Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'N. Norman' 'C. Russell' 'R.Angharad, Baber' 'Jonathan Charmant' 'Alistair J. R. Cook' 'Natalie E. Farthing' 'Mairi F. Haddow' 'A. Orpen' John M. Slattery' _publ_contact_author_name 'Nicholas Norman' _publ_contact_author_address ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_email N.C.NORMAN@BRISTOL.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Primary Amido Substituted Diborane(4) Compounds and Imidodiborate(4) Anions ; data_2 _database_code_depnum_ccdc_archive 'CCDC 277645' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C24 H24 B2 N4' _chemical_formula_sum 'C24 H24 B2 N4' _chemical_formula_weight 390.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.484(11) _cell_length_b 11.494(9) _cell_length_c 15.965(12) _cell_angle_alpha 83.96(4) _cell_angle_beta 75.16(4) _cell_angle_gamma 89.92(5) _cell_volume 2025(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 144 _cell_measurement_theta_min 5.466 _cell_measurement_theta_max 69.971 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method none _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.847 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15811 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 70.24 _reflns_number_total 6860 _reflns_number_gt 4711 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^] 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_number_reflns 6860 _refine_ls_number_parameters 573 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.47599(19) 0.4580(2) 0.25245(14) 0.0187(5) Uani 1 1 d . . . B2 B 0.58298(19) 0.35433(19) 0.25203(14) 0.0172(4) Uani 1 1 d . . . B3 B -0.0112(2) 0.86113(19) 0.24781(14) 0.0170(4) Uani 1 1 d . . . B4 B 0.09293(19) 0.96777(19) 0.24779(14) 0.0172(4) Uani 1 1 d . . . N1 N 0.35065(15) 0.43851(14) 0.29368(11) 0.0191(4) Uani 1 1 d . . . H1A H 0.306(2) 0.501(2) 0.2856(16) 0.037(7) Uiso 1 1 d . . . N2 N 0.50431(14) 0.57390(15) 0.21114(11) 0.0187(4) Uani 1 1 d . . . H2A H 0.4462(19) 0.6230(19) 0.2210(13) 0.017(5) Uiso 1 1 d . . . N3 N 0.67847(15) 0.36502(15) 0.29287(11) 0.0191(4) Uani 1 1 d . . . H3A H 0.735(2) 0.313(2) 0.2811(15) 0.031(7) Uiso 1 1 d . . . N4 N 0.58709(14) 0.24928(14) 0.21129(11) 0.0187(4) Uani 1 1 d . . . H4A H 0.641(2) 0.194(2) 0.2208(14) 0.026(6) Uiso 1 1 d . . . N5 N 0.01728(14) 0.75584(14) 0.20744(11) 0.0194(4) Uani 1 1 d . . . H5A H -0.045(2) 0.705(2) 0.2172(15) 0.032(6) Uiso 1 1 d . . . N6 N -0.13678(14) 0.86752(14) 0.28824(11) 0.0192(4) Uani 1 1 d . . . H6A H -0.183(2) 0.811(2) 0.2829(16) 0.040(7) Uiso 1 1 d . . . N7 N 0.09343(14) 1.08343(14) 0.20585(11) 0.0194(4) Uani 1 1 d . . . H7A H 0.150(2) 1.136(2) 0.2157(16) 0.036(7) Uiso 1 1 d . . . N8 N 0.18739(14) 0.94936(14) 0.29007(10) 0.0186(3) Uani 1 1 d . . . H8A H 0.246(2) 1.002(2) 0.2790(14) 0.025(6) Uiso 1 1 d . . . C1 C 0.28310(17) 0.33995(17) 0.33988(12) 0.0187(4) Uani 1 1 d . . . C2 C 0.33388(17) 0.24390(18) 0.37696(13) 0.0219(4) Uani 1 1 d . . . H2 H 0.4185 0.2431 0.3703 0.026 Uiso 1 1 calc R . . C3 C 0.26253(18) 0.15011(18) 0.42315(13) 0.0241(4) Uani 1 1 d . . . H3 H 0.2986 0.0853 0.4478 0.029 Uiso 1 1 calc R . . C4 C 0.13890(19) 0.14915(18) 0.43405(13) 0.0252(5) Uani 1 1 d . . . H4 H 0.0902 0.0844 0.4659 0.030 Uiso 1 1 calc R . . C5 C 0.08775(18) 0.24368(19) 0.39791(14) 0.0268(5) Uani 1 1 d . . . H5 H 0.0031 0.2441 0.4049 0.032 Uiso 1 1 calc R . . C6 C 0.15899(17) 0.33835(19) 0.35137(13) 0.0236(4) Uani 1 1 d . . . H6 H 0.1224 0.4030 0.3270 0.028 Uiso 1 1 calc R . . C7 C 0.61504(17) 0.62783(17) 0.16434(12) 0.0181(4) Uani 1 1 d . . . C8 C 0.63148(17) 0.74775(17) 0.16475(12) 0.0207(4) Uani 1 1 d . . . H8 H 0.5677 0.7915 0.1960 0.025 Uiso 1 1 calc R . . C9 C 0.73938(18) 0.80412(18) 0.12024(13) 0.0238(4) Uani 1 1 d . . . H9 H 0.7493 0.8859 0.1217 0.029 Uiso 1 1 calc R . . C10 C 0.83283(18) 0.74211(18) 0.07367(13) 0.0234(4) Uani 1 1 d . . . H10 H 0.9071 0.7805 0.0432 0.028 Uiso 1 1 calc R . . C11 C 0.81621(18) 0.62306(18) 0.07230(13) 0.0232(4) Uani 1 1 d . . . H11 H 0.8800 0.5796 0.0408 0.028 Uiso 1 1 calc R . . C12 C 0.70777(18) 0.56627(17) 0.11634(13) 0.0216(4) Uani 1 1 d . . . H12 H 0.6972 0.4849 0.1135 0.026 Uiso 1 1 calc R . . C13 C 0.71090(17) 0.45355(16) 0.33773(12) 0.0179(4) Uani 1 1 d . . . C14 C 0.62681(18) 0.52564(17) 0.38418(12) 0.0214(4) Uani 1 1 d . . . H14 H 0.5439 0.5161 0.3864 0.026 Uiso 1 1 calc R . . C15 C 0.66385(19) 0.61169(17) 0.42740(13) 0.0240(4) Uani 1 1 d . . . H15 H 0.6057 0.6611 0.4584 0.029 Uiso 1 1 calc R . . C16 C 0.78388(19) 0.62675(17) 0.42609(13) 0.0233(4) Uani 1 1 d . . . H16 H 0.8084 0.6861 0.4556 0.028 Uiso 1 1 calc R . . C17 C 0.86720(18) 0.55395(18) 0.38120(13) 0.0240(5) Uani 1 1 d . . . H17 H 0.9498 0.5625 0.3803 0.029 Uiso 1 1 calc R . . C18 C 0.83097(17) 0.46818(18) 0.33732(13) 0.0219(4) Uani 1 1 d . . . H18 H 0.8894 0.4188 0.3066 0.026 Uiso 1 1 calc R . . C19 C 0.51264(16) 0.20347(17) 0.16452(12) 0.0178(4) Uani 1 1 d . . . C20 C 0.43735(17) 0.27202(18) 0.12554(12) 0.0212(4) Uani 1 1 d . . . H20 H 0.4338 0.3537 0.1305 0.025 Uiso 1 1 calc R . . C21 C 0.36702(17) 0.22132(19) 0.07925(13) 0.0234(4) Uani 1 1 d . . . H21 H 0.3150 0.2686 0.0533 0.028 Uiso 1 1 calc R . . C22 C 0.37199(18) 0.10249(18) 0.07046(13) 0.0245(5) Uani 1 1 d . . . H22 H 0.3238 0.0684 0.0387 0.029 Uiso 1 1 calc R . . C23 C 0.44754(18) 0.03472(18) 0.10823(13) 0.0249(5) Uani 1 1 d . . . H23 H 0.4517 -0.0467 0.1023 0.030 Uiso 1 1 calc R . . C24 C 0.51783(18) 0.08409(17) 0.15492(13) 0.0214(4) Uani 1 1 d . . . H24 H 0.5698 0.0363 0.1805 0.026 Uiso 1 1 calc R . . C25 C 0.12540(17) 0.70961(17) 0.16248(12) 0.0180(4) Uani 1 1 d . . . C26 C 0.12769(18) 0.59042(17) 0.15235(13) 0.0220(4) Uani 1 1 d . . . H26 H 0.0572 0.5428 0.1771 0.026 Uiso 1 1 calc R . . C27 C 0.23113(19) 0.54074(18) 0.10672(13) 0.0259(5) Uani 1 1 d . . . H27 H 0.2311 0.4595 0.1004 0.031 Uiso 1 1 calc R . . C28 C 0.33441(18) 0.60815(19) 0.07024(13) 0.0246(4) Uani 1 1 d . . . H28 H 0.4056 0.5738 0.0392 0.029 Uiso 1 1 calc R . . C29 C 0.33288(17) 0.72698(19) 0.07944(13) 0.0235(4) Uani 1 1 d . . . H29 H 0.4033 0.7743 0.0538 0.028 Uiso 1 1 calc R . . C30 C 0.22974(17) 0.77743(18) 0.12554(13) 0.0220(4) Uani 1 1 d . . . H30 H 0.2303 0.8586 0.1319 0.026 Uiso 1 1 calc R . . C31 C -0.20735(16) 0.95133(16) 0.33385(12) 0.0170(4) Uani 1 1 d . . . C32 C -0.33167(17) 0.94526(18) 0.34477(13) 0.0219(4) Uani 1 1 d . . . H32 H -0.3657 0.8857 0.3207 0.026 Uiso 1 1 calc R . . C33 C -0.40587(18) 1.02456(19) 0.39000(13) 0.0246(5) Uani 1 1 d . . . H33 H -0.4903 1.0193 0.3964 0.029 Uiso 1 1 calc R . . C34 C -0.35888(18) 1.11187(18) 0.42627(13) 0.0232(4) Uani 1 1 d . . . H34 H -0.4103 1.1665 0.4573 0.028 Uiso 1 1 calc R . . C35 C -0.23594(18) 1.11806(17) 0.41656(13) 0.0230(4) Uani 1 1 d . . . H35 H -0.2028 1.1773 0.4415 0.028 Uiso 1 1 calc R . . C36 C -0.16036(17) 1.03920(17) 0.37109(13) 0.0207(4) Uani 1 1 d . . . H36 H -0.0760 1.0448 0.3651 0.025 Uiso 1 1 calc R . . C37 C 0.01465(16) 1.13654(17) 0.16059(12) 0.0174(4) Uani 1 1 d . . . C38 C -0.04676(17) 1.07355(17) 0.11381(13) 0.0212(4) Uani 1 1 d . . . H38 H -0.0346 0.9921 0.1114 0.025 Uiso 1 1 calc R . . C39 C -0.12513(17) 1.13018(19) 0.07116(13) 0.0238(4) Uani 1 1 d . . . H39 H -0.1682 1.0865 0.0410 0.029 Uiso 1 1 calc R . . C40 C -0.14179(18) 1.24904(19) 0.07175(13) 0.0254(5) Uani 1 1 d . . . H40 H -0.1953 1.2872 0.0419 0.030 Uiso 1 1 calc R . . C41 C -0.07922(18) 1.31208(18) 0.11663(13) 0.0250(5) Uani 1 1 d . . . H41 H -0.0897 1.3940 0.1173 0.030 Uiso 1 1 calc R . . C42 C -0.00205(17) 1.25642(17) 0.16019(13) 0.0217(4) Uani 1 1 d . . . H42 H 0.0404 1.3006 0.1904 0.026 Uiso 1 1 calc R . . C43 C 0.21762(17) 0.84881(16) 0.33699(12) 0.0180(4) Uani 1 1 d . . . C44 C 0.13088(18) 0.76498(17) 0.38415(13) 0.0211(4) Uani 1 1 d . . . H44 H 0.0483 0.7758 0.3858 0.025 Uiso 1 1 calc R . . C45 C 0.16502(19) 0.66654(18) 0.42831(13) 0.0234(4) Uani 1 1 d . . . H45 H 0.1056 0.6093 0.4592 0.028 Uiso 1 1 calc R . . C46 C 0.28431(19) 0.64974(18) 0.42848(13) 0.0240(4) Uani 1 1 d . . . H46 H 0.3071 0.5815 0.4588 0.029 Uiso 1 1 calc R . . C47 C 0.36990(18) 0.73432(18) 0.38355(13) 0.0241(4) Uani 1 1 d . . . H47 H 0.4520 0.7246 0.3838 0.029 Uiso 1 1 calc R . . C48 C 0.33695(17) 0.83255(17) 0.33843(13) 0.0202(4) Uani 1 1 d . . . H48 H 0.3967 0.8898 0.3080 0.024 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 B1 0.0201(11) 0.0209(11) 0.0181(11) -0.0054(9) -0.0092(9) -0.0025(9) B2 0.0168(10) 0.0178(11) 0.0154(11) 0.0001(9) -0.0019(9) -0.0047(9) B3 0.0201(11) 0.0185(11) 0.0142(10) 0.0001(9) -0.0081(9) 0.0028(9) B4 0.0149(10) 0.0192(11) 0.0176(11) -0.0050(9) -0.0030(9) 0.0050(9) N1 0.0186(8) 0.0155(8) 0.0254(9) -0.0026(7) -0.0093(7) 0.0019(7) N2 0.0137(8) 0.0184(8) 0.0256(9) -0.0042(7) -0.0074(7) 0.0043(7) N3 0.0185(8) 0.0177(8) 0.0240(9) -0.0060(7) -0.0092(7) 0.0037(7) N4 0.0160(8) 0.0180(8) 0.0253(9) -0.0052(7) -0.0098(7) 0.0033(7) N5 0.0166(8) 0.0187(8) 0.0240(9) -0.0050(7) -0.0064(7) -0.0018(7) N6 0.0176(8) 0.0175(8) 0.0238(9) -0.0050(7) -0.0068(7) -0.0023(7) N7 0.0171(8) 0.0191(8) 0.0240(9) -0.0013(7) -0.0090(7) -0.0015(7) N8 0.0191(8) 0.0159(8) 0.0224(9) -0.0019(7) -0.0085(7) -0.0011(7) C1 0.0186(10) 0.0196(9) 0.0186(10) -0.0075(8) -0.0038(8) -0.0021(8) C2 0.0167(10) 0.0239(10) 0.0241(11) -0.0049(9) -0.0025(8) 0.0019(8) C3 0.0275(11) 0.0201(10) 0.0234(11) -0.0041(9) -0.0034(9) 0.0014(9) C4 0.0276(11) 0.0234(10) 0.0232(11) -0.0055(9) -0.0030(9) -0.0088(9) C5 0.0179(10) 0.0356(12) 0.0281(11) -0.0059(10) -0.0071(9) -0.0059(9) C6 0.0194(10) 0.0285(11) 0.0254(11) -0.0049(9) -0.0092(8) 0.0005(9) C7 0.0176(9) 0.0204(10) 0.0184(10) -0.0014(8) -0.0090(8) 0.0001(8) C8 0.0214(10) 0.0210(10) 0.0207(10) -0.0047(8) -0.0062(8) 0.0012(8) C9 0.0273(11) 0.0197(10) 0.0257(11) -0.0019(9) -0.0094(9) -0.0060(9) C10 0.0195(10) 0.0291(11) 0.0205(10) 0.0054(9) -0.0063(8) -0.0067(9) C11 0.0201(10) 0.0263(11) 0.0224(11) -0.0005(9) -0.0052(8) 0.0064(9) C12 0.0248(10) 0.0179(9) 0.0227(10) -0.0007(8) -0.0076(9) 0.0022(8) C13 0.0228(10) 0.0149(9) 0.0173(9) 0.0003(8) -0.0086(8) -0.0020(8) C14 0.0219(10) 0.0241(10) 0.0221(10) -0.0042(9) -0.0121(8) 0.0018(9) C15 0.0328(11) 0.0202(10) 0.0213(10) -0.0033(8) -0.0109(9) 0.0052(9) C16 0.0330(11) 0.0177(10) 0.0226(10) -0.0020(8) -0.0135(9) -0.0055(9) C17 0.0210(10) 0.0278(11) 0.0259(11) -0.0014(9) -0.0112(9) -0.0061(9) C18 0.0205(10) 0.0247(10) 0.0214(10) -0.0033(9) -0.0064(8) -0.0003(9) C19 0.0152(9) 0.0213(10) 0.0159(9) -0.0028(8) -0.0018(8) -0.0033(8) C20 0.0227(10) 0.0215(10) 0.0208(10) -0.0061(8) -0.0064(8) 0.0026(8) C21 0.0192(10) 0.0302(11) 0.0229(11) -0.0055(9) -0.0085(8) 0.0040(9) C22 0.0232(10) 0.0287(11) 0.0236(11) -0.0068(9) -0.0080(9) -0.0044(9) C23 0.0281(11) 0.0203(10) 0.0271(11) -0.0066(9) -0.0072(9) -0.0039(9) C24 0.0226(10) 0.0190(10) 0.0250(11) -0.0039(8) -0.0098(8) 0.0023(8) C25 0.0186(9) 0.0195(10) 0.0187(10) -0.0038(8) -0.0094(8) 0.0035(8) C26 0.0237(10) 0.0179(10) 0.0248(11) -0.0017(8) -0.0070(9) -0.0008(8) C27 0.0350(12) 0.0184(10) 0.0268(11) -0.0067(9) -0.0111(9) 0.0071(9) C28 0.0236(10) 0.0296(11) 0.0237(11) -0.0096(9) -0.0093(9) 0.0115(9) C29 0.0175(10) 0.0302(11) 0.0247(11) -0.0087(9) -0.0066(8) -0.0010(9) C30 0.0235(10) 0.0204(10) 0.0246(11) -0.0099(9) -0.0078(8) -0.0003(9) C31 0.0174(9) 0.0176(9) 0.0149(9) 0.0001(8) -0.0032(8) 0.0002(8) C32 0.0214(10) 0.0231(10) 0.0224(11) -0.0061(9) -0.0064(8) -0.0015(8) C33 0.0173(10) 0.0313(11) 0.0264(11) -0.0061(9) -0.0069(8) 0.0040(9) C34 0.0235(10) 0.0229(10) 0.0222(10) -0.0039(9) -0.0036(8) 0.0052(9) C35 0.0253(10) 0.0195(10) 0.0238(11) -0.0044(8) -0.0046(9) -0.0023(9) C36 0.0163(9) 0.0232(10) 0.0218(10) -0.0039(9) -0.0029(8) -0.0035(8) C37 0.0142(9) 0.0191(9) 0.0178(9) 0.0010(8) -0.0033(8) 0.0021(8) C38 0.0225(10) 0.0198(10) 0.0209(10) 0.0016(8) -0.0066(8) -0.0028(8) C39 0.0171(10) 0.0310(11) 0.0227(11) 0.0028(9) -0.0065(8) -0.0052(9) C40 0.0185(10) 0.0347(12) 0.0222(11) 0.0036(9) -0.0067(8) 0.0062(9) C41 0.0275(11) 0.0216(10) 0.0243(11) -0.0008(9) -0.0046(9) 0.0084(9) C42 0.0212(10) 0.0223(10) 0.0219(10) -0.0029(8) -0.0059(8) 0.0015(8) C43 0.0208(10) 0.0179(9) 0.0179(9) -0.0064(8) -0.0082(8) 0.0021(8) C44 0.0194(10) 0.0243(10) 0.0227(10) -0.0046(8) -0.0099(8) 0.0003(8) C45 0.0284(11) 0.0218(10) 0.0229(10) -0.0022(8) -0.0116(9) -0.0031(9) C46 0.0331(12) 0.0215(10) 0.0204(10) -0.0048(8) -0.0117(9) 0.0056(9) C47 0.0214(10) 0.0297(11) 0.0247(11) -0.0069(9) -0.0107(9) 0.0072(9) C48 0.0176(9) 0.0216(10) 0.0222(10) -0.0039(8) -0.0058(8) 0.0002(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 B1 N2 1.422(3) . ? B1 N1 1.428(3) . ? B1 B2 1.709(3) . ? B2 N3 1.424(3) . ? B2 N4 1.426(3) . ? B3 N6 1.427(3) . ? B3 N5 1.429(3) . ? B3 B4 1.713(3) . ? B4 N8 1.422(3) . ? B4 N7 1.423(3) . ? N1 C1 1.401(3) . ? N1 H1A 0.90(3) . ? N2 C7 1.406(3) . ? N2 H2A 0.87(2) . ? N3 C13 1.406(3) . ? N3 H3A 0.88(2) . ? N4 C19 1.406(2) . ? N4 H4A 0.91(2) . ? N5 C25 1.400(3) . ? N5 H5A 0.89(2) . ? N6 C31 1.399(3) . ? N6 H6A 0.86(3) . ? N7 C37 1.398(3) . ? N7 H7A 0.95(2) . ? N8 C43 1.403(3) . ? N8 H8A 0.88(2) . ? C1 C6 1.390(3) . ? C1 C2 1.395(3) . ? C2 C3 1.380(3) . ? C2 H2 0.9500 . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.378(3) . ? C4 H4 0.9500 . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.384(3) . ? C7 C8 1.393(3) . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C12 1.389(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.388(3) . ? C13 C14 1.389(3) . ? C14 C15 1.389(3) . ? C14 H14 0.9500 . ? C15 C16 1.384(3) . ? C15 H15 0.9500 . ? C16 C17 1.379(3) . ? C16 H16 0.9500 . ? C17 C18 1.390(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.388(3) . ? C19 C24 1.396(3) . ? C20 C21 1.391(3) . ? C20 H20 0.9500 . ? C21 C22 1.387(3) . ? C21 H21 0.9500 . ? C22 C23 1.375(3) . ? C22 H22 0.9500 . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.391(3) . ? C25 C26 1.396(3) . ? C26 C27 1.382(3) . ? C26 H26 0.9500 . ? C27 C28 1.378(3) . ? C27 H27 0.9500 . ? C28 C29 1.389(3) . ? C28 H28 0.9500 . ? C29 C30 1.386(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.394(3) . ? C31 C36 1.399(3) . ? C32 C33 1.378(3) . ? C32 H32 0.9500 . ? C33 C34 1.385(3) . ? C33 H33 0.9500 . ? C34 C35 1.381(3) . ? C34 H34 0.9500 . ? C35 C36 1.384(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.391(3) . ? C37 C38 1.402(3) . ? C38 C39 1.384(3) . ? C38 H38 0.9500 . ? C39 C40 1.380(3) . ? C39 H39 0.9500 . ? C40 C41 1.389(3) . ? C40 H40 0.9500 . ? C41 C42 1.378(3) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.389(3) . ? C43 C44 1.398(3) . ? C44 C45 1.380(3) . ? C44 H44 0.9500 . ? C45 C46 1.384(3) . ? C45 H45 0.9500 . ? C46 C47 1.386(3) . ? C46 H46 0.9500 . ? C47 C48 1.380(3) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 B1 N1 113.11(19) . . ? N2 B1 B2 122.54(18) . . ? N1 B1 B2 124.35(18) . . ? N3 B2 N4 112.87(18) . . ? N3 B2 B1 122.76(17) . . ? N4 B2 B1 124.38(17) . . ? N6 B3 N5 112.15(17) . . ? N6 B3 B4 123.70(17) . . ? N5 B3 B4 124.15(18) . . ? N8 B4 N7 113.30(17) . . ? N8 B4 B3 123.16(18) . . ? N7 B4 B3 123.54(17) . . ? C1 N1 B1 132.79(18) . . ? C1 N1 H1A 113.7(15) . . ? B1 N1 H1A 113.4(15) . . ? C7 N2 B1 130.93(18) . . ? C7 N2 H2A 112.7(13) . . ? B1 N2 H2A 115.9(13) . . ? C13 N3 B2 132.19(18) . . ? C13 N3 H3A 112.4(15) . . ? B2 N3 H3A 114.6(15) . . ? C19 N4 B2 132.21(18) . . ? C19 N4 H4A 108.8(14) . . ? B2 N4 H4A 118.5(14) . . ? C25 N5 B3 133.26(17) . . ? C25 N5 H5A 112.3(15) . . ? B3 N5 H5A 114.1(15) . . ? C31 N6 B3 133.56(17) . . ? C31 N6 H6A 109.3(17) . . ? B3 N6 H6A 117.0(17) . . ? C37 N7 B4 130.73(17) . . ? C37 N7 H7A 113.6(15) . . ? B4 N7 H7A 115.2(15) . . ? C43 N8 B4 130.46(17) . . ? C43 N8 H8A 109.9(15) . . ? B4 N8 H8A 118.6(15) . . ? C6 C1 C2 118.04(19) . . ? C6 C1 N1 118.70(19) . . ? C2 C1 N1 123.24(18) . . ? C3 C2 C1 120.69(19) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 120.9(2) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 118.94(19) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 120.5(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 121.0(2) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C12 C7 C8 118.66(18) . . ? C12 C7 N2 122.30(18) . . ? C8 C7 N2 119.03(18) . . ? C9 C8 C7 120.92(19) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 120.4(2) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 118.83(19) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C10 C11 C12 121.0(2) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C7 C12 C11 120.2(2) . . ? C7 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C18 C13 C14 118.49(18) . . ? C18 C13 N3 119.01(18) . . ? C14 C13 N3 122.48(18) . . ? C13 C14 C15 120.08(19) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 121.23(19) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C17 C16 C15 118.75(18) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C16 C17 C18 120.36(19) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 121.08(19) . . ? C13 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C20 C19 C24 118.81(18) . . ? C20 C19 N4 123.01(18) . . ? C24 C19 N4 118.15(18) . . ? C19 C20 C21 120.09(19) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.8(2) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C23 C22 C21 119.16(19) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 120.6(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C19 120.49(19) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C30 C25 C26 118.46(18) . . ? C30 C25 N5 123.10(18) . . ? C26 C25 N5 118.42(17) . . ? C27 C26 C25 120.86(19) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 120.5(2) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.06(19) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C30 C29 C28 120.79(19) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C25 120.3(2) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? C32 C31 C36 118.10(18) . . ? C32 C31 N6 118.29(17) . . ? C36 C31 N6 123.59(18) . . ? C33 C32 C31 120.88(18) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 120.82(19) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C35 C34 C33 118.80(19) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C35 C36 120.98(19) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 120.41(19) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C42 C37 N7 119.22(17) . . ? C42 C37 C38 118.47(18) . . ? N7 C37 C38 122.30(18) . . ? C39 C38 C37 119.94(19) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C40 C39 C38 121.10(19) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 119.1(2) . . ? C39 C40 H40 120.5 . . ? C41 C40 H40 120.5 . . ? C42 C41 C40 120.3(2) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C37 121.05(19) . . ? C41 C42 H42 119.5 . . ? C37 C42 H42 119.5 . . ? C48 C43 C44 118.57(19) . . ? C48 C43 N8 119.33(17) . . ? C44 C43 N8 122.09(18) . . ? C45 C44 C43 120.07(19) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 121.16(19) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C45 C46 C47 118.8(2) . . ? C45 C46 H46 120.6 . . ? C47 C46 H46 120.6 . . ? C48 C47 C46 120.6(2) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C43 120.83(19) . . ? C47 C48 H48 119.6 . . ? C43 C48 H48 119.6 . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 70.24 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 0.257 _refine_diff_density_min -0.213 _refine_diff_density_rms 0.043 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 277646' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 B2 N4' _chemical_formula_sum 'C32 H40 B2 N4' _chemical_formula_weight 502.30 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 19.740(4) _cell_length_b 8.8681(18) _cell_length_c 16.550(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2897.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 94 _cell_measurement_theta_min 2.462 _cell_measurement_theta_max 22.185 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.891152 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS V2.05 (Bruker AXS, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19501 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3334 _reflns_number_gt 2499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _computing_publication_material 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _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^)+(0.0366P)^2^+1.8282P] 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 3334 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.71504(9) 0.1910(2) 0.16664(11) 0.0183(4) Uani 1 1 d . . . N1 N 0.72006(7) 0.03273(16) 0.15530(9) 0.0201(3) Uani 1 1 d . . . N2 N 0.64822(7) 0.25007(17) 0.17797(9) 0.0208(3) Uani 1 1 d . . . C1 C 0.77944(8) -0.05444(18) 0.13910(10) 0.0191(3) Uani 1 1 d . . . C2 C 0.81686(8) -0.11335(19) 0.20356(10) 0.0205(4) Uani 1 1 d . . . C3 C 0.87400(8) -0.20007(19) 0.18670(11) 0.0234(4) Uani 1 1 d . . . H3 H 0.8993 -0.2399 0.2290 0.028 Uiso 1 1 calc R . . C4 C 0.89356(9) -0.2277(2) 0.10790(12) 0.0272(4) Uani 1 1 d . . . H4 H 0.9316 -0.2863 0.0974 0.033 Uiso 1 1 calc R . . C5 C 0.85650(9) -0.1683(2) 0.04471(11) 0.0273(4) Uani 1 1 d . . . H5 H 0.8700 -0.1872 -0.0082 0.033 Uiso 1 1 calc R . . C6 C 0.79911(8) -0.08032(19) 0.05897(11) 0.0229(4) Uani 1 1 d . . . C7 C 0.79604(9) -0.0821(2) 0.28951(11) 0.0251(4) Uani 1 1 d . . . H7A H 0.8254 -0.1358 0.3257 0.038 Uiso 1 1 calc R . . H7B H 0.7502 -0.1147 0.2976 0.038 Uiso 1 1 calc R . . H7C H 0.7993 0.0241 0.3000 0.038 Uiso 1 1 calc R . . C8 C 0.75967(10) -0.0139(2) -0.00995(11) 0.0331(5) Uani 1 1 d . . . H8A H 0.7801 -0.0432 -0.0602 0.050 Uiso 1 1 calc R . . H8B H 0.7598 0.0941 -0.0056 0.050 Uiso 1 1 calc R . . H8C H 0.7138 -0.0500 -0.0081 0.050 Uiso 1 1 calc R . . C9 C 0.58674(8) 0.16497(18) 0.17421(11) 0.0200(4) Uani 1 1 d . . . C11 C 0.50793(9) -0.0099(2) 0.23314(12) 0.0284(4) Uani 1 1 d . . . H11 H 0.4948 -0.0712 0.2759 0.034 Uiso 1 1 calc R . . C10 C 0.56702(8) 0.07539(19) 0.23998(11) 0.0228(4) Uani 1 1 d . . . C12 C 0.46864(9) -0.0053(2) 0.16455(13) 0.0313(5) Uani 1 1 d . . . H12 H 0.4297 -0.0639 0.1611 0.038 Uiso 1 1 calc R . . C13 C 0.48724(8) 0.0865(2) 0.10087(12) 0.0289(4) Uani 1 1 d . . . H13 H 0.4599 0.0912 0.0552 0.035 Uiso 1 1 calc R . . C14 C 0.54641(8) 0.1723(2) 0.10408(11) 0.0249(4) Uani 1 1 d . . . C15 C 0.56737(10) 0.2701(2) 0.03452(12) 0.0364(5) Uani 1 1 d . . . H15A H 0.5368 0.2549 -0.0099 0.055 Uiso 1 1 calc R . . H15B H 0.6125 0.2440 0.0182 0.055 Uiso 1 1 calc R . . H15C H 0.5662 0.3740 0.0507 0.055 Uiso 1 1 calc R . . C16 C 0.60801(10) 0.0697(2) 0.31661(11) 0.0314(4) Uani 1 1 d . . . H16A H 0.6469 0.0065 0.3086 0.047 Uiso 1 1 calc R . . H16B H 0.5807 0.0293 0.3595 0.047 Uiso 1 1 calc R . . H16C H 0.6225 0.1697 0.3306 0.047 Uiso 1 1 calc R . . H17 H 0.6823(11) -0.021(2) 0.1520(13) 0.040(6) Uiso 1 1 d . . . H18 H 0.6413(10) 0.347(3) 0.1725(13) 0.041(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0186(8) 0.0198(9) 0.0164(9) 0.0015(7) -0.0004(7) -0.0010(7) N1 0.0153(7) 0.0178(7) 0.0274(8) -0.0003(6) 0.0022(6) -0.0022(6) N2 0.0168(6) 0.0152(7) 0.0303(8) -0.0003(6) 0.0006(6) -0.0022(6) C1 0.0177(8) 0.0132(7) 0.0265(9) -0.0022(6) 0.0021(7) -0.0036(6) C2 0.0203(8) 0.0161(8) 0.0249(9) -0.0022(7) 0.0016(7) -0.0048(7) C3 0.0209(8) 0.0175(8) 0.0318(10) 0.0015(7) -0.0017(7) -0.0026(7) C4 0.0228(8) 0.0197(9) 0.0391(11) -0.0054(8) 0.0058(7) 0.0008(7) C5 0.0284(9) 0.0260(9) 0.0274(9) -0.0067(8) 0.0093(7) -0.0019(8) C6 0.0222(8) 0.0200(9) 0.0267(9) -0.0019(7) 0.0004(7) -0.0046(7) C7 0.0239(8) 0.0260(10) 0.0253(9) 0.0015(7) 0.0006(7) -0.0003(7) C8 0.0336(10) 0.0403(12) 0.0253(9) 0.0008(9) 0.0000(8) -0.0003(9) C9 0.0135(7) 0.0155(8) 0.0311(9) -0.0035(7) 0.0037(7) 0.0022(6) C11 0.0231(9) 0.0214(9) 0.0407(11) 0.0012(8) 0.0142(8) 0.0016(7) C10 0.0193(8) 0.0190(8) 0.0302(9) -0.0026(7) 0.0080(7) 0.0041(7) C12 0.0161(8) 0.0228(10) 0.0548(13) -0.0070(9) 0.0069(8) -0.0023(7) C13 0.0185(8) 0.0254(10) 0.0428(11) -0.0051(8) -0.0064(8) 0.0023(7) C14 0.0200(8) 0.0206(9) 0.0340(10) -0.0017(7) 0.0003(7) 0.0011(7) C15 0.0337(10) 0.0394(12) 0.0362(11) 0.0072(9) -0.0107(8) -0.0068(9) C16 0.0334(10) 0.0327(11) 0.0281(10) 0.0038(8) 0.0067(8) 0.0000(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 B1 N1 1.420(2) . ? B1 N2 1.431(2) . ? B1 B1 1.732(4) 2_655 ? N1 C1 1.429(2) . ? N1 H17 0.88(2) . ? N2 C9 1.431(2) . ? N2 H18 0.87(2) . ? C1 C2 1.399(2) . ? C1 C6 1.401(2) . ? C2 C3 1.393(2) . ? C2 C7 1.506(2) . ? C3 C4 1.382(3) . ? C3 H3 0.9300 . ? C4 C5 1.381(3) . ? C4 H4 0.9300 . ? C5 C6 1.395(2) . ? C5 H5 0.9300 . ? C6 C8 1.501(3) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.403(2) . ? C9 C14 1.409(2) . ? C11 C12 1.375(3) . ? C11 C10 1.395(2) . ? C11 H11 0.9300 . ? C10 C16 1.505(3) . ? C12 C13 1.382(3) . ? C12 H12 0.9300 . ? C13 C14 1.395(2) . ? C13 H13 0.9300 . ? C14 C15 1.500(3) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 N1 B1 N2 116.32(15) . . ? N1 B1 B1 122.79(18) . 2_655 ? N2 B1 B1 120.88(18) . 2_655 ? B1 N1 C1 128.08(14) . . ? B1 N1 H17 118.7(14) . . ? C1 N1 H17 112.8(14) . . ? B1 N2 C9 125.66(15) . . ? B1 N2 H18 119.3(14) . . ? C9 N2 H18 112.4(14) . . ? C2 C1 C6 120.96(15) . . ? C2 C1 N1 119.46(15) . . ? C6 C1 N1 119.58(15) . . ? C3 C2 C1 118.74(16) . . ? C3 C2 C7 120.75(15) . . ? C1 C2 C7 120.50(15) . . ? C4 C3 C2 120.87(16) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.92(16) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 121.02(17) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 118.48(16) . . ? C5 C6 C8 120.78(16) . . ? C1 C6 C8 120.74(15) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 120.58(15) . . ? C10 C9 N2 120.02(15) . . ? C14 C9 N2 119.39(15) . . ? C12 C11 C10 121.51(18) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C10 C9 118.43(17) . . ? C11 C10 C16 119.99(17) . . ? C9 C10 C16 121.58(15) . . ? C11 C12 C13 119.80(17) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C14 120.99(18) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C9 118.63(17) . . ? C13 C14 C15 121.14(17) . . ? C9 C14 C15 120.22(15) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 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 N2 B1 N1 C1 176.86(15) . . . . ? B1 B1 N1 C1 -2.9(2) 2_655 . . . ? N1 B1 N2 C9 -3.8(2) . . . . ? B1 B1 N2 C9 175.97(12) 2_655 . . . ? B1 N1 C1 C2 90.2(2) . . . . ? B1 N1 C1 C6 -90.2(2) . . . . ? C6 C1 C2 C3 -0.7(2) . . . . ? N1 C1 C2 C3 178.99(14) . . . . ? C6 C1 C2 C7 178.73(15) . . . . ? N1 C1 C2 C7 -1.6(2) . . . . ? C1 C2 C3 C4 0.0(2) . . . . ? C7 C2 C3 C4 -179.40(16) . . . . ? C2 C3 C4 C5 0.4(3) . . . . ? C3 C4 C5 C6 -0.1(3) . . . . ? C4 C5 C6 C1 -0.5(3) . . . . ? C4 C5 C6 C8 179.00(17) . . . . ? C2 C1 C6 C5 0.9(2) . . . . ? N1 C1 C6 C5 -178.73(15) . . . . ? C2 C1 C6 C8 -178.60(16) . . . . ? N1 C1 C6 C8 1.7(2) . . . . ? B1 N2 C9 C10 78.4(2) . . . . ? B1 N2 C9 C14 -101.7(2) . . . . ? C12 C11 C10 C9 -1.2(3) . . . . ? C12 C11 C10 C16 178.85(16) . . . . ? C14 C9 C10 C11 2.2(2) . . . . ? N2 C9 C10 C11 -177.93(15) . . . . ? C14 C9 C10 C16 -177.91(16) . . . . ? N2 C9 C10 C16 2.0(2) . . . . ? C10 C11 C12 C13 -0.7(3) . . . . ? C11 C12 C13 C14 1.7(3) . . . . ? C12 C13 C14 C9 -0.7(3) . . . . ? C12 C13 C14 C15 178.95(18) . . . . ? C10 C9 C14 C13 -1.2(2) . . . . ? N2 C9 C14 C13 178.86(15) . . . . ? C10 C9 C14 C15 179.12(16) . . . . ? N2 C9 C14 C15 -0.8(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.343 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.046 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 277647' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C48 H68 B2 Li4 N4 O6' _chemical_formula_sum 'C48 H68 B2 Li4 N4 O6' _chemical_formula_weight 846.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Li Li -0.0003 0.0001 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.9789(8) _cell_length_b 13.8833(6) _cell_length_c 19.6293(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4899.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 157 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method none _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _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 'CCD Area Detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30851 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5620 _reflns_number_gt 3436 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+1.0443P] 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_number_reflns 5620 _refine_ls_number_parameters 427 _refine_ls_number_restraints 217 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B -0.00914(11) 0.54572(13) -0.03070(9) 0.0348(4) Uani 1 1 d . . . C100 C 0.09223(9) 0.43369(12) 0.13502(8) 0.0343(4) Uani 1 1 d . . . C101 C 0.12236(10) 0.34171(12) 0.12227(9) 0.0417(4) Uani 1 1 d . . . H101 H 0.1132 0.3116 0.0796 0.050 Uiso 1 1 calc R . . C102 C 0.16497(11) 0.29415(14) 0.17035(11) 0.0502(5) Uani 1 1 d . . . H102 H 0.1847 0.2324 0.1599 0.060 Uiso 1 1 calc R . . C103 C 0.17942(10) 0.33466(14) 0.23334(10) 0.0497(5) Uani 1 1 d . . . H103 H 0.2088 0.3016 0.2661 0.060 Uiso 1 1 calc R . . C104 C 0.15020(9) 0.42417(14) 0.24746(9) 0.0452(4) Uani 1 1 d . . . H104 H 0.1594 0.4530 0.2905 0.054 Uiso 1 1 calc R . . C105 C 0.10776(9) 0.47254(12) 0.19983(8) 0.0390(4) Uani 1 1 d . . . H105 H 0.0884 0.5342 0.2111 0.047 Uiso 1 1 calc R . . C106 C 0.03339(8) 0.71791(11) -0.05443(8) 0.0326(4) Uani 1 1 d . . . C107 C 0.02580(9) 0.81074(12) -0.02749(9) 0.0376(4) Uani 1 1 d . . . H107 H 0.0116 0.8178 0.0189 0.045 Uiso 1 1 calc R . . C108 C 0.03824(10) 0.89246(13) -0.06608(10) 0.0458(5) Uani 1 1 d . . . H108 H 0.0319 0.9541 -0.0459 0.055 Uiso 1 1 calc R . . C109 C 0.05956(11) 0.88587(13) -0.13289(10) 0.0500(5) Uani 1 1 d . . . H109 H 0.0682 0.9422 -0.1592 0.060 Uiso 1 1 calc R . . C110 C 0.06812(13) 0.79567(14) -0.16089(10) 0.0567(5) Uani 1 1 d . . . H110 H 0.0831 0.7897 -0.2071 0.068 Uiso 1 1 calc R . . C111 C 0.05518(12) 0.71339(13) -0.12275(10) 0.0499(5) Uani 1 1 d . . . H111 H 0.0613 0.6522 -0.1436 0.060 Uiso 1 1 calc R . . Li1 Li 0.10908(16) 0.5688(2) 0.02355(16) 0.0468(7) Uani 1 1 d . . . Li2 Li 0.00145(16) 0.6206(2) 0.08934(14) 0.0389(7) Uani 1 1 d . . . N1 N 0.05382(8) 0.48719(9) 0.08707(7) 0.0363(3) Uani 1 1 d . . . N2 N 0.02312(8) 0.63773(9) -0.01337(7) 0.0357(3) Uani 1 1 d . A . O1 O 0.2127(5) 0.5920(5) 0.0246(5) 0.0450(16) Uani 0.51(2) 1 d PDU A 1 C10 C 0.2554(5) 0.6653(6) -0.0081(5) 0.0529(19) Uani 0.51(2) 1 d PDU A 1 H10A H 0.2580 0.7238 0.0206 0.064 Uiso 0.51(2) 1 calc PR A 1 H10B H 0.2335 0.6825 -0.0527 0.064 Uiso 0.51(2) 1 calc PR A 1 C11 C 0.3322(5) 0.6207(11) -0.0170(6) 0.067(3) Uani 0.51(2) 1 d PDU A 1 H11A H 0.3366 0.5887 -0.0619 0.080 Uiso 0.51(2) 1 calc PR A 1 H11B H 0.3715 0.6703 -0.0130 0.080 Uiso 0.51(2) 1 calc PR A 1 C12 C 0.3375(6) 0.5491(12) 0.0396(8) 0.098(4) Uani 0.51(2) 1 d PDU A 1 H12A H 0.3559 0.4866 0.0221 0.118 Uiso 0.51(2) 1 calc PR A 1 H12B H 0.3723 0.5723 0.0751 0.118 Uiso 0.51(2) 1 calc PR A 1 C13 C 0.2619(7) 0.5381(8) 0.0680(7) 0.061(2) Uani 0.51(2) 1 d PDU A 1 H13A H 0.2474 0.4693 0.0688 0.073 Uiso 0.51(2) 1 calc PR A 1 H13B H 0.2600 0.5634 0.1152 0.073 Uiso 0.51(2) 1 calc PR A 1 O1' O 0.2109(6) 0.5862(8) 0.0125(8) 0.100(4) Uani 0.49(2) 1 d PDU A 2 C10' C 0.2464(7) 0.6646(9) -0.0233(9) 0.114(5) Uani 0.49(2) 1 d PDU A 2 H10C H 0.2402 0.7260 0.0018 0.137 Uiso 0.49(2) 1 calc PR A 2 H10D H 0.2253 0.6721 -0.0696 0.137 Uiso 0.49(2) 1 calc PR A 2 C11' C 0.3258(7) 0.6368(14) -0.0267(9) 0.105(5) Uani 0.49(2) 1 d PDU A 2 H11C H 0.3582 0.6945 -0.0278 0.126 Uiso 0.49(2) 1 calc PR A 2 H11D H 0.3358 0.5972 -0.0676 0.126 Uiso 0.49(2) 1 calc PR A 2 C12' C 0.3388(7) 0.5783(11) 0.0388(8) 0.093(4) Uani 0.49(2) 1 d PDU A 2 H12C H 0.3799 0.5315 0.0332 0.112 Uiso 0.49(2) 1 calc PR A 2 H12D H 0.3494 0.6206 0.0782 0.112 Uiso 0.49(2) 1 calc PR A 2 C13' C 0.2663(7) 0.5292(10) 0.0462(10) 0.090(4) Uani 0.49(2) 1 d PDU A 2 H13C H 0.2686 0.4643 0.0256 0.108 Uiso 0.49(2) 1 calc PR A 2 H13D H 0.2537 0.5222 0.0951 0.108 Uiso 0.49(2) 1 calc PR A 2 O2 O 0.0437(6) 0.7231(8) 0.1525(11) 0.0372(16) Uani 0.641(10) 1 d PDU B 1 C20 C 0.1195(5) 0.7517(5) 0.1415(6) 0.0474(19) Uani 0.641(10) 1 d PDU B 1 H20A H 0.1296 0.7594 0.0922 0.057 Uiso 0.641(10) 1 calc PR B 1 H20B H 0.1541 0.7030 0.1602 0.057 Uiso 0.641(10) 1 calc PR B 1 C21 C 0.1285(2) 0.8461(3) 0.1778(3) 0.0548(14) Uani 0.641(10) 1 d PDU B 1 H21A H 0.1674 0.8864 0.1563 0.066 Uiso 0.641(10) 1 calc PR B 1 H21B H 0.1409 0.8365 0.2265 0.066 Uiso 0.641(10) 1 calc PR B 1 C22 C 0.0518(4) 0.8904(5) 0.1693(4) 0.0550(16) Uani 0.641(10) 1 d PDU B 1 H22A H 0.0416 0.9383 0.2054 0.066 Uiso 0.641(10) 1 calc PR B 1 H22B H 0.0468 0.9218 0.1242 0.066 Uiso 0.641(10) 1 calc PR B 1 C23 C 0.0007(5) 0.8050(6) 0.1752(8) 0.0432(17) Uani 0.641(10) 1 d PDU B 1 H23A H -0.0156 0.7961 0.2230 0.052 Uiso 0.641(10) 1 calc PR B 1 H23B H -0.0439 0.8137 0.1462 0.052 Uiso 0.641(10) 1 calc PR B 1 O2' O 0.0502(13) 0.7228(16) 0.142(2) 0.046(5) Uani 0.359(10) 1 d PDU B 2 C20' C 0.1295(12) 0.7438(9) 0.1409(14) 0.071(5) Uani 0.359(10) 1 d PDU B 2 H20C H 0.1537 0.7131 0.1011 0.085 Uiso 0.359(10) 1 calc PR B 2 H20D H 0.1543 0.7216 0.1831 0.085 Uiso 0.359(10) 1 calc PR B 2 C21' C 0.1318(4) 0.8522(6) 0.1352(6) 0.071(3) Uani 0.359(10) 1 d PDU B 2 H21C H 0.1197 0.8740 0.0885 0.085 Uiso 0.359(10) 1 calc PR B 2 H21D H 0.1809 0.8781 0.1487 0.085 Uiso 0.359(10) 1 calc PR B 2 C22' C 0.0715(8) 0.8810(10) 0.1856(7) 0.067(3) Uani 0.359(10) 1 d PDU B 2 H22C H 0.0892 0.8763 0.2332 0.081 Uiso 0.359(10) 1 calc PR B 2 H22D H 0.0532 0.9471 0.1768 0.081 Uiso 0.359(10) 1 calc PR B 2 C23' C 0.0128(9) 0.8066(14) 0.1703(13) 0.052(4) Uani 0.359(10) 1 d PDU B 2 H23C H -0.0142 0.7890 0.2125 0.063 Uiso 0.359(10) 1 calc PR B 2 H23D H -0.0235 0.8323 0.1370 0.063 Uiso 0.359(10) 1 calc PR B 2 O3 O -0.1012(6) 0.6304(15) 0.1323(7) 0.0421(19) Uani 0.534(13) 1 d PDU C 1 C30 C -0.1057(7) 0.5824(14) 0.1979(5) 0.060(3) Uani 0.534(13) 1 d PDU C 1 H30A H -0.0858 0.6241 0.2345 0.071 Uiso 0.534(13) 1 calc PR C 1 H30B H -0.0775 0.5212 0.1974 0.071 Uiso 0.534(13) 1 calc PR C 1 C31 C -0.1870(6) 0.5643(8) 0.2078(4) 0.058(2) Uani 0.534(13) 1 d PDU C 1 H31A H -0.2124 0.6214 0.2270 0.069 Uiso 0.534(13) 1 calc PR C 1 H31B H -0.1957 0.5082 0.2379 0.069 Uiso 0.534(13) 1 calc PR C 1 C32 C -0.2123(5) 0.5442(9) 0.1354(3) 0.085(3) Uani 0.534(13) 1 d PDU C 1 H32A H -0.2074 0.4749 0.1243 0.102 Uiso 0.534(13) 1 calc PR C 1 H32B H -0.2647 0.5639 0.1288 0.102 Uiso 0.534(13) 1 calc PR C 1 C33 C -0.1645(5) 0.5999(10) 0.0952(4) 0.083(3) Uani 0.534(13) 1 d PDU C 1 H33A H -0.1917 0.6570 0.0781 0.099 Uiso 0.534(13) 1 calc PR C 1 H33B H -0.1483 0.5616 0.0553 0.099 Uiso 0.534(13) 1 calc PR C 1 O3' O -0.0955(8) 0.6171(18) 0.1258(8) 0.052(4) Uani 0.466(13) 1 d PDU C 2 C30' C -0.1054(7) 0.5902(18) 0.1957(7) 0.069(4) Uani 0.466(13) 1 d PDU C 2 H30C H -0.0987 0.6469 0.2257 0.082 Uiso 0.466(13) 1 calc PR C 2 H30D H -0.0686 0.5405 0.2088 0.082 Uiso 0.466(13) 1 calc PR C 2 C31' C -0.1831(7) 0.5513(12) 0.2026(6) 0.111(5) Uani 0.466(13) 1 d PDU C 2 H31C H -0.1836 0.4801 0.1992 0.133 Uiso 0.466(13) 1 calc PR C 2 H31D H -0.2057 0.5707 0.2465 0.133 Uiso 0.466(13) 1 calc PR C 2 C32' C -0.2230(4) 0.5965(8) 0.1437(5) 0.071(2) Uani 0.466(13) 1 d PDU C 2 H32C H -0.2534 0.5479 0.1195 0.085 Uiso 0.466(13) 1 calc PR C 2 H32D H -0.2562 0.6487 0.1597 0.085 Uiso 0.466(13) 1 calc PR C 2 C33' C -0.1663(6) 0.6347(11) 0.0990(7) 0.102(5) Uani 0.466(13) 1 d PDU C 2 H33C H -0.1706 0.6043 0.0536 0.123 Uiso 0.466(13) 1 calc PR C 2 H33D H -0.1736 0.7049 0.0935 0.123 Uiso 0.466(13) 1 calc PR C 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 0.0392(10) 0.0332(10) 0.0320(10) -0.0012(8) 0.0029(8) -0.0026(8) C100 0.0341(8) 0.0334(9) 0.0353(9) 0.0031(7) 0.0018(7) -0.0060(7) C101 0.0451(10) 0.0392(9) 0.0408(10) -0.0033(8) -0.0024(8) -0.0004(8) C102 0.0500(11) 0.0428(10) 0.0580(13) -0.0005(9) -0.0044(9) 0.0081(9) C103 0.0440(10) 0.0570(12) 0.0480(12) 0.0085(9) -0.0086(9) 0.0033(9) C104 0.0408(10) 0.0560(12) 0.0388(10) -0.0008(9) -0.0055(8) -0.0027(9) C105 0.0397(10) 0.0398(9) 0.0375(10) -0.0026(8) -0.0032(7) -0.0026(7) C106 0.0308(8) 0.0342(9) 0.0328(9) 0.0005(7) -0.0024(7) -0.0051(7) C107 0.0430(9) 0.0358(9) 0.0340(9) -0.0002(7) 0.0011(7) -0.0009(8) C108 0.0552(11) 0.0326(9) 0.0496(11) 0.0000(8) 0.0005(9) -0.0016(8) C109 0.0628(12) 0.0395(10) 0.0479(11) 0.0108(9) 0.0036(9) -0.0085(9) C110 0.0813(15) 0.0525(12) 0.0362(11) 0.0039(9) 0.0135(10) -0.0127(11) C111 0.0743(14) 0.0365(10) 0.0388(11) -0.0052(8) 0.0109(9) -0.0079(9) Li1 0.0388(16) 0.0472(17) 0.0544(19) 0.0064(15) 0.0011(13) -0.0039(14) Li2 0.0429(16) 0.0361(15) 0.0377(16) 0.0011(12) -0.0003(12) -0.0028(12) N1 0.0435(8) 0.0324(7) 0.0331(8) 0.0017(6) -0.0037(6) -0.0030(6) N2 0.0416(8) 0.0324(7) 0.0332(8) 0.0021(6) -0.0011(6) -0.0056(6) O1 0.033(3) 0.044(3) 0.058(3) 0.001(2) 0.0012(17) -0.005(2) C10 0.043(4) 0.055(3) 0.061(4) 0.006(3) -0.004(3) -0.005(3) C11 0.034(3) 0.113(8) 0.053(4) -0.008(4) 0.004(3) 0.001(4) C12 0.060(5) 0.107(8) 0.128(9) 0.040(7) 0.026(5) 0.034(5) C13 0.047(4) 0.065(4) 0.071(5) 0.012(3) -0.014(3) 0.000(3) O1' 0.047(4) 0.116(7) 0.137(8) 0.057(5) 0.004(4) -0.006(4) C10' 0.061(5) 0.140(8) 0.141(10) 0.060(7) 0.016(6) -0.041(5) C11' 0.085(7) 0.092(7) 0.139(11) -0.026(6) 0.037(7) -0.037(6) C12' 0.055(4) 0.091(7) 0.134(10) -0.046(6) -0.002(5) -0.004(4) C13' 0.045(4) 0.129(8) 0.096(10) 0.024(6) 0.002(5) 0.008(4) O2 0.035(3) 0.038(2) 0.039(4) -0.014(2) 0.005(3) -0.0026(18) C20 0.033(3) 0.049(3) 0.060(4) -0.013(3) 0.006(3) 0.001(2) C21 0.049(2) 0.046(2) 0.069(3) 0.004(2) -0.008(2) -0.0115(16) C22 0.061(3) 0.039(2) 0.065(3) -0.007(2) -0.010(3) 0.006(2) C23 0.041(3) 0.036(3) 0.053(4) -0.008(2) 0.002(2) 0.010(2) O2' 0.043(5) 0.046(4) 0.048(11) -0.007(3) 0.011(4) 0.000(3) C20' 0.036(6) 0.079(7) 0.099(11) -0.013(7) 0.003(6) -0.018(6) C21' 0.066(4) 0.090(5) 0.056(5) 0.018(4) -0.015(4) -0.037(4) C22' 0.086(9) 0.036(4) 0.080(7) 0.003(4) -0.026(5) -0.010(5) C23' 0.045(6) 0.073(9) 0.038(6) -0.014(5) -0.003(5) 0.002(5) O3 0.036(3) 0.045(3) 0.044(4) -0.002(2) 0.008(2) -0.002(2) C30 0.071(6) 0.078(7) 0.030(4) 0.009(4) 0.000(4) -0.003(6) C31 0.067(5) 0.064(4) 0.042(3) -0.001(3) 0.011(3) -0.014(3) C32 0.085(5) 0.107(6) 0.063(4) 0.008(4) -0.013(3) -0.053(5) C33 0.048(4) 0.161(10) 0.039(3) 0.031(4) -0.007(2) -0.032(5) O3' 0.049(4) 0.067(9) 0.039(4) 0.012(5) 0.004(3) 0.000(4) C30' 0.045(6) 0.093(10) 0.068(7) 0.028(7) 0.006(5) -0.014(7) C31' 0.058(7) 0.152(12) 0.122(10) 0.072(8) -0.003(6) -0.032(7) C32' 0.042(3) 0.072(5) 0.099(5) -0.001(4) 0.000(3) -0.017(3) C33' 0.054(5) 0.119(8) 0.135(8) 0.073(7) -0.018(4) 0.011(5) _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 N1 1.442(2) 5_565 ? B1 N2 1.443(2) . ? B1 B1 1.781(4) 5_565 ? B1 Li1 2.399(4) . ? B1 Li1 2.403(3) 5_565 ? B1 Li2 2.582(3) . ? B1 Li2 2.584(3) 5_565 ? C100 N1 1.384(2) . ? C100 C101 1.410(2) . ? C100 C105 1.410(2) . ? C101 C102 1.383(3) . ? C101 H101 0.9500 . ? C102 C103 1.383(3) . ? C102 H102 0.9500 . ? C103 C104 1.377(3) . ? C103 H103 0.9500 . ? C104 C105 1.381(2) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 N2 1.387(2) . ? C106 C111 1.399(2) . ? C106 C107 1.400(2) . ? C107 C108 1.382(2) . ? C107 H107 0.9500 . ? C108 C109 1.369(3) . ? C108 H108 0.9500 . ? C109 C110 1.376(3) . ? C109 H109 0.9500 . ? C110 C111 1.385(3) . ? C110 H110 0.9500 . ? C111 H111 0.9500 . ? Li1 O1' 1.858(11) . ? Li1 O1 1.890(9) . ? Li1 N1 1.956(3) . ? Li1 N2 1.957(3) . ? Li1 B1 2.403(3) 5_565 ? Li1 Li2 2.435(4) . ? Li2 O3' 1.884(15) . ? Li2 O2' 1.97(2) . ? Li2 O3 2.033(14) . ? Li2 O2 2.035(12) . ? Li2 N2 2.067(3) . ? Li2 N1 2.078(3) . ? Li2 B1 2.584(3) 5_565 ? N1 B1 1.442(2) 5_565 ? O1 C10 1.426(8) . ? O1 C13 1.439(9) . ? C10 C11 1.523(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.493(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.479(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O1' C13' 1.434(10) . ? O1' C10' 1.446(10) . ? C10' C11' 1.480(11) . ? C10' H10C 0.9900 . ? C10' H10D 0.9900 . ? C11' C12' 1.539(11) . ? C11' H11C 0.9900 . ? C11' H11D 0.9900 . ? C12' C13' 1.477(11) . ? C12' H12C 0.9900 . ? C12' H12D 0.9900 . ? C13' H13C 0.9900 . ? C13' H13D 0.9900 . ? O2 C20 1.436(7) . ? O2 C23 1.445(7) . ? C20 C21 1.501(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.519(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.505(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? O2' C23' 1.450(12) . ? O2' C20' 1.455(13) . ? C20' C21' 1.509(13) . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C21' C22' 1.520(13) . ? C21' H21C 0.9900 . ? C21' H21D 0.9900 . ? C22' C23' 1.507(12) . ? C22' H22C 0.9900 . ? C22' H22D 0.9900 . ? C23' H23C 0.9900 . ? C23' H23D 0.9900 . ? O3 C33 1.416(11) . ? O3 C30 1.452(10) . ? C30 C31 1.496(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.518(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.401(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? O3' C33' 1.398(12) . ? O3' C30' 1.435(11) . ? C30' C31' 1.504(11) . ? C30' H30C 0.9900 . ? C30' H30D 0.9900 . ? C31' C32' 1.499(11) . ? C31' H31C 0.9900 . ? C31' H31D 0.9900 . ? C32' C33' 1.446(10) . ? C32' H32C 0.9900 . ? C32' H32D 0.9900 . ? C33' H33C 0.9900 . ? C33' H33D 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 N1 B1 N2 133.25(16) 5_565 . ? N1 B1 B1 113.34(17) 5_565 5_565 ? N2 B1 B1 113.41(17) . 5_565 ? N1 B1 Li1 151.25(15) 5_565 . ? N2 B1 Li1 54.64(11) . . ? B1 B1 Li1 68.37(14) 5_565 . ? N1 B1 Li1 54.45(11) 5_565 5_565 ? N2 B1 Li1 150.69(15) . 5_565 ? B1 B1 Li1 68.09(13) 5_565 5_565 ? Li1 B1 Li1 136.46(10) . 5_565 ? N1 B1 Li2 150.34(14) 5_565 . ? N2 B1 Li2 53.08(10) . . ? B1 B1 Li2 69.87(13) 5_565 . ? Li1 B1 Li2 58.39(11) . . ? Li1 B1 Li2 105.55(12) 5_565 . ? N1 B1 Li2 53.46(10) 5_565 5_565 ? N2 B1 Li2 150.96(14) . 5_565 ? B1 B1 Li2 69.79(13) 5_565 5_565 ? Li1 B1 Li2 105.65(12) . 5_565 ? Li1 B1 Li2 58.32(11) 5_565 5_565 ? Li2 B1 Li2 139.66(9) . 5_565 ? N1 C100 C101 123.87(15) . . ? N1 C100 C105 120.49(15) . . ? C101 C100 C105 115.52(15) . . ? C102 C101 C100 121.60(17) . . ? C102 C101 H101 119.2 . . ? C100 C101 H101 119.2 . . ? C103 C102 C101 121.33(18) . . ? C103 C102 H102 119.3 . . ? C101 C102 H102 119.3 . . ? C104 C103 C102 118.37(18) . . ? C104 C103 H103 120.8 . . ? C102 C103 H103 120.8 . . ? C103 C104 C105 120.88(17) . . ? C103 C104 H104 119.6 . . ? C105 C104 H104 119.6 . . ? C104 C105 C100 122.29(16) . . ? C104 C105 H105 118.9 . . ? C100 C105 H105 118.9 . . ? N2 C106 C111 123.96(15) . . ? N2 C106 C107 120.44(15) . . ? C111 C106 C107 115.52(15) . . ? C108 C107 C106 122.21(16) . . ? C108 C107 H107 118.9 . . ? C106 C107 H107 118.9 . . ? C109 C108 C107 121.01(17) . . ? C109 C108 H108 119.5 . . ? C107 C108 H108 119.5 . . ? C108 C109 C110 118.33(17) . . ? C108 C109 H109 120.8 . . ? C110 C109 H109 120.8 . . ? C109 C110 C111 121.04(18) . . ? C109 C110 H110 119.5 . . ? C111 C110 H110 119.5 . . ? C110 C111 C106 121.88(17) . . ? C110 C111 H111 119.1 . . ? C106 C111 H111 119.1 . . ? O1' Li1 O1 7.6(6) . . ? O1' Li1 N1 130.5(4) . . ? O1 Li1 N1 126.3(3) . . ? O1' Li1 N2 132.2(4) . . ? O1 Li1 N2 134.3(3) . . ? N1 Li1 N2 96.79(14) . . ? O1' Li1 B1 147.0(5) . . ? O1 Li1 B1 154.2(3) . . ? N1 Li1 B1 75.85(11) . . ? N2 Li1 B1 36.98(8) . . ? O1' Li1 B1 146.0(4) . 5_565 ? O1 Li1 B1 148.1(3) . 5_565 ? N1 Li1 B1 36.85(8) . 5_565 ? N2 Li1 B1 75.80(11) . 5_565 ? B1 Li1 B1 43.54(10) . 5_565 ? O1' Li1 Li2 143.7(5) . . ? O1 Li1 Li2 136.7(3) . . ? N1 Li1 Li2 55.19(11) . . ? N2 Li1 Li2 54.86(11) . . ? B1 Li1 Li2 64.58(11) . . ? B1 Li1 Li2 64.54(11) 5_565 . ? O3' Li2 O2' 103.3(10) . . ? O3' Li2 O3 5.7(13) . . ? O2' Li2 O3 97.9(9) . . ? O3' Li2 O2 97.5(8) . . ? O2' Li2 O2 6.3(14) . . ? O3 Li2 O2 92.2(6) . . ? O3' Li2 N2 123.2(5) . . ? O2' Li2 N2 110.5(11) . . ? O3 Li2 N2 124.6(4) . . ? O2 Li2 N2 116.3(6) . . ? O3' Li2 N1 113.9(7) . . ? O2' Li2 N1 116.9(9) . . ? O3 Li2 N1 118.7(6) . . ? O2 Li2 N1 117.9(5) . . ? N2 Li2 N1 89.79(12) . . ? O3' Li2 Li1 158.2(8) . . ? O2' Li2 Li1 98.0(7) . . ? O3 Li2 Li1 163.9(6) . . ? O2 Li2 Li1 103.5(4) . . ? N2 Li2 Li1 50.73(11) . . ? N1 Li2 Li1 50.61(10) . . ? O3' Li2 B1 105.5(6) . . ? O2' Li2 B1 143.8(11) . . ? O3 Li2 B1 109.8(5) . . ? O2 Li2 B1 149.9(6) . . ? N2 Li2 B1 33.93(7) . . ? N1 Li2 B1 69.83(10) . . ? Li1 Li2 B1 57.03(11) . . ? O3' Li2 B1 101.3(8) . 5_565 ? O2' Li2 B1 149.0(8) . 5_565 ? O3 Li2 B1 107.0(6) . 5_565 ? O2 Li2 B1 151.3(4) . 5_565 ? N2 Li2 B1 70.02(10) . 5_565 ? N1 Li2 B1 33.88(7) . 5_565 ? Li1 Li2 B1 57.13(10) . 5_565 ? B1 Li2 B1 40.34(9) . 5_565 ? C100 N1 B1 129.05(14) . 5_565 ? C100 N1 Li1 119.42(14) . . ? B1 N1 Li1 88.70(13) 5_565 . ? C100 N1 Li2 133.63(13) . . ? B1 N1 Li2 92.66(13) 5_565 . ? Li1 N1 Li2 74.20(13) . . ? C106 N2 B1 128.83(14) . . ? C106 N2 Li1 120.18(14) . . ? B1 N2 Li1 88.38(13) . . ? C106 N2 Li2 133.19(13) . . ? B1 N2 Li2 92.98(12) . . ? Li1 N2 Li2 74.41(13) . . ? C10 O1 C13 107.8(6) . . ? C10 O1 Li1 130.3(6) . . ? C13 O1 Li1 121.6(7) . . ? O1 C10 C11 104.5(6) . . ? O1 C10 H10A 110.9 . . ? C11 C10 H10A 110.9 . . ? O1 C10 H10B 110.9 . . ? C11 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? C12 C11 C10 104.1(6) . . ? C12 C11 H11A 110.9 . . ? C10 C11 H11A 110.9 . . ? C12 C11 H11B 110.9 . . ? C10 C11 H11B 110.9 . . ? H11A C11 H11B 109.0 . . ? C13 C12 C11 106.9(7) . . ? C13 C12 H12A 110.3 . . ? C11 C12 H12A 110.3 . . ? C13 C12 H12B 110.3 . . ? C11 C12 H12B 110.3 . . ? H12A C12 H12B 108.6 . . ? O1 C13 C12 106.7(7) . . ? O1 C13 H13A 110.4 . . ? C12 C13 H13A 110.4 . . ? O1 C13 H13B 110.4 . . ? C12 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? C13' O1' C10' 109.4(9) . . ? C13' O1' Li1 124.0(8) . . ? C10' O1' Li1 126.1(9) . . ? O1' C10' C11' 104.6(9) . . ? O1' C10' H10C 110.8 . . ? C11' C10' H10C 110.8 . . ? O1' C10' H10D 110.8 . . ? C11' C10' H10D 110.8 . . ? H10C C10' H10D 108.9 . . ? C10' C11' C12' 104.3(8) . . ? C10' C11' H11C 110.9 . . ? C12' C11' H11C 110.9 . . ? C10' C11' H11D 110.9 . . ? C12' C11' H11D 110.9 . . ? H11C C11' H11D 108.9 . . ? C13' C12' C11' 101.1(8) . . ? C13' C12' H12C 111.6 . . ? C11' C12' H12C 111.6 . . ? C13' C12' H12D 111.6 . . ? C11' C12' H12D 111.6 . . ? H12C C12' H12D 109.4 . . ? O1' C13' C12' 108.3(9) . . ? O1' C13' H13C 110.0 . . ? C12' C13' H13C 110.0 . . ? O1' C13' H13D 110.0 . . ? C12' C13' H13D 110.0 . . ? H13C C13' H13D 108.4 . . ? C20 O2 C23 109.7(6) . . ? C20 O2 Li2 117.1(9) . . ? C23 O2 Li2 122.6(10) . . ? O2 C20 C21 105.8(6) . . ? O2 C20 H20A 110.6 . . ? C21 C20 H20A 110.6 . . ? O2 C20 H20B 110.6 . . ? C21 C20 H20B 110.6 . . ? H20A C20 H20B 108.7 . . ? C20 C21 C22 101.6(5) . . ? C20 C21 H21A 111.4 . . ? C22 C21 H21A 111.4 . . ? C20 C21 H21B 111.4 . . ? C22 C21 H21B 111.4 . . ? H21A C21 H21B 109.3 . . ? C23 C22 C21 103.1(6) . . ? C23 C22 H22A 111.1 . . ? C21 C22 H22A 111.1 . . ? C23 C22 H22B 111.1 . . ? C21 C22 H22B 111.1 . . ? H22A C22 H22B 109.1 . . ? O2 C23 C22 105.6(6) . . ? O2 C23 H23A 110.6 . . ? C22 C23 H23A 110.6 . . ? O2 C23 H23B 110.6 . . ? C22 C23 H23B 110.6 . . ? H23A C23 H23B 108.7 . . ? C23' O2' C20' 107.5(12) . . ? C23' O2' Li2 124.8(17) . . ? C20' O2' Li2 124.8(16) . . ? O2' C20' C21' 103.2(13) . . ? O2' C20' H20C 111.1 . . ? C21' C20' H20C 111.1 . . ? O2' C20' H20D 111.1 . . ? C21' C20' H20D 111.1 . . ? H20C C20' H20D 109.1 . . ? C20' C21' C22' 101.3(10) . . ? C20' C21' H21C 111.5 . . ? C22' C21' H21C 111.5 . . ? C20' C21' H21D 111.5 . . ? C22' C21' H21D 111.5 . . ? H21C C21' H21D 109.3 . . ? C23' C22' C21' 100.9(10) . . ? C23' C22' H22C 111.6 . . ? C21' C22' H22C 111.6 . . ? C23' C22' H22D 111.6 . . ? C21' C22' H22D 111.6 . . ? H22C C22' H22D 109.4 . . ? O2' C23' C22' 107.5(10) . . ? O2' C23' H23C 110.2 . . ? C22' C23' H23C 110.2 . . ? O2' C23' H23D 110.2 . . ? C22' C23' H23D 110.2 . . ? H23C C23' H23D 108.5 . . ? C33 O3 C30 105.9(8) . . ? C33 O3 Li2 119.8(11) . . ? C30 O3 Li2 112.8(10) . . ? O3 C30 C31 104.3(8) . . ? O3 C30 H30A 110.9 . . ? C31 C30 H30A 110.9 . . ? O3 C30 H30B 110.9 . . ? C31 C30 H30B 110.9 . . ? H30A C30 H30B 108.9 . . ? C30 C31 C32 101.7(7) . . ? C30 C31 H31A 111.4 . . ? C32 C31 H31A 111.4 . . ? C30 C31 H31B 111.4 . . ? C32 C31 H31B 111.4 . . ? H31A C31 H31B 109.3 . . ? C33 C32 C31 104.0(6) . . ? C33 C32 H32A 111.0 . . ? C31 C32 H32A 111.0 . . ? C33 C32 H32B 111.0 . . ? C31 C32 H32B 111.0 . . ? H32A C32 H32B 109.0 . . ? C32 C33 O3 111.6(6) . . ? C32 C33 H33A 109.3 . . ? O3 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? O3 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C33' O3' C30' 106.9(11) . . ? C33' O3' Li2 134.0(10) . . ? C30' O3' Li2 119.0(10) . . ? O3' C30' C31' 107.2(9) . . ? O3' C30' H30C 110.3 . . ? C31' C30' H30C 110.3 . . ? O3' C30' H30D 110.3 . . ? C31' C30' H30D 110.3 . . ? H30C C30' H30D 108.5 . . ? C32' C31' C30' 103.0(9) . . ? C32' C31' H31C 111.2 . . ? C30' C31' H31C 111.2 . . ? C32' C31' H31D 111.2 . . ? C30' C31' H31D 111.2 . . ? H31C C31' H31D 109.1 . . ? C33' C32' C31' 106.5(7) . . ? C33' C32' H32C 110.4 . . ? C31' C32' H32C 110.4 . . ? C33' C32' H32D 110.4 . . ? C31' C32' H32D 110.4 . . ? H32C C32' H32D 108.6 . . ? O3' C33' C32' 110.5(9) . . ? O3' C33' H33C 109.5 . . ? C32' C33' H33C 109.5 . . ? O3' C33' H33D 109.5 . . ? C32' C33' H33D 109.5 . . ? H33C C33' H33D 108.1 . . ? 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 N1 C100 C101 C102 175.19(17) . . . . ? C105 C100 C101 C102 -0.7(2) . . . . ? C100 C101 C102 C103 0.5(3) . . . . ? C101 C102 C103 C104 0.1(3) . . . . ? C102 C103 C104 C105 -0.3(3) . . . . ? C103 C104 C105 C100 -0.1(3) . . . . ? N1 C100 C105 C104 -175.53(15) . . . . ? C101 C100 C105 C104 0.5(2) . . . . ? N2 C106 C107 C108 177.59(16) . . . . ? C111 C106 C107 C108 0.7(3) . . . . ? C106 C107 C108 C109 -0.7(3) . . . . ? C107 C108 C109 C110 0.2(3) . . . . ? C108 C109 C110 C111 0.3(3) . . . . ? C109 C110 C111 C106 -0.4(3) . . . . ? N2 C106 C111 C110 -176.92(18) . . . . ? C107 C106 C111 C110 -0.1(3) . . . . ? N1 B1 Li1 O1' 26.7(8) 5_565 . . . ? N2 B1 Li1 O1' -90.2(7) . . . . ? B1 B1 Li1 O1' 126.1(7) 5_565 . . . ? Li1 B1 Li1 O1' 126.1(7) 5_565 . . . ? Li2 B1 Li1 O1' -154.9(7) . . . . ? Li2 B1 Li1 O1' 65.9(7) 5_565 . . . ? N1 B1 Li1 O1 31.5(8) 5_565 . . . ? N2 B1 Li1 O1 -85.5(6) . . . . ? B1 B1 Li1 O1 130.9(6) 5_565 . . . ? Li1 B1 Li1 O1 130.9(6) 5_565 . . . ? Li2 B1 Li1 O1 -150.1(6) . . . . ? Li2 B1 Li1 O1 70.7(6) 5_565 . . . ? N1 B1 Li1 N1 -120.5(3) 5_565 . . . ? N2 B1 Li1 N1 122.51(15) . . . . ? B1 B1 Li1 N1 -21.15(12) 5_565 . . . ? Li1 B1 Li1 N1 -21.15(12) 5_565 . . . ? Li2 B1 Li1 N1 57.86(11) . . . . ? Li2 B1 Li1 N1 -81.35(13) 5_565 . . . ? N1 B1 Li1 N2 117.0(3) 5_565 . . . ? B1 B1 Li1 N2 -143.66(19) 5_565 . . . ? Li1 B1 Li1 N2 -143.66(19) 5_565 . . . ? Li2 B1 Li1 N2 -64.65(13) . . . . ? Li2 B1 Li1 N2 156.14(15) 5_565 . . . ? N1 B1 Li1 B1 -99.4(3) 5_565 . . 5_565 ? N2 B1 Li1 B1 143.66(19) . . . 5_565 ? Li1 B1 Li1 B1 0.0 5_565 . . 5_565 ? Li2 B1 Li1 B1 79.01(14) . . . 5_565 ? Li2 B1 Li1 B1 -60.20(12) 5_565 . . 5_565 ? N1 B1 Li1 Li2 -178.4(3) 5_565 . . . ? N2 B1 Li1 Li2 64.65(13) . . . . ? B1 B1 Li1 Li2 -79.01(14) 5_565 . . . ? Li1 B1 Li1 Li2 -79.01(14) 5_565 . . . ? Li2 B1 Li1 Li2 -139.21(9) 5_565 . . . ? O1' Li1 Li2 O3' -162.8(14) . . . . ? O1 Li1 Li2 O3' -158.2(13) . . . . ? N1 Li1 Li2 O3' -49.8(13) . . . . ? N2 Li1 Li2 O3' 81.9(13) . . . . ? B1 Li1 Li2 O3' 40.2(13) . . . . ? B1 Li1 Li2 O3' -8.3(13) 5_565 . . . ? O1' Li1 Li2 O2' 5.4(14) . . . . ? O1 Li1 Li2 O2' 10.0(13) . . . . ? N1 Li1 Li2 O2' 118.4(12) . . . . ? N2 Li1 Li2 O2' -109.9(12) . . . . ? B1 Li1 Li2 O2' -151.6(12) . . . . ? B1 Li1 Li2 O2' 159.9(12) 5_565 . . . ? O1' Li1 Li2 O3 -165.6(16) . . . . ? O1 Li1 Li2 O3 -161.0(15) . . . . ? N1 Li1 Li2 O3 -52.6(15) . . . . ? N2 Li1 Li2 O3 79.1(15) . . . . ? B1 Li1 Li2 O3 37.4(15) . . . . ? B1 Li1 Li2 O3 -11.1(15) 5_565 . . . ? O1' Li1 Li2 O2 2.2(9) . . . . ? O1 Li1 Li2 O2 6.8(8) . . . . ? N1 Li1 Li2 O2 115.1(6) . . . . ? N2 Li1 Li2 O2 -113.1(6) . . . . ? B1 Li1 Li2 O2 -154.8(6) . . . . ? B1 Li1 Li2 O2 156.7(6) 5_565 . . . ? O1' Li1 Li2 N2 115.3(7) . . . . ? O1 Li1 Li2 N2 119.9(5) . . . . ? N1 Li1 Li2 N2 -131.71(15) . . . . ? B1 Li1 Li2 N2 -41.66(8) . . . . ? B1 Li1 Li2 N2 -90.16(11) 5_565 . . . ? O1' Li1 Li2 N1 -112.9(7) . . . . ? O1 Li1 Li2 N1 -108.4(5) . . . . ? N2 Li1 Li2 N1 131.71(15) . . . . ? B1 Li1 Li2 N1 90.05(11) . . . . ? B1 Li1 Li2 N1 41.55(8) 5_565 . . . ? O1' Li1 Li2 B1 157.0(7) . . . . ? O1 Li1 Li2 B1 161.6(5) . . . . ? N1 Li1 Li2 B1 -90.05(11) . . . . ? N2 Li1 Li2 B1 41.66(8) . . . . ? B1 Li1 Li2 B1 -48.50(10) 5_565 . . . ? O1' Li1 Li2 B1 -154.5(7) . . . 5_565 ? O1 Li1 Li2 B1 -149.9(5) . . . 5_565 ? N1 Li1 Li2 B1 -41.55(8) . . . 5_565 ? N2 Li1 Li2 B1 90.16(11) . . . 5_565 ? B1 Li1 Li2 B1 48.50(10) . . . 5_565 ? N1 B1 Li2 O3' 12.8(7) 5_565 . . . ? N2 B1 Li2 O3' 127.2(7) . . . . ? B1 B1 Li2 O3' -89.2(7) 5_565 . . . ? Li1 B1 Li2 O3' -165.6(7) . . . . ? Li1 B1 Li2 O3' -30.2(7) 5_565 . . . ? Li2 B1 Li2 O3' -89.2(7) 5_565 . . . ? N1 B1 Li2 O2' -128.7(15) 5_565 . . . ? N2 B1 Li2 O2' -14.3(15) . . . . ? B1 B1 Li2 O2' 129.3(15) 5_565 . . . ? Li1 B1 Li2 O2' 52.9(15) . . . . ? Li1 B1 Li2 O2' -171.7(15) 5_565 . . . ? Li2 B1 Li2 O2' 129.3(15) 5_565 . . . ? N1 B1 Li2 O3 8.8(6) 5_565 . . . ? N2 B1 Li2 O3 123.1(6) . . . . ? B1 B1 Li2 O3 -93.3(6) 5_565 . . . ? Li1 B1 Li2 O3 -169.7(6) . . . . ? Li1 B1 Li2 O3 -34.3(6) 5_565 . . . ? Li2 B1 Li2 O3 -93.3(6) 5_565 . . . ? N1 B1 Li2 O2 -125.9(9) 5_565 . . . ? N2 B1 Li2 O2 -11.6(9) . . . . ? B1 B1 Li2 O2 132.0(9) 5_565 . . . ? Li1 B1 Li2 O2 55.6(9) . . . . ? Li1 B1 Li2 O2 -168.9(9) 5_565 . . . ? Li2 B1 Li2 O2 132.0(9) 5_565 . . . ? N1 B1 Li2 N2 -114.4(3) 5_565 . . . ? B1 B1 Li2 N2 143.6(2) 5_565 . . . ? Li1 B1 Li2 N2 67.20(13) . . . . ? Li1 B1 Li2 N2 -157.38(16) 5_565 . . . ? Li2 B1 Li2 N2 143.6(2) 5_565 . . . ? N1 B1 Li2 N1 123.0(3) 5_565 . . . ? N2 B1 Li2 N1 -122.62(14) . . . . ? B1 B1 Li2 N1 20.96(11) 5_565 . . . ? Li1 B1 Li2 N1 -55.42(11) . . . . ? Li1 B1 Li2 N1 80.00(12) 5_565 . . . ? Li2 B1 Li2 N1 20.96(11) 5_565 . . . ? N1 B1 Li2 Li1 178.4(3) 5_565 . . . ? N2 B1 Li2 Li1 -67.20(13) . . . . ? B1 B1 Li2 Li1 76.38(15) 5_565 . . . ? Li1 B1 Li2 Li1 135.42(10) 5_565 . . . ? Li2 B1 Li2 Li1 76.38(15) 5_565 . . . ? N1 B1 Li2 B1 102.1(3) 5_565 . . 5_565 ? N2 B1 Li2 B1 -143.6(2) . . . 5_565 ? Li1 B1 Li2 B1 -76.38(15) . . . 5_565 ? Li1 B1 Li2 B1 59.03(13) 5_565 . . 5_565 ? Li2 B1 Li2 B1 0.0 5_565 . . 5_565 ? C101 C100 N1 B1 29.6(3) . . . 5_565 ? C105 C100 N1 B1 -154.62(17) . . . 5_565 ? C101 C100 N1 Li1 -85.4(2) . . . . ? C105 C100 N1 Li1 90.3(2) . . . . ? C101 C100 N1 Li2 178.50(16) . . . . ? C105 C100 N1 Li2 -5.8(3) . . . . ? O1' Li1 N1 C100 2.6(6) . . . . ? O1 Li1 N1 C100 -5.6(4) . . . . ? N2 Li1 N1 C100 -169.51(13) . . . . ? B1 Li1 N1 C100 159.77(13) . . . . ? B1 Li1 N1 C100 135.29(18) 5_565 . . . ? Li2 Li1 N1 C100 -131.57(16) . . . . ? O1' Li1 N1 B1 -132.7(6) . . . 5_565 ? O1 Li1 N1 B1 -140.8(3) . . . 5_565 ? N2 Li1 N1 B1 55.20(15) . . . 5_565 ? B1 Li1 N1 B1 24.48(14) . . . 5_565 ? Li2 Li1 N1 B1 93.14(13) . . . 5_565 ? O1' Li1 N1 Li2 134.2(6) . . . . ? O1 Li1 N1 Li2 126.0(4) . . . . ? N2 Li1 N1 Li2 -37.94(13) . . . . ? B1 Li1 N1 Li2 -68.66(11) . . . . ? B1 Li1 N1 Li2 -93.14(13) 5_565 . . . ? O3' Li2 N1 C100 -82.2(6) . . . . ? O2' Li2 N1 C100 38.2(12) . . . . ? O3 Li2 N1 C100 -78.7(5) . . . . ? O2 Li2 N1 C100 31.1(6) . . . . ? N2 Li2 N1 C100 151.11(15) . . . . ? Li1 Li2 N1 C100 115.81(19) . . . . ? B1 Li2 N1 C100 179.16(16) . . . . ? B1 Li2 N1 C100 -156.3(2) 5_565 . . . ? O3' Li2 N1 B1 74.1(6) . . . 5_565 ? O2' Li2 N1 B1 -165.5(12) . . . 5_565 ? O3 Li2 N1 B1 77.6(5) . . . 5_565 ? O2 Li2 N1 B1 -172.6(6) . . . 5_565 ? N2 Li2 N1 B1 -52.59(13) . . . 5_565 ? Li1 Li2 N1 B1 -87.90(14) . . . 5_565 ? B1 Li2 N1 B1 -24.54(13) . . . 5_565 ? O3' Li2 N1 Li1 162.0(6) . . . . ? O2' Li2 N1 Li1 -77.6(12) . . . . ? O3 Li2 N1 Li1 165.5(5) . . . . ? O2 Li2 N1 Li1 -84.7(6) . . . . ? N2 Li2 N1 Li1 35.30(12) . . . . ? B1 Li2 N1 Li1 63.35(11) . . . . ? B1 Li2 N1 Li1 87.90(14) 5_565 . . . ? C111 C106 N2 B1 -38.8(3) . . . . ? C107 C106 N2 B1 144.53(18) . . . . ? C111 C106 N2 Li1 76.4(2) . . . . ? C107 C106 N2 Li1 -100.3(2) . . . . ? C111 C106 N2 Li2 173.25(18) . . . . ? C107 C106 N2 Li2 -3.4(3) . . . . ? N1 B1 N2 C106 -15.4(3) 5_565 . . . ? B1 B1 N2 C106 165.41(16) 5_565 . . . ? Li1 B1 N2 C106 128.5(2) . . . . ? Li1 B1 N2 C106 -108.0(3) 5_565 . . . ? Li2 B1 N2 C106 -157.2(2) . . . . ? Li2 B1 N2 C106 75.2(3) 5_565 . . . ? N1 B1 N2 Li1 -143.9(2) 5_565 . . . ? B1 B1 N2 Li1 36.89(19) 5_565 . . . ? Li1 B1 N2 Li1 123.5(3) 5_565 . . . ? Li2 B1 N2 Li1 74.30(13) . . . . ? Li2 B1 N2 Li1 -53.4(3) 5_565 . . . ? N1 B1 N2 Li2 141.8(2) 5_565 . . . ? B1 B1 N2 Li2 -37.4(2) 5_565 . . . ? Li1 B1 N2 Li2 -74.30(13) . . . . ? Li1 B1 N2 Li2 49.2(3) 5_565 . . . ? Li2 B1 N2 Li2 -127.7(3) 5_565 . . . ? O1' Li1 N2 C106 -2.5(7) . . . . ? O1 Li1 N2 C106 7.5(5) . . . . ? N1 Li1 N2 C106 169.40(13) . . . . ? B1 Li1 N2 C106 -135.16(18) . . . . ? B1 Li1 N2 C106 -160.07(13) 5_565 . . . ? Li2 Li1 N2 C106 131.28(16) . . . . ? O1' Li1 N2 B1 132.7(7) . . . . ? O1 Li1 N2 B1 142.7(4) . . . . ? N1 Li1 N2 B1 -55.44(14) . . . . ? B1 Li1 N2 B1 -24.91(13) 5_565 . . . ? Li2 Li1 N2 B1 -93.55(13) . . . . ? O1' Li1 N2 Li2 -133.8(7) . . . . ? O1 Li1 N2 Li2 -123.8(4) . . . . ? N1 Li1 N2 Li2 38.12(13) . . . . ? B1 Li1 N2 Li2 93.55(13) . . . . ? B1 Li1 N2 Li2 68.65(11) 5_565 . . . ? O3' Li2 N2 C106 89.0(9) . . . . ? O2' Li2 N2 C106 -33.5(9) . . . . ? O3 Li2 N2 C106 82.3(7) . . . . ? O2 Li2 N2 C106 -30.9(5) . . . . ? N1 Li2 N2 C106 -152.23(15) . . . . ? Li1 Li2 N2 C106 -117.00(19) . . . . ? B1 Li2 N2 C106 155.5(2) . . . . ? B1 Li2 N2 C106 179.66(16) 5_565 . . . ? O3' Li2 N2 B1 -66.5(9) . . . . ? O2' Li2 N2 B1 171.0(9) . . . . ? O3 Li2 N2 B1 -73.2(7) . . . . ? O2 Li2 N2 B1 173.6(5) . . . . ? N1 Li2 N2 B1 52.24(13) . . . . ? Li1 Li2 N2 B1 87.48(14) . . . . ? B1 Li2 N2 B1 24.13(13) 5_565 . . . ? O3' Li2 N2 Li1 -154.0(9) . . . . ? O2' Li2 N2 Li1 83.5(9) . . . . ? O3 Li2 N2 Li1 -160.7(7) . . . . ? O2 Li2 N2 Li1 86.1(5) . . . . ? N1 Li2 N2 Li1 -35.24(12) . . . . ? B1 Li2 N2 Li1 -87.48(14) . . . . ? B1 Li2 N2 Li1 -63.34(11) 5_565 . . . ? O1' Li1 O1 C10 71(4) . . . . ? N1 Li1 O1 C10 -163.6(7) . . . . ? N2 Li1 O1 C10 -6.2(10) . . . . ? B1 Li1 O1 C10 50.8(11) . . . . ? B1 Li1 O1 C10 150.6(6) 5_565 . . . ? Li2 Li1 O1 C10 -88.3(9) . . . . ? O1' Li1 O1 C13 -116(4) . . . . ? N1 Li1 O1 C13 9.4(9) . . . . ? N2 Li1 O1 C13 166.9(7) . . . . ? B1 Li1 O1 C13 -136.2(9) . . . . ? B1 Li1 O1 C13 -36.3(11) 5_565 . . . ? Li2 Li1 O1 C13 84.8(9) . . . . ? C13 O1 C10 C11 32.6(11) . . . . ? Li1 O1 C10 C11 -153.6(8) . . . . ? O1 C10 C11 C12 -27.3(13) . . . . ? C10 C11 C12 C13 12.5(17) . . . . ? C10 O1 C13 C12 -25.0(15) . . . . ? Li1 O1 C13 C12 160.6(11) . . . . ? C11 C12 C13 O1 6.7(18) . . . . ? O1 Li1 O1' C13' 68(4) . . . . ? N1 Li1 O1' C13' 8.4(14) . . . . ? N2 Li1 O1' C13' 177.8(9) . . . . ? B1 Li1 O1' C13' -128.0(10) . . . . ? B1 Li1 O1' C13' -43.6(15) 5_565 . . . ? Li2 Li1 O1' C13' 92.3(12) . . . . ? O1 Li1 O1' C10' -104(5) . . . . ? N1 Li1 O1' C10' -163.3(9) . . . . ? N2 Li1 O1' C10' 6.1(15) . . . . ? B1 Li1 O1' C10' 60.3(15) . . . . ? B1 Li1 O1' C10' 144.7(9) 5_565 . . . ? Li2 Li1 O1' C10' -79.4(14) . . . . ? C13' O1' C10' C11' 16.1(17) . . . . ? Li1 O1' C10' C11' -171.2(13) . . . . ? O1' C10' C11' C12' -31.5(16) . . . . ? C10' C11' C12' C13' 34.7(16) . . . . ? C10' O1' C13' C12' 6.7(17) . . . . ? Li1 O1' C13' C12' -166.2(13) . . . . ? C11' C12' C13' O1' -25.3(16) . . . . ? O3' Li2 O2 C20 -178.4(13) . . . . ? O2' Li2 O2 C20 -23(12) . . . . ? O3 Li2 O2 C20 -176.2(13) . . . . ? N2 Li2 O2 C20 -45.4(14) . . . . ? N1 Li2 O2 C20 59.5(15) . . . . ? Li1 Li2 O2 C20 7.2(14) . . . . ? B1 Li2 O2 C20 -38.2(19) . . . . ? B1 Li2 O2 C20 51(2) 5_565 . . . ? O3' Li2 O2 C23 -37.5(16) . . . . ? O2' Li2 O2 C23 118(15) . . . . ? O3 Li2 O2 C23 -35.3(15) . . . . ? N2 Li2 O2 C23 95.5(14) . . . . ? N1 Li2 O2 C23 -159.6(12) . . . . ? Li1 Li2 O2 C23 148.1(13) . . . . ? B1 Li2 O2 C23 102.6(12) . . . . ? B1 Li2 O2 C23 -168.2(7) 5_565 . . . ? C23 O2 C20 C21 16.9(18) . . . . ? Li2 O2 C20 C21 162.5(10) . . . . ? O2 C20 C21 C22 -33.3(13) . . . . ? C20 C21 C22 C23 36.9(10) . . . . ? C20 O2 C23 C22 7.1(19) . . . . ? Li2 O2 C23 C22 -136.3(11) . . . . ? C21 C22 C23 O2 -27.7(14) . . . . ? O3' Li2 O2' C23' -31(3) . . . . ? O3 Li2 O2' C23' -29(3) . . . . ? O2 Li2 O2' C23' -57(11) . . . . ? N2 Li2 O2' C23' 102(3) . . . . ? N1 Li2 O2' C23' -157(3) . . . . ? Li1 Li2 O2' C23' 153(3) . . . . ? B1 Li2 O2' C23' 111(2) . . . . ? B1 Li2 O2' C23' -172.8(15) 5_565 . . . ? O3' Li2 O2' C20' 170(3) . . . . ? O3 Li2 O2' C20' 172(3) . . . . ? O2 Li2 O2' C20' 145(16) . . . . ? N2 Li2 O2' C20' -56(3) . . . . ? N1 Li2 O2' C20' 44(3) . . . . ? Li1 Li2 O2' C20' -5(3) . . . . ? B1 Li2 O2' C20' -48(4) . . . . ? B1 Li2 O2' C20' 29(5) 5_565 . . . ? C23' O2' C20' C21' -27(3) . . . . ? Li2 O2' C20' C21' 135(2) . . . . ? O2' C20' C21' C22' 43(2) . . . . ? C20' C21' C22' C23' -41.2(18) . . . . ? C20' O2' C23' C22' 0(4) . . . . ? Li2 O2' C23' C22' -161(2) . . . . ? C21' C22' C23' O2' 26(3) . . . . ? O3' Li2 O3 C33 -44(7) . . . . ? O2' Li2 O3 C33 154.9(17) . . . . ? O2 Li2 O3 C33 157.8(14) . . . . ? N2 Li2 O3 C33 33.3(16) . . . . ? N1 Li2 O3 C33 -78.5(12) . . . . ? Li1 Li2 O3 C33 -34(2) . . . . ? B1 Li2 O3 C33 -1.3(14) . . . . ? B1 Li2 O3 C33 -43.8(13) 5_565 . . . ? O3' Li2 O3 C30 81(8) . . . . ? O2' Li2 O3 C30 -79.4(18) . . . . ? O2 Li2 O3 C30 -76.5(15) . . . . ? N2 Li2 O3 C30 159.0(11) . . . . ? N1 Li2 O3 C30 47.1(15) . . . . ? Li1 Li2 O3 C30 91.5(18) . . . . ? B1 Li2 O3 C30 124.4(12) . . . . ? B1 Li2 O3 C30 81.8(14) 5_565 . . . ? C33 O3 C30 C31 -26(2) . . . . ? Li2 O3 C30 C31 -158.9(10) . . . . ? O3 C30 C31 C32 34.8(17) . . . . ? C30 C31 C32 C33 -30.9(12) . . . . ? C31 C32 C33 O3 16.0(14) . . . . ? C30 O3 C33 C32 6.2(19) . . . . ? Li2 O3 C33 C32 135.1(10) . . . . ? O2' Li2 O3' C33' 117(3) . . . . ? O3 Li2 O3' C33' 97(9) . . . . ? O2 Li2 O3' C33' 120(2) . . . . ? N2 Li2 O3' C33' -9(3) . . . . ? N1 Li2 O3' C33' -115(2) . . . . ? Li1 Li2 O3' C33' -75(3) . . . . ? B1 Li2 O3' C33' -41(3) . . . . ? B1 Li2 O3' C33' -82(2) 5_565 . . . ? O2' Li2 O3' C30' -64(2) . . . . ? O3 Li2 O3' C30' -84(8) . . . . ? O2 Li2 O3' C30' -61(2) . . . . ? N2 Li2 O3' C30' 170.5(16) . . . . ? N1 Li2 O3' C30' 64(2) . . . . ? Li1 Li2 O3' C30' 104(2) . . . . ? B1 Li2 O3' C30' 138.4(19) . . . . ? B1 Li2 O3' C30' 97(2) 5_565 . . . ? C33' O3' C30' C31' 24(3) . . . . ? Li2 O3' C30' C31' -155.3(15) . . . . ? O3' C30' C31' C32' -23(2) . . . . ? C30' C31' C32' C33' 14.3(17) . . . . ? C30' O3' C33' C32' -15(2) . . . . ? Li2 O3' C33' C32' 164.3(18) . . . . ? C31' C32' C33' O3' -0.3(18) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.211 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.034 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 277648' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C48 H68 B2 Li4 N4 O4' _chemical_formula_sum 'C48 H68 B2 Li4 N4 O4' _chemical_formula_weight 814.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Li Li -0.0003 0.0001 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.9600(9) _cell_length_b 15.0470(8) _cell_length_c 18.4848(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4717.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 137 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _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 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_decay_% 0 _diffrn_reflns_number 29694 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5399 _reflns_number_gt 3535 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+1.4690P] 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_number_reflns 5399 _refine_ls_number_parameters 330 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1273 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.033 _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 0.03584(11) 0.98794(12) 0.46493(11) 0.0258(4) Uani 1 1 d . . . C30 C 0.03425(10) 0.95998(11) 0.32754(9) 0.0266(4) Uani 1 1 d . . . C31 C 0.01126(11) 0.88877(12) 0.28160(10) 0.0320(4) Uani 1 1 d . . . C32 C 0.04395(12) 0.87939(13) 0.21324(10) 0.0390(5) Uani 1 1 d . . . H32 H 0.0289 0.8302 0.1841 0.047 Uiso 1 1 calc R . . C33 C 0.09773(13) 0.93967(14) 0.18665(11) 0.0429(5) Uani 1 1 d . . . H33 H 0.1213 0.9313 0.1405 0.051 Uiso 1 1 calc R . . C34 C 0.11666(12) 1.01287(13) 0.22879(11) 0.0386(5) Uani 1 1 d . . . H34 H 0.1521 1.0561 0.2101 0.046 Uiso 1 1 calc R . . C35 C 0.08534(11) 1.02482(11) 0.29755(10) 0.0304(4) Uani 1 1 d . . . C36 C -0.04998(12) 0.82331(13) 0.30708(11) 0.0423(5) Uani 1 1 d . . . H36A H -0.0618 0.7813 0.2681 0.063 Uiso 1 1 calc R . . H36B H -0.0981 0.8553 0.3206 0.063 Uiso 1 1 calc R . . H36C H -0.0298 0.7908 0.3491 0.063 Uiso 1 1 calc R . . C37 C 0.10153(12) 1.11034(12) 0.33691(11) 0.0367(4) Uani 1 1 d . . . H37A H 0.1358 1.1480 0.3073 0.055 Uiso 1 1 calc R . . H37B H 0.1276 1.0974 0.3830 0.055 Uiso 1 1 calc R . . H37C H 0.0517 1.1413 0.3461 0.055 Uiso 1 1 calc R . . C38 C 0.18517(10) 0.96906(12) 0.45368(9) 0.0281(4) Uani 1 1 d . A . C39 C 0.19521(10) 0.88601(12) 0.41861(10) 0.0314(4) Uani 1 1 d . . . C40 C 0.26389(11) 0.86923(13) 0.37943(10) 0.0394(5) Uani 1 1 d . . . H40 H 0.2691 0.8142 0.3546 0.047 Uiso 1 1 calc R . . C41 C 0.32451(12) 0.93024(15) 0.37565(11) 0.0437(5) Uani 1 1 d . . . H41 H 0.3695 0.9192 0.3464 0.052 Uiso 1 1 calc R . . C42 C 0.31853(11) 1.00767(14) 0.41528(11) 0.0397(5) Uani 1 1 d . . . H42 H 0.3613 1.0484 0.4154 0.048 Uiso 1 1 calc R . . C43 C 0.25110(10) 1.02740(12) 0.45508(10) 0.0334(4) Uani 1 1 d . . . C44 C 0.13432(12) 0.81403(12) 0.42685(11) 0.0378(5) Uani 1 1 d . . . H44A H 0.1213 0.8067 0.4782 0.057 Uiso 1 1 calc R . . H44B H 0.1553 0.7580 0.4078 0.057 Uiso 1 1 calc R . . H44C H 0.0867 0.8304 0.3999 0.057 Uiso 1 1 calc R . . C45 C 0.24757(12) 1.11110(13) 0.49924(12) 0.0428(5) Uani 1 1 d . . . H45A H 0.2997 1.1392 0.5000 0.064 Uiso 1 1 calc R . . H45B H 0.2314 1.0967 0.5488 0.064 Uiso 1 1 calc R . . H45C H 0.2093 1.1521 0.4777 0.064 Uiso 1 1 calc R . . Li1 Li -0.08386(18) 1.0546(2) 0.41494(17) 0.0348(7) Uani 1 1 d . . . Li2 Li -0.07888(18) 0.8955(2) 0.45584(17) 0.0339(7) Uani 1 1 d . . . N1 N 0.00027(8) 0.96808(9) 0.39596(7) 0.0262(3) Uani 1 1 d . A . N2 N 0.11624(8) 0.99233(9) 0.49053(8) 0.0270(3) Uani 1 1 d . . . O1 O -0.1171(6) 1.1406(8) 0.3465(6) 0.0302(17) Uani 0.415(16) 1 d PDU A 1 C10 C -0.1738(8) 1.2066(9) 0.3630(7) 0.036(2) Uani 0.415(16) 1 d PDU A 1 H10A H -0.1478 1.2595 0.3842 0.043 Uiso 0.415(16) 1 calc PR A 1 H10B H -0.2126 1.1834 0.3983 0.043 Uiso 0.415(16) 1 calc PR A 1 C11 C -0.2137(12) 1.2303(14) 0.2941(8) 0.046(4) Uani 0.415(16) 1 d PDU A 1 H11A H -0.2129 1.2954 0.2864 0.055 Uiso 0.415(16) 1 calc PR A 1 H11B H -0.2691 1.2098 0.2943 0.055 Uiso 0.415(16) 1 calc PR A 1 C12 C -0.1674(6) 1.1838(8) 0.2366(4) 0.051(2) Uani 0.415(16) 1 d PDU A 1 H12A H -0.2025 1.1442 0.2084 0.061 Uiso 0.415(16) 1 calc PR A 1 H12B H -0.1440 1.2279 0.2032 0.061 Uiso 0.415(16) 1 calc PR A 1 C13 C -0.1083(4) 1.1344(6) 0.2694(5) 0.0354(17) Uani 0.415(16) 1 d PDU A 1 H13A H -0.0560 1.1574 0.2549 0.042 Uiso 0.415(16) 1 calc PR A 1 H13B H -0.1120 1.0715 0.2541 0.042 Uiso 0.415(16) 1 calc PR A 1 O1' O -0.1279(7) 1.1330(8) 0.3487(5) 0.070(3) Uani 0.585(16) 1 d PDU A 2 C10' C -0.1910(7) 1.1909(8) 0.3583(5) 0.061(3) Uani 0.585(16) 1 d PDU A 2 H10C H -0.1731 1.2447 0.3844 0.073 Uiso 0.585(16) 1 calc PR A 2 H10D H -0.2324 1.1617 0.3877 0.073 Uiso 0.585(16) 1 calc PR A 2 C11' C -0.2237(8) 1.2162(10) 0.2861(6) 0.040(2) Uani 0.585(16) 1 d PDU A 2 H11C H -0.2059 1.2762 0.2712 0.048 Uiso 0.585(16) 1 calc PR A 2 H11D H -0.2821 1.2143 0.2858 0.048 Uiso 0.585(16) 1 calc PR A 2 C12' C -0.1890(4) 1.1452(6) 0.2386(3) 0.0487(16) Uani 0.585(16) 1 d PDU A 2 H12C H -0.2306 1.1022 0.2247 0.058 Uiso 0.585(16) 1 calc PR A 2 H12D H -0.1676 1.1722 0.1939 0.058 Uiso 0.585(16) 1 calc PR A 2 C13' C -0.1314(7) 1.1031(7) 0.2745(4) 0.082(3) Uani 0.585(16) 1 d PDU A 2 H13C H -0.0802 1.1147 0.2504 0.099 Uiso 0.585(16) 1 calc PR A 2 H13D H -0.1411 1.0382 0.2733 0.099 Uiso 0.585(16) 1 calc PR A 2 O2 O -0.07873(7) 0.76805(8) 0.48246(7) 0.0363(3) Uani 1 1 d . . . C20 C -0.03324(11) 0.72849(12) 0.53945(10) 0.0348(4) Uani 1 1 d . A . H20A H -0.0660 0.7201 0.5832 0.042 Uiso 1 1 calc R . . H20B H 0.0123 0.7666 0.5520 0.042 Uiso 1 1 calc R . . C21 C -0.00545(13) 0.63959(14) 0.51032(13) 0.0475(5) Uani 1 1 d . . . H21A H -0.0080 0.5932 0.5482 0.057 Uiso 1 1 calc R A . H21B H 0.0493 0.6437 0.4921 0.057 Uiso 1 1 calc R . . C22 C -0.06271(16) 0.61906(14) 0.44886(13) 0.0575(6) Uani 1 1 d . A . H22A H -0.0350 0.6174 0.4018 0.069 Uiso 1 1 calc R . . H22B H -0.0893 0.5613 0.4568 0.069 Uiso 1 1 calc R . . C23 C -0.12119(13) 0.69464(14) 0.45124(12) 0.0442(5) Uani 1 1 d . A . H23A H -0.1398 0.7096 0.4020 0.053 Uiso 1 1 calc R . . H23B H -0.1673 0.6788 0.4815 0.053 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 B1 0.0258(10) 0.0229(9) 0.0288(10) 0.0027(7) -0.0010(8) -0.0002(8) C30 0.0244(9) 0.0291(8) 0.0264(9) 0.0024(7) -0.0034(7) 0.0051(7) C31 0.0342(10) 0.0335(9) 0.0282(9) 0.0002(7) -0.0059(7) 0.0028(8) C32 0.0511(12) 0.0376(10) 0.0282(10) -0.0027(8) -0.0051(8) 0.0022(9) C33 0.0555(13) 0.0468(12) 0.0264(10) 0.0003(8) 0.0071(9) 0.0036(10) C34 0.0447(12) 0.0378(11) 0.0335(10) 0.0075(8) 0.0052(9) -0.0021(9) C35 0.0317(10) 0.0297(9) 0.0298(9) 0.0035(7) -0.0030(8) 0.0029(7) C36 0.0446(12) 0.0434(11) 0.0389(11) -0.0074(9) -0.0027(9) -0.0101(9) C37 0.0435(11) 0.0320(10) 0.0348(11) 0.0054(8) 0.0015(8) -0.0044(8) C38 0.0234(9) 0.0352(9) 0.0256(9) 0.0043(7) -0.0039(7) 0.0018(7) C39 0.0288(9) 0.0370(10) 0.0284(9) 0.0030(8) -0.0052(7) 0.0066(8) C40 0.0352(11) 0.0462(11) 0.0366(11) -0.0030(9) -0.0028(8) 0.0143(9) C41 0.0297(10) 0.0615(14) 0.0397(12) 0.0050(10) 0.0067(9) 0.0097(10) C42 0.0244(9) 0.0502(12) 0.0445(12) 0.0074(9) 0.0003(8) -0.0001(8) C43 0.0249(9) 0.0383(10) 0.0368(10) 0.0054(8) -0.0031(8) 0.0013(8) C44 0.0384(11) 0.0313(10) 0.0436(12) -0.0019(8) -0.0039(9) 0.0044(8) C45 0.0273(10) 0.0433(11) 0.0578(13) -0.0034(10) -0.0018(9) -0.0075(8) Li1 0.0348(17) 0.0372(17) 0.0324(17) 0.0042(13) -0.0021(13) 0.0063(13) Li2 0.0327(17) 0.0307(15) 0.0384(17) -0.0016(13) -0.0001(13) -0.0021(13) N1 0.0247(7) 0.0269(7) 0.0270(8) 0.0008(6) -0.0011(6) 0.0008(6) N2 0.0246(7) 0.0276(7) 0.0286(8) 0.0013(6) -0.0006(6) 0.0011(6) O1 0.028(3) 0.034(3) 0.029(3) 0.005(3) -0.003(2) 0.013(2) C10 0.029(5) 0.039(3) 0.039(4) 0.004(3) -0.012(3) 0.009(3) C11 0.043(6) 0.038(5) 0.057(6) -0.004(4) -0.026(4) 0.006(5) C12 0.060(5) 0.061(5) 0.032(3) 0.014(3) -0.015(3) -0.009(4) C13 0.040(3) 0.036(4) 0.031(3) 0.004(3) 0.006(2) 0.008(3) O1' 0.091(6) 0.082(6) 0.036(3) 0.005(3) -0.004(3) 0.048(4) C10' 0.041(5) 0.098(7) 0.045(3) -0.012(4) -0.005(3) 0.035(5) C11' 0.036(4) 0.044(5) 0.041(3) -0.003(3) -0.015(3) 0.004(4) C12' 0.044(3) 0.058(4) 0.044(2) -0.009(3) -0.007(2) 0.006(2) C13' 0.148(8) 0.063(5) 0.036(3) -0.008(3) -0.015(4) 0.048(5) O2 0.0355(7) 0.0300(6) 0.0433(8) 0.0038(6) -0.0071(6) -0.0030(5) C20 0.0351(10) 0.0328(9) 0.0365(11) 0.0004(8) -0.0059(8) 0.0006(8) C21 0.0477(13) 0.0390(11) 0.0559(14) -0.0055(10) -0.0005(10) 0.0092(10) C22 0.0896(19) 0.0386(12) 0.0442(13) -0.0070(10) -0.0040(12) -0.0049(12) C23 0.0455(12) 0.0451(12) 0.0420(12) 0.0068(9) -0.0118(9) -0.0165(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N1 1.442(2) . ? B1 N2 1.445(2) . ? B1 B1 1.814(4) 5_576 ? B1 Li2 2.398(4) . ? B1 Li2 2.399(4) 5_576 ? B1 Li1 2.446(4) . ? B1 Li1 2.450(4) 5_576 ? C30 N1 1.395(2) . ? C30 C35 1.418(2) . ? C30 C31 1.422(2) . ? C31 C32 1.387(3) . ? C31 C36 1.507(3) . ? C32 C33 1.377(3) . ? C32 H32 0.9500 . ? C33 C34 1.387(3) . ? C33 H33 0.9500 . ? C34 C35 1.389(3) . ? C34 H34 0.9500 . ? C35 C37 1.503(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 N2 1.398(2) . ? C38 C39 1.418(3) . ? C38 C43 1.422(2) . ? C39 C40 1.395(3) . ? C39 C44 1.504(3) . ? C40 C41 1.380(3) . ? C40 H40 0.9500 . ? C41 C42 1.380(3) . ? C41 H41 0.9500 . ? C42 C43 1.392(3) . ? C42 H42 0.9500 . ? C43 C45 1.502(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? Li1 O1' 1.857(10) . ? Li1 O1 1.896(11) . ? Li1 N2 1.963(3) 5_576 ? Li1 N1 1.963(3) . ? Li1 B1 2.450(4) 5_576 ? Li1 Li2 2.512(4) . ? Li2 O2 1.980(3) . ? Li2 N1 2.054(3) . ? Li2 N2 2.057(3) 5_576 ? Li2 B1 2.399(4) 5_576 ? N2 Li1 1.963(3) 5_576 ? N2 Li2 2.057(3) 5_576 ? O1 C10 1.415(10) . ? O1 C13 1.435(10) . ? C10 C11 1.487(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.494(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.388(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O1' C10' 1.391(9) . ? O1' C13' 1.446(9) . ? C10' C11' 1.497(9) . ? C10' H10C 0.9900 . ? C10' H10D 0.9900 . ? C11' C12' 1.503(8) . ? C11' H11C 0.9900 . ? C11' H11D 0.9900 . ? C12' C13' 1.340(7) . ? C12' H12C 0.9900 . ? C12' H12D 0.9900 . ? C13' H13C 0.9900 . ? C13' H13D 0.9900 . ? O2 C20 1.435(2) . ? O2 C23 1.439(2) . ? C20 C21 1.517(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.526(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.510(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 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 N1 B1 N2 133.95(16) . . ? N1 B1 B1 113.14(18) . 5_576 ? N2 B1 B1 112.90(18) . 5_576 ? N1 B1 Li2 58.55(12) . . ? N2 B1 Li2 144.62(15) . . ? B1 B1 Li2 67.81(13) 5_576 . ? N1 B1 Li2 144.97(14) . 5_576 ? N2 B1 Li2 58.63(11) . 5_576 ? B1 B1 Li2 67.75(13) 5_576 5_576 ? Li2 B1 Li2 135.55(10) . 5_576 ? N1 B1 Li1 53.39(11) . . ? N2 B1 Li1 152.67(15) . . ? B1 B1 Li1 68.39(13) 5_576 . ? Li2 B1 Li1 62.48(11) . . ? Li2 B1 Li1 100.57(13) 5_576 . ? N1 B1 Li1 152.40(15) . 5_576 ? N2 B1 Li1 53.23(11) . 5_576 ? B1 B1 Li1 68.12(13) 5_576 5_576 ? Li2 B1 Li1 100.46(13) . 5_576 ? Li2 B1 Li1 62.39(11) 5_576 5_576 ? Li1 B1 Li1 136.51(10) . 5_576 ? N1 C30 C35 123.14(15) . . ? N1 C30 C31 119.60(16) . . ? C35 C30 C31 116.93(16) . . ? C32 C31 C30 120.75(17) . . ? C32 C31 C36 119.57(17) . . ? C30 C31 C36 119.68(16) . . ? C33 C32 C31 121.51(18) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C32 C33 C34 118.43(18) . . ? C32 C33 H33 120.8 . . ? C34 C33 H33 120.8 . . ? C33 C34 C35 121.89(18) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? C34 C35 C30 120.14(17) . . ? C34 C35 C37 118.93(17) . . ? C30 C35 C37 120.76(16) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N2 C38 C39 122.96(16) . . ? N2 C38 C43 119.62(16) . . ? C39 C38 C43 117.26(16) . . ? C40 C39 C38 119.82(17) . . ? C40 C39 C44 119.71(17) . . ? C38 C39 C44 120.38(16) . . ? C41 C40 C39 121.87(18) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C42 C41 C40 118.69(18) . . ? C42 C41 H41 120.7 . . ? C40 C41 H41 120.7 . . ? C41 C42 C43 121.40(18) . . ? C41 C42 H42 119.3 . . ? C43 C42 H42 119.3 . . ? C42 C43 C38 120.33(18) . . ? C42 C43 C45 119.92(17) . . ? C38 C43 C45 119.75(16) . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O1' Li1 O1 6.6(7) . . ? O1' Li1 N2 134.7(4) . 5_576 ? O1 Li1 N2 139.2(4) . 5_576 ? O1' Li1 N1 126.6(4) . . ? O1 Li1 N1 123.4(4) . . ? N2 Li1 N1 97.10(14) 5_576 . ? O1' Li1 B1 147.5(4) . . ? O1 Li1 B1 141.2(4) . . ? N2 Li1 B1 75.42(12) 5_576 . ? N1 Li1 B1 36.12(8) . . ? O1' Li1 B1 153.8(4) . 5_576 ? O1 Li1 B1 151.9(4) . 5_576 ? N2 Li1 B1 36.13(8) 5_576 5_576 ? N1 Li1 B1 75.35(11) . 5_576 ? B1 Li1 B1 43.49(10) . 5_576 ? O1' Li1 Li2 144.8(4) . . ? O1 Li1 Li2 149.5(4) . . ? N2 Li1 Li2 53.03(11) 5_576 . ? N1 Li1 Li2 52.93(11) . . ? B1 Li1 Li2 57.82(11) . . ? B1 Li1 Li2 57.79(11) 5_576 . ? O2 Li2 N1 130.39(17) . . ? O2 Li2 N2 132.47(17) . 5_576 ? N1 Li2 N2 91.42(13) . 5_576 ? O2 Li2 B1 122.92(16) . . ? N1 Li2 B1 36.78(8) . . ? N2 Li2 B1 74.95(11) 5_576 . ? O2 Li2 B1 123.78(16) . 5_576 ? N1 Li2 B1 75.01(11) . 5_576 ? N2 Li2 B1 36.84(8) 5_576 5_576 ? B1 Li2 B1 44.45(10) . 5_576 ? O2 Li2 Li1 176.36(18) . . ? N1 Li2 Li1 49.70(10) . . ? N2 Li2 Li1 49.67(11) 5_576 . ? B1 Li2 Li1 59.70(11) . . ? B1 Li2 Li1 59.81(11) 5_576 . ? C30 N1 B1 130.30(15) . . ? C30 N1 Li1 121.35(14) . . ? B1 N1 Li1 90.50(14) . . ? C30 N1 Li2 135.39(14) . . ? B1 N1 Li2 84.68(13) . . ? Li1 N1 Li2 77.37(13) . . ? C38 N2 B1 128.19(15) . . ? C38 N2 Li1 125.29(14) . 5_576 ? B1 N2 Li1 90.64(14) . 5_576 ? C38 N2 Li2 134.27(14) . 5_576 ? B1 N2 Li2 84.53(13) . 5_576 ? Li1 N2 Li2 77.30(14) 5_576 5_576 ? C10 O1 C13 109.4(8) . . ? C10 O1 Li1 122.5(9) . . ? C13 O1 Li1 125.9(8) . . ? O1 C10 C11 107.0(9) . . ? O1 C10 H10A 110.3 . . ? C11 C10 H10A 110.3 . . ? O1 C10 H10B 110.3 . . ? C11 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? C10 C11 C12 104.9(9) . . ? C10 C11 H11A 110.8 . . ? C12 C11 H11A 110.8 . . ? C10 C11 H11B 110.8 . . ? C12 C11 H11B 110.8 . . ? H11A C11 H11B 108.8 . . ? C13 C12 C11 108.6(7) . . ? C13 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? C13 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.3 . . ? C12 C13 O1 108.8(7) . . ? C12 C13 H13A 109.9 . . ? O1 C13 H13A 109.9 . . ? C12 C13 H13B 109.9 . . ? O1 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C10' O1' C13' 106.5(7) . . ? C10' O1' Li1 128.5(8) . . ? C13' O1' Li1 116.4(7) . . ? O1' C10' C11' 109.3(7) . . ? O1' C10' H10C 109.8 . . ? C11' C10' H10C 109.8 . . ? O1' C10' H10D 109.8 . . ? C11' C10' H10D 109.8 . . ? H10C C10' H10D 108.3 . . ? C10' C11' C12' 101.2(7) . . ? C10' C11' H11C 111.5 . . ? C12' C11' H11C 111.5 . . ? C10' C11' H11D 111.5 . . ? C12' C11' H11D 111.5 . . ? H11C C11' H11D 109.3 . . ? C13' C12' C11' 109.5(6) . . ? C13' C12' H12C 109.8 . . ? C11' C12' H12C 109.8 . . ? C13' C12' H12D 109.8 . . ? C11' C12' H12D 109.8 . . ? H12C C12' H12D 108.2 . . ? C12' C13' O1' 110.6(6) . . ? C12' C13' H13C 109.5 . . ? O1' C13' H13C 109.5 . . ? C12' C13' H13D 109.5 . . ? O1' C13' H13D 109.5 . . ? H13C C13' H13D 108.1 . . ? C20 O2 C23 104.18(13) . . ? C20 O2 Li2 125.80(14) . . ? C23 O2 Li2 130.02(15) . . ? O2 C20 C21 105.79(15) . . ? O2 C20 H20A 110.6 . . ? C21 C20 H20A 110.6 . . ? O2 C20 H20B 110.6 . . ? C21 C20 H20B 110.6 . . ? H20A C20 H20B 108.7 . . ? C20 C21 C22 104.19(17) . . ? C20 C21 H21A 110.9 . . ? C22 C21 H21A 110.9 . . ? C20 C21 H21B 110.9 . . ? C22 C21 H21B 110.9 . . ? H21A C21 H21B 108.9 . . ? C23 C22 C21 104.11(17) . . ? C23 C22 H22A 110.9 . . ? C21 C22 H22A 110.9 . . ? C23 C22 H22B 110.9 . . ? C21 C22 H22B 110.9 . . ? H22A C22 H22B 109.0 . . ? O2 C23 C22 105.13(16) . . ? O2 C23 H23A 110.7 . . ? C22 C23 H23A 110.7 . . ? O2 C23 H23B 110.7 . . ? C22 C23 H23B 110.7 . . ? H23A C23 H23B 108.8 . . ? 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 N1 C30 C31 C32 179.78(16) . . . . ? C35 C30 C31 C32 6.2(3) . . . . ? N1 C30 C31 C36 0.5(2) . . . . ? C35 C30 C31 C36 -173.12(16) . . . . ? C30 C31 C32 C33 -1.9(3) . . . . ? C36 C31 C32 C33 177.36(19) . . . . ? C31 C32 C33 C34 -2.5(3) . . . . ? C32 C33 C34 C35 2.5(3) . . . . ? C33 C34 C35 C30 1.9(3) . . . . ? C33 C34 C35 C37 -173.50(19) . . . . ? N1 C30 C35 C34 -179.48(16) . . . . ? C31 C30 C35 C34 -6.1(3) . . . . ? N1 C30 C35 C37 -4.2(3) . . . . ? C31 C30 C35 C37 169.18(16) . . . . ? N2 C38 C39 C40 176.42(16) . . . . ? C43 C38 C39 C40 -8.3(2) . . . . ? N2 C38 C39 C44 -7.0(3) . . . . ? C43 C38 C39 C44 168.31(16) . . . . ? C38 C39 C40 C41 2.4(3) . . . . ? C44 C39 C40 C41 -174.19(18) . . . . ? C39 C40 C41 C42 3.8(3) . . . . ? C40 C41 C42 C43 -3.9(3) . . . . ? C41 C42 C43 C38 -2.3(3) . . . . ? C41 C42 C43 C45 178.29(18) . . . . ? N2 C38 C43 C42 -176.29(16) . . . . ? C39 C38 C43 C42 8.2(3) . . . . ? N2 C38 C43 C45 3.2(3) . . . . ? C39 C38 C43 C45 -172.33(16) . . . . ? N1 B1 Li1 O1' -74.3(7) . . . . ? N2 B1 Li1 O1' 42.2(8) . . . . ? B1 B1 Li1 O1' 140.5(7) 5_576 . . . ? Li2 B1 Li1 O1' -144.1(7) . . . . ? Li2 B1 Li1 O1' 79.7(7) 5_576 . . . ? Li1 B1 Li1 O1' 140.5(7) 5_576 . . . ? N1 B1 Li1 O1 -77.5(6) . . . . ? N2 B1 Li1 O1 38.9(7) . . . . ? B1 B1 Li1 O1 137.3(6) 5_576 . . . ? Li2 B1 Li1 O1 -147.3(6) . . . . ? Li2 B1 Li1 O1 76.5(6) 5_576 . . . ? Li1 B1 Li1 O1 137.3(6) 5_576 . . . ? N1 B1 Li1 N2 124.97(16) . . . 5_576 ? N2 B1 Li1 N2 -118.6(3) . . . 5_576 ? B1 B1 Li1 N2 -20.21(12) 5_576 . . 5_576 ? Li2 B1 Li1 N2 55.21(12) . . . 5_576 ? Li2 B1 Li1 N2 -80.98(13) 5_576 . . 5_576 ? Li1 B1 Li1 N2 -20.21(12) 5_576 . . 5_576 ? N2 B1 Li1 N1 116.5(4) . . . . ? B1 B1 Li1 N1 -145.19(19) 5_576 . . . ? Li2 B1 Li1 N1 -69.76(14) . . . . ? Li2 B1 Li1 N1 154.04(16) 5_576 . . . ? Li1 B1 Li1 N1 -145.19(19) 5_576 . . . ? N1 B1 Li1 B1 145.19(19) . . . 5_576 ? N2 B1 Li1 B1 -98.3(4) . . . 5_576 ? Li2 B1 Li1 B1 75.42(14) . . . 5_576 ? Li2 B1 Li1 B1 -60.77(13) 5_576 . . 5_576 ? Li1 B1 Li1 B1 0.0 5_576 . . 5_576 ? N1 B1 Li1 Li2 69.76(14) . . . . ? N2 B1 Li1 Li2 -173.8(3) . . . . ? B1 B1 Li1 Li2 -75.42(14) 5_576 . . . ? Li2 B1 Li1 Li2 -136.19(10) 5_576 . . . ? Li1 B1 Li1 Li2 -75.42(14) 5_576 . . . ? N1 B1 Li2 O2 115.0(2) . . . . ? N2 B1 Li2 O2 -7.9(4) . . . . ? B1 B1 Li2 O2 -106.6(2) 5_576 . . . ? Li2 B1 Li2 O2 -106.6(2) 5_576 . . . ? Li1 B1 Li2 O2 177.0(2) . . . . ? Li1 B1 Li2 O2 -45.6(2) 5_576 . . . ? N2 B1 Li2 N1 -122.9(3) . . . . ? B1 B1 Li2 N1 138.34(18) 5_576 . . . ? Li2 B1 Li2 N1 138.34(18) 5_576 . . . ? Li1 B1 Li2 N1 61.99(13) . . . . ? Li1 B1 Li2 N1 -160.65(15) 5_576 . . . ? N1 B1 Li2 N2 -113.74(14) . . . 5_576 ? N2 B1 Li2 N2 123.3(2) . . . 5_576 ? B1 B1 Li2 N2 24.60(12) 5_576 . . 5_576 ? Li2 B1 Li2 N2 24.60(12) 5_576 . . 5_576 ? Li1 B1 Li2 N2 -51.75(11) . . . 5_576 ? Li1 B1 Li2 N2 85.61(13) 5_576 . . 5_576 ? N1 B1 Li2 B1 -138.34(18) . . . 5_576 ? N2 B1 Li2 B1 98.7(3) . . . 5_576 ? Li2 B1 Li2 B1 0.0 5_576 . . 5_576 ? Li1 B1 Li2 B1 -76.35(14) . . . 5_576 ? Li1 B1 Li2 B1 61.01(13) 5_576 . . 5_576 ? N1 B1 Li2 Li1 -61.99(13) . . . . ? N2 B1 Li2 Li1 175.1(3) . . . . ? B1 B1 Li2 Li1 76.35(14) 5_576 . . . ? Li2 B1 Li2 Li1 76.35(14) 5_576 . . . ? Li1 B1 Li2 Li1 137.36(10) 5_576 . . . ? O1' Li1 Li2 N1 102.9(6) . . . . ? O1 Li1 Li2 N1 94.3(8) . . . . ? N2 Li1 Li2 N1 -139.70(17) 5_576 . . . ? B1 Li1 Li2 N1 -43.88(9) . . . . ? B1 Li1 Li2 N1 -95.81(13) 5_576 . . . ? O1' Li1 Li2 N2 -117.4(7) . . . 5_576 ? O1 Li1 Li2 N2 -126.0(8) . . . 5_576 ? N1 Li1 Li2 N2 139.70(17) . . . 5_576 ? B1 Li1 Li2 N2 95.82(13) . . . 5_576 ? B1 Li1 Li2 N2 43.89(9) 5_576 . . 5_576 ? O1' Li1 Li2 B1 146.8(7) . . . . ? O1 Li1 Li2 B1 138.2(8) . . . . ? N2 Li1 Li2 B1 -95.82(13) 5_576 . . . ? N1 Li1 Li2 B1 43.88(9) . . . . ? B1 Li1 Li2 B1 -51.93(11) 5_576 . . . ? O1' Li1 Li2 B1 -161.3(7) . . . 5_576 ? O1 Li1 Li2 B1 -169.9(8) . . . 5_576 ? N2 Li1 Li2 B1 -43.89(9) 5_576 . . 5_576 ? N1 Li1 Li2 B1 95.81(13) . . . 5_576 ? B1 Li1 Li2 B1 51.93(11) . . . 5_576 ? C35 C30 N1 B1 -50.5(3) . . . . ? C31 C30 N1 B1 136.33(18) . . . . ? C35 C30 N1 Li1 71.5(2) . . . . ? C31 C30 N1 Li1 -101.67(19) . . . . ? C35 C30 N1 Li2 176.16(17) . . . . ? C31 C30 N1 Li2 3.0(3) . . . . ? N2 B1 N1 C30 -11.6(3) . . . . ? B1 B1 N1 C30 168.84(16) 5_576 . . . ? Li2 B1 N1 C30 -149.1(2) . . . . ? Li2 B1 N1 C30 85.0(3) 5_576 . . . ? Li1 B1 N1 C30 133.6(2) . . . . ? Li1 B1 N1 C30 -104.4(3) 5_576 . . . ? N2 B1 N1 Li1 -145.2(2) . . . . ? B1 B1 N1 Li1 35.26(19) 5_576 . . . ? Li2 B1 N1 Li1 77.27(13) . . . . ? Li2 B1 N1 Li1 -48.6(3) 5_576 . . . ? Li1 B1 N1 Li1 122.0(3) 5_576 . . . ? N2 B1 N1 Li2 137.5(2) . . . . ? B1 B1 N1 Li2 -42.01(18) 5_576 . . . ? Li2 B1 N1 Li2 -125.8(2) 5_576 . . . ? Li1 B1 N1 Li2 -77.27(13) . . . . ? Li1 B1 N1 Li2 44.7(3) 5_576 . . . ? O1' Li1 N1 C30 0.2(5) . . . . ? O1 Li1 N1 C30 -6.8(5) . . . . ? N2 Li1 N1 C30 167.25(14) 5_576 . . . ? B1 Li1 N1 C30 -139.70(19) . . . . ? B1 Li1 N1 C30 -163.66(14) 5_576 . . . ? Li2 Li1 N1 C30 135.87(17) . . . . ? O1' Li1 N1 B1 139.9(5) . . . . ? O1 Li1 N1 B1 132.9(5) . . . . ? N2 Li1 N1 B1 -53.05(15) 5_576 . . . ? B1 Li1 N1 B1 -23.96(14) 5_576 . . . ? Li2 Li1 N1 B1 -84.43(13) . . . . ? O1' Li1 N1 Li2 -135.7(5) . . . . ? O1 Li1 N1 Li2 -142.7(5) . . . . ? N2 Li1 N1 Li2 31.38(14) 5_576 . . . ? B1 Li1 N1 Li2 84.43(13) . . . . ? B1 Li1 N1 Li2 60.47(11) 5_576 . . . ? O2 Li2 N1 C30 53.1(3) . . . . ? N2 Li2 N1 C30 -151.69(16) 5_576 . . . ? B1 Li2 N1 C30 146.2(2) . . . . ? B1 Li2 N1 C30 174.96(17) 5_576 . . . ? Li1 Li2 N1 C30 -122.1(2) . . . . ? O2 Li2 N1 B1 -93.1(2) . . . . ? N2 Li2 N1 B1 62.15(13) 5_576 . . . ? B1 Li2 N1 B1 28.80(13) 5_576 . . . ? Li1 Li2 N1 B1 91.71(14) . . . . ? O2 Li2 N1 Li1 175.2(2) . . . . ? N2 Li2 N1 Li1 -29.55(13) 5_576 . . . ? B1 Li2 N1 Li1 -91.71(14) . . . . ? B1 Li2 N1 Li1 -62.90(12) 5_576 . . . ? C39 C38 N2 B1 -51.2(2) . . . . ? C43 C38 N2 B1 133.55(18) . . . . ? C39 C38 N2 Li1 73.8(2) . . . 5_576 ? C43 C38 N2 Li1 -101.4(2) . . . 5_576 ? C39 C38 N2 Li2 -177.90(18) . . . 5_576 ? C43 C38 N2 Li2 6.9(3) . . . 5_576 ? N1 B1 N2 C38 -6.7(3) . . . . ? B1 B1 N2 C38 172.89(16) 5_576 . . . ? Li2 B1 N2 C38 89.4(3) . . . . ? Li2 B1 N2 C38 -144.8(2) 5_576 . . . ? Li1 B1 N2 C38 -100.2(3) . . . . ? Li1 B1 N2 C38 138.1(2) 5_576 . . . ? N1 B1 N2 Li1 -144.7(2) . . . 5_576 ? B1 B1 N2 Li1 34.84(19) 5_576 . . 5_576 ? Li2 B1 N2 Li1 -48.7(3) . . . 5_576 ? Li2 B1 N2 Li1 77.18(14) 5_576 . . 5_576 ? Li1 B1 N2 Li1 121.8(3) . . . 5_576 ? N1 B1 N2 Li2 138.1(2) . . . 5_576 ? B1 B1 N2 Li2 -42.34(18) 5_576 . . 5_576 ? Li2 B1 N2 Li2 -125.8(2) . . . 5_576 ? Li1 B1 N2 Li2 44.6(3) . . . 5_576 ? Li1 B1 N2 Li2 -77.18(14) 5_576 . . 5_576 ? O1' Li1 O1 C10 64(5) . . . . ? N2 Li1 O1 C10 13.8(13) 5_576 . . . ? N1 Li1 O1 C10 -175.2(8) . . . . ? B1 Li1 O1 C10 -131.7(9) . . . . ? B1 Li1 O1 C10 -49.1(15) 5_576 . . . ? Li2 Li1 O1 C10 112.5(10) . . . . ? O1' Li1 O1 C13 -97(6) . . . . ? N2 Li1 O1 C13 -147.2(7) 5_576 . . . ? N1 Li1 O1 C13 23.8(11) . . . . ? B1 Li1 O1 C13 67.3(11) . . . . ? B1 Li1 O1 C13 149.9(6) 5_576 . . . ? Li2 Li1 O1 C13 -48.5(14) . . . . ? C13 O1 C10 C11 11.4(17) . . . . ? Li1 O1 C10 C11 -152.4(13) . . . . ? O1 C10 C11 C12 -8(2) . . . . ? C10 C11 C12 C13 2.4(19) . . . . ? C11 C12 C13 O1 4.4(14) . . . . ? C10 O1 C13 C12 -10.0(12) . . . . ? Li1 O1 C13 C12 153.0(8) . . . . ? O1 Li1 O1' C10' -122(6) . . . . ? N2 Li1 O1' C10' 13.3(13) 5_576 . . . ? N1 Li1 O1' C10' 175.1(8) . . . . ? B1 Li1 O1' C10' -140.0(8) . . . . ? B1 Li1 O1' C10' -42.4(16) 5_576 . . . ? Li2 Li1 O1' C10' 99.6(11) . . . . ? O1 Li1 O1' C13' 95(6) . . . . ? N2 Li1 O1' C13' -129.9(7) 5_576 . . . ? N1 Li1 O1' C13' 31.9(10) . . . . ? B1 Li1 O1' C13' 76.8(11) . . . . ? B1 Li1 O1' C13' 174.4(8) 5_576 . . . ? Li2 Li1 O1' C13' -43.6(11) . . . . ? C13' O1' C10' C11' -14.0(15) . . . . ? Li1 O1' C10' C11' -160.0(11) . . . . ? O1' C10' C11' C12' 17.0(15) . . . . ? C10' C11' C12' C13' -14.0(13) . . . . ? C11' C12' C13' O1' 6.4(11) . . . . ? C10' O1' C13' C12' 4.8(12) . . . . ? Li1 O1' C13' C12' 155.5(7) . . . . ? N1 Li2 O2 C20 79.3(3) . . . . ? N2 Li2 O2 C20 -66.0(3) 5_576 . . . ? B1 Li2 O2 C20 33.9(3) . . . . ? B1 Li2 O2 C20 -19.9(3) 5_576 . . . ? N1 Li2 O2 C23 -100.1(3) . . . . ? N2 Li2 O2 C23 114.5(2) 5_576 . . . ? B1 Li2 O2 C23 -145.51(18) . . . . ? B1 Li2 O2 C23 160.65(18) 5_576 . . . ? C23 O2 C20 C21 38.5(2) . . . . ? Li2 O2 C20 C21 -141.07(18) . . . . ? O2 C20 C21 C22 -20.9(2) . . . . ? C20 C21 C22 C23 -3.5(2) . . . . ? C20 O2 C23 C22 -40.8(2) . . . . ? Li2 O2 C23 C22 138.71(19) . . . . ? C21 C22 C23 O2 26.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.310 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.040 #===END