# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Matthias Wagner' _publ_contact_author_email MATTHIAS.WAGNER@CHEMIE.UNI-FRANKFURT.DE _publ_section_title ; Lewis-Base Adducts of 9,10-Dihydro-9,10-diboraanthracene: Ditopic Hydroboration Reagents and a B-N Analogue of Triptycene ; _publ_author_name 'Matthias Wagner' # Attachment 'Combined.cif' data_wa953 _database_code_depnum_ccdc_archive 'CCDC 762845' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H22 B2 S2' _chemical_formula_sum 'C16 H22 B2 S2' _chemical_formula_weight 300.08 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' 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 14.0791(11) _cell_length_b 7.3214(5) _cell_length_c 16.6356(14) _cell_angle_alpha 90.00 _cell_angle_beta 102.414(6) _cell_angle_gamma 90.00 _cell_volume 1674.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14503 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 26.0 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.305 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8853 _exptl_absorpt_correction_T_max 0.9644 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 18440 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 25.65 _reflns_number_total 3128 _reflns_number_gt 2561 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0592P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3128 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.78270(3) 0.67270(6) 0.46995(3) 0.02682(14) Uani 1 1 d . . . S2 S 0.54689(3) 0.38110(7) 0.38559(3) 0.02974(14) Uani 1 1 d . . . B1 B 0.82708(14) 0.4155(3) 0.50539(12) 0.0243(4) Uani 1 1 d . . . H1 H 0.9082(18) 0.435(3) 0.5439(14) 0.046(6) Uiso 1 1 d . . . B2 B 0.64372(16) 0.1884(3) 0.43922(14) 0.0278(4) Uani 1 1 d . . . H2 H 0.5976(17) 0.051(3) 0.4230(13) 0.043(6) Uiso 1 1 d . . . C1 C 0.81565(13) 0.3019(2) 0.42101(11) 0.0242(4) Uani 1 1 d . . . C2 C 0.73052(13) 0.1981(2) 0.39059(11) 0.0258(4) Uani 1 1 d . . . C3 C 0.72450(14) 0.0980(3) 0.31743(12) 0.0322(4) Uani 1 1 d . . . H3 H 0.6683 0.0258 0.2975 0.039 Uiso 1 1 calc R . . C4 C 0.79795(15) 0.1012(3) 0.27338(12) 0.0346(5) Uani 1 1 d . . . H4 H 0.7911 0.0346 0.2235 0.042 Uiso 1 1 calc R . . C5 C 0.88130(15) 0.2027(3) 0.30318(12) 0.0331(4) Uani 1 1 d . . . H5 H 0.9322 0.2058 0.2739 0.040 Uiso 1 1 calc R . . C6 C 0.88972(14) 0.2998(3) 0.37631(11) 0.0288(4) Uani 1 1 d . . . H6 H 0.9476 0.3670 0.3967 0.035 Uiso 1 1 calc R . . C7 C 0.87679(15) 0.7547(3) 0.42118(12) 0.0346(5) Uani 1 1 d . . . H7A H 0.8711 0.6941 0.3678 0.052 Uiso 1 1 calc R . . H7B H 0.9406 0.7276 0.4562 0.052 Uiso 1 1 calc R . . H7C H 0.8700 0.8869 0.4129 0.052 Uiso 1 1 calc R . . C8 C 0.81245(16) 0.8057(3) 0.56305(13) 0.0364(5) Uani 1 1 d . . . H8A H 0.7666 0.7770 0.5980 0.055 Uiso 1 1 calc R . . H8B H 0.8082 0.9360 0.5492 0.055 Uiso 1 1 calc R . . H8C H 0.8787 0.7766 0.5926 0.055 Uiso 1 1 calc R . . C11 C 0.75872(13) 0.3475(2) 0.56508(11) 0.0251(4) Uani 1 1 d . . . C12 C 0.67275(13) 0.2463(2) 0.53465(11) 0.0265(4) Uani 1 1 d . . . C13 C 0.61661(16) 0.1905(3) 0.59060(13) 0.0349(5) Uani 1 1 d . . . H13 H 0.5592 0.1213 0.5709 0.042 Uiso 1 1 calc R . . C14 C 0.64248(18) 0.2334(3) 0.67412(13) 0.0427(5) Uani 1 1 d . . . H14 H 0.6023 0.1962 0.7103 0.051 Uiso 1 1 calc R . . C15 C 0.72697(18) 0.3306(3) 0.70400(13) 0.0427(5) Uani 1 1 d . . . H15 H 0.7458 0.3591 0.7609 0.051 Uiso 1 1 calc R . . C16 C 0.78377(15) 0.3859(3) 0.65000(11) 0.0331(4) Uani 1 1 d . . . H16 H 0.8418 0.4522 0.6710 0.040 Uiso 1 1 calc R . . C17 C 0.50556(16) 0.3032(3) 0.28137(13) 0.0426(5) Uani 1 1 d . . . H17A H 0.5568 0.3230 0.2507 0.064 Uiso 1 1 calc R . . H17B H 0.4472 0.3714 0.2552 0.064 Uiso 1 1 calc R . . H17C H 0.4902 0.1727 0.2815 0.064 Uiso 1 1 calc R . . C18 C 0.44028(15) 0.3280(3) 0.42398(15) 0.0380(5) Uani 1 1 d . . . H18A H 0.4508 0.3629 0.4821 0.057 Uiso 1 1 calc R . . H18B H 0.4273 0.1966 0.4185 0.057 Uiso 1 1 calc R . . H18C H 0.3845 0.3955 0.3923 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0239(2) 0.0243(2) 0.0305(2) 0.00059(17) 0.00195(17) 0.00142(17) S2 0.0206(2) 0.0268(3) 0.0399(3) -0.00216(19) 0.00223(18) -0.00026(18) B1 0.0209(10) 0.0218(10) 0.0283(10) 0.0003(8) 0.0013(8) 0.0034(8) B2 0.0220(10) 0.0206(10) 0.0397(11) -0.0024(8) 0.0038(8) 0.0006(8) C1 0.0214(9) 0.0217(9) 0.0279(8) 0.0014(7) 0.0018(7) 0.0042(7) C2 0.0223(9) 0.0214(9) 0.0314(9) -0.0018(7) 0.0006(7) 0.0036(7) C3 0.0289(10) 0.0288(10) 0.0350(10) -0.0073(8) -0.0019(8) 0.0043(8) C4 0.0392(11) 0.0363(11) 0.0264(9) -0.0055(8) 0.0028(8) 0.0118(9) C5 0.0349(11) 0.0351(11) 0.0314(9) 0.0034(8) 0.0114(8) 0.0105(9) C6 0.0241(9) 0.0286(10) 0.0327(9) 0.0025(8) 0.0040(7) 0.0035(7) C7 0.0357(11) 0.0314(11) 0.0374(10) 0.0064(8) 0.0094(9) -0.0010(9) C8 0.0395(12) 0.0305(11) 0.0397(11) -0.0063(8) 0.0094(9) 0.0009(9) C11 0.0249(9) 0.0208(9) 0.0288(8) 0.0031(7) 0.0037(7) 0.0063(7) C12 0.0264(9) 0.0176(9) 0.0357(10) 0.0050(7) 0.0070(8) 0.0056(7) C13 0.0327(11) 0.0239(10) 0.0503(12) 0.0090(9) 0.0136(9) 0.0025(8) C14 0.0504(14) 0.0405(13) 0.0426(11) 0.0177(10) 0.0216(10) 0.0082(10) C15 0.0504(14) 0.0492(14) 0.0284(10) 0.0119(9) 0.0083(9) 0.0076(11) C16 0.0322(10) 0.0366(11) 0.0278(9) 0.0054(8) 0.0007(8) 0.0054(9) C17 0.0318(11) 0.0495(14) 0.0410(11) -0.0052(10) -0.0044(9) -0.0001(10) C18 0.0250(10) 0.0302(11) 0.0597(13) 0.0016(9) 0.0110(9) 0.0021(8) _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 S1 C7 1.799(2) . ? S1 C8 1.801(2) . ? S1 B1 2.031(2) . ? S2 C18 1.796(2) . ? S2 C17 1.799(2) . ? S2 B2 2.030(2) . ? B1 C11 1.603(3) . ? B1 C1 1.610(3) . ? B1 H1 1.19(2) . ? B2 C2 1.606(3) . ? B2 C12 1.609(3) . ? B2 H2 1.19(2) . ? C1 C6 1.405(3) . ? C1 C2 1.417(3) . ? C2 C3 1.407(3) . ? C3 C4 1.390(3) . ? C3 H3 0.9500 . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 C6 1.392(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 C16 1.409(3) . ? C11 C12 1.417(3) . ? C12 C13 1.405(3) . ? C13 C14 1.394(3) . ? C13 H13 0.9500 . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 C16 1.385(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 C7 S1 C8 98.62(10) . . ? C7 S1 B1 103.28(9) . . ? C8 S1 B1 104.57(9) . . ? C18 S2 C17 98.75(11) . . ? C18 S2 B2 103.11(10) . . ? C17 S2 B2 104.52(10) . . ? C11 B1 C1 114.75(15) . . ? C11 B1 S1 106.22(12) . . ? C1 B1 S1 105.02(12) . . ? C11 B1 H1 109.7(12) . . ? C1 B1 H1 115.7(12) . . ? S1 B1 H1 104.2(12) . . ? C2 B2 C12 115.22(16) . . ? C2 B2 S2 105.06(13) . . ? C12 B2 S2 104.75(13) . . ? C2 B2 H2 111.1(11) . . ? C12 B2 H2 117.0(11) . . ? S2 B2 H2 101.7(11) . . ? C6 C1 C2 118.17(16) . . ? C6 C1 B1 121.38(16) . . ? C2 C1 B1 120.45(16) . . ? C3 C2 C1 118.48(18) . . ? C3 C2 B2 120.12(17) . . ? C1 C2 B2 121.37(16) . . ? C4 C3 C2 122.27(19) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C5 C4 C3 119.24(18) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 119.50(19) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C5 C6 C1 122.32(18) . . ? C5 C6 H6 118.8 . . ? C1 C6 H6 118.8 . . ? S1 C7 H7A 109.5 . . ? S1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S1 C8 H8A 109.5 . . ? S1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C16 C11 C12 118.23(18) . . ? C16 C11 B1 120.32(17) . . ? C12 C11 B1 121.44(15) . . ? C13 C12 C11 118.33(17) . . ? C13 C12 B2 121.15(18) . . ? C11 C12 B2 120.44(16) . . ? C14 C13 C12 122.1(2) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C15 C14 C13 119.6(2) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.3(2) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C15 C16 C11 122.5(2) . . ? C15 C16 H16 118.8 . . ? C11 C16 H16 118.8 . . ? S2 C17 H17A 109.5 . . ? S2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S2 C18 H18A 109.5 . . ? S2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? S2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 C7 S1 B1 C11 168.91(12) . . . . ? C8 S1 B1 C11 66.18(14) . . . . ? C7 S1 B1 C1 -69.11(14) . . . . ? C8 S1 B1 C1 -171.84(13) . . . . ? C18 S2 B2 C2 166.58(13) . . . . ? C17 S2 B2 C2 63.77(15) . . . . ? C18 S2 B2 C12 -71.60(15) . . . . ? C17 S2 B2 C12 -174.41(14) . . . . ? C11 B1 C1 C6 -158.02(16) . . . . ? S1 B1 C1 C6 85.74(17) . . . . ? C11 B1 C1 C2 20.9(2) . . . . ? S1 B1 C1 C2 -95.39(17) . . . . ? C6 C1 C2 C3 0.1(3) . . . . ? B1 C1 C2 C3 -178.77(16) . . . . ? C6 C1 C2 B2 178.24(16) . . . . ? B1 C1 C2 B2 -0.7(2) . . . . ? C12 B2 C2 C3 159.30(17) . . . . ? S2 B2 C2 C3 -85.98(18) . . . . ? C12 B2 C2 C1 -18.8(2) . . . . ? S2 B2 C2 C1 95.95(17) . . . . ? C1 C2 C3 C4 -1.5(3) . . . . ? B2 C2 C3 C4 -179.64(18) . . . . ? C2 C3 C4 C5 1.6(3) . . . . ? C3 C4 C5 C6 -0.2(3) . . . . ? C4 C5 C6 C1 -1.2(3) . . . . ? C2 C1 C6 C5 1.2(3) . . . . ? B1 C1 C6 C5 -179.91(17) . . . . ? C1 B1 C11 C16 157.20(16) . . . . ? S1 B1 C11 C16 -87.25(17) . . . . ? C1 B1 C11 C12 -22.1(2) . . . . ? S1 B1 C11 C12 93.48(17) . . . . ? C16 C11 C12 C13 0.4(3) . . . . ? B1 C11 C12 C13 179.71(16) . . . . ? C16 C11 C12 B2 -176.46(16) . . . . ? B1 C11 C12 B2 2.8(3) . . . . ? C2 B2 C12 C13 -159.18(17) . . . . ? S2 B2 C12 C13 85.93(18) . . . . ? C2 B2 C12 C11 17.6(2) . . . . ? S2 B2 C12 C11 -97.29(17) . . . . ? C11 C12 C13 C14 0.7(3) . . . . ? B2 C12 C13 C14 177.57(18) . . . . ? C12 C13 C14 C15 -1.4(3) . . . . ? C13 C14 C15 C16 0.9(3) . . . . ? C14 C15 C16 C11 0.2(3) . . . . ? C12 C11 C16 C15 -0.9(3) . . . . ? B1 C11 C16 C15 179.80(19) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.532 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.054 data_wa975 _database_code_depnum_ccdc_archive 'CCDC 762846' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 B2 N2, C4 H8 O' _chemical_formula_sum 'C24 H24 B2 N2 O' _chemical_formula_weight 378.07 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6419(7) _cell_length_b 13.8641(8) _cell_length_c 13.8898(9) _cell_angle_alpha 91.748(5) _cell_angle_beta 95.552(5) _cell_angle_gamma 92.350(5) _cell_volume 2036.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25837 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 26.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details . _exptl_special_details ; ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 34216 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 25.70 _reflns_number_total 7626 _reflns_number_gt 5610 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.1254P)^2^+0.4703P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.030(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7626 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2108 _refine_ls_wR_factor_gt 0.1956 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.7126(3) 0.8218(2) 0.2910(2) 0.0428(6) Uani 1 1 d . . . H1 H 0.695(3) 0.887(2) 0.247(2) 0.052(8) Uiso 1 1 d . . . B2 B 0.7686(3) 0.6767(2) 0.4144(2) 0.0414(6) Uani 1 1 d . . . H2 H 0.792(3) 0.622(2) 0.4760(19) 0.043(7) Uiso 1 1 d . . . N1 N 0.76542(19) 0.85878(14) 0.40144(14) 0.0374(5) Uani 1 1 d . . . N2 N 0.79295(19) 0.78537(14) 0.46412(14) 0.0377(5) Uani 1 1 d . . . C3 C 0.8347(2) 0.80602(19) 0.55402(18) 0.0410(6) Uani 1 1 d . . . H3 H 0.8507 0.7543 0.5962 0.049 Uiso 1 1 calc R . . C4 C 0.8571(2) 0.90171(19) 0.59170(18) 0.0412(6) Uani 1 1 d . . . C5 C 0.9059(3) 0.9245(2) 0.6878(2) 0.0522(7) Uani 1 1 d . . . H5 H 0.9238 0.8748 0.7320 0.063 Uiso 1 1 calc R . . C6 C 0.9271(3) 1.0198(3) 0.7165(2) 0.0607(8) Uani 1 1 d . . . H6 H 0.9617 1.0356 0.7810 0.073 Uiso 1 1 calc R . . C7 C 0.8989(3) 1.0944(2) 0.6532(2) 0.0601(8) Uani 1 1 d . . . H7 H 0.9136 1.1598 0.6753 0.072 Uiso 1 1 calc R . . C8 C 0.8503(3) 1.0738(2) 0.5594(2) 0.0547(7) Uani 1 1 d . . . H8 H 0.8307 1.1243 0.5166 0.066 Uiso 1 1 calc R . . C9 C 0.8299(2) 0.97659(19) 0.52750(18) 0.0420(6) Uani 1 1 d . . . C10 C 0.7824(2) 0.94919(18) 0.43206(19) 0.0424(6) Uani 1 1 d . . . H10 H 0.7618 0.9984 0.3879 0.051 Uiso 1 1 calc R . . C11 C 0.8249(2) 0.75578(18) 0.26022(17) 0.0392(5) Uani 1 1 d . . . C12 C 0.8551(2) 0.68163(18) 0.32525(18) 0.0396(5) Uani 1 1 d . . . C13 C 0.9521(3) 0.62148(19) 0.30691(19) 0.0450(6) Uani 1 1 d . . . H13 H 0.9738 0.5720 0.3506 0.054 Uiso 1 1 calc R . . C14 C 1.0180(3) 0.6324(2) 0.2259(2) 0.0512(7) Uani 1 1 d . . . H14 H 1.0840 0.5907 0.2145 0.061 Uiso 1 1 calc R . . C15 C 0.9868(3) 0.7043(2) 0.1620(2) 0.0511(7) Uani 1 1 d . . . H15 H 1.0309 0.7115 0.1062 0.061 Uiso 1 1 calc R . . C16 C 0.8911(3) 0.76589(19) 0.17939(18) 0.0443(6) Uani 1 1 d . . . H16 H 0.8708 0.8155 0.1355 0.053 Uiso 1 1 calc R . . C21 C 0.5934(2) 0.75256(19) 0.30899(18) 0.0446(6) Uani 1 1 d . . . C22 C 0.6222(3) 0.67631(18) 0.37233(18) 0.0426(6) Uani 1 1 d . . . C23 C 0.5252(3) 0.6125(2) 0.3937(2) 0.0528(7) Uani 1 1 d . . . H23 H 0.5433 0.5614 0.4361 0.063 Uiso 1 1 calc R . . C24 C 0.4014(3) 0.6231(2) 0.3531(3) 0.0638(9) Uani 1 1 d . . . H24 H 0.3362 0.5782 0.3669 0.077 Uiso 1 1 calc R . . C25 C 0.3735(3) 0.6980(3) 0.2934(3) 0.0677(9) Uani 1 1 d . . . H25 H 0.2886 0.7057 0.2676 0.081 Uiso 1 1 calc R . . C26 C 0.4683(3) 0.7626(2) 0.2704(2) 0.0556(7) Uani 1 1 d . . . H26 H 0.4483 0.8138 0.2284 0.067 Uiso 1 1 calc R . . B1A B 0.6586(3) 0.79444(19) 0.8657(2) 0.0378(6) Uani 1 1 d . . . H1A H 0.657(2) 0.8380(18) 0.9409(18) 0.033(6) Uiso 1 1 d . . . B2A B 0.6305(3) 0.6630(2) 0.71413(19) 0.0379(6) Uani 1 1 d . . . H2A H 0.606(2) 0.6035(18) 0.6587(18) 0.035(6) Uiso 1 1 d . . . N1A N 0.55784(19) 0.70356(14) 0.87896(13) 0.0352(4) Uani 1 1 d . . . N2A N 0.54499(19) 0.63707(13) 0.80303(13) 0.0343(4) Uani 1 1 d . . . C3A C 0.4706(2) 0.55962(17) 0.80613(17) 0.0373(5) Uani 1 1 d . . . H3A H 0.4651 0.5137 0.7535 0.045 Uiso 1 1 calc R . . C4A C 0.3980(2) 0.54143(17) 0.88487(17) 0.0368(5) Uani 1 1 d . . . C5A C 0.3164(3) 0.4590(2) 0.8874(2) 0.0469(6) Uani 1 1 d . . . H5A H 0.3074 0.4124 0.8354 0.056 Uiso 1 1 calc R . . C6A C 0.2502(3) 0.4475(2) 0.9668(2) 0.0527(7) Uani 1 1 d . . . H6A H 0.1954 0.3920 0.9698 0.063 Uiso 1 1 calc R . . C7A C 0.2622(3) 0.5163(2) 1.0430(2) 0.0537(7) Uani 1 1 d . . . H7A H 0.2153 0.5066 1.0970 0.064 Uiso 1 1 calc R . . C8A C 0.3403(3) 0.5975(2) 1.0418(2) 0.0478(6) Uani 1 1 d . . . H8A H 0.3475 0.6438 1.0941 0.057 Uiso 1 1 calc R . . C9A C 0.4095(2) 0.61050(17) 0.96116(17) 0.0370(5) Uani 1 1 d . . . C10A C 0.4940(2) 0.69105(18) 0.95404(17) 0.0378(5) Uani 1 1 d . . . H10A H 0.5047 0.7380 1.0058 0.045 Uiso 1 1 calc R . . C11A C 0.6031(2) 0.83802(16) 0.76526(17) 0.0356(5) Uani 1 1 d . . . C12A C 0.5875(2) 0.77037(16) 0.68662(16) 0.0351(5) Uani 1 1 d . . . C13A C 0.5389(2) 0.79886(18) 0.59584(18) 0.0393(5) Uani 1 1 d . . . H13A H 0.5263 0.7528 0.5434 0.047 Uiso 1 1 calc R . . C14A C 0.5083(2) 0.89489(19) 0.58128(19) 0.0440(6) Uani 1 1 d . . . H14A H 0.4765 0.9141 0.5188 0.053 Uiso 1 1 calc R . . C15A C 0.5244(3) 0.96160(19) 0.6576(2) 0.0460(6) Uani 1 1 d . . . H15A H 0.5046 1.0269 0.6475 0.055 Uiso 1 1 calc R . . C16A C 0.5697(2) 0.93351(18) 0.74951(19) 0.0418(6) Uani 1 1 d . . . H16A H 0.5782 0.9795 0.8021 0.050 Uiso 1 1 calc R . . C21A C 0.7855(2) 0.73814(17) 0.84803(17) 0.0375(5) Uani 1 1 d . . . C22A C 0.7698(2) 0.67040(17) 0.76939(17) 0.0377(5) Uani 1 1 d . . . C23A C 0.8717(2) 0.61538(18) 0.74955(19) 0.0434(6) Uani 1 1 d . . . H23A H 0.8616 0.5691 0.6972 0.052 Uiso 1 1 calc R . . C24A C 0.9867(3) 0.6270(2) 0.8045(2) 0.0523(7) Uani 1 1 d . . . H24A H 1.0550 0.5888 0.7899 0.063 Uiso 1 1 calc R . . C25A C 1.0027(3) 0.6944(2) 0.8809(2) 0.0544(7) Uani 1 1 d . . . H25A H 1.0820 0.7028 0.9185 0.065 Uiso 1 1 calc R . . C26A C 0.9019(3) 0.7499(2) 0.90246(19) 0.0453(6) Uani 1 1 d . . . H26A H 0.9130 0.7961 0.9548 0.054 Uiso 1 1 calc R . . O31 O 0.1239(3) 0.7592(2) 0.6024(3) 0.1058(10) Uani 1 1 d . . . C32 C 0.2409(5) 0.7236(5) 0.6821(4) 0.141(3) Uani 1 1 d . A . H32A H 0.3171 0.7675 0.6861 0.169 Uiso 1 1 calc R . . H32B H 0.2134 0.7148 0.7475 0.169 Uiso 1 1 calc R . . C33 C 0.2585(4) 0.6309(4) 0.6310(3) 0.0916(13) Uani 1 1 d . . . H33A H 0.3461 0.6292 0.6128 0.110 Uiso 1 1 calc R A . H33B H 0.2449 0.5769 0.6743 0.110 Uiso 1 1 calc R . . C34 C 0.1694(10) 0.6194(8) 0.5441(6) 0.212(5) Uani 1 1 d . A . H34A H 0.2058 0.5800 0.4939 0.254 Uiso 0.52(2) 1 calc PR A 1 H34B H 0.0898 0.5864 0.5595 0.254 Uiso 0.52(2) 1 calc PR A 1 H34C H 0.2120 0.6328 0.4853 0.254 Uiso 0.48(2) 1 calc PR A 2 H34D H 0.1305 0.5531 0.5377 0.254 Uiso 0.48(2) 1 calc PR A 2 C35 C 0.1492(15) 0.6980(10) 0.5156(11) 0.120(5) Uiso 0.52(2) 1 d P A 1 H35A H 0.0750 0.6954 0.4665 0.143 Uiso 0.52(2) 1 calc PR A 1 H35B H 0.2232 0.7251 0.4858 0.143 Uiso 0.52(2) 1 calc PR A 1 C35' C 0.0919(14) 0.6771(9) 0.5560(10) 0.098(5) Uiso 0.48(2) 1 d P A 2 H35C H 0.0256 0.6447 0.5904 0.117 Uiso 0.48(2) 1 calc PR A 2 H35D H 0.0519 0.6924 0.4912 0.117 Uiso 0.48(2) 1 calc PR A 2 O31A O 0.3585(4) 0.8741(3) 1.0318(3) 0.0640(14) Uiso 0.608(9) 1 d P B 1 O31" O 0.2995(9) 0.8293(7) 0.9963(7) 0.098(3) Uiso 0.392(9) 1 d P B 2 C32A C 0.2433(4) 0.8738(3) 1.0686(3) 0.0771(10) Uani 1 1 d . . . H32C H 0.2555 0.8862 1.1395 0.093 Uiso 0.608(9) 1 calc PR B 1 H32D H 0.1992 0.8098 1.0558 0.093 Uiso 0.608(9) 1 calc PR B 1 H32E H 0.3078 0.9031 1.1182 0.093 Uiso 0.392(9) 1 calc PR B 2 H32F H 0.1893 0.8268 1.1000 0.093 Uiso 0.392(9) 1 calc PR B 2 C33A C 0.1678(4) 0.9475(3) 1.0238(3) 0.0786(10) Uani 1 1 d . B . H33C H 0.1830 1.0099 1.0605 0.094 Uiso 1 1 calc R . . H33D H 0.0767 0.9287 1.0202 0.094 Uiso 1 1 calc R . . C34A C 0.2101(6) 0.9542(4) 0.9261(4) 0.1118(17) Uani 1 1 d . . . H34E H 0.2017 1.0201 0.9013 0.134 Uiso 0.608(9) 1 calc PR B 1 H34F H 0.1630 0.9070 0.8797 0.134 Uiso 0.608(9) 1 calc PR B 1 H34G H 0.2505 1.0188 0.9185 0.134 Uiso 0.392(9) 1 calc PR B 2 H34H H 0.1368 0.9449 0.8766 0.134 Uiso 0.392(9) 1 calc PR B 2 C35A C 0.3486(6) 0.9294(5) 0.9465(5) 0.0756(19) Uiso 0.608(9) 1 d P B 1 H35E H 0.3758 0.8916 0.8913 0.091 Uiso 0.608(9) 1 calc PR B 1 H35F H 0.4029 0.9892 0.9566 0.091 Uiso 0.608(9) 1 calc PR B 1 C35" C 0.3014(16) 0.8785(13) 0.9134(12) 0.118(5) Uiso 0.392(9) 1 d P B 2 H35G H 0.2743 0.8361 0.8559 0.142 Uiso 0.392(9) 1 calc PR B 2 H35H H 0.3868 0.9072 0.9069 0.142 Uiso 0.392(9) 1 calc PR B 2 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 0.0539(17) 0.0391(15) 0.0343(14) -0.0008(11) -0.0014(12) 0.0043(13) B2 0.0553(17) 0.0305(14) 0.0381(14) 0.0000(11) 0.0053(12) -0.0008(12) N1 0.0451(11) 0.0330(10) 0.0345(10) 0.0024(8) 0.0044(8) 0.0038(8) N2 0.0438(11) 0.0347(11) 0.0347(11) 0.0024(8) 0.0052(8) -0.0003(8) C3 0.0467(14) 0.0421(14) 0.0340(12) 0.0023(10) 0.0059(10) -0.0044(11) C4 0.0419(13) 0.0456(14) 0.0362(13) -0.0035(11) 0.0094(10) -0.0072(11) C5 0.0568(16) 0.0617(18) 0.0368(14) -0.0051(12) 0.0065(12) -0.0116(13) C6 0.0644(19) 0.073(2) 0.0428(15) -0.0175(14) 0.0071(13) -0.0155(15) C7 0.0614(18) 0.0544(18) 0.0630(19) -0.0212(15) 0.0093(15) -0.0070(14) C8 0.0605(17) 0.0429(15) 0.0588(17) -0.0095(13) 0.0013(13) 0.0006(13) C9 0.0434(13) 0.0405(14) 0.0417(14) -0.0051(11) 0.0059(10) -0.0004(10) C10 0.0481(14) 0.0350(13) 0.0439(14) -0.0013(10) 0.0048(11) 0.0020(10) C11 0.0457(13) 0.0360(13) 0.0349(12) -0.0022(10) 0.0013(10) -0.0022(10) C12 0.0450(13) 0.0359(13) 0.0371(12) -0.0018(10) 0.0025(10) -0.0030(10) C13 0.0491(14) 0.0393(14) 0.0464(14) -0.0004(11) 0.0023(11) 0.0053(11) C14 0.0468(15) 0.0501(16) 0.0573(17) -0.0093(13) 0.0102(12) 0.0047(12) C15 0.0556(16) 0.0536(16) 0.0452(15) -0.0063(12) 0.0159(12) -0.0037(13) C16 0.0560(15) 0.0402(14) 0.0365(13) -0.0011(10) 0.0056(11) -0.0036(11) C21 0.0481(14) 0.0451(14) 0.0394(13) -0.0130(11) 0.0030(11) 0.0032(11) C22 0.0523(15) 0.0387(13) 0.0370(13) -0.0096(10) 0.0097(11) -0.0006(11) C23 0.0620(18) 0.0442(15) 0.0530(16) -0.0165(12) 0.0203(13) -0.0101(13) C24 0.0527(17) 0.0592(19) 0.079(2) -0.0293(17) 0.0216(16) -0.0142(14) C25 0.0460(16) 0.070(2) 0.084(2) -0.0334(19) 0.0009(15) -0.0018(15) C26 0.0503(16) 0.0571(18) 0.0566(17) -0.0207(14) -0.0042(13) 0.0077(13) B1A 0.0505(16) 0.0294(13) 0.0334(13) 0.0009(10) 0.0066(11) -0.0034(11) B2A 0.0520(16) 0.0310(13) 0.0324(13) 0.0033(11) 0.0124(11) 0.0006(11) N1A 0.0470(11) 0.0299(10) 0.0291(10) 0.0002(8) 0.0060(8) 0.0014(8) N2A 0.0460(11) 0.0271(10) 0.0305(10) 0.0012(7) 0.0076(8) 0.0011(8) C3A 0.0456(13) 0.0325(12) 0.0335(12) 0.0029(9) 0.0024(10) -0.0008(10) C4A 0.0409(13) 0.0361(12) 0.0335(12) 0.0078(9) 0.0023(9) -0.0002(10) C5A 0.0506(15) 0.0441(14) 0.0449(14) 0.0100(11) 0.0001(11) -0.0085(11) C6A 0.0466(15) 0.0553(17) 0.0557(17) 0.0191(14) 0.0029(12) -0.0115(12) C7A 0.0504(15) 0.0610(18) 0.0533(16) 0.0188(14) 0.0178(13) 0.0025(13) C8A 0.0547(16) 0.0493(15) 0.0425(14) 0.0084(12) 0.0167(12) 0.0058(12) C9A 0.0406(12) 0.0371(12) 0.0341(12) 0.0063(10) 0.0052(9) 0.0028(10) C10A 0.0486(14) 0.0362(12) 0.0297(11) 0.0028(9) 0.0075(10) 0.0051(10) C11A 0.0425(13) 0.0293(11) 0.0360(12) 0.0024(9) 0.0098(10) 0.0000(9) C12A 0.0420(12) 0.0310(12) 0.0337(12) 0.0029(9) 0.0104(9) -0.0005(9) C13A 0.0462(13) 0.0383(13) 0.0342(12) 0.0030(10) 0.0089(10) -0.0004(10) C14A 0.0504(14) 0.0421(14) 0.0412(14) 0.0130(11) 0.0077(11) 0.0051(11) C15A 0.0542(15) 0.0345(13) 0.0516(15) 0.0115(11) 0.0105(12) 0.0084(11) C16A 0.0503(14) 0.0304(12) 0.0457(14) 0.0019(10) 0.0095(11) 0.0015(10) C21A 0.0486(14) 0.0315(12) 0.0333(12) 0.0089(9) 0.0078(10) -0.0032(10) C22A 0.0507(14) 0.0303(12) 0.0342(12) 0.0104(9) 0.0123(10) 0.0004(10) C23A 0.0520(15) 0.0378(13) 0.0433(14) 0.0104(11) 0.0156(11) 0.0036(11) C24A 0.0501(16) 0.0521(16) 0.0584(17) 0.0138(14) 0.0182(13) 0.0091(13) C25A 0.0444(15) 0.0655(19) 0.0542(17) 0.0164(14) 0.0045(12) 0.0023(13) C26A 0.0513(15) 0.0451(15) 0.0396(13) 0.0085(11) 0.0058(11) -0.0040(11) O31 0.104(2) 0.081(2) 0.136(3) 0.0075(19) 0.019(2) 0.0261(18) C32 0.109(4) 0.193(6) 0.121(4) -0.044(4) 0.068(4) -0.090(4) C33 0.075(3) 0.104(3) 0.096(3) 0.033(3) -0.002(2) 0.012(2) C34 0.246(10) 0.242(11) 0.144(6) 0.031(7) -0.052(7) 0.119(9) C32A 0.072(2) 0.074(2) 0.084(3) -0.004(2) 0.0060(19) -0.0021(18) C33A 0.063(2) 0.071(2) 0.101(3) -0.004(2) 0.0069(19) 0.0033(17) C34A 0.145(5) 0.088(3) 0.102(4) 0.040(3) -0.008(3) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 C21 1.602(4) . ? B1 C11 1.617(4) . ? B1 N1 1.641(3) . ? B1 H1 1.12(3) . ? B2 C22 1.609(4) . ? B2 C12 1.614(4) . ? B2 N2 1.639(3) . ? B2 H2 1.17(3) . ? N1 C10 1.311(3) . ? N1 N2 1.382(3) . ? N2 C3 1.303(3) . ? C3 C4 1.414(4) . ? C3 H3 0.9500 . ? C4 C5 1.406(4) . ? C4 C9 1.410(4) . ? C5 C6 1.372(4) . ? C5 H5 0.9500 . ? C6 C7 1.402(5) . ? C6 H6 0.9500 . ? C7 C8 1.372(4) . ? C7 H7 0.9500 . ? C8 C9 1.407(4) . ? C8 H8 0.9500 . ? C9 C10 1.407(4) . ? C10 H10 0.9500 . ? C11 C16 1.390(4) . ? C11 C12 1.415(3) . ? C12 C13 1.391(4) . ? C13 C14 1.391(4) . ? C13 H13 0.9500 . ? C14 C15 1.383(4) . ? C14 H14 0.9500 . ? C15 C16 1.390(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.400(4) . ? C21 C22 1.420(4) . ? C22 C23 1.392(4) . ? C23 C24 1.397(5) . ? C23 H23 0.9500 . ? C24 C25 1.373(5) . ? C24 H24 0.9500 . ? C25 C26 1.390(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? B1A C11A 1.607(4) . ? B1A C21A 1.623(4) . ? B1A N1A 1.647(3) . ? B1A H1A 1.19(2) . ? B2A C22A 1.600(4) . ? B2A C12A 1.621(3) . ? B2A N2A 1.643(3) . ? B2A H2A 1.12(3) . ? N1A C10A 1.311(3) . ? N1A N2A 1.372(3) . ? N2A C3A 1.312(3) . ? C3A C4A 1.422(3) . ? C3A H3A 0.9500 . ? C4A C9A 1.399(4) . ? C4A C5A 1.410(4) . ? C5A C6A 1.375(4) . ? C5A H5A 0.9500 . ? C6A C7A 1.396(5) . ? C6A H6A 0.9500 . ? C7A C8A 1.373(4) . ? C7A H7A 0.9500 . ? C8A C9A 1.412(3) . ? C8A H8A 0.9500 . ? C9A C10A 1.416(3) . ? C10A H10A 0.9500 . ? C11A C16A 1.403(3) . ? C11A C12A 1.411(3) . ? C12A C13A 1.391(3) . ? C13A C14A 1.400(4) . ? C13A H13A 0.9500 . ? C14A C15A 1.378(4) . ? C14A H14A 0.9500 . ? C15A C16A 1.393(4) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C21A C26A 1.388(4) . ? C21A C22A 1.411(3) . ? C22A C23A 1.395(4) . ? C23A C24A 1.379(4) . ? C23A H23A 0.9500 . ? C24A C25A 1.386(5) . ? C24A H24A 0.9500 . ? C25A C26A 1.396(4) . ? C25A H25A 0.9500 . ? C26A H26A 0.9500 . ? O31 C35' 1.307(12) . ? O31 C35 1.505(14) . ? O31 C32 1.684(8) . ? C32 C33 1.477(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.461(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35' 1.192(13) . ? C34 C35 1.192(15) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 H34C 0.9900 . ? C34 H34D 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35' H35C 0.9900 . ? C35' H35D 0.9900 . ? O31A C32A 1.373(5) . ? O31A C35A 1.428(7) . ? O31" C35" 1.357(16) . ? O31" C32A 1.362(9) . ? C32A C33A 1.444(5) . ? C32A H32C 0.9900 . ? C32A H32D 0.9900 . ? C32A H32E 0.9900 . ? C32A H32F 0.9900 . ? C33A C34A 1.475(6) . ? C33A H33C 0.9900 . ? C33A H33D 0.9900 . ? C34A C35" 1.477(16) . ? C34A C35A 1.529(9) . ? C34A H34E 0.9900 . ? C34A H34F 0.9900 . ? C34A H34G 0.9900 . ? C34A H34H 0.9900 . ? C35A H35E 0.9900 . ? C35A H35F 0.9900 . ? C35" H35G 0.9900 . ? C35" H35H 0.9900 . ? 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 C21 B1 C11 108.7(2) . . ? C21 B1 N1 102.3(2) . . ? C11 B1 N1 102.2(2) . . ? C21 B1 H1 117.9(15) . . ? C11 B1 H1 115.8(15) . . ? N1 B1 H1 107.8(15) . . ? C22 B2 C12 108.9(2) . . ? C22 B2 N2 102.6(2) . . ? C12 B2 N2 101.91(19) . . ? C22 B2 H2 115.4(13) . . ? C12 B2 H2 119.3(13) . . ? N2 B2 H2 106.5(14) . . ? C10 N1 N2 120.1(2) . . ? C10 N1 B1 125.5(2) . . ? N2 N1 B1 114.45(19) . . ? C3 N2 N1 120.0(2) . . ? C3 N2 B2 126.0(2) . . ? N1 N2 B2 114.06(18) . . ? N2 C3 C4 123.1(2) . . ? N2 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C5 C4 C9 119.7(3) . . ? C5 C4 C3 123.4(3) . . ? C9 C4 C3 116.9(2) . . ? C6 C5 C4 118.8(3) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C5 C6 C7 121.6(3) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C8 C7 C6 120.5(3) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 119.1(3) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C8 C9 C10 122.6(3) . . ? C8 C9 C4 120.3(2) . . ? C10 C9 C4 117.0(2) . . ? N1 C10 C9 122.9(2) . . ? N1 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C16 C11 C12 119.6(2) . . ? C16 C11 B1 126.7(2) . . ? C12 C11 B1 113.7(2) . . ? C13 C12 C11 118.7(2) . . ? C13 C12 B2 127.1(2) . . ? C11 C12 B2 114.2(2) . . ? C12 C13 C14 121.3(2) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C15 C14 C13 119.6(3) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.1(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 120.7(2) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C26 C21 C22 119.5(3) . . ? C26 C21 B1 126.2(3) . . ? C22 C21 B1 114.3(2) . . ? C23 C22 C21 119.0(3) . . ? C23 C22 B2 127.2(3) . . ? C21 C22 B2 113.8(2) . . ? C22 C23 C24 120.5(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 120.3(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.5(3) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 120.1(3) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? C11A B1A C21A 108.80(19) . . ? C11A B1A N1A 102.67(19) . . ? C21A B1A N1A 101.42(18) . . ? C11A B1A H1A 121.5(12) . . ? C21A B1A H1A 117.6(12) . . ? N1A B1A H1A 101.0(12) . . ? C22A B2A C12A 109.2(2) . . ? C22A B2A N2A 101.35(18) . . ? C12A B2A N2A 102.60(18) . . ? C22A B2A H2A 118.9(13) . . ? C12A B2A H2A 117.3(13) . . ? N2A B2A H2A 104.6(13) . . ? C10A N1A N2A 120.2(2) . . ? C10A N1A B1A 125.6(2) . . ? N2A N1A B1A 114.12(17) . . ? C3A N2A N1A 120.11(19) . . ? C3A N2A B2A 125.35(19) . . ? N1A N2A B2A 114.52(18) . . ? N2A C3A C4A 122.8(2) . . ? N2A C3A H3A 118.6 . . ? C4A C3A H3A 118.6 . . ? C9A C4A C5A 120.4(2) . . ? C9A C4A C3A 116.8(2) . . ? C5A C4A C3A 122.8(2) . . ? C6A C5A C4A 118.7(3) . . ? C6A C5A H5A 120.7 . . ? C4A C5A H5A 120.7 . . ? C5A C6A C7A 120.8(3) . . ? C5A C6A H6A 119.6 . . ? C7A C6A H6A 119.6 . . ? C8A C7A C6A 121.6(2) . . ? C8A C7A H7A 119.2 . . ? C6A C7A H7A 119.2 . . ? C7A C8A C9A 118.4(3) . . ? C7A C8A H8A 120.8 . . ? C9A C8A H8A 120.8 . . ? C4A C9A C8A 120.1(2) . . ? C4A C9A C10A 117.3(2) . . ? C8A C9A C10A 122.6(2) . . ? N1A C10A C9A 122.7(2) . . ? N1A C10A H10A 118.6 . . ? C9A C10A H10A 118.6 . . ? C16A C11A C12A 118.8(2) . . ? C16A C11A B1A 127.0(2) . . ? C12A C11A B1A 114.3(2) . . ? C13A C12A C11A 119.9(2) . . ? C13A C12A B2A 126.2(2) . . ? C11A C12A B2A 113.9(2) . . ? C12A C13A C14A 120.5(2) . . ? C12A C13A H13A 119.8 . . ? C14A C13A H13A 119.8 . . ? C15A C14A C13A 120.0(2) . . ? C15A C14A H14A 120.0 . . ? C13A C14A H14A 120.0 . . ? C14A C15A C16A 120.2(2) . . ? C14A C15A H15A 119.9 . . ? C16A C15A H15A 119.9 . . ? C15A C16A C11A 120.7(2) . . ? C15A C16A H16A 119.6 . . ? C11A C16A H16A 119.6 . . ? C26A C21A C22A 119.6(2) . . ? C26A C21A B1A 126.5(2) . . ? C22A C21A B1A 113.9(2) . . ? C23A C22A C21A 118.9(2) . . ? C23A C22A B2A 126.8(2) . . ? C21A C22A B2A 114.3(2) . . ? C24A C23A C22A 121.2(3) . . ? C24A C23A H23A 119.4 . . ? C22A C23A H23A 119.4 . . ? C23A C24A C25A 120.0(3) . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C24A C25A C26A 119.8(3) . . ? C24A C25A H25A 120.1 . . ? C26A C25A H25A 120.1 . . ? C21A C26A C25A 120.6(3) . . ? C21A C26A H26A 119.7 . . ? C25A C26A H26A 119.7 . . ? C35' O31 C35 37.0(6) . . ? C35' O31 C32 100.0(6) . . ? C35 O31 C32 99.2(6) . . ? C33 C32 O31 95.7(4) . . ? C33 C32 H32A 112.6 . . ? O31 C32 H32A 112.6 . . ? C33 C32 H32B 112.6 . . ? O31 C32 H32B 112.6 . . ? H32A C32 H32B 110.1 . . ? C34 C33 C32 110.1(6) . . ? C34 C33 H33A 109.6 . . ? C32 C33 H33A 109.6 . . ? C34 C33 H33B 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.2 . . ? C35' C34 C35 45.0(7) . . ? C35' C34 C33 104.3(10) . . ? C35 C34 C33 107.6(11) . . ? C35' C34 H34A 143.2 . . ? C35 C34 H34A 110.2 . . ? C33 C34 H34A 110.2 . . ? C35' C34 H34B 69.8 . . ? C35 C34 H34B 110.2 . . ? C33 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? C35' C34 H34C 110.9 . . ? C35 C34 H34C 68.1 . . ? C33 C34 H34C 110.9 . . ? H34A C34 H34C 44.3 . . ? H34B C34 H34C 137.0 . . ? C35' C34 H34D 110.9 . . ? C35 C34 H34D 139.2 . . ? C33 C34 H34D 110.9 . . ? H34A C34 H34D 68.3 . . ? H34B C34 H34D 43.0 . . ? H34C C34 H34D 108.9 . . ? C34 C35 O31 106.5(13) . . ? C34 C35 H35A 110.4 . . ? O31 C35 H35A 110.4 . . ? C34 C35 H35B 110.4 . . ? O31 C35 H35B 110.4 . . ? H35A C35 H35B 108.6 . . ? C34 C35' O31 120.4(12) . . ? C34 C35' H35C 107.2 . . ? O31 C35' H35C 107.2 . . ? C34 C35' H35D 107.2 . . ? O31 C35' H35D 107.2 . . ? H35C C35' H35D 106.9 . . ? C32A O31A C35A 107.4(4) . . ? C35" O31" C32A 115.6(9) . . ? O31" C32A O31A 40.9(4) . . ? O31" C32A C33A 106.4(5) . . ? O31A C32A C33A 109.6(4) . . ? O31" C32A H32C 140.4 . . ? O31A C32A H32C 109.8 . . ? C33A C32A H32C 109.8 . . ? O31" C32A H32D 73.2 . . ? O31A C32A H32D 109.8 . . ? C33A C32A H32D 109.8 . . ? H32C C32A H32D 108.2 . . ? O31" C32A H32E 110.5 . . ? O31A C32A H32E 71.5 . . ? C33A C32A H32E 110.5 . . ? H32C C32A H32E 40.9 . . ? H32D C32A H32E 136.3 . . ? O31" C32A H32F 110.5 . . ? O31A C32A H32F 136.6 . . ? C33A C32A H32F 110.5 . . ? H32C C32A H32F 71.1 . . ? H32D C32A H32F 39.6 . . ? H32E C32A H32F 108.6 . . ? C32A C33A C34A 104.3(4) . . ? C32A C33A H33C 110.9 . . ? C34A C33A H33C 110.9 . . ? C32A C33A H33D 110.9 . . ? C34A C33A H33D 110.9 . . ? H33C C33A H33D 108.9 . . ? C33A C34A C35" 108.4(7) . . ? C33A C34A C35A 100.5(4) . . ? C35" C34A C35A 36.0(7) . . ? C33A C34A H34E 111.7 . . ? C35" C34A H34E 133.1 . . ? C35A C34A H34E 111.7 . . ? C33A C34A H34F 111.7 . . ? C35" C34A H34F 76.3 . . ? C35A C34A H34F 111.7 . . ? H34E C34A H34F 109.4 . . ? C33A C34A H34G 110.0 . . ? C35" C34A H34G 110.0 . . ? C35A C34A H34G 80.8 . . ? H34E C34A H34G 32.3 . . ? H34F C34A H34G 132.9 . . ? C33A C34A H34H 110.0 . . ? C35" C34A H34H 110.0 . . ? C35A C34A H34H 141.8 . . ? H34E C34A H34H 78.1 . . ? H34F C34A H34H 35.6 . . ? H34G C34A H34H 108.4 . . ? O31A C35A C34A 107.3(5) . . ? O31A C35A H35E 110.2 . . ? C34A C35A H35E 110.2 . . ? O31A C35A H35F 110.2 . . ? C34A C35A H35F 110.2 . . ? H35E C35A H35F 108.5 . . ? O31" C35" C34A 102.8(11) . . ? O31" C35" H35G 111.2 . . ? C34A C35" H35G 111.2 . . ? O31" C35" H35H 111.2 . . ? C34A C35" H35H 111.2 . . ? H35G C35" H35H 109.1 . . ? 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 C21 B1 N1 C10 -124.4(3) . . . . ? C11 B1 N1 C10 123.1(2) . . . . ? C21 B1 N1 N2 55.8(2) . . . . ? C11 B1 N1 N2 -56.8(3) . . . . ? C10 N1 N2 C3 0.7(3) . . . . ? B1 N1 N2 C3 -179.4(2) . . . . ? C10 N1 N2 B2 -179.2(2) . . . . ? B1 N1 N2 B2 0.7(3) . . . . ? C22 B2 N2 C3 123.6(2) . . . . ? C12 B2 N2 C3 -123.7(2) . . . . ? C22 B2 N2 N1 -56.6(2) . . . . ? C12 B2 N2 N1 56.1(2) . . . . ? N1 N2 C3 C4 -1.7(4) . . . . ? B2 N2 C3 C4 178.1(2) . . . . ? N2 C3 C4 C5 -177.9(2) . . . . ? N2 C3 C4 C9 1.2(4) . . . . ? C9 C4 C5 C6 -0.7(4) . . . . ? C3 C4 C5 C6 178.4(3) . . . . ? C4 C5 C6 C7 1.3(5) . . . . ? C5 C6 C7 C8 -0.8(5) . . . . ? C6 C7 C8 C9 -0.4(5) . . . . ? C7 C8 C9 C10 -178.9(3) . . . . ? C7 C8 C9 C4 1.1(4) . . . . ? C5 C4 C9 C8 -0.5(4) . . . . ? C3 C4 C9 C8 -179.7(2) . . . . ? C5 C4 C9 C10 179.4(2) . . . . ? C3 C4 C9 C10 0.3(3) . . . . ? N2 N1 C10 C9 0.8(4) . . . . ? B1 N1 C10 C9 -179.0(2) . . . . ? C8 C9 C10 N1 178.7(3) . . . . ? C4 C9 C10 N1 -1.3(4) . . . . ? C21 B1 C11 C16 127.7(3) . . . . ? N1 B1 C11 C16 -124.6(3) . . . . ? C21 B1 C11 C12 -52.6(3) . . . . ? N1 B1 C11 C12 55.0(3) . . . . ? C16 C11 C12 C13 0.9(4) . . . . ? B1 C11 C12 C13 -178.8(2) . . . . ? C16 C11 C12 B2 -178.6(2) . . . . ? B1 C11 C12 B2 1.7(3) . . . . ? C22 B2 C12 C13 -129.1(3) . . . . ? N2 B2 C12 C13 123.0(3) . . . . ? C22 B2 C12 C11 50.3(3) . . . . ? N2 B2 C12 C11 -57.5(3) . . . . ? C11 C12 C13 C14 -0.8(4) . . . . ? B2 C12 C13 C14 178.7(3) . . . . ? C12 C13 C14 C15 0.0(4) . . . . ? C13 C14 C15 C16 0.7(4) . . . . ? C12 C11 C16 C15 -0.3(4) . . . . ? B1 C11 C16 C15 179.4(3) . . . . ? C14 C15 C16 C11 -0.6(4) . . . . ? C11 B1 C21 C26 -130.5(3) . . . . ? N1 B1 C21 C26 121.9(3) . . . . ? C11 B1 C21 C22 51.1(3) . . . . ? N1 B1 C21 C22 -56.6(3) . . . . ? C26 C21 C22 C23 0.8(4) . . . . ? B1 C21 C22 C23 179.3(2) . . . . ? C26 C21 C22 B2 -177.5(2) . . . . ? B1 C21 C22 B2 1.0(3) . . . . ? C12 B2 C22 C23 129.9(3) . . . . ? N2 B2 C22 C23 -122.6(3) . . . . ? C12 B2 C22 C21 -52.0(3) . . . . ? N2 B2 C22 C21 55.5(3) . . . . ? C21 C22 C23 C24 0.2(4) . . . . ? B2 C22 C23 C24 178.3(3) . . . . ? C22 C23 C24 C25 -1.5(4) . . . . ? C23 C24 C25 C26 1.8(5) . . . . ? C24 C25 C26 C21 -0.8(5) . . . . ? C22 C21 C26 C25 -0.5(4) . . . . ? B1 C21 C26 C25 -178.9(3) . . . . ? C11A B1A N1A C10A -124.0(2) . . . . ? C21A B1A N1A C10A 123.5(2) . . . . ? C11A B1A N1A N2A 56.8(2) . . . . ? C21A B1A N1A N2A -55.7(2) . . . . ? C10A N1A N2A C3A -1.4(3) . . . . ? B1A N1A N2A C3A 177.8(2) . . . . ? C10A N1A N2A B2A 179.7(2) . . . . ? B1A N1A N2A B2A -1.1(3) . . . . ? C22A B2A N2A C3A -121.0(2) . . . . ? C12A B2A N2A C3A 126.1(2) . . . . ? C22A B2A N2A N1A 57.8(2) . . . . ? C12A B2A N2A N1A -55.0(2) . . . . ? N1A N2A C3A C4A 1.7(3) . . . . ? B2A N2A C3A C4A -179.5(2) . . . . ? N2A C3A C4A C9A -0.4(3) . . . . ? N2A C3A C4A C5A 178.9(2) . . . . ? C9A C4A C5A C6A -0.9(4) . . . . ? C3A C4A C5A C6A 179.9(2) . . . . ? C4A C5A C6A C7A 0.6(4) . . . . ? C5A C6A C7A C8A -0.1(4) . . . . ? C6A C7A C8A C9A -0.2(4) . . . . ? C5A C4A C9A C8A 0.7(4) . . . . ? C3A C4A C9A C8A 179.9(2) . . . . ? C5A C4A C9A C10A 179.5(2) . . . . ? C3A C4A C9A C10A -1.2(3) . . . . ? C7A C8A C9A C4A -0.1(4) . . . . ? C7A C8A C9A C10A -178.9(2) . . . . ? N2A N1A C10A C9A -0.3(3) . . . . ? B1A N1A C10A C9A -179.4(2) . . . . ? C4A C9A C10A N1A 1.5(3) . . . . ? C8A C9A C10A N1A -179.6(2) . . . . ? C21A B1A C11A C16A -128.8(2) . . . . ? N1A B1A C11A C16A 124.3(2) . . . . ? C21A B1A C11A C12A 51.4(3) . . . . ? N1A B1A C11A C12A -55.5(2) . . . . ? C16A C11A C12A C13A -0.6(3) . . . . ? B1A C11A C12A C13A 179.3(2) . . . . ? C16A C11A C12A B2A 179.5(2) . . . . ? B1A C11A C12A B2A -0.6(3) . . . . ? C22A B2A C12A C13A 129.2(2) . . . . ? N2A B2A C12A C13A -123.9(2) . . . . ? C22A B2A C12A C11A -50.9(3) . . . . ? N2A B2A C12A C11A 56.0(3) . . . . ? C11A C12A C13A C14A 1.7(4) . . . . ? B2A C12A C13A C14A -178.4(2) . . . . ? C12A C13A C14A C15A -1.1(4) . . . . ? C13A C14A C15A C16A -0.7(4) . . . . ? C14A C15A C16A C11A 1.9(4) . . . . ? C12A C11A C16A C15A -1.2(4) . . . . ? B1A C11A C16A C15A 178.9(2) . . . . ? C11A B1A C21A C26A 129.7(2) . . . . ? N1A B1A C21A C26A -122.5(2) . . . . ? C11A B1A C21A C22A -51.3(3) . . . . ? N1A B1A C21A C22A 56.5(2) . . . . ? C26A C21A C22A C23A 1.3(3) . . . . ? B1A C21A C22A C23A -177.84(19) . . . . ? C26A C21A C22A B2A 179.0(2) . . . . ? B1A C21A C22A B2A -0.1(3) . . . . ? C12A B2A C22A C23A -131.4(2) . . . . ? N2A B2A C22A C23A 120.8(2) . . . . ? C12A B2A C22A C21A 51.1(2) . . . . ? N2A B2A C22A C21A -56.7(2) . . . . ? C21A C22A C23A C24A -0.8(3) . . . . ? B2A C22A C23A C24A -178.2(2) . . . . ? C22A C23A C24A C25A -0.1(4) . . . . ? C23A C24A C25A C26A 0.4(4) . . . . ? C22A C21A C26A C25A -0.9(4) . . . . ? B1A C21A C26A C25A 178.1(2) . . . . ? C24A C25A C26A C21A 0.1(4) . . . . ? C35' O31 C32 C33 15.8(8) . . . . ? C35 O31 C32 C33 -21.7(8) . . . . ? O31 C32 C33 C34 -0.6(7) . . . . ? C32 C33 C34 C35' -16.5(13) . . . . ? C32 C33 C34 C35 30.2(13) . . . . ? C35' C34 C35 O31 46.0(11) . . . . ? C33 C34 C35 O31 -46.8(14) . . . . ? C35' O31 C35 C34 -50.4(13) . . . . ? C32 O31 C35 C34 43.9(13) . . . . ? C35 C34 C35' O31 -67.2(15) . . . . ? C33 C34 C35' O31 33.5(17) . . . . ? C35 O31 C35' C34 59.1(14) . . . . ? C32 O31 C35' C34 -33.1(15) . . . . ? C35" O31" C32A O31A -83.6(11) . . . . ? C35" O31" C32A C33A 17.5(12) . . . . ? C35A O31A C32A O31" 78.1(7) . . . . ? C35A O31A C32A C33A -14.6(6) . . . . ? O31" C32A C33A C34A -12.5(6) . . . . ? O31A C32A C33A C34A 30.5(5) . . . . ? C32A C33A C34A C35" 4.7(10) . . . . ? C32A C33A C34A C35A -31.7(5) . . . . ? C32A O31A C35A C34A -6.6(7) . . . . ? C33A C34A C35A O31A 24.0(6) . . . . ? C35" C34A C35A O31A -82.7(12) . . . . ? C32A O31" C35" C34A -13.9(15) . . . . ? C33A C34A C35" O31" 4.8(14) . . . . ? C35A C34A C35" O31" 87.4(14) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.174 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.066 data_wa983 _database_code_depnum_ccdc_archive 'CCDC 762847' #TrackingRef 'Combined.cif' # start Validation Reply Form _vrf_PLAT201_wa983 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 11 RESPONSE: The disordered atoms of the THF molecules have been isotropically refined. ; _vrf_PLAT242_wa983 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C44 RESPONSE: This atom is not disordered, while its neighbours are disordered. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H32 Li O4, C18 H21 B2 N2 Si, C4 H8 O' _chemical_formula_sum 'C38 H61 B2 Li N2 O5 Si' _chemical_formula_weight 682.54 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' Li Li -0.0003 0.0001 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.0824(12) _cell_length_b 17.4274(15) _cell_length_c 12.4327(16) _cell_angle_alpha 90.00 _cell_angle_beta 110.322(9) _cell_angle_gamma 90.00 _cell_volume 2048.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9688 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 25.9 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9628 _exptl_absorpt_correction_T_max 0.9694 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 12751 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7065 _reflns_number_gt 5188 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.1283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(19) _refine_ls_number_reflns 7065 _refine_ls_number_parameters 444 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1706 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.77359(10) 0.43939(7) 0.47320(8) 0.0572(3) Uani 1 1 d . . . B1 B 0.3689(4) 0.5806(2) 0.0992(3) 0.0443(9) Uani 1 1 d . . . H1 H 0.456(5) 0.625(3) 0.089(4) 0.063(12) Uiso 1 1 d . . . B2 B 0.2134(4) 0.4778(2) 0.1721(3) 0.0406(8) Uani 1 1 d . . . H2 H 0.166(4) 0.428(3) 0.211(3) 0.059(11) Uiso 1 1 d . . . N1 N 0.4560(3) 0.52964(16) 0.2077(2) 0.0395(6) Uani 1 1 d . A . N2 N 0.3805(3) 0.47836(16) 0.2443(2) 0.0386(6) Uani 1 1 d . A . C3 C 0.4694(3) 0.4408(2) 0.3348(3) 0.0426(7) Uani 1 1 d . . . H3 H 0.4429 0.4013 0.3760 0.051 Uiso 1 1 calc R A . C4 C 0.6070(3) 0.4687(2) 0.3595(3) 0.0425(8) Uani 1 1 d . A . C5 C 0.5916(3) 0.5242(2) 0.2740(3) 0.0434(8) Uani 1 1 d . . . H5 H 0.6665 0.5534 0.2649 0.052 Uiso 1 1 calc R A . C6 C 0.8416(11) 0.5217(6) 0.5758(9) 0.086(3) Uiso 0.588(12) 1 d P A 1 H6A H 0.7694 0.5368 0.6080 0.128 Uiso 0.588(12) 1 calc PR A 1 H6B H 0.8630 0.5654 0.5348 0.128 Uiso 0.588(12) 1 calc PR A 1 H6C H 0.9276 0.5059 0.6379 0.128 Uiso 0.588(12) 1 calc PR A 1 C7 C 0.9126(13) 0.4274(9) 0.4116(11) 0.112(4) Uiso 0.588(12) 1 d P A 1 H7A H 1.0005 0.4119 0.4719 0.168 Uiso 0.588(12) 1 calc PR A 1 H7B H 0.9275 0.4761 0.3780 0.168 Uiso 0.588(12) 1 calc PR A 1 H7C H 0.8842 0.3879 0.3519 0.168 Uiso 0.588(12) 1 calc PR A 1 C8 C 0.7369(11) 0.3637(6) 0.5595(9) 0.087(3) Uiso 0.588(12) 1 d P A 1 H8A H 0.6670 0.3819 0.5921 0.130 Uiso 0.588(12) 1 calc PR A 1 H8B H 0.8244 0.3498 0.6217 0.130 Uiso 0.588(12) 1 calc PR A 1 H8C H 0.6996 0.3187 0.5113 0.130 Uiso 0.588(12) 1 calc PR A 1 C6' C 0.889(2) 0.5200(13) 0.5212(19) 0.121(6) Uiso 0.412(12) 1 d P A 2 H6'1 H 0.9757 0.5037 0.5823 0.181 Uiso 0.412(12) 1 calc PR A 2 H6'2 H 0.8417 0.5596 0.5507 0.181 Uiso 0.412(12) 1 calc PR A 2 H6'3 H 0.9129 0.5407 0.4570 0.181 Uiso 0.412(12) 1 calc PR A 2 C7' C 0.8749(19) 0.3747(12) 0.4149(15) 0.105(5) Uiso 0.412(12) 1 d P A 2 H7'1 H 0.8272 0.3248 0.3978 0.157 Uiso 0.412(12) 1 calc PR A 2 H7'2 H 0.9701 0.3679 0.4714 0.157 Uiso 0.412(12) 1 calc PR A 2 H7'3 H 0.8816 0.3967 0.3445 0.157 Uiso 0.412(12) 1 calc PR A 2 C8' C 0.756(3) 0.4386(17) 0.616(2) 0.155(9) Uiso 0.412(12) 1 d P A 2 H8'1 H 0.6769 0.4055 0.6146 0.233 Uiso 0.412(12) 1 calc PR A 2 H8'2 H 0.7388 0.4909 0.6372 0.233 Uiso 0.412(12) 1 calc PR A 2 H8'3 H 0.8436 0.4189 0.6730 0.233 Uiso 0.412(12) 1 calc PR A 2 C11 C 0.2889(3) 0.51756(19) 0.0040(3) 0.0391(7) Uani 1 1 d . . . C12 C 0.2058(3) 0.46447(17) 0.0408(3) 0.0368(7) Uani 1 1 d . . . C13 C 0.1288(3) 0.4102(2) -0.0367(3) 0.0438(8) Uani 1 1 d . . . H13 H 0.0733 0.3743 -0.0130 0.053 Uiso 1 1 calc R . . C14 C 0.1296(4) 0.4062(2) -0.1477(3) 0.0492(9) Uani 1 1 d . . . H14 H 0.0728 0.3692 -0.1994 0.059 Uiso 1 1 calc R . . C15 C 0.2115(4) 0.4552(2) -0.1830(3) 0.0516(9) Uani 1 1 d . . . H15 H 0.2150 0.4512 -0.2582 0.062 Uiso 1 1 calc R . . C16 C 0.2914(4) 0.5121(2) -0.1066(3) 0.0468(8) Uani 1 1 d . . . H16 H 0.3474 0.5470 -0.1313 0.056 Uiso 1 1 calc R . . C21 C 0.2495(4) 0.6194(2) 0.1397(3) 0.0465(9) Uani 1 1 d . . . C22 C 0.1686(3) 0.5666(2) 0.1779(3) 0.0477(9) Uani 1 1 d . . . C23 C 0.0596(4) 0.5940(3) 0.2126(3) 0.0609(11) Uani 1 1 d . . . H23 H 0.0037 0.5594 0.2378 0.073 Uiso 1 1 calc R . . C24 C 0.0327(5) 0.6755(3) 0.2096(4) 0.0801(18) Uani 1 1 d . . . H24 H -0.0409 0.6949 0.2332 0.096 Uiso 1 1 calc R . . C25 C 0.1139(6) 0.7247(3) 0.1726(4) 0.0748(15) Uani 1 1 d . . . H25 H 0.0954 0.7782 0.1698 0.090 Uiso 1 1 calc R . . C26 C 0.2208(4) 0.6977(2) 0.1398(3) 0.0584(11) Uani 1 1 d . . . H26 H 0.2772 0.7331 0.1163 0.070 Uiso 1 1 calc R . . Li1 Li 0.6552(7) 0.6258(4) 0.7887(5) 0.0502(14) Uani 1 1 d . B . O31 O 0.5755(3) 0.70893(17) 0.8447(3) 0.0677(9) Uani 1 1 d . . . C32 C 0.6331(10) 0.7408(6) 0.9671(10) 0.068(3) Uiso 0.497(15) 1 d P B 1 H32A H 0.6293 0.7014 1.0233 0.082 Uiso 0.497(15) 1 calc PR B 1 H32B H 0.7322 0.7582 0.9865 0.082 Uiso 0.497(15) 1 calc PR B 1 C32' C 0.6585(8) 0.7669(5) 0.9178(8) 0.050(3) Uiso 0.503(15) 1 d P B 2 H32C H 0.6918 0.8055 0.8745 0.060 Uiso 0.503(15) 1 calc PR B 2 H32D H 0.7406 0.7450 0.9797 0.060 Uiso 0.503(15) 1 calc PR B 2 C33 C 0.5449(6) 0.8019(4) 0.9663(6) 0.108(2) Uani 1 1 d . . . H33A H 0.5941 0.8508 0.9639 0.129 Uiso 0.497(15) 1 calc PR B 1 H33B H 0.5219 0.8014 1.0375 0.129 Uiso 0.497(15) 1 calc PR B 1 H33C H 0.5382 0.7712 1.0312 0.129 Uiso 0.503(15) 1 calc PR B 2 H33D H 0.5679 0.8557 0.9915 0.129 Uiso 0.503(15) 1 calc PR B 2 C34 C 0.4182(6) 0.7974(4) 0.8696(6) 0.110(2) Uani 1 1 d . B . H34A H 0.3954 0.8485 0.8330 0.132 Uiso 0.497(15) 1 calc PR B 1 H34B H 0.3391 0.7815 0.8945 0.132 Uiso 0.497(15) 1 calc PR B 1 H34C H 0.4148 0.8378 0.8127 0.132 Uiso 0.503(15) 1 calc PR B 2 H34D H 0.3337 0.8019 0.8924 0.132 Uiso 0.503(15) 1 calc PR B 2 C35 C 0.4351(10) 0.7418(7) 0.7867(11) 0.064(3) Uiso 0.497(15) 1 d P B 1 H35A H 0.3611 0.7016 0.7693 0.077 Uiso 0.497(15) 1 calc PR B 1 H35B H 0.4303 0.7674 0.7144 0.077 Uiso 0.497(15) 1 calc PR B 1 C35' C 0.4290(8) 0.7184(6) 0.8231(9) 0.053(2) Uiso 0.503(15) 1 d P B 2 H35C H 0.3936 0.6787 0.8634 0.064 Uiso 0.503(15) 1 calc PR B 2 H35D H 0.3743 0.7156 0.7400 0.064 Uiso 0.503(15) 1 calc PR B 2 O41 O 0.6822(3) 0.53672(16) 0.8847(2) 0.0624(8) Uani 1 1 d . . . C42 C 0.629(2) 0.4615(10) 0.8516(14) 0.106(6) Uiso 0.433(13) 1 d P B 1 H42A H 0.6301 0.4479 0.7747 0.127 Uiso 0.433(13) 1 calc PR B 1 H42B H 0.5313 0.4558 0.8524 0.127 Uiso 0.433(13) 1 calc PR B 1 C42' C 0.7305(8) 0.4626(4) 0.8556(6) 0.052(2) Uiso 0.567(13) 1 d P B 2 H42C H 0.6632 0.4428 0.7824 0.063 Uiso 0.567(13) 1 calc PR B 2 H42D H 0.8248 0.4677 0.8485 0.063 Uiso 0.567(13) 1 calc PR B 2 C43 C 0.7367(7) 0.4128(4) 0.9477(6) 0.0988(18) Uani 1 1 d . . . H43A H 0.6882 0.3686 0.9678 0.119 Uiso 0.433(13) 1 calc PR B 1 H43B H 0.8116 0.3930 0.9207 0.119 Uiso 0.433(13) 1 calc PR B 1 H43C H 0.8277 0.3847 0.9747 0.119 Uiso 0.567(13) 1 calc PR B 2 H43D H 0.6585 0.3751 0.9234 0.119 Uiso 0.567(13) 1 calc PR B 2 C44 C 0.7940(8) 0.4579(4) 1.0401(6) 0.035(2) Uiso 0.433(13) 1 d P B 1 H44A H 0.8968 0.4641 1.0571 0.042 Uiso 0.433(13) 1 calc PR B 1 H44B H 0.7788 0.4356 1.1082 0.042 Uiso 0.433(13) 1 calc PR B 1 C44' C 0.7215(16) 0.4700(7) 1.0525(11) 0.101(4) Uiso 0.567(13) 1 d P B 2 H44C H 0.6358 0.4574 1.0705 0.121 Uiso 0.567(13) 1 calc PR B 2 H44D H 0.8056 0.4658 1.1233 0.121 Uiso 0.567(13) 1 calc PR B 2 C45 C 0.7119(6) 0.5405(3) 1.0055(4) 0.0735(13) Uani 1 1 d . B . H45A H 0.6246 0.5426 1.0248 0.088 Uiso 0.433(13) 1 calc PR B 1 H45B H 0.7739 0.5844 1.0413 0.088 Uiso 0.433(13) 1 calc PR B 1 H45C H 0.8020 0.5683 1.0421 0.088 Uiso 0.567(13) 1 calc PR B 2 H45D H 0.6360 0.5697 1.0206 0.088 Uiso 0.567(13) 1 calc PR B 2 O51 O 0.5235(3) 0.60012(17) 0.6392(2) 0.0595(8) Uani 1 1 d . . . C52 C 0.4294(10) 0.5364(5) 0.6084(6) 0.044(2) Uiso 0.53(2) 1 d P B 1 H52A H 0.4053 0.5174 0.6745 0.053 Uiso 0.53(2) 1 calc PR B 1 H52B H 0.4689 0.4938 0.5764 0.053 Uiso 0.53(2) 1 calc PR B 1 C52' C 0.3896(16) 0.5574(10) 0.6190(11) 0.078(4) Uiso 0.47(2) 1 d P B 2 H52C H 0.4086 0.5015 0.6240 0.093 Uiso 0.47(2) 1 calc PR B 2 H52D H 0.3492 0.5712 0.6784 0.093 Uiso 0.47(2) 1 calc PR B 2 C53 C 0.2952(6) 0.5752(5) 0.5125(5) 0.110(2) Uani 1 1 d . . . H53A H 0.2557 0.5397 0.4470 0.131 Uiso 0.53(2) 1 calc PR B 1 H53B H 0.2207 0.5864 0.5452 0.131 Uiso 0.53(2) 1 calc PR B 1 H53C H 0.2130 0.6032 0.5191 0.131 Uiso 0.47(2) 1 calc PR B 2 H53D H 0.2610 0.5281 0.4668 0.131 Uiso 0.47(2) 1 calc PR B 2 C54 C 0.3355(13) 0.6381(6) 0.4781(10) 0.069(3) Uiso 0.53(2) 1 d P B 1 H54A H 0.2881 0.6826 0.4986 0.082 Uiso 0.53(2) 1 calc PR B 1 H54B H 0.3104 0.6372 0.3937 0.082 Uiso 0.53(2) 1 calc PR B 1 C54' C 0.3858(13) 0.6312(6) 0.4509(9) 0.062(3) Uiso 0.47(2) 1 d P B 2 H54C H 0.4061 0.6037 0.3886 0.074 Uiso 0.47(2) 1 calc PR B 2 H54D H 0.3339 0.6792 0.4201 0.074 Uiso 0.47(2) 1 calc PR B 2 C55 C 0.5031(5) 0.6450(4) 0.5392(4) 0.0801(15) Uani 1 1 d . B . H55A H 0.5541 0.6231 0.4911 0.096 Uiso 0.53(2) 1 calc PR B 1 H55B H 0.5331 0.6988 0.5585 0.096 Uiso 0.53(2) 1 calc PR B 1 H55C H 0.5035 0.6998 0.5602 0.096 Uiso 0.47(2) 1 calc PR B 2 H55D H 0.5850 0.6366 0.5140 0.096 Uiso 0.47(2) 1 calc PR B 2 O61 O 0.8356(3) 0.65986(17) 0.7916(2) 0.0602(8) Uani 1 1 d . . . C62 C 0.9720(4) 0.6287(3) 0.8585(4) 0.0714(13) Uani 1 1 d . B . H62A H 0.9803 0.5746 0.8372 0.086 Uiso 1 1 calc R . . H62B H 0.9874 0.6312 0.9415 0.086 Uiso 1 1 calc R . . C63 C 1.0754(5) 0.6782(4) 0.8295(6) 0.0904(18) Uani 1 1 d . . . H63A H 1.0869 0.6617 0.7571 0.108 Uiso 0.57(2) 1 calc PR B 1 H63B H 1.1688 0.6780 0.8917 0.108 Uiso 0.57(2) 1 calc PR B 1 H63C H 1.1511 0.6946 0.9008 0.108 Uiso 0.43(2) 1 calc PR B 2 H63D H 1.1195 0.6488 0.7826 0.108 Uiso 0.43(2) 1 calc PR B 2 C64 C 1.0059(8) 0.7562(6) 0.8170(10) 0.062(3) Uiso 0.57(2) 1 d P B 1 H64A H 1.0279 0.7812 0.8927 0.074 Uiso 0.57(2) 1 calc PR B 1 H64B H 1.0380 0.7898 0.7667 0.074 Uiso 0.57(2) 1 calc PR B 1 C65 C 0.8533(11) 0.7400(8) 0.7650(15) 0.084(4) Uiso 0.57(2) 1 d P B 1 H65A H 0.7985 0.7741 0.7978 0.101 Uiso 0.57(2) 1 calc PR B 1 H65B H 0.8205 0.7480 0.6810 0.101 Uiso 0.57(2) 1 calc PR B 1 C64' C 1.0096(16) 0.7393(11) 0.772(2) 0.091(5) Uiso 0.43(2) 1 d P B 2 H64C H 1.0471 0.7521 0.7100 0.110 Uiso 0.43(2) 1 calc PR B 2 H64D H 1.0239 0.7840 0.8235 0.110 Uiso 0.43(2) 1 calc PR B 2 C65' C 0.8565(10) 0.7200(7) 0.7215(11) 0.050(3) Uiso 0.43(2) 1 d P B 2 H65C H 0.7976 0.7651 0.7233 0.060 Uiso 0.43(2) 1 calc PR B 2 H65D H 0.8317 0.7027 0.6411 0.060 Uiso 0.43(2) 1 calc PR B 2 O71 O 0.3994(5) 0.3237(3) 0.5556(4) 0.1176(16) Uani 1 1 d . . . C72 C 0.418(2) 0.3055(13) 0.701(2) 0.083(7) Uiso 0.32(3) 1 d P C 1 H72A H 0.5173 0.2931 0.7488 0.100 Uiso 0.32(3) 1 calc PR C 1 H72B H 0.3840 0.3488 0.7359 0.100 Uiso 0.32(3) 1 calc PR C 1 C72' C 0.4553(12) 0.2916(6) 0.6621(10) 0.085(4) Uiso 0.68(3) 1 d P C 2 H72C H 0.4920 0.3321 0.7208 0.102 Uiso 0.68(3) 1 calc PR C 2 H72D H 0.5342 0.2568 0.6653 0.102 Uiso 0.68(3) 1 calc PR C 2 C73 C 0.3371(11) 0.2467(5) 0.6847(9) 0.149(4) Uani 1 1 d . . . H73A H 0.3174 0.2328 0.7549 0.178 Uiso 0.32(3) 1 calc PR C 1 H73B H 0.3781 0.2018 0.6586 0.178 Uiso 0.32(3) 1 calc PR C 1 H73C H 0.3491 0.1907 0.6779 0.178 Uiso 0.68(3) 1 calc PR C 2 H73D H 0.3341 0.2581 0.7618 0.178 Uiso 0.68(3) 1 calc PR C 2 C74 C 0.2090(8) 0.2746(5) 0.5939(6) 0.116(2) Uani 1 1 d . C . H74A H 0.1641 0.2332 0.5389 0.139 Uiso 1 1 calc R . . H74B H 0.1396 0.2946 0.6270 0.139 Uiso 1 1 calc R . . C75 C 0.2602(6) 0.3356(4) 0.5384(5) 0.0836(15) Uani 1 1 d . C . H75A H 0.2051 0.3361 0.4552 0.100 Uiso 1 1 calc R . . H75B H 0.2479 0.3859 0.5708 0.100 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 Si1 0.0426(5) 0.0786(8) 0.0383(5) 0.0051(5) -0.0012(4) 0.0214(5) B1 0.049(2) 0.0338(19) 0.0376(19) 0.0100(16) -0.0007(16) 0.0022(17) B2 0.0352(17) 0.042(2) 0.0394(18) 0.0028(16) 0.0061(14) 0.0004(15) N1 0.0350(13) 0.0376(15) 0.0377(14) 0.0029(12) 0.0023(11) 0.0013(11) N2 0.0363(13) 0.0397(15) 0.0356(13) 0.0072(11) 0.0071(11) 0.0072(12) C3 0.0455(16) 0.0441(19) 0.0352(14) 0.0052(15) 0.0102(13) 0.0127(16) C4 0.0378(15) 0.053(2) 0.0326(15) 0.0023(14) 0.0070(13) 0.0069(14) C5 0.0341(15) 0.048(2) 0.0396(16) -0.0027(15) 0.0020(13) -0.0015(14) C11 0.0372(15) 0.0345(17) 0.0368(15) 0.0049(13) 0.0018(12) 0.0027(13) C12 0.0335(14) 0.0285(16) 0.0448(17) 0.0003(13) 0.0090(13) 0.0046(12) C13 0.0401(16) 0.0381(18) 0.0493(19) -0.0040(15) 0.0106(14) -0.0032(14) C14 0.0464(18) 0.045(2) 0.0480(19) -0.0125(16) 0.0062(15) -0.0061(16) C15 0.0523(19) 0.059(2) 0.0380(16) -0.0065(16) 0.0086(14) 0.0034(18) C16 0.0491(18) 0.044(2) 0.0407(17) 0.0032(15) 0.0074(14) -0.0007(15) C21 0.0493(19) 0.0384(19) 0.0342(16) -0.0065(14) -0.0078(14) 0.0057(15) C22 0.0387(16) 0.056(2) 0.0350(16) -0.0099(15) -0.0038(13) 0.0122(15) C23 0.0376(17) 0.080(3) 0.051(2) -0.021(2) -0.0024(15) 0.0140(19) C24 0.059(2) 0.099(4) 0.060(3) -0.030(3) -0.007(2) 0.043(3) C25 0.077(3) 0.058(3) 0.066(3) -0.016(2) -0.006(2) 0.018(3) C26 0.067(2) 0.037(2) 0.049(2) -0.0050(16) -0.0073(18) 0.0102(18) Li1 0.051(3) 0.045(3) 0.045(3) 0.005(3) 0.005(3) -0.001(3) O31 0.0493(14) 0.0507(17) 0.088(2) -0.0217(15) 0.0050(14) 0.0048(12) C33 0.076(3) 0.101(5) 0.128(5) -0.061(4) 0.013(3) -0.002(3) C34 0.072(3) 0.128(6) 0.114(5) -0.048(4) 0.013(3) 0.024(3) O41 0.088(2) 0.0467(16) 0.0438(13) 0.0064(12) 0.0116(13) 0.0037(14) C43 0.114(4) 0.073(4) 0.117(5) 0.029(3) 0.050(4) 0.022(3) C45 0.082(3) 0.082(3) 0.047(2) 0.004(2) 0.012(2) -0.003(2) O51 0.0550(14) 0.073(2) 0.0396(13) 0.0069(12) 0.0030(11) -0.0176(13) C53 0.062(3) 0.169(7) 0.079(4) -0.024(4) 0.000(3) -0.009(4) C55 0.079(3) 0.110(4) 0.047(2) 0.029(3) 0.016(2) 0.011(3) O61 0.0415(13) 0.0627(17) 0.0639(16) 0.0181(14) 0.0026(12) 0.0013(12) C62 0.042(2) 0.085(3) 0.075(3) 0.023(2) 0.0047(19) 0.004(2) C63 0.050(2) 0.111(4) 0.102(4) 0.036(3) 0.015(2) -0.002(3) O71 0.087(3) 0.147(4) 0.110(3) 0.035(3) 0.024(2) 0.009(3) C73 0.191(9) 0.108(6) 0.147(8) 0.058(5) 0.059(7) 0.044(6) C74 0.113(5) 0.140(6) 0.098(4) 0.002(5) 0.041(4) -0.023(5) C75 0.073(3) 0.097(4) 0.078(3) -0.011(3) 0.024(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C6' 1.79(2) . ? Si1 C8 1.817(11) . ? Si1 C7 1.827(13) . ? Si1 C7' 1.831(18) . ? Si1 C8' 1.85(2) . ? Si1 C4 1.852(3) . ? Si1 C6 1.884(11) . ? B1 N1 1.599(4) . ? B1 C21 1.607(6) . ? B1 C11 1.611(5) . ? B1 H1 1.21(5) . ? B2 N2 1.610(4) . ? B2 C22 1.620(5) . ? B2 C12 1.624(5) . ? B2 H2 1.17(4) . ? N1 C5 1.332(4) . ? N1 N2 1.352(4) . ? N2 C3 1.340(4) . ? C3 C4 1.400(5) . ? C3 H3 0.9500 . ? C4 C5 1.405(5) . ? C5 H5 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C6' H6'1 0.9800 . ? C6' H6'2 0.9800 . ? C6' H6'3 0.9800 . ? C7' H7'1 0.9800 . ? C7' H7'2 0.9800 . ? C7' H7'3 0.9800 . ? C8' H8'1 0.9800 . ? C8' H8'2 0.9800 . ? C8' H8'3 0.9800 . ? C11 C16 1.386(5) . ? C11 C12 1.426(5) . ? C12 C13 1.381(5) . ? C13 C14 1.385(5) . ? C13 H13 0.9500 . ? C14 C15 1.363(6) . ? C14 H14 0.9500 . ? C15 C16 1.416(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.395(5) . ? C21 C22 1.417(6) . ? C22 C23 1.397(6) . ? C23 C24 1.444(7) . ? C23 H23 0.9500 . ? C24 C25 1.371(8) . ? C24 H24 0.9500 . ? C25 C26 1.361(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? Li1 O61 1.902(7) . ? Li1 O31 1.902(7) . ? Li1 O41 1.918(7) . ? Li1 O51 1.925(6) . ? O31 C35' 1.417(9) . ? O31 C32' 1.420(8) . ? O31 C35 1.464(10) . ? O31 C32 1.532(11) . ? C32 C33 1.386(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32' C33 1.589(11) . ? C32' H32C 0.9900 . ? C32' H32D 0.9900 . ? C33 C34 1.420(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 H33C 0.9900 . ? C33 H33D 0.9900 . ? C34 C35 1.467(12) . ? C34 C35' 1.511(11) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 H34C 0.9900 . ? C34 H34D 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35' H35C 0.9900 . ? C35' H35D 0.9900 . ? O41 C42 1.423(17) . ? O41 C45 1.427(5) . ? O41 C42' 1.469(8) . ? C42 C43 1.559(17) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42' C43 1.420(9) . ? C42' H42C 0.9900 . ? C42' H42D 0.9900 . ? C43 C44 1.344(10) . ? C43 C44' 1.689(15) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 H43C 0.9900 . ? C43 H43D 0.9900 . ? C44 C45 1.642(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44' C45 1.350(13) . ? C44' H44C 0.9900 . ? C44' H44D 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 H45C 0.9900 . ? C45 H45D 0.9900 . ? O51 C55 1.422(5) . ? O51 C52 1.424(8) . ? O51 C52' 1.484(13) . ? C52 C53 1.609(10) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C52' C53 1.371(13) . ? C52' H52C 0.9900 . ? C52' H52D 0.9900 . ? C53 C54 1.292(13) . ? C53 C54' 1.691(15) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C53 H53C 0.9900 . ? C53 H53D 0.9900 . ? C54 C55 1.599(13) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C54' C55 1.327(10) . ? C54' H54C 0.9900 . ? C54' H54D 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C55 H55C 0.9900 . ? C55 H55D 0.9900 . ? O61 C65' 1.424(10) . ? O61 C62 1.444(5) . ? O61 C65 1.460(12) . ? C62 C63 1.490(7) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64' 1.327(17) . ? C63 C64 1.512(11) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C63 H63C 0.9900 . ? C63 H63D 0.9900 . ? C64 C65 1.475(13) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C64' C65' 1.488(18) . ? C64' H64C 0.9900 . ? C64' H64D 0.9900 . ? C65' H65C 0.9900 . ? C65' H65D 0.9900 . ? O71 C75 1.361(7) . ? O71 C72' 1.366(11) . ? O71 C72 1.78(3) . ? C72 C73 1.28(2) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C72' C73 1.531(16) . ? C72' H72C 0.9900 . ? C72' H72D 0.9900 . ? C73 C74 1.472(11) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C73 H73C 0.9900 . ? C73 H73D 0.9900 . ? C74 C75 1.456(9) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? 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 C8 Si1 C7 120.5(6) . . ? C6' Si1 C7' 103.2(10) . . ? C6' Si1 C8' 87.3(12) . . ? C7' Si1 C8' 129.0(11) . . ? C6' Si1 C4 110.5(7) . . ? C8 Si1 C4 109.5(3) . . ? C7 Si1 C4 109.6(4) . . ? C7' Si1 C4 110.5(6) . . ? C8' Si1 C4 111.9(8) . . ? C8 Si1 C6 104.7(5) . . ? C7 Si1 C6 102.6(6) . . ? C4 Si1 C6 109.1(3) . . ? N1 B1 C21 102.8(3) . . ? N1 B1 C11 103.3(3) . . ? C21 B1 C11 106.2(3) . . ? N1 B1 H1 104(2) . . ? C21 B1 H1 114(2) . . ? C11 B1 H1 124(2) . . ? N2 B2 C22 103.0(3) . . ? N2 B2 C12 103.7(3) . . ? C22 B2 C12 105.4(3) . . ? N2 B2 H2 105.6(19) . . ? C22 B2 H2 122(2) . . ? C12 B2 H2 115(2) . . ? C5 N1 N2 108.7(3) . . ? C5 N1 B1 135.0(3) . . ? N2 N1 B1 116.3(2) . . ? C3 N2 N1 108.4(3) . . ? C3 N2 B2 136.9(3) . . ? N1 N2 B2 114.7(2) . . ? N2 C3 C4 109.7(3) . . ? N2 C3 H3 125.1 . . ? C4 C3 H3 125.1 . . ? C3 C4 C5 103.4(3) . . ? C3 C4 Si1 129.7(3) . . ? C5 C4 Si1 126.9(3) . . ? N1 C5 C4 109.8(3) . . ? N1 C5 H5 125.1 . . ? C4 C5 H5 125.1 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C6' H6'1 109.5 . . ? Si1 C6' H6'2 109.5 . . ? H6'1 C6' H6'2 109.5 . . ? Si1 C6' H6'3 109.5 . . ? H6'1 C6' H6'3 109.5 . . ? H6'2 C6' H6'3 109.5 . . ? Si1 C7' H7'1 109.5 . . ? Si1 C7' H7'2 109.5 . . ? H7'1 C7' H7'2 109.5 . . ? Si1 C7' H7'3 109.5 . . ? H7'1 C7' H7'3 109.5 . . ? H7'2 C7' H7'3 109.5 . . ? Si1 C8' H8'1 109.5 . . ? Si1 C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? Si1 C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C16 C11 C12 119.2(3) . . ? C16 C11 B1 126.8(3) . . ? C12 C11 B1 114.0(3) . . ? C13 C12 C11 118.2(3) . . ? C13 C12 B2 128.2(3) . . ? C11 C12 B2 113.7(3) . . ? C12 C13 C14 122.2(3) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.3(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C11 C16 C15 120.8(3) . . ? C11 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C26 C21 C22 119.5(4) . . ? C26 C21 B1 126.2(4) . . ? C22 C21 B1 114.4(3) . . ? C23 C22 C21 119.2(4) . . ? C23 C22 B2 127.0(4) . . ? C21 C22 B2 113.8(3) . . ? C22 C23 C24 119.3(5) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 119.7(4) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 120.8(4) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C21 121.6(5) . . ? C25 C26 H26 119.2 . . ? C21 C26 H26 119.2 . . ? O61 Li1 O31 106.1(3) . . ? O61 Li1 O41 108.2(3) . . ? O31 Li1 O41 112.1(4) . . ? O61 Li1 O51 115.1(4) . . ? O31 Li1 O51 107.0(3) . . ? O41 Li1 O51 108.3(3) . . ? C35' O31 C32' 112.4(5) . . ? C32' O31 C35 106.9(5) . . ? C35' O31 C32 99.0(6) . . ? C35 O31 C32 108.4(6) . . ? C35' O31 Li1 124.4(4) . . ? C32' O31 Li1 123.1(4) . . ? C35 O31 Li1 125.2(5) . . ? C32 O31 Li1 125.2(4) . . ? C33 C32 O31 104.5(7) . . ? C33 C32 H32A 110.9 . . ? O31 C32 H32A 110.9 . . ? C33 C32 H32B 110.9 . . ? O31 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? O31 C32' C33 100.0(5) . . ? O31 C32' H32C 111.8 . . ? C33 C32' H32C 111.8 . . ? O31 C32' H32D 111.8 . . ? C33 C32' H32D 111.8 . . ? H32C C32' H32D 109.5 . . ? C32 C33 C34 110.5(6) . . ? C34 C33 C32' 102.3(5) . . ? C32 C33 H33A 109.6 . . ? C34 C33 H33A 109.6 . . ? C32 C33 H33B 109.6 . . ? C34 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? C34 C33 H33C 111.3 . . ? C32' C33 H33C 111.3 . . ? C32 C33 H33D 130.3 . . ? C34 C33 H33D 111.3 . . ? C32' C33 H33D 111.3 . . ? H33C C33 H33D 109.2 . . ? C33 C34 C35 110.0(6) . . ? C33 C34 C35' 102.2(6) . . ? C33 C34 H34A 109.7 . . ? C35 C34 H34A 109.7 . . ? C33 C34 H34B 109.7 . . ? C35 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? C35' C34 H34C 111.3 . . ? C33 C34 H34D 111.3 . . ? C35 C34 H34D 125.0 . . ? C35' C34 H34D 111.3 . . ? H34C C34 H34D 109.2 . . ? O31 C35 C34 103.9(7) . . ? O31 C35 H35A 111.0 . . ? C34 C35 H35A 111.0 . . ? O31 C35 H35B 111.0 . . ? C34 C35 H35B 111.0 . . ? H35A C35 H35B 109.0 . . ? O31 C35' C34 104.0(6) . . ? O31 C35' H35C 110.9 . . ? C34 C35' H35C 110.9 . . ? O31 C35' H35D 110.9 . . ? C34 C35' H35D 110.9 . . ? H35C C35' H35D 109.0 . . ? C42 O41 C45 105.5(7) . . ? C45 O41 C42' 109.5(4) . . ? C42 O41 Li1 127.4(7) . . ? C45 O41 Li1 123.3(3) . . ? C42' O41 Li1 123.1(4) . . ? O41 C42 C43 100.7(11) . . ? O41 C42 H42A 111.6 . . ? C43 C42 H42A 111.6 . . ? O41 C42 H42B 111.6 . . ? C43 C42 H42B 111.6 . . ? H42A C42 H42B 109.4 . . ? C43 C42' O41 105.3(5) . . ? C43 C42' H42C 110.7 . . ? O41 C42' H42C 110.7 . . ? C43 C42' H42D 110.7 . . ? O41 C42' H42D 110.7 . . ? H42C C42' H42D 108.8 . . ? C44 C43 C42' 102.6(6) . . ? C44 C43 C42 108.4(8) . . ? C42' C43 C44' 105.8(6) . . ? C42 C43 C44' 92.5(9) . . ? C44 C43 H43A 110.0 . . ? C42 C43 H43A 110.0 . . ? C44 C43 H43B 110.0 . . ? C42 C43 H43B 110.0 . . ? H43A C43 H43B 108.4 . . ? C44 C43 H43C 85.8 . . ? C42' C43 H43C 110.6 . . ? C44' C43 H43C 110.6 . . ? C42' C43 H43D 110.6 . . ? C44' C43 H43D 110.6 . . ? H43B C43 H43D 106.6 . . ? H43C C43 H43D 108.7 . . ? C43 C44 C45 105.1(5) . . ? C43 C44 H44A 110.7 . . ? C45 C44 H44A 110.7 . . ? C43 C44 H44B 110.7 . . ? C45 C44 H44B 110.7 . . ? H44A C44 H44B 108.8 . . ? C45 C44' C43 102.4(9) . . ? C45 C44' H44C 111.3 . . ? C43 C44' H44C 111.3 . . ? C45 C44' H44D 111.3 . . ? C43 C44' H44D 111.3 . . ? H44C C44' H44D 109.2 . . ? C44' C45 O41 111.8(7) . . ? O41 C45 C44 97.9(4) . . ? O41 C45 H45A 112.2 . . ? C44 C45 H45A 112.2 . . ? O41 C45 H45B 112.2 . . ? C44 C45 H45B 112.2 . . ? H45A C45 H45B 109.8 . . ? C44' C45 H45C 109.3 . . ? O41 C45 H45C 109.3 . . ? H45A C45 H45C 128.5 . . ? C44' C45 H45D 109.3 . . ? O41 C45 H45D 109.3 . . ? C44 C45 H45D 138.9 . . ? H45C C45 H45D 107.9 . . ? C55 O51 C52 108.2(4) . . ? C55 O51 C52' 106.3(5) . . ? C55 O51 Li1 124.0(4) . . ? C52 O51 Li1 127.8(4) . . ? C52' O51 Li1 124.2(6) . . ? O51 C52 C53 100.4(6) . . ? O51 C52 H52A 111.7 . . ? C53 C52 H52A 111.7 . . ? O51 C52 H52B 111.7 . . ? C53 C52 H52B 111.7 . . ? H52A C52 H52B 109.5 . . ? C53 C52' O51 109.6(9) . . ? C53 C52' H52C 109.7 . . ? O51 C52' H52C 109.7 . . ? C53 C52' H52D 109.7 . . ? O51 C52' H52D 109.7 . . ? H52C C52' H52D 108.2 . . ? C54 C53 C52' 108.6(8) . . ? C54 C53 C52 108.8(6) . . ? C52' C53 C54' 105.4(7) . . ? C52 C53 C54' 97.6(5) . . ? C54 C53 H53A 109.9 . . ? C52 C53 H53A 109.9 . . ? C54' C53 H53A 96.6 . . ? C54 C53 H53B 109.9 . . ? C52 C53 H53B 109.9 . . ? C54' C53 H53B 132.8 . . ? H53A C53 H53B 108.3 . . ? C52' C53 H53C 110.7 . . ? C54' C53 H53C 110.7 . . ? H53A C53 H53C 105.5 . . ? C52' C53 H53D 110.7 . . ? C54' C53 H53D 110.7 . . ? H53B C53 H53D 103.6 . . ? H53C C53 H53D 108.8 . . ? C53 C54 C55 107.9(7) . . ? C53 C54 H54A 110.1 . . ? C55 C54 H54A 110.1 . . ? C53 C54 H54B 110.1 . . ? C55 C54 H54B 110.1 . . ? H54A C54 H54B 108.4 . . ? C55 C54' C53 101.3(7) . . ? C55 C54' H54C 111.5 . . ? C53 C54' H54C 111.5 . . ? C55 C54' H54D 111.5 . . ? C53 C54' H54D 111.5 . . ? H54C C54' H54D 109.3 . . ? C54' C55 O51 116.1(7) . . ? O51 C55 C54 100.5(6) . . ? O51 C55 H55A 111.7 . . ? C54 C55 H55A 111.7 . . ? O51 C55 H55B 111.7 . . ? C54 C55 H55B 111.7 . . ? H55A C55 H55B 109.4 . . ? C54' C55 H55C 108.3 . . ? O51 C55 H55C 108.3 . . ? C54' C55 H55D 108.3 . . ? O51 C55 H55D 108.3 . . ? C54 C55 H55D 134.3 . . ? H55C C55 H55D 107.4 . . ? C65' O61 C62 108.4(4) . . ? C62 O61 C65 108.9(5) . . ? C65' O61 Li1 124.2(4) . . ? C62 O61 Li1 127.3(3) . . ? C65 O61 Li1 119.0(5) . . ? O61 C62 C63 104.4(4) . . ? O61 C62 H62A 110.9 . . ? C63 C62 H62A 110.9 . . ? O61 C62 H62B 110.9 . . ? C63 C62 H62B 110.9 . . ? H62A C62 H62B 108.9 . . ? C64' C63 C62 109.6(8) . . ? C62 C63 C64 102.0(5) . . ? C64' C63 H63A 86.3 . . ? C62 C63 H63A 111.4 . . ? C64 C63 H63A 111.4 . . ? C64' C63 H63B 126.0 . . ? C62 C63 H63B 111.4 . . ? C64 C63 H63B 111.4 . . ? H63A C63 H63B 109.2 . . ? C64' C63 H63C 109.7 . . ? C62 C63 H63C 109.7 . . ? C64' C63 H63D 109.7 . . ? C62 C63 H63D 109.7 . . ? C64 C63 H63D 133.7 . . ? H63C C63 H63D 108.2 . . ? C65 C64 C63 104.4(7) . . ? C65 C64 H64A 110.9 . . ? C63 C64 H64A 110.9 . . ? C65 C64 H64B 110.9 . . ? C63 C64 H64B 110.9 . . ? H64A C64 H64B 108.9 . . ? O61 C65 C64 105.9(8) . . ? O61 C65 H65A 110.6 . . ? C64 C65 H65A 110.6 . . ? O61 C65 H65B 110.6 . . ? C64 C65 H65B 110.6 . . ? H65A C65 H65B 108.7 . . ? C63 C64' C65' 107.2(12) . . ? C63 C64' H64C 110.3 . . ? C65' C64' H64C 110.3 . . ? C63 C64' H64D 110.3 . . ? C65' C64' H64D 110.3 . . ? H64C C64' H64D 108.5 . . ? O61 C65' C64' 105.2(9) . . ? O61 C65' H65C 110.7 . . ? C64' C65' H65C 110.7 . . ? O61 C65' H65D 110.7 . . ? C64' C65' H65D 110.7 . . ? H65C C65' H65D 108.8 . . ? C75 O71 C72' 105.7(8) . . ? C75 O71 C72 85.9(9) . . ? C73 C72 O71 98.2(15) . . ? C73 C72 H72A 112.1 . . ? O71 C72 H72A 112.1 . . ? C73 C72 H72B 112.1 . . ? O71 C72 H72B 112.1 . . ? H72A C72 H72B 109.8 . . ? O71 C72' C73 107.6(7) . . ? O71 C72' H72C 110.2 . . ? C73 C72' H72C 110.2 . . ? O71 C72' H72D 110.2 . . ? C73 C72' H72D 110.2 . . ? H72C C72' H72D 108.5 . . ? C72 C73 C74 101.5(10) . . ? C74 C73 C72' 102.8(6) . . ? C72 C73 H73A 111.5 . . ? C74 C73 H73A 111.5 . . ? C72 C73 H73B 111.5 . . ? C74 C73 H73B 111.5 . . ? H73A C73 H73B 109.3 . . ? C72' C73 H73C 111.2 . . ? C72' C73 H73D 111.2 . . ? H73C C73 H73D 109.1 . . ? C75 C74 C73 104.1(6) . . ? C75 C74 H74A 110.9 . . ? C73 C74 H74A 110.9 . . ? C75 C74 H74B 110.9 . . ? C73 C74 H74B 110.9 . . ? H74A C74 H74B 109.0 . . ? O71 C75 C74 109.3(6) . . ? O71 C75 H75A 109.8 . . ? C74 C75 H75A 109.8 . . ? O71 C75 H75B 109.8 . . ? C74 C75 H75B 109.8 . . ? H75A C75 H75B 108.3 . . ? 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 C21 B1 N1 C5 -125.3(4) . . . . ? C11 B1 N1 C5 124.3(4) . . . . ? C21 B1 N1 N2 55.4(3) . . . . ? C11 B1 N1 N2 -54.9(4) . . . . ? C5 N1 N2 C3 0.4(4) . . . . ? B1 N1 N2 C3 179.9(3) . . . . ? C5 N1 N2 B2 -179.9(3) . . . . ? B1 N1 N2 B2 -0.5(4) . . . . ? C22 B2 N2 C3 124.8(4) . . . . ? C12 B2 N2 C3 -125.5(4) . . . . ? C22 B2 N2 N1 -54.7(4) . . . . ? C12 B2 N2 N1 54.9(3) . . . . ? N1 N2 C3 C4 0.7(4) . . . . ? B2 N2 C3 C4 -178.9(4) . . . . ? N2 C3 C4 C5 -1.4(4) . . . . ? N2 C3 C4 Si1 -179.7(3) . . . . ? C6' Si1 C4 C3 -146.6(9) . . . . ? C8 Si1 C4 C3 -0.6(5) . . . . ? C7 Si1 C4 C3 133.7(6) . . . . ? C7' Si1 C4 C3 99.8(8) . . . . ? C8' Si1 C4 C3 -51.0(10) . . . . ? C6 Si1 C4 C3 -114.6(5) . . . . ? C6' Si1 C4 C5 35.5(9) . . . . ? C8 Si1 C4 C5 -178.5(5) . . . . ? C7 Si1 C4 C5 -44.2(6) . . . . ? C7' Si1 C4 C5 -78.1(8) . . . . ? C8' Si1 C4 C5 131.0(10) . . . . ? C6 Si1 C4 C5 67.4(5) . . . . ? N2 N1 C5 C4 -1.4(4) . . . . ? B1 N1 C5 C4 179.3(4) . . . . ? C3 C4 C5 N1 1.7(4) . . . . ? Si1 C4 C5 N1 -179.9(3) . . . . ? N1 B1 C11 C16 -126.8(3) . . . . ? C21 B1 C11 C16 125.4(4) . . . . ? N1 B1 C11 C12 54.8(4) . . . . ? C21 B1 C11 C12 -53.0(3) . . . . ? C16 C11 C12 C13 -1.1(4) . . . . ? B1 C11 C12 C13 177.4(3) . . . . ? C16 C11 C12 B2 179.9(3) . . . . ? B1 C11 C12 B2 -1.5(4) . . . . ? N2 B2 C12 C13 128.2(3) . . . . ? C22 B2 C12 C13 -123.9(4) . . . . ? N2 B2 C12 C11 -52.9(3) . . . . ? C22 B2 C12 C11 54.9(3) . . . . ? C11 C12 C13 C14 -0.3(5) . . . . ? B2 C12 C13 C14 178.5(3) . . . . ? C12 C13 C14 C15 2.1(6) . . . . ? C13 C14 C15 C16 -2.5(6) . . . . ? C12 C11 C16 C15 0.7(5) . . . . ? B1 C11 C16 C15 -177.6(3) . . . . ? C14 C15 C16 C11 1.1(5) . . . . ? N1 B1 C21 C26 126.3(3) . . . . ? C11 B1 C21 C26 -125.6(3) . . . . ? N1 B1 C21 C22 -53.9(3) . . . . ? C11 B1 C21 C22 54.2(3) . . . . ? C26 C21 C22 C23 1.3(4) . . . . ? B1 C21 C22 C23 -178.5(3) . . . . ? C26 C21 C22 B2 179.6(3) . . . . ? B1 C21 C22 B2 -0.2(4) . . . . ? N2 B2 C22 C23 -127.5(3) . . . . ? C12 B2 C22 C23 124.1(3) . . . . ? N2 B2 C22 C21 54.4(3) . . . . ? C12 B2 C22 C21 -54.0(3) . . . . ? C21 C22 C23 C24 -0.5(5) . . . . ? B2 C22 C23 C24 -178.5(3) . . . . ? C22 C23 C24 C25 0.2(6) . . . . ? C23 C24 C25 C26 -0.7(6) . . . . ? C24 C25 C26 C21 1.6(6) . . . . ? C22 C21 C26 C25 -1.9(5) . . . . ? B1 C21 C26 C25 177.9(3) . . . . ? O61 Li1 O31 C35' 158.5(7) . . . . ? O41 Li1 O31 C35' -83.5(8) . . . . ? O51 Li1 O31 C35' 35.1(8) . . . . ? O61 Li1 O31 C32' -24.4(7) . . . . ? O41 Li1 O31 C32' 93.5(6) . . . . ? O51 Li1 O31 C32' -147.9(6) . . . . ? O61 Li1 O31 C35 127.9(8) . . . . ? O41 Li1 O31 C35 -114.2(8) . . . . ? O51 Li1 O31 C35 4.4(9) . . . . ? O61 Li1 O31 C32 -65.8(7) . . . . ? O41 Li1 O31 C32 52.2(8) . . . . ? O51 Li1 O31 C32 170.8(7) . . . . ? C35' O31 C32 C33 -37.9(9) . . . . ? C32' O31 C32 C33 79.2(11) . . . . ? C35 O31 C32 C33 -13.9(10) . . . . ? Li1 O31 C32 C33 177.8(6) . . . . ? C35' O31 C32' C33 14.6(8) . . . . ? C35 O31 C32' C33 40.6(8) . . . . ? C32 O31 C32' C33 -57.4(9) . . . . ? Li1 O31 C32' C33 -162.7(5) . . . . ? O31 C32 C33 C34 16.9(11) . . . . ? O31 C32 C33 C32' -64.0(9) . . . . ? O31 C32' C33 C32 72.4(9) . . . . ? O31 C32' C33 C34 -36.4(8) . . . . ? C32 C33 C34 C35 -14.3(14) . . . . ? C32' C33 C34 C35 19.2(11) . . . . ? C32 C33 C34 C35' 9.7(12) . . . . ? C32' C33 C34 C35' 43.2(9) . . . . ? C35' O31 C35 C34 76.8(15) . . . . ? C32' O31 C35 C34 -30.1(10) . . . . ? C32 O31 C35 C34 5.6(11) . . . . ? Li1 O31 C35 C34 173.9(6) . . . . ? C33 C34 C35 O31 4.6(12) . . . . ? C35' C34 C35 O31 -70.4(13) . . . . ? C32' O31 C35' C34 10.9(10) . . . . ? C35 O31 C35' C34 -71.1(15) . . . . ? C32 O31 C35' C34 43.5(9) . . . . ? Li1 O31 C35' C34 -171.8(5) . . . . ? C33 C34 C35' O31 -34.9(10) . . . . ? C35 C34 C35' O31 76.9(14) . . . . ? O61 Li1 O41 C42 -119.2(10) . . . . ? O31 Li1 O41 C42 124.1(10) . . . . ? O51 Li1 O41 C42 6.3(11) . . . . ? O61 Li1 O41 C45 86.0(5) . . . . ? O31 Li1 O41 C45 -30.7(5) . . . . ? O51 Li1 O41 C45 -148.5(4) . . . . ? O61 Li1 O41 C42' -68.8(5) . . . . ? O31 Li1 O41 C42' 174.5(4) . . . . ? O51 Li1 O41 C42' 56.7(5) . . . . ? C45 O41 C42 C43 -45.3(11) . . . . ? C42' O41 C42 C43 56.8(9) . . . . ? Li1 O41 C42 C43 156.3(5) . . . . ? C42 O41 C42' C43 -69.2(11) . . . . ? C45 O41 C42' C43 22.1(6) . . . . ? Li1 O41 C42' C43 179.9(4) . . . . ? O41 C42' C43 C44 -41.9(7) . . . . ? O41 C42' C43 C42 61.8(11) . . . . ? O41 C42' C43 C44' -12.4(8) . . . . ? O41 C42 C43 C44 24.2(12) . . . . ? O41 C42 C43 C42' -63.3(10) . . . . ? O41 C42 C43 C44' 48.7(11) . . . . ? C42' C43 C44 C45 43.8(7) . . . . ? C42 C43 C44 C45 3.3(10) . . . . ? C44' C43 C44 C45 -56.1(10) . . . . ? C44 C43 C44' C45 86.6(13) . . . . ? C42' C43 C44' C45 -0.9(11) . . . . ? C42 C43 C44' C45 -38.5(11) . . . . ? C43 C44' C45 O41 14.8(11) . . . . ? C43 C44' C45 C44 -51.9(10) . . . . ? C42 O41 C45 C44' 18.4(13) . . . . ? C42' O41 C45 C44' -24.3(10) . . . . ? Li1 O41 C45 C44' 177.9(8) . . . . ? C42 O41 C45 C44 46.0(9) . . . . ? C42' O41 C45 C44 3.3(5) . . . . ? Li1 O41 C45 C44 -154.4(4) . . . . ? C43 C44 C45 C44' 91.1(13) . . . . ? C43 C44 C45 O41 -29.5(7) . . . . ? O61 Li1 O51 C55 -43.3(6) . . . . ? O31 Li1 O51 C55 74.4(5) . . . . ? O41 Li1 O51 C55 -164.6(4) . . . . ? O61 Li1 O51 C52 138.0(7) . . . . ? O31 Li1 O51 C52 -104.3(7) . . . . ? O41 Li1 O51 C52 16.7(8) . . . . ? O61 Li1 O51 C52' 166.6(10) . . . . ? O31 Li1 O51 C52' -75.7(10) . . . . ? O41 Li1 O51 C52' 45.3(10) . . . . ? C55 O51 C52 C53 -35.0(7) . . . . ? C52' O51 C52 C53 53.9(15) . . . . ? Li1 O51 C52 C53 143.8(5) . . . . ? C55 O51 C52' C53 0.5(15) . . . . ? C52 O51 C52' C53 -98(2) . . . . ? Li1 O51 C52' C53 155.0(8) . . . . ? O51 C52' C53 C54 -18.1(14) . . . . ? O51 C52' C53 C52 76.0(19) . . . . ? O51 C52' C53 C54' 5.7(14) . . . . ? O51 C52 C53 C54 17.6(9) . . . . ? O51 C52 C53 C52' -75.5(18) . . . . ? O51 C52 C53 C54' 38.2(7) . . . . ? C52' C53 C54 C55 26.7(12) . . . . ? C52 C53 C54 C55 4.6(11) . . . . ? C54' C53 C54 C55 -58.8(14) . . . . ? C54 C53 C54' C55 91.3(16) . . . . ? C52' C53 C54' C55 -10.2(11) . . . . ? C52 C53 C54' C55 -30.1(9) . . . . ? C53 C54' C55 O51 11.3(11) . . . . ? C53 C54' C55 C54 -45.9(13) . . . . ? C52 O51 C55 C54' 15.7(11) . . . . ? C52' O51 C55 C54' -8.6(14) . . . . ? Li1 O51 C55 C54' -163.2(8) . . . . ? C52 O51 C55 C54 37.7(9) . . . . ? C52' O51 C55 C54 13.4(12) . . . . ? Li1 O51 C55 C54 -141.2(6) . . . . ? C53 C54 C55 C54' 104.5(18) . . . . ? C53 C54 C55 O51 -25.4(11) . . . . ? O31 Li1 O61 C65' -66.1(8) . . . . ? O41 Li1 O61 C65' 173.5(8) . . . . ? O51 Li1 O61 C65' 52.1(9) . . . . ? O31 Li1 O61 C62 117.0(5) . . . . ? O41 Li1 O61 C62 -3.5(6) . . . . ? O51 Li1 O61 C62 -124.8(4) . . . . ? O31 Li1 O61 C65 -35.8(9) . . . . ? O41 Li1 O61 C65 -156.3(9) . . . . ? O51 Li1 O61 C65 82.3(9) . . . . ? C65' O61 C62 C63 4.0(8) . . . . ? C65 O61 C62 C63 -23.6(10) . . . . ? Li1 O61 C62 C63 -178.7(5) . . . . ? O61 C62 C63 C64' 11.1(14) . . . . ? O61 C62 C63 C64 36.3(7) . . . . ? C64' C63 C64 C65 75(2) . . . . ? C62 C63 C64 C65 -36.0(9) . . . . ? C65' O61 C65 C64 -92.7(17) . . . . ? C62 O61 C65 C64 0.7(12) . . . . ? Li1 O61 C65 C64 158.1(7) . . . . ? C63 C64 C65 O61 22.2(12) . . . . ? C62 C63 C64' C65' -21.1(18) . . . . ? C64 C63 C64' C65' -97(2) . . . . ? C62 O61 C65' C64' -15.9(11) . . . . ? C65 O61 C65' C64' 79.7(16) . . . . ? Li1 O61 C65' C64' 166.7(10) . . . . ? C63 C64' C65' O61 23.1(17) . . . . ? C75 O71 C72 C73 62.2(15) . . . . ? C72' O71 C72 C73 -88(3) . . . . ? C75 O71 C72' C73 29.2(11) . . . . ? C72 O71 C72' C73 60(2) . . . . ? O71 C72 C73 C74 -50.1(16) . . . . ? O71 C72 C73 C72' 45.6(16) . . . . ? O71 C72' C73 C72 -105(2) . . . . ? O71 C72' C73 C74 -13.9(13) . . . . ? C72 C73 C74 C75 24.0(19) . . . . ? C72' C73 C74 C75 -5.7(10) . . . . ? C72' O71 C75 C74 -34.0(9) . . . . ? C72 O71 C75 C74 -45.7(9) . . . . ? C73 C74 C75 O71 24.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.416 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.053