# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Hiromitsu Maeda' _publ_contact_author_email MAEDAHIR@PH.RITSUMEI.AC.JP _publ_section_title ; Diol-substituted boron complexes of dipyrrolyldiketones as anion receptors and covalently linked 'pivotal' dimers ; loop_ _publ_author_name 'Hiromitsu Maeda' 'Yasunobu Fujii' 'Yuta Mihashi' # Attachment 'BO2_HMaeda_CIF.CIF' data_shelxl1 _database_code_depnum_ccdc_archive 'CCDC 684820' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H13 B N2 O4' _chemical_formula_weight 320.10 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' B B 0.0013 0.0007 '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 n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y, z+1/2' _cell_length_a 9.035(3) _cell_length_b 18.435(7) _cell_length_c 8.794(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1464.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 10575 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9597 _exptl_absorpt_correction_T_max 0.9897 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13780 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3346 _reflns_number_gt 2728 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.6.0' _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^)+(0.0397P)^2^+0.0819P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.2(9) _refine_ls_number_reflns 3346 _refine_ls_number_parameters 218 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 O1 O 0.75780(15) 0.40449(7) 0.56610(14) 0.0231(3) Uani 1 1 d . . . O2 O 0.98998(15) 0.33904(7) 0.57229(15) 0.0220(3) Uani 1 1 d . . . O3 O 0.77988(16) 0.29158(7) 0.43456(14) 0.0225(3) Uani 1 1 d . . . O4 O 0.90664(15) 0.39306(7) 0.33862(15) 0.0230(3) Uani 1 1 d . . . N1 N 0.56943(18) 0.50849(9) 0.65727(18) 0.0269(4) Uani 1 1 d . . . H1 H 0.5342 0.4799 0.5858 0.032 Uiso 1 1 calc R . . N2 N 1.27602(18) 0.32019(9) 0.66475(18) 0.0228(4) Uani 1 1 d . . . H2 H 1.2488 0.2887 0.5949 0.027 Uiso 1 1 calc R . . C1 C 0.4933(3) 0.56205(12) 0.7260(3) 0.0326(5) Uani 1 1 d . . . H1A H 0.3935 0.5750 0.7053 0.039 Uiso 1 1 calc R . . C2 C 0.5840(3) 0.59472(11) 0.8309(3) 0.0338(5) Uani 1 1 d . . . H2A H 0.5584 0.6339 0.8960 0.041 Uiso 1 1 calc R . . C3 C 0.7212(2) 0.55958(11) 0.8241(2) 0.0299(5) Uani 1 1 d . . . H3 H 0.8062 0.5709 0.8831 0.036 Uiso 1 1 calc R . . C4 C 0.7105(2) 0.50516(11) 0.7155(2) 0.0227(4) Uani 1 1 d . . . C5 C 0.8131(2) 0.45264(10) 0.6620(2) 0.0204(4) Uani 1 1 d . . . C6 C 0.9603(2) 0.44889(11) 0.7071(2) 0.0215(4) Uani 1 1 d . . . H6 H 1.0027 0.4868 0.7660 0.026 Uiso 1 1 calc R . . C7 C 1.0447(2) 0.38920(10) 0.66528(19) 0.0189(4) Uani 1 1 d . . . C8 C 1.1900(2) 0.37631(11) 0.7192(2) 0.0207(4) Uani 1 1 d . . . C9 C 1.2739(2) 0.41237(11) 0.8288(2) 0.0255(4) Uani 1 1 d . . . H9 H 1.2437 0.4535 0.8861 0.031 Uiso 1 1 calc R . . C10 C 1.4098(2) 0.37724(11) 0.8389(3) 0.0300(5) Uani 1 1 d . . . H10 H 1.4891 0.3896 0.9050 0.036 Uiso 1 1 calc R . . C11 C 1.4079(2) 0.32110(11) 0.7352(2) 0.0269(5) Uani 1 1 d . . . H11 H 1.4871 0.2884 0.7166 0.032 Uiso 1 1 calc R . . C12 C 0.7700(2) 0.29372(11) 0.2780(2) 0.0199(4) Uani 1 1 d . . . C13 C 0.6944(2) 0.24712(11) 0.1852(2) 0.0253(5) Uani 1 1 d . . . H13 H 0.6408 0.2070 0.2250 0.030 Uiso 1 1 calc R . . C14 C 0.6997(2) 0.26138(12) 0.0286(2) 0.0291(5) Uani 1 1 d . . . H14 H 0.6480 0.2305 -0.0397 0.035 Uiso 1 1 calc R . . C15 C 0.7789(3) 0.31960(12) -0.0283(2) 0.0288(5) Uani 1 1 d . . . H15 H 0.7820 0.3273 -0.1351 0.035 Uiso 1 1 calc R . . C16 C 0.8545(2) 0.36734(11) 0.0681(2) 0.0234(4) Uani 1 1 d . . . H16 H 0.9085 0.4075 0.0296 0.028 Uiso 1 1 calc R . . C17 C 0.8465(2) 0.35314(11) 0.2209(2) 0.0197(4) Uani 1 1 d . . . B1 B 0.8597(3) 0.35689(13) 0.4785(2) 0.0220(5) Uani 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 0.0214(8) 0.0225(8) 0.0255(7) -0.0010(6) -0.0049(6) -0.0004(6) O2 0.0245(8) 0.0184(7) 0.0232(6) -0.0030(6) -0.0044(5) -0.0004(6) O3 0.0294(8) 0.0196(7) 0.0185(7) 0.0025(6) -0.0028(6) -0.0047(6) O4 0.0253(7) 0.0207(7) 0.0231(6) -0.0003(6) -0.0031(6) -0.0051(6) N1 0.0227(9) 0.0279(9) 0.0299(9) -0.0009(8) -0.0015(7) 0.0022(7) N2 0.0254(9) 0.0211(9) 0.0219(8) -0.0041(7) -0.0030(7) 0.0013(7) C1 0.0246(12) 0.0323(12) 0.0407(11) 0.0013(10) 0.0041(9) 0.0066(9) C2 0.0364(13) 0.0295(11) 0.0355(11) -0.0026(11) 0.0058(10) 0.0081(10) C3 0.0320(12) 0.0283(11) 0.0295(11) -0.0034(10) -0.0023(9) 0.0011(9) C4 0.0233(11) 0.0210(10) 0.0238(9) 0.0060(9) 0.0026(8) 0.0005(8) C5 0.0244(11) 0.0176(10) 0.0191(9) 0.0038(8) -0.0001(7) -0.0024(8) C6 0.0235(11) 0.0206(10) 0.0205(9) -0.0018(8) 0.0009(7) -0.0013(8) C7 0.0233(10) 0.0178(9) 0.0155(8) 0.0022(8) 0.0008(7) -0.0041(8) C8 0.0250(11) 0.0173(9) 0.0198(8) -0.0007(8) 0.0004(7) 0.0019(8) C9 0.0264(11) 0.0229(10) 0.0273(10) -0.0066(9) -0.0026(9) -0.0003(8) C10 0.0270(11) 0.0305(11) 0.0327(10) -0.0037(11) -0.0072(9) 0.0002(9) C11 0.0225(12) 0.0257(11) 0.0327(11) -0.0009(9) -0.0019(9) 0.0036(9) C12 0.0197(11) 0.0191(10) 0.0210(9) 0.0004(8) -0.0018(8) 0.0033(8) C13 0.0262(12) 0.0230(11) 0.0268(11) -0.0015(9) -0.0043(8) -0.0025(8) C14 0.0337(13) 0.0284(12) 0.0252(10) -0.0065(9) -0.0072(8) -0.0008(10) C15 0.0330(13) 0.0343(13) 0.0191(9) 0.0003(9) -0.0024(9) 0.0038(10) C16 0.0242(11) 0.0220(10) 0.0240(9) 0.0027(9) 0.0021(8) 0.0006(9) C17 0.0155(10) 0.0201(10) 0.0235(9) -0.0013(9) -0.0017(8) 0.0036(8) B1 0.0233(13) 0.0187(11) 0.0240(11) -0.0010(10) -0.0021(9) -0.0026(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 C5 1.322(2) . ? O1 B1 1.487(3) . ? O2 C7 1.330(2) . ? O2 B1 1.474(3) . ? O3 C12 1.381(2) . ? O3 B1 1.456(3) . ? O4 C17 1.381(2) . ? O4 B1 1.462(3) . ? N1 C1 1.346(3) . ? N1 C4 1.375(3) . ? N1 H1 0.8800 . ? N2 C11 1.343(3) . ? N2 C8 1.380(2) . ? N2 H2 0.8800 . ? C1 C2 1.373(3) . ? C1 H1A 0.9500 . ? C2 C3 1.400(3) . ? C2 H2A 0.9500 . ? C3 C4 1.388(3) . ? C3 H3 0.9500 . ? C4 C5 1.421(3) . ? C5 C6 1.390(3) . ? C6 C7 1.388(3) . ? C6 H6 0.9500 . ? C7 C8 1.415(3) . ? C8 C9 1.395(3) . ? C9 C10 1.391(3) . ? C9 H9 0.9500 . ? C10 C11 1.380(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.367(3) . ? C12 C17 1.389(3) . ? C13 C14 1.403(3) . ? C13 H13 0.9500 . ? C14 C15 1.384(3) . ? C14 H14 0.9500 . ? C15 C16 1.400(3) . ? C15 H15 0.9500 . ? C16 C17 1.371(3) . ? C16 H16 0.9500 . ? 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 C5 O1 B1 119.51(15) . . ? C7 O2 B1 119.05(16) . . ? C12 O3 B1 105.85(15) . . ? C17 O4 B1 105.87(14) . . ? C1 N1 C4 109.83(18) . . ? C1 N1 H1 125.1 . . ? C4 N1 H1 125.1 . . ? C11 N2 C8 109.31(17) . . ? C11 N2 H2 125.3 . . ? C8 N2 H2 125.3 . . ? N1 C1 C2 108.5(2) . . ? N1 C1 H1A 125.7 . . ? C2 C1 H1A 125.7 . . ? C1 C2 C3 107.3(2) . . ? C1 C2 H2A 126.4 . . ? C3 C2 H2A 126.4 . . ? C4 C3 C2 107.6(2) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? N1 C4 C3 106.75(18) . . ? N1 C4 C5 120.77(18) . . ? C3 C4 C5 132.5(2) . . ? O1 C5 C6 120.68(17) . . ? O1 C5 C4 114.99(17) . . ? C6 C5 C4 124.31(18) . . ? C7 C6 C5 119.31(18) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? O2 C7 C6 120.64(17) . . ? O2 C7 C8 115.72(17) . . ? C6 C7 C8 123.62(17) . . ? N2 C8 C9 106.91(17) . . ? N2 C8 C7 122.16(17) . . ? C9 C8 C7 130.93(18) . . ? C10 C9 C8 107.60(18) . . ? C10 C9 H9 126.2 . . ? C8 C9 H9 126.2 . . ? C11 C10 C9 107.21(19) . . ? C11 C10 H10 126.4 . . ? C9 C10 H10 126.4 . . ? N2 C11 C10 108.97(19) . . ? N2 C11 H11 125.5 . . ? C10 C11 H11 125.5 . . ? C13 C12 O3 127.52(18) . . ? C13 C12 C17 121.93(17) . . ? O3 C12 C17 110.52(17) . . ? C12 C13 C14 116.77(19) . . ? C12 C13 H13 121.6 . . ? C14 C13 H13 121.6 . . ? C15 C14 C13 121.20(19) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 121.41(18) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C17 C16 C15 116.61(19) . . ? C17 C16 H16 121.7 . . ? C15 C16 H16 121.7 . . ? C16 C17 O4 127.75(18) . . ? C16 C17 C12 122.05(17) . . ? O4 C17 C12 110.20(16) . . ? O3 B1 O4 107.31(15) . . ? O3 B1 O2 111.06(17) . . ? O4 B1 O2 109.94(17) . . ? O3 B1 O1 108.59(17) . . ? O4 B1 O1 110.26(17) . . ? O2 B1 O1 109.65(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C2 0.0(2) . . . . ? N1 C1 C2 C3 0.5(3) . . . . ? C1 C2 C3 C4 -0.7(3) . . . . ? C1 N1 C4 C3 -0.4(2) . . . . ? C1 N1 C4 C5 179.71(18) . . . . ? C2 C3 C4 N1 0.7(2) . . . . ? C2 C3 C4 C5 -179.5(2) . . . . ? B1 O1 C5 C6 -14.3(3) . . . . ? B1 O1 C5 C4 167.39(16) . . . . ? N1 C4 C5 O1 -6.4(3) . . . . ? C3 C4 C5 O1 173.8(2) . . . . ? N1 C4 C5 C6 175.33(18) . . . . ? C3 C4 C5 C6 -4.5(3) . . . . ? O1 C5 C6 C7 -7.7(3) . . . . ? C4 C5 C6 C7 170.51(17) . . . . ? B1 O2 C7 C6 18.1(2) . . . . ? B1 O2 C7 C8 -163.26(17) . . . . ? C5 C6 C7 O2 5.7(3) . . . . ? C5 C6 C7 C8 -172.74(18) . . . . ? C11 N2 C8 C9 -0.5(2) . . . . ? C11 N2 C8 C7 179.73(18) . . . . ? O2 C7 C8 N2 7.6(3) . . . . ? C6 C7 C8 N2 -173.87(17) . . . . ? O2 C7 C8 C9 -172.1(2) . . . . ? C6 C7 C8 C9 6.5(3) . . . . ? N2 C8 C9 C10 -0.1(2) . . . . ? C7 C8 C9 C10 179.6(2) . . . . ? C8 C9 C10 C11 0.6(3) . . . . ? C8 N2 C11 C10 0.9(2) . . . . ? C9 C10 C11 N2 -1.0(2) . . . . ? B1 O3 C12 C13 -174.3(2) . . . . ? B1 O3 C12 C17 4.0(2) . . . . ? O3 C12 C13 C14 179.19(19) . . . . ? C17 C12 C13 C14 1.1(3) . . . . ? C12 C13 C14 C15 0.5(3) . . . . ? C13 C14 C15 C16 -1.2(3) . . . . ? C14 C15 C16 C17 0.3(3) . . . . ? C15 C16 C17 O4 -177.65(19) . . . . ? C15 C16 C17 C12 1.2(3) . . . . ? B1 O4 C17 C16 177.1(2) . . . . ? B1 O4 C17 C12 -1.9(2) . . . . ? C13 C12 C17 C16 -2.0(3) . . . . ? O3 C12 C17 C16 179.61(18) . . . . ? C13 C12 C17 O4 177.04(18) . . . . ? O3 C12 C17 O4 -1.3(2) . . . . ? C12 O3 B1 O4 -5.0(2) . . . . ? C12 O3 B1 O2 -125.23(17) . . . . ? C12 O3 B1 O1 114.13(17) . . . . ? C17 O4 B1 O3 4.3(2) . . . . ? C17 O4 B1 O2 125.18(17) . . . . ? C17 O4 B1 O1 -113.82(17) . . . . ? C7 O2 B1 O3 -156.50(15) . . . . ? C7 O2 B1 O4 84.9(2) . . . . ? C7 O2 B1 O1 -36.5(2) . . . . ? C5 O1 B1 O3 156.18(15) . . . . ? C5 O1 B1 O4 -86.51(19) . . . . ? C5 O1 B1 O2 34.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.154 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.042 #============================================================================== # End of CIF #============================================================================== data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 684821' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H29 B N2 O4' _chemical_formula_sum 'C25 H29 B N2 O4' _chemical_formula_weight 432.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 23.638(8) _cell_length_b 23.638(8) _cell_length_c 16.043(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8964(5) _cell_formula_units_Z 16 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 20788 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.6 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3680 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9705 _exptl_absorpt_correction_T_max 0.9872 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41224 _diffrn_reflns_av_R_equivalents 0.1761 _diffrn_reflns_av_sigmaI/netI 0.1178 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5121 _reflns_number_gt 3426 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.6.0' _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^)+(0.0717P)^2^+1.4588P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5121 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1616 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 O1 O 0.14012(6) 0.03257(6) 0.66809(8) 0.0242(4) Uani 1 1 d . . . O2 O 0.15132(6) 0.05602(6) 0.81496(8) 0.0246(4) Uani 1 1 d . . . O3 O 0.23085(6) 0.06236(6) 0.72183(8) 0.0218(3) Uani 1 1 d . . . O4 O 0.19587(6) -0.02682(6) 0.75766(8) 0.0219(3) Uani 1 1 d . . . N1 N 0.08702(7) 0.03321(7) 0.52278(10) 0.0219(4) Uani 1 1 d . . . H1A H 0.1175 0.0119 0.5248 0.026 Uiso 1 1 calc R . . N2 N 0.11526(7) 0.08811(7) 0.96267(10) 0.0238(4) Uani 1 1 d . . . H2A H 0.1518 0.0815 0.9590 0.029 Uiso 1 1 calc R . . C1 C 0.05720(9) 0.04427(9) 0.45348(12) 0.0226(5) Uani 1 1 d . . . H1 H 0.0656 0.0302 0.3994 0.027 Uiso 1 1 calc R . . C2 C 0.01236(9) 0.07941(9) 0.47333(12) 0.0227(5) Uani 1 1 d . . . C3 C 0.01594(9) 0.08994(9) 0.55966(12) 0.0236(5) Uani 1 1 d . . . C4 C 0.06302(8) 0.05994(9) 0.58992(11) 0.0202(4) Uani 1 1 d . . . C5 C 0.09046(8) 0.05737(9) 0.66886(12) 0.0201(4) Uani 1 1 d . . . C6 C 0.06785(9) 0.07804(9) 0.74298(12) 0.0232(5) Uani 1 1 d . . . H6 H 0.0311 0.0944 0.7435 0.028 Uiso 1 1 calc R . . C7 C 0.09892(8) 0.07472(8) 0.81592(12) 0.0207(4) Uani 1 1 d . . . C8 C 0.07833(9) 0.08986(9) 0.89641(12) 0.0212(5) Uani 1 1 d . . . C9 C 0.02469(9) 0.10163(9) 0.92895(12) 0.0246(5) Uani 1 1 d . . . C10 C 0.03075(10) 0.10698(10) 1.01587(13) 0.0272(5) Uani 1 1 d . . . C11 C 0.08702(10) 0.09805(9) 1.03388(12) 0.0270(5) Uani 1 1 d . . . H11 H 0.1033 0.0988 1.0880 0.032 Uiso 1 1 calc R . . C12 C -0.03060(9) 0.10246(10) 0.41423(12) 0.0283(5) Uani 1 1 d . . . H12A H -0.0331 0.1439 0.4220 0.034 Uiso 1 1 calc R . . H12B H -0.0680 0.0862 0.4282 0.034 Uiso 1 1 calc R . . C13 C -0.01778(11) 0.09024(11) 0.32348(13) 0.0381(6) Uani 1 1 d . . . H13A H -0.0475 0.1066 0.2884 0.046 Uiso 1 1 calc R . . H13B H -0.0164 0.0492 0.3147 0.046 Uiso 1 1 calc R . . H13C H 0.0188 0.1069 0.3086 0.046 Uiso 1 1 calc R . . C14 C -0.02353(9) 0.12795(10) 0.60690(13) 0.0291(5) Uani 1 1 d . . . H14A H -0.0400 0.1560 0.5680 0.035 Uiso 1 1 calc R . . H14B H -0.0018 0.1489 0.6498 0.035 Uiso 1 1 calc R . . C15 C -0.07061(10) 0.09578(11) 0.64850(14) 0.0351(6) Uani 1 1 d . . . H15A H -0.0950 0.1222 0.6788 0.042 Uiso 1 1 calc R . . H15B H -0.0546 0.0683 0.6877 0.042 Uiso 1 1 calc R . . H15C H -0.0929 0.0758 0.6062 0.042 Uiso 1 1 calc R . . C16 C -0.02979(9) 0.10908(11) 0.88263(13) 0.0327(6) Uani 1 1 d . . . H16A H -0.0617 0.1001 0.9203 0.039 Uiso 1 1 calc R . . H16B H -0.0310 0.0821 0.8355 0.039 Uiso 1 1 calc R . . C17 C -0.03686(12) 0.16897(12) 0.84946(16) 0.0486(7) Uani 1 1 d . . . H17A H -0.0728 0.1719 0.8193 0.058 Uiso 1 1 calc R . . H17B H -0.0056 0.1779 0.8116 0.058 Uiso 1 1 calc R . . H17C H -0.0368 0.1957 0.8961 0.058 Uiso 1 1 calc R . . C18 C -0.01571(10) 0.11376(11) 1.07888(14) 0.0351(6) Uani 1 1 d . . . H18A H -0.0464 0.1370 1.0546 0.042 Uiso 1 1 calc R . . H18B H -0.0008 0.1339 1.1283 0.042 Uiso 1 1 calc R . . C19 C -0.03964(11) 0.05644(11) 1.10589(14) 0.0392(6) Uani 1 1 d . . . H19A H -0.0698 0.0623 1.1470 0.047 Uiso 1 1 calc R . . H19B H -0.0094 0.0336 1.1308 0.047 Uiso 1 1 calc R . . H19C H -0.0551 0.0367 1.0572 0.047 Uiso 1 1 calc R . . C20 C 0.27429(9) 0.02391(9) 0.72795(12) 0.0211(5) Uani 1 1 d . . . C21 C 0.33077(9) 0.03288(9) 0.71507(12) 0.0242(5) Uani 1 1 d . . . H21 H 0.3449 0.0690 0.6996 0.029 Uiso 1 1 calc R . . C22 C 0.36646(9) -0.01323(10) 0.72563(13) 0.0287(5) Uani 1 1 d . . . H22 H 0.4060 -0.0085 0.7174 0.034 Uiso 1 1 calc R . . C23 C 0.34598(10) -0.06559(10) 0.74767(13) 0.0276(5) Uani 1 1 d . . . H23 H 0.3715 -0.0962 0.7545 0.033 Uiso 1 1 calc R . . C24 C 0.28847(9) -0.07434(9) 0.76005(12) 0.0244(5) Uani 1 1 d . . . H24 H 0.2740 -0.1104 0.7750 0.029 Uiso 1 1 calc R . . C25 C 0.25341(9) -0.02863(9) 0.74968(12) 0.0200(4) Uani 1 1 d . . . B1 B 0.17869(10) 0.03152(10) 0.74067(14) 0.0205(5) Uani 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 0.0189(8) 0.0268(9) 0.0268(8) -0.0047(6) -0.0029(6) 0.0048(6) O2 0.0188(8) 0.0284(9) 0.0265(8) -0.0056(6) -0.0028(6) 0.0045(6) O3 0.0185(8) 0.0179(8) 0.0290(8) -0.0001(6) -0.0018(6) 0.0021(6) O4 0.0174(8) 0.0190(8) 0.0292(8) -0.0007(6) -0.0016(6) 0.0009(6) N1 0.0171(9) 0.0236(10) 0.0250(9) -0.0021(7) 0.0013(7) 0.0029(7) N2 0.0192(10) 0.0268(10) 0.0254(9) 0.0004(7) -0.0027(7) 0.0021(8) C1 0.0236(12) 0.0239(12) 0.0203(10) -0.0004(8) 0.0013(8) -0.0013(9) C2 0.0211(11) 0.0231(12) 0.0240(11) 0.0022(8) 0.0002(8) -0.0031(9) C3 0.0207(11) 0.0274(12) 0.0228(11) -0.0004(9) 0.0002(8) 0.0004(9) C4 0.0171(11) 0.0221(11) 0.0215(10) 0.0007(8) 0.0013(8) -0.0007(8) C5 0.0149(10) 0.0189(11) 0.0266(11) 0.0026(8) -0.0008(8) -0.0007(8) C6 0.0187(11) 0.0276(12) 0.0233(11) 0.0007(8) 0.0018(8) 0.0031(9) C7 0.0169(11) 0.0177(11) 0.0275(11) 0.0011(8) -0.0002(8) -0.0001(8) C8 0.0188(11) 0.0235(11) 0.0212(10) 0.0019(8) -0.0025(8) 0.0022(9) C9 0.0217(12) 0.0279(12) 0.0243(11) -0.0003(9) 0.0003(8) 0.0013(9) C10 0.0292(13) 0.0280(13) 0.0244(11) -0.0013(9) 0.0000(9) 0.0019(10) C11 0.0326(13) 0.0306(13) 0.0177(10) -0.0009(9) 0.0003(9) -0.0004(10) C12 0.0241(12) 0.0338(13) 0.0270(11) 0.0044(9) -0.0031(9) 0.0026(10) C13 0.0355(15) 0.0538(17) 0.0249(12) 0.0038(11) -0.0048(10) 0.0059(12) C14 0.0260(13) 0.0358(14) 0.0256(12) 0.0018(9) -0.0025(9) 0.0085(10) C15 0.0272(13) 0.0434(16) 0.0346(13) -0.0042(11) 0.0002(10) 0.0055(11) C16 0.0197(12) 0.0520(16) 0.0265(12) -0.0045(10) 0.0002(9) 0.0063(11) C17 0.0453(17) 0.0529(18) 0.0476(15) -0.0107(13) -0.0136(12) 0.0241(14) C18 0.0331(14) 0.0456(16) 0.0266(12) -0.0034(10) 0.0058(10) 0.0045(11) C19 0.0349(15) 0.0543(18) 0.0284(13) 0.0016(11) 0.0046(10) -0.0040(12) C20 0.0196(11) 0.0226(11) 0.0211(10) -0.0029(8) -0.0029(8) 0.0035(9) C21 0.0210(11) 0.0273(12) 0.0242(11) -0.0023(9) 0.0003(8) -0.0011(9) C22 0.0182(11) 0.0368(14) 0.0311(12) -0.0056(10) 0.0016(9) 0.0009(10) C23 0.0240(12) 0.0281(13) 0.0306(12) -0.0047(9) -0.0041(9) 0.0108(10) C24 0.0273(12) 0.0222(12) 0.0238(11) -0.0012(8) -0.0033(9) 0.0039(9) C25 0.0179(11) 0.0216(11) 0.0205(10) -0.0019(8) -0.0019(8) 0.0007(9) B1 0.0181(12) 0.0199(12) 0.0234(12) -0.0023(9) -0.0025(9) 0.0017(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 C5 1.312(2) . ? O1 B1 1.479(3) . ? O2 C7 1.315(2) . ? O2 B1 1.475(3) . ? O3 C20 1.375(2) . ? O3 B1 1.464(3) . ? O4 C25 1.367(2) . ? O4 B1 1.463(3) . ? N1 C1 1.342(3) . ? N1 C4 1.372(2) . ? N1 H1A 0.8800 . ? N2 C11 1.344(3) . ? N2 C8 1.376(3) . ? N2 H2A 0.8800 . ? C1 C2 1.384(3) . ? C1 H1 0.9500 . ? C2 C3 1.410(3) . ? C2 C12 1.492(3) . ? C3 C4 1.406(3) . ? C3 C14 1.501(3) . ? C4 C5 1.424(3) . ? C5 C6 1.392(3) . ? C6 C7 1.384(3) . ? C6 H6 0.9500 . ? C7 C8 1.426(3) . ? C8 C9 1.399(3) . ? C9 C10 1.408(3) . ? C9 C16 1.497(3) . ? C10 C11 1.377(3) . ? C10 C18 1.501(3) . ? C11 H11 0.9500 . ? C12 C13 1.515(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.504(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.522(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.531(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.367(3) . ? C20 C25 1.381(3) . ? C21 C22 1.389(3) . ? C21 H21 0.9500 . ? C22 C23 1.375(3) . ? C22 H22 0.9500 . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 C25 1.372(3) . ? C24 H24 0.9500 . ? 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 C5 O1 B1 123.47(16) . . ? C7 O2 B1 123.69(16) . . ? C20 O3 B1 106.56(16) . . ? C25 O4 B1 106.75(16) . . ? C1 N1 C4 110.09(18) . . ? C1 N1 H1A 125.0 . . ? C4 N1 H1A 125.0 . . ? C11 N2 C8 109.66(18) . . ? C11 N2 H2A 125.2 . . ? C8 N2 H2A 125.2 . . ? N1 C1 C2 109.19(18) . . ? N1 C1 H1 125.4 . . ? C2 C1 H1 125.4 . . ? C1 C2 C3 106.62(18) . . ? C1 C2 C12 126.46(19) . . ? C3 C2 C12 126.9(2) . . ? C4 C3 C2 107.32(18) . . ? C4 C3 C14 128.29(18) . . ? C2 C3 C14 124.37(19) . . ? N1 C4 C3 106.77(17) . . ? N1 C4 C5 119.36(18) . . ? C3 C4 C5 133.55(18) . . ? O1 C5 C6 120.54(18) . . ? O1 C5 C4 114.72(17) . . ? C6 C5 C4 124.73(19) . . ? C7 C6 C5 119.9(2) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? O2 C7 C6 120.59(18) . . ? O2 C7 C8 114.61(17) . . ? C6 C7 C8 124.79(19) . . ? N2 C8 C9 107.01(17) . . ? N2 C8 C7 118.40(18) . . ? C9 C8 C7 134.20(18) . . ? C8 C9 C10 107.17(18) . . ? C8 C9 C16 128.15(19) . . ? C10 C9 C16 124.65(19) . . ? C11 C10 C9 107.00(18) . . ? C11 C10 C18 125.6(2) . . ? C9 C10 C18 127.0(2) . . ? N2 C11 C10 109.16(18) . . ? N2 C11 H11 125.4 . . ? C10 C11 H11 125.4 . . ? C2 C12 C13 113.88(19) . . ? C2 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? C2 C12 H12B 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 C15 112.4(2) . . ? C3 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? C3 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C9 C16 C17 112.2(2) . . ? C9 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? C9 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 C19 111.5(2) . . ? C10 C18 H18A 109.3 . . ? C19 C18 H18A 109.3 . . ? C10 C18 H18B 109.3 . . ? C19 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 O3 128.01(19) . . ? C21 C20 C25 121.8(2) . . ? O3 C20 C25 110.22(18) . . ? C20 C21 C22 116.9(2) . . ? C20 C21 H21 121.5 . . ? C22 C21 H21 121.5 . . ? C23 C22 C21 121.6(2) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 121.0(2) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 117.2(2) . . ? C25 C24 H24 121.4 . . ? C23 C24 H24 121.4 . . ? O4 C25 C24 127.90(19) . . ? O4 C25 C20 110.56(17) . . ? C24 C25 C20 121.5(2) . . ? O4 B1 O3 105.90(17) . . ? O4 B1 O2 109.97(16) . . ? O3 B1 O2 109.92(17) . . ? O4 B1 O1 109.49(17) . . ? O3 B1 O1 110.37(17) . . ? O2 B1 O1 111.06(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C2 0.4(2) . . . . ? N1 C1 C2 C3 0.2(2) . . . . ? N1 C1 C2 C12 179.1(2) . . . . ? C1 C2 C3 C4 -0.7(2) . . . . ? C12 C2 C3 C4 -179.6(2) . . . . ? C1 C2 C3 C14 177.8(2) . . . . ? C12 C2 C3 C14 -1.1(3) . . . . ? C1 N1 C4 C3 -0.9(2) . . . . ? C1 N1 C4 C5 -175.25(18) . . . . ? C2 C3 C4 N1 0.9(2) . . . . ? C14 C3 C4 N1 -177.4(2) . . . . ? C2 C3 C4 C5 174.2(2) . . . . ? C14 C3 C4 C5 -4.2(4) . . . . ? B1 O1 C5 C6 -8.7(3) . . . . ? B1 O1 C5 C4 172.31(18) . . . . ? N1 C4 C5 O1 5.4(3) . . . . ? C3 C4 C5 O1 -167.2(2) . . . . ? N1 C4 C5 C6 -173.61(19) . . . . ? C3 C4 C5 C6 13.8(4) . . . . ? O1 C5 C6 C7 2.9(3) . . . . ? C4 C5 C6 C7 -178.21(19) . . . . ? B1 O2 C7 C6 -7.2(3) . . . . ? B1 O2 C7 C8 172.18(18) . . . . ? C5 C6 C7 O2 5.0(3) . . . . ? C5 C6 C7 C8 -174.2(2) . . . . ? C11 N2 C8 C9 0.1(2) . . . . ? C11 N2 C8 C7 -173.77(18) . . . . ? O2 C7 C8 N2 5.1(3) . . . . ? C6 C7 C8 N2 -175.54(19) . . . . ? O2 C7 C8 C9 -166.7(2) . . . . ? C6 C7 C8 C9 12.6(4) . . . . ? N2 C8 C9 C10 0.2(2) . . . . ? C7 C8 C9 C10 172.7(2) . . . . ? N2 C8 C9 C16 178.7(2) . . . . ? C7 C8 C9 C16 -8.8(4) . . . . ? C8 C9 C10 C11 -0.4(3) . . . . ? C16 C9 C10 C11 -179.0(2) . . . . ? C8 C9 C10 C18 -173.4(2) . . . . ? C16 C9 C10 C18 8.1(4) . . . . ? C8 N2 C11 C10 -0.4(2) . . . . ? C9 C10 C11 N2 0.5(3) . . . . ? C18 C10 C11 N2 173.6(2) . . . . ? C1 C2 C12 C13 -7.4(3) . . . . ? C3 C2 C12 C13 171.3(2) . . . . ? C4 C3 C14 C15 -85.3(3) . . . . ? C2 C3 C14 C15 96.5(2) . . . . ? C8 C9 C16 C17 -83.8(3) . . . . ? C10 C9 C16 C17 94.5(3) . . . . ? C11 C10 C18 C19 -86.1(3) . . . . ? C9 C10 C18 C19 85.6(3) . . . . ? B1 O3 C20 C21 179.4(2) . . . . ? B1 O3 C20 C25 -0.4(2) . . . . ? O3 C20 C21 C22 179.71(18) . . . . ? C25 C20 C21 C22 -0.6(3) . . . . ? C20 C21 C22 C23 0.3(3) . . . . ? C21 C22 C23 C24 0.2(3) . . . . ? C22 C23 C24 C25 -0.3(3) . . . . ? B1 O4 C25 C24 179.77(19) . . . . ? B1 O4 C25 C20 -0.7(2) . . . . ? C23 C24 C25 O4 179.43(18) . . . . ? C23 C24 C25 C20 -0.1(3) . . . . ? C21 C20 C25 O4 -179.05(17) . . . . ? O3 C20 C25 O4 0.7(2) . . . . ? C21 C20 C25 C24 0.5(3) . . . . ? O3 C20 C25 C24 -179.75(17) . . . . ? C25 O4 B1 O3 0.46(19) . . . . ? C25 O4 B1 O2 -118.26(17) . . . . ? C25 O4 B1 O1 119.45(17) . . . . ? C20 O3 B1 O4 -0.06(19) . . . . ? C20 O3 B1 O2 118.68(17) . . . . ? C20 O3 B1 O1 -118.48(17) . . . . ? C7 O2 B1 O4 -119.6(2) . . . . ? C7 O2 B1 O3 124.16(19) . . . . ? C7 O2 B1 O1 1.7(3) . . . . ? C5 O1 B1 O4 127.95(19) . . . . ? C5 O1 B1 O3 -115.8(2) . . . . ? C5 O1 B1 O2 6.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.265 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.059 #============================================================================== # End of CIF #============================================================================== data_70111mae _database_code_depnum_ccdc_archive 'CCDC 684822' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H37 B N2 O4' _chemical_formula_sum 'C25 H37 B N2 O4' _chemical_formula_weight 440.38 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' B B 0.0013 0.0007 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.663(3) _cell_length_b 14.346(4) _cell_length_c 27.938(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.864(9) _cell_angle_gamma 90.00 _cell_volume 5049(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 30772 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9625 _exptl_absorpt_correction_T_max 0.9923 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47101 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11492 _reflns_number_gt 7778 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+1.4296P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11492 _refine_ls_number_parameters 604 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.042 _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 0.69897(12) 0.72329(11) 0.29704(5) 0.0250(3) Uani 1 1 d . . . H1 H 0.6367 0.6979 0.2884 0.030 Uiso 1 1 calc R . . N2 N 0.95637(12) 0.78851(12) 0.10675(6) 0.0321(4) Uani 1 1 d . . . H2 H 0.9745 0.8233 0.1322 0.039 Uiso 1 1 calc R . . N3 N 0.72544(11) 0.50898(10) 0.20081(5) 0.0226(3) Uani 1 1 d . . . H3 H 0.6601 0.5300 0.2006 0.027 Uiso 1 1 calc R . . N4 N 0.90361(11) 0.40185(11) 0.42575(5) 0.0239(3) Uani 1 1 d . . . H4 H 0.9380 0.3796 0.4024 0.029 Uiso 1 1 calc R . . O1 O 0.64901(9) 0.71160(9) 0.20178(4) 0.0241(3) Uani 1 1 d . . . O2 O 0.69208(9) 0.70839(9) 0.11827(4) 0.0263(3) Uani 1 1 d . . . O3 O 0.55840(9) 0.60561(9) 0.14601(4) 0.0260(3) Uani 1 1 d . . . O4 O 0.52214(9) 0.76346(9) 0.13560(4) 0.0240(3) Uani 1 1 d . . . O5 O 0.64712(9) 0.50993(9) 0.28511(4) 0.0235(3) Uani 1 1 d . . . O6 O 0.66278(9) 0.50963(9) 0.37287(4) 0.0267(3) Uani 1 1 d . . . O7 O 0.53743(9) 0.61044(9) 0.32540(5) 0.0278(3) Uani 1 1 d . . . O8 O 0.50414(9) 0.45181(9) 0.33033(4) 0.0247(3) Uani 1 1 d . . . B1 B 0.60555(16) 0.69681(15) 0.15043(7) 0.0243(4) Uani 1 1 d . . . B2 B 0.58745(15) 0.52058(15) 0.32829(7) 0.0239(4) Uani 1 1 d . . . C1 C 0.73655(15) 0.74500(14) 0.34239(6) 0.0291(4) Uani 1 1 d . . . H5 H 0.7005 0.7346 0.3701 0.035 Uiso 1 1 calc R . . C2 C 0.83587(15) 0.78483(13) 0.34232(6) 0.0277(4) Uani 1 1 d . . . C3 C 0.86024(14) 0.78586(12) 0.29441(6) 0.0235(4) Uani 1 1 d . . . C4 C 0.77283(13) 0.74698(12) 0.26624(6) 0.0219(4) Uani 1 1 d . . . C5 C 0.74837(13) 0.73572(12) 0.21556(6) 0.0217(4) Uani 1 1 d . . . C6 C 0.82062(14) 0.74744(13) 0.18193(6) 0.0243(4) Uani 1 1 d . . . H6 H 0.8915 0.7656 0.1922 0.029 Uiso 1 1 calc R . . C7 C 0.78999(13) 0.73289(12) 0.13366(6) 0.0225(4) Uani 1 1 d . . . C8 C 0.86290(14) 0.73926(13) 0.09794(6) 0.0255(4) Uani 1 1 d . . . C9 C 0.86537(15) 0.69240(14) 0.05414(6) 0.0295(4) Uani 1 1 d . . . C10 C 0.96334(16) 0.71457(18) 0.03692(7) 0.0407(5) Uani 1 1 d . . . C11 C 1.01584(16) 0.77450(19) 0.06965(7) 0.0442(6) Uani 1 1 d . . . H7 H 1.0832 0.8018 0.0667 0.053 Uiso 1 1 calc R . . C12 C 0.90293(17) 0.82646(17) 0.38458(7) 0.0396(5) Uani 1 1 d . . . H8 H 0.9098 0.8943 0.3792 0.048 Uiso 1 1 calc R . . H9 H 0.9749 0.7990 0.3863 0.048 Uiso 1 1 calc R . . C13 C 0.8584(2) 0.8110(3) 0.43224(8) 0.0728(10) Uani 1 1 d . . . H10 H 0.7892 0.8417 0.4317 0.109 Uiso 1 1 calc R . . H11 H 0.9072 0.8372 0.4583 0.109 Uiso 1 1 calc R . . H12 H 0.8501 0.7440 0.4376 0.109 Uiso 1 1 calc R . . C14 C 0.96236(14) 0.82273(14) 0.27883(7) 0.0289(4) Uani 1 1 d . . . H13 H 0.9910 0.8712 0.3018 0.035 Uiso 1 1 calc R . . H14 H 0.9480 0.8522 0.2468 0.035 Uiso 1 1 calc R . . C15 C 1.04524(16) 0.74585(17) 0.27628(9) 0.0452(6) Uani 1 1 d . . . H15 H 1.0584 0.7155 0.3078 0.068 Uiso 1 1 calc R . . H16 H 1.1114 0.7731 0.2674 0.068 Uiso 1 1 calc R . . H17 H 1.0190 0.6997 0.2521 0.068 Uiso 1 1 calc R . . C16 C 0.78292(17) 0.62881(15) 0.02973(7) 0.0355(5) Uani 1 1 d . . . H18 H 0.7370 0.6055 0.0537 0.043 Uiso 1 1 calc R . . H19 H 0.8183 0.5745 0.0165 0.043 Uiso 1 1 calc R . . C17 C 0.71421(18) 0.67771(18) -0.01091(8) 0.0477(6) Uani 1 1 d . . . H20 H 0.6764 0.7298 0.0023 0.072 Uiso 1 1 calc R . . H21 H 0.6627 0.6334 -0.0264 0.072 Uiso 1 1 calc R . . H22 H 0.7595 0.7013 -0.0346 0.072 Uiso 1 1 calc R . . C18 C 1.0061(2) 0.6746(2) -0.00707(8) 0.0560(7) Uani 1 1 d . . . H23 H 0.9515 0.6335 -0.0239 0.067 Uiso 1 1 calc R . . H24 H 1.0191 0.7263 -0.0292 0.067 Uiso 1 1 calc R . . C19 C 1.1053(3) 0.6208(3) 0.00331(10) 0.0796(10) Uani 1 1 d . . . H25 H 1.1606 0.6613 0.0192 0.119 Uiso 1 1 calc R . . H26 H 1.1283 0.5972 -0.0269 0.119 Uiso 1 1 calc R . . H27 H 1.0929 0.5684 0.0245 0.119 Uiso 1 1 calc R . . C20 C 0.45812(14) 0.61382(13) 0.11672(6) 0.0260(4) Uani 1 1 d . . . C21 C 0.38445(15) 0.53634(14) 0.12947(7) 0.0332(4) Uani 1 1 d . . . H28 H 0.4113 0.4764 0.1191 0.050 Uiso 1 1 calc R . . H29 H 0.3132 0.5472 0.1132 0.050 Uiso 1 1 calc R . . H30 H 0.3812 0.5354 0.1644 0.050 Uiso 1 1 calc R . . C22 C 0.47896(16) 0.60487(15) 0.06392(6) 0.0334(4) Uani 1 1 d . . . H31 H 0.5234 0.6569 0.0553 0.050 Uiso 1 1 calc R . . H32 H 0.4113 0.6060 0.0435 0.050 Uiso 1 1 calc R . . H33 H 0.5156 0.5459 0.0592 0.050 Uiso 1 1 calc R . . C23 C 0.42266(13) 0.71363(13) 0.12986(6) 0.0253(4) Uani 1 1 d . . . C24 C 0.37468(15) 0.71621(15) 0.17751(7) 0.0322(4) Uani 1 1 d . . . H34 H 0.4225 0.6850 0.2023 0.048 Uiso 1 1 calc R . . H35 H 0.3060 0.6842 0.1741 0.048 Uiso 1 1 calc R . . H36 H 0.3646 0.7811 0.1869 0.048 Uiso 1 1 calc R . . C25 C 0.34880(15) 0.76165(15) 0.09095(7) 0.0331(4) Uani 1 1 d . . . H37 H 0.3337 0.8251 0.1013 0.050 Uiso 1 1 calc R . . H38 H 0.2823 0.7265 0.0855 0.050 Uiso 1 1 calc R . . H39 H 0.3829 0.7642 0.0610 0.050 Uiso 1 1 calc R . . C26 C 0.77902(14) 0.50142(13) 0.16210(6) 0.0260(4) Uani 1 1 d . . . H40 H 0.7526 0.5182 0.1302 0.031 Uiso 1 1 calc R . . C27 C 0.87890(15) 0.46536(14) 0.17584(6) 0.0275(4) Uani 1 1 d . . . C28 C 0.88562(14) 0.45060(12) 0.22600(6) 0.0233(4) Uani 1 1 d . . . C29 C 0.78823(13) 0.47887(12) 0.24120(6) 0.0206(3) Uani 1 1 d . . . C30 C 0.74644(13) 0.48149(12) 0.28680(6) 0.0204(3) Uani 1 1 d . . . C31 C 0.80234(13) 0.45776(12) 0.33054(6) 0.0224(4) Uani 1 1 d . . . H41 H 0.8714 0.4316 0.3312 0.027 Uiso 1 1 calc R . . C32 C 0.75758(13) 0.47216(12) 0.37293(6) 0.0212(4) Uani 1 1 d . . . C33 C 0.80949(13) 0.45110(13) 0.41975(6) 0.0246(4) Uani 1 1 d . . . C34 C 0.78262(15) 0.47420(15) 0.46542(7) 0.0331(4) Uani 1 1 d . A . C35 C 0.86254(15) 0.43823(14) 0.49931(6) 0.0299(4) Uani 1 1 d . . . C36 C 0.93433(14) 0.39332(13) 0.47350(6) 0.0271(4) Uani 1 1 d . . . H42 H 0.9959 0.3613 0.4871 0.033 Uiso 1 1 calc R . . C37 C 0.96217(18) 0.44642(18) 0.14252(7) 0.0452(6) Uani 1 1 d . . . H43 H 0.9272 0.4408 0.1093 0.054 Uiso 1 1 calc R . . H44 H 0.9962 0.3858 0.1513 0.054 Uiso 1 1 calc R . . C38 C 1.0475(2) 0.5207(2) 0.14334(11) 0.0693(9) Uani 1 1 d . . . H45 H 1.0145 0.5812 0.1353 0.104 Uiso 1 1 calc R . . H46 H 1.0970 0.5051 0.1198 0.104 Uiso 1 1 calc R . . H47 H 1.0861 0.5237 0.1755 0.104 Uiso 1 1 calc R . . C39 C 0.97929(14) 0.41015(14) 0.25609(7) 0.0278(4) Uani 1 1 d . . . H48 H 1.0242 0.3761 0.2349 0.033 Uiso 1 1 calc R . . H49 H 0.9538 0.3647 0.2790 0.033 Uiso 1 1 calc R . . C40 C 1.04684(16) 0.48433(16) 0.28435(8) 0.0414(5) Uani 1 1 d . . . H50 H 1.0805 0.5244 0.2619 0.062 Uiso 1 1 calc R . . H51 H 1.1017 0.4538 0.3062 0.062 Uiso 1 1 calc R . . H52 H 1.0015 0.5223 0.3031 0.062 Uiso 1 1 calc R . . C41 C 0.68690(19) 0.5254(2) 0.47850(8) 0.0633(9) Uani 1 1 d D . . H53 H 0.6258 0.5033 0.4565 0.076 Uiso 0.510(6) 1 calc PR A 1 H54 H 0.6742 0.5050 0.5113 0.076 Uiso 0.510(6) 1 calc PR A 1 H55 H 0.7086 0.5608 0.5083 0.076 Uiso 0.490(6) 1 calc PR A 2 H56 H 0.6681 0.5719 0.4528 0.076 Uiso 0.490(6) 1 calc PR A 2 C42 C 0.6835(3) 0.6161(3) 0.47823(16) 0.0405(13) Uani 0.510(6) 1 d PD A 1 H57 H 0.6147 0.6370 0.4875 0.061 Uiso 0.510(6) 1 calc PR A 1 H58 H 0.6925 0.6390 0.4459 0.061 Uiso 0.510(6) 1 calc PR A 1 H59 H 0.7406 0.6407 0.5011 0.061 Uiso 0.510(6) 1 calc PR A 1 C43 C 0.5997(3) 0.4803(4) 0.48541(16) 0.0463(15) Uani 0.490(6) 1 d PD A 2 H60 H 0.5463 0.5245 0.4947 0.069 Uiso 0.490(6) 1 calc PR A 2 H61 H 0.6150 0.4343 0.5111 0.069 Uiso 0.490(6) 1 calc PR A 2 H62 H 0.5725 0.4485 0.4556 0.069 Uiso 0.490(6) 1 calc PR A 2 C44 C 0.86684(17) 0.44646(18) 0.55319(7) 0.0412(5) Uani 1 1 d . . . H63 H 0.7979 0.4261 0.5634 0.049 Uiso 1 1 calc R . . H64 H 0.8769 0.5128 0.5623 0.049 Uiso 1 1 calc R . . C45 C 0.9545(2) 0.38965(17) 0.57992(7) 0.0462(6) Uani 1 1 d . . . H65 H 0.9452 0.3238 0.5712 0.069 Uiso 1 1 calc R . . H66 H 0.9518 0.3969 0.6147 0.069 Uiso 1 1 calc R . . H67 H 1.0234 0.4114 0.5712 0.069 Uiso 1 1 calc R . . C46 C 0.43220(13) 0.60078(14) 0.33961(7) 0.0273(4) Uani 1 1 d . . . C47 C 0.36178(16) 0.67606(16) 0.31506(8) 0.0399(5) Uani 1 1 d . . . H68 H 0.3860 0.7373 0.3271 0.060 Uiso 1 1 calc R . . H69 H 0.2883 0.6661 0.3220 0.060 Uiso 1 1 calc R . . H70 H 0.3656 0.6733 0.2802 0.060 Uiso 1 1 calc R . . C48 C 0.43857(15) 0.61438(16) 0.39390(7) 0.0350(5) Uani 1 1 d . . . H71 H 0.4805 0.5639 0.4100 0.053 Uiso 1 1 calc R . . H72 H 0.3668 0.6137 0.4041 0.053 Uiso 1 1 calc R . . H73 H 0.4725 0.6743 0.4025 0.053 Uiso 1 1 calc R . . C49 C 0.40324(13) 0.49946(14) 0.32339(7) 0.0270(4) Uani 1 1 d . . . C50 C 0.36375(16) 0.49328(17) 0.27009(7) 0.0393(5) Uani 1 1 d . . . H74 H 0.4145 0.5244 0.2512 0.059 Uiso 1 1 calc R . . H75 H 0.2944 0.5238 0.2643 0.059 Uiso 1 1 calc R . . H76 H 0.3570 0.4277 0.2605 0.059 Uiso 1 1 calc R . . C51 C 0.32659(15) 0.45127(16) 0.35373(8) 0.0387(5) Uani 1 1 d . . . H77 H 0.3127 0.3878 0.3417 0.058 Uiso 1 1 calc R . . H78 H 0.2598 0.4862 0.3518 0.058 Uiso 1 1 calc R . . H79 H 0.3578 0.4487 0.3873 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0256(8) 0.0266(8) 0.0226(7) 0.0004(6) 0.0010(6) -0.0014(6) N2 0.0276(8) 0.0446(11) 0.0253(8) -0.0085(7) 0.0083(7) -0.0027(7) N3 0.0221(7) 0.0242(8) 0.0215(7) 0.0022(6) 0.0021(6) 0.0023(6) N4 0.0256(7) 0.0280(8) 0.0183(7) -0.0015(6) 0.0031(6) 0.0012(6) O1 0.0209(6) 0.0274(7) 0.0234(6) 0.0016(5) -0.0006(5) -0.0028(5) O2 0.0237(6) 0.0313(7) 0.0232(6) -0.0008(5) -0.0006(5) 0.0009(5) O3 0.0248(6) 0.0243(7) 0.0268(6) 0.0029(5) -0.0067(5) -0.0010(5) O4 0.0207(6) 0.0244(7) 0.0264(6) 0.0033(5) -0.0003(5) -0.0008(5) O5 0.0181(6) 0.0301(7) 0.0225(6) 0.0016(5) 0.0038(5) 0.0018(5) O6 0.0203(6) 0.0377(8) 0.0222(6) -0.0024(5) 0.0032(5) 0.0027(5) O7 0.0219(6) 0.0271(7) 0.0359(7) 0.0031(5) 0.0109(5) 0.0026(5) O8 0.0182(6) 0.0270(7) 0.0291(6) 0.0025(5) 0.0035(5) -0.0007(5) B1 0.0224(9) 0.0278(11) 0.0218(9) 0.0008(8) -0.0021(8) -0.0016(8) B2 0.0212(9) 0.0269(11) 0.0238(9) 0.0018(8) 0.0037(8) -0.0004(8) C1 0.0327(10) 0.0326(11) 0.0220(8) 0.0005(7) 0.0029(8) 0.0023(8) C2 0.0310(9) 0.0274(10) 0.0236(8) -0.0015(7) -0.0020(8) 0.0019(7) C3 0.0265(9) 0.0192(9) 0.0242(8) 0.0019(7) -0.0010(7) 0.0015(7) C4 0.0230(8) 0.0201(9) 0.0224(8) 0.0017(7) 0.0019(7) 0.0011(6) C5 0.0220(8) 0.0167(8) 0.0255(8) 0.0009(7) -0.0024(7) 0.0015(6) C6 0.0219(8) 0.0255(10) 0.0249(8) -0.0011(7) -0.0002(7) -0.0005(7) C7 0.0220(8) 0.0187(9) 0.0263(8) 0.0005(7) 0.0005(7) 0.0034(6) C8 0.0258(9) 0.0262(10) 0.0240(8) -0.0017(7) 0.0006(7) 0.0046(7) C9 0.0328(10) 0.0310(11) 0.0242(9) -0.0035(7) 0.0001(8) 0.0080(8) C10 0.0344(11) 0.0606(15) 0.0275(10) -0.0101(10) 0.0052(9) 0.0088(10) C11 0.0281(10) 0.0732(17) 0.0332(11) -0.0112(11) 0.0116(9) -0.0017(10) C12 0.0405(11) 0.0479(14) 0.0283(10) -0.0072(9) -0.0068(9) 0.0022(10) C13 0.0561(16) 0.134(3) 0.0271(11) -0.0239(15) -0.0026(12) -0.0019(17) C14 0.0254(9) 0.0292(10) 0.0306(9) 0.0019(8) -0.0044(8) -0.0047(7) C15 0.0283(10) 0.0488(14) 0.0587(14) 0.0171(11) 0.0047(10) 0.0048(9) C16 0.0427(11) 0.0331(11) 0.0293(10) -0.0078(8) -0.0027(9) 0.0055(9) C17 0.0459(13) 0.0607(16) 0.0340(11) -0.0022(10) -0.0079(10) 0.0034(11) C18 0.0502(14) 0.088(2) 0.0309(11) -0.0164(12) 0.0112(11) 0.0160(13) C19 0.104(2) 0.090(2) 0.0474(15) -0.0160(15) 0.0176(16) 0.045(2) C20 0.0246(9) 0.0284(10) 0.0233(8) 0.0028(7) -0.0053(8) -0.0005(7) C21 0.0325(10) 0.0306(11) 0.0346(10) 0.0008(8) -0.0062(9) -0.0063(8) C22 0.0349(10) 0.0385(12) 0.0254(9) -0.0025(8) -0.0032(8) 0.0024(8) C23 0.0205(8) 0.0282(10) 0.0266(9) 0.0027(7) -0.0003(7) -0.0021(7) C24 0.0296(10) 0.0340(11) 0.0334(10) -0.0013(8) 0.0059(8) -0.0045(8) C25 0.0265(9) 0.0352(11) 0.0363(10) 0.0054(8) -0.0029(8) 0.0044(8) C26 0.0318(10) 0.0271(10) 0.0188(8) 0.0025(7) 0.0006(7) 0.0015(7) C27 0.0307(9) 0.0309(11) 0.0220(8) 0.0023(7) 0.0080(8) 0.0019(8) C28 0.0241(9) 0.0237(9) 0.0224(8) 0.0009(7) 0.0036(7) 0.0005(7) C29 0.0226(8) 0.0188(9) 0.0203(8) 0.0015(6) 0.0016(7) -0.0010(6) C30 0.0192(8) 0.0178(9) 0.0245(8) -0.0010(7) 0.0037(7) -0.0019(6) C31 0.0200(8) 0.0263(10) 0.0213(8) 0.0003(7) 0.0036(7) 0.0015(7) C32 0.0172(8) 0.0223(9) 0.0242(8) -0.0013(7) 0.0026(7) -0.0037(6) C33 0.0220(8) 0.0299(10) 0.0219(8) -0.0013(7) 0.0027(7) -0.0010(7) C34 0.0284(10) 0.0489(13) 0.0222(9) -0.0047(8) 0.0039(8) 0.0054(8) C35 0.0296(10) 0.0392(12) 0.0212(8) 0.0001(8) 0.0034(8) -0.0017(8) C36 0.0279(9) 0.0303(10) 0.0224(8) 0.0016(7) -0.0014(8) 0.0001(7) C37 0.0445(12) 0.0659(17) 0.0271(10) 0.0057(10) 0.0135(10) 0.0177(11) C38 0.0452(14) 0.104(3) 0.0642(17) 0.0288(17) 0.0316(13) 0.0055(14) C39 0.0239(9) 0.0334(11) 0.0265(9) 0.0052(8) 0.0046(8) 0.0073(7) C40 0.0280(10) 0.0474(14) 0.0463(12) 0.0090(10) -0.0081(10) -0.0047(9) C41 0.0431(14) 0.126(3) 0.0199(10) -0.0113(13) 0.0001(10) 0.0392(15) C42 0.039(2) 0.040(3) 0.043(2) -0.0075(19) 0.0055(19) 0.0092(19) C43 0.025(2) 0.077(4) 0.038(2) 0.012(2) 0.0092(19) -0.005(2) C44 0.0368(11) 0.0648(16) 0.0218(9) -0.0017(9) 0.0018(9) -0.0032(10) C45 0.0658(15) 0.0456(14) 0.0246(10) 0.0044(9) -0.0084(10) -0.0033(11) C46 0.0197(8) 0.0338(11) 0.0295(9) 0.0030(8) 0.0078(8) 0.0025(7) C47 0.0354(11) 0.0433(13) 0.0423(12) 0.0072(10) 0.0107(10) 0.0147(9) C48 0.0280(10) 0.0469(13) 0.0310(10) -0.0062(9) 0.0071(8) 0.0009(9) C49 0.0173(8) 0.0356(11) 0.0280(9) 0.0002(8) 0.0023(7) 0.0013(7) C50 0.0291(10) 0.0558(15) 0.0316(10) -0.0066(9) -0.0028(9) 0.0099(9) C51 0.0248(10) 0.0473(14) 0.0453(12) -0.0010(10) 0.0098(9) -0.0069(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.344(2) . ? N1 C4 1.377(2) . ? N1 H1 0.8800 . ? N2 C11 1.357(3) . ? N2 C8 1.379(2) . ? N2 H2 0.8800 . ? N3 C26 1.339(2) . ? N3 C29 1.382(2) . ? N3 H3 0.8800 . ? N4 C36 1.357(2) . ? N4 C33 1.381(2) . ? N4 H4 0.8800 . ? O1 C5 1.324(2) . ? O1 B1 1.498(2) . ? O2 C7 1.318(2) . ? O2 B1 1.496(2) . ? O3 B1 1.438(2) . ? O3 C20 1.444(2) . ? O4 C23 1.443(2) . ? O4 B1 1.453(2) . ? O5 C30 1.318(2) . ? O5 B2 1.495(2) . ? O6 C32 1.315(2) . ? O6 B2 1.498(2) . ? O7 B2 1.435(2) . ? O7 C46 1.436(2) . ? O8 C49 1.445(2) . ? O8 B2 1.450(2) . ? C1 C2 1.382(3) . ? C1 H5 0.9500 . ? C2 C3 1.404(3) . ? C2 C12 1.506(2) . ? C3 C4 1.406(2) . ? C3 C14 1.502(3) . ? C4 C5 1.427(2) . ? C5 C6 1.387(3) . ? C6 C7 1.381(2) . ? C6 H6 0.9500 . ? C7 C8 1.430(3) . ? C8 C9 1.399(2) . ? C9 C10 1.412(3) . ? C9 C16 1.497(3) . ? C10 C11 1.376(3) . ? C10 C18 1.507(3) . ? C11 H7 0.9500 . ? C12 C13 1.514(3) . ? C12 H8 0.9900 . ? C12 H9 0.9900 . ? C13 H10 0.9800 . ? C13 H11 0.9800 . ? C13 H12 0.9800 . ? C14 C15 1.529(3) . ? C14 H13 0.9900 . ? C14 H14 0.9900 . ? C15 H15 0.9800 . ? C15 H16 0.9800 . ? C15 H17 0.9800 . ? C16 C17 1.529(3) . ? C16 H18 0.9900 . ? C16 H19 0.9900 . ? C17 H20 0.9800 . ? C17 H21 0.9800 . ? C17 H22 0.9800 . ? C18 C19 1.477(4) . ? C18 H23 0.9900 . ? C18 H24 0.9900 . ? C19 H25 0.9800 . ? C19 H26 0.9800 . ? C19 H27 0.9800 . ? C20 C21 1.517(3) . ? C20 C22 1.530(3) . ? C20 C23 1.556(3) . ? C21 H28 0.9800 . ? C21 H29 0.9800 . ? C21 H30 0.9800 . ? C22 H31 0.9800 . ? C22 H32 0.9800 . ? C22 H33 0.9800 . ? C23 C24 1.519(3) . ? C23 C25 1.524(2) . ? C24 H34 0.9800 . ? C24 H35 0.9800 . ? C24 H36 0.9800 . ? C25 H37 0.9800 . ? C25 H38 0.9800 . ? C25 H39 0.9800 . ? C26 C27 1.384(3) . ? C26 H40 0.9500 . ? C27 C28 1.411(2) . ? C27 C37 1.501(3) . ? C28 C29 1.405(2) . ? C28 C39 1.499(2) . ? C29 C30 1.429(2) . ? C30 C31 1.391(2) . ? C31 C32 1.380(2) . ? C31 H41 0.9500 . ? C32 C33 1.435(2) . ? C33 C34 1.393(3) . ? C34 C35 1.411(3) . ? C34 C41 1.495(3) . ? C35 C36 1.377(3) . ? C35 C44 1.506(3) . ? C36 H42 0.9500 . ? C37 C38 1.516(4) . ? C37 H43 0.9900 . ? C37 H44 0.9900 . ? C38 H45 0.9800 . ? C38 H46 0.9800 . ? C38 H47 0.9800 . ? C39 C40 1.533(3) . ? C39 H48 0.9900 . ? C39 H49 0.9900 . ? C40 H50 0.9800 . ? C40 H51 0.9800 . ? C40 H52 0.9800 . ? C41 C42 1.302(5) . ? C41 C43 1.312(5) . ? C41 H53 0.9900 . ? C41 H54 0.9900 . ? C41 H55 0.9900 . ? C41 H56 0.9900 . ? C42 H57 0.9800 . ? C42 H58 0.9800 . ? C42 H59 0.9800 . ? C43 H60 0.9800 . ? C43 H61 0.9800 . ? C43 H62 0.9800 . ? C44 C45 1.512(3) . ? C44 H63 0.9900 . ? C44 H64 0.9900 . ? C45 H65 0.9800 . ? C45 H66 0.9800 . ? C45 H67 0.9800 . ? C46 C47 1.519(3) . ? C46 C48 1.523(3) . ? C46 C49 1.555(3) . ? C47 H68 0.9800 . ? C47 H69 0.9800 . ? C47 H70 0.9800 . ? C48 H71 0.9800 . ? C48 H72 0.9800 . ? C48 H73 0.9800 . ? C49 C51 1.519(3) . ? C49 C50 1.524(3) . ? C50 H74 0.9800 . ? C50 H75 0.9800 . ? C50 H76 0.9800 . ? C51 H77 0.9800 . ? C51 H78 0.9800 . ? C51 H79 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 109.53(15) . . ? C1 N1 H1 125.2 . . ? C4 N1 H1 125.2 . . ? C11 N2 C8 108.72(16) . . ? C11 N2 H2 125.6 . . ? C8 N2 H2 125.6 . . ? C26 N3 C29 109.74(14) . . ? C26 N3 H3 125.1 . . ? C29 N3 H3 125.1 . . ? C36 N4 C33 108.82(15) . . ? C36 N4 H4 125.6 . . ? C33 N4 H4 125.6 . . ? C5 O1 B1 124.11(14) . . ? C7 O2 B1 123.80(13) . . ? B1 O3 C20 107.93(13) . . ? C23 O4 B1 107.85(13) . . ? C30 O5 B2 124.17(13) . . ? C32 O6 B2 123.21(14) . . ? B2 O7 C46 108.33(14) . . ? C49 O8 B2 108.05(14) . . ? O3 B1 O4 106.91(14) . . ? O3 B1 O2 111.89(16) . . ? O4 B1 O2 108.14(14) . . ? O3 B1 O1 108.64(15) . . ? O4 B1 O1 111.41(15) . . ? O2 B1 O1 109.84(14) . . ? O7 B2 O8 107.15(14) . . ? O7 B2 O5 107.64(15) . . ? O8 B2 O5 113.08(15) . . ? O7 B2 O6 112.39(15) . . ? O8 B2 O6 107.46(15) . . ? O5 B2 O6 109.19(14) . . ? N1 C1 C2 109.22(17) . . ? N1 C1 H5 125.4 . . ? C2 C1 H5 125.4 . . ? C1 C2 C3 107.14(15) . . ? C1 C2 C12 127.11(18) . . ? C3 C2 C12 125.60(18) . . ? C2 C3 C4 106.99(16) . . ? C2 C3 C14 124.03(16) . . ? C4 C3 C14 128.98(16) . . ? N1 C4 C3 107.11(15) . . ? N1 C4 C5 119.98(15) . . ? C3 C4 C5 132.75(17) . . ? O1 C5 C6 120.52(15) . . ? O1 C5 C4 114.94(15) . . ? C6 C5 C4 124.54(15) . . ? C7 C6 C5 120.30(16) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? O2 C7 C6 121.34(16) . . ? O2 C7 C8 116.26(15) . . ? C6 C7 C8 122.34(15) . . ? N2 C8 C9 107.87(16) . . ? N2 C8 C7 120.79(15) . . ? C9 C8 C7 130.78(17) . . ? C8 C9 C10 106.78(17) . . ? C8 C9 C16 127.89(18) . . ? C10 C9 C16 125.32(18) . . ? C11 C10 C9 107.21(18) . . ? C11 C10 C18 126.2(2) . . ? C9 C10 C18 126.5(2) . . ? N2 C11 C10 109.40(19) . . ? N2 C11 H7 125.3 . . ? C10 C11 H7 125.3 . . ? C2 C12 C13 113.63(19) . . ? C2 C12 H8 108.8 . . ? C13 C12 H8 108.8 . . ? C2 C12 H9 108.8 . . ? C13 C12 H9 108.8 . . ? H8 C12 H9 107.7 . . ? C12 C13 H10 109.5 . . ? C12 C13 H11 109.5 . . ? H10 C13 H11 109.5 . . ? C12 C13 H12 109.5 . . ? H10 C13 H12 109.5 . . ? H11 C13 H12 109.5 . . ? C3 C14 C15 112.01(16) . . ? C3 C14 H13 109.2 . . ? C15 C14 H13 109.2 . . ? C3 C14 H14 109.2 . . ? C15 C14 H14 109.2 . . ? H13 C14 H14 107.9 . . ? C14 C15 H15 109.5 . . ? C14 C15 H16 109.5 . . ? H15 C15 H16 109.5 . . ? C14 C15 H17 109.5 . . ? H15 C15 H17 109.5 . . ? H16 C15 H17 109.5 . . ? C9 C16 C17 112.10(18) . . ? C9 C16 H18 109.2 . . ? C17 C16 H18 109.2 . . ? C9 C16 H19 109.2 . . ? C17 C16 H19 109.2 . . ? H18 C16 H19 107.9 . . ? C16 C17 H20 109.5 . . ? C16 C17 H21 109.5 . . ? H20 C17 H21 109.5 . . ? C16 C17 H22 109.5 . . ? H20 C17 H22 109.5 . . ? H21 C17 H22 109.5 . . ? C19 C18 C10 114.1(2) . . ? C19 C18 H23 108.7 . . ? C10 C18 H23 108.7 . . ? C19 C18 H24 108.7 . . ? C10 C18 H24 108.7 . . ? H23 C18 H24 107.6 . . ? C18 C19 H25 109.5 . . ? C18 C19 H26 109.5 . . ? H25 C19 H26 109.5 . . ? C18 C19 H27 109.5 . . ? H25 C19 H27 109.5 . . ? H26 C19 H27 109.5 . . ? O3 C20 C21 109.49(14) . . ? O3 C20 C22 108.14(15) . . ? C21 C20 C22 109.61(16) . . ? O3 C20 C23 101.52(13) . . ? C21 C20 C23 114.82(16) . . ? C22 C20 C23 112.77(15) . . ? C20 C21 H28 109.5 . . ? C20 C21 H29 109.5 . . ? H28 C21 H29 109.5 . . ? C20 C21 H30 109.5 . . ? H28 C21 H30 109.5 . . ? H29 C21 H30 109.5 . . ? C20 C22 H31 109.5 . . ? C20 C22 H32 109.5 . . ? H31 C22 H32 109.5 . . ? C20 C22 H33 109.5 . . ? H31 C22 H33 109.5 . . ? H32 C22 H33 109.5 . . ? O4 C23 C24 108.26(14) . . ? O4 C23 C25 108.69(15) . . ? C24 C23 C25 110.04(15) . . ? O4 C23 C20 102.26(13) . . ? C24 C23 C20 112.34(15) . . ? C25 C23 C20 114.75(15) . . ? C23 C24 H34 109.5 . . ? C23 C24 H35 109.5 . . ? H34 C24 H35 109.5 . . ? C23 C24 H36 109.5 . . ? H34 C24 H36 109.5 . . ? H35 C24 H36 109.5 . . ? C23 C25 H37 109.5 . . ? C23 C25 H38 109.5 . . ? H37 C25 H38 109.5 . . ? C23 C25 H39 109.5 . . ? H37 C25 H39 109.5 . . ? H38 C25 H39 109.5 . . ? N3 C26 C27 109.29(15) . . ? N3 C26 H40 125.4 . . ? C27 C26 H40 125.4 . . ? C26 C27 C28 106.99(16) . . ? C26 C27 C37 125.14(16) . . ? C28 C27 C37 127.86(17) . . ? C29 C28 C27 106.93(15) . . ? C29 C28 C39 127.67(16) . . ? C27 C28 C39 125.38(16) . . ? N3 C29 C28 107.04(15) . . ? N3 C29 C30 119.03(15) . . ? C28 C29 C30 133.93(15) . . ? O5 C30 C31 120.35(15) . . ? O5 C30 C29 114.52(14) . . ? C31 C30 C29 125.12(15) . . ? C32 C31 C30 120.05(16) . . ? C32 C31 H41 120.0 . . ? C30 C31 H41 120.0 . . ? O6 C32 C31 121.00(15) . . ? O6 C32 C33 114.85(15) . . ? C31 C32 C33 124.12(15) . . ? N4 C33 C34 107.40(15) . . ? N4 C33 C32 121.84(15) . . ? C34 C33 C32 130.74(17) . . ? C33 C34 C35 107.57(17) . . ? C33 C34 C41 128.38(17) . . ? C35 C34 C41 124.03(17) . . ? C36 C35 C34 106.65(16) . . ? C36 C35 C44 127.01(18) . . ? C34 C35 C44 126.33(18) . . ? N4 C36 C35 109.54(16) . . ? N4 C36 H42 125.2 . . ? C35 C36 H42 125.2 . . ? C27 C37 C38 114.1(2) . . ? C27 C37 H43 108.7 . . ? C38 C37 H43 108.7 . . ? C27 C37 H44 108.7 . . ? C38 C37 H44 108.7 . . ? H43 C37 H44 107.6 . . ? C37 C38 H45 109.5 . . ? C37 C38 H46 109.5 . . ? H45 C38 H46 109.5 . . ? C37 C38 H47 109.5 . . ? H45 C38 H47 109.5 . . ? H46 C38 H47 109.5 . . ? C28 C39 C40 112.84(16) . . ? C28 C39 H48 109.0 . . ? C40 C39 H48 109.0 . . ? C28 C39 H49 109.0 . . ? C40 C39 H49 109.0 . . ? H48 C39 H49 107.8 . . ? C39 C40 H50 109.5 . . ? C39 C40 H51 109.5 . . ? H50 C40 H51 109.5 . . ? C39 C40 H52 109.5 . . ? H50 C40 H52 109.5 . . ? H51 C40 H52 109.5 . . ? C42 C41 C43 117.8(4) . . ? C42 C41 C34 121.2(3) . . ? C43 C41 C34 120.6(4) . . ? C42 C41 H53 107.0 . . ? C43 C41 H53 46.9 . . ? C34 C41 H53 107.0 . . ? C42 C41 H54 107.0 . . ? C43 C41 H54 59.9 . . ? C34 C41 H54 107.0 . . ? H53 C41 H54 106.8 . . ? C42 C41 H55 59.9 . . ? C43 C41 H55 107.2 . . ? C34 C41 H55 107.2 . . ? H53 C41 H55 145.0 . . ? H54 C41 H55 55.3 . . ? C42 C41 H56 46.9 . . ? C43 C41 H56 107.2 . . ? C34 C41 H56 107.2 . . ? H53 C41 H56 69.6 . . ? H54 C41 H56 145.0 . . ? H55 C41 H56 106.8 . . ? C41 C42 H57 109.5 . . ? C41 C42 H58 109.5 . . ? C41 C42 H59 109.5 . . ? C41 C43 H60 109.5 . . ? C41 C43 H61 109.5 . . ? H60 C43 H61 109.5 . . ? C41 C43 H62 109.5 . . ? H60 C43 H62 109.5 . . ? H61 C43 H62 109.5 . . ? C35 C44 C45 113.66(19) . . ? C35 C44 H63 108.8 . . ? C45 C44 H63 108.8 . . ? C35 C44 H64 108.8 . . ? C45 C44 H64 108.8 . . ? H63 C44 H64 107.7 . . ? C44 C45 H65 109.5 . . ? C44 C45 H66 109.5 . . ? H65 C45 H66 109.5 . . ? C44 C45 H67 109.5 . . ? H65 C45 H67 109.5 . . ? H66 C45 H67 109.5 . . ? O7 C46 C47 108.98(15) . . ? O7 C46 C48 107.86(14) . . ? C47 C46 C48 109.12(17) . . ? O7 C46 C49 101.98(14) . . ? C47 C46 C49 115.02(16) . . ? C48 C46 C49 113.38(16) . . ? C46 C47 H68 109.5 . . ? C46 C47 H69 109.5 . . ? H68 C47 H69 109.5 . . ? C46 C47 H70 109.5 . . ? H68 C47 H70 109.5 . . ? H69 C47 H70 109.5 . . ? C46 C48 H71 109.5 . . ? C46 C48 H72 109.5 . . ? H71 C48 H72 109.5 . . ? C46 C48 H73 109.5 . . ? H71 C48 H73 109.5 . . ? H72 C48 H73 109.5 . . ? O8 C49 C51 108.46(15) . . ? O8 C49 C50 107.51(15) . . ? C51 C49 C50 110.75(16) . . ? O8 C49 C46 102.96(13) . . ? C51 C49 C46 114.07(16) . . ? C50 C49 C46 112.52(17) . . ? C49 C50 H74 109.5 . . ? C49 C50 H75 109.5 . . ? H74 C50 H75 109.5 . . ? C49 C50 H76 109.5 . . ? H74 C50 H76 109.5 . . ? H75 C50 H76 109.5 . . ? C49 C51 H77 109.5 . . ? C49 C51 H78 109.5 . . ? H77 C51 H78 109.5 . . ? C49 C51 H79 109.5 . . ? H77 C51 H79 109.5 . . ? H78 C51 H79 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 O3 B1 O4 15.68(19) . . . . ? C20 O3 B1 O2 -102.53(16) . . . . ? C20 O3 B1 O1 136.02(14) . . . . ? C23 O4 B1 O3 9.06(18) . . . . ? C23 O4 B1 O2 129.69(14) . . . . ? C23 O4 B1 O1 -109.50(15) . . . . ? C7 O2 B1 O3 -124.05(16) . . . . ? C7 O2 B1 O4 118.47(16) . . . . ? C7 O2 B1 O1 -3.3(2) . . . . ? C5 O1 B1 O3 125.67(17) . . . . ? C5 O1 B1 O4 -116.82(17) . . . . ? C5 O1 B1 O2 3.0(2) . . . . ? C46 O7 B2 O8 16.63(19) . . . . ? C46 O7 B2 O5 138.53(14) . . . . ? C46 O7 B2 O6 -101.20(17) . . . . ? C49 O8 B2 O7 6.15(18) . . . . ? C49 O8 B2 O5 -112.28(16) . . . . ? C49 O8 B2 O6 127.15(14) . . . . ? C30 O5 B2 O7 131.63(16) . . . . ? C30 O5 B2 O8 -110.23(17) . . . . ? C30 O5 B2 O6 9.4(2) . . . . ? C32 O6 B2 O7 -135.97(16) . . . . ? C32 O6 B2 O8 106.39(18) . . . . ? C32 O6 B2 O5 -16.6(2) . . . . ? C4 N1 C1 C2 0.8(2) . . . . ? N1 C1 C2 C3 -1.0(2) . . . . ? N1 C1 C2 C12 174.69(18) . . . . ? C1 C2 C3 C4 0.7(2) . . . . ? C12 C2 C3 C4 -175.01(18) . . . . ? C1 C2 C3 C14 -179.25(17) . . . . ? C12 C2 C3 C14 5.0(3) . . . . ? C1 N1 C4 C3 -0.4(2) . . . . ? C1 N1 C4 C5 -176.24(16) . . . . ? C2 C3 C4 N1 -0.2(2) . . . . ? C14 C3 C4 N1 179.73(17) . . . . ? C2 C3 C4 C5 174.90(19) . . . . ? C14 C3 C4 C5 -5.1(3) . . . . ? B1 O1 C5 C6 -1.1(2) . . . . ? B1 O1 C5 C4 179.45(15) . . . . ? N1 C4 C5 O1 6.9(2) . . . . ? C3 C4 C5 O1 -167.72(18) . . . . ? N1 C4 C5 C6 -172.46(16) . . . . ? C3 C4 C5 C6 12.9(3) . . . . ? O1 C5 C6 C7 -0.8(3) . . . . ? C4 C5 C6 C7 178.51(17) . . . . ? B1 O2 C7 C6 1.8(3) . . . . ? B1 O2 C7 C8 179.08(16) . . . . ? C5 C6 C7 O2 0.5(3) . . . . ? C5 C6 C7 C8 -176.60(16) . . . . ? C11 N2 C8 C9 0.7(2) . . . . ? C11 N2 C8 C7 172.99(18) . . . . ? O2 C7 C8 N2 161.43(16) . . . . ? C6 C7 C8 N2 -21.3(3) . . . . ? O2 C7 C8 C9 -28.3(3) . . . . ? C6 C7 C8 C9 149.0(2) . . . . ? N2 C8 C9 C10 0.2(2) . . . . ? C7 C8 C9 C10 -171.02(19) . . . . ? N2 C8 C9 C16 178.93(18) . . . . ? C7 C8 C9 C16 7.7(3) . . . . ? C8 C9 C10 C11 -1.1(2) . . . . ? C16 C9 C10 C11 -179.8(2) . . . . ? C8 C9 C10 C18 174.7(2) . . . . ? C16 C9 C10 C18 -4.0(4) . . . . ? C8 N2 C11 C10 -1.4(3) . . . . ? C9 C10 C11 N2 1.5(3) . . . . ? C18 C10 C11 N2 -174.3(2) . . . . ? C1 C2 C12 C13 7.5(3) . . . . ? C3 C2 C12 C13 -177.6(2) . . . . ? C2 C3 C14 C15 93.4(2) . . . . ? C4 C3 C14 C15 -86.6(2) . . . . ? C8 C9 C16 C17 100.7(2) . . . . ? C10 C9 C16 C17 -80.8(3) . . . . ? C11 C10 C18 C19 58.1(4) . . . . ? C9 C10 C18 C19 -116.9(3) . . . . ? B1 O3 C20 C21 -153.65(16) . . . . ? B1 O3 C20 C22 86.97(18) . . . . ? B1 O3 C20 C23 -31.88(17) . . . . ? B1 O4 C23 C24 90.90(17) . . . . ? B1 O4 C23 C25 -149.59(15) . . . . ? B1 O4 C23 C20 -27.87(16) . . . . ? O3 C20 C23 O4 36.23(16) . . . . ? C21 C20 C23 O4 154.22(14) . . . . ? C22 C20 C23 O4 -79.25(16) . . . . ? O3 C20 C23 C24 -79.61(17) . . . . ? C21 C20 C23 C24 38.4(2) . . . . ? C22 C20 C23 C24 164.91(15) . . . . ? O3 C20 C23 C25 153.70(15) . . . . ? C21 C20 C23 C25 -88.31(19) . . . . ? C22 C20 C23 C25 38.2(2) . . . . ? C29 N3 C26 C27 0.4(2) . . . . ? N3 C26 C27 C28 -0.1(2) . . . . ? N3 C26 C27 C37 179.8(2) . . . . ? C26 C27 C28 C29 -0.2(2) . . . . ? C37 C27 C28 C29 179.9(2) . . . . ? C26 C27 C28 C39 178.55(17) . . . . ? C37 C27 C28 C39 -1.4(3) . . . . ? C26 N3 C29 C28 -0.5(2) . . . . ? C26 N3 C29 C30 179.68(15) . . . . ? C27 C28 C29 N3 0.4(2) . . . . ? C39 C28 C29 N3 -178.28(17) . . . . ? C27 C28 C29 C30 -179.81(19) . . . . ? C39 C28 C29 C30 1.5(3) . . . . ? B2 O5 C30 C31 1.0(2) . . . . ? B2 O5 C30 C29 -178.44(15) . . . . ? N3 C29 C30 O5 2.7(2) . . . . ? C28 C29 C30 O5 -177.09(18) . . . . ? N3 C29 C30 C31 -176.68(16) . . . . ? C28 C29 C30 C31 3.5(3) . . . . ? O5 C30 C31 C32 -6.1(3) . . . . ? C29 C30 C31 C32 173.23(16) . . . . ? B2 O6 C32 C31 13.4(3) . . . . ? B2 O6 C32 C33 -168.36(16) . . . . ? C30 C31 C32 O6 -1.1(3) . . . . ? C30 C31 C32 C33 -179.15(16) . . . . ? C36 N4 C33 C34 0.6(2) . . . . ? C36 N4 C33 C32 179.38(17) . . . . ? O6 C32 C33 N4 172.32(16) . . . . ? C31 C32 C33 N4 -9.5(3) . . . . ? O6 C32 C33 C34 -9.3(3) . . . . ? C31 C32 C33 C34 168.9(2) . . . . ? N4 C33 C34 C35 0.2(2) . . . . ? C32 C33 C34 C35 -178.39(19) . . . . ? N4 C33 C34 C41 -178.5(3) . . . . ? C32 C33 C34 C41 2.9(4) . . . . ? C33 C34 C35 C36 -0.9(2) . . . . ? C41 C34 C35 C36 177.8(2) . . . . ? C33 C34 C35 C44 179.9(2) . . . . ? C41 C34 C35 C44 -1.3(4) . . . . ? C33 N4 C36 C35 -1.3(2) . . . . ? C34 C35 C36 N4 1.4(2) . . . . ? C44 C35 C36 N4 -179.5(2) . . . . ? C26 C27 C37 C38 100.5(3) . . . . ? C28 C27 C37 C38 -79.6(3) . . . . ? C29 C28 C39 C40 -79.5(2) . . . . ? C27 C28 C39 C40 102.0(2) . . . . ? C33 C34 C41 C42 -83.3(4) . . . . ? C35 C34 C41 C42 98.2(3) . . . . ? C33 C34 C41 C43 89.1(4) . . . . ? C35 C34 C41 C43 -89.4(4) . . . . ? C36 C35 C44 C45 -6.8(3) . . . . ? C34 C35 C44 C45 172.2(2) . . . . ? B2 O7 C46 C47 -152.64(16) . . . . ? B2 O7 C46 C48 89.02(18) . . . . ? B2 O7 C46 C49 -30.63(17) . . . . ? B2 O8 C49 C51 -145.44(16) . . . . ? B2 O8 C49 C50 94.76(18) . . . . ? B2 O8 C49 C46 -24.23(17) . . . . ? O7 C46 C49 O8 33.27(16) . . . . ? C47 C46 C49 O8 151.03(15) . . . . ? C48 C46 C49 O8 -82.41(17) . . . . ? O7 C46 C49 C51 150.57(15) . . . . ? C47 C46 C49 C51 -91.7(2) . . . . ? C48 C46 C49 C51 34.9(2) . . . . ? O7 C46 C49 C50 -82.18(17) . . . . ? C47 C46 C49 C50 35.6(2) . . . . ? C48 C46 C49 C50 162.14(15) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.623 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.046 #============================================================================== # End of CIF #============================================================================== data_70705m _database_code_depnum_ccdc_archive 'CCDC 684823' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H60 B2 N4 O8' _chemical_formula_sum 'C56 H60 B2 N4 O8' _chemical_formula_weight 938.70 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' B B 0.0013 0.0007 '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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.6794(18) _cell_length_b 19.643(2) _cell_length_c 38.369(4) _cell_angle_alpha 87.700(2) _cell_angle_beta 83.602(2) _cell_angle_gamma 80.897(2) _cell_volume 11593(2) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9652 _exptl_absorpt_correction_T_max 0.9859 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71820 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 28.30 _reflns_number_total 47048 _reflns_number_gt 31128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1388P)^2^+14.3781P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 47048 _refine_ls_number_parameters 2554 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1304 _refine_ls_R_factor_gt 0.0993 _refine_ls_wR_factor_ref 0.2800 _refine_ls_wR_factor_gt 0.2622 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.079 _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 B1A B 0.5070(3) 0.3024(2) 0.85889(10) 0.0221(8) Uani 1 1 d . . . B2A B 0.4773(3) -0.1394(2) 0.92084(10) 0.0243(8) Uani 1 1 d . . . C1A C 0.5771(2) 0.17716(19) 0.79006(9) 0.0230(7) Uani 1 1 d . . . C2A C 0.5496(2) 0.23279(18) 0.81222(9) 0.0222(7) Uani 1 1 d . . . C3A C 0.5523(2) 0.30125(19) 0.80086(9) 0.0244(8) Uani 1 1 d . . . C4A C 0.5838(3) 0.31775(19) 0.76698(9) 0.0268(8) Uani 1 1 d . . . H231 H 0.5856 0.3641 0.7593 0.032 Uiso 1 1 calc R . . C5A C 0.6131(3) 0.2621(2) 0.74451(9) 0.0285(8) Uani 1 1 d . . . H234 H 0.6364 0.2711 0.7211 0.034 Uiso 1 1 calc R . . C6A C 0.6091(3) 0.19493(19) 0.75543(9) 0.0279(8) Uani 1 1 d . . . H227 H 0.6284 0.1592 0.7391 0.033 Uiso 1 1 calc R . . C7A C 0.5583(2) -0.03488(18) 0.82006(8) 0.0217(7) Uani 1 1 d . . . C8A C 0.4988(3) 0.01950(19) 0.83518(9) 0.0255(8) Uani 1 1 d . . . H223 H 0.4532 0.0097 0.8522 0.031 Uiso 1 1 calc R . . C9A C 0.5056(3) 0.08740(19) 0.82566(9) 0.0257(8) Uani 1 1 d . . . H235 H 0.4640 0.1232 0.8362 0.031 Uiso 1 1 calc R . . C10A C 0.5712(3) 0.10466(18) 0.80135(9) 0.0241(8) Uani 1 1 d . . . C11A C 0.6318(3) 0.05063(19) 0.78662(9) 0.0251(8) Uani 1 1 d . . . H233 H 0.6780 0.0608 0.7701 0.030 Uiso 1 1 calc R . . C12A C 0.6254(3) -0.01759(19) 0.79583(9) 0.0254(8) Uani 1 1 d . . . H226 H 0.6675 -0.0533 0.7855 0.031 Uiso 1 1 calc R . . C13A C 0.5541(3) -0.25104(19) 0.84754(10) 0.0277(8) Uani 1 1 d . . . H225 H 0.5552 -0.2985 0.8538 0.033 Uiso 1 1 calc R . . C14A C 0.5274(2) -0.20085(18) 0.87172(8) 0.0199(7) Uani 1 1 d . . . C15A C 0.5230(2) -0.13056(18) 0.86244(8) 0.0200(7) Uani 1 1 d . . . C16A C 0.5522(2) -0.10823(18) 0.82917(8) 0.0206(7) Uani 1 1 d . . . C17A C 0.5795(3) -0.16054(18) 0.80435(9) 0.0248(8) Uani 1 1 d . . . H220 H 0.5982 -0.1480 0.7809 0.030 Uiso 1 1 calc R . . C18A C 0.5798(3) -0.22994(19) 0.81323(9) 0.0261(8) Uani 1 1 d . . . H230 H 0.5978 -0.2636 0.7957 0.031 Uiso 1 1 calc R . . C19A C 0.7743(3) 0.31024(18) 0.93735(9) 0.0245(7) Uani 1 1 d . . . H232 H 0.8341 0.3114 0.9304 0.029 Uiso 1 1 calc R . . C20A C 0.7362(3) 0.30754(18) 0.97178(9) 0.0248(7) Uani 1 1 d . . . C21A C 0.6472(3) 0.30479(18) 0.97046(10) 0.0260(8) Uani 1 1 d . . . C22A C 0.6336(2) 0.30791(17) 0.93458(9) 0.0219(7) Uani 1 1 d . . . C23A C 0.5585(2) 0.31049(17) 0.91672(9) 0.0228(7) Uani 1 1 d . . . C24A C 0.4739(3) 0.31430(18) 0.93245(9) 0.0260(8) Uani 1 1 d . . . H229 H 0.4629 0.3123 0.9573 0.031 Uiso 1 1 calc R . . C25A C 0.4049(2) 0.32105(17) 0.91196(9) 0.0220(7) Uani 1 1 d . . . C26A C 0.3158(3) 0.32772(18) 0.92530(9) 0.0244(7) Uani 1 1 d . . . C27A C 0.2718(3) 0.3308(2) 0.96018(10) 0.0305(8) Uani 1 1 d . . . C28A C 0.1840(3) 0.33257(19) 0.95721(10) 0.0296(8) Uani 1 1 d . . . C29A C 0.1741(3) 0.33302(19) 0.92100(10) 0.0282(8) Uani 1 1 d . . . H29A H 0.1206 0.3343 0.9113 0.034 Uiso 1 1 calc R . . C30A C 0.7806(3) 0.3061(2) 1.00467(10) 0.0305(8) Uani 1 1 d . . . H101 H 0.7691 0.2648 1.0190 0.037 Uiso 1 1 calc R . . H102 H 0.7545 0.3472 1.0185 0.037 Uiso 1 1 calc R . . C31A C 0.8777(3) 0.3050(2) 0.99847(10) 0.0315(9) Uani 1 1 d . . . H105 H 0.9049 0.2626 0.9866 0.047 Uiso 1 1 calc R . . H106 H 0.9011 0.3067 1.0210 0.047 Uiso 1 1 calc R . . H107 H 0.8901 0.3451 0.9838 0.047 Uiso 1 1 calc R . . C32A C 0.5826(3) 0.3011(2) 1.00244(10) 0.0298(8) Uani 1 1 d . . . H103 H 0.6128 0.2766 1.0217 0.036 Uiso 1 1 calc R . . H104 H 0.5376 0.2743 0.9970 0.036 Uiso 1 1 calc R . . C33A C 0.5394(3) 0.3724(2) 1.01444(12) 0.0442(11) Uani 1 1 d . . . H118 H 0.5833 0.3978 1.0215 0.066 Uiso 1 1 calc R . . H119 H 0.4957 0.3678 1.0344 0.066 Uiso 1 1 calc R . . H120 H 0.5113 0.3974 0.9951 0.066 Uiso 1 1 calc R . . C34A C 0.3123(3) 0.3353(2) 0.99459(10) 0.0354(9) Uani 1 1 d . . . H110 H 0.3582 0.3649 0.9907 0.042 Uiso 1 1 calc R . . H111 H 0.2672 0.3566 1.0127 0.042 Uiso 1 1 calc R . . C35A C 0.3512(3) 0.2644(2) 1.00748(12) 0.0446(11) Uani 1 1 d . . . H112 H 0.3045 0.2375 1.0151 0.067 Uiso 1 1 calc R . . H113 H 0.3841 0.2691 1.0273 0.067 Uiso 1 1 calc R . . H114 H 0.3900 0.2406 0.9884 0.067 Uiso 1 1 calc R . . C36A C 0.1119(3) 0.3315(2) 0.98730(11) 0.0361(9) Uani 1 1 d . . . H108 H 0.1217 0.3616 1.0061 0.043 Uiso 1 1 calc R . . H109 H 0.0554 0.3504 0.9787 0.043 Uiso 1 1 calc R . . C37A C 0.1077(3) 0.2591(2) 1.00247(12) 0.0424(10) Uani 1 1 d . . . H115 H 0.0990 0.2289 0.9839 0.064 Uiso 1 1 calc R . . H116 H 0.0593 0.2606 1.0211 0.064 Uiso 1 1 calc R . . H117 H 0.1623 0.2412 1.0122 0.064 Uiso 1 1 calc R . . C38A C 0.7109(3) -0.0862(2) 1.00541(9) 0.0269(8) Uani 1 1 d . . . H228 H 0.7718 -0.0875 1.0003 0.032 Uiso 1 1 calc R . . C39A C 0.6626(2) -0.06794(18) 1.03775(9) 0.0222(7) Uani 1 1 d . . . C40A C 0.5754(2) -0.07284(17) 1.03345(8) 0.0197(7) Uani 1 1 d . . . C41A C 0.5735(2) -0.09457(18) 0.99934(9) 0.0219(7) Uani 1 1 d . . . C42A C 0.5060(2) -0.10897(17) 0.97953(8) 0.0190(7) Uani 1 1 d . . . C43A C 0.4190(2) -0.10432(17) 0.99158(8) 0.0197(7) Uani 1 1 d . . . H221 H 0.3997 -0.0938 1.0154 0.024 Uiso 1 1 calc R . . C44A C 0.3601(2) -0.11495(16) 0.96888(8) 0.0187(7) Uani 1 1 d . . . C45A C 0.2683(2) -0.11336(16) 0.97770(8) 0.0179(7) Uani 1 1 d . . . C46A C 0.2106(2) -0.09800(16) 1.00847(8) 0.0183(7) Uani 1 1 d . . . C47A C 0.1286(2) -0.11092(17) 1.00146(9) 0.0213(7) Uani 1 1 d . . . C48A C 0.1372(2) -0.13221(17) 0.96706(8) 0.0201(7) Uani 1 1 d . . . H222 H 0.0919 -0.1446 0.9553 0.024 Uiso 1 1 calc R . . C49A C 0.6976(3) -0.04746(19) 1.06967(10) 0.0291(8) Uani 1 1 d . . . H85 H 0.6570 -0.0086 1.0807 0.035 Uiso 1 1 calc R . . H86 H 0.7539 -0.0313 1.0627 0.035 Uiso 1 1 calc R . . C50A C 0.7109(3) -0.1075(2) 1.09685(11) 0.0353(9) Uani 1 1 d . . . H95 H 0.6547 -0.1213 1.1053 0.053 Uiso 1 1 calc R . . H96 H 0.7371 -0.0925 1.1167 0.053 Uiso 1 1 calc R . . H97 H 0.7494 -0.1468 1.0858 0.053 Uiso 1 1 calc R . . C51A C 0.5000(2) -0.05893(18) 1.06173(9) 0.0225(7) Uani 1 1 d . . . H83 H 0.4492 -0.0334 1.0512 0.027 Uiso 1 1 calc R . . H84 H 0.5156 -0.0292 1.0795 0.027 Uiso 1 1 calc R . . C52A C 0.4744(3) -0.1245(2) 1.07999(10) 0.0311(9) Uani 1 1 d . . . H90 H 0.4589 -0.1543 1.0626 0.047 Uiso 1 1 calc R . . H91 H 0.4246 -0.1122 1.0976 0.047 Uiso 1 1 calc R . . H92 H 0.5235 -0.1490 1.0915 0.047 Uiso 1 1 calc R . . C53A C 0.2303(2) -0.07198(17) 1.04244(8) 0.0212(7) Uani 1 1 d . . . H81 H 0.1810 -0.0372 1.0517 0.025 Uiso 1 1 calc R . . H82 H 0.2824 -0.0490 1.0381 0.025 Uiso 1 1 calc R . . C54A C 0.2461(3) -0.12980(19) 1.07001(9) 0.0273(8) Uani 1 1 d . . . H98 H 0.1957 -0.1541 1.0736 0.041 Uiso 1 1 calc R . . H99 H 0.2546 -0.1100 1.0922 0.041 Uiso 1 1 calc R . . H100 H 0.2980 -0.1622 1.0619 0.041 Uiso 1 1 calc R . . C55A C 0.0488(2) -0.10766(19) 1.02732(9) 0.0238(7) Uani 1 1 d . . . H93 H 0.0507 -0.0722 1.0447 0.029 Uiso 1 1 calc R . . H94 H 0.0505 -0.1526 1.0401 0.029 Uiso 1 1 calc R . . C56A C -0.0381(3) -0.0910(2) 1.01125(10) 0.0338(9) Uani 1 1 d . . . H87 H -0.0431 -0.0447 1.0004 0.051 Uiso 1 1 calc R . . H88 H -0.0862 -0.0928 1.0297 0.051 Uiso 1 1 calc R . . H89 H -0.0401 -0.1248 0.9934 0.051 Uiso 1 1 calc R . . N1A N 0.7122(2) 0.31095(15) 0.91542(8) 0.0237(6) Uani 1 1 d . . . H219 H 0.7210 0.3130 0.8924 0.028 Uiso 1 1 calc R . . N2A N 0.2524(2) 0.33130(14) 0.90242(8) 0.0226(6) Uani 1 1 d . . . H217 H 0.2620 0.3323 0.8794 0.027 Uiso 1 1 calc R . . N3A N 0.6575(2) -0.10140(16) 0.98309(8) 0.0257(7) Uani 1 1 d . . . H218 H 0.6735 -0.1139 0.9613 0.031 Uiso 1 1 calc R . . N4A N 0.21937(19) -0.13255(14) 0.95308(7) 0.0198(6) Uani 1 1 d . . . H216 H 0.2393 -0.1434 0.9313 0.024 Uiso 1 1 calc R . . O1A O 0.52048(17) 0.34570(12) 0.82725(6) 0.0248(5) Uani 1 1 d . . . O2A O 0.51783(17) 0.23101(12) 0.84674(6) 0.0239(5) Uani 1 1 d . . . O3A O 0.57479(17) 0.31022(14) 0.88207(6) 0.0273(6) Uani 1 1 d . . . O4A O 0.41844(17) 0.32180(13) 0.87709(6) 0.0233(5) Uani 1 1 d . . . O5A O 0.49017(16) -0.09088(12) 0.89093(6) 0.0220(5) Uani 1 1 d . . . O6A O 0.50068(17) -0.20905(13) 0.90650(6) 0.0247(5) Uani 1 1 d . . . O7A O 0.53455(17) -0.12788(14) 0.94712(6) 0.0289(6) Uani 1 1 d . . . O8A O 0.38525(16) -0.12913(13) 0.93548(6) 0.0228(5) Uani 1 1 d . . . B1B B 0.5493(3) 1.1903(2) 0.57687(10) 0.0259(9) Uani 1 1 d . . . B2B B 0.5519(3) 0.7435(2) 0.62483(11) 0.0262(9) Uani 1 1 d . . . C1B C 0.4934(2) 1.14721(18) 0.66898(9) 0.0220(7) Uani 1 1 d . . . C2B C 0.5132(2) 1.17452(18) 0.63550(9) 0.0218(7) Uani 1 1 d . . . C3B C 0.5043(2) 1.24541(18) 0.62830(9) 0.0225(7) Uani 1 1 d . . . C4B C 0.4779(3) 1.29287(19) 0.65415(9) 0.0273(8) Uani 1 1 d . . . H166 H 0.4721 1.3410 0.6491 0.033 Uiso 1 1 calc R . . C5B C 0.4598(3) 1.26675(19) 0.68847(9) 0.0279(8) Uani 1 1 d . . . H176 H 0.4423 1.2981 0.7071 0.033 Uiso 1 1 calc R . . C6B C 0.4667(3) 1.1971(2) 0.69575(9) 0.0271(8) Uani 1 1 d . . . H169 H 0.4534 1.1817 0.7192 0.032 Uiso 1 1 calc R . . C7B C 0.4941(2) 0.92875(18) 0.69153(8) 0.0209(7) Uani 1 1 d . . . C8B C 0.4829(2) 0.95837(19) 0.65798(8) 0.0216(7) Uani 1 1 d . . . H171 H 0.4738 0.9297 0.6398 0.026 Uiso 1 1 calc R . . C9B C 0.4847(2) 1.02741(19) 0.65058(9) 0.0239(7) Uani 1 1 d . . . H179 H 0.4767 1.0452 0.6276 0.029 Uiso 1 1 calc R . . C10B C 0.4984(2) 1.07239(18) 0.67668(9) 0.0221(7) Uani 1 1 d . . . C11B C 0.5110(2) 1.04331(19) 0.70961(9) 0.0224(7) Uani 1 1 d . . . H177 H 0.5204 1.0720 0.7277 0.027 Uiso 1 1 calc R . . C12B C 0.5103(3) 0.97350(19) 0.71702(9) 0.0244(8) Uani 1 1 d . . . H178 H 0.5209 0.9556 0.7398 0.029 Uiso 1 1 calc R . . C13B C 0.4784(2) 0.71362(19) 0.71648(9) 0.0255(8) Uani 1 1 d . . . H175 H 0.4744 0.6665 0.7219 0.031 Uiso 1 1 calc R . . C14B C 0.5063(2) 0.73494(18) 0.68335(9) 0.0223(7) Uani 1 1 d . . . C15B C 0.5079(2) 0.80481(18) 0.67473(8) 0.0197(7) Uani 1 1 d . . . C16B C 0.4872(2) 0.85598(18) 0.69966(8) 0.0202(7) Uani 1 1 d . . . C17B C 0.4597(3) 0.83330(19) 0.73394(9) 0.0253(8) Uani 1 1 d . . . H170 H 0.4434 0.8662 0.7519 0.030 Uiso 1 1 calc R . . C18B C 0.4558(3) 0.7639(2) 0.74201(9) 0.0294(8) Uani 1 1 d . . . H174 H 0.4375 0.7505 0.7654 0.035 Uiso 1 1 calc R . . C19B C 0.3037(3) 1.14820(19) 0.49403(10) 0.0277(8) Uani 1 1 d . . . H172 H 0.2422 1.1561 0.4984 0.033 Uiso 1 1 calc R . . C20B C 0.3508(3) 1.12429(18) 0.46281(9) 0.0244(7) Uani 1 1 d . . . C21B C 0.4391(3) 1.11972(17) 0.46777(9) 0.0238(7) Uani 1 1 d . . . C22B C 0.4435(2) 1.14145(17) 0.50163(8) 0.0207(7) Uani 1 1 d . . . C23B C 0.5132(2) 1.15092(17) 0.52120(8) 0.0210(7) Uani 1 1 d . . . C24B C 0.6007(2) 1.12909(17) 0.51131(8) 0.0221(7) Uani 1 1 d . . . H167 H 0.6184 1.1005 0.4916 0.027 Uiso 1 1 calc R . . C25B C 0.6633(3) 1.14953(18) 0.53066(9) 0.0237(7) Uani 1 1 d . . . C26B C 0.7540(3) 1.13602(18) 0.52235(9) 0.0240(7) Uani 1 1 d . . . C27B C 0.8096(3) 1.1100(2) 0.49257(9) 0.0290(8) Uani 1 1 d . . . C28B C 0.8952(3) 1.1113(2) 0.49916(10) 0.0314(9) Uani 1 1 d . . . C29B C 0.8913(3) 1.1378(2) 0.53280(10) 0.0335(9) Uani 1 1 d . . . H180 H 0.9399 1.1446 0.5442 0.040 Uiso 1 1 calc R . . C30B C 0.3120(3) 1.1098(2) 0.43011(10) 0.0322(9) Uani 1 1 d . . . H63 H 0.3504 1.1221 0.4094 0.039 Uiso 1 1 calc R . . H64 H 0.2552 1.1399 0.4296 0.039 Uiso 1 1 calc R . . C31B C 0.2988(3) 1.0354(2) 0.42715(12) 0.0387(10) Uani 1 1 d . . . H67 H 0.2754 1.0299 0.4050 0.058 Uiso 1 1 calc R . . H68 H 0.2579 1.0234 0.4468 0.058 Uiso 1 1 calc R . . H69 H 0.3546 1.0050 0.4278 0.058 Uiso 1 1 calc R . . C32B C 0.5137(3) 1.0959(2) 0.44053(9) 0.0282(8) Uani 1 1 d . . . H61 H 0.5620 1.1217 0.4429 0.034 Uiso 1 1 calc R . . H62 H 0.4947 1.1063 0.4169 0.034 Uiso 1 1 calc R . . C33B C 0.5463(3) 1.0189(2) 0.44398(11) 0.0373(10) Uani 1 1 d . . . H70 H 0.4978 0.9932 0.4432 0.056 Uiso 1 1 calc R . . H71 H 0.5710 1.0090 0.4663 0.056 Uiso 1 1 calc R . . H72 H 0.5911 1.0049 0.4246 0.056 Uiso 1 1 calc R . . C34B C 0.7827(3) 1.0845(2) 0.45943(10) 0.0349(9) Uani 1 1 d . . . H65 H 0.8283 1.0890 0.4398 0.042 Uiso 1 1 calc R . . H66 H 0.7283 1.1135 0.4536 0.042 Uiso 1 1 calc R . . C35B C 0.7684(3) 1.0094(2) 0.46334(12) 0.0440(11) Uani 1 1 d . . . H73 H 0.8228 0.9802 0.4679 0.066 Uiso 1 1 calc R . . H74 H 0.7492 0.9951 0.4417 0.066 Uiso 1 1 calc R . . H75 H 0.7238 1.0046 0.4829 0.066 Uiso 1 1 calc R . . C36B C 0.9761(3) 1.0881(3) 0.47481(11) 0.0402(10) Uani 1 1 d . . . H76 H 0.9884 1.0371 0.4756 0.048 Uiso 1 1 calc R . . H77 H 0.9649 1.1028 0.4505 0.048 Uiso 1 1 calc R . . C37B C 1.0552(3) 1.1159(3) 0.48340(13) 0.0474(12) Uani 1 1 d . . . H78 H 1.0456 1.1662 0.4808 0.071 Uiso 1 1 calc R . . H79 H 1.1056 1.0967 0.4674 0.071 Uiso 1 1 calc R . . H80 H 1.0661 1.1028 0.5076 0.071 Uiso 1 1 calc R . . C38B C 0.2990(3) 0.71986(19) 0.54273(10) 0.0263(8) Uani 1 1 d . . . H168 H 0.2376 0.7286 0.5480 0.032 Uiso 1 1 calc R . . C39B C 0.3432(3) 0.69323(19) 0.51159(9) 0.0261(8) Uani 1 1 d . . . C40B C 0.4316(3) 0.68973(17) 0.51441(9) 0.0237(7) Uani 1 1 d . . . C41B C 0.4399(3) 0.71258(17) 0.54808(9) 0.0228(7) Uani 1 1 d . . . C42B C 0.5119(2) 0.71723(16) 0.56721(8) 0.0208(7) Uani 1 1 d . . . C43B C 0.5986(2) 0.69965(17) 0.55472(9) 0.0221(7) Uani 1 1 d . . . H165 H 0.6143 0.6818 0.5318 0.027 Uiso 1 1 calc R . . C44B C 0.6629(2) 0.70821(16) 0.57591(8) 0.0208(7) Uani 1 1 d . . . C45B C 0.7542(2) 0.69993(16) 0.56499(8) 0.0209(7) Uani 1 1 d . . . C46B C 0.8043(2) 0.68702(18) 0.53223(9) 0.0238(7) Uani 1 1 d . . . C47B C 0.8910(3) 0.68954(19) 0.53751(9) 0.0264(8) Uani 1 1 d . . . C48B C 0.8920(3) 0.70378(19) 0.57270(9) 0.0262(8) Uani 1 1 d . . . H173 H 0.9422 0.7081 0.5837 0.031 Uiso 1 1 calc R . . C49B C 0.3035(3) 0.6710(2) 0.48076(10) 0.0349(9) Uani 1 1 d . . . H51 H 0.3315 0.6237 0.4746 0.042 Uiso 1 1 calc R . . H52 H 0.3159 0.7018 0.4604 0.042 Uiso 1 1 calc R . . C50B C 0.2064(4) 0.6723(3) 0.48748(14) 0.0616(16) Uani 1 1 d . . . H58 H 0.1938 0.6386 0.5061 0.092 Uiso 1 1 calc R . . H59 H 0.1841 0.6606 0.4660 0.092 Uiso 1 1 calc R . . H60 H 0.1783 0.7185 0.4947 0.092 Uiso 1 1 calc R . . C51B C 0.5028(3) 0.66120(18) 0.48644(9) 0.0261(8) Uani 1 1 d . . . H41 H 0.5533 0.6855 0.4870 0.031 Uiso 1 1 calc R . . H42 H 0.4815 0.6697 0.4631 0.031 Uiso 1 1 calc R . . C52B C 0.5312(3) 0.5839(2) 0.49205(11) 0.0360(10) Uani 1 1 d . . . H43 H 0.5548 0.5756 0.5147 0.054 Uiso 1 1 calc R . . H44 H 0.5759 0.5668 0.4732 0.054 Uiso 1 1 calc R . . H45 H 0.4811 0.5599 0.4919 0.054 Uiso 1 1 calc R . . C53B C 0.7744(3) 0.67064(19) 0.49797(9) 0.0247(8) Uani 1 1 d . . . H46 H 0.8177 0.6811 0.4785 0.030 Uiso 1 1 calc R . . H47 H 0.7187 0.7006 0.4948 0.030 Uiso 1 1 calc R . . C54B C 0.7622(3) 0.5946(2) 0.49621(9) 0.0307(9) Uani 1 1 d . . . H48 H 0.8150 0.5647 0.5021 0.046 Uiso 1 1 calc R . . H49 H 0.7507 0.5850 0.4724 0.046 Uiso 1 1 calc R . . H50 H 0.7130 0.5859 0.5130 0.046 Uiso 1 1 calc R . . C55B C 0.9688(3) 0.6809(2) 0.51043(10) 0.0323(9) Uani 1 1 d . . . H53 H 1.0195 0.6917 0.5212 0.039 Uiso 1 1 calc R . . H54 H 0.9577 0.7147 0.4910 0.039 Uiso 1 1 calc R . . C56B C 0.9918(3) 0.6077(2) 0.49516(11) 0.0395(10) Uani 1 1 d . . . H55 H 0.9924 0.5733 0.5144 0.059 Uiso 1 1 calc R . . H56 H 1.0492 0.6029 0.4817 0.059 Uiso 1 1 calc R . . H57 H 0.9483 0.6007 0.4798 0.059 Uiso 1 1 calc R . . N1B N 0.3594(2) 1.15841(15) 0.51706(8) 0.0242(6) Uani 1 1 d . . . H162 H 0.3443 1.1735 0.5385 0.029 Uiso 1 1 calc R . . N2B N 0.8070(2) 1.15227(17) 0.54632(8) 0.0279(7) Uani 1 1 d . . . H164 H 0.7887 1.1694 0.5672 0.033 Uiso 1 1 calc R . . N3B N 0.3574(2) 0.73124(16) 0.56417(8) 0.0253(7) Uani 1 1 d . . . H161 H 0.3446 0.7481 0.5853 0.030 Uiso 1 1 calc R . . N4B N 0.8099(2) 0.71043(15) 0.58863(7) 0.0232(6) Uani 1 1 d . . . H163 H 0.7945 0.7201 0.6109 0.028 Uiso 1 1 calc R . . O1B O 0.52411(18) 1.25851(13) 0.59355(6) 0.0266(6) Uani 1 1 d . . . O2B O 0.54088(17) 1.13874(12) 0.60555(6) 0.0235(5) Uani 1 1 d . . . O3B O 0.48706(17) 1.18380(13) 0.55103(6) 0.0241(5) Uani 1 1 d . . . O4B O 0.63797(18) 1.18308(13) 0.56029(6) 0.0262(6) Uani 1 1 d . . . O5B O 0.53700(17) 0.81261(12) 0.64034(6) 0.0222(5) Uani 1 1 d . . . O6B O 0.53462(18) 0.69539(13) 0.65464(6) 0.0255(5) Uani 1 1 d . . . O7B O 0.48906(18) 0.74052(14) 0.59927(6) 0.0288(6) Uani 1 1 d . . . O8B O 0.64205(18) 0.72783(14) 0.60891(6) 0.0275(6) Uani 1 1 d . . . B1C B 0.0387(3) 0.7014(2) 0.66737(10) 0.0254(9) Uani 1 1 d . . . B2C B 0.0076(3) 0.7762(2) 0.89010(10) 0.0237(8) Uani 1 1 d . . . C1C C -0.0484(2) 0.87883(18) 0.69013(8) 0.0208(7) Uani 1 1 d . . . C2C C -0.0140(2) 0.81493(17) 0.67617(9) 0.0207(7) Uani 1 1 d . . . C3C C -0.0153(2) 0.80099(18) 0.64065(9) 0.0229(7) Uani 1 1 d . . . C4C C -0.0529(3) 0.85022(19) 0.61807(9) 0.0274(8) Uani 1 1 d . . . H185 H -0.0557 0.8403 0.5942 0.033 Uiso 1 1 calc R . . C5C C -0.0866(3) 0.91471(19) 0.63139(9) 0.0270(8) Uani 1 1 d . . . H194 H -0.1111 0.9500 0.6162 0.032 Uiso 1 1 calc R . . C6C C -0.0852(2) 0.92899(18) 0.66656(9) 0.0229(7) Uani 1 1 d . . . H188 H -0.1096 0.9735 0.6749 0.028 Uiso 1 1 calc R . . C7C C -0.0420(2) 0.92024(17) 0.79975(8) 0.0187(7) Uani 1 1 d . . . C8C C 0.0207(2) 0.87079(17) 0.78207(8) 0.0201(7) Uani 1 1 d . . . H183 H 0.0651 0.8454 0.7944 0.024 Uiso 1 1 calc R . . C9C C 0.0189(2) 0.85840(18) 0.74696(9) 0.0224(7) Uani 1 1 d . . . H187 H 0.0628 0.8252 0.7356 0.027 Uiso 1 1 calc R . . C10C C -0.0461(2) 0.89360(17) 0.72770(9) 0.0207(7) Uani 1 1 d . . . C11C C -0.1093(2) 0.94258(18) 0.74570(9) 0.0229(7) Uani 1 1 d . . . H191 H -0.1546 0.9672 0.7336 0.027 Uiso 1 1 calc R . . C12C C -0.1067(3) 0.95571(17) 0.78069(9) 0.0246(8) Uani 1 1 d . . . H193 H -0.1498 0.9895 0.7920 0.030 Uiso 1 1 calc R . . C13C C -0.0325(2) 0.95806(18) 0.91011(9) 0.0227(7) Uani 1 1 d . . . H184 H -0.0295 0.9660 0.9342 0.027 Uiso 1 1 calc R . . C14C C -0.0151(2) 0.89281(17) 0.89687(9) 0.0203(7) Uani 1 1 d . . . C15C C -0.0160(2) 0.88024(17) 0.86135(9) 0.0203(7) Uani 1 1 d . . . C16C C -0.0380(2) 0.93322(16) 0.83720(8) 0.0183(7) Uani 1 1 d . . . C17C C -0.0586(2) 1.00013(17) 0.85133(9) 0.0226(7) Uani 1 1 d . . . H189 H -0.0756 1.0380 0.8361 0.027 Uiso 1 1 calc R . . C18C C -0.0552(3) 1.01277(18) 0.88618(9) 0.0250(8) Uani 1 1 d . . . H186 H -0.0683 1.0588 0.8942 0.030 Uiso 1 1 calc R . . C19C C -0.2137(3) 0.5499(2) 0.70701(11) 0.0371(10) Uani 1 1 d . . . H195 H -0.2743 0.5615 0.7053 0.044 Uiso 1 1 calc R . . C20C C -0.1723(3) 0.4870(2) 0.71947(10) 0.0354(10) Uani 1 1 d . . . C21C C -0.0829(3) 0.4915(2) 0.71810(9) 0.0300(9) Uani 1 1 d . . . C22C C -0.0731(3) 0.55699(19) 0.70359(9) 0.0280(8) Uani 1 1 d . . . C23C C -0.0003(3) 0.59241(18) 0.69329(9) 0.0258(8) Uani 1 1 d . . . C24C C 0.0858(3) 0.56873(19) 0.69846(9) 0.0252(8) Uani 1 1 d . . . H192 H 0.1009 0.5272 0.7115 0.030 Uiso 1 1 calc R . . C25C C 0.1499(2) 0.60684(17) 0.68430(8) 0.0221(7) Uani 1 1 d . . . C26C C 0.2408(3) 0.58704(18) 0.68573(9) 0.0253(8) Uani 1 1 d . . . C27C C 0.2921(3) 0.5321(2) 0.70189(10) 0.0352(9) Uani 1 1 d . . . C28C C 0.3800(3) 0.5380(2) 0.69206(11) 0.0382(10) Uani 1 1 d . . . C29C C 0.3806(3) 0.5980(2) 0.67129(11) 0.0361(9) Uani 1 1 d . . . H190 H 0.4311 0.6157 0.6613 0.043 Uiso 1 1 calc R . . C30C C -0.2172(3) 0.4265(2) 0.73131(11) 0.0408(11) Uani 1 1 d . . . H23 H -0.2782 0.4436 0.7403 0.049 Uiso 1 1 calc R . . H24 H -0.1883 0.4018 0.7509 0.049 Uiso 1 1 calc R . . C31C C -0.2161(4) 0.3761(2) 0.70189(12) 0.0491(13) Uani 1 1 d . . . H28 H -0.1561 0.3549 0.6948 0.074 Uiso 1 1 calc R . . H29 H -0.2408 0.4009 0.6818 0.074 Uiso 1 1 calc R . . H30 H -0.2506 0.3401 0.7102 0.074 Uiso 1 1 calc R . . C32C C -0.0142(3) 0.4349(2) 0.72806(10) 0.0338(9) Uani 1 1 d . . . H21 H -0.0406 0.4042 0.7458 0.041 Uiso 1 1 calc R . . H22 H 0.0300 0.4551 0.7390 0.041 Uiso 1 1 calc R . . C33C C 0.0305(3) 0.3918(2) 0.69682(11) 0.0381(10) Uani 1 1 d . . . H25 H 0.0564 0.4219 0.6790 0.057 Uiso 1 1 calc R . . H26 H -0.0123 0.3695 0.6867 0.057 Uiso 1 1 calc R . . H27 H 0.0761 0.3565 0.7048 0.057 Uiso 1 1 calc R . . C34C C 0.2618(4) 0.4729(3) 0.72386(13) 0.0499(12) Uani 1 1 d . . . H31 H 0.2058 0.4898 0.7376 0.060 Uiso 1 1 calc R . . H32 H 0.3046 0.4564 0.7406 0.060 Uiso 1 1 calc R . . C35C C 0.2506(4) 0.4128(3) 0.70184(15) 0.0547(13) Uani 1 1 d . . . H38 H 0.3073 0.3921 0.6905 0.082 Uiso 1 1 calc R . . H39 H 0.2120 0.4295 0.6839 0.082 Uiso 1 1 calc R . . H40 H 0.2252 0.3782 0.7170 0.082 Uiso 1 1 calc R . . C36C C 0.4580(4) 0.4842(3) 0.70045(15) 0.0578(14) Uani 1 1 d . . . H33 H 0.4489 0.4689 0.7253 0.069 Uiso 1 1 calc R . . H34 H 0.4609 0.4435 0.6857 0.069 Uiso 1 1 calc R . . C37C C 0.5442(4) 0.5115(3) 0.69418(15) 0.0588(14) Uani 1 1 d . . . H35 H 0.5539 0.5265 0.6696 0.088 Uiso 1 1 calc R . . H36 H 0.5914 0.4749 0.6995 0.088 Uiso 1 1 calc R . . H37 H 0.5427 0.5506 0.7094 0.088 Uiso 1 1 calc R . . C38C C -0.2780(3) 0.6468(2) 0.91265(10) 0.0386(10) Uani 1 1 d . . . H38C H -0.3382 0.6645 0.9140 0.046 Uiso 1 1 calc R . . C39C C -0.2413(3) 0.5771(2) 0.91101(10) 0.0376(10) Uani 1 1 d . . . C40C C -0.1511(3) 0.5733(2) 0.90979(9) 0.0337(10) Uani 1 1 d . . . C41C C -0.1334(3) 0.64135(19) 0.91049(9) 0.0292(8) Uani 1 1 d . . . C42C C -0.0551(3) 0.67043(17) 0.90606(8) 0.0259(8) Uani 1 1 d . . . C43C C 0.0276(3) 0.63468(19) 0.90960(9) 0.0288(8) Uani 1 1 d . . . H236 H 0.0346 0.5879 0.9175 0.035 Uiso 1 1 calc R . . C44C C 0.0998(3) 0.66728(18) 0.90160(9) 0.0267(8) Uani 1 1 d . . . C45C C 0.1878(3) 0.63694(19) 0.90455(9) 0.0290(8) Uani 1 1 d . . . C46C C 0.2285(3) 0.5696(2) 0.91208(10) 0.0367(10) Uani 1 1 d . . . C47C C 0.3179(4) 0.5719(2) 0.90924(12) 0.0471(12) Uani 1 1 d . . . C48C C 0.3304(3) 0.6392(2) 0.90020(12) 0.0437(11) Uani 1 1 d . . . H48C H 0.3848 0.6553 0.8964 0.052 Uiso 1 1 calc R . . C49C C -0.2916(4) 0.5177(3) 0.91058(12) 0.0508(13) Uani 1 1 d . . . H9 H -0.2537 0.4786 0.8984 0.061 Uiso 1 1 calc R . . H10 H -0.3415 0.5319 0.8968 0.061 Uiso 1 1 calc R . . C50C C -0.3253(3) 0.4928(2) 0.94687(12) 0.0394(10) Uani 1 1 d . . . H1 H -0.2765 0.4796 0.9609 0.059 Uiso 1 1 calc R . . H2 H -0.3546 0.4529 0.9446 0.059 Uiso 1 1 calc R . . H3 H -0.3665 0.5300 0.9584 0.059 Uiso 1 1 calc R . . C51C C -0.0853(3) 0.5084(2) 0.90745(10) 0.0394(11) Uani 1 1 d . . . H4 H -0.0316 0.5184 0.8935 0.047 Uiso 1 1 calc R . . H5 H -0.1084 0.4733 0.8950 0.047 Uiso 1 1 calc R . . C52C C -0.0630(4) 0.4790(2) 0.94337(11) 0.0443(12) Uani 1 1 d . . . H6 H -0.0334 0.5111 0.9546 0.066 Uiso 1 1 calc R . . H7 H -0.0247 0.4346 0.9405 0.066 Uiso 1 1 calc R . . H8 H -0.1165 0.4724 0.9580 0.066 Uiso 1 1 calc R . . C53C C 0.1863(3) 0.5084(2) 0.92396(11) 0.0391(10) Uani 1 1 d . . . H14 H 0.2284 0.4658 0.9193 0.047 Uiso 1 1 calc R . . H15 H 0.1365 0.5069 0.9104 0.047 Uiso 1 1 calc R . . C54C C 0.1543(3) 0.5112(2) 0.96317(11) 0.0422(11) Uani 1 1 d . . . H11 H 0.2042 0.5074 0.9768 0.063 Uiso 1 1 calc R . . H12 H 0.1220 0.4729 0.9697 0.063 Uiso 1 1 calc R . . H13 H 0.1161 0.5550 0.9681 0.063 Uiso 1 1 calc R . . C55C C 0.3889(4) 0.5112(3) 0.91407(18) 0.0737(19) Uani 1 1 d U . . H19 H 0.3998 0.5094 0.9390 0.088 Uiso 1 1 calc R . . H20 H 0.3652 0.4688 0.9098 0.088 Uiso 1 1 calc R . . C56C C 0.4645(7) 0.5078(5) 0.8952(3) 0.167(5) Uani 1 1 d U . . H16 H 0.4590 0.4950 0.8713 0.251 Uiso 1 1 calc R . . H17 H 0.5069 0.4730 0.9056 0.251 Uiso 1 1 calc R . . H18 H 0.4841 0.5528 0.8947 0.251 Uiso 1 1 calc R . . N1C N -0.1542(2) 0.59138(18) 0.69775(9) 0.0326(8) Uani 1 1 d . . . H182 H -0.1652 0.6338 0.6893 0.039 Uiso 1 1 calc R . . N2C N 0.2974(2) 0.62710(16) 0.66764(8) 0.0276(7) Uani 1 1 d . . . H181 H 0.2818 0.6654 0.6557 0.033 Uiso 1 1 calc R . . N3C N -0.2129(2) 0.68470(17) 0.91193(8) 0.0310(8) Uani 1 1 d . . . H3C H -0.2198 0.7300 0.9123 0.037 Uiso 1 1 calc R . . N4C N 0.2525(2) 0.67762(17) 0.89771(8) 0.0332(8) Uani 1 1 d . . . H4C H 0.2437 0.7220 0.8925 0.040 Uiso 1 1 calc R . . O1C O 0.02153(17) 0.73462(12) 0.63374(6) 0.0245(5) Uani 1 1 d . . . O2C O 0.02311(17) 0.75756(12) 0.69312(6) 0.0236(5) Uani 1 1 d . . . O3C O -0.02195(18) 0.65183(13) 0.67670(7) 0.0289(6) Uani 1 1 d . . . O4C O 0.12905(17) 0.66595(12) 0.66685(6) 0.0249(5) Uani 1 1 d . . . O5C O 0.00049(17) 0.81135(11) 0.85554(6) 0.0215(5) Uani 1 1 d . . . O6C O -0.00081(17) 0.83246(12) 0.91542(6) 0.0238(5) Uani 1 1 d . . . O7C O -0.06644(18) 0.73733(12) 0.89779(6) 0.0263(6) Uani 1 1 d . . . O8C O 0.09135(18) 0.73197(13) 0.89057(7) 0.0283(6) Uani 1 1 d . . . B1D B 1.0210(3) 0.2421(2) 0.60651(12) 0.0309(10) Uani 1 1 d . . . B2D B 0.9870(3) 0.3714(2) 0.83514(11) 0.0251(9) Uani 1 1 d . . . C1D C 1.0548(2) 0.10667(18) 0.67378(9) 0.0226(7) Uani 1 1 d . . . C2D C 1.0428(2) 0.15060(18) 0.64477(10) 0.0251(8) Uani 1 1 d . . . C3D C 1.0451(2) 0.12533(19) 0.61092(9) 0.0244(7) Uani 1 1 d . . . C4D C 1.0598(3) 0.0563(2) 0.60436(10) 0.0298(8) Uani 1 1 d . . . H211 H 1.0598 0.0398 0.5814 0.036 Uiso 1 1 calc R . . C5D C 1.0749(3) 0.01101(19) 0.63265(10) 0.0283(8) Uani 1 1 d . . . H205 H 1.0873 -0.0372 0.6289 0.034 Uiso 1 1 calc R . . C6D C 1.0720(3) 0.03560(19) 0.66641(10) 0.0283(8) Uani 1 1 d . . . H207 H 1.0820 0.0033 0.6852 0.034 Uiso 1 1 calc R . . C7D C 1.0537(2) 0.17013(17) 0.78040(9) 0.0226(7) Uani 1 1 d . . . C8D C 1.0731(3) 0.21442(18) 0.75210(9) 0.0252(8) Uani 1 1 d . . . H214 H 1.0876 0.2583 0.7564 0.030 Uiso 1 1 calc R . . C9D C 1.0715(3) 0.19508(18) 0.71774(9) 0.0276(8) Uani 1 1 d . . . H208 H 1.0852 0.2260 0.6990 0.033 Uiso 1 1 calc R . . C10D C 1.0503(2) 0.13108(18) 0.70998(9) 0.0222(7) Uani 1 1 d . . . C11D C 1.0287(3) 0.08785(19) 0.73864(9) 0.0261(8) Uani 1 1 d . . . H210 H 1.0125 0.0445 0.7345 0.031 Uiso 1 1 calc R . . C12D C 1.0308(3) 0.10738(19) 0.77277(10) 0.0260(8) Uani 1 1 d . . . H213 H 1.0162 0.0769 0.7915 0.031 Uiso 1 1 calc R . . C13D C 1.0400(2) 0.22045(18) 0.89038(9) 0.0232(7) Uani 1 1 d . . . H196 H 1.0339 0.2310 0.9146 0.028 Uiso 1 1 calc R . . C14D C 1.0241(2) 0.27095(17) 0.86527(9) 0.0212(7) Uani 1 1 d . . . C15D C 1.0335(2) 0.25569(17) 0.82943(9) 0.0219(7) Uani 1 1 d . . . C16D C 1.0553(2) 0.18863(17) 0.81764(9) 0.0219(7) Uani 1 1 d . . . C17D C 1.0724(2) 0.13785(17) 0.84402(10) 0.0248(7) Uani 1 1 d . . . H203 H 1.0893 0.0912 0.8373 0.030 Uiso 1 1 calc R . . C18D C 1.0658(3) 0.15243(19) 0.87912(9) 0.0261(8) Uani 1 1 d . . . H201 H 1.0788 0.1163 0.8958 0.031 Uiso 1 1 calc R . . C19D C 1.3027(3) 0.3688(2) 0.59193(9) 0.0292(8) Uani 1 1 d . . . H206 H 1.3625 0.3500 0.5885 0.035 Uiso 1 1 calc R . . C20D C 1.2697(3) 0.4372(2) 0.59919(9) 0.0303(9) Uani 1 1 d . . . C21D C 1.1790(3) 0.4437(2) 0.60199(9) 0.0281(8) Uani 1 1 d . . . C22D C 1.1588(3) 0.37747(19) 0.59669(9) 0.0254(8) Uani 1 1 d . . . C23D C 1.0801(3) 0.34937(18) 0.59825(8) 0.0255(8) Uani 1 1 d . . . C24D C 0.9959(3) 0.38615(19) 0.60225(9) 0.0280(8) Uani 1 1 d . . . H209 H 0.9868 0.4347 0.6051 0.034 Uiso 1 1 calc R . . C25D C 0.9250(3) 0.35114(19) 0.60202(9) 0.0280(8) Uani 1 1 d . . . C26D C 0.8372(3) 0.3833(2) 0.60158(10) 0.0336(9) Uani 1 1 d . . . C27D C 0.8002(3) 0.4516(2) 0.59474(10) 0.0370(10) Uani 1 1 d . . . C28D C 0.7099(3) 0.4518(2) 0.59715(11) 0.0431(11) Uani 1 1 d . . . C29D C 0.6944(3) 0.3847(3) 0.60457(11) 0.0424(11) Uani 1 1 d . . . H215 H 0.6389 0.3703 0.6075 0.051 Uiso 1 1 calc R . . C30D C 1.3257(3) 0.4914(2) 0.60397(11) 0.0370(10) Uani 1 1 d . . . H143 H 1.3870 0.4689 0.6031 0.044 Uiso 1 1 calc R . . H144 H 1.3088 0.5110 0.6276 0.044 Uiso 1 1 calc R . . C31D C 1.3198(4) 0.5507(2) 0.57668(12) 0.0437(11) Uani 1 1 d . . . H145 H 1.3281 0.5318 0.5531 0.066 Uiso 1 1 calc R . . H146 H 1.3650 0.5789 0.5791 0.066 Uiso 1 1 calc R . . H147 H 1.2626 0.5793 0.5804 0.066 Uiso 1 1 calc R . . C32D C 1.1174(3) 0.50942(19) 0.60870(10) 0.0319(9) Uani 1 1 d . . . H141 H 1.1472 0.5422 0.6199 0.038 Uiso 1 1 calc R . . H142 H 1.0675 0.4997 0.6253 0.038 Uiso 1 1 calc R . . C33D C 1.0835(3) 0.5432(2) 0.57517(11) 0.0395(10) Uani 1 1 d . . . H148 H 1.1326 0.5525 0.5585 0.059 Uiso 1 1 calc R . . H149 H 1.0452 0.5867 0.5809 0.059 Uiso 1 1 calc R . . H150 H 1.0509 0.5122 0.5646 0.059 Uiso 1 1 calc R . . C34D C 0.8445(3) 0.5140(2) 0.58689(12) 0.0417(10) Uani 1 1 d . . . H151 H 0.8085 0.5479 0.5727 0.050 Uiso 1 1 calc R . . H152 H 0.9013 0.5001 0.5730 0.050 Uiso 1 1 calc R . . C35D C 0.8585(4) 0.5473(2) 0.62032(11) 0.0465(12) Uani 1 1 d . . . H153 H 0.8023 0.5680 0.6322 0.070 Uiso 1 1 calc R . . H154 H 0.8950 0.5832 0.6146 0.070 Uiso 1 1 calc R . . H155 H 0.8873 0.5123 0.6358 0.070 Uiso 1 1 calc R . . C36D C 0.6419(4) 0.5161(3) 0.59231(15) 0.0624(16) Uani 1 1 d . . . H156 H 0.6431 0.5484 0.6113 0.075 Uiso 1 1 calc R . . H157 H 0.6583 0.5394 0.5698 0.075 Uiso 1 1 calc R . . C37D C 0.5544(4) 0.5014(4) 0.59250(16) 0.0714(17) Uani 1 1 d . . . H158 H 0.5522 0.4704 0.5734 0.107 Uiso 1 1 calc R . . H159 H 0.5148 0.5445 0.5893 0.107 Uiso 1 1 calc R . . H160 H 0.5370 0.4793 0.6150 0.107 Uiso 1 1 calc R . . C38D C 1.2320(3) 0.5399(2) 0.81712(10) 0.0288(8) Uani 1 1 d . . . H212 H 1.2930 0.5293 0.8181 0.035 Uiso 1 1 calc R . . C39D C 1.1854(3) 0.60594(19) 0.81291(9) 0.0255(8) Uani 1 1 d . . . C40D C 1.0974(3) 0.59845(18) 0.81264(8) 0.0223(7) Uani 1 1 d . . . C41D C 1.0935(2) 0.52718(17) 0.81682(9) 0.0228(7) Uani 1 1 d . . . C42D C 1.0233(2) 0.48734(16) 0.81962(8) 0.0196(7) Uani 1 1 d . . . C43D C 0.9393(2) 0.51108(17) 0.81444(8) 0.0206(7) Uani 1 1 d . . . H200 H 0.9237 0.5574 0.8065 0.025 Uiso 1 1 calc R . . C44D C 0.8753(2) 0.46816(16) 0.82061(8) 0.0193(7) Uani 1 1 d . . . C45D C 0.7853(2) 0.48655(17) 0.81666(8) 0.0198(7) Uani 1 1 d . . . C46D C 0.7350(2) 0.54569(17) 0.80366(9) 0.0207(7) Uani 1 1 d . . . C47D C 0.6492(3) 0.53197(18) 0.80453(9) 0.0257(8) Uani 1 1 d . . . C48D C 0.6499(2) 0.46455(18) 0.81796(9) 0.0248(8) Uani 1 1 d . . . H204 H 0.6009 0.4412 0.8217 0.030 Uiso 1 1 calc R . . C49D C 1.2248(3) 0.6712(2) 0.80892(10) 0.0311(9) Uani 1 1 d . . . H128 H 1.2822 0.6626 0.8181 0.037 Uiso 1 1 calc R . . H129 H 1.1874 0.7072 0.8234 0.037 Uiso 1 1 calc R . . C50D C 1.2363(3) 0.6981(3) 0.77129(11) 0.0459(12) Uani 1 1 d . . . H135 H 1.1795 0.7090 0.7623 0.069 Uiso 1 1 calc R . . H136 H 1.2734 0.6629 0.7567 0.069 Uiso 1 1 calc R . . H137 H 1.2635 0.7399 0.7705 0.069 Uiso 1 1 calc R . . C51D C 1.0241(3) 0.65732(17) 0.81107(9) 0.0231(7) Uani 1 1 d . . . H121 H 1.0425 0.6993 0.8194 0.028 Uiso 1 1 calc R . . H122 H 0.9740 0.6469 0.8273 0.028 Uiso 1 1 calc R . . C52D C 0.9944(3) 0.6726(2) 0.77422(10) 0.0305(8) Uani 1 1 d . . . H132 H 1.0436 0.6827 0.7578 0.046 Uiso 1 1 calc R . . H133 H 0.9480 0.7124 0.7751 0.046 Uiso 1 1 calc R . . H134 H 0.9727 0.6323 0.7663 0.046 Uiso 1 1 calc R . . C53D C 0.7654(3) 0.61252(17) 0.79051(9) 0.0235(7) Uani 1 1 d . . . H123 H 0.7228 0.6379 0.7756 0.028 Uiso 1 1 calc R . . H124 H 0.8217 0.6018 0.7758 0.028 Uiso 1 1 calc R . . C54D C 0.7763(3) 0.65895(18) 0.82056(9) 0.0258(8) Uani 1 1 d . . . H125 H 0.7215 0.6680 0.8358 0.039 Uiso 1 1 calc R . . H126 H 0.7922 0.7026 0.8108 0.039 Uiso 1 1 calc R . . H127 H 0.8221 0.6357 0.8342 0.039 Uiso 1 1 calc R . . C55D C 0.5728(3) 0.5788(2) 0.79235(12) 0.0371(10) Uani 1 1 d . . . H130 H 0.5897 0.5972 0.7686 0.044 Uiso 1 1 calc R . . H131 H 0.5573 0.6183 0.8083 0.044 Uiso 1 1 calc R . . C56D C 0.4935(4) 0.5444(3) 0.79103(16) 0.0586(14) Uani 1 1 d . . . H138 H 0.4450 0.5788 0.7846 0.088 Uiso 1 1 calc R . . H139 H 0.4779 0.5239 0.8141 0.088 Uiso 1 1 calc R . . H140 H 0.5063 0.5083 0.7735 0.088 Uiso 1 1 calc R . . N1D N 1.2370(2) 0.33371(16) 0.59046(8) 0.0269(7) Uani 1 1 d . . . H198 H 1.2425 0.2895 0.5862 0.032 Uiso 1 1 calc R . . N2D N 0.7715(2) 0.34298(19) 0.60688(8) 0.0349(8) Uani 1 1 d . . . H202 H 0.7787 0.2982 0.6110 0.042 Uiso 1 1 calc R . . N3D N 1.1766(2) 0.49344(16) 0.81953(8) 0.0249(6) Uani 1 1 d . . . H199 H 1.1912 0.4486 0.8224 0.030 Uiso 1 1 calc R . . N4D N 0.7311(2) 0.43814(14) 0.82474(7) 0.0218(6) Uani 1 1 d . . . H197 H 0.7471 0.3962 0.8331 0.026 Uiso 1 1 calc R . . O1D O 1.03133(18) 0.17845(13) 0.58706(7) 0.0285(6) Uani 1 1 d . . . O2D O 1.02466(18) 0.22110(13) 0.64407(7) 0.0274(6) Uani 1 1 d . . . O3D O 1.09122(18) 0.28199(13) 0.59455(7) 0.0277(6) Uani 1 1 d . . . O4D O 0.93644(19) 0.28325(13) 0.60158(7) 0.0321(6) Uani 1 1 d . . . O5D O 1.01124(17) 0.31423(11) 0.81004(6) 0.0216(5) Uani 1 1 d . . . O6D O 0.99549(17) 0.33919(12) 0.87004(6) 0.0249(5) Uani 1 1 d . . . O7D O 1.04815(17) 0.42157(12) 0.82851(7) 0.0261(5) Uani 1 1 d . . . O8D O 0.89699(17) 0.40373(12) 0.83206(7) 0.0242(5) Uani 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 B1A 0.015(2) 0.0265(19) 0.0254(19) -0.0015(15) -0.0039(15) -0.0042(16) B2A 0.018(2) 0.033(2) 0.0223(19) -0.0027(15) -0.0017(15) -0.0055(17) C1A 0.020(2) 0.0309(18) 0.0194(16) -0.0009(13) 0.0012(13) -0.0093(15) C2A 0.018(2) 0.0292(18) 0.0206(16) 0.0024(13) -0.0046(13) -0.0062(15) C3A 0.020(2) 0.0295(18) 0.0259(17) -0.0023(14) -0.0023(14) -0.0101(15) C4A 0.029(2) 0.0290(18) 0.0248(18) 0.0042(14) -0.0030(15) -0.0118(16) C5A 0.026(2) 0.044(2) 0.0183(16) 0.0006(15) 0.0000(14) -0.0149(18) C6A 0.031(2) 0.0309(19) 0.0237(17) -0.0071(14) -0.0025(15) -0.0093(16) C7A 0.022(2) 0.0275(17) 0.0161(15) -0.0034(12) -0.0028(13) -0.0041(15) C8A 0.019(2) 0.0291(18) 0.0274(18) -0.0012(14) 0.0010(14) -0.0025(15) C9A 0.027(2) 0.0255(18) 0.0235(17) -0.0026(13) 0.0020(15) -0.0024(15) C10A 0.027(2) 0.0280(18) 0.0184(16) -0.0045(13) -0.0034(14) -0.0045(15) C11A 0.023(2) 0.0296(18) 0.0221(17) -0.0027(14) -0.0036(14) -0.0016(15) C12A 0.023(2) 0.0347(19) 0.0180(16) -0.0078(14) 0.0005(14) -0.0020(16) C13A 0.030(2) 0.0234(17) 0.0293(19) -0.0038(14) -0.0080(16) -0.0004(15) C14A 0.0123(19) 0.0290(17) 0.0182(15) -0.0020(13) -0.0044(13) -0.0007(14) C15A 0.0144(19) 0.0267(17) 0.0195(16) -0.0094(13) -0.0028(13) -0.0019(14) C16A 0.0174(19) 0.0275(17) 0.0169(15) -0.0025(12) -0.0041(13) -0.0011(14) C17A 0.025(2) 0.0294(18) 0.0203(16) -0.0032(13) -0.0070(14) -0.0008(15) C18A 0.026(2) 0.0270(18) 0.0236(17) -0.0085(14) -0.0045(15) 0.0056(15) C19A 0.020(2) 0.0240(17) 0.0290(18) -0.0002(14) -0.0022(14) -0.0013(14) C20A 0.025(2) 0.0200(16) 0.0294(18) -0.0002(13) -0.0054(15) -0.0010(14) C21A 0.025(2) 0.0226(17) 0.0291(18) -0.0010(14) -0.0018(15) -0.0010(15) C22A 0.021(2) 0.0192(16) 0.0250(17) -0.0036(13) -0.0035(14) 0.0007(13) C23A 0.027(2) 0.0167(15) 0.0248(17) -0.0023(12) 0.0003(14) -0.0046(14) C24A 0.027(2) 0.0248(18) 0.0246(17) -0.0006(13) -0.0050(15) 0.0012(15) C25A 0.022(2) 0.0165(15) 0.0260(17) 0.0010(12) -0.0003(14) -0.0005(13) C26A 0.025(2) 0.0228(17) 0.0253(17) 0.0040(13) -0.0055(15) -0.0037(15) C27A 0.021(2) 0.035(2) 0.032(2) 0.0024(15) 0.0015(16) 0.0024(16) C28A 0.028(2) 0.0264(18) 0.033(2) 0.0038(15) -0.0016(16) -0.0021(16) C29A 0.023(2) 0.0265(18) 0.034(2) -0.0013(15) -0.0039(16) -0.0023(15) C30A 0.029(2) 0.032(2) 0.0310(19) 0.0008(15) -0.0107(16) -0.0004(16) C31A 0.029(2) 0.034(2) 0.032(2) -0.0036(15) -0.0076(16) -0.0003(17) C32A 0.027(2) 0.038(2) 0.0242(18) -0.0010(15) -0.0023(15) -0.0039(17) C33A 0.041(3) 0.051(3) 0.042(2) -0.015(2) 0.001(2) -0.011(2) C34A 0.034(3) 0.039(2) 0.030(2) 0.0034(16) 0.0047(17) -0.0015(18) C35A 0.041(3) 0.046(3) 0.045(3) 0.011(2) -0.001(2) -0.006(2) C36A 0.029(2) 0.037(2) 0.042(2) 0.0039(17) -0.0085(18) 0.0004(18) C37A 0.038(3) 0.043(2) 0.046(3) 0.0054(19) 0.000(2) -0.008(2) C38A 0.019(2) 0.037(2) 0.0252(18) 0.0024(15) -0.0067(15) -0.0029(16) C39A 0.0170(19) 0.0245(17) 0.0250(17) 0.0018(13) -0.0034(14) -0.0028(14) C40A 0.0206(19) 0.0192(16) 0.0194(16) 0.0005(12) -0.0033(13) -0.0034(13) C41A 0.018(2) 0.0263(17) 0.0205(16) 0.0006(13) -0.0012(13) -0.0010(14) C42A 0.0200(19) 0.0212(16) 0.0155(15) 0.0021(12) -0.0039(13) -0.0012(13) C43A 0.0183(19) 0.0220(16) 0.0183(15) -0.0033(12) -0.0023(13) -0.0007(13) C44A 0.0194(19) 0.0143(15) 0.0210(16) 0.0004(12) 0.0019(13) -0.0017(13) C45A 0.025(2) 0.0150(15) 0.0146(14) -0.0013(11) -0.0039(13) -0.0025(13) C46A 0.0171(19) 0.0170(15) 0.0198(15) 0.0014(12) -0.0007(13) -0.0012(13) C47A 0.022(2) 0.0223(16) 0.0205(16) 0.0017(12) -0.0022(13) -0.0078(14) C48A 0.0201(19) 0.0205(16) 0.0209(16) -0.0002(12) -0.0043(13) -0.0059(14) C49A 0.029(2) 0.0293(19) 0.0301(19) -0.0024(15) -0.0098(16) -0.0032(16) C50A 0.031(2) 0.042(2) 0.035(2) 0.0025(17) -0.0169(18) -0.0034(18) C51A 0.022(2) 0.0268(17) 0.0194(16) -0.0036(13) -0.0012(13) -0.0055(15) C52A 0.036(2) 0.037(2) 0.0221(18) 0.0048(15) -0.0016(16) -0.0119(18) C53A 0.021(2) 0.0228(16) 0.0196(16) -0.0026(12) 0.0022(13) -0.0044(14) C54A 0.030(2) 0.0291(19) 0.0219(17) 0.0012(14) -0.0042(15) -0.0013(16) C55A 0.021(2) 0.0273(18) 0.0230(17) -0.0029(13) -0.0031(14) -0.0025(15) C56A 0.027(2) 0.048(2) 0.0275(19) -0.0046(16) 0.0023(16) -0.0122(19) N1A 0.0203(17) 0.0250(15) 0.0256(15) -0.0006(11) -0.0034(12) -0.0023(12) N2A 0.0199(17) 0.0224(14) 0.0257(15) -0.0040(11) -0.0004(12) -0.0047(12) N3A 0.0172(17) 0.0377(17) 0.0214(14) 0.0002(12) -0.0008(12) -0.0025(13) N4A 0.0165(16) 0.0222(14) 0.0194(13) -0.0018(11) 0.0006(11) -0.0007(11) O1A 0.0277(16) 0.0244(12) 0.0243(12) -0.0017(9) -0.0017(10) -0.0104(11) O2A 0.0279(15) 0.0269(12) 0.0168(11) -0.0006(9) 0.0002(10) -0.0053(11) O3A 0.0215(15) 0.0386(14) 0.0229(12) -0.0047(10) -0.0009(10) -0.0079(12) O4A 0.0204(14) 0.0308(13) 0.0191(11) -0.0027(9) -0.0013(10) -0.0050(11) O5A 0.0173(14) 0.0278(12) 0.0205(11) -0.0091(9) 0.0005(9) -0.0015(10) O6A 0.0233(15) 0.0284(13) 0.0207(12) -0.0005(9) 0.0008(10) -0.0011(11) O7A 0.0197(15) 0.0468(16) 0.0201(12) -0.0061(11) -0.0021(10) -0.0034(12) O8A 0.0146(13) 0.0337(13) 0.0203(12) -0.0035(10) -0.0023(9) -0.0031(10) B1B 0.027(3) 0.029(2) 0.0223(19) 0.0006(15) -0.0066(17) -0.0040(18) B2B 0.020(2) 0.035(2) 0.0240(19) -0.0065(16) -0.0010(16) -0.0050(18) C1B 0.016(2) 0.0261(17) 0.0225(17) -0.0040(13) -0.0027(13) 0.0009(14) C2B 0.0162(19) 0.0281(18) 0.0210(16) -0.0058(13) 0.0012(13) -0.0043(14) C3B 0.017(2) 0.0282(18) 0.0211(16) -0.0015(13) -0.0002(13) -0.0022(14) C4B 0.032(2) 0.0239(17) 0.0267(18) -0.0019(14) -0.0052(16) -0.0059(16) C5B 0.030(2) 0.0326(19) 0.0201(17) -0.0071(14) -0.0014(15) -0.0011(16) C6B 0.026(2) 0.035(2) 0.0187(16) 0.0015(14) -0.0040(14) -0.0012(16) C7B 0.0127(19) 0.0317(18) 0.0174(15) -0.0019(13) 0.0021(12) -0.0030(14) C8B 0.0129(18) 0.0350(19) 0.0164(15) -0.0071(13) -0.0010(12) -0.0012(14) C9B 0.022(2) 0.0335(19) 0.0158(15) -0.0019(13) 0.0005(13) -0.0048(15) C10B 0.017(2) 0.0298(18) 0.0189(16) -0.0004(13) 0.0031(13) -0.0043(14) C11B 0.0173(19) 0.0333(19) 0.0169(15) -0.0054(13) -0.0014(13) -0.0043(15) C12B 0.029(2) 0.0314(19) 0.0136(15) -0.0027(13) -0.0054(14) -0.0039(16) C13B 0.022(2) 0.0307(19) 0.0253(17) -0.0036(14) -0.0019(14) -0.0080(16) C14B 0.0157(19) 0.0294(18) 0.0229(17) -0.0066(13) -0.0046(13) -0.0033(14) C15B 0.0125(18) 0.0302(18) 0.0167(15) -0.0036(13) -0.0013(12) -0.0033(14) C16B 0.0101(18) 0.0327(18) 0.0186(16) -0.0031(13) -0.0037(12) -0.0033(14) C17B 0.027(2) 0.0313(19) 0.0183(16) -0.0021(13) 0.0011(14) -0.0078(16) C18B 0.029(2) 0.042(2) 0.0178(16) 0.0010(14) -0.0006(15) -0.0097(18) C19B 0.022(2) 0.0267(18) 0.035(2) -0.0002(15) -0.0051(16) -0.0038(15) C20B 0.025(2) 0.0234(17) 0.0256(17) 0.0019(13) -0.0060(15) -0.0057(15) C21B 0.031(2) 0.0193(16) 0.0219(16) 0.0047(13) -0.0056(15) -0.0068(15) C22B 0.024(2) 0.0197(16) 0.0164(15) 0.0001(12) -0.0011(13) 0.0004(14) C23B 0.029(2) 0.0181(15) 0.0158(15) -0.0016(12) -0.0040(14) -0.0023(14) C24B 0.026(2) 0.0229(17) 0.0160(15) -0.0014(12) 0.0005(13) -0.0014(14) C25B 0.025(2) 0.0290(18) 0.0174(16) 0.0047(13) -0.0053(14) -0.0033(15) C26B 0.024(2) 0.0294(18) 0.0183(16) 0.0030(13) -0.0040(14) -0.0039(15) C27B 0.026(2) 0.037(2) 0.0231(18) 0.0051(15) -0.0059(15) -0.0009(17) C28B 0.025(2) 0.045(2) 0.0252(18) 0.0061(16) -0.0072(15) -0.0079(18) C29B 0.021(2) 0.049(2) 0.031(2) 0.0025(17) -0.0028(16) -0.0076(18) C30B 0.031(2) 0.040(2) 0.0282(19) 0.0022(16) -0.0065(16) -0.0118(18) C31B 0.029(3) 0.042(2) 0.048(2) -0.0122(19) -0.0110(19) -0.0060(19) C32B 0.024(2) 0.040(2) 0.0206(17) -0.0051(15) -0.0005(14) -0.0035(17) C33B 0.032(3) 0.043(2) 0.037(2) -0.0121(18) -0.0034(18) -0.0031(19) C34B 0.021(2) 0.058(3) 0.0227(18) -0.0061(17) -0.0030(15) 0.0033(19) C35B 0.031(3) 0.059(3) 0.041(2) -0.022(2) -0.0052(19) 0.004(2) C36B 0.031(3) 0.056(3) 0.031(2) 0.0014(19) 0.0011(18) -0.004(2) C37B 0.022(3) 0.073(3) 0.044(3) -0.005(2) 0.0016(19) -0.003(2) C38B 0.019(2) 0.0315(19) 0.0295(18) 0.0035(14) -0.0090(15) -0.0041(15) C39B 0.032(2) 0.0283(18) 0.0218(17) 0.0065(13) -0.0094(15) -0.0132(16) C40B 0.031(2) 0.0210(16) 0.0215(16) 0.0051(13) -0.0087(15) -0.0089(15) C41B 0.028(2) 0.0203(16) 0.0199(16) 0.0009(12) -0.0049(14) -0.0026(14) C42B 0.028(2) 0.0152(15) 0.0190(16) -0.0001(12) -0.0052(14) -0.0011(13) C43B 0.025(2) 0.0239(17) 0.0170(15) -0.0032(12) -0.0047(13) -0.0007(14) C44B 0.027(2) 0.0170(15) 0.0185(15) -0.0030(12) -0.0012(14) -0.0023(14) C45B 0.027(2) 0.0174(15) 0.0179(15) -0.0014(12) -0.0029(14) -0.0016(14) C46B 0.025(2) 0.0240(17) 0.0227(17) -0.0028(13) -0.0039(14) -0.0019(15) C47B 0.025(2) 0.0302(19) 0.0236(17) -0.0018(14) -0.0018(15) -0.0043(16) C48B 0.020(2) 0.0289(18) 0.0286(18) -0.0024(14) -0.0017(15) -0.0007(15) C49B 0.038(3) 0.042(2) 0.030(2) 0.0045(16) -0.0090(17) -0.021(2) C50B 0.054(4) 0.098(4) 0.043(3) 0.014(3) -0.019(2) -0.039(3) C51B 0.035(2) 0.0284(18) 0.0178(16) -0.0032(13) -0.0023(15) -0.0122(16) C52B 0.045(3) 0.033(2) 0.032(2) -0.0036(16) -0.0023(18) -0.0114(19) C53B 0.021(2) 0.037(2) 0.0151(15) -0.0051(13) -0.0026(13) 0.0005(15) C54B 0.036(2) 0.037(2) 0.0185(17) -0.0075(14) -0.0023(15) -0.0020(18) C55B 0.018(2) 0.051(2) 0.0278(19) -0.0085(17) -0.0008(15) -0.0048(18) C56B 0.034(3) 0.053(3) 0.029(2) -0.0105(18) -0.0005(17) 0.001(2) N1B 0.0246(18) 0.0257(15) 0.0213(14) -0.0033(11) -0.0025(12) -0.0006(13) N2B 0.0278(19) 0.0373(17) 0.0200(14) -0.0009(12) -0.0069(13) -0.0063(14) N3B 0.0236(18) 0.0287(16) 0.0252(15) -0.0048(12) -0.0046(12) -0.0066(13) N4B 0.0257(18) 0.0246(15) 0.0189(14) -0.0060(11) -0.0074(12) 0.0022(12) O1B 0.0318(16) 0.0289(13) 0.0190(12) -0.0017(10) -0.0015(10) -0.0045(11) O2B 0.0250(15) 0.0266(12) 0.0178(11) -0.0043(9) -0.0012(10) -0.0006(10) O3B 0.0215(15) 0.0291(13) 0.0210(12) -0.0022(9) 0.0003(10) -0.0030(11) O4B 0.0278(16) 0.0355(14) 0.0165(11) -0.0035(10) 0.0004(10) -0.0096(12) O5B 0.0215(14) 0.0303(13) 0.0147(11) -0.0032(9) 0.0002(9) -0.0048(11) O6B 0.0283(16) 0.0267(13) 0.0220(12) -0.0057(10) -0.0034(10) -0.0038(11) O7B 0.0257(16) 0.0380(14) 0.0217(12) -0.0100(10) -0.0007(11) -0.0006(12) O8B 0.0243(15) 0.0385(14) 0.0194(12) -0.0087(10) -0.0044(10) -0.0008(11) B1C 0.029(3) 0.025(2) 0.0233(19) -0.0010(15) -0.0022(17) -0.0075(17) B2C 0.026(2) 0.0218(19) 0.0250(19) 0.0009(15) -0.0114(17) -0.0014(16) C1C 0.020(2) 0.0254(17) 0.0182(15) 0.0010(12) 0.0000(13) -0.0088(14) C2C 0.0151(19) 0.0251(17) 0.0221(16) 0.0033(13) -0.0021(13) -0.0048(14) C3C 0.024(2) 0.0267(17) 0.0197(16) 0.0007(13) 0.0005(14) -0.0112(15) C4C 0.033(2) 0.034(2) 0.0174(16) 0.0047(14) -0.0061(15) -0.0120(17) C5C 0.027(2) 0.0286(19) 0.0259(18) 0.0089(14) -0.0072(15) -0.0062(16) C6C 0.021(2) 0.0237(17) 0.0253(17) 0.0041(13) -0.0048(14) -0.0057(14) C7C 0.0188(19) 0.0198(15) 0.0179(15) 0.0012(12) 0.0002(13) -0.0058(13) C8C 0.0143(19) 0.0257(17) 0.0199(16) -0.0023(13) -0.0026(13) -0.0008(14) C9C 0.0172(19) 0.0248(17) 0.0244(17) -0.0021(13) -0.0002(14) -0.0019(14) C10C 0.021(2) 0.0210(16) 0.0201(16) 0.0015(12) -0.0023(13) -0.0047(14) C11C 0.021(2) 0.0232(17) 0.0241(17) 0.0041(13) -0.0036(14) -0.0016(14) C12C 0.028(2) 0.0194(16) 0.0248(17) -0.0021(13) 0.0018(15) -0.0023(14) C13C 0.019(2) 0.0269(17) 0.0231(17) -0.0042(13) -0.0010(14) -0.0074(15) C14C 0.020(2) 0.0222(16) 0.0202(16) -0.0006(12) -0.0053(13) -0.0057(14) C15C 0.0187(19) 0.0217(16) 0.0218(16) -0.0019(12) -0.0012(13) -0.0073(14) C16C 0.0164(19) 0.0194(15) 0.0186(15) 0.0004(12) 0.0003(13) -0.0034(13) C17C 0.024(2) 0.0194(16) 0.0230(17) 0.0012(13) 0.0049(14) -0.0027(14) C18C 0.030(2) 0.0217(17) 0.0235(17) -0.0039(13) 0.0038(15) -0.0070(15) C19C 0.038(3) 0.040(2) 0.035(2) -0.0073(17) 0.0073(18) -0.019(2) C20C 0.042(3) 0.039(2) 0.0266(19) -0.0089(16) 0.0058(17) -0.017(2) C21C 0.038(2) 0.0318(19) 0.0211(17) -0.0076(14) 0.0063(16) -0.0136(17) C22C 0.032(2) 0.0279(18) 0.0251(18) -0.0057(14) 0.0028(15) -0.0105(16) C23C 0.036(2) 0.0253(18) 0.0170(16) -0.0055(13) 0.0011(14) -0.0085(16) C24C 0.030(2) 0.0266(18) 0.0194(16) -0.0006(13) -0.0028(14) -0.0055(15) C25C 0.027(2) 0.0215(16) 0.0166(15) -0.0090(12) -0.0018(13) 0.0005(14) C26C 0.026(2) 0.0269(18) 0.0230(17) -0.0051(13) -0.0034(14) -0.0021(15) C27C 0.037(3) 0.043(2) 0.0263(19) -0.0013(16) -0.0065(17) -0.0057(19) C28C 0.029(3) 0.051(3) 0.034(2) -0.0010(18) -0.0082(18) -0.002(2) C29C 0.026(2) 0.047(2) 0.038(2) -0.0114(18) -0.0075(17) -0.0058(19) C30C 0.050(3) 0.044(2) 0.032(2) -0.0053(17) 0.0103(19) -0.027(2) C31C 0.062(4) 0.044(3) 0.046(3) -0.017(2) 0.010(2) -0.030(2) C32C 0.052(3) 0.0270(19) 0.0227(18) 0.0045(14) 0.0020(17) -0.0130(18) C33C 0.050(3) 0.032(2) 0.033(2) -0.0043(16) -0.0037(19) -0.010(2) C34C 0.039(3) 0.059(3) 0.049(3) 0.016(2) -0.011(2) 0.002(2) C35C 0.052(4) 0.043(3) 0.068(3) 0.016(2) -0.012(3) -0.006(2) C36C 0.039(3) 0.080(4) 0.058(3) -0.003(3) -0.013(2) -0.014(3) C37C 0.043(3) 0.073(4) 0.059(3) -0.005(3) -0.015(3) 0.003(3) C38C 0.046(3) 0.048(2) 0.027(2) 0.0057(17) -0.0084(18) -0.023(2) C39C 0.056(3) 0.039(2) 0.0221(18) 0.0064(15) -0.0074(18) -0.021(2) C40C 0.061(3) 0.0282(19) 0.0170(17) 0.0060(14) -0.0129(17) -0.0166(19) C41C 0.042(3) 0.0284(19) 0.0190(17) 0.0044(13) -0.0102(16) -0.0080(17) C42C 0.044(3) 0.0196(16) 0.0144(15) 0.0002(12) -0.0038(15) -0.0064(16) C43C 0.039(3) 0.0224(17) 0.0236(17) 0.0023(13) -0.0036(16) -0.0014(16) C44C 0.038(2) 0.0242(17) 0.0155(16) -0.0034(13) -0.0018(15) 0.0018(16) C45C 0.038(2) 0.0265(18) 0.0194(17) -0.0011(13) -0.0005(15) 0.0041(16) C46C 0.046(3) 0.034(2) 0.0249(19) -0.0047(15) -0.0032(18) 0.0105(19) C47C 0.048(3) 0.046(3) 0.038(2) 0.0064(19) 0.003(2) 0.015(2) C48C 0.030(3) 0.054(3) 0.040(2) 0.008(2) -0.0009(19) 0.013(2) C49C 0.074(4) 0.052(3) 0.035(2) -0.003(2) -0.002(2) -0.038(3) C50C 0.042(3) 0.029(2) 0.046(2) 0.0010(17) 0.005(2) -0.0077(19) C51C 0.068(3) 0.026(2) 0.028(2) 0.0022(15) -0.009(2) -0.018(2) C52C 0.070(4) 0.033(2) 0.030(2) 0.0051(17) -0.006(2) -0.008(2) C53C 0.051(3) 0.0243(19) 0.038(2) 0.0006(16) -0.008(2) 0.0087(18) C54C 0.058(3) 0.032(2) 0.034(2) 0.0006(17) -0.009(2) 0.002(2) C55C 0.054(4) 0.060(3) 0.089(4) 0.011(3) 0.014(3) 0.029(3) C56C 0.110(8) 0.141(7) 0.187(9) 0.098(7) 0.085(7) 0.081(6) N1C 0.032(2) 0.0348(18) 0.0329(17) -0.0037(14) 0.0017(14) -0.0141(15) N2C 0.0241(19) 0.0297(16) 0.0299(16) -0.0075(12) -0.0051(13) -0.0039(13) N3C 0.042(2) 0.0301(16) 0.0239(15) 0.0038(12) -0.0072(14) -0.0139(15) N4C 0.036(2) 0.0332(17) 0.0265(16) 0.0012(13) 0.0002(14) 0.0036(15) O1C 0.0261(15) 0.0268(13) 0.0217(12) -0.0015(9) -0.0040(10) -0.0064(11) O2C 0.0282(16) 0.0226(12) 0.0202(12) 0.0022(9) -0.0053(10) -0.0033(11) O3C 0.0287(16) 0.0260(13) 0.0335(14) 0.0025(10) -0.0056(11) -0.0086(11) O4C 0.0219(15) 0.0247(12) 0.0270(13) 0.0002(10) 0.0015(10) -0.0034(10) O5C 0.0291(15) 0.0176(11) 0.0181(11) -0.0026(9) -0.0046(10) -0.0028(10) O6C 0.0287(16) 0.0223(12) 0.0209(12) -0.0006(9) -0.0052(10) -0.0037(11) O7C 0.0319(16) 0.0209(12) 0.0264(13) -0.0001(9) -0.0052(11) -0.0040(11) O8C 0.0294(16) 0.0236(13) 0.0309(13) -0.0003(10) -0.0047(11) 0.0004(11) B1D 0.027(3) 0.035(2) 0.032(2) 0.0013(18) -0.0067(18) -0.0063(19) B2D 0.028(3) 0.0181(18) 0.030(2) -0.0009(15) -0.0051(17) -0.0044(16) C1D 0.0167(19) 0.0256(17) 0.0263(17) -0.0034(13) -0.0012(14) -0.0052(14) C2D 0.017(2) 0.0249(17) 0.0336(19) -0.0042(14) -0.0019(15) -0.0049(14) C3D 0.016(2) 0.0333(19) 0.0243(17) 0.0014(14) -0.0030(14) -0.0047(15) C4D 0.026(2) 0.0315(19) 0.034(2) -0.0079(15) -0.0052(16) -0.0082(17) C5D 0.027(2) 0.0260(18) 0.0324(19) -0.0069(14) 0.0022(16) -0.0089(16) C6D 0.027(2) 0.0261(18) 0.033(2) -0.0011(15) -0.0048(16) -0.0071(16) C7D 0.018(2) 0.0195(16) 0.0285(18) -0.0019(13) 0.0010(14) 0.0006(13) C8D 0.027(2) 0.0195(16) 0.0289(18) -0.0008(13) 0.0013(15) -0.0053(15) C9D 0.036(2) 0.0210(17) 0.0254(18) 0.0001(13) 0.0005(16) -0.0071(16) C10D 0.0168(19) 0.0260(17) 0.0228(17) -0.0017(13) 0.0009(13) -0.0023(14) C11D 0.023(2) 0.0260(18) 0.0297(18) -0.0044(14) 0.0021(15) -0.0082(15) C12D 0.023(2) 0.0271(18) 0.0284(18) 0.0022(14) -0.0002(15) -0.0076(15) C13D 0.022(2) 0.0253(17) 0.0230(17) 0.0020(13) -0.0057(14) -0.0043(15) C14D 0.0178(19) 0.0191(16) 0.0277(17) 0.0005(13) -0.0031(14) -0.0059(14) C15D 0.021(2) 0.0204(16) 0.0244(17) 0.0027(13) -0.0038(14) -0.0041(14) C16D 0.0153(19) 0.0222(16) 0.0271(17) 0.0014(13) 0.0008(14) -0.0018(14) C17D 0.022(2) 0.0158(16) 0.0359(19) 0.0011(13) -0.0029(15) -0.0028(14) C18D 0.023(2) 0.0269(18) 0.0284(18) 0.0111(14) -0.0079(15) -0.0047(15) C19D 0.033(2) 0.034(2) 0.0209(17) 0.0041(14) -0.0032(15) -0.0083(17) C20D 0.042(3) 0.033(2) 0.0168(16) 0.0024(14) -0.0018(15) -0.0113(18) C21D 0.037(2) 0.0328(19) 0.0154(16) 0.0005(13) -0.0041(15) -0.0063(17) C22D 0.032(2) 0.0295(18) 0.0142(15) 0.0016(13) -0.0008(14) -0.0054(16) C23D 0.038(2) 0.0267(18) 0.0120(15) 0.0012(12) -0.0071(14) -0.0039(16) C24D 0.038(2) 0.0247(18) 0.0203(17) 0.0015(13) -0.0053(15) -0.0021(16) C25D 0.036(2) 0.0307(19) 0.0173(16) -0.0028(13) -0.0077(15) 0.0001(17) C26D 0.037(3) 0.038(2) 0.0257(19) -0.0017(15) -0.0085(17) -0.0019(18) C27D 0.041(3) 0.043(2) 0.0223(18) -0.0016(16) -0.0004(17) 0.0091(19) C28D 0.040(3) 0.049(3) 0.033(2) 0.0102(19) 0.0008(19) 0.008(2) C29D 0.031(3) 0.063(3) 0.030(2) 0.0006(19) 0.0004(18) 0.001(2) C30D 0.043(3) 0.038(2) 0.033(2) -0.0044(17) -0.0036(18) -0.013(2) C31D 0.057(3) 0.028(2) 0.045(2) 0.0004(18) 0.005(2) -0.013(2) C32D 0.040(3) 0.0279(19) 0.0266(19) -0.0040(15) 0.0012(17) -0.0061(17) C33D 0.049(3) 0.030(2) 0.036(2) 0.0058(16) -0.0008(19) 0.0015(19) C34D 0.040(3) 0.041(2) 0.039(2) 0.0043(18) 0.0022(19) 0.004(2) C35D 0.064(4) 0.036(2) 0.032(2) 0.0005(17) 0.008(2) 0.004(2) C36D 0.044(4) 0.081(4) 0.052(3) 0.024(3) 0.004(2) 0.012(3) C37D 0.063(4) 0.089(4) 0.060(4) 0.010(3) -0.017(3) -0.002(4) C38D 0.024(2) 0.035(2) 0.0283(19) 0.0010(15) 0.0004(15) -0.0106(17) C39D 0.030(2) 0.0325(19) 0.0157(16) -0.0017(13) -0.0035(14) -0.0099(16) C40D 0.029(2) 0.0264(17) 0.0127(15) -0.0021(12) -0.0029(13) -0.0061(15) C41D 0.025(2) 0.0222(17) 0.0201(16) 0.0001(13) 0.0000(14) -0.0016(14) C42D 0.023(2) 0.0182(15) 0.0173(15) -0.0004(12) -0.0014(13) -0.0015(13) C43D 0.023(2) 0.0187(16) 0.0201(16) -0.0006(12) -0.0024(13) -0.0030(14) C44D 0.025(2) 0.0177(15) 0.0143(14) -0.0019(11) -0.0002(13) -0.0016(13) C45D 0.026(2) 0.0190(15) 0.0146(15) -0.0026(12) 0.0022(13) -0.0073(14) C46D 0.022(2) 0.0175(15) 0.0223(16) -0.0029(12) -0.0027(13) -0.0010(13) C47D 0.026(2) 0.0249(18) 0.0268(18) -0.0050(14) -0.0011(15) -0.0051(15) C48D 0.022(2) 0.0288(18) 0.0252(17) -0.0053(14) -0.0006(14) -0.0077(15) C49D 0.032(2) 0.036(2) 0.0276(19) -0.0009(15) -0.0017(16) -0.0135(18) C50D 0.053(3) 0.056(3) 0.035(2) 0.008(2) -0.002(2) -0.033(3) C51D 0.027(2) 0.0210(16) 0.0218(16) -0.0060(13) -0.0022(14) -0.0045(14) C52D 0.037(2) 0.0294(19) 0.0262(18) 0.0040(14) -0.0025(16) -0.0096(17) C53D 0.024(2) 0.0223(17) 0.0243(17) -0.0006(13) -0.0049(14) -0.0013(14) C54D 0.030(2) 0.0220(17) 0.0254(17) -0.0038(13) -0.0038(15) -0.0036(15) C55D 0.027(2) 0.034(2) 0.053(3) -0.0046(18) -0.0129(19) -0.0037(18) C56D 0.035(3) 0.074(4) 0.069(4) 0.021(3) -0.019(3) -0.013(3) N1D 0.0294(19) 0.0266(15) 0.0241(15) 0.0027(12) -0.0033(13) -0.0028(13) N2D 0.033(2) 0.0429(19) 0.0277(17) -0.0022(14) -0.0086(14) 0.0028(16) N3D 0.0217(18) 0.0261(15) 0.0262(15) 0.0006(12) 0.0008(12) -0.0040(13) N4D 0.0249(18) 0.0190(14) 0.0214(14) -0.0012(11) -0.0004(12) -0.0046(12) O1D 0.0279(16) 0.0300(13) 0.0291(13) -0.0023(10) -0.0097(11) -0.0034(12) O2D 0.0295(16) 0.0241(13) 0.0289(13) -0.0019(10) -0.0056(11) -0.0032(11) O3D 0.0275(16) 0.0236(13) 0.0319(14) 0.0006(10) -0.0069(11) -0.0012(11) O4D 0.0317(17) 0.0268(13) 0.0385(15) -0.0008(11) -0.0105(12) -0.0014(12) O5D 0.0248(15) 0.0170(11) 0.0228(12) 0.0017(9) -0.0024(10) -0.0029(10) O6D 0.0264(15) 0.0222(12) 0.0259(13) -0.0025(9) -0.0040(10) -0.0021(10) O7D 0.0207(15) 0.0204(12) 0.0367(14) 0.0007(10) -0.0035(11) -0.0023(10) O8D 0.0220(15) 0.0173(11) 0.0333(13) 0.0027(10) -0.0050(11) -0.0022(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 B1A O1A 1.469(5) . ? B1A O2A 1.474(5) . ? B1A O4A 1.483(5) . ? B1A O3A 1.489(5) . ? B2A O7A 1.468(5) . ? B2A O6A 1.472(5) . ? B2A O8A 1.475(5) . ? B2A O5A 1.479(5) . ? C1A C2A 1.395(5) . ? C1A C6A 1.417(5) . ? C1A C10A 1.486(5) . ? C2A O2A 1.363(4) . ? C2A C3A 1.403(5) . ? C3A O1A 1.363(4) . ? C3A C4A 1.383(5) . ? C4A C5A 1.406(5) . ? C4A H231 0.9500 . ? C5A C6A 1.378(5) . ? C5A H234 0.9500 . ? C6A H227 0.9500 . ? C7A C12A 1.399(5) . ? C7A C8A 1.401(5) . ? C7A C16A 1.484(5) . ? C8A C9A 1.386(5) . ? C8A H223 0.9500 . ? C9A C10A 1.383(5) . ? C9A H235 0.9500 . ? C10A C11A 1.399(5) . ? C11A C12A 1.388(5) . ? C11A H233 0.9500 . ? C12A H226 0.9500 . ? C13A C14A 1.365(5) . ? C13A C18A 1.399(5) . ? C13A H225 0.9500 . ? C14A O6A 1.364(4) . ? C14A C15A 1.405(5) . ? C15A O5A 1.372(4) . ? C15A C16A 1.386(5) . ? C16A C17A 1.412(5) . ? C17A C18A 1.391(5) . ? C17A H220 0.9500 . ? C18A H230 0.9500 . ? C19A N1A 1.354(5) . ? C19A C20A 1.391(5) . ? C19A H232 0.9500 . ? C20A C21A 1.412(6) . ? C20A C30A 1.505(5) . ? C21A C22A 1.414(5) . ? C21A C32A 1.508(5) . ? C22A N1A 1.372(5) . ? C22A C23A 1.419(5) . ? C23A O3A 1.326(4) . ? C23A C24A 1.387(5) . ? C24A C25A 1.393(5) . ? C24A H229 0.9500 . ? C25A O4A 1.331(4) . ? C25A C26A 1.422(5) . ? C26A N2A 1.389(5) . ? C26A C27A 1.434(5) . ? C27A C28A 1.390(6) . ? C27A C34A 1.539(6) . ? C28A C29A 1.415(5) . ? C28A C36A 1.526(6) . ? C29A N2A 1.346(5) . ? C29A H29A 0.9500 . ? C30A C31A 1.511(6) . ? C30A H101 0.9900 . ? C30A H102 0.9900 . ? C31A H105 0.9800 . ? C31A H106 0.9800 . ? C31A H107 0.9800 . ? C32A C33A 1.521(6) . ? C32A H103 0.9900 . ? C32A H104 0.9900 . ? C33A H118 0.9800 . ? C33A H119 0.9800 . ? C33A H120 0.9800 . ? C34A C35A 1.516(6) . ? C34A H110 0.9900 . ? C34A H111 0.9900 . ? C35A H112 0.9800 . ? C35A H113 0.9800 . ? C35A H114 0.9800 . ? C36A C37A 1.524(6) . ? C36A H108 0.9900 . ? C36A H109 0.9900 . ? C37A H115 0.9800 . ? C37A H116 0.9800 . ? C37A H117 0.9800 . ? C38A N3A 1.335(5) . ? C38A C39A 1.408(5) . ? C38A H228 0.9500 . ? C39A C40A 1.414(5) . ? C39A C49A 1.491(5) . ? C40A C41A 1.398(5) . ? C40A C51A 1.512(5) . ? C41A N3A 1.383(5) . ? C41A C42A 1.437(5) . ? C42A O7A 1.321(4) . ? C42A C43A 1.382(5) . ? C43A C44A 1.382(5) . ? C43A H221 0.9500 . ? C44A O8A 1.326(4) . ? C44A C45A 1.438(5) . ? C45A N4A 1.380(4) . ? C45A C46A 1.416(5) . ? C46A C47A 1.405(5) . ? C46A C53A 1.499(4) . ? C47A C48A 1.386(5) . ? C47A C55A 1.503(5) . ? C48A N4A 1.339(5) . ? C48A H222 0.9500 . ? C49A C50A 1.548(5) . ? C49A H85 0.9900 . ? C49A H86 0.9900 . ? C50A H95 0.9800 . ? C50A H96 0.9800 . ? C50A H97 0.9800 . ? C51A C52A 1.529(5) . ? C51A H83 0.9900 . ? C51A H84 0.9900 . ? C52A H90 0.9800 . ? C52A H91 0.9800 . ? C52A H92 0.9800 . ? C53A C54A 1.531(5) . ? C53A H81 0.9900 . ? C53A H82 0.9900 . ? C54A H98 0.9800 . ? C54A H99 0.9800 . ? C54A H100 0.9800 . ? C55A C56A 1.540(5) . ? C55A H93 0.9900 . ? C55A H94 0.9900 . ? C56A H87 0.9800 . ? C56A H88 0.9800 . ? C56A H89 0.9800 . ? N1A H219 0.8800 . ? N2A H217 0.8800 . ? N3A H218 0.8800 . ? N4A H216 0.8800 . ? B1B O4B 1.452(5) . ? B1B O2B 1.475(5) . ? B1B O1B 1.484(5) . ? B1B O3B 1.489(5) . ? B2B O8B 1.466(5) . ? B2B O7B 1.475(5) . ? B2B O5B 1.479(5) . ? B2B O6B 1.483(5) . ? C1B C2B 1.394(5) . ? C1B C6B 1.430(5) . ? C1B C10B 1.479(5) . ? C2B O2B 1.364(4) . ? C2B C3B 1.397(5) . ? C3B O1B 1.359(4) . ? C3B C4B 1.373(5) . ? C4B C5B 1.410(5) . ? C4B H166 0.9500 . ? C5B C6B 1.375(5) . ? C5B H176 0.9500 . ? C6B H169 0.9500 . ? C7B C8B 1.409(5) . ? C7B C12B 1.410(5) . ? C7B C16B 1.469(5) . ? C8B C9B 1.379(5) . ? C8B H171 0.9500 . ? C9B C10B 1.417(5) . ? C9B H179 0.9500 . ? C10B C11B 1.387(5) . ? C11B C12B 1.391(5) . ? C11B H177 0.9500 . ? C12B H178 0.9500 . ? C13B C14B 1.369(5) . ? C13B C18B 1.396(5) . ? C13B H175 0.9500 . ? C14B O6B 1.365(4) . ? C14B C15B 1.402(5) . ? C15B O5B 1.358(4) . ? C15B C16B 1.391(5) . ? C16B C17B 1.415(5) . ? C17B C18B 1.395(5) . ? C17B H170 0.9500 . ? C18B H174 0.9500 . ? C19B N1B 1.350(5) . ? C19B C20B 1.392(5) . ? C19B H172 0.9500 . ? C20B C21B 1.407(5) . ? C20B C30B 1.510(5) . ? C21B C22B 1.396(5) . ? C21B C32B 1.507(5) . ? C22B N1B 1.381(5) . ? C22B C23B 1.432(5) . ? C23B O3B 1.329(4) . ? C23B C24B 1.386(5) . ? C24B C25B 1.408(5) . ? C24B H167 0.9500 . ? C25B O4B 1.327(4) . ? C25B C26B 1.408(5) . ? C26B N2B 1.384(5) . ? C26B C27B 1.418(5) . ? C27B C28B 1.398(6) . ? C27B C34B 1.511(5) . ? C28B C29B 1.403(6) . ? C28B C36B 1.508(6) . ? C29B N2B 1.356(5) . ? C29B H180 0.9500 . ? C30B C31B 1.517(6) . ? C30B H63 0.9900 . ? C30B H64 0.9900 . ? C31B H67 0.9800 . ? C31B H68 0.9800 . ? C31B H69 0.9800 . ? C32B C33B 1.523(6) . ? C32B H61 0.9900 . ? C32B H62 0.9900 . ? C33B H70 0.9800 . ? C33B H71 0.9800 . ? C33B H72 0.9800 . ? C34B C35B 1.526(7) . ? C34B H65 0.9900 . ? C34B H66 0.9900 . ? C35B H73 0.9800 . ? C35B H74 0.9800 . ? C35B H75 0.9800 . ? C36B C37B 1.506(7) . ? C36B H76 0.9900 . ? C36B H77 0.9900 . ? C37B H78 0.9800 . ? C37B H79 0.9800 . ? C37B H80 0.9800 . ? C38B N3B 1.347(5) . ? C38B C39B 1.390(5) . ? C38B H168 0.9500 . ? C39B C40B 1.392(5) . ? C39B C49B 1.506(5) . ? C40B C41B 1.411(5) . ? C40B C51B 1.515(5) . ? C41B N3B 1.370(5) . ? C41B C42B 1.430(5) . ? C42B O7B 1.321(4) . ? C42B C43B 1.384(5) . ? C43B C44B 1.399(5) . ? C43B H165 0.9500 . ? C44B O8B 1.329(4) . ? C44B C45B 1.431(5) . ? C45B N4B 1.370(4) . ? C45B C46B 1.415(5) . ? C46B C47B 1.406(5) . ? C46B C53B 1.506(5) . ? C47B C48B 1.392(5) . ? C47B C55B 1.504(5) . ? C48B N4B 1.352(5) . ? C48B H173 0.9500 . ? C49B C50B 1.512(7) . ? C49B H51 0.9900 . ? C49B H52 0.9900 . ? C50B H58 0.9800 . ? C50B H59 0.9800 . ? C50B H60 0.9800 . ? C51B C52B 1.526(5) . ? C51B H41 0.9900 . ? C51B H42 0.9900 . ? C52B H43 0.9800 . ? C52B H44 0.9800 . ? C52B H45 0.9800 . ? C53B C54B 1.540(5) . ? C53B H46 0.9900 . ? C53B H47 0.9900 . ? C54B H48 0.9800 . ? C54B H49 0.9800 . ? C54B H50 0.9800 . ? C55B C56B 1.549(6) . ? C55B H53 0.9900 . ? C55B H54 0.9900 . ? C56B H55 0.9800 . ? C56B H56 0.9800 . ? C56B H57 0.9800 . ? N1B H162 0.8800 . ? N2B H164 0.8800 . ? N3B H161 0.8800 . ? N4B H163 0.8800 . ? B1C O1C 1.456(5) . ? B1C O3C 1.473(5) . ? B1C O4C 1.474(5) . ? B1C O2C 1.484(5) . ? B2C O8C 1.457(5) . ? B2C O5C 1.477(4) . ? B2C O6C 1.481(5) . ? B2C O7C 1.486(5) . ? C1C C2C 1.389(5) . ? C1C C6C 1.409(5) . ? C1C C10C 1.487(4) . ? C2C O2C 1.360(4) . ? C2C C3C 1.403(5) . ? C3C O1C 1.363(4) . ? C3C C4C 1.379(5) . ? C4C C5C 1.387(6) . ? C4C H185 0.9500 . ? C5C C6C 1.392(5) . ? C5C H194 0.9500 . ? C6C H188 0.9500 . ? C7C C12C 1.397(5) . ? C7C C8C 1.404(5) . ? C7C C16C 1.479(4) . ? C8C C9C 1.383(5) . ? C8C H183 0.9500 . ? C9C C10C 1.403(5) . ? C9C H187 0.9500 . ? C10C C11C 1.408(5) . ? C11C C12C 1.383(5) . ? C11C H191 0.9500 . ? C12C H193 0.9500 . ? C13C C14C 1.373(5) . ? C13C C18C 1.414(5) . ? C13C H184 0.9500 . ? C14C O6C 1.359(4) . ? C14C C15C 1.397(5) . ? C15C O5C 1.360(4) . ? C15C C16C 1.393(5) . ? C16C C17C 1.418(5) . ? C17C C18C 1.378(5) . ? C17C H189 0.9500 . ? C18C H186 0.9500 . ? C19C N1C 1.344(5) . ? C19C C20C 1.394(6) . ? C19C H195 0.9500 . ? C20C C21C 1.412(6) . ? C20C C30C 1.505(5) . ? C21C C22C 1.406(5) . ? C21C C32C 1.490(6) . ? C22C N1C 1.379(6) . ? C22C C23C 1.439(5) . ? C23C O3C 1.321(4) . ? C23C C24C 1.391(6) . ? C24C C25C 1.396(5) . ? C24C H192 0.9500 . ? C25C O4C 1.330(4) . ? C25C C26C 1.422(5) . ? C26C N2C 1.389(5) . ? C26C C27C 1.407(6) . ? C27C C28C 1.409(6) . ? C27C C34C 1.515(6) . ? C28C C29C 1.396(6) . ? C28C C36C 1.539(7) . ? C29C N2C 1.359(5) . ? C29C H190 0.9500 . ? C30C C31C 1.528(6) . ? C30C H23 0.9900 . ? C30C H24 0.9900 . ? C31C H28 0.9800 . ? C31C H29 0.9800 . ? C31C H30 0.9800 . ? C32C C33C 1.533(6) . ? C32C H21 0.9900 . ? C32C H22 0.9900 . ? C33C H25 0.9800 . ? C33C H26 0.9800 . ? C33C H27 0.9800 . ? C34C C35C 1.522(8) . ? C34C H31 0.9900 . ? C34C H32 0.9900 . ? C35C H38 0.9800 . ? C35C H39 0.9800 . ? C35C H40 0.9800 . ? C36C C37C 1.521(8) . ? C36C H33 0.9900 . ? C36C H34 0.9900 . ? C37C H35 0.9800 . ? C37C H36 0.9800 . ? C37C H37 0.9800 . ? C38C N3C 1.353(5) . ? C38C C39C 1.401(7) . ? C38C H38C 0.9500 . ? C39C C40C 1.399(7) . ? C39C C49C 1.510(6) . ? C40C C41C 1.410(5) . ? C40C C51C 1.506(6) . ? C41C N3C 1.391(5) . ? C41C C42C 1.425(6) . ? C42C O7C 1.328(4) . ? C42C C43C 1.391(6) . ? C43C C44C 1.386(6) . ? C43C H236 0.9500 . ? C44C O8C 1.314(4) . ? C44C C45C 1.429(6) . ? C45C N4C 1.384(6) . ? C45C C46C 1.409(5) . ? C46C C47C 1.401(7) . ? C46C C53C 1.494(6) . ? C47C C48C 1.392(7) . ? C47C C55C 1.518(7) . ? C48C N4C 1.342(6) . ? C48C H48C 0.9500 . ? C49C C50C 1.523(6) . ? C49C H9 0.9900 . ? C49C H10 0.9900 . ? C50C H1 0.9800 . ? C50C H2 0.9800 . ? C50C H3 0.9800 . ? C51C C52C 1.529(6) . ? C51C H4 0.9900 . ? C51C H5 0.9900 . ? C52C H6 0.9800 . ? C52C H7 0.9800 . ? C52C H8 0.9800 . ? C53C C54C 1.532(6) . ? C53C H14 0.9900 . ? C53C H15 0.9900 . ? C54C H11 0.9800 . ? C54C H12 0.9800 . ? C54C H13 0.9800 . ? C55C C56C 1.312(10) . ? C55C H19 0.9900 . ? C55C H20 0.9900 . ? C56C H16 0.9800 . ? C56C H17 0.9800 . ? C56C H18 0.9800 . ? N1C H182 0.8800 . ? N2C H181 0.8800 . ? N3C H3C 0.8800 . ? N4C H4C 0.8800 . ? B1D O1D 1.459(5) . ? B1D O4D 1.467(6) . ? B1D O3D 1.473(5) . ? B1D O2D 1.488(5) . ? B2D O6D 1.469(5) . ? B2D O8D 1.469(5) . ? B2D O7D 1.476(5) . ? B2D O5D 1.484(5) . ? C1D C2D 1.392(5) . ? C1D C6D 1.413(5) . ? C1D C10D 1.478(5) . ? C2D O2D 1.369(4) . ? C2D C3D 1.404(5) . ? C3D O1D 1.367(4) . ? C3D C4D 1.368(5) . ? C4D C5D 1.392(6) . ? C4D H211 0.9500 . ? C5D C6D 1.394(5) . ? C5D H205 0.9500 . ? C6D H207 0.9500 . ? C7D C12D 1.388(5) . ? C7D C8D 1.401(5) . ? C7D C16D 1.492(5) . ? C8D C9D 1.390(5) . ? C8D H214 0.9500 . ? C9D C10D 1.402(5) . ? C9D H208 0.9500 . ? C10D C11D 1.406(5) . ? C11D C12D 1.385(5) . ? C11D H210 0.9500 . ? C12D H213 0.9500 . ? C13D C14D 1.369(5) . ? C13D C18D 1.404(5) . ? C13D H196 0.9500 . ? C14D O6D 1.357(4) . ? C14D C15D 1.406(5) . ? C15D O5D 1.364(4) . ? C15D C16D 1.388(5) . ? C16D C17D 1.409(5) . ? C17D C18D 1.377(5) . ? C17D H203 0.9500 . ? C18D H201 0.9500 . ? C19D N1D 1.334(5) . ? C19D C20D 1.388(6) . ? C19D H206 0.9500 . ? C20D C21D 1.400(6) . ? C20D C30D 1.513(6) . ? C21D C22D 1.415(5) . ? C21D C32D 1.497(6) . ? C22D N1D 1.385(5) . ? C22D C23D 1.424(6) . ? C23D O3D 1.319(4) . ? C23D C24D 1.397(6) . ? C24D C25D 1.398(6) . ? C24D H209 0.9500 . ? C25D O4D 1.318(5) . ? C25D C26D 1.422(6) . ? C26D N2D 1.388(6) . ? C26D C27D 1.402(6) . ? C27D C28D 1.409(7) . ? C27D C34D 1.506(7) . ? C28D C29D 1.390(7) . ? C28D C36D 1.538(7) . ? C29D N2D 1.359(6) . ? C29D H215 0.9500 . ? C30D C31D 1.532(6) . ? C30D H143 0.9900 . ? C30D H144 0.9900 . ? C31D H145 0.9800 . ? C31D H146 0.9800 . ? C31D H147 0.9800 . ? C32D C33D 1.534(6) . ? C32D H141 0.9900 . ? C32D H142 0.9900 . ? C33D H148 0.9800 . ? C33D H149 0.9800 . ? C33D H150 0.9800 . ? C34D C35D 1.516(6) . ? C34D H151 0.9900 . ? C34D H152 0.9900 . ? C35D H153 0.9800 . ? C35D H154 0.9800 . ? C35D H155 0.9800 . ? C36D C37D 1.445(9) . ? C36D H156 0.9900 . ? C36D H157 0.9900 . ? C37D H158 0.9800 . ? C37D H159 0.9800 . ? C37D H160 0.9800 . ? C38D N3D 1.351(5) . ? C38D C39D 1.398(6) . ? C38D H212 0.9500 . ? C39D C40D 1.412(5) . ? C39D C49D 1.504(5) . ? C40D C41D 1.413(5) . ? C40D C51D 1.500(5) . ? C41D N3D 1.378(5) . ? C41D C42D 1.440(5) . ? C42D O7D 1.331(4) . ? C42D C43D 1.359(5) . ? C43D C44D 1.405(5) . ? C43D H200 0.9500 . ? C44D O8D 1.328(4) . ? C44D C45D 1.423(5) . ? C45D N4D 1.377(4) . ? C45D C46D 1.404(5) . ? C46D C47D 1.410(5) . ? C46D C53D 1.515(5) . ? C47D C48D 1.401(5) . ? C47D C55D 1.498(6) . ? C48D N4D 1.346(5) . ? C48D H204 0.9500 . ? C49D C50D 1.519(5) . ? C49D H128 0.9900 . ? C49D H129 0.9900 . ? C50D H135 0.9800 . ? C50D H136 0.9800 . ? C50D H137 0.9800 . ? C51D C52D 1.541(5) . ? C51D H121 0.9900 . ? C51D H122 0.9900 . ? C52D H132 0.9800 . ? C52D H133 0.9800 . ? C52D H134 0.9800 . ? C53D C54D 1.539(5) . ? C53D H123 0.9900 . ? C53D H124 0.9900 . ? C54D H125 0.9800 . ? C54D H126 0.9800 . ? C54D H127 0.9800 . ? C55D C56D 1.511(6) . ? C55D H130 0.9900 . ? C55D H131 0.9900 . ? C56D H138 0.9800 . ? C56D H139 0.9800 . ? C56D H140 0.9800 . ? N1D H198 0.8800 . ? N2D H202 0.8800 . ? N3D H199 0.8800 . ? N4D H197 0.8800 . ? 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 O1A B1A O2A 106.0(3) . . ? O1A B1A O4A 111.0(3) . . ? O2A B1A O4A 109.7(3) . . ? O1A B1A O3A 108.0(3) . . ? O2A B1A O3A 110.6(3) . . ? O4A B1A O3A 111.3(3) . . ? O7A B2A O6A 111.4(3) . . ? O7A B2A O8A 111.7(3) . . ? O6A B2A O8A 109.1(3) . . ? O7A B2A O5A 108.4(3) . . ? O6A B2A O5A 106.1(3) . . ? O8A B2A O5A 110.0(3) . . ? C2A C1A C6A 115.0(3) . . ? C2A C1A C10A 122.9(3) . . ? C6A C1A C10A 122.0(3) . . ? O2A C2A C1A 127.8(3) . . ? O2A C2A C3A 109.8(3) . . ? C1A C2A C3A 122.4(3) . . ? O1A C3A C4A 127.3(3) . . ? O1A C3A C2A 110.8(3) . . ? C4A C3A C2A 121.9(3) . . ? C3A C4A C5A 116.4(3) . . ? C3A C4A H231 121.8 . . ? C5A C4A H231 121.8 . . ? C6A C5A C4A 121.8(3) . . ? C6A C5A H234 119.1 . . ? C4A C5A H234 119.1 . . ? C5A C6A C1A 122.5(3) . . ? C5A C6A H227 118.8 . . ? C1A C6A H227 118.8 . . ? C12A C7A C8A 117.3(3) . . ? C12A C7A C16A 120.4(3) . . ? C8A C7A C16A 122.3(3) . . ? C9A C8A C7A 120.8(3) . . ? C9A C8A H223 119.6 . . ? C7A C8A H223 119.6 . . ? C10A C9A C8A 122.1(4) . . ? C10A C9A H235 119.0 . . ? C8A C9A H235 119.0 . . ? C9A C10A C11A 117.4(3) . . ? C9A C10A C1A 122.4(3) . . ? C11A C10A C1A 120.2(3) . . ? C12A C11A C10A 121.0(3) . . ? C12A C11A H233 119.5 . . ? C10A C11A H233 119.5 . . ? C11A C12A C7A 121.4(3) . . ? C11A C12A H226 119.3 . . ? C7A C12A H226 119.3 . . ? C14A C13A C18A 117.4(3) . . ? C14A C13A H225 121.3 . . ? C18A C13A H225 121.3 . . ? O6A C14A C13A 127.8(3) . . ? O6A C14A C15A 110.6(3) . . ? C13A C14A C15A 121.6(3) . . ? O5A C15A C16A 127.6(3) . . ? O5A C15A C14A 110.1(3) . . ? C16A C15A C14A 122.2(3) . . ? C15A C16A C17A 115.5(3) . . ? C15A C16A C7A 123.1(3) . . ? C17A C16A C7A 121.4(3) . . ? C18A C17A C16A 121.9(3) . . ? C18A C17A H220 119.0 . . ? C16A C17A H220 119.0 . . ? C17A C18A C13A 121.1(3) . . ? C17A C18A H230 119.4 . . ? C13A C18A H230 119.4 . . ? N1A C19A C20A 108.8(3) . . ? N1A C19A H232 125.6 . . ? C20A C19A H232 125.6 . . ? C19A C20A C21A 107.2(3) . . ? C19A C20A C30A 127.1(4) . . ? C21A C20A C30A 125.6(3) . . ? C20A C21A C22A 106.6(3) . . ? C20A C21A C32A 124.0(3) . . ? C22A C21A C32A 129.4(4) . . ? N1A C22A C21A 107.6(3) . . ? N1A C22A C23A 119.1(3) . . ? C21A C22A C23A 133.3(3) . . ? O3A C23A C24A 120.3(3) . . ? O3A C23A C22A 114.0(3) . . ? C24A C23A C22A 125.7(3) . . ? C23A C24A C25A 120.3(3) . . ? C23A C24A H229 119.9 . . ? C25A C24A H229 119.9 . . ? O4A C25A C24A 121.3(3) . . ? O4A C25A C26A 113.8(3) . . ? C24A C25A C26A 124.9(3) . . ? N2A C26A C25A 120.1(3) . . ? N2A C26A C27A 107.0(3) . . ? C25A C26A C27A 132.9(3) . . ? C28A C27A C26A 107.1(3) . . ? C28A C27A C34A 125.7(4) . . ? C26A C27A C34A 127.2(4) . . ? C27A C28A C29A 107.3(3) . . ? C27A C28A C36A 126.6(4) . . ? C29A C28A C36A 126.1(4) . . ? N2A C29A C28A 109.2(3) . . ? N2A C29A H29A 125.4 . . ? C28A C29A H29A 125.4 . . ? C20A C30A C31A 114.6(3) . . ? C20A C30A H101 108.6 . . ? C31A C30A H101 108.6 . . ? C20A C30A H102 108.6 . . ? C31A C30A H102 108.6 . . ? H101 C30A H102 107.6 . . ? C30A C31A H105 109.5 . . ? C30A C31A H106 109.5 . . ? H105 C31A H106 109.5 . . ? C30A C31A H107 109.5 . . ? H105 C31A H107 109.5 . . ? H106 C31A H107 109.5 . . ? C21A C32A C33A 111.9(3) . . ? C21A C32A H103 109.2 . . ? C33A C32A H103 109.2 . . ? C21A C32A H104 109.2 . . ? C33A C32A H104 109.2 . . ? H103 C32A H104 107.9 . . ? C32A C33A H118 109.5 . . ? C32A C33A H119 109.5 . . ? H118 C33A H119 109.5 . . ? C32A C33A H120 109.5 . . ? H118 C33A H120 109.5 . . ? H119 C33A H120 109.5 . . ? C35A C34A C27A 111.1(4) . . ? C35A C34A H110 109.4 . . ? C27A C34A H110 109.4 . . ? C35A C34A H111 109.4 . . ? C27A C34A H111 109.4 . . ? H110 C34A H111 108.0 . . ? C34A C35A H112 109.5 . . ? C34A C35A H113 109.5 . . ? H112 C35A H113 109.5 . . ? C34A C35A H114 109.5 . . ? H112 C35A H114 109.5 . . ? H113 C35A H114 109.5 . . ? C37A C36A C28A 112.3(4) . . ? C37A C36A H108 109.2 . . ? C28A C36A H108 109.2 . . ? C37A C36A H109 109.2 . . ? C28A C36A H109 109.2 . . ? H108 C36A H109 107.9 . . ? C36A C37A H115 109.5 . . ? C36A C37A H116 109.5 . . ? H115 C37A H116 109.5 . . ? C36A C37A H117 109.5 . . ? H115 C37A H117 109.5 . . ? H116 C37A H117 109.5 . . ? N3A C38A C39A 109.2(3) . . ? N3A C38A H228 125.4 . . ? C39A C38A H228 125.4 . . ? C38A C39A C40A 106.0(3) . . ? C38A C39A C49A 126.2(3) . . ? C40A C39A C49A 127.8(3) . . ? C41A C40A C39A 107.6(3) . . ? C41A C40A C51A 127.5(3) . . ? C39A C40A C51A 124.8(3) . . ? N3A C41A C40A 107.2(3) . . ? N3A C41A C42A 118.4(3) . . ? C40A C41A C42A 134.3(3) . . ? O7A C42A C43A 120.7(3) . . ? O7A C42A C41A 113.4(3) . . ? C43A C42A C41A 125.9(3) . . ? C42A C43A C44A 119.8(3) . . ? C42A C43A H221 120.1 . . ? C44A C43A H221 120.1 . . ? O8A C44A C43A 121.3(3) . . ? O8A C44A C45A 112.5(3) . . ? C43A C44A C45A 126.2(3) . . ? N4A C45A C46A 106.5(3) . . ? N4A C45A C44A 119.3(3) . . ? C46A C45A C44A 134.2(3) . . ? C47A C46A C45A 107.1(3) . . ? C47A C46A C53A 125.0(3) . . ? C45A C46A C53A 127.9(3) . . ? C48A C47A C46A 107.1(3) . . ? C48A C47A C55A 126.6(3) . . ? C46A C47A C55A 126.2(3) . . ? N4A C48A C47A 109.2(3) . . ? N4A C48A H222 125.4 . . ? C47A C48A H222 125.4 . . ? C39A C49A C50A 112.4(3) . . ? C39A C49A H85 109.1 . . ? C50A C49A H85 109.1 . . ? C39A C49A H86 109.1 . . ? C50A C49A H86 109.1 . . ? H85 C49A H86 107.9 . . ? C49A C50A H95 109.5 . . ? C49A C50A H96 109.5 . . ? H95 C50A H96 109.5 . . ? C49A C50A H97 109.5 . . ? H95 C50A H97 109.5 . . ? H96 C50A H97 109.5 . . ? C40A C51A C52A 113.3(3) . . ? C40A C51A H83 108.9 . . ? C52A C51A H83 108.9 . . ? C40A C51A H84 108.9 . . ? C52A C51A H84 108.9 . . ? H83 C51A H84 107.7 . . ? C51A C52A H90 109.5 . . ? C51A C52A H91 109.5 . . ? H90 C52A H91 109.5 . . ? C51A C52A H92 109.5 . . ? H90 C52A H92 109.5 . . ? H91 C52A H92 109.5 . . ? C46A C53A C54A 112.4(3) . . ? C46A C53A H81 109.1 . . ? C54A C53A H81 109.1 . . ? C46A C53A H82 109.1 . . ? C54A C53A H82 109.1 . . ? H81 C53A H82 107.9 . . ? C53A C54A H98 109.5 . . ? C53A C54A H99 109.5 . . ? H98 C54A H99 109.5 . . ? C53A C54A H100 109.5 . . ? H98 C54A H100 109.5 . . ? H99 C54A H100 109.5 . . ? C47A C55A C56A 115.1(3) . . ? C47A C55A H93 108.5 . . ? C56A C55A H93 108.5 . . ? C47A C55A H94 108.5 . . ? C56A C55A H94 108.5 . . ? H93 C55A H94 107.5 . . ? C55A C56A H87 109.5 . . ? C55A C56A H88 109.5 . . ? H87 C56A H88 109.5 . . ? C55A C56A H89 109.5 . . ? H87 C56A H89 109.5 . . ? H88 C56A H89 109.5 . . ? C19A N1A C22A 109.7(3) . . ? C19A N1A H219 125.2 . . ? C22A N1A H219 125.2 . . ? C29A N2A C26A 109.3(3) . . ? C29A N2A H217 125.3 . . ? C26A N2A H217 125.3 . . ? C38A N3A C41A 109.9(3) . . ? C38A N3A H218 125.0 . . ? C41A N3A H218 125.0 . . ? C48A N4A C45A 110.1(3) . . ? C48A N4A H216 124.9 . . ? C45A N4A H216 124.9 . . ? C3A O1A B1A 105.8(3) . . ? C2A O2A B1A 106.4(3) . . ? C23A O3A B1A 122.1(3) . . ? C25A O4A B1A 120.8(3) . . ? C15A O5A B2A 106.4(3) . . ? C14A O6A B2A 106.6(3) . . ? C42A O7A B2A 123.6(3) . . ? C44A O8A B2A 122.6(3) . . ? O4B B1B O2B 110.8(3) . . ? O4B B1B O1B 110.5(3) . . ? O2B B1B O1B 105.6(3) . . ? O4B B1B O3B 111.4(3) . . ? O2B B1B O3B 109.8(3) . . ? O1B B1B O3B 108.6(3) . . ? O8B B2B O7B 112.1(3) . . ? O8B B2B O5B 109.6(3) . . ? O7B B2B O5B 109.7(3) . . ? O8B B2B O6B 111.1(3) . . ? O7B B2B O6B 109.0(3) . . ? O5B B2B O6B 105.1(3) . . ? C2B C1B C6B 115.0(3) . . ? C2B C1B C10B 123.2(3) . . ? C6B C1B C10B 121.8(3) . . ? O2B C2B C1B 127.1(3) . . ? O2B C2B C3B 110.3(3) . . ? C1B C2B C3B 122.6(3) . . ? O1B C3B C4B 127.1(3) . . ? O1B C3B C2B 111.0(3) . . ? C4B C3B C2B 121.9(3) . . ? C3B C4B C5B 116.8(3) . . ? C3B C4B H166 121.6 . . ? C5B C4B H166 121.6 . . ? C6B C5B C4B 121.8(3) . . ? C6B C5B H176 119.1 . . ? C4B C5B H176 119.1 . . ? C5B C6B C1B 121.9(3) . . ? C5B C6B H169 119.1 . . ? C1B C6B H169 119.1 . . ? C8B C7B C12B 116.0(3) . . ? C8B C7B C16B 121.9(3) . . ? C12B C7B C16B 122.0(3) . . ? C9B C8B C7B 122.4(3) . . ? C9B C8B H171 118.8 . . ? C7B C8B H171 118.8 . . ? C8B C9B C10B 121.2(3) . . ? C8B C9B H179 119.4 . . ? C10B C9B H179 119.4 . . ? C11B C10B C9B 116.8(3) . . ? C11B C10B C1B 122.8(3) . . ? C9B C10B C1B 120.3(3) . . ? C10B C11B C12B 122.2(3) . . ? C10B C11B H177 118.9 . . ? C12B C11B H177 118.9 . . ? C11B C12B C7B 121.5(3) . . ? C11B C12B H178 119.3 . . ? C7B C12B H178 119.3 . . ? C14B C13B C18B 117.3(3) . . ? C14B C13B H175 121.3 . . ? C18B C13B H175 121.3 . . ? O6B C14B C13B 127.9(3) . . ? O6B C14B C15B 110.4(3) . . ? C13B C14B C15B 121.7(3) . . ? O5B C15B C16B 127.2(3) . . ? O5B C15B C14B 110.4(3) . . ? C16B C15B C14B 122.3(3) . . ? C15B C16B C17B 115.5(3) . . ? C15B C16B C7B 123.0(3) . . ? C17B C16B C7B 121.5(3) . . ? C18B C17B C16B 121.7(3) . . ? C18B C17B H170 119.2 . . ? C16B C17B H170 119.2 . . ? C17B C18B C13B 121.4(3) . . ? C17B C18B H174 119.3 . . ? C13B C18B H174 119.3 . . ? N1B C19B C20B 109.3(4) . . ? N1B C19B H172 125.4 . . ? C20B C19B H172 125.4 . . ? C19B C20B C21B 106.4(3) . . ? C19B C20B C30B 125.3(4) . . ? C21B C20B C30B 128.2(3) . . ? C22B C21B C20B 107.7(3) . . ? C22B C21B C32B 127.6(3) . . ? C20B C21B C32B 124.7(3) . . ? N1B C22B C21B 107.4(3) . . ? N1B C22B C23B 118.4(3) . . ? C21B C22B C23B 134.1(3) . . ? O3B C23B C24B 120.8(3) . . ? O3B C23B C22B 113.7(3) . . ? C24B C23B C22B 125.5(3) . . ? C23B C24B C25B 119.6(3) . . ? C23B C24B H167 120.2 . . ? C25B C24B H167 120.2 . . ? O4B C25B C26B 114.1(3) . . ? O4B C25B C24B 119.7(3) . . ? C26B C25B C24B 126.2(3) . . ? N2B C26B C25B 119.0(3) . . ? N2B C26B C27B 106.7(3) . . ? C25B C26B C27B 134.3(3) . . ? C28B C27B C26B 107.9(3) . . ? C28B C27B C34B 125.2(4) . . ? C26B C27B C34B 126.9(4) . . ? C27B C28B C29B 106.8(4) . . ? C27B C28B C36B 126.5(4) . . ? C29B C28B C36B 126.7(4) . . ? N2B C29B C28B 109.0(3) . . ? N2B C29B H180 125.5 . . ? C28B C29B H180 125.5 . . ? C20B C30B C31B 114.4(3) . . ? C20B C30B H63 108.7 . . ? C31B C30B H63 108.7 . . ? C20B C30B H64 108.7 . . ? C31B C30B H64 108.7 . . ? H63 C30B H64 107.6 . . ? C30B C31B H67 109.5 . . ? C30B C31B H68 109.5 . . ? H67 C31B H68 109.5 . . ? C30B C31B H69 109.5 . . ? H67 C31B H69 109.5 . . ? H68 C31B H69 109.5 . . ? C21B C32B C33B 112.2(3) . . ? C21B C32B H61 109.2 . . ? C33B C32B H61 109.2 . . ? C21B C32B H62 109.2 . . ? C33B C32B H62 109.2 . . ? H61 C32B H62 107.9 . . ? C32B C33B H70 109.5 . . ? C32B C33B H71 109.5 . . ? H70 C33B H71 109.5 . . ? C32B C33B H72 109.5 . . ? H70 C33B H72 109.5 . . ? H71 C33B H72 109.5 . . ? C27B C34B C35B 111.8(3) . . ? C27B C34B H65 109.3 . . ? C35B C34B H65 109.3 . . ? C27B C34B H66 109.3 . . ? C35B C34B H66 109.3 . . ? H65 C34B H66 107.9 . . ? C34B C35B H73 109.5 . . ? C34B C35B H74 109.5 . . ? H73 C35B H74 109.5 . . ? C34B C35B H75 109.5 . . ? H73 C35B H75 109.5 . . ? H74 C35B H75 109.5 . . ? C37B C36B C28B 114.2(4) . . ? C37B C36B H76 108.7 . . ? C28B C36B H76 108.7 . . ? C37B C36B H77 108.7 . . ? C28B C36B H77 108.7 . . ? H76 C36B H77 107.6 . . ? C36B C37B H78 109.5 . . ? C36B C37B H79 109.5 . . ? H78 C37B H79 109.5 . . ? C36B C37B H80 109.5 . . ? H78 C37B H80 109.5 . . ? H79 C37B H80 109.5 . . ? N3B C38B C39B 108.7(3) . . ? N3B C38B H168 125.6 . . ? C39B C38B H168 125.6 . . ? C38B C39B C40B 107.1(3) . . ? C38B C39B C49B 126.7(4) . . ? C40B C39B C49B 126.2(4) . . ? C39B C40B C41B 107.3(3) . . ? C39B C40B C51B 124.1(3) . . ? C41B C40B C51B 128.4(3) . . ? N3B C41B C40B 106.9(3) . . ? N3B C41B C42B 118.7(3) . . ? C40B C41B C42B 134.3(4) . . ? O7B C42B C43B 120.8(3) . . ? O7B C42B C41B 113.7(3) . . ? C43B C42B C41B 125.5(3) . . ? C42B C43B C44B 119.7(3) . . ? C42B C43B H165 120.1 . . ? C44B C43B H165 120.1 . . ? O8B C44B C43B 120.8(3) . . ? O8B C44B C45B 113.7(3) . . ? C43B C44B C45B 125.5(3) . . ? N4B C45B C46B 107.4(3) . . ? N4B C45B C44B 119.1(3) . . ? C46B C45B C44B 133.3(3) . . ? C47B C46B C45B 106.8(3) . . ? C47B C46B C53B 124.7(3) . . ? C45B C46B C53B 128.5(3) . . ? C48B C47B C46B 107.2(3) . . ? C48B C47B C55B 125.5(4) . . ? C46B C47B C55B 127.3(3) . . ? N4B C48B C47B 108.8(3) . . ? N4B C48B H173 125.6 . . ? C47B C48B H173 125.6 . . ? C39B C49B C50B 113.6(4) . . ? C39B C49B H51 108.8 . . ? C50B C49B H51 108.8 . . ? C39B C49B H52 108.8 . . ? C50B C49B H52 108.8 . . ? H51 C49B H52 107.7 . . ? C49B C50B H58 109.5 . . ? C49B C50B H59 109.5 . . ? H58 C50B H59 109.5 . . ? C49B C50B H60 109.5 . . ? H58 C50B H60 109.5 . . ? H59 C50B H60 109.5 . . ? C40B C51B C52B 111.4(3) . . ? C40B C51B H41 109.3 . . ? C52B C51B H41 109.3 . . ? C40B C51B H42 109.3 . . ? C52B C51B H42 109.3 . . ? H41 C51B H42 108.0 . . ? C51B C52B H43 109.5 . . ? C51B C52B H44 109.5 . . ? H43 C52B H44 109.5 . . ? C51B C52B H45 109.5 . . ? H43 C52B H45 109.5 . . ? H44 C52B H45 109.5 . . ? C46B C53B C54B 112.6(3) . . ? C46B C53B H46 109.1 . . ? C54B C53B H46 109.1 . . ? C46B C53B H47 109.1 . . ? C54B C53B H47 109.1 . . ? H46 C53B H47 107.8 . . ? C53B C54B H48 109.5 . . ? C53B C54B H49 109.5 . . ? H48 C54B H49 109.5 . . ? C53B C54B H50 109.5 . . ? H48 C54B H50 109.5 . . ? H49 C54B H50 109.5 . . ? C47B C55B C56B 114.0(4) . . ? C47B C55B H53 108.8 . . ? C56B C55B H53 108.8 . . ? C47B C55B H54 108.8 . . ? C56B C55B H54 108.8 . . ? H53 C55B H54 107.7 . . ? C55B C56B H55 109.5 . . ? C55B C56B H56 109.5 . . ? H55 C56B H56 109.5 . . ? C55B C56B H57 109.5 . . ? H55 C56B H57 109.5 . . ? H56 C56B H57 109.5 . . ? C19B N1B C22B 109.2(3) . . ? C19B N1B H162 125.4 . . ? C22B N1B H162 125.4 . . ? C29B N2B C26B 109.6(3) . . ? C29B N2B H164 125.2 . . ? C26B N2B H164 125.2 . . ? C38B N3B C41B 109.8(3) . . ? C38B N3B H161 125.1 . . ? C41B N3B H161 125.1 . . ? C48B N4B C45B 109.8(3) . . ? C48B N4B H163 125.1 . . ? C45B N4B H163 125.1 . . ? C3B O1B B1B 106.3(3) . . ? C2B O2B B1B 106.7(3) . . ? C23B O3B B1B 121.0(3) . . ? C25B O4B B1B 122.5(3) . . ? C15B O5B B2B 107.2(3) . . ? C14B O6B B2B 106.7(3) . . ? C42B O7B B2B 123.1(3) . . ? C44B O8B B2B 122.8(3) . . ? O1C B1C O3C 109.4(3) . . ? O1C B1C O4C 112.0(3) . . ? O3C B1C O4C 110.0(3) . . ? O1C B1C O2C 105.7(3) . . ? O3C B1C O2C 110.1(3) . . ? O4C B1C O2C 109.5(3) . . ? O8C B2C O5C 110.7(3) . . ? O8C B2C O6C 110.7(3) . . ? O5C B2C O6C 105.1(3) . . ? O8C B2C O7C 112.4(3) . . ? O5C B2C O7C 108.2(3) . . ? O6C B2C O7C 109.6(3) . . ? C2C C1C C6C 116.1(3) . . ? C2C C1C C10C 122.0(3) . . ? C6C C1C C10C 121.9(3) . . ? O2C C2C C1C 128.0(3) . . ? O2C C2C C3C 109.8(3) . . ? C1C C2C C3C 122.2(3) . . ? O1C C3C C4C 128.3(3) . . ? O1C C3C C2C 110.6(3) . . ? C4C C3C C2C 121.1(3) . . ? C3C C4C C5C 117.7(3) . . ? C3C C4C H185 121.2 . . ? C5C C4C H185 121.2 . . ? C4C C5C C6C 121.5(3) . . ? C4C C5C H194 119.2 . . ? C6C C5C H194 119.2 . . ? C5C C6C C1C 121.5(3) . . ? C5C C6C H188 119.3 . . ? C1C C6C H188 119.3 . . ? C12C C7C C8C 117.6(3) . . ? C12C C7C C16C 122.3(3) . . ? C8C C7C C16C 120.1(3) . . ? C9C C8C C7C 121.1(3) . . ? C9C C8C H183 119.5 . . ? C7C C8C H183 119.5 . . ? C8C C9C C10C 121.6(3) . . ? C8C C9C H187 119.2 . . ? C10C C9C H187 119.2 . . ? C9C C10C C11C 116.9(3) . . ? C9C C10C C1C 121.1(3) . . ? C11C C10C C1C 121.9(3) . . ? C12C C11C C10C 121.4(3) . . ? C12C C11C H191 119.3 . . ? C10C C11C H191 119.3 . . ? C11C C12C C7C 121.3(3) . . ? C11C C12C H193 119.3 . . ? C7C C12C H193 119.3 . . ? C14C C13C C18C 116.7(3) . . ? C14C C13C H184 121.7 . . ? C18C C13C H184 121.7 . . ? O6C C14C C13C 126.8(3) . . ? O6C C14C C15C 110.5(3) . . ? C13C C14C C15C 122.5(3) . . ? O5C C15C C16C 127.4(3) . . ? O5C C15C C14C 110.5(3) . . ? C16C C15C C14C 121.9(3) . . ? C15C C16C C17C 115.1(3) . . ? C15C C16C C7C 122.3(3) . . ? C17C C16C C7C 122.5(3) . . ? C18C C17C C16C 123.0(3) . . ? C18C C17C H189 118.5 . . ? C16C C17C H189 118.5 . . ? C17C C18C C13C 120.7(3) . . ? C17C C18C H186 119.6 . . ? C13C C18C H186 119.6 . . ? N1C C19C C20C 109.1(4) . . ? N1C C19C H195 125.5 . . ? C20C C19C H195 125.5 . . ? C19C C20C C21C 107.3(4) . . ? C19C C20C C30C 124.7(4) . . ? C21C C20C C30C 128.0(4) . . ? C22C C21C C20C 106.2(4) . . ? C22C C21C C32C 128.4(4) . . ? C20C C21C C32C 125.3(4) . . ? N1C C22C C21C 108.1(3) . . ? N1C C22C C23C 116.9(3) . . ? C21C C22C C23C 134.9(4) . . ? O3C C23C C24C 120.6(3) . . ? O3C C23C C22C 113.2(4) . . ? C24C C23C C22C 126.2(4) . . ? C23C C24C C25C 119.1(3) . . ? C23C C24C H192 120.5 . . ? C25C C24C H192 120.5 . . ? O4C C25C C24C 120.7(3) . . ? O4C C25C C26C 114.0(3) . . ? C24C C25C C26C 125.3(3) . . ? N2C C26C C27C 106.9(3) . . ? N2C C26C C25C 118.8(3) . . ? C27C C26C C25C 134.3(4) . . ? C26C C27C C28C 107.9(4) . . ? C26C C27C C34C 127.8(4) . . ? C28C C27C C34C 124.2(4) . . ? C29C C28C C27C 106.6(4) . . ? C29C C28C C36C 128.0(4) . . ? C27C C28C C36C 125.2(4) . . ? N2C C29C C28C 109.1(4) . . ? N2C C29C H190 125.4 . . ? C28C C29C H190 125.4 . . ? C20C C30C C31C 112.6(3) . . ? C20C C30C H23 109.1 . . ? C31C C30C H23 109.1 . . ? C20C C30C H24 109.1 . . ? C31C C30C H24 109.1 . . ? H23 C30C H24 107.8 . . ? C30C C31C H28 109.5 . . ? C30C C31C H29 109.5 . . ? H28 C31C H29 109.5 . . ? C30C C31C H30 109.5 . . ? H28 C31C H30 109.5 . . ? H29 C31C H30 109.5 . . ? C21C C32C C33C 113.1(3) . . ? C21C C32C H21 109.0 . . ? C33C C32C H21 109.0 . . ? C21C C32C H22 109.0 . . ? C33C C32C H22 109.0 . . ? H21 C32C H22 107.8 . . ? C32C C33C H25 109.5 . . ? C32C C33C H26 109.5 . . ? H25 C33C H26 109.5 . . ? C32C C33C H27 109.5 . . ? H25 C33C H27 109.5 . . ? H26 C33C H27 109.5 . . ? C27C C34C C35C 112.8(4) . . ? C27C C34C H31 109.0 . . ? C35C C34C H31 109.0 . . ? C27C C34C H32 109.0 . . ? C35C C34C H32 109.0 . . ? H31 C34C H32 107.8 . . ? C34C C35C H38 109.5 . . ? C34C C35C H39 109.5 . . ? H38 C35C H39 109.5 . . ? C34C C35C H40 109.5 . . ? H38 C35C H40 109.5 . . ? H39 C35C H40 109.5 . . ? C37C C36C C28C 113.1(5) . . ? C37C C36C H33 109.0 . . ? C28C C36C H33 109.0 . . ? C37C C36C H34 109.0 . . ? C28C C36C H34 109.0 . . ? H33 C36C H34 107.8 . . ? C36C C37C H35 109.5 . . ? C36C C37C H36 109.5 . . ? H35 C37C H36 109.5 . . ? C36C C37C H37 109.5 . . ? H35 C37C H37 109.5 . . ? H36 C37C H37 109.5 . . ? N3C C38C C39C 108.2(4) . . ? N3C C38C H38C 125.9 . . ? C39C C38C H38C 125.9 . . ? C40C C39C C38C 107.7(4) . . ? C40C C39C C49C 127.2(4) . . ? C38C C39C C49C 125.2(5) . . ? C39C C40C C41C 107.4(4) . . ? C39C C40C C51C 126.1(4) . . ? C41C C40C C51C 126.5(4) . . ? N3C C41C C40C 106.9(4) . . ? N3C C41C C42C 119.4(3) . . ? C40C C41C C42C 133.2(4) . . ? O7C C42C C43C 120.6(4) . . ? O7C C42C C41C 114.0(4) . . ? C43C C42C C41C 125.5(3) . . ? C44C C43C C42C 120.1(3) . . ? C44C C43C H236 120.0 . . ? C42C C43C H236 120.0 . . ? O8C C44C C43C 120.8(4) . . ? O8C C44C C45C 113.5(4) . . ? C43C C44C C45C 125.7(3) . . ? N4C C45C C46C 107.3(4) . . ? N4C C45C C44C 118.9(3) . . ? C46C C45C C44C 133.8(4) . . ? C47C C46C C45C 106.4(4) . . ? C47C C46C C53C 125.6(4) . . ? C45C C46C C53C 127.8(4) . . ? C48C C47C C46C 108.0(4) . . ? C48C C47C C55C 125.9(5) . . ? C46C C47C C55C 126.0(5) . . ? N4C C48C C47C 108.3(5) . . ? N4C C48C H48C 125.8 . . ? C47C C48C H48C 125.8 . . ? C39C C49C C50C 114.0(4) . . ? C39C C49C H9 108.8 . . ? C50C C49C H9 108.8 . . ? C39C C49C H10 108.8 . . ? C50C C49C H10 108.8 . . ? H9 C49C H10 107.6 . . ? C49C C50C H1 109.5 . . ? C49C C50C H2 109.5 . . ? H1 C50C H2 109.5 . . ? C49C C50C H3 109.5 . . ? H1 C50C H3 109.5 . . ? H2 C50C H3 109.5 . . ? C40C C51C C52C 112.9(4) . . ? C40C C51C H4 109.0 . . ? C52C C51C H4 109.0 . . ? C40C C51C H5 109.0 . . ? C52C C51C H5 109.0 . . ? H4 C51C H5 107.8 . . ? C51C C52C H6 109.5 . . ? C51C C52C H7 109.5 . . ? H6 C52C H7 109.5 . . ? C51C C52C H8 109.5 . . ? H6 C52C H8 109.5 . . ? H7 C52C H8 109.5 . . ? C46C C53C C54C 111.4(3) . . ? C46C C53C H14 109.4 . . ? C54C C53C H14 109.4 . . ? C46C C53C H15 109.4 . . ? C54C C53C H15 109.4 . . ? H14 C53C H15 108.0 . . ? C53C C54C H11 109.5 . . ? C53C C54C H12 109.5 . . ? H11 C54C H12 109.5 . . ? C53C C54C H13 109.5 . . ? H11 C54C H13 109.5 . . ? H12 C54C H13 109.5 . . ? C56C C55C C47C 120.1(6) . . ? C56C C55C H19 107.3 . . ? C47C C55C H19 107.3 . . ? C56C C55C H20 107.3 . . ? C47C C55C H20 107.3 . . ? H19 C55C H20 106.9 . . ? C55C C56C H16 109.5 . . ? C55C C56C H17 109.5 . . ? H16 C56C H17 109.5 . . ? C55C C56C H18 109.5 . . ? H16 C56C H18 109.5 . . ? H17 C56C H18 109.5 . . ? C19C N1C C22C 109.2(4) . . ? C19C N1C H182 125.4 . . ? C22C N1C H182 125.4 . . ? C29C N2C C26C 109.4(3) . . ? C29C N2C H181 125.3 . . ? C26C N2C H181 125.3 . . ? C38C N3C C41C 109.8(4) . . ? C38C N3C H3C 125.1 . . ? C41C N3C H3C 125.1 . . ? C48C N4C C45C 109.9(4) . . ? C48C N4C H4C 125.1 . . ? C45C N4C H4C 125.1 . . ? C3C O1C B1C 106.5(3) . . ? C2C O2C B1C 106.3(3) . . ? C23C O3C B1C 123.3(3) . . ? C25C O4C B1C 122.3(3) . . ? C15C O5C B2C 106.9(3) . . ? C14C O6C B2C 106.9(3) . . ? C42C O7C B2C 122.2(3) . . ? C44C O8C B2C 123.3(3) . . ? O1D B1D O4D 109.4(3) . . ? O1D B1D O3D 110.6(4) . . ? O4D B1D O3D 110.0(3) . . ? O1D B1D O2D 106.4(3) . . ? O4D B1D O2D 110.2(3) . . ? O3D B1D O2D 110.2(3) . . ? O6D B2D O8D 110.9(3) . . ? O6D B2D O7D 109.2(3) . . ? O8D B2D O7D 111.8(3) . . ? O6D B2D O5D 105.5(3) . . ? O8D B2D O5D 109.3(3) . . ? O7D B2D O5D 110.0(3) . . ? C2D C1D C6D 115.2(3) . . ? C2D C1D C10D 123.5(3) . . ? C6D C1D C10D 121.3(3) . . ? O2D C2D C1D 127.9(3) . . ? O2D C2D C3D 110.2(3) . . ? C1D C2D C3D 121.8(3) . . ? O1D C3D C4D 127.1(3) . . ? O1D C3D C2D 110.7(3) . . ? C4D C3D C2D 122.2(3) . . ? C3D C4D C5D 117.4(3) . . ? C3D C4D H211 121.3 . . ? C5D C4D H211 121.3 . . ? C4D C5D C6D 120.8(3) . . ? C4D C5D H205 119.6 . . ? C6D C5D H205 119.6 . . ? C5D C6D C1D 122.5(4) . . ? C5D C6D H207 118.7 . . ? C1D C6D H207 118.7 . . ? C12D C7D C8D 117.4(3) . . ? C12D C7D C16D 119.9(3) . . ? C8D C7D C16D 122.6(3) . . ? C9D C8D C7D 120.9(3) . . ? C9D C8D H214 119.5 . . ? C7D C8D H214 119.5 . . ? C8D C9D C10D 121.7(3) . . ? C8D C9D H208 119.1 . . ? C10D C9D H208 119.1 . . ? C9D C10D C11D 116.8(3) . . ? C9D C10D C1D 123.0(3) . . ? C11D C10D C1D 120.1(3) . . ? C12D C11D C10D 121.1(3) . . ? C12D C11D H210 119.4 . . ? C10D C11D H210 119.4 . . ? C11D C12D C7D 122.0(3) . . ? C11D C12D H213 119.0 . . ? C7D C12D H213 119.0 . . ? C14D C13D C18D 117.6(3) . . ? C14D C13D H196 121.2 . . ? C18D C13D H196 121.2 . . ? O6D C14D C13D 127.9(3) . . ? O6D C14D C15D 110.6(3) . . ? C13D C14D C15D 121.5(3) . . ? O5D C15D C16D 127.6(3) . . ? O5D C15D C14D 110.0(3) . . ? C16D C15D C14D 122.1(3) . . ? C15D C16D C17D 115.0(3) . . ? C15D C16D C7D 123.1(3) . . ? C17D C16D C7D 121.7(3) . . ? C18D C17D C16D 123.3(3) . . ? C18D C17D H203 118.4 . . ? C16D C17D H203 118.4 . . ? C17D C18D C13D 120.4(3) . . ? C17D C18D H201 119.8 . . ? C13D C18D H201 119.8 . . ? N1D C19D C20D 109.3(4) . . ? N1D C19D H206 125.4 . . ? C20D C19D H206 125.4 . . ? C19D C20D C21D 107.4(4) . . ? C19D C20D C30D 123.8(4) . . ? C21D C20D C30D 128.8(4) . . ? C20D C21D C22D 106.7(3) . . ? C20D C21D C32D 125.3(4) . . ? C22D C21D C32D 128.0(4) . . ? N1D C22D C21D 106.9(3) . . ? N1D C22D C23D 118.7(3) . . ? C21D C22D C23D 134.3(4) . . ? O3D C23D C24D 119.3(4) . . ? O3D C23D C22D 114.2(4) . . ? C24D C23D C22D 126.5(3) . . ? C23D C24D C25D 119.6(3) . . ? C23D C24D H209 120.2 . . ? C25D C24D H209 120.2 . . ? O4D C25D C24D 120.5(4) . . ? O4D C25D C26D 114.5(4) . . ? C24D C25D C26D 124.9(4) . . ? N2D C26D C27D 108.9(4) . . ? N2D C26D C25D 119.1(4) . . ? C27D C26D C25D 132.0(4) . . ? C26D C27D C28D 105.9(4) . . ? C26D C27D C34D 128.9(4) . . ? C28D C27D C34D 125.2(4) . . ? C29D C28D C27D 108.1(4) . . ? C29D C28D C36D 127.1(5) . . ? C27D C28D C36D 124.8(5) . . ? N2D C29D C28D 108.9(4) . . ? N2D C29D H215 125.5 . . ? C28D C29D H215 125.5 . . ? C20D C30D C31D 114.8(4) . . ? C20D C30D H143 108.6 . . ? C31D C30D H143 108.6 . . ? C20D C30D H144 108.6 . . ? C31D C30D H144 108.6 . . ? H143 C30D H144 107.5 . . ? C30D C31D H145 109.5 . . ? C30D C31D H146 109.5 . . ? H145 C31D H146 109.5 . . ? C30D C31D H147 109.5 . . ? H145 C31D H147 109.5 . . ? H146 C31D H147 109.5 . . ? C21D C32D C33D 112.9(3) . . ? C21D C32D H141 109.0 . . ? C33D C32D H141 109.0 . . ? C21D C32D H142 109.0 . . ? C33D C32D H142 109.0 . . ? H141 C32D H142 107.8 . . ? C32D C33D H148 109.5 . . ? C32D C33D H149 109.5 . . ? H148 C33D H149 109.5 . . ? C32D C33D H150 109.5 . . ? H148 C33D H150 109.5 . . ? H149 C33D H150 109.5 . . ? C27D C34D C35D 111.3(4) . . ? C27D C34D H151 109.4 . . ? C35D C34D H151 109.4 . . ? C27D C34D H152 109.4 . . ? C35D C34D H152 109.4 . . ? H151 C34D H152 108.0 . . ? C34D C35D H153 109.5 . . ? C34D C35D H154 109.5 . . ? H153 C35D H154 109.5 . . ? C34D C35D H155 109.5 . . ? H153 C35D H155 109.5 . . ? H154 C35D H155 109.5 . . ? C37D C36D C28D 113.9(5) . . ? C37D C36D H156 108.8 . . ? C28D C36D H156 108.8 . . ? C37D C36D H157 108.8 . . ? C28D C36D H157 108.8 . . ? H156 C36D H157 107.7 . . ? C36D C37D H158 109.5 . . ? C36D C37D H159 109.5 . . ? H158 C37D H159 109.5 . . ? C36D C37D H160 109.5 . . ? H158 C37D H160 109.5 . . ? H159 C37D H160 109.5 . . ? N3D C38D C39D 109.1(4) . . ? N3D C38D H212 125.5 . . ? C39D C38D H212 125.5 . . ? C38D C39D C40D 107.1(3) . . ? C38D C39D C49D 124.8(4) . . ? C40D C39D C49D 128.1(4) . . ? C39D C40D C41D 106.6(3) . . ? C39D C40D C51D 124.5(3) . . ? C41D C40D C51D 128.7(3) . . ? N3D C41D C40D 107.8(3) . . ? N3D C41D C42D 118.7(3) . . ? C40D C41D C42D 133.5(4) . . ? O7D C42D C43D 120.8(3) . . ? O7D C42D C41D 112.8(3) . . ? C43D C42D C41D 126.4(3) . . ? C42D C43D C44D 120.9(3) . . ? C42D C43D H200 119.5 . . ? C44D C43D H200 119.5 . . ? O8D C44D C43D 119.5(3) . . ? O8D C44D C45D 113.8(3) . . ? C43D C44D C45D 126.7(3) . . ? N4D C45D C46D 107.3(3) . . ? N4D C45D C44D 118.9(3) . . ? C46D C45D C44D 133.7(3) . . ? C45D C46D C47D 107.5(3) . . ? C45D C46D C53D 127.5(3) . . ? C47D C46D C53D 125.0(3) . . ? C48D C47D C46D 106.4(3) . . ? C48D C47D C55D 126.4(4) . . ? C46D C47D C55D 127.2(3) . . ? N4D C48D C47D 109.1(3) . . ? N4D C48D H204 125.5 . . ? C47D C48D H204 125.5 . . ? C39D C49D C50D 113.7(3) . . ? C39D C49D H128 108.8 . . ? C50D C49D H128 108.8 . . ? C39D C49D H129 108.8 . . ? C50D C49D H129 108.8 . . ? H128 C49D H129 107.7 . . ? C49D C50D H135 109.5 . . ? C49D C50D H136 109.5 . . ? H135 C50D H136 109.5 . . ? C49D C50D H137 109.5 . . ? H135 C50D H137 109.5 . . ? H136 C50D H137 109.5 . . ? C40D C51D C52D 114.2(3) . . ? C40D C51D H121 108.7 . . ? C52D C51D H121 108.7 . . ? C40D C51D H122 108.7 . . ? C52D C51D H122 108.7 . . ? H121 C51D H122 107.6 . . ? C51D C52D H132 109.5 . . ? C51D C52D H133 109.5 . . ? H132 C52D H133 109.5 . . ? C51D C52D H134 109.5 . . ? H132 C52D H134 109.5 . . ? H133 C52D H134 109.5 . . ? C46D C53D C54D 112.6(3) . . ? C46D C53D H123 109.1 . . ? C54D C53D H123 109.1 . . ? C46D C53D H124 109.1 . . ? C54D C53D H124 109.1 . . ? H123 C53D H124 107.8 . . ? C53D C54D H125 109.5 . . ? C53D C54D H126 109.5 . . ? H125 C54D H126 109.5 . . ? C53D C54D H127 109.5 . . ? H125 C54D H127 109.5 . . ? H126 C54D H127 109.5 . . ? C47D C55D C56D 114.0(4) . . ? C47D C55D H130 108.7 . . ? C56D C55D H130 108.7 . . ? C47D C55D H131 108.7 . . ? C56D C55D H131 108.7 . . ? H130 C55D H131 107.6 . . ? C55D C56D H138 109.5 . . ? C55D C56D H139 109.5 . . ? H138 C56D H139 109.5 . . ? C55D C56D H140 109.5 . . ? H138 C56D H140 109.5 . . ? H139 C56D H140 109.5 . . ? C19D N1D C22D 109.7(3) . . ? C19D N1D H198 125.2 . . ? C22D N1D H198 125.2 . . ? C29D N2D C26D 108.2(4) . . ? C29D N2D H202 125.9 . . ? C26D N2D H202 125.9 . . ? C38D N3D C41D 109.4(3) . . ? C38D N3D H199 125.3 . . ? C41D N3D H199 125.3 . . ? C48D N4D C45D 109.8(3) . . ? C48D N4D H197 125.1 . . ? C45D N4D H197 125.1 . . ? C3D O1D B1D 106.6(3) . . ? C2D O2D B1D 106.0(3) . . ? C23D O3D B1D 120.9(3) . . ? C25D O4D B1D 121.3(3) . . ? C15D O5D B2D 106.7(3) . . ? C14D O6D B2D 107.1(3) . . ? C42D O7D B2D 123.0(3) . . ? C44D O8D B2D 123.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6A C1A C2A O2A -178.6(3) . . . . ? C10A C1A C2A O2A 3.1(6) . . . . ? C6A C1A C2A C3A 0.9(6) . . . . ? C10A C1A C2A C3A -177.5(3) . . . . ? O2A C2A C3A O1A -1.6(4) . . . . ? C1A C2A C3A O1A 178.9(3) . . . . ? O2A C2A C3A C4A 178.5(3) . . . . ? C1A C2A C3A C4A -1.0(6) . . . . ? O1A C3A C4A C5A -179.9(4) . . . . ? C2A C3A C4A C5A -0.1(6) . . . . ? C3A C4A C5A C6A 1.3(6) . . . . ? C4A C5A C6A C1A -1.4(6) . . . . ? C2A C1A C6A C5A 0.3(6) . . . . ? C10A C1A C6A C5A 178.7(4) . . . . ? C12A C7A C8A C9A 1.5(5) . . . . ? C16A C7A C8A C9A -179.0(3) . . . . ? C7A C8A C9A C10A -0.7(6) . . . . ? C8A C9A C10A C11A -0.5(5) . . . . ? C8A C9A C10A C1A 177.7(3) . . . . ? C2A C1A C10A C9A 32.1(6) . . . . ? C6A C1A C10A C9A -146.1(4) . . . . ? C2A C1A C10A C11A -149.7(4) . . . . ? C6A C1A C10A C11A 32.1(5) . . . . ? C9A C10A C11A C12A 0.8(5) . . . . ? C1A C10A C11A C12A -177.5(3) . . . . ? C10A C11A C12A C7A 0.1(5) . . . . ? C8A C7A C12A C11A -1.3(5) . . . . ? C16A C7A C12A C11A 179.3(3) . . . . ? C18A C13A C14A O6A -179.1(3) . . . . ? C18A C13A C14A C15A 2.0(6) . . . . ? O6A C14A C15A O5A -2.1(4) . . . . ? C13A C14A C15A O5A 176.9(3) . . . . ? O6A C14A C15A C16A 175.4(3) . . . . ? C13A C14A C15A C16A -5.5(6) . . . . ? O5A C15A C16A C17A -177.5(3) . . . . ? C14A C15A C16A C17A 5.4(5) . . . . ? O5A C15A C16A C7A 4.8(6) . . . . ? C14A C15A C16A C7A -172.2(3) . . . . ? C12A C7A C16A C15A 145.1(4) . . . . ? C8A C7A C16A C15A -34.3(5) . . . . ? C12A C7A C16A C17A -32.4(5) . . . . ? C8A C7A C16A C17A 148.2(4) . . . . ? C15A C16A C17A C18A -2.2(6) . . . . ? C7A C16A C17A C18A 175.4(3) . . . . ? C16A C17A C18A C13A -1.0(6) . . . . ? C14A C13A C18A C17A 1.1(6) . . . . ? N1A C19A C20A C21A 1.5(4) . . . . ? N1A C19A C20A C30A -179.8(3) . . . . ? C19A C20A C21A C22A -1.6(4) . . . . ? C30A C20A C21A C22A 179.6(3) . . . . ? C19A C20A C21A C32A 179.8(3) . . . . ? C30A C20A C21A C32A 1.0(6) . . . . ? C20A C21A C22A N1A 1.2(4) . . . . ? C32A C21A C22A N1A 179.7(3) . . . . ? C20A C21A C22A C23A -176.5(4) . . . . ? C32A C21A C22A C23A 2.0(7) . . . . ? N1A C22A C23A O3A 5.1(4) . . . . ? C21A C22A C23A O3A -177.4(4) . . . . ? N1A C22A C23A C24A -173.7(3) . . . . ? C21A C22A C23A C24A 3.8(6) . . . . ? O3A C23A C24A C25A -2.9(5) . . . . ? C22A C23A C24A C25A 175.8(3) . . . . ? C23A C24A C25A O4A 2.2(5) . . . . ? C23A C24A C25A C26A -177.8(3) . . . . ? O4A C25A C26A N2A 2.7(5) . . . . ? C24A C25A C26A N2A -177.4(3) . . . . ? O4A C25A C26A C27A -178.6(4) . . . . ? C24A C25A C26A C27A 1.4(6) . . . . ? N2A C26A C27A C28A 3.0(4) . . . . ? C25A C26A C27A C28A -175.8(4) . . . . ? N2A C26A C27A C34A -174.1(4) . . . . ? C25A C26A C27A C34A 7.0(7) . . . . ? C26A C27A C28A C29A -2.0(4) . . . . ? C34A C27A C28A C29A 175.1(4) . . . . ? C26A C27A C28A C36A 175.9(4) . . . . ? C34A C27A C28A C36A -6.9(6) . . . . ? C27A C28A C29A N2A 0.3(4) . . . . ? C36A C28A C29A N2A -177.7(3) . . . . ? C19A C20A C30A C31A -2.3(5) . . . . ? C21A C20A C30A C31A 176.2(3) . . . . ? C20A C21A C32A C33A 90.9(5) . . . . ? C22A C21A C32A C33A -87.4(5) . . . . ? C28A C27A C34A C35A 99.7(5) . . . . ? C26A C27A C34A C35A -83.6(5) . . . . ? C27A C28A C36A C37A -79.9(5) . . . . ? C29A C28A C36A C37A 97.7(5) . . . . ? N3A C38A C39A C40A -0.3(4) . . . . ? N3A C38A C39A C49A 180.0(3) . . . . ? C38A C39A C40A C41A 0.9(4) . . . . ? C49A C39A C40A C41A -179.4(3) . . . . ? C38A C39A C40A C51A 179.0(3) . . . . ? C49A C39A C40A C51A -1.2(6) . . . . ? C39A C40A C41A N3A -1.1(4) . . . . ? C51A C40A C41A N3A -179.2(3) . . . . ? C39A C40A C41A C42A 179.9(4) . . . . ? C51A C40A C41A C42A 1.8(6) . . . . ? N3A C41A C42A O7A 0.3(5) . . . . ? C40A C41A C42A O7A 179.2(4) . . . . ? N3A C41A C42A C43A -179.6(3) . . . . ? C40A C41A C42A C43A -0.6(6) . . . . ? O7A C42A C43A C44A -4.4(5) . . . . ? C41A C42A C43A C44A 175.4(3) . . . . ? C42A C43A C44A O8A -0.5(5) . . . . ? C42A C43A C44A C45A 178.5(3) . . . . ? O8A C44A C45A N4A 6.3(4) . . . . ? C43A C44A C45A N4A -172.8(3) . . . . ? O8A C44A C45A C46A -176.6(3) . . . . ? C43A C44A C45A C46A 4.3(6) . . . . ? N4A C45A C46A C47A 2.0(4) . . . . ? C44A C45A C46A C47A -175.4(3) . . . . ? N4A C45A C46A C53A -177.4(3) . . . . ? C44A C45A C46A C53A 5.3(6) . . . . ? C45A C46A C47A C48A -1.1(4) . . . . ? C53A C46A C47A C48A 178.2(3) . . . . ? C45A C46A C47A C55A 174.5(3) . . . . ? C53A C46A C47A C55A -6.2(5) . . . . ? C46A C47A C48A N4A -0.2(4) . . . . ? C55A C47A C48A N4A -175.8(3) . . . . ? C38A C39A C49A C50A -99.7(5) . . . . ? C40A C39A C49A C50A 80.6(5) . . . . ? C41A C40A C51A C52A 78.7(5) . . . . ? C39A C40A C51A C52A -99.1(4) . . . . ? C47A C46A C53A C54A 82.3(4) . . . . ? C45A C46A C53A C54A -98.5(4) . . . . ? C48A C47A C55A C56A -32.2(5) . . . . ? C46A C47A C55A C56A 153.1(3) . . . . ? C20A C19A N1A C22A -0.7(4) . . . . ? C21A C22A N1A C19A -0.3(4) . . . . ? C23A C22A N1A C19A 177.8(3) . . . . ? C28A C29A N2A C26A 1.7(4) . . . . ? C25A C26A N2A C29A 176.1(3) . . . . ? C27A C26A N2A C29A -2.9(4) . . . . ? C39A C38A N3A C41A -0.4(4) . . . . ? C40A C41A N3A C38A 1.0(4) . . . . ? C42A C41A N3A C38A -179.8(3) . . . . ? C47A C48A N4A C45A 1.5(4) . . . . ? C46A C45A N4A C48A -2.1(4) . . . . ? C44A C45A N4A C48A 175.7(3) . . . . ? C4A C3A O1A B1A -172.4(4) . . . . ? C2A C3A O1A B1A 7.7(4) . . . . ? O2A B1A O1A C3A -10.5(4) . . . . ? O4A B1A O1A C3A -129.7(3) . . . . ? O3A B1A O1A C3A 108.0(3) . . . . ? C1A C2A O2A B1A 174.3(4) . . . . ? C3A C2A O2A B1A -5.3(4) . . . . ? O1A B1A O2A C2A 9.7(4) . . . . ? O4A B1A O2A C2A 129.6(3) . . . . ? O3A B1A O2A C2A -107.2(3) . . . . ? C24A C23A O3A B1A -10.2(5) . . . . ? C22A C23A O3A B1A 170.9(3) . . . . ? O1A B1A O3A C23A 143.8(3) . . . . ? O2A B1A O3A C23A -100.6(4) . . . . ? O4A B1A O3A C23A 21.7(4) . . . . ? C24A C25A O4A B1A 11.6(5) . . . . ? C26A C25A O4A B1A -168.4(3) . . . . ? O1A B1A O4A C25A -142.6(3) . . . . ? O2A B1A O4A C25A 100.6(3) . . . . ? O3A B1A O4A C25A -22.2(4) . . . . ? C16A C15A O5A B2A -174.1(4) . . . . ? C14A C15A O5A B2A 3.2(4) . . . . ? O7A B2A O5A C15A 116.6(3) . . . . ? O6A B2A O5A C15A -3.2(4) . . . . ? O8A B2A O5A C15A -121.1(3) . . . . ? C13A C14A O6A B2A -179.0(4) . . . . ? C15A C14A O6A B2A 0.0(4) . . . . ? O7A B2A O6A C14A -115.8(3) . . . . ? O8A B2A O6A C14A 120.4(3) . . . . ? O5A B2A O6A C14A 1.9(4) . . . . ? C43A C42A O7A B2A 5.5(5) . . . . ? C41A C42A O7A B2A -174.4(3) . . . . ? O6A B2A O7A C42A -124.0(4) . . . . ? O8A B2A O7A C42A -1.7(5) . . . . ? O5A B2A O7A C42A 119.6(3) . . . . ? C43A C44A O8A B2A 4.4(5) . . . . ? C45A C44A O8A B2A -174.8(3) . . . . ? O7A B2A O8A C44A -3.3(5) . . . . ? O6A B2A O8A C44A 120.3(3) . . . . ? O5A B2A O8A C44A -123.6(3) . . . . ? C6B C1B C2B O2B 179.3(4) . . . . ? C10B C1B C2B O2B -1.3(6) . . . . ? C6B C1B C2B C3B -2.5(5) . . . . ? C10B C1B C2B C3B 176.9(4) . . . . ? O2B C2B C3B O1B 1.1(4) . . . . ? C1B C2B C3B O1B -177.4(3) . . . . ? O2B C2B C3B C4B -179.4(4) . . . . ? C1B C2B C3B C4B 2.1(6) . . . . ? O1B C3B C4B C5B 179.2(4) . . . . ? C2B C3B C4B C5B -0.2(6) . . . . ? C3B C4B C5B C6B -1.1(6) . . . . ? C4B C5B C6B C1B 0.5(6) . . . . ? C2B C1B C6B C5B 1.2(6) . . . . ? C10B C1B C6B C5B -178.2(4) . . . . ? C12B C7B C8B C9B -2.1(5) . . . . ? C16B C7B C8B C9B 176.6(4) . . . . ? C7B C8B C9B C10B 0.2(6) . . . . ? C8B C9B C10B C11B 0.9(5) . . . . ? C8B C9B C10B C1B -175.3(4) . . . . ? C2B C1B C10B C11B 155.1(4) . . . . ? C6B C1B C10B C11B -25.5(6) . . . . ? C2B C1B C10B C9B -28.8(5) . . . . ? C6B C1B C10B C9B 150.5(4) . . . . ? C9B C10B C11B C12B -0.1(5) . . . . ? C1B C10B C11B C12B 176.0(4) . . . . ? C10B C11B C12B C7B -1.9(6) . . . . ? C8B C7B C12B C11B 2.9(5) . . . . ? C16B C7B C12B C11B -175.8(4) . . . . ? C18B C13B C14B O6B 177.4(4) . . . . ? C18B C13B C14B C15B -3.4(6) . . . . ? O6B C14B C15B O5B 0.1(4) . . . . ? C13B C14B C15B O5B -179.2(3) . . . . ? O6B C14B C15B C16B -176.1(3) . . . . ? C13B C14B C15B C16B 4.6(6) . . . . ? O5B C15B C16B C17B -178.9(3) . . . . ? C14B C15B C16B C17B -3.4(5) . . . . ? O5B C15B C16B C7B 0.4(6) . . . . ? C14B C15B C16B C7B 175.9(3) . . . . ? C8B C7B C16B C15B 29.6(6) . . . . ? C12B C7B C16B C15B -151.9(4) . . . . ? C8B C7B C16B C17B -151.2(3) . . . . ? C12B C7B C16B C17B 27.4(5) . . . . ? C15B C16B C17B C18B 1.5(6) . . . . ? C7B C16B C17B C18B -177.9(4) . . . . ? C16B C17B C18B C13B -0.6(6) . . . . ? C14B C13B C18B C17B 1.5(6) . . . . ? N1B C19B C20B C21B 0.4(4) . . . . ? N1B C19B C20B C30B -177.2(3) . . . . ? C19B C20B C21B C22B -0.5(4) . . . . ? C30B C20B C21B C22B 177.0(3) . . . . ? C19B C20B C21B C32B 180.0(3) . . . . ? C30B C20B C21B C32B -2.6(6) . . . . ? C20B C21B C22B N1B 0.4(4) . . . . ? C32B C21B C22B N1B 180.0(3) . . . . ? C20B C21B C22B C23B -177.1(4) . . . . ? C32B C21B C22B C23B 2.5(6) . . . . ? N1B C22B C23B O3B -8.1(4) . . . . ? C21B C22B C23B O3B 169.2(4) . . . . ? N1B C22B C23B C24B 172.0(3) . . . . ? C21B C22B C23B C24B -10.7(6) . . . . ? O3B C23B C24B C25B -8.2(5) . . . . ? C22B C23B C24B C25B 171.8(3) . . . . ? C23B C24B C25B O4B 7.3(5) . . . . ? C23B C24B C25B C26B -174.8(3) . . . . ? O4B C25B C26B N2B 5.8(5) . . . . ? C24B C25B C26B N2B -172.1(3) . . . . ? O4B C25B C26B C27B -171.2(4) . . . . ? C24B C25B C26B C27B 10.8(7) . . . . ? N2B C26B C27B C28B -0.2(4) . . . . ? C25B C26B C27B C28B 177.2(4) . . . . ? N2B C26B C27B C34B 179.3(4) . . . . ? C25B C26B C27B C34B -3.4(7) . . . . ? C26B C27B C28B C29B 0.1(4) . . . . ? C34B C27B C28B C29B -179.4(4) . . . . ? C26B C27B C28B C36B 179.8(4) . . . . ? C34B C27B C28B C36B 0.3(7) . . . . ? C27B C28B C29B N2B 0.0(5) . . . . ? C36B C28B C29B N2B -179.7(4) . . . . ? C19B C20B C30B C31B -93.7(5) . . . . ? C21B C20B C30B C31B 89.3(5) . . . . ? C22B C21B C32B C33B 87.4(4) . . . . ? C20B C21B C32B C33B -93.1(4) . . . . ? C28B C27B C34B C35B 95.5(5) . . . . ? C26B C27B C34B C35B -83.8(5) . . . . ? C27B C28B C36B C37B 161.3(4) . . . . ? C29B C28B C36B C37B -19.1(6) . . . . ? N3B C38B C39B C40B -1.0(4) . . . . ? N3B C38B C39B C49B 178.0(3) . . . . ? C38B C39B C40B C41B 1.8(4) . . . . ? C49B C39B C40B C41B -177.2(3) . . . . ? C38B C39B C40B C51B 177.9(3) . . . . ? C49B C39B C40B C51B -1.1(6) . . . . ? C39B C40B C41B N3B -1.9(4) . . . . ? C51B C40B C41B N3B -177.8(3) . . . . ? C39B C40B C41B C42B 175.7(4) . . . . ? C51B C40B C41B C42B -0.1(6) . . . . ? N3B C41B C42B O7B -0.6(5) . . . . ? C40B C41B C42B O7B -178.0(4) . . . . ? N3B C41B C42B C43B 179.3(3) . . . . ? C40B C41B C42B C43B 1.9(6) . . . . ? O7B C42B C43B C44B -1.6(5) . . . . ? C41B C42B C43B C44B 178.5(3) . . . . ? C42B C43B C44B O8B 5.4(5) . . . . ? C42B C43B C44B C45B -172.2(3) . . . . ? O8B C44B C45B N4B 1.8(4) . . . . ? C43B C44B C45B N4B 179.6(3) . . . . ? O8B C44B C45B C46B -172.6(4) . . . . ? C43B C44B C45B C46B 5.2(6) . . . . ? N4B C45B C46B C47B 0.6(4) . . . . ? C44B C45B C46B C47B 175.5(4) . . . . ? N4B C45B C46B C53B 178.3(3) . . . . ? C44B C45B C46B C53B -6.8(6) . . . . ? C45B C46B C47B C48B -0.1(4) . . . . ? C53B C46B C47B C48B -177.9(3) . . . . ? C45B C46B C47B C55B -178.3(4) . . . . ? C53B C46B C47B C55B 3.9(6) . . . . ? C46B C47B C48B N4B -0.5(4) . . . . ? C55B C47B C48B N4B 177.7(4) . . . . ? C38B C39B C49B C50B -6.6(6) . . . . ? C40B C39B C49B C50B 172.2(4) . . . . ? C39B C40B C51B C52B -90.2(4) . . . . ? C41B C40B C51B C52B 85.0(4) . . . . ? C47B C46B C53B C54B 97.9(4) . . . . ? C45B C46B C53B C54B -79.5(5) . . . . ? C48B C47B C55B C56B 115.8(4) . . . . ? C46B C47B C55B C56B -66.3(5) . . . . ? C20B C19B N1B C22B -0.1(4) . . . . ? C21B C22B N1B C19B -0.2(4) . . . . ? C23B C22B N1B C19B 177.8(3) . . . . ? C28B C29B N2B C26B -0.1(5) . . . . ? C25B C26B N2B C29B -177.6(3) . . . . ? C27B C26B N2B C29B 0.2(4) . . . . ? C39B C38B N3B C41B -0.2(4) . . . . ? C40B C41B N3B C38B 1.3(4) . . . . ? C42B C41B N3B C38B -176.8(3) . . . . ? C47B C48B N4B C45B 0.9(4) . . . . ? C46B C45B N4B C48B -0.9(4) . . . . ? C44B C45B N4B C48B -176.7(3) . . . . ? C4B C3B O1B B1B 179.7(4) . . . . ? C2B C3B O1B B1B -0.8(4) . . . . ? O4B B1B O1B C3B -119.5(3) . . . . ? O2B B1B O1B C3B 0.3(4) . . . . ? O3B B1B O1B C3B 118.1(3) . . . . ? C1B C2B O2B B1B 177.5(4) . . . . ? C3B C2B O2B B1B -0.8(4) . . . . ? O4B B1B O2B C2B 119.9(3) . . . . ? O1B B1B O2B C2B 0.3(4) . . . . ? O3B B1B O2B C2B -116.6(3) . . . . ? C24B C23B O3B B1B -7.9(5) . . . . ? C22B C23B O3B B1B 172.1(3) . . . . ? O4B B1B O3B C23B 22.8(4) . . . . ? O2B B1B O3B C23B -100.3(4) . . . . ? O1B B1B O3B C23B 144.6(3) . . . . ? C26B C25B O4B B1B -168.0(3) . . . . ? C24B C25B O4B B1B 10.1(5) . . . . ? O2B B1B O4B C25B 98.6(4) . . . . ? O1B B1B O4B C25B -144.7(3) . . . . ? O3B B1B O4B C25B -24.0(5) . . . . ? C16B C15B O5B B2B 178.6(4) . . . . ? C14B C15B O5B B2B 2.6(4) . . . . ? O8B B2B O5B C15B -123.6(3) . . . . ? O7B B2B O5B C15B 112.9(3) . . . . ? O6B B2B O5B C15B -4.2(4) . . . . ? C13B C14B O6B B2B 176.5(4) . . . . ? C15B C14B O6B B2B -2.8(4) . . . . ? O8B B2B O6B C14B 122.7(3) . . . . ? O7B B2B O6B C14B -113.3(3) . . . . ? O5B B2B O6B C14B 4.2(4) . . . . ? C43B C42B O7B B2B -5.8(5) . . . . ? C41B C42B O7B B2B 174.1(3) . . . . ? O8B B2B O7B C42B 8.7(5) . . . . ? O5B B2B O7B C42B 130.7(3) . . . . ? O6B B2B O7B C42B -114.7(4) . . . . ? C43B C44B O8B B2B -1.8(5) . . . . ? C45B C44B O8B B2B 176.1(3) . . . . ? O7B B2B O8B C44B -4.8(5) . . . . ? O5B B2B O8B C44B -126.9(3) . . . . ? O6B B2B O8B C44B 117.4(3) . . . . ? C6C C1C C2C O2C -178.4(3) . . . . ? C10C C1C C2C O2C 1.9(6) . . . . ? C6C C1C C2C C3C 0.4(5) . . . . ? C10C C1C C2C C3C -179.3(3) . . . . ? O2C C2C C3C O1C -0.4(4) . . . . ? C1C C2C C3C O1C -179.4(3) . . . . ? O2C C2C C3C C4C 177.4(3) . . . . ? C1C C2C C3C C4C -1.6(6) . . . . ? O1C C3C C4C C5C 179.8(4) . . . . ? C2C C3C C4C C5C 2.4(6) . . . . ? C3C C4C C5C C6C -2.1(6) . . . . ? C4C C5C C6C C1C 0.9(6) . . . . ? C2C C1C C6C C5C 0.0(5) . . . . ? C10C C1C C6C C5C 179.7(3) . . . . ? C12C C7C C8C C9C 0.8(5) . . . . ? C16C C7C C8C C9C -179.2(3) . . . . ? C7C C8C C9C C10C -1.1(5) . . . . ? C8C C9C C10C C11C 0.5(5) . . . . ? C8C C9C C10C C1C -178.8(3) . . . . ? C2C C1C C10C C9C 27.4(5) . . . . ? C6C C1C C10C C9C -152.2(3) . . . . ? C2C C1C C10C C11C -151.7(3) . . . . ? C6C C1C C10C C11C 28.6(5) . . . . ? C9C C10C C11C C12C 0.5(5) . . . . ? C1C C10C C11C C12C 179.7(3) . . . . ? C10C C11C C12C C7C -0.9(5) . . . . ? C8C C7C C12C C11C 0.2(5) . . . . ? C16C C7C C12C C11C -179.8(3) . . . . ? C18C C13C C14C O6C -172.8(3) . . . . ? C18C C13C C14C C15C 2.5(6) . . . . ? O6C C14C C15C O5C -2.0(4) . . . . ? C13C C14C C15C O5C -177.9(3) . . . . ? O6C C14C C15C C16C 173.4(3) . . . . ? C13C C14C C15C C16C -2.5(6) . . . . ? O5C C15C C16C C17C 175.0(3) . . . . ? C14C C15C C16C C17C 0.4(5) . . . . ? O5C C15C C16C C7C -3.4(6) . . . . ? C14C C15C C16C C7C -178.0(3) . . . . ? C12C C7C C16C C15C 140.2(4) . . . . ? C8C C7C C16C C15C -39.8(5) . . . . ? C12C C7C C16C C17C -38.0(5) . . . . ? C8C C7C C16C C17C 142.0(4) . . . . ? C15C C16C C17C C18C 1.6(5) . . . . ? C7C C16C C17C C18C 180.0(3) . . . . ? C16C C17C C18C C13C -1.6(6) . . . . ? C14C C13C C18C C17C -0.5(6) . . . . ? N1C C19C C20C C21C 0.9(4) . . . . ? N1C C19C C20C C30C -178.1(3) . . . . ? C19C C20C C21C C22C -1.9(4) . . . . ? C30C C20C C21C C22C 177.1(4) . . . . ? C19C C20C C21C C32C -178.1(3) . . . . ? C30C C20C C21C C32C 0.8(6) . . . . ? C20C C21C C22C N1C 2.2(4) . . . . ? C32C C21C C22C N1C 178.3(3) . . . . ? C20C C21C C22C C23C -175.7(4) . . . . ? C32C C21C C22C C23C 0.4(7) . . . . ? N1C C22C C23C O3C -5.4(4) . . . . ? C21C C22C C23C O3C 172.3(4) . . . . ? N1C C22C C23C C24C 176.4(3) . . . . ? C21C C22C C23C C24C -5.8(6) . . . . ? O3C C23C C24C C25C -3.3(5) . . . . ? C22C C23C C24C C25C 174.7(3) . . . . ? C23C C24C C25C O4C 1.7(5) . . . . ? C23C C24C C25C C26C -176.2(3) . . . . ? O4C C25C C26C N2C -3.9(4) . . . . ? C24C C25C C26C N2C 174.1(3) . . . . ? O4C C25C C26C C27C 176.9(4) . . . . ? C24C C25C C26C C27C -5.1(6) . . . . ? N2C C26C C27C C28C -2.5(4) . . . . ? C25C C26C C27C C28C 176.7(4) . . . . ? N2C C26C C27C C34C -178.2(4) . . . . ? C25C C26C C27C C34C 1.0(7) . . . . ? C26C C27C C28C C29C 2.4(5) . . . . ? C34C C27C C28C C29C 178.3(4) . . . . ? C26C C27C C28C C36C -172.7(4) . . . . ? C34C C27C C28C C36C 3.1(7) . . . . ? C27C C28C C29C N2C -1.4(5) . . . . ? C36C C28C C29C N2C 173.5(4) . . . . ? C19C C20C C30C C31C 92.8(5) . . . . ? C21C C20C C30C C31C -86.0(6) . . . . ? C22C C21C C32C C33C -81.6(5) . . . . ? C20C C21C C32C C33C 93.8(5) . . . . ? C26C C27C C34C C35C 86.3(6) . . . . ? C28C C27C C34C C35C -88.7(5) . . . . ? C29C C28C C36C C37C 19.4(7) . . . . ? C27C C28C C36C C37C -166.6(4) . . . . ? N3C C38C C39C C40C 0.9(4) . . . . ? N3C C38C C39C C49C -179.0(4) . . . . ? C38C C39C C40C C41C -0.4(4) . . . . ? C49C C39C C40C C41C 179.5(4) . . . . ? C38C C39C C40C C51C -179.2(3) . . . . ? C49C C39C C40C C51C 0.6(6) . . . . ? C39C C40C C41C N3C -0.3(4) . . . . ? C51C C40C C41C N3C 178.6(3) . . . . ? C39C C40C C41C C42C -171.9(4) . . . . ? C51C C40C C41C C42C 6.9(6) . . . . ? N3C C41C C42C O7C -10.8(5) . . . . ? C40C C41C C42C O7C 160.0(4) . . . . ? N3C C41C C42C C43C 169.4(3) . . . . ? C40C C41C C42C C43C -19.8(6) . . . . ? O7C C42C C43C C44C -5.5(5) . . . . ? C41C C42C C43C C44C 174.3(3) . . . . ? C42C C43C C44C O8C -0.1(5) . . . . ? C42C C43C C44C C45C 179.1(3) . . . . ? O8C C44C C45C N4C 3.4(5) . . . . ? C43C C44C C45C N4C -175.8(3) . . . . ? O8C C44C C45C C46C -173.6(4) . . . . ? C43C C44C C45C C46C 7.2(6) . . . . ? N4C C45C C46C C47C -0.4(4) . . . . ? C44C C45C C46C C47C 176.8(4) . . . . ? N4C C45C C46C C53C 174.5(4) . . . . ? C44C C45C C46C C53C -8.2(7) . . . . ? C45C C46C C47C C48C 0.0(5) . . . . ? C53C C46C C47C C48C -175.1(4) . . . . ? C45C C46C C47C C55C -178.3(5) . . . . ? C53C C46C C47C C55C 6.6(8) . . . . ? C46C C47C C48C N4C 0.4(5) . . . . ? C55C C47C C48C N4C 178.7(5) . . . . ? C40C C39C C49C C50C 95.0(6) . . . . ? C38C C39C C49C C50C -85.1(6) . . . . ? C39C C40C C51C C52C -92.3(5) . . . . ? C41C C40C C51C C52C 89.1(5) . . . . ? C47C C46C C53C C54C 95.6(5) . . . . ? C45C C46C C53C C54C -78.5(5) . . . . ? C48C C47C C55C C56C -32.5(13) . . . . ? C46C C47C C55C C56C 145.5(10) . . . . ? C20C C19C N1C C22C 0.5(4) . . . . ? C21C C22C N1C C19C -1.7(4) . . . . ? C23C C22C N1C C19C 176.6(3) . . . . ? C28C C29C N2C C26C -0.2(4) . . . . ? C27C C26C N2C C29C 1.7(4) . . . . ? C25C C26C N2C C29C -177.7(3) . . . . ? C39C C38C N3C C41C -1.1(4) . . . . ? C40C C41C N3C C38C 0.9(4) . . . . ? C42C C41C N3C C38C 173.9(3) . . . . ? C47C C48C N4C C45C -0.7(5) . . . . ? C46C C45C N4C C48C 0.7(4) . . . . ? C44C C45C N4C C48C -177.0(3) . . . . ? C4C C3C O1C B1C -171.0(4) . . . . ? C2C C3C O1C B1C 6.6(4) . . . . ? O3C B1C O1C C3C 108.8(3) . . . . ? O4C B1C O1C C3C -129.0(3) . . . . ? O2C B1C O1C C3C -9.8(4) . . . . ? C1C C2C O2C B1C 173.1(4) . . . . ? C3C C2C O2C B1C -5.8(4) . . . . ? O1C B1C O2C C2C 9.6(4) . . . . ? O3C B1C O2C C2C -108.5(3) . . . . ? O4C B1C O2C C2C 130.4(3) . . . . ? C24C C23C O3C B1C -9.4(5) . . . . ? C22C C23C O3C B1C 172.3(3) . . . . ? O1C B1C O3C C23C 144.2(3) . . . . ? O4C B1C O3C C23C 20.9(4) . . . . ? O2C B1C O3C C23C -99.9(4) . . . . ? C24C C25C O4C B1C 12.4(5) . . . . ? C26C C25C O4C B1C -169.4(3) . . . . ? O1C B1C O4C C25C -144.1(3) . . . . ? O3C B1C O4C C25C -22.3(4) . . . . ? O2C B1C O4C C25C 98.9(3) . . . . ? C16C C15C O5C B2C -171.6(4) . . . . ? C14C C15C O5C B2C 3.5(4) . . . . ? O8C B2C O5C C15C -123.0(3) . . . . ? O6C B2C O5C C15C -3.6(4) . . . . ? O7C B2C O5C C15C 113.4(3) . . . . ? C13C C14C O6C B2C 175.3(4) . . . . ? C15C C14C O6C B2C -0.4(4) . . . . ? O8C B2C O6C C14C 121.9(3) . . . . ? O5C B2C O6C C14C 2.4(4) . . . . ? O7C B2C O6C C14C -113.6(3) . . . . ? C43C C42C O7C B2C 3.3(5) . . . . ? C41C C42C O7C B2C -176.5(3) . . . . ? O8C B2C O7C C42C 3.6(4) . . . . ? O5C B2C O7C C42C 126.1(3) . . . . ? O6C B2C O7C C42C -119.8(3) . . . . ? C43C C44C O8C B2C 7.9(5) . . . . ? C45C C44C O8C B2C -171.3(3) . . . . ? O5C B2C O8C C44C -130.4(3) . . . . ? O6C B2C O8C C44C 113.5(3) . . . . ? O7C B2C O8C C44C -9.4(4) . . . . ? C6D C1D C2D O2D 179.4(4) . . . . ? C10D C1D C2D O2D -0.7(6) . . . . ? C6D C1D C2D C3D 2.0(5) . . . . ? C10D C1D C2D C3D -178.1(3) . . . . ? O2D C2D C3D O1D 2.0(4) . . . . ? C1D C2D C3D O1D 179.8(3) . . . . ? O2D C2D C3D C4D -178.4(4) . . . . ? C1D C2D C3D C4D -0.6(6) . . . . ? O1D C3D C4D C5D 178.0(4) . . . . ? C2D C3D C4D C5D -1.5(6) . . . . ? C3D C4D C5D C6D 2.1(6) . . . . ? C4D C5D C6D C1D -0.6(6) . . . . ? C2D C1D C6D C5D -1.4(6) . . . . ? C10D C1D C6D C5D 178.7(4) . . . . ? C12D C7D C8D C9D -1.6(6) . . . . ? C16D C7D C8D C9D 179.5(4) . . . . ? C7D C8D C9D C10D 0.3(6) . . . . ? C8D C9D C10D C11D 1.3(6) . . . . ? C8D C9D C10D C1D -175.0(4) . . . . ? C2D C1D C10D C9D -29.0(6) . . . . ? C6D C1D C10D C9D 150.9(4) . . . . ? C2D C1D C10D C11D 154.9(4) . . . . ? C6D C1D C10D C11D -25.2(6) . . . . ? C9D C10D C11D C12D -1.6(6) . . . . ? C1D C10D C11D C12D 174.8(4) . . . . ? C10D C11D C12D C7D 0.3(6) . . . . ? C8D C7D C12D C11D 1.3(6) . . . . ? C16D C7D C12D C11D -179.7(4) . . . . ? C18D C13D C14D O6D 177.2(4) . . . . ? C18D C13D C14D C15D -0.4(6) . . . . ? O6D C14D C15D O5D 0.1(4) . . . . ? C13D C14D C15D O5D 178.1(3) . . . . ? O6D C14D C15D C16D -174.8(3) . . . . ? C13D C14D C15D C16D 3.2(6) . . . . ? O5D C15D C16D C17D -177.7(3) . . . . ? C14D C15D C16D C17D -3.8(5) . . . . ? O5D C15D C16D C7D -2.7(6) . . . . ? C14D C15D C16D C7D 171.2(3) . . . . ? C12D C7D C16D C15D -146.1(4) . . . . ? C8D C7D C16D C15D 32.7(6) . . . . ? C12D C7D C16D C17D 28.5(5) . . . . ? C8D C7D C16D C17D -152.6(4) . . . . ? C15D C16D C17D C18D 1.8(6) . . . . ? C7D C16D C17D C18D -173.2(4) . . . . ? C16D C17D C18D C13D 0.8(6) . . . . ? C14D C13D C18D C17D -1.5(6) . . . . ? N1D C19D C20D C21D -0.4(4) . . . . ? N1D C19D C20D C30D 177.8(3) . . . . ? C19D C20D C21D C22D 0.7(4) . . . . ? C30D C20D C21D C22D -177.4(4) . . . . ? C19D C20D C21D C32D -178.3(3) . . . . ? C30D C20D C21D C32D 3.6(6) . . . . ? C20D C21D C22D N1D -0.8(4) . . . . ? C32D C21D C22D N1D 178.2(3) . . . . ? C20D C21D C22D C23D 175.6(4) . . . . ? C32D C21D C22D C23D -5.4(6) . . . . ? N1D C22D C23D O3D 2.1(4) . . . . ? C21D C22D C23D O3D -173.9(4) . . . . ? N1D C22D C23D C24D -176.1(3) . . . . ? C21D C22D C23D C24D 7.9(6) . . . . ? O3D C23D C24D C25D -0.4(5) . . . . ? C22D C23D C24D C25D 177.7(3) . . . . ? C23D C24D C25D O4D 6.8(5) . . . . ? C23D C24D C25D C26D -172.0(3) . . . . ? O4D C25D C26D N2D 11.1(5) . . . . ? C24D C25D C26D N2D -170.1(3) . . . . ? O4D C25D C26D C27D -165.0(4) . . . . ? C24D C25D C26D C27D 13.8(7) . . . . ? N2D C26D C27D C28D 1.8(4) . . . . ? C25D C26D C27D C28D 178.2(4) . . . . ? N2D C26D C27D C34D -179.1(4) . . . . ? C25D C26D C27D C34D -2.7(7) . . . . ? C26D C27D C28D C29D -1.1(5) . . . . ? C34D C27D C28D C29D 179.7(4) . . . . ? C26D C27D C28D C36D 178.8(4) . . . . ? C34D C27D C28D C36D -0.4(7) . . . . ? C27D C28D C29D N2D 0.0(5) . . . . ? C36D C28D C29D N2D -179.9(4) . . . . ? C19D C20D C30D C31D 116.7(4) . . . . ? C21D C20D C30D C31D -65.4(5) . . . . ? C20D C21D C32D C33D 99.0(4) . . . . ? C22D C21D C32D C33D -79.7(5) . . . . ? C26D C27D C34D C35D -85.9(5) . . . . ? C28D C27D C34D C35D 93.1(5) . . . . ? C29D C28D C36D C37D -6.1(8) . . . . ? C27D C28D C36D C37D 174.0(5) . . . . ? N3D C38D C39D C40D -0.3(4) . . . . ? N3D C38D C39D C49D -179.3(3) . . . . ? C38D C39D C40D C41D 0.1(4) . . . . ? C49D C39D C40D C41D 179.2(3) . . . . ? C38D C39D C40D C51D 175.7(3) . . . . ? C49D C39D C40D C51D -5.2(5) . . . . ? C39D C40D C41D N3D 0.1(4) . . . . ? C51D C40D C41D N3D -175.3(3) . . . . ? C39D C40D C41D C42D 177.9(4) . . . . ? C51D C40D C41D C42D 2.5(6) . . . . ? N3D C41D C42D O7D 6.9(4) . . . . ? C40D C41D C42D O7D -170.7(3) . . . . ? N3D C41D C42D C43D -173.6(3) . . . . ? C40D C41D C42D C43D 8.8(6) . . . . ? O7D C42D C43D C44D 4.4(5) . . . . ? C41D C42D C43D C44D -175.1(3) . . . . ? C42D C43D C44D O8D 0.8(5) . . . . ? C42D C43D C44D C45D 179.2(3) . . . . ? O8D C44D C45D N4D 0.1(4) . . . . ? C43D C44D C45D N4D -178.4(3) . . . . ? O8D C44D C45D C46D -175.4(3) . . . . ? C43D C44D C45D C46D 6.1(6) . . . . ? N4D C45D C46D C47D 0.7(4) . . . . ? C44D C45D C46D C47D 176.6(3) . . . . ? N4D C45D C46D C53D -178.7(3) . . . . ? C44D C45D C46D C53D -2.8(6) . . . . ? C45D C46D C47D C48D -0.2(4) . . . . ? C53D C46D C47D C48D 179.2(3) . . . . ? C45D C46D C47D C55D -178.2(4) . . . . ? C53D C46D C47D C55D 1.2(6) . . . . ? C46D C47D C48D N4D -0.4(4) . . . . ? C55D C47D C48D N4D 177.6(4) . . . . ? C38D C39D C49D C50D 101.3(5) . . . . ? C40D C39D C49D C50D -77.6(5) . . . . ? C39D C40D C51D C52D 99.9(4) . . . . ? C41D C40D C51D C52D -85.5(4) . . . . ? C45D C46D C53D C54D -78.6(4) . . . . ? C47D C46D C53D C54D 102.1(4) . . . . ? C48D C47D C55D C56D -7.6(6) . . . . ? C46D C47D C55D C56D 170.0(4) . . . . ? C20D C19D N1D C22D 0.0(4) . . . . ? C21D C22D N1D C19D 0.5(4) . . . . ? C23D C22D N1D C19D -176.5(3) . . . . ? C28D C29D N2D C26D 1.1(5) . . . . ? C27D C26D N2D C29D -1.8(4) . . . . ? C25D C26D N2D C29D -178.8(3) . . . . ? C39D C38D N3D C41D 0.3(4) . . . . ? C40D C41D N3D C38D -0.2(4) . . . . ? C42D C41D N3D C38D -178.4(3) . . . . ? C47D C48D N4D C45D 0.9(4) . . . . ? C46D C45D N4D C48D -1.0(4) . . . . ? C44D C45D N4D C48D -177.6(3) . . . . ? C4D C3D O1D B1D -178.6(4) . . . . ? C2D C3D O1D B1D 1.0(4) . . . . ? O4D B1D O1D C3D -122.3(3) . . . . ? O3D B1D O1D C3D 116.4(3) . . . . ? O2D B1D O1D C3D -3.3(4) . . . . ? C1D C2D O2D B1D 178.4(4) . . . . ? C3D C2D O2D B1D -4.0(4) . . . . ? O1D B1D O2D C2D 4.5(4) . . . . ? O4D B1D O2D C2D 122.9(3) . . . . ? O3D B1D O2D C2D -115.5(3) . . . . ? C24D C23D O3D B1D -21.5(5) . . . . ? C22D C23D O3D B1D 160.2(3) . . . . ? O1D B1D O3D C23D 155.1(3) . . . . ? O4D B1D O3D C23D 34.1(5) . . . . ? O2D B1D O3D C23D -87.5(4) . . . . ? C24D C25D O4D B1D 9.1(5) . . . . ? C26D C25D O4D B1D -172.0(3) . . . . ? O1D B1D O4D C25D -149.3(3) . . . . ? O3D B1D O4D C25D -27.6(5) . . . . ? O2D B1D O4D C25D 94.1(4) . . . . ? C16D C15D O5D B2D 175.5(4) . . . . ? C14D C15D O5D B2D 0.9(4) . . . . ? O6D B2D O5D C15D -1.5(4) . . . . ? O8D B2D O5D C15D -120.8(3) . . . . ? O7D B2D O5D C15D 116.1(3) . . . . ? C13D C14D O6D B2D -178.9(4) . . . . ? C15D C14D O6D B2D -1.1(4) . . . . ? O8D B2D O6D C14D 119.8(3) . . . . ? O7D B2D O6D C14D -116.6(3) . . . . ? O5D B2D O6D C14D 1.6(4) . . . . ? C43D C42D O7D B2D -3.3(5) . . . . ? C41D C42D O7D B2D 176.1(3) . . . . ? O6D B2D O7D C42D -125.3(3) . . . . ? O8D B2D O7D C42D -2.2(5) . . . . ? O5D B2D O7D C42D 119.3(3) . . . . ? C43D C44D O8D B2D -7.0(5) . . . . ? C45D C44D O8D B2D 174.4(3) . . . . ? O6D B2D O8D C44D 129.6(3) . . . . ? O7D B2D O8D C44D 7.5(5) . . . . ? O5D B2D O8D C44D -114.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.816 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.816 _refine_diff_density_max 1.256 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.086 #============================================================================== # End of CIF #============================================================================== data_61207maeda _database_code_depnum_ccdc_archive 'CCDC 686903' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H30 B N2 O4' _chemical_formula_weight 469.35 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' B B 0.0013 0.0007 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.944(4) _cell_length_b 23.283(5) _cell_length_c 24.446(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.271(4) _cell_angle_gamma 90.00 _cell_volume 10152(3) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 2988 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 24.53 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 0.041 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9959 _exptl_absorpt_correction_T_max 0.9959 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51663 _diffrn_reflns_av_R_equivalents 0.1157 _diffrn_reflns_av_sigmaI/netI 0.2518 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17843 _reflns_number_gt 5149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1187P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17843 _refine_ls_number_parameters 641 _refine_ls_number_restraints 480 _refine_ls_R_factor_all 0.2036 _refine_ls_R_factor_gt 0.1091 _refine_ls_wR_factor_ref 0.2888 _refine_ls_wR_factor_gt 0.2642 _refine_ls_goodness_of_fit_ref 0.817 _refine_ls_restrained_S_all 0.837 _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 B1 B 0.1124(3) 0.2237(2) 0.7246(2) 0.0376(8) Uani 1 1 d U . . B2 B 0.6114(4) 0.1903(2) 0.7352(3) 0.0446(9) Uani 1 1 d U . . C1 C 0.1727(3) 0.29298(18) 0.77320(19) 0.0348(8) Uani 1 1 d U . . C2 C 0.0948(3) 0.30223(19) 0.7737(2) 0.0401(9) Uani 1 1 d U . . C3 C 0.0657(3) 0.34722(19) 0.7991(2) 0.0467(10) Uani 1 1 d U . . H3 H 0.0131 0.3521 0.7988 0.056 Uiso 1 1 calc R . . C4 C 0.1164(3) 0.38614(19) 0.8257(2) 0.0447(10) Uani 1 1 d U . . H4 H 0.0983 0.4185 0.8439 0.054 Uiso 1 1 calc R . . C5 C 0.1935(3) 0.37809(19) 0.8257(2) 0.0423(10) Uani 1 1 d U . . H5 H 0.2263 0.4053 0.8445 0.051 Uiso 1 1 calc R . . C6 C 0.2245(3) 0.33270(17) 0.79985(19) 0.0334(8) Uani 1 1 d U . . C7 C 0.3074(3) 0.32548(17) 0.8004(2) 0.0319(8) Uani 1 1 d U . . C8 C 0.3536(3) 0.34100(18) 0.8474(2) 0.0368(9) Uani 1 1 d U . . H8 H 0.3312 0.3550 0.8783 0.044 Uiso 1 1 calc R . . C9 C 0.4325(3) 0.33679(17) 0.8511(2) 0.0369(9) Uani 1 1 d U . . H9 H 0.4630 0.3452 0.8844 0.044 Uiso 1 1 calc R . . C10 C 0.4640(3) 0.31976(18) 0.8036(2) 0.0367(9) Uani 1 1 d U . . C11 C 0.4184(3) 0.30478(18) 0.7567(2) 0.0356(9) Uani 1 1 d U . . H11 H 0.4400 0.2913 0.7253 0.043 Uiso 1 1 calc R . . C12 C 0.3395(3) 0.30943(17) 0.75527(19) 0.0328(9) Uani 1 1 d U . . H12 H 0.3086 0.3012 0.7221 0.039 Uiso 1 1 calc R . . C13 C 0.5469(3) 0.31448(19) 0.8072(2) 0.0397(9) Uani 1 1 d U . . C14 C 0.5959(3) 0.3566(2) 0.8338(2) 0.0469(10) Uani 1 1 d U . . H14 H 0.5743 0.3889 0.8498 0.056 Uiso 1 1 calc R . . C15 C 0.6725(3) 0.3528(2) 0.8375(2) 0.0482(11) Uani 1 1 d U . . H15 H 0.7030 0.3817 0.8560 0.058 Uiso 1 1 calc R . . C16 C 0.7055(3) 0.3054(2) 0.8135(2) 0.0467(10) Uani 1 1 d U . . H16 H 0.7585 0.3015 0.8163 0.056 Uiso 1 1 calc R . . C17 C 0.6614(3) 0.2663(2) 0.7869(2) 0.0436(9) Uani 1 1 d U . . C18 C 0.5847(3) 0.2696(2) 0.7831(2) 0.0420(9) Uani 1 1 d U . . C19 C 0.1078(3) -0.03175(18) 0.73954(19) 0.0321(9) Uani 1 1 d U . . H19 H 0.1128 -0.0709 0.7296 0.038 Uiso 1 1 calc R . . C20 C 0.0846(3) -0.01436(19) 0.7881(2) 0.0363(9) Uani 1 1 d U . . C21 C 0.0899(3) 0.04690(18) 0.7889(2) 0.0351(9) Uani 1 1 d U . . C22 C 0.1135(3) 0.06209(18) 0.73640(19) 0.0306(8) Uani 1 1 d U . . C23 C 0.1172(3) 0.11722(18) 0.71138(19) 0.0303(8) Uani 1 1 d U . . C24 C 0.1265(3) 0.12444(18) 0.65594(19) 0.0323(9) Uani 1 1 d U . . H24 H 0.1387 0.0927 0.6341 0.039 Uiso 1 1 calc R . . C25 C 0.1173(3) 0.18104(19) 0.6326(2) 0.0382(9) Uani 1 1 d U . . C26 C 0.1221(3) 0.1935(2) 0.5761(2) 0.0431(9) Uani 1 1 d U . . C27 C 0.1225(3) 0.2459(2) 0.5484(2) 0.0520(10) Uani 1 1 d U . . C28 C 0.1387(3) 0.2348(2) 0.4970(2) 0.0609(10) Uani 1 1 d U . . C29 C 0.1478(3) 0.1759(2) 0.4938(2) 0.0589(11) Uani 1 1 d U . . H29 H 0.1610 0.1560 0.4623 0.071 Uiso 1 1 calc R . . C30 C 0.0607(3) -0.0514(2) 0.8338(2) 0.0439(11) Uani 1 1 d U . . H30A H 0.0429 -0.0889 0.8183 0.053 Uiso 1 1 calc R . . H30B H 0.0181 -0.0327 0.8493 0.053 Uiso 1 1 calc R . . C31 C 0.1233(3) -0.0617(2) 0.8798(2) 0.0641(15) Uani 1 1 d U . . H31A H 0.1423 -0.0247 0.8945 0.096 Uiso 1 1 calc R . . H31B H 0.1640 -0.0830 0.8654 0.096 Uiso 1 1 calc R . . H31C H 0.1039 -0.0840 0.9092 0.096 Uiso 1 1 calc R . . C32 C 0.0773(3) 0.0849(2) 0.8345(2) 0.0424(11) Uani 1 1 d U . . H32A H 0.0473 0.0645 0.8601 0.051 Uiso 1 1 calc R . . H32B H 0.0483 0.1189 0.8200 0.051 Uiso 1 1 calc R . . C33 C 0.1506(3) 0.1046(2) 0.8655(2) 0.0619(15) Uani 1 1 d U . . H33A H 0.1772 0.0714 0.8828 0.093 Uiso 1 1 calc R . . H33B H 0.1403 0.1323 0.8940 0.093 Uiso 1 1 calc R . . H33C H 0.1816 0.1229 0.8399 0.093 Uiso 1 1 calc R . . C34 C 0.1133(3) 0.3049(2) 0.5720(2) 0.0576(12) Uani 1 1 d U . . H34A H 0.1414 0.3067 0.6091 0.069 Uiso 1 1 calc R . . H34B H 0.1355 0.3335 0.5486 0.069 Uiso 1 1 calc R . . C35 C 0.0357(3) 0.3205(2) 0.5762(3) 0.0641(15) Uani 1 1 d U . . H35A H 0.0335 0.3599 0.5902 0.096 Uiso 1 1 calc R . . H35B H 0.0142 0.2941 0.6015 0.096 Uiso 1 1 calc R . . H35C H 0.0070 0.3181 0.5398 0.096 Uiso 1 1 calc R . . C36 C 0.1499(4) 0.2747(3) 0.4478(3) 0.0722(13) Uani 1 1 d U . . H36A H 0.1820 0.3076 0.4610 0.087 Uiso 1 1 calc R . . H36B H 0.1760 0.2533 0.4205 0.087 Uiso 1 1 calc R . . C37 C 0.0794(4) 0.2959(3) 0.4217(3) 0.0841(19) Uani 1 1 d U . . H37A H 0.0428 0.2646 0.4182 0.126 Uiso 1 1 calc R . . H37B H 0.0863 0.3107 0.3850 0.126 Uiso 1 1 calc R . . H37C H 0.0613 0.3268 0.4440 0.126 Uiso 1 1 calc R . . C38 C 0.6092(3) -0.0652(2) 0.7306(2) 0.0484(10) Uani 1 1 d U . . H38 H 0.6082 -0.1029 0.7155 0.058 Uiso 1 1 calc R . . C39 C 0.5958(3) -0.0501(2) 0.7842(2) 0.0554(10) Uani 1 1 d U . . C40 C 0.5980(3) 0.0111(2) 0.7880(2) 0.0465(9) Uani 1 1 d U . . C41 C 0.6153(3) 0.0305(2) 0.7377(2) 0.0366(9) Uani 1 1 d U . . C42 C 0.6206(3) 0.08871(19) 0.7156(2) 0.0354(9) Uani 1 1 d U . . C43 C 0.6370(3) 0.10084(19) 0.6635(2) 0.0348(9) Uani 1 1 d U . . H43 H 0.6558 0.0717 0.6415 0.042 Uiso 1 1 calc R . . C44 C 0.6259(3) 0.1561(2) 0.6431(2) 0.0389(9) Uani 1 1 d U . . C45 C 0.6337(3) 0.1729(2) 0.5903(2) 0.0446(9) Uani 1 1 d U . . C46 C 0.6290(3) 0.2260(2) 0.5618(2) 0.0541(10) Uani 1 1 d U . . C47 C 0.6410(3) 0.2168(2) 0.5095(2) 0.0540(10) Uani 1 1 d U . . C48 C 0.6479(3) 0.1589(2) 0.4999(2) 0.0503(11) Uani 1 1 d U . . H48 H 0.6524 0.1413 0.4653 0.060 Uiso 1 1 calc R . . C49 C 0.5770(4) -0.0910(3) 0.8293(3) 0.0718(13) Uani 1 1 d U . . H49A H 0.5515 -0.0688 0.8563 0.086 Uiso 1 1 calc R . . H49B H 0.5408 -0.1198 0.8126 0.086 Uiso 1 1 calc R . . C50 C 0.6410(4) -0.1221(4) 0.8594(3) 0.112(2) Uani 1 1 d U . . H50A H 0.6220 -0.1515 0.8830 0.167 Uiso 1 1 calc R . . H50B H 0.6725 -0.0949 0.8821 0.167 Uiso 1 1 calc R . . H50C H 0.6707 -0.1405 0.8330 0.167 Uiso 1 1 calc R . . C51 C 0.5920(3) 0.0453(2) 0.8402(2) 0.0532(12) Uani 1 1 d U . . H51A H 0.5637 0.0810 0.8307 0.064 Uiso 1 1 calc R . . H51B H 0.5634 0.0226 0.8650 0.064 Uiso 1 1 calc R . . C52 C 0.6646(3) 0.0599(3) 0.8689(2) 0.0672(16) Uani 1 1 d U . . H52A H 0.6986 0.0270 0.8681 0.101 Uiso 1 1 calc R . . H52B H 0.6588 0.0697 0.9072 0.101 Uiso 1 1 calc R . . H52C H 0.6855 0.0929 0.8509 0.101 Uiso 1 1 calc R . . C53 C 0.6199(3) 0.2866(2) 0.5883(3) 0.0623(13) Uani 1 1 d U . . H53A H 0.6490 0.2880 0.6251 0.075 Uiso 1 1 calc R . . H53B H 0.6397 0.3165 0.5650 0.075 Uiso 1 1 calc R . . C54 C 0.5404(4) 0.2977(3) 0.5934(3) 0.0809(18) Uani 1 1 d U . . H54A H 0.5122 0.2983 0.5567 0.121 Uiso 1 1 calc R . . H54B H 0.5353 0.3349 0.6114 0.121 Uiso 1 1 calc R . . H54C H 0.5206 0.2673 0.6155 0.121 Uiso 1 1 calc R . . C55 C 0.6420(4) 0.2627(2) 0.4636(2) 0.0655(13) Uani 1 1 d U . . H55A H 0.5905 0.2777 0.4546 0.079 Uiso 1 1 calc R . . H55B H 0.6740 0.2951 0.4780 0.079 Uiso 1 1 calc R . . C56 C 0.6683(4) 0.2425(3) 0.4149(3) 0.0803(18) Uani 1 1 d U . . H56A H 0.7114 0.2171 0.4242 0.120 Uiso 1 1 calc R . . H56B H 0.6836 0.2752 0.3934 0.120 Uiso 1 1 calc R . . H56C H 0.6283 0.2212 0.3931 0.120 Uiso 1 1 calc R . . N1 N 0.1227(2) 0.01231(14) 0.70751(15) 0.0317(8) Uani 1 1 d U . . H1 H 0.1360 0.0100 0.6740 0.038 Uiso 1 1 calc R . . N2 N 0.1353(3) 0.15095(17) 0.54090(18) 0.0535(10) Uani 1 1 d U . . H2 H 0.1355 0.1139 0.5478 0.064 Uiso 1 1 calc R . . N3 N 0.6237(2) -0.01633(16) 0.70460(17) 0.0403(9) Uani 1 1 d U . . H3A H 0.6368 -0.0145 0.6710 0.048 Uiso 1 1 calc R . . N4 N 0.6470(2) 0.13170(17) 0.54868(16) 0.0449(9) Uani 1 1 d U . . H4A H 0.6535 0.0946 0.5541 0.054 Uiso 1 1 calc R . . O1 O 0.05648(18) 0.25699(12) 0.74579(13) 0.0419(8) Uani 1 1 d U . . O2 O 0.18718(17) 0.24473(11) 0.74490(12) 0.0334(7) Uani 1 1 d U . . O3 O 0.10509(18) 0.16188(12) 0.74281(12) 0.0377(7) Uani 1 1 d U . . O4 O 0.10331(18) 0.22442(12) 0.66359(13) 0.0382(7) Uani 1 1 d U . . O5 O 0.55029(18) 0.22338(13) 0.75556(13) 0.0440(8) Uani 1 1 d U . . O6 O 0.68173(19) 0.21656(13) 0.76272(14) 0.0474(8) Uani 1 1 d U . . O7 O 0.60408(18) 0.12956(13) 0.75069(13) 0.0419(8) Uani 1 1 d U . . O8 O 0.60729(19) 0.19754(13) 0.67393(13) 0.0441(8) Uani 1 1 d U . . 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 B1 0.0423(16) 0.0243(15) 0.0449(16) -0.0043(15) -0.0006(15) 0.0026(15) B2 0.0465(16) 0.0382(15) 0.0493(17) -0.0087(15) 0.0065(16) 0.0039(15) C1 0.0400(17) 0.0222(15) 0.0422(18) -0.0002(15) 0.0033(16) 0.0041(15) C2 0.0439(18) 0.0261(16) 0.0500(19) -0.0011(16) 0.0039(17) 0.0021(16) C3 0.045(2) 0.0303(18) 0.063(2) -0.0020(18) 0.001(2) 0.0047(18) C4 0.046(2) 0.0260(18) 0.061(2) -0.0054(18) 0.003(2) 0.0018(18) C5 0.046(2) 0.0260(18) 0.054(2) -0.0054(18) 0.0021(19) 0.0024(18) C6 0.0406(17) 0.0199(15) 0.0396(18) -0.0008(15) 0.0047(16) 0.0038(15) C7 0.0404(18) 0.0162(15) 0.0396(18) 0.0000(15) 0.0071(16) -0.0015(15) C8 0.042(2) 0.0246(17) 0.045(2) -0.0006(17) 0.0082(19) -0.0035(17) C9 0.043(2) 0.0232(17) 0.045(2) -0.0011(17) 0.0050(19) -0.0027(17) C10 0.0412(18) 0.0245(16) 0.0444(18) -0.0009(16) 0.0038(16) -0.0031(16) C11 0.045(2) 0.0205(17) 0.041(2) -0.0006(17) 0.0028(18) -0.0015(18) C12 0.043(2) 0.0173(16) 0.038(2) -0.0015(16) 0.0034(18) -0.0019(17) C13 0.0421(18) 0.0304(16) 0.0463(18) -0.0031(16) 0.0030(17) -0.0024(16) C14 0.048(2) 0.044(2) 0.049(2) -0.0048(18) 0.005(2) -0.0006(19) C15 0.046(2) 0.049(2) 0.051(2) -0.0048(19) 0.009(2) -0.003(2) C16 0.042(2) 0.047(2) 0.051(2) -0.0052(19) 0.0079(19) 0.0019(19) C17 0.0408(18) 0.0397(17) 0.0507(19) -0.0083(16) 0.0065(17) 0.0009(16) C18 0.0423(18) 0.0345(16) 0.0488(18) -0.0089(16) 0.0024(17) -0.0001(16) C19 0.0354(19) 0.0223(17) 0.038(2) -0.0024(17) 0.0038(18) 0.0014(17) C20 0.0372(18) 0.0294(16) 0.0416(19) 0.0008(16) 0.0014(17) 0.0010(16) C21 0.0345(18) 0.0296(16) 0.0403(18) -0.0038(16) -0.0004(16) 0.0005(16) C22 0.0294(17) 0.0256(15) 0.0362(17) -0.0024(15) 0.0008(15) 0.0000(15) C23 0.0306(17) 0.0231(15) 0.0367(17) -0.0040(15) 0.0017(16) -0.0020(15) C24 0.0337(19) 0.0241(17) 0.039(2) 0.0021(17) 0.0023(18) -0.0050(16) C25 0.0396(17) 0.0297(16) 0.0447(18) -0.0003(16) 0.0018(16) -0.0023(16) C26 0.0515(19) 0.0329(17) 0.0456(19) 0.0015(16) 0.0078(17) -0.0014(17) C27 0.062(2) 0.0396(17) 0.055(2) 0.0004(18) 0.0097(19) -0.0018(18) C28 0.077(2) 0.0456(19) 0.060(2) 0.0029(19) 0.008(2) -0.0043(19) C29 0.078(2) 0.043(2) 0.056(2) 0.005(2) 0.008(2) -0.003(2) C30 0.046(2) 0.036(2) 0.049(2) 0.000(2) 0.004(2) 0.002(2) C31 0.062(4) 0.060(3) 0.072(4) 0.010(3) 0.018(3) 0.007(3) C32 0.047(2) 0.036(2) 0.043(2) -0.0034(19) 0.001(2) 0.002(2) C33 0.082(4) 0.047(3) 0.054(3) -0.010(3) -0.004(3) 0.001(3) C34 0.063(3) 0.047(2) 0.064(3) 0.001(2) 0.010(2) -0.002(2) C35 0.061(3) 0.052(3) 0.081(4) 0.003(3) 0.014(3) 0.004(3) C36 0.085(3) 0.057(3) 0.074(3) 0.003(2) 0.008(3) -0.005(2) C37 0.088(4) 0.076(4) 0.088(4) -0.002(3) 0.008(4) -0.012(4) C38 0.043(2) 0.050(2) 0.052(2) 0.0066(19) 0.002(2) -0.0007(19) C39 0.048(2) 0.062(2) 0.057(2) 0.0082(19) 0.0037(19) -0.0011(19) C40 0.0386(19) 0.0535(19) 0.048(2) 0.0031(18) 0.0054(18) 0.0034(18) C41 0.0290(17) 0.0390(17) 0.0412(18) 0.0048(16) 0.0013(16) 0.0033(16) C42 0.0289(17) 0.0353(16) 0.0415(18) -0.0031(16) 0.0011(16) 0.0052(15) C43 0.0323(19) 0.0305(17) 0.042(2) -0.0061(17) 0.0043(18) 0.0021(17) C44 0.0414(18) 0.0315(16) 0.0447(18) -0.0053(16) 0.0088(17) 0.0034(16) C45 0.0470(18) 0.0354(17) 0.0525(19) -0.0036(16) 0.0104(17) 0.0049(16) C46 0.055(2) 0.0464(18) 0.062(2) 0.0025(18) 0.0131(19) 0.0013(18) C47 0.058(2) 0.0457(18) 0.060(2) 0.0057(18) 0.0153(19) 0.0019(18) C48 0.054(2) 0.043(2) 0.056(2) 0.0062(19) 0.014(2) 0.0048(19) C49 0.062(3) 0.079(3) 0.073(3) 0.014(2) 0.003(2) -0.002(2) C50 0.096(5) 0.122(5) 0.116(5) 0.018(4) 0.011(4) -0.001(4) C51 0.051(2) 0.058(2) 0.050(3) 0.002(2) 0.001(2) 0.003(2) C52 0.072(4) 0.069(3) 0.060(4) -0.007(3) 0.004(3) 0.011(3) C53 0.066(3) 0.050(2) 0.072(3) 0.004(2) 0.013(2) 0.005(2) C54 0.093(4) 0.062(3) 0.088(4) 0.002(3) 0.009(4) 0.012(3) C55 0.073(3) 0.058(2) 0.068(3) 0.010(2) 0.017(2) 0.004(2) C56 0.096(4) 0.070(4) 0.076(4) 0.002(3) 0.010(4) 0.007(3) N1 0.0336(17) 0.0215(15) 0.0390(18) -0.0009(15) -0.0009(15) 0.0011(15) N2 0.069(2) 0.0382(18) 0.054(2) 0.0069(17) 0.0068(19) -0.0039(18) N3 0.0347(18) 0.0408(18) 0.044(2) 0.0068(16) -0.0003(16) -0.0021(16) N4 0.050(2) 0.0361(17) 0.051(2) 0.0013(16) 0.0157(18) 0.0031(17) O1 0.0431(17) 0.0294(14) 0.0525(17) -0.0046(14) 0.0018(15) 0.0024(13) O2 0.0352(15) 0.0202(13) 0.0437(16) -0.0079(13) -0.0007(13) 0.0025(12) O3 0.0424(16) 0.0280(14) 0.0414(16) -0.0042(13) -0.0011(14) -0.0028(13) O4 0.0434(16) 0.0253(14) 0.0441(17) -0.0013(13) -0.0031(14) 0.0007(13) O5 0.0445(17) 0.0351(15) 0.0518(17) -0.0087(14) 0.0031(15) -0.0027(14) O6 0.0455(17) 0.0441(16) 0.0534(17) -0.0110(14) 0.0087(15) 0.0059(14) O7 0.0409(16) 0.0399(15) 0.0453(17) -0.0050(14) 0.0066(14) 0.0067(14) O8 0.0538(17) 0.0305(14) 0.0488(17) -0.0068(14) 0.0090(15) 0.0037(14) _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 B1 O1 1.410(6) . ? B1 O2 1.462(6) . ? B1 O4 1.483(6) . ? B1 O3 1.517(6) . ? B2 O5 1.471(6) . ? B2 O7 1.473(6) . ? B2 O6 1.495(7) . ? B2 O8 1.501(7) . ? C1 O2 1.359(5) . ? C1 C2 1.415(6) . ? C1 C6 1.419(6) . ? C2 C3 1.351(6) . ? C2 O1 1.395(5) . ? C3 C4 1.394(7) . ? C3 H3 0.9500 . ? C4 C5 1.396(7) . ? C4 H4 0.9500 . ? C5 C6 1.380(6) . ? C5 H5 0.9500 . ? C6 C7 1.496(6) . ? C7 C12 1.351(6) . ? C7 C8 1.389(6) . ? C8 C9 1.412(6) . ? C8 H8 0.9500 . ? C9 C10 1.403(6) . ? C9 H9 0.9500 . ? C10 C11 1.379(6) . ? C10 C13 1.487(7) . ? C11 C12 1.418(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.410(6) . ? C13 C14 1.424(6) . ? C14 C15 1.372(7) . ? C14 H14 0.9500 . ? C15 C16 1.410(7) . ? C15 H15 0.9500 . ? C16 C17 1.328(6) . ? C16 H16 0.9500 . ? C17 O6 1.368(5) . ? C17 C18 1.371(7) . ? C18 O5 1.379(5) . ? C19 N1 1.336(5) . ? C19 C20 1.362(6) . ? C19 H19 0.9500 . ? C20 C21 1.430(6) . ? C20 C30 1.510(6) . ? C21 C22 1.439(6) . ? C21 C32 1.460(6) . ? C22 N1 1.377(5) . ? C22 C23 1.427(6) . ? C23 O3 1.325(5) . ? C23 C24 1.394(6) . ? C24 C25 1.438(6) . ? C24 H24 0.9500 . ? C25 O4 1.303(5) . ? C25 C26 1.422(6) . ? C26 N2 1.350(6) . ? C26 C27 1.396(7) . ? C27 C28 1.344(7) . ? C27 C34 1.507(7) . ? C28 C29 1.384(7) . ? C28 C36 1.552(8) . ? C29 N2 1.330(6) . ? C29 H29 0.9500 . ? C30 C31 1.519(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.516(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.453(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.440(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 N3 1.343(6) . ? C38 C39 1.403(7) . ? C38 H38 0.9500 . ? C39 C40 1.430(7) . ? C39 C49 1.521(8) . ? C40 C41 1.377(6) . ? C40 C51 1.516(7) . ? C41 N3 1.375(6) . ? C41 C42 1.466(6) . ? C42 O7 1.336(5) . ? C42 C43 1.368(6) . ? C43 C44 1.387(6) . ? C43 H43 0.9500 . ? C44 O8 1.291(5) . ? C44 C45 1.369(6) . ? C45 C46 1.417(7) . ? C45 N4 1.439(6) . ? C46 C47 1.336(7) . ? C46 C53 1.567(7) . ? C47 C48 1.377(7) . ? C47 C55 1.550(7) . ? C48 N4 1.352(6) . ? C48 H48 0.9500 . ? C49 C50 1.483(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.451(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.468(8) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.410(7) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? N1 H1 0.8800 . ? N2 H2 0.8800 . ? N3 H3A 0.8800 . ? N4 H4A 0.8800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 B1 O2 110.8(4) . . ? O1 B1 O4 111.0(4) . . ? O2 B1 O4 109.5(4) . . ? O1 B1 O3 109.0(4) . . ? O2 B1 O3 108.9(4) . . ? O4 B1 O3 107.5(4) . . ? O5 B2 O7 109.0(4) . . ? O5 B2 O6 104.9(4) . . ? O7 B2 O6 111.8(5) . . ? O5 B2 O8 108.8(4) . . ? O7 B2 O8 111.6(4) . . ? O6 B2 O8 110.5(4) . . ? O2 C1 C2 112.0(4) . . ? O2 C1 C6 128.3(4) . . ? C2 C1 C6 119.7(4) . . ? C3 C2 O1 127.9(5) . . ? C3 C2 C1 123.6(5) . . ? O1 C2 C1 108.4(4) . . ? C2 C3 C4 116.9(5) . . ? C2 C3 H3 121.6 . . ? C4 C3 H3 121.6 . . ? C3 C4 C5 120.6(5) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 123.5(5) . . ? C6 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C5 C6 C1 115.6(4) . . ? C5 C6 C7 122.2(4) . . ? C1 C6 C7 122.2(4) . . ? C12 C7 C8 118.7(5) . . ? C12 C7 C6 122.3(5) . . ? C8 C7 C6 118.7(4) . . ? C7 C8 C9 122.5(5) . . ? C7 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? C10 C9 C8 117.4(5) . . ? C10 C9 H9 121.3 . . ? C8 C9 H9 121.3 . . ? C11 C10 C9 120.2(5) . . ? C11 C10 C13 121.8(4) . . ? C9 C10 C13 117.8(5) . . ? C10 C11 C12 120.1(5) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 120.9(5) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C18 C13 C14 113.6(5) . . ? C18 C13 C10 124.1(4) . . ? C14 C13 C10 122.2(4) . . ? C15 C14 C13 123.3(5) . . ? C15 C14 H14 118.3 . . ? C13 C14 H14 118.3 . . ? C14 C15 C16 119.1(5) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C17 C16 C15 119.1(5) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 O6 128.3(5) . . ? C16 C17 C18 122.3(5) . . ? O6 C17 C18 109.3(4) . . ? C17 C18 O5 112.5(4) . . ? C17 C18 C13 122.6(5) . . ? O5 C18 C13 124.9(4) . . ? N1 C19 C20 112.5(4) . . ? N1 C19 H19 123.7 . . ? C20 C19 H19 123.7 . . ? C19 C20 C21 106.4(4) . . ? C19 C20 C30 127.9(4) . . ? C21 C20 C30 125.7(4) . . ? C20 C21 C22 105.0(4) . . ? C20 C21 C32 126.9(4) . . ? C22 C21 C32 128.1(4) . . ? N1 C22 C23 121.6(4) . . ? N1 C22 C21 108.3(4) . . ? C23 C22 C21 129.5(4) . . ? O3 C23 C24 120.9(4) . . ? O3 C23 C22 116.0(4) . . ? C24 C23 C22 122.8(4) . . ? C23 C24 C25 118.4(4) . . ? C23 C24 H24 120.8 . . ? C25 C24 H24 120.8 . . ? O4 C25 C26 116.2(4) . . ? O4 C25 C24 120.0(4) . . ? C26 C25 C24 123.7(4) . . ? N2 C26 C27 108.7(5) . . ? N2 C26 C25 120.2(4) . . ? C27 C26 C25 130.8(5) . . ? C28 C27 C26 107.4(5) . . ? C28 C27 C34 125.3(5) . . ? C26 C27 C34 127.1(5) . . ? C27 C28 C29 106.5(5) . . ? C27 C28 C36 131.9(5) . . ? C29 C28 C36 121.6(5) . . ? N2 C29 C28 110.5(5) . . ? N2 C29 H29 124.7 . . ? C28 C29 H29 124.7 . . ? C20 C30 C31 113.0(4) . . ? C20 C30 H30A 109.0 . . ? C31 C30 H30A 109.0 . . ? C20 C30 H30B 109.0 . . ? C31 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C21 C32 C33 111.5(4) . . ? C21 C32 H32A 109.3 . . ? C33 C32 H32A 109.3 . . ? C21 C32 H32B 109.3 . . ? C33 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C27 113.7(5) . . ? C35 C34 H34A 108.8 . . ? C27 C34 H34A 108.8 . . ? C35 C34 H34B 108.8 . . ? C27 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C28 111.5(6) . . ? C37 C36 H36A 109.3 . . ? C28 C36 H36A 109.3 . . ? C37 C36 H36B 109.3 . . ? C28 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N3 C38 C39 107.0(5) . . ? N3 C38 H38 126.5 . . ? C39 C38 H38 126.5 . . ? C38 C39 C40 107.7(5) . . ? C38 C39 C49 126.5(5) . . ? C40 C39 C49 125.8(5) . . ? C41 C40 C39 106.1(5) . . ? C41 C40 C51 128.6(5) . . ? C39 C40 C51 125.0(5) . . ? N3 C41 C40 108.4(4) . . ? N3 C41 C42 120.1(4) . . ? C40 C41 C42 131.4(5) . . ? O7 C42 C43 122.4(4) . . ? O7 C42 C41 113.2(4) . . ? C43 C42 C41 124.2(4) . . ? C42 C43 C44 119.3(4) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? O8 C44 C45 113.3(4) . . ? O8 C44 C43 121.3(5) . . ? C45 C44 C43 125.4(5) . . ? C44 C45 C46 135.0(5) . . ? C44 C45 N4 121.2(4) . . ? C46 C45 N4 103.8(4) . . ? C47 C46 C45 108.9(5) . . ? C47 C46 C53 125.0(5) . . ? C45 C46 C53 125.8(5) . . ? C46 C47 C48 110.3(5) . . ? C46 C47 C55 126.7(5) . . ? C48 C47 C55 122.8(5) . . ? N4 C48 C47 107.3(5) . . ? N4 C48 H48 126.3 . . ? C47 C48 H48 126.3 . . ? C50 C49 C39 116.4(6) . . ? C50 C49 H49A 108.2 . . ? C39 C49 H49A 108.2 . . ? C50 C49 H49B 108.2 . . ? C39 C49 H49B 108.2 . . ? H49A C49 H49B 107.3 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C40 112.9(5) . . ? C52 C51 H51A 109.0 . . ? C40 C51 H51A 109.0 . . ? C52 C51 H51B 109.0 . . ? C40 C51 H51B 109.0 . . ? H51A C51 H51B 107.8 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C46 109.9(5) . . ? C54 C53 H53A 109.7 . . ? C46 C53 H53A 109.7 . . ? C54 C53 H53B 109.7 . . ? C46 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 C47 114.4(5) . . ? C56 C55 H55A 108.7 . . ? C47 C55 H55A 108.7 . . ? C56 C55 H55B 108.7 . . ? C47 C55 H55B 108.7 . . ? H55A C55 H55B 107.6 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C19 N1 C22 107.6(4) . . ? C19 N1 H1 126.2 . . ? C22 N1 H1 126.2 . . ? C29 N2 C26 106.9(4) . . ? C29 N2 H2 126.6 . . ? C26 N2 H2 126.6 . . ? C38 N3 C41 110.7(4) . . ? C38 N3 H3A 124.6 . . ? C41 N3 H3A 124.6 . . ? C48 N4 C45 109.3(4) . . ? C48 N4 H4A 125.3 . . ? C45 N4 H4A 125.3 . . ? C2 O1 B1 105.1(4) . . ? C1 O2 B1 103.2(4) . . ? C23 O3 B1 123.4(4) . . ? C25 O4 B1 124.7(4) . . ? C18 O5 B2 105.3(4) . . ? C17 O6 B2 106.8(4) . . ? C42 O7 B2 119.1(4) . . ? C44 O8 B2 120.8(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.421 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.088 #============================================================================== # End of CIF #==============================================================================