# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'ProfD Norbert Mitzel' _publ_contact_author_email MITZEL@UNI-MUENSTER.DE _publ_section_title ; Organoaluminium and -gallium complexes with ?-NH-functional alkoxide ligands ; loop_ _publ_author_name 'Norbert Mitzel' 'Alexander Hepp' 'Alexander Willner' # Attachment 'merged.cif' data_2d _database_code_depnum_ccdc_archive 'CCDC 694707' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-{mu2-O-[2-(tert.-butylamino)ethanolato-O]}-tetrakis-(tert.-butyl)digallium ; _chemical_name_common ;Bis-(mu2-O-(2-(tert.-butylamino)ethanolato-O))-tetrakis- (tert.-butyl)digallium ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H64 Ga2 N2 O2' _chemical_formula_weight 600.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1031(15) _cell_length_b 17.365(2) _cell_length_c 8.9371(12) _cell_angle_alpha 90.00 _cell_angle_beta 98.722(3) _cell_angle_gamma 90.00 _cell_volume 1703.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description sticks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6898 _exptl_absorpt_correction_T_max 0.8823 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.787736 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19618 _diffrn_reflns_av_R_equivalents 0.0926 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 30.07 _reflns_number_total 4995 _reflns_number_gt 3007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT and SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3, L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0677P)^2^+0.0558P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4995 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1504 _refine_ls_wR_factor_gt 0.1299 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.60648(3) -0.05267(2) 0.06252(4) 0.02604(13) Uani 1 1 d . . . O1 O 0.5455(2) 0.05205(12) 0.0803(3) 0.0277(5) Uani 1 1 d . . . N1 N 0.7659(3) 0.1680(2) 0.3349(4) 0.0516(10) Uani 1 1 d . . . H1A H 0.7438 0.2140 0.2991 0.062 Uiso 1 1 calc R . . C1 C 0.6114(3) 0.1184(2) 0.1411(5) 0.0398(10) Uani 1 1 d . . . H1B H 0.5530 0.1585 0.1625 0.048 Uiso 1 1 calc R . . H1C H 0.6588 0.1393 0.0649 0.048 Uiso 1 1 calc R . . C2 C 0.6957(4) 0.1006(2) 0.2826(4) 0.0395(10) Uani 1 1 d . . . H2A H 0.6483 0.0831 0.3616 0.047 Uiso 1 1 calc R . . H2B H 0.7514 0.0584 0.2633 0.047 Uiso 1 1 calc R . . C3 C 0.8742(3) 0.1584(3) 0.4483(4) 0.0404(10) Uani 1 1 d . . . C31 C 0.9664(5) 0.1149(4) 0.3771(8) 0.105(3) Uani 1 1 d . . . H31A H 0.9527 0.0595 0.3870 0.157 Uiso 1 1 calc R . . H31B H 1.0483 0.1280 0.4278 0.157 Uiso 1 1 calc R . . H31C H 0.9588 0.1284 0.2696 0.157 Uiso 1 1 calc R . . C32 C 0.8481(6) 0.1206(4) 0.5892(6) 0.103(3) Uani 1 1 d . . . H32A H 0.8117 0.0699 0.5645 0.154 Uiso 1 1 calc R . . H32B H 0.7914 0.1524 0.6362 0.154 Uiso 1 1 calc R . . H32C H 0.9242 0.1144 0.6597 0.154 Uiso 1 1 calc R . . C33 C 0.9241(5) 0.2390(3) 0.4851(6) 0.088(2) Uani 1 1 d . . . H33A H 0.9301 0.2666 0.3909 0.132 Uiso 1 1 calc R . . H33B H 1.0050 0.2354 0.5461 0.132 Uiso 1 1 calc R . . H33C H 0.8692 0.2670 0.5420 0.132 Uiso 1 1 calc R . . C11 C 0.7493(3) -0.0587(2) -0.0502(5) 0.0391(9) Uani 1 1 d . . . C12 C 0.8477(5) -0.1101(4) 0.0250(8) 0.112(3) Uani 1 1 d . . . H12A H 0.9164 -0.1094 -0.0320 0.169 Uiso 1 1 calc R . . H12B H 0.8165 -0.1627 0.0282 0.169 Uiso 1 1 calc R . . H12C H 0.8750 -0.0919 0.1284 0.169 Uiso 1 1 calc R . . C13 C 0.8101(5) 0.0205(3) -0.0639(6) 0.0645(14) Uani 1 1 d . . . H13A H 0.8782 0.0149 -0.1211 0.097 Uiso 1 1 calc R . . H13B H 0.8404 0.0404 0.0374 0.097 Uiso 1 1 calc R . . H13C H 0.7502 0.0565 -0.1167 0.097 Uiso 1 1 calc R . . C14 C 0.7061(5) -0.0841(4) -0.2128(6) 0.088(2) Uani 1 1 d . . . H14A H 0.7734 -0.0797 -0.2716 0.132 Uiso 1 1 calc R . . H14B H 0.6385 -0.0511 -0.2578 0.132 Uiso 1 1 calc R . . H14C H 0.6785 -0.1377 -0.2135 0.132 Uiso 1 1 calc R . . C21 C 0.5919(4) -0.1198(2) 0.2432(4) 0.0404(10) Uani 1 1 d . . . C22 C 0.5737(6) -0.2033(3) 0.1841(7) 0.105(3) Uani 1 1 d . . . H22A H 0.5912 -0.2393 0.2690 0.158 Uiso 1 1 calc R . . H22B H 0.6291 -0.2134 0.1107 0.158 Uiso 1 1 calc R . . H22C H 0.4893 -0.2101 0.1350 0.158 Uiso 1 1 calc R . . C23 C 0.4923(6) -0.0960(4) 0.3230(7) 0.114(3) Uani 1 1 d . . . H23A H 0.4802 -0.1350 0.3986 0.172 Uiso 1 1 calc R . . H23B H 0.4173 -0.0905 0.2503 0.172 Uiso 1 1 calc R . . H23C H 0.5127 -0.0466 0.3735 0.172 Uiso 1 1 calc R . . C24 C 0.7090(5) -0.1206(3) 0.3533(5) 0.0650(14) Uani 1 1 d . . . H24A H 0.7036 -0.1592 0.4320 0.097 Uiso 1 1 calc R . . H24B H 0.7227 -0.0697 0.4001 0.097 Uiso 1 1 calc R . . H24C H 0.7770 -0.1334 0.2994 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0263(2) 0.0224(2) 0.0292(2) -0.00026(18) 0.00336(14) 0.00039(17) O1 0.0264(12) 0.0215(11) 0.0341(13) -0.0058(11) 0.0012(10) -0.0011(10) N1 0.053(2) 0.0326(19) 0.061(2) -0.0050(17) -0.0189(19) -0.0139(17) C1 0.037(2) 0.029(2) 0.050(2) -0.0072(18) -0.0051(18) -0.0027(17) C2 0.042(2) 0.035(2) 0.040(2) -0.0069(18) -0.0006(18) -0.0100(18) C3 0.036(2) 0.050(2) 0.034(2) -0.0068(19) 0.0031(17) -0.0148(19) C31 0.044(3) 0.156(7) 0.108(5) -0.062(5) -0.010(3) 0.012(4) C32 0.107(5) 0.158(7) 0.040(3) 0.006(4) -0.001(3) -0.076(5) C33 0.099(4) 0.074(4) 0.078(4) -0.008(3) -0.028(3) -0.050(3) C11 0.030(2) 0.045(2) 0.045(2) -0.0077(19) 0.0113(17) 0.0068(18) C12 0.073(4) 0.145(6) 0.133(6) 0.081(5) 0.060(4) 0.074(4) C13 0.059(3) 0.080(4) 0.062(3) -0.001(3) 0.034(3) -0.011(3) C14 0.058(4) 0.136(6) 0.075(4) -0.045(4) 0.030(3) -0.006(4) C21 0.042(2) 0.037(2) 0.041(2) 0.0139(18) 0.0016(19) -0.0015(18) C22 0.180(7) 0.047(3) 0.080(4) 0.029(3) -0.013(4) -0.038(4) C23 0.093(5) 0.172(7) 0.092(5) 0.096(5) 0.057(4) 0.065(5) C24 0.070(3) 0.069(3) 0.052(3) 0.029(3) -0.005(2) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 O1 1.955(2) . ? Ga1 O1 1.956(2) 3_655 ? Ga1 C11 2.007(4) . ? Ga1 C21 2.018(4) . ? O1 C1 1.428(4) . ? O1 Ga1 1.956(2) 3_655 ? N1 C2 1.445(5) . ? N1 C3 1.460(5) . ? N1 H1A 0.8800 . ? C1 C2 1.487(5) . ? C1 H1B 0.9900 . ? C1 H1C 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C32 1.488(6) . ? C3 C31 1.491(7) . ? C3 C33 1.522(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C11 C12 1.489(6) . ? C11 C14 1.525(6) . ? C11 C13 1.546(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 C23 1.463(7) . ? C21 C24 1.507(6) . ? C21 C22 1.545(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga1 O1 76.87(10) . 3_655 ? O1 Ga1 C11 113.53(14) . . ? O1 Ga1 C11 110.01(14) 3_655 . ? O1 Ga1 C21 113.68(14) . . ? O1 Ga1 C21 111.07(13) 3_655 . ? C11 Ga1 C21 122.47(17) . . ? C1 O1 Ga1 128.2(2) . . ? C1 O1 Ga1 125.8(2) . 3_655 ? Ga1 O1 Ga1 103.13(10) . 3_655 ? C2 N1 C3 118.6(3) . . ? C2 N1 H1A 120.7 . . ? C3 N1 H1A 120.7 . . ? O1 C1 C2 112.0(3) . . ? O1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? O1 C1 H1C 109.2 . . ? C2 C1 H1C 109.2 . . ? H1B C1 H1C 107.9 . . ? N1 C2 C1 110.2(3) . . ? N1 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? N1 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? N1 C3 C32 113.1(4) . . ? N1 C3 C31 107.9(4) . . ? C32 C3 C31 111.8(5) . . ? N1 C3 C33 106.2(4) . . ? C32 C3 C33 109.5(4) . . ? C31 C3 C33 107.9(4) . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C3 C32 H32A 109.5 . . ? C3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C3 C33 H33A 109.5 . . ? C3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C12 C11 C14 111.2(5) . . ? C12 C11 C13 105.7(4) . . ? C14 C11 C13 105.0(4) . . ? C12 C11 Ga1 112.7(3) . . ? C14 C11 Ga1 109.6(3) . . ? C13 C11 Ga1 112.4(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C23 C21 C24 109.0(4) . . ? C23 C21 C22 111.2(5) . . ? C24 C21 C22 105.7(4) . . ? C23 C21 Ga1 112.6(3) . . ? C24 C21 Ga1 111.2(3) . . ? C22 C21 Ga1 106.9(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ga1 O1 C1 -161.5(4) 3_655 . . . ? C11 Ga1 O1 C1 -55.2(3) . . . . ? C21 Ga1 O1 C1 91.0(3) . . . . ? O1 Ga1 O1 Ga1 0.0 3_655 . . 3_655 ? C11 Ga1 O1 Ga1 106.36(16) . . . 3_655 ? C21 Ga1 O1 Ga1 -107.51(15) . . . 3_655 ? Ga1 O1 C1 C2 -42.4(5) . . . . ? Ga1 O1 C1 C2 160.0(3) 3_655 . . . ? C3 N1 C2 C1 -164.7(4) . . . . ? O1 C1 C2 N1 176.4(3) . . . . ? C2 N1 C3 C32 -57.2(6) . . . . ? C2 N1 C3 C31 67.0(6) . . . . ? C2 N1 C3 C33 -177.4(4) . . . . ? O1 Ga1 C11 C12 135.7(4) . . . . ? O1 Ga1 C11 C12 -140.3(4) 3_655 . . . ? C21 Ga1 C11 C12 -7.1(5) . . . . ? O1 Ga1 C11 C14 -100.0(4) . . . . ? O1 Ga1 C11 C14 -16.0(4) 3_655 . . . ? C21 Ga1 C11 C14 117.3(4) . . . . ? O1 Ga1 C11 C13 16.4(4) . . . . ? O1 Ga1 C11 C13 100.4(3) 3_655 . . . ? C21 Ga1 C11 C13 -126.3(3) . . . . ? O1 Ga1 C21 C23 27.0(5) . . . . ? O1 Ga1 C21 C23 -57.5(5) 3_655 . . . ? C11 Ga1 C21 C23 169.7(4) . . . . ? O1 Ga1 C21 C24 -95.7(3) . . . . ? O1 Ga1 C21 C24 179.9(3) 3_655 . . . ? C11 Ga1 C21 C24 47.0(4) . . . . ? O1 Ga1 C21 C22 149.4(3) . . . . ? O1 Ga1 C21 C22 65.0(4) 3_655 . . . ? C11 Ga1 C21 C22 -67.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.955 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.098 #===END data_3a _database_code_depnum_ccdc_archive 'CCDC 694708' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-{mu2-O-[2-methylamino-1-propanolato-O,N-]} tetramethyldialuminium ; _chemical_name_common ;Bis-(mu2-O-(2-methylamino-1-propanolato-O,N-)) tetramethyldialuminium ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 Al2 N2 O2' _chemical_formula_weight 290.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.6720(3) _cell_length_b 12.1738(5) _cell_length_c 10.6722(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.544(3) _cell_angle_gamma 90.00 _cell_volume 866.52(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1705 _cell_measurement_theta_min 5.51 _cell_measurement_theta_max 69.64 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 320 _exptl_absorpt_coefficient_mu 1.499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'goebel mirror' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4601 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 5.51 _diffrn_reflns_theta_max 69.97 _reflns_number_total 1506 _reflns_number_gt 1123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT and SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3, L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1251P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1506 _refine_ls_number_parameters 95 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1731 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.54772(12) 0.94807(7) 0.12428(7) 0.0290(3) Uani 1 1 d . . . O1 O 0.6094(3) 1.06990(15) 0.03292(18) 0.0314(5) Uani 1 1 d . . . N1 N 0.7700(4) 0.9993(2) 0.2653(2) 0.0412(7) Uani 1 1 d . . . C1 C 0.6939(6) 1.1733(3) 0.0643(4) 0.0565(10) Uani 1 1 d . . . H1A H 0.588 1.2206 0.0976 0.068 Uiso 1 1 calc R . . H1B H 0.7418 1.2080 -0.013 0.068 Uiso 1 1 calc R . . C2 C 0.8633(6) 1.1677(3) 0.1579(4) 0.0572(11) Uani 1 1 d . . . H2A H 0.9111 1.241 0.1736 0.069 Uiso 1 1 calc R . . H2B H 0.971 1.1271 0.1221 0.069 Uiso 1 1 calc R . . C3 C 0.8135(5) 1.1160(3) 0.2806(3) 0.0508(10) Uani 1 1 d . . . H3A H 0.924 1.1251 0.3387 0.061 Uiso 1 1 calc R . . H3B H 0.700 1.1522 0.3143 0.061 Uiso 1 1 calc R . . C4 C 0.7413(6) 0.9447(4) 0.3881(3) 0.0695(14) Uani 1 1 d . . . H4A H 0.858 0.947 0.4341 0.104 Uiso 1 1 calc R . . H4B H 0.705 0.873 0.3751 0.104 Uiso 1 1 calc R . . H4C H 0.644 0.9801 0.4302 0.104 Uiso 1 1 calc R . . C11 C 0.7047(5) 0.8095(2) 0.1084(3) 0.0428(8) Uani 1 1 d . . . H11A H 0.626 0.7572 0.073 0.064 Uiso 1 1 calc R . . H11B H 0.748 0.7873 0.1848 0.064 Uiso 1 1 calc R . . H11C H 0.811 0.8215 0.060 0.064 Uiso 1 1 calc R . . C21 C 0.3134(5) 0.9601(3) 0.2340(3) 0.0444(8) Uani 1 1 d . . . H21A H 0.202 0.9277 0.1947 0.067 Uiso 1 1 calc R . . H21B H 0.287 1.0338 0.2492 0.067 Uiso 1 1 calc R . . H21C H 0.3415 0.9245 0.3095 0.067 Uiso 1 1 calc R . . H1 H 0.893(6) 0.971(3) 0.238(3) 0.049(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0275(5) 0.0344(5) 0.0250(5) 0.0031(3) -0.0042(3) 0.0022(3) O1 0.0347(12) 0.0302(11) 0.0287(10) 0.0029(8) -0.0095(8) -0.0028(8) N1 0.0357(16) 0.0616(18) 0.0258(14) 0.0008(12) -0.0078(12) 0.0017(12) C1 0.059(2) 0.0387(19) 0.070(3) 0.0042(17) -0.029(2) -0.0076(15) C2 0.060(2) 0.0377(18) 0.072(3) 0.0015(17) -0.034(2) -0.0085(15) C3 0.041(2) 0.065(2) 0.0460(19) -0.0238(17) -0.0146(16) 0.0081(16) C4 0.053(3) 0.126(4) 0.0279(18) 0.017(2) -0.0139(17) -0.012(2) C11 0.0371(18) 0.0453(19) 0.0459(19) 0.0052(14) -0.0037(15) 0.0045(13) C21 0.0312(18) 0.057(2) 0.0451(19) 0.0043(15) 0.0050(14) 0.0063(13) _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 O1 1.828(2) . ? Al1 O1 1.966(2) 3_675 ? Al1 C21 1.984(3) . ? Al1 C11 1.995(3) . ? Al1 N1 2.175(3) . ? Al1 Al1 2.9916(15) 3_675 ? O1 C1 1.416(4) . ? O1 Al1 1.966(2) 3_675 ? N1 C3 1.458(5) . ? N1 C4 1.487(4) . ? N1 H1 0.94(4) . ? C1 C2 1.490(4) . ? C1 H1A 0.9830 . ? C1 H1B 0.9830 . ? C2 C3 1.498(5) . ? C2 H2A 0.9576 . ? C2 H2B 0.9576 . ? C3 H3A 0.9571 . ? C3 H3B 0.9571 . ? C4 H4A 0.9109 . ? C4 H4B 0.9109 . ? C4 H4C 0.9109 . ? C11 H11A 0.8989 . ? C11 H11B 0.8989 . ? C11 H11C 0.8989 . ? C21 H21A 0.9297 . ? C21 H21B 0.9297 . ? C21 H21C 0.9297 . ? 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 O1 Al1 O1 75.97(9) . 3_675 ? O1 Al1 C21 116.56(12) . . ? O1 Al1 C21 95.82(12) 3_675 . ? O1 Al1 C11 120.98(13) . . ? O1 Al1 C11 95.88(12) 3_675 . ? C21 Al1 C11 122.43(14) . . ? O1 Al1 N1 88.69(10) . . ? O1 Al1 N1 163.70(11) 3_675 . ? C21 Al1 N1 95.97(13) . . ? C11 Al1 N1 87.24(12) . . ? O1 Al1 Al1 39.62(6) . 3_675 ? O1 Al1 Al1 36.35(6) 3_675 3_675 ? C21 Al1 Al1 109.87(10) . 3_675 ? C11 Al1 Al1 112.45(11) . 3_675 ? N1 Al1 Al1 128.09(9) . 3_675 ? C1 O1 Al1 133.6(2) . . ? C1 O1 Al1 120.01(18) . 3_675 ? Al1 O1 Al1 104.03(9) . 3_675 ? C3 N1 C4 111.6(3) . . ? C3 N1 Al1 119.15(19) . . ? C4 N1 Al1 112.3(2) . . ? C3 N1 H1 103(2) . . ? C4 N1 H1 104(2) . . ? Al1 N1 H1 105(2) . . ? O1 C1 C2 114.0(3) . . ? O1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? O1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C1 C2 C3 115.0(3) . . ? C1 C2 H2A 108.5 . . ? C3 C2 H2A 108.5 . . ? C1 C2 H2B 108.5 . . ? C3 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? N1 C3 C2 111.1(3) . . ? N1 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Al1 C11 H11A 109.5 . . ? Al1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Al1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Al1 C21 H21A 109.5 . . ? Al1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Al1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Al1 O1 C1 161.7(3) 3_675 . . . ? C21 Al1 O1 C1 72.2(3) . . . . ? C11 Al1 O1 C1 -109.8(3) . . . . ? N1 Al1 O1 C1 -23.8(3) . . . . ? Al1 Al1 O1 C1 161.7(3) 3_675 . . . ? O1 Al1 O1 Al1 0.0 3_675 . . 3_675 ? C21 Al1 O1 Al1 -89.54(15) . . . 3_675 ? C11 Al1 O1 Al1 88.46(15) . . . 3_675 ? N1 Al1 O1 Al1 174.45(12) . . . 3_675 ? O1 Al1 N1 C3 28.6(3) . . . . ? O1 Al1 N1 C3 48.2(5) 3_675 . . . ? C21 Al1 N1 C3 -88.0(3) . . . . ? C11 Al1 N1 C3 149.7(3) . . . . ? Al1 Al1 N1 C3 33.1(3) 3_675 . . . ? O1 Al1 N1 C4 161.7(3) . . . . ? O1 Al1 N1 C4 -178.7(3) 3_675 . . . ? C21 Al1 N1 C4 45.2(3) . . . . ? C11 Al1 N1 C4 -77.2(3) . . . . ? Al1 Al1 N1 C4 166.2(2) 3_675 . . . ? Al1 O1 C1 C2 41.1(5) . . . . ? Al1 O1 C1 C2 -159.5(3) 3_675 . . . ? O1 C1 C2 C3 -58.2(5) . . . . ? C4 N1 C3 C2 174.0(3) . . . . ? Al1 N1 C3 C2 -52.5(4) . . . . ? C1 C2 C3 N1 67.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 69.97 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.560 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.085 #===END data_3c _database_code_depnum_ccdc_archive 'CCDC 694709' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [3-Methylamino-1-propanolato-O,N]-dimethylgallium ; _chemical_name_common (3-Methylamino-1-propanolato-O,N)-dimethylgallium _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H16 Ga N O' _chemical_formula_weight 187.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.613(9) _cell_length_b 7.188(5) _cell_length_c 8.594(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.80(12) _cell_angle_gamma 90.00 _cell_volume 452.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 5.57 _cell_measurement_theta_max 25.57 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 196 _exptl_absorpt_coefficient_mu 2.975 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'STOE IPDS-1' _diffrn_measurement_method '\phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5871 _diffrn_reflns_av_R_equivalents 0.1425 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 5.57 _diffrn_reflns_theta_max 25.57 _reflns_number_total 1653 _reflns_number_gt 1564 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS-1' _computing_cell_refinement 'XArea (STOE 2003)' _computing_data_reduction 'XArea (STOE 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0728P)^2^+0.7461P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(5) _refine_ls_number_reflns 1653 _refine_ls_number_parameters 85 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.189 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga -0.10011(8) -0.23489(16) -0.27468(7) 0.0252(3) Uani 1 1 d . . . O1 O -0.1264(7) -0.3771(8) -0.0994(7) 0.0299(11) Uani 1 1 d . . . N1 N -0.1496(7) 0.0138(9) -0.1782(8) 0.0247(13) Uani 1 1 d . . . H1 H -0.0535 0.0361 -0.0869 0.030 Uiso 1 1 calc R . . C1 C -0.2907(11) -0.3453(13) -0.0546(12) 0.034(2) Uani 1 1 d . . . H1A H -0.2974 -0.4346 0.0314 0.040 Uiso 1 1 calc R . . H1B H -0.3961 -0.3694 -0.1492 0.040 Uiso 1 1 calc R . . C2 C -0.3053(11) -0.1473(13) 0.0062(11) 0.0299(19) Uani 1 1 d . . . H2A H -0.1964 -0.1211 0.0971 0.036 Uiso 1 1 calc R . . H2B H -0.4138 -0.1394 0.0483 0.036 Uiso 1 1 calc R . . C3 C -0.3205(9) 0.0036(11) -0.1254(10) 0.0295(16) Uani 1 1 d . . . H3A H -0.4247 -0.0257 -0.2197 0.035 Uiso 1 1 calc R . . H3B H -0.3441 0.1259 -0.0821 0.035 Uiso 1 1 calc R . . C4 C -0.1594(12) 0.1714(11) -0.2887(10) 0.0328(17) Uani 1 1 d . . . H4A H -0.1764 0.2868 -0.2339 0.049 Uiso 1 1 calc R . . H4B H -0.2624 0.1538 -0.3847 0.049 Uiso 1 1 calc R . . H4C H -0.0458 0.1788 -0.3212 0.049 Uiso 1 1 calc R . . C11 C -0.3031(13) -0.2727(11) -0.4710(12) 0.044(2) Uani 1 1 d . . . H11A H -0.2593 -0.3423 -0.5510 0.066 Uiso 1 1 calc R . . H11B H -0.3502 -0.1516 -0.5161 0.066 Uiso 1 1 calc R . . H11C H -0.4008 -0.3428 -0.4433 0.066 Uiso 1 1 calc R . . C21 C 0.1581(9) -0.237(2) -0.2811(8) 0.0353(15) Uani 1 1 d . . . H21A H 0.1774 -0.3405 -0.3489 0.053 Uiso 1 1 calc R . . H21B H 0.2379 -0.2524 -0.1713 0.053 Uiso 1 1 calc R . . H21C H 0.1867 -0.1194 -0.3265 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 Ga1 0.0208(4) 0.0272(4) 0.0238(4) -0.0034(5) -0.0001(2) 0.0021(4) O1 0.018(2) 0.029(3) 0.038(3) -0.006(2) 0.001(2) 0.003(2) N1 0.012(2) 0.030(3) 0.029(3) 0.002(3) 0.001(2) -0.004(2) C1 0.014(3) 0.042(5) 0.046(6) 0.010(4) 0.010(3) 0.001(3) C2 0.016(3) 0.041(4) 0.036(5) 0.007(4) 0.012(3) 0.001(3) C3 0.018(3) 0.030(4) 0.040(4) 0.002(3) 0.007(3) 0.003(3) C4 0.036(4) 0.025(4) 0.030(4) 0.004(3) -0.003(3) 0.002(3) C11 0.044(4) 0.032(7) 0.049(5) -0.009(3) 0.000(4) 0.004(3) C21 0.038(3) 0.041(4) 0.030(3) 0.014(7) 0.014(3) 0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 O1 1.875(6) . ? Ga1 C11 1.972(10) . ? Ga1 C21 1.982(7) . ? Ga1 N1 2.048(7) . ? O1 C1 1.424(10) . ? N1 C4 1.466(10) . ? N1 C3 1.492(9) . ? N1 H1 0.9300 . ? C1 C2 1.531(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.549(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga1 C11 112.4(3) . . ? O1 Ga1 C21 110.0(3) . . ? C11 Ga1 C21 121.8(4) . . ? O1 Ga1 N1 94.5(3) . . ? C11 Ga1 N1 106.2(3) . . ? C21 Ga1 N1 108.1(4) . . ? C1 O1 Ga1 115.1(5) . . ? C4 N1 C3 109.9(6) . . ? C4 N1 Ga1 113.3(5) . . ? C3 N1 Ga1 110.6(5) . . ? C4 N1 H1 107.6 . . ? C3 N1 H1 107.6 . . ? Ga1 N1 H1 107.6 . . ? O1 C1 C2 113.1(7) . . ? O1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? O1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C1 C2 C3 113.6(7) . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2B 108.9 . . ? C3 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? N1 C3 C2 111.0(6) . . ? N1 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Ga1 C11 H11A 109.5 . . ? Ga1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Ga1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Ga1 C21 H21A 109.5 . . ? Ga1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Ga1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Ga1 O1 C1 -57.5(6) . . . . ? C21 Ga1 O1 C1 163.3(7) . . . . ? N1 Ga1 O1 C1 52.1(6) . . . . ? O1 Ga1 N1 C4 -174.5(5) . . . . ? C11 Ga1 N1 C4 -59.6(6) . . . . ? C21 Ga1 N1 C4 72.7(5) . . . . ? O1 Ga1 N1 C3 -50.6(5) . . . . ? C11 Ga1 N1 C3 64.3(6) . . . . ? C21 Ga1 N1 C3 -163.4(5) . . . . ? Ga1 O1 C1 C2 -64.0(8) . . . . ? O1 C1 C2 C3 65.8(10) . . . . ? C4 N1 C3 C2 -173.5(7) . . . . ? Ga1 N1 C3 C2 60.7(7) . . . . ? C1 C2 C3 N1 -65.7(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 0.93 1.91 2.827(9) 170.3 2 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.696 _refine_diff_density_min -2.101 _refine_diff_density_rms 0.158 #===END data_3d _database_code_depnum_ccdc_archive 'CCDC 694710' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [3-Methylamino-1-propanolato-O,N]-di-tert.-butylgallium ; _chemical_name_common (3-Methylamino-1-propanolato-O,N)-di-tert.-butylgallium _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 Ga N O' _chemical_formula_weight 272.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.0328(13) _cell_length_b 19.091(3) _cell_length_c 15.374(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2944.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 1.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7563 _exptl_absorpt_correction_T_max 0.8971 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27191 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3375 _reflns_number_gt 2524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _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^)+(0.0288P)^2^+0.8583P] 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 3375 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Ga1 Ga 0.22961(2) 0.347954(12) 0.016508(16) 0.02134(8) Uani 1 1 d . . . N1 N 0.04583(19) 0.31281(10) 0.06385(13) 0.0234(4) Uani 1 1 d . . . H1 H 0.002(2) 0.2925(13) 0.0259(16) 0.026(7) Uiso 1 1 d . . . O1 O 0.31437(15) 0.26072(8) 0.01751(10) 0.0257(3) Uani 1 1 d . . . C1 C 0.2936(2) 0.21759(13) 0.09086(16) 0.0309(6) Uani 1 1 d . . . H1A H 0.3291 0.2416 0.1430 0.037 Uiso 1 1 calc R . . H1B H 0.3445 0.1736 0.0832 0.037 Uiso 1 1 calc R . . C2 C 0.1480(2) 0.19953(12) 0.10649(16) 0.0319(6) Uani 1 1 d . . . H2A H 0.1102 0.1799 0.0522 0.038 Uiso 1 1 calc R . . H2B H 0.1430 0.1627 0.1517 0.038 Uiso 1 1 calc R . . C3 C 0.0632(2) 0.26105(12) 0.13488(15) 0.0281(5) Uani 1 1 d . . . H3A H -0.0253 0.2438 0.1536 0.034 Uiso 1 1 calc R . . H3B H 0.1058 0.2842 0.1853 0.034 Uiso 1 1 calc R . . C4 C -0.0461(2) 0.36940(12) 0.09185(17) 0.0344(6) Uani 1 1 d . . . H4A H -0.1322 0.3490 0.1081 0.052 Uiso 1 1 calc R . . H4B H -0.0588 0.4026 0.0439 0.052 Uiso 1 1 calc R . . H4C H -0.0080 0.3939 0.1420 0.052 Uiso 1 1 calc R . . C21 C 0.3133(2) 0.41434(13) 0.10265(16) 0.0303(5) Uani 1 1 d . . . C22 C 0.4632(3) 0.40870(14) 0.08756(19) 0.0411(7) Uani 1 1 d . . . H22A H 0.5100 0.4400 0.1278 0.062 Uiso 1 1 calc R . . H22B H 0.4838 0.4221 0.0275 0.062 Uiso 1 1 calc R . . H22C H 0.4920 0.3603 0.0977 0.062 Uiso 1 1 calc R . . C23 C 0.2705(3) 0.48991(13) 0.0843(2) 0.0444(7) Uani 1 1 d . . . H23A H 0.1745 0.4947 0.0943 0.067 Uiso 1 1 calc R . . H23B H 0.2909 0.5017 0.0236 0.067 Uiso 1 1 calc R . . H23C H 0.3189 0.5217 0.1230 0.067 Uiso 1 1 calc R . . C24 C 0.2870(3) 0.39873(16) 0.19918(18) 0.0485(8) Uani 1 1 d . . . H24A H 0.3153 0.3508 0.2125 0.073 Uiso 1 1 calc R . . H24B H 0.1916 0.4037 0.2114 0.073 Uiso 1 1 calc R . . H24C H 0.3374 0.4317 0.2352 0.073 Uiso 1 1 calc R . . C11 C 0.2003(2) 0.37454(12) -0.10808(14) 0.0247(5) Uani 1 1 d . . . C12 C 0.3301(3) 0.40495(13) -0.14598(17) 0.0347(6) Uani 1 1 d . . . H12A H 0.3169 0.4160 -0.2076 0.052 Uiso 1 1 calc R . . H12B H 0.4019 0.3705 -0.1401 0.052 Uiso 1 1 calc R . . H12C H 0.3540 0.4477 -0.1144 0.052 Uiso 1 1 calc R . . C13 C 0.0913(3) 0.42954(13) -0.11931(17) 0.0365(6) Uani 1 1 d . . . H13A H 0.0831 0.4417 -0.1810 0.055 Uiso 1 1 calc R . . H13B H 0.1145 0.4715 -0.0859 0.055 Uiso 1 1 calc R . . H13C H 0.0064 0.4107 -0.0982 0.055 Uiso 1 1 calc R . . C14 C 0.1617(2) 0.30974(13) -0.16057(15) 0.0308(6) Uani 1 1 d . . . H14A H 0.0790 0.2900 -0.1372 0.046 Uiso 1 1 calc R . . H14B H 0.2331 0.2748 -0.1566 0.046 Uiso 1 1 calc R . . H14C H 0.1484 0.3229 -0.2216 0.046 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 Ga1 0.02065(13) 0.02205(13) 0.02132(13) -0.00075(10) -0.00032(10) -0.00125(10) N1 0.0217(10) 0.0241(10) 0.0244(11) -0.0032(8) -0.0001(8) 0.0002(8) O1 0.0262(8) 0.0261(8) 0.0249(8) 0.0043(7) 0.0034(7) 0.0028(6) C1 0.0241(14) 0.0348(14) 0.0337(14) 0.0106(11) 0.0009(10) 0.0036(10) C2 0.0295(14) 0.0295(13) 0.0366(15) 0.0118(11) 0.0020(11) -0.0002(10) C3 0.0243(13) 0.0336(13) 0.0265(13) 0.0043(10) 0.0029(10) -0.0036(10) C4 0.0302(14) 0.0315(13) 0.0415(15) -0.0056(11) 0.0072(11) 0.0061(10) C21 0.0300(13) 0.0318(13) 0.0292(14) -0.0063(10) -0.0029(10) -0.0081(10) C22 0.0315(15) 0.0454(16) 0.0464(17) -0.0065(13) -0.0066(12) -0.0114(12) C23 0.0454(17) 0.0340(14) 0.0536(18) -0.0129(13) -0.0024(14) -0.0027(13) C24 0.0564(19) 0.060(2) 0.0286(15) -0.0092(13) -0.0033(13) -0.0201(15) C11 0.0222(12) 0.0255(11) 0.0264(13) 0.0028(10) -0.0003(9) 0.0002(9) C12 0.0356(15) 0.0381(15) 0.0304(14) 0.0080(11) 0.0052(11) 0.0008(11) C13 0.0358(15) 0.0363(14) 0.0375(15) 0.0041(12) -0.0036(11) 0.0079(11) C14 0.0280(14) 0.0378(14) 0.0264(13) -0.0032(11) -0.0026(10) -0.0015(11) _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 Ga1 O1 1.8700(15) . ? Ga1 C11 2.003(2) . ? Ga1 C21 2.016(2) . ? Ga1 N1 2.0927(19) . ? N1 C3 1.483(3) . ? N1 C4 1.484(3) . ? N1 H1 0.83(2) . ? O1 C1 1.412(3) . ? C1 C2 1.520(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.514(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C21 C22 1.525(4) . ? C21 C23 1.532(3) . ? C21 C24 1.536(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C11 C13 1.526(3) . ? C11 C14 1.527(3) . ? C11 C12 1.540(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga1 C11 107.47(8) . . ? O1 Ga1 C21 111.41(9) . . ? C11 Ga1 C21 122.00(10) . . ? O1 Ga1 N1 96.45(7) . . ? C11 Ga1 N1 106.53(8) . . ? C21 Ga1 N1 109.87(9) . . ? C3 N1 C4 110.15(18) . . ? C3 N1 Ga1 111.47(14) . . ? C4 N1 Ga1 114.53(14) . . ? C3 N1 H1 105.6(17) . . ? C4 N1 H1 102.5(17) . . ? Ga1 N1 H1 111.9(17) . . ? C1 O1 Ga1 117.31(14) . . ? O1 C1 C2 113.61(19) . . ? O1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? O1 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C3 C2 C1 114.2(2) . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N1 C3 C2 111.76(19) . . ? N1 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C22 C21 C23 108.3(2) . . ? C22 C21 C24 107.6(2) . . ? C23 C21 C24 108.2(2) . . ? C22 C21 Ga1 105.44(16) . . ? C23 C21 Ga1 110.75(17) . . ? C24 C21 Ga1 116.18(17) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C13 C11 C14 108.44(19) . . ? C13 C11 C12 107.7(2) . . ? C14 C11 C12 108.6(2) . . ? C13 C11 Ga1 112.81(16) . . ? C14 C11 Ga1 109.71(15) . . ? C12 C11 Ga1 109.47(16) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ga1 N1 C3 41.36(15) . . . . ? C11 Ga1 N1 C3 151.77(15) . . . . ? C21 Ga1 N1 C3 -74.20(16) . . . . ? O1 Ga1 N1 C4 167.26(16) . . . . ? C11 Ga1 N1 C4 -82.33(17) . . . . ? C21 Ga1 N1 C4 51.70(18) . . . . ? C11 Ga1 O1 C1 -152.54(16) . . . . ? C21 Ga1 O1 C1 71.39(18) . . . . ? N1 Ga1 O1 C1 -42.93(16) . . . . ? Ga1 O1 C1 C2 59.1(2) . . . . ? O1 C1 C2 C3 -68.7(3) . . . . ? C4 N1 C3 C2 175.6(2) . . . . ? Ga1 N1 C3 C2 -56.1(2) . . . . ? C1 C2 C3 N1 68.8(3) . . . . ? O1 Ga1 C21 C22 47.43(19) . . . . ? C11 Ga1 C21 C22 -81.28(19) . . . . ? N1 Ga1 C21 C22 153.09(16) . . . . ? O1 Ga1 C21 C23 164.39(16) . . . . ? C11 Ga1 C21 C23 35.7(2) . . . . ? N1 Ga1 C21 C23 -89.94(19) . . . . ? O1 Ga1 C21 C24 -71.6(2) . . . . ? C11 Ga1 C21 C24 159.69(19) . . . . ? N1 Ga1 C21 C24 34.1(2) . . . . ? O1 Ga1 C11 C13 159.46(16) . . . . ? C21 Ga1 C11 C13 -70.15(19) . . . . ? N1 Ga1 C11 C13 56.97(18) . . . . ? O1 Ga1 C11 C14 38.45(17) . . . . ? C21 Ga1 C11 C14 168.84(15) . . . . ? N1 Ga1 C11 C14 -64.04(17) . . . . ? O1 Ga1 C11 C12 -80.68(17) . . . . ? C21 Ga1 C11 C12 49.7(2) . . . . ? N1 Ga1 C11 C12 176.83(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 0.83(2) 2.24(3) 2.988(3) 150(2) 4_455 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.404 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.062 #===END data_4d _database_code_depnum_ccdc_archive 'CCDC 694711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-{mu2-O-[2-(tert.-butylamino)-1-propanolato-O]} -tetrakis-(tert.-butyl)digallium ; _chemical_name_common ; Bis-(mu2-O-(2-(tert.-butylamino)-1-propanolato-O)) -tetrakis- (tert.-butyl)digallium ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H68 Ga2 N2 O2' _chemical_formula_weight 628.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 24.362(3) _cell_length_b 11.1489(15) _cell_length_c 27.184(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.305(3) _cell_angle_gamma 90.00 _cell_volume 7049.2(17) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 1.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8355 _exptl_absorpt_correction_T_max 0.9405 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.868454 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40001 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 30.11 _reflns_number_total 10299 _reflns_number_gt 7530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT and SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3, L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0357P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10299 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.0960 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.387782(10) 0.85323(2) 0.103271(9) 0.01848(7) Uani 1 1 d . A . O1 O 0.34004(6) 0.99701(12) 0.09273(6) 0.0210(3) Uani 1 1 d . . . N1 N 0.16868(9) 0.9661(2) 0.15029(9) 0.0284(5) Uani 1 1 d . . . H1 H 0.1913(12) 0.982(2) 0.1778(11) 0.037(9) Uiso 1 1 d . . . C1 C 0.27898(9) 1.0100(2) 0.07859(9) 0.0261(5) Uani 1 1 d . . . H1A H 0.2614 0.9614 0.0474 0.031 Uiso 1 1 calc R . . H1B H 0.2689 1.0950 0.0699 0.031 Uiso 1 1 calc R . . C2 C 0.25405(10) 0.9718(2) 0.12066(10) 0.0301(6) Uani 1 1 d . . . H2A H 0.2561 0.8833 0.1238 0.036 Uiso 1 1 calc R . . H2B H 0.2776 1.0061 0.1538 0.036 Uiso 1 1 calc R . . C3 C 0.19255(10) 1.0111(2) 0.11073(9) 0.0281(5) Uani 1 1 d . . . H3A H 0.1907 1.0998 0.1100 0.034 Uiso 1 1 calc R . . H3B H 0.1693 0.9811 0.0766 0.034 Uiso 1 1 calc R . . C4 C 0.11083(10) 1.0084(2) 0.14869(9) 0.0252(5) Uani 1 1 d . . . C41 C 0.10589(12) 1.1442(2) 0.14964(12) 0.0456(8) Uani 1 1 d . . . H41A H 0.1338 1.1757 0.1808 0.068 Uiso 1 1 calc R . . H41B H 0.0669 1.1665 0.1495 0.068 Uiso 1 1 calc R . . H41C H 0.1138 1.1781 0.1192 0.068 Uiso 1 1 calc R . . C42 C 0.06736(10) 0.9585(2) 0.10087(10) 0.0336(6) Uani 1 1 d . . . H42A H 0.0734 0.9954 0.0701 0.050 Uiso 1 1 calc R . . H42B H 0.0284 0.9765 0.1020 0.050 Uiso 1 1 calc R . . H42C H 0.0722 0.8714 0.0995 0.050 Uiso 1 1 calc R . . C43 C 0.09905(11) 0.9549(3) 0.19633(10) 0.0378(6) Uani 1 1 d . . . H43A H 0.1001 0.8672 0.1946 0.057 Uiso 1 1 calc R . . H43B H 0.0610 0.9806 0.1976 0.057 Uiso 1 1 calc R . . H43C H 0.1284 0.9826 0.2274 0.057 Uiso 1 1 calc R . . C11 C 0.40097(10) 0.7683(2) 0.17066(9) 0.0254(5) Uani 1 1 d . . . C12 C 0.41234(13) 0.8547(2) 0.21595(10) 0.0398(7) Uani 1 1 d . . . H12A H 0.4208 0.8092 0.2482 0.060 Uiso 1 1 calc R . . H12B H 0.3783 0.9048 0.2123 0.060 Uiso 1 1 calc R . . H12C H 0.4452 0.9059 0.2166 0.060 Uiso 1 1 calc R . . C13 C 0.45393(11) 0.6878(2) 0.17818(10) 0.0320(6) Uani 1 1 d . . . H13A H 0.4878 0.7378 0.1808 0.048 Uiso 1 1 calc R . . H13B H 0.4477 0.6333 0.1487 0.048 Uiso 1 1 calc R . . H13C H 0.4602 0.6409 0.2099 0.048 Uiso 1 1 calc R . . C14 C 0.34998(11) 0.6885(3) 0.17092(12) 0.0449(7) Uani 1 1 d . . . H14A H 0.3585 0.6461 0.2039 0.067 Uiso 1 1 calc R . . H14B H 0.3431 0.6300 0.1428 0.067 Uiso 1 1 calc R . . H14C H 0.3156 0.7383 0.1662 0.067 Uiso 1 1 calc R . . C21 C 0.37629(11) 0.7596(2) 0.03802(9) 0.0289(5) Uani 1 1 d . . . C22 C 0.33146(12) 0.8153(2) -0.00794(10) 0.0391(7) Uani 1 1 d . . . H22A H 0.3428 0.8976 -0.0131 0.059 Uiso 1 1 calc R . . H22B H 0.2940 0.8162 -0.0014 0.059 Uiso 1 1 calc R . . H22C H 0.3287 0.7678 -0.0389 0.059 Uiso 1 1 calc R . . C23 C 0.35574(14) 0.6324(2) 0.04416(11) 0.0514(9) Uani 1 1 d . . . H23A H 0.3186 0.6361 0.0512 0.077 Uiso 1 1 calc R . . H23B H 0.3839 0.5925 0.0729 0.077 Uiso 1 1 calc R . . H23C H 0.3516 0.5871 0.0124 0.077 Uiso 1 1 calc R . . C24 C 0.43390(13) 0.7515(3) 0.02610(11) 0.0547(9) Uani 1 1 d . . . H24A H 0.4291 0.7032 -0.0050 0.082 Uiso 1 1 calc R . . H24B H 0.4626 0.7139 0.0552 0.082 Uiso 1 1 calc R . . H24C H 0.4468 0.8323 0.0205 0.082 Uiso 1 1 calc R . . Ga1A Ga 0.395904(10) 1.12604(2) 0.095449(9) 0.01886(7) Uani 1 1 d . A . O1A O 0.44399(6) 0.98290(12) 0.11169(6) 0.0197(3) Uani 1 1 d . . . N1A N 0.63114(9) 0.99726(19) 0.17162(10) 0.0291(5) Uani 1 1 d . A . H1AA H 0.6211(15) 0.991(3) 0.1927(13) 0.057(12) Uiso 1 1 d . . . C1A C 0.50395(11) 0.9740(3) 0.11729(19) 0.0235(8) Uani 0.875(10) 1 d P A 1 H1A1 H 0.5095 0.9575 0.0833 0.028 Uiso 0.875(10) 1 calc PR A 1 H1A2 H 0.5205 0.9061 0.1404 0.028 Uiso 0.875(10) 1 calc PR A 1 C2A C 0.53506(11) 1.0883(3) 0.13917(18) 0.0276(9) Uani 0.875(10) 1 d P A 1 H2A1 H 0.5148 1.1568 0.1184 0.033 Uiso 0.875(10) 1 calc PR A 1 H2A2 H 0.5329 1.0990 0.1747 0.033 Uiso 0.875(10) 1 calc PR A 1 C1AA C 0.5055(9) 0.9850(19) 0.1397(11) 0.020(5) Uiso 0.125(10) 1 d P A 2 H1A3 H 0.5108 1.0124 0.1755 0.023 Uiso 0.125(10) 1 calc PR A 2 H1A4 H 0.5212 0.9027 0.1413 0.023 Uiso 0.125(10) 1 calc PR A 2 C2AA C 0.5372(9) 1.063(2) 0.1156(11) 0.024(6) Uiso 0.125(10) 1 d P A 2 H2A3 H 0.5161 1.1403 0.1088 0.029 Uiso 0.125(10) 1 calc PR A 2 H2A4 H 0.5349 1.0279 0.0817 0.029 Uiso 0.125(10) 1 calc PR A 2 C3A C 0.59748(9) 1.0922(2) 0.14052(10) 0.0314(6) Uani 1 1 d . . . H3A1 H 0.5999 1.0854 0.1049 0.038 Uiso 1 1 calc R A 1 H3A2 H 0.6140 1.1706 0.1545 0.038 Uiso 1 1 calc R A 1 C4A C 0.69427(10) 1.0081(2) 0.18523(9) 0.0243(5) Uani 1 1 d . . . C41A C 0.71189(11) 1.0129(3) 0.13615(10) 0.0403(7) Uani 1 1 d . A . H41D H 0.6941 0.9460 0.1136 0.060 Uiso 1 1 calc R . . H41E H 0.7538 1.0067 0.1448 0.060 Uiso 1 1 calc R . . H41F H 0.6992 1.0889 0.1183 0.060 Uiso 1 1 calc R . . C42A C 0.71713(11) 1.1186(3) 0.21795(11) 0.0407(7) Uani 1 1 d . A . H42D H 0.7032 1.1911 0.1977 0.061 Uiso 1 1 calc R . . H42E H 0.7593 1.1176 0.2287 0.061 Uiso 1 1 calc R . . H42F H 0.7036 1.1181 0.2485 0.061 Uiso 1 1 calc R . . C43A C 0.71921(11) 0.8961(3) 0.21544(12) 0.0463(8) Uani 1 1 d . A . H43D H 0.7048 0.8888 0.2454 0.069 Uiso 1 1 calc R . . H43E H 0.7613 0.9018 0.2271 0.069 Uiso 1 1 calc R . . H43F H 0.7076 0.8255 0.1933 0.069 Uiso 1 1 calc R . . C11A C 0.39018(10) 1.1881(2) 0.02483(9) 0.0253(5) Uani 1 1 d . . . C12A C 0.42329(12) 1.1110(2) -0.00312(10) 0.0379(6) Uani 1 1 d . A . H12D H 0.4183 1.1438 -0.0376 0.057 Uiso 1 1 calc R . . H12E H 0.4086 1.0287 -0.0061 0.057 Uiso 1 1 calc R . . H12F H 0.4642 1.1111 0.0164 0.057 Uiso 1 1 calc R . . C13A C 0.32685(11) 1.1911(3) -0.00740(10) 0.0424(7) Uani 1 1 d . A . H13D H 0.3237 1.2230 -0.0417 0.064 Uiso 1 1 calc R . . H13E H 0.3053 1.2426 0.0095 0.064 Uiso 1 1 calc R . . H13F H 0.3110 1.1097 -0.0106 0.064 Uiso 1 1 calc R . . C14A C 0.41406(14) 1.3154(2) 0.02792(11) 0.0469(8) Uani 1 1 d . A . H14D H 0.4549 1.3149 0.0476 0.070 Uiso 1 1 calc R . . H14E H 0.3930 1.3676 0.0450 0.070 Uiso 1 1 calc R . . H14F H 0.4096 1.3454 -0.0069 0.070 Uiso 1 1 calc R . . C21A C 0.39690(10) 1.2361(2) 0.15429(9) 0.0281(5) Uani 1 1 d . . . C22A C 0.40255(14) 1.1683(2) 0.20412(10) 0.0456(8) Uani 1 1 d . A . H22D H 0.4004 1.2250 0.2310 0.068 Uiso 1 1 calc R . . H22E H 0.4396 1.1264 0.2149 0.068 Uiso 1 1 calc R . . H22F H 0.3713 1.1097 0.1986 0.068 Uiso 1 1 calc R . . C23A C 0.44543(13) 1.3280(2) 0.16486(11) 0.0428(7) Uani 1 1 d . A . H23D H 0.4416 1.3759 0.1338 0.064 Uiso 1 1 calc R . . H23E H 0.4825 1.2863 0.1745 0.064 Uiso 1 1 calc R . . H23F H 0.4434 1.3807 0.1931 0.064 Uiso 1 1 calc R . . C24A C 0.34013(12) 1.3042(3) 0.13950(13) 0.0541(9) Uani 1 1 d . A . H24D H 0.3082 1.2472 0.1341 0.081 Uiso 1 1 calc R . . H24E H 0.3361 1.3493 0.1077 0.081 Uiso 1 1 calc R . . H24F H 0.3395 1.3599 0.1672 0.081 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 Ga1 0.01660(12) 0.01837(12) 0.02022(13) 0.00074(9) 0.00509(10) -0.00125(9) O1 0.0112(7) 0.0231(8) 0.0295(9) 0.0008(6) 0.0071(6) 0.0011(6) N1 0.0167(10) 0.0461(13) 0.0244(12) 0.0065(10) 0.0093(9) 0.0023(9) C1 0.0129(10) 0.0396(14) 0.0266(13) -0.0003(10) 0.0069(9) 0.0026(9) C2 0.0199(12) 0.0382(14) 0.0354(14) 0.0112(11) 0.0131(11) 0.0069(10) C3 0.0196(12) 0.0413(15) 0.0268(13) 0.0078(11) 0.0122(10) 0.0049(10) C4 0.0209(12) 0.0297(13) 0.0292(13) -0.0051(10) 0.0137(10) -0.0041(9) C41 0.0376(15) 0.0382(16) 0.073(2) -0.0117(14) 0.0349(16) -0.0029(12) C42 0.0228(13) 0.0452(16) 0.0334(14) -0.0027(12) 0.0094(11) -0.0067(11) C43 0.0309(14) 0.0553(18) 0.0327(15) -0.0038(13) 0.0180(12) -0.0080(13) C11 0.0217(12) 0.0287(13) 0.0260(13) 0.0071(10) 0.0074(10) 0.0020(9) C12 0.0488(17) 0.0456(17) 0.0260(14) 0.0053(12) 0.0126(13) 0.0132(13) C13 0.0312(14) 0.0313(14) 0.0317(14) 0.0045(11) 0.0065(12) 0.0037(11) C14 0.0320(15) 0.0469(17) 0.0555(19) 0.0274(15) 0.0127(14) 0.0007(13) C21 0.0333(14) 0.0243(12) 0.0245(13) -0.0036(10) 0.0014(11) 0.0005(10) C22 0.0515(18) 0.0308(14) 0.0266(14) -0.0017(11) -0.0014(13) -0.0011(13) C23 0.075(2) 0.0223(14) 0.0410(17) -0.0031(12) -0.0077(16) -0.0042(14) C24 0.0495(19) 0.069(2) 0.0470(19) -0.0279(17) 0.0170(16) 0.0075(17) Ga1A 0.01685(12) 0.01779(12) 0.02339(13) -0.00098(10) 0.00824(10) 0.00108(9) O1A 0.0117(7) 0.0213(8) 0.0269(8) 0.0002(6) 0.0068(6) 0.0011(6) N1A 0.0153(10) 0.0354(13) 0.0365(14) 0.0116(10) 0.0077(10) -0.0017(8) C1A 0.0126(13) 0.0243(15) 0.033(2) -0.0003(13) 0.0058(13) 0.0009(10) C2A 0.0191(14) 0.0254(15) 0.037(2) -0.0027(14) 0.0060(13) 0.0001(11) C3A 0.0181(12) 0.0289(13) 0.0450(16) 0.0035(11) 0.0063(11) -0.0027(10) C4A 0.0151(11) 0.0302(13) 0.0275(13) 0.0024(10) 0.0062(9) -0.0005(9) C41A 0.0255(14) 0.068(2) 0.0296(15) -0.0047(13) 0.0111(12) 0.0017(13) C42A 0.0243(13) 0.0532(18) 0.0428(16) -0.0141(14) 0.0074(12) -0.0049(12) C43A 0.0241(14) 0.0477(18) 0.061(2) 0.0199(15) 0.0037(14) 0.0011(12) C11A 0.0259(12) 0.0251(12) 0.0261(13) 0.0028(10) 0.0096(10) 0.0003(10) C12A 0.0444(16) 0.0400(15) 0.0386(15) 0.0048(12) 0.0263(13) 0.0015(12) C13A 0.0349(15) 0.0592(19) 0.0310(15) 0.0117(13) 0.0068(13) 0.0060(14) C14A 0.071(2) 0.0281(15) 0.0444(18) 0.0090(13) 0.0207(16) -0.0071(14) C21A 0.0291(13) 0.0237(12) 0.0343(14) -0.0089(10) 0.0135(11) -0.0041(10) C22A 0.069(2) 0.0392(16) 0.0356(16) -0.0099(13) 0.0264(16) -0.0096(15) C23A 0.0524(18) 0.0326(15) 0.0468(18) -0.0161(13) 0.0199(15) -0.0129(13) C24A 0.0433(18) 0.0499(19) 0.070(2) -0.0242(17) 0.0174(17) 0.0154(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 O1 1.9510(14) . ? Ga1 O1A 1.9573(14) . ? Ga1 C11 2.002(2) . ? Ga1 C21 2.005(2) . ? O1 C1 1.429(2) . ? O1 Ga1A 1.9666(14) . ? N1 C3 1.455(3) . ? N1 C4 1.474(3) . ? N1 H1 0.80(3) . ? C1 C2 1.507(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.506(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C42 1.517(3) . ? C4 C41 1.520(3) . ? C4 C43 1.528(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C11 C12 1.523(3) . ? C11 C14 1.530(3) . ? C11 C13 1.534(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 C22 1.526(3) . ? C21 C23 1.530(3) . ? C21 C24 1.534(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Ga1A O1A 1.9510(14) . ? Ga1A C11A 2.006(2) . ? Ga1A C21A 2.010(2) . ? O1A C1A 1.426(3) . ? O1A C1AA 1.47(2) . ? N1A C3A 1.447(3) . ? N1A C4A 1.476(3) . ? N1A H1AA 0.69(3) . ? C1A C2A 1.512(5) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? C2A C3A 1.511(4) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C1AA C2AA 1.44(3) . ? C1AA H1A3 0.9900 . ? C1AA H1A4 0.9900 . ? C2AA C3A 1.46(2) . ? C2AA H2A3 0.9900 . ? C2AA H2A4 0.9900 . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A C43A 1.519(3) . ? C4A C41A 1.519(3) . ? C4A C42A 1.524(3) . ? C41A H41D 0.9800 . ? C41A H41E 0.9800 . ? C41A H41F 0.9800 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C43A H43D 0.9800 . ? C43A H43E 0.9800 . ? C43A H43F 0.9800 . ? C11A C14A 1.526(3) . ? C11A C12A 1.527(3) . ? C11A C13A 1.531(3) . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C21A C22A 1.521(4) . ? C21A C24A 1.523(4) . ? C21A C23A 1.526(3) . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga1 O1A 77.07(6) . . ? O1 Ga1 C11 116.72(8) . . ? O1A Ga1 C11 109.04(8) . . ? O1 Ga1 C21 112.19(8) . . ? O1A Ga1 C21 113.37(9) . . ? C11 Ga1 C21 120.36(10) . . ? C1 O1 Ga1 130.56(13) . . ? C1 O1 Ga1A 126.13(13) . . ? Ga1 O1 Ga1A 102.69(7) . . ? C3 N1 C4 117.17(19) . . ? C3 N1 H1 107(2) . . ? C4 N1 H1 110(2) . . ? O1 C1 C2 112.92(19) . . ? O1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? O1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C3 C2 C1 112.68(19) . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N1 C3 C2 111.23(19) . . ? N1 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N1 C4 C42 109.02(19) . . ? N1 C4 C41 113.4(2) . . ? C42 C4 C41 109.9(2) . . ? N1 C4 C43 105.6(2) . . ? C42 C4 C43 108.9(2) . . ? C41 C4 C43 109.8(2) . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 H42A 109.5 . . ? C4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C4 C43 H43A 109.5 . . ? C4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C12 C11 C14 108.5(2) . . ? C12 C11 C13 108.6(2) . . ? C14 C11 C13 108.1(2) . . ? C12 C11 Ga1 112.42(16) . . ? C14 C11 Ga1 111.71(17) . . ? C13 C11 Ga1 107.36(15) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C22 C21 C23 106.8(2) . . ? C22 C21 C24 109.1(2) . . ? C23 C21 C24 108.6(2) . . ? C22 C21 Ga1 112.97(17) . . ? C23 C21 Ga1 110.52(18) . . ? C24 C21 Ga1 108.77(17) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1A Ga1A O1 76.85(6) . . ? O1A Ga1A C11A 111.40(8) . . ? O1 Ga1A C11A 111.48(8) . . ? O1A Ga1A C21A 117.05(9) . . ? O1 Ga1A C21A 108.70(8) . . ? C11A Ga1A C21A 122.13(10) . . ? C1A O1A C1AA 24.4(10) . . ? C1A O1A Ga1A 127.46(14) . . ? C1AA O1A Ga1A 123.8(9) . . ? C1A O1A Ga1 128.28(15) . . ? C1AA O1A Ga1 130.1(8) . . ? Ga1A O1A Ga1 103.04(7) . . ? C3A N1A C4A 116.96(19) . . ? C3A N1A H1AA 106(3) . . ? C4A N1A H1AA 114(3) . . ? O1A C1A C2A 111.1(3) . . ? O1A C1A H1A1 109.4 . . ? C2A C1A H1A1 109.4 . . ? O1A C1A H1A2 109.4 . . ? C2A C1A H1A2 109.4 . . ? H1A1 C1A H1A2 108.0 . . ? C3A C2A C1A 114.6(3) . . ? C3A C2A H2A1 108.6 . . ? C1A C2A H2A1 108.6 . . ? C3A C2A H2A2 108.6 . . ? C1A C2A H2A2 108.6 . . ? H2A1 C2A H2A2 107.6 . . ? C2AA C1AA O1A 112.1(19) . . ? C2AA C1AA H1A3 109.2 . . ? O1A C1AA H1A3 109.2 . . ? C2AA C1AA H1A4 109.2 . . ? O1A C1AA H1A4 109.2 . . ? H1A3 C1AA H1A4 107.9 . . ? C1AA C2AA C3A 122(2) . . ? C1AA C2AA H2A3 106.9 . . ? C3A C2AA H2A3 106.9 . . ? C1AA C2AA H2A4 106.9 . . ? C3A C2AA H2A4 106.9 . . ? H2A3 C2AA H2A4 106.7 . . ? N1A C3A C2AA 115.2(8) . . ? N1A C3A C2A 112.6(2) . . ? C2AA C3A C2A 27.8(11) . . ? N1A C3A H3A1 109.1 . . ? C2AA C3A H3A1 82.8 . . ? C2A C3A H3A1 109.1 . . ? N1A C3A H3A2 109.1 . . ? C2AA C3A H3A2 127.7 . . ? C2A C3A H3A2 109.1 . . ? H3A1 C3A H3A2 107.8 . . ? N1A C4A C43A 106.71(19) . . ? N1A C4A C41A 109.2(2) . . ? C43A C4A C41A 109.3(2) . . ? N1A C4A C42A 112.7(2) . . ? C43A C4A C42A 109.3(2) . . ? C41A C4A C42A 109.6(2) . . ? C4A C41A H41D 109.5 . . ? C4A C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C4A C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C4A C42A H42D 109.5 . . ? C4A C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C4A C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C4A C43A H43D 109.5 . . ? C4A C43A H43E 109.5 . . ? H43D C43A H43E 109.5 . . ? C4A C43A H43F 109.5 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? C14A C11A C12A 107.6(2) . . ? C14A C11A C13A 108.3(2) . . ? C12A C11A C13A 108.6(2) . . ? C14A C11A Ga1A 110.57(17) . . ? C12A C11A Ga1A 112.66(17) . . ? C13A C11A Ga1A 109.05(16) . . ? C11A C12A H12D 109.5 . . ? C11A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C11A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C11A C13A H13D 109.5 . . ? C11A C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C11A C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C11A C14A H14D 109.5 . . ? C11A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C11A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C22A C21A C24A 108.5(2) . . ? C22A C21A C23A 107.8(2) . . ? C24A C21A C23A 107.9(2) . . ? C22A C21A Ga1A 112.44(17) . . ? C24A C21A Ga1A 107.41(18) . . ? C23A C21A Ga1A 112.63(16) . . ? C21A C22A H22D 109.5 . . ? C21A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C21A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C21A C23A H23D 109.5 . . ? C21A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C21A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C21A C24A H24D 109.5 . . ? C21A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C21A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1A Ga1 O1 C1 175.80(19) . . . . ? C11 Ga1 O1 C1 -79.18(19) . . . . ? C21 Ga1 O1 C1 65.6(2) . . . . ? O1A Ga1 O1 Ga1A 4.56(6) . . . . ? C11 Ga1 O1 Ga1A 109.59(9) . . . . ? C21 Ga1 O1 Ga1A -105.68(10) . . . . ? Ga1 O1 C1 C2 69.9(3) . . . . ? Ga1A O1 C1 C2 -120.66(19) . . . . ? O1 C1 C2 C3 167.0(2) . . . . ? C4 N1 C3 C2 173.6(2) . . . . ? C1 C2 C3 N1 176.3(2) . . . . ? C3 N1 C4 C42 67.3(3) . . . . ? C3 N1 C4 C41 -55.6(3) . . . . ? C3 N1 C4 C43 -175.9(2) . . . . ? O1 Ga1 C11 C12 -41.77(19) . . . . ? O1A Ga1 C11 C12 42.99(19) . . . . ? C21 Ga1 C11 C12 176.51(17) . . . . ? O1 Ga1 C11 C14 80.46(19) . . . . ? O1A Ga1 C11 C14 165.21(17) . . . . ? C21 Ga1 C11 C14 -61.3(2) . . . . ? O1 Ga1 C11 C13 -161.14(14) . . . . ? O1A Ga1 C11 C13 -76.38(17) . . . . ? C21 Ga1 C11 C13 57.14(19) . . . . ? O1 Ga1 C21 C22 -1.3(2) . . . . ? O1A Ga1 C21 C22 -86.33(19) . . . . ? C11 Ga1 C21 C22 141.97(18) . . . . ? O1 Ga1 C21 C23 -120.90(18) . . . . ? O1A Ga1 C21 C23 154.10(18) . . . . ? C11 Ga1 C21 C23 22.4(2) . . . . ? O1 Ga1 C21 C24 120.02(18) . . . . ? O1A Ga1 C21 C24 35.0(2) . . . . ? C11 Ga1 C21 C24 -96.7(2) . . . . ? C1 O1 Ga1A O1A -176.34(18) . . . . ? Ga1 O1 Ga1A O1A -4.58(6) . . . . ? C1 O1 Ga1A C11A -68.24(18) . . . . ? Ga1 O1 Ga1A C11A 103.52(9) . . . . ? C1 O1 Ga1A C21A 69.21(18) . . . . ? Ga1 O1 Ga1A C21A -119.04(9) . . . . ? O1 Ga1A O1A C1A 172.7(3) . . . . ? C11A Ga1A O1A C1A 64.5(3) . . . . ? C21A Ga1A O1A C1A -82.8(3) . . . . ? O1 Ga1A O1A C1AA -157.5(13) . . . . ? C11A Ga1A O1A C1AA 94.3(13) . . . . ? C21A Ga1A O1A C1AA -53.0(13) . . . . ? O1 Ga1A O1A Ga1 4.57(6) . . . . ? C11A Ga1A O1A Ga1 -103.62(9) . . . . ? C21A Ga1A O1A Ga1 109.07(9) . . . . ? O1 Ga1 O1A C1A -172.6(3) . . . . ? C11 Ga1 O1A C1A 73.3(3) . . . . ? C21 Ga1 O1A C1A -63.7(3) . . . . ? O1 Ga1 O1A C1AA 155.9(15) . . . . ? C11 Ga1 O1A C1AA 41.8(15) . . . . ? C21 Ga1 O1A C1AA -95.3(15) . . . . ? O1 Ga1 O1A Ga1A -4.61(6) . . . . ? C11 Ga1 O1A Ga1A -118.73(9) . . . . ? C21 Ga1 O1A Ga1A 104.23(9) . . . . ? C1AA O1A C1A C2A -58(2) . . . . ? Ga1A O1A C1A C2A 32.7(5) . . . . ? Ga1 O1A C1A C2A -162.1(3) . . . . ? O1A C1A C2A C3A -173.1(2) . . . . ? C1A O1A C1AA C2AA 52(3) . . . . ? Ga1A O1A C1AA C2AA -55(3) . . . . ? Ga1 O1A C1AA C2AA 147.9(17) . . . . ? O1A C1AA C2AA C3A 171.5(14) . . . . ? C4A N1A C3A C2AA 163.1(14) . . . . ? C4A N1A C3A C2A -166.6(3) . . . . ? C1AA C2AA C3A N1A 33(3) . . . . ? C1AA C2AA C3A C2A -58(3) . . . . ? C1A C2A C3A N1A -60.2(5) . . . . ? C1A C2A C3A C2AA 41.4(18) . . . . ? C3A N1A C4A C43A -177.5(2) . . . . ? C3A N1A C4A C41A -59.4(3) . . . . ? C3A N1A C4A C42A 62.5(3) . . . . ? O1A Ga1A C11A C14A -119.29(18) . . . . ? O1 Ga1A C11A C14A 156.94(17) . . . . ? C21A Ga1A C11A C14A 26.1(2) . . . . ? O1A Ga1A C11A C12A 1.1(2) . . . . ? O1 Ga1A C11A C12A -82.68(18) . . . . ? C21A Ga1A C11A C12A 146.48(17) . . . . ? O1A Ga1A C11A C13A 121.75(17) . . . . ? O1 Ga1A C11A C13A 37.97(19) . . . . ? C21A Ga1A C11A C13A -92.87(19) . . . . ? O1A Ga1A C21A C22A -35.4(2) . . . . ? O1 Ga1A C21A C22A 49.0(2) . . . . ? C11A Ga1A C21A C22A -178.98(17) . . . . ? O1A Ga1A C21A C24A -154.72(17) . . . . ? O1 Ga1A C21A C24A -70.3(2) . . . . ? C11A Ga1A C21A C24A 61.7(2) . . . . ? O1A Ga1A C21A C23A 86.7(2) . . . . ? O1 Ga1A C21A C23A 171.10(17) . . . . ? C11A Ga1A C21A C23A -56.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.11 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.595 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.081 #===END data_5a _database_code_depnum_ccdc_archive 'CCDC 694712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis{mu2-O-[2,2-dimethyl-3-methylamino-1-propanolato-O,N-] tetramethyldialuminium} ; _chemical_name_common ; Bis(mu2-O-(2,2-dimethyl-3-methylamino-1-propanolato-O,N-) tetramethyldialuminium) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H40 Al2 N2 O2' _chemical_formula_weight 346.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4522(17) _cell_length_b 11.701(2) _cell_length_c 11.483(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.59(3) _cell_angle_gamma 90.00 _cell_volume 1063.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 947 _cell_measurement_theta_min 5.59 _cell_measurement_theta_max 70.17 _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 1.290 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.411 _exptl_absorpt_correction_T_max 0.835 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'goebel mirror' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5987 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 5.59 _diffrn_reflns_theta_max 70.17 _reflns_number_total 1959 _reflns_number_gt 1714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT and SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3, L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0913P)^2^+1.0115P] 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 1959 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.15250(8) 0.03455(6) 0.60784(6) 0.0171(3) Uani 1 1 d . . . N1 N 0.1622(2) 0.10004(19) 0.7887(2) 0.0205(5) Uani 1 1 d . . . H1 H 0.153(4) 0.172(3) 0.773(3) 0.033(9) Uiso 1 1 d . . . O1 O -0.0753(2) 0.01409(15) 0.56704(15) 0.0192(4) Uani 1 1 d . . . C1 C -0.1787(3) -0.0036(2) 0.6395(2) 0.0232(5) Uani 1 1 d . . . H1A H -0.1591 -0.0792 0.6735 0.028 Uiso 1 1 calc R . . H1B H -0.295 0.0009 0.5861 0.028 Uiso 1 1 calc R . . C2 C -0.1487(3) 0.0813(2) 0.7455(2) 0.0226(6) Uani 1 1 d . . . C3 C 0.0300(3) 0.0673(2) 0.8389(2) 0.0235(6) Uani 1 1 d . . . H3A H 0.0424 0.1148 0.9131 0.028 Uiso 1 1 calc R . . H3B H 0.0471 -0.0136 0.8662 0.028 Uiso 1 1 calc R . . C4 C 0.3299(3) 0.0877(3) 0.8865(2) 0.0285(6) Uani 1 1 d . . . H4A H 0.3345 0.1334 0.9581 0.043 Uiso 1 1 calc R . . H4B H 0.4163 0.1135 0.8550 0.043 Uiso 1 1 calc R . . H4C H 0.3493 0.0081 0.9108 0.043 Uiso 1 1 calc R . . C5 C -0.1822(3) 0.2034(2) 0.6967(3) 0.0298(6) Uani 1 1 d . . . H5A H -0.109 0.2213 0.649 0.045 Uiso 1 1 calc R . . H5B H -0.158 0.2568 0.7673 0.045 Uiso 1 1 calc R . . H5C H -0.302 0.2110 0.6425 0.045 Uiso 1 1 calc R . . C6 C -0.2718(3) 0.0503(3) 0.8119(3) 0.0336(7) Uani 1 1 d . . . H6A H -0.250 -0.0299 0.844 0.050 Uiso 1 1 calc R . . H6B H -0.391 0.0567 0.7521 0.050 Uiso 1 1 calc R . . H6C H -0.255 0.1038 0.883 0.050 Uiso 1 1 calc R . . C11 C 0.2899(3) -0.1041(2) 0.6708(3) 0.0262(6) Uani 1 1 d . . . H11A H 0.354 -0.1201 0.6211 0.039 Uiso 1 1 calc R . . H11B H 0.2187 -0.1658 0.6682 0.039 Uiso 1 1 calc R . . H11C H 0.362 -0.0920 0.7526 0.039 Uiso 1 1 calc R . . C21 C 0.2502(3) 0.1831(2) 0.5792(3) 0.0267(6) Uani 1 1 d . . . H21A H 0.312 0.1713 0.5297 0.040 Uiso 1 1 calc R . . H21B H 0.318 0.2123 0.6533 0.040 Uiso 1 1 calc R . . H21C H 0.1652 0.2330 0.542 0.040 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 0.0156(4) 0.0171(4) 0.0207(4) 0.0000(2) 0.0089(3) -0.0001(2) N1 0.0163(9) 0.0219(11) 0.0239(11) -0.0003(8) 0.0079(8) 0.0005(8) O1 0.0173(8) 0.0240(9) 0.0194(9) -0.0015(7) 0.0104(7) -0.0023(6) C1 0.0220(11) 0.0255(13) 0.0281(13) -0.0025(10) 0.0163(10) -0.0051(10) C2 0.0199(11) 0.0264(13) 0.0257(13) -0.0040(10) 0.0132(10) -0.0022(9) C3 0.0233(12) 0.0287(14) 0.0214(13) -0.0012(10) 0.0116(10) -0.0007(10) C4 0.0184(11) 0.0382(16) 0.0270(14) -0.0042(11) 0.0056(10) 0.0020(10) C5 0.0228(12) 0.0280(14) 0.0395(16) -0.0053(12) 0.0121(11) 0.0033(10) C6 0.0284(13) 0.0485(18) 0.0320(15) -0.0120(13) 0.0206(12) -0.0091(12) C11 0.0265(12) 0.0229(12) 0.0284(14) 0.0016(10) 0.0086(10) 0.0051(10) C21 0.0311(13) 0.0236(13) 0.0309(14) -0.0008(10) 0.0178(11) -0.0040(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.8300(17) . ? Al1 O1 1.9649(18) 3_556 ? Al1 C11 1.978(3) . ? Al1 C21 2.000(3) . ? Al1 N1 2.188(2) . ? Al1 Al1 2.9903(17) 3_556 ? N1 C4 1.474(3) . ? N1 C3 1.477(3) . ? N1 H1 0.86(4) . ? O1 C1 1.418(3) . ? O1 Al1 1.9649(18) 3_556 ? C1 C2 1.522(3) . ? C1 H1A 0.9580 . ? C1 H1B 0.9580 . ? C2 C3 1.523(3) . ? C2 C5 1.524(4) . ? C2 C6 1.534(3) . ? C3 H3A 0.9919 . ? C3 H3B 0.9919 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9870 . ? C5 H5B 0.9870 . ? C5 H5C 0.9870 . ? C6 H6A 1.0006 . ? C6 H6B 1.0006 . ? C6 H6C 1.0006 . ? C11 H11A 0.9334 . ? C11 H11B 0.9334 . ? C11 H11C 0.9334 . ? C21 H21A 0.9081 . ? C21 H21B 0.9081 . ? C21 H21C 0.9081 . ? 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 O1 Al1 O1 76.06(8) . 3_556 ? O1 Al1 C11 114.58(10) . . ? O1 Al1 C11 94.41(10) 3_556 . ? O1 Al1 C21 121.97(10) . . ? O1 Al1 C21 95.25(10) 3_556 . ? C11 Al1 C21 123.32(11) . . ? O1 Al1 N1 88.48(8) . . ? O1 Al1 N1 163.66(7) 3_556 . ? C11 Al1 N1 96.87(10) . . ? C21 Al1 N1 88.39(10) . . ? O1 Al1 Al1 39.62(6) . 3_556 ? O1 Al1 Al1 36.44(5) 3_556 3_556 ? C11 Al1 Al1 107.76(9) . 3_556 ? C21 Al1 Al1 112.59(9) . 3_556 ? N1 Al1 Al1 127.90(6) . 3_556 ? C4 N1 C3 109.5(2) . . ? C4 N1 Al1 113.19(15) . . ? C3 N1 Al1 119.93(16) . . ? C4 N1 H1 104(2) . . ? C3 N1 H1 108(2) . . ? Al1 N1 H1 100(2) . . ? C1 O1 Al1 132.78(15) . . ? C1 O1 Al1 120.36(14) . 3_556 ? Al1 O1 Al1 103.94(8) . 3_556 ? O1 C1 C2 114.2(2) . . ? O1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? O1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C1 C2 C3 109.7(2) . . ? C1 C2 C5 111.1(2) . . ? C3 C2 C5 111.7(2) . . ? C1 C2 C6 107.0(2) . . ? C3 C2 C6 107.6(2) . . ? C5 C2 C6 109.5(2) . . ? N1 C3 C2 113.3(2) . . ? N1 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? N1 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Al1 C11 H11A 109.5 . . ? Al1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Al1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Al1 C21 H21A 109.5 . . ? Al1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Al1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Al1 N1 C4 155.49(18) . . . . ? O1 Al1 N1 C4 174.3(3) 3_556 . . . ? C11 Al1 N1 C4 40.9(2) . . . . ? C21 Al1 N1 C4 -82.46(19) . . . . ? Al1 Al1 N1 C4 159.81(15) 3_556 . . . ? O1 Al1 N1 C3 23.73(19) . . . . ? O1 Al1 N1 C3 42.5(4) 3_556 . . . ? C11 Al1 N1 C3 -90.8(2) . . . . ? C21 Al1 N1 C3 145.8(2) . . . . ? Al1 Al1 N1 C3 28.1(2) 3_556 . . . ? O1 Al1 O1 C1 159.9(3) 3_556 . . . ? C11 Al1 O1 C1 71.4(2) . . . . ? C21 Al1 O1 C1 -112.6(2) . . . . ? N1 Al1 O1 C1 -25.4(2) . . . . ? Al1 Al1 O1 C1 159.9(3) 3_556 . . . ? O1 Al1 O1 Al1 0.0 3_556 . . 3_556 ? C11 Al1 O1 Al1 -88.49(12) . . . 3_556 ? C21 Al1 O1 Al1 87.50(12) . . . 3_556 ? N1 Al1 O1 Al1 174.65(9) . . . 3_556 ? Al1 O1 C1 C2 49.7(3) . . . . ? Al1 O1 C1 C2 -153.01(17) 3_556 . . . ? O1 C1 C2 C3 -64.2(3) . . . . ? O1 C1 C2 C5 59.8(3) . . . . ? O1 C1 C2 C6 179.3(2) . . . . ? C4 N1 C3 C2 178.0(2) . . . . ? Al1 N1 C3 C2 -48.7(3) . . . . ? C1 C2 C3 N1 66.8(3) . . . . ? C5 C2 C3 N1 -57.0(3) . . . . ? C6 C2 C3 N1 -177.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 70.17 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.563 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.088 #===END data_6a _database_code_depnum_ccdc_archive 'CCDC 694713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [3-tert.-Butylamino-2,2-dimethyl-1-propanolato-O,N]- dimethylaluminium-O-trimethylaluminium adduct ; _chemical_name_common ; (3-tert.-Butylamino-2,2-dimethyl-1-propanolato-O,N)- dimethylaluminium-O-trimethylaluminium adduct ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H35 Al2 N O' _chemical_formula_weight 287.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.393(3) _cell_length_b 22.611(5) _cell_length_c 14.830(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.20(3) _cell_angle_gamma 90.00 _cell_volume 3847.6(13) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1853 _cell_measurement_theta_min 4.43 _cell_measurement_theta_max 25.60 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.992 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.144 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'STOE IPDS-1' _diffrn_measurement_method '\phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39303 _diffrn_reflns_av_R_equivalents 0.2213 _diffrn_reflns_av_sigmaI/netI 0.1148 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.43 _diffrn_reflns_theta_max 25.60 _reflns_number_total 7107 _reflns_number_gt 4978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS-1 software package' _computing_cell_refinement 'X-Area (STOE 2003)' _computing_data_reduction 'X-Area (STOE 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0001P)^2^+10.6701P] 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 7107 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1675 _refine_ls_R_factor_gt 0.1203 _refine_ls_wR_factor_ref 0.2236 _refine_ls_wR_factor_gt 0.2045 _refine_ls_goodness_of_fit_ref 1.250 _refine_ls_restrained_S_all 1.250 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al -0.36538(14) 0.08170(8) 0.16252(11) 0.0288(4) Uani 1 1 d . . . O1 O -0.3062(3) 0.14695(16) 0.2385(2) 0.0288(8) Uani 1 1 d . . . N1 N -0.2917(4) 0.0231(2) 0.2722(3) 0.0304(11) Uani 1 1 d . . . H1 H -0.215(5) 0.022(3) 0.282(4) 0.037(17) Uiso 1 1 d . . . C1 C -0.1974(5) 0.1369(3) 0.3184(4) 0.0293(12) Uani 1 1 d . . . H1B H -0.1618 0.1745 0.3434 0.035 Uiso 1 1 calc R . . H1C H -0.145 0.1157 0.2950 0.035 Uiso 1 1 calc R . . Al2 Al -0.32733(16) 0.22633(8) 0.19281(13) 0.0360(4) Uani 1 1 d . . . C2 C -0.2119(5) 0.1018(3) 0.4007(4) 0.0328(13) Uani 1 1 d . . . C3 C -0.2990(6) 0.0509(3) 0.3607(4) 0.0369(14) Uani 1 1 d . . . H3A H -0.2826 0.0176 0.416 0.044 Uiso 1 1 calc R . . H3B H -0.386 0.0674 0.3434 0.044 Uiso 1 1 calc R . . C6 C -0.0928(6) 0.0789(3) 0.4679(4) 0.0466(17) Uani 1 1 d . . . H6A H -0.064 0.0489 0.4322 0.070 Uiso 1 1 calc R . . H6B H -0.0997 0.0599 0.527 0.070 Uiso 1 1 calc R . . H6C H -0.036 0.1129 0.489 0.070 Uiso 1 1 calc R . . C5 C -0.2618(6) 0.1421(3) 0.4593(4) 0.0448(16) Uani 1 1 d . . . H5A H -0.280 0.1172 0.510 0.067 Uiso 1 1 calc R . . H5B H -0.337 0.1619 0.4128 0.067 Uiso 1 1 calc R . . H5C H -0.202 0.1740 0.495 0.067 Uiso 1 1 calc R . . C4 C -0.3259(6) -0.0430(3) 0.2596(4) 0.0394(15) Uani 1 1 d . . . C41 C -0.4424(6) -0.0516(3) 0.2689(6) 0.057(2) Uani 1 1 d . . . H41A H -0.468 -0.0957 0.255 0.086 Uiso 1 1 calc R . . H41B H -0.505 -0.0245 0.219 0.086 Uiso 1 1 calc R . . H41C H -0.4349 -0.041 0.339 0.086 Uiso 1 1 calc R . . C42 C -0.2317(6) -0.0777(3) 0.3383(5) 0.0550(19) Uani 1 1 d . . . H42A H -0.152 -0.0721 0.330 0.083 Uiso 1 1 calc R . . H42B H -0.254 -0.1226 0.332 0.083 Uiso 1 1 calc R . . H42C H -0.225 -0.0623 0.407 0.083 Uiso 1 1 calc R . . C43 C -0.3305(7) -0.0619(3) 0.1604(5) 0.0552(19) Uani 1 1 d . . . H43A H -0.253 -0.053 0.1548 0.083 Uiso 1 1 calc R . . H43B H -0.395 -0.0397 0.108 0.083 Uiso 1 1 calc R . . H43C H -0.346 -0.1058 0.1518 0.083 Uiso 1 1 calc R . . C31 C -0.4680(6) 0.2267(4) 0.0718(6) 0.065(2) Uani 1 1 d . . . H31A H -0.537 0.217 0.0871 0.098 Uiso 1 1 calc R . . H31B H -0.459 0.197 0.026 0.098 Uiso 1 1 calc R . . H31C H -0.478 0.2662 0.042 0.098 Uiso 1 1 calc R . . C32 C -0.1809(6) 0.2427(3) 0.1715(5) 0.0496(18) Uani 1 1 d . . . H32A H -0.165 0.2114 0.139 0.074 Uiso 1 1 calc R . . H32B H -0.120 0.248 0.231 0.074 Uiso 1 1 calc R . . H32C H -0.1899 0.2766 0.135 0.074 Uiso 1 1 calc R . . C33 C -0.3441(7) 0.2741(3) 0.2986(6) 0.062(2) Uani 1 1 d . . . H33A H -0.404 0.2580 0.316 0.094 Uiso 1 1 calc R . . H33B H -0.363 0.3135 0.2770 0.094 Uiso 1 1 calc R . . H33C H -0.273 0.2736 0.353 0.094 Uiso 1 1 calc R . . C11 C -0.2903(6) 0.0756(3) 0.0688(4) 0.0496(18) Uani 1 1 d . . . H11A H -0.304 0.1085 0.033 0.074 Uiso 1 1 calc R . . H11B H -0.319 0.0446 0.030 0.074 Uiso 1 1 calc R . . H11C H -0.214 0.071 0.1004 0.074 Uiso 1 1 calc R . . C21 C -0.5351(5) 0.0782(3) 0.1225(5) 0.0477(17) Uani 1 1 d . . . H21A H -0.5709 0.1113 0.079 0.072 Uiso 1 1 calc R . . H21B H -0.5554 0.081 0.180 0.072 Uiso 1 1 calc R . . H21C H -0.5641 0.0407 0.089 0.072 Uiso 1 1 calc R . . Al1A Al 0.22034(14) 0.15773(7) 0.30090(10) 0.0254(4) Uani 1 1 d . . . Al2A Al 0.17532(16) 0.01538(7) 0.25643(12) 0.0309(4) Uani 1 1 d . . . O1A O 0.1632(3) 0.09578(15) 0.2171(2) 0.0259(8) Uani 1 1 d . . . N1A N 0.1532(4) 0.21972(19) 0.1951(3) 0.0227(9) Uani 1 1 d . . . H1A H 0.088(5) 0.221(3) 0.189(4) 0.022(16) Uiso 1 1 d . . . C1A C 0.0594(5) 0.1080(2) 0.1317(3) 0.0274(12) Uani 1 1 d . . . H1D H 0.005 0.1275 0.1511 0.033 Uiso 1 1 calc R . . H1E H 0.0263 0.0721 0.1025 0.033 Uiso 1 1 calc R . . C2A C 0.0845(5) 0.1459(2) 0.0575(3) 0.0269(12) Uani 1 1 d . . . C3A C 0.1722(5) 0.1955(2) 0.1086(3) 0.0267(12) Uani 1 1 d . . . H3C H 0.252 0.1798 0.1295 0.032 Uiso 1 1 calc R . . H3D H 0.1644 0.2278 0.0619 0.032 Uiso 1 1 calc R . . C6A C -0.0300(5) 0.1732(3) -0.0103(4) 0.0359(14) Uani 1 1 d . . . H6D H -0.060 0.2019 0.0284 0.054 Uiso 1 1 calc R . . H6E H -0.090 0.1404 -0.040 0.054 Uiso 1 1 calc R . . H6F H -0.0166 0.1958 -0.065 0.054 Uiso 1 1 calc R . . C5A C 0.1385(5) 0.1092(3) -0.0016(4) 0.0357(14) Uani 1 1 d . . . H5D H 0.081 0.0801 -0.041 0.053 Uiso 1 1 calc R . . H5E H 0.208 0.0885 0.0429 0.053 Uiso 1 1 calc R . . H5F H 0.161 0.1353 -0.044 0.053 Uiso 1 1 calc R . . C4A C 0.1834(5) 0.2855(2) 0.2167(4) 0.0281(12) Uani 1 1 d . . . C41A C 0.3059(5) 0.2966(3) 0.2202(4) 0.0346(13) Uani 1 1 d . . . H41D H 0.3085 0.2884 0.156 0.052 Uiso 1 1 calc R . . H41E H 0.361 0.2706 0.269 0.052 Uiso 1 1 calc R . . H41F H 0.3273 0.3379 0.238 0.052 Uiso 1 1 calc R . . C42A C 0.1746(5) 0.2990(3) 0.3145(4) 0.0368(14) Uani 1 1 d . . . H42D H 0.188 0.3400 0.3284 0.055 Uiso 1 1 calc R . . H42E H 0.232 0.2768 0.3643 0.055 Uiso 1 1 calc R . . H42F H 0.099 0.2887 0.3118 0.055 Uiso 1 1 calc R . . C43A C 0.0938(5) 0.3227(3) 0.1366(5) 0.0399(15) Uani 1 1 d . . . H43D H 0.098 0.3134 0.074 0.060 Uiso 1 1 calc R . . H43E H 0.110 0.3646 0.1509 0.060 Uiso 1 1 calc R . . H43F H 0.016 0.3137 0.134 0.060 Uiso 1 1 calc R . . C31A C 0.3074(6) 0.0120(3) 0.3822(5) 0.0531(19) Uani 1 1 d . . . H31D H 0.377 0.021 0.3730 0.080 Uiso 1 1 calc R . . H31E H 0.312 -0.0262 0.409 0.080 Uiso 1 1 calc R . . H31F H 0.296 0.040 0.425 0.080 Uiso 1 1 calc R . . C32A C 0.1994(6) -0.0295(3) 0.1526(5) 0.0471(17) Uani 1 1 d . . . H32D H 0.267 -0.0169 0.146 0.071 Uiso 1 1 calc R . . H32E H 0.137 -0.0237 0.095 0.071 Uiso 1 1 calc R . . H32F H 0.206 -0.0691 0.1679 0.071 Uiso 1 1 calc R . . C33A C 0.0231(6) -0.0029(3) 0.2661(5) 0.0472(17) Uani 1 1 d . . . H33D H -0.039 0.0044 0.204 0.071 Uiso 1 1 calc R . . H33E H 0.0126 0.0220 0.315 0.071 Uiso 1 1 calc R . . H33F H 0.0218 -0.0441 0.284 0.071 Uiso 1 1 calc R . . C11A C 0.3903(5) 0.1610(3) 0.3499(4) 0.0411(15) Uani 1 1 d . . . H11D H 0.4217 0.1267 0.387 0.062 Uiso 1 1 calc R . . H11E H 0.4168 0.1951 0.389 0.062 Uiso 1 1 calc R . . H11F H 0.4149 0.1628 0.2967 0.062 Uiso 1 1 calc R . . C21A C 0.1387(6) 0.1599(3) 0.3898(4) 0.0422(16) Uani 1 1 d . . . H21D H 0.133 0.1217 0.411 0.063 Uiso 1 1 calc R . . H21E H 0.064 0.1754 0.3579 0.063 Uiso 1 1 calc R . . H21F H 0.180 0.1835 0.443 0.063 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 0.0310(9) 0.0296(9) 0.0233(8) -0.0024(7) 0.0075(7) -0.0023(7) O1 0.031(2) 0.028(2) 0.0255(18) 0.0038(16) 0.0073(15) 0.0003(17) N1 0.034(3) 0.023(3) 0.035(3) -0.002(2) 0.015(2) -0.004(2) C1 0.030(3) 0.031(3) 0.029(3) 0.001(2) 0.014(2) 0.002(2) Al2 0.0377(10) 0.0253(9) 0.0493(11) 0.0048(8) 0.0211(8) 0.0038(8) C2 0.036(3) 0.038(3) 0.025(3) -0.004(2) 0.011(2) -0.002(3) C3 0.056(4) 0.034(3) 0.027(3) -0.001(2) 0.023(3) -0.007(3) C6 0.047(4) 0.058(5) 0.032(3) 0.014(3) 0.012(3) 0.006(3) C5 0.060(4) 0.045(4) 0.035(3) -0.004(3) 0.024(3) -0.001(3) C4 0.056(4) 0.018(3) 0.049(4) -0.002(3) 0.024(3) -0.007(3) C41 0.054(4) 0.036(4) 0.092(5) 0.001(4) 0.038(4) -0.010(3) C42 0.068(5) 0.030(4) 0.067(5) 0.010(3) 0.025(4) 0.008(3) C43 0.075(5) 0.030(4) 0.065(5) -0.017(3) 0.032(4) -0.005(3) C31 0.054(4) 0.052(5) 0.078(5) 0.029(4) 0.011(4) 0.012(4) C32 0.059(4) 0.032(4) 0.072(5) 0.014(3) 0.041(4) 0.003(3) C33 0.070(5) 0.039(4) 0.096(6) -0.010(4) 0.052(5) 0.001(4) C11 0.065(5) 0.048(4) 0.039(3) 0.000(3) 0.024(3) -0.001(4) C21 0.038(4) 0.048(4) 0.050(4) -0.003(3) 0.008(3) -0.006(3) Al1A 0.0319(9) 0.0222(8) 0.0174(7) -0.0007(6) 0.0041(6) -0.0024(7) Al2A 0.0432(10) 0.0199(9) 0.0302(8) 0.0048(7) 0.0145(7) 0.0019(8) O1A 0.034(2) 0.0204(19) 0.0192(17) 0.0011(14) 0.0055(15) 0.0021(16) N1A 0.028(3) 0.016(2) 0.023(2) -0.0008(17) 0.0090(19) 0.000(2) C1A 0.031(3) 0.024(3) 0.023(3) -0.002(2) 0.005(2) -0.004(2) C2A 0.034(3) 0.026(3) 0.015(2) -0.002(2) 0.003(2) -0.005(2) C3A 0.029(3) 0.028(3) 0.021(2) 0.004(2) 0.007(2) -0.003(2) C6A 0.037(3) 0.034(3) 0.024(3) 0.001(2) -0.003(2) 0.003(3) C5A 0.048(4) 0.032(3) 0.026(3) -0.006(2) 0.013(3) -0.001(3) C4A 0.033(3) 0.021(3) 0.032(3) -0.003(2) 0.013(2) -0.007(2) C41A 0.039(3) 0.025(3) 0.038(3) -0.003(2) 0.012(3) -0.008(3) C42A 0.050(4) 0.024(3) 0.038(3) -0.011(2) 0.019(3) -0.008(3) C43A 0.042(3) 0.024(3) 0.052(4) 0.007(3) 0.016(3) 0.000(3) C31A 0.067(5) 0.038(4) 0.049(4) 0.011(3) 0.016(3) 0.004(4) C32A 0.054(4) 0.032(4) 0.057(4) -0.002(3) 0.023(3) 0.002(3) C33A 0.055(4) 0.046(4) 0.048(4) 0.007(3) 0.028(3) -0.007(3) C11A 0.039(3) 0.032(3) 0.040(3) 0.002(3) 0.000(3) -0.002(3) C21A 0.063(4) 0.032(3) 0.032(3) 0.004(3) 0.017(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.833(4) . ? Al1 C11 1.947(6) . ? Al1 C21 1.960(6) . ? Al1 N1 2.028(5) . ? O1 C1 1.438(6) . ? O1 Al2 1.901(4) . ? N1 C3 1.487(7) . ? N1 C4 1.546(7) . ? N1 H1 0.91(6) . ? C1 C2 1.522(7) . ? C1 H1B 0.9655 . ? C1 H1C 0.9655 . ? Al2 C31 1.974(7) . ? Al2 C33 1.978(7) . ? Al2 C32 1.991(7) . ? C2 C6 1.526(8) . ? C2 C3 1.537(8) . ? C2 C5 1.540(8) . ? C3 H3A 1.0777 . ? C3 H3B 1.0777 . ? C6 H6A 1.0066 . ? C6 H6B 1.0066 . ? C6 H6C 1.0066 . ? C5 H5A 1.0266 . ? C5 H5B 1.0266 . ? C5 H5C 1.0266 . ? C4 C41 1.513(9) . ? C4 C43 1.513(9) . ? C4 C42 1.520(9) . ? C41 H41A 1.0427 . ? C41 H41B 1.0427 . ? C41 H41C 1.0427 . ? C42 H42A 1.0456 . ? C42 H42B 1.0456 . ? C42 H42C 1.0456 . ? C43 H43A 1.0099 . ? C43 H43B 1.0099 . ? C43 H43C 1.0099 . ? C31 H31A 0.9844 . ? C31 H31B 0.9844 . ? C31 H31C 0.9844 . ? C32 H32A 0.9206 . ? C32 H32B 0.9206 . ? C32 H32C 0.9206 . ? C33 H33A 0.9461 . ? C33 H33B 0.9461 . ? C33 H33C 0.9461 . ? C11 H11A 0.8913 . ? C11 H11B 0.8913 . ? C11 H11C 0.8913 . ? C21 H21A 0.9816 . ? C21 H21B 0.9816 . ? C21 H21C 0.9816 . ? Al1A O1A 1.828(4) . ? Al1A C21A 1.942(6) . ? Al1A C11A 1.953(6) . ? Al1A N1A 2.033(5) . ? Al2A O1A 1.898(4) . ? Al2A C32A 1.959(7) . ? Al2A C31A 1.964(7) . ? Al2A C33A 1.988(7) . ? O1A C1A 1.451(6) . ? N1A C3A 1.492(7) . ? N1A C4A 1.538(6) . ? N1A H1A 0.78(5) . ? C1A C2A 1.517(7) . ? C1A H1D 0.9385 . ? C1A H1E 0.9385 . ? C2A C6A 1.526(7) . ? C2A C5A 1.533(8) . ? C2A C3A 1.546(7) . ? C3A H3C 0.9857 . ? C3A H3D 0.9857 . ? C6A H6D 1.0258 . ? C6A H6E 1.0258 . ? C6A H6F 1.0258 . ? C5A H5D 0.9812 . ? C5A H5E 0.9812 . ? C5A H5F 0.9812 . ? C4A C41A 1.519(8) . ? C4A C43A 1.534(8) . ? C4A C42A 1.527(7) . ? C41A H41D 0.9797 . ? C41A H41E 0.9797 . ? C41A H41F 0.9797 . ? C42A H42D 0.9495 . ? C42A H42E 0.9495 . ? C42A H42F 0.9495 . ? C43A H43D 0.9756 . ? C43A H43E 0.9756 . ? C43A H43F 0.9756 . ? C31A H31D 0.9445 . ? C31A H31E 0.9445 . ? C31A H31F 0.9445 . ? C32A H32D 0.9192 . ? C32A H32E 0.9192 . ? C32A H32F 0.9192 . ? C33A H33D 0.9703 . ? C33A H33E 0.9703 . ? C33A H33F 0.9703 . ? C11A H11D 0.9485 . ? C11A H11E 0.9485 . ? C11A H11F 0.9485 . ? C21A H21D 0.9298 . ? C21A H21E 0.9298 . ? C21A H21F 0.9298 . ? 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 O1 Al1 C11 107.9(3) . . ? O1 Al1 C21 110.7(2) . . ? C11 Al1 C21 121.9(3) . . ? O1 Al1 N1 94.51(18) . . ? C11 Al1 N1 109.6(3) . . ? C21 Al1 N1 108.8(3) . . ? C1 O1 Al1 114.3(3) . . ? C1 O1 Al2 113.8(3) . . ? Al1 O1 Al2 124.87(19) . . ? C3 N1 C4 114.2(4) . . ? C3 N1 Al1 105.8(4) . . ? C4 N1 Al1 121.0(4) . . ? C3 N1 H1 107(4) . . ? C4 N1 H1 102(4) . . ? Al1 N1 H1 106(4) . . ? O1 C1 C2 112.7(4) . . ? O1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? O1 C1 H1C 109.1 . . ? C2 C1 H1C 109.1 . . ? H1B C1 H1C 107.8 . . ? O1 Al2 C31 106.5(3) . . ? O1 Al2 C33 105.9(3) . . ? C31 Al2 C33 113.4(4) . . ? O1 Al2 C32 102.8(2) . . ? C31 Al2 C32 113.5(3) . . ? C33 Al2 C32 113.5(3) . . ? C1 C2 C6 108.8(5) . . ? C1 C2 C3 111.0(4) . . ? C6 C2 C3 111.3(5) . . ? C1 C2 C5 109.8(5) . . ? C6 C2 C5 109.1(5) . . ? C3 C2 C5 106.8(5) . . ? N1 C3 C2 112.9(5) . . ? N1 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? N1 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C41 C4 C43 111.5(6) . . ? C41 C4 C42 110.2(6) . . ? C43 C4 C42 109.7(6) . . ? C41 C4 N1 109.9(5) . . ? C43 C4 N1 107.4(5) . . ? C42 C4 N1 108.1(5) . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 H42A 109.5 . . ? C4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C4 C43 H43A 109.5 . . ? C4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Al2 C31 H31A 109.5 . . ? Al2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Al2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Al2 C32 H32A 109.5 . . ? Al2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Al2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Al2 C33 H33A 109.5 . . ? Al2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Al2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Al1 C11 H11A 109.5 . . ? Al1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Al1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Al1 C21 H21A 109.5 . . ? Al1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Al1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1A Al1A C21A 108.3(2) . . ? O1A Al1A C11A 111.6(2) . . ? C21A Al1A C11A 120.8(3) . . ? O1A Al1A N1A 93.62(17) . . ? C21A Al1A N1A 109.9(2) . . ? C11A Al1A N1A 109.3(2) . . ? O1A Al2A C32A 105.8(2) . . ? O1A Al2A C31A 105.6(2) . . ? C32A Al2A C31A 114.0(3) . . ? O1A Al2A C33A 104.7(2) . . ? C32A Al2A C33A 112.3(3) . . ? C31A Al2A C33A 113.4(3) . . ? C1A O1A Al1A 115.8(3) . . ? C1A O1A Al2A 113.1(3) . . ? Al1A O1A Al2A 124.04(19) . . ? C3A N1A C4A 115.3(4) . . ? C3A N1A Al1A 105.0(3) . . ? C4A N1A Al1A 120.6(3) . . ? C3A N1A H1A 114(4) . . ? C4A N1A H1A 99(4) . . ? Al1A N1A H1A 102(4) . . ? O1A C1A C2A 112.5(4) . . ? O1A C1A H1D 109.1 . . ? C2A C1A H1D 109.1 . . ? O1A C1A H1E 109.1 . . ? C2A C1A H1E 109.1 . . ? H1D C1A H1E 107.8 . . ? C1A C2A C6A 108.1(5) . . ? C1A C2A C5A 111.2(5) . . ? C6A C2A C5A 110.0(4) . . ? C1A C2A C3A 110.6(4) . . ? C6A C2A C3A 109.6(5) . . ? C5A C2A C3A 107.3(5) . . ? N1A C3A C2A 112.2(4) . . ? N1A C3A H3C 109.2 . . ? C2A C3A H3C 109.2 . . ? N1A C3A H3D 109.2 . . ? C2A C3A H3D 109.2 . . ? H3C C3A H3D 107.9 . . ? C2A C6A H6D 109.5 . . ? C2A C6A H6E 109.5 . . ? H6D C6A H6E 109.5 . . ? C2A C6A H6F 109.5 . . ? H6D C6A H6F 109.5 . . ? H6E C6A H6F 109.5 . . ? C2A C5A H5D 109.5 . . ? C2A C5A H5E 109.5 . . ? H5D C5A H5E 109.5 . . ? C2A C5A H5F 109.5 . . ? H5D C5A H5F 109.5 . . ? H5E C5A H5F 109.5 . . ? C41A C4A C43A 111.0(5) . . ? C41A C4A C42A 111.3(4) . . ? C43A C4A C42A 109.6(5) . . ? C41A C4A N1A 109.2(4) . . ? C43A C4A N1A 108.7(4) . . ? C42A C4A N1A 107.0(4) . . ? C4A C41A H41D 109.5 . . ? C4A C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C4A C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C4A C42A H42D 109.5 . . ? C4A C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C4A C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C4A C43A H43D 109.5 . . ? C4A C43A H43E 109.5 . . ? H43D C43A H43E 109.5 . . ? C4A C43A H43F 109.5 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? Al2A C31A H31D 109.5 . . ? Al2A C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? Al2A C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? Al2A C32A H32D 109.5 . . ? Al2A C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? Al2A C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? Al2A C33A H33D 109.5 . . ? Al2A C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? Al2A C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? Al1A C11A H11D 109.5 . . ? Al1A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? Al1A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? Al1A C21A H21D 109.5 . . ? Al1A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? Al1A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Al1 O1 C1 -83.3(4) . . . . ? C21 Al1 O1 C1 141.0(4) . . . . ? N1 Al1 O1 C1 29.0(4) . . . . ? C11 Al1 O1 Al2 65.4(3) . . . . ? C21 Al1 O1 Al2 -70.3(3) . . . . ? N1 Al1 O1 Al2 177.7(3) . . . . ? O1 Al1 N1 C3 37.6(4) . . . . ? C11 Al1 N1 C3 148.4(4) . . . . ? C21 Al1 N1 C3 -76.1(4) . . . . ? O1 Al1 N1 C4 169.5(4) . . . . ? C11 Al1 N1 C4 -79.7(5) . . . . ? C21 Al1 N1 C4 55.8(5) . . . . ? Al1 O1 C1 C2 -74.4(5) . . . . ? Al2 O1 C1 C2 133.4(4) . . . . ? C1 O1 Al2 C31 171.1(4) . . . . ? Al1 O1 Al2 C31 22.2(4) . . . . ? C1 O1 Al2 C33 -67.9(4) . . . . ? Al1 O1 Al2 C33 143.3(3) . . . . ? C1 O1 Al2 C32 51.5(4) . . . . ? Al1 O1 Al2 C32 -97.4(3) . . . . ? O1 C1 C2 C6 164.7(5) . . . . ? O1 C1 C2 C3 41.9(6) . . . . ? O1 C1 C2 C5 -76.0(6) . . . . ? C4 N1 C3 C2 150.7(5) . . . . ? Al1 N1 C3 C2 -73.7(5) . . . . ? C1 C2 C3 N1 36.3(7) . . . . ? C6 C2 C3 N1 -85.0(6) . . . . ? C5 C2 C3 N1 156.0(5) . . . . ? C3 N1 C4 C41 50.7(7) . . . . ? Al1 N1 C4 C41 -77.5(6) . . . . ? C3 N1 C4 C43 172.1(5) . . . . ? Al1 N1 C4 C43 43.9(6) . . . . ? C3 N1 C4 C42 -69.6(7) . . . . ? Al1 N1 C4 C42 162.1(4) . . . . ? C21A Al1A O1A C1A 85.6(4) . . . . ? C11A Al1A O1A C1A -139.2(4) . . . . ? N1A Al1A O1A C1A -26.8(4) . . . . ? C21A Al1A O1A Al2A -62.8(3) . . . . ? C11A Al1A O1A Al2A 72.4(3) . . . . ? N1A Al1A O1A Al2A -175.2(3) . . . . ? C32A Al2A O1A C1A 67.0(4) . . . . ? C31A Al2A O1A C1A -171.8(4) . . . . ? C33A Al2A O1A C1A -51.8(4) . . . . ? C32A Al2A O1A Al1A -143.9(3) . . . . ? C31A Al2A O1A Al1A -22.6(4) . . . . ? C33A Al2A O1A Al1A 97.3(3) . . . . ? O1A Al1A N1A C3A -40.3(3) . . . . ? C21A Al1A N1A C3A -151.2(4) . . . . ? C11A Al1A N1A C3A 74.1(4) . . . . ? O1A Al1A N1A C4A -172.7(4) . . . . ? C21A Al1A N1A C4A 76.4(4) . . . . ? C11A Al1A N1A C4A -58.3(5) . . . . ? Al1A O1A C1A C2A 73.3(5) . . . . ? Al2A O1A C1A C2A -134.9(4) . . . . ? O1A C1A C2A C6A -161.1(4) . . . . ? O1A C1A C2A C5A 78.1(5) . . . . ? O1A C1A C2A C3A -41.0(6) . . . . ? C4A N1A C3A C2A -148.4(4) . . . . ? Al1A N1A C3A C2A 76.2(4) . . . . ? C1A C2A C3A N1A -37.0(6) . . . . ? C6A C2A C3A N1A 82.2(5) . . . . ? C5A C2A C3A N1A -158.5(4) . . . . ? C3A N1A C4A C41A -51.6(6) . . . . ? Al1A N1A C4A C41A 76.2(5) . . . . ? C3A N1A C4A C43A 69.6(6) . . . . ? Al1A N1A C4A C43A -162.5(4) . . . . ? C3A N1A C4A C42A -172.1(4) . . . . ? Al1A N1A C4A C42A -44.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.60 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.306 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.066 #===END