# 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 _publ_section_title ;Poly(methyl methacrylate)s with pendant calixpyrroles: Polymeric extractants for halide anion salts ; _publ_contact_author_name 'Prof. Christopher Bielawski' _publ_contact_author_email BIELAWSKI@CM.UTEXAS.ED loop_ _publ_author_name 'Christopher Bielawski' 'Ahmet Akar' 'Abdullah Aydogan' 'Daniel J. Coady' 'Vince Lynch' 'Manuel Marquez' ; J.L.Sessler ; # Attachment 'CALEST.CIF' data_calest _database_code_depnum_ccdc_archive 'CCDC 668095' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 N4 O2, C H2 Cl2' _chemical_formula_sum 'C33 H42 Cl2 N4 O2' _chemical_formula_weight 597.61 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3136(4) _cell_length_b 12.6502(6) _cell_length_c 13.1335(6) _cell_angle_alpha 98.569(1) _cell_angle_beta 105.772(1) _cell_angle_gamma 102.182(1) _cell_volume 1572.61(12) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6147 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prisms _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 0.242 _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 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13019 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7138 _reflns_number_gt 4928 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+1.4744P] 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 SHELXL _refine_ls_extinction_coef 0.0044(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7138 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1498 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 Cl1A Cl 0.43388(8) 0.32511(6) 0.70770(7) 0.0512(2) Uani 1 1 d . . . Cl2A Cl 0.45089(9) 0.09736(7) 0.69713(7) 0.0578(2) Uani 1 1 d . . . C1A C 0.3887(3) 0.1917(2) 0.6257(2) 0.0480(7) Uani 1 1 d . . . H1AA H 0.2857 0.1652 0.5949 0.058 Uiso 1 1 calc R . . H1AB H 0.4274 0.1953 0.5647 0.058 Uiso 1 1 calc R . . O1 O 0.60448(17) 0.32085(14) 0.50012(13) 0.0304(4) Uani 1 1 d . . . O2 O 0.71098(19) 0.49931(15) 0.57913(15) 0.0385(4) Uani 1 1 d . . . N1 N 0.28918(19) 0.23337(16) 0.12547(15) 0.0246(4) Uani 1 1 d . . . H1A H 0.2379 0.1679 0.1245 0.030 Uiso 1 1 calc R . . N2 N -0.0397(2) 0.25314(17) 0.00100(15) 0.0276(4) Uani 1 1 d . . . H2B H 0.0007 0.3227 0.0349 0.033 Uiso 1 1 calc R . . N3 N -0.11976(19) 0.22801(16) 0.23059(15) 0.0242(4) Uani 1 1 d . . . H3B H -0.1132 0.1618 0.2045 0.029 Uiso 1 1 calc R . . N4 N 0.23221(18) 0.25736(15) 0.37237(15) 0.0221(4) Uani 1 1 d . . . H4A H 0.2433 0.3292 0.3785 0.027 Uiso 1 1 calc R . . C1 C 0.3995(2) 0.29764(18) 0.21248(18) 0.0222(5) Uani 1 1 d . . . C2 C 0.4522(2) 0.3919(2) 0.1816(2) 0.0292(5) Uani 1 1 d . . . H2A H 0.5296 0.4517 0.2250 0.035 Uiso 1 1 calc R . . C3 C 0.3706(3) 0.3846(2) 0.0733(2) 0.0309(6) Uani 1 1 d . . . H3A H 0.3837 0.4388 0.0316 0.037 Uiso 1 1 calc R . . C4 C 0.2701(2) 0.2859(2) 0.03968(18) 0.0274(5) Uani 1 1 d . . . C5 C 0.1611(3) 0.2309(2) -0.06869(19) 0.0327(6) Uani 1 1 d . . . C6 C 0.0202(2) 0.1867(2) -0.05489(18) 0.0297(5) Uani 1 1 d . . . C7 C -0.0745(3) 0.0866(2) -0.0950(2) 0.0409(7) Uani 1 1 d . . . H7A H -0.0625 0.0236 -0.1370 0.049 Uiso 1 1 calc R . . C8 C -0.1948(3) 0.0921(2) -0.0635(2) 0.0389(6) Uani 1 1 d . . . H8A H -0.2773 0.0335 -0.0813 0.047 Uiso 1 1 calc R . . C9 C -0.1712(2) 0.1956(2) -0.00362(18) 0.0267(5) Uani 1 1 d . . . C10 C -0.2611(2) 0.2493(2) 0.04961(19) 0.0283(5) Uani 1 1 d . . . C11 C -0.1865(2) 0.29224(19) 0.16932(18) 0.0236(5) Uani 1 1 d . . . C12 C -0.1736(2) 0.3877(2) 0.23983(19) 0.0286(5) Uani 1 1 d . . . H12A H -0.2091 0.4482 0.2214 0.034 Uiso 1 1 calc R . . C13 C -0.0981(2) 0.3808(2) 0.34534(19) 0.0293(5) Uani 1 1 d . . . H13A H -0.0746 0.4357 0.4099 0.035 Uiso 1 1 calc R . . C14 C -0.0650(2) 0.28197(19) 0.33813(18) 0.0239(5) Uani 1 1 d . . . C15 C 0.0094(2) 0.2267(2) 0.42240(18) 0.0267(5) Uani 1 1 d . . . C16 C 0.1224(2) 0.18622(19) 0.38878(17) 0.0235(5) Uani 1 1 d . . . C17 C 0.1432(2) 0.0821(2) 0.37076(19) 0.0279(5) Uani 1 1 d . . . H17A H 0.0840 0.0157 0.3757 0.033 Uiso 1 1 calc R . . C18 C 0.2688(2) 0.09124(19) 0.34349(19) 0.0271(5) Uani 1 1 d . . . H18A H 0.3087 0.0322 0.3271 0.032 Uiso 1 1 calc R . . C19 C 0.3219(2) 0.20029(18) 0.34515(17) 0.0214(5) Uani 1 1 d . . . C20 C 0.4480(2) 0.25636(18) 0.31546(17) 0.0216(5) Uani 1 1 d . . . C21 C 0.5416(2) 0.35795(19) 0.40355(18) 0.0247(5) Uani 1 1 d . . . H21A H 0.6154 0.3984 0.3780 0.030 Uiso 1 1 calc R . . H21B H 0.4854 0.4087 0.4202 0.030 Uiso 1 1 calc R . . C22 C 0.6925(2) 0.4031(2) 0.58360(19) 0.0290(5) Uani 1 1 d . . . C23 C 0.7627(3) 0.3639(2) 0.6799(2) 0.0340(6) Uani 1 1 d . . . C24 C 0.7600(3) 0.2584(2) 0.6749(2) 0.0403(6) Uani 1 1 d . . . H24A H 0.7124 0.2055 0.6087 0.048 Uiso 1 1 calc R . . H24B H 0.8056 0.2355 0.7377 0.048 Uiso 1 1 calc R . . C25 C 0.8358(3) 0.4550(3) 0.7798(2) 0.0469(7) Uani 1 1 d . . . H25A H 0.8800 0.4236 0.8398 0.070 Uiso 1 1 calc R . . H25B H 0.7677 0.4908 0.7992 0.070 Uiso 1 1 calc R . . H25C H 0.9073 0.5098 0.7654 0.070 Uiso 1 1 calc R . . C26 C 0.5340(2) 0.17329(19) 0.29777(19) 0.0268(5) Uani 1 1 d . . . H26A H 0.4783 0.1131 0.2350 0.040 Uiso 1 1 calc R . . H26B H 0.5594 0.1427 0.3625 0.040 Uiso 1 1 calc R . . H26C H 0.6191 0.2113 0.2846 0.040 Uiso 1 1 calc R . . C27 C 0.1503(3) 0.3166(3) -0.1407(2) 0.0479(8) Uani 1 1 d . . . H27A H 0.0804 0.2813 -0.2116 0.072 Uiso 1 1 calc R . . H27B H 0.2412 0.3446 -0.1505 0.072 Uiso 1 1 calc R . . H27C H 0.1225 0.3782 -0.1059 0.072 Uiso 1 1 calc R . . C28 C 0.2052(3) 0.1345(3) -0.1238(2) 0.0493(8) Uani 1 1 d . . . H28A H 0.2122 0.0798 -0.0784 0.074 Uiso 1 1 calc R . . H28B H 0.2961 0.1629 -0.1335 0.074 Uiso 1 1 calc R . . H28C H 0.1354 0.0993 -0.1948 0.074 Uiso 1 1 calc R . . C29 C -0.3999(2) 0.1628(2) 0.0318(2) 0.0373(6) Uani 1 1 d . . . H29A H -0.3810 0.1025 0.0675 0.056 Uiso 1 1 calc R . . H29B H -0.4463 0.1330 -0.0461 0.056 Uiso 1 1 calc R . . H29C H -0.4607 0.1982 0.0627 0.056 Uiso 1 1 calc R . . C30 C -0.2945(3) 0.3459(2) -0.0021(2) 0.0392(6) Uani 1 1 d . . . H30A H -0.3567 0.3777 0.0303 0.059 Uiso 1 1 calc R . . H30B H -0.3404 0.3186 -0.0803 0.059 Uiso 1 1 calc R . . H30C H -0.2076 0.4030 0.0109 0.059 Uiso 1 1 calc R . . C31 C -0.0974(3) 0.1275(3) 0.4338(2) 0.0409(7) Uani 1 1 d . . . H31A H -0.1398 0.0743 0.3639 0.061 Uiso 1 1 calc R . . H31B H -0.1703 0.1536 0.4564 0.061 Uiso 1 1 calc R . . H31C H -0.0501 0.0915 0.4883 0.061 Uiso 1 1 calc R . . C32 C 0.0731(3) 0.3110(2) 0.5322(2) 0.0368(6) Uiso 1 1 d . . . H32A H 0.1193 0.2754 0.5877 0.055 Uiso 1 1 calc R . . H32B H -0.0011 0.3369 0.5529 0.055 Uiso 1 1 calc R . . H32C H 0.1417 0.3741 0.5257 0.055 Uiso 1 1 calc R . . 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 Cl1A 0.0423(4) 0.0423(4) 0.0644(5) -0.0012(3) 0.0150(4) 0.0126(3) Cl2A 0.0626(5) 0.0491(5) 0.0737(6) 0.0278(4) 0.0263(4) 0.0236(4) C1A 0.0499(18) 0.0416(16) 0.0415(16) 0.0052(13) -0.0013(13) 0.0120(14) O1 0.0296(9) 0.0300(9) 0.0261(9) 0.0056(7) 0.0028(7) 0.0045(7) O2 0.0390(10) 0.0292(10) 0.0390(10) 0.0010(8) 0.0059(8) 0.0046(8) N1 0.0215(10) 0.0289(10) 0.0217(10) 0.0064(8) 0.0057(8) 0.0040(8) N2 0.0233(10) 0.0333(11) 0.0252(10) 0.0032(8) 0.0075(8) 0.0076(9) N3 0.0243(10) 0.0268(10) 0.0226(10) 0.0051(8) 0.0069(8) 0.0098(8) N4 0.0213(9) 0.0207(9) 0.0261(10) 0.0067(8) 0.0088(8) 0.0064(8) C1 0.0190(11) 0.0249(12) 0.0236(11) 0.0042(9) 0.0067(9) 0.0082(9) C2 0.0264(12) 0.0280(13) 0.0335(13) 0.0073(10) 0.0090(10) 0.0080(10) C3 0.0317(13) 0.0358(14) 0.0338(14) 0.0175(11) 0.0141(11) 0.0148(11) C4 0.0238(12) 0.0428(15) 0.0231(12) 0.0120(10) 0.0107(9) 0.0172(11) C5 0.0254(12) 0.0543(17) 0.0216(12) 0.0082(11) 0.0085(10) 0.0161(12) C6 0.0258(12) 0.0463(15) 0.0180(11) 0.0045(10) 0.0057(9) 0.0151(11) C7 0.0357(15) 0.0445(16) 0.0376(15) -0.0060(12) 0.0107(12) 0.0116(13) C8 0.0289(14) 0.0387(15) 0.0408(15) -0.0025(12) 0.0089(12) 0.0022(12) C9 0.0197(11) 0.0383(14) 0.0217(11) 0.0075(10) 0.0051(9) 0.0083(10) C10 0.0222(12) 0.0412(14) 0.0235(12) 0.0100(10) 0.0074(9) 0.0103(10) C11 0.0176(11) 0.0315(12) 0.0236(11) 0.0091(9) 0.0068(9) 0.0078(9) C12 0.0258(12) 0.0279(13) 0.0328(13) 0.0096(10) 0.0075(10) 0.0092(10) C13 0.0250(12) 0.0312(13) 0.0269(12) 0.0003(10) 0.0056(10) 0.0049(10) C14 0.0181(11) 0.0322(13) 0.0218(11) 0.0059(9) 0.0069(9) 0.0064(9) C15 0.0231(12) 0.0381(14) 0.0218(11) 0.0114(10) 0.0084(9) 0.0090(10) C16 0.0192(11) 0.0313(12) 0.0191(11) 0.0094(9) 0.0039(9) 0.0051(9) C17 0.0273(12) 0.0250(12) 0.0285(13) 0.0078(10) 0.0082(10) 0.0005(10) C18 0.0274(12) 0.0235(12) 0.0304(13) 0.0045(10) 0.0102(10) 0.0066(10) C19 0.0202(11) 0.0240(11) 0.0194(11) 0.0033(9) 0.0046(9) 0.0075(9) C20 0.0195(11) 0.0227(11) 0.0212(11) 0.0036(9) 0.0053(9) 0.0047(9) C21 0.0228(11) 0.0251(12) 0.0241(12) 0.0067(9) 0.0043(9) 0.0051(9) C22 0.0234(12) 0.0342(14) 0.0288(13) 0.0037(10) 0.0096(10) 0.0064(10) C23 0.0238(12) 0.0494(17) 0.0284(13) 0.0091(11) 0.0085(10) 0.0077(11) C24 0.0326(14) 0.0513(18) 0.0414(16) 0.0202(13) 0.0093(12) 0.0167(13) C25 0.0332(15) 0.069(2) 0.0301(14) 0.0032(14) 0.0092(12) 0.0020(14) C26 0.0236(12) 0.0289(13) 0.0290(12) 0.0054(10) 0.0083(10) 0.0099(10) C27 0.0331(15) 0.087(2) 0.0324(15) 0.0291(15) 0.0124(12) 0.0197(15) C28 0.0342(15) 0.081(2) 0.0298(15) -0.0066(14) 0.0091(12) 0.0230(15) C29 0.0207(12) 0.0561(17) 0.0291(13) 0.0038(12) 0.0056(10) 0.0043(12) C30 0.0404(15) 0.0572(18) 0.0314(14) 0.0195(13) 0.0138(12) 0.0266(14) C31 0.0294(14) 0.0597(18) 0.0469(16) 0.0328(14) 0.0193(12) 0.0149(13) _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 Cl1A C1A 1.754(3) . ? Cl2A C1A 1.745(3) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? O1 C22 1.353(3) . ? O1 C21 1.452(3) . ? O2 C22 1.204(3) . ? N1 C1 1.374(3) . ? N1 C4 1.381(3) . ? N1 H1A 0.8800 . ? N2 C9 1.378(3) . ? N2 C6 1.382(3) . ? N2 H2B 0.8800 . ? N3 C14 1.377(3) . ? N3 C11 1.382(3) . ? N3 H3B 0.8800 . ? N4 C19 1.375(3) . ? N4 C16 1.378(3) . ? N4 H4A 0.8800 . ? C1 C2 1.368(3) . ? C1 C20 1.518(3) . ? C2 C3 1.420(3) . ? C2 H2A 0.9500 . ? C3 C4 1.367(4) . ? C3 H3A 0.9500 . ? C4 C5 1.510(3) . ? C5 C6 1.512(3) . ? C5 C28 1.539(4) . ? C5 C27 1.543(4) . ? C6 C7 1.354(4) . ? C7 C8 1.422(4) . ? C7 H7A 0.9500 . ? C8 C9 1.359(4) . ? C8 H8A 0.9500 . ? C9 C10 1.512(3) . ? C10 C11 1.507(3) . ? C10 C30 1.540(3) . ? C10 C29 1.543(3) . ? C11 C12 1.366(3) . ? C12 C13 1.419(3) . ? C12 H12A 0.9500 . ? C13 C14 1.360(3) . ? C13 H13A 0.9500 . ? C14 C15 1.516(3) . ? C15 C16 1.510(3) . ? C15 C31 1.540(3) . ? C15 C32 1.542(3) . ? C16 C17 1.375(3) . ? C17 C18 1.422(3) . ? C17 H17A 0.9500 . ? C18 C19 1.367(3) . ? C18 H18A 0.9500 . ? C19 C20 1.521(3) . ? C20 C21 1.532(3) . ? C20 C26 1.542(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.487(3) . ? C23 C24 1.320(4) . ? C23 C25 1.504(4) . ? C24 H24A 0.9500 . ? C24 H24B 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? 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 Cl2A C1A Cl1A 112.43(16) . . ? Cl2A C1A H1AA 109.1 . . ? Cl1A C1A H1AA 109.1 . . ? Cl2A C1A H1AB 109.1 . . ? Cl1A C1A H1AB 109.1 . . ? H1AA C1A H1AB 107.8 . . ? C22 O1 C21 114.43(18) . . ? C1 N1 C4 110.48(19) . . ? C1 N1 H1A 124.8 . . ? C4 N1 H1A 124.8 . . ? C9 N2 C6 110.7(2) . . ? C9 N2 H2B 124.6 . . ? C6 N2 H2B 124.6 . . ? C14 N3 C11 110.59(19) . . ? C14 N3 H3B 124.7 . . ? C11 N3 H3B 124.7 . . ? C19 N4 C16 110.42(18) . . ? C19 N4 H4A 124.8 . . ? C16 N4 H4A 124.8 . . ? C2 C1 N1 106.9(2) . . ? C2 C1 C20 131.7(2) . . ? N1 C1 C20 121.21(19) . . ? C1 C2 C3 107.8(2) . . ? C1 C2 H2A 126.1 . . ? C3 C2 H2A 126.1 . . ? C4 C3 C2 108.1(2) . . ? C4 C3 H3A 126.0 . . ? C2 C3 H3A 126.0 . . ? C3 C4 N1 106.6(2) . . ? C3 C4 C5 131.5(2) . . ? N1 C4 C5 121.7(2) . . ? C4 C5 C6 110.84(19) . . ? C4 C5 C28 109.3(2) . . ? C6 C5 C28 109.2(2) . . ? C4 C5 C27 109.0(2) . . ? C6 C5 C27 109.4(2) . . ? C28 C5 C27 109.2(2) . . ? C7 C6 N2 106.4(2) . . ? C7 C6 C5 131.6(2) . . ? N2 C6 C5 121.9(2) . . ? C6 C7 C8 108.3(2) . . ? C6 C7 H7A 125.8 . . ? C8 C7 H7A 125.8 . . ? C9 C8 C7 108.2(2) . . ? C9 C8 H8A 125.9 . . ? C7 C8 H8A 125.9 . . ? C8 C9 N2 106.4(2) . . ? C8 C9 C10 131.8(2) . . ? N2 C9 C10 121.8(2) . . ? C11 C10 C9 110.14(18) . . ? C11 C10 C30 109.3(2) . . ? C9 C10 C30 110.07(19) . . ? C11 C10 C29 109.78(19) . . ? C9 C10 C29 109.1(2) . . ? C30 C10 C29 108.4(2) . . ? C12 C11 N3 106.38(19) . . ? C12 C11 C10 132.7(2) . . ? N3 C11 C10 120.9(2) . . ? C11 C12 C13 108.0(2) . . ? C11 C12 H12A 126.0 . . ? C13 C12 H12A 126.0 . . ? C14 C13 C12 108.3(2) . . ? C14 C13 H13A 125.9 . . ? C12 C13 H13A 125.9 . . ? C13 C14 N3 106.7(2) . . ? C13 C14 C15 132.7(2) . . ? N3 C14 C15 120.6(2) . . ? C16 C15 C14 110.42(18) . . ? C16 C15 C31 109.3(2) . . ? C14 C15 C31 109.01(19) . . ? C16 C15 C32 110.22(19) . . ? C14 C15 C32 108.8(2) . . ? C31 C15 C32 109.0(2) . . ? C17 C16 N4 106.64(19) . . ? C17 C16 C15 131.4(2) . . ? N4 C16 C15 122.0(2) . . ? C16 C17 C18 107.9(2) . . ? C16 C17 H17A 126.0 . . ? C18 C17 H17A 126.0 . . ? C19 C18 C17 107.7(2) . . ? C19 C18 H18A 126.2 . . ? C17 C18 H18A 126.2 . . ? C18 C19 N4 107.31(19) . . ? C18 C19 C20 130.5(2) . . ? N4 C19 C20 122.06(19) . . ? C1 C20 C19 109.68(17) . . ? C1 C20 C21 106.63(18) . . ? C19 C20 C21 111.76(18) . . ? C1 C20 C26 109.61(18) . . ? C19 C20 C26 109.78(18) . . ? C21 C20 C26 109.32(18) . . ? O1 C21 C20 108.64(17) . . ? O1 C21 H21A 110.0 . . ? C20 C21 H21A 110.0 . . ? O1 C21 H21B 110.0 . . ? C20 C21 H21B 110.0 . . ? H21A C21 H21B 108.3 . . ? O2 C22 O1 122.2(2) . . ? O2 C22 C23 123.7(2) . . ? O1 C22 C23 114.1(2) . . ? C24 C23 C22 121.7(2) . . ? C24 C23 C25 124.7(3) . . ? C22 C23 C25 113.7(2) . . ? C23 C24 H24A 120.0 . . ? C23 C24 H24B 120.0 . . ? H24A C24 H24B 120.0 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 H26A 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C5 C27 H27A 109.5 . . ? C5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C5 C28 H28A 109.5 . . ? C5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C10 C29 H29A 109.5 . . ? C10 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C10 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C10 C30 H30A 109.5 . . ? C10 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C10 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C15 C31 H31A 109.5 . . ? C15 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C15 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C15 C32 H32A 109.5 . . ? C15 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C15 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? 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 C4 N1 C1 C2 -0.5(2) . . . . ? C4 N1 C1 C20 -176.60(18) . . . . ? N1 C1 C2 C3 0.5(3) . . . . ? C20 C1 C2 C3 176.0(2) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C2 C3 C4 N1 0.0(3) . . . . ? C2 C3 C4 C5 -175.5(2) . . . . ? C1 N1 C4 C3 0.3(2) . . . . ? C1 N1 C4 C5 176.38(19) . . . . ? C3 C4 C5 C6 -134.1(3) . . . . ? N1 C4 C5 C6 51.0(3) . . . . ? C3 C4 C5 C28 105.5(3) . . . . ? N1 C4 C5 C28 -69.4(3) . . . . ? C3 C4 C5 C27 -13.7(3) . . . . ? N1 C4 C5 C27 171.4(2) . . . . ? C9 N2 C6 C7 0.1(3) . . . . ? C9 N2 C6 C5 176.2(2) . . . . ? C4 C5 C6 C7 -131.2(3) . . . . ? C28 C5 C6 C7 -10.7(4) . . . . ? C27 C5 C6 C7 108.7(3) . . . . ? C4 C5 C6 N2 53.7(3) . . . . ? C28 C5 C6 N2 174.2(2) . . . . ? C27 C5 C6 N2 -66.4(3) . . . . ? N2 C6 C7 C8 0.3(3) . . . . ? C5 C6 C7 C8 -175.4(2) . . . . ? C6 C7 C8 C9 -0.5(3) . . . . ? C7 C8 C9 N2 0.5(3) . . . . ? C7 C8 C9 C10 179.1(2) . . . . ? C6 N2 C9 C8 -0.4(3) . . . . ? C6 N2 C9 C10 -179.1(2) . . . . ? C8 C9 C10 C11 123.3(3) . . . . ? N2 C9 C10 C11 -58.3(3) . . . . ? C8 C9 C10 C30 -116.1(3) . . . . ? N2 C9 C10 C30 62.3(3) . . . . ? C8 C9 C10 C29 2.7(4) . . . . ? N2 C9 C10 C29 -178.9(2) . . . . ? C14 N3 C11 C12 -0.2(2) . . . . ? C14 N3 C11 C10 -177.06(19) . . . . ? C9 C10 C11 C12 138.6(3) . . . . ? C30 C10 C11 C12 17.5(3) . . . . ? C29 C10 C11 C12 -101.3(3) . . . . ? C9 C10 C11 N3 -45.6(3) . . . . ? C30 C10 C11 N3 -166.7(2) . . . . ? C29 C10 C11 N3 74.6(3) . . . . ? N3 C11 C12 C13 -0.1(3) . . . . ? C10 C11 C12 C13 176.2(2) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? C12 C13 C14 N3 -0.5(3) . . . . ? C12 C13 C14 C15 -177.7(2) . . . . ? C11 N3 C14 C13 0.4(3) . . . . ? C11 N3 C14 C15 178.04(19) . . . . ? C13 C14 C15 C16 -130.5(3) . . . . ? N3 C14 C15 C16 52.6(3) . . . . ? C13 C14 C15 C31 109.4(3) . . . . ? N3 C14 C15 C31 -67.5(3) . . . . ? C13 C14 C15 C32 -9.4(3) . . . . ? N3 C14 C15 C32 173.7(2) . . . . ? C19 N4 C16 C17 -0.4(2) . . . . ? C19 N4 C16 C15 178.45(19) . . . . ? C14 C15 C16 C17 -121.5(3) . . . . ? C31 C15 C16 C17 -1.6(3) . . . . ? C32 C15 C16 C17 118.2(3) . . . . ? C14 C15 C16 N4 60.0(3) . . . . ? C31 C15 C16 N4 179.9(2) . . . . ? C32 C15 C16 N4 -60.3(3) . . . . ? N4 C16 C17 C18 0.3(3) . . . . ? C15 C16 C17 C18 -178.4(2) . . . . ? C16 C17 C18 C19 -0.1(3) . . . . ? C17 C18 C19 N4 -0.1(3) . . . . ? C17 C18 C19 C20 -175.4(2) . . . . ? C16 N4 C19 C18 0.3(2) . . . . ? C16 N4 C19 C20 176.12(18) . . . . ? C2 C1 C20 C19 141.7(2) . . . . ? N1 C1 C20 C19 -43.3(3) . . . . ? C2 C1 C20 C21 20.5(3) . . . . ? N1 C1 C20 C21 -164.46(19) . . . . ? C2 C1 C20 C26 -97.7(3) . . . . ? N1 C1 C20 C26 77.3(2) . . . . ? C18 C19 C20 C1 110.9(3) . . . . ? N4 C19 C20 C1 -63.9(3) . . . . ? C18 C19 C20 C21 -131.1(2) . . . . ? N4 C19 C20 C21 54.2(3) . . . . ? C18 C19 C20 C26 -9.6(3) . . . . ? N4 C19 C20 C26 175.63(19) . . . . ? C22 O1 C21 C20 178.58(18) . . . . ? C1 C20 C21 O1 -173.00(17) . . . . ? C19 C20 C21 O1 67.1(2) . . . . ? C26 C20 C21 O1 -54.6(2) . . . . ? C21 O1 C22 O2 3.5(3) . . . . ? C21 O1 C22 C23 -176.70(18) . . . . ? O2 C22 C23 C24 -167.3(3) . . . . ? O1 C22 C23 C24 12.9(3) . . . . ? O2 C22 C23 C25 12.0(3) . . . . ? O1 C22 C23 C25 -167.7(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A O2 0.88 2.07 2.945(3) 170.0 2_666 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.643 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.060 # Attachment 'CALEST.CIF' # Attachment 'calixoh_revised.cif' data_calixoh _database_code_depnum_ccdc_archive 'CCDC 668096' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3 C28 H36 N4 O, C H2 Cl2' _chemical_formula_sum 'C85 H110 Cl2 N12 O3' _chemical_formula_weight 1418.75 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2467(3) _cell_length_b 15.5098(5) _cell_length_c 25.4110(7) _cell_angle_alpha 76.983(3) _cell_angle_beta 82.586(3) _cell_angle_gamma 81.178(3) _cell_volume 3869.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 12768 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27.5 _exptl_crystal_description laths _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 0.141 _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 153(2) _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 'Nonius Kappa CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25243 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.2013 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 17015 _reflns_number_gt 6824 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydroxyl group was disordered on two of the three calixpyrrole molecules. In one calixpyrrole, the hydroxyl group was disordered over two different methyl groups. In the second calixpyrrole, the disorder amounted to a conformational difference on the same methyl group. The disorder was modeled in the same way for both groups. The site occupancy factor for one oxygen atom was assigned the variable x. The site occupancy factor for the alternate oxygen atom was assigned to (1-x). A common isotropic displacement parameter was refined for both oxygen atoms while refining the site occupancy factor. The C-O bond lengths and the C-C-O bond angles were restrained to be equivalent throughout the refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+1.9114P] 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 SHELXL _refine_ls_extinction_coef 0.0042(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 17015 _refine_ls_number_parameters 963 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2336 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.1998 _refine_ls_wR_factor_gt 0.1556 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 N1 N 0.3690(3) 0.9694(2) 0.19791(13) 0.0374(8) Uani 1 1 d . . . H1A H 0.3974 0.9375 0.1731 0.045 Uiso 1 1 calc R . . O1 O 0.7240(6) 1.1252(4) 0.1290(3) 0.130(3) Uani 0.73 1 d PD . . H1 H 0.7657 1.0880 0.1114 0.194 Uiso 0.73 1 calc PR . . O1' O 0.520(2) 1.0941(11) 0.1037(5) 0.168(9) Uani 0.27 1 d PD . . H1' H 0.5129 1.0399 0.1065 0.252 Uiso 0.27 1 calc PR . . N2 N 0.6721(3) 0.8654(2) 0.21857(14) 0.0397(8) Uani 1 1 d . . . H2B H 0.6383 0.8599 0.2526 0.048 Uiso 1 1 calc R . . N3 N 0.5456(3) 0.6710(2) 0.23665(13) 0.0354(8) Uani 1 1 d . . . H3B H 0.5345 0.6986 0.2029 0.042 Uiso 1 1 calc R . . N4 N 0.2374(3) 0.7768(2) 0.23629(13) 0.0352(8) Uani 1 1 d . . . H4A H 0.2592 0.7843 0.2672 0.042 Uiso 1 1 calc R . . C1 C 0.2417(4) 0.9765(3) 0.22370(16) 0.0382(10) Uani 1 1 d . . . C2 C 0.2387(4) 1.0325(3) 0.25884(18) 0.0502(12) Uani 1 1 d . . . H2A H 0.1642 1.0501 0.2822 0.060 Uiso 1 1 calc R . . C3 C 0.3659(4) 1.0591(3) 0.25407(17) 0.0473(11) Uani 1 1 d . . . H3A H 0.3917 1.0980 0.2737 0.057 Uiso 1 1 calc R . . C4 C 0.4451(4) 1.0201(2) 0.21693(16) 0.0358(10) Uani 1 1 d . . . C5 C 0.5880(4) 1.0278(3) 0.19481(17) 0.0434(11) Uani 1 1 d D . . C6 C 0.6578(4) 0.9426(3) 0.18019(17) 0.0376(10) Uani 1 1 d . . . C7 C 0.7239(4) 0.9235(3) 0.13356(18) 0.0505(12) Uani 1 1 d . . . H7A H 0.7321 0.9642 0.0996 0.061 Uiso 1 1 calc R . . C8 C 0.7784(4) 0.8328(3) 0.14438(18) 0.0491(12) Uani 1 1 d . . . H8A H 0.8292 0.8018 0.1187 0.059 Uiso 1 1 calc R . . C9 C 0.7463(4) 0.7973(3) 0.19734(16) 0.0340(9) Uani 1 1 d . . . C10 C 0.7809(4) 0.7069(3) 0.23196(16) 0.0364(10) Uani 1 1 d . . . C11 C 0.6580(4) 0.6675(2) 0.26179(16) 0.0328(9) Uani 1 1 d . . . C12 C 0.6365(4) 0.6204(3) 0.31313(17) 0.0414(10) Uani 1 1 d . . . H12B H 0.6970 0.6074 0.3401 0.050 Uiso 1 1 calc R . . C13 C 0.5068(4) 0.5936(3) 0.31971(18) 0.0424(10) Uani 1 1 d . . . H13B H 0.4659 0.5597 0.3518 0.051 Uiso 1 1 calc R . . C14 C 0.4526(4) 0.6252(2) 0.27185(16) 0.0352(10) Uani 1 1 d . . . C15 C 0.3225(4) 0.6127(3) 0.25402(17) 0.0392(10) Uani 1 1 d . . . C16 C 0.2606(4) 0.6970(3) 0.21951(17) 0.0360(10) Uani 1 1 d . . . C17 C 0.2114(4) 0.7133(3) 0.16993(17) 0.0461(11) Uani 1 1 d . . . H17B H 0.2125 0.6707 0.1482 0.055 Uiso 1 1 calc R . . C18 C 0.1589(4) 0.8042(3) 0.15688(18) 0.0478(11) Uani 1 1 d . . . H18B H 0.1189 0.8334 0.1248 0.057 Uiso 1 1 calc R . . C19 C 0.1757(4) 0.8432(3) 0.19869(17) 0.0408(10) Uani 1 1 d . . . C20 C 0.1314(4) 0.9357(3) 0.20809(19) 0.0486(12) Uani 1 1 d . . . C21 C 0.5902(4) 1.1037(3) 0.1458(2) 0.0620(14) Uani 1 1 d D . . H21F H 0.5453 1.0908 0.1182 0.093 Uiso 0.65 1 d PR . . H21G H 0.5458 1.1573 0.1563 0.093 Uiso 1 1 d R . . H21H H 0.6803 1.1116 0.1321 0.093 Uiso 0.35 1 d PR . . C22 C 0.6618(4) 1.0529(3) 0.2376(2) 0.0671(15) Uani 1 1 d . . . H22A H 0.6628 1.0051 0.2702 0.101 Uiso 1 1 calc R . . H22B H 0.6162 1.1085 0.2471 0.101 Uiso 1 1 calc R . . H22C H 0.7532 1.0612 0.2226 0.101 Uiso 1 1 calc R . . C23 C 0.8737(4) 0.7128(3) 0.27364(17) 0.0470(11) Uani 1 1 d . . . H23A H 0.9542 0.7366 0.2546 0.071 Uiso 1 1 calc R . . H23B H 0.8978 0.6532 0.2956 0.071 Uiso 1 1 calc R . . H23C H 0.8284 0.7524 0.2973 0.071 Uiso 1 1 calc R . . C24 C 0.8556(4) 0.6442(3) 0.19622(18) 0.0465(11) Uani 1 1 d . . . H24A H 0.7992 0.6396 0.1689 0.070 Uiso 1 1 calc R . . H24B H 0.8786 0.5850 0.2188 0.070 Uiso 1 1 calc R . . H24C H 0.9369 0.6679 0.1781 0.070 Uiso 1 1 calc R . . C25 C 0.3497(4) 0.5380(3) 0.2213(2) 0.0623(14) Uani 1 1 d . . . H25A H 0.2659 0.5273 0.2108 0.093 Uiso 1 1 calc R . . H25B H 0.3909 0.4832 0.2438 0.093 Uiso 1 1 calc R . . H25C H 0.4096 0.5562 0.1887 0.093 Uiso 1 1 calc R . . C26 C 0.2267(4) 0.5825(3) 0.30447(19) 0.0535(12) Uani 1 1 d . . . H26A H 0.2050 0.6301 0.3250 0.080 Uiso 1 1 calc R . . H26B H 0.2689 0.5286 0.3274 0.080 Uiso 1 1 calc R . . H26C H 0.1452 0.5697 0.2931 0.080 Uiso 1 1 calc R . . C27 C 0.0169(4) 0.9319(3) 0.2550(2) 0.0760(17) Uani 1 1 d . . . H27A H -0.0574 0.9081 0.2450 0.114 Uiso 1 1 calc R . . H27B H -0.0128 0.9921 0.2615 0.114 Uiso 1 1 calc R . . H27C H 0.0490 0.8931 0.2881 0.114 Uiso 1 1 calc R . . C28 C 0.0799(5) 0.9959(3) 0.1563(2) 0.0825(18) Uani 1 1 d . . . H28A H 0.1523 1.0004 0.1270 0.124 Uiso 1 1 calc R . . H28B H 0.0463 1.0555 0.1631 0.124 Uiso 1 1 calc R . . H28C H 0.0081 0.9702 0.1458 0.124 Uiso 1 1 calc R . . O1B O 0.4538(5) 0.8194(4) 0.1247(2) 0.0776(19) Uani 0.60 1 d PD . . H1B H 0.3735 0.8133 0.1340 0.116 Uiso 0.60 1 calc PR . . O1BA O 0.7688(8) 0.8057(4) -0.1448(3) 0.079(3) Uani 0.40 1 d PD . . H1BA H 0.7921 0.8238 -0.1191 0.119 Uiso 0.40 1 calc PR . . N1B N 0.2947(3) 0.7572(2) 0.00960(13) 0.0393(8) Uani 1 1 d . . . H1BN H 0.3226 0.6999 0.0126 0.047 Uiso 1 1 calc R . . N2B N 0.6192(3) 0.7307(2) -0.05018(13) 0.0416(8) Uani 1 1 d . . . H2BN H 0.6125 0.7831 -0.0726 0.050 Uiso 1 1 calc R . . N3B N 0.4945(3) 0.6448(2) -0.14370(13) 0.0385(8) Uani 1 1 d . . . H3BN H 0.4687 0.6171 -0.1107 0.046 Uiso 1 1 calc R . . N4B N 0.1794(3) 0.7059(2) -0.09657(12) 0.0383(8) Uani 1 1 d . . . H4BN H 0.1948 0.7610 -0.1108 0.046 Uiso 1 1 calc R . . C1B C 0.1696(4) 0.7965(3) -0.00221(16) 0.0409(10) Uani 1 1 d . . . C2B C 0.1650(4) 0.8848(3) -0.00170(18) 0.0541(12) Uani 1 1 d . . . H2BB H 0.0906 0.9293 -0.0079 0.065 Uiso 1 1 calc R . . C3B C 0.2920(5) 0.8981(3) 0.00991(19) 0.0574(13) Uani 1 1 d . . . H3BB H 0.3171 0.9532 0.0128 0.069 Uiso 1 1 calc R . . C4B C 0.3706(4) 0.8189(3) 0.01615(17) 0.0448(11) Uani 1 1 d . . . C5B C 0.5112(4) 0.7917(3) 0.03130(16) 0.0502(12) Uani 1 1 d D . . C6B C 0.5773(4) 0.7177(3) 0.00400(18) 0.0479(11) Uani 1 1 d . . . C7B C 0.5956(7) 0.6274(4) 0.0230(2) 0.106(2) Uani 1 1 d . . . H7BA H 0.5741 0.5967 0.0592 0.127 Uiso 1 1 calc R . . C8B C 0.6532(7) 0.5875(4) -0.0216(3) 0.107(2) Uani 1 1 d . . . H8BA H 0.6741 0.5253 -0.0204 0.128 Uiso 1 1 calc R . . C9B C 0.6728(4) 0.6525(3) -0.06536(18) 0.0471(11) Uani 1 1 d . . . C10B C 0.7284(4) 0.6485(3) -0.12248(18) 0.0482(12) Uani 1 1 d D . . C11B C 0.6193(4) 0.6694(3) -0.16049(18) 0.0424(11) Uani 1 1 d . . . C12B C 0.6190(4) 0.7087(3) -0.21365(18) 0.0453(11) Uani 1 1 d . . . H12C H 0.6918 0.7324 -0.2364 0.054 Uiso 1 1 calc R . . C13B C 0.4921(4) 0.7086(3) -0.22982(17) 0.0403(10) Uani 1 1 d . . . H13C H 0.4650 0.7316 -0.2652 0.048 Uiso 1 1 calc R . . C14B C 0.4162(4) 0.6697(2) -0.18586(16) 0.0342(9) Uani 1 1 d . . . C15B C 0.2751(4) 0.6473(3) -0.18067(16) 0.0366(10) Uani 1 1 d . . . C16B C 0.2133(4) 0.6355(3) -0.12267(16) 0.0366(10) Uani 1 1 d . . . C17B C 0.1728(4) 0.5627(3) -0.08767(19) 0.0517(12) Uani 1 1 d . . . H17C H 0.1820 0.5040 -0.0942 0.062 Uiso 1 1 calc R . . C18B C 0.1134(4) 0.5904(3) -0.03894(19) 0.0548(12) Uani 1 1 d . . . H18C H 0.0765 0.5530 -0.0073 0.066 Uiso 1 1 calc R . . C19B C 0.1188(4) 0.6787(3) -0.04567(15) 0.0388(10) Uani 1 1 d . . . C20B C 0.0655(4) 0.7416(3) -0.00884(17) 0.0464(11) Uani 1 1 d . . . C21B C 0.5111(4) 0.7563(4) 0.09309(18) 0.0757(17) Uani 1 1 d D . . H21C H 0.4629 0.7057 0.1038 0.114 Uiso 1 1 d R . . H21D H 0.6010 0.7386 0.1019 0.114 Uiso 1 1 d R . . H21E H 0.4699 0.8021 0.1119 0.114 Uiso 0.40 1 d PR . . C22B C 0.5884(4) 0.8719(4) 0.0145(2) 0.0750(17) Uani 1 1 d . . . H22D H 0.6801 0.8535 0.0235 0.113 Uiso 1 1 calc R . . H22E H 0.5465 0.9185 0.0338 0.113 Uiso 1 1 calc R . . H22F H 0.5882 0.8950 -0.0247 0.113 Uiso 1 1 calc R . . C23B C 0.8279(4) 0.7163(3) -0.1435(2) 0.0696(16) Uani 1 1 d D . . H23G H 0.8976 0.7044 -0.1200 0.104 Uiso 1 1 d R . . H23H H 0.8651 0.7108 -0.1794 0.104 Uiso 1 1 d R . . H23I H 0.7836 0.7758 -0.1445 0.104 Uiso 0.60 1 d PR . . C24B C 0.8036(5) 0.5556(3) -0.1235(2) 0.0798(18) Uani 1 1 d . . . H24D H 0.8759 0.5437 -0.1000 0.120 Uiso 1 1 calc R . . H24E H 0.8405 0.5528 -0.1607 0.120 Uiso 1 1 calc R . . H24F H 0.7427 0.5107 -0.1103 0.120 Uiso 1 1 calc R . . C25B C 0.2784(4) 0.5599(3) -0.20006(19) 0.0541(13) Uani 1 1 d . . . H25D H 0.3319 0.5116 -0.1771 0.081 Uiso 1 1 calc R . . H25E H 0.3177 0.5671 -0.2378 0.081 Uiso 1 1 calc R . . H25F H 0.1878 0.5452 -0.1976 0.081 Uiso 1 1 calc R . . C26B C 0.1923(4) 0.7217(3) -0.21687(17) 0.0506(12) Uani 1 1 d . . . H26D H 0.1021 0.7066 -0.2148 0.076 Uiso 1 1 calc R . . H26E H 0.2326 0.7288 -0.2545 0.076 Uiso 1 1 calc R . . H26F H 0.1889 0.7777 -0.2046 0.076 Uiso 1 1 calc R . . C27B C -0.0545(5) 0.8054(4) -0.0317(2) 0.0777(17) Uani 1 1 d . . . H27D H -0.0276 0.8384 -0.0682 0.116 Uiso 1 1 calc R . . H27E H -0.0866 0.8475 -0.0079 0.116 Uiso 1 1 calc R . . H27F H -0.1255 0.7708 -0.0336 0.116 Uiso 1 1 calc R . . C28B C 0.0190(5) 0.6876(4) 0.04753(19) 0.0731(16) Uani 1 1 d . . . H28D H -0.0539 0.6556 0.0441 0.110 Uiso 1 1 calc R . . H28E H -0.0118 0.7283 0.0723 0.110 Uiso 1 1 calc R . . H28F H 0.0930 0.6446 0.0619 0.110 Uiso 1 1 calc R . . Cl1A Cl 0.29686(14) 0.52129(8) 0.55833(5) 0.0673(4) Uani 1 1 d . . . Cl2A Cl 0.23350(13) 0.57189(9) 0.44621(5) 0.0690(4) Uani 1 1 d . . . C1C C 0.2526(4) 0.6100(3) 0.50405(16) 0.0445(11) Uani 1 1 d . . . H1CA H 0.1684 0.6447 0.5153 0.053 Uiso 1 1 calc R . . H1CB H 0.3221 0.6503 0.4952 0.053 Uiso 1 1 calc R . . O1A O 0.3396(3) 0.7672(2) 0.34438(14) 0.0682(9) Uani 1 1 d . . . H1A1 H 0.3885 0.7191 0.3423 0.102 Uiso 1 1 calc R . . N1A N 0.4316(3) 0.8061(2) 0.49632(12) 0.0336(8) Uani 1 1 d . . . H1AA H 0.3812 0.8518 0.5066 0.040 Uiso 1 1 calc R . . N2A N 0.1606(3) 0.8353(2) 0.42269(13) 0.0383(8) Uani 1 1 d . . . H2AB H 0.1792 0.7789 0.4202 0.046 Uiso 1 1 calc R . . N3A N -0.0260(3) 0.7750(2) 0.54659(13) 0.0383(8) Uani 1 1 d . . . H3AB H -0.0037 0.8271 0.5476 0.046 Uiso 1 1 calc R . . N4A N 0.2581(3) 0.7130(2) 0.61851(12) 0.0354(8) Uani 1 1 d . . . H4AA H 0.2711 0.6587 0.6122 0.043 Uiso 1 1 calc R . . C1A C 0.4987(4) 0.7374(3) 0.53053(16) 0.0330(9) Uani 1 1 d . . . C2A C 0.5634(4) 0.6801(3) 0.49947(16) 0.0361(10) Uani 1 1 d . . . H2AA H 0.6174 0.6256 0.5120 0.043 Uiso 1 1 calc R . . C3A C 0.5356(4) 0.7164(3) 0.44526(17) 0.0393(10) Uani 1 1 d . . . H3AA H 0.5691 0.6905 0.4149 0.047 Uiso 1 1 calc R . . C4A C 0.4532(4) 0.7942(3) 0.44364(16) 0.0345(10) Uani 1 1 d . . . C5A C 0.3979(4) 0.8656(3) 0.39857(15) 0.0359(10) Uani 1 1 d . . . C6A C 0.2524(4) 0.8948(3) 0.41325(15) 0.0339(9) Uani 1 1 d . . . C7A C 0.1851(4) 0.9733(3) 0.42250(17) 0.0442(11) Uani 1 1 d . . . H7AA H 0.2222 1.0269 0.4196 0.053 Uiso 1 1 calc R . . C8A C 0.0502(4) 0.9613(3) 0.43720(17) 0.0486(11) Uani 1 1 d . . . H8AA H -0.0188 1.0056 0.4461 0.058 Uiso 1 1 calc R . . C9A C 0.0356(4) 0.8764(3) 0.43655(15) 0.0376(10) Uani 1 1 d . . . C10A C -0.0821(4) 0.8244(3) 0.45023(16) 0.0427(11) Uani 1 1 d . . . C11A C -0.0666(4) 0.7546(3) 0.50167(16) 0.0373(10) Uani 1 1 d . . . C12A C -0.0916(4) 0.6685(3) 0.51670(17) 0.0431(11) Uani 1 1 d . . . H12A H -0.1214 0.6355 0.4943 0.052 Uiso 1 1 calc R . . C13A C -0.0658(4) 0.6364(3) 0.57146(17) 0.0423(11) Uani 1 1 d . . . H13A H -0.0753 0.5781 0.5922 0.051 Uiso 1 1 calc R . . C14A C -0.0248(4) 0.7035(3) 0.58930(16) 0.0386(10) Uani 1 1 d . . . C15A C 0.0134(4) 0.7098(3) 0.64382(16) 0.0401(10) Uani 1 1 d . . . C16A C 0.1374(4) 0.7552(3) 0.63559(15) 0.0363(10) Uani 1 1 d . . . C17A C 0.1590(4) 0.8366(3) 0.64049(16) 0.0422(11) Uani 1 1 d . . . H17A H 0.0934 0.8810 0.6517 0.051 Uiso 1 1 calc R . . C18A C 0.2963(4) 0.8451(3) 0.62606(16) 0.0391(10) Uani 1 1 d . . . H18A H 0.3383 0.8957 0.6259 0.047 Uiso 1 1 calc R . . C19A C 0.3564(4) 0.7673(3) 0.61254(15) 0.0327(9) Uani 1 1 d . . . C20A C 0.4962(4) 0.7386(2) 0.58996(15) 0.0341(9) Uani 1 1 d . . . C21A C 0.4187(4) 0.8335(3) 0.34487(17) 0.0453(11) Uani 1 1 d . . . H21A H 0.3981 0.8851 0.3149 0.054 Uiso 1 1 calc R . . H21B H 0.5133 0.8096 0.3382 0.054 Uiso 1 1 calc R . . C22A C 0.4750(4) 0.9465(3) 0.38881(18) 0.0512(12) Uani 1 1 d . . . H22G H 0.4730 0.9662 0.4230 0.077 Uiso 1 1 calc R . . H22H H 0.4337 0.9953 0.3619 0.077 Uiso 1 1 calc R . . H22I H 0.5672 0.9295 0.3753 0.077 Uiso 1 1 calc R . . C23A C -0.0966(5) 0.7801(3) 0.40306(17) 0.0627(14) Uani 1 1 d . . . H23D H -0.0148 0.7408 0.3959 0.094 Uiso 1 1 calc R . . H23E H -0.1129 0.8263 0.3704 0.094 Uiso 1 1 calc R . . H23F H -0.1713 0.7450 0.4129 0.094 Uiso 1 1 calc R . . C24A C -0.2086(4) 0.8896(3) 0.45871(19) 0.0606(13) Uani 1 1 d . . . H24G H -0.2860 0.8570 0.4665 0.091 Uiso 1 1 calc R . . H24H H -0.2185 0.9362 0.4258 0.091 Uiso 1 1 calc R . . H24I H -0.2019 0.9170 0.4893 0.091 Uiso 1 1 calc R . . C25A C 0.0341(4) 0.6165(3) 0.67965(17) 0.0540(12) Uani 1 1 d . . . H25G H 0.1049 0.5794 0.6620 0.081 Uiso 1 1 calc R . . H25H H -0.0484 0.5895 0.6850 0.081 Uiso 1 1 calc R . . H25I H 0.0591 0.6205 0.7149 0.081 Uiso 1 1 calc R . . C26A C -0.1000(4) 0.7670(3) 0.67144(18) 0.0572(13) Uani 1 1 d . . . H26G H -0.0763 0.7710 0.7069 0.086 Uiso 1 1 calc R . . H26H H -0.1816 0.7392 0.6764 0.086 Uiso 1 1 calc R . . H26I H -0.1139 0.8270 0.6486 0.086 Uiso 1 1 calc R . . C27A C 0.5493(4) 0.6465(3) 0.62117(17) 0.0458(11) Uani 1 1 d . . . H27G H 0.4955 0.6023 0.6164 0.069 Uiso 1 1 calc R . . H27H H 0.5449 0.6473 0.6598 0.069 Uiso 1 1 calc R . . H27I H 0.6416 0.6308 0.6073 0.069 Uiso 1 1 calc R . . C28A C 0.5871(4) 0.8065(3) 0.59581(17) 0.0450(11) Uani 1 1 d . . . H28G H 0.6782 0.7881 0.5817 0.067 Uiso 1 1 calc R . . H28H H 0.5850 0.8084 0.6342 0.067 Uiso 1 1 calc R . . H28I H 0.5555 0.8658 0.5753 0.067 Uiso 1 1 calc R . . 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 N1 0.035(2) 0.036(2) 0.043(2) -0.0114(16) -0.0036(17) -0.0059(16) O1 0.111(5) 0.088(5) 0.184(7) -0.041(4) 0.057(5) -0.035(4) O1' 0.24(3) 0.119(16) 0.137(18) -0.027(14) 0.055(18) -0.073(18) N2 0.042(2) 0.035(2) 0.040(2) -0.0066(18) 0.0037(17) -0.0066(16) N3 0.0332(19) 0.040(2) 0.0347(19) -0.0079(16) -0.0067(16) -0.0069(16) N4 0.0312(18) 0.040(2) 0.038(2) -0.0112(17) -0.0060(16) -0.0085(16) C1 0.031(2) 0.037(2) 0.043(3) 0.000(2) -0.004(2) -0.0039(19) C2 0.047(3) 0.046(3) 0.052(3) -0.007(2) 0.002(2) 0.000(2) C3 0.056(3) 0.040(3) 0.049(3) -0.013(2) -0.006(2) -0.007(2) C4 0.031(2) 0.030(2) 0.045(3) -0.005(2) -0.004(2) -0.0052(18) C5 0.042(3) 0.029(2) 0.060(3) -0.006(2) -0.007(2) -0.007(2) C6 0.027(2) 0.039(3) 0.047(3) -0.007(2) -0.006(2) -0.0058(19) C7 0.066(3) 0.045(3) 0.041(3) -0.004(2) -0.011(2) -0.012(2) C8 0.059(3) 0.045(3) 0.043(3) -0.014(2) 0.000(2) -0.002(2) C9 0.029(2) 0.037(2) 0.038(3) -0.011(2) -0.0027(19) -0.0089(19) C10 0.028(2) 0.038(2) 0.046(3) -0.011(2) -0.0040(19) -0.0077(18) C11 0.030(2) 0.034(2) 0.035(2) -0.007(2) -0.0062(19) -0.0024(18) C12 0.036(3) 0.043(3) 0.046(3) -0.008(2) -0.012(2) -0.004(2) C13 0.040(3) 0.036(2) 0.046(3) -0.003(2) -0.001(2) -0.002(2) C14 0.030(2) 0.033(2) 0.042(3) -0.010(2) 0.000(2) -0.0036(19) C15 0.032(2) 0.036(2) 0.052(3) -0.014(2) -0.006(2) -0.0061(19) C16 0.026(2) 0.039(3) 0.047(3) -0.016(2) 0.000(2) -0.0106(19) C17 0.036(3) 0.065(3) 0.044(3) -0.020(2) -0.003(2) -0.016(2) C18 0.039(3) 0.064(3) 0.041(3) -0.005(2) -0.008(2) -0.013(2) C19 0.023(2) 0.046(3) 0.049(3) 0.003(2) -0.007(2) -0.0093(19) C20 0.028(2) 0.041(3) 0.074(3) 0.001(2) -0.012(2) -0.005(2) C21 0.040(3) 0.051(3) 0.088(4) -0.008(3) 0.010(3) -0.008(2) C22 0.048(3) 0.056(3) 0.113(5) -0.043(3) -0.022(3) -0.006(2) C23 0.043(3) 0.050(3) 0.050(3) -0.003(2) -0.016(2) -0.014(2) C24 0.037(2) 0.044(3) 0.060(3) -0.019(2) 0.005(2) -0.006(2) C25 0.054(3) 0.047(3) 0.100(4) -0.038(3) -0.020(3) -0.006(2) C26 0.035(3) 0.048(3) 0.071(3) 0.003(2) -0.006(2) -0.011(2) C27 0.038(3) 0.055(3) 0.133(5) -0.032(3) 0.017(3) -0.006(2) C28 0.069(4) 0.054(3) 0.124(5) 0.015(3) -0.060(3) -0.013(3) O1B 0.045(3) 0.152(6) 0.060(4) -0.062(4) 0.018(3) -0.047(4) O1BA 0.095(7) 0.083(6) 0.063(6) -0.008(5) -0.012(5) -0.029(5) N1B 0.033(2) 0.045(2) 0.043(2) -0.0132(17) -0.0085(16) -0.0043(17) N2B 0.042(2) 0.049(2) 0.036(2) -0.0119(18) -0.0018(17) -0.0086(17) N3B 0.0330(19) 0.045(2) 0.038(2) -0.0063(17) -0.0055(16) -0.0086(16) N4B 0.039(2) 0.038(2) 0.039(2) -0.0066(16) -0.0023(16) -0.0118(16) C1B 0.032(2) 0.056(3) 0.035(2) -0.012(2) -0.003(2) -0.001(2) C2B 0.048(3) 0.060(3) 0.050(3) -0.013(2) 0.001(2) 0.004(2) C3B 0.052(3) 0.056(3) 0.071(4) -0.027(3) 0.007(3) -0.017(3) C4B 0.036(3) 0.058(3) 0.047(3) -0.024(2) 0.002(2) -0.011(2) C5B 0.035(3) 0.077(3) 0.047(3) -0.029(3) -0.001(2) -0.014(2) C6B 0.037(3) 0.068(3) 0.037(3) -0.009(3) -0.008(2) -0.004(2) C7B 0.150(6) 0.089(5) 0.050(4) 0.005(4) 0.003(4) 0.031(4) C8B 0.159(7) 0.065(4) 0.071(4) -0.002(4) 0.004(4) 0.035(4) C9B 0.041(3) 0.055(3) 0.046(3) -0.013(3) -0.008(2) 0.002(2) C10B 0.036(2) 0.059(3) 0.056(3) -0.028(2) -0.009(2) 0.000(2) C11B 0.032(2) 0.049(3) 0.051(3) -0.022(2) -0.003(2) -0.004(2) C12B 0.033(3) 0.053(3) 0.050(3) -0.016(2) 0.005(2) -0.006(2) C13B 0.040(3) 0.041(3) 0.038(3) -0.009(2) -0.004(2) 0.001(2) C14B 0.032(2) 0.035(2) 0.037(2) -0.010(2) -0.011(2) -0.0004(19) C15B 0.037(2) 0.037(2) 0.039(3) -0.012(2) -0.009(2) -0.0043(19) C16B 0.028(2) 0.041(2) 0.045(3) -0.011(2) -0.0117(19) -0.0060(19) C17B 0.056(3) 0.042(3) 0.057(3) -0.008(2) -0.006(2) -0.012(2) C18B 0.058(3) 0.056(3) 0.048(3) 0.001(2) -0.002(2) -0.019(2) C19B 0.031(2) 0.058(3) 0.029(2) -0.007(2) -0.0064(18) -0.010(2) C20B 0.030(2) 0.077(3) 0.037(3) -0.020(2) -0.006(2) -0.005(2) C21B 0.045(3) 0.148(5) 0.045(3) -0.041(3) -0.002(2) -0.019(3) C22B 0.042(3) 0.107(4) 0.096(4) -0.065(4) 0.018(3) -0.029(3) C23B 0.040(3) 0.117(4) 0.070(4) -0.053(3) 0.004(3) -0.023(3) C24B 0.063(3) 0.098(4) 0.091(4) -0.056(4) -0.039(3) 0.032(3) C25B 0.052(3) 0.055(3) 0.064(3) -0.028(3) -0.002(2) -0.015(2) C26B 0.044(3) 0.070(3) 0.037(3) -0.004(2) -0.010(2) -0.011(2) C27B 0.044(3) 0.113(5) 0.091(4) -0.058(4) -0.021(3) 0.011(3) C28B 0.060(3) 0.115(5) 0.054(3) -0.033(3) 0.022(3) -0.042(3) Cl1A 0.0974(10) 0.0478(7) 0.0539(8) -0.0061(6) -0.0194(7) 0.0022(7) Cl2A 0.0829(9) 0.0782(9) 0.0506(8) -0.0217(7) -0.0115(7) -0.0085(7) C1C 0.048(3) 0.042(3) 0.045(3) -0.011(2) -0.007(2) -0.006(2) O1A 0.069(2) 0.071(2) 0.069(2) -0.025(2) -0.0101(19) -0.0031(19) N1A 0.0328(19) 0.0329(19) 0.035(2) -0.0083(16) -0.0063(16) -0.0012(15) N2A 0.040(2) 0.0364(19) 0.039(2) -0.0073(16) -0.0089(16) -0.0031(17) N3A 0.038(2) 0.043(2) 0.034(2) -0.0067(18) -0.0046(16) -0.0085(16) N4A 0.033(2) 0.0378(19) 0.037(2) -0.0122(16) -0.0057(16) -0.0027(16) C1A 0.028(2) 0.034(2) 0.035(2) -0.004(2) -0.0017(19) -0.0056(18) C2A 0.034(2) 0.036(2) 0.037(3) -0.006(2) -0.007(2) 0.0010(19) C3A 0.033(2) 0.044(3) 0.042(3) -0.014(2) -0.002(2) -0.003(2) C4A 0.032(2) 0.042(3) 0.032(2) -0.009(2) -0.0035(19) -0.010(2) C5A 0.033(2) 0.040(2) 0.036(2) -0.009(2) -0.0047(19) -0.0075(19) C6A 0.039(2) 0.036(2) 0.028(2) -0.0021(19) -0.0093(19) -0.009(2) C7A 0.047(3) 0.034(3) 0.052(3) -0.008(2) -0.006(2) -0.006(2) C8A 0.046(3) 0.043(3) 0.054(3) -0.012(2) -0.005(2) 0.007(2) C9A 0.030(2) 0.052(3) 0.030(2) -0.006(2) -0.0095(19) -0.001(2) C10A 0.029(2) 0.062(3) 0.036(3) -0.008(2) -0.0076(19) -0.004(2) C11A 0.027(2) 0.055(3) 0.034(2) -0.015(2) -0.0067(19) -0.007(2) C12A 0.034(2) 0.058(3) 0.044(3) -0.016(2) -0.008(2) -0.014(2) C13A 0.034(2) 0.048(3) 0.045(3) -0.004(2) -0.004(2) -0.012(2) C14A 0.029(2) 0.053(3) 0.034(2) -0.007(2) -0.0050(19) -0.007(2) C15A 0.032(2) 0.057(3) 0.030(2) -0.001(2) -0.0056(19) -0.010(2) C16A 0.032(2) 0.047(3) 0.030(2) -0.005(2) -0.0067(19) -0.005(2) C17A 0.039(3) 0.042(3) 0.045(3) -0.013(2) -0.006(2) 0.005(2) C18A 0.037(3) 0.036(2) 0.045(3) -0.008(2) -0.006(2) -0.004(2) C19A 0.031(2) 0.040(2) 0.028(2) -0.0064(19) -0.0062(18) -0.0047(19) C20A 0.034(2) 0.036(2) 0.032(2) -0.0028(19) -0.0106(19) -0.0043(18) C21A 0.044(3) 0.050(3) 0.044(3) -0.009(2) -0.005(2) -0.015(2) C22A 0.051(3) 0.052(3) 0.050(3) -0.002(2) -0.005(2) -0.020(2) C23A 0.063(3) 0.099(4) 0.039(3) -0.016(3) -0.013(2) -0.038(3) C24A 0.039(3) 0.080(4) 0.054(3) 0.003(3) -0.010(2) 0.000(2) C25A 0.051(3) 0.071(3) 0.042(3) 0.002(2) -0.013(2) -0.025(2) C26A 0.038(3) 0.096(4) 0.040(3) -0.020(3) 0.000(2) -0.012(3) C27A 0.044(3) 0.049(3) 0.042(3) -0.009(2) -0.007(2) 0.004(2) C28A 0.037(2) 0.057(3) 0.045(3) -0.013(2) -0.004(2) -0.013(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 N1 C1 1.383(5) . ? N1 C4 1.384(4) . ? N1 H1A 0.8800 . ? O1 C21 1.448(5) . ? O1 H1 0.8400 . ? O1 H21H 0.5128 . ? O1' C21 1.414(8) . ? O1' H1' 0.8400 . ? O1' H21F 0.4689 . ? N2 C6 1.365(5) . ? N2 C9 1.375(5) . ? N2 H2B 0.8800 . ? N3 C11 1.375(4) . ? N3 C14 1.384(5) . ? N3 H3B 0.8800 . ? N4 C19 1.374(5) . ? N4 C16 1.375(4) . ? N4 H4A 0.8800 . ? C1 C2 1.373(5) . ? C1 C20 1.511(5) . ? C2 C3 1.409(6) . ? C2 H2A 0.9500 . ? C3 C4 1.350(5) . ? C3 H3A 0.9500 . ? C4 C5 1.511(5) . ? C5 C6 1.503(5) . ? C5 C21 1.509(6) . ? C5 C22 1.549(6) . ? C6 C7 1.356(5) . ? C7 C8 1.412(6) . ? C7 H7A 0.9500 . ? C8 C9 1.353(5) . ? C8 H8A 0.9500 . ? C9 C10 1.496(5) . ? C10 C11 1.521(5) . ? C10 C24 1.531(5) . ? C10 C23 1.538(5) . ? C11 C12 1.353(5) . ? C12 C13 1.431(5) . ? C12 H12B 0.9500 . ? C13 C14 1.361(5) . ? C13 H13B 0.9500 . ? C14 C15 1.515(5) . ? C15 C16 1.501(6) . ? C15 C26 1.540(5) . ? C15 C25 1.544(5) . ? C16 C17 1.373(5) . ? C17 C18 1.410(6) . ? C17 H17B 0.9500 . ? C18 C19 1.376(5) . ? C18 H18B 0.9500 . ? C19 C20 1.500(6) . ? C20 C28 1.535(6) . ? C20 C27 1.559(6) . ? C21 H21F 0.9599 . ? C21 H21G 0.9599 . ? C21 H21H 0.9600 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O1B C21B 1.417(4) . ? O1B H1B 0.8400 . ? O1BA C23B 1.420(6) . ? O1BA H1BA 0.8400 . ? N1B C4B 1.372(5) . ? N1B C1B 1.372(5) . ? N1B H1BN 0.8800 . ? N2B C6B 1.367(5) . ? N2B C9B 1.369(5) . ? N2B H2BN 0.8800 . ? N3B C14B 1.371(4) . ? N3B C11B 1.378(4) . ? N3B H3BN 0.8800 . ? N4B C19B 1.365(4) . ? N4B C16B 1.380(4) . ? N4B H4BN 0.8800 . ? C1B C2B 1.365(6) . ? C1B C20B 1.510(4) . ? C2B C3B 1.426(6) . ? C2B H2BB 0.9500 . ? C3B C4B 1.350(6) . ? C3B H3BB 0.9500 . ? C4B C5B 1.513(6) . ? C5B C6B 1.501(6) . ? C5B C22B 1.526(4) . ? C5B C21B 1.542(5) . ? C6B C7B 1.368(7) . ? C7B C8B 1.431(7) . ? C7B H7BA 0.9500 . ? C8B C9B 1.339(7) . ? C8B H8BA 0.9500 . ? C9B C10B 1.501(6) . ? C10B C11B 1.521(4) . ? C10B C24B 1.531(5) . ? C10B C23B 1.538(4) . ? C11B C12B 1.351(6) . ? C12B C13B 1.413(5) . ? C12B H12C 0.9500 . ? C13B C14B 1.353(5) . ? C13B H13C 0.9500 . ? C14B C15B 1.522(5) . ? C15B C16B 1.510(5) . ? C15B C26B 1.524(6) . ? C15B C25B 1.537(5) . ? C16B C17B 1.354(5) . ? C17B C18B 1.433(6) . ? C17B H17C 0.9500 . ? C18B C19B 1.350(5) . ? C18B H18C 0.9500 . ? C19B C20B 1.498(5) . ? C20B C27B 1.543(6) . ? C20B C28B 1.545(6) . ? C21B H21C 0.9600 . ? C21B H21D 0.9601 . ? C21B H21E 0.9600 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23B H23G 0.9600 . ? C23B H23H 0.9600 . ? C23B H23I 0.9599 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? Cl1A C1C 1.765(4) . ? Cl2A C1C 1.746(4) . ? C1C H1CA 0.9900 . ? C1C H1CB 0.9900 . ? O1A C21A 1.406(4) . ? O1A H1A1 0.8400 . ? N1A C1A 1.370(5) . ? N1A C4A 1.377(5) . ? N1A H1AA 0.8800 . ? N2A C6A 1.379(4) . ? N2A C9A 1.381(5) . ? N2A H2AB 0.8800 . ? N3A C14A 1.365(5) . ? N3A C11A 1.379(5) . ? N3A H3AB 0.8800 . ? N4A C16A 1.374(5) . ? N4A C19A 1.381(4) . ? N4A H4AA 0.8800 . ? C1A C2A 1.361(5) . ? C1A C20A 1.511(5) . ? C2A C3A 1.414(5) . ? C2A H2AA 0.9500 . ? C3A C4A 1.359(5) . ? C3A H3AA 0.9500 . ? C4A C5A 1.504(5) . ? C5A C6A 1.514(5) . ? C5A C21A 1.534(5) . ? C5A C22A 1.540(5) . ? C6A C7A 1.358(5) . ? C7A C8A 1.414(5) . ? C7A H7AA 0.9500 . ? C8A C9A 1.352(5) . ? C8A H8AA 0.9500 . ? C9A C10A 1.513(5) . ? C10A C11A 1.507(6) . ? C10A C24A 1.540(6) . ? C10A C23A 1.543(5) . ? C11A C12A 1.359(5) . ? C12A C13A 1.413(6) . ? C12A H12A 0.9500 . ? C13A C14A 1.365(5) . ? C13A H13A 0.9500 . ? C14A C15A 1.515(5) . ? C15A C16A 1.514(5) . ? C15A C25A 1.527(6) . ? C15A C26A 1.543(6) . ? C16A C17A 1.350(5) . ? C17A C18A 1.426(5) . ? C17A H17A 0.9500 . ? C18A C19A 1.363(5) . ? C18A H18A 0.9500 . ? C19A C20A 1.512(5) . ? C20A C27A 1.526(5) . ? C20A C28A 1.551(5) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? C22A H22G 0.9800 . ? C22A H22H 0.9800 . ? C22A H22I 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A H24G 0.9800 . ? C24A H24H 0.9800 . ? C24A H24I 0.9800 . ? C25A H25G 0.9800 . ? C25A H25H 0.9800 . ? C25A H25I 0.9800 . ? C26A H26G 0.9800 . ? C26A H26H 0.9800 . ? C26A H26I 0.9800 . ? C27A H27G 0.9800 . ? C27A H27H 0.9800 . ? C27A H27I 0.9800 . ? C28A H28G 0.9800 . ? C28A H28H 0.9800 . ? C28A H28I 0.9800 . ? 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 C4 109.7(3) . . ? C1 N1 H1A 125.1 . . ? C4 N1 H1A 125.1 . . ? C21 O1 H1 109.5 . . ? C21 O1' H1' 109.5 . . ? C6 N2 C9 111.4(3) . . ? C6 N2 H2B 124.3 . . ? C9 N2 H2B 124.3 . . ? C11 N3 C14 110.4(3) . . ? C11 N3 H3B 124.8 . . ? C14 N3 H3B 124.8 . . ? C19 N4 C16 111.4(3) . . ? C19 N4 H4A 124.3 . . ? C16 N4 H4A 124.3 . . ? C2 C1 N1 106.6(3) . . ? C2 C1 C20 130.6(4) . . ? N1 C1 C20 122.5(3) . . ? C1 C2 C3 107.8(4) . . ? C1 C2 H2A 126.1 . . ? C3 C2 H2A 126.1 . . ? C4 C3 C2 108.7(4) . . ? C4 C3 H3A 125.6 . . ? C2 C3 H3A 125.6 . . ? C3 C4 N1 107.1(3) . . ? C3 C4 C5 131.1(3) . . ? N1 C4 C5 121.8(3) . . ? C6 C5 C21 110.6(4) . . ? C6 C5 C4 112.0(3) . . ? C21 C5 C4 108.4(3) . . ? C6 C5 C22 109.6(3) . . ? C21 C5 C22 106.9(3) . . ? C4 C5 C22 109.3(3) . . ? C7 C6 N2 106.2(4) . . ? C7 C6 C5 132.6(4) . . ? N2 C6 C5 121.0(4) . . ? C6 C7 C8 108.0(4) . . ? C6 C7 H7A 126.0 . . ? C8 C7 H7A 126.0 . . ? C9 C8 C7 108.6(4) . . ? C9 C8 H8A 125.7 . . ? C7 C8 H8A 125.7 . . ? C8 C9 N2 105.7(4) . . ? C8 C9 C10 132.6(4) . . ? N2 C9 C10 121.6(3) . . ? C9 C10 C11 111.8(3) . . ? C9 C10 C24 109.3(3) . . ? C11 C10 C24 109.1(3) . . ? C9 C10 C23 109.8(3) . . ? C11 C10 C23 109.1(3) . . ? C24 C10 C23 107.6(3) . . ? C12 C11 N3 107.1(3) . . ? C12 C11 C10 130.5(4) . . ? N3 C11 C10 122.3(3) . . ? C11 C12 C13 108.0(4) . . ? C11 C12 H12B 126.0 . . ? C13 C12 H12B 126.0 . . ? C14 C13 C12 107.8(4) . . ? C14 C13 H13B 126.1 . . ? C12 C13 H13B 126.1 . . ? C13 C14 N3 106.6(3) . . ? C13 C14 C15 131.2(4) . . ? N3 C14 C15 122.1(4) . . ? C16 C15 C14 111.5(3) . . ? C16 C15 C26 110.0(3) . . ? C14 C15 C26 109.3(3) . . ? C16 C15 C25 109.5(3) . . ? C14 C15 C25 108.4(3) . . ? C26 C15 C25 108.1(3) . . ? C17 C16 N4 106.2(4) . . ? C17 C16 C15 131.6(4) . . ? N4 C16 C15 122.2(3) . . ? C16 C17 C18 108.2(4) . . ? C16 C17 H17B 125.9 . . ? C18 C17 H17B 125.9 . . ? C19 C18 C17 108.2(4) . . ? C19 C18 H18B 125.9 . . ? C17 C18 H18B 125.9 . . ? N4 C19 C18 106.0(4) . . ? N4 C19 C20 122.6(4) . . ? C18 C19 C20 131.2(4) . . ? C19 C20 C1 112.5(3) . . ? C19 C20 C28 109.5(4) . . ? C1 C20 C28 108.6(3) . . ? C19 C20 C27 108.8(3) . . ? C1 C20 C27 108.2(4) . . ? C28 C20 C27 109.1(4) . . ? O1' C21 O1 115.0(10) . . ? O1' C21 C5 114.4(6) . . ? O1 C21 C5 110.8(5) . . ? O1 C21 H21F 115.3 . . ? C5 C21 H21F 109.7 . . ? O1' C21 H21G 104.2 . . ? O1 C21 H21G 102.3 . . ? C5 C21 H21G 108.9 . . ? H21F C21 H21G 109.5 . . ? O1' C21 H21H 109.8 . . ? C5 C21 H21H 109.8 . . ? H21F C21 H21H 109.5 . . ? H21G C21 H21H 109.5 . . ? C5 C22 H22A 109.5 . . ? C5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C10 C24 H24A 109.5 . . ? C10 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C10 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C15 C25 H25A 109.5 . . ? C15 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C15 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C15 C26 H26A 109.5 . . ? C15 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C15 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C20 C28 H28A 109.5 . . ? C20 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C20 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C21B O1B H1B 109.5 . . ? H1B O1B H21E 108.3 . . ? C23B O1BA H1BA 109.5 . . ? H1BA O1BA H23I 113.3 . . ? C4B N1B C1B 111.1(3) . . ? C4B N1B H1BN 124.5 . . ? C1B N1B H1BN 124.5 . . ? C6B N2B C9B 111.9(4) . . ? C6B N2B H2BN 124.0 . . ? C9B N2B H2BN 124.0 . . ? C14B N3B C11B 110.3(2) . . ? C14B N3B H3BN 124.9 . . ? C11B N3B H3BN 124.9 . . ? C19B N4B C16B 111.0(2) . . ? C19B N4B H4BN 124.5 . . ? C16B N4B H4BN 124.5 . . ? C2B C1B N1B 106.3(3) . . ? C2B C1B C20B 132.5(4) . . ? N1B C1B C20B 121.0(3) . . ? C1B C2B C3B 107.6(4) . . ? C1B C2B H2BB 126.2 . . ? C3B C2B H2BB 126.2 . . ? C4B C3B C2B 108.3(4) . . ? C4B C3B H3BB 125.9 . . ? C2B C3B H3BB 125.9 . . ? C3B C4B N1B 106.7(4) . . ? C3B C4B C5B 131.9(4) . . ? N1B C4B C5B 121.3(4) . . ? C6B C5B C4B 109.7(3) . . ? C6B C5B C22B 110.3(3) . . ? C4B C5B C22B 109.8(3) . . ? C6B C5B C21B 107.6(3) . . ? C4B C5B C21B 110.3(3) . . ? C22B C5B C21B 109.1(3) . . ? N2B C6B C7B 105.6(4) . . ? N2B C6B C5B 123.3(4) . . ? C7B C6B C5B 130.7(5) . . ? C6B C7B C8B 107.4(5) . . ? C6B C7B H7BA 126.3 . . ? C8B C7B H7BA 126.3 . . ? C9B C8B C7B 108.6(5) . . ? C9B C8B H8BA 125.7 . . ? C7B C8B H8BA 125.7 . . ? C8B C9B N2B 106.1(4) . . ? C8B C9B C10B 131.0(5) . . ? N2B C9B C10B 122.6(4) . . ? C9B C10B C11B 111.3(3) . . ? C9B C10B C24B 109.2(3) . . ? C11B C10B C24B 110.1(2) . . ? C9B C10B C23B 110.5(3) . . ? C11B C10B C23B 108.2(3) . . ? C24B C10B C23B 107.5(3) . . ? C12B C11B N3B 106.4(3) . . ? C12B C11B C10B 131.6(3) . . ? N3B C11B C10B 121.9(3) . . ? C11B C12B C13B 108.6(4) . . ? C11B C12B H12C 125.7 . . ? C13B C12B H12C 125.7 . . ? C14B C13B C12B 107.7(4) . . ? C14B C13B H13C 126.1 . . ? C12B C13B H13C 126.1 . . ? C13B C14B N3B 107.1(3) . . ? C13B C14B C15B 130.2(4) . . ? N3B C14B C15B 122.6(3) . . ? C16B C15B C14B 111.5(3) . . ? C16B C15B C26B 109.9(3) . . ? C14B C15B C26B 109.0(3) . . ? C16B C15B C25B 108.9(3) . . ? C14B C15B C25B 108.6(3) . . ? C26B C15B C25B 108.8(3) . . ? C17B C16B N4B 106.6(3) . . ? C17B C16B C15B 130.9(4) . . ? N4B C16B C15B 122.4(3) . . ? C16B C17B C18B 107.5(4) . . ? C16B C17B H17C 126.3 . . ? C18B C17B H17C 126.3 . . ? C19B C18B C17B 108.2(4) . . ? C19B C18B H18C 125.9 . . ? C17B C18B H18C 125.9 . . ? C18B C19B N4B 106.7(3) . . ? C18B C19B C20B 130.4(4) . . ? N4B C19B C20B 122.8(3) . . ? C19B C20B C1B 111.5(3) . . ? C19B C20B C27B 110.2(3) . . ? C1B C20B C27B 108.6(3) . . ? C19B C20B C28B 109.2(4) . . ? C1B C20B C28B 108.8(3) . . ? C27B C20B C28B 108.4(4) . . ? O1B C21B C5B 114.4(4) . . ? O1B C21B H21C 107.8 . . ? C5B C21B H21C 109.3 . . ? O1B C21B H21D 106.6 . . ? C5B C21B H21D 109.2 . . ? H21C C21B H21D 109.5 . . ? C5B C21B H21E 109.9 . . ? H21C C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C5B C22B H22D 109.5 . . ? C5B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C5B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? O1BA C23B C10B 112.6(4) . . ? O1BA C23B H23G 107.1 . . ? C10B C23B H23G 109.5 . . ? O1BA C23B H23H 109.1 . . ? C10B C23B H23H 109.0 . . ? H23G C23B H23H 109.5 . . ? C10B C23B H23I 109.9 . . ? H23G C23B H23I 109.5 . . ? H23H C23B H23I 109.5 . . ? C10B C24B H24D 109.5 . . ? C10B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C10B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C15B C25B H25D 109.5 . . ? C15B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C15B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C15B C26B H26D 109.5 . . ? C15B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C15B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C20B C27B H27D 109.5 . . ? C20B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C20B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C20B C28B H28D 109.5 . . ? C20B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C20B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? Cl2A C1C Cl1A 111.9(2) . . ? Cl2A C1C H1CA 109.2 . . ? Cl1A C1C H1CA 109.2 . . ? Cl2A C1C H1CB 109.2 . . ? Cl1A C1C H1CB 109.2 . . ? H1CA C1C H1CB 107.9 . . ? C21A O1A H1A1 109.5 . . ? C1A N1A C4A 111.1(3) . . ? C1A N1A H1AA 124.4 . . ? C4A N1A H1AA 124.4 . . ? C6A N2A C9A 110.6(3) . . ? C6A N2A H2AB 124.7 . . ? C9A N2A H2AB 124.7 . . ? C14A N3A C11A 111.1(3) . . ? C14A N3A H3AB 124.5 . . ? C11A N3A H3AB 124.5 . . ? C16A N4A C19A 111.0(3) . . ? C16A N4A H4AA 124.5 . . ? C19A N4A H4AA 124.5 . . ? C2A C1A N1A 106.6(3) . . ? C2A C1A C20A 132.7(4) . . ? N1A C1A C20A 120.6(3) . . ? C1A C2A C3A 107.6(4) . . ? C1A C2A H2AA 126.2 . . ? C3A C2A H2AA 126.2 . . ? C4A C3A C2A 108.9(3) . . ? C4A C3A H3AA 125.6 . . ? C2A C3A H3AA 125.6 . . ? C3A C4A N1A 105.7(4) . . ? C3A C4A C5A 134.0(4) . . ? N1A C4A C5A 120.0(3) . . ? C4A C5A C6A 110.4(3) . . ? C4A C5A C21A 111.0(3) . . ? C6A C5A C21A 111.0(3) . . ? C4A C5A C22A 109.4(3) . . ? C6A C5A C22A 109.2(3) . . ? C21A C5A C22A 105.8(3) . . ? C7A C6A N2A 106.4(3) . . ? C7A C6A C5A 132.5(3) . . ? N2A C6A C5A 121.0(3) . . ? C6A C7A C8A 108.0(3) . . ? C6A C7A H7AA 126.0 . . ? C8A C7A H7AA 126.0 . . ? C9A C8A C7A 108.8(4) . . ? C9A C8A H8AA 125.6 . . ? C7A C8A H8AA 125.6 . . ? C8A C9A N2A 106.2(3) . . ? C8A C9A C10A 133.0(4) . . ? N2A C9A C10A 120.7(4) . . ? C11A C10A C9A 110.5(3) . . ? C11A C10A C24A 108.8(3) . . ? C9A C10A C24A 108.7(4) . . ? C11A C10A C23A 110.1(4) . . ? C9A C10A C23A 110.2(3) . . ? C24A C10A C23A 108.6(4) . . ? C12A C11A N3A 106.2(4) . . ? C12A C11A C10A 132.9(4) . . ? N3A C11A C10A 120.8(4) . . ? C11A C12A C13A 108.2(3) . . ? C11A C12A H12A 125.9 . . ? C13A C12A H12A 125.9 . . ? C14A C13A C12A 108.1(4) . . ? C14A C13A H13A 125.9 . . ? C12A C13A H13A 125.9 . . ? N3A C14A C13A 106.4(3) . . ? N3A C14A C15A 121.2(3) . . ? C13A C14A C15A 132.5(4) . . ? C16A C15A C14A 109.6(3) . . ? C16A C15A C25A 111.4(3) . . ? C14A C15A C25A 109.5(3) . . ? C16A C15A C26A 108.3(3) . . ? C14A C15A C26A 109.0(3) . . ? C25A C15A C26A 109.0(3) . . ? C17A C16A N4A 106.4(3) . . ? C17A C16A C15A 132.8(4) . . ? N4A C16A C15A 120.8(3) . . ? C16A C17A C18A 108.8(3) . . ? C16A C17A H17A 125.6 . . ? C18A C17A H17A 125.6 . . ? C19A C18A C17A 107.5(3) . . ? C19A C18A H18A 126.3 . . ? C17A C18A H18A 126.3 . . ? C18A C19A N4A 106.4(3) . . ? C18A C19A C20A 132.4(3) . . ? N4A C19A C20A 121.0(3) . . ? C1A C20A C19A 109.9(3) . . ? C1A C20A C27A 109.9(3) . . ? C19A C20A C27A 110.8(3) . . ? C1A C20A C28A 108.9(3) . . ? C19A C20A C28A 108.8(3) . . ? C27A C20A C28A 108.4(3) . . ? O1A C21A C5A 113.0(3) . . ? O1A C21A H21A 109.0 . . ? C5A C21A H21A 109.0 . . ? O1A C21A H21B 109.0 . . ? C5A C21A H21B 109.0 . . ? H21A C21A H21B 107.8 . . ? C5A C22A H22G 109.5 . . ? C5A C22A H22H 109.5 . . ? H22G C22A H22H 109.5 . . ? C5A C22A H22I 109.5 . . ? H22G C22A H22I 109.5 . . ? H22H C22A H22I 109.5 . . ? C10A C23A H23D 109.5 . . ? C10A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C10A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C10A C24A H24G 109.5 . . ? C10A C24A H24H 109.5 . . ? H24G C24A H24H 109.5 . . ? C10A C24A H24I 109.5 . . ? H24G C24A H24I 109.5 . . ? H24H C24A H24I 109.5 . . ? C15A C25A H25G 109.5 . . ? C15A C25A H25H 109.5 . . ? H25G C25A H25H 109.5 . . ? C15A C25A H25I 109.5 . . ? H25G C25A H25I 109.5 . . ? H25H C25A H25I 109.5 . . ? C15A C26A H26G 109.5 . . ? C15A C26A H26H 109.5 . . ? H26G C26A H26H 109.5 . . ? C15A C26A H26I 109.5 . . ? H26G C26A H26I 109.5 . . ? H26H C26A H26I 109.5 . . ? C20A C27A H27G 109.5 . . ? C20A C27A H27H 109.5 . . ? H27G C27A H27H 109.5 . . ? C20A C27A H27I 109.5 . . ? H27G C27A H27I 109.5 . . ? H27H C27A H27I 109.5 . . ? C20A C28A H28G 109.5 . . ? C20A C28A H28H 109.5 . . ? H28G C28A H28H 109.5 . . ? C20A C28A H28I 109.5 . . ? H28G C28A H28I 109.5 . . ? H28H C28A H28I 109.5 . . ? 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 C4 N1 C1 C2 0.3(4) . . . . ? C4 N1 C1 C20 174.2(4) . . . . ? N1 C1 C2 C3 -0.1(5) . . . . ? C20 C1 C2 C3 -173.4(4) . . . . ? C1 C2 C3 C4 -0.1(5) . . . . ? C2 C3 C4 N1 0.3(5) . . . . ? C2 C3 C4 C5 177.6(4) . . . . ? C1 N1 C4 C3 -0.4(4) . . . . ? C1 N1 C4 C5 -178.0(4) . . . . ? C3 C4 C5 C6 148.2(4) . . . . ? N1 C4 C5 C6 -34.9(5) . . . . ? C3 C4 C5 C21 -89.6(5) . . . . ? N1 C4 C5 C21 87.3(5) . . . . ? C3 C4 C5 C22 26.5(6) . . . . ? N1 C4 C5 C22 -156.5(4) . . . . ? C9 N2 C6 C7 0.0(4) . . . . ? C9 N2 C6 C5 -175.9(3) . . . . ? C21 C5 C6 C7 3.1(6) . . . . ? C4 C5 C6 C7 124.0(5) . . . . ? C22 C5 C6 C7 -114.5(5) . . . . ? C21 C5 C6 N2 177.7(3) . . . . ? C4 C5 C6 N2 -61.3(5) . . . . ? C22 C5 C6 N2 60.2(5) . . . . ? N2 C6 C7 C8 0.3(4) . . . . ? C5 C6 C7 C8 175.5(4) . . . . ? C6 C7 C8 C9 -0.5(5) . . . . ? C7 C8 C9 N2 0.4(4) . . . . ? C7 C8 C9 C10 -176.8(4) . . . . ? C6 N2 C9 C8 -0.2(4) . . . . ? C6 N2 C9 C10 177.3(3) . . . . ? C8 C9 C10 C11 -127.8(4) . . . . ? N2 C9 C10 C11 55.4(4) . . . . ? C8 C9 C10 C24 -6.9(6) . . . . ? N2 C9 C10 C24 176.3(3) . . . . ? C8 C9 C10 C23 110.9(5) . . . . ? N2 C9 C10 C23 -65.9(4) . . . . ? C14 N3 C11 C12 -0.7(4) . . . . ? C14 N3 C11 C10 175.9(3) . . . . ? C9 C10 C11 C12 -139.8(4) . . . . ? C24 C10 C11 C12 99.2(5) . . . . ? C23 C10 C11 C12 -18.1(5) . . . . ? C9 C10 C11 N3 44.5(5) . . . . ? C24 C10 C11 N3 -76.5(4) . . . . ? C23 C10 C11 N3 166.2(3) . . . . ? N3 C11 C12 C13 0.3(4) . . . . ? C10 C11 C12 C13 -175.8(4) . . . . ? C11 C12 C13 C14 0.1(4) . . . . ? C12 C13 C14 N3 -0.5(4) . . . . ? C12 C13 C14 C15 175.7(4) . . . . ? C11 N3 C14 C13 0.7(4) . . . . ? C11 N3 C14 C15 -175.9(3) . . . . ? C13 C14 C15 C16 141.3(4) . . . . ? N3 C14 C15 C16 -43.1(5) . . . . ? C13 C14 C15 C26 19.5(6) . . . . ? N3 C14 C15 C26 -164.8(3) . . . . ? C13 C14 C15 C25 -98.1(5) . . . . ? N3 C14 C15 C25 77.6(5) . . . . ? C19 N4 C16 C17 -0.4(4) . . . . ? C19 N4 C16 C15 -177.7(3) . . . . ? C14 C15 C16 C17 129.8(4) . . . . ? C26 C15 C16 C17 -108.8(5) . . . . ? C25 C15 C16 C17 9.8(6) . . . . ? C14 C15 C16 N4 -53.6(5) . . . . ? C26 C15 C16 N4 67.8(4) . . . . ? C25 C15 C16 N4 -173.6(3) . . . . ? N4 C16 C17 C18 0.4(4) . . . . ? C15 C16 C17 C18 177.3(4) . . . . ? C16 C17 C18 C19 -0.2(5) . . . . ? C16 N4 C19 C18 0.3(4) . . . . ? C16 N4 C19 C20 176.2(3) . . . . ? C17 C18 C19 N4 0.0(4) . . . . ? C17 C18 C19 C20 -175.5(4) . . . . ? N4 C19 C20 C1 53.2(5) . . . . ? C18 C19 C20 C1 -131.9(4) . . . . ? N4 C19 C20 C28 174.1(4) . . . . ? C18 C19 C20 C28 -11.0(6) . . . . ? N4 C19 C20 C27 -66.7(5) . . . . ? C18 C19 C20 C27 108.2(5) . . . . ? C2 C1 C20 C19 -144.4(4) . . . . ? N1 C1 C20 C19 43.2(5) . . . . ? C2 C1 C20 C28 94.2(6) . . . . ? N1 C1 C20 C28 -78.2(5) . . . . ? C2 C1 C20 C27 -24.1(6) . . . . ? N1 C1 C20 C27 163.5(4) . . . . ? C6 C5 C21 O1' 64.3(12) . . . . ? C4 C5 C21 O1' -58.7(12) . . . . ? C22 C5 C21 O1' -176.4(11) . . . . ? C6 C5 C21 O1 -67.7(5) . . . . ? C4 C5 C21 O1 169.3(4) . . . . ? C22 C5 C21 O1 51.6(5) . . . . ? C4B N1B C1B C2B -1.6(5) . . . . ? C4B N1B C1B C20B -177.3(3) . . . . ? N1B C1B C2B C3B 0.9(5) . . . . ? C20B C1B C2B C3B 176.0(4) . . . . ? C1B C2B C3B C4B 0.0(5) . . . . ? C2B C3B C4B N1B -1.0(5) . . . . ? C2B C3B C4B C5B -176.7(4) . . . . ? C1B N1B C4B C3B 1.6(5) . . . . ? C1B N1B C4B C5B 177.9(3) . . . . ? C3B C4B C5B C6B -148.4(5) . . . . ? N1B C4B C5B C6B 36.4(5) . . . . ? C3B C4B C5B C22B -27.0(6) . . . . ? N1B C4B C5B C22B 157.8(3) . . . . ? C3B C4B C5B C21B 93.2(6) . . . . ? N1B C4B C5B C21B -82.0(4) . . . . ? C9B N2B C6B C7B -4.7(5) . . . . ? C9B N2B C6B C5B -178.3(3) . . . . ? C4B C5B C6B N2B 74.0(5) . . . . ? C22B C5B C6B N2B -47.1(5) . . . . ? C21B C5B C6B N2B -166.0(3) . . . . ? C4B C5B C6B C7B -97.9(6) . . . . ? C22B C5B C6B C7B 141.0(5) . . . . ? C21B C5B C6B C7B 22.1(6) . . . . ? N2B C6B C7B C8B 1.5(7) . . . . ? C5B C6B C7B C8B 174.5(5) . . . . ? C6B C7B C8B C9B 2.1(8) . . . . ? C7B C8B C9B N2B -4.8(7) . . . . ? C7B C8B C9B C10B -179.3(5) . . . . ? C6B N2B C9B C8B 6.0(5) . . . . ? C6B N2B C9B C10B -178.9(4) . . . . ? C8B C9B C10B C11B 104.7(6) . . . . ? N2B C9B C10B C11B -69.1(4) . . . . ? C8B C9B C10B C24B -17.1(7) . . . . ? N2B C9B C10B C24B 169.2(3) . . . . ? C8B C9B C10B C23B -135.1(6) . . . . ? N2B C9B C10B C23B 51.1(5) . . . . ? C14B N3B C11B C12B -0.9(4) . . . . ? C14B N3B C11B C10B -178.7(3) . . . . ? C9B C10B C11B C12B 148.7(4) . . . . ? C24B C10B C11B C12B -90.1(5) . . . . ? C23B C10B C11B C12B 27.1(5) . . . . ? C9B C10B C11B N3B -34.1(4) . . . . ? C24B C10B C11B N3B 87.1(4) . . . . ? C23B C10B C11B N3B -155.7(3) . . . . ? N3B C11B C12B C13B 0.2(4) . . . . ? C10B C11B C12B C13B 177.7(3) . . . . ? C11B C12B C13B C14B 0.6(4) . . . . ? C12B C13B C14B N3B -1.1(4) . . . . ? C12B C13B C14B C15B -176.0(4) . . . . ? C11B N3B C14B C13B 1.2(3) . . . . ? C11B N3B C14B C15B 176.6(3) . . . . ? C13B C14B C15B C16B -159.6(4) . . . . ? N3B C14B C15B C16B 26.2(5) . . . . ? C13B C14B C15B C26B -38.1(5) . . . . ? N3B C14B C15B C26B 147.7(3) . . . . ? C13B C14B C15B C25B 80.4(5) . . . . ? N3B C14B C15B C25B -93.8(4) . . . . ? C19B N4B C16B C17B 0.3(4) . . . . ? C19B N4B C16B C15B 176.6(3) . . . . ? C14B C15B C16B C17B -115.0(5) . . . . ? C26B C15B C16B C17B 124.0(5) . . . . ? C25B C15B C16B C17B 4.8(6) . . . . ? C14B C15B C16B N4B 69.6(4) . . . . ? C26B C15B C16B N4B -51.5(4) . . . . ? C25B C15B C16B N4B -170.6(3) . . . . ? N4B C16B C17B C18B -0.3(4) . . . . ? C15B C16B C17B C18B -176.3(4) . . . . ? C16B C17B C18B C19B 0.3(5) . . . . ? C17B C18B C19B N4B -0.1(4) . . . . ? C17B C18B C19B C20B 176.6(4) . . . . ? C16B N4B C19B C18B -0.1(4) . . . . ? C16B N4B C19B C20B -177.1(3) . . . . ? C18B C19B C20B C1B 130.6(4) . . . . ? N4B C19B C20B C1B -53.1(4) . . . . ? C18B C19B C20B C27B -108.6(5) . . . . ? N4B C19B C20B C27B 67.7(5) . . . . ? C18B C19B C20B C28B 10.4(6) . . . . ? N4B C19B C20B C28B -173.4(3) . . . . ? C2B C1B C20B C19B 137.3(4) . . . . ? N1B C1B C20B C19B -48.3(4) . . . . ? C2B C1B C20B C27B 15.6(5) . . . . ? N1B C1B C20B C27B -170.0(3) . . . . ? C2B C1B C20B C28B -102.2(4) . . . . ? N1B C1B C20B C28B 72.2(3) . . . . ? C6B C5B C21B O1B 178.9(3) . . . . ? C4B C5B C21B O1B -61.5(4) . . . . ? C22B C5B C21B O1B 59.2(4) . . . . ? C9B C10B C23B O1BA -61.3(5) . . . . ? C11B C10B C23B O1BA 60.8(4) . . . . ? C24B C10B C23B O1BA 179.6(4) . . . . ? C4A N1A C1A C2A -0.6(4) . . . . ? C4A N1A C1A C20A 176.6(3) . . . . ? N1A C1A C2A C3A 0.9(4) . . . . ? C20A C1A C2A C3A -175.8(4) . . . . ? C1A C2A C3A C4A -0.9(4) . . . . ? C2A C3A C4A N1A 0.5(4) . . . . ? C2A C3A C4A C5A 174.5(4) . . . . ? C1A N1A C4A C3A 0.0(4) . . . . ? C1A N1A C4A C5A -174.9(3) . . . . ? C3A C4A C5A C6A 137.4(4) . . . . ? N1A C4A C5A C6A -49.3(4) . . . . ? C3A C4A C5A C21A 13.9(6) . . . . ? N1A C4A C5A C21A -172.8(3) . . . . ? C3A C4A C5A C22A -102.4(5) . . . . ? N1A C4A C5A C22A 70.9(4) . . . . ? C9A N2A C6A C7A 1.4(4) . . . . ? C9A N2A C6A C5A 178.6(3) . . . . ? C4A C5A C6A C7A 114.9(5) . . . . ? C21A C5A C6A C7A -121.6(5) . . . . ? C22A C5A C6A C7A -5.4(6) . . . . ? C4A C5A C6A N2A -61.4(4) . . . . ? C21A C5A C6A N2A 62.1(5) . . . . ? C22A C5A C6A N2A 178.3(3) . . . . ? N2A C6A C7A C8A -0.6(5) . . . . ? C5A C6A C7A C8A -177.4(4) . . . . ? C6A C7A C8A C9A -0.4(5) . . . . ? C7A C8A C9A N2A 1.2(5) . . . . ? C7A C8A C9A C10A 177.5(4) . . . . ? C6A N2A C9A C8A -1.7(4) . . . . ? C6A N2A C9A C10A -178.5(3) . . . . ? C8A C9A C10A C11A -110.0(5) . . . . ? N2A C9A C10A C11A 65.9(5) . . . . ? C8A C9A C10A C24A 9.3(6) . . . . ? N2A C9A C10A C24A -174.8(3) . . . . ? C8A C9A C10A C23A 128.1(5) . . . . ? N2A C9A C10A C23A -56.0(5) . . . . ? C14A N3A C11A C12A 0.1(4) . . . . ? C14A N3A C11A C10A 177.0(3) . . . . ? C9A C10A C11A C12A -138.9(4) . . . . ? C24A C10A C11A C12A 101.9(5) . . . . ? C23A C10A C11A C12A -17.0(6) . . . . ? C9A C10A C11A N3A 45.1(5) . . . . ? C24A C10A C11A N3A -74.1(4) . . . . ? C23A C10A C11A N3A 167.1(3) . . . . ? N3A C11A C12A C13A 0.0(4) . . . . ? C10A C11A C12A C13A -176.4(4) . . . . ? C11A C12A C13A C14A -0.1(5) . . . . ? C11A N3A C14A C13A -0.2(4) . . . . ? C11A N3A C14A C15A -178.6(3) . . . . ? C12A C13A C14A N3A 0.2(4) . . . . ? C12A C13A C14A C15A 178.4(4) . . . . ? N3A C14A C15A C16A -45.7(5) . . . . ? C13A C14A C15A C16A 136.3(4) . . . . ? N3A C14A C15A C25A -168.2(3) . . . . ? C13A C14A C15A C25A 13.8(6) . . . . ? N3A C14A C15A C26A 72.6(4) . . . . ? C13A C14A C15A C26A -105.4(5) . . . . ? C19A N4A C16A C17A 0.0(4) . . . . ? C19A N4A C16A C15A 178.6(3) . . . . ? C14A C15A C16A C17A 108.0(5) . . . . ? C25A C15A C16A C17A -130.6(5) . . . . ? C26A C15A C16A C17A -10.7(6) . . . . ? C14A C15A C16A N4A -70.1(5) . . . . ? C25A C15A C16A N4A 51.2(5) . . . . ? C26A C15A C16A N4A 171.1(3) . . . . ? N4A C16A C17A C18A 0.1(5) . . . . ? C15A C16A C17A C18A -178.3(4) . . . . ? C16A C17A C18A C19A -0.1(5) . . . . ? C17A C18A C19A N4A 0.1(4) . . . . ? C17A C18A C19A C20A 174.5(4) . . . . ? C16A N4A C19A C18A -0.1(4) . . . . ? C16A N4A C19A C20A -175.2(3) . . . . ? C2A C1A C20A C19A -139.4(4) . . . . ? N1A C1A C20A C19A 44.3(4) . . . . ? C2A C1A C20A C27A -17.2(6) . . . . ? N1A C1A C20A C27A 166.5(3) . . . . ? C2A C1A C20A C28A 101.5(5) . . . . ? N1A C1A C20A C28A -74.8(4) . . . . ? C18A C19A C20A C1A -104.9(5) . . . . ? N4A C19A C20A C1A 68.8(4) . . . . ? C18A C19A C20A C27A 133.4(4) . . . . ? N4A C19A C20A C27A -52.9(4) . . . . ? C18A C19A C20A C28A 14.2(6) . . . . ? N4A C19A C20A C28A -172.1(3) . . . . ? C4A C5A C21A O1A 69.8(4) . . . . ? C6A C5A C21A O1A -53.4(5) . . . . ? C22A C5A C21A O1A -171.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.884 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.060