# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email michael.ingleson@manchester.ac.uk _publ_contact_author_name 'Michael Ingleson' loop_ _publ_author_name 'Michael Ingleson' 'Alessandro Del Grosso' 'Ewan Clark' 'Nicholas Montoute' data_c:\workdo~1\crystals\omji13~3\squeezed\squeezed _database_code_depnum_ccdc_archive 'CCDC 876412' #TrackingRef '- finalcif-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H40 Al3 B5 Cl14 N4 O6' _chemical_formula_sum 'C34 H40 Al3 B5 Cl14 N4 O6' _chemical_formula_weight 1231.99 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 23.9228(10) _cell_length_b 25.3459(10) _cell_length_c 38.9296(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 23604.8(17) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9498 _cell_measurement_theta_min 2.8589 _cell_measurement_theta_max 28.4864 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9952 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7089 _exptl_absorpt_correction_T_max 0.8972 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_reflns_number 29021 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.0948 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5219 _reflns_number_gt 2740 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. One molecule of disorder C6H4Cl2 could not be satisfactorily modelled so the squeeze protocol in platon was applied ; _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^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5219 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.824 _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 Cl3 Cl 0.53897(4) 0.37619(4) 0.01628(3) 0.0408(3) Uani 1 1 d . . . Cl4 Cl 0.62178(6) 0.27201(4) -0.01024(3) 0.0557(4) Uani 1 1 d . . . Cl5 Cl 0.58615(5) 0.37229(5) -0.06784(3) 0.0542(3) Uani 1 1 d . . . Al2 Al 0.60700(5) 0.35449(4) -0.01590(3) 0.0298(3) Uani 1 1 d . . . Cl6 Cl 0.68034(5) 0.39674(5) -0.00263(3) 0.0528(3) Uani 1 1 d . . . Cl7 Cl 0.68669(8) 0.10247(5) 0.17097(4) 0.1075(7) Uani 1 1 d . . . O3 O 0.62546(9) 0.40936(9) 0.09380(5) 0.0221(6) Uani 1 1 d . . . O4 O 0.6250 0.48988(12) 0.1250 0.0249(8) Uani 1 2 d S . . O1 O 0.67580(9) 0.34370(8) 0.12535(5) 0.0207(5) Uani 1 1 d . . . O2 O 0.6250 0.26307(12) 0.1250 0.0231(8) Uani 1 2 d S . . N1 N 0.72719(11) 0.25990(10) 0.12550(7) 0.0191(7) Uani 1 1 d . . . N2 N 0.61886(12) 0.49215(10) 0.06192(7) 0.0223(7) Uani 1 1 d . . . C1 C 0.74267(14) 0.23409(13) 0.15475(9) 0.0214(8) Uani 1 1 d . . . B2 B 0.67346(17) 0.29214(16) 0.12538(9) 0.0185(9) Uani 1 1 d . . . C2 C 0.79078(16) 0.20462(14) 0.15469(10) 0.0315(9) Uani 1 1 d . . . H2 H 0.8017 0.1857 0.1747 0.038 Uiso 1 1 calc R . . C3 C 0.82312(16) 0.20256(15) 0.12558(11) 0.0365(10) Uani 1 1 d . . . H3 H 0.8567 0.1825 0.1256 0.044 Uiso 1 1 calc R . . C8 C 0.56669(16) 0.50513(14) 0.05061(9) 0.0282(9) Uani 1 1 d . . . C12 C 0.66606(17) 0.50597(14) 0.04431(9) 0.0309(10) Uani 1 1 d . . . C9 C 0.56190(18) 0.53330(14) 0.02026(10) 0.0347(10) Uani 1 1 d . . . H9 H 0.5259 0.5427 0.0119 0.042 Uiso 1 1 calc R . . C6 C 0.70675(15) 0.24137(14) 0.18571(8) 0.0287(9) Uani 1 1 d . . . H6A H 0.7035 0.2791 0.1909 0.043 Uiso 1 1 calc R . . H6B H 0.7236 0.2230 0.2053 0.043 Uiso 1 1 calc R . . H6C H 0.6695 0.2268 0.1812 0.043 Uiso 1 1 calc R . . B3 B 0.62382(17) 0.46041(16) 0.09525(10) 0.0208(9) Uani 1 1 d . . . C11 C 0.66071(19) 0.53423(15) 0.01417(9) 0.0391(11) Uani 1 1 d . . . H11 H 0.6931 0.5444 0.0017 0.047 Uiso 1 1 calc R . . C10 C 0.6085(2) 0.54771(15) 0.00224(10) 0.0397(11) Uani 1 1 d . . . H10 H 0.6048 0.5670 -0.0185 0.048 Uiso 1 1 calc R . . B1 B 0.6250 0.3760(2) 0.1250 0.0205(13) Uani 1 2 d S . . C5 C 0.75870(15) 0.25743(14) 0.09623(9) 0.0285(9) Uani 1 1 d . . . C4 C 0.80729(16) 0.22927(15) 0.09647(10) 0.0343(10) Uani 1 1 d . . . H4 H 0.8302 0.2281 0.0765 0.041 Uiso 1 1 calc R . . C13 C 0.51792(16) 0.48831(16) 0.07222(9) 0.0369(10) Uani 1 1 d . . . H13A H 0.5188 0.4499 0.0753 0.055 Uiso 1 1 calc R . . H13B H 0.4830 0.4984 0.0608 0.055 Uiso 1 1 calc R . . H13C H 0.5200 0.5056 0.0947 0.055 Uiso 1 1 calc R . . C14 C 0.72064(16) 0.49036(17) 0.05961(10) 0.0434(11) Uani 1 1 d . . . H14A H 0.7266 0.5100 0.0810 0.065 Uiso 1 1 calc R . . H14B H 0.7508 0.4984 0.0434 0.065 Uiso 1 1 calc R . . H14C H 0.7204 0.4524 0.0645 0.065 Uiso 1 1 calc R . . C15 C 0.65250(17) 0.11524(14) 0.20873(12) 0.0411(11) Uani 1 1 d . . . C7 C 0.73720(19) 0.28601(17) 0.06515(9) 0.0490(12) Uani 1 1 d . . . H7A H 0.6983 0.2757 0.0609 0.074 Uiso 1 1 calc R . . H7B H 0.7601 0.2768 0.0452 0.074 Uiso 1 1 calc R . . H7C H 0.7391 0.3241 0.0691 0.074 Uiso 1 1 calc R . . C16 C 0.67821(19) 0.10663(17) 0.23997(15) 0.0563(14) Uani 1 1 d . . . H16 H 0.7156 0.0941 0.2407 0.068 Uiso 1 1 calc R . . C17 C 0.6503(2) 0.11597(19) 0.26939(14) 0.077(2) Uani 1 1 d . . . H17 H 0.6682 0.1091 0.2907 0.092 Uiso 1 1 calc R . . Cl2 Cl 0.31660(4) 0.41268(4) 0.07546(2) 0.0441(3) Uani 1 1 d . . . Al1 Al 0.3750 0.3750 0.10841(4) 0.0259(4) Uani 1 2 d S . . Cl1 Cl 0.33129(5) 0.32037(5) 0.14000(3) 0.0562(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 Cl3 0.0380(6) 0.0370(6) 0.0473(6) 0.0071(5) 0.0079(5) 0.0112(5) Cl4 0.1013(10) 0.0276(6) 0.0381(6) 0.0065(5) 0.0237(6) 0.0195(6) Cl5 0.0794(9) 0.0533(7) 0.0301(5) 0.0135(6) -0.0089(6) -0.0042(7) Al2 0.0393(7) 0.0251(6) 0.0251(6) 0.0003(5) -0.0001(6) 0.0050(5) Cl6 0.0383(7) 0.0671(8) 0.0531(7) -0.0091(6) -0.0012(6) -0.0050(6) Cl7 0.1639(16) 0.0384(8) 0.1203(12) -0.0238(8) 0.0985(12) -0.0150(9) O3 0.0323(15) 0.0150(13) 0.0189(12) 0.0000(10) -0.0034(11) 0.0011(11) O4 0.044(2) 0.0136(18) 0.0174(17) 0.000 -0.0061(17) 0.000 O1 0.0243(14) 0.0117(13) 0.0261(13) -0.0002(11) -0.0020(11) -0.0002(11) O2 0.0182(19) 0.0163(18) 0.035(2) 0.000 0.0019(16) 0.000 N1 0.0190(16) 0.0131(15) 0.0253(16) 0.0006(14) 0.0009(14) -0.0006(12) N2 0.0328(19) 0.0146(16) 0.0195(15) 0.0001(13) -0.0055(15) 0.0002(14) C1 0.025(2) 0.0116(19) 0.028(2) -0.0005(17) -0.0078(17) 0.0000(16) B2 0.022(2) 0.021(2) 0.0128(19) 0.0017(19) 0.0001(19) -0.0008(19) C2 0.031(2) 0.024(2) 0.040(2) 0.0042(18) -0.008(2) 0.0048(18) C3 0.024(2) 0.029(2) 0.056(3) 0.004(2) -0.002(2) 0.0083(18) C8 0.036(2) 0.019(2) 0.030(2) -0.0016(17) -0.0118(19) 0.0010(18) C12 0.039(3) 0.026(2) 0.027(2) 0.0017(18) -0.003(2) -0.002(2) C9 0.045(3) 0.023(2) 0.036(2) 0.0058(19) -0.019(2) 0.0011(19) C6 0.039(2) 0.024(2) 0.024(2) 0.0040(17) -0.0045(18) 0.0049(18) B3 0.025(2) 0.016(2) 0.022(2) 0.0043(18) -0.005(2) -0.0002(19) C11 0.056(3) 0.036(3) 0.025(2) 0.007(2) 0.007(2) -0.005(2) C10 0.072(3) 0.023(2) 0.024(2) 0.0092(18) -0.011(2) -0.004(2) B1 0.024(3) 0.019(3) 0.019(3) 0.000 0.002(3) 0.000 C5 0.028(2) 0.025(2) 0.032(2) 0.0027(18) 0.0082(19) -0.0023(18) C4 0.030(2) 0.031(2) 0.042(2) 0.004(2) 0.017(2) 0.0048(19) C13 0.035(3) 0.036(3) 0.040(2) 0.001(2) -0.008(2) 0.001(2) C14 0.035(3) 0.050(3) 0.044(3) 0.012(2) -0.001(2) -0.003(2) C15 0.048(3) 0.014(2) 0.061(3) -0.005(2) 0.020(2) -0.004(2) C7 0.061(3) 0.049(3) 0.037(2) 0.017(2) 0.023(2) 0.018(2) C16 0.039(3) 0.028(3) 0.102(4) 0.000(3) -0.024(3) 0.002(2) C17 0.131(6) 0.035(4) 0.065(3) -0.006(3) -0.025(4) 0.013(3) Cl2 0.0415(7) 0.0570(7) 0.0337(6) -0.0017(5) -0.0068(5) 0.0242(6) Al1 0.0205(9) 0.0372(10) 0.0199(8) 0.000 0.000 0.0025(8) Cl1 0.0519(8) 0.0699(9) 0.0469(7) 0.0183(6) 0.0102(6) -0.0123(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 Cl3 Al2 2.1262(15) . ? Cl4 Al2 2.1316(15) . ? Cl5 Al2 2.1312(15) . ? Al2 Cl6 2.1194(16) . ? Cl7 C15 1.713(4) . ? O3 B3 1.296(4) . ? O3 B1 1.479(4) . ? O4 B3 1.378(4) 4_655 ? O4 B3 1.378(4) . ? O1 B2 1.308(4) . ? O1 B1 1.466(4) . ? O2 B2 1.374(4) 4_655 ? O2 B2 1.374(4) . ? N1 C1 1.364(4) . ? N1 C5 1.368(4) . ? N1 B2 1.523(5) . ? N2 C8 1.364(4) . ? N2 C12 1.367(4) . ? N2 B3 1.531(5) . ? C1 C2 1.372(5) . ? C1 C6 1.492(5) . ? C2 C3 1.373(5) . ? C2 H2 0.9500 . ? C3 C4 1.373(5) . ? C3 H3 0.9500 . ? C8 C9 1.385(5) . ? C8 C13 1.500(5) . ? C12 C11 1.381(5) . ? C12 C14 1.489(5) . ? C9 C10 1.366(5) . ? C9 H9 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C10 1.377(5) . ? C11 H11 0.9500 . ? C10 H10 0.9500 . ? B1 O1 1.466(4) 4_655 ? B1 O3 1.479(4) 4_655 ? C5 C4 1.364(5) . ? C5 C7 1.501(5) . ? C4 H4 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.380(6) . ? C15 C15 1.406(8) 2_655 ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C16 C17 1.347(6) . ? C16 H16 0.9500 . ? C17 C17 1.294(11) 2_655 ? C17 H17 0.9500 . ? Cl2 Al1 2.1235(13) . ? Al1 Cl2 2.1235(13) 14 ? Al1 Cl1 2.1268(14) 14 ? Al1 Cl1 2.1268(14) . ? 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 Cl6 Al2 Cl3 111.06(6) . . ? Cl6 Al2 Cl5 108.55(7) . . ? Cl3 Al2 Cl5 108.97(7) . . ? Cl6 Al2 Cl4 109.45(7) . . ? Cl3 Al2 Cl4 108.66(6) . . ? Cl5 Al2 Cl4 110.15(7) . . ? B3 O3 B1 122.3(3) . . ? B3 O4 B3 114.4(4) 4_655 . ? B2 O1 B1 121.5(3) . . ? B2 O2 B2 115.1(4) 4_655 . ? C1 N1 C5 121.6(3) . . ? C1 N1 B2 119.3(3) . . ? C5 N1 B2 119.2(3) . . ? C8 N2 C12 122.2(3) . . ? C8 N2 B3 118.1(3) . . ? C12 N2 B3 119.7(3) . . ? N1 C1 C2 119.2(3) . . ? N1 C1 C6 117.3(3) . . ? C2 C1 C6 123.5(3) . . ? O1 B2 O2 124.9(3) . . ? O1 B2 N1 120.0(3) . . ? O2 B2 N1 115.1(3) . . ? C1 C2 C3 119.6(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 120.5(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? N2 C8 C9 118.4(4) . . ? N2 C8 C13 117.5(3) . . ? C9 C8 C13 124.1(4) . . ? N2 C12 C11 118.9(4) . . ? N2 C12 C14 117.1(3) . . ? C11 C12 C14 124.0(4) . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 B3 O4 125.3(3) . . ? O3 B3 N2 119.3(3) . . ? O4 B3 N2 115.4(3) . . ? C10 C11 C12 120.0(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C9 C10 C11 120.1(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? O1 B1 O1 112.0(4) 4_655 . ? O1 B1 O3 108.70(12) 4_655 4_655 ? O1 B1 O3 108.52(12) . 4_655 ? O1 B1 O3 108.52(12) 4_655 . ? O1 B1 O3 108.70(12) . . ? O3 B1 O3 110.4(4) 4_655 . ? C4 C5 N1 119.2(3) . . ? C4 C5 C7 123.4(3) . . ? N1 C5 C7 117.4(3) . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C15 118.2(3) . 2_655 ? C16 C15 Cl7 120.9(4) . . ? C15 C15 Cl7 120.89(17) 2_655 . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C17 C16 C15 120.1(5) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C17 C16 121.7(3) 2_655 . ? C17 C17 H17 119.1 2_655 . ? C16 C17 H17 119.1 . . ? Cl2 Al1 Cl2 105.67(8) . 14 ? Cl2 Al1 Cl1 112.33(5) . 14 ? Cl2 Al1 Cl1 108.58(4) 14 14 ? Cl2 Al1 Cl1 108.58(4) . . ? Cl2 Al1 Cl1 112.33(5) 14 . ? Cl1 Al1 Cl1 109.35(9) 14 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C2 -0.5(5) . . . . ? B2 N1 C1 C2 179.3(3) . . . . ? C5 N1 C1 C6 177.3(3) . . . . ? B2 N1 C1 C6 -2.9(4) . . . . ? B1 O1 B2 O2 0.2(5) . . . . ? B1 O1 B2 N1 179.6(2) . . . . ? B2 O2 B2 O1 -0.1(2) 4_655 . . . ? B2 O2 B2 N1 -179.5(3) 4_655 . . . ? C1 N1 B2 O1 107.2(4) . . . . ? C5 N1 B2 O1 -72.9(4) . . . . ? C1 N1 B2 O2 -73.3(4) . . . . ? C5 N1 B2 O2 106.5(3) . . . . ? N1 C1 C2 C3 1.5(5) . . . . ? C6 C1 C2 C3 -176.1(3) . . . . ? C1 C2 C3 C4 -0.7(6) . . . . ? C12 N2 C8 C9 -0.1(5) . . . . ? B3 N2 C8 C9 -179.2(3) . . . . ? C12 N2 C8 C13 -179.5(3) . . . . ? B3 N2 C8 C13 1.4(5) . . . . ? C8 N2 C12 C11 0.3(5) . . . . ? B3 N2 C12 C11 179.5(3) . . . . ? C8 N2 C12 C14 178.9(3) . . . . ? B3 N2 C12 C14 -1.9(5) . . . . ? N2 C8 C9 C10 -0.1(5) . . . . ? C13 C8 C9 C10 179.2(3) . . . . ? B1 O3 B3 O4 4.3(5) . . . . ? B1 O3 B3 N2 -174.3(2) . . . . ? B3 O4 B3 O3 -2.2(3) 4_655 . . . ? B3 O4 B3 N2 176.4(4) 4_655 . . . ? C8 N2 B3 O3 91.8(4) . . . . ? C12 N2 B3 O3 -87.4(4) . . . . ? C8 N2 B3 O4 -86.9(4) . . . . ? C12 N2 B3 O4 93.9(4) . . . . ? N2 C12 C11 C10 -0.4(6) . . . . ? C14 C12 C11 C10 -178.9(4) . . . . ? C8 C9 C10 C11 0.0(6) . . . . ? C12 C11 C10 C9 0.2(6) . . . . ? B2 O1 B1 O1 -0.1(2) . . . 4_655 ? B2 O1 B1 O3 119.9(3) . . . 4_655 ? B2 O1 B1 O3 -120.0(3) . . . . ? B3 O3 B1 O1 117.0(4) . . . 4_655 ? B3 O3 B1 O1 -121.0(4) . . . . ? B3 O3 B1 O3 -2.0(2) . . . 4_655 ? C1 N1 C5 C4 -1.2(5) . . . . ? B2 N1 C5 C4 178.9(3) . . . . ? C1 N1 C5 C7 178.3(3) . . . . ? B2 N1 C5 C7 -1.5(5) . . . . ? N1 C5 C4 C3 2.0(6) . . . . ? C7 C5 C4 C3 -177.6(4) . . . . ? C2 C3 C4 C5 -1.0(6) . . . . ? C15 C15 C16 C17 1.2(7) 2_655 . . . ? Cl7 C15 C16 C17 -178.8(4) . . . . ? C15 C16 C17 C17 -1.4(10) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.890 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.080 # Attachment '- finalcif-3.cif' data_omji118_attempt1 _database_code_depnum_ccdc_archive 'CCDC 876413' #TrackingRef '- finalcif-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H5 B Cl2 N, Al Cl4' _chemical_formula_sum 'C5 H5 Al B Cl6 N' _chemical_formula_weight 329.59 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P 3 c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x+y, y, z+1/2' 'x, x-y, z+1/2' '-y, -x, z+1/2' _cell_length_a 12.708(5) _cell_length_b 12.708(5) _cell_length_c 13.720(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 1918.8(13) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4894 _cell_measurement_theta_min 2.9644 _cell_measurement_theta_max 28.3961 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 1.371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.48385 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12034 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2621 _reflns_number_gt 2187 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXS-97 (Sheldrick, 1990)' _computing_cell_refinement 'SHELXS-97 (Sheldrick, 1990)' _computing_data_reduction 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(8) _refine_ls_number_reflns 2621 _refine_ls_number_parameters 127 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _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 Cl7 Cl 0.0000 0.0000 0.24414(11) 0.0247(3) Uani 1 3 d S . . Cl3 Cl 0.30312(8) 0.49441(7) 0.00423(7) 0.0283(2) Uani 1 1 d . . . Cl8 Cl 0.16005(7) 0.00404(10) 0.45259(8) 0.02908(19) Uani 1 1 d . . . Cl6 Cl 0.68711(8) 0.50129(7) 0.40263(7) 0.0299(2) Uani 1 1 d . . . Cl2 Cl 0.35845(8) 0.42761(8) 0.33808(7) 0.0347(2) Uani 1 1 d . . . Al3 Al 0.0000 0.0000 0.40007(13) 0.0188(4) Uani 1 3 d S . . Cl4 Cl 0.3333 0.6667 0.20856(12) 0.0338(4) Uani 1 3 d S . . Cl5 Cl 0.6667 0.3333 0.19656(11) 0.0310(4) Uani 1 3 d S . . Cl1 Cl 0.35680(9) 0.29749(8) 0.15711(8) 0.0387(3) Uani 1 1 d . . . Al2 Al 0.6667 0.3333 0.35214(13) 0.0189(4) Uani 1 3 d S . . Al1 Al 0.3333 0.6667 0.05179(15) 0.0189(4) Uani 1 3 d S . . N1 N 0.5325(2) 0.5380(2) 0.19230(19) 0.0199(6) Uani 1 1 d . . . C1 C 0.5830(3) 0.5392(3) 0.1045(2) 0.0230(8) Uani 1 1 d . . . H1 H 0.5478 0.4696 0.0661 0.028 Uiso 1 1 calc R . . C3 C 0.7370(3) 0.7452(3) 0.1283(2) 0.0244(8) Uani 1 1 d . . . H3 H 0.8052 0.8152 0.1062 0.029 Uiso 1 1 calc R . . B1 B 0.4221(4) 0.4267(3) 0.2268(3) 0.0230(9) Uani 1 1 d . . . C4 C 0.6857(3) 0.7426(3) 0.2183(3) 0.0257(8) Uani 1 1 d . . . H4 H 0.7206 0.8113 0.2578 0.031 Uiso 1 1 calc R . . C5 C 0.5850(3) 0.6404(3) 0.2486(3) 0.0233(8) Uani 1 1 d . . . H5 H 0.5510 0.6399 0.3088 0.028 Uiso 1 1 calc R . . C2 C 0.6833(3) 0.6399(3) 0.0721(2) 0.0267(8) Uani 1 1 d . . . H2 H 0.7165 0.6388 0.0120 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl7 0.0269(5) 0.0269(5) 0.0204(7) 0.000 0.000 0.0135(2) Cl3 0.0262(5) 0.0178(5) 0.0412(6) -0.0033(4) -0.0015(4) 0.0111(4) Cl8 0.0232(4) 0.0388(5) 0.0293(4) -0.0022(4) -0.0045(4) 0.0185(4) Cl6 0.0332(5) 0.0219(5) 0.0375(6) -0.0042(4) -0.0001(4) 0.0160(4) Cl2 0.0299(5) 0.0353(5) 0.0300(5) 0.0025(4) 0.0058(4) 0.0095(4) Al3 0.0173(5) 0.0173(5) 0.0218(9) 0.000 0.000 0.0087(3) Cl4 0.0367(6) 0.0367(6) 0.0279(10) 0.000 0.000 0.0183(3) Cl5 0.0355(5) 0.0355(5) 0.0219(8) 0.000 0.000 0.0177(3) Cl1 0.0386(6) 0.0215(5) 0.0483(6) -0.0066(5) -0.0002(5) 0.0092(4) Al2 0.0175(6) 0.0175(6) 0.0216(10) 0.000 0.000 0.0088(3) Al1 0.0157(5) 0.0157(5) 0.0252(10) 0.000 0.000 0.0079(3) N1 0.0211(15) 0.0217(15) 0.0196(15) -0.0044(12) -0.0039(13) 0.0127(12) C1 0.0238(18) 0.0265(19) 0.025(2) -0.0092(16) -0.0098(15) 0.0174(16) C3 0.0190(18) 0.0269(18) 0.028(2) 0.0086(16) -0.0001(16) 0.0118(15) B1 0.027(2) 0.023(2) 0.025(2) 0.0006(18) -0.0083(18) 0.0176(18) C4 0.0238(19) 0.0242(18) 0.029(2) -0.0090(16) -0.0110(16) 0.0118(15) C5 0.0219(18) 0.0313(19) 0.0217(18) 0.0000(16) 0.0034(15) 0.0171(16) C2 0.0249(19) 0.042(2) 0.021(2) 0.0031(17) 0.0019(15) 0.0224(18) _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 Cl7 Al3 2.139(2) . ? Cl3 Al1 2.1272(13) . ? Cl8 Al3 2.1341(12) . ? Cl6 Al2 2.1327(13) . ? Cl2 B1 1.730(4) . ? Al3 Cl8 2.1341(12) 3 ? Al3 Cl8 2.1341(12) 2 ? Cl4 Al1 2.151(3) . ? Cl5 Al2 2.135(3) . ? Cl1 B1 1.714(4) . ? Al2 Cl6 2.1327(13) 3_665 ? Al2 Cl6 2.1327(13) 2_655 ? Al1 Cl3 2.1272(13) 3_565 ? Al1 Cl3 2.1272(13) 2_665 ? N1 C1 1.361(4) . ? N1 C5 1.367(4) . ? N1 B1 1.487(5) . ? C1 C2 1.352(5) . ? C1 H1 0.9300 . ? C3 C4 1.389(5) . ? C3 C2 1.392(5) . ? C3 H3 0.9300 . ? C4 C5 1.356(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C2 H2 0.9300 . ? 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 Cl8 Al3 Cl8 109.20(5) 3 . ? Cl8 Al3 Cl8 109.20(5) 3 2 ? Cl8 Al3 Cl8 109.20(5) . 2 ? Cl8 Al3 Cl7 109.74(5) 3 . ? Cl8 Al3 Cl7 109.74(5) . . ? Cl8 Al3 Cl7 109.74(5) 2 . ? Cl6 Al2 Cl6 109.98(5) 3_665 2_655 ? Cl6 Al2 Cl6 109.98(5) 3_665 . ? Cl6 Al2 Cl6 109.98(5) 2_655 . ? Cl6 Al2 Cl5 108.95(6) 3_665 . ? Cl6 Al2 Cl5 108.95(6) 2_655 . ? Cl6 Al2 Cl5 108.95(6) . . ? Cl3 Al1 Cl3 111.03(6) 3_565 2_665 ? Cl3 Al1 Cl3 111.03(6) 3_565 . ? Cl3 Al1 Cl3 111.03(6) 2_665 . ? Cl3 Al1 Cl4 107.87(6) 3_565 . ? Cl3 Al1 Cl4 107.87(6) 2_665 . ? Cl3 Al1 Cl4 107.87(6) . . ? C1 N1 C5 119.1(3) . . ? C1 N1 B1 120.6(3) . . ? C5 N1 B1 120.3(3) . . ? C2 C1 N1 121.2(3) . . ? C2 C1 H1 119.4 . . ? N1 C1 H1 119.4 . . ? C4 C3 C2 118.1(3) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? N1 B1 Cl1 120.5(3) . . ? N1 B1 Cl2 119.8(3) . . ? Cl1 B1 Cl2 119.7(2) . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 N1 121.1(3) . . ? C4 C5 H5 119.5 . . ? N1 C5 H5 119.5 . . ? C1 C2 C3 120.3(3) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.757 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.076 # Attachment '- finalcif-4.cif' data_omji126 _database_code_depnum_ccdc_archive 'CCDC 876414' #TrackingRef '- finalcif-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H5 B Br2 N, Al Br4' _chemical_formula_sum 'C5 H5 Al B Br6 N' _chemical_formula_weight 596.29 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 7.6227(3) _cell_length_b 13.8546(6) _cell_length_c 13.6784(5) _cell_angle_alpha 90.0 _cell_angle_beta 95.281(3) _cell_angle_gamma 90.0 _cell_volume 1438.43(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3718 _cell_measurement_theta_min 3.0547 _cell_measurement_theta_max 28.3859 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 16.772 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0898 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3367 _diffrn_reflns_number 5603 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3680 _reflns_number_gt 3169 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+0.3655P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.07(4) _refine_ls_number_reflns 3680 _refine_ls_number_parameters 254 _refine_ls_number_restraints 254 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.049 _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 Br11 Br 0.83898(19) 0.52972(12) 0.33996(11) 0.0211(3) Uani 1 1 d . . . Br3 Br 0.3141(2) 0.94491(12) 0.38153(11) 0.0219(3) Uani 1 1 d . . . Br9 Br 0.8613(2) 0.32358(12) 0.52140(12) 0.0237(3) Uani 1 1 d . . . Br5 Br 0.2977(2) 0.80642(11) 0.61681(12) 0.0220(3) Uani 1 1 d . . . Br12 Br 1.0719(2) 0.56186(12) 0.58860(12) 0.0241(3) Uani 1 1 d . . . Br2 Br 0.88017(19) 0.81415(12) 0.26324(12) 0.0237(4) Uani 1 1 d . . . Br10 Br 0.57846(18) 0.53656(12) 0.55993(12) 0.0244(4) Uani 1 1 d . . . Br4 Br 0.5652(2) 1.03220(13) 0.61306(12) 0.0267(4) Uani 1 1 d . . . Br6 Br 0.0705(2) 1.04583(12) 0.58334(12) 0.0269(4) Uani 1 1 d . . . Br8 Br 0.3959(2) 0.40146(12) 0.30296(12) 0.0266(4) Uani 1 1 d . . . Br1 Br 0.7723(2) 0.80367(14) 0.48567(12) 0.0311(4) Uani 1 1 d . . . Br7 Br 0.3049(2) 0.21767(13) 0.43404(13) 0.0298(4) Uani 1 1 d . . . Al1 Al 0.8368(6) 0.4881(3) 0.5032(3) 0.0165(9) Uani 1 1 d . . . Al2 Al 0.3118(6) 0.9581(3) 0.5494(4) 0.0170(9) Uani 1 1 d . . . N1 N 0.5500(16) 0.7309(9) 0.3168(9) 0.0179(18) Uani 1 1 d U . . B1 B 0.720(2) 0.7762(13) 0.3518(13) 0.0179(18) Uani 1 1 d U . . C10 C 0.723(2) 0.2689(12) 0.2618(11) 0.0202(12) Uani 1 1 d U . . H10 H 0.6898 0.3283 0.2342 0.024 Uiso 1 1 calc R . . N2 N 0.6133(17) 0.2277(10) 0.3222(10) 0.0202(12) Uani 1 1 d U . . C7 C 0.811(2) 0.0898(12) 0.3412(12) 0.0204(12) Uani 1 1 d U . . H7 H 0.8411 0.0302 0.3694 0.025 Uiso 1 1 calc R . . C4 C 0.359(2) 0.6628(12) 0.1853(12) 0.022(3) Uani 1 1 d U . . H4 H 0.3351 0.6479 0.1191 0.026 Uiso 1 1 calc R . . C1 C 0.430(2) 0.7069(11) 0.3814(12) 0.019(2) Uani 1 1 d U . . H1 H 0.4549 0.7206 0.4478 0.023 Uiso 1 1 calc R . . C5 C 0.514(2) 0.7059(12) 0.2177(11) 0.021(3) Uani 1 1 d U . . H5 H 0.5967 0.7189 0.1736 0.026 Uiso 1 1 calc R . . C9 C 0.875(2) 0.2303(12) 0.2388(11) 0.0203(12) Uani 1 1 d U . . H9 H 0.9487 0.2626 0.1993 0.024 Uiso 1 1 calc R . . C2 C 0.2718(19) 0.6629(12) 0.3503(12) 0.021(2) Uani 1 1 d U . . H2 H 0.1910 0.6482 0.3951 0.025 Uiso 1 1 calc R . . C3 C 0.235(2) 0.6408(12) 0.2514(12) 0.023(3) Uani 1 1 d U . . H3 H 0.1286 0.6117 0.2293 0.027 Uiso 1 1 calc R . . C6 C 0.6572(19) 0.1368(11) 0.3595(11) 0.0204(12) Uani 1 1 d U . . H6 H 0.5801 0.1062 0.3983 0.024 Uiso 1 1 calc R . . C8 C 0.919(2) 0.1350(12) 0.2792(11) 0.0204(12) Uani 1 1 d U . . H8 H 1.0202 0.1041 0.2630 0.025 Uiso 1 1 calc R . . B2 B 0.454(2) 0.2743(14) 0.3512(13) 0.0203(13) Uani 1 1 d U . . 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 Br11 0.0223(7) 0.0251(8) 0.0157(7) 0.0032(6) 0.0015(6) -0.0038(6) Br3 0.0284(8) 0.0212(8) 0.0156(7) 0.0002(6) 0.0002(6) -0.0005(7) Br9 0.0307(8) 0.0181(8) 0.0219(7) 0.0006(6) 0.0002(6) -0.0002(7) Br5 0.0231(7) 0.0210(8) 0.0223(7) 0.0052(6) 0.0037(6) -0.0006(6) Br12 0.0217(8) 0.0259(8) 0.0234(8) 0.0002(7) -0.0057(6) -0.0066(7) Br2 0.0183(7) 0.0257(9) 0.0272(8) 0.0048(7) 0.0024(6) -0.0044(6) Br10 0.0198(8) 0.0300(9) 0.0239(8) -0.0006(7) 0.0053(6) 0.0033(7) Br4 0.0208(7) 0.0313(9) 0.0269(8) -0.0013(7) -0.0044(6) -0.0090(7) Br6 0.0216(8) 0.0295(9) 0.0305(9) 0.0013(7) 0.0082(6) 0.0087(7) Br8 0.0280(8) 0.0217(8) 0.0295(8) 0.0028(7) -0.0011(6) 0.0044(7) Br1 0.0297(9) 0.0414(11) 0.0209(8) -0.0060(7) -0.0041(7) -0.0084(7) Br7 0.0284(8) 0.0275(9) 0.0354(9) 0.0036(7) 0.0141(7) 0.0001(7) Al1 0.016(2) 0.018(2) 0.016(2) 0.0030(18) 0.0012(17) -0.0030(18) Al2 0.015(2) 0.019(2) 0.017(2) 0.0009(18) 0.0010(17) -0.0004(17) N1 0.0178(19) 0.0178(19) 0.0180(19) 0.0000(8) 0.0016(8) 0.0002(8) B1 0.0179(19) 0.018(2) 0.0180(19) 0.0000(8) 0.0015(8) 0.0001(8) C10 0.0203(13) 0.0201(13) 0.0202(13) -0.0002(6) 0.0018(6) -0.0001(6) N2 0.0203(13) 0.0201(13) 0.0202(13) -0.0002(6) 0.0018(6) -0.0001(6) C7 0.0205(13) 0.0202(13) 0.0205(14) -0.0002(6) 0.0018(6) 0.0000(6) C4 0.023(5) 0.021(5) 0.021(5) 0.002(4) -0.002(4) -0.001(4) C1 0.018(4) 0.019(5) 0.020(4) 0.001(4) 0.000(4) 0.002(4) C5 0.019(5) 0.025(5) 0.020(4) 0.000(4) 0.000(4) 0.001(4) C9 0.0203(13) 0.0204(13) 0.0202(14) -0.0002(6) 0.0019(6) 0.0000(6) C2 0.018(4) 0.020(5) 0.025(5) -0.001(4) 0.002(4) 0.003(4) C3 0.021(5) 0.021(5) 0.025(5) 0.000(4) -0.001(4) 0.000(4) C6 0.0205(13) 0.0202(13) 0.0204(13) -0.0001(6) 0.0018(6) -0.0001(6) C8 0.0205(13) 0.0204(13) 0.0204(14) -0.0002(6) 0.0019(6) 0.0000(6) B2 0.0202(14) 0.0202(14) 0.0203(14) -0.0003(8) 0.0018(7) -0.0001(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 Br11 Al1 2.308(5) . ? Br3 Al2 2.305(5) . ? Br9 Al1 2.298(5) . ? Br5 Al2 2.301(5) . ? Br12 Al1 2.288(5) . ? Br2 B1 1.874(17) . ? Br10 Al1 2.283(5) . ? Br4 Al2 2.288(5) . ? Br6 Al2 2.288(5) . ? Br8 B2 1.918(19) . ? Br1 B1 1.877(17) . ? Br7 B2 1.851(18) . ? N1 C1 1.37(2) . ? N1 C5 1.401(19) . ? N1 B1 1.48(2) . ? C10 C9 1.34(2) . ? C10 N2 1.35(2) . ? C10 H10 0.9300 . ? N2 C6 1.39(2) . ? N2 B2 1.46(2) . ? C7 C8 1.38(2) . ? C7 C6 1.39(2) . ? C7 H7 0.9300 . ? C4 C5 1.36(2) . ? C4 C3 1.40(2) . ? C4 H4 0.9300 . ? C1 C2 1.38(2) . ? C1 H1 0.9300 . ? C5 H5 0.9300 . ? C9 C8 1.46(2) . ? C9 H9 0.9300 . ? C2 C3 1.39(2) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C6 H6 0.9300 . ? C8 H8 0.9300 . ? 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 Br10 Al1 Br12 110.8(2) . . ? Br10 Al1 Br9 108.59(19) . . ? Br12 Al1 Br9 109.63(19) . . ? Br10 Al1 Br11 109.77(18) . . ? Br12 Al1 Br11 107.89(19) . . ? Br9 Al1 Br11 110.2(2) . . ? Br4 Al2 Br6 110.5(2) . . ? Br4 Al2 Br5 109.04(19) . . ? Br6 Al2 Br5 109.6(2) . . ? Br4 Al2 Br3 109.4(2) . . ? Br6 Al2 Br3 108.93(19) . . ? Br5 Al2 Br3 109.4(2) . . ? C1 N1 C5 118.7(12) . . ? C1 N1 B1 120.8(13) . . ? C5 N1 B1 120.4(13) . . ? N1 B1 Br2 120.9(11) . . ? N1 B1 Br1 120.2(11) . . ? Br2 B1 Br1 118.7(9) . . ? C9 C10 N2 124.7(15) . . ? C9 C10 H10 117.6 . . ? N2 C10 H10 117.6 . . ? C10 N2 C6 117.8(13) . . ? C10 N2 B2 123.6(13) . . ? C6 N2 B2 118.6(13) . . ? C8 C7 C6 117.2(15) . . ? C8 C7 H7 121.4 . . ? C6 C7 H7 121.4 . . ? C5 C4 C3 120.1(15) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C1 C2 121.6(14) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C4 C5 N1 120.7(14) . . ? C4 C5 H5 119.6 . . ? N1 C5 H5 119.6 . . ? C10 C9 C8 116.4(14) . . ? C10 C9 H9 121.8 . . ? C8 C9 H9 121.8 . . ? C1 C2 C3 119.3(14) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 119.5(15) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? N2 C6 C7 122.7(14) . . ? N2 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C7 C8 C9 121.1(14) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? N2 B2 Br7 123.4(12) . . ? N2 B2 Br8 118.8(12) . . ? Br7 B2 Br8 117.7(9) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.009 _refine_diff_density_min -1.478 _refine_diff_density_rms 0.272 # Attachment '- finalcif-6.cif' data_c:\workdo~1\crystals\omji12~2\fromch~1\omji127 _database_code_depnum_ccdc_archive 'CCDC 876415' #TrackingRef '- finalcif-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H40 Al8 B6 Br30 N8 O6' _chemical_formula_sum 'C40 H40 Al8 B6 Br30 N8 O6' _chemical_formula_weight 3406.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 10.3692(3) _cell_length_b 11.1756(3) _cell_length_c 41.7001(12) _cell_angle_alpha 83.535(2) _cell_angle_beta 84.176(2) _cell_angle_gamma 75.954(3) _cell_volume 4644.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11876 _cell_measurement_theta_min 2.9588 _cell_measurement_theta_max 28.5044 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 13.036 _exptl_absorpt_correction_T_min 0.12826 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_reflns_number 29161 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.1193 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.03 _reflns_number_total 16359 _reflns_number_gt 11913 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0453P)^2^+2.0625P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16359 _refine_ls_number_parameters 883 _refine_ls_number_restraints 570 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1546 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.088 _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 Br1 Br 0.15223(12) 0.48606(11) 0.24327(3) 0.0177(3) Uani 1 1 d . . . Br2 Br -0.12304(12) 0.38496(12) 0.21071(3) 0.0280(3) Uani 1 1 d . . . Br3 Br 0.02649(11) 0.63425(10) 0.16487(3) 0.0141(2) Uani 1 1 d . . . Br4 Br 0.22387(11) 0.30633(11) 0.17104(3) 0.0204(3) Uani 1 1 d . . . Br5 Br 0.74868(12) 0.85388(11) 0.21779(3) 0.0192(3) Uani 1 1 d . . . Br6 Br 0.45607(11) 0.98034(11) 0.17036(3) 0.0192(3) Uani 1 1 d . . . Br7 Br 0.66413(11) 0.66972(11) 0.15383(3) 0.0220(3) Uani 1 1 d . . . Br8 Br 0.80091(12) 0.94902(10) 0.12993(3) 0.0196(3) Uani 1 1 d . . . Br9 Br 0.53568(12) 0.60012(12) 0.34825(3) 0.0209(3) Uani 1 1 d . . . Br10 Br 0.19395(12) 0.67659(12) 0.32011(4) 0.0289(3) Uani 1 1 d . . . Br11 Br 0.40893(12) 0.35905(10) 0.31362(3) 0.0196(3) Uani 1 1 d . . . Br12 Br 0.48935(11) 0.63485(11) 0.26067(3) 0.0176(3) Uani 1 1 d . . . Br13 Br 0.99337(11) -0.01516(10) 0.34181(3) 0.0203(3) Uani 1 1 d . . . Br14 Br 0.78386(11) 0.27794(10) 0.37105(3) 0.0176(3) Uani 1 1 d . . . Br15 Br 0.62312(11) 0.02896(11) 0.35309(3) 0.0221(3) Uani 1 1 d . . . Br16 Br 0.78543(13) 0.21127(13) 0.28559(3) 0.0329(3) Uani 1 1 d . . . Br17 Br 0.41165(12) 0.67286(11) 0.48649(3) 0.0213(3) Uani 1 1 d . . . Br18 Br 0.31610(12) 1.02381(11) 0.47646(3) 0.0198(3) Uani 1 1 d . . . Br19 Br 0.34577(12) 0.84253(11) 0.40475(3) 0.0227(3) Uani 1 1 d . . . Br20 Br 0.64528(11) 0.86917(10) 0.44390(3) 0.0205(3) Uani 1 1 d . . . Br21 Br 0.72959(12) 0.54623(11) 0.42145(3) 0.0228(3) Uani 1 1 d . . . Br22 Br 0.79751(13) 0.60470(12) 0.50451(3) 0.0274(3) Uani 1 1 d . . . Br23 Br 0.99594(12) 0.71100(12) 0.43072(4) 0.0278(3) Uani 1 1 d . . . Br24 Br 1.22821(13) -0.02442(11) 0.02488(3) 0.0248(3) Uani 1 1 d . . . Br25 Br 1.10280(12) 0.32299(10) 0.01509(3) 0.0189(3) Uani 1 1 d . . . Br26 Br 1.15073(14) 0.15128(12) 0.09824(3) 0.0282(3) Uani 1 1 d . . . Br27 Br 0.88024(12) 0.11199(11) 0.04959(3) 0.0212(3) Uani 1 1 d . . . Br28 Br 0.78551(13) 0.41335(12) 0.08611(3) 0.0295(3) Uani 1 1 d . . . Br29 Br 0.52374(13) 0.25434(13) 0.06989(4) 0.0351(4) Uani 1 1 d . . . Br30 Br 0.70828(14) 0.39895(12) 0.00010(3) 0.0299(3) Uani 1 1 d . . . Al1 Al 0.0667(3) 0.4528(3) 0.19721(8) 0.0141(8) Uani 1 1 d . . . Al2 Al 0.6705(3) 0.8585(3) 0.16827(8) 0.0133(7) Uani 1 1 d . . . Al3 Al 0.4079(3) 0.5652(3) 0.31095(8) 0.0120(7) Uani 1 1 d . . . Al4 Al 0.7919(3) 0.1266(3) 0.33792(8) 0.0121(7) Uani 1 1 d . . . Al5 Al 0.4171(3) 0.8470(3) 0.45392(8) 0.0139(7) Uani 1 1 d . . . Al6 Al 0.7975(3) 0.6700(3) 0.45149(9) 0.0145(8) Uani 1 1 d . . . Al7 Al 1.1037(4) 0.1461(3) 0.04691(8) 0.0183(8) Uani 1 1 d . . . Al8 Al 0.7168(4) 0.3074(3) 0.05077(9) 0.0205(8) Uani 1 1 d . . . O1 O 0.4062(7) 0.5744(7) 0.12902(18) 0.0133(6) Uani 1 1 d U . . O2 O 0.3408(7) 0.6443(6) 0.18147(18) 0.0130(6) Uani 1 1 d U . . O3 O 0.2702(7) 0.7810(6) 0.13607(18) 0.0130(6) Uani 1 1 d U . . O4 O 0.0778(7) 0.3048(6) 0.32259(18) 0.0130(6) Uani 1 1 d U . . O5 O 0.2025(7) 0.1863(7) 0.36433(18) 0.0134(6) Uani 1 1 d U . . O6 O 0.0644(7) 0.3896(7) 0.37213(18) 0.0133(6) Uani 1 1 d U . . N1 N 0.2193(9) 0.6602(8) 0.0955(2) 0.0141(6) Uani 1 1 d U . . N2 N 0.4282(9) 0.7450(8) 0.0878(2) 0.0150(6) Uani 1 1 d U . . N3 N 0.1816(9) 0.8416(8) 0.1888(2) 0.0137(7) Uani 1 1 d U . . N4 N 0.4898(9) 0.4437(8) 0.1752(2) 0.0136(7) Uani 1 1 d U . . N5 N 0.0712(9) 0.2225(8) 0.4161(2) 0.0141(6) Uani 1 1 d U . . N6 N 0.2723(9) 0.3129(8) 0.4003(2) 0.0138(6) Uani 1 1 d U . . N7 N 0.2476(9) 0.1216(8) 0.3096(2) 0.0129(7) Uani 1 1 d U . . N8 N -0.0650(9) 0.5082(8) 0.3300(2) 0.0135(7) Uani 1 1 d U . . C1 C 0.1234(11) 0.7555(10) 0.0838(3) 0.0145(7) Uani 1 1 d U . . H1 H 0.1301 0.8380 0.0852 0.017 Uiso 1 1 calc R . . C2 C 0.0162(11) 0.7359(10) 0.0699(3) 0.0148(8) Uani 1 1 d U . . H2 H -0.0509 0.8038 0.0621 0.018 Uiso 1 1 calc R . . C3 C 0.0081(11) 0.6172(10) 0.0676(3) 0.0148(8) Uani 1 1 d U . . H3 H -0.0649 0.6018 0.0581 0.018 Uiso 1 1 calc R . . C4 C 0.1060(11) 0.5201(10) 0.0792(3) 0.0147(7) Uani 1 1 d U . . H4 H 0.1010 0.4371 0.0778 0.018 Uiso 1 1 calc R . . C5 C 0.2115(11) 0.5445(10) 0.0929(3) 0.0144(7) Uani 1 1 d U . . H5 H 0.2800 0.4775 0.1007 0.017 Uiso 1 1 calc R . . C6 C 0.4598(11) 0.8558(10) 0.0907(3) 0.0154(7) Uani 1 1 d U . . H6 H 0.4196 0.9027 0.1083 0.018 Uiso 1 1 calc R . . C7 C 0.5474(11) 0.8990(10) 0.0689(3) 0.0162(8) Uani 1 1 d U . . H7 H 0.5690 0.9755 0.0711 0.019 Uiso 1 1 calc R . . C8 C 0.6046(11) 0.8310(10) 0.0435(3) 0.0165(8) Uani 1 1 d U . . H8 H 0.6653 0.8612 0.0279 0.020 Uiso 1 1 calc R . . C9 C 0.5755(11) 0.7217(10) 0.0405(3) 0.0165(8) Uani 1 1 d U . . H9 H 0.6167 0.6743 0.0231 0.020 Uiso 1 1 calc R . . C10 C 0.4853(11) 0.6793(10) 0.0629(3) 0.0158(7) Uani 1 1 d U . . H10 H 0.4634 0.6030 0.0606 0.019 Uiso 1 1 calc R . . C11 C 0.1760(11) 0.8128(10) 0.2217(3) 0.0140(8) Uani 1 1 d U . . H11 H 0.2254 0.7355 0.2308 0.017 Uiso 1 1 calc R . . C12 C 0.0978(11) 0.8977(10) 0.2414(3) 0.0148(8) Uani 1 1 d U . . H12 H 0.0903 0.8785 0.2642 0.018 Uiso 1 1 calc R . . C13 C 0.0313(11) 1.0089(10) 0.2279(3) 0.0149(8) Uani 1 1 d U . . H13 H -0.0222 1.0674 0.2415 0.018 Uiso 1 1 calc R . . C14 C 0.0400(11) 1.0390(10) 0.1947(3) 0.0147(8) Uani 1 1 d U . . H14 H -0.0040 1.1183 0.1855 0.018 Uiso 1 1 calc R . . C15 C 0.1141(11) 0.9508(10) 0.1753(3) 0.0143(8) Uani 1 1 d U . . H15 H 0.1174 0.9672 0.1525 0.017 Uiso 1 1 calc R . . C16 C 0.5608(11) 0.3547(10) 0.1562(3) 0.0140(8) Uani 1 1 d U . . H16 H 0.5630 0.3706 0.1334 0.017 Uiso 1 1 calc R . . C17 C 0.6286(11) 0.2433(10) 0.1696(3) 0.0141(8) Uani 1 1 d U . . H17 H 0.6794 0.1839 0.1559 0.017 Uiso 1 1 calc R . . C18 C 0.6253(11) 0.2145(10) 0.2030(3) 0.0141(8) Uani 1 1 d U . . H18 H 0.6737 0.1373 0.2123 0.017 Uiso 1 1 calc R . . C19 C 0.5494(11) 0.3021(10) 0.2216(3) 0.0139(8) Uani 1 1 d U . . H19 H 0.5403 0.2847 0.2444 0.017 Uiso 1 1 calc R . . C20 C 0.4873(11) 0.4132(10) 0.2078(3) 0.0138(8) Uani 1 1 d U . . H20 H 0.4390 0.4737 0.2216 0.017 Uiso 1 1 calc R . . C21 C 0.0172(11) 0.2936(10) 0.4398(3) 0.0149(7) Uani 1 1 d U . . H21 H 0.0324 0.3744 0.4388 0.018 Uiso 1 1 calc R . . C22 C -0.0590(11) 0.2547(10) 0.4655(3) 0.0156(8) Uani 1 1 d U . . H22 H -0.0962 0.3078 0.4820 0.019 Uiso 1 1 calc R . . C23 C -0.0820(11) 0.1362(10) 0.4674(3) 0.0156(8) Uani 1 1 d U . . H23 H -0.1361 0.1075 0.4849 0.019 Uiso 1 1 calc R . . C24 C -0.0250(11) 0.0626(10) 0.4434(3) 0.0151(8) Uani 1 1 d U . . H24 H -0.0388 -0.0186 0.4438 0.018 Uiso 1 1 calc R . . C25 C 0.0526(11) 0.1076(10) 0.4184(3) 0.0145(7) Uani 1 1 d U . . H25 H 0.0948 0.0548 0.4022 0.017 Uiso 1 1 calc R . . C26 C 0.3754(11) 0.2231(10) 0.4086(3) 0.0142(7) Uani 1 1 d U . . H26 H 0.3773 0.1404 0.4048 0.017 Uiso 1 1 calc R . . C27 C 0.4806(11) 0.2470(10) 0.4226(3) 0.0147(8) Uani 1 1 d U . . H27 H 0.5536 0.1814 0.4287 0.018 Uiso 1 1 calc R . . C28 C 0.4779(11) 0.3661(10) 0.4275(3) 0.0149(8) Uani 1 1 d U . . H28 H 0.5480 0.3848 0.4375 0.018 Uiso 1 1 calc R . . C29 C 0.3721(11) 0.4588(10) 0.4177(3) 0.0147(7) Uani 1 1 d U . . H29 H 0.3706 0.5423 0.4205 0.018 Uiso 1 1 calc R . . C30 C 0.2716(11) 0.4335(10) 0.4043(3) 0.0142(7) Uani 1 1 d U . . H30 H 0.1994 0.4987 0.3975 0.017 Uiso 1 1 calc R . . C31 C 0.2433(11) 0.1568(10) 0.2783(3) 0.0133(8) Uani 1 1 d U . . H31 H 0.1871 0.2344 0.2715 0.016 Uiso 1 1 calc R . . C32 C 0.3168(10) 0.0856(9) 0.2552(3) 0.0135(8) Uani 1 1 d U . . H32 H 0.3101 0.1123 0.2329 0.016 Uiso 1 1 calc R . . C33 C 0.4004(11) -0.0252(10) 0.2648(3) 0.0135(8) Uani 1 1 d U . . H33 H 0.4542 -0.0758 0.2494 0.016 Uiso 1 1 calc R . . C34 C 0.4041(11) -0.0615(10) 0.2981(3) 0.0133(8) Uani 1 1 d U . . H34 H 0.4593 -0.1385 0.3056 0.016 Uiso 1 1 calc R . . C35 C 0.3280(10) 0.0146(9) 0.3195(3) 0.0129(8) Uani 1 1 d U . . H35 H 0.3323 -0.0092 0.3421 0.015 Uiso 1 1 calc R . . C36 C -0.0972(10) 0.6108(9) 0.3466(3) 0.0136(8) Uani 1 1 d U . . H36 H -0.0684 0.6050 0.3678 0.016 Uiso 1 1 calc R . . C37 C -0.1684(11) 0.7197(10) 0.3340(3) 0.0141(8) Uani 1 1 d U . . H37 H -0.1892 0.7904 0.3460 0.017 Uiso 1 1 calc R . . C38 C -0.2110(11) 0.7271(10) 0.3033(3) 0.0144(8) Uani 1 1 d U . . H38 H -0.2616 0.8039 0.2942 0.017 Uiso 1 1 calc R . . C40 C -0.1109(11) 0.5191(10) 0.2996(3) 0.0139(8) Uani 1 1 d U . . H40 H -0.0916 0.4476 0.2880 0.017 Uiso 1 1 calc R . . B1 B 0.3317(13) 0.6880(12) 0.1137(3) 0.0138(6) Uani 1 1 d U . . B2 B 0.2660(13) 0.7531(12) 0.1668(3) 0.0130(6) Uani 1 1 d U . . B3 B 0.4115(13) 0.5631(12) 0.1607(3) 0.0131(6) Uani 1 1 d U . . B4 B 0.1522(13) 0.2772(12) 0.3859(3) 0.0135(5) Uani 1 1 d U . . B5 B 0.1709(13) 0.2067(12) 0.3337(3) 0.0131(6) Uani 1 1 d U . . B6 B 0.0270(13) 0.3944(12) 0.3436(3) 0.0132(6) Uani 1 1 d U . . C39 C -0.1819(11) 0.6265(10) 0.2856(3) 0.0143(8) Uani 1 1 d U . . H39 H -0.2105 0.6319 0.2645 0.017 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0254(6) 0.0233(6) 0.0035(5) 0.0030(5) 0.0008(5) -0.0068(5) Br2 0.0220(6) 0.0297(7) 0.0325(8) 0.0061(6) 0.0051(6) -0.0134(6) Br3 0.0146(6) 0.0167(6) 0.0090(6) 0.0044(5) 0.0009(5) -0.0032(5) Br4 0.0202(6) 0.0185(6) 0.0211(7) -0.0074(6) 0.0004(6) -0.0001(5) Br5 0.0248(6) 0.0255(7) 0.0055(6) 0.0034(5) -0.0044(5) -0.0031(5) Br6 0.0149(6) 0.0255(6) 0.0152(6) -0.0075(6) -0.0008(5) 0.0014(5) Br7 0.0165(6) 0.0162(6) 0.0340(8) -0.0052(6) -0.0053(6) -0.0023(5) Br8 0.0269(6) 0.0184(6) 0.0087(6) 0.0029(5) 0.0085(5) -0.0023(5) Br9 0.0277(7) 0.0342(7) 0.0043(6) -0.0033(5) 0.0016(5) -0.0147(6) Br10 0.0154(6) 0.0253(7) 0.0407(9) -0.0023(7) 0.0080(6) 0.0011(6) Br11 0.0239(6) 0.0151(6) 0.0190(7) -0.0006(5) 0.0029(6) -0.0054(5) Br12 0.0239(6) 0.0227(6) 0.0068(6) -0.0007(5) -0.0001(5) -0.0074(5) Br13 0.0134(6) 0.0166(6) 0.0299(8) -0.0070(6) -0.0019(6) 0.0009(5) Br14 0.0190(6) 0.0178(6) 0.0161(6) -0.0062(5) 0.0038(5) -0.0047(5) Br15 0.0143(6) 0.0193(6) 0.0331(8) -0.0061(6) 0.0023(6) -0.0049(5) Br16 0.0345(8) 0.0501(9) 0.0046(6) 0.0016(6) 0.0046(6) 0.0042(7) Br17 0.0275(7) 0.0208(6) 0.0117(6) 0.0100(5) -0.0010(6) -0.0037(5) Br18 0.0248(6) 0.0201(6) 0.0118(6) -0.0036(5) 0.0047(5) -0.0015(5) Br19 0.0323(7) 0.0254(7) 0.0069(6) 0.0000(5) -0.0041(6) 0.0001(6) Br20 0.0205(6) 0.0172(6) 0.0221(7) 0.0006(6) 0.0032(6) -0.0040(5) Br21 0.0295(7) 0.0291(7) 0.0147(6) -0.0108(6) 0.0038(6) -0.0144(6) Br22 0.0322(7) 0.0384(8) 0.0096(6) 0.0039(6) -0.0056(6) -0.0058(6) Br23 0.0190(6) 0.0293(7) 0.0362(8) -0.0099(7) 0.0083(6) -0.0089(6) Br24 0.0354(7) 0.0221(7) 0.0125(6) -0.0005(6) 0.0029(6) -0.0006(6) Br25 0.0313(7) 0.0188(6) 0.0058(6) 0.0049(5) 0.0001(5) -0.0076(5) Br26 0.0478(8) 0.0320(7) 0.0057(6) 0.0017(6) -0.0082(6) -0.0099(7) Br27 0.0278(7) 0.0190(6) 0.0179(7) 0.0014(6) 0.0008(6) -0.0099(5) Br28 0.0355(7) 0.0388(8) 0.0204(7) -0.0151(7) 0.0115(6) -0.0204(7) Br29 0.0277(7) 0.0353(8) 0.0451(10) -0.0107(8) 0.0118(7) -0.0158(7) Br30 0.0389(8) 0.0289(7) 0.0187(7) 0.0038(6) -0.0020(6) -0.0042(6) Al1 0.0180(18) 0.0161(18) 0.0075(18) -0.0003(15) 0.0048(16) -0.0051(15) Al2 0.0137(17) 0.0155(18) 0.0095(18) -0.0001(15) 0.0000(15) -0.0019(15) Al3 0.0179(17) 0.0159(18) 0.0036(17) -0.0021(15) 0.0009(15) -0.0068(15) Al4 0.0129(17) 0.0154(17) 0.0062(17) -0.0019(15) 0.0037(15) -0.0015(15) Al5 0.0167(17) 0.0148(18) 0.0079(18) 0.0021(15) -0.0025(15) 0.0002(15) Al6 0.0148(17) 0.0175(18) 0.0110(18) -0.0049(16) 0.0005(16) -0.0024(15) Al7 0.031(2) 0.0210(19) 0.0021(17) 0.0005(16) -0.0025(16) -0.0042(17) Al8 0.0226(19) 0.024(2) 0.017(2) -0.0064(18) 0.0058(17) -0.0097(17) O1 0.0192(13) 0.0147(12) 0.0062(12) 0.0009(11) -0.0012(11) -0.0048(11) O2 0.0180(13) 0.0148(12) 0.0063(12) 0.0007(11) -0.0011(12) -0.0047(11) O3 0.0185(13) 0.0143(12) 0.0065(12) 0.0011(11) -0.0014(11) -0.0055(11) O4 0.0173(13) 0.0143(12) 0.0050(12) 0.0025(11) 0.0013(12) -0.0014(11) O5 0.0178(13) 0.0151(12) 0.0048(12) 0.0025(11) 0.0011(11) -0.0015(11) O6 0.0176(12) 0.0151(12) 0.0047(12) 0.0025(11) 0.0014(11) -0.0014(11) N1 0.0214(13) 0.0152(13) 0.0061(13) 0.0013(12) -0.0024(12) -0.0054(11) N2 0.0220(13) 0.0155(13) 0.0072(13) 0.0015(11) -0.0002(12) -0.0056(11) N3 0.0175(14) 0.0154(13) 0.0080(13) 0.0001(12) 0.0000(13) -0.0047(11) N4 0.0188(14) 0.0155(13) 0.0062(14) 0.0005(12) -0.0022(13) -0.0039(11) N5 0.0182(13) 0.0166(13) 0.0048(12) 0.0034(11) 0.0014(12) -0.0018(11) N6 0.0182(12) 0.0164(13) 0.0046(13) 0.0031(12) 0.0010(11) -0.0024(11) N7 0.0181(14) 0.0136(13) 0.0052(13) 0.0016(12) 0.0001(13) -0.0017(11) N8 0.0172(14) 0.0148(13) 0.0058(14) 0.0031(12) 0.0012(12) -0.0010(11) C1 0.0221(14) 0.0156(14) 0.0061(15) 0.0018(14) -0.0029(13) -0.0056(12) C2 0.0224(15) 0.0162(15) 0.0062(16) 0.0019(15) -0.0033(14) -0.0057(14) C3 0.0224(16) 0.0163(16) 0.0063(17) 0.0015(15) -0.0034(14) -0.0058(13) C4 0.0222(16) 0.0159(15) 0.0065(16) 0.0010(14) -0.0029(14) -0.0057(13) C5 0.0218(15) 0.0155(14) 0.0063(15) 0.0010(13) -0.0026(13) -0.0055(12) C6 0.0229(15) 0.0156(14) 0.0076(15) 0.0020(13) 0.0000(13) -0.0061(12) C7 0.0237(16) 0.0161(15) 0.0082(16) 0.0026(14) 0.0006(14) -0.0061(13) C8 0.0241(16) 0.0165(16) 0.0081(16) 0.0027(15) 0.0009(14) -0.0060(14) C9 0.0242(16) 0.0163(15) 0.0080(15) 0.0022(14) 0.0011(13) -0.0056(14) C10 0.0234(15) 0.0158(15) 0.0078(15) 0.0016(13) 0.0007(13) -0.0056(13) C11 0.0177(16) 0.0157(15) 0.0082(14) -0.0001(14) 0.0007(15) -0.0042(13) C12 0.0180(17) 0.0166(16) 0.0090(15) -0.0004(14) 0.0012(16) -0.0037(14) C13 0.0177(17) 0.0168(16) 0.0093(16) -0.0006(15) 0.0011(16) -0.0035(14) C14 0.0175(17) 0.0165(15) 0.0094(16) -0.0002(14) 0.0010(16) -0.0039(13) C15 0.0175(16) 0.0161(14) 0.0088(15) 0.0001(14) 0.0005(15) -0.0041(13) C16 0.0192(16) 0.0157(14) 0.0065(15) 0.0007(13) -0.0021(15) -0.0034(13) C17 0.0193(17) 0.0158(15) 0.0067(16) 0.0010(14) -0.0020(16) -0.0034(13) C18 0.0192(17) 0.0159(15) 0.0067(16) 0.0010(14) -0.0025(16) -0.0036(14) C19 0.0191(17) 0.0159(15) 0.0065(15) 0.0009(13) -0.0027(15) -0.0039(14) C20 0.0189(16) 0.0159(15) 0.0063(14) 0.0007(13) -0.0025(15) -0.0038(13) C21 0.0190(15) 0.0174(14) 0.0052(14) 0.0033(13) 0.0020(13) -0.0013(13) C22 0.0194(16) 0.0183(15) 0.0056(15) 0.0036(14) 0.0023(13) -0.0014(14) C23 0.0193(16) 0.0184(16) 0.0056(15) 0.0042(14) 0.0021(14) -0.0016(14) C24 0.0190(16) 0.0177(15) 0.0053(15) 0.0044(13) 0.0019(14) -0.0018(13) C25 0.0187(15) 0.0170(14) 0.0051(14) 0.0039(13) 0.0016(13) -0.0020(13) C26 0.0182(14) 0.0173(14) 0.0050(15) 0.0034(14) 0.0008(13) -0.0026(12) C27 0.0184(14) 0.0180(15) 0.0056(16) 0.0035(15) 0.0007(13) -0.0031(13) C28 0.0186(15) 0.0184(16) 0.0059(16) 0.0032(15) 0.0009(14) -0.0035(13) C29 0.0186(15) 0.0179(15) 0.0057(16) 0.0029(14) 0.0011(14) -0.0035(13) C30 0.0184(14) 0.0170(14) 0.0053(15) 0.0031(13) 0.0013(13) -0.0032(12) C31 0.0187(15) 0.0138(15) 0.0052(13) 0.0011(13) -0.0001(15) -0.0011(13) C32 0.0192(16) 0.0138(16) 0.0054(14) 0.0008(14) -0.0002(16) -0.0011(14) C33 0.0192(17) 0.0136(16) 0.0058(15) 0.0007(15) 0.0000(16) -0.0012(14) C34 0.0189(16) 0.0135(15) 0.0058(15) 0.0011(14) -0.0002(16) -0.0016(13) C35 0.0184(15) 0.0133(14) 0.0053(14) 0.0014(13) -0.0002(15) -0.0019(12) C36 0.0172(16) 0.0145(14) 0.0062(15) 0.0033(13) 0.0010(14) -0.0011(13) C37 0.0174(17) 0.0149(14) 0.0068(16) 0.0037(14) 0.0013(15) -0.0007(14) C38 0.0177(17) 0.0155(15) 0.0068(16) 0.0042(14) 0.0011(15) -0.0005(14) C40 0.0175(16) 0.0153(14) 0.0059(15) 0.0034(13) 0.0009(13) -0.0008(13) B1 0.0202(12) 0.0149(12) 0.0064(12) 0.0012(10) -0.0014(11) -0.0052(10) B2 0.0178(13) 0.0147(12) 0.0067(12) 0.0007(11) -0.0010(12) -0.0049(11) B3 0.0185(13) 0.0148(12) 0.0061(12) 0.0006(11) -0.0015(12) -0.0046(10) B4 0.0179(12) 0.0156(11) 0.0046(11) 0.0028(10) 0.0012(10) -0.0017(10) B5 0.0176(13) 0.0143(12) 0.0050(12) 0.0022(11) 0.0010(12) -0.0014(11) B6 0.0173(13) 0.0147(12) 0.0050(12) 0.0025(11) 0.0012(11) -0.0012(11) C39 0.0175(17) 0.0157(15) 0.0064(16) 0.0040(14) 0.0010(14) -0.0007(14) _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 Br1 Al1 2.298(4) . ? Br2 Al1 2.273(3) . ? Br3 Al1 2.278(4) . ? Br4 Al1 2.297(3) . ? Br5 Al2 2.285(4) . ? Br6 Al2 2.307(3) . ? Br7 Al2 2.276(3) . ? Br8 Al2 2.295(4) . ? Br9 Al3 2.266(3) . ? Br10 Al3 2.283(3) . ? Br11 Al3 2.291(3) . ? Br12 Al3 2.304(3) . ? Br13 Al4 2.303(3) . ? Br14 Al4 2.283(3) . ? Br15 Al4 2.280(3) . ? Br16 Al4 2.279(4) . ? Br17 Al5 2.253(4) . ? Br18 Al5 2.258(3) . ? Br19 Al5 2.259(4) . ? Br20 Al6 2.405(4) . ? Br20 Al5 2.428(4) . ? Br21 Al6 2.240(3) . ? Br22 Al6 2.249(4) . ? Br23 Al6 2.281(4) . ? Br24 Al7 2.259(4) . ? Br25 Al7 2.252(4) . ? Br26 Al7 2.253(4) . ? Br27 Al8 2.419(4) . ? Br27 Al7 2.428(4) . ? Br28 Al8 2.258(4) . ? Br29 Al8 2.267(4) . ? Br30 Al8 2.242(4) . ? O1 B3 1.318(14) . ? O1 B1 1.435(15) . ? O2 B3 1.355(14) . ? O2 B2 1.388(15) . ? O3 B2 1.283(15) . ? O3 B1 1.461(14) . ? O4 B5 1.345(14) . ? O4 B6 1.377(14) . ? O5 B5 1.334(15) . ? O5 B4 1.403(14) . ? O6 B6 1.279(15) . ? O6 B4 1.459(15) . ? N1 C5 1.332(13) . ? N1 C1 1.351(14) . ? N1 B1 1.561(15) . ? N2 C10 1.346(13) . ? N2 C6 1.376(13) . ? N2 B1 1.582(15) . ? N3 C15 1.345(14) . ? N3 C11 1.372(14) . ? N3 B2 1.487(15) . ? N4 C16 1.363(13) . ? N4 C20 1.366(14) . ? N4 B3 1.483(16) . ? N5 C21 1.332(13) . ? N5 C25 1.335(13) . ? N5 B4 1.588(15) . ? N6 C26 1.321(14) . ? N6 C30 1.374(13) . ? N6 B4 1.587(15) . ? N7 C31 1.325(14) . ? N7 C35 1.331(13) . ? N7 B5 1.492(15) . ? N8 C36 1.362(13) . ? N8 C40 1.379(14) . ? N8 B6 1.487(16) . ? C1 C2 1.377(15) . ? C1 H1 0.9500 . ? C2 C3 1.363(14) . ? C2 H2 0.9500 . ? C3 C4 1.374(15) . ? C3 H3 0.9500 . ? C4 C5 1.380(15) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.355(15) . ? C6 H6 0.9500 . ? C7 C8 1.373(15) . ? C7 H7 0.9500 . ? C8 C9 1.349(14) . ? C8 H8 0.9500 . ? C9 C10 1.382(15) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.376(14) . ? C11 H11 0.9500 . ? C12 C13 1.357(15) . ? C12 H12 0.9500 . ? C13 C14 1.387(15) . ? C13 H13 0.9500 . ? C14 C15 1.378(14) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.361(15) . ? C16 H16 0.9500 . ? C17 C18 1.389(15) . ? C17 H17 0.9500 . ? C18 C19 1.362(14) . ? C18 H18 0.9500 . ? C19 C20 1.346(15) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.360(14) . ? C21 H21 0.9500 . ? C22 C23 1.394(15) . ? C22 H22 0.9500 . ? C23 C24 1.362(14) . ? C23 H23 0.9500 . ? C24 C25 1.375(14) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.381(15) . ? C26 H26 0.9500 . ? C27 C28 1.362(14) . ? C27 H27 0.9500 . ? C28 C29 1.374(15) . ? C28 H28 0.9500 . ? C29 C30 1.332(15) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.366(14) . ? C31 H31 0.9500 . ? C32 C33 1.372(15) . ? C32 H32 0.9500 . ? C33 C34 1.402(15) . ? C33 H33 0.9500 . ? C34 C35 1.358(14) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.342(15) . ? C36 H36 0.9500 . ? C37 C38 1.386(15) . ? C37 H37 0.9500 . ? C38 C39 1.370(14) . ? C38 H38 0.9500 . ? C40 C39 1.351(15) . ? C40 H40 0.9500 . ? C39 H39 0.9500 . ? 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 Al6 Br20 Al5 109.91(12) . . ? Al8 Br27 Al7 110.15(12) . . ? Br2 Al1 Br3 111.27(15) . . ? Br2 Al1 Br4 110.13(14) . . ? Br3 Al1 Br4 109.39(14) . . ? Br2 Al1 Br1 109.68(14) . . ? Br3 Al1 Br1 108.14(14) . . ? Br4 Al1 Br1 108.17(15) . . ? Br7 Al2 Br5 114.46(16) . . ? Br7 Al2 Br8 109.34(14) . . ? Br5 Al2 Br8 108.70(14) . . ? Br7 Al2 Br6 108.17(14) . . ? Br5 Al2 Br6 106.98(14) . . ? Br8 Al2 Br6 109.07(15) . . ? Br9 Al3 Br10 109.57(13) . . ? Br9 Al3 Br11 110.69(15) . . ? Br10 Al3 Br11 109.12(13) . . ? Br9 Al3 Br12 108.00(13) . . ? Br10 Al3 Br12 107.99(15) . . ? Br11 Al3 Br12 111.42(13) . . ? Br16 Al4 Br15 112.17(15) . . ? Br16 Al4 Br14 109.24(14) . . ? Br15 Al4 Br14 110.48(13) . . ? Br16 Al4 Br13 107.12(13) . . ? Br15 Al4 Br13 109.27(14) . . ? Br14 Al4 Br13 108.45(14) . . ? Br17 Al5 Br18 114.33(15) . . ? Br17 Al5 Br19 112.47(14) . . ? Br18 Al5 Br19 111.97(15) . . ? Br17 Al5 Br20 109.72(14) . . ? Br18 Al5 Br20 101.63(13) . . ? Br19 Al5 Br20 105.80(14) . . ? Br21 Al6 Br22 113.85(15) . . ? Br21 Al6 Br23 111.78(14) . . ? Br22 Al6 Br23 112.54(15) . . ? Br21 Al6 Br20 105.76(14) . . ? Br22 Al6 Br20 109.65(14) . . ? Br23 Al6 Br20 102.38(14) . . ? Br25 Al7 Br26 114.41(15) . . ? Br25 Al7 Br24 113.51(15) . . ? Br26 Al7 Br24 111.75(16) . . ? Br25 Al7 Br27 106.98(15) . . ? Br26 Al7 Br27 106.79(15) . . ? Br24 Al7 Br27 102.31(14) . . ? Br30 Al8 Br28 114.39(16) . . ? Br30 Al8 Br29 112.48(17) . . ? Br28 Al8 Br29 111.37(16) . . ? Br30 Al8 Br27 107.83(14) . . ? Br28 Al8 Br27 105.51(16) . . ? Br29 Al8 Br27 104.43(15) . . ? B3 O1 B1 119.0(9) . . ? B3 O2 B2 114.8(9) . . ? B2 O3 B1 121.1(10) . . ? B5 O4 B6 116.3(9) . . ? B5 O5 B4 120.3(10) . . ? B6 O6 B4 120.1(9) . . ? C5 N1 C1 119.3(9) . . ? C5 N1 B1 121.3(10) . . ? C1 N1 B1 119.3(9) . . ? C10 N2 C6 119.2(10) . . ? C10 N2 B1 118.1(9) . . ? C6 N2 B1 122.7(9) . . ? C15 N3 C11 121.8(9) . . ? C15 N3 B2 117.5(9) . . ? C11 N3 B2 120.7(10) . . ? C16 N4 C20 116.4(10) . . ? C16 N4 B3 121.2(9) . . ? C20 N4 B3 122.2(9) . . ? C21 N5 C25 118.1(10) . . ? C21 N5 B4 119.5(9) . . ? C25 N5 B4 122.5(9) . . ? C26 N6 C30 119.7(10) . . ? C26 N6 B4 118.3(9) . . ? C30 N6 B4 121.9(9) . . ? C31 N7 C35 119.7(9) . . ? C31 N7 B5 119.8(10) . . ? C35 N7 B5 120.4(9) . . ? C36 N8 C40 117.6(10) . . ? C36 N8 B6 119.2(9) . . ? C40 N8 B6 122.9(9) . . ? N1 C1 C2 121.6(10) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 118.9(11) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.7(10) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 119.3(10) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.2(11) . . ? N1 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C7 C6 N2 121.0(10) . . ? C7 C6 H6 119.5 . . ? N2 C6 H6 119.5 . . ? C6 C7 C8 119.2(10) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C9 C8 C7 120.6(11) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 119.6(10) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 120.5(10) . . ? N2 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? N3 C11 C12 118.9(11) . . ? N3 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C13 C12 C11 119.5(11) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 121.4(10) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C15 C14 C13 118.2(11) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? N3 C15 C14 120.0(11) . . ? N3 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 N4 121.0(10) . . ? C17 C16 H16 119.5 . . ? N4 C16 H16 119.5 . . ? C16 C17 C18 121.5(10) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C19 C18 C17 116.9(11) . . ? C19 C18 H18 121.5 . . ? C17 C18 H18 121.5 . . ? C20 C19 C18 120.3(11) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 N4 123.6(10) . . ? C19 C20 H20 118.2 . . ? N4 C20 H20 118.2 . . ? N5 C21 C22 122.4(10) . . ? N5 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C21 C22 C23 119.3(10) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 118.3(11) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C23 C24 C25 119.0(11) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? N5 C25 C24 122.8(10) . . ? N5 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? N6 C26 C27 121.4(10) . . ? N6 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 118.9(11) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C27 C28 C29 119.0(11) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C30 C29 C28 121.1(11) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 N6 119.9(11) . . ? C29 C30 H30 120.0 . . ? N6 C30 H30 120.0 . . ? N7 C31 C32 122.3(11) . . ? N7 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? C31 C32 C33 119.1(11) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C32 C33 C34 118.1(10) . . ? C32 C33 H33 121.0 . . ? C34 C33 H33 121.0 . . ? C35 C34 C33 119.4(11) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? N7 C35 C34 121.4(10) . . ? N7 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C37 C36 N8 121.9(10) . . ? C37 C36 H36 119.1 . . ? N8 C36 H36 119.1 . . ? C36 C37 C38 118.8(11) . . ? C36 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? C39 C38 C37 121.6(11) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C39 C40 N8 123.1(10) . . ? C39 C40 H40 118.4 . . ? N8 C40 H40 118.4 . . ? O1 B1 O3 113.9(10) . . ? O1 B1 N1 109.3(9) . . ? O3 B1 N1 108.3(9) . . ? O1 B1 N2 108.9(9) . . ? O3 B1 N2 108.2(9) . . ? N1 B1 N2 108.2(9) . . ? O3 B2 O2 123.6(10) . . ? O3 B2 N3 120.1(11) . . ? O2 B2 N3 116.3(10) . . ? O1 B3 O2 126.1(11) . . ? O1 B3 N4 116.5(10) . . ? O2 B3 N4 116.9(10) . . ? O5 B4 O6 114.8(10) . . ? O5 B4 N6 109.5(9) . . ? O6 B4 N6 109.0(9) . . ? O5 B4 N5 109.9(9) . . ? O6 B4 N5 107.6(9) . . ? N6 B4 N5 105.6(9) . . ? O5 B5 O4 123.3(11) . . ? O5 B5 N7 119.0(11) . . ? O4 B5 N7 117.5(10) . . ? O6 B6 O4 124.0(11) . . ? O6 B6 N8 119.9(10) . . ? O4 B6 N8 115.7(10) . . ? C40 C39 C38 117.1(11) . . ? C40 C39 H39 121.5 . . ? C38 C39 H39 121.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Al6 Br20 Al5 Br17 23.83(18) . . . . ? Al6 Br20 Al5 Br18 145.20(13) . . . . ? Al6 Br20 Al5 Br19 -97.72(15) . . . . ? Al5 Br20 Al6 Br21 51.49(17) . . . . ? Al5 Br20 Al6 Br22 -71.66(16) . . . . ? Al5 Br20 Al6 Br23 168.66(13) . . . . ? Al8 Br27 Al7 Br25 -36.94(17) . . . . ? Al8 Br27 Al7 Br26 85.98(17) . . . . ? Al8 Br27 Al7 Br24 -156.51(14) . . . . ? Al7 Br27 Al8 Br30 78.57(16) . . . . ? Al7 Br27 Al8 Br28 -44.08(18) . . . . ? Al7 Br27 Al8 Br29 -161.59(14) . . . . ? C5 N1 C1 C2 1.4(15) . . . . ? B1 N1 C1 C2 -174.7(10) . . . . ? N1 C1 C2 C3 -0.8(16) . . . . ? C1 C2 C3 C4 0.2(16) . . . . ? C2 C3 C4 C5 -0.3(16) . . . . ? C1 N1 C5 C4 -1.5(16) . . . . ? B1 N1 C5 C4 174.6(10) . . . . ? C3 C4 C5 N1 0.9(16) . . . . ? C10 N2 C6 C7 -0.2(17) . . . . ? B1 N2 C6 C7 177.0(11) . . . . ? N2 C6 C7 C8 0.3(18) . . . . ? C6 C7 C8 C9 -0.8(18) . . . . ? C7 C8 C9 C10 1.2(18) . . . . ? C6 N2 C10 C9 0.6(17) . . . . ? B1 N2 C10 C9 -176.8(10) . . . . ? C8 C9 C10 N2 -1.1(18) . . . . ? C15 N3 C11 C12 0.8(15) . . . . ? B2 N3 C11 C12 179.4(10) . . . . ? N3 C11 C12 C13 -2.0(16) . . . . ? C11 C12 C13 C14 0.3(17) . . . . ? C12 C13 C14 C15 2.5(16) . . . . ? C11 N3 C15 C14 2.1(16) . . . . ? B2 N3 C15 C14 -176.5(10) . . . . ? C13 C14 C15 N3 -3.7(16) . . . . ? C20 N4 C16 C17 -2.1(15) . . . . ? B3 N4 C16 C17 -177.5(10) . . . . ? N4 C16 C17 C18 1.8(17) . . . . ? C16 C17 C18 C19 1.0(16) . . . . ? C17 C18 C19 C20 -3.4(16) . . . . ? C18 C19 C20 N4 3.2(17) . . . . ? C16 N4 C20 C19 -0.4(16) . . . . ? B3 N4 C20 C19 175.0(10) . . . . ? C25 N5 C21 C22 -2.2(17) . . . . ? B4 N5 C21 C22 176.6(10) . . . . ? N5 C21 C22 C23 0.0(18) . . . . ? C21 C22 C23 C24 1.0(17) . . . . ? C22 C23 C24 C25 0.1(17) . . . . ? C21 N5 C25 C24 3.3(17) . . . . ? B4 N5 C25 C24 -175.3(10) . . . . ? C23 C24 C25 N5 -2.3(17) . . . . ? C30 N6 C26 C27 3.0(15) . . . . ? B4 N6 C26 C27 -177.0(10) . . . . ? N6 C26 C27 C28 -0.9(16) . . . . ? C26 C27 C28 C29 -1.4(16) . . . . ? C27 C28 C29 C30 1.7(16) . . . . ? C28 C29 C30 N6 0.4(16) . . . . ? C26 N6 C30 C29 -2.7(15) . . . . ? B4 N6 C30 C29 177.3(10) . . . . ? C35 N7 C31 C32 1.5(16) . . . . ? B5 N7 C31 C32 176.6(10) . . . . ? N7 C31 C32 C33 -1.5(17) . . . . ? C31 C32 C33 C34 1.4(16) . . . . ? C32 C33 C34 C35 -1.5(16) . . . . ? C31 N7 C35 C34 -1.5(16) . . . . ? B5 N7 C35 C34 -176.6(10) . . . . ? C33 C34 C35 N7 1.5(16) . . . . ? C40 N8 C36 C37 -1.4(15) . . . . ? B6 N8 C36 C37 173.0(10) . . . . ? N8 C36 C37 C38 0.5(16) . . . . ? C36 C37 C38 C39 -0.1(17) . . . . ? C36 N8 C40 C39 2.0(16) . . . . ? B6 N8 C40 C39 -172.2(10) . . . . ? B3 O1 B1 O3 0.8(14) . . . . ? B3 O1 B1 N1 -120.4(11) . . . . ? B3 O1 B1 N2 121.6(10) . . . . ? B2 O3 B1 O1 -11.2(15) . . . . ? B2 O3 B1 N1 110.6(11) . . . . ? B2 O3 B1 N2 -132.4(10) . . . . ? C5 N1 B1 O1 -6.9(14) . . . . ? C1 N1 B1 O1 169.1(9) . . . . ? C5 N1 B1 O3 -131.5(10) . . . . ? C1 N1 B1 O3 44.6(13) . . . . ? C5 N1 B1 N2 111.5(11) . . . . ? C1 N1 B1 N2 -72.4(12) . . . . ? C10 N2 B1 O1 62.3(13) . . . . ? C6 N2 B1 O1 -115.0(11) . . . . ? C10 N2 B1 O3 -173.5(10) . . . . ? C6 N2 B1 O3 9.3(15) . . . . ? C10 N2 B1 N1 -56.4(13) . . . . ? C6 N2 B1 N1 126.4(10) . . . . ? B1 O3 B2 O2 13.9(17) . . . . ? B1 O3 B2 N3 -168.5(10) . . . . ? B3 O2 B2 O3 -5.4(16) . . . . ? B3 O2 B2 N3 177.0(9) . . . . ? C15 N3 B2 O3 -1.5(16) . . . . ? C11 N3 B2 O3 179.9(10) . . . . ? C15 N3 B2 O2 176.3(9) . . . . ? C11 N3 B2 O2 -2.4(15) . . . . ? B1 O1 B3 O2 7.7(17) . . . . ? B1 O1 B3 N4 180.0(9) . . . . ? B2 O2 B3 O1 -5.9(17) . . . . ? B2 O2 B3 N4 -178.2(9) . . . . ? C16 N4 B3 O1 5.0(16) . . . . ? C20 N4 B3 O1 -170.1(10) . . . . ? C16 N4 B3 O2 178.0(9) . . . . ? C20 N4 B3 O2 2.9(16) . . . . ? B5 O5 B4 O6 0.9(15) . . . . ? B5 O5 B4 N6 -122.1(11) . . . . ? B5 O5 B4 N5 122.3(11) . . . . ? B6 O6 B4 O5 7.7(15) . . . . ? B6 O6 B4 N6 130.9(10) . . . . ? B6 O6 B4 N5 -115.0(11) . . . . ? C26 N6 B4 O5 -41.5(13) . . . . ? C30 N6 B4 O5 138.5(10) . . . . ? C26 N6 B4 O6 -167.8(9) . . . . ? C30 N6 B4 O6 12.2(13) . . . . ? C26 N6 B4 N5 76.8(11) . . . . ? C30 N6 B4 N5 -103.1(11) . . . . ? C21 N5 B4 O5 178.7(10) . . . . ? C25 N5 B4 O5 -2.6(15) . . . . ? C21 N5 B4 O6 -55.6(13) . . . . ? C25 N5 B4 O6 123.1(11) . . . . ? C21 N5 B4 N6 60.7(12) . . . . ? C25 N5 B4 N6 -120.6(11) . . . . ? B4 O5 B5 O4 -9.1(17) . . . . ? B4 O5 B5 N7 166.9(10) . . . . ? B6 O4 B5 O5 8.3(16) . . . . ? B6 O4 B5 N7 -167.7(10) . . . . ? C31 N7 B5 O5 -162.2(10) . . . . ? C35 N7 B5 O5 12.8(16) . . . . ? C31 N7 B5 O4 14.0(16) . . . . ? C35 N7 B5 O4 -171.0(9) . . . . ? B4 O6 B6 O4 -8.9(17) . . . . ? B4 O6 B6 N8 178.6(9) . . . . ? B5 O4 B6 O6 1.0(17) . . . . ? B5 O4 B6 N8 173.8(9) . . . . ? C36 N8 B6 O6 6.8(16) . . . . ? C40 N8 B6 O6 -179.0(10) . . . . ? C36 N8 B6 O4 -166.3(9) . . . . ? C40 N8 B6 O4 7.9(16) . . . . ? N8 C40 C39 C38 -1.6(16) . . . . ? C37 C38 C39 C40 0.6(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.245 _refine_diff_density_min -2.036 _refine_diff_density_rms 0.275