Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'F. Gabbai' 'Ching-Wen Chiu.' _publ_contact_author_name 'F. Gabbai' _publ_contact_author_address ; Department of Chemistry Texas A&M University College Station Texas 77843-3255 UNITED STATES OF AMERICA ; _publ_contact_author_email FRANCOIS@TAMU.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Cyanide ion complexation by a cationic borane ; data_cc1 _database_code_depnum_ccdc_archive 'CCDC 663259' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 1-{Mes2B}-8-{CH2NMe2}-C10H6 _chemical_formula_sum 'C31 H36 B N' _chemical_formula_weight 433.42 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8202(13) _cell_length_b 10.2595(8) _cell_length_c 17.3207(14) _cell_angle_alpha 90.00 _cell_angle_beta 116.6200(10) _cell_angle_gamma 90.00 _cell_volume 2513.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9734 _exptl_absorpt_correction_T_max 0.9898 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12734 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.28 _reflns_number_total 4544 _reflns_number_gt 3319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.8000P] 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 4544 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1315 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 B B 0.30835(19) 0.3577(3) 0.18956(17) 0.0296(6) Uani 1 1 d . . . N N 0.12407(17) 0.7072(2) 0.10352(14) 0.0464(6) Uani 1 1 d . . . C1 C 0.32154(16) 0.4131(2) 0.11120(14) 0.0305(5) Uani 1 1 d . . . C2 C 0.40367(17) 0.3676(2) 0.11061(15) 0.0335(5) Uani 1 1 d . . . H2A H 0.4528 0.3363 0.1632 0.040 Uiso 1 1 calc R . . C3 C 0.41816(18) 0.3653(3) 0.03627(16) 0.0385(6) Uani 1 1 d . . . H3A H 0.4755 0.3324 0.0389 0.046 Uiso 1 1 calc R . . C4 C 0.34880(18) 0.4108(2) -0.03970(16) 0.0381(6) Uani 1 1 d . . . H4A H 0.3563 0.4043 -0.0910 0.046 Uiso 1 1 calc R . . C5 C 0.19562(18) 0.5163(3) -0.12250(16) 0.0399(6) Uani 1 1 d . . . H5A H 0.2044 0.5095 -0.1731 0.048 Uiso 1 1 calc R . . C6 C 0.11563(19) 0.5727(3) -0.12681(16) 0.0434(6) Uani 1 1 d . . . H6A H 0.0680 0.6030 -0.1806 0.052 Uiso 1 1 calc R . . C7 C 0.10397(18) 0.5860(3) -0.05143(16) 0.0393(6) Uani 1 1 d . . . H7A H 0.0485 0.6271 -0.0550 0.047 Uiso 1 1 calc R . . C8 C 0.17058(17) 0.5412(2) 0.02758(15) 0.0324(5) Uani 1 1 d . . . C9 C 0.25194(16) 0.4738(2) 0.03284(15) 0.0310(5) Uani 1 1 d . . . C10 C 0.26563(17) 0.4677(2) -0.04306(15) 0.0346(5) Uani 1 1 d . . . C11 C 0.21456(16) 0.2873(2) 0.17716(14) 0.0290(5) Uani 1 1 d . . . C12 C 0.18000(16) 0.2998(2) 0.23977(14) 0.0293(5) Uani 1 1 d . . . C13 C 0.09863(16) 0.2351(2) 0.22946(15) 0.0333(5) Uani 1 1 d . . . H13A H 0.0765 0.2463 0.2718 0.040 Uiso 1 1 calc R . . C14 C 0.04841(16) 0.1544(2) 0.15912(16) 0.0345(6) Uani 1 1 d . . . C15 C 0.08265(16) 0.1407(2) 0.09880(15) 0.0340(5) Uani 1 1 d . . . H15A H 0.0494 0.0856 0.0505 0.041 Uiso 1 1 calc R . . C16 C 0.16330(16) 0.2036(2) 0.10557(15) 0.0322(5) Uani 1 1 d . . . C17 C 0.22733(17) 0.3862(2) 0.31872(15) 0.0353(6) Uani 1 1 d . . . H17A H 0.1925 0.3810 0.3533 0.053 Uiso 1 1 calc R . . H17B H 0.2276 0.4765 0.3004 0.053 Uiso 1 1 calc R . . H17C H 0.2925 0.3568 0.3535 0.053 Uiso 1 1 calc R . . C18 C -0.04084(18) 0.0869(3) 0.14822(18) 0.0445(6) Uani 1 1 d . . . H18A H -0.0661 0.0348 0.0952 0.067 Uiso 1 1 calc R . . H18B H -0.0877 0.1522 0.1445 0.067 Uiso 1 1 calc R . . H18C H -0.0268 0.0298 0.1978 0.067 Uiso 1 1 calc R . . C19 C 0.19354(19) 0.1734(3) 0.03622(16) 0.0408(6) Uani 1 1 d . . . H19A H 0.1476 0.1142 -0.0064 0.061 Uiso 1 1 calc R . . H19B H 0.2560 0.1319 0.0624 0.061 Uiso 1 1 calc R . . H19C H 0.1967 0.2544 0.0076 0.061 Uiso 1 1 calc R . . C21 C 0.40031(16) 0.3512(2) 0.27960(14) 0.0302(5) Uani 1 1 d . . . C22 C 0.44575(17) 0.4647(2) 0.32480(15) 0.0333(5) Uani 1 1 d . . . C23 C 0.52756(17) 0.4543(3) 0.40354(15) 0.0377(6) Uani 1 1 d . . . H23A H 0.5562 0.5315 0.4346 0.045 Uiso 1 1 calc R . . C24 C 0.56789(17) 0.3347(3) 0.43730(15) 0.0389(6) Uani 1 1 d . . . C25 C 0.52423(17) 0.2233(3) 0.39142(15) 0.0350(6) Uani 1 1 d . . . H25A H 0.5517 0.1407 0.4131 0.042 Uiso 1 1 calc R . . C26 C 0.44065(16) 0.2292(2) 0.31389(14) 0.0313(5) Uani 1 1 d . . . C27 C 0.40737(18) 0.5980(2) 0.29166(17) 0.0396(6) Uani 1 1 d . . . H27A H 0.4484 0.6641 0.3318 0.059 Uiso 1 1 calc R . . H27B H 0.3435 0.6060 0.2869 0.059 Uiso 1 1 calc R . . H27C H 0.4052 0.6109 0.2347 0.059 Uiso 1 1 calc R . . C28 C 0.65668(19) 0.3264(3) 0.52236(16) 0.0493(7) Uani 1 1 d . . . H28A H 0.6751 0.2348 0.5359 0.074 Uiso 1 1 calc R . . H28B H 0.6445 0.3645 0.5683 0.074 Uiso 1 1 calc R . . H28C H 0.7079 0.3743 0.5179 0.074 Uiso 1 1 calc R . . C29 C 0.39873(12) 0.10341(17) 0.26689(11) 0.0351(6) Uani 1 1 d . . . H29A H 0.4364 0.0297 0.3009 0.053 Uiso 1 1 calc R . . H29B H 0.3990 0.1042 0.2104 0.053 Uiso 1 1 calc R . . H29C H 0.3336 0.0948 0.2589 0.053 Uiso 1 1 calc R . . C01 C 0.15396(12) 0.57200(17) 0.10530(11) 0.0360(6) Uani 1 1 d R . . H01A H 0.1047 0.5130 0.1059 0.043 Uiso 1 1 calc R . . H01B H 0.2130 0.5566 0.1588 0.043 Uiso 1 1 calc R . . C02 C 0.0871(3) 0.7257(3) 0.1662(2) 0.0642(9) Uani 1 1 d . . . H02A H 0.0672 0.8166 0.1646 0.096 Uiso 1 1 calc R . . H02B H 0.1365 0.7050 0.2241 0.096 Uiso 1 1 calc R . . H02C H 0.0328 0.6680 0.1519 0.096 Uiso 1 1 calc R . . C03 C 0.1996(3) 0.7976(3) 0.1189(2) 0.0606(9) Uani 1 1 d . . . H03A H 0.1768 0.8869 0.1171 0.091 Uiso 1 1 calc R . . H03B H 0.2211 0.7867 0.0744 0.091 Uiso 1 1 calc R . . H03C H 0.2523 0.7806 0.1759 0.091 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 B 0.0338(14) 0.0261(13) 0.0308(14) -0.0035(11) 0.0163(12) 0.0036(11) N 0.0601(15) 0.0402(13) 0.0468(13) 0.0067(10) 0.0312(12) 0.0161(11) C1 0.0328(12) 0.0298(12) 0.0298(12) -0.0035(10) 0.0150(10) -0.0015(10) C2 0.0320(13) 0.0350(13) 0.0330(13) 0.0004(10) 0.0142(11) 0.0010(11) C3 0.0409(14) 0.0408(14) 0.0415(14) 0.0009(12) 0.0254(12) 0.0062(12) C4 0.0479(15) 0.0405(14) 0.0316(13) 0.0007(11) 0.0229(12) 0.0038(12) C5 0.0480(16) 0.0402(14) 0.0296(13) -0.0023(11) 0.0157(12) 0.0017(12) C6 0.0441(15) 0.0463(16) 0.0326(14) 0.0038(12) 0.0109(12) 0.0048(13) C7 0.0361(14) 0.0396(14) 0.0410(14) 0.0029(12) 0.0163(12) 0.0069(12) C8 0.0339(13) 0.0312(13) 0.0329(13) 0.0008(10) 0.0157(11) 0.0002(10) C9 0.0319(12) 0.0292(12) 0.0308(12) -0.0013(10) 0.0133(11) -0.0004(10) C10 0.0398(14) 0.0330(13) 0.0320(13) -0.0011(10) 0.0169(11) 0.0001(11) C11 0.0301(12) 0.0284(12) 0.0260(11) 0.0020(9) 0.0104(10) 0.0021(10) C12 0.0290(12) 0.0273(12) 0.0280(12) 0.0034(9) 0.0096(10) 0.0031(10) C13 0.0312(12) 0.0353(13) 0.0348(13) 0.0036(10) 0.0161(11) 0.0037(11) C14 0.0285(12) 0.0319(13) 0.0395(14) 0.0030(11) 0.0122(11) 0.0000(10) C15 0.0320(13) 0.0315(13) 0.0326(13) -0.0024(10) 0.0092(11) -0.0013(11) C16 0.0330(13) 0.0320(13) 0.0290(12) -0.0001(10) 0.0117(11) 0.0021(10) C17 0.0344(13) 0.0406(14) 0.0335(13) -0.0031(11) 0.0176(11) -0.0021(11) C18 0.0353(14) 0.0417(15) 0.0536(17) -0.0043(13) 0.0174(13) -0.0063(12) C19 0.0458(15) 0.0411(15) 0.0359(14) -0.0089(11) 0.0187(12) -0.0074(12) C21 0.0284(12) 0.0362(13) 0.0301(12) -0.0027(10) 0.0168(10) -0.0033(10) C22 0.0334(13) 0.0370(13) 0.0350(13) -0.0038(10) 0.0201(11) -0.0051(11) C23 0.0357(13) 0.0466(15) 0.0330(13) -0.0103(11) 0.0175(11) -0.0101(12) C24 0.0317(13) 0.0549(17) 0.0313(13) -0.0046(12) 0.0152(11) -0.0031(12) C25 0.0320(13) 0.0431(14) 0.0318(13) 0.0017(11) 0.0160(11) 0.0030(11) C26 0.0314(12) 0.0380(13) 0.0288(12) -0.0017(10) 0.0174(11) -0.0024(11) C27 0.0425(15) 0.0335(14) 0.0451(15) -0.0062(11) 0.0217(13) -0.0073(12) C28 0.0392(15) 0.070(2) 0.0321(14) -0.0067(13) 0.0102(12) -0.0037(14) C29 0.0357(13) 0.0346(13) 0.0346(13) 0.0001(11) 0.0156(11) 0.0034(11) C01 0.0345(13) 0.0379(14) 0.0371(13) 0.0065(11) 0.0172(11) 0.0065(11) C02 0.085(2) 0.059(2) 0.068(2) 0.0107(16) 0.052(2) 0.0307(18) C03 0.096(3) 0.0324(15) 0.068(2) 0.0034(14) 0.050(2) 0.0057(16) _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 B C1 1.570(3) . ? B C11 1.576(3) . ? B C21 1.587(3) . ? N C03 1.440(4) . ? N C02 1.457(3) . ? N C01 1.462(3) . ? C1 C2 1.385(3) . ? C1 C9 1.450(3) . ? C2 C3 1.406(3) . ? C2 H2A 0.9500 . ? C3 C4 1.364(3) . ? C3 H3A 0.9500 . ? C4 C10 1.417(3) . ? C4 H4A 0.9500 . ? C5 C6 1.363(4) . ? C5 C10 1.415(3) . ? C5 H5A 0.9500 . ? C6 C7 1.405(3) . ? C6 H6A 0.9500 . ? C7 C8 1.379(3) . ? C7 H7A 0.9500 . ? C8 C9 1.428(3) . ? C8 C01 1.516(3) . ? C9 C10 1.426(3) . ? C11 C16 1.425(3) . ? C11 C12 1.422(3) . ? C12 C13 1.387(3) . ? C12 C17 1.516(3) . ? C13 C14 1.391(3) . ? C13 H13A 0.9500 . ? C14 C15 1.383(3) . ? C14 C18 1.506(3) . ? C15 C16 1.387(3) . ? C15 H15A 0.9500 . ? C16 C19 1.511(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C22 1.407(3) . ? C21 C26 1.409(3) . ? C22 C23 1.402(3) . ? C22 C27 1.502(3) . ? C23 C24 1.386(4) . ? C23 H23A 0.9500 . ? C24 C25 1.387(4) . ? C24 C28 1.515(3) . ? C25 C26 1.401(3) . ? C25 H25A 0.9500 . ? C26 C29 1.512(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C01 H01A 0.9900 . ? C01 H01B 0.9900 . ? C02 H02A 0.9800 . ? C02 H02B 0.9800 . ? C02 H02C 0.9800 . ? C03 H03A 0.9800 . ? C03 H03B 0.9800 . ? C03 H03C 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 C1 B C11 122.0(2) . . ? C1 B C21 116.5(2) . . ? C11 B C21 120.5(2) . . ? C03 N C02 110.8(2) . . ? C03 N C01 111.9(2) . . ? C02 N C01 110.0(2) . . ? C2 C1 C9 117.3(2) . . ? C2 C1 B 111.9(2) . . ? C9 C1 B 128.7(2) . . ? C1 C2 C3 123.4(2) . . ? C1 C2 H2A 118.3 . . ? C3 C2 H2A 118.3 . . ? C4 C3 C2 119.2(2) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C4 C10 120.8(2) . . ? C3 C4 H4A 119.6 . . ? C10 C4 H4A 119.6 . . ? C6 C5 C10 120.4(2) . . ? C6 C5 H5A 119.8 . . ? C10 C5 H5A 119.8 . . ? C5 C6 C7 119.7(2) . . ? C5 C6 H6A 120.1 . . ? C7 C6 H6A 120.1 . . ? C8 C7 C6 122.0(2) . . ? C8 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? C7 C8 C9 119.4(2) . . ? C7 C8 C01 116.9(2) . . ? C9 C8 C01 123.7(2) . . ? C8 C9 C10 117.8(2) . . ? C8 C9 C1 123.5(2) . . ? C10 C9 C1 118.6(2) . . ? C5 C10 C4 119.5(2) . . ? C5 C10 C9 120.3(2) . . ? C4 C10 C9 120.1(2) . . ? C16 C11 C12 117.0(2) . . ? C16 C11 B 121.9(2) . . ? C12 C11 B 121.0(2) . . ? C13 C12 C11 120.7(2) . . ? C13 C12 C17 116.8(2) . . ? C11 C12 C17 122.5(2) . . ? C12 C13 C14 122.1(2) . . ? C12 C13 H13A 119.0 . . ? C14 C13 H13A 119.0 . . ? C15 C14 C13 117.3(2) . . ? C15 C14 C18 121.4(2) . . ? C13 C14 C18 121.3(2) . . ? C14 C15 C16 123.1(2) . . ? C14 C15 H15A 118.5 . . ? C16 C15 H15A 118.5 . . ? C15 C16 C11 119.8(2) . . ? C15 C16 C19 116.4(2) . . ? C11 C16 C19 123.8(2) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C21 C26 118.6(2) . . ? C22 C21 B 121.8(2) . . ? C26 C21 B 119.6(2) . . ? C23 C22 C21 119.8(2) . . ? C23 C22 C27 118.7(2) . . ? C21 C22 C27 121.5(2) . . ? C24 C23 C22 121.8(2) . . ? C24 C23 H23A 119.1 . . ? C22 C23 H23A 119.1 . . ? C23 C24 C25 118.1(2) . . ? C23 C24 C28 120.8(2) . . ? C25 C24 C28 121.1(3) . . ? C24 C25 C26 121.8(2) . . ? C24 C25 H25A 119.1 . . ? C26 C25 H25A 119.1 . . ? C25 C26 C21 119.8(2) . . ? C25 C26 C29 118.5(2) . . ? C21 C26 C29 121.65(19) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N C01 C8 111.25(16) . . ? N C01 H01A 109.4 . . ? C8 C01 H01A 109.4 . . ? N C01 H01B 109.4 . . ? C8 C01 H01B 109.4 . . ? H01A C01 H01B 108.0 . . ? N C02 H02A 109.5 . . ? N C02 H02B 109.5 . . ? H02A C02 H02B 109.5 . . ? N C02 H02C 109.5 . . ? H02A C02 H02C 109.5 . . ? H02B C02 H02C 109.5 . . ? N C03 H03A 109.5 . . ? N C03 H03B 109.5 . . ? H03A C03 H03B 109.5 . . ? N C03 H03C 109.5 . . ? H03A C03 H03C 109.5 . . ? H03B C03 H03C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.28 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.417 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.055 # Attachment 'napcn.cif' data_napcn _database_code_depnum_ccdc_archive 'CCDC 663260' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 1-{Mes2B}-CN-8-{CH2NMe3}C10H6 _chemical_formula_sum 'C33 H39 B N2' _chemical_formula_weight 474.47 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.009(3) _cell_length_b 10.329(2) _cell_length_c 17.540(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.12(3) _cell_angle_gamma 90.00 _cell_volume 2705.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9862 _exptl_absorpt_correction_T_max 0.9980 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13047 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.1087 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4757 _reflns_number_gt 2677 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0049P)^2^+12.7300P] 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 SHELXL _refine_ls_extinction_coef 0.0052(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4757 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1393 _refine_ls_R_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.1961 _refine_ls_wR_factor_gt 0.1762 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 N1 N 0.3743(2) 0.5826(3) 0.2841(2) 0.0187(9) Uani 1 1 d . . . N2 N 0.4037(3) 0.8171(4) 0.0524(3) 0.0281(10) Uani 1 1 d . . . C25 C 0.0858(3) 1.0640(4) -0.1233(3) 0.0257(12) Uani 1 1 d . . . H3A H 0.0266 1.0490 -0.1607 0.031 Uiso 1 1 calc R . . C7 C 0.4942(3) 0.8208(5) 0.3281(3) 0.0258(12) Uani 1 1 d . . . H4A H 0.5342 0.7499 0.3352 0.031 Uiso 1 1 calc R . . C01 C 0.3886(3) 0.6853(4) 0.2226(3) 0.0199(11) Uani 1 1 d . . . H5A H 0.4357 0.6543 0.2027 0.024 Uiso 1 1 calc R . . H5B H 0.3324 0.6958 0.1749 0.024 Uiso 1 1 calc R . . C9 C 0.3630(3) 0.9271(4) 0.2495(3) 0.0176(10) Uani 1 1 d . . . C2 C 0.2433(3) 1.0564(4) 0.1769(3) 0.0215(11) Uani 1 1 d . . . H7A H 0.1915 1.0759 0.1306 0.026 Uiso 1 1 calc R . . C23 C 0.2081(3) 1.1831(5) -0.0819(3) 0.0228(11) Uani 1 1 d . . . H8A H 0.2430 1.2558 -0.0852 0.027 Uiso 1 1 calc R . . C16 C 0.1604(3) 0.7043(4) 0.1273(3) 0.0206(11) Uani 1 1 d . . . C4 C 0.3415(3) 1.1377(4) 0.3117(3) 0.0245(11) Uani 1 1 d . . . H10A H 0.3584 1.2009 0.3538 0.029 Uiso 1 1 calc R . . C11 C 0.2064(3) 0.7305(4) 0.0721(3) 0.0182(10) Uani 1 1 d . . . C21 C 0.2071(3) 0.9755(4) -0.0050(3) 0.0212(11) Uani 1 1 d . . . C26 C 0.1221(3) 0.9679(5) -0.0616(3) 0.0222(11) Uani 1 1 d . . . C5 C 0.4709(3) 1.0265(5) 0.3814(3) 0.0237(11) Uani 1 1 d . . . H14A H 0.4865 1.0927 0.4217 0.028 Uiso 1 1 calc R . . C10 C 0.3916(3) 1.0296(4) 0.3142(3) 0.0207(11) Uani 1 1 d . . . C19 C 0.1424(3) 0.8038(5) 0.1866(3) 0.0270(12) Uani 1 1 d . . . H16A H 0.1710 0.8864 0.1834 0.040 Uiso 1 1 calc R . . H16B H 0.1673 0.7706 0.2427 0.040 Uiso 1 1 calc R . . H16C H 0.0778 0.8167 0.1711 0.040 Uiso 1 1 calc R . . C8 C 0.4164(3) 0.8151(4) 0.2661(3) 0.0187(10) Uani 1 1 d . . . C6 C 0.5229(3) 0.9265(5) 0.3857(3) 0.0248(11) Uani 1 1 d . . . H18A H 0.5805 0.9234 0.4276 0.030 Uiso 1 1 calc R . . C1 C 0.2881(3) 0.9469(4) 0.1729(3) 0.0197(11) Uani 1 1 d . . . C13 C 0.1679(3) 0.5117(5) 0.0109(3) 0.0259(12) Uani 1 1 d . . . H20A H 0.1695 0.4477 -0.0275 0.031 Uiso 1 1 calc R . . C27 C 0.3372(3) 1.1185(5) 0.0336(3) 0.0278(12) Uani 1 1 d . . . H21A H 0.3565 1.1996 0.0161 0.042 Uiso 1 1 calc R . . H21B H 0.3773 1.0483 0.0312 0.042 Uiso 1 1 calc R . . H21C H 0.3390 1.1277 0.0898 0.042 Uiso 1 1 calc R . . C29 C 0.0647(3) 0.8597(5) -0.0579(3) 0.0372(15) Uani 1 1 d . . . H22A H 0.0068 0.8668 -0.1029 0.056 Uiso 1 1 calc R . . H22B H 0.0554 0.8618 -0.0057 0.056 Uiso 1 1 calc R . . H22C H 0.0934 0.7779 -0.0627 0.056 Uiso 1 1 calc R . . C3 C 0.2667(3) 1.1478(4) 0.2454(3) 0.0234(11) Uani 1 1 d . . . H23A H 0.2269 1.2174 0.2426 0.028 Uiso 1 1 calc R . . C15 C 0.1232(3) 0.5830(4) 0.1252(3) 0.0230(11) Uani 1 1 d . . . H24A H 0.0944 0.5636 0.1627 0.028 Uiso 1 1 calc R . . C22 C 0.2474(3) 1.0890(4) -0.0195(3) 0.0199(11) Uani 1 1 d . . . C24 C 0.1256(3) 1.1736(5) -0.1349(3) 0.0238(11) Uani 1 1 d . . . C14 C 0.1268(3) 0.4851(5) 0.0681(3) 0.0239(11) Uani 1 1 d . . . C28 C 0.0815(3) 1.2811(5) -0.1977(3) 0.0325(13) Uani 1 1 d . . . H28A H 0.0200 1.2560 -0.2306 0.049 Uiso 1 1 calc R . . H28B H 0.1158 1.2935 -0.2335 0.049 Uiso 1 1 calc R . . H28C H 0.0807 1.3621 -0.1688 0.049 Uiso 1 1 calc R . . C12 C 0.2057(3) 0.6313(4) 0.0114(3) 0.0241(11) Uani 1 1 d . . . B1 B 0.2555(3) 0.8699(5) 0.0751(4) 0.0202(12) Uani 1 1 d . . . C30 C 0.3415(3) 0.8365(4) 0.0606(3) 0.0209(11) Uani 1 1 d . . . C02 C 0.3304(3) 0.4720(5) 0.2268(3) 0.0288(12) Uani 1 1 d . . . H32A H 0.3174 0.4011 0.2581 0.043 Uiso 1 1 calc R . . H32B H 0.3710 0.4411 0.2002 0.043 Uiso 1 1 calc R . . H32C H 0.2745 0.5022 0.1853 0.043 Uiso 1 1 calc R . . C03 C 0.3214(3) 0.6354(5) 0.3313(3) 0.0263(12) Uani 1 1 d . . . H33A H 0.3148 0.5688 0.3685 0.039 Uiso 1 1 calc R . . H33B H 0.2621 0.6616 0.2935 0.039 Uiso 1 1 calc R . . H33C H 0.3524 0.7107 0.3629 0.039 Uiso 1 1 calc R . . C04 C 0.4526(3) 0.5303(5) 0.3524(3) 0.0319(13) Uani 1 1 d . . . H34A H 0.4317 0.4697 0.3847 0.048 Uiso 1 1 calc R . . H34B H 0.4851 0.6016 0.3874 0.048 Uiso 1 1 calc R . . H34C H 0.4925 0.4849 0.3301 0.048 Uiso 1 1 calc R . . C18 C 0.0853(3) 0.3553(5) 0.0654(3) 0.0333(13) Uani 1 1 d . . . H35A H 0.0946 0.3028 0.0227 0.050 Uiso 1 1 calc R . . H35B H 0.0210 0.3655 0.0535 0.050 Uiso 1 1 calc R . . H35C H 0.1130 0.3124 0.1184 0.050 Uiso 1 1 calc R . . C17 C 0.2403(3) 0.6489(5) -0.0617(3) 0.0310(13) Uani 1 1 d . . . H36A H 0.2318 0.5679 -0.0927 0.046 Uiso 1 1 calc R . . H36B H 0.3041 0.6712 -0.0400 0.046 Uiso 1 1 calc R . . H36C H 0.2066 0.7184 -0.0977 0.046 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 N1 0.0076(17) 0.016(2) 0.029(2) 0.0040(17) 0.0027(16) 0.0025(15) N2 0.020(2) 0.028(2) 0.038(3) 0.001(2) 0.012(2) 0.0022(18) C25 0.010(2) 0.024(3) 0.038(3) 0.005(2) 0.003(2) 0.0007(19) C7 0.012(2) 0.027(3) 0.038(3) 0.002(2) 0.008(2) 0.002(2) C01 0.011(2) 0.016(2) 0.031(3) 0.003(2) 0.006(2) 0.0015(18) C9 0.012(2) 0.019(2) 0.023(3) 0.001(2) 0.0079(19) -0.0016(18) C2 0.009(2) 0.021(3) 0.035(3) 0.000(2) 0.008(2) 0.0001(18) C23 0.015(2) 0.020(2) 0.039(3) 0.004(2) 0.016(2) -0.0018(19) C16 0.0067(19) 0.019(2) 0.032(3) 0.001(2) 0.002(2) 0.0016(18) C4 0.018(2) 0.016(2) 0.040(3) -0.006(2) 0.013(2) -0.0032(19) C11 0.0056(19) 0.019(2) 0.026(3) 0.004(2) 0.0009(19) 0.0022(17) C21 0.010(2) 0.023(3) 0.028(3) -0.002(2) 0.004(2) -0.0033(19) C26 0.013(2) 0.023(3) 0.029(3) 0.003(2) 0.006(2) -0.0028(19) C5 0.018(2) 0.026(3) 0.024(3) 0.000(2) 0.005(2) -0.005(2) C10 0.014(2) 0.021(2) 0.028(3) -0.003(2) 0.008(2) -0.0042(19) C19 0.016(2) 0.029(3) 0.040(3) -0.001(2) 0.014(2) -0.004(2) C8 0.010(2) 0.021(2) 0.022(3) 0.001(2) 0.0031(19) 0.0000(18) C6 0.012(2) 0.026(3) 0.031(3) 0.002(2) 0.002(2) -0.002(2) C1 0.011(2) 0.020(3) 0.030(3) 0.004(2) 0.009(2) -0.0007(18) C13 0.017(2) 0.022(3) 0.037(3) -0.003(2) 0.008(2) -0.002(2) C27 0.015(2) 0.024(3) 0.042(3) 0.005(2) 0.007(2) -0.004(2) C29 0.009(2) 0.033(3) 0.056(4) 0.011(3) -0.004(2) -0.010(2) C3 0.013(2) 0.015(2) 0.043(3) -0.002(2) 0.011(2) 0.0001(18) C15 0.009(2) 0.024(3) 0.037(3) 0.005(2) 0.009(2) -0.0015(19) C22 0.010(2) 0.018(2) 0.031(3) -0.002(2) 0.007(2) -0.0021(18) C24 0.016(2) 0.026(3) 0.032(3) 0.005(2) 0.012(2) 0.000(2) C14 0.013(2) 0.019(3) 0.035(3) 0.003(2) 0.003(2) -0.0045(19) C28 0.017(2) 0.031(3) 0.050(4) 0.011(3) 0.013(2) 0.006(2) C12 0.014(2) 0.018(2) 0.039(3) 0.000(2) 0.008(2) -0.0022(19) B1 0.009(2) 0.021(3) 0.032(3) -0.002(2) 0.009(2) -0.004(2) C30 0.020(2) 0.015(2) 0.030(3) -0.002(2) 0.011(2) -0.0022(19) C02 0.017(2) 0.020(3) 0.049(4) 0.001(2) 0.011(2) -0.004(2) C03 0.017(2) 0.034(3) 0.035(3) 0.007(2) 0.018(2) 0.002(2) C04 0.009(2) 0.029(3) 0.048(4) 0.016(3) -0.001(2) 0.004(2) C18 0.022(2) 0.025(3) 0.049(4) 0.000(3) 0.008(2) -0.011(2) C17 0.030(3) 0.029(3) 0.039(3) -0.013(2) 0.018(2) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C03 1.484(6) . ? N1 C04 1.489(5) . ? N1 C02 1.517(6) . ? N1 C01 1.587(6) . ? N2 C30 1.074(5) . ? C25 C24 1.350(6) . ? C25 C26 1.429(6) . ? C25 H3A 0.9500 . ? C7 C8 1.328(6) . ? C7 C6 1.445(7) . ? C7 H4A 0.9500 . ? C01 C8 1.527(6) . ? C01 H5A 0.9900 . ? C01 H5B 0.9900 . ? C9 C8 1.405(6) . ? C9 C1 1.457(6) . ? C9 C10 1.498(6) . ? C2 C1 1.354(6) . ? C2 C3 1.467(6) . ? C2 H7A 0.9500 . ? C23 C24 1.317(6) . ? C23 C22 1.429(6) . ? C23 H8A 0.9500 . ? C16 C15 1.382(6) . ? C16 C11 1.437(6) . ? C16 C19 1.561(6) . ? C4 C3 1.339(7) . ? C4 C10 1.366(6) . ? C4 H10A 0.9500 . ? C11 C12 1.474(7) . ? C11 B1 1.633(6) . ? C21 C26 1.367(6) . ? C21 C22 1.406(6) . ? C21 B1 1.726(7) . ? C26 C29 1.463(6) . ? C5 C6 1.312(6) . ? C5 C10 1.386(6) . ? C5 H14A 0.9500 . ? C19 H16A 0.9800 . ? C19 H16B 0.9800 . ? C19 H16C 0.9800 . ? C6 H18A 0.9500 . ? C1 B1 1.791(7) . ? C13 C12 1.375(6) . ? C13 C14 1.412(7) . ? C13 H20A 0.9500 . ? C27 C22 1.435(6) . ? C27 H21A 0.9800 . ? C27 H21B 0.9800 . ? C27 H21C 0.9800 . ? C29 H22A 0.9800 . ? C29 H22B 0.9800 . ? C29 H22C 0.9800 . ? C3 H23A 0.9500 . ? C15 C14 1.440(7) . ? C15 H24A 0.9500 . ? C24 C28 1.544(6) . ? C14 C18 1.489(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C12 C17 1.580(7) . ? B1 C30 1.527(6) . ? C02 H32A 0.9800 . ? C02 H32B 0.9800 . ? C02 H32C 0.9800 . ? C03 H33A 0.9800 . ? C03 H33B 0.9800 . ? C03 H33C 0.9800 . ? C04 H34A 0.9800 . ? C04 H34B 0.9800 . ? C04 H34C 0.9800 . ? C18 H35A 0.9800 . ? C18 H35B 0.9800 . ? C18 H35C 0.9800 . ? C17 H36A 0.9800 . ? C17 H36B 0.9800 . ? C17 H36C 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 C03 N1 C04 99.7(4) . . ? C03 N1 C02 115.1(3) . . ? C04 N1 C02 108.3(4) . . ? C03 N1 C01 112.6(3) . . ? C04 N1 C01 120.2(3) . . ? C02 N1 C01 101.5(3) . . ? C24 C25 C26 127.7(4) . . ? C24 C25 H3A 116.2 . . ? C26 C25 H3A 116.2 . . ? C8 C7 C6 125.0(4) . . ? C8 C7 H4A 117.5 . . ? C6 C7 H4A 117.5 . . ? C8 C01 N1 109.5(4) . . ? C8 C01 H5A 109.8 . . ? N1 C01 H5A 109.8 . . ? C8 C01 H5B 109.8 . . ? N1 C01 H5B 109.8 . . ? H5A C01 H5B 108.2 . . ? C8 C9 C1 122.9(4) . . ? C8 C9 C10 115.3(4) . . ? C1 C9 C10 121.6(4) . . ? C1 C2 C3 126.6(4) . . ? C1 C2 H7A 116.7 . . ? C3 C2 H7A 116.7 . . ? C24 C23 C22 122.9(4) . . ? C24 C23 H8A 118.5 . . ? C22 C23 H8A 118.5 . . ? C15 C16 C11 118.3(4) . . ? C15 C16 C19 115.7(4) . . ? C11 C16 C19 126.0(4) . . ? C3 C4 C10 115.0(5) . . ? C3 C4 H10A 122.5 . . ? C10 C4 H10A 122.5 . . ? C16 C11 C12 118.9(4) . . ? C16 C11 B1 120.2(4) . . ? C12 C11 B1 120.9(4) . . ? C26 C21 C22 108.6(4) . . ? C26 C21 B1 126.3(4) . . ? C22 C21 B1 125.0(4) . . ? C21 C26 C25 122.5(4) . . ? C21 C26 C29 119.2(4) . . ? C25 C26 C29 118.3(4) . . ? C6 C5 C10 115.8(5) . . ? C6 C5 H14A 122.1 . . ? C10 C5 H14A 122.1 . . ? C4 C10 C5 113.2(4) . . ? C4 C10 C9 122.5(4) . . ? C5 C10 C9 124.3(4) . . ? C16 C19 H16A 109.5 . . ? C16 C19 H16B 109.5 . . ? H16A C19 H16B 109.5 . . ? C16 C19 H16C 109.5 . . ? H16A C19 H16C 109.5 . . ? H16B C19 H16C 109.5 . . ? C7 C8 C9 117.0(4) . . ? C7 C8 C01 117.8(4) . . ? C9 C8 C01 125.0(4) . . ? C5 C6 C7 121.3(4) . . ? C5 C6 H18A 119.4 . . ? C7 C6 H18A 119.4 . . ? C2 C1 C9 110.2(4) . . ? C2 C1 B1 116.3(4) . . ? C9 C1 B1 132.8(4) . . ? C12 C13 C14 119.1(5) . . ? C12 C13 H20A 120.4 . . ? C14 C13 H20A 120.4 . . ? C22 C27 H21A 109.5 . . ? C22 C27 H21B 109.5 . . ? H21A C27 H21B 109.5 . . ? C22 C27 H21C 109.5 . . ? H21A C27 H21C 109.5 . . ? H21B C27 H21C 109.5 . . ? C26 C29 H22A 109.5 . . ? C26 C29 H22B 109.5 . . ? H22A C29 H22B 109.5 . . ? C26 C29 H22C 109.5 . . ? H22A C29 H22C 109.5 . . ? H22B C29 H22C 109.5 . . ? C4 C3 C2 123.0(4) . . ? C4 C3 H23A 118.5 . . ? C2 C3 H23A 118.5 . . ? C16 C15 C14 122.0(4) . . ? C16 C15 H24A 119.0 . . ? C14 C15 H24A 119.0 . . ? C21 C22 C23 127.0(4) . . ? C21 C22 C27 118.5(4) . . ? C23 C22 C27 114.5(4) . . ? C23 C24 C25 111.4(4) . . ? C23 C24 C28 122.3(4) . . ? C25 C24 C28 126.2(4) . . ? C13 C14 C15 120.3(4) . . ? C13 C14 C18 118.0(5) . . ? C15 C14 C18 121.6(4) . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C13 C12 C11 121.2(4) . . ? C13 C12 C17 112.3(4) . . ? C11 C12 C17 126.3(4) . . ? C30 B1 C11 104.4(4) . . ? C30 B1 C21 100.1(4) . . ? C11 B1 C21 117.5(4) . . ? C30 B1 C1 107.0(4) . . ? C11 B1 C1 113.1(4) . . ? C21 B1 C1 112.9(4) . . ? N2 C30 B1 177.0(5) . . ? N1 C02 H32A 109.5 . . ? N1 C02 H32B 109.5 . . ? H32A C02 H32B 109.5 . . ? N1 C02 H32C 109.5 . . ? H32A C02 H32C 109.5 . . ? H32B C02 H32C 109.5 . . ? N1 C03 H33A 109.5 . . ? N1 C03 H33B 109.5 . . ? H33A C03 H33B 109.5 . . ? N1 C03 H33C 109.5 . . ? H33A C03 H33C 109.5 . . ? H33B C03 H33C 109.5 . . ? N1 C04 H34A 109.5 . . ? N1 C04 H34B 109.5 . . ? H34A C04 H34B 109.5 . . ? N1 C04 H34C 109.5 . . ? H34A C04 H34C 109.5 . . ? H34B C04 H34C 109.5 . . ? C14 C18 H35A 109.5 . . ? C14 C18 H35B 109.5 . . ? H35A C18 H35B 109.5 . . ? C14 C18 H35C 109.5 . . ? H35A C18 H35C 109.5 . . ? H35B C18 H35C 109.5 . . ? C12 C17 H36A 109.5 . . ? C12 C17 H36B 109.5 . . ? H36A C17 H36B 109.5 . . ? C12 C17 H36C 109.5 . . ? H36A C17 H36C 109.5 . . ? H36B C17 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.444 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.086