C8 N6 C9 125.6(4) . . ? C10 N7 C13 124.1(4) . . ? C10 N7 C11 109.8(4) . . ? C13 N7 C11 125.9(4) . . ? C12 N8 C14 123.0(4) . . ? C12 N8 C11 110.8(4) . . ? C14 N8 C11 125.6(4) . . ? C15 N9 C16 116.0(4) . . ? C15 N9 C13 120.9(4) . . ? C16 N9 C13 123.0(4) . . ? C17 N10 C16 113.3(5) . . ? C17 N10 C14 120.2(4) . . ? C16 N10 C14 126.3(4) . . ? N1 C1 N1 111.9(5) 4_755 . ? N1 C2 N2 117.7(4) . . ? N1 C2 C5 104.0(4) . . ? N2 C2 C5 102.6(4) . . ? N2 C3 N2 111.8(5) . 4_755 ? O1 C4 N1 128.7(4) . . ? O1 C4 N3 125.1(4) . . ? N1 C4 N3 106.2(4) . . ? N3 C5 N4 118.4(4) . . ? N3 C5 C2 102.0(4) . . ? N4 C5 C2 103.2(4) . . ? O2 C6 N2 128.3(4) . . ? O2 C6 N4 123.7(4) . . ? N2 C6 N4 107.7(4) . . ? N5 C7 N3 114.8(4) . . ? N6 C8 N4 114.9(4) . . ? N5 C9 N6 117.3(4) . . ? N5 C9 C11 105.6(4) . . ? N6 C9 C11 104.8(4) . . ? O3 C10 N7 124.3(5) . . ? O3 C10 N5 125.1(5) . . ? N7 C10 N5 110.4(4) . . ? N7 C11 N8 113.5(4) . . ? N7 C11 C9 104.1(4) . . ? N8 C11 C9 103.4(4) . . ? O4 C12 N6 126.4(5) . . ? O4 C12 N8 124.4(5) . . ? N6 C12 N8 109.1(4) . . ? N7 C13 N9 113.5(4) . . ? N8 C14 N10 112.9(4) . . ? O5 C15 N9 127.1(3) . 4_755 ? O5 C15 N9 127.1(3) . . ? N9 C15 N9 105.7(6) 4_755 . ? N9 C16 N10 115.5(4) . . ? N9 C16 C16 101.1(2) . 4_755 ? N10 C16 C16 102.5(3) . 4_755 ? O6 C17 N10 125.9(3) . . ? O6 C17 N10 125.9(3) . 4_755 ? N10 C17 N10 108.2(6) . 4_755 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.42 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.386 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.185 # Attachment 'david2revised.cif' data_david2 _database_code_depnum_ccdc_archive 'CCDC 687156' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common cucurbit(5)uril _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48.75 Cl2.75 N20 O18' _chemical_formula_weight 1075.13 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' Cl Cl 0.1484 0.1585 '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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 37.248(3) _cell_length_b 14.1905(11) _cell_length_c 37.892(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.999(4) _cell_angle_gamma 90.00 _cell_volume 20016(2) _cell_formula_units_Z 16 _cell_measurement_temperature 100.0(1)K _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8952 _exptl_absorpt_coefficient_mu 0.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8715 _exptl_absorpt_correction_T_max 0.9797 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1)K _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEXII CCD' _diffrn_measurement_method ' \f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 149575 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 24.71 _reflns_number_total 17755 _reflns_number_gt 12658 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS V.5.0' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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.OH distances and HOH angles in water molecules were fixed. Some of the hydrogen atoms of water molecules could not be found, but included in the formula. ; _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^)+(0.2000P)^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 17755 _refine_ls_number_parameters 1549 _refine_ls_number_restraints 143 _refine_ls_R_factor_all 0.1618 _refine_ls_R_factor_gt 0.1273 _refine_ls_wR_factor_ref 0.4173 _refine_ls_wR_factor_gt 0.3796 _refine_ls_goodness_of_fit_ref 1.742 _refine_ls_restrained_S_all 1.767 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.06095(10) 0.5000 0.45855(10) 0.0285(10) Uani 1 2 d S . . O2 O 0.08358(8) 0.3183(2) 0.41398(8) 0.0340(8) Uani 1 1 d . . . O3 O 0.12037(8) 0.3922(2) 0.33953(8) 0.0342(8) Uani 1 1 d . . . O4 O -0.08303(13) 0.5000 0.37684(13) 0.0563(16) Uani 1 2 d S . . O5 O -0.06397(9) 0.3132(3) 0.33481(9) 0.0517(10) Uani 1 1 d . . . O6 O -0.02708(9) 0.3876(2) 0.26606(9) 0.0410(8) Uani 1 1 d . . . N1 N 0.00612(9) 0.4222(3) 0.45523(10) 0.0337(9) Uani 1 1 d . . . N2 N -0.05017(10) 0.4218(3) 0.42127(10) 0.0426(11) Uani 1 1 d . . . N3 N 0.02287(10) 0.2889(3) 0.41944(10) 0.0334(9) Uani 1 1 d . . . N4 N 0.04962(10) 0.2386(3) 0.37174(10) 0.0354(10) Uani 1 1 d . . . N5 N -0.03546(11) 0.2813(4) 0.38916(10) 0.0474(12) Uani 1 1 d . . . N6 N -0.00886(11) 0.2372(3) 0.34029(10) 0.0409(10) Uani 1 1 d . . . N7 N 0.07557(10) 0.2947(3) 0.31763(9) 0.0325(9) Uani 1 1 d . . . N8 N 0.09247(10) 0.4144(3) 0.28505(9) 0.0314(9) Uani 1 1 d . . . N9 N 0.01751(10) 0.2867(3) 0.28558(10) 0.0349(9) Uani 1 1 d . . . N10 N 0.03242(9) 0.4139(3) 0.25641(9) 0.0320(9) Uani 1 1 d . . . C1 C 0.02782(16) 0.5000 0.45646(15) 0.0297(15) Uani 1 2 d S . . C2 C 0.02034(13) 0.3269(3) 0.45470(11) 0.0335(11) Uani 1 1 d . . . H2A H 0.0445 0.3266 0.4664 0.040 Uiso 1 1 calc R . . H2B H 0.0047 0.2854 0.4685 0.040 Uiso 1 1 calc R . . C3 C -0.00411(13) 0.2311(4) 0.40201(12) 0.0401(12) Uani 1 1 d . . . H3 H -0.0107 0.1761 0.4170 0.048 Uiso 1 1 calc R . . C4 C -0.06025(13) 0.3267(4) 0.40956(12) 0.0519(15) Uani 1 1 d D . . H4A H -0.0644 0.2877 0.4307 0.062 Uiso 1 1 calc R . . H4B H -0.0833 0.3307 0.3958 0.062 Uiso 1 1 calc R . . C5 C -0.03129(11) 0.4462(4) 0.45394(12) 0.0384(12) Uani 1 1 d . . . H5 H -0.0438 0.4205 0.4748 0.046 Uiso 1 1 calc R . . C6 C -0.06317(17) 0.5000 0.40341(18) 0.0435(19) Uani 1 2 d S . . C7 C 0.05489(12) 0.2866(3) 0.40273(11) 0.0285(10) Uani 1 1 d . . . C8 C 0.01378(14) 0.1989(3) 0.36786(12) 0.0398(12) Uani 1 1 d . . . H8 H 0.0147 0.1286 0.3664 0.048 Uiso 1 1 calc R . . C9 C -0.03843(14) 0.2825(4) 0.35242(13) 0.0456(14) Uani 1 1 d . . . C10 C 0.07776(13) 0.2274(3) 0.34646(12) 0.0345(11) Uani 1 1 d . . . H10A H 0.1014 0.2343 0.3590 0.041 Uiso 1 1 calc R . . H10B H 0.0764 0.1629 0.3366 0.041 Uiso 1 1 calc R . . C11 C -0.00513(14) 0.2192(4) 0.30282(12) 0.0421(13) Uani 1 1 d . . . H11A H 0.0050 0.1554 0.2998 0.051 Uiso 1 1 calc R . . H11B H -0.0293 0.2200 0.2910 0.051 Uiso 1 1 calc R . . C12 C 0.09851(11) 0.3704(3) 0.31658(12) 0.0287(10) Uani 1 1 d . . . C13 C 0.05664(12) 0.2793(3) 0.28429(12) 0.0339(11) Uani 1 1 d . . . H13 H 0.0642 0.2191 0.2729 0.041 Uiso 1 1 calc R . . C14 C 0.06678(12) 0.3659(3) 0.26227(11) 0.0314(11) Uani 1 1 d . . . H14 H 0.0775 0.3471 0.2395 0.038 Uiso 1 1 calc R . . C15 C 0.00461(12) 0.3669(3) 0.26940(11) 0.0319(11) Uani 1 1 d . . . C16 C 0.11105(17) 0.5000 0.27512(18) 0.0337(16) Uani 1 2 d S . . H16A H 0.1354 0.5000 0.2865 0.040 Uiso 1 2 calc SR . . H16B H 0.1139 0.5000 0.2492 0.040 Uiso 1 2 calc SR . . C17 C 0.02768(17) 0.5000 0.23589(17) 0.0337(16) Uani 1 2 d S . . H17A H 0.0451 0.5000 0.2167 0.040 Uiso 1 2 calc SR . . H17B H 0.0033 0.5000 0.2247 0.040 Uiso 1 2 calc SR . . O1A O 0.34027(12) 0.0000 0.43957(11) 0.0338(11) Uani 1 2 d S . . O2A O 0.29478(8) 0.1807(2) 0.45941(9) 0.0387(8) Uani 1 1 d . . . O3A O 0.21877(8) 0.1087(2) 0.49068(8) 0.0358(8) Uani 1 1 d . . . O4A O 0.27107(12) 0.0000 0.29082(12) 0.0458(13) Uani 1 2 d S . . O5A O 0.22536(8) 0.1848(3) 0.30999(9) 0.0422(9) Uani 1 1 d . . . O6A O 0.15261(8) 0.1111(2) 0.34191(8) 0.0359(8) Uani 1 1 d . . . N1A N 0.33990(10) 0.0778(3) 0.38604(9) 0.0315(9) Uani 1 1 d . . . N2A N 0.31233(10) 0.0776(3) 0.32656(10) 0.0373(10) Uani 1 1 d . . . N3A N 0.30571(10) 0.2151(3) 0.40107(10) 0.0338(9) Uani 1 1 d . . . N4A N 0.25399(10) 0.2614(3) 0.42319(10) 0.0341(9) Uani 1 1 d . . . N5A N 0.27800(10) 0.2154(3) 0.34128(10) 0.0406(11) Uani 1 1 d . . . N6A N 0.22661(10) 0.2636(3) 0.36301(10) 0.0360(10) Uani 1 1 d . . . N7A N 0.19821(10) 0.2084(3) 0.44597(10) 0.0342(9) Uani 1 1 d . . . N8A N 0.16490(10) 0.0858(3) 0.46013(10) 0.0347(10) Uani 1 1 d . . . N9A N 0.17045(10) 0.2120(3) 0.38682(10) 0.0360(10) Uani 1 1 d . . . N10A N 0.13874(10) 0.0858(3) 0.39956(10) 0.0339(9) Uani 1 1 d . . . C1A C 0.34001(16) 0.0000 0.40728(16) 0.0296(15) Uani 1 2 d S . . C2A C 0.34067(12) 0.1726(3) 0.40016(13) 0.0354(11) Uani 1 1 d . . . H2A1 H 0.3514 0.1711 0.4244 0.043 Uiso 1 1 calc R . . H2A2 H 0.3562 0.2122 0.3856 0.043 Uiso 1 1 calc R . . C3A C 0.28952(13) 0.2692(3) 0.37212(13) 0.0380(12) Uani 1 1 d . . . H3A H 0.3050 0.3236 0.3656 0.046 Uiso 1 1 calc R . . C4A C 0.30195(12) 0.1735(3) 0.31701(12) 0.0370(12) Uani 1 1 d . . . H4A1 H 0.3238 0.2129 0.3160 0.044 Uiso 1 1 calc R . . H4A2 H 0.2902 0.1730 0.2932 0.044 Uiso 1 1 calc R . . C5A C 0.34348(12) 0.0550(3) 0.34928(12) 0.0361(11) Uani 1 1 d . . . H5A H 0.3661 0.0811 0.3398 0.043 Uiso 1 1 calc R . . C6A C 0.29618(18) 0.0000 0.31272(17) 0.0396(18) Uani 1 2 d S . . C7A C 0.28556(12) 0.2155(3) 0.43005(12) 0.0299(11) Uani 1 1 d . . . C8A C 0.25325(12) 0.3032(3) 0.38805(13) 0.0354(11) Uani 1 1 d . . . H8A H 0.2517 0.3735 0.3890 0.043 Uiso 1 1 calc R . . C9A C 0.24182(12) 0.2176(3) 0.33593(12) 0.0367(12) Uani 1 1 d . . . C10A C 0.22711(12) 0.2755(3) 0.44839(13) 0.0359(12) Uani 1 1 d . . . H10C H 0.2170 0.3396 0.4453 0.043 Uiso 1 1 calc R . . H10D H 0.2385 0.2720 0.4724 0.043 Uiso 1 1 calc R . . C11A C 0.16601(12) 0.2212(3) 0.42439(12) 0.0326(11) Uani 1 1 d . . . H11C H 0.1535 0.2812 0.4303 0.039 Uiso 1 1 calc R . . C12A C 0.18891(12) 0.2792(3) 0.36518(13) 0.0349(11) Uani 1 1 d . . . H12A H 0.1779 0.2775 0.3410 0.042 Uiso 1 1 calc R . . H12B H 0.1851 0.3432 0.3748 0.042 Uiso 1 1 calc R . . C13A C 0.19650(11) 0.1306(3) 0.46791(12) 0.0283(10) Uani 1 1 d . . . C14A C 0.14292(12) 0.1335(3) 0.43348(12) 0.0333(11) Uani 1 1 d . . . H14A H 0.1192 0.1524 0.4428 0.040 Uiso 1 1 calc R . . C15A C 0.15442(12) 0.1324(3) 0.37321(12) 0.0319(11) Uani 1 1 d . . . C16A C 0.15478(18) 0.0000 0.47794(17) 0.0360(16) Uani 1 2 d S . . H16C H 0.1284 0.0000 0.4805 0.043 Uiso 1 2 calc SR . . H16D H 0.1661 0.0000 0.5020 0.043 Uiso 1 2 calc SR . . C17A C 0.11799(18) 0.0000 0.39412(17) 0.0349(16) Uani 1 2 d S . . H17C H 0.0979 0.0000 0.4105 0.042 Uiso 1 2 calc SR . . H17D H 0.1076 0.0000 0.3697 0.042 Uiso 1 2 calc SR . . O1B O 0.37676(9) 0.1089(3) 0.08283(10) 0.0507(10) Uani 1 1 d . . . O2B O 0.34951(8) 0.1806(2) 0.16261(9) 0.0412(9) Uani 1 1 d . . . O3B O 0.33293(12) 0.0000 0.20916(12) 0.0408(12) Uani 1 2 d S . . O4B O 0.21824(11) 0.1284(3) 0.02703(10) 0.0636(12) Uani 1 1 d . . . O5B O 0.19460(9) 0.1916(3) 0.10237(10) 0.0547(10) Uani 1 1 d . . . O6B O 0.18428(15) 0.0000 0.14413(15) 0.0650(17) Uani 1 2 d S . . N1B N 0.34006(12) 0.0853(3) 0.03255(12) 0.0525(13) Uani 1 1 d . . . N2B N 0.32794(11) 0.2026(3) 0.06881(11) 0.0429(11) Uani 1 1 d . . . N3B N 0.27650(12) 0.0866(3) 0.01481(11) 0.0523(13) Uani 1 1 d . . . N4B N 0.26755(11) 0.2207(3) 0.04271(11) 0.0464(12) Uani 1 1 d . . . N5B N 0.31142(11) 0.2647(3) 0.12552(11) 0.0390(10) Uani 1 1 d . . . N6B N 0.29186(10) 0.2154(3) 0.17661(10) 0.0352(10) Uani 1 1 d . . . N7B N 0.25000(11) 0.2661(3) 0.10069(11) 0.0430(11) Uani 1 1 d . . . N8B N 0.23015(11) 0.2169(3) 0.15246(11) 0.0477(12) Uani 1 1 d . . . N9B N 0.27903(10) 0.0772(3) 0.21189(10) 0.0376(10) Uani 1 1 d . . . N10B N 0.21802(11) 0.0781(3) 0.18678(11) 0.0454(11) Uani 1 1 d . . . C1B C 0.3568(2) 0.0000 0.0199(2) 0.059(2) Uani 1 2 d S . . H1B1 H 0.3825 0.0000 0.0275 0.071 Uiso 1 2 calc SR . . H1B2 H 0.3555 0.0000 -0.0062 0.071 Uiso 1 2 calc SR . . C2B C 0.35076(13) 0.1304(4) 0.06362(13) 0.0433(13) Uani 1 1 d . . . C3B C 0.31014(16) 0.1324(4) 0.01465(14) 0.0537(15) Uani 1 1 d . . . H3B H 0.3163 0.1505 -0.0099 0.064 Uiso 1 1 calc R . . C4B C 0.30531(15) 0.2205(4) 0.03776(13) 0.0498(15) Uani 1 1 d . . . H4B1 H 0.3130 0.2788 0.0253 0.060 Uiso 1 1 calc R . . C5B C 0.25082(16) 0.1418(4) 0.02815(13) 0.0471(14) Uani 1 1 d . . . C6B C 0.2684(3) 0.0000 -0.0053(2) 0.065(3) Uani 1 2 d S . . H6B1 H 0.2826 0.0000 -0.0270 0.077 Uiso 1 2 calc SR . . H6B2 H 0.2427 0.0000 -0.0127 0.077 Uiso 1 2 calc SR . . C7B C 0.33499(15) 0.2725(4) 0.09674(14) 0.0469(14) Uani 1 1 d . . . H7B1 H 0.3601 0.2652 0.1058 0.056 Uiso 1 1 calc R . . H7B2 H 0.3326 0.3364 0.0864 0.056 Uiso 1 1 calc R . . C8B C 0.24874(15) 0.2881(4) 0.06370(14) 0.0500(14) Uani 1 1 d . . . H8B1 H 0.2594 0.3513 0.0603 0.060 Uiso 1 1 calc R . . H8B2 H 0.2233 0.2909 0.0552 0.060 Uiso 1 1 calc R . . C9B C 0.31992(12) 0.2154(3) 0.15508(13) 0.0357(12) Uani 1 1 d . . . C10B C 0.27605(14) 0.3059(4) 0.12667(13) 0.0421(13) Uani 1 1 d . . . H10E H 0.2769 0.3762 0.1254 0.051 Uiso 1 1 calc R . . C11B C 0.26189(14) 0.2714(4) 0.16191(14) 0.0473(14) Uani 1 1 d . . . H11D H 0.2561 0.3253 0.1777 0.057 Uiso 1 1 calc R . . C12B C 0.22228(14) 0.2208(4) 0.11717(14) 0.0457(14) Uani 1 1 d . . . C13B C 0.29311(14) 0.1732(4) 0.21141(12) 0.0412(12) Uani 1 1 d . . . H13A H 0.2791 0.2128 0.2274 0.049 Uiso 1 1 calc R . . H13B H 0.3183 0.1726 0.2206 0.049 Uiso 1 1 calc R . . C14B C 0.20705(13) 0.1730(4) 0.17666(14) 0.0447(13) Uani 1 1 d . . . H14B H 0.1825 0.1705 0.1659 0.054 Uiso 1 1 calc R . . H14C H 0.2062 0.2124 0.1982 0.054 Uiso 1 1 calc R . . C15B C 0.30006(18) 0.0000 0.21104(16) 0.0359(16) Uani 1 2 d S . . C16B C 0.24142(13) 0.0535(4) 0.21624(12) 0.0422(13) Uani 1 1 d . . . H16E H 0.2324 0.0792 0.2389 0.051 Uiso 1 1 calc R . . C17B C 0.20498(18) 0.0000 0.17041(19) 0.047(2) Uani 1 2 d S . . O1C O 0.47317(9) 0.3930(2) 0.23327(8) 0.0367(8) Uani 1 1 d . . . O2C O 0.55382(9) 0.3170(2) 0.20772(8) 0.0392(8) Uani 1 1 d . . . O3C O 0.60011(12) 0.5000 0.19186(12) 0.0447(13) Uani 1 2 d S . . O4C O 0.41776(9) 0.3858(3) 0.07917(8) 0.0422(9) Uani 1 1 d . . . O5C O 0.49467(10) 0.3183(3) 0.05540(9) 0.0501(10) Uani 1 1 d . . . O6C O 0.54352(14) 0.5000 0.03769(12) 0.0509(14) Uani 1 2 d S . . N1C N 0.42173(10) 0.4146(3) 0.19851(10) 0.0338(9) Uani 1 1 d . . . N2C N 0.45826(10) 0.2964(3) 0.18587(10) 0.0336(9) Uani 1 1 d . . . N3C N 0.40106(10) 0.4152(3) 0.13623(10) 0.0381(10) Uani 1 1 d . . . N4C N 0.43299(11) 0.2875(3) 0.12544(10) 0.0383(10) Uani 1 1 d . . . N5C N 0.51570(10) 0.2386(3) 0.16859(10) 0.0376(10) Uani 1 1 d . . . N6C N 0.56909(10) 0.2810(3) 0.15096(11) 0.0396(10) Uani 1 1 d . . . N7C N 0.49176(12) 0.2375(3) 0.10768(11) 0.0448(11) Uani 1 1 d . . . N8C N 0.54477(11) 0.2879(3) 0.09077(11) 0.0454(11) Uani 1 1 d . . . N9C N 0.60312(11) 0.4216(3) 0.13825(10) 0.0415(11) Uani 1 1 d . . . N10C N 0.58184(11) 0.4225(3) 0.07683(11) 0.0462(11) Uani 1 1 d . . . C1C C 0.40989(17) 0.5000 0.21547(17) 0.0325(15) Uani 1 2 d S . . H1C1 H 0.4190 0.5000 0.2403 0.039 Uiso 1 2 calc SR . . H1C2 H 0.3833 0.5000 0.2156 0.039 Uiso 1 2 calc SR . . C2C C 0.45382(11) 0.3714(3) 0.20791(11) 0.0310(11) Uani 1 1 d D . . C3C C 0.40278(12) 0.3672(3) 0.16996(12) 0.0319(11) Uani 1 1 d . . . H3C H 0.3783 0.3475 0.1771 0.038 Uiso 1 1 calc R . . C4C C 0.42655(12) 0.2803(3) 0.16285(12) 0.0335(11) Uani 1 1 d . . . H4C H 0.4141 0.2201 0.1687 0.040 Uiso 1 1 calc R . . C5C C 0.41769(12) 0.3652(3) 0.11058(12) 0.0342(11) Uani 1 1 d . . . C6C C 0.38121(17) 0.5000 0.12845(18) 0.0371(17) Uani 1 2 d S . . H6C1 H 0.3591 0.5000 0.1422 0.045 Uiso 1 2 calc SR . . H6C2 H 0.3738 0.5000 0.1031 0.045 Uiso 1 2 calc SR . . C7C C 0.48596(12) 0.2284(3) 0.19211(13) 0.0343(11) Uani 1 1 d . . . H7C1 H 0.4756 0.1645 0.1892 0.041 Uiso 1 1 calc R . . H7C2 H 0.4952 0.2344 0.2168 0.041 Uiso 1 1 calc R . . C8C C 0.45333(13) 0.2196(4) 0.10608(13) 0.0418(13) Uani 1 1 d . . . H8C1 H 0.4447 0.2202 0.0811 0.050 Uiso 1 1 calc R . . H8C2 H 0.4488 0.1560 0.1157 0.050 Uiso 1 1 calc R . . C9C C 0.54705(13) 0.2823(3) 0.17828(12) 0.0344(11) Uani 1 1 d . . . C10C C 0.51683(14) 0.1974(4) 0.13384(13) 0.0415(13) Uani 1 1 d . . . H10F H 0.5152 0.1271 0.1347 0.050 Uiso 1 1 calc R . . C11C C 0.55409(14) 0.2313(4) 0.12055(13) 0.0420(13) Uani 1 1 d . . . H11E H 0.5695 0.1768 0.1140 0.050 Uiso 1 1 calc R . . C12C C 0.50868(14) 0.2850(4) 0.08192(13) 0.0440(13) Uani 1 1 d . . . C13C C 0.60395(12) 0.3269(4) 0.15273(14) 0.0434(13) Uani 1 1 d . . . H13C H 0.6127 0.3298 0.1777 0.052 Uiso 1 1 calc R . . H13D H 0.6212 0.2885 0.1396 0.052 Uiso 1 1 calc R . . C14C C 0.57058(13) 0.3272(4) 0.06687(13) 0.0445(13) Uani 1 1 d . . . H14D H 0.5597 0.3285 0.0427 0.053 Uiso 1 1 calc R . . H14E H 0.5920 0.2859 0.0667 0.053 Uiso 1 1 calc R . . C15C C 0.60230(16) 0.5000 0.15943(18) 0.0391(18) Uani 1 2 d S . . C16C C 0.61038(13) 0.4454(4) 0.10195(12) 0.0432(13) Uani 1 1 d . . . H16F H 0.6340 0.4194 0.0947 0.052 Uiso 1 1 calc R . . C17C C 0.56642(19) 0.5000 0.06107(18) 0.0437(19) Uani 1 2 d S . . Cl1A Cl 0.20066(5) 0.5000 0.41678(5) 0.0290(5) Uani 0.83 2 d SP A 1 Cl1B Cl 0.1931(3) 0.5000 0.4296(3) 0.0290(5) Uani 0.17 2 d SP B 2 Cl2A Cl 0.30976(7) 0.5000 0.06268(7) 0.0478(6) Uani 0.82 2 d SP C 3 Cl2B Cl 0.2959(4) 0.5000 0.0711(3) 0.0478(6) Uani 0.18 2 d SP D 4 Cl3A Cl 0.45818(6) 0.0000 0.16198(7) 0.0730(7) Uani 1 2 d S E 5 Cl4A Cl 0.04459(8) 0.0000 0.31870(7) 0.0333(7) Uani 0.60 2 d SP F 6 Cl4B Cl 0.06117(13) 0.0000 0.31211(12) 0.0333(7) Uani 0.40 2 d SP G 7 Cl5A Cl 0.2393(2) 0.0000 0.0921(2) 0.0815(15) Uani 0.34 2 d SP H 8 Cl5B Cl 0.2733(3) 0.0000 0.1063(3) 0.0815(15) Uani 0.28 2 d SP I 9 Cl5C Cl 0.2810(3) 0.0000 0.1350(3) 0.0815(15) Uani 0.26 2 d SP J 10 Cl5D Cl 0.3065(6) 0.0000 0.1200(6) 0.0815(15) Uani 0.12 2 d SP K 11 Cl6A Cl 0.4901(3) 0.5000 0.1087(2) 0.120(2) Uani 0.36 2 d SP L 12 Cl6B Cl 0.5044(4) 0.5000 0.1347(3) 0.120(2) Uani 0.28 2 d SP M 13 Cl6C Cl 0.5122(2) 0.5000 0.1620(2) 0.120(2) Uani 0.36 2 d SPD N 14 Cl7A Cl 0.2550(2) 0.0000 0.4225(2) 0.123(2) Uani 0.48 2 d SP O 15 Cl7B Cl 0.2402(3) 0.0000 0.3921(3) 0.123(2) Uani 0.34 2 d SP P 16 Cl7C Cl 0.2279(6) 0.0000 0.3678(6) 0.123(2) Uani 0.18 2 d SP Q 17 Cl8A Cl 0.12141(16) 0.3632(5) 0.49460(16) 0.0628(10) Uani 0.25 1 d P R 18 Cl8B Cl -0.10664(19) 0.3450(7) 0.48074(18) 0.0628(10) Uani 0.20 1 d PD S 19 Cl8C Cl 0.34543(18) 0.1509(6) 0.50891(19) 0.0628(10) Uani 0.22 1 d P T 20 Cl8D Cl 0.3540(3) 0.0953(9) 0.5237(3) 0.0628(10) Uani 0.14 1 d P U 21 Cl8E Cl 0.3888(2) 0.1112(7) 0.4753(2) 0.0628(10) Uani 0.19 1 d P V 22 Cl9A Cl -0.12725(18) 0.6395(5) 0.27353(18) 0.1006(14) Uani 0.33 1 d PU W 23 Cl9B Cl 0.4076(3) 0.2014(7) 0.2436(3) 0.1006(14) Uani 0.19 1 d PDU X 24 Cl9C Cl -0.1130(3) 0.6887(8) 0.2568(3) 0.1006(14) Uani 0.22 1 d PU Y 25 Cl9D Cl 0.3839(3) 0.2636(11) 0.2444(4) 0.1006(14) Uani 0.14 1 d PDU Z 26 Cl9E Cl -0.0973(5) 0.5520(14) 0.2281(5) 0.1006(14) Uani 0.12 1 d PU . 27 O1W O 0.30628(12) 0.5000 0.18978(14) 0.0256(12) Uani 0.78 2 d SP A 28 H1W H 0.3130 0.5567 0.1776 0.038 Uiso 0.39 1 d P B 28 H1Y H 0.3130 0.4434 0.1776 0.038 Uiso 0.39 1 d P C 28 O52W O 0.3192(6) 0.4313(18) 0.2119(7) 0.0256(12) Uani 0.11 1 d P D 29 H52W H 0.3159 0.4279 0.1823 0.038 Uiso 0.11 1 d P E 29 H52Y H 0.3104 0.4986 0.2150 0.038 Uiso 0.22 2 d SP F 29 O2W O 0.08651(12) 0.5000 0.16364(12) 0.0479(13) Uani 1 2 d S G 30 H2W H 0.1118 0.5000 0.1767 0.072 Uiso 1 2 d S H 30 H2Y H 0.0920 0.5000 0.1387 0.072 Uiso 1 2 d S I 30 O3W O 0.53840(15) 0.5000 0.23459(14) 0.0541(15) Uani 1 2 d S J 31 H3W H 0.5118 0.5000 0.2320 0.081 Uiso 1 2 d S K 31 H3Y H 0.5459 0.5000 0.2593 0.081 Uiso 1 2 d S L 31 O4W O 0.11522(13) 0.5000 0.40393(14) 0.0466(13) Uani 1 2 d S M 32 H4W H 0.0995 0.5237 0.4226 0.070 Uiso 0.50 1 d P N 32 H4Y H 0.1374 0.4767 0.4162 0.070 Uiso 0.50 1 d P O 32 O5W O 0.28403(15) 0.0000 0.49536(15) 0.0569(15) Uani 1 2 d S P 33 H5W H 0.2804 0.0000 0.4692 0.085 Uiso 1 2 d S Q 33 H5Y H 0.2603 0.0000 0.5058 0.085 Uiso 1 2 d S R 33 O6W O -0.04433(16) 0.0000 0.40400(18) 0.0667(18) Uani 1 2 d S S 34 H6W H -0.0271 0.0000 0.3853 0.100 Uiso 1 2 d S T 34 H6Y H -0.0689 0.0000 0.3952 0.100 Uiso 1 2 d S U 34 O7W O 0.19543(17) 0.0000 0.29973(16) 0.0693(18) Uani 1 2 d S V 35 H7W H 0.1872 0.0000 0.2752 0.104 Uiso 1 2 d S W 35 H7Y H 0.2219 0.0000 0.3015 0.104 Uiso 1 2 d S X 35 O8W O 0.46442(16) 0.5000 0.03682(14) 0.0639(17) Uani 1 2 d S Y 36 H8W H 0.4891 0.5000 0.0467 0.096 Uiso 1 2 d S Z 36 H8Y H 0.4475 0.5000 0.0561 0.096 Uiso 1 2 d S A 36 O9W O 0.37596(16) 0.0000 0.14586(17) 0.0689(18) Uani 1 2 d S B 37 H9W H 0.3502 0.0000 0.1507 0.103 Uiso 1 2 d S C 37 H9Y H 0.3897 0.0000 0.1686 0.103 Uiso 1 2 d S D 37 O10W O -0.07486(17) 0.5000 0.30349(17) 0.082(2) Uani 1 2 d S E 38 H10W H -0.1005 0.5000 0.3064 0.122 Uiso 1 2 d S F 38 H10Y H -0.0684 0.5000 0.2789 0.122 Uiso 1 2 d S G 38 O11W O 0.2828(3) 0.5000 0.3345(2) 0.076(3) Uani 0.78 2 d SP H 39 H11W H 0.3027 0.5000 0.3170 0.114 Uiso 0.78 2 d SP I 39 H11Y H 0.2934 0.5000 0.3579 0.114 Uiso 0.78 2 d SP J 39 O12W O 0.322(3) 0.5000 0.355(3) 0.076(3) Uani 0.06 2 d SP K 40 H12W H 0.3330 0.5000 0.3244 0.114 Uiso 0.06 2 d SP L 40 H12Y H 0.3450 0.5000 0.3654 0.114 Uiso 0.06 2 d SP M 40 O13W O 0.3135(14) 0.5000 0.3339(12) 0.076(3) Uani 0.16 2 d SP N 41 H13W H 0.3080 0.5000 0.3089 0.114 Uiso 0.16 2 d SP O 41 H13Y H 0.2874 0.5000 0.3452 0.114 Uiso 0.16 2 d SP P 41 O14W O 0.1713(6) 0.5000 0.0732(5) 0.097(5) Uani 0.38 2 d SPU Q 42 H14W H 0.1458 0.5000 0.0803 0.146 Uiso 0.38 2 d SP R 42 H14Y H 0.1869 0.5000 0.0943 0.146 Uiso 0.38 2 d SP S 42 O15W O 0.5563(8) 0.0000 0.0903(6) 0.097(5) Uani 0.30 2 d SPU T 43 H15Y H 0.5542 0.0000 0.0647 0.146 Uiso 0.30 2 d SP U 43 O54W O 0.5352(9) -0.0982(13) 0.0496(7) 0.097(5) Uani 0.16 1 d PD V 44 H54Y H 0.5430 -0.0359 0.0584 0.146 Uiso 0.16 1 d PD W 44 O16W O 0.02702(16) 0.0000 0.43168(17) 0.050(2) Uani 0.73 2 d SP X 45 H16W H 0.0466 0.0000 0.4494 0.076 Uiso 0.73 2 d SP Y 45 H16Y H 0.0039 0.0000 0.4432 0.076 Uiso 0.73 2 d SP Z 45 O17W O 0.0391(6) 0.066(2) 0.4408(6) 0.050(2) Uani 0.14 1 d P A 46 H17W H 0.0164 0.0558 0.4536 0.076 Uiso 0.14 1 d P B 46 H17Y H 0.0564 0.0955 0.4580 0.076 Uiso 0.14 1 d P C 46 O18W O 0.3210(2) 0.4215(5) 0.4277(2) 0.0320(18) Uani 0.35 1 d P D 47 H18W H 0.2995 0.4292 0.4421 0.048 Uiso 0.35 1 d P E 47 H18Y H 0.3405 0.3969 0.4429 0.048 Uiso 0.35 1 d P F 47 O19W O 0.1945(4) 0.0000 0.5711(4) 0.0320(18) Uani 0.30 2 d SP G 48 H19W H 0.2186 0.0000 0.5620 0.048 Uiso 0.30 2 d SP H 48 H19Y H 0.1953 0.0000 0.5969 0.048 Uiso 0.30 2 d SP I 48 O20W O 0.0567(3) 0.1519(7) 0.5048(3) 0.046(2) Uani 0.31 1 d P J 49 H20W H 0.0352 0.1157 0.5034 0.069 Uiso 0.64 1 d P K 49 H20Y H 0.0608 0.1793 0.5283 0.069 Uiso 0.64 1 d P L 49 O21W O 0.0582(6) 0.1173(13) 0.4705(5) 0.046(2) Uani 0.17 1 d P M 50 H21W H 0.0440 0.1780 0.4739 0.069 Uiso 0.36 1 d P N 50 H21Y H 0.0772 0.1146 0.4881 0.069 Uiso 0.36 1 d P O 50 O22W O 0.0479(3) 0.1932(7) 0.5207(3) 0.046(2) Uani 0.33 1 d P P 51 O23W O 0.0384(6) 0.1484(13) 0.5185(5) 0.046(2) Uani 0.19 1 d P Q 52 O24W O 0.0204(3) 0.5000 0.3548(3) 0.046(2) Uani 0.34 2 d SP R 53 H24W H -0.0053 0.5000 0.3589 0.069 Uiso 0.34 2 d SP S 53 H24Y H 0.0337 0.5000 0.3780 0.069 Uiso 0.34 2 d SP T 53 O25W O 0.0433(3) 0.5000 0.3741(3) 0.046(2) Uani 0.34 2 d SP U 54 H25W H 0.0676 0.5000 0.3672 0.069 Uiso 0.34 2 d SP V 54 H25Y H 0.0396 0.5000 0.3989 0.069 Uiso 0.34 2 d SP W 54 O26W O -0.0040(4) 0.5000 0.3362(4) 0.046(2) Uani 0.32 2 d SP X 55 H26W H -0.0028 0.5000 0.3109 0.069 Uiso 0.32 2 d SP Y 55 H26Y H -0.0287 0.5000 0.3437 0.069 Uiso 0.32 2 d SP Z 55 O27W O 0.3855(2) 0.2877(5) 0.0133(2) 0.068(2) Uani 0.50 1 d PU A 56 H27W H 0.4097 0.2965 0.0178 0.101 Uiso 0.50 1 d P B 56 H27Y H 0.3714 0.3456 0.0102 0.101 Uiso 0.50 1 d P C 56 O28W O 0.1632(2) 0.1245(7) 0.2423(2) 0.071(3) Uani 0.50 1 d P D 57 H28W H 0.1717 0.1890 0.2499 0.106 Uiso 0.50 1 d P E 57 H28Y H 0.1384 0.1190 0.2512 0.106 Uiso 0.50 1 d P F 57 O29W O 0.3705(3) 0.3296(11) 0.3351(4) 0.114(5) Uani 0.43 1 d P G 58 H29W H 0.3506 0.3676 0.3255 0.150 Uiso 0.50 1 d P H 58 H29Y H 0.3930 0.3653 0.3331 0.150 Uiso 0.50 1 d P I 58 O53W O -0.107(2) 0.144(7) 0.378(2) 0.114(5) Uani 0.07 1 d P J 59 O30W O 0.3517(2) 0.2101(7) -0.0577(3) 0.075(3) Uani 0.50 1 d PU K 60 H30W H 0.3369 0.2669 -0.0561 0.113 Uiso 0.50 1 d P L 60 H30Y H 0.3690 0.2104 -0.0370 0.113 Uiso 0.50 1 d P M 60 O31W O 0.2285(4) 0.3272(11) 0.2432(4) 0.142(5) Uani 0.50 1 d PU N 61 H31W H 0.2233 0.2603 0.2519 0.150 Uiso 0.50 1 d P O 61 H31Y H 0.2190 0.3691 0.2618 0.150 Uiso 0.50 1 d P P 61 O32W O 0.1346(3) 0.0376(8) -0.0103(3) 0.116(4) Uani 0.50 1 d PU . 62 H32W H 0.1267 0.0428 0.0144 0.150 Uiso 0.50 1 d P Q 62 H32Y H 0.1202 -0.0156 -0.0214 0.150 Uiso 0.50 1 d P R 62 O33W O -0.0444(5) 0.0000 0.3100(5) 0.095(6) Uani 0.50 2 d SP S 63 H33W H -0.0368 0.0000 0.2847 0.143 Uiso 1 2 d S T 63 H33Y H -0.0714 0.0000 0.3086 0.143 Uiso 1 2 d S U 63 O34W O 0.1676(3) 0.0000 0.0452(3) 0.048(3) Uani 0.50 2 d SP V 64 O35W O 0.2157(4) 0.5000 0.1372(4) 0.087(3) Uani 0.56 2 d SPU W 65 H35W H 0.2225 0.5000 0.1125 0.130 Uiso 0.56 2 d SP X 65 H35Y H 0.1894 0.5000 0.1382 0.130 Uiso 0.56 2 d SP Y 65 O47W O 0.2218(8) 0.5000 0.1586(8) 0.087(3) Uani 0.28 2 d SPU Z 66 H47W H 0.2135 0.5000 0.1827 0.130 Uiso 0.28 2 d SP A 66 H47Y H 0.2490 0.5000 0.1601 0.130 Uiso 0.28 2 d SP B 66 O51W O 0.2039(17) 0.426(5) 0.1384(18) 0.087(3) Uani 0.08 1 d P C 67 H51W H 0.2168 0.3656 0.1330 0.130 Uiso 0.08 1 d P D 67 H51Y H 0.2040 0.4657 0.1180 0.130 Uiso 0.08 1 d P E 67 O36W O 0.1992(5) 0.5000 0.3275(3) 0.089(5) Uani 0.50 2 d SP F 68 H36W H 0.2240 0.5000 0.3358 0.133 Uiso 0.50 2 d SP G 68 H36Y H 0.1829 0.5000 0.3466 0.133 Uiso 0.50 2 d SP H 68 O37W O 0.4470(4) 0.0000 0.0617(4) 0.088(5) Uani 0.50 2 d SP I 69 H37W H 0.4724 0.0000 0.0674 0.132 Uiso 0.50 2 d SP J 69 H37Y H 0.4432 0.0000 0.0355 0.132 Uiso 0.50 2 d SP K 69 O38W O 0.3892(4) 0.3730(11) 0.4262(5) 0.059(5) Uani 0.25 1 d PU L 70 H38W H 0.3703 0.3265 0.4321 0.088 Uiso 0.25 1 d P M 70 H38Y H 0.3871 0.3805 0.3995 0.088 Uiso 0.25 1 d P N 70 O39W O 0.1380(6) 0.3488(17) 0.0778(7) 0.099(6) Uani 0.25 1 d PU O 71 H39W H 0.1568 0.3954 0.0854 0.148 Uiso 0.25 1 d P P 71 H39Y H 0.1353 0.3044 0.0983 0.148 Uiso 0.25 1 d P Q 71 O40W O 0.1494(4) 0.3594(10) 0.1864(5) 0.059(4) Uani 0.25 1 d PU R 72 H40W H 0.1675 0.3744 0.2013 0.089 Uiso 0.25 1 d P S 72 H40Y H 0.1541 0.3676 0.1606 0.089 Uiso 0.25 1 d P T 72 O41W O 0.3165(4) 0.3683(10) 0.2553(5) 0.059(4) Uani 0.25 1 d PU U 73 H41W H 0.3426 0.3627 0.2623 0.089 Uiso 0.25 1 d P V 73 H41Y H 0.3026 0.3740 0.2760 0.089 Uiso 0.25 1 d P W 73 O42W O 0.3494(4) 0.2898(11) -0.0393(4) 0.051(4) Uani 0.25 1 d PU X 74 H42W H 0.3557 0.2309 -0.0487 0.077 Uiso 0.25 1 d P Y 74 H42Y H 0.3620 0.3006 -0.0157 0.077 Uiso 0.25 1 d P Z 74 O43W O 0.4524 0.1992(18) 0.0118(7) 0.105(6) Uani 0.25 1 d PU A 75 H43W H 0.4519 0.2411 0.0202 0.158 Uiso 0.25 1 d P B 75 H43Y H 0.4403 0.1346 0.0120 0.158 Uiso 0.25 1 d P C 75 O44W O 0.1464(4) 0.1788(11) 0.2580(4) 0.052(4) Uani 0.25 1 d PU D 76 H44W H 0.1707 0.2201 0.2599 0.078 Uiso 0.25 1 d P E 76 H44Y H 0.1346 0.2034 0.2803 0.078 Uiso 0.25 1 d P F 76 O45W O -0.0388(4) 0.0000 0.3341(6) 0.125(8) Uani 0.50 2 d SP G 77 H45W H -0.0562 0.0000 0.3135 0.150 Uiso 0.50 2 d SP H 77 H45Y H -0.0143 0.0000 0.3243 0.150 Uiso 0.50 2 d SP I 77 O46W O 0.1895(6) 0.0000 0.0749(7) 0.155(9) Uani 0.50 2 d SP J 78 H46W H 0.1668 0.0000 0.0609 0.150 Uiso 0.50 2 d SP K 78 H46Y H 0.1827 0.0000 0.1005 0.150 Uiso 0.50 2 d SP L 78 O48W O 0.3877(5) 0.3795(14) 0.4039(6) 0.071(5) Uani 0.25 1 d PU M 79 H48Y H 0.4001 0.3384 0.3872 0.107 Uiso 0.25 1 d P N 79 O49W O 0.1380 0.2670 0.2500 0.088(6) Uani 0.25 1 d PU O 80 H49W H 0.1531 0.2346 0.2684 0.132 Uiso 0.25 1 d P P 80 H49Y H 0.1418 0.2375 0.2273 0.132 Uiso 0.25 1 d P Q 80 O50W O 0.4371(5) 0.1543(13) 0.0107(5) 0.067(4) Uani 0.25 1 d PU R 81 H50W H 0.4450 0.2262 0.0131 0.100 Uiso 0.25 1 d P S 81 H50Y H 0.4584 0.1191 0.0117 0.100 Uiso 0.25 1 d P T 81 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 0.026(2) 0.037(2) 0.022(2) 0.000 -0.0043(16) 0.000 O2 0.0384(17) 0.0311(16) 0.0318(16) -0.0081(13) -0.0083(13) 0.0050(14) O3 0.0310(16) 0.0317(16) 0.0390(18) -0.0055(14) -0.0112(14) 0.0054(13) O4 0.031(2) 0.104(4) 0.033(3) 0.000 -0.007(2) 0.000 O5 0.0322(17) 0.088(3) 0.0339(19) -0.0045(18) -0.0124(15) -0.0177(18) O6 0.0354(17) 0.050(2) 0.0366(18) -0.0048(15) -0.0043(14) -0.0025(15) N1 0.0261(18) 0.038(2) 0.037(2) -0.0041(17) -0.0007(16) -0.0046(16) N2 0.033(2) 0.068(3) 0.026(2) 0.0100(19) -0.0096(16) -0.016(2) N3 0.036(2) 0.034(2) 0.0296(19) -0.0009(16) -0.0098(16) -0.0051(16) N4 0.041(2) 0.034(2) 0.031(2) -0.0031(17) -0.0020(17) -0.0061(17) N5 0.032(2) 0.082(3) 0.027(2) -0.004(2) -0.0028(17) -0.011(2) N6 0.041(2) 0.054(2) 0.028(2) -0.0059(18) -0.0028(17) -0.013(2) N7 0.038(2) 0.031(2) 0.0281(19) -0.0028(16) -0.0101(16) -0.0025(16) N8 0.0304(19) 0.035(2) 0.0289(19) -0.0008(16) -0.0060(16) -0.0001(16) N9 0.036(2) 0.037(2) 0.031(2) 0.0009(17) -0.0045(17) -0.0093(17) N10 0.0290(19) 0.038(2) 0.0283(19) 0.0018(16) -0.0059(16) -0.0007(16) C1 0.032(3) 0.035(3) 0.021(3) 0.000 -0.007(2) 0.000 C2 0.041(2) 0.034(2) 0.026(2) 0.0005(19) -0.0036(19) -0.005(2) C3 0.047(3) 0.046(3) 0.027(2) 0.003(2) -0.006(2) -0.020(2) C4 0.036(3) 0.086(4) 0.033(3) -0.005(3) -0.004(2) -0.028(3) C5 0.025(2) 0.066(3) 0.024(2) -0.004(2) 0.0020(18) -0.006(2) C6 0.019(3) 0.083(5) 0.029(4) 0.000 0.004(3) 0.000 C7 0.038(2) 0.022(2) 0.025(2) 0.0014(17) -0.0071(19) -0.0019(18) C8 0.058(3) 0.031(2) 0.029(2) 0.001(2) -0.008(2) -0.018(2) C9 0.045(3) 0.056(3) 0.036(3) 0.004(2) -0.008(2) -0.024(2) C10 0.043(3) 0.029(2) 0.031(2) -0.0033(19) -0.005(2) 0.006(2) C11 0.051(3) 0.042(3) 0.032(3) -0.007(2) -0.009(2) -0.015(2) C12 0.027(2) 0.026(2) 0.033(2) -0.0015(18) -0.0027(19) 0.0085(18) C13 0.040(2) 0.031(2) 0.031(2) -0.0074(19) -0.002(2) -0.002(2) C14 0.036(2) 0.035(2) 0.023(2) -0.0028(18) -0.0059(18) -0.0010(19) C15 0.032(2) 0.039(3) 0.025(2) -0.0063(19) -0.0026(18) -0.002(2) C16 0.028(3) 0.032(3) 0.040(4) 0.000 0.006(3) 0.000 C17 0.034(3) 0.036(4) 0.031(3) 0.000 -0.005(3) 0.000 O1A 0.039(2) 0.031(2) 0.030(2) 0.000 -0.0061(19) 0.000 O2A 0.0363(17) 0.0345(17) 0.0448(19) 0.0072(15) -0.0064(15) 0.0074(14) O3A 0.0365(17) 0.0320(16) 0.0382(18) 0.0010(14) -0.0085(14) 0.0058(14) O4A 0.037(3) 0.067(3) 0.033(3) 0.000 -0.005(2) 0.000 O5A 0.0352(17) 0.055(2) 0.0359(18) 0.0086(16) -0.0083(14) 0.0019(16) O6A 0.0329(16) 0.0398(17) 0.0344(17) -0.0033(14) -0.0061(14) 0.0047(14) N1A 0.0324(19) 0.033(2) 0.0284(19) 0.0013(16) -0.0031(16) 0.0033(16) N2A 0.0275(19) 0.050(2) 0.034(2) 0.0113(18) -0.0069(16) -0.0033(17) N3A 0.035(2) 0.030(2) 0.035(2) 0.0038(16) -0.0104(17) 0.0073(16) N4A 0.037(2) 0.030(2) 0.035(2) 0.0059(16) -0.0065(17) 0.0077(16) N5A 0.032(2) 0.056(3) 0.033(2) 0.0043(19) -0.0071(17) -0.0041(19) N6A 0.0293(19) 0.040(2) 0.038(2) -0.0015(18) -0.0124(17) 0.0037(17) N7A 0.0309(19) 0.033(2) 0.038(2) 0.0006(17) -0.0091(16) 0.0091(16) N8A 0.035(2) 0.035(2) 0.034(2) 0.0001(17) -0.0038(17) -0.0009(17) N9A 0.037(2) 0.037(2) 0.033(2) 0.0015(17) -0.0060(17) 0.0042(17) N10A 0.033(2) 0.039(2) 0.029(2) 0.0009(17) -0.0042(16) -0.0017(17) C1A 0.028(3) 0.033(3) 0.027(3) 0.000 -0.004(3) 0.000 C2A 0.029(2) 0.036(3) 0.040(3) 0.001(2) -0.008(2) -0.006(2) C3A 0.040(3) 0.033(2) 0.040(3) 0.007(2) -0.010(2) -0.001(2) C4A 0.029(2) 0.051(3) 0.030(2) 0.018(2) 0.0005(19) -0.003(2) C5A 0.032(2) 0.042(3) 0.034(2) 0.006(2) 0.0017(19) -0.004(2) C6A 0.031(3) 0.063(5) 0.024(3) 0.000 -0.002(3) 0.000 C7A 0.034(2) 0.018(2) 0.038(3) 0.0014(18) -0.010(2) 0.0009(17) C8A 0.030(2) 0.030(2) 0.045(3) 0.007(2) -0.016(2) -0.0025(19) C9A 0.029(2) 0.044(3) 0.036(3) 0.017(2) -0.010(2) -0.004(2) C10A 0.035(2) 0.027(2) 0.045(3) -0.003(2) -0.008(2) 0.0032(19) C11A 0.031(2) 0.032(2) 0.033(2) -0.0063(19) -0.0098(19) 0.0060(19) C12A 0.036(2) 0.032(2) 0.036(2) 0.001(2) -0.009(2) 0.001(2) C13A 0.024(2) 0.026(2) 0.035(2) -0.0036(19) 0.0003(18) 0.0055(17) C14A 0.031(2) 0.038(3) 0.030(2) -0.001(2) -0.0077(19) 0.005(2) C15A 0.027(2) 0.032(2) 0.036(3) 0.001(2) -0.0054(19) 0.0048(18) C16A 0.034(3) 0.044(4) 0.031(3) 0.000 0.013(3) 0.000 C17A 0.035(3) 0.039(4) 0.030(3) 0.000 -0.010(3) 0.000 O1B 0.0357(18) 0.054(2) 0.063(2) 0.0067(19) 0.0057(17) -0.0074(17) O2B 0.0330(17) 0.0432(19) 0.047(2) 0.0062(16) -0.0127(15) -0.0072(15) O3B 0.033(2) 0.057(3) 0.031(2) 0.000 -0.0077(19) 0.000 O4B 0.057(2) 0.084(3) 0.048(2) 0.015(2) -0.0298(18) -0.021(2) O5B 0.0380(19) 0.079(3) 0.046(2) 0.0127(19) -0.0185(16) -0.0057(18) O6B 0.054(3) 0.093(4) 0.047(3) 0.000 -0.022(3) 0.000 N1B 0.052(3) 0.067(3) 0.038(2) 0.012(2) 0.005(2) -0.005(2) N2B 0.042(2) 0.046(2) 0.040(2) 0.0131(19) -0.0057(19) -0.004(2) N3B 0.053(3) 0.066(3) 0.036(2) 0.005(2) -0.020(2) -0.009(2) N4B 0.045(2) 0.060(3) 0.034(2) 0.014(2) -0.0048(19) -0.009(2) N5B 0.042(2) 0.037(2) 0.038(2) 0.0060(18) -0.0079(18) -0.0026(18) N6B 0.035(2) 0.036(2) 0.033(2) 0.0011(17) -0.0139(17) 0.0030(17) N7B 0.040(2) 0.050(2) 0.038(2) 0.0083(19) -0.0123(18) 0.0026(19) N8B 0.032(2) 0.070(3) 0.040(2) 0.000(2) -0.0038(19) 0.008(2) N9B 0.031(2) 0.049(2) 0.032(2) 0.0098(18) -0.0040(16) 0.0031(18) N10B 0.034(2) 0.063(3) 0.039(2) -0.009(2) -0.0013(18) 0.007(2) C1B 0.061(5) 0.070(6) 0.048(5) 0.000 0.022(4) 0.000 C2B 0.034(3) 0.056(3) 0.040(3) 0.019(2) -0.003(2) -0.013(2) C3B 0.066(4) 0.065(4) 0.030(3) 0.018(3) -0.008(2) 0.006(3) C4B 0.055(3) 0.061(3) 0.034(3) 0.019(2) -0.005(2) -0.008(3) C5B 0.062(3) 0.047(3) 0.030(3) 0.018(2) -0.010(2) -0.006(3) C6B 0.090(6) 0.061(5) 0.040(4) 0.000 -0.034(4) 0.000 C7B 0.050(3) 0.044(3) 0.047(3) 0.010(2) -0.006(2) -0.008(2) C8B 0.052(3) 0.050(3) 0.047(3) 0.017(3) -0.014(3) 0.002(3) C9B 0.033(2) 0.029(2) 0.044(3) -0.002(2) -0.010(2) -0.0037(19) C10B 0.046(3) 0.035(3) 0.044(3) 0.000(2) -0.009(2) 0.005(2) C11B 0.053(3) 0.047(3) 0.041(3) -0.004(2) -0.010(2) 0.008(2) C12B 0.042(3) 0.053(3) 0.040(3) 0.006(2) -0.015(2) 0.008(2) C13B 0.052(3) 0.044(3) 0.026(2) -0.004(2) -0.010(2) 0.003(2) C14B 0.034(2) 0.061(3) 0.039(3) -0.002(2) 0.001(2) 0.013(2) C15B 0.037(4) 0.047(4) 0.024(3) 0.000 0.000(3) 0.000 C16B 0.037(2) 0.064(3) 0.026(2) 0.002(2) 0.000(2) 0.007(2) C17B 0.025(3) 0.080(6) 0.035(4) 0.000 0.005(3) 0.000 O1C 0.0473(18) 0.0348(17) 0.0275(16) 0.0029(14) -0.0046(14) -0.0064(15) O2C 0.0436(18) 0.0383(18) 0.0349(18) 0.0065(15) -0.0106(14) -0.0021(15) O3C 0.037(3) 0.071(3) 0.026(2) 0.000 -0.003(2) 0.000 O4C 0.0414(18) 0.056(2) 0.0288(17) -0.0037(15) -0.0059(14) -0.0054(16) O5C 0.048(2) 0.070(2) 0.0315(18) -0.0076(17) -0.0070(16) 0.0090(18) O6C 0.058(3) 0.073(4) 0.021(2) 0.000 -0.004(2) 0.000 N1C 0.038(2) 0.029(2) 0.033(2) -0.0003(16) -0.0072(17) 0.0015(16) N2C 0.0303(19) 0.039(2) 0.031(2) -0.0038(17) -0.0066(16) -0.0008(17) N3C 0.033(2) 0.049(2) 0.032(2) -0.0025(18) -0.0041(17) 0.0015(18) N4C 0.042(2) 0.039(2) 0.034(2) -0.0080(18) -0.0028(18) -0.0010(18) N5C 0.039(2) 0.036(2) 0.038(2) -0.0039(18) -0.0028(18) -0.0015(18) N6C 0.034(2) 0.047(2) 0.038(2) -0.0015(19) -0.0018(17) -0.0072(18) N7C 0.046(2) 0.052(3) 0.036(2) -0.003(2) -0.0047(19) 0.001(2) N8C 0.037(2) 0.069(3) 0.031(2) -0.004(2) 0.0017(18) 0.010(2) N9C 0.036(2) 0.056(3) 0.032(2) -0.0033(19) 0.0028(17) -0.0087(19) N10C 0.038(2) 0.065(3) 0.035(2) -0.006(2) -0.0062(18) 0.006(2) C1C 0.029(3) 0.033(3) 0.036(4) 0.000 0.004(3) 0.000 C2C 0.040(2) 0.029(2) 0.024(2) 0.0060(18) -0.0020(19) -0.0061(19) C3C 0.034(2) 0.030(2) 0.032(2) 0.0025(19) 0.0003(19) -0.0050(19) C4C 0.035(2) 0.033(2) 0.032(2) -0.005(2) -0.0009(19) -0.008(2) C5C 0.028(2) 0.042(3) 0.032(3) -0.006(2) -0.0015(19) -0.010(2) C6C 0.031(3) 0.046(4) 0.034(4) 0.000 -0.007(3) 0.000 C7C 0.040(2) 0.026(2) 0.037(3) 0.0102(19) 0.000(2) -0.0028(19) C8C 0.041(3) 0.044(3) 0.039(3) -0.008(2) -0.008(2) 0.000(2) C9C 0.038(2) 0.035(3) 0.030(2) 0.001(2) -0.006(2) 0.010(2) C10C 0.048(3) 0.032(3) 0.044(3) -0.009(2) -0.005(2) 0.007(2) C11C 0.045(3) 0.042(3) 0.039(3) -0.009(2) 0.000(2) 0.008(2) C12C 0.042(3) 0.058(3) 0.032(3) -0.015(2) 0.000(2) 0.006(2) C13C 0.025(2) 0.065(3) 0.040(3) 0.000(2) -0.005(2) 0.005(2) C14C 0.040(3) 0.060(3) 0.034(3) -0.013(2) 0.008(2) 0.006(2) C15C 0.020(3) 0.057(4) 0.040(4) 0.000 -0.006(3) 0.000 C16C 0.031(2) 0.067(3) 0.031(3) -0.004(2) 0.004(2) 0.005(2) C17C 0.042(4) 0.065(5) 0.025(3) 0.000 0.005(3) 0.000 Cl1A 0.0272(9) 0.0210(8) 0.0382(12) 0.000 -0.0083(8) 0.000 Cl1B 0.0272(9) 0.0210(8) 0.0382(12) 0.000 -0.0083(8) 0.000 Cl2A 0.0600(15) 0.0298(9) 0.0515(13) 0.000 -0.0269(11) 0.000 Cl2B 0.0600(15) 0.0298(9) 0.0515(13) 0.000 -0.0269(11) 0.000 Cl3A 0.0632(11) 0.0242(9) 0.1271(19) 0.000 -0.0587(12) 0.000 Cl4A 0.049(2) 0.0213(9) 0.0283(11) 0.000 -0.0107(13) 0.000 Cl4B 0.049(2) 0.0213(9) 0.0283(11) 0.000 -0.0107(13) 0.000 Cl5A 0.073(3) 0.103(4) 0.068(3) 0.000 -0.005(2) 0.000 Cl5B 0.073(3) 0.103(4) 0.068(3) 0.000 -0.005(2) 0.000 Cl5C 0.073(3) 0.103(4) 0.068(3) 0.000 -0.005(2) 0.000 Cl5D 0.073(3) 0.103(4) 0.068(3) 0.000 -0.005(2) 0.000 Cl6A 0.113(4) 0.188(6) 0.059(3) 0.000 -0.019(3) 0.000 Cl6B 0.113(4) 0.188(6) 0.059(3) 0.000 -0.019(3) 0.000 Cl6C 0.113(4) 0.188(6) 0.059(3) 0.000 -0.019(3) 0.000 Cl7A 0.111(4) 0.147(5) 0.108(4) 0.000 -0.026(3) 0.000 Cl7B 0.111(4) 0.147(5) 0.108(4) 0.000 -0.026(3) 0.000 Cl7C 0.111(4) 0.147(5) 0.108(4) 0.000 -0.026(3) 0.000 Cl8A 0.0493(16) 0.084(3) 0.0550(18) -0.0152(16) -0.0018(13) 0.0043(16) Cl8B 0.0493(16) 0.084(3) 0.0550(18) -0.0152(16) -0.0018(13) 0.0043(16) Cl8C 0.0493(16) 0.084(3) 0.0550(18) -0.0152(16) -0.0018(13) 0.0043(16) Cl8D 0.0493(16) 0.084(3) 0.0550(18) -0.0152(16) -0.0018(13) 0.0043(16) Cl8E 0.0493(16) 0.084(3) 0.0550(18) -0.0152(16) -0.0018(13) 0.0043(16) Cl9A 0.081(2) 0.128(3) 0.093(3) 0.033(2) 0.002(2) -0.005(2) Cl9B 0.081(2) 0.128(3) 0.093(3) 0.033(2) 0.002(2) -0.005(2) Cl9C 0.081(2) 0.128(3) 0.093(3) 0.033(2) 0.002(2) -0.005(2) Cl9D 0.081(2) 0.128(3) 0.093(3) 0.033(2) 0.002(2) -0.005(2) Cl9E 0.081(2) 0.128(3) 0.093(3) 0.033(2) 0.002(2) -0.005(2) O1W 0.006(2) 0.029(3) 0.043(3) 0.000 0.007(2) 0.000 O52W 0.006(2) 0.029(3) 0.043(3) 0.000 0.007(2) 0.000 O2W 0.040(2) 0.065(3) 0.042(3) 0.000 0.035(2) 0.000 O3W 0.059(3) 0.059(3) 0.044(3) 0.000 -0.002(3) 0.000 O4W 0.039(3) 0.044(3) 0.056(3) 0.000 -0.005(2) 0.000 O5W 0.052(3) 0.055(3) 0.063(4) 0.000 -0.005(3) 0.000 O6W 0.067(4) 0.033(3) 0.101(5) 0.000 0.018(3) 0.000 O7W 0.068(4) 0.083(4) 0.058(4) 0.000 0.015(3) 0.000 O8W 0.062(3) 0.091(4) 0.038(3) 0.000 -0.007(3) 0.000 O9W 0.060(3) 0.070(4) 0.077(4) 0.000 0.014(3) 0.000 O10W 0.064(4) 0.117(6) 0.064(4) 0.000 0.020(3) 0.000 O11W 0.131(7) 0.024(3) 0.071(5) 0.000 -0.037(5) 0.000 O12W 0.131(7) 0.024(3) 0.071(5) 0.000 -0.037(5) 0.000 O13W 0.131(7) 0.024(3) 0.071(5) 0.000 -0.037(5) 0.000 O14W 0.159(12) 0.083(9) 0.053(7) 0.000 0.047(8) 0.000 O15W 0.159(12) 0.083(9) 0.053(7) 0.000 0.047(8) 0.000 O54W 0.159(12) 0.083(9) 0.053(7) 0.000 0.047(8) 0.000 O16W 0.024(3) 0.098(6) 0.029(3) 0.000 -0.006(3) 0.000 O17W 0.024(3) 0.098(6) 0.029(3) 0.000 -0.006(3) 0.000 O18W 0.045(4) 0.019(3) 0.030(4) -0.006(4) -0.018(3) -0.013(4) O19W 0.045(4) 0.019(3) 0.030(4) -0.006(4) -0.018(3) -0.013(4) O20W 0.074(5) 0.035(4) 0.029(4) -0.006(3) 0.003(3) 0.041(4) O21W 0.074(5) 0.035(4) 0.029(4) -0.006(3) 0.003(3) 0.041(4) O22W 0.074(5) 0.035(4) 0.029(4) -0.006(3) 0.003(3) 0.041(4) O23W 0.074(5) 0.035(4) 0.029(4) -0.006(3) 0.003(3) 0.041(4) O24W 0.020(4) 0.086(6) 0.030(4) 0.000 -0.013(3) 0.000 O25W 0.020(4) 0.086(6) 0.030(4) 0.000 -0.013(3) 0.000 O26W 0.020(4) 0.086(6) 0.030(4) 0.000 -0.013(3) 0.000 O27W 0.092(5) 0.044(4) 0.071(4) -0.002(3) 0.061(4) -0.008(4) O28W 0.052(4) 0.108(7) 0.053(5) 0.021(5) 0.018(4) 0.037(5) O29W 0.102(8) 0.134(11) 0.111(9) -0.010(8) 0.064(7) -0.053(8) O53W 0.102(8) 0.134(11) 0.111(9) -0.010(8) 0.064(7) -0.053(8) O30W 0.050(4) 0.095(6) 0.080(5) 0.028(5) -0.014(4) -0.010(4) O31W 0.147(8) 0.139(8) 0.140(8) -0.031(6) 0.038(6) -0.012(7) O32W 0.142(7) 0.116(8) 0.090(6) -0.014(5) 0.019(5) -0.015(6) O33W 0.102(12) 0.062(9) 0.122(14) 0.000 -0.010(10) 0.000 O34W 0.037(5) 0.072(7) 0.035(5) 0.000 0.008(4) 0.000 O35W 0.084(5) 0.078(5) 0.098(6) 0.000 -0.001(5) 0.000 O47W 0.084(5) 0.078(5) 0.098(6) 0.000 -0.001(5) 0.000 O51W 0.084(5) 0.078(5) 0.098(6) 0.000 -0.001(5) 0.000 O36W 0.172(14) 0.035(6) 0.061(8) 0.000 0.021(9) 0.000 O37W 0.082(9) 0.077(9) 0.106(11) 0.000 0.027(8) 0.000 O38W 0.047(8) 0.047(9) 0.081(12) 0.015(9) -0.018(8) -0.004(7) O39W 0.089(9) 0.102(9) 0.104(9) -0.016(7) -0.007(7) -0.006(7) O40W 0.068(7) 0.035(6) 0.075(7) -0.014(6) -0.003(6) 0.012(6) O41W 0.062(7) 0.034(6) 0.079(7) 0.011(6) -0.019(6) -0.006(5) O42W 0.029(5) 0.075(7) 0.049(6) 0.029(6) 0.009(5) -0.009(5) O43W 0.117(9) 0.105(9) 0.094(9) 0.016(7) -0.007(7) -0.023(7) O44W 0.049(6) 0.062(7) 0.047(6) 0.014(5) 0.019(5) 0.031(6) O45W 0.043(8) 0.20(2) 0.133(17) 0.000 0.006(10) 0.000 O46W 0.140(15) 0.096(13) 0.24(2) 0.000 0.106(16) 0.000 O48W 0.067(8) 0.066(8) 0.081(8) 0.005(7) 0.001(7) -0.011(6) O49W 0.059(9) 0.128(14) 0.077(12) -0.008(10) -0.008(8) 0.080(9) O50W 0.054(7) 0.081(8) 0.065(7) 0.006(7) -0.001(6) 0.002(6) _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 C1 1.234(7) . ? O2 C7 1.222(5) . ? O3 C12 1.211(5) . ? O4 C6 1.228(8) . ? O5 C9 1.223(6) . ? O6 C15 1.219(5) . ? N1 C1 1.368(5) . ? N1 C5 1.433(6) . ? N1 C2 1.453(6) . ? N2 C6 1.379(6) . ? N2 C5 1.444(6) . ? N2 C4 1.464(7) . ? N3 C7 1.370(6) . ? N3 C3 1.440(6) . ? N3 C2 1.446(6) . ? N4 C7 1.365(6) . ? N4 C8 1.451(6) . ? N4 C10 1.453(6) . ? N5 C4 1.384(7) . ? N5 C9 1.393(6) . ? N5 C3 1.438(7) . ? N6 C9 1.369(7) . ? N6 C8 1.427(6) . ? N6 C11 1.454(6) . ? N7 C12 1.373(6) . ? N7 C13 1.442(6) . ? N7 C10 1.451(6) . ? N8 C12 1.360(6) . ? N8 C14 1.441(6) . ? N8 C16 1.454(5) . ? N9 C15 1.371(6) . ? N9 C11 1.447(6) . ? N9 C13 1.464(6) . ? N10 C15 1.341(6) . ? N10 C17 1.455(5) . ? N10 C14 1.460(6) . ? C1 N1 1.368(5) 6_565 ? C3 C8 1.545(7) . ? C5 C5 1.528(11) 6_565 ? C6 N2 1.379(6) 6_565 ? C13 C14 1.540(6) . ? C16 N8 1.454(5) 6_565 ? C17 N10 1.455(5) 6_565 ? O1A C1A 1.223(7) . ? O2A C7A 1.254(5) . ? O3A C13A 1.216(5) . ? O4A C6A 1.229(8) . ? O5A C9A 1.232(6) . ? O6A C15A 1.223(5) . ? N1A C1A 1.366(5) . ? N1A C5A 1.441(6) . ? N1A C2A 1.448(6) . ? N2A C6A 1.352(5) . ? N2A C5A 1.456(6) . ? N2A C4A 1.457(6) . ? N3A C7A 1.352(6) . ? N3A C2A 1.436(6) . ? N3A C3A 1.453(6) . ? N4A C7A 1.362(6) . ? N4A C10A 1.421(6) . ? N4A C8A 1.457(6) . ? N5A C9A 1.356(6) . ? N5A C4A 1.432(6) . ? N5A C3A 1.448(6) . ? N6A C9A 1.356(6) . ? N6A C12A 1.427(6) . ? N6A C8A 1.462(6) . ? N7A C13A 1.384(6) . ? N7A C10A 1.438(6) . ? N7A C11A 1.439(6) . ? N8A C13A 1.361(6) . ? N8A C14A 1.446(6) . ? N8A C16A 1.449(5) . ? N9A C15A 1.371(6) . ? N9A C11A 1.445(6) . ? N9A C12A 1.447(6) . ? N10A C15A 1.347(6) . ? N10A C17A 1.453(5) . ? N10A C14A 1.456(6) . ? C1A N1A 1.366(5) 6 ? C3A C8A 1.575(7) . ? C5A C5A 1.560(10) 6 ? C6A N2A 1.352(5) 6 ? C11A C14A 1.557(7) . ? C16A N8A 1.449(5) 6 ? C17A N10A 1.453(5) 6 ? O1B C2B 1.230(6) . ? O2B C9B 1.232(5) . ? O3B C15B 1.229(8) . ? O4B C5B 1.228(7) . ? O5B C12B 1.228(6) . ? O6B C17B 1.238(9) . ? N1B C2B 1.387(7) . ? N1B C3B 1.448(7) . ? N1B C1B 1.450(6) . ? N2B C2B 1.350(7) . ? N2B C4B 1.446(7) . ? N2B C7B 1.467(7) . ? N3B C5B 1.348(7) . ? N3B C3B 1.411(8) . ? N3B C6B 1.473(6) . ? N4B C5B 1.386(7) . ? N4B C4B 1.425(7) . ? N4B C8B 1.442(7) . ? N5B C9B 1.349(6) . ? N5B C7B 1.428(7) . ? N5B C10B 1.443(6) . ? N6B C9B 1.348(6) . ? N6B C13B 1.447(6) . ? N6B C11B 1.465(6) . ? N7B C12B 1.384(7) . ? N7B C8B 1.435(7) . ? N7B C10B 1.471(6) . ? N8B C12B 1.360(7) . ? N8B C14B 1.422(7) . ? N8B C11B 1.447(7) . ? N9B C15B 1.348(5) . ? N9B C16B 1.456(6) . ? N9B C13B 1.460(7) . ? N10B C17B 1.352(6) . ? N10B C16B 1.436(6) . ? N10B C14B 1.455(7) . ? C1B N1B 1.450(6) 6 ? C3B C4B 1.541(8) . ? C6B N3B 1.473(6) 6 ? C10B C11B 1.533(8) . ? C15B N9B 1.348(5) 6 ? C16B C16B 1.517(11) 6 ? C17B N10B 1.352(6) 6 ? O1C C2C 1.220(5) . ? O2C C9C 1.238(5) . ? O3C C15C 1.235(8) . ? O4C C5C 1.226(6) . ? O5C C12C 1.212(6) . ? O6C C17C 1.208(8) . ? N1C C2C 1.379(6) . ? N1C C3C 1.438(6) . ? N1C C1C 1.447(5) . ? N2C C2C 1.367(6) . ? N2C C7C 1.426(6) . ? N2C C4C 1.462(6) . ? N3C C5C 1.369(6) . ? N3C C6C 1.437(5) . ? N3C C3C 1.448(6) . ? N4C C5C 1.354(6) . ? N4C C8C 1.442(6) . ? N4C C4C 1.450(6) . ? N5C C9C 1.361(6) . ? N5C C10C 1.443(6) . ? N5C C7C 1.453(6) . ? N6C C9C 1.343(6) . ? N6C C11C 1.446(6) . ? N6C C13C 1.452(6) . ? N7C C12C 1.359(7) . ? N7C C10C 1.453(7) . ? N7C C8C 1.453(7) . ? N8C C12C 1.375(7) . ? N8C C11C 1.418(7) . ? N8C C14C 1.455(7) . ? N9C C15C 1.372(6) . ? N9C C13C 1.452(7) . ? N9C C16C 1.451(6) . ? N10C C17C 1.369(6) . ? N10C C16C 1.439(6) . ? N10C C14C 1.460(7) . ? C1C N1C 1.447(5) 6_565 ? C3C C4C 1.547(6) . ? C6C N3C 1.437(5) 6_565 ? C10C C11C 1.568(7) . ? C15C N9C 1.372(6) 6_565 ? C16C C16C 1.549(11) 6_565 ? C17C N10C 1.369(6) 6_565 ? Cl9E Cl9E 1.48(4) 6_565 ? O32W O32W 1.07(2) 6 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C5 112.5(4) . . ? C1 N1 C2 122.4(4) . . ? C5 N1 C2 125.1(4) . . ? C6 N2 C5 112.3(4) . . ? C6 N2 C4 120.7(4) . . ? C5 N2 C4 126.3(4) . . ? C7 N3 C3 112.3(4) . . ? C7 N3 C2 121.4(4) . . ? C3 N3 C2 124.7(4) . . ? C7 N4 C8 112.6(4) . . ? C7 N4 C10 122.4(4) . . ? C8 N4 C10 124.9(4) . . ? C4 N5 C9 121.4(4) . . ? C4 N5 C3 126.3(4) . . ? C9 N5 C3 112.3(4) . . ? C9 N6 C8 113.3(4) . . ? C9 N6 C11 121.1(4) . . ? C8 N6 C11 125.0(4) . . ? C12 N7 C13 112.3(4) . . ? C12 N7 C10 121.2(4) . . ? C13 N7 C10 124.9(4) . . ? C12 N8 C14 113.1(4) . . ? C12 N8 C16 123.1(4) . . ? C14 N8 C16 123.8(4) . . ? C15 N9 C11 123.4(4) . . ? C15 N9 C13 112.2(4) . . ? C11 N9 C13 124.3(4) . . ? C15 N10 C17 122.2(4) . . ? C15 N10 C14 113.3(4) . . ? C17 N10 C14 124.2(4) . . ? O1 C1 N1 126.2(3) . 6_565 ? O1 C1 N1 126.2(3) . . ? N1 C1 N1 107.6(5) 6_565 . ? N3 C2 N1 113.3(4) . . ? N5 C3 N3 114.8(4) . . ? N5 C3 C8 103.4(4) . . ? N3 C3 C8 103.8(4) . . ? N5 C4 N2 115.4(4) . . ? N1 C5 N2 114.6(4) . . ? N1 C5 C5 103.7(3) . 6_565 ? N2 C5 C5 103.9(3) . 6_565 ? O4 C6 N2 126.4(3) . 6_565 ? O4 C6 N2 126.4(3) . . ? N2 C6 N2 107.2(6) 6_565 . ? O2 C7 N4 125.5(4) . . ? O2 C7 N3 126.5(4) . . ? N4 C7 N3 107.9(4) . . ? N6 C8 N4 116.4(4) . . ? N6 C8 C3 103.9(4) . . ? N4 C8 C3 102.9(4) . . ? O5 C9 N6 127.1(5) . . ? O5 C9 N5 125.6(5) . . ? N6 C9 N5 107.1(4) . . ? N7 C10 N4 113.7(4) . . ? N9 C11 N6 113.7(4) . . ? O3 C12 N8 126.8(4) . . ? O3 C12 N7 125.6(4) . . ? N8 C12 N7 107.5(4) . . ? N7 C13 N9 114.6(4) . . ? N7 C13 C14 103.4(3) . . ? N9 C13 C14 102.9(4) . . ? N8 C14 N10 115.3(4) . . ? N8 C14 C13 103.1(3) . . ? N10 C14 C13 103.0(4) . . ? O6 C15 N10 126.9(4) . . ? O6 C15 N9 124.7(4) . . ? N10 C15 N9 108.3(4) . . ? N8 C16 N8 113.3(5) 6_565 . ? N10 C17 N10 114.1(5) 6_565 . ? C1A N1A C5A 112.9(4) . . ? C1A N1A C2A 122.3(4) . . ? C5A N1A C2A 124.4(4) . . ? C6A N2A C5A 112.6(4) . . ? C6A N2A C4A 123.6(4) . . ? C5A N2A C4A 123.5(4) . . ? C7A N3A C2A 123.4(4) . . ? C7A N3A C3A 112.6(4) . . ? C2A N3A C3A 123.8(4) . . ? C7A N4A C10A 124.2(4) . . ? C7A N4A C8A 111.0(4) . . ? C10A N4A C8A 124.4(4) . . ? C9A N5A C4A 123.5(4) . . ? C9A N5A C3A 111.9(4) . . ? C4A N5A C3A 124.3(4) . . ? C9A N6A C12A 123.8(4) . . ? C9A N6A C8A 112.6(4) . . ? C12A N6A C8A 123.4(4) . . ? C13A N7A C10A 122.6(4) . . ? C13A N7A C11A 112.7(4) . . ? C10A N7A C11A 124.1(4) . . ? C13A N8A C14A 113.4(4) . . ? C13A N8A C16A 121.9(4) . . ? C14A N8A C16A 124.7(4) . . ? C15A N9A C11A 112.4(4) . . ? C15A N9A C12A 122.7(4) . . ? C11A N9A C12A 124.9(4) . . ? C15A N10A C17A 123.2(4) . . ? C15A N10A C14A 112.9(4) . . ? C17A N10A C14A 123.7(4) . . ? O1A C1A N1A 126.1(3) . . ? O1A C1A N1A 126.1(3) . 6 ? N1A C1A N1A 107.8(5) . 6 ? N3A C2A N1A 113.1(4) . . ? N5A C3A N3A 115.7(4) . . ? N5A C3A C8A 103.7(4) . . ? N3A C3A C8A 102.2(4) . . ? N5A C4A N2A 113.2(4) . . ? N1A C5A N2A 115.0(4) . . ? N1A C5A C5A 103.0(2) . 6 ? N2A C5A C5A 102.8(3) . 6 ? O4A C6A N2A 125.5(3) . . ? O4A C6A N2A 125.5(3) . 6 ? N2A C6A N2A 109.1(5) . 6 ? O2A C7A N3A 125.2(4) . . ? O2A C7A N4A 124.5(4) . . ? N3A C7A N4A 110.3(4) . . ? N4A C8A N6A 115.3(4) . . ? N4A C8A C3A 103.7(3) . . ? N6A C8A C3A 101.8(4) . . ? O5A C9A N5A 125.1(5) . . ? O5A C9A N6A 125.2(4) . . ? N5A C9A N6A 109.7(4) . . ? N4A C10A N7A 114.1(4) . . ? N7A C11A N9A 115.2(4) . . ? N7A C11A C14A 103.3(4) . . ? N9A C11A C14A 103.3(3) . . ? N6A C12A N9A 114.7(4) . . ? O3A C13A N8A 126.7(4) . . ? O3A C13A N7A 125.9(4) . . ? N8A C13A N7A 107.4(4) . . ? N8A C14A N10A 116.0(4) . . ? N8A C14A C11A 103.0(3) . . ? N10A C14A C11A 102.7(4) . . ? O6A C15A N10A 125.9(4) . . ? O6A C15A N9A 125.2(4) . . ? N10A C15A N9A 108.7(4) . . ? N8A C16A N8A 114.4(5) . 6 ? N10A C17A N10A 113.8(5) 6 . ? C2B N1B C3B 112.2(5) . . ? C2B N1B C1B 123.5(5) . . ? C3B N1B C1B 124.2(5) . . ? C2B N2B C4B 111.5(4) . . ? C2B N2B C7B 121.3(4) . . ? C4B N2B C7B 123.6(4) . . ? C5B N3B C3B 112.1(5) . . ? C5B N3B C6B 123.0(6) . . ? C3B N3B C6B 123.1(6) . . ? C5B N4B C4B 112.2(5) . . ? C5B N4B C8B 122.4(5) . . ? C4B N4B C8B 125.1(5) . . ? C9B N5B C7B 122.8(4) . . ? C9B N5B C10B 111.9(4) . . ? C7B N5B C10B 125.3(4) . . ? C9B N6B C13B 123.4(4) . . ? C9B N6B C11B 111.5(4) . . ? C13B N6B C11B 124.8(4) . . ? C12B N7B C8B 122.9(4) . . ? C12B N7B C10B 111.2(4) . . ? C8B N7B C10B 124.6(4) . . ? C12B N8B C14B 122.5(4) . . ? C12B N8B C11B 111.6(4) . . ? C14B N8B C11B 125.5(4) . . ? C15B N9B C16B 112.1(4) . . ? C15B N9B C13B 123.3(4) . . ? C16B N9B C13B 124.4(4) . . ? C17B N10B C16B 110.8(5) . . ? C17B N10B C14B 123.0(4) . . ? C16B N10B C14B 126.0(4) . . ? N1B C1B N1B 113.1(6) . 6 ? O1B C2B N2B 126.1(5) . . ? O1B C2B N1B 125.8(5) . . ? N2B C2B N1B 108.1(4) . . ? N3B C3B N1B 117.1(5) . . ? N3B C3B C4B 104.4(5) . . ? N1B C3B C4B 102.2(4) . . ? N4B C4B N2B 116.3(4) . . ? N4B C4B C3B 102.2(5) . . ? N2B C4B C3B 104.1(4) . . ? O4B C5B N3B 127.6(5) . . ? O4B C5B N4B 124.7(5) . . ? N3B C5B N4B 107.6(5) . . ? N3B C6B N3B 113.2(6) . 6 ? N5B C7B N2B 113.5(4) . . ? N7B C8B N4B 113.2(4) . . ? O2B C9B N6B 124.4(4) . . ? O2B C9B N5B 125.6(5) . . ? N6B C9B N5B 109.8(4) . . ? N5B C10B N7B 114.0(4) . . ? N5B C10B C11B 103.8(4) . . ? N7B C10B C11B 102.8(4) . . ? N8B C11B N6B 114.2(4) . . ? N8B C11B C10B 105.0(4) . . ? N6B C11B C10B 102.9(4) . . ? O5B C12B N8B 125.7(5) . . ? O5B C12B N7B 125.3(5) . . ? N8B C12B N7B 108.9(4) . . ? N6B C13B N9B 113.4(4) . . ? N8B C14B N10B 113.8(4) . . ? O3B C15B N9B 125.6(3) . . ? O3B C15B N9B 125.6(3) . 6 ? N9B C15B N9B 108.8(6) . 6 ? N10B C16B N9B 114.6(4) . . ? N10B C16B C16B 104.1(3) . 6 ? N9B C16B C16B 103.4(3) . 6 ? O6B C17B N10B 124.9(3) . 6 ? O6B C17B N10B 124.9(3) . . ? N10B C17B N10B 110.1(6) 6 . ? C2C N1C C3C 112.6(4) . . ? C2C N1C C1C 122.2(4) . . ? C3C N1C C1C 125.2(4) . . ? C2C N2C C7C 121.9(4) . . ? C2C N2C C4C 112.0(4) . . ? C7C N2C C4C 123.9(4) . . ? C5C N3C C6C 122.1(4) . . ? C5C N3C C3C 112.0(4) . . ? C6C N3C C3C 125.6(4) . . ? C5C N4C C8C 123.6(4) . . ? C5C N4C C4C 112.5(4) . . ? C8C N4C C4C 123.9(4) . . ? C9C N5C C10C 112.2(4) . . ? C9C N5C C7C 123.1(4) . . ? C10C N5C C7C 124.5(4) . . ? C9C N6C C11C 113.0(4) . . ? C9C N6C C13C 121.8(4) . . ? C11C N6C C13C 125.1(4) . . ? C12C N7C C10C 112.4(4) . . ? C12C N7C C8C 122.5(4) . . ? C10C N7C C8C 124.7(4) . . ? C12C N8C C11C 112.8(4) . . ? C12C N8C C14C 121.4(4) . . ? C11C N8C C14C 124.3(4) . . ? C15C N9C C13C 122.0(4) . . ? C15C N9C C16C 112.0(4) . . ? C13C N9C C16C 124.9(4) . . ? C17C N10C C16C 113.3(5) . . ? C17C N10C C14C 121.3(4) . . ? C16C N10C C14C 125.4(4) . . ? N1C C1C N1C 113.6(5) . 6_565 ? O1C C2C N2C 126.6(4) . . ? O1C C2C N1C 125.1(4) . . ? N2C C2C N1C 108.1(4) . . ? N1C C3C N3C 116.7(4) . . ? N1C C3C C4C 103.6(4) . . ? N3C C3C C4C 103.3(4) . . ? N4C C4C N2C 114.5(4) . . ? N4C C4C C3C 103.2(4) . . ? N2C C4C C3C 103.1(4) . . ? O4C C5C N4C 125.7(4) . . ? O4C C5C N3C 125.6(5) . . ? N4C C5C N3C 108.7(4) . . ? N3C C6C N3C 113.7(5) . 6_565 ? N2C C7C N5C 113.2(4) . . ? N4C C8C N7C 113.4(4) . . ? O2C C9C N6C 126.1(4) . . ? O2C C9C N5C 124.8(4) . . ? N6C C9C N5C 109.1(4) . . ? N5C C10C N7C 115.2(4) . . ? N5C C10C C11C 102.9(4) . . ? N7C C10C C11C 102.5(4) . . ? N8C C11C N6C 115.8(4) . . ? N8C C11C C10C 103.6(4) . . ? N6C C11C C10C 102.5(4) . . ? O5C C12C N7C 126.3(5) . . ? O5C C12C N8C 125.4(5) . . ? N7C C12C N8C 108.3(4) . . ? N9C C13C N6C 113.0(4) . . ? N8C C14C N10C 112.6(4) . . ? O3C C15C N9C 125.9(3) . 6_565 ? O3C C15C N9C 125.9(3) . . ? N9C C15C N9C 108.2(6) 6_565 . ? N10C C16C N9C 114.6(4) . . ? N10C C16C C16C 103.1(3) . 6_565 ? N9C C16C C16C 103.5(3) . 6_565 ? O6C C17C N10C 126.5(3) . 6_565 ? O6C C17C N10C 126.5(3) . . ? N10C C17C N10C 107.0(6) 6_565 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.617 _refine_diff_density_min -1.690 _refine_diff_density_rms 0.224