Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Michael F. Lappert' 'Jean Philippe Bezombes' 'Barbara Gehrhus' 'P. B. Hitchcock' 'Philippe G. Merle' _publ_contact_author_name 'Prof Michael F. Lappert' _publ_contact_author_address ; Department of Chemistry University of Sussex CPES Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; A comparative study of the behaviour of N-trimethylsilyl and N-neopentyl-anilines and 1,2-diaminobenzenes towards trimethylalene; X-ray structures of nine Al-N compounds ; data_lappert-1 _database_code_CSD 202056 _audit_creation_date 2000-10-13T11:48:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [{AlMe2(PhNSiMe3)}2] _chemical_formula_moiety 'C22 H40 Al2 N2 Si2' _chemical_formula_structural 'C22 H40 Al2 N2 Si2' _chemical_formula_sum 'C22 H40 Al2 N2 Si2' _chemical_formula_weight 442.7 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-42(1)c _symmetry_Int_Tables_number 114 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' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' 'y+1/2, x+1/2, z+1/2' _cell_length_a 17.2628(3) _cell_length_b 17.2628(3) _cell_length_c 18.0235(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5371.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12614 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_T_min 0.9215 _exptl_absorpt_correction_T_max 0.9215 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 22802 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_unetI/netI 0.049 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 4738 _reflns_number_gt 3976 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0361P)^2^+3.4732P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 4738 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.092 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.10(15) _refine_diff_density_max 0.296 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.041 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.81327(5) 0.77573(5) 0.95142(5) 0.0319(2) Uani 1 1 d . . . Al2 Al 0.82874(5) 0.69415(5) 0.81864(5) 0.0295(2) Uani 1 1 d . . . Si1 Si 0.90947(5) 0.86455(5) 0.81625(6) 0.0461(3) Uani 1 1 d . . . Si2 Si 0.67811(5) 0.64817(5) 0.91551(5) 0.0381(2) Uani 1 1 d . . . N1 N 0.82659(14) 0.80794(13) 0.84444(12) 0.0298(5) Uani 1 1 d . . . N2 N 0.78035(13) 0.67078(13) 0.91616(12) 0.0286(5) Uani 1 1 d . . . C1 C 0.7359(2) 0.8264(2) 1.01435(19) 0.0504(9) Uani 1 1 d . . . H1A H 0.6859 0.8274 0.9886 0.076 Uiso 1 1 calc R . . H1B H 0.7524 0.8796 1.025 0.076 Uiso 1 1 calc R . . H1C H 0.7306 0.7976 1.061 0.076 Uiso 1 1 calc R . . C2 C 0.9134(2) 0.7730(2) 1.00224(19) 0.0535(9) Uani 1 1 d . . . H2A H 0.9519 0.7479 0.9703 0.08 Uiso 1 1 calc R . . H2B H 0.9084 0.7437 1.0486 0.08 Uiso 1 1 calc R . . H2C H 0.9302 0.826 1.0133 0.08 Uiso 1 1 calc R . . C3 C 0.7702(2) 0.6554(2) 0.73266(17) 0.0454(8) Uani 1 1 d . . . H3A H 0.7166 0.6738 0.7355 0.068 Uiso 1 1 calc R . . H3B H 0.7708 0.5986 0.7328 0.068 Uiso 1 1 calc R . . H3C H 0.7941 0.6745 0.6868 0.068 Uiso 1 1 calc R . . C4 C 0.93570(19) 0.65630(19) 0.8112(2) 0.0460(8) Uani 1 1 d . . . H4A H 0.9656 0.6747 0.854 0.069 Uiso 1 1 calc R . . H4B H 0.9593 0.6758 0.7654 0.069 Uiso 1 1 calc R . . H4C H 0.9357 0.5995 0.8106 0.069 Uiso 1 1 calc R . . C5 C 0.75890(16) 0.85116(16) 0.81493(17) 0.0317(7) Uani 1 1 d . . . C6 C 0.72463(19) 0.91011(18) 0.85609(19) 0.0394(8) Uani 1 1 d . . . H6 H 0.7445 0.9229 0.9037 0.047 Uiso 1 1 calc R . . C7 C 0.6613(2) 0.95046(19) 0.8278(2) 0.0504(10) Uani 1 1 d . . . H7 H 0.6388 0.9913 0.8558 0.06 Uiso 1 1 calc R . . C8 C 0.6312(2) 0.9316(2) 0.7594(2) 0.0597(11) Uani 1 1 d . . . H8 H 0.5862 0.9573 0.7415 0.072 Uiso 1 1 calc R . . C9 C 0.6663(2) 0.8756(2) 0.7172(2) 0.0576(11) Uani 1 1 d . . . H9 H 0.6469 0.8637 0.6693 0.069 Uiso 1 1 calc R . . C10 C 0.7301(2) 0.83644(19) 0.74466(18) 0.0456(8) Uani 1 1 d . . . H10 H 0.7547 0.7985 0.7146 0.055 Uiso 1 1 calc R . . C11 C 1.0054(2) 0.8318(3) 0.8513(2) 0.0629(11) Uani 1 1 d . . . H11A H 1.0131 0.7771 0.8386 0.094 Uiso 1 1 calc R . . H11B H 1.0073 0.838 0.9054 0.094 Uiso 1 1 calc R . . H11C H 1.0464 0.8629 0.8285 0.094 Uiso 1 1 calc R . . C12 C 0.9149(2) 0.8617(3) 0.7133(2) 0.0848(17) Uani 1 1 d . . . H12A H 0.9233 0.8082 0.697 0.127 Uiso 1 1 calc R . . H12B H 0.958 0.8942 0.6964 0.127 Uiso 1 1 calc R . . H12C H 0.8663 0.8811 0.6923 0.127 Uiso 1 1 calc R . . C13 C 0.8948(3) 0.9661(2) 0.8439(4) 0.122(3) Uani 1 1 d . . . H13A H 0.8918 0.9694 0.8981 0.182 Uiso 1 1 calc R . . H13B H 0.8465 0.9854 0.8222 0.182 Uiso 1 1 calc R . . H13C H 0.9383 0.9975 0.8262 0.182 Uiso 1 1 calc R . . C14 C 0.81874(18) 0.60836(17) 0.95802(16) 0.0327(7) Uani 1 1 d . . . C15 C 0.8467(2) 0.54309(17) 0.92236(19) 0.0421(8) Uani 1 1 d . . . H15 H 0.8401 0.5378 0.8703 0.051 Uiso 1 1 calc R . . C16 C 0.8841(2) 0.4852(2) 0.9622(2) 0.0548(10) Uani 1 1 d . . . H16 H 0.9042 0.4412 0.9371 0.066 Uiso 1 1 calc R . . C17 C 0.8922(2) 0.4916(2) 1.0382(2) 0.0616(11) Uani 1 1 d . . . H17 H 0.9182 0.4524 1.0654 0.074 Uiso 1 1 calc R . . C18 C 0.8623(2) 0.5551(2) 1.0744(2) 0.0565(10) Uani 1 1 d . . . H18 H 0.8668 0.559 1.1267 0.068 Uiso 1 1 calc R . . C19 C 0.8257(2) 0.61306(19) 1.03473(17) 0.0426(8) Uani 1 1 d . . . H19 H 0.8052 0.6566 1.0602 0.051 Uiso 1 1 calc R . . C20 C 0.62100(19) 0.7237(2) 0.8672(2) 0.0470(9) Uani 1 1 d . . . H20A H 0.6404 0.7299 0.8165 0.07 Uiso 1 1 calc R . . H20B H 0.626 0.773 0.8939 0.07 Uiso 1 1 calc R . . H20C H 0.5664 0.7083 0.8657 0.07 Uiso 1 1 calc R . . C21 C 0.6397(2) 0.6384(3) 1.0112(2) 0.0656(11) Uani 1 1 d . . . H21A H 0.669 0.5986 1.0378 0.098 Uiso 1 1 calc R . . H21B H 0.5849 0.6235 1.0092 0.098 Uiso 1 1 calc R . . H21C H 0.6447 0.688 1.0372 0.098 Uiso 1 1 calc R . . C22 C 0.6616(2) 0.5540(2) 0.8685(2) 0.0570(10) Uani 1 1 d . . . H22A H 0.681 0.5568 0.8174 0.086 Uiso 1 1 calc R . . H22B H 0.6061 0.5424 0.8678 0.086 Uiso 1 1 calc R . . H22C H 0.6892 0.513 0.8953 0.086 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 0.0362(5) 0.0338(5) 0.0258(4) -0.0060(4) 0.0001(4) -0.0052(4) Al2 0.0368(5) 0.0277(4) 0.0241(4) -0.0022(4) 0.0025(4) 0.0008(3) Si1 0.0371(5) 0.0319(5) 0.0693(7) 0.0015(5) 0.0181(5) -0.0034(4) Si2 0.0363(5) 0.0395(5) 0.0386(5) 0.0022(4) -0.0002(4) -0.0102(4) N1 0.0309(13) 0.0278(13) 0.0306(12) 0.0010(10) 0.0021(10) -0.0018(11) N2 0.0324(13) 0.0289(13) 0.0245(12) 0.0002(11) -0.0017(10) -0.0030(10) C1 0.064(2) 0.048(2) 0.0391(19) -0.0109(17) 0.0098(16) 0.0002(19) C2 0.058(2) 0.065(2) 0.0371(19) 0.0017(19) -0.0137(18) -0.0162(19) C3 0.065(2) 0.041(2) 0.0301(17) -0.0057(15) -0.0007(16) 0.0022(17) C4 0.045(2) 0.044(2) 0.049(2) -0.0013(17) 0.0088(17) 0.0062(16) C5 0.0334(16) 0.0264(15) 0.0353(16) 0.0022(14) 0.0027(14) -0.0028(12) C6 0.0397(19) 0.0303(18) 0.048(2) 0.0035(14) 0.0113(16) -0.0022(15) C7 0.047(2) 0.0317(18) 0.072(3) 0.0175(17) 0.021(2) 0.0043(15) C8 0.047(2) 0.050(2) 0.083(3) 0.027(2) -0.007(2) -0.0021(18) C9 0.067(3) 0.048(2) 0.059(2) 0.0178(19) -0.017(2) 0.0010(19) C10 0.060(2) 0.0344(19) 0.0427(19) 0.0061(16) -0.0068(17) 0.0031(16) C11 0.037(2) 0.082(3) 0.069(3) 0.010(2) 0.0023(18) -0.0142(19) C12 0.057(3) 0.117(4) 0.081(3) 0.058(3) 0.031(2) 0.026(3) C13 0.049(3) 0.055(3) 0.260(8) -0.048(4) 0.045(4) -0.022(2) C14 0.0370(18) 0.0324(17) 0.0289(16) 0.0049(13) -0.0030(14) -0.0046(13) C15 0.055(2) 0.0319(18) 0.0396(19) 0.0033(14) -0.0052(16) -0.0001(15) C16 0.064(3) 0.035(2) 0.065(3) 0.0082(18) -0.012(2) 0.0031(17) C17 0.063(3) 0.053(3) 0.069(3) 0.029(2) -0.020(2) -0.002(2) C18 0.071(3) 0.060(3) 0.038(2) 0.0165(19) -0.0169(19) -0.015(2) C19 0.057(2) 0.0408(19) 0.0297(17) 0.0046(14) -0.0044(16) -0.0059(16) C20 0.0314(19) 0.048(2) 0.061(2) -0.0005(18) -0.0015(16) -0.0043(15) C21 0.049(2) 0.088(3) 0.059(3) 0.011(2) 0.0157(19) -0.014(2) C22 0.061(3) 0.043(2) 0.067(3) 0.0071(18) -0.012(2) -0.0204(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C2 1.957(4) . ? Al1 C1 1.958(3) . ? Al1 N2 2.002(2) . ? Al1 N1 2.020(2) . ? Al1 Al2 2.7895(12) . ? Al2 C4 1.963(3) . ? Al2 C3 1.967(3) . ? Al2 N2 1.987(2) . ? Al2 N1 2.019(2) . ? Si1 N1 1.806(2) . ? Si1 C13 1.840(4) . ? Si1 C12 1.858(5) . ? Si1 C11 1.861(4) . ? Si2 N2 1.808(2) . ? Si2 C20 1.853(4) . ? Si2 C21 1.856(4) . ? Si2 C22 1.856(4) . ? N1 C5 1.485(4) . ? N2 C14 1.473(4) . ? C5 C10 1.384(4) . ? C5 C6 1.392(4) . ? C6 C7 1.393(5) . ? C7 C8 1.378(5) . ? C8 C9 1.371(6) . ? C9 C10 1.383(5) . ? C14 C15 1.384(4) . ? C14 C19 1.390(4) . ? C15 C16 1.390(5) . ? C16 C17 1.381(5) . ? C17 C18 1.375(6) . ? C18 C19 1.382(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 C2 Al1 C1 110.01(16) . . ? C2 Al1 N2 112.18(14) . . ? C1 Al1 N2 113.22(14) . . ? C2 Al1 N1 110.66(13) . . ? C1 Al1 N1 120.50(14) . . ? N2 Al1 N1 88.76(10) . . ? C2 Al1 Al2 107.75(12) . . ? C1 Al1 Al2 141.96(12) . . ? N2 Al1 Al2 45.42(7) . . ? N1 Al1 Al2 46.30(7) . . ? C4 Al2 C3 108.42(15) . . ? C4 Al2 N2 112.83(13) . . ? C3 Al2 N2 114.33(13) . . ? C4 Al2 N1 110.91(13) . . ? C3 Al2 N1 120.19(13) . . ? N2 Al2 N1 89.20(10) . . ? C4 Al2 Al1 108.45(11) . . ? C3 Al2 Al1 142.98(12) . . ? N2 Al2 Al1 45.85(7) . . ? N1 Al2 Al1 46.33(7) . . ? N1 Si1 C13 109.28(16) . . ? N1 Si1 C12 107.84(18) . . ? C13 Si1 C12 107.7(3) . . ? N1 Si1 C11 116.42(15) . . ? C13 Si1 C11 108.7(2) . . ? C12 Si1 C11 106.63(18) . . ? N2 Si2 C20 111.75(13) . . ? N2 Si2 C21 111.27(15) . . ? C20 Si2 C21 108.08(19) . . ? N2 Si2 C22 109.98(15) . . ? C20 Si2 C22 108.71(18) . . ? C21 Si2 C22 106.89(19) . . ? C5 N1 Si1 104.52(17) . . ? C5 N1 Al2 114.89(17) . . ? Si1 N1 Al2 116.57(12) . . ? C5 N1 Al1 113.00(18) . . ? Si1 N1 Al1 120.52(13) . . ? Al2 N1 Al1 87.37(9) . . ? C14 N2 Si2 106.54(18) . . ? C14 N2 Al2 114.35(18) . . ? Si2 N2 Al2 116.64(12) . . ? C14 N2 Al1 111.82(17) . . ? Si2 N2 Al1 118.33(13) . . ? Al2 N2 Al1 88.72(10) . . ? C10 C5 C6 118.0(3) . . ? C10 C5 N1 121.2(3) . . ? C6 C5 N1 120.7(3) . . ? C5 C6 C7 120.3(3) . . ? C8 C7 C6 120.4(4) . . ? C9 C8 C7 119.7(4) . . ? C8 C9 C10 119.9(4) . . ? C9 C10 C5 121.6(3) . . ? C15 C14 C19 118.6(3) . . ? C15 C14 N2 121.0(3) . . ? C19 C14 N2 120.4(3) . . ? C14 C15 C16 120.5(3) . . ? C17 C16 C15 120.1(4) . . ? C18 C17 C16 119.8(3) . . ? C17 C18 C19 120.2(3) . . ? C18 C19 C14 120.7(3) . . ? #===END data_lappert-2 _database_code_CSD 202057 _audit_creation_date 2000-06-16T10:10:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [Me3AlNH(Ph)(CH2tBu)] _chemical_formula_moiety 'C14 H26 Al1 N1' _chemical_formula_structural 'C14 H26 Al N' _chemical_formula_sum 'C14 H26 Al N' _chemical_formula_weight 235.34 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 11.7498(6) _cell_length_b 15.3318(14) _cell_length_c 8.6902(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1565.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9876 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 0.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.109 _exptl_absorpt_correction_T_min 0.9578 _exptl_absorpt_correction_T_max 0.9892 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 8383 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_unetI/netI 0.0421 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.95 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 1410 _reflns_number_gt 1193 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The structure was initially solved in Pn2(1)a , but clearly showed disorder of the neopentyl and phenyl groups giving mirror symmetry perpendicular to 'b'. The structure was then refined as disordered in Pnma with the Al and C1 atoms on the mirror plane. 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^)+(0.0124P)^2^+1.1416P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 1410 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.061 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.228 _refine_ls_restrained_S_all 1.228 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.219 _refine_diff_density_min -0.147 _refine_diff_density_rms 0.034 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Al Al 0.38735(8) 0.25 0.16928(11) 0.0387(3) Uani 1 2 d S . . N N 0.3974(3) 0.2334(5) 0.4050(5) 0.031(2) Uani 0.5 1 d P . . H1 H 0.464(4) 0.221(3) 0.418(5) 0.038(14) Uiso 0.5 1 d P . . C1 C 0.4678(2) 0.3575(2) 0.1175(4) 0.0797(11) Uani 1 1 d . . . H1C H 0.5405 0.3593 0.1726 0.12 Uiso 1 1 calc R . . H1B H 0.4214 0.4078 0.1475 0.12 Uiso 1 1 calc R . . H1A H 0.4819 0.3594 0.0064 0.12 Uiso 1 1 calc R . . C2 C 0.2233(3) 0.25 0.1182(4) 0.0606(12) Uani 1 2 d S . . H2C H 0.1852 0.297 0.1745 0.091 Uiso 0.5 1 calc PR . . H2B H 0.1898 0.1938 0.1473 0.091 Uiso 0.5 1 calc PR . . H2A H 0.2137 0.2591 0.0073 0.091 Uiso 0.5 1 calc PR . . C4 C 0.3734(5) 0.3113(4) 0.4958(6) 0.0360(12) Uani 0.5 1 d P . 1 C5 C 0.4591(4) 0.3517(4) 0.5778(7) 0.0452(13) Uani 0.5 1 d P . 1 H5 H 0.5341 0.3286 0.5754 0.054 Uiso 0.5 1 calc PR . 1 C6 C 0.4360(8) 0.4263(6) 0.6642(12) 0.058(2) Uani 0.5 1 d P . 1 H6 H 0.4948 0.4543 0.7205 0.07 Uiso 0.5 1 calc PR . 1 C7 C 0.3248(8) 0.4592(6) 0.6667(11) 0.069(2) Uani 0.5 1 d P . 1 H7 H 0.3075 0.5093 0.7267 0.083 Uiso 0.5 1 calc PR . 1 C8 C 0.2415(5) 0.4196(5) 0.5832(7) 0.0617(16) Uani 0.5 1 d P . 1 H8 H 0.1667 0.4431 0.5843 0.074 Uiso 0.5 1 calc PR . 1 C9 C 0.2639(5) 0.3455(4) 0.4964(7) 0.0508(14) Uani 0.5 1 d P . 1 H9 H 0.2051 0.3185 0.4384 0.061 Uiso 0.5 1 calc PR . 1 C10 C 0.3309(6) 0.1537(4) 0.4477(7) 0.0377(13) Uani 0.5 1 d P . 2 H10B H 0.3479 0.1082 0.3701 0.045 Uiso 0.5 1 calc PR . 2 H10A H 0.2492 0.1682 0.4376 0.045 Uiso 0.5 1 calc PR . 2 C11 C 0.3484(4) 0.1132(3) 0.6065(6) 0.0437(12) Uani 0.5 1 d P . 2 C12 C 0.4740(8) 0.1018(6) 0.6393(11) 0.052(2) Uani 0.5 1 d P . 2 H12C H 0.4838 0.0711 0.7374 0.079 Uiso 0.5 1 calc PR . 2 H12B H 0.5106 0.1592 0.6452 0.079 Uiso 0.5 1 calc PR . 2 H12A H 0.5091 0.0677 0.5565 0.079 Uiso 0.5 1 calc PR . 2 C13 C 0.2920(5) 0.1658(4) 0.7356(6) 0.0574(14) Uani 0.5 1 d P . 2 H13C H 0.3013 0.1349 0.8335 0.086 Uiso 0.5 1 calc PR . 2 H13B H 0.2108 0.1728 0.7132 0.086 Uiso 0.5 1 calc PR . 2 H13A H 0.3279 0.2234 0.7426 0.086 Uiso 0.5 1 calc PR . 2 C14 C 0.2920(10) 0.0231(7) 0.5978(11) 0.069(3) Uani 0.5 1 d P . 2 H14C H 0.3284 -0.0114 0.5166 0.104 Uiso 0.5 1 calc PR . 2 H14B H 0.2109 0.03 0.5746 0.104 Uiso 0.5 1 calc PR . 2 H14A H 0.3008 -0.0068 0.6967 0.104 Uiso 0.5 1 calc PR . 2 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 Al 0.0253(5) 0.0586(7) 0.0323(5) 0 -0.0010(4) 0 N 0.0227(17) 0.036(7) 0.0357(17) -0.004(2) -0.0014(14) 0.0026(19) C1 0.0552(18) 0.084(2) 0.100(3) 0.042(2) -0.0090(17) -0.0054(16) C2 0.0309(19) 0.111(4) 0.040(2) 0 -0.0032(15) 0 C4 0.033(3) 0.036(3) 0.039(3) 0.002(3) 0.003(2) -0.001(2) C5 0.038(3) 0.045(4) 0.052(4) -0.005(3) 0.005(2) 0.000(3) C6 0.066(7) 0.046(5) 0.063(4) -0.016(4) 0.010(4) -0.002(4) C7 0.075(6) 0.055(6) 0.077(7) -0.018(5) 0.024(5) 0.002(4) C8 0.056(4) 0.055(4) 0.073(4) -0.009(3) 0.011(3) 0.013(3) C9 0.040(3) 0.059(4) 0.053(4) -0.002(3) -0.001(3) 0.013(3) C10 0.033(3) 0.043(4) 0.037(3) -0.001(3) 0.000(3) -0.007(3) C11 0.045(3) 0.046(3) 0.041(3) 0.004(2) 0.002(2) -0.003(2) C12 0.056(6) 0.045(6) 0.057(5) 0.014(4) -0.007(4) 0.000(4) C13 0.060(3) 0.067(4) 0.045(3) 0.005(3) 0.011(3) 0.003(3) C14 0.087(6) 0.056(6) 0.065(6) 0.010(5) 0.004(5) -0.017(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Al C1 1.953(3) . ? Al C1 1.953(3) 8_565 ? Al C2 1.978(3) . ? Al N 2.067(4) 8_565 ? Al N 2.067(4) . ? N N 0.510(16) 8_565 ? N C4 1.082(7) 8_565 ? N C4 1.459(9) . ? N C10 1.496(9) . ? N C10 1.935(10) 8_565 ? C4 N 1.082(7) 8_565 ? C4 C5 1.381(8) . ? C4 C9 1.389(8) . ? C4 C4 1.880(13) 8_565 ? C5 C6 1.394(9) . ? C6 C7 1.401(12) . ? C7 C8 1.361(12) . ? C8 C9 1.389(8) . ? C10 C11 1.528(7) . ? C10 N 1.935(10) 8_565 ? C11 C12 1.513(11) . ? C11 C14 1.534(11) . ? C11 C13 1.532(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 C1 Al C1 115.2(2) . 8_565 ? C1 Al C2 114.84(10) . . ? C1 Al C2 114.84(10) 8_565 . ? C1 Al N 95.5(2) . 8_565 ? C1 Al N 107.8(2) 8_565 8_565 ? C2 Al N 106.14(16) . 8_565 ? C1 Al N 107.8(2) . . ? C1 Al N 95.5(2) 8_565 . ? C2 Al N 106.14(16) . . ? N Al N 14.2(4) 8_565 . ? N N C4 129.3(4) 8_565 8_565 ? N N C4 35.0(3) 8_565 . ? C4 N C4 94.2(6) 8_565 . ? N N C10 144.7(3) 8_565 . ? C4 N C10 33.6(4) 8_565 . ? C4 N C10 115.7(4) . . ? N N C10 26.5(2) 8_565 8_565 ? C4 N C10 108.8(5) 8_565 8_565 ? C4 N C10 23.9(3) . 8_565 ? C10 N C10 118.2(5) . 8_565 ? N N Al 82.9(2) 8_565 . ? C4 N Al 141.8(5) 8_565 . ? C4 N Al 115.1(5) . . ? C10 N Al 108.5(4) . . ? C10 N Al 93.2(3) 8_565 . ? N C4 C5 118.1(6) 8_565 . ? N C4 C9 118.9(6) 8_565 . ? C5 C4 C9 120.3(6) . . ? N C4 N 15.7(5) 8_565 . ? C5 C4 N 120.4(5) . . ? C9 C4 N 119.3(5) . . ? N C4 C4 50.7(4) 8_565 8_565 ? C5 C4 C4 116.7(4) . 8_565 ? C9 C4 C4 112.2(4) . 8_565 ? N C4 C4 35.0(3) . 8_565 ? C4 C5 C6 120.2(6) . . ? C5 C6 C7 119.1(9) . . ? C8 C7 C6 120.1(9) . . ? C7 C8 C9 121.2(6) . . ? C8 C9 C4 119.1(6) . . ? N C10 C11 119.1(5) . . ? N C10 N 8.8(3) . 8_565 ? C11 C10 N 118.9(5) . 8_565 ? C12 C11 C10 110.4(5) . . ? C12 C11 C14 109.1(7) . . ? C10 C11 C14 105.3(5) . . ? C12 C11 C13 110.2(5) . . ? C10 C11 C13 112.9(4) . . ? C14 C11 C13 108.8(6) . . ? #===END data_lappert-3 _database_code_CSD 202058 _audit_creation_date 2000-05-25T09:50:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [{AlMe2(PhNCH2tBu)}2] _chemical_formula_moiety 'C26 H44 Al2 N2' _chemical_formula_structural 'C26 H44 AL2 N2' _chemical_formula_sum 'C26 H44 Al2 N2' _chemical_formula_weight 438.59 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.0800(7) _cell_length_b 9.1565(4) _cell_length_c 15.8407(4) _cell_angle_alpha 90 _cell_angle_beta 126.852(2) _cell_angle_gamma 90 _cell_volume 2678.74(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8069 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_T_min 0.964 _exptl_absorpt_correction_T_max 0.9878 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 14357 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_unetI/netI 0.041 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 27.91 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 3181 _reflns_number_gt 2625 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0291P)^2^+6.7409P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0017(15) _refine_ls_number_reflns 3181 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.48 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.054 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Al Al 0.04322(3) 0.44486(7) 0.36007(4) 0.0222(2) Uani 1 1 d . . . N N 0.06301(9) 0.40556(19) 0.25635(12) 0.0210(4) Uani 1 1 d . . . C1 C 0.07688(10) 0.2590(2) 0.23565(15) 0.0238(4) Uani 1 1 d . . . C2 C 0.07774(13) 0.2336(3) 0.14899(18) 0.0333(5) Uani 1 1 d . . . H2 H 0.0726 0.3136 0.1068 0.04 Uiso 1 1 calc R . . C3 C 0.08589(14) 0.0947(3) 0.1242(2) 0.0398(6) Uani 1 1 d . . . H3 H 0.086 0.0799 0.0649 0.048 Uiso 1 1 calc R . . C4 C 0.09397(14) -0.0235(3) 0.1849(2) 0.0415(6) Uani 1 1 d . . . H4 H 0.0994 -0.1194 0.1675 0.05 Uiso 1 1 calc R . . C5 C 0.09406(14) 0.0001(3) 0.2711(2) 0.0408(6) Uani 1 1 d . . . H5 H 0.0998 -0.0802 0.3135 0.049 Uiso 1 1 calc R . . C6 C 0.08581(12) 0.1407(3) 0.29651(18) 0.0307(5) Uani 1 1 d . . . H6 H 0.0863 0.1552 0.3564 0.037 Uiso 1 1 calc R . . C7 C 0.11163(11) 0.5191(2) 0.25882(16) 0.0259(5) Uani 1 1 d . . . H7A H 0.0973 0.6154 0.2692 0.031 Uiso 1 1 calc R . . H7B H 0.1008 0.5207 0.1881 0.031 Uiso 1 1 calc R . . C8 C 0.19496(11) 0.5052(3) 0.34153(19) 0.0340(5) Uani 1 1 d . . . C9 C 0.22492(14) 0.6570(3) 0.3472(3) 0.0533(8) Uani 1 1 d . . . H9A H 0.2042 0.7288 0.3681 0.08 Uiso 1 1 calc R . . H9B H 0.212 0.6832 0.2778 0.08 Uiso 1 1 calc R . . H9C H 0.2777 0.6563 0.3992 0.08 Uiso 1 1 calc R . . C10 C 0.22884(14) 0.3966(3) 0.3090(3) 0.0527(8) Uani 1 1 d . . . H10A H 0.2158 0.4242 0.2398 0.079 Uiso 1 1 calc R . . H10B H 0.2107 0.2982 0.3051 0.079 Uiso 1 1 calc R . . H10C H 0.2816 0.3981 0.3612 0.079 Uiso 1 1 calc R . . C11 C 0.21592(13) 0.4622(3) 0.4494(2) 0.0464(7) Uani 1 1 d . . . H11A H 0.1944 0.5312 0.4706 0.07 Uiso 1 1 calc R . . H11B H 0.2688 0.4641 0.5012 0.07 Uiso 1 1 calc R . . H11C H 0.1981 0.3635 0.4458 0.07 Uiso 1 1 calc R . . C12 C 0.08562(13) 0.3271(3) 0.48870(17) 0.0392(6) Uani 1 1 d . . . H12A H 0.0807 0.2231 0.4708 0.059 Uiso 1 1 calc R . . H12B H 0.0603 0.3481 0.5195 0.059 Uiso 1 1 calc R . . H12C H 0.137 0.3515 0.5397 0.059 Uiso 1 1 calc R . . C13 C 0.05348(12) 0.6540(3) 0.39504(18) 0.0331(5) Uani 1 1 d . . . H13A H 0.0323 0.7119 0.3308 0.05 Uiso 1 1 calc R . . H13B H 0.1049 0.6782 0.4458 0.05 Uiso 1 1 calc R . . H13C H 0.0283 0.676 0.426 0.05 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 Al 0.0223(3) 0.0264(4) 0.0176(3) -0.0011(2) 0.0117(2) -0.0012(2) N 0.0223(8) 0.0225(9) 0.0215(8) 0.0000(7) 0.0149(7) -0.0004(7) C1 0.0212(9) 0.0238(11) 0.0255(9) 0.0008(8) 0.0135(8) 0.0022(8) C2 0.0396(12) 0.0336(13) 0.0349(12) 0.0022(10) 0.0267(10) 0.0051(10) C3 0.0446(13) 0.0399(15) 0.0413(13) -0.0069(11) 0.0292(12) 0.0042(11) C4 0.0425(13) 0.0303(14) 0.0510(15) -0.0068(11) 0.0277(12) 0.0033(11) C5 0.0457(14) 0.0255(12) 0.0501(15) 0.0052(11) 0.0281(12) 0.0038(11) C6 0.0315(11) 0.0301(12) 0.0323(11) 0.0026(9) 0.0202(10) 0.0013(9) C7 0.0239(10) 0.0254(11) 0.0302(10) 0.0032(8) 0.0171(9) 0.0009(8) C8 0.0233(10) 0.0328(13) 0.0439(13) 0.0030(10) 0.0191(10) 0.0013(9) C9 0.0317(13) 0.0416(16) 0.079(2) 0.0026(15) 0.0292(14) -0.0079(11) C10 0.0308(12) 0.0546(18) 0.074(2) -0.0039(15) 0.0317(14) 0.0054(12) C11 0.0240(11) 0.0570(18) 0.0391(13) 0.0055(12) 0.0086(10) 0.0003(11) C12 0.0393(13) 0.0528(16) 0.0239(11) 0.0078(11) 0.0181(10) 0.0030(11) C13 0.0348(12) 0.0329(13) 0.0333(11) -0.0097(10) 0.0214(10) -0.0063(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Al C13 1.968(2) . ? Al C12 1.970(2) . ? Al N 1.9844(16) . ? Al N 2.0294(17) 2 ? Al Al 2.7921(11) 2 ? N C1 1.462(3) . ? N C7 1.513(3) . ? N Al 2.0294(17) 2 ? C1 C6 1.381(3) . ? C1 C2 1.404(3) . ? C2 C3 1.377(3) . ? C3 C4 1.385(4) . ? C4 C5 1.382(4) . ? C5 C6 1.396(3) . ? C7 C8 1.552(3) . ? C8 C11 1.522(4) . ? C8 C9 1.532(4) . ? C8 C10 1.532(4) . ? 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 C13 Al C12 109.90(11) . . ? C13 Al N 111.15(9) . . ? C12 Al N 122.61(10) . . ? C13 Al N 107.71(9) . 2 ? C12 Al N 115.02(9) . 2 ? N Al N 88.17(7) . 2 ? C13 Al Al 103.11(7) . 2 ? C12 Al Al 146.25(8) . 2 ? N Al Al 46.59(5) . 2 ? N Al Al 45.26(5) 2 2 ? C1 N C7 112.19(15) . . ? C1 N Al 122.84(13) . . ? C7 N Al 112.93(13) . . ? C1 N Al 105.46(12) . 2 ? C7 N Al 112.01(12) . 2 ? Al N Al 88.15(7) . 2 ? C6 C1 C2 118.0(2) . . ? C6 C1 N 121.64(18) . . ? C2 C1 N 120.33(18) . . ? C3 C2 C1 121.1(2) . . ? C2 C3 C4 120.6(2) . . ? C5 C4 C3 119.0(2) . . ? C4 C5 C6 120.6(2) . . ? C1 C6 C5 120.8(2) . . ? N C7 C8 119.33(18) . . ? C11 C8 C9 109.9(2) . . ? C11 C8 C10 109.1(2) . . ? C9 C8 C10 107.7(2) . . ? C11 C8 C7 111.56(18) . . ? C9 C8 C7 105.20(19) . . ? C10 C8 C7 113.1(2) . . ? #===END data_lappert-4 _database_code_CSD 202059 _audit_creation_date 2000-03-24T15:21:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [1,2C6H4(NSiMe3)2(AlMe2)2] _chemical_formula_moiety 'C16 H34 Al2 N2 Si2' _chemical_formula_structural 'C16 H34 AL2 N2 SI2' _chemical_formula_sum 'C16 H34 Al2 N2 Si2' _chemical_formula_weight 364.59 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 9.9516(3) _cell_length_b 10.0786(3) _cell_length_c 11.4394(3) _cell_angle_alpha 90 _cell_angle_beta 100.846(2) _cell_angle_gamma 90 _cell_volume 1126.86(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7497 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION not applied # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.235 _exptl_absorpt_correction_T_min 0.9329 _exptl_absorpt_correction_T_max 0.9329 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 12321 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.024 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.55 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 1962 _reflns_number_gt 1817 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Shledrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 1962 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1858 _refine_ls_wR_factor_gt 0.1829 _refine_ls_goodness_of_fit_ref 1.646 _refine_ls_restrained_S_all 1.646 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.301 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.051 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Si Si 0.20592(6) 0.27089(7) 0.50227(5) 0.0318(3) Uani 1 1 d . . . Al Al 0.10680(6) 0.31022(6) 0.21020(5) 0.0281(3) Uani 1 1 d . . . N N 0.23295(19) 0.24403(18) 0.35604(16) 0.0255(5) Uani 1 1 d . . . C1 C 0.2406(2) 0.1097(2) 0.30944(18) 0.0265(5) Uani 1 1 d . . . C2 C 0.2330(2) -0.0091(2) 0.36910(19) 0.0316(6) Uani 1 1 d . . . H2 H 0.2215 -0.0096 0.4497 0.038 Uiso 1 1 calc R . . C3 C 0.2424(2) -0.1285(2) 0.3082(2) 0.0362(6) Uani 1 1 d . . . H3 H 0.2383 -0.2105 0.3484 0.043 Uiso 1 1 calc R . . C4 C 0.0352(3) 0.2051(3) 0.5156(3) 0.0535(8) Uani 1 1 d . . . H4A H -0.0354 0.2482 0.4564 0.08 Uiso 1 1 calc R . . H4B H 0.0179 0.2233 0.5956 0.08 Uiso 1 1 calc R . . H4C H 0.0328 0.1092 0.5017 0.08 Uiso 1 1 calc R . . C5 C 0.3476(3) 0.1960(3) 0.6116(3) 0.0488(7) Uani 1 1 d . . . H5A H 0.3488 0.0998 0.5994 0.073 Uiso 1 1 calc R . . H5B H 0.3338 0.2148 0.6925 0.073 Uiso 1 1 calc R . . H5C H 0.435 0.234 0.6004 0.073 Uiso 1 1 calc R . . C6 C 0.2035(3) 0.4533(3) 0.5250(2) 0.0438(7) Uani 1 1 d . . . H6A H 0.1288 0.4925 0.4672 0.066 Uiso 1 1 calc R . . H6B H 0.2909 0.4913 0.5138 0.066 Uiso 1 1 calc R . . H6C H 0.1895 0.4723 0.6058 0.066 Uiso 1 1 calc R . . C7 C 0.0710(3) 0.5014(3) 0.2049(2) 0.0445(7) Uani 1 1 d . . . H7A H 0.1572 0.5495 0.2302 0.067 Uiso 1 1 calc R . . H7B H 0.008 0.5231 0.2584 0.067 Uiso 1 1 calc R . . H7C H 0.03 0.5274 0.1234 0.067 Uiso 1 1 calc R . . C8 C -0.0574(3) 0.2007(3) 0.1617(3) 0.0477(7) Uani 1 1 d . . . H8A H -0.0318 0.1067 0.1666 0.071 Uiso 1 1 calc R . . H8B H -0.1003 0.2225 0.0797 0.071 Uiso 1 1 calc R . . H8C H -0.1222 0.2182 0.2147 0.071 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 Si 0.0341(5) 0.0312(5) 0.0315(5) -0.0049(2) 0.0094(3) -0.0034(3) Al 0.0229(5) 0.0252(5) 0.0353(5) -0.0030(2) 0.0033(3) 0.0010(2) N 0.0277(10) 0.0196(9) 0.0295(10) -0.0031(7) 0.0063(7) -0.0016(7) C1 0.0241(11) 0.0215(11) 0.0349(11) -0.0028(8) 0.0077(8) -0.0014(8) C2 0.0327(12) 0.0268(12) 0.0368(12) 0.0020(8) 0.0106(9) -0.0006(9) C3 0.0371(13) 0.0226(12) 0.0511(13) 0.0046(9) 0.0136(10) -0.0009(9) C4 0.0522(18) 0.0588(19) 0.0572(18) -0.0130(13) 0.0301(14) -0.0153(13) C5 0.064(2) 0.0436(16) 0.0363(13) 0.0014(11) 0.0038(12) 0.0022(13) C6 0.0456(15) 0.0413(16) 0.0449(13) -0.0141(11) 0.0097(11) 0.0015(11) C7 0.0385(14) 0.0357(15) 0.0570(16) -0.0003(11) 0.0028(11) 0.0108(11) C8 0.0278(13) 0.0508(17) 0.0617(17) -0.0104(12) 0.0016(11) -0.0064(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si N 1.7644(18) . ? Si C6 1.857(3) . ? Si C5 1.859(3) . ? Si C4 1.857(3) . ? Al C7 1.959(3) . ? Al C8 1.964(3) . ? Al N 2.0041(19) . ? Al N 2.0043(19) 2 ? Al Al 2.8242(12) 2 ? N C1 1.462(3) . ? N Al 2.0043(19) 2 ? C1 C2 1.387(3) . ? C1 C1 1.407(4) 2 ? C2 C3 1.402(3) . ? C3 C3 1.369(5) 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 N Si C6 107.02(11) . . ? N Si C5 110.09(12) . . ? C6 Si C5 109.62(12) . . ? N Si C4 109.15(11) . . ? C6 Si C4 107.79(13) . . ? C5 Si C4 112.97(15) . . ? C7 Al C8 114.06(12) . . ? C7 Al N 115.79(10) . . ? C8 Al N 113.93(11) . . ? C7 Al N 117.94(10) . 2 ? C8 Al N 112.67(10) . 2 ? N Al N 77.62(9) . 2 ? C7 Al Al 100.16(8) . 2 ? C8 Al Al 145.78(9) . 2 ? N Al Al 45.21(5) . 2 ? N Al Al 45.20(5) 2 2 ? C1 N Si 121.02(14) . . ? C1 N Al 94.14(12) . . ? Si N Al 123.70(10) . . ? C1 N Al 94.05(12) . 2 ? Si N Al 125.56(10) . 2 ? Al N Al 89.59(8) . 2 ? C2 C1 C1 120.33(12) . 2 ? C2 C1 N 127.47(18) . . ? C1 C1 N 112.20(10) 2 . ? C1 C2 C3 118.77(19) . . ? C3 C3 C2 120.89(13) 2 . ? #===END data_lappert-5 _database_code_CSD 202060 _audit_creation_date 2000-07-13T14:26:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [C6H4{N(CH2tBu)AlMe2}] _chemical_formula_moiety 'C20 H38 Al2 N2' _chemical_formula_structural 'C20 H38 AL2 N2' _chemical_formula_sum 'C20 H38 Al2 N2' _chemical_formula_weight 360.48 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9936(2) _cell_length_b 10.0922(2) _cell_length_c 28.6783(6) _cell_angle_alpha 86.587(1) _cell_angle_beta 86.748(1) _cell_angle_gamma 85.995(1) _cell_volume 2300.61(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24855 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_T_min 0.9496 _exptl_absorpt_correction_T_max 0.9496 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 23948 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_unetI/netI 0.0504 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.07 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 8008 _reflns_number_gt 6742 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0470P)^2^+2.7195P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 8008 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.34 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.72253(10) 0.30142(7) 0.41877(3) 0.02508(19) Uani 1 1 d . A 1 Al2 Al 0.56864(10) 0.10667(8) 0.37254(3) 0.02724(19) Uani 1 1 d . A 1 N1 N 0.7953(3) 0.1217(2) 0.39508(7) 0.0227(4) Uani 1 1 d . A 1 N2 N 0.6125(3) 0.2968(2) 0.35790(7) 0.0245(5) Uani 1 1 d . A 1 C1 C 0.8748(3) 0.1739(2) 0.35181(9) 0.0247(5) Uani 1 1 d . A 1 C2 C 0.7668(3) 0.2731(2) 0.32982(9) 0.0261(5) Uani 1 1 d . A 1 C3 C 0.8177(4) 0.3340(3) 0.28738(9) 0.0339(6) Uani 1 1 d . A 1 H3 H 0.7445 0.3982 0.2719 0.041 Uiso 1 1 calc R A 1 C4 C 0.9768(4) 0.3006(3) 0.26764(10) 0.0397(7) Uani 1 1 d . A 1 H4 H 1.0113 0.3414 0.2383 0.048 Uiso 1 1 calc R A 1 C5 C 1.0852(4) 0.2087(3) 0.29024(10) 0.0364(7) Uani 1 1 d . A 1 H5 H 1.1952 0.1895 0.277 0.044 Uiso 1 1 calc R A 1 C6 C 1.0338(3) 0.1440(3) 0.33242(9) 0.0303(6) Uani 1 1 d . A 1 H6 H 1.1077 0.0798 0.3477 0.036 Uiso 1 1 calc R A 1 C7 C 0.8970(3) 0.0280(2) 0.42592(9) 0.0263(6) Uani 1 1 d . A 1 H7A H 0.8596 0.0444 0.4587 0.032 Uiso 1 1 calc R A 1 H7B H 1.0152 0.0517 0.4216 0.032 Uiso 1 1 calc R A 1 C8 C 0.8946(3) -0.1232(2) 0.41989(9) 0.0288(6) Uani 1 1 d . A 1 C9 C 0.7171(4) -0.1683(3) 0.42799(11) 0.0374(7) Uani 1 1 d . A 1 H9A H 0.6713 -0.1428 0.4588 0.056 Uiso 1 1 calc R A 1 H9B H 0.7194 -0.2652 0.4266 0.056 Uiso 1 1 calc R A 1 H9C H 0.6462 -0.126 0.4038 0.056 Uiso 1 1 calc R A 1 C10 C 0.9648(4) -0.1636(3) 0.37190(11) 0.0422(7) Uani 1 1 d . A 1 H10A H 1.079 -0.1344 0.3664 0.063 Uiso 1 1 calc R A 1 H10B H 0.8933 -0.1218 0.3478 0.063 Uiso 1 1 calc R A 1 H10C H 0.9672 -0.2605 0.3707 0.063 Uiso 1 1 calc R A 1 C11 C 1.0033(4) -0.1918(3) 0.45776(12) 0.0458(8) Uani 1 1 d . A 1 H11A H 1.1181 -0.1634 0.4531 0.069 Uiso 1 1 calc R A 1 H11B H 1.0046 -0.2884 0.4558 0.069 Uiso 1 1 calc R A 1 H11C H 0.9567 -0.1672 0.4886 0.069 Uiso 1 1 calc R A 1 C12 C 0.4730(3) 0.3796(3) 0.33624(9) 0.0290(6) Uani 1 1 d . A 1 H12A H 0.3667 0.3397 0.3468 0.035 Uiso 1 1 calc R A 1 H12B H 0.487 0.3719 0.302 0.035 Uiso 1 1 calc R A 1 C13 C 0.4518(4) 0.5290(3) 0.34547(9) 0.0315(6) Uani 1 1 d . A 1 C14 C 0.6069(4) 0.6019(3) 0.32922(12) 0.0444(8) Uani 1 1 d . A 1 H14A H 0.6331 0.589 0.2959 0.067 Uiso 1 1 calc R A 1 H14B H 0.7021 0.5666 0.3473 0.067 Uiso 1 1 calc R A 1 H14C H 0.5853 0.6971 0.3339 0.067 Uiso 1 1 calc R A 1 C15 C 0.3018(4) 0.5857(3) 0.31784(12) 0.0500(8) Uani 1 1 d . A 1 H15A H 0.3263 0.5735 0.2844 0.075 Uiso 1 1 calc R A 1 H15B H 0.2814 0.6808 0.3229 0.075 Uiso 1 1 calc R A 1 H15C H 0.2018 0.5392 0.3285 0.075 Uiso 1 1 calc R A 1 C16 C 0.4100(4) 0.5491(3) 0.39755(10) 0.0422(7) Uani 1 1 d . A 1 H16A H 0.5047 0.5133 0.4158 0.063 Uiso 1 1 calc R A 1 H16B H 0.3096 0.5026 0.4078 0.063 Uiso 1 1 calc R A 1 H16C H 0.389 0.6443 0.4023 0.063 Uiso 1 1 calc R A 1 C17 C 0.9147(4) 0.4118(3) 0.41752(11) 0.0393(7) Uani 1 1 d . A 1 H17A H 0.9752 0.4087 0.3869 0.059 Uiso 1 1 calc R A 1 H17B H 0.9901 0.378 0.4419 0.059 Uiso 1 1 calc R A 1 H17C H 0.875 0.5038 0.4231 0.059 Uiso 1 1 calc R A 1 C18 C 0.5856(4) 0.2948(3) 0.47741(10) 0.0404(7) Uani 1 1 d . A 1 H18A H 0.493 0.2375 0.4746 0.061 Uiso 0.5 1 calc PR A 1 H18B H 0.54 0.3847 0.4841 0.061 Uiso 0.5 1 calc PR A 1 H18C H 0.6551 0.2589 0.5029 0.061 Uiso 0.5 1 calc PR A 1 H18D H 0.6324 0.3499 0.4998 0.061 Uiso 0.5 1 calc PR A 1 H18E H 0.5854 0.2027 0.4903 0.061 Uiso 0.5 1 calc PR A 1 H18F H 0.4703 0.3285 0.4715 0.061 Uiso 0.5 1 calc PR A 1 C19 C 0.5556(4) 0.0190(3) 0.31386(11) 0.0424(7) Uani 1 1 d . A 1 H19A H 0.6522 0.04 0.2928 0.064 Uiso 1 1 calc R A 1 H19B H 0.4516 0.0507 0.299 0.064 Uiso 1 1 calc R A 1 H19C H 0.5565 -0.0775 0.3204 0.064 Uiso 1 1 calc R A 1 C20 C 0.3869(4) 0.0789(3) 0.42013(12) 0.0421(7) Uani 1 1 d . A 1 H20A H 0.4064 0.1271 0.4478 0.063 Uiso 0.5 1 calc PR A 1 H20B H 0.3839 -0.0163 0.4289 0.063 Uiso 0.5 1 calc PR A 1 H20C H 0.2795 0.1121 0.4075 0.063 Uiso 0.5 1 calc PR A 1 H20D H 0.3068 0.0215 0.4084 0.063 Uiso 0.5 1 calc PR A 1 H20E H 0.3293 0.1649 0.4272 0.063 Uiso 0.5 1 calc PR A 1 H20F H 0.4337 0.0366 0.4486 0.063 Uiso 0.5 1 calc PR A 1 Al1B Al 0.51938(9) 0.56572(7) 0.12697(3) 0.02549(19) Uani 1 1 d . B 2 Al2B Al 0.69145(10) 0.77550(7) 0.08126(3) 0.02580(19) Uani 1 1 d . B 2 N1B N 0.7554(2) 0.5875(2) 0.10492(7) 0.0224(4) Uani 1 1 d . B 2 N2B N 0.5578(3) 0.7507(2) 0.14210(7) 0.0244(5) Uani 1 1 d . B 2 C1B C 0.8180(3) 0.6268(2) 0.14817(9) 0.0239(5) Uani 1 1 d . B 2 C2B C 0.7025(3) 0.7182(2) 0.17001(9) 0.0249(5) Uani 1 1 d . B 2 C3B C 0.7373(4) 0.7672(3) 0.21214(9) 0.0322(6) Uani 1 1 d . B 2 H3B H 0.6584 0.827 0.2275 0.039 Uiso 1 1 calc R B 2 C4B C 0.8890(4) 0.7279(3) 0.23174(10) 0.0380(7) Uani 1 1 d . B 2 H4B H 0.913 0.7603 0.2609 0.046 Uiso 1 1 calc R B 2 C5B C 1.0047(4) 0.6430(3) 0.20951(10) 0.0365(7) Uani 1 1 d . B 2 H5B H 1.1096 0.6198 0.2229 0.044 Uiso 1 1 calc R B 2 C6B C 0.9699(3) 0.5904(3) 0.16743(9) 0.0301(6) Uani 1 1 d . B 2 H6B H 1.0494 0.5306 0.1523 0.036 Uiso 1 1 calc R B 2 C7B C 0.8682(3) 0.5042(2) 0.07388(9) 0.0261(5) Uani 1 1 d . B 2 H7B1 H 0.9849 0.5267 0.078 0.031 Uiso 1 1 calc R B 2 H7B2 H 0.8426 0.5312 0.0412 0.031 Uiso 1 1 calc R B 2 C8B C 0.8636(3) 0.3511(3) 0.07992(9) 0.0288(6) Uani 1 1 d . B 2 C9B C 0.6891(4) 0.3083(3) 0.07216(11) 0.0359(7) Uani 1 1 d . B 2 H9B1 H 0.6538 0.3443 0.0415 0.054 Uiso 1 1 calc R B 2 H9B2 H 0.6097 0.3421 0.0967 0.054 Uiso 1 1 calc R B 2 H9B3 H 0.6913 0.2109 0.0733 0.054 Uiso 1 1 calc R B 2 C10B C 0.9186(4) 0.2946(3) 0.12765(11) 0.0413(7) Uani 1 1 d . B 2 H10D H 1.0312 0.322 0.1327 0.062 Uiso 1 1 calc R B 2 H10E H 0.9207 0.1973 0.1287 0.062 Uiso 1 1 calc R B 2 H10F H 0.8394 0.3283 0.1522 0.062 Uiso 1 1 calc R B 2 C11B C 0.9857(4) 0.2950(3) 0.04166(12) 0.0458(8) Uani 1 1 d . B 2 H11D H 1.0989 0.322 0.0461 0.069 Uiso 1 1 calc R B 2 H11E H 0.9497 0.3295 0.0109 0.069 Uiso 1 1 calc R B 2 H11F H 0.9866 0.1977 0.0435 0.069 Uiso 1 1 calc R B 2 C12B C 0.4109(3) 0.8261(3) 0.16399(10) 0.0303(6) Uani 1 1 d . B 2 H12C H 0.4128 0.8072 0.1982 0.036 Uiso 1 1 calc R B 2 H12D H 0.3085 0.7893 0.1536 0.036 Uiso 1 1 calc R B 2 C13B C 0.3914(4) 0.9782(3) 0.15512(10) 0.0362(7) Uani 1 1 d . B 2 C14B C 0.5417(5) 1.0474(3) 0.17080(12) 0.0475(8) Uani 1 1 d . B 2 H14D H 0.5237 1.1436 0.1645 0.071 Uiso 1 1 calc R B 2 H14E H 0.6442 1.0146 0.1536 0.071 Uiso 1 1 calc R B 2 H14F H 0.5534 1.0281 0.2044 0.071 Uiso 1 1 calc R B 2 C15B C 0.2320(5) 1.0246(3) 0.18352(13) 0.0573(9) Uani 1 1 d . B 2 H15D H 0.2131 1.1214 0.1791 0.086 Uiso 1 1 calc R B 2 H15E H 0.2453 1.0001 0.2168 0.086 Uiso 1 1 calc R B 2 H15F H 0.1357 0.9819 0.1729 0.086 Uiso 1 1 calc R B 2 C16B C 0.3682(5) 1.0153(3) 0.10330(11) 0.0474(8) Uani 1 1 d . B 2 H16D H 0.3559 1.1124 0.0984 0.071 Uiso 1 1 calc R B 2 H16E H 0.2674 0.9767 0.0936 0.071 Uiso 1 1 calc R B 2 H16F H 0.4665 0.9806 0.0847 0.071 Uiso 1 1 calc R B 2 C17B C 0.4815(4) 0.4580(3) 0.18537(10) 0.0387(7) Uani 1 1 d . B 2 H17D H 0.5695 0.4712 0.2067 0.058 Uiso 1 1 calc R B 2 H17E H 0.4844 0.3638 0.1786 0.058 Uiso 1 1 calc R B 2 H17F H 0.3716 0.4851 0.2 0.058 Uiso 1 1 calc R B 2 C18B C 0.3565(4) 0.5543(3) 0.07884(11) 0.0384(7) Uani 1 1 d . B 2 H18G H 0.3873 0.6117 0.0514 0.058 Uiso 0.5 1 calc PR B 2 H18H H 0.2441 0.5834 0.0913 0.058 Uiso 0.5 1 calc PR B 2 H18I H 0.3568 0.4621 0.0699 0.058 Uiso 0.5 1 calc PR B 2 H18J H 0.2714 0.4931 0.0903 0.058 Uiso 0.5 1 calc PR B 2 H18K H 0.4147 0.5214 0.0504 0.058 Uiso 0.5 1 calc PR B 2 H18L H 0.302 0.6427 0.0718 0.058 Uiso 0.5 1 calc PR B 2 C19B C 0.8830(4) 0.8851(3) 0.08269(11) 0.0404(7) Uani 1 1 d . B 2 H19D H 0.9319 0.8719 0.1133 0.061 Uiso 1 1 calc R B 2 H19E H 0.8454 0.979 0.0772 0.061 Uiso 1 1 calc R B 2 H19F H 0.9676 0.8594 0.0582 0.061 Uiso 1 1 calc R B 2 C20B C 0.5776(4) 0.7889(3) 0.02255(10) 0.0406(7) Uani 1 1 d . B 2 H20G H 0.4838 0.7309 0.0251 0.061 Uiso 0.5 1 calc PR B 2 H20H H 0.6569 0.7614 -0.0029 0.061 Uiso 0.5 1 calc PR B 2 H20I H 0.5349 0.8812 0.016 0.061 Uiso 0.5 1 calc PR B 2 H20J H 0.6333 0.8514 0.0004 0.061 Uiso 0.5 1 calc PR B 2 H20K H 0.4601 0.8209 0.0284 0.061 Uiso 0.5 1 calc PR B 2 H20L H 0.5822 0.7012 0.0094 0.061 Uiso 0.5 1 calc PR B 2 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 0.0280(4) 0.0247(4) 0.0230(4) -0.0032(3) -0.0023(3) -0.0025(3) Al2 0.0260(4) 0.0261(4) 0.0306(4) -0.0034(3) -0.0064(3) -0.0031(3) N1 0.0244(11) 0.0220(10) 0.0217(10) -0.0006(8) -0.0030(8) -0.0009(8) N2 0.0236(11) 0.0252(11) 0.0243(11) -0.0026(9) -0.0028(9) 0.0031(9) C1 0.0284(14) 0.0236(12) 0.0226(13) -0.0038(10) -0.0017(10) -0.0023(10) C2 0.0294(14) 0.0253(13) 0.0239(13) -0.0054(10) -0.0012(10) 0.0004(11) C3 0.0432(17) 0.0336(15) 0.0238(14) 0.0005(11) -0.0010(12) 0.0041(12) C4 0.0493(18) 0.0397(16) 0.0273(15) 0.0030(12) 0.0101(13) 0.0024(14) C5 0.0363(16) 0.0382(16) 0.0328(15) -0.0022(12) 0.0093(12) 0.0023(13) C6 0.0304(15) 0.0296(14) 0.0304(14) -0.0020(11) -0.0013(11) 0.0014(11) C7 0.0284(14) 0.0267(13) 0.0243(13) -0.0004(10) -0.0065(11) -0.0016(11) C8 0.0316(15) 0.0244(13) 0.0308(14) -0.0008(11) -0.0071(11) -0.0012(11) C9 0.0386(17) 0.0302(15) 0.0439(17) -0.0006(12) -0.0029(13) -0.0074(12) C10 0.0509(19) 0.0294(15) 0.0458(18) -0.0096(13) 0.0031(15) 0.0016(13) C11 0.054(2) 0.0297(15) 0.055(2) 0.0048(14) -0.0222(16) -0.0004(14) C12 0.0281(14) 0.0298(14) 0.0292(14) -0.0028(11) -0.0075(11) 0.0038(11) C13 0.0369(16) 0.0280(14) 0.0283(14) -0.0029(11) -0.0013(12) 0.0080(12) C14 0.053(2) 0.0277(15) 0.0505(19) 0.0000(13) 0.0048(15) 0.0011(14) C15 0.052(2) 0.0493(19) 0.0458(19) -0.0048(15) -0.0104(16) 0.0230(16) C16 0.054(2) 0.0369(16) 0.0347(16) -0.0063(13) 0.0027(14) 0.0061(14) C17 0.0410(17) 0.0345(16) 0.0444(17) -0.0053(13) -0.0095(14) -0.0085(13) C18 0.0465(18) 0.0470(18) 0.0270(15) -0.0029(13) 0.0022(13) -0.0005(14) C19 0.0506(19) 0.0357(16) 0.0430(17) -0.0085(13) -0.0195(15) 0.0009(14) C20 0.0288(15) 0.0425(17) 0.0550(19) 0.0032(14) -0.0018(14) -0.0085(13) Al1B 0.0237(4) 0.0244(4) 0.0286(4) -0.0029(3) -0.0010(3) -0.0031(3) Al2B 0.0296(4) 0.0240(4) 0.0238(4) 0.0001(3) -0.0027(3) -0.0023(3) N1B 0.0215(11) 0.0239(10) 0.0224(11) -0.0027(8) -0.0038(8) -0.0022(8) N2B 0.0238(11) 0.0254(11) 0.0240(11) -0.0015(9) -0.0030(9) 0.0006(9) C1B 0.0256(13) 0.0230(12) 0.0237(13) 0.0012(10) -0.0041(10) -0.0062(10) C2B 0.0290(14) 0.0225(12) 0.0233(13) 0.0023(10) -0.0025(10) -0.0045(10) C3B 0.0434(17) 0.0286(14) 0.0251(14) -0.0015(11) -0.0031(12) -0.0051(12) C4B 0.0492(18) 0.0423(17) 0.0243(14) -0.0022(12) -0.0114(13) -0.0086(14) C5B 0.0335(16) 0.0434(17) 0.0339(15) 0.0025(13) -0.0125(12) -0.0061(13) C6B 0.0293(14) 0.0307(14) 0.0308(14) -0.0004(11) -0.0047(11) -0.0046(11) C7B 0.0241(13) 0.0265(13) 0.0275(13) -0.0027(10) 0.0012(10) -0.0023(10) C8B 0.0300(14) 0.0250(13) 0.0310(14) -0.0040(11) 0.0011(11) 0.0008(11) C9B 0.0387(16) 0.0288(14) 0.0417(16) -0.0049(12) -0.0055(13) -0.0065(12) C10B 0.0476(18) 0.0285(15) 0.0479(18) 0.0046(13) -0.0130(15) -0.0004(13) C11B 0.0472(19) 0.0324(16) 0.057(2) -0.0114(14) 0.0143(15) -0.0003(14) C12B 0.0312(15) 0.0286(14) 0.0305(14) -0.0036(11) 0.0012(11) 0.0016(11) C13B 0.0457(17) 0.0293(14) 0.0326(15) -0.0057(12) -0.0026(13) 0.0088(12) C14B 0.072(2) 0.0255(15) 0.0465(19) -0.0030(13) -0.0111(17) -0.0025(15) C15B 0.065(2) 0.0456(19) 0.057(2) -0.0070(16) 0.0083(18) 0.0225(17) C16B 0.061(2) 0.0384(17) 0.0413(18) -0.0005(14) -0.0094(15) 0.0134(15) C17B 0.0415(17) 0.0332(15) 0.0405(17) 0.0004(13) 0.0056(13) -0.0044(13) C18B 0.0273(15) 0.0432(17) 0.0459(18) -0.0067(14) -0.0062(13) -0.0045(12) C19B 0.0438(18) 0.0359(16) 0.0420(17) -0.0001(13) 0.0016(14) -0.0112(13) C20B 0.0489(19) 0.0439(17) 0.0289(15) -0.0008(13) -0.0067(13) -0.0001(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C18 1.954(3) . ? Al1 C17 1.957(3) . ? Al1 N2 2.003(2) . ? Al1 N1 2.011(2) . ? Al1 Al2 2.8226(10) . ? Al2 C19 1.959(3) . ? Al2 C20 1.959(3) . ? Al2 N1 1.977(2) . ? Al2 N2 1.990(2) . ? N1 C1 1.450(3) . ? N1 C7 1.487(3) . ? N2 C2 1.447(3) . ? N2 C12 1.488(3) . ? C1 C6 1.379(4) . ? C1 C2 1.418(4) . ? C2 C3 1.384(4) . ? C3 C4 1.390(4) . ? C4 C5 1.383(4) . ? C5 C6 1.395(4) . ? C7 C8 1.547(3) . ? C8 C9 1.521(4) . ? C8 C10 1.524(4) . ? C8 C11 1.532(4) . ? C12 C13 1.542(4) . ? C13 C14 1.522(4) . ? C13 C15 1.533(4) . ? C13 C16 1.534(4) . ? Al1B C17B 1.962(3) . ? Al1B C18B 1.964(3) . ? Al1B N1B 1.978(2) . ? Al1B N2B 1.990(2) . ? Al1B Al2B 2.8221(11) . ? Al2B C20B 1.952(3) . ? Al2B C19B 1.954(3) . ? Al2B N2B 2.006(2) . ? Al2B N1B 2.018(2) . ? N1B C1B 1.450(3) . ? N1B C7B 1.485(3) . ? N2B C2B 1.452(3) . ? N2B C12B 1.484(3) . ? C1B C6B 1.380(4) . ? C1B C2B 1.407(4) . ? C2B C3B 1.382(4) . ? C3B C4B 1.388(4) . ? C4B C5B 1.373(4) . ? C5B C6B 1.397(4) . ? C7B C8B 1.548(3) . ? C8B C9B 1.521(4) . ? C8B C10B 1.527(4) . ? C8B C11B 1.533(4) . ? C12B C13B 1.539(4) . ? C13B C16B 1.529(4) . ? C13B C14B 1.533(4) . ? C13B C15B 1.533(4) . ? 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 C18 Al1 C17 115.53(14) . . ? C18 Al1 N2 119.63(12) . . ? C17 Al1 N2 115.38(12) . . ? C18 Al1 N1 114.08(12) . . ? C17 Al1 N1 110.10(12) . . ? N2 Al1 N1 75.11(8) . . ? C18 Al1 Al2 98.58(10) . . ? C17 Al1 Al2 145.18(10) . . ? N2 Al1 Al2 44.84(6) . . ? N1 Al1 Al2 44.45(6) . . ? C19 Al2 C20 116.63(14) . . ? C19 Al2 N1 116.86(12) . . ? C20 Al2 N1 116.95(12) . . ? C19 Al2 N2 108.92(12) . . ? C20 Al2 N2 114.17(12) . . ? N1 Al2 N2 76.17(9) . . ? C19 Al2 Al1 145.95(11) . . ? C20 Al2 Al1 96.52(10) . . ? N1 Al2 Al1 45.45(6) . . ? N2 Al2 Al1 45.21(6) . . ? C1 N1 C7 118.2(2) . . ? C1 N1 Al2 98.18(14) . . ? C7 N1 Al2 129.81(16) . . ? C1 N1 Al1 94.81(14) . . ? C7 N1 Al1 117.62(15) . . ? Al2 N1 Al1 90.10(9) . . ? C2 N2 C12 117.9(2) . . ? C2 N2 Al2 96.78(15) . . ? C12 N2 Al2 115.32(16) . . ? C2 N2 Al1 95.71(14) . . ? C12 N2 Al1 133.04(16) . . ? Al2 N2 Al1 89.95(9) . . ? C6 C1 C2 120.2(2) . . ? C6 C1 N1 129.3(2) . . ? C2 C1 N1 110.5(2) . . ? C3 C2 C1 119.7(2) . . ? C3 C2 N2 129.2(2) . . ? C1 C2 N2 111.1(2) . . ? C2 C3 C4 119.5(3) . . ? C5 C4 C3 120.8(3) . . ? C4 C5 C6 120.3(3) . . ? C1 C6 C5 119.5(3) . . ? N1 C7 C8 118.8(2) . . ? C9 C8 C10 109.1(2) . . ? C9 C8 C11 108.5(2) . . ? C10 C8 C11 109.5(2) . . ? C9 C8 C7 110.6(2) . . ? C10 C8 C7 112.8(2) . . ? C11 C8 C7 106.1(2) . . ? N2 C12 C13 118.8(2) . . ? C14 C13 C15 109.6(3) . . ? C14 C13 C16 109.7(2) . . ? C15 C13 C16 108.4(2) . . ? C14 C13 C12 112.3(2) . . ? C15 C13 C12 106.0(2) . . ? C16 C13 C12 110.8(2) . . ? C17B Al1B C18B 116.38(13) . . ? C17B Al1B N1B 117.02(11) . . ? C18B Al1B N1B 116.93(11) . . ? C17B Al1B N2B 109.12(11) . . ? C18B Al1B N2B 114.14(11) . . ? N1B Al1B N2B 76.24(9) . . ? C17B Al1B Al2B 146.43(10) . . ? C18B Al1B Al2B 96.27(10) . . ? N1B Al1B Al2B 45.66(6) . . ? N2B Al1B Al2B 45.29(6) . . ? C20B Al2B C19B 115.26(14) . . ? C20B Al2B N2B 119.74(12) . . ? C19B Al2B N2B 115.49(11) . . ? C20B Al2B N1B 114.41(11) . . ? C19B Al2B N1B 110.04(11) . . ? N2B Al2B N1B 75.01(9) . . ? C20B Al2B Al1B 98.70(10) . . ? C19B Al2B Al1B 145.32(10) . . ? N2B Al2B Al1B 44.84(6) . . ? N1B Al2B Al1B 44.51(6) . . ? C1B N1B C7B 118.8(2) . . ? C1B N1B Al1B 98.47(15) . . ? C7B N1B Al1B 129.68(15) . . ? C1B N1B Al2B 94.38(14) . . ? C7B N1B Al2B 117.37(15) . . ? Al1B N1B Al2B 89.83(9) . . ? C2B N2B C12B 117.8(2) . . ? C2B N2B Al1B 97.09(14) . . ? C12B N2B Al1B 115.43(16) . . ? C2B N2B Al2B 95.27(15) . . ? C12B N2B Al2B 133.25(17) . . ? Al1B N2B Al2B 89.87(9) . . ? C6B C1B C2B 120.3(2) . . ? C6B C1B N1B 128.8(2) . . ? C2B C1B N1B 110.8(2) . . ? C3B C2B C1B 120.0(2) . . ? C3B C2B N2B 128.6(2) . . ? C1B C2B N2B 111.3(2) . . ? C2B C3B C4B 119.1(3) . . ? C5B C4B C3B 120.8(3) . . ? C4B C5B C6B 120.6(3) . . ? C1B C6B C5B 118.9(3) . . ? N1B C7B C8B 118.6(2) . . ? C9B C8B C10B 109.4(2) . . ? C9B C8B C11B 108.4(2) . . ? C10B C8B C11B 109.1(2) . . ? C9B C8B C7B 110.8(2) . . ? C10B C8B C7B 113.1(2) . . ? C11B C8B C7B 105.9(2) . . ? N2B C12B C13B 119.2(2) . . ? C16B C13B C14B 109.0(3) . . ? C16B C13B C15B 109.0(3) . . ? C14B C13B C15B 109.7(3) . . ? C16B C13B C12B 110.7(2) . . ? C14B C13B C12B 112.4(2) . . ? C15B C13B C12B 105.9(3) . . ? #===END data_lappert-6 _database_code_CSD 202061 _audit_creation_date 2000-04-18T17:13:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [{1,2-C6H4(NSiMe3)2AlMe}2] _chemical_formula_moiety 'C26 H50 Al2 N4 Si4' _chemical_formula_structural 'C26 H50 N4 AL2 SI4' _chemical_formula_sum 'C26 H50 Al2 N4 Si4' _chemical_formula_weight 585.02 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.1014(5) _cell_length_b 11.6579(3) _cell_length_c 17.7117(5) _cell_angle_alpha 90 _cell_angle_beta 100.098(2) _cell_angle_gamma 90 _cell_volume 3476.42(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7671 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_T_min 0.9093 _exptl_absorpt_correction_T_max 0.9308 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 14155 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.21 _diffrn_reflns_theta_max 27.9 _diffrn_reflns_theta_full 27.9 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 4117 _reflns_number_gt 3225 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 4117 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1581 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.728 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.053 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Si1 Si 0.09602(4) 0.17105(9) 0.41493(4) 0.0624(3) Uani 1 1 d . . . Si2 Si 0.32097(6) -0.05682(9) 0.62568(6) 0.0800(4) Uani 1 1 d . . . Al Al 0.27544(4) 0.13665(5) 0.49521(4) 0.03396(18) Uani 1 1 d . . . N1 N 0.17178(10) 0.21336(14) 0.49307(9) 0.0310(4) Uani 1 1 d . . . N2 N 0.26751(12) 0.06116(17) 0.58452(12) 0.0460(5) Uani 1 1 d . . . C1 C 0.15114(12) 0.18093(17) 0.56781(11) 0.0312(4) Uani 1 1 d . . . C2 C 0.20180(13) 0.10297(18) 0.61333(12) 0.0372(5) Uani 1 1 d . . . C3 C 0.18230(16) 0.0738(2) 0.68469(14) 0.0494(6) Uani 1 1 d . . . H3 H 0.2154 0.0217 0.717 0.059 Uiso 1 1 calc R . . C4 C 0.11648(16) 0.1185(2) 0.70919(13) 0.0494(6) Uani 1 1 d . . . H4 H 0.1044 0.096 0.7574 0.059 Uiso 1 1 calc R . . C5 C 0.06810(14) 0.1957(2) 0.66432(13) 0.0445(5) Uani 1 1 d . . . H5 H 0.0229 0.2269 0.6814 0.053 Uiso 1 1 calc R . . C6 C 0.08615(13) 0.2272(2) 0.59387(13) 0.0389(5) Uani 1 1 d . . . H6 H 0.0534 0.2813 0.563 0.047 Uiso 1 1 calc R . . C7 C 0.1304(2) 0.1985(3) 0.32242(15) 0.0745(9) Uani 1 1 d . . . H7A H 0.1801 0.1569 0.3218 0.112 Uiso 1 1 calc R . . H7B H 0.1393 0.2809 0.317 0.112 Uiso 1 1 calc R . . H7C H 0.0899 0.1722 0.2798 0.112 Uiso 1 1 calc R . . C8 C 0.0792(3) 0.0153(4) 0.4278(2) 0.1107(17) Uani 1 1 d . . . H8A H 0.0609 0.0028 0.4765 0.166 Uiso 1 1 calc R . . H8B H 0.129 -0.0265 0.4281 0.166 Uiso 1 1 calc R . . H8C H 0.0389 -0.0126 0.3855 0.166 Uiso 1 1 calc R . . C9 C 0.0020(2) 0.2511(7) 0.4121(2) 0.141(3) Uani 1 1 d . . . H9A H -0.018 0.2384 0.4599 0.212 Uiso 1 1 calc R . . H9B H -0.0373 0.2242 0.3687 0.212 Uiso 1 1 calc R . . H9C H 0.0117 0.3332 0.406 0.212 Uiso 1 1 calc R . . C10 C 0.3814(2) -0.0223(4) 0.7214(2) 0.1101(17) Uani 1 1 d . . . H10A H 0.3462 0.002 0.7564 0.165 Uiso 1 1 calc R . . H10B H 0.4186 0.0397 0.7158 0.165 Uiso 1 1 calc R . . H10C H 0.4111 -0.0905 0.7421 0.165 Uiso 1 1 calc R . . C11 C 0.2537(3) -0.1816(3) 0.6333(3) 0.1222(18) Uani 1 1 d . . . H11A H 0.2165 -0.1617 0.6674 0.183 Uiso 1 1 calc R . . H11B H 0.2855 -0.2481 0.654 0.183 Uiso 1 1 calc R . . H11C H 0.224 -0.2004 0.5823 0.183 Uiso 1 1 calc R . . C12 C 0.3915(3) -0.0996(5) 0.5616(3) 0.155(3) Uani 1 1 d . . . H12A H 0.3617 -0.1193 0.5108 0.233 Uiso 1 1 calc R . . H12B H 0.4224 -0.1663 0.5834 0.233 Uiso 1 1 calc R . . H12C H 0.4276 -0.0358 0.5568 0.233 Uiso 1 1 calc R . . C13 C 0.29895(19) 0.0497(2) 0.40796(17) 0.0591(7) Uani 1 1 d . . . H13A H 0.3012 0.102 0.365 0.089 Uiso 1 1 calc R . . H13B H 0.2572 -0.0076 0.3926 0.089 Uiso 1 1 calc R . . H13C H 0.3503 0.011 0.4223 0.089 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 Si1 0.0425(4) 0.1076(7) 0.0358(4) -0.0171(4) 0.0033(3) -0.0136(4) Si2 0.0877(7) 0.0768(6) 0.0861(7) 0.0454(5) 0.0444(5) 0.0479(5) Al 0.0403(4) 0.0314(3) 0.0337(3) 0.0012(2) 0.0161(3) 0.0048(3) N1 0.0311(8) 0.0366(9) 0.0264(8) -0.0006(6) 0.0080(6) 0.0007(7) N2 0.0504(11) 0.0443(11) 0.0485(11) 0.0173(9) 0.0232(9) 0.0164(9) C1 0.0337(10) 0.0340(10) 0.0274(9) -0.0025(7) 0.0091(8) -0.0045(8) C2 0.0428(11) 0.0349(10) 0.0371(11) 0.0036(8) 0.0155(9) 0.0006(9) C3 0.0584(15) 0.0511(14) 0.0421(12) 0.0139(10) 0.0187(11) 0.0037(12) C4 0.0581(15) 0.0582(15) 0.0375(12) 0.0021(10) 0.0241(11) -0.0077(12) C5 0.0432(12) 0.0507(13) 0.0450(12) -0.0073(10) 0.0225(10) -0.0052(10) C6 0.0343(10) 0.0427(11) 0.0418(11) -0.0020(9) 0.0125(9) 0.0005(9) C7 0.079(2) 0.111(3) 0.0318(13) -0.0079(15) 0.0042(13) -0.002(2) C8 0.129(3) 0.129(4) 0.081(2) -0.045(2) 0.040(2) -0.091(3) C9 0.054(2) 0.296(8) 0.064(2) -0.030(3) -0.0171(17) 0.050(3) C10 0.074(2) 0.155(4) 0.103(3) 0.082(3) 0.017(2) 0.038(3) C11 0.171(5) 0.054(2) 0.149(4) 0.038(2) 0.048(4) 0.024(3) C12 0.165(5) 0.177(5) 0.151(4) 0.086(4) 0.099(4) 0.137(4) C13 0.0774(19) 0.0454(14) 0.0643(16) -0.0158(12) 0.0397(15) -0.0054(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si1 N1 1.7912(18) . ? Si1 C9 1.852(4) . ? Si1 C8 1.859(4) . ? Si1 C7 1.863(3) . ? Si2 N2 1.739(2) . ? Si2 C12 1.864(4) . ? Si2 C10 1.868(5) . ? Si2 C11 1.874(5) . ? Al N2 1.8358(19) . ? Al C13 1.948(2) . ? Al N1 1.9621(18) 7_556 ? Al N1 1.9799(18) . ? Al Al 2.7968(12) 7_556 ? N1 C1 1.478(2) . ? N1 Al 1.9621(18) 7_556 ? N2 C2 1.401(3) . ? C1 C6 1.385(3) . ? C1 C2 1.408(3) . ? C2 C3 1.404(3) . ? C3 C4 1.378(4) . ? C4 C5 1.376(4) . ? C5 C6 1.386(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 Si1 C9 112.90(16) . . ? N1 Si1 C8 106.30(16) . . ? C9 Si1 C8 110.1(3) . . ? N1 Si1 C7 109.58(12) . . ? C9 Si1 C7 107.2(2) . . ? C8 Si1 C7 110.78(18) . . ? N2 Si2 C12 107.77(15) . . ? N2 Si2 C10 112.12(17) . . ? C12 Si2 C10 107.2(3) . . ? N2 Si2 C11 111.09(18) . . ? C12 Si2 C11 107.9(3) . . ? C10 Si2 C11 110.6(2) . . ? N2 Al C13 119.39(11) . . ? N2 Al N1 115.99(9) . 7_556 ? C13 Al N1 113.10(10) . 7_556 ? N2 Al N1 91.83(8) . . ? C13 Al N1 121.90(11) . . ? N1 Al N1 89.62(7) 7_556 . ? N2 Al Al 109.27(7) . 7_556 ? C13 Al Al 130.49(10) . 7_556 ? N1 Al Al 45.06(5) 7_556 7_556 ? N1 Al Al 44.55(5) . 7_556 ? C1 N1 Si1 111.58(13) . . ? C1 N1 Al 108.12(12) . 7_556 ? Si1 N1 Al 125.74(10) . 7_556 ? C1 N1 Al 102.76(12) . . ? Si1 N1 Al 114.48(9) . . ? Al N1 Al 90.38(7) 7_556 . ? C2 N2 Si2 121.26(15) . . ? C2 N2 Al 109.40(14) . . ? Si2 N2 Al 128.86(11) . . ? C6 C1 C2 120.63(19) . . ? C6 C1 N1 122.04(19) . . ? C2 C1 N1 117.30(17) . . ? N2 C2 C3 125.1(2) . . ? N2 C2 C1 117.94(18) . . ? C3 C2 C1 116.9(2) . . ? C4 C3 C2 121.8(2) . . ? C5 C4 C3 120.5(2) . . ? C4 C5 C6 119.1(2) . . ? C5 C6 C1 121.0(2) . . ? #===END data_lappert-7 _database_code_CSD 202062 _audit_creation_date 2001-04-13T10:58:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [Me2Al{C6H4(NHCH2tBu)(NCH2tBu)}] _chemical_formula_moiety 'C18 H33 Al1 N2' _chemical_formula_structural 'C18 H33 AL N2' _chemical_formula_sum 'C18 H33 Al N2' _chemical_formula_weight 304.44 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6526(5) _cell_length_b 9.7157(5) _cell_length_c 10.6710(6) _cell_angle_alpha 90.773(3) _cell_angle_beta 96.342(3) _cell_angle_gamma 102.991(3) _cell_volume 968.40(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5216 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_T_min 0.9602 _exptl_absorpt_correction_T_max 0.9602 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 7681 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_unetI/netI 0.0533 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 4542 _reflns_number_gt 3879 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXs-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0650P)^2^+0.3827P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 4542 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.334 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.043 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Al Al 0.34665(4) 0.79462(4) 0.18066(4) 0.02368(13) Uani 1 1 d . . . N1 N 0.50478(12) 0.82760(13) 0.32643(10) 0.0230(2) Uani 1 1 d . . . H1 H 0.5434(18) 0.9157(19) 0.3429(16) 0.027(4) Uiso 1 1 d . . . N2 N 0.25620(12) 0.64484(12) 0.27178(10) 0.0238(2) Uani 1 1 d . . . C1 C 0.42477(15) 0.77480(14) 0.43283(12) 0.0247(3) Uani 1 1 d . . . C2 C 0.29517(15) 0.67412(14) 0.39919(12) 0.0241(3) Uani 1 1 d . . . C3 C 0.22108(17) 0.61647(16) 0.50036(14) 0.0327(3) Uani 1 1 d . . . H3 H 0.1328 0.5488 0.4834 0.039 Uiso 1 1 calc R . . C4 C 0.27612(19) 0.65776(18) 0.62432(14) 0.0381(4) Uani 1 1 d . . . H4 H 0.2246 0.6168 0.6906 0.046 Uiso 1 1 calc R . . C5 C 0.40371(19) 0.75672(18) 0.65436(14) 0.0372(4) Uani 1 1 d . . . H5 H 0.4393 0.7839 0.7398 0.045 Uiso 1 1 calc R . . C6 C 0.47908(17) 0.81581(16) 0.55617(13) 0.0304(3) Uani 1 1 d . . . H6 H 0.5671 0.8837 0.5742 0.037 Uiso 1 1 calc R . . C7 C 0.62458(14) 0.75241(15) 0.31372(13) 0.0269(3) Uani 1 1 d . . . H7B H 0.593 0.6794 0.2446 0.032 Uiso 1 1 calc R . . H7A H 0.642 0.7035 0.3927 0.032 Uiso 1 1 calc R . . C8 C 0.76552(15) 0.84962(16) 0.28696(14) 0.0309(3) Uani 1 1 d . . . C9 C 0.74748(19) 0.9254(2) 0.16354(16) 0.0422(4) Uani 1 1 d . . . H9C H 0.7149 0.8553 0.0934 0.063 Uiso 1 1 calc R . . H9B H 0.8394 0.9867 0.1492 0.063 Uiso 1 1 calc R . . H9A H 0.6766 0.9827 0.1689 0.063 Uiso 1 1 calc R . . C10 C 0.82485(18) 0.9586(2) 0.39583(17) 0.0443(4) Uani 1 1 d . . . H10C H 0.7553 1.0161 0.4069 0.066 Uiso 1 1 calc R . . H10B H 0.9148 1.0198 0.3766 0.066 Uiso 1 1 calc R . . H10A H 0.8423 0.9097 0.4737 0.066 Uiso 1 1 calc R . . C11 C 0.87000(19) 0.7527(2) 0.2758(2) 0.0503(5) Uani 1 1 d . . . H11C H 0.8821 0.7047 0.3551 0.075 Uiso 1 1 calc R . . H11B H 0.9629 0.8095 0.2583 0.075 Uiso 1 1 calc R . . H11A H 0.8316 0.6822 0.2068 0.075 Uiso 1 1 calc R . . C12 C 0.13109(15) 0.53482(15) 0.22546(13) 0.0265(3) Uani 1 1 d . . . H12B H 0.0872 0.5647 0.1451 0.032 Uiso 1 1 calc R . . H12A H 0.0603 0.5273 0.2869 0.032 Uiso 1 1 calc R . . C13 C 0.15935(16) 0.38643(15) 0.20276(14) 0.0289(3) Uani 1 1 d . . . C14 C 0.0226(2) 0.2916(2) 0.1359(2) 0.0518(5) Uani 1 1 d . . . H14C H 0.0387 0.1972 0.1198 0.078 Uiso 1 1 calc R . . H14B H -0.0039 0.3321 0.0556 0.078 Uiso 1 1 calc R . . H14A H -0.0548 0.2846 0.1893 0.078 Uiso 1 1 calc R . . C15 C 0.1996(2) 0.32251(19) 0.32726(17) 0.0491(5) Uani 1 1 d . . . H15C H 0.2138 0.2274 0.3109 0.074 Uiso 1 1 calc R . . H15B H 0.1226 0.3169 0.381 0.074 Uiso 1 1 calc R . . H15A H 0.2884 0.382 0.37 0.074 Uiso 1 1 calc R . . C16 C 0.2796(2) 0.39461(19) 0.12018(19) 0.0480(4) Uani 1 1 d . . . H16C H 0.3681 0.4542 0.1632 0.072 Uiso 1 1 calc R . . H16B H 0.2543 0.4354 0.0397 0.072 Uiso 1 1 calc R . . H16A H 0.2938 0.2994 0.1044 0.072 Uiso 1 1 calc R . . C17 C 0.40189(18) 0.74932(19) 0.01650(14) 0.0368(4) Uani 1 1 d . . . H17C H 0.3171 0.7288 -0.0463 0.055 Uiso 1 1 calc R . . H17B H 0.444 0.6665 0.0231 0.055 Uiso 1 1 calc R . . H17A H 0.4722 0.83 -0.0095 0.055 Uiso 1 1 calc R . . C18 C 0.25982(17) 0.95885(16) 0.18501(16) 0.0352(3) Uani 1 1 d . . . H18C H 0.3277 1.043 0.1618 0.053 Uiso 1 1 calc R . . H18B H 0.2358 0.9736 0.2703 0.053 Uiso 1 1 calc R . . H18A H 0.1726 0.9418 0.1251 0.053 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 Al 0.0263(2) 0.0277(2) 0.0180(2) 0.00377(15) 0.00319(15) 0.00777(16) N1 0.0246(5) 0.0249(6) 0.0203(5) 0.0025(4) 0.0045(4) 0.0066(4) N2 0.0264(6) 0.0251(5) 0.0203(5) 0.0017(4) 0.0033(4) 0.0062(4) C1 0.0297(7) 0.0287(7) 0.0185(6) 0.0024(5) 0.0066(5) 0.0107(5) C2 0.0286(7) 0.0261(6) 0.0205(6) 0.0018(5) 0.0066(5) 0.0103(5) C3 0.0357(8) 0.0351(8) 0.0290(7) 0.0037(6) 0.0139(6) 0.0066(6) C4 0.0501(9) 0.0443(9) 0.0249(7) 0.0059(6) 0.0181(7) 0.0146(7) C5 0.0503(9) 0.0462(9) 0.0182(6) -0.0001(6) 0.0065(6) 0.0167(8) C6 0.0350(7) 0.0353(7) 0.0217(7) -0.0015(5) 0.0020(5) 0.0104(6) C7 0.0254(6) 0.0301(7) 0.0275(7) 0.0061(5) 0.0058(5) 0.0099(5) C8 0.0241(7) 0.0375(8) 0.0306(7) 0.0087(6) 0.0042(5) 0.0055(6) C9 0.0392(9) 0.0501(10) 0.0345(8) 0.0158(7) 0.0086(7) 0.0013(7) C10 0.0325(8) 0.0510(10) 0.0420(9) 0.0040(8) -0.0065(7) -0.0006(7) C11 0.0305(8) 0.0639(12) 0.0629(12) 0.0159(10) 0.0160(8) 0.0184(8) C12 0.0250(6) 0.0274(7) 0.0274(7) 0.0029(5) 0.0006(5) 0.0075(5) C13 0.0323(7) 0.0260(7) 0.0283(7) -0.0002(5) 0.0020(5) 0.0068(6) C14 0.0480(10) 0.0369(9) 0.0628(12) -0.0064(8) -0.0049(9) -0.0008(8) C15 0.0801(14) 0.0362(9) 0.0377(9) 0.0045(7) 0.0008(9) 0.0305(9) C16 0.0562(11) 0.0352(9) 0.0556(11) -0.0078(8) 0.0244(9) 0.0084(8) C17 0.0384(8) 0.0508(9) 0.0206(7) 0.0028(6) 0.0053(6) 0.0076(7) C18 0.0376(8) 0.0316(7) 0.0378(8) 0.0078(6) 0.0008(6) 0.0122(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Al N2 1.8655(12) . ? Al C17 1.9590(15) . ? Al C18 1.9643(15) . ? Al N1 2.0234(12) . ? N1 C1 1.4765(16) . ? N1 C7 1.5169(17) . ? N2 C2 1.3782(17) . ? N2 C12 1.4555(18) . ? C1 C6 1.3804(19) . ? C1 C2 1.411(2) . ? C2 C3 1.4134(18) . ? C3 C4 1.388(2) . ? C4 C5 1.384(3) . ? C5 C6 1.398(2) . ? C7 C8 1.5296(19) . ? C8 C9 1.529(2) . ? C8 C10 1.532(2) . ? C8 C11 1.539(2) . ? C12 C13 1.5471(19) . ? C13 C15 1.523(2) . ? C13 C16 1.522(2) . ? C13 C14 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 N2 Al C17 117.64(7) . . ? N2 Al C18 113.00(6) . . ? C17 Al C18 115.09(7) . . ? N2 Al N1 85.62(5) . . ? C17 Al N1 115.70(6) . . ? C18 Al N1 105.77(6) . . ? C1 N1 C7 111.26(10) . . ? C1 N1 Al 101.62(8) . . ? C7 N1 Al 115.63(9) . . ? C2 N2 C12 121.20(11) . . ? C2 N2 Al 109.83(9) . . ? C12 N2 Al 126.39(9) . . ? C6 C1 C2 123.27(13) . . ? C6 C1 N1 121.48(13) . . ? C2 C1 N1 115.13(11) . . ? N2 C2 C1 115.98(12) . . ? N2 C2 C3 128.08(13) . . ? C1 C2 C3 115.94(13) . . ? C4 C3 C2 120.64(14) . . ? C5 C4 C3 122.07(14) . . ? C4 C5 C6 118.53(14) . . ? C1 C6 C5 119.54(15) . . ? N1 C7 C8 114.32(11) . . ? C9 C8 C7 111.52(12) . . ? C9 C8 C10 109.72(14) . . ? C7 C8 C10 110.87(13) . . ? C9 C8 C11 109.51(14) . . ? C7 C8 C11 105.73(13) . . ? C10 C8 C11 109.40(14) . . ? N2 C12 C13 115.66(11) . . ? C15 C13 C16 109.01(15) . . ? C15 C13 C14 109.04(15) . . ? C16 C13 C14 109.10(15) . . ? C15 C13 C12 110.83(12) . . ? C16 C13 C12 110.58(12) . . ? C14 C13 C12 108.25(13) . . ? #===END data_lappert-9 _database_code_CSD 202063 _audit_creation_date 2000-03-22T16:07:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [{(C6H4(NCH2tBu)2)AlCl}2]' _chemical_formula_moiety 'C32 H52 Al2 Cl2 N4' _chemical_formula_structural 'C32 H52 Al2 Cl2 N4' _chemical_formula_sum 'C32 H52 Al2 Cl2 N4' _chemical_formula_weight 617.64 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 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 12.0101(7) _cell_length_b 14.8750(9) _cell_length_c 20.3163(10) _cell_angle_alpha 90 _cell_angle_beta 106.504(3) _cell_angle_gamma 90 _cell_volume 3480.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22330 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.264 _exptl_absorpt_correction_T_min 0.9251 _exptl_absorpt_correction_T_max 0.9251 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 9892 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.17 _diffrn_reflns_theta_max 22.98 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.945 _diffrn_measured_fraction_theta_max 0.945 _reflns_number_total 4566 _reflns_number_gt 3780 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0347P)^2^+2.1748P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 4566 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.354 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.04 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 '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' 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 0.34556(6) 0.33458(5) 0.06914(4) 0.0304(2) Uani 1 1 d . . . Al2 Al 0.34065(6) 0.23887(5) 0.18241(4) 0.0322(2) Uani 1 1 d . . . Cl1 Cl 0.30960(6) 0.46988(5) 0.04017(4) 0.0484(2) Uani 1 1 d . . . Cl2 Cl 0.23616(6) 0.24246(5) 0.24982(4) 0.0469(2) Uani 1 1 d . . . N1 N 0.38795(18) 0.24967(14) 0.01697(11) 0.0326(5) Uani 1 1 d . . . N2 N 0.23455(17) 0.25343(14) 0.08907(11) 0.0323(5) Uani 1 1 d . . . N3 N 0.43545(17) 0.33616(14) 0.16715(11) 0.0308(5) Uani 1 1 d . . . N4 N 0.45821(18) 0.15977(14) 0.18988(11) 0.0343(5) Uani 1 1 d . . . C1 C 0.3316(2) 0.16799(18) 0.01921(13) 0.0356(6) Uani 1 1 d . . . C2 C 0.2453(2) 0.16884(18) 0.05427(13) 0.0345(6) Uani 1 1 d . . . C3 C 0.1851(3) 0.09180(19) 0.06105(15) 0.0445(7) Uani 1 1 d . . . H3 H 0.1287 0.0938 0.0857 0.053 Uiso 1 1 calc R . . C4 C 0.2066(3) 0.0118(2) 0.03207(17) 0.0532(8) Uani 1 1 d . . . H4 H 0.1639 -0.0408 0.0356 0.064 Uiso 1 1 calc R . . C5 C 0.2906(3) 0.0094(2) -0.00184(17) 0.0563(9) Uani 1 1 d . . . H5 H 0.3062 -0.0456 -0.0213 0.068 Uiso 1 1 calc R . . C6 C 0.3530(3) 0.0856(2) -0.00832(15) 0.0457(7) Uani 1 1 d . . . H6 H 0.411 0.0819 -0.0317 0.055 Uiso 1 1 calc R . . C7 C 0.4840(2) 0.2537(2) -0.01455(14) 0.0407(7) Uani 1 1 d . . . H7A H 0.5207 0.1936 -0.0103 0.049 Uiso 1 1 calc R . . H7B H 0.5429 0.2962 0.0125 0.049 Uiso 1 1 calc R . . C8 C 0.4536(3) 0.2821(2) -0.09016(15) 0.0483(8) Uani 1 1 d . . . C9 C 0.5659(3) 0.2762(3) -0.11156(19) 0.0697(11) Uani 1 1 d . . . H9A H 0.5947 0.2142 -0.1061 0.105 Uiso 1 1 calc R . . H9B H 0.6244 0.3162 -0.0826 0.105 Uiso 1 1 calc R . . H9C H 0.5503 0.2943 -0.1597 0.105 Uiso 1 1 calc R . . C10 C 0.4082(3) 0.3786(2) -0.09878(18) 0.0608(9) Uani 1 1 d . . . H10A H 0.3362 0.3822 -0.0852 0.091 Uiso 1 1 calc R . . H10B H 0.3927 0.3968 -0.1469 0.091 Uiso 1 1 calc R . . H10C H 0.4664 0.4188 -0.0697 0.091 Uiso 1 1 calc R . . C11 C 0.3605(3) 0.2206(3) -0.13651(16) 0.0619(10) Uani 1 1 d . . . H11A H 0.3882 0.1584 -0.1318 0.093 Uiso 1 1 calc R . . H11B H 0.3453 0.2397 -0.1844 0.093 Uiso 1 1 calc R . . H11C H 0.2887 0.2248 -0.1228 0.093 Uiso 1 1 calc R . . C12 C 0.1135(2) 0.2848(2) 0.08529(14) 0.0375(7) Uani 1 1 d . . . H12A H 0.1206 0.3436 0.109 0.045 Uiso 1 1 calc R . . H12B H 0.0808 0.242 0.1122 0.045 Uiso 1 1 calc R . . C13 C 0.0232(2) 0.2958(2) 0.01406(14) 0.0395(7) Uani 1 1 d . . . C14 C 0.0776(2) 0.3207(2) -0.04262(15) 0.0481(8) Uani 1 1 d . . . H14A H 0.1246 0.3752 -0.0295 0.072 Uiso 1 1 calc R . . H14B H 0.0162 0.3317 -0.0853 0.072 Uiso 1 1 calc R . . H14C H 0.1271 0.2713 -0.0495 0.072 Uiso 1 1 calc R . . C15 C -0.0575(3) 0.3720(2) 0.02199(18) 0.0589(9) Uani 1 1 d . . . H15A H -0.0123 0.4273 0.0353 0.088 Uiso 1 1 calc R . . H15B H -0.0948 0.356 0.0575 0.088 Uiso 1 1 calc R . . H15C H -0.1171 0.3815 -0.0217 0.088 Uiso 1 1 calc R . . C16 C -0.0505(3) 0.2108(2) -0.00706(18) 0.0568(9) Uani 1 1 d . . . H16A H -0.0856 0.1943 0.0293 0.085 Uiso 1 1 calc R . . H16B H -0.0012 0.1614 -0.0143 0.085 Uiso 1 1 calc R . . H16C H -0.1119 0.2222 -0.0497 0.085 Uiso 1 1 calc R . . C17 C 0.5471(2) 0.29596(18) 0.16698(13) 0.0327(6) Uani 1 1 d . . . C18 C 0.5547(2) 0.20203(18) 0.17727(13) 0.0345(6) Uani 1 1 d . . . C19 C 0.6557(2) 0.1593(2) 0.17168(15) 0.0431(7) Uani 1 1 d . . . H19 H 0.6643 0.0963 0.1786 0.052 Uiso 1 1 calc R . . C20 C 0.7427(3) 0.2082(2) 0.15624(16) 0.0490(8) Uani 1 1 d . . . H20 H 0.8105 0.1781 0.1527 0.059 Uiso 1 1 calc R . . C21 C 0.7334(2) 0.2997(2) 0.14591(15) 0.0471(8) Uani 1 1 d . . . H21 H 0.7946 0.3324 0.1359 0.057 Uiso 1 1 calc R . . C22 C 0.6339(2) 0.3438(2) 0.15026(14) 0.0391(7) Uani 1 1 d . . . H22 H 0.6254 0.4066 0.1418 0.047 Uiso 1 1 calc R . . C23 C 0.4410(2) 0.42529(18) 0.20327(13) 0.0360(6) Uani 1 1 d . . . H23A H 0.3604 0.443 0.2007 0.043 Uiso 1 1 calc R . . H23B H 0.4709 0.4703 0.1766 0.043 Uiso 1 1 calc R . . C24 C 0.5144(2) 0.4336(2) 0.27952(14) 0.0414(7) Uani 1 1 d . . . C25 C 0.6409(3) 0.4583(2) 0.28644(16) 0.0546(8) Uani 1 1 d . . . H25A H 0.6779 0.4095 0.268 0.082 Uiso 1 1 calc R . . H25B H 0.6823 0.4675 0.335 0.082 Uiso 1 1 calc R . . H25C H 0.6434 0.5137 0.2608 0.082 Uiso 1 1 calc R . . C26 C 0.5162(4) 0.3487(3) 0.32083(18) 0.0752(12) Uani 1 1 d . . . H26A H 0.5504 0.2996 0.3008 0.113 Uiso 1 1 calc R . . H26B H 0.4367 0.3326 0.3201 0.113 Uiso 1 1 calc R . . H26C H 0.5628 0.3587 0.3684 0.113 Uiso 1 1 calc R . . C27 C 0.4622(3) 0.5114(3) 0.3088(2) 0.0881(15) Uani 1 1 d . . . H27A H 0.4618 0.5653 0.281 0.132 Uiso 1 1 calc R . . H27B H 0.5088 0.5228 0.3561 0.132 Uiso 1 1 calc R . . H27C H 0.3825 0.4965 0.3082 0.132 Uiso 1 1 calc R . . C28 C 0.4538(2) 0.06119(18) 0.19237(14) 0.0394(7) Uani 1 1 d . . . H28A H 0.5052 0.037 0.1662 0.047 Uiso 1 1 calc R . . H28B H 0.3736 0.042 0.1682 0.047 Uiso 1 1 calc R . . C29 C 0.4886(2) 0.01701(19) 0.26405(14) 0.0392(7) Uani 1 1 d . . . C30 C 0.6096(2) 0.0455(2) 0.30701(16) 0.0470(7) Uani 1 1 d . . . H30A H 0.6111 0.1106 0.3143 0.07 Uiso 1 1 calc R . . H30B H 0.6667 0.0294 0.2828 0.07 Uiso 1 1 calc R . . H30C H 0.6288 0.0146 0.3515 0.07 Uiso 1 1 calc R . . C31 C 0.4852(3) -0.0847(2) 0.25283(18) 0.0586(9) Uani 1 1 d . . . H31A H 0.5419 -0.1014 0.2285 0.088 Uiso 1 1 calc R . . H31B H 0.4073 -0.1026 0.2255 0.088 Uiso 1 1 calc R . . H31C H 0.5044 -0.1154 0.2973 0.088 Uiso 1 1 calc R . . C32 C 0.3996(3) 0.0412(2) 0.30248(16) 0.0502(8) Uani 1 1 d . . . H32A H 0.4007 0.1063 0.3101 0.075 Uiso 1 1 calc R . . H32B H 0.4194 0.01 0.3468 0.075 Uiso 1 1 calc R . . H32C H 0.3219 0.0228 0.2751 0.075 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 0.0307(4) 0.0286(4) 0.0343(4) 0.0007(3) 0.0131(3) -0.0027(3) Al2 0.0334(4) 0.0307(4) 0.0358(4) 0.0011(4) 0.0154(3) -0.0024(3) Cl1 0.0549(5) 0.0314(4) 0.0523(5) 0.0039(3) 0.0047(3) -0.0007(3) Cl2 0.0465(4) 0.0559(5) 0.0468(4) 0.0064(4) 0.0268(3) 0.0064(3) N1 0.0309(11) 0.0347(13) 0.0353(12) -0.0002(10) 0.0147(9) -0.0026(10) N2 0.0300(11) 0.0311(12) 0.0387(12) -0.0015(10) 0.0145(9) -0.0041(9) N3 0.0307(11) 0.0283(12) 0.0361(12) -0.0023(10) 0.0137(9) -0.0015(9) N4 0.0370(12) 0.0301(12) 0.0388(13) 0.0040(10) 0.0155(10) -0.0009(10) C1 0.0395(15) 0.0328(16) 0.0337(14) 0.0006(12) 0.0089(12) 0.0011(12) C2 0.0358(15) 0.0309(15) 0.0364(15) -0.0027(12) 0.0096(12) -0.0039(12) C3 0.0483(17) 0.0400(18) 0.0444(17) 0.0008(14) 0.0120(13) -0.0112(14) C4 0.066(2) 0.0326(17) 0.059(2) -0.0043(15) 0.0140(17) -0.0148(15) C5 0.075(2) 0.0327(17) 0.057(2) -0.0071(15) 0.0110(18) -0.0002(16) C6 0.0512(18) 0.0418(18) 0.0460(17) -0.0077(14) 0.0166(14) 0.0019(14) C7 0.0313(15) 0.0524(18) 0.0409(16) -0.0087(14) 0.0145(12) -0.0038(13) C8 0.0441(17) 0.064(2) 0.0434(17) -0.0054(15) 0.0233(14) -0.0135(15) C9 0.059(2) 0.101(3) 0.064(2) -0.014(2) 0.0415(18) -0.016(2) C10 0.065(2) 0.070(2) 0.0522(19) 0.0104(18) 0.0243(16) -0.0084(18) C11 0.063(2) 0.086(3) 0.0383(17) -0.0055(17) 0.0167(16) -0.0212(19) C12 0.0330(15) 0.0417(16) 0.0417(16) -0.0022(13) 0.0167(12) -0.0027(12) C13 0.0327(15) 0.0435(17) 0.0431(16) -0.0017(13) 0.0119(12) -0.0031(13) C14 0.0393(16) 0.064(2) 0.0402(16) 0.0021(15) 0.0099(13) -0.0040(15) C15 0.0496(19) 0.066(2) 0.059(2) -0.0018(18) 0.0134(16) 0.0123(16) C16 0.0457(18) 0.058(2) 0.061(2) 0.0002(17) 0.0058(15) -0.0157(16) C17 0.0309(14) 0.0366(16) 0.0324(14) 0.0012(12) 0.0120(11) 0.0001(12) C18 0.0351(15) 0.0384(16) 0.0321(14) 0.0030(12) 0.0130(11) 0.0008(12) C19 0.0428(17) 0.0433(17) 0.0484(17) 0.0046(14) 0.0212(14) 0.0067(14) C20 0.0372(16) 0.063(2) 0.0530(18) 0.0028(16) 0.0233(14) 0.0089(15) C21 0.0353(16) 0.061(2) 0.0500(18) -0.0025(16) 0.0205(13) -0.0071(14) C22 0.0371(15) 0.0417(17) 0.0400(15) -0.0025(13) 0.0132(12) -0.0090(13) C23 0.0382(15) 0.0339(15) 0.0375(15) -0.0046(12) 0.0132(12) -0.0016(12) C24 0.0436(16) 0.0446(17) 0.0372(15) -0.0066(13) 0.0137(13) -0.0055(13) C25 0.0451(18) 0.066(2) 0.0464(18) -0.0067(16) 0.0033(14) -0.0066(16) C26 0.095(3) 0.080(3) 0.0445(19) 0.0042(19) 0.0106(19) -0.032(2) C27 0.061(2) 0.122(4) 0.070(2) -0.053(3) -0.0002(19) 0.025(2) C28 0.0424(16) 0.0307(15) 0.0442(16) 0.0000(13) 0.0107(13) -0.0018(12) C29 0.0399(16) 0.0347(16) 0.0424(16) 0.0064(13) 0.0106(13) 0.0005(12) C30 0.0437(17) 0.0495(19) 0.0470(17) 0.0053(15) 0.0117(14) 0.0027(14) C31 0.074(2) 0.0361(18) 0.062(2) 0.0097(16) 0.0130(17) -0.0012(16) C32 0.0442(17) 0.056(2) 0.0513(18) 0.0119(16) 0.0156(14) 0.0001(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.812(2) . ? Al1 N2 1.925(2) . ? Al1 N3 1.977(2) . ? Al1 Cl1 2.1069(10) . ? Al1 Al2 2.7208(11) . ? Al2 N4 1.811(2) . ? Al2 N3 1.920(2) . ? Al2 N2 1.973(2) . ? Al2 Cl2 2.1047(10) . ? N1 C1 1.398(3) . ? N1 C7 1.471(3) . ? N2 C2 1.467(3) . ? N2 C12 1.507(3) . ? N3 C17 1.470(3) . ? N3 C23 1.508(3) . ? N4 C18 1.405(3) . ? N4 C28 1.469(3) . ? C1 C6 1.401(4) . ? C1 C2 1.415(4) . ? C2 C3 1.383(4) . ? C3 C4 1.384(4) . ? C4 C5 1.374(5) . ? C5 C6 1.385(4) . ? C7 C8 1.534(4) . ? C8 C10 1.529(5) . ? C8 C9 1.532(4) . ? C8 C11 1.541(4) . ? C12 C13 1.551(4) . ? C13 C14 1.522(4) . ? C13 C15 1.530(4) . ? C13 C16 1.533(4) . ? C17 C22 1.381(4) . ? C17 C18 1.412(4) . ? C18 C19 1.402(4) . ? C19 C20 1.381(4) . ? C20 C21 1.376(4) . ? C21 C22 1.388(4) . ? C23 C24 1.554(4) . ? C24 C26 1.513(5) . ? C24 C27 1.516(4) . ? C24 C25 1.530(4) . ? C28 C29 1.543(4) . ? C29 C30 1.527(4) . ? C29 C31 1.529(4) . ? C29 C32 1.535(4) . ? 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 N2 90.71(10) . . ? N1 Al1 N3 115.69(10) . . ? N2 Al1 N3 90.47(9) . . ? N1 Al1 Cl1 124.87(8) . . ? N2 Al1 Cl1 123.95(8) . . ? N3 Al1 Cl1 106.25(7) . . ? N1 Al1 Al2 101.96(8) . . ? N2 Al1 Al2 46.47(7) . . ? N3 Al1 Al2 44.87(6) . . ? Cl1 Al1 Al2 133.16(4) . . ? N4 Al2 N3 91.10(9) . . ? N4 Al2 N2 115.28(10) . . ? N3 Al2 N2 90.74(9) . . ? N4 Al2 Cl2 123.83(8) . . ? N3 Al2 Cl2 125.20(7) . . ? N2 Al2 Cl2 106.32(7) . . ? N4 Al2 Al1 101.95(7) . . ? N3 Al2 Al1 46.59(7) . . ? N2 Al2 Al1 45.01(6) . . ? Cl2 Al2 Al1 134.21(4) . . ? C1 N1 C7 119.8(2) . . ? C1 N1 Al1 111.58(17) . . ? C7 N1 Al1 127.68(18) . . ? C2 N2 C12 117.2(2) . . ? C2 N2 Al1 105.98(15) . . ? C12 N2 Al1 120.69(17) . . ? C2 N2 Al2 104.35(15) . . ? C12 N2 Al2 115.66(16) . . ? Al1 N2 Al2 88.52(9) . . ? C17 N3 C23 116.41(19) . . ? C17 N3 Al2 106.09(16) . . ? C23 N3 Al2 122.03(16) . . ? C17 N3 Al1 103.32(15) . . ? C23 N3 Al1 115.89(16) . . ? Al2 N3 Al1 88.53(9) . . ? C18 N4 C28 119.5(2) . . ? C18 N4 Al2 110.98(17) . . ? C28 N4 Al2 128.07(18) . . ? N1 C1 C6 127.0(3) . . ? N1 C1 C2 116.1(2) . . ? C6 C1 C2 116.9(3) . . ? C3 C2 C1 121.4(3) . . ? C3 C2 N2 122.9(2) . . ? C1 C2 N2 115.3(2) . . ? C2 C3 C4 120.3(3) . . ? C5 C4 C3 119.2(3) . . ? C4 C5 C6 121.4(3) . . ? C5 C6 C1 120.8(3) . . ? N1 C7 C8 117.0(2) . . ? C10 C8 C9 109.6(3) . . ? C10 C8 C7 110.4(3) . . ? C9 C8 C7 106.9(3) . . ? C10 C8 C11 108.3(3) . . ? C9 C8 C11 109.7(3) . . ? C7 C8 C11 112.0(3) . . ? N2 C12 C13 119.3(2) . . ? C14 C13 C15 108.7(3) . . ? C14 C13 C16 109.1(3) . . ? C15 C13 C16 107.9(2) . . ? C14 C13 C12 113.2(2) . . ? C15 C13 C12 106.0(2) . . ? C16 C13 C12 111.7(2) . . ? C22 C17 C18 121.7(2) . . ? C22 C17 N3 122.9(2) . . ? C18 C17 N3 115.0(2) . . ? C19 C18 N4 126.1(3) . . ? C19 C18 C17 117.2(2) . . ? N4 C18 C17 116.6(2) . . ? C20 C19 C18 120.5(3) . . ? C21 C20 C19 121.4(3) . . ? C20 C21 C22 119.4(3) . . ? C17 C22 C21 119.7(3) . . ? N3 C23 C24 119.3(2) . . ? C26 C24 C27 111.3(3) . . ? C26 C24 C25 107.0(3) . . ? C27 C24 C25 106.9(3) . . ? C26 C24 C23 113.7(2) . . ? C27 C24 C23 105.7(2) . . ? C25 C24 C23 112.2(2) . . ? N4 C28 C29 117.1(2) . . ? C30 C29 C31 109.9(2) . . ? C30 C29 C32 109.4(2) . . ? C31 C29 C32 108.4(3) . . ? C30 C29 C28 112.3(2) . . ? C31 C29 C28 107.0(2) . . ? C32 C29 C28 109.8(2) . . ? #===END data_lappert-10 _database_code_CSD 202064 _audit_creation_date 2000-03-31T15:06:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [C6H4{NH(CH2tBu)(AlMe3)}2] _chemical_formula_moiety 'C22 H46 Al2 N2' _chemical_formula_structural 'C22 H46 AL2 N2' _chemical_formula_sum 'C22 H46 Al2 N2' _chemical_formula_weight 392.57 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8445(2) _cell_length_b 10.7407(4) _cell_length_c 13.0190(4) _cell_angle_alpha 98.740(2) _cell_angle_beta 99.440(2) _cell_angle_gamma 97.884(2) _cell_volume 1323.50(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8407 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 0.985 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_T_min 0.9712 _exptl_absorpt_correction_T_max 0.9768 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 13539 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 27.85 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 6225 _reflns_number_gt 5143 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0543P)^2^+0.6088P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 6225 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.299 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.044 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.19159(5) 0.23568(4) 0.85936(4) 0.02793(13) Uani 1 1 d . . . Al2 Al 0.39570(5) -0.33717(4) 0.67484(4) 0.02757(13) Uani 1 1 d . . . N1 N 0.35274(12) 0.18878(11) 0.78267(9) 0.0236(3) Uani 1 1 d . . . H1 H 0.3782 0.2576 0.7504 0.028 Uiso 1 1 calc R . . N2 N 0.20407(13) -0.27385(11) 0.65936(9) 0.0245(3) Uani 1 1 d . . . H2 H 0.149 -0.3245 0.5985 0.029 Uiso 1 1 calc R . . C1 C 0.30140(14) 0.08005(13) 0.69741(11) 0.0230(3) Uani 1 1 d . . . C2 C 0.27696(14) -0.04234(14) 0.71977(11) 0.0236(3) Uani 1 1 d . . . H2' H 0.2993 -0.0564 0.7904 0.028 Uiso 1 1 calc R . . C3 C 0.21963(15) -0.14406(13) 0.63816(11) 0.0238(3) Uani 1 1 d . . . C4 C 0.18583(18) -0.12446(15) 0.53463(12) 0.0317(3) Uani 1 1 d . . . H4 H 0.1458 -0.1943 0.479 0.038 Uiso 1 1 calc R . . C5 C 0.2113(2) -0.00158(16) 0.51351(12) 0.0358(4) Uani 1 1 d . . . H5 H 0.189 0.0124 0.4428 0.043 Uiso 1 1 calc R . . C6 C 0.26892(17) 0.10107(15) 0.59400(12) 0.0306(3) Uani 1 1 d . . . H6 H 0.2861 0.1849 0.5788 0.037 Uiso 1 1 calc R . . C7 C 0.47963(15) 0.18062(15) 0.86144(12) 0.0272(3) Uani 1 1 d . . . H7A H 0.4657 0.0959 0.883 0.033 Uiso 1 1 calc R . . H7B H 0.4852 0.2458 0.9252 0.033 Uiso 1 1 calc R . . C8 C 0.62080(16) 0.19892(15) 0.82521(13) 0.0298(3) Uani 1 1 d . . . C9 C 0.64426(19) 0.32405(19) 0.78471(17) 0.0455(4) Uani 1 1 d . . . H9A H 0.6362 0.3946 0.8395 0.068 Uiso 1 1 calc R . . H9B H 0.574 0.3209 0.7212 0.068 Uiso 1 1 calc R . . H9C H 0.7377 0.3374 0.7673 0.068 Uiso 1 1 calc R . . C10 C 0.73191(19) 0.2051(2) 0.92426(16) 0.0473(5) Uani 1 1 d . . . H10A H 0.7176 0.1247 0.951 0.071 Uiso 1 1 calc R . . H10B H 0.7241 0.276 0.9788 0.071 Uiso 1 1 calc R . . H10C H 0.825 0.2185 0.9062 0.071 Uiso 1 1 calc R . . C11 C 0.6336(2) 0.0880(2) 0.74080(18) 0.0536(6) Uani 1 1 d . . . H11A H 0.6182 0.0078 0.7676 0.08 Uiso 1 1 calc R . . H11B H 0.7273 0.1009 0.7236 0.08 Uiso 1 1 calc R . . H11C H 0.5637 0.0842 0.677 0.08 Uiso 1 1 calc R . . C12 C 0.1641(2) 0.10170(18) 0.94556(15) 0.0430(4) Uani 1 1 d . . . H12A H 0.2449 0.113 1.0032 0.064 Uiso 1 1 calc R . . H12B H 0.1543 0.0175 0.9011 0.064 Uiso 1 1 calc R . . H12C H 0.0795 0.1079 0.9752 0.064 Uiso 1 1 calc R . . C13 C 0.04011(18) 0.2306(2) 0.73812(15) 0.0428(4) Uani 1 1 d . . . H13A H 0.0643 0.3009 0.7009 0.064 Uiso 1 1 calc R . . H13B H -0.0469 0.2395 0.7637 0.064 Uiso 1 1 calc R . . H13C H 0.0278 0.149 0.6896 0.064 Uiso 1 1 calc R . . C14 C 0.2710(2) 0.40910(16) 0.93898(14) 0.0402(4) Uani 1 1 d . . . H14A H 0.2805 0.4683 0.8893 0.06 Uiso 1 1 calc R . . H14B H 0.363 0.408 0.9809 0.06 Uiso 1 1 calc R . . H14C H 0.2089 0.437 0.9863 0.06 Uiso 1 1 calc R . . C15 C 0.13159(16) -0.30030(15) 0.74812(12) 0.0278(3) Uani 1 1 d . . . H15A H 0.1626 -0.2267 0.8071 0.033 Uiso 1 1 calc R . . H15B H 0.1631 -0.3758 0.7736 0.033 Uiso 1 1 calc R . . C16 C -0.02886(17) -0.32483(16) 0.72315(15) 0.0358(4) Uani 1 1 d . . . C17 C -0.0870(2) -0.2066(2) 0.6965(2) 0.0685(7) Uani 1 1 d . . . H17A H -0.051 -0.1346 0.755 0.103 Uiso 1 1 calc R . . H17B H -0.1892 -0.2237 0.6856 0.103 Uiso 1 1 calc R . . H17C H -0.0582 -0.1854 0.6318 0.103 Uiso 1 1 calc R . . C18 C -0.0751(2) -0.3582(2) 0.82371(18) 0.0539(5) Uani 1 1 d . . . H18A H -0.0414 -0.2856 0.882 0.081 Uiso 1 1 calc R . . H18B H -0.0362 -0.433 0.8419 0.081 Uiso 1 1 calc R . . H18C H -0.1773 -0.3774 0.8116 0.081 Uiso 1 1 calc R . . C19 C -0.0826(2) -0.4386(2) 0.63368(18) 0.0593(6) Uani 1 1 d . . . H19A H -0.0443 -0.5134 0.6526 0.089 Uiso 1 1 calc R . . H19B H -0.0532 -0.4188 0.5688 0.089 Uiso 1 1 calc R . . H19C H -0.1848 -0.4569 0.6221 0.089 Uiso 1 1 calc R . . C20 C 0.3309(2) -0.52388(16) 0.65047(15) 0.0404(4) Uani 1 1 d . . . H20A H 0.2917 -0.5465 0.711 0.061 Uiso 1 1 calc R . . H20B H 0.4099 -0.5686 0.6423 0.061 Uiso 1 1 calc R . . H20C H 0.2591 -0.549 0.5861 0.061 Uiso 1 1 calc R . . C21 C 0.4890(2) -0.26346(19) 0.82119(14) 0.0427(4) Uani 1 1 d . . . H21A H 0.4379 -0.3015 0.8704 0.064 Uiso 1 1 calc R . . H21B H 0.4909 -0.1709 0.8334 0.064 Uiso 1 1 calc R . . H21C H 0.5848 -0.2813 0.8327 0.064 Uiso 1 1 calc R . . C22 C 0.4775(2) -0.2771(2) 0.55973(16) 0.0462(5) Uani 1 1 d . . . H22A H 0.4211 -0.3211 0.4915 0.069 Uiso 1 1 calc R . . H22B H 0.573 -0.2954 0.5648 0.069 Uiso 1 1 calc R . . H22C H 0.4793 -0.1849 0.5655 0.069 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 0.0286(2) 0.0265(2) 0.0293(2) 0.00216(18) 0.00910(18) 0.00543(18) Al2 0.0307(2) 0.0269(2) 0.0280(2) 0.00669(18) 0.00856(18) 0.00903(18) N1 0.0266(6) 0.0198(6) 0.0245(6) 0.0041(5) 0.0051(5) 0.0035(5) N2 0.0294(6) 0.0197(6) 0.0240(6) 0.0033(5) 0.0046(5) 0.0042(5) C1 0.0249(7) 0.0219(7) 0.0231(7) 0.0025(5) 0.0065(5) 0.0059(5) C2 0.0257(7) 0.0246(7) 0.0217(7) 0.0055(5) 0.0052(5) 0.0065(5) C3 0.0265(7) 0.0205(7) 0.0256(7) 0.0048(5) 0.0052(5) 0.0068(5) C4 0.0444(9) 0.0249(8) 0.0235(7) 0.0011(6) 0.0011(6) 0.0082(6) C5 0.0561(11) 0.0306(8) 0.0218(7) 0.0079(6) 0.0038(7) 0.0119(7) C6 0.0436(9) 0.0237(7) 0.0277(8) 0.0080(6) 0.0093(6) 0.0094(6) C7 0.0271(7) 0.0282(8) 0.0256(7) 0.0040(6) 0.0033(6) 0.0048(6) C8 0.0266(7) 0.0282(8) 0.0334(8) 0.0024(6) 0.0051(6) 0.0042(6) C9 0.0338(9) 0.0457(11) 0.0591(12) 0.0200(9) 0.0098(8) 0.0009(8) C10 0.0302(9) 0.0622(13) 0.0487(11) 0.0142(9) -0.0011(8) 0.0101(8) C11 0.0354(10) 0.0513(12) 0.0678(14) -0.0171(10) 0.0198(9) 0.0035(8) C12 0.0548(11) 0.0364(10) 0.0420(10) 0.0086(8) 0.0225(8) 0.0044(8) C13 0.0283(8) 0.0523(11) 0.0468(10) 0.0062(8) 0.0057(7) 0.0086(7) C14 0.0531(11) 0.0291(9) 0.0382(9) 0.0000(7) 0.0119(8) 0.0091(7) C15 0.0310(8) 0.0253(7) 0.0287(7) 0.0062(6) 0.0085(6) 0.0044(6) C16 0.0298(8) 0.0321(9) 0.0474(10) 0.0083(7) 0.0114(7) 0.0054(6) C17 0.0368(11) 0.0625(15) 0.121(2) 0.0416(15) 0.0217(12) 0.0228(10) C18 0.0461(11) 0.0582(13) 0.0616(13) 0.0103(10) 0.0286(10) 0.0019(9) C19 0.0421(11) 0.0660(15) 0.0569(13) -0.0049(11) 0.0049(9) -0.0125(10) C20 0.0535(11) 0.0273(8) 0.0449(10) 0.0083(7) 0.0131(8) 0.0157(7) C21 0.0393(10) 0.0470(11) 0.0384(9) 0.0067(8) -0.0023(7) 0.0076(8) C22 0.0492(11) 0.0534(12) 0.0457(10) 0.0153(9) 0.0252(9) 0.0156(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C12 1.9714(19) . ? Al1 C13 1.9744(19) . ? Al1 C14 1.9756(18) . ? Al1 N1 2.0864(13) . ? Al2 C22 1.9641(19) . ? Al2 C21 1.9670(18) . ? Al2 C20 1.9794(18) . ? Al2 N2 2.0811(13) . ? N1 C1 1.4532(17) . ? N1 C7 1.5022(18) . ? N2 C3 1.4544(18) . ? N2 C15 1.4967(19) . ? C1 C2 1.387(2) . ? C1 C6 1.392(2) . ? C2 C3 1.386(2) . ? C3 C4 1.389(2) . ? C4 C5 1.387(2) . ? C5 C6 1.385(2) . ? C7 C8 1.537(2) . ? C8 C9 1.519(2) . ? C8 C11 1.527(2) . ? C8 C10 1.535(2) . ? C15 C16 1.537(2) . ? C16 C19 1.522(3) . ? C16 C17 1.526(3) . ? C16 C18 1.531(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 C12 Al1 C13 116.19(9) . . ? C12 Al1 C14 115.78(8) . . ? C13 Al1 C14 114.30(9) . . ? C12 Al1 N1 104.05(7) . . ? C13 Al1 N1 101.43(7) . . ? C14 Al1 N1 102.10(7) . . ? C22 Al2 C21 117.87(9) . . ? C22 Al2 C20 114.20(9) . . ? C21 Al2 C20 114.11(8) . . ? C22 Al2 N2 103.44(7) . . ? C21 Al2 N2 104.32(7) . . ? C20 Al2 N2 99.84(7) . . ? C1 N1 C7 117.07(11) . . ? C1 N1 Al1 110.42(9) . . ? C7 N1 Al1 110.75(9) . . ? C3 N2 C15 117.34(11) . . ? C3 N2 Al2 110.34(9) . . ? C15 N2 Al2 111.05(9) . . ? C2 C1 C6 120.47(13) . . ? C2 C1 N1 120.22(12) . . ? C6 C1 N1 119.19(13) . . ? C3 C2 C1 119.47(13) . . ? C2 C3 C4 120.71(13) . . ? C2 C3 N2 119.90(12) . . ? C4 C3 N2 119.24(13) . . ? C5 C4 C3 119.12(14) . . ? C6 C5 C4 120.94(14) . . ? C5 C6 C1 119.28(14) . . ? N1 C7 C8 116.90(12) . . ? C9 C8 C11 110.07(16) . . ? C9 C8 C10 108.88(14) . . ? C11 C8 C10 109.08(16) . . ? C9 C8 C7 110.61(13) . . ? C11 C8 C7 112.32(13) . . ? C10 C8 C7 105.74(13) . . ? N2 C15 C16 116.67(13) . . ? C19 C16 C17 110.9(2) . . ? C19 C16 C18 108.57(16) . . ? C17 C16 C18 109.31(18) . . ? C19 C16 C15 110.39(15) . . ? C17 C16 C15 111.64(15) . . ? C18 C16 C15 105.86(15) . . ? #===END