# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2003data_global _journal_coden_Cambridge 177 loop_ _publ_author_name 'Rex Palmer' 'Babur Z. Chowdhry' 'Terence C. Jenkins' 'Brian S. Potter' 'Robert Withnall' _publ_contact_author_name 'Dr Rex Palmer' _publ_contact_author_address ; School of Crystallography Birkbeck College, University of London Malet Street London WC1E 7HX UNITED KINGDOM ; _publ_contact_author_email R.PALMER@BBK.AC.UK _publ_requested_journal 'Organic & Biomolecular Chemistry' _publ_section_title ; Two new cyclosporin folds observed in the structures of the immunosuppressant cyclosporin G and the formyl peptide receptor antagonist cyclosporin H at ultra high resolution ; data_CsG_I _database_code_CSD 195320 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cyclosporin G crystal form I ex MeOH LT ; _chemical_name_common 'cyclosporin G' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C63 H113 O12 N11. 2.4H2O 0.5CH3OH' _chemical_compound_source Sandoz-Novartis _chemical_formula_sum 'C63.50 H119.80 N11 O14.90' _chemical_formula_weight 1275.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.3997(2) _cell_length_b 20.1710(4) _cell_length_c 30.6428(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7664.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 138783 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 27 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2788 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type SORTAV _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details ; SORTAV absorption correction software package: R.H. Blessing (1997) ; _exptl_special_details ; Oxford Cryosystems Cryostream cooler: J. Cosier and A.M. Glazer (1986) ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Denzo,Z. Otwinowski and W. Minor (1997)' _diffrn_detector_area_resol_mean '0.5 deg' _diffrn_standards_number NA _diffrn_standards_interval_count NA _diffrn_standards_interval_time NA _diffrn_standards_decay_% NA _diffrn_reflns_number 138783 _diffrn_reflns_av_R_equivalents 0.1752 _diffrn_reflns_av_sigmaI/netI 0.0918 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.03 _reflns_number_total 8187 _reflns_number_gt 4564 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Collect Data collection and processing user interface: Collect: Data collection software, R. Hooft, Nonius B.V.(1998) ; _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution 'SHELX-S (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1998)' _computing_publication_material SHELX97 _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^)+(0.1022P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(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 0.4(16) _refine_ls_number_reflns 8187 _refine_ls_number_parameters 901 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1427 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1813 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.004 _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 1.5716(3) -0.09218(19) 1.00228(11) 0.0505(10) Uani 1 1 d . . . O2 O 1.1967(3) -0.14319(19) 0.97084(12) 0.0558(10) Uani 1 1 d . . . O3 O 1.3284(3) -0.2497(2) 0.91206(11) 0.0504(10) Uani 1 1 d . . . O4 O 1.2093(3) -0.29838(19) 0.76924(11) 0.0472(10) Uani 1 1 d . . . O5 O 1.0451(4) -0.1095(2) 0.82296(12) 0.0660(12) Uani 1 1 d . . . O6 O 0.9946(3) 0.0377(2) 0.71212(13) 0.0574(11) Uani 1 1 d . . . O7 O 0.8295(3) 0.05893(18) 0.85598(11) 0.0491(10) Uani 1 1 d . . . O8 O 0.9602(3) 0.23651(18) 0.83863(11) 0.0415(9) Uani 1 1 d . . . O9 O 1.1118(3) 0.19447(19) 0.98809(12) 0.0522(10) Uani 1 1 d . . . O10 O 1.2812(3) -0.00285(19) 0.91543(13) 0.0486(10) Uani 1 1 d . . . O11 O 1.5897(3) 0.1389(2) 0.92609(12) 0.0530(10) Uani 1 1 d . . . O12 O 1.6542(4) -0.0287(3) 0.87255(13) 0.0699(13) Uani 1 1 d . . . H12 H 1.7203 -0.0199 0.8711 0.07(2) Uiso 1 1 calc R . . N1 N 1.5682(3) 0.0328(2) 0.94550(13) 0.0438(11) Uani 1 1 d . . . N2 N 1.4016(4) -0.0914(2) 0.97707(14) 0.0441(11) Uani 1 1 d . . . H2 H 1.3566 -0.0756 0.9574 0.034(14) Uiso 1 1 calc R . . N3 N 1.2649(4) -0.2403(2) 0.99362(12) 0.0397(11) Uani 1 1 d . . . N4 N 1.1872(3) -0.3093(2) 0.88696(12) 0.0362(10) Uani 1 1 d . . . N5 N 1.1021(3) -0.2427(2) 0.81656(13) 0.0393(10) Uani 1 1 d . . . H5 H 1.0880 -0.2338 0.8441 0.031(13) Uiso 1 1 calc R . . N6 N 1.0847(4) -0.1001(2) 0.75140(13) 0.0427(11) Uani 1 1 d . . . N7 N 0.9406(4) 0.0147(2) 0.78062(15) 0.0474(12) Uani 1 1 d . . . H7 H 0.9583 -0.0046 0.8054 0.055(18) Uiso 1 1 calc R . . N8 N 0.7971(3) 0.1505(2) 0.81525(14) 0.0397(11) Uani 1 1 d . . . H8 H 0.7891 0.1668 0.7888 0.15(4) Uiso 1 1 calc R . . N9 N 0.9215(3) 0.21523(19) 0.90973(13) 0.0352(10) Uani 1 1 d . . . N10 N 1.1097(3) 0.1259(2) 0.92992(13) 0.0379(10) Uani 1 1 d . . . N11 N 1.3451(3) 0.1016(2) 0.92289(13) 0.0381(10) Uani 1 1 d . . . C1A C 1.6655(5) 0.0421(3) 0.9728(2) 0.0611(18) Uani 1 1 d . . . H1A1 H 1.6718 0.0051 0.9934 0.068(10) Uiso 1 1 calc R . . H1A2 H 1.6594 0.0838 0.9891 0.068(10) Uiso 1 1 calc R . . H1A3 H 1.7296 0.0435 0.9542 0.068(10) Uiso 1 1 calc R . . C2A C 1.5389(5) -0.0357(3) 0.93415(16) 0.0458(14) Uani 1 1 d . . . H2A H 1.4760 -0.0341 0.9137 0.055 Uiso 1 1 calc R . . C3A C 1.5052(5) -0.0749(3) 0.97449(17) 0.0402(13) Uani 1 1 d . . . C4A C 1.6343(5) -0.0675(3) 0.9098(2) 0.0610(17) Uani 1 1 d . . . H4A H 1.6993 -0.0657 0.9291 0.046(14) Uiso 1 1 calc R . . C5A C 1.6168(6) -0.1380(3) 0.8959(2) 0.0658(18) Uani 1 1 d . . . H5A H 1.5977 -0.1649 0.9222 0.10(2) Uiso 1 1 calc R . . C6A C 1.5228(6) -0.1430(4) 0.8622(2) 0.075(2) Uani 1 1 d . . . H6A1 H 1.4536 -0.1349 0.8774 0.19(4) Uiso 1 1 calc R . . H6A2 H 1.5319 -0.1080 0.8399 0.19(4) Uiso 1 1 calc R . . C7A C 1.5180(6) -0.2085(4) 0.8402(3) 0.094(3) Uani 1 1 d . . . H7A H 1.5110 -0.2470 0.8578 0.113 Uiso 1 1 calc R . . C8A C 1.5230(7) -0.2163(6) 0.7967(3) 0.105(3) Uani 1 1 d . . . H8A H 1.5327 -0.1791 0.7781 0.18(6) Uiso 1 1 calc R . . C9A C 1.5128(10) -0.2870(6) 0.7775(4) 0.145(4) Uani 1 1 d . . . H9A1 H 1.4464 -0.2903 0.7604 0.25(4) Uiso 1 1 calc R . . H9A2 H 1.5107 -0.3194 0.8014 0.25(4) Uiso 1 1 calc R . . H9A3 H 1.5750 -0.2963 0.7587 0.25(4) Uiso 1 1 calc R . . C10A C 1.7243(6) -0.1638(4) 0.8773(2) 0.080(2) Uani 1 1 d . . . H10A H 1.7176 -0.2112 0.8706 0.19(3) Uiso 1 1 calc R . . H10B H 1.7818 -0.1573 0.8988 0.19(3) Uiso 1 1 calc R . . H10C H 1.7419 -0.1395 0.8505 0.19(3) Uiso 1 1 calc R . . C1B C 1.3593(5) -0.1349(3) 1.01141(16) 0.0431(14) Uani 1 1 d . . . H1B H 1.4172 -0.1662 1.0209 0.034(13) Uiso 1 1 calc R . . C2B C 1.2673(5) -0.1742(3) 0.99048(16) 0.0412(13) Uani 1 1 d . . . C3B C 1.3204(5) -0.0960(3) 1.05027(17) 0.0535(16) Uani 1 1 d . . . H3B1 H 1.2651 -0.0640 1.0403 0.043(10) Uiso 1 1 calc R . . H3B2 H 1.3817 -0.0702 1.0621 0.043(10) Uiso 1 1 calc R . . C4B C 1.2727(6) -0.1378(4) 1.0869(2) 0.0670(18) Uani 1 1 d . . . H4B1 H 1.2056 -0.1591 1.0763 0.100(18) Uiso 1 1 calc R . . H4B2 H 1.3242 -0.1735 1.0945 0.100(18) Uiso 1 1 calc R . . C5B C 1.2477(7) -0.0982(5) 1.1272(2) 0.092(2) Uani 1 1 d . . . H5B1 H 1.2109 -0.1265 1.1485 0.128(19) Uiso 1 1 calc R . . H5B2 H 1.2009 -0.0608 1.1195 0.128(19) Uiso 1 1 calc R . . H5B3 H 1.3150 -0.0814 1.1398 0.128(19) Uiso 1 1 calc R . . C1C C 1.3535(5) -0.2801(3) 1.01069(19) 0.0578(16) Uani 1 1 d . . . H1C1 H 1.3288 -0.3258 1.0153 0.081(12) Uiso 1 1 calc R . . H1C2 H 1.3779 -0.2615 1.0385 0.081(12) Uiso 1 1 calc R . . H1C3 H 1.4133 -0.2800 0.9898 0.081(12) Uiso 1 1 calc R . . C2C C 1.1919(5) -0.2746(3) 0.96406(15) 0.0408(13) Uani 1 1 d . . . H2C1 H 1.1217 -0.2514 0.9631 0.033(9) Uiso 1 1 calc R . . H2C2 H 1.1794 -0.3204 0.9746 0.033(9) Uiso 1 1 calc R . . C3C C 1.2415(4) -0.2763(3) 0.91858(17) 0.0396(13) Uani 1 1 d . . . C1D C 1.0846(4) -0.3428(3) 0.89579(17) 0.0454(14) Uani 1 1 d . . . H1D1 H 1.0566 -0.3621 0.8687 0.068(10) Uiso 1 1 calc R . . H1D2 H 1.0325 -0.3106 0.9072 0.068(10) Uiso 1 1 calc R . . H1D3 H 1.0959 -0.3780 0.9173 0.068(10) Uiso 1 1 calc R . . C2D C 1.2380(4) -0.3189(3) 0.84500(15) 0.0372(12) Uani 1 1 d . . . H2D H 1.3108 -0.2976 0.8471 0.038(13) Uiso 1 1 calc R . . C3D C 1.1811(4) -0.2853(3) 0.80697(17) 0.0385(13) Uani 1 1 d . . . C4D C 1.2586(4) -0.3931(3) 0.83418(17) 0.0449(14) Uani 1 1 d . . . H4D1 H 1.1883 -0.4147 0.8286 0.046(10) Uiso 1 1 calc R . . H4D2 H 1.3010 -0.3956 0.8069 0.046(10) Uiso 1 1 calc R . . C5D C 1.3177(5) -0.4321(3) 0.86946(19) 0.0551(16) Uani 1 1 d . . . H5D H 1.2765 -0.4276 0.8973 0.061(17) Uiso 1 1 calc R . . C6D C 1.4311(6) -0.4057(4) 0.8769(3) 0.082(2) Uani 1 1 d . . . H6D1 H 1.4673 -0.4325 0.8991 0.091(13) Uiso 1 1 calc R . . H6D2 H 1.4272 -0.3595 0.8867 0.091(13) Uiso 1 1 calc R . . H6D3 H 1.4719 -0.4079 0.8495 0.091(13) Uiso 1 1 calc R . . C7D C 1.3208(7) -0.5048(3) 0.8573(2) 0.075(2) Uani 1 1 d . . . H7D1 H 1.3503 -0.5304 0.8817 0.094(13) Uiso 1 1 calc R . . H7D2 H 1.3665 -0.5108 0.8315 0.094(13) Uiso 1 1 calc R . . H7D3 H 1.2475 -0.5201 0.8509 0.094(13) Uiso 1 1 calc R . . C1E C 1.0382(4) -0.2103(3) 0.78235(17) 0.0441(14) Uani 1 1 d . . . H1E H 1.0647 -0.2251 0.7531 0.033(12) Uiso 1 1 calc R . . C2E C 1.0555(5) -0.1359(3) 0.78685(18) 0.0438(13) Uani 1 1 d . . . C3E C 0.9182(5) -0.2276(3) 0.7867(2) 0.0606(17) Uani 1 1 d . . . H3E H 0.8963 -0.2193 0.8177 0.036(13) Uiso 1 1 calc R . . C4E C 0.9037(6) -0.3027(4) 0.7773(3) 0.092(3) Uani 1 1 d . . . H4E1 H 0.9454 -0.3285 0.7985 0.14(2) Uiso 1 1 calc R . . H4E2 H 0.9292 -0.3126 0.7478 0.14(2) Uiso 1 1 calc R . . H4E3 H 0.8272 -0.3144 0.7797 0.14(2) Uiso 1 1 calc R . . C5E C 0.8446(6) -0.1896(4) 0.7580(3) 0.085(2) Uani 1 1 d . . . H5E1 H 0.7697 -0.2006 0.7652 0.116(16) Uiso 1 1 calc R . . H5E2 H 0.8590 -0.2009 0.7275 0.116(16) Uiso 1 1 calc R . . H5E3 H 0.8564 -0.1420 0.7624 0.116(16) Uiso 1 1 calc R . . C1F C 1.0689(5) -0.1220(3) 0.70603(17) 0.0528(16) Uani 1 1 d . . . H1F1 H 1.0077 -0.0982 0.6932 0.089(12) Uiso 1 1 calc R . . H1F2 H 1.0544 -0.1698 0.7056 0.089(12) Uiso 1 1 calc R . . H1F3 H 1.1342 -0.1127 0.6891 0.089(12) Uiso 1 1 calc R . . C2F C 1.1104(4) -0.0295(3) 0.7573(2) 0.0496(15) Uani 1 1 d . . . H2F H 1.1276 -0.0228 0.7889 0.070(19) Uiso 1 1 calc R . . C3F C 1.0104(5) 0.0117(3) 0.7472(2) 0.0442(14) Uani 1 1 d . . . C4F C 1.2077(5) -0.0086(3) 0.7317(3) 0.072(2) Uani 1 1 d . . . H4F1 H 1.2235 0.0384 0.7386 0.051(11) Uiso 1 1 calc R . . H4F2 H 1.1901 -0.0112 0.7003 0.051(11) Uiso 1 1 calc R . . C5F C 1.3107(6) -0.0498(4) 0.7401(3) 0.098(3) Uani 1 1 d . . . H5F H 1.2968 -0.0956 0.7290 0.057(17) Uiso 1 1 calc R . . C6F C 1.3998(7) -0.0239(7) 0.7162(5) 0.174(6) Uani 1 1 d . . . H6F1 H 1.4668 -0.0435 0.7272 0.17(3) Uiso 1 1 calc R . . H6F2 H 1.4025 0.0244 0.7197 0.17(3) Uiso 1 1 calc R . . H6F3 H 1.3914 -0.0348 0.6852 0.17(3) Uiso 1 1 calc R . . C7F C 1.3344(8) -0.0554(6) 0.7911(3) 0.123(3) Uani 1 1 d . . . H7F1 H 1.2815 -0.0852 0.8045 0.23(4) Uiso 1 1 calc R . . H7F2 H 1.3291 -0.0114 0.8045 0.23(4) Uiso 1 1 calc R . . H7F3 H 1.4071 -0.0732 0.7956 0.23(4) Uiso 1 1 calc R . . C1G C 0.8382(4) 0.0480(3) 0.77786(16) 0.0409(13) Uani 1 1 d . . . H1G H 0.8411 0.0804 0.7531 0.025(11) Uiso 1 1 calc R . . C2G C 0.8215(4) 0.0861(3) 0.81982(17) 0.0394(13) Uani 1 1 d . . . C3G C 0.7446(5) -0.0005(3) 0.76959(19) 0.0574(16) Uani 1 1 d . . . H3G1 H 0.6769 0.0242 0.7674 0.072(11) Uiso 1 1 calc R . . H3G2 H 0.7400 -0.0321 0.7938 0.072(11) Uiso 1 1 calc R . . H3G3 H 0.7574 -0.0246 0.7423 0.072(11) Uiso 1 1 calc R . . C1H C 0.7836(4) 0.1942(3) 0.85248(17) 0.0393(13) Uani 1 1 d . . . H1H H 0.7477 0.1699 0.8770 0.043(14) Uiso 1 1 calc R . . C2H C 0.8960(4) 0.2173(2) 0.86643(17) 0.0378(12) Uani 1 1 d . . . C3H C 0.7168(4) 0.2538(3) 0.83926(19) 0.0530(15) Uani 1 1 d . . . H3H1 H 0.6444 0.2392 0.8308 0.076(11) Uiso 1 1 calc R . . H3H2 H 0.7513 0.2762 0.8145 0.076(11) Uiso 1 1 calc R . . H3H3 H 0.7115 0.2846 0.8639 0.076(11) Uiso 1 1 calc R . . C1I C 0.8466(4) 0.1940(3) 0.94368(17) 0.0491(15) Uani 1 1 d . . . H1I1 H 0.8812 0.1984 0.9723 0.072(11) Uiso 1 1 calc R . . H1I2 H 0.8265 0.1476 0.9388 0.072(11) Uiso 1 1 calc R . . H1I3 H 0.7819 0.2218 0.9427 0.072(11) Uiso 1 1 calc R . . C2I C 1.0282(4) 0.2374(2) 0.92353(17) 0.0371(12) Uani 1 1 d . . . H2I H 1.0716 0.2462 0.8966 0.042(13) Uiso 1 1 calc R . . C3I C 1.0861(4) 0.1835(3) 0.94957(18) 0.0424(13) Uani 1 1 d . . . C4I C 1.0195(5) 0.3030(3) 0.94908(18) 0.0500(15) Uani 1 1 d . . . H4I1 H 0.9679 0.2971 0.9734 0.055(11) Uiso 1 1 calc R . . H4I2 H 1.0907 0.3138 0.9618 0.055(11) Uiso 1 1 calc R . . C5I C 0.9825(5) 0.3608(3) 0.9209(2) 0.0585(17) Uani 1 1 d . . . H5I H 0.9319 0.3429 0.8984 0.048(15) Uiso 1 1 calc R . . C6I C 1.0742(7) 0.3923(4) 0.8979(3) 0.094(3) Uani 1 1 d . . . H6I1 H 1.1043 0.3611 0.8766 0.104(14) Uiso 1 1 calc R . . H6I2 H 1.1300 0.4045 0.9191 0.104(14) Uiso 1 1 calc R . . H6I3 H 1.0490 0.4322 0.8827 0.104(14) Uiso 1 1 calc R . . C7I C 0.9199(8) 0.4119(4) 0.9487(3) 0.107(3) Uani 1 1 d . . . H7I1 H 0.8482 0.3944 0.9556 0.15(2) Uiso 1 1 calc R . . H7I2 H 0.9124 0.4533 0.9322 0.15(2) Uiso 1 1 calc R . . H7I3 H 0.9594 0.4205 0.9758 0.15(2) Uiso 1 1 calc R . . C1J C 1.0770(5) 0.1086(3) 0.88534(18) 0.0482(14) Uani 1 1 d . . . H1J1 H 1.0017 0.0938 0.8854 0.072 Uiso 1 1 calc R . . H1J2 H 1.1232 0.0729 0.8744 0.072 Uiso 1 1 calc R . . H1J3 H 1.0843 0.1476 0.8665 0.072 Uiso 1 1 calc R . . C2J C 1.1666(4) 0.0733(3) 0.95393(18) 0.0434(13) Uani 1 1 d . . . H2J H 1.1879 0.0913 0.9831 0.068(19) Uiso 1 1 calc R . . C3J C 1.2694(4) 0.0542(3) 0.92936(17) 0.0407(13) Uani 1 1 d . . . C4J C 1.0955(5) 0.0123(3) 0.9614(2) 0.066(2) Uani 1 1 d . . . H4J1 H 1.0728 -0.0051 0.9326 0.091(16) Uiso 1 1 calc R . . H4J2 H 1.1398 -0.0224 0.9756 0.091(16) Uiso 1 1 calc R . . C5J C 0.9969(6) 0.0233(4) 0.9885(4) 0.100(3) Uani 1 1 d . . . H5J H 0.9531 0.0585 0.9739 0.08(2) Uiso 1 1 calc R . . C6J C 0.9296(6) -0.0413(4) 0.9883(4) 0.125(4) Uani 1 1 d . . . H6J1 H 0.9146 -0.0544 0.9581 0.187 Uiso 0.50 1 calc PR . . H6J2 H 0.8614 -0.0338 1.0037 0.187 Uiso 0.50 1 calc PR . . H6J3 H 0.9700 -0.0766 1.0029 0.187 Uiso 0.50 1 calc PR . . H6J4 H 0.9161 -0.0554 1.0184 0.187 Uiso 0.50 1 calc PR . . H6J5 H 0.9693 -0.0761 0.9728 0.187 Uiso 0.50 1 calc PR . . H6J6 H 0.8607 -0.0332 0.9735 0.187 Uiso 0.50 1 calc PR . . C7J C 1.0245(11) 0.0474(5) 1.0330(5) 0.163(6) Uani 1 1 d . . . H7J1 H 1.0780 0.0178 1.0462 0.15(2) Uiso 1 1 calc R . . H7J2 H 0.9593 0.0481 1.0511 0.15(2) Uiso 1 1 calc R . . H7J3 H 1.0543 0.0923 1.0310 0.15(2) Uiso 1 1 calc R . . C1K C 1.3404(5) 0.1685(3) 0.94096(18) 0.0469(14) Uani 1 1 d . . . H1K1 H 1.4134 0.1834 0.9482 0.056(9) Uiso 1 1 calc R . . H1K2 H 1.2959 0.1683 0.9674 0.056(9) Uiso 1 1 calc R . . H1K3 H 1.3087 0.1986 0.9194 0.056(9) Uiso 1 1 calc R . . C2K C 1.4371(4) 0.0856(3) 0.89426(16) 0.0395(13) Uani 1 1 d . . . H2K H 1.4267 0.0395 0.8830 0.009(9) Uiso 1 1 calc R . . C3K C 1.5388(4) 0.0863(3) 0.92221(17) 0.0397(13) Uani 1 1 d . . . C4K C 1.4459(4) 0.1321(3) 0.85491(18) 0.0508(15) Uani 1 1 d . . . H4K H 1.4698 0.1767 0.8654 0.041(14) Uiso 1 1 calc R . . C5K C 1.3376(5) 0.1395(3) 0.83215(19) 0.0608(17) Uani 1 1 d . . . H5K1 H 1.3478 0.1625 0.8043 0.069(11) Uiso 1 1 calc R . . H5K2 H 1.2887 0.1653 0.8507 0.069(11) Uiso 1 1 calc R . . H5K3 H 1.3067 0.0956 0.8268 0.069(11) Uiso 1 1 calc R . . C6K C 1.5300(5) 0.1052(4) 0.8238(2) 0.0612(17) Uani 1 1 d . . . H6K1 H 1.5991 0.1009 0.8391 0.066(10) Uiso 1 1 calc R . . H6K2 H 1.5382 0.1356 0.7991 0.066(10) Uiso 1 1 calc R . . H6K3 H 1.5072 0.0616 0.8131 0.066(10) Uiso 1 1 calc R . . OW1 O 1.0403(3) -0.1726(2) 0.90402(12) 0.0662(12) Uani 1 1 d U . . OW2 O 1.0638(5) 0.2220(3) 1.07397(16) 0.0996(17) Uani 1 1 d U . . OW3 O 0.871(2) -0.0648(13) 0.8978(9) 0.198(9) Uani 0.40 1 d PU . . O13 O 0.8677(12) 0.1851(8) 1.1136(5) 0.142(5) Uani 0.50 1 d PU . . C13 C 0.909(3) 0.172(2) 1.1607(12) 0.219(14) Uani 0.50 1 d PU . . H13 H 0.9272 0.1969 1.1021 0.328 Uiso 0.50 1 d P . . H13A H 0.9185 0.2152 1.1754 0.328 Uiso 0.50 1 d P . . H13B H 0.9658 0.1449 1.1613 0.328 Uiso 0.50 1 d P . . H13C H 0.8422 0.1516 1.1752 0.328 Uiso 0.50 1 d P . . HW11 H 1.0912 -0.1601 0.9238 0.328 Uiso 1 1 d . . . HW12 H 1.0362 -0.1523 0.8772 0.328 Uiso 1 1 d . . . HW21 H 1.1053 0.2027 1.0524 0.328 Uiso 1 1 d . . . HW22 H 1.0686 0.2676 1.0801 0.328 Uiso 1 1 d . . . HW31 H 0.9144 -0.0930 0.9006 0.328 Uiso 0.40 1 d P . . HW32 H 0.8554 -0.0263 0.8863 0.328 Uiso 0.20 1 d P . . HW33 H 0.8031 -0.0527 0.8913 0.328 Uiso 0.20 1 d P . . 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 0.052(2) 0.057(2) 0.042(2) 0.0113(18) -0.0130(19) 0.007(2) O2 0.069(3) 0.043(2) 0.055(2) 0.004(2) -0.023(2) 0.000(2) O3 0.048(2) 0.060(2) 0.043(2) -0.0040(19) 0.0019(18) -0.016(2) O4 0.060(2) 0.050(2) 0.031(2) -0.0024(17) 0.0028(18) 0.0075(19) O5 0.119(4) 0.048(2) 0.032(2) -0.0020(19) -0.011(2) 0.011(2) O6 0.066(3) 0.060(3) 0.046(2) 0.013(2) 0.009(2) 0.013(2) O7 0.072(3) 0.040(2) 0.035(2) 0.0056(17) -0.0049(19) -0.0073(19) O8 0.043(2) 0.046(2) 0.0349(19) 0.0057(17) 0.0056(17) -0.0007(18) O9 0.060(2) 0.058(3) 0.038(2) 0.0084(18) 0.0013(19) 0.010(2) O10 0.043(2) 0.036(2) 0.067(3) 0.0038(19) 0.0015(19) 0.0001(18) O11 0.050(2) 0.050(2) 0.059(2) -0.0030(19) -0.003(2) -0.009(2) O12 0.054(3) 0.110(4) 0.045(2) 0.014(2) 0.006(2) 0.002(3) N1 0.042(2) 0.053(3) 0.036(2) 0.002(2) -0.009(2) -0.003(2) N2 0.055(3) 0.038(3) 0.039(3) 0.008(2) -0.013(2) 0.000(2) N3 0.059(3) 0.032(3) 0.027(2) 0.0063(19) -0.007(2) -0.003(2) N4 0.043(2) 0.039(3) 0.027(2) 0.0016(19) -0.0027(19) -0.006(2) N5 0.047(3) 0.042(3) 0.029(2) 0.001(2) -0.001(2) 0.008(2) N6 0.051(3) 0.037(3) 0.040(3) 0.000(2) -0.001(2) 0.001(2) N7 0.054(3) 0.051(3) 0.037(3) 0.004(2) 0.001(2) 0.009(2) N8 0.049(3) 0.036(3) 0.034(3) -0.003(2) 0.001(2) 0.000(2) N9 0.037(2) 0.035(2) 0.033(2) 0.0008(18) 0.000(2) -0.0040(19) N10 0.039(2) 0.034(3) 0.041(3) 0.005(2) 0.000(2) 0.003(2) N11 0.034(2) 0.038(3) 0.043(2) 0.004(2) 0.006(2) 0.001(2) C1A 0.040(3) 0.085(5) 0.058(4) 0.007(3) -0.013(3) -0.012(3) C2A 0.054(3) 0.049(4) 0.034(3) 0.001(3) -0.004(3) 0.010(3) C3A 0.046(3) 0.034(3) 0.041(3) 0.002(2) -0.008(3) 0.011(3) C4A 0.058(4) 0.067(4) 0.059(4) 0.001(3) -0.007(3) 0.025(3) C5A 0.085(5) 0.063(4) 0.050(4) 0.006(3) -0.002(4) 0.014(4) C6A 0.086(5) 0.062(4) 0.077(5) -0.023(4) 0.008(4) 0.005(4) C7A 0.088(5) 0.085(6) 0.109(7) -0.029(5) 0.009(5) -0.012(5) C8A 0.087(6) 0.137(9) 0.090(6) -0.075(7) 0.019(5) -0.020(5) C9A 0.143(9) 0.156(10) 0.136(9) -0.077(8) 0.023(7) -0.025(8) C10A 0.071(5) 0.095(6) 0.073(5) -0.015(4) 0.005(4) 0.027(4) C1B 0.059(4) 0.030(3) 0.040(3) -0.002(2) -0.012(3) -0.007(3) C2B 0.055(3) 0.032(3) 0.036(3) 0.006(2) -0.006(3) 0.000(3) C3B 0.066(4) 0.050(4) 0.044(3) -0.003(3) -0.011(3) -0.006(3) C4B 0.069(4) 0.077(5) 0.055(4) -0.006(4) 0.004(4) -0.012(4) C5B 0.099(6) 0.112(7) 0.065(5) -0.019(5) 0.012(4) 0.009(5) C1C 0.077(4) 0.040(3) 0.056(4) 0.010(3) -0.007(3) 0.000(3) C2C 0.054(3) 0.039(3) 0.030(3) 0.003(2) 0.001(2) -0.008(3) C3C 0.040(3) 0.035(3) 0.044(3) 0.001(2) -0.003(3) -0.002(3) C1D 0.047(3) 0.056(4) 0.034(3) 0.006(3) 0.003(3) -0.014(3) C2D 0.039(3) 0.042(3) 0.031(3) -0.001(2) -0.004(2) -0.002(3) C3D 0.042(3) 0.034(3) 0.040(3) 0.004(2) -0.001(3) -0.001(3) C4D 0.047(3) 0.046(3) 0.042(3) 0.004(3) -0.005(3) 0.006(3) C5D 0.072(4) 0.045(4) 0.048(4) 0.003(3) -0.005(3) 0.020(3) C6D 0.068(5) 0.083(5) 0.096(6) 0.001(4) -0.034(4) 0.016(4) C7D 0.110(6) 0.055(4) 0.061(4) 0.007(3) -0.017(4) 0.022(4) C1E 0.058(4) 0.038(3) 0.036(3) 0.003(2) -0.007(3) 0.002(3) C2E 0.059(4) 0.038(3) 0.034(3) 0.000(3) -0.012(3) 0.010(3) C3E 0.057(4) 0.050(4) 0.075(5) 0.006(3) -0.014(4) 0.002(3) C4E 0.077(5) 0.064(5) 0.136(7) 0.009(5) -0.021(5) -0.011(4) C5E 0.076(5) 0.076(5) 0.102(6) 0.018(5) -0.014(5) -0.003(4) C1F 0.076(4) 0.049(4) 0.033(3) 0.003(3) 0.003(3) 0.004(3) C2F 0.054(4) 0.031(3) 0.064(4) -0.001(3) -0.005(3) 0.003(3) C3F 0.053(3) 0.028(3) 0.052(4) 0.001(3) -0.002(3) 0.001(3) C4F 0.049(4) 0.047(4) 0.120(6) 0.003(4) 0.016(4) 0.001(3) C5F 0.066(5) 0.068(6) 0.161(9) 0.028(5) 0.029(5) 0.015(4) C6F 0.065(6) 0.175(12) 0.282(16) 0.093(11) 0.036(8) 0.039(7) C7F 0.098(6) 0.153(10) 0.118(8) 0.005(7) -0.033(6) 0.034(6) C1G 0.049(3) 0.039(3) 0.035(3) 0.006(2) 0.001(3) 0.004(3) C2G 0.044(3) 0.042(3) 0.033(3) 0.003(3) -0.003(2) -0.001(3) C3G 0.070(4) 0.056(4) 0.046(3) -0.007(3) 0.004(3) -0.012(3) C1H 0.037(3) 0.041(3) 0.039(3) -0.004(3) 0.007(2) 0.000(3) C2H 0.046(3) 0.030(3) 0.037(3) 0.001(2) 0.004(3) 0.004(2) C3H 0.043(3) 0.050(4) 0.065(4) -0.009(3) -0.005(3) 0.001(3) C1I 0.044(3) 0.065(4) 0.038(3) 0.005(3) 0.006(3) -0.008(3) C2I 0.035(3) 0.039(3) 0.038(3) -0.001(2) -0.001(2) 0.003(2) C3I 0.041(3) 0.048(4) 0.039(3) 0.005(3) 0.005(3) -0.002(3) C4I 0.056(4) 0.042(3) 0.052(4) -0.004(3) -0.005(3) 0.006(3) C5I 0.083(4) 0.037(3) 0.056(4) -0.001(3) -0.023(4) 0.003(3) C6I 0.128(7) 0.079(5) 0.075(5) 0.031(4) -0.026(5) -0.025(5) C7I 0.153(8) 0.066(5) 0.100(6) -0.018(5) -0.032(6) 0.044(5) C1J 0.044(3) 0.043(3) 0.057(4) -0.004(3) -0.007(3) -0.001(3) C2J 0.038(3) 0.044(3) 0.048(3) 0.014(3) -0.004(3) 0.001(3) C3J 0.036(3) 0.039(3) 0.047(3) 0.007(3) -0.003(3) 0.000(3) C4J 0.041(3) 0.056(4) 0.100(5) 0.037(4) 0.019(4) 0.004(3) C5J 0.071(5) 0.075(6) 0.154(9) 0.054(6) 0.066(6) 0.024(4) C6J 0.059(4) 0.081(6) 0.234(11) 0.074(7) 0.052(6) 0.002(4) C7J 0.195(12) 0.096(8) 0.198(13) 0.015(8) 0.154(11) -0.008(8) C1K 0.042(3) 0.044(3) 0.055(3) -0.009(3) 0.002(3) -0.004(3) C2K 0.038(3) 0.042(3) 0.038(3) 0.003(2) 0.005(2) 0.000(3) C3K 0.036(3) 0.042(3) 0.042(3) 0.002(3) 0.008(3) 0.002(3) C4K 0.046(3) 0.056(4) 0.050(3) 0.010(3) -0.004(3) -0.005(3) C5K 0.059(4) 0.076(5) 0.048(3) 0.024(3) 0.006(3) 0.007(4) C6K 0.056(4) 0.078(4) 0.050(4) 0.008(3) 0.005(3) -0.009(3) OW1 0.062(3) 0.091(3) 0.046(2) 0.003(2) -0.001(2) 0.014(2) OW2 0.128(4) 0.098(4) 0.073(3) -0.007(3) 0.011(3) 0.014(3) OW3 0.195(12) 0.190(12) 0.210(12) 0.011(9) 0.004(9) 0.005(9) O13 0.137(8) 0.126(8) 0.162(9) 0.032(7) 0.025(7) -0.018(7) C13 0.221(16) 0.213(16) 0.222(16) -0.010(10) 0.003(10) -0.009(10) _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 C3A 1.235(6) . ? O2 C2B 1.233(6) . ? O3 C3C 1.221(6) . ? O4 C3D 1.236(6) . ? O5 C2E 1.235(6) . ? O6 C3F 1.213(6) . ? O7 C2G 1.240(6) . ? O8 C2H 1.229(6) . ? O9 C3I 1.243(6) . ? O10 C3J 1.237(6) . ? O11 C3K 1.240(6) . ? O12 C4A 1.405(7) . ? N1 C3K 1.345(7) . ? N1 C2A 1.471(7) . ? N1 C1A 1.480(7) . ? N2 C3A 1.330(7) . ? N2 C1B 1.467(7) . ? N3 C2B 1.337(7) . ? N3 C2C 1.455(6) . ? N3 C1C 1.458(7) . ? N4 C3C 1.354(6) . ? N4 C2D 1.445(6) . ? N4 C1D 1.466(7) . ? N5 C3D 1.336(6) . ? N5 C1E 1.467(6) . ? N6 C2E 1.353(7) . ? N6 C2F 1.470(7) . ? N6 C1F 1.472(7) . ? N7 C3F 1.342(7) . ? N7 C1G 1.439(7) . ? N8 C2G 1.341(7) . ? N8 C1H 1.451(6) . ? N9 C2H 1.365(6) . ? N9 C1I 1.458(6) . ? N9 C2I 1.459(6) . ? N10 C3I 1.340(7) . ? N10 C1J 1.467(7) . ? N10 C2J 1.472(6) . ? N11 C3J 1.353(7) . ? N11 C1K 1.459(7) . ? N11 C2K 1.475(6) . ? C2A C3A 1.525(8) . ? C2A C4A 1.538(8) . ? C4A C5A 1.500(9) . ? C5A C10A 1.541(9) . ? C5A C6A 1.560(10) . ? C6A C7A 1.485(10) . ? C7A C8A 1.344(11) . ? C8A C9A 1.549(14) . ? C1B C3B 1.505(8) . ? C1B C2B 1.531(7) . ? C3B C4B 1.523(9) . ? C4B C5B 1.503(9) . ? C2C C3C 1.523(7) . ? C2D C3D 1.521(7) . ? C2D C4D 1.554(8) . ? C4D C5D 1.526(7) . ? C5D C7D 1.512(9) . ? C5D C6D 1.521(9) . ? C1E C2E 1.524(8) . ? C1E C3E 1.534(8) . ? C3E C5E 1.482(9) . ? C3E C4E 1.552(10) . ? C2F C4F 1.500(8) . ? C2F C3F 1.524(8) . ? C4F C5F 1.544(10) . ? C5F C6F 1.425(12) . ? C5F C7F 1.595(12) . ? C1G C2G 1.512(7) . ? C1G C3G 1.540(8) . ? C1H C3H 1.516(8) . ? C1H C2H 1.531(7) . ? C2I C3I 1.529(8) . ? C2I C4I 1.541(7) . ? C4I C5I 1.520(8) . ? C5I C6I 1.482(10) . ? C5I C7I 1.546(10) . ? C2J C3J 1.530(8) . ? C2J C4J 1.531(8) . ? C4J C5J 1.494(10) . ? C5J C7J 1.488(16) . ? C5J C6J 1.547(12) . ? C2K C3K 1.524(7) . ? C2K C4K 1.532(7) . ? C4K C6K 1.513(8) . ? C4K C5K 1.520(8) . ? O13 C13 1.56(4) . ? 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 C3K N1 C2A 124.2(4) . . ? C3K N1 C1A 114.8(5) . . ? C2A N1 C1A 117.1(5) . . ? C3A N2 C1B 122.5(4) . . ? C2B N3 C2C 116.3(4) . . ? C2B N3 C1C 123.9(5) . . ? C2C N3 C1C 115.4(4) . . ? C3C N4 C2D 119.0(4) . . ? C3C N4 C1D 121.7(4) . . ? C2D N4 C1D 118.8(4) . . ? C3D N5 C1E 121.7(4) . . ? C2E N6 C2F 118.4(4) . . ? C2E N6 C1F 124.2(4) . . ? C2F N6 C1F 115.9(4) . . ? C3F N7 C1G 123.1(5) . . ? C2G N8 C1H 122.1(4) . . ? C2H N9 C1I 123.7(4) . . ? C2H N9 C2I 118.9(4) . . ? C1I N9 C2I 117.4(4) . . ? C3I N10 C1J 124.3(4) . . ? C3I N10 C2J 120.3(4) . . ? C1J N10 C2J 115.2(4) . . ? C3J N11 C1K 124.7(4) . . ? C3J N11 C2K 118.0(4) . . ? C1K N11 C2K 117.3(4) . . ? N1 C2A C3A 111.3(4) . . ? N1 C2A C4A 108.4(5) . . ? C3A C2A C4A 112.9(5) . . ? O1 C3A N2 122.2(5) . . ? O1 C3A C2A 121.5(5) . . ? N2 C3A C2A 116.3(5) . . ? O12 C4A C5A 108.8(5) . . ? O12 C4A C2A 107.3(5) . . ? C5A C4A C2A 114.9(6) . . ? C4A C5A C10A 107.5(6) . . ? C4A C5A C6A 110.9(5) . . ? C10A C5A C6A 112.2(5) . . ? C7A C6A C5A 112.8(6) . . ? C8A C7A C6A 123.5(9) . . ? C7A C8A C9A 118.7(12) . . ? N2 C1B C3B 111.7(4) . . ? N2 C1B C2B 106.0(4) . . ? C3B C1B C2B 111.3(5) . . ? O2 C2B N3 121.7(5) . . ? O2 C2B C1B 118.0(5) . . ? N3 C2B C1B 120.3(5) . . ? C1B C3B C4B 114.7(5) . . ? C5B C4B C3B 113.0(6) . . ? N3 C2C C3C 109.3(4) . . ? O3 C3C N4 122.5(5) . . ? O3 C3C C2C 119.7(5) . . ? N4 C3C C2C 117.7(4) . . ? N4 C2D C3D 114.9(4) . . ? N4 C2D C4D 112.9(4) . . ? C3D C2D C4D 109.9(4) . . ? O4 C3D N5 123.4(5) . . ? O4 C3D C2D 119.4(5) . . ? N5 C3D C2D 117.2(5) . . ? C5D C4D C2D 115.2(4) . . ? C7D C5D C6D 110.7(6) . . ? C7D C5D C4D 109.8(5) . . ? C6D C5D C4D 111.6(5) . . ? N5 C1E C2E 107.3(4) . . ? N5 C1E C3E 111.1(4) . . ? C2E C1E C3E 110.7(5) . . ? O5 C2E N6 121.2(5) . . ? O5 C2E C1E 119.5(5) . . ? N6 C2E C1E 119.4(5) . . ? C5E C3E C1E 115.3(6) . . ? C5E C3E C4E 108.9(6) . . ? C1E C3E C4E 108.6(5) . . ? N6 C2F C4F 112.4(5) . . ? N6 C2F C3F 109.1(4) . . ? C4F C2F C3F 113.3(5) . . ? O6 C3F N7 123.6(5) . . ? O6 C3F C2F 123.2(5) . . ? N7 C3F C2F 113.2(5) . . ? C2F C4F C5F 115.3(6) . . ? C6F C5F C4F 111.1(7) . . ? C6F C5F C7F 112.8(9) . . ? C4F C5F C7F 110.7(7) . . ? N7 C1G C2G 108.0(4) . . ? N7 C1G C3G 112.2(4) . . ? C2G C1G C3G 111.1(4) . . ? O7 C2G N8 122.6(5) . . ? O7 C2G C1G 121.6(5) . . ? N8 C2G C1G 115.7(4) . . ? N8 C1H C3H 109.6(4) . . ? N8 C1H C2H 107.4(4) . . ? C3H C1H C2H 109.3(4) . . ? O8 C2H N9 122.2(5) . . ? O8 C2H C1H 119.5(4) . . ? N9 C2H C1H 118.3(5) . . ? N9 C2I C3I 111.0(4) . . ? N9 C2I C4I 110.3(4) . . ? C3I C2I C4I 112.3(4) . . ? O9 C3I N10 121.7(5) . . ? O9 C3I C2I 119.3(5) . . ? N10 C3I C2I 119.0(5) . . ? C5I C4I C2I 113.0(4) . . ? C6I C5I C4I 111.6(6) . . ? C6I C5I C7I 111.1(6) . . ? C4I C5I C7I 110.5(5) . . ? N10 C2J C3J 109.5(4) . . ? N10 C2J C4J 112.2(4) . . ? C3J C2J C4J 110.6(5) . . ? O10 C3J N11 121.6(5) . . ? O10 C3J C2J 120.1(5) . . ? N11 C3J C2J 118.2(5) . . ? C5J C4J C2J 115.8(6) . . ? C7J C5J C4J 111.7(8) . . ? C7J C5J C6J 113.8(8) . . ? C4J C5J C6J 108.3(7) . . ? N11 C2K C3K 107.7(4) . . ? N11 C2K C4K 112.9(4) . . ? C3K C2K C4K 112.2(4) . . ? O11 C3K N1 119.9(5) . . ? O11 C3K C2K 118.9(5) . . ? N1 C3K C2K 121.0(5) . . ? C6K C4K C5K 110.8(5) . . ? C6K C4K C2K 109.0(5) . . ? C5K C4K C2K 111.0(4) . . ? 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 C3K N1 C2A C3A -137.4(5) . . . . ? C1A N1 C2A C3A 66.2(6) . . . . ? C3K N1 C2A C4A 97.9(6) . . . . ? C1A N1 C2A C4A -58.4(6) . . . . ? C1B N2 C3A O1 -4.1(8) . . . . ? C1B N2 C3A C2A 173.3(4) . . . . ? N1 C2A C3A O1 -71.5(6) . . . . ? C4A C2A C3A O1 50.6(7) . . . . ? N1 C2A C3A N2 111.0(5) . . . . ? C4A C2A C3A N2 -126.9(5) . . . . ? N1 C2A C4A O12 -58.9(6) . . . . ? C3A C2A C4A O12 177.4(5) . . . . ? N1 C2A C4A C5A 180.0(5) . . . . ? C3A C2A C4A C5A 56.3(7) . . . . ? O12 C4A C5A C10A 66.3(6) . . . . ? C2A C4A C5A C10A -173.3(5) . . . . ? O12 C4A C5A C6A -56.7(7) . . . . ? C2A C4A C5A C6A 63.6(7) . . . . ? C4A C5A C6A C7A 167.3(6) . . . . ? C10A C5A C6A C7A 47.0(9) . . . . ? C5A C6A C7A C8A -122.7(8) . . . . ? C6A C7A C8A C9A -177.7(8) . . . . ? C3A N2 C1B C3B 92.0(6) . . . . ? C3A N2 C1B C2B -146.6(5) . . . . ? C2C N3 C2B O2 15.0(7) . . . . ? C1C N3 C2B O2 170.6(5) . . . . ? C2C N3 C2B C1B -164.8(4) . . . . ? C1C N3 C2B C1B -9.3(7) . . . . ? N2 C1B C2B O2 -51.3(6) . . . . ? C3B C1B C2B O2 70.4(6) . . . . ? N2 C1B C2B N3 128.5(5) . . . . ? C3B C1B C2B N3 -109.8(6) . . . . ? N2 C1B C3B C4B 178.6(5) . . . . ? C2B C1B C3B C4B 60.2(7) . . . . ? C1B C3B C4B C5B 172.8(6) . . . . ? C2B N3 C2C C3C 76.4(6) . . . . ? C1C N3 C2C C3C -81.3(5) . . . . ? C2D N4 C3C O3 5.8(7) . . . . ? C1D N4 C3C O3 178.0(5) . . . . ? C2D N4 C3C C2C -172.5(4) . . . . ? C1D N4 C3C C2C -0.3(7) . . . . ? N3 C2C C3C O3 -1.6(6) . . . . ? N3 C2C C3C N4 176.8(4) . . . . ? C3C N4 C2D C3D -116.6(5) . . . . ? C1D N4 C2D C3D 70.9(6) . . . . ? C3C N4 C2D C4D 116.2(5) . . . . ? C1D N4 C2D C4D -56.2(6) . . . . ? C1E N5 C3D O4 3.2(7) . . . . ? C1E N5 C3D C2D -176.7(4) . . . . ? N4 C2D C3D O4 -169.6(4) . . . . ? C4D C2D C3D O4 -41.0(6) . . . . ? N4 C2D C3D N5 10.3(6) . . . . ? C4D C2D C3D N5 139.0(5) . . . . ? N4 C2D C4D C5D -51.6(6) . . . . ? C3D C2D C4D C5D 178.7(5) . . . . ? C2D C4D C5D C7D 173.3(5) . . . . ? C2D C4D C5D C6D -63.5(7) . . . . ? C3D N5 C1E C2E -119.0(5) . . . . ? C3D N5 C1E C3E 119.8(5) . . . . ? C2F N6 C2E O5 3.7(8) . . . . ? C1F N6 C2E O5 -161.5(5) . . . . ? C2F N6 C2E C1E -174.6(4) . . . . ? C1F N6 C2E C1E 20.2(8) . . . . ? N5 C1E C2E O5 -49.6(7) . . . . ? C3E C1E C2E O5 71.8(7) . . . . ? N5 C1E C2E N6 128.7(5) . . . . ? C3E C1E C2E N6 -109.9(6) . . . . ? N5 C1E C3E C5E 171.1(5) . . . . ? C2E C1E C3E C5E 52.0(8) . . . . ? N5 C1E C3E C4E -66.5(7) . . . . ? C2E C1E C3E C4E 174.4(5) . . . . ? C2E N6 C2F C4F 137.9(6) . . . . ? C1F N6 C2F C4F -55.6(7) . . . . ? C2E N6 C2F C3F -95.6(6) . . . . ? C1F N6 C2F C3F 70.9(6) . . . . ? C1G N7 C3F O6 1.5(8) . . . . ? C1G N7 C3F C2F -176.8(5) . . . . ? N6 C2F C3F O6 -96.9(6) . . . . ? C4F C2F C3F O6 29.1(8) . . . . ? N6 C2F C3F N7 81.4(6) . . . . ? C4F C2F C3F N7 -152.6(5) . . . . ? N6 C2F C4F C5F -54.6(9) . . . . ? C3F C2F C4F C5F -178.8(7) . . . . ? C2F C4F C5F C6F -176.8(9) . . . . ? C2F C4F C5F C7F -50.7(10) . . . . ? C3F N7 C1G C2G -137.9(5) . . . . ? C3F N7 C1G C3G 99.3(6) . . . . ? C1H N8 C2G O7 3.3(8) . . . . ? C1H N8 C2G C1G -177.2(4) . . . . ? N7 C1G C2G O7 -52.7(6) . . . . ? C3G C1G C2G O7 70.7(6) . . . . ? N7 C1G C2G N8 127.7(5) . . . . ? C3G C1G C2G N8 -108.9(5) . . . . ? C2G N8 C1H C3H -158.4(5) . . . . ? C2G N8 C1H C2H 83.0(6) . . . . ? C1I N9 C2H O8 178.6(5) . . . . ? C2I N9 C2H O8 0.8(7) . . . . ? C1I N9 C2H C1H -1.8(7) . . . . ? C2I N9 C2H C1H -179.7(4) . . . . ? N8 C1H C2H O8 46.1(6) . . . . ? C3H C1H C2H O8 -72.6(6) . . . . ? N8 C1H C2H N9 -133.4(4) . . . . ? C3H C1H C2H N9 107.8(5) . . . . ? C2H N9 C2I C3I -124.6(5) . . . . ? C1I N9 C2I C3I 57.4(6) . . . . ? C2H N9 C2I C4I 110.3(5) . . . . ? C1I N9 C2I C4I -67.8(6) . . . . ? C1J N10 C3I O9 176.8(5) . . . . ? C2J N10 C3I O9 0.5(7) . . . . ? C1J N10 C3I C2I -4.5(7) . . . . ? C2J N10 C3I C2I 179.3(4) . . . . ? N9 C2I C3I O9 -118.4(5) . . . . ? C4I C2I C3I O9 5.6(7) . . . . ? N9 C2I C3I N10 62.9(6) . . . . ? C4I C2I C3I N10 -173.1(4) . . . . ? N9 C2I C4I C5I -66.9(6) . . . . ? C3I C2I C4I C5I 168.7(5) . . . . ? C2I C4I C5I C6I -85.3(7) . . . . ? C2I C4I C5I C7I 150.5(6) . . . . ? C3I N10 C2J C3J -123.7(5) . . . . ? C1J N10 C2J C3J 59.7(6) . . . . ? C3I N10 C2J C4J 113.0(6) . . . . ? C1J N10 C2J C4J -63.6(6) . . . . ? C1K N11 C3J O10 -175.4(5) . . . . ? C2K N11 C3J O10 7.0(7) . . . . ? C1K N11 C3J C2J 5.6(7) . . . . ? C2K N11 C3J C2J -172.0(4) . . . . ? N10 C2J C3J O10 -118.4(5) . . . . ? C4J C2J C3J O10 5.8(7) . . . . ? N10 C2J C3J N11 60.6(6) . . . . ? C4J C2J C3J N11 -175.2(5) . . . . ? N10 C2J C4J C5J -62.4(8) . . . . ? C3J C2J C4J C5J 174.9(6) . . . . ? C2J C4J C5J C7J -59.9(9) . . . . ? C2J C4J C5J C6J 174.0(7) . . . . ? C3J N11 C2K C3K -115.0(5) . . . . ? C1K N11 C2K C3K 67.1(5) . . . . ? C3J N11 C2K C4K 120.6(5) . . . . ? C1K N11 C2K C4K -57.2(6) . . . . ? C2A N1 C3K O11 -159.7(5) . . . . ? C1A N1 C3K O11 -2.8(7) . . . . ? C2A N1 C3K C2K 26.3(7) . . . . ? C1A N1 C3K C2K -176.9(4) . . . . ? N11 C2K C3K O11 -90.2(5) . . . . ? C4K C2K C3K O11 34.6(6) . . . . ? N11 C2K C3K N1 84.0(6) . . . . ? C4K C2K C3K N1 -151.3(5) . . . . ? N11 C2K C4K C6K -170.6(4) . . . . ? C3K C2K C4K C6K 67.5(6) . . . . ? N11 C2K C4K C5K -48.4(7) . . . . ? C3K C2K C4K C5K -170.2(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O12 H12 O7 0.84 2.14 2.847(6) 141.9 1_655 O12 H12 OW3 0.84 2.23 2.89(3) 135.3 1_655 N2 H2 O10 0.88 2.16 2.997(6) 157.8 . N5 H5 OW1 0.88 2.29 3.126(6) 158.3 . N7 H7 O5 0.88 2.43 3.104(6) 133.3 . N8 H8 O4 0.88 1.91 2.788(6) 172.9 3_756 O13 H13 OW2 0.852(14) 1.967(6) 2.819(15) 178.1(12) . OW1 HW12 O5 0.919(4) 1.876(4) 2.792(5) 173.4(3) . OW1 HW11 O2 0.911(4) 1.976(4) 2.881(5) 172.8(3) . OW2 HW22 O11 0.940(6) 1.913(4) 2.823(7) 162.3(3) 4_457 OW2 HW21 O9 0.923(5) 1.980(4) 2.755(6) 140.4(4) . OW3 HW31 OW1 0.79(3) 2.242(4) 3.03(3) 176.4(19) . OW3 HW32 O7 0.87(3) 1.980(4) 2.85(3) 174.9(18) . OW3 HW33 O12 0.90(3) 1.993(4) 2.89(3) 175.8(18) 1_455 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.417 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.050 data_CsG_II _database_code_CSD 195321 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cyclosporin G crystal form II ex MeOH and Mg (ClO4)2 LT ; _chemical_name_common 'cyclosporin G' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C63 H113 O12 N11. 2.4H2O CH3OH' _chemical_formula_sum 'C64 H121.80 N11 O15.40' _chemical_formula_weight 1291.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.4300(17) _cell_length_b 20.256(3) _cell_length_c 30.617(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7708.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 119743 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 27 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type SORTAV _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details ; SORTAV absorption correction software package: R.H. Blessing (1997) ; _exptl_special_details ; Oxford Cryosystems Cryostream cooler: J. Cosier and A.M. Glazer (1986) ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 119743 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.10 _reflns_number_total 6702 _reflns_number_gt 5480 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Collect Data collection and processing user interface: Collect: Data collection software, R. Hooft, Nonius B.V.(1998) ; _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution 'SHELX-S (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1998)' _computing_publication_material SHELX97 _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^)+(0.0930P)^2^+2.3760P] 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 0.0022(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 -0.8(13) _refine_ls_number_reflns 6702 _refine_ls_number_parameters 905 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _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 1.5707(3) -0.09323(15) 1.00247(10) 0.0497(8) Uani 1 1 d . . . O2 O 1.1955(3) -0.14274(15) 0.97113(10) 0.0526(8) Uani 1 1 d . . . O3 O 1.3272(3) -0.24882(16) 0.91236(9) 0.0484(8) Uani 1 1 d . . . O4 O 1.2083(3) -0.29841(16) 0.76983(9) 0.0466(8) Uani 1 1 d . . . O5 O 1.0430(4) -0.10992(16) 0.82305(10) 0.0673(11) Uani 1 1 d . . . O6 O 0.9964(3) 0.03785(16) 0.71253(10) 0.0538(8) Uani 1 1 d . . . O7 O 0.8287(3) 0.05849(14) 0.85552(9) 0.0486(8) Uani 1 1 d . . . O8 O 0.9598(2) 0.23534(14) 0.83795(9) 0.0397(7) Uani 1 1 d . . . O9 O 1.1103(2) 0.19269(15) 0.98774(9) 0.0450(7) Uani 1 1 d . . . O10 O 1.2801(2) -0.00370(14) 0.91563(10) 0.0436(7) Uani 1 1 d . . . O11 O 1.5887(2) 0.13739(15) 0.92715(10) 0.0481(8) Uani 1 1 d . . . O12 O 1.6545(3) -0.0288(2) 0.87318(11) 0.0636(9) Uani 1 1 d . . . H12 H 1.7200 -0.0188 0.8725 0.10(3) Uiso 1 1 calc R . . N1 N 1.5681(3) 0.03157(18) 0.94624(11) 0.0401(8) Uani 1 1 d . . . N2 N 1.4004(3) -0.09155(16) 0.97711(11) 0.0408(9) Uani 1 1 d . . . H2 H 1.3561 -0.0762 0.9571 0.032(11) Uiso 1 1 calc R . . N3 N 1.2637(3) -0.23932(16) 0.99400(10) 0.0372(8) Uani 1 1 d . . . N4 N 1.1854(3) -0.30821(16) 0.88742(10) 0.0336(8) Uani 1 1 d . . . N5 N 1.1022(3) -0.24229(17) 0.81629(11) 0.0398(8) Uani 1 1 d . . . H5 H 1.0886 -0.2330 0.8438 0.051(13) Uiso 1 1 calc R . . N6 N 1.0850(3) -0.09997(17) 0.75142(11) 0.0420(9) Uani 1 1 d . . . N7 N 0.9398(3) 0.01317(18) 0.78047(12) 0.0469(10) Uani 1 1 d . . . H7 H 0.9563 -0.0067 0.8051 0.051(14) Uiso 1 1 calc R . . N8 N 0.7979(3) 0.14872(16) 0.81444(10) 0.0351(8) Uani 1 1 d . . . H8 H 0.7901 0.1645 0.7879 0.024(10) Uiso 1 1 calc R . . N9 N 0.9217(3) 0.21323(15) 0.90897(10) 0.0327(8) Uani 1 1 d . . . N10 N 1.1090(3) 0.12481(16) 0.92943(11) 0.0358(8) Uani 1 1 d . . . N11 N 1.3445(3) 0.09968(16) 0.92318(11) 0.0352(8) Uani 1 1 d . . . C1A C 1.6637(4) 0.0406(3) 0.97376(16) 0.0556(13) Uani 1 1 d . . . H1A1 H 1.6719 0.0024 0.9931 0.062(8) Uiso 1 1 calc R . . H1A2 H 1.6555 0.0807 0.9913 0.062(8) Uiso 1 1 calc R . . H1A3 H 1.7276 0.0446 0.9552 0.062(8) Uiso 1 1 calc R . . C2A C 1.5380(4) -0.0367(2) 0.93474(12) 0.0390(10) Uani 1 1 d . . . H2A H 1.4753 -0.0348 0.9143 0.047 Uiso 1 1 calc R . . C3A C 1.5043(4) -0.0753(2) 0.97489(14) 0.0388(10) Uani 1 1 d . . . C4A C 1.6339(4) -0.0681(3) 0.91014(15) 0.0545(13) Uani 1 1 d . . . H4A H 1.6985 -0.0666 0.9296 0.040(11) Uiso 1 1 calc R . . C5A C 1.6160(5) -0.1385(3) 0.89603(17) 0.0629(15) Uani 1 1 d . . . H5A H 1.5962 -0.1656 0.9221 0.10(2) Uiso 1 1 calc R . . C6A C 1.5243(5) -0.1430(3) 0.86188(18) 0.0670(15) Uani 1 1 d . . . H6A1 H 1.4551 -0.1329 0.8765 0.13(2) Uiso 1 1 calc R . . H6A2 H 1.5362 -0.1089 0.8392 0.13(2) Uiso 1 1 calc R . . C7A C 1.5157(5) -0.2082(4) 0.8404(2) 0.0799(18) Uani 1 1 d . . . H7A H 1.5048 -0.2456 0.8586 0.23(6) Uiso 1 1 calc R . . C8A C 1.5220(5) -0.2183(3) 0.7984(2) 0.0760(18) Uani 1 1 d . . . H8A H 1.5356 -0.1815 0.7801 0.041(13) Uiso 1 1 calc R . . C9A C 1.5090(7) -0.2856(4) 0.7772(3) 0.115(3) Uani 1 1 d . . . H9A1 H 1.4444 -0.2855 0.7588 0.19(3) Uiso 1 1 calc R . . H9A2 H 1.5018 -0.3194 0.7998 0.19(3) Uiso 1 1 calc R . . H9A3 H 1.5722 -0.2952 0.7591 0.19(3) Uiso 1 1 calc R . . C10A C 1.7232(5) -0.1640(3) 0.8773(2) 0.0731(17) Uani 1 1 d . . . H10A H 1.7160 -0.2108 0.8697 0.120(15) Uiso 1 1 calc R . . H10B H 1.7801 -0.1587 0.8992 0.120(15) Uiso 1 1 calc R . . H10C H 1.7418 -0.1387 0.8511 0.120(15) Uiso 1 1 calc R . . C1B C 1.3574(4) -0.1342(2) 1.01182(13) 0.0417(11) Uani 1 1 d . . . H1B H 1.4150 -0.1655 1.0214 0.027(10) Uiso 1 1 calc R . . C2B C 1.2656(4) -0.1736(2) 0.99086(13) 0.0385(10) Uani 1 1 d . . . C3B C 1.3192(4) -0.0954(2) 1.05088(15) 0.0515(12) Uani 1 1 d . . . H3B1 H 1.2641 -0.0634 1.0411 0.041(8) Uiso 1 1 calc R . . H3B2 H 1.3806 -0.0700 1.0628 0.041(8) Uiso 1 1 calc R . . C4B C 1.2721(5) -0.1372(3) 1.08711(16) 0.0620(14) Uani 1 1 d . . . H4B1 H 1.2060 -0.1590 1.0763 0.079(13) Uiso 1 1 calc R . . H4B2 H 1.3243 -0.1722 1.0949 0.079(13) Uiso 1 1 calc R . . C5B C 1.2451(6) -0.0982(4) 1.12751(19) 0.090(2) Uani 1 1 d . . . H5B1 H 1.2069 -0.0578 1.1192 0.16(2) Uiso 1 1 calc R . . H5B2 H 1.3116 -0.0866 1.1429 0.16(2) Uiso 1 1 calc R . . H5B3 H 1.1993 -0.1248 1.1467 0.16(2) Uiso 1 1 calc R . . C1C C 1.3528(4) -0.2789(2) 1.01134(16) 0.0530(13) Uani 1 1 d . . . H1C1 H 1.3283 -0.3243 1.0163 0.073(9) Uiso 1 1 calc R . . H1C2 H 1.3774 -0.2598 1.0390 0.073(9) Uiso 1 1 calc R . . H1C3 H 1.4123 -0.2790 0.9903 0.073(9) Uiso 1 1 calc R . . C2C C 1.1921(4) -0.2739(2) 0.96462(12) 0.0373(10) Uani 1 1 d . . . H2C1 H 1.1215 -0.2513 0.9637 0.033(7) Uiso 1 1 calc R . . H2C2 H 1.1806 -0.3196 0.9752 0.033(7) Uiso 1 1 calc R . . C3C C 1.2410(3) -0.2755(2) 0.91909(13) 0.0363(10) Uani 1 1 d . . . C1D C 1.0828(4) -0.3403(2) 0.89615(14) 0.0448(11) Uani 1 1 d . . . H1D1 H 1.0537 -0.3583 0.8689 0.066(8) Uiso 1 1 calc R . . H1D2 H 1.0322 -0.3080 0.9082 0.066(8) Uiso 1 1 calc R . . H1D3 H 1.0935 -0.3762 0.9172 0.066(8) Uiso 1 1 calc R . . C2D C 1.2379(3) -0.3185(2) 0.84526(12) 0.0337(9) Uani 1 1 d . . . H2D H 1.3109 -0.2978 0.8473 0.024(9) Uiso 1 1 calc R . . C3D C 1.1799(4) -0.2850(2) 0.80717(13) 0.0363(10) Uani 1 1 d . . . C4D C 1.2552(4) -0.3917(2) 0.83511(14) 0.0420(10) Uani 1 1 d . . . H4D1 H 1.2967 -0.3954 0.8076 0.034(7) Uiso 1 1 calc R . . H4D2 H 1.1842 -0.4126 0.8302 0.034(7) Uiso 1 1 calc R . . C5D C 1.3143(4) -0.4302(2) 0.87090(16) 0.0565(13) Uani 1 1 d . . . H5D H 1.2733 -0.4250 0.8988 0.054(13) Uiso 1 1 calc R . . C6D C 1.4276(5) -0.4046(3) 0.8780(2) 0.0741(17) Uani 1 1 d . . . H6D1 H 1.4632 -0.4310 0.9006 0.096(12) Uiso 1 1 calc R . . H6D2 H 1.4246 -0.3584 0.8874 0.096(12) Uiso 1 1 calc R . . H6D3 H 1.4683 -0.4078 0.8507 0.096(12) Uiso 1 1 calc R . . C7D C 1.3152(6) -0.5036(2) 0.85875(19) 0.0707(17) Uani 1 1 d . . . H7D1 H 1.3543 -0.5097 0.8313 0.084(11) Uiso 1 1 calc R . . H7D2 H 1.2410 -0.5193 0.8553 0.084(11) Uiso 1 1 calc R . . H7D3 H 1.3507 -0.5289 0.8819 0.084(11) Uiso 1 1 calc R . . C1E C 1.0380(4) -0.2100(2) 0.78229(14) 0.0452(11) Uani 1 1 d . . . H1E H 1.0649 -0.2245 0.7530 0.021(9) Uiso 1 1 calc R . . C2E C 1.0556(4) -0.1355(2) 0.78683(14) 0.0445(11) Uani 1 1 d . . . C3E C 0.9180(4) -0.2277(2) 0.7861(2) 0.0627(14) Uani 1 1 d . . . H3E H 0.8953 -0.2192 0.8169 0.013(8) Uiso 1 1 calc R . . C4E C 0.9026(6) -0.3017(3) 0.7769(3) 0.088(2) Uani 1 1 d . . . H4E1 H 0.9419 -0.3275 0.7987 0.113(14) Uiso 1 1 calc R . . H4E2 H 0.9302 -0.3121 0.7477 0.113(14) Uiso 1 1 calc R . . H4E3 H 0.8259 -0.3126 0.7783 0.113(14) Uiso 1 1 calc R . . C5E C 0.8450(5) -0.1899(3) 0.7571(2) 0.0812(18) Uani 1 1 d . . . H5E1 H 0.7704 -0.2029 0.7628 0.082(10) Uiso 1 1 calc R . . H5E2 H 0.8628 -0.1994 0.7265 0.082(10) Uiso 1 1 calc R . . H5E3 H 0.8536 -0.1426 0.7627 0.082(10) Uiso 1 1 calc R . . C1F C 1.0709(4) -0.1217(2) 0.70613(13) 0.0488(12) Uani 1 1 d . . . H1F1 H 1.0128 -0.0963 0.6925 0.073(9) Uiso 1 1 calc R . . H1F2 H 1.0526 -0.1687 0.7057 0.073(9) Uiso 1 1 calc R . . H1F3 H 1.1378 -0.1145 0.6899 0.073(9) Uiso 1 1 calc R . . C2F C 1.1116(4) -0.0301(2) 0.75785(17) 0.0484(12) Uani 1 1 d . . . H2F H 1.1283 -0.0236 0.7895 0.059(14) Uiso 1 1 calc R . . C3F C 1.0111(4) 0.0109(2) 0.74728(15) 0.0411(10) Uani 1 1 d . . . C4F C 1.2083(4) -0.0091(3) 0.7323(2) 0.0670(16) Uani 1 1 d . . . H4F1 H 1.2239 0.0377 0.7391 0.044(9) Uiso 1 1 calc R . . H4F2 H 1.1909 -0.0118 0.7008 0.044(9) Uiso 1 1 calc R . . C5F C 1.3100(5) -0.0500(3) 0.7409(3) 0.086(2) Uani 1 1 d . . . H5F H 1.2967 -0.0951 0.7288 0.060(15) Uiso 1 1 calc R . . C6F C 1.4019(6) -0.0221(5) 0.7166(4) 0.146(4) Uani 1 1 d . . . H6F1 H 1.4685 -0.0437 0.7260 0.16(2) Uiso 1 1 calc R . . H6F2 H 1.4068 0.0254 0.7224 0.16(2) Uiso 1 1 calc R . . H6F3 H 1.3914 -0.0294 0.6852 0.16(2) Uiso 1 1 calc R . . C7F C 1.3344(7) -0.0585(4) 0.7905(3) 0.111(3) Uani 1 1 d . . . H7F1 H 1.3491 -0.0152 0.8034 0.23(3) Uiso 1 1 calc R . . H7F2 H 1.3973 -0.0871 0.7942 0.23(3) Uiso 1 1 calc R . . H7F3 H 1.2721 -0.0785 0.8050 0.23(3) Uiso 1 1 calc R . . C1G C 0.8382(4) 0.0464(2) 0.77734(13) 0.0411(10) Uani 1 1 d . . . H1G H 0.8419 0.0784 0.7525 0.033(10) Uiso 1 1 calc R . . C2G C 0.8218(3) 0.0850(2) 0.81909(13) 0.0372(10) Uani 1 1 d . . . C3G C 0.7440(5) -0.0009(3) 0.76923(17) 0.0567(13) Uani 1 1 d . . . H3G1 H 0.6776 0.0246 0.7655 0.074(10) Uiso 1 1 calc R . . H3G2 H 0.7363 -0.0307 0.7942 0.074(10) Uiso 1 1 calc R . . H3G3 H 0.7579 -0.0267 0.7428 0.074(10) Uiso 1 1 calc R . . C1H C 0.7843(3) 0.1933(2) 0.85118(13) 0.0361(10) Uani 1 1 d . . . H1H H 0.7482 0.1696 0.8758 0.036(11) Uiso 1 1 calc R . . C2H C 0.8962(3) 0.21570(18) 0.86544(13) 0.0324(9) Uani 1 1 d . . . C3H C 0.7174(4) 0.2520(2) 0.83796(15) 0.0459(11) Uani 1 1 d . . . H3H1 H 0.6461 0.2371 0.8286 0.059(8) Uiso 1 1 calc R . . H3H2 H 0.7528 0.2752 0.8138 0.059(8) Uiso 1 1 calc R . . H3H3 H 0.7100 0.2821 0.8629 0.059(8) Uiso 1 1 calc R . . C1I C 0.8466(4) 0.1913(3) 0.94259(13) 0.0466(11) Uani 1 1 d . . . H1I1 H 0.8821 0.1926 0.9712 0.069(9) Uiso 1 1 calc R . . H1I2 H 0.8235 0.1461 0.9363 0.069(9) Uiso 1 1 calc R . . H1I3 H 0.7838 0.2206 0.9429 0.069(9) Uiso 1 1 calc R . . C2I C 1.0285(3) 0.23657(19) 0.92307(14) 0.0350(9) Uani 1 1 d . . . H2I H 1.0725 0.2453 0.8963 0.042(11) Uiso 1 1 calc R . . C3I C 1.0848(3) 0.1820(2) 0.94955(14) 0.0376(10) Uani 1 1 d . . . C4I C 1.0186(4) 0.3007(2) 0.94837(15) 0.0477(11) Uani 1 1 d . . . H4I1 H 0.9678 0.2941 0.9729 0.048(9) Uiso 1 1 calc R . . H4I2 H 1.0897 0.3119 0.9610 0.048(9) Uiso 1 1 calc R . . C5I C 0.9802(5) 0.3584(2) 0.92102(16) 0.0552(13) Uani 1 1 d . . . H5I H 0.9300 0.3409 0.8983 0.041(11) Uiso 1 1 calc R . . C6I C 1.0736(7) 0.3899(4) 0.8981(2) 0.102(3) Uani 1 1 d . . . H6I1 H 1.0480 0.4270 0.8804 0.114(14) Uiso 1 1 calc R . . H6I2 H 1.1085 0.3573 0.8792 0.114(14) Uiso 1 1 calc R . . H6I3 H 1.1254 0.4059 0.9198 0.114(14) Uiso 1 1 calc R . . C7I C 0.9187(8) 0.4088(3) 0.9484(2) 0.114(3) Uani 1 1 d . . . H7I1 H 0.8510 0.3892 0.9585 0.130(17) Uiso 1 1 calc R . . H7I2 H 0.9031 0.4479 0.9307 0.130(17) Uiso 1 1 calc R . . H7I3 H 0.9623 0.4216 0.9737 0.130(17) Uiso 1 1 calc R . . C1J C 1.0773(4) 0.1082(2) 0.88485(14) 0.0417(10) Uani 1 1 d . . . H1J1 H 1.0034 0.0912 0.8849 0.063 Uiso 1 1 calc R . . H1J2 H 1.1259 0.0745 0.8732 0.063 Uiso 1 1 calc R . . H1J3 H 1.0811 0.1478 0.8665 0.063 Uiso 1 1 calc R . . C2J C 1.1658(3) 0.0721(2) 0.95348(15) 0.0412(10) Uani 1 1 d . . . H2J H 1.1866 0.0900 0.9827 0.039(11) Uiso 1 1 calc R . . C3J C 1.2685(3) 0.0530(2) 0.92932(14) 0.0367(10) Uani 1 1 d . . . C4J C 1.0948(4) 0.0117(2) 0.96071(19) 0.0571(14) Uani 1 1 d . . . H4J1 H 1.0712 -0.0050 0.9319 0.074(12) Uiso 1 1 calc R . . H4J2 H 1.1389 -0.0233 0.9745 0.074(12) Uiso 1 1 calc R . . C5J C 0.9955(5) 0.0229(3) 0.9889(3) 0.091(2) Uani 1 1 d . . . H5J H 0.9510 0.0583 0.9749 0.12(3) Uiso 1 1 calc R . . C6J C 0.9294(5) -0.0407(3) 0.9896(3) 0.113(3) Uani 1 1 d . . . H6J1 H 0.8684 -0.0355 1.0096 0.129(17) Uiso 1 1 calc R . . H6J2 H 0.9749 -0.0773 0.9996 0.129(17) Uiso 1 1 calc R . . H6J3 H 0.9027 -0.0502 0.9602 0.129(17) Uiso 1 1 calc R . . C7J C 1.0269(9) 0.0460(4) 1.0350(4) 0.140(4) Uani 1 1 d . . . H7J1 H 1.0665 0.0877 1.0330 0.18(2) Uiso 1 1 calc R . . H7J2 H 1.0724 0.0125 1.0488 0.18(2) Uiso 1 1 calc R . . H7J3 H 0.9617 0.0524 1.0525 0.18(2) Uiso 1 1 calc R . . C1K C 1.3398(4) 0.1667(2) 0.94103(15) 0.0444(11) Uani 1 1 d . . . H1K1 H 1.4124 0.1813 0.9489 0.049(7) Uiso 1 1 calc R . . H1K2 H 1.2940 0.1671 0.9671 0.049(7) Uiso 1 1 calc R . . H1K3 H 1.3097 0.1967 0.9191 0.049(7) Uiso 1 1 calc R . . C2K C 1.4369(3) 0.0841(2) 0.89461(13) 0.0360(9) Uani 1 1 d . . . H2K H 1.4271 0.0381 0.8833 0.011(8) Uiso 1 1 calc R . . C3K C 1.5381(3) 0.0851(2) 0.92270(14) 0.0386(10) Uani 1 1 d . . . C4K C 1.4466(4) 0.1304(2) 0.85538(14) 0.0428(11) Uani 1 1 d . . . H4K H 1.4705 0.1748 0.8657 0.024(9) Uiso 1 1 calc R . . C5K C 1.3388(4) 0.1373(3) 0.83202(16) 0.0557(13) Uani 1 1 d . . . H5K1 H 1.2893 0.1629 0.8502 0.092(11) Uiso 1 1 calc R . . H5K2 H 1.3084 0.0933 0.8267 0.092(11) Uiso 1 1 calc R . . H5K3 H 1.3494 0.1599 0.8041 0.092(11) Uiso 1 1 calc R . . C6K C 1.5311(4) 0.1023(3) 0.82432(16) 0.0546(13) Uani 1 1 d . . . H6K1 H 1.5406 0.1323 0.7995 0.052(7) Uiso 1 1 calc R . . H6K2 H 1.5074 0.0590 0.8137 0.052(7) Uiso 1 1 calc R . . H6K3 H 1.5996 0.0974 0.8398 0.052(7) Uiso 1 1 calc R . . O13 O 0.8720(7) 0.1873(4) 1.1144(3) 0.158(3) Uani 1 1 d . . . C13 C 0.9017(14) 0.1742(5) 1.1595(4) 0.181(6) Uani 1 1 d . . . OW1 O 1.0388(3) -0.17174(19) 0.90417(10) 0.0670(10) Uani 1 1 d . . . OW2 O 1.0654(3) 0.22538(17) 1.07340(11) 0.0674(10) Uani 1 1 d . . . OW3 O 0.8709(16) -0.0646(9) 0.8953(9) 0.201(10) Uani 0.40 1 d P . . H13A H 0.9185 0.2152 1.1754 0.302 Uiso 1 1 d . . . H13B H 0.9658 0.1449 1.1613 0.302 Uiso 1 1 d . . . H13C H 0.8422 0.1516 1.1752 0.302 Uiso 1 1 d . . . HW11 H 1.1009 -0.1611 0.9321 0.302 Uiso 1 1 d . . . HW12 H 1.0544 -0.1347 0.8847 0.302 Uiso 1 1 d . . . HW21 H 1.0876 0.2063 1.0407 0.302 Uiso 1 1 d . . . HW22 H 1.0984 0.2724 1.0719 0.302 Uiso 1 1 d . . . HW31 H 0.9144 -0.0930 0.9006 0.302 Uiso 0.40 1 d P . . HW32 H 0.8554 -0.0263 0.8863 0.302 Uiso 0.20 1 d P . . HW33 H 0.8031 -0.0527 0.8913 0.302 Uiso 0.20 1 d P . . H13 H 0.9306 0.1992 1.1022 0.302 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0552(19) 0.0497(18) 0.0441(17) 0.0079(14) -0.0143(16) 0.0052(16) O2 0.066(2) 0.0402(17) 0.0520(19) 0.0046(15) -0.0168(17) 0.0011(17) O3 0.0514(19) 0.0574(19) 0.0364(16) -0.0034(14) 0.0030(14) -0.0189(17) O4 0.063(2) 0.0467(18) 0.0299(16) -0.0036(13) -0.0004(14) 0.0080(16) O5 0.124(3) 0.0421(17) 0.0357(18) -0.0017(15) -0.011(2) 0.015(2) O6 0.059(2) 0.0521(19) 0.0499(19) 0.0124(17) 0.0074(16) 0.0120(16) O7 0.073(2) 0.0373(16) 0.0355(16) 0.0061(14) -0.0067(15) -0.0074(16) O8 0.0445(16) 0.0415(16) 0.0330(15) 0.0065(13) 0.0045(14) -0.0026(14) O9 0.0526(18) 0.0496(17) 0.0329(16) 0.0052(13) -0.0013(14) 0.0062(15) O10 0.0419(17) 0.0300(16) 0.0588(19) 0.0035(14) 0.0047(15) 0.0019(13) O11 0.0406(17) 0.0457(18) 0.0579(19) -0.0023(15) -0.0002(15) -0.0091(15) O12 0.054(2) 0.092(3) 0.0452(19) 0.0015(19) 0.0059(16) 0.000(2) N1 0.0395(19) 0.044(2) 0.0370(18) -0.0005(16) -0.0057(17) -0.0030(17) N2 0.054(2) 0.0321(18) 0.0359(19) 0.0080(15) -0.0103(18) 0.0018(17) N3 0.056(2) 0.0289(18) 0.0262(17) 0.0030(14) -0.0023(16) -0.0028(17) N4 0.0391(19) 0.0351(18) 0.0265(16) 0.0007(14) -0.0012(15) -0.0023(16) N5 0.051(2) 0.0393(19) 0.0296(19) 0.0019(15) 0.0003(16) 0.0078(18) N6 0.054(2) 0.0337(19) 0.038(2) -0.0047(16) -0.0058(18) 0.0043(17) N7 0.058(2) 0.045(2) 0.038(2) 0.0043(17) -0.0043(19) 0.0102(19) N8 0.041(2) 0.038(2) 0.0263(18) 0.0024(15) -0.0020(15) -0.0021(16) N9 0.0373(18) 0.0288(16) 0.0320(18) 0.0021(14) 0.0034(15) 0.0022(15) N10 0.0354(18) 0.0321(18) 0.0399(19) 0.0046(16) 0.0016(16) 0.0028(15) N11 0.0380(18) 0.0308(17) 0.0368(18) 0.0018(15) -0.0006(16) 0.0026(16) C1A 0.047(3) 0.068(3) 0.052(3) 0.008(3) -0.014(2) -0.010(3) C2A 0.044(2) 0.045(2) 0.027(2) -0.0010(18) -0.0068(19) 0.008(2) C3A 0.045(3) 0.035(2) 0.037(2) -0.0035(19) -0.009(2) 0.007(2) C4A 0.054(3) 0.064(3) 0.046(3) -0.002(2) -0.011(2) 0.020(3) C5A 0.091(4) 0.053(3) 0.045(3) 0.000(2) -0.004(3) 0.018(3) C6A 0.078(4) 0.054(3) 0.070(3) -0.015(3) 0.001(3) 0.002(3) C7A 0.074(4) 0.085(4) 0.081(4) -0.027(4) 0.015(3) -0.013(4) C8A 0.081(4) 0.083(4) 0.064(4) -0.026(3) 0.006(3) -0.013(3) C9A 0.118(6) 0.125(6) 0.101(6) -0.054(5) 0.015(5) -0.012(5) C10A 0.077(4) 0.071(4) 0.071(4) -0.010(3) 0.002(3) 0.015(3) C1B 0.060(3) 0.028(2) 0.037(2) 0.0028(18) -0.009(2) -0.005(2) C2B 0.052(3) 0.035(2) 0.029(2) 0.0040(18) -0.002(2) 0.003(2) C3B 0.064(3) 0.045(3) 0.046(3) -0.007(2) -0.009(2) -0.004(2) C4B 0.072(4) 0.066(3) 0.048(3) -0.005(3) 0.005(3) -0.010(3) C5B 0.102(5) 0.117(6) 0.051(3) -0.015(4) 0.010(3) 0.002(4) C1C 0.074(3) 0.037(2) 0.047(3) 0.002(2) -0.012(3) 0.006(2) C2C 0.048(3) 0.034(2) 0.030(2) 0.0012(17) 0.0014(19) -0.0045(19) C3C 0.040(2) 0.033(2) 0.036(2) 0.0030(18) -0.002(2) -0.003(2) C1D 0.053(3) 0.047(3) 0.035(2) 0.003(2) -0.002(2) -0.009(2) C2D 0.035(2) 0.036(2) 0.031(2) 0.0029(17) -0.0013(18) 0.0015(19) C3D 0.046(2) 0.032(2) 0.031(2) -0.0036(17) -0.0001(19) -0.002(2) C4D 0.050(3) 0.040(2) 0.037(2) 0.0016(19) -0.001(2) 0.007(2) C5D 0.076(4) 0.047(3) 0.046(3) 0.001(2) -0.009(3) 0.022(3) C6D 0.068(4) 0.068(4) 0.086(4) 0.004(3) -0.028(3) 0.019(3) C7D 0.101(5) 0.044(3) 0.068(3) 0.007(3) -0.013(3) 0.022(3) C1E 0.065(3) 0.036(2) 0.035(2) 0.0021(19) -0.006(2) 0.009(2) C2E 0.063(3) 0.033(2) 0.038(2) -0.002(2) -0.013(2) 0.010(2) C3E 0.063(3) 0.052(3) 0.074(4) 0.003(3) -0.019(3) 0.009(3) C4E 0.079(4) 0.056(3) 0.130(6) -0.003(4) -0.033(4) -0.002(3) C5E 0.068(4) 0.069(4) 0.107(5) 0.011(4) -0.019(4) -0.002(3) C1F 0.070(3) 0.043(3) 0.034(2) 0.002(2) 0.002(2) 0.003(2) C2F 0.050(3) 0.032(2) 0.063(3) 0.003(2) -0.008(2) 0.001(2) C3F 0.052(3) 0.026(2) 0.045(3) 0.001(2) -0.007(2) -0.002(2) C4F 0.052(3) 0.039(3) 0.109(5) 0.003(3) 0.001(3) 0.001(2) C5F 0.058(4) 0.060(4) 0.139(6) 0.013(4) 0.009(4) 0.004(3) C6F 0.066(5) 0.138(8) 0.236(12) 0.058(8) 0.015(6) 0.021(5) C7F 0.097(5) 0.114(6) 0.122(6) -0.007(5) -0.041(5) 0.028(5) C1G 0.052(3) 0.036(2) 0.035(2) 0.0032(19) -0.003(2) 0.006(2) C2G 0.042(2) 0.033(2) 0.037(2) 0.0055(19) -0.0042(19) -0.0072(19) C3G 0.071(3) 0.053(3) 0.046(3) -0.010(2) 0.002(3) -0.009(3) C1H 0.041(2) 0.038(2) 0.029(2) -0.0017(18) 0.0069(18) -0.002(2) C2H 0.043(2) 0.0217(19) 0.033(2) 0.0002(16) 0.003(2) 0.0027(18) C3H 0.043(2) 0.049(3) 0.046(3) -0.005(2) -0.002(2) -0.001(2) C1I 0.043(2) 0.064(3) 0.033(2) 0.005(2) 0.002(2) -0.003(2) C2I 0.035(2) 0.031(2) 0.039(2) 0.0036(18) -0.0005(19) 0.0009(18) C3I 0.039(2) 0.038(2) 0.036(2) 0.0033(19) 0.004(2) 0.001(2) C4I 0.058(3) 0.039(2) 0.046(3) -0.002(2) -0.007(2) 0.004(2) C5I 0.078(3) 0.033(2) 0.055(3) -0.005(2) -0.025(3) 0.004(2) C6I 0.133(6) 0.085(5) 0.087(5) 0.041(4) -0.035(5) -0.030(5) C7I 0.182(8) 0.067(4) 0.093(5) -0.017(4) -0.033(5) 0.058(5) C1J 0.041(2) 0.037(2) 0.047(3) -0.0052(19) -0.003(2) 0.004(2) C2J 0.040(2) 0.037(2) 0.047(3) 0.010(2) 0.003(2) 0.005(2) C3J 0.036(2) 0.032(2) 0.042(2) 0.0054(19) -0.003(2) 0.0022(19) C4J 0.043(3) 0.041(3) 0.088(4) 0.022(3) 0.017(3) 0.003(2) C5J 0.063(4) 0.056(3) 0.153(7) 0.047(4) 0.057(4) 0.016(3) C6J 0.052(3) 0.081(4) 0.207(9) 0.072(5) 0.040(5) -0.001(3) C7J 0.176(9) 0.075(5) 0.169(9) 0.022(6) 0.121(8) 0.003(5) C1K 0.040(2) 0.043(2) 0.051(3) -0.004(2) 0.004(2) -0.004(2) C2K 0.033(2) 0.036(2) 0.039(2) -0.0005(18) 0.0040(18) -0.0013(19) C3K 0.035(2) 0.039(2) 0.042(2) -0.007(2) 0.010(2) -0.002(2) C4K 0.045(3) 0.040(2) 0.043(2) 0.005(2) 0.003(2) -0.004(2) C5K 0.058(3) 0.060(3) 0.049(3) 0.019(2) 0.001(2) 0.003(3) C6K 0.053(3) 0.067(3) 0.044(3) 0.003(2) 0.008(2) -0.010(3) O13 0.184(7) 0.128(5) 0.162(6) 0.049(5) 0.032(6) -0.019(5) C13 0.279(17) 0.108(7) 0.157(9) 0.009(7) 0.067(11) -0.045(9) OW1 0.068(2) 0.090(3) 0.0426(18) -0.0010(18) -0.0017(17) 0.024(2) OW2 0.098(3) 0.059(2) 0.0451(18) -0.0056(16) 0.003(2) 0.011(2) OW3 0.146(14) 0.131(13) 0.33(3) 0.095(17) 0.072(18) 0.031(12) _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 C3A 1.235(5) . ? O2 C2B 1.231(5) . ? O3 C3C 1.219(5) . ? O4 C3D 1.227(5) . ? O5 C2E 1.234(5) . ? O6 C3F 1.209(5) . ? O7 C2G 1.241(5) . ? O8 C2H 1.222(5) . ? O9 C3I 1.231(5) . ? O10 C3J 1.231(5) . ? O11 C3K 1.239(5) . ? O12 C4A 1.407(6) . ? N1 C3K 1.355(6) . ? N1 C1A 1.469(6) . ? N1 C2A 1.474(6) . ? N2 C3A 1.334(6) . ? N2 C1B 1.470(6) . ? N3 C2B 1.335(5) . ? N3 C2C 1.447(5) . ? N3 C1C 1.466(6) . ? N4 C3C 1.362(5) . ? N4 C1D 1.456(6) . ? N4 C2D 1.461(5) . ? N5 C3D 1.326(5) . ? N5 C1E 1.465(5) . ? N6 C2E 1.352(6) . ? N6 C1F 1.465(5) . ? N6 C2F 1.467(6) . ? N7 C3F 1.350(6) . ? N7 C1G 1.434(6) . ? N8 C2G 1.332(5) . ? N8 C1H 1.453(5) . ? N9 C2H 1.371(5) . ? N9 C1I 1.459(5) . ? N9 C2I 1.473(5) . ? N10 C3I 1.346(5) . ? N10 C1J 1.460(5) . ? N10 C2J 1.476(5) . ? N11 C3J 1.350(5) . ? N11 C1K 1.465(5) . ? N11 C2K 1.479(5) . ? C2A C3A 1.517(6) . ? C2A C4A 1.547(6) . ? C4A C5A 1.508(7) . ? C5A C10A 1.540(8) . ? C5A C6A 1.550(8) . ? C6A C7A 1.480(8) . ? C7A C8A 1.304(8) . ? C8A C9A 1.519(10) . ? C1B C3B 1.507(6) . ? C1B C2B 1.534(6) . ? C3B C4B 1.513(7) . ? C4B C5B 1.506(8) . ? C2C C3C 1.521(6) . ? C2D C3D 1.530(6) . ? C2D C4D 1.531(6) . ? C4D C5D 1.532(6) . ? C5D C6D 1.517(8) . ? C5D C7D 1.533(7) . ? C1E C2E 1.531(6) . ? C1E C3E 1.539(8) . ? C3E C5E 1.483(8) . ? C3E C4E 1.537(8) . ? C2F C4F 1.496(7) . ? C2F C3F 1.534(7) . ? C4F C5F 1.535(8) . ? C5F C6F 1.475(11) . ? C5F C7F 1.556(11) . ? C1G C2G 1.512(6) . ? C1G C3G 1.534(7) . ? C1H C3H 1.506(6) . ? C1H C2H 1.527(6) . ? C2I C4I 1.518(6) . ? C2I C3I 1.539(6) . ? C4I C5I 1.515(6) . ? C5I C6I 1.498(9) . ? C5I C7I 1.526(9) . ? C2J C3J 1.525(6) . ? C2J C4J 1.526(6) . ? C4J C5J 1.522(8) . ? C5J C6J 1.529(9) . ? C5J C7J 1.538(13) . ? C2K C3K 1.524(6) . ? C2K C4K 1.529(6) . ? C4K C5K 1.525(7) . ? C4K C6K 1.527(7) . ? O13 C13 1.456(14) . ? 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 C3K N1 C1A 115.4(4) . . ? C3K N1 C2A 123.6(3) . . ? C1A N1 C2A 117.3(4) . . ? C3A N2 C1B 122.3(4) . . ? C2B N3 C2C 116.7(3) . . ? C2B N3 C1C 123.9(4) . . ? C2C N3 C1C 115.1(3) . . ? C3C N4 C1D 122.0(3) . . ? C3C N4 C2D 118.1(3) . . ? C1D N4 C2D 119.3(3) . . ? C3D N5 C1E 122.5(3) . . ? C2E N6 C1F 124.5(4) . . ? C2E N6 C2F 117.9(4) . . ? C1F N6 C2F 116.3(4) . . ? C3F N7 C1G 122.9(4) . . ? C2G N8 C1H 123.1(3) . . ? C2H N9 C1I 123.3(3) . . ? C2H N9 C2I 118.8(3) . . ? C1I N9 C2I 117.8(3) . . ? C3I N10 C1J 124.4(3) . . ? C3I N10 C2J 120.0(4) . . ? C1J N10 C2J 115.4(3) . . ? C3J N11 C1K 124.7(4) . . ? C3J N11 C2K 118.4(3) . . ? C1K N11 C2K 116.8(3) . . ? N1 C2A C3A 111.1(3) . . ? N1 C2A C4A 107.9(4) . . ? C3A C2A C4A 113.3(4) . . ? O1 C3A N2 122.6(4) . . ? O1 C3A C2A 121.4(4) . . ? N2 C3A C2A 115.9(4) . . ? O12 C4A C5A 109.4(4) . . ? O12 C4A C2A 107.4(4) . . ? C5A C4A C2A 114.5(5) . . ? C4A C5A C10A 107.2(5) . . ? C4A C5A C6A 110.9(4) . . ? C10A C5A C6A 111.5(4) . . ? C7A C6A C5A 113.8(5) . . ? C8A C7A C6A 125.0(7) . . ? C7A C8A C9A 123.9(7) . . ? N2 C1B C3B 112.5(3) . . ? N2 C1B C2B 105.9(3) . . ? C3B C1B C2B 111.6(4) . . ? O2 C2B N3 122.0(4) . . ? O2 C2B C1B 117.9(4) . . ? N3 C2B C1B 120.2(4) . . ? C1B C3B C4B 114.4(4) . . ? C5B C4B C3B 113.3(5) . . ? N3 C2C C3C 109.5(3) . . ? O3 C3C N4 122.8(4) . . ? O3 C3C C2C 119.8(4) . . ? N4 C3C C2C 117.4(4) . . ? N4 C2D C3D 113.6(3) . . ? N4 C2D C4D 112.3(3) . . ? C3D C2D C4D 109.9(3) . . ? O4 C3D N5 123.4(4) . . ? O4 C3D C2D 118.4(4) . . ? N5 C3D C2D 118.2(3) . . ? C2D C4D C5D 114.5(4) . . ? C6D C5D C4D 111.9(4) . . ? C6D C5D C7D 111.1(5) . . ? C4D C5D C7D 108.9(4) . . ? N5 C1E C2E 107.3(4) . . ? N5 C1E C3E 111.7(4) . . ? C2E C1E C3E 111.1(4) . . ? O5 C2E N6 122.1(4) . . ? O5 C2E C1E 118.5(4) . . ? N6 C2E C1E 119.4(4) . . ? C5E C3E C4E 108.5(5) . . ? C5E C3E C1E 115.3(5) . . ? C4E C3E C1E 109.5(5) . . ? N6 C2F C4F 112.6(4) . . ? N6 C2F C3F 108.1(4) . . ? C4F C2F C3F 113.0(4) . . ? O6 C3F N7 123.2(4) . . ? O6 C3F C2F 123.5(4) . . ? N7 C3F C2F 113.2(4) . . ? C2F C4F C5F 114.8(5) . . ? C6F C5F C4F 110.1(5) . . ? C6F C5F C7F 112.5(7) . . ? C4F C5F C7F 112.8(6) . . ? N7 C1G C2G 107.8(4) . . ? N7 C1G C3G 112.9(4) . . ? C2G C1G C3G 110.9(4) . . ? O7 C2G N8 122.1(4) . . ? O7 C2G C1G 121.8(4) . . ? N8 C2G C1G 116.1(4) . . ? N8 C1H C3H 110.3(3) . . ? N8 C1H C2H 107.4(3) . . ? C3H C1H C2H 110.2(3) . . ? O8 C2H N9 122.1(4) . . ? O8 C2H C1H 119.3(3) . . ? N9 C2H C1H 118.6(3) . . ? N9 C2I C4I 110.6(3) . . ? N9 C2I C3I 109.5(3) . . ? C4I C2I C3I 112.5(3) . . ? O9 C3I N10 121.9(4) . . ? O9 C3I C2I 119.4(4) . . ? N10 C3I C2I 118.6(4) . . ? C5I C4I C2I 113.8(4) . . ? C6I C5I C4I 110.0(5) . . ? C6I C5I C7I 111.2(6) . . ? C4I C5I C7I 111.7(5) . . ? N10 C2J C3J 110.0(3) . . ? N10 C2J C4J 112.1(4) . . ? C3J C2J C4J 110.5(4) . . ? O10 C3J N11 121.6(4) . . ? O10 C3J C2J 120.0(4) . . ? N11 C3J C2J 118.4(4) . . ? C5J C4J C2J 115.5(4) . . ? C4J C5J C6J 108.5(6) . . ? C4J C5J C7J 111.1(6) . . ? C6J C5J C7J 112.2(6) . . ? N11 C2K C3K 107.7(3) . . ? N11 C2K C4K 113.2(3) . . ? C3K C2K C4K 111.7(3) . . ? O11 C3K N1 119.1(4) . . ? O11 C3K C2K 119.6(4) . . ? N1 C3K C2K 121.0(4) . . ? C5K C4K C6K 110.3(4) . . ? C5K C4K C2K 110.8(4) . . ? C6K C4K C2K 108.3(4) . . ? 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 C3K N1 C2A C3A -137.1(4) . . . . ? C1A N1 C2A C3A 65.6(5) . . . . ? C3K N1 C2A C4A 98.1(4) . . . . ? C1A N1 C2A C4A -59.1(5) . . . . ? C1B N2 C3A O1 -2.3(6) . . . . ? C1B N2 C3A C2A 174.2(3) . . . . ? N1 C2A C3A O1 -72.1(5) . . . . ? C4A C2A C3A O1 49.5(5) . . . . ? N1 C2A C3A N2 111.5(4) . . . . ? C4A C2A C3A N2 -126.9(4) . . . . ? N1 C2A C4A O12 -58.4(4) . . . . ? C3A C2A C4A O12 178.2(4) . . . . ? N1 C2A C4A C5A 179.9(4) . . . . ? C3A C2A C4A C5A 56.5(5) . . . . ? O12 C4A C5A C10A 66.0(5) . . . . ? C2A C4A C5A C10A -173.4(4) . . . . ? O12 C4A C5A C6A -55.9(6) . . . . ? C2A C4A C5A C6A 64.7(5) . . . . ? C4A C5A C6A C7A 169.1(5) . . . . ? C10A C5A C6A C7A 49.7(7) . . . . ? C5A C6A C7A C8A -122.1(7) . . . . ? C6A C7A C8A C9A -177.7(7) . . . . ? C3A N2 C1B C3B 90.9(5) . . . . ? C3A N2 C1B C2B -146.8(4) . . . . ? C2C N3 C2B O2 14.9(6) . . . . ? C1C N3 C2B O2 170.6(4) . . . . ? C2C N3 C2B C1B -164.6(4) . . . . ? C1C N3 C2B C1B -8.9(6) . . . . ? N2 C1B C2B O2 -52.0(5) . . . . ? C3B C1B C2B O2 70.7(5) . . . . ? N2 C1B C2B N3 127.5(4) . . . . ? C3B C1B C2B N3 -109.7(5) . . . . ? N2 C1B C3B C4B 178.8(4) . . . . ? C2B C1B C3B C4B 59.9(5) . . . . ? C1B C3B C4B C5B 174.1(5) . . . . ? C2B N3 C2C C3C 76.1(5) . . . . ? C1C N3 C2C C3C -81.7(4) . . . . ? C1D N4 C3C O3 179.5(4) . . . . ? C2D N4 C3C O3 7.8(6) . . . . ? C1D N4 C3C C2C 0.4(5) . . . . ? C2D N4 C3C C2C -171.4(3) . . . . ? N3 C2C C3C O3 -1.1(5) . . . . ? N3 C2C C3C N4 178.0(3) . . . . ? C3C N4 C2D C3D -117.9(4) . . . . ? C1D N4 C2D C3D 70.2(5) . . . . ? C3C N4 C2D C4D 116.6(4) . . . . ? C1D N4 C2D C4D -55.4(5) . . . . ? C1E N5 C3D O4 3.9(6) . . . . ? C1E N5 C3D C2D -176.9(4) . . . . ? N4 C2D C3D O4 -169.5(4) . . . . ? C4D C2D C3D O4 -42.8(5) . . . . ? N4 C2D C3D N5 11.2(5) . . . . ? C4D C2D C3D N5 138.0(4) . . . . ? N4 C2D C4D C5D -53.3(5) . . . . ? C3D C2D C4D C5D 179.3(4) . . . . ? C2D C4D C5D C6D -62.8(6) . . . . ? C2D C4D C5D C7D 174.0(5) . . . . ? C3D N5 C1E C2E -119.6(4) . . . . ? C3D N5 C1E C3E 118.3(5) . . . . ? C1F N6 C2E O5 -161.0(5) . . . . ? C2F N6 C2E O5 5.4(7) . . . . ? C1F N6 C2E C1E 19.5(7) . . . . ? C2F N6 C2E C1E -174.0(4) . . . . ? N5 C1E C2E O5 -51.3(6) . . . . ? C3E C1E C2E O5 71.1(6) . . . . ? N5 C1E C2E N6 128.2(4) . . . . ? C3E C1E C2E N6 -109.4(5) . . . . ? N5 C1E C3E C5E 171.6(5) . . . . ? C2E C1E C3E C5E 51.8(6) . . . . ? N5 C1E C3E C4E -65.7(6) . . . . ? C2E C1E C3E C4E 174.5(5) . . . . ? C2E N6 C2F C4F 138.2(5) . . . . ? C1F N6 C2F C4F -54.2(5) . . . . ? C2E N6 C2F C3F -96.3(5) . . . . ? C1F N6 C2F C3F 71.3(5) . . . . ? C1G N7 C3F O6 1.6(7) . . . . ? C1G N7 C3F C2F -177.5(4) . . . . ? N6 C2F C3F O6 -98.1(5) . . . . ? C4F C2F C3F O6 27.2(7) . . . . ? N6 C2F C3F N7 81.0(5) . . . . ? C4F C2F C3F N7 -153.7(4) . . . . ? N6 C2F C4F C5F -55.6(7) . . . . ? C3F C2F C4F C5F -178.5(5) . . . . ? C2F C4F C5F C6F -175.8(7) . . . . ? C2F C4F C5F C7F -49.1(8) . . . . ? C3F N7 C1G C2G -136.2(4) . . . . ? C3F N7 C1G C3G 101.0(5) . . . . ? C1H N8 C2G O7 3.7(6) . . . . ? C1H N8 C2G C1G -177.2(4) . . . . ? N7 C1G C2G O7 -53.1(5) . . . . ? C3G C1G C2G O7 70.9(5) . . . . ? N7 C1G C2G N8 127.8(4) . . . . ? C3G C1G C2G N8 -108.2(4) . . . . ? C2G N8 C1H C3H -157.7(4) . . . . ? C2G N8 C1H C2H 82.1(5) . . . . ? C1I N9 C2H O8 178.7(4) . . . . ? C2I N9 C2H O8 1.5(5) . . . . ? C1I N9 C2H C1H -1.1(5) . . . . ? C2I N9 C2H C1H -178.2(3) . . . . ? N8 C1H C2H O8 48.3(5) . . . . ? C3H C1H C2H O8 -71.9(4) . . . . ? N8 C1H C2H N9 -131.9(3) . . . . ? C3H C1H C2H N9 107.9(4) . . . . ? C2H N9 C2I C4I 109.7(4) . . . . ? C1I N9 C2I C4I -67.6(5) . . . . ? C2H N9 C2I C3I -125.8(4) . . . . ? C1I N9 C2I C3I 56.9(4) . . . . ? C1J N10 C3I O9 177.4(4) . . . . ? C2J N10 C3I O9 1.3(6) . . . . ? C1J N10 C3I C2I -5.6(6) . . . . ? C2J N10 C3I C2I 178.3(3) . . . . ? N9 C2I C3I O9 -119.4(4) . . . . ? C4I C2I C3I O9 4.0(6) . . . . ? N9 C2I C3I N10 63.5(5) . . . . ? C4I C2I C3I N10 -173.0(4) . . . . ? N9 C2I C4I C5I -66.6(5) . . . . ? C3I C2I C4I C5I 170.6(4) . . . . ? C2I C4I C5I C6I -85.0(6) . . . . ? C2I C4I C5I C7I 151.0(6) . . . . ? C3I N10 C2J C3J -124.2(4) . . . . ? C1J N10 C2J C3J 59.4(5) . . . . ? C3I N10 C2J C4J 112.5(4) . . . . ? C1J N10 C2J C4J -64.0(5) . . . . ? C1K N11 C3J O10 -175.6(4) . . . . ? C2K N11 C3J O10 7.7(6) . . . . ? C1K N11 C3J C2J 5.0(6) . . . . ? C2K N11 C3J C2J -171.6(3) . . . . ? N10 C2J C3J O10 -118.6(4) . . . . ? C4J C2J C3J O10 5.7(6) . . . . ? N10 C2J C3J N11 60.8(5) . . . . ? C4J C2J C3J N11 -174.9(4) . . . . ? N10 C2J C4J C5J -63.3(6) . . . . ? C3J C2J C4J C5J 173.6(5) . . . . ? C2J C4J C5J C6J 175.5(6) . . . . ? C2J C4J C5J C7J -60.7(7) . . . . ? C3J N11 C2K C3K -115.8(4) . . . . ? C1K N11 C2K C3K 67.3(4) . . . . ? C3J N11 C2K C4K 120.2(4) . . . . ? C1K N11 C2K C4K -56.7(5) . . . . ? C1A N1 C3K O11 -3.0(6) . . . . ? C2A N1 C3K O11 -160.7(4) . . . . ? C1A N1 C3K C2K -176.7(4) . . . . ? C2A N1 C3K C2K 25.6(6) . . . . ? N11 C2K C3K O11 -89.7(4) . . . . ? C4K C2K C3K O11 35.2(5) . . . . ? N11 C2K C3K N1 83.9(4) . . . . ? C4K C2K C3K N1 -151.2(4) . . . . ? N11 C2K C4K C5K -48.8(5) . . . . ? C3K C2K C4K C5K -170.7(4) . . . . ? N11 C2K C4K C6K -170.0(4) . . . . ? C3K C2K C4K C6K 68.2(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O12 H12 O7 0.84 2.13 2.847(5) 142.9 1_655 O12 H12 OW3 0.84 2.20 2.87(2) 135.7 1_655 N2 H2 O10 0.88 2.16 2.991(4) 157.4 . N5 H5 OW1 0.88 2.31 3.147(5) 158.8 . N7 H7 O5 0.88 2.42 3.092(5) 134.0 . N8 H8 O4 0.88 1.92 2.795(4) 172.8 3_756 O13 H13 OW2 0.853(8) 1.966(4) 2.819(9) 179.0(6) . OW1 HW12 O5 0.976(4) 1.960(3) 2.782(5) 140.3(2) . OW1 HW11 O2 1.172(4) 1.717(3) 2.888(5) 176.9(2) . OW2 HW22 O11 1.038(4) 1.832(3) 2.795(5) 152.7(2) 4_457 OW2 HW21 O9 1.109(3) 1.668(3) 2.762(4) 167.9(2) . OW3 HW31 OW1 0.807(18) 2.224(4) 3.024(18) 171.1(19) . OW3 HW32 O7 0.844(17) 1.987(3) 2.823(17) 170.2(18) . OW3 HW33 O12 0.88(2) 1.989(4) 2.87(2) 171.6(19) 1_455 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.10 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.403 _refine_diff_density_min -0.196 _refine_diff_density_rms 0.050 data_CsH_I _database_code_CSD 195322 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cyclosporin H crystal form I ex MeOH RT ; _chemical_name_common 'cyclosporin H' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C62 H111 O12 N11. 6H2O' _chemical_compound_source Sandoz-Novartis _chemical_formula_sum 'C62 H123 O18 N11' _chemical_formula_weight 1309 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' O O 0.0492 0.0322 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 17.2986(8) _cell_length_b 19.690(1) _cell_length_c 24.137(4) _cell_angle_alpha 90.000(0) _cell_angle_beta 90.000(0) _cell_angle_gamma 90.000(0) _cell_volume 8221.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 25 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2864 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type 'empirical via \psi scans' _exptl_absorpt_process_details '(North, Philips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.778 _exptl_absorpt_correction_T_max 0.974 _exptl_special_details ; Room temperature capillary mounted ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method \w-/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 97 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18188 _diffrn_reflns_av_R_equivalents 0.2187 _diffrn_reflns_av_sigmaI/netI 0.1343 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 69.99 _reflns_number_total 9833 _reflns_number_gt 5049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4-PC Software (Enraf-Nonius, 1992)' _computing_cell_refinement 'SET4 and CELDIM in CAD-4-PC Software (Enraf-Nonius, 1992)' _computing_data_reduction ; CCP4: CAD77, CADRAL, CADSHEL The HKL Manual, 4th edition in Sawyer et al., 1993: Data Collection and Processing: Proceedings of the CCP4 Study Weekend 29-30 January 1993 (Eds. L.Sawyer, N.Isaacs and S.Bailey) SERC Daresbury Laboratory* DL/SC1/R34. ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1998)' _computing_publication_material SHELX97 _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^)+(0.1420P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00167(19) _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 0.1(5) _refine_ls_number_reflns 7278 _refine_ls_number_parameters 993 _refine_ls_number_restraints 1292 _refine_ls_R_factor_all 0.1343 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.2418 _refine_ls_wR_factor_gt 0.2212 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.6223(4) 0.6468(4) 0.6229(3) 0.0730(14) Uani 1 1 d U . . N2 N 0.7910(4) 0.5473(3) 0.5838(3) 0.0674(14) Uani 1 1 d U . . H2 H 0.7855 0.5443 0.5485 0.25(10) Uiso 1 1 calc R . . N3 N 0.9739(4) 0.5618(3) 0.6613(3) 0.0601(13) Uani 1 1 d U . . N4 N 1.0771(3) 0.6968(3) 0.7383(3) 0.0598(13) Uani 1 1 d U . . N5 N 0.9565(3) 0.8187(3) 0.7532(2) 0.0518(12) Uani 1 1 d U . . H5 H 0.9274 0.7916 0.7717 0.06(2) Uiso 1 1 calc R . . N6 N 0.8230(4) 0.9588(3) 0.7325(2) 0.0572(12) Uani 1 1 d U . . N7 N 0.6953(4) 0.9511(3) 0.8469(3) 0.0591(13) Uani 1 1 d U . . H7 H 0.6593 0.9298 0.8296 0.11(4) Uiso 1 1 calc R . . N8 N 0.7913(3) 0.8626(3) 0.9025(2) 0.0511(12) Uani 1 1 d U . . H8 H 0.7774 0.8581 0.8685 0.05(2) Uiso 1 1 calc R . . N9 N 0.7979(3) 0.7080(3) 0.9145(2) 0.0528(11) Uani 1 1 d U . . N10 N 0.6674(4) 0.6729(3) 0.8387(3) 0.0624(13) Uani 1 1 d U . . N11 N 0.5482(4) 0.6318(3) 0.7423(3) 0.0701(14) Uani 1 1 d U . . O1 O 0.7373(4) 0.5751(4) 0.6638(3) 0.092(2) Uani 1 1 d U . . O2 O 0.9136(4) 0.6311(3) 0.6012(3) 0.0792(16) Uani 1 1 d U . . O3 O 0.9589(3) 0.6490(3) 0.7489(2) 0.0650(13) Uani 1 1 d U . . O4 O 1.0782(3) 0.8529(3) 0.7380(3) 0.0890(19) Uani 1 1 d U . . O5 O 0.8171(3) 0.8646(2) 0.78433(19) 0.0555(12) Uani 1 1 d U . . O6 O 0.8041(3) 1.0121(3) 0.8403(2) 0.0709(14) Uani 1 1 d U . . O7 O 0.7625(4) 0.9096(3) 0.9846(2) 0.0832(18) Uani 1 1 d U . . O8 O 0.8928(3) 0.7383(3) 0.8558(2) 0.0622(13) Uani 1 1 d U . . O9 O 0.6654(4) 0.5858(3) 0.8979(3) 0.0837(17) Uani 1 1 d U . . O10 O 0.5317(3) 0.7426(3) 0.7640(3) 0.0795(16) Uani 1 1 d U . . O11 O 0.5468(5) 0.5546(3) 0.6224(3) 0.100(2) Uani 1 1 d U . . C1A C 0.6519(5) 0.7065(5) 0.6525(4) 0.087(3) Uani 1 1 d U . . H1A1 H 0.6897 0.6923 0.6793 0.23(5) Uiso 1 1 calc R . . H1A2 H 0.6101 0.7290 0.6711 0.23(5) Uiso 1 1 calc R . . H1A3 H 0.6754 0.7371 0.6266 0.23(5) Uiso 1 1 calc R . . C3A C 0.7374(5) 0.5766(4) 0.6135(4) 0.0682(15) Uani 1 1 d U . . C1B C 0.8603(5) 0.5195(4) 0.6102(4) 0.0648(15) Uani 1 1 d U . . H1B H 0.8455 0.4952 0.6440 0.06(2) Uiso 1 1 calc R . . C2B C 0.9176(5) 0.5760(4) 0.6249(3) 0.0613(14) Uani 1 1 d U . . C3B C 0.9004(5) 0.4692(4) 0.5698(4) 0.079(2) Uani 1 1 d DU . . C4B C 0.8498(6) 0.4082(4) 0.5570(5) 0.102(3) Uani 1 1 d DU . . H4B1 H 0.8764 0.3785 0.5319 0.153 Uiso 1 1 calc R . . H4B2 H 0.8023 0.4232 0.5404 0.153 Uiso 1 1 calc R . . H4B3 H 0.8386 0.3842 0.5907 0.153 Uiso 1 1 calc R . . C1C C 0.9799(5) 0.4993(4) 0.6944(4) 0.071(2) Uani 1 1 d U . . H1C1 H 1.0246 0.4740 0.6828 0.12(2) Uiso 1 1 calc R . . H1C2 H 0.9344 0.4723 0.6890 0.12(2) Uiso 1 1 calc R . . H1C3 H 0.9848 0.5109 0.7328 0.12(2) Uiso 1 1 calc R . . C2C C 1.0336(4) 0.6104(4) 0.6711(3) 0.0595(15) Uani 1 1 d U . . H2C1 H 1.0379 0.6402 0.6392 0.055(14) Uiso 1 1 calc R . . H2C2 H 1.0825 0.5869 0.6753 0.055(14) Uiso 1 1 calc R . . C3C C 1.0181(4) 0.6534(4) 0.7232(3) 0.0557(14) Uani 1 1 d U . . C1D C 1.1447(5) 0.7077(5) 0.7027(4) 0.080(2) Uani 1 1 d U . . H1D1 H 1.1505 0.7554 0.6955 0.19(4) Uiso 1 1 calc R . . H1D2 H 1.1377 0.6839 0.6684 0.19(4) Uiso 1 1 calc R . . H1D3 H 1.1902 0.6910 0.7211 0.19(4) Uiso 1 1 calc R . . C2D C 1.0608(4) 0.7456(4) 0.7835(3) 0.0566(13) Uani 1 1 d U . . H2D H 1.0190 0.7271 0.8064 0.17(6) Uiso 1 1 calc R . . C3D C 1.0324(4) 0.8114(4) 0.7570(3) 0.0586(13) Uani 1 1 d U . . C4D C 1.1320(5) 0.7587(5) 0.8213(4) 0.0723(17) Uani 1 1 d U . . H4D1 H 1.1751 0.7726 0.7982 0.12(3) Uiso 1 1 calc R . . H4D2 H 1.1201 0.7961 0.8460 0.12(3) Uiso 1 1 calc R . . C5D C 1.1566(6) 0.6985(5) 0.8554(4) 0.092(2) Uani 1 1 d DU . . C6D C 1.2380(7) 0.7065(7) 0.8767(6) 0.117(4) Uani 1 1 d U . . H6D1 H 1.2522 0.6669 0.8976 0.102(19) Uiso 1 1 calc R . . H6D2 H 1.2409 0.7459 0.9001 0.102(19) Uiso 1 1 calc R . . H6D3 H 1.2727 0.7119 0.8460 0.102(19) Uiso 1 1 calc R . . C1E C 0.9208(4) 0.8703(4) 0.7194(3) 0.0531(12) Uani 1 1 d U . . H1E H 0.9579 0.9071 0.7132 0.043(17) Uiso 1 1 calc R . . C2E C 0.8512(4) 0.8983(3) 0.7493(3) 0.0502(12) Uani 1 1 d U . . C3E C 0.8949(5) 0.8414(5) 0.6631(3) 0.0690(17) Uani 1 1 d U . . H3E H 0.8699 0.8786 0.6428 0.08(3) Uiso 1 1 calc R . . C4E C 0.9623(7) 0.8174(6) 0.6280(4) 0.094(3) Uani 1 1 d U . . H4E1 H 0.9893 0.8560 0.6133 0.087(17) Uiso 1 1 calc R . . H4E2 H 0.9434 0.7900 0.5981 0.087(17) Uiso 1 1 calc R . . H4E3 H 0.9969 0.7911 0.6505 0.087(17) Uiso 1 1 calc R . . C5E C 0.8368(6) 0.7862(6) 0.6689(4) 0.094(3) Uani 1 1 d U . . H5E1 H 0.8170 0.7744 0.6331 0.13(2) Uiso 1 1 calc R . . H5E2 H 0.7952 0.8015 0.6921 0.13(2) Uiso 1 1 calc R . . H5E3 H 0.8607 0.7472 0.6854 0.13(2) Uiso 1 1 calc R . . C1F C 0.8645(5) 1.0076(4) 0.6967(3) 0.069(2) Uani 1 1 d U . . H1F1 H 0.8478 1.0020 0.6590 0.12(2) Uiso 1 1 calc R . . H1F2 H 0.9191 0.9993 0.6990 0.12(2) Uiso 1 1 calc R . . H1F3 H 0.8536 1.0530 0.7087 0.12(2) Uiso 1 1 calc R . . C2F C 0.7473(5) 0.9803(4) 0.7535(3) 0.0619(13) Uani 1 1 d U . . H2F H 0.7406 1.0275 0.7416 0.07(2) Uiso 1 1 calc R . . C3F C 0.7513(5) 0.9821(4) 0.8178(3) 0.0568(13) Uani 1 1 d U . . C4F C 0.6816(5) 0.9411(5) 0.7281(3) 0.0731(17) Uani 1 1 d U . . H4F1 H 0.6336 0.9568 0.7446 0.10(2) Uiso 1 1 calc R . . H4F2 H 0.6876 0.8936 0.7377 0.10(2) Uiso 1 1 calc R . . C5F C 0.6745(7) 0.9468(5) 0.6650(4) 0.090(2) Uani 1 1 d U . . H5F H 0.7237 0.9315 0.6493 0.14(5) Uiso 1 1 calc R . . C6F C 0.6614(8) 1.0197(6) 0.6447(4) 0.107(3) Uani 1 1 d U . . H6F1 H 0.6967 1.0497 0.6632 0.160 Uiso 1 1 calc R . . H6F2 H 0.6093 1.0332 0.6527 0.160 Uiso 1 1 calc R . . H6F3 H 0.6701 1.0219 0.6055 0.160 Uiso 1 1 calc R . . C7F C 0.6117(9) 0.8976(7) 0.6443(6) 0.131(4) Uani 1 1 d U . . H7F1 H 0.5643 0.9062 0.6638 0.196 Uiso 1 1 calc R . . H7F2 H 0.6279 0.8517 0.6509 0.196 Uiso 1 1 calc R . . H7F3 H 0.6038 0.9043 0.6054 0.196 Uiso 1 1 calc R . . C1G C 0.6946(5) 0.9528(4) 0.9057(3) 0.0643(14) Uani 1 1 d U . . H1G H 0.7068 0.9994 0.9168 0.08(3) Uiso 1 1 calc R . . C2G C 0.7529(5) 0.9067(4) 0.9339(3) 0.0596(14) Uani 1 1 d U . . C3G C 0.6127(5) 0.9372(6) 0.9271(4) 0.087(3) Uani 1 1 d U . . H3G1 H 0.6133 0.9356 0.9668 0.086(16) Uiso 1 1 calc R . . H3G2 H 0.5959 0.8941 0.9128 0.086(16) Uiso 1 1 calc R . . H3G3 H 0.5779 0.9721 0.9150 0.086(16) Uiso 1 1 calc R . . C1H C 0.8558(4) 0.8214(4) 0.9224(3) 0.0504(12) Uani 1 1 d U . . H1H H 0.8502 0.8154 0.9625 0.033(15) Uiso 1 1 calc R . . C2H C 0.8514(4) 0.7518(4) 0.8950(3) 0.0499(12) Uani 1 1 d U . . C3H C 0.9327(4) 0.8554(4) 0.9113(4) 0.066(2) Uani 1 1 d U . . H3H1 H 0.9737 0.8268 0.9245 0.058(12) Uiso 1 1 calc R . . H3H2 H 0.9345 0.8982 0.9302 0.058(12) Uiso 1 1 calc R . . H3H3 H 0.9386 0.8626 0.8722 0.058(12) Uiso 1 1 calc R . . C1I C 0.7499(5) 0.7209(4) 0.9631(3) 0.069(2) Uani 1 1 d U . . H1I1 H 0.7231 0.7632 0.9584 0.102(19) Uiso 1 1 calc R . . H1I2 H 0.7820 0.7233 0.9954 0.102(19) Uiso 1 1 calc R . . H1I3 H 0.7131 0.6848 0.9673 0.102(19) Uiso 1 1 calc R . . C2I C 0.7872(4) 0.6412(4) 0.8870(3) 0.0577(13) Uani 1 1 d U . . H2I H 0.8153 0.6420 0.8518 0.07(2) Uiso 1 1 calc R . . C3I C 0.7016(5) 0.6303(4) 0.8743(3) 0.0622(14) Uani 1 1 d U . . C4I C 0.8206(5) 0.5821(4) 0.9229(4) 0.0695(17) Uani 1 1 d U . . H4I1 H 0.7956 0.5833 0.9588 0.078(18) Uiso 1 1 calc R . . H4I2 H 0.8066 0.5394 0.9054 0.078(18) Uiso 1 1 calc R . . C5I C 0.9072(6) 0.5824(5) 0.9319(4) 0.0803(19) Uani 1 1 d U . . H5I H 0.9233 0.6288 0.9409 0.07(2) Uiso 1 1 calc R . . C6I C 0.9237(8) 0.5360(7) 0.9830(6) 0.120(4) Uani 1 1 d U . . C7I C 0.9492(7) 0.5605(7) 0.8820(5) 0.106(3) Uani 1 1 d U . . H7I1 H 1.0021 0.5749 0.8845 0.16(3) Uiso 1 1 calc R . . H7I2 H 0.9257 0.5804 0.8498 0.16(3) Uiso 1 1 calc R . . H7I3 H 0.9472 0.5119 0.8791 0.16(3) Uiso 1 1 calc R . . C1J C 0.7064(5) 0.7290(4) 0.8093(3) 0.067(2) Uani 1 1 d U . . H1J1 H 0.7002 0.7231 0.7700 0.090(17) Uiso 1 1 calc R . . H1J2 H 0.7604 0.7290 0.8184 0.090(17) Uiso 1 1 calc R . . H1J3 H 0.6838 0.7715 0.8203 0.090(17) Uiso 1 1 calc R . . C2J C 0.5825(5) 0.6721(5) 0.8359(4) 0.0717(15) Uani 1 1 d U . . H2J H 0.5657 0.6265 0.8467 0.12(4) Uiso 1 1 calc R . . C3J C 0.5531(4) 0.6845(4) 0.7781(4) 0.0688(15) Uani 1 1 d U . . C4J C 0.5514(5) 0.7217(6) 0.8802(5) 0.097(2) Uani 1 1 d DU . . H4J1 H 0.5827 0.7167 0.9133 0.14(3) Uiso 1 1 calc R . . H4J2 H 0.5588 0.7677 0.8667 0.14(3) Uiso 1 1 calc R . . C5J C 0.4673(5) 0.7135(7) 0.8964(6) 0.118(3) Uani 1 1 d DU . . H5J H 0.4325 0.7168 0.8645 0.177 Uiso 1 1 calc R . . C6J C 0.4515(9) 0.7701(8) 0.9406(6) 0.150(5) Uani 1 1 d U . . H6J1 H 0.4549 0.8139 0.9234 0.14(3) Uiso 1 1 calc R . . H6J2 H 0.4892 0.7670 0.9697 0.14(3) Uiso 1 1 calc R . . H6J3 H 0.4007 0.7641 0.9559 0.14(3) Uiso 1 1 calc R . . C7J C 0.4587(8) 0.6455(7) 0.9274(6) 0.129(4) Uani 1 1 d U . . H7J1 H 0.4049 0.6338 0.9300 0.19(4) Uiso 1 1 calc R . . H7J2 H 0.4801 0.6497 0.9639 0.19(4) Uiso 1 1 calc R . . H7J3 H 0.4857 0.6106 0.9075 0.19(4) Uiso 1 1 calc R . . C1K C 0.5729(6) 0.5631(4) 0.7561(5) 0.090(3) Uani 1 1 d U . . H1K1 H 0.5290 0.5333 0.7558 0.13(2) Uiso 1 1 calc R . . H1K2 H 0.5960 0.5629 0.7923 0.13(2) Uiso 1 1 calc R . . H1K3 H 0.6100 0.5478 0.7293 0.13(2) Uiso 1 1 calc R . . C2K C 0.5112(5) 0.6426(4) 0.6867(4) 0.0727(15) Uani 1 1 d U . . H2K H 0.5093 0.6917 0.6800 0.10(3) Uiso 1 1 calc R . . C3K C 0.5625(5) 0.6115(5) 0.6419(4) 0.0756(16) Uani 1 1 d U . . C4K C 0.4272(5) 0.6159(5) 0.6852(5) 0.089(2) Uani 1 1 d U . . H4K H 0.4287 0.5663 0.6884 0.133 Uiso 1 1 calc R . . C5K C 0.3926(6) 0.6339(7) 0.6293(6) 0.112(3) Uani 1 1 d U . . H5K1 H 0.3919 0.6823 0.6250 0.168 Uiso 1 1 calc R . . H5K2 H 0.3407 0.6167 0.6272 0.168 Uiso 1 1 calc R . . H5K3 H 0.4232 0.6139 0.6004 0.168 Uiso 1 1 calc R . . C6K C 0.3810(6) 0.6435(6) 0.7330(6) 0.106(3) Uani 1 1 d U . . H6K1 H 0.3290 0.6266 0.7309 0.160 Uiso 1 1 calc R . . H6K2 H 0.3804 0.6922 0.7313 0.160 Uiso 1 1 calc R . . H6K3 H 0.4041 0.6292 0.7672 0.160 Uiso 1 1 calc R . . OW1 O 0.8192(4) 0.5769(4) 0.7622(3) 0.093(2) Uani 1 1 d U . . OW2 O 0.4542(6) 0.3812(5) 0.6961(4) 0.131(3) Uani 1 1 d U . . OW3 O 0.6863(6) 0.4605(4) 0.9619(3) 0.120(3) Uani 1 1 d U . . OW4 O 1.1999(10) 0.9396(8) 0.7045(7) 0.230(6) Uani 1 1 d U . . OW5 O 0.4099(9) 0.9201(7) 0.8560(6) 0.197(5) Uani 1 1 d U . . OW8 O 0.6782(8) 1.0026(7) 1.0587(5) 0.191(5) Uani 1 1 d U . . O121 O 0.7641(9) 0.6980(9) 0.5571(9) 0.079(2) Uani 0.582(9) 1 d PDU . . C2A1 C 0.6707(12) 0.6108(10) 0.5862(8) 0.0693(16) Uani 0.582(9) 1 d PDU . . C4A1 C 0.7006(7) 0.6581(7) 0.5393(7) 0.0775(18) Uani 0.582(9) 1 d PDU . . C5A1 C 0.6365(7) 0.7044(5) 0.5183(5) 0.0844(19) Uani 0.582(9) 1 d PDU . . C6A1 C 0.6639(8) 0.7493(5) 0.4709(5) 0.092(2) Uani 0.582(9) 1 d PDU . . C7A1 C 0.6171(8) 0.8144(5) 0.4664(7) 0.093(2) Uani 0.582(9) 1 d PDU . . C8A1 C 0.6485(11) 0.8765(6) 0.4698(9) 0.095(3) Uani 0.582(9) 1 d PDU . . C9A1 C 0.6074(13) 0.9422(9) 0.4604(10) 0.094(3) Uani 0.582(9) 1 d PDU . . C10A C 0.5627(7) 0.6661(8) 0.5044(7) 0.088(3) Uani 0.582(9) 1 d PDU . . C7D1 C 1.0964(17) 0.660(2) 0.8891(17) 0.098(3) Uani 0.29(2) 1 d PDU . . O122 O 0.7799(13) 0.7078(14) 0.5608(13) 0.079(3) Uani 0.418(9) 1 d PDU . . C2A2 C 0.6797(18) 0.6207(15) 0.5767(12) 0.0709(17) Uani 0.418(9) 1 d PDU . . C4A2 C 0.7193(11) 0.6716(10) 0.5368(9) 0.0790(19) Uani 0.418(9) 1 d PDU . . C5A2 C 0.6667(9) 0.7222(7) 0.5076(6) 0.086(2) Uani 0.418(9) 1 d PDU . . C6A2 C 0.7121(9) 0.7704(8) 0.4709(8) 0.093(2) Uani 0.418(9) 1 d PDU . . C7A2 C 0.6692(13) 0.8345(9) 0.4547(8) 0.094(3) Uani 0.418(9) 1 d PDU . . C8A2 C 0.6161(15) 0.8664(11) 0.4853(10) 0.095(3) Uani 0.418(9) 1 d PDU . . C9A2 C 0.5814(18) 0.9356(12) 0.4726(14) 0.095(3) Uani 0.418(9) 1 d PDU . . C10B C 0.6006(11) 0.6875(10) 0.4771(9) 0.088(2) Uani 0.418(9) 1 d PDU . . C7D2 C 1.1081(9) 0.6947(10) 0.9080(6) 0.099(3) Uani 0.71(2) 1 d PDU . . H3B1 H 0.9096 0.4898 0.5340 0.148 Uiso 1 1 d . . . H3B2 H 0.9492 0.4534 0.5847 0.148 Uiso 1 1 d . . . H5D H 1.1483 0.6546 0.8354 0.148 Uiso 1 1 d . . . H121 H 0.8207 0.6819 0.5725 0.070 Uiso 0.582(9) 1 d P . . H2A1 H 0.6404 0.5735 0.5683 0.105 Uiso 0.582(9) 1 d P . . H4A1 H 0.7184 0.6300 0.5079 0.105 Uiso 0.582(9) 1 d P . . H5A1 H 0.6243 0.7356 0.5484 0.105 Uiso 0.582(9) 1 d P . . H6A1 H 0.7193 0.7589 0.4754 0.105 Uiso 0.582(9) 1 d P . . H6A2 H 0.6598 0.7236 0.4358 0.105 Uiso 0.582(9) 1 d P . . H7A1 H 0.5666 0.8125 0.4610 0.105 Uiso 0.582(9) 1 d P . . H8A1 H 0.7057 0.8784 0.4762 0.105 Uiso 0.582(9) 1 d P . . H9A1 H 0.6441 0.9804 0.4632 0.105 Uiso 0.582(9) 1 d P . . H9A2 H 0.5686 0.9467 0.4863 0.105 Uiso 0.582(9) 1 d P . . H9A3 H 0.5872 0.9432 0.4228 0.105 Uiso 0.582(9) 1 d P . . H10A H 0.5248 0.6983 0.4906 0.105 Uiso 0.582(9) 1 d P . . H10B H 0.5438 0.6440 0.5362 0.105 Uiso 0.582(9) 1 d P . . H10C H 0.5734 0.6337 0.4754 0.105 Uiso 0.582(9) 1 d P . . H7D1 H 1.1151 0.6255 0.9117 0.105 Uiso 0.29(2) 1 d P . . H7D2 H 1.0511 0.6477 0.8694 0.105 Uiso 0.29(2) 1 d P . . H7D3 H 1.0734 0.6957 0.9187 0.105 Uiso 0.29(2) 1 d P . . H122 H 0.8201 0.6839 0.5727 0.080 Uiso 0.418(9) 1 d P . . H2A2 H 0.6469 0.5889 0.5557 0.120 Uiso 0.418(9) 1 d P . . H4A2 H 0.7382 0.6418 0.5081 0.120 Uiso 0.418(9) 1 d P . . H5A2 H 0.6410 0.7499 0.5358 0.120 Uiso 0.418(9) 1 d P . . H6A3 H 0.7594 0.7812 0.4903 0.120 Uiso 0.418(9) 1 d P . . H6A4 H 0.7279 0.7438 0.4377 0.120 Uiso 0.418(9) 1 d P . . H7A2 H 0.6842 0.8506 0.4182 0.120 Uiso 0.418(9) 1 d P . . H8A2 H 0.6012 0.8442 0.5139 0.120 Uiso 0.418(9) 1 d P . . H9A4 H 0.5460 0.9473 0.5015 0.120 Uiso 0.418(9) 1 d P . . H9A5 H 0.5563 0.9378 0.4374 0.120 Uiso 0.418(9) 1 d P . . H9A6 H 0.6223 0.9714 0.4724 0.120 Uiso 0.418(9) 1 d P . . H10D H 0.5728 0.6571 0.5004 0.120 Uiso 0.418(9) 1 d P . . H10E H 0.6228 0.6596 0.4463 0.120 Uiso 0.418(9) 1 d P . . H10F H 0.5666 0.7196 0.4604 0.120 Uiso 0.418(9) 1 d P . . H7D4 H 1.1198 0.6563 0.9311 0.120 Uiso 0.71(2) 1 d P . . H7D5 H 1.0520 0.6928 0.9000 0.120 Uiso 0.71(2) 1 d P . . H7D6 H 1.1153 0.7358 0.9305 0.120 Uiso 0.71(2) 1 d P . . H6I1 H 0.9373 0.5621 1.0149 0.120 Uiso 1 1 d . . . H6I2 H 0.9682 0.5059 0.9744 0.120 Uiso 1 1 d . . . H6I3 H 0.8805 0.5074 0.9910 0.120 Uiso 1 1 d . . . HW11 H 0.7992 0.5851 0.7328 0.120 Uiso 1 1 d . . . HW12 H 0.8626 0.5905 0.7681 0.120 Uiso 1 1 d . . . HW21 H 0.4564 0.3391 0.7075 0.120 Uiso 1 1 d . . . HW22 H 0.4006 0.3850 0.6901 0.120 Uiso 1 1 d . . . HW31 H 0.6889 0.4944 0.9443 0.120 Uiso 1 1 d . . . HW32 H 0.6472 0.4360 0.9585 0.120 Uiso 1 1 d . . . HW42 H 1.1936 0.9821 0.7168 0.120 Uiso 1 1 d . . . HW41 H 1.1625 0.9143 0.7167 0.120 Uiso 1 1 d . . . HW51 H 0.4200 0.9652 0.8638 0.120 Uiso 1 1 d . . . HW52 H 0.4566 0.9066 0.8390 0.120 Uiso 1 1 d . . . HW81 H 0.7021 0.9782 1.0360 0.120 Uiso 1 1 d . . . HW82 H 0.6679 1.0426 1.0435 0.120 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.062(3) 0.074(3) 0.083(3) -0.026(3) -0.021(2) 0.006(2) N2 0.063(3) 0.073(4) 0.066(3) -0.015(3) -0.020(2) 0.012(3) N3 0.062(3) 0.052(3) 0.066(3) -0.011(2) -0.011(2) 0.008(2) N4 0.048(2) 0.062(3) 0.069(3) -0.016(2) -0.002(2) 0.002(2) N5 0.0462(19) 0.055(3) 0.055(3) 0.006(2) 0.008(2) -0.005(2) N6 0.066(3) 0.053(3) 0.052(3) 0.005(2) 0.008(2) 0.008(2) N7 0.055(3) 0.058(3) 0.065(2) 0.002(3) 0.008(2) 0.010(3) N8 0.053(3) 0.058(3) 0.042(3) 0.002(2) 0.001(2) 0.001(2) N9 0.058(3) 0.053(2) 0.047(3) 0.004(2) 0.003(2) -0.004(2) N10 0.055(2) 0.068(3) 0.064(3) -0.001(2) 0.008(2) -0.012(2) N11 0.055(3) 0.058(3) 0.097(3) -0.009(2) -0.015(3) -0.003(3) O1 0.077(4) 0.134(5) 0.066(2) -0.010(4) -0.009(3) 0.035(4) O2 0.088(4) 0.065(3) 0.084(4) 0.004(3) -0.020(3) 0.008(3) O3 0.057(3) 0.070(3) 0.069(3) -0.024(3) 0.006(2) -0.010(2) O4 0.057(3) 0.078(4) 0.133(5) 0.020(4) 0.008(3) -0.006(3) O5 0.063(3) 0.054(3) 0.050(3) 0.013(2) 0.007(2) 0.011(2) O6 0.070(3) 0.075(3) 0.067(3) -0.007(3) 0.008(3) -0.007(3) O7 0.104(4) 0.094(4) 0.051(2) -0.007(3) 0.006(3) 0.026(4) O8 0.067(3) 0.059(3) 0.061(3) 0.002(2) 0.022(2) -0.002(2) O9 0.074(4) 0.074(4) 0.103(4) 0.017(3) 0.012(3) -0.013(3) O10 0.070(3) 0.064(3) 0.105(4) -0.014(3) -0.005(3) -0.001(3) O11 0.111(5) 0.067(3) 0.123(5) -0.028(3) -0.036(4) -0.007(3) C1A 0.067(5) 0.085(6) 0.109(7) -0.045(5) 0.010(5) -0.012(4) C3A 0.064(3) 0.075(4) 0.065(2) -0.019(3) -0.021(2) 0.011(3) C1B 0.063(3) 0.064(3) 0.067(4) -0.010(3) -0.015(3) 0.013(2) C2B 0.063(3) 0.057(3) 0.065(4) -0.010(2) -0.008(3) 0.016(2) C3B 0.069(4) 0.078(4) 0.090(5) -0.030(4) -0.021(4) 0.018(3) C4B 0.099(7) 0.075(5) 0.132(8) -0.032(5) -0.043(6) 0.013(4) C1C 0.076(5) 0.055(4) 0.081(5) -0.006(3) -0.029(4) 0.012(4) C2C 0.055(3) 0.064(3) 0.060(3) -0.010(3) -0.007(3) 0.005(2) C3C 0.043(2) 0.061(3) 0.063(3) -0.010(3) -0.006(2) 0.006(2) C1D 0.058(4) 0.087(6) 0.094(6) -0.034(5) 0.016(3) -0.006(4) C2D 0.046(3) 0.058(3) 0.066(3) -0.012(2) -0.003(2) 0.000(3) C3D 0.048(2) 0.062(3) 0.066(4) -0.006(3) 0.003(3) 0.000(2) C4D 0.066(4) 0.072(4) 0.079(4) -0.019(3) -0.020(3) -0.001(3) C5D 0.092(4) 0.083(4) 0.100(5) -0.012(3) -0.033(3) 0.010(4) C6D 0.094(5) 0.126(8) 0.132(8) -0.017(7) -0.046(5) 0.022(6) C1E 0.055(3) 0.056(3) 0.048(3) 0.006(2) 0.009(2) -0.004(2) C2E 0.058(3) 0.050(3) 0.043(3) 0.003(2) 0.002(2) 0.001(2) C3E 0.072(4) 0.083(4) 0.052(3) -0.004(3) 0.002(3) 0.005(3) C4E 0.104(6) 0.126(8) 0.054(5) -0.007(5) 0.019(4) 0.020(6) C5E 0.095(6) 0.110(7) 0.079(6) -0.028(5) -0.001(5) -0.024(5) C1F 0.083(5) 0.064(4) 0.059(4) 0.015(3) 0.009(4) 0.005(4) C2F 0.065(3) 0.058(3) 0.062(2) 0.008(3) 0.003(2) 0.018(2) C3F 0.051(3) 0.057(3) 0.062(2) 0.000(3) 0.007(2) 0.012(2) C4F 0.068(4) 0.081(4) 0.070(3) -0.001(3) -0.006(3) 0.019(3) C5F 0.097(5) 0.102(4) 0.070(3) -0.008(4) -0.017(4) 0.024(4) C6F 0.125(8) 0.115(5) 0.081(6) 0.015(5) -0.021(6) 0.021(6) C7F 0.153(10) 0.127(8) 0.112(8) -0.011(7) -0.042(7) -0.010(7) C1G 0.063(3) 0.065(4) 0.065(2) -0.005(3) 0.012(3) 0.008(3) C2G 0.065(3) 0.063(3) 0.051(2) -0.002(3) 0.011(3) 0.001(3) C3G 0.066(4) 0.112(7) 0.083(6) 0.001(5) 0.019(4) 0.003(5) C1H 0.053(3) 0.057(3) 0.041(3) 0.007(2) -0.001(3) -0.002(2) C2H 0.048(3) 0.059(3) 0.042(3) 0.004(2) 0.003(2) 0.000(2) C3H 0.055(3) 0.067(5) 0.075(5) -0.007(4) -0.001(4) -0.011(3) C1I 0.071(5) 0.070(5) 0.065(4) -0.001(4) 0.021(3) -0.015(4) C2I 0.064(3) 0.054(3) 0.056(3) 0.003(2) 0.002(3) -0.005(3) C3I 0.061(3) 0.062(3) 0.063(4) -0.004(2) 0.010(3) -0.009(2) C4I 0.077(3) 0.064(3) 0.068(4) 0.012(3) 0.003(3) 0.002(3) C5I 0.079(3) 0.077(5) 0.085(4) 0.015(4) -0.006(4) 0.002(4) C6I 0.119(8) 0.118(8) 0.122(7) 0.049(6) -0.030(6) 0.005(7) C7I 0.087(6) 0.122(8) 0.109(6) -0.002(6) 0.002(5) 0.026(6) C1J 0.062(4) 0.080(5) 0.060(4) 0.009(3) -0.003(4) -0.018(4) C2J 0.055(2) 0.073(4) 0.086(3) -0.013(3) 0.009(3) -0.011(3) C3J 0.049(3) 0.064(3) 0.094(3) -0.012(2) 0.001(3) -0.005(3) C4J 0.090(4) 0.101(5) 0.099(5) -0.021(4) 0.027(4) 0.000(4) C5J 0.094(4) 0.138(6) 0.122(6) -0.019(5) 0.034(5) -0.005(5) C6J 0.137(9) 0.152(8) 0.161(10) -0.033(7) 0.071(8) 0.014(9) C7J 0.110(8) 0.142(7) 0.134(9) -0.021(6) 0.045(7) -0.041(7) C1K 0.096(6) 0.061(4) 0.113(7) -0.007(4) -0.027(6) 0.005(4) C2K 0.055(3) 0.059(3) 0.104(3) -0.008(3) -0.022(2) -0.004(3) C3K 0.061(3) 0.065(3) 0.100(4) -0.023(3) -0.033(3) 0.000(2) C4K 0.058(3) 0.078(5) 0.130(5) 0.001(4) -0.026(3) -0.011(3) C5K 0.074(6) 0.115(8) 0.148(7) 0.008(7) -0.050(5) -0.017(6) C6K 0.057(5) 0.115(7) 0.147(7) 0.016(6) 0.004(5) -0.016(5) OW1 0.082(4) 0.121(5) 0.077(4) -0.002(4) -0.011(3) -0.018(4) OW2 0.121(6) 0.124(6) 0.149(6) 0.014(5) 0.004(5) 0.026(5) OW3 0.145(6) 0.107(5) 0.107(5) 0.023(4) -0.003(5) -0.006(5) OW4 0.222(10) 0.201(9) 0.267(10) -0.012(8) 0.037(8) -0.017(8) OW5 0.211(9) 0.157(7) 0.222(9) -0.010(7) 0.033(8) 0.021(7) OW8 0.200(9) 0.231(9) 0.144(7) -0.046(7) 0.043(7) 0.015(7) O121 0.086(5) 0.084(5) 0.068(4) -0.009(4) -0.015(4) 0.006(3) C2A1 0.070(3) 0.071(4) 0.067(4) -0.017(2) -0.024(2) 0.011(3) C4A1 0.083(4) 0.080(4) 0.070(3) -0.012(3) -0.020(3) 0.012(3) C5A1 0.091(4) 0.086(4) 0.077(4) 0.001(3) -0.020(3) 0.014(3) C6A1 0.100(4) 0.091(3) 0.083(4) 0.004(3) -0.014(4) 0.011(3) C7A1 0.102(5) 0.089(4) 0.087(5) 0.009(4) -0.007(5) 0.010(3) C8A1 0.103(6) 0.091(4) 0.091(5) 0.007(4) -0.002(5) 0.007(4) C9A1 0.101(7) 0.089(4) 0.092(6) 0.009(5) -0.003(6) 0.003(5) C10A 0.089(5) 0.091(6) 0.084(6) 0.003(5) -0.024(4) 0.015(4) C7D1 0.105(6) 0.084(7) 0.104(7) -0.003(5) -0.031(6) 0.008(6) O122 0.084(5) 0.084(6) 0.069(5) -0.006(5) -0.015(4) 0.005(4) C2A2 0.072(4) 0.073(4) 0.068(3) -0.016(2) -0.023(2) 0.011(3) C4A2 0.085(4) 0.082(4) 0.071(4) -0.010(3) -0.019(3) 0.011(3) C5A2 0.092(4) 0.087(4) 0.078(4) -0.002(3) -0.018(3) 0.012(3) C6A2 0.101(4) 0.094(5) 0.084(5) 0.003(4) -0.016(5) 0.009(3) C7A2 0.101(5) 0.092(4) 0.089(5) 0.006(4) -0.008(5) 0.009(4) C8A2 0.103(6) 0.089(4) 0.092(6) 0.009(4) -0.002(5) 0.006(4) C9A2 0.103(7) 0.088(5) 0.092(7) 0.010(5) 0.000(6) 0.006(5) C10B 0.093(5) 0.091(4) 0.081(5) 0.002(4) -0.024(4) 0.012(4) C7D2 0.106(6) 0.084(6) 0.106(6) 0.000(5) -0.026(5) -0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C3K 1.329(12) . ? N1 C2A1 1.41(3) . ? N1 C1A 1.467(11) . ? N1 C2A2 1.58(3) . ? N2 C3A 1.305(11) . ? N2 C1B 1.465(10) . ? N2 H2 0.8600 . ? N3 C2B 1.340(10) . ? N3 C2C 1.429(10) . ? N3 C1C 1.471(10) . ? N4 C3C 1.380(9) . ? N4 C1D 1.467(11) . ? N4 C2D 1.482(9) . ? N5 C3D 1.323(9) . ? N5 C1E 1.441(9) . ? N5 H5 0.8600 . ? N6 C2E 1.349(9) . ? N6 C2F 1.468(10) . ? N6 C1F 1.478(10) . ? N7 C3F 1.343(10) . ? N7 C1G 1.418(10) . ? N7 H7 0.8600 . ? N8 C2G 1.331(9) . ? N8 C1H 1.461(9) . ? N8 H8 0.8600 . ? N9 C2H 1.351(9) . ? N9 C1I 1.458(9) . ? N9 C2I 1.486(9) . ? N10 C3I 1.340(10) . ? N10 C2J 1.471(11) . ? N10 C1J 1.476(10) . ? N11 C3J 1.353(11) . ? N11 C1K 1.457(11) . ? N11 C2K 1.503(11) . ? O1 C3A 1.216(10) . ? O2 C2B 1.227(10) . ? O3 C3C 1.200(9) . ? O4 C3D 1.226(9) . ? O5 C2E 1.226(8) . ? O6 C3F 1.216(9) . ? O7 C2G 1.237(9) . ? O8 C2H 1.216(8) . ? O9 C3I 1.218(9) . ? O10 C3J 1.249(10) . ? O11 C3K 1.247(10) . ? C1A H1A1 0.9600 . ? C1A H1A2 0.9600 . ? C1A H1A3 0.9600 . ? C3A C2A1 1.49(2) . ? C3A C2A2 1.59(3) . ? C1B C2B 1.532(12) . ? C1B C3B 1.553(11) . ? C1B H1B 0.9800 . ? C3B C4B 1.519(4) . ? C3B H3B1 0.967(10) . ? C3B H3B2 0.969(8) . ? C4B H4B1 0.9600 . ? C4B H4B2 0.9600 . ? C4B H4B3 0.9600 . ? C1C H1C1 0.9600 . ? C1C H1C2 0.9600 . ? C1C H1C3 0.9600 . ? C2C C3C 1.540(10) . ? C2C H2C1 0.9700 . ? C2C H2C2 0.9700 . ? C1D H1D1 0.9600 . ? C1D H1D2 0.9600 . ? C1D H1D3 0.9600 . ? C2D C3D 1.527(11) . ? C2D C4D 1.553(10) . ? C2D H2D 0.9800 . ? C4D C5D 1.505(13) . ? C4D H4D1 0.9700 . ? C4D H4D2 0.9700 . ? C5D C7D1 1.518(4) . ? C5D C7D2 1.523(4) . ? C5D C6D 1.508(15) . ? C5D H5D 1.000(10) . ? C6D H6D1 0.9600 . ? C6D H6D2 0.9600 . ? C6D H6D3 0.9600 . ? C1E C2E 1.508(10) . ? C1E C3E 1.541(11) . ? C1E H1E 0.9800 . ? C3E C5E 1.487(13) . ? C3E C4E 1.516(12) . ? C3E H3E 0.9800 . ? C4E H4E1 0.9600 . ? C4E H4E2 0.9600 . ? C4E H4E3 0.9600 . ? C5E H5E1 0.9600 . ? C5E H5E2 0.9600 . ? C5E H5E3 0.9600 . ? C1F H1F1 0.9600 . ? C1F H1F2 0.9600 . ? C1F H1F3 0.9600 . ? C2F C4F 1.504(12) . ? C2F C3F 1.554(11) . ? C2F H2F 0.9800 . ? C4F C5F 1.532(13) . ? C4F H4F1 0.9700 . ? C4F H4F2 0.9700 . ? C5F C7F 1.538(17) . ? C5F C6F 1.533(15) . ? C5F H5F 0.9800 . ? C6F H6F1 0.9600 . ? C6F H6F2 0.9600 . ? C6F H6F3 0.9600 . ? C7F H7F1 0.9600 . ? C7F H7F2 0.9600 . ? C7F H7F3 0.9600 . ? C1G C2G 1.518(11) . ? C1G C3G 1.538(12) . ? C1G H1G 0.9800 . ? C3G H3G1 0.9600 . ? C3G H3G2 0.9600 . ? C3G H3G3 0.9600 . ? C1H C3H 1.511(10) . ? C1H C2H 1.524(10) . ? C1H H1H 0.9800 . ? C3H H3H1 0.9600 . ? C3H H3H2 0.9600 . ? C3H H3H3 0.9600 . ? C1I H1I1 0.9600 . ? C1I H1I2 0.9600 . ? C1I H1I3 0.9600 . ? C2I C3I 1.526(11) . ? C2I C4I 1.561(11) . ? C2I H2I 0.9800 . ? C4I C5I 1.514(13) . ? C4I H4I1 0.9700 . ? C4I H4I2 0.9700 . ? C5I C7I 1.470(15) . ? C5I C6I 1.562(14) . ? C5I H5I 0.9800 . ? C6I H6I1 0.954(15) . ? C6I H6I2 0.992(14) . ? C6I H6I3 0.955(14) . ? C7I H7I1 0.9600 . ? C7I H7I2 0.9600 . ? C7I H7I3 0.9600 . ? C1J H1J1 0.9600 . ? C1J H1J2 0.9600 . ? C1J H1J3 0.9600 . ? C2J C3J 1.506(13) . ? C2J C4J 1.544(13) . ? C2J H2J 0.9800 . ? C4J C5J 1.516(4) . ? C4J H4J1 0.9700 . ? C4J H4J2 0.9700 . ? C5J C7J 1.540(19) . ? C5J C6J 1.567(18) . ? C5J H5J 0.9800 . ? C6J H6J1 0.9600 . ? C6J H6J2 0.9600 . ? C6J H6J3 0.9600 . ? C7J H7J1 0.9600 . ? C7J H7J2 0.9600 . ? C7J H7J3 0.9600 . ? C1K H1K1 0.9600 . ? C1K H1K2 0.9600 . ? C1K H1K3 0.9600 . ? C2K C3K 1.525(13) . ? C2K C4K 1.547(12) . ? C2K H2K 0.9800 . ? C4K C6K 1.504(16) . ? C4K C5K 1.518(15) . ? C4K H4K 0.9800 . ? C5K H5K1 0.9600 . ? C5K H5K2 0.9600 . ? C5K H5K3 0.9600 . ? C6K H6K1 0.9600 . ? C6K H6K2 0.9600 . ? C6K H6K3 0.9600 . ? OW1 HW11 0.807 . ? OW1 HW12 0.809 . ? OW2 HW21 0.874 . ? OW2 HW22 0.943 . ? OW3 HW31 0.794 . ? OW3 HW32 0.834 . ? OW4 HW42 0.894 . ? OW4 HW41 0.869 . ? OW5 HW51 0.925 . ? OW5 HW52 0.944 . ? OW8 HW81 0.839 . ? OW8 HW82 0.886 . ? O121 C4A2 1.05(3) . ? O121 C4A1 1.417(13) . ? O121 H121 1.093(16) . ? O121 H122 1.075(16) . ? C2A1 C4A1 1.555(16) . ? C2A1 C4A2 1.89(3) . ? C2A1 H2A1 1.00(2) . ? C2A1 H2A2 0.95(2) . ? C4A1 C2A2 1.22(3) . ? C4A1 C5A1 1.521(4) . ? C4A1 C5A2 1.587(18) . ? C4A1 O122 1.76(3) . ? C4A1 H4A1 0.987(18) . ? C4A1 H4A2 1.046(18) . ? C5A1 C5A2 0.679(17) . ? C5A1 C10B 1.22(2) . ? C5A1 C10A 1.520(4) . ? C5A1 C6A1 1.521(4) . ? C5A1 C4A2 1.63(2) . ? C5A1 H5A1 0.976(13) . ? C5A1 H5A2 0.994(12) . ? C5A1 H10D 1.507(11) . ? C6A1 C6A2 0.933(18) . ? C6A1 C5A2 1.036(18) . ? C6A1 C7A1 1.520(4) . ? C6A1 C10B 1.643(18) . ? C6A1 C7A2 1.725(18) . ? C6A1 H6A1 0.984(15) . ? C6A1 H6A2 0.990(14) . ? C6A1 H6A4 1.371(13) . ? C7A1 C7A2 1.02(2) . ? C7A1 C8A2 1.12(3) . ? C7A1 C8A1 1.340(4) . ? C7A1 C6A2 1.861(18) . ? C7A1 H7A1 0.884(13) . ? C7A1 H8A2 1.315(18) . ? C8A1 C8A2 0.70(3) . ? C8A1 C7A2 0.97(2) . ? C8A1 C9A1 1.493(17) . ? C8A1 C9A2 1.65(3) . ? C8A1 H8A1 1.003(18) . ? C8A1 H7A2 1.48(2) . ? C8A1 H8A2 1.486(19) . ? C9A1 C9A2 0.55(4) . ? C9A1 C8A2 1.61(3) . ? C9A1 H9A1 0.99(2) . ? C9A1 H9A2 0.92(2) . ? C9A1 H9A3 0.97(2) . ? C9A1 H9A4 1.46(2) . ? C9A1 H9A5 1.05(2) . ? C9A1 H9A6 0.69(2) . ? C10A C10B 1.02(2) . ? C10A H10A 0.971(13) . ? C10A H10B 0.941(16) . ? C10A H10C 0.965(18) . ? C10A H10D 0.266(17) . ? C10A H10F 1.495(15) . ? C7D1 C7D2 0.84(4) . ? C7D1 H7D1 0.94(4) . ? C7D1 H7D2 0.95(4) . ? C7D1 H7D3 1.07(5) . ? C7D1 H7D4 1.10(4) . ? C7D1 H7D5 1.03(4) . ? O122 C4A2 1.394(16) . ? O122 H121 0.92(2) . ? O122 H122 0.89(2) . ? C2A2 C4A2 1.550(18) . ? C2A2 H2A1 1.17(3) . ? C2A2 H2A2 0.99(3) . ? C4A2 C5A2 1.522(4) . ? C4A2 H4A1 1.08(3) . ? C4A2 H4A2 0.96(3) . ? C5A2 C6A2 1.519(4) . ? C5A2 C10B 1.521(4) . ? C5A2 H5A1 1.256(17) . ? C5A2 H6A1 1.399(16) . ? C5A2 H5A2 0.979(17) . ? C6A2 C7A2 1.515(4) . ? C6A2 H6A1 0.281(14) . ? C6A2 H6A2 1.55(2) . ? C6A2 H6A3 0.966(19) . ? C6A2 H6A4 0.99(2) . ? C7A2 C8A2 1.337(4) . ? C7A2 H8A1 1.19(3) . ? C7A2 H7A2 0.970(16) . ? C8A2 C9A2 1.520(19) . ? C8A2 H7A1 1.49(3) . ? C8A2 H8A1 1.58(3) . ? C8A2 H8A2 0.86(2) . ? C9A2 H9A1 1.42(3) . ? C9A2 H9A2 0.45(3) . ? C9A2 H9A3 1.22(3) . ? C9A2 H9A4 0.95(3) . ? C9A2 H9A5 0.96(3) . ? C9A2 H9A6 1.00(3) . ? C10B H10A 1.37(2) . ? C10B H10C 1.160(18) . ? C10B H10D 0.95(2) . ? C10B H10E 1.00(3) . ? C10B H10F 0.952(18) . ? C7D2 H7D1 1.369(19) . ? C7D2 H7D3 0.654(13) . ? C7D2 H7D4 0.961(16) . ? C7D2 H7D5 0.990(17) . ? C7D2 H7D6 0.98(2) . ? 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 C3K N1 C2A1 114.6(10) . . ? C3K N1 C1A 121.5(8) . . ? C2A1 N1 C1A 120.1(10) . . ? C3K N1 C2A2 124.3(12) . . ? C2A1 N1 C2A2 11.3(12) . . ? C1A N1 C2A2 112.7(12) . . ? C3A N2 C1B 120.5(7) . . ? C3A N2 H2 119.7 . . ? C1B N2 H2 119.7 . . ? C2B N3 C2C 119.7(7) . . ? C2B N3 C1C 125.6(7) . . ? C2C N3 C1C 114.7(6) . . ? C3C N4 C1D 121.8(6) . . ? C3C N4 C2D 117.1(6) . . ? C1D N4 C2D 119.2(6) . . ? C3D N5 C1E 122.7(6) . . ? C3D N5 H5 118.6 . . ? C1E N5 H5 118.6 . . ? C2E N6 C2F 118.2(6) . . ? C2E N6 C1F 125.0(7) . . ? C2F N6 C1F 116.7(6) . . ? C3F N7 C1G 121.3(8) . . ? C3F N7 H7 119.3 . . ? C1G N7 H7 119.3 . . ? C2G N8 C1H 123.8(6) . . ? C2G N8 H8 118.1 . . ? C1H N8 H8 118.1 . . ? C2H N9 C1I 124.0(6) . . ? C2H N9 C2I 119.7(6) . . ? C1I N9 C2I 116.3(6) . . ? C3I N10 C2J 117.6(7) . . ? C3I N10 C1J 125.2(7) . . ? C2J N10 C1J 116.3(7) . . ? C3J N11 C1K 123.3(8) . . ? C3J N11 C2K 119.2(7) . . ? C1K N11 C2K 117.4(7) . . ? N1 C1A H1A1 109.5 . . ? N1 C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? N1 C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? O1 C3A N2 122.7(8) . . ? O1 C3A C2A1 116.7(11) . . ? N2 C3A C2A1 120.5(11) . . ? O1 C3A C2A2 124.6(14) . . ? N2 C3A C2A2 112.4(13) . . ? C2A1 C3A C2A2 12.0(12) . . ? N2 C1B C2B 111.0(6) . . ? N2 C1B C3B 109.3(6) . . ? C2B C1B C3B 108.7(7) . . ? N2 C1B H1B 109.3 . . ? C2B C1B H1B 109.3 . . ? C3B C1B H1B 109.3 . . ? O2 C2B N3 122.0(8) . . ? O2 C2B C1B 119.9(7) . . ? N3 C2B C1B 118.0(7) . . ? C4B C3B C1B 112.0(8) . . ? C4B C3B H3B1 104.3(8) . . ? C1B C3B H3B1 111.6(8) . . ? C4B C3B H3B2 108.9(8) . . ? C1B C3B H3B2 111.0(7) . . ? H3B1 C3B H3B2 108.9(9) . . ? C3B C4B H4B1 109.5 . . ? C3B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C3B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? N3 C1C H1C1 109.5 . . ? N3 C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? N3 C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? N3 C2C C3C 112.1(6) . . ? N3 C2C H2C1 109.2 . . ? C3C C2C H2C1 109.2 . . ? N3 C2C H2C2 109.2 . . ? C3C C2C H2C2 109.2 . . ? H2C1 C2C H2C2 107.9 . . ? O3 C3C N4 122.7(7) . . ? O3 C3C C2C 122.1(7) . . ? N4 C3C C2C 115.3(6) . . ? N4 C1D H1D1 109.5 . . ? N4 C1D H1D2 109.5 . . ? H1D1 C1D H1D2 109.5 . . ? N4 C1D H1D3 109.5 . . ? H1D1 C1D H1D3 109.5 . . ? H1D2 C1D H1D3 109.5 . . ? N4 C2D C3D 107.6(6) . . ? N4 C2D C4D 112.8(6) . . ? C3D C2D C4D 111.1(6) . . ? N4 C2D H2D 108.4 . . ? C3D C2D H2D 108.4 . . ? C4D C2D H2D 108.4 . . ? O4 C3D N5 122.9(7) . . ? O4 C3D C2D 120.9(7) . . ? N5 C3D C2D 116.1(7) . . ? C5D C4D C2D 114.5(7) . . ? C5D C4D H4D1 108.6 . . ? C2D C4D H4D1 108.6 . . ? C5D C4D H4D2 108.6 . . ? C2D C4D H4D2 108.6 . . ? H4D1 C4D H4D2 107.6 . . ? C4D C5D C7D1 119.2(17) . . ? C4D C5D C7D2 109.9(10) . . ? C7D1 C5D C7D2 32.0(16) . . ? C4D C5D C6D 111.6(10) . . ? C7D1 C5D C6D 120.7(18) . . ? C7D2 C5D C6D 103.6(11) . . ? C4D C5D H5D 112.1(8) . . ? C7D1 C5D H5D 75(2) . . ? C7D2 C5D H5D 106.3(12) . . ? C6D C5D H5D 112.8(10) . . ? C5D C6D H6D1 109.5 . . ? C5D C6D H6D2 109.5 . . ? H6D1 C6D H6D2 109.5 . . ? C5D C6D H6D3 109.5 . . ? H6D1 C6D H6D3 109.5 . . ? H6D2 C6D H6D3 109.5 . . ? N5 C1E C2E 109.3(5) . . ? N5 C1E C3E 111.4(6) . . ? C2E C1E C3E 108.9(6) . . ? N5 C1E H1E 109.1 . . ? C2E C1E H1E 109.1 . . ? C3E C1E H1E 109.1 . . ? O5 C2E N6 120.7(7) . . ? O5 C2E C1E 121.1(6) . . ? N6 C2E C1E 117.9(6) . . ? C5E C3E C4E 110.2(8) . . ? C5E C3E C1E 112.4(7) . . ? C4E C3E C1E 112.6(7) . . ? C5E C3E H3E 107.1 . . ? C4E C3E H3E 107.1 . . ? C1E C3E H3E 107.1 . . ? C3E C4E H4E1 109.5 . . ? C3E C4E H4E2 109.5 . . ? H4E1 C4E H4E2 109.5 . . ? C3E C4E H4E3 109.5 . . ? H4E1 C4E H4E3 109.5 . . ? H4E2 C4E H4E3 109.5 . . ? C3E C5E H5E1 109.5 . . ? C3E C5E H5E2 109.5 . . ? H5E1 C5E H5E2 109.5 . . ? C3E C5E H5E3 109.5 . . ? H5E1 C5E H5E3 109.5 . . ? H5E2 C5E H5E3 109.5 . . ? N6 C1F H1F1 109.5 . . ? N6 C1F H1F2 109.5 . . ? H1F1 C1F H1F2 109.5 . . ? N6 C1F H1F3 109.5 . . ? H1F1 C1F H1F3 109.5 . . ? H1F2 C1F H1F3 109.5 . . ? N6 C2F C4F 112.7(6) . . ? N6 C2F C3F 108.2(6) . . ? C4F C2F C3F 117.0(7) . . ? N6 C2F H2F 106.1 . . ? C4F C2F H2F 106.1 . . ? C3F C2F H2F 106.1 . . ? O6 C3F N7 122.0(7) . . ? O6 C3F C2F 119.4(7) . . ? N7 C3F C2F 118.6(7) . . ? C2F C4F C5F 115.4(8) . . ? C2F C4F H4F1 108.4 . . ? C5F C4F H4F1 108.4 . . ? C2F C4F H4F2 108.4 . . ? C5F C4F H4F2 108.4 . . ? H4F1 C4F H4F2 107.5 . . ? C7F C5F C4F 109.4(10) . . ? C7F C5F C6F 112.5(9) . . ? C4F C5F C6F 113.4(9) . . ? C7F C5F H5F 107.0 . . ? C4F C5F H5F 107.0 . . ? C6F C5F H5F 107.0 . . ? C5F C6F H6F1 109.5 . . ? C5F C6F H6F2 109.5 . . ? H6F1 C6F H6F2 109.5 . . ? C5F C6F H6F3 109.5 . . ? H6F1 C6F H6F3 109.5 . . ? H6F2 C6F H6F3 109.5 . . ? C5F C7F H7F1 109.5 . . ? C5F C7F H7F2 109.5 . . ? H7F1 C7F H7F2 109.5 . . ? C5F C7F H7F3 109.5 . . ? H7F1 C7F H7F3 109.5 . . ? H7F2 C7F H7F3 109.5 . . ? N7 C1G C2G 115.4(6) . . ? N7 C1G C3G 109.9(8) . . ? C2G C1G C3G 110.0(7) . . ? N7 C1G H1G 107.1 . . ? C2G C1G H1G 107.1 . . ? C3G C1G H1G 107.1 . . ? O7 C2G N8 121.8(8) . . ? O7 C2G C1G 120.4(7) . . ? N8 C2G C1G 117.8(7) . . ? C1G C3G H3G1 109.5 . . ? C1G C3G H3G2 109.5 . . ? H3G1 C3G H3G2 109.5 . . ? C1G C3G H3G3 109.5 . . ? H3G1 C3G H3G3 109.5 . . ? H3G2 C3G H3G3 109.5 . . ? N8 C1H C3H 111.6(6) . . ? N8 C1H C2H 108.5(5) . . ? C3H C1H C2H 111.4(6) . . ? N8 C1H H1H 108.4 . . ? C3H C1H H1H 108.4 . . ? C2H C1H H1H 108.4 . . ? O8 C2H N9 122.4(7) . . ? O8 C2H C1H 120.4(6) . . ? N9 C2H C1H 117.2(6) . . ? C1H C3H H3H1 109.5 . . ? C1H C3H H3H2 109.5 . . ? H3H1 C3H H3H2 109.5 . . ? C1H C3H H3H3 109.5 . . ? H3H1 C3H H3H3 109.5 . . ? H3H2 C3H H3H3 109.5 . . ? N9 C1I H1I1 109.5 . . ? N9 C1I H1I2 109.5 . . ? H1I1 C1I H1I2 109.5 . . ? N9 C1I H1I3 109.5 . . ? H1I1 C1I H1I3 109.5 . . ? H1I2 C1I H1I3 109.5 . . ? N9 C2I C3I 109.6(6) . . ? N9 C2I C4I 111.5(6) . . ? C3I C2I C4I 111.5(6) . . ? N9 C2I H2I 108.1 . . ? C3I C2I H2I 108.1 . . ? C4I C2I H2I 108.1 . . ? O9 C3I N10 121.5(8) . . ? O9 C3I C2I 120.4(8) . . ? N10 C3I C2I 118.0(7) . . ? C5I C4I C2I 116.3(7) . . ? C5I C4I H4I1 108.2 . . ? C2I C4I H4I1 108.2 . . ? C5I C4I H4I2 108.2 . . ? C2I C4I H4I2 108.2 . . ? H4I1 C4I H4I2 107.4 . . ? C7I C5I C4I 111.7(9) . . ? C7I C5I C6I 112.7(10) . . ? C4I C5I C6I 107.0(9) . . ? C7I C5I H5I 108.4 . . ? C4I C5I H5I 108.4 . . ? C6I C5I H5I 108.4 . . ? C5I C6I H6I1 111.5(11) . . ? C5I C6I H6I2 108.9(12) . . ? H6I1 C6I H6I2 107.4(12) . . ? C5I C6I H6I3 111.1(11) . . ? H6I1 C6I H6I3 110.4(14) . . ? H6I2 C6I H6I3 107.3(13) . . ? C5I C7I H7I1 109.5 . . ? C5I C7I H7I2 109.5 . . ? H7I1 C7I H7I2 109.5 . . ? C5I C7I H7I3 109.5 . . ? H7I1 C7I H7I3 109.5 . . ? H7I2 C7I H7I3 109.5 . . ? N10 C1J H1J1 109.5 . . ? N10 C1J H1J2 109.5 . . ? H1J1 C1J H1J2 109.5 . . ? N10 C1J H1J3 109.5 . . ? H1J1 C1J H1J3 109.5 . . ? H1J2 C1J H1J3 109.5 . . ? N10 C2J C3J 112.1(7) . . ? N10 C2J C4J 108.0(7) . . ? C3J C2J C4J 115.0(8) . . ? N10 C2J H2J 107.1 . . ? C3J C2J H2J 107.1 . . ? C4J C2J H2J 107.1 . . ? O10 C3J N11 120.7(8) . . ? O10 C3J C2J 120.0(8) . . ? N11 C3J C2J 119.2(8) . . ? C5J C4J C2J 116.4(9) . . ? C5J C4J H4J1 108.2 . . ? C2J C4J H4J1 108.2 . . ? C5J C4J H4J2 108.2 . . ? C2J C4J H4J2 108.2 . . ? H4J1 C4J H4J2 107.3 . . ? C4J C5J C7J 108.1(11) . . ? C4J C5J C6J 105.5(10) . . ? C7J C5J C6J 105.8(11) . . ? C4J C5J H5J 112.3 . . ? C7J C5J H5J 112.3 . . ? C6J C5J H5J 112.3 . . ? C5J C6J H6J1 109.5 . . ? C5J C6J H6J2 109.5 . . ? H6J1 C6J H6J2 109.5 . . ? C5J C6J H6J3 109.5 . . ? H6J1 C6J H6J3 109.5 . . ? H6J2 C6J H6J3 109.5 . . ? C5J C7J H7J1 109.5 . . ? C5J C7J H7J2 109.5 . . ? H7J1 C7J H7J2 109.5 . . ? C5J C7J H7J3 109.5 . . ? H7J1 C7J H7J3 109.5 . . ? H7J2 C7J H7J3 109.5 . . ? N11 C1K H1K1 109.5 . . ? N11 C1K H1K2 109.5 . . ? H1K1 C1K H1K2 109.5 . . ? N11 C1K H1K3 109.5 . . ? H1K1 C1K H1K3 109.5 . . ? H1K2 C1K H1K3 109.5 . . ? N11 C2K C3K 109.1(6) . . ? N11 C2K C4K 111.8(8) . . ? C3K C2K C4K 113.2(8) . . ? N11 C2K H2K 107.5 . . ? C3K C2K H2K 107.5 . . ? C4K C2K H2K 107.5 . . ? O11 C3K N1 120.6(9) . . ? O11 C3K C2K 120.2(9) . . ? N1 C3K C2K 119.2(7) . . ? C6K C4K C5K 112.8(9) . . ? C6K C4K C2K 111.1(8) . . ? C5K C4K C2K 108.1(9) . . ? C6K C4K H4K 108.2 . . ? C5K C4K H4K 108.2 . . ? C2K C4K H4K 108.2 . . ? C4K C5K H5K1 109.5 . . ? C4K C5K H5K2 109.5 . . ? H5K1 C5K H5K2 109.5 . . ? C4K C5K H5K3 109.5 . . ? H5K1 C5K H5K3 109.5 . . ? H5K2 C5K H5K3 109.5 . . ? C4K C6K H6K1 109.5 . . ? C4K C6K H6K2 109.5 . . ? H6K1 C6K H6K2 109.5 . . ? C4K C6K H6K3 109.5 . . ? H6K1 C6K H6K3 109.5 . . ? H6K2 C6K H6K3 109.5 . . ? HW11 OW1 HW12 119.1 . . ? HW21 OW2 HW22 99.6 . . ? HW31 OW3 HW32 118.6 . . ? HW42 OW4 HW41 109.5 . . ? HW51 OW5 HW52 101.4 . . ? HW81 OW8 HW82 109.7 . . ? C4A2 O121 C4A1 10.2(15) . . ? C4A2 O121 H121 132(2) . . ? C4A1 O121 H121 129.6(15) . . ? C4A2 O121 H122 134(3) . . ? C4A1 O121 H122 131.5(16) . . ? H121 O121 H122 1.94(4) . . ? N1 C2A1 C3A 114.2(15) . . ? N1 C2A1 C4A1 110.7(14) . . ? C3A C2A1 C4A1 109.5(13) . . ? N1 C2A1 C4A2 110.0(15) . . ? C3A C2A1 C4A2 102.7(13) . . ? C4A1 C2A1 C4A2 8.7(8) . . ? N1 C2A1 H2A1 109.3(17) . . ? C3A C2A1 H2A1 105.3(17) . . ? C4A1 C2A1 H2A1 107.5(16) . . ? C4A2 C2A1 H2A1 115.3(18) . . ? N1 C2A1 H2A2 117.4(19) . . ? C3A C2A1 H2A2 118(2) . . ? C4A1 C2A1 H2A2 81.5(12) . . ? C4A2 C2A1 H2A2 89.5(14) . . ? H2A1 C2A1 H2A2 26.2(6) . . ? C2A2 C4A1 O121 110(2) . . ? C2A2 C4A1 C5A1 113.2(19) . . ? O121 C4A1 C5A1 109.6(10) . . ? C2A2 C4A1 C2A1 2(2) . . ? O121 C4A1 C2A1 111.6(12) . . ? C5A1 C4A1 C2A1 111.1(11) . . ? C2A2 C4A1 C5A2 137(2) . . ? O121 C4A1 C5A2 89.6(11) . . ? C5A1 C4A1 C5A2 25.1(7) . . ? C2A1 C4A1 C5A2 134.8(14) . . ? C2A2 C4A1 O122 110.3(19) . . ? O121 C4A1 O122 0.6(19) . . ? C5A1 C4A1 O122 109.5(13) . . ? C2A1 C4A1 O122 112.2(17) . . ? C5A2 C4A1 O122 89.3(12) . . ? C2A2 C4A1 H4A1 109(2) . . ? O121 C4A1 H4A1 107.5(14) . . ? C5A1 C4A1 H4A1 107.9(10) . . ? C2A1 C4A1 H4A1 109.0(13) . . ? C5A2 C4A1 H4A1 101.0(12) . . ? O122 C4A1 H4A1 107.1(16) . . ? C2A2 C4A1 H4A2 122(2) . . ? O121 C4A1 H4A2 84.6(13) . . ? C5A1 C4A1 H4A2 113.4(10) . . ? C2A1 C4A1 H4A2 123.1(13) . . ? C5A2 C4A1 H4A2 97.3(12) . . ? O122 C4A1 H4A2 84.1(14) . . ? H4A1 C4A1 H4A2 23.3(4) . . ? C5A2 C5A1 C10B 103(2) . . ? C5A2 C5A1 C10A 144.8(19) . . ? C10B C5A1 C10A 41.9(10) . . ? C5A2 C5A1 C4A1 82.9(16) . . ? C10B C5A1 C4A1 118.7(15) . . ? C10A C5A1 C4A1 112.9(6) . . ? C5A2 C5A1 C6A1 34.5(15) . . ? C10B C5A1 C6A1 72.8(10) . . ? C10A C5A1 C6A1 112.5(6) . . ? C4A1 C5A1 C6A1 111.9(6) . . ? C5A2 C5A1 C4A2 68.6(16) . . ? C10B C5A1 C4A2 124.3(18) . . ? C10A C5A1 C4A2 127.0(11) . . ? C4A1 C5A1 C4A2 14.9(8) . . ? C6A1 C5A1 C4A2 99.4(10) . . ? C5A2 C5A1 H5A1 97(2) . . ? C10B C5A1 H5A1 132.0(15) . . ? C10A C5A1 H5A1 107.1(11) . . ? C4A1 C5A1 H5A1 106.6(10) . . ? C6A1 C5A1 H5A1 105.2(9) . . ? C4A2 C5A1 H5A1 103.6(12) . . ? C5A2 C5A1 H5A2 68.6(18) . . ? C10B C5A1 H5A2 129.3(14) . . ? C10A C5A1 H5A2 127.3(11) . . ? C4A1 C5A1 H5A2 109.9(10) . . ? C6A1 C5A1 H5A2 76.8(8) . . ? C4A2 C5A1 H5A2 99.8(11) . . ? H5A1 C5A1 H5A2 29.7(4) . . ? C5A2 C5A1 H10D 141(2) . . ? C10B C5A1 H10D 39.2(10) . . ? C10A C5A1 H10D 10.1(6) . . ? C4A1 C5A1 H10D 105.0(7) . . ? C6A1 C5A1 H10D 111.9(8) . . ? C4A2 C5A1 H10D 118.4(11) . . ? H5A1 C5A1 H10D 116.3(10) . . ? H5A2 C5A1 H10D 137.4(11) . . ? C6A2 C6A1 C5A2 100.9(18) . . ? C6A2 C6A1 C7A1 95.7(12) . . ? C5A2 C6A1 C7A1 121.4(14) . . ? C6A2 C6A1 C5A1 122.6(15) . . ? C5A2 C6A1 C5A1 21.8(9) . . ? C7A1 C6A1 C5A1 112.2(7) . . ? C6A2 C6A1 C10B 157.9(16) . . ? C5A2 C6A1 C10B 64.7(9) . . ? C7A1 C6A1 C10B 106.0(11) . . ? C5A1 C6A1 C10B 45.1(9) . . ? C6A2 C6A1 C7A2 61.2(10) . . ? C5A2 C6A1 C7A2 133.8(17) . . ? C7A1 C6A1 C7A2 36.1(8) . . ? C5A1 C6A1 C7A2 138.8(10) . . ? C10B C6A1 C7A2 140.9(13) . . ? C6A2 C6A1 H6A1 16.6(9) . . ? C5A2 C6A1 H6A1 87.6(13) . . ? C7A1 C6A1 H6A1 111.4(10) . . ? C5A1 C6A1 H6A1 109.4(9) . . ? C10B C6A1 H6A1 141.4(11) . . ? C7A2 C6A1 H6A1 77.6(10) . . ? C6A2 C6A1 H6A2 106.9(18) . . ? C5A2 C6A1 H6A2 118.2(14) . . ? C7A1 C6A1 H6A2 109.4(11) . . ? C5A1 C6A1 H6A2 108.9(10) . . ? C10B C6A1 H6A2 69.6(13) . . ? C7A2 C6A1 H6A2 107.9(11) . . ? H6A1 C6A1 H6A2 105.2(11) . . ? C6A2 C6A1 H6A4 46.5(14) . . ? C5A2 C6A1 H6A4 114.9(13) . . ? C7A1 C6A1 H6A4 117.1(8) . . ? C5A1 C6A1 H6A4 130.1(7) . . ? C10B C6A1 H6A4 122.2(13) . . ? C7A2 C6A1 H6A4 84.3(8) . . ? H6A1 C6A1 H6A4 44.9(5) . . ? H6A2 C6A1 H6A4 61.2(6) . . ? C7A2 C7A1 C8A2 77.0(15) . . ? C7A2 C7A1 C8A1 46.2(12) . . ? C8A2 C7A1 C8A1 31.7(13) . . ? C7A2 C7A1 C6A1 82.9(11) . . ? C8A2 C7A1 C6A1 138.6(19) . . ? C8A1 C7A1 C6A1 123.3(8) . . ? C7A2 C7A1 C6A2 54.4(8) . . ? C8A2 C7A1 C6A2 114.6(17) . . ? C8A1 C7A1 C6A2 93.6(9) . . ? C6A1 C7A1 C6A2 29.9(6) . . ? C7A2 C7A1 H7A1 147.6(19) . . ? C8A2 C7A1 H7A1 94.9(19) . . ? C8A1 C7A1 H7A1 116.7(11) . . ? C6A1 C7A1 H7A1 120.0(11) . . ? C6A2 C7A1 H7A1 149.4(13) . . ? C7A2 C7A1 H8A2 104.7(18) . . ? C8A2 C7A1 H8A2 40.2(14) . . ? C8A1 C7A1 H8A2 68.0(12) . . ? C6A1 C7A1 H8A2 115.2(10) . . ? C6A2 C7A1 H8A2 110.0(11) . . ? H7A1 C7A1 H8A2 86.7(12) . . ? C8A2 C8A1 C7A2 105(2) . . ? C8A2 C8A1 C7A1 57(2) . . ? C7A2 C8A1 C7A1 49.5(14) . . ? C8A2 C8A1 C9A1 87(2) . . ? C7A2 C8A1 C9A1 149(2) . . ? C7A1 C8A1 C9A1 126.0(14) . . ? C8A2 C8A1 C9A2 67.3(19) . . ? C7A2 C8A1 C9A2 151(3) . . ? C7A1 C8A1 C9A2 111.2(16) . . ? C9A1 C8A1 C9A2 19.5(13) . . ? C8A2 C8A1 H8A1 136(4) . . ? C7A2 C8A1 H8A1 74(2) . . ? C7A1 C8A1 H8A1 116.4(11) . . ? C9A1 C8A1 H8A1 117.5(13) . . ? C9A2 C8A1 H8A1 131.6(17) . . ? C8A2 C8A1 H7A2 133(3) . . ? C7A2 C8A1 H7A2 40.3(12) . . ? C7A1 C8A1 H7A2 78.7(11) . . ? C9A1 C8A1 H7A2 111.7(15) . . ? C9A2 C8A1 H7A2 125.0(18) . . ? H8A1 C8A1 H7A2 74.4(12) . . ? C8A2 C8A1 H8A2 20(2) . . ? C7A2 C8A1 H8A2 96.2(14) . . ? C7A1 C8A1 H8A2 55.2(10) . . ? C9A1 C8A1 H8A2 102.5(13) . . ? C9A2 C8A1 H8A2 83.4(13) . . ? H8A1 C8A1 H8A2 116.7(16) . . ? H7A2 C8A1 H8A2 133.2(8) . . ? C9A2 C9A1 C8A1 96(3) . . ? C9A2 C9A1 C8A2 70(3) . . ? C8A1 C9A1 C8A2 25.8(10) . . ? C9A2 C9A1 H9A1 132(6) . . ? C8A1 C9A1 H9A1 110.2(17) . . ? C8A2 C9A1 H9A1 128(2) . . ? C9A2 C9A1 H9A2 21(4) . . ? C8A1 C9A1 H9A2 109.2(17) . . ? C8A2 C9A1 H9A2 84.6(14) . . ? H9A1 C9A1 H9A2 110(2) . . ? C9A2 C9A1 H9A3 102(6) . . ? C8A1 C9A1 H9A3 109.3(19) . . ? C8A2 C9A1 H9A3 114(2) . . ? H9A1 C9A1 H9A3 106.1(18) . . ? H9A2 C9A1 H9A3 112(2) . . ? C9A2 C9A1 H9A4 20(4) . . ? C8A1 C9A1 H9A4 107.7(14) . . ? C8A2 C9A1 H9A4 83.0(12) . . ? H9A1 C9A1 H9A4 111.8(18) . . ? H9A2 C9A1 H9A4 1.7(4) . . ? H9A3 C9A1 H9A4 111.8(18) . . ? C9A2 C9A1 H9A5 65(5) . . ? C8A1 C9A1 H9A5 114.2(18) . . ? C8A2 C9A1 H9A5 101.5(18) . . ? H9A1 C9A1 H9A5 129.8(18) . . ? H9A2 C9A1 H9A5 75.7(16) . . ? H9A3 C9A1 H9A5 37.2(9) . . ? H9A4 C9A1 H9A5 75.6(13) . . ? C9A2 C9A1 H9A6 106(6) . . ? C8A1 C9A1 H9A6 119(2) . . ? C8A2 C9A1 H9A6 125(3) . . ? H9A1 C9A1 H9A6 25.9(8) . . ? H9A2 C9A1 H9A6 85(2) . . ? H9A3 C9A1 H9A6 120(2) . . ? H9A4 C9A1 H9A6 86(2) . . ? H9A5 C9A1 H9A6 127(2) . . ? C10B C10A C5A1 53.0(12) . . ? C10B C10A H10A 86.8(16) . . ? C5A1 C10A H10A 108.7(11) . . ? C10B C10A H10B 160.2(16) . . ? C5A1 C10A H10B 110.0(11) . . ? H10A C10A H10B 110.1(15) . . ? C10B C10A H10C 71.5(18) . . ? C5A1 C10A H10C 109.1(12) . . ? H10A C10A H10C 108.2(14) . . ? H10B C10A H10C 110.6(14) . . ? C10B C10A H10D 68(3) . . ? C5A1 C10A H10D 82(2) . . ? H10A C10A H10D 139(4) . . ? H10B C10A H10D 102(3) . . ? H10C C10A H10D 34(2) . . ? C10B C10A H10F 39.0(12) . . ? C5A1 C10A H10F 76.7(6) . . ? H10A C10A H10F 47.9(6) . . ? H10B C10A H10F 156.8(16) . . ? H10C C10A H10F 86.7(11) . . ? H10D C10A H10F 101(4) . . ? C7D2 C7D1 C5D 74.3(9) . . ? C7D2 C7D1 H7D1 101(5) . . ? C5D C7D1 H7D1 116(3) . . ? C7D2 C7D1 H7D2 133(5) . . ? C5D C7D1 H7D2 115(3) . . ? H7D1 C7D1 H7D2 112(3) . . ? C7D2 C7D1 H7D3 38(2) . . ? C5D C7D1 H7D3 107(3) . . ? H7D1 C7D1 H7D3 102(4) . . ? H7D2 C7D1 H7D3 101(3) . . ? C7D2 C7D1 H7D4 58(3) . . ? C5D C7D1 H7D4 106(2) . . ? H7D1 C7D1 H7D4 43.6(17) . . ? H7D2 C7D1 H7D4 138.5(14) . . ? H7D3 C7D1 H7D4 64(3) . . ? C7D2 C7D1 H7D5 63(4) . . ? C5D C7D1 H7D5 110(3) . . ? H7D1 C7D1 H7D5 124(3) . . ? H7D2 C7D1 H7D5 71(2) . . ? H7D3 C7D1 H7D5 32.3(14) . . ? H7D4 C7D1 H7D5 95(4) . . ? C4A2 O122 C4A1 7.6(11) . . ? C4A2 O122 H121 115(2) . . ? C4A1 O122 H121 112(2) . . ? C4A2 O122 H122 117(2) . . ? C4A1 O122 H122 114(2) . . ? H121 O122 H122 1.92(9) . . ? C4A1 C2A2 C4A2 11.1(11) . . ? C4A1 C2A2 N1 121(3) . . ? C4A2 C2A2 N1 120(2) . . ? C4A1 C2A2 C3A 124(2) . . ? C4A2 C2A2 C3A 115.0(18) . . ? N1 C2A2 C3A 100.3(15) . . ? C4A1 C2A2 H2A1 122(3) . . ? C4A2 C2A2 H2A1 132(2) . . ? N1 C2A2 H2A1 90.9(17) . . ? C3A C2A2 H2A1 91.6(16) . . ? C4A1 C2A2 H2A2 100(3) . . ? C4A2 C2A2 H2A2 110(2) . . ? N1 C2A2 H2A2 102(2) . . ? C3A C2A2 H2A2 108(2) . . ? H2A1 C2A2 H2A2 21.7(6) . . ? O121 C4A2 O122 3(2) . . ? O121 C4A2 C5A2 109.5(19) . . ? O122 C4A2 C5A2 107.9(13) . . ? O121 C4A2 C2A2 111(2) . . ? O122 C4A2 C2A2 113.8(16) . . ? C5A2 C4A2 C2A2 116.6(14) . . ? O121 C4A2 C5A1 125(2) . . ? O122 C4A2 C5A1 124.9(17) . . ? C5A2 C4A2 C5A1 24.5(6) . . ? C2A2 C4A2 C5A1 92.2(15) . . ? O121 C4A2 C2A1 110.2(19) . . ? O122 C4A2 C2A1 113.4(18) . . ? C5A2 C4A2 C2A1 116.2(13) . . ? C2A2 C4A2 C2A1 1(2) . . ? C5A1 C4A2 C2A1 91.9(13) . . ? O121 C4A2 H4A1 133(3) . . ? O122 C4A2 H4A1 132(2) . . ? C5A2 C4A2 H4A1 101.0(11) . . ? C2A2 C4A2 H4A1 84.4(17) . . ? C5A1 C4A2 H4A1 96.4(12) . . ? C2A1 C4A2 H4A1 85.4(13) . . ? O121 C4A2 H4A2 113(3) . . ? O122 C4A2 H4A2 111(2) . . ? C5A2 C4A2 H4A2 105.7(13) . . ? C2A2 C4A2 H4A2 101.7(19) . . ? C5A1 C4A2 H4A2 110.0(15) . . ? C2A1 C4A2 H4A2 102.6(16) . . ? H4A1 C4A2 H4A2 22.6(6) . . ? C5A1 C5A2 C6A1 124(2) . . ? C5A1 C5A2 C6A2 160.3(17) . . ? C6A1 C5A2 C6A2 37.1(10) . . ? C5A1 C5A2 C10B 51.3(18) . . ? C6A1 C5A2 C10B 77.4(12) . . ? C6A2 C5A2 C10B 112.8(7) . . ? C5A1 C5A2 C4A2 86.9(17) . . ? C6A1 C5A2 C4A2 139.6(14) . . ? C6A2 C5A2 C4A2 111.7(7) . . ? C10B C5A2 C4A2 112.3(7) . . ? C5A1 C5A2 C4A1 72.0(14) . . ? C6A1 C5A2 C4A1 147(2) . . ? C6A2 C5A2 C4A1 126.0(11) . . ? C10B C5A2 C4A1 98.9(10) . . ? C4A2 C5A2 C4A1 15.5(9) . . ? C5A1 C5A2 H5A1 50.4(17) . . ? C6A1 C5A2 H5A1 122.4(15) . . ? C6A2 C5A2 H5A1 129.0(12) . . ? C10B C5A2 H5A1 92.0(12) . . ? C4A2 C5A2 H5A1 97.1(12) . . ? C4A1 C5A2 H5A1 90.2(10) . . ? C5A1 C5A2 H6A1 168(2) . . ? C6A1 C5A2 H6A1 44.7(9) . . ? C6A2 C5A2 H6A1 10.0(6) . . ? C10B C5A2 H6A1 116.9(10) . . ? C4A2 C5A2 H6A1 101.9(8) . . ? C4A1 C5A2 H6A1 116.0(12) . . ? H5A1 C5A2 H6A1 135.1(12) . . ? C5A1 C5A2 H5A2 71(2) . . ? C6A1 C5A2 H5A2 106.7(15) . . ? C6A2 C5A2 H5A2 107.1(12) . . ? C10B C5A2 H5A2 104.2(14) . . ? C4A2 C5A2 H5A2 108.3(14) . . ? C4A1 C5A2 H5A2 105.9(13) . . ? H5A1 C5A2 H5A2 22.0(4) . . ? H6A1 C5A2 H5A2 113.3(12) . . ? C6A1 C6A2 C7A2 86.1(13) . . ? C6A1 C6A2 C5A2 42.0(11) . . ? C7A2 C6A2 C5A2 114.7(7) . . ? C6A1 C6A2 C7A1 54.3(9) . . ? C7A2 C6A2 C7A1 33.4(8) . . ? C5A2 C6A2 C7A1 82.4(8) . . ? C6A1 C6A2 H6A1 92(4) . . ? C7A2 C6A2 H6A1 172(4) . . ? C5A2 C6A2 H6A1 60(3) . . ? C7A1 C6A2 H6A1 142(4) . . ? C6A1 C6A2 H6A2 37.8(13) . . ? C7A2 C6A2 H6A2 93.9(12) . . ? C5A2 C6A2 H6A2 69.1(8) . . ? C7A1 C6A2 H6A2 74.2(9) . . ? H6A1 C6A2 H6A2 89(4) . . ? C6A1 C6A2 H6A3 149(2) . . ? C7A2 C6A2 H6A3 110.9(16) . . ? C5A2 C6A2 H6A3 107.0(13) . . ? C7A1 C6A2 H6A3 132.3(17) . . ? H6A1 C6A2 H6A3 67(4) . . ? H6A2 C6A2 H6A3 153.3(14) . . ? C6A1 C6A2 H6A4 91(2) . . ? C7A2 C6A2 H6A4 111.5(15) . . ? C5A2 C6A2 H6A4 106.4(13) . . ? C7A1 C6A2 H6A4 116.2(16) . . ? H6A1 C6A2 H6A4 76(4) . . ? H6A2 C6A2 H6A4 53.5(10) . . ? H6A3 C6A2 H6A4 105.9(14) . . ? C8A1 C7A2 C7A1 84.3(16) . . ? C8A1 C7A2 C8A2 30.6(14) . . ? C7A1 C7A2 C8A2 54.8(16) . . ? C8A1 C7A2 C6A2 142(2) . . ? C7A1 C7A2 C6A2 92.2(11) . . ? C8A2 C7A2 C6A2 125.9(9) . . ? C8A1 C7A2 C6A1 136.2(18) . . ? C7A1 C7A2 C6A1 61.0(9) . . ? C8A2 C7A2 C6A1 107.2(13) . . ? C6A2 C7A2 C6A1 32.7(7) . . ? C8A1 C7A2 H8A1 54.1(16) . . ? C7A1 C7A2 H8A1 129(2) . . ? C8A2 C7A2 H8A1 77.4(18) . . ? C6A2 C7A2 H8A1 103.4(16) . . ? C6A1 C7A2 H8A1 129.4(15) . . ? C8A1 C7A2 H7A2 99.3(18) . . ? C7A1 C7A2 H7A2 128(3) . . ? C8A2 C7A2 H7A2 122.1(14) . . ? C6A2 C7A2 H7A2 112.0(14) . . ? C6A1 C7A2 H7A2 122.5(17) . . ? H8A1 C7A2 H7A2 91.0(16) . . ? C8A1 C8A2 C7A1 92(2) . . ? C8A1 C8A2 C7A2 44.7(16) . . ? C7A1 C8A2 C7A2 48.3(13) . . ? C8A1 C8A2 C9A2 87(2) . . ? C7A1 C8A2 C9A2 138(3) . . ? C7A2 C8A2 C9A2 125.5(17) . . ? C8A1 C8A2 C9A1 67(2) . . ? C7A1 C8A2 C9A1 134(2) . . ? C7A2 C8A2 C9A1 107.0(16) . . ? C9A2 C8A2 C9A1 20.0(13) . . ? C8A1 C8A2 H7A1 117(3) . . ? C7A1 C8A2 H7A1 36.4(12) . . ? C7A2 C8A2 H7A1 80.8(18) . . ? C9A2 C8A2 H7A1 109(2) . . ? C9A1 C8A2 H7A1 117(2) . . ? C8A1 C8A2 H8A1 26(2) . . ? C7A1 C8A2 H8A1 93.7(14) . . ? C7A2 C8A2 H8A1 47.2(14) . . ? C9A2 C8A2 H8A1 103.0(18) . . ? C9A1 C8A2 H8A1 84.4(14) . . ? H7A1 C8A2 H8A1 128.0(13) . . ? C8A1 C8A2 H8A2 144(4) . . ? C7A1 C8A2 H8A2 82(2) . . ? C7A2 C8A2 H8A2 114.3(16) . . ? C9A2 C8A2 H8A2 120.2(19) . . ? C9A1 C8A2 H8A2 138(2) . . ? H7A1 C8A2 H8A2 77(2) . . ? H8A1 C8A2 H8A2 119(2) . . ? C9A1 C9A2 C8A2 90(3) . . ? C9A1 C9A2 C8A1 64(3) . . ? C8A2 C9A2 C8A1 25.3(10) . . ? C9A1 C9A2 H9A1 31(4) . . ? C8A2 C9A2 H9A1 107(2) . . ? C8A1 C9A2 H9A1 83.9(15) . . ? C9A1 C9A2 H9A2 132(8) . . ? C8A2 C9A2 H9A2 119(4) . . ? C8A1 C9A2 H9A2 136(5) . . ? H9A1 C9A2 H9A2 101(5) . . ? C9A1 C9A2 H9A3 52(5) . . ? C8A2 C9A2 H9A3 106(2) . . ? C8A1 C9A2 H9A3 89.3(17) . . ? H9A1 C9A2 H9A3 72.6(15) . . ? H9A2 C9A2 H9A3 134(4) . . ? C9A1 C9A2 H9A4 149(7) . . ? C8A2 C9A2 H9A4 109(2) . . ? C8A1 C9A2 H9A4 131(2) . . ? H9A1 C9A2 H9A4 117(3) . . ? H9A2 C9A2 H9A4 17(2) . . ? H9A3 C9A2 H9A4 138(3) . . ? C9A1 C9A2 H9A5 83(6) . . ? C8A2 C9A2 H9A5 114(3) . . ? C8A1 C9A2 H9A5 108(2) . . ? H9A1 C9A2 H9A5 100(2) . . ? H9A2 C9A2 H9A5 114(4) . . ? H9A3 C9A2 H9A5 32.0(10) . . ? H9A4 C9A2 H9A5 110(3) . . ? C9A1 C9A2 H9A6 42(4) . . ? C8A2 C9A2 H9A6 111(2) . . ? C8A1 C9A2 H9A6 89.9(19) . . ? H9A1 C9A2 H9A6 10.6(6) . . ? H9A2 C9A2 H9A6 90(5) . . ? H9A3 C9A2 H9A6 81(2) . . ? H9A4 C9A2 H9A6 107(3) . . ? H9A5 C9A2 H9A6 107(3) . . ? C10A C10B C5A1 85.1(17) . . ? C10A C10B C5A2 110.9(17) . . ? C5A1 C10B C5A2 25.8(8) . . ? C10A C10B C6A1 142(2) . . ? C5A1 C10B C6A1 62.2(8) . . ? C5A2 C10B C6A1 38.0(7) . . ? C10A C10B H10A 45.1(12) . . ? C5A1 C10B H10A 104.7(19) . . ? C5A2 C10B H10A 122.4(16) . . ? C6A1 C10B H10A 123.1(16) . . ? C10A C10B H10C 52.1(13) . . ? C5A1 C10B H10C 119.0(17) . . ? C5A2 C10B H10C 137.1(13) . . ? C6A1 C10B H10C 161(2) . . ? H10A C10B H10C 76.1(11) . . ? C10A C10B H10D 15.0(10) . . ? C5A1 C10B H10D 87.0(16) . . ? C5A2 C10B H10D 112.1(14) . . ? C6A1 C10B H10D 148.9(18) . . ? H10A C10B H10D 58.1(12) . . ? H10C C10B H10D 40.7(7) . . ? C10A C10B H10E 120(2) . . ? C5A1 C10B H10E 124.1(18) . . ? C5A2 C10B H10E 108.6(15) . . ? C6A1 C10B H10E 94.8(16) . . ? H10A C10B H10E 128.9(13) . . ? H10C C10B H10E 68.0(12) . . ? H10D C10B H10E 106.6(19) . . ? C10A C10B H10F 99(2) . . ? C5A1 C10B H10F 119(2) . . ? C5A2 C10B H10F 111.8(14) . . ? C6A1 C10B H10F 83.3(14) . . ? H10A C10B H10F 53.5(11) . . ? H10C C10B H10F 109.8(13) . . ? H10D C10B H10F 111(2) . . ? H10E C10B H10F 106.7(19) . . ? C7D1 C7D2 C5D 73.7(9) . . ? C7D1 C7D2 H7D1 42(3) . . ? C5D C7D2 H7D1 93.2(10) . . ? C7D1 C7D2 H7D3 91(3) . . ? C5D C7D2 H7D3 146(2) . . ? H7D1 C7D2 H7D3 95.0(18) . . ? C7D1 C7D2 H7D4 75(3) . . ? C5D C7D2 H7D4 114.0(13) . . ? H7D1 C7D2 H7D4 33.0(7) . . ? H7D3 C7D2 H7D4 89.4(15) . . ? C7D1 C7D2 H7D5 68(3) . . ? C5D C7D2 H7D5 112.3(13) . . ? H7D1 C7D2 H7D5 93.5(15) . . ? H7D3 C7D2 H7D5 34.7(9) . . ? H7D4 C7D2 H7D5 106.9(16) . . ? C7D1 C7D2 H7D6 173(3) . . ? C5D C7D2 H7D6 110.5(14) . . ? H7D1 C7D2 H7D6 140.5(14) . . ? H7D3 C7D2 H7D6 82.6(16) . . ? H7D4 C7D2 H7D6 107.5(15) . . ? H7D5 C7D2 H7D6 105.2(14) . . ? 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 C1B N2 C3A O1 -9.1(14) . . . . ? C1B N2 C3A C2A1 174.0(11) . . . . ? C1B N2 C3A C2A2 164.1(13) . . . . ? C3A N2 C1B C2B -77.7(10) . . . . ? C3A N2 C1B C3B 162.5(8) . . . . ? C2C N3 C2B O2 -3.2(12) . . . . ? C1C N3 C2B O2 175.5(8) . . . . ? C2C N3 C2B C1B 172.6(7) . . . . ? C1C N3 C2B C1B -8.8(12) . . . . ? N2 C1B C2B O2 -20.8(11) . . . . ? C3B C1B C2B O2 99.4(9) . . . . ? N2 C1B C2B N3 163.4(7) . . . . ? C3B C1B C2B N3 -76.5(9) . . . . ? N2 C1B C3B C4B -63.7(10) . . . . ? C2B C1B C3B C4B 175.0(8) . . . . ? C2B N3 C2C C3C 97.6(8) . . . . ? C1C N3 C2C C3C -81.2(8) . . . . ? C1D N4 C3C O3 -172.2(8) . . . . ? C2D N4 C3C O3 -8.4(11) . . . . ? C1D N4 C3C C2C 8.1(11) . . . . ? C2D N4 C3C C2C 172.0(6) . . . . ? N3 C2C C3C O3 -5.7(11) . . . . ? N3 C2C C3C N4 173.9(6) . . . . ? C3C N4 C2D C3D -92.6(8) . . . . ? C1D N4 C2D C3D 71.7(8) . . . . ? C3C N4 C2D C4D 144.4(7) . . . . ? C1D N4 C2D C4D -51.3(10) . . . . ? C1E N5 C3D O4 9.7(12) . . . . ? C1E N5 C3D C2D -166.7(6) . . . . ? N4 C2D C3D O4 -81.4(9) . . . . ? C4D C2D C3D O4 42.6(11) . . . . ? N4 C2D C3D N5 95.1(8) . . . . ? C4D C2D C3D N5 -140.9(7) . . . . ? N4 C2D C4D C5D -67.4(10) . . . . ? C3D C2D C4D C5D 171.6(7) . . . . ? C2D C4D C5D C7D1 -50(2) . . . . ? C2D C4D C5D C7D2 -83.5(12) . . . . ? C2D C4D C5D C6D 162.2(9) . . . . ? C3D N5 C1E C2E -141.4(7) . . . . ? C3D N5 C1E C3E 98.1(8) . . . . ? C2F N6 C2E O5 -5.5(10) . . . . ? C1F N6 C2E O5 171.0(7) . . . . ? C2F N6 C2E C1E 168.3(6) . . . . ? C1F N6 C2E C1E -15.3(11) . . . . ? N5 C1E C2E O5 -24.6(9) . . . . ? C3E C1E C2E O5 97.3(8) . . . . ? N5 C1E C2E N6 161.7(6) . . . . ? C3E C1E C2E N6 -76.4(8) . . . . ? N5 C1E C3E C5E 60.9(9) . . . . ? C2E C1E C3E C5E -59.7(9) . . . . ? N5 C1E C3E C4E -64.2(9) . . . . ? C2E C1E C3E C4E 175.2(7) . . . . ? C2E N6 C2F C4F -72.8(9) . . . . ? C1F N6 C2F C4F 110.4(8) . . . . ? C2E N6 C2F C3F 58.1(9) . . . . ? C1F N6 C2F C3F -118.6(7) . . . . ? C1G N7 C3F O6 1.0(11) . . . . ? C1G N7 C3F C2F -178.1(7) . . . . ? N6 C2F C3F O6 50.1(10) . . . . ? C4F C2F C3F O6 178.7(7) . . . . ? N6 C2F C3F N7 -130.7(7) . . . . ? C4F C2F C3F N7 -2.1(10) . . . . ? N6 C2F C4F C5F -60.0(9) . . . . ? C3F C2F C4F C5F 173.6(7) . . . . ? C2F C4F C5F C7F 173.0(9) . . . . ? C2F C4F C5F C6F -60.5(12) . . . . ? C3F N7 C1G C2G -75.3(9) . . . . ? C3F N7 C1G C3G 159.6(7) . . . . ? C1H N8 C2G O7 -9.8(12) . . . . ? C1H N8 C2G C1G 171.9(6) . . . . ? N7 C1G C2G O7 172.4(8) . . . . ? C3G C1G C2G O7 -62.6(11) . . . . ? N7 C1G C2G N8 -9.2(11) . . . . ? C3G C1G C2G N8 115.8(8) . . . . ? C2G N8 C1H C3H -93.5(8) . . . . ? C2G N8 C1H C2H 143.4(7) . . . . ? C1I N9 C2H O8 176.8(7) . . . . ? C2I N9 C2H O8 -1.3(10) . . . . ? C1I N9 C2H C1H -6.1(10) . . . . ? C2I N9 C2H C1H 175.8(6) . . . . ? N8 C1H C2H O8 100.8(7) . . . . ? C3H C1H C2H O8 -22.4(9) . . . . ? N8 C1H C2H N9 -76.4(7) . . . . ? C3H C1H C2H N9 160.4(6) . . . . ? C2H N9 C2I C3I -129.3(7) . . . . ? C1I N9 C2I C3I 52.5(8) . . . . ? C2H N9 C2I C4I 106.9(7) . . . . ? C1I N9 C2I C4I -71.4(8) . . . . ? C2J N10 C3I O9 10.2(12) . . . . ? C1J N10 C3I O9 178.6(8) . . . . ? C2J N10 C3I C2I -166.7(7) . . . . ? C1J N10 C3I C2I 1.6(11) . . . . ? N9 C2I C3I O9 -113.4(8) . . . . ? C4I C2I C3I O9 10.4(11) . . . . ? N9 C2I C3I N10 63.6(9) . . . . ? C4I C2I C3I N10 -172.5(7) . . . . ? N9 C2I C4I C5I -64.9(10) . . . . ? C3I C2I C4I C5I 172.3(8) . . . . ? C2I C4I C5I C7I -74.9(11) . . . . ? C2I C4I C5I C6I 161.3(9) . . . . ? C3I N10 C2J C3J -144.9(7) . . . . ? C1J N10 C2J C3J 45.7(10) . . . . ? C3I N10 C2J C4J 87.4(10) . . . . ? C1J N10 C2J C4J -82.0(10) . . . . ? C1K N11 C3J O10 179.4(8) . . . . ? C2K N11 C3J O10 -4.5(12) . . . . ? C1K N11 C3J C2J -2.5(12) . . . . ? C2K N11 C3J C2J 173.6(7) . . . . ? N10 C2J C3J O10 -97.9(9) . . . . ? C4J C2J C3J O10 26.0(11) . . . . ? N10 C2J C3J N11 84.0(9) . . . . ? C4J C2J C3J N11 -152.1(8) . . . . ? N10 C2J C4J C5J -162.2(10) . . . . ? C3J C2J C4J C5J 71.7(13) . . . . ? C2J C4J C5J C7J 68.0(14) . . . . ? C2J C4J C5J C6J -179.2(11) . . . . ? C3J N11 C2K C3K 133.1(8) . . . . ? C1K N11 C2K C3K -50.6(10) . . . . ? C3J N11 C2K C4K -100.8(9) . . . . ? C1K N11 C2K C4K 75.5(10) . . . . ? C2A1 N1 C3K O11 -8.8(14) . . . . ? C1A N1 C3K O11 -166.8(8) . . . . ? C2A2 N1 C3K O11 -2.2(17) . . . . ? C2A1 N1 C3K C2K 173.5(11) . . . . ? C1A N1 C3K C2K 15.4(12) . . . . ? C2A2 N1 C3K C2K -179.9(13) . . . . ? N11 C2K C3K O11 99.8(9) . . . . ? C4K C2K C3K O11 -25.5(12) . . . . ? N11 C2K C3K N1 -82.5(10) . . . . ? C4K C2K C3K N1 152.3(8) . . . . ? N11 C2K C4K C6K 51.3(11) . . . . ? C3K C2K C4K C6K 175.1(9) . . . . ? N11 C2K C4K C5K 175.7(8) . . . . ? C3K C2K C4K C5K -60.5(11) . . . . ? C3K N1 C2A1 C3A -93.0(15) . . . . ? C1A N1 C2A1 C3A 65.3(15) . . . . ? C2A2 N1 C2A1 C3A 116(10) . . . . ? C3K N1 C2A1 C4A1 142.8(11) . . . . ? C1A N1 C2A1 C4A1 -58.8(17) . . . . ? C2A2 N1 C2A1 C4A1 -8(9) . . . . ? C3K N1 C2A1 C4A2 152.1(11) . . . . ? C1A N1 C2A1 C4A2 -49.6(17) . . . . ? C2A2 N1 C2A1 C4A2 1(9) . . . . ? O1 C3A C2A1 N1 9.9(18) . . . . ? N2 C3A C2A1 N1 -173.0(10) . . . . ? C2A2 C3A C2A1 N1 -123(11) . . . . ? O1 C3A C2A1 C4A1 134.7(13) . . . . ? N2 C3A C2A1 C4A1 -48.2(19) . . . . ? C2A2 C3A C2A1 C4A1 1(9) . . . . ? O1 C3A C2A1 C4A2 129.0(14) . . . . ? N2 C3A C2A1 C4A2 -53.9(18) . . . . ? C2A2 C3A C2A1 C4A2 -4(9) . . . . ? C4A2 O121 C4A1 C2A2 169(11) . . . . ? C4A2 O121 C4A1 C5A1 -66(9) . . . . ? C4A2 O121 C4A1 C2A1 170(10) . . . . ? C4A2 O121 C4A1 C5A2 -51(9) . . . . ? C4A2 O121 C4A1 O122 13(100) . . . . ? N1 C2A1 C4A1 C2A2 117(65) . . . . ? C3A C2A1 C4A1 C2A2 -10(63) . . . . ? C4A2 C2A1 C4A1 C2A2 30(64) . . . . ? N1 C2A1 C4A1 O121 80.8(18) . . . . ? C3A C2A1 C4A1 O121 -46(2) . . . . ? C4A2 C2A1 C4A1 O121 -6(7) . . . . ? N1 C2A1 C4A1 C5A1 -41.8(18) . . . . ? C3A C2A1 C4A1 C5A1 -168.6(13) . . . . ? C4A2 C2A1 C4A1 C5A1 -129(8) . . . . ? N1 C2A1 C4A1 C5A2 -32(3) . . . . ? C3A C2A1 C4A1 C5A2 -158.5(17) . . . . ? C4A2 C2A1 C4A1 C5A2 -119(9) . . . . ? N1 C2A1 C4A1 O122 81.0(19) . . . . ? C3A C2A1 C4A1 O122 -46(2) . . . . ? C4A2 C2A1 C4A1 O122 -6(7) . . . . ? C2A2 C4A1 C5A1 C5A2 162(3) . . . . ? O121 C4A1 C5A1 C5A2 39(2) . . . . ? C2A1 C4A1 C5A1 C5A2 163(2) . . . . ? O122 C4A1 C5A1 C5A2 39(2) . . . . ? C2A2 C4A1 C5A1 C10B -97(3) . . . . ? O121 C4A1 C5A1 C10B 140.0(17) . . . . ? C2A1 C4A1 C5A1 C10B -96.2(17) . . . . ? C5A2 C4A1 C5A1 C10B 101(2) . . . . ? O122 C4A1 C5A1 C10B 139.4(19) . . . . ? C2A2 C4A1 C5A1 C10A -51(2) . . . . ? O121 C4A1 C5A1 C10A -173.6(14) . . . . ? C2A1 C4A1 C5A1 C10A -49.8(15) . . . . ? C5A2 C4A1 C5A1 C10A 147(2) . . . . ? O122 C4A1 C5A1 C10A -174.2(17) . . . . ? C2A2 C4A1 C5A1 C6A1 -179(2) . . . . ? O121 C4A1 C5A1 C6A1 58.3(15) . . . . ? C2A1 C4A1 C5A1 C6A1 -177.9(13) . . . . ? C5A2 C4A1 C5A1 C6A1 19.2(18) . . . . ? O122 C4A1 C5A1 C6A1 57.7(18) . . . . ? C2A2 C4A1 C5A1 C4A2 147(7) . . . . ? O121 C4A1 C5A1 C4A2 24(5) . . . . ? C2A1 C4A1 C5A1 C4A2 148(6) . . . . ? C5A2 C4A1 C5A1 C4A2 -15(5) . . . . ? O122 C4A1 C5A1 C4A2 24(5) . . . . ? C5A2 C5A1 C6A1 C6A2 -6(3) . . . . ? C10B C5A1 C6A1 C6A2 -156(2) . . . . ? C10A C5A1 C6A1 C6A2 -169.9(19) . . . . ? C4A1 C5A1 C6A1 C6A2 -42(2) . . . . ? C4A2 C5A1 C6A1 C6A2 -33(2) . . . . ? C10B C5A1 C6A1 C5A2 -150(4) . . . . ? C10A C5A1 C6A1 C5A2 -163(4) . . . . ? C4A1 C5A1 C6A1 C5A2 -35(3) . . . . ? C4A2 C5A1 C6A1 C5A2 -27(3) . . . . ? C5A2 C5A1 C6A1 C7A1 -119(3) . . . . ? C10B C5A1 C6A1 C7A1 90.8(16) . . . . ? C10A C5A1 C6A1 C7A1 77.2(13) . . . . ? C4A1 C5A1 C6A1 C7A1 -154.5(11) . . . . ? C4A2 C5A1 C6A1 C7A1 -146.1(15) . . . . ? C5A2 C5A1 C6A1 C10B 150(4) . . . . ? C10A C5A1 C6A1 C10B -13.6(14) . . . . ? C4A1 C5A1 C6A1 C10B 114.7(16) . . . . ? C4A2 C5A1 C6A1 C10B 123.1(18) . . . . ? C5A2 C5A1 C6A1 C7A2 -89(4) . . . . ? C10B C5A1 C6A1 C7A2 122(2) . . . . ? C10A C5A1 C6A1 C7A2 108.0(19) . . . . ? C4A1 C5A1 C6A1 C7A2 -123.6(18) . . . . ? C4A2 C5A1 C6A1 C7A2 -115(2) . . . . ? C6A2 C6A1 C7A1 C7A2 16(2) . . . . ? C5A2 C6A1 C7A1 C7A2 123(2) . . . . ? C5A1 C6A1 C7A1 C7A2 145.1(18) . . . . ? C10B C6A1 C7A1 C7A2 -168(2) . . . . ? C6A2 C6A1 C7A1 C8A2 -45(3) . . . . ? C5A2 C6A1 C7A1 C8A2 62(3) . . . . ? C5A1 C6A1 C7A1 C8A2 84(3) . . . . ? C10B C6A1 C7A1 C8A2 131(3) . . . . ? C7A2 C6A1 C7A1 C8A2 -61(2) . . . . ? C6A2 C6A1 C7A1 C8A1 -7(2) . . . . ? C5A2 C6A1 C7A1 C8A1 99(2) . . . . ? C5A1 C6A1 C7A1 C8A1 121.4(18) . . . . ? C10B C6A1 C7A1 C8A1 168.9(19) . . . . ? C7A2 C6A1 C7A1 C8A1 -23.6(17) . . . . ? C5A2 C6A1 C7A1 C6A2 106(2) . . . . ? C5A1 C6A1 C7A1 C6A2 129(2) . . . . ? C10B C6A1 C7A1 C6A2 176(2) . . . . ? C7A2 C6A1 C7A1 C6A2 -16(2) . . . . ? C7A2 C7A1 C8A1 C8A2 -164(5) . . . . ? C6A1 C7A1 C8A1 C8A2 -130(3) . . . . ? C6A2 C7A1 C8A1 C8A2 -134(3) . . . . ? C8A2 C7A1 C8A1 C7A2 164(5) . . . . ? C6A1 C7A1 C8A1 C7A2 33(2) . . . . ? C6A2 C7A1 C8A1 C7A2 29.8(18) . . . . ? C7A2 C7A1 C8A1 C9A1 140(3) . . . . ? C8A2 C7A1 C8A1 C9A1 -56(3) . . . . ? C6A1 C7A1 C8A1 C9A1 173.8(17) . . . . ? C6A2 C7A1 C8A1 C9A1 170(2) . . . . ? C7A2 C7A1 C8A1 C9A2 155(3) . . . . ? C8A2 C7A1 C8A1 C9A2 -42(3) . . . . ? C6A1 C7A1 C8A1 C9A2 -171.6(17) . . . . ? C6A2 C7A1 C8A1 C9A2 -175.3(18) . . . . ? C8A2 C8A1 C9A1 C9A2 1(6) . . . . ? C7A2 C8A1 C9A1 C9A2 114(7) . . . . ? C7A1 C8A1 C9A1 C9A2 45(7) . . . . ? C7A2 C8A1 C9A1 C8A2 114(5) . . . . ? C7A1 C8A1 C9A1 C8A2 44(3) . . . . ? C9A2 C8A1 C9A1 C8A2 -1(6) . . . . ? C5A2 C5A1 C10A C10B 3(3) . . . . ? C4A1 C5A1 C10A C10B -108(2) . . . . ? C6A1 C5A1 C10A C10B 19.7(19) . . . . ? C4A2 C5A1 C10A C10B -103(2) . . . . ? C4D C5D C7D1 C7D2 -81(3) . . . . ? C6D C5D C7D1 C7D2 64(3) . . . . ? C2A2 C4A1 O122 C4A2 169(10) . . . . ? O121 C4A1 O122 C4A2 -167(100) . . . . ? C5A1 C4A1 O122 C4A2 -66(8) . . . . ? C2A1 C4A1 O122 C4A2 170(9) . . . . ? C5A2 C4A1 O122 C4A2 -51(8) . . . . ? O121 C4A1 C2A2 C4A2 -7(8) . . . . ? C5A1 C4A1 C2A2 C4A2 -130(9) . . . . ? C2A1 C4A1 C2A2 C4A2 -151(61) . . . . ? C5A2 C4A1 C2A2 C4A2 -119(10) . . . . ? O122 C4A1 C2A2 C4A2 -7(7) . . . . ? O121 C4A1 C2A2 N1 84(3) . . . . ? C5A1 C4A1 C2A2 N1 -38(3) . . . . ? C2A1 C4A1 C2A2 N1 -60(63) . . . . ? C5A2 C4A1 C2A2 N1 -27(5) . . . . ? O122 C4A1 C2A2 N1 85(3) . . . . ? O121 C4A1 C2A2 C3A -46(4) . . . . ? C5A1 C4A1 C2A2 C3A -169(2) . . . . ? C2A1 C4A1 C2A2 C3A 170(67) . . . . ? C5A2 C4A1 C2A2 C3A -157.9(18) . . . . ? O122 C4A1 C2A2 C3A -46(4) . . . . ? C3K N1 C2A2 C4A1 136(2) . . . . ? C2A1 N1 C2A2 C4A1 169(12) . . . . ? C1A N1 C2A2 C4A1 -58(3) . . . . ? C3K N1 C2A2 C4A2 149.2(16) . . . . ? C2A1 N1 C2A2 C4A2 -178(11) . . . . ? C1A N1 C2A2 C4A2 -45(2) . . . . ? C3K N1 C2A2 C3A -83.6(18) . . . . ? C2A1 N1 C2A2 C3A -51(9) . . . . ? C1A N1 C2A2 C3A 82.2(14) . . . . ? O1 C3A C2A2 C4A1 130(3) . . . . ? N2 C3A C2A2 C4A1 -43(4) . . . . ? C2A1 C3A C2A2 C4A1 -178(13) . . . . ? O1 C3A C2A2 C4A2 122(2) . . . . ? N2 C3A C2A2 C4A2 -51(3) . . . . ? C2A1 C3A C2A2 C4A2 174(12) . . . . ? O1 C3A C2A2 N1 -8(2) . . . . ? N2 C3A C2A2 N1 178.5(11) . . . . ? C2A1 C3A C2A2 N1 44(9) . . . . ? C4A1 O121 C4A2 O122 -177(100) . . . . ? C4A1 O121 C4A2 C5A2 121(10) . . . . ? C4A1 O121 C4A2 C2A2 -9(8) . . . . ? C4A1 O121 C4A2 C5A1 100(11) . . . . ? C4A1 O121 C4A2 C2A1 -8(8) . . . . ? C4A1 O122 C4A2 O121 3(42) . . . . ? C4A1 O122 C4A2 C5A2 122(10) . . . . ? C4A1 O122 C4A2 C2A2 -9(8) . . . . ? C4A1 O122 C4A2 C5A1 102(10) . . . . ? C4A1 O122 C4A2 C2A1 -8(8) . . . . ? C4A1 C2A2 C4A2 O121 170(10) . . . . ? N1 C2A2 C4A2 O121 75(3) . . . . ? C3A C2A2 C4A2 O121 -45(3) . . . . ? C4A1 C2A2 C4A2 O122 171(9) . . . . ? N1 C2A2 C4A2 O122 76(3) . . . . ? C3A C2A2 C4A2 O122 -44(3) . . . . ? C4A1 C2A2 C4A2 C5A2 44(8) . . . . ? N1 C2A2 C4A2 C5A2 -51(3) . . . . ? C3A C2A2 C4A2 C5A2 -170.8(18) . . . . ? C4A1 C2A2 C4A2 C5A1 41(7) . . . . ? N1 C2A2 C4A2 C5A1 -54(2) . . . . ? C3A C2A2 C4A2 C5A1 -174(2) . . . . ? C4A1 C2A2 C4A2 C2A1 110(100) . . . . ? N1 C2A2 C4A2 C2A1 15(100) . . . . ? C3A C2A2 C4A2 C2A1 -105(100) . . . . ? C5A2 C5A1 C4A2 O121 55(4) . . . . ? C10B C5A1 C4A2 O121 147(3) . . . . ? C10A C5A1 C4A2 O121 -161(2) . . . . ? C4A1 C5A1 C4A2 O121 -141(8) . . . . ? C6A1 C5A1 C4A2 O121 71(3) . . . . ? C5A2 C5A1 C4A2 O122 51(3) . . . . ? C10B C5A1 C4A2 O122 143(2) . . . . ? C10A C5A1 C4A2 O122 -165.0(19) . . . . ? C4A1 C5A1 C4A2 O122 -145(7) . . . . ? C6A1 C5A1 C4A2 O122 67(2) . . . . ? C10B C5A1 C4A2 C5A2 91(2) . . . . ? C10A C5A1 C4A2 C5A2 143(3) . . . . ? C4A1 C5A1 C4A2 C5A2 164(5) . . . . ? C6A1 C5A1 C4A2 C5A2 15.9(17) . . . . ? C5A2 C5A1 C4A2 C2A2 173(2) . . . . ? C10B C5A1 C4A2 C2A2 -96(2) . . . . ? C10A C5A1 C4A2 C2A2 -44(2) . . . . ? C4A1 C5A1 C4A2 C2A2 -23(5) . . . . ? C6A1 C5A1 C4A2 C2A2 -171.3(15) . . . . ? C5A2 C5A1 C4A2 C2A1 172(2) . . . . ? C10B C5A1 C4A2 C2A1 -96.7(19) . . . . ? C10A C5A1 C4A2 C2A1 -45(2) . . . . ? C4A1 C5A1 C4A2 C2A1 -24(5) . . . . ? C6A1 C5A1 C4A2 C2A1 -172.2(12) . . . . ? N1 C2A1 C4A2 O121 75(3) . . . . ? C3A C2A1 C4A2 O121 -47(3) . . . . ? C4A1 C2A1 C4A2 O121 171(9) . . . . ? N1 C2A1 C4A2 O122 76(2) . . . . ? C3A C2A1 C4A2 O122 -46(2) . . . . ? C4A1 C2A1 C4A2 O122 172(8) . . . . ? N1 C2A1 C4A2 C5A2 -50(2) . . . . ? C3A C2A1 C4A2 C5A2 -171.8(13) . . . . ? C4A1 C2A1 C4A2 C5A2 46(7) . . . . ? N1 C2A1 C4A2 C2A2 -165(100) . . . . ? C3A C2A1 C4A2 C2A2 73(100) . . . . ? C4A1 C2A1 C4A2 C2A2 -69(100) . . . . ? N1 C2A1 C4A2 C5A1 -53.5(18) . . . . ? C3A C2A1 C4A2 C5A1 -175.5(14) . . . . ? C4A1 C2A1 C4A2 C5A1 43(7) . . . . ? C10B C5A1 C5A2 C6A1 30(4) . . . . ? C10A C5A1 C5A2 C6A1 27(5) . . . . ? C4A1 C5A1 C5A2 C6A1 147(3) . . . . ? C4A2 C5A1 C5A2 C6A1 152(3) . . . . ? C10B C5A1 C5A2 C6A2 40(8) . . . . ? C10A C5A1 C5A2 C6A2 37(10) . . . . ? C4A1 C5A1 C5A2 C6A2 157(7) . . . . ? C6A1 C5A1 C5A2 C6A2 10(5) . . . . ? C4A2 C5A1 C5A2 C6A2 162(7) . . . . ? C10A C5A1 C5A2 C10B -2(2) . . . . ? C4A1 C5A1 C5A2 C10B 118.0(16) . . . . ? C6A1 C5A1 C5A2 C10B -30(4) . . . . ? C4A2 C5A1 C5A2 C10B 122.1(17) . . . . ? C10B C5A1 C5A2 C4A2 -122.1(17) . . . . ? C10A C5A1 C5A2 C4A2 -124(3) . . . . ? C4A1 C5A1 C5A2 C4A2 -4.1(13) . . . . ? C6A1 C5A1 C5A2 C4A2 -152(3) . . . . ? C10B C5A1 C5A2 C4A1 -118.0(16) . . . . ? C10A C5A1 C5A2 C4A1 -120(3) . . . . ? C6A1 C5A1 C5A2 C4A1 -147(3) . . . . ? C4A2 C5A1 C5A2 C4A1 4.1(13) . . . . ? C6A2 C6A1 C5A2 C5A1 174(3) . . . . ? C7A1 C6A1 C5A2 C5A1 71(3) . . . . ? C10B C6A1 C5A2 C5A1 -23(3) . . . . ? C7A2 C6A1 C5A2 C5A1 114(3) . . . . ? C7A1 C6A1 C5A2 C6A2 -104(2) . . . . ? C5A1 C6A1 C5A2 C6A2 -174(3) . . . . ? C10B C6A1 C5A2 C6A2 162.3(18) . . . . ? C7A2 C6A1 C5A2 C6A2 -60.3(17) . . . . ? C6A2 C6A1 C5A2 C10B -162.3(18) . . . . ? C7A1 C6A1 C5A2 C10B 94.0(15) . . . . ? C5A1 C6A1 C5A2 C10B 23(3) . . . . ? C7A2 C6A1 C5A2 C10B 137.4(19) . . . . ? C6A2 C6A1 C5A2 C4A2 -53(3) . . . . ? C7A1 C6A1 C5A2 C4A2 -156.3(16) . . . . ? C5A1 C6A1 C5A2 C4A2 133(4) . . . . ? C10B C6A1 C5A2 C4A2 109.7(18) . . . . ? C7A2 C6A1 C5A2 C4A2 -113(2) . . . . ? C6A2 C6A1 C5A2 C4A1 -76(3) . . . . ? C7A1 C6A1 C5A2 C4A1 -179(2) . . . . ? C5A1 C6A1 C5A2 C4A1 110(5) . . . . ? C10B C6A1 C5A2 C4A1 87(3) . . . . ? C7A2 C6A1 C5A2 C4A1 -136(2) . . . . ? O121 C4A2 C5A2 C5A1 -135(3) . . . . ? O122 C4A2 C5A2 C5A1 -138(3) . . . . ? C2A2 C4A2 C5A2 C5A1 -8(2) . . . . ? C2A1 C4A2 C5A2 C5A1 -9(2) . . . . ? O121 C4A2 C5A2 C6A1 83(3) . . . . ? O122 C4A2 C5A2 C6A1 80(3) . . . . ? C2A2 C4A2 C5A2 C6A1 -150(3) . . . . ? C5A1 C4A2 C5A2 C6A1 -142(4) . . . . ? C2A1 C4A2 C5A2 C6A1 -151(2) . . . . ? O121 C4A2 C5A2 C6A2 52(3) . . . . ? O122 C4A2 C5A2 C6A2 49(2) . . . . ? C2A2 C4A2 C5A2 C6A2 178.5(19) . . . . ? C5A1 C4A2 C5A2 C6A2 -173(2) . . . . ? C2A1 C4A2 C5A2 C6A2 177.6(17) . . . . ? O121 C4A2 C5A2 C10B 180(3) . . . . ? O122 C4A2 C5A2 C10B 177(2) . . . . ? C2A2 C4A2 C5A2 C10B -54(2) . . . . ? C5A1 C4A2 C5A2 C10B -46(2) . . . . ? C2A1 C4A2 C5A2 C10B -54.6(19) . . . . ? O121 C4A2 C5A2 C4A1 -149(7) . . . . ? O122 C4A2 C5A2 C4A1 -152(6) . . . . ? C2A2 C4A2 C5A2 C4A1 -23(5) . . . . ? C5A1 C4A2 C5A2 C4A1 -15(5) . . . . ? C2A1 C4A2 C5A2 C4A1 -24(4) . . . . ? C2A2 C4A1 C5A2 C5A1 -24(4) . . . . ? O121 C4A1 C5A2 C5A1 -144(2) . . . . ? C2A1 C4A1 C5A2 C5A1 -23(3) . . . . ? O122 C4A1 C5A2 C5A1 -144(2) . . . . ? C2A2 C4A1 C5A2 C6A1 -149(3) . . . . ? O121 C4A1 C5A2 C6A1 92(3) . . . . ? C5A1 C4A1 C5A2 C6A1 -125(4) . . . . ? C2A1 C4A1 C5A2 C6A1 -147(3) . . . . ? O122 C4A1 C5A2 C6A1 91(3) . . . . ? C2A2 C4A1 C5A2 C6A2 165(3) . . . . ? O121 C4A1 C5A2 C6A2 45.6(18) . . . . ? C5A1 C4A1 C5A2 C6A2 -171(3) . . . . ? C2A1 C4A1 C5A2 C6A2 166.5(17) . . . . ? O122 C4A1 C5A2 C6A2 45(2) . . . . ? C2A2 C4A1 C5A2 C10B -69(4) . . . . ? O121 C4A1 C5A2 C10B 172.3(14) . . . . ? C5A1 C4A1 C5A2 C10B -44.2(19) . . . . ? C2A1 C4A1 C5A2 C10B -67(2) . . . . ? O122 C4A1 C5A2 C10B 171.7(15) . . . . ? C2A2 C4A1 C5A2 C4A2 140(8) . . . . ? O121 C4A1 C5A2 C4A2 21(5) . . . . ? C5A1 C4A1 C5A2 C4A2 164(5) . . . . ? C2A1 C4A1 C5A2 C4A2 142(7) . . . . ? O122 C4A1 C5A2 C4A2 20(5) . . . . ? C5A2 C6A1 C6A2 C7A2 -134.4(15) . . . . ? C7A1 C6A1 C6A2 C7A2 -10.9(13) . . . . ? C5A1 C6A1 C6A2 C7A2 -131.9(13) . . . . ? C10B C6A1 C6A2 C7A2 179(100) . . . . ? C7A1 C6A1 C6A2 C5A2 123.5(18) . . . . ? C5A1 C6A1 C6A2 C5A2 2.5(11) . . . . ? C10B C6A1 C6A2 C5A2 -47(4) . . . . ? C7A2 C6A1 C6A2 C5A2 134.4(15) . . . . ? C5A2 C6A1 C6A2 C7A1 -123.5(18) . . . . ? C5A1 C6A1 C6A2 C7A1 -121.0(16) . . . . ? C10B C6A1 C6A2 C7A1 -170(6) . . . . ? C7A2 C6A1 C6A2 C7A1 10.9(13) . . . . ? C5A1 C5A2 C6A2 C6A1 -14(6) . . . . ? C10B C5A2 C6A2 C6A1 18.7(19) . . . . ? C4A2 C5A2 C6A2 C6A1 146(2) . . . . ? C4A1 C5A2 C6A2 C6A1 139(3) . . . . ? C5A1 C5A2 C6A2 C7A2 38(8) . . . . ? C6A1 C5A2 C6A2 C7A2 52(2) . . . . ? C10B C5A2 C6A2 C7A2 70.4(18) . . . . ? C4A2 C5A2 C6A2 C7A2 -162.0(16) . . . . ? C4A1 C5A2 C6A2 C7A2 -168.9(18) . . . . ? C5A1 C5A2 C6A2 C7A1 29(7) . . . . ? C6A1 C5A2 C6A2 C7A1 43.1(15) . . . . ? C10B C5A2 C6A2 C7A1 61.8(13) . . . . ? C4A2 C5A2 C6A2 C7A1 -170.6(13) . . . . ? C4A1 C5A2 C6A2 C7A1 -177.5(16) . . . . ? C7A2 C7A1 C6A2 C6A1 -160(3) . . . . ? C8A2 C7A1 C6A2 C6A1 149(2) . . . . ? C8A1 C7A1 C6A2 C6A1 173.9(19) . . . . ? C8A2 C7A1 C6A2 C7A2 -50.8(16) . . . . ? C8A1 C7A1 C6A2 C7A2 -26.2(18) . . . . ? C6A1 C7A1 C6A2 C7A2 160(3) . . . . ? C7A2 C7A1 C6A2 C5A2 166(2) . . . . ? C8A2 C7A1 C6A2 C5A2 115.0(19) . . . . ? C8A1 C7A1 C6A2 C5A2 139.6(15) . . . . ? C6A1 C7A1 C6A2 C5A2 -34.3(14) . . . . ? C8A2 C8A1 C7A2 C7A1 14(4) . . . . ? C9A1 C8A1 C7A2 C7A1 -95(4) . . . . ? C9A2 C8A1 C7A2 C7A1 -55(4) . . . . ? C7A1 C8A1 C7A2 C8A2 -14(4) . . . . ? C9A1 C8A1 C7A2 C8A2 -109(6) . . . . ? C9A2 C8A1 C7A2 C8A2 -70(4) . . . . ? C8A2 C8A1 C7A2 C6A2 -72(5) . . . . ? C7A1 C8A1 C7A2 C6A2 -86(3) . . . . ? C9A1 C8A1 C7A2 C6A2 179(2) . . . . ? C9A2 C8A1 C7A2 C6A2 -142(4) . . . . ? C8A2 C8A1 C7A2 C6A1 -22(6) . . . . ? C7A1 C8A1 C7A2 C6A1 -36(2) . . . . ? C9A1 C8A1 C7A2 C6A1 -131(3) . . . . ? C9A2 C8A1 C7A2 C6A1 -91(5) . . . . ? C8A2 C7A1 C7A2 C8A1 -9(2) . . . . ? C6A1 C7A1 C7A2 C8A1 -152.3(18) . . . . ? C6A2 C7A1 C7A2 C8A1 -142(2) . . . . ? C8A1 C7A1 C7A2 C8A2 9(2) . . . . ? C6A1 C7A1 C7A2 C8A2 -143.6(17) . . . . ? C6A2 C7A1 C7A2 C8A2 -133.6(15) . . . . ? C8A2 C7A1 C7A2 C6A2 133.6(15) . . . . ? C8A1 C7A1 C7A2 C6A2 142(2) . . . . ? C6A1 C7A1 C7A2 C6A2 -9.9(13) . . . . ? C8A2 C7A1 C7A2 C6A1 143.6(17) . . . . ? C8A1 C7A1 C7A2 C6A1 152.3(18) . . . . ? C6A2 C7A1 C7A2 C6A1 9.9(13) . . . . ? C6A1 C6A2 C7A2 C8A1 100(4) . . . . ? C5A2 C6A2 C7A2 C8A1 68(4) . . . . ? C7A1 C6A2 C7A2 C8A1 84(3) . . . . ? C6A1 C6A2 C7A2 C7A1 16(2) . . . . ? C5A2 C6A2 C7A2 C7A1 -16(2) . . . . ? C6A1 C6A2 C7A2 C8A2 63(3) . . . . ? C5A2 C6A2 C7A2 C8A2 31(3) . . . . ? C7A1 C6A2 C7A2 C8A2 47(2) . . . . ? C5A2 C6A2 C7A2 C6A1 -31.8(13) . . . . ? C7A1 C6A2 C7A2 C6A1 -16(2) . . . . ? C6A2 C6A1 C7A2 C8A1 -120(4) . . . . ? C5A2 C6A1 C7A2 C8A1 -43(4) . . . . ? C7A1 C6A1 C7A2 C8A1 42(3) . . . . ? C5A1 C6A1 C7A2 C8A1 -12(4) . . . . ? C10B C6A1 C7A2 C8A1 61(5) . . . . ? C6A2 C6A1 C7A2 C7A1 -161(2) . . . . ? C5A2 C6A1 C7A2 C7A1 -85(2) . . . . ? C5A1 C6A1 C7A2 C7A1 -54(2) . . . . ? C10B C6A1 C7A2 C7A1 19(3) . . . . ? C6A2 C6A1 C7A2 C8A2 -131(2) . . . . ? C5A2 C6A1 C7A2 C8A2 -54(3) . . . . ? C7A1 C6A1 C7A2 C8A2 30.5(18) . . . . ? C5A1 C6A1 C7A2 C8A2 -23(3) . . . . ? C10B C6A1 C7A2 C8A2 50(3) . . . . ? C5A2 C6A1 C7A2 C6A2 77(2) . . . . ? C7A1 C6A1 C7A2 C6A2 161(2) . . . . ? C5A1 C6A1 C7A2 C6A2 108(2) . . . . ? C10B C6A1 C7A2 C6A2 -179(3) . . . . ? C7A2 C8A1 C8A2 C7A1 -13(4) . . . . ? C9A1 C8A1 C8A2 C7A1 137.7(19) . . . . ? C9A2 C8A1 C8A2 C7A1 138(3) . . . . ? C7A1 C8A1 C8A2 C7A2 13(4) . . . . ? C9A1 C8A1 C8A2 C7A2 151(3) . . . . ? C9A2 C8A1 C8A2 C7A2 151(3) . . . . ? C7A2 C8A1 C8A2 C9A2 -151(3) . . . . ? C7A1 C8A1 C8A2 C9A2 -138(3) . . . . ? C9A1 C8A1 C8A2 C9A2 0(2) . . . . ? C7A2 C8A1 C8A2 C9A1 -151(3) . . . . ? C7A1 C8A1 C8A2 C9A1 -137.7(19) . . . . ? C9A2 C8A1 C8A2 C9A1 0(2) . . . . ? C7A2 C7A1 C8A2 C8A1 12(3) . . . . ? C6A1 C7A1 C8A2 C8A1 75(4) . . . . ? C6A2 C7A1 C8A2 C8A1 52(3) . . . . ? C8A1 C7A1 C8A2 C7A2 -12(3) . . . . ? C6A1 C7A1 C8A2 C7A2 63(2) . . . . ? C6A2 C7A1 C8A2 C7A2 40.3(11) . . . . ? C7A2 C7A1 C8A2 C9A2 100(3) . . . . ? C8A1 C7A1 C8A2 C9A2 88(4) . . . . ? C6A1 C7A1 C8A2 C9A2 163(2) . . . . ? C6A2 C7A1 C8A2 C9A2 140(3) . . . . ? C7A2 C7A1 C8A2 C9A1 72(3) . . . . ? C8A1 C7A1 C8A2 C9A1 60(3) . . . . ? C6A1 C7A1 C8A2 C9A1 135(3) . . . . ? C6A2 C7A1 C8A2 C9A1 112(3) . . . . ? C7A1 C7A2 C8A2 C8A1 -163(5) . . . . ? C6A2 C7A2 C8A2 C8A1 134(4) . . . . ? C6A1 C7A2 C8A2 C8A1 164(4) . . . . ? C8A1 C7A2 C8A2 C7A1 163(5) . . . . ? C6A2 C7A2 C8A2 C7A1 -63(2) . . . . ? C6A1 C7A2 C8A2 C7A1 -32.9(16) . . . . ? C8A1 C7A2 C8A2 C9A2 37(4) . . . . ? C7A1 C7A2 C8A2 C9A2 -126(4) . . . . ? C6A2 C7A2 C8A2 C9A2 171(3) . . . . ? C6A1 C7A2 C8A2 C9A2 -159(3) . . . . ? C8A1 C7A2 C8A2 C9A1 28(3) . . . . ? C7A1 C7A2 C8A2 C9A1 -134(3) . . . . ? C6A2 C7A2 C8A2 C9A1 162(2) . . . . ? C6A1 C7A2 C8A2 C9A1 -167.3(19) . . . . ? C9A2 C9A1 C8A2 C8A1 -179(7) . . . . ? C9A2 C9A1 C8A2 C7A1 112(6) . . . . ? C8A1 C9A1 C8A2 C7A1 -69(3) . . . . ? C9A2 C9A1 C8A2 C7A2 159(6) . . . . ? C8A1 C9A1 C8A2 C7A2 -21(2) . . . . ? C8A1 C9A1 C8A2 C9A2 179(7) . . . . ? C8A1 C9A1 C9A2 C8A2 0(3) . . . . ? C8A2 C9A1 C9A2 C8A1 0(3) . . . . ? C8A1 C8A2 C9A2 C9A1 1(6) . . . . ? C7A1 C8A2 C9A2 C9A1 -89(7) . . . . ? C7A2 C8A2 C9A2 C9A1 -24(7) . . . . ? C7A1 C8A2 C9A2 C8A1 -89(4) . . . . ? C7A2 C8A2 C9A2 C8A1 -25(2) . . . . ? C9A1 C8A2 C9A2 C8A1 -1(6) . . . . ? C8A2 C8A1 C9A2 C9A1 -179(7) . . . . ? C7A2 C8A1 C9A2 C9A1 -100(7) . . . . ? C7A1 C8A1 C9A2 C9A1 -142(6) . . . . ? C7A2 C8A1 C9A2 C8A2 79(4) . . . . ? C7A1 C8A1 C9A2 C8A2 37(3) . . . . ? C9A1 C8A1 C9A2 C8A2 179(7) . . . . ? C5A1 C10A C10B C5A2 -0.9(9) . . . . ? C5A1 C10A C10B C6A1 -28(2) . . . . ? C5A2 C5A1 C10B C10A -178(2) . . . . ? C4A1 C5A1 C10B C10A 93.0(17) . . . . ? C6A1 C5A1 C10B C10A -161.0(18) . . . . ? C4A2 C5A1 C10B C10A 109.3(18) . . . . ? C10A C5A1 C10B C5A2 178(2) . . . . ? C4A1 C5A1 C10B C5A2 -89(2) . . . . ? C6A1 C5A1 C10B C5A2 17(2) . . . . ? C4A2 C5A1 C10B C5A2 -73(2) . . . . ? C5A2 C5A1 C10B C6A1 -17(2) . . . . ? C10A C5A1 C10B C6A1 161.0(18) . . . . ? C4A1 C5A1 C10B C6A1 -106.0(9) . . . . ? C4A2 C5A1 C10B C6A1 -89.7(13) . . . . ? C5A1 C5A2 C10B C10A 2(2) . . . . ? C6A1 C5A2 C10B C10A -153(2) . . . . ? C6A2 C5A2 C10B C10A -164.5(19) . . . . ? C4A2 C5A2 C10B C10A 68(2) . . . . ? C4A1 C5A2 C10B C10A 60(2) . . . . ? C6A1 C5A2 C10B C5A1 -155(3) . . . . ? C6A2 C5A2 C10B C5A1 -167(3) . . . . ? C4A2 C5A2 C10B C5A1 66(2) . . . . ? C4A1 C5A2 C10B C5A1 58.2(19) . . . . ? C5A1 C5A2 C10B C6A1 155(3) . . . . ? C6A2 C5A2 C10B C6A1 -11.4(11) . . . . ? C4A2 C5A2 C10B C6A1 -138.7(16) . . . . ? C4A1 C5A2 C10B C6A1 -146.7(19) . . . . ? C6A2 C6A1 C10B C10A 96(6) . . . . ? C5A2 C6A1 C10B C10A 44(3) . . . . ? C7A1 C6A1 C10B C10A -73(3) . . . . ? C5A1 C6A1 C10B C10A 32(2) . . . . ? C7A2 C6A1 C10B C10A -85(4) . . . . ? C6A2 C6A1 C10B C5A1 64(6) . . . . ? C5A2 C6A1 C10B C5A1 11.9(16) . . . . ? C7A1 C6A1 C10B C5A1 -105.6(12) . . . . ? C7A2 C6A1 C10B C5A1 -117.3(19) . . . . ? C6A2 C6A1 C10B C5A2 52(5) . . . . ? C7A1 C6A1 C10B C5A2 -117.6(15) . . . . ? C5A1 C6A1 C10B C5A2 -11.9(16) . . . . ? C7A2 C6A1 C10B C5A2 -129(3) . . . . ? C4D C5D C7D2 C7D1 114(3) . . . . ? C6D C5D C7D2 C7D1 -127(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 OW3 0.86 2.15 2.972(11) 160.5 2_664 N5 H5 O8 0.86 2.36 3.139(7) 150.6 . N7 H7 OW2 0.86 2.27 3.110(12) 164.9 3_656 N8 H8 O5 0.86 2.15 2.886(7) 143.8 . O122 H122 O2 0.89(2) 2.042(6) 2.93(2) 178.5(17) . O122 H122 O2 0.89(2) 2.042(6) 2.93(2) 178.5(17) . OW1 HW11 O1 0.807(7) 1.989(6) 2.767(9) 161.6(6) . OW1 HW12 O3 0.809(7) 2.078(5) 2.821(8) 152.7(5) . OW2 HW21 O10 0.874(9) 2.031(6) 2.903(11) 176.3(7) 3_646 OW2 HW22 N7 0.943(10) 2.291(7) 3.110(12) 145.0(6) 3_646 OW3 HW31 O9 0.794(8) 2.159(6) 2.935(10) 165.9(7) . OW4 HW42 OW1 0.894(16) 1.947(8) 2.839(18) 175.6(12) 3_756 OW4 HW41 O4 0.869(16) 1.963(6) 2.830(17) 174.9(12) . OW5 HW51 O11 0.925(14) 1.881(7) 2.801(15) 173.0(10) 3_656 OW5 HW52 OW2 0.944(14) 1.830(10) 2.774(17) 178.2(10) 3_656 OW8 HW81 O7 0.839(11) 2.110(6) 2.946(13) 174.7(10) . _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 69.99 _diffrn_measured_fraction_theta_full 0.857 _refine_diff_density_max 0.631 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.071 data_CsHII _database_code_CSD 195323 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cyclosporin H crystal form II ex MeOH+Mg(ClO4)2 RT ; _chemical_name_common 'cyclosporin H' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C62 H111 O12 N11. 6.4H2O' _chemical_compound_source Sandoz-Novartis _chemical_formula_sum 'C62 H123.8 O18.4 N11' _chemical_formula_weight 1327 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' O O 0.0492 0.0322 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 17.358(2) _cell_length_b 19.515(1) _cell_length_c 23.225(3) _cell_angle_alpha 90.000(0) _cell_angle_beta 90.000(0) _cell_angle_gamma 90.000(0) _cell_volume 7867.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 25 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2883 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type 'empirical via \psi scans' _exptl_absorpt_process_details '(North, Philips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.984 _exptl_special_details ; Room temperature capillary mounted ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method \w-/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 97 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12266 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 74.61 _reflns_number_total 11462 _reflns_number_gt 7298 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4-PC Software (Enraf-Nonius, 1992)' _computing_cell_refinement 'SET4 and CELDIM in CAD-4-PC Software (Enraf-Nonius, 1992)' _computing_data_reduction ; CCP4: CAD77, CADRAL, CADSHEL The HKL Manual, 4th edition in Sawyer et al., 1993: Data Collection and Processing": Proceedings of the CCP4 Study Weekend 29-30 January 1993 (Eds. L.Sawyer, N.Isaacs and S.Bailey) SERC Daresbury Laboratory* DL/SC1/R34. ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1998)' _computing_publication_material SHELX97 _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^)+(0.0938P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00111(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 -0.4(2) _refine_ls_number_reflns 11462 _refine_ls_number_parameters 911 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1555 _refine_ls_wR_factor_gt 0.1429 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.004 _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 N1 N 0.62692(11) 0.65245(11) 0.61396(10) 0.0677(6) Uani 1 1 d . . . N2 N 0.79343(12) 0.54877(11) 0.57459(9) 0.0630(6) Uani 1 1 d . . . H1 H 0.7903 0.5476 0.5376 0.108(10) Uiso 1 1 calc R . . N3 N 0.97444(11) 0.56595(10) 0.65451(9) 0.0561(6) Uani 1 1 d . . . N4 N 1.06890(11) 0.71139(10) 0.72828(9) 0.0573(6) Uani 1 1 d . . . N5 N 0.94486(12) 0.83165(10) 0.74543(9) 0.0612(6) Uani 1 1 d . . . H2 H 0.9168 0.8028 0.7640 0.106(10) Uiso 1 1 calc R . . N6 N 0.80817(12) 0.97320(11) 0.73508(9) 0.0670(6) Uani 1 1 d . . . N7 N 0.69690(13) 0.96536(11) 0.86413(9) 0.0694(7) Uani 1 1 d . . . H3 H 0.6559 0.9478 0.8494 0.062(7) Uiso 1 1 calc R . . N8 N 0.79281(11) 0.86783(10) 0.90933(9) 0.0595(6) Uani 1 1 d . . . H4 H 0.7763 0.8682 0.8744 0.077(8) Uiso 1 1 calc R . . N9 N 0.79243(12) 0.71023(10) 0.91142(8) 0.0574(6) Uani 1 1 d . . . N10 N 0.66013(11) 0.68406(11) 0.83179(9) 0.0623(6) Uani 1 1 d . . . N11 N 0.54204(12) 0.64347(11) 0.73312(10) 0.0639(6) Uani 1 1 d . . . O1 O 0.73273(12) 0.56946(12) 0.65709(8) 0.0905(7) Uani 1 1 d . . . O2 O 0.91303(10) 0.63262(10) 0.59145(9) 0.0785(6) Uani 1 1 d . . . O3 O 0.95394(10) 0.65879(9) 0.74032(8) 0.0735(5) Uani 1 1 d . . . O4 O 1.06377(11) 0.86721(10) 0.72507(10) 0.0867(7) Uani 1 1 d . . . O5 O 0.80887(10) 0.87406(9) 0.78437(8) 0.0701(5) Uani 1 1 d . . . O6 O 0.80927(12) 1.01790(10) 0.84824(9) 0.0841(6) Uani 1 1 d . . . O7 O 0.77307(14) 0.90493(12) 0.99988(9) 0.1000(7) Uani 1 1 d . . . O8 O 0.88710(10) 0.74289(9) 0.85017(7) 0.0682(5) Uani 1 1 d . . . O9 O 0.65762(11) 0.59051(10) 0.88896(9) 0.0868(6) Uani 1 1 d . . . O10 O 0.52497(11) 0.75486(10) 0.75388(9) 0.0820(6) Uani 1 1 d . . . O11 O 0.54531(12) 0.56345(11) 0.60882(9) 0.0901(7) Uani 1 1 d . . . O12 O 0.78054(11) 0.70395(10) 0.55560(8) 0.0785(6) Uani 1 1 d . . . H5 H 0.8157 0.6767 0.5611 0.118 Uiso 1 1 calc R . . C1A C 0.65819(18) 0.70921(16) 0.64833(14) 0.0910(10) Uani 1 1 d . . . H6 H 0.6739 0.6924 0.6854 0.152(9) Uiso 1 1 calc R . . H7 H 0.6193 0.7437 0.6532 0.152(9) Uiso 1 1 calc R . . H8 H 0.7018 0.7286 0.6289 0.152(9) Uiso 1 1 calc R . . C2A C 0.67820(16) 0.61902(15) 0.57230(12) 0.0691(8) Uani 1 1 d . . . H9 H 0.6468 0.5874 0.5494 0.071(7) Uiso 1 1 calc R . . C3A C 0.73742(15) 0.57661(15) 0.60460(11) 0.0662(8) Uani 1 1 d . . . C4A C 0.71832(16) 0.66996(15) 0.52952(13) 0.0737(9) Uani 1 1 d . . . H10 H 0.7387 0.6431 0.4973 0.086(9) Uiso 1 1 calc R . . C5A C 0.66406(18) 0.72318(17) 0.50510(14) 0.0872(10) Uani 1 1 d . . . H11 H 0.6430 0.7492 0.5376 0.141(13) Uiso 1 1 calc R . . C6A C 0.7084(2) 0.77407(19) 0.46634(16) 0.1101(13) Uani 1 1 d . . . H12 H 0.7593 0.7812 0.4825 0.170(12) Uiso 1 1 calc R . . H13 H 0.7149 0.7536 0.4286 0.170(12) Uiso 1 1 calc R . . C17A C 0.6696(3) 0.8433(2) 0.45912(17) 0.1194(14) Uani 1 1 d . . . H14 H 0.6834 0.8652 0.4251 0.179 Uiso 1 1 calc R . . C8A C 0.6254(3) 0.8757(2) 0.48731(19) 0.1419(17) Uani 1 1 d . . . H15 H 0.6079 0.8530 0.5200 0.24(2) Uiso 1 1 calc R . . C9A C 0.5927(3) 0.9459(2) 0.4800(2) 0.1271(15) Uani 1 1 d . . . H16 H 0.5376 0.9440 0.4832 0.235(14) Uiso 1 1 calc R . . H17 H 0.6066 0.9634 0.4428 0.235(14) Uiso 1 1 calc R . . H18 H 0.6129 0.9756 0.5093 0.235(14) Uiso 1 1 calc R . . C10A C 0.5973(2) 0.6910(2) 0.47388(19) 0.1252(15) Uani 1 1 d . . . H19 H 0.5705 0.7255 0.4522 0.207(13) Uiso 1 1 calc R . . H20 H 0.5627 0.6708 0.5013 0.207(13) Uiso 1 1 calc R . . H21 H 0.6160 0.6563 0.4482 0.207(13) Uiso 1 1 calc R . . C1B C 0.86107(14) 0.51969(13) 0.60309(12) 0.0630(8) Uani 1 1 d . . . H22 H 0.8452 0.4973 0.6389 0.055(6) Uiso 1 1 calc R . . C2B C 0.91792(15) 0.57801(13) 0.61699(11) 0.0601(7) Uani 1 1 d . . . C3B C 0.89991(18) 0.46683(15) 0.56347(14) 0.0841(10) Uani 1 1 d . . . H23 H 0.9136 0.4889 0.5275 0.098(7) Uiso 1 1 calc R . . H24 H 0.9471 0.4511 0.5815 0.098(7) Uiso 1 1 calc R . . C4B C 0.8500(2) 0.40644(17) 0.55096(17) 0.1160(13) Uani 1 1 d . . . H25 H 0.8769 0.3754 0.5260 0.154(9) Uiso 1 1 calc R . . H26 H 0.8035 0.4215 0.5325 0.154(9) Uiso 1 1 calc R . . H27 H 0.8374 0.3835 0.5863 0.154(9) Uiso 1 1 calc R . . C1C C 0.98224(17) 0.50553(15) 0.69046(12) 0.0745(9) Uani 1 1 d . . . H28 H 1.0304 0.4834 0.6823 0.107(6) Uiso 1 1 calc R . . H29 H 0.9406 0.4745 0.6826 0.107(6) Uiso 1 1 calc R . . H30 H 0.9809 0.5188 0.7303 0.107(6) Uiso 1 1 calc R . . C2C C 1.03265(14) 0.61852(14) 0.66259(11) 0.0614(8) Uani 1 1 d . . . H31 H 1.0361 0.6463 0.6280 0.065(5) Uiso 1 1 calc R . . H32 H 1.0823 0.5969 0.6686 0.065(5) Uiso 1 1 calc R . . C3C C 1.01429(14) 0.66434(13) 0.71365(11) 0.0569(7) Uani 1 1 d . . . C1D C 1.13782(16) 0.72276(17) 0.69369(14) 0.0834(10) Uani 1 1 d . . . H33 H 1.1773 0.7427 0.7173 0.168(10) Uiso 1 1 calc R . . H34 H 1.1259 0.7532 0.6625 0.168(10) Uiso 1 1 calc R . . H35 H 1.1556 0.6798 0.6785 0.168(10) Uiso 1 1 calc R . . C2D C 1.05107(14) 0.76019(12) 0.77562(11) 0.0560(7) Uani 1 1 d . . . H36 H 1.0103 0.7405 0.7997 0.053(6) Uiso 1 1 calc R . . C3D C 1.02055(14) 0.82469(13) 0.74749(11) 0.0596(7) Uani 1 1 d . . . C4D C 1.12048(16) 0.77490(14) 0.81326(12) 0.0704(8) Uani 1 1 d . . . H37 H 1.1071 0.8110 0.8402 0.055(4) Uiso 1 1 calc R . . H38 H 1.1619 0.7919 0.7891 0.055(4) Uiso 1 1 calc R . . C5D C 1.1501(2) 0.71287(17) 0.84729(15) 0.0966(11) Uani 1 1 d . . . H39 H 1.1486 0.6726 0.8221 0.138(12) Uiso 1 1 calc R . . C6D C 1.2315(2) 0.7239(2) 0.8663(2) 0.1428(17) Uani 1 1 d . . . H40 H 1.2334 0.7614 0.8931 0.147(8) Uiso 1 1 calc R . . H41 H 1.2630 0.7344 0.8334 0.147(8) Uiso 1 1 calc R . . H42 H 1.2504 0.6831 0.8846 0.147(8) Uiso 1 1 calc R . . C7D C 1.0998(3) 0.6986(2) 0.8999(2) 0.1514(18) Uani 1 1 d . . . H43 H 1.0469 0.6954 0.8883 0.256(16) Uiso 1 1 calc R . . H44 H 1.1056 0.7352 0.9272 0.256(16) Uiso 1 1 calc R . . H45 H 1.1154 0.6562 0.9173 0.256(16) Uiso 1 1 calc R . . C1E C 0.90676(15) 0.88590(14) 0.71313(11) 0.0615(8) Uani 1 1 d . . . H46 H 0.9429 0.9240 0.7081 0.071(7) Uiso 1 1 calc R . . C2E C 0.83878(15) 0.91057(14) 0.74802(11) 0.0615(7) Uani 1 1 d . . . C3E C 0.88049(18) 0.86187(19) 0.65465(14) 0.0896(11) Uani 1 1 d . . . H47 H 0.8545 0.9005 0.6360 0.098(9) Uiso 1 1 calc R . . C4E C 0.9462(3) 0.8408(3) 0.61644(17) 0.159(2) Uani 1 1 d . . . H48 H 0.9286 0.8377 0.5773 0.197(12) Uiso 1 1 calc R . . H49 H 0.9654 0.7969 0.6286 0.197(12) Uiso 1 1 calc R . . H50 H 0.9867 0.8742 0.6190 0.197(12) Uiso 1 1 calc R . . C5E C 0.8250(2) 0.8061(2) 0.65865(19) 0.1321(16) Uani 1 1 d . . . H51 H 0.8070 0.7944 0.6208 0.245(15) Uiso 1 1 calc R . . H52 H 0.7822 0.8202 0.6820 0.245(15) Uiso 1 1 calc R . . H53 H 0.8491 0.7668 0.6758 0.245(15) Uiso 1 1 calc R . . C1F C 0.84634(19) 1.02559(15) 0.70064(13) 0.0817(9) Uani 1 1 d . . . H54 H 0.8154 1.0360 0.6675 0.114(6) Uiso 1 1 calc R . . H55 H 0.8957 1.0090 0.6883 0.114(6) Uiso 1 1 calc R . . H56 H 0.8531 1.0662 0.7234 0.114(6) Uiso 1 1 calc R . . C2F C 0.73522(15) 0.99202(15) 0.76435(12) 0.0677(8) Uani 1 1 d . . . H57 H 0.7255 1.0399 0.7539 0.079(8) Uiso 1 1 calc R . . C3F C 0.74989(16) 0.99216(14) 0.82858(13) 0.0662(8) Uani 1 1 d . . . C4F C 0.66679(17) 0.95210(16) 0.74192(13) 0.0785(9) Uani 1 1 d . . . H58 H 0.6727 0.9048 0.7540 0.074(5) Uiso 1 1 calc R . . H59 H 0.6209 0.9697 0.7606 0.074(5) Uiso 1 1 calc R . . C5F C 0.6529(2) 0.95258(19) 0.67812(15) 0.1016(12) Uani 1 1 d . . . H60 H 0.6999 0.9354 0.6597 0.150(14) Uiso 1 1 calc R . . C6F C 0.6382(3) 1.0247(2) 0.65419(18) 0.1345(16) Uani 1 1 d . . . H61 H 0.6782 1.0551 0.6670 0.191(11) Uiso 1 1 calc R . . H62 H 0.5893 1.0411 0.6677 0.191(11) Uiso 1 1 calc R . . H63 H 0.6379 1.0232 0.6129 0.191(11) Uiso 1 1 calc R . . C7F C 0.5890(3) 0.9050(2) 0.66176(19) 0.1319(16) Uani 1 1 d . . . H64 H 0.6028 0.8590 0.6720 0.198(12) Uiso 1 1 calc R . . H65 H 0.5803 0.9076 0.6210 0.198(12) Uiso 1 1 calc R . . H66 H 0.5428 0.9179 0.6818 0.198(12) Uiso 1 1 calc R . . C1G C 0.70544(17) 0.96464(15) 0.92570(13) 0.0742(9) Uani 1 1 d . . . H67 H 0.7275 1.0090 0.9366 0.091(9) Uiso 1 1 calc R . . C2G C 0.76053(16) 0.90950(15) 0.94780(12) 0.0679(8) Uani 1 1 d . . . C3G C 0.6283(2) 0.9590(2) 0.95590(16) 0.1204(14) Uani 1 1 d . . . H68 H 0.6359 0.9604 0.9968 0.136(8) Uiso 1 1 calc R . . H69 H 0.6041 0.9165 0.9456 0.136(8) Uiso 1 1 calc R . . H70 H 0.5959 0.9965 0.9444 0.136(8) Uiso 1 1 calc R . . C1H C 0.85518(14) 0.82178(13) 0.92496(12) 0.0598(7) Uani 1 1 d . . . H71 H 0.8520 0.8124 0.9663 0.062(7) Uiso 1 1 calc R . . C2H C 0.84702(14) 0.75445(13) 0.89257(10) 0.0551(7) Uani 1 1 d . . . C3H C 0.93296(16) 0.85555(15) 0.91230(15) 0.0802(9) Uani 1 1 d . . . H72 H 0.9738 0.8254 0.9239 0.115(6) Uiso 1 1 calc R . . H73 H 0.9368 0.8978 0.9333 0.115(6) Uiso 1 1 calc R . . H74 H 0.9371 0.8646 0.8718 0.115(6) Uiso 1 1 calc R . . C1I C 0.74602(16) 0.72166(15) 0.96309(11) 0.0719(9) Uani 1 1 d . . . H75 H 0.7027 0.6911 0.9629 0.111(6) Uiso 1 1 calc R . . H76 H 0.7281 0.7682 0.9636 0.111(6) Uiso 1 1 calc R . . H77 H 0.7768 0.7132 0.9967 0.111(6) Uiso 1 1 calc R . . C2I C 0.78044(15) 0.64560(13) 0.88029(12) 0.0613(8) Uani 1 1 d . . . H78 H 0.8086 0.6480 0.8438 0.053(6) Uiso 1 1 calc R . . C3I C 0.69481(17) 0.63782(14) 0.86696(12) 0.0668(8) Uani 1 1 d . . . C4I C 0.81038(17) 0.58405(14) 0.91411(13) 0.0719(8) Uani 1 1 d . . . H79 H 0.7830 0.5822 0.9505 0.095(6) Uiso 1 1 calc R . . H80 H 0.7973 0.5429 0.8929 0.095(6) Uiso 1 1 calc R . . C5I C 0.89584(18) 0.58245(16) 0.92678(13) 0.0806(10) Uani 1 1 d . . . H81 H 0.9110 0.6282 0.9401 0.100(9) Uiso 1 1 calc R . . C6I C 0.9129(3) 0.5316(2) 0.97534(19) 0.1290(16) Uani 1 1 d . . . H82 H 0.8887 0.5471 1.0102 0.263(17) Uiso 1 1 calc R . . H83 H 0.9675 0.5286 0.9811 0.263(17) Uiso 1 1 calc R . . H84 H 0.8931 0.4873 0.9652 0.263(17) Uiso 1 1 calc R . . C7I C 0.9419(2) 0.5663(2) 0.87451(15) 0.1023(12) Uani 1 1 d . . . H85 H 0.9306 0.5205 0.8620 0.127(7) Uiso 1 1 calc R . . H86 H 0.9958 0.5699 0.8834 0.127(7) Uiso 1 1 calc R . . H87 H 0.9292 0.5980 0.8444 0.127(7) Uiso 1 1 calc R . . C1J C 0.70044(17) 0.74213(15) 0.80628(12) 0.0730(9) Uani 1 1 d . . . H88 H 0.6727 0.7578 0.7730 0.110(6) Uiso 1 1 calc R . . H89 H 0.7513 0.7283 0.7950 0.110(6) Uiso 1 1 calc R . . H90 H 0.7039 0.7785 0.8339 0.110(6) Uiso 1 1 calc R . . C2J C 0.57546(15) 0.68585(15) 0.83110(12) 0.0676(8) Uani 1 1 d . . . H91 H 0.5566 0.6413 0.8446 0.093(9) Uiso 1 1 calc R . . C3J C 0.54571(15) 0.69696(15) 0.77009(13) 0.0672(8) Uani 1 1 d . . . C4J C 0.54585(18) 0.74031(18) 0.87181(14) 0.0892(10) Uani 1 1 d . . . H92 H 0.5782 0.7401 0.9059 0.122(8) Uiso 1 1 calc R . . H93 H 0.5523 0.7845 0.8534 0.122(8) Uiso 1 1 calc R . . C5J C 0.4638(2) 0.7344(2) 0.89086(18) 0.1119(14) Uani 1 1 d . . . H94 H 0.4308 0.7337 0.8566 0.201(19) Uiso 1 1 calc R . . C6J C 0.4399(3) 0.7942(3) 0.9283(2) 0.1681(19) Uani 1 1 d . . . H95 H 0.4424 0.8358 0.9062 0.220(13) Uiso 1 1 calc R . . H96 H 0.4740 0.7975 0.9607 0.220(13) Uiso 1 1 calc R . . H97 H 0.3881 0.7873 0.9416 0.220(13) Uiso 1 1 calc R . . C7J C 0.4514(3) 0.6668(2) 0.9245(2) 0.1475(17) Uani 1 1 d . . . H98 H 0.4638 0.6286 0.9001 0.194(12) Uiso 1 1 calc R . . H99 H 0.3986 0.6636 0.9364 0.194(12) Uiso 1 1 calc R . . H100 H 0.4843 0.6662 0.9577 0.194(12) Uiso 1 1 calc R . . C1K C 0.56818(19) 0.57397(15) 0.74853(14) 0.0839(10) Uani 1 1 d . . . H101 H 0.5321 0.5409 0.7341 0.158(9) Uiso 1 1 calc R . . H102 H 0.5715 0.5700 0.7897 0.158(9) Uiso 1 1 calc R . . H103 H 0.6180 0.5657 0.7319 0.158(9) Uiso 1 1 calc R . . C2K C 0.51056(14) 0.65353(15) 0.67503(13) 0.0697(9) Uani 1 1 d . . . H104 H 0.5120 0.7029 0.6673 0.059(6) Uiso 1 1 calc R . . C3K C 0.56297(16) 0.61947(15) 0.63055(12) 0.0671(8) Uani 1 1 d . . . C4K C 0.42598(16) 0.63093(18) 0.66872(16) 0.0888(11) Uani 1 1 d . . . H105 H 0.4238 0.5809 0.6723 0.073(8) Uiso 1 1 calc R . . C5K C 0.3966(2) 0.6504(2) 0.60993(19) 0.1308(16) Uani 1 1 d . . . H106 H 0.4040 0.6986 0.6040 0.160(9) Uiso 1 1 calc R . . H107 H 0.3428 0.6397 0.6073 0.160(9) Uiso 1 1 calc R . . H108 H 0.4244 0.6252 0.5811 0.160(9) Uiso 1 1 calc R . . C6K C 0.37581(18) 0.66229(19) 0.71643(19) 0.1090(14) Uani 1 1 d . . . H109 H 0.3232 0.6485 0.7111 0.128(7) Uiso 1 1 calc R . . H110 H 0.3792 0.7114 0.7148 0.128(7) Uiso 1 1 calc R . . H111 H 0.3937 0.6467 0.7533 0.128(7) Uiso 1 1 calc R . . OW1 O 0.81963(12) 0.57871(12) 0.75527(8) 0.0872(7) Uani 1 1 d . . . OW2 O 0.47068(15) 0.44183(15) 0.65610(14) 0.1311(10) Uani 1 1 d . . . OW3 O 0.67489(19) 0.45707(14) 0.94855(11) 0.1276(10) Uani 1 1 d . . . OW4 O 1.20018(16) 0.94016(16) 0.72231(19) 0.1674(15) Uani 1 1 d . . . OW5 O 0.4334(2) 0.87639(19) 0.76058(19) 0.1808(16) Uani 1 1 d . . . OW6 O 0.7021(3) 0.4100(3) 0.6845(2) 0.238(2) Uani 1 1 d . . . OW7 O 1.3195(5) 0.8789(4) 0.6537(3) 0.152(3) Uani 0.40 1 d P . . HW11 H 0.7974 0.5798 0.7210 0.228 Uiso 1 1 d . . . HW12 H 0.8557 0.6005 0.7473 0.228 Uiso 1 1 d . . . HW21 H 0.4967 0.4772 0.6345 0.228 Uiso 1 1 d . . . HW22 H 0.5023 0.4184 0.6805 0.228 Uiso 1 1 d . . . HW31 H 0.6621 0.5001 0.9374 0.228 Uiso 1 1 d . . . HW32 H 0.6803 0.4355 0.9147 0.228 Uiso 1 1 d . . . HW41 H 1.2049 0.9828 0.7275 0.228 Uiso 1 1 d . . . HW42 H 1.1608 0.9293 0.7043 0.228 Uiso 1 1 d . . . HW51 H 0.4582 0.8408 0.7681 0.228 Uiso 1 1 d . . . HW52 H 0.3890 0.8760 0.7775 0.228 Uiso 1 1 d . . . HW61 H 0.7376 0.4051 0.7134 0.228 Uiso 1 1 d . . . HW62 H 0.6947 0.4533 0.6808 0.228 Uiso 1 1 d . . . HW71 H 1.2761 0.8756 0.6679 0.228 Uiso 0.40 1 d P . . HW72 H 1.3497 0.8773 0.6826 0.228 Uiso 0.40 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0532(12) 0.0744(14) 0.0755(13) -0.0158(12) -0.0021(11) -0.0007(11) N2 0.0600(12) 0.0671(13) 0.0618(13) -0.0033(11) -0.0125(11) 0.0079(11) N3 0.0539(11) 0.0530(11) 0.0614(12) -0.0081(10) -0.0097(10) 0.0003(10) N4 0.0477(10) 0.0583(12) 0.0659(12) -0.0176(11) 0.0026(10) -0.0034(10) N5 0.0590(12) 0.0538(12) 0.0707(13) 0.0038(11) 0.0130(11) 0.0027(10) N6 0.0673(12) 0.0596(12) 0.0742(13) 0.0180(11) 0.0109(12) 0.0075(11) N7 0.0617(12) 0.0673(13) 0.0793(15) 0.0093(12) 0.0093(12) 0.0089(12) N8 0.0583(12) 0.0652(13) 0.0549(12) 0.0027(10) 0.0027(10) 0.0063(11) N9 0.0632(12) 0.0519(11) 0.0570(11) 0.0021(10) 0.0135(10) -0.0075(10) N10 0.0574(12) 0.0640(13) 0.0656(13) 0.0002(11) 0.0084(11) -0.0089(11) N11 0.0571(11) 0.0578(12) 0.0767(14) -0.0009(11) -0.0011(11) 0.0010(10) O1 0.0799(12) 0.1271(17) 0.0645(11) 0.0098(12) -0.0095(10) 0.0154(12) O2 0.0750(11) 0.0651(11) 0.0954(13) 0.0077(11) -0.0200(10) -0.0031(10) O3 0.0605(10) 0.0761(12) 0.0840(12) -0.0242(10) 0.0173(10) -0.0146(9) O4 0.0607(11) 0.0775(12) 0.1219(16) 0.0138(12) 0.0069(11) -0.0081(10) O5 0.0701(10) 0.0621(10) 0.0779(11) 0.0203(9) 0.0197(9) 0.0117(9) O6 0.0822(12) 0.0850(13) 0.0850(13) -0.0030(11) 0.0090(11) -0.0090(11) O7 0.1306(17) 0.0994(15) 0.0699(12) -0.0073(12) 0.0071(13) 0.0321(14) O8 0.0633(10) 0.0680(11) 0.0731(11) -0.0001(10) 0.0217(9) -0.0007(9) O9 0.0777(12) 0.0730(12) 0.1096(15) 0.0250(11) 0.0141(12) -0.0159(10) O10 0.0814(12) 0.0662(11) 0.0984(14) -0.0037(11) 0.0061(11) 0.0109(10) O11 0.0904(13) 0.0782(13) 0.1017(14) -0.0180(12) -0.0070(12) -0.0185(11) O12 0.0791(12) 0.0697(12) 0.0868(13) 0.0078(11) -0.0053(11) 0.0025(10) C1A 0.0782(18) 0.092(2) 0.102(2) -0.0403(18) 0.0056(17) -0.0232(18) C2A 0.0706(17) 0.0727(17) 0.0641(16) -0.0107(14) -0.0153(14) 0.0046(15) C3A 0.0644(15) 0.0730(18) 0.0612(16) -0.0058(14) -0.0137(14) -0.0023(14) C4A 0.0763(17) 0.0759(18) 0.0691(17) -0.0048(16) -0.0171(15) 0.0104(16) C5A 0.089(2) 0.091(2) 0.082(2) 0.0023(18) -0.0203(17) 0.0139(18) C6A 0.136(3) 0.098(2) 0.096(2) 0.025(2) -0.009(2) 0.016(2) C17A 0.160(3) 0.100(3) 0.099(3) 0.008(2) -0.030(3) 0.028(3) C8A 0.181(4) 0.149(3) 0.095(3) 0.012(3) 0.006(3) 0.080(3) C9A 0.158(4) 0.092(3) 0.131(3) 0.003(2) -0.010(3) 0.027(3) C10A 0.115(3) 0.116(3) 0.145(3) 0.014(3) -0.063(2) 0.015(2) C1B 0.0607(15) 0.0598(15) 0.0687(16) -0.0047(14) -0.0151(14) 0.0009(13) C2B 0.0657(15) 0.0520(15) 0.0628(15) -0.0057(13) -0.0051(14) 0.0028(13) C3B 0.0778(18) 0.0748(19) 0.100(2) -0.0222(18) -0.0245(17) 0.0159(16) C4B 0.136(3) 0.0648(19) 0.147(3) -0.032(2) -0.066(2) 0.008(2) C1C 0.0787(18) 0.0662(17) 0.0787(18) 0.0029(15) -0.0222(15) 0.0088(15) C2C 0.0535(14) 0.0721(17) 0.0585(15) -0.0095(14) -0.0036(12) 0.0000(13) C3C 0.0527(14) 0.0603(15) 0.0577(14) -0.0113(13) -0.0030(12) 0.0022(13) C1D 0.0649(17) 0.085(2) 0.100(2) -0.0236(17) 0.0219(16) -0.0069(16) C2D 0.0556(13) 0.0530(14) 0.0594(14) -0.0088(12) 0.0029(12) -0.0033(12) C3D 0.0522(14) 0.0569(15) 0.0697(16) -0.0087(13) 0.0114(13) -0.0107(13) C4D 0.0697(17) 0.0663(17) 0.0754(17) -0.0199(14) -0.0120(15) 0.0014(15) C5D 0.114(2) 0.0723(18) 0.103(2) -0.0270(18) -0.044(2) 0.0269(19) C6D 0.118(3) 0.151(4) 0.159(4) -0.019(3) -0.061(3) 0.049(3) C7D 0.147(4) 0.130(3) 0.177(4) 0.070(3) -0.035(3) -0.021(3) C1E 0.0593(15) 0.0619(16) 0.0631(16) 0.0060(13) 0.0078(13) 0.0004(13) C2E 0.0594(15) 0.0628(15) 0.0622(15) 0.0058(14) 0.0050(13) 0.0029(13) C3E 0.0754(19) 0.110(2) 0.084(2) 0.002(2) 0.0033(17) 0.002(2) C4E 0.117(3) 0.274(6) 0.086(2) -0.043(3) 0.020(2) 0.035(4) C5E 0.131(3) 0.130(3) 0.136(3) -0.045(3) 0.001(3) -0.040(3) C1F 0.090(2) 0.0663(18) 0.089(2) 0.0191(16) 0.0112(18) -0.0024(17) C2F 0.0678(16) 0.0596(16) 0.0758(18) 0.0096(14) 0.0085(15) 0.0136(14) C3F 0.0627(15) 0.0541(15) 0.0817(19) 0.0102(14) 0.0090(15) 0.0131(13) C4F 0.0705(17) 0.0833(19) 0.0819(19) 0.0093(17) 0.0015(16) 0.0152(16) C5F 0.108(2) 0.106(3) 0.091(2) -0.001(2) -0.017(2) 0.022(2) C6F 0.164(4) 0.130(3) 0.110(3) 0.020(3) -0.039(3) 0.018(3) C7F 0.155(4) 0.127(3) 0.114(3) -0.017(3) -0.030(3) 0.001(3) C1G 0.0742(18) 0.0672(18) 0.0811(19) 0.0043(16) 0.0145(16) 0.0104(15) C2G 0.0705(17) 0.0623(16) 0.0709(17) -0.0005(15) 0.0124(15) 0.0004(15) C3G 0.103(2) 0.151(3) 0.107(3) 0.032(2) 0.039(2) 0.044(2) C1H 0.0587(14) 0.0604(15) 0.0603(15) 0.0021(13) 0.0027(13) -0.0065(13) C2H 0.0513(13) 0.0570(14) 0.0570(14) 0.0048(13) 0.0029(12) 0.0008(12) C3H 0.0664(17) 0.0710(18) 0.103(2) -0.0010(18) 0.0027(17) -0.0118(15) C1I 0.0839(18) 0.0741(18) 0.0576(15) -0.0010(14) 0.0242(15) -0.0128(15) C2I 0.0652(15) 0.0568(15) 0.0618(15) -0.0020(13) 0.0119(13) 0.0023(13) C3I 0.0733(17) 0.0578(15) 0.0694(16) -0.0046(14) 0.0129(15) -0.0081(15) C4I 0.0833(18) 0.0573(16) 0.0753(18) 0.0071(14) 0.0117(16) -0.0006(15) C5I 0.090(2) 0.0711(19) 0.0806(19) 0.0153(17) -0.0075(17) 0.0037(17) C6I 0.142(3) 0.124(3) 0.122(3) 0.045(3) -0.028(3) 0.006(3) C7I 0.088(2) 0.114(3) 0.105(3) 0.006(2) -0.004(2) 0.010(2) C1J 0.0756(17) 0.0731(18) 0.0701(17) 0.0186(15) -0.0027(15) -0.0207(16) C2J 0.0595(15) 0.0691(17) 0.0742(17) -0.0076(15) 0.0170(14) -0.0037(14) C3J 0.0482(14) 0.0699(18) 0.0835(18) -0.0078(16) 0.0093(14) 0.0006(13) C4J 0.0819(19) 0.099(2) 0.087(2) -0.0188(19) 0.0278(17) -0.0086(18) C5J 0.092(2) 0.130(3) 0.113(3) -0.030(2) 0.019(2) -0.005(2) C6J 0.150(3) 0.145(4) 0.209(4) -0.040(4) 0.102(3) 0.009(3) C7J 0.145(3) 0.147(4) 0.151(3) -0.030(3) 0.073(3) -0.045(3) C1K 0.091(2) 0.0573(17) 0.103(2) 0.0038(17) -0.0128(19) -0.0041(16) C2K 0.0530(15) 0.0643(18) 0.092(2) 0.0003(16) -0.0099(15) -0.0066(14) C3K 0.0658(16) 0.0616(16) 0.0740(17) -0.0002(15) -0.0151(15) -0.0001(14) C4K 0.0558(16) 0.075(2) 0.135(3) 0.011(2) -0.0176(19) -0.0030(15) C5K 0.094(2) 0.147(4) 0.151(3) 0.022(3) -0.057(2) -0.014(3) C6K 0.0614(18) 0.101(3) 0.165(3) 0.007(3) 0.020(2) 0.0001(19) OW1 0.0854(13) 0.1016(15) 0.0745(12) -0.0083(12) 0.0011(11) -0.0125(12) OW2 0.0977(16) 0.1122(19) 0.183(2) -0.021(2) 0.0168(18) -0.0077(15) OW3 0.163(2) 0.1113(19) 0.1086(18) 0.0151(15) -0.0099(18) -0.0054(18) OW4 0.0866(16) 0.116(2) 0.300(4) -0.012(3) 0.013(2) -0.0218(16) OW5 0.154(3) 0.163(3) 0.225(4) -0.008(3) 0.005(3) 0.050(2) OW6 0.232(4) 0.184(4) 0.298(6) 0.014(4) 0.009(5) -0.032(4) OW7 0.190(7) 0.173(6) 0.093(4) 0.030(4) 0.032(5) 0.064(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C3K 1.340(3) . ? N1 C2A 1.468(3) . ? N1 C1A 1.469(4) . ? N2 C3A 1.314(3) . ? N2 C1B 1.462(3) . ? N2 H1 0.8600 . ? N3 C2B 1.333(3) . ? N3 C1C 1.451(3) . ? N3 C2C 1.452(3) . ? N4 C3C 1.363(3) . ? N4 C1D 1.458(3) . ? N4 C2D 1.487(3) . ? N5 C3D 1.322(3) . ? N5 C1E 1.456(3) . ? N5 H2 0.8600 . ? N6 C2E 1.366(3) . ? N6 C1F 1.457(4) . ? N6 C2F 1.483(3) . ? N7 C3F 1.342(3) . ? N7 C1G 1.438(4) . ? N7 H3 0.8600 . ? N8 C2G 1.331(3) . ? N8 C1H 1.453(3) . ? N8 H4 0.8600 . ? N9 C2H 1.354(3) . ? N9 C1I 1.462(3) . ? N9 C2I 1.469(3) . ? N10 C3I 1.358(3) . ? N10 C1J 1.458(3) . ? N10 C2J 1.470(3) . ? N11 C3J 1.353(4) . ? N11 C2K 1.469(4) . ? N11 C1K 1.474(4) . ? O1 C3A 1.230(3) . ? O2 C2B 1.223(3) . ? O3 C3C 1.222(3) . ? O4 C3D 1.234(3) . ? O5 C2E 1.221(3) . ? O6 C3F 1.234(3) . ? O7 C2G 1.232(3) . ? O8 C2H 1.227(3) . ? O9 C3I 1.237(3) . ? O10 C3J 1.244(3) . ? O11 C3K 1.242(3) . ? O12 C4A 1.405(3) . ? O12 H5 0.8200 . ? C1A H6 0.9600 . ? C1A H7 0.9600 . ? C1A H8 0.9600 . ? C2A C3A 1.518(4) . ? C2A C4A 1.569(4) . ? C2A H9 0.9800 . ? C4A C5A 1.512(4) . ? C4A H10 0.9800 . ? C5A C10A 1.505(5) . ? C5A C6A 1.545(5) . ? C5A H11 0.9800 . ? C6A C17A 1.519(5) . ? C6A H12 0.9700 . ? C6A H13 0.9700 . ? C17A C8A 1.190(6) . ? C17A H14 0.9300 . ? C8A C9A 1.493(6) . ? C8A H15 0.9300 . ? C9A H16 0.9600 . ? C9A H17 0.9600 . ? C9A H18 0.9600 . ? C10A H19 0.9600 . ? C10A H20 0.9600 . ? C10A H21 0.9600 . ? C1B C3B 1.538(4) . ? C1B C2B 1.541(4) . ? C1B H22 0.9800 . ? C3B C4B 1.492(4) . ? C3B H23 0.9700 . ? C3B H24 0.9700 . ? C4B H25 0.9600 . ? C4B H26 0.9600 . ? C4B H27 0.9600 . ? C1C H28 0.9600 . ? C1C H29 0.9600 . ? C1C H30 0.9600 . ? C2C C3C 1.519(4) . ? C2C H31 0.9700 . ? C2C H32 0.9700 . ? C1D H33 0.9600 . ? C1D H34 0.9600 . ? C1D H35 0.9600 . ? C2D C3D 1.514(4) . ? C2D C4D 1.516(4) . ? C2D H36 0.9800 . ? C4D C5D 1.534(4) . ? C4D H37 0.9700 . ? C4D H38 0.9700 . ? C5D C6D 1.497(5) . ? C5D C7D 1.528(6) . ? C5D H39 0.9800 . ? C6D H40 0.9600 . ? C6D H41 0.9600 . ? C6D H42 0.9600 . ? C7D H43 0.9600 . ? C7D H44 0.9600 . ? C7D H45 0.9600 . ? C1E C3E 1.507(4) . ? C1E C2E 1.510(4) . ? C1E H46 0.9800 . ? C3E C5E 1.457(5) . ? C3E C4E 1.503(5) . ? C3E H47 0.9800 . ? C4E H48 0.9600 . ? C4E H49 0.9600 . ? C4E H50 0.9600 . ? C5E H51 0.9600 . ? C5E H52 0.9600 . ? C5E H53 0.9600 . ? C1F H54 0.9600 . ? C1F H55 0.9600 . ? C1F H56 0.9600 . ? C2F C4F 1.513(4) . ? C2F C3F 1.513(4) . ? C2F H57 0.9800 . ? C4F C5F 1.501(4) . ? C4F H58 0.9700 . ? C4F H59 0.9700 . ? C5F C7F 1.496(6) . ? C5F C6F 1.535(5) . ? C5F H60 0.9800 . ? C6F H61 0.9600 . ? C6F H62 0.9600 . ? C6F H63 0.9600 . ? C7F H64 0.9600 . ? C7F H65 0.9600 . ? C7F H66 0.9600 . ? C1G C3G 1.516(4) . ? C1G C2G 1.528(4) . ? C1G H67 0.9800 . ? C3G H68 0.9600 . ? C3G H69 0.9600 . ? C3G H70 0.9600 . ? C1H C2H 1.521(4) . ? C1H C3H 1.531(4) . ? C1H H71 0.9800 . ? C3H H72 0.9600 . ? C3H H73 0.9600 . ? C3H H74 0.9600 . ? C1I H75 0.9600 . ? C1I H76 0.9600 . ? C1I H77 0.9600 . ? C2I C3I 1.526(4) . ? C2I C4I 1.526(4) . ? C2I H78 0.9800 . ? C4I C5I 1.513(4) . ? C4I H79 0.9700 . ? C4I H80 0.9700 . ? C5I C7I 1.488(5) . ? C5I C6I 1.531(5) . ? C5I H81 0.9800 . ? C6I H82 0.9600 . ? C6I H83 0.9600 . ? C6I H84 0.9600 . ? C7I H85 0.9600 . ? C7I H86 0.9600 . ? C7I H87 0.9600 . ? C1J H88 0.9600 . ? C1J H89 0.9600 . ? C1J H90 0.9600 . ? C2J C4J 1.512(4) . ? C2J C3J 1.524(4) . ? C2J H91 0.9800 . ? C4J C5J 1.497(5) . ? C4J H92 0.9700 . ? C4J H93 0.9700 . ? C5J C6J 1.513(6) . ? C5J C7J 1.547(6) . ? C5J H94 0.9800 . ? C6J H95 0.9600 . ? C6J H96 0.9600 . ? C6J H97 0.9600 . ? C7J H98 0.9600 . ? C7J H99 0.9600 . ? C7J H100 0.9600 . ? C1K H101 0.9600 . ? C1K H102 0.9600 . ? C1K H103 0.9600 . ? C2K C3K 1.529(4) . ? C2K C4K 1.540(4) . ? C2K H104 0.9800 . ? C4K C5K 1.506(5) . ? C4K C6K 1.536(5) . ? C4K H105 0.9800 . ? C5K H106 0.9600 . ? C5K H107 0.9600 . ? C5K H108 0.9600 . ? C6K H109 0.9600 . ? C6K H110 0.9600 . ? C6K H111 0.9600 . ? OW1 HW11 0.885 . ? OW1 HW12 0.779 . ? OW2 HW21 0.965 . ? OW2 HW22 0.912 . ? OW3 HW31 0.906 . ? OW3 HW32 0.897 . ? OW4 HW41 0.844 . ? OW4 HW42 0.828 . ? OW5 HW51 0.835 . ? OW5 HW52 0.866 . ? OW6 HW61 0.916 . ? OW6 HW62 0.859 . ? OW7 HW71 0.824 . ? OW7 HW72 0.852 . ? 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 C3K N1 C2A 118.6(2) . . ? C3K N1 C1A 120.8(2) . . ? C2A N1 C1A 118.0(2) . . ? C3A N2 C1B 121.0(2) . . ? C3A N2 H1 119.5 . . ? C1B N2 H1 119.5 . . ? C2B N3 C1C 126.0(2) . . ? C2B N3 C2C 118.2(2) . . ? C1C N3 C2C 115.8(2) . . ? C3C N4 C1D 122.4(2) . . ? C3C N4 C2D 118.10(19) . . ? C1D N4 C2D 118.7(2) . . ? C3D N5 C1E 123.0(2) . . ? C3D N5 H2 118.5 . . ? C1E N5 H2 118.5 . . ? C2E N6 C1F 124.8(2) . . ? C2E N6 C2F 116.9(2) . . ? C1F N6 C2F 117.8(2) . . ? C3F N7 C1G 123.0(2) . . ? C3F N7 H3 118.5 . . ? C1G N7 H3 118.5 . . ? C2G N8 C1H 121.6(2) . . ? C2G N8 H4 119.2 . . ? C1H N8 H4 119.2 . . ? C2H N9 C1I 123.6(2) . . ? C2H N9 C2I 119.2(2) . . ? C1I N9 C2I 117.2(2) . . ? C3I N10 C1J 123.2(2) . . ? C3I N10 C2J 117.7(2) . . ? C1J N10 C2J 117.2(2) . . ? C3J N11 C2K 119.8(2) . . ? C3J N11 C1K 122.8(2) . . ? C2K N11 C1K 117.4(2) . . ? C4A O12 H5 109.5 . . ? N1 C1A H6 109.5 . . ? N1 C1A H7 109.5 . . ? H6 C1A H7 109.5 . . ? N1 C1A H8 109.5 . . ? H6 C1A H8 109.5 . . ? H7 C1A H8 109.5 . . ? N1 C2A C3A 109.1(2) . . ? N1 C2A C4A 113.9(2) . . ? C3A C2A C4A 111.0(2) . . ? N1 C2A H9 107.5 . . ? C3A C2A H9 107.5 . . ? C4A C2A H9 107.5 . . ? O1 C3A N2 121.9(3) . . ? O1 C3A C2A 120.5(3) . . ? N2 C3A C2A 117.7(2) . . ? O12 C4A C5A 108.4(2) . . ? O12 C4A C2A 111.6(2) . . ? C5A C4A C2A 113.3(2) . . ? O12 C4A H10 107.8 . . ? C5A C4A H10 107.8 . . ? C2A C4A H10 107.8 . . ? C10A C5A C4A 112.0(3) . . ? C10A C5A C6A 111.8(3) . . ? C4A C5A C6A 110.5(3) . . ? C10A C5A H11 107.5 . . ? C4A C5A H11 107.5 . . ? C6A C5A H11 107.5 . . ? C17A C6A C5A 114.5(3) . . ? C17A C6A H12 108.6 . . ? C5A C6A H12 108.6 . . ? C17A C6A H13 108.6 . . ? C5A C6A H13 108.6 . . ? H12 C6A H13 107.6 . . ? C8A C17A C6A 134.2(4) . . ? C8A C17A H14 112.9 . . ? C6A C17A H14 112.9 . . ? C17A C8A C9A 132.0(5) . . ? C17A C8A H15 114.0 . . ? C9A C8A H15 114.0 . . ? C8A C9A H16 109.5 . . ? C8A C9A H17 109.5 . . ? H16 C9A H17 109.5 . . ? C8A C9A H18 109.5 . . ? H16 C9A H18 109.5 . . ? H17 C9A H18 109.5 . . ? C5A C10A H19 109.5 . . ? C5A C10A H20 109.5 . . ? H19 C10A H20 109.5 . . ? C5A C10A H21 109.5 . . ? H19 C10A H21 109.5 . . ? H20 C10A H21 109.5 . . ? N2 C1B C3B 110.0(2) . . ? N2 C1B C2B 108.8(2) . . ? C3B C1B C2B 109.9(2) . . ? N2 C1B H22 109.4 . . ? C3B C1B H22 109.4 . . ? C2B C1B H22 109.4 . . ? O2 C2B N3 121.5(2) . . ? O2 C2B C1B 119.9(2) . . ? N3 C2B C1B 118.5(2) . . ? C4B C3B C1B 113.1(3) . . ? C4B C3B H23 109.0 . . ? C1B C3B H23 109.0 . . ? C4B C3B H24 109.0 . . ? C1B C3B H24 109.0 . . ? H23 C3B H24 107.8 . . ? C3B C4B H25 109.5 . . ? C3B C4B H26 109.5 . . ? H25 C4B H26 109.5 . . ? C3B C4B H27 109.5 . . ? H25 C4B H27 109.5 . . ? H26 C4B H27 109.5 . . ? N3 C1C H28 109.5 . . ? N3 C1C H29 109.5 . . ? H28 C1C H29 109.5 . . ? N3 C1C H30 109.5 . . ? H28 C1C H30 109.5 . . ? H29 C1C H30 109.5 . . ? N3 C2C C3C 111.8(2) . . ? N3 C2C H31 109.3 . . ? C3C C2C H31 109.3 . . ? N3 C2C H32 109.3 . . ? C3C C2C H32 109.3 . . ? H31 C2C H32 107.9 . . ? O3 C3C N4 122.0(2) . . ? O3 C3C C2C 121.6(2) . . ? N4 C3C C2C 116.4(2) . . ? N4 C1D H33 109.5 . . ? N4 C1D H34 109.5 . . ? H33 C1D H34 109.5 . . ? N4 C1D H35 109.5 . . ? H33 C1D H35 109.5 . . ? H34 C1D H35 109.5 . . ? N4 C2D C3D 106.6(2) . . ? N4 C2D C4D 112.5(2) . . ? C3D C2D C4D 111.7(2) . . ? N4 C2D H36 108.6 . . ? C3D C2D H36 108.6 . . ? C4D C2D H36 108.6 . . ? O4 C3D N5 121.3(2) . . ? O4 C3D C2D 121.9(2) . . ? N5 C3D C2D 116.7(2) . . ? C2D C4D C5D 114.5(2) . . ? C2D C4D H37 108.6 . . ? C5D C4D H37 108.6 . . ? C2D C4D H38 108.6 . . ? C5D C4D H38 108.6 . . ? H37 C4D H38 107.6 . . ? C6D C5D C7D 109.3(3) . . ? C6D C5D C4D 110.8(3) . . ? C7D C5D C4D 111.4(3) . . ? C6D C5D H39 108.4 . . ? C7D C5D H39 108.4 . . ? C4D C5D H39 108.4 . . ? C5D C6D H40 109.5 . . ? C5D C6D H41 109.5 . . ? H40 C6D H41 109.5 . . ? C5D C6D H42 109.5 . . ? H40 C6D H42 109.5 . . ? H41 C6D H42 109.5 . . ? C5D C7D H43 109.5 . . ? C5D C7D H44 109.5 . . ? H43 C7D H44 109.5 . . ? C5D C7D H45 109.5 . . ? H43 C7D H45 109.5 . . ? H44 C7D H45 109.5 . . ? N5 C1E C3E 112.0(2) . . ? N5 C1E C2E 108.1(2) . . ? C3E C1E C2E 110.3(2) . . ? N5 C1E H46 108.8 . . ? C3E C1E H46 108.8 . . ? C2E C1E H46 108.8 . . ? O5 C2E N6 120.6(2) . . ? O5 C2E C1E 121.2(2) . . ? N6 C2E C1E 118.1(2) . . ? C5E C3E C4E 109.6(4) . . ? C5E C3E C1E 112.0(3) . . ? C4E C3E C1E 112.8(3) . . ? C5E C3E H47 107.4 . . ? C4E C3E H47 107.4 . . ? C1E C3E H47 107.4 . . ? C3E C4E H48 109.5 . . ? C3E C4E H49 109.5 . . ? H48 C4E H49 109.5 . . ? C3E C4E H50 109.5 . . ? H48 C4E H50 109.5 . . ? H49 C4E H50 109.5 . . ? C3E C5E H51 109.5 . . ? C3E C5E H52 109.5 . . ? H51 C5E H52 109.5 . . ? C3E C5E H53 109.5 . . ? H51 C5E H53 109.5 . . ? H52 C5E H53 109.5 . . ? N6 C1F H54 109.5 . . ? N6 C1F H55 109.5 . . ? H54 C1F H55 109.5 . . ? N6 C1F H56 109.5 . . ? H54 C1F H56 109.5 . . ? H55 C1F H56 109.5 . . ? N6 C2F C4F 112.6(2) . . ? N6 C2F C3F 108.0(2) . . ? C4F C2F C3F 118.2(2) . . ? N6 C2F H57 105.7 . . ? C4F C2F H57 105.7 . . ? C3F C2F H57 105.7 . . ? O6 C3F N7 120.2(3) . . ? O6 C3F C2F 120.4(3) . . ? N7 C3F C2F 119.4(2) . . ? C5F C4F C2F 117.5(3) . . ? C5F C4F H58 107.9 . . ? C2F C4F H58 107.9 . . ? C5F C4F H59 107.9 . . ? C2F C4F H59 107.9 . . ? H58 C4F H59 107.2 . . ? C7F C5F C4F 111.5(3) . . ? C7F C5F C6F 110.7(3) . . ? C4F C5F C6F 112.9(3) . . ? C7F C5F H60 107.1 . . ? C4F C5F H60 107.1 . . ? C6F C5F H60 107.1 . . ? C5F C6F H61 109.5 . . ? C5F C6F H62 109.5 . . ? H61 C6F H62 109.5 . . ? C5F C6F H63 109.5 . . ? H61 C6F H63 109.5 . . ? H62 C6F H63 109.5 . . ? C5F C7F H64 109.5 . . ? C5F C7F H65 109.5 . . ? H64 C7F H65 109.5 . . ? C5F C7F H66 109.5 . . ? H64 C7F H66 109.5 . . ? H65 C7F H66 109.5 . . ? N7 C1G C3G 111.7(3) . . ? N7 C1G C2G 113.9(2) . . ? C3G C1G C2G 110.3(3) . . ? N7 C1G H67 106.8 . . ? C3G C1G H67 106.8 . . ? C2G C1G H67 106.8 . . ? O7 C2G N8 122.7(3) . . ? O7 C2G C1G 119.4(3) . . ? N8 C2G C1G 117.9(2) . . ? C1G C3G H68 109.5 . . ? C1G C3G H69 109.5 . . ? H68 C3G H69 109.5 . . ? C1G C3G H70 109.5 . . ? H68 C3G H70 109.5 . . ? H69 C3G H70 109.5 . . ? N8 C1H C2H 110.0(2) . . ? N8 C1H C3H 110.1(2) . . ? C2H C1H C3H 111.0(2) . . ? N8 C1H H71 108.6 . . ? C2H C1H H71 108.6 . . ? C3H C1H H71 108.6 . . ? O8 C2H N9 122.6(2) . . ? O8 C2H C1H 120.2(2) . . ? N9 C2H C1H 117.1(2) . . ? C1H C3H H72 109.5 . . ? C1H C3H H73 109.5 . . ? H72 C3H H73 109.5 . . ? C1H C3H H74 109.5 . . ? H72 C3H H74 109.5 . . ? H73 C3H H74 109.5 . . ? N9 C1I H75 109.5 . . ? N9 C1I H76 109.5 . . ? H75 C1I H76 109.5 . . ? N9 C1I H77 109.5 . . ? H75 C1I H77 109.5 . . ? H76 C1I H77 109.5 . . ? N9 C2I C3I 108.9(2) . . ? N9 C2I C4I 112.0(2) . . ? C3I C2I C4I 111.0(2) . . ? N9 C2I H78 108.3 . . ? C3I C2I H78 108.3 . . ? C4I C2I H78 108.3 . . ? O9 C3I N10 120.9(3) . . ? O9 C3I C2I 119.9(3) . . ? N10 C3I C2I 119.2(2) . . ? C5I C4I C2I 116.8(2) . . ? C5I C4I H79 108.1 . . ? C2I C4I H79 108.1 . . ? C5I C4I H80 108.1 . . ? C2I C4I H80 108.1 . . ? H79 C4I H80 107.3 . . ? C7I C5I C4I 111.9(3) . . ? C7I C5I C6I 111.1(3) . . ? C4I C5I C6I 110.2(3) . . ? C7I C5I H81 107.8 . . ? C4I C5I H81 107.8 . . ? C6I C5I H81 107.8 . . ? C5I C6I H82 109.5 . . ? C5I C6I H83 109.5 . . ? H82 C6I H83 109.5 . . ? C5I C6I H84 109.5 . . ? H82 C6I H84 109.5 . . ? H83 C6I H84 109.5 . . ? C5I C7I H85 109.5 . . ? C5I C7I H86 109.5 . . ? H85 C7I H86 109.5 . . ? C5I C7I H87 109.5 . . ? H85 C7I H87 109.5 . . ? H86 C7I H87 109.5 . . ? N10 C1J H88 109.5 . . ? N10 C1J H89 109.5 . . ? H88 C1J H89 109.5 . . ? N10 C1J H90 109.5 . . ? H88 C1J H90 109.5 . . ? H89 C1J H90 109.5 . . ? N10 C2J C4J 110.5(2) . . ? N10 C2J C3J 110.6(2) . . ? C4J C2J C3J 111.5(2) . . ? N10 C2J H91 108.1 . . ? C4J C2J H91 108.1 . . ? C3J C2J H91 108.1 . . ? O10 C3J N11 119.7(3) . . ? O10 C3J C2J 120.6(3) . . ? N11 C3J C2J 119.7(2) . . ? C5J C4J C2J 117.0(3) . . ? C5J C4J H92 108.0 . . ? C2J C4J H92 108.0 . . ? C5J C4J H93 108.0 . . ? C2J C4J H93 108.0 . . ? H92 C4J H93 107.3 . . ? C4J C5J C6J 111.8(3) . . ? C4J C5J C7J 110.3(3) . . ? C6J C5J C7J 109.3(4) . . ? C4J C5J H94 108.5 . . ? C6J C5J H94 108.5 . . ? C7J C5J H94 108.5 . . ? C5J C6J H95 109.5 . . ? C5J C6J H96 109.5 . . ? H95 C6J H96 109.5 . . ? C5J C6J H97 109.5 . . ? H95 C6J H97 109.5 . . ? H96 C6J H97 109.5 . . ? C5J C7J H98 109.5 . . ? C5J C7J H99 109.5 . . ? H98 C7J H99 109.5 . . ? C5J C7J H100 109.5 . . ? H98 C7J H100 109.5 . . ? H99 C7J H100 109.5 . . ? N11 C1K H101 109.5 . . ? N11 C1K H102 109.5 . . ? H101 C1K H102 109.5 . . ? N11 C1K H103 109.5 . . ? H101 C1K H103 109.5 . . ? H102 C1K H103 109.5 . . ? N11 C2K C3K 110.0(2) . . ? N11 C2K C4K 113.8(2) . . ? C3K C2K C4K 112.2(2) . . ? N11 C2K H104 106.8 . . ? C3K C2K H104 106.8 . . ? C4K C2K H104 106.8 . . ? O11 C3K N1 120.7(3) . . ? O11 C3K C2K 120.7(3) . . ? N1 C3K C2K 118.6(2) . . ? C5K C4K C6K 111.2(3) . . ? C5K C4K C2K 109.7(3) . . ? C6K C4K C2K 111.0(3) . . ? C5K C4K H105 108.3 . . ? C6K C4K H105 108.3 . . ? C2K C4K H105 108.3 . . ? C4K C5K H106 109.5 . . ? C4K C5K H107 109.5 . . ? H106 C5K H107 109.5 . . ? C4K C5K H108 109.5 . . ? H106 C5K H108 109.5 . . ? H107 C5K H108 109.5 . . ? C4K C6K H109 109.5 . . ? C4K C6K H110 109.5 . . ? H109 C6K H110 109.5 . . ? C4K C6K H111 109.5 . . ? H109 C6K H111 109.5 . . ? H110 C6K H111 109.5 . . ? HW11 OW1 HW12 97.1 . . ? HW21 OW2 HW22 113.6 . . ? HW31 OW3 HW32 102.1 . . ? HW41 OW4 HW42 113.8 . . ? HW51 OW5 HW52 110.9 . . ? HW61 OW6 HW62 106.1 . . ? HW71 OW7 HW72 104.2 . . ? 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 C3K N1 C2A C3A -90.0(3) . . . . ? C1A N1 C2A C3A 71.8(3) . . . . ? C3K N1 C2A C4A 145.4(2) . . . . ? C1A N1 C2A C4A -52.8(3) . . . . ? C1B N2 C3A O1 -12.4(4) . . . . ? C1B N2 C3A C2A 167.0(2) . . . . ? N1 C2A C3A O1 6.6(4) . . . . ? C4A C2A C3A O1 132.9(3) . . . . ? N1 C2A C3A N2 -172.8(2) . . . . ? C4A C2A C3A N2 -46.6(3) . . . . ? N1 C2A C4A O12 78.0(3) . . . . ? C3A C2A C4A O12 -45.6(3) . . . . ? N1 C2A C4A C5A -44.7(3) . . . . ? C3A C2A C4A C5A -168.3(2) . . . . ? O12 C4A C5A C10A 177.4(3) . . . . ? C2A C4A C5A C10A -58.1(4) . . . . ? O12 C4A C5A C6A 52.1(3) . . . . ? C2A C4A C5A C6A 176.6(3) . . . . ? C10A C5A C6A C17A 77.9(4) . . . . ? C4A C5A C6A C17A -156.8(3) . . . . ? C5A C6A C17A C8A 25.3(7) . . . . ? C6A C17A C8A C9A 175.4(5) . . . . ? C3A N2 C1B C3B 157.3(2) . . . . ? C3A N2 C1B C2B -82.3(3) . . . . ? C1C N3 C2B O2 174.7(2) . . . . ? C2C N3 C2B O2 -2.7(4) . . . . ? C1C N3 C2B C1B -9.3(4) . . . . ? C2C N3 C2B C1B 173.3(2) . . . . ? N2 C1B C2B O2 -19.5(3) . . . . ? C3B C1B C2B O2 101.0(3) . . . . ? N2 C1B C2B N3 164.5(2) . . . . ? C3B C1B C2B N3 -75.1(3) . . . . ? N2 C1B C3B C4B -63.8(3) . . . . ? C2B C1B C3B C4B 176.5(3) . . . . ? C2B N3 C2C C3C 95.4(3) . . . . ? C1C N3 C2C C3C -82.3(3) . . . . ? C1D N4 C3C O3 -174.2(3) . . . . ? C2D N4 C3C O3 -4.4(4) . . . . ? C1D N4 C3C C2C 6.3(4) . . . . ? C2D N4 C3C C2C 176.2(2) . . . . ? N3 C2C C3C O3 -5.4(3) . . . . ? N3 C2C C3C N4 174.1(2) . . . . ? C3C N4 C2D C3D -95.0(2) . . . . ? C1D N4 C2D C3D 75.2(3) . . . . ? C3C N4 C2D C4D 142.2(2) . . . . ? C1D N4 C2D C4D -47.6(3) . . . . ? C1E N5 C3D O4 5.1(4) . . . . ? C1E N5 C3D C2D -171.5(2) . . . . ? N4 C2D C3D O4 -78.7(3) . . . . ? C4D C2D C3D O4 44.5(3) . . . . ? N4 C2D C3D N5 97.9(3) . . . . ? C4D C2D C3D N5 -138.9(2) . . . . ? N4 C2D C4D C5D -65.2(3) . . . . ? C3D C2D C4D C5D 174.9(2) . . . . ? C2D C4D C5D C6D 160.3(3) . . . . ? C2D C4D C5D C7D -77.9(3) . . . . ? C3D N5 C1E C3E 97.2(3) . . . . ? C3D N5 C1E C2E -141.2(2) . . . . ? C1F N6 C2E O5 168.3(3) . . . . ? C2F N6 C2E O5 -3.7(4) . . . . ? C1F N6 C2E C1E -16.2(4) . . . . ? C2F N6 C2E C1E 171.8(2) . . . . ? N5 C1E C2E O5 -23.2(3) . . . . ? C3E C1E C2E O5 99.6(3) . . . . ? N5 C1E C2E N6 161.3(2) . . . . ? C3E C1E C2E N6 -76.0(3) . . . . ? N5 C1E C3E C5E 61.0(3) . . . . ? C2E C1E C3E C5E -59.4(4) . . . . ? N5 C1E C3E C4E -63.2(4) . . . . ? C2E C1E C3E C4E 176.4(3) . . . . ? C2E N6 C2F C4F -72.0(3) . . . . ? C1F N6 C2F C4F 115.4(3) . . . . ? C2E N6 C2F C3F 60.3(3) . . . . ? C1F N6 C2F C3F -112.3(3) . . . . ? C1G N7 C3F O6 -0.2(4) . . . . ? C1G N7 C3F C2F -178.7(2) . . . . ? N6 C2F C3F O6 43.1(3) . . . . ? C4F C2F C3F O6 172.4(3) . . . . ? N6 C2F C3F N7 -138.3(2) . . . . ? C4F C2F C3F N7 -9.1(4) . . . . ? N6 C2F C4F C5F -53.1(4) . . . . ? C3F C2F C4F C5F 179.9(3) . . . . ? C2F C4F C5F C7F 173.7(3) . . . . ? C2F C4F C5F C6F -60.9(4) . . . . ? C3F N7 C1G C3G 157.0(3) . . . . ? C3F N7 C1G C2G -77.3(3) . . . . ? C1H N8 C2G O7 -10.8(4) . . . . ? C1H N8 C2G C1G 169.6(2) . . . . ? N7 C1G C2G O7 178.9(3) . . . . ? C3G C1G C2G O7 -54.6(4) . . . . ? N7 C1G C2G N8 -1.5(4) . . . . ? C3G C1G C2G N8 125.0(3) . . . . ? C2G N8 C1H C2H 143.2(2) . . . . ? C2G N8 C1H C3H -94.1(3) . . . . ? C1I N9 C2H O8 177.6(2) . . . . ? C2I N9 C2H O8 0.2(4) . . . . ? C1I N9 C2H C1H -4.8(3) . . . . ? C2I N9 C2H C1H 177.8(2) . . . . ? N8 C1H C2H O8 101.6(3) . . . . ? C3H C1H C2H O8 -20.4(3) . . . . ? N8 C1H C2H N9 -76.0(3) . . . . ? C3H C1H C2H N9 161.9(2) . . . . ? C2H N9 C2I C3I -129.2(2) . . . . ? C1I N9 C2I C3I 53.3(3) . . . . ? C2H N9 C2I C4I 107.8(3) . . . . ? C1I N9 C2I C4I -69.7(3) . . . . ? C1J N10 C3I O9 177.8(2) . . . . ? C2J N10 C3I O9 13.6(4) . . . . ? C1J N10 C3I C2I -0.9(4) . . . . ? C2J N10 C3I C2I -165.1(2) . . . . ? N9 C2I C3I O9 -115.3(3) . . . . ? C4I C2I C3I O9 8.4(4) . . . . ? N9 C2I C3I N10 63.4(3) . . . . ? C4I C2I C3I N10 -172.9(2) . . . . ? N9 C2I C4I C5I -62.3(3) . . . . ? C3I C2I C4I C5I 175.9(2) . . . . ? C2I C4I C5I C7I -73.3(4) . . . . ? C2I C4I C5I C6I 162.5(3) . . . . ? C3I N10 C2J C4J 95.5(3) . . . . ? C1J N10 C2J C4J -69.7(3) . . . . ? C3I N10 C2J C3J -140.6(2) . . . . ? C1J N10 C2J C3J 54.2(3) . . . . ? C2K N11 C3J O10 -2.6(4) . . . . ? C1K N11 C3J O10 177.7(3) . . . . ? C2K N11 C3J C2J 177.6(2) . . . . ? C1K N11 C3J C2J -2.0(4) . . . . ? N10 C2J C3J O10 -99.6(3) . . . . ? C4J C2J C3J O10 23.7(4) . . . . ? N10 C2J C3J N11 80.2(3) . . . . ? C4J C2J C3J N11 -156.5(2) . . . . ? N10 C2J C4J C5J -160.8(3) . . . . ? C3J C2J C4J C5J 75.8(4) . . . . ? C2J C4J C5J C6J -176.4(4) . . . . ? C2J C4J C5J C7J 61.9(4) . . . . ? C3J N11 C2K C3K 134.0(2) . . . . ? C1K N11 C2K C3K -46.3(3) . . . . ? C3J N11 C2K C4K -99.1(3) . . . . ? C1K N11 C2K C4K 80.6(3) . . . . ? C2A N1 C3K O11 -3.8(4) . . . . ? C1A N1 C3K O11 -165.1(3) . . . . ? C2A N1 C3K C2K 178.6(2) . . . . ? C1A N1 C3K C2K 17.3(4) . . . . ? N11 C2K C3K O11 102.4(3) . . . . ? C4K C2K C3K O11 -25.4(4) . . . . ? N11 C2K C3K N1 -80.0(3) . . . . ? C4K C2K C3K N1 152.2(3) . . . . ? N11 C2K C4K C5K 173.8(3) . . . . ? C3K C2K C4K C5K -60.5(4) . . . . ? N11 C2K C4K C6K 50.6(4) . . . . ? C3K C2K C4K C6K 176.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H1 OW3 0.86 2.16 2.981(3) 160.0 2_664 N5 H2 O8 0.86 2.37 3.150(3) 150.2 . N7 H3 OW2 0.86 2.20 2.982(4) 150.2 3_656 N8 H4 O5 0.86 2.17 2.918(3) 145.4 . O12 H5 O2 0.82 2.02 2.814(3) 162.3 . O12 H5 N2 0.82 2.54 3.068(3) 122.9 . OW1 HW11 O1 0.885(2) 1.8719(19) 2.740(3) 166.48(15) . OW1 HW12 O3 0.779(2) 2.0562(17) 2.828(3) 170.77(15) . OW2 HW21 O11 0.965(3) 1.975(2) 2.918(4) 165.04(19) . OW2 HW22 OW5 0.912(3) 1.947(4) 2.854(5) 173.2(2) 3_646 OW3 HW31 O9 0.906(3) 2.094(2) 2.964(3) 160.71(19) . OW3 HW32 OW7 0.897(3) 1.936(7) 2.825(7) 171.1(3) 3_746 OW4 HW41 OW1 0.844(3) 1.962(2) 2.775(4) 161.5(2) 3_756 OW4 HW42 O4 0.828(3) 2.1310(19) 2.764(3) 133.1(3) . OW5 HW51 O10 0.835(4) 2.0652(19) 2.859(4) 158.5(3) . OW5 HW52 OW6 0.866(4) 1.929(5) 2.755(7) 159.2(3) 3_656 OW6 HW61 OW4 0.916(6) 1.966(4) 2.812(7) 152.9(3) 3_746 OW6 HW62 O1 0.859(5) 2.424(2) 3.220(5) 154.4(4) . OW7 HW71 OW4 0.824(8) 2.218(3) 2.873(8) 136.5(6) . OW7 HW72 OW5 0.852(8) 2.322(4) 3.174(9) 178.2(6) 1_655 _diffrn_measured_fraction_theta_max 0.840 _diffrn_reflns_theta_full 74.61 _diffrn_measured_fraction_theta_full 0.840 _refine_diff_density_max 0.340 _refine_diff_density_min -0.161 _refine_diff_density_rms 0.043