# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'D W Stephan' _publ_contact_author_email DSTEPHAN@CHEM.UTORONTO.CA _publ_section_title ; Hemilabile Biphenyl-Amide Ligand Complexes of Li and Al ; loop_ _publ_author_name 'D W Stephan' 'Meghan A Dureen' # Attachment 'cif.txt' data_(2-C6H4-Ph)tBuNH _database_code_depnum_ccdc_archive 'CCDC 674908' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C16 H19 N' _chemical_formula_weight 225.32 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/C 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 13.969(2) _cell_length_b 6.1361(10) _cell_length_c 17.014(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.286(2) _cell_angle_gamma 90.00 _cell_volume 1358.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type NONE _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 12397 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2394 _reflns_number_gt 1310 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0492P)^2^+0.1312P] 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_number_reflns 2394 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _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 N1 N 0.25060(12) 0.2380(3) 0.32188(8) 0.0745(5) Uani 1 1 d . . . H1A H 0.2862 0.1243 0.3209 0.089 Uiso 1 1 calc R . . C1 C 0.16713(14) 0.2758(3) 0.24876(10) 0.0530(5) Uani 1 1 d . . . C2 C 0.15850(12) 0.1583(3) 0.17533(10) 0.0485(4) Uani 1 1 d . . . C3 C 0.07224(14) 0.1893(3) 0.10318(11) 0.0624(5) Uani 1 1 d . . . H3A H 0.0664 0.1110 0.0549 0.075 Uiso 1 1 calc R . . C4 C -0.00522(15) 0.3317(4) 0.10026(13) 0.0743(6) Uani 1 1 d . . . H4A H -0.0622 0.3497 0.0509 0.089 Uiso 1 1 calc R . . C5 C 0.00366(14) 0.4461(4) 0.17171(13) 0.0710(6) Uani 1 1 d . . . H5A H -0.0480 0.5426 0.1710 0.085 Uiso 1 1 calc R . . C6 C 0.08812(15) 0.4201(3) 0.24450(11) 0.0647(5) Uani 1 1 d . . . H6A H 0.0927 0.5005 0.2921 0.078 Uiso 1 1 calc R . . C7 C 0.23810(13) 0.0026(3) 0.17114(9) 0.0472(4) Uani 1 1 d . . . C8 C 0.20989(15) -0.2062(3) 0.13929(11) 0.0603(5) Uani 1 1 d . . . H8A H 0.1422 -0.2512 0.1254 0.072 Uiso 1 1 calc R . . C9 C 0.28050(19) -0.3476(3) 0.12792(12) 0.0713(6) Uani 1 1 d . . . H9A H 0.2599 -0.4864 0.1064 0.086 Uiso 1 1 calc R . . C10 C 0.38035(19) -0.2854(4) 0.14794(12) 0.0735(6) Uani 1 1 d . . . H10A H 0.4276 -0.3808 0.1397 0.088 Uiso 1 1 calc R . . C11 C 0.41066(14) -0.0811(4) 0.18036(12) 0.0670(6) Uani 1 1 d . . . H11A H 0.4788 -0.0383 0.1946 0.080 Uiso 1 1 calc R . . C12 C 0.34019(13) 0.0608(3) 0.19177(10) 0.0543(5) Uani 1 1 d . . . H12A H 0.3617 0.1987 0.2138 0.065 Uiso 1 1 calc R . . C13 C 0.28750(14) 0.3614(3) 0.40039(11) 0.0594(5) Uani 1 1 d . . . C14 C 0.21529(16) 0.3399(4) 0.44872(12) 0.0855(7) Uani 1 1 d . . . H14A H 0.2057 0.1885 0.4580 0.128 Uiso 1 1 calc R . . H14B H 0.1502 0.4045 0.4166 0.128 Uiso 1 1 calc R . . H14C H 0.2444 0.4131 0.5020 0.128 Uiso 1 1 calc R . . C15 C 0.39019(15) 0.2589(3) 0.45350(12) 0.0831(7) Uani 1 1 d . . . H15A H 0.3799 0.1082 0.4635 0.125 Uiso 1 1 calc R . . H15B H 0.4183 0.3341 0.5064 0.125 Uiso 1 1 calc R . . H15C H 0.4370 0.2698 0.4240 0.125 Uiso 1 1 calc R . . C16 C 0.30450(18) 0.6006(3) 0.38488(15) 0.1008(8) Uani 1 1 d . . . H16A H 0.2401 0.6659 0.3514 0.151 Uiso 1 1 calc R . . H16B H 0.3515 0.6111 0.3555 0.151 Uiso 1 1 calc R . . H16C H 0.3326 0.6753 0.4379 0.151 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 N1 0.0925(13) 0.0819(12) 0.0365(9) -0.0108(8) 0.0084(8) 0.0288(9) C1 0.0629(12) 0.0573(11) 0.0399(10) 0.0016(9) 0.0201(9) 0.0010(10) C2 0.0511(10) 0.0581(11) 0.0386(10) -0.0026(8) 0.0190(8) -0.0064(9) C3 0.0536(11) 0.0854(14) 0.0463(11) -0.0099(10) 0.0159(9) -0.0069(11) C4 0.0541(12) 0.1060(17) 0.0560(13) 0.0008(12) 0.0118(10) 0.0059(12) C5 0.0626(12) 0.0896(15) 0.0641(13) 0.0079(12) 0.0271(11) 0.0146(11) C6 0.0790(14) 0.0707(13) 0.0502(12) -0.0004(10) 0.0302(11) 0.0110(11) C7 0.0572(11) 0.0526(11) 0.0318(9) -0.0011(8) 0.0162(8) -0.0054(9) C8 0.0743(13) 0.0597(13) 0.0492(11) -0.0034(9) 0.0251(10) -0.0120(11) C9 0.1068(18) 0.0504(12) 0.0574(13) -0.0037(10) 0.0305(12) -0.0008(13) C10 0.0892(16) 0.0705(16) 0.0620(13) 0.0027(11) 0.0288(12) 0.0230(13) C11 0.0580(12) 0.0771(14) 0.0629(13) -0.0009(11) 0.0184(10) 0.0070(12) C12 0.0570(11) 0.0563(11) 0.0467(10) -0.0047(9) 0.0152(9) -0.0019(10) C13 0.0688(12) 0.0663(13) 0.0420(10) -0.0097(9) 0.0186(9) -0.0083(10) C14 0.0854(15) 0.1268(19) 0.0489(11) -0.0059(12) 0.0298(11) -0.0098(14) C15 0.0770(15) 0.1074(18) 0.0536(12) -0.0109(12) 0.0102(11) -0.0025(13) C16 0.1129(19) 0.0783(16) 0.1060(18) -0.0006(14) 0.0336(15) -0.0196(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 N1 C1 1.381(2) . ? N1 C13 1.457(2) . ? C1 C6 1.396(2) . ? C1 C2 1.409(2) . ? C2 C3 1.386(2) . ? C2 C7 1.487(2) . ? C3 C4 1.378(3) . ? C4 C5 1.370(3) . ? C5 C6 1.375(2) . ? C7 C12 1.386(2) . ? C7 C8 1.391(2) . ? C8 C9 1.379(3) . ? C9 C10 1.364(3) . ? C10 C11 1.373(3) . ? C11 C12 1.380(2) . ? C13 C14 1.521(3) . ? C13 C16 1.525(3) . ? C13 C15 1.526(2) . ? 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 C1 N1 C13 129.81(16) . . ? N1 C1 C6 123.11(16) . . ? N1 C1 C2 119.01(16) . . ? C6 C1 C2 117.83(16) . . ? C3 C2 C1 118.81(16) . . ? C3 C2 C7 118.07(15) . . ? C1 C2 C7 123.12(15) . . ? C4 C3 C2 122.55(18) . . ? C5 C4 C3 118.44(19) . . ? C4 C5 C6 120.75(19) . . ? C5 C6 C1 121.62(18) . . ? C12 C7 C8 117.13(17) . . ? C12 C7 C2 122.73(15) . . ? C8 C7 C2 119.95(16) . . ? C9 C8 C7 121.21(19) . . ? C10 C9 C8 120.49(19) . . ? C9 C10 C11 119.6(2) . . ? C10 C11 C12 120.07(19) . . ? C11 C12 C7 121.51(17) . . ? N1 C13 C14 111.53(16) . . ? N1 C13 C16 111.54(16) . . ? C14 C13 C16 110.65(18) . . ? N1 C13 C15 105.79(15) . . ? C14 C13 C15 108.02(16) . . ? C16 C13 C15 109.11(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.115 _refine_diff_density_min -0.131 _refine_diff_density_rms 0.024 #===end data_(2-C6H4-Ph)2NH _database_code_depnum_ccdc_archive 'CCDC 674909' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C24 H19 N' _chemical_formula_weight 321.40 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' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P2(1)/n 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 12.522(9) _cell_length_b 9.269(6) _cell_length_c 15.116(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.663(12) _cell_angle_gamma 90.00 _cell_volume 1751(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.817103 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 14224 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 23.38 _reflns_number_total 2557 _reflns_number_gt 1532 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0571P)^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_number_reflns 2557 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 N1 N 0.78868(15) 0.1626(2) 0.22825(12) 0.0667(6) Uani 1 1 d . . . H1A H 0.8379 0.1927 0.2661 0.080 Uiso 1 1 calc R . . C1 C 0.69893(17) 0.1043(2) 0.26310(15) 0.0499(6) Uani 1 1 d . . . C2 C 0.68491(17) 0.1190(2) 0.35440(15) 0.0492(6) Uani 1 1 d . . . C3 C 0.59131(19) 0.0677(2) 0.38662(17) 0.0614(7) Uani 1 1 d . . . H3A H 0.5805 0.0792 0.4465 0.074 Uiso 1 1 calc R . . C4 C 0.51426(19) 0.0008(3) 0.33352(19) 0.0692(7) Uani 1 1 d . . . H4A H 0.4513 -0.0307 0.3566 0.083 Uiso 1 1 calc R . . C5 C 0.53093(19) -0.0195(3) 0.24586(18) 0.0650(7) Uani 1 1 d . . . H5A H 0.4798 -0.0678 0.2097 0.078 Uiso 1 1 calc R . . C6 C 0.62200(17) 0.0307(2) 0.21080(15) 0.0566(6) Uani 1 1 d . . . H6A H 0.6324 0.0151 0.1512 0.068 Uiso 1 1 calc R . . C7 C 0.76744(17) 0.1887(3) 0.41423(14) 0.0516(6) Uani 1 1 d . . . C8 C 0.87118(19) 0.1376(3) 0.42227(16) 0.0690(7) Uani 1 1 d . . . H8A H 0.8892 0.0562 0.3905 0.083 Uiso 1 1 calc R . . C9 C 0.9479(2) 0.2045(3) 0.47601(19) 0.0835(8) Uani 1 1 d . . . H9A H 1.0174 0.1685 0.4804 0.100 Uiso 1 1 calc R . . C10 C 0.9230(3) 0.3241(3) 0.52338(18) 0.0833(9) Uani 1 1 d . . . H10A H 0.9757 0.3708 0.5588 0.100 Uiso 1 1 calc R . . C11 C 0.8207(3) 0.3746(3) 0.51853(17) 0.0779(8) Uani 1 1 d . . . H11A H 0.8029 0.4540 0.5523 0.093 Uiso 1 1 calc R . . C12 C 0.7435(2) 0.3083(3) 0.46363(16) 0.0618(7) Uani 1 1 d . . . H12A H 0.6741 0.3448 0.4598 0.074 Uiso 1 1 calc R . . C13 C 0.80945(18) 0.1787(2) 0.13870(15) 0.0542(6) Uani 1 1 d . . . C14 C 0.90939(18) 0.1396(2) 0.11034(15) 0.0528(6) Uani 1 1 d . . . C15 C 0.92926(19) 0.1676(2) 0.02314(16) 0.0626(7) Uani 1 1 d . . . H15A H 0.9958 0.1435 0.0033 0.075 Uiso 1 1 calc R . . C16 C 0.8544(2) 0.2296(3) -0.03531(17) 0.0727(7) Uani 1 1 d . . . H16A H 0.8698 0.2459 -0.0938 0.087 Uiso 1 1 calc R . . C17 C 0.7570(2) 0.2669(3) -0.00639(18) 0.0723(8) Uani 1 1 d . . . H17A H 0.7056 0.3089 -0.0454 0.087 Uiso 1 1 calc R . . C18 C 0.73484(19) 0.2424(3) 0.08030(16) 0.0646(7) Uani 1 1 d . . . H18A H 0.6687 0.2692 0.0997 0.077 Uiso 1 1 calc R . . C19 C 0.99186(18) 0.0710(2) 0.17115(15) 0.0546(6) Uani 1 1 d . . . C20 C 1.0942(2) 0.1266(3) 0.18146(18) 0.0721(8) Uani 1 1 d . . . H20A H 1.1112 0.2087 0.1500 0.086 Uiso 1 1 calc R . . C21 C 1.1713(2) 0.0634(3) 0.2370(2) 0.0903(9) Uani 1 1 d . . . H21A H 1.2396 0.1030 0.2431 0.108 Uiso 1 1 calc R . . C22 C 1.1478(3) -0.0580(4) 0.2837(2) 0.0899(9) Uani 1 1 d . . . H22A H 1.1995 -0.1001 0.3224 0.108 Uiso 1 1 calc R . . C23 C 1.0477(3) -0.1164(3) 0.27272(19) 0.0819(8) Uani 1 1 d . . . H23A H 1.0319 -0.2002 0.3031 0.098 Uiso 1 1 calc R . . C24 C 0.9705(2) -0.0530(3) 0.21745(17) 0.0663(7) Uani 1 1 d . . . H24A H 0.9027 -0.0941 0.2110 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 N1 0.0491(12) 0.0999(16) 0.0517(13) -0.0110(12) 0.0071(10) -0.0135(11) C1 0.0402(13) 0.0518(14) 0.0578(16) -0.0018(12) 0.0051(12) 0.0035(11) C2 0.0478(14) 0.0486(14) 0.0517(15) -0.0002(12) 0.0074(12) 0.0075(11) C3 0.0632(16) 0.0605(16) 0.0621(17) 0.0042(13) 0.0167(14) 0.0027(13) C4 0.0574(17) 0.0702(19) 0.081(2) 0.0071(16) 0.0130(15) -0.0124(14) C5 0.0576(16) 0.0587(16) 0.078(2) 0.0029(14) -0.0039(14) -0.0080(13) C6 0.0542(15) 0.0571(15) 0.0587(16) -0.0012(13) 0.0054(13) 0.0007(13) C7 0.0550(15) 0.0570(15) 0.0432(14) 0.0050(12) 0.0077(11) 0.0044(12) C8 0.0618(17) 0.0772(18) 0.0666(18) -0.0087(15) -0.0068(14) 0.0142(15) C9 0.0641(18) 0.105(2) 0.079(2) -0.0077(19) -0.0127(16) 0.0026(18) C10 0.097(2) 0.088(2) 0.0617(19) 0.0023(17) -0.0163(17) -0.0187(19) C11 0.109(2) 0.0685(18) 0.0560(17) -0.0052(15) 0.0034(17) -0.0025(19) C12 0.0690(16) 0.0645(17) 0.0528(15) 0.0017(14) 0.0093(13) 0.0058(14) C13 0.0513(15) 0.0605(16) 0.0513(16) -0.0038(12) 0.0067(12) -0.0113(12) C14 0.0511(14) 0.0502(14) 0.0581(16) -0.0024(12) 0.0110(12) -0.0073(12) C15 0.0629(16) 0.0638(16) 0.0638(17) -0.0005(14) 0.0244(14) -0.0036(13) C16 0.0793(19) 0.0806(19) 0.0594(17) 0.0089(15) 0.0135(15) -0.0059(16) C17 0.0645(18) 0.083(2) 0.070(2) 0.0126(16) 0.0056(14) -0.0044(15) C18 0.0528(15) 0.0766(18) 0.0647(18) 0.0002(15) 0.0070(14) -0.0025(13) C19 0.0560(16) 0.0487(15) 0.0606(16) -0.0050(12) 0.0149(13) -0.0011(12) C20 0.0608(17) 0.0620(17) 0.094(2) 0.0063(15) 0.0102(16) 0.0016(14) C21 0.066(2) 0.087(2) 0.117(3) 0.002(2) -0.0046(19) 0.0034(17) C22 0.091(2) 0.082(2) 0.095(2) 0.007(2) -0.0070(19) 0.0216(19) C23 0.104(2) 0.0650(19) 0.077(2) 0.0066(16) 0.0098(18) 0.0063(19) C24 0.0771(18) 0.0565(16) 0.0661(17) -0.0023(14) 0.0101(15) -0.0032(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.381(3) . ? N1 C13 1.403(3) . ? C1 C6 1.386(3) . ? C1 C2 1.409(3) . ? C2 C3 1.382(3) . ? C2 C7 1.478(3) . ? C3 C4 1.364(3) . ? C4 C5 1.367(3) . ? C5 C6 1.369(3) . ? C7 C12 1.380(3) . ? C7 C8 1.381(3) . ? C8 C9 1.367(3) . ? C9 C10 1.366(4) . ? C10 C11 1.361(4) . ? C11 C12 1.378(3) . ? C13 C18 1.377(3) . ? C13 C14 1.396(3) . ? C14 C15 1.382(3) . ? C14 C19 1.481(3) . ? C15 C16 1.372(3) . ? C16 C17 1.366(3) . ? C17 C18 1.375(3) . ? C19 C24 1.381(3) . ? C19 C20 1.381(3) . ? C20 C21 1.369(3) . ? C21 C22 1.370(4) . ? C22 C23 1.365(4) . ? C23 C24 1.370(3) . ? 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 C1 N1 C13 127.97(19) . . ? N1 C1 C6 121.9(2) . . ? N1 C1 C2 119.4(2) . . ? C6 C1 C2 118.7(2) . . ? C3 C2 C1 118.3(2) . . ? C3 C2 C7 120.7(2) . . ? C1 C2 C7 121.0(2) . . ? C4 C3 C2 122.2(2) . . ? C3 C4 C5 119.1(2) . . ? C4 C5 C6 120.7(2) . . ? C5 C6 C1 120.8(2) . . ? C12 C7 C8 117.6(2) . . ? C12 C7 C2 121.0(2) . . ? C8 C7 C2 121.4(2) . . ? C9 C8 C7 121.2(3) . . ? C10 C9 C8 120.3(3) . . ? C11 C10 C9 119.8(3) . . ? C10 C11 C12 120.0(3) . . ? C11 C12 C7 121.1(3) . . ? C18 C13 C14 120.0(2) . . ? C18 C13 N1 120.3(2) . . ? C14 C13 N1 119.6(2) . . ? C15 C14 C13 117.6(2) . . ? C15 C14 C19 120.8(2) . . ? C13 C14 C19 121.6(2) . . ? C16 C15 C14 122.4(2) . . ? C17 C16 C15 119.2(2) . . ? C16 C17 C18 120.1(3) . . ? C17 C18 C13 120.8(2) . . ? C24 C19 C20 117.5(2) . . ? C24 C19 C14 121.5(2) . . ? C20 C19 C14 121.0(2) . . ? C21 C20 C19 121.5(3) . . ? C20 C21 C22 120.0(3) . . ? C23 C22 C21 119.3(3) . . ? C22 C23 C24 120.7(3) . . ? C23 C24 C19 120.9(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.38 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.108 _refine_diff_density_min -0.128 _refine_diff_density_rms 0.027 #===END data_(C6H4Ph)2NH _database_code_depnum_ccdc_archive 'CCDC 674910' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C24 H19 N' _chemical_formula_weight 321.40 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.782(3) _cell_length_b 12.569(3) _cell_length_c 23.822(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3527.8(16) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.613290 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 27103 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 23.25 _reflns_number_total 2524 _reflns_number_gt 1773 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0444P)^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_number_reflns 2524 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0870 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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 N1 N 0.17107(15) 0.91114(13) 0.13244(7) 0.0628(5) Uani 1 1 d . . . H1A H 0.1557 0.9602 0.1565 0.075 Uiso 1 1 calc R . . C2 C 0.17954(15) 1.03482(14) 0.05330(7) 0.0449(5) Uani 1 1 d . . . C3 C 0.30285(18) 0.88219(16) 0.05560(9) 0.0598(6) Uani 1 1 d . . . H3A H 0.3272 0.8202 0.0732 0.072 Uiso 1 1 calc R . . C4 C 0.16266(16) 0.77160(15) 0.20316(8) 0.0497(5) Uani 1 1 d . . . C5 C 0.14901(16) 0.80572(15) 0.14750(8) 0.0503(5) Uani 1 1 d . . . C6 C 0.21717(16) 0.94218(15) 0.08001(8) 0.0492(5) Uani 1 1 d . . . C7 C 0.08764(16) 1.10352(13) 0.07640(8) 0.0462(5) Uani 1 1 d . . . C8 C 0.10928(17) 0.73382(17) 0.10758(9) 0.0602(6) Uani 1 1 d . . . H8A H 0.0987 0.7565 0.0708 0.072 Uiso 1 1 calc R . . C9 C 0.09103(17) 1.14481(14) 0.13031(8) 0.0504(5) Uani 1 1 d . . . H9A H 0.1505 1.1262 0.1540 0.060 Uiso 1 1 calc R . . C10 C 0.23145(17) 1.06333(16) 0.00306(8) 0.0559(5) Uani 1 1 d . . . H10A H 0.2075 1.1248 -0.0152 0.067 Uiso 1 1 calc R . . C11 C 0.00790(18) 1.21309(16) 0.14947(9) 0.0605(6) Uani 1 1 d . . . H11A H 0.0119 1.2404 0.1857 0.073 Uiso 1 1 calc R . . C12 C -0.00278(18) 1.13327(15) 0.04229(8) 0.0570(6) Uani 1 1 d . . . H12A H -0.0069 1.1074 0.0058 0.068 Uiso 1 1 calc R . . C13 C 0.31685(19) 1.00387(19) -0.02058(9) 0.0653(6) Uani 1 1 d . . . H13A H 0.3502 1.0251 -0.0541 0.078 Uiso 1 1 calc R . . C14 C 0.20804(17) 0.84243(16) 0.24773(8) 0.0511(5) Uani 1 1 d . . . C15 C 0.10016(19) 0.59556(17) 0.17578(11) 0.0697(6) Uani 1 1 d . . . H15A H 0.0851 0.5252 0.1853 0.084 Uiso 1 1 calc R . . C16 C 0.35242(19) 0.91254(17) 0.00597(9) 0.0651(6) Uani 1 1 d . . . H16A H 0.4099 0.8715 -0.0097 0.078 Uiso 1 1 calc R . . C17 C 0.13741(18) 0.66617(16) 0.21585(9) 0.0606(6) Uani 1 1 d . . . H17A H 0.1460 0.6427 0.2526 0.073 Uiso 1 1 calc R . . C18 C -0.08652(19) 1.20056(17) 0.06176(10) 0.0670(6) Uani 1 1 d . . . H18A H -0.1470 1.2186 0.0385 0.080 Uiso 1 1 calc R . . C19 C 0.15248(19) 0.93419(16) 0.26478(8) 0.0595(6) Uani 1 1 d . . . H19A H 0.0856 0.9542 0.2469 0.071 Uiso 1 1 calc R . . C20 C -0.08108(19) 1.24080(17) 0.11482(10) 0.0665(6) Uani 1 1 d . . . H20A H -0.1372 1.2868 0.1276 0.080 Uiso 1 1 calc R . . C21 C 0.30733(19) 0.81595(19) 0.27572(9) 0.0698(7) Uani 1 1 d . . . H21A H 0.3462 0.7546 0.2655 0.084 Uiso 1 1 calc R . . C22 C 0.08538(18) 0.62978(18) 0.12149(10) 0.0660(6) Uani 1 1 d . . . H22A H 0.0593 0.5829 0.0942 0.079 Uiso 1 1 calc R . . C23 C 0.1946(2) 0.99651(19) 0.30784(9) 0.0725(7) Uani 1 1 d . . . H23A H 0.1554 1.0572 0.3190 0.087 Uiso 1 1 calc R . . C24 C 0.3495(2) 0.8783(2) 0.31827(10) 0.0828(7) Uani 1 1 d . . . H24A H 0.4163 0.8587 0.3364 0.099 Uiso 1 1 calc R . . C25 C 0.2942(2) 0.9690(2) 0.33424(10) 0.0806(7) Uani 1 1 d . . . H25A H 0.3237 1.0117 0.3626 0.097 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 N1 0.0940(14) 0.0471(10) 0.0472(10) 0.0058(8) 0.0121(10) 0.0145(9) C2 0.0482(12) 0.0443(11) 0.0422(11) 0.0012(9) -0.0042(9) -0.0018(9) C3 0.0661(14) 0.0564(13) 0.0571(14) 0.0034(11) -0.0001(12) 0.0116(11) C4 0.0479(12) 0.0527(13) 0.0485(12) 0.0051(10) 0.0094(10) 0.0098(10) C5 0.0499(12) 0.0507(12) 0.0504(12) 0.0056(10) 0.0062(10) 0.0111(10) C6 0.0574(13) 0.0496(12) 0.0406(11) 0.0013(10) -0.0009(10) 0.0029(10) C7 0.0514(12) 0.0394(10) 0.0479(12) 0.0055(9) -0.0034(10) -0.0053(9) C8 0.0597(14) 0.0670(15) 0.0538(13) 0.0048(11) 0.0004(11) 0.0067(12) C9 0.0493(12) 0.0507(12) 0.0512(13) 0.0032(10) -0.0033(10) -0.0017(10) C10 0.0598(14) 0.0564(13) 0.0514(13) 0.0082(10) -0.0011(11) 0.0003(11) C11 0.0624(14) 0.0638(14) 0.0553(13) -0.0048(11) 0.0042(12) 0.0002(12) C12 0.0640(14) 0.0531(12) 0.0539(12) 0.0005(10) -0.0118(11) 0.0025(11) C13 0.0672(16) 0.0753(15) 0.0533(13) 0.0049(12) 0.0105(12) -0.0033(13) C14 0.0498(12) 0.0602(13) 0.0434(11) 0.0107(10) 0.0079(10) 0.0030(11) C15 0.0688(15) 0.0545(14) 0.0860(18) 0.0053(13) 0.0242(14) -0.0020(11) C16 0.0620(14) 0.0697(15) 0.0636(15) -0.0007(12) 0.0085(12) 0.0100(12) C17 0.0633(14) 0.0593(14) 0.0591(14) 0.0123(11) 0.0144(11) 0.0077(11) C18 0.0594(15) 0.0675(14) 0.0740(16) 0.0030(13) -0.0109(13) 0.0116(12) C19 0.0624(14) 0.0634(14) 0.0526(13) 0.0046(11) 0.0026(11) 0.0050(12) C20 0.0612(15) 0.0627(14) 0.0755(17) 0.0012(12) 0.0092(13) 0.0120(12) C21 0.0574(15) 0.0922(18) 0.0599(14) 0.0079(13) 0.0051(12) 0.0106(13) C22 0.0581(14) 0.0682(16) 0.0717(16) -0.0048(13) 0.0062(12) -0.0043(12) C23 0.0844(19) 0.0695(15) 0.0636(15) -0.0025(13) 0.0125(14) -0.0063(14) C24 0.0552(15) 0.125(2) 0.0682(17) 0.0050(17) -0.0056(13) -0.0043(16) C25 0.0806(19) 0.098(2) 0.0633(16) -0.0020(14) 0.0038(15) -0.0324(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C5 1.397(2) . ? N1 C6 1.417(2) . ? C2 C10 1.391(3) . ? C2 C6 1.399(2) . ? C2 C7 1.490(2) . ? C3 C16 1.373(3) . ? C3 C6 1.388(3) . ? C4 C17 1.392(3) . ? C4 C5 1.403(3) . ? C4 C14 1.485(3) . ? C5 C8 1.393(3) . ? C7 C9 1.386(2) . ? C7 C12 1.391(3) . ? C8 C22 1.378(3) . ? C9 C11 1.380(3) . ? C10 C13 1.374(3) . ? C11 C20 1.379(3) . ? C12 C18 1.380(3) . ? C13 C16 1.376(3) . ? C14 C21 1.387(3) . ? C14 C19 1.387(3) . ? C15 C22 1.374(3) . ? C15 C17 1.375(3) . ? C18 C20 1.363(3) . ? C19 C23 1.383(3) . ? C21 C24 1.375(3) . ? C23 C25 1.376(3) . ? C24 C25 1.367(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 N1 C6 123.97(16) . . ? C10 C2 C6 117.80(18) . . ? C10 C2 C7 119.21(16) . . ? C6 C2 C7 122.99(17) . . ? C16 C3 C6 121.29(19) . . ? C17 C4 C5 118.17(19) . . ? C17 C4 C14 119.50(18) . . ? C5 C4 C14 122.26(18) . . ? C8 C5 N1 120.18(18) . . ? C8 C5 C4 119.04(18) . . ? N1 C5 C4 120.75(18) . . ? C3 C6 C2 119.49(18) . . ? C3 C6 N1 119.91(17) . . ? C2 C6 N1 120.57(17) . . ? C9 C7 C12 117.56(18) . . ? C9 C7 C2 122.57(17) . . ? C12 C7 C2 119.77(17) . . ? C22 C8 C5 121.3(2) . . ? C11 C9 C7 121.27(19) . . ? C13 C10 C2 122.31(19) . . ? C20 C11 C9 119.9(2) . . ? C18 C12 C7 121.07(19) . . ? C10 C13 C16 119.2(2) . . ? C21 C14 C19 117.2(2) . . ? C21 C14 C4 120.23(19) . . ? C19 C14 C4 122.54(19) . . ? C22 C15 C17 119.5(2) . . ? C3 C16 C13 119.9(2) . . ? C15 C17 C4 122.1(2) . . ? C20 C18 C12 120.4(2) . . ? C23 C19 C14 121.3(2) . . ? C18 C20 C11 119.8(2) . . ? C24 C21 C14 121.5(2) . . ? C15 C22 C8 119.8(2) . . ? C25 C23 C19 120.2(2) . . ? C25 C24 C21 120.6(2) . . ? C24 C25 C23 119.3(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.202 _refine_diff_density_min -0.145 _refine_diff_density_rms 0.028 #===end data_(2-C6H4-Ph)tBuNLi(THF)2 _database_code_depnum_ccdc_archive 'CCDC 674911' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C24 H34 Li N O2' _chemical_formula_weight 375.46 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.1057(19) _cell_length_b 12.335(3) _cell_length_c 10.325(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.574(3) _cell_angle_gamma 90.00 _cell_volume 1105.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.714207 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 8897 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3160 _reflns_number_gt 2801 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0879P)^2^+0.2551P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(19) _refine_ls_number_reflns 3160 _refine_ls_number_parameters 253 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.010 _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 -0.0844(6) 0.7586(4) -0.0836(5) 0.0472(12) Uani 1 1 d . . . N1 N 0.0077(3) 0.7189(2) 0.1069(2) 0.0449(6) Uani 1 1 d . . . O1 O -0.2384(3) 0.87472(19) -0.1468(2) 0.0605(6) Uani 1 1 d . . . O2 O -0.1232(3) 0.64915(17) -0.2252(2) 0.0583(6) Uani 1 1 d . . . C1 C 0.1535(3) 0.7414(2) 0.1853(3) 0.0393(7) Uani 1 1 d . . . C2 C 0.2604(3) 0.7853(2) 0.1215(3) 0.0396(7) Uani 1 1 d . . . C3 C 0.4104(3) 0.8110(3) 0.1963(3) 0.0468(7) Uani 1 1 d . . . H3A H 0.4779 0.8388 0.1499 0.056 Uiso 1 1 calc R . . C4 C 0.4659(4) 0.7979(3) 0.3361(3) 0.0531(8) Uani 1 1 d . . . H4A H 0.5683 0.8174 0.3859 0.064 Uiso 1 1 calc R . . C5 C 0.3666(4) 0.7555(3) 0.3992(3) 0.0510(8) Uani 1 1 d . . . H5A H 0.4019 0.7444 0.4947 0.061 Uiso 1 1 calc R . . C6 C 0.2163(3) 0.7281(3) 0.3286(3) 0.0458(8) Uani 1 1 d . . . H6A H 0.1523 0.6993 0.3778 0.055 Uiso 1 1 calc R . . C7 C 0.2191(3) 0.7989(2) -0.0299(3) 0.0394(7) Uani 1 1 d . . . C8 C 0.1313(4) 0.8854(3) -0.0972(3) 0.0485(8) Uani 1 1 d . . . H8A H 0.0911 0.9361 -0.0475 0.058 Uiso 1 1 calc R . . C9 C 0.1014(4) 0.8991(3) -0.2369(3) 0.0561(8) Uani 1 1 d . . . H9A H 0.0392 0.9579 -0.2817 0.067 Uiso 1 1 calc R . . C10 C 0.1608(4) 0.8287(3) -0.3091(3) 0.0569(9) Uani 1 1 d . . . H10A H 0.1419 0.8389 -0.4040 0.068 Uiso 1 1 calc R . . C11 C 0.2487(4) 0.7423(3) -0.2445(3) 0.0562(9) Uani 1 1 d . . . H11A H 0.2891 0.6924 -0.2949 0.067 Uiso 1 1 calc R . . C12 C 0.2779(4) 0.7283(2) -0.1064(3) 0.0497(8) Uani 1 1 d . . . H12A H 0.3397 0.6690 -0.0627 0.060 Uiso 1 1 calc R . . C13 C -0.1031(4) 0.6668(3) 0.1654(3) 0.0531(8) Uani 1 1 d . . . C14 C -0.0513(5) 0.5538(3) 0.2217(4) 0.0758(12) Uani 1 1 d . . . H14A H -0.0246 0.5106 0.1523 0.114 Uiso 1 1 calc R . . H14B H -0.1350 0.5181 0.2467 0.114 Uiso 1 1 calc R . . H14C H 0.0391 0.5601 0.3021 0.114 Uiso 1 1 calc R . . C15 C -0.1460(4) 0.7359(3) 0.2726(4) 0.0616(9) Uani 1 1 d . . . H15A H -0.0548 0.7462 0.3514 0.092 Uiso 1 1 calc R . . H15B H -0.2264 0.6990 0.3012 0.092 Uiso 1 1 calc R . . H15C H -0.1842 0.8067 0.2335 0.092 Uiso 1 1 calc R . . C16 C -0.2541(5) 0.6541(4) 0.0489(4) 0.0830(13) Uani 1 1 d . . . H16A H -0.2352 0.6107 -0.0239 0.124 Uiso 1 1 calc R . . H16B H -0.2925 0.7258 0.0137 0.124 Uiso 1 1 calc R . . H16C H -0.3309 0.6176 0.0828 0.124 Uiso 1 1 calc R . . C17 C -0.3276(9) 0.9021(6) -0.2795(5) 0.150(3) Uani 1 1 d . . . H17A H -0.3653 0.8351 -0.3318 0.180 Uiso 1 1 calc R . . H17B H -0.2632 0.9420 -0.3254 0.180 Uiso 1 1 calc R . . C18 C -0.4574(4) 0.9686(3) -0.2763(3) 0.0603(9) Uani 1 1 d . . . H18A H -0.5557 0.9345 -0.3289 0.072 Uiso 1 1 calc R . . H18B H -0.4505 1.0414 -0.3145 0.072 Uiso 1 1 calc R . . C19 C -0.4463(4) 0.9762(3) -0.1283(3) 0.0621(9) Uani 1 1 d . . . H19A H -0.4739 1.0495 -0.1043 0.074 Uiso 1 1 calc R . . H19B H -0.5130 0.9219 -0.1031 0.074 Uiso 1 1 calc R . . C20 C -0.2809(6) 0.9524(4) -0.0630(4) 0.0910(15) Uani 1 1 d . . . H20A H -0.2186 1.0192 -0.0563 0.109 Uiso 1 1 calc R . . H20B H -0.2643 0.9230 0.0295 0.109 Uiso 1 1 calc R . . C21 C -0.1976(6) 0.6483(4) -0.3669(4) 0.0835(14) Uani 1 1 d . . . H21A H -0.1594 0.7081 -0.4121 0.100 Uiso 1 1 calc R . . H21B H -0.3105 0.6558 -0.3866 0.100 Uiso 1 1 calc R . . C22 C -0.1576(12) 0.5404(5) -0.4136(6) 0.159(3) Uani 1 1 d . . . H22A H -0.2502 0.4936 -0.4417 0.191 Uiso 1 1 calc R . . H22B H -0.1182 0.5499 -0.4924 0.191 Uiso 1 1 calc R . . C23 C -0.0441(8) 0.4924(4) -0.3051(6) 0.113(2) Uani 1 1 d . . . H23A H -0.0627 0.4135 -0.3013 0.136 Uiso 1 1 calc R . . H23B H 0.0596 0.5037 -0.3150 0.136 Uiso 1 1 calc R . . C24 C -0.0563(6) 0.5439(3) -0.1880(5) 0.0880(14) Uani 1 1 d . . . H24A H 0.0469 0.5512 -0.1207 0.106 Uiso 1 1 calc R . . H24B H -0.1219 0.5004 -0.1467 0.106 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 0.053(3) 0.046(3) 0.040(3) -0.003(2) 0.010(2) 0.005(2) N1 0.0489(15) 0.0510(15) 0.0361(14) -0.0034(11) 0.0146(11) -0.0093(12) O1 0.0557(13) 0.0612(14) 0.0576(14) -0.0040(12) 0.0066(11) 0.0100(11) O2 0.0776(16) 0.0488(13) 0.0403(13) -0.0067(10) 0.0053(11) 0.0098(12) C1 0.0415(16) 0.0377(15) 0.0385(18) -0.0012(12) 0.0118(14) 0.0070(12) C2 0.0435(17) 0.0393(15) 0.0373(16) 0.0011(12) 0.0140(13) 0.0050(13) C3 0.0432(17) 0.0554(18) 0.0459(18) -0.0005(15) 0.0195(14) 0.0009(14) C4 0.0429(18) 0.070(2) 0.0431(19) -0.0067(16) 0.0081(15) 0.0049(16) C5 0.0509(19) 0.068(2) 0.0321(15) 0.0030(14) 0.0093(14) 0.0097(16) C6 0.0525(19) 0.0526(18) 0.0341(17) 0.0034(14) 0.0157(15) -0.0007(14) C7 0.0397(15) 0.0373(15) 0.0416(17) 0.0019(13) 0.0129(13) -0.0014(13) C8 0.0521(18) 0.0463(18) 0.0507(19) 0.0065(15) 0.0211(15) 0.0061(15) C9 0.062(2) 0.056(2) 0.049(2) 0.0141(16) 0.0152(16) 0.0066(16) C10 0.072(2) 0.065(2) 0.0359(17) 0.0038(15) 0.0199(16) -0.0101(18) C11 0.081(2) 0.0468(18) 0.0474(19) -0.0005(16) 0.0298(18) -0.0002(17) C12 0.066(2) 0.0410(17) 0.0474(18) 0.0088(14) 0.0240(16) 0.0050(15) C13 0.0564(19) 0.062(2) 0.0424(18) -0.0026(16) 0.0174(15) -0.0178(16) C14 0.104(3) 0.067(2) 0.071(3) -0.0024(19) 0.048(2) -0.026(2) C15 0.052(2) 0.082(3) 0.056(2) 0.0008(18) 0.0245(17) -0.0076(17) C16 0.070(3) 0.121(4) 0.061(2) -0.006(2) 0.024(2) -0.044(3) C17 0.175(6) 0.207(7) 0.067(3) 0.040(4) 0.035(4) 0.136(6) C18 0.066(2) 0.057(2) 0.050(2) 0.0030(16) 0.0051(16) 0.0084(17) C19 0.060(2) 0.058(2) 0.068(2) -0.0057(17) 0.0201(18) 0.0070(17) C20 0.107(4) 0.082(3) 0.062(3) -0.015(2) -0.007(2) 0.022(3) C21 0.108(3) 0.070(3) 0.052(2) -0.0043(19) -0.007(2) 0.004(2) C22 0.310(10) 0.084(4) 0.060(3) -0.033(3) 0.021(5) 0.025(5) C23 0.158(6) 0.073(3) 0.139(5) -0.009(3) 0.091(5) 0.017(3) C24 0.104(3) 0.052(2) 0.083(3) -0.009(2) -0.010(2) 0.015(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 Li1 O2 1.943(5) . ? Li1 N1 1.952(5) . ? Li1 O1 1.973(5) . ? Li1 C8 2.548(6) . ? Li1 C16 2.683(7) . ? Li1 C7 2.695(6) . ? N1 C1 1.359(4) . ? N1 C13 1.472(4) . ? O1 C17 1.407(5) . ? O1 C20 1.420(5) . ? O2 C21 1.414(4) . ? O2 C24 1.436(4) . ? C1 C6 1.425(4) . ? C1 C2 1.436(4) . ? C2 C3 1.388(4) . ? C2 C7 1.502(4) . ? C3 C4 1.387(4) . ? C4 C5 1.368(5) . ? C5 C6 1.384(5) . ? C7 C12 1.386(4) . ? C7 C8 1.388(4) . ? C8 C9 1.395(4) . ? C9 C10 1.360(5) . ? C10 C11 1.377(5) . ? C11 C12 1.380(5) . ? C13 C14 1.529(5) . ? C13 C16 1.537(5) . ? C13 C15 1.539(5) . ? C17 C18 1.448(6) . ? C18 C19 1.504(5) . ? C19 C20 1.482(6) . ? C21 C22 1.498(7) . ? C22 C23 1.406(9) . ? C23 C24 1.399(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 O2 Li1 N1 120.6(3) . . ? O2 Li1 O1 107.8(2) . . ? N1 Li1 O1 124.1(3) . . ? O2 Li1 C8 110.7(3) . . ? N1 Li1 C8 96.1(2) . . ? O1 Li1 C8 91.1(2) . . ? O2 Li1 C16 92.7(2) . . ? N1 Li1 C16 60.29(18) . . ? O1 Li1 C16 93.2(2) . . ? C8 Li1 C16 153.6(2) . . ? O2 Li1 C7 103.0(2) . . ? N1 Li1 C7 74.78(18) . . ? O1 Li1 C7 121.1(2) . . ? C8 Li1 C7 30.54(11) . . ? C16 Li1 C7 134.1(2) . . ? C1 N1 C13 120.8(2) . . ? C1 N1 Li1 126.5(3) . . ? C13 N1 Li1 112.6(2) . . ? C17 O1 C20 104.3(3) . . ? C17 O1 Li1 129.8(3) . . ? C20 O1 Li1 125.8(3) . . ? C21 O2 C24 107.6(3) . . ? C21 O2 Li1 134.9(3) . . ? C24 O2 Li1 117.4(3) . . ? N1 C1 C6 127.5(3) . . ? N1 C1 C2 118.6(2) . . ? C6 C1 C2 113.9(2) . . ? C3 C2 C1 121.3(3) . . ? C3 C2 C7 116.7(3) . . ? C1 C2 C7 121.9(2) . . ? C4 C3 C2 122.7(3) . . ? C5 C4 C3 117.0(3) . . ? C4 C5 C6 122.2(3) . . ? C5 C6 C1 122.8(3) . . ? C12 C7 C8 117.4(3) . . ? C12 C7 C2 120.3(3) . . ? C8 C7 C2 122.2(3) . . ? C12 C7 Li1 108.4(2) . . ? C8 C7 Li1 68.8(2) . . ? C2 C7 Li1 96.45(19) . . ? C7 C8 C9 121.0(3) . . ? C7 C8 Li1 80.6(2) . . ? C9 C8 Li1 102.6(2) . . ? C10 C9 C8 120.2(3) . . ? C9 C10 C11 119.8(3) . . ? C10 C11 C12 120.0(3) . . ? C11 C12 C7 121.5(3) . . ? N1 C13 C14 112.5(3) . . ? N1 C13 C16 106.6(3) . . ? C14 C13 C16 107.8(3) . . ? N1 C13 C15 114.1(3) . . ? C14 C13 C15 110.4(3) . . ? C16 C13 C15 105.0(3) . . ? C13 C16 Li1 80.4(2) . . ? O1 C17 C18 110.5(4) . . ? C17 C18 C19 104.7(3) . . ? C20 C19 C18 101.4(3) . . ? O1 C20 C19 106.4(3) . . ? O2 C21 C22 104.7(3) . . ? C23 C22 C21 108.0(4) . . ? C24 C23 C22 105.4(5) . . ? C23 C24 O2 108.5(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.383 _refine_diff_density_min -0.191 _refine_diff_density_rms 0.034 #===end data_(2-C6H4-Ph)tBuNLi(OEt2) _database_code_depnum_ccdc_archive 'CCDC 674912' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C20 H28 Li N O' _chemical_formula_weight 305.37 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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 7.85(2) _cell_length_b 13.74(4) _cell_length_c 18.83(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.63(5) _cell_angle_gamma 90.00 _cell_volume 2007(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.060 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.388678 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 16083 _diffrn_reflns_av_R_equivalents 0.1775 _diffrn_reflns_av_sigmaI/netI 0.1401 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3529 _reflns_number_gt 1006 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.1268P)^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_number_reflns 3529 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2408 _refine_ls_R_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.3042 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.887 _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 -0.3335(12) 0.3149(7) 0.1340(6) 0.102(3) Uani 1 1 d . . . N1 N -0.1908(5) 0.2207(3) 0.0986(2) 0.0772(13) Uani 1 1 d . . . O1 O -0.4748(6) 0.4283(4) 0.1240(3) 0.1425(19) Uani 1 1 d . . . C1 C -0.0418(6) 0.1823(4) 0.1368(3) 0.0699(14) Uani 1 1 d . . . C2 C 0.0041(6) 0.2114(3) 0.2129(3) 0.0682(14) Uani 1 1 d . . . C3 C 0.1564(7) 0.1790(4) 0.2538(3) 0.0807(15) Uani 1 1 d . . . H3A H 0.1803 0.1989 0.3014 0.097 Uiso 1 1 calc R . . C4 C 0.2754(6) 0.1184(4) 0.2274(4) 0.0918(18) Uani 1 1 d . . . H4A H 0.3769 0.0985 0.2557 0.110 Uiso 1 1 calc R . . C5 C 0.2325(7) 0.0897(4) 0.1564(4) 0.0973(19) Uani 1 1 d . . . H5A H 0.3066 0.0478 0.1371 0.117 Uiso 1 1 calc R . . C6 C 0.0846(7) 0.1207(4) 0.1129(3) 0.0865(16) Uani 1 1 d . . . H6A H 0.0665 0.1001 0.0653 0.104 Uiso 1 1 calc R . . C7 C -0.1161(6) 0.2770(4) 0.2472(3) 0.0695(14) Uani 1 1 d . . . C8 C -0.0593(6) 0.3674(4) 0.2741(3) 0.0855(17) Uani 1 1 d . . . H8A H 0.0509 0.3885 0.2690 0.103 Uiso 1 1 calc R . . C9 C -0.1671(7) 0.4279(4) 0.3092(3) 0.0986(19) Uani 1 1 d . . . H9A H -0.1291 0.4891 0.3257 0.118 Uiso 1 1 calc R . . C10 C -0.3281(8) 0.3956(5) 0.3186(3) 0.109(2) Uani 1 1 d . . . H10A H -0.3978 0.4347 0.3425 0.131 Uiso 1 1 calc R . . C11 C -0.3877(8) 0.3049(6) 0.2926(3) 0.113(2) Uani 1 1 d . . . H11A H -0.4966 0.2833 0.2993 0.136 Uiso 1 1 calc R . . C12 C -0.2826(6) 0.2465(4) 0.2565(3) 0.0907(17) Uani 1 1 d . . . H12A H -0.2992 0.1761 0.2601 0.109 Uiso 1 1 calc R . . C13 C -0.2477(7) 0.1908(4) 0.0219(3) 0.0871(16) Uani 1 1 d . . . C14 C -0.4237(7) 0.2418(5) -0.0012(3) 0.125(2) Uani 1 1 d . . . H14A H -0.5042 0.2206 0.0293 0.188 Uiso 1 1 calc R . . H14B H -0.4669 0.2252 -0.0501 0.188 Uiso 1 1 calc R . . H14C H -0.4090 0.3110 0.0029 0.188 Uiso 1 1 calc R . . C15 C -0.1257(9) 0.2287(5) -0.0297(3) 0.139(3) Uani 1 1 d . . . H15A H -0.0143 0.1991 -0.0175 0.208 Uiso 1 1 calc R . . H15B H -0.1148 0.2981 -0.0253 0.208 Uiso 1 1 calc R . . H15C H -0.1727 0.2122 -0.0783 0.208 Uiso 1 1 calc R . . C16 C -0.2815(8) 0.0803(5) 0.0123(3) 0.124(2) Uani 1 1 d . . . H16A H -0.3571 0.0592 0.0449 0.185 Uiso 1 1 calc R . . H16B H -0.1743 0.0457 0.0222 0.185 Uiso 1 1 calc R . . H16C H -0.3341 0.0675 -0.0362 0.185 Uiso 1 1 calc R . . C17 C -0.6526(12) 0.4192(12) 0.1396(6) 0.267(8) Uani 1 1 d . . . H17A H -0.6438 0.3818 0.1837 0.321 Uiso 1 1 calc R . . H17B H -0.6863 0.4844 0.1516 0.321 Uiso 1 1 calc R . . C18 C -0.7695(16) 0.3877(11) 0.1026(7) 0.303(9) Uani 1 1 d . . . H18A H -0.8695 0.3910 0.1263 0.455 Uiso 1 1 calc R . . H18B H -0.7470 0.3211 0.0916 0.455 Uiso 1 1 calc R . . H18C H -0.7895 0.4248 0.0589 0.455 Uiso 1 1 calc R . . C19 C -0.4134(19) 0.5242(9) 0.1262(7) 0.238(8) Uani 1 1 d . . . H19A H -0.4088 0.5503 0.1743 0.285 Uiso 1 1 calc R . . H19B H -0.4907 0.5645 0.0935 0.285 Uiso 1 1 calc R . . C20 C -0.2371(16) 0.5255(8) 0.1050(6) 0.213(5) Uani 1 1 d . . . H20B H -0.1949 0.5912 0.1064 0.320 Uiso 1 1 calc R . . H20C H -0.2425 0.5001 0.0572 0.320 Uiso 1 1 calc R . . H20D H -0.1609 0.4861 0.1378 0.320 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 0.113(7) 0.093(7) 0.102(8) -0.001(6) 0.020(6) 0.018(5) N1 0.080(3) 0.084(3) 0.065(3) -0.007(2) 0.006(2) 0.014(2) O1 0.134(4) 0.144(5) 0.141(4) -0.038(4) -0.006(3) 0.054(3) C1 0.070(3) 0.068(3) 0.073(4) 0.003(3) 0.015(3) 0.000(3) C2 0.064(3) 0.069(3) 0.073(4) 0.002(3) 0.014(3) -0.005(2) C3 0.075(3) 0.093(4) 0.071(4) 0.005(3) 0.003(3) -0.012(3) C4 0.063(3) 0.098(4) 0.111(5) 0.009(4) 0.000(3) 0.007(3) C5 0.085(4) 0.101(5) 0.106(5) -0.013(4) 0.014(4) 0.021(3) C6 0.086(4) 0.096(4) 0.079(4) -0.006(3) 0.021(3) 0.020(3) C7 0.063(3) 0.088(4) 0.058(3) 0.000(3) 0.012(2) -0.013(3) C8 0.076(3) 0.101(5) 0.082(4) -0.011(3) 0.018(3) -0.022(3) C9 0.097(4) 0.100(5) 0.102(5) -0.026(4) 0.024(4) -0.014(4) C10 0.104(5) 0.129(6) 0.099(5) -0.031(4) 0.033(4) -0.010(4) C11 0.093(4) 0.148(6) 0.109(5) -0.034(5) 0.050(4) -0.038(4) C12 0.083(4) 0.099(4) 0.097(4) -0.011(3) 0.036(3) -0.013(3) C13 0.102(4) 0.093(4) 0.063(4) -0.006(3) 0.001(3) 0.015(3) C14 0.124(5) 0.149(6) 0.091(5) -0.018(4) -0.020(4) 0.044(4) C15 0.167(6) 0.178(8) 0.074(5) 0.015(5) 0.028(5) 0.012(5) C16 0.157(6) 0.113(6) 0.093(5) -0.030(4) -0.009(4) 0.007(4) C17 0.097(6) 0.43(2) 0.260(13) -0.124(13) -0.012(8) 0.112(10) C18 0.268(14) 0.44(2) 0.226(14) -0.096(13) 0.132(11) -0.228(16) C19 0.37(2) 0.154(11) 0.167(11) 0.001(9) -0.021(12) 0.117(15) C20 0.342(16) 0.134(9) 0.158(9) 0.003(7) 0.021(11) -0.049(10) _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 N1 1.898(11) . ? Li1 O1 1.905(11) . ? Li1 C12 2.466(13) . ? Li1 C7 2.575(12) . ? Li1 C14 2.730(14) . ? N1 C1 1.382(6) . ? N1 C13 1.502(7) . ? O1 C19 1.401(13) . ? O1 C17 1.473(12) . ? C1 C6 1.428(7) . ? C1 C2 1.479(7) . ? C2 C3 1.394(7) . ? C2 C7 1.517(7) . ? C3 C4 1.397(8) . ? C4 C5 1.386(8) . ? C5 C6 1.383(7) . ? C7 C8 1.390(7) . ? C7 C12 1.407(7) . ? C8 C9 1.418(7) . ? C9 C10 1.375(8) . ? C10 C11 1.394(9) . ? C11 C12 1.398(8) . ? C13 C16 1.547(9) . ? C13 C14 1.551(8) . ? C13 C15 1.553(8) . ? C17 C18 1.150(11) . ? C19 C20 1.496(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 N1 Li1 O1 152.7(6) . . ? N1 Li1 C12 92.8(4) . . ? O1 Li1 C12 114.5(5) . . ? N1 Li1 C7 78.5(4) . . ? O1 Li1 C7 123.4(5) . . ? C12 Li1 C7 32.3(2) . . ? N1 Li1 C14 60.3(3) . . ? O1 Li1 C14 98.2(4) . . ? C12 Li1 C14 135.6(5) . . ? C7 Li1 C14 138.1(4) . . ? C1 N1 C13 120.2(4) . . ? C1 N1 Li1 125.0(5) . . ? C13 N1 Li1 114.7(4) . . ? C19 O1 C17 113.9(9) . . ? C19 O1 Li1 125.0(7) . . ? C17 O1 Li1 117.7(8) . . ? N1 C1 C6 129.4(5) . . ? N1 C1 C2 117.8(4) . . ? C6 C1 C2 112.7(4) . . ? C3 C2 C1 120.8(5) . . ? C3 C2 C7 119.4(5) . . ? C1 C2 C7 119.7(4) . . ? C2 C3 C4 123.9(6) . . ? C5 C4 C3 115.7(5) . . ? C6 C5 C4 123.0(5) . . ? C5 C6 C1 123.8(5) . . ? C8 C7 C12 118.2(5) . . ? C8 C7 C2 120.0(4) . . ? C12 C7 C2 121.6(5) . . ? C8 C7 Li1 104.9(4) . . ? C12 C7 Li1 69.6(4) . . ? C2 C7 Li1 98.4(4) . . ? C7 C8 C9 120.9(5) . . ? C10 C9 C8 119.6(6) . . ? C9 C10 C11 120.7(6) . . ? C10 C11 C12 119.5(5) . . ? C11 C12 C7 121.1(5) . . ? C11 C12 Li1 102.3(5) . . ? C7 C12 Li1 78.1(4) . . ? N1 C13 C16 113.7(5) . . ? N1 C13 C14 105.7(4) . . ? C16 C13 C14 106.3(5) . . ? N1 C13 C15 112.8(5) . . ? C16 C13 C15 111.5(5) . . ? C14 C13 C15 106.2(6) . . ? C13 C14 Li1 79.0(4) . . ? C18 C17 O1 127.1(12) . . ? O1 C19 C20 109.3(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.172 _refine_diff_density_min -0.174 _refine_diff_density_rms 0.038 #===end data_(2-C6H4-Ph)2NLi _database_code_depnum_ccdc_archive 'CCDC 674913' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C27 H21 Li N' _chemical_formula_weight 654.71 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 13.960(3) _cell_length_b 22.820(5) _cell_length_c 24.218(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7715(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.699412 _exptl_absorpt_correction_T_max 1.0000 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 15204 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 23.29 _reflns_number_total 1399 _reflns_number_gt 1181 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0431P)^2^+6.7791P] 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 1399 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.6250 0.1250 0.07387(15) 0.0360(9) Uani 1 2 d S . . N1 N 0.6250 0.05520(7) 0.1250 0.0303(4) Uani 1 2 d S . . C1 C 0.54032(11) 0.02211(6) 0.12950(6) 0.0294(4) Uani 1 1 d . . . C2 C 0.45645(11) 0.03597(6) 0.09973(6) 0.0304(4) Uani 1 1 d . . . C3 C 0.37152(11) 0.00612(7) 0.11137(6) 0.0359(4) Uani 1 1 d . . . H3A H 0.3150 0.0166 0.0919 0.043 Uiso 1 1 calc R . . C4 C 0.36699(12) -0.03805(7) 0.15023(7) 0.0390(4) Uani 1 1 d . . . H4A H 0.3081 -0.0573 0.1579 0.047 Uiso 1 1 calc R . . C5 C 0.45004(11) -0.05368(7) 0.17767(6) 0.0375(4) Uani 1 1 d . . . H5A H 0.4488 -0.0848 0.2037 0.045 Uiso 1 1 calc R . . C6 C 0.53428(11) -0.02442(6) 0.16753(6) 0.0340(4) Uani 1 1 d . . . H6A H 0.5904 -0.0360 0.1868 0.041 Uiso 1 1 calc R . . C7 C 0.45397(11) 0.07930(6) 0.05347(6) 0.0304(4) Uani 1 1 d . . . C8 C 0.51732(11) 0.07520(7) 0.00894(6) 0.0334(4) Uani 1 1 d . . . H8A H 0.5678 0.0473 0.0100 0.040 Uiso 1 1 calc R . . C9 C 0.50749(11) 0.11135(7) -0.03677(7) 0.0391(4) Uani 1 1 d . . . H9A H 0.5500 0.1072 -0.0672 0.047 Uiso 1 1 calc R . . C10 C 0.43631(12) 0.15327(7) -0.03830(7) 0.0439(5) Uani 1 1 d . . . H10A H 0.4304 0.1784 -0.0694 0.053 Uiso 1 1 calc R . . C11 C 0.37399(12) 0.15838(7) 0.00535(7) 0.0426(4) Uani 1 1 d . . . H11A H 0.3251 0.1873 0.0045 0.051 Uiso 1 1 calc R . . C12 C 0.38223(12) 0.12155(7) 0.05044(6) 0.0373(4) Uani 1 1 d . . . H12A H 0.3379 0.1252 0.0800 0.045 Uiso 1 1 calc R . . C13 C 0.12478(19) 0.09557(13) 0.07689(10) 0.0949(10) Uani 1 1 d . . . H13A H 0.1243 0.0748 0.0429 0.114 Uiso 1 1 calc R . . C14 C 0.1250 0.06577(17) 0.1250 0.0904(12) Uani 1 2 d S . . H14A H 0.1250 0.0241 0.1250 0.109 Uiso 1 2 calc SR . . 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 0.039(2) 0.0306(19) 0.038(2) 0.000 0.000 -0.0025(16) N1 0.0272(10) 0.0262(9) 0.0374(10) 0.000 -0.0021(8) 0.000 C1 0.0317(8) 0.0256(8) 0.0310(8) -0.0032(6) 0.0009(7) -0.0002(7) C2 0.0311(9) 0.0271(8) 0.0328(8) -0.0030(7) 0.0018(7) 0.0002(7) C3 0.0304(9) 0.0364(9) 0.0410(10) -0.0016(8) 0.0005(7) -0.0004(7) C4 0.0354(10) 0.0379(9) 0.0438(10) 0.0013(8) 0.0072(8) -0.0066(7) C5 0.0446(10) 0.0314(9) 0.0366(9) 0.0037(7) 0.0038(8) -0.0036(8) C6 0.0368(10) 0.0301(8) 0.0350(9) 0.0010(7) -0.0022(7) 0.0012(7) C7 0.0291(8) 0.0285(8) 0.0335(8) -0.0041(7) -0.0050(7) -0.0042(7) C8 0.0301(9) 0.0330(9) 0.0371(9) -0.0025(7) -0.0038(7) -0.0029(7) C9 0.0378(10) 0.0438(10) 0.0356(9) 0.0005(8) 0.0003(7) -0.0086(8) C10 0.0516(11) 0.0402(10) 0.0398(10) 0.0077(8) -0.0080(8) -0.0063(8) C11 0.0465(10) 0.0356(10) 0.0458(10) 0.0007(8) -0.0087(8) 0.0080(8) C12 0.0382(9) 0.0384(9) 0.0351(9) -0.0028(8) -0.0026(7) 0.0035(8) C13 0.0581(14) 0.159(3) 0.0680(15) -0.0406(16) 0.0191(14) -0.023(2) C14 0.0435(19) 0.085(3) 0.143(4) 0.000 0.036(2) 0.000 _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 N1 2.017(3) 14_545 ? Li1 N1 2.017(3) . ? Li1 C8 2.454(3) . ? Li1 C8 2.454(3) 14_545 ? Li1 Li1 2.476(7) 11_554 ? Li1 C7 2.6518(16) . ? Li1 C7 2.6518(16) 14_545 ? N1 C1 1.4069(17) 11_554 ? N1 C1 1.4069(17) . ? N1 Li1 2.017(3) 11_554 ? C1 C6 1.408(2) . ? C1 C2 1.411(2) . ? C2 C3 1.396(2) . ? C2 C7 1.495(2) . ? C3 C4 1.381(2) . ? C4 C5 1.383(2) . ? C5 C6 1.375(2) . ? C7 C12 1.392(2) . ? C7 C8 1.398(2) . ? C8 C9 1.388(2) . ? C9 C10 1.380(2) . ? C10 C11 1.374(2) . ? C11 C12 1.383(2) . ? C13 C13 1.343(6) 14_445 ? C13 C14 1.349(3) . ? C14 C13 1.349(3) 11_454 ? 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 N1 Li1 N1 104.28(18) 14_545 . ? N1 Li1 C8 139.36(4) 14_545 . ? N1 Li1 C8 91.58(5) . . ? N1 Li1 C8 91.58(5) 14_545 14_545 ? N1 Li1 C8 139.36(4) . 14_545 ? C8 Li1 C8 100.31(15) . 14_545 ? N1 Li1 Li1 52.14(9) 14_545 11_554 ? N1 Li1 Li1 52.14(9) . 11_554 ? C8 Li1 Li1 129.84(8) . 11_554 ? C8 Li1 Li1 129.84(8) 14_545 11_554 ? N1 Li1 C7 115.14(6) 14_545 . ? N1 Li1 C7 78.69(4) . . ? C8 Li1 C7 31.47(5) . . ? C8 Li1 C7 127.89(15) 14_545 . ? Li1 Li1 C7 100.74(8) 11_554 . ? N1 Li1 C7 78.69(4) 14_545 14_545 ? N1 Li1 C7 115.14(6) . 14_545 ? C8 Li1 C7 127.89(15) . 14_545 ? C8 Li1 C7 31.47(5) 14_545 14_545 ? Li1 Li1 C7 100.74(9) 11_554 14_545 ? C7 Li1 C7 158.52(17) . 14_545 ? C1 N1 C1 115.09(16) 11_554 . ? C1 N1 Li1 118.11(7) 11_554 11_554 ? C1 N1 Li1 112.09(7) . 11_554 ? C1 N1 Li1 112.09(7) 11_554 . ? C1 N1 Li1 118.12(7) . . ? Li1 N1 Li1 75.72(18) 11_554 . ? N1 C1 C6 120.38(13) . . ? N1 C1 C2 122.51(13) . . ? C6 C1 C2 116.97(14) . . ? C3 C2 C1 119.49(14) . . ? C3 C2 C7 117.03(13) . . ? C1 C2 C7 123.40(13) . . ? C4 C3 C2 122.19(15) . . ? C3 C4 C5 118.53(15) . . ? C6 C5 C4 120.39(15) . . ? C5 C6 C1 122.31(15) . . ? C12 C7 C8 117.45(14) . . ? C12 C7 C2 120.95(14) . . ? C8 C7 C2 121.28(13) . . ? C12 C7 Li1 112.66(10) . . ? C8 C7 Li1 66.45(11) . . ? C2 C7 Li1 95.72(11) . . ? C9 C8 C7 120.87(15) . . ? C9 C8 Li1 107.25(11) . . ? C7 C8 Li1 82.08(11) . . ? C10 C9 C8 120.32(16) . . ? C11 C10 C9 119.62(15) . . ? C10 C11 C12 120.22(16) . . ? C11 C12 C7 121.49(15) . . ? C13 C13 C14 120.27(18) 14_445 . ? C13 C14 C13 119.5(4) . 11_454 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.138 _refine_diff_density_min -0.145 _refine_diff_density_rms 0.027 #===end data_(2-C6H4-Ph)2NLi(THF)2 _database_code_depnum_ccdc_archive 'CCDC 674914' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C32 H33 Li N O2' _chemical_formula_weight 470.53 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' O O 0.0106 0.0060 '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 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 11.2795(18) _cell_length_b 9.7923(16) _cell_length_c 24.471(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.352(3) _cell_angle_gamma 90.00 _cell_volume 2666.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.722594 _exptl_absorpt_correction_T_max 1.0000 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 21490 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 23.33 _reflns_number_total 3855 _reflns_number_gt 2396 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.1239P)^2^+3.1512P] 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_number_reflns 3855 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1359 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.2630 _refine_ls_wR_factor_gt 0.2261 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Li1 Li 0.1899(8) 0.6875(9) 0.1348(4) 0.072(2) Uani 1 1 d . . . N1 N 0.1794(3) 0.4902(4) 0.11963(15) 0.0492(9) Uani 1 1 d . . . O1 O 0.2876(3) 0.7971(3) 0.09460(16) 0.0773(11) Uani 1 1 d . . . O2 O 0.1529(3) 0.7911(4) 0.19561(16) 0.0812(11) Uani 1 1 d . . . C1 C 0.2893(4) 0.4474(4) 0.10751(18) 0.0470(11) Uani 1 1 d . . . C2 C 0.3974(4) 0.4771(4) 0.14350(18) 0.0497(11) Uani 1 1 d . . . C3 C 0.5052(4) 0.4538(5) 0.1248(2) 0.0640(13) Uani 1 1 d . . . H3A H 0.5780 0.4747 0.1486 0.077 Uiso 1 1 calc R . . C4 C 0.5112(4) 0.4020(6) 0.0734(2) 0.0717(15) Uani 1 1 d . . . H4A H 0.5867 0.3900 0.0616 0.086 Uiso 1 1 calc R . . C5 C 0.4063(4) 0.3671(5) 0.0389(2) 0.0651(14) Uani 1 1 d . . . H5A H 0.4093 0.3286 0.0035 0.078 Uiso 1 1 calc R . . C6 C 0.2979(4) 0.3883(5) 0.05577(19) 0.0559(12) Uani 1 1 d . . . H6A H 0.2264 0.3624 0.0319 0.067 Uiso 1 1 calc R . . C7 C 0.3974(4) 0.5265(5) 0.20096(19) 0.0535(12) Uani 1 1 d . . . C8 C 0.3205(4) 0.4715(5) 0.2339(2) 0.0638(13) Uani 1 1 d . . . H8A H 0.2625 0.4057 0.2186 0.077 Uiso 1 1 calc R . . C9 C 0.3265(5) 0.5104(6) 0.2884(2) 0.0803(16) Uani 1 1 d . . . H9A H 0.2731 0.4711 0.3102 0.096 Uiso 1 1 calc R . . C10 C 0.4091(6) 0.6057(7) 0.3113(3) 0.0937(19) Uani 1 1 d . . . H10A H 0.4125 0.6326 0.3488 0.112 Uiso 1 1 calc R . . C11 C 0.4858(6) 0.6610(6) 0.2802(3) 0.0891(18) Uani 1 1 d . . . H11A H 0.5440 0.7259 0.2962 0.107 Uiso 1 1 calc R . . C12 C 0.4797(5) 0.6232(5) 0.2249(2) 0.0714(15) Uani 1 1 d . . . H12A H 0.5327 0.6642 0.2032 0.086 Uiso 1 1 calc R . . C13 C 0.0846(4) 0.4012(5) 0.11158(17) 0.0478(11) Uani 1 1 d . . . C14 C -0.0355(4) 0.4499(5) 0.09825(18) 0.0546(12) Uani 1 1 d . . . C15 C -0.1292(4) 0.3584(6) 0.0974(2) 0.0714(15) Uani 1 1 d . . . H15A H -0.2092 0.3921 0.0892 0.086 Uiso 1 1 calc R . . C16 C -0.1124(5) 0.2221(7) 0.1077(2) 0.0822(18) Uani 1 1 d . . . H16A H -0.1793 0.1630 0.1075 0.099 Uiso 1 1 calc R . . C17 C 0.0038(5) 0.1713(6) 0.1185(2) 0.0732(15) Uani 1 1 d . . . H17A H 0.0172 0.0764 0.1247 0.088 Uiso 1 1 calc R . . C18 C 0.1001(4) 0.2597(5) 0.12021(19) 0.0600(13) Uani 1 1 d . . . H18A H 0.1793 0.2237 0.1274 0.072 Uiso 1 1 calc R . . C19 C -0.0620(4) 0.5961(5) 0.08223(19) 0.0597(13) Uani 1 1 d . . . C20 C 0.0038(4) 0.6639(5) 0.0472(2) 0.0655(14) Uani 1 1 d . . . H20A H 0.0242 0.6040 0.0170 0.079 Uiso 1 1 calc R . . C21 C -0.0252(6) 0.7952(7) 0.0295(3) 0.0857(18) Uani 1 1 d . . . H21A H 0.0193 0.8390 0.0048 0.103 Uiso 1 1 calc R . . C22 C -0.1157(7) 0.8611(8) 0.0471(3) 0.102(2) Uani 1 1 d . . . H22A H -0.1327 0.9525 0.0353 0.122 Uiso 1 1 calc R . . C23 C -0.1841(6) 0.8017(7) 0.0814(3) 0.093(2) Uani 1 1 d . . . H23A H -0.2481 0.8506 0.0932 0.112 Uiso 1 1 calc R . . C24 C -0.1584(5) 0.6660(7) 0.0990(2) 0.0833(17) Uani 1 1 d . . . H24A H -0.2064 0.6220 0.1222 0.100 Uiso 1 1 calc R . . C25 C 0.3371(8) 0.7545(7) 0.0478(4) 0.137(3) Uani 1 1 d . . . H25A H 0.2748 0.7080 0.0210 0.164 Uiso 1 1 calc R . . H25B H 0.4035 0.6891 0.0593 0.164 Uiso 1 1 calc R . . C26 C 0.3816(8) 0.8723(8) 0.0222(5) 0.136(3) Uani 1 1 d . . . H26A H 0.4591 0.8518 0.0100 0.163 Uiso 1 1 calc R . . H26B H 0.3232 0.9026 -0.0102 0.163 Uiso 1 1 calc R . . C28 C 0.3144(12) 0.9326(9) 0.1019(5) 0.199(6) Uani 1 1 d . . . H28A H 0.3545 0.9499 0.1403 0.239 Uiso 1 1 calc R . . H28B H 0.2402 0.9881 0.0947 0.239 Uiso 1 1 calc R . . C29 C 0.0603(7) 0.7501(9) 0.2222(3) 0.122(3) Uani 1 1 d . . . H29A H 0.0885 0.6836 0.2520 0.147 Uiso 1 1 calc R . . H29B H -0.0060 0.7089 0.1959 0.147 Uiso 1 1 calc R . . C30 C 0.0215(12) 0.8828(15) 0.2458(4) 0.248(8) Uani 1 1 d . . . H30A H -0.0104 0.8690 0.2807 0.298 Uiso 1 1 calc R . . H30B H -0.0379 0.9331 0.2189 0.298 Uiso 1 1 calc R . . C31 C 0.1719(9) 0.9676(13) 0.2573(5) 0.196(6) Uani 1 1 d . . . H31A H 0.1682 1.0614 0.2420 0.235 Uiso 1 1 calc R . . H31B H 0.2078 0.9698 0.2970 0.235 Uiso 1 1 calc R . . C32 C 0.2285(6) 0.8855(8) 0.2295(4) 0.144(4) Uani 1 1 d . . . H32A H 0.3133 0.8876 0.2314 0.173 Uiso 1 1 calc R . . C33 C 0.3957(15) 0.9689(14) 0.0621(4) 0.255(9) Uani 1 1 d . . . H33A H 0.3747 1.0600 0.0458 0.307 Uiso 1 1 calc R . . H33B H 0.4801 0.9711 0.0811 0.307 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 0.063(5) 0.059(5) 0.095(6) -0.014(4) 0.018(5) -0.008(4) N1 0.036(2) 0.054(2) 0.057(2) -0.0043(18) 0.0071(16) -0.0043(17) O1 0.081(3) 0.057(2) 0.096(3) -0.0013(19) 0.022(2) -0.0144(18) O2 0.076(2) 0.078(3) 0.092(3) -0.027(2) 0.021(2) -0.006(2) C1 0.038(2) 0.047(3) 0.055(3) 0.001(2) 0.005(2) -0.0040(19) C2 0.038(2) 0.053(3) 0.056(3) 0.007(2) 0.003(2) -0.006(2) C3 0.039(3) 0.083(4) 0.066(3) 0.007(3) 0.000(2) -0.005(2) C4 0.038(3) 0.105(4) 0.073(4) 0.002(3) 0.011(2) 0.000(3) C5 0.052(3) 0.086(4) 0.059(3) -0.006(3) 0.015(2) 0.004(3) C6 0.042(3) 0.067(3) 0.058(3) -0.005(2) 0.006(2) -0.004(2) C7 0.045(3) 0.053(3) 0.058(3) 0.005(2) -0.005(2) 0.000(2) C8 0.067(3) 0.068(3) 0.054(3) 0.003(2) 0.003(2) -0.005(3) C9 0.085(4) 0.090(4) 0.065(4) -0.003(3) 0.009(3) 0.003(3) C10 0.108(5) 0.106(5) 0.062(4) -0.012(4) -0.002(4) 0.016(4) C11 0.084(4) 0.084(4) 0.088(5) -0.023(4) -0.018(4) 0.003(3) C12 0.064(3) 0.067(3) 0.078(4) -0.002(3) -0.004(3) -0.005(3) C13 0.041(2) 0.057(3) 0.047(2) -0.005(2) 0.0115(19) -0.006(2) C14 0.037(2) 0.075(3) 0.052(3) -0.012(2) 0.007(2) -0.005(2) C15 0.043(3) 0.091(4) 0.082(4) -0.016(3) 0.015(2) -0.013(3) C16 0.062(4) 0.097(5) 0.093(4) -0.016(3) 0.028(3) -0.036(3) C17 0.087(4) 0.065(3) 0.071(3) -0.006(3) 0.022(3) -0.022(3) C18 0.057(3) 0.059(3) 0.064(3) -0.003(2) 0.010(2) -0.007(2) C19 0.040(3) 0.079(4) 0.055(3) -0.023(3) -0.010(2) 0.010(2) C20 0.066(3) 0.066(3) 0.058(3) -0.003(3) -0.009(3) -0.009(3) C21 0.084(4) 0.079(4) 0.084(4) -0.004(3) -0.018(3) -0.001(3) C22 0.111(6) 0.090(5) 0.091(5) -0.014(4) -0.023(4) 0.009(5) C23 0.081(4) 0.097(5) 0.090(5) -0.033(4) -0.018(4) 0.045(4) C24 0.062(3) 0.108(5) 0.076(4) -0.025(3) 0.000(3) 0.012(3) C25 0.193(8) 0.084(5) 0.161(7) 0.002(5) 0.113(7) -0.022(5) C26 0.131(7) 0.096(6) 0.200(9) 0.027(6) 0.082(7) 0.004(5) C28 0.324(15) 0.102(7) 0.198(10) -0.045(7) 0.123(11) -0.092(8) C29 0.107(5) 0.173(8) 0.093(5) -0.041(5) 0.036(4) -0.044(5) C30 0.279(15) 0.378(19) 0.112(7) 0.061(9) 0.107(9) 0.219(15) C31 0.121(7) 0.251(13) 0.199(11) -0.139(10) -0.021(7) 0.037(8) C32 0.071(4) 0.141(7) 0.223(9) -0.120(7) 0.027(5) -0.014(4) C33 0.42(2) 0.249(14) 0.102(7) -0.016(8) 0.053(9) -0.258(15) _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 O2 1.903(9) . ? Li1 O1 1.920(9) . ? Li1 N1 1.967(9) . ? Li1 C1 2.734(9) . ? Li1 C20 2.756(10) . ? N1 C13 1.369(5) . ? N1 C1 1.385(5) . ? O1 C28 1.366(8) . ? O1 C25 1.416(7) . ? O2 C29 1.377(7) . ? O2 C32 1.429(7) . ? C1 C6 1.410(6) . ? C1 C2 1.414(6) . ? C2 C3 1.386(6) . ? C2 C7 1.487(6) . ? C3 C4 1.367(7) . ? C4 C5 1.380(7) . ? C5 C6 1.368(6) . ? C7 C8 1.386(6) . ? C7 C12 1.387(6) . ? C8 C9 1.377(7) . ? C9 C10 1.372(8) . ? C10 C11 1.355(9) . ? C11 C12 1.395(8) . ? C13 C18 1.408(6) . ? C13 C14 1.423(6) . ? C14 C15 1.384(7) . ? C14 C19 1.501(7) . ? C15 C16 1.366(8) . ? C16 C17 1.387(8) . ? C17 C18 1.384(7) . ? C19 C20 1.390(7) . ? C19 C24 1.400(7) . ? C20 C21 1.378(8) . ? C21 C22 1.336(9) . ? C22 C23 1.359(9) . ? C23 C24 1.413(9) . ? C25 C26 1.441(9) . ? C26 C33 1.350(12) . ? C28 C33 1.484(13) . ? C29 C30 1.515(13) . ? C30 C31 1.869(18) . ? C31 C32 1.287(10) . ? 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 O2 Li1 O1 108.6(4) . . ? O2 Li1 N1 131.1(5) . . ? O1 Li1 N1 118.3(5) . . ? O2 Li1 C1 143.2(5) . . ? O1 Li1 C1 93.6(3) . . ? N1 Li1 C1 28.81(18) . . ? O2 Li1 C20 114.6(4) . . ? O1 Li1 C20 94.4(4) . . ? N1 Li1 C20 75.9(3) . . ? C1 Li1 C20 91.6(3) . . ? C13 N1 C1 118.8(4) . . ? C13 N1 Li1 132.4(4) . . ? C1 N1 Li1 108.0(4) . . ? C28 O1 C25 106.5(6) . . ? C28 O1 Li1 127.6(6) . . ? C25 O1 Li1 125.7(4) . . ? C29 O2 C32 110.0(5) . . ? C29 O2 Li1 119.6(5) . . ? C32 O2 Li1 127.8(5) . . ? N1 C1 C6 120.8(4) . . ? N1 C1 C2 121.0(4) . . ? C6 C1 C2 117.7(4) . . ? N1 C1 Li1 43.2(3) . . ? C6 C1 Li1 131.6(4) . . ? C2 C1 Li1 91.0(3) . . ? C3 C2 C1 118.3(4) . . ? C3 C2 C7 120.1(4) . . ? C1 C2 C7 121.5(4) . . ? C4 C3 C2 122.8(4) . . ? C3 C4 C5 119.3(4) . . ? C6 C5 C4 119.8(5) . . ? C5 C6 C1 121.9(4) . . ? C8 C7 C12 117.4(5) . . ? C8 C7 C2 121.4(4) . . ? C12 C7 C2 121.1(4) . . ? C9 C8 C7 121.2(5) . . ? C10 C9 C8 120.5(6) . . ? C11 C10 C9 119.7(6) . . ? C10 C11 C12 120.2(6) . . ? C7 C12 C11 121.0(5) . . ? N1 C13 C18 122.0(4) . . ? N1 C13 C14 120.8(4) . . ? C18 C13 C14 117.0(4) . . ? C15 C14 C13 118.9(5) . . ? C15 C14 C19 119.6(4) . . ? C13 C14 C19 121.4(4) . . ? C16 C15 C14 123.2(5) . . ? C15 C16 C17 119.0(5) . . ? C18 C17 C16 119.6(5) . . ? C17 C18 C13 122.2(5) . . ? C20 C19 C24 117.7(5) . . ? C20 C19 C14 120.8(4) . . ? C24 C19 C14 121.4(5) . . ? C21 C20 C19 121.0(6) . . ? C21 C20 Li1 106.1(4) . . ? C19 C20 Li1 88.6(3) . . ? C22 C21 C20 120.3(7) . . ? C21 C22 C23 122.1(7) . . ? C22 C23 C24 118.8(6) . . ? C19 C24 C23 120.1(6) . . ? O1 C25 C26 109.0(6) . . ? C33 C26 C25 104.8(8) . . ? O1 C28 C33 107.1(8) . . ? O2 C29 C30 102.6(8) . . ? C29 C30 C31 97.3(6) . . ? C32 C31 C30 99.1(7) . . ? C31 C32 O2 114.2(7) . . ? C26 C33 C28 107.1(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.424 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.052 #===end data_(2-C6H4-Ph)2NAlCl2 _database_code_depnum_ccdc_archive 'CCDC 674915' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C24 H18 Al Cl2 N' _chemical_formula_weight 418.27 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' Cl Cl 0.1484 0.1585 '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 9.854(5) _cell_length_b 10.114(5) _cell_length_c 11.680(6) _cell_angle_alpha 73.971(8) _cell_angle_beta 70.399(8) _cell_angle_gamma 72.274(8) _cell_volume 1024.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 0.369 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.469972 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 296(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 ? _diffrn_reflns_number 9862 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3584 _reflns_number_gt 2308 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0681P)^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 3584 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1334 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Al1 Al 0.26235(11) 0.26874(10) 0.31897(9) 0.0563(3) Uani 1 1 d . . . Cl1 Cl 0.04437(10) 0.31872(10) 0.30639(8) 0.0731(3) Uani 1 1 d . . . Cl2 Cl 0.35195(12) 0.44530(9) 0.27758(9) 0.0798(3) Uani 1 1 d . . . N1 N 0.3981(3) 0.1111(2) 0.2747(2) 0.0500(6) Uani 1 1 d . . . C7 C 0.3826(3) 0.2578(3) 0.0218(3) 0.0491(7) Uani 1 1 d . . . C2 C 0.5236(3) 0.2058(3) 0.0589(3) 0.0464(7) Uani 1 1 d . . . C19 C 0.2072(3) 0.0731(3) 0.5270(3) 0.0487(7) Uani 1 1 d . . . C13 C 0.3933(3) -0.0270(3) 0.3438(3) 0.0474(7) Uani 1 1 d . . . C1 C 0.5312(3) 0.1298(3) 0.1769(3) 0.0467(7) Uani 1 1 d . . . C14 C 0.3021(3) -0.0473(3) 0.4659(3) 0.0464(7) Uani 1 1 d . . . C15 C 0.2967(4) -0.1853(3) 0.5297(3) 0.0593(9) Uani 1 1 d . . . H15A H 0.2355 -0.1992 0.6102 0.071 Uiso 1 1 calc R . . C20 C 0.2619(4) 0.1884(3) 0.5229(3) 0.0549(8) Uani 1 1 d . . . H20A H 0.3604 0.1897 0.4815 0.066 Uiso 1 1 calc R . . C18 C 0.4746(4) -0.1454(3) 0.2920(3) 0.0560(8) Uani 1 1 d . . . H18A H 0.5354 -0.1334 0.2113 0.067 Uiso 1 1 calc R . . C24 C 0.0591(4) 0.0766(4) 0.5923(3) 0.0597(9) Uani 1 1 d . . . H24A H 0.0200 0.0013 0.5983 0.072 Uiso 1 1 calc R . . C3 C 0.6542(3) 0.2318(3) -0.0272(3) 0.0557(8) Uani 1 1 d . . . H3A H 0.6505 0.2836 -0.1058 0.067 Uiso 1 1 calc R . . C16 C 0.3788(4) -0.3010(3) 0.4774(3) 0.0678(10) Uani 1 1 d . . . H16A H 0.3746 -0.3919 0.5223 0.081 Uiso 1 1 calc R . . C23 C -0.0294(4) 0.1871(4) 0.6473(3) 0.0730(10) Uani 1 1 d . . . H23A H -0.1278 0.1864 0.6897 0.088 Uiso 1 1 calc R . . C12 C 0.3419(4) 0.3983(4) -0.0359(3) 0.0634(9) Uani 1 1 d . . . H12A H 0.3979 0.4612 -0.0439 0.076 Uiso 1 1 calc R . . C17 C 0.4673(4) -0.2806(3) 0.3579(3) 0.0655(9) Uani 1 1 d . . . H17A H 0.5225 -0.3582 0.3212 0.079 Uiso 1 1 calc R . . C8 C 0.2956(4) 0.1676(4) 0.0339(3) 0.0599(9) Uani 1 1 d . . . H8A H 0.3198 0.0736 0.0731 0.072 Uiso 1 1 calc R . . C6 C 0.6667(4) 0.0825(3) 0.2031(3) 0.0601(9) Uani 1 1 d . . . H6A H 0.6714 0.0314 0.2817 0.072 Uiso 1 1 calc R . . C4 C 0.7880(4) 0.1840(4) -0.0008(3) 0.0659(9) Uani 1 1 d . . . H4A H 0.8737 0.2020 -0.0609 0.079 Uiso 1 1 calc R . . C5 C 0.7940(4) 0.1086(4) 0.1167(3) 0.0671(9) Uani 1 1 d . . . H5A H 0.8839 0.0760 0.1367 0.080 Uiso 1 1 calc R . . C21 C 0.1690(5) 0.3012(4) 0.5809(3) 0.0697(10) Uani 1 1 d . . . H21A H 0.2061 0.3766 0.5780 0.084 Uiso 1 1 calc R . . C9 C 0.1734(4) 0.2154(5) -0.0116(4) 0.0748(11) Uani 1 1 d . . . H9A H 0.1160 0.1535 -0.0030 0.090 Uiso 1 1 calc R . . C10 C 0.1358(4) 0.3539(5) -0.0694(4) 0.0848(12) Uani 1 1 d . . . H10A H 0.0537 0.3856 -0.1006 0.102 Uiso 1 1 calc R . . C22 C 0.0255(5) 0.3004(4) 0.6407(3) 0.0766(11) Uani 1 1 d . . . H22A H -0.0363 0.3761 0.6776 0.092 Uiso 1 1 calc R . . C11 C 0.2196(5) 0.4452(4) -0.0810(3) 0.0795(11) Uani 1 1 d . . . H11A H 0.1939 0.5392 -0.1195 0.095 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 0.0570(6) 0.0447(5) 0.0581(6) -0.0039(4) -0.0100(5) -0.0110(5) Cl1 0.0584(6) 0.0768(6) 0.0718(6) -0.0049(5) -0.0188(5) -0.0058(5) Cl2 0.0938(7) 0.0526(5) 0.0857(7) -0.0074(5) -0.0089(6) -0.0299(5) N1 0.0520(15) 0.0461(15) 0.0436(14) -0.0050(11) -0.0064(12) -0.0106(12) C7 0.0491(18) 0.0568(19) 0.0387(16) -0.0110(14) -0.0054(14) -0.0144(16) C2 0.0478(18) 0.0434(16) 0.0441(16) -0.0071(13) -0.0084(14) -0.0112(14) C19 0.0546(19) 0.0491(18) 0.0371(15) -0.0034(13) -0.0125(14) -0.0091(15) C13 0.0527(19) 0.0434(17) 0.0441(17) -0.0045(14) -0.0136(15) -0.0120(14) C1 0.0483(18) 0.0428(17) 0.0449(17) -0.0076(13) -0.0086(14) -0.0105(14) C14 0.0508(18) 0.0437(17) 0.0439(16) -0.0057(13) -0.0128(14) -0.0129(14) C15 0.066(2) 0.054(2) 0.0502(18) -0.0034(16) -0.0058(16) -0.0202(17) C20 0.062(2) 0.0538(19) 0.0454(17) -0.0076(15) -0.0137(15) -0.0113(16) C18 0.060(2) 0.053(2) 0.0504(18) -0.0133(16) -0.0080(16) -0.0122(16) C24 0.062(2) 0.065(2) 0.0475(18) -0.0101(17) -0.0099(17) -0.0159(18) C3 0.055(2) 0.0569(19) 0.0487(18) 0.0017(15) -0.0118(16) -0.0180(16) C16 0.080(3) 0.045(2) 0.070(2) -0.0051(17) -0.012(2) -0.0172(18) C23 0.060(2) 0.093(3) 0.053(2) -0.020(2) -0.0042(18) -0.007(2) C12 0.062(2) 0.059(2) 0.064(2) -0.0022(17) -0.0181(18) -0.0139(18) C17 0.066(2) 0.049(2) 0.077(2) -0.0202(18) -0.015(2) -0.0053(17) C8 0.056(2) 0.064(2) 0.060(2) -0.0188(17) -0.0117(17) -0.0137(17) C6 0.066(2) 0.062(2) 0.0482(18) 0.0031(15) -0.0201(17) -0.0166(18) C4 0.049(2) 0.080(2) 0.060(2) -0.0026(18) -0.0055(17) -0.0239(18) C5 0.048(2) 0.080(2) 0.069(2) -0.0041(19) -0.0177(18) -0.0178(18) C21 0.089(3) 0.056(2) 0.065(2) -0.0196(18) -0.024(2) -0.009(2) C9 0.060(2) 0.093(3) 0.080(3) -0.035(2) -0.010(2) -0.026(2) C10 0.062(3) 0.116(4) 0.082(3) -0.031(3) -0.030(2) -0.006(3) C22 0.083(3) 0.067(3) 0.067(2) -0.029(2) -0.014(2) 0.008(2) C11 0.076(3) 0.074(3) 0.077(3) -0.007(2) -0.028(2) 0.000(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 N1 1.814(3) . ? Al1 Cl2 2.0973(16) . ? Al1 Cl1 2.0976(17) . ? Al1 C20 2.294(3) . ? N1 C13 1.413(4) . ? N1 C1 1.444(4) . ? C7 C8 1.382(4) . ? C7 C12 1.393(4) . ? C7 C2 1.492(4) . ? C2 C3 1.388(4) . ? C2 C1 1.395(4) . ? C19 C24 1.396(4) . ? C19 C20 1.410(4) . ? C19 C14 1.485(4) . ? C13 C18 1.390(4) . ? C13 C14 1.405(4) . ? C1 C6 1.381(4) . ? C14 C15 1.396(4) . ? C15 C16 1.373(4) . ? C20 C21 1.405(4) . ? C18 C17 1.382(4) . ? C24 C23 1.360(5) . ? C3 C4 1.367(4) . ? C16 C17 1.372(5) . ? C23 C22 1.383(5) . ? C12 C11 1.376(5) . ? C8 C9 1.377(5) . ? C6 C5 1.366(4) . ? C4 C5 1.385(5) . ? C21 C22 1.352(5) . ? C9 C10 1.373(6) . ? C10 C11 1.369(5) . ? 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 N1 Al1 Cl2 113.70(10) . . ? N1 Al1 Cl1 122.70(10) . . ? Cl2 Al1 Cl1 114.00(6) . . ? N1 Al1 C20 91.83(11) . . ? Cl2 Al1 C20 100.04(10) . . ? Cl1 Al1 C20 109.07(10) . . ? C13 N1 C1 117.8(2) . . ? C13 N1 Al1 123.52(19) . . ? C1 N1 Al1 117.76(18) . . ? C8 C7 C12 118.1(3) . . ? C8 C7 C2 121.8(3) . . ? C12 C7 C2 119.9(3) . . ? C3 C2 C1 117.8(3) . . ? C3 C2 C7 119.3(3) . . ? C1 C2 C7 122.9(3) . . ? C24 C19 C20 116.8(3) . . ? C24 C19 C14 121.2(3) . . ? C20 C19 C14 121.9(3) . . ? C18 C13 C14 118.5(3) . . ? C18 C13 N1 121.2(3) . . ? C14 C13 N1 120.3(3) . . ? C6 C1 C2 119.3(3) . . ? C6 C1 N1 119.7(3) . . ? C2 C1 N1 120.8(3) . . ? C15 C14 C13 118.6(3) . . ? C15 C14 C19 119.2(3) . . ? C13 C14 C19 122.1(3) . . ? C16 C15 C14 122.1(3) . . ? C21 C20 C19 120.5(3) . . ? C21 C20 Al1 104.0(2) . . ? C19 C20 Al1 89.82(18) . . ? C17 C18 C13 121.5(3) . . ? C23 C24 C19 121.8(3) . . ? C4 C3 C2 122.5(3) . . ? C17 C16 C15 119.1(3) . . ? C24 C23 C22 120.6(4) . . ? C11 C12 C7 120.8(3) . . ? C16 C17 C18 120.3(3) . . ? C9 C8 C7 120.7(3) . . ? C5 C6 C1 121.9(3) . . ? C3 C4 C5 119.1(3) . . ? C6 C5 C4 119.3(3) . . ? C22 C21 C20 120.1(4) . . ? C10 C9 C8 120.4(4) . . ? C11 C10 C9 119.7(4) . . ? C21 C22 C23 120.1(3) . . ? C10 C11 C12 120.2(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.279 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.053 #===end data_(2-C6H4-Ph)2NAlMe2 _database_code_depnum_ccdc_archive 'CCDC 674916' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C26 H24 Al N' _chemical_formula_weight 377.44 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.958(9) _cell_length_b 10.240(9) _cell_length_c 11.867(10) _cell_angle_alpha 74.860(14) _cell_angle_beta 70.517(14) _cell_angle_gamma 71.186(13) _cell_volume 1063.8(16) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 0.106 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.489378 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 10243 _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_av_sigmaI/netI 0.1151 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3720 _reflns_number_gt 1711 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0539P)^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_number_reflns 3720 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1511 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1112 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _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 Al1 Al 0.24023(12) 0.72458(12) 0.20087(11) 0.0627(4) Uani 1 1 d . . . N1 N 0.0989(3) 0.8899(3) 0.2291(2) 0.0459(7) Uani 1 1 d . . . C1 C -0.0335(4) 0.8756(3) 0.3216(3) 0.0458(9) Uani 1 1 d . . . C6 C -0.1693(4) 0.9259(4) 0.2956(3) 0.0571(10) Uani 1 1 d . . . H6A H -0.1745 0.9778 0.2194 0.069 Uiso 1 1 calc R . . C5 C -0.2963(4) 0.9007(4) 0.3797(4) 0.0657(11) Uani 1 1 d . . . H5A H -0.3854 0.9344 0.3595 0.079 Uiso 1 1 calc R . . C4 C -0.2916(4) 0.8257(4) 0.4939(4) 0.0642(11) Uani 1 1 d . . . H4A H -0.3770 0.8086 0.5512 0.077 Uiso 1 1 calc R . . C3 C -0.1581(4) 0.7764(3) 0.5214(3) 0.0542(10) Uani 1 1 d . . . H3A H -0.1545 0.7248 0.5980 0.065 Uiso 1 1 calc R . . C2 C -0.0286(4) 0.8013(3) 0.4381(3) 0.0437(9) Uani 1 1 d . . . C7 C 0.1121(4) 0.7479(4) 0.4746(3) 0.0462(9) Uani 1 1 d . . . C8 C 0.1975(4) 0.8373(4) 0.4621(3) 0.0573(10) Uani 1 1 d . . . H8A H 0.1721 0.9298 0.4239 0.069 Uiso 1 1 calc R . . C9 C 0.3204(5) 0.7891(5) 0.5064(4) 0.0715(12) Uani 1 1 d . . . H9A H 0.3769 0.8496 0.4981 0.086 Uiso 1 1 calc R . . C10 C 0.3592(5) 0.6527(6) 0.5626(4) 0.0832(14) Uani 1 1 d . . . H10A H 0.4415 0.6211 0.5924 0.100 Uiso 1 1 calc R . . C11 C 0.2768(5) 0.5629(5) 0.5748(4) 0.0781(13) Uani 1 1 d . . . H11A H 0.3037 0.4702 0.6122 0.094 Uiso 1 1 calc R . . C12 C 0.1532(4) 0.6104(4) 0.5313(3) 0.0621(11) Uani 1 1 d . . . H12A H 0.0973 0.5492 0.5402 0.074 Uiso 1 1 calc R . . C13 C 0.1050(3) 1.0242(3) 0.1610(3) 0.0437(9) Uani 1 1 d . . . C18 C 0.0262(4) 1.1453(4) 0.2109(3) 0.0544(10) Uani 1 1 d . . . H18A H -0.0359 1.1371 0.2894 0.065 Uiso 1 1 calc R . . C17 C 0.0374(4) 1.2769(4) 0.1474(4) 0.0627(11) Uani 1 1 d . . . H17A H -0.0147 1.3555 0.1837 0.075 Uiso 1 1 calc R . . C16 C 0.1267(4) 1.2914(4) 0.0290(4) 0.0647(11) Uani 1 1 d . . . H16A H 0.1334 1.3796 -0.0153 0.078 Uiso 1 1 calc R . . C15 C 0.2052(4) 1.1731(4) -0.0218(3) 0.0568(10) Uani 1 1 d . . . H15A H 0.2659 1.1831 -0.1007 0.068 Uiso 1 1 calc R . . C14 C 0.1970(4) 1.0387(3) 0.0409(3) 0.0450(9) Uani 1 1 d . . . C19 C 0.2856(4) 0.9168(3) -0.0207(3) 0.0446(9) Uani 1 1 d . . . C20 C 0.4336(4) 0.9057(4) -0.0841(3) 0.0578(10) Uani 1 1 d . . . H20A H 0.4766 0.9748 -0.0861 0.069 Uiso 1 1 calc R . . C21 C 0.5178(5) 0.7947(5) -0.1439(3) 0.0729(12) Uani 1 1 d . . . H21A H 0.6166 0.7891 -0.1845 0.088 Uiso 1 1 calc R . . C22 C 0.4555(5) 0.6921(5) -0.1434(4) 0.0823(14) Uani 1 1 d . . . H22A H 0.5120 0.6173 -0.1836 0.099 Uiso 1 1 calc R . . C23 C 0.3102(5) 0.7008(4) -0.0835(4) 0.0721(12) Uani 1 1 d . . . H23A H 0.2682 0.6319 -0.0836 0.087 Uiso 1 1 calc R . . C24 C 0.2243(4) 0.8120(4) -0.0222(3) 0.0551(10) Uani 1 1 d . . . H24A H 0.1256 0.8166 0.0180 0.066 Uiso 1 1 calc R . . C25 C 0.1577(5) 0.5666(4) 0.2275(4) 0.0884(14) Uani 1 1 d . . . H25A H 0.0565 0.6009 0.2258 0.133 Uiso 1 1 calc R . . H25D H 0.1636 0.5098 0.3050 0.133 Uiso 1 1 calc R . . H25B H 0.2126 0.5114 0.1647 0.133 Uiso 1 1 calc R . . C26 C 0.4431(4) 0.7013(4) 0.1973(3) 0.0720(12) Uani 1 1 d . . . H26D H 0.4611 0.7917 0.1831 0.108 Uiso 1 1 calc R . . H26A H 0.5087 0.6512 0.1334 0.108 Uiso 1 1 calc R . . H26B H 0.4597 0.6496 0.2737 0.108 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 0.0551(8) 0.0486(7) 0.0718(9) -0.0040(6) -0.0055(6) -0.0143(6) N1 0.0421(17) 0.0425(18) 0.0428(17) -0.0023(14) -0.0024(14) -0.0109(14) C1 0.043(2) 0.044(2) 0.047(2) -0.0036(18) -0.0085(19) -0.0137(18) C6 0.053(2) 0.060(3) 0.053(2) 0.004(2) -0.018(2) -0.013(2) C5 0.045(2) 0.080(3) 0.069(3) -0.002(2) -0.019(2) -0.017(2) C4 0.044(2) 0.071(3) 0.069(3) 0.000(2) -0.006(2) -0.022(2) C3 0.054(2) 0.054(2) 0.049(2) 0.0028(18) -0.009(2) -0.020(2) C2 0.041(2) 0.044(2) 0.041(2) -0.0059(17) -0.0046(18) -0.0136(18) C7 0.042(2) 0.048(2) 0.044(2) -0.0078(18) -0.0060(18) -0.0123(19) C8 0.054(2) 0.062(3) 0.054(2) -0.016(2) -0.010(2) -0.013(2) C9 0.060(3) 0.088(4) 0.077(3) -0.030(3) -0.016(2) -0.025(3) C10 0.062(3) 0.115(4) 0.076(3) -0.028(3) -0.033(3) -0.006(3) C11 0.070(3) 0.074(3) 0.078(3) -0.003(2) -0.029(3) -0.001(3) C12 0.059(3) 0.062(3) 0.062(3) -0.001(2) -0.021(2) -0.014(2) C13 0.042(2) 0.042(2) 0.046(2) -0.0015(18) -0.0124(18) -0.0135(18) C18 0.052(2) 0.049(2) 0.052(2) -0.013(2) -0.0003(19) -0.011(2) C17 0.063(3) 0.047(2) 0.075(3) -0.020(2) -0.010(2) -0.011(2) C16 0.073(3) 0.043(2) 0.074(3) -0.003(2) -0.014(2) -0.021(2) C15 0.056(2) 0.057(3) 0.053(2) -0.005(2) -0.005(2) -0.023(2) C14 0.046(2) 0.047(2) 0.042(2) -0.0067(18) -0.0080(18) -0.0169(18) C19 0.044(2) 0.049(2) 0.038(2) -0.0055(17) -0.0092(18) -0.0117(19) C20 0.055(3) 0.067(3) 0.049(2) -0.013(2) -0.008(2) -0.016(2) C21 0.056(3) 0.093(3) 0.060(3) -0.029(3) -0.002(2) -0.007(3) C22 0.081(3) 0.081(3) 0.077(3) -0.041(3) -0.017(3) 0.007(3) C23 0.082(3) 0.060(3) 0.078(3) -0.026(2) -0.024(3) -0.012(3) C24 0.057(2) 0.058(3) 0.052(2) -0.008(2) -0.016(2) -0.017(2) C25 0.099(3) 0.060(3) 0.094(3) -0.016(2) 0.000(3) -0.030(3) C26 0.056(2) 0.074(3) 0.070(3) -0.001(2) -0.013(2) -0.009(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 N1 1.845(3) . ? Al1 C26 1.944(4) . ? Al1 C25 1.952(4) . ? N1 C13 1.411(4) . ? N1 C1 1.428(4) . ? C1 C6 1.391(4) . ? C1 C2 1.402(4) . ? C6 C5 1.377(4) . ? C5 C4 1.380(5) . ? C4 C3 1.379(5) . ? C3 C2 1.392(4) . ? C2 C7 1.495(5) . ? C7 C12 1.385(4) . ? C7 C8 1.390(4) . ? C8 C9 1.387(5) . ? C9 C10 1.372(5) . ? C10 C11 1.369(5) . ? C11 C12 1.388(5) . ? C13 C18 1.397(4) . ? C13 C14 1.413(4) . ? C18 C17 1.381(5) . ? C17 C16 1.389(5) . ? C16 C15 1.378(5) . ? C15 C14 1.397(4) . ? C14 C19 1.486(4) . ? C19 C20 1.396(4) . ? C19 C24 1.402(4) . ? C20 C21 1.382(5) . ? C21 C22 1.380(5) . ? C22 C23 1.368(5) . ? C23 C24 1.395(5) . ? 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 N1 Al1 C26 120.93(16) . . ? N1 Al1 C25 113.45(17) . . ? C26 Al1 C25 122.83(18) . . ? C13 N1 C1 118.3(3) . . ? C13 N1 Al1 126.0(2) . . ? C1 N1 Al1 115.4(2) . . ? C6 C1 C2 118.3(3) . . ? C6 C1 N1 120.7(3) . . ? C2 C1 N1 120.8(3) . . ? C5 C6 C1 121.7(3) . . ? C6 C5 C4 120.1(3) . . ? C3 C4 C5 118.8(3) . . ? C4 C3 C2 122.0(3) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C7 119.4(3) . . ? C1 C2 C7 121.7(3) . . ? C12 C7 C8 118.5(3) . . ? C12 C7 C2 120.3(3) . . ? C8 C7 C2 120.9(3) . . ? C9 C8 C7 120.3(4) . . ? C10 C9 C8 120.3(4) . . ? C11 C10 C9 120.1(4) . . ? C10 C11 C12 119.9(4) . . ? C7 C12 C11 120.8(4) . . ? C18 C13 N1 121.5(3) . . ? C18 C13 C14 118.3(3) . . ? N1 C13 C14 120.2(3) . . ? C17 C18 C13 122.1(3) . . ? C18 C17 C16 119.7(3) . . ? C15 C16 C17 119.0(3) . . ? C16 C15 C14 122.4(3) . . ? C15 C14 C13 118.5(3) . . ? C15 C14 C19 118.9(3) . . ? C13 C14 C19 122.6(3) . . ? C20 C19 C24 117.3(3) . . ? C20 C19 C14 120.5(3) . . ? C24 C19 C14 122.2(3) . . ? C21 C20 C19 121.7(4) . . ? C22 C21 C20 120.0(4) . . ? C23 C22 C21 119.7(4) . . ? C22 C23 C24 120.7(4) . . ? C23 C24 C19 120.5(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.153 _refine_diff_density_min -0.196 _refine_diff_density_rms 0.038 #===end data_(2-C6H4-Ph)2NAlEt2 _database_code_depnum_ccdc_archive 'CCDC 674917' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C28 H28 Al N' _chemical_formula_weight 405.49 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.838(3) _cell_length_b 11.125(3) _cell_length_c 11.994(4) _cell_angle_alpha 77.709(5) _cell_angle_beta 69.532(5) _cell_angle_gamma 72.918(5) _cell_volume 1166.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 297(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.655032 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 11279 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0910 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4097 _reflns_number_gt 1904 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0664P)^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_number_reflns 4097 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1463 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1581 _refine_ls_wR_factor_gt 0.1221 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 Al1 Al 0.74763(12) 0.23436(10) 0.18553(10) 0.0718(4) Uani 1 1 d . . . N1 N 0.5998(3) 0.3760(2) 0.2272(2) 0.0542(7) Uani 1 1 d . . . C7 C 0.7806(3) 0.4239(3) -0.0233(3) 0.0520(8) Uani 1 1 d . . . C2 C 0.6948(3) 0.5252(3) 0.0543(3) 0.0517(8) Uani 1 1 d . . . C1 C 0.6071(3) 0.5010(3) 0.1736(3) 0.0526(8) Uani 1 1 d . . . C14 C 0.4679(3) 0.2913(3) 0.4286(3) 0.0577(9) Uani 1 1 d . . . C6 C 0.5311(4) 0.6032(3) 0.2393(3) 0.0690(10) Uani 1 1 d . . . H6A H 0.4721 0.5889 0.3183 0.083 Uiso 1 1 calc R . . C13 C 0.4645(3) 0.3621(3) 0.3183(3) 0.0542(8) Uani 1 1 d . . . C12 C 0.9268(4) 0.4208(3) -0.0931(3) 0.0644(9) Uani 1 1 d . . . H12A H 0.9709 0.4825 -0.0890 0.077 Uiso 1 1 calc R . . C8 C 0.7172(4) 0.3309(3) -0.0334(3) 0.0610(9) Uani 1 1 d . . . H8A H 0.6185 0.3310 0.0108 0.073 Uiso 1 1 calc R . . C3 C 0.7038(4) 0.6493(3) 0.0076(3) 0.0664(10) Uani 1 1 d . . . H3A H 0.7626 0.6655 -0.0711 0.080 Uiso 1 1 calc R . . C19 C 0.6061(4) 0.2442(4) 0.4639(3) 0.0595(9) Uani 1 1 d . . . C18 C 0.3280(4) 0.4103(3) 0.2959(3) 0.0692(10) Uani 1 1 d . . . H18A H 0.3249 0.4582 0.2228 0.083 Uiso 1 1 calc R . . C4 C 0.6286(4) 0.7487(3) 0.0741(4) 0.0769(11) Uani 1 1 d . . . H4A H 0.6364 0.8309 0.0411 0.092 Uiso 1 1 calc R . . C15 C 0.3344(4) 0.2698(4) 0.5104(3) 0.0777(11) Uani 1 1 d . . . H15A H 0.3360 0.2214 0.5836 0.093 Uiso 1 1 calc R . . C20 C 0.6921(4) 0.3253(4) 0.4597(3) 0.0723(10) Uani 1 1 d . . . H20A H 0.6676 0.4094 0.4270 0.087 Uiso 1 1 calc R . . C9 C 0.8004(5) 0.2384(3) -0.1089(3) 0.0779(11) Uani 1 1 d . . . H9A H 0.7572 0.1770 -0.1149 0.093 Uiso 1 1 calc R . . C5 C 0.5417(4) 0.7243(4) 0.1900(4) 0.0792(11) Uani 1 1 d . . . H5A H 0.4893 0.7909 0.2357 0.095 Uiso 1 1 calc R . . C10 C 0.9463(5) 0.2376(4) -0.1747(3) 0.0855(12) Uani 1 1 d . . . H10A H 1.0026 0.1744 -0.2237 0.103 Uiso 1 1 calc R . . C24 C 0.6489(4) 0.1188(4) 0.5113(3) 0.0755(11) Uani 1 1 d . . . H24A H 0.5949 0.0615 0.5144 0.091 Uiso 1 1 calc R . . C17 C 0.1978(4) 0.3888(4) 0.3792(4) 0.0836(12) Uani 1 1 d . . . H17A H 0.1075 0.4226 0.3627 0.100 Uiso 1 1 calc R . . C16 C 0.2010(4) 0.3171(4) 0.4873(3) 0.0894(13) Uani 1 1 d . . . H16A H 0.1134 0.3011 0.5440 0.107 Uiso 1 1 calc R . . C11 C 1.0093(4) 0.3303(4) -0.1682(3) 0.0791(11) Uani 1 1 d . . . H11A H 1.1071 0.3315 -0.2144 0.095 Uiso 1 1 calc R . . C21 C 0.8121(4) 0.2842(5) 0.5029(4) 0.0889(13) Uani 1 1 d . . . H21A H 0.8672 0.3404 0.5002 0.107 Uiso 1 1 calc R . . C23 C 0.7704(5) 0.0782(4) 0.5538(3) 0.0928(13) Uani 1 1 d . . . H23A H 0.7974 -0.0060 0.5854 0.111 Uiso 1 1 calc R . . C22 C 0.8509(5) 0.1602(6) 0.5499(4) 0.0998(15) Uani 1 1 d . . . H22A H 0.9323 0.1322 0.5792 0.120 Uiso 1 1 calc R . . C25 C 0.9513(4) 0.2295(4) 0.1707(3) 0.0865(12) Uani 1 1 d . . . H25A H 0.9962 0.2663 0.0898 0.104 Uiso 1 1 calc R . . H25B H 0.9470 0.2854 0.2245 0.104 Uiso 1 1 calc R . . C27 C 0.6855(5) 0.0800(3) 0.1985(3) 0.0899(12) Uani 1 1 d . . . H27A H 0.7590 0.0310 0.1363 0.108 Uiso 1 1 calc R . . H27B H 0.6911 0.0313 0.2747 0.108 Uiso 1 1 calc R . . C28 C 0.5335(6) 0.0888(4) 0.1899(4) 0.1272(17) Uani 1 1 d . . . H28A H 0.5198 0.0050 0.1982 0.191 Uiso 1 1 calc R . . H28B H 0.5263 0.1331 0.1135 0.191 Uiso 1 1 calc R . . H28C H 0.4578 0.1338 0.2527 0.191 Uiso 1 1 calc R . . C26 C 1.0515(5) 0.1122(5) 0.1930(6) 0.194(3) Uani 1 1 d . . . H26A H 1.1472 0.1266 0.1817 0.292 Uiso 1 1 calc R . . H26B H 1.0620 0.0557 0.1385 0.292 Uiso 1 1 calc R . . H26C H 1.0127 0.0750 0.2740 0.292 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 0.0623(7) 0.0582(7) 0.0795(8) -0.0035(6) -0.0071(6) -0.0131(6) N1 0.0518(16) 0.0515(17) 0.0494(16) -0.0014(13) -0.0014(13) -0.0186(13) C7 0.050(2) 0.057(2) 0.0444(19) -0.0039(16) -0.0099(17) -0.0149(17) C2 0.052(2) 0.053(2) 0.049(2) -0.0057(17) -0.0100(16) -0.0184(17) C1 0.0468(19) 0.056(2) 0.052(2) -0.0076(18) -0.0071(16) -0.0159(17) C14 0.050(2) 0.074(2) 0.048(2) -0.0034(18) -0.0107(18) -0.0210(18) C6 0.070(2) 0.063(2) 0.062(2) -0.015(2) -0.0025(19) -0.016(2) C13 0.047(2) 0.061(2) 0.049(2) -0.0056(17) -0.0067(17) -0.0166(17) C12 0.061(2) 0.077(3) 0.050(2) -0.0113(19) -0.0069(19) -0.020(2) C8 0.060(2) 0.063(2) 0.054(2) -0.0067(18) -0.0101(18) -0.0163(19) C3 0.066(2) 0.065(3) 0.062(2) -0.001(2) -0.0093(19) -0.024(2) C19 0.050(2) 0.081(3) 0.045(2) -0.0074(18) -0.0073(17) -0.020(2) C18 0.059(2) 0.083(3) 0.060(2) 0.0051(19) -0.017(2) -0.019(2) C4 0.084(3) 0.055(2) 0.084(3) -0.005(2) -0.009(2) -0.028(2) C15 0.059(2) 0.115(3) 0.054(2) 0.015(2) -0.013(2) -0.036(2) C20 0.056(2) 0.097(3) 0.063(2) -0.017(2) -0.012(2) -0.022(2) C9 0.094(3) 0.065(3) 0.072(3) -0.020(2) -0.019(2) -0.016(2) C5 0.080(3) 0.061(3) 0.088(3) -0.024(2) -0.008(2) -0.015(2) C10 0.088(3) 0.082(3) 0.067(3) -0.029(2) -0.006(2) -0.001(2) C24 0.072(3) 0.092(3) 0.062(2) -0.001(2) -0.024(2) -0.022(2) C17 0.054(2) 0.116(3) 0.076(3) 0.006(2) -0.022(2) -0.026(2) C16 0.053(2) 0.139(4) 0.069(3) 0.013(3) -0.011(2) -0.040(2) C11 0.068(3) 0.094(3) 0.060(2) -0.012(2) -0.002(2) -0.017(2) C21 0.063(3) 0.136(4) 0.080(3) -0.031(3) -0.018(2) -0.034(3) C23 0.082(3) 0.106(4) 0.081(3) -0.002(2) -0.033(3) -0.006(3) C22 0.064(3) 0.150(5) 0.084(3) -0.022(3) -0.030(2) -0.011(3) C25 0.065(2) 0.085(3) 0.089(3) -0.004(2) -0.016(2) -0.001(2) C27 0.112(4) 0.066(3) 0.082(3) -0.007(2) -0.018(3) -0.023(2) C28 0.142(4) 0.088(3) 0.157(5) -0.008(3) -0.032(4) -0.057(3) C26 0.098(4) 0.111(4) 0.333(9) 0.059(5) -0.079(5) -0.011(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 Al1 N1 1.824(3) . ? Al1 C25 1.934(4) . ? Al1 C27 1.945(4) . ? N1 C1 1.414(4) . ? N1 C13 1.421(4) . ? C7 C12 1.384(4) . ? C7 C8 1.399(4) . ? C7 C2 1.479(4) . ? C2 C3 1.391(4) . ? C2 C1 1.405(4) . ? C1 C6 1.394(4) . ? C14 C15 1.388(4) . ? C14 C13 1.394(4) . ? C14 C19 1.481(4) . ? C6 C5 1.369(4) . ? C13 C18 1.389(4) . ? C12 C11 1.370(4) . ? C8 C9 1.390(4) . ? C3 C4 1.374(4) . ? C19 C24 1.390(4) . ? C19 C20 1.390(5) . ? C18 C17 1.371(4) . ? C4 C5 1.372(5) . ? C15 C16 1.365(4) . ? C20 C21 1.371(5) . ? C9 C10 1.374(5) . ? C10 C11 1.378(5) . ? C24 C23 1.380(5) . ? C17 C16 1.375(5) . ? C21 C22 1.370(6) . ? C23 C22 1.357(6) . ? C25 C26 1.424(5) . ? C27 C28 1.507(5) . ? 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 N1 Al1 C25 119.98(15) . . ? N1 Al1 C27 116.88(16) . . ? C25 Al1 C27 121.23(18) . . ? C1 N1 C13 116.2(2) . . ? C1 N1 Al1 124.9(2) . . ? C13 N1 Al1 118.8(2) . . ? C12 C7 C8 117.2(3) . . ? C12 C7 C2 120.5(3) . . ? C8 C7 C2 122.2(3) . . ? C3 C2 C1 118.8(3) . . ? C3 C2 C7 118.4(3) . . ? C1 C2 C7 122.8(3) . . ? C6 C1 C2 118.3(3) . . ? C6 C1 N1 120.7(3) . . ? C2 C1 N1 121.0(3) . . ? C15 C14 C13 118.3(3) . . ? C15 C14 C19 119.0(3) . . ? C13 C14 C19 122.7(3) . . ? C5 C6 C1 121.3(3) . . ? C18 C13 C14 118.8(3) . . ? C18 C13 N1 120.7(3) . . ? C14 C13 N1 120.3(3) . . ? C11 C12 C7 122.4(3) . . ? C9 C8 C7 120.7(3) . . ? C4 C3 C2 122.1(3) . . ? C24 C19 C20 117.2(3) . . ? C24 C19 C14 121.2(3) . . ? C20 C19 C14 121.4(3) . . ? C17 C18 C13 121.5(3) . . ? C5 C4 C3 118.7(3) . . ? C16 C15 C14 122.5(3) . . ? C21 C20 C19 121.5(4) . . ? C10 C9 C8 120.1(4) . . ? C6 C5 C4 120.9(3) . . ? C9 C10 C11 120.0(4) . . ? C23 C24 C19 120.8(4) . . ? C18 C17 C16 119.8(3) . . ? C15 C16 C17 119.1(3) . . ? C12 C11 C10 119.6(4) . . ? C22 C21 C20 120.0(4) . . ? C22 C23 C24 120.6(4) . . ? C23 C22 C21 119.9(4) . . ? C26 C25 Al1 120.2(3) . . ? C28 C27 Al1 119.6(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.250 _refine_diff_density_min -0.151 _refine_diff_density_rms 0.034 #===end data_(2-C6H4-Ph)2NAlMe2(THF) _database_code_depnum_ccdc_archive 'CCDC 674918' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C30 H32 Al N O' _chemical_formula_weight 449.55 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 8.6605(15) _cell_length_b 30.207(5) _cell_length_c 10.2180(18) _cell_angle_alpha 90.00 _cell_angle_beta 103.730(3) _cell_angle_gamma 90.00 _cell_volume 2596.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.481298 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 24804 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4561 _reflns_number_gt 2847 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0871P)^2^+0.2828P] 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_number_reflns 4561 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1666 _refine_ls_wR_factor_gt 0.1411 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Al1 Al 0.71790(10) 0.06732(3) 0.16700(9) 0.0649(3) Uani 1 1 d . . . N1 N 0.8277(3) 0.11222(6) 0.2739(2) 0.0574(5) Uani 1 1 d . . . O1 O 0.5308(2) 0.09424(6) 0.05522(18) 0.0724(5) Uani 1 1 d . . . C15 C 0.8468(3) 0.11486(9) 0.4163(3) 0.0574(7) Uani 1 1 d . . . C16 C 0.8265(3) 0.15432(9) 0.4823(3) 0.0574(7) Uani 1 1 d . . . C21 C 0.7799(3) 0.19681(9) 0.4077(2) 0.0572(6) Uani 1 1 d . . . C3 C 0.9056(3) 0.14567(8) 0.2136(3) 0.0588(7) Uani 1 1 d . . . C4 C 1.0670(3) 0.15641(9) 0.2622(3) 0.0648(7) Uani 1 1 d . . . C20 C 0.8819(3) 0.07647(10) 0.4944(3) 0.0708(8) Uani 1 1 d . . . H20A H 0.8966 0.0499 0.4528 0.085 Uiso 1 1 calc R . . C9 C 1.1799(3) 0.13155(10) 0.3693(3) 0.0683(8) Uani 1 1 d . . . C26 C 0.6253(3) 0.20281(9) 0.3332(3) 0.0634(7) Uani 1 1 d . . . H26A H 0.5512 0.1803 0.3301 0.076 Uiso 1 1 calc R . . C17 C 0.8442(3) 0.15420(11) 0.6215(3) 0.0720(8) Uani 1 1 d . . . H17A H 0.8334 0.1807 0.6651 0.086 Uiso 1 1 calc R . . C8 C 0.8191(4) 0.16818(9) 0.1010(3) 0.0702(8) Uani 1 1 d . . . H8A H 0.7130 0.1608 0.0664 0.084 Uiso 1 1 calc R . . C22 C 0.8866(3) 0.23099(9) 0.4124(3) 0.0674(7) Uani 1 1 d . . . H22A H 0.9904 0.2278 0.4631 0.081 Uiso 1 1 calc R . . C5 C 1.1294(4) 0.19114(9) 0.2006(3) 0.0761(8) Uani 1 1 d . . . H5A H 1.2347 0.1994 0.2351 0.091 Uiso 1 1 calc R . . C25 C 0.5799(4) 0.24150(10) 0.2639(3) 0.0718(8) Uani 1 1 d . . . H25A H 0.4759 0.2449 0.2139 0.086 Uiso 1 1 calc R . . C7 C 0.8867(4) 0.20123(10) 0.0391(3) 0.0813(9) Uani 1 1 d . . . H7A H 0.8273 0.2151 -0.0377 0.098 Uiso 1 1 calc R . . C24 C 0.6879(4) 0.27512(10) 0.2683(3) 0.0773(8) Uani 1 1 d . . . H24A H 0.6576 0.3013 0.2211 0.093 Uiso 1 1 calc R . . C19 C 0.8953(4) 0.07706(12) 0.6323(3) 0.0820(9) Uani 1 1 d . . . H19A H 0.9166 0.0510 0.6818 0.098 Uiso 1 1 calc R . . C23 C 0.8411(4) 0.26984(10) 0.3430(3) 0.0794(9) Uani 1 1 d . . . H23A H 0.9145 0.2926 0.3468 0.095 Uiso 1 1 calc R . . C18 C 0.8772(4) 0.11610(13) 0.6959(3) 0.0842(10) Uani 1 1 d . . . H18A H 0.8872 0.1167 0.7886 0.101 Uiso 1 1 calc R . . C10 C 1.1897(4) 0.08579(11) 0.3642(3) 0.0782(9) Uani 1 1 d . . . H10A H 1.1158 0.0702 0.2998 0.094 Uiso 1 1 calc R . . C1 C 0.6200(4) 0.02368(10) 0.2637(3) 0.0956(11) Uani 1 1 d . . . H1A H 0.5695 0.0386 0.3253 0.143 Uiso 1 1 calc R . . H1B H 0.7003 0.0041 0.3129 0.143 Uiso 1 1 calc R . . H1C H 0.5422 0.0069 0.2004 0.143 Uiso 1 1 calc R . . C6 C 1.0420(5) 0.21354(11) 0.0914(4) 0.0875(10) Uani 1 1 d . . . H6A H 1.0869 0.2367 0.0532 0.105 Uiso 1 1 calc R . . C11 C 1.3080(5) 0.06319(13) 0.4537(4) 0.0946(11) Uani 1 1 d . . . H11A H 1.3129 0.0325 0.4486 0.113 Uiso 1 1 calc R . . C2 C 0.8307(4) 0.04551(11) 0.0345(3) 0.0910(10) Uani 1 1 d . . . H2A H 0.8729 0.0701 -0.0052 0.136 Uiso 1 1 calc R . . H2B H 0.7582 0.0293 -0.0346 0.136 Uiso 1 1 calc R . . H2C H 0.9160 0.0265 0.0784 0.136 Uiso 1 1 calc R . . C28 C 0.3000(4) 0.09617(16) -0.1191(4) 0.1139(13) Uani 1 1 d . . . H28A H 0.2731 0.1222 -0.1756 0.137 Uiso 1 1 calc R . . H28B H 0.2440 0.0709 -0.1665 0.137 Uiso 1 1 calc R . . C27 C 0.4735(4) 0.08843(16) -0.0870(3) 0.1140(13) Uani 1 1 d . . . H27A H 0.4961 0.0587 -0.1128 0.137 Uiso 1 1 calc R . . H27B H 0.5246 0.1093 -0.1352 0.137 Uiso 1 1 calc R . . C14 C 1.2897(4) 0.15337(12) 0.4687(3) 0.0854(9) Uani 1 1 d . . . H14A H 1.2837 0.1840 0.4762 0.102 Uiso 1 1 calc R . . C30 C 0.4005(4) 0.11176(15) 0.1082(4) 0.1083(13) Uani 1 1 d . . . H30A H 0.3980 0.0974 0.1926 0.130 Uiso 1 1 calc R . . H30B H 0.4131 0.1434 0.1237 0.130 Uiso 1 1 calc R . . C13 C 1.4094(4) 0.13020(18) 0.5579(4) 0.1060(13) Uani 1 1 d . . . H13A H 1.4835 0.1454 0.6232 0.127 Uiso 1 1 calc R . . C29 C 0.2565(5) 0.10260(18) 0.0074(5) 0.1335(16) Uani 1 1 d . . . H29A H 0.1829 0.1272 0.0007 0.160 Uiso 1 1 calc R . . H29B H 0.2056 0.0762 0.0313 0.160 Uiso 1 1 calc R . . C12 C 1.4179(5) 0.0852(2) 0.5496(4) 0.1100(14) Uani 1 1 d . . . H12A H 1.4978 0.0696 0.6086 0.132 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 0.0723(6) 0.0581(5) 0.0660(5) -0.0025(4) 0.0202(4) 0.0000(4) N1 0.0631(13) 0.0558(12) 0.0552(13) 0.0062(10) 0.0179(10) -0.0021(10) O1 0.0687(12) 0.0850(13) 0.0633(12) -0.0108(10) 0.0152(10) 0.0032(10) C15 0.0503(15) 0.0664(17) 0.0542(15) 0.0109(13) 0.0103(12) -0.0041(12) C16 0.0502(15) 0.0690(17) 0.0512(15) 0.0040(13) 0.0084(12) -0.0078(12) C21 0.0588(16) 0.0638(16) 0.0496(15) -0.0064(12) 0.0138(12) -0.0039(13) C3 0.0711(18) 0.0554(15) 0.0539(15) -0.0002(12) 0.0227(13) -0.0005(13) C4 0.0686(18) 0.0676(17) 0.0657(17) 0.0040(14) 0.0311(15) -0.0005(14) C20 0.0679(18) 0.0694(18) 0.072(2) 0.0173(15) 0.0113(15) -0.0010(14) C9 0.0592(17) 0.084(2) 0.0688(19) 0.0097(16) 0.0286(15) -0.0016(15) C26 0.0598(17) 0.0680(17) 0.0618(16) -0.0025(14) 0.0130(13) -0.0055(14) C17 0.0666(18) 0.092(2) 0.0550(17) -0.0003(15) 0.0090(14) -0.0132(15) C8 0.081(2) 0.0707(18) 0.0573(17) 0.0084(14) 0.0132(15) -0.0039(15) C22 0.0639(17) 0.0684(18) 0.0679(18) -0.0050(14) 0.0115(14) -0.0044(14) C5 0.077(2) 0.0755(19) 0.085(2) 0.0099(17) 0.0361(17) -0.0050(16) C25 0.0661(18) 0.078(2) 0.0684(19) 0.0020(15) 0.0100(14) 0.0071(16) C7 0.108(3) 0.073(2) 0.0657(19) 0.0192(16) 0.0262(18) 0.0069(19) C24 0.086(2) 0.0663(18) 0.080(2) 0.0082(16) 0.0217(18) 0.0046(17) C19 0.073(2) 0.094(2) 0.073(2) 0.0354(19) 0.0061(16) -0.0074(17) C23 0.080(2) 0.0642(19) 0.096(2) -0.0008(17) 0.0244(18) -0.0119(16) C18 0.083(2) 0.113(3) 0.0517(17) 0.0176(19) 0.0057(16) -0.016(2) C10 0.072(2) 0.085(2) 0.083(2) 0.0144(18) 0.0300(17) 0.0106(17) C1 0.114(3) 0.074(2) 0.098(3) 0.0012(18) 0.025(2) -0.0244(19) C6 0.110(3) 0.077(2) 0.088(2) 0.0174(19) 0.047(2) -0.006(2) C11 0.088(3) 0.108(3) 0.097(3) 0.030(2) 0.040(2) 0.024(2) C2 0.096(2) 0.093(2) 0.087(2) -0.0169(19) 0.029(2) 0.0133(19) C28 0.088(3) 0.141(3) 0.099(3) -0.024(3) -0.005(2) 0.020(2) C27 0.093(3) 0.171(4) 0.070(2) -0.026(2) 0.0027(19) 0.018(3) C14 0.071(2) 0.106(3) 0.082(2) 0.008(2) 0.0247(18) -0.0102(19) C30 0.076(2) 0.159(4) 0.091(2) -0.030(2) 0.022(2) 0.019(2) C13 0.075(2) 0.160(4) 0.081(3) 0.015(3) 0.015(2) -0.012(3) C29 0.077(3) 0.206(5) 0.114(3) -0.041(3) 0.016(2) 0.005(3) C12 0.077(3) 0.163(4) 0.093(3) 0.040(3) 0.026(2) 0.026(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 Al1 N1 1.856(2) . ? Al1 O1 1.927(2) . ? Al1 C1 1.957(3) . ? Al1 C2 1.962(3) . ? N1 C15 1.427(3) . ? N1 C3 1.433(3) . ? O1 C27 1.430(4) . ? O1 C30 1.461(4) . ? C15 C20 1.399(4) . ? C15 C16 1.401(4) . ? C16 C17 1.395(4) . ? C16 C21 1.498(4) . ? C21 C22 1.379(4) . ? C21 C26 1.386(4) . ? C3 C8 1.393(4) . ? C3 C4 1.405(4) . ? C4 C5 1.397(4) . ? C4 C9 1.487(4) . ? C20 C19 1.387(4) . ? C9 C14 1.383(4) . ? C9 C10 1.387(4) . ? C26 C25 1.375(4) . ? C17 C18 1.372(4) . ? C8 C7 1.384(4) . ? C22 C23 1.379(4) . ? C5 C6 1.369(4) . ? C25 C24 1.374(4) . ? C7 C6 1.375(5) . ? C24 C23 1.374(4) . ? C19 C18 1.373(5) . ? C10 C11 1.381(4) . ? C11 C12 1.365(6) . ? C28 C29 1.443(6) . ? C28 C27 1.479(5) . ? C14 C13 1.395(5) . ? C30 C29 1.443(5) . ? C13 C12 1.366(6) . ? 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 N1 Al1 O1 106.37(9) . . ? N1 Al1 C1 114.70(13) . . ? O1 Al1 C1 100.34(14) . . ? N1 Al1 C2 112.48(13) . . ? O1 Al1 C2 102.64(12) . . ? C1 Al1 C2 117.93(15) . . ? C15 N1 C3 116.5(2) . . ? C15 N1 Al1 124.09(16) . . ? C3 N1 Al1 119.33(17) . . ? C27 O1 C30 108.0(2) . . ? C27 O1 Al1 126.2(2) . . ? C30 O1 Al1 123.2(2) . . ? C20 C15 C16 117.8(2) . . ? C20 C15 N1 119.5(2) . . ? C16 C15 N1 122.7(2) . . ? C17 C16 C15 119.5(3) . . ? C17 C16 C21 118.2(2) . . ? C15 C16 C21 122.3(2) . . ? C22 C21 C26 118.3(3) . . ? C22 C21 C16 121.8(2) . . ? C26 C21 C16 120.0(2) . . ? C8 C3 C4 118.3(2) . . ? C8 C3 N1 118.9(2) . . ? C4 C3 N1 122.8(2) . . ? C5 C4 C3 118.2(3) . . ? C5 C4 C9 117.0(3) . . ? C3 C4 C9 124.6(2) . . ? C19 C20 C15 121.5(3) . . ? C14 C9 C10 117.7(3) . . ? C14 C9 C4 121.2(3) . . ? C10 C9 C4 120.8(3) . . ? C25 C26 C21 121.0(3) . . ? C18 C17 C16 121.7(3) . . ? C7 C8 C3 121.8(3) . . ? C21 C22 C23 120.8(3) . . ? C6 C5 C4 122.7(3) . . ? C24 C25 C26 120.1(3) . . ? C6 C7 C8 119.9(3) . . ? C23 C24 C25 119.5(3) . . ? C18 C19 C20 120.0(3) . . ? C24 C23 C22 120.3(3) . . ? C17 C18 C19 119.4(3) . . ? C11 C10 C9 120.7(3) . . ? C5 C6 C7 118.9(3) . . ? C12 C11 C10 121.1(4) . . ? C29 C28 C27 106.9(3) . . ? O1 C27 C28 107.2(3) . . ? C9 C14 C13 121.0(4) . . ? C29 C30 O1 106.2(3) . . ? C12 C13 C14 120.1(4) . . ? C30 C29 C28 107.4(3) . . ? C11 C12 C13 119.3(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.220 _refine_diff_density_min -0.155 _refine_diff_density_rms 0.038 #===end data_(2-C6H4-Ph)2NAlMe2(CH2PPh3) _database_code_depnum_ccdc_archive 'CCDC 674919' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C45 H41 Al N P' _chemical_formula_weight 653.74 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' P P 0.1023 0.0942 '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 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 9.8623(11) _cell_length_b 19.289(2) _cell_length_c 19.463(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.741(2) _cell_angle_gamma 90.00 _cell_volume 3689.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.29 _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.482415 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 35173 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6494 _reflns_number_gt 4729 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0791P)^2^+0.6720P] 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_number_reflns 6494 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Al1 Al -0.22559(7) 0.67491(3) 0.41456(3) 0.05426(19) Uani 1 1 d . . . P1 P 0.05403(5) 0.62467(3) 0.33517(3) 0.04937(17) Uani 1 1 d . . . N1 N -0.27882(17) 0.76942(9) 0.41571(9) 0.0521(4) Uani 1 1 d . . . C1 C -0.1819(2) 0.82266(11) 0.42884(11) 0.0539(5) Uani 1 1 d . . . C2 C -0.1864(2) 0.88524(12) 0.39129(12) 0.0585(6) Uani 1 1 d . . . C3 C -0.0886(3) 0.93591(13) 0.40961(14) 0.0740(7) Uani 1 1 d . . . H3A H -0.0948 0.9785 0.3872 0.089 Uiso 1 1 calc R . . C4 C 0.0161(3) 0.92525(16) 0.45928(16) 0.0806(8) Uani 1 1 d . . . H4A H 0.0806 0.9597 0.4697 0.097 Uiso 1 1 calc R . . C5 C 0.0242(3) 0.86341(16) 0.49325(15) 0.0763(7) Uani 1 1 d . . . H5A H 0.0963 0.8547 0.5260 0.092 Uiso 1 1 calc R . . C6 C -0.0745(2) 0.81378(13) 0.47905(13) 0.0663(6) Uani 1 1 d . . . H6A H -0.0691 0.7726 0.5041 0.080 Uiso 1 1 calc R . . C7 C -0.2825(3) 0.89853(12) 0.32939(12) 0.0636(6) Uani 1 1 d . . . C8 C -0.3847(3) 0.94763(14) 0.32864(14) 0.0772(7) Uani 1 1 d . . . H8A H -0.3980 0.9716 0.3690 0.093 Uiso 1 1 calc R . . C9 C -0.4677(3) 0.96207(16) 0.26950(16) 0.0914(9) Uani 1 1 d . . . H9A H -0.5368 0.9947 0.2706 0.110 Uiso 1 1 calc R . . C10 C -0.4478(4) 0.92836(18) 0.20994(17) 0.1047(11) Uani 1 1 d . . . H10A H -0.5027 0.9382 0.1699 0.126 Uiso 1 1 calc R . . C11 C -0.3472(4) 0.8800(2) 0.20898(16) 0.1099(12) Uani 1 1 d . . . H11A H -0.3331 0.8573 0.1680 0.132 Uiso 1 1 calc R . . C12 C -0.2657(4) 0.86434(16) 0.26825(14) 0.0901(9) Uani 1 1 d . . . H12A H -0.1989 0.8304 0.2669 0.108 Uiso 1 1 calc R . . C13 C -0.4162(2) 0.79176(11) 0.40659(11) 0.0517(5) Uani 1 1 d . . . C14 C -0.4738(2) 0.83344(11) 0.45612(12) 0.0548(5) Uani 1 1 d . . . C15 C -0.6066(2) 0.85787(13) 0.44272(14) 0.0672(6) Uani 1 1 d . . . H15A H -0.6433 0.8869 0.4745 0.081 Uiso 1 1 calc R . . C16 C -0.6839(3) 0.83986(15) 0.38357(16) 0.0772(7) Uani 1 1 d . . . H16A H -0.7724 0.8564 0.3755 0.093 Uiso 1 1 calc R . . C17 C -0.6299(3) 0.79727(14) 0.33631(15) 0.0729(7) Uani 1 1 d . . . H17A H -0.6826 0.7842 0.2966 0.087 Uiso 1 1 calc R . . C18 C -0.4980(2) 0.77375(12) 0.34738(13) 0.0630(6) Uani 1 1 d . . . H18A H -0.4628 0.7453 0.3147 0.076 Uiso 1 1 calc R . . C19 C -0.3996(2) 0.85103(12) 0.52383(12) 0.0572(5) Uani 1 1 d . . . C20 C -0.3759(3) 0.91933(14) 0.54369(14) 0.0746(7) Uani 1 1 d . . . H20A H -0.4025 0.9549 0.5132 0.089 Uiso 1 1 calc R . . C21 C -0.3136(3) 0.93560(16) 0.60774(16) 0.0878(8) Uani 1 1 d . . . H21A H -0.2972 0.9817 0.6197 0.105 Uiso 1 1 calc R . . C22 C -0.2760(3) 0.88400(18) 0.65356(15) 0.0861(8) Uani 1 1 d . . . H22A H -0.2356 0.8949 0.6971 0.103 Uiso 1 1 calc R . . C23 C -0.2981(3) 0.81652(16) 0.63516(14) 0.0800(8) Uani 1 1 d . . . H23A H -0.2723 0.7814 0.6663 0.096 Uiso 1 1 calc R . . C24 C -0.3587(2) 0.79981(14) 0.57058(13) 0.0670(6) Uani 1 1 d . . . H24A H -0.3720 0.7535 0.5585 0.080 Uiso 1 1 calc R . . C25 C -0.1594(3) 0.63733(14) 0.50704(13) 0.0789(8) Uani 1 1 d . . . H25A H -0.2342 0.6341 0.5355 0.118 Uiso 1 1 calc R . . H25B H -0.0913 0.6677 0.5284 0.118 Uiso 1 1 calc R . . H25C H -0.1211 0.5921 0.5017 0.118 Uiso 1 1 calc R . . C26 C -0.3700(3) 0.61481(14) 0.36995(16) 0.0788(7) Uani 1 1 d . . . H26A H -0.4416 0.6095 0.4001 0.118 Uiso 1 1 calc R . . H26B H -0.3325 0.5702 0.3607 0.118 Uiso 1 1 calc R . . H26C H -0.4058 0.6356 0.3274 0.118 Uiso 1 1 calc R . . C27 C -0.0745(2) 0.68453(11) 0.34782(12) 0.0566(5) Uani 1 1 d . . . H27A H -0.1214 0.6921 0.3027 0.068 Uiso 1 1 calc R . . H27B H -0.0282 0.7276 0.3603 0.068 Uiso 1 1 calc R . . C28 C -0.0161(2) 0.53998(11) 0.31885(11) 0.0536(5) Uani 1 1 d . . . C29 C -0.0735(3) 0.50412(13) 0.37104(14) 0.0759(7) Uani 1 1 d . . . H29A H -0.0729 0.5236 0.4148 0.091 Uiso 1 1 calc R . . C30 C -0.1313(3) 0.43994(15) 0.35860(17) 0.0894(9) Uani 1 1 d . . . H30A H -0.1685 0.4160 0.3940 0.107 Uiso 1 1 calc R . . C31 C -0.1343(3) 0.41155(15) 0.29471(18) 0.0955(10) Uani 1 1 d . . . H31A H -0.1752 0.3686 0.2861 0.115 Uiso 1 1 calc R . . C32 C -0.0776(4) 0.44575(17) 0.24342(17) 0.1105(12) Uani 1 1 d . . . H32A H -0.0791 0.4259 0.1998 0.133 Uiso 1 1 calc R . . C33 C -0.0176(3) 0.50968(14) 0.25525(14) 0.0839(8) Uani 1 1 d . . . H33A H 0.0221 0.5323 0.2198 0.101 Uiso 1 1 calc R . . C34 C 0.1756(2) 0.61889(12) 0.40904(11) 0.0550(5) Uani 1 1 d . . . C35 C 0.2162(3) 0.67910(15) 0.44356(13) 0.0725(7) Uani 1 1 d . . . H35A H 0.1749 0.7211 0.4311 0.087 Uiso 1 1 calc R . . C36 C 0.3181(3) 0.6767(2) 0.49646(15) 0.0929(9) Uani 1 1 d . . . H36A H 0.3463 0.7172 0.5193 0.111 Uiso 1 1 calc R . . C37 C 0.3778(3) 0.6149(2) 0.51547(16) 0.1016(11) Uani 1 1 d . . . H37A H 0.4471 0.6138 0.5509 0.122 Uiso 1 1 calc R . . C38 C 0.3361(3) 0.5541(2) 0.48274(18) 0.0976(10) Uani 1 1 d . . . H38A H 0.3750 0.5120 0.4969 0.117 Uiso 1 1 calc R . . C39 C 0.2367(3) 0.55646(15) 0.42894(14) 0.0756(7) Uani 1 1 d . . . H39A H 0.2101 0.5159 0.4057 0.091 Uiso 1 1 calc R . . C40 C 0.1500(2) 0.64821(11) 0.26299(11) 0.0530(5) Uani 1 1 d . . . C41 C 0.2773(3) 0.62048(14) 0.25663(14) 0.0747(7) Uani 1 1 d . . . H41A H 0.3137 0.5886 0.2889 0.090 Uiso 1 1 calc R . . C42 C 0.3506(3) 0.63992(18) 0.20246(16) 0.0924(9) Uani 1 1 d . . . H42A H 0.4368 0.6214 0.1987 0.111 Uiso 1 1 calc R . . C43 C 0.2976(3) 0.68612(17) 0.15433(15) 0.0867(9) Uani 1 1 d . . . H43A H 0.3471 0.6985 0.1176 0.104 Uiso 1 1 calc R . . C44 C 0.1714(3) 0.71438(16) 0.16011(13) 0.0827(8) Uani 1 1 d . . . H44A H 0.1356 0.7463 0.1277 0.099 Uiso 1 1 calc R . . C45 C 0.0980(3) 0.69507(14) 0.21438(12) 0.0679(6) Uani 1 1 d . . . H45A H 0.0121 0.7140 0.2182 0.082 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 0.0530(4) 0.0500(4) 0.0609(4) 0.0033(3) 0.0113(3) 0.0050(3) P1 0.0471(3) 0.0479(3) 0.0538(3) -0.0017(2) 0.0083(2) 0.0020(2) N1 0.0469(9) 0.0490(10) 0.0607(11) -0.0018(8) 0.0075(8) 0.0042(8) C1 0.0507(12) 0.0540(13) 0.0586(13) -0.0092(10) 0.0134(10) 0.0032(10) C2 0.0630(14) 0.0556(13) 0.0588(13) -0.0061(11) 0.0170(11) -0.0015(11) C3 0.0856(18) 0.0596(15) 0.0791(17) -0.0094(13) 0.0208(15) -0.0121(13) C4 0.0673(17) 0.083(2) 0.093(2) -0.0266(16) 0.0137(15) -0.0179(14) C5 0.0553(15) 0.087(2) 0.0854(18) -0.0150(15) 0.0012(13) -0.0019(13) C6 0.0547(13) 0.0701(16) 0.0735(16) -0.0047(12) 0.0024(12) 0.0034(12) C7 0.0788(16) 0.0511(13) 0.0624(14) 0.0033(11) 0.0155(12) -0.0070(12) C8 0.098(2) 0.0656(16) 0.0689(16) 0.0030(13) 0.0125(15) 0.0068(15) C9 0.112(2) 0.0808(19) 0.080(2) 0.0122(16) 0.0015(18) 0.0171(17) C10 0.140(3) 0.094(2) 0.077(2) 0.0099(18) -0.012(2) 0.009(2) C11 0.158(3) 0.110(3) 0.0606(18) -0.0145(17) 0.003(2) 0.017(2) C12 0.117(2) 0.083(2) 0.0697(18) -0.0099(15) 0.0062(17) 0.0169(17) C13 0.0490(12) 0.0462(11) 0.0600(13) 0.0059(10) 0.0059(10) 0.0017(9) C14 0.0495(12) 0.0519(12) 0.0636(13) 0.0076(10) 0.0084(10) 0.0057(9) C15 0.0560(14) 0.0669(15) 0.0799(17) 0.0085(13) 0.0125(13) 0.0123(11) C16 0.0542(14) 0.0792(18) 0.097(2) 0.0180(16) 0.0005(14) 0.0130(13) C17 0.0632(15) 0.0709(16) 0.0811(17) 0.0096(14) -0.0146(13) -0.0016(13) C18 0.0651(14) 0.0561(13) 0.0667(14) 0.0007(11) -0.0007(12) 0.0025(11) C19 0.0508(12) 0.0603(13) 0.0625(13) 0.0006(11) 0.0180(10) 0.0072(10) C20 0.0904(19) 0.0626(16) 0.0719(17) -0.0027(13) 0.0140(14) 0.0084(13) C21 0.106(2) 0.0769(19) 0.082(2) -0.0193(16) 0.0155(17) -0.0053(17) C22 0.086(2) 0.105(2) 0.0673(17) -0.0116(17) 0.0057(15) -0.0067(17) C23 0.0810(18) 0.091(2) 0.0674(16) 0.0097(15) 0.0010(14) 0.0020(15) C24 0.0645(14) 0.0657(15) 0.0713(16) 0.0049(12) 0.0078(12) 0.0012(12) C25 0.102(2) 0.0672(16) 0.0680(16) 0.0107(13) 0.0111(14) 0.0141(14) C26 0.0667(16) 0.0617(15) 0.108(2) 0.0027(14) 0.0073(15) -0.0018(12) C27 0.0570(13) 0.0510(12) 0.0626(13) 0.0002(10) 0.0096(11) 0.0050(10) C28 0.0481(11) 0.0505(12) 0.0623(13) -0.0025(10) 0.0044(10) 0.0017(9) C29 0.0907(19) 0.0615(15) 0.0780(17) -0.0044(13) 0.0228(15) -0.0112(14) C30 0.099(2) 0.0724(18) 0.100(2) 0.0033(16) 0.0260(18) -0.0203(16) C31 0.111(2) 0.0644(18) 0.112(3) -0.0168(17) 0.012(2) -0.0308(17) C32 0.155(3) 0.091(2) 0.087(2) -0.0279(18) 0.022(2) -0.052(2) C33 0.108(2) 0.0766(18) 0.0688(16) -0.0144(14) 0.0194(15) -0.0270(16) C34 0.0522(12) 0.0589(13) 0.0547(12) 0.0012(10) 0.0093(10) -0.0024(10) C35 0.0737(16) 0.0782(17) 0.0662(15) -0.0054(13) 0.0090(13) -0.0120(13) C36 0.088(2) 0.124(3) 0.0657(17) -0.0103(18) -0.0005(16) -0.034(2) C37 0.0737(19) 0.161(4) 0.0679(19) 0.026(2) -0.0098(15) -0.024(2) C38 0.0762(19) 0.111(3) 0.102(2) 0.036(2) -0.0131(17) 0.0011(18) C39 0.0644(15) 0.0763(17) 0.0840(18) 0.0093(14) -0.0060(14) 0.0040(13) C40 0.0522(12) 0.0542(12) 0.0534(12) -0.0036(10) 0.0082(10) -0.0027(10) C41 0.0648(15) 0.0854(18) 0.0761(16) 0.0156(14) 0.0203(13) 0.0148(13) C42 0.0714(18) 0.116(2) 0.095(2) 0.0107(19) 0.0365(16) 0.0164(17) C43 0.088(2) 0.107(2) 0.0696(17) 0.0081(16) 0.0317(15) -0.0014(17) C44 0.092(2) 0.096(2) 0.0610(16) 0.0153(14) 0.0112(15) 0.0006(16) C45 0.0618(14) 0.0805(17) 0.0621(15) 0.0050(13) 0.0084(12) 0.0048(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 Al1 N1 1.8977(18) . ? Al1 C26 1.980(3) . ? Al1 C25 1.999(3) . ? Al1 C27 2.064(2) . ? P1 C27 1.747(2) . ? P1 C28 1.792(2) . ? P1 C34 1.798(2) . ? P1 C40 1.815(2) . ? N1 C1 1.412(3) . ? N1 C13 1.419(3) . ? C1 C6 1.391(3) . ? C1 C2 1.410(3) . ? C2 C3 1.399(3) . ? C2 C7 1.492(3) . ? C3 C4 1.370(4) . ? C4 C5 1.363(4) . ? C5 C6 1.377(3) . ? C7 C8 1.382(4) . ? C7 C12 1.382(4) . ? C8 C9 1.385(4) . ? C9 C10 1.357(4) . ? C10 C11 1.363(5) . ? C11 C12 1.384(4) . ? C13 C18 1.395(3) . ? C13 C14 1.410(3) . ? C14 C15 1.396(3) . ? C14 C19 1.492(3) . ? C15 C16 1.372(4) . ? C16 C17 1.373(4) . ? C17 C18 1.377(3) . ? C19 C24 1.381(3) . ? C19 C20 1.387(3) . ? C20 C21 1.379(4) . ? C21 C22 1.367(4) . ? C22 C23 1.363(4) . ? C23 C24 1.385(4) . ? C28 C33 1.368(3) . ? C28 C29 1.388(3) . ? C29 C30 1.376(4) . ? C30 C31 1.357(4) . ? C31 C32 1.355(4) . ? C32 C33 1.379(4) . ? C34 C35 1.384(3) . ? C34 C39 1.387(3) . ? C35 C36 1.378(4) . ? C36 C37 1.367(5) . ? C37 C38 1.380(5) . ? C38 C39 1.375(4) . ? C40 C45 1.377(3) . ? C40 C41 1.379(3) . ? C41 C42 1.379(4) . ? C42 C43 1.365(4) . ? C43 C44 1.372(4) . ? C44 C45 1.380(3) . ? 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 N1 Al1 C26 112.20(10) . . ? N1 Al1 C25 114.06(10) . . ? C26 Al1 C25 110.60(13) . . ? N1 Al1 C27 97.80(8) . . ? C26 Al1 C27 107.88(11) . . ? C25 Al1 C27 113.60(11) . . ? C27 P1 C28 110.69(10) . . ? C27 P1 C34 111.84(11) . . ? C28 P1 C34 107.91(10) . . ? C27 P1 C40 111.99(11) . . ? C28 P1 C40 108.02(10) . . ? C34 P1 C40 106.17(10) . . ? C1 N1 C13 115.27(17) . . ? C1 N1 Al1 121.14(14) . . ? C13 N1 Al1 123.54(14) . . ? C6 C1 C2 117.3(2) . . ? C6 C1 N1 120.2(2) . . ? C2 C1 N1 122.5(2) . . ? C3 C2 C1 118.3(2) . . ? C3 C2 C7 117.7(2) . . ? C1 C2 C7 123.8(2) . . ? C4 C3 C2 122.6(3) . . ? C5 C4 C3 119.0(3) . . ? C4 C5 C6 119.9(3) . . ? C5 C6 C1 122.7(3) . . ? C8 C7 C12 117.2(3) . . ? C8 C7 C2 122.7(2) . . ? C12 C7 C2 120.0(2) . . ? C7 C8 C9 121.8(3) . . ? C10 C9 C8 119.8(3) . . ? C9 C10 C11 119.7(3) . . ? C10 C11 C12 120.8(3) . . ? C7 C12 C11 120.7(3) . . ? C18 C13 C14 117.9(2) . . ? C18 C13 N1 120.6(2) . . ? C14 C13 N1 121.46(19) . . ? C15 C14 C13 119.3(2) . . ? C15 C14 C19 118.2(2) . . ? C13 C14 C19 122.53(19) . . ? C16 C15 C14 121.3(2) . . ? C15 C16 C17 119.6(2) . . ? C16 C17 C18 120.4(2) . . ? C17 C18 C13 121.4(2) . . ? C24 C19 C20 117.5(2) . . ? C24 C19 C14 121.0(2) . . ? C20 C19 C14 121.4(2) . . ? C21 C20 C19 121.3(3) . . ? C22 C21 C20 120.0(3) . . ? C23 C22 C21 119.7(3) . . ? C22 C23 C24 120.6(3) . . ? C19 C24 C23 120.8(3) . . ? P1 C27 Al1 126.80(12) . . ? C33 C28 C29 118.4(2) . . ? C33 C28 P1 121.65(18) . . ? C29 C28 P1 119.97(18) . . ? C30 C29 C28 120.5(3) . . ? C31 C30 C29 120.1(3) . . ? C32 C31 C30 120.0(3) . . ? C31 C32 C33 120.7(3) . . ? C28 C33 C32 120.4(3) . . ? C35 C34 C39 119.4(2) . . ? C35 C34 P1 118.91(19) . . ? C39 C34 P1 121.50(19) . . ? C36 C35 C34 119.9(3) . . ? C37 C36 C35 120.2(3) . . ? C36 C37 C38 120.7(3) . . ? C39 C38 C37 119.3(3) . . ? C38 C39 C34 120.5(3) . . ? C45 C40 C41 118.9(2) . . ? C45 C40 P1 120.50(17) . . ? C41 C40 P1 120.60(18) . . ? C42 C41 C40 120.1(3) . . ? C43 C42 C41 120.4(3) . . ? C42 C43 C44 120.1(3) . . ? C43 C44 C45 119.5(3) . . ? C40 C45 C44 120.9(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.273 _refine_diff_density_min -0.156 _refine_diff_density_rms 0.038 #===end data_(2-C6H4-Ph)2NAl(C6F5)2 _database_code_depnum_ccdc_archive 'CCDC 674920' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C36 H18 Al F10 N' _chemical_formula_weight 681.49 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' F F 0.0171 0.0103 '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 orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 34.524(14) _cell_length_b 7.611(3) _cell_length_c 11.416(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3000(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.29 _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.627396 _exptl_absorpt_correction_T_max 1.000000 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 26939 _diffrn_reflns_av_R_equivalents 0.0795 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5283 _reflns_number_gt 3120 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0511P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(2) _refine_ls_number_reflns 5283 _refine_ls_number_parameters 433 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1110 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _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 0.10599(3) 0.68141(16) 0.55711(11) 0.0475(3) Uani 1 1 d . . . F1 F 0.10090(7) 0.5041(4) 0.3076(2) 0.0704(7) Uani 1 1 d . . . F2 F 0.04530(7) 0.3115(3) 0.2073(2) 0.0775(8) Uani 1 1 d . . . F4 F -0.02234(7) 0.2946(4) 0.5627(3) 0.0882(8) Uani 1 1 d . . . F3 F -0.01702(7) 0.2084(3) 0.3337(3) 0.0817(8) Uani 1 1 d . . . F5 F 0.03243(7) 0.4886(3) 0.6641(2) 0.0724(8) Uani 1 1 d . . . C14 C 0.20803(12) 0.6485(6) 0.6046(4) 0.0552(12) Uani 1 1 d . . . C3 C 0.12953(13) 1.0579(6) 0.2497(4) 0.0602(12) Uani 1 1 d . . . H3A H 0.1083 1.1183 0.2195 0.072 Uiso 1 1 calc R . . C19 C 0.20279(11) 0.7914(7) 0.6904(4) 0.0588(13) Uani 1 1 d . . . C32 C 0.10353(12) 0.8132(8) 0.8068(4) 0.0646(13) Uani 1 1 d . . . C30 C 0.03712(12) 0.4458(5) 0.5498(4) 0.0532(10) Uani 1 1 d . . . C27 C 0.04234(12) 0.3564(6) 0.3221(4) 0.0579(12) Uani 1 1 d . . . C7 C 0.08490(12) 0.9183(5) 0.3926(4) 0.0502(11) Uani 1 1 d . . . F10 F 0.11989(10) 0.3762(4) 0.7153(3) 0.1114(11) Uani 1 1 d . . . C8 C 0.07759(13) 0.9502(6) 0.5118(4) 0.0552(11) Uani 1 1 d . . . H8A H 0.0974 0.9883 0.5607 0.066 Uiso 1 1 calc R . . C1 C 0.15601(11) 0.8489(5) 0.3883(4) 0.0463(11) Uani 1 1 d . . . N1 N 0.15106(8) 0.7322(4) 0.4825(3) 0.0470(8) Uani 1 1 d . . . C31 C 0.10818(11) 0.6761(7) 0.7292(4) 0.0552(11) Uani 1 1 d . . . C24 C 0.19574(12) 0.9630(7) 0.6567(5) 0.0639(13) Uani 1 1 d . . . H24A H 0.1935 0.9902 0.5775 0.077 Uiso 1 1 calc R . . C29 C 0.00871(12) 0.3475(6) 0.5006(4) 0.0594(12) Uani 1 1 d . . . F6 F 0.09616(9) 0.9768(4) 0.7680(2) 0.0862(9) Uani 1 1 d . . . C2 C 0.12422(11) 0.9433(6) 0.3433(3) 0.0478(11) Uani 1 1 d . . . C9 C 0.04007(14) 0.9242(6) 0.5566(4) 0.0639(12) Uani 1 1 d . . . H9A H 0.0351 0.9446 0.6355 0.077 Uiso 1 1 calc R . . C11 C 0.01783(14) 0.8414(6) 0.3677(5) 0.0704(14) Uani 1 1 d . . . H11A H -0.0024 0.8064 0.3193 0.084 Uiso 1 1 calc R . . C25 C 0.06933(12) 0.5057(5) 0.4913(4) 0.0487(10) Uani 1 1 d . . . C28 C 0.01102(12) 0.3026(6) 0.3848(4) 0.0570(11) Uani 1 1 d . . . C16 C 0.24599(16) 0.3938(7) 0.5470(5) 0.0826(15) Uani 1 1 d . . . H16A H 0.2671 0.3201 0.5592 0.099 Uiso 1 1 calc R . . C12 C 0.05431(12) 0.8645(5) 0.3198(4) 0.0595(12) Uani 1 1 d . . . H12A H 0.0585 0.8447 0.2404 0.071 Uiso 1 1 calc R . . C13 C 0.18359(11) 0.6188(5) 0.5084(4) 0.0490(10) Uani 1 1 d . . . C10 C 0.01066(14) 0.8685(6) 0.4837(5) 0.0746(15) Uani 1 1 d . . . H10A H -0.0140 0.8495 0.5137 0.090 Uiso 1 1 calc R . . C4 C 0.16554(15) 1.0836(7) 0.2011(4) 0.0681(13) Uani 1 1 d . . . H4A H 0.1688 1.1623 0.1396 0.082 Uiso 1 1 calc R . . C26 C 0.07107(11) 0.4536(6) 0.3754(4) 0.0503(11) Uani 1 1 d . . . C22 C 0.19445(18) 1.0539(12) 0.8578(7) 0.108(3) Uani 1 1 d . . . H22A H 0.1913 1.1410 0.9142 0.130 Uiso 1 1 calc R . . C23 C 0.19186(15) 1.0976(8) 0.7413(6) 0.0915(19) Uani 1 1 d . . . H23A H 0.1876 1.2134 0.7185 0.110 Uiso 1 1 calc R . . C20 C 0.20547(12) 0.7565(8) 0.8098(4) 0.0738(15) Uani 1 1 d . . . H20A H 0.2101 0.6419 0.8345 0.089 Uiso 1 1 calc R . . C33 C 0.10544(15) 0.7967(9) 0.9264(4) 0.0781(15) Uani 1 1 d . . . F7 F 0.09911(11) 0.9362(6) 0.9968(3) 0.1224(13) Uani 1 1 d . . . C34 C 0.11236(17) 0.6397(12) 0.9735(5) 0.099(2) Uani 1 1 d . . . C6 C 0.19185(12) 0.8786(6) 0.3359(4) 0.0588(11) Uani 1 1 d . . . H6A H 0.2134 0.8191 0.3643 0.071 Uiso 1 1 calc R . . C5 C 0.19641(14) 0.9927(7) 0.2438(4) 0.0685(14) Uani 1 1 d . . . H5A H 0.2207 1.0080 0.2104 0.082 Uiso 1 1 calc R . . C18 C 0.19086(13) 0.4771(6) 0.4360(4) 0.0643(13) Uani 1 1 d . . . H18A H 0.1745 0.4570 0.3727 0.077 Uiso 1 1 calc R . . C21 C 0.20141(15) 0.8867(12) 0.8924(6) 0.099(2) Uani 1 1 d . . . H21A H 0.2034 0.8601 0.9716 0.118 Uiso 1 1 calc R . . C15 C 0.23918(14) 0.5323(7) 0.6212(5) 0.0760(15) Uani 1 1 d . . . H15A H 0.2557 0.5498 0.6844 0.091 Uiso 1 1 calc R . . C36 C 0.11475(15) 0.5206(8) 0.7830(5) 0.0761(15) Uani 1 1 d . . . F9 F 0.12374(15) 0.3372(7) 0.9488(4) 0.175(2) Uani 1 1 d . . . C17 C 0.22135(15) 0.3653(6) 0.4545(5) 0.0785(15) Uani 1 1 d . . . H17A H 0.2253 0.2704 0.4046 0.094 Uiso 1 1 calc R . . F8 F 0.11442(13) 0.6191(8) 1.0902(3) 0.165(2) Uani 1 1 d . . . C35 C 0.11676(19) 0.4954(10) 0.9027(6) 0.100(2) 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 Al1 0.0397(6) 0.0582(7) 0.0447(7) -0.0010(7) 0.0014(6) -0.0026(6) F1 0.0572(15) 0.098(2) 0.0558(16) -0.0042(15) 0.0100(14) -0.0089(14) F2 0.0703(17) 0.100(2) 0.0623(18) -0.0197(17) -0.0137(13) 0.0024(15) F4 0.0577(15) 0.113(2) 0.094(2) 0.0111(19) 0.0104(16) -0.0286(15) F3 0.0618(16) 0.0835(18) 0.100(2) -0.0003(18) -0.0264(15) -0.0168(14) F5 0.0605(16) 0.096(2) 0.0613(18) -0.0090(15) 0.0164(14) -0.0162(14) C14 0.045(2) 0.069(3) 0.052(3) 0.001(2) -0.001(2) 0.003(2) C3 0.057(3) 0.072(3) 0.052(3) 0.007(2) 0.006(2) 0.002(2) C19 0.034(2) 0.083(4) 0.059(3) -0.005(3) -0.006(2) -0.004(2) C32 0.048(3) 0.096(4) 0.050(3) 0.007(3) 0.002(2) -0.008(3) C30 0.048(3) 0.066(3) 0.046(3) -0.002(3) 0.002(2) -0.002(2) C27 0.055(3) 0.067(3) 0.051(3) -0.004(2) -0.008(2) 0.006(2) C7 0.046(3) 0.051(3) 0.053(3) 0.007(2) 0.002(2) 0.009(2) F10 0.146(3) 0.092(2) 0.096(2) 0.017(2) 0.001(2) 0.039(2) C8 0.052(3) 0.065(3) 0.048(3) 0.003(2) 0.003(2) 0.009(2) C1 0.040(2) 0.049(3) 0.050(3) -0.001(2) 0.000(2) -0.0050(19) N1 0.0343(18) 0.056(2) 0.051(2) 0.0051(18) -0.0027(15) -0.0018(16) C31 0.043(2) 0.075(3) 0.048(3) 0.004(3) 0.004(2) -0.002(2) C24 0.048(3) 0.073(3) 0.071(3) -0.015(3) -0.005(2) -0.006(2) C29 0.042(3) 0.067(3) 0.069(3) 0.010(3) 0.004(2) -0.008(2) F6 0.106(2) 0.082(2) 0.0710(19) -0.0127(17) -0.0015(17) -0.0149(17) C2 0.038(2) 0.062(3) 0.043(3) -0.004(2) 0.000(2) 0.000(2) C9 0.064(3) 0.071(3) 0.057(3) 0.009(3) 0.020(3) 0.015(2) C11 0.054(3) 0.087(4) 0.070(4) 0.015(3) -0.006(3) 0.000(3) C25 0.044(3) 0.052(3) 0.050(3) 0.003(2) -0.006(2) 0.003(2) C28 0.049(3) 0.057(3) 0.065(3) 0.003(3) -0.019(2) -0.007(2) C16 0.076(4) 0.074(3) 0.097(4) -0.004(4) -0.012(4) 0.027(3) C12 0.048(3) 0.069(3) 0.061(3) 0.012(2) -0.008(2) 0.000(2) C13 0.040(2) 0.051(3) 0.056(3) 0.001(2) 0.002(2) -0.001(2) C10 0.050(3) 0.081(4) 0.093(4) 0.029(3) 0.013(3) 0.004(3) C4 0.070(4) 0.079(3) 0.055(3) 0.017(3) 0.011(3) -0.008(3) C26 0.036(2) 0.065(3) 0.050(3) -0.002(2) -0.001(2) -0.002(2) C22 0.070(4) 0.158(7) 0.096(6) -0.068(5) 0.009(4) -0.012(5) C23 0.060(3) 0.091(4) 0.124(6) -0.037(4) 0.013(4) -0.014(3) C20 0.043(3) 0.116(5) 0.062(4) -0.004(3) -0.006(2) -0.005(3) C33 0.067(3) 0.117(5) 0.050(3) -0.010(4) -0.001(3) -0.017(3) F7 0.134(3) 0.173(4) 0.0605(19) -0.036(2) 0.002(2) -0.025(3) C34 0.086(4) 0.169(8) 0.043(4) 0.025(4) 0.000(3) 0.001(5) C6 0.041(2) 0.079(3) 0.056(3) 0.006(3) 0.008(2) -0.005(2) C5 0.055(3) 0.083(4) 0.068(3) 0.005(3) 0.020(3) -0.007(3) C18 0.058(3) 0.065(3) 0.070(3) -0.003(3) 0.001(3) 0.002(3) C21 0.057(4) 0.171(7) 0.068(4) -0.031(5) -0.003(3) -0.006(4) C15 0.060(3) 0.093(4) 0.075(4) 0.011(3) -0.014(3) 0.017(3) C36 0.080(4) 0.085(4) 0.064(4) -0.002(3) 0.003(3) 0.012(3) F9 0.246(6) 0.171(5) 0.109(3) 0.069(3) -0.001(3) 0.055(4) C17 0.078(4) 0.061(3) 0.096(4) -0.008(3) 0.011(3) 0.013(3) F8 0.183(4) 0.265(6) 0.049(2) 0.035(3) -0.001(2) -0.008(4) C35 0.108(5) 0.116(6) 0.077(5) 0.043(5) 0.002(4) 0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 1.815(3) . ? Al1 C31 1.966(4) . ? Al1 C25 1.988(4) . ? Al1 C8 2.327(4) . ? F1 C26 1.345(4) . ? F2 C27 1.358(5) . ? F4 C29 1.346(5) . ? F3 C28 1.338(5) . ? F5 C30 1.354(5) . ? C14 C13 1.403(6) . ? C14 C15 1.405(6) . ? C14 C19 1.475(6) . ? C3 C4 1.375(6) . ? C3 C2 1.392(6) . ? C19 C24 1.383(6) . ? C19 C20 1.393(6) . ? C32 F6 1.346(5) . ? C32 C33 1.372(6) . ? C32 C31 1.379(6) . ? C30 C29 1.356(6) . ? C30 C25 1.375(6) . ? C27 C28 1.360(6) . ? C27 C26 1.379(6) . ? C7 C8 1.405(6) . ? C7 C12 1.405(6) . ? C7 C2 1.482(5) . ? F10 C36 1.356(6) . ? C8 C9 1.407(6) . ? C1 C6 1.393(5) . ? C1 N1 1.405(5) . ? C1 C2 1.409(5) . ? N1 C13 1.447(5) . ? C31 C36 1.352(6) . ? C24 C23 1.414(7) . ? C29 C28 1.368(6) . ? C9 C10 1.379(6) . ? C11 C10 1.363(7) . ? C11 C12 1.384(6) . ? C25 C26 1.383(6) . ? C16 C15 1.372(6) . ? C16 C17 1.373(7) . ? C13 C18 1.381(6) . ? C4 C5 1.361(6) . ? C22 C21 1.353(9) . ? C22 C23 1.375(8) . ? C20 C21 1.375(8) . ? C33 C34 1.332(8) . ? C33 F7 1.349(6) . ? C34 F8 1.343(6) . ? C34 C35 1.372(9) . ? C6 C5 1.373(6) . ? C18 C17 1.370(6) . ? C36 C35 1.382(7) . ? F9 C35 1.336(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 N1 Al1 C31 116.09(16) . . ? N1 Al1 C25 120.77(17) . . ? C31 Al1 C25 112.83(19) . . ? N1 Al1 C8 94.00(16) . . ? C31 Al1 C8 104.87(19) . . ? C25 Al1 C8 103.83(17) . . ? C13 C14 C15 117.7(4) . . ? C13 C14 C19 124.4(4) . . ? C15 C14 C19 117.9(4) . . ? C4 C3 C2 121.2(4) . . ? C24 C19 C20 117.7(5) . . ? C24 C19 C14 122.2(4) . . ? C20 C19 C14 120.1(5) . . ? F6 C32 C33 114.9(5) . . ? F6 C32 C31 120.7(4) . . ? C33 C32 C31 124.4(6) . . ? F5 C30 C29 116.5(4) . . ? F5 C30 C25 119.0(4) . . ? C29 C30 C25 124.5(4) . . ? F2 C27 C28 119.5(4) . . ? F2 C27 C26 120.4(4) . . ? C28 C27 C26 120.1(4) . . ? C8 C7 C12 119.2(4) . . ? C8 C7 C2 120.7(4) . . ? C12 C7 C2 120.1(4) . . ? C7 C8 C9 119.6(4) . . ? C7 C8 Al1 89.3(3) . . ? C9 C8 Al1 100.6(3) . . ? C6 C1 N1 122.6(4) . . ? C6 C1 C2 116.9(4) . . ? N1 C1 C2 120.4(3) . . ? C1 N1 C13 116.0(3) . . ? C1 N1 Al1 126.7(3) . . ? C13 N1 Al1 116.3(3) . . ? C36 C31 C32 112.9(4) . . ? C36 C31 Al1 118.6(4) . . ? C32 C31 Al1 128.5(4) . . ? C19 C24 C23 120.7(5) . . ? F4 C29 C30 121.5(4) . . ? F4 C29 C28 118.7(4) . . ? C30 C29 C28 119.8(4) . . ? C3 C2 C1 119.8(4) . . ? C3 C2 C7 119.5(4) . . ? C1 C2 C7 120.6(4) . . ? C10 C9 C8 120.1(5) . . ? C10 C11 C12 122.0(5) . . ? C30 C25 C26 113.9(4) . . ? C30 C25 Al1 123.7(3) . . ? C26 C25 Al1 121.8(3) . . ? F3 C28 C27 120.4(4) . . ? F3 C28 C29 120.9(4) . . ? C27 C28 C29 118.7(4) . . ? C15 C16 C17 119.3(5) . . ? C11 C12 C7 119.1(5) . . ? C18 C13 C14 119.0(4) . . ? C18 C13 N1 119.0(4) . . ? C14 C13 N1 122.0(4) . . ? C11 C10 C9 119.9(5) . . ? C5 C4 C3 119.4(4) . . ? F1 C26 C27 116.8(4) . . ? F1 C26 C25 120.1(4) . . ? C27 C26 C25 123.0(4) . . ? C21 C22 C23 121.4(6) . . ? C22 C23 C24 118.7(6) . . ? C21 C20 C19 121.8(6) . . ? C34 C33 F7 119.6(6) . . ? C34 C33 C32 119.5(6) . . ? F7 C33 C32 120.8(6) . . ? C33 C34 F8 121.0(8) . . ? C33 C34 C35 120.0(5) . . ? F8 C34 C35 119.0(7) . . ? C5 C6 C1 122.2(4) . . ? C4 C5 C6 120.4(4) . . ? C17 C18 C13 122.2(5) . . ? C22 C21 C20 119.8(7) . . ? C16 C15 C14 122.1(5) . . ? C31 C36 F10 118.2(5) . . ? C31 C36 C35 125.4(6) . . ? F10 C36 C35 116.4(6) . . ? C18 C17 C16 119.7(5) . . ? F9 C35 C34 120.6(6) . . ? F9 C35 C36 121.6(7) . . ? C34 C35 C36 117.8(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.154 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.035 #===end