Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Mark A. Fox' ; Department of Chemistry Durham University Durham DH1 3LE UK ; 'Andres E. Goeta' ; Department of Chemistry Durham University Durham DH1 3LE UK ; 'Andrew K. Hughes' ; Department of Chemistry Durham University Durham DH1 3LE UK ; 'Andrew L. Johnson' ; Department of Chemistry Durham University Durham DH1 3LE UK ; _publ_contact_author_name 'Dr Mark Fox' _publ_contact_author_address ; Department of Chemistry University of Durham University Science Laboratories South Road Durham County Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_phone '+44 191 3744702' _publ_contact_author_fax '+44 191 3844737' _publ_contact_author_email M.A.FOX@DURHAM.AC.UK _publ_requested_journal 'Dalton Transactions' #====================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Crystal and molecular structures of the nido-carborane anions, 7,9- and 2,9-C2B9H12- ; _publ_section_references ; Bruker (1998a). SMART-NT V5.0. Data Collection Software. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Bruker (1998b). SAINT-NT V5.0. Data Reduction Software. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Bruker (1998c). SHELXTL-NT. Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1990) Acta Cryst. A46, 467-473 Sheldrick, G.M. (1997) SHELXL-97. Program for the Refinement of Crystal Structures. University of Gottingen, Germany. ; data_1 _database_code_CSD 171782 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H17.5 B4.50 N' _chemical_formula_weight 152.35 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 triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.517(1) _cell_length_b 8.799(2) _cell_length_c 9.158(2) _cell_angle_alpha 65.513(3) _cell_angle_beta 85.279(3) _cell_angle_gamma 83.910(3) _cell_volume 474.79(17) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 938 _cell_measurement_theta_min 13.82 _cell_measurement_theta_max 30.81 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 166 _exptl_absorpt_coefficient_mu 0.054 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART-CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5747 _diffrn_reflns_av_R_equivalents 0.0155 _diffrn_reflns_av_sigmaI/netI 0.0142 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.31 _reflns_number_total 2601 _reflns_number_gt 2342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998a)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998a)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1 (Bruker, 1998c)' _computing_publication_material 'SHELXTL-NT V5.1 (Bruker, 1998c)' _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^)+(0.0932P)^2^+0.1100P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2601 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 N1 N 0.47741(14) 0.61356(10) 0.85011(10) 0.0232(2) Uani 1 1 d . . . H1N H 0.421(2) 0.706(2) 0.8571(18) 0.034(4) Uiso 1 1 d . . . H2N H 0.489(5) 0.536(3) 0.955(3) 0.025(7) Uiso 0.50 1 d P . . C2 C 0.30351(17) 0.68774(14) 0.59542(13) 0.0282(2) Uani 1 1 d . . . H21 H 0.212(2) 0.6442(19) 0.5452(18) 0.032(4) Uiso 1 1 d . . . H22 H 0.232(2) 0.787(2) 0.6034(19) 0.036(4) Uiso 1 1 d . . . C4 C 0.65794(17) 0.77801(13) 0.59090(12) 0.0266(2) Uani 1 1 d . . . H41 H 0.608(2) 0.885(2) 0.5961(18) 0.035(4) Uiso 1 1 d . . . H42 H 0.788(3) 0.796(2) 0.533(2) 0.043(4) Uiso 1 1 d . . . C5 C 0.68109(16) 0.64706(13) 0.76213(12) 0.0252(2) Uani 1 1 d . . . H51 H 0.746(2) 0.539(2) 0.7624(18) 0.036(4) Uiso 1 1 d . . . H52 H 0.763(2) 0.685(2) 0.8240(19) 0.038(4) Uiso 1 1 d . . . C3 C 0.50987(18) 0.72650(15) 0.50215(12) 0.0293(2) Uani 1 1 d . . . H31 H 0.577(2) 0.629(2) 0.4887(19) 0.039(4) Uiso 1 1 d . . . H32 H 0.497(3) 0.814(2) 0.393(2) 0.043(4) Uiso 1 1 d . . . C1 C 0.33448(16) 0.55844(13) 0.76642(12) 0.0251(2) Uani 1 1 d . . . H11 H 0.400(2) 0.4510(19) 0.7663(18) 0.032(4) Uiso 1 1 d . . . H12 H 0.208(2) 0.5379(19) 0.8306(19) 0.033(4) Uiso 1 1 d . . . B1 B 0.19940(18) 0.87844(15) 0.09615(15) 0.0237(2) Uani 0.75 1 d P . . C1B C 0.19940(18) 0.87844(15) 0.09615(15) 0.0237(2) Uani 0.17 1 d P . . H1B H 0.325(3) 0.802(2) 0.154(2) 0.040(4) Uiso 0.92 1 d P . . B2 B 0.2048(2) 1.09253(17) 0.00153(17) 0.0296(3) Uani 0.75 1 d P . . C2B C 0.2048(2) 1.09253(17) 0.00153(17) 0.0296(3) Uani 0.17 1 d P . . H2B H 0.345(3) 1.154(3) 0.007(3) 0.061(6) Uiso 0.92 1 d P . . B3 B 0.20519(19) 0.98139(15) -0.11510(15) 0.0255(3) Uani 0.75 1 d P . . C3B C 0.20519(19) 0.98139(15) -0.11510(15) 0.0255(3) Uani 0.17 1 d P . . H3B H 0.352(3) 0.960(2) -0.189(2) 0.044(5) Uiso 0.92 1 d P . . B4 B 0.0380(2) 0.82090(15) -0.01138(14) 0.0266(3) Uani 0.75 1 d P . . C4B C 0.0380(2) 0.82090(15) -0.01138(14) 0.0266(3) Uani 0.17 1 d P . . H4B H 0.057(3) 0.700(2) -0.017(2) 0.038(4) Uiso 0.92 1 d P . . B5 B -0.0510(2) 0.83130(16) 0.16551(16) 0.0291(3) Uani 0.75 1 d P . . C5B C -0.0510(2) 0.83130(16) 0.16551(16) 0.0291(3) Uani 0.17 1 d P . . H5B H -0.089(3) 0.720(3) 0.276(2) 0.055(5) Uiso 0.92 1 d P . . B6 B 0.05000(18) 0.99927(13) 0.17483(13) 0.0209(2) Uani 0.75 1 d P . . C6B C 0.05000(18) 0.99927(13) 0.17483(13) 0.0209(2) Uani 0.17 1 d P . . H6B H 0.076(3) 1.000(2) 0.278(2) 0.044(5) Uiso 0.92 1 d P . . 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 0.0315(4) 0.0193(4) 0.0181(4) -0.0069(3) -0.0024(3) -0.0011(3) C2 0.0286(5) 0.0305(5) 0.0239(5) -0.0083(4) -0.0071(4) -0.0029(4) C4 0.0316(5) 0.0252(5) 0.0223(5) -0.0077(4) 0.0001(4) -0.0087(4) C5 0.0266(5) 0.0238(5) 0.0246(5) -0.0087(4) -0.0045(4) -0.0028(4) C3 0.0371(6) 0.0322(5) 0.0192(4) -0.0098(4) -0.0006(4) -0.0094(4) C1 0.0274(5) 0.0244(5) 0.0226(4) -0.0079(4) -0.0007(4) -0.0056(4) B1 0.0217(5) 0.0224(5) 0.0277(5) -0.0104(4) -0.0013(4) -0.0034(4) C1B 0.0217(5) 0.0224(5) 0.0277(5) -0.0104(4) -0.0013(4) -0.0034(4) B2 0.0248(5) 0.0320(6) 0.0352(6) -0.0165(5) -0.0025(5) -0.0026(5) C2B 0.0248(5) 0.0320(6) 0.0352(6) -0.0165(5) -0.0025(5) -0.0026(5) B3 0.0285(6) 0.0214(5) 0.0263(5) -0.0103(4) 0.0035(4) -0.0022(4) C3B 0.0285(6) 0.0214(5) 0.0263(5) -0.0103(4) 0.0035(4) -0.0022(4) B4 0.0363(6) 0.0209(5) 0.0229(5) -0.0082(4) -0.0031(4) -0.0054(4) C4B 0.0363(6) 0.0209(5) 0.0229(5) -0.0082(4) -0.0031(4) -0.0054(4) B5 0.0328(6) 0.0288(6) 0.0278(6) -0.0130(5) 0.0004(5) -0.0068(5) C5B 0.0328(6) 0.0288(6) 0.0278(6) -0.0130(5) 0.0004(5) -0.0068(5) B6 0.0270(5) 0.0185(5) 0.0183(5) -0.0079(4) -0.0034(4) -0.0032(4) C6B 0.0270(5) 0.0185(5) 0.0183(5) -0.0079(4) -0.0034(4) -0.0032(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C5 1.4860(13) . ? N1 C1 1.4872(13) . ? N1 H1N 0.879(16) . ? N1 H2N 0.93(2) . ? C2 C1 1.5212(14) . ? C2 C3 1.5236(15) . ? C2 H21 0.975(15) . ? C2 H22 0.975(16) . ? C4 C5 1.5210(14) . ? C4 C3 1.5247(14) . ? C4 H41 0.982(16) . ? C4 H42 0.957(17) . ? C5 H51 0.999(16) . ? C5 H52 0.980(16) . ? C3 H31 0.971(17) . ? C3 H32 0.981(17) . ? C1 H11 0.996(15) . ? C1 H12 0.963(16) . ? B1 B6 1.7021(17) . ? B1 B2 1.7194(18) . ? B1 B5 1.7302(18) . ? B1 B4 1.7404(17) . ? B1 B3 1.7627(18) . ? B1 H1B 1.028(18) . ? B2 C4B 1.6943(19) 2_575 ? B2 B4 1.6943(19) 2_575 ? B2 B3 1.7210(18) . ? B2 B6 1.7444(18) . ? B2 C5B 1.748(2) 2_575 ? B2 B5 1.748(2) 2_575 ? B2 H2B 1.12(2) . ? B3 C5B 1.7415(19) 2_575 ? B3 B5 1.7415(19) 2_575 ? B3 C6B 1.7626(17) 2_575 ? B3 B6 1.7626(17) 2_575 ? B3 B4 1.7685(17) . ? B3 H3B 1.173(18) . ? B4 C2B 1.6943(19) 2_575 ? B4 B2 1.6943(19) 2_575 ? B4 B5 1.7106(19) . ? B4 C6B 1.7489(17) 2_575 ? B4 B6 1.7489(17) 2_575 ? B4 H4B 1.079(17) . ? B5 B6 1.7162(17) . ? B5 C3B 1.7415(19) 2_575 ? B5 B3 1.7415(19) 2_575 ? B5 B2 1.748(2) 2_575 ? B5 C2B 1.748(2) 2_575 ? B5 H5B 1.11(2) . ? B6 C4B 1.7489(17) 2_575 ? B6 B4 1.7489(17) 2_575 ? B6 B3 1.7626(17) 2_575 ? B6 C3B 1.7626(17) 2_575 ? B6 H6B 0.972(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 C5 N1 C1 111.58(8) . . ? C5 N1 H1N 109.0(10) . . ? C1 N1 H1N 108.6(10) . . ? C5 N1 H2N 112.3(19) . . ? C1 N1 H2N 109.8(19) . . ? H1N N1 H2N 105(2) . . ? C1 C2 C3 110.88(9) . . ? C1 C2 H21 107.9(9) . . ? C3 C2 H21 111.8(9) . . ? C1 C2 H22 106.7(9) . . ? C3 C2 H22 111.3(9) . . ? H21 C2 H22 108.1(13) . . ? C5 C4 C3 110.92(8) . . ? C5 C4 H41 107.8(9) . . ? C3 C4 H41 111.0(9) . . ? C5 C4 H42 111.3(10) . . ? C3 C4 H42 109.6(10) . . ? H41 C4 H42 106.0(13) . . ? N1 C5 C4 111.34(8) . . ? N1 C5 H51 107.6(9) . . ? C4 C5 H51 110.5(9) . . ? N1 C5 H52 106.0(9) . . ? C4 C5 H52 111.6(9) . . ? H51 C5 H52 109.7(13) . . ? C2 C3 C4 111.04(8) . . ? C2 C3 H31 111.3(10) . . ? C4 C3 H31 106.7(10) . . ? C2 C3 H32 113.5(10) . . ? C4 C3 H32 108.7(10) . . ? H31 C3 H32 105.2(13) . . ? N1 C1 C2 111.27(8) . . ? N1 C1 H11 106.0(9) . . ? C2 C1 H11 110.5(9) . . ? N1 C1 H12 106.8(9) . . ? C2 C1 H12 112.7(9) . . ? H11 C1 H12 109.3(12) . . ? B6 B1 B2 61.30(7) . . ? B6 B1 B5 59.99(7) . . ? B2 B1 B5 108.71(9) . . ? B6 B1 B4 106.85(9) . . ? B2 B1 B4 106.79(9) . . ? B5 B1 B4 59.06(7) . . ? B6 B1 B3 109.10(8) . . ? B2 B1 B3 59.22(7) . . ? B5 B1 B3 108.98(9) . . ? B4 B1 B3 60.64(7) . . ? B6 B1 H1B 122.1(10) . . ? B2 B1 H1B 122.0(10) . . ? B5 B1 H1B 121.7(10) . . ? B4 B1 H1B 122.3(10) . . ? B3 B1 H1B 120.3(10) . . ? C4B B2 B4 0.00(4) 2_575 2_575 ? C4B B2 B1 107.94(9) 2_575 . ? B4 B2 B1 107.94(9) 2_575 . ? C4B B2 B3 108.29(9) 2_575 . ? B4 B2 B3 108.29(9) 2_575 . ? B1 B2 B3 61.64(7) . . ? C4B B2 B6 61.12(7) 2_575 . ? B4 B2 B6 61.12(7) 2_575 . ? B1 B2 B6 58.86(7) . . ? B3 B2 B6 109.08(9) . . ? C4B B2 C5B 59.58(8) 2_575 2_575 ? B4 B2 C5B 59.58(8) 2_575 2_575 ? B1 B2 C5B 109.17(9) . 2_575 ? B3 B2 C5B 60.27(8) . 2_575 ? B6 B2 C5B 109.02(9) . 2_575 ? C4B B2 B5 59.58(8) 2_575 2_575 ? B4 B2 B5 59.58(8) 2_575 2_575 ? B1 B2 B5 109.17(9) . 2_575 ? B3 B2 B5 60.27(8) . 2_575 ? B6 B2 B5 109.02(9) . 2_575 ? C5B B2 B5 0.00(7) 2_575 2_575 ? C4B B2 H2B 122.0(11) 2_575 . ? B4 B2 H2B 122.0(11) 2_575 . ? B1 B2 H2B 120.2(11) . . ? B3 B2 H2B 121.7(11) . . ? B6 B2 H2B 119.6(11) . . ? C5B B2 H2B 123.0(11) 2_575 . ? B5 B2 H2B 123.0(11) 2_575 . ? B2 B3 C5B 60.62(7) . 2_575 ? B2 B3 B5 60.62(7) . 2_575 ? C5B B3 B5 0.00(8) 2_575 2_575 ? B2 B3 C6B 106.85(9) . 2_575 ? C5B B3 C6B 58.65(7) 2_575 2_575 ? B5 B3 C6B 58.65(7) 2_575 2_575 ? B2 B3 B6 106.85(9) . 2_575 ? C5B B3 B6 58.65(7) 2_575 2_575 ? B5 B3 B6 58.65(7) 2_575 2_575 ? C6B B3 B6 0.00(2) 2_575 2_575 ? B2 B3 B1 59.14(7) . . ? C5B B3 B1 107.47(9) 2_575 . ? B5 B3 B1 107.47(9) 2_575 . ? C6B B3 B1 107.07(8) 2_575 . ? B6 B3 B1 107.07(8) 2_575 . ? B2 B3 B4 105.48(9) . . ? C5B B3 B4 105.62(9) 2_575 . ? B5 B3 B4 105.62(9) 2_575 . ? C6B B3 B4 59.38(7) 2_575 . ? B6 B3 B4 59.38(7) 2_575 . ? B1 B3 B4 59.06(7) . . ? B2 B3 H3B 122.7(9) . . ? C5B B3 H3B 125.4(9) 2_575 . ? B5 B3 H3B 125.4(9) 2_575 . ? C6B B3 H3B 124.0(9) 2_575 . ? B6 B3 H3B 124.0(9) 2_575 . ? B1 B3 H3B 119.3(9) . . ? B4 B3 H3B 121.4(9) . . ? C2B B4 B2 0.00(4) 2_575 2_575 ? C2B B4 B5 61.76(8) 2_575 . ? B2 B4 B5 61.76(8) 2_575 . ? C2B B4 B1 109.43(9) 2_575 . ? B2 B4 B1 109.43(9) 2_575 . ? B5 B4 B1 60.17(7) . . ? C2B B4 C6B 60.85(8) 2_575 2_575 ? B2 B4 C6B 60.85(8) 2_575 2_575 ? B5 B4 C6B 110.54(9) . 2_575 ? B1 B4 C6B 108.68(8) . 2_575 ? C2B B4 B6 60.85(8) 2_575 2_575 ? B2 B4 B6 60.85(8) 2_575 2_575 ? B5 B4 B6 110.54(9) . 2_575 ? B1 B4 B6 108.68(8) . 2_575 ? C6B B4 B6 0.00(7) 2_575 2_575 ? C2B B4 B3 109.47(9) 2_575 . ? B2 B4 B3 109.47(9) 2_575 . ? B5 B4 B3 109.61(9) . . ? B1 B4 B3 60.31(7) . . ? C6B B4 B3 60.14(7) 2_575 . ? B6 B4 B3 60.14(7) 2_575 . ? C2B B4 H4B 118.4(9) 2_575 . ? B2 B4 H4B 118.4(9) 2_575 . ? B5 B4 H4B 118.4(9) . . ? B1 B4 H4B 122.4(10) . . ? C6B B4 H4B 121.3(10) 2_575 . ? B6 B4 H4B 121.3(10) 2_575 . ? B3 B4 H4B 123.4(9) . . ? B4 B5 B6 107.57(9) . . ? B4 B5 B1 60.77(7) . . ? B6 B5 B1 59.19(7) . . ? B4 B5 C3B 106.62(9) . 2_575 ? B6 B5 C3B 61.29(7) . 2_575 ? B1 B5 C3B 108.27(9) . 2_575 ? B4 B5 B3 106.62(9) . 2_575 ? B6 B5 B3 61.29(7) . 2_575 ? B1 B5 B3 108.27(9) . 2_575 ? C3B B5 B3 0.00(7) 2_575 2_575 ? B4 B5 B2 58.66(8) . 2_575 ? B6 B5 B2 107.74(9) . 2_575 ? B1 B5 B2 107.45(9) . 2_575 ? C3B B5 B2 59.11(8) 2_575 2_575 ? B3 B5 B2 59.11(8) 2_575 2_575 ? B4 B5 C2B 58.66(8) . 2_575 ? B6 B5 C2B 107.74(9) . 2_575 ? B1 B5 C2B 107.45(9) . 2_575 ? C3B B5 C2B 59.11(8) 2_575 2_575 ? B3 B5 C2B 59.11(8) 2_575 2_575 ? B2 B5 C2B 0.00(7) 2_575 2_575 ? B4 B5 H5B 123.6(11) . . ? B6 B5 H5B 121.4(11) . . ? B1 B5 H5B 123.3(11) . . ? C3B B5 H5B 119.9(11) 2_575 . ? B3 B5 H5B 119.9(11) 2_575 . ? B2 B5 H5B 121.6(11) 2_575 . ? C2B B5 H5B 121.6(11) 2_575 . ? B1 B6 B5 60.82(7) . . ? B1 B6 B2 59.84(7) . . ? B5 B6 B2 108.20(9) . . ? B1 B6 C4B 106.25(8) . 2_575 ? B5 B6 C4B 107.60(9) . 2_575 ? B2 B6 C4B 58.03(7) . 2_575 ? B1 B6 B4 106.25(8) . 2_575 ? B5 B6 B4 107.60(9) . 2_575 ? B2 B6 B4 58.03(7) . 2_575 ? C4B B6 B4 0.00(9) 2_575 2_575 ? B1 B6 B3 108.58(8) . 2_575 ? B5 B6 B3 60.06(7) . 2_575 ? B2 B6 B3 107.47(8) . 2_575 ? C4B B6 B3 60.48(7) 2_575 2_575 ? B4 B6 B3 60.48(7) 2_575 2_575 ? B1 B6 C3B 108.58(8) . 2_575 ? B5 B6 C3B 60.06(7) . 2_575 ? B2 B6 C3B 107.47(8) . 2_575 ? C4B B6 C3B 60.48(7) 2_575 2_575 ? B4 B6 C3B 60.48(7) 2_575 2_575 ? B3 B6 C3B 0.00(2) 2_575 2_575 ? B1 B6 H6B 122.4(11) . . ? B5 B6 H6B 120.9(11) . . ? B2 B6 H6B 123.2(11) . . ? C4B B6 H6B 122.8(11) 2_575 . ? B4 B6 H6B 122.8(11) 2_575 . ? B3 B6 H6B 120.4(11) 2_575 . ? C3B B6 H6B 120.4(11) 2_575 . ? 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 C1 N1 C5 C4 57.28(10) . . . . ? C3 C4 C5 N1 -55.35(11) . . . . ? C1 C2 C3 C4 -53.93(12) . . . . ? C5 C4 C3 C2 53.80(12) . . . . ? C5 N1 C1 C2 -57.38(11) . . . . ? C3 C2 C1 N1 55.58(12) . . . . ? B6 B1 B2 C4B -37.94(8) . . . 2_575 ? B5 B1 B2 C4B 0.13(12) . . . 2_575 ? B4 B1 B2 C4B 62.43(12) . . . 2_575 ? B3 B1 B2 C4B 101.54(10) . . . 2_575 ? B6 B1 B2 B4 -37.94(8) . . . 2_575 ? B5 B1 B2 B4 0.13(12) . . . 2_575 ? B4 B1 B2 B4 62.43(12) . . . 2_575 ? B3 B1 B2 B4 101.54(10) . . . 2_575 ? B6 B1 B2 B3 -139.48(9) . . . . ? B5 B1 B2 B3 -101.41(10) . . . . ? B4 B1 B2 B3 -39.12(8) . . . . ? B5 B1 B2 B6 38.07(8) . . . . ? B4 B1 B2 B6 100.37(9) . . . . ? B3 B1 B2 B6 139.48(9) . . . . ? B6 B1 B2 C5B -101.13(10) . . . 2_575 ? B5 B1 B2 C5B -63.07(12) . . . 2_575 ? B4 B1 B2 C5B -0.77(12) . . . 2_575 ? B3 B1 B2 C5B 38.35(9) . . . 2_575 ? B6 B1 B2 B5 -101.13(10) . . . 2_575 ? B5 B1 B2 B5 -63.07(12) . . . 2_575 ? B4 B1 B2 B5 -0.77(12) . . . 2_575 ? B3 B1 B2 B5 38.35(9) . . . 2_575 ? C4B B2 B3 C5B 36.59(9) 2_575 . . 2_575 ? B4 B2 B3 C5B 36.59(9) 2_575 . . 2_575 ? B1 B2 B3 C5B 137.56(9) . . . 2_575 ? B6 B2 B3 C5B 101.51(10) . . . 2_575 ? B5 B2 B3 C5B 0.0 2_575 . . 2_575 ? C4B B2 B3 B5 36.59(9) 2_575 . . 2_575 ? B4 B2 B3 B5 36.59(9) 2_575 . . 2_575 ? B1 B2 B3 B5 137.56(9) . . . 2_575 ? B6 B2 B3 B5 101.51(10) . . . 2_575 ? C5B B2 B3 B5 0.0 2_575 . . 2_575 ? C4B B2 B3 C6B -0.81(12) 2_575 . . 2_575 ? B4 B2 B3 C6B -0.81(12) 2_575 . . 2_575 ? B1 B2 B3 C6B 100.15(9) . . . 2_575 ? B6 B2 B3 C6B 64.11(11) . . . 2_575 ? C5B B2 B3 C6B -37.41(8) 2_575 . . 2_575 ? B5 B2 B3 C6B -37.41(8) 2_575 . . 2_575 ? C4B B2 B3 B6 -0.81(12) 2_575 . . 2_575 ? B4 B2 B3 B6 -0.81(12) 2_575 . . 2_575 ? B1 B2 B3 B6 100.15(9) . . . 2_575 ? B6 B2 B3 B6 64.11(11) . . . 2_575 ? C5B B2 B3 B6 -37.41(8) 2_575 . . 2_575 ? B5 B2 B3 B6 -37.41(8) 2_575 . . 2_575 ? C4B B2 B3 B1 -100.96(10) 2_575 . . . ? B4 B2 B3 B1 -100.96(10) 2_575 . . . ? B6 B2 B3 B1 -36.04(8) . . . . ? C5B B2 B3 B1 -137.56(9) 2_575 . . . ? B5 B2 B3 B1 -137.56(9) 2_575 . . . ? C4B B2 B3 B4 -62.88(12) 2_575 . . . ? B4 B2 B3 B4 -62.88(12) 2_575 . . . ? B1 B2 B3 B4 38.08(8) . . . . ? B6 B2 B3 B4 2.04(12) . . . . ? C5B B2 B3 B4 -99.48(10) 2_575 . . . ? B5 B2 B3 B4 -99.48(10) 2_575 . . . ? B6 B1 B3 B2 37.09(8) . . . . ? B5 B1 B3 B2 100.95(10) . . . . ? B4 B1 B3 B2 136.13(9) . . . . ? B6 B1 B3 C5B -0.97(11) . . . 2_575 ? B2 B1 B3 C5B -38.06(8) . . . 2_575 ? B5 B1 B3 C5B 62.89(11) . . . 2_575 ? B4 B1 B3 C5B 98.07(10) . . . 2_575 ? B6 B1 B3 B5 -0.97(11) . . . 2_575 ? B2 B1 B3 B5 -38.06(8) . . . 2_575 ? B5 B1 B3 B5 62.89(11) . . . 2_575 ? B4 B1 B3 B5 98.07(10) . . . 2_575 ? B6 B1 B3 C6B -62.68(11) . . . 2_575 ? B2 B1 B3 C6B -99.77(9) . . . 2_575 ? B5 B1 B3 C6B 1.18(11) . . . 2_575 ? B4 B1 B3 C6B 36.36(8) . . . 2_575 ? B6 B1 B3 B6 -62.68(11) . . . 2_575 ? B2 B1 B3 B6 -99.77(9) . . . 2_575 ? B5 B1 B3 B6 1.18(11) . . . 2_575 ? B4 B1 B3 B6 36.36(8) . . . 2_575 ? B6 B1 B3 B4 -99.04(9) . . . . ? B2 B1 B3 B4 -136.13(9) . . . . ? B5 B1 B3 B4 -35.18(9) . . . . ? B6 B1 B4 C2B 0.95(11) . . . 2_575 ? B2 B1 B4 C2B -63.41(12) . . . 2_575 ? B5 B1 B4 C2B 38.69(9) . . . 2_575 ? B3 B1 B4 C2B -101.87(10) . . . 2_575 ? B6 B1 B4 B2 0.95(11) . . . 2_575 ? B2 B1 B4 B2 -63.41(12) . . . 2_575 ? B5 B1 B4 B2 38.69(9) . . . 2_575 ? B3 B1 B4 B2 -101.87(10) . . . 2_575 ? B6 B1 B4 B5 -37.74(8) . . . . ? B2 B1 B4 B5 -102.10(10) . . . . ? B3 B1 B4 B5 -140.56(9) . . . . ? B6 B1 B4 C6B 65.74(11) . . . 2_575 ? B2 B1 B4 C6B 1.37(12) . . . 2_575 ? B5 B1 B4 C6B 103.48(10) . . . 2_575 ? B3 B1 B4 C6B -37.08(8) . . . 2_575 ? B6 B1 B4 B6 65.74(11) . . . 2_575 ? B2 B1 B4 B6 1.37(12) . . . 2_575 ? B5 B1 B4 B6 103.48(10) . . . 2_575 ? B3 B1 B4 B6 -37.08(8) . . . 2_575 ? B6 B1 B4 B3 102.82(9) . . . . ? B2 B1 B4 B3 38.46(8) . . . . ? B5 B1 B4 B3 140.56(10) . . . . ? B2 B3 B4 C2B 63.68(12) . . . 2_575 ? C5B B3 B4 C2B 0.50(12) 2_575 . . 2_575 ? B5 B3 B4 C2B 0.50(12) 2_575 . . 2_575 ? C6B B3 B4 C2B -37.00(9) 2_575 . . 2_575 ? B6 B3 B4 C2B -37.00(9) 2_575 . . 2_575 ? B1 B3 B4 C2B 101.80(10) . . . 2_575 ? B2 B3 B4 B2 63.68(12) . . . 2_575 ? C5B B3 B4 B2 0.50(12) 2_575 . . 2_575 ? B5 B3 B4 B2 0.50(12) 2_575 . . 2_575 ? C6B B3 B4 B2 -37.00(9) 2_575 . . 2_575 ? B6 B3 B4 B2 -37.00(9) 2_575 . . 2_575 ? B1 B3 B4 B2 101.80(10) . . . 2_575 ? B2 B3 B4 B5 -2.31(12) . . . . ? C5B B3 B4 B5 -65.49(12) 2_575 . . . ? B5 B3 B4 B5 -65.49(12) 2_575 . . . ? C6B B3 B4 B5 -103.00(10) 2_575 . . . ? B6 B3 B4 B5 -103.00(10) 2_575 . . . ? B1 B3 B4 B5 35.81(9) . . . . ? B2 B3 B4 B1 -38.12(8) . . . . ? C5B B3 B4 B1 -101.30(9) 2_575 . . . ? B5 B3 B4 B1 -101.30(9) 2_575 . . . ? C6B B3 B4 B1 -138.80(9) 2_575 . . . ? B6 B3 B4 B1 -138.80(9) 2_575 . . . ? B2 B3 B4 C6B 100.69(9) . . . 2_575 ? C5B B3 B4 C6B 37.51(8) 2_575 . . 2_575 ? B5 B3 B4 C6B 37.51(8) 2_575 . . 2_575 ? B6 B3 B4 C6B 0.0 2_575 . . 2_575 ? B1 B3 B4 C6B 138.80(9) . . . 2_575 ? B2 B3 B4 B6 100.69(9) . . . 2_575 ? C5B B3 B4 B6 37.51(8) 2_575 . . 2_575 ? B5 B3 B4 B6 37.51(8) 2_575 . . 2_575 ? C6B B3 B4 B6 0.0 2_575 . . 2_575 ? B1 B3 B4 B6 138.80(9) . . . 2_575 ? C2B B4 B5 B6 -100.45(10) 2_575 . . . ? B2 B4 B5 B6 -100.45(10) 2_575 . . . ? B1 B4 B5 B6 37.55(8) . . . . ? C6B B4 B5 B6 -62.79(12) 2_575 . . . ? B6 B4 B5 B6 -62.79(12) 2_575 . . . ? B3 B4 B5 B6 1.69(13) . . . . ? C2B B4 B5 B1 -138.00(9) 2_575 . . . ? B2 B4 B5 B1 -138.00(9) 2_575 . . . ? C6B B4 B5 B1 -100.34(9) 2_575 . . . ? B6 B4 B5 B1 -100.34(9) 2_575 . . . ? B3 B4 B5 B1 -35.86(9) . . . . ? C2B B4 B5 C3B -36.00(9) 2_575 . . 2_575 ? B2 B4 B5 C3B -36.00(9) 2_575 . . 2_575 ? B1 B4 B5 C3B 101.99(9) . . . 2_575 ? C6B B4 B5 C3B 1.66(12) 2_575 . . 2_575 ? B6 B4 B5 C3B 1.66(12) 2_575 . . 2_575 ? B3 B4 B5 C3B 66.13(12) . . . 2_575 ? C2B B4 B5 B3 -36.00(9) 2_575 . . 2_575 ? B2 B4 B5 B3 -36.00(9) 2_575 . . 2_575 ? B1 B4 B5 B3 101.99(9) . . . 2_575 ? C6B B4 B5 B3 1.66(12) 2_575 . . 2_575 ? B6 B4 B5 B3 1.66(12) 2_575 . . 2_575 ? B3 B4 B5 B3 66.13(12) . . . 2_575 ? C2B B4 B5 B2 0.0 2_575 . . 2_575 ? B1 B4 B5 B2 138.00(9) . . . 2_575 ? C6B B4 B5 B2 37.66(9) 2_575 . . 2_575 ? B6 B4 B5 B2 37.66(9) 2_575 . . 2_575 ? B3 B4 B5 B2 102.14(10) . . . 2_575 ? B2 B4 B5 C2B 0.0 2_575 . . 2_575 ? B1 B4 B5 C2B 138.00(9) . . . 2_575 ? C6B B4 B5 C2B 37.66(9) 2_575 . . 2_575 ? B6 B4 B5 C2B 37.66(9) 2_575 . . 2_575 ? B3 B4 B5 C2B 102.14(10) . . . 2_575 ? B6 B1 B5 B4 137.43(9) . . . . ? B2 B1 B5 B4 98.78(10) . . . . ? B3 B1 B5 B4 35.84(9) . . . . ? B2 B1 B5 B6 -38.65(9) . . . . ? B4 B1 B5 B6 -137.43(9) . . . . ? B3 B1 B5 B6 -101.59(9) . . . . ? B6 B1 B5 C3B 38.20(8) . . . 2_575 ? B2 B1 B5 C3B -0.45(12) . . . 2_575 ? B4 B1 B5 C3B -99.23(10) . . . 2_575 ? B3 B1 B5 C3B -63.39(12) . . . 2_575 ? B6 B1 B5 B3 38.20(8) . . . 2_575 ? B2 B1 B5 B3 -0.45(12) . . . 2_575 ? B4 B1 B5 B3 -99.23(10) . . . 2_575 ? B3 B1 B5 B3 -63.39(12) . . . 2_575 ? B6 B1 B5 B2 100.62(10) . . . 2_575 ? B2 B1 B5 B2 61.97(12) . . . 2_575 ? B4 B1 B5 B2 -36.81(8) . . . 2_575 ? B3 B1 B5 B2 -0.97(12) . . . 2_575 ? B6 B1 B5 C2B 100.62(10) . . . 2_575 ? B2 B1 B5 C2B 61.97(12) . . . 2_575 ? B4 B1 B5 C2B -36.81(8) . . . 2_575 ? B3 B1 B5 C2B -0.97(12) . . . 2_575 ? B2 B1 B6 B5 137.59(9) . . . . ? B4 B1 B6 B5 37.32(8) . . . . ? B3 B1 B6 B5 101.39(9) . . . . ? B5 B1 B6 B2 -137.59(9) . . . . ? B4 B1 B6 B2 -100.27(9) . . . . ? B3 B1 B6 B2 -36.21(8) . . . . ? B2 B1 B6 C4B 36.17(8) . . . 2_575 ? B5 B1 B6 C4B -101.42(9) . . . 2_575 ? B4 B1 B6 C4B -64.10(10) . . . 2_575 ? B3 B1 B6 C4B -0.03(11) . . . 2_575 ? B2 B1 B6 B4 36.17(8) . . . 2_575 ? B5 B1 B6 B4 -101.42(9) . . . 2_575 ? B4 B1 B6 B4 -64.10(10) . . . 2_575 ? B3 B1 B6 B4 -0.03(11) . . . 2_575 ? B2 B1 B6 B3 99.85(9) . . . 2_575 ? B5 B1 B6 B3 -37.74(8) . . . 2_575 ? B4 B1 B6 B3 -0.43(10) . . . 2_575 ? B3 B1 B6 B3 63.64(11) . . . 2_575 ? B2 B1 B6 C3B 99.85(9) . . . 2_575 ? B5 B1 B6 C3B -37.74(8) . . . 2_575 ? B4 B1 B6 C3B -0.43(10) . . . 2_575 ? B3 B1 B6 C3B 63.64(11) . . . 2_575 ? B4 B5 B6 B1 -38.26(9) . . . . ? C3B B5 B6 B1 -137.97(9) 2_575 . . . ? B3 B5 B6 B1 -137.97(9) 2_575 . . . ? B2 B5 B6 B1 -100.13(10) 2_575 . . . ? C2B B5 B6 B1 -100.13(10) 2_575 . . . ? B4 B5 B6 B2 -0.39(12) . . . . ? B1 B5 B6 B2 37.87(9) . . . . ? C3B B5 B6 B2 -100.10(9) 2_575 . . . ? B3 B5 B6 B2 -100.10(9) 2_575 . . . ? B2 B5 B6 B2 -62.27(12) 2_575 . . . ? C2B B5 B6 B2 -62.27(12) 2_575 . . . ? B4 B5 B6 C4B 60.89(13) . . . 2_575 ? B1 B5 B6 C4B 99.15(9) . . . 2_575 ? C3B B5 B6 C4B -38.82(9) 2_575 . . 2_575 ? B3 B5 B6 C4B -38.82(9) 2_575 . . 2_575 ? B2 B5 B6 C4B -0.98(12) 2_575 . . 2_575 ? C2B B5 B6 C4B -0.98(12) 2_575 . . 2_575 ? B4 B5 B6 B4 60.89(13) . . . 2_575 ? B1 B5 B6 B4 99.15(9) . . . 2_575 ? C3B B5 B6 B4 -38.82(9) 2_575 . . 2_575 ? B3 B5 B6 B4 -38.82(9) 2_575 . . 2_575 ? B2 B5 B6 B4 -0.98(12) 2_575 . . 2_575 ? C2B B5 B6 B4 -0.98(12) 2_575 . . 2_575 ? B4 B5 B6 B3 99.71(10) . . . 2_575 ? B1 B5 B6 B3 137.97(9) . . . 2_575 ? C3B B5 B6 B3 0.0 2_575 . . 2_575 ? B2 B5 B6 B3 37.84(9) 2_575 . . 2_575 ? C2B B5 B6 B3 37.84(9) 2_575 . . 2_575 ? B4 B5 B6 C3B 99.71(10) . . . 2_575 ? B1 B5 B6 C3B 137.97(9) . . . 2_575 ? B3 B5 B6 C3B 0.0 2_575 . . 2_575 ? B2 B5 B6 C3B 37.84(9) 2_575 . . 2_575 ? C2B B5 B6 C3B 37.84(9) 2_575 . . 2_575 ? C4B B2 B6 B1 138.09(9) 2_575 . . . ? B4 B2 B6 B1 138.09(9) 2_575 . . . ? B3 B2 B6 B1 37.23(9) . . . . ? C5B B2 B6 B1 101.39(10) 2_575 . . . ? B5 B2 B6 B1 101.39(10) 2_575 . . . ? C4B B2 B6 B5 99.79(9) 2_575 . . . ? B4 B2 B6 B5 99.79(9) 2_575 . . . ? B1 B2 B6 B5 -38.30(9) . . . . ? B3 B2 B6 B5 -1.07(12) . . . . ? C5B B2 B6 B5 63.09(12) 2_575 . . . ? B5 B2 B6 B5 63.09(12) 2_575 . . . ? B4 B2 B6 C4B 0.0 2_575 . . 2_575 ? B1 B2 B6 C4B -138.09(9) . . . 2_575 ? B3 B2 B6 C4B -100.86(10) . . . 2_575 ? C5B B2 B6 C4B -36.69(8) 2_575 . . 2_575 ? B5 B2 B6 C4B -36.69(8) 2_575 . . 2_575 ? C4B B2 B6 B4 0.0 2_575 . . 2_575 ? B1 B2 B6 B4 -138.09(9) . . . 2_575 ? B3 B2 B6 B4 -100.86(10) . . . 2_575 ? C5B B2 B6 B4 -36.69(8) 2_575 . . 2_575 ? B5 B2 B6 B4 -36.69(8) 2_575 . . 2_575 ? C4B B2 B6 B3 36.35(8) 2_575 . . 2_575 ? B4 B2 B6 B3 36.35(8) 2_575 . . 2_575 ? B1 B2 B6 B3 -101.74(9) . . . 2_575 ? B3 B2 B6 B3 -64.51(11) . . . 2_575 ? C5B B2 B6 B3 -0.34(11) 2_575 . . 2_575 ? B5 B2 B6 B3 -0.34(11) 2_575 . . 2_575 ? C4B B2 B6 C3B 36.35(8) 2_575 . . 2_575 ? B4 B2 B6 C3B 36.35(8) 2_575 . . 2_575 ? B1 B2 B6 C3B -101.74(9) . . . 2_575 ? B3 B2 B6 C3B -64.51(11) . . . 2_575 ? C5B B2 B6 C3B -0.34(11) 2_575 . . 2_575 ? B5 B2 B6 C3B -0.34(11) 2_575 . . 2_575 ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 30.31 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.378 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.052 #===END data_6 _database_code_CSD 171783 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H31 B9 N2' _chemical_formula_weight 348.72 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 triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.578(2) _cell_length_b 10.464(2) _cell_length_c 12.493(3) _cell_angle_alpha 70.326(6) _cell_angle_beta 82.553(6) _cell_angle_gamma 77.184(7) _cell_volume 1027.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 382 _cell_measurement_theta_min 7.65 _cell_measurement_theta_max 25.18 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 372 _exptl_absorpt_coefficient_mu 0.059 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 'Bruker SMART-CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12457 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 30.46 _reflns_number_total 5616 _reflns_number_gt 3719 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998a)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998a)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1 (Bruker, 1998c)' _computing_publication_material 'SHELXTL-NT V5.1 (Bruker, 1998c)' _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^)+(0.1588P)^2^+0.4316P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5616 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2732 _refine_ls_wR_factor_gt 0.2447 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 B1 B 0.7124(3) 0.0702(3) 0.1952(3) 0.0314(6) Uani 1 1 d . . . H1 H 0.808(4) -0.008(4) 0.177(3) 0.054(10) Uiso 1 1 d . . . B2 B 0.6663(4) 0.2346(3) 0.0954(2) 0.0326(6) Uani 1 1 d . . . H2 H 0.727(4) 0.272(3) 0.013(3) 0.039(8) Uiso 1 1 d . . . B3 B 0.5271(3) 0.1242(3) 0.1264(2) 0.0305(6) Uani 1 1 d . . . H3 H 0.499(4) 0.086(3) 0.060(3) 0.041(8) Uiso 1 1 d . . . B4 B 0.5291(3) 0.0304(3) 0.2724(3) 0.0301(6) Uani 1 1 d . . . H4 H 0.504(4) -0.071(3) 0.317(3) 0.037(8) Uiso 1 1 d . . . B5 B 0.6691(3) 0.0819(3) 0.3330(2) 0.0295(6) Uani 1 1 d . . . H5 H 0.733(3) 0.014(3) 0.413(2) 0.030(7) Uiso 1 1 d . . . B6 B 0.7492(3) 0.2172(3) 0.2250(2) 0.0290(5) Uani 1 1 d . . . H6 H 0.877(3) 0.228(3) 0.228(2) 0.032(7) Uiso 1 1 d . . . C7 C 0.4702(3) 0.2935(3) 0.1177(2) 0.0318(5) Uani 1 1 d . . . H7 H 0.408(3) 0.353(3) 0.052(2) 0.031(7) Uiso 1 1 d . . . B8 B 0.3845(3) 0.1888(3) 0.2245(2) 0.0283(5) Uani 1 1 d . . . H8 H 0.251(4) 0.187(3) 0.228(3) 0.041(8) Uiso 1 1 d . . . C9 C 0.4732(3) 0.1486(3) 0.3420(2) 0.0297(5) Uani 1 1 d . . . H9 H 0.418(4) 0.102(4) 0.415(3) 0.049(9) Uiso 1 1 d . . . B10 B 0.5892(3) 0.2607(3) 0.3231(2) 0.0292(5) Uani 1 1 d . . . H10 H 0.615(4) 0.292(3) 0.392(3) 0.041(8) Uiso 1 1 d . . . H12 H 0.510(3) 0.364(3) 0.259(2) 0.031(7) Uiso 1 1 d . . . B11 B 0.5874(4) 0.3601(3) 0.1699(2) 0.0338(6) Uani 1 1 d . . . H11 H 0.611(3) 0.466(3) 0.124(2) 0.030(7) Uiso 1 1 d . . . C12 C 0.1006(3) 0.7735(2) 0.32016(18) 0.0218(4) Uani 1 1 d . . . C13 C 0.1412(3) 0.8333(3) 0.3923(2) 0.0285(5) Uani 1 1 d . . . H13 H 0.233(4) 0.887(3) 0.369(2) 0.035(7) Uiso 1 1 d . . . C14 C 0.0570(3) 0.8201(3) 0.4991(2) 0.0310(5) Uani 1 1 d . . . H14 H 0.088(3) 0.859(3) 0.547(2) 0.031(7) Uiso 1 1 d . . . C15 C -0.0651(3) 0.7480(3) 0.5303(2) 0.0294(5) Uani 1 1 d . . . H15 H -0.119(3) 0.738(3) 0.603(2) 0.027(7) Uiso 1 1 d . . . C16 C -0.1090(3) 0.6854(2) 0.45703(19) 0.0245(5) Uani 1 1 d . . . C17 C -0.2370(3) 0.6107(3) 0.4911(2) 0.0306(5) Uani 1 1 d . . . H17 H -0.285(4) 0.602(3) 0.564(3) 0.041(8) Uiso 1 1 d . . . C18 C -0.2786(3) 0.5480(3) 0.4221(2) 0.0340(6) Uani 1 1 d . . . H18 H -0.365(4) 0.494(4) 0.445(3) 0.054(10) Uiso 1 1 d . . . C19 C -0.1981(3) 0.5597(3) 0.3145(2) 0.0304(5) Uani 1 1 d . . . H19 H -0.227(4) 0.513(3) 0.267(3) 0.045(9) Uiso 1 1 d . . . C20 C -0.0760(3) 0.6327(2) 0.27739(18) 0.0224(4) Uani 1 1 d . . . C21 C -0.0260(2) 0.6973(2) 0.34829(17) 0.0206(4) Uani 1 1 d . . . C22 C -0.1064(4) 0.7221(3) 0.0721(2) 0.0377(6) Uani 1 1 d . . . H22A H -0.166(4) 0.815(4) 0.087(3) 0.048(9) Uiso 1 1 d . . . H22B H -0.185(4) 0.667(4) 0.072(3) 0.053(10) Uiso 1 1 d . . . H22C H -0.044(4) 0.738(3) -0.001(3) 0.048(9) Uiso 1 1 d . . . C23 C 0.0881(4) 0.5118(3) 0.1531(2) 0.0365(6) Uani 1 1 d . . . H23A H 0.139(4) 0.529(3) 0.080(3) 0.044(9) Uiso 1 1 d . . . H23B H 0.005(4) 0.452(4) 0.158(3) 0.057(10) Uiso 1 1 d . . . H23C H 0.165(4) 0.463(4) 0.212(3) 0.049(9) Uiso 1 1 d . . . C24 C 0.1846(3) 0.9334(3) 0.1354(2) 0.0299(5) Uani 1 1 d . . . H24A H 0.077(4) 0.974(3) 0.129(2) 0.029(7) Uiso 1 1 d . . . H24B H 0.231(4) 0.934(3) 0.064(3) 0.042(8) Uiso 1 1 d . . . H24C H 0.242(4) 0.980(4) 0.169(3) 0.056(10) Uiso 1 1 d . . . C25 C 0.3629(3) 0.7110(3) 0.2238(2) 0.0339(6) Uani 1 1 d . . . H25A H 0.364(4) 0.616(4) 0.273(3) 0.043(8) Uiso 1 1 d . . . H25B H 0.422(4) 0.759(3) 0.262(2) 0.035(7) Uiso 1 1 d . . . H25C H 0.411(4) 0.718(3) 0.152(3) 0.045(9) Uiso 1 1 d . . . N26 N 0.1927(2) 0.7864(2) 0.20935(16) 0.0237(4) Uani 1 1 d . . . H26 H 0.125(5) 0.732(4) 0.172(3) 0.066(11) Uiso 1 1 d . . . N27 N 0.0047(2) 0.64749(19) 0.16395(16) 0.0246(4) 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 B1 0.0222(12) 0.0312(13) 0.0457(16) -0.0200(12) 0.0049(11) -0.0066(10) B2 0.0361(14) 0.0414(15) 0.0263(13) -0.0141(11) 0.0066(11) -0.0188(12) B3 0.0272(12) 0.0392(15) 0.0331(13) -0.0205(12) 0.0036(10) -0.0116(11) B4 0.0267(12) 0.0244(12) 0.0397(15) -0.0111(11) 0.0039(11) -0.0078(10) B5 0.0270(12) 0.0252(12) 0.0333(14) -0.0032(10) -0.0047(10) -0.0072(10) B6 0.0289(12) 0.0326(13) 0.0284(12) -0.0100(11) 0.0009(10) -0.0129(10) C7 0.0347(12) 0.0333(13) 0.0267(12) -0.0079(10) -0.0051(9) -0.0061(10) B8 0.0234(12) 0.0347(14) 0.0295(13) -0.0147(11) 0.0011(10) -0.0052(10) C9 0.0301(11) 0.0333(12) 0.0250(11) -0.0092(9) 0.0037(9) -0.0081(9) B10 0.0362(14) 0.0278(13) 0.0259(12) -0.0104(10) -0.0022(10) -0.0075(11) B11 0.0472(16) 0.0258(13) 0.0273(13) -0.0042(11) -0.0038(12) -0.0103(12) C12 0.0238(10) 0.0211(10) 0.0208(10) -0.0068(8) -0.0010(8) -0.0048(8) C13 0.0288(11) 0.0311(12) 0.0305(12) -0.0136(10) -0.0031(9) -0.0085(9) C14 0.0341(12) 0.0338(12) 0.0286(12) -0.0154(10) -0.0070(9) -0.0020(10) C15 0.0343(12) 0.0298(12) 0.0209(10) -0.0085(9) -0.0016(9) 0.0013(9) C16 0.0242(10) 0.0222(10) 0.0236(10) -0.0057(8) 0.0009(8) -0.0012(8) C17 0.0283(11) 0.0296(12) 0.0289(12) -0.0070(9) 0.0075(9) -0.0046(9) C18 0.0274(12) 0.0331(13) 0.0419(14) -0.0117(11) 0.0070(10) -0.0119(10) C19 0.0284(11) 0.0325(12) 0.0340(12) -0.0128(10) 0.0022(9) -0.0123(9) C20 0.0239(10) 0.0210(10) 0.0227(10) -0.0076(8) -0.0002(8) -0.0049(8) C21 0.0218(9) 0.0179(9) 0.0203(9) -0.0040(8) -0.0020(7) -0.0027(7) C22 0.0458(15) 0.0407(15) 0.0275(12) -0.0079(11) -0.0090(11) -0.0108(12) C23 0.0461(15) 0.0279(12) 0.0363(14) -0.0149(11) 0.0108(12) -0.0091(11) C24 0.0301(12) 0.0273(12) 0.0307(12) -0.0062(10) 0.0042(10) -0.0102(9) C25 0.0257(11) 0.0381(14) 0.0398(14) -0.0187(12) -0.0001(10) -0.0013(10) N26 0.0226(9) 0.0257(9) 0.0249(9) -0.0099(7) 0.0022(7) -0.0081(7) N27 0.0300(9) 0.0242(9) 0.0220(9) -0.0087(7) -0.0001(7) -0.0085(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 B1 B2 1.747(4) . ? B1 B5 1.752(4) . ? B1 B4 1.789(4) . ? B1 B3 1.792(4) . ? B1 B6 1.799(4) . ? B1 H1 1.09(4) . ? B2 C7 1.680(4) . ? B2 B3 1.761(4) . ? B2 B6 1.790(4) . ? B2 B11 1.821(4) . ? B2 H2 1.08(3) . ? B3 C7 1.700(4) . ? B3 B4 1.756(4) . ? B3 B8 1.805(4) . ? B3 H3 1.10(3) . ? B4 C9 1.694(4) . ? B4 B5 1.761(4) . ? B4 B8 1.805(4) . ? B4 H4 1.07(3) . ? B5 C9 1.675(4) . ? B5 B6 1.789(4) . ? B5 B10 1.811(4) . ? B5 H5 1.13(3) . ? B6 B10 1.803(4) . ? B6 B11 1.808(4) . ? B6 H6 1.13(3) . ? C7 B8 1.624(4) . ? C7 B11 1.646(4) . ? C7 H7 0.98(3) . ? B8 C9 1.626(4) . ? B8 H8 1.15(3) . ? C9 B10 1.641(4) . ? C9 H9 0.99(4) . ? B10 B11 1.845(4) . ? B10 H10 1.08(3) . ? B10 H12 1.23(3) . ? B11 H12 1.23(3) . ? B11 H11 1.11(3) . ? C12 C13 1.372(3) . ? C12 C21 1.426(3) . ? C12 N26 1.482(3) . ? C13 C14 1.412(3) . ? C13 H13 1.02(3) . ? C14 C15 1.365(4) . ? C14 H14 0.92(3) . ? C15 C16 1.418(3) . ? C15 H15 0.95(3) . ? C16 C17 1.426(3) . ? C16 C21 1.429(3) . ? C17 C18 1.366(4) . ? C17 H17 0.93(3) . ? C18 C19 1.409(4) . ? C18 H18 0.98(4) . ? C19 C20 1.373(3) . ? C19 H19 0.97(3) . ? C20 C21 1.435(3) . ? C20 N27 1.469(3) . ? C22 N27 1.478(3) . ? C22 H22A 1.06(3) . ? C22 H22B 0.98(4) . ? C22 H22C 0.98(3) . ? C23 N27 1.483(3) . ? C23 H23A 0.94(3) . ? C23 H23B 1.03(4) . ? C23 H23C 0.98(4) . ? C24 N26 1.496(3) . ? C24 H24A 0.93(3) . ? C24 H24B 0.92(3) . ? C24 H24C 0.98(4) . ? C25 N26 1.499(3) . ? C25 H25A 0.97(3) . ? C25 H25B 1.03(3) . ? C25 H25C 0.93(3) . ? N26 H26 1.13(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B2 B1 B5 109.6(2) . . ? B2 B1 B4 107.2(2) . . ? B5 B1 B4 59.65(16) . . ? B2 B1 B3 59.66(17) . . ? B5 B1 B3 107.27(19) . . ? B4 B1 B3 58.74(16) . . ? B2 B1 B6 60.63(16) . . ? B5 B1 B6 60.49(15) . . ? B4 B1 B6 106.88(19) . . ? B3 B1 B6 107.0(2) . . ? B2 B1 H1 121.1(18) . . ? B5 B1 H1 121.5(18) . . ? B4 B1 H1 122.4(19) . . ? B3 B1 H1 122.1(18) . . ? B6 B1 H1 122.7(19) . . ? C7 B2 B1 106.67(19) . . ? C7 B2 B3 59.17(16) . . ? B1 B2 B3 61.45(16) . . ? C7 B2 B6 103.46(19) . . ? B1 B2 B6 61.11(16) . . ? B3 B2 B6 108.76(19) . . ? C7 B2 B11 55.92(16) . . ? B1 B2 B11 109.10(19) . . ? B3 B2 B11 106.17(19) . . ? B6 B2 B11 60.08(16) . . ? C7 B2 H2 120.9(16) . . ? B1 B2 H2 126.4(17) . . ? B3 B2 H2 124.2(16) . . ? B6 B2 H2 122.6(16) . . ? B11 B2 H2 117.0(16) . . ? C7 B3 B4 106.02(19) . . ? C7 B3 B2 58.04(16) . . ? B4 B3 B2 108.01(19) . . ? C7 B3 B1 103.79(18) . . ? B4 B3 B1 60.53(16) . . ? B2 B3 B1 58.88(16) . . ? C7 B3 B8 55.11(15) . . ? B4 B3 B8 60.89(16) . . ? B2 B3 B8 101.77(19) . . ? B1 B3 B8 104.34(18) . . ? C7 B3 H3 121.1(17) . . ? B4 B3 H3 124.7(17) . . ? B2 B3 H3 120.3(17) . . ? B1 B3 H3 125.2(17) . . ? B8 B3 H3 126.1(17) . . ? C9 B4 B3 106.3(2) . . ? C9 B4 B5 57.96(15) . . ? B3 B4 B5 108.45(19) . . ? C9 B4 B1 103.97(19) . . ? B3 B4 B1 60.72(16) . . ? B5 B4 B1 59.13(16) . . ? C9 B4 B8 55.26(14) . . ? B3 B4 B8 60.88(16) . . ? B5 B4 B8 101.91(18) . . ? B1 B4 B8 104.47(19) . . ? C9 B4 H4 116.2(16) . . ? B3 B4 H4 129.9(16) . . ? B5 B4 H4 115.8(16) . . ? B1 B4 H4 126.8(16) . . ? B8 B4 H4 126.5(16) . . ? C9 B5 B1 106.39(19) . . ? C9 B5 B4 59.00(15) . . ? B1 B5 B4 61.22(16) . . ? C9 B5 B6 103.49(19) . . ? B1 B5 B6 61.04(16) . . ? B4 B5 B6 108.51(19) . . ? C9 B5 B10 55.98(15) . . ? B1 B5 B10 108.92(19) . . ? B4 B5 B10 105.95(18) . . ? B6 B5 B10 60.12(15) . . ? C9 B5 H5 120.3(14) . . ? B1 B5 H5 127.2(14) . . ? B4 B5 H5 124.0(14) . . ? B6 B5 H5 123.2(14) . . ? B10 B5 H5 116.8(14) . . ? B5 B6 B2 106.01(18) . . ? B5 B6 B1 58.47(16) . . ? B2 B6 B1 58.26(16) . . ? B5 B6 B10 60.56(15) . . ? B2 B6 B10 108.99(19) . . ? B1 B6 B10 107.23(18) . . ? B5 B6 B11 109.10(19) . . ? B2 B6 B11 60.81(17) . . ? B1 B6 B11 107.40(19) . . ? B10 B6 B11 61.43(16) . . ? B5 B6 H6 119.6(14) . . ? B2 B6 H6 122.4(14) . . ? B1 B6 H6 119.6(15) . . ? B10 B6 H6 122.8(14) . . ? B11 B6 H6 124.4(15) . . ? B8 C7 B11 107.6(2) . . ? B8 C7 B2 113.7(2) . . ? B11 C7 B2 66.38(18) . . ? B8 C7 B3 65.72(16) . . ? B11 C7 B3 117.7(2) . . ? B2 C7 B3 62.79(16) . . ? B8 C7 H7 119.6(17) . . ? B11 C7 H7 119.3(17) . . ? B2 C7 H7 118.6(17) . . ? B3 C7 H7 115.4(17) . . ? C7 B8 C9 112.4(2) . . ? C7 B8 B4 107.14(19) . . ? C9 B8 B4 58.90(16) . . ? C7 B8 B3 59.17(16) . . ? C9 B8 B3 107.05(19) . . ? B4 B8 B3 58.23(16) . . ? C7 B8 H8 121.7(16) . . ? C9 B8 H8 119.8(16) . . ? B4 B8 H8 120.6(16) . . ? B3 B8 H8 121.7(16) . . ? B8 C9 B10 107.5(2) . . ? B8 C9 B5 114.10(19) . . ? B10 C9 B5 66.21(16) . . ? B8 C9 B4 65.84(17) . . ? B10 C9 B4 117.61(19) . . ? B5 C9 B4 63.04(16) . . ? B8 C9 H9 118.7(19) . . ? B10 C9 H9 126.0(19) . . ? B5 C9 H9 113(2) . . ? B4 C9 H9 106(2) . . ? C9 B10 B6 104.29(18) . . ? C9 B10 B5 57.81(15) . . ? B6 B10 B5 59.32(15) . . ? C9 B10 B11 105.30(19) . . ? B6 B10 B11 59.41(16) . . ? B5 B10 B11 106.53(19) . . ? C9 B10 H10 122.4(17) . . ? B6 B10 H10 119.8(17) . . ? B5 B10 H10 115.5(17) . . ? B11 B10 H10 127.9(17) . . ? C9 B10 H12 100.2(13) . . ? B6 B10 H12 100.6(14) . . ? B5 B10 H12 139.0(13) . . ? B11 B10 H12 41.4(13) . . ? H10 B10 H12 106(2) . . ? C7 B11 B6 104.07(19) . . ? C7 B11 B2 57.69(16) . . ? B6 B11 B2 59.11(16) . . ? C7 B11 B10 104.9(2) . . ? B6 B11 B10 59.16(15) . . ? B2 B11 B10 105.87(19) . . ? C7 B11 H12 100.0(13) . . ? B6 B11 H12 100.4(13) . . ? B2 B11 H12 138.3(13) . . ? B10 B11 H12 41.4(13) . . ? C7 B11 H11 120.6(14) . . ? B6 B11 H11 121.0(15) . . ? B2 B11 H11 114.7(15) . . ? B10 B11 H11 130.2(14) . . ? H12 B11 H11 107(2) . . ? C13 C12 C21 122.5(2) . . ? C13 C12 N26 119.1(2) . . ? C21 C12 N26 118.40(18) . . ? C12 C13 C14 120.0(2) . . ? C12 C13 H13 120.1(17) . . ? C14 C13 H13 119.9(17) . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 121.7(18) . . ? C13 C14 H14 118.4(18) . . ? C14 C15 C16 121.1(2) . . ? C14 C15 H15 119.1(17) . . ? C16 C15 H15 119.8(17) . . ? C15 C16 C17 120.2(2) . . ? C15 C16 C21 120.3(2) . . ? C17 C16 C21 119.5(2) . . ? C18 C17 C16 120.8(2) . . ? C18 C17 H17 122(2) . . ? C16 C17 H17 117(2) . . ? C17 C18 C19 120.2(2) . . ? C17 C18 H18 122(2) . . ? C19 C18 H18 118(2) . . ? C20 C19 C18 121.0(2) . . ? C20 C19 H19 119(2) . . ? C18 C19 H19 120(2) . . ? C19 C20 C21 120.6(2) . . ? C19 C20 N27 120.7(2) . . ? C21 C20 N27 118.65(18) . . ? C12 C21 C16 116.32(19) . . ? C12 C21 C20 125.78(19) . . ? C16 C21 C20 117.90(19) . . ? N27 C22 H22A 107.1(18) . . ? N27 C22 H22B 111(2) . . ? H22A C22 H22B 110(3) . . ? N27 C22 H22C 108(2) . . ? H22A C22 H22C 113(3) . . ? H22B C22 H22C 107(3) . . ? N27 C23 H23A 107(2) . . ? N27 C23 H23B 110(2) . . ? H23A C23 H23B 107(3) . . ? N27 C23 H23C 112(2) . . ? H23A C23 H23C 111(3) . . ? H23B C23 H23C 110(3) . . ? N26 C24 H24A 107.2(17) . . ? N26 C24 H24B 109(2) . . ? H24A C24 H24B 109(3) . . ? N26 C24 H24C 110(2) . . ? H24A C24 H24C 112(3) . . ? H24B C24 H24C 110(3) . . ? N26 C25 H25A 109(2) . . ? N26 C25 H25B 109.2(17) . . ? H25A C25 H25B 109(2) . . ? N26 C25 H25C 108(2) . . ? H25A C25 H25C 114(3) . . ? H25B C25 H25C 108(3) . . ? C12 N26 C24 112.78(18) . . ? C12 N26 C25 112.08(18) . . ? C24 N26 C25 111.13(19) . . ? C12 N26 H26 100(2) . . ? C24 N26 H26 110(2) . . ? C25 N26 H26 110(2) . . ? C20 N27 C22 112.0(2) . . ? C20 N27 C23 111.57(18) . . ? C22 N27 C23 111.0(2) . . ? 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 B5 B1 B2 C7 -59.6(2) . . . . ? B4 B1 B2 C7 3.6(3) . . . . ? B3 B1 B2 C7 39.48(18) . . . . ? B6 B1 B2 C7 -96.4(2) . . . . ? B5 B1 B2 B3 -99.0(2) . . . . ? B4 B1 B2 B3 -35.86(18) . . . . ? B6 B1 B2 B3 -135.92(19) . . . . ? B5 B1 B2 B6 36.88(18) . . . . ? B4 B1 B2 B6 100.1(2) . . . . ? B3 B1 B2 B6 135.92(19) . . . . ? B5 B1 B2 B11 -0.6(3) . . . . ? B4 B1 B2 B11 62.6(2) . . . . ? B3 B1 B2 B11 98.5(2) . . . . ? B6 B1 B2 B11 -37.46(19) . . . . ? B1 B2 B3 C7 134.8(2) . . . . ? B6 B2 B3 C7 94.8(2) . . . . ? B11 B2 B3 C7 31.53(18) . . . . ? C7 B2 B3 B4 -98.0(2) . . . . ? B1 B2 B3 B4 36.83(19) . . . . ? B6 B2 B3 B4 -3.2(3) . . . . ? B11 B2 B3 B4 -66.5(2) . . . . ? C7 B2 B3 B1 -134.8(2) . . . . ? B6 B2 B3 B1 -40.04(19) . . . . ? B11 B2 B3 B1 -103.3(2) . . . . ? C7 B2 B3 B8 -35.05(17) . . . . ? B1 B2 B3 B8 99.8(2) . . . . ? B6 B2 B3 B8 59.7(2) . . . . ? B11 B2 B3 B8 -3.5(2) . . . . ? B2 B1 B3 C7 -38.29(18) . . . . ? B5 B1 B3 C7 64.7(2) . . . . ? B4 B1 B3 C7 100.8(2) . . . . ? B6 B1 B3 C7 1.1(2) . . . . ? B2 B1 B3 B4 -139.1(2) . . . . ? B5 B1 B3 B4 -36.13(19) . . . . ? B6 B1 B3 B4 -99.8(2) . . . . ? B5 B1 B3 B2 103.0(2) . . . . ? B4 B1 B3 B2 139.1(2) . . . . ? B6 B1 B3 B2 39.35(18) . . . . ? B2 B1 B3 B8 -95.3(2) . . . . ? B5 B1 B3 B8 7.7(3) . . . . ? B4 B1 B3 B8 43.85(18) . . . . ? B6 B1 B3 B8 -55.9(2) . . . . ? C7 B3 B4 C9 0.1(2) . . . . ? B2 B3 B4 C9 61.0(2) . . . . ? B1 B3 B4 C9 97.2(2) . . . . ? B8 B3 B4 C9 -32.65(17) . . . . ? C7 B3 B4 B5 -60.9(2) . . . . ? B2 B3 B4 B5 0.1(3) . . . . ? B1 B3 B4 B5 36.18(18) . . . . ? B8 B3 B4 B5 -93.6(2) . . . . ? C7 B3 B4 B1 -97.05(19) . . . . ? B2 B3 B4 B1 -36.12(19) . . . . ? B8 B3 B4 B1 -129.81(19) . . . . ? C7 B3 B4 B8 32.76(17) . . . . ? B2 B3 B4 B8 93.7(2) . . . . ? B1 B3 B4 B8 129.81(19) . . . . ? B2 B1 B4 C9 -64.8(2) . . . . ? B5 B1 B4 C9 38.23(18) . . . . ? B3 B1 B4 C9 -101.0(2) . . . . ? B6 B1 B4 C9 -1.0(3) . . . . ? B2 B1 B4 B3 36.27(19) . . . . ? B5 B1 B4 B3 139.3(2) . . . . ? B6 B1 B4 B3 100.0(2) . . . . ? B2 B1 B4 B5 -103.0(2) . . . . ? B3 B1 B4 B5 -139.3(2) . . . . ? B6 B1 B4 B5 -39.28(19) . . . . ? B2 B1 B4 B8 -7.6(2) . . . . ? B5 B1 B4 B8 95.4(2) . . . . ? B3 B1 B4 B8 -43.88(18) . . . . ? B6 B1 B4 B8 56.1(2) . . . . ? B2 B1 B5 C9 59.7(2) . . . . ? B4 B1 B5 C9 -39.27(18) . . . . ? B3 B1 B5 C9 -3.5(3) . . . . ? B6 B1 B5 C9 96.6(2) . . . . ? B2 B1 B5 B4 98.9(2) . . . . ? B3 B1 B5 B4 35.74(18) . . . . ? B6 B1 B5 B4 135.9(2) . . . . ? B2 B1 B5 B6 -36.94(18) . . . . ? B4 B1 B5 B6 -135.9(2) . . . . ? B3 B1 B5 B6 -100.1(2) . . . . ? B2 B1 B5 B10 0.7(3) . . . . ? B4 B1 B5 B10 -98.2(2) . . . . ? B3 B1 B5 B10 -62.5(2) . . . . ? B6 B1 B5 B10 37.66(18) . . . . ? B3 B4 B5 C9 98.0(2) . . . . ? B1 B4 B5 C9 134.9(2) . . . . ? B8 B4 B5 C9 35.02(17) . . . . ? C9 B4 B5 B1 -134.9(2) . . . . ? B3 B4 B5 B1 -36.87(19) . . . . ? B8 B4 B5 B1 -99.9(2) . . . . ? C9 B4 B5 B6 -94.9(2) . . . . ? B3 B4 B5 B6 3.1(3) . . . . ? B1 B4 B5 B6 39.96(19) . . . . ? B8 B4 B5 B6 -59.9(2) . . . . ? C9 B4 B5 B10 -31.72(18) . . . . ? B3 B4 B5 B10 66.3(2) . . . . ? B1 B4 B5 B10 103.2(2) . . . . ? B8 B4 B5 B10 3.3(2) . . . . ? C9 B5 B6 B2 -66.4(2) . . . . ? B1 B5 B6 B2 35.09(19) . . . . ? B4 B5 B6 B2 -5.0(3) . . . . ? B10 B5 B6 B2 -103.1(2) . . . . ? C9 B5 B6 B1 -101.5(2) . . . . ? B4 B5 B6 B1 -40.05(19) . . . . ? B10 B5 B6 B1 -138.2(2) . . . . ? C9 B5 B6 B10 36.72(17) . . . . ? B1 B5 B6 B10 138.2(2) . . . . ? B4 B5 B6 B10 98.2(2) . . . . ? C9 B5 B6 B11 -2.3(2) . . . . ? B1 B5 B6 B11 99.1(2) . . . . ? B4 B5 B6 B11 59.1(2) . . . . ? B10 B5 B6 B11 -39.06(18) . . . . ? C7 B2 B6 B5 66.6(2) . . . . ? B1 B2 B6 B5 -35.18(18) . . . . ? B3 B2 B6 B5 5.0(3) . . . . ? B11 B2 B6 B5 103.3(2) . . . . ? C7 B2 B6 B1 101.8(2) . . . . ? B3 B2 B6 B1 40.20(19) . . . . ? B11 B2 B6 B1 138.5(2) . . . . ? C7 B2 B6 B10 2.9(2) . . . . ? B1 B2 B6 B10 -98.9(2) . . . . ? B3 B2 B6 B10 -58.8(3) . . . . ? B11 B2 B6 B10 39.51(19) . . . . ? C7 B2 B6 B11 -36.64(18) . . . . ? B1 B2 B6 B11 -138.5(2) . . . . ? B3 B2 B6 B11 -98.3(2) . . . . ? B2 B1 B6 B5 139.5(2) . . . . ? B4 B1 B6 B5 38.88(19) . . . . ? B3 B1 B6 B5 100.6(2) . . . . ? B5 B1 B6 B2 -139.5(2) . . . . ? B4 B1 B6 B2 -100.6(2) . . . . ? B3 B1 B6 B2 -38.90(18) . . . . ? B2 B1 B6 B10 102.0(2) . . . . ? B5 B1 B6 B10 -37.42(18) . . . . ? B4 B1 B6 B10 1.5(3) . . . . ? B3 B1 B6 B10 63.2(2) . . . . ? B2 B1 B6 B11 37.35(19) . . . . ? B5 B1 B6 B11 -102.1(2) . . . . ? B4 B1 B6 B11 -63.2(2) . . . . ? B3 B1 B6 B11 -1.5(3) . . . . ? B1 B2 C7 B8 2.5(3) . . . . ? B3 B2 C7 B8 43.0(2) . . . . ? B6 B2 C7 B8 -61.0(2) . . . . ? B11 B2 C7 B8 -99.6(2) . . . . ? B1 B2 C7 B11 102.1(2) . . . . ? B3 B2 C7 B11 142.7(2) . . . . ? B6 B2 C7 B11 38.65(18) . . . . ? B1 B2 C7 B3 -40.57(19) . . . . ? B6 B2 C7 B3 -104.0(2) . . . . ? B11 B2 C7 B3 -142.7(2) . . . . ? B4 B3 C7 B8 -35.19(18) . . . . ? B2 B3 C7 B8 -136.7(2) . . . . ? B1 B3 C7 B8 -98.0(2) . . . . ? B4 B3 C7 B11 62.7(3) . . . . ? B2 B3 C7 B11 -38.9(2) . . . . ? B1 B3 C7 B11 -0.2(3) . . . . ? B8 B3 C7 B11 97.9(2) . . . . ? B4 B3 C7 B2 101.5(2) . . . . ? B1 B3 C7 B2 38.70(18) . . . . ? B8 B3 C7 B2 136.7(2) . . . . ? B11 C7 B8 C9 -16.0(3) . . . . ? B2 C7 B8 C9 55.4(3) . . . . ? B3 C7 B8 C9 97.1(2) . . . . ? B11 C7 B8 B4 -78.7(2) . . . . ? B2 C7 B8 B4 -7.4(3) . . . . ? B3 C7 B8 B4 34.34(18) . . . . ? B11 C7 B8 B3 -113.1(2) . . . . ? B2 C7 B8 B3 -41.75(19) . . . . ? C9 B4 B8 C7 106.2(2) . . . . ? B3 B4 B8 C7 -34.73(18) . . . . ? B5 B4 B8 C7 69.9(2) . . . . ? B1 B4 B8 C7 9.1(2) . . . . ? B3 B4 B8 C9 -140.9(2) . . . . ? B5 B4 B8 C9 -36.29(18) . . . . ? B1 B4 B8 C9 -97.1(2) . . . . ? C9 B4 B8 B3 140.9(2) . . . . ? B5 B4 B8 B3 104.6(2) . . . . ? B1 B4 B8 B3 43.79(18) . . . . ? B4 B3 B8 C7 140.7(2) . . . . ? B2 B3 B8 C7 36.44(18) . . . . ? B1 B3 B8 C7 97.0(2) . . . . ? C7 B3 B8 C9 -106.3(2) . . . . ? B4 B3 B8 C9 34.36(19) . . . . ? B2 B3 B8 C9 -69.8(2) . . . . ? B1 B3 B8 C9 -9.3(3) . . . . ? C7 B3 B8 B4 -140.7(2) . . . . ? B2 B3 B8 B4 -104.2(2) . . . . ? B1 B3 B8 B4 -43.66(18) . . . . ? C7 B8 C9 B10 15.9(3) . . . . ? B4 B8 C9 B10 113.0(2) . . . . ? B3 B8 C9 B10 79.0(2) . . . . ? C7 B8 C9 B5 -55.3(3) . . . . ? B4 B8 C9 B5 41.84(19) . . . . ? B3 B8 C9 B5 7.8(3) . . . . ? C7 B8 C9 B4 -97.1(2) . . . . ? B3 B8 C9 B4 -34.08(18) . . . . ? B1 B5 C9 B8 -2.7(3) . . . . ? B4 B5 C9 B8 -43.1(2) . . . . ? B6 B5 C9 B8 60.6(2) . . . . ? B10 B5 C9 B8 99.3(2) . . . . ? B1 B5 C9 B10 -102.1(2) . . . . ? B4 B5 C9 B10 -142.4(2) . . . . ? B6 B5 C9 B10 -38.72(17) . . . . ? B1 B5 C9 B4 40.33(19) . . . . ? B6 B5 C9 B4 103.7(2) . . . . ? B10 B5 C9 B4 142.4(2) . . . . ? B3 B4 C9 B8 35.00(18) . . . . ? B5 B4 C9 B8 136.9(2) . . . . ? B1 B4 C9 B8 98.1(2) . . . . ? B3 B4 C9 B10 -62.9(3) . . . . ? B5 B4 C9 B10 39.0(2) . . . . ? B1 B4 C9 B10 0.2(3) . . . . ? B8 B4 C9 B10 -97.9(2) . . . . ? B3 B4 C9 B5 -101.9(2) . . . . ? B1 B4 C9 B5 -38.80(19) . . . . ? B8 B4 C9 B5 -136.9(2) . . . . ? B8 C9 B10 B6 -70.7(2) . . . . ? B5 C9 B10 B6 38.51(18) . . . . ? B4 C9 B10 B6 0.7(3) . . . . ? B8 C9 B10 B5 -109.2(2) . . . . ? B4 C9 B10 B5 -37.8(2) . . . . ? B8 C9 B10 B11 -9.0(2) . . . . ? B5 C9 B10 B11 100.2(2) . . . . ? B4 C9 B10 B11 62.3(3) . . . . ? B5 B6 B10 C9 -37.78(17) . . . . ? B2 B6 B10 C9 60.3(2) . . . . ? B1 B6 B10 C9 -1.3(2) . . . . ? B11 B6 B10 C9 99.5(2) . . . . ? B2 B6 B10 B5 98.1(2) . . . . ? B1 B6 B10 B5 36.50(18) . . . . ? B11 B6 B10 B5 137.3(2) . . . . ? B5 B6 B10 B11 -137.3(2) . . . . ? B2 B6 B10 B11 -39.23(19) . . . . ? B1 B6 B10 B11 -100.8(2) . . . . ? B1 B5 B10 C9 97.4(2) . . . . ? B4 B5 B10 C9 32.94(18) . . . . ? B6 B5 B10 C9 135.45(19) . . . . ? C9 B5 B10 B6 -135.45(19) . . . . ? B1 B5 B10 B6 -38.06(18) . . . . ? B4 B5 B10 B6 -102.5(2) . . . . ? C9 B5 B10 B11 -97.9(2) . . . . ? B1 B5 B10 B11 -0.6(2) . . . . ? B4 B5 B10 B11 -65.0(2) . . . . ? B6 B5 B10 B11 37.50(18) . . . . ? B8 C7 B11 B6 70.5(2) . . . . ? B2 C7 B11 B6 -38.31(19) . . . . ? B3 C7 B11 B6 -0.8(3) . . . . ? B8 C7 B11 B2 108.8(2) . . . . ? B3 C7 B11 B2 37.5(2) . . . . ? B8 C7 B11 B10 9.2(3) . . . . ? B2 C7 B11 B10 -99.6(2) . . . . ? B3 C7 B11 B10 -62.1(3) . . . . ? B5 B6 B11 C7 -60.5(2) . . . . ? B2 B6 B11 C7 37.63(18) . . . . ? B1 B6 B11 C7 1.4(3) . . . . ? B10 B6 B11 C7 -99.1(2) . . . . ? B5 B6 B11 B2 -98.1(2) . . . . ? B1 B6 B11 B2 -36.23(18) . . . . ? B10 B6 B11 B2 -136.76(19) . . . . ? B5 B6 B11 B10 38.66(18) . . . . ? B2 B6 B11 B10 136.76(19) . . . . ? B1 B6 B11 B10 100.5(2) . . . . ? B1 B2 B11 C7 -97.6(2) . . . . ? B3 B2 B11 C7 -32.83(19) . . . . ? B6 B2 B11 C7 -135.5(2) . . . . ? C7 B2 B11 B6 135.5(2) . . . . ? B1 B2 B11 B6 37.91(19) . . . . ? B3 B2 B11 B6 102.7(2) . . . . ? C7 B2 B11 B10 97.8(2) . . . . ? B1 B2 B11 B10 0.2(3) . . . . ? B3 B2 B11 B10 65.0(2) . . . . ? B6 B2 B11 B10 -37.70(18) . . . . ? C9 B10 B11 C7 -0.1(3) . . . . ? B6 B10 B11 C7 97.7(2) . . . . ? B5 B10 B11 C7 60.3(2) . . . . ? C9 B10 B11 B6 -97.8(2) . . . . ? B5 B10 B11 B6 -37.46(18) . . . . ? C9 B10 B11 B2 -60.1(2) . . . . ? B6 B10 B11 B2 37.67(18) . . . . ? B5 B10 B11 B2 0.2(2) . . . . ? C21 C12 C13 C14 0.3(4) . . . . ? N26 C12 C13 C14 -178.8(2) . . . . ? C12 C13 C14 C15 -0.1(4) . . . . ? C13 C14 C15 C16 0.1(4) . . . . ? C14 C15 C16 C17 -179.9(2) . . . . ? C14 C15 C16 C21 -0.2(3) . . . . ? C15 C16 C17 C18 -178.9(2) . . . . ? C21 C16 C17 C18 1.5(3) . . . . ? C16 C17 C18 C19 -1.8(4) . . . . ? C17 C18 C19 C20 0.6(4) . . . . ? C18 C19 C20 C21 0.9(4) . . . . ? C18 C19 C20 N27 -178.4(2) . . . . ? C13 C12 C21 C16 -0.4(3) . . . . ? N26 C12 C21 C16 178.73(18) . . . . ? C13 C12 C21 C20 179.6(2) . . . . ? N26 C12 C21 C20 -1.3(3) . . . . ? C15 C16 C21 C12 0.4(3) . . . . ? C17 C16 C21 C12 -180.0(2) . . . . ? C15 C16 C21 C20 -179.6(2) . . . . ? C17 C16 C21 C20 0.0(3) . . . . ? C19 C20 C21 C12 178.8(2) . . . . ? N27 C20 C21 C12 -1.8(3) . . . . ? C19 C20 C21 C16 -1.2(3) . . . . ? N27 C20 C21 C16 178.16(18) . . . . ? C13 C12 N26 C24 -60.1(3) . . . . ? C21 C12 N26 C24 120.7(2) . . . . ? C13 C12 N26 C25 66.2(3) . . . . ? C21 C12 N26 C25 -113.0(2) . . . . ? C19 C20 N27 C22 62.2(3) . . . . ? C21 C20 N27 C22 -117.2(2) . . . . ? C19 C20 N27 C23 -63.0(3) . . . . ? C21 C20 N27 C23 117.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 30.46 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 0.637 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.105 #===END data_9 _database_code_CSD 171784 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H31 B9 N2' _chemical_formula_weight 348.72 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 triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.456(1) _cell_length_b 10.317(1) _cell_length_c 12.945(1) _cell_angle_alpha 68.443(3) _cell_angle_beta 84.683(3) _cell_angle_gamma 76.976(3) _cell_volume 1023.26(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 669 _cell_measurement_theta_min 13.66 _cell_measurement_theta_max 25.35 _exptl_crystal_description 'thin plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 372 _exptl_absorpt_coefficient_mu 0.059 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 'Bruker SMART-CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8405 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 23.25 _reflns_number_total 2946 _reflns_number_gt 2536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998a)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998a)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1 (Bruker, 1998c)' _computing_publication_material 'SHELXTL-NT V5.1 (Bruker, 1998c)' _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^)+(0.0474P)^2^+0.2666P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2946 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 B1 B -0.20626(19) -0.07338(18) 0.30733(14) 0.0281(4) Uani 1 1 d . . . H1 H -0.3063(18) 0.0132(16) 0.3104(12) 0.035(4) Uiso 1 1 d . . . C2 C -0.14266(16) -0.08384(15) 0.18003(12) 0.0278(3) Uani 1 1 d . . . H2 H -0.2019(19) -0.0068(18) 0.1159(13) 0.038(4) Uiso 1 1 d . . . B3 B -0.01609(19) -0.03429(18) 0.25144(14) 0.0272(4) Uani 1 1 d . . . H3 H -0.0044(18) 0.0757(17) 0.2185(12) 0.036(4) Uiso 1 1 d . . . B4 B -0.02743(19) -0.14409(18) 0.38902(13) 0.0277(4) Uani 1 1 d . . . H4 H -0.0095(17) -0.1184(16) 0.4630(12) 0.036(4) Uiso 1 1 d . . . B5 B -0.17045(19) -0.25314(18) 0.39934(13) 0.0281(4) Uani 1 1 d . . . H5 H -0.2400(18) -0.2919(16) 0.4766(12) 0.035(4) Uiso 1 1 d . . . B6 B -0.24713(19) -0.21041(18) 0.26863(14) 0.0284(4) Uani 1 1 d . . . H6 H -0.3742(18) -0.2017(16) 0.2454(12) 0.036(4) Uiso 1 1 d . . . B7 B 0.06189(19) -0.13572(19) 0.16475(14) 0.0299(4) Uani 1 1 d . . . H7 H 0.1115(17) -0.0793(16) 0.0847(13) 0.036(4) Uiso 1 1 d . . . B8 B 0.13343(18) -0.18964(18) 0.30166(13) 0.0271(4) Uani 1 1 d . . . H8 H 0.2587(18) -0.1903(16) 0.3218(12) 0.034(4) Uiso 1 1 d . . . C9 C 0.03369(17) -0.31088(15) 0.38111(12) 0.0273(3) Uani 1 1 d . . . H9 H 0.0878(18) -0.3827(17) 0.4486(13) 0.035(4) Uiso 1 1 d . . . B10 B -0.0895(2) -0.36011(18) 0.31858(14) 0.0297(4) Uani 1 1 d . . . H10 H -0.1124(18) -0.4717(17) 0.3525(13) 0.041(4) Uiso 1 1 d . . . B11 B -0.0877(2) -0.25196(19) 0.17642(14) 0.0311(4) Uani 1 1 d . . . H11 H -0.1211(17) -0.2623(16) 0.1006(13) 0.036(4) Uiso 1 1 d . . . H12 H 0.063(2) -0.2688(18) 0.1869(13) 0.049(5) Uiso 1 1 d . . . C12 C 0.40026(15) 0.22720(14) 0.19359(11) 0.0224(3) Uani 1 1 d . . . C13 C 0.35324(17) 0.15985(15) 0.13201(12) 0.0284(3) Uani 1 1 d . . . H13 H 0.2668(19) 0.1091(17) 0.1575(12) 0.034(4) Uiso 1 1 d . . . C14 C 0.43124(17) 0.16506(16) 0.03000(12) 0.0303(3) Uani 1 1 d . . . H14 H 0.3946(18) 0.1195(16) -0.0150(12) 0.034(4) Uiso 1 1 d . . . C15 C 0.55357(17) 0.23778(15) -0.00793(12) 0.0288(3) Uani 1 1 d . . . H15 H 0.6054(18) 0.2421(16) -0.0768(14) 0.036(4) Uiso 1 1 d . . . C16 C 0.60576(15) 0.30848(14) 0.05390(11) 0.0250(3) Uani 1 1 d . . . C17 C 0.73270(17) 0.38472(16) 0.01413(12) 0.0311(4) Uani 1 1 d . . . H17 H 0.7841(18) 0.3855(16) -0.0565(13) 0.034(4) Uiso 1 1 d . . . C18 C 0.78076(18) 0.45511(16) 0.07261(13) 0.0337(4) Uani 1 1 d . . . H18 H 0.865(2) 0.5114(18) 0.0450(13) 0.042(4) Uiso 1 1 d . . . C19 C 0.70792(17) 0.44915(16) 0.17613(12) 0.0299(3) Uani 1 1 d . . . H19 H 0.7446(18) 0.4962(16) 0.2165(12) 0.033(4) Uiso 1 1 d . . . C20 C 0.58732(15) 0.37487(14) 0.21881(11) 0.0229(3) Uani 1 1 d . . . C21 C 0.52870(15) 0.30382(14) 0.15833(10) 0.0222(3) Uani 1 1 d . . . C22 C 0.6363(2) 0.28308(19) 0.41859(13) 0.0377(4) Uani 1 1 d . . . H22A H 0.723(2) 0.3373(18) 0.4134(13) 0.045(5) Uiso 1 1 d . . . H22B H 0.5783(19) 0.2644(17) 0.4925(14) 0.042(4) Uiso 1 1 d . . . H22C H 0.688(2) 0.189(2) 0.4101(14) 0.048(5) Uiso 1 1 d . . . C23 C 0.4382(2) 0.50446(17) 0.33564(14) 0.0370(4) Uani 1 1 d . . . H23A H 0.354(2) 0.5523(18) 0.2755(14) 0.045(5) Uiso 1 1 d . . . H23B H 0.3870(19) 0.4867(17) 0.4098(14) 0.040(4) Uiso 1 1 d . . . H23C H 0.520(2) 0.5624(19) 0.3275(13) 0.048(5) Uiso 1 1 d . . . C24 C 0.32313(19) 0.07589(15) 0.38099(12) 0.0283(3) Uani 1 1 d . . . H24A H 0.2824(19) 0.0838(17) 0.4531(14) 0.042(4) Uiso 1 1 d . . . H24B H 0.2553(19) 0.0275(17) 0.3552(12) 0.037(4) Uiso 1 1 d . . . H24C H 0.436(2) 0.0237(17) 0.3886(12) 0.037(4) Uiso 1 1 d . . . C25 C 0.14621(18) 0.30761(18) 0.28258(14) 0.0324(4) Uani 1 1 d . . . H25A H 0.1486(18) 0.4066(19) 0.2309(14) 0.041(4) Uiso 1 1 d . . . H25B H 0.1014(18) 0.3051(17) 0.3567(14) 0.040(4) Uiso 1 1 d . . . H25C H 0.081(2) 0.2629(18) 0.2499(13) 0.044(4) Uiso 1 1 d . . . N26 N 0.31671(13) 0.22352(12) 0.29973(9) 0.0238(3) Uani 1 1 d . . . H26 H 0.399(2) 0.284(2) 0.3311(15) 0.062(5) Uiso 1 1 d . . . N27 N 0.51613(13) 0.36358(12) 0.32896(9) 0.0256(3) 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 B1 0.0236(8) 0.0268(9) 0.0345(9) -0.0136(8) 0.0041(7) -0.0037(7) C2 0.0256(7) 0.0275(8) 0.0254(8) -0.0049(7) -0.0026(6) -0.0027(6) B3 0.0249(8) 0.0231(9) 0.0331(9) -0.0096(7) 0.0027(7) -0.0060(7) B4 0.0287(9) 0.0302(9) 0.0287(9) -0.0151(7) 0.0027(7) -0.0084(7) B5 0.0303(9) 0.0292(9) 0.0261(9) -0.0100(7) 0.0037(7) -0.0102(7) B6 0.0256(8) 0.0287(9) 0.0312(9) -0.0098(7) -0.0010(7) -0.0071(7) B7 0.0269(9) 0.0352(10) 0.0257(9) -0.0105(8) 0.0042(7) -0.0047(7) B8 0.0220(8) 0.0302(9) 0.0304(9) -0.0137(7) 0.0003(7) -0.0030(7) C9 0.0301(8) 0.0245(8) 0.0244(8) -0.0063(6) -0.0048(6) -0.0024(6) B10 0.0343(9) 0.0236(9) 0.0324(9) -0.0106(8) -0.0043(7) -0.0057(7) B11 0.0320(9) 0.0351(10) 0.0294(9) -0.0161(8) -0.0040(7) -0.0037(7) C12 0.0226(7) 0.0205(7) 0.0221(7) -0.0070(6) -0.0018(5) -0.0008(6) C13 0.0276(8) 0.0277(8) 0.0317(8) -0.0122(7) -0.0030(6) -0.0054(6) C14 0.0329(8) 0.0305(8) 0.0302(8) -0.0161(7) -0.0069(6) -0.0001(7) C15 0.0305(8) 0.0297(8) 0.0221(8) -0.0106(6) -0.0020(6) 0.0046(6) C16 0.0234(7) 0.0211(7) 0.0250(7) -0.0063(6) -0.0010(6) 0.0030(6) C17 0.0283(8) 0.0304(8) 0.0286(8) -0.0078(7) 0.0058(6) -0.0015(6) C18 0.0255(8) 0.0328(9) 0.0409(9) -0.0109(7) 0.0064(6) -0.0088(7) C19 0.0268(7) 0.0280(8) 0.0359(8) -0.0119(7) -0.0020(6) -0.0066(6) C20 0.0225(7) 0.0190(7) 0.0241(7) -0.0061(6) -0.0022(5) -0.0002(6) C21 0.0211(7) 0.0187(7) 0.0227(7) -0.0052(6) -0.0035(5) 0.0016(5) C22 0.0453(10) 0.0380(10) 0.0291(9) -0.0072(7) -0.0103(7) -0.0117(8) C23 0.0481(10) 0.0278(9) 0.0378(10) -0.0165(8) 0.0102(8) -0.0090(8) C24 0.0304(8) 0.0241(8) 0.0286(8) -0.0073(7) 0.0031(6) -0.0068(7) C25 0.0285(8) 0.0320(9) 0.0341(9) -0.0128(8) 0.0019(7) -0.0001(7) N26 0.0238(6) 0.0233(6) 0.0239(6) -0.0089(5) 0.0021(5) -0.0043(5) N27 0.0316(6) 0.0234(6) 0.0227(6) -0.0090(5) -0.0009(5) -0.0062(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 B1 C2 1.720(2) . ? B1 B3 1.770(2) . ? B1 B5 1.772(2) . ? B1 B6 1.773(2) . ? B1 B4 1.780(2) . ? B1 H1 1.092(15) . ? C2 B7 1.707(2) . ? C2 B11 1.708(2) . ? C2 B6 1.741(2) . ? C2 B3 1.743(2) . ? C2 H2 0.992(17) . ? B3 B4 1.732(2) . ? B3 B8 1.750(2) . ? B3 B7 1.790(2) . ? B3 H3 1.080(16) . ? B4 C9 1.720(2) . ? B4 B8 1.780(2) . ? B4 B5 1.794(2) . ? B4 H4 1.115(15) . ? B5 C9 1.719(2) . ? B5 B6 1.733(2) . ? B5 B10 1.776(2) . ? B5 H5 1.100(15) . ? B6 B10 1.754(2) . ? B6 B11 1.801(2) . ? B6 H6 1.118(15) . ? B7 B8 1.772(2) . ? B7 B11 1.891(2) . ? B7 H7 1.084(15) . ? B7 H12 1.293(17) . ? B8 C9 1.644(2) . ? B8 H8 1.112(14) . ? C9 B10 1.642(2) . ? C9 H9 0.983(16) . ? B10 B11 1.768(2) . ? B10 H10 1.126(16) . ? B11 H11 1.094(15) . ? B11 H12 1.261(16) . ? C12 C13 1.3663(19) . ? C12 C21 1.4293(19) . ? C12 N26 1.4772(16) . ? C13 C14 1.409(2) . ? C13 H13 0.958(16) . ? C14 C15 1.363(2) . ? C14 H14 0.978(16) . ? C15 C16 1.417(2) . ? C15 H15 0.947(16) . ? C16 C17 1.420(2) . ? C16 C21 1.4345(18) . ? C17 C18 1.364(2) . ? C17 H17 0.973(16) . ? C18 C19 1.408(2) . ? C18 H18 0.979(17) . ? C19 C20 1.367(2) . ? C19 H19 0.943(16) . ? C20 C21 1.4330(18) . ? C20 N27 1.4695(17) . ? C22 N27 1.4829(19) . ? C22 H22A 1.001(18) . ? C22 H22B 1.007(17) . ? C22 H22C 1.009(18) . ? C23 N27 1.4847(19) . ? C23 H23A 1.009(17) . ? C23 H23B 0.985(17) . ? C23 H23C 0.987(18) . ? C24 N26 1.4918(18) . ? C24 H24A 0.990(17) . ? C24 H24B 0.988(17) . ? C24 H24C 0.975(17) . ? C25 N26 1.4948(18) . ? C25 H25A 0.998(17) . ? C25 H25B 0.992(16) . ? C25 H25C 0.998(17) . ? N26 H26 1.212(18) . ? N27 H26 1.415(18) . ? 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 C2 B1 B3 59.91(9) . . ? C2 B1 B5 104.11(11) . . ? B3 B1 B5 107.45(11) . . ? C2 B1 B6 59.80(9) . . ? B3 B1 B6 109.69(11) . . ? B5 B1 B6 58.55(9) . . ? C2 B1 B4 104.27(10) . . ? B3 B1 B4 58.38(9) . . ? B5 B1 B4 60.67(9) . . ? B6 B1 B4 107.81(11) . . ? C2 B1 H1 118.6(8) . . ? B3 B1 H1 119.4(8) . . ? B5 B1 H1 127.5(8) . . ? B6 B1 H1 118.9(7) . . ? B4 B1 H1 127.6(7) . . ? B7 C2 B11 67.23(10) . . ? B7 C2 B1 115.52(11) . . ? B11 C2 B1 115.64(11) . . ? B7 C2 B6 117.85(11) . . ? B11 C2 B6 62.93(9) . . ? B1 C2 B6 61.61(9) . . ? B7 C2 B3 62.49(9) . . ? B11 C2 B3 117.16(11) . . ? B1 C2 B3 61.49(9) . . ? B6 C2 B3 112.46(11) . . ? B7 C2 H2 117.3(9) . . ? B11 C2 H2 118.6(9) . . ? B1 C2 H2 114.5(9) . . ? B6 C2 H2 118.0(9) . . ? B3 C2 H2 116.6(9) . . ? B4 B3 C2 105.33(11) . . ? B4 B3 B8 61.47(9) . . ? C2 B3 B8 102.19(11) . . ? B4 B3 B1 61.09(9) . . ? C2 B3 B1 58.60(8) . . ? B8 B3 B1 108.53(12) . . ? B4 B3 B7 111.20(12) . . ? C2 B3 B7 57.77(8) . . ? B8 B3 B7 60.05(9) . . ? B1 B3 B7 108.99(11) . . ? B4 B3 H3 128.5(8) . . ? C2 B3 H3 116.8(8) . . ? B8 B3 H3 129.6(8) . . ? B1 B3 H3 118.4(8) . . ? B7 B3 H3 115.7(8) . . ? C9 B4 B3 102.13(11) . . ? C9 B4 B8 56.01(9) . . ? B3 B4 B8 59.78(9) . . ? C9 B4 B1 102.31(11) . . ? B3 B4 B1 60.52(9) . . ? B8 B4 B1 106.80(11) . . ? C9 B4 B5 58.53(9) . . ? B3 B4 B5 108.17(11) . . ? B8 B4 B5 106.30(11) . . ? B1 B4 B5 59.44(9) . . ? C9 B4 H4 124.1(8) . . ? B3 B4 H4 126.1(8) . . ? B8 B4 H4 123.9(7) . . ? B1 B4 H4 124.0(8) . . ? B5 B4 H4 118.5(8) . . ? C9 B5 B6 102.57(11) . . ? C9 B5 B1 102.67(11) . . ? B6 B5 B1 60.74(9) . . ? C9 B5 B10 56.01(8) . . ? B6 B5 B10 59.98(9) . . ? B1 B5 B10 107.06(11) . . ? C9 B5 B4 58.57(8) . . ? B6 B5 B4 108.93(11) . . ? B1 B5 B4 59.89(9) . . ? B10 B5 B4 106.50(11) . . ? C9 B5 H5 125.6(8) . . ? B6 B5 H5 123.3(8) . . ? B1 B5 H5 123.6(8) . . ? B10 B5 H5 122.7(8) . . ? B4 B5 H5 120.4(8) . . ? B5 B6 C2 104.85(11) . . ? B5 B6 B10 61.22(9) . . ? C2 B6 B10 101.79(11) . . ? B5 B6 B1 60.71(9) . . ? C2 B6 B1 58.59(9) . . ? B10 B6 B1 107.99(11) . . ? B5 B6 B11 110.37(11) . . ? C2 B6 B11 57.64(9) . . ? B10 B6 B11 59.62(9) . . ? B1 B6 B11 108.57(11) . . ? B5 B6 H6 128.5(7) . . ? C2 B6 H6 116.8(8) . . ? B10 B6 H6 130.5(8) . . ? B1 B6 H6 118.0(8) . . ? B11 B6 H6 116.8(7) . . ? C2 B7 B8 102.77(11) . . ? C2 B7 B3 59.74(9) . . ? B8 B7 B3 58.86(9) . . ? C2 B7 B11 56.42(8) . . ? B8 B7 B11 104.63(11) . . ? B3 B7 B11 106.28(10) . . ? C2 B7 H7 115.0(8) . . ? B8 B7 H7 131.8(8) . . ? B3 B7 H7 116.6(8) . . ? B11 B7 H7 120.7(8) . . ? C2 B7 H12 96.5(7) . . ? B8 B7 H12 86.1(7) . . ? B3 B7 H12 126.8(7) . . ? B11 B7 H12 41.6(7) . . ? H7 B7 H12 116.6(11) . . ? C9 B8 B3 104.50(11) . . ? C9 B8 B7 106.72(11) . . ? B3 B8 B7 61.09(9) . . ? C9 B8 B4 60.15(9) . . ? B3 B8 B4 58.75(9) . . ? B7 B8 B4 109.83(11) . . ? C9 B8 H8 121.5(8) . . ? B3 B8 H8 123.5(8) . . ? B7 B8 H8 124.1(7) . . ? B4 B8 H8 117.5(7) . . ? B10 C9 B8 116.77(12) . . ? B10 C9 B5 63.75(9) . . ? B8 C9 B5 116.49(11) . . ? B10 C9 B4 116.62(11) . . ? B8 C9 B4 63.84(9) . . ? B5 C9 B4 62.90(9) . . ? B10 C9 H9 117.6(9) . . ? B8 C9 H9 117.4(9) . . ? B5 C9 H9 113.7(9) . . ? B4 C9 H9 113.4(9) . . ? C9 B10 B6 104.91(11) . . ? C9 B10 B11 106.63(12) . . ? B6 B10 B11 61.50(9) . . ? C9 B10 B5 60.24(9) . . ? B6 B10 B5 58.80(9) . . ? B11 B10 B5 109.94(12) . . ? C9 B10 H10 121.1(8) . . ? B6 B10 H10 121.9(8) . . ? B11 B10 H10 125.5(8) . . ? B5 B10 H10 115.5(8) . . ? C2 B11 B10 102.57(11) . . ? C2 B11 B6 59.43(9) . . ? B10 B11 B6 58.88(9) . . ? C2 B11 B7 56.35(8) . . ? B10 B11 B7 105.08(11) . . ? B6 B11 B7 106.25(11) . . ? C2 B11 H11 114.9(8) . . ? B10 B11 H11 133.4(8) . . ? B6 B11 H11 118.5(8) . . ? B7 B11 H11 118.3(8) . . ? C2 B11 H12 97.7(8) . . ? B10 B11 H12 86.2(7) . . ? B6 B11 H12 127.6(7) . . ? B7 B11 H12 42.9(8) . . ? H11 B11 H12 113.8(11) . . ? C13 C12 C21 122.06(12) . . ? C13 C12 N26 120.10(12) . . ? C21 C12 N26 117.84(11) . . ? C12 C13 C14 120.14(14) . . ? C12 C13 H13 120.4(9) . . ? C14 C13 H13 119.4(9) . . ? C15 C14 C13 120.16(13) . . ? C15 C14 H14 120.0(9) . . ? C13 C14 H14 119.8(9) . . ? C14 C15 C16 121.22(13) . . ? C14 C15 H15 120.2(9) . . ? C16 C15 H15 118.5(9) . . ? C15 C16 C17 121.19(13) . . ? C15 C16 C21 119.56(12) . . ? C17 C16 C21 119.24(12) . . ? C18 C17 C16 121.18(13) . . ? C18 C17 H17 121.0(9) . . ? C16 C17 H17 117.8(9) . . ? C17 C18 C19 120.03(14) . . ? C17 C18 H18 122.2(9) . . ? C19 C18 H18 117.7(9) . . ? C20 C19 C18 120.89(14) . . ? C20 C19 H19 120.1(9) . . ? C18 C19 H19 119.0(9) . . ? C19 C20 C21 121.00(12) . . ? C19 C20 N27 120.88(12) . . ? C21 C20 N27 118.11(11) . . ? C12 C21 C20 125.54(12) . . ? C12 C21 C16 116.86(12) . . ? C20 C21 C16 117.60(12) . . ? N27 C22 H22A 110.7(10) . . ? N27 C22 H22B 108.8(9) . . ? H22A C22 H22B 110.7(13) . . ? N27 C22 H22C 108.6(9) . . ? H22A C22 H22C 108.8(13) . . ? H22B C22 H22C 109.2(13) . . ? N27 C23 H23A 107.6(9) . . ? N27 C23 H23B 107.2(9) . . ? H23A C23 H23B 110.8(13) . . ? N27 C23 H23C 110.6(10) . . ? H23A C23 H23C 111.7(14) . . ? H23B C23 H23C 108.8(13) . . ? N26 C24 H24A 107.3(9) . . ? N26 C24 H24B 110.1(9) . . ? H24A C24 H24B 110.8(12) . . ? N26 C24 H24C 109.0(9) . . ? H24A C24 H24C 109.6(13) . . ? H24B C24 H24C 110.2(12) . . ? N26 C25 H25A 108.4(9) . . ? N26 C25 H25B 107.0(9) . . ? H25A C25 H25B 112.1(13) . . ? N26 C25 H25C 109.6(9) . . ? H25A C25 H25C 109.9(13) . . ? H25B C25 H25C 109.9(13) . . ? C12 N26 C24 113.00(10) . . ? C12 N26 C25 111.99(10) . . ? C24 N26 C25 111.29(11) . . ? C12 N26 H26 99.8(8) . . ? C24 N26 H26 110.4(9) . . ? C25 N26 H26 109.8(9) . . ? C20 N27 C22 111.82(11) . . ? C20 N27 C23 112.55(11) . . ? C22 N27 C23 111.02(12) . . ? C20 N27 H26 98.3(7) . . ? C22 N27 H26 111.1(7) . . ? C23 N27 H26 111.4(7) . . ? 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 B3 B1 C2 B7 32.67(12) . . . . ? B5 B1 C2 B7 -69.55(14) . . . . ? B6 B1 C2 B7 -109.29(13) . . . . ? B4 B1 C2 B7 -6.76(15) . . . . ? B3 B1 C2 B11 108.39(13) . . . . ? B5 B1 C2 B11 6.18(15) . . . . ? B6 B1 C2 B11 -33.57(11) . . . . ? B4 B1 C2 B11 68.97(14) . . . . ? B3 B1 C2 B6 141.96(12) . . . . ? B5 B1 C2 B6 39.75(10) . . . . ? B4 B1 C2 B6 102.54(12) . . . . ? B5 B1 C2 B3 -102.22(12) . . . . ? B6 B1 C2 B3 -141.96(12) . . . . ? B4 B1 C2 B3 -39.43(10) . . . . ? B7 C2 B3 B4 -105.69(12) . . . . ? B11 C2 B3 B4 -64.95(14) . . . . ? B1 C2 B3 B4 41.00(10) . . . . ? B6 C2 B3 B4 5.09(15) . . . . ? B7 C2 B3 B8 -42.26(10) . . . . ? B11 C2 B3 B8 -1.53(15) . . . . ? B1 C2 B3 B8 104.43(12) . . . . ? B6 C2 B3 B8 68.51(13) . . . . ? B7 C2 B3 B1 -146.69(12) . . . . ? B11 C2 B3 B1 -105.95(13) . . . . ? B6 C2 B3 B1 -35.91(11) . . . . ? B11 C2 B3 B7 40.74(12) . . . . ? B1 C2 B3 B7 146.69(12) . . . . ? B6 C2 B3 B7 110.78(13) . . . . ? C2 B1 B3 B4 -133.71(12) . . . . ? B5 B1 B3 B4 -37.21(11) . . . . ? B6 B1 B3 B4 -99.27(13) . . . . ? B5 B1 B3 C2 96.51(12) . . . . ? B6 B1 B3 C2 34.44(11) . . . . ? B4 B1 B3 C2 133.71(12) . . . . ? C2 B1 B3 B8 -93.23(12) . . . . ? B5 B1 B3 B8 3.28(15) . . . . ? B6 B1 B3 B8 -58.78(15) . . . . ? B4 B1 B3 B8 40.49(11) . . . . ? C2 B1 B3 B7 -29.43(11) . . . . ? B5 B1 B3 B7 67.08(14) . . . . ? B6 B1 B3 B7 5.01(16) . . . . ? B4 B1 B3 B7 104.29(13) . . . . ? C2 B3 B4 C9 57.65(12) . . . . ? B8 B3 B4 C9 -38.10(10) . . . . ? B1 B3 B4 C9 97.41(11) . . . . ? B7 B3 B4 C9 -3.22(14) . . . . ? C2 B3 B4 B8 95.75(11) . . . . ? B1 B3 B4 B8 135.52(12) . . . . ? B7 B3 B4 B8 34.88(11) . . . . ? C2 B3 B4 B1 -39.77(10) . . . . ? B8 B3 B4 B1 -135.52(12) . . . . ? B7 B3 B4 B1 -100.64(12) . . . . ? C2 B3 B4 B5 -2.92(14) . . . . ? B8 B3 B4 B5 -98.67(12) . . . . ? B1 B3 B4 B5 36.85(11) . . . . ? B7 B3 B4 B5 -63.79(14) . . . . ? C2 B1 B4 C9 -56.91(13) . . . . ? B3 B1 B4 C9 -97.10(11) . . . . ? B5 B1 B4 C9 41.47(10) . . . . ? B6 B1 B4 C9 5.47(14) . . . . ? C2 B1 B4 B3 40.19(10) . . . . ? B5 B1 B4 B3 138.57(12) . . . . ? B6 B1 B4 B3 102.58(12) . . . . ? C2 B1 B4 B8 0.96(14) . . . . ? B3 B1 B4 B8 -39.23(11) . . . . ? B5 B1 B4 B8 99.34(12) . . . . ? B6 B1 B4 B8 63.35(14) . . . . ? C2 B1 B4 B5 -98.38(12) . . . . ? B3 B1 B4 B5 -138.57(12) . . . . ? B6 B1 B4 B5 -35.99(10) . . . . ? C2 B1 B5 C9 57.08(12) . . . . ? B3 B1 B5 C9 -5.36(14) . . . . ? B6 B1 B5 C9 97.45(11) . . . . ? B4 B1 B5 C9 -41.56(10) . . . . ? C2 B1 B5 B6 -40.38(10) . . . . ? B3 B1 B5 B6 -102.81(12) . . . . ? B4 B1 B5 B6 -139.01(11) . . . . ? C2 B1 B5 B10 -0.89(14) . . . . ? B3 B1 B5 B10 -63.33(14) . . . . ? B6 B1 B5 B10 39.48(10) . . . . ? B4 B1 B5 B10 -99.53(12) . . . . ? C2 B1 B5 B4 98.64(11) . . . . ? B3 B1 B5 B4 36.20(10) . . . . ? B6 B1 B5 B4 139.01(11) . . . . ? B3 B4 B5 C9 93.34(12) . . . . ? B8 B4 B5 C9 30.47(10) . . . . ? B1 B4 B5 C9 130.67(11) . . . . ? C9 B4 B5 B6 -93.44(12) . . . . ? B3 B4 B5 B6 -0.10(15) . . . . ? B8 B4 B5 B6 -62.97(14) . . . . ? B1 B4 B5 B6 37.22(11) . . . . ? C9 B4 B5 B1 -130.67(11) . . . . ? B3 B4 B5 B1 -37.32(11) . . . . ? B8 B4 B5 B1 -100.19(12) . . . . ? C9 B4 B5 B10 -30.19(10) . . . . ? B3 B4 B5 B10 63.15(14) . . . . ? B8 B4 B5 B10 0.28(14) . . . . ? B1 B4 B5 B10 100.48(12) . . . . ? C9 B5 B6 C2 -57.70(13) . . . . ? B1 B5 B6 C2 39.93(10) . . . . ? B10 B5 B6 C2 -95.48(12) . . . . ? B4 B5 B6 C2 3.07(15) . . . . ? C9 B5 B6 B10 37.78(10) . . . . ? B1 B5 B6 B10 135.41(11) . . . . ? B4 B5 B6 B10 98.55(12) . . . . ? C9 B5 B6 B1 -97.63(11) . . . . ? B10 B5 B6 B1 -135.41(11) . . . . ? B4 B5 B6 B1 -36.86(10) . . . . ? C9 B5 B6 B11 2.81(14) . . . . ? B1 B5 B6 B11 100.44(12) . . . . ? B10 B5 B6 B11 -34.97(11) . . . . ? B4 B5 B6 B11 63.58(15) . . . . ? B7 C2 B6 B5 64.58(15) . . . . ? B11 C2 B6 B5 104.97(12) . . . . ? B1 C2 B6 B5 -40.99(10) . . . . ? B3 C2 B6 B5 -5.12(15) . . . . ? B7 C2 B6 B10 1.55(15) . . . . ? B11 C2 B6 B10 41.94(10) . . . . ? B1 C2 B6 B10 -104.02(11) . . . . ? B3 C2 B6 B10 -68.16(13) . . . . ? B7 C2 B6 B1 105.57(13) . . . . ? B11 C2 B6 B1 145.96(12) . . . . ? B3 C2 B6 B1 35.86(11) . . . . ? B7 C2 B6 B11 -40.39(12) . . . . ? B1 C2 B6 B11 -145.96(12) . . . . ? B3 C2 B6 B11 -110.09(12) . . . . ? C2 B1 B6 B5 133.37(11) . . . . ? B3 B1 B6 B5 98.89(13) . . . . ? B4 B1 B6 B5 36.91(10) . . . . ? B3 B1 B6 C2 -34.49(11) . . . . ? B5 B1 B6 C2 -133.37(11) . . . . ? B4 B1 B6 C2 -96.46(11) . . . . ? C2 B1 B6 B10 93.06(12) . . . . ? B3 B1 B6 B10 58.57(15) . . . . ? B5 B1 B6 B10 -40.31(11) . . . . ? B4 B1 B6 B10 -3.40(15) . . . . ? C2 B1 B6 B11 29.92(10) . . . . ? B3 B1 B6 B11 -4.56(16) . . . . ? B5 B1 B6 B11 -103.45(12) . . . . ? B4 B1 B6 B11 -66.54(14) . . . . ? B11 C2 B7 B8 -99.23(12) . . . . ? B1 C2 B7 B8 9.42(15) . . . . ? B6 C2 B7 B8 -60.49(15) . . . . ? B3 C2 B7 B8 41.75(10) . . . . ? B11 C2 B7 B3 -140.97(12) . . . . ? B1 C2 B7 B3 -32.33(12) . . . . ? B6 C2 B7 B3 -102.23(13) . . . . ? B1 C2 B7 B11 108.64(13) . . . . ? B6 C2 B7 B11 38.74(11) . . . . ? B3 C2 B7 B11 140.97(12) . . . . ? B4 B3 B7 C2 95.21(12) . . . . ? B8 B3 B7 C2 130.65(11) . . . . ? B1 B3 B7 C2 29.72(11) . . . . ? B4 B3 B7 B8 -35.44(11) . . . . ? C2 B3 B7 B8 -130.65(11) . . . . ? B1 B3 B7 B8 -100.93(13) . . . . ? B4 B3 B7 B11 62.08(14) . . . . ? C2 B3 B7 B11 -33.13(10) . . . . ? B8 B3 B7 B11 97.53(12) . . . . ? B1 B3 B7 B11 -3.41(15) . . . . ? B4 B3 B8 C9 40.68(10) . . . . ? C2 B3 B8 C9 -60.30(12) . . . . ? B1 B3 B8 C9 0.37(14) . . . . ? B7 B3 B8 C9 -101.34(12) . . . . ? B4 B3 B8 B7 142.02(12) . . . . ? C2 B3 B8 B7 41.04(10) . . . . ? B1 B3 B8 B7 101.71(12) . . . . ? C2 B3 B8 B4 -100.98(11) . . . . ? B1 B3 B8 B4 -40.31(11) . . . . ? B7 B3 B8 B4 -142.02(12) . . . . ? C2 B7 B8 C9 55.42(14) . . . . ? B3 B7 B8 C9 97.63(12) . . . . ? B11 B7 B8 C9 -2.78(14) . . . . ? C2 B7 B8 B3 -42.22(10) . . . . ? B11 B7 B8 B3 -100.41(11) . . . . ? C2 B7 B8 B4 -8.21(15) . . . . ? B3 B7 B8 B4 34.00(11) . . . . ? B11 B7 B8 B4 -66.41(14) . . . . ? B3 B4 B8 C9 -133.31(11) . . . . ? B1 B4 B8 C9 -93.73(12) . . . . ? B5 B4 B8 C9 -31.44(10) . . . . ? C9 B4 B8 B3 133.31(11) . . . . ? B1 B4 B8 B3 39.58(11) . . . . ? B5 B4 B8 B3 101.87(12) . . . . ? C9 B4 B8 B7 98.38(12) . . . . ? B3 B4 B8 B7 -34.93(11) . . . . ? B1 B4 B8 B7 4.65(15) . . . . ? B5 B4 B8 B7 66.94(14) . . . . ? B3 B8 C9 B10 68.16(14) . . . . ? B7 B8 C9 B10 4.50(16) . . . . ? B4 B8 C9 B10 108.14(13) . . . . ? B3 B8 C9 B5 -4.26(15) . . . . ? B7 B8 C9 B5 -67.92(14) . . . . ? B4 B8 C9 B5 35.72(11) . . . . ? B3 B8 C9 B4 -39.98(10) . . . . ? B7 B8 C9 B4 -103.64(12) . . . . ? B6 B5 C9 B10 -39.77(11) . . . . ? B1 B5 C9 B10 -102.18(12) . . . . ? B4 B5 C9 B10 -144.44(12) . . . . ? B6 B5 C9 B8 68.61(14) . . . . ? B1 B5 C9 B8 6.20(15) . . . . ? B10 B5 C9 B8 108.38(13) . . . . ? B4 B5 C9 B8 -36.06(11) . . . . ? B6 B5 C9 B4 104.67(12) . . . . ? B1 B5 C9 B4 42.26(10) . . . . ? B10 B5 C9 B4 144.44(12) . . . . ? B3 B4 C9 B10 -68.35(14) . . . . ? B8 B4 C9 B10 -108.37(13) . . . . ? B1 B4 C9 B10 -6.27(15) . . . . ? B5 B4 C9 B10 35.69(12) . . . . ? B3 B4 C9 B8 40.02(10) . . . . ? B1 B4 C9 B8 102.10(11) . . . . ? B5 B4 C9 B8 144.06(11) . . . . ? B3 B4 C9 B5 -104.04(11) . . . . ? B8 B4 C9 B5 -144.06(11) . . . . ? B1 B4 C9 B5 -41.96(10) . . . . ? B8 C9 B10 B6 -68.28(15) . . . . ? B5 C9 B10 B6 39.67(10) . . . . ? B4 C9 B10 B6 4.29(16) . . . . ? B8 C9 B10 B11 -4.12(16) . . . . ? B5 C9 B10 B11 103.84(12) . . . . ? B4 C9 B10 B11 68.45(15) . . . . ? B8 C9 B10 B5 -107.95(13) . . . . ? B4 C9 B10 B5 -35.38(12) . . . . ? B5 B6 B10 C9 -40.38(10) . . . . ? C2 B6 B10 C9 60.22(13) . . . . ? B1 B6 B10 C9 -0.30(15) . . . . ? B11 B6 B10 C9 101.10(12) . . . . ? B5 B6 B10 B11 -141.48(12) . . . . ? C2 B6 B10 B11 -40.88(10) . . . . ? B1 B6 B10 B11 -101.40(12) . . . . ? C2 B6 B10 B5 100.60(11) . . . . ? B1 B6 B10 B5 40.08(11) . . . . ? B11 B6 B10 B5 141.48(12) . . . . ? B6 B5 B10 C9 133.85(12) . . . . ? B1 B5 B10 C9 94.01(12) . . . . ? B4 B5 B10 C9 31.16(11) . . . . ? C9 B5 B10 B6 -133.85(12) . . . . ? B1 B5 B10 B6 -39.84(11) . . . . ? B4 B5 B10 B6 -102.68(12) . . . . ? C9 B5 B10 B11 -98.24(13) . . . . ? B6 B5 B10 B11 35.61(11) . . . . ? B1 B5 B10 B11 -4.23(15) . . . . ? B4 B5 B10 B11 -67.08(14) . . . . ? B7 C2 B11 B10 99.89(11) . . . . ? B1 C2 B11 B10 -8.58(15) . . . . ? B6 C2 B11 B10 -41.69(10) . . . . ? B3 C2 B11 B10 61.01(14) . . . . ? B7 C2 B11 B6 141.59(11) . . . . ? B1 C2 B11 B6 33.11(11) . . . . ? B3 C2 B11 B6 102.70(12) . . . . ? B1 C2 B11 B7 -108.47(12) . . . . ? B6 C2 B11 B7 -141.59(11) . . . . ? B3 C2 B11 B7 -38.88(11) . . . . ? C9 B10 B11 C2 -56.26(14) . . . . ? B6 B10 B11 C2 41.99(10) . . . . ? B5 B10 B11 C2 7.47(14) . . . . ? C9 B10 B11 B6 -98.24(12) . . . . ? B5 B10 B11 B6 -34.52(11) . . . . ? C9 B10 B11 B7 1.89(14) . . . . ? B6 B10 B11 B7 100.13(11) . . . . ? B5 B10 B11 B7 65.61(14) . . . . ? B5 B6 B11 C2 -95.07(12) . . . . ? B10 B6 B11 C2 -130.68(11) . . . . ? B1 B6 B11 C2 -30.26(11) . . . . ? B5 B6 B11 B10 35.61(11) . . . . ? C2 B6 B11 B10 130.68(11) . . . . ? B1 B6 B11 B10 100.41(12) . . . . ? B5 B6 B11 B7 -62.47(14) . . . . ? C2 B6 B11 B7 32.60(10) . . . . ? B10 B6 B11 B7 -98.08(12) . . . . ? B1 B6 B11 B7 2.34(15) . . . . ? B8 B7 B11 C2 95.79(11) . . . . ? B3 B7 B11 C2 34.51(10) . . . . ? C2 B7 B11 B10 -95.24(12) . . . . ? B8 B7 B11 B10 0.55(14) . . . . ? B3 B7 B11 B10 -60.73(14) . . . . ? C2 B7 B11 B6 -33.86(10) . . . . ? B8 B7 B11 B6 61.93(13) . . . . ? B3 B7 B11 B6 0.65(14) . . . . ? C21 C12 C13 C14 -0.3(2) . . . . ? N26 C12 C13 C14 179.06(12) . . . . ? C12 C13 C14 C15 -0.3(2) . . . . ? C13 C14 C15 C16 0.4(2) . . . . ? C14 C15 C16 C17 -179.73(13) . . . . ? C14 C15 C16 C21 -0.1(2) . . . . ? C15 C16 C17 C18 178.69(13) . . . . ? C21 C16 C17 C18 -1.0(2) . . . . ? C16 C17 C18 C19 2.1(2) . . . . ? C17 C18 C19 C20 -0.9(2) . . . . ? C18 C19 C20 C21 -1.5(2) . . . . ? C18 C19 C20 N27 177.37(12) . . . . ? C13 C12 C21 C20 -178.74(12) . . . . ? N26 C12 C21 C20 1.85(19) . . . . ? C13 C12 C21 C16 0.69(19) . . . . ? N26 C12 C21 C16 -178.72(10) . . . . ? C19 C20 C21 C12 -177.98(13) . . . . ? N27 C20 C21 C12 3.07(19) . . . . ? C19 C20 C21 C16 2.58(19) . . . . ? N27 C20 C21 C16 -176.36(11) . . . . ? C15 C16 C21 C12 -0.50(18) . . . . ? C17 C16 C21 C12 179.18(12) . . . . ? C15 C16 C21 C20 178.99(11) . . . . ? C17 C16 C21 C20 -1.33(18) . . . . ? C13 C12 N26 C24 57.99(16) . . . . ? C21 C12 N26 C24 -122.59(13) . . . . ? C13 C12 N26 C25 -68.66(16) . . . . ? C21 C12 N26 C25 110.76(13) . . . . ? C19 C20 N27 C22 -64.97(16) . . . . ? C21 C20 N27 C22 113.97(13) . . . . ? C19 C20 N27 C23 60.81(17) . . . . ? C21 C20 N27 C23 -120.25(13) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.149 _refine_diff_density_min -0.180 _refine_diff_density_rms 0.030 #===END