data_91211mae _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H48 B F2 N3 O7' _chemical_formula_weight 647.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P212121' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.686(2) _cell_length_b 16.213(5) _cell_length_c 21.630(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3396.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(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 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9586 _exptl_absorpt_correction_T_max 0.9859 _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 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31437 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7770 _reflns_number_gt 6041 _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^)+(0.0421P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(6) _refine_ls_number_reflns 7770 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O2 O 0.09749(12) 0.54249(8) 0.89998(6) 0.0267(3) Uani 1 1 d . . . O1 O -0.08329(12) 0.63703(8) 0.93443(6) 0.0265(3) Uani 1 1 d . . . F1 F 0.05703(12) 0.66775(8) 0.84972(6) 0.0410(3) Uani 1 1 d . . . F2 F 0.14836(11) 0.66709(8) 0.94691(6) 0.0422(3) Uani 1 1 d . . . O3 O 0.16265(14) 0.44707(8) 1.20467(6) 0.0319(3) Uani 1 1 d . . . C22 C 0.13100(18) 0.30316(12) 1.17348(8) 0.0248(4) Uani 1 1 d . . . H1 H 0.1869 0.2832 1.2063 0.030 Uiso 1 1 calc R . . C16 C -0.54209(19) 0.58995(13) 0.94340(8) 0.0286(4) Uani 1 1 d . . . H2 H -0.6333 0.5689 0.9400 0.034 Uiso 1 1 calc R . . C23 C -0.03790(18) 0.36056(12) 1.07917(9) 0.0261(4) Uani 1 1 d . . . C17 C -0.31494(17) 0.60111(12) 0.93597(8) 0.0226(4) Uani 1 1 d . . . C24 C -0.01610(18) 0.27625(12) 1.08573(8) 0.0243(4) Uani 1 1 d . . . H3 H -0.0599 0.2383 1.0586 0.029 Uiso 1 1 calc R . . C25 C 0.10999(18) 0.38772(12) 1.16664(8) 0.0245(4) Uani 1 1 d . . . C19 C 0.05114(18) 0.41075(12) 0.86292(8) 0.0237(4) Uani 1 1 d . . . C13 C -0.17657(18) 0.58126(12) 0.91934(8) 0.0238(4) Uani 1 1 d . . . C26 C 0.07078(18) 0.24803(12) 1.13257(8) 0.0233(4) Uani 1 1 d . . . C20 C 0.1798(2) 0.30068(13) 0.83695(9) 0.0320(5) Uani 1 1 d . . . H4 H 0.2560 0.2649 0.8303 0.038 Uiso 1 1 calc R . . C27 C 0.02998(18) 0.41667(12) 1.11725(8) 0.0253(4) Uani 1 1 d . . . C14 C 0.00058(18) 0.48889(11) 0.88393(8) 0.0220(4) Uani 1 1 d . . . C21 C 0.0433(2) 0.28335(12) 0.82492(9) 0.0308(4) Uani 1 1 d . . . H5 H 0.0093 0.2331 0.8082 0.037 Uiso 1 1 calc R . . C18 C -0.50698(19) 0.66480(13) 0.96929(9) 0.0291(4) Uani 1 1 d . . . H6 H -0.5687 0.7039 0.9868 0.035 Uiso 1 1 calc R . . C15 C -0.13761(18) 0.50834(11) 0.89025(8) 0.0233(4) Uani 1 1 d . . . H7 H -0.2061 0.4719 0.8747 0.028 Uiso 1 1 calc R . . B1 B 0.0572(2) 0.63027(15) 0.90728(11) 0.0295(5) Uani 1 1 d . . . N1 N 0.07382(16) 0.95638(10) 0.84588(7) 0.0256(3) Uani 1 1 d . . . C1 C 0.18728(19) 0.89801(12) 0.86695(9) 0.0268(4) Uani 1 1 d . . . H8 H 0.2634 0.9313 0.8845 0.032 Uiso 1 1 calc R . . H9 H 0.1502 0.8632 0.9007 0.032 Uiso 1 1 calc R . . C2 C 0.2468(2) 0.84185(14) 0.81779(9) 0.0355(5) Uani 1 1 d . . . H10 H 0.2840 0.8752 0.7833 0.043 Uiso 1 1 calc R . . H11 H 0.1736 0.8054 0.8012 0.043 Uiso 1 1 calc R . . C3 C -0.1217(2) 0.85294(13) 0.86888(9) 0.0308(4) Uani 1 1 d . . . H12 H -0.1437 0.8833 0.9074 0.037 Uiso 1 1 calc R . . H13 H -0.0593 0.8066 0.8794 0.037 Uiso 1 1 calc R . . C4 C -0.05238(18) 0.90981(12) 0.82329(8) 0.0262(4) Uani 1 1 d . . . H14 H -0.1214 0.9507 0.8092 0.031 Uiso 1 1 calc R . . H15 H -0.0250 0.8768 0.7868 0.031 Uiso 1 1 calc R . . C5 C 0.2451(2) 1.06379(14) 0.80313(9) 0.0354(5) Uani 1 1 d . . . H16 H 0.3226 1.0301 0.8190 0.042 Uiso 1 1 calc R . . H17 H 0.2218 1.1057 0.8347 0.042 Uiso 1 1 calc R . . C6 C 0.1212(2) 1.00910(12) 0.79141(8) 0.0286(4) Uani 1 1 d . . . H18 H 0.1431 0.9720 0.7564 0.034 Uiso 1 1 calc R . . H19 H 0.0431 1.0445 0.7784 0.034 Uiso 1 1 calc R . . C7 C -0.2544(2) 0.81994(15) 0.83950(10) 0.0389(5) Uani 1 1 d . . . H20 H -0.2323 0.7928 0.8002 0.058 Uiso 1 1 calc R . . H21 H -0.3181 0.8658 0.8319 0.058 Uiso 1 1 calc R . . H22 H -0.2977 0.7801 0.8675 0.058 Uiso 1 1 calc R . . C8 C 0.03997(19) 1.00927(13) 0.90199(8) 0.0282(4) Uani 1 1 d . . . H23 H 0.0206 0.9723 0.9373 0.034 Uiso 1 1 calc R . . H24 H 0.1227 1.0422 0.9127 0.034 Uiso 1 1 calc R . . C9 C -0.0807(2) 1.06743(13) 0.89439(9) 0.0345(5) Uani 1 1 d . . . H25 H -0.0651 1.1029 0.8578 0.041 Uiso 1 1 calc R . . H26 H -0.1659 1.0351 0.8872 0.041 Uiso 1 1 calc R . . C10 C 0.2881(2) 1.10641(15) 0.74345(10) 0.0417(5) Uani 1 1 d . . . H27 H 0.2095 1.1370 0.7265 0.063 Uiso 1 1 calc R . . H28 H 0.3185 1.0650 0.7134 0.063 Uiso 1 1 calc R . . H29 H 0.3641 1.1447 0.7520 0.063 Uiso 1 1 calc R . . C11 C -0.0991(3) 1.12084(16) 0.95099(11) 0.0504(7) Uani 1 1 d . . . H30 H -0.0175 1.1559 0.9564 0.076 Uiso 1 1 calc R . . H31 H -0.1106 1.0857 0.9875 0.076 Uiso 1 1 calc R . . H32 H -0.1810 1.1556 0.9458 0.076 Uiso 1 1 calc R . . C12 C 0.3612(2) 0.79023(14) 0.84601(11) 0.0397(5) Uani 1 1 d . . . H33 H 0.3216 0.7519 0.8762 0.060 Uiso 1 1 calc R . . H34 H 0.4277 0.8265 0.8667 0.060 Uiso 1 1 calc R . . H35 H 0.4080 0.7590 0.8134 0.060 Uiso 1 1 calc R . . O6 O 0.19063(12) 0.13385(9) 1.17551(6) 0.0291(3) Uani 1 1 d . . . O4 O 0.01094(15) 0.50054(9) 1.11163(6) 0.0336(3) Uani 1 1 d . . . O7 O 0.02667(13) 0.10864(8) 1.10545(6) 0.0307(3) Uani 1 1 d . . . N3 N -0.42731(14) 0.55142(10) 0.92370(7) 0.0242(3) Uani 1 1 d . . . H36 H -0.4243 0.5026 0.9059 0.029 Uiso 1 1 calc R . . N2 N -0.03471(15) 0.34940(10) 0.84070(7) 0.0254(3) Uani 1 1 d . . . H37 H -0.1251 0.3527 0.8374 0.030 Uiso 1 1 calc R . . O5 O -0.12893(14) 0.39478(9) 1.03770(6) 0.0335(3) Uani 1 1 d . . . C33 C -0.36391(18) 0.67231(12) 0.96502(8) 0.0250(4) Uani 1 1 d . . . H38 H -0.3098 0.7174 0.9792 0.030 Uiso 1 1 calc R . . C31 C 0.09633(17) 0.15631(12) 1.13860(8) 0.0231(4) Uani 1 1 d . . . C29 C 0.0553(2) 0.53539(14) 1.05378(9) 0.0364(5) Uani 1 1 d . . . H39 H -0.0018 0.5134 1.0202 0.055 Uiso 1 1 calc R . . H40 H 0.1521 0.5210 1.0464 0.055 Uiso 1 1 calc R . . H41 H 0.0457 0.5955 1.0553 0.055 Uiso 1 1 calc R . . C32 C 0.18540(19) 0.38098(12) 0.86091(9) 0.0276(4) Uani 1 1 d . . . H42 H 0.2662 0.4097 0.8734 0.033 Uiso 1 1 calc R . . C30 C -0.2018(2) 0.33967(14) 0.99796(10) 0.0386(5) Uani 1 1 d . . . H43 H -0.2524 0.2993 1.0229 0.058 Uiso 1 1 calc R . . H44 H -0.1361 0.3109 0.9711 0.058 Uiso 1 1 calc R . . H45 H -0.2671 0.3710 0.9725 0.058 Uiso 1 1 calc R . . C34 C 0.2195(3) 0.42074(17) 1.26204(10) 0.0478(6) Uani 1 1 d . . . H46 H 0.2986 0.3845 1.2543 0.072 Uiso 1 1 calc R . . H47 H 0.1492 0.3907 1.2856 0.072 Uiso 1 1 calc R . . H48 H 0.2499 0.4689 1.2857 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.0217(6) 0.0230(7) 0.0355(7) -0.0040(6) 0.0009(6) -0.0025(5) O1 0.0237(6) 0.0193(7) 0.0364(7) -0.0053(6) 0.0030(6) -0.0024(5) F1 0.0436(6) 0.0302(7) 0.0492(7) 0.0081(6) 0.0179(6) 0.0033(5) F2 0.0269(5) 0.0376(8) 0.0619(8) -0.0217(6) 0.0044(6) -0.0073(5) O3 0.0441(7) 0.0269(8) 0.0247(6) -0.0032(6) -0.0055(6) -0.0086(7) C22 0.0238(9) 0.0276(11) 0.0230(9) -0.0003(8) 0.0001(8) 0.0004(8) C16 0.0250(9) 0.0300(11) 0.0310(10) 0.0040(8) 0.0030(8) 0.0050(8) C23 0.0263(9) 0.0267(11) 0.0254(9) -0.0010(8) 0.0000(8) 0.0029(8) C17 0.0230(8) 0.0210(10) 0.0239(9) 0.0017(7) -0.0005(8) 0.0013(7) C24 0.0224(8) 0.0243(10) 0.0262(9) -0.0053(8) 0.0009(8) -0.0004(7) C25 0.0240(8) 0.0273(11) 0.0221(9) -0.0054(7) 0.0039(8) -0.0042(7) C19 0.0258(9) 0.0197(10) 0.0255(9) -0.0001(7) 0.0003(8) -0.0009(7) C13 0.0269(9) 0.0189(10) 0.0257(9) 0.0037(7) -0.0006(8) -0.0001(7) C26 0.0200(8) 0.0250(10) 0.0248(9) -0.0023(7) 0.0034(8) -0.0003(7) C20 0.0319(10) 0.0258(11) 0.0383(11) -0.0016(9) 0.0026(9) 0.0079(8) C27 0.0270(9) 0.0213(10) 0.0276(9) -0.0025(8) 0.0059(8) 0.0013(7) C14 0.0259(8) 0.0195(10) 0.0207(8) -0.0006(7) 0.0005(8) -0.0010(7) C21 0.0383(11) 0.0174(10) 0.0367(10) -0.0034(8) 0.0028(10) 0.0028(8) C18 0.0306(9) 0.0278(11) 0.0290(10) 0.0014(8) 0.0049(9) 0.0090(8) C15 0.0237(8) 0.0201(10) 0.0261(9) -0.0018(8) -0.0013(8) -0.0001(7) B1 0.0250(10) 0.0241(12) 0.0392(13) -0.0072(10) 0.0080(10) -0.0023(9) N1 0.0321(8) 0.0203(9) 0.0245(7) 0.0002(6) -0.0041(7) -0.0011(7) C1 0.0292(9) 0.0244(11) 0.0268(9) 0.0034(8) -0.0030(8) 0.0008(8) C2 0.0427(11) 0.0317(13) 0.0321(11) 0.0005(9) 0.0036(10) 0.0033(10) C3 0.0331(10) 0.0255(11) 0.0336(10) 0.0025(8) 0.0018(9) 0.0006(8) C4 0.0286(9) 0.0217(10) 0.0282(9) -0.0039(8) -0.0019(8) -0.0027(8) C5 0.0392(11) 0.0342(13) 0.0328(11) 0.0062(9) -0.0101(9) -0.0140(9) C6 0.0381(10) 0.0233(11) 0.0246(9) 0.0024(8) -0.0025(9) -0.0054(9) C7 0.0415(11) 0.0365(14) 0.0386(12) -0.0025(10) 0.0065(10) -0.0105(10) C8 0.0336(10) 0.0261(11) 0.0249(9) -0.0044(8) -0.0025(9) 0.0000(8) C9 0.0409(11) 0.0290(12) 0.0337(10) -0.0047(9) -0.0057(10) 0.0031(9) C10 0.0454(12) 0.0398(15) 0.0399(12) 0.0074(10) -0.0047(10) -0.0161(10) C11 0.0525(14) 0.0489(16) 0.0498(14) -0.0222(12) -0.0114(12) 0.0182(12) C12 0.0354(11) 0.0330(13) 0.0508(13) -0.0058(10) -0.0016(11) 0.0039(9) O6 0.0259(6) 0.0301(8) 0.0314(7) -0.0029(6) -0.0032(6) 0.0056(6) O4 0.0492(8) 0.0218(8) 0.0299(7) 0.0013(6) 0.0042(7) 0.0003(6) O7 0.0292(6) 0.0246(8) 0.0383(7) -0.0051(6) -0.0046(6) 0.0007(6) N3 0.0214(7) 0.0224(9) 0.0288(8) -0.0017(6) 0.0016(7) 0.0024(6) N2 0.0246(7) 0.0209(9) 0.0305(8) 0.0012(6) 0.0030(7) 0.0012(6) O5 0.0370(7) 0.0288(8) 0.0347(7) -0.0012(6) -0.0125(7) 0.0035(6) C33 0.0296(9) 0.0213(10) 0.0242(9) -0.0012(7) 0.0015(8) 0.0012(8) C31 0.0215(8) 0.0255(11) 0.0223(9) -0.0014(8) 0.0053(8) 0.0020(8) C29 0.0447(11) 0.0329(12) 0.0316(10) 0.0062(9) -0.0003(10) -0.0032(10) C32 0.0255(9) 0.0252(11) 0.0322(10) -0.0003(8) 0.0001(8) 0.0027(8) C30 0.0457(12) 0.0342(13) 0.0359(11) 0.0001(9) -0.0153(10) -0.0008(10) C34 0.0683(16) 0.0442(15) 0.0308(11) -0.0032(10) -0.0116(12) -0.0159(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2 C14 1.325(2) . ? O2 B1 1.484(3) . ? O1 C13 1.319(2) . ? O1 B1 1.487(2) . ? F1 B1 1.385(3) . ? F2 B1 1.368(3) . ? O3 C25 1.365(2) . ? O3 C34 1.423(3) . ? C22 C26 1.386(3) . ? C22 C25 1.394(3) . ? C22 H1 0.9500 . ? C16 N3 1.345(2) . ? C16 C18 1.379(3) . ? C16 H2 0.9500 . ? C23 O5 1.375(2) . ? C23 C24 1.391(3) . ? C23 C27 1.392(3) . ? C17 N3 1.380(2) . ? C17 C33 1.397(3) . ? C17 C13 1.424(2) . ? C24 C26 1.394(3) . ? C24 H3 0.9500 . ? C25 C27 1.401(3) . ? C19 N2 1.383(2) . ? C19 C32 1.388(3) . ? C19 C14 1.432(3) . ? C13 C15 1.391(3) . ? C26 C31 1.513(3) . ? C20 C21 1.376(3) . ? C20 C32 1.402(3) . ? C20 H4 0.9500 . ? C27 O4 1.378(2) . ? C14 C15 1.382(2) . ? C21 N2 1.354(2) . ? C21 H5 0.9500 . ? C18 C33 1.394(3) . ? C18 H6 0.9500 . ? C15 H7 0.9500 . ? N1 C4 1.518(2) . ? N1 C1 1.520(2) . ? N1 C8 1.522(2) . ? N1 C6 1.526(2) . ? C1 C2 1.514(3) . ? C1 H8 0.9900 . ? C1 H9 0.9900 . ? C2 C12 1.516(3) . ? C2 H10 0.9900 . ? C2 H11 0.9900 . ? C3 C4 1.508(3) . ? C3 C7 1.530(3) . ? C3 H12 0.9900 . ? C3 H13 0.9900 . ? C4 H14 0.9900 . ? C4 H15 0.9900 . ? C5 C6 1.514(3) . ? C5 C10 1.522(3) . ? C5 H16 0.9900 . ? C5 H17 0.9900 . ? C6 H18 0.9900 . ? C6 H19 0.9900 . ? C7 H20 0.9800 . ? C7 H21 0.9800 . ? C7 H22 0.9800 . ? C8 C9 1.511(3) . ? C8 H23 0.9900 . ? C8 H24 0.9900 . ? C9 C11 1.510(3) . ? C9 H25 0.9900 . ? C9 H26 0.9900 . ? C10 H27 0.9800 . ? C10 H28 0.9800 . ? C10 H29 0.9800 . ? C11 H30 0.9800 . ? C11 H31 0.9800 . ? C11 H32 0.9800 . ? C12 H33 0.9800 . ? C12 H34 0.9800 . ? C12 H35 0.9800 . ? O6 C31 1.267(2) . ? O4 C29 1.439(2) . ? O7 C31 1.252(2) . ? N3 H36 0.8800 . ? N2 H37 0.8800 . ? O5 C30 1.427(2) . ? C33 H38 0.9500 . ? C29 H39 0.9800 . ? C29 H40 0.9800 . ? C29 H41 0.9800 . ? C32 H42 0.9500 . ? C30 H43 0.9800 . ? C30 H44 0.9800 . ? C30 H45 0.9800 . ? C34 H46 0.9800 . ? C34 H47 0.9800 . ? C34 H48 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 C14 O2 B1 118.07(14) . . ? C13 O1 B1 118.61(15) . . ? C25 O3 C34 117.31(17) . . ? C26 C22 C25 120.33(17) . . ? C26 C22 H1 119.8 . . ? C25 C22 H1 119.8 . . ? N3 C16 C18 109.48(16) . . ? N3 C16 H2 125.3 . . ? C18 C16 H2 125.3 . . ? O5 C23 C24 124.10(17) . . ? O5 C23 C27 115.17(17) . . ? C24 C23 C27 120.68(17) . . ? N3 C17 C33 107.52(15) . . ? N3 C17 C13 124.17(16) . . ? C33 C17 C13 128.29(17) . . ? C23 C24 C26 119.23(17) . . ? C23 C24 H3 120.4 . . ? C26 C24 H3 120.4 . . ? O3 C25 C22 125.09(16) . . ? O3 C25 C27 115.48(17) . . ? C22 C25 C27 119.43(17) . . ? N2 C19 C32 107.61(16) . . ? N2 C19 C14 122.75(16) . . ? C32 C19 C14 129.64(17) . . ? O1 C13 C15 120.56(16) . . ? O1 C13 C17 115.28(16) . . ? C15 C13 C17 124.15(17) . . ? C22 C26 C24 120.41(18) . . ? C22 C26 C31 120.65(16) . . ? C24 C26 C31 118.93(16) . . ? C21 C20 C32 107.26(17) . . ? C21 C20 H4 126.4 . . ? C32 C20 H4 126.4 . . ? O4 C27 C23 121.97(17) . . ? O4 C27 C25 118.17(16) . . ? C23 C27 C25 119.58(18) . . ? O2 C14 C15 120.70(17) . . ? O2 C14 C19 114.89(15) . . ? C15 C14 C19 124.36(17) . . ? N2 C21 C20 109.08(18) . . ? N2 C21 H5 125.5 . . ? C20 C21 H5 125.5 . . ? C16 C18 C33 107.16(17) . . ? C16 C18 H6 126.4 . . ? C33 C18 H6 126.4 . . ? C14 C15 C13 120.09(17) . . ? C14 C15 H7 120.0 . . ? C13 C15 H7 120.0 . . ? F2 B1 F1 111.89(18) . . ? F2 B1 O2 108.41(17) . . ? F1 B1 O2 109.00(16) . . ? F2 B1 O1 108.12(16) . . ? F1 B1 O1 108.74(17) . . ? O2 B1 O1 110.69(16) . . ? C4 N1 C1 111.66(14) . . ? C4 N1 C8 111.32(14) . . ? C1 N1 C8 105.52(13) . . ? C4 N1 C6 105.79(13) . . ? C1 N1 C6 111.28(14) . . ? C8 N1 C6 111.40(15) . . ? C2 C1 N1 116.06(15) . . ? C2 C1 H8 108.3 . . ? N1 C1 H8 108.3 . . ? C2 C1 H9 108.3 . . ? N1 C1 H9 108.3 . . ? H8 C1 H9 107.4 . . ? C1 C2 C12 109.11(17) . . ? C1 C2 H10 109.9 . . ? C12 C2 H10 109.9 . . ? C1 C2 H11 109.9 . . ? C12 C2 H11 109.9 . . ? H10 C2 H11 108.3 . . ? C4 C3 C7 108.43(16) . . ? C4 C3 H12 110.0 . . ? C7 C3 H12 110.0 . . ? C4 C3 H13 110.0 . . ? C7 C3 H13 110.0 . . ? H12 C3 H13 108.4 . . ? C3 C4 N1 116.89(15) . . ? C3 C4 H14 108.1 . . ? N1 C4 H14 108.1 . . ? C3 C4 H15 108.1 . . ? N1 C4 H15 108.1 . . ? H14 C4 H15 107.3 . . ? C6 C5 C10 109.95(16) . . ? C6 C5 H16 109.7 . . ? C10 C5 H16 109.7 . . ? C6 C5 H17 109.7 . . ? C10 C5 H17 109.7 . . ? H16 C5 H17 108.2 . . ? C5 C6 N1 115.92(15) . . ? C5 C6 H18 108.3 . . ? N1 C6 H18 108.3 . . ? C5 C6 H19 108.3 . . ? N1 C6 H19 108.3 . . ? H18 C6 H19 107.4 . . ? C3 C7 H20 109.5 . . ? C3 C7 H21 109.5 . . ? H20 C7 H21 109.5 . . ? C3 C7 H22 109.5 . . ? H20 C7 H22 109.5 . . ? H21 C7 H22 109.5 . . ? C9 C8 N1 115.58(15) . . ? C9 C8 H23 108.4 . . ? N1 C8 H23 108.4 . . ? C9 C8 H24 108.4 . . ? N1 C8 H24 108.4 . . ? H23 C8 H24 107.4 . . ? C11 C9 C8 111.16(17) . . ? C11 C9 H25 109.4 . . ? C8 C9 H25 109.4 . . ? C11 C9 H26 109.4 . . ? C8 C9 H26 109.4 . . ? H25 C9 H26 108.0 . . ? C5 C10 H27 109.5 . . ? C5 C10 H28 109.5 . . ? H27 C10 H28 109.5 . . ? C5 C10 H29 109.5 . . ? H27 C10 H29 109.5 . . ? H28 C10 H29 109.5 . . ? C9 C11 H30 109.5 . . ? C9 C11 H31 109.5 . . ? H30 C11 H31 109.5 . . ? C9 C11 H32 109.5 . . ? H30 C11 H32 109.5 . . ? H31 C11 H32 109.5 . . ? C2 C12 H33 109.5 . . ? C2 C12 H34 109.5 . . ? H33 C12 H34 109.5 . . ? C2 C12 H35 109.5 . . ? H33 C12 H35 109.5 . . ? H34 C12 H35 109.5 . . ? C27 O4 C29 115.12(15) . . ? C16 N3 C17 108.66(15) . . ? C16 N3 H36 125.7 . . ? C17 N3 H36 125.7 . . ? C21 N2 C19 108.71(15) . . ? C21 N2 H37 125.6 . . ? C19 N2 H37 125.6 . . ? C23 O5 C30 117.25(16) . . ? C18 C33 C17 107.16(17) . . ? C18 C33 H38 126.4 . . ? C17 C33 H38 126.4 . . ? O7 C31 O6 124.92(18) . . ? O7 C31 C26 117.98(16) . . ? O6 C31 C26 117.05(16) . . ? O4 C29 H39 109.5 . . ? O4 C29 H40 109.5 . . ? H39 C29 H40 109.5 . . ? O4 C29 H41 109.5 . . ? H39 C29 H41 109.5 . . ? H40 C29 H41 109.5 . . ? C19 C32 C20 107.34(18) . . ? C19 C32 H42 126.3 . . ? C20 C32 H42 126.3 . . ? O5 C30 H43 109.5 . . ? O5 C30 H44 109.5 . . ? H43 C30 H44 109.5 . . ? O5 C30 H45 109.5 . . ? H43 C30 H45 109.5 . . ? H44 C30 H45 109.5 . . ? O3 C34 H46 109.5 . . ? O3 C34 H47 109.5 . . ? H46 C34 H47 109.5 . . ? O3 C34 H48 109.5 . . ? H46 C34 H48 109.5 . . ? H47 C34 H48 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 O5 C23 C24 C26 -175.05(16) . . . . ? C27 C23 C24 C26 2.4(3) . . . . ? C34 O3 C25 C22 -13.2(3) . . . . ? C34 O3 C25 C27 167.22(18) . . . . ? C26 C22 C25 O3 179.04(16) . . . . ? C26 C22 C25 C27 -1.4(3) . . . . ? B1 O1 C13 C15 14.1(3) . . . . ? B1 O1 C13 C17 -166.99(17) . . . . ? N3 C17 C13 O1 179.29(16) . . . . ? C33 C17 C13 O1 1.2(3) . . . . ? N3 C17 C13 C15 -1.9(3) . . . . ? C33 C17 C13 C15 -179.91(19) . . . . ? C25 C22 C26 C24 -2.7(3) . . . . ? C25 C22 C26 C31 178.27(16) . . . . ? C23 C24 C26 C22 2.2(3) . . . . ? C23 C24 C26 C31 -178.76(16) . . . . ? O5 C23 C27 O4 -2.6(3) . . . . ? C24 C23 C27 O4 179.67(16) . . . . ? O5 C23 C27 C25 171.17(15) . . . . ? C24 C23 C27 C25 -6.5(3) . . . . ? O3 C25 C27 O4 -0.4(2) . . . . ? C22 C25 C27 O4 180.00(16) . . . . ? O3 C25 C27 C23 -174.43(16) . . . . ? C22 C25 C27 C23 6.0(3) . . . . ? B1 O2 C14 C15 -17.4(3) . . . . ? B1 O2 C14 C19 165.18(16) . . . . ? N2 C19 C14 O2 -175.83(16) . . . . ? C32 C19 C14 O2 5.0(3) . . . . ? N2 C19 C14 C15 6.9(3) . . . . ? C32 C19 C14 C15 -172.33(19) . . . . ? C32 C20 C21 N2 -0.2(2) . . . . ? N3 C16 C18 C33 0.1(2) . . . . ? O2 C14 C15 C13 -6.5(3) . . . . ? C19 C14 C15 C13 170.69(17) . . . . ? O1 C13 C15 C14 8.2(3) . . . . ? C17 C13 C15 C14 -170.57(17) . . . . ? C14 O2 B1 F2 155.00(15) . . . . ? C14 O2 B1 F1 -82.98(19) . . . . ? C14 O2 B1 O1 36.6(2) . . . . ? C13 O1 B1 F2 -153.60(16) . . . . ? C13 O1 B1 F1 84.7(2) . . . . ? C13 O1 B1 O2 -35.0(2) . . . . ? C4 N1 C1 C2 62.9(2) . . . . ? C8 N1 C1 C2 -176.03(17) . . . . ? C6 N1 C1 C2 -55.1(2) . . . . ? N1 C1 C2 C12 178.10(16) . . . . ? C7 C3 C4 N1 173.77(16) . . . . ? C1 N1 C4 C3 59.4(2) . . . . ? C8 N1 C4 C3 -58.2(2) . . . . ? C6 N1 C4 C3 -179.39(16) . . . . ? C10 C5 C6 N1 174.82(18) . . . . ? C4 N1 C6 C5 178.42(17) . . . . ? C1 N1 C6 C5 -60.1(2) . . . . ? C8 N1 C6 C5 57.3(2) . . . . ? C4 N1 C8 C9 -53.1(2) . . . . ? C1 N1 C8 C9 -174.39(16) . . . . ? C6 N1 C8 C9 64.7(2) . . . . ? N1 C8 C9 C11 -176.11(19) . . . . ? C23 C27 O4 C29 -63.6(2) . . . . ? C25 C27 O4 C29 122.55(18) . . . . ? C18 C16 N3 C17 -0.6(2) . . . . ? C33 C17 N3 C16 0.7(2) . . . . ? C13 C17 N3 C16 -177.66(18) . . . . ? C20 C21 N2 C19 0.4(2) . . . . ? C32 C19 N2 C21 -0.3(2) . . . . ? C14 C19 N2 C21 -179.67(17) . . . . ? C24 C23 O5 C30 -1.9(3) . . . . ? C27 C23 O5 C30 -179.53(17) . . . . ? C16 C18 C33 C17 0.3(2) . . . . ? N3 C17 C33 C18 -0.6(2) . . . . ? C13 C17 C33 C18 177.67(18) . . . . ? C22 C26 C31 O7 171.46(16) . . . . ? C24 C26 C31 O7 -7.6(2) . . . . ? C22 C26 C31 O6 -11.0(2) . . . . ? C24 C26 C31 O6 170.00(15) . . . . ? N2 C19 C32 C20 0.2(2) . . . . ? C14 C19 C32 C20 179.46(18) . . . . ? C21 C20 C32 C19 0.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.212 _refine_diff_density_min -0.176 _refine_diff_density_rms 0.038