data_ap4145 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H28 B2 N4, 2(Al2 Br7)' _chemical_formula_sum 'C14 H28 Al4 B2 Br14 N4' _chemical_formula_weight 1500.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.6763 1.2805 '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 9.4348(2) _cell_length_b 9.4885(2) _cell_length_c 11.5808(8) _cell_angle_alpha 98.386(7) _cell_angle_beta 92.646(7) _cell_angle_gamma 93.785(7) _cell_volume 1021.78(8) _cell_formula_units_Z 1 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 17391 _cell_measurement_theta_min 3.90 _cell_measurement_theta_max 68.20 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 17.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1964 _exptl_absorpt_correction_T_max 0.2775 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'micro-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn 944+ CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.629 _diffrn_reflns_number 26707 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.70 _diffrn_reflns_theta_max 68.23 _reflns_number_total 3680 _reflns_number_gt 3490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r12' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r12' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _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^)+(0.0404P)^2^+4.6037P] 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 3680 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 0.06971(5) 0.60780(6) 0.21111(5) 0.02293(15) Uani 1 1 d . . . Br2 Br 0.25264(6) 0.30618(6) 0.04934(5) 0.03025(17) Uani 1 1 d . . . Br3 Br 0.33046(5) 0.40370(6) 0.37610(5) 0.02131(15) Uani 1 1 d . . . Br4 Br 0.46478(5) 0.62739(5) 0.15348(4) 0.01665(14) Uani 1 1 d . . . Br5 Br 0.47360(6) 1.02226(6) 0.18729(5) 0.02664(16) Uani 1 1 d . . . Br6 Br 0.76101(5) 0.83782(6) 0.32804(5) 0.02324(16) Uani 1 1 d . . . Br7 Br 0.38617(5) 0.82583(6) 0.44478(5) 0.02289(15) Uani 1 1 d . . . Al1 Al 0.26560(14) 0.48160(15) 0.20708(12) 0.0144(3) Uani 1 1 d . . . Al2 Al 0.52366(14) 0.84567(15) 0.29280(12) 0.0140(3) Uani 1 1 d . . . N1 N 0.1533(4) -0.2114(5) -0.1629(4) 0.0224(10) Uani 1 1 d . . . N2 N 0.0022(4) -0.1339(5) -0.2789(4) 0.0207(10) Uani 1 1 d . . . C1 C 0.0523(5) -0.1161(6) -0.1681(5) 0.0258(13) Uani 1 1 d . . . C2 C 0.1650(5) -0.2883(5) -0.2722(4) 0.0167(10) Uani 1 1 d . . . C3 C 0.0690(5) -0.2386(6) -0.3448(4) 0.0173(11) Uani 1 1 d . . . C4 C 0.2367(7) -0.2307(9) -0.0583(5) 0.0417(18) Uani 1 1 d . . . H4A H 0.2689 -0.1371 -0.0141 0.063 Uiso 1 1 calc R . . H4B H 0.3195 -0.2835 -0.0807 0.063 Uiso 1 1 calc R . . H4C H 0.1780 -0.2845 -0.0096 0.063 Uiso 1 1 calc R . . C6 C 0.0365(6) -0.2853(7) -0.4731(5) 0.0264(13) Uani 1 1 d . . . H6A H 0.0986 -0.3600 -0.5017 0.040 Uiso 1 1 calc R . . H6B H 0.0527 -0.2035 -0.5149 0.040 Uiso 1 1 calc R . . H6C H -0.0631 -0.3229 -0.4866 0.040 Uiso 1 1 calc R . . C7 C -0.1095(6) -0.0534(6) -0.3295(6) 0.0292(13) Uani 1 1 d . . . H7A H -0.1989 -0.0694 -0.2918 0.044 Uiso 1 1 calc R . . H7B H -0.1237 -0.0867 -0.4137 0.044 Uiso 1 1 calc R . . H7C H -0.0795 0.0487 -0.3163 0.044 Uiso 1 1 calc R . . C11 C 0.2662(6) -0.3988(7) -0.2960(6) 0.0306(13) Uani 1 1 d . . . H11A H 0.2553 -0.4408 -0.3787 0.046 Uiso 1 1 calc R . . H11B H 0.2473 -0.4735 -0.2473 0.046 Uiso 1 1 calc R . . H11C H 0.3635 -0.3559 -0.2779 0.046 Uiso 1 1 calc R . . B1 B -0.0009(7) 0.0057(8) -0.0760(6) 0.0308(16) Uani 1 1 d . . . H1A H -0.081(6) -0.052(6) -0.010(5) 0.026(16) Uiso 1 1 d . . . H1B H -0.054(8) 0.107(8) -0.106(6) 0.04(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0110(2) 0.0347(3) 0.0244(3) 0.0067(2) 0.0055(2) 0.0032(2) Br2 0.0348(3) 0.0267(3) 0.0232(3) -0.0106(2) 0.0118(2) -0.0173(2) Br3 0.0191(3) 0.0269(3) 0.0191(3) 0.0067(2) 0.0050(2) 0.0000(2) Br4 0.0116(2) 0.0221(3) 0.0140(3) -0.0024(2) 0.00504(18) -0.00732(19) Br5 0.0259(3) 0.0235(3) 0.0314(3) 0.0091(2) -0.0005(2) -0.0011(2) Br6 0.0076(2) 0.0317(3) 0.0273(3) -0.0037(2) -0.00194(19) -0.0026(2) Br7 0.0196(3) 0.0262(3) 0.0198(3) -0.0052(2) 0.0093(2) -0.0080(2) Al1 0.0099(6) 0.0183(7) 0.0137(7) -0.0010(6) 0.0044(5) -0.0044(5) Al2 0.0075(6) 0.0180(7) 0.0159(7) 0.0016(6) 0.0014(5) -0.0025(5) N1 0.015(2) 0.038(3) 0.013(2) 0.0044(19) 0.0017(16) -0.0100(19) N2 0.0136(19) 0.015(2) 0.032(3) -0.0007(19) 0.0094(18) -0.0023(16) C1 0.017(2) 0.031(3) 0.024(3) -0.009(2) 0.008(2) -0.012(2) C2 0.011(2) 0.021(3) 0.017(2) 0.003(2) 0.0048(18) -0.0079(19) C3 0.008(2) 0.026(3) 0.017(2) -0.002(2) 0.0070(18) -0.0058(19) C4 0.028(3) 0.082(5) 0.015(3) 0.013(3) -0.002(2) -0.004(3) C6 0.017(2) 0.046(4) 0.016(3) 0.006(2) 0.002(2) 0.001(2) C7 0.018(3) 0.027(3) 0.041(3) -0.001(3) 0.004(2) 0.001(2) C11 0.019(3) 0.034(3) 0.039(3) 0.003(3) -0.001(2) 0.007(2) B1 0.024(3) 0.042(4) 0.026(3) 0.001(3) 0.008(3) -0.002(3) _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 2.2662(16) . ? Br2 Al1 2.2778(14) . ? Br3 Al1 2.2635(16) . ? Br4 Al1 2.4178(14) . ? Br4 Al2 2.4479(14) . ? Br5 Al2 2.2742(17) . ? Br6 Al2 2.2656(14) . ? Br7 Al2 2.2564(14) . ? N1 C1 1.361(8) . ? N1 C2 1.379(6) . ? N1 C4 1.455(8) . ? N2 C1 1.330(8) . ? N2 C3 1.368(6) . ? N2 C7 1.489(8) . ? C1 B1 1.579(8) . ? C2 C3 1.360(8) . ? C2 C11 1.470(8) . ? C3 C6 1.499(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? B1 B1 1.778(14) 2 ? B1 H1A 1.25(6) . ? B1 H1B 1.20(7) . ? 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 Al1 Br4 Al2 113.27(5) . . ? Br3 Al1 Br1 115.82(6) . . ? Br3 Al1 Br2 113.04(7) . . ? Br1 Al1 Br2 111.26(6) . . ? Br3 Al1 Br4 107.72(6) . . ? Br1 Al1 Br4 108.99(6) . . ? Br2 Al1 Br4 98.44(5) . . ? Br7 Al2 Br6 116.47(7) . . ? Br7 Al2 Br5 115.56(6) . . ? Br6 Al2 Br5 111.75(6) . . ? Br7 Al2 Br4 105.52(5) . . ? Br6 Al2 Br4 102.09(6) . . ? Br5 Al2 Br4 103.30(6) . . ? C1 N1 C2 109.8(4) . . ? C1 N1 C4 125.6(5) . . ? C2 N1 C4 124.6(5) . . ? C1 N2 C3 110.6(5) . . ? C1 N2 C7 126.8(5) . . ? C3 N2 C7 122.6(5) . . ? N2 C1 N1 106.1(4) . . ? N2 C1 B1 120.3(6) . . ? N1 C1 B1 133.4(5) . . ? C3 C2 N1 106.2(4) . . ? C3 C2 C11 130.7(5) . . ? N1 C2 C11 123.1(5) . . ? C2 C3 N2 107.3(4) . . ? C2 C3 C6 128.7(5) . . ? N2 C3 C6 124.0(5) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 B1 B1 122.3(8) . 2 ? C1 B1 H1A 108(3) . . ? B1 B1 H1A 44(3) 2 . ? C1 B1 H1B 121(3) . . ? B1 B1 H1B 116(3) 2 . ? H1A B1 H1B 110(4) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 68.23 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.132 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.180