mentary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full ? _journal_coden_cambridge ? _journal_year ? _journal_volume ? _journal_page_first ? data_zb1 _database_code_depnum_ccdc_archive 'CCDC 603841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H21 B8 N' _chemical_formula_sum 'C6 H21 B8 N' _chemical_formula_weight 193.72 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 orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 22.8108(7) _cell_length_b 24.1768(10) _cell_length_c 8.9796(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4952.2(3) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 1.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.050 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9379 _exptl_absorpt_correction_T_max 0.9970 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Fine-focus Sealed tube' _diffrn_radiation_collimation miracol _diffrn_radiation_polarisn_norm ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_detector 'CCD plate' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8136 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2669 _reflns_number_gt 2384 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_data_reduction ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SHELXS-97 (Sheldrick, 1986) ; _computing_structure_refinement ; SHELXS-97 (Sheldrick, 1986) ; _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material ; 'enCIFer (CCDC, 2002)' ; _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 'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+1.6076P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 2.2(17) _refine_ls_number_reflns 2669 _refine_ls_number_parameters 220 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 N11 N 0.09220(5) 0.30011(5) 0.54159(13) 0.0270(3) Uani 1 1 d . . . C5 C 0.12787(6) 0.33105(6) 0.28939(17) 0.0306(3) Uani 1 1 d . . . C10 C 0.09406(6) 0.37909(6) 0.35827(16) 0.0307(3) Uani 1 1 d . . . C12 C 0.14283(6) 0.30739(6) 0.65577(16) 0.0325(3) Uani 1 1 d . . . C13 C 0.16105(8) 0.24970(8) 0.7040(2) 0.0450(4) Uani 1 1 d . . . C14 C 0.11956(8) 0.33884(9) 0.7912(2) 0.0468(4) Uani 1 1 d . . . C15 C 0.19473(7) 0.33834(8) 0.58882(19) 0.0424(4) Uani 1 1 d . . . B1 B 0.07493(8) 0.36013(7) 0.18399(18) 0.0330(4) Uani 1 1 d . . . B2 B 0.08411(8) 0.28736(7) 0.20024(17) 0.0321(4) Uani 1 1 d . . . B3 B 0.01163(8) 0.31648(7) 0.20140(19) 0.0337(4) Uani 1 1 d . . . B4 B 0.02239(7) 0.37384(7) 0.32446(18) 0.0318(4) Uani 1 1 d . . . B6 B 0.11127(7) 0.27475(7) 0.38689(17) 0.0286(3) Uani 1 1 d . . . B7 B 0.03043(7) 0.25762(7) 0.30752(18) 0.0314(3) Uani 1 1 d . . . B8 B -0.01025(7) 0.31505(7) 0.38970(18) 0.0310(3) Uani 1 1 d . . . B9 B 0.05612(7) 0.35347(7) 0.49961(18) 0.0293(3) Uani 1 1 d . . . H1 H 0.0839(7) 0.3863(7) 0.0870(19) 0.037(4) Uiso 1 1 d . . . H2 H 0.1025(7) 0.2610(7) 0.113(2) 0.039(4) Uiso 1 1 d . . . H3 H -0.0207(8) 0.3147(8) 0.107(2) 0.052(5) Uiso 1 1 d . . . H4 H -0.0048(7) 0.4133(7) 0.3280(19) 0.043(5) Uiso 1 1 d . . . H5 H 0.1662(8) 0.3355(7) 0.251(2) 0.044(5) Uiso 1 1 d . . . H6 H 0.1412(6) 0.2411(6) 0.3912(17) 0.028(4) Uiso 1 1 d . . . H7 H 0.0135(6) 0.2155(6) 0.286(2) 0.031(4) Uiso 1 1 d . . . H8 H -0.0566(8) 0.3145(7) 0.4249(18) 0.042(5) Uiso 1 1 d . . . H9 H 0.0422(7) 0.3811(7) 0.587(2) 0.040(4) Uiso 1 1 d . . . H10 H 0.1126(7) 0.4144(7) 0.3617(17) 0.033(4) Uiso 1 1 d . . . H11 H 0.0699(6) 0.2768(6) 0.5841(18) 0.026(4) Uiso 1 1 d . . . H13A H 0.1797(9) 0.2288(8) 0.617(3) 0.061(6) Uiso 1 1 d . . . H13B H 0.1287(8) 0.2287(8) 0.742(2) 0.053(5) Uiso 1 1 d . . . H13C H 0.1896(9) 0.2529(8) 0.787(3) 0.063(6) Uiso 1 1 d . . . H14A H 0.1503(9) 0.3367(9) 0.870(3) 0.057(6) Uiso 1 1 d . . . H14B H 0.0840(10) 0.3214(9) 0.828(3) 0.073(7) Uiso 1 1 d . . . H14C H 0.1122(9) 0.3781(11) 0.769(3) 0.068(6) Uiso 1 1 d . . . H15A H 0.2260(8) 0.3407(8) 0.672(2) 0.055(5) Uiso 1 1 d . . . H15B H 0.1838(8) 0.3733(8) 0.555(2) 0.047(5) Uiso 1 1 d . . . H15C H 0.2124(8) 0.3165(8) 0.501(2) 0.054(5) Uiso 1 1 d . . . H78 H 0.0120(7) 0.2702(7) 0.431(2) 0.043(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N11 0.0260(6) 0.0283(6) 0.0265(6) 0.0006(5) 0.0017(5) -0.0042(5) C5 0.0311(7) 0.0301(7) 0.0305(7) 0.0002(6) 0.0072(6) -0.0019(6) C10 0.0360(7) 0.0240(7) 0.0321(7) -0.0006(6) 0.0051(6) -0.0025(6) C12 0.0282(7) 0.0394(8) 0.0299(7) 0.0011(6) -0.0025(6) -0.0048(6) C13 0.0370(8) 0.0485(10) 0.0496(11) 0.0121(8) -0.0146(8) -0.0054(8) C14 0.0424(9) 0.0667(13) 0.0315(8) -0.0092(8) -0.0034(7) -0.0025(9) C15 0.0341(8) 0.0514(11) 0.0417(9) 0.0023(8) -0.0038(7) -0.0139(8) B1 0.0403(9) 0.0298(8) 0.0290(8) 0.0016(6) 0.0053(7) 0.0002(7) B2 0.0390(9) 0.0300(8) 0.0273(8) -0.0024(6) 0.0038(6) 0.0021(7) B3 0.0380(9) 0.0324(9) 0.0307(8) 0.0003(6) -0.0015(7) 0.0018(7) B4 0.0352(8) 0.0290(8) 0.0313(9) 0.0010(6) 0.0032(6) 0.0050(7) B6 0.0298(7) 0.0261(8) 0.0300(8) -0.0010(6) 0.0022(6) -0.0001(6) B7 0.0339(8) 0.0291(8) 0.0312(8) -0.0012(6) -0.0029(6) -0.0021(7) B8 0.0282(8) 0.0330(9) 0.0317(8) 0.0019(6) 0.0008(7) 0.0004(6) B9 0.0305(7) 0.0285(8) 0.0289(8) -0.0015(6) 0.0055(6) 0.0002(6) _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 N11 C12 1.5543(17) . ? N11 B9 1.576(2) . ? N11 B6 1.5796(19) . ? N11 H11 0.851(16) . ? C5 C10 1.5253(19) . ? C5 B2 1.659(2) . ? C5 B6 1.662(2) . ? C5 B1 1.688(2) . ? C5 H5 0.948(18) . ? C10 B9 1.656(2) . ? C10 B4 1.668(2) . ? C10 B1 1.688(2) . ? C10 H10 0.954(18) . ? C12 C13 1.518(2) . ? C12 C15 1.524(2) . ? C12 C14 1.529(2) . ? C13 H13A 1.03(2) . ? C13 H13B 0.96(2) . ? C13 H13C 0.99(2) . ? C14 H14A 1.00(2) . ? C14 H14B 0.97(2) . ? C14 H14C 0.98(2) . ? C15 H15A 1.04(2) . ? C15 H15B 0.93(2) . ? C15 H15C 1.03(2) . ? B1 B4 1.771(2) . ? B1 B2 1.778(2) . ? B1 B3 1.795(2) . ? B1 H1 1.096(17) . ? B2 B7 1.716(2) . ? B2 B3 1.797(2) . ? B2 B6 1.813(2) . ? B2 H2 1.093(17) . ? B3 B8 1.763(2) . ? B3 B7 1.765(2) . ? B3 B4 1.790(2) . ? B3 H3 1.127(19) . ? B4 B8 1.708(2) . ? B4 B9 1.819(2) . ? B4 H4 1.137(17) . ? B6 B7 2.020(2) . ? B6 H6 1.061(15) . ? B7 B8 1.826(2) . ? B7 H7 1.106(15) . ? B7 H78 1.227(18) . ? B8 B9 2.032(2) . ? B8 H8 1.104(17) . ? B8 H78 1.254(18) . ? B9 H9 1.079(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 C12 N11 B9 116.95(11) . . ? C12 N11 B6 114.80(10) . . ? B9 N11 B6 104.55(10) . . ? C12 N11 H11 102.9(10) . . ? B9 N11 H11 109.8(10) . . ? B6 N11 H11 107.6(10) . . ? C10 C5 B2 112.10(12) . . ? C10 C5 B6 107.15(11) . . ? B2 C5 B6 66.15(10) . . ? C10 C5 B1 63.15(9) . . ? B2 C5 B1 64.16(10) . . ? B6 C5 B1 118.26(12) . . ? C10 C5 H5 121.9(11) . . ? B2 C5 H5 116.8(11) . . ? B6 C5 H5 119.8(11) . . ? B1 C5 H5 114.1(11) . . ? C5 C10 B9 106.86(12) . . ? C5 C10 B4 111.34(12) . . ? B9 C10 B4 66.35(9) . . ? C5 C10 B1 63.13(10) . . ? B9 C10 B1 118.28(12) . . ? B4 C10 B1 63.71(10) . . ? C5 C10 H10 118.1(9) . . ? B9 C10 H10 122.8(10) . . ? B4 C10 H10 120.5(9) . . ? B1 C10 H10 112.8(10) . . ? C13 C12 C15 110.54(14) . . ? C13 C12 C14 108.94(14) . . ? C15 C12 C14 109.82(14) . . ? C13 C12 N11 106.72(11) . . ? C15 C12 N11 111.87(12) . . ? C14 C12 N11 108.85(12) . . ? C12 C13 H13A 110.4(11) . . ? C12 C13 H13B 112.2(11) . . ? H13A C13 H13B 109.2(16) . . ? C12 C13 H13C 108.9(11) . . ? H13A C13 H13C 109.9(17) . . ? H13B C13 H13C 106.2(17) . . ? C12 C14 H14A 107.0(12) . . ? C12 C14 H14B 110.0(14) . . ? H14A C14 H14B 109.2(19) . . ? C12 C14 H14C 112.3(14) . . ? H14A C14 H14C 108.1(18) . . ? H14B C14 H14C 110.1(18) . . ? C12 C15 H15A 106.1(11) . . ? C12 C15 H15B 111.5(11) . . ? H15A C15 H15B 111.8(15) . . ? C12 C15 H15C 110.8(11) . . ? H15A C15 H15C 108.2(14) . . ? H15B C15 H15C 108.4(16) . . ? C5 B1 C10 53.72(9) . . ? C5 B1 B4 99.36(11) . . ? C10 B1 B4 57.58(9) . . ? C5 B1 B2 57.14(9) . . ? C10 B1 B2 99.34(11) . . ? B4 B1 B2 101.91(11) . . ? C5 B1 B3 106.37(12) . . ? C10 B1 B3 106.67(11) . . ? B4 B1 B3 60.25(10) . . ? B2 B1 B3 60.39(10) . . ? C5 B1 H1 123.5(8) . . ? C10 B1 H1 122.1(9) . . ? B4 B1 H1 125.8(9) . . ? B2 B1 H1 127.9(9) . . ? B3 B1 H1 124.0(8) . . ? C5 B2 B7 115.16(12) . . ? C5 B2 B1 58.70(9) . . ? B7 B2 B1 112.13(12) . . ? C5 B2 B3 107.53(11) . . ? B7 B2 B3 60.29(10) . . ? B1 B2 B3 60.29(9) . . ? C5 B2 B6 57.00(9) . . ? B7 B2 B6 69.78(9) . . ? B1 B2 B6 106.42(11) . . ? B3 B2 B6 112.02(11) . . ? C5 B2 H2 119.0(9) . . ? B7 B2 H2 115.6(9) . . ? B1 B2 H2 124.3(9) . . ? B3 B2 H2 125.9(9) . . ? B6 B2 H2 115.6(9) . . ? B8 B3 B7 62.32(9) . . ? B8 B3 B4 57.45(9) . . ? B7 B3 B4 104.95(11) . . ? B8 B3 B1 108.82(12) . . ? B7 B3 B1 108.99(12) . . ? B4 B3 B1 59.21(9) . . ? B8 B3 B2 104.97(11) . . ? B7 B3 B2 57.58(9) . . ? B4 B3 B2 100.43(12) . . ? B1 B3 B2 59.33(10) . . ? B8 B3 H3 122.6(9) . . ? B7 B3 H3 122.4(9) . . ? B4 B3 H3 125.9(9) . . ? B1 B3 H3 118.9(9) . . ? B2 B3 H3 125.6(9) . . ? C10 B4 B8 115.36(12) . . ? C10 B4 B1 58.71(9) . . ? B8 B4 B1 112.55(12) . . ? C10 B4 B3 107.81(12) . . ? B8 B4 B3 60.49(9) . . ? B1 B4 B3 60.54(10) . . ? C10 B4 B9 56.53(8) . . ? B8 B4 B9 70.27(10) . . ? B1 B4 B9 106.20(11) . . ? B3 B4 B9 112.46(11) . . ? C10 B4 H4 117.7(9) . . ? B8 B4 H4 116.8(9) . . ? B1 B4 H4 123.0(9) . . ? B3 B4 H4 126.3(9) . . ? B9 B4 H4 115.7(9) . . ? N11 B6 C5 102.00(11) . . ? N11 B6 B2 130.82(11) . . ? C5 B6 B2 56.85(9) . . ? N11 B6 B7 97.96(10) . . ? C5 B6 B7 100.96(11) . . ? B2 B6 B7 52.86(8) . . ? N11 B6 H6 116.3(8) . . ? C5 B6 H6 120.0(8) . . ? B2 B6 H6 112.4(8) . . ? B7 B6 H6 116.3(8) . . ? B2 B7 B3 62.13(10) . . ? B2 B7 B8 105.72(11) . . ? B3 B7 B8 58.78(9) . . ? B2 B7 B6 57.37(9) . . ? B3 B7 B6 104.30(11) . . ? B8 B7 B6 99.52(10) . . ? B2 B7 H7 122.4(9) . . ? B3 B7 H7 124.1(9) . . ? B8 B7 H7 126.4(8) . . ? B6 B7 H7 124.8(8) . . ? B2 B7 H78 130.5(8) . . ? B3 B7 H78 101.9(8) . . ? B8 B7 H78 43.2(8) . . ? B6 B7 H78 86.7(8) . . ? H7 B7 H78 105.6(12) . . ? B4 B8 B3 62.06(10) . . ? B4 B8 B7 105.82(11) . . ? B3 B8 B7 58.90(9) . . ? B4 B8 B9 57.42(9) . . ? B3 B8 B9 104.24(11) . . ? B7 B8 B9 99.51(10) . . ? B4 B8 H8 121.8(9) . . ? B3 B8 H8 123.1(9) . . ? B7 B8 H8 126.3(9) . . ? B9 B8 H8 125.5(9) . . ? B4 B8 H78 130.2(7) . . ? B3 B8 H78 100.8(8) . . ? B7 B8 H78 42.0(8) . . ? B9 B8 H78 87.1(8) . . ? H8 B8 H78 106.9(12) . . ? N11 B9 C10 102.51(11) . . ? N11 B9 B4 130.50(12) . . ? C10 B9 B4 57.12(9) . . ? N11 B9 B8 97.54(10) . . ? C10 B9 B8 100.84(10) . . ? B4 B9 B8 52.31(8) . . ? N11 B9 H9 119.1(10) . . ? C10 B9 H9 118.7(9) . . ? B4 B9 H9 109.7(10) . . ? B8 B9 H9 114.6(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.107 _refine_diff_density_min -0.103 _refine_diff_density_rms 0.026