# om020809f.cif data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 B10' _chemical_formula_weight 246.34 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2351(9) _cell_length_b 20.900(3) _cell_length_c 9.3366(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.886(3) _cell_angle_gamma 90.00 _cell_volume 1411.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.054 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.6828 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Siemens Smart CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8180 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2773 _reflns_number_gt 1490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2773 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1150 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1770 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 C1 C 0.3048(3) 0.66024(10) 0.3342(2) 0.0364(6) Uani 1 1 d . . . C2 C 0.1969(3) 0.60251(10) 0.4188(2) 0.0377(6) Uani 1 1 d . . . C3 C 0.4375(3) 0.70139(12) 0.4219(3) 0.0491(7) Uani 1 1 d . . . H3A H 0.5431 0.7114 0.3633 0.059 Uiso 1 1 calc R . . H3B H 0.3762 0.7414 0.4439 0.059 Uiso 1 1 calc R . . C5 C 0.6708(3) 0.69628(12) 0.6187(3) 0.0501(7) Uani 1 1 d . . . H5A H 0.7333 0.7285 0.5709 0.060 Uiso 1 1 calc R . . C6 C 0.7419(4) 0.67337(14) 0.7460(3) 0.0608(8) Uani 1 1 d . . . H6A H 0.8504 0.6906 0.7843 0.073 Uiso 1 1 calc R . . C7 C 0.6525(4) 0.62506(14) 0.8164(3) 0.0619(8) Uani 1 1 d . . . H7A H 0.7007 0.6090 0.9021 0.074 Uiso 1 1 calc R . . C8 C 0.4908(4) 0.60053(12) 0.7592(3) 0.0520(7) Uani 1 1 d . . . H8A H 0.4306 0.5678 0.8071 0.062 Uiso 1 1 calc R . . C9 C 0.4157(3) 0.62369(11) 0.6314(2) 0.0415(6) Uani 1 1 d . . . C4 C 0.5068(3) 0.67219(11) 0.5598(2) 0.0400(6) Uani 1 1 d . . . C10 C 0.2357(3) 0.59500(13) 0.5772(3) 0.0512(7) Uani 1 1 d . . . H10A H 0.2359 0.5497 0.5999 0.061 Uiso 1 1 calc R . . H10B H 0.1351 0.6145 0.6290 0.061 Uiso 1 1 calc R . . B3 B 0.3689(4) 0.58241(13) 0.3018(3) 0.0433(7) Uani 1 1 d . . . H3 H 0.498(3) 0.5668(10) 0.350(2) 0.048(6) Uiso 1 1 d . . . B4 B 0.3498(4) 0.63906(14) 0.1629(3) 0.0460(7) Uani 1 1 d . . . H4 H 0.477(3) 0.6570(11) 0.119(2) 0.056(7) Uiso 1 1 d . . . B5 B 0.1683(4) 0.69204(15) 0.2028(3) 0.0485(8) Uani 1 1 d . . . H5 H 0.179(3) 0.7427(11) 0.184(2) 0.047(6) Uiso 1 1 d . . . B6 B 0.0737(4) 0.66923(14) 0.3666(3) 0.0466(8) Uani 1 1 d . . . H6 H 0.041(3) 0.7010(10) 0.448(2) 0.042(6) Uiso 1 1 d . . . B7 B 0.1620(4) 0.53861(14) 0.3077(3) 0.0477(8) Uani 1 1 d . . . H7 H 0.168(3) 0.4925(11) 0.358(2) 0.056(7) Uiso 1 1 d . . . B8 B 0.2569(4) 0.56120(15) 0.1422(4) 0.0525(8) Uani 1 1 d . . . H8 H 0.318(3) 0.5246(13) 0.068(3) 0.082(8) Uiso 1 1 d . . . B9 B 0.1307(4) 0.62928(15) 0.0794(4) 0.0553(8) Uani 1 1 d . . . H9 H 0.104(3) 0.6383(11) -0.038(3) 0.074(8) Uiso 1 1 d . . . B10 B -0.0392(4) 0.64837(16) 0.2081(4) 0.0572(9) Uani 1 1 d . . . H10 H -0.176(3) 0.6707(11) 0.181(3) 0.071(8) Uiso 1 1 d . . . B11 B -0.0201(4) 0.59191(14) 0.3480(4) 0.0492(8) Uani 1 1 d . . . H11 H -0.124(3) 0.5782(10) 0.422(2) 0.051(7) Uiso 1 1 d . . . B12 B 0.0138(4) 0.56730(16) 0.1700(4) 0.0572(9) Uani 1 1 d . . . H12 H -0.088(3) 0.5350(11) 0.125(2) 0.056(7) 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 C1 0.0361(12) 0.0361(12) 0.0371(14) 0.0037(10) 0.0028(10) -0.0049(9) C2 0.0360(12) 0.0379(12) 0.0390(15) 0.0049(11) -0.0014(10) -0.0074(10) C3 0.0520(15) 0.0502(15) 0.0452(16) 0.0002(12) 0.0029(12) -0.0186(12) C5 0.0383(13) 0.0542(16) 0.0579(18) -0.0135(14) 0.0037(12) -0.0031(11) C6 0.0489(16) 0.0664(19) 0.067(2) -0.0228(16) -0.0163(14) 0.0065(14) C7 0.0619(18) 0.0693(19) 0.0540(19) -0.0115(16) -0.0187(15) 0.0170(15) C8 0.0594(17) 0.0537(16) 0.0430(16) 0.0027(13) -0.0010(13) 0.0076(13) C9 0.0399(13) 0.0476(14) 0.0369(15) -0.0038(12) 0.0036(11) 0.0003(11) C4 0.0375(12) 0.0440(13) 0.0385(14) -0.0068(11) 0.0019(10) -0.0005(10) C10 0.0515(16) 0.0607(17) 0.0415(16) 0.0078(13) 0.0013(12) -0.0144(12) B3 0.0374(15) 0.0423(16) 0.0502(19) 0.0024(14) 0.0012(13) 0.0028(12) B4 0.0428(16) 0.0537(18) 0.0417(18) -0.0010(15) 0.0039(13) -0.0006(13) B5 0.0491(17) 0.0466(17) 0.0497(19) 0.0083(15) -0.0064(14) 0.0028(13) B6 0.0406(16) 0.0446(17) 0.055(2) -0.0023(15) 0.0095(14) 0.0047(13) B7 0.0494(17) 0.0379(16) 0.056(2) -0.0014(15) -0.0028(14) -0.0052(13) B8 0.0555(19) 0.0518(19) 0.050(2) -0.0081(15) -0.0011(15) 0.0005(14) B9 0.0539(19) 0.066(2) 0.046(2) 0.0030(17) -0.0101(15) 0.0018(15) B10 0.0367(16) 0.065(2) 0.070(2) 0.0072(18) -0.0077(15) 0.0067(14) B11 0.0343(15) 0.0537(18) 0.060(2) -0.0004(16) 0.0007(14) -0.0110(13) B12 0.0520(19) 0.059(2) 0.061(2) -0.0064(17) -0.0114(16) -0.0101(15) _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 C1 C3 1.519(3) . ? C1 C2 1.646(3) . ? C1 B4 1.696(4) . ? C1 B5 1.698(3) . ? C1 B6 1.714(3) . ? C1 B3 1.720(3) . ? C2 C10 1.509(3) . ? C2 B7 1.708(4) . ? C2 B11 1.708(3) . ? C2 B6 1.721(4) . ? C2 B3 1.721(4) . ? C3 C4 1.504(3) . ? C5 C6 1.373(3) . ? C5 C4 1.394(3) . ? C6 C7 1.372(4) . ? C7 C8 1.378(3) . ? C8 C9 1.390(3) . ? C9 C4 1.387(3) . ? C9 C10 1.513(3) . ? B3 B8 1.742(4) . ? B3 B7 1.756(4) . ? B3 B4 1.760(4) . ? B4 B5 1.762(4) . ? B4 B9 1.768(4) . ? B4 B8 1.770(4) . ? B5 B6 1.751(4) . ? B5 B10 1.758(4) . ? B5 B9 1.765(4) . ? B6 B10 1.735(4) . ? B6 B11 1.760(4) . ? B7 B8 1.765(5) . ? B7 B12 1.766(4) . ? B7 B11 1.770(4) . ? B8 B9 1.785(4) . ? B8 B12 1.786(4) . ? B9 B12 1.770(5) . ? B9 B10 1.778(5) . ? B10 B11 1.764(5) . ? B10 B12 1.775(5) . ? B11 B12 1.760(5) . ? 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 C3 C1 C2 117.21(18) . . ? C3 C1 B4 121.79(19) . . ? C2 C1 B4 111.14(18) . . ? C3 C1 B5 121.6(2) . . ? C2 C1 B5 111.01(17) . . ? B4 C1 B5 62.56(16) . . ? C3 C1 B6 116.9(2) . . ? C2 C1 B6 61.59(14) . . ? B4 C1 B6 113.41(18) . . ? B5 C1 B6 61.76(16) . . ? C3 C1 B3 117.43(19) . . ? C2 C1 B3 61.46(14) . . ? B4 C1 B3 62.00(16) . . ? B5 C1 B3 113.46(19) . . ? B6 C1 B3 113.64(18) . . ? C10 C2 C1 117.64(18) . . ? C10 C2 B7 122.5(2) . . ? C1 C2 B7 110.41(18) . . ? C10 C2 B11 121.5(2) . . ? C1 C2 B11 110.45(18) . . ? B7 C2 B11 62.42(16) . . ? C10 C2 B6 116.7(2) . . ? C1 C2 B6 61.16(14) . . ? B7 C2 B6 113.00(19) . . ? B11 C2 B6 61.77(16) . . ? C10 C2 B3 118.12(19) . . ? C1 C2 B3 61.39(14) . . ? B7 C2 B3 61.63(16) . . ? B11 C2 B3 113.1(2) . . ? B6 C2 B3 113.24(19) . . ? C4 C3 C1 115.5(2) . . ? C6 C5 C4 121.4(3) . . ? C7 C6 C5 119.9(3) . . ? C6 C7 C8 119.4(3) . . ? C7 C8 C9 121.5(3) . . ? C4 C9 C8 119.1(2) . . ? C4 C9 C10 122.8(2) . . ? C8 C9 C10 118.2(2) . . ? C9 C4 C5 118.8(2) . . ? C9 C4 C3 123.7(2) . . ? C5 C4 C3 117.5(2) . . ? C2 C10 C9 115.63(19) . . ? C1 B3 C2 57.15(13) . . ? C1 B3 B8 105.6(2) . . ? C2 B3 B8 105.9(2) . . ? C1 B3 B7 104.79(19) . . ? C2 B3 B7 58.81(15) . . ? B8 B3 B7 60.59(17) . . ? C1 B3 B4 58.34(15) . . ? C2 B3 B4 104.75(19) . . ? B8 B3 B4 60.74(17) . . ? B7 B3 B4 108.5(2) . . ? C1 B4 B3 59.65(15) . . ? C1 B4 B5 58.78(15) . . ? B3 B4 B5 108.5(2) . . ? C1 B4 B9 105.2(2) . . ? B3 B4 B9 107.9(2) . . ? B5 B4 B9 59.98(17) . . ? C1 B4 B8 105.3(2) . . ? B3 B4 B8 59.13(17) . . ? B5 B4 B8 108.5(2) . . ? B9 B4 B8 60.59(17) . . ? C1 B5 B6 59.56(15) . . ? C1 B5 B10 105.3(2) . . ? B6 B5 B10 59.25(18) . . ? C1 B5 B4 58.67(15) . . ? B6 B5 B4 108.4(2) . . ? B10 B5 B4 108.6(2) . . ? C1 B5 B9 105.2(2) . . ? B6 B5 B9 108.0(2) . . ? B10 B5 B9 60.62(18) . . ? B4 B5 B9 60.17(17) . . ? C1 B6 C2 57.25(13) . . ? C1 B6 B10 105.6(2) . . ? C2 B6 B10 105.8(2) . . ? C1 B6 B5 58.68(15) . . ? C2 B6 B5 105.1(2) . . ? B10 B6 B5 60.57(17) . . ? C1 B6 B11 104.92(19) . . ? C2 B6 B11 58.76(15) . . ? B10 B6 B11 60.62(18) . . ? B5 B6 B11 108.6(2) . . ? C2 B7 B3 59.56(15) . . ? C2 B7 B8 105.5(2) . . ? B3 B7 B8 59.30(17) . . ? C2 B7 B12 105.0(2) . . ? B3 B7 B12 107.9(2) . . ? B8 B7 B12 60.78(18) . . ? C2 B7 B11 58.81(15) . . ? B3 B7 B11 108.4(2) . . ? B8 B7 B11 108.6(2) . . ? B12 B7 B11 59.71(18) . . ? B3 B8 B7 60.11(17) . . ? B3 B8 B4 60.13(17) . . ? B7 B8 B4 107.6(2) . . ? B3 B8 B9 107.9(2) . . ? B7 B8 B9 107.3(2) . . ? B4 B8 B9 59.65(17) . . ? B3 B8 B12 107.7(2) . . ? B7 B8 B12 59.65(18) . . ? B4 B8 B12 107.0(2) . . ? B9 B8 B12 59.42(18) . . ? B5 B9 B4 59.85(16) . . ? B5 B9 B12 107.6(2) . . ? B4 B9 B12 107.8(2) . . ? B5 B9 B10 59.50(18) . . ? B4 B9 B10 107.5(2) . . ? B12 B9 B10 60.03(19) . . ? B5 B9 B8 107.7(2) . . ? B4 B9 B8 59.76(17) . . ? B12 B9 B8 60.32(18) . . ? B10 B9 B8 108.2(2) . . ? B6 B10 B5 60.18(17) . . ? B6 B10 B11 60.40(17) . . ? B5 B10 B11 108.1(2) . . ? B6 B10 B12 108.1(2) . . ? B5 B10 B12 107.6(2) . . ? B11 B10 B12 59.66(19) . . ? B6 B10 B9 108.2(2) . . ? B5 B10 B9 59.88(18) . . ? B11 B10 B9 107.7(2) . . ? B12 B10 B9 59.75(19) . . ? C2 B11 B12 105.2(2) . . ? C2 B11 B6 59.48(14) . . ? B12 B11 B6 107.6(2) . . ? C2 B11 B10 105.11(19) . . ? B12 B11 B10 60.47(19) . . ? B6 B11 B10 58.98(18) . . ? C2 B11 B7 58.78(15) . . ? B12 B11 B7 60.03(18) . . ? B6 B11 B7 108.18(19) . . ? B10 B11 B7 108.3(2) . . ? B11 B12 B7 60.26(17) . . ? B11 B12 B9 108.2(2) . . ? B7 B12 B9 107.9(2) . . ? B11 B12 B10 59.87(18) . . ? B7 B12 B10 108.0(2) . . ? B9 B12 B10 60.22(18) . . ? B11 B12 B8 108.0(2) . . ? B7 B12 B8 59.57(17) . . ? B9 B12 B8 60.26(18) . . ? B10 B12 B8 108.3(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.185 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.041 #===END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 B10' _chemical_formula_weight 322.44 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 6.6799(13) _cell_length_b 12.698(3) _cell_length_c 21.689(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1839.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.057 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1613 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1613 _reflns_number_gt 946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1287P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.035(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1613 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.2282 _refine_ls_wR_factor_gt 0.1935 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.080 _refine_ls_shift/su_mean 0.010 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 C3 C 0.8377(5) 0.1298(2) 0.11037(14) 0.0504(9) Uani 1 1 d . . . H3A H 0.8679 0.0572 0.1000 0.060 Uiso 1 1 calc R . . H3B H 0.9583 0.1601 0.1279 0.060 Uiso 1 1 calc R . . C1 C 0.7922(4) 0.1882(2) 0.05059(12) 0.0432(8) Uani 1 1 d . . . C9 C 0.6758(5) 0.2065(2) 0.20579(12) 0.0471(8) Uani 1 1 d . . . C4 C 0.6790(5) 0.1293(2) 0.15981(14) 0.0469(8) Uani 1 1 d . . . C5 C 0.5347(5) 0.0499(3) 0.16118(17) 0.0588(10) Uani 1 1 d . . . H5A H 0.5333 -0.0008 0.1302 0.071 Uiso 1 1 calc R . . C8 C 0.5339(5) 0.1995(3) 0.25224(16) 0.0597(10) Uani 1 1 d . . . H8A H 0.5332 0.2501 0.2832 0.072 Uiso 1 1 calc R . . C6 C 0.3940(6) 0.0451(3) 0.20773(17) 0.0698(11) Uani 1 1 d . . . H6A H 0.2993 -0.0086 0.2080 0.084 Uiso 1 1 calc R . . C7 C 0.3941(6) 0.1200(3) 0.25379(19) 0.0719(11) Uani 1 1 d . . . H7A H 0.3007 0.1167 0.2855 0.086 Uiso 1 1 calc R . . B3 B 0.5467(5) 0.2108(3) 0.02932(17) 0.0449(9) Uani 1 1 d . . . H3 H 0.4159 0.1858 0.0564 0.054 Uiso 1 1 calc R . . B4 B 0.6981(5) 0.1205(3) -0.01107(16) 0.0488(10) Uani 1 1 d . . . H4 H 0.6650 0.0356 -0.0105 0.059 Uiso 1 1 calc R . . B5 B 0.9476(6) 0.1681(3) -0.01077(17) 0.0509(10) Uani 1 1 d . . . H5 H 1.0762 0.1140 -0.0098 0.061 Uiso 1 1 calc R . . B11 B 0.9531(6) 0.2895(3) -0.05201(18) 0.0564(11) Uani 1 1 d . . . H11 H 1.0845 0.3152 -0.0786 0.068 Uiso 1 1 calc R . . B10 B 0.7968(6) 0.1837(3) -0.07760(18) 0.0584(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C3 0.0561(19) 0.0360(17) 0.0591(19) 0.0003(13) -0.0011(16) 0.0078(15) C1 0.0438(18) 0.0334(17) 0.0522(18) -0.0021(12) 0.0012(15) 0.0044(14) C9 0.0514(19) 0.0421(16) 0.0476(17) 0.0059(13) -0.0012(15) 0.0022(15) C4 0.0529(19) 0.0367(16) 0.0510(17) 0.0059(13) -0.0049(16) 0.0047(14) C5 0.073(2) 0.0401(18) 0.063(2) 0.0071(15) -0.011(2) -0.0061(17) C8 0.065(2) 0.054(2) 0.060(2) 0.0004(16) 0.0084(19) 0.0048(18) C6 0.074(2) 0.055(2) 0.081(3) 0.0166(19) 0.004(2) -0.018(2) C7 0.068(2) 0.070(3) 0.078(3) 0.014(2) 0.018(2) -0.008(2) B3 0.040(2) 0.0377(18) 0.057(2) 0.0041(16) -0.0020(16) -0.0018(16) B4 0.048(2) 0.0396(19) 0.059(2) -0.0090(16) -0.0001(19) -0.0066(16) B5 0.049(2) 0.042(2) 0.061(2) -0.0046(17) 0.0079(19) 0.0023(17) B11 0.053(2) 0.053(2) 0.064(2) 0.0012(17) 0.0098(19) -0.002(2) B10 0.059(3) 0.053(2) 0.063(2) 0.0001(18) -0.003(2) -0.0007(19) _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 C3 C4 1.508(4) . ? C3 C1 1.524(4) . ? C1 C1 1.667(5) 2_655 ? C1 B4 1.710(4) . ? C1 B5 1.707(5) . ? C1 B3 1.727(5) . ? C1 B3 1.736(4) 2_655 ? C9 C8 1.386(4) . ? C9 C4 1.398(4) . ? C9 C9 1.484(6) 2_655 ? C4 C5 1.395(4) . ? C5 C6 1.381(5) . ? C8 C7 1.377(5) . ? C6 C7 1.379(5) . ? B3 C1 1.736(4) 2_655 ? B3 B11 1.764(5) 2_655 ? B3 B4 1.762(5) . ? B3 B5 1.767(5) 2_655 ? B4 B11 1.765(5) 2_655 ? B4 B10 1.778(5) . ? B4 B5 1.773(5) . ? B5 B10 1.776(6) . ? B5 B3 1.767(5) 2_655 ? B5 B11 1.783(6) . ? B11 B3 1.764(5) 2_655 ? B11 B4 1.765(5) 2_655 ? B11 B10 1.790(6) . ? B11 B10 1.792(6) 2_655 ? B10 B11 1.792(6) 2_655 ? B10 B10 1.796(8) 2_655 ? 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 C4 C3 C1 117.8(3) . . ? C3 C1 C1 121.68(15) . 2_655 ? C3 C1 B4 119.6(2) . . ? C1 C1 B4 110.4(2) 2_655 . ? C3 C1 B5 118.0(2) . . ? C1 C1 B5 110.3(2) 2_655 . ? B4 C1 B5 62.50(19) . . ? C3 C1 B3 119.8(2) . . ? C1 C1 B3 61.5(2) 2_655 . ? B4 C1 B3 61.7(2) . . ? B5 C1 B3 113.2(2) . . ? C3 C1 B3 117.5(3) . 2_655 ? C1 C1 B3 61.0(2) 2_655 2_655 ? B4 C1 B3 113.0(2) . 2_655 ? B5 C1 B3 61.75(19) . 2_655 ? B3 C1 B3 113.2(2) . 2_655 ? C8 C9 C4 118.9(3) . . ? C8 C9 C9 120.3(2) . 2_655 ? C4 C9 C9 120.8(3) . 2_655 ? C5 C4 C9 118.8(3) . . ? C5 C4 C3 120.3(3) . . ? C9 C4 C3 121.0(3) . . ? C6 C5 C4 121.2(3) . . ? C7 C8 C9 121.9(3) . . ? C5 C6 C7 119.9(3) . . ? C8 C7 C6 119.2(3) . . ? C1 B3 C1 57.55(19) . 2_655 ? C1 B3 B11 105.4(3) . 2_655 ? C1 B3 B11 105.5(2) 2_655 2_655 ? C1 B3 B4 58.66(18) . . ? C1 B3 B4 104.9(2) 2_655 . ? B11 B3 B4 60.1(2) 2_655 . ? C1 B3 B5 104.8(2) . 2_655 ? C1 B3 B5 58.32(19) 2_655 2_655 ? B11 B3 B5 60.7(2) 2_655 2_655 ? B4 B3 B5 108.0(3) . 2_655 ? C1 B4 B11 106.2(2) . 2_655 ? C1 B4 B3 59.65(19) . . ? B11 B4 B3 60.0(2) 2_655 . ? C1 B4 B10 105.7(2) . . ? B11 B4 B10 60.8(2) 2_655 . ? B3 B4 B10 108.8(3) . . ? C1 B4 B5 58.67(19) . . ? B11 B4 B5 108.6(3) 2_655 . ? B3 B4 B5 108.4(2) . . ? B10 B4 B5 60.0(2) . . ? C1 B5 B10 106.0(3) . . ? C1 B5 B4 58.83(19) . . ? B10 B5 B4 60.1(2) . . ? C1 B5 B3 59.93(19) . 2_655 ? B10 B5 B3 108.5(3) . 2_655 ? B4 B5 B3 108.6(3) . 2_655 ? C1 B5 B11 105.9(3) . . ? B10 B5 B11 60.4(2) . . ? B4 B5 B11 108.2(3) . . ? B3 B5 B11 59.6(2) 2_655 . ? B3 B11 B4 59.9(2) 2_655 2_655 ? B3 B11 B5 59.7(2) 2_655 . ? B4 B11 B5 107.2(3) 2_655 . ? B3 B11 B10 108.0(3) 2_655 . ? B4 B11 B10 108.0(3) 2_655 . ? B5 B11 B10 59.6(2) . . ? B3 B11 B10 108.1(3) 2_655 2_655 ? B4 B11 B10 60.0(2) 2_655 2_655 ? B5 B11 B10 107.5(3) . 2_655 ? B10 B11 B10 60.2(3) . 2_655 ? B5 B10 B4 59.8(2) . . ? B5 B10 B11 60.0(2) . . ? B4 B10 B11 107.7(3) . . ? B5 B10 B11 107.2(3) . 2_655 ? B4 B10 B11 59.2(2) . 2_655 ? B11 B10 B11 107.8(3) . 2_655 ? B5 B10 B10 107.6(2) . 2_655 ? B4 B10 B10 107.1(2) . 2_655 ? B11 B10 B10 60.0(3) . 2_655 ? B11 B10 B10 59.8(3) 2_655 2_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.607 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.057 #===END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H42 B10 Na2 O3' _chemical_formula_weight 508.64 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P(-1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7671(17) _cell_length_b 11.7823(16) _cell_length_c 12.4196(19) _cell_angle_alpha 103.805(3) _cell_angle_beta 90.036(3) _cell_angle_gamma 116.463(3) _cell_volume 1485.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.47 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _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 'Bruker Smart CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8390 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5207 _reflns_number_gt 2446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART CCD' _computing_cell_refinement 'Bruker SMART CCD' _computing_data_reduction 'Bruker SMART CCD' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.1103P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5207 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1386 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.2102 _refine_ls_wR_factor_gt 0.1677 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.005 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 Na2 Na 0.91812(13) 0.48688(14) 0.14323(12) 0.0626(5) Uani 1 1 d . . . Na1 Na 0.45631(12) 0.33134(13) -0.02651(13) 0.0617(5) Uani 1 1 d . . . C1 C 0.5299(3) 0.3923(3) -0.2396(3) 0.0476(9) Uani 1 1 d . . . C2 C 0.5321(3) 0.2711(3) -0.2385(3) 0.0471(9) Uani 1 1 d . . . C3 C 0.4243(4) 0.3788(5) -0.3203(4) 0.0596(11) Uani 1 1 d . . . H3B H 0.435(3) 0.457(3) -0.330(3) 0.057(11) Uiso 1 1 d . . . H3A H 0.347(4) 0.353(3) -0.286(3) 0.063(11) Uiso 1 1 d . . . C4 C 0.4300(4) 0.1461(4) -0.3170(3) 0.0582(10) Uani 1 1 d . . . H4B H 0.459(4) 0.077(4) -0.332(3) 0.087(14) Uiso 1 1 d . . . H4A H 0.353(4) 0.121(3) -0.288(3) 0.070(12) Uiso 1 1 d . . . C11 C 0.3973(3) 0.1608(4) -0.4282(3) 0.0588(10) Uani 1 1 d . . . C12 C 0.3705(4) 0.0654(5) -0.5265(4) 0.0754(12) Uani 1 1 d . . . H12A H 0.375(3) -0.020(3) -0.528(3) 0.064(11) Uiso 1 1 d . . . C13 C 0.3386(5) 0.0823(8) -0.6272(4) 0.1007(19) Uani 1 1 d . . . H13A H 0.313(4) 0.015(4) -0.686(4) 0.082(15) Uiso 1 1 d . . . C14 C 0.3370(5) 0.1993(7) -0.6270(5) 0.0966(18) Uani 1 1 d . . . H14A H 0.312(4) 0.204(4) -0.690(4) 0.100(17) Uiso 1 1 d . . . C15 C 0.3647(5) 0.2944(6) -0.5307(4) 0.0796(14) Uani 1 1 d . . . H15A H 0.366(4) 0.365(4) -0.529(4) 0.075(16) Uiso 1 1 d . . . C16 C 0.3948(3) 0.2780(4) -0.4295(3) 0.0618(11) Uani 1 1 d . . . C21 C 0.6974(5) 0.3327(6) 0.2893(5) 0.1144(18) Uani 1 1 d . . . H21A H 0.6903 0.4135 0.3011 0.137 Uiso 1 1 calc R . . H21B H 0.6310 0.2654 0.2307 0.137 Uiso 1 1 calc R . . C22 C 0.6861(8) 0.2938(12) 0.3865(7) 0.223(5) Uani 1 1 d . . . H22A H 0.6045 0.2170 0.3805 0.268 Uiso 1 1 calc R . . H22B H 0.6904 0.3639 0.4489 0.268 Uiso 1 1 calc R . . C23 C 0.7892(8) 0.2632(11) 0.4046(8) 0.222(5) Uani 1 1 d . . . H23A H 0.8339 0.3097 0.4795 0.267 Uiso 1 1 calc R . . H23B H 0.7563 0.1695 0.3955 0.267 Uiso 1 1 calc R . . C24 C 0.8680(6) 0.3012(7) 0.3290(6) 0.138(3) Uani 1 1 d . . . H24A H 0.8770 0.2268 0.2839 0.166 Uiso 1 1 calc R . . H24B H 0.9519 0.3678 0.3664 0.166 Uiso 1 1 calc R . . C31 C 0.9480(6) 0.7866(5) 0.2342(5) 0.1086(18) Uani 1 1 d . . . H31A H 0.8796 0.7727 0.1810 0.130 Uiso 1 1 calc R . . H31B H 1.0265 0.8139 0.1997 0.130 Uiso 1 1 calc R . . C32 C 0.9627(7) 0.8878(6) 0.3352(7) 0.144(3) Uani 1 1 d . . . H32A H 0.8851 0.8974 0.3424 0.172 Uiso 1 1 calc R . . H32B H 1.0333 0.9720 0.3349 0.172 Uiso 1 1 calc R . . C33 C 0.9893(7) 0.8377(7) 0.4282(6) 0.147(3) Uani 1 1 d . . . H33A H 1.0777 0.8901 0.4618 0.176 Uiso 1 1 calc R . . H33B H 0.9339 0.8400 0.4856 0.176 Uiso 1 1 calc R . . C34 C 0.9632(8) 0.7032(7) 0.3745(5) 0.144(3) Uani 1 1 d . . . H34A H 1.0408 0.6945 0.3819 0.173 Uiso 1 1 calc R . . H34B H 0.8997 0.6439 0.4112 0.173 Uiso 1 1 calc R . . C41 C 0.1818(5) 0.0582(5) -0.0524(5) 0.1104(19) Uani 1 1 d . . . H41A H 0.1470 0.0241 -0.1307 0.132 Uiso 1 1 calc R . . H41B H 0.1524 0.1213 -0.0165 0.132 Uiso 1 1 calc R . . C42 C 0.1426(6) -0.0465(7) 0.0007(7) 0.160(3) Uani 1 1 d . . . H42A H 0.1190 -0.0204 0.0739 0.192 Uiso 1 1 calc R . . H42B H 0.0691 -0.1239 -0.0437 0.192 Uiso 1 1 calc R . . C43 C 0.2450(7) -0.0740(7) 0.0108(7) 0.157(3) Uani 1 1 d . . . H43A H 0.2316 -0.1529 -0.0459 0.188 Uiso 1 1 calc R . . H43B H 0.2548 -0.0871 0.0838 0.188 Uiso 1 1 calc R . . C44 C 0.3567(5) 0.0383(6) -0.0039(7) 0.145(3) Uani 1 1 d . . . H44A H 0.4119 0.0866 0.0664 0.174 Uiso 1 1 calc R . . H44B H 0.4043 0.0099 -0.0581 0.174 Uiso 1 1 calc R . . O1 O 0.3162(3) 0.1177(3) -0.0409(3) 0.0934(11) Uani 1 1 d . . . O2 O 0.8194(3) 0.3524(3) 0.2598(3) 0.1024(11) Uani 1 1 d . . . O3 O 0.9192(3) 0.6694(3) 0.2636(3) 0.0868(9) Uani 1 1 d . . . B3 B 0.6215(4) 0.2569(4) -0.1566(3) 0.0487(10) Uani 1 1 d . . . B4 B 0.7035(4) 0.3931(4) -0.0343(4) 0.0503(11) Uani 1 1 d . . . H4 H 0.714(3) 0.371(3) 0.046(3) 0.070(10) Uiso 1 1 d . . . B5 B 0.6973(4) 0.5350(4) -0.0344(4) 0.0514(11) Uani 1 1 d . . . H5 H 0.701(3) 0.609(3) 0.048(3) 0.053(9) Uiso 1 1 d . . . B6 B 0.6112(4) 0.5282(4) -0.1583(4) 0.0516(11) Uani 1 1 d . . . H6 H 0.575(3) 0.594(3) -0.164(2) 0.053(9) Uiso 1 1 d . . . B7 B 0.6939(4) 0.3203(4) -0.2737(4) 0.0522(11) Uani 1 1 d . . . H7 H 0.702(3) 0.265(3) -0.351(3) 0.051(9) Uiso 1 1 d . . . B8 B 0.7878(4) 0.3563(4) -0.1422(4) 0.0512(11) Uani 1 1 d . . . H8 H 0.849(3) 0.304(3) -0.143(3) 0.057(9) Uiso 1 1 d . . . B9 B 0.8373(4) 0.5208(4) -0.0693(4) 0.0520(11) Uani 1 1 d . . . H9 H 0.936(3) 0.585(3) -0.015(3) 0.057(9) Uiso 1 1 d . . . B10 B 0.7798(4) 0.5976(4) -0.1436(4) 0.0538(11) Uani 1 1 d . . . H10 H 0.841(3) 0.704(3) -0.142(2) 0.045(8) Uiso 1 1 d . . . B11 B 0.6912(4) 0.4837(4) -0.2715(4) 0.0539(11) Uani 1 1 d . . . H11 H 0.682(3) 0.500(3) -0.340(3) 0.055(10) Uiso 1 1 d . . . B12 B 0.8206(4) 0.4746(4) -0.2194(4) 0.0530(11) Uani 1 1 d . . . H12 H 0.900(3) 0.502(3) -0.266(3) 0.068(10) Uiso 1 1 d . . . H3 H 0.601(3) 0.153(3) -0.167(2) 0.050(8) 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 Na2 0.0568(9) 0.0792(10) 0.0638(10) 0.0345(8) 0.0169(7) 0.0337(8) Na1 0.0492(9) 0.0548(9) 0.0836(11) 0.0239(8) 0.0258(7) 0.0233(7) C1 0.043(2) 0.062(2) 0.052(2) 0.0277(18) 0.0143(16) 0.0296(18) C2 0.0438(19) 0.054(2) 0.049(2) 0.0198(17) 0.0143(16) 0.0247(17) C3 0.054(3) 0.075(3) 0.063(3) 0.027(2) 0.005(2) 0.036(2) C4 0.050(2) 0.060(3) 0.062(3) 0.021(2) 0.009(2) 0.021(2) C11 0.043(2) 0.072(3) 0.053(2) 0.016(2) 0.0021(17) 0.019(2) C12 0.063(3) 0.077(3) 0.069(3) 0.015(3) 0.001(2) 0.021(2) C13 0.091(4) 0.121(5) 0.058(4) 0.006(4) -0.009(3) 0.029(4) C14 0.090(4) 0.134(5) 0.059(4) 0.034(4) -0.002(3) 0.042(4) C15 0.071(3) 0.099(4) 0.072(4) 0.036(3) -0.005(2) 0.036(3) C16 0.041(2) 0.082(3) 0.066(3) 0.029(2) 0.0030(18) 0.027(2) C21 0.102(4) 0.170(5) 0.109(4) 0.075(4) 0.051(3) 0.076(4) C22 0.142(7) 0.438(16) 0.173(8) 0.195(10) 0.096(6) 0.149(9) C23 0.139(7) 0.390(14) 0.231(10) 0.242(10) 0.075(6) 0.123(8) C24 0.114(5) 0.197(6) 0.176(6) 0.152(6) 0.061(4) 0.083(5) C31 0.132(5) 0.086(4) 0.117(5) 0.026(4) 0.023(4) 0.058(4) C32 0.131(6) 0.106(5) 0.182(8) 0.006(5) 0.003(5) 0.061(4) C33 0.139(6) 0.159(7) 0.109(5) -0.004(5) 0.005(4) 0.059(5) C34 0.236(8) 0.139(6) 0.081(4) -0.005(4) -0.010(5) 0.125(6) C41 0.070(3) 0.090(4) 0.180(6) 0.056(4) 0.015(3) 0.035(3) C42 0.080(4) 0.165(6) 0.270(9) 0.155(6) 0.041(5) 0.038(4) C43 0.132(6) 0.139(5) 0.245(9) 0.129(6) 0.024(5) 0.063(5) C44 0.083(4) 0.138(5) 0.265(9) 0.123(6) 0.039(5) 0.060(4) O1 0.065(2) 0.0712(19) 0.164(3) 0.059(2) 0.037(2) 0.0350(17) O2 0.077(2) 0.152(3) 0.126(3) 0.102(2) 0.0460(19) 0.062(2) O3 0.095(2) 0.084(2) 0.080(2) 0.0166(18) 0.0108(18) 0.0432(18) B3 0.051(2) 0.054(3) 0.054(3) 0.025(2) 0.016(2) 0.030(2) B4 0.043(2) 0.068(3) 0.050(3) 0.029(2) 0.0118(19) 0.028(2) B5 0.044(2) 0.061(3) 0.055(3) 0.018(2) 0.010(2) 0.027(2) B6 0.054(3) 0.056(2) 0.059(3) 0.025(2) 0.014(2) 0.032(2) B7 0.051(2) 0.065(3) 0.050(3) 0.019(2) 0.019(2) 0.033(2) B8 0.043(2) 0.064(3) 0.060(3) 0.028(2) 0.017(2) 0.030(2) B9 0.041(2) 0.061(3) 0.057(3) 0.023(2) 0.008(2) 0.022(2) B10 0.048(2) 0.059(3) 0.061(3) 0.027(2) 0.014(2) 0.025(2) B11 0.053(3) 0.067(3) 0.056(3) 0.036(2) 0.018(2) 0.030(2) B12 0.047(2) 0.064(3) 0.060(3) 0.030(2) 0.020(2) 0.028(2) _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 Na2 O3 2.303(3) . ? Na2 O2 2.327(3) . ? Na2 B4 2.967(4) . ? Na2 B9 2.978(4) . ? Na2 B12 3.017(4) 2_765 ? Na2 B9 3.054(4) 2_765 ? Na2 B8 3.114(4) 2_765 ? Na2 Na2 4.058(3) 2_765 ? Na1 O1 2.274(3) . ? Na1 B4 2.673(4) . ? Na1 B5 2.803(4) . ? Na1 C2 2.812(4) . ? Na1 B3 2.829(4) . ? Na1 B6 2.828(5) 2_665 ? Na1 B5 2.879(4) 2_665 ? Na1 C1 2.937(4) . ? Na1 B6 3.071(4) . ? Na1 Na1 3.521(3) 2_665 ? C1 C2 1.444(4) . ? C1 C3 1.523(5) . ? C1 B6 1.536(5) . ? C1 B11 1.818(5) . ? C2 C4 1.516(5) . ? C2 B3 1.551(5) . ? C2 B7 1.813(5) . ? C3 C16 1.495(6) . ? C4 C11 1.503(5) . ? C11 C12 1.372(6) . ? C11 C16 1.397(5) . ? C12 C13 1.389(7) . ? C13 C14 1.386(8) . ? C14 C15 1.352(7) . ? C15 C16 1.385(6) . ? C21 C22 1.376(7) . ? C21 O2 1.412(6) . ? C22 C23 1.443(9) . ? C23 C24 1.332(8) . ? C24 O2 1.408(5) . ? C31 O3 1.407(5) . ? C31 C32 1.459(7) . ? C32 C33 1.507(8) . ? C33 C34 1.453(8) . ? C34 O3 1.370(6) . ? C41 O1 1.406(5) . ? C41 C42 1.432(7) . ? C42 C43 1.394(7) . ? C43 C44 1.441(8) . ? C44 O1 1.384(5) . ? B3 B8 1.758(6) . ? B3 B4 1.807(6) . ? B3 B7 1.830(6) . ? B4 B5 1.706(6) . ? B4 B8 1.754(6) . ? B4 B9 1.770(6) . ? B5 B9 1.773(6) . ? B5 B10 1.779(6) . ? B5 B6 1.808(6) . ? B5 Na1 2.879(4) 2_665 ? B6 B10 1.767(6) . ? B6 B11 1.797(6) . ? B6 Na1 2.828(5) 2_665 ? B7 B12 1.727(6) . ? B7 B8 1.822(6) . ? B7 B11 1.934(6) . ? B8 B9 1.752(6) . ? B8 B12 1.781(6) . ? B8 Na2 3.114(4) 2_765 ? B9 B10 1.753(6) . ? B9 B12 1.797(6) . ? B9 Na2 3.054(4) 2_765 ? B10 B11 1.774(6) . ? B10 B12 1.786(6) . ? B11 B12 1.710(6) . ? B12 Na2 3.017(4) 2_765 ? 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 O3 Na2 O2 93.35(13) . . ? O3 Na2 B4 104.84(12) . . ? O2 Na2 B4 100.99(12) . . ? O3 Na2 B9 98.19(12) . . ? O2 Na2 B9 135.63(13) . . ? B4 Na2 B9 34.64(11) . . ? O3 Na2 B12 99.69(13) . 2_765 ? O2 Na2 B12 92.56(12) . 2_765 ? B4 Na2 B12 151.07(13) . 2_765 ? B9 Na2 B12 126.89(12) . 2_765 ? O3 Na2 B9 122.58(12) . 2_765 ? O2 Na2 B9 113.75(12) . 2_765 ? B4 Na2 B9 117.01(12) . 2_765 ? B9 Na2 B9 95.45(11) . 2_765 ? B12 Na2 B9 34.44(12) 2_765 2_765 ? O3 Na2 B8 89.87(12) . 2_765 ? O2 Na2 B8 125.54(12) . 2_765 ? B4 Na2 B8 130.44(12) . 2_765 ? B9 Na2 B8 97.30(11) . 2_765 ? B12 Na2 B8 33.73(11) 2_765 2_765 ? B9 Na2 B8 32.99(11) 2_765 2_765 ? O3 Na2 Na2 120.65(11) . 2_765 ? O2 Na2 Na2 145.86(12) . 2_765 ? B4 Na2 Na2 74.81(9) . 2_765 ? B9 Na2 Na2 48.52(9) . 2_765 ? B12 Na2 Na2 79.62(10) 2_765 2_765 ? B9 Na2 Na2 46.93(8) 2_765 2_765 ? B8 Na2 Na2 57.45(9) 2_765 2_765 ? O1 Na1 B4 117.83(13) . . ? O1 Na1 B5 153.60(13) . . ? B4 Na1 B5 36.21(12) . . ? O1 Na1 C2 93.11(12) . . ? B4 Na1 C2 63.03(12) . . ? B5 Na1 C2 71.33(12) . . ? O1 Na1 B3 91.61(12) . . ? B4 Na1 B3 38.22(13) . . ? B5 Na1 B3 63.79(13) . . ? C2 Na1 B3 31.92(10) . . ? O1 Na1 B6 103.41(13) . 2_665 ? B4 Na1 B6 118.26(14) . 2_665 ? B5 Na1 B6 97.44(13) . 2_665 ? C2 Na1 B6 158.70(12) . 2_665 ? B3 Na1 B6 156.39(13) . 2_665 ? O1 Na1 B5 102.96(12) . 2_665 ? B4 Na1 B5 138.18(13) . 2_665 ? B5 Na1 B5 103.44(11) . 2_665 ? C2 Na1 B5 126.42(12) . 2_665 ? B3 Na1 B5 155.71(13) . 2_665 ? B6 Na1 B5 36.92(12) 2_665 2_665 ? O1 Na1 C1 115.02(13) . . ? B4 Na1 C1 70.92(11) . . ? B5 Na1 C1 59.79(11) . . ? C2 Na1 C1 28.98(9) . . ? B3 Na1 C1 54.95(10) . . ? B6 Na1 C1 129.72(11) 2_665 . ? B5 Na1 C1 100.93(11) 2_665 . ? O1 Na1 B6 144.53(14) . . ? B4 Na1 B6 61.71(12) . . ? B5 Na1 B6 35.48(12) . . ? C2 Na1 B6 53.57(11) . . ? B3 Na1 B6 66.88(12) . . ? B6 Na1 B6 106.84(11) 2_665 . ? B5 Na1 B6 90.63(12) 2_665 . ? C1 Na1 B6 29.52(10) . . ? O1 Na1 Na1 153.71(11) . 2_665 ? B4 Na1 Na1 88.10(10) . 2_665 ? B5 Na1 Na1 52.68(9) . 2_665 ? C2 Na1 Na1 103.33(9) . 2_665 ? B3 Na1 Na1 113.18(10) . 2_665 ? B6 Na1 Na1 56.59(9) 2_665 2_665 ? B5 Na1 Na1 50.76(9) 2_665 2_665 ? C1 Na1 Na1 75.79(8) . 2_665 ? B6 Na1 Na1 50.25(9) . 2_665 ? C2 C1 C3 115.6(3) . . ? C2 C1 B6 126.5(3) . . ? C3 C1 B6 117.4(3) . . ? C2 C1 B11 99.6(3) . . ? C3 C1 B11 114.8(3) . . ? B6 C1 B11 64.2(3) . . ? C2 C1 Na1 70.70(18) . . ? C3 C1 Na1 116.4(2) . . ? B6 C1 Na1 80.0(2) . . ? B11 C1 Na1 126.8(2) . . ? C1 C2 C4 116.7(3) . . ? C1 C2 B3 125.4(3) . . ? C4 C2 B3 117.6(3) . . ? C1 C2 B7 95.9(3) . . ? C4 C2 B7 115.3(3) . . ? B3 C2 B7 65.4(2) . . ? C1 C2 Na1 80.32(19) . . ? C4 C2 Na1 112.8(2) . . ? B3 C2 Na1 74.6(2) . . ? B7 C2 Na1 127.5(2) . . ? C16 C3 C1 114.9(3) . . ? C11 C4 C2 114.6(3) . . ? C12 C11 C16 119.6(4) . . ? C12 C11 C4 123.0(4) . . ? C16 C11 C4 117.4(4) . . ? C11 C12 C13 121.0(5) . . ? C14 C13 C12 118.6(6) . . ? C15 C14 C13 120.6(6) . . ? C14 C15 C16 121.3(6) . . ? C15 C16 C11 118.8(4) . . ? C15 C16 C3 123.6(4) . . ? C11 C16 C3 117.6(3) . . ? C22 C21 O2 106.1(5) . . ? C21 C22 C23 108.5(6) . . ? C24 C23 C22 106.8(6) . . ? C23 C24 O2 109.9(6) . . ? O3 C31 C32 108.5(5) . . ? C31 C32 C33 103.8(5) . . ? C34 C33 C32 104.6(5) . . ? O3 C34 C33 110.7(5) . . ? O1 C41 C42 106.0(4) . . ? C43 C42 C41 107.8(5) . . ? C42 C43 C44 106.1(5) . . ? O1 C44 C43 108.0(4) . . ? C44 O1 C41 108.8(4) . . ? C44 O1 Na1 120.0(3) . . ? C41 O1 Na1 128.5(3) . . ? C24 O2 C21 107.3(4) . . ? C24 O2 Na2 131.3(3) . . ? C21 O2 Na2 120.2(3) . . ? C34 O3 C31 107.4(4) . . ? C34 O3 Na2 119.9(3) . . ? C31 O3 Na2 123.5(3) . . ? C2 B3 B8 120.0(3) . . ? C2 B3 B4 117.2(3) . . ? B8 B3 B4 58.9(2) . . ? C2 B3 B7 64.2(2) . . ? B8 B3 B7 61.0(2) . . ? B4 B3 B7 104.6(3) . . ? C2 B3 Na1 73.45(19) . . ? B8 B3 Na1 123.3(2) . . ? B4 B3 Na1 66.22(18) . . ? B7 B3 Na1 125.7(2) . . ? B5 B4 B8 109.8(3) . . ? B5 B4 B9 61.3(2) . . ? B8 B4 B9 59.6(2) . . ? B5 B4 B3 115.7(3) . . ? B8 B4 B3 59.1(2) . . ? B9 B4 B3 110.5(3) . . ? B5 B4 Na1 76.05(19) . . ? B8 B4 Na1 132.5(2) . . ? B9 B4 Na1 135.4(2) . . ? B3 B4 Na1 75.56(18) . . ? B5 B4 Na2 102.1(2) . . ? B8 B4 Na2 93.8(2) . . ? B9 B4 Na2 73.02(19) . . ? B3 B4 Na2 138.7(2) . . ? Na1 B4 Na2 132.16(16) . . ? B4 B5 B9 61.1(2) . . ? B4 B5 B10 109.3(3) . . ? B9 B5 B10 59.1(2) . . ? B4 B5 B6 115.1(3) . . ? B9 B5 B6 109.6(3) . . ? B10 B5 B6 59.0(2) . . ? B4 B5 Na1 67.75(19) . . ? B9 B5 Na1 127.2(2) . . ? B10 B5 Na1 134.3(3) . . ? B6 B5 Na1 80.4(2) . . ? B4 B5 Na1 141.8(3) . 2_665 ? B9 B5 Na1 156.2(3) . 2_665 ? B10 B5 Na1 105.1(2) . 2_665 ? B6 B5 Na1 70.02(19) . 2_665 ? Na1 B5 Na1 76.56(11) . 2_665 ? C1 B6 B10 120.1(3) . . ? C1 B6 B11 65.5(2) . . ? B10 B6 B11 59.7(2) . . ? C1 B6 B5 117.6(3) . . ? B10 B6 B5 59.7(2) . . ? B11 B6 B5 104.8(3) . . ? C1 B6 Na1 130.0(3) . 2_665 ? B10 B6 Na1 107.5(2) . 2_665 ? B11 B6 Na1 163.9(3) . 2_665 ? B5 B6 Na1 73.1(2) . 2_665 ? C1 B6 Na1 70.43(19) . . ? B10 B6 Na1 120.1(2) . . ? B11 B6 Na1 120.9(2) . . ? B5 B6 Na1 64.17(18) . . ? Na1 B6 Na1 73.16(11) 2_665 . ? B12 B7 C2 124.3(3) . . ? B12 B7 B8 60.2(2) . . ? C2 B7 B8 104.2(3) . . ? B12 B7 B3 107.9(3) . . ? C2 B7 B3 50.39(19) . . ? B8 B7 B3 57.6(2) . . ? B12 B7 B11 55.4(2) . . ? C2 B7 B11 83.7(2) . . ? B8 B7 B11 104.3(3) . . ? B3 B7 B11 111.8(3) . . ? B9 B8 B4 60.6(2) . . ? B9 B8 B3 113.7(3) . . ? B4 B8 B3 61.9(2) . . ? B9 B8 B12 61.1(2) . . ? B4 B8 B12 106.1(3) . . ? B3 B8 B12 108.8(3) . . ? B9 B8 B7 108.8(3) . . ? B4 B8 B7 107.2(3) . . ? B3 B8 B7 61.5(2) . . ? B12 B8 B7 57.3(2) . . ? B9 B8 Na2 71.61(18) . 2_765 ? B4 B8 Na2 124.5(2) . 2_765 ? B3 B8 Na2 173.6(3) . 2_765 ? B12 B8 Na2 70.13(19) . 2_765 ? B7 B8 Na2 113.9(2) . 2_765 ? B8 B9 B10 111.1(3) . . ? B8 B9 B4 59.7(2) . . ? B10 B9 B4 107.6(3) . . ? B8 B9 B5 106.9(3) . . ? B10 B9 B5 60.6(2) . . ? B4 B9 B5 57.6(2) . . ? B8 B9 B12 60.2(2) . . ? B10 B9 B12 60.4(2) . . ? B4 B9 B12 104.8(3) . . ? B5 B9 B12 105.1(3) . . ? B8 B9 Na2 93.5(2) . . ? B10 B9 Na2 151.8(3) . . ? B4 B9 Na2 72.34(19) . . ? B5 B9 Na2 100.0(2) . . ? B12 B9 Na2 147.8(2) . . ? B8 B9 Na2 75.40(19) . 2_765 ? B10 B9 Na2 114.2(2) . 2_765 ? B4 B9 Na2 127.0(2) . 2_765 ? B5 B9 Na2 174.7(2) . 2_765 ? B12 B9 Na2 71.65(19) . 2_765 ? Na2 B9 Na2 84.55(11) . 2_765 ? B9 B10 B6 112.5(3) . . ? B9 B10 B11 109.1(3) . . ? B6 B10 B11 61.0(2) . . ? B9 B10 B5 60.3(2) . . ? B6 B10 B5 61.3(2) . . ? B11 B10 B5 107.0(3) . . ? B9 B10 B12 61.0(2) . . ? B6 B10 B12 107.5(3) . . ? B11 B10 B12 57.4(2) . . ? B5 B10 B12 105.4(3) . . ? B12 B11 B10 61.6(3) . . ? B12 B11 B6 109.5(3) . . ? B10 B11 B6 59.3(2) . . ? B12 B11 C1 123.2(3) . . ? B10 B11 C1 105.8(3) . . ? B6 B11 C1 50.3(2) . . ? B12 B11 B7 56.2(2) . . ? B10 B11 B7 106.6(3) . . ? B6 B11 B7 110.9(3) . . ? C1 B11 B7 80.7(2) . . ? B11 B12 B7 68.5(3) . . ? B11 B12 B8 116.3(3) . . ? B7 B12 B8 62.5(2) . . ? B11 B12 B10 60.9(2) . . ? B7 B12 B10 115.7(3) . . ? B8 B12 B10 108.3(3) . . ? B11 B12 B9 110.0(3) . . ? B7 B12 B9 111.1(3) . . ? B8 B12 B9 58.6(2) . . ? B10 B12 B9 58.6(2) . . ? B11 B12 Na2 167.4(3) . 2_765 ? B7 B12 Na2 122.1(2) . 2_765 ? B8 B12 Na2 76.14(19) . 2_765 ? B10 B12 Na2 114.7(2) . 2_765 ? B9 B12 Na2 73.92(19) . 2_765 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.244 _refine_diff_density_min -0.201 _refine_diff_density_rms 0.049 #===END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H114 B20 K4 N2 O18' _chemical_formula_weight 1524.13 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 '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 triclinic _symmetry_space_group_name_H-M P(-1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6454(7) _cell_length_b 12.2087(7) _cell_length_c 16.1936(10) _cell_angle_alpha 97.7730(10) _cell_angle_beta 103.4560(10) _cell_angle_gamma 104.2300(10) _cell_volume 2124.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.98 _exptl_crystal_size_mid 0.64 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.269 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.7634 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Smart CCD 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11476 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7439 _reflns_number_gt 3736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SHELXTL' _computing_cell_refinement 'Siemens SHELXTL' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens 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^)+(0.1155P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7439 _refine_ls_number_parameters 509 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1583 _refine_ls_goodness_of_fit_ref 0.858 _refine_ls_restrained_S_all 0.861 _refine_ls_shift/su_max 0.121 _refine_ls_shift/su_mean 0.008 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 K1 K 0.22008(8) 0.88439(7) 0.23368(5) 0.0652(3) Uani 1 1 d . . . K2 K 0.0000 1.0000 0.5000 0.0690(4) Uani 1 2 d S . . C1 C 0.1467(3) 1.1919(2) 0.43650(19) 0.0448(8) Uani 1 1 d . . . C2 C 0.0390(3) 1.2239(2) 0.44605(19) 0.0433(7) Uani 1 1 d . . . C11 C 0.2650(3) 1.2514(3) 0.5087(2) 0.0555(9) Uani 1 1 d . . . H11A H 0.2649 1.2122 0.5570 0.067 Uiso 1 1 calc R . . H11B H 0.3347 1.2437 0.4877 0.067 Uiso 1 1 calc R . . C12 C 0.2817(3) 1.3775(3) 0.5408(2) 0.0542(9) Uani 1 1 d . . . C13 C 0.3935(4) 1.4614(3) 0.5617(2) 0.0682(10) Uani 1 1 d . . . H13A H 0.4634 1.4411 0.5556 0.082 Uiso 1 1 calc R . . C14 C 0.4021(5) 1.5752(3) 0.5916(3) 0.0791(12) Uani 1 1 d . . . H14A H 0.4779 1.6311 0.6060 0.095 Uiso 1 1 calc R . . C15 C 0.3000(5) 1.6065(3) 0.6001(2) 0.0807(13) Uani 1 1 d . . . H15A H 0.3062 1.6835 0.6199 0.097 Uiso 1 1 calc R . . C16 C 0.1877(4) 1.5237(3) 0.5795(2) 0.0659(10) Uani 1 1 d . . . H16A H 0.1181 1.5450 0.5851 0.079 Uiso 1 1 calc R . . C17 C 0.1780(3) 1.4082(3) 0.5501(2) 0.0523(9) Uani 1 1 d . . . C18 C 0.0590(3) 1.3132(3) 0.5275(2) 0.0542(9) Uani 1 1 d . . . H18A H -0.0089 1.3470 0.5195 0.065 Uiso 1 1 calc R . . H18B H 0.0578 1.2743 0.5759 0.065 Uiso 1 1 calc R . . C31 C 0.4333(6) 1.0813(5) 0.1393(4) 0.127(2) Uani 1 1 d . . . H31A H 0.4370 1.1505 0.1156 0.153 Uiso 1 1 calc R . . H31B H 0.4822 1.0395 0.1143 0.153 Uiso 1 1 calc R . . C32 C 0.4852(6) 1.1134(4) 0.2323(4) 0.122(2) Uani 1 1 d . . . H32A H 0.5712 1.1576 0.2461 0.147 Uiso 1 1 calc R . . H32B H 0.4416 1.1614 0.2572 0.147 Uiso 1 1 calc R . . C33 C 0.5343(5) 1.0372(5) 0.3561(4) 0.1096(17) Uani 1 1 d . . . H33A H 0.4948 1.0830 0.3874 0.132 Uiso 1 1 calc R . . H33B H 0.6197 1.0814 0.3668 0.132 Uiso 1 1 calc R . . C34 C 0.5285(4) 0.9291(5) 0.3871(3) 0.1012(15) Uani 1 1 d . . . H34A H 0.5641 0.8815 0.3535 0.121 Uiso 1 1 calc R . . H34B H 0.5764 0.9459 0.4474 0.121 Uiso 1 1 calc R . . C35 C 0.3931(5) 0.7633(5) 0.4056(3) 0.1112(17) Uani 1 1 d . . . H35A H 0.4339 0.7765 0.4670 0.133 Uiso 1 1 calc R . . H35B H 0.4323 0.7169 0.3744 0.133 Uiso 1 1 calc R . . C36 C 0.2602(5) 0.6999(5) 0.3885(3) 0.1150(18) Uani 1 1 d . . . H36A H 0.2521 0.6299 0.4115 0.138 Uiso 1 1 calc R . . H36B H 0.2192 0.7477 0.4166 0.138 Uiso 1 1 calc R . . C37 C 0.0843(5) 0.6005(5) 0.2730(4) 0.1146(18) Uani 1 1 d . . . H37A H 0.0334 0.6383 0.2990 0.138 Uiso 1 1 calc R . . H37B H 0.0822 0.5292 0.2936 0.138 Uiso 1 1 calc R . . C38 C 0.0360(5) 0.5750(5) 0.1776(4) 0.1107(18) Uani 1 1 d . . . H38A H 0.0868 0.5366 0.1519 0.133 Uiso 1 1 calc R . . H38B H -0.0473 0.5234 0.1605 0.133 Uiso 1 1 calc R . . C39 C -0.0130(6) 0.6575(6) 0.0584(4) 0.130(2) Uani 1 1 d . . . H39A H -0.0972 0.6082 0.0420 0.156 Uiso 1 1 calc R . . H39B H 0.0343 0.6181 0.0296 0.156 Uiso 1 1 calc R . . C40 C -0.0114(5) 0.7631(7) 0.0297(4) 0.140(2) Uani 1 1 d . . . H40A H -0.0529 0.7469 -0.0318 0.168 Uiso 1 1 calc R . . H40B H -0.0550 0.8049 0.0604 0.168 Uiso 1 1 calc R . . C41 C 0.1210(6) 0.9295(6) 0.0162(3) 0.1232(19) Uani 1 1 d . . . H41A H 0.0792 0.9756 0.0450 0.148 Uiso 1 1 calc R . . H41B H 0.0797 0.9115 -0.0455 0.148 Uiso 1 1 calc R . . C42 C 0.2476(6) 0.9972(5) 0.0302(3) 0.1035(16) Uani 1 1 d . . . H42A H 0.2860 0.9577 -0.0067 0.124 Uiso 1 1 calc R . . H42B H 0.2490 1.0715 0.0147 0.124 Uiso 1 1 calc R . . O1 O 0.3134(3) 1.0138(3) 0.1166(2) 0.1006(10) Uani 1 1 d . . . O2 O 0.4753(3) 1.0137(3) 0.2674(2) 0.0992(10) Uani 1 1 d . . . O3 O 0.4056(3) 0.8684(3) 0.3794(2) 0.0911(9) Uani 1 1 d . . . O4 O 0.2056(3) 0.6722(3) 0.2972(2) 0.0938(9) Uani 1 1 d . . . O5 O 0.0357(3) 0.6753(3) 0.1474(2) 0.0985(10) Uani 1 1 d . . . O6 O 0.1107(4) 0.8307(4) 0.0453(2) 0.1123(11) Uani 1 1 d . . . B3 B -0.0950(4) 1.1657(3) 0.3915(3) 0.0516(10) Uani 1 1 d . . . H3 H -0.163(3) 1.198(3) 0.424(2) 0.062(9) Uiso 1 1 d . . . B4 B -0.1240(4) 1.0285(4) 0.3206(3) 0.0611(11) Uani 1 1 d . . . H4 H -0.213(4) 0.964(3) 0.321(2) 0.091(12) Uiso 1 1 d . . . B5 B 0.0030(4) 0.9904(4) 0.3077(3) 0.0605(11) Uani 1 1 d . . . H5 H 0.002(3) 0.901(3) 0.290(2) 0.069(10) Uiso 1 1 d . . . B6 B 0.1501(4) 1.0926(3) 0.3681(3) 0.0534(10) Uani 1 1 d . . . H6 H 0.240(3) 1.075(3) 0.378(2) 0.062(9) Uiso 1 1 d . . . B7 B -0.0006(4) 1.2695(4) 0.3454(3) 0.0582(11) Uani 1 1 d . . . H7 H 0.004(3) 1.359(3) 0.354(2) 0.062(9) Uiso 1 1 d . . . B8 B -0.1311(5) 1.1517(4) 0.2781(3) 0.0684(13) Uani 1 1 d . . . H8 H -0.205(3) 1.167(3) 0.249(2) 0.074(11) Uiso 1 1 d . . . B9 B -0.0761(5) 1.0488(4) 0.2265(3) 0.0724(13) Uani 1 1 d . . . H9 H -0.131(3) 1.000(3) 0.162(2) 0.073(10) Uiso 1 1 d . . . B10 B 0.0828(5) 1.0885(4) 0.2572(3) 0.0667(12) Uani 1 1 d . . . H10 H 0.134(4) 1.071(3) 0.211(3) 0.092(12) Uiso 1 1 d . . . B11 B 0.1427(4) 1.2273(4) 0.3326(3) 0.0588(11) Uani 1 1 d . . . H11 H 0.225(3) 1.293(3) 0.336(2) 0.066(10) Uiso 1 1 d . . . B12 B 0.0086(5) 1.1976(4) 0.2485(3) 0.0690(13) Uani 1 1 d . . . H12 H 0.021(3) 1.256(3) 0.202(2) 0.083(11) Uiso 1 1 d . . . K3 K 0.5000 0.5000 0.0000 0.0691(4) Uani 1 2 d S . . O7 O 0.5694(4) 0.2978(3) 0.0149(2) 0.1156(12) Uani 1 1 d . A . O8 O 0.6954(3) 0.5005(2) 0.14064(18) 0.0858(8) Uani 1 1 d . A . O9 O 0.5873(4) 0.6839(3) 0.1438(2) 0.1096(11) Uani 1 1 d . A . C53 C 0.5572(9) 0.2354(6) -0.0678(4) 0.190(4) Uani 1 1 d . . . H53A H 0.5765 0.1633 -0.0627 0.228 Uiso 1 1 calc R A . H53B H 0.6144 0.2796 -0.0944 0.228 Uiso 1 1 calc R . . C54 C 0.6877(5) 0.3157(4) 0.0733(3) 0.1055(16) Uani 1 1 d . . . H54A H 0.7514 0.3520 0.0480 0.127 Uiso 1 1 calc R A . H54B H 0.6990 0.2420 0.0833 0.127 Uiso 1 1 calc R . . C55 C 0.6991(4) 0.3904(4) 0.1570(3) 0.0946(14) Uani 1 1 d . A . H55A H 0.6317 0.3579 0.1803 0.114 Uiso 1 1 calc R . . H55B H 0.7762 0.3964 0.1987 0.114 Uiso 1 1 calc R . . C56 C 0.7118(5) 0.5805(4) 0.2172(3) 0.0914(14) Uani 1 1 d . . . H56A H 0.7905 0.5886 0.2578 0.110 Uiso 1 1 calc R A . H56B H 0.6472 0.5531 0.2443 0.110 Uiso 1 1 calc R . . C57 C 0.7077(5) 0.6951(4) 0.1949(3) 0.1110(18) Uani 1 1 d . A . H57A H 0.7284 0.7529 0.2475 0.133 Uiso 1 1 calc R . . H57B H 0.7671 0.7192 0.1629 0.133 Uiso 1 1 calc R . . C58 C 0.5709(8) 0.7884(5) 0.1226(5) 0.193(4) Uani 1 1 d . . . H58A H 0.6290 0.8194 0.0913 0.232 Uiso 1 1 calc R A . H58B H 0.5853 0.8447 0.1750 0.232 Uiso 1 1 calc R . . N1 N 0.3241(9) 0.3656(9) 0.0762(7) 0.116(3) Uiso 0.50 1 d P A 1 C51 C 0.3272(12) 0.3863(12) 0.1373(9) 0.113(4) Uiso 0.50 1 d P A 1 C52 C 0.3364(11) 0.4672(11) 0.2343(7) 0.110(3) Uiso 0.50 1 d P A 1 N1' N 0.3117(11) 0.4481(10) 0.0788(8) 0.146(4) Uiso 0.50 1 d PD A 2 C51' C 0.3202(13) 0.4451(11) 0.1424(8) 0.128(5) Uiso 0.50 1 d PD A 2 C52' C 0.339(2) 0.3945(19) 0.2270(10) 0.232(10) Uiso 0.50 1 d PD A 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 K1 0.0593(5) 0.0656(5) 0.0586(5) 0.0090(4) 0.0024(4) 0.0112(4) K2 0.0960(9) 0.0603(7) 0.0522(7) 0.0262(6) 0.0210(6) 0.0168(7) C1 0.0489(19) 0.0443(17) 0.0424(18) 0.0114(14) 0.0128(15) 0.0140(15) C2 0.052(2) 0.0440(17) 0.0393(17) 0.0139(14) 0.0158(15) 0.0184(15) C11 0.051(2) 0.056(2) 0.059(2) 0.0088(17) 0.0104(17) 0.0214(18) C12 0.058(2) 0.052(2) 0.047(2) 0.0067(16) 0.0065(17) 0.0149(18) C13 0.061(3) 0.065(3) 0.064(2) 0.008(2) 0.0039(19) 0.008(2) C14 0.086(3) 0.057(3) 0.068(3) 0.011(2) -0.005(2) -0.001(2) C15 0.116(4) 0.049(2) 0.056(2) 0.0018(18) -0.008(2) 0.020(3) C16 0.088(3) 0.058(2) 0.051(2) 0.0047(18) 0.007(2) 0.033(2) C17 0.066(2) 0.052(2) 0.0360(17) 0.0080(15) 0.0068(16) 0.0196(19) C18 0.061(2) 0.060(2) 0.0464(19) 0.0070(16) 0.0148(17) 0.0277(19) C31 0.145(6) 0.083(4) 0.120(5) 0.003(3) 0.031(4) -0.014(4) C32 0.124(5) 0.068(3) 0.137(5) 0.013(3) 0.012(4) -0.013(3) C33 0.076(3) 0.101(4) 0.114(4) -0.002(3) -0.010(3) 0.006(3) C34 0.060(3) 0.115(4) 0.101(4) 0.007(3) -0.017(2) 0.022(3) C35 0.124(5) 0.116(4) 0.085(4) 0.033(3) 0.004(3) 0.035(4) C36 0.121(5) 0.140(5) 0.073(3) 0.045(3) 0.011(3) 0.019(4) C37 0.088(4) 0.110(4) 0.123(5) 0.030(4) 0.028(3) -0.014(3) C38 0.096(4) 0.091(4) 0.117(5) 0.014(3) 0.018(3) -0.011(3) C39 0.114(5) 0.141(5) 0.084(4) -0.003(4) -0.015(3) 0.000(4) C40 0.083(4) 0.190(7) 0.101(4) 0.038(5) -0.023(3) -0.004(5) C41 0.133(6) 0.171(6) 0.075(3) 0.044(4) 0.028(3) 0.052(5) C42 0.137(5) 0.112(4) 0.068(3) 0.032(3) 0.025(3) 0.042(4) O1 0.105(3) 0.110(2) 0.081(2) 0.0216(19) 0.028(2) 0.018(2) O2 0.079(2) 0.082(2) 0.104(3) -0.0006(19) -0.0011(18) 0.0012(17) O3 0.075(2) 0.097(2) 0.090(2) 0.0155(18) 0.0007(16) 0.0278(18) O4 0.094(2) 0.094(2) 0.081(2) 0.0280(17) 0.0148(17) 0.0076(19) O5 0.087(2) 0.099(2) 0.079(2) 0.0011(19) 0.0009(17) 0.0019(19) O6 0.106(3) 0.128(3) 0.086(2) 0.031(2) 0.000(2) 0.023(2) B3 0.049(2) 0.058(2) 0.049(2) 0.0162(19) 0.0125(19) 0.017(2) B4 0.061(3) 0.065(3) 0.043(2) 0.008(2) 0.006(2) 0.003(2) B5 0.083(3) 0.050(2) 0.044(2) 0.0077(19) 0.013(2) 0.015(2) B6 0.064(3) 0.047(2) 0.054(2) 0.0121(19) 0.021(2) 0.020(2) B7 0.072(3) 0.058(2) 0.052(2) 0.023(2) 0.017(2) 0.026(2) B8 0.066(3) 0.083(3) 0.052(3) 0.022(2) -0.001(2) 0.024(3) B9 0.093(4) 0.076(3) 0.034(2) 0.008(2) 0.006(2) 0.012(3) B10 0.095(4) 0.070(3) 0.041(2) 0.011(2) 0.030(2) 0.026(3) B11 0.068(3) 0.063(3) 0.054(2) 0.023(2) 0.028(2) 0.018(2) B12 0.096(4) 0.075(3) 0.044(2) 0.026(2) 0.023(2) 0.027(3) K3 0.0749(8) 0.0651(7) 0.0511(7) -0.0019(6) 0.0026(6) 0.0125(6) O7 0.139(3) 0.076(2) 0.098(2) -0.0080(18) -0.016(2) 0.031(2) O8 0.086(2) 0.0810(19) 0.0698(18) 0.0119(16) 0.0022(15) 0.0079(16) O9 0.128(3) 0.085(2) 0.083(2) -0.0120(18) -0.010(2) 0.024(2) C53 0.280(10) 0.146(6) 0.106(5) -0.047(4) -0.046(6) 0.126(6) C54 0.110(4) 0.088(3) 0.101(4) 0.008(3) -0.009(3) 0.040(3) C55 0.087(3) 0.085(3) 0.095(4) 0.029(3) -0.001(3) 0.012(3) C56 0.100(4) 0.094(3) 0.052(2) -0.005(2) -0.007(2) 0.013(3) C57 0.121(5) 0.094(4) 0.073(3) -0.017(3) -0.013(3) 0.005(3) C58 0.274(10) 0.075(4) 0.142(6) -0.047(4) -0.096(6) 0.073(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 K1 O5 2.833(3) . ? K1 O1 2.863(3) . ? K1 O3 2.870(3) . ? K1 O2 2.885(3) . ? K1 O4 2.896(3) . ? K1 O6 2.932(3) . ? K1 B10 3.301(5) . ? K1 B5 3.479(5) . ? K1 B6 3.495(4) . ? K2 C2 2.943(3) 2_576 ? K2 C2 2.943(3) . ? K2 C1 2.994(3) 2_576 ? K2 C1 2.994(3) . ? K2 B4 3.036(4) . ? K2 B4 3.036(4) 2_576 ? K2 B3 3.092(4) 2_576 ? K2 B3 3.092(4) . ? K2 B5 3.109(4) . ? K2 B5 3.109(4) 2_576 ? K2 B6 3.212(4) 2_576 ? K2 B6 3.212(4) . ? C1 C2 1.437(4) . ? C1 C11 1.524(4) . ? C1 B6 1.542(5) . ? C1 B11 1.787(5) . ? C2 C18 1.525(4) . ? C2 B3 1.537(5) . ? C2 B7 1.789(5) . ? C11 C12 1.507(4) . ? C12 C13 1.380(5) . ? C12 C17 1.383(5) . ? C13 C14 1.379(5) . ? C14 C15 1.366(6) . ? C15 C16 1.378(6) . ? C16 C17 1.394(5) . ? C17 C18 1.503(5) . ? C31 O1 1.370(6) . ? C31 C32 1.445(7) . ? C32 O2 1.403(6) . ? C33 O2 1.396(6) . ? C33 C34 1.467(7) . ? C34 O3 1.408(5) . ? C35 O3 1.390(5) . ? C35 C36 1.492(7) . ? C36 O4 1.424(5) . ? C37 O4 1.399(5) . ? C37 C38 1.477(7) . ? C38 O5 1.379(6) . ? C39 O5 1.387(6) . ? C39 C40 1.425(8) . ? C40 O6 1.402(6) . ? C41 O6 1.342(6) . ? C41 C42 1.450(7) . ? C42 O1 1.392(5) . ? B3 B8 1.761(6) . ? B3 B4 1.806(6) . ? B3 B7 1.824(6) . ? B4 B5 1.704(7) . ? B4 B8 1.749(6) . ? B4 B9 1.769(6) . ? B5 B10 1.743(6) . ? B5 B9 1.760(6) . ? B5 B6 1.814(6) . ? B6 B10 1.774(6) . ? B6 B11 1.830(6) . ? B7 B12 1.731(6) . ? B7 B8 1.815(7) . ? B7 B11 1.910(6) . ? B8 B9 1.746(7) . ? B8 B12 1.781(7) . ? B9 B10 1.724(7) . ? B9 B12 1.783(7) . ? B10 B12 1.761(7) . ? B10 B11 1.820(6) . ? B11 B12 1.738(7) . ? K3 O9 2.803(3) 2_665 ? K3 O9 2.803(3) . ? K3 O7 2.802(3) 2_665 ? K3 O7 2.802(3) . ? K3 O8 2.818(3) 2_665 ? K3 O8 2.818(3) . ? K3 N1 2.913(10) 2_665 ? K3 N1 2.913(10) . ? K3 N1' 2.770(12) . ? K3 N1' 2.770(12) 2_665 ? K3 C51' 3.482(14) . ? K3 C51' 3.482(14) 2_665 ? O7 C53 1.405(6) . ? O7 C54 1.426(5) . ? O8 C55 1.413(5) . ? O8 C56 1.414(5) . ? O9 C57 1.416(6) . ? O9 C58 1.412(6) . ? C53 C58 1.483(9) 2_665 ? C54 C55 1.486(6) . ? C56 C57 1.500(6) . ? C58 C53 1.483(9) 2_665 ? N1 C51 0.976(13) . ? C51 C52 1.705(17) . ? N1' C51' 1.018(4) . ? C51' C52' 1.570(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 K1 O1 112.88(10) . . ? O5 K1 O3 115.69(10) . . ? O1 K1 O3 114.59(10) . . ? O5 K1 O2 145.67(10) . . ? O1 K1 O2 56.38(11) . . ? O3 K1 O2 58.64(10) . . ? O5 K1 O4 57.63(10) . . ? O1 K1 O4 143.76(10) . . ? O3 K1 O4 58.30(9) . . ? O2 K1 O4 109.51(10) . . ? O5 K1 O6 57.94(11) . . ? O1 K1 O6 55.74(11) . . ? O3 K1 O6 148.50(10) . . ? O2 K1 O6 107.48(11) . . ? O4 K1 O6 109.65(10) . . ? O5 K1 B10 107.90(12) . . ? O1 K1 B10 82.77(10) . . ? O3 K1 B10 118.67(10) . . ? O2 K1 B10 102.96(11) . . ? O4 K1 B10 133.06(10) . . ? O6 K1 B10 91.14(11) . . ? O5 K1 B5 90.10(10) . . ? O1 K1 B5 111.70(10) . . ? O3 K1 B5 109.26(10) . . ? O2 K1 B5 124.18(10) . . ? O4 K1 B5 103.54(10) . . ? O6 K1 B5 101.78(11) . . ? B10 K1 B5 29.65(10) . . ? O5 K1 B6 119.64(10) . . ? O1 K1 B6 102.02(9) . . ? O3 K1 B6 89.49(10) . . ? O2 K1 B6 94.64(10) . . ? O4 K1 B6 112.87(9) . . ? O6 K1 B6 121.11(11) . . ? B10 K1 B6 30.09(10) . . ? B5 K1 B6 30.15(10) . . ? C2 K2 C2 180.000(1) 2_576 . ? C2 K2 C1 28.00(8) 2_576 2_576 ? C2 K2 C1 152.00(8) . 2_576 ? C2 K2 C1 152.00(8) 2_576 . ? C2 K2 C1 28.00(8) . . ? C1 K2 C1 180.0 2_576 . ? C2 K2 B4 123.22(10) 2_576 . ? C2 K2 B4 56.78(10) . . ? C1 K2 B4 114.70(10) 2_576 . ? C1 K2 B4 65.30(10) . . ? C2 K2 B4 56.78(10) 2_576 2_576 ? C2 K2 B4 123.22(10) . 2_576 ? C1 K2 B4 65.30(10) 2_576 2_576 ? C1 K2 B4 114.70(10) . 2_576 ? B4 K2 B4 180.000(1) . 2_576 ? C2 K2 B3 29.38(9) 2_576 2_576 ? C2 K2 B3 150.62(9) . 2_576 ? C1 K2 B3 51.89(10) 2_576 2_576 ? C1 K2 B3 128.11(10) . 2_576 ? B4 K2 B3 145.74(11) . 2_576 ? B4 K2 B3 34.26(11) 2_576 2_576 ? C2 K2 B3 150.62(9) 2_576 . ? C2 K2 B3 29.38(9) . . ? C1 K2 B3 128.11(10) 2_576 . ? C1 K2 B3 51.89(10) . . ? B4 K2 B3 34.26(11) . . ? B4 K2 B3 145.74(11) 2_576 . ? B3 K2 B3 180.000(1) 2_576 . ? C2 K2 B5 115.09(10) 2_576 . ? C2 K2 B5 64.91(10) . . ? C1 K2 B5 124.21(10) 2_576 . ? C1 K2 B5 55.79(10) . . ? B4 K2 B5 32.17(12) . . ? B4 K2 B5 147.83(13) 2_576 . ? B3 K2 B5 122.62(11) 2_576 . ? B3 K2 B5 57.38(11) . . ? C2 K2 B5 64.91(10) 2_576 2_576 ? C2 K2 B5 115.09(10) . 2_576 ? C1 K2 B5 55.79(10) 2_576 2_576 ? C1 K2 B5 124.21(10) . 2_576 ? B4 K2 B5 147.83(13) . 2_576 ? B4 K2 B5 32.17(12) 2_576 2_576 ? B3 K2 B5 57.38(11) 2_576 2_576 ? B3 K2 B5 122.62(11) . 2_576 ? B5 K2 B5 180.000(1) . 2_576 ? C2 K2 B6 50.97(9) 2_576 2_576 ? C2 K2 B6 129.03(9) . 2_576 ? C1 K2 B6 28.50(9) 2_576 2_576 ? C1 K2 B6 151.50(9) . 2_576 ? B4 K2 B6 123.16(12) . 2_576 ? B4 K2 B6 56.84(12) 2_576 2_576 ? B3 K2 B6 62.67(11) 2_576 2_576 ? B3 K2 B6 117.33(11) . 2_576 ? B5 K2 B6 146.70(11) . 2_576 ? B5 K2 B6 33.30(11) 2_576 2_576 ? C2 K2 B6 129.03(9) 2_576 . ? C2 K2 B6 50.97(9) . . ? C1 K2 B6 151.50(9) 2_576 . ? C1 K2 B6 28.50(9) . . ? B4 K2 B6 56.84(12) . . ? B4 K2 B6 123.16(12) 2_576 . ? B3 K2 B6 117.33(11) 2_576 . ? B3 K2 B6 62.67(11) . . ? B5 K2 B6 33.30(11) . . ? B5 K2 B6 146.70(12) 2_576 . ? B6 K2 B6 180.000(1) 2_576 . ? C2 C1 C11 115.9(3) . . ? C2 C1 B6 126.4(3) . . ? C11 C1 B6 117.1(3) . . ? C2 C1 B11 96.8(3) . . ? C11 C1 B11 116.3(3) . . ? B6 C1 B11 66.2(2) . . ? C2 C1 K2 74.03(16) . . ? C11 C1 K2 107.2(2) . . ? B6 C1 K2 83.61(18) . . ? B11 C1 K2 134.7(2) . . ? C1 C2 C18 115.2(3) . . ? C1 C2 B3 127.1(3) . . ? C18 C2 B3 116.9(3) . . ? C1 C2 B7 98.4(2) . . ? C18 C2 B7 115.8(3) . . ? B3 C2 B7 66.0(2) . . ? C1 C2 K2 77.97(16) . . ? C18 C2 K2 105.53(18) . . ? B3 C2 K2 80.69(18) . . ? B7 C2 K2 135.1(2) . . ? C12 C11 C1 113.7(3) . . ? C13 C12 C17 119.6(3) . . ? C13 C12 C11 123.6(3) . . ? C17 C12 C11 116.8(3) . . ? C12 C13 C14 120.3(4) . . ? C15 C14 C13 120.5(4) . . ? C14 C15 C16 119.8(4) . . ? C15 C16 C17 120.3(4) . . ? C12 C17 C16 119.5(3) . . ? C12 C17 C18 117.3(3) . . ? C16 C17 C18 123.2(3) . . ? C17 C18 C2 113.8(3) . . ? O1 C31 C32 111.8(5) . . ? O2 C32 C31 109.6(4) . . ? O2 C33 C34 110.1(4) . . ? O3 C34 C33 110.6(4) . . ? O3 C35 C36 110.4(5) . . ? O4 C36 C35 108.2(4) . . ? O4 C37 C38 109.3(4) . . ? O5 C38 C37 110.6(5) . . ? O5 C39 C40 112.1(5) . . ? O6 C40 C39 109.9(6) . . ? O6 C41 C42 113.5(5) . . ? O1 C42 C41 110.4(4) . . ? C31 O1 C42 116.1(4) . . ? C31 O1 K1 121.0(3) . . ? C42 O1 K1 122.1(3) . . ? C33 O2 C32 112.9(4) . . ? C33 O2 K1 110.3(3) . . ? C32 O2 K1 110.7(3) . . ? C35 O3 C34 113.7(4) . . ? C35 O3 K1 118.4(3) . . ? C34 O3 K1 117.0(3) . . ? C37 O4 C36 113.1(4) . . ? C37 O4 K1 111.4(3) . . ? C36 O4 K1 108.9(3) . . ? C38 O5 C39 113.8(5) . . ? C38 O5 K1 120.4(3) . . ? C39 O5 K1 118.4(3) . . ? C41 O6 C40 113.9(5) . . ? C41 O6 K1 109.2(3) . . ? C40 O6 K1 106.8(3) . . ? C2 B3 B8 118.9(3) . . ? C2 B3 B4 116.4(3) . . ? B8 B3 B4 58.7(2) . . ? C2 B3 B7 63.7(2) . . ? B8 B3 B7 60.8(2) . . ? B4 B3 B7 104.3(3) . . ? C2 B3 K2 69.93(18) . . ? B8 B3 K2 127.6(3) . . ? B4 B3 K2 71.16(18) . . ? B7 B3 K2 124.8(2) . . ? B5 B4 B8 109.6(3) . . ? B5 B4 B9 60.9(3) . . ? B8 B4 B9 59.5(3) . . ? B5 B4 B3 116.0(3) . . ? B8 B4 B3 59.4(2) . . ? B9 B4 B3 110.5(3) . . ? B5 B4 K2 76.3(2) . . ? B8 B4 K2 131.5(2) . . ? B9 B4 K2 134.8(3) . . ? B3 B4 K2 74.58(18) . . ? B4 B5 B10 109.1(3) . . ? B4 B5 B9 61.4(3) . . ? B10 B5 B9 58.9(3) . . ? B4 B5 B6 115.6(3) . . ? B10 B5 B6 59.8(2) . . ? B9 B5 B6 110.8(3) . . ? B4 B5 K2 71.54(19) . . ? B10 B5 K2 132.0(2) . . ? B9 B5 K2 130.7(3) . . ? B6 B5 K2 76.45(18) . . ? B4 B5 K1 167.0(2) . . ? B10 B5 K1 69.5(2) . . ? B9 B5 K1 109.1(2) . . ? B6 B5 K1 75.4(2) . . ? K2 B5 K1 119.53(14) . . ? C1 B6 B10 118.4(3) . . ? C1 B6 B5 116.5(3) . . ? B10 B6 B5 58.1(2) . . ? C1 B6 B11 63.3(2) . . ? B10 B6 B11 60.7(2) . . ? B5 B6 B11 104.0(3) . . ? C1 B6 K2 67.89(17) . . ? B10 B6 K2 124.8(3) . . ? B5 B6 K2 70.25(18) . . ? B11 B6 K2 120.8(2) . . ? C1 B6 K1 168.7(3) . . ? B10 B6 K1 68.89(19) . . ? B5 B6 K1 74.45(19) . . ? B11 B6 K1 118.3(2) . . ? K2 B6 K1 116.19(11) . . ? B12 B7 C2 123.3(3) . . ? B12 B7 B8 60.3(3) . . ? C2 B7 B8 104.1(3) . . ? B12 B7 B3 108.1(3) . . ? C2 B7 B3 50.34(19) . . ? B8 B7 B3 57.9(2) . . ? B12 B7 B11 56.8(2) . . ? C2 B7 B11 81.7(2) . . ? B8 B7 B11 105.7(3) . . ? B3 B7 B11 111.6(3) . . ? B4 B8 B9 60.8(3) . . ? B4 B8 B3 61.9(2) . . ? B9 B8 B3 113.8(3) . . ? B4 B8 B12 105.8(4) . . ? B9 B8 B12 60.7(3) . . ? B3 B8 B12 108.7(3) . . ? B4 B8 B7 107.1(3) . . ? B9 B8 B7 108.8(4) . . ? B3 B8 B7 61.3(2) . . ? B12 B8 B7 57.5(2) . . ? B10 B9 B8 111.1(3) . . ? B10 B9 B5 60.0(3) . . ? B8 B9 B5 107.2(3) . . ? B10 B9 B4 107.0(3) . . ? B8 B9 B4 59.7(3) . . ? B5 B9 B4 57.8(2) . . ? B10 B9 B12 60.3(3) . . ? B8 B9 B12 60.6(3) . . ? B5 B9 B12 105.2(3) . . ? B4 B9 B12 104.9(3) . . ? B9 B10 B5 61.0(3) . . ? B9 B10 B12 61.5(3) . . ? B5 B10 B12 106.9(3) . . ? B9 B10 B6 114.5(3) . . ? B5 B10 B6 62.1(2) . . ? B12 B10 B6 109.5(3) . . ? B9 B10 B11 109.8(3) . . ? B5 B10 B11 107.3(3) . . ? B12 B10 B11 58.0(3) . . ? B6 B10 B11 61.2(2) . . ? B9 B10 K1 118.1(3) . . ? B5 B10 K1 80.9(2) . . ? B12 B10 K1 168.9(2) . . ? B6 B10 K1 81.0(2) . . ? B11 B10 K1 128.1(3) . . ? B12 B11 C1 124.0(3) . . ? B12 B11 B10 59.3(3) . . ? C1 B11 B10 104.4(3) . . ? B12 B11 B6 108.0(3) . . ? C1 B11 B6 50.46(19) . . ? B10 B11 B6 58.2(2) . . ? B12 B11 B7 56.4(2) . . ? C1 B11 B7 83.1(2) . . ? B10 B11 B7 104.6(3) . . ? B6 B11 B7 112.4(3) . . ? B11 B12 B7 66.8(3) . . ? B11 B12 B10 62.7(3) . . ? B7 B12 B10 115.5(3) . . ? B11 B12 B9 110.9(3) . . ? B7 B12 B9 111.0(3) . . ? B10 B12 B9 58.2(3) . . ? B11 B12 B8 115.0(3) . . ? B7 B12 B8 62.2(3) . . ? B10 B12 B8 107.7(3) . . ? B9 B12 B8 58.7(3) . . ? O9 K3 O9 180.00(11) 2_665 . ? O9 K3 O7 118.75(10) 2_665 2_665 ? O9 K3 O7 61.25(10) . 2_665 ? O9 K3 O7 61.25(10) 2_665 . ? O9 K3 O7 118.75(10) . . ? O7 K3 O7 180.000(1) 2_665 . ? O9 K3 O8 60.35(10) 2_665 2_665 ? O9 K3 O8 119.65(10) . 2_665 ? O7 K3 O8 59.95(9) 2_665 2_665 ? O7 K3 O8 120.05(9) . 2_665 ? O9 K3 O8 119.65(10) 2_665 . ? O9 K3 O8 60.35(10) . . ? O7 K3 O8 120.05(9) 2_665 . ? O7 K3 O8 59.95(9) . . ? O8 K3 O8 180.00(12) 2_665 . ? O9 K3 N1 92.7(2) 2_665 2_665 ? O9 K3 N1 87.3(2) . 2_665 ? O7 K3 N1 74.9(2) 2_665 2_665 ? O7 K3 N1 105.1(2) . 2_665 ? O8 K3 N1 90.0(2) 2_665 2_665 ? O8 K3 N1 90.0(2) . 2_665 ? O9 K3 N1 87.3(2) 2_665 . ? O9 K3 N1 92.7(2) . . ? O7 K3 N1 105.1(2) 2_665 . ? O7 K3 N1 74.9(2) . . ? O8 K3 N1 90.0(2) 2_665 . ? O8 K3 N1 90.0(2) . . ? N1 K3 N1 180.0 2_665 . ? O9 K3 N1' 100.3(3) 2_665 . ? O9 K3 N1' 79.7(3) . . ? O7 K3 N1' 84.3(3) 2_665 . ? O7 K3 N1' 95.7(3) . . ? O8 K3 N1' 82.3(3) 2_665 . ? O8 K3 N1' 97.7(3) . . ? N1 K3 N1' 158.9(3) 2_665 . ? N1 K3 N1' 21.1(3) . . ? O9 K3 N1' 79.7(3) 2_665 2_665 ? O9 K3 N1' 100.3(3) . 2_665 ? O7 K3 N1' 95.7(3) 2_665 2_665 ? O7 K3 N1' 84.3(3) . 2_665 ? O8 K3 N1' 97.7(3) 2_665 2_665 ? O8 K3 N1' 82.3(3) . 2_665 ? N1 K3 N1' 21.1(3) 2_665 2_665 ? N1 K3 N1' 158.9(3) . 2_665 ? N1' K3 N1' 180.0(5) . 2_665 ? O9 K3 C51' 108.9(2) 2_665 . ? O9 K3 C51' 71.1(2) . . ? O7 K3 C51' 89.1(2) 2_665 . ? O7 K3 C51' 90.9(2) . . ? O8 K3 C51' 95.6(2) 2_665 . ? O8 K3 C51' 84.4(2) . . ? N1 K3 C51' 157.6(3) 2_665 . ? N1 K3 C51' 22.4(3) . . ? N1' K3 C51' 13.5(3) . . ? N1' K3 C51' 166.5(3) 2_665 . ? O9 K3 C51' 71.1(2) 2_665 2_665 ? O9 K3 C51' 108.9(2) . 2_665 ? O7 K3 C51' 90.9(2) 2_665 2_665 ? O7 K3 C51' 89.1(2) . 2_665 ? O8 K3 C51' 84.4(2) 2_665 2_665 ? O8 K3 C51' 95.6(2) . 2_665 ? N1 K3 C51' 22.4(3) 2_665 2_665 ? N1 K3 C51' 157.6(3) . 2_665 ? N1' K3 C51' 166.5(3) . 2_665 ? N1' K3 C51' 13.5(3) 2_665 2_665 ? C51' K3 C51' 180.0(4) . 2_665 ? C53 O7 C54 112.4(5) . . ? C53 O7 K3 110.0(3) . . ? C54 O7 K3 114.4(3) . . ? C55 O8 C56 112.3(3) . . ? C55 O8 K3 115.2(2) . . ? C56 O8 K3 114.6(3) . . ? C57 O9 C58 113.5(4) . . ? C57 O9 K3 113.8(3) . . ? C58 O9 K3 113.0(3) . . ? O7 C53 C58 109.4(7) . 2_665 ? O7 C53 K3 48.1(2) . . ? C58 C53 K3 80.2(3) 2_665 . ? O7 C54 C55 110.1(4) . . ? O8 C55 C54 107.6(4) . . ? O8 C56 C57 109.2(4) . . ? O9 C57 C56 108.6(4) . . ? O9 C58 C53 108.2(6) . 2_665 ? C51 N1 K3 122.1(11) . . ? N1 C51 C52 160.4(16) . . ? N1 C51 K3 44.4(9) . . ? C52 C51 K3 121.1(7) . . ? C51' N1' K3 127.2(13) . . ? N1' C51' C52' 158.0(13) . . ? N1' C51' K3 39.3(10) . . ? C52' C51' K3 132.7(11) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.488 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.047 #===END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H88 B20 K2 O13' _chemical_formula_weight 1119.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.253(3) _cell_length_b 11.361(2) _cell_length_c 21.675(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.01(3) _cell_angle_gamma 90.00 _cell_volume 3136.(1) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 0.205 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.90700 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'AFC7R Rigaku Diffractometer' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5762 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.1078 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5503 _reflns_number_gt 2555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'AFC7R Rigaku Diffractometer' _computing_cell_refinement 'AFC7R Rigaku Diffractometer' _computing_data_reduction 'AFC7R Rigaku Diffractometer' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.1243P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5503 _refine_ls_number_parameters 403 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.1839 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.2583 _refine_ls_wR_factor_gt 0.2076 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.228 _refine_ls_shift/su_mean 0.010 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 K1 K 0.16610(4) 0.84294(6) 0.03154(3) 0.07314(19) Uani 1 1 d . . . C1 C 0.58211(16) 0.6271(2) 0.11319(9) 0.0492(6) Uani 1 1 d . . . C2 C 0.58156(17) 0.5002(2) 0.11749(10) 0.0506(6) Uani 1 1 d . . . C3 C 0.69024(18) 0.4418(2) 0.13602(12) 0.0618(8) Uani 1 1 d . . . H3A H 0.6836 0.3624 0.1509 0.074 Uiso 1 1 calc R . . H3B H 0.7154 0.4362 0.0981 0.074 Uiso 1 1 calc R . . C4 C 0.76979(16) 0.5073(2) 0.18734(10) 0.0543(7) Uani 1 1 d . . . C5 C 0.84187(18) 0.4501(3) 0.23672(12) 0.0703(9) Uani 1 1 d . . . H5A H 0.8416 0.3684 0.2393 0.084 Uiso 1 1 calc R . . C6 C 0.91499(19) 0.5156(3) 0.28273(13) 0.0781(9) Uani 1 1 d . . . H6A H 0.9655 0.4776 0.3150 0.094 Uiso 1 1 calc R . . C7 C 0.91182(19) 0.6354(3) 0.27996(13) 0.0820(10) Uani 1 1 d . . . H7A H 0.9593 0.6790 0.3112 0.098 Uiso 1 1 calc R . . C8 C 0.83872(18) 0.6928(2) 0.23130(12) 0.0683(8) Uani 1 1 d . . . H8A H 0.8365 0.7746 0.2302 0.082 Uiso 1 1 calc R . . C9 C 0.76903(16) 0.6284(2) 0.18429(10) 0.0540(7) Uani 1 1 d . . . C10 C 0.68992(18) 0.6845(2) 0.12868(11) 0.0605(7) Uani 1 1 d . . . H10A H 0.7159 0.6805 0.0910 0.073 Uiso 1 1 calc R . . H10B H 0.6830 0.7670 0.1383 0.073 Uiso 1 1 calc R . . C21 C 0.2398(4) 0.9478(5) 0.19508(17) 0.295(3) Uani 1 1 d D . . H21A H 0.2960 0.8903 0.2036 0.354 Uiso 1 1 calc R . . H21B H 0.2281 0.9709 0.2357 0.354 Uiso 1 1 calc R . . C22 C 0.2700(4) 1.0551(4) 0.1618(2) 0.274(2) Uani 1 1 d D . . H22A H 0.2126 1.1112 0.1516 0.329 Uiso 1 1 calc R . . H22B H 0.3310 1.0932 0.1899 0.329 Uiso 1 1 calc R . . C23 C 0.3198(4) 1.1100(4) 0.0746(3) 0.269(3) Uani 1 1 d D . . H23A H 0.3761 1.1546 0.1031 0.323 Uiso 1 1 calc R . . H23B H 0.2604 1.1620 0.0583 0.323 Uiso 1 1 calc R . . C24 C 0.3553(3) 1.0600(4) 0.0204(3) 0.244(3) Uani 1 1 d D . . H24A H 0.3873 1.1213 0.0009 0.293 Uiso 1 1 calc R . . H24B H 0.4072 0.9990 0.0362 0.293 Uiso 1 1 calc R . . C25 C 0.2929(3) 0.9585(4) -0.0775(2) 0.2542(18) Uani 1 1 d D . . H25A H 0.3331 0.8872 -0.0637 0.305 Uiso 1 1 calc R . . H25B H 0.3341 1.0109 -0.0963 0.305 Uiso 1 1 calc R . . C26 C 0.1924(4) 0.9300(5) -0.12504(19) 0.246(2) Uani 1 1 d D . . H26A H 0.1470 0.9985 -0.1337 0.295 Uiso 1 1 calc R . . H26B H 0.2045 0.9036 -0.1650 0.295 Uiso 1 1 calc R . . C27 C 0.0492(4) 0.8134(5) -0.13850(18) 0.250(3) Uani 1 1 d D . . H27A H 0.0548 0.7976 -0.1814 0.300 Uiso 1 1 calc R . . H27B H 0.0016 0.8792 -0.1409 0.300 Uiso 1 1 calc R . . C28 C 0.0069(5) 0.7077(5) -0.1134(2) 0.288(3) Uani 1 1 d D . . H28A H -0.0564 0.6796 -0.1441 0.346 Uiso 1 1 calc R . . H28B H 0.0583 0.6447 -0.1043 0.346 Uiso 1 1 calc R . . C29 C -0.0534(4) 0.6544(4) -0.0271(3) 0.259(5) Uani 1 1 d D . . H29A H -0.0039 0.5894 -0.0194 0.311 Uiso 1 1 calc R . . H29B H -0.1190 0.6263 -0.0554 0.311 Uiso 1 1 calc R . . C30 C -0.0718(3) 0.6915(5) 0.0363(3) 0.291(4) Uani 1 1 d D . . H30A H -0.1210 0.7566 0.0294 0.349 Uiso 1 1 calc R . . H30B H -0.1014 0.6265 0.0545 0.349 Uiso 1 1 calc R . . C31 C 0.0185(3) 0.7499(6) 0.1420(2) 0.325(2) Uani 1 1 d D . . H31A H 0.0007 0.6786 0.1614 0.390 Uiso 1 1 calc R . . H31B H -0.0357 0.8080 0.1407 0.390 Uiso 1 1 calc R . . C32 C 0.1238(4) 0.7960(5) 0.1815(2) 0.322(3) Uani 1 1 d D . . H32A H 0.1211 0.8099 0.2252 0.387 Uiso 1 1 calc R . . H32B H 0.1775 0.7374 0.1828 0.387 Uiso 1 1 calc R . . B3 B 0.4883(2) 0.4167(2) 0.09978(13) 0.0591(9) Uani 1 1 d . . . H3 H 0.5035(16) 0.3318(18) 0.1010(9) 0.059(6) Uiso 1 1 d . . . B4 B 0.3656(2) 0.4799(3) 0.04970(14) 0.0658(10) Uani 1 1 d . . . H4 H 0.3208(19) 0.423(2) 0.0102(12) 0.095(8) Uiso 1 1 d . . . B5 B 0.3661(2) 0.6394(3) 0.04338(13) 0.0619(9) Uani 1 1 d . . . H1 H 0.4229(17) 0.560(2) 0.0323(11) 0.079(7) Uiso 1 1 d . . . H5 H 0.3200(18) 0.678(2) 0.0014(12) 0.082(8) Uiso 1 1 d . . . B6 B 0.4885(2) 0.7091(3) 0.08886(13) 0.0565(8) Uani 1 1 d . . . H6 H 0.5058(17) 0.802(2) 0.0803(10) 0.068(7) Uiso 1 1 d . . . B7 B 0.5081(2) 0.4899(3) 0.17695(13) 0.0594(9) Uani 1 1 d . . . H7 H 0.5536(17) 0.456(2) 0.2226(11) 0.082(8) Uiso 1 1 d . . . B8 B 0.3817(2) 0.4445(3) 0.12970(15) 0.0660(9) Uani 1 1 d . . . H8 H 0.3420(16) 0.379(2) 0.1418(10) 0.070(7) Uiso 1 1 d . . . B9 B 0.3071(2) 0.5686(3) 0.09632(14) 0.0667(10) Uani 1 1 d . . . H4 H 0.2189(17) 0.563(2) 0.0980(10) 0.073(7) Uiso 1 1 d . . . B10 B 0.3817(2) 0.6959(3) 0.12004(14) 0.0621(9) Uani 1 1 d . . . H10 H 0.3463(14) 0.7765(17) 0.1228(9) 0.048(6) Uiso 1 1 d . . . B11 B 0.5082(2) 0.6578(2) 0.17017(11) 0.0511(7) Uani 1 1 d . . . H11 H 0.5530(17) 0.7034(19) 0.2118(10) 0.065(6) Uiso 1 1 d . . . B12 B 0.3999(2) 0.5765(3) 0.17484(13) 0.0588(9) Uani 1 1 d . . . H12 H 0.3771(17) 0.578(2) 0.2232(11) 0.079(7) Uiso 1 1 d . . . O1 O 0.1502(2) 0.9000(3) 0.15595(13) 0.2080(14) Uani 1 1 d D . . O2 O 0.2919(2) 1.0177(2) 0.10661(15) 0.1694(13) Uani 1 1 d D . . O3 O 0.26923(18) 1.0135(2) -0.02461(15) 0.1478(12) Uani 1 1 d D . . O4 O 0.1481(2) 0.8425(3) -0.09827(11) 0.1505(11) Uani 1 1 d D . . O5 O -0.0144(2) 0.7458(2) -0.05813(17) 0.1690(15) Uani 1 1 d D . . O6 O 0.02429(19) 0.7257(3) 0.07889(16) 0.2212(11) Uani 1 1 d D . . O7 O 0.0000 1.0000 0.0000 0.259(4) Uani 1 2 d S . . 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 K1 0.0624(3) 0.0930(4) 0.0635(3) 0.0040(3) 0.0165(2) -0.0008(3) C1 0.0564(12) 0.0541(14) 0.0382(10) 0.0012(10) 0.0149(9) 0.0019(11) C2 0.0612(12) 0.0516(13) 0.0413(10) -0.0048(10) 0.0179(9) -0.0009(11) C3 0.0648(14) 0.0536(15) 0.0652(14) -0.0062(12) 0.0149(12) 0.0101(12) C4 0.0489(11) 0.0638(15) 0.0525(12) 0.0005(11) 0.0179(10) 0.0050(12) C5 0.0631(14) 0.0752(17) 0.0711(15) 0.0058(14) 0.0158(12) 0.0101(14) C6 0.0575(14) 0.103(2) 0.0654(16) 0.0017(15) 0.0032(13) 0.0157(16) C7 0.0561(14) 0.121(2) 0.0646(15) -0.0184(17) 0.0093(12) -0.0114(17) C8 0.0597(14) 0.0754(17) 0.0711(15) -0.0126(14) 0.0200(12) -0.0113(13) C9 0.0480(11) 0.0655(15) 0.0512(11) 0.0003(11) 0.0181(10) -0.0014(12) C10 0.0667(13) 0.0527(15) 0.0661(14) 0.0024(12) 0.0250(11) -0.0063(12) C21 0.317(4) 0.490(7) 0.062(2) -0.044(3) 0.023(3) 0.276(4) C22 0.168(4) 0.306(4) 0.258(4) -0.214(3) -0.094(3) 0.122(4) C23 0.182(4) 0.082(3) 0.398(7) -0.057(4) -0.162(4) 0.012(3) C24 0.091(3) 0.148(3) 0.475(7) 0.176(4) 0.048(4) -0.019(2) C25 0.287(3) 0.183(4) 0.401(4) 0.181(3) 0.277(3) 0.098(3) C26 0.348(5) 0.302(5) 0.141(3) 0.133(3) 0.154(3) 0.202(4) C27 0.212(5) 0.436(8) 0.067(2) -0.080(4) -0.021(3) 0.127(5) C28 0.203(6) 0.272(5) 0.302(6) -0.214(4) -0.078(5) 0.036(5) C29 0.132(4) 0.100(3) 0.494(12) 0.041(5) 0.002(6) -0.030(3) C30 0.088(2) 0.187(4) 0.618(10) 0.160(5) 0.130(4) -0.002(3) C31 0.290(3) 0.369(6) 0.449(4) 0.278(4) 0.326(2) 0.178(4) C32 0.372(4) 0.476(8) 0.214(3) 0.228(4) 0.239(2) 0.267(5) B3 0.0787(18) 0.0421(16) 0.0541(15) -0.0015(13) 0.0142(14) 0.0007(14) B4 0.0564(16) 0.076(2) 0.0586(16) -0.0189(15) 0.0054(14) -0.0024(16) B5 0.0531(15) 0.076(2) 0.0514(15) -0.0018(15) 0.0057(12) 0.0118(16) B6 0.0696(17) 0.0522(16) 0.0455(13) 0.0047(13) 0.0122(12) 0.0028(14) B7 0.0740(17) 0.0587(17) 0.0426(13) -0.0001(13) 0.0110(13) -0.0036(15) B8 0.0672(16) 0.0628(18) 0.0684(17) -0.0030(15) 0.0194(14) -0.0278(15) B9 0.0612(16) 0.076(2) 0.0612(16) -0.0112(16) 0.0139(14) -0.0087(16) B10 0.0710(17) 0.0583(18) 0.0563(15) -0.0020(14) 0.0165(13) 0.0082(15) B11 0.0639(14) 0.0500(15) 0.0395(12) -0.0088(12) 0.0145(11) -0.0027(14) B12 0.0614(15) 0.0676(19) 0.0487(14) -0.0054(14) 0.0171(12) -0.0081(15) O1 0.211(2) 0.333(4) 0.0912(16) 0.025(2) 0.0611(16) 0.174(2) O2 0.143(2) 0.1066(17) 0.198(3) -0.0698(17) -0.054(2) 0.0482(16) O3 0.1000(15) 0.1137(18) 0.236(3) 0.0677(18) 0.0567(17) 0.0108(15) O4 0.175(2) 0.201(3) 0.0758(13) 0.0331(16) 0.0369(14) 0.0991(19) O5 0.1055(18) 0.0967(18) 0.258(4) -0.039(2) -0.028(2) 0.0006(16) O6 0.1175(13) 0.238(2) 0.362(3) 0.208(2) 0.1561(14) 0.0846(16) O7 0.176(4) 0.171(4) 0.416(10) 0.034(5) 0.058(5) 0.092(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O6 2.725(3) . ? K1 O4 2.757(3) . ? K1 O7 2.7688(8) . ? K1 O2 2.806(3) . ? K1 O3 2.833(3) . ? K1 O1 2.838(3) . ? K1 O5 2.855(3) . ? K1 B10 3.407(3) . ? K1 B5 3.473(3) . ? K1 C32 3.489(5) . ? K1 C25 3.511(5) . ? C1 C2 1.445(3) . ? C1 C10 1.521(3) . ? C1 B6 1.524(4) . ? C1 B11 1.809(4) . ? C2 B3 1.521(4) . ? C2 C3 1.535(3) . ? C2 B7 1.821(4) . ? C3 C4 1.502(3) . ? C4 C9 1.377(3) . ? C4 C5 1.385(3) . ? C5 C6 1.398(4) . ? C6 C7 1.363(4) . ? C7 C8 1.383(3) . ? C8 C9 1.382(3) . ? C9 C10 1.504(3) . ? C21 O1 1.367(5) . ? C21 C22 1.524(7) . ? C22 O2 1.375(6) . ? C23 O2 1.363(5) . ? C23 C24 1.493(7) . ? C24 O3 1.385(5) . ? C25 O3 1.415(5) . ? C25 C26 1.477(6) . ? C26 O4 1.363(5) . ? C27 O4 1.398(5) . ? C27 C28 1.490(8) . ? C28 O5 1.374(6) . ? C29 O5 1.410(5) . ? C29 C30 1.522(8) . ? C30 O6 1.405(5) . ? C31 O6 1.419(6) . ? C31 C32 1.515(6) . ? C32 O1 1.390(6) . ? B3 B8 1.738(5) . ? B3 B7 1.821(4) . ? B3 B4 1.834(4) . ? B4 B8 1.735(4) . ? B4 B9 1.751(5) . ? B4 B5 1.817(5) . ? B5 B10 1.739(4) . ? B5 B9 1.752(5) . ? B5 B6 1.830(4) . ? B6 B10 1.736(5) . ? B6 B11 1.806(4) . ? B7 B12 1.728(4) . ? B7 B8 1.782(4) . ? B7 B11 1.913(4) . ? B8 B9 1.758(4) . ? B8 B12 1.770(4) . ? B9 B10 1.747(4) . ? B9 B12 1.806(4) . ? B10 B12 1.775(4) . ? B10 B11 1.782(4) . ? B11 B12 1.733(4) . ? O7 K1 2.7688(8) 3_575 ? 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 O6 K1 O4 120.59(10) . . ? O6 K1 O7 79.86(6) . . ? O4 K1 O7 84.85(6) . . ? O6 K1 O2 119.25(11) . . ? O4 K1 O2 117.61(10) . . ? O7 K1 O2 89.52(6) . . ? O6 K1 O3 163.96(8) . . ? O4 K1 O3 58.61(9) . . ? O7 K1 O3 84.15(5) . . ? O2 K1 O3 59.01(10) . . ? O6 K1 O1 60.91(11) . . ? O4 K1 O1 164.16(9) . . ? O7 K1 O1 79.91(7) . . ? O2 K1 O1 58.34(11) . . ? O3 K1 O1 115.04(10) . . ? O6 K1 O5 62.10(10) . . ? O4 K1 O5 58.95(10) . . ? O7 K1 O5 67.76(6) . . ? O2 K1 O5 156.99(8) . . ? O3 K1 O5 112.64(9) . . ? O1 K1 O5 117.86(10) . . ? O6 K1 B10 96.13(8) . . ? O4 K1 B10 113.37(8) . . ? O7 K1 B10 160.22(6) . . ? O2 K1 B10 75.45(8) . . ? O3 K1 B10 98.53(8) . . ? O1 K1 B10 81.24(8) . . ? O5 K1 B10 127.49(8) . . ? O6 K1 B5 103.79(8) . . ? O4 K1 B5 85.62(8) . . ? O7 K1 B5 170.34(5) . . ? O2 K1 B5 96.27(8) . . ? O3 K1 B5 92.20(8) . . ? O1 K1 B5 109.71(8) . . ? O5 K1 B5 105.77(8) . . ? B10 K1 B5 29.27(7) . . ? O6 K1 C32 43.07(11) . . ? O4 K1 C32 163.65(11) . . ? O7 K1 C32 90.41(9) . . ? O2 K1 C32 77.89(12) . . ? O3 K1 C32 136.51(12) . . ? O1 K1 C32 22.51(12) . . ? O5 K1 C32 104.80(12) . . ? B10 K1 C32 74.10(10) . . ? B5 K1 C32 98.34(11) . . ? O6 K1 C25 160.81(10) . . ? O4 K1 C25 40.22(9) . . ? O7 K1 C25 95.08(8) . . ? O2 K1 C25 78.91(11) . . ? O3 K1 C25 22.72(10) . . ? O1 K1 C25 136.83(11) . . ? O5 K1 C25 98.80(11) . . ? B10 K1 C25 94.56(9) . . ? B5 K1 C25 78.54(9) . . ? C32 K1 C25 156.10(12) . . ? C2 C1 C10 115.76(19) . . ? C2 C1 B6 127.9(2) . . ? C10 C1 B6 116.1(2) . . ? C2 C1 B11 97.74(18) . . ? C10 C1 B11 114.78(17) . . ? B6 C1 B11 64.95(16) . . ? C1 C2 B3 128.6(2) . . ? C1 C2 C3 115.28(19) . . ? B3 C2 C3 115.8(2) . . ? C1 C2 B7 97.06(18) . . ? B3 C2 B7 65.32(17) . . ? C3 C2 B7 115.69(18) . . ? C4 C3 C2 113.3(2) . . ? C9 C4 C5 120.0(2) . . ? C9 C4 C3 117.71(19) . . ? C5 C4 C3 122.2(2) . . ? C4 C5 C6 119.7(3) . . ? C7 C6 C5 119.6(2) . . ? C6 C7 C8 120.8(2) . . ? C9 C8 C7 119.8(3) . . ? C4 C9 C8 120.0(2) . . ? C4 C9 C10 117.18(19) . . ? C8 C9 C10 122.8(2) . . ? C9 C10 C1 113.5(2) . . ? O1 C21 C22 108.7(3) . . ? O2 C22 C21 108.1(4) . . ? O2 C23 C24 107.3(3) . . ? O3 C24 C23 108.8(4) . . ? O3 C25 C26 107.6(4) . . ? O3 C25 K1 50.62(18) . . ? C26 C25 K1 83.1(3) . . ? O4 C26 C25 105.9(3) . . ? O4 C27 C28 110.2(4) . . ? O5 C28 C27 104.6(4) . . ? O5 C29 C30 113.4(4) . . ? O6 C30 C29 109.1(4) . . ? O6 C31 C32 109.0(4) . . ? O1 C32 C31 111.3(4) . . ? O1 C32 K1 51.4(2) . . ? C31 C32 K1 83.5(3) . . ? C2 B3 B8 118.7(2) . . ? C2 B3 B7 65.30(17) . . ? B8 B3 B7 60.02(17) . . ? C2 B3 B4 115.5(2) . . ? B8 B3 B4 58.04(17) . . ? B7 B3 B4 104.1(2) . . ? B8 B4 B9 60.57(18) . . ? B8 B4 B5 107.7(2) . . ? B9 B4 B5 58.77(18) . . ? B8 B4 B3 58.21(17) . . ? B9 B4 B3 110.2(2) . . ? B5 B4 B3 114.47(19) . . ? B10 B5 B9 60.06(18) . . ? B10 B5 B4 107.3(2) . . ? B9 B5 B4 58.73(18) . . ? B10 B5 B6 58.12(17) . . ? B9 B5 B6 109.60(19) . . ? B4 B5 B6 114.33(19) . . ? B10 B5 K1 73.27(14) . . ? B9 B5 K1 83.41(15) . . ? B4 B5 K1 130.61(16) . . ? B6 B5 K1 107.27(15) . . ? C1 B6 B10 119.1(2) . . ? C1 B6 B11 65.17(16) . . ? B10 B6 B11 60.38(16) . . ? C1 B6 B5 116.0(2) . . ? B10 B6 B5 58.32(16) . . ? B11 B6 B5 104.7(2) . . ? B12 B7 B8 60.53(17) . . ? B12 B7 C2 123.1(2) . . ? B8 B7 C2 102.32(18) . . ? B12 B7 B3 109.09(19) . . ? B8 B7 B3 57.68(17) . . ? C2 B7 B3 49.38(14) . . ? B12 B7 B11 56.57(16) . . ? B8 B7 B11 105.37(19) . . ? C2 B7 B11 82.50(17) . . ? B3 B7 B11 112.81(18) . . ? B4 B8 B3 63.75(18) . . ? B4 B8 B9 60.18(18) . . ? B3 B8 B9 114.5(2) . . ? B4 B8 B12 108.5(2) . . ? B3 B8 B12 111.1(2) . . ? B9 B8 B12 61.60(17) . . ? B4 B8 B7 110.1(2) . . ? B3 B8 B7 62.30(17) . . ? B9 B8 B7 109.7(2) . . ? B12 B8 B7 58.24(16) . . ? B10 B9 B4 110.0(2) . . ? B10 B9 B5 59.62(18) . . ? B4 B9 B5 62.49(19) . . ? B10 B9 B8 109.5(2) . . ? B4 B9 B8 59.26(18) . . ? B5 B9 B8 109.7(2) . . ? B10 B9 B12 59.93(16) . . ? B4 B9 B12 106.1(2) . . ? B5 B9 B12 106.5(2) . . ? B8 B9 B12 59.52(17) . . ? B6 B10 B5 63.56(17) . . ? B6 B10 B9 114.4(2) . . ? B5 B10 B9 60.33(18) . . ? B6 B10 B12 110.6(2) . . ? B5 B10 B12 108.4(2) . . ? B9 B10 B12 61.69(17) . . ? B6 B10 B11 61.76(16) . . ? B5 B10 B11 109.7(2) . . ? B9 B10 B11 109.8(2) . . ? B12 B10 B11 58.31(16) . . ? B6 B10 K1 112.69(15) . . ? B5 B10 K1 77.46(13) . . ? B9 B10 K1 85.53(14) . . ? B12 B10 K1 133.60(18) . . ? B11 B10 K1 164.66(17) . . ? B12 B11 B10 60.66(16) . . ? B12 B11 B6 109.28(18) . . ? B10 B11 B6 57.86(16) . . ? B12 B11 C1 123.38(19) . . ? B10 B11 C1 103.07(17) . . ? B6 B11 C1 49.88(14) . . ? B12 B11 B7 56.33(16) . . ? B10 B11 B7 105.57(18) . . ? B6 B11 B7 113.22(18) . . ? C1 B11 B7 82.69(16) . . ? B7 B12 B11 67.09(17) . . ? B7 B12 B8 61.23(17) . . ? B11 B12 B8 114.1(2) . . ? B7 B12 B10 114.3(2) . . ? B11 B12 B10 61.03(17) . . ? B8 B12 B10 107.7(2) . . ? B7 B12 B9 109.9(2) . . ? B11 B12 B9 109.3(2) . . ? B8 B12 B9 58.89(16) . . ? B10 B12 B9 58.39(16) . . ? C21 O1 C32 111.2(3) . . ? C21 O1 K1 113.6(3) . . ? C32 O1 K1 106.1(3) . . ? C23 O2 C22 111.0(3) . . ? C23 O2 K1 116.7(3) . . ? C22 O2 K1 119.3(3) . . ? C24 O3 C25 114.5(3) . . ? C24 O3 K1 111.1(3) . . ? C25 O3 K1 106.7(2) . . ? C26 O4 C27 110.3(3) . . ? C26 O4 K1 120.5(2) . . ? C27 O4 K1 116.1(2) . . ? C28 O5 C29 112.0(4) . . ? C28 O5 K1 112.4(3) . . ? C29 O5 K1 108.0(3) . . ? C30 O6 C31 114.0(4) . . ? C30 O6 K1 118.8(3) . . ? C31 O6 K1 119.7(3) . . ? K1 O7 K1 180.0 . 3_575 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.275 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.053 #===END data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H43 B10 K O6' _chemical_formula_weight 550.76 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9528(10) _cell_length_b 18.667(2) _cell_length_c 18.642(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.116(2) _cell_angle_gamma 90.00 _cell_volume 3056.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.87 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.51 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.7498 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Smart CCD 1000' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14719 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4787 _reflns_number_gt 3350 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SHELXTL' _computing_cell_refinement 'Siemens SHELXTL' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0876P)^2^+1.8160P] 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 4787 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1887 _refine_ls_wR_factor_gt 0.1711 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.121 _refine_ls_shift/su_mean 0.013 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 K1 K 0.5000 -0.5000 0.5000 0.07247(13) Uani 1 2 d S . . O1 O 0.38625(11) -0.47782(5) 0.35439(5) 0.0757(3) Uani 1 1 d . . . O2 O 0.66437(10) -0.39218(5) 0.58189(5) 0.0793(3) Uani 1 1 d . . . O3 O 0.69880(10) 0.07054(5) 0.61549(5) 0.0771(3) Uani 1 1 d . . . O4 O 0.39937(11) 0.11883(5) 0.56957(5) 0.0800(3) Uani 1 1 d . . . O5 O 0.19157(10) 0.02971(5) 0.47431(5) 0.0758(3) Uani 1 1 d . . . O6 O 0.59508(10) -0.38001(5) 0.43060(5) 0.0725(3) Uani 1 1 d . . . C1 C 0.30042(18) -0.24625(7) 0.69914(7) 0.0759(5) Uani 1 1 d . . . C2 C 0.2825(2) -0.20547(7) 0.62793(8) 0.0873(6) Uani 1 1 d . . . C3 C 0.1632(2) -0.23508(8) 0.56578(8) 0.0886(6) Uani 1 1 d . . . H3A H 0.0630 -0.2207 0.5729 0.106 Uiso 1 1 calc R . . H3B H 0.1791 -0.2147 0.5200 0.106 Uiso 1 1 calc R . . C4 C 0.16909(15) -0.31502(8) 0.56115(7) 0.0699(4) Uani 1 1 d . . . C5 C 0.15537(17) -0.35093(10) 0.49570(9) 0.0954(6) Uani 1 1 d . . . H5A H 0.1453 -0.3252 0.4523 0.115 Uiso 1 1 calc R . . C6 C 0.1565(2) -0.42493(11) 0.49410(12) 0.1270(7) Uani 1 1 d . . . H6A H 0.1449 -0.4489 0.4496 0.152 Uiso 1 1 calc R . . C7 C 0.1743(2) -0.46199(10) 0.55658(15) 0.1340(9) Uani 1 1 d . . . H7A H 0.1776 -0.5118 0.5551 0.161 Uiso 1 1 calc R . . C8 C 0.18791(17) -0.42797(9) 0.62303(12) 0.1026(6) Uani 1 1 d . . . H8B H 0.1982 -0.4546 0.6659 0.123 Uiso 1 1 calc R . . C9 C 0.18611(15) -0.35325(8) 0.62577(8) 0.0718(4) Uani 1 1 d . . . C10 C 0.19669(18) -0.31186(9) 0.69534(8) 0.0897(5) Uani 1 1 d . . . H10A H 0.2350 -0.3431 0.7363 0.108 Uiso 1 1 calc R . . H10B H 0.0955 -0.2963 0.6999 0.108 Uiso 1 1 calc R . . C31 C 0.75290(18) -0.41358(9) 0.64967(8) 0.0870(5) Uani 1 1 d . . . H31A H 0.7880 -0.3718 0.6791 0.104 Uiso 1 1 calc R . . H31B H 0.8412 -0.4404 0.6418 0.104 Uiso 1 1 calc R . . C32 C 0.74008(19) -0.34277(8) 0.54380(9) 0.0927(6) Uani 1 1 d . . . H32A H 0.8298 -0.3649 0.5315 0.111 Uiso 1 1 calc R . . H32B H 0.7722 -0.3014 0.5744 0.111 Uiso 1 1 calc R . . C33 C 0.6345(2) -0.31993(8) 0.47589(9) 0.0950(6) Uani 1 1 d . . . H33A H 0.5436 -0.2988 0.4881 0.114 Uiso 1 1 calc R . . H33B H 0.6834 -0.2842 0.4505 0.114 Uiso 1 1 calc R . . C35 C 0.49482(17) -0.36220(8) 0.36371(8) 0.0802(5) Uani 1 1 d . . . H35A H 0.5411 -0.3258 0.3379 0.096 Uiso 1 1 calc R . . H35B H 0.4003 -0.3432 0.3739 0.096 Uiso 1 1 calc R . . C36 C 0.46360(18) -0.42730(9) 0.31789(7) 0.0822(5) Uani 1 1 d . . . H36A H 0.4014 -0.4151 0.2709 0.099 Uiso 1 1 calc R . . H36B H 0.5585 -0.4476 0.3095 0.099 Uiso 1 1 calc R . . C37 C 0.3441(2) -0.54068(9) 0.31197(8) 0.0897(6) Uani 1 1 d . . . H37A H 0.4345 -0.5669 0.3060 0.108 Uiso 1 1 calc R . . H37B H 0.2881 -0.5277 0.2639 0.108 Uiso 1 1 calc R . . C41 C 0.85094(17) 0.06810(10) 0.60916(9) 0.0903(6) Uani 1 1 d . . . H41A H 0.9148 0.0856 0.6537 0.108 Uiso 1 1 calc R . . H41B H 0.8672 0.0982 0.5690 0.108 Uiso 1 1 calc R . . C42 C 0.6482(2) 0.13960(8) 0.63248(8) 0.0899(6) Uani 1 1 d . . . H42A H 0.6601 0.1733 0.5944 0.108 Uiso 1 1 calc R . . H42B H 0.7086 0.1563 0.6783 0.108 Uiso 1 1 calc R . . C43 C 0.48559(19) 0.13509(9) 0.63849(8) 0.0920(5) Uani 1 1 d . . . H43A H 0.4721 0.0981 0.6733 0.110 Uiso 1 1 calc R . . H43B H 0.4525 0.1804 0.6556 0.110 Uiso 1 1 calc R . . C44 C 0.24041(16) 0.11646(9) 0.56813(9) 0.0975(5) Uani 1 1 d . . . H44A H 0.2059 0.1623 0.5832 0.117 Uiso 1 1 calc R . . H44B H 0.2179 0.0800 0.6016 0.117 Uiso 1 1 calc R . . C45 C 0.16109(17) 0.09963(9) 0.49262(9) 0.0929(5) Uani 1 1 d . . . H45A H 0.0523 0.1057 0.4889 0.111 Uiso 1 1 calc R . . H45B H 0.1945 0.1325 0.4586 0.111 Uiso 1 1 calc R . . C46 C 0.10947(16) 0.00630(10) 0.40412(8) 0.0904(6) Uani 1 1 d . . . H46A H 0.1346 0.0369 0.3661 0.108 Uiso 1 1 calc R . . H46B H 0.0009 0.0100 0.4027 0.108 Uiso 1 1 calc R . . B9 B 0.5445(2) -0.1597(2) 0.76729(12) 0.2304(16) Uani 1 1 d . . . H9 H 0.6285 -0.1612 0.8188 0.277 Uiso 1 1 calc R . . B4 B 0.5996(2) -0.19326(14) 0.69335(12) 0.1038(8) Uani 1 1 d . . . H4 H 0.7210(17) -0.2005(9) 0.6880(8) 0.108(5) Uiso 1 1 d . . . B8 B 0.5123(3) -0.11082(11) 0.66955(13) 0.1118(7) Uani 1 1 d . . . H8 H 0.5849(19) -0.0697(10) 0.6583(9) 0.131(6) Uiso 1 1 d . . . B12 B 0.3751(3) -0.09134(13) 0.72090(14) 0.1201(9) Uani 1 1 d . . . H12 H 0.340(3) -0.0326(13) 0.7270(12) 0.180(9) Uiso 1 1 d . . . B11 B 0.3951(5) -0.1380(3) 0.7855(3) 0.253(2) Uani 1 1 d . . . H11 H 0.4061 -0.1165 0.8412 0.304 Uiso 1 1 calc R . . B10 B 0.3579(3) -0.2072(2) 0.77219(11) 0.1728(16) Uani 1 1 d . . . H10 H 0.3583 -0.2224 0.8292 0.207 Uiso 1 1 calc R . . B5 B 0.4823(2) -0.25088(11) 0.73233(16) 0.1154(9) Uani 1 1 d . . . H5 H 0.501(3) -0.3139(15) 0.7507(16) 0.241(12) Uiso 1 1 d . . . H1 H 0.4899(12) -0.2526(5) 0.6683(6) 0.049(3) Uiso 1 1 d . . . B3 B 0.4552(2) -0.18372(12) 0.61490(11) 0.0995(7) Uani 1 1 d . . . H3 H 0.487(2) -0.1842(10) 0.5581(10) 0.137(6) Uiso 1 1 d . . . B7 B 0.3229(3) -0.11973(10) 0.63206(11) 0.0979(7) Uani 1 1 d . . . H7 H 0.259(2) -0.0829(11) 0.5800(10) 0.147(7) Uiso 1 1 d . . . B6 B 0.2332(4) -0.1555(2) 0.69562(18) 0.1674(15) Uani 1 1 d . . . K2 K 0.5000 0.0000 0.5000 0.09001(16) Uani 1 2 d S . . H6 H 0.063(3) -0.1551(14) 0.6840(14) 0.213(10) 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 K1 0.0732(2) 0.0846(3) 0.0551(2) 0.0058(2) 0.00122(18) -0.0269(2) O1 0.0852(6) 0.0858(6) 0.0534(5) -0.0001(5) 0.0064(4) -0.0100(5) O2 0.0778(6) 0.0899(6) 0.0666(5) -0.0039(5) 0.0049(4) -0.0224(5) O3 0.0735(5) 0.0863(6) 0.0720(5) 0.0038(5) 0.0151(4) -0.0182(5) O4 0.0953(6) 0.0756(6) 0.0779(5) -0.0027(5) 0.0386(4) 0.0022(5) O5 0.0620(5) 0.0835(6) 0.0826(5) 0.0211(5) 0.0159(4) 0.0177(5) O6 0.0811(5) 0.0656(5) 0.0708(5) 0.0038(4) 0.0144(4) -0.0057(5) C1 0.1073(10) 0.0686(8) 0.0525(6) 0.0091(6) 0.0174(7) 0.0175(8) C2 0.1377(13) 0.0520(8) 0.0604(8) 0.0037(7) -0.0107(8) 0.0115(8) C3 0.1170(12) 0.0758(9) 0.0626(8) 0.0091(7) -0.0085(8) 0.0034(9) C4 0.0647(7) 0.0734(8) 0.0725(8) -0.0044(7) 0.0154(6) -0.0072(7) C5 0.0832(9) 0.1142(12) 0.0911(9) -0.0325(9) 0.0222(8) -0.0245(9) C6 0.0940(11) 0.1238(13) 0.1665(15) -0.0745(11) 0.0334(11) -0.0159(10) C7 0.0866(11) 0.0762(11) 0.234(2) -0.0397(14) 0.0171(14) -0.0117(9) C8 0.0734(9) 0.0795(10) 0.1515(15) 0.0277(10) 0.0133(10) -0.0117(8) C9 0.0597(7) 0.0674(8) 0.0891(8) 0.0134(7) 0.0164(6) -0.0057(6) C10 0.0890(9) 0.1102(11) 0.0734(8) 0.0309(8) 0.0246(7) -0.0051(9) C31 0.0874(9) 0.0961(10) 0.0695(8) -0.0170(8) -0.0050(7) -0.0192(8) C32 0.1040(10) 0.0795(9) 0.0939(10) -0.0132(8) 0.0169(8) -0.0379(8) C33 0.1252(12) 0.0667(9) 0.0925(10) -0.0024(8) 0.0195(9) -0.0193(9) C35 0.0865(9) 0.0777(9) 0.0769(8) 0.0202(7) 0.0169(7) 0.0020(8) C36 0.0870(9) 0.1008(11) 0.0586(7) 0.0151(8) 0.0138(7) -0.0015(9) C37 0.1096(11) 0.0974(11) 0.0567(8) -0.0121(8) 0.0027(8) -0.0062(10) C41 0.0756(9) 0.1129(12) 0.0788(9) 0.0118(9) 0.0055(7) -0.0193(9) C42 0.1336(12) 0.0663(8) 0.0681(8) -0.0096(7) 0.0153(8) -0.0183(9) C43 0.1303(11) 0.0724(9) 0.0838(8) -0.0093(8) 0.0467(8) -0.0027(9) C44 0.0953(8) 0.0816(10) 0.1340(11) -0.0011(9) 0.0681(7) 0.0154(8) C45 0.0729(8) 0.0946(10) 0.1195(11) 0.0282(9) 0.0393(7) 0.0265(8) C46 0.0501(7) 0.1401(13) 0.0765(8) 0.0347(9) 0.0009(7) -0.0002(8) B9 0.0439(9) 0.539(5) 0.1014(11) -0.1600(17) -0.0040(9) 0.0165(18) B4 0.0688(10) 0.1311(17) 0.1119(14) 0.0064(13) 0.0189(10) -0.0203(11) B8 0.1346(13) 0.0761(11) 0.1409(15) -0.0155(11) 0.0667(11) -0.0405(10) B12 0.1330(17) 0.1023(14) 0.1255(15) -0.0495(12) 0.0265(13) -0.0119(13) B11 0.226(4) 0.282(5) 0.213(4) -0.051(4) -0.054(3) 0.082(4) B10 0.1014(14) 0.364(4) 0.0585(10) -0.0443(18) 0.0284(10) -0.020(2) B5 0.0724(11) 0.0955(13) 0.174(2) 0.0476(13) 0.0144(13) 0.0158(10) B3 0.0966(13) 0.1110(15) 0.0894(11) -0.0269(11) 0.0142(10) 0.0060(12) B7 0.1334(15) 0.0690(10) 0.0955(11) 0.0249(9) 0.0327(11) 0.0285(10) B6 0.130(2) 0.232(4) 0.147(2) 0.012(2) 0.0435(17) 0.004(2) K2 0.0537(2) 0.1101(3) 0.1033(3) -0.0451(3) 0.0079(2) 0.0119(2) _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 K1 O1 2.7406(9) . ? K1 O1 2.7406(9) 3_646 ? K1 O2 2.7714(10) . ? K1 O2 2.7714(9) 3_646 ? K1 O6 2.7999(10) . ? K1 O6 2.7999(10) 3_646 ? K1 C6 3.3619(19) . ? K1 C6 3.3619(19) 3_646 ? K1 C7 3.362(2) 3_646 ? K1 C7 3.362(2) . ? O1 C36 1.4191(19) . ? O1 C37 1.4245(18) . ? O2 C31 1.4136(17) . ? O2 C32 1.4141(19) . ? O3 C41 1.3905(18) . ? O3 C42 1.4221(19) . ? O3 K2 2.8389(9) . ? O4 C43 1.3988(17) . ? O4 C44 1.4188(18) . ? O4 K2 2.8044(10) . ? O5 C45 1.3893(19) . ? O5 C46 1.4396(17) . ? O5 K2 2.7662(9) . ? O6 C33 1.4073(18) . ? O6 C35 1.4281(16) . ? C1 C2 1.5118(19) . ? C1 C10 1.530(2) . ? C1 B10 1.543(3) . ? C1 B5 1.629(3) . ? C1 B6 1.795(4) . ? C2 C3 1.520(2) . ? C2 B7 1.639(2) . ? C2 B3 1.661(3) . ? C2 B6 1.695(4) . ? C3 C4 1.496(2) . ? C4 C5 1.377(2) . ? C4 C9 1.383(2) . ? C5 C6 1.382(3) . ? C6 C7 1.337(3) . ? C7 C8 1.376(3) . ? C8 C9 1.396(2) . ? C9 C10 1.497(2) . ? C31 C37 1.495(2) 3_646 ? C32 C33 1.489(2) . ? C35 C36 1.481(2) . ? C37 C31 1.495(2) 3_646 ? C41 C46 1.466(3) 3_656 ? C42 C43 1.484(2) . ? C44 C45 1.483(2) . ? C45 K2 3.5388(16) . ? C46 C41 1.466(3) 3_656 ? B9 B11 1.498(6) . ? B9 B4 1.672(3) . ? B9 B5 1.868(4) . ? B9 B8 2.008(4) . ? B9 B12 2.042(4) . ? B4 B8 1.744(3) . ? B4 B5 1.755(3) . ? B4 B3 1.764(3) . ? B8 B7 1.713(3) . ? B8 B3 1.718(3) . ? B8 B12 1.735(4) . ? B12 B11 1.469(6) . ? B12 B7 1.716(3) . ? B12 B6 1.744(4) . ? B11 B10 1.344(7) . ? B11 B6 2.020(6) . ? B10 B5 1.666(4) . ? B10 B6 1.898(5) . ? B3 B7 1.755(3) . ? B7 B6 1.692(4) . ? K2 O5 2.7662(9) 3_656 ? K2 O4 2.8044(10) 3_656 ? K2 O3 2.8389(9) 3_656 ? K2 C45 3.5388(16) 3_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 K1 O1 180.0 . 3_646 ? O1 K1 O2 119.49(3) . . ? O1 K1 O2 60.51(3) 3_646 . ? O1 K1 O2 60.51(3) . 3_646 ? O1 K1 O2 119.49(3) 3_646 3_646 ? O2 K1 O2 180.0 . 3_646 ? O1 K1 O6 60.63(3) . . ? O1 K1 O6 119.37(3) 3_646 . ? O2 K1 O6 59.81(3) . . ? O2 K1 O6 120.19(3) 3_646 . ? O1 K1 O6 119.37(3) . 3_646 ? O1 K1 O6 60.63(3) 3_646 3_646 ? O2 K1 O6 120.19(3) . 3_646 ? O2 K1 O6 59.81(3) 3_646 3_646 ? O6 K1 O6 180.0 . 3_646 ? O1 K1 C6 75.03(4) . . ? O1 K1 C6 104.97(4) 3_646 . ? O2 K1 C6 95.77(4) . . ? O2 K1 C6 84.23(4) 3_646 . ? O6 K1 C6 90.52(4) . . ? O6 K1 C6 89.48(4) 3_646 . ? O1 K1 C6 104.97(4) . 3_646 ? O1 K1 C6 75.03(4) 3_646 3_646 ? O2 K1 C6 84.23(4) . 3_646 ? O2 K1 C6 95.77(4) 3_646 3_646 ? O6 K1 C6 89.48(4) . 3_646 ? O6 K1 C6 90.52(4) 3_646 3_646 ? C6 K1 C6 180.0 . 3_646 ? O1 K1 C7 84.28(5) . 3_646 ? O1 K1 C7 95.72(5) 3_646 3_646 ? O2 K1 C7 85.73(4) . 3_646 ? O2 K1 C7 94.27(4) 3_646 3_646 ? O6 K1 C7 70.40(4) . 3_646 ? O6 K1 C7 109.60(4) 3_646 3_646 ? C6 K1 C7 157.05(6) . 3_646 ? C6 K1 C7 22.95(6) 3_646 3_646 ? O1 K1 C7 95.72(5) . . ? O1 K1 C7 84.28(5) 3_646 . ? O2 K1 C7 94.27(4) . . ? O2 K1 C7 85.73(4) 3_646 . ? O6 K1 C7 109.60(4) . . ? O6 K1 C7 70.40(4) 3_646 . ? C6 K1 C7 22.95(6) . . ? C6 K1 C7 157.05(6) 3_646 . ? C7 K1 C7 180.0 3_646 . ? C36 O1 C37 112.51(11) . . ? C36 O1 K1 116.92(7) . . ? C37 O1 K1 115.69(8) . . ? C31 O2 C32 113.12(11) . . ? C31 O2 K1 115.71(9) . . ? C32 O2 K1 116.88(8) . . ? C41 O3 C42 114.09(12) . . ? C41 O3 K2 113.67(8) . . ? C42 O3 K2 114.15(8) . . ? C43 O4 C44 113.45(12) . . ? C43 O4 K2 115.26(9) . . ? C44 O4 K2 112.16(8) . . ? C45 O5 C46 114.73(11) . . ? C45 O5 K2 112.50(8) . . ? C46 O5 K2 114.47(8) . . ? C33 O6 C35 112.40(11) . . ? C33 O6 K1 115.07(9) . . ? C35 O6 K1 113.19(8) . . ? C2 C1 C10 113.68(11) . . ? C2 C1 B10 119.86(18) . . ? C10 C1 B10 121.00(17) . . ? C2 C1 B5 106.82(15) . . ? C10 C1 B5 121.90(13) . . ? B10 C1 B5 63.31(15) . . ? C2 C1 B6 60.95(13) . . ? C10 C1 B6 123.87(16) . . ? B10 C1 B6 68.82(19) . . ? B5 C1 B6 111.57(15) . . ? C1 C2 C3 115.22(13) . . ? C1 C2 B7 117.73(12) . . ? C3 C2 B7 120.47(13) . . ? C1 C2 B3 107.89(13) . . ? C3 C2 B3 120.95(14) . . ? B7 C2 B3 64.23(13) . . ? C1 C2 B6 67.80(16) . . ? C3 C2 B6 121.47(17) . . ? B7 C2 B6 60.95(17) . . ? B3 C2 B6 110.97(16) . . ? C4 C3 C2 112.30(12) . . ? C5 C4 C9 119.78(14) . . ? C5 C4 C3 122.59(13) . . ? C9 C4 C3 117.62(13) . . ? C4 C5 C6 120.41(17) . . ? C7 C6 C5 119.9(2) . . ? C7 C6 K1 78.53(12) . . ? C5 C6 K1 115.25(11) . . ? C6 C7 C8 121.34(18) . . ? C6 C7 K1 78.52(13) . . ? C8 C7 K1 116.63(11) . . ? C7 C8 C9 119.62(18) . . ? C4 C9 C8 118.93(15) . . ? C4 C9 C10 117.79(13) . . ? C8 C9 C10 123.24(15) . . ? C9 C10 C1 112.93(13) . . ? O2 C31 C37 108.16(12) . 3_646 ? O2 C32 C33 109.06(13) . . ? O6 C33 C32 109.06(12) . . ? O6 C35 C36 109.24(12) . . ? O1 C36 C35 108.91(12) . . ? O1 C37 C31 108.74(12) . 3_646 ? O3 C41 C46 108.55(13) . 3_656 ? O3 C42 C43 108.95(13) . . ? O4 C43 C42 108.58(13) . . ? O4 C44 C45 108.63(13) . . ? O5 C45 C44 110.58(13) . . ? O5 C45 K2 46.24(6) . . ? C44 C45 K2 79.88(8) . . ? O5 C46 C41 110.08(12) . 3_656 ? B11 B9 B4 134.9(2) . . ? B11 B9 B5 96.1(3) . . ? B4 B9 B5 59.13(16) . . ? B11 B9 B8 96.0(3) . . ? B4 B9 B8 55.66(13) . . ? B5 B9 B8 96.69(15) . . ? B11 B9 B12 45.9(2) . . ? B4 B9 B12 101.41(15) . . ? B5 B9 B12 105.94(13) . . ? B8 B9 B12 50.73(13) . . ? B9 B4 B8 71.98(18) . . ? B9 B4 B5 66.01(18) . . ? B8 B4 B5 111.83(15) . . ? B9 B4 B3 111.11(16) . . ? B8 B4 B3 58.63(12) . . ? B5 B4 B3 90.23(14) . . ? B7 B8 B3 61.51(12) . . ? B7 B8 B12 59.67(13) . . ? B3 B8 B12 109.38(16) . . ? B7 B8 B4 112.20(15) . . ? B3 B8 B4 61.28(12) . . ? B12 B8 B4 112.00(17) . . ? B7 B8 B9 106.47(15) . . ? B3 B8 B9 98.76(16) . . ? B12 B8 B9 65.65(14) . . ? B4 B8 B9 52.36(14) . . ? B11 B12 B7 125.1(3) . . ? B11 B12 B8 109.9(3) . . ? B7 B12 B8 59.53(14) . . ? B11 B12 B6 77.4(3) . . ? B7 B12 B6 58.54(16) . . ? B8 B12 B6 105.28(19) . . ? B11 B12 B9 47.1(2) . . ? B7 B12 B9 104.93(16) . . ? B8 B12 B9 63.63(13) . . ? B6 B12 B9 97.37(19) . . ? B10 B11 B12 115.6(4) . . ? B10 B11 B9 84.2(3) . . ? B12 B11 B9 87.0(3) . . ? B10 B11 B6 65.1(2) . . ? B12 B11 B6 57.4(2) . . ? B9 B11 B6 107.3(3) . . ? B11 B10 C1 130.2(3) . . ? B11 B10 B5 112.9(3) . . ? C1 B10 B5 60.86(15) . . ? B11 B10 B6 74.9(3) . . ? C1 B10 B6 61.88(15) . . ? B5 B10 B6 105.10(18) . . ? C1 B5 B10 55.83(12) . . ? C1 B5 B4 116.37(16) . . ? B10 B5 B4 112.9(2) . . ? C1 B5 B9 107.04(14) . . ? B10 B5 B9 65.07(17) . . ? B4 B5 B9 54.86(13) . . ? C2 B3 B8 106.62(16) . . ? C2 B3 B7 57.28(11) . . ? B8 B3 B7 59.12(13) . . ? C2 B3 B4 114.08(15) . . ? B8 B3 B4 60.09(13) . . ? B7 B3 B4 109.27(15) . . ? C2 B7 B6 61.14(17) . . ? C2 B7 B8 107.81(14) . . ? B6 B7 B8 108.60(17) . . ? C2 B7 B12 111.32(15) . . ? B6 B7 B12 61.56(17) . . ? B8 B7 B12 60.80(14) . . ? C2 B7 B3 58.49(12) . . ? B6 B7 B3 106.71(19) . . ? B8 B7 B3 59.36(12) . . ? B12 B7 B3 108.56(15) . . ? B7 B6 C2 57.90(14) . . ? B7 B6 B12 59.90(17) . . ? C2 B6 B12 107.4(2) . . ? B7 B6 C1 101.4(2) . . ? C2 B6 C1 51.24(13) . . ? B12 B6 C1 114.6(2) . . ? B7 B6 B10 115.9(2) . . ? C2 B6 B10 94.6(2) . . ? B12 B6 B10 81.56(19) . . ? C1 B6 B10 49.30(16) . . ? B7 B6 B11 98.9(2) . . ? C2 B6 B11 117.3(2) . . ? B12 B6 B11 45.22(19) . . ? C1 B6 B11 86.6(2) . . ? B10 B6 B11 40.0(2) . . ? O5 K2 O5 180.0 3_656 . ? O5 K2 O4 61.48(3) 3_656 3_656 ? O5 K2 O4 118.52(3) . 3_656 ? O5 K2 O4 118.52(3) 3_656 . ? O5 K2 O4 61.48(3) . . ? O4 K2 O4 180.00(3) 3_656 . ? O5 K2 O3 60.18(3) 3_656 . ? O5 K2 O3 119.82(3) . . ? O4 K2 O3 120.48(3) 3_656 . ? O4 K2 O3 59.52(3) . . ? O5 K2 O3 119.82(3) 3_656 3_656 ? O5 K2 O3 60.18(3) . 3_656 ? O4 K2 O3 59.52(3) 3_656 3_656 ? O4 K2 O3 120.48(3) . 3_656 ? O3 K2 O3 180.0 . 3_656 ? O5 K2 C45 158.73(3) 3_656 . ? O5 K2 C45 21.27(3) . . ? O4 K2 C45 138.35(3) 3_656 . ? O4 K2 C45 41.65(3) . . ? O3 K2 C45 101.14(3) . . ? O3 K2 C45 78.86(3) 3_656 . ? O5 K2 C45 21.27(3) 3_656 3_656 ? O5 K2 C45 158.73(3) . 3_656 ? O4 K2 C45 41.65(3) 3_656 3_656 ? O4 K2 C45 138.35(3) . 3_656 ? O3 K2 C45 78.86(3) . 3_656 ? O3 K2 C45 101.14(3) 3_656 3_656 ? C45 K2 C45 180.00(6) . 3_656 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.534 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.040 #===END data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H53 B10 K O7' _chemical_formula_weight 672.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9624(8) _cell_length_b 19.3838(12) _cell_length_c 15.6977(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.065(2) _cell_angle_gamma 90.00 _cell_volume 3808.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.181 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8205 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20547 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6708 _reflns_number_gt 2999 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0876P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6708 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1477 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1840 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.006 _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 K1 K 0.22124(7) 0.60904(4) 0.73827(5) 0.0643(3) Uani 1 1 d . . . O1 O 0.1890(3) 0.58895(14) 0.90715(17) 0.0758(8) Uani 1 1 d . . . O2 O 0.0150(2) 0.57628(14) 0.75940(19) 0.0743(8) Uani 1 1 d . . . O3 O 0.0592(2) 0.57518(14) 0.59153(17) 0.0788(8) Uani 1 1 d . . . O4 O 0.2420(3) 0.64316(16) 0.5669(2) 0.0953(10) Uani 1 1 d . . . O5 O 0.4124(3) 0.65558(15) 0.7188(2) 0.0939(10) Uani 1 1 d . . . O6 O 0.3740(3) 0.65621(15) 0.8862(2) 0.0853(9) Uani 1 1 d . . . O7 O 0.1435(6) 0.7427(2) 0.7265(5) 0.196(3) Uani 1 1 d . . . C1 C 0.2714(3) 0.27608(16) 0.7924(2) 0.0518(9) Uani 1 1 d . . . C2 C 0.2325(3) 0.27759(17) 0.6977(2) 0.0543(9) Uani 1 1 d . . . C3 C 0.2282(4) 0.2177(2) 0.8390(3) 0.0620(11) Uani 1 1 d . . . C4 C 0.2729(3) 0.14826(18) 0.8262(2) 0.0548(10) Uani 1 1 d . . . C5 C 0.3246(4) 0.1113(3) 0.8999(3) 0.0732(12) Uani 1 1 d . . . C6 C 0.3701(4) 0.0466(3) 0.8943(4) 0.0899(16) Uani 1 1 d . . . C7 C 0.3670(4) 0.0194(3) 0.8149(4) 0.0858(14) Uani 1 1 d . . . C8 C 0.3154(3) 0.0537(2) 0.7371(3) 0.0700(12) Uani 1 1 d . . . C9 C 0.3130(5) 0.0248(3) 0.6535(4) 0.0881(16) Uani 1 1 d . . . C10 C 0.2638(5) 0.0570(3) 0.5793(4) 0.0928(17) Uani 1 1 d . . . C11 C 0.2137(4) 0.1208(3) 0.5816(3) 0.0759(13) Uani 1 1 d . . . C12 C 0.2135(3) 0.15166(18) 0.6604(2) 0.0576(10) Uani 1 1 d . . . C13 C 0.1547(4) 0.2197(2) 0.6570(3) 0.0659(11) Uani 1 1 d . . . C14 C 0.2660(3) 0.11939(17) 0.7409(2) 0.0538(9) Uani 1 1 d . . . C15 C 0.0824(5) 0.5876(3) 0.9131(4) 0.0897(15) Uani 1 1 d . . . C16 C 0.0191(5) 0.5436(3) 0.8418(4) 0.0863(15) Uani 1 1 d . . . C17 C -0.0448(4) 0.5381(3) 0.6866(4) 0.0856(15) Uani 1 1 d . . . C18 C -0.0458(4) 0.5761(3) 0.6052(4) 0.0888(16) Uani 1 1 d . . . C19 C 0.0640(6) 0.6042(3) 0.5105(4) 0.1027(18) Uani 1 1 d . . . C20 C 0.1750(7) 0.6004(4) 0.5027(4) 0.106(2) Uani 1 1 d . . . C21 C 0.3510(7) 0.6397(4) 0.5646(5) 0.120(2) Uani 1 1 d . . . C22 C 0.4144(7) 0.6835(4) 0.6357(5) 0.124(2) Uani 1 1 d . . . C23 C 0.4787(5) 0.6913(4) 0.7914(6) 0.112(2) Uani 1 1 d . . . C24 C 0.4778(5) 0.6528(5) 0.8724(6) 0.118(2) Uani 1 1 d . . . C25 C 0.3667(6) 0.6232(4) 0.9656(4) 0.1031(19) Uani 1 1 d . . . C26 C 0.2568(6) 0.6286(3) 0.9744(3) 0.0949(17) Uani 1 1 d . . . C32 C 0.0946(9) 0.7805(5) 0.6560(7) 0.233(5) Uani 1 1 d . . . H32A H 0.0188 0.7699 0.6402 0.280 Uiso 1 1 calc R . . H32B H 0.1226 0.7678 0.6066 0.280 Uiso 1 1 calc R . . C33 C 0.1074(11) 0.8490(5) 0.6700(7) 0.227(5) Uani 1 1 d . . . H33A H 0.0400 0.8710 0.6692 0.273 Uiso 1 1 calc R . . H33B H 0.1370 0.8704 0.6257 0.273 Uiso 1 1 calc R . . C34 C 0.1773(11) 0.8534(5) 0.7520(7) 0.261(7) Uani 1 1 d . . . H34A H 0.1547 0.8882 0.7877 0.314 Uiso 1 1 calc R . . H34B H 0.2489 0.8642 0.7478 0.314 Uiso 1 1 calc R . . C35 C 0.1728(13) 0.7862(6) 0.7874(6) 0.297(8) Uani 1 1 d . . . H35A H 0.2427 0.7736 0.8241 0.356 Uiso 1 1 calc R . . H35B H 0.1230 0.7861 0.8241 0.356 Uiso 1 1 calc R . . B3 B 0.2620(5) 0.3267(3) 0.6345(3) 0.0794(15) Uani 1 1 d . . . B4 B 0.3883(5) 0.3742(3) 0.6736(3) 0.0724(14) Uani 1 1 d . . . B5 B 0.4432(4) 0.3693(2) 0.7927(3) 0.0652(13) Uani 1 1 d . . . B6 B 0.3619(4) 0.3196(2) 0.8509(3) 0.0618(12) Uani 1 1 d . . . B7 B 0.2340(5) 0.3603(2) 0.8205(3) 0.0644(13) Uani 1 1 d . . . B8 B 0.1753(4) 0.3616(2) 0.6960(3) 0.0675(13) Uani 1 1 d . . . B9 B 0.2666(4) 0.4143(2) 0.6546(3) 0.0744(15) Uani 1 1 d . . . B10 B 0.3708(4) 0.4422(3) 0.7423(3) 0.0711(14) Uani 1 1 d . . . B11 B 0.3525(4) 0.4095(2) 0.8413(3) 0.0696(14) Uani 1 1 d . . . B12 B 0.2406(4) 0.4306(2) 0.7557(3) 0.0717(14) Uani 1 1 d . . . H6 H 0.397(2) 0.2954(15) 0.916(2) 0.057(9) Uiso 1 1 d . . . H H 0.417(3) 0.3309(18) 0.729(2) 0.071(10) Uiso 1 1 d . . . H13A H 0.126(3) 0.2284(17) 0.597(3) 0.073(12) Uiso 1 1 d . . . H11 H 0.389(3) 0.4387(18) 0.906(2) 0.082(11) Uiso 1 1 d . . . H8 H 0.089(3) 0.3637(17) 0.674(2) 0.079(12) Uiso 1 1 d . . . H3A H 0.249(3) 0.2254(18) 0.903(3) 0.073(12) Uiso 1 1 d . . . H4 H 0.446(4) 0.379(2) 0.629(3) 0.104(14) Uiso 1 1 d . . . H18A H -0.084(4) 0.557(2) 0.555(3) 0.094(15) Uiso 1 1 d . . . H3B H 0.148(3) 0.2180(18) 0.811(2) 0.077(13) Uiso 1 1 d . . . H17A H -0.008(3) 0.492(2) 0.689(2) 0.087(13) Uiso 1 1 d . . . H16A H -0.058(4) 0.541(2) 0.843(2) 0.089(14) Uiso 1 1 d . . . H9 H 0.240(3) 0.4431(19) 0.593(3) 0.094(13) Uiso 1 1 d . . . H12 H 0.192(3) 0.471(2) 0.765(2) 0.095(13) Uiso 1 1 d . . . H15A H 0.085(4) 0.564(2) 0.967(3) 0.114(18) Uiso 1 1 d . . . H17B H -0.118(4) 0.5314(19) 0.691(2) 0.080(13) Uiso 1 1 d . . . H3 H 0.230(3) 0.3142(18) 0.566(2) 0.079(11) Uiso 1 1 d . . . H7 H 0.184(3) 0.3610(18) 0.859(2) 0.078(12) Uiso 1 1 d . . . H13B H 0.087(4) 0.217(2) 0.688(3) 0.110(15) Uiso 1 1 d . . . H11A H 0.175(3) 0.1434(18) 0.531(3) 0.074(13) Uiso 1 1 d . . . H20A H 0.197(4) 0.549(3) 0.515(3) 0.118(18) Uiso 1 1 d . . . H10 H 0.411(3) 0.492(2) 0.740(2) 0.092(12) Uiso 1 1 d . . . H6A H 0.405(4) 0.024(2) 0.946(3) 0.105(16) Uiso 1 1 d . . . H16B H 0.057(3) 0.498(2) 0.841(2) 0.091(14) Uiso 1 1 d . . . H5 H 0.531(3) 0.3689(16) 0.816(2) 0.062(10) Uiso 1 1 d . . . H25A H 0.401(4) 0.575(3) 0.965(3) 0.14(2) Uiso 1 1 d . . . H25B H 0.412(5) 0.642(3) 1.016(4) 0.14(2) Uiso 1 1 d . . . H26A H 0.256(4) 0.610(2) 1.034(4) 0.131(18) Uiso 1 1 d . . . H5A H 0.331(3) 0.133(2) 0.956(3) 0.091(15) Uiso 1 1 d . . . H9A H 0.346(4) -0.017(2) 0.661(3) 0.093(16) Uiso 1 1 d . . . H10A H 0.262(4) 0.044(2) 0.521(3) 0.100(15) Uiso 1 1 d . . . H26B H 0.235(4) 0.680(2) 0.962(3) 0.113(17) Uiso 1 1 d . . . H7A H 0.408(4) -0.026(2) 0.817(3) 0.107(15) Uiso 1 1 d . . . H24A H 0.530(5) 0.671(3) 0.914(3) 0.12(2) Uiso 1 1 d . . . H15A H 0.052(4) 0.641(3) 0.907(3) 0.130(18) Uiso 1 1 d . . . H20B H 0.181(5) 0.615(3) 0.448(4) 0.15(2) Uiso 1 1 d . . . H19A H 0.047(3) 0.655(2) 0.515(3) 0.087(14) Uiso 1 1 d . . . H21A H 0.379(5) 0.591(3) 0.575(4) 0.17(3) Uiso 1 1 d . . . H23A H 0.544(5) 0.691(3) 0.772(3) 0.13(2) Uiso 1 1 d . . . H22A H 0.383(4) 0.730(3) 0.634(3) 0.12(2) Uiso 1 1 d . . . H23B H 0.444(5) 0.742(3) 0.794(4) 0.17(2) Uiso 1 1 d . . . H21B H 0.352(5) 0.654(3) 0.506(4) 0.17(3) Uiso 1 1 d . . . H17B H -0.068(4) 0.626(2) 0.607(3) 0.106(16) Uiso 1 1 d . . . H19B H 0.014(5) 0.579(3) 0.461(4) 0.14(2) Uiso 1 1 d . . . H22B H 0.478(5) 0.693(3) 0.625(4) 0.16(3) Uiso 1 1 d . . . H24B H 0.494(5) 0.604(3) 0.874(4) 0.15(3) 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 K1 0.0645(6) 0.0649(5) 0.0582(5) 0.0009(4) 0.0068(4) -0.0099(5) O1 0.079(2) 0.083(2) 0.0655(18) -0.0003(14) 0.0184(16) 0.0073(16) O2 0.0599(18) 0.0714(17) 0.088(2) -0.0138(16) 0.0133(16) -0.0031(15) O3 0.072(2) 0.092(2) 0.0598(19) -0.0078(15) -0.0051(15) 0.0190(17) O4 0.123(3) 0.089(2) 0.084(2) 0.0019(18) 0.045(2) 0.007(2) O5 0.084(2) 0.076(2) 0.127(3) -0.010(2) 0.039(2) -0.0173(18) O6 0.064(2) 0.091(2) 0.085(2) -0.0098(17) -0.0072(17) -0.0018(17) O7 0.307(8) 0.071(3) 0.207(6) 0.006(4) 0.063(5) 0.030(4) C1 0.061(3) 0.047(2) 0.048(2) -0.0037(16) 0.0152(18) 0.0025(18) C2 0.061(3) 0.049(2) 0.048(2) 0.0006(17) 0.0052(18) 0.0037(18) C3 0.076(3) 0.059(3) 0.055(3) -0.003(2) 0.024(2) -0.008(2) C4 0.057(3) 0.053(2) 0.056(2) 0.0023(18) 0.018(2) -0.0078(19) C5 0.075(3) 0.077(3) 0.066(3) 0.009(3) 0.016(2) -0.009(3) C6 0.081(4) 0.078(4) 0.104(4) 0.036(3) 0.011(3) 0.007(3) C7 0.081(4) 0.060(3) 0.120(5) 0.016(3) 0.033(3) 0.008(3) C8 0.070(3) 0.050(2) 0.097(3) -0.003(2) 0.035(3) -0.007(2) C9 0.095(4) 0.059(3) 0.123(5) -0.024(3) 0.051(4) -0.010(3) C10 0.115(5) 0.088(4) 0.089(4) -0.036(3) 0.053(4) -0.029(3) C11 0.092(4) 0.071(3) 0.066(3) -0.008(3) 0.023(3) -0.020(3) C12 0.066(3) 0.054(2) 0.056(2) -0.0096(19) 0.020(2) -0.015(2) C13 0.071(3) 0.058(3) 0.060(3) -0.001(2) 0.002(2) -0.009(2) C14 0.050(2) 0.048(2) 0.067(3) -0.0004(18) 0.022(2) -0.0057(18) C15 0.098(5) 0.098(4) 0.084(4) 0.007(3) 0.042(3) 0.019(3) C16 0.077(4) 0.085(4) 0.109(4) 0.008(3) 0.045(3) 0.008(3) C17 0.052(3) 0.073(3) 0.123(5) -0.023(3) 0.006(3) 0.001(3) C18 0.061(4) 0.084(4) 0.101(4) -0.029(3) -0.016(3) 0.013(3) C19 0.124(6) 0.097(4) 0.066(4) -0.002(3) -0.012(3) 0.018(4) C20 0.161(7) 0.105(5) 0.055(3) 0.002(3) 0.031(4) 0.012(5) C21 0.141(7) 0.124(6) 0.120(6) 0.007(5) 0.080(5) 0.003(5) C22 0.140(7) 0.101(5) 0.160(7) 0.008(5) 0.094(6) -0.019(5) C23 0.075(4) 0.108(5) 0.163(7) -0.045(5) 0.047(4) -0.036(4) C24 0.057(4) 0.145(7) 0.135(6) -0.044(5) -0.005(4) -0.010(4) C25 0.095(5) 0.115(5) 0.075(4) -0.005(3) -0.023(3) 0.014(4) C26 0.125(6) 0.098(4) 0.051(3) -0.002(3) 0.004(3) 0.006(4) C32 0.272(12) 0.117(8) 0.266(13) -0.015(8) -0.011(10) 0.026(8) C33 0.401(18) 0.123(7) 0.176(9) 0.047(6) 0.106(10) 0.061(9) C34 0.43(2) 0.157(9) 0.160(9) 0.003(7) 0.002(10) -0.100(11) C35 0.58(2) 0.123(7) 0.166(9) -0.003(7) 0.063(12) 0.139(11) B3 0.089(4) 0.090(4) 0.054(3) -0.006(3) 0.010(3) -0.015(3) B4 0.079(4) 0.073(3) 0.067(3) 0.004(3) 0.022(3) 0.000(3) B5 0.057(3) 0.062(3) 0.070(3) -0.009(2) 0.005(3) 0.000(2) B6 0.077(4) 0.056(3) 0.049(3) -0.003(2) 0.009(2) 0.002(2) B7 0.078(4) 0.057(3) 0.062(3) -0.007(2) 0.026(3) 0.006(3) B8 0.058(3) 0.062(3) 0.077(3) 0.009(2) 0.007(3) 0.011(3) B9 0.086(4) 0.060(3) 0.071(3) 0.021(2) 0.009(3) 0.005(3) B10 0.073(4) 0.052(3) 0.088(4) 0.002(2) 0.021(3) -0.001(3) B11 0.076(4) 0.055(3) 0.074(3) -0.015(2) 0.012(3) 0.003(2) B12 0.070(4) 0.054(3) 0.090(4) 0.003(2) 0.020(3) 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O5 2.728(3) . ? K1 O3 2.763(3) . ? K1 O7 2.769(5) . ? K1 O6 2.786(3) . ? K1 O1 2.816(3) . ? K1 O4 2.850(3) . ? K1 O2 2.849(3) . ? K1 B12 3.474(5) . ? O1 C15 1.409(6) . ? O1 C26 1.412(6) . ? O2 C17 1.413(5) . ? O2 C16 1.429(5) . ? O3 C19 1.406(6) . ? O3 C18 1.431(6) . ? O4 C20 1.415(7) . ? O4 C21 1.424(8) . ? O5 C23 1.418(7) . ? O5 C22 1.419(7) . ? O6 C24 1.420(7) . ? O6 C25 1.425(6) . ? O7 C35 1.257(10) . ? O7 C32 1.341(10) . ? C1 C2 1.441(5) . ? C1 C3 1.531(5) . ? C1 B6 1.539(6) . ? C1 B7 1.790(6) . ? C2 B3 1.495(6) . ? C2 C13 1.533(5) . ? C2 B8 1.787(6) . ? C3 C4 1.500(5) . ? C4 C5 1.377(5) . ? C4 C14 1.433(5) . ? C5 C6 1.399(6) . ? C6 C7 1.344(7) . ? C7 C8 1.398(6) . ? C8 C9 1.419(6) . ? C8 C14 1.433(5) . ? C9 C10 1.330(7) . ? C10 C11 1.402(7) . ? C11 C12 1.375(5) . ? C12 C14 1.415(5) . ? C12 C13 1.516(5) . ? C15 C16 1.476(7) . ? C17 C18 1.471(7) . ? C19 C20 1.479(8) . ? C21 C22 1.472(9) . ? C23 C24 1.478(9) . ? C25 C26 1.469(8) . ? C32 C33 1.349(10) . ? C33 C34 1.370(11) . ? C34 C35 1.424(11) . ? B3 B9 1.726(7) . ? B3 B8 1.794(8) . ? B3 B4 1.838(8) . ? B4 B9 1.714(8) . ? B4 B10 1.756(7) . ? B4 B5 1.822(7) . ? B5 B11 1.741(7) . ? B5 B10 1.766(7) . ? B5 B6 1.837(7) . ? B6 B11 1.750(6) . ? B6 B7 1.784(7) . ? B7 B12 1.715(7) . ? B7 B11 1.765(7) . ? B7 B8 1.904(7) . ? B8 B12 1.723(7) . ? B8 B9 1.808(7) . ? B9 B12 1.736(7) . ? B9 B10 1.746(7) . ? B10 B11 1.750(7) . ? B10 B12 1.769(8) . ? B11 B12 1.750(7) . ? 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 O5 K1 O3 120.06(11) . . ? O5 K1 O7 90.49(16) . . ? O3 K1 O7 88.96(18) . . ? O5 K1 O6 61.03(11) . . ? O3 K1 O6 174.07(9) . . ? O7 K1 O6 85.19(18) . . ? O5 K1 O1 120.85(11) . . ? O3 K1 O1 119.03(10) . . ? O7 K1 O1 92.97(16) . . ? O6 K1 O1 60.51(10) . . ? O5 K1 O4 60.38(12) . . ? O3 K1 O4 60.41(11) . . ? O7 K1 O4 80.90(16) . . ? O6 K1 O4 119.32(12) . . ? O1 K1 O4 173.82(9) . . ? O5 K1 O2 173.56(9) . . ? O3 K1 O2 60.73(9) . . ? O7 K1 O2 83.11(16) . . ? O6 K1 O2 117.45(10) . . ? O1 K1 O2 59.09(9) . . ? O4 K1 O2 118.90(11) . . ? O5 K1 B12 106.81(11) . . ? O3 K1 B12 81.54(10) . . ? O7 K1 B12 162.67(18) . . ? O6 K1 B12 103.88(11) . . ? O1 K1 B12 79.24(10) . . ? O4 K1 B12 106.44(11) . . ? O2 K1 B12 79.60(11) . . ? C15 O1 C26 113.1(4) . . ? C15 O1 K1 116.9(3) . . ? C26 O1 K1 114.3(3) . . ? C17 O2 C16 112.5(4) . . ? C17 O2 K1 110.9(3) . . ? C16 O2 K1 112.9(3) . . ? C19 O3 C18 113.4(4) . . ? C19 O3 K1 117.1(3) . . ? C18 O3 K1 114.7(3) . . ? C20 O4 C21 112.5(5) . . ? C20 O4 K1 110.2(3) . . ? C21 O4 K1 110.6(4) . . ? C23 O5 C22 113.6(6) . . ? C23 O5 K1 116.8(4) . . ? C22 O5 K1 117.6(4) . . ? C24 O6 C25 113.2(5) . . ? C24 O6 K1 110.7(3) . . ? C25 O6 K1 112.8(3) . . ? C35 O7 C32 104.2(6) . . ? C35 O7 K1 122.9(7) . . ? C32 O7 K1 130.7(6) . . ? C2 C1 C3 115.8(3) . . ? C2 C1 B6 127.8(3) . . ? C3 C1 B6 115.9(3) . . ? C2 C1 B7 101.0(3) . . ? C3 C1 B7 113.6(3) . . ? B6 C1 B7 64.3(3) . . ? C1 C2 B3 128.1(3) . . ? C1 C2 C13 115.5(3) . . ? B3 C2 C13 116.4(3) . . ? C1 C2 B8 93.8(3) . . ? B3 C2 B8 65.6(3) . . ? C13 C2 B8 115.9(3) . . ? C4 C3 C1 113.4(3) . . ? C5 C4 C14 118.7(4) . . ? C5 C4 C3 118.3(4) . . ? C14 C4 C3 122.9(3) . . ? C4 C5 C6 122.3(5) . . ? C7 C6 C5 119.9(5) . . ? C6 C7 C8 121.0(5) . . ? C7 C8 C9 120.6(5) . . ? C7 C8 C14 120.3(4) . . ? C9 C8 C14 119.1(5) . . ? C10 C9 C8 121.0(5) . . ? C9 C10 C11 120.8(5) . . ? C12 C11 C10 121.0(5) . . ? C11 C12 C14 119.9(4) . . ? C11 C12 C13 117.7(4) . . ? C14 C12 C13 122.4(3) . . ? C12 C13 C2 110.6(3) . . ? C12 C14 C8 118.2(3) . . ? C12 C14 C4 124.1(3) . . ? C8 C14 C4 117.7(3) . . ? O1 C15 C16 108.8(4) . . ? O2 C16 C15 108.2(4) . . ? O2 C17 C18 108.6(4) . . ? O3 C18 C17 109.3(4) . . ? O3 C19 C20 109.2(5) . . ? O4 C20 C19 110.0(5) . . ? O4 C21 C22 108.4(6) . . ? O5 C22 C21 109.7(6) . . ? O5 C23 C24 107.8(5) . . ? O6 C24 C23 109.1(6) . . ? O6 C25 C26 109.7(5) . . ? O1 C26 C25 108.8(5) . . ? O7 C32 C33 113.0(9) . . ? C32 C33 C34 103.8(8) . . ? C33 C34 C35 103.1(9) . . ? O7 C35 C34 110.6(8) . . ? C2 B3 B9 120.5(4) . . ? C2 B3 B8 65.1(3) . . ? B9 B3 B8 61.8(3) . . ? C2 B3 B4 117.1(4) . . ? B9 B3 B4 57.4(3) . . ? B8 B3 B4 105.0(4) . . ? B9 B4 B10 60.4(3) . . ? B9 B4 B5 107.4(4) . . ? B10 B4 B5 59.1(3) . . ? B9 B4 B3 58.0(3) . . ? B10 B4 B3 109.6(4) . . ? B5 B4 B3 113.1(4) . . ? B11 B5 B10 59.9(3) . . ? B11 B5 B4 107.3(4) . . ? B10 B5 B4 58.6(3) . . ? B11 B5 B6 58.5(3) . . ? B10 B5 B6 109.6(4) . . ? B4 B5 B6 114.6(4) . . ? C1 B6 B11 118.0(4) . . ? C1 B6 B7 64.7(3) . . ? B11 B6 B7 59.9(3) . . ? C1 B6 B5 115.9(3) . . ? B11 B6 B5 58.0(3) . . ? B7 B6 B5 104.4(3) . . ? B12 B7 B11 60.4(3) . . ? B12 B7 B6 108.9(4) . . ? B11 B7 B6 59.1(3) . . ? B12 B7 C1 121.3(4) . . ? B11 B7 C1 105.1(3) . . ? B6 B7 C1 51.0(2) . . ? B12 B7 B8 56.6(3) . . ? B11 B7 B8 106.2(3) . . ? B6 B7 B8 112.1(3) . . ? C1 B7 B8 79.7(3) . . ? B12 B8 C2 123.8(4) . . ? B12 B8 B3 107.3(4) . . ? C2 B8 B3 49.4(2) . . ? B12 B8 B9 58.8(3) . . ? C2 B8 B9 102.3(3) . . ? B3 B8 B9 57.3(3) . . ? B12 B8 B7 56.2(3) . . ? C2 B8 B7 85.3(3) . . ? B3 B8 B7 114.1(4) . . ? B9 B8 B7 104.6(4) . . ? B4 B9 B3 64.6(3) . . ? B4 B9 B12 108.2(4) . . ? B3 B9 B12 109.9(4) . . ? B4 B9 B10 61.0(3) . . ? B3 B9 B10 115.6(4) . . ? B12 B9 B10 61.1(3) . . ? B4 B9 B8 109.8(3) . . ? B3 B9 B8 61.0(3) . . ? B12 B9 B8 58.2(3) . . ? B10 B9 B8 109.6(3) . . ? B9 B10 B11 109.4(4) . . ? B9 B10 B4 58.6(3) . . ? B11 B10 B4 110.0(3) . . ? B9 B10 B5 108.5(3) . . ? B11 B10 B5 59.4(3) . . ? B4 B10 B5 62.3(3) . . ? B9 B10 B12 59.2(3) . . ? B11 B10 B12 59.7(3) . . ? B4 B10 B12 104.9(4) . . ? B5 B10 B12 104.9(4) . . ? B5 B11 B6 63.5(3) . . ? B5 B11 B10 60.8(3) . . ? B6 B11 B10 114.6(3) . . ? B5 B11 B12 106.7(4) . . ? B6 B11 B12 108.9(3) . . ? B10 B11 B12 60.7(3) . . ? B5 B11 B7 109.4(3) . . ? B6 B11 B7 61.0(3) . . ? B10 B11 B7 110.1(4) . . ? B12 B11 B7 58.4(3) . . ? B7 B12 B8 67.3(3) . . ? B7 B12 B9 116.7(4) . . ? B8 B12 B9 63.0(3) . . ? B7 B12 B11 61.2(3) . . ? B8 B12 B11 115.3(3) . . ? B9 B12 B11 109.9(4) . . ? B7 B12 B10 111.6(4) . . ? B8 B12 B10 112.5(4) . . ? B9 B12 B10 59.7(3) . . ? B11 B12 B10 59.6(3) . . ? B7 B12 K1 145.5(3) . . ? B8 B12 K1 135.6(3) . . ? B9 B12 K1 97.8(2) . . ? B11 B12 K1 108.8(3) . . ? B10 B12 K1 85.1(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.304 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.038 #===END data_11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H54 B10 Na2 O4' _chemical_formula_weight 656.83 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 25.2027(15) _cell_length_b 13.9213(8) _cell_length_c 11.4686(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4023.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8652 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16889 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5180 _reflns_number_gt 2957 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1153P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_number_reflns 5180 _refine_ls_number_parameters 435 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1986 _refine_ls_wR_factor_gt 0.1726 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.181 _refine_ls_shift/su_mean 0.002 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 Na1 Na 0.43599(3) 0.93694(6) 0.54111(7) 0.0648(3) Uani 1 1 d . . . C1 C 0.54214(8) 1.23113(13) 0.77792(17) 0.0469(6) Uani 1 1 d . . . Na2 Na 0.50757(3) 1.12984(6) 0.32862(7) 0.0645(3) Uani 1 1 d . . . B2 B 0.49795(9) 1.19184(18) 0.6873(2) 0.0516(8) Uani 1 1 d . . . H2 H 0.4679 1.2479 0.6734 0.062 Uiso 1 1 calc R . . B3 B 0.55304(9) 1.19458(18) 0.5611(2) 0.0542(8) Uani 1 1 d . . . H3 H 0.5623 1.2718 0.5595 0.065 Uiso 1 1 calc R . . B5 B 0.60455(10) 1.06585(19) 0.6808(2) 0.0583(8) Uani 1 1 d . . . H5 H 0.6447 1.0370 0.6941 0.070 Uiso 1 1 calc R . . B6 B 0.58253(9) 1.15997(18) 0.8086(2) 0.0543(8) Uani 1 1 d . . . H6 H 0.6177 1.2067 0.8103 0.065 Uiso 1 1 calc R . . B7 B 0.51236(9) 1.14322(17) 0.8334(2) 0.0516(7) Uani 1 1 d . . . H7 H 0.4892 1.1460 0.9146 0.062 Uiso 1 1 calc R . . B8 B 0.49248(10) 1.06489(19) 0.7207(2) 0.0571(8) Uani 1 1 d . . . H8 H 0.4552 1.0264 0.7382 0.069 Uiso 1 1 calc R . . B9 B 0.50802(10) 1.09984(18) 0.5774(2) 0.0563(8) Uani 1 1 d . . . H9 H 0.4770 1.0925 0.5105 0.068 Uiso 1 1 calc R . . B10 B 0.57458(10) 1.07286(19) 0.5344(2) 0.0598(8) Uani 1 1 d . . . H10 H 0.5863 1.0373 0.4527 0.072 Uiso 1 1 calc R . . B11 B 0.54230(10) 1.0065(2) 0.6446(2) 0.0587(8) Uani 1 1 d . . . H11 H 0.5377 0.9295 0.6257 0.070 Uiso 1 1 calc R . . B12 B 0.55398(9) 1.04559(17) 0.7892(2) 0.0499(8) Uani 1 1 d . . . H12 H 0.5634 0.9910 0.8554 0.060 Uiso 1 1 calc R . . C4 C 0.60637(7) 1.15931(15) 0.59450(17) 0.0496(6) Uani 1 1 d . . . C5 C 0.65806(8) 1.20649(16) 0.56452(19) 0.0638(7) Uani 1 1 d . . . H5A H 0.6528 1.2533 0.5030 0.077 Uiso 1 1 calc R . . H5B H 0.6832 1.1588 0.5371 0.077 Uiso 1 1 calc R . . C6 C 0.67964(8) 1.25612(16) 0.6742(2) 0.0676(8) Uani 1 1 d . . . C7 C 0.72112(9) 1.2121(2) 0.7340(2) 0.0989(11) Uani 1 1 d . . . H7A H 0.7376 1.1578 0.7035 0.119 Uiso 1 1 calc R . . C8 C 0.73762(10) 1.2505(2) 0.8404(3) 0.1203(11) Uani 1 1 d . . . H8A H 0.7648 1.2198 0.8807 0.144 Uiso 1 1 calc R . . C9 C 0.71610(11) 1.3293(2) 0.8866(3) 0.1226(12) Uani 1 1 d . . . H9A H 0.7287 1.3539 0.9568 0.147 Uiso 1 1 calc R . . C10 C 0.67402(10) 1.37476(19) 0.8279(2) 0.0953(10) Uani 1 1 d . . . H10A H 0.6579 1.4288 0.8600 0.114 Uiso 1 1 calc R . . C11 C 0.65649(9) 1.33823(16) 0.7211(2) 0.0681(8) Uani 1 1 d . . . C12 C 0.61326(9) 1.39172(15) 0.6607(2) 0.0676(8) Uani 1 1 d . . . C13 C 0.62610(11) 1.44387(17) 0.5598(2) 0.0878(9) Uani 1 1 d . . . H13 H 0.6607 1.4431 0.5316 0.105 Uiso 1 1 calc R . . C14 C 0.58737(12) 1.49676(18) 0.5018(3) 0.0948(10) Uani 1 1 d . . . H14 H 0.5961 1.5304 0.4344 0.114 Uiso 1 1 calc R . . C15 C 0.53719(12) 1.49936(19) 0.5429(2) 0.1007(11) Uani 1 1 d . . . H15 H 0.5115 1.5349 0.5039 0.121 Uiso 1 1 calc R . . C16 C 0.52424(10) 1.45031(16) 0.6410(2) 0.0749(9) Uani 1 1 d . . . H16 H 0.4895 1.4531 0.6680 0.090 Uiso 1 1 calc R . . C17 C 0.56092(9) 1.39619(15) 0.70241(19) 0.0650(8) Uani 1 1 d . . . C18 C 0.54274(9) 1.33698(14) 0.80707(19) 0.0659(8) Uani 1 1 d . . . H18A H 0.5665 1.3482 0.8722 0.079 Uiso 1 1 calc R . . H18B H 0.5074 1.3571 0.8301 0.079 Uiso 1 1 calc R . . O3 O 0.43208(6) 0.80806(10) 0.68396(12) 0.0645(5) Uani 1 1 d . . . C31 C 0.37982(9) 0.79240(16) 0.7304(2) 0.0759(9) Uani 1 1 d . . . H31A H 0.3775 0.8173 0.8093 0.091 Uiso 1 1 calc R . . H31B H 0.3535 0.8248 0.6828 0.091 Uiso 1 1 calc R . . C32 C 0.37068(13) 0.6909(2) 0.7300(4) 0.1528(16) Uani 1 1 d . . . H32A H 0.3355 0.6773 0.6998 0.183 Uiso 1 1 calc R . . H32B H 0.3728 0.6660 0.8089 0.183 Uiso 1 1 calc R . . C33 C 0.41129(12) 0.6443(2) 0.6558(4) 0.1324(14) Uani 1 1 d . . . H33A H 0.4268 0.5896 0.6957 0.159 Uiso 1 1 calc R . . H33B H 0.3957 0.6224 0.5833 0.159 Uiso 1 1 calc R . . C34 C 0.45148(10) 0.71737(17) 0.6335(2) 0.0815(9) Uani 1 1 d . . . H34A H 0.4571 0.7246 0.5503 0.098 Uiso 1 1 calc R . . H34B H 0.4849 0.6992 0.6693 0.098 Uiso 1 1 calc R . . O4 O 0.44224(6) 1.24386(13) 0.31549(16) 0.0964(7) Uani 1 1 d . . . C41 C 0.39750(12) 1.2417(3) 0.2407(4) 0.1805(19) Uani 1 1 d . . . H41A H 0.4083 1.2566 0.1616 0.217 Uiso 1 1 calc R . . H41B H 0.3819 1.1780 0.2411 0.217 Uiso 1 1 calc R . . C42 C 0.36109(15) 1.3071(4) 0.2777(5) 0.229(2) Uani 1 1 d . . . H42A H 0.3277 1.2755 0.2946 0.275 Uiso 1 1 calc R . . H42B H 0.3550 1.3549 0.2176 0.275 Uiso 1 1 calc R . . C43 C 0.38296(17) 1.3554(4) 0.3884(5) 0.241(2) Uani 1 1 d . . . H43A H 0.3823 1.4248 0.3813 0.289 Uiso 1 1 calc R . . H43B H 0.3626 1.3368 0.4566 0.289 Uiso 1 1 calc R . . C44 C 0.43488(14) 1.3214(3) 0.3954(4) 0.1657(17) Uani 1 1 d . . . H44A H 0.4421 1.2995 0.4742 0.199 Uiso 1 1 calc R . . H44B H 0.4595 1.3728 0.3772 0.199 Uiso 1 1 calc R . . O5 O 0.35207(6) 0.99949(13) 0.56592(16) 0.0940(6) Uani 1 1 d D . . C51 C 0.30888(10) 0.9867(2) 0.4889(3) 0.1364(13) Uani 1 1 d D . . H51A H 0.2957 0.9215 0.4950 0.164 Uiso 1 1 calc R . . H51B H 0.3206 0.9971 0.4093 0.164 Uiso 1 1 calc R . . C52 C 0.26775(13) 1.0521(3) 0.5162(4) 0.186(2) Uani 1 1 d D . . H52A H 0.2342 1.0188 0.5254 0.223 Uiso 1 1 calc R . . H52B H 0.2640 1.1001 0.4554 0.223 Uiso 1 1 calc R . . C53 C 0.28479(13) 1.0989(3) 0.6313(4) 0.224(2) Uani 1 1 d D . . H53A H 0.2851 1.1683 0.6237 0.268 Uiso 1 1 calc R . . H53B H 0.2605 1.0815 0.6933 0.268 Uiso 1 1 calc R . . C54 C 0.33605(13) 1.0646(2) 0.6561(3) 0.1600(16) Uani 1 1 d D . . H54A H 0.3361 1.0319 0.7307 0.192 Uiso 1 1 calc R . . H54B H 0.3607 1.1179 0.6603 0.192 Uiso 1 1 calc R . . O6 O 0.35574(11) 1.3124(3) 0.7932(4) 0.6150(19) Uani 1 1 d D . . C61 C 0.3285(2) 1.2919(4) 0.8975(5) 0.667(3) Uani 1 1 d D . . H61A H 0.3524 1.3000 0.9632 0.801 Uiso 1 1 calc R . . H61B H 0.3166 1.2257 0.8966 0.801 Uiso 1 1 calc R . . C62 C 0.28425(12) 1.3539(3) 0.9105(4) 0.368(2) Uani 1 1 d D . . H62A H 0.2874 1.3901 0.9825 0.441 Uiso 1 1 calc R . . H62B H 0.2518 1.3165 0.9139 0.441 Uiso 1 1 calc R . . C63 C 0.28218(18) 1.4259(3) 0.8018(6) 0.520(5) Uani 1 1 d D . . H63A H 0.2482 1.4238 0.7623 0.624 Uiso 1 1 calc R . . H63B H 0.2901 1.4915 0.8245 0.624 Uiso 1 1 calc R . . C64 C 0.3239(2) 1.3848(4) 0.7322(5) 0.544(3) Uani 1 1 d D . . H64A H 0.3472 1.4360 0.7060 0.653 Uiso 1 1 calc R . . H64B H 0.3083 1.3556 0.6635 0.653 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 Na1 0.0803(5) 0.0770(5) 0.0370(4) 0.0039(4) 0.0013(4) -0.0127(5) C1 0.0630(12) 0.0451(11) 0.0325(11) 0.0012(10) 0.0054(10) -0.0003(10) Na2 0.0815(5) 0.0703(5) 0.0416(4) 0.0039(4) 0.0041(4) -0.0067(5) B2 0.0603(14) 0.0591(15) 0.0354(13) -0.0069(13) -0.0028(12) 0.0008(13) B3 0.0630(14) 0.0568(14) 0.0430(15) -0.0006(13) 0.0086(13) -0.0218(12) B5 0.0573(14) 0.0794(17) 0.0383(13) 0.0025(14) 0.0036(12) -0.0011(13) B6 0.0514(13) 0.0631(15) 0.0484(16) 0.0035(13) -0.0004(13) -0.0112(12) B7 0.0598(13) 0.0627(15) 0.0322(12) 0.0033(12) 0.0030(12) -0.0059(12) B8 0.0747(16) 0.0686(16) 0.0280(13) 0.0045(13) -0.0027(12) -0.0201(14) B9 0.0670(15) 0.0655(15) 0.0365(14) -0.0001(13) -0.0100(13) -0.0063(13) B10 0.0872(17) 0.0704(17) 0.0218(12) -0.0048(12) 0.0046(13) -0.0089(15) B11 0.0740(16) 0.0639(16) 0.0381(14) 0.0016(13) 0.0032(14) -0.0026(14) B12 0.0689(15) 0.0494(13) 0.0313(13) 0.0077(12) 0.0040(12) -0.0059(12) C4 0.0517(11) 0.0688(13) 0.0283(10) 0.0047(10) 0.0030(9) 0.0020(10) C5 0.0596(12) 0.0896(16) 0.0421(13) 0.0034(12) 0.0024(11) -0.0013(12) C6 0.0473(11) 0.0923(16) 0.0633(14) 0.0242(13) 0.0037(12) -0.0240(12) C7 0.0622(14) 0.148(2) 0.0868(19) 0.0321(17) -0.0260(14) -0.0148(16) C8 0.0802(15) 0.197(3) 0.0839(18) 0.053(2) -0.0408(15) -0.0493(18) C9 0.133(2) 0.149(2) 0.086(2) 0.005(2) -0.0338(18) -0.062(2) C10 0.1139(17) 0.1041(18) 0.0678(17) 0.0162(15) -0.0355(16) -0.0454(16) C11 0.0700(13) 0.0723(14) 0.0622(15) 0.0131(13) -0.0114(12) -0.0275(12) C12 0.0975(15) 0.0565(13) 0.0489(13) 0.0085(12) -0.0120(13) -0.0293(12) C13 0.1153(18) 0.0802(16) 0.0680(18) 0.0179(15) 0.0017(16) -0.0207(15) C14 0.143(2) 0.0733(17) 0.0685(17) 0.0255(15) -0.0032(18) 0.0019(17) C15 0.142(2) 0.0716(16) 0.089(2) 0.0237(16) -0.0134(19) 0.0218(17) C16 0.1035(17) 0.0656(15) 0.0555(15) 0.0084(13) -0.0035(14) 0.0111(14) C17 0.0987(16) 0.0517(12) 0.0446(13) 0.0002(11) -0.0073(13) -0.0113(12) C18 0.0853(15) 0.0684(14) 0.0439(14) -0.0018(12) 0.0016(13) -0.0020(13) O3 0.0774(9) 0.0725(9) 0.0437(8) -0.0088(8) 0.0088(7) -0.0191(8) C31 0.0751(14) 0.0788(16) 0.0738(17) -0.0093(14) 0.0176(13) -0.0096(13) C32 0.133(2) 0.113(2) 0.212(4) -0.038(2) 0.078(2) -0.0499(19) C33 0.132(2) 0.0854(19) 0.180(3) -0.016(2) 0.060(2) -0.0310(18) C34 0.0923(16) 0.0809(16) 0.0712(17) -0.0198(14) -0.0021(15) -0.0026(14) O4 0.1054(12) 0.1004(12) 0.0832(13) -0.0100(11) -0.0141(11) 0.0180(10) C41 0.128(2) 0.187(3) 0.226(4) -0.067(3) -0.072(3) 0.078(2) C42 0.153(3) 0.308(5) 0.225(5) 0.039(5) -0.013(3) 0.124(3) C43 0.225(4) 0.348(5) 0.149(4) -0.072(4) -0.036(3) 0.169(3) C44 0.186(3) 0.149(3) 0.162(3) -0.056(3) -0.068(3) 0.058(3) O5 0.0900(11) 0.1086(12) 0.0833(12) -0.0174(11) 0.0028(10) 0.0044(10) C51 0.108(2) 0.185(3) 0.116(2) -0.065(2) -0.0488(19) 0.054(2) C52 0.143(3) 0.222(4) 0.193(4) -0.048(4) -0.025(3) 0.070(3) C53 0.152(3) 0.299(4) 0.220(5) -0.099(4) -0.015(3) 0.113(3) C54 0.155(3) 0.138(2) 0.188(3) -0.090(2) -0.050(3) 0.042(2) O6 0.123(2) 0.754(3) 0.967(5) -0.778(2) 0.093(3) -0.094(2) C61 0.274(4) 0.932(6) 0.796(7) -0.760(4) 0.222(5) -0.355(4) C62 0.127(2) 0.452(4) 0.524(4) -0.410(3) 0.196(3) -0.167(3) C63 0.262(4) 0.188(4) 1.109(16) -0.212(6) -0.331(6) -0.033(4) C64 0.513(6) 0.812(7) 0.309(5) -0.377(4) 0.177(5) -0.520 _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 Na1 O5 2.3049(18) . ? Na1 O3 2.4318(16) . ? Na1 B12 2.910(3) 2_674 ? Na1 B9 2.934(3) . ? Na1 B7 2.935(3) 2_674 ? Na1 B6 3.025(3) 2_674 ? Na1 B8 3.073(3) . ? Na1 B11 3.086(3) . ? Na1 Na2 3.7095(11) 2_675 ? Na1 Na2 4.0501(11) . ? C1 B6 1.463(3) . ? C1 C18 1.511(3) . ? C1 B7 1.570(3) . ? C1 B2 1.618(3) . ? Na2 O4 2.2921(19) . ? Na2 O3 2.4110(16) 2_674 ? Na2 B9 2.883(3) . ? Na2 B12 2.928(2) 2_674 ? Na2 B8 2.980(3) 2_674 ? Na2 B10 3.008(3) . ? Na2 B3 3.039(3) . ? Na2 B11 3.104(3) 2_674 ? Na2 Na1 3.7095(11) 2_674 ? B2 B9 1.815(4) . ? B2 B8 1.814(4) . ? B2 B7 1.844(3) . ? B2 B3 2.006(3) . ? B3 C4 1.481(3) . ? B3 B9 1.750(3) . ? B3 B10 1.805(4) . ? B5 C4 1.635(3) . ? B5 B12 1.803(3) . ? B5 B11 1.821(4) . ? B5 B10 1.843(4) . ? B5 B6 2.043(4) . ? B6 B12 1.761(3) . ? B6 B7 1.806(3) . ? B6 Na1 3.025(3) 2_675 ? B7 B8 1.764(3) . ? B7 B12 1.790(3) . ? B7 Na1 2.935(3) 2_675 ? B8 B11 1.731(4) . ? B8 B12 1.759(3) . ? B8 B9 1.758(3) . ? B8 Na2 2.980(3) 2_675 ? B9 B11 1.741(4) . ? B9 B10 1.788(4) . ? B10 C4 1.602(3) . ? B10 B11 1.765(4) . ? B11 B12 1.770(3) . ? B11 Na2 3.104(3) 2_675 ? B12 Na1 2.910(3) 2_675 ? B12 Na2 2.928(2) 2_675 ? C4 C5 1.499(3) . ? C5 C6 1.535(3) . ? C6 C11 1.392(3) . ? C6 C7 1.393(3) . ? C7 C8 1.395(4) . ? C8 C9 1.334(4) . ? C9 C10 1.407(4) . ? C10 C11 1.398(3) . ? C11 C12 1.490(3) . ? C12 C13 1.404(3) . ? C12 C17 1.404(3) . ? C13 C14 1.392(4) . ? C14 C15 1.350(4) . ? C15 C16 1.356(4) . ? C16 C17 1.385(3) . ? C17 C18 1.526(3) . ? O3 C31 1.438(3) . ? O3 C34 1.472(3) . ? O3 Na2 2.4110(16) 2_675 ? C31 C32 1.432(4) . ? C32 C33 1.480(5) . ? C33 C34 1.458(4) . ? O4 C41 1.417(4) . ? O4 C44 1.428(4) . ? C41 C42 1.361(6) . ? C42 C43 1.539(7) . ? C43 C44 1.394(5) . ? O5 C51 1.413(3) . ? O5 C54 1.433(4) . ? C51 C52 1.415(4) . ? C52 C53 1.533(6) . ? C53 C54 1.406(4) . ? O6 C61 1.407(7) . ? O6 C64 1.467(7) . ? C61 C62 1.419(6) . ? C62 C63 1.600(8) . ? C63 C64 1.439(8) . ? 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 O5 Na1 O3 99.11(6) . . ? O5 Na1 B12 99.83(7) . 2_674 ? O3 Na1 B12 137.22(7) . 2_674 ? O5 Na1 B9 104.97(7) . . ? O3 Na1 B9 119.98(7) . . ? B12 Na1 B9 91.29(7) 2_674 . ? O5 Na1 B7 130.61(7) . 2_674 ? O3 Na1 B7 106.51(6) . 2_674 ? B12 Na1 B7 35.67(7) 2_674 2_674 ? B9 Na1 B7 97.73(7) . 2_674 ? O5 Na1 B6 97.80(7) . 2_674 ? O3 Na1 B6 104.99(6) . 2_674 ? B12 Na1 B6 34.46(7) 2_674 2_674 ? B9 Na1 B6 124.41(7) . 2_674 ? B7 Na1 B6 35.25(6) 2_674 2_674 ? O5 Na1 B8 97.09(7) . . ? O3 Na1 B8 89.71(6) . . ? B12 Na1 B8 125.22(7) 2_674 . ? B9 Na1 B8 33.94(7) . . ? B7 Na1 B8 123.98(7) 2_674 . ? B6 Na1 B8 157.07(7) 2_674 . ? O5 Na1 B11 129.09(7) . . ? O3 Na1 B11 90.42(6) . . ? B12 Na1 B11 106.28(7) 2_674 . ? B9 Na1 B11 33.49(7) . . ? B7 Na1 B11 92.66(7) 2_674 . ? B6 Na1 B11 127.81(7) 2_674 . ? B8 Na1 B11 32.65(7) . . ? O5 Na1 Na2 109.68(5) . 2_675 ? O3 Na1 Na2 39.80(4) . 2_675 ? B12 Na1 Na2 150.46(5) 2_674 2_675 ? B9 Na1 Na2 80.24(5) . 2_675 ? B7 Na1 Na2 117.13(5) 2_674 2_675 ? B6 Na1 Na2 136.97(6) 2_674 2_675 ? B8 Na1 Na2 51.08(5) . 2_675 ? B11 Na1 Na2 53.40(5) . 2_675 ? O5 Na1 Na2 103.45(5) . . ? O3 Na1 Na2 155.87(5) . . ? B12 Na1 Na2 46.26(5) 2_674 . ? B9 Na1 Na2 45.36(5) . . ? B7 Na1 Na2 64.29(5) 2_674 . ? B6 Na1 Na2 80.45(5) 2_674 . ? B8 Na1 Na2 79.20(5) . . ? B11 Na1 Na2 68.71(5) . . ? Na2 Na1 Na2 122.02(2) 2_675 . ? B6 C1 C18 126.87(19) . . ? B6 C1 B7 72.99(15) . . ? C18 C1 B7 132.45(18) . . ? B6 C1 B2 113.84(18) . . ? C18 C1 B2 118.59(17) . . ? B7 C1 B2 70.62(15) . . ? O4 Na2 O3 99.18(6) . 2_674 ? O4 Na2 B9 99.68(7) . . ? O3 Na2 B9 136.91(7) 2_674 . ? O4 Na2 B12 100.77(7) . 2_674 ? O3 Na2 B12 121.81(6) 2_674 2_674 ? B9 Na2 B12 91.95(7) . 2_674 ? O4 Na2 B8 127.04(7) . 2_674 ? O3 Na2 B8 92.33(6) 2_674 2_674 ? B9 Na2 B8 106.22(7) . 2_674 ? B12 Na2 B8 34.62(7) 2_674 2_674 ? O4 Na2 B10 129.60(7) . . ? O3 Na2 B10 106.28(6) 2_674 . ? B9 Na2 B10 35.26(7) . . ? B12 Na2 B10 101.45(7) 2_674 . ? B8 Na2 B10 94.95(7) 2_674 . ? O4 Na2 B3 97.07(7) . . ? O3 Na2 B3 105.04(6) 2_674 . ? B9 Na2 B3 34.24(7) . . ? B12 Na2 B3 125.63(7) 2_674 . ? B8 Na2 B3 129.38(7) 2_674 . ? B10 Na2 B3 34.74(7) . . ? O4 Na2 B11 95.05(7) . 2_674 ? O3 Na2 B11 90.40(6) 2_674 2_674 ? B9 Na2 B11 125.85(8) . 2_674 ? B12 Na2 B11 33.96(7) 2_674 2_674 ? B8 Na2 B11 32.98(7) 2_674 2_674 ? B10 Na2 B11 126.82(7) . 2_674 ? B3 Na2 B11 158.51(7) . 2_674 ? O4 Na2 Na1 112.99(6) . 2_674 ? O3 Na2 Na1 40.21(4) 2_674 2_674 ? B9 Na2 Na1 147.32(6) . 2_674 ? B12 Na2 Na1 81.77(5) 2_674 2_674 ? B8 Na2 Na1 53.34(5) 2_674 2_674 ? B10 Na2 Na1 114.58(6) . 2_674 ? B3 Na2 Na1 135.21(5) . 2_674 ? B11 Na2 Na1 52.97(5) 2_674 2_674 ? O4 Na2 Na1 100.30(5) . . ? O3 Na2 Na1 158.87(5) 2_674 . ? B9 Na2 Na1 46.40(5) . . ? B12 Na2 Na1 45.89(5) 2_674 . ? B8 Na2 Na1 69.31(5) 2_674 . ? B10 Na2 Na1 66.62(5) . . ? B3 Na2 Na1 80.60(5) . . ? B11 Na2 Na1 79.82(5) 2_674 . ? Na1 Na2 Na1 122.65(2) 2_674 . ? C1 B2 B9 126.04(18) . . ? C1 B2 B8 104.25(16) . . ? B9 B2 B8 57.96(13) . . ? C1 B2 B7 53.48(12) . . ? B9 B2 B7 110.17(17) . . ? B8 B2 B7 57.68(13) . . ? C1 B2 B3 88.90(14) . . ? B9 B2 B3 54.23(12) . . ? B8 B2 B3 102.91(16) . . ? B7 B2 B3 121.78(16) . . ? C4 B3 B9 108.11(18) . . ? C4 B3 B10 57.31(14) . . ? B9 B3 B10 60.37(14) . . ? C4 B3 B2 115.78(18) . . ? B9 B3 B2 57.31(13) . . ? B10 B3 B2 108.21(16) . . ? C4 B3 Na2 118.09(15) . . ? B9 B3 Na2 68.02(11) . . ? B10 B3 Na2 71.72(11) . . ? B2 B3 Na2 111.50(11) . . ? C4 B5 B12 124.17(18) . . ? C4 B5 B11 104.33(17) . . ? B12 B5 B11 58.46(13) . . ? C4 B5 B10 54.44(13) . . ? B12 B5 B10 110.29(17) . . ? B11 B5 B10 57.57(14) . . ? C4 B5 B6 86.07(15) . . ? B12 B5 B6 54.08(12) . . ? B11 B5 B6 102.72(16) . . ? B10 B5 B6 120.54(17) . . ? C1 B6 B12 107.31(17) . . ? C1 B6 B7 56.24(13) . . ? B12 B6 B7 60.22(13) . . ? C1 B6 B5 116.79(18) . . ? B12 B6 B5 55.99(13) . . ? B7 B6 B5 107.24(16) . . ? C1 B6 Na1 113.99(14) . 2_675 ? B12 B6 Na1 69.20(11) . 2_675 ? B7 B6 Na1 69.65(11) . 2_675 ? B5 B6 Na1 112.86(12) . 2_675 ? C1 B7 B8 108.68(18) . . ? C1 B7 B12 101.34(16) . . ? B8 B7 B12 59.30(14) . . ? C1 B7 B6 50.77(12) . . ? B8 B7 B6 104.01(17) . . ? B12 B7 B6 58.64(13) . . ? C1 B7 B2 55.91(13) . . ? B8 B7 B2 60.31(14) . . ? B12 B7 B2 97.85(16) . . ? B6 B7 B2 90.11(15) . . ? C1 B7 Na1 114.41(13) . 2_675 ? B8 B7 Na1 119.06(13) . 2_675 ? B12 B7 Na1 71.41(11) . 2_675 ? B6 B7 Na1 75.10(11) . 2_675 ? B2 B7 Na1 164.74(14) . 2_675 ? B11 B8 B12 60.94(14) . . ? B11 B8 B9 59.84(14) . . ? B12 B8 B9 105.29(17) . . ? B11 B8 B7 116.97(18) . . ? B12 B8 B7 61.09(13) . . ? B9 B8 B7 116.80(18) . . ? B11 B8 B2 107.22(18) . . ? B12 B8 B2 100.15(17) . . ? B9 B8 B2 61.06(14) . . ? B7 B8 B2 62.01(14) . . ? B11 B8 Na2 77.44(13) . 2_675 ? B12 B8 Na2 71.08(11) . 2_675 ? B9 B8 Na2 129.81(15) . 2_675 ? B7 B8 Na2 104.95(13) . 2_675 ? B2 B8 Na2 166.94(14) . 2_675 ? B11 B8 Na1 74.12(12) . . ? B12 B8 Na1 128.28(14) . . ? B9 B8 Na1 68.72(11) . . ? B7 B8 Na1 168.87(15) . . ? B2 B8 Na1 117.30(13) . . ? Na2 B8 Na1 75.58(6) 2_675 . ? B11 B9 B3 106.75(17) . . ? B11 B9 B8 59.31(14) . . ? B3 B9 B8 116.93(18) . . ? B11 B9 B10 59.99(14) . . ? B3 B9 B10 61.36(14) . . ? B8 B9 B10 114.11(18) . . ? B11 B9 B2 106.76(18) . . ? B3 B9 B2 68.47(14) . . ? B8 B9 B2 60.98(14) . . ? B10 B9 B2 118.09(18) . . ? B11 B9 Na2 123.27(15) . . ? B3 B9 Na2 77.74(12) . . ? B8 B9 Na2 164.60(15) . . ? B10 B9 Na2 76.20(12) . . ? B2 B9 Na2 125.77(14) . . ? B11 B9 Na1 78.05(12) . . ? B3 B9 Na1 165.57(16) . . ? B8 B9 Na1 77.34(12) . . ? B10 B9 Na1 112.26(14) . . ? B2 B9 Na1 123.87(14) . . ? Na2 B9 Na1 88.24(7) . . ? C4 B10 B11 108.40(18) . . ? C4 B10 B9 101.12(17) . . ? B11 B10 B9 58.67(14) . . ? C4 B10 B3 51.12(12) . . ? B11 B10 B3 103.37(17) . . ? B9 B10 B3 58.27(13) . . ? C4 B10 B5 56.14(13) . . ? B11 B10 B5 60.58(14) . . ? B9 B10 B5 98.31(16) . . ? B3 B10 B5 91.07(16) . . ? C4 B10 Na2 114.85(14) . . ? B11 B10 Na2 116.19(14) . . ? B9 B10 Na2 68.55(11) . . ? B3 B10 Na2 73.54(11) . . ? B5 B10 Na2 163.41(15) . . ? B8 B11 B9 60.85(14) . . ? B8 B11 B10 116.71(19) . . ? B9 B11 B10 61.34(15) . . ? B8 B11 B12 60.29(14) . . ? B9 B11 B12 105.56(18) . . ? B10 B11 B12 115.70(18) . . ? B8 B11 B5 107.29(18) . . ? B9 B11 B5 100.94(18) . . ? B10 B11 B5 61.85(14) . . ? B12 B11 B5 60.26(14) . . ? B8 B11 Na1 73.23(12) . . ? B9 B11 Na1 68.46(11) . . ? B10 B11 Na1 106.78(13) . . ? B12 B11 Na1 126.97(14) . . ? B5 B11 Na1 167.91(16) . . ? B8 B11 Na2 69.58(12) . 2_675 ? B9 B11 Na2 123.84(14) . 2_675 ? B10 B11 Na2 173.66(16) . 2_675 ? B12 B11 Na2 67.58(11) . 2_675 ? B5 B11 Na2 118.15(14) . 2_675 ? Na1 B11 Na2 73.63(6) . 2_675 ? B8 B12 B6 106.16(17) . . ? B8 B12 B11 58.77(14) . . ? B6 B12 B11 117.65(18) . . ? B8 B12 B7 59.61(13) . . ? B6 B12 B7 61.14(13) . . ? B11 B12 B7 113.66(17) . . ? B8 B12 B5 106.90(17) . . ? B6 B12 B5 69.93(14) . . ? B11 B12 B5 61.28(14) . . ? B7 B12 B5 119.40(17) . . ? B8 B12 Na1 120.50(13) . 2_675 ? B6 B12 Na1 76.34(12) . 2_675 ? B11 B12 Na1 165.98(15) . 2_675 ? B7 B12 Na1 72.92(11) . 2_675 ? B5 B12 Na1 127.61(14) . 2_675 ? B8 B12 Na2 74.30(11) . 2_675 ? B6 B12 Na2 161.97(15) . 2_675 ? B11 B12 Na2 78.46(12) . 2_675 ? B7 B12 Na2 106.20(12) . 2_675 ? B5 B12 Na2 127.69(14) . 2_675 ? Na1 B12 Na2 87.85(7) 2_675 2_675 ? B3 C4 C5 125.73(19) . . ? B3 C4 B10 71.57(16) . . ? C5 C4 B10 131.71(18) . . ? B3 C4 B5 113.25(17) . . ? C5 C4 B5 120.79(17) . . ? B10 C4 B5 69.42(15) . . ? C4 C5 C6 108.50(17) . . ? C11 C6 C7 119.1(2) . . ? C11 C6 C5 122.57(19) . . ? C7 C6 C5 118.1(2) . . ? C8 C7 C6 119.0(3) . . ? C9 C8 C7 122.8(3) . . ? C8 C9 C10 119.1(3) . . ? C11 C10 C9 119.6(2) . . ? C6 C11 C10 120.4(2) . . ? C6 C11 C12 122.5(2) . . ? C10 C11 C12 117.1(2) . . ? C13 C12 C17 118.3(2) . . ? C13 C12 C11 118.2(2) . . ? C17 C12 C11 123.4(2) . . ? C14 C13 C12 120.4(2) . . ? C15 C14 C13 120.3(3) . . ? C14 C15 C16 120.1(3) . . ? C15 C16 C17 122.4(2) . . ? C16 C17 C12 118.6(2) . . ? C16 C17 C18 119.6(2) . . ? C12 C17 C18 121.7(2) . . ? C1 C18 C17 110.83(17) . . ? C31 O3 C34 108.65(16) . . ? C31 O3 Na2 112.16(13) . 2_675 ? C34 O3 Na2 111.62(13) . 2_675 ? C31 O3 Na1 113.50(12) . . ? C34 O3 Na1 110.77(13) . . ? Na2 O3 Na1 99.99(6) 2_675 . ? C32 C31 O3 107.2(2) . . ? C31 C32 C33 108.9(3) . . ? C34 C33 C32 106.0(2) . . ? C33 C34 O3 107.4(2) . . ? C41 O4 C44 107.5(2) . . ? C41 O4 Na2 126.65(19) . . ? C44 O4 Na2 125.06(19) . . ? C42 C41 O4 109.5(4) . . ? C41 C42 C43 107.9(4) . . ? C44 C43 C42 103.6(4) . . ? C43 C44 O4 110.0(3) . . ? C51 O5 C54 108.3(2) . . ? C51 O5 Na1 125.59(16) . . ? C54 O5 Na1 125.91(16) . . ? O5 C51 C52 110.2(3) . . ? C51 C52 C53 105.0(3) . . ? C54 C53 C52 106.7(3) . . ? C53 C54 O5 109.1(3) . . ? C61 O6 C64 106.1(4) . . ? O6 C61 C62 110.5(5) . . ? C61 C62 C63 108.9(4) . . ? C64 C63 C62 99.2(4) . . ? C63 C64 O6 114.1(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.299 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.051 #===END data_13 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H66 B10 Li4 O6' _chemical_formula_weight 706.73 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P(-1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.922(8) _cell_length_b 12.742(8) _cell_length_c 14.538(10) _cell_angle_alpha 88.423(15) _cell_angle_beta 89.103(16) _cell_angle_gamma 86.097(16) _cell_volume 2202(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.9162 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Bruker Smart CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5268 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5248 _reflns_number_gt 2449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart CCD' _computing_cell_refinement 'Bruker Smart CCD' _computing_data_reduction 'Bruker Smart CCD' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.1823P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5248 _refine_ls_number_parameters 527 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1477 _refine_ls_R_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.2874 _refine_ls_wR_factor_gt 0.2420 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.6531(3) 0.9591(3) 0.6345(3) 0.0955(11) Uani 1 1 d . . . O2 O 0.6890(4) 1.1792(4) 0.6331(3) 0.1397(17) Uani 1 1 d . . . O3 O 0.7512(4) 1.0723(3) 0.0501(3) 0.1110(13) Uani 1 1 d . . . O4 O 0.8518(4) 1.4951(3) 0.3913(3) 0.1147(14) Uani 1 1 d . . . O5 O 0.7241(4) 1.4384(3) 0.2198(3) 0.1160(14) Uani 1 1 d . . . O6 O 0.9834(4) 1.4573(3) 0.2094(3) 0.1106(13) Uani 1 1 d . . . C1 C 0.8184(3) 0.9914(3) 0.3227(3) 0.0549(12) Uani 1 1 d . . . C2 C 0.9368(3) 0.9663(3) 0.2779(3) 0.0539(11) Uani 1 1 d . . . C4 C 0.9509(4) 0.8543(3) 0.2393(3) 0.0697(14) Uani 1 1 d . . . H4A H 1.0185 0.8476 0.2014 0.084 Uiso 1 1 calc R . . H4B H 0.9587 0.8031 0.2897 0.084 Uiso 1 1 calc R . . C11 C 0.8499(5) 0.8326(4) 0.1823(4) 0.0789(15) Uani 1 1 d . . . C12 C 0.8596(5) 0.7983(4) 0.0912(4) 0.1020(18) Uani 1 1 d . . . H12A H 0.9304 0.7836 0.0650 0.122 Uiso 1 1 calc R . . C13 C 0.7631(7) 0.7863(6) 0.0396(5) 0.126(2) Uani 1 1 d . . . H13A H 0.7701 0.7666 -0.0214 0.151 Uiso 1 1 calc R . . C14 C 0.6616(7) 0.8028(5) 0.0778(6) 0.123(2) Uani 1 1 d . . . H14A H 0.5985 0.7891 0.0447 0.148 Uiso 1 1 calc R . . C15 C 0.6480(5) 0.8412(4) 0.1685(5) 0.1015(19) Uani 1 1 d . . . H15A H 0.5763 0.8567 0.1927 0.122 Uiso 1 1 calc R . . C16 C 0.7435(5) 0.8556(4) 0.2215(4) 0.0749(15) Uani 1 1 d . . . C3 C 0.7404(4) 0.8995(3) 0.3160(3) 0.0712(14) Uani 1 1 d . . . H3A H 0.7637 0.8442 0.3602 0.085 Uiso 1 1 calc R . . H3B H 0.6639 0.9244 0.3314 0.085 Uiso 1 1 calc R . . C5 C 0.6374(6) 0.9360(7) 0.7300(5) 0.130(2) Uani 1 1 d . . . H5A H 0.5803 0.9854 0.7553 0.156 Uiso 1 1 calc R . . H5B H 0.7070 0.9434 0.7621 0.156 Uiso 1 1 calc R . . C6 C 0.6029(6) 0.8292(8) 0.7432(7) 0.157(3) Uani 1 1 d . . . H6A H 0.6606 0.7850 0.7745 0.188 Uiso 1 1 calc R . . H6B H 0.5336 0.8286 0.7791 0.188 Uiso 1 1 calc R . . C7 C 0.5868(10) 0.7938(6) 0.6521(8) 0.213(6) Uani 1 1 d . . . H7A H 0.5137 0.7653 0.6478 0.256 Uiso 1 1 calc R . . H7B H 0.6441 0.7390 0.6371 0.256 Uiso 1 1 calc R . . C8 C 0.5945(6) 0.8859(6) 0.5869(5) 0.144(3) Uani 1 1 d . . . H8A H 0.6350 0.8652 0.5312 0.173 Uiso 1 1 calc R . . H8B H 0.5202 0.9155 0.5706 0.173 Uiso 1 1 calc R . . C21 C 0.7280(9) 1.2710(7) 0.6672(6) 0.156(3) Uani 1 1 d . . . H21A H 0.7726 1.3052 0.6203 0.187 Uiso 1 1 calc R . . H21B H 0.7753 1.2539 0.7199 0.187 Uiso 1 1 calc R . . C22 C 0.6303(10) 1.3433(9) 0.6949(7) 0.188(4) Uani 1 1 d . . . H22A H 0.6499 1.4160 0.6930 0.225 Uiso 1 1 calc R . . H22B H 0.6035 1.3255 0.7563 0.225 Uiso 1 1 calc R . . C23 C 0.5421(9) 1.3247(12) 0.6226(11) 0.250(6) Uani 1 1 d . . . H23A H 0.4678 1.3204 0.6498 0.300 Uiso 1 1 calc R . . H23B H 0.5399 1.3786 0.5741 0.300 Uiso 1 1 calc R . . C24 C 0.5892(7) 1.2193(9) 0.5882(6) 0.178(4) Uani 1 1 d . . . H24A H 0.5324 1.1687 0.5966 0.214 Uiso 1 1 calc R . . H24B H 0.6050 1.2263 0.5227 0.214 Uiso 1 1 calc R . . C31 C 0.6481(7) 1.1129(10) 0.0274(7) 0.241(6) Uani 1 1 d . . . H31A H 0.6168 1.1582 0.0753 0.289 Uiso 1 1 calc R . . H31B H 0.5979 1.0574 0.0184 0.289 Uiso 1 1 calc R . . C32 C 0.6638(11) 1.1745(14) -0.0599(8) 0.333(11) Uani 1 1 d . . . H32A H 0.6161 1.1501 -0.1072 0.400 Uiso 1 1 calc R . . H32B H 0.6433 1.2484 -0.0504 0.400 Uiso 1 1 calc R . . C33 C 0.7679(12) 1.1620(14) -0.0852(9) 0.323(10) Uani 1 1 d . . . H33A H 0.8048 1.2271 -0.0800 0.387 Uiso 1 1 calc R . . H33B H 0.7742 1.1399 -0.1485 0.387 Uiso 1 1 calc R . . C34 C 0.8157(9) 1.0850(11) -0.0265(7) 0.266(7) Uani 1 1 d . . . H34A H 0.8250 1.0190 -0.0583 0.320 Uiso 1 1 calc R . . H34B H 0.8896 1.1042 -0.0089 0.320 Uiso 1 1 calc R . . C41 C 0.8303(9) 1.4653(6) 0.4853(6) 0.174(4) Uani 1 1 d . . . H41A H 0.7753 1.4125 0.4883 0.209 Uiso 1 1 calc R . . H41B H 0.8990 1.4353 0.5131 0.209 Uiso 1 1 calc R . . C42 C 0.7892(10) 1.5549(8) 0.5340(6) 0.211(5) Uani 1 1 d . . . H42A H 0.8362 1.5649 0.5865 0.253 Uiso 1 1 calc R . . H42B H 0.7130 1.5465 0.5559 0.253 Uiso 1 1 calc R . . C43 C 0.7916(9) 1.6435(6) 0.4711(6) 0.173(4) Uani 1 1 d . . . H43A H 0.7164 1.6762 0.4632 0.208 Uiso 1 1 calc R . . H43B H 0.8389 1.6953 0.4945 0.208 Uiso 1 1 calc R . . C44 C 0.8354(9) 1.6059(6) 0.3853(6) 0.186(4) Uani 1 1 d . . . H44A H 0.7832 1.6265 0.3364 0.223 Uiso 1 1 calc R . . H44B H 0.9063 1.6363 0.3711 0.223 Uiso 1 1 calc R . . C51 C 0.7074(8) 1.5194(8) 0.1569(8) 0.235(6) Uani 1 1 d . . . H51A H 0.7698 1.5175 0.1132 0.282 Uiso 1 1 calc R . . H51B H 0.7062 1.5857 0.1883 0.282 Uiso 1 1 calc R . . C52 C 0.6038(9) 1.5145(8) 0.1077(8) 0.222(5) Uani 1 1 d . . . H52A H 0.6186 1.5011 0.0431 0.267 Uiso 1 1 calc R . . H52B H 0.5575 1.5798 0.1126 0.267 Uiso 1 1 calc R . . C53 C 0.5484(7) 1.4271(7) 0.1524(7) 0.196(4) Uani 1 1 d . . . H53A H 0.4748 1.4509 0.1762 0.236 Uiso 1 1 calc R . . H53B H 0.5394 1.3717 0.1092 0.236 Uiso 1 1 calc R . . C54 C 0.6223(6) 1.3890(7) 0.2276(7) 0.180(4) Uani 1 1 d . . . H54A H 0.5862 1.4048 0.2864 0.216 Uiso 1 1 calc R . . H54B H 0.6368 1.3133 0.2246 0.216 Uiso 1 1 calc R . . C61 C 1.0529(11) 1.5290(11) 0.2282(8) 0.286(8) Uani 1 1 d . . . H61A H 1.0845 1.5135 0.2885 0.343 Uiso 1 1 calc R . . H61B H 1.0115 1.5972 0.2302 0.343 Uiso 1 1 calc R . . C62 C 1.1434(15) 1.5339(17) 0.1609(12) 0.326(10) Uani 1 1 d . . . H62A H 1.1245 1.5851 0.1120 0.391 Uiso 1 1 calc R . . H62B H 1.2128 1.5509 0.1892 0.391 Uiso 1 1 calc R . . C63 C 1.1506(14) 1.4413(9) 0.1314(12) 0.257(8) Uani 1 1 d . . . H63A H 1.1956 1.3945 0.1722 0.308 Uiso 1 1 calc R . . H63B H 1.1842 1.4395 0.0703 0.308 Uiso 1 1 calc R . . C64 C 1.0296(12) 1.4096(9) 0.1296(7) 0.246(7) Uani 1 1 d . . . H64A H 0.9915 1.4369 0.0746 0.295 Uiso 1 1 calc R . . H64B H 1.0263 1.3337 0.1333 0.295 Uiso 1 1 calc R . . B3 B 1.0523(4) 1.0137(4) 0.3161(4) 0.0578(14) Uani 1 1 d . . . H3 H 1.131(3) 0.965(3) 0.302(2) 0.046(10) Uiso 1 1 d . . . B4 B 1.0453(4) 1.1044(4) 0.4030(4) 0.0591(14) Uani 1 1 d . . . H4 H 1.125(3) 1.118(3) 0.445(2) 0.070(11) Uiso 1 1 d . . . B5 B 0.9113(4) 1.1337(4) 0.4546(4) 0.0599(14) Uani 1 1 d . . . H5 H 0.909(3) 1.159(3) 0.526(3) 0.069(12) Uiso 1 1 d . . . B6 B 0.7995(4) 1.0656(4) 0.4116(4) 0.0604(14) Uani 1 1 d . . . H6 H 0.727(4) 1.057(3) 0.456(3) 0.081(13) Uiso 1 1 d . . . B7 B 0.9773(4) 1.0658(4) 0.2174(4) 0.0609(15) Uani 1 1 d . . . H7 H 1.007(4) 1.059(3) 0.155(3) 0.084(14) Uiso 1 1 d . . . B8 B 1.0440(5) 1.1498(4) 0.2854(4) 0.0666(16) Uani 1 1 d . . . H8 H 1.114(4) 1.184(3) 0.255(3) 0.092(14) Uiso 1 1 d . . . B9 B 0.9631(5) 1.2188(4) 0.3667(4) 0.0684(17) Uani 1 1 d . . . H9 H 0.991(3) 1.300(3) 0.381(2) 0.060(10) Uiso 1 1 d . . . B10 B 0.8192(5) 1.1980(4) 0.3706(4) 0.0596(15) Uani 1 1 d . . . H10 H 0.764(3) 1.268(3) 0.385(2) 0.053(11) Uiso 1 1 d . . . B11 B 0.7706(4) 1.1078(4) 0.2960(4) 0.0610(15) Uani 1 1 d . . . H11 H 0.692(4) 1.117(4) 0.269(3) 0.113(17) Uiso 1 1 d . . . B12 B 0.8937(5) 1.1832(4) 0.2575(4) 0.0692(17) Uani 1 1 d . . . H12 H 0.880(3) 1.255(3) 0.208(2) 0.070(11) Uiso 1 1 d . . . Li1 Li 0.9498(6) 0.9494(5) 0.4346(5) 0.0590(19) Uani 1 1 d . . . Li3 Li 0.7860(7) 1.0357(7) 0.5833(6) 0.086(3) Uani 1 1 d . . . Li2 Li 0.8126(7) 1.0361(7) 0.1666(6) 0.083(2) Uani 1 1 d . . . Li4 Li 0.8682(8) 1.3866(6) 0.2904(6) 0.085(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.083(2) 0.109(3) 0.096(3) -0.006(2) 0.009(2) -0.018(2) O2 0.123(4) 0.138(4) 0.159(4) -0.009(3) -0.022(3) -0.012(3) O3 0.100(3) 0.149(4) 0.080(3) 0.006(2) -0.013(2) 0.025(3) O4 0.178(4) 0.049(2) 0.113(3) 0.001(2) 0.027(3) 0.016(2) O5 0.108(3) 0.087(3) 0.151(4) 0.041(3) -0.023(3) 0.000(2) O6 0.136(3) 0.090(3) 0.109(3) 0.007(2) 0.012(3) -0.032(3) C1 0.047(3) 0.045(3) 0.071(3) 0.002(2) -0.005(2) 0.002(2) C2 0.052(3) 0.045(3) 0.063(3) -0.008(2) 0.001(2) 0.010(2) C4 0.064(3) 0.057(3) 0.088(3) -0.006(3) -0.007(3) 0.008(3) C11 0.094(4) 0.047(3) 0.095(4) -0.014(3) -0.019(3) 0.003(3) C12 0.104(5) 0.080(4) 0.122(5) -0.037(4) -0.020(4) 0.016(4) C13 0.124(6) 0.121(6) 0.133(6) -0.059(5) -0.046(5) 0.025(5) C14 0.112(6) 0.109(5) 0.152(7) -0.047(5) -0.059(5) -0.005(5) C15 0.091(4) 0.077(4) 0.139(5) -0.018(4) -0.027(4) -0.013(3) C16 0.072(4) 0.052(3) 0.102(4) -0.006(3) -0.020(3) -0.007(3) C3 0.058(3) 0.058(3) 0.098(4) 0.005(3) -0.009(3) -0.006(2) C5 0.118(5) 0.161(7) 0.113(6) -0.017(5) 0.040(4) -0.031(5) C6 0.108(5) 0.195(9) 0.165(8) 0.040(7) 0.019(5) -0.016(6) C7 0.341(14) 0.098(6) 0.204(10) -0.039(6) 0.156(10) -0.062(7) C8 0.142(6) 0.174(7) 0.128(6) -0.025(6) 0.014(5) -0.083(6) C21 0.191(10) 0.133(7) 0.150(7) -0.014(6) -0.020(6) -0.044(7) C22 0.146(8) 0.190(10) 0.222(10) -0.072(8) 0.020(8) 0.049(8) C23 0.113(8) 0.273(15) 0.354(17) -0.022(13) -0.003(10) 0.072(9) C24 0.093(5) 0.230(10) 0.203(9) -0.034(8) -0.035(6) 0.066(7) C31 0.127(7) 0.399(17) 0.177(9) 0.129(10) -0.005(6) 0.060(9) C32 0.149(9) 0.64(3) 0.184(10) 0.181(15) 0.018(8) 0.108(13) C33 0.174(11) 0.54(3) 0.226(13) 0.205(15) 0.056(10) 0.068(14) C34 0.229(11) 0.417(19) 0.121(7) 0.084(10) 0.054(7) 0.169(12) C41 0.299(12) 0.100(6) 0.122(6) -0.001(5) 0.050(7) -0.010(7) C42 0.380(16) 0.098(6) 0.151(8) -0.014(7) 0.090(9) 0.000(8) C43 0.288(12) 0.091(6) 0.139(7) -0.028(6) -0.005(7) 0.013(7) C44 0.321(13) 0.077(6) 0.149(8) 0.014(5) 0.050(8) 0.050(7) C51 0.181(8) 0.228(10) 0.297(12) 0.161(10) -0.111(9) -0.063(8) C52 0.229(11) 0.192(9) 0.252(11) 0.098(8) -0.126(9) -0.070(8) C53 0.157(7) 0.161(8) 0.271(11) 0.064(8) -0.094(8) -0.021(6) C54 0.111(6) 0.169(7) 0.255(10) 0.100(7) -0.033(6) -0.016(6) C61 0.284(14) 0.377(19) 0.226(11) -0.149(12) 0.115(11) -0.216(15) C62 0.262(17) 0.40(3) 0.335(18) -0.086(19) 0.129(14) -0.19(2) C63 0.251(15) 0.114(8) 0.40(2) -0.047(10) 0.144(14) 0.020(10) C64 0.376(17) 0.242(12) 0.144(7) -0.029(8) 0.086(9) -0.207(12) B3 0.047(3) 0.048(3) 0.076(4) -0.003(3) 0.004(3) 0.010(3) B4 0.052(3) 0.051(3) 0.074(3) 0.006(3) -0.007(3) -0.006(3) B5 0.064(3) 0.048(3) 0.067(3) -0.003(3) -0.004(3) 0.005(3) B6 0.046(3) 0.061(3) 0.073(4) 0.004(3) 0.006(3) -0.001(3) B7 0.062(3) 0.061(4) 0.058(3) 0.000(3) 0.008(3) 0.005(3) B8 0.059(3) 0.063(4) 0.077(4) 0.015(3) 0.002(3) -0.006(3) B9 0.076(4) 0.050(3) 0.080(4) 0.010(3) -0.016(3) -0.013(3) B10 0.060(3) 0.039(3) 0.077(4) 0.002(3) 0.000(3) 0.018(3) B11 0.048(3) 0.055(3) 0.078(4) 0.005(3) -0.004(3) 0.007(3) B12 0.076(4) 0.055(4) 0.076(4) 0.019(3) -0.011(3) -0.012(3) Li1 0.058(4) 0.049(4) 0.070(4) 0.005(4) -0.012(3) -0.002(4) Li3 0.063(5) 0.107(7) 0.085(5) 0.001(5) -0.003(4) 0.008(5) Li2 0.079(5) 0.083(6) 0.088(6) 0.004(5) -0.015(4) -0.001(5) Li4 0.100(6) 0.050(5) 0.103(6) 0.007(4) 0.002(5) 0.010(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 O1 C8 1.405(6) . ? O1 C5 1.422(7) . ? O1 Li3 2.038(9) . ? O2 C21 1.393(7) . ? O2 C24 1.423(8) . ? O2 Li3 2.228(11) . ? O3 C31 1.344(8) . ? O3 C34 1.356(9) . ? O3 Li2 1.890(9) . ? O4 C44 1.412(7) . ? O4 C41 1.432(7) . ? O4 Li4 2.042(10) . ? O5 C51 1.366(8) . ? O5 C54 1.407(7) . ? O5 Li4 2.074(10) . ? O6 C61 1.311(9) . ? O6 C64 1.411(10) . ? O6 Li4 2.037(9) . ? C1 C3 1.551(5) . ? C1 C2 1.562(6) . ? C1 B11 1.592(6) . ? C1 B6 1.626(7) . ? C1 Li1 2.303(7) . ? C1 Li2 2.325(9) . ? C2 C4 1.545(6) . ? C2 B7 1.618(6) . ? C2 B3 1.651(6) . ? C2 Li1 2.290(8) . ? C2 Li2 2.327(9) . ? C4 C11 1.517(6) . ? C11 C16 1.398(7) . ? C11 C12 1.407(7) . ? C11 Li2 2.605(10) . ? C12 C13 1.402(8) . ? C13 C14 1.329(9) . ? C14 C15 1.421(8) . ? C15 C16 1.411(7) . ? C16 C3 1.496(7) . ? C16 Li2 2.595(9) . ? C5 C6 1.456(10) . ? C6 C7 1.431(10) . ? C7 C8 1.495(10) . ? C21 C22 1.493(10) . ? C22 C23 1.533(13) . ? C23 C24 1.515(12) . ? C31 C32 1.489(13) . ? C32 C33 1.291(12) . ? C33 C34 1.381(13) . ? C41 C42 1.415(9) . ? C42 C43 1.434(10) . ? C43 C44 1.427(9) . ? C51 C52 1.444(10) . ? C52 C53 1.466(11) . ? C53 C54 1.466(10) . ? C61 C62 1.448(14) . ? C62 C63 1.263(16) . ? C63 C64 1.525(17) . ? B3 B4 1.733(7) . ? B3 B8 1.775(7) . ? B3 B7 1.789(7) . ? B3 Li1 2.265(8) . ? B3 Li3 2.475(9) 2_776 ? B4 B9 1.774(7) . ? B4 B5 1.774(8) . ? B4 B8 1.790(7) . ? B4 Li1 2.376(8) . ? B4 Li1 2.440(8) 2_776 ? B4 Li3 2.603(10) 2_776 ? B5 B6 1.770(7) . ? B5 B9 1.783(7) . ? B5 B10 1.798(7) . ? B5 Li1 2.388(9) . ? B5 Li1 2.492(8) 2_776 ? B5 Li3 2.708(10) . ? B6 B11 1.782(7) . ? B6 B10 1.802(7) . ? B6 Li1 2.269(8) . ? B6 Li3 2.519(10) . ? B7 B8 1.718(8) . ? B7 B12 1.843(9) . ? B7 Li2 2.170(9) . ? B8 B9 1.735(9) . ? B8 B12 1.861(8) . ? B9 B10 1.754(8) . ? B9 B12 1.883(8) . ? B9 Li4 2.580(9) . ? B10 B11 1.735(8) . ? B10 B12 1.865(8) . ? B10 Li4 2.737(9) . ? B11 B12 1.877(7) . ? B11 Li2 2.150(10) . ? B12 Li2 2.572(10) . ? B12 Li4 2.645(10) . ? Li1 B4 2.440(8) 2_776 ? Li1 B5 2.492(8) 2_776 ? Li1 Li1 2.671(13) 2_776 ? Li1 Li3 3.067(12) . ? Li1 Li3 3.175(11) 2_776 ? Li3 B3 2.475(9) 2_776 ? Li3 B4 2.603(10) 2_776 ? Li3 Li1 3.175(11) 2_776 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 O1 C5 106.7(5) . . ? C8 O1 Li3 125.4(4) . . ? C5 O1 Li3 123.0(4) . . ? C21 O2 C24 101.2(7) . . ? C21 O2 Li3 129.4(6) . . ? C24 O2 Li3 120.8(6) . . ? C31 O3 C34 105.3(6) . . ? C31 O3 Li2 130.3(6) . . ? C34 O3 Li2 122.8(6) . . ? C44 O4 C41 106.6(5) . . ? C44 O4 Li4 130.5(5) . . ? C41 O4 Li4 121.7(5) . . ? C51 O5 C54 106.7(6) . . ? C51 O5 Li4 129.8(5) . . ? C54 O5 Li4 123.4(4) . . ? C61 O6 C64 104.5(6) . . ? C61 O6 Li4 130.8(6) . . ? C64 O6 Li4 121.6(5) . . ? C3 C1 C2 112.8(3) . . ? C3 C1 B11 119.1(3) . . ? C2 C1 B11 111.1(3) . . ? C3 C1 B6 116.6(4) . . ? C2 C1 B6 122.5(3) . . ? B11 C1 B6 67.2(3) . . ? C3 C1 Li1 108.9(3) . . ? C2 C1 Li1 69.7(3) . . ? B11 C1 Li1 124.8(3) . . ? B6 C1 Li1 68.0(3) . . ? C3 C1 Li2 94.9(3) . . ? C2 C1 Li2 70.4(3) . . ? B11 C1 Li2 63.4(3) . . ? B6 C1 Li2 129.9(3) . . ? Li1 C1 Li2 139.0(3) . . ? C4 C2 C1 112.8(3) . . ? C4 C2 B7 120.2(4) . . ? C1 C2 B7 111.4(3) . . ? C4 C2 B3 115.8(4) . . ? C1 C2 B3 122.9(4) . . ? B7 C2 B3 66.4(3) . . ? C4 C2 Li1 107.1(3) . . ? C1 C2 Li1 70.6(3) . . ? B7 C2 Li1 124.4(3) . . ? B3 C2 Li1 67.9(3) . . ? C4 C2 Li2 96.3(3) . . ? C1 C2 Li2 70.3(3) . . ? B7 C2 Li2 63.8(3) . . ? B3 C2 Li2 129.4(3) . . ? Li1 C2 Li2 139.7(4) . . ? C11 C4 C2 110.4(4) . . ? C16 C11 C12 119.9(5) . . ? C16 C11 C4 117.1(5) . . ? C12 C11 C4 122.8(6) . . ? C16 C11 Li2 74.0(3) . . ? C12 C11 Li2 104.7(4) . . ? C4 C11 Li2 86.4(3) . . ? C13 C12 C11 120.4(6) . . ? C14 C13 C12 120.2(7) . . ? C13 C14 C15 121.2(6) . . ? C16 C15 C14 119.8(6) . . ? C11 C16 C15 118.5(5) . . ? C11 C16 C3 116.7(4) . . ? C15 C16 C3 124.8(5) . . ? C11 C16 Li2 74.8(3) . . ? C15 C16 Li2 105.4(4) . . ? C3 C16 Li2 85.9(3) . . ? C16 C3 C1 111.5(4) . . ? O1 C5 C6 110.0(6) . . ? C7 C6 C5 104.6(7) . . ? C6 C7 C8 108.0(7) . . ? O1 C8 C7 105.3(7) . . ? O2 C21 C22 109.4(8) . . ? C21 C22 C23 103.1(8) . . ? C24 C23 C22 99.5(8) . . ? O2 C24 C23 114.0(8) . . ? O3 C31 C32 105.5(7) . . ? C33 C32 C31 108.6(9) . . ? C32 C33 C34 105.6(10) . . ? O3 C34 C33 111.4(9) . . ? C42 C41 O4 109.4(6) . . ? C41 C42 C43 107.0(7) . . ? C44 C43 C42 107.6(7) . . ? O4 C44 C43 109.0(7) . . ? O5 C51 C52 112.4(7) . . ? C51 C52 C53 104.5(7) . . ? C54 C53 C52 105.7(7) . . ? O5 C54 C53 109.2(7) . . ? O6 C61 C62 112.3(9) . . ? C63 C62 C61 101.8(14) . . ? C62 C63 C64 104.8(14) . . ? O6 C64 C63 101.6(8) . . ? C2 B3 B4 120.6(4) . . ? C2 B3 B8 106.5(4) . . ? B4 B3 B8 61.4(3) . . ? C2 B3 B7 56.0(3) . . ? B4 B3 B7 110.4(4) . . ? B8 B3 B7 57.6(3) . . ? C2 B3 Li1 69.6(3) . . ? B4 B3 Li1 71.5(3) . . ? B8 B3 Li1 121.7(4) . . ? B7 B3 Li1 117.3(4) . . ? C2 B3 Li3 140.9(4) . 2_776 ? B4 B3 Li3 74.1(3) . 2_776 ? B8 B3 Li3 111.9(4) . 2_776 ? B7 B3 Li3 158.7(4) . 2_776 ? Li1 B3 Li3 84.0(3) . 2_776 ? B3 B4 B9 109.6(4) . . ? B3 B4 B5 116.9(4) . . ? B9 B4 B5 60.3(3) . . ? B3 B4 B8 60.5(3) . . ? B9 B4 B8 58.3(3) . . ? B5 B4 B8 109.7(4) . . ? B3 B4 Li1 64.7(3) . . ? B9 B4 Li1 117.4(3) . . ? B5 B4 Li1 68.5(3) . . ? B8 B4 Li1 115.4(3) . . ? B3 B4 Li1 122.1(3) . 2_776 ? B9 B4 Li1 120.3(4) . 2_776 ? B5 B4 Li1 70.5(3) . 2_776 ? B8 B4 Li1 177.2(4) . 2_776 ? Li1 B4 Li1 67.3(3) . 2_776 ? B3 B4 Li3 66.1(3) . 2_776 ? B9 B4 Li3 160.3(4) . 2_776 ? B5 B4 Li3 139.3(3) . 2_776 ? B8 B4 Li3 106.0(4) . 2_776 ? Li1 B4 Li3 79.1(3) . 2_776 ? Li1 B4 Li3 74.8(3) 2_776 2_776 ? B6 B5 B4 115.9(4) . . ? B6 B5 B9 109.7(4) . . ? B4 B5 B9 59.8(3) . . ? B6 B5 B10 60.7(3) . . ? B4 B5 B10 109.2(4) . . ? B9 B5 B10 58.6(3) . . ? B6 B5 Li1 64.1(3) . . ? B4 B5 Li1 67.8(3) . . ? B9 B5 Li1 116.4(4) . . ? B10 B5 Li1 114.8(3) . . ? B6 B5 Li1 122.5(3) . 2_776 ? B4 B5 Li1 67.4(3) . 2_776 ? B9 B5 Li1 117.3(3) . 2_776 ? B10 B5 Li1 176.0(4) . 2_776 ? Li1 B5 Li1 66.3(3) . 2_776 ? B6 B5 Li3 64.6(3) . . ? B4 B5 Li3 134.2(3) . . ? B9 B5 Li3 165.9(4) . . ? B10 B5 Li3 108.9(3) . . ? Li1 B5 Li3 73.7(3) . . ? Li1 B5 Li3 75.1(3) 2_776 . ? C1 B6 B5 120.8(4) . . ? C1 B6 B11 55.5(3) . . ? B5 B6 B11 110.1(4) . . ? C1 B6 B10 106.1(4) . . ? B5 B6 B10 60.4(3) . . ? B11 B6 B10 57.9(3) . . ? C1 B6 Li1 70.3(3) . . ? B5 B6 Li1 71.3(3) . . ? B11 B6 Li1 117.2(4) . . ? B10 B6 Li1 120.5(3) . . ? C1 B6 Li3 135.8(4) . . ? B5 B6 Li3 76.1(3) . . ? B11 B6 Li3 163.2(4) . . ? B10 B6 Li3 117.0(4) . . ? Li1 B6 Li3 79.5(3) . . ? C2 B7 B8 110.7(4) . . ? C2 B7 B3 57.7(3) . . ? B8 B7 B3 60.8(3) . . ? C2 B7 B12 106.9(4) . . ? B8 B7 B12 62.9(3) . . ? B3 B7 B12 105.5(4) . . ? C2 B7 Li2 74.2(3) . . ? B8 B7 Li2 141.9(5) . . ? B3 B7 Li2 131.1(4) . . ? B12 B7 Li2 79.3(4) . . ? B7 B8 B9 117.5(4) . . ? B7 B8 B3 61.6(3) . . ? B9 B8 B3 109.4(4) . . ? B7 B8 B4 111.1(4) . . ? B9 B8 B4 60.4(3) . . ? B3 B8 B4 58.2(3) . . ? B7 B8 B12 61.8(3) . . ? B9 B8 B12 63.0(3) . . ? B3 B8 B12 105.3(3) . . ? B4 B8 B12 106.0(4) . . ? B8 B9 B10 116.6(4) . . ? B8 B9 B4 61.4(3) . . ? B10 B9 B4 111.3(3) . . ? B8 B9 B5 111.8(4) . . ? B10 B9 B5 61.1(3) . . ? B4 B9 B5 59.8(3) . . ? B8 B9 B12 61.8(3) . . ? B10 B9 B12 61.6(3) . . ? B4 B9 B12 105.8(4) . . ? B5 B9 B12 105.8(3) . . ? B8 B9 Li4 109.5(3) . . ? B10 B9 Li4 75.6(3) . . ? B4 B9 Li4 170.1(4) . . ? B5 B9 Li4 129.8(4) . . ? B12 B9 Li4 70.7(3) . . ? B11 B10 B9 117.7(4) . . ? B11 B10 B5 111.0(4) . . ? B9 B10 B5 60.3(3) . . ? B11 B10 B6 60.5(3) . . ? B9 B10 B6 109.6(4) . . ? B5 B10 B6 58.9(3) . . ? B11 B10 B12 62.7(3) . . ? B9 B10 B12 62.6(3) . . ? B5 B10 B12 105.9(4) . . ? B6 B10 B12 105.2(4) . . ? B11 B10 Li4 115.0(3) . . ? B9 B10 Li4 66.0(3) . . ? B5 B10 Li4 120.6(3) . . ? B6 B10 Li4 172.2(4) . . ? B12 B10 Li4 67.1(3) . . ? C1 B11 B10 110.9(4) . . ? C1 B11 B6 57.3(3) . . ? B10 B11 B6 61.6(3) . . ? C1 B11 B12 107.1(4) . . ? B10 B11 B12 62.0(3) . . ? B6 B11 B12 105.5(3) . . ? C1 B11 Li2 75.2(3) . . ? B10 B11 Li2 140.8(4) . . ? B6 B11 Li2 131.7(4) . . ? B12 B11 Li2 79.1(3) . . ? B7 B12 B10 126.8(4) . . ? B7 B12 B8 55.3(3) . . ? B10 B12 B8 105.6(3) . . ? B7 B12 B11 94.2(3) . . ? B10 B12 B11 55.3(3) . . ? B8 B12 B11 126.5(4) . . ? B7 B12 B9 104.8(4) . . ? B10 B12 B9 55.8(3) . . ? B8 B12 B9 55.2(3) . . ? B11 B12 B9 105.2(4) . . ? B7 B12 Li2 56.0(3) . . ? B10 B12 Li2 110.3(3) . . ? B8 B12 Li2 111.1(4) . . ? B11 B12 Li2 55.2(3) . . ? B9 B12 Li2 146.2(3) . . ? B7 B12 Li4 152.0(4) . . ? B10 B12 Li4 72.4(3) . . ? B8 B12 Li4 102.8(3) . . ? B11 B12 Li4 113.7(4) . . ? B9 B12 Li4 67.1(3) . . ? Li2 B12 Li4 143.2(3) . . ? B3 Li1 B6 94.6(3) . . ? B3 Li1 C2 42.5(2) . . ? B6 Li1 C2 75.7(3) . . ? B3 Li1 C1 76.3(3) . . ? B6 Li1 C1 41.7(2) . . ? C2 Li1 C1 39.77(18) . . ? B3 Li1 B4 43.8(2) . . ? B6 Li1 B4 80.6(3) . . ? C2 Li1 B4 78.0(3) . . ? C1 Li1 B4 92.7(3) . . ? B3 Li1 B5 79.9(3) . . ? B6 Li1 B5 44.6(2) . . ? C2 Li1 B5 92.6(3) . . ? C1 Li1 B5 78.0(3) . . ? B4 Li1 B5 43.7(2) . . ? B3 Li1 B4 144.2(3) . 2_776 ? B6 Li1 B4 108.8(3) . 2_776 ? C2 Li1 B4 168.7(3) . 2_776 ? C1 Li1 B4 138.7(3) . 2_776 ? B4 Li1 B4 112.7(3) . 2_776 ? B5 Li1 B4 97.8(3) . 2_776 ? B3 Li1 B5 105.9(3) . 2_776 ? B6 Li1 B5 147.3(4) . 2_776 ? C2 Li1 B5 136.0(4) . 2_776 ? C1 Li1 B5 168.3(4) . 2_776 ? B4 Li1 B5 96.7(3) . 2_776 ? B5 Li1 B5 113.7(3) . 2_776 ? B4 Li1 B5 42.2(2) 2_776 2_776 ? B3 Li1 Li1 95.6(4) . 2_776 ? B6 Li1 Li1 98.5(4) . 2_776 ? C2 Li1 Li1 135.4(4) . 2_776 ? C1 Li1 Li1 136.7(4) . 2_776 ? B4 Li1 Li1 57.5(3) . 2_776 ? B5 Li1 Li1 58.7(3) . 2_776 ? B4 Li1 Li1 55.2(3) 2_776 2_776 ? B5 Li1 Li1 55.0(3) 2_776 2_776 ? B3 Li1 Li3 137.7(4) . . ? B6 Li1 Li3 53.9(3) . . ? C2 Li1 Li3 129.0(3) . . ? C1 Li1 Li3 90.6(3) . . ? B4 Li1 Li3 98.4(3) . . ? B5 Li1 Li3 57.9(3) . . ? B4 Li1 Li3 55.0(2) 2_776 . ? B5 Li1 Li3 94.9(3) 2_776 . ? Li1 Li1 Li3 66.8(3) 2_776 . ? B3 Li1 Li3 50.8(2) . 2_776 ? B6 Li1 Li3 134.0(3) . 2_776 ? C2 Li1 Li3 89.5(3) . 2_776 ? C1 Li1 Li3 127.0(3) . 2_776 ? B4 Li1 Li3 53.6(2) . 2_776 ? B5 Li1 Li3 94.3(3) . 2_776 ? B4 Li1 Li3 94.2(3) 2_776 2_776 ? B5 Li1 Li3 55.5(2) 2_776 2_776 ? Li1 Li1 Li3 62.6(3) 2_776 2_776 ? Li3 Li1 Li3 129.4(2) . 2_776 ? O1 Li3 O2 84.3(4) . . ? O1 Li3 B3 107.0(4) . 2_776 ? O2 Li3 B3 111.0(4) . 2_776 ? O1 Li3 B6 117.9(4) . . ? O2 Li3 B6 104.2(4) . . ? B3 Li3 B6 124.7(4) 2_776 . ? O1 Li3 B4 103.7(4) . 2_776 ? O2 Li3 B4 150.8(4) . 2_776 ? B3 Li3 B4 39.8(2) 2_776 2_776 ? B6 Li3 B4 96.8(3) . 2_776 ? O1 Li3 B5 156.9(4) . . ? O2 Li3 B5 97.0(4) . . ? B3 Li3 B5 94.1(3) 2_776 . ? B6 Li3 B5 39.4(2) . . ? B4 Li3 B5 86.4(3) 2_776 . ? O1 Li3 Li1 124.4(4) . . ? O2 Li3 Li1 144.7(4) . . ? B3 Li3 Li1 82.1(3) 2_776 . ? B6 Li3 Li1 46.7(2) . . ? B4 Li3 Li1 50.2(2) 2_776 . ? B5 Li3 Li1 48.4(2) . . ? O1 Li3 Li1 149.0(4) . 2_776 ? O2 Li3 Li1 115.8(4) . 2_776 ? B3 Li3 Li1 45.2(2) 2_776 2_776 ? B6 Li3 Li1 81.6(3) . 2_776 ? B4 Li3 Li1 47.3(2) 2_776 2_776 ? B5 Li3 Li1 49.3(2) . 2_776 ? Li1 Li3 Li1 50.6(3) . 2_776 ? O3 Li2 B11 127.7(5) . . ? O3 Li2 B7 128.3(5) . . ? B11 Li2 B7 78.2(3) . . ? O3 Li2 C1 159.0(5) . . ? B11 Li2 C1 41.5(2) . . ? B7 Li2 C1 71.4(3) . . ? O3 Li2 C2 160.3(5) . . ? B11 Li2 C2 70.9(3) . . ? B7 Li2 C2 42.0(2) . . ? C1 Li2 C2 39.24(19) . . ? O3 Li2 B12 117.6(4) . . ? B11 Li2 B12 45.8(2) . . ? B7 Li2 B12 44.7(3) . . ? C1 Li2 B12 69.4(3) . . ? C2 Li2 B12 69.1(3) . . ? O3 Li2 C16 108.9(4) . . ? B11 Li2 C16 93.0(3) . . ? B7 Li2 C16 113.6(4) . . ? C1 Li2 C16 61.3(2) . . ? C2 Li2 C16 72.6(3) . . ? B12 Li2 C16 130.7(4) . . ? O3 Li2 C11 109.7(4) . . ? B11 Li2 C11 112.7(4) . . ? B7 Li2 C11 93.2(3) . . ? C1 Li2 C11 72.3(3) . . ? C2 Li2 C11 61.0(2) . . ? B12 Li2 C11 130.1(3) . . ? C16 Li2 C11 31.20(18) . . ? O6 Li4 O4 98.4(4) . . ? O6 Li4 O5 98.7(4) . . ? O4 Li4 O5 96.4(4) . . ? O6 Li4 B9 109.0(4) . . ? O4 Li4 B9 105.8(4) . . ? O5 Li4 B9 141.0(4) . . ? O6 Li4 B12 106.4(4) . . ? O4 Li4 B12 144.5(4) . . ? O5 Li4 B12 104.3(4) . . ? B9 Li4 B12 42.2(2) . . ? O6 Li4 B10 143.2(4) . . ? O4 Li4 B10 106.5(4) . . ? O5 Li4 B10 104.9(4) . . ? B9 Li4 B10 38.4(2) . . ? B12 Li4 B10 40.5(2) . . ? _diffrn_measured_fraction_theta_max 0.757 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.757 _refine_diff_density_max 0.274 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.046 #===END data_14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H60 B10 Li4 O6' _chemical_formula_weight 652.64 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P(-1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.429(3) _cell_length_b 12.784(3) _cell_length_c 14.486(4) _cell_angle_alpha 69.766(5) _cell_angle_beta 79.778(6) _cell_angle_gamma 86.327(7) _cell_volume 1954.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.8367 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Bruker Smart CCD' _diffrn_measurement_method 'omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9748 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0917 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6105 _reflns_number_gt 2882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart CCD' _computing_cell_refinement 'Bruker Smart CCD' _computing_data_reduction 'Bruker Smart CCD' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.1392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6105 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1515 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2518 _refine_ls_wR_factor_gt 0.2023 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.192 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.17369(14) 0.40225(15) 0.40191(13) 0.0563(5) Uani 1 1 d . . . O2 O 0.15192(15) 0.61830(16) 0.38084(13) 0.0585(5) Uani 1 1 d . . . O3 O 0.20477(18) 0.34979(19) 1.01176(14) 0.0780(7) Uani 1 1 d . . . O4 O 0.3470(2) 0.78028(18) 0.87761(16) 0.0947(8) Uani 1 1 d . . . O5 O 0.4878(2) 0.91173(19) 0.67527(19) 0.1044(8) Uani 1 1 d . . . O6 O 0.2182(2) 0.89622(19) 0.69604(19) 0.1001(8) Uani 1 1 d . . . B3 B 0.2731(2) 0.4799(2) 0.6087(2) 0.0394(7) Uani 1 1 d . A . H3 H 0.2100(16) 0.4554(15) 0.5717(13) 0.025(5) Uiso 1 1 d . . . B4 B 0.3705(2) 0.5922(2) 0.5454(2) 0.0383(7) Uani 1 1 d . . . H4 H 0.3715(16) 0.6453(16) 0.4616(14) 0.032(6) Uiso 1 1 d . . . B5 B 0.5057(2) 0.5899(2) 0.5889(2) 0.0409(8) Uani 1 1 d . . . H5 H 0.5849(18) 0.6403(18) 0.5368(15) 0.050(7) Uiso 1 1 d . . . B6 B 0.5304(2) 0.4752(2) 0.6926(2) 0.0392(7) Uani 1 1 d . . . H6 H 0.6228(17) 0.4458(16) 0.7051(14) 0.033(6) Uiso 1 1 d . . . B7 B 0.2179(2) 0.4819(2) 0.7310(2) 0.0426(8) Uani 1 1 d . . . H7 H 0.1295(18) 0.4684(18) 0.7679(15) 0.044(6) Uiso 1 1 d . . . B8 B 0.2476(2) 0.6063(2) 0.6362(2) 0.0425(8) Uani 1 1 d . A . H8 H 0.1647(18) 0.6661(18) 0.6160(15) 0.044(6) Uiso 1 1 d . . . B9 B 0.3829(3) 0.6706(2) 0.6225(2) 0.0432(8) Uani 1 1 d . . . H9 H 0.387(2) 0.766(2) 0.5925(18) 0.077(9) Uiso 1 1 d . . . B10 B 0.4742(2) 0.6017(2) 0.7108(2) 0.0428(8) Uani 1 1 d . A . H10 H 0.5240(19) 0.6558(19) 0.7361(16) 0.053(7) Uiso 1 1 d . . . B11 B 0.4274(2) 0.4762(2) 0.8004(2) 0.0426(8) Uani 1 1 d . . . H11 H 0.4402(18) 0.4572(18) 0.8741(15) 0.044(6) Uiso 1 1 d . . . B12 B 0.3099(2) 0.5833(2) 0.7509(2) 0.0441(8) Uani 1 1 d . A . H12 H 0.2624(17) 0.6313(17) 0.7983(14) 0.038(6) Uiso 1 1 d . . . Li1 Li 0.4615(3) 0.4152(3) 0.5829(3) 0.0416(11) Uani 1 1 d . . . Li3 Li 0.2873(4) 0.5037(4) 0.4308(3) 0.0517(13) Uani 1 1 d . . . Li2 Li 0.2688(4) 0.3831(4) 0.8741(3) 0.0594(14) Uani 1 1 d . A . Li4 Li 0.3618(5) 0.7908(4) 0.7320(4) 0.0686(15) Uani 1 1 d . A . C1 C 0.4247(2) 0.38215(19) 0.75040(17) 0.0380(7) Uani 1 1 d . A . C2 C 0.3052(2) 0.38571(19) 0.71087(16) 0.0366(6) Uani 1 1 d . A . C4 C 0.2554(2) 0.2697(2) 0.73281(18) 0.0488(7) Uani 1 1 d . . . H4A H 0.1736 0.2768 0.7215 0.059 Uiso 1 1 calc R A . H4B H 0.3008 0.2360 0.6871 0.059 Uiso 1 1 calc R . . C11 C 0.2598(2) 0.1950(2) 0.83792(19) 0.0515(8) Uani 1 1 d . A . C12 C 0.1630(3) 0.1349(3) 0.9028(2) 0.0718(10) Uani 1 1 d . . . H12A H 0.0905 0.1396 0.8809 0.086 Uiso 1 1 calc R A . C13 C 0.1730(4) 0.0677(3) 1.0003(2) 0.0912(13) Uani 1 1 d . A . H13A H 0.1077 0.0283 1.0434 0.109 Uiso 1 1 calc R . . C14 C 0.2804(4) 0.0606(3) 1.0316(3) 0.0935(13) Uani 1 1 d . . . H14A H 0.2888 0.0137 1.0955 0.112 Uiso 1 1 calc R A . C15 C 0.3757(3) 0.1220(3) 0.9696(2) 0.0735(10) Uani 1 1 d . A . H15A H 0.4471 0.1181 0.9931 0.088 Uiso 1 1 calc R . . C16 C 0.3679(2) 0.1895(2) 0.87265(19) 0.0519(8) Uani 1 1 d . . . C3 C 0.4667(2) 0.2628(2) 0.80180(19) 0.0506(8) Uani 1 1 d . A . H3A H 0.4998 0.2303 0.7513 0.061 Uiso 1 1 calc R . . H3B H 0.5293 0.2653 0.8382 0.061 Uiso 1 1 calc R . . C21 C 0.1556(3) 0.2901(3) 0.4626(3) 0.0875(12) Uani 1 1 d . . . H21A H 0.1013 0.2568 0.4375 0.131 Uiso 1 1 calc R . . H21B H 0.1231 0.2860 0.5296 0.131 Uiso 1 1 calc R . . H21C H 0.2301 0.2509 0.4622 0.131 Uiso 1 1 calc R . . C22 C 0.0657(2) 0.4577(3) 0.3817(2) 0.0620(9) Uani 1 1 d . . . H22A H 0.0124 0.4509 0.4435 0.074 Uiso 1 1 calc R . . H22B H 0.0274 0.4251 0.3434 0.074 Uiso 1 1 calc R . . C23 C 0.0929(2) 0.5764(3) 0.3241(2) 0.0668(9) Uani 1 1 d . . . H23A H 0.1429 0.5834 0.2608 0.080 Uiso 1 1 calc R . . H23B H 0.0200 0.6178 0.3110 0.080 Uiso 1 1 calc R . . C24 C 0.1743(3) 0.7326(3) 0.3393(3) 0.0927(13) Uani 1 1 d . . . H24A H 0.1028 0.7715 0.3205 0.139 Uiso 1 1 calc R . . H24B H 0.2350 0.7472 0.2814 0.139 Uiso 1 1 calc R . . H24C H 0.2004 0.7579 0.3874 0.139 Uiso 1 1 calc R . . C31 C 0.0868(4) 0.3552(4) 1.0492(3) 0.1266(16) Uani 1 1 d . . . H31A H 0.0491 0.2836 1.0661 0.152 Uiso 1 1 calc R . . H31B H 0.0466 0.4107 1.0003 0.152 Uiso 1 1 calc R . . C32 C 0.0806(4) 0.3863(4) 1.1398(3) 0.145(2) Uani 1 1 d . . . H32A H 0.0788 0.4667 1.1230 0.174 Uiso 1 1 calc R . . H32B H 0.0106 0.3547 1.1883 0.174 Uiso 1 1 calc R . . C33 C 0.1876(4) 0.3396(4) 1.1777(3) 0.1378(19) Uani 1 1 d . . . H33A H 0.1733 0.2655 1.2267 0.165 Uiso 1 1 calc R . . H33B H 0.2184 0.3865 1.2081 0.165 Uiso 1 1 calc R . . C34 C 0.2709(3) 0.3355(3) 1.0882(2) 0.1019(13) Uani 1 1 d . . . H34A H 0.3296 0.3942 1.0677 0.122 Uiso 1 1 calc R . . H34B H 0.3120 0.2644 1.1030 0.122 Uiso 1 1 calc R . . C41 C 0.2910(7) 0.8458(7) 0.9291(5) 0.094(2) Uiso 0.50 1 d P A 1 H41A H 0.2323 0.8936 0.8937 0.113 Uiso 0.50 1 calc PR A 1 H41B H 0.3475 0.8917 0.9404 0.113 Uiso 0.50 1 calc PR A 1 C41' C 0.2187(7) 0.8013(7) 0.9277(5) 0.098(2) Uiso 0.50 1 d P A 2 H41C H 0.1991 0.8801 0.9068 0.118 Uiso 0.50 1 calc PR A 2 H41D H 0.1594 0.7612 0.9130 0.118 Uiso 0.50 1 calc PR A 2 C42 C 0.2293(5) 0.7579(5) 1.0319(3) 0.169(2) Uani 1 1 d . . . H42A H 0.2390 0.7793 1.0881 0.203 Uiso 1 1 calc R A 1 H42B H 0.1451 0.7509 1.0323 0.203 Uiso 1 1 calc R A 1 C43 C 0.2931(4) 0.6536(4) 1.0345(3) 0.135(2) Uani 1 1 d . A . H43A H 0.3230 0.6198 1.0969 0.162 Uiso 1 1 calc R . . H43B H 0.2416 0.6008 1.0268 0.162 Uiso 1 1 calc R . . C44 C 0.3891(3) 0.6871(3) 0.9518(3) 0.1000(12) Uani 1 1 d . A . H44A H 0.4579 0.7077 0.9723 0.120 Uiso 1 1 calc R . . H44B H 0.4113 0.6266 0.9261 0.120 Uiso 1 1 calc R . . C51 C 0.5900(4) 0.9040(4) 0.6085(4) 0.1312(17) Uani 1 1 d . A . H51A H 0.5723 0.9264 0.5412 0.157 Uiso 1 1 calc R . . H51B H 0.6193 0.8279 0.6267 0.157 Uiso 1 1 calc R . . C52 C 0.6766(5) 0.9760(5) 0.6134(5) 0.202(3) Uani 1 1 d . . . H52A H 0.7041 1.0292 0.5477 0.243 Uiso 1 1 calc R A . H52B H 0.7443 0.9334 0.6389 0.243 Uiso 1 1 calc R . . C53 C 0.6200(5) 1.0323(5) 0.6789(4) 0.197(2) Uani 1 1 d . A . H53A H 0.6634 1.0191 0.7337 0.237 Uiso 1 1 calc R . . H53B H 0.6181 1.1119 0.6433 0.237 Uiso 1 1 calc R . . C54 C 0.5092(5) 0.9928(4) 0.7138(4) 0.235(2) Uani 1 1 d . A . H54A H 0.4528 1.0535 0.6956 0.282 Uiso 1 1 calc R . . H54B H 0.4980 0.9612 0.7860 0.282 Uiso 1 1 calc R . . C61 C 0.2036(5) 1.0086(4) 0.6825(4) 0.152(2) Uani 1 1 d . A . H61A H 0.2412 1.0539 0.6164 0.182 Uiso 1 1 calc R . . H61B H 0.2371 1.0275 0.7317 0.182 Uiso 1 1 calc R . . C62 C 0.0733(5) 1.0250(6) 0.6955(6) 0.229(3) Uani 1 1 d . . . H62A H 0.0391 1.0045 0.7656 0.275 Uiso 1 1 calc R A . H62B H 0.0530 1.1020 0.6615 0.275 Uiso 1 1 calc R . . C63 C 0.0333(5) 0.9552(6) 0.6532(6) 0.265(3) Uani 1 1 d . A . H63A H 0.0311 0.9933 0.5828 0.318 Uiso 1 1 calc R . . H63B H -0.0452 0.9265 0.6869 0.318 Uiso 1 1 calc R . . C64 C 0.1197(5) 0.8688(5) 0.6677(6) 0.254(3) Uani 1 1 d . A . H64A H 0.0846 0.8017 0.7185 0.304 Uiso 1 1 calc R . . H64B H 0.1433 0.8529 0.6062 0.304 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 O1 0.0465(10) 0.0658(12) 0.0624(10) -0.0267(9) -0.0133(8) -0.0010(9) O2 0.0493(10) 0.0663(12) 0.0671(10) -0.0300(9) -0.0167(8) 0.0088(9) O3 0.0764(13) 0.1032(16) 0.0522(11) -0.0308(11) -0.0014(10) 0.0148(12) O4 0.139(2) 0.0763(14) 0.0784(13) -0.0476(11) 0.0005(13) 0.0007(14) O5 0.0838(15) 0.0965(14) 0.1569(18) -0.0874(12) 0.0170(13) -0.0216(12) O6 0.0875(15) 0.0701(14) 0.1591(19) -0.0629(13) -0.0192(14) 0.0161(12) B3 0.0366(15) 0.0442(16) 0.0463(14) -0.0279(12) -0.0073(12) 0.0087(12) B4 0.0417(15) 0.0401(16) 0.0385(14) -0.0209(12) -0.0085(12) 0.0097(12) B5 0.0370(15) 0.0473(16) 0.0443(15) -0.0253(13) -0.0026(12) 0.0019(13) B6 0.0361(14) 0.0441(16) 0.0461(14) -0.0257(12) -0.0110(12) 0.0096(12) B7 0.0315(15) 0.0534(17) 0.0517(15) -0.0313(13) -0.0045(12) 0.0074(13) B8 0.0397(15) 0.0435(16) 0.0527(16) -0.0275(13) -0.0110(12) 0.0121(13) B9 0.0474(17) 0.0400(16) 0.0477(15) -0.0228(13) -0.0075(13) 0.0041(13) B10 0.0438(16) 0.0494(16) 0.0464(14) -0.0308(12) -0.0083(12) 0.0037(13) B11 0.0399(15) 0.0540(17) 0.0419(14) -0.0270(13) -0.0098(12) 0.0115(13) B12 0.0426(16) 0.0485(17) 0.0496(15) -0.0300(13) -0.0065(13) 0.0120(13) Li1 0.039(2) 0.044(2) 0.045(2) -0.0203(18) -0.0090(17) 0.0057(18) Li3 0.040(2) 0.066(3) 0.054(2) -0.025(2) -0.0114(19) 0.005(2) Li2 0.060(3) 0.072(3) 0.051(2) -0.027(2) -0.007(2) 0.003(2) Li4 0.081(3) 0.066(3) 0.072(3) -0.045(2) -0.004(2) -0.008(3) C1 0.0387(13) 0.0360(13) 0.0429(12) -0.0173(10) -0.0113(10) 0.0086(10) C2 0.0367(13) 0.0386(13) 0.0385(12) -0.0196(10) -0.0038(10) 0.0017(10) C4 0.0458(15) 0.0501(15) 0.0576(14) -0.0287(12) -0.0065(12) 0.0018(12) C11 0.0670(17) 0.0370(15) 0.0503(14) -0.0194(12) 0.0000(13) -0.0014(13) C12 0.081(2) 0.0599(19) 0.0717(19) -0.0248(15) 0.0041(16) -0.0143(16) C13 0.131(3) 0.067(2) 0.066(2) -0.0199(17) 0.014(2) -0.033(2) C14 0.154(3) 0.056(2) 0.062(2) -0.0068(17) -0.016(2) -0.021(2) C15 0.105(2) 0.0472(19) 0.0680(18) -0.0147(15) -0.0259(17) 0.0026(17) C16 0.0661(17) 0.0386(15) 0.0522(15) -0.0178(12) -0.0122(13) 0.0105(13) C3 0.0528(15) 0.0491(16) 0.0542(14) -0.0227(12) -0.0146(12) 0.0135(12) C21 0.100(2) 0.066(2) 0.099(2) -0.0256(19) -0.024(2) -0.0101(19) C22 0.0389(15) 0.096(2) 0.0664(15) -0.0452(14) -0.0118(12) 0.0024(14) C23 0.0485(16) 0.088(2) 0.0716(17) -0.0314(16) -0.0264(14) 0.0141(15) C24 0.084(2) 0.054(2) 0.132(3) -0.020(2) -0.027(2) 0.0150(18) C31 0.089(3) 0.191(4) 0.120(3) -0.093(3) 0.009(2) 0.017(3) C32 0.136(4) 0.193(4) 0.109(3) -0.077(3) 0.010(3) 0.041(3) C33 0.190(4) 0.144(4) 0.073(2) -0.044(2) -0.008(3) 0.045(4) C34 0.116(3) 0.127(3) 0.074(2) -0.050(2) -0.0279(19) 0.043(2) C42 0.181(4) 0.203(5) 0.084(3) -0.025(3) 0.003(3) 0.087(4) C43 0.145(4) 0.131(4) 0.108(3) -0.023(3) -0.006(3) 0.007(3) C44 0.111(3) 0.114(3) 0.099(2) -0.061(2) -0.043(2) 0.036(2) C51 0.095(3) 0.135(3) 0.167(4) -0.078(3) 0.035(3) -0.031(3) C52 0.116(4) 0.217(5) 0.310(7) -0.155(5) 0.027(4) -0.054(4) C53 0.169(5) 0.217(4) 0.270(5) -0.175(4) 0.011(4) -0.070(4) C54 0.185(4) 0.245(3) 0.356(5) -0.259(3) 0.115(4) -0.126(3) C61 0.176(4) 0.068(3) 0.210(5) -0.046(3) -0.042(4) 0.028(3) C62 0.159(4) 0.250(6) 0.301(7) -0.133(5) -0.061(5) 0.127(4) C63 0.194(5) 0.295(7) 0.436(8) -0.240(6) -0.193(5) 0.119(5) C64 0.118(4) 0.157(4) 0.574(10) -0.218(5) -0.115(5) 0.057(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C21 1.404(4) . ? O1 C22 1.409(3) . ? O1 Li3 2.081(5) . ? O2 C24 1.396(4) . ? O2 C23 1.402(4) . ? O2 Li3 2.106(5) . ? O3 C31 1.368(4) . ? O3 C34 1.404(4) . ? O3 Li2 1.904(5) . ? O4 C41 1.365(8) . ? O4 C44 1.425(4) . ? O4 C41' 1.567(8) . ? O4 Li4 2.044(5) . ? O5 C54 1.388(5) . ? O5 C51 1.401(4) . ? O5 Li4 2.030(5) . ? O6 C64 1.368(6) . ? O6 C61 1.384(5) . ? O6 Li4 2.078(6) . ? B3 C2 1.636(3) . ? B3 B4 1.752(4) . ? B3 B7 1.779(4) . ? B3 B8 1.788(4) . ? B3 Li1 2.272(5) . ? B3 Li3 2.465(5) . ? B4 B5 1.764(4) . ? B4 B9 1.767(4) . ? B4 B8 1.792(4) . ? B4 Li1 2.355(5) . ? B4 Li1 2.446(5) 2_666 ? B4 Li3 2.633(6) . ? B5 B6 1.749(4) . ? B5 B9 1.786(4) . ? B5 B10 1.796(4) . ? B5 Li1 2.355(5) . ? B5 Li1 2.473(5) 2_666 ? B5 Li3 2.598(5) 2_666 ? B6 C1 1.647(4) . ? B6 B11 1.784(4) . ? B6 B10 1.789(4) . ? B6 Li1 2.258(5) . ? B6 Li3 2.455(5) 2_666 ? B7 C2 1.606(4) . ? B7 B8 1.710(4) . ? B7 B12 1.847(4) . ? B7 Li2 2.181(5) . ? B8 B9 1.746(4) . ? B8 B12 1.846(4) . ? B9 B10 1.754(4) . ? B9 B12 1.880(4) . ? B9 Li4 2.537(6) . ? B10 B11 1.722(4) . ? B10 B12 1.869(4) . ? B10 Li4 2.750(6) . ? B11 C1 1.608(4) . ? B11 B12 1.903(4) . ? B11 Li2 2.134(5) . ? B12 Li2 2.580(5) . ? B12 Li4 2.666(6) . ? Li1 C1 2.279(5) . ? Li1 C2 2.280(4) . ? Li1 B4 2.446(5) 2_666 ? Li1 B5 2.473(5) 2_666 ? Li1 Li1 2.672(7) 2_666 ? Li1 Li3 3.065(6) 2_666 ? Li1 Li3 3.105(6) . ? Li3 B6 2.455(5) 2_666 ? Li3 B5 2.598(5) 2_666 ? Li3 Li1 3.065(6) 2_666 ? Li2 C1 2.294(5) . ? Li2 C2 2.316(5) . ? Li2 C11 2.644(6) . ? Li2 C16 2.660(6) . ? C1 C3 1.537(3) . ? C1 C2 1.564(3) . ? C2 C4 1.531(3) . ? C4 C11 1.499(3) . ? C11 C12 1.392(4) . ? C11 C16 1.403(4) . ? C12 C13 1.397(4) . ? C13 C14 1.369(5) . ? C14 C15 1.373(5) . ? C15 C16 1.386(4) . ? C16 C3 1.504(3) . ? C22 C23 1.479(4) . ? C31 C32 1.488(6) . ? C32 C33 1.439(6) . ? C33 C34 1.481(5) . ? C41 C42 1.596(8) . ? C41' C42 1.440(8) . ? C42 C43 1.470(7) . ? C43 C44 1.435(5) . ? C51 C52 1.421(7) . ? C52 C53 1.425(8) . ? C53 C54 1.339(7) . ? C61 C62 1.478(7) . ? C62 C63 1.382(10) . ? C63 C64 1.419(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 O1 C22 111.8(2) . . ? C21 O1 Li3 121.4(2) . . ? C22 O1 Li3 110.7(2) . . ? C24 O2 C23 114.2(2) . . ? C24 O2 Li3 121.2(2) . . ? C23 O2 Li3 107.2(2) . . ? C31 O3 C34 108.6(3) . . ? C31 O3 Li2 124.9(3) . . ? C34 O3 Li2 125.6(2) . . ? C41 O4 C44 104.4(4) . . ? C41 O4 C41' 40.8(4) . . ? C44 O4 C41' 104.0(3) . . ? C41 O4 Li4 132.4(4) . . ? C44 O4 Li4 123.0(3) . . ? C41' O4 Li4 114.9(4) . . ? C54 O5 C51 107.1(3) . . ? C54 O5 Li4 127.8(3) . . ? C51 O5 Li4 122.4(3) . . ? C64 O6 C61 104.2(4) . . ? C64 O6 Li4 124.9(3) . . ? C61 O6 Li4 130.5(3) . . ? C2 B3 B4 118.8(2) . . ? C2 B3 B7 55.91(15) . . ? B4 B3 B7 109.2(2) . . ? C2 B3 B8 105.7(2) . . ? B4 B3 B8 60.79(16) . . ? B7 B3 B8 57.30(16) . . ? C2 B3 Li1 69.19(15) . . ? B4 B3 Li1 70.30(16) . . ? B7 B3 Li1 116.41(19) . . ? B8 B3 Li1 119.9(2) . . ? C2 B3 Li3 138.5(2) . . ? B4 B3 Li3 75.13(17) . . ? B7 B3 Li3 161.8(2) . . ? B8 B3 Li3 114.42(19) . . ? Li1 B3 Li3 81.80(16) . . ? B3 B4 B5 117.6(2) . . ? B3 B4 B9 110.61(19) . . ? B5 B4 B9 60.76(17) . . ? B3 B4 B8 60.58(16) . . ? B5 B4 B8 110.3(2) . . ? B9 B4 B8 58.75(16) . . ? B3 B4 Li1 65.24(16) . . ? B5 B4 Li1 67.97(17) . . ? B9 B4 Li1 117.67(19) . . ? B8 B4 Li1 115.65(18) . . ? B3 B4 Li1 122.5(2) . 2_666 ? B5 B4 Li1 69.80(16) . 2_666 ? B9 B4 Li1 119.38(19) . 2_666 ? B8 B4 Li1 176.6(2) . 2_666 ? Li1 B4 Li1 67.59(16) . 2_666 ? B3 B4 Li3 64.82(16) . . ? B5 B4 Li3 136.73(19) . . ? B9 B4 Li3 162.5(2) . . ? B8 B4 Li3 107.12(18) . . ? Li1 B4 Li3 76.77(16) . . ? Li1 B4 Li3 74.14(15) 2_666 . ? B6 B5 B4 116.8(2) . . ? B6 B5 B9 110.40(19) . . ? B4 B5 B9 59.70(16) . . ? B6 B5 B10 60.61(16) . . ? B4 B5 B10 108.93(19) . . ? B9 B5 B10 58.66(16) . . ? B6 B5 Li1 64.82(16) . . ? B4 B5 Li1 68.03(17) . . ? B9 B5 Li1 116.89(19) . . ? B10 B5 Li1 114.98(18) . . ? B6 B5 Li1 123.2(2) . 2_666 ? B4 B5 Li1 68.16(16) . 2_666 ? B9 B5 Li1 117.23(19) . 2_666 ? B10 B5 Li1 175.8(2) . 2_666 ? Li1 B5 Li1 67.16(17) . 2_666 ? B6 B5 Li3 65.42(15) . 2_666 ? B4 B5 Li3 136.4(2) . 2_666 ? B9 B5 Li3 163.9(2) . 2_666 ? B10 B5 Li3 108.40(18) . 2_666 ? Li1 B5 Li3 76.30(16) . 2_666 ? Li1 B5 Li3 75.48(15) 2_666 2_666 ? C1 B6 B5 119.8(2) . . ? C1 B6 B11 55.72(16) . . ? B5 B6 B11 110.33(19) . . ? C1 B6 B10 105.64(19) . . ? B5 B6 B10 61.00(16) . . ? B11 B6 B10 57.63(15) . . ? C1 B6 Li1 69.40(17) . . ? B5 B6 Li1 70.69(17) . . ? B11 B6 Li1 116.77(19) . . ? B10 B6 Li1 120.02(19) . . ? C1 B6 Li3 138.1(2) . 2_666 ? B5 B6 Li3 74.21(16) . 2_666 ? B11 B6 Li3 162.2(2) . 2_666 ? B10 B6 Li3 114.85(19) . 2_666 ? Li1 B6 Li3 81.02(17) . 2_666 ? C2 B7 B8 110.9(2) . . ? C2 B7 B3 57.54(15) . . ? B8 B7 B3 61.61(16) . . ? C2 B7 B12 107.35(19) . . ? B8 B7 B12 62.38(17) . . ? B3 B7 B12 106.31(19) . . ? C2 B7 Li2 73.65(19) . . ? B8 B7 Li2 141.1(2) . . ? B3 B7 Li2 130.5(2) . . ? B12 B7 Li2 79.16(19) . . ? B7 B8 B9 117.8(2) . . ? B7 B8 B3 61.09(16) . . ? B9 B8 B3 110.0(2) . . ? B7 B8 B4 110.6(2) . . ? B9 B8 B4 59.93(16) . . ? B3 B8 B4 58.63(15) . . ? B7 B8 B12 62.44(17) . . ? B9 B8 B12 63.06(16) . . ? B3 B8 B12 105.99(19) . . ? B4 B8 B12 105.63(19) . . ? B8 B9 B10 116.0(2) . . ? B8 B9 B4 61.32(17) . . ? B10 B9 B4 110.7(2) . . ? B8 B9 B5 111.4(2) . . ? B10 B9 B5 60.95(16) . . ? B4 B9 B5 59.55(16) . . ? B8 B9 B12 61.07(16) . . ? B10 B9 B12 61.80(16) . . ? B4 B9 B12 105.2(2) . . ? B5 B9 B12 105.73(19) . . ? B8 B9 Li4 109.9(2) . . ? B10 B9 Li4 77.33(19) . . ? B4 B9 Li4 169.8(2) . . ? B5 B9 Li4 130.6(2) . . ? B12 B9 Li4 72.54(17) . . ? B11 B10 B9 118.7(2) . . ? B11 B10 B6 61.06(16) . . ? B9 B10 B6 110.0(2) . . ? B11 B10 B5 111.0(2) . . ? B9 B10 B5 60.39(16) . . ? B6 B10 B5 58.39(16) . . ? B11 B10 B12 63.83(16) . . ? B9 B10 B12 62.41(16) . . ? B6 B10 B12 106.4(2) . . ? B5 B10 B12 105.8(2) . . ? B11 B10 Li4 117.08(19) . . ? B9 B10 Li4 64.17(17) . . ? B6 B10 Li4 172.8(2) . . ? B5 B10 Li4 118.69(19) . . ? B12 B10 Li4 67.42(17) . . ? C1 B11 B10 110.6(2) . . ? C1 B11 B6 57.82(16) . . ? B10 B11 B6 61.31(16) . . ? C1 B11 B12 106.2(2) . . ? B10 B11 B12 61.85(16) . . ? B6 B11 B12 105.16(18) . . ? C1 B11 Li2 74.1(2) . . ? B10 B11 Li2 140.7(2) . . ? B6 B11 Li2 131.3(2) . . ? B12 B11 Li2 79.21(19) . . ? B8 B12 B7 55.18(15) . . ? B8 B12 B10 106.03(18) . . ? B7 B12 B10 126.1(2) . . ? B8 B12 B9 55.87(15) . . ? B7 B12 B9 105.1(2) . . ? B10 B12 B9 55.80(15) . . ? B8 B12 B11 126.5(2) . . ? B7 B12 B11 94.11(19) . . ? B10 B12 B11 54.32(14) . . ? B9 B12 B11 104.51(18) . . ? B8 B12 Li2 111.1(2) . . ? B7 B12 Li2 56.15(16) . . ? B10 B12 Li2 108.52(18) . . ? B9 B12 Li2 145.3(2) . . ? B11 B12 Li2 54.36(15) . . ? B8 B12 Li4 101.59(18) . . ? B7 B12 Li4 151.7(2) . . ? B10 B12 Li4 72.24(17) . . ? B9 B12 Li4 65.19(16) . . ? B11 B12 Li4 113.9(2) . . ? Li2 B12 Li4 145.1(2) . . ? B6 Li1 B3 95.93(19) . . ? B6 Li1 C1 42.58(12) . . ? B3 Li1 C1 76.75(15) . . ? B6 Li1 C2 76.72(16) . . ? B3 Li1 C2 42.13(11) . . ? C1 Li1 C2 40.12(11) . . ? B6 Li1 B5 44.49(13) . . ? B3 Li1 B5 81.10(17) . . ? C1 Li1 B5 78.67(16) . . ? C2 Li1 B5 93.10(17) . . ? B6 Li1 B4 80.83(17) . . ? B3 Li1 B4 44.46(12) . . ? C1 Li1 B4 93.18(17) . . ? C2 Li1 B4 77.99(15) . . ? B5 Li1 B4 44.00(13) . . ? B6 Li1 B4 107.77(18) . 2_666 ? B3 Li1 B4 144.1(2) . 2_666 ? C1 Li1 B4 138.4(2) . 2_666 ? C2 Li1 B4 169.0(2) . 2_666 ? B5 Li1 B4 97.04(16) . 2_666 ? B4 Li1 B4 112.41(16) . 2_666 ? B6 Li1 B5 146.0(2) . 2_666 ? B3 Li1 B5 105.59(18) . 2_666 ? C1 Li1 B5 168.4(2) . 2_666 ? C2 Li1 B5 136.2(2) . 2_666 ? B5 Li1 B5 112.84(17) . 2_666 ? B4 Li1 B5 96.28(16) . 2_666 ? B4 Li1 B5 42.04(11) 2_666 2_666 ? B6 Li1 Li1 98.0(2) . 2_666 ? B3 Li1 Li1 96.4(2) . 2_666 ? C1 Li1 Li1 137.2(3) . 2_666 ? C2 Li1 Li1 135.7(3) . 2_666 ? B5 Li1 Li1 58.53(17) . 2_666 ? B4 Li1 Li1 57.81(16) . 2_666 ? B4 Li1 Li1 54.59(15) 2_666 2_666 ? B5 Li1 Li1 54.31(16) 2_666 2_666 ? B6 Li1 Li3 52.29(14) . 2_666 ? B3 Li1 Li3 136.4(2) . 2_666 ? C1 Li1 Li3 90.69(16) . 2_666 ? C2 Li1 Li3 128.8(2) . 2_666 ? B5 Li1 Li3 55.42(14) . 2_666 ? B4 Li1 Li3 96.18(17) . 2_666 ? B4 Li1 Li3 55.72(13) 2_666 2_666 ? B5 Li1 Li3 94.92(15) 2_666 2_666 ? Li1 Li1 Li3 65.12(17) 2_666 2_666 ? B6 Li1 Li3 136.3(2) . . ? B3 Li1 Li3 51.79(13) . . ? C1 Li1 Li3 128.26(18) . . ? C2 Li1 Li3 89.82(15) . . ? B5 Li1 Li3 96.37(17) . . ? B4 Li1 Li3 55.63(14) . . ? B4 Li1 Li3 93.30(16) 2_666 . ? B5 Li1 Li3 54.08(13) 2_666 . ? Li1 Li1 Li3 63.57(17) 2_666 . ? Li3 Li1 Li3 128.69(14) 2_666 . ? O1 Li3 O2 79.30(16) . . ? O1 Li3 B6 106.9(2) . 2_666 ? O2 Li3 B6 114.17(19) . 2_666 ? O1 Li3 B3 114.53(19) . . ? O2 Li3 B3 105.1(2) . . ? B6 Li3 B3 126.9(2) 2_666 . ? O1 Li3 B5 104.0(2) . 2_666 ? O2 Li3 B5 154.5(2) . 2_666 ? B6 Li3 B5 40.37(11) 2_666 2_666 ? B3 Li3 B5 96.60(17) . 2_666 ? O1 Li3 B4 154.2(2) . . ? O2 Li3 B4 101.0(2) . . ? B6 Li3 B4 96.63(17) 2_666 . ? B3 Li3 B4 40.04(11) . . ? B5 Li3 B4 86.89(16) 2_666 . ? O1 Li3 Li1 150.4(2) . 2_666 ? O2 Li3 Li1 120.6(2) . 2_666 ? B6 Li3 Li1 46.69(12) 2_666 2_666 ? B3 Li3 Li1 83.13(16) . 2_666 ? B5 Li3 Li1 48.27(12) 2_666 2_666 ? B4 Li3 Li1 50.14(12) . 2_666 ? O1 Li3 Li1 123.8(2) . . ? O2 Li3 Li1 147.2(2) . . ? B6 Li3 Li1 83.38(15) 2_666 . ? B3 Li3 Li1 46.40(12) . . ? B5 Li3 Li1 50.44(12) 2_666 . ? B4 Li3 Li1 47.60(12) . . ? Li1 Li3 Li1 51.31(14) 2_666 . ? O3 Li2 B11 124.6(3) . . ? O3 Li2 B7 137.2(3) . . ? B11 Li2 B7 79.00(18) . . ? O3 Li2 C1 150.5(3) . . ? B11 Li2 C1 42.39(13) . . ? B7 Li2 C1 71.78(16) . . ? O3 Li2 C2 163.1(3) . . ? B11 Li2 C2 71.97(16) . . ? B7 Li2 C2 41.71(12) . . ? C1 Li2 C2 39.65(11) . . ? O3 Li2 B12 123.3(3) . . ? B11 Li2 B12 46.44(13) . . ? B7 Li2 B12 44.68(14) . . ? C1 Li2 B12 70.21(14) . . ? C2 Li2 B12 69.12(14) . . ? O3 Li2 C11 105.9(2) . . ? B11 Li2 C11 113.5(2) . . ? B7 Li2 C11 92.2(2) . . ? C1 Li2 C11 72.03(16) . . ? C2 Li2 C11 60.48(14) . . ? B12 Li2 C11 129.6(2) . . ? O3 Li2 C16 101.8(2) . . ? B11 Li2 C16 93.91(19) . . ? B7 Li2 C16 112.3(2) . . ? C1 Li2 C16 60.89(14) . . ? C2 Li2 C16 71.82(16) . . ? B12 Li2 C16 131.02(19) . . ? C11 Li2 C16 30.68(10) . . ? O5 Li4 O4 96.7(2) . . ? O5 Li4 O6 96.1(2) . . ? O4 Li4 O6 98.0(2) . . ? O5 Li4 B9 109.2(2) . . ? O4 Li4 B9 141.8(2) . . ? O6 Li4 B9 106.3(2) . . ? O5 Li4 B12 144.9(3) . . ? O4 Li4 B12 101.7(2) . . ? O6 Li4 B12 110.4(2) . . ? B9 Li4 B12 42.27(12) . . ? O5 Li4 B10 105.3(2) . . ? O4 Li4 B10 108.5(2) . . ? O6 Li4 B10 143.2(3) . . ? B9 Li4 B10 38.49(12) . . ? B12 Li4 B10 40.34(11) . . ? C3 C1 C2 112.8(2) . . ? C3 C1 B11 120.5(2) . . ? C2 C1 B11 111.29(19) . . ? C3 C1 B6 115.86(19) . . ? C2 C1 B6 122.53(19) . . ? B11 C1 B6 66.47(17) . . ? C3 C1 Li1 107.25(19) . . ? C2 C1 Li1 69.97(15) . . ? B11 C1 Li1 124.30(19) . . ? B6 C1 Li1 68.02(16) . . ? C3 C1 Li2 96.35(18) . . ? C2 C1 Li2 70.92(17) . . ? B11 C1 Li2 63.47(18) . . ? B6 C1 Li2 129.3(2) . . ? Li1 C1 Li2 139.72(19) . . ? C4 C2 C1 113.00(19) . . ? C4 C2 B7 119.6(2) . . ? C1 C2 B7 111.8(2) . . ? C4 C2 B3 114.5(2) . . ? C1 C2 B3 123.98(19) . . ? B7 C2 B3 66.55(17) . . ? C4 C2 Li1 107.82(19) . . ? C1 C2 Li1 69.91(15) . . ? B7 C2 Li1 124.47(18) . . ? B3 C2 Li1 68.67(15) . . ? C4 C2 Li2 96.49(18) . . ? C1 C2 Li2 69.42(17) . . ? B7 C2 Li2 64.64(18) . . ? B3 C2 Li2 130.5(2) . . ? Li1 C2 Li2 138.21(19) . . ? C11 C4 C2 112.1(2) . . ? C12 C11 C16 118.9(3) . . ? C12 C11 C4 124.0(3) . . ? C16 C11 C4 117.0(2) . . ? C12 C11 Li2 107.1(2) . . ? C16 C11 Li2 75.29(19) . . ? C4 C11 Li2 84.70(18) . . ? C11 C12 C13 121.1(3) . . ? C14 C13 C12 119.0(3) . . ? C13 C14 C15 120.6(3) . . ? C14 C15 C16 121.4(3) . . ? C15 C16 C11 118.9(3) . . ? C15 C16 C3 124.5(3) . . ? C11 C16 C3 116.6(2) . . ? C15 C16 Li2 109.3(2) . . ? C11 C16 Li2 74.03(19) . . ? C3 C16 Li2 83.29(18) . . ? C16 C3 C1 112.6(2) . . ? O1 C22 C23 107.8(2) . . ? O2 C23 C22 107.9(2) . . ? O3 C31 C32 106.7(4) . . ? C33 C32 C31 103.9(4) . . ? C32 C33 C34 103.9(3) . . ? O3 C34 C33 108.1(3) . . ? O4 C41 C42 103.5(5) . . ? C42 C41' O4 101.4(5) . . ? C41' C42 C43 99.3(5) . . ? C41' C42 C41 39.6(4) . . ? C43 C42 C41 103.2(4) . . ? C44 C43 C42 104.3(4) . . ? O4 C44 C43 106.5(3) . . ? O5 C51 C52 107.4(4) . . ? C51 C52 C53 106.5(5) . . ? C54 C53 C52 107.9(5) . . ? C53 C54 O5 110.9(5) . . ? O6 C61 C62 104.1(4) . . ? C63 C62 C61 104.2(6) . . ? C62 C63 C64 102.6(6) . . ? O6 C64 C63 112.3(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.330 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.048 #===END data_15 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H13 Li N2 O' _chemical_formula_weight 160.14 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.900(3) _cell_length_b 9.559(3) _cell_length_c 11.956(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.452(6) _cell_angle_gamma 90.00 _cell_volume 985.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4238 _diffrn_reflns_av_R_equivalents 0.0855 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1291 _reflns_number_gt 944 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1581P)^2^+0.2221P] 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 1291 _refine_ls_number_parameters 117 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.2738 _refine_ls_wR_factor_gt 0.2469 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _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 C1 C 0.7173(4) 0.2652(4) 0.3004(3) 0.0706(11) Uani 1 1 d . . . C2 C 0.8158(5) 0.1998(4) 0.2424(3) 0.0737(11) Uani 1 1 d . . . H2 H 0.916(7) 0.218(5) 0.272(4) 0.122(17) Uiso 1 1 d . . . C3 C 0.7595(4) 0.1059(3) 0.1542(3) 0.0600(10) Uani 1 1 d . . . C4 C 0.8748(5) 0.0418(5) 0.0956(4) 0.0880(13) Uani 1 1 d . . . H4A H 0.8222 -0.0224 0.0371 0.132 Uiso 1 1 calc R . . H4B H 0.9531 -0.0073 0.1517 0.132 Uiso 1 1 calc R . . H4C H 0.9225 0.1143 0.0608 0.132 Uiso 1 1 calc R . . C5 C 0.3029(6) 0.1203(6) 0.3841(5) 0.1173(18) Uani 1 1 d . . . H5A H 0.3878 0.0761 0.3601 0.141 Uiso 1 1 calc R . . H5B H 0.2318 0.1599 0.3166 0.141 Uiso 1 1 calc R . . C6 C 0.2215(10) 0.0163(7) 0.4404(7) 0.157(3) Uani 1 1 d . . . H6A H 0.1262 -0.0152 0.3877 0.189 Uiso 1 1 calc R . . H6B H 0.2870 -0.0640 0.4676 0.189 Uiso 1 1 calc R . . C7 C 0.1892(9) 0.0952(8) 0.5374(7) 0.170(3) Uani 1 1 d . . . H7A H 0.0880 0.1393 0.5146 0.204 Uiso 1 1 calc R . . H7B H 0.1916 0.0337 0.6024 0.204 Uiso 1 1 calc R . . C8 C 0.3074(8) 0.1971(6) 0.5670(5) 0.129(2) Uani 1 1 d . . . H8A H 0.3924 0.1627 0.6282 0.155 Uiso 1 1 calc R . . H8B H 0.2673 0.2819 0.5936 0.155 Uiso 1 1 calc R . . O1 O 0.3593(4) 0.2249(3) 0.4659(3) 0.0997(12) Uani 1 1 d . . . N1 N 0.6323(4) 0.3160(4) 0.3464(3) 0.0882(11) Uani 1 1 d . . . N2 N 0.6152(4) 0.0641(3) 0.1164(2) 0.0638(9) Uani 1 1 d . . . H2 H 0.564(4) 0.098(4) 0.151(3) 0.059(11) Uiso 1 1 d . . . Li1 Li 0.4948(7) 0.3795(5) 0.4458(5) 0.0673(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.083(2) 0.070(2) 0.058(2) -0.0130(17) 0.0166(19) -0.0058(19) C2 0.065(2) 0.084(2) 0.075(2) -0.0115(19) 0.0235(18) -0.0023(18) C3 0.066(2) 0.0621(19) 0.0578(19) 0.0058(14) 0.0267(15) 0.0061(15) C4 0.085(3) 0.104(3) 0.085(3) -0.011(2) 0.039(2) 0.015(2) C5 0.119(4) 0.120(4) 0.113(4) -0.035(3) 0.029(3) -0.033(3) C6 0.193(6) 0.103(4) 0.187(6) -0.042(4) 0.067(5) -0.072(4) C7 0.199(7) 0.161(6) 0.161(6) -0.003(5) 0.066(5) -0.099(6) C8 0.164(5) 0.131(4) 0.103(4) -0.005(3) 0.054(3) -0.058(4) O1 0.138(3) 0.0766(18) 0.096(2) -0.0138(14) 0.0515(18) -0.0412(16) N1 0.102(2) 0.090(2) 0.078(2) -0.0257(17) 0.033(2) 0.0029(19) N2 0.073(2) 0.0673(18) 0.0586(18) -0.0077(13) 0.0295(15) 0.0066(14) Li1 0.092(4) 0.054(3) 0.061(3) -0.007(2) 0.028(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.148(5) . ? C1 C2 1.394(6) . ? C2 C3 1.380(5) . ? C3 N2 1.313(4) . ? C3 C4 1.509(5) . ? C5 O1 1.401(5) . ? C5 C6 1.485(9) . ? C6 C7 1.471(10) . ? C7 C8 1.412(8) . ? C8 O1 1.423(6) . ? O1 Li1 1.960(6) . ? N1 Li1 2.001(7) . ? N2 Li1 2.064(6) 2_645 ? N2 Li1 2.123(6) 4_565 ? Li1 N2 2.064(6) 2_655 ? Li1 N2 2.123(6) 4_566 ? Li1 Li1 2.633(10) 3_666 ? 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 C1 C2 177.7(4) . . ? C3 C2 C1 121.2(3) . . ? N2 C3 C2 126.7(3) . . ? N2 C3 C4 115.9(3) . . ? C2 C3 C4 117.4(3) . . ? O1 C5 C6 107.0(5) . . ? C7 C6 C5 103.2(4) . . ? C8 C7 C6 105.7(6) . . ? C7 C8 O1 107.2(5) . . ? C5 O1 C8 108.9(4) . . ? C5 O1 Li1 125.3(3) . . ? C8 O1 Li1 125.8(3) . . ? C1 N1 Li1 170.5(4) . . ? C3 N2 Li1 136.0(3) . 2_645 ? C3 N2 Li1 118.0(3) . 4_565 ? Li1 N2 Li1 77.9(2) 2_645 4_565 ? O1 Li1 N1 109.3(3) . . ? O1 Li1 N2 116.0(3) . 2_655 ? N1 Li1 N2 110.5(3) . 2_655 ? O1 Li1 N2 104.6(3) . 4_566 ? N1 Li1 N2 114.2(3) . 4_566 ? N2 Li1 N2 102.1(2) 2_655 4_566 ? O1 Li1 Li1 123.1(4) . 3_666 ? N1 Li1 Li1 127.3(4) . 3_666 ? N2 Li1 Li1 52.0(2) 2_655 3_666 ? N2 Li1 Li1 50.06(19) 4_566 3_666 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.272 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.047 #===END data_16 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H61 B10 K O8' _chemical_formula_weight 696.99 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 26.977(2) _cell_length_b 12.8293(10) _cell_length_c 11.6629(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4036.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.174 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5350 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16931 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4857 _reflns_number_gt 1967 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.31(16) _refine_ls_number_reflns 4857 _refine_ls_number_parameters 442 _refine_ls_number_restraints 133 _refine_ls_R_factor_all 0.1706 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.2548 _refine_ls_wR_factor_gt 0.1917 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.104 _refine_ls_shift/su_mean 0.019 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 K1 K 0.091511(19) 0.22590(5) 0.66575(11) 0.1014(2) Uani 1 1 d . . . O1 O -0.00264(6) 0.15151(17) 0.6636(3) 0.1964(13) Uani 1 1 d D . . O2 O 0.04188(9) 0.2082(2) 0.8793(2) 0.1805(12) Uani 1 1 d D . . O3 O 0.14129(9) 0.27272(16) 0.87193(18) 0.1235(9) Uani 1 1 d D . . O4 O 0.18178(7) 0.33278(15) 0.6586(3) 0.1584(10) Uani 1 1 d D . . O5 O 0.13547(11) 0.2648(2) 0.4500(3) 0.1926(15) Uani 1 1 d D . . O6 O 0.03859(9) 0.2144(2) 0.4575(3) 0.1868(12) Uani 1 1 d D . . O8 O 0.05121(10) 0.42319(17) 0.6672(3) 0.2152(12) Uani 1 1 d D . . C1 C 0.17699(13) -0.2721(4) 0.6124(3) 0.198(2) Uani 1 1 d . . . H1 H 0.1547 -0.3283 0.6311 0.237 Uiso 1 1 d . . . C2 C 0.18535(13) -0.2394(2) 0.7282(2) 0.0977(11) Uani 1 1 d . . . C3 C 0.20910(13) -0.3323(2) 0.7883(2) 0.1303(14) Uani 1 1 d . . . H3A H 0.2220 -0.3089 0.8615 0.156 Uiso 1 1 calc R . . H3B H 0.1835 -0.3834 0.8039 0.156 Uiso 1 1 calc R . . C4 C 0.24858(12) -0.3831(2) 0.7263(2) 0.0926(11) Uani 1 1 d . . . C5 C 0.28918(14) -0.4309(2) 0.7830(3) 0.1340(16) Uani 1 1 d . . . H5A H 0.2907 -0.4238 0.8622 0.161 Uiso 1 1 calc R . . C6 C 0.32651(11) -0.4866(2) 0.7313(3) 0.1293(15) Uani 1 1 d . . . H6A H 0.3491 -0.5270 0.7721 0.155 Uiso 1 1 calc R . . C7 C 0.32747(12) -0.4772(3) 0.6139(3) 0.1419(17) Uani 1 1 d . . . H7A H 0.3560 -0.4995 0.5763 0.170 Uiso 1 1 calc R . . C8 C 0.28913(13) -0.4370(2) 0.5462(3) 0.1186(14) Uani 1 1 d . . . H8A H 0.2881 -0.4441 0.4669 0.142 Uiso 1 1 calc R . . C9 C 0.25342(11) -0.3866(2) 0.6072(3) 0.0949(11) Uani 1 1 d . . . C10 C 0.21109(13) -0.3340(2) 0.5393(2) 0.1160(14) Uani 1 1 d . . . H10A H 0.2254 -0.2886 0.4816 0.139 Uiso 1 1 calc R . . H10B H 0.1922 -0.3873 0.4999 0.139 Uiso 1 1 calc R . . C31 C -0.02572(12) 0.1438(5) 0.7703(4) 0.339(3) Uani 1 1 d D . . H31A H -0.0459 0.2056 0.7819 0.407 Uiso 1 1 calc R . . H31B H -0.0479 0.0843 0.7690 0.407 Uiso 1 1 calc R . . C32 C 0.00573(14) 0.1335(4) 0.8618(5) 0.345(5) Uani 1 1 d D . . H32A H 0.0222 0.0667 0.8546 0.414 Uiso 1 1 calc R . . H32B H -0.0144 0.1304 0.9306 0.414 Uiso 1 1 calc R . . C33 C 0.07114(17) 0.1975(4) 0.9748(3) 0.257(3) Uani 1 1 d D . . H33A H 0.0843 0.1272 0.9792 0.309 Uiso 1 1 calc R . . H33B H 0.0520 0.2111 1.0436 0.309 Uiso 1 1 calc R . . C34 C 0.10991(16) 0.2698(3) 0.9647(4) 0.196(2) Uani 1 1 d D . . H34A H 0.0950 0.3384 0.9705 0.235 Uiso 1 1 calc R . . H34B H 0.1306 0.2612 1.0320 0.235 Uiso 1 1 calc R . . C35 C 0.18177(13) 0.3386(3) 0.8567(4) 0.213(2) Uani 1 1 d D . . H35A H 0.2039 0.3312 0.9218 0.256 Uiso 1 1 calc R . . H35B H 0.1702 0.4101 0.8552 0.256 Uiso 1 1 calc R . . C36 C 0.20834(16) 0.3183(4) 0.7557(3) 0.206(2) Uani 1 1 d D . . H36A H 0.2372 0.3634 0.7536 0.247 Uiso 1 1 calc R . . H36B H 0.2200 0.2469 0.7577 0.247 Uiso 1 1 calc R . . C37 C 0.20672(11) 0.3224(4) 0.5583(3) 0.222(2) Uani 1 1 d D . . H37A H 0.2227 0.2548 0.5543 0.267 Uiso 1 1 calc R . . H37B H 0.2319 0.3760 0.5515 0.267 Uiso 1 1 calc R . . C38 C 0.17209(15) 0.3325(4) 0.4718(5) 0.233(3) Uani 1 1 d D . . H38A H 0.1562 0.3995 0.4838 0.279 Uiso 1 1 calc R . . H38B H 0.1908 0.3387 0.4011 0.279 Uiso 1 1 calc R . . C39 C 0.10667(17) 0.2724(4) 0.3575(4) 0.299(4) Uani 1 1 d D . . H39A H 0.1257 0.2585 0.2886 0.359 Uiso 1 1 calc R . . H39B H 0.0926 0.3417 0.3519 0.359 Uiso 1 1 calc R . . C40 C 0.06990(15) 0.1994(3) 0.3706(4) 0.211(3) Uani 1 1 d D . . H40A H 0.0508 0.1969 0.3002 0.253 Uiso 1 1 calc R . . H40B H 0.0854 0.1318 0.3804 0.253 Uiso 1 1 calc R . . C41 C 0.00062(14) 0.1491(3) 0.4607(4) 0.204(2) Uani 1 1 d D . . H41A H 0.0128 0.0780 0.4578 0.245 Uiso 1 1 calc R . . H41B H -0.0203 0.1604 0.3942 0.245 Uiso 1 1 calc R . . C42 C -0.02722(15) 0.1631(5) 0.5601(4) 0.253(3) Uani 1 1 d D . . H42A H -0.0414 0.2325 0.5579 0.304 Uiso 1 1 calc R . . H42B H -0.0545 0.1139 0.5585 0.304 Uiso 1 1 calc R . . C61 C 0.0526(2) 0.4772(4) 0.5656(4) 0.257(3) Uani 1 1 d D . . H61A H 0.0448 0.4314 0.5020 0.309 Uiso 1 1 calc R . . H61B H 0.0854 0.5063 0.5532 0.309 Uiso 1 1 calc R . . C62 C 0.01497(19) 0.5623(4) 0.5747(4) 0.352(5) Uani 1 1 d D . . H62A H 0.0271 0.6268 0.5417 0.422 Uiso 1 1 calc R . . H62B H -0.0158 0.5430 0.5374 0.422 Uiso 1 1 calc R . . C63 C 0.00852(16) 0.5714(3) 0.7021(4) 0.261(3) Uani 1 1 d D . . H63A H 0.0199 0.6390 0.7286 0.313 Uiso 1 1 calc R . . H63B H -0.0261 0.5635 0.7227 0.313 Uiso 1 1 calc R . . C64 C 0.0381(2) 0.4883(4) 0.7535(4) 0.318(4) Uani 1 1 d D . . H64A H 0.0674 0.5170 0.7900 0.382 Uiso 1 1 calc R . . H64B H 0.0189 0.4512 0.8108 0.382 Uiso 1 1 calc R . . B3 B 0.12521(13) -0.2150(3) 0.7648(3) 0.1195(18) Uani 1 1 d D . . H3 H 0.1053 -0.2886 0.7797 0.143 Uiso 1 1 calc R . . B4 B 0.09789(12) -0.1314(2) 0.6837(3) 0.1395(17) Uani 1 1 d D . . H4 H 0.0573 -0.1243 0.6824 0.167 Uiso 1 1 calc R . . B5 B 0.12702(13) -0.1846(4) 0.5630(4) 0.223(3) Uani 1 1 d D . . H5 H 0.1024 -0.2343 0.5113 0.267 Uiso 1 1 calc R . . B6 B 0.17218(18) -0.1363(4) 0.7904(5) 0.366(4) Uani 1 1 d D . . H6 H 0.1927 -0.1263 0.8711 0.440 Uiso 1 1 calc R . . B7 B 0.11942(16) -0.0872(4) 0.8057(5) 0.419(5) Uani 1 1 d D . . H7 H 0.0990 -0.0471 0.8743 0.503 Uiso 1 1 calc R . . B8 B 0.1577(2) -0.0201(4) 0.7235(3) 0.301(6) Uani 1 1 d D . . H8 H 0.1624 0.0600 0.7556 0.362 Uiso 1 1 calc R . . B9 B 0.13214(11) -0.0570(3) 0.5919(3) 0.1238(15) Uani 1 1 d D . . H9 H 0.1071 -0.0010 0.5503 0.149 Uiso 1 1 calc R . . B10 B 0.18259(12) -0.1265(3) 0.5356(3) 0.1429(16) Uani 1 1 d D . . H10 H 0.1981 -0.1209 0.4485 0.171 Uiso 1 1 calc R . . B11 B 0.22012(12) -0.1422(2) 0.6571(4) 0.1269(14) Uani 1 1 d D . . H11 H 0.2605 -0.1527 0.6518 0.152 Uiso 1 1 calc R . . B12 B 0.19127(12) -0.0367(2) 0.6144(4) 0.155(2) Uani 1 1 d D . . H12 H 0.2156 0.0307 0.5992 0.186 Uiso 1 1 calc R . . O7 O 0.15196(17) 0.5850(3) 0.2502(3) 0.367(3) Uani 1 1 d D . . C51 C 0.1255(2) 0.5214(3) 0.1774(5) 0.317(3) Uani 1 1 d D . . H51A H 0.1443 0.4605 0.1543 0.381 Uiso 1 1 calc R . . H51B H 0.0941 0.4999 0.2104 0.381 Uiso 1 1 calc R . . C52 C 0.11979(15) 0.5862(4) 0.0951(4) 0.312(3) Uani 1 1 d D . . H52A H 0.0898 0.6267 0.1065 0.374 Uiso 1 1 calc R . . H52B H 0.1171 0.5494 0.0227 0.374 Uiso 1 1 calc R . . C53 C 0.16430(18) 0.6568(4) 0.0936(4) 0.307(3) Uani 1 1 d D . . H53A H 0.1934 0.6214 0.0645 0.368 Uiso 1 1 calc R . . H53B H 0.1583 0.7192 0.0487 0.368 Uiso 1 1 calc R . . C54 C 0.1690(2) 0.6807(3) 0.2159(4) 0.314(3) Uani 1 1 d D . . H54A H 0.2030 0.6937 0.2391 0.377 Uiso 1 1 calc R . . H54B H 0.1478 0.7376 0.2402 0.377 Uiso 1 1 calc R . . H50 H 0.1604 -0.2219 0.4792 0.050 Uiso 1 1 d . . . H45 H 0.0925 -0.2180 0.6265 0.050 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 K1 0.0773(3) 0.1193(4) 0.1075(4) -0.0001(7) 0.0006(6) -0.0172(3) O1 0.0817(11) 0.1515(17) 0.356(3) 0.015(4) -0.042(3) -0.0228(12) O2 0.1569(19) 0.197(2) 0.188(2) 0.0621(18) 0.0847(18) 0.0656(18) O3 0.1459(17) 0.1128(16) 0.1119(17) -0.0125(13) -0.0166(15) 0.0270(14) O4 0.0987(12) 0.1280(15) 0.248(2) -0.005(3) -0.002(3) -0.0007(12) O5 0.173(2) 0.232(3) 0.173(3) 0.059(2) 0.027(2) 0.044(2) O6 0.150(2) 0.198(2) 0.212(2) -0.1045(19) -0.060(2) 0.0663(18) O8 0.309(3) 0.1521(18) 0.185(2) -0.025(3) -0.027(4) 0.0999(18) C1 0.118(2) 0.365(5) 0.110(3) -0.105(3) -0.037(2) 0.084(3) C2 0.151(3) 0.0841(19) 0.0577(16) -0.0088(15) -0.0239(19) 0.012(2) C3 0.212(3) 0.098(2) 0.081(2) 0.0240(18) 0.066(2) 0.049(2) C4 0.150(3) 0.0689(17) 0.0593(16) 0.0132(15) 0.0029(18) -0.0067(18) C5 0.189(3) 0.115(3) 0.097(3) 0.012(2) -0.016(3) 0.019(3) C6 0.125(3) 0.092(2) 0.170(3) 0.030(2) 0.021(2) -0.004(2) C7 0.113(2) 0.148(3) 0.165(4) 0.016(3) 0.046(2) -0.008(2) C8 0.166(3) 0.105(2) 0.085(2) -0.009(2) 0.032(2) 0.019(2) C9 0.117(2) 0.0682(17) 0.099(2) 0.0018(17) 0.0011(19) 0.0067(18) C10 0.183(3) 0.098(2) 0.0670(19) -0.0116(18) 0.023(2) 0.030(2) C31 0.083(2) 0.483(7) 0.450(7) 0.190(6) 0.073(3) -0.113(3) C32 0.091(3) 0.234(5) 0.708(13) 0.168(7) 0.045(5) -0.034(3) C33 0.400(7) 0.278(5) 0.095(3) 0.103(3) 0.080(4) 0.100(6) C34 0.285(5) 0.167(3) 0.136(4) 0.008(3) 0.035(4) 0.117(3) C35 0.143(3) 0.220(4) 0.276(4) -0.133(3) -0.099(3) -0.004(3) C36 0.179(4) 0.181(4) 0.257(5) -0.041(4) 0.042(4) 0.039(4) C37 0.104(2) 0.206(4) 0.356(6) 0.002(4) 0.143(3) -0.057(2) C38 0.210(5) 0.204(5) 0.285(6) -0.057(5) -0.085(4) 0.064(4) C39 0.305(6) 0.508(9) 0.085(3) 0.073(4) -0.003(4) 0.196(6) C40 0.182(4) 0.143(3) 0.307(7) 0.017(4) -0.066(4) 0.078(3) C41 0.183(3) 0.148(4) 0.281(4) -0.082(3) -0.144(3) 0.035(3) C42 0.112(3) 0.214(5) 0.435(9) -0.053(6) -0.069(4) 0.007(3) C61 0.357(7) 0.213(5) 0.202(5) 0.051(4) 0.017(6) 0.079(5) C62 0.287(5) 0.248(5) 0.521(13) -0.090(6) -0.040(7) 0.162(4) C63 0.218(4) 0.160(3) 0.405(7) -0.160(4) 0.080(5) 0.019(3) C64 0.565(9) 0.204(5) 0.184(5) -0.017(4) -0.113(5) 0.188(5) B3 0.078(2) 0.152(4) 0.129(3) -0.011(3) -0.015(3) -0.014(3) B4 0.117(2) 0.122(3) 0.180(4) 0.031(4) 0.043(4) 0.054(2) B5 0.071(2) 0.437(7) 0.159(3) -0.173(4) -0.060(3) 0.096(3) B6 0.533(8) 0.440(7) 0.126(4) -0.122(5) -0.168(5) 0.361(5) B7 0.128(5) 0.392(8) 0.739(13) -0.384(7) -0.086(7) 0.056(5) B8 0.638(17) 0.160(5) 0.107(4) -0.052(3) -0.042(6) 0.098(7) B9 0.096(2) 0.140(3) 0.136(3) 0.085(2) 0.002(2) 0.055(2) B10 0.119(3) 0.172(3) 0.138(3) 0.121(2) 0.031(3) 0.047(3) B11 0.107(2) 0.089(2) 0.185(3) -0.068(3) 0.054(4) -0.0184(18) B12 0.128(3) 0.0478(19) 0.288(7) 0.022(3) -0.083(3) 0.000(2) O7 0.622(6) 0.255(4) 0.223(3) 0.060(3) -0.201(3) -0.198(4) C51 0.465(6) 0.146(3) 0.341(6) -0.001(5) -0.244(6) -0.074(4) C52 0.263(4) 0.329(7) 0.344(5) 0.128(5) -0.238(3) -0.074(5) C53 0.426(6) 0.350(7) 0.143(4) -0.011(4) 0.145(4) -0.193(5) C54 0.493(8) 0.146(4) 0.303(7) -0.026(4) 0.245(5) -0.097(4) _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 K1 O1 2.7134(19) . ? K1 O8 2.755(2) . ? K1 O4 2.7960(19) . ? K1 O3 2.819(2) . ? K1 O6 2.821(3) . ? K1 O5 2.826(3) . ? K1 O2 2.837(3) . ? K1 C38 3.423(5) . ? K1 C32 3.462(5) . ? K1 C40 3.507(5) . ? K1 C42 3.525(4) . ? K1 C36 3.527(4) . ? O1 C42 1.385(5) . ? O1 C31 1.395(5) . ? O2 C33 1.372(5) . ? O2 C32 1.383(5) . ? O3 C34 1.374(5) . ? O3 C35 1.392(4) . ? O4 C37 1.356(5) . ? O4 C36 1.353(5) . ? O5 C39 1.333(5) . ? O5 C38 1.340(5) . ? O6 C41 1.324(4) . ? O6 C40 1.333(5) . ? O8 C64 1.355(5) . ? O8 C61 1.373(5) . ? C1 C2 1.432(4) . ? C1 C10 1.484(5) . ? C1 B5 1.846(6) . ? C1 B10 2.077(6) . ? C2 C3 1.524(4) . ? C2 B6 1.550(6) . ? C2 B3 1.706(5) . ? C2 B11 1.766(5) . ? C3 C4 1.443(4) . ? C4 C9 1.395(4) . ? C4 C5 1.418(5) . ? C5 C6 1.374(5) . ? C6 C7 1.375(5) . ? C7 C8 1.399(5) . ? C8 C9 1.362(4) . ? C9 C10 1.545(4) . ? C31 C32 1.370(6) . ? C33 C34 1.403(6) . ? C35 C36 1.403(5) . ? C37 C38 1.381(6) . ? C39 C40 1.372(6) . ? C41 C42 1.392(6) . ? C61 C62 1.495(7) . ? C62 C63 1.501(6) . ? C63 C64 1.461(6) . ? B3 B4 1.609(5) . ? B3 B6 1.648(6) . ? B3 B7 1.715(6) . ? B4 B7 1.639(6) . ? B4 B9 1.707(5) . ? B4 B5 1.751(5) . ? B5 B9 1.677(5) . ? B5 B10 1.704(5) . ? B6 B7 1.566(6) . ? B6 B8 1.727(6) . ? B6 B11 2.023(7) . ? B7 B8 1.651(7) . ? B8 B12 1.576(6) . ? B8 B9 1.748(5) . ? B9 B12 1.637(4) . ? B9 B10 1.755(4) . ? B10 B12 1.493(5) . ? B10 B11 1.754(5) . ? B11 B12 1.639(4) . ? O7 C51 1.377(6) . ? O7 C54 1.372(6) . ? C51 C52 1.280(7) . ? C52 C53 1.504(6) . ? C53 C54 1.464(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 K1 O8 87.35(7) . . ? O1 K1 O4 170.93(7) . . ? O8 K1 O4 83.88(7) . . ? O1 K1 O3 121.93(10) . . ? O8 K1 O3 89.26(8) . . ? O4 K1 O3 60.41(9) . . ? O1 K1 O6 59.98(9) . . ? O8 K1 O6 81.58(9) . . ? O4 K1 O6 116.15(10) . . ? O3 K1 O6 170.62(7) . . ? O1 K1 O5 116.52(10) . . ? O8 K1 O5 90.49(10) . . ? O4 K1 O5 61.39(10) . . ? O3 K1 O5 121.46(8) . . ? O6 K1 O5 56.99(8) . . ? O1 K1 O2 62.52(9) . . ? O8 K1 O2 83.22(9) . . ? O4 K1 O2 118.46(10) . . ? O3 K1 O2 59.52(7) . . ? O6 K1 O2 120.86(7) . . ? O5 K1 O2 173.65(9) . . ? O1 K1 C38 136.78(11) . . ? O8 K1 C38 83.53(10) . . ? O4 K1 C38 39.74(11) . . ? O3 K1 C38 100.15(9) . . ? O6 K1 C38 76.90(10) . . ? O5 K1 C38 22.23(10) . . ? O2 K1 C38 155.78(10) . . ? O1 K1 C32 42.29(11) . . ? O8 K1 C32 92.68(10) . . ? O4 K1 C32 140.33(12) . . ? O3 K1 C32 80.09(10) . . ? O6 K1 C32 102.26(10) . . ? O5 K1 C32 158.27(11) . . ? O2 K1 C32 22.69(10) . . ? C38 K1 C32 176.20(11) . . ? O1 K1 C40 78.53(10) . . ? O8 K1 C40 91.67(10) . . ? O4 K1 C40 99.37(10) . . ? O3 K1 C40 159.54(8) . . ? O6 K1 C40 20.93(8) . . ? O5 K1 C40 38.11(9) . . ? O2 K1 C40 140.85(9) . . ? C38 K1 C40 59.71(11) . . ? C32 K1 C40 120.26(11) . . ? O1 K1 C42 20.90(10) . . ? O8 K1 C42 81.58(11) . . ? O4 K1 C42 153.25(11) . . ? O3 K1 C42 141.24(9) . . ? O6 K1 C42 39.40(9) . . ? O5 K1 C42 96.34(10) . . ? O2 K1 C42 81.95(9) . . ? C38 K1 C42 115.93(11) . . ? C32 K1 C42 62.96(11) . . ? C40 K1 C42 58.92(10) . . ? O1 K1 C36 163.24(11) . . ? O8 K1 C36 92.40(9) . . ? O4 K1 C36 20.89(9) . . ? O3 K1 C36 41.32(8) . . ? O6 K1 C36 136.55(9) . . ? O5 K1 C36 80.24(9) . . ? O2 K1 C36 100.80(9) . . ? C38 K1 C36 59.65(10) . . ? C32 K1 C36 121.05(11) . . ? C40 K1 C36 118.23(10) . . ? C42 K1 C36 173.09(12) . . ? C42 O1 C31 124.8(3) . . ? C42 O1 K1 114.8(2) . . ? C31 O1 K1 115.7(2) . . ? C33 O2 C32 117.1(3) . . ? C33 O2 K1 116.7(2) . . ? C32 O2 K1 105.0(3) . . ? C34 O3 C35 126.9(3) . . ? C34 O3 K1 111.9(2) . . ? C35 O3 K1 113.2(2) . . ? C37 O4 C36 116.5(3) . . ? C37 O4 K1 114.2(2) . . ? C36 O4 K1 111.6(2) . . ? C39 O5 C38 122.4(4) . . ? C39 O5 K1 119.3(3) . . ? C38 O5 K1 104.8(3) . . ? C41 O6 C40 114.9(3) . . ? C41 O6 K1 113.6(2) . . ? C40 O6 K1 110.0(2) . . ? C64 O8 C61 109.7(3) . . ? C64 O8 K1 132.3(3) . . ? C61 O8 K1 116.6(3) . . ? C2 C1 C10 126.9(3) . . ? C2 C1 B5 103.4(3) . . ? C10 C1 B5 126.8(3) . . ? C2 C1 B10 97.6(3) . . ? C10 C1 B10 100.9(3) . . ? B5 C1 B10 51.08(19) . . ? C1 C2 C3 105.7(3) . . ? C1 C2 B6 131.0(3) . . ? C3 C2 B6 123.3(3) . . ? C1 C2 B3 98.0(3) . . ? C3 C2 B3 115.3(3) . . ? B6 C2 B3 60.6(2) . . ? C1 C2 B11 81.3(3) . . ? C3 C2 B11 123.0(3) . . ? B6 C2 B11 74.9(3) . . ? B3 C2 B11 119.6(2) . . ? C4 C3 C2 115.7(2) . . ? C9 C4 C5 112.2(3) . . ? C9 C4 C3 125.6(3) . . ? C5 C4 C3 122.1(3) . . ? C6 C5 C4 125.9(3) . . ? C5 C6 C7 113.9(3) . . ? C6 C7 C8 125.4(3) . . ? C9 C8 C7 113.8(3) . . ? C8 C9 C4 127.0(3) . . ? C8 C9 C10 117.6(3) . . ? C4 C9 C10 115.3(3) . . ? C1 C10 C9 113.4(3) . . ? C32 C31 O1 115.2(3) . . ? C31 C32 O2 119.0(4) . . ? C31 C32 K1 82.3(3) . . ? O2 C32 K1 52.3(2) . . ? O2 C33 C34 107.1(3) . . ? O3 C34 C33 122.9(4) . . ? O3 C35 C36 113.3(4) . . ? O4 C36 C35 114.0(4) . . ? O4 C36 K1 47.46(18) . . ? C35 C36 K1 81.7(2) . . ? O4 C37 C38 106.6(3) . . ? O5 C38 C37 125.2(4) . . ? O5 C38 K1 53.0(2) . . ? C37 C38 K1 84.8(3) . . ? O5 C39 C40 106.4(4) . . ? O6 C40 C39 116.4(4) . . ? O6 C40 K1 49.1(2) . . ? C39 C40 K1 85.6(3) . . ? O6 C41 C42 111.1(4) . . ? O1 C42 C41 116.9(3) . . ? O1 C42 K1 44.35(17) . . ? C41 C42 K1 80.2(2) . . ? O8 C61 C62 106.8(4) . . ? C63 C62 C61 101.9(4) . . ? C64 C63 C62 106.6(4) . . ? O8 C64 C63 106.7(4) . . ? B4 B3 B6 92.9(3) . . ? B4 B3 B7 59.0(2) . . ? B6 B3 B7 55.5(2) . . ? B4 B3 C2 114.2(3) . . ? B6 B3 C2 55.0(2) . . ? B7 B3 C2 109.3(3) . . ? B3 B4 B7 63.8(2) . . ? B3 B4 B9 119.6(3) . . ? B7 B4 B9 99.1(3) . . ? B3 B4 B5 90.4(2) . . ? B7 B4 B5 132.4(3) . . ? B9 B4 B5 58.0(2) . . ? B9 B5 B10 62.5(2) . . ? B9 B5 B4 59.7(2) . . ? B10 B5 B4 112.0(3) . . ? B9 B5 C1 118.1(3) . . ? B10 B5 C1 71.5(2) . . ? B4 B5 C1 108.3(3) . . ? B7 B6 C2 127.2(4) . . ? B7 B6 B3 64.5(3) . . ? C2 B6 B3 64.4(3) . . ? B7 B6 B8 59.9(3) . . ? C2 B6 B8 125.2(4) . . ? B3 B6 B8 105.9(3) . . ? B7 B6 B11 133.1(4) . . ? C2 B6 B11 57.4(2) . . ? B3 B6 B11 109.2(3) . . ? B8 B6 B11 80.2(3) . . ? B6 B7 B8 64.9(3) . . ? B6 B7 B4 94.8(3) . . ? B8 B7 B4 84.2(3) . . ? B6 B7 B3 60.1(3) . . ? B8 B7 B3 106.3(3) . . ? B4 B7 B3 57.3(2) . . ? B12 B8 B7 139.2(4) . . ? B12 B8 B6 96.8(3) . . ? B7 B8 B6 55.2(3) . . ? B12 B8 B9 58.8(2) . . ? B7 B8 B9 97.0(3) . . ? B6 B8 B9 104.6(3) . . ? B12 B9 B5 105.5(2) . . ? B12 B9 B4 121.0(3) . . ? B5 B9 B4 62.3(2) . . ? B12 B9 B10 52.08(18) . . ? B5 B9 B10 59.50(19) . . ? B4 B9 B10 111.7(2) . . ? B12 B9 B8 55.4(2) . . ? B5 B9 B8 118.3(3) . . ? B4 B9 B8 79.3(2) . . ? B10 B9 B8 99.2(3) . . ? B12 B10 B5 111.1(3) . . ? B12 B10 B9 59.9(2) . . ? B5 B10 B9 58.0(2) . . ? B12 B10 B11 60.0(2) . . ? B5 B10 B11 107.8(3) . . ? B9 B10 B11 101.7(2) . . ? B12 B10 C1 116.1(3) . . ? B5 B10 C1 57.4(2) . . ? B9 B10 C1 103.8(2) . . ? B11 B10 C1 65.78(18) . . ? B12 B11 B10 52.1(2) . . ? B12 B11 C2 118.2(2) . . ? B10 B11 C2 98.9(2) . . ? B12 B11 B6 84.2(2) . . ? B10 B11 B6 104.3(2) . . ? C2 B11 B6 47.69(19) . . ? B10 B12 B8 120.8(3) . . ? B10 B12 B9 68.0(2) . . ? B8 B12 B9 65.9(3) . . ? B10 B12 B11 67.9(2) . . ? B8 B12 B11 98.0(3) . . ? B9 B12 B11 112.3(2) . . ? C51 O7 C54 121.7(4) . . ? C52 C51 O7 98.0(4) . . ? C51 C52 C53 107.7(4) . . ? C54 C53 C52 100.7(4) . . ? O7 C54 C53 93.9(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.244 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.047 #===END