# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Takayuki Kawashima' _publ_contact_author_email TAKAYUKI@CHEM.S.U-TOKYO.AC.JP _publ_section_title ; Synthesis and reactivity of a bis(dimesitylboryl)azaborine and its fluoride sensing ability ; loop_ _publ_author_name 'Takayuki Kawashima' 'Tomohiro Agou' 'Junji Kobayashi' 'Masaki Sekine' # Attachment 'BMes2.cif' data_crystalclear _database_code_depnum_ccdc_archive 'CCDC 697739' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H76 B3 N' _chemical_formula_weight 891.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 14.1943(11) _cell_length_b 23.5686(13) _cell_length_c 16.7739(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.4178(10) _cell_angle_gamma 90.00 _cell_volume 5324.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11920 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9877 _exptl_absorpt_correction_T_max 0.9877 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ccd _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40560 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11920 _reflns_number_gt 9120 _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^)+(0.0800P)^2^+0.5501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11920 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1544 _refine_ls_wR_factor_gt 0.1401 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 N2 N 0.40601(8) 0.54375(5) 0.42785(7) 0.0198(2) Uani 1 1 d . . . C1 C 0.31510(10) 0.45853(5) 0.36498(8) 0.0186(3) Uani 1 1 d . . . C2 C 0.45256(10) 0.54811(5) 0.36600(8) 0.0185(3) Uani 1 1 d . . . C3 C 0.15932(10) 0.30103(6) 0.39009(9) 0.0220(3) Uani 1 1 d . . . C4 C 0.25358(10) 0.41326(5) 0.37216(9) 0.0202(3) Uani 1 1 d . . . H1 H 0.2380 0.3851 0.3294 0.024 Uiso 1 1 calc R . . C5 C 0.34225(10) 0.49916(5) 0.43046(8) 0.0184(3) Uani 1 1 d . . . C6 C 0.56900(11) 0.59615(6) 0.31070(9) 0.0253(3) Uani 1 1 d . . . H2 H 0.6132 0.6270 0.3141 0.030 Uiso 1 1 calc R . . C7 C 0.24031(11) 0.44990(6) 0.49971(9) 0.0241(3) Uani 1 1 d . . . H3 H 0.2135 0.4482 0.5449 0.029 Uiso 1 1 calc R . . C8 C 0.52212(11) 0.59160(6) 0.37085(9) 0.0237(3) Uani 1 1 d . . . H4 H 0.5368 0.6180 0.4159 0.028 Uiso 1 1 calc R . . C9 C 0.42943(10) 0.51003(5) 0.29670(8) 0.0183(3) Uani 1 1 d . . . C10 C 0.19831(11) 0.35555(6) 0.07228(9) 0.0235(3) Uani 1 1 d . . . C11 C 0.70448(10) 0.46124(6) 0.20622(9) 0.0237(3) Uani 1 1 d . . . C12 C 0.30301(10) 0.49391(6) 0.49751(9) 0.0225(3) Uani 1 1 d . . . H5 H 0.3201 0.5211 0.5416 0.027 Uiso 1 1 calc R . . C13 C 0.21414(10) 0.40711(5) 0.43783(8) 0.0206(3) Uani 1 1 d . . . C14 C 0.48311(10) 0.51558(5) 0.23934(8) 0.0207(3) Uani 1 1 d . . . H6 H 0.4697 0.4892 0.1943 0.025 Uiso 1 1 calc R . . C15 C 0.30077(10) 0.42681(5) 0.20764(8) 0.0186(3) Uani 1 1 d . . . C16 C 0.29451(11) 0.34350(6) 0.12130(9) 0.0223(3) Uani 1 1 d . . . H7 H 0.3261 0.3107 0.1089 0.027 Uiso 1 1 calc R . . C17 C 0.06659(11) 0.36048(6) 0.48784(9) 0.0242(3) Uani 1 1 d . . . C18 C 0.65964(10) 0.50641(6) 0.15145(9) 0.0229(3) Uani 1 1 d . . . C19 C 0.55423(10) 0.55702(6) 0.24428(9) 0.0222(3) Uani 1 1 d . . . C20 C 0.34664(10) 0.37800(6) 0.18835(8) 0.0202(3) Uani 1 1 d . . . C21 C 0.47120(11) 0.64565(7) 0.08146(11) 0.0332(4) Uani 1 1 d . . . H56 H 0.4289 0.6775 0.0863 0.050 Uiso 1 1 calc R . . H57 H 0.4566 0.6126 0.1110 0.050 Uiso 1 1 calc R . . H58 H 0.4582 0.6363 0.0220 0.050 Uiso 1 1 calc R . . C22 C -0.07223(12) 0.40843(7) 0.51473(11) 0.0345(4) Uani 1 1 d . . . H8 H -0.1199 0.4382 0.5018 0.041 Uiso 1 1 calc R . . C23 C 0.66077(11) 0.50286(6) 0.06722(9) 0.0256(3) Uani 1 1 d . . . C24 C 0.25023(10) 0.27125(6) 0.41559(9) 0.0230(3) Uani 1 1 d . . . C25 C 0.20338(11) 0.43990(6) 0.15720(9) 0.0222(3) Uani 1 1 d . . . C26 C 0.65045(10) 0.62269(6) 0.16536(9) 0.0226(3) Uani 1 1 d . . . C27 C 0.74979(11) 0.41656(6) 0.17812(9) 0.0276(3) Uani 1 1 d . . . H9 H 0.7816 0.3876 0.2167 0.033 Uiso 1 1 calc R . . C28 C 0.14031(13) 0.27321(7) 0.57729(10) 0.0341(4) Uani 1 1 d . . . H15 H 0.2041 0.2889 0.6117 0.051 Uiso 1 1 calc R . . H16 H 0.1484 0.2549 0.5274 0.051 Uiso 1 1 calc R . . H17 H 0.1172 0.2452 0.6101 0.051 Uiso 1 1 calc R . . C29 C 0.75073(11) 0.64010(6) 0.19623(9) 0.0257(3) Uani 1 1 d . . . C30 C 0.15395(11) 0.40437(6) 0.09026(9) 0.0244(3) Uani 1 1 d . . . H10 H 0.0885 0.4138 0.0563 0.029 Uiso 1 1 calc R . . C31 C 0.06520(11) 0.32036(6) 0.55050(10) 0.0276(3) Uani 1 1 d . . . C32 C 0.70541(11) 0.73444(6) 0.13708(10) 0.0277(3) Uani 1 1 d . . . C33 C 0.42642(13) 0.58752(6) 0.49350(10) 0.0339(4) Uani 1 1 d . . . H29 H 0.3704 0.5899 0.5156 0.051 Uiso 1 1 calc R . . H30 H 0.4357 0.6242 0.4696 0.051 Uiso 1 1 calc R . . H31 H 0.4868 0.5776 0.5391 0.051 Uiso 1 1 calc R . . C34 C 0.70394(12) 0.45651(7) 0.04143(10) 0.0305(3) Uani 1 1 d . . . H18 H 0.7020 0.4544 -0.0156 0.037 Uiso 1 1 calc R . . C35 C 0.26286(11) 0.22329(6) 0.37152(10) 0.0258(3) Uani 1 1 d . . . H11 H 0.3239 0.2032 0.3904 0.031 Uiso 1 1 calc R . . C36 C 0.61468(13) 0.54768(7) 0.00247(10) 0.0347(4) Uani 1 1 d . . . H59 H 0.6254 0.5378 -0.0508 0.052 Uiso 1 1 calc R . . H60 H 0.6454 0.5845 0.0220 0.052 Uiso 1 1 calc R . . H61 H 0.5432 0.5498 -0.0059 0.052 Uiso 1 1 calc R . . C37 C -0.01313(12) 0.44806(7) 0.40184(11) 0.0350(4) Uani 1 1 d . . . H41 H -0.0444 0.4303 0.3470 0.053 Uiso 1 1 calc R . . H42 H 0.0531 0.4618 0.4049 0.053 Uiso 1 1 calc R . . H43 H -0.0539 0.4800 0.4090 0.053 Uiso 1 1 calc R . . B8 B 0.14542(12) 0.35599(7) 0.43936(10) 0.0215(3) Uani 1 1 d . . . C39 C 0.14463(12) 0.31373(6) 0.00377(9) 0.0301(3) Uani 1 1 d . . . H19 H 0.1933 0.3007 -0.0244 0.036 Uiso 1 1 calc R . . C40 C 0.10105(12) 0.23444(6) 0.27464(9) 0.0279(3) Uani 1 1 d . . . H12 H 0.0502 0.2224 0.2256 0.033 Uiso 1 1 calc R . . C41 C -0.00420(11) 0.40502(6) 0.47060(10) 0.0287(3) Uani 1 1 d . . . B11 B 0.34998(11) 0.46449(6) 0.28775(9) 0.0185(3) Uani 1 1 d . . . C43 C 0.51841(12) 0.35074(7) 0.18817(10) 0.0325(4) Uani 1 1 d . . . H32 H 0.4908 0.3204 0.1475 0.049 Uiso 1 1 calc R . . H33 H 0.5845 0.3396 0.2247 0.049 Uiso 1 1 calc R . . H34 H 0.5236 0.3857 0.1582 0.049 Uiso 1 1 calc R . . C44 C 0.57911(11) 0.66205(6) 0.12012(9) 0.0254(3) Uani 1 1 d . . . C45 C -0.00436(12) 0.32582(7) 0.59318(10) 0.0344(4) Uani 1 1 d . . . H20 H -0.0048 0.2985 0.6347 0.041 Uiso 1 1 calc R . . C46 C 0.77568(11) 0.69562(6) 0.18283(9) 0.0280(3) Uani 1 1 d . . . H13 H 0.8429 0.7074 0.2057 0.034 Uiso 1 1 calc R . . C47 C 0.08479(11) 0.28200(6) 0.31767(9) 0.0245(3) Uani 1 1 d . . . C48 C 0.70945(12) 0.45953(7) 0.29765(9) 0.0283(3) Uani 1 1 d . . . H35 H 0.6447 0.4483 0.3017 0.042 Uiso 1 1 calc R . . H36 H 0.7270 0.4972 0.3226 0.042 Uiso 1 1 calc R . . H37 H 0.7599 0.4320 0.3278 0.042 Uiso 1 1 calc R . . C49 C 0.33590(11) 0.28886(6) 0.49110(10) 0.0306(3) Uani 1 1 d . . . H44 H 0.3658 0.2551 0.5234 0.046 Uiso 1 1 calc R . . H45 H 0.3117 0.3142 0.5266 0.046 Uiso 1 1 calc R . . H46 H 0.3858 0.3086 0.4723 0.046 Uiso 1 1 calc R . . C50 C 0.75002(12) 0.41294(6) 0.09571(10) 0.0299(3) Uani 1 1 d . . . C51 C 0.14973(11) 0.49259(6) 0.17386(9) 0.0272(3) Uani 1 1 d . . . H21 H 0.1943 0.5109 0.2259 0.033 Uiso 1 1 calc R . . C52 C 0.20350(13) 0.15063(7) 0.25701(12) 0.0392(4) Uani 1 1 d . . . H47 H 0.2742 0.1407 0.2748 0.059 Uiso 1 1 calc R . . H48 H 0.1798 0.1568 0.1961 0.059 Uiso 1 1 calc R . . H49 H 0.1658 0.1196 0.2714 0.059 Uiso 1 1 calc R . . C53 C 0.60780(11) 0.71667(6) 0.10546(10) 0.0286(3) Uani 1 1 d . . . H14 H 0.5590 0.7423 0.0729 0.034 Uiso 1 1 calc R . . C54 C 0.73462(13) 0.79414(7) 0.12124(12) 0.0397(4) Uani 1 1 d . . . H71 H 0.6768 0.8138 0.0836 0.060 Uiso 1 1 calc R . . H72 H 0.7874 0.7926 0.0952 0.060 Uiso 1 1 calc R . . H73 H 0.7586 0.8147 0.1747 0.060 Uiso 1 1 calc R . . C55 C -0.01171(12) 0.31423(7) 0.28330(11) 0.0335(4) Uani 1 1 d . . . H38 H -0.0013 0.3474 0.2518 0.050 Uiso 1 1 calc R . . H39 H -0.0344 0.3267 0.3299 0.050 Uiso 1 1 calc R . . H40 H -0.0620 0.2895 0.2459 0.050 Uiso 1 1 calc R . . C56 C 0.05617(14) 0.33867(8) -0.06356(11) 0.0432(4) Uani 1 1 d . . . H22 H 0.0049 0.3494 -0.0386 0.065 Uiso 1 1 calc R . . H23 H 0.0292 0.3104 -0.1077 0.065 Uiso 1 1 calc R . . H24 H 0.0772 0.3723 -0.0878 0.065 Uiso 1 1 calc R . . C57 C 0.45050(10) 0.36077(6) 0.24132(9) 0.0233(3) Uani 1 1 d . . . H25 H 0.4792 0.3927 0.2809 0.028 Uiso 1 1 calc R . . C58 C -0.07260(12) 0.36966(8) 0.57710(11) 0.0379(4) Uani 1 1 d . . . C59 C 0.18922(12) 0.20400(6) 0.30111(10) 0.0279(3) Uani 1 1 d . . . C60 C 0.79905(14) 0.36417(7) 0.06617(11) 0.0404(4) Uani 1 1 d . . . H62 H 0.8682 0.3739 0.0729 0.061 Uiso 1 1 calc R . . H63 H 0.7637 0.3565 0.0068 0.061 Uiso 1 1 calc R . . H64 H 0.7971 0.3303 0.0996 0.061 Uiso 1 1 calc R . . B9 B 0.61950(12) 0.56088(7) 0.18461(10) 0.0223(3) Uani 1 1 d . . . C62 C 0.44688(13) 0.30822(8) 0.29425(12) 0.0411(4) Uani 1 1 d . . . H26 H 0.4037 0.3158 0.3285 0.062 Uiso 1 1 calc R . . H27 H 0.5140 0.2993 0.3311 0.062 Uiso 1 1 calc R . . H28 H 0.4207 0.2759 0.2570 0.062 Uiso 1 1 calc R . . C63 C 0.83073(12) 0.59956(7) 0.24410(11) 0.0379(4) Uani 1 1 d . . . H50 H 0.8956 0.6181 0.2572 0.057 Uiso 1 1 calc R . . H51 H 0.8297 0.5658 0.2098 0.057 Uiso 1 1 calc R . . H52 H 0.8189 0.5884 0.2964 0.057 Uiso 1 1 calc R . . C64 C 0.11300(16) 0.26165(8) 0.04337(13) 0.0504(5) Uani 1 1 d . . . H65 H 0.0653 0.2730 0.0717 0.076 Uiso 1 1 calc R . . H66 H 0.1714 0.2447 0.0844 0.076 Uiso 1 1 calc R . . H67 H 0.0821 0.2339 -0.0006 0.076 Uiso 1 1 calc R . . C67 C 0.13192(16) 0.53558(7) 0.10302(12) 0.0459(5) Uani 1 1 d . . . H53 H 0.1957 0.5473 0.0974 0.069 Uiso 1 1 calc R . . H54 H 0.0976 0.5688 0.1157 0.069 Uiso 1 1 calc R . . H55 H 0.0909 0.5183 0.0503 0.069 Uiso 1 1 calc R . . C66 C 0.05299(14) 0.47818(8) 0.19016(14) 0.0477(5) Uani 1 1 d . . . H68 H 0.0237 0.5129 0.2043 0.072 Uiso 1 1 calc R . . H69 H 0.0662 0.4513 0.2370 0.072 Uiso 1 1 calc R . . H70 H 0.0067 0.4610 0.1397 0.072 Uiso 1 1 calc R . . C65 C -0.14486(15) 0.37480(11) 0.62636(14) 0.0596(6) Uani 1 1 d . . . H74 H -0.2032 0.3511 0.6002 0.089 Uiso 1 1 calc R . . H75 H -0.1655 0.4145 0.6266 0.089 Uiso 1 1 calc R . . H76 H -0.1127 0.3621 0.6842 0.089 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 N2 0.0241(6) 0.0175(5) 0.0187(6) -0.0032(4) 0.0081(5) -0.0038(4) C1 0.0191(7) 0.0171(6) 0.0195(7) -0.0005(5) 0.0060(5) 0.0006(5) C2 0.0186(7) 0.0177(6) 0.0183(7) 0.0001(5) 0.0045(5) 0.0003(5) C3 0.0243(7) 0.0200(6) 0.0248(7) 0.0003(5) 0.0124(6) -0.0043(5) C4 0.0210(7) 0.0184(6) 0.0216(7) -0.0022(5) 0.0071(6) -0.0010(5) C5 0.0176(7) 0.0172(6) 0.0199(7) 0.0000(5) 0.0053(5) 0.0009(5) C6 0.0263(8) 0.0216(7) 0.0297(8) -0.0047(6) 0.0114(6) -0.0075(5) C7 0.0283(8) 0.0240(7) 0.0234(7) -0.0018(5) 0.0131(6) -0.0024(6) C8 0.0260(8) 0.0218(6) 0.0252(7) -0.0067(5) 0.0110(6) -0.0047(5) C9 0.0201(7) 0.0168(6) 0.0176(6) -0.0003(5) 0.0054(5) 0.0001(5) C10 0.0252(8) 0.0234(7) 0.0218(7) -0.0041(5) 0.0070(6) -0.0046(5) C11 0.0239(7) 0.0252(7) 0.0231(7) -0.0028(5) 0.0089(6) -0.0046(5) C12 0.0261(7) 0.0214(6) 0.0219(7) -0.0059(5) 0.0103(6) -0.0029(5) C13 0.0210(7) 0.0192(6) 0.0231(7) 0.0000(5) 0.0093(6) -0.0002(5) C14 0.0243(7) 0.0190(6) 0.0186(7) -0.0021(5) 0.0067(6) -0.0011(5) C15 0.0205(7) 0.0186(6) 0.0181(6) -0.0007(5) 0.0082(5) -0.0034(5) C16 0.0253(7) 0.0190(6) 0.0239(7) -0.0036(5) 0.0095(6) -0.0008(5) C17 0.0248(7) 0.0227(7) 0.0280(8) -0.0054(6) 0.0125(6) -0.0056(5) C18 0.0230(7) 0.0247(7) 0.0227(7) -0.0018(5) 0.0095(6) -0.0044(5) C19 0.0237(7) 0.0217(7) 0.0227(7) 0.0001(5) 0.0096(6) -0.0003(5) C20 0.0219(7) 0.0200(6) 0.0201(7) 0.0003(5) 0.0085(6) -0.0026(5) C21 0.0253(8) 0.0325(8) 0.0398(9) 0.0018(7) 0.0073(7) -0.0022(6) C22 0.0265(8) 0.0376(9) 0.0432(10) -0.0111(7) 0.0161(7) -0.0019(6) C23 0.0272(8) 0.0281(7) 0.0240(7) -0.0037(6) 0.0114(6) -0.0068(6) C24 0.0230(7) 0.0214(6) 0.0269(7) 0.0006(5) 0.0113(6) -0.0048(5) C25 0.0233(7) 0.0220(6) 0.0213(7) -0.0012(5) 0.0071(6) -0.0004(5) C26 0.0250(7) 0.0248(7) 0.0215(7) -0.0030(5) 0.0120(6) -0.0034(5) C27 0.0272(8) 0.0269(7) 0.0282(8) -0.0012(6) 0.0079(6) -0.0004(6) C28 0.0407(10) 0.0328(8) 0.0343(9) 0.0058(7) 0.0200(8) -0.0008(7) C29 0.0259(8) 0.0273(7) 0.0244(7) -0.0011(6) 0.0087(6) -0.0037(6) C30 0.0203(7) 0.0272(7) 0.0220(7) -0.0029(6) 0.0015(6) -0.0006(5) C31 0.0281(8) 0.0289(7) 0.0295(8) -0.0058(6) 0.0142(7) -0.0080(6) C32 0.0310(8) 0.0233(7) 0.0313(8) -0.0025(6) 0.0134(7) -0.0038(6) C33 0.0487(10) 0.0300(8) 0.0307(8) -0.0145(6) 0.0234(8) -0.0171(7) C34 0.0342(9) 0.0361(8) 0.0245(8) -0.0064(6) 0.0142(7) -0.0054(7) C35 0.0242(7) 0.0227(7) 0.0351(8) 0.0002(6) 0.0160(6) -0.0003(5) C36 0.0468(10) 0.0369(9) 0.0216(8) 0.0010(6) 0.0124(7) 0.0003(7) C37 0.0300(9) 0.0287(8) 0.0489(10) -0.0001(7) 0.0159(8) 0.0024(6) B8 0.0201(8) 0.0223(7) 0.0224(8) 0.0013(6) 0.0072(6) -0.0002(6) C39 0.0296(8) 0.0307(8) 0.0267(8) -0.0107(6) 0.0042(7) -0.0023(6) C40 0.0312(8) 0.0283(7) 0.0246(7) -0.0041(6) 0.0095(6) -0.0065(6) C41 0.0260(8) 0.0260(7) 0.0361(8) -0.0072(6) 0.0126(7) -0.0040(6) B11 0.0193(7) 0.0162(7) 0.0199(7) 0.0001(5) 0.0061(6) 0.0012(5) C43 0.0256(8) 0.0375(9) 0.0356(9) -0.0026(7) 0.0112(7) 0.0028(6) C44 0.0245(8) 0.0261(7) 0.0272(8) -0.0026(6) 0.0106(6) -0.0032(6) C45 0.0340(9) 0.0426(9) 0.0319(9) -0.0035(7) 0.0178(7) -0.0093(7) C46 0.0249(8) 0.0295(8) 0.0292(8) -0.0026(6) 0.0080(6) -0.0067(6) C47 0.0258(8) 0.0234(7) 0.0257(7) 0.0016(5) 0.0104(6) -0.0044(5) C48 0.0301(8) 0.0321(8) 0.0230(7) 0.0030(6) 0.0088(6) 0.0020(6) C49 0.0248(8) 0.0287(8) 0.0366(9) -0.0029(6) 0.0075(7) -0.0019(6) C50 0.0283(8) 0.0312(8) 0.0319(8) -0.0099(6) 0.0119(7) -0.0030(6) C51 0.0260(8) 0.0265(7) 0.0263(8) -0.0050(6) 0.0044(6) 0.0041(6) C52 0.0425(10) 0.0337(9) 0.0475(10) -0.0124(7) 0.0228(8) -0.0021(7) C53 0.0296(8) 0.0241(7) 0.0326(8) -0.0006(6) 0.0107(7) 0.0009(6) C54 0.0396(10) 0.0256(8) 0.0549(11) 0.0004(7) 0.0162(8) -0.0075(7) C55 0.0311(9) 0.0311(8) 0.0347(9) -0.0011(7) 0.0055(7) 0.0003(6) C56 0.0388(10) 0.0445(10) 0.0353(10) -0.0161(8) -0.0040(8) 0.0008(8) C57 0.0224(7) 0.0222(7) 0.0245(7) -0.0011(5) 0.0060(6) 0.0006(5) C58 0.0287(9) 0.0530(10) 0.0370(9) -0.0116(8) 0.0175(7) -0.0067(7) C59 0.0336(8) 0.0239(7) 0.0318(8) -0.0033(6) 0.0183(7) -0.0046(6) C60 0.0445(10) 0.0393(9) 0.0393(10) -0.0115(7) 0.0159(8) 0.0044(8) B9 0.0224(8) 0.0255(8) 0.0178(7) -0.0005(6) 0.0046(6) -0.0044(6) C62 0.0352(9) 0.0429(10) 0.0425(10) 0.0186(8) 0.0082(8) 0.0059(7) C63 0.0268(8) 0.0321(8) 0.0478(10) 0.0053(7) 0.0017(7) -0.0045(7) C64 0.0573(12) 0.0360(9) 0.0496(11) -0.0095(8) 0.0050(10) -0.0201(9) C67 0.0615(13) 0.0310(9) 0.0487(11) 0.0067(8) 0.0226(10) 0.0141(8) C66 0.0438(11) 0.0403(10) 0.0689(13) -0.0045(9) 0.0319(10) 0.0072(8) C65 0.0429(12) 0.0916(17) 0.0566(13) -0.0035(12) 0.0335(10) 0.0039(11) _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 N2 C5 1.3967(16) . ? N2 C2 1.3988(17) . ? N2 C33 1.4693(17) . ? C1 C4 1.4078(18) . ? C1 C5 1.4158(18) . ? C1 B11 1.5324(19) . ? C2 C8 1.4077(18) . ? C2 C9 1.4225(18) . ? C3 C47 1.409(2) . ? C3 C24 1.411(2) . ? C3 B8 1.582(2) . ? C4 C13 1.3919(18) . ? C4 H1 0.9500 . ? C5 C12 1.4094(18) . ? C6 C8 1.3771(19) . ? C6 C19 1.4100(19) . ? C6 H2 0.9500 . ? C7 C12 1.3750(19) . ? C7 C13 1.4103(19) . ? C7 H3 0.9500 . ? C8 H4 0.9500 . ? C9 C14 1.4096(18) . ? C9 B11 1.5294(19) . ? C10 C16 1.383(2) . ? C10 C30 1.3897(19) . ? C10 C39 1.5228(19) . ? C11 C27 1.391(2) . ? C11 C18 1.419(2) . ? C11 C48 1.513(2) . ? C12 H5 0.9500 . ? C13 B8 1.555(2) . ? C14 C19 1.3881(19) . ? C14 H6 0.9500 . ? C15 C25 1.408(2) . ? C15 C20 1.4089(18) . ? C15 B11 1.578(2) . ? C16 C20 1.3957(19) . ? C16 H7 0.9500 . ? C17 C31 1.418(2) . ? C17 C41 1.418(2) . ? C17 B8 1.581(2) . ? C18 C23 1.4205(19) . ? C18 B9 1.576(2) . ? C19 B9 1.567(2) . ? C20 C57 1.517(2) . ? C21 C44 1.513(2) . ? C21 H56 0.9800 . ? C21 H57 0.9800 . ? C21 H58 0.9800 . ? C22 C58 1.390(2) . ? C22 C41 1.392(2) . ? C22 H8 0.9500 . ? C23 C34 1.387(2) . ? C23 C36 1.508(2) . ? C24 C35 1.3929(19) . ? C24 C49 1.511(2) . ? C25 C30 1.3989(19) . ? C25 C51 1.5278(19) . ? C26 C44 1.406(2) . ? C26 C29 1.413(2) . ? C26 B9 1.584(2) . ? C27 C50 1.386(2) . ? C27 H9 0.9500 . ? C28 C31 1.507(2) . ? C28 H15 0.9800 . ? C28 H16 0.9800 . ? C28 H17 0.9800 . ? C29 C46 1.392(2) . ? C29 C63 1.507(2) . ? C30 H10 0.9500 . ? C31 C45 1.397(2) . ? C32 C53 1.383(2) . ? C32 C46 1.392(2) . ? C32 C54 1.514(2) . ? C33 H29 0.9800 . ? C33 H30 0.9800 . ? C33 H31 0.9800 . ? C34 C50 1.391(2) . ? C34 H18 0.9500 . ? C35 C59 1.384(2) . ? C35 H11 0.9500 . ? C36 H59 0.9800 . ? C36 H60 0.9800 . ? C36 H61 0.9800 . ? C37 C41 1.511(2) . ? C37 H41 0.9800 . ? C37 H42 0.9800 . ? C37 H43 0.9800 . ? C39 C56 1.517(2) . ? C39 C64 1.529(2) . ? C39 H19 1.0000 . ? C40 C59 1.388(2) . ? C40 C47 1.391(2) . ? C40 H12 0.9500 . ? C43 C57 1.524(2) . ? C43 H32 0.9800 . ? C43 H33 0.9800 . ? C43 H34 0.9800 . ? C44 C53 1.395(2) . ? C45 C58 1.383(2) . ? C45 H20 0.9500 . ? C46 H13 0.9500 . ? C47 C55 1.512(2) . ? C48 H35 0.9800 . ? C48 H36 0.9800 . ? C48 H37 0.9800 . ? C49 H44 0.9800 . ? C49 H45 0.9800 . ? C49 H46 0.9800 . ? C50 C60 1.506(2) . ? C51 C67 1.521(2) . ? C51 C66 1.521(2) . ? C51 H21 1.0000 . ? C52 C59 1.505(2) . ? C52 H47 0.9800 . ? C52 H48 0.9800 . ? C52 H49 0.9800 . ? C53 H14 0.9500 . ? C54 H71 0.9800 . ? C54 H72 0.9800 . ? C54 H73 0.9800 . ? C55 H38 0.9800 . ? C55 H39 0.9800 . ? C55 H40 0.9800 . ? C56 H22 0.9800 . ? C56 H23 0.9800 . ? C56 H24 0.9800 . ? C57 C62 1.534(2) . ? C57 H25 1.0000 . ? C58 C65 1.512(2) . ? C60 H62 0.9800 . ? C60 H63 0.9800 . ? C60 H64 0.9800 . ? C62 H26 0.9800 . ? C62 H27 0.9800 . ? C62 H28 0.9800 . ? C63 H50 0.9800 . ? C63 H51 0.9800 . ? C63 H52 0.9800 . ? C64 H65 0.9800 . ? C64 H66 0.9800 . ? C64 H67 0.9800 . ? C67 H53 0.9800 . ? C67 H54 0.9800 . ? C67 H55 0.9800 . ? C66 H68 0.9800 . ? C66 H69 0.9800 . ? C66 H70 0.9800 . ? C65 H74 0.9800 . ? C65 H75 0.9800 . ? C65 H76 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 N2 C2 122.76(11) . . ? C5 N2 C33 118.76(11) . . ? C2 N2 C33 118.48(11) . . ? C4 C1 C5 118.06(12) . . ? C4 C1 B11 121.11(12) . . ? C5 C1 B11 120.82(11) . . ? N2 C2 C8 119.85(12) . . ? N2 C2 C9 121.24(11) . . ? C8 C2 C9 118.89(12) . . ? C47 C3 C24 117.95(13) . . ? C47 C3 B8 121.84(13) . . ? C24 C3 B8 120.12(12) . . ? C13 C4 C1 124.20(12) . . ? C13 C4 H1 117.9 . . ? C1 C4 H1 117.9 . . ? N2 C5 C12 120.96(11) . . ? N2 C5 C1 120.33(11) . . ? C12 C5 C1 118.71(12) . . ? C8 C6 C19 122.84(13) . . ? C8 C6 H2 118.6 . . ? C19 C6 H2 118.6 . . ? C12 C7 C13 122.81(12) . . ? C12 C7 H3 118.6 . . ? C13 C7 H3 118.6 . . ? C6 C8 C2 120.46(12) . . ? C6 C8 H4 119.8 . . ? C2 C8 H4 119.8 . . ? C14 C9 C2 117.66(12) . . ? C14 C9 B11 122.61(12) . . ? C2 C9 B11 119.71(11) . . ? C16 C10 C30 118.10(13) . . ? C16 C10 C39 118.72(13) . . ? C30 C10 C39 123.13(13) . . ? C27 C11 C18 120.62(13) . . ? C27 C11 C48 116.40(13) . . ? C18 C11 C48 122.95(12) . . ? C7 C12 C5 120.66(12) . . ? C7 C12 H5 119.7 . . ? C5 C12 H5 119.7 . . ? C4 C13 C7 115.46(12) . . ? C4 C13 B8 120.32(12) . . ? C7 C13 B8 124.22(12) . . ? C19 C14 C9 124.35(12) . . ? C19 C14 H6 117.8 . . ? C9 C14 H6 117.8 . . ? C25 C15 C20 118.56(12) . . ? C25 C15 B11 118.35(11) . . ? C20 C15 B11 122.87(12) . . ? C10 C16 C20 122.15(13) . . ? C10 C16 H7 118.9 . . ? C20 C16 H7 118.9 . . ? C31 C17 C41 118.01(13) . . ? C31 C17 B8 120.96(13) . . ? C41 C17 B8 121.03(13) . . ? C11 C18 C23 117.13(13) . . ? C11 C18 B9 121.41(12) . . ? C23 C18 B9 121.21(13) . . ? C14 C19 C6 115.54(12) . . ? C14 C19 B9 124.64(12) . . ? C6 C19 B9 119.76(12) . . ? C16 C20 C15 119.67(13) . . ? C16 C20 C57 119.07(12) . . ? C15 C20 C57 121.22(12) . . ? C44 C21 H56 109.5 . . ? C44 C21 H57 109.5 . . ? H56 C21 H57 109.5 . . ? C44 C21 H58 109.5 . . ? H56 C21 H58 109.5 . . ? H57 C21 H58 109.5 . . ? C58 C22 C41 122.02(15) . . ? C58 C22 H8 119.0 . . ? C41 C22 H8 119.0 . . ? C34 C23 C18 120.10(14) . . ? C34 C23 C36 117.45(13) . . ? C18 C23 C36 122.44(13) . . ? C35 C24 C3 120.09(13) . . ? C35 C24 C49 117.60(13) . . ? C3 C24 C49 122.30(13) . . ? C30 C25 C15 119.95(12) . . ? C30 C25 C51 118.74(13) . . ? C15 C25 C51 121.30(12) . . ? C44 C26 C29 118.46(13) . . ? C44 C26 B9 121.20(12) . . ? C29 C26 B9 120.30(13) . . ? C50 C27 C11 122.10(14) . . ? C50 C27 H9 119.0 . . ? C11 C27 H9 119.0 . . ? C31 C28 H15 109.5 . . ? C31 C28 H16 109.5 . . ? H15 C28 H16 109.5 . . ? C31 C28 H17 109.5 . . ? H15 C28 H17 109.5 . . ? H16 C28 H17 109.5 . . ? C46 C29 C26 119.46(14) . . ? C46 C29 C63 119.64(13) . . ? C26 C29 C63 120.89(13) . . ? C10 C30 C25 121.55(13) . . ? C10 C30 H10 119.2 . . ? C25 C30 H10 119.2 . . ? C45 C31 C17 119.74(14) . . ? C45 C31 C28 117.59(14) . . ? C17 C31 C28 122.57(13) . . ? C53 C32 C46 117.98(13) . . ? C53 C32 C54 120.72(14) . . ? C46 C32 C54 121.29(14) . . ? N2 C33 H29 109.5 . . ? N2 C33 H30 109.5 . . ? H29 C33 H30 109.5 . . ? N2 C33 H31 109.5 . . ? H29 C33 H31 109.5 . . ? H30 C33 H31 109.5 . . ? C23 C34 C50 122.68(14) . . ? C23 C34 H18 118.7 . . ? C50 C34 H18 118.7 . . ? C59 C35 C24 122.04(14) . . ? C59 C35 H11 119.0 . . ? C24 C35 H11 119.0 . . ? C23 C36 H59 109.5 . . ? C23 C36 H60 109.5 . . ? H59 C36 H60 109.5 . . ? C23 C36 H61 109.5 . . ? H59 C36 H61 109.5 . . ? H60 C36 H61 109.5 . . ? C41 C37 H41 109.5 . . ? C41 C37 H42 109.5 . . ? H41 C37 H42 109.5 . . ? C41 C37 H43 109.5 . . ? H41 C37 H43 109.5 . . ? H42 C37 H43 109.5 . . ? C13 B8 C17 120.41(12) . . ? C13 B8 C3 116.31(11) . . ? C17 B8 C3 123.28(12) . . ? C56 C39 C10 114.22(13) . . ? C56 C39 C64 110.30(14) . . ? C10 C39 C64 109.72(13) . . ? C56 C39 H19 107.4 . . ? C10 C39 H19 107.4 . . ? C64 C39 H19 107.4 . . ? C59 C40 C47 122.08(14) . . ? C59 C40 H12 119.0 . . ? C47 C40 H12 119.0 . . ? C22 C41 C17 120.00(14) . . ? C22 C41 C37 117.52(14) . . ? C17 C41 C37 122.40(13) . . ? C9 B11 C1 113.99(12) . . ? C9 B11 C15 126.36(12) . . ? C1 B11 C15 119.61(11) . . ? C57 C43 H32 109.5 . . ? C57 C43 H33 109.5 . . ? H32 C43 H33 109.5 . . ? C57 C43 H34 109.5 . . ? H32 C43 H34 109.5 . . ? H33 C43 H34 109.5 . . ? C53 C44 C26 120.23(13) . . ? C53 C44 C21 118.19(14) . . ? C26 C44 C21 121.47(13) . . ? C58 C45 C31 122.25(15) . . ? C58 C45 H20 118.9 . . ? C31 C45 H20 118.9 . . ? C32 C46 C29 122.16(14) . . ? C32 C46 H13 118.9 . . ? C29 C46 H13 118.9 . . ? C40 C47 C3 120.09(14) . . ? C40 C47 C55 119.06(13) . . ? C3 C47 C55 120.79(13) . . ? C11 C48 H35 109.5 . . ? C11 C48 H36 109.5 . . ? H35 C48 H36 109.5 . . ? C11 C48 H37 109.5 . . ? H35 C48 H37 109.5 . . ? H36 C48 H37 109.5 . . ? C24 C49 H44 109.5 . . ? C24 C49 H45 109.5 . . ? H44 C49 H45 109.5 . . ? C24 C49 H46 109.5 . . ? H44 C49 H46 109.5 . . ? H45 C49 H46 109.5 . . ? C27 C50 C34 117.30(13) . . ? C27 C50 C60 121.46(15) . . ? C34 C50 C60 121.23(14) . . ? C67 C51 C66 110.64(14) . . ? C67 C51 C25 111.59(13) . . ? C66 C51 C25 112.45(13) . . ? C67 C51 H21 107.3 . . ? C66 C51 H21 107.3 . . ? C25 C51 H21 107.3 . . ? C59 C52 H47 109.5 . . ? C59 C52 H48 109.5 . . ? H47 C52 H48 109.5 . . ? C59 C52 H49 109.5 . . ? H47 C52 H49 109.5 . . ? H48 C52 H49 109.5 . . ? C32 C53 C44 121.64(14) . . ? C32 C53 H14 119.2 . . ? C44 C53 H14 119.2 . . ? C32 C54 H71 109.5 . . ? C32 C54 H72 109.5 . . ? H71 C54 H72 109.5 . . ? C32 C54 H73 109.5 . . ? H71 C54 H73 109.5 . . ? H72 C54 H73 109.5 . . ? C47 C55 H38 109.5 . . ? C47 C55 H39 109.5 . . ? H38 C55 H39 109.5 . . ? C47 C55 H40 109.5 . . ? H38 C55 H40 109.5 . . ? H39 C55 H40 109.5 . . ? C39 C56 H22 109.5 . . ? C39 C56 H23 109.5 . . ? H22 C56 H23 109.5 . . ? C39 C56 H24 109.5 . . ? H22 C56 H24 109.5 . . ? H23 C56 H24 109.5 . . ? C20 C57 C43 112.11(12) . . ? C20 C57 C62 110.56(12) . . ? C43 C57 C62 110.87(13) . . ? C20 C57 H25 107.7 . . ? C43 C57 H25 107.7 . . ? C62 C57 H25 107.7 . . ? C45 C58 C22 117.95(14) . . ? C45 C58 C65 120.50(17) . . ? C22 C58 C65 121.55(17) . . ? C35 C59 C40 117.70(13) . . ? C35 C59 C52 120.76(14) . . ? C40 C59 C52 121.50(14) . . ? C50 C60 H62 109.5 . . ? C50 C60 H63 109.5 . . ? H62 C60 H63 109.5 . . ? C50 C60 H64 109.5 . . ? H62 C60 H64 109.5 . . ? H63 C60 H64 109.5 . . ? C19 B9 C18 122.07(12) . . ? C19 B9 C26 116.22(12) . . ? C18 B9 C26 121.52(12) . . ? C57 C62 H26 109.5 . . ? C57 C62 H27 109.5 . . ? H26 C62 H27 109.5 . . ? C57 C62 H28 109.5 . . ? H26 C62 H28 109.5 . . ? H27 C62 H28 109.5 . . ? C29 C63 H50 109.5 . . ? C29 C63 H51 109.5 . . ? H50 C63 H51 109.5 . . ? C29 C63 H52 109.5 . . ? H50 C63 H52 109.5 . . ? H51 C63 H52 109.5 . . ? C39 C64 H65 109.5 . . ? C39 C64 H66 109.5 . . ? H65 C64 H66 109.5 . . ? C39 C64 H67 109.5 . . ? H65 C64 H67 109.5 . . ? H66 C64 H67 109.5 . . ? C51 C67 H53 109.5 . . ? C51 C67 H54 109.5 . . ? H53 C67 H54 109.5 . . ? C51 C67 H55 109.5 . . ? H53 C67 H55 109.5 . . ? H54 C67 H55 109.5 . . ? C51 C66 H68 109.5 . . ? C51 C66 H69 109.5 . . ? H68 C66 H69 109.5 . . ? C51 C66 H70 109.5 . . ? H68 C66 H70 109.5 . . ? H69 C66 H70 109.5 . . ? C58 C65 H74 109.5 . . ? C58 C65 H75 109.5 . . ? H74 C65 H75 109.5 . . ? C58 C65 H76 109.5 . . ? H74 C65 H76 109.5 . . ? H75 C65 H76 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N2 C2 C8 -174.89(12) . . . . ? C33 N2 C2 C8 4.13(19) . . . . ? C5 N2 C2 C9 6.52(19) . . . . ? C33 N2 C2 C9 -174.47(13) . . . . ? C5 C1 C4 C13 2.9(2) . . . . ? B11 C1 C4 C13 -175.85(13) . . . . ? C2 N2 C5 C12 174.94(12) . . . . ? C33 N2 C5 C12 -4.1(2) . . . . ? C2 N2 C5 C1 -5.63(19) . . . . ? C33 N2 C5 C1 175.36(13) . . . . ? C4 C1 C5 N2 177.71(12) . . . . ? B11 C1 C5 N2 -3.58(19) . . . . ? C4 C1 C5 C12 -2.86(19) . . . . ? B11 C1 C5 C12 175.85(12) . . . . ? C19 C6 C8 C2 -3.0(2) . . . . ? N2 C2 C8 C6 179.56(13) . . . . ? C9 C2 C8 C6 -1.8(2) . . . . ? N2 C2 C9 C14 -177.00(12) . . . . ? C8 C2 C9 C14 4.39(19) . . . . ? N2 C2 C9 B11 1.89(19) . . . . ? C8 C2 C9 B11 -176.72(12) . . . . ? C13 C7 C12 C5 2.0(2) . . . . ? N2 C5 C12 C7 -179.98(13) . . . . ? C1 C5 C12 C7 0.6(2) . . . . ? C1 C4 C13 C7 -0.4(2) . . . . ? C1 C4 C13 B8 179.01(13) . . . . ? C12 C7 C13 C4 -2.0(2) . . . . ? C12 C7 C13 B8 178.55(14) . . . . ? C2 C9 C14 C19 -2.5(2) . . . . ? B11 C9 C14 C19 178.61(13) . . . . ? C30 C10 C16 C20 1.3(2) . . . . ? C39 C10 C16 C20 -176.29(13) . . . . ? C27 C11 C18 C23 1.8(2) . . . . ? C48 C11 C18 C23 179.55(13) . . . . ? C27 C11 C18 B9 -172.49(13) . . . . ? C48 C11 C18 B9 5.2(2) . . . . ? C9 C14 C19 C6 -1.9(2) . . . . ? C9 C14 C19 B9 175.46(13) . . . . ? C8 C6 C19 C14 4.8(2) . . . . ? C8 C6 C19 B9 -172.77(14) . . . . ? C10 C16 C20 C15 0.1(2) . . . . ? C10 C16 C20 C57 177.66(13) . . . . ? C25 C15 C20 C16 -1.12(19) . . . . ? B11 C15 C20 C16 173.43(12) . . . . ? C25 C15 C20 C57 -178.61(12) . . . . ? B11 C15 C20 C57 -4.06(19) . . . . ? C11 C18 C23 C34 0.3(2) . . . . ? B9 C18 C23 C34 174.67(13) . . . . ? C11 C18 C23 C36 179.29(14) . . . . ? B9 C18 C23 C36 -6.4(2) . . . . ? C47 C3 C24 C35 -2.48(19) . . . . ? B8 C3 C24 C35 -179.17(12) . . . . ? C47 C3 C24 C49 178.57(13) . . . . ? B8 C3 C24 C49 1.88(19) . . . . ? C20 C15 C25 C30 0.74(19) . . . . ? B11 C15 C25 C30 -174.06(12) . . . . ? C20 C15 C25 C51 -179.19(12) . . . . ? B11 C15 C25 C51 6.01(19) . . . . ? C18 C11 C27 C50 -2.5(2) . . . . ? C48 C11 C27 C50 179.64(14) . . . . ? C44 C26 C29 C46 1.5(2) . . . . ? B9 C26 C29 C46 -176.29(13) . . . . ? C44 C26 C29 C63 -179.13(14) . . . . ? B9 C26 C29 C63 3.1(2) . . . . ? C16 C10 C30 C25 -1.6(2) . . . . ? C39 C10 C30 C25 175.79(13) . . . . ? C15 C25 C30 C10 0.7(2) . . . . ? C51 C25 C30 C10 -179.41(13) . . . . ? C41 C17 C31 C45 -0.3(2) . . . . ? B8 C17 C31 C45 179.09(14) . . . . ? C41 C17 C31 C28 -176.60(14) . . . . ? B8 C17 C31 C28 2.8(2) . . . . ? C18 C23 C34 C50 -2.0(2) . . . . ? C36 C23 C34 C50 179.00(15) . . . . ? C3 C24 C35 C59 1.6(2) . . . . ? C49 C24 C35 C59 -179.42(13) . . . . ? C4 C13 B8 C17 -154.44(13) . . . . ? C7 C13 B8 C17 25.0(2) . . . . ? C4 C13 B8 C3 25.30(19) . . . . ? C7 C13 B8 C3 -155.30(13) . . . . ? C31 C17 B8 C13 -124.95(15) . . . . ? C41 C17 B8 C13 54.4(2) . . . . ? C31 C17 B8 C3 55.3(2) . . . . ? C41 C17 B8 C3 -125.29(15) . . . . ? C47 C3 B8 C13 -113.42(15) . . . . ? C24 C3 B8 C13 63.13(17) . . . . ? C47 C3 B8 C17 66.31(19) . . . . ? C24 C3 B8 C17 -117.14(15) . . . . ? C16 C10 C39 C56 -160.68(14) . . . . ? C30 C10 C39 C56 21.9(2) . . . . ? C16 C10 C39 C64 74.90(18) . . . . ? C30 C10 C39 C64 -102.51(17) . . . . ? C58 C22 C41 C17 1.0(2) . . . . ? C58 C22 C41 C37 177.68(15) . . . . ? C31 C17 C41 C22 0.1(2) . . . . ? B8 C17 C41 C22 -179.33(14) . . . . ? C31 C17 C41 C37 -176.45(14) . . . . ? B8 C17 C41 C37 4.2(2) . . . . ? C14 C9 B11 C1 168.90(12) . . . . ? C2 C9 B11 C1 -9.93(18) . . . . ? C14 C9 B11 C15 -13.6(2) . . . . ? C2 C9 B11 C15 167.59(12) . . . . ? C4 C1 B11 C9 -170.47(12) . . . . ? C5 C1 B11 C9 10.85(18) . . . . ? C4 C1 B11 C15 11.82(19) . . . . ? C5 C1 B11 C15 -166.85(12) . . . . ? C25 C15 B11 C9 -104.47(16) . . . . ? C20 C15 B11 C9 80.97(18) . . . . ? C25 C15 B11 C1 72.93(16) . . . . ? C20 C15 B11 C1 -101.64(15) . . . . ? C29 C26 C44 C53 0.9(2) . . . . ? B9 C26 C44 C53 178.60(13) . . . . ? C29 C26 C44 C21 176.91(13) . . . . ? B9 C26 C44 C21 -5.4(2) . . . . ? C17 C31 C45 C58 -0.5(2) . . . . ? C28 C31 C45 C58 175.97(15) . . . . ? C53 C32 C46 C29 0.9(2) . . . . ? C54 C32 C46 C29 -178.30(15) . . . . ? C26 C29 C46 C32 -2.4(2) . . . . ? C63 C29 C46 C32 178.16(14) . . . . ? C59 C40 C47 C3 0.6(2) . . . . ? C59 C40 C47 C55 177.83(14) . . . . ? C24 C3 C47 C40 1.41(19) . . . . ? B8 C3 C47 C40 178.04(12) . . . . ? C24 C3 C47 C55 -175.74(13) . . . . ? B8 C3 C47 C55 0.9(2) . . . . ? C11 C27 C50 C34 0.9(2) . . . . ? C11 C27 C50 C60 -179.74(14) . . . . ? C23 C34 C50 C27 1.4(2) . . . . ? C23 C34 C50 C60 -178.00(15) . . . . ? C30 C25 C51 C67 -66.68(18) . . . . ? C15 C25 C51 C67 113.24(16) . . . . ? C30 C25 C51 C66 58.33(18) . . . . ? C15 C25 C51 C66 -121.74(16) . . . . ? C46 C32 C53 C44 1.5(2) . . . . ? C54 C32 C53 C44 -179.27(15) . . . . ? C26 C44 C53 C32 -2.4(2) . . . . ? C21 C44 C53 C32 -178.57(14) . . . . ? C16 C20 C57 C43 54.33(17) . . . . ? C15 C20 C57 C43 -128.16(13) . . . . ? C16 C20 C57 C62 -69.93(17) . . . . ? C15 C20 C57 C62 107.58(15) . . . . ? C31 C45 C58 C22 1.5(2) . . . . ? C31 C45 C58 C65 -178.41(17) . . . . ? C41 C22 C58 C45 -1.8(2) . . . . ? C41 C22 C58 C65 178.17(17) . . . . ? C24 C35 C59 C40 0.5(2) . . . . ? C24 C35 C59 C52 -177.40(13) . . . . ? C47 C40 C59 C35 -1.6(2) . . . . ? C47 C40 C59 C52 176.27(14) . . . . ? C14 C19 B9 C18 -36.7(2) . . . . ? C6 C19 B9 C18 140.58(14) . . . . ? C14 C19 B9 C26 148.16(14) . . . . ? C6 C19 B9 C26 -34.54(19) . . . . ? C11 C18 B9 C19 -46.4(2) . . . . ? C23 C18 B9 C19 139.57(14) . . . . ? C11 C18 B9 C26 128.52(14) . . . . ? C23 C18 B9 C26 -45.6(2) . . . . ? C44 C26 B9 C19 -65.67(18) . . . . ? C29 C26 B9 C19 112.02(15) . . . . ? C44 C26 B9 C18 119.17(15) . . . . ? C29 C26 B9 C18 -63.13(18) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.381 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.046