data_[Me3NH][3a] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H31 B12 N O' _chemical_formula_weight 299.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 22.267(5) _cell_length_b 7.9141(16) _cell_length_c 22.267(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.30 _cell_angle_gamma 90.00 _cell_volume 3917.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1357 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.052 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.7187445 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 KAPPA APEXII DUO DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27985 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6875 _reflns_number_gt 3924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_cell_refinement 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_data_reduction 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1737P)^2^+38.2006P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6875 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2530 _refine_ls_R_factor_gt 0.1930 _refine_ls_wR_factor_ref 0.5466 _refine_ls_wR_factor_gt 0.5015 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.013 _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 O1' O 0.4120(3) 0.4167(9) 0.5226(3) 0.068(2) Uani 1 1 d . . . O1 O 1.0184(3) 0.5797(9) 0.4100(3) 0.066(2) Uani 1 1 d . . . N1 N 0.4122(4) 0.1839(11) 0.6164(4) 0.060(2) Uani 1 1 d . . . H1A H 0.4045 0.2362 0.5804 0.072 Uiso 1 1 calc R . . N1' N 0.1132(4) 0.8110(11) 0.4103(4) 0.063(2) Uani 1 1 d . . . H1'A H 0.0767 0.7595 0.4049 0.075 Uiso 1 1 calc R . . C15 C 0.3790(10) 0.265(3) 0.6591(7) 0.170(10) Uani 1 1 d . . . H15A H 0.3929 0.3791 0.6643 0.255 Uiso 1 1 calc R . . H15B H 0.3839 0.2060 0.6968 0.255 Uiso 1 1 calc R . . H15C H 0.3372 0.2655 0.6458 0.255 Uiso 1 1 calc R . . C16 C 0.4753(7) 0.181(3) 0.6288(10) 0.199(13) Uani 1 1 d . . . H16A H 0.4902 0.2950 0.6316 0.298 Uiso 1 1 calc R . . H16B H 0.4941 0.1233 0.5970 0.298 Uiso 1 1 calc R . . H16C H 0.4844 0.1237 0.6661 0.298 Uiso 1 1 calc R . . C17 C 0.3873(10) 0.015(2) 0.6123(7) 0.153(9) Uani 1 1 d . . . H17A H 0.3447 0.0219 0.6034 0.230 Uiso 1 1 calc R . . H17B H 0.3951 -0.0424 0.6498 0.230 Uiso 1 1 calc R . . H17C H 0.4056 -0.0457 0.5808 0.230 Uiso 1 1 calc R . . C8' C 0.3738(4) 0.3446(13) 0.3370(4) 0.053(2) Uani 1 1 d . . . C9' C 0.3151(4) 0.4214(11) 0.3564(4) 0.048(2) Uani 1 1 d . . . C11' C 0.4041(6) 0.4741(16) 0.3004(5) 0.075(3) Uani 1 1 d . . . H11C H 0.4213 0.4224 0.2658 0.090 Uiso 1 1 calc R . . H11D H 0.4357 0.5311 0.3243 0.090 Uiso 1 1 calc R . . C12' C 0.3547(7) 0.5964(17) 0.2807(6) 0.090(4) Uani 1 1 d . . . H12C H 0.3353 0.5611 0.2426 0.108 Uiso 1 1 calc R . . H12D H 0.3710 0.7089 0.2759 0.108 Uiso 1 1 calc R . . C13' C 0.3100(6) 0.5956(14) 0.3293(5) 0.079(4) Uani 1 1 d . . . H13C H 0.3200 0.6814 0.3593 0.094 Uiso 1 1 calc R . . H13D H 0.2695 0.6160 0.3124 0.094 Uiso 1 1 calc R . . C14' C 0.4326(7) 0.5863(19) 0.5350(6) 0.104(5) Uani 1 1 d . . . H14D H 0.4473 0.5943 0.5763 0.156 Uiso 1 1 calc R . . H14E H 0.3998 0.6638 0.5278 0.156 Uiso 1 1 calc R . . H14F H 0.4643 0.6137 0.5093 0.156 Uiso 1 1 calc R . . C15' C 0.1264(8) 0.827(2) 0.4755(6) 0.127(6) Uani 1 1 d . . . H15D H 0.0954 0.8920 0.4928 0.190 Uiso 1 1 calc R . . H15E H 0.1644 0.8825 0.4829 0.190 Uiso 1 1 calc R . . H15F H 0.1281 0.7166 0.4935 0.190 Uiso 1 1 calc R . . C16' C 0.1566(7) 0.711(3) 0.3774(9) 0.162(9) Uani 1 1 d . . . H16D H 0.1601 0.5996 0.3946 0.243 Uiso 1 1 calc R . . H16E H 0.1952 0.7652 0.3802 0.243 Uiso 1 1 calc R . . H16F H 0.1427 0.7017 0.3359 0.243 Uiso 1 1 calc R . . C17' C 0.1071(6) 0.9831(18) 0.3836(8) 0.111(6) Uani 1 1 d . . . H17D H 0.0785 1.0472 0.4049 0.166 Uiso 1 1 calc R . . H17E H 0.0935 0.9741 0.3420 0.166 Uiso 1 1 calc R . . H17F H 0.1454 1.0390 0.3867 0.166 Uiso 1 1 calc R . . B1' B 0.2981(5) 0.0760(16) 0.3575(6) 0.065(4) Uani 1 1 d . . . B2' B 0.3720(6) 0.1366(15) 0.3219(5) 0.058(3) Uani 1 1 d . . . H2' H 0.3908 0.0726 0.2833 0.069 Uiso 1 1 calc R . . B3' B 0.3100(5) 0.2661(13) 0.3054(5) 0.053(3) Uani 1 1 d . . . H3' H 0.2937 0.2755 0.2579 0.063 Uiso 1 1 calc R . . B4' B 0.2577(5) 0.2830(15) 0.3596(6) 0.061(3) Uani 1 1 d . . . H4' H 0.2109 0.3007 0.3422 0.073 Uiso 1 1 calc R . . B5' B 0.2647(5) 0.1783(15) 0.4253(6) 0.060(3) Uani 1 1 d . . . H5' H 0.2214 0.1401 0.4424 0.072 Uiso 1 1 calc R . . B6' B 0.3245(6) 0.0414(15) 0.4402(6) 0.064(3) Uani 1 1 d . . . H6' H 0.3149 -0.0753 0.4647 0.077 Uiso 1 1 calc R . . B7' B 0.3779(5) 0.0240(14) 0.3879(5) 0.056(3) Uani 1 1 d . . . H7' H 0.3987 -0.1010 0.3832 0.067 Uiso 1 1 calc R . . B10' B 0.2926(5) 0.3912(15) 0.4246(6) 0.056(3) Uani 1 1 d . . . H10' H 0.2942 0.5130 0.4485 0.067 Uiso 1 1 calc R . . B11' B 0.3233(5) 0.2436(15) 0.4744(6) 0.056(3) Uani 1 1 d . . . H11' H 0.3123 0.2663 0.5212 0.067 Uiso 1 1 calc R . . B12' B 0.3914(5) 0.1453(14) 0.4534(5) 0.048(3) Uani 1 1 d . . . H12' H 0.4267 0.0995 0.4861 0.057 Uiso 1 1 calc R . . B13' B 0.4169(5) 0.2247(15) 0.3827(5) 0.054(3) Uani 1 1 d . . . H13' H 0.4600 0.2899 0.3927 0.065 Uiso 1 1 calc R . . B14' B 0.3878(5) 0.3815(15) 0.4626(5) 0.051(3) Uani 1 1 d . . . H14' H 0.3894 0.4614 0.4291 0.062 Uiso 1 1 calc R . . H1' H 0.263(5) -0.019(13) 0.341(4) 0.07(3) Uiso 1 1 d . . . B1 B 0.8559(6) 0.9304(14) 0.3007(5) 0.059(3) Uani 1 1 d . . . B2 B 0.8524(7) 0.7211(19) 0.2604(6) 0.078(4) Uani 1 1 d . . . H2 H 0.8320 0.7020 0.2147 0.093 Uiso 1 1 calc R . . B3 B 0.8027(5) 0.7503(15) 0.3131(5) 0.058(3) Uani 1 1 d . . . H3 H 0.7549 0.7480 0.2973 0.070 Uiso 1 1 calc R . . B4 B 0.8220(6) 0.8790(14) 0.3741(5) 0.057(3) Uani 1 1 d . . . H4 H 0.7847 0.9489 0.3928 0.068 Uiso 1 1 calc R . . B5 B 0.8878(5) 0.9773(14) 0.3793(5) 0.053(3) Uani 1 1 d . . . H5 H 0.8849 1.1009 0.4016 0.064 Uiso 1 1 calc R . . B6 B 0.9378(6) 0.9582(15) 0.3204(6) 0.062(3) Uani 1 1 d . . . H6 H 0.9624 1.0716 0.3073 0.074 Uiso 1 1 calc R . . B7 B 0.9180(7) 0.8171(18) 0.2626(6) 0.070(4) Uani 1 1 d . . . H7 H 0.9322 0.8481 0.2175 0.084 Uiso 1 1 calc R . . B10 B 0.8834(5) 0.7857(13) 0.4186(5) 0.048(3) Uani 1 1 d . . . H10 H 0.8943 0.7219 0.4617 0.058 Uiso 1 1 calc R . . B11 B 0.9536(6) 0.8560(15) 0.3907(6) 0.058(3) Uani 1 1 d . . . H11 H 0.9879 0.9013 0.4244 0.070 Uiso 1 1 calc R . . B12 B 0.9710(5) 0.7536(16) 0.3221(5) 0.055(3) Uani 1 1 d . . . H12 H 1.0176 0.7282 0.3109 0.066 Uiso 1 1 calc R . . B13 B 0.9174(6) 0.6103(15) 0.2921(5) 0.064(3) Uani 1 1 d . . . H13 H 0.9405 0.4873 0.2928 0.076 Uiso 1 1 calc R . . B14 B 0.9596(5) 0.6196(14) 0.3863(5) 0.050(3) Uani 1 1 d . . . H14 H 0.9252 0.5434 0.3888 0.060 Uiso 1 1 calc R . . C8 C 0.8509(4) 0.5851(12) 0.3179(5) 0.057(3) Uani 1 1 d . . . C9 C 0.8341(4) 0.6662(12) 0.3781(5) 0.054(2) Uani 1 1 d . . . C11 C 0.8215(6) 0.4110(15) 0.3179(7) 0.092(5) Uani 1 1 d . . . H11A H 0.8031 0.3855 0.2784 0.110 Uiso 1 1 calc R . . H11B H 0.8513 0.3250 0.3284 0.110 Uiso 1 1 calc R . . C12 C 0.7743(6) 0.4146(17) 0.3638(7) 0.093(4) Uani 1 1 d . . . H12A H 0.7692 0.3036 0.3812 0.112 Uiso 1 1 calc R . . H12B H 0.7359 0.4522 0.3457 0.112 Uiso 1 1 calc R . . C13 C 0.7983(6) 0.5391(17) 0.4111(6) 0.085(4) Uani 1 1 d . . . H13A H 0.7655 0.5938 0.4303 0.102 Uiso 1 1 calc R . . H13B H 0.8236 0.4820 0.4416 0.102 Uiso 1 1 calc R . . C14 C 1.0315(6) 0.4047(16) 0.4279(7) 0.095(4) Uani 1 1 d . . . H14A H 1.0727 0.3960 0.4429 0.142 Uiso 1 1 calc R . . H14B H 1.0249 0.3318 0.3937 0.142 Uiso 1 1 calc R . . H14C H 1.0055 0.3717 0.4587 0.142 Uiso 1 1 calc R . . H1 H 0.8286 1.0518 0.2819 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 O1' 0.079(5) 0.064(5) 0.059(4) -0.010(4) -0.012(4) -0.018(4) O1 0.057(4) 0.065(5) 0.076(5) 0.009(4) -0.002(4) 0.010(4) N1 0.061(5) 0.066(6) 0.055(5) -0.003(4) 0.008(4) 0.005(4) N1' 0.058(5) 0.067(6) 0.064(5) 0.000(4) 0.003(4) -0.006(4) C15 0.22(2) 0.20(2) 0.102(12) 0.049(13) 0.079(14) 0.127(19) C16 0.055(9) 0.31(3) 0.22(2) 0.16(2) -0.029(11) -0.006(14) C17 0.26(2) 0.122(14) 0.076(10) 0.036(10) -0.026(13) -0.083(16) C8' 0.049(6) 0.055(6) 0.054(6) -0.015(5) -0.006(4) -0.002(4) C9' 0.055(6) 0.031(5) 0.058(6) -0.008(4) -0.010(5) 0.004(4) C11' 0.079(8) 0.085(9) 0.060(7) 0.001(6) -0.003(6) -0.024(7) C12' 0.114(11) 0.068(8) 0.087(9) 0.009(7) 0.002(8) -0.013(8) C13' 0.117(10) 0.044(6) 0.073(8) 0.004(5) -0.010(7) 0.019(6) C14' 0.116(12) 0.103(11) 0.092(10) -0.037(9) -0.008(9) -0.033(9) C15' 0.171(17) 0.134(15) 0.071(9) 0.003(9) -0.031(10) -0.050(13) C16' 0.077(10) 0.23(2) 0.186(19) -0.081(18) 0.053(11) 0.026(13) C17' 0.069(8) 0.092(10) 0.168(15) 0.037(10) -0.022(9) -0.023(8) B1' 0.049(7) 0.048(7) 0.094(10) -0.021(6) -0.023(7) 0.014(5) B2' 0.070(8) 0.051(7) 0.051(6) -0.012(5) -0.001(6) 0.016(6) B3' 0.063(7) 0.039(6) 0.054(6) -0.013(5) -0.013(5) -0.003(5) B4' 0.034(6) 0.054(7) 0.093(9) -0.004(6) -0.009(6) 0.006(5) B5' 0.041(6) 0.053(7) 0.087(9) -0.017(6) 0.004(6) -0.009(5) B6' 0.065(8) 0.043(6) 0.085(9) -0.001(6) 0.006(7) -0.012(6) B7' 0.061(7) 0.039(6) 0.066(7) -0.005(5) -0.006(6) 0.009(5) B10' 0.049(6) 0.050(6) 0.070(8) -0.004(6) 0.014(6) 0.007(5) B11' 0.055(7) 0.050(7) 0.063(7) -0.011(6) 0.015(6) -0.002(5) B12' 0.046(6) 0.047(6) 0.048(6) -0.001(5) -0.007(5) 0.004(5) B13' 0.041(6) 0.062(7) 0.058(7) -0.019(6) -0.001(5) 0.010(5) B14' 0.046(6) 0.055(7) 0.054(6) 0.005(5) 0.007(5) -0.003(5) B1 0.084(9) 0.037(6) 0.056(7) 0.000(5) 0.002(6) 0.011(6) B2 0.100(11) 0.080(10) 0.050(7) -0.019(7) -0.022(7) 0.040(8) B3 0.056(7) 0.048(6) 0.068(7) 0.008(6) -0.017(6) 0.002(5) B4 0.071(8) 0.043(6) 0.058(7) 0.003(5) 0.007(6) 0.008(6) B5 0.071(8) 0.034(5) 0.056(7) 0.003(5) 0.009(6) 0.005(5) B6 0.062(7) 0.043(6) 0.082(9) 0.010(6) 0.012(7) -0.005(5) B7 0.090(10) 0.069(9) 0.052(7) 0.006(6) 0.007(7) 0.018(7) B10 0.056(6) 0.041(6) 0.046(6) 0.004(5) -0.009(5) 0.014(5) B11 0.067(8) 0.046(6) 0.061(7) 0.004(5) -0.008(6) 0.003(6) B12 0.056(7) 0.061(7) 0.049(6) 0.010(5) 0.012(5) 0.008(6) B13 0.087(9) 0.041(6) 0.061(7) -0.016(5) -0.007(6) 0.032(6) B14 0.050(6) 0.049(6) 0.050(6) 0.004(5) -0.008(5) 0.001(5) C8 0.049(6) 0.037(5) 0.083(7) 0.000(5) -0.021(5) 0.003(4) C9 0.056(6) 0.042(5) 0.064(6) 0.009(5) 0.000(5) 0.006(4) C11 0.095(10) 0.047(7) 0.129(12) -0.009(7) -0.038(9) 0.004(6) C12 0.068(8) 0.073(9) 0.139(13) 0.021(9) 0.009(9) -0.015(7) C13 0.065(7) 0.079(9) 0.110(10) 0.038(8) 0.001(7) -0.005(6) C14 0.086(9) 0.073(9) 0.123(11) 0.021(8) -0.016(8) 0.028(7) _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' B14' 1.438(13) . ? O1' C14' 1.440(14) . ? O1 B14 1.418(12) . ? O1 C14 1.466(13) . ? N1 C15 1.394(16) . ? N1 C16 1.417(16) . ? N1 C17 1.446(17) . ? N1' C15' 1.471(15) . ? N1' C16' 1.479(16) . ? N1' C17' 1.490(16) . ? C8' C11' 1.494(15) . ? C8' C9' 1.526(13) . ? C8' B13' 1.658(15) . ? C8' B3' 1.668(14) . ? C8' B2' 1.680(15) . ? C9' C13' 1.506(13) . ? C9' B10' 1.644(15) . ? C9' B3' 1.674(13) . ? C9' B4' 1.688(15) . ? C11' C12' 1.511(18) . ? C12' C13' 1.512(18) . ? B1' B4' 1.871(16) . ? B1' B5' 1.902(18) . ? B1' B7' 1.909(16) . ? B1' B6' 1.92(2) . ? B1' B2' 1.927(19) . ? B1' B3' 1.928(19) . ? B2' B7' 1.718(17) . ? B2' B3' 1.740(16) . ? B2' B13' 1.780(16) . ? B3' B4' 1.731(18) . ? B4' B5' 1.682(19) . ? B4' B10' 1.818(18) . ? B5' B11' 1.731(16) . ? B5' B6' 1.733(18) . ? B5' B10' 1.796(17) . ? B6' B12' 1.713(16) . ? B6' B7' 1.717(18) . ? B6' B11' 1.773(16) . ? B7' B12' 1.759(15) . ? B7' B13' 1.818(17) . ? B10' B11' 1.724(17) . ? B11' B12' 1.790(16) . ? B11' B14' 1.835(16) . ? B12' B13' 1.816(16) . ? B12' B14' 1.883(16) . ? B1 B6 1.865(19) . ? B1 B2 1.884(17) . ? B1 B3 1.884(18) . ? B1 B4 1.884(17) . ? B1 B7 1.889(18) . ? B1 B5 1.889(17) . ? B2 B7 1.64(2) . ? B2 C8 1.675(18) . ? B2 B3 1.67(2) . ? B2 B13 1.802(17) . ? B3 C8 1.691(14) . ? B3 C9 1.707(14) . ? B3 B4 1.733(17) . ? B4 B5 1.656(17) . ? B4 C9 1.707(15) . ? B4 B10 1.799(16) . ? B5 B10 1.756(15) . ? B5 B11 1.758(16) . ? B5 B6 1.775(17) . ? B6 B7 1.742(19) . ? B6 B11 1.778(17) . ? B6 B12 1.780(17) . ? B7 B13 1.764(18) . ? B7 B12 1.794(17) . ? B10 C9 1.673(15) . ? B10 B11 1.804(17) . ? B11 B12 1.792(17) . ? B11 B14 1.879(16) . ? B12 B13 1.750(18) . ? B12 B14 1.811(15) . ? B13 C8 1.631(18) . ? C8 C11 1.526(15) . ? C8 C9 1.553(15) . ? C9 C13 1.500(15) . ? C11 C12 1.507(19) . ? C12 C13 1.516(19) . ? 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 B14' O1' C14' 117.2(9) . . ? B14 O1 C14 118.4(9) . . ? C15 N1 C16 115.7(16) . . ? C15 N1 C17 104.6(15) . . ? C16 N1 C17 111.8(16) . . ? C15' N1' C16' 115.9(13) . . ? C15' N1' C17' 108.9(12) . . ? C16' N1' C17' 109.9(13) . . ? C11' C8' C9' 107.6(9) . . ? C11' C8' B13' 117.7(9) . . ? C9' C8' B13' 121.9(8) . . ? C11' C8' B3' 115.2(9) . . ? C9' C8' B3' 63.0(6) . . ? B13' C8' B3' 119.7(8) . . ? C11' C8' B2' 124.7(9) . . ? C9' C8' B2' 115.8(8) . . ? B13' C8' B2' 64.5(7) . . ? B3' C8' B2' 62.6(6) . . ? C13' C9' C8' 107.3(9) . . ? C13' C9' B10' 118.9(8) . . ? C8' C9' B10' 121.0(8) . . ? C13' C9' B3' 113.6(8) . . ? C8' C9' B3' 62.6(6) . . ? B10' C9' B3' 120.6(8) . . ? C13' C9' B4' 124.8(9) . . ? C8' C9' B4' 114.6(7) . . ? B10' C9' B4' 66.1(7) . . ? B3' C9' B4' 62.0(7) . . ? C8' C11' C12' 104.7(10) . . ? C11' C12' C13' 106.7(10) . . ? C9' C13' C12' 104.6(10) . . ? B4' B1' B5' 52.9(7) . . ? B4' B1' B7' 128.3(8) . . ? B5' B1' B7' 102.0(8) . . ? B4' B1' B6' 102.8(8) . . ? B5' B1' B6' 53.9(7) . . ? B7' B1' B6' 53.3(6) . . ? B4' B1' B2' 102.4(8) . . ? B5' B1' B2' 127.1(8) . . ? B7' B1' B2' 53.2(6) . . ? B6' B1' B2' 102.1(7) . . ? B4' B1' B3' 54.2(6) . . ? B5' B1' B3' 102.7(7) . . ? B7' B1' B3' 103.0(8) . . ? B6' B1' B3' 130.1(8) . . ? B2' B1' B3' 53.7(6) . . ? C8' B2' B7' 109.7(8) . . ? C8' B2' B3' 58.3(6) . . ? B7' B2' B3' 120.5(9) . . ? C8' B2' B13' 57.2(6) . . ? B7' B2' B13' 62.6(7) . . ? B3' B2' B13' 109.5(8) . . ? C8' B2' B1' 99.9(8) . . ? B7' B2' B1' 62.8(7) . . ? B3' B2' B1' 63.2(7) . . ? B13' B2' B1' 103.9(8) . . ? C8' B3' C9' 54.4(5) . . ? C8' B3' B4' 105.5(8) . . ? C9' B3' B4' 59.4(6) . . ? C8' B3' B2' 59.0(6) . . ? C9' B3' B2' 105.5(7) . . ? B4' B3' B2' 117.1(9) . . ? C8' B3' B1' 100.4(8) . . ? C9' B3' B1' 99.8(8) . . ? B4' B3' B1' 61.2(7) . . ? B2' B3' B1' 63.1(7) . . ? B5' B4' C9' 108.9(8) . . ? B5' B4' B3' 122.5(8) . . ? C9' B4' B3' 58.6(6) . . ? B5' B4' B10' 61.6(7) . . ? C9' B4' B10' 55.8(6) . . ? B3' B4' B10' 108.6(8) . . ? B5' B4' B1' 64.5(7) . . ? C9' B4' B1' 101.6(7) . . ? B3' B4' B1' 64.6(7) . . ? B10' B4' B1' 104.4(8) . . ? B4' B5' B11' 115.5(9) . . ? B4' B5' B6' 120.4(9) . . ? B11' B5' B6' 61.6(7) . . ? B4' B5' B10' 62.9(7) . . ? B11' B5' B10' 58.5(7) . . ? B6' B5' B10' 109.1(8) . . ? B4' B5' B1' 62.6(7) . . ? B11' B5' B1' 108.3(8) . . ? B6' B5' B1' 63.5(7) . . ? B10' B5' B1' 104.0(9) . . ? B12' B6' B7' 61.7(7) . . ? B12' B6' B5' 112.5(8) . . ? B7' B6' B5' 118.3(10) . . ? B12' B6' B11' 61.8(6) . . ? B7' B6' B11' 113.0(8) . . ? B5' B6' B11' 59.2(7) . . ? B12' B6' B1' 108.2(9) . . ? B7' B6' B1' 63.0(7) . . ? B5' B6' B1' 62.5(7) . . ? B11' B6' B1' 105.8(8) . . ? B6' B7' B2' 121.1(9) . . ? B6' B7' B12' 59.1(7) . . ? B2' B7' B12' 115.3(8) . . ? B6' B7' B13' 109.0(8) . . ? B2' B7' B13' 60.4(7) . . ? B12' B7' B13' 61.0(6) . . ? B6' B7' B1' 63.7(8) . . ? B2' B7' B1' 63.9(7) . . ? B12' B7' B1' 106.8(8) . . ? B13' B7' B1' 103.1(8) . . ? C9' B10' B11' 124.1(8) . . ? C9' B10' B5' 105.6(8) . . ? B11' B10' B5' 58.9(7) . . ? C9' B10' B4' 58.1(7) . . ? B11' B10' B4' 109.2(8) . . ? B5' B10' B4' 55.5(7) . . ? B10' B11' B5' 62.6(7) . . ? B10' B11' B6' 110.5(9) . . ? B5' B11' B6' 59.3(7) . . ? B10' B11' B12' 116.0(8) . . ? B5' B11' B12' 109.0(8) . . ? B6' B11' B12' 57.5(6) . . ? B10' B11' B14' 77.9(7) . . ? B5' B11' B14' 130.9(9) . . ? B6' B11' B14' 116.4(8) . . ? B12' B11' B14' 62.6(6) . . ? B6' B12' B7' 59.3(7) . . ? B6' B12' B11' 60.8(7) . . ? B7' B12' B11' 110.2(8) . . ? B6' B12' B13' 109.2(8) . . ? B7' B12' B13' 61.1(6) . . ? B11' B12' B13' 112.8(8) . . ? B6' B12' B14' 116.9(8) . . ? B7' B12' B14' 128.7(8) . . ? B11' B12' B14' 59.9(6) . . ? B13' B12' B14' 76.6(7) . . ? C8' B13' B2' 58.4(6) . . ? C8' B13' B12' 122.2(8) . . ? B2' B13' B12' 109.6(8) . . ? C8' B13' B7' 106.1(8) . . ? B2' B13' B7' 57.0(7) . . ? B12' B13' B7' 57.9(6) . . ? O1' B14' B11' 103.7(8) . . ? O1' B14' B12' 106.1(8) . . ? B11' B14' B12' 57.6(6) . . ? B6 B1 B2 103.3(8) . . ? B6 B1 B3 132.0(8) . . ? B2 B1 B3 52.8(7) . . ? B6 B1 B4 104.8(8) . . ? B2 B1 B4 102.5(8) . . ? B3 B1 B4 54.8(6) . . ? B6 B1 B7 55.3(7) . . ? B2 B1 B7 51.7(7) . . ? B3 B1 B7 100.9(8) . . ? B4 B1 B7 128.8(8) . . ? B6 B1 B5 56.4(7) . . ? B2 B1 B5 128.1(8) . . ? B3 B1 B5 102.7(8) . . ? B4 B1 B5 52.1(6) . . ? B7 B1 B5 105.2(8) . . ? B7 B2 C8 109.3(9) . . ? B7 B2 B3 122.4(10) . . ? C8 B2 B3 60.7(7) . . ? B7 B2 B13 61.3(8) . . ? C8 B2 B13 55.8(7) . . ? B3 B2 B13 110.0(9) . . ? B7 B2 B1 64.3(8) . . ? C8 B2 B1 101.7(8) . . ? B3 B2 B1 63.6(7) . . ? B13 B2 B1 103.4(9) . . ? B2 B3 C8 59.7(7) . . ? B2 B3 C9 106.6(8) . . ? C8 B3 C9 54.4(6) . . ? B2 B3 B4 119.1(10) . . ? C8 B3 B4 106.0(8) . . ? C9 B3 B4 59.5(6) . . ? B2 B3 B1 63.6(8) . . ? C8 B3 B1 101.1(8) . . ? C9 B3 B1 100.9(8) . . ? B4 B3 B1 62.6(7) . . ? B5 B4 C9 108.9(9) . . ? B5 B4 B3 120.7(9) . . ? C9 B4 B3 59.5(6) . . ? B5 B4 B10 60.9(7) . . ? C9 B4 B10 56.9(6) . . ? B3 B4 B10 109.7(8) . . ? B5 B4 B1 64.1(7) . . ? C9 B4 B1 100.9(8) . . ? B3 B4 B1 62.6(7) . . ? B10 B4 B1 103.8(8) . . ? B4 B5 B10 63.5(7) . . ? B4 B5 B11 118.7(8) . . ? B10 B5 B11 61.8(6) . . ? B4 B5 B6 119.9(9) . . ? B10 B5 B6 110.5(8) . . ? B11 B5 B6 60.4(7) . . ? B4 B5 B1 63.8(7) . . ? B10 B5 B1 105.3(8) . . ? B11 B5 B1 107.0(8) . . ? B6 B5 B1 61.1(7) . . ? B7 B6 B5 117.2(9) . . ? B7 B6 B11 112.8(9) . . ? B5 B6 B11 59.3(7) . . ? B7 B6 B12 61.2(7) . . ? B5 B6 B12 109.9(8) . . ? B11 B6 B12 60.5(7) . . ? B7 B6 B1 63.1(7) . . ? B5 B6 B1 62.5(7) . . ? B11 B6 B1 107.2(8) . . ? B12 B6 B1 107.3(8) . . ? B2 B7 B6 120.4(10) . . ? B2 B7 B13 63.7(8) . . ? B6 B7 B13 109.1(9) . . ? B2 B7 B12 116.0(10) . . ? B6 B7 B12 60.4(7) . . ? B13 B7 B12 58.9(7) . . ? B2 B7 B1 64.0(8) . . ? B6 B7 B1 61.6(7) . . ? B13 B7 B1 104.6(9) . . ? B12 B7 B1 105.7(8) . . ? C9 B10 B5 105.9(7) . . ? C9 B10 B4 58.8(6) . . ? B5 B10 B4 55.5(6) . . ? C9 B10 B11 122.9(8) . . ? B5 B10 B11 59.2(6) . . ? B4 B10 B11 109.2(8) . . ? B5 B11 B6 60.2(7) . . ? B5 B11 B12 110.1(8) . . ? B6 B11 B12 59.8(7) . . ? B5 B11 B10 59.1(6) . . ? B6 B11 B10 108.2(8) . . ? B12 B11 B10 112.9(9) . . ? B5 B11 B14 126.7(9) . . ? B6 B11 B14 114.7(9) . . ? B12 B11 B14 59.1(6) . . ? B10 B11 B14 77.1(7) . . ? B13 B12 B6 108.0(8) . . ? B13 B12 B11 116.2(9) . . ? B6 B12 B11 59.7(7) . . ? B13 B12 B7 59.7(7) . . ? B6 B12 B7 58.3(7) . . ? B11 B12 B7 109.7(8) . . ? B13 B12 B14 78.4(7) . . ? B6 B12 B14 118.2(8) . . ? B11 B12 B14 62.9(6) . . ? B7 B12 B14 129.1(9) . . ? C8 B13 B12 123.9(8) . . ? C8 B13 B7 105.7(8) . . ? B12 B13 B7 61.4(7) . . ? C8 B13 B2 58.1(8) . . ? B12 B13 B2 110.4(9) . . ? B7 B13 B2 54.9(8) . . ? O1 B14 B12 104.8(8) . . ? O1 B14 B11 105.7(8) . . ? B12 B14 B11 58.1(6) . . ? C11 C8 C9 104.3(10) . . ? C11 C8 B13 120.6(9) . . ? C9 C8 B13 121.5(8) . . ? C11 C8 B2 127.5(10) . . ? C9 C8 B2 114.3(8) . . ? B13 C8 B2 66.1(8) . . ? C11 C8 B3 115.2(9) . . ? C9 C8 B3 63.3(7) . . ? B13 C8 B3 118.0(8) . . ? B2 C8 B3 59.7(7) . . ? C13 C9 C8 107.8(9) . . ? C13 C9 B10 117.8(9) . . ? C8 C9 B10 121.0(8) . . ? C13 C9 B4 127.0(10) . . ? C8 C9 B4 114.1(8) . . ? B10 C9 B4 64.3(7) . . ? C13 C9 B3 118.2(9) . . ? C8 C9 B3 62.3(6) . . ? B10 C9 B3 117.4(8) . . ? B4 C9 B3 61.0(7) . . ? C12 C11 C8 107.5(11) . . ? C11 C12 C13 104.5(10) . . ? C9 C13 C12 105.8(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.496 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.094 #===END data_[(Me3NH)2Cl][4] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H114 B33 Cl3 N6' _chemical_formula_weight 1058.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 11.8388(15) _cell_length_b 34.882(4) _cell_length_c 16.429(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6784.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 0.166 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.697990 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _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 50071 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6070 _reflns_number_gt 3749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_cell_refinement 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_data_reduction 'BRUKER KAPPA APEXII DUO 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^)+(0.1319P)^2^+24.8388P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6070 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1626 _refine_ls_R_factor_gt 0.1056 _refine_ls_wR_factor_ref 0.3113 _refine_ls_wR_factor_gt 0.2622 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 C8 C 0.9892(3) 0.05767(14) 0.6272(3) 0.0270(11) Uani 1 1 d . . . C9 C 0.9904(4) 0.09873(15) 0.5880(3) 0.0347(12) Uani 1 1 d . . . C11 C 1.0842(4) 0.03509(17) 0.5833(3) 0.0443(14) Uani 1 1 d . . . H11A H 1.1495 0.0314 0.6201 0.053 Uiso 1 1 calc R . . H11B H 1.0564 0.0096 0.5659 0.053 Uiso 1 1 calc R . . C12 C 1.1177(7) 0.0584(2) 0.5110(5) 0.095(3) Uani 1 1 d . . . H12A H 1.0811 0.0481 0.4615 0.114 Uiso 1 1 calc R . . H12B H 1.2006 0.0571 0.5034 0.114 Uiso 1 1 calc R . . C13 C 1.0822(6) 0.0993(2) 0.5238(4) 0.067(2) Uani 1 1 d . . . H13A H 1.0530 0.1104 0.4725 0.081 Uiso 1 1 calc R . . H13B H 1.1470 0.1149 0.5425 0.081 Uiso 1 1 calc R . . B1 B 0.7688(5) 0.08560(18) 0.6395(5) 0.0454(17) Uani 1 1 d . . . H1 H 0.6900 0.0701 0.6209 0.055 Uiso 1 1 calc R . . B2 B 0.8567(5) 0.03930(17) 0.6420(4) 0.0380(15) Uani 1 1 d . . . H2 H 0.7942 0.0172 0.6213 0.046 Uiso 1 1 calc R . . B3 B 0.8798(5) 0.06876(17) 0.5621(4) 0.0360(14) Uani 1 1 d . . . H3 H 0.8618 0.0559 0.5010 0.043 Uiso 1 1 calc R . . B4 B 0.8566(6) 0.11728(18) 0.5698(4) 0.0423(15) Uani 1 1 d . . . H4 H 0.8233 0.1311 0.5131 0.051 Uiso 1 1 calc R . . B5 B 0.8147(5) 0.13668(17) 0.6597(4) 0.0402(15) Uani 1 1 d . . . H5 H 0.7567 0.1618 0.6525 0.048 Uiso 1 1 calc R . . B6 B 0.7918(5) 0.10774(19) 0.7464(4) 0.0456(16) Uani 1 1 d . . . H6 H 0.7219 0.1164 0.7885 0.055 Uiso 1 1 calc R . . B7 B 0.8165(6) 0.0588(2) 0.7358(5) 0.0537(19) Uani 1 1 d . . . H7 H 0.7599 0.0397 0.7726 0.064 Uiso 1 1 calc R . . B10 B 0.9594(5) 0.13827(18) 0.6341(4) 0.0382(14) Uani 1 1 d . . . H10 H 1.0336 0.1581 0.6303 0.046 Uiso 1 1 calc R . . B11 B 0.9144(5) 0.13485(18) 0.7371(4) 0.0366(14) Uani 1 1 d . . . H11 H 0.9672 0.1549 0.7744 0.044 Uiso 1 1 calc R . . B12 B 0.9155(6) 0.08730(19) 0.7831(4) 0.0459(16) Uani 1 1 d . . . H12 H 0.9697 0.0876 0.8390 0.055 Uiso 1 1 calc R . . B13 B 0.9577(6) 0.04803(18) 0.7191(4) 0.0405(15) Uani 1 1 d . . . H13 H 1.0310 0.0330 0.7481 0.049 Uiso 1 1 calc R . . C8' C -0.0352(4) 0.22833(14) 0.3940(4) 0.0389(13) Uani 1 1 d . . . C11' C -0.1520(5) 0.2164(2) 0.4266(6) 0.099(4) Uani 1 1 d . . . H11C H -0.2017 0.2084 0.3812 0.119 Uiso 1 1 calc R . . H11D H -0.1444 0.1946 0.4650 0.119 Uiso 1 1 calc R . . C12' C -0.2001(9) 0.2500 0.4686(7) 0.123(7) Uani 1 2 d S . . H12C H -0.1786 0.2500 0.5269 0.148 Uiso 1 2 calc SR . . H12D H -0.2835 0.2500 0.4646 0.148 Uiso 1 2 calc SR . . N1 N 0.4637(3) 0.17514(14) 0.5108(3) 0.0416(11) Uani 1 1 d . . . H1A H 0.4609 0.1971 0.5428 0.050 Uiso 1 1 calc R . . N2 N 0.7099(4) 0.08569(13) 0.2775(3) 0.0457(12) Uani 1 1 d . . . H2A H 0.6460 0.0860 0.3105 0.055 Uiso 1 1 calc R . . N3 N 0.2440(4) 0.2500 0.7159(3) 0.0239(12) Uani 1 2 d S . . H3A H 0.3068 0.2500 0.6819 0.029 Uiso 1 2 calc SR . . N4 N 0.5042(9) 0.0091(3) 0.4843(6) 0.035(3) Uani 0.50 1 d P . . C21 C 0.4779(4) 0.18899(16) 0.4263(3) 0.0406(13) Uani 1 1 d . . . H21A H 0.5521 0.2011 0.4206 0.061 Uiso 1 1 calc R . . H21B H 0.4186 0.2077 0.4138 0.061 Uiso 1 1 calc R . . H21C H 0.4723 0.1673 0.3886 0.061 Uiso 1 1 calc R . . C22 C 0.3561(4) 0.15538(15) 0.5249(3) 0.0366(12) Uani 1 1 d . . . H22A H 0.3533 0.1461 0.5812 0.055 Uiso 1 1 calc R . . H22B H 0.3495 0.1336 0.4875 0.055 Uiso 1 1 calc R . . H22C H 0.2935 0.1732 0.5156 0.055 Uiso 1 1 calc R . . C23 C 0.5620(4) 0.15346(18) 0.5403(3) 0.0457(14) Uani 1 1 d . . . H23A H 0.5471 0.1441 0.5955 0.069 Uiso 1 1 calc R . . H23B H 0.6285 0.1702 0.5409 0.069 Uiso 1 1 calc R . . H23C H 0.5760 0.1316 0.5041 0.069 Uiso 1 1 calc R . . C24 C 0.6718(6) 0.0907(2) 0.1928(4) 0.072(2) Uani 1 1 d . . . H24A H 0.6282 0.0682 0.1759 0.107 Uiso 1 1 calc R . . H24B H 0.7377 0.0937 0.1572 0.107 Uiso 1 1 calc R . . H24C H 0.6243 0.1137 0.1890 0.107 Uiso 1 1 calc R . . C25 C 0.7838(7) 0.1177(2) 0.3039(4) 0.076(2) Uani 1 1 d . . . H25A H 0.7458 0.1422 0.2935 0.114 Uiso 1 1 calc R . . H25B H 0.8549 0.1168 0.2734 0.114 Uiso 1 1 calc R . . H25C H 0.7995 0.1153 0.3622 0.114 Uiso 1 1 calc R . . C26 C 0.7662(7) 0.04823(19) 0.2892(5) 0.075(2) Uani 1 1 d . . . H26A H 0.7165 0.0277 0.2698 0.112 Uiso 1 1 calc R . . H26B H 0.7822 0.0444 0.3472 0.112 Uiso 1 1 calc R . . H26C H 0.8370 0.0478 0.2584 0.112 Uiso 1 1 calc R . . C27 C 0.1773(4) 0.21494(14) 0.6975(3) 0.0371(12) Uani 1 1 d . . . H27A H 0.1523 0.2156 0.6406 0.056 Uiso 1 1 calc R . . H27B H 0.1112 0.2139 0.7334 0.056 Uiso 1 1 calc R . . H27C H 0.2243 0.1922 0.7063 0.056 Uiso 1 1 calc R . . C28 C 0.2855(6) 0.2500 0.8016(4) 0.0361(17) Uani 1 2 d S . . H28A H 0.3282 0.2264 0.8120 0.054 Uiso 0.50 1 calc PR . . H28B H 0.2210 0.2513 0.8389 0.054 Uiso 1 2 calc SR . . H28C H 0.3347 0.2722 0.8103 0.054 Uiso 0.50 1 calc PR . . C29 C 0.4896(12) 0.0205(4) 0.5688(7) 0.056(3) Uani 0.50 1 d P . . C30 C 0.4192(9) -0.0171(3) 0.4505(7) 0.043(3) Uani 0.50 1 d P . . Cl1 Cl 0.47126(13) 0.2500 0.61953(10) 0.0314(4) Uani 1 2 d S . . Cl2 Cl 0.48519(13) 0.08240(4) 0.37291(9) 0.0523(5) Uani 1 1 d . . . B1' B 0.1909(6) 0.2500 0.4123(5) 0.0326(18) Uani 1 2 d S . . H1' H 0.2420 0.2500 0.4696 0.039 Uiso 1 2 calc SR . . B2' B 0.0904(6) 0.2086(2) 0.4253(8) 0.098(4) Uani 1 1 d . . . H2' H 0.1031 0.1849 0.4704 0.117 Uiso 1 1 calc R . . B3' B 0.0485(7) 0.2500 0.4639(5) 0.054(3) Uani 1 2 d S . . H3' H 0.0730 0.2500 0.5297 0.065 Uiso 1 2 calc SR . . B6' B 0.2215(10) 0.2500 0.3026(7) 0.201(16) Uani 1 2 d S . . H6' H 0.3107 0.2500 0.2798 0.241 Uiso 1 2 calc SR . . B7' B 0.1739(7) 0.2089(4) 0.3427(10) 0.181(9) Uani 1 1 d . . . H7' H 0.2340 0.1841 0.3405 0.217 Uiso 1 1 calc R . . B12' B 0.1098(7) 0.2282(7) 0.2552(6) 0.29(2) Uani 1 1 d . . . H12' H 0.0805 0.2198 0.1929 0.343 Uiso 1 1 calc R . . B13' B 0.0294(7) 0.2033(4) 0.3276(10) 0.169(8) Uani 1 1 d . . . H13' H -0.0332 0.1848 0.2948 0.203 Uiso 1 1 calc R . . C31 C 0.3762(8) 0.0065(4) 0.5308(8) 0.053(3) Uani 0.50 1 d P . . H12E H 0.984(4) 0.1072(15) 0.741(3) 0.039(14) 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 C8 0.026(2) 0.026(3) 0.030(2) -0.008(2) -0.0048(18) 0.0026(19) C9 0.046(3) 0.028(3) 0.030(2) -0.003(2) 0.005(2) -0.013(2) C11 0.045(3) 0.042(4) 0.045(3) -0.016(3) 0.003(2) 0.003(3) C12 0.107(6) 0.073(6) 0.105(6) 0.007(5) 0.077(5) 0.016(5) C13 0.085(5) 0.052(4) 0.065(4) -0.014(3) 0.037(4) -0.018(4) B1 0.031(3) 0.025(4) 0.081(5) -0.015(3) -0.013(3) -0.002(3) B2 0.030(3) 0.019(3) 0.065(4) -0.005(3) 0.003(3) -0.003(2) B3 0.047(3) 0.022(3) 0.039(3) -0.004(3) -0.020(3) -0.001(3) B4 0.064(4) 0.023(4) 0.041(3) -0.001(3) -0.018(3) 0.000(3) B5 0.046(3) 0.016(3) 0.059(4) -0.008(3) -0.018(3) 0.004(3) B6 0.044(3) 0.036(4) 0.056(4) -0.003(3) 0.014(3) 0.002(3) B7 0.062(4) 0.032(4) 0.067(5) 0.002(3) 0.027(4) -0.002(3) B10 0.047(3) 0.030(4) 0.038(3) -0.001(3) -0.004(3) -0.015(3) B11 0.043(3) 0.024(3) 0.042(3) -0.009(3) -0.001(3) 0.005(3) B12 0.068(4) 0.035(4) 0.035(3) 0.000(3) 0.012(3) 0.013(3) B13 0.063(4) 0.028(4) 0.031(3) -0.002(3) 0.001(3) 0.011(3) C8' 0.030(2) 0.019(3) 0.068(4) 0.002(3) -0.017(2) -0.001(2) C11' 0.038(3) 0.088(7) 0.172(9) 0.100(7) -0.024(4) -0.023(4) C12' 0.045(6) 0.28(2) 0.046(6) 0.000 -0.002(5) 0.000 N1 0.034(2) 0.047(3) 0.044(3) 0.015(2) 0.0006(19) 0.002(2) N2 0.069(3) 0.030(3) 0.038(2) -0.002(2) -0.004(2) -0.005(2) N3 0.028(3) 0.019(3) 0.025(3) 0.000 -0.001(2) 0.000 N4 0.037(4) 0.030(9) 0.039(7) -0.010(5) -0.004(5) -0.001(6) C21 0.045(3) 0.043(4) 0.034(3) 0.014(2) 0.009(2) 0.003(2) C22 0.033(2) 0.038(3) 0.039(3) 0.007(2) 0.002(2) -0.001(2) C23 0.039(3) 0.054(4) 0.044(3) 0.008(3) -0.002(2) 0.015(3) C24 0.070(4) 0.101(6) 0.044(4) 0.005(4) -0.005(3) -0.006(4) C25 0.104(6) 0.051(5) 0.073(5) -0.018(4) -0.006(4) -0.024(4) C26 0.103(6) 0.036(4) 0.084(5) 0.011(4) 0.015(4) 0.011(4) C27 0.044(3) 0.022(3) 0.046(3) -0.002(2) -0.008(2) -0.002(2) C28 0.041(4) 0.038(5) 0.029(4) 0.000 -0.009(3) 0.000 C29 0.083(9) 0.040(8) 0.044(7) -0.024(6) 0.011(6) -0.009(7) C30 0.040(6) 0.033(7) 0.055(7) -0.009(5) -0.014(5) -0.012(5) Cl1 0.0321(8) 0.0287(10) 0.0335(9) 0.000 0.0007(7) 0.000 Cl2 0.0688(10) 0.0394(9) 0.0487(8) -0.0019(7) 0.0061(7) 0.0039(7) B1' 0.033(4) 0.027(5) 0.038(4) 0.000 -0.014(3) 0.000 B2' 0.043(4) 0.026(4) 0.224(13) 0.035(6) -0.057(6) -0.003(3) B3' 0.040(5) 0.098(9) 0.025(4) 0.000 -0.017(4) 0.000 B6' 0.027(6) 0.56(5) 0.019(5) 0.000 -0.011(4) 0.000 B7' 0.040(5) 0.199(15) 0.305(19) -0.239(15) -0.067(8) 0.052(6) B12' 0.039(4) 0.72(6) 0.104(8) -0.25(2) -0.015(5) 0.037(11) B13' 0.038(4) 0.162(12) 0.308(19) -0.201(13) -0.062(8) 0.028(6) C31 0.023(5) 0.062(9) 0.073(8) 0.008(7) 0.010(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 C8 C11 1.552(6) . ? C8 C9 1.570(7) . ? C8 B13 1.591(7) . ? C8 B2 1.711(7) . ? C8 B3 1.723(7) . ? C9 C13 1.514(7) . ? C9 B10 1.616(8) . ? C9 B3 1.729(7) . ? C9 B4 1.737(8) . ? C11 C12 1.493(9) . ? C12 C13 1.502(10) . ? B1 B5 1.892(8) . ? B1 B4 1.902(10) . ? B1 B3 1.920(9) . ? B1 B7 1.923(10) . ? B1 B6 1.937(10) . ? B2 B3 1.688(9) . ? B2 B7 1.751(9) . ? B2 B13 1.769(9) . ? B3 B4 1.719(9) . ? B4 B5 1.699(9) . ? B4 B10 1.771(8) . ? B5 B11 1.737(8) . ? B5 B10 1.765(9) . ? B5 B6 1.767(10) . ? B6 B12 1.737(10) . ? B6 B11 1.739(9) . ? B6 B7 1.742(10) . ? B7 B12 1.723(11) . ? B7 B13 1.735(9) . ? B10 B11 1.778(8) . ? B11 B12 1.822(9) . ? B12 B13 1.797(8) . ? C8' C8' 1.512(10) 7_565 ? C8' C11' 1.541(8) . ? C8' B13' 1.593(12) . ? C8' B3' 1.695(8) . ? C8' B2' 1.718(8) . ? C11' C12' 1.476(11) . ? C12' C11' 1.476(11) 7_565 ? N1 C22 1.468(6) . ? N1 C23 1.470(6) . ? N1 C21 1.478(6) . ? N2 C24 1.473(7) . ? N2 C26 1.479(8) . ? N2 C25 1.483(8) . ? N3 C27 1.487(5) . ? N3 C27 1.487(5) 7_565 ? N3 C28 1.493(8) . ? N4 N4 0.823(15) 5_656 ? N4 C29 1.354(16) 5_656 ? N4 C30 1.431(15) 5_656 ? N4 C29 1.454(15) . ? N4 C30 1.467(15) . ? N4 C31 1.537(15) 5_656 ? N4 C31 1.699(14) . ? C29 C30 1.132(16) 5_656 ? C29 N4 1.354(16) 5_656 ? C29 C31 1.559(17) . ? C30 C29 1.132(16) 5_656 ? C30 N4 1.431(15) 5_656 ? C30 C31 1.635(17) . ? B1' B6' 1.838(14) . ? B1' B7' 1.844(9) . ? B1' B7' 1.844(9) 7_565 ? B1' B2' 1.884(9) . ? B1' B2' 1.884(9) 7_565 ? B2' B3' 1.654(11) . ? B2' B7' 1.679(19) . ? B2' B13' 1.769(17) . ? B3' B2' 1.654(11) 7_565 ? B3' C8' 1.695(8) 7_565 ? B6' B7' 1.674(19) . ? B6' B7' 1.674(19) 7_565 ? B6' B12' 1.712(15) . ? B6' B12' 1.712(15) 7_565 ? B7' B13' 1.740(11) . ? B7' B12' 1.76(2) . ? B12' B12' 1.52(5) 7_565 ? B12' B13' 1.75(3) . ? C31 N4 1.537(15) 5_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 C11 C8 C9 105.4(4) . . ? C11 C8 B13 120.3(4) . . ? C9 C8 B13 125.7(4) . . ? C11 C8 B2 122.7(4) . . ? C9 C8 B2 114.1(4) . . ? B13 C8 B2 64.6(4) . . ? C11 C8 B3 111.7(4) . . ? C9 C8 B3 63.1(3) . . ? B13 C8 B3 117.4(4) . . ? B2 C8 B3 58.9(3) . . ? C13 C9 C8 107.8(5) . . ? C13 C9 B10 118.5(5) . . ? C8 C9 B10 125.7(4) . . ? C13 C9 B3 112.4(5) . . ? C8 C9 B3 62.8(3) . . ? B10 C9 B3 117.4(4) . . ? C13 C9 B4 121.9(5) . . ? C8 C9 B4 113.7(4) . . ? B10 C9 B4 63.6(3) . . ? B3 C9 B4 59.5(3) . . ? C12 C11 C8 106.6(5) . . ? C11 C12 C13 109.4(5) . . ? C12 C13 C9 106.6(5) . . ? B5 B1 B4 53.2(3) . . ? B5 B1 B3 102.0(4) . . ? B4 B1 B3 53.5(3) . . ? B5 B1 B7 103.3(4) . . ? B4 B1 B7 128.2(4) . . ? B3 B1 B7 101.2(4) . . ? B5 B1 B6 54.9(3) . . ? B4 B1 B6 103.7(4) . . ? B3 B1 B6 128.7(4) . . ? B7 B1 B6 53.6(4) . . ? B3 B2 C8 60.9(3) . . ? B3 B2 B7 119.5(5) . . ? C8 B2 B7 103.2(4) . . ? B3 B2 B13 110.0(4) . . ? C8 B2 B13 54.4(3) . . ? B7 B2 B13 59.1(4) . . ? B2 B3 B4 121.1(5) . . ? B2 B3 C8 60.2(3) . . ? B4 B3 C8 107.2(4) . . ? B2 B3 C9 107.4(4) . . ? B4 B3 C9 60.5(3) . . ? C8 B3 C9 54.1(3) . . ? B2 B3 B1 64.0(4) . . ? B4 B3 B1 62.7(4) . . ? C8 B3 B1 99.9(4) . . ? C9 B3 B1 99.8(4) . . ? B5 B4 B3 120.1(5) . . ? B5 B4 C9 105.4(4) . . ? B3 B4 C9 60.0(3) . . ? B5 B4 B10 61.1(3) . . ? B3 B4 B10 109.9(4) . . ? C9 B4 B10 54.8(3) . . ? B5 B4 B1 63.1(4) . . ? B3 B4 B1 63.8(4) . . ? C9 B4 B1 100.3(4) . . ? B10 B4 B1 104.8(4) . . ? B4 B5 B11 115.1(4) . . ? B4 B5 B10 61.5(4) . . ? B11 B5 B10 61.0(3) . . ? B4 B5 B6 121.2(5) . . ? B11 B5 B6 59.5(4) . . ? B10 B5 B6 111.0(4) . . ? B4 B5 B1 63.7(4) . . ? B11 B5 B1 106.8(4) . . ? B10 B5 B1 105.5(4) . . ? B6 B5 B1 63.8(4) . . ? B12 B6 B11 63.2(4) . . ? B12 B6 B7 59.4(4) . . ? B11 B6 B7 112.6(5) . . ? B12 B6 B5 112.6(4) . . ? B11 B6 B5 59.4(3) . . ? B7 B6 B5 117.0(5) . . ? B12 B6 B1 105.6(4) . . ? B11 B6 B1 104.8(4) . . ? B7 B6 B1 62.8(4) . . ? B5 B6 B1 61.2(4) . . ? B12 B7 B13 62.6(4) . . ? B12 B7 B6 60.2(4) . . ? B13 B7 B6 112.9(5) . . ? B12 B7 B2 115.8(5) . . ? B13 B7 B2 61.0(3) . . ? B6 B7 B2 120.9(5) . . ? B12 B7 B1 106.8(5) . . ? B13 B7 B1 104.9(4) . . ? B6 B7 B1 63.6(4) . . ? B2 B7 B1 62.9(4) . . ? C9 B10 B5 107.8(4) . . ? C9 B10 B4 61.5(3) . . ? B5 B10 B4 57.4(3) . . ? C9 B10 B11 117.2(4) . . ? B5 B10 B11 58.7(3) . . ? B4 B10 B11 109.5(4) . . ? B5 B11 B6 61.1(4) . . ? B5 B11 B10 60.3(4) . . ? B6 B11 B10 111.7(4) . . ? B5 B11 B12 110.0(4) . . ? B6 B11 B12 58.3(4) . . ? B10 B11 B12 116.9(4) . . ? B7 B12 B6 60.5(4) . . ? B7 B12 B13 59.0(4) . . ? B6 B12 B13 110.1(5) . . ? B7 B12 B11 109.5(5) . . ? B6 B12 B11 58.4(3) . . ? B13 B12 B11 117.0(4) . . ? C8 B13 B7 109.3(5) . . ? C8 B13 B2 61.0(3) . . ? B7 B13 B2 60.0(4) . . ? C8 B13 B12 117.3(5) . . ? B7 B13 B12 58.3(4) . . ? B2 B13 B12 111.2(5) . . ? C8' C8' C11' 105.7(4) 7_565 . ? C8' C8' B13' 123.3(7) 7_565 . ? C11' C8' B13' 121.4(7) . . ? C8' C8' B3' 63.5(2) 7_565 . ? C11' C8' B3' 114.2(6) . . ? B13' C8' B3' 115.3(5) . . ? C8' C8' B2' 113.7(3) 7_565 . ? C11' C8' B2' 124.3(5) . . ? B13' C8' B2' 64.5(6) . . ? B3' C8' B2' 58.0(4) . . ? C12' C11' C8' 107.1(7) . . ? C11' C12' C11' 105.4(9) . 7_565 ? C22 N1 C23 113.2(4) . . ? C22 N1 C21 113.6(4) . . ? C23 N1 C21 112.8(4) . . ? C24 N2 C26 111.5(5) . . ? C24 N2 C25 111.5(5) . . ? C26 N2 C25 111.1(6) . . ? C27 N3 C27 110.7(5) . 7_565 ? C27 N3 C28 111.5(3) . . ? C27 N3 C28 111.5(3) 7_565 . ? N4 N4 C29 79.8(17) 5_656 5_656 ? N4 N4 C30 75.9(16) 5_656 5_656 ? C29 N4 C30 126.6(11) 5_656 5_656 ? N4 N4 C29 66.4(16) 5_656 . ? C29 N4 C29 146.2(7) 5_656 . ? C30 N4 C29 46.2(7) 5_656 . ? N4 N4 C30 71.1(15) 5_656 . ? C29 N4 C30 47.1(8) 5_656 . ? C30 N4 C30 147.0(6) 5_656 . ? C29 N4 C30 116.8(9) . . ? N4 N4 C31 86.5(17) 5_656 5_656 ? C29 N4 C31 64.9(9) 5_656 5_656 ? C30 N4 C31 66.8(8) 5_656 5_656 ? C29 N4 C31 111.1(10) . 5_656 ? C30 N4 C31 110.5(10) . 5_656 ? N4 N4 C31 64.6(15) 5_656 . ? C29 N4 C31 107.3(10) 5_656 . ? C30 N4 C31 103.8(9) 5_656 . ? C29 N4 C31 58.7(8) . . ? C30 N4 C31 61.7(8) . . ? C31 N4 C31 151.1(6) 5_656 . ? C30 C29 N4 71.7(10) 5_656 5_656 ? C30 C29 N4 65.8(9) 5_656 . ? N4 C29 N4 33.8(7) 5_656 . ? C30 C29 C31 132.5(11) 5_656 . ? N4 C29 C31 63.2(8) 5_656 . ? N4 C29 C31 68.5(8) . . ? C29 C30 N4 68.0(9) 5_656 5_656 ? C29 C30 N4 61.2(9) 5_656 . ? N4 C30 N4 33.0(6) 5_656 . ? C29 C30 C31 125.2(10) 5_656 . ? N4 C30 C31 59.7(7) 5_656 . ? N4 C30 C31 66.1(7) . . ? B6' B1' B7' 54.1(6) . . ? B6' B1' B7' 54.1(6) . 7_565 ? B7' B1' B7' 101.9(13) . 7_565 ? B6' B1' B2' 103.6(5) . . ? B7' B1' B2' 53.5(6) . . ? B7' B1' B2' 126.7(6) 7_565 . ? B6' B1' B2' 103.6(5) . 7_565 ? B7' B1' B2' 126.7(6) . 7_565 ? B7' B1' B2' 53.5(6) 7_565 7_565 ? B2' B1' B2' 100.2(6) . 7_565 ? B3' B2' B7' 118.7(8) . . ? B3' B2' C8' 60.3(4) . . ? B7' B2' C8' 105.4(8) . . ? B3' B2' B13' 108.5(6) . . ? B7' B2' B13' 60.5(6) . . ? C8' B2' B13' 54.3(4) . . ? B3' B2' B1' 64.1(4) . . ? B7' B2' B1' 62.0(5) . . ? C8' B2' B1' 101.8(5) . . ? B13' B2' B1' 103.6(8) . . ? B2' B3' B2' 121.7(10) . 7_565 ? B2' B3' C8' 61.7(4) . . ? B2' B3' C8' 107.8(6) 7_565 . ? B2' B3' C8' 107.8(6) . 7_565 ? B2' B3' C8' 61.7(4) 7_565 7_565 ? C8' B3' C8' 53.0(4) . 7_565 ? B7' B6' B7' 117.6(9) . 7_565 ? B7' B6' B12' 62.6(9) . . ? B7' B6' B12' 107.3(9) 7_565 . ? B7' B6' B12' 107.3(9) . 7_565 ? B7' B6' B12' 62.6(9) 7_565 7_565 ? B12' B6' B12' 52.6(16) . 7_565 ? B7' B6' B1' 63.1(5) . . ? B7' B6' B1' 63.1(5) 7_565 . ? B12' B6' B1' 107.0(8) . . ? B12' B6' B1' 107.0(8) 7_565 . ? B6' B7' B2' 121.5(7) . . ? B6' B7' B13' 111.9(12) . . ? B2' B7' B13' 62.3(7) . . ? B6' B7' B12' 59.8(11) . . ? B2' B7' B12' 114.1(6) . . ? B13' B7' B12' 60.2(9) . . ? B6' B7' B1' 62.8(6) . . ? B2' B7' B1' 64.4(5) . . ? B13' B7' B1' 106.5(6) . . ? B12' B7' B1' 104.8(10) . . ? B12' B12' B6' 63.7(8) 7_565 . ? B12' B12' B13' 119.8(7) 7_565 . ? B6' B12' B13' 109.3(8) . . ? B12' B12' B7' 112.5(8) 7_565 . ? B6' B12' B7' 57.7(6) . . ? B13' B12' B7' 59.4(8) . . ? C8' B13' B7' 108.2(6) . . ? C8' B13' B12' 116.9(10) . . ? B7' B13' B12' 60.4(9) . . ? C8' B13' B2' 61.2(6) . . ? B7' B13' B2' 57.2(7) . . ? B12' B13' B2' 110.0(6) . . ? N4 C31 C29 51.8(7) 5_656 . ? N4 C31 C30 53.5(7) 5_656 . ? C29 C31 C30 102.3(7) . . ? N4 C31 N4 28.9(6) 5_656 . ? C29 C31 N4 52.8(7) . . ? C30 C31 N4 52.2(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.873 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.088 #===END