# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_dw1248 _database_code_depnum_ccdc_archive 'CCDC 907276' #TrackingRef 'dw1248.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H30 Al B2 Li N2 O' _chemical_formula_sum 'C8 H30 Al B2 Li N2 O' _chemical_formula_weight 225.88 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' Li Li -0.0003 0.0001 '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' Al Al 0.0645 0.0514 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0663(3) _cell_length_b 12.0196(3) _cell_length_c 13.9142(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.849(1) _cell_angle_gamma 90.00 _cell_volume 1679.72(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8630 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; The -BH3 and Al-H hydrogen atoms were allowed to refine freely (not AFIXed with 137). ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 13233 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.05 _diffrn_reflns_theta_max 30.02 _reflns_number_total 4803 _reflns_number_gt 3235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement '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^)+(0.1126P)^2^+0.0234P] 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_number_reflns 4803 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1881 _refine_ls_wR_factor_gt 0.1730 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 Al1 Al 0.20717(4) 0.15764(3) 0.77735(3) 0.03153(16) Uani 1 1 d . . . H1A H 0.1036(17) 0.2350(14) 0.8009(12) 0.047 Uiso 1 1 d . . . H1B H 0.3300(17) 0.2066(14) 0.7372(12) 0.047 Uiso 1 1 d . . . N1 N 0.13559(11) 0.06831(9) 0.66941(8) 0.0338(3) Uani 1 1 d . . . B1 B 0.03115(16) -0.01899(13) 0.70395(13) 0.0360(4) Uani 1 1 d . . . H11 H 0.0812(18) -0.0770(15) 0.7561(13) 0.054 Uiso 1 1 d . . . H12 H -0.0212(18) -0.0638(15) 0.6397(13) 0.054 Uiso 1 1 d . . . H13 H -0.0382(18) 0.0216(15) 0.7487(13) 0.054 Uiso 1 1 d . . . O1 O -0.13213(12) -0.25912(11) 0.74768(10) 0.0578(4) Uani 1 1 d . . . Li1 Li 0.0257(2) -0.21837(19) 0.68508(19) 0.0396(5) Uani 1 1 d . . . N2 N 0.27066(12) 0.07462(10) 0.88953(9) 0.0366(3) Uani 1 1 d . . . B2 B 0.36689(19) 0.16618(14) 0.94161(14) 0.0413(4) Uani 1 1 d . . . H21 H 0.373(2) 0.1524(15) 1.0172(15) 0.062 Uiso 1 1 d . . . H22 H 0.472(2) 0.1597(15) 0.9128(15) 0.062 Uiso 1 1 d . . . H23 H 0.3340(19) 0.2498(16) 0.9319(14) 0.062 Uiso 1 1 d . . . C11 C 0.24020(16) 0.01160(13) 0.61786(12) 0.0447(4) Uani 1 1 d . . . H11A H 0.1992 -0.0277 0.5617 0.067 Uiso 1 1 calc R . . H11B H 0.2870 -0.0419 0.6611 0.067 Uiso 1 1 calc R . . H11C H 0.3036 0.0668 0.5966 0.067 Uiso 1 1 calc R . . C12 C 0.06581(18) 0.14841(12) 0.60207(12) 0.0467(4) Uani 1 1 d . . . H12A H 0.0290 0.1086 0.5448 0.070 Uiso 1 1 calc R . . H12B H 0.1290 0.2049 0.5828 0.070 Uiso 1 1 calc R . . H12C H -0.0065 0.1845 0.6341 0.070 Uiso 1 1 calc R . . C21 C 0.34771(18) -0.02829(12) 0.87457(13) 0.0541(5) Uani 1 1 d . . . H21A H 0.3900 -0.0533 0.9363 0.081 Uiso 1 1 calc R . . H21B H 0.4164 -0.0132 0.8296 0.081 Uiso 1 1 calc R . . H21C H 0.2877 -0.0864 0.8479 0.081 Uiso 1 1 calc R . . C22 C 0.1605(2) 0.04802(16) 0.95134(13) 0.0572(5) Uani 1 1 d . . . H22A H 0.1975 0.0234 1.0147 0.086 Uiso 1 1 calc R . . H22B H 0.1055 -0.0114 0.9213 0.086 Uiso 1 1 calc R . . H22C H 0.1058 0.1145 0.9588 0.086 Uiso 1 1 calc R . . C31 C -0.2659(2) -0.2439(3) 0.7161(2) 0.0979(9) Uani 1 1 d . . . H31A H -0.3005 -0.1772 0.7479 0.117 Uiso 1 1 calc R . . H31B H -0.3179 -0.3089 0.7361 0.117 Uiso 1 1 calc R . . C32 C -0.2859(3) -0.2309(3) 0.6144(2) 0.1077(11) Uani 1 1 d . . . H32A H -0.3815 -0.2293 0.5959 0.162 Uiso 1 1 calc R . . H32B H -0.2447 -0.2933 0.5822 0.162 Uiso 1 1 calc R . . H32C H -0.2451 -0.1610 0.5951 0.162 Uiso 1 1 calc R . . C33 C -0.1163(3) -0.2759(3) 0.8531(2) 0.1046(10) Uani 1 1 d . . . H33A H -0.0268 -0.2497 0.8771 0.126 Uiso 1 1 calc R . . H33B H -0.1830 -0.2300 0.8841 0.126 Uiso 1 1 calc R . . C34 C -0.1315(3) -0.3884(4) 0.8806(3) 0.1500(18) Uani 1 1 d . . . H34A H -0.0952 -0.3986 0.9471 0.225 Uiso 1 1 calc R . . H34B H -0.0837 -0.4366 0.8378 0.225 Uiso 1 1 calc R . . H34C H -0.2263 -0.4080 0.8759 0.225 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 Al1 0.0330(3) 0.0225(2) 0.0383(3) -0.00087(14) -0.00299(17) 0.00079(13) N1 0.0346(6) 0.0281(5) 0.0380(6) -0.0015(4) -0.0024(5) 0.0007(4) B1 0.0333(8) 0.0301(8) 0.0443(9) -0.0030(6) 0.0001(7) -0.0014(6) O1 0.0425(7) 0.0623(8) 0.0702(9) 0.0053(6) 0.0156(6) -0.0123(5) Li1 0.0352(13) 0.0333(12) 0.0502(15) 0.0002(10) 0.0028(10) -0.0002(9) N2 0.0411(7) 0.0303(6) 0.0375(7) 0.0030(4) -0.0032(5) -0.0034(5) B2 0.0466(10) 0.0353(9) 0.0405(9) 0.0017(6) -0.0075(7) -0.0047(7) C11 0.0420(8) 0.0414(8) 0.0517(10) -0.0116(6) 0.0106(7) -0.0042(6) C12 0.0576(10) 0.0377(8) 0.0426(9) 0.0052(6) -0.0130(7) -0.0022(6) C21 0.0626(11) 0.0309(8) 0.0654(11) 0.0010(7) -0.0218(9) 0.0091(7) C22 0.0614(11) 0.0666(11) 0.0435(10) 0.0056(8) 0.0039(8) -0.0243(9) C31 0.0495(13) 0.138(2) 0.107(2) 0.0287(18) 0.0133(13) -0.0017(15) C32 0.0717(17) 0.154(3) 0.096(2) 0.0183(19) -0.0049(15) -0.0330(18) C33 0.094(2) 0.149(3) 0.0742(18) -0.0184(17) 0.0332(15) -0.0167(19) C34 0.076(2) 0.228(4) 0.146(3) 0.113(3) 0.012(2) -0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N2 1.9253(12) . ? Al1 N1 1.9449(12) . ? Al1 Li1 3.088(2) 2_556 ? Al1 H1A 1.451(17) . ? Al1 H1B 1.509(17) . ? N1 C11 1.4795(19) . ? N1 C12 1.4866(19) . ? N1 B1 1.5828(19) . ? B1 H11 1.103(19) . ? B1 H12 1.142(18) . ? B1 H13 1.082(17) . ? O1 C31 1.400(3) . ? O1 C33 1.479(3) . ? O1 Li1 1.926(3) . ? Li1 B2 2.541(3) 2_546 ? Li1 Al1 3.088(2) 2_546 ? Li1 H11 2.026(18) . ? Li1 H12 2.008(18) . ? N2 C21 1.482(2) . ? N2 C22 1.483(2) . ? N2 B2 1.606(2) . ? B2 Li1 2.541(3) 2_556 ? B2 H21 1.06(2) . ? B2 H22 1.16(2) . ? B2 H23 1.06(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 C32 1.424(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.417(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al1 N1 115.19(6) . . ? N2 Al1 Li1 82.82(6) . 2_556 ? N1 Al1 Li1 132.10(6) . 2_556 ? N2 Al1 H1A 110.7(7) . . ? N1 Al1 H1A 107.1(7) . . ? Li1 Al1 H1A 106.5(7) 2_556 . ? N2 Al1 H1B 105.4(7) . . ? N1 Al1 H1B 101.5(7) . . ? Li1 Al1 H1B 31.7(7) 2_556 . ? H1A Al1 H1B 116.9(9) . . ? C11 N1 C12 108.32(13) . . ? C11 N1 B1 110.53(11) . . ? C12 N1 B1 108.99(11) . . ? C11 N1 Al1 112.95(9) . . ? C12 N1 Al1 105.31(9) . . ? B1 N1 Al1 110.53(9) . . ? N1 B1 H11 109.6(9) . . ? N1 B1 H12 110.8(9) . . ? H11 B1 H12 112.6(13) . . ? N1 B1 H13 110.0(10) . . ? H11 B1 H13 101.0(13) . . ? H12 B1 H13 112.4(13) . . ? C31 O1 C33 111.50(19) . . ? C31 O1 Li1 129.07(17) . . ? C33 O1 Li1 116.49(16) . . ? O1 Li1 B2 125.25(12) . 2_546 ? O1 Li1 Al1 122.42(11) . 2_546 ? B2 Li1 Al1 56.48(6) 2_546 2_546 ? O1 Li1 H11 101.6(5) . . ? B2 Li1 H11 132.9(5) 2_546 . ? Al1 Li1 H11 96.5(5) 2_546 . ? O1 Li1 H12 101.2(5) . . ? B2 Li1 H12 112.9(5) 2_546 . ? Al1 Li1 H12 133.1(5) 2_546 . ? H11 Li1 H12 55.2(7) . . ? C21 N2 C22 108.68(13) . . ? C21 N2 B2 109.25(12) . . ? C22 N2 B2 109.75(13) . . ? C21 N2 Al1 117.84(10) . . ? C22 N2 Al1 111.19(10) . . ? B2 N2 Al1 99.67(9) . . ? N2 B2 Li1 109.45(12) . 2_556 ? N2 B2 H21 109.4(11) . . ? Li1 B2 H21 140.6(11) 2_556 . ? N2 B2 H22 109.6(10) . . ? Li1 B2 H22 49.9(9) 2_556 . ? H21 B2 H22 109.7(15) . . ? N2 B2 H23 114.6(10) . . ? Li1 B2 H23 62.6(11) 2_556 . ? H21 B2 H23 105.7(14) . . ? H22 B2 H23 107.7(14) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1 C31 C32 113.2(2) . . ? O1 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? O1 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 O1 113.0(3) . . ? C34 C33 H33A 109.0 . . ? O1 C33 H33A 109.0 . . ? C34 C33 H33B 109.0 . . ? O1 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.673 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.046 data_dw1251 _database_code_depnum_ccdc_archive 'CCDC 907277' #TrackingRef 'dw1251.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H24 Al3 N3' _chemical_formula_sum 'C6 H24 Al3 N3' _chemical_formula_weight 219.22 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.5108(2) _cell_length_b 8.7748(2) _cell_length_c 25.5084(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.212(1) _cell_angle_gamma 90.00 _cell_volume 1455.03(7) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 14500 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 32.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.001 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.755 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; Entry CASNEP in CSD ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 11098 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 32.02 _reflns_number_total 4821 _reflns_number_gt 2774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement '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^)+(0.0386P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4821 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 0.002 _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 Al1 Al 0.38016(5) 0.07811(4) 0.576488(13) 0.03312(9) Uani 1 1 d . . . H11 H 0.6012(16) 0.1073(14) 0.5867(4) 0.0555(15) Uiso 1 1 d . . . H12 H 0.3190(16) -0.0535(13) 0.5407(5) 0.0555(15) Uiso 1 1 d . . . Al2 Al 0.27217(5) 0.43496(4) 0.598655(13) 0.03547(10) Uani 1 1 d . . . H21 H 0.4987(16) 0.4772(13) 0.6054(5) 0.0555(15) Uiso 1 1 d . . . H22 H 0.1208(17) 0.5616(13) 0.5807(5) 0.0555(15) Uiso 1 1 d . . . Al3 Al 0.30773(5) 0.18949(4) 0.695970(12) 0.03515(10) Uani 1 1 d . . . H31 H 0.1877(17) 0.1375(14) 0.7421(4) 0.0555(15) Uiso 1 1 d . . . H32 H 0.5306(16) 0.2264(14) 0.7033(4) 0.0555(15) Uiso 1 1 d . . . N1 N 0.28070(12) 0.02614(10) 0.64471(3) 0.0333(2) Uani 1 1 d . . . N2 N 0.24605(12) 0.26286(10) 0.55110(3) 0.0321(2) Uani 1 1 d . . . N3 N 0.18038(12) 0.37142(11) 0.66619(3) 0.0330(2) Uani 1 1 d . . . C1 C 0.07001(17) -0.04300(14) 0.64084(5) 0.0452(3) Uani 1 1 d . . . H1A H 0.0686 -0.1300 0.6167 0.0560(9) Uiso 1 1 calc R . . H1B H -0.0299 0.0333 0.6276 0.0560(9) Uiso 1 1 calc R . . H1C H 0.0335 -0.0775 0.6756 0.0560(9) Uiso 1 1 calc R . . C2 C 0.42347(18) -0.09682(14) 0.66493(5) 0.0485(3) Uani 1 1 d . . . H2A H 0.4205 -0.1816 0.6399 0.0560(9) Uiso 1 1 calc R . . H2B H 0.3798 -0.1331 0.6989 0.0560(9) Uiso 1 1 calc R . . H2C H 0.5636 -0.0563 0.6692 0.0560(9) Uiso 1 1 calc R . . C3 C 0.35888(18) 0.30819(15) 0.50390(4) 0.0473(3) Uani 1 1 d . . . H3A H 0.2943 0.3990 0.4879 0.0560(9) Uiso 1 1 calc R . . H3B H 0.3535 0.2245 0.4784 0.0560(9) Uiso 1 1 calc R . . H3C H 0.5026 0.3306 0.5146 0.0560(9) Uiso 1 1 calc R . . C4 C 0.02814(16) 0.23456(14) 0.53209(4) 0.0434(3) Uani 1 1 d . . . H4A H -0.0303 0.3281 0.5164 0.0560(9) Uiso 1 1 calc R . . H4B H -0.0521 0.2037 0.5617 0.0560(9) Uiso 1 1 calc R . . H4C H 0.0239 0.1534 0.5057 0.0560(9) Uiso 1 1 calc R . . C5 C -0.04959(15) 0.36414(16) 0.66680(5) 0.0485(3) Uani 1 1 d . . . H5A H -0.0892 0.3409 0.7024 0.0560(9) Uiso 1 1 calc R . . H5B H -0.1015 0.2842 0.6427 0.0560(9) Uiso 1 1 calc R . . H5C H -0.1084 0.4625 0.6556 0.0560(9) Uiso 1 1 calc R . . C6 C 0.24833(18) 0.49699(14) 0.70347(5) 0.0457(3) Uani 1 1 d . . . H6A H 0.2073 0.4722 0.7388 0.0560(9) Uiso 1 1 calc R . . H6B H 0.1837 0.5930 0.6919 0.0560(9) Uiso 1 1 calc R . . H6C H 0.3983 0.5075 0.7039 0.0560(9) 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 Al1 0.03095(16) 0.03355(19) 0.03464(18) -0.00074(14) -0.00028(13) -0.00130(14) Al2 0.04119(18) 0.03059(19) 0.03415(18) 0.00339(14) -0.00226(14) -0.00435(14) Al3 0.03752(18) 0.0384(2) 0.02909(17) 0.00410(15) -0.00175(13) -0.00617(14) N1 0.0307(4) 0.0294(5) 0.0393(5) 0.0053(4) -0.0027(4) -0.0034(4) N2 0.0306(4) 0.0365(5) 0.0288(4) 0.0040(4) -0.0017(3) -0.0049(4) N3 0.0309(4) 0.0340(5) 0.0340(5) -0.0041(4) 0.0001(4) -0.0026(4) C1 0.0431(6) 0.0417(7) 0.0508(7) 0.0023(6) 0.0032(5) -0.0151(5) C2 0.0540(7) 0.0377(7) 0.0525(8) 0.0117(6) -0.0085(6) 0.0013(6) C3 0.0563(7) 0.0503(8) 0.0359(6) 0.0056(6) 0.0086(5) -0.0036(6) C4 0.0392(6) 0.0464(7) 0.0426(6) 0.0027(6) -0.0143(5) -0.0035(5) C5 0.0311(6) 0.0599(8) 0.0549(8) -0.0072(7) 0.0064(5) 0.0008(6) C6 0.0525(7) 0.0415(7) 0.0426(7) -0.0105(6) -0.0016(5) -0.0049(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 Al1 N2 1.9356(9) . ? Al1 N1 1.9446(10) . ? Al1 H11 1.471(11) . ? Al1 H12 1.512(11) . ? Al2 N3 1.9367(10) . ? Al2 N2 1.9385(9) . ? Al2 H21 1.521(11) . ? Al2 H22 1.538(11) . ? Al3 N3 1.9346(10) . ? Al3 N1 1.9415(10) . ? Al3 H31 1.519(12) . ? Al3 H32 1.488(11) . ? N1 C2 1.4969(13) . ? N1 C1 1.4982(13) . ? N2 C4 1.4942(12) . ? N2 C3 1.4989(13) . ? N3 C5 1.4996(13) . ? N3 C6 1.5056(13) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al1 N1 109.22(4) . . ? N2 Al1 H11 109.4(5) . . ? N1 Al1 H11 104.7(4) . . ? N2 Al1 H12 109.8(4) . . ? N1 Al1 H12 105.8(5) . . ? H11 Al1 H12 117.5(7) . . ? N3 Al2 N2 108.16(4) . . ? N3 Al2 H21 108.4(5) . . ? N2 Al2 H21 108.1(5) . . ? N3 Al2 H22 104.4(5) . . ? N2 Al2 H22 110.1(4) . . ? H21 Al2 H22 117.3(6) . . ? N3 Al3 N1 108.91(4) . . ? N3 Al3 H31 108.9(5) . . ? N1 Al3 H31 105.6(5) . . ? N3 Al3 H32 105.3(5) . . ? N1 Al3 H32 107.2(4) . . ? H31 Al3 H32 120.6(6) . . ? C2 N1 C1 106.23(9) . . ? C2 N1 Al3 105.60(6) . . ? C1 N1 Al3 113.04(7) . . ? C2 N1 Al1 104.24(7) . . ? C1 N1 Al1 112.68(6) . . ? Al3 N1 Al1 114.04(5) . . ? C4 N2 C3 106.41(8) . . ? C4 N2 Al1 111.82(7) . . ? C3 N2 Al1 105.00(7) . . ? C4 N2 Al2 112.39(7) . . ? C3 N2 Al2 105.44(7) . . ? Al1 N2 Al2 114.90(4) . . ? C5 N3 C6 106.43(9) . . ? C5 N3 Al3 111.53(7) . . ? C6 N3 Al3 104.57(6) . . ? C5 N3 Al2 112.30(6) . . ? C6 N3 Al2 104.87(7) . . ? Al3 N3 Al2 116.11(5) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 32.02 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.230 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.044 data_dw1264 _database_code_depnum_ccdc_archive 'CCDC 907278' #TrackingRef 'dw1264.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H12 B2 N 1-, Li 1+' _chemical_formula_sum 'C2 H12 B2 Li N' _chemical_formula_weight 78.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 Pnna _symmetry_space_group_name_Hall '-P 2a 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 23.9585(8) _cell_length_b 17.9749(4) _cell_length_c 12.0272(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5179.5(2) _cell_formula_units_Z 32 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 21923 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.35 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.041 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 1.003 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 22701 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 25.36 _reflns_number_total 4713 _reflns_number_gt 2296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement '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^)+(0.1109P)^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 4713 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1246 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1973 _refine_ls_wR_factor_gt 0.1806 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _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 Li1 Li 0.2500 0.0000 0.7863(5) 0.0483(14) Uani 1 2 d S . . Li2 Li 0.15071(17) 0.0913(2) 0.5186(3) 0.0512(11) Uani 1 1 d . . . Li3 Li 0.31141(16) 0.12135(19) 0.3799(3) 0.0437(10) Uani 1 1 d . . . Li4 Li 0.37400(17) 0.3373(2) 0.4416(4) 0.0579(12) Uani 1 1 d . . . Li5 Li 0.5151(2) 0.2500 0.2500 0.0474(14) Uani 1 2 d S . . N2 N 0.24692(7) 0.24039(8) 0.49597(14) 0.0334(5) Uani 1 1 d . . . B21 B 0.22000(11) 0.17350(13) 0.4332(2) 0.0364(6) Uani 1 1 d . . . H21D H 0.1793 0.1766 0.4390 0.055 Uiso 1 1 calc R . . H21E H 0.2329 0.1268 0.4663 0.055 Uiso 1 1 calc R . . H21F H 0.2309 0.1751 0.3547 0.055 Uiso 1 1 calc R . . B22 B 0.31235(11) 0.23483(13) 0.4873(2) 0.0386(7) Uani 1 1 d . . . H22D H 0.3294 0.2766 0.5272 0.058 Uiso 1 1 calc R . . H22E H 0.3235 0.2366 0.4089 0.058 Uiso 1 1 calc R . . H22F H 0.3249 0.1879 0.5203 0.058 Uiso 1 1 calc R . . C21 C 0.23091(11) 0.23980(12) 0.61486(19) 0.0500(7) Uani 1 1 d . . . H21A H 0.1902 0.2427 0.6213 0.075 Uiso 1 1 calc R . . H21B H 0.2478 0.2826 0.6525 0.075 Uiso 1 1 calc R . . H21C H 0.2441 0.1937 0.6495 0.075 Uiso 1 1 calc R . . C22 C 0.22775(10) 0.31160(11) 0.4465(2) 0.0473(7) Uani 1 1 d . . . H22A H 0.1870 0.3149 0.4519 0.071 Uiso 1 1 calc R . . H22B H 0.2389 0.3137 0.3682 0.071 Uiso 1 1 calc R . . H22C H 0.2447 0.3533 0.4868 0.071 Uiso 1 1 calc R . . N1 N 0.12683(7) -0.00187(9) 0.77797(15) 0.0351(5) Uani 1 1 d . . . B11 B 0.16496(13) -0.05936(15) 0.8417(3) 0.0500(8) Uani 1 1 d . . . H11D H 0.1414 -0.0949 0.8819 0.075 Uiso 1 1 calc R . . H11E H 0.1888 -0.0327 0.8946 0.075 Uiso 1 1 calc R . . H11F H 0.1883 -0.0861 0.7881 0.075 Uiso 1 1 calc R . . B12 B 0.16410(12) 0.05520(14) 0.7125(2) 0.0407(7) Uani 1 1 d . . . H12D H 0.1401 0.0904 0.6727 0.061 Uiso 1 1 calc R . . H12E H 0.1875 0.0284 0.6590 0.061 Uiso 1 1 calc R . . H12F H 0.1879 0.0824 0.7648 0.061 Uiso 1 1 calc R . . C11 C 0.08951(10) -0.04163(14) 0.6997(2) 0.0548(7) Uani 1 1 d . . . H11A H 0.0673 -0.0054 0.6579 0.082 Uiso 1 1 calc R . . H11B H 0.0646 -0.0746 0.7415 0.082 Uiso 1 1 calc R . . H11C H 0.1120 -0.0712 0.6479 0.082 Uiso 1 1 calc R . . C12 C 0.09189(11) 0.03821(14) 0.8589(2) 0.0596(8) Uani 1 1 d . . . H12A H 0.0686 0.0746 0.8198 0.089 Uiso 1 1 calc R . . H12B H 0.1159 0.0641 0.9124 0.089 Uiso 1 1 calc R . . H12C H 0.0680 0.0027 0.8983 0.089 Uiso 1 1 calc R . . N3 N 0.37760(7) 0.00907(9) 0.25649(15) 0.0334(5) Uani 1 1 d . . . B31 B 0.37207(11) 0.01257(13) 0.3871(2) 0.0381(7) Uani 1 1 d . . . H31D H 0.3928 -0.0288 0.4203 0.057 Uiso 1 1 calc R . . H31E H 0.3326 0.0089 0.4079 0.057 Uiso 1 1 calc R . . H31F H 0.3874 0.0598 0.4141 0.057 Uiso 1 1 calc R . . B32 B 0.34440(11) 0.07543(13) 0.2032(2) 0.0384(7) Uani 1 1 d . . . H32D H 0.3478 0.0732 0.1220 0.058 Uiso 1 1 calc R . . H32E H 0.3597 0.1227 0.2301 0.058 Uiso 1 1 calc R . . H32F H 0.3050 0.0718 0.2241 0.058 Uiso 1 1 calc R . . C31 C 0.35480(10) -0.06205(11) 0.2141(2) 0.0476(7) Uani 1 1 d . . . H31A H 0.3605 -0.0648 0.1335 0.071 Uiso 1 1 calc R . . H31B H 0.3148 -0.0647 0.2306 0.071 Uiso 1 1 calc R . . H31C H 0.3740 -0.1037 0.2501 0.071 Uiso 1 1 calc R . . C32 C 0.43713(9) 0.01326(12) 0.2261(2) 0.0489(7) Uani 1 1 d . . . H32A H 0.4409 0.0107 0.1450 0.073 Uiso 1 1 calc R . . H32B H 0.4573 -0.0284 0.2600 0.073 Uiso 1 1 calc R . . H32C H 0.4528 0.0603 0.2529 0.073 Uiso 1 1 calc R . . N4 N 0.50827(7) 0.24868(9) 0.50121(14) 0.0364(5) Uani 1 1 d . . . B41 B 0.47255(11) 0.30263(14) 0.4272(2) 0.0404(7) Uani 1 1 d . . . H41D H 0.4501 0.3351 0.4751 0.061 Uiso 1 1 calc R . . H41E H 0.4478 0.2735 0.3792 0.061 Uiso 1 1 calc R . . H41F H 0.4974 0.3330 0.3812 0.061 Uiso 1 1 calc R . . B42 B 0.54442(12) 0.19653(14) 0.4234(2) 0.0456(7) Uani 1 1 d . . . H42D H 0.5667 0.1627 0.4693 0.068 Uiso 1 1 calc R . . H42E H 0.5693 0.2271 0.3776 0.068 Uiso 1 1 calc R . . H42F H 0.5196 0.1675 0.3753 0.068 Uiso 1 1 calc R . . C41 C 0.47152(10) 0.20334(13) 0.5729(2) 0.0534(7) Uani 1 1 d . . . H41A H 0.4496 0.2361 0.6212 0.080 Uiso 1 1 calc R . . H41B H 0.4943 0.1699 0.6186 0.080 Uiso 1 1 calc R . . H41C H 0.4462 0.1739 0.5263 0.080 Uiso 1 1 calc R . . C42 C 0.54610(10) 0.29303(13) 0.5732(2) 0.0531(7) Uani 1 1 d . . . H42A H 0.5239 0.3258 0.6211 0.080 Uiso 1 1 calc R . . H42B H 0.5709 0.3232 0.5266 0.080 Uiso 1 1 calc R . . H42C H 0.5685 0.2594 0.6194 0.080 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 Li1 0.043(3) 0.050(3) 0.051(4) 0.000 0.000 0.003(3) Li2 0.065(3) 0.050(2) 0.039(2) 0.0062(19) -0.005(2) -0.015(2) Li3 0.049(2) 0.041(2) 0.042(2) -0.0044(17) 0.000(2) 0.0061(17) Li4 0.041(2) 0.052(2) 0.081(3) 0.024(2) -0.008(2) -0.0063(19) Li5 0.051(4) 0.042(3) 0.049(4) 0.008(3) 0.000 0.000 N2 0.0433(12) 0.0270(9) 0.0298(10) 0.0002(7) 0.0037(9) -0.0017(8) B21 0.0385(16) 0.0382(14) 0.0324(15) -0.0006(12) 0.0026(13) -0.0029(12) B22 0.0453(17) 0.0318(14) 0.0387(16) -0.0006(11) -0.0024(13) -0.0033(11) C21 0.0697(17) 0.0469(14) 0.0335(14) -0.0052(11) 0.0130(13) -0.0080(12) C22 0.0529(16) 0.0331(13) 0.0560(17) 0.0061(11) 0.0024(13) 0.0049(11) N1 0.0353(11) 0.0369(10) 0.0331(11) 0.0005(8) 0.0026(9) 0.0034(8) B11 0.0527(19) 0.0487(16) 0.0487(19) 0.0172(14) 0.0066(16) 0.0025(13) B12 0.0455(17) 0.0385(14) 0.0382(17) 0.0051(12) -0.0041(14) 0.0031(12) C11 0.0485(16) 0.0632(16) 0.0527(17) 0.0003(13) -0.0021(14) -0.0151(13) C12 0.0573(18) 0.0659(17) 0.0556(18) -0.0042(14) 0.0178(15) 0.0149(13) N3 0.0332(11) 0.0296(10) 0.0373(11) -0.0008(8) 0.0048(9) -0.0026(7) B31 0.0438(17) 0.0319(14) 0.0385(16) 0.0028(11) -0.0009(14) -0.0003(11) B32 0.0425(17) 0.0373(15) 0.0356(16) 0.0011(12) 0.0036(13) -0.0019(12) C31 0.0630(17) 0.0341(13) 0.0458(16) -0.0074(11) 0.0089(13) -0.0077(11) C32 0.0406(15) 0.0499(15) 0.0563(18) 0.0071(12) 0.0096(13) 0.0028(11) N4 0.0353(11) 0.0370(10) 0.0369(11) 0.0042(9) -0.0022(9) -0.0011(8) B41 0.0385(17) 0.0392(15) 0.0436(17) 0.0014(12) 0.0019(14) 0.0001(12) B42 0.0466(18) 0.0446(16) 0.0456(18) 0.0052(13) -0.0018(15) 0.0096(13) C41 0.0527(17) 0.0609(16) 0.0465(17) 0.0160(12) 0.0061(14) -0.0028(12) C42 0.0499(16) 0.0599(16) 0.0497(17) -0.0068(12) -0.0139(13) -0.0010(12) _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 Li1 B11 2.394(3) 2 ? Li1 B12 2.452(3) 2 ? Li2 B12 2.442(5) . ? Li2 B31 2.508(5) 2 ? Li4 B32 2.448(5) 4 ? Li5 B42 2.401(3) 4 ? Li5 B41 2.545(4) 4 ? N2 C21 1.480(3) . ? N2 C22 1.485(3) . ? N2 B21 1.560(3) . ? N2 B22 1.574(3) . ? B21 H21D 0.9800 . ? B21 H21E 0.9800 . ? B21 H21F 0.9800 . ? B22 H22D 0.9800 . ? B22 H22E 0.9800 . ? B22 H22F 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N1 C12 1.472(3) . ? N1 C11 1.482(3) . ? N1 B12 1.572(3) . ? N1 B11 1.578(3) . ? B11 H11D 0.9800 . ? B11 H11E 0.9800 . ? B11 H11F 0.9800 . ? B12 H12D 0.9800 . ? B12 H12E 0.9800 . ? B12 H12F 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N3 C32 1.474(3) . ? N3 C31 1.481(3) . ? N3 B32 1.571(3) . ? N3 B31 1.577(3) . ? B31 Li2 2.508(5) 2 ? B31 H31D 0.9800 . ? B31 H31E 0.9800 . ? B31 H31F 0.9800 . ? B32 Li4 2.448(5) 4 ? B32 H32D 0.9800 . ? B32 H32E 0.9800 . ? B32 H32F 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N4 C41 1.477(3) . ? N4 C42 1.485(3) . ? N4 B41 1.570(3) . ? N4 B42 1.582(3) . ? B41 H41D 0.9800 . ? B41 H41E 0.9800 . ? B41 H41F 0.9800 . ? B42 H42D 0.9800 . ? B42 H42E 0.9800 . ? B42 H42F 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B11 Li1 B12 64.32(9) 2 2 ? B12 Li2 B31 115.63(17) . 2 ? B42 Li5 B41 62.51(8) 4 4 ? C21 N2 C22 108.25(17) . . ? C21 N2 B21 110.81(17) . . ? C22 N2 B21 110.03(17) . . ? C21 N2 B22 108.76(18) . . ? C22 N2 B22 109.65(17) . . ? B21 N2 B22 109.32(16) . . ? N2 B21 H21D 109.5 . . ? N2 B21 H21E 109.5 . . ? H21D B21 H21E 109.5 . . ? N2 B21 H21F 109.5 . . ? H21D B21 H21F 109.5 . . ? H21E B21 H21F 109.5 . . ? N2 B22 H22D 109.5 . . ? N2 B22 H22E 109.5 . . ? H22D B22 H22E 109.5 . . ? N2 B22 H22F 109.5 . . ? H22D B22 H22F 109.5 . . ? H22E B22 H22F 109.5 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C12 N1 C11 108.25(18) . . ? C12 N1 B12 109.57(18) . . ? C11 N1 B12 109.81(18) . . ? C12 N1 B11 109.2(2) . . ? C11 N1 B11 110.00(18) . . ? B12 N1 B11 109.99(18) . . ? N1 B11 H11D 109.5 . . ? N1 B11 H11E 109.5 . . ? H11D B11 H11E 109.5 . . ? N1 B11 H11F 109.5 . . ? H11D B11 H11F 109.5 . . ? H11E B11 H11F 109.5 . . ? N1 B12 Li2 125.30(19) . . ? N1 B12 H12D 109.5 . . ? Li2 B12 H12D 44.3 . . ? N1 B12 H12E 109.5 . . ? Li2 B12 H12E 65.2 . . ? H12D B12 H12E 109.5 . . ? N1 B12 H12F 109.5 . . ? Li2 B12 H12F 123.9 . . ? H12D B12 H12F 109.5 . . ? H12E B12 H12F 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C32 N3 C31 108.39(17) . . ? C32 N3 B32 110.48(17) . . ? C31 N3 B32 109.15(18) . . ? C32 N3 B31 109.05(18) . . ? C31 N3 B31 110.26(17) . . ? B32 N3 B31 109.50(17) . . ? N3 B31 Li2 128.06(17) . 2 ? N3 B31 H31D 109.5 . . ? Li2 B31 H31D 44.5 2 . ? N3 B31 H31E 109.5 . . ? Li2 B31 H31E 65.1 2 . ? H31D B31 H31E 109.5 . . ? N3 B31 H31F 109.5 . . ? Li2 B31 H31F 121.2 2 . ? H31D B31 H31F 109.5 . . ? H31E B31 H31F 109.5 . . ? N3 B32 Li4 129.06(19) . 4 ? N3 B32 H32D 109.5 . . ? Li4 B32 H32D 45.1 4 . ? N3 B32 H32E 109.5 . . ? Li4 B32 H32E 64.6 4 . ? H32D B32 H32E 109.5 . . ? N3 B32 H32F 109.5 . . ? Li4 B32 H32F 120.3 4 . ? H32D B32 H32F 109.5 . . ? H32E B32 H32F 109.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C41 N4 C42 108.64(18) . . ? C41 N4 B41 110.28(18) . . ? C42 N4 B41 109.36(17) . . ? C41 N4 B42 110.14(18) . . ? C42 N4 B42 109.18(19) . . ? B41 N4 B42 109.22(18) . . ? N4 B41 H41D 109.5 . . ? N4 B41 H41E 109.5 . . ? H41D B41 H41E 109.5 . . ? N4 B41 H41F 109.5 . . ? H41D B41 H41F 109.5 . . ? H41E B41 H41F 109.5 . . ? N4 B42 H42D 109.5 . . ? N4 B42 H42E 109.5 . . ? H42D B42 H42E 109.5 . . ? N4 B42 H42F 109.5 . . ? H42D B42 H42F 109.5 . . ? H42E B42 H42F 109.5 . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N4 C42 H42A 109.5 . . ? N4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.218 _refine_diff_density_min -0.155 _refine_diff_density_rms 0.040 # Attachment 'dw1264.bcc' #ADATE 20121011 #ATOM Li1 0.2500 .0 0.7863,5 #AUTHOR R.Less,D.S.Wright,J.E.Davies #BOND Li1 B11 2.394,3