Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_mag149 _database_code_CSD 160870 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Graham, Mark A.' 'Rayner, Chris' 'Thornton-Pett, Mark' 'Wadsworth, Alan H.' _publ_contact_author_name 'Dr Chris Rayner' _publ_contact_author_address ; Dr Chris Rayner Department of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_email 'CHRISR@CHEM.LEEDS.AC.UK' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H42 B N O' _chemical_formula_weight 551.55 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' '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.0282(2) _cell_length_b 9.7091(2) _cell_length_c 10.3036(2) _cell_angle_alpha 114.3040(10) _cell_angle_beta 97.6460(10) _cell_angle_gamma 99.5540(10) _cell_volume 791.07(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9677 _exptl_absorpt_correction_T_max 0.9886 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8491 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5075 _reflns_number_gt 4754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.1688P] 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 0.164(15) _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 2.4(17) _refine_ls_number_reflns 5075 _refine_ls_number_parameters 382 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.051 _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 C2 C 0.6046(2) 0.3589(3) 0.1888(2) 0.0428(5) Uani 1 1 d . . . H2A H 0.7117 0.4199 0.2398 0.051 Uiso 1 1 calc R . . H2B H 0.5917 0.2847 0.0851 0.051 Uiso 1 1 calc R . . C3 C 0.4794(3) 0.4361(3) 0.2293(3) 0.0516(6) Uani 1 1 d . . . H3 H 0.5074 0.5468 0.3060 0.062 Uiso 1 1 calc R . . C4 C 0.3305(4) 0.3786(4) 0.1239(3) 0.0686(9) Uani 1 1 d . . . H4A H 0.3380 0.4101 0.0445 0.082 Uiso 1 1 calc R . . H4B H 0.2494 0.4201 0.1726 0.082 Uiso 1 1 calc R . . C5 C 0.2949(3) 0.2034(4) 0.0642(3) 0.0652(9) Uani 1 1 d . . . H5 H 0.1811 0.1595 0.0415 0.078 Uiso 1 1 calc R . . C6 C 0.3763(3) 0.1713(3) 0.1863(2) 0.0518(6) Uani 1 1 d . . . H6A H 0.3044 0.1557 0.2464 0.062 Uiso 1 1 calc R . . H6B H 0.4168 0.0774 0.1445 0.062 Uiso 1 1 calc R . . C8 C 0.2640(3) -0.0061(3) -0.1700(3) 0.0596(7) Uani 1 1 d . . . H8A H 0.1621 0.0024 -0.2105 0.071 Uiso 1 1 calc R . . H8B H 0.2479 -0.0780 -0.1246 0.071 Uiso 1 1 calc R . . C9 C 0.3490(4) -0.0670(3) -0.2893(3) 0.0682(8) Uani 1 1 d . . . H9A H 0.3677 0.0068 -0.3311 0.102 Uiso 1 1 calc R . . H9B H 0.2871 -0.1681 -0.3657 0.102 Uiso 1 1 calc R . . H9C H 0.4478 -0.0794 -0.2489 0.102 Uiso 1 1 calc R . . C10 C 0.5740(2) 0.3522(2) 0.4311(2) 0.0374(5) Uani 1 1 d . . . H10 H 0.6474 0.4572 0.4736 0.045 Uiso 1 1 calc R . . C11 C 0.6675(3) 0.2375(3) 0.4329(3) 0.0521(6) Uani 1 1 d . . . H11A H 0.5992 0.1327 0.3908 0.078 Uiso 1 1 calc R . . H11B H 0.7186 0.2668 0.5339 0.078 Uiso 1 1 calc R . . H11C H 0.7453 0.2383 0.3753 0.078 Uiso 1 1 calc R . . C12 C 0.4491(2) 0.3670(3) 0.5179(2) 0.0380(5) Uani 1 1 d . . . C13 C 0.4131(3) 0.5098(3) 0.5848(2) 0.0475(6) Uani 1 1 d . . . H13 H 0.4685 0.5977 0.5777 0.057 Uiso 1 1 calc R . . C14 C 0.2978(3) 0.5256(3) 0.6616(3) 0.0561(6) Uani 1 1 d . . . H14 H 0.2747 0.6242 0.7067 0.067 Uiso 1 1 calc R . . C15 C 0.2162(3) 0.4006(3) 0.6735(2) 0.0527(6) Uani 1 1 d . . . H15 H 0.1363 0.4119 0.7256 0.063 Uiso 1 1 calc R . . C16 C 0.2517(3) 0.2582(3) 0.6086(2) 0.0481(6) Uani 1 1 d . . . H16 H 0.1960 0.1710 0.6165 0.058 Uiso 1 1 calc R . . C17 C 0.3678(3) 0.2413(3) 0.5321(2) 0.0433(5) Uani 1 1 d . . . H17 H 0.3921 0.1429 0.4891 0.052 Uiso 1 1 calc R . . C111 C 1.1794(2) 0.7468(2) 0.1714(2) 0.0321(4) Uani 1 1 d . . . C112 C 1.2415(2) 0.7347(2) 0.0501(2) 0.0369(5) Uani 1 1 d . . . H112 H 1.1731 0.7073 -0.0399 0.044 Uiso 1 1 calc R . . C113 C 1.3988(3) 0.7613(3) 0.0568(2) 0.0430(5) Uani 1 1 d . . . H113 H 1.4355 0.7491 -0.0286 0.052 Uiso 1 1 calc R . . C114 C 1.5024(3) 0.8051(3) 0.1860(3) 0.0430(5) Uani 1 1 d . . . H114 H 1.6101 0.8239 0.1909 0.052 Uiso 1 1 calc R . . C115 C 1.4458(2) 0.8212(3) 0.3090(2) 0.0430(5) Uani 1 1 d . . . H115 H 1.5153 0.8523 0.3994 0.052 Uiso 1 1 calc R . . C116 C 1.2887(2) 0.7922(2) 0.3005(2) 0.0378(5) Uani 1 1 d . . . H116 H 1.2533 0.8036 0.3862 0.045 Uiso 1 1 calc R . . C121 C 0.9507(2) 0.7165(2) 0.3102(2) 0.0330(4) Uani 1 1 d . . . C122 C 0.9904(2) 0.6049(2) 0.3527(2) 0.0376(5) Uani 1 1 d . . . H122 H 1.0379 0.5305 0.2915 0.045 Uiso 1 1 calc R . . C123 C 0.9636(3) 0.5981(3) 0.4799(2) 0.0439(5) Uani 1 1 d . . . H123 H 0.9933 0.5209 0.5044 0.053 Uiso 1 1 calc R . . C124 C 0.8933(3) 0.7048(3) 0.5714(2) 0.0463(6) Uani 1 1 d . . . H124 H 0.8756 0.7019 0.6592 0.056 Uiso 1 1 calc R . . C125 C 0.8499(3) 0.8142(3) 0.5327(2) 0.0469(6) Uani 1 1 d . . . H125 H 0.8004 0.8866 0.5936 0.056 Uiso 1 1 calc R . . C126 C 0.8777(2) 0.8202(3) 0.4042(2) 0.0386(5) Uani 1 1 d . . . H126 H 0.8462 0.8969 0.3800 0.046 Uiso 1 1 calc R . . C131 C 0.9449(2) 0.8625(2) 0.1320(2) 0.0353(4) Uani 1 1 d . . . C132 C 1.0056(3) 1.0163(2) 0.2421(3) 0.0410(5) Uani 1 1 d . . . H132 H 1.0680 1.0321 0.3313 0.049 Uiso 1 1 calc R . . C133 C 0.9785(3) 1.1458(3) 0.2262(3) 0.0489(6) Uani 1 1 d . . . H133 H 1.0219 1.2473 0.3037 0.059 Uiso 1 1 calc R . . C134 C 0.8886(3) 1.1274(3) 0.0978(3) 0.0554(7) Uani 1 1 d . . . H134 H 0.8682 1.2152 0.0865 0.066 Uiso 1 1 calc R . . C135 C 0.8293(3) 0.9788(3) -0.0135(3) 0.0575(7) Uani 1 1 d . . . H135 H 0.7688 0.9644 -0.1029 0.069 Uiso 1 1 calc R . . C136 C 0.8568(3) 0.8493(3) 0.0035(2) 0.0439(5) Uani 1 1 d . . . H136 H 0.8140 0.7485 -0.0752 0.053 Uiso 1 1 calc R . . C141 C 0.8975(2) 0.5474(2) 0.0242(2) 0.0325(4) Uani 1 1 d . . . C142 C 0.9680(2) 0.4303(2) -0.0520(2) 0.0379(5) Uani 1 1 d . . . H142 H 1.0772 0.4502 -0.0281 0.045 Uiso 1 1 calc R . . C143 C 0.8839(3) 0.2850(3) -0.1622(2) 0.0449(5) Uani 1 1 d . . . H143 H 0.9361 0.2082 -0.2111 0.054 Uiso 1 1 calc R . . C144 C 0.7265(3) 0.2532(3) -0.1999(2) 0.0476(6) Uani 1 1 d . . . H144 H 0.6691 0.1548 -0.2754 0.057 Uiso 1 1 calc R . . C145 C 0.6520(3) 0.3650(3) -0.1273(2) 0.0476(6) Uani 1 1 d . . . H145 H 0.5428 0.3442 -0.1523 0.057 Uiso 1 1 calc R . . C146 C 0.7374(2) 0.5081(3) -0.0175(2) 0.0401(5) Uani 1 1 d . . . H146 H 0.6837 0.5832 0.0319 0.048 Uiso 1 1 calc R . . N1 N 0.50405(19) 0.31238(19) 0.27501(18) 0.0340(4) Uani 1 1 d . . . O7 O 0.3530(2) 0.1414(2) -0.06510(17) 0.0630(5) Uani 1 1 d . . . B1 B 0.9913(3) 0.7180(3) 0.1585(2) 0.0326(5) 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 C2 0.0406(12) 0.0491(12) 0.0390(11) 0.0237(10) 0.0074(9) 0.0015(10) C3 0.0788(17) 0.0433(13) 0.0402(12) 0.0216(11) 0.0136(12) 0.0258(12) C4 0.0704(18) 0.105(2) 0.0464(14) 0.0343(16) 0.0198(13) 0.0544(18) C5 0.0310(12) 0.109(3) 0.0346(12) 0.0178(14) 0.0066(10) 0.0030(13) C6 0.0486(14) 0.0470(13) 0.0388(12) 0.0068(10) 0.0102(10) -0.0097(11) C8 0.0735(18) 0.0538(15) 0.0377(12) 0.0190(12) 0.0064(12) -0.0111(13) C9 0.103(2) 0.0465(14) 0.0404(13) 0.0122(11) 0.0163(14) -0.0013(14) C10 0.0382(11) 0.0377(11) 0.0323(10) 0.0157(9) 0.0036(9) 0.0021(9) C11 0.0486(13) 0.0731(17) 0.0534(14) 0.0408(13) 0.0188(11) 0.0234(12) C12 0.0411(12) 0.0407(11) 0.0274(9) 0.0133(9) 0.0041(8) 0.0055(9) C13 0.0643(15) 0.0365(12) 0.0376(12) 0.0131(10) 0.0139(11) 0.0088(11) C14 0.0773(17) 0.0481(14) 0.0421(13) 0.0137(11) 0.0229(12) 0.0227(13) C15 0.0562(15) 0.0640(16) 0.0369(12) 0.0193(12) 0.0162(11) 0.0156(12) C16 0.0494(14) 0.0550(14) 0.0408(12) 0.0242(11) 0.0128(10) 0.0051(11) C17 0.0491(13) 0.0404(12) 0.0401(11) 0.0185(10) 0.0119(10) 0.0073(10) C111 0.0364(10) 0.0262(9) 0.0323(10) 0.0117(8) 0.0083(8) 0.0072(8) C112 0.0413(11) 0.0349(11) 0.0346(10) 0.0152(9) 0.0111(9) 0.0083(9) C113 0.0417(12) 0.0393(12) 0.0435(12) 0.0127(10) 0.0165(10) 0.0081(10) C114 0.0322(11) 0.0334(11) 0.0539(13) 0.0101(10) 0.0111(10) 0.0071(9) C115 0.0389(12) 0.0376(11) 0.0459(12) 0.0140(10) 0.0037(10) 0.0095(9) C116 0.0400(12) 0.0373(11) 0.0347(10) 0.0150(9) 0.0079(9) 0.0090(9) C121 0.0296(10) 0.0343(11) 0.0297(9) 0.0122(8) 0.0038(8) 0.0017(8) C122 0.0436(12) 0.0346(10) 0.0355(10) 0.0175(9) 0.0096(9) 0.0059(9) C123 0.0477(13) 0.0431(12) 0.0399(11) 0.0246(10) 0.0026(10) -0.0023(10) C124 0.0497(14) 0.0515(14) 0.0286(10) 0.0163(10) 0.0067(9) -0.0047(11) C125 0.0506(13) 0.0504(13) 0.0334(11) 0.0124(10) 0.0162(10) 0.0074(11) C126 0.0382(11) 0.0407(11) 0.0341(10) 0.0143(9) 0.0091(9) 0.0079(9) C131 0.0350(11) 0.0402(11) 0.0387(11) 0.0215(9) 0.0165(9) 0.0124(9) C132 0.0423(12) 0.0382(11) 0.0480(12) 0.0219(10) 0.0168(10) 0.0109(9) C133 0.0523(14) 0.0411(12) 0.0662(15) 0.0283(12) 0.0306(12) 0.0186(11) C134 0.0638(16) 0.0579(15) 0.0777(18) 0.0474(15) 0.0401(14) 0.0340(13) C135 0.0647(16) 0.0782(19) 0.0576(15) 0.0473(15) 0.0242(13) 0.0345(14) C136 0.0518(13) 0.0505(13) 0.0407(11) 0.0263(11) 0.0162(10) 0.0204(11) C141 0.0386(11) 0.0352(10) 0.0280(9) 0.0186(8) 0.0081(8) 0.0075(9) C142 0.0421(12) 0.0341(11) 0.0372(11) 0.0169(9) 0.0071(9) 0.0069(9) C143 0.0572(15) 0.0368(11) 0.0364(11) 0.0143(9) 0.0088(10) 0.0071(10) C144 0.0593(15) 0.0407(12) 0.0292(10) 0.0113(10) 0.0042(10) -0.0074(11) C145 0.0394(12) 0.0615(15) 0.0343(11) 0.0207(11) 0.0052(9) -0.0030(11) C146 0.0408(12) 0.0463(12) 0.0307(10) 0.0154(10) 0.0087(9) 0.0075(9) N1 0.0370(9) 0.0311(8) 0.0322(8) 0.0132(7) 0.0075(7) 0.0060(7) O7 0.0474(10) 0.0797(13) 0.0346(8) 0.0071(9) 0.0099(7) -0.0053(9) B1 0.0370(12) 0.0320(11) 0.0293(10) 0.0143(9) 0.0084(9) 0.0071(9) _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 C2 C3 1.471(3) . ? C2 N1 1.492(3) . ? C3 C4 1.470(4) . ? C3 N1 1.497(3) . ? C4 C5 1.510(5) . ? C5 O7 1.429(3) . ? C5 C6 1.540(4) . ? C6 N1 1.486(3) . ? C8 O7 1.406(3) . ? C8 C9 1.501(4) . ? C10 N1 1.507(3) . ? C10 C11 1.510(3) . ? C10 C12 1.520(3) . ? C12 C13 1.387(3) . ? C12 C17 1.389(3) . ? C13 C14 1.381(4) . ? C14 C15 1.371(4) . ? C15 C16 1.381(4) . ? C16 C17 1.384(3) . ? C111 C116 1.401(3) . ? C111 C112 1.406(3) . ? C111 B1 1.652(3) . ? C112 C113 1.388(3) . ? C113 C114 1.378(3) . ? C114 C115 1.388(3) . ? C115 C116 1.383(3) . ? C121 C122 1.404(3) . ? C121 C126 1.405(3) . ? C121 B1 1.657(3) . ? C122 C123 1.389(3) . ? C123 C124 1.392(3) . ? C124 C125 1.374(4) . ? C125 C126 1.402(3) . ? C131 C136 1.396(3) . ? C131 C132 1.409(3) . ? C131 B1 1.644(3) . ? C132 C133 1.389(3) . ? C133 C134 1.383(4) . ? C134 C135 1.379(4) . ? C135 C136 1.395(3) . ? C141 C146 1.392(3) . ? C141 C142 1.397(3) . ? C141 B1 1.646(3) . ? C142 C143 1.397(3) . ? C143 C144 1.370(4) . ? C144 C145 1.378(4) . ? C145 C146 1.387(3) . ? 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 C2 N1 60.70(14) . . ? C4 C3 C2 119.1(2) . . ? C4 C3 N1 108.5(2) . . ? C2 C3 N1 60.32(14) . . ? C3 C4 C5 105.2(2) . . ? O7 C5 C4 108.7(2) . . ? O7 C5 C6 111.8(2) . . ? C4 C5 C6 105.6(2) . . ? N1 C6 C5 104.9(2) . . ? O7 C8 C9 108.1(2) . . ? N1 C10 C11 109.17(18) . . ? N1 C10 C12 109.60(16) . . ? C11 C10 C12 116.16(18) . . ? C13 C12 C17 118.3(2) . . ? C13 C12 C10 119.56(19) . . ? C17 C12 C10 122.1(2) . . ? C14 C13 C12 120.7(2) . . ? C15 C14 C13 120.8(2) . . ? C14 C15 C16 119.1(2) . . ? C15 C16 C17 120.6(2) . . ? C16 C17 C12 120.4(2) . . ? C116 C111 C112 114.79(18) . . ? C116 C111 B1 124.48(17) . . ? C112 C111 B1 120.66(17) . . ? C113 C112 C111 122.6(2) . . ? C114 C113 C112 120.6(2) . . ? C113 C114 C115 118.5(2) . . ? C116 C115 C114 120.3(2) . . ? C115 C116 C111 123.14(19) . . ? C122 C121 C126 115.16(18) . . ? C122 C121 B1 119.59(17) . . ? C126 C121 B1 125.25(18) . . ? C123 C122 C121 123.1(2) . . ? C122 C123 C124 119.9(2) . . ? C125 C124 C123 118.9(2) . . ? C124 C125 C126 120.7(2) . . ? C125 C126 C121 122.2(2) . . ? C136 C131 C132 115.0(2) . . ? C136 C131 B1 125.72(18) . . ? C132 C131 B1 119.13(19) . . ? C133 C132 C131 123.0(2) . . ? C134 C133 C132 120.2(2) . . ? C135 C134 C133 118.5(2) . . ? C134 C135 C136 120.9(2) . . ? C135 C136 C131 122.4(2) . . ? C146 C141 C142 114.92(18) . . ? C146 C141 B1 120.87(18) . . ? C142 C141 B1 124.17(17) . . ? C143 C142 C141 122.5(2) . . ? C144 C143 C142 120.1(2) . . ? C143 C144 C145 119.4(2) . . ? C144 C145 C146 119.6(2) . . ? C145 C146 C141 123.5(2) . . ? C6 N1 C2 114.45(16) . . ? C6 N1 C3 108.10(19) . . ? C2 N1 C3 58.98(15) . . ? C6 N1 C10 120.49(17) . . ? C2 N1 C10 118.22(16) . . ? C3 N1 C10 121.45(16) . . ? C8 O7 C5 113.63(19) . . ? C131 B1 C141 111.76(16) . . ? C131 B1 C111 105.07(15) . . ? C141 B1 C111 111.61(16) . . ? C131 B1 C121 112.43(16) . . ? C141 B1 C121 106.32(15) . . ? C111 B1 C121 109.74(16) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.400 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.029