# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Crystalline inclusion complex of a calixarene with a nitroxide ; _publ_contact_author_name 'Gennady Ananchenko' _publ_contact_author_email GENNADY.ANANCHENKO@NRC-CNRC.GC.CA loop_ _publ_author_name G.Ananchenko E.G.Bagryanskaya A.W.Coleman D.N.Polovyanenko ; J.Ripmeester ; K.A.Udachin # Attachment 'gena50.cif' data_gena50 _database_code_depnum_ccdc_archive 'CCDC 661588' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'para hexanoyl calix(4)arene SG1' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14.63 H19.63 N0.13 O2.50 P0.13' _chemical_formula_weight 241.05 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/nnc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 15.5336(9) _cell_length_b 15.5336(9) _cell_length_c 22.658(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5467.2(7) _cell_formula_units_Z 16 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2082 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9596 _exptl_absorpt_correction_T_max 0.9728 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63264 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0117 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 29.55 _reflns_number_total 3808 _reflns_number_gt 2839 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+2.4850P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3808 _refine_ls_number_parameters 441 _refine_ls_number_restraints 781 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.2138 _refine_ls_wR_factor_gt 0.1730 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.21518(7) 0.13110(8) 0.30965(4) 0.0352(3) Uani 1 1 d U . . H1 H 0.2661 0.1482 0.3053 0.053 Uiso 1 1 calc R . . C1 C 0.20854(9) 0.08553(9) 0.36148(6) 0.0304(3) Uani 1 1 d U . . C2 C 0.12660(9) 0.08140(9) 0.38695(6) 0.0299(3) Uani 1 1 d U . . C3 C 0.11706(10) 0.03640(9) 0.43949(6) 0.0318(3) Uani 1 1 d U . . H3 H 0.0618 0.0323 0.4573 0.038 Uiso 1 1 calc R . . C4 C 0.18773(10) -0.00300(9) 0.46655(7) 0.0334(3) Uani 1 1 d DU . . C5 C 0.26823(10) 0.00154(9) 0.43953(6) 0.0326(3) Uani 1 1 d U . . H5 H 0.3161 -0.0257 0.4577 0.039 Uiso 1 1 calc R . . C6 C 0.27984(9) 0.04515(9) 0.38654(6) 0.0307(3) Uani 1 1 d U . . C7 C 0.36987(9) 0.05121(9) 0.36066(6) 0.0317(3) Uani 1 1 d U . . H7A H 0.4016 -0.0028 0.3688 0.038 Uiso 1 1 calc R . . H7B H 0.3660 0.0584 0.3173 0.038 Uiso 1 1 calc R . . O2 O 0.0957(18) -0.039(4) 0.5457(17) 0.041(7) Uani 0.17 1 d PDU A 1 C8 C 0.1700(15) -0.0323(13) 0.5294(7) 0.026(5) Uani 0.17 1 d PDU A 1 C9 C 0.2361(19) -0.094(2) 0.5557(10) 0.059(9) Uani 0.17 1 d PDU A 1 H9A H 0.2938 -0.0816 0.5392 0.071 Uiso 0.17 1 calc PR A 1 H9B H 0.2207 -0.1540 0.5459 0.071 Uiso 0.17 1 calc PR A 1 C10 C 0.2371(12) -0.0817(11) 0.6229(8) 0.058(5) Uani 0.17 1 d PDU A 1 H10A H 0.2146 -0.0237 0.6325 0.069 Uiso 0.17 1 calc PR A 1 H10B H 0.1982 -0.1246 0.6411 0.069 Uiso 0.17 1 calc PR A 1 C11 C 0.3269(13) -0.0913(18) 0.6499(8) 0.093(7) Uani 0.17 1 d PDU A 1 H11A H 0.3622 -0.0398 0.6415 0.112 Uiso 0.17 1 calc PR A 1 H11B H 0.3564 -0.1424 0.6334 0.112 Uiso 0.17 1 calc PR A 1 C12 C 0.3134(10) -0.1023(14) 0.7197(7) 0.075(4) Uani 0.17 1 d PDU A 1 H12A H 0.2959 -0.0466 0.7372 0.090 Uiso 0.17 1 calc PR A 1 H12B H 0.2671 -0.1447 0.7273 0.090 Uiso 0.17 1 calc PR A 1 C13 C 0.3972(12) -0.1330(17) 0.7485(12) 0.093(6) Uani 0.17 1 d PDU A 1 H13A H 0.4352 -0.1574 0.7183 0.112 Uiso 0.17 1 calc PR A 1 H13B H 0.3842 -0.1772 0.7781 0.112 Uiso 0.17 1 calc PR A 1 H13C H 0.4259 -0.0842 0.7676 0.112 Uiso 0.17 1 calc PR A 1 O2A O 0.1064(10) -0.045(2) 0.5489(9) 0.043(4) Uani 0.40 1 d PDU A -3 C8A C 0.1755(8) -0.0498(11) 0.5241(5) 0.034(4) Uani 0.40 1 d PDU A -3 C9A C 0.2535(12) -0.0785(18) 0.5587(7) 0.098(7) Uani 0.40 1 d PDU A -3 H9A1 H 0.2886 -0.1165 0.5332 0.118 Uiso 0.40 1 calc PR A -3 H9A2 H 0.2887 -0.0271 0.5680 0.118 Uiso 0.40 1 calc PR A -3 C10A C 0.2350(12) -0.1253(18) 0.6153(8) 0.127(7) Uani 0.40 1 d PDU A -3 H10C H 0.2158 -0.1849 0.6072 0.152 Uiso 0.40 1 calc PR A -3 H10D H 0.1895 -0.0954 0.6380 0.152 Uiso 0.40 1 calc PR A -3 C11A C 0.3196(12) -0.1259(10) 0.6500(6) 0.089(4) Uani 0.40 1 d PDU A -3 H11C H 0.3624 -0.1587 0.6268 0.107 Uiso 0.40 1 calc PR A -3 H11D H 0.3406 -0.0658 0.6525 0.107 Uiso 0.40 1 calc PR A -3 C12A C 0.3185(5) -0.1627(9) 0.7121(3) 0.092(3) Uani 0.40 1 d PDU A -3 H12C H 0.2979 -0.1166 0.7388 0.110 Uiso 0.40 1 calc PR A -3 H12D H 0.2746 -0.2089 0.7129 0.110 Uiso 0.40 1 calc PR A -3 C13A C 0.3992(6) -0.1987(11) 0.7385(4) 0.118(4) Uani 0.40 1 d PDU A -3 H13D H 0.4140 -0.2528 0.7186 0.142 Uiso 0.40 1 calc PR A -3 H13E H 0.3901 -0.2097 0.7806 0.142 Uiso 0.40 1 calc PR A -3 H13F H 0.4462 -0.1574 0.7335 0.142 Uiso 0.40 1 calc PR A -3 O2B O 0.1065(8) -0.0598(19) 0.5446(9) 0.045(4) Uani 0.43 1 d PDU A 4 C8B C 0.1771(7) -0.0480(9) 0.5230(5) 0.042(4) Uani 0.43 1 d PDU A 4 C9B C 0.2559(6) -0.0818(8) 0.5552(3) 0.0345(17) Uani 0.43 1 d PDU A 4 H9B1 H 0.2828 -0.1274 0.5308 0.041 Uiso 0.43 1 calc PR A 4 H9B2 H 0.2981 -0.0344 0.5591 0.041 Uiso 0.43 1 calc PR A 4 C10B C 0.2378(6) -0.1182(12) 0.6161(5) 0.076(4) Uani 0.43 1 d PDU A 4 H10E H 0.1931 -0.1633 0.6125 0.091 Uiso 0.43 1 calc PR A 4 H10F H 0.2141 -0.0717 0.6411 0.091 Uiso 0.43 1 calc PR A 4 C11B C 0.3169(7) -0.1571(7) 0.6474(4) 0.070(3) Uani 0.43 1 d PDU A 4 H11E H 0.3575 -0.1837 0.6191 0.083 Uiso 0.43 1 calc PR A 4 H11F H 0.3001 -0.1998 0.6777 0.083 Uiso 0.43 1 calc PR A 4 C12B C 0.3552(6) -0.0717(9) 0.6760(4) 0.116(3) Uani 0.43 1 d PDU A 4 H12E H 0.3813 -0.0370 0.6441 0.139 Uiso 0.43 1 calc PR A 4 H12F H 0.3066 -0.0379 0.6923 0.139 Uiso 0.43 1 calc PR A 4 C13B C 0.4229(5) -0.0826(11) 0.7252(3) 0.128(4) Uani 0.43 1 d PDU A 4 H13G H 0.4558 -0.0291 0.7295 0.154 Uiso 0.43 1 calc PR A 4 H13H H 0.4620 -0.1298 0.7149 0.154 Uiso 0.43 1 calc PR A 4 H13I H 0.3939 -0.0959 0.7625 0.154 Uiso 0.43 1 calc PR A 4 P1H P 0.3085(16) 0.2316(17) 0.7103(9) 0.228(7) Uani 0.13 1 d PDU B -99 O1H O 0.361(2) 0.284(2) 0.7516(18) 0.217(11) Uani 0.13 1 d PDU B -99 O2H O 0.342(3) 0.136(2) 0.706(2) 0.221(10) Uani 0.13 1 d PDU B -99 O3H O 0.223(2) 0.213(2) 0.7475(16) 0.180(8) Uani 0.13 1 d PDU B -99 O4H O 0.344(3) 0.159(3) 0.572(2) 0.201(12) Uani 0.13 1 d PDU B -99 N1H N 0.322(2) 0.235(3) 0.5922(14) 0.183(7) Uani 0.13 1 d PDU B -99 C1H C 0.413(4) 0.089(3) 0.683(2) 0.198(14) Uani 0.13 1 d PDU B -99 H1H1 H 0.4635 0.1281 0.6784 0.237 Uiso 0.13 1 calc PR B -99 H1H2 H 0.3985 0.0662 0.6433 0.237 Uiso 0.13 1 calc PR B -99 C2H C 0.436(4) 0.015(4) 0.725(3) 0.24(2) Uani 0.13 1 d PDU B -99 H2H1 H 0.3937 -0.0318 0.7203 0.358 Uiso 0.13 1 calc PR B -99 H2H2 H 0.4338 0.0357 0.7661 0.358 Uiso 0.13 1 calc PR B -99 H2H3 H 0.4935 -0.0067 0.7164 0.358 Uiso 0.13 1 calc PR B -99 C3H C 0.223(5) 0.147(3) 0.794(2) 0.199(15) Uani 0.13 1 d PDU B -99 H3H1 H 0.2810 0.1196 0.7961 0.239 Uiso 0.13 1 calc PR B -99 H3H2 H 0.1806 0.1016 0.7842 0.239 Uiso 0.13 1 calc PR B -99 C4H C 0.201(5) 0.190(4) 0.8520(17) 0.189(14) Uani 0.13 1 d PDU B -99 H4H1 H 0.1426 0.2145 0.8497 0.284 Uiso 0.13 1 calc PR B -99 H4H2 H 0.2421 0.2367 0.8600 0.284 Uiso 0.13 1 calc PR B -99 H4H3 H 0.2032 0.1479 0.8840 0.284 Uiso 0.13 1 calc PR B -99 C5H C 0.373(2) 0.269(2) 0.6426(12) 0.188(7) Uani 0.13 1 d PDU B -99 H5H H 0.4281 0.2364 0.6432 0.225 Uiso 0.13 1 calc PR B -99 C6H C 0.398(2) 0.364(2) 0.6483(16) 0.200(9) Uani 0.13 1 d PDU B -99 C7H C 0.384(4) 0.407(3) 0.5888(19) 0.199(12) Uani 0.13 1 d PDU B -99 H7H1 H 0.3351 0.4473 0.5915 0.298 Uiso 0.13 1 calc PR B -99 H7H2 H 0.3715 0.3636 0.5589 0.298 Uiso 0.13 1 calc PR B -99 H7H3 H 0.4358 0.4392 0.5778 0.298 Uiso 0.13 1 calc PR B -99 C8H C 0.339(4) 0.399(4) 0.697(2) 0.203(13) Uani 0.13 1 d PDU B -99 H8H1 H 0.2796 0.3822 0.6887 0.305 Uiso 0.13 1 calc PR B -99 H8H2 H 0.3434 0.4620 0.6977 0.305 Uiso 0.13 1 calc PR B -99 H8H3 H 0.3573 0.3755 0.7349 0.305 Uiso 0.13 1 calc PR B -99 C9H C 0.491(3) 0.384(3) 0.666(2) 0.182(12) Uani 0.13 1 d PDU B -99 H9H1 H 0.5008 0.3644 0.7063 0.273 Uiso 0.13 1 calc PR B -99 H9H2 H 0.5006 0.4461 0.6632 0.273 Uiso 0.13 1 calc PR B -99 H9H3 H 0.5300 0.3539 0.6390 0.273 Uiso 0.13 1 calc PR B -99 C10H C 0.2416(18) 0.259(2) 0.5625(7) 0.112(5) Uani 0.13 1 d PDU B -99 C11H C 0.2577(19) 0.252(4) 0.4954(7) 0.082(4) Uani 0.13 1 d PDU B -99 H11I H 0.2861 0.3049 0.4814 0.123 Uiso 0.13 1 calc PR B -99 H11J H 0.2027 0.2452 0.4749 0.123 Uiso 0.13 1 calc PR B -99 H11K H 0.2947 0.2026 0.4874 0.123 Uiso 0.13 1 calc PR B -99 C12H C 0.215(3) 0.3510(19) 0.5770(16) 0.104(7) Uani 0.13 1 d PDU B -99 H12G H 0.2182 0.3599 0.6198 0.156 Uiso 0.13 1 calc PR B -99 H12H H 0.1565 0.3612 0.5632 0.156 Uiso 0.13 1 calc PR B -99 H12I H 0.2547 0.3912 0.5573 0.156 Uiso 0.13 1 calc PR B -99 C13H C 0.171(2) 0.1915(18) 0.5706(16) 0.102(8) Uani 0.13 1 d PDU B -99 H13M H 0.1957 0.1405 0.5897 0.154 Uiso 0.13 1 calc PR B -99 H13N H 0.1478 0.1756 0.5320 0.154 Uiso 0.13 1 calc PR B -99 H13O H 0.1251 0.2151 0.5953 0.154 Uiso 0.13 1 calc PR B -99 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 0.0361(6) 0.0423(6) 0.0274(5) 0.0033(4) 0.0038(4) 0.0025(4) C1 0.0358(7) 0.0289(6) 0.0263(6) -0.0020(5) 0.0023(5) -0.0013(5) C2 0.0325(7) 0.0283(6) 0.0290(6) -0.0044(5) 0.0001(5) -0.0017(5) C3 0.0334(7) 0.0289(6) 0.0332(7) -0.0029(5) 0.0037(5) -0.0050(5) C4 0.0370(7) 0.0303(7) 0.0330(7) 0.0015(5) 0.0029(6) -0.0042(5) C5 0.0344(7) 0.0293(7) 0.0342(7) 0.0015(5) 0.0011(5) -0.0007(5) C6 0.0339(7) 0.0282(6) 0.0300(6) -0.0032(5) 0.0023(5) -0.0008(5) C7 0.0333(7) 0.0305(7) 0.0315(7) -0.0013(5) 0.0034(5) 0.0018(5) O2 0.019(5) 0.063(17) 0.042(9) 0.022(8) 0.009(5) -0.001(7) C8 0.030(6) 0.022(6) 0.028(6) -0.001(4) 0.001(4) 0.002(4) C9 0.048(14) 0.073(11) 0.057(12) 0.010(7) 0.011(7) -0.013(9) C10 0.050(8) 0.058(8) 0.065(8) 0.021(6) -0.033(7) -0.001(6) C11 0.089(11) 0.114(14) 0.077(10) -0.030(9) -0.062(9) 0.041(10) C12 0.069(8) 0.096(10) 0.060(8) 0.010(8) 0.007(6) -0.017(8) C13 0.061(9) 0.113(13) 0.105(13) 0.017(11) -0.040(9) -0.004(9) O2A 0.046(7) 0.041(10) 0.042(4) 0.014(6) 0.005(4) 0.002(5) C8A 0.052(7) 0.030(6) 0.020(4) 0.012(4) 0.008(4) -0.014(4) C9A 0.073(12) 0.126(14) 0.096(8) 0.043(9) 0.014(6) 0.019(9) C10A 0.144(10) 0.166(16) 0.069(8) 0.043(9) -0.015(6) 0.021(10) C11A 0.105(7) 0.086(9) 0.076(6) 0.026(6) 0.012(5) 0.011(7) C12A 0.064(4) 0.157(8) 0.054(3) 0.016(5) 0.009(3) 0.011(5) C13A 0.073(5) 0.214(12) 0.067(5) 0.028(6) 0.000(4) 0.023(6) O2B 0.041(4) 0.041(7) 0.053(5) 0.011(4) 0.005(3) -0.008(3) C8B 0.031(5) 0.036(6) 0.058(7) -0.011(4) 0.003(4) 0.010(4) C9B 0.022(4) 0.060(4) 0.021(2) 0.021(2) 0.0030(18) 0.001(3) C10B 0.051(4) 0.121(9) 0.056(5) 0.048(5) 0.032(3) 0.036(5) C11B 0.067(4) 0.107(8) 0.035(2) 0.026(4) 0.003(2) 0.035(5) C12B 0.074(5) 0.215(11) 0.058(4) 0.011(5) -0.004(4) 0.042(6) C13B 0.066(4) 0.270(12) 0.049(3) 0.038(5) 0.008(3) 0.051(6) P1H 0.248(12) 0.218(11) 0.217(10) -0.023(11) 0.022(9) -0.009(9) O1H 0.203(16) 0.234(19) 0.216(11) 0.018(16) 0.013(16) -0.031(14) O2H 0.218(18) 0.222(10) 0.222(19) 0.020(10) 0.018(15) 0.000(13) O3H 0.223(15) 0.172(15) 0.145(11) -0.051(12) -0.023(11) -0.030(10) O4H 0.184(19) 0.200(16) 0.218(19) -0.007(14) -0.036(16) 0.048(14) N1H 0.202(13) 0.140(14) 0.206(9) 0.028(12) -0.052(11) -0.006(11) C1H 0.18(2) 0.190(18) 0.22(2) -0.006(14) 0.004(17) -0.040(14) C2H 0.24(3) 0.24(2) 0.23(3) 0.007(17) -0.012(19) 0.020(17) C3H 0.21(2) 0.20(2) 0.188(17) -0.013(11) -0.017(16) 0.006(17) C4H 0.20(2) 0.20(2) 0.164(12) 0.015(15) -0.018(18) 0.024(17) C5H 0.150(15) 0.203(11) 0.210(10) 0.011(9) -0.037(8) -0.004(13) C6H 0.205(14) 0.211(14) 0.184(13) -0.031(9) -0.021(10) -0.014(13) C7H 0.20(2) 0.193(18) 0.207(15) -0.005(15) -0.004(14) -0.024(18) C8H 0.186(18) 0.20(2) 0.219(18) 0.022(16) 0.013(17) 0.007(18) C9H 0.189(13) 0.18(2) 0.17(2) -0.029(17) 0.014(13) -0.017(14) C10H 0.120(11) 0.116(10) 0.100(6) -0.039(13) 0.034(10) -0.011(8) C11H 0.085(12) 0.052(11) 0.109(5) 0.004(11) 0.077(7) 0.021(12) C12H 0.145(18) 0.101(8) 0.067(12) -0.029(10) 0.034(13) -0.029(9) C13H 0.145(12) 0.066(10) 0.097(14) 0.029(10) 0.075(10) 0.019(9) _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 1.3751(17) . ? C1 C6 1.394(2) . ? C1 C2 1.399(2) . ? C2 C3 1.389(2) . ? C2 C7 1.516(2) 4 ? C3 C4 1.398(2) . ? C4 C5 1.394(2) . ? C4 C8B 1.466(9) . ? C4 C8A 1.504(7) . ? C4 C8 1.519(15) . ? C5 C6 1.390(2) . ? C6 C7 1.519(2) . ? C7 C2 1.516(2) 3 ? O2 C8 1.216(14) . ? C8 C9 1.524(17) . ? C9 C10 1.535(18) . ? C10 C11 1.530(16) . ? C11 C12 1.604(17) . ? C12 C13 1.532(16) . ? O2A C8A 1.215(11) . ? C8A C9A 1.511(13) . ? C9A C10A 1.503(16) . ? C10A C11A 1.531(16) . ? C11A C12A 1.518(13) . ? C12A C13A 1.497(10) . ? O2B C8B 1.214(10) . ? C8B C9B 1.520(10) . ? C9B C10B 1.516(9) . ? C10B C11B 1.541(10) . ? C11B C12B 1.592(14) . ? C12B C13B 1.542(10) . ? P1H O1H 1.482(19) . ? P1H O2H 1.569(18) . ? P1H O3H 1.597(19) . ? P1H C5H 1.923(19) . ? O2H C1H 1.44(2) . ? O3H C3H 1.46(2) . ? O4H N1H 1.299(19) . ? N1H C10H 1.473(18) . ? N1H C5H 1.484(18) . ? C1H C2H 1.55(2) . ? C3H C4H 1.53(2) . ? C5H C6H 1.525(10) . ? C6H C7H 1.520(10) . ? C6H C8H 1.523(10) . ? C6H C9H 1.530(10) . ? C10H C12H 1.517(18) . ? C10H C13H 1.528(19) . ? C10H C11H 1.544(15) . ? 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 O1 C1 C6 121.33(13) . . ? O1 C1 C2 116.36(13) . . ? C6 C1 C2 122.31(13) . . ? C3 C2 C1 118.28(13) . . ? C3 C2 C7 120.37(13) . 4 ? C1 C2 C7 121.19(13) . 4 ? C2 C3 C4 120.83(13) . . ? C5 C4 C3 119.30(13) . . ? C5 C4 C8B 120.5(4) . . ? C3 C4 C8B 120.2(4) . . ? C5 C4 C8A 121.2(5) . . ? C3 C4 C8A 119.5(5) . . ? C8B C4 C8A 0.9(10) . . ? C5 C4 C8 126.1(9) . . ? C3 C4 C8 113.6(9) . . ? C8B C4 C8 11.5(9) . . ? C8A C4 C8 11.7(14) . . ? C6 C5 C4 121.35(14) . . ? C5 C6 C1 117.90(13) . . ? C5 C6 C7 118.87(13) . . ? C1 C6 C7 123.12(13) . . ? C2 C7 C6 110.84(11) 3 . ? O2 C8 C4 118.8(16) . . ? O2 C8 C9 117.9(17) . . ? C4 C8 C9 115.6(14) . . ? C8 C9 C10 108.6(18) . . ? C11 C10 C9 113.2(17) . . ? C10 C11 C12 106.6(16) . . ? C13 C12 C11 110.0(15) . . ? O2A C8A C4 119.1(10) . . ? O2A C8A C9A 119.0(10) . . ? C4 C8A C9A 119.4(9) . . ? C10A C9A C8A 115.7(14) . . ? C9A C10A C11A 106.1(13) . . ? C12A C11A C10A 117.9(13) . . ? C13A C12A C11A 120.1(9) . . ? O2B C8B C4 121.7(9) . . ? O2B C8B C9B 118.7(10) . . ? C4 C8B C9B 119.5(7) . . ? C10B C9B C8B 114.6(7) . . ? C9B C10B C11B 114.7(6) . . ? C10B C11B C12B 99.1(10) . . ? C13B C12B C11B 117.2(10) . . ? O1H P1H O2H 112(3) . . ? O1H P1H O3H 102.8(19) . . ? O2H P1H O3H 98(2) . . ? O1H P1H C5H 93(2) . . ? O2H P1H C5H 94(2) . . ? O3H P1H C5H 155(3) . . ? C1H O2H P1H 139(4) . . ? C3H O3H P1H 120(4) . . ? O4H N1H C10H 107(2) . . ? O4H N1H C5H 117(3) . . ? C10H N1H C5H 135(3) . . ? O2H C1H C2H 109(2) . . ? O3H C3H C4H 107.8(19) . . ? N1H C5H C6H 123(3) . . ? N1H C5H P1H 103(2) . . ? C6H C5H P1H 111(2) . . ? C7H C6H C8H 113(3) . . ? C7H C6H C5H 108(2) . . ? C8H C6H C5H 105(2) . . ? C7H C6H C9H 106(2) . . ? C8H C6H C9H 108(3) . . ? C5H C6H C9H 117(3) . . ? N1H C10H C12H 112(2) . . ? N1H C10H C13H 112(2) . . ? C12H C10H C13H 115(2) . . ? N1H C10H C11H 107(2) . . ? C12H C10H C11H 109(2) . . ? C13H C10H C11H 101(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.55 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.653 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.063 # Attachment 'gena59a.cif' data_gena59a _database_code_depnum_ccdc_archive 'CCDC 661589' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'para hexanoyl calix(4)arene tert butylamine' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H139 N O16' _chemical_formula_weight 1707.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6128(10) _cell_length_b 42.409(3) _cell_length_c 16.2745(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.935(4) _cell_angle_gamma 90.00 _cell_volume 9360.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3688 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9612 _exptl_absorpt_correction_T_max 0.9881 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 123801 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.1161 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 23.48 _reflns_number_total 13592 _reflns_number_gt 8823 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+6.1931P] 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 SHELXL _refine_ls_extinction_coef 0.0034(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13592 _refine_ls_number_parameters 1218 _refine_ls_number_restraints 143 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1866 _refine_ls_wR_factor_gt 0.1556 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O2 O -0.5049(8) 0.1445(3) 0.6497(8) 0.0303(16) Uani 0.50 1 d PD A 21 C8 C -0.4936(9) 0.1207(5) 0.6043(14) 0.0345(18) Uani 0.50 1 d PD A 21 C9 C -0.5822(6) 0.0991(2) 0.5856(6) 0.035(2) Uani 0.50 1 d PD A 21 H9A H -0.6433 0.1107 0.5951 0.042 Uiso 0.50 1 calc PR A 21 H9B H -0.5862 0.0928 0.5268 0.042 Uiso 0.50 1 calc PR A 21 C10 C -0.5749(5) 0.07003(16) 0.6391(5) 0.0364(15) Uani 0.50 1 d PD A 21 H10A H -0.5464 0.0763 0.6947 0.044 Uiso 0.50 1 calc PR A 21 H10B H -0.5275 0.0554 0.6162 0.044 Uiso 0.50 1 calc PRD A 21 C11 C -0.6703(8) 0.0519(2) 0.6488(7) 0.0405(19) Uani 0.50 1 d PD A 21 H11A H -0.7120 0.0640 0.6845 0.049 Uiso 0.50 1 calc PR A 21 H11B H -0.7074 0.0493 0.5942 0.049 Uiso 0.50 1 calc PR A 21 C12 C -0.6473(7) 0.0196(2) 0.6869(6) 0.034(2) Uani 0.50 1 d PD A 21 H12A H -0.6035 0.0223 0.7382 0.041 Uiso 0.50 1 calc PR A 21 H12B H -0.6115 0.0068 0.6482 0.041 Uiso 0.50 1 calc PR A 21 C13 C -0.7406(5) 0.00170(19) 0.7069(5) 0.0358(17) Uani 0.50 1 d PD A 21 H13A H -0.7773 0.0144 0.7441 0.043 Uiso 0.50 1 calc PR A 21 H13B H -0.7218 -0.0184 0.7335 0.043 Uiso 0.50 1 calc PR A 21 H13C H -0.7821 -0.0023 0.6557 0.043 Uiso 0.50 1 calc PR A 21 O2F O -0.479(3) 0.1416(13) 0.675(3) 0.0303(16) Uani 0.04 1 d PD A 22 C8F C -0.486(2) 0.1209(16) 0.621(3) 0.0345(18) Uani 0.04 1 d PD A 22 C9F C -0.5873(14) 0.1129(13) 0.578(4) 0.035(2) Uani 0.04 1 d PD A 22 H9F1 H -0.6207 0.1329 0.5614 0.042 Uiso 0.04 1 calc PR A 22 H9F2 H -0.5774 0.1010 0.5273 0.042 Uiso 0.04 1 calc PR A 22 C10F C -0.656(4) 0.0938(11) 0.629(6) 0.0364(15) Uani 0.04 1 d PD A 22 H10C H -0.7257 0.0990 0.6114 0.044 Uiso 0.04 1 calc PR A 22 H10D H -0.6431 0.0989 0.6881 0.044 Uiso 0.04 1 calc PR A 22 C11F C -0.637(6) 0.0587(11) 0.614(5) 0.0405(19) Uani 0.04 1 d PD A 22 H11C H -0.6442 0.0544 0.5541 0.049 Uiso 0.04 1 calc PR A 22 H11D H -0.5679 0.0536 0.6347 0.049 Uiso 0.04 1 calc PR A 22 C12F C -0.707(5) 0.0378(15) 0.657(6) 0.034(2) Uani 0.04 1 d PD A 22 H12C H -0.7453 0.0243 0.6163 0.041 Uiso 0.04 1 calc PR A 22 H12D H -0.7542 0.0510 0.6853 0.041 Uiso 0.04 1 calc PR A 22 C13F C -0.647(9) 0.0171(15) 0.721(2) 0.0358(17) Uani 0.04 1 d PD A 22 H13D H -0.6885 0.0003 0.7572 0.043 Uiso 0.04 1 d P B 22 H13E H -0.5932 0.0224 0.7575 0.043 Uiso 0.04 1 d P C 22 H13F H -0.6136 -0.0037 0.6872 0.043 Uiso 0.04 1 d P D 22 O2G O -0.5146(9) 0.1384(3) 0.6527(9) 0.0303(16) Uani 0.46 1 d PD A 23 C8G C -0.4981(10) 0.1214(6) 0.5944(16) 0.0345(18) Uani 0.46 1 d PD A 23 C9G C -0.5822(7) 0.1043(3) 0.5450(6) 0.035(2) Uani 0.46 1 d PD A 23 H9G1 H -0.5983 0.1152 0.4919 0.042 Uiso 0.46 1 calc PR A 23 H9G2 H -0.5618 0.0825 0.5330 0.042 Uiso 0.46 1 calc PR A 23 C10G C -0.6722(6) 0.1035(2) 0.5933(5) 0.0364(15) Uani 0.46 1 d PD A 23 H10E H -0.7311 0.0999 0.5544 0.044 Uiso 0.46 1 calc PR A 23 H10F H -0.6797 0.1244 0.6192 0.044 Uiso 0.46 1 calc PR A 23 C11G C -0.6696(7) 0.07812(19) 0.6609(5) 0.0405(19) Uani 0.46 1 d PD A 23 H11E H -0.6076 0.0802 0.6969 0.049 Uiso 0.46 1 calc PR A 23 H11F H -0.7251 0.0817 0.6953 0.049 Uiso 0.46 1 calc PR A 23 C12G C -0.6766(10) 0.0448(2) 0.6263(7) 0.034(2) Uani 0.46 1 d PD A 23 H12E H -0.6168 0.0402 0.5978 0.041 Uiso 0.46 1 calc PR A 23 H12F H -0.7343 0.0434 0.5850 0.041 Uiso 0.46 1 calc PR A 23 C13G C -0.6867(8) 0.0198(3) 0.6933(7) 0.0358(17) Uani 0.46 1 d PD A 23 H13G H -0.6266 0.0195 0.7310 0.043 Uiso 0.46 1 calc PR A 23 H13H H -0.6968 -0.0010 0.6674 0.043 Uiso 0.46 1 calc PR A 23 H13I H -0.7433 0.0249 0.7242 0.043 Uiso 0.46 1 calc PR A 23 O1 O -0.1132(2) 0.09776(6) 0.51184(17) 0.0340(7) Uani 1 1 d . . . H1 H -0.075(3) 0.1051(11) 0.538(3) 0.051 Uiso 1 1 d . . . O3 O 0.01285(19) 0.11204(6) 0.63865(16) 0.0322(7) Uani 1 1 d . . . H3 H 0.036(3) 0.0954(10) 0.651(3) 0.048 Uiso 1 1 d . . . O4 O -0.20123(19) 0.19577(6) 0.88837(16) 0.0360(7) Uani 1 1 d . . . O5 O 0.07311(19) 0.05237(6) 0.65851(17) 0.0337(7) Uani 1 1 d . . . H5 H 0.039(3) 0.0477(10) 0.616(3) 0.051 Uiso 1 1 d . . . O6 O -0.08487(17) 0.02934(6) 1.00661(16) 0.0306(6) Uani 1 1 d . . . O7 O -0.06170(19) 0.03783(6) 0.53184(16) 0.0334(7) Uani 1 1 d . . . H7 H -0.083(3) 0.0533(10) 0.507(3) 0.050 Uiso 1 1 d . . . O8 O -0.4555(2) -0.03832(6) 0.56515(19) 0.0502(8) Uani 1 1 d . . . C1 C -0.2068(3) 0.10407(8) 0.5313(2) 0.0270(9) Uani 1 1 d . A . C2 C -0.2811(3) 0.08271(8) 0.5052(2) 0.0291(9) Uani 1 1 d . . . C3 C -0.3757(3) 0.08869(8) 0.5261(2) 0.0324(9) Uani 1 1 d . A . H3S H -0.4275 0.0746 0.5081 0.039 Uiso 1 1 calc R . . C4 C -0.3965(3) 0.11497(8) 0.5732(2) 0.0307(9) Uani 1 1 d D . . C5K C -0.3201(3) 0.13595(8) 0.5963(2) 0.0264(9) Uani 1 1 d . A . H5K H -0.3341 0.1540 0.6277 0.032 Uiso 1 1 calc R . . C6 C -0.2257(3) 0.13146(8) 0.5753(2) 0.0253(8) Uani 1 1 d . . . C7 C -0.1450(3) 0.15516(8) 0.6017(2) 0.0261(8) Uani 1 1 d . A . H7B H -0.0930 0.1541 0.5629 0.031 Uiso 1 1 calc R . . H7C H -0.1732 0.1767 0.5990 0.031 Uiso 1 1 calc R . . C14 C -0.0251(2) 0.12640(8) 0.7054(2) 0.0228(8) Uani 1 1 d . A . C15 C -0.0992(2) 0.14888(8) 0.6889(2) 0.0229(8) Uani 1 1 d . . . C16 C -0.1326(2) 0.16444(8) 0.7556(2) 0.0240(8) Uani 1 1 d . A . H16 H -0.1818 0.1802 0.7460 0.029 Uiso 1 1 calc R . . C17 C -0.0968(2) 0.15782(8) 0.8366(2) 0.0218(8) Uani 1 1 d D . . C18 C -0.0244(2) 0.13471(8) 0.8507(2) 0.0235(8) Uani 1 1 d . A . H18 H -0.0001 0.1297 0.9056 0.028 Uiso 1 1 calc R . . C19 C 0.0126(2) 0.11891(8) 0.7851(2) 0.0234(8) Uani 1 1 d . . . C20 C 0.0900(2) 0.09308(8) 0.8012(2) 0.0261(8) Uani 1 1 d . A . H20B H 0.1380 0.0943 0.7589 0.031 Uiso 1 1 calc R . . H20A H 0.1263 0.0966 0.8558 0.031 Uiso 1 1 calc R . . C21 C -0.1372(2) 0.17612(8) 0.9049(2) 0.0250(8) Uani 1 1 d D A . C22 C -0.0968(3) 0.17040(8) 0.9930(2) 0.0281(9) Uani 1 1 d D . . H22B H -0.0269 0.1770 0.9993 0.034 Uiso 1 1 calc R A . H22A H -0.0989 0.1475 1.0043 0.034 Uiso 1 1 calc R . . C23 C -0.1520(3) 0.18758(9) 1.0569(2) 0.0311(9) Uani 1 1 d D A . H23B H -0.2197 0.1790 1.0559 0.037 Uiso 1 1 calc R . . H23A H -0.1573 0.2102 1.0419 0.037 Uiso 1 1 calc R . . C24 C -0.1023(3) 0.18469(10) 1.1441(2) 0.0388(10) Uani 1 1 d D . . H24B H -0.1483 0.1925 1.1834 0.047 Uiso 1 1 calc R A . H24A H -0.0897 0.1621 1.1563 0.047 Uiso 1 1 calc R . . C25 C -0.0068(3) 0.20238(13) 1.1586(3) 0.0659(15) Uani 1 1 d D A . H25B H 0.0396 0.1945 1.1198 0.079 Uiso 1 1 calc R . . H25A H 0.0223 0.1980 1.2153 0.079 Uiso 1 1 calc R . . C26 C -0.0179(5) 0.23761(15) 1.1479(4) 0.095(2) Uani 1 1 d DU . . H26C H -0.0666 0.2455 1.1839 0.114 Uiso 1 1 calc R A . H26B H -0.0401 0.2424 1.0903 0.114 Uiso 1 1 calc R . . H26A H 0.0457 0.2479 1.1624 0.114 Uiso 1 1 calc R . . C27 C 0.0359(2) 0.04124(8) 0.7291(2) 0.0254(8) Uani 1 1 d . A . C28 C 0.0442(2) 0.06034(8) 0.7993(2) 0.0236(8) Uani 1 1 d . . . C29 C 0.0031(2) 0.04962(8) 0.8691(2) 0.0251(8) Uani 1 1 d . A . H29 H 0.0077 0.0624 0.9173 0.030 Uiso 1 1 calc R . . C30 C -0.0450(2) 0.02041(8) 0.8705(2) 0.0245(8) Uani 1 1 d D . . C31 C -0.0482(2) 0.00146(8) 0.8003(2) 0.0259(8) Uani 1 1 d . A . H31 H -0.0786 -0.0187 0.8014 0.031 Uiso 1 1 calc R . . C32 C -0.0081(2) 0.01111(8) 0.7287(2) 0.0254(8) Uani 1 1 d . . . C33 C -0.0176(3) -0.00938(8) 0.6518(2) 0.0283(9) Uani 1 1 d . A . H33B H 0.0341 -0.0034 0.6155 0.034 Uiso 1 1 calc R . . H33A H -0.0070 -0.0317 0.6679 0.034 Uiso 1 1 calc R . . C34 C -0.0940(2) 0.01206(8) 0.9460(2) 0.0251(8) Uani 1 1 d D A . C35 C -0.1554(3) -0.01734(8) 0.9476(2) 0.0301(9) Uani 1 1 d D . . H35B H -0.1110 -0.0359 0.9527 0.036 Uiso 1 1 calc R A . H35A H -0.1964 -0.0192 0.8946 0.036 Uiso 1 1 calc R . . C36 C -0.2226(3) -0.01814(8) 1.0176(2) 0.0311(9) Uani 1 1 d D A . H36B H -0.1824 -0.0150 1.0707 0.037 Uiso 1 1 calc R . . H36A H -0.2702 -0.0005 1.0107 0.037 Uiso 1 1 calc R . . C37 C -0.2788(3) -0.04892(9) 1.0207(2) 0.0347(9) Uani 1 1 d D . . H37B H -0.2309 -0.0665 1.0273 0.042 Uiso 1 1 calc R A . H37A H -0.3187 -0.0519 0.9675 0.042 Uiso 1 1 calc R . . C38 C -0.3463(3) -0.05050(10) 1.0901(3) 0.0514(12) Uani 1 1 d D A . H38B H -0.3949 -0.0331 1.0834 0.062 Uiso 1 1 calc R . . H38A H -0.3067 -0.0474 1.1434 0.062 Uiso 1 1 calc RD . . C39 C -0.4012(4) -0.08177(11) 1.0921(3) 0.0680(15) Uani 1 1 d D . . H39C H -0.3539 -0.0989 1.1049 0.082 Uiso 1 1 calc R A . H39B H -0.4370 -0.0856 1.0382 0.082 Uiso 1 1 calc R . . H39A H -0.4481 -0.0809 1.1345 0.082 Uiso 1 1 calc R . . C40 C -0.1391(3) 0.01881(8) 0.5501(2) 0.0273(9) Uani 1 1 d . A . C41 C -0.1180(3) -0.00603(8) 0.6046(2) 0.0267(9) Uani 1 1 d . . . C42 C -0.1943(3) -0.02613(8) 0.6201(2) 0.0304(9) Uani 1 1 d . A . H42 H -0.1811 -0.0436 0.6557 0.036 Uiso 1 1 calc R . . C43 C -0.2903(3) -0.02128(8) 0.5846(2) 0.0323(9) Uani 1 1 d D . . C44 C -0.3083(3) 0.00436(8) 0.5324(2) 0.0346(10) Uani 1 1 d . A . H44 H -0.3736 0.0080 0.5087 0.041 Uiso 1 1 calc R . . C45 C -0.2339(3) 0.02496(8) 0.5137(2) 0.0318(9) Uani 1 1 d . . . C46 C -0.2587(3) 0.05310(8) 0.4572(2) 0.0330(9) Uani 1 1 d . A . H46B H -0.2024 0.0573 0.4241 0.040 Uiso 1 1 calc R . . H46A H -0.3166 0.0478 0.4186 0.040 Uiso 1 1 calc R . . C47 C -0.3738(3) -0.04226(9) 0.6020(3) 0.0396(10) Uani 1 1 d D A . C48 C -0.3565(3) -0.06830(9) 0.6650(3) 0.0383(10) Uani 1 1 d D . . H48B H -0.3220 -0.0594 0.7158 0.046 Uiso 1 1 calc R A . H48A H -0.3126 -0.0843 0.6432 0.046 Uiso 1 1 calc R . . C49 C -0.4507(3) -0.08447(9) 0.6872(3) 0.0409(10) Uani 1 1 d D A . H49B H -0.4896 -0.0908 0.6357 0.049 Uiso 1 1 calc R . . H49A H -0.4326 -0.1039 0.7187 0.049 Uiso 1 1 calc R . . C50 C -0.5154(3) -0.06415(10) 0.7379(3) 0.0443(11) Uani 1 1 d D . . H50B H -0.5215 -0.0429 0.7128 0.053 Uiso 1 1 calc R A . H50A H -0.5822 -0.0735 0.7355 0.053 Uiso 1 1 calc R . . C51 C -0.4759(3) -0.06082(11) 0.8279(3) 0.0557(13) Uani 1 1 d D A . H51B H -0.4090 -0.0515 0.8306 0.067 Uiso 1 1 calc R . . H51A H -0.4702 -0.0820 0.8534 0.067 Uiso 1 1 calc R . . C52 C -0.5417(4) -0.04025(12) 0.8773(3) 0.0643(14) Uani 1 1 d D . . H52C H -0.6083 -0.0492 0.8741 0.077 Uiso 1 1 calc R A . H52B H -0.5443 -0.0189 0.8544 0.077 Uiso 1 1 calc R . . H52A H -0.5146 -0.0395 0.9350 0.077 Uiso 1 1 calc R . . O1A O 0.75053(17) 0.10385(6) 0.28828(15) 0.0315(6) Uani 1 1 d D . . H1A H 0.8158 0.0980 0.2988 0.050 Uiso 1 1 d D . . O2A O 0.6590(2) 0.13277(6) -0.09005(16) 0.0397(7) Uani 1 1 d . . . O3A O 0.73143(18) 0.15674(5) 0.35858(15) 0.0302(6) Uani 1 1 d . . . H3A H 0.7028 0.1407 0.3381 0.036 Uiso 1 1 calc R . . O4A O 0.68912(17) 0.28783(5) 0.17530(15) 0.0300(6) Uani 1 1 d . . . O5A O 0.90933(18) 0.15145(5) 0.40367(15) 0.0303(6) Uani 1 1 d . . . H5A H 0.8498 0.1569 0.3991 0.049(14) Uiso 1 1 calc R . . O6A O 1.24620(19) 0.25015(6) 0.3571(2) 0.0515(8) Uani 1 1 d . . . O7A O 0.95390(18) 0.09109(6) 0.35825(15) 0.0331(6) Uani 1 1 d D . . H7A H 0.9429 0.1000 0.3975 0.052 Uiso 1 1 d D . . C1A C 0.7384(2) 0.10545(8) 0.2053(2) 0.0245(8) Uani 1 1 d . . . C2A C 0.7975(3) 0.08638(8) 0.1592(2) 0.0248(8) Uani 1 1 d . . . C3A C 0.7834(3) 0.08702(8) 0.0741(2) 0.0275(9) Uani 1 1 d . . . H3A2 H 0.8212 0.0734 0.0430 0.033 Uiso 1 1 calc R . . C4A C 0.7150(2) 0.10719(8) 0.0326(2) 0.0247(8) Uani 1 1 d D . . C5A C 0.6577(2) 0.12615(8) 0.0803(2) 0.0268(9) Uani 1 1 d . . . H5L H 0.6106 0.1400 0.0531 0.032 Uiso 1 1 calc R . . C6A C 0.6671(2) 0.12552(8) 0.1651(2) 0.0240(8) Uani 1 1 d . . . C7K C 0.6024(3) 0.14675(8) 0.2133(2) 0.0270(9) Uani 1 1 d . . . H7A1 H 0.5392 0.1505 0.1798 0.032 Uiso 1 1 calc R . . H3K H 0.5873 0.1358 0.2644 0.032 Uiso 1 1 calc R . . C8A C 0.7031(3) 0.10992(8) -0.0574(2) 0.0279(9) Uani 1 1 d D . . C9A C 0.7441(3) 0.08499(8) -0.1115(2) 0.0316(9) Uani 1 1 d D . . H9A2 H 0.7209 0.0641 -0.0943 0.038 Uiso 1 1 calc R . . H9A1 H 0.8169 0.0852 -0.1021 0.038 Uiso 1 1 calc R . . C10A C 0.7158(3) 0.08900(8) -0.2029(2) 0.0325(9) Uani 1 1 d D . . H10K H 0.6430 0.0903 -0.2122 0.039 Uiso 1 1 calc R . . H10L H 0.7433 0.1091 -0.2214 0.039 Uiso 1 1 calc R . . C11A C 0.7516(3) 0.06253(9) -0.2547(3) 0.0387(10) Uani 1 1 d D . . H11K H 0.8244 0.0616 -0.2462 0.046 Uiso 1 1 calc R . . H11L H 0.7338 0.0675 -0.3136 0.046 Uiso 1 1 calc R . . C12A C 0.7104(3) 0.03029(10) -0.2361(3) 0.0535(13) Uani 1 1 d D . . H12K H 0.7436 0.0144 -0.2687 0.064 Uiso 1 1 calc R . . H12L H 0.7280 0.0256 -0.1771 0.064 Uiso 1 1 calc R . . C13A C 0.6039(4) 0.02637(15) -0.2529(5) 0.109(2) Uani 1 1 d DU . . H13K H 0.5846 0.0317 -0.3107 0.131 Uiso 1 1 calc R . . H13L H 0.5697 0.0404 -0.2169 0.131 Uiso 1 1 calc R . . H13M H 0.5859 0.0044 -0.2426 0.131 Uiso 1 1 calc R . . C14A C 0.7113(2) 0.18133(8) 0.3093(2) 0.0251(8) Uani 1 1 d . . . C15A C 0.6496(2) 0.17822(8) 0.2360(2) 0.0246(8) Uani 1 1 d . . . C16A C 0.6330(2) 0.20419(8) 0.1847(2) 0.0250(8) Uani 1 1 d . . . H16A H 0.5920 0.2019 0.1347 0.030 Uiso 1 1 calc R . . C17A C 0.6753(2) 0.23369(8) 0.2045(2) 0.0238(8) Uani 1 1 d D . . C18A C 0.7341(2) 0.23640(8) 0.2792(2) 0.0236(8) Uani 1 1 d . . . H18A H 0.7616 0.2564 0.2945 0.028 Uiso 1 1 calc R . . C19A C 0.7533(2) 0.21102(8) 0.3313(2) 0.0242(8) Uani 1 1 d . . . C20A C 0.8210(2) 0.21420(8) 0.4102(2) 0.0262(8) Uani 1 1 d . . . H20D H 0.8149 0.2358 0.4321 0.031 Uiso 1 1 calc R . . H20C H 0.7991 0.1993 0.4517 0.031 Uiso 1 1 calc R . . C21A C 0.6584(2) 0.26151(8) 0.1511(2) 0.0257(8) Uani 1 1 d D . . C22A C 0.6057(3) 0.25883(8) 0.0659(2) 0.0315(9) Uani 1 1 d D . . H22D H 0.5475 0.2450 0.0687 0.038 Uiso 1 1 calc R . . H22C H 0.6504 0.2485 0.0291 0.038 Uiso 1 1 calc R . . C23A C 0.5720(3) 0.29019(8) 0.0281(2) 0.0324(9) Uani 1 1 d D . . H23D H 0.6308 0.3034 0.0212 0.039 Uiso 1 1 calc R . . H23C H 0.5317 0.3012 0.0669 0.039 Uiso 1 1 calc R . . C24A C 0.5120(3) 0.28734(8) -0.0553(2) 0.0303(9) Uani 1 1 d D . . H24D H 0.5544 0.2786 -0.0961 0.036 Uiso 1 1 calc R . . H24C H 0.4569 0.2724 -0.0502 0.036 Uiso 1 1 calc R . . C25A C 0.4704(3) 0.31887(9) -0.0865(3) 0.0386(10) Uani 1 1 d D . . H25D H 0.5253 0.3340 -0.0900 0.046 Uiso 1 1 calc R . . H25C H 0.4262 0.3273 -0.0466 0.046 Uiso 1 1 calc R . . C26A C 0.4131(3) 0.31608(10) -0.1711(3) 0.0416(11) Uani 1 1 d D . . H26F H 0.3605 0.3004 -0.1686 0.050 Uiso 1 1 calc R . . H26E H 0.4578 0.3095 -0.2119 0.050 Uiso 1 1 calc R . . H26D H 0.3842 0.3366 -0.1871 0.050 Uiso 1 1 calc R . . C27A C 0.9670(3) 0.17713(8) 0.3954(2) 0.0261(9) Uani 1 1 d . . . C28A C 0.9278(2) 0.20787(8) 0.3985(2) 0.0248(8) Uani 1 1 d . . . C29A C 0.9926(3) 0.23280(9) 0.3901(2) 0.0276(9) Uani 1 1 d . . . H29A H 0.9679 0.2537 0.3917 0.033 Uiso 1 1 calc R . . C30A C 1.0915(3) 0.22845(8) 0.3793(2) 0.0303(9) Uani 1 1 d D . . C31A C 1.1273(3) 0.19749(8) 0.3779(2) 0.0299(9) Uani 1 1 d . . . H31A H 1.1951 0.1940 0.3711 0.036 Uiso 1 1 calc R . . C32A C 1.0663(3) 0.17193(8) 0.3860(2) 0.0260(8) Uani 1 1 d . . . C33A C 1.1083(3) 0.13839(8) 0.3841(2) 0.0310(9) Uani 1 1 d . . . H33D H 1.1810 0.1394 0.3939 0.037 Uiso 1 1 calc R . . H33C H 1.0834 0.1260 0.4295 0.037 Uiso 1 1 calc RD . . C34A C 1.1601(3) 0.25490(9) 0.3681(3) 0.0399(10) Uani 1 1 d D . . C35A C 1.1230(3) 0.28862(9) 0.3734(3) 0.0476(12) Uani 1 1 d D . . H35D H 1.0524 0.2893 0.3530 0.057 Uiso 1 1 calc R . . H35C H 1.1283 0.2952 0.4320 0.057 Uiso 1 1 calc R . . C36A C 1.1794(3) 0.31183(9) 0.3242(3) 0.0407(11) Uani 1 1 d D . . H36D H 1.1639 0.3336 0.3410 0.049 Uiso 1 1 calc R . . H36C H 1.2510 0.3084 0.3371 0.049 Uiso 1 1 calc R . . C37A C 1.1547(3) 0.30849(10) 0.2318(3) 0.0512(12) Uani 1 1 d D . . H37D H 1.1718 0.2869 0.2152 0.061 Uiso 1 1 calc R . . H37C H 1.0827 0.3111 0.2196 0.061 Uiso 1 1 calc R . . C38A C 1.2068(4) 0.33169(11) 0.1802(3) 0.0577(13) Uani 1 1 d D . . H38D H 1.2789 0.3282 0.1893 0.069 Uiso 1 1 calc R . . H38C H 1.1928 0.3534 0.1984 0.069 Uiso 1 1 calc R . . C39A C 1.1753(5) 0.32866(14) 0.0887(3) 0.089(2) Uani 1 1 d D . . H39F H 1.1047 0.3332 0.0788 0.106 Uiso 1 1 calc R . . H39E H 1.1882 0.3071 0.0704 0.106 Uiso 1 1 calc R . . H39D H 1.2128 0.3436 0.0577 0.106 Uiso 1 1 calc R . . C40A C 1.0026(3) 0.10002(8) 0.2926(2) 0.0280(9) Uani 1 1 d D . . C41A C 1.0812(3) 0.12150(8) 0.3030(2) 0.0273(9) Uani 1 1 d . . . C42A C 1.1349(3) 0.12715(8) 0.2356(2) 0.0291(9) Uani 1 1 d . . . H42A H 1.1902 0.1409 0.2419 0.035 Uiso 1 1 calc R . . C43A C 1.1099(3) 0.11322(8) 0.1589(2) 0.0284(9) Uani 1 1 d D . . C44A C 1.0284(3) 0.09343(8) 0.1499(2) 0.0278(9) Uani 1 1 d . . . H44A H 1.0097 0.0845 0.0974 0.033 Uiso 1 1 calc R . . C45A C 0.9735(3) 0.08641(8) 0.2156(2) 0.0255(8) Uani 1 1 d . . . C46A C 0.8801(3) 0.06669(8) 0.2021(2) 0.0284(9) Uani 1 1 d . . . H46D H 0.8927 0.0481 0.1678 0.034 Uiso 1 1 calc R . . H46C H 0.8604 0.0591 0.2558 0.034 Uiso 1 1 calc R . . O8A O 1.1322(3) 0.1164(2) 0.0168(2) 0.0440(12) Uani 0.83 1 d PD E 81 C47A C 1.1685(5) 0.1195(3) 0.0880(4) 0.0318(11) Uani 0.83 1 d PD E 81 C48A C 1.2775(3) 0.12629(13) 0.1023(4) 0.0400(14) Uani 0.83 1 d PD E 81 H48C H 1.3140 0.1073 0.0870 0.048 Uiso 0.83 1 calc PR E 81 H48D H 1.2938 0.1300 0.1619 0.048 Uiso 0.83 1 calc PR E 81 C49A C 1.3139(4) 0.15414(12) 0.0553(3) 0.0484(14) Uani 0.83 1 d PD E 81 H49C H 1.2864 0.1529 -0.0029 0.058 Uiso 0.83 1 calc PR E 81 H49D H 1.3866 0.1531 0.0562 0.058 Uiso 0.83 1 calc PR E 81 C50A C 1.2842(5) 0.18591(12) 0.0919(4) 0.0542(15) Uani 0.83 1 d PD E 81 H50C H 1.2117 0.1882 0.0829 0.065 Uiso 0.83 1 calc PR E 81 H50D H 1.3018 0.1855 0.1522 0.065 Uiso 0.83 1 calc PR E 81 C51A C 1.3318(4) 0.21430(12) 0.0562(4) 0.0501(14) Uani 0.83 1 d PD E 81 H51C H 1.3147 0.2151 -0.0041 0.060 Uiso 0.83 1 calc PR E 81 H51D H 1.4044 0.2127 0.0663 0.060 Uiso 0.83 1 calc PR E 81 C52A C 1.2956(7) 0.24417(17) 0.0965(5) 0.076(3) Uani 0.83 1 d PD E 81 H52D H 1.2247 0.2466 0.0821 0.114 Uiso 0.83 1 calc PR E 81 H52E H 1.3306 0.2625 0.0768 0.114 Uiso 0.83 1 calc PR E 81 H52F H 1.3085 0.2425 0.1566 0.114 Uiso 0.83 1 calc PR E 81 O8B O 1.110(2) 0.1172(13) 0.0147(10) 0.0440(12) Uani 0.17 1 d PD E 82 C47B C 1.157(3) 0.1180(13) 0.0800(17) 0.0318(11) Uani 0.17 1 d PD E 82 C48B C 1.2581(15) 0.1341(6) 0.088(2) 0.0400(14) Uani 0.17 1 d PD E 82 H48E H 1.2915 0.1297 0.1433 0.048 Uiso 0.17 1 calc PR E 82 H48F H 1.2993 0.1254 0.0463 0.048 Uiso 0.17 1 calc PR E 82 C49B C 1.2481(17) 0.1696(5) 0.0764(19) 0.0484(14) Uani 0.17 1 d PD E 82 H49E H 1.2032 0.1782 0.1154 0.058 Uiso 0.17 1 calc PR E 82 H49F H 1.2200 0.1743 0.0196 0.058 Uiso 0.17 1 calc PR E 82 C50B C 1.3525(18) 0.1852(5) 0.0921(19) 0.0542(15) Uani 0.17 1 d PD E 82 H50E H 1.3910 0.1742 0.1379 0.065 Uiso 0.17 1 calc PR E 82 H50F H 1.3886 0.1833 0.0420 0.065 Uiso 0.17 1 calc PR E 82 C51B C 1.3411(18) 0.2192(5) 0.1134(18) 0.0501(14) Uani 0.17 1 d PD E 82 H51E H 1.4086 0.2280 0.1206 0.060 Uiso 0.17 1 calc PR E 82 H51F H 1.3158 0.2195 0.1687 0.060 Uiso 0.17 1 calc PR E 82 C52B C 1.280(4) 0.2427(9) 0.062(3) 0.076(3) Uani 0.17 1 d PD E 82 H52G H 1.2983 0.2420 0.0054 0.114 Uiso 0.17 1 calc PR E 82 H52H H 1.2928 0.2639 0.0849 0.114 Uiso 0.17 1 calc PR E 82 H52I H 1.2103 0.2376 0.0635 0.114 Uiso 0.17 1 calc PR E 82 N1G N 0.5947(2) 0.17365(7) -0.21555(19) 0.0276(7) Uani 1 1 d . . . H1G1 H 0.6365 0.1890 -0.2304 0.041 Uiso 0.50 1 calc PR . . H1G2 H 0.5685 0.1634 -0.2614 0.041 Uiso 0.50 1 calc PR . . H1G3 H 0.6284 0.1597 -0.1813 0.041 Uiso 1 1 calc R . . C1G C 0.5128(2) 0.18843(8) -0.1716(2) 0.0271(9) Uani 1 1 d . . . C2G C 0.5597(3) 0.20426(9) -0.0943(2) 0.0367(10) Uani 1 1 d . . . H2G3 H 0.6059 0.2205 -0.1097 0.055 Uiso 1 1 calc R . . H2G2 H 0.5953 0.1885 -0.0592 0.055 Uiso 1 1 calc R . . H2G1 H 0.5083 0.2140 -0.0642 0.055 Uiso 1 1 calc R . . C3G C 0.4598(3) 0.21216(9) -0.2299(3) 0.0368(10) Uani 1 1 d . . . H3G3 H 0.4364 0.2016 -0.2814 0.055 Uiso 1 1 calc R . . H3G2 H 0.5054 0.2291 -0.2417 0.055 Uiso 1 1 calc R . . H3G1 H 0.4035 0.2211 -0.2041 0.055 Uiso 1 1 calc R . . C4G C 0.4457(3) 0.16164(9) -0.1495(3) 0.0378(10) Uani 1 1 d . . . H4G3 H 0.4844 0.1458 -0.1170 0.057 Uiso 1 1 calc R . . H4G2 H 0.4155 0.1519 -0.2002 0.057 Uiso 1 1 calc R . . H4G1 H 0.3939 0.1699 -0.1172 0.057 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 O2 0.031(2) 0.024(4) 0.035(2) -0.001(3) -0.0061(16) -0.012(2) C8 0.037(2) 0.026(2) 0.037(5) 0.006(3) -0.015(2) -0.005(2) C9 0.042(3) 0.024(4) 0.036(7) -0.004(5) -0.015(4) 0.005(3) C10 0.029(3) 0.032(3) 0.047(4) -0.007(3) -0.008(3) 0.002(3) C11 0.039(4) 0.042(4) 0.042(5) -0.011(4) 0.011(3) -0.001(4) C12 0.033(4) 0.037(4) 0.034(4) -0.007(3) 0.016(3) -0.001(3) C13 0.028(4) 0.040(4) 0.040(4) -0.006(3) 0.003(3) -0.001(3) O2F 0.031(2) 0.024(4) 0.035(2) -0.001(3) -0.0061(16) -0.012(2) C8F 0.037(2) 0.026(2) 0.037(5) 0.006(3) -0.015(2) -0.005(2) C9F 0.042(3) 0.024(4) 0.036(7) -0.004(5) -0.015(4) 0.005(3) C10F 0.029(3) 0.032(3) 0.047(4) -0.007(3) -0.008(3) 0.002(3) C11F 0.039(4) 0.042(4) 0.042(5) -0.011(4) 0.011(3) -0.001(4) C12F 0.033(4) 0.037(4) 0.034(4) -0.007(3) 0.016(3) -0.001(3) C13F 0.028(4) 0.040(4) 0.040(4) -0.006(3) 0.003(3) -0.001(3) O2G 0.031(2) 0.024(4) 0.035(2) -0.001(3) -0.0061(16) -0.012(2) C8G 0.037(2) 0.026(2) 0.037(5) 0.006(3) -0.015(2) -0.005(2) C9G 0.042(3) 0.024(4) 0.036(7) -0.004(5) -0.015(4) 0.005(3) C10G 0.029(3) 0.032(3) 0.047(4) -0.007(3) -0.008(3) 0.002(3) C11G 0.039(4) 0.042(4) 0.042(5) -0.011(4) 0.011(3) -0.001(4) C12G 0.033(4) 0.037(4) 0.034(4) -0.007(3) 0.016(3) -0.001(3) C13G 0.028(4) 0.040(4) 0.040(4) -0.006(3) 0.003(3) -0.001(3) O1 0.0486(19) 0.0267(15) 0.0267(17) -0.0025(12) 0.0033(12) 0.0001(13) O3 0.0401(16) 0.0276(15) 0.0301(16) -0.0024(12) 0.0109(12) 0.0009(12) O4 0.0455(16) 0.0312(15) 0.0306(16) -0.0023(12) -0.0015(12) 0.0137(13) O5 0.0384(16) 0.0361(16) 0.0273(16) -0.0015(13) 0.0065(12) -0.0006(12) O6 0.0386(15) 0.0242(14) 0.0291(16) -0.0014(12) 0.0036(11) 0.0027(11) O7 0.0486(17) 0.0207(14) 0.0316(17) 0.0040(12) 0.0079(12) 0.0025(13) O8 0.0534(19) 0.0341(16) 0.058(2) 0.0096(14) -0.0269(16) -0.0133(14) C1 0.038(2) 0.023(2) 0.019(2) 0.0008(16) -0.0047(16) 0.0027(17) C2 0.050(2) 0.0163(19) 0.019(2) 0.0037(16) -0.0083(17) 0.0004(17) C3 0.042(2) 0.022(2) 0.030(2) 0.0028(17) -0.0144(18) -0.0071(18) C4 0.035(2) 0.022(2) 0.032(2) 0.0020(17) -0.0117(17) -0.0002(17) C5K 0.038(2) 0.0170(19) 0.022(2) 0.0017(15) -0.0062(16) 0.0033(16) C6 0.040(2) 0.0172(19) 0.017(2) 0.0040(15) -0.0036(16) -0.0016(16) C7 0.037(2) 0.0183(18) 0.022(2) 0.0007(16) -0.0002(16) 0.0014(16) C14 0.0287(19) 0.0176(18) 0.023(2) -0.0046(16) 0.0043(15) -0.0058(16) C15 0.0278(19) 0.0173(18) 0.023(2) 0.0008(15) 0.0019(15) -0.0064(15) C16 0.0211(18) 0.0203(19) 0.030(2) 0.0007(16) -0.0011(15) -0.0027(15) C17 0.0229(18) 0.0189(18) 0.024(2) -0.0011(15) 0.0025(15) -0.0029(15) C18 0.0249(19) 0.0221(19) 0.022(2) -0.0002(16) -0.0040(15) -0.0062(16) C19 0.0254(19) 0.0167(18) 0.028(2) -0.0020(16) 0.0019(15) -0.0049(15) C20 0.0246(19) 0.0228(19) 0.031(2) -0.0014(16) 0.0009(15) -0.0016(15) C21 0.0232(19) 0.0202(19) 0.031(2) -0.0006(16) -0.0024(16) -0.0025(16) C22 0.031(2) 0.027(2) 0.026(2) -0.0006(17) -0.0014(16) 0.0017(16) C23 0.036(2) 0.031(2) 0.026(2) -0.0062(17) 0.0021(17) -0.0009(17) C24 0.046(2) 0.042(2) 0.029(2) -0.0051(19) 0.0061(18) 0.008(2) C25 0.047(3) 0.109(5) 0.042(3) -0.025(3) 0.000(2) -0.003(3) C26 0.115(4) 0.104(5) 0.065(4) -0.007(3) -0.003(3) -0.072(4) C27 0.0245(19) 0.026(2) 0.025(2) 0.0012(17) 0.0011(15) 0.0077(16) C28 0.0234(19) 0.0185(19) 0.028(2) 0.0005(16) -0.0008(15) 0.0042(15) C29 0.0248(19) 0.023(2) 0.026(2) -0.0025(16) -0.0031(15) 0.0044(16) C30 0.0261(19) 0.024(2) 0.023(2) 0.0017(16) -0.0016(15) 0.0066(16) C31 0.0257(19) 0.0219(19) 0.030(2) 0.0026(17) -0.0006(16) 0.0030(15) C32 0.0230(19) 0.021(2) 0.032(2) -0.0022(16) 0.0003(16) 0.0020(15) C33 0.037(2) 0.0198(19) 0.029(2) -0.0002(16) 0.0068(17) 0.0044(16) C34 0.0261(19) 0.022(2) 0.026(2) -0.0009(17) -0.0026(15) 0.0082(16) C35 0.035(2) 0.028(2) 0.027(2) -0.0007(17) -0.0019(16) -0.0012(17) C36 0.034(2) 0.027(2) 0.033(2) 0.0013(17) 0.0054(17) -0.0044(17) C37 0.044(2) 0.028(2) 0.033(2) -0.0023(18) 0.0057(18) -0.0032(18) C38 0.069(3) 0.036(2) 0.052(3) -0.007(2) 0.025(2) -0.014(2) C39 0.090(4) 0.046(3) 0.074(4) -0.008(3) 0.041(3) -0.026(3) C40 0.041(2) 0.0193(19) 0.022(2) -0.0042(16) 0.0043(17) -0.0009(17) C41 0.039(2) 0.0174(19) 0.024(2) -0.0043(16) 0.0009(16) 0.0038(17) C42 0.047(2) 0.0177(19) 0.026(2) -0.0022(16) -0.0028(17) -0.0005(18) C43 0.044(2) 0.019(2) 0.032(2) -0.0021(17) -0.0122(18) -0.0024(17) C44 0.046(2) 0.022(2) 0.032(2) -0.0044(18) -0.0146(18) -0.0030(18) C45 0.056(3) 0.018(2) 0.020(2) -0.0031(16) -0.0065(18) 0.0036(18) C46 0.055(3) 0.0185(19) 0.023(2) -0.0009(16) -0.0084(18) -0.0053(18) C47 0.049(3) 0.023(2) 0.044(3) -0.0025(19) -0.015(2) -0.0058(19) C48 0.045(2) 0.023(2) 0.045(3) 0.0073(19) -0.0094(19) -0.0050(18) C49 0.042(2) 0.030(2) 0.049(3) 0.006(2) -0.013(2) -0.0041(19) C50 0.037(2) 0.035(2) 0.059(3) 0.004(2) -0.010(2) -0.0061(19) C51 0.046(3) 0.055(3) 0.063(3) -0.008(3) -0.013(2) 0.006(2) C52 0.057(3) 0.061(3) 0.073(4) -0.015(3) -0.006(3) 0.004(3) O1A 0.0378(15) 0.0294(14) 0.0273(16) 0.0014(11) 0.0022(11) 0.0060(11) O2A 0.0553(17) 0.0302(15) 0.0323(17) 0.0047(13) -0.0031(13) 0.0154(13) O3A 0.0451(15) 0.0181(13) 0.0275(15) 0.0001(11) 0.0038(11) -0.0028(11) O4A 0.0359(14) 0.0211(14) 0.0327(16) -0.0006(12) 0.0016(11) -0.0011(11) O5A 0.0338(15) 0.0250(14) 0.0323(16) 0.0005(11) 0.0041(11) 0.0032(12) O6A 0.0298(16) 0.0345(17) 0.091(3) -0.0021(16) 0.0080(15) 0.0054(13) O7A 0.0498(16) 0.0287(14) 0.0215(15) -0.0003(11) 0.0065(12) 0.0051(12) C1A 0.032(2) 0.0169(19) 0.024(2) -0.0005(16) 0.0033(16) -0.0016(16) C2A 0.033(2) 0.0144(18) 0.026(2) 0.0010(16) 0.0014(16) 0.0001(16) C3A 0.034(2) 0.0188(19) 0.030(2) -0.0027(16) 0.0052(16) 0.0029(16) C4A 0.0292(19) 0.0197(19) 0.025(2) 0.0019(16) 0.0024(16) -0.0001(16) C5A 0.029(2) 0.0192(19) 0.032(2) 0.0020(16) 0.0020(16) 0.0020(16) C6A 0.029(2) 0.0141(18) 0.029(2) 0.0001(16) 0.0050(16) 0.0010(15) C7K 0.0282(19) 0.0198(19) 0.033(2) -0.0003(16) 0.0039(16) -0.0004(16) C8A 0.028(2) 0.025(2) 0.030(2) -0.0014(18) -0.0007(16) -0.0003(17) C9A 0.041(2) 0.024(2) 0.029(2) -0.0006(17) 0.0018(17) 0.0018(17) C10A 0.043(2) 0.028(2) 0.027(2) -0.0005(17) -0.0001(17) -0.0007(18) C11A 0.039(2) 0.047(3) 0.030(2) -0.003(2) -0.0010(18) 0.0052(19) C12A 0.055(3) 0.038(3) 0.070(4) -0.023(2) 0.021(2) -0.007(2) C13A 0.090(4) 0.097(4) 0.147(4) -0.050(3) 0.038(3) -0.018(3) C14A 0.028(2) 0.021(2) 0.026(2) 0.0014(17) 0.0068(16) 0.0059(16) C15A 0.0238(19) 0.0212(19) 0.029(2) -0.0004(16) 0.0057(16) 0.0006(15) C16A 0.0249(19) 0.022(2) 0.028(2) -0.0011(17) 0.0018(15) 0.0028(15) C17A 0.0278(19) 0.0185(19) 0.025(2) -0.0003(16) 0.0039(16) 0.0023(15) C18A 0.0243(19) 0.0188(19) 0.028(2) -0.0043(16) 0.0053(16) 0.0014(15) C19A 0.029(2) 0.022(2) 0.022(2) -0.0031(16) 0.0053(15) 0.0019(16) C20A 0.038(2) 0.0213(19) 0.020(2) -0.0031(16) 0.0052(16) 0.0032(16) C21A 0.0215(18) 0.023(2) 0.032(2) -0.0046(17) 0.0041(16) -0.0002(16) C22A 0.044(2) 0.021(2) 0.029(2) -0.0003(17) 0.0004(17) -0.0017(17) C23A 0.040(2) 0.027(2) 0.030(2) 0.0005(17) -0.0012(17) -0.0037(17) C24A 0.034(2) 0.025(2) 0.032(2) 0.0022(17) 0.0014(17) 0.0004(17) C25A 0.039(2) 0.034(2) 0.042(3) 0.0060(19) -0.0017(19) 0.0007(18) C26A 0.037(2) 0.039(2) 0.049(3) 0.013(2) 0.0007(19) -0.0028(19) C27A 0.038(2) 0.025(2) 0.015(2) 0.0003(16) -0.0022(16) 0.0001(17) C28A 0.031(2) 0.025(2) 0.018(2) -0.0026(16) -0.0019(15) 0.0063(16) C29A 0.033(2) 0.026(2) 0.023(2) -0.0045(16) -0.0052(16) 0.0070(17) C30A 0.033(2) 0.027(2) 0.030(2) -0.0049(17) -0.0015(16) 0.0045(17) C31A 0.030(2) 0.031(2) 0.028(2) -0.0062(17) -0.0036(16) 0.0068(18) C32A 0.032(2) 0.027(2) 0.018(2) -0.0027(16) -0.0027(15) 0.0063(17) C33A 0.037(2) 0.028(2) 0.027(2) -0.0033(17) -0.0028(17) 0.0125(17) C34A 0.033(2) 0.033(2) 0.054(3) -0.005(2) 0.0021(19) 0.0021(19) C35A 0.033(2) 0.029(2) 0.082(4) -0.008(2) 0.008(2) 0.0032(19) C36A 0.028(2) 0.032(2) 0.061(3) -0.004(2) -0.0027(19) 0.0052(18) C37A 0.045(3) 0.041(3) 0.064(3) -0.011(2) -0.018(2) 0.011(2) C38A 0.066(3) 0.058(3) 0.046(3) -0.006(2) -0.015(2) 0.027(3) C39A 0.124(5) 0.084(4) 0.051(4) -0.019(3) -0.033(3) 0.060(4) C40A 0.036(2) 0.0190(19) 0.029(2) 0.0051(17) 0.0024(17) 0.0169(17) C41A 0.036(2) 0.0208(19) 0.024(2) 0.0000(16) -0.0031(16) 0.0141(17) C42A 0.030(2) 0.024(2) 0.032(2) 0.0011(17) -0.0024(17) 0.0102(16) C43A 0.032(2) 0.026(2) 0.027(2) 0.0007(17) -0.0003(16) 0.0129(17) C44A 0.035(2) 0.026(2) 0.022(2) -0.0026(16) -0.0011(16) 0.0139(17) C45A 0.032(2) 0.0205(19) 0.024(2) -0.0006(16) -0.0008(16) 0.0099(16) C46A 0.040(2) 0.0206(19) 0.025(2) -0.0011(16) 0.0011(16) 0.0062(17) O8A 0.030(3) 0.073(2) 0.0296(19) 0.0056(16) 0.0014(15) 0.013(3) C47A 0.038(3) 0.030(2) 0.028(3) 0.001(2) 0.002(2) 0.009(2) C48A 0.045(3) 0.041(3) 0.034(3) -0.004(3) 0.002(2) 0.004(2) C49A 0.045(3) 0.053(3) 0.047(3) 0.004(3) 0.006(2) 0.003(3) C50A 0.050(4) 0.052(3) 0.061(4) 0.003(3) 0.007(3) 0.007(3) C51A 0.038(3) 0.060(4) 0.051(4) -0.007(3) 0.003(3) -0.003(3) C52A 0.079(5) 0.053(4) 0.093(8) -0.024(5) -0.008(5) 0.007(3) O8B 0.030(3) 0.073(2) 0.0296(19) 0.0056(16) 0.0014(15) 0.013(3) C47B 0.038(3) 0.030(2) 0.028(3) 0.001(2) 0.002(2) 0.009(2) C48B 0.045(3) 0.041(3) 0.034(3) -0.004(3) 0.002(2) 0.004(2) C49B 0.045(3) 0.053(3) 0.047(3) 0.004(3) 0.006(2) 0.003(3) C50B 0.050(4) 0.052(3) 0.061(4) 0.003(3) 0.007(3) 0.007(3) C51B 0.038(3) 0.060(4) 0.051(4) -0.007(3) 0.003(3) -0.003(3) C52B 0.079(5) 0.053(4) 0.093(8) -0.024(5) -0.008(5) 0.007(3) N1G 0.0284(16) 0.0219(16) 0.0319(19) 0.0028(14) -0.0005(13) 0.0058(13) C1G 0.0271(19) 0.024(2) 0.031(2) 0.0026(17) 0.0030(16) 0.0027(16) C2G 0.040(2) 0.031(2) 0.039(3) -0.0035(19) 0.0070(18) 0.0066(18) C3G 0.033(2) 0.027(2) 0.051(3) 0.0070(19) 0.0057(19) 0.0007(17) C4G 0.032(2) 0.033(2) 0.049(3) 0.010(2) 0.0056(19) 0.0025(18) _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 O2 C8 1.271(19) . ? C8 C4 1.475(14) . ? C8 C9 1.523(14) . ? C9 C10 1.509(10) . ? C10 C11 1.530(12) . ? C11 C12 1.525(12) . ? C12 C13 1.537(10) . ? O2F C8F 1.23(2) . ? C8F C4 1.52(2) . ? C8F C9F 1.53(2) . ? C9F C10F 1.53(2) . ? C10F C11F 1.54(2) . ? C11F C12F 1.52(2) . ? C12F C13F 1.54(2) . ? O2G C8G 1.23(2) . ? C8G C4 1.478(15) . ? C8G C9G 1.524(16) . ? C9G C10G 1.512(11) . ? C10G C11G 1.536(11) . ? C11G C12G 1.521(11) . ? C12G C13G 1.535(14) . ? O1 C1 1.365(4) . ? O3 C14 1.384(4) . ? O4 C21 1.219(4) . ? O5 C27 1.379(4) . ? O6 C34 1.226(4) . ? O7 C40 1.380(4) . ? O8 C47 1.229(5) . ? C1 C2 1.397(5) . ? C1 C6 1.400(5) . ? C2 C3 1.384(5) . ? C2 C46 1.524(5) . ? C3 C4 1.395(5) . ? C4 C5K 1.395(5) . ? C5K C6 1.371(5) . ? C6 C7 1.523(5) . ? C7 C15 1.523(5) . ? C14 C19 1.390(5) . ? C14 C15 1.397(5) . ? C15 C16 1.381(5) . ? C16 C17 1.395(5) . ? C17 C18 1.394(5) . ? C17 C21 1.498(5) . ? C18 C19 1.391(5) . ? C19 C20 1.526(5) . ? C20 C28 1.521(5) . ? C21 C22 1.510(5) . ? C22 C23 1.521(5) . ? C23 C24 1.523(5) . ? C24 C25 1.501(6) . ? C25 C26 1.510(7) . ? C27 C28 1.396(5) . ? C27 C32 1.411(5) . ? C28 C29 1.386(5) . ? C29 C30 1.402(5) . ? C30 C31 1.395(5) . ? C30 C34 1.490(5) . ? C31 C32 1.390(5) . ? C32 C33 1.520(5) . ? C33 C41 1.515(5) . ? C34 C35 1.503(5) . ? C35 C36 1.521(5) . ? C36 C37 1.516(5) . ? C37 C38 1.517(5) . ? C38 C39 1.524(6) . ? C40 C41 1.390(5) . ? C40 C45 1.398(5) . ? C41 C42 1.384(5) . ? C42 C43 1.398(5) . ? C43 C44 1.389(5) . ? C43 C47 1.489(5) . ? C44 C45 1.391(5) . ? C45 C46 1.526(5) . ? C47 C48 1.511(5) . ? C48 C49 1.525(5) . ? C49 C50 1.525(6) . ? C50 C51 1.523(6) . ? C51 C52 1.527(6) . ? O1A C1A 1.348(4) . ? O2A C8A 1.236(4) . ? O3A C14A 1.330(4) . ? O4A C21A 1.244(4) . ? O5A C27A 1.356(4) . ? O6A C34A 1.217(4) . ? O7A C40A 1.358(4) . ? C1A C2A 1.403(5) . ? C1A C6A 1.409(5) . ? C2A C3A 1.382(5) . ? C2A C46A 1.521(5) . ? C3A C4A 1.394(5) . ? C4A C5A 1.401(5) . ? C4A C8A 1.465(5) . ? C5A C6A 1.375(5) . ? C6A C7K 1.524(5) . ? C7K C15A 1.513(5) . ? C8A C9A 1.513(5) . ? C9A C10A 1.514(5) . ? C10A C11A 1.510(5) . ? C11A C12A 1.518(6) . ? C12A C13A 1.462(7) . ? C14A C15A 1.405(5) . ? C14A C19A 1.416(5) . ? C15A C16A 1.389(5) . ? C16A C17A 1.403(5) . ? C17A C18A 1.401(5) . ? C17A C21A 1.472(5) . ? C18A C19A 1.382(5) . ? C19A C20A 1.520(5) . ? C20A C28A 1.506(5) . ? C21A C22A 1.509(5) . ? C22A C23A 1.520(5) . ? C23A C24A 1.527(5) . ? C24A C25A 1.522(5) . ? C25A C26A 1.527(5) . ? C27A C32A 1.390(5) . ? C27A C28A 1.411(5) . ? C28A C29A 1.391(5) . ? C29A C30A 1.386(5) . ? C30A C31A 1.402(5) . ? C30A C34A 1.481(5) . ? C31A C32A 1.379(5) . ? C32A C33A 1.534(5) . ? C33A C41A 1.519(5) . ? C34A C35A 1.522(5) . ? C35A C36A 1.520(6) . ? C36A C37A 1.518(6) . ? C37A C38A 1.510(6) . ? C38A C39A 1.520(6) . ? C40A C41A 1.405(5) . ? C40A C45A 1.406(5) . ? C41A C42A 1.390(5) . ? C42A C43A 1.397(5) . ? C43A C44A 1.389(5) . ? C43A C47A 1.481(7) . ? C43A C47B 1.50(2) . ? C44A C45A 1.388(5) . ? C45A C46A 1.522(5) . ? O8A C47A 1.227(7) . ? C47A C48A 1.509(7) . ? C48A C49A 1.513(7) . ? C49A C50A 1.541(7) . ? C50A C51A 1.508(7) . ? C51A C52A 1.528(8) . ? O8B C47B 1.20(4) . ? C47B C48B 1.53(2) . ? C48B C49B 1.520(19) . ? C49B C50B 1.568(18) . ? C50B C51B 1.494(18) . ? C51B C52B 1.50(2) . ? N1G C1G 1.511(4) . ? C1G C2G 1.516(5) . ? C1G C4G 1.520(5) . ? C1G C3G 1.522(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C8 C4 119.1(11) . . ? O2 C8 C9 117.5(11) . . ? C4 C8 C9 123.4(13) . . ? C10 C9 C8 111.3(11) . . ? C9 C10 C11 117.1(7) . . ? C12 C11 C10 110.3(8) . . ? C11 C12 C13 112.6(8) . . ? O2F C8F C4 118(2) . . ? O2F C8F C9F 119(2) . . ? C4 C8F C9F 117(2) . . ? C10F C9F C8F 116(4) . . ? C9F C10F C11F 108(3) . . ? C12F C11F C10F 112(3) . . ? C11F C12F C13F 109(3) . . ? O2G C8G C4 121.7(13) . . ? O2G C8G C9G 120.5(12) . . ? C4 C8G C9G 117.8(14) . . ? C10G C9G C8G 110.0(10) . . ? C9G C10G C11G 114.7(7) . . ? C12G C11G C10G 112.9(8) . . ? C11G C12G C13G 112.7(9) . . ? O1 C1 C2 117.9(3) . . ? O1 C1 C6 119.8(3) . . ? C2 C1 C6 122.2(3) . . ? C3 C2 C1 118.1(3) . . ? C3 C2 C46 120.6(3) . . ? C1 C2 C46 121.2(3) . . ? C2 C3 C4 121.2(3) . . ? C3 C4 C5K 118.4(3) . . ? C3 C4 C8 123.3(7) . . ? C5K C4 C8 118.2(7) . . ? C3 C4 C8G 120.8(8) . . ? C5K C4 C8G 120.7(8) . . ? C8 C4 C8G 7(2) . . ? C3 C4 C8F 128.5(19) . . ? C5K C4 C8F 111.5(15) . . ? C8 C4 C8F 11(2) . . ? C8G C4 C8F 17(2) . . ? C6 C5K C4 122.5(3) . . ? C5K C6 C1 117.4(3) . . ? C5K C6 C7 120.5(3) . . ? C1 C6 C7 122.1(3) . . ? C15 C7 C6 112.0(3) . . ? O3 C14 C19 120.0(3) . . ? O3 C14 C15 117.4(3) . . ? C19 C14 C15 122.6(3) . . ? C16 C15 C14 117.1(3) . . ? C16 C15 C7 120.8(3) . . ? C14 C15 C7 122.0(3) . . ? C15 C16 C17 122.3(3) . . ? C18 C17 C16 118.7(3) . . ? C18 C17 C21 122.8(3) . . ? C16 C17 C21 118.4(3) . . ? C19 C18 C17 120.7(3) . . ? C14 C19 C18 118.5(3) . . ? C14 C19 C20 121.2(3) . . ? C18 C19 C20 120.3(3) . . ? C28 C20 C19 112.1(3) . . ? O4 C21 C17 119.5(3) . . ? O4 C21 C22 120.9(3) . . ? C17 C21 C22 119.6(3) . . ? C21 C22 C23 114.3(3) . . ? C22 C23 C24 113.1(3) . . ? C25 C24 C23 114.5(3) . . ? C24 C25 C26 113.6(4) . . ? O5 C27 C28 118.3(3) . . ? O5 C27 C32 119.5(3) . . ? C28 C27 C32 122.2(3) . . ? C29 C28 C27 118.1(3) . . ? C29 C28 C20 118.4(3) . . ? C27 C28 C20 123.4(3) . . ? C28 C29 C30 121.7(3) . . ? C31 C30 C29 118.5(3) . . ? C31 C30 C34 123.7(3) . . ? C29 C30 C34 117.8(3) . . ? C32 C31 C30 122.0(3) . . ? C31 C32 C27 117.4(3) . . ? C31 C32 C33 120.7(3) . . ? C27 C32 C33 121.9(3) . . ? C41 C33 C32 112.0(3) . . ? O6 C34 C30 120.0(3) . . ? O6 C34 C35 120.0(3) . . ? C30 C34 C35 120.0(3) . . ? C34 C35 C36 113.8(3) . . ? C37 C36 C35 112.4(3) . . ? C36 C37 C38 113.7(3) . . ? C37 C38 C39 112.6(3) . . ? O7 C40 C41 117.4(3) . . ? O7 C40 C45 119.6(3) . . ? C41 C40 C45 123.0(3) . . ? C42 C41 C40 117.7(3) . . ? C42 C41 C33 120.5(3) . . ? C40 C41 C33 121.5(3) . . ? C41 C42 C43 121.6(3) . . ? C44 C43 C42 118.5(3) . . ? C44 C43 C47 119.1(3) . . ? C42 C43 C47 122.3(3) . . ? C43 C44 C45 122.2(4) . . ? C44 C45 C40 116.9(3) . . ? C44 C45 C46 119.7(3) . . ? C40 C45 C46 123.4(3) . . ? C2 C46 C45 112.3(3) . . ? O8 C47 C43 120.0(4) . . ? O8 C47 C48 120.8(4) . . ? C43 C47 C48 119.3(3) . . ? C47 C48 C49 113.9(3) . . ? C50 C49 C48 114.3(3) . . ? C51 C50 C49 113.6(3) . . ? C50 C51 C52 112.6(4) . . ? O1A C1A C2A 118.7(3) . . ? O1A C1A C6A 121.0(3) . . ? C2A C1A C6A 120.3(3) . . ? C3A C2A C1A 119.2(3) . . ? C3A C2A C46A 120.3(3) . . ? C1A C2A C46A 120.4(3) . . ? C2A C3A C4A 121.8(3) . . ? C3A C4A C5A 117.6(3) . . ? C3A C4A C8A 123.0(3) . . ? C5A C4A C8A 119.3(3) . . ? C6A C5A C4A 122.5(3) . . ? C5A C6A C1A 118.6(3) . . ? C5A C6A C7K 119.8(3) . . ? C1A C6A C7K 121.6(3) . . ? C15A C7K C6A 113.2(3) . . ? O2A C8A C4A 120.0(3) . . ? O2A C8A C9A 119.2(3) . . ? C4A C8A C9A 120.8(3) . . ? C8A C9A C10A 114.7(3) . . ? C11A C10A C9A 113.4(3) . . ? C10A C11A C12A 114.6(3) . . ? C13A C12A C11A 116.2(4) . . ? O3A C14A C15A 121.0(3) . . ? O3A C14A C19A 119.1(3) . . ? C15A C14A C19A 119.8(3) . . ? C16A C15A C14A 119.4(3) . . ? C16A C15A C7K 120.6(3) . . ? C14A C15A C7K 120.0(3) . . ? C15A C16A C17A 121.8(3) . . ? C18A C17A C16A 117.7(3) . . ? C18A C17A C21A 119.7(3) . . ? C16A C17A C21A 122.6(3) . . ? C19A C18A C17A 122.2(3) . . ? C18A C19A C14A 119.1(3) . . ? C18A C19A C20A 121.2(3) . . ? C14A C19A C20A 119.7(3) . . ? C28A C20A C19A 113.5(3) . . ? O4A C21A C17A 120.0(3) . . ? O4A C21A C22A 118.6(3) . . ? C17A C21A C22A 121.3(3) . . ? C21A C22A C23A 114.2(3) . . ? C22A C23A C24A 114.2(3) . . ? C25A C24A C23A 112.5(3) . . ? C24A C25A C26A 112.3(3) . . ? O5A C27A C32A 117.4(3) . . ? O5A C27A C28A 120.9(3) . . ? C32A C27A C28A 121.7(3) . . ? C29A C28A C27A 117.0(3) . . ? C29A C28A C20A 120.2(3) . . ? C27A C28A C20A 122.8(3) . . ? C30A C29A C28A 122.9(3) . . ? C29A C30A C31A 118.0(3) . . ? C29A C30A C34A 123.0(3) . . ? C31A C30A C34A 118.9(3) . . ? C32A C31A C30A 121.4(3) . . ? C31A C32A C27A 119.0(3) . . ? C31A C32A C33A 119.9(3) . . ? C27A C32A C33A 121.1(3) . . ? C41A C33A C32A 113.1(3) . . ? O6A C34A C30A 121.2(3) . . ? O6A C34A C35A 119.5(3) . . ? C30A C34A C35A 119.2(3) . . ? C36A C35A C34A 113.1(3) . . ? C37A C36A C35A 112.5(4) . . ? C38A C37A C36A 114.6(4) . . ? C37A C38A C39A 112.6(5) . . ? O7A C40A C41A 120.3(3) . . ? O7A C40A C45A 117.9(3) . . ? C41A C40A C45A 121.7(3) . . ? C42A C41A C40A 117.7(3) . . ? C42A C41A C33A 120.0(3) . . ? C40A C41A C33A 122.4(3) . . ? C41A C42A C43A 121.9(3) . . ? C44A C43A C42A 118.7(3) . . ? C44A C43A C47A 120.4(4) . . ? C42A C43A C47A 120.9(4) . . ? C44A C43A C47B 113.1(12) . . ? C42A C43A C47B 128.2(12) . . ? C47A C43A C47B 7.7(13) . . ? C45A C44A C43A 121.8(3) . . ? C44A C45A C40A 118.0(3) . . ? C44A C45A C46A 120.3(3) . . ? C40A C45A C46A 121.5(3) . . ? C2A C46A C45A 109.9(3) . . ? O8A C47A C43A 121.0(5) . . ? O8A C47A C48A 118.4(5) . . ? C43A C47A C48A 120.2(5) . . ? C47A C48A C49A 115.5(5) . . ? C48A C49A C50A 112.3(5) . . ? C51A C50A C49A 114.4(5) . . ? C50A C51A C52A 109.3(6) . . ? O8B C47B C43A 121(2) . . ? O8B C47B C48B 120(2) . . ? C43A C47B C48B 116(2) . . ? C49B C48B C47B 111(3) . . ? C48B C49B C50B 109.1(17) . . ? C51B C50B C49B 109.5(18) . . ? C50B C51B C52B 125(3) . . ? N1G C1G C2G 107.5(3) . . ? N1G C1G C4G 106.5(3) . . ? C2G C1G C4G 110.7(3) . . ? N1G C1G C3G 107.9(3) . . ? C2G C1G C3G 111.6(3) . . ? C4G C1G C3G 112.3(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 23.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.767 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.063