# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1275 data_global _publ_contact_letter ; this is the CIF submission for two crystal structures for the paper (your ref. 9/01718F) 'N-Nitrosopiperidines with chirality solely due to hindered rotation about the N-N bond: enantioselective inclusion complexation with optically active hosts' by T. Olszewska, M.J. Milewska, M. Gdaniec, T. Polonski sent for publication in Chem. Commun. On Febryary 25, 1999 we have forwarded the cif file for this paper to Prof. Roberts (ccomm@liverpool.ac.uk) to whom the manuscript have been submitted. ; _publ_contact_author ; Maria Gdaniec Faculty of Chemistry A.Mickiewicz University 60-780 Pozna\'n Poland ; _publ_contact_author_phone '48 61 8699181 ext. 489' _publ_contact_author_fax '48 61 8658 008' _publ_contact_author_email mg31@krystal.amu.edu.pl loop_ _publ_author_name _publ_author_address 'Olszewska, T.' ; Department of Chemistry Technical University of Gda\'nsk 80952 Gda\'nsk Poland ; 'Milewska, M.J.' ; Department of Chemistry Technical University of Gda\'nsk 80952 Gda\'nsk Poland ; 'Gdaniec, M.' ; Faculty of Chemistry A. Mickiewicz University 60-780 Pozna\'n Poland ; 'Polo\'nski, T.' ; Department of Chemistry Technical University of Gda\'nsk 80952 Gda\'nsk Poland ; _publ_requested_journal 'Chemical Communication' data_4-2(5b) _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(R,R)-(-)-trans-2,3-bis(diphenylhydroxymethyl)-1,4-dioxaspiro(4.4)nonane N-nitroso-4-benzylpiperidine 2:1 clathrate ; _chemical_melting_point 130C _chemical_formula_moiety '2 (C33 H32 O4).C12 H16 N2 O1' _chemical_formula_sum 'C78 H80 N2 O9' _chemical_formula_weight 1189.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 35.720(7) _cell_length_b 8.605(2) _cell_length_c 23.661(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.94(3) _cell_angle_gamma 90.00 _cell_volume 6425.0(24) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5 _cell_measurement_theta_max 22 _exptl_crystal_description PLATE _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 0.632 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'KM-4 four-circle diffractometer' _diffrn_measurement_method '\w/2\q scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 1.5 _diffrn_reflns_number 4792 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 60.04 _reflns_number_total 4710 _reflns_number_observed 3928 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Kuma KM-4 sofware (Kuma Diffraction, 1991)' _computing_cell_refinement 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_data_reduction 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Stereochemical Workstation (Siemens Analytical X-Ray Instruments, Inc., 1989)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 319 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+0.8612P] 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 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00075(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(25) _refine_ls_number_reflns 4391 _refine_ls_number_parameters 812 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_obs 0.0404 _refine_ls_wR_factor_all 0.1139 _refine_ls_wR_factor_obs 0.1020 _refine_ls_goodness_of_fit_all 1.069 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.126 _refine_ls_restrained_S_obs 1.134 _refine_ls_shift/esd_max -0.013 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group N2G N 0.16892(12) 0.1939(6) 0.0396(2) 0.078(2) Uani 0.800(13) d PD . O1G O 0.17683(11) 0.2226(5) 0.0953(2) 0.076(2) Uani 0.800(13) d PD . N2'G N 0.1703(2) 0.1535(14) 0.0717(6) 0.083(10) Uiso 0.200(13) d PD . O1'G O 0.1753(4) 0.2805(13) 0.0516(9) 0.088(9) Uiso 0.200(13) d PD . N1G N 0.15913(9) 0.0443(5) 0.0257(2) 0.0816(12) Uani 1 d D . C2G C 0.1566(2) -0.0779(7) 0.0651(2) 0.088(2) Uani 1 d D . H22G H 0.1285(2) -0.1187(7) 0.0492(2) 0.105 Uiso 1 d R . H21G H 0.1655(2) -0.0365(7) 0.1071(2) 0.105 Uiso 1 d R . C3G C 0.1863(2) -0.2083(7) 0.0687(2) 0.0778(14) Uani 1 d . . H32G H 0.2149(2) -0.1710(7) 0.0916(2) 0.093 Uiso 1 d R . H31G H 0.1836(2) -0.2960(7) 0.0916(2) 0.093 Uiso 1 d R . C4G C 0.17848(15) -0.2599(5) 0.0021(2) 0.0588(11) Uani 1 d . . H4G H 0.15039(15) -0.3024(5) -0.0195(2) 0.071 Uiso 1 d R . C5G C 0.1803(2) -0.1202(6) -0.0359(2) 0.0709(13) Uani 1 d . . H52G H 0.1728(2) -0.1527(6) -0.0787(2) 0.085 Uiso 1 d R . H51G H 0.2088(2) -0.0817(6) -0.0167(2) 0.085 Uiso 1 d R . C6G C 0.1502(2) 0.0098(7) -0.0388(2) 0.092(2) Uani 1 d D . H62G H 0.1550(2) 0.1011(7) -0.0579(2) 0.110 Uiso 1 d R . H61G H 0.1213(2) -0.0221(7) -0.0645(2) 0.110 Uiso 1 d R . C7G C 0.2088(2) -0.3893(7) 0.0058(2) 0.0809(15) Uani 1 d . . H72G H 0.2110(2) -0.4668(7) 0.0364(2) 0.097 Uiso 1 d R . H71G H 0.2363(2) -0.3431(7) 0.0205(2) 0.097 Uiso 1 d R . C8G C 0.1975(2) -0.4594(7) -0.0581(2) 0.0747(14) Uani 1 d . . C9G C 0.1646(2) -0.5665(7) -0.0845(3) 0.098(2) Uani 1 d . . H9G H 0.1509(2) -0.5998(7) -0.0600(3) 0.118 Uiso 1 d R . C10G C 0.1512(3) -0.6262(10) -0.1437(4) 0.135(3) Uani 1 d . . H10G H 0.1280(3) -0.6981(10) -0.1600(4) 0.162 Uiso 1 d R . C11G C 0.1702(5) -0.5864(14) -0.1774(5) 0.164(5) Uani 1 d . . H11G H 0.1588(5) -0.6267(14) -0.2201(5) 0.196 Uiso 1 d R . C12G C 0.2034(4) -0.4819(14) -0.1547(5) 0.154(4) Uani 1 d . . H12G H 0.2174(4) -0.4600(14) -0.1799(5) 0.185 Uiso 1 d R . C13G C 0.2172(2) -0.4177(9) -0.0931(3) 0.109(2) Uani 1 d . . H13G H 0.2403(2) -0.3449(9) -0.0776(3) 0.131 Uiso 1 d R . O1A O 0.11301(7) 0.3305(3) 0.27242(10) 0.0442(6) Uani 1 d . . C2A C 0.06983(11) 0.3346(5) 0.2254(2) 0.0449(9) Uani 1 d . . O3A O 0.07101(7) 0.3100(3) 0.16644(10) 0.0461(6) Uani 1 d . . C4A C 0.11248(10) 0.3447(4) 0.1750(2) 0.0385(8) Uani 1 d . . H4A H 0.12569(10) 0.2490(4) 0.1731(2) 0.046 Uiso 1 d R . C5A C 0.13603(10) 0.4075(4) 0.24471(14) 0.0375(8) Uani 1 d . . H5A H 0.13147(10) 0.5176(4) 0.24426(14) 0.045 Uiso 1 d R . C6A C 0.18358(11) 0.3728(4) 0.2853(2) 0.0389(8) Uani 1 d . . C7A C 0.10826(11) 0.4512(5) 0.1198(2) 0.0416(9) Uani 1 d . . C8A C 0.19298(11) 0.1990(5) 0.2898(2) 0.0419(9) Uani 1 d . . C9A C 0.20675(12) 0.1277(5) 0.2502(2) 0.0517(10) Uani 1 d . . H9A H 0.21042(12) 0.1884(5) 0.2191(2) 0.062 Uiso 1 d R . C10A C 0.21508(14) -0.0305(6) 0.2546(2) 0.0646(12) Uani 1 d . . H10A H 0.22452(14) -0.0770(6) 0.2266(2) 0.078 Uiso 1 d R . C11A C 0.20986(14) -0.1175(6) 0.2978(2) 0.0735(14) Uani 1 d . . H11A H 0.21582(14) -0.2268(6) 0.3003(2) 0.088 Uiso 1 d R . C12A C 0.1964(2) -0.0524(6) 0.3378(3) 0.0724(14) Uani 1 d . . H12A H 0.1923(2) -0.1157(6) 0.3679(3) 0.087 Uiso 1 d R . C13A C 0.18841(13) 0.1060(6) 0.3341(2) 0.0563(11) Uani 1 d . . H13A H 0.17979(13) 0.1533(6) 0.3629(2) 0.068 Uiso 1 d R . C14A C 0.20174(12) 0.4446(5) 0.3525(2) 0.0455(9) Uani 1 d . . C15A C 0.24470(14) 0.4497(7) 0.3885(2) 0.0750(15) Uani 1 d . . H15A H 0.26184(14) 0.4074(7) 0.3708(2) 0.090 Uiso 1 d R . C16A C 0.2638(2) 0.5173(9) 0.4484(2) 0.102(2) Uani 1 d . . H16A H 0.2942(2) 0.5137(9) 0.4722(2) 0.122 Uiso 1 d R . C17A C 0.2400(2) 0.5816(8) 0.4732(2) 0.088(2) Uani 1 d . . H17A H 0.2538(2) 0.6278(8) 0.5150(2) 0.105 Uiso 1 d R . C18A C 0.1972(2) 0.5775(8) 0.4383(2) 0.088(2) Uani 1 d . . H18A H 0.1797(2) 0.6275(8) 0.4538(2) 0.106 Uiso 1 d R . C19A C 0.17799(14) 0.5109(6) 0.3782(2) 0.0669(13) Uani 1 d . . H19A H 0.14766(14) 0.5073(6) 0.3539(2) 0.080 Uiso 1 d R . C20A C 0.08767(12) 0.6053(5) 0.1204(2) 0.0456(9) Uani 1 d . . C21A C 0.04396(13) 0.6215(5) 0.0878(2) 0.0548(11) Uani 1 d . . H21A H 0.02694(13) 0.5353(5) 0.0636(2) 0.066 Uiso 1 d R . C22A C 0.0245(2) 0.7585(6) 0.0900(2) 0.0663(12) Uani 1 d . . H22A H -0.0058(2) 0.7675(6) 0.0666(2) 0.080 Uiso 1 d R . C23A C 0.0487(2) 0.8814(6) 0.1255(2) 0.0755(14) Uani 1 d . . H23A H 0.0351(2) 0.9770(6) 0.1264(2) 0.091 Uiso 1 d R . C24A C 0.0922(2) 0.8680(6) 0.1583(2) 0.0729(13) Uani 1 d . . H24A H 0.1090(2) 0.9527(6) 0.1843(2) 0.088 Uiso 1 d R . C25A C 0.11178(14) 0.7310(5) 0.1557(2) 0.0551(11) Uani 1 d . . H25A H 0.14211(14) 0.7223(5) 0.1777(2) 0.066 Uiso 1 d R . C26A C 0.08554(11) 0.3731(5) 0.0546(2) 0.0462(9) Uani 1 d . . C27A C 0.08297(13) 0.4524(6) 0.0021(2) 0.0600(11) Uani 1 d . . H27A H 0.09430(13) 0.5556(6) 0.0073(2) 0.072 Uiso 1 d R . C28A C 0.0655(2) 0.3857(8) -0.0578(2) 0.080(2) Uani 1 d . . H28A H 0.0631(2) 0.4413(8) -0.0945(2) 0.096 Uiso 1 d R . C29A C 0.0502(2) 0.2368(8) -0.0660(2) 0.088(2) Uani 1 d . . H29A H 0.0389(2) 0.1878(8) -0.1072(2) 0.106 Uiso 1 d R . C30A C 0.0519(2) 0.1566(7) -0.0148(2) 0.083(2) Uani 1 d . . H30A H 0.0411(2) 0.0523(7) -0.0211(2) 0.099 Uiso 1 d R . C31A C 0.06950(14) 0.2241(6) 0.0456(2) 0.0638(12) Uani 1 d . . H31A H 0.06967(14) 0.1680(6) 0.0808(2) 0.077 Uiso 1 d R . C32A C 0.04576(13) 0.2069(5) 0.2389(2) 0.0548(10) Uani 1 d . . H32B H 0.06505(13) 0.1265(5) 0.2639(2) 0.066 Uiso 1 d R . H32A H 0.02467(13) 0.1629(5) 0.1995(2) 0.066 Uiso 1 d R . C33A C 0.0256(2) 0.2805(7) 0.2747(3) 0.089(2) Uani 1 d . . H33B H 0.0358(2) 0.2330(7) 0.3160(3) 0.107 Uiso 1 d R . H33A H -0.0046(2) 0.2685(7) 0.2518(3) 0.107 Uiso 1 d R . C34A C 0.0370(2) 0.4519(7) 0.2816(3) 0.0805(15) Uani 1 d . . H34B H 0.0135(2) 0.5152(7) 0.2766(3) 0.097 Uiso 1 d R . H34A H 0.0607(2) 0.4724(7) 0.3227(3) 0.097 Uiso 1 d R . C35A C 0.04829(13) 0.4829(6) 0.2282(2) 0.0573(11) Uani 1 d . . H35B H 0.02350(13) 0.5044(6) 0.1885(2) 0.069 Uiso 1 d R . H35A H 0.06770(13) 0.5683(6) 0.2387(2) 0.069 Uiso 1 d R . O2A O 0.20534(8) 0.4516(3) 0.25633(12) 0.0483(7) Uani 1 d . . H2OA H 0.18693(8) 0.4835(3) 0.21060(12) 0.058 Uiso 1 d R . O4A O 0.15118(7) 0.4843(3) 0.13127(11) 0.0454(6) Uani 1 d . . H4OA H 0.15967(7) 0.3992(3) 0.11073(11) 0.054 Uiso 1 d R . O1B O -0.12947(7) -0.0294(4) 0.29502(11) 0.0527(7) Uani 1 d . . C2B C -0.16512(11) -0.0248(5) 0.3065(2) 0.0493(9) Uani 1 d . . O3B O -0.14804(7) -0.0176(4) 0.37369(12) 0.0515(7) Uani 1 d . . C4B C -0.10412(11) -0.0566(5) 0.4034(2) 0.0434(9) Uani 1 d . . H4B H -0.08802(11) 0.0367(5) 0.4206(2) 0.052 Uiso 1 d R . C5B C -0.09691(10) -0.1105(5) 0.34749(15) 0.0390(8) Uani 1 d . . H5B H -0.10247(10) -0.2199(5) 0.34115(15) 0.047 Uiso 1 d R . C6B C -0.05424(11) -0.0753(4) 0.3487(2) 0.0393(8) Uani 1 d . . C7B C -0.09418(11) -0.1688(5) 0.4591(2) 0.0468(9) Uani 1 d . . C8B C -0.04267(12) 0.0973(5) 0.3596(2) 0.0446(9) Uani 1 d . . C9B C -0.0095(2) 0.1512(6) 0.4157(2) 0.0647(12) Uani 1 d . . H9B H 0.0066(2) 0.0785(6) 0.4491(2) 0.078 Uiso 1 d R . C10B C 0.0011(2) 0.3052(7) 0.4241(3) 0.084(2) Uani 1 d . . H10B H 0.0239(2) 0.3388(7) 0.4641(3) 0.101 Uiso 1 d R . C11B C -0.0209(2) 0.4108(6) 0.3780(3) 0.084(2) Uani 1 d . . H11B H -0.0125(2) 0.5181(6) 0.3845(3) 0.101 Uiso 1 d R . C12B C -0.0542(2) 0.3606(6) 0.3216(3) 0.0760(15) Uani 1 d . . H12B H -0.0707(2) 0.4347(6) 0.2891(3) 0.091 Uiso 1 d R . C13B C -0.06492(14) 0.2038(5) 0.3121(2) 0.0610(11) Uani 1 d . . H13B H -0.08756(14) 0.1686(5) 0.2722(2) 0.073 Uiso 1 d R . C14B C -0.05330(11) -0.1307(5) 0.2876(2) 0.0448(9) Uani 1 d . . C15B C -0.01680(14) -0.1031(5) 0.2827(2) 0.0593(11) Uani 1 d . . H15B H 0.00656(14) -0.0503(5) 0.3168(2) 0.071 Uiso 1 d R . C16B C -0.0126(2) -0.1545(6) 0.2307(2) 0.0732(13) Uani 1 d . . H16B H 0.0127(2) -0.1323(6) 0.2277(2) 0.088 Uiso 1 d R . C17B C -0.0449(2) -0.2344(6) 0.1821(2) 0.0732(13) Uani 1 d . . H17B H -0.0416(2) -0.2708(6) 0.1464(2) 0.088 Uiso 1 d R . C18B C -0.0809(2) -0.2640(7) 0.1869(2) 0.0745(14) Uani 1 d . . H18B H -0.1039(2) -0.3176(7) 0.1527(2) 0.089 Uiso 1 d R . C19B C -0.08517(13) -0.2132(6) 0.2394(2) 0.0598(11) Uani 1 d . . H19B H -0.11024(13) -0.2371(6) 0.2429(2) 0.072 Uiso 1 d R . C20B C -0.11924(12) -0.3188(5) 0.4368(2) 0.0474(9) Uani 1 d . . C21B C -0.16048(12) -0.3262(5) 0.4278(2) 0.0531(10) Uani 1 d . . H21B H -0.17252(12) -0.2354(5) 0.4365(2) 0.064 Uiso 1 d R . C22B C -0.1836(2) -0.4599(7) 0.4075(2) 0.0705(13) Uani 1 d . . H22B H -0.2122(2) -0.4631(7) 0.4011(2) 0.085 Uiso 1 d R . C23B C -0.1663(2) -0.5909(7) 0.3956(3) 0.101(2) Uani 1 d . . H23B H -0.1820(2) -0.6861(7) 0.3819(3) 0.121 Uiso 1 d R . C24B C -0.1265(2) -0.5847(7) 0.4022(3) 0.100(2) Uani 1 d . . H24B H -0.1146(2) -0.6737(7) 0.3918(3) 0.120 Uiso 1 d R . C25B C -0.1023(2) -0.4494(6) 0.4239(2) 0.0709(13) Uani 1 d . . H25B H -0.0736(2) -0.4476(6) 0.4307(2) 0.085 Uiso 1 d R . C26B C -0.10105(13) -0.0951(8) 0.5127(2) 0.0686(15) Uani 1 d . . C27B C -0.0940(2) -0.1904(10) 0.5644(2) 0.100(2) Uani 1 d . . H27B H -0.0859(2) -0.2962(10) 0.5632(2) 0.120 Uiso 1 d R . C28B C -0.0998(2) -0.1303(18) 0.6147(3) 0.152(5) Uani 1 d . . H28B H -0.0929(2) -0.1972(18) 0.6507(3) 0.182 Uiso 1 d R . C29B C -0.1125(3) 0.0207(22) 0.6125(5) 0.196(8) Uani 1 d . . H29B H -0.1174(3) 0.0556(22) 0.6470(5) 0.235 Uiso 1 d R . C30B C -0.1190(2) 0.1127(15) 0.5625(4) 0.162(5) Uani 1 d . . H30B H -0.1274(2) 0.2179(15) 0.5642(4) 0.194 Uiso 1 d R . C31B C -0.1134(2) 0.0555(9) 0.5117(3) 0.096(2) Uani 1 d . . H31B H -0.1188(2) 0.1218(9) 0.4761(3) 0.116 Uiso 1 d R . C32B C -0.1922(2) 0.1153(6) 0.2736(2) 0.0749(14) Uani 1 d . . H32D H -0.1746(2) 0.2017(6) 0.2756(2) 0.090 Uiso 1 d R . H32C H -0.2091(2) 0.1431(6) 0.2937(2) 0.090 Uiso 1 d R . C33B C -0.2210(2) 0.0647(8) 0.2061(3) 0.099(2) Uani 1 d . . H33D H -0.2499(2) 0.0951(8) 0.1915(3) 0.119 Uiso 1 d R . H33C H -0.2112(2) 0.1108(8) 0.1785(3) 0.119 Uiso 1 d R . C34B C -0.2176(2) -0.1108(8) 0.2044(2) 0.081(2) Uani 1 d . . H34D H -0.2452(2) -0.1573(8) 0.1827(2) 0.097 Uiso 1 d R . H34C H -0.2014(2) -0.1417(8) 0.1834(2) 0.097 Uiso 1 d R . C35B C -0.19426(12) -0.1605(6) 0.2748(2) 0.0564(10) Uani 1 d . . H35D H -0.17824(12) -0.2544(6) 0.2812(2) 0.068 Uiso 1 d R . H35C H -0.21406(12) -0.1744(6) 0.2912(2) 0.068 Uiso 1 d R . O2B O -0.02344(7) -0.1689(3) 0.39943(11) 0.0472(6) Uani 1 d . . H2OB H -0.03335(7) -0.1639(3) 0.44064(11) 0.057 Uiso 1 d R . O4B O -0.04972(7) -0.2015(4) 0.48580(11) 0.0648(9) Uani 1 d . . H4OB H -0.03825(7) -0.2371(4) 0.51908(11) 0.078 Uiso 1 d 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 N2G 0.083(4) 0.071(5) 0.078(4) 0.009(4) 0.037(3) 0.021(3) O1G 0.073(3) 0.087(4) 0.060(3) -0.019(3) 0.024(2) 0.012(2) N1G 0.095(3) 0.056(3) 0.094(3) -0.018(2) 0.044(3) -0.009(2) C2G 0.109(4) 0.088(4) 0.075(3) -0.016(3) 0.051(3) -0.011(3) C3G 0.097(4) 0.075(4) 0.056(3) 0.004(3) 0.031(3) -0.004(3) C4G 0.066(3) 0.053(3) 0.053(2) 0.001(2) 0.024(2) -0.003(2) C5G 0.094(4) 0.053(3) 0.071(3) 0.006(2) 0.043(3) 0.003(3) C6G 0.134(5) 0.065(4) 0.084(3) 0.006(3) 0.057(3) 0.014(3) C7G 0.088(4) 0.069(3) 0.070(3) 0.011(3) 0.025(3) 0.018(3) C8G 0.086(4) 0.063(3) 0.069(3) 0.012(3) 0.031(3) 0.028(3) C9G 0.124(5) 0.069(4) 0.086(4) 0.003(3) 0.036(3) 0.017(4) C10G 0.181(8) 0.097(6) 0.094(5) -0.027(4) 0.037(5) 0.027(6) C11G 0.257(14) 0.132(9) 0.105(6) -0.001(6) 0.088(8) 0.092(9) C12G 0.221(11) 0.150(9) 0.147(8) 0.065(7) 0.134(8) 0.114(8) C13G 0.124(5) 0.112(5) 0.112(5) 0.034(4) 0.073(4) 0.053(4) O1A 0.0347(14) 0.058(2) 0.0385(12) 0.0061(12) 0.0154(11) -0.0007(12) C2A 0.034(2) 0.056(2) 0.042(2) 0.007(2) 0.016(2) -0.002(2) O3A 0.0342(13) 0.058(2) 0.0413(12) 0.0012(12) 0.0137(11) -0.0067(12) C4A 0.033(2) 0.037(2) 0.042(2) 0.002(2) 0.015(2) 0.000(2) C5A 0.037(2) 0.037(2) 0.038(2) 0.0028(15) 0.017(2) 0.001(2) C6A 0.035(2) 0.040(2) 0.037(2) 0.000(2) 0.012(2) -0.002(2) C7A 0.037(2) 0.048(2) 0.038(2) 0.003(2) 0.016(2) 0.001(2) C8A 0.030(2) 0.047(2) 0.044(2) 0.002(2) 0.012(2) -0.001(2) C9A 0.045(2) 0.057(3) 0.046(2) -0.001(2) 0.016(2) 0.002(2) C10A 0.058(3) 0.053(3) 0.070(3) -0.011(2) 0.020(2) 0.005(2) C11A 0.053(3) 0.047(3) 0.094(4) -0.004(3) 0.013(3) 0.004(2) C12A 0.066(3) 0.054(3) 0.089(3) 0.024(3) 0.029(3) -0.002(2) C13A 0.053(3) 0.058(3) 0.058(2) 0.008(2) 0.026(2) 0.000(2) C14A 0.041(2) 0.048(3) 0.040(2) -0.001(2) 0.012(2) -0.001(2) C15A 0.049(3) 0.100(4) 0.057(2) -0.021(3) 0.009(2) 0.008(3) C16A 0.054(3) 0.154(7) 0.065(3) -0.041(4) 0.001(2) 0.001(4) C17A 0.079(4) 0.105(5) 0.054(2) -0.025(3) 0.011(3) 0.004(3) C18A 0.083(4) 0.116(5) 0.058(3) -0.030(3) 0.027(3) 0.007(3) C19A 0.051(2) 0.094(4) 0.051(2) -0.016(2) 0.019(2) 0.000(2) C20A 0.049(3) 0.046(2) 0.040(2) 0.006(2) 0.020(2) 0.004(2) C21A 0.053(3) 0.058(3) 0.051(2) 0.010(2) 0.023(2) 0.009(2) C22A 0.066(3) 0.070(3) 0.063(3) 0.015(2) 0.030(2) 0.023(3) C23A 0.100(4) 0.056(3) 0.084(3) 0.012(3) 0.054(3) 0.027(3) C24A 0.097(4) 0.046(3) 0.078(3) -0.004(2) 0.043(3) -0.001(3) C25A 0.064(3) 0.042(3) 0.057(2) 0.004(2) 0.026(2) 0.000(2) C26A 0.039(2) 0.055(3) 0.038(2) -0.003(2) 0.013(2) 0.001(2) C27A 0.063(3) 0.069(3) 0.042(2) 0.002(2) 0.020(2) 0.003(2) C28A 0.082(4) 0.101(4) 0.046(2) 0.006(3) 0.022(2) 0.007(3) C29A 0.076(4) 0.123(6) 0.044(3) -0.025(3) 0.011(2) -0.004(4) C30A 0.078(3) 0.086(4) 0.068(3) -0.028(3) 0.021(3) -0.028(3) C31A 0.061(3) 0.070(3) 0.051(2) -0.012(2) 0.018(2) -0.018(2) C32A 0.044(2) 0.061(3) 0.058(2) 0.008(2) 0.023(2) -0.007(2) C33A 0.103(4) 0.081(4) 0.122(4) 0.021(3) 0.085(4) 0.004(3) C34A 0.094(4) 0.077(4) 0.098(4) 0.008(3) 0.068(3) 0.011(3) C35A 0.049(2) 0.062(3) 0.063(2) 0.013(2) 0.029(2) 0.009(2) O2A 0.0396(14) 0.055(2) 0.0480(14) 0.0060(12) 0.0188(12) -0.0073(13) O4A 0.0426(14) 0.052(2) 0.0456(12) 0.0010(12) 0.0239(11) -0.0051(12) O1B 0.0337(13) 0.068(2) 0.0517(14) 0.0173(14) 0.0159(12) 0.0017(13) C2B 0.036(2) 0.053(2) 0.055(2) 0.008(2) 0.019(2) 0.005(2) O3B 0.0356(15) 0.058(2) 0.0556(15) -0.0024(13) 0.0171(12) 0.0062(13) C4B 0.031(2) 0.046(2) 0.048(2) -0.007(2) 0.014(2) -0.005(2) C5B 0.032(2) 0.039(2) 0.041(2) 0.003(2) 0.013(2) -0.002(2) C6B 0.035(2) 0.039(2) 0.043(2) 0.001(2) 0.017(2) 0.001(2) C7B 0.032(2) 0.065(3) 0.042(2) -0.004(2) 0.016(2) -0.003(2) C8B 0.044(2) 0.043(2) 0.056(2) -0.002(2) 0.031(2) -0.005(2) C9B 0.070(3) 0.053(3) 0.069(3) -0.013(2) 0.031(2) -0.017(2) C10B 0.101(4) 0.070(4) 0.088(3) -0.030(3) 0.050(3) -0.032(3) C11B 0.107(4) 0.046(3) 0.136(5) -0.023(4) 0.087(4) -0.021(3) C12B 0.084(4) 0.043(3) 0.125(4) 0.015(3) 0.068(4) 0.008(3) C13B 0.057(3) 0.050(3) 0.082(3) 0.012(2) 0.038(2) 0.004(2) C14B 0.045(2) 0.037(2) 0.050(2) 0.004(2) 0.021(2) 0.001(2) C15B 0.061(3) 0.053(3) 0.077(3) -0.014(2) 0.042(2) -0.009(2) C16B 0.086(3) 0.064(3) 0.100(3) -0.010(3) 0.068(3) -0.010(3) C17B 0.099(4) 0.070(3) 0.067(3) -0.006(3) 0.052(3) 0.003(3) C18B 0.078(3) 0.079(4) 0.060(3) -0.020(2) 0.027(2) -0.009(3) C19B 0.051(2) 0.073(3) 0.050(2) -0.010(2) 0.019(2) -0.011(2) C20B 0.044(2) 0.058(3) 0.042(2) 0.007(2) 0.021(2) 0.003(2) C21B 0.044(2) 0.060(3) 0.051(2) -0.001(2) 0.020(2) -0.003(2) C22B 0.061(3) 0.076(4) 0.076(3) -0.012(3) 0.033(2) -0.019(3) C23B 0.125(5) 0.062(4) 0.140(5) -0.020(4) 0.084(4) -0.032(4) C24B 0.126(5) 0.054(3) 0.150(6) -0.008(4) 0.091(5) 0.000(4) C25B 0.074(3) 0.059(3) 0.094(3) 0.009(3) 0.051(3) 0.010(3) C26B 0.034(2) 0.121(5) 0.047(2) -0.030(3) 0.017(2) -0.020(3) C27B 0.080(4) 0.175(7) 0.051(3) -0.018(4) 0.035(2) -0.046(4) C28B 0.090(5) 0.319(15) 0.059(4) -0.039(7) 0.045(4) -0.069(8) C29B 0.059(4) 0.420(23) 0.108(6) -0.161(12) 0.038(4) -0.048(8) C30B 0.065(4) 0.281(14) 0.123(6) -0.131(8) 0.030(4) -0.006(6) C31B 0.058(3) 0.127(6) 0.089(4) -0.065(4) 0.022(3) -0.010(3) C32B 0.058(3) 0.069(3) 0.086(3) 0.022(3) 0.024(3) 0.020(2) C33B 0.078(4) 0.105(5) 0.082(4) 0.034(3) 0.011(3) -0.001(3) C34B 0.050(3) 0.120(5) 0.059(3) 0.001(3) 0.014(2) -0.019(3) C35B 0.041(2) 0.065(3) 0.061(2) -0.001(2) 0.022(2) -0.008(2) O2B 0.0411(14) 0.049(2) 0.0480(13) 0.0086(12) 0.0181(12) 0.0068(13) O4B 0.0315(14) 0.114(3) 0.0427(13) 0.011(2) 0.0121(11) 0.008(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 N2G O1G 1.234(5) . ? N2G N1G 1.335(5) . ? N2'G O1'G 1.237(7) . ? N2'G N1G 1.350(7) . ? N1G C2G 1.435(7) . ? N1G C6G 1.437(7) . ? C2G C3G 1.517(8) . ? C2G H22G 0.96 . ? C2G H21G 0.96 . ? C3G C4G 1.533(6) . ? C3G H32G 0.96 . ? C3G H31G 0.96 . ? C4G C5G 1.521(6) . ? C4G C7G 1.527(7) . ? C4G H4G 0.96 . ? C5G C6G 1.530(7) . ? C5G H52G 0.96 . ? C5G H51G 0.96 . ? C6G H62G 0.96 . ? C6G H61G 0.96 . ? C7G C8G 1.497(7) . ? C7G H72G 0.96 . ? C7G H71G 0.96 . ? C8G C13G 1.363(8) . ? C8G C9G 1.391(8) . ? C9G C10G 1.351(9) . ? C9G H9G 0.96 . ? C10G C11G 1.309(14) . ? C10G H10G 0.96 . ? C11G C12G 1.381(14) . ? C11G H11G 0.96 . ? C12G C13G 1.414(12) . ? C12G H12G 0.96 . ? C13G H13G 0.96 . ? O1A C2A 1.417(4) . ? O1A C5A 1.432(4) . ? C2A O3A 1.432(4) . ? C2A C35A 1.507(6) . ? C2A C32A 1.518(6) . ? O3A C4A 1.430(4) . ? C4A C7A 1.544(5) . ? C4A C5A 1.556(5) . ? C4A H4A 0.96 . ? C5A C6A 1.539(5) . ? C5A H5A 0.96 . ? C6A O2A 1.426(4) . ? C6A C8A 1.525(6) . ? C6A C14A 1.538(5) . ? C7A O4A 1.455(4) . ? C7A C20A 1.520(6) . ? C7A C26A 1.522(5) . ? C8A C9A 1.388(5) . ? C8A C13A 1.388(5) . ? C9A C10A 1.387(7) . ? C9A H9A 0.96 . ? C10A C11A 1.349(7) . ? C10A H10A 0.96 . ? C11A C12A 1.366(7) . ? C11A H11A 0.96 . ? C12A C13A 1.387(7) . ? C12A H12A 0.96 . ? C13A H13A 0.96 . ? C14A C15A 1.363(6) . ? C14A C19A 1.378(6) . ? C15A C16A 1.381(6) . ? C15A H15A 0.96 . ? C16A C17A 1.357(7) . ? C16A H16A 0.96 . ? C17A C18A 1.354(8) . ? C17A H17A 0.96 . ? C18A C19A 1.381(6) . ? C18A H18A 0.96 . ? C19A H19A 0.96 . ? C20A C21A 1.387(6) . ? C20A C25A 1.391(6) . ? C21A C22A 1.383(6) . ? C21A H21A 0.96 . ? C22A C23A 1.375(7) . ? C22A H22A 0.96 . ? C23A C24A 1.380(7) . ? C23A H23A 0.96 . ? C24A C25A 1.386(7) . ? C24A H24A 0.96 . ? C25A H25A 0.96 . ? C26A C31A 1.380(6) . ? C26A C27A 1.381(5) . ? C27A C28A 1.379(6) . ? C27A H27A 0.96 . ? C28A C29A 1.370(9) . ? C28A H28A 0.96 . ? C29A C30A 1.372(8) . ? C29A H29A 0.96 . ? C30A C31A 1.390(6) . ? C30A H30A 0.96 . ? C31A H31A 0.96 . ? C32A C33A 1.486(7) . ? C32A H32B 0.96 . ? C32A H32A 0.96 . ? C33A C34A 1.518(8) . ? C33A H33B 0.96 . ? C33A H33A 0.96 . ? C34A C35A 1.519(6) . ? C34A H34B 0.96 . ? C34A H34A 0.96 . ? C35A H35B 0.96 . ? C35A H35A 0.96 . ? O2A H2OA 1.01 . ? O4A H4OA 1.00 . ? O1B C2B 1.422(4) . ? O1B C5B 1.424(4) . ? C2B O3B 1.411(4) . ? C2B C35B 1.510(6) . ? C2B C32B 1.513(6) . ? O3B C4B 1.426(4) . ? C4B C5B 1.533(5) . ? C4B C7B 1.535(5) . ? C4B H4B 0.96 . ? C5B C6B 1.541(5) . ? C5B H5B 0.96 . ? C6B O2B 1.436(4) . ? C6B C8B 1.531(6) . ? C6B C14B 1.537(5) . ? C7B O4B 1.435(4) . ? C7B C20B 1.517(6) . ? C7B C26B 1.538(6) . ? C8B C13B 1.378(6) . ? C8B C9B 1.381(6) . ? C9B C10B 1.367(8) . ? C9B H9B 0.96 . ? C10B C11B 1.352(8) . ? C10B H10B 0.96 . ? C11B C12B 1.378(8) . ? C11B H11B 0.96 . ? C12B C13B 1.391(7) . ? C12B H12B 0.96 . ? C13B H13B 0.96 . ? C14B C19B 1.373(5) . ? C14B C15B 1.383(5) . ? C15B C16B 1.380(6) . ? C15B H15B 0.96 . ? C16B C17B 1.372(7) . ? C16B H16B 0.96 . ? C17B C18B 1.363(7) . ? C17B H17B 0.96 . ? C18B C19B 1.392(6) . ? C18B H18B 0.96 . ? C19B H19B 0.96 . ? C20B C25B 1.376(6) . ? C20B C21B 1.388(5) . ? C21B C22B 1.365(7) . ? C21B H21B 0.96 . ? C22B C23B 1.376(8) . ? C22B H22B 0.96 . ? C23B C24B 1.357(9) . ? C23B H23B 0.96 . ? C24B C25B 1.397(8) . ? C24B H24B 0.96 . ? C25B H25B 0.96 . ? C26B C31B 1.366(9) . ? C26B C27B 1.393(8) . ? C27B C28B 1.399(11) . ? C27B H27B 0.96 . ? C28B C29B 1.37(2) . ? C28B H28B 0.96 . ? C29B C30B 1.35(2) . ? C29B H29B 0.96 . ? C30B C31B 1.398(9) . ? C30B H30B 0.96 . ? C31B H31B 0.96 . ? C32B C33B 1.502(8) . ? C32B H32D 0.96 . ? C32B H32C 0.96 . ? C33B C34B 1.517(9) . ? C33B H33D 0.96 . ? C33B H33C 0.96 . ? C34B C35B 1.533(6) . ? C34B H34D 0.96 . ? C34B H34C 0.96 . ? C35B H35D 0.96 . ? C35B H35C 0.96 . ? O2B H2OB 1.18 . ? O4B H4OB 0.76 . ? 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 O1G N2G N1G 111.1(5) . . ? O1'G N2'G N1G 110.3(9) . . ? N2G N1G C2G 129.4(4) . . ? N2'G N1G C2G 94.1(8) . . ? N2G N1G C6G 111.4(4) . . ? N2'G N1G C6G 146.7(8) . . ? C2G N1G C6G 119.2(4) . . ? N1G C2G C3G 109.0(4) . . ? N1G C2G H22G 112.7(2) . . ? C3G C2G H22G 109.1(3) . . ? N1G C2G H21G 108.0(3) . . ? C3G C2G H21G 109.4(3) . . ? H22G C2G H21G 108.5 . . ? C2G C3G C4G 111.7(4) . . ? C2G C3G H32G 108.3(3) . . ? C4G C3G H32G 108.0(3) . . ? C2G C3G H31G 111.2(3) . . ? C4G C3G H31G 109.5(3) . . ? H32G C3G H31G 107.9 . . ? C5G C4G C7G 112.6(4) . . ? C5G C4G C3G 110.0(4) . . ? C7G C4G C3G 111.7(4) . . ? C5G C4G H4G 108.0(3) . . ? C7G C4G H4G 106.8(3) . . ? C3G C4G H4G 107.4(3) . . ? C4G C5G C6G 112.4(4) . . ? C4G C5G H52G 109.0(2) . . ? C6G C5G H52G 108.8(3) . . ? C4G C5G H51G 108.8(3) . . ? C6G C5G H51G 109.7(3) . . ? H52G C5G H51G 108.0 . . ? N1G C6G C5G 107.6(4) . . ? N1G C6G H62G 109.3(3) . . ? C5G C6G H62G 110.1(3) . . ? N1G C6G H61G 111.6(2) . . ? C5G C6G H61G 110.1(3) . . ? H62G C6G H61G 108.2 . . ? C8G C7G C4G 112.7(4) . . ? C8G C7G H72G 111.7(3) . . ? C4G C7G H72G 110.8(3) . . ? C8G C7G H71G 106.2(3) . . ? C4G C7G H71G 107.3(3) . . ? H72G C7G H71G 107.9 . . ? C13G C8G C9G 118.0(6) . . ? C13G C8G C7G 122.4(6) . . ? C9G C8G C7G 119.6(5) . . ? C10G C9G C8G 122.1(8) . . ? C10G C9G H9G 118.8(6) . . ? C8G C9G H9G 119.1(4) . . ? C11G C10G C9G 120.0(10) . . ? C11G C10G H10G 121.4(7) . . ? C9G C10G H10G 118.6(6) . . ? C10G C11G C12G 121.9(10) . . ? C10G C11G H11G 117.4(7) . . ? C12G C11G H11G 120.5(7) . . ? C11G C12G C13G 118.4(9) . . ? C11G C12G H12G 119.3(7) . . ? C13G C12G H12G 122.1(6) . . ? C8G C13G C12G 119.6(8) . . ? C8G C13G H13G 122.4(4) . . ? C12G C13G H13G 118.0(6) . . ? C2A O1A C5A 106.1(2) . . ? O1A C2A O3A 104.0(3) . . ? O1A C2A C35A 112.2(3) . . ? O3A C2A C35A 114.6(3) . . ? O1A C2A C32A 109.4(3) . . ? O3A C2A C32A 112.1(3) . . ? C35A C2A C32A 104.6(3) . . ? C4A O3A C2A 109.4(2) . . ? O3A C4A C7A 108.7(3) . . ? O3A C4A C5A 103.4(2) . . ? C7A C4A C5A 118.7(3) . . ? O3A C4A H4A 108.3(2) . . ? C7A C4A H4A 109.0(2) . . ? C5A C4A H4A 108.3(2) . . ? O1A C5A C6A 109.1(3) . . ? O1A C5A C4A 100.6(3) . . ? C6A C5A C4A 119.0(3) . . ? O1A C5A H5A 109.3(2) . . ? C6A C5A H5A 109.3(2) . . ? C4A C5A H5A 109.1(2) . . ? O2A C6A C8A 110.3(3) . . ? O2A C6A C14A 104.2(3) . . ? C8A C6A C14A 110.5(3) . . ? O2A C6A C5A 107.4(3) . . ? C8A C6A C5A 112.1(3) . . ? C14A C6A C5A 112.0(3) . . ? O4A C7A C20A 107.4(3) . . ? O4A C7A C26A 106.9(3) . . ? C20A C7A C26A 111.3(3) . . ? O4A C7A C4A 106.4(3) . . ? C20A C7A C4A 111.5(3) . . ? C26A C7A C4A 113.0(3) . . ? C9A C8A C13A 117.3(4) . . ? C9A C8A C6A 121.5(3) . . ? C13A C8A C6A 121.2(4) . . ? C10A C9A C8A 121.0(4) . . ? C10A C9A H9A 119.3(3) . . ? C8A C9A H9A 119.6(2) . . ? C11A C10A C9A 120.0(5) . . ? C11A C10A H10A 120.7(3) . . ? C9A C10A H10A 119.3(3) . . ? C10A C11A C12A 121.1(5) . . ? C10A C11A H11A 119.1(3) . . ? C12A C11A H11A 119.9(3) . . ? C11A C12A C13A 119.2(5) . . ? C11A C12A H12A 120.4(3) . . ? C13A C12A H12A 120.4(3) . . ? C12A C13A C8A 121.4(5) . . ? C12A C13A H13A 119.8(3) . . ? C8A C13A H13A 118.8(3) . . ? C15A C14A C19A 117.2(4) . . ? C15A C14A C6A 117.7(4) . . ? C19A C14A C6A 125.0(3) . . ? C14A C15A C16A 121.6(5) . . ? C14A C15A H15A 118.5(2) . . ? C16A C15A H15A 119.8(3) . . ? C17A C16A C15A 120.5(5) . . ? C17A C16A H16A 121.7(3) . . ? C15A C16A H16A 117.8(3) . . ? C18A C17A C16A 118.9(5) . . ? C18A C17A H17A 121.8(3) . . ? C16A C17A H17A 119.3(3) . . ? C17A C18A C19A 120.9(5) . . ? C17A C18A H18A 120.4(3) . . ? C19A C18A H18A 118.6(3) . . ? C14A C19A C18A 120.9(4) . . ? C14A C19A H19A 118.5(2) . . ? C18A C19A H19A 120.6(3) . . ? C21A C20A C25A 118.3(4) . . ? C21A C20A C7A 120.4(4) . . ? C25A C20A C7A 121.2(3) . . ? C22A C21A C20A 121.3(5) . . ? C22A C21A H21A 119.5(3) . . ? C20A C21A H21A 119.2(3) . . ? C23A C22A C21A 119.7(4) . . ? C23A C22A H22A 120.4(3) . . ? C21A C22A H22A 119.9(3) . . ? C22A C23A C24A 120.0(5) . . ? C22A C23A H23A 119.5(3) . . ? C24A C23A H23A 120.4(3) . . ? C23A C24A C25A 120.3(5) . . ? C23A C24A H24A 119.7(3) . . ? C25A C24A H24A 119.9(3) . . ? C24A C25A C20A 120.4(4) . . ? C24A C25A H25A 120.4(3) . . ? C20A C25A H25A 119.2(2) . . ? C31A C26A C27A 118.2(4) . . ? C31A C26A C7A 123.5(4) . . ? C27A C26A C7A 118.2(4) . . ? C28A C27A C26A 121.7(5) . . ? C28A C27A H27A 118.5(3) . . ? C26A C27A H27A 119.8(2) . . ? C29A C28A C27A 119.6(5) . . ? C29A C28A H28A 118.6(3) . . ? C27A C28A H28A 121.8(3) . . ? C28A C29A C30A 119.7(5) . . ? C28A C29A H29A 120.3(3) . . ? C30A C29A H29A 120.1(3) . . ? C29A C30A C31A 120.7(6) . . ? C29A C30A H30A 118.8(3) . . ? C31A C30A H30A 120.5(3) . . ? C26A C31A C30A 120.1(5) . . ? C26A C31A H31A 120.0(2) . . ? C30A C31A H31A 119.8(3) . . ? C33A C32A C2A 106.5(4) . . ? C33A C32A H32B 110.9(3) . . ? C2A C32A H32B 109.7(2) . . ? C33A C32A H32A 110.6(3) . . ? C2A C32A H32A 110.3(2) . . ? H32B C32A H32A 108.9 . . ? C32A C33A C34A 107.4(4) . . ? C32A C33A H33B 110.2(3) . . ? C34A C33A H33B 110.5(3) . . ? C32A C33A H33A 110.5(3) . . ? C34A C33A H33A 109.8(3) . . ? H33B C33A H33A 108.5 . . ? C33A C34A C35A 104.1(4) . . ? C33A C34A H34B 111.3(3) . . ? C35A C34A H34B 110.8(3) . . ? C33A C34A H34A 110.6(4) . . ? C35A C34A H34A 111.1(3) . . ? H34B C34A H34A 108.9 . . ? C2A C35A C34A 103.2(4) . . ? C2A C35A H35B 112.1(2) . . ? C34A C35A H35B 111.4(3) . . ? C2A C35A H35A 109.7(2) . . ? C34A C35A H35A 111.2(3) . . ? H35B C35A H35A 109.2 . . ? C6A O2A H2OA 114.7(2) . . ? C7A O4A H4OA 107.3(2) . . ? C2B O1B C5B 106.6(3) . . ? O3B C2B O1B 105.3(3) . . ? O3B C2B C35B 115.3(3) . . ? O1B C2B C35B 110.7(3) . . ? O3B C2B C32B 112.3(4) . . ? O1B C2B C32B 109.6(4) . . ? C35B C2B C32B 103.6(3) . . ? C2B O3B C4B 109.9(3) . . ? O3B C4B C5B 103.7(3) . . ? O3B C4B C7B 109.3(3) . . ? C5B C4B C7B 119.0(3) . . ? O3B C4B H4B 108.3(2) . . ? C5B C4B H4B 107.9(2) . . ? C7B C4B H4B 108.2(2) . . ? O1B C5B C4B 101.9(3) . . ? O1B C5B C6B 108.5(3) . . ? C4B C5B C6B 119.3(3) . . ? O1B C5B H5B 108.7(2) . . ? C4B C5B H5B 109.0(2) . . ? C6B C5B H5B 109.0(2) . . ? O2B C6B C8B 111.3(3) . . ? O2B C6B C14B 105.4(3) . . ? C8B C6B C14B 109.7(3) . . ? O2B C6B C5B 105.6(3) . . ? C8B C6B C5B 112.4(3) . . ? C14B C6B C5B 112.2(3) . . ? O4B C7B C20B 109.7(3) . . ? O4B C7B C4B 105.3(3) . . ? C20B C7B C4B 112.1(3) . . ? O4B C7B C26B 106.7(3) . . ? C20B C7B C26B 109.9(3) . . ? C4B C7B C26B 112.8(4) . . ? C13B C8B C9B 117.9(4) . . ? C13B C8B C6B 120.1(4) . . ? C9B C8B C6B 122.0(4) . . ? C10B C9B C8B 121.3(5) . . ? C10B C9B H9B 119.5(4) . . ? C8B C9B H9B 119.1(3) . . ? C11B C10B C9B 121.1(5) . . ? C11B C10B H10B 119.8(3) . . ? C9B C10B H10B 119.0(4) . . ? C10B C11B C12B 118.9(5) . . ? C10B C11B H11B 119.9(3) . . ? C12B C11B H11B 121.2(3) . . ? C11B C12B C13B 120.5(5) . . ? C11B C12B H12B 119.7(3) . . ? C13B C12B H12B 119.7(3) . . ? C8B C13B C12B 120.2(5) . . ? C8B C13B H13B 119.4(3) . . ? C12B C13B H13B 120.4(3) . . ? C19B C14B C15B 117.7(4) . . ? C19B C14B C6B 124.6(3) . . ? C15B C14B C6B 117.6(3) . . ? C16B C15B C14B 121.4(4) . . ? C16B C15B H15B 119.0(3) . . ? C14B C15B H15B 119.6(2) . . ? C17B C16B C15B 120.4(4) . . ? C17B C16B H16B 119.4(3) . . ? C15B C16B H16B 120.1(3) . . ? C18B C17B C16B 118.7(4) . . ? C18B C17B H17B 121.5(3) . . ? C16B C17B H17B 119.8(3) . . ? C17B C18B C19B 121.1(5) . . ? C17B C18B H18B 119.4(3) . . ? C19B C18B H18B 119.5(3) . . ? C14B C19B C18B 120.6(4) . . ? C14B C19B H19B 118.8(2) . . ? C18B C19B H19B 120.6(3) . . ? C25B C20B C21B 118.3(4) . . ? C25B C20B C7B 121.5(3) . . ? C21B C20B C7B 120.2(4) . . ? C22B C21B C20B 121.0(4) . . ? C22B C21B H21B 120.3(3) . . ? C20B C21B H21B 118.7(3) . . ? C21B C22B C23B 120.5(4) . . ? C21B C22B H22B 120.2(3) . . ? C23B C22B H22B 119.4(3) . . ? C24B C23B C22B 119.4(5) . . ? C24B C23B H23B 119.3(4) . . ? C22B C23B H23B 121.3(3) . . ? C23B C24B C25B 120.6(5) . . ? C23B C24B H24B 120.1(4) . . ? C25B C24B H24B 119.3(3) . . ? C20B C25B C24B 120.1(5) . . ? C20B C25B H25B 119.8(3) . . ? C24B C25B H25B 120.1(3) . . ? C31B C26B C27B 119.8(5) . . ? C31B C26B C7B 123.5(5) . . ? C27B C26B C7B 116.7(6) . . ? C26B C27B C28B 119.4(9) . . ? C26B C27B H27B 117.7(4) . . ? C28B C27B H27B 122.9(7) . . ? C29B C28B C27B 119.8(10) . . ? C29B C28B H28B 123.1(7) . . ? C27B C28B H28B 117.1(7) . . ? C30B C29B C28B 120.5(8) . . ? C30B C29B H29B 122.4(7) . . ? C28B C29B H29B 117.0(7) . . ? C29B C30B C31B 120.8(11) . . ? C29B C30B H30B 116.6(7) . . ? C31B C30B H30B 122.7(7) . . ? C26B C31B C30B 119.6(8) . . ? C26B C31B H31B 120.7(3) . . ? C30B C31B H31B 119.7(7) . . ? C33B C32B C2B 105.7(5) . . ? C33B C32B H32D 112.6(3) . . ? C2B C32B H32D 110.3(3) . . ? C33B C32B H32C 108.8(3) . . ? C2B C32B H32C 110.0(3) . . ? H32D C32B H32C 109.3 . . ? C32B C33B C34B 107.0(5) . . ? C32B C33B H33D 112.9(3) . . ? C34B C33B H33D 110.3(3) . . ? C32B C33B H33C 108.5(3) . . ? C34B C33B H33C 109.6(4) . . ? H33D C33B H33C 108.5 . . ? C33B C34B C35B 105.0(5) . . ? C33B C34B H34D 110.8(3) . . ? C35B C34B H34D 111.4(2) . . ? C33B C34B H34C 111.4(4) . . ? C35B C34B H34C 109.3(3) . . ? H34D C34B H34C 108.9 . . ? C2B C35B C34B 102.8(4) . . ? C2B C35B H35D 110.6(2) . . ? C34B C35B H35D 112.7(3) . . ? C2B C35B H35C 111.2(2) . . ? C34B C35B H35C 110.1(2) . . ? H35D C35B H35C 109.3 . . ? C6B O2B H2OB 105.1(2) . . ? C7B O4B H2OB 111.7(2) . . ? C7B O4B H4OB 118.9(2) . . ? H2OB O4B H4OB 129.34(13) . . ? 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 O1G N2G N1G C2G 0.5(3) . . . . ? O1G N2G N1G C6G -179.5(2) . . . . ? O1'G N2'G N1G C2G 179.9(3) . . . . ? O1'G N2'G N1G C6G 0.2(5) . . . . ? N2G N1G C2G C3G -123.0(4) . . . . ? N2'G N1G C2G C3G -122.8(5) . . . . ? C6G N1G C2G C3G 57.0(4) . . . . ? N1G C2G C3G C4G -52.1(6) . . . . ? C2G C3G C4G C5G 53.2(6) . . . . ? C2G C3G C4G C7G 179.0(4) . . . . ? C7G C4G C5G C6G -179.3(4) . . . . ? C3G C4G C5G C6G -54.0(6) . . . . ? N2G N1G C6G C5G 123.3(4) . . . . ? N2'G N1G C6G C5G 122.9(7) . . . . ? C2G N1G C6G C5G -56.7(4) . . . . ? C4G C5G C6G N1G 53.0(6) . . . . ? C5G C4G C7G C8G -64.9(6) . . . . ? C3G C4G C7G C8G 170.7(5) . . . . ? C4G C7G C8G C13G 98.9(6) . . . . ? C4G C7G C8G C9G -78.4(6) . . . . ? C13G C8G C9G C10G -1.6(9) . . . . ? C7G C8G C9G C10G 175.8(6) . . . . ? C8G C9G C10G C11G 1.7(11) . . . . ? C9G C10G C11G C12G -1.1(14) . . . . ? C10G C11G C12G C13G 0.4(14) . . . . ? C9G C8G C13G C12G 0.9(8) . . . . ? C7G C8G C13G C12G -176.5(5) . . . . ? C11G C12G C13G C8G -0.3(11) . . . . ? C5A O1A C2A O3A 38.4(4) . . . . ? C5A O1A C2A C35A -86.0(3) . . . . ? C5A O1A C2A C32A 158.3(3) . . . . ? O1A C2A O3A C4A -19.7(4) . . . . ? C35A C2A O3A C4A 103.1(4) . . . . ? C32A C2A O3A C4A -137.8(3) . . . . ? C2A O3A C4A C7A -131.7(3) . . . . ? C2A O3A C4A C5A -4.7(4) . . . . ? C2A O1A C5A C6A -166.0(3) . . . . ? C2A O1A C5A C4A -40.1(3) . . . . ? O3A C4A C5A O1A 26.8(3) . . . . ? C7A C4A C5A O1A 147.2(3) . . . . ? O3A C4A C5A C6A 145.7(3) . . . . ? C7A C4A C5A C6A -93.9(4) . . . . ? O1A C5A C6A O2A -179.9(3) . . . . ? C4A C5A C6A O2A 65.7(4) . . . . ? O1A C5A C6A C8A 58.8(4) . . . . ? C4A C5A C6A C8A -55.6(4) . . . . ? O1A C5A C6A C14A -66.0(4) . . . . ? C4A C5A C6A C14A 179.6(3) . . . . ? O3A C4A C7A O4A 179.3(3) . . . . ? C5A C4A C7A O4A 61.6(4) . . . . ? O3A C4A C7A C20A 62.5(4) . . . . ? C5A C4A C7A C20A -55.2(4) . . . . ? O3A C4A C7A C26A -63.8(4) . . . . ? C5A C4A C7A C26A 178.5(3) . . . . ? O2A C6A C8A C9A -22.0(5) . . . . ? C14A C6A C8A C9A -136.7(4) . . . . ? C5A C6A C8A C9A 97.6(4) . . . . ? O2A C6A C8A C13A 157.5(3) . . . . ? C14A C6A C8A C13A 42.8(5) . . . . ? C5A C6A C8A C13A -82.9(4) . . . . ? C13A C8A C9A C10A 0.7(6) . . . . ? C6A C8A C9A C10A -179.8(4) . . . . ? C8A C9A C10A C11A 0.0(7) . . . . ? C9A C10A C11A C12A 0.0(7) . . . . ? C10A C11A C12A C13A -0.6(7) . . . . ? C11A C12A C13A C8A 1.3(7) . . . . ? C9A C8A C13A C12A -1.3(6) . . . . ? C6A C8A C13A C12A 179.2(4) . . . . ? O2A C6A C14A C15A -51.2(5) . . . . ? C8A C6A C14A C15A 67.3(5) . . . . ? C5A C6A C14A C15A -167.0(4) . . . . ? O2A C6A C14A C19A 125.5(4) . . . . ? C8A C6A C14A C19A -116.0(5) . . . . ? C5A C6A C14A C19A 9.8(6) . . . . ? C19A C14A C15A C16A 0.5(8) . . . . ? C6A C14A C15A C16A 177.5(5) . . . . ? C14A C15A C16A C17A -0.2(10) . . . . ? C15A C16A C17A C18A 0.3(11) . . . . ? C16A C17A C18A C19A -0.7(10) . . . . ? C15A C14A C19A C18A -0.9(8) . . . . ? C6A C14A C19A C18A -177.7(5) . . . . ? C17A C18A C19A C14A 1.0(10) . . . . ? O4A C7A C20A C21A 155.0(3) . . . . ? C26A C7A C20A C21A 38.4(4) . . . . ? C4A C7A C20A C21A -88.8(4) . . . . ? O4A C7A C20A C25A -27.9(4) . . . . ? C26A C7A C20A C25A -144.6(3) . . . . ? C4A C7A C20A C25A 88.3(4) . . . . ? C25A C20A C21A C22A 0.0(6) . . . . ? C7A C20A C21A C22A 177.1(3) . . . . ? C20A C21A C22A C23A -0.5(6) . . . . ? C21A C22A C23A C24A 0.5(7) . . . . ? C22A C23A C24A C25A -0.1(7) . . . . ? C23A C24A C25A C20A -0.4(7) . . . . ? C21A C20A C25A C24A 0.5(6) . . . . ? C7A C20A C25A C24A -176.6(3) . . . . ? O4A C7A C26A C31A 118.1(4) . . . . ? C20A C7A C26A C31A -124.9(4) . . . . ? C4A C7A C26A C31A 1.5(5) . . . . ? O4A C7A C26A C27A -58.0(4) . . . . ? C20A C7A C26A C27A 59.0(4) . . . . ? C4A C7A C26A C27A -174.7(3) . . . . ? C31A C26A C27A C28A -0.8(6) . . . . ? C7A C26A C27A C28A 175.6(4) . . . . ? C26A C27A C28A C29A -0.1(8) . . . . ? C27A C28A C29A C30A 1.0(9) . . . . ? C28A C29A C30A C31A -0.8(9) . . . . ? C27A C26A C31A C30A 0.9(6) . . . . ? C7A C26A C31A C30A -175.2(4) . . . . ? C29A C30A C31A C26A -0.1(8) . . . . ? O1A C2A C32A C33A 96.9(4) . . . . ? O3A C2A C32A C33A -148.2(4) . . . . ? C35A C2A C32A C33A -23.4(4) . . . . ? C2A C32A C33A C34A 0.9(6) . . . . ? C32A C33A C34A C35A 21.7(6) . . . . ? O1A C2A C35A C34A -81.9(4) . . . . ? O3A C2A C35A C34A 159.7(3) . . . . ? C32A C2A C35A C34A 36.6(4) . . . . ? C33A C34A C35A C2A -35.8(5) . . . . ? C5B O1B C2B O3B 32.4(4) . . . . ? C5B O1B C2B C35B -92.9(3) . . . . ? C5B O1B C2B C32B 153.5(3) . . . . ? O1B C2B O3B C4B -14.5(4) . . . . ? C35B C2B O3B C4B 107.9(4) . . . . ? C32B C2B O3B C4B -133.8(4) . . . . ? C2B O3B C4B C5B -7.4(4) . . . . ? C2B O3B C4B C7B -135.2(3) . . . . ? C2B O1B C5B C4B -35.9(4) . . . . ? C2B O1B C5B C6B -162.6(3) . . . . ? O3B C4B C5B O1B 26.1(3) . . . . ? C7B C4B C5B O1B 147.6(3) . . . . ? O3B C4B C5B C6B 145.4(3) . . . . ? C7B C4B C5B C6B -93.1(4) . . . . ? O1B C5B C6B O2B -175.9(3) . . . . ? C4B C5B C6B O2B 68.3(4) . . . . ? O1B C5B C6B C8B 62.6(4) . . . . ? C4B C5B C6B C8B -53.2(4) . . . . ? O1B C5B C6B C14B -61.5(4) . . . . ? C4B C5B C6B C14B -177.3(3) . . . . ? O3B C4B C7B O4B 179.9(3) . . . . ? C5B C4B C7B O4B 61.2(4) . . . . ? O3B C4B C7B C20B 60.7(4) . . . . ? C5B C4B C7B C20B -58.0(4) . . . . ? O3B C4B C7B C26B -64.0(4) . . . . ? C5B C4B C7B C26B 177.3(3) . . . . ? O2B C6B C8B C13B 171.0(3) . . . . ? C14B C6B C8B C13B 54.7(4) . . . . ? C5B C6B C8B C13B -70.8(4) . . . . ? O2B C6B C8B C9B -7.5(5) . . . . ? C14B C6B C8B C9B -123.7(4) . . . . ? C5B C6B C8B C9B 110.7(4) . . . . ? C13B C8B C9B C10B -0.1(7) . . . . ? C6B C8B C9B C10B 178.4(4) . . . . ? C8B C9B C10B C11B 0.9(8) . . . . ? C9B C10B C11B C12B -0.7(8) . . . . ? C10B C11B C12B C13B -0.2(7) . . . . ? C9B C8B C13B C12B -0.8(6) . . . . ? C6B C8B C13B C12B -179.3(4) . . . . ? C11B C12B C13B C8B 1.0(7) . . . . ? O2B C6B C14B C19B 109.6(4) . . . . ? C8B C6B C14B C19B -130.5(4) . . . . ? C5B C6B C14B C19B -4.9(5) . . . . ? O2B C6B C14B C15B -66.6(4) . . . . ? C8B C6B C14B C15B 53.3(5) . . . . ? C5B C6B C14B C15B 178.9(4) . . . . ? C19B C14B C15B C16B 0.9(7) . . . . ? C6B C14B C15B C16B 177.3(4) . . . . ? C14B C15B C16B C17B 0.3(8) . . . . ? C15B C16B C17B C18B -1.1(8) . . . . ? C16B C17B C18B C19B 0.8(8) . . . . ? C15B C14B C19B C18B -1.2(7) . . . . ? C6B C14B C19B C18B -177.4(4) . . . . ? C17B C18B C19B C14B 0.4(8) . . . . ? O4B C7B C20B C25B -21.1(5) . . . . ? C4B C7B C20B C25B 95.5(4) . . . . ? C26B C7B C20B C25B -138.2(4) . . . . ? O4B C7B C20B C21B 160.1(3) . . . . ? C4B C7B C20B C21B -83.3(4) . . . . ? C26B C7B C20B C21B 43.0(5) . . . . ? C25B C20B C21B C22B 0.8(6) . . . . ? C7B C20B C21B C22B 179.7(4) . . . . ? C20B C21B C22B C23B 0.1(7) . . . . ? C21B C22B C23B C24B -2.1(9) . . . . ? C22B C23B C24B C25B 3.1(10) . . . . ? C21B C20B C25B C24B 0.2(7) . . . . ? C7B C20B C25B C24B -178.7(4) . . . . ? C23B C24B C25B C20B -2.2(9) . . . . ? O4B C7B C26B C31B 113.3(5) . . . . ? C20B C7B C26B C31B -127.8(5) . . . . ? C4B C7B C26B C31B -1.9(5) . . . . ? O4B C7B C26B C27B -66.7(5) . . . . ? C20B C7B C26B C27B 52.2(5) . . . . ? C4B C7B C26B C27B 178.1(4) . . . . ? C31B C26B C27B C28B 0.0(7) . . . . ? C7B C26B C27B C28B -179.9(5) . . . . ? C26B C27B C28B C29B 0.4(10) . . . . ? C27B C28B C29B C30B -0.8(13) . . . . ? C28B C29B C30B C31B 0.6(13) . . . . ? C27B C26B C31B C30B -0.2(7) . . . . ? C7B C26B C31B C30B 179.8(4) . . . . ? C29B C30B C31B C26B -0.1(10) . . . . ? O3B C2B C32B C33B -158.0(4) . . . . ? O1B C2B C32B C33B 85.3(5) . . . . ? C35B C2B C32B C33B -32.9(5) . . . . ? C2B C32B C33B C34B 12.5(6) . . . . ? C32B C33B C34B C35B 12.3(7) . . . . ? O3B C2B C35B C34B 163.2(3) . . . . ? O1B C2B C35B C34B -77.4(4) . . . . ? C32B C2B C35B C34B 40.0(4) . . . . ? C33B C34B C35B C2B -32.3(5) . . . . ? _refine_diff_density_max 0.191 _refine_diff_density_min -0.170 _refine_diff_density_rms 0.041 #===END data_3-5b _audit_creation_method SHELXL _chemical_name_systematic ; bis(R,R)-(-)-trans-2,3-bis(diphenylhydroxymethyl)-1,4-dioxaspiro(4.4)nonane N-nitroso-4-phenylpiperidine clathrate ; _chemical_formula_moiety '(C33 H32 O4 . C11 H14 N2 O1)' _chemical_formula_sum 'C44 H46 N2 O5' _chemical_formula_weight 682.83 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.292(2) _cell_length_b 9.536(2) _cell_length_c 17.654(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.04(2) _cell_angle_gamma 90.00 _cell_volume 1886.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 8 _cell_measurement_theta_max 29 _exptl_crystal_description NEEDLE _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'NOT MEASURED' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.620 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'KM-4 four-circle diffractometer' _diffrn_measurement_method '\w/2\q scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 1.7 _diffrn_reflns_number 3511 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 66.09 _reflns_number_total 3418 _reflns_number_observed 2633 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Kuma KM-4 sofware (Kuma Diffraction, 1991)' _computing_cell_refinement 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_data_reduction 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ; Stereochemical Workstation (Siemens Analytical X-Ray Instruments, Inc., 1989) ; _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 296 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+0.1176P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, hydroxy H atom difmap' _refine_ls_hydrogen_treatment 'hydroxy H atoms refall; riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.21(32) _refine_ls_number_reflns 3122 _refine_ls_number_parameters 478 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_obs 0.0418 _refine_ls_wR_factor_all 0.1271 _refine_ls_wR_factor_obs 0.1108 _refine_ls_goodness_of_fit_all 1.072 _refine_ls_goodness_of_fit_obs 1.126 _refine_ls_restrained_S_all 1.146 _refine_ls_restrained_S_obs 1.177 _refine_ls_shift/esd_max -0.085 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O1 O 0.6173(2) 0.4327(3) 0.25370(13) 0.0591(7) Uani 1 d . . O2 O 0.9157(2) 0.5542(3) 0.2306(2) 0.0633(7) Uani 1 d . . H2O H 0.9193(35) 0.4900(52) 0.1908(24) 0.071(12) Uiso 1 d . . O3 O 0.6223(2) 0.2369(3) 0.18079(13) 0.0544(6) Uani 1 d . . O4 O 0.9029(2) 0.3587(3) 0.11900(13) 0.0490(5) Uani 1 d . . H4O H 0.9529(43) 0.2998(58) 0.1404(27) 0.086(16) Uiso 1 d . . C2 C 0.5434(3) 0.3268(4) 0.2162(2) 0.0559(9) Uani 1 d . . C4 C 0.7389(3) 0.2978(3) 0.1855(2) 0.0431(7) Uani 1 d . . H4 H 0.7918(3) 0.2492(3) 0.2234(2) 0.052 Uiso 1 d R . C5 C 0.7195(3) 0.4484(4) 0.2148(2) 0.0456(7) Uani 1 d . . H5 H 0.7004(3) 0.5092(4) 0.1717(2) 0.055 Uiso 1 d R . C6 C 0.8181(3) 0.5166(4) 0.2715(2) 0.0512(8) Uani 1 d . . C7 C 0.7889(3) 0.2871(3) 0.1079(2) 0.0403(7) Uani 1 d . . C8 C 0.8576(4) 0.4168(4) 0.3374(2) 0.0621(10) Uani 1 d . . C9 C 0.9652(4) 0.3491(5) 0.3427(3) 0.0867(14) Uani 1 d . . H9 H 1.0205(4) 0.3668(5) 0.3066(3) 0.104 Uiso 1 d R . C10 C 0.9975(7) 0.2510(7) 0.4038(4) 0.121(3) Uani 1 d . . H10 H 1.0722(7) 0.2016(7) 0.4096(4) 0.145 Uiso 1 d R . C11 C 0.9193(9) 0.2271(7) 0.4558(4) 0.129(3) Uani 1 d . . H11 H 0.9370(9) 0.1658(7) 0.4988(4) 0.155 Uiso 1 d R . C12 C 0.8129(7) 0.2940(7) 0.4503(3) 0.109(2) Uani 1 d . . H12 H 0.7552(7) 0.2787(7) 0.4851(3) 0.131 Uiso 1 d R . C13 C 0.7817(5) 0.3887(5) 0.3924(2) 0.0801(13) Uani 1 d . . H13 H 0.7063(5) 0.4362(5) 0.3892(2) 0.096 Uiso 1 d R . C14 C 0.7781(3) 0.6588(4) 0.3014(2) 0.0547(8) Uani 1 d . . C15 C 0.8440(4) 0.7180(5) 0.3645(2) 0.0708(11) Uani 1 d . . H15 H 0.9084(4) 0.6657(5) 0.3916(2) 0.085 Uiso 1 d R . C16 C 0.8201(5) 0.8521(6) 0.3884(3) 0.0861(14) Uani 1 d . . H16 H 0.8673(5) 0.8917(6) 0.4321(3) 0.103 Uiso 1 d R . C17 C 0.7292(5) 0.9287(5) 0.3500(3) 0.0830(13) Uani 1 d . . H17 H 0.7115(5) 1.0209(5) 0.3673(3) 0.100 Uiso 1 d R . C18 C 0.6617(4) 0.8710(5) 0.2886(2) 0.0729(11) Uani 1 d . . H18 H 0.6001(4) 0.9255(5) 0.2600(2) 0.088 Uiso 1 d R . C19 C 0.6853(4) 0.7369(4) 0.2639(2) 0.0649(10) Uani 1 d . . H19 H 0.6360(4) 0.6959(4) 0.2214(2) 0.078 Uiso 1 d R . C20 C 0.7097(3) 0.3604(4) 0.0442(2) 0.0463(7) Uani 1 d . . C21 C 0.6123(3) 0.2914(4) 0.0055(2) 0.0587(9) Uani 1 d . . H21 H 0.5966(3) 0.1961(4) 0.0186(2) 0.070 Uiso 1 d R . C22 C 0.5379(3) 0.3586(5) -0.0518(2) 0.0697(11) Uani 1 d . . H22 H 0.4709(3) 0.3084(5) -0.0773(2) 0.084 Uiso 1 d R . C23 C 0.5615(4) 0.4961(5) -0.0712(2) 0.0730(11) Uani 1 d . . H23 H 0.5145(4) 0.5421(5) -0.1129(2) 0.088 Uiso 1 d R . C24 C 0.6576(4) 0.5638(5) -0.0339(2) 0.0735(11) Uani 1 d . . H24 H 0.6711(4) 0.6610(5) -0.0440(2) 0.088 Uiso 1 d R . C25 C 0.7326(3) 0.4979(4) 0.0232(2) 0.0568(9) Uani 1 d . . H25 H 0.8013(3) 0.5470(4) 0.0473(2) 0.068 Uiso 1 d R . C26 C 0.8123(3) 0.1361(3) 0.0842(2) 0.0444(7) Uani 1 d . . C27 C 0.8656(3) 0.1179(4) 0.0175(2) 0.0598(9) Uani 1 d . . H27 H 0.8859(3) 0.1992(4) -0.0104(2) 0.072 Uiso 1 d R . C28 C 0.8939(4) -0.0129(5) -0.0076(2) 0.0721(11) Uani 1 d . . H28 H 0.9291(4) -0.0236(5) -0.0541(2) 0.086 Uiso 1 d R . C29 C 0.8689(4) -0.1305(5) 0.0337(3) 0.0727(11) Uani 1 d . . H29 H 0.8888(4) -0.2225(5) 0.0170(3) 0.087 Uiso 1 d R . C30 C 0.8160(4) -0.1147(4) 0.0994(3) 0.0670(10) Uani 1 d . . H30 H 0.7975(4) -0.1968(4) 0.1272(3) 0.080 Uiso 1 d R . C31 C 0.7877(3) 0.0181(4) 0.1248(2) 0.0540(8) Uani 1 d . . H31 H 0.7517(3) 0.0291(4) 0.1710(2) 0.065 Uiso 1 d R . C32 C 0.4796(4) 0.2501(6) 0.2752(3) 0.0809(12) Uani 1 d . . H32B H 0.4921(4) 0.2989(6) 0.3231(3) 0.097 Uiso 1 d R . H32A H 0.5112(4) 0.1569(6) 0.2825(3) 0.097 Uiso 1 d R . C33 C 0.3552(5) 0.2526(11) 0.2500(4) 0.137(3) Uani 1 d . . H33B H 0.3076(5) 0.2522(11) 0.2914(4) 0.164 Uiso 1 d R . H33A H 0.3364(5) 0.1710(11) 0.2190(4) 0.164 Uiso 1 d R . C34 C 0.3348(5) 0.3790(9) 0.1993(4) 0.125(2) Uani 1 d . . H34B H 0.2620(5) 0.3735(9) 0.1650(4) 0.151 Uiso 1 d R . H34A H 0.3311(5) 0.4592(9) 0.2318(4) 0.151 Uiso 1 d R . C35 C 0.4452(3) 0.3876(5) 0.1588(3) 0.0773(12) Uani 1 d . . H35B H 0.4354(3) 0.3306(5) 0.1136(3) 0.093 Uiso 1 d R . H35A H 0.4620(3) 0.4825(5) 0.1455(3) 0.093 Uiso 1 d R . O1G O 1.0550(4) 0.1794(5) 0.1945(3) 0.093(2) Uani 0.737(12) d PD . N2G N 1.1037(4) 0.0842(5) 0.1627(3) 0.078(2) Uani 0.737(12) d PD . O1'G O 1.0954(10) 0.1550(11) 0.1398(7) 0.083(5) Uiso 0.263(12) d PD . N2'G N 1.0628(7) 0.1007(8) 0.1976(6) 0.093(8) Uiso 0.263(12) d PD . N1G N 1.0980(3) -0.0348(4) 0.2022(2) 0.0814(11) Uani 1 d D . C2G C 1.0489(4) -0.0688(7) 0.2706(3) 0.095(2) Uani 1 d D . H2GB H 0.9881(4) -0.1387(7) 0.2591(3) 0.114 Uiso 1 d R . H2GA H 1.0142(4) 0.0115(7) 0.2921(3) 0.114 Uiso 1 d R . C3G C 1.1438(4) -0.1331(6) 0.3283(2) 0.0854(13) Uani 1 d . . H3GB H 1.2006(4) -0.0598(6) 0.3421(2) 0.103 Uiso 1 d R . H3GA H 1.1138(4) -0.1647(6) 0.3740(2) 0.103 Uiso 1 d R . C4G C 1.2053(4) -0.2520(5) 0.2954(2) 0.0673(10) Uani 1 d . . H4G H 1.1443(4) -0.3196(5) 0.2797(2) 0.081 Uiso 1 d R . C5G C 1.2539(5) -0.2078(7) 0.2232(3) 0.097(2) Uani 1 d . . H5GB H 1.2901(5) -0.2864(7) 0.2010(3) 0.116 Uiso 1 d R . H5GA H 1.3144(5) -0.1380(7) 0.2358(3) 0.116 Uiso 1 d R . C6G C 1.1579(5) -0.1438(7) 0.1658(3) 0.102(2) Uani 1 d D . H6GB H 1.1921(5) -0.1035(7) 0.1237(3) 0.122 Uiso 1 d R . H6GA H 1.1036(5) -0.2166(7) 0.1467(3) 0.122 Uiso 1 d R . C7G C 1.2954(4) -0.3235(4) 0.3542(2) 0.0659(10) Uani 1 d . . C8G C 1.2653(5) -0.4432(5) 0.3916(3) 0.0823(13) Uani 1 d . . H8G H 1.1901(5) -0.4869(5) 0.3746(3) 0.099 Uiso 1 d R . C9G C 1.3453(6) -0.5086(7) 0.4455(3) 0.101(2) Uani 1 d . . H9G H 1.3194(6) -0.5865(7) 0.4737(3) 0.122 Uiso 1 d R . C10G C 1.4585(6) -0.4533(8) 0.4629(3) 0.110(2) Uani 1 d . . H10G H 1.5163(6) -0.5004(8) 0.4985(3) 0.132 Uiso 1 d R . C11G C 1.4892(5) -0.3365(8) 0.4269(4) 0.114(2) Uani 1 d . . H11G H 1.5679(5) -0.2985(8) 0.4390(4) 0.137 Uiso 1 d R . C12G C 1.4097(4) -0.2716(6) 0.3729(3) 0.0910(14) Uani 1 d . . H12G H 1.4317(4) -0.1874(6) 0.3483(3) 0.109 Uiso 1 d 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 O1 0.0538(13) 0.068(2) 0.0571(13) -0.0201(12) 0.0131(11) -0.0128(12) O2 0.0606(14) 0.060(2) 0.071(2) -0.0144(14) 0.0184(12) -0.0209(13) O3 0.0517(12) 0.0508(14) 0.0629(13) -0.0137(12) 0.0163(10) -0.0146(11) O4 0.0474(12) 0.0463(13) 0.0534(12) 0.0039(11) 0.0065(10) -0.0052(11) C2 0.050(2) 0.058(2) 0.061(2) -0.011(2) 0.011(2) -0.009(2) C4 0.0420(15) 0.045(2) 0.0421(15) 0.0009(13) 0.0038(12) -0.0076(13) C5 0.048(2) 0.046(2) 0.0424(15) -0.0033(14) 0.0064(13) -0.0066(14) C6 0.054(2) 0.050(2) 0.049(2) -0.0062(15) 0.0041(14) -0.010(2) C7 0.044(2) 0.036(2) 0.0404(14) 0.0026(12) 0.0027(12) -0.0035(13) C8 0.075(2) 0.053(2) 0.053(2) -0.007(2) -0.012(2) -0.013(2) C9 0.095(3) 0.077(3) 0.077(3) -0.017(2) -0.032(2) 0.011(3) C10 0.153(6) 0.085(4) 0.105(4) -0.021(4) -0.064(4) 0.028(4) C11 0.215(8) 0.081(4) 0.074(4) 0.009(3) -0.050(5) -0.015(5) C12 0.170(6) 0.091(4) 0.058(3) 0.014(3) -0.025(3) -0.036(4) C13 0.107(3) 0.079(3) 0.050(2) 0.003(2) -0.006(2) -0.024(3) C14 0.067(2) 0.049(2) 0.049(2) -0.005(2) 0.013(2) -0.013(2) C15 0.079(3) 0.063(3) 0.068(2) -0.016(2) -0.001(2) -0.008(2) C16 0.105(4) 0.073(3) 0.079(3) -0.032(2) 0.003(3) -0.018(3) C17 0.108(4) 0.059(3) 0.086(3) -0.019(2) 0.027(3) -0.006(3) C18 0.093(3) 0.055(2) 0.073(3) -0.003(2) 0.017(2) 0.004(2) C19 0.080(2) 0.057(2) 0.058(2) -0.006(2) 0.007(2) -0.006(2) C20 0.056(2) 0.044(2) 0.0399(15) 0.0017(14) 0.0076(13) 0.006(2) C21 0.061(2) 0.056(2) 0.055(2) 0.004(2) -0.004(2) -0.001(2) C22 0.066(2) 0.080(3) 0.058(2) 0.003(2) -0.011(2) 0.010(2) C23 0.085(3) 0.074(3) 0.057(2) 0.014(2) -0.004(2) 0.024(2) C24 0.095(3) 0.050(2) 0.072(2) 0.016(2) -0.004(2) 0.014(2) C25 0.074(2) 0.043(2) 0.053(2) 0.005(2) 0.002(2) 0.002(2) C26 0.046(2) 0.041(2) 0.045(2) 0.0015(14) 0.0041(13) 0.0057(14) C27 0.073(2) 0.052(2) 0.057(2) 0.005(2) 0.020(2) 0.006(2) C28 0.076(3) 0.066(3) 0.077(2) -0.016(2) 0.024(2) 0.009(2) C29 0.068(2) 0.046(2) 0.104(3) -0.013(2) 0.013(2) 0.005(2) C30 0.070(2) 0.043(2) 0.088(3) 0.003(2) 0.013(2) -0.002(2) C31 0.061(2) 0.044(2) 0.058(2) 0.005(2) 0.011(2) 0.001(2) C32 0.076(3) 0.076(3) 0.099(3) -0.006(3) 0.042(2) -0.011(2) C33 0.079(3) 0.191(8) 0.144(5) 0.016(6) 0.034(3) -0.020(5) C34 0.071(3) 0.145(6) 0.160(6) -0.029(5) 0.013(3) 0.038(4) C35 0.070(2) 0.064(3) 0.093(3) -0.020(2) -0.010(2) 0.005(2) O1G 0.075(3) 0.087(4) 0.108(4) -0.004(3) -0.027(2) 0.026(3) N2G 0.070(3) 0.083(4) 0.078(4) 0.016(3) -0.005(3) -0.005(3) N1G 0.090(2) 0.070(3) 0.081(2) 0.016(2) -0.005(2) 0.001(2) C2G 0.092(3) 0.120(4) 0.072(3) 0.007(3) 0.009(2) 0.027(3) C3G 0.088(3) 0.104(4) 0.065(2) 0.002(3) 0.010(2) 0.020(3) C4G 0.072(2) 0.060(2) 0.069(2) 0.002(2) 0.006(2) -0.010(2) C5G 0.106(4) 0.109(4) 0.080(3) 0.025(3) 0.029(3) 0.028(3) C6G 0.118(4) 0.115(4) 0.074(3) 0.026(3) 0.021(3) 0.019(4) C7G 0.076(2) 0.058(2) 0.065(2) 0.003(2) 0.012(2) -0.001(2) C8G 0.098(3) 0.072(3) 0.078(3) 0.010(2) 0.017(2) -0.005(3) C9G 0.128(5) 0.092(4) 0.085(3) 0.029(3) 0.018(3) 0.013(4) C10G 0.113(4) 0.115(5) 0.098(4) 0.015(4) -0.004(3) 0.025(4) C11G 0.090(4) 0.120(5) 0.127(5) 0.017(4) -0.011(3) 0.007(4) C12G 0.082(3) 0.082(3) 0.106(3) 0.012(3) 0.002(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.421(4) . ? O1 C5 1.421(4) . ? O2 C6 1.436(4) . ? O2 H2O 0.94(5) . ? O3 C4 1.433(4) . ? O3 C2 1.434(4) . ? O4 C7 1.450(4) . ? O4 H4O 0.85(5) . ? C2 C35 1.523(5) . ? C2 C32 1.524(5) . ? C4 C7 1.546(4) . ? C4 C5 1.551(5) . ? C4 H4 0.96 . ? C5 C6 1.546(4) . ? C5 H5 0.96 . ? C6 C8 1.528(5) . ? C6 C14 1.542(5) . ? C7 C20 1.519(4) . ? C7 C26 1.531(5) . ? C8 C9 1.369(6) . ? C8 C13 1.397(6) . ? C9 C10 1.441(8) . ? C9 H9 0.96 . ? C10 C11 1.368(10) . ? C10 H10 0.96 . ? C11 C12 1.353(10) . ? C11 H11 0.96 . ? C12 C13 1.377(7) . ? C12 H12 0.96 . ? C13 H13 0.96 . ? C14 C15 1.382(5) . ? C14 C19 1.386(6) . ? C15 C16 1.384(7) . ? C15 H15 0.96 . ? C16 C17 1.369(7) . ? C16 H16 0.96 . ? C17 C18 1.363(6) . ? C17 H17 0.96 . ? C18 C19 1.388(6) . ? C18 H18 0.96 . ? C19 H19 0.96 . ? C20 C21 1.387(5) . ? C20 C25 1.395(5) . ? C21 C22 1.390(5) . ? C21 H21 0.96 . ? C22 C23 1.389(7) . ? C22 H22 0.96 . ? C23 C24 1.361(6) . ? C23 H23 0.96 . ? C24 C25 1.385(5) . ? C24 H24 0.96 . ? C25 H25 0.96 . ? C26 C31 1.380(5) . ? C26 C27 1.398(5) . ? C27 C28 1.375(6) . ? C27 H27 0.96 . ? C28 C29 1.385(7) . ? C28 H28 0.96 . ? C29 C30 1.377(6) . ? C29 H29 0.96 . ? C30 C31 1.394(6) . ? C30 H30 0.96 . ? C31 H31 0.96 . ? C32 C33 1.421(7) . ? C32 H32B 0.96 . ? C32 H32A 0.96 . ? C33 C34 1.502(11) . ? C33 H33B 0.96 . ? C33 H33A 0.96 . ? C34 C35 1.513(7) . ? C34 H34B 0.96 . ? C34 H34A 0.96 . ? C35 H35B 0.96 . ? C35 H35A 0.96 . ? O1G N2G 1.232(5) . ? N2G N1G 1.337(5) . ? O1'G N2'G 1.239(7) . ? N2'G N1G 1.352(7) . ? N1G C2G 1.426(6) . ? N1G C6G 1.434(7) . ? C2G C3G 1.516(6) . ? C2G H2GB 0.96 . ? C2G H2GA 0.96 . ? C3G C4G 1.484(7) . ? C3G H3GB 0.96 . ? C3G H3GA 0.96 . ? C4G C5G 1.509(6) . ? C4G C7G 1.522(6) . ? C4G H4G 0.96 . ? C5G C6G 1.517(7) . ? C5G H5GB 0.96 . ? C5G H5GA 0.96 . ? C6G H6GB 0.96 . ? C6G H6GA 0.96 . ? C7G C12G 1.384(6) . ? C7G C8G 1.383(6) . ? C8G C9G 1.377(7) . ? C8G H8G 0.96 . ? C9G C10G 1.382(8) . ? C9G H9G 0.96 . ? C10G C11G 1.348(9) . ? C10G H10G 0.96 . ? C11G C12G 1.374(7) . ? C11G H11G 0.96 . ? C12G H12G 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 C5 108.4(2) . . ? C6 O2 H2O 108.7(25) . . ? C4 O3 C2 110.4(2) . . ? C7 O4 H4O 106.2(34) . . ? O1 C2 O3 105.5(2) . . ? O1 C2 C35 112.2(3) . . ? O3 C2 C35 112.2(3) . . ? O1 C2 C32 108.8(3) . . ? O3 C2 C32 112.5(3) . . ? C35 C2 C32 105.8(3) . . ? O3 C4 C7 110.8(2) . . ? O3 C4 C5 103.2(2) . . ? C7 C4 C5 116.0(2) . . ? O3 C4 H4 109.4(2) . . ? C7 C4 H4 108.9(2) . . ? C5 C4 H4 108.4(2) . . ? O1 C5 C6 107.1(2) . . ? O1 C5 C4 102.7(3) . . ? C6 C5 C4 119.0(3) . . ? O1 C5 H5 109.3(2) . . ? C6 C5 H5 109.4(2) . . ? C4 C5 H5 108.8(2) . . ? O2 C6 C8 111.6(3) . . ? O2 C6 C14 103.2(3) . . ? C8 C6 C14 110.9(3) . . ? O2 C6 C5 108.4(2) . . ? C8 C6 C5 110.6(3) . . ? C14 C6 C5 111.9(3) . . ? O4 C7 C20 108.4(2) . . ? O4 C7 C26 107.4(2) . . ? C20 C7 C26 109.6(2) . . ? O4 C7 C4 105.3(2) . . ? C20 C7 C4 112.3(2) . . ? C26 C7 C4 113.5(2) . . ? C9 C8 C13 118.5(4) . . ? C9 C8 C6 121.3(4) . . ? C13 C8 C6 120.1(4) . . ? C8 C9 C10 119.9(6) . . ? C8 C9 H9 121.0(3) . . ? C10 C9 H9 119.1(4) . . ? C11 C10 C9 119.0(6) . . ? C11 C10 H10 118.6(4) . . ? C9 C10 H10 122.4(4) . . ? C12 C11 C10 121.0(6) . . ? C12 C11 H11 116.2(4) . . ? C10 C11 H11 122.8(4) . . ? C11 C12 C13 120.4(7) . . ? C11 C12 H12 123.3(4) . . ? C13 C12 H12 116.3(4) . . ? C12 C13 C8 121.2(6) . . ? C12 C13 H13 119.8(4) . . ? C8 C13 H13 119.0(3) . . ? C15 C14 C19 117.8(4) . . ? C15 C14 C6 118.9(4) . . ? C19 C14 C6 123.0(3) . . ? C14 C15 C16 121.1(4) . . ? C14 C15 H15 119.3(3) . . ? C16 C15 H15 119.5(3) . . ? C17 C16 C15 120.3(4) . . ? C17 C16 H16 119.7(3) . . ? C15 C16 H16 119.9(3) . . ? C18 C17 C16 119.4(4) . . ? C18 C17 H17 120.3(3) . . ? C16 C17 H17 120.3(3) . . ? C17 C18 C19 120.8(5) . . ? C17 C18 H18 119.9(3) . . ? C19 C18 H18 119.2(3) . . ? C18 C19 C14 120.5(4) . . ? C18 C19 H19 120.4(3) . . ? C14 C19 H19 119.1(2) . . ? C21 C20 C25 118.5(3) . . ? C21 C20 C7 120.3(3) . . ? C25 C20 C7 121.2(3) . . ? C20 C21 C22 120.8(4) . . ? C20 C21 H21 119.3(2) . . ? C22 C21 H21 119.9(3) . . ? C23 C22 C21 119.8(4) . . ? C23 C22 H22 121.3(2) . . ? C21 C22 H22 118.8(3) . . ? C24 C23 C22 119.6(4) . . ? C24 C23 H23 119.2(2) . . ? C22 C23 H23 121.0(2) . . ? C23 C24 C25 121.1(4) . . ? C23 C24 H24 120.2(2) . . ? C25 C24 H24 118.5(2) . . ? C24 C25 C20 120.2(4) . . ? C24 C25 H25 119.3(3) . . ? C20 C25 H25 120.4(2) . . ? C31 C26 C27 118.1(3) . . ? C31 C26 C7 124.9(3) . . ? C27 C26 C7 117.0(3) . . ? C28 C27 C26 121.6(4) . . ? C28 C27 H27 119.3(2) . . ? C26 C27 H27 119.0(2) . . ? C27 C28 C29 119.7(3) . . ? C27 C28 H28 120.5(2) . . ? C29 C28 H28 119.7(2) . . ? C30 C29 C28 119.5(4) . . ? C30 C29 H29 120.0(3) . . ? C28 C29 H29 120.5(2) . . ? C29 C30 C31 120.7(4) . . ? C29 C30 H30 118.9(3) . . ? C31 C30 H30 120.3(2) . . ? C26 C31 C30 120.3(3) . . ? C26 C31 H31 119.0(2) . . ? C30 C31 H31 120.6(2) . . ? C33 C32 C2 108.0(5) . . ? C33 C32 H32B 107.5(4) . . ? C2 C32 H32B 109.8(2) . . ? C33 C32 H32A 113.2(5) . . ? C2 C32 H32A 109.7(2) . . ? H32B C32 H32A 108.6 . . ? C32 C33 C34 105.9(5) . . ? C32 C33 H33B 112.7(3) . . ? C34 C33 H33B 113.4(4) . . ? C32 C33 H33A 107.8(4) . . ? C34 C33 H33A 107.7(4) . . ? H33B C33 H33A 109.1 . . ? C33 C34 C35 104.5(4) . . ? C33 C34 H34B 112.9(4) . . ? C35 C34 H34B 113.4(3) . . ? C33 C34 H34A 107.3(4) . . ? C35 C34 H34A 109.7(4) . . ? H34B C34 H34A 108.8 . . ? C34 C35 C2 103.8(4) . . ? C34 C35 H35B 110.1(3) . . ? C2 C35 H35B 109.8(2) . . ? C34 C35 H35A 111.4(4) . . ? C2 C35 H35A 111.8(2) . . ? H35B C35 H35A 109.7 . . ? O1G N2G N1G 109.6(5) . . ? O1'G N2'G N1G 109.5(9) . . ? N2G N1G C2G 133.1(5) . . ? N2'G N1G C2G 97.3(7) . . ? N2G N1G C6G 109.0(4) . . ? N2'G N1G C6G 144.8(6) . . ? C2G N1G C6G 117.9(4) . . ? N1G C2G C3G 110.2(4) . . ? N1G C2G H2GB 108.8(2) . . ? C3G C2G H2GB 106.8(3) . . ? N1G C2G H2GA 111.9(3) . . ? C3G C2G H2GA 110.2(3) . . ? H2GB C2G H2GA 108.7 . . ? C4G C3G C2G 111.9(4) . . ? C4G C3G H3GB 109.0(3) . . ? C2G C3G H3GB 105.7(3) . . ? C4G C3G H3GA 108.6(2) . . ? C2G C3G H3GA 113.5(3) . . ? H3GB C3G H3GA 108.0 . . ? C3G C4G C5G 110.7(4) . . ? C3G C4G C7G 112.4(3) . . ? C5G C4G C7G 114.8(4) . . ? C3G C4G H4G 105.8(3) . . ? C5G C4G H4G 105.4(3) . . ? C7G C4G H4G 107.0(2) . . ? C6G C5G C4G 111.9(4) . . ? C6G C5G H5GB 110.3(3) . . ? C4G C5G H5GB 110.1(3) . . ? C6G C5G H5GA 107.8(3) . . ? C4G C5G H5GA 108.6(3) . . ? H5GB C5G H5GA 108.0 . . ? N1G C6G C5G 109.3(4) . . ? N1G C6G H6GB 108.3(3) . . ? C5G C6G H6GB 110.9(3) . . ? N1G C6G H6GA 111.5(2) . . ? C5G C6G H6GA 108.5(4) . . ? H6GB C6G H6GA 108.4 . . ? C12G C7G C8G 117.3(4) . . ? C12G C7G C4G 121.9(4) . . ? C8G C7G C4G 120.9(4) . . ? C9G C8G C7G 121.6(5) . . ? C9G C8G H8G 120.0(3) . . ? C7G C8G H8G 117.9(3) . . ? C8G C9G C10G 119.5(5) . . ? C8G C9G H9G 119.6(3) . . ? C10G C9G H9G 120.7(3) . . ? C11G C10G C9G 119.6(6) . . ? C11G C10G H10G 120.1(4) . . ? C9G C10G H10G 120.2(4) . . ? C10G C11G C12G 121.0(6) . . ? C10G C11G H11G 119.4(4) . . ? C12G C11G H11G 119.5(4) . . ? C11G C12G C7G 121.0(5) . . ? C11G C12G H12G 120.5(4) . . ? C7G C12G H12G 118.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 O1 C2 O3 26.8(4) . . . . ? C5 O1 C2 C35 -95.6(3) . . . . ? C5 O1 C2 C32 147.7(3) . . . . ? C4 O3 C2 O1 -9.3(4) . . . . ? C4 O3 C2 C35 113.2(3) . . . . ? C4 O3 C2 C32 -127.7(3) . . . . ? C2 O3 C4 C7 -134.6(3) . . . . ? C2 O3 C4 C5 -9.8(3) . . . . ? C2 O1 C5 C6 -158.3(3) . . . . ? C2 O1 C5 C4 -32.2(3) . . . . ? O3 C4 C5 O1 25.1(3) . . . . ? C7 C4 C5 O1 146.4(2) . . . . ? O3 C4 C5 C6 143.2(3) . . . . ? C7 C4 C5 C6 -95.6(3) . . . . ? O1 C5 C6 O2 -171.0(3) . . . . ? C4 C5 C6 O2 73.2(4) . . . . ? O1 C5 C6 C8 66.4(4) . . . . ? C4 C5 C6 C8 -49.4(4) . . . . ? O1 C5 C6 C14 -57.9(3) . . . . ? C4 C5 C6 C14 -173.6(3) . . . . ? O3 C4 C7 O4 176.9(3) . . . . ? C5 C4 C7 O4 59.7(3) . . . . ? O3 C4 C7 C20 59.1(3) . . . . ? C5 C4 C7 C20 -58.0(3) . . . . ? O3 C4 C7 C26 -65.9(3) . . . . ? C5 C4 C7 C26 176.9(3) . . . . ? O2 C6 C8 C9 -14.4(5) . . . . ? C14 C6 C8 C9 -128.8(4) . . . . ? C5 C6 C8 C9 106.4(4) . . . . ? O2 C6 C8 C13 168.1(3) . . . . ? C14 C6 C8 C13 53.7(4) . . . . ? C5 C6 C8 C13 -71.1(4) . . . . ? C13 C8 C9 C10 0.2(6) . . . . ? C6 C8 C9 C10 -177.3(4) . . . . ? C8 C9 C10 C11 0.2(8) . . . . ? C9 C10 C11 C12 0.0(9) . . . . ? C10 C11 C12 C13 -0.5(9) . . . . ? C11 C12 C13 C8 0.9(8) . . . . ? C9 C8 C13 C12 -0.7(6) . . . . ? C6 C8 C13 C12 176.8(4) . . . . ? O2 C6 C14 C15 -78.0(4) . . . . ? C8 C6 C14 C15 41.6(4) . . . . ? C5 C6 C14 C15 165.7(3) . . . . ? O2 C6 C14 C19 95.9(4) . . . . ? C8 C6 C14 C19 -144.5(3) . . . . ? C5 C6 C14 C19 -20.5(4) . . . . ? C19 C14 C15 C16 -1.5(6) . . . . ? C6 C14 C15 C16 172.7(4) . . . . ? C14 C15 C16 C17 0.5(7) . . . . ? C15 C16 C17 C18 0.8(7) . . . . ? C16 C17 C18 C19 -1.1(7) . . . . ? C17 C18 C19 C14 0.1(6) . . . . ? C15 C14 C19 C18 1.2(6) . . . . ? C6 C14 C19 C18 -172.8(3) . . . . ? O4 C7 C20 C21 159.7(3) . . . . ? C26 C7 C20 C21 42.7(4) . . . . ? C4 C7 C20 C21 -84.4(4) . . . . ? O4 C7 C20 C25 -20.4(4) . . . . ? C26 C7 C20 C25 -137.4(3) . . . . ? C4 C7 C20 C25 95.5(3) . . . . ? C25 C20 C21 C22 -1.3(5) . . . . ? C7 C20 C21 C22 178.7(3) . . . . ? C20 C21 C22 C23 0.5(6) . . . . ? C21 C22 C23 C24 0.1(6) . . . . ? C22 C23 C24 C25 0.0(7) . . . . ? C23 C24 C25 C20 -0.8(6) . . . . ? C21 C20 C25 C24 1.4(5) . . . . ? C7 C20 C25 C24 -178.5(3) . . . . ? O4 C7 C26 C31 118.6(3) . . . . ? C20 C7 C26 C31 -123.8(3) . . . . ? C4 C7 C26 C31 2.6(4) . . . . ? O4 C7 C26 C27 -59.5(4) . . . . ? C20 C7 C26 C27 58.1(4) . . . . ? C4 C7 C26 C27 -175.5(3) . . . . ? C31 C26 C27 C28 -0.3(6) . . . . ? C7 C26 C27 C28 177.9(4) . . . . ? C26 C27 C28 C29 0.3(6) . . . . ? C27 C28 C29 C30 0.0(6) . . . . ? C28 C29 C30 C31 -0.2(6) . . . . ? C27 C26 C31 C30 0.1(5) . . . . ? C7 C26 C31 C30 -178.0(4) . . . . ? C29 C30 C31 C26 0.1(6) . . . . ? O1 C2 C32 C33 126.6(5) . . . . ? O3 C2 C32 C33 -116.9(5) . . . . ? C35 C2 C32 C33 5.8(6) . . . . ? C2 C32 C33 C34 -25.4(7) . . . . ? C32 C33 C34 C35 35.4(7) . . . . ? C33 C34 C35 C2 -30.7(6) . . . . ? O1 C2 C35 C34 -102.8(5) . . . . ? O3 C2 C35 C34 138.7(4) . . . . ? C32 C2 C35 C34 15.7(5) . . . . ? O1G N2G N1G C2G -0.2(3) . . . . ? O1'G N2G N1G C6G 131.1(66) . . . . ? O1G N2G N1G C6G -178.4(2) . . . . ? O1G N2'G N1G C2G 126.7(74) . . . . ? O1'G N2'G N1G C2G -179.3(3) . . . . ? O1'G N2'G N1G C6G -1.2(5) . . . . ? N2G N1G C2G C3G -124.0(5) . . . . ? N2'G N1G C2G C3G -127.2(5) . . . . ? C6G N1G C2G C3G 54.1(5) . . . . ? N1G C2G C3G C4G -52.1(6) . . . . ? C2G C3G C4G C5G 53.8(6) . . . . ? C2G C3G C4G C7G -176.4(4) . . . . ? C3G C4G C5G C6G -54.2(6) . . . . ? C7G C4G C5G C6G 177.2(5) . . . . ? N2G N1G C6G C5G 124.5(4) . . . . ? N2'G N1G C6G C5G 128.1(6) . . . . ? C2G N1G C6G C5G -54.0(5) . . . . ? C4G C5G C6G N1G 52.0(6) . . . . ? C3G C4G C7G C12G -82.6(5) . . . . ? C5G C4G C7G C12G 45.1(6) . . . . ? C3G C4G C7G C8G 96.8(5) . . . . ? C5G C4G C7G C8G -135.5(5) . . . . ? C12G C7G C8G C9G 0.1(7) . . . . ? C4G C7G C8G C9G -179.4(4) . . . . ? C7G C8G C9G C10G 0.2(8) . . . . ? C8G C9G C10G C11G -0.2(9) . . . . ? C9G C10G C11G C12G -0.1(10) . . . . ? C10G C11G C12G C7G 0.4(10) . . . . ? C8G C7G C12G C11G -0.4(8) . . . . ? C4G C7G C12G C11G 179.0(5) . . . . ? _refine_diff_density_max 0.157 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.035 #===END