Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Vincenzo Passarelli' _publ_contact_author_address ; Corso Stati Uniti 4 ICIS-CNR Padova 35127 ITALY ; _publ_contact_author_email PASSARELLI@ICIS.CNR.IT _publ_section_title ; Solution dynamics and molecular structure elucidation of novel aluminium derivatives containing diaminodimethylsilane ligands ; loop_ _publ_author_name 'Vincenzo Passarelli' 'Franco Benetollo' 'Pierino Zanella' data_new _database_code_depnum_ccdc_archive 'CCDC 229173' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety AlCl~2~[SiMe~2~(NC~4~H~8~)(NCH~2~CH~2~NMe~2~] _chemical_formula_sum 'C10 H24 Al Cl2 N3 Si' _chemical_formula_weight 312.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, y, -z+1/2' '-x, -y, -z' '-x, y-1/2, -z' 'x-1/2, -y-1/2, -z-1/2' '-x-1/2, -y, z-1/2' _cell_length_a 14.554(3) _cell_length_b 11.561(2) _cell_length_c 9.921(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1669.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.499 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_correction_T_min 0.984 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW1100' _diffrn_measurement_method \Q/2\Q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1348 _diffrn_reflns_av_R_equivalents 0.0057 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1341 _reflns_number_gt 1300 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+5.1121P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1341 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0913 _refine_ls_wR_factor_ref 0.1993 _refine_ls_wR_factor_gt 0.1975 _refine_ls_goodness_of_fit_ref 1.238 _refine_ls_restrained_S_all 1.238 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al Al 0.15852(15) 0.2500 0.4273(2) 0.0537(6) Uani 1 2 d S . 1 Si Si 0.34746(15) 0.2500 0.4493(2) 0.0676(8) Uani 1 2 d S . 1 N1 N 0.2809(4) 0.2500 0.2961(6) 0.0526(15) Uani 1 2 d S . 1 N2 N 0.2536(5) 0.2500 0.5446(7) 0.077(2) Uani 1 2 d S . 1 N3 N 0.0818(4) 0.2500 0.6104(7) 0.0633(18) Uani 1 2 d S . 1 Cl Cl 0.09375(15) 0.0981(2) 0.3446(2) 0.1231(10) Uani 1 1 d . . 1 C1 C 0.2941(5) 0.1507(6) 0.2027(6) 0.0777(18) Uani 1 1 d . . 1 H1A H 0.2679 0.0806 0.2402 0.093 Uiso 1 1 calc R . 1 H1B H 0.3588 0.1379 0.1850 0.093 Uiso 1 1 calc R . 1 C2 C 0.2443(5) 0.1853(7) 0.0751(7) 0.106(3) Uani 1 1 d . . 1 H2A H 0.2760 0.1557 -0.0037 0.127 Uiso 1 1 calc R . 1 H2B H 0.1820 0.1557 0.0752 0.127 Uiso 1 1 calc R . 1 C3 C 0.2387(7) 0.2078(11) 0.6905(11) 0.073(4) Uani 0.50 1 d P . 1 C5 C -0.0173(8) 0.282(4) 0.6047(14) 0.113(17) Uani 0.50 1 d P . 1 C6 C 0.0863(14) 0.3799(14) 0.6658(19) 0.102(6) Uani 0.50 1 d P . 1 C4 C 0.1340(11) 0.1736(13) 0.6986(13) 0.074(4) Uani 0.50 1 d P . 1 C7 C 0.4200(6) 0.1197(10) 0.4638(10) 0.147(4) Uani 1 1 d . . 1 H7A H 0.4377 0.1089 0.5562 0.176 Uiso 1 1 calc R . 1 H7B H 0.4740 0.1290 0.4093 0.176 Uiso 1 1 calc R . 1 H7C H 0.3861 0.0534 0.4335 0.176 Uiso 1 1 calc R . 1 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 0.0470(12) 0.0589(14) 0.0552(13) 0.000 -0.0056(11) 0.000 Si 0.0439(12) 0.098(2) 0.0612(14) 0.000 -0.0030(10) 0.000 N1 0.057(4) 0.052(3) 0.048(3) 0.000 -0.001(3) 0.000 N2 0.050(4) 0.136(7) 0.046(4) 0.000 0.001(3) 0.000 N3 0.055(4) 0.068(4) 0.066(4) 0.000 0.009(3) 0.000 Cl 0.1145(16) 0.145(2) 0.1095(16) -0.0557(15) 0.0234(13) -0.0737(15) C1 0.074(4) 0.082(4) 0.077(4) -0.021(4) 0.010(3) 0.000(4) C2 0.089(5) 0.163(8) 0.065(4) -0.027(4) 0.000(4) -0.014(5) C3 0.050(6) 0.108(12) 0.061(6) 0.002(6) -0.004(5) 0.007(6) C5 0.049(5) 0.20(5) 0.089(8) -0.009(13) 0.013(6) 0.015(12) C6 0.140(16) 0.060(10) 0.106(14) -0.020(9) 0.034(12) 0.028(10) C4 0.094(10) 0.077(10) 0.050(7) 0.026(7) 0.020(7) 0.016(8) C7 0.130(7) 0.199(11) 0.111(7) 0.008(7) -0.021(6) 0.096(8) _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 1.808(7) . ? Al N3 2.132(7) . ? Al Cl 2.156(2) . ? Al Cl 2.156(2) 2 ? Al N1 2.206(7) . ? Al Si 2.758(3) . ? Si N2 1.662(7) . ? Si N1 1.802(6) . ? Si C7 1.846(6) 2 ? Si C7 1.846(6) . ? N1 C1 1.488(7) . ? N1 C1 1.488(7) 2 ? N2 C3 1.542(12) 2 ? N2 C3 1.542(12) . ? N3 C4 1.456(14) 2 ? N3 C4 1.456(14) . ? N3 C5 1.490(17) 2 ? N3 C5 1.490(17) . ? N3 C6 1.600(16) . ? N3 C6 1.600(16) 2 ? C1 C2 1.512(9) . ? C2 C2 1.496(17) 2 ? C3 C3 0.98(3) 2 ? C3 C4 1.58(2) . ? C5 C5 0.73(9) 2 ? C5 C6 1.98(3) . ? C6 C4 0.984(19) 2 ? C4 C6 0.984(19) 2 ? C4 C4 1.77(3) 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 N3 81.5(3) . . ? N2 Al Cl 125.42(9) . . ? N3 Al Cl 95.47(14) . . ? N2 Al Cl 125.42(9) . 2 ? N3 Al Cl 95.47(14) . 2 ? Cl Al Cl 109.14(18) . 2 ? N2 Al N1 76.2(3) . . ? N3 Al N1 157.7(3) . . ? Cl Al N1 97.38(13) . . ? Cl Al N1 97.38(13) 2 . ? N2 Al Si 35.6(2) . . ? N3 Al Si 117.0(2) . . ? Cl Al Si 117.77(9) . . ? Cl Al Si 117.77(9) 2 . ? N1 Al Si 40.68(17) . . ? N2 Si N1 92.2(3) . . ? N2 Si C7 115.2(3) . 2 ? N1 Si C7 111.9(3) . 2 ? N2 Si C7 115.2(3) . . ? N1 Si C7 111.9(3) . . ? C7 Si C7 109.4(7) 2 . ? N2 Si Al 39.2(2) . . ? N1 Si Al 53.0(2) . . ? C7 Si Al 125.2(3) 2 . ? C7 Si Al 125.2(3) . . ? C1 N1 C1 101.0(7) . 2 ? C1 N1 Si 117.2(4) . . ? C1 N1 Si 117.2(4) 2 . ? C1 N1 Al 118.1(4) . . ? C1 N1 Al 118.1(4) 2 . ? Si N1 Al 86.4(3) . . ? C3 N2 C3 36.9(10) 2 . ? C3 N2 Si 130.5(6) 2 . ? C3 N2 Si 130.5(6) . . ? C3 N2 Al 119.8(6) 2 . ? C3 N2 Al 119.8(6) . . ? Si N2 Al 105.2(4) . . ? C4 N3 C4 74.6(15) 2 . ? C4 N3 C5 132.6(13) 2 2 ? C4 N3 C5 112.2(16) . 2 ? C4 N3 C5 112.2(15) 2 . ? C4 N3 C5 132.6(13) . . ? C5 N3 C5 29(3) 2 . ? C4 N3 C6 37.2(8) 2 . ? C4 N3 C6 109.9(13) . . ? C5 N3 C6 106.5(18) 2 . ? C5 N3 C6 79.7(18) . . ? C4 N3 C6 109.9(13) 2 2 ? C4 N3 C6 37.2(8) . 2 ? C5 N3 C6 79.7(18) 2 2 ? C5 N3 C6 106.5(18) . 2 ? C6 N3 C6 139.5(15) . 2 ? C4 N3 Al 103.8(6) 2 . ? C4 N3 Al 103.8(6) . . ? C5 N3 Al 118.3(7) 2 . ? C5 N3 Al 118.3(7) . . ? C6 N3 Al 105.7(7) . . ? C6 N3 Al 105.7(7) 2 . ? N1 C1 C2 104.8(6) . . ? C2 C2 C1 105.3(4) 2 . ? C3 C3 N2 71.6(5) 2 . ? C3 C3 C4 104.5(7) 2 . ? N2 C3 C4 105.2(8) . . ? C5 C5 N3 75.7(17) 2 . ? C5 C5 C6 124.9(12) 2 . ? N3 C5 C6 52.6(8) . . ? C4 C6 N3 63.4(12) 2 . ? C4 C6 C5 106.1(19) 2 . ? N3 C6 C5 47.7(12) . . ? C6 C4 N3 79.4(15) 2 . ? C6 C4 C3 145.2(19) 2 . ? N3 C4 C3 108.7(10) . . ? C6 C4 C4 128.9(15) 2 2 ? N3 C4 C4 52.7(7) . 2 ? C3 C4 C4 75.5(7) . 2 ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 0.427 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.067