Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email Mitzel@uni-muenster.de _publ_contact_author_name 'ProfD Norbert W. Mitzel' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie Universitat Munster Wilhelm-Klemm-Str. 8 Munster 48329 GERMANY ; _publ_contact_author_phone '++49 251 83 36006' _publ_contact_author_fax '++49 251 83 36007' _publ_requested_coeditor_name ? _publ_section_title ; Different modes of aggregation in organoaluminium and -gallium hydroxylamides ; loop_ _publ_author_name 'Norbert W. Mitzel' 'Christian Lustig' 'Markus Woski' data_woski2_(compound_4) _database_code_depnum_ccdc_archive 'CCDC 204071' _chemical_name_common 'Di(tert-butyl)-N,N-dimethylaminoxygallane - Dimer' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Di(tert-butyl)-N,N-dimethylaminoxygallane - Dimer ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H24 Ga N O' _chemical_formula_weight 244.02 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5724(2) _cell_length_b 11.0474(2) _cell_length_c 14.2735(3) _cell_angle_alpha 74.1676(12) _cell_angle_beta 76.1084(9) _cell_angle_gamma 80.8968(9) _cell_volume 1256.19(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 62090 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 29.13 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 2.160 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Intensity corrections were applied by SCALEPACK: Z. Otwinowski, W. Minor Methods Enzymol 1997, 276, 307. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius DIP 2020' _diffrn_measurement_method 'phi scans 2.0' _diffrn_detector_area_resol_mean '8 - 0.73' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 62090 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 29.13 _reflns_number_total 6173 _reflns_number_gt 5515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius-DIP 2020 Software' _computing_cell_refinement SCALEPACK _computing_data_reduction 'SCALEPACK, DIPSHEL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _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^)+(0.0622P)^2^+1.6245P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6173 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.32047(3) 0.14367(3) 0.222435(19) 0.02136(9) Uani 1 1 d . . . O1 O 0.1989(2) 0.25720(17) 0.30405(13) 0.0253(4) Uani 1 1 d . . . N1 N 0.0946(3) 0.1809(2) 0.38858(17) 0.0304(5) Uani 1 1 d . . . C1 C 0.1365(5) 0.1929(4) 0.4782(2) 0.0492(9) Uani 1 1 d . . . H1A H 0.239(5) 0.166(4) 0.480(3) 0.041(10) Uiso 1 1 d . . . H1B H 0.076(6) 0.150(5) 0.534(4) 0.062(13) Uiso 1 1 d . . . H1C H 0.111(5) 0.289(4) 0.489(3) 0.049(11) Uiso 1 1 d . . . Ga2 Ga 0.21242(3) 0.44416(3) 0.256135(19) 0.02118(9) Uani 1 1 d . . . O2 O 0.3277(2) 0.41548(18) 0.13031(13) 0.0267(4) Uani 1 1 d . . . N2 N 0.4316(2) 0.3022(2) 0.12212(15) 0.0223(4) Uani 1 1 d . . . C2 C -0.0710(4) 0.2333(4) 0.3861(3) 0.0437(8) Uani 1 1 d . . . H2A H -0.095(5) 0.231(4) 0.323(3) 0.040(10) Uiso 1 1 d . . . H2B H -0.090(6) 0.315(6) 0.391(4) 0.080(17) Uiso 1 1 d . . . H2C H -0.136(5) 0.187(4) 0.432(3) 0.056(12) Uiso 1 1 d . . . C3 C 0.5904(3) 0.3214(3) 0.1371(2) 0.0320(6) Uani 1 1 d . . . H3A H 0.630(5) 0.404(4) 0.087(3) 0.050(11) Uiso 1 1 d . . . H3B H 0.664(4) 0.248(4) 0.122(3) 0.039(10) Uiso 1 1 d . . . H3C H 0.582(5) 0.331(4) 0.206(3) 0.042(10) Uiso 1 1 d . . . C4 C 0.4532(4) 0.2980(3) 0.0172(2) 0.0322(6) Uani 1 1 d . . . H4A H 0.508(6) 0.376(4) -0.026(3) 0.061(13) Uiso 1 1 d . . . H4B H 0.345(4) 0.303(3) 0.002(3) 0.032(9) Uiso 1 1 d . . . H4C H 0.529(4) 0.219(4) 0.002(3) 0.038(9) Uiso 1 1 d . . . C11 C 0.4858(3) 0.0201(3) 0.2902(2) 0.0306(6) Uani 1 1 d . . . C12 C 0.6073(5) -0.0411(4) 0.2129(3) 0.0465(8) Uani 1 1 d . . . H12A H 0.674(5) -0.102(4) 0.246(3) 0.057(12) Uiso 1 1 d . . . H12B H 0.670(5) 0.022(4) 0.155(3) 0.054(12) Uiso 1 1 d . . . H12C H 0.540(5) -0.090(4) 0.183(3) 0.055(12) Uiso 1 1 d . . . C13 C 0.5822(4) 0.0774(3) 0.3423(3) 0.0413(7) Uani 1 1 d . . . H13A H 0.646(6) 0.011(5) 0.382(4) 0.080(16) Uiso 1 1 d . . . H13B H 0.508(6) 0.122(5) 0.392(4) 0.070(15) Uiso 1 1 d . . . H13C H 0.649(5) 0.140(4) 0.290(3) 0.057(12) Uiso 1 1 d . . . C14 C 0.3976(5) -0.0842(4) 0.3697(3) 0.0495(9) Uani 1 1 d . . . H14A H 0.484(5) -0.141(4) 0.395(3) 0.050(11) Uiso 1 1 d . . . H14B H 0.343(6) -0.121(5) 0.340(4) 0.067(15) Uiso 1 1 d . . . H14C H 0.323(6) -0.058(4) 0.419(3) 0.058(13) Uiso 1 1 d . . . C15 C 0.1718(3) 0.0783(3) 0.1601(2) 0.0282(5) Uani 1 1 d . . . C16 C 0.0724(4) -0.0186(3) 0.2418(3) 0.0409(7) Uani 1 1 d . . . H16A H 0.001(5) -0.041(4) 0.209(3) 0.045(11) Uiso 1 1 d . . . H16B H 0.012(5) 0.011(4) 0.294(3) 0.055(12) Uiso 1 1 d . . . H16C H 0.168(6) -0.098(5) 0.273(4) 0.080(16) Uiso 1 1 d . . . C17 C 0.0521(4) 0.1827(3) 0.1137(3) 0.0390(7) Uani 1 1 d . . . H17A H -0.019(6) 0.139(5) 0.091(4) 0.075(15) Uiso 1 1 d . . . H17B H 0.107(5) 0.247(4) 0.059(3) 0.049(11) Uiso 1 1 d . . . H17C H -0.017(5) 0.231(4) 0.166(3) 0.055(12) Uiso 1 1 d . . . C18 C 0.2673(4) 0.0096(4) 0.0806(3) 0.0420(7) Uani 1 1 d . . . H18A H 0.192(5) -0.024(4) 0.053(3) 0.042(10) Uiso 1 1 d . . . H18B H 0.335(5) -0.072(5) 0.106(3) 0.058(13) Uiso 1 1 d . . . H18C H 0.333(5) 0.065(4) 0.028(3) 0.056(12) Uiso 1 1 d . . . C21 C 0.0189(3) 0.5571(3) 0.2132(2) 0.0265(5) Uani 1 1 d . . . C22 C -0.1099(4) 0.5988(4) 0.2963(3) 0.0421(7) Uani 1 1 d . . . H22A H -0.192(6) 0.666(4) 0.266(3) 0.060(13) Uiso 1 1 d . . . H22B H -0.059(5) 0.640(4) 0.333(3) 0.051(11) Uiso 1 1 d . . . H22C H -0.165(5) 0.529(4) 0.344(4) 0.059(13) Uiso 1 1 d . . . C23 C 0.0894(4) 0.6763(3) 0.1419(3) 0.0413(7) Uani 1 1 d . . . H23A H 0.003(5) 0.730(4) 0.118(3) 0.043(10) Uiso 1 1 d . . . H23B H 0.171(6) 0.657(5) 0.085(4) 0.065(14) Uiso 1 1 d . . . H23C H 0.147(5) 0.724(4) 0.183(3) 0.060(13) Uiso 1 1 d . . . C24 C -0.0636(4) 0.4990(3) 0.1543(3) 0.0398(7) Uani 1 1 d . . . H24A H -0.144(6) 0.568(5) 0.122(4) 0.067(14) Uiso 1 1 d . . . H24B H -0.123(5) 0.422(4) 0.202(3) 0.040(10) Uiso 1 1 d . . . H24C H 0.021(6) 0.470(5) 0.099(4) 0.068(14) Uiso 1 1 d . . . C25 C 0.3440(3) 0.5059(3) 0.33207(19) 0.0264(5) Uani 1 1 d . . . C26 C 0.4522(4) 0.6021(3) 0.2561(3) 0.0361(6) Uani 1 1 d . . . H26A H 0.503(5) 0.639(4) 0.295(3) 0.040(10) Uiso 1 1 d . . . H26B H 0.385(6) 0.673(5) 0.221(3) 0.064(14) Uiso 1 1 d . . . H26C H 0.543(5) 0.563(4) 0.210(3) 0.041(10) Uiso 1 1 d . . . C27 C 0.4522(5) 0.4056(4) 0.3911(3) 0.0416(7) Uani 1 1 d . . . H27A H 0.508(5) 0.444(4) 0.423(3) 0.053(12) Uiso 1 1 d . . . H27B H 0.529(5) 0.361(4) 0.347(3) 0.048(11) Uiso 1 1 d . . . H27C H 0.391(5) 0.345(4) 0.442(3) 0.057(12) Uiso 1 1 d . . . C28 C 0.2294(4) 0.5764(3) 0.4046(2) 0.0364(6) Uani 1 1 d . . . H28A H 0.289(5) 0.608(4) 0.438(3) 0.048(11) Uiso 1 1 d . . . H28B H 0.152(5) 0.523(4) 0.452(3) 0.046(11) Uiso 1 1 d . . . H28C H 0.165(5) 0.648(4) 0.371(3) 0.044(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 Ga1 0.02169(14) 0.02178(15) 0.01891(14) -0.00452(11) -0.00175(10) -0.00185(10) O1 0.0297(9) 0.0228(9) 0.0183(8) -0.0041(7) 0.0052(7) -0.0049(7) N1 0.0336(12) 0.0270(11) 0.0222(10) -0.0006(9) 0.0060(9) -0.0061(9) C1 0.057(2) 0.060(2) 0.0228(14) -0.0040(15) -0.0015(14) -0.0036(18) Ga2 0.01943(14) 0.02322(15) 0.02040(14) -0.00598(11) -0.00258(10) -0.00194(10) O2 0.0291(9) 0.0230(9) 0.0219(8) -0.0034(7) 0.0005(7) 0.0029(7) N2 0.0200(9) 0.0222(10) 0.0210(9) -0.0042(8) 0.0009(7) -0.0007(7) C2 0.0310(15) 0.050(2) 0.0406(18) -0.0069(16) 0.0101(13) -0.0116(14) C3 0.0231(12) 0.0311(14) 0.0393(15) -0.0069(13) -0.0042(11) -0.0026(10) C4 0.0398(15) 0.0333(15) 0.0210(12) -0.0078(11) 0.0026(10) -0.0080(12) C11 0.0318(13) 0.0271(13) 0.0303(13) -0.0019(11) -0.0107(10) 0.0022(10) C12 0.0433(18) 0.0409(18) 0.052(2) -0.0155(17) -0.0099(15) 0.0147(15) C13 0.0438(17) 0.0380(17) 0.0444(18) -0.0055(15) -0.0234(15) 0.0029(14) C14 0.057(2) 0.0341(17) 0.047(2) 0.0078(16) -0.0117(18) -0.0067(16) C15 0.0261(12) 0.0319(13) 0.0287(12) -0.0101(11) -0.0043(10) -0.0061(10) C16 0.0406(17) 0.0373(17) 0.0429(17) -0.0080(15) 0.0012(14) -0.0170(13) C17 0.0385(16) 0.0397(17) 0.0426(17) -0.0088(15) -0.0171(13) -0.0041(13) C18 0.0437(17) 0.0460(19) 0.0434(17) -0.0263(16) -0.0011(14) -0.0102(15) C21 0.0222(11) 0.0274(12) 0.0299(12) -0.0076(11) -0.0080(9) 0.0023(9) C22 0.0304(15) 0.0474(19) 0.0468(18) -0.0186(16) -0.0055(13) 0.0100(13) C23 0.0403(17) 0.0277(14) 0.0489(19) 0.0030(14) -0.0128(14) 0.0003(12) C24 0.0351(15) 0.0424(18) 0.0480(18) -0.0131(15) -0.0222(14) 0.0027(13) C25 0.0258(12) 0.0317(13) 0.0258(12) -0.0118(11) -0.0069(9) -0.0038(10) C26 0.0319(14) 0.0390(16) 0.0408(16) -0.0135(14) -0.0046(12) -0.0107(12) C27 0.0450(18) 0.0459(19) 0.0410(17) -0.0134(16) -0.0241(15) 0.0024(15) C28 0.0379(16) 0.0419(17) 0.0350(15) -0.0213(14) -0.0041(12) -0.0042(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 Ga1 O1 1.9537(19) . ? Ga1 C15 2.031(3) . ? Ga1 C11 2.032(3) . ? Ga1 N2 2.128(2) . ? O1 N1 1.460(3) . ? O1 Ga2 2.0036(18) . ? N1 C2 1.451(4) . ? N1 C1 1.453(4) . ? C1 H1A 0.88(4) . ? C1 H1B 0.89(5) . ? C1 H1C 1.10(4) . ? Ga2 O2 1.9135(18) . ? Ga2 C21 2.025(2) . ? Ga2 C25 2.036(3) . ? O2 N2 1.432(3) . ? N2 C4 1.477(3) . ? N2 C3 1.483(3) . ? C2 H2A 0.98(4) . ? C2 H2B 0.91(6) . ? C2 H2C 0.86(5) . ? C3 H3A 1.05(4) . ? C3 H3B 0.98(4) . ? C3 H3C 1.00(4) . ? C4 H4A 1.03(5) . ? C4 H4B 0.99(4) . ? C4 H4C 1.04(4) . ? C11 C14 1.529(4) . ? C11 C13 1.535(5) . ? C11 C12 1.547(4) . ? C12 H12A 0.91(5) . ? C12 H12B 1.02(5) . ? C12 H12C 1.08(5) . ? C13 H13A 0.97(6) . ? C13 H13B 1.01(5) . ? C13 H13C 1.00(5) . ? C14 H14A 0.97(4) . ? C14 H14B 0.90(5) . ? C14 H14C 0.90(5) . ? C15 C17 1.535(4) . ? C15 C18 1.536(4) . ? C15 C16 1.537(4) . ? C16 H16A 0.95(4) . ? C16 H16B 0.91(5) . ? C16 H16C 1.17(5) . ? C17 H17A 0.99(5) . ? C17 H17B 0.98(4) . ? C17 H17C 1.05(5) . ? C18 H18A 1.00(4) . ? C18 H18B 1.02(5) . ? C18 H18C 0.95(5) . ? C21 C24 1.531(4) . ? C21 C22 1.532(4) . ? C21 C23 1.536(4) . ? C22 H22A 1.02(5) . ? C22 H22B 0.99(4) . ? C22 H22C 0.98(5) . ? C23 H23A 0.94(4) . ? C23 H23B 0.98(5) . ? C23 H23C 1.12(5) . ? C24 H24A 1.03(5) . ? C24 H24B 1.05(4) . ? C24 H24C 1.02(5) . ? C25 C27 1.530(4) . ? C25 C28 1.534(4) . ? C25 C26 1.538(4) . ? C26 H26A 0.98(4) . ? C26 H26B 0.98(5) . ? C26 H26C 1.01(4) . ? C27 H27A 0.95(4) . ? C27 H27B 0.98(4) . ? C27 H27C 0.95(5) . ? C28 H28A 0.93(4) . ? C28 H28B 0.97(4) . ? C28 H28C 0.97(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga1 C15 110.90(10) . . ? O1 Ga1 C11 112.27(10) . . ? C15 Ga1 C11 119.38(12) . . ? O1 Ga1 N2 88.25(8) . . ? C15 Ga1 N2 111.37(10) . . ? C11 Ga1 N2 110.41(10) . . ? N1 O1 Ga1 107.03(14) . . ? N1 O1 Ga2 132.07(15) . . ? Ga1 O1 Ga2 120.40(8) . . ? C2 N1 C1 109.8(3) . . ? C2 N1 O1 107.6(2) . . ? C1 N1 O1 107.1(2) . . ? N1 C1 H1A 112(3) . . ? N1 C1 H1B 113(3) . . ? H1A C1 H1B 108(4) . . ? N1 C1 H1C 114(2) . . ? H1A C1 H1C 109(3) . . ? H1B C1 H1C 101(4) . . ? O2 Ga2 O1 87.61(7) . . ? O2 Ga2 C21 99.56(10) . . ? O1 Ga2 C21 118.90(10) . . ? O2 Ga2 C25 115.15(10) . . ? O1 Ga2 C25 111.71(10) . . ? C21 Ga2 C25 118.75(11) . . ? N2 O2 Ga2 122.14(14) . . ? O2 N2 C4 104.84(19) . . ? O2 N2 C3 106.7(2) . . ? C4 N2 C3 107.3(2) . . ? O2 N2 Ga1 109.50(13) . . ? C4 N2 Ga1 112.07(17) . . ? C3 N2 Ga1 115.74(16) . . ? N1 C2 H2A 109(2) . . ? N1 C2 H2B 113(3) . . ? H2A C2 H2B 108(4) . . ? N1 C2 H2C 110(3) . . ? H2A C2 H2C 106(4) . . ? H2B C2 H2C 111(4) . . ? N2 C3 H3A 109(2) . . ? N2 C3 H3B 106(2) . . ? H3A C3 H3B 109(3) . . ? N2 C3 H3C 111(2) . . ? H3A C3 H3C 108(3) . . ? H3B C3 H3C 114(3) . . ? N2 C4 H4A 108(3) . . ? N2 C4 H4B 108(2) . . ? H4A C4 H4B 109(3) . . ? N2 C4 H4C 112(2) . . ? H4A C4 H4C 107(3) . . ? H4B C4 H4C 113(3) . . ? C14 C11 C13 106.9(3) . . ? C14 C11 C12 108.4(3) . . ? C13 C11 C12 108.0(3) . . ? C14 C11 Ga1 108.5(2) . . ? C13 C11 Ga1 115.2(2) . . ? C12 C11 Ga1 109.6(2) . . ? C11 C12 H12A 108(3) . . ? C11 C12 H12B 114(3) . . ? H12A C12 H12B 112(4) . . ? C11 C12 H12C 107(2) . . ? H12A C12 H12C 106(4) . . ? H12B C12 H12C 108(3) . . ? C11 C13 H13A 110(3) . . ? C11 C13 H13B 111(3) . . ? H13A C13 H13B 105(4) . . ? C11 C13 H13C 108(3) . . ? H13A C13 H13C 114(4) . . ? H13B C13 H13C 109(4) . . ? C11 C14 H14A 103(3) . . ? C11 C14 H14B 108(3) . . ? H14A C14 H14B 112(4) . . ? C11 C14 H14C 116(3) . . ? H14A C14 H14C 112(4) . . ? H14B C14 H14C 106(4) . . ? C17 C15 C18 108.9(3) . . ? C17 C15 C16 107.4(3) . . ? C18 C15 C16 107.1(3) . . ? C17 C15 Ga1 113.0(2) . . ? C18 C15 Ga1 111.7(2) . . ? C16 C15 Ga1 108.5(2) . . ? C15 C16 H16A 104(2) . . ? C15 C16 H16B 115(3) . . ? H16A C16 H16B 108(4) . . ? C15 C16 H16C 105(3) . . ? H16A C16 H16C 118(4) . . ? H16B C16 H16C 107(4) . . ? C15 C17 H17A 106(3) . . ? C15 C17 H17B 112(2) . . ? H17A C17 H17B 112(4) . . ? C15 C17 H17C 111(2) . . ? H17A C17 H17C 110(4) . . ? H17B C17 H17C 106(3) . . ? C15 C18 H18A 110(2) . . ? C15 C18 H18B 116(3) . . ? H18A C18 H18B 100(3) . . ? C15 C18 H18C 111(3) . . ? H18A C18 H18C 110(3) . . ? H18B C18 H18C 110(4) . . ? C24 C21 C22 108.4(3) . . ? C24 C21 C23 107.3(3) . . ? C22 C21 C23 107.6(3) . . ? C24 C21 Ga2 112.34(19) . . ? C22 C21 Ga2 116.0(2) . . ? C23 C21 Ga2 104.67(19) . . ? C21 C22 H22A 110(3) . . ? C21 C22 H22B 109(2) . . ? H22A C22 H22B 106(3) . . ? C21 C22 H22C 114(3) . . ? H22A C22 H22C 110(4) . . ? H22B C22 H22C 108(4) . . ? C21 C23 H23A 107(2) . . ? C21 C23 H23B 112(3) . . ? H23A C23 H23B 109(4) . . ? C21 C23 H23C 109(2) . . ? H23A C23 H23C 111(3) . . ? H23B C23 H23C 109(4) . . ? C21 C24 H24A 108(3) . . ? C21 C24 H24B 110(2) . . ? H24A C24 H24B 111(3) . . ? C21 C24 H24C 109(3) . . ? H24A C24 H24C 109(4) . . ? H24B C24 H24C 110(4) . . ? C27 C25 C28 107.8(3) . . ? C27 C25 C26 107.8(3) . . ? C28 C25 C26 107.3(3) . . ? C27 C25 Ga2 116.8(2) . . ? C28 C25 Ga2 109.19(18) . . ? C26 C25 Ga2 107.57(18) . . ? C25 C26 H26A 106(2) . . ? C25 C26 H26B 110(3) . . ? H26A C26 H26B 106(3) . . ? C25 C26 H26C 114(2) . . ? H26A C26 H26C 106(3) . . ? H26B C26 H26C 114(3) . . ? C25 C27 H27A 110(3) . . ? C25 C27 H27B 110(2) . . ? H27A C27 H27B 110(4) . . ? C25 C27 H27C 112(3) . . ? H27A C27 H27C 106(4) . . ? H27B C27 H27C 108(4) . . ? C25 C28 H28A 110(3) . . ? C25 C28 H28B 112(2) . . ? H28A C28 H28B 111(3) . . ? C25 C28 H28C 113(2) . . ? H28A C28 H28C 107(3) . . ? H28B C28 H28C 105(3) . . ? 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 C15 Ga1 O1 N1 66.76(17) . . . . ? C11 Ga1 O1 N1 -69.61(18) . . . . ? N2 Ga1 O1 N1 179.01(16) . . . . ? C15 Ga1 O1 Ga2 -106.09(13) . . . . ? C11 Ga1 O1 Ga2 117.53(13) . . . . ? N2 Ga1 O1 Ga2 6.15(11) . . . . ? Ga1 O1 N1 C2 -120.7(2) . . . . ? Ga2 O1 N1 C2 51.0(3) . . . . ? Ga1 O1 N1 C1 121.3(2) . . . . ? Ga2 O1 N1 C1 -67.1(3) . . . . ? N1 O1 Ga2 O2 -161.8(2) . . . . ? Ga1 O1 Ga2 O2 9.01(11) . . . . ? N1 O1 Ga2 C21 -62.2(2) . . . . ? Ga1 O1 Ga2 C21 108.61(13) . . . . ? N1 O1 Ga2 C25 82.0(2) . . . . ? Ga1 O1 Ga2 C25 -107.17(13) . . . . ? O1 Ga2 O2 N2 -32.30(17) . . . . ? C21 Ga2 O2 N2 -151.22(18) . . . . ? C25 Ga2 O2 N2 80.62(19) . . . . ? Ga2 O2 N2 C4 162.23(17) . . . . ? Ga2 O2 N2 C3 -84.1(2) . . . . ? Ga2 O2 N2 Ga1 41.8(2) . . . . ? O1 Ga1 N2 O2 -25.35(15) . . . . ? C15 Ga1 N2 O2 86.45(17) . . . . ? C11 Ga1 N2 O2 -138.51(16) . . . . ? O1 Ga1 N2 C4 -141.25(18) . . . . ? C15 Ga1 N2 C4 -29.5(2) . . . . ? C11 Ga1 N2 C4 105.59(19) . . . . ? O1 Ga1 N2 C3 95.3(2) . . . . ? C15 Ga1 N2 C3 -152.95(19) . . . . ? C11 Ga1 N2 C3 -17.9(2) . . . . ? O1 Ga1 C11 C14 76.9(3) . . . . ? C15 Ga1 C11 C14 -55.4(3) . . . . ? N2 Ga1 C11 C14 173.7(2) . . . . ? O1 Ga1 C11 C13 -42.8(3) . . . . ? C15 Ga1 C11 C13 -175.1(2) . . . . ? N2 Ga1 C11 C13 53.9(3) . . . . ? O1 Ga1 C11 C12 -164.8(2) . . . . ? C15 Ga1 C11 C12 62.9(3) . . . . ? N2 Ga1 C11 C12 -68.1(2) . . . . ? O1 Ga1 C15 C17 46.1(2) . . . . ? C11 Ga1 C15 C17 179.0(2) . . . . ? N2 Ga1 C15 C17 -50.5(2) . . . . ? O1 Ga1 C15 C18 169.3(2) . . . . ? C11 Ga1 C15 C18 -57.9(3) . . . . ? N2 Ga1 C15 C18 72.7(2) . . . . ? O1 Ga1 C15 C16 -73.0(2) . . . . ? C11 Ga1 C15 C16 59.9(2) . . . . ? N2 Ga1 C15 C16 -169.53(19) . . . . ? O2 Ga2 C21 C24 52.5(2) . . . . ? O1 Ga2 C21 C24 -40.1(2) . . . . ? C25 Ga2 C21 C24 178.2(2) . . . . ? O2 Ga2 C21 C22 178.0(2) . . . . ? O1 Ga2 C21 C22 85.4(2) . . . . ? C25 Ga2 C21 C22 -56.3(3) . . . . ? O2 Ga2 C21 C23 -63.6(2) . . . . ? O1 Ga2 C21 C23 -156.16(19) . . . . ? C25 Ga2 C21 C23 62.1(2) . . . . ? O2 Ga2 C25 C27 -81.1(2) . . . . ? O1 Ga2 C25 C27 16.8(3) . . . . ? C21 Ga2 C25 C27 161.1(2) . . . . ? O2 Ga2 C25 C28 156.32(19) . . . . ? O1 Ga2 C25 C28 -105.8(2) . . . . ? C21 Ga2 C25 C28 38.5(2) . . . . ? O2 Ga2 C25 C26 40.2(2) . . . . ? O1 Ga2 C25 C26 138.06(19) . . . . ? C21 Ga2 C25 C26 -77.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 2.525 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.091 data_woski8_(compound_3) _database_code_depnum_ccdc_archive 'CCDC 204072' _chemical_name_common 'N,N-Dimethylaminoxy-di-tert-butyl-aluminium - Dimer' _audit_creation_method SHELXL-97 _chemical_name_systematic ; N,N-Dimethylaminoxy-di-tert-butyl-aluminium - Dimer ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H24 Al N O' _chemical_formula_weight 201.28 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5972(3) _cell_length_b 8.9228(3) _cell_length_c 9.9334(4) _cell_angle_alpha 71.997(2) _cell_angle_beta 78.505(3) _cell_angle_gamma 63.939(3) _cell_volume 649.21(4) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 30908 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 30.68 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.030 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 224 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Intensity corrections were applied by SCALEPACK: Z. Otwinowski, W. Minor Methods Enzymol 1997, 276, 307. ; _diffrn_ambient_temperature 243(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 'Nonius DIP 2020' _diffrn_measurement_method 'Phi scans 2.0 deg' _diffrn_detector_area_resol_mean '8 - 0.68' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 30908 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 30.68 _reflns_number_total 3577 _reflns_number_gt 3092 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius-DIP 2020 Software' _computing_cell_refinement SCALEPACK _computing_data_reduction 'SCALEPACK, DIPSHEL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _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^)+(0.2000P)^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 ride _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 4.4(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3577 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1533 _refine_ls_R_factor_gt 0.1452 _refine_ls_wR_factor_ref 0.4038 _refine_ls_wR_factor_gt 0.3858 _refine_ls_goodness_of_fit_ref 1.743 _refine_ls_restrained_S_all 1.743 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al Al 0.02706(7) -0.12724(9) 0.16365(6) 0.0519(5) Uani 1 1 d . . . C11 C 0.2659(8) -0.3001(8) 0.2224(9) 0.125(2) Uani 1 1 d . . . C12 C 0.2669(18) -0.4826(13) 0.2382(19) 0.203(6) Uani 1 1 d . . . H12A H 0.3795 -0.5722 0.2658 0.305 Uiso 1 1 calc R . . H12B H 0.2443 -0.4878 0.1483 0.305 Uiso 1 1 calc R . . H12C H 0.1777 -0.4997 0.3103 0.305 Uiso 1 1 calc R . . C13 C 0.4099(13) -0.2810(16) 0.1169(16) 0.164(4) Uani 1 1 d . . . H13A H 0.5201 -0.3681 0.1520 0.246 Uiso 1 1 calc R . . H13B H 0.4075 -0.1674 0.1023 0.246 Uiso 1 1 calc R . . H13C H 0.3959 -0.2950 0.0276 0.246 Uiso 1 1 calc R . . C14 C 0.3105(16) -0.3020(15) 0.3558(14) 0.190(5) Uani 1 1 d . . . H14A H 0.4271 -0.3887 0.3745 0.285 Uiso 1 1 calc R . . H14B H 0.2290 -0.3290 0.4316 0.285 Uiso 1 1 calc R . . H14C H 0.3054 -0.1897 0.3510 0.285 Uiso 1 1 calc R . . C15 C -0.1793(9) -0.1318(11) 0.3029(9) 0.125(2) Uani 1 1 d . . . C16 C -0.1925(16) -0.2950(19) 0.328(2) 0.225(8) Uani 1 1 d . . . H16A H -0.2921 -0.2962 0.3936 0.337 Uiso 1 1 calc R . . H16B H -0.0878 -0.3885 0.3676 0.337 Uiso 1 1 calc R . . H16C H -0.2065 -0.3095 0.2386 0.337 Uiso 1 1 calc R . . C17 C -0.163(2) -0.1208(19) 0.4390(16) 0.195(5) Uani 1 1 d . . . H17A H -0.2650 -0.1229 0.5010 0.293 Uiso 1 1 calc R . . H17B H -0.1524 -0.0142 0.4297 0.293 Uiso 1 1 calc R . . H17C H -0.0605 -0.2178 0.4791 0.293 Uiso 1 1 calc R . . C18 C -0.3536(15) 0.010(2) 0.245(2) 0.185(5) Uani 1 1 d . . . H18A H -0.4486 0.0024 0.3141 0.277 Uiso 1 1 calc R . . H18B H -0.3693 -0.0075 0.1573 0.277 Uiso 1 1 calc R . . H18C H -0.3520 0.1222 0.2261 0.277 Uiso 1 1 calc R . . O O 0.0163(8) 0.0881(10) 0.0413(9) 0.195(3) Uani 1 1 d . . . N N 0.0294(13) 0.2397(13) 0.0448(14) 0.197(4) Uani 1 1 d . . . C1 C -0.115(3) 0.287(3) 0.167(2) 0.331(15) Uani 1 1 d . . . H1A H -0.1222 0.3902 0.1868 0.497 Uiso 1 1 calc R . . H1B H -0.0856 0.1928 0.2515 0.497 Uiso 1 1 calc R . . H1C H -0.2253 0.3086 0.1381 0.497 Uiso 1 1 calc R . . C2 C 0.204(2) 0.184(2) 0.0929(18) 0.218(6) Uani 1 1 d . . . H2A H 0.2922 0.1469 0.0184 0.327 Uiso 1 1 calc R . . H2B H 0.2224 0.0898 0.1775 0.327 Uiso 1 1 calc R . . H2C H 0.2108 0.2803 0.1140 0.327 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al 0.0371(6) 0.0692(7) 0.0507(7) -0.0229(4) -0.0036(4) -0.0173(4) C11 0.096(4) 0.112(4) 0.158(6) -0.040(4) -0.019(4) -0.027(3) C12 0.187(11) 0.121(6) 0.265(17) -0.060(8) -0.038(10) -0.014(6) C13 0.090(5) 0.154(7) 0.214(12) -0.038(7) -0.026(6) -0.020(5) C14 0.176(10) 0.175(8) 0.193(11) 0.012(7) -0.083(9) -0.058(7) C15 0.100(4) 0.164(6) 0.125(5) -0.051(4) 0.012(3) -0.065(4) C16 0.133(8) 0.195(10) 0.284(18) 0.055(11) -0.041(10) -0.078(8) C17 0.227(13) 0.201(11) 0.176(11) -0.064(9) 0.012(9) -0.103(10) C18 0.102(6) 0.207(11) 0.222(14) -0.046(9) 0.004(7) -0.055(7) O 0.122(4) 0.172(5) 0.227(8) 0.023(5) -0.008(5) -0.052(4) N 0.156(7) 0.155(6) 0.271(13) -0.024(7) -0.049(7) -0.061(5) C1 0.28(2) 0.258(19) 0.28(2) -0.133(17) 0.028(17) 0.077(17) C2 0.195(12) 0.214(12) 0.251(17) -0.020(11) -0.050(11) -0.100(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 Al O 1.903(7) . ? Al C11 2.018(6) . ? Al C15 2.028(7) . ? Al O 2.038(9) 2 ? C11 C14 1.444(14) . ? C11 C13 1.490(15) . ? C11 C12 1.583(14) . ? C15 C17 1.423(15) . ? C15 C16 1.451(17) . ? C15 C18 1.551(15) . ? O N 1.418(11) . ? O Al 2.038(9) 2 ? N C2 1.487(16) . ? N C1 1.56(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Al C11 115.4(3) . . ? O Al C15 118.7(3) . . ? C11 Al C15 117.9(4) . . ? O Al O 65.0(5) . 2 ? C11 Al O 115.5(3) . 2 ? C15 Al O 113.4(3) . 2 ? C14 C11 C13 105.5(9) . . ? C14 C11 C12 107.5(9) . . ? C13 C11 C12 108.4(9) . . ? C14 C11 Al 115.7(7) . . ? C13 C11 Al 114.1(6) . . ? C12 C11 Al 105.3(6) . . ? C17 C15 C16 105.3(11) . . ? C17 C15 C18 110.3(11) . . ? C16 C15 C18 105.9(9) . . ? C17 C15 Al 112.9(7) . . ? C16 C15 Al 109.8(8) . . ? C18 C15 Al 112.2(8) . . ? N O Al 140.2(8) . . ? N O Al 104.8(6) . 2 ? Al O Al 115.0(5) . 2 ? O N C2 106.5(10) . . ? O N C1 97.6(13) . . ? C2 N C1 110.6(16) . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 30.68 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 1.508 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.138 data_lus50_(compound_5) _database_code_depnum_ccdc_archive 'CCDC 204073' _chemical_name_common 'N,N-Diisopropylaminoxy-dimethylaluminium - Dimer' _audit_creation_method SHELXL-97 _chemical_name_systematic ; N,N-Diisopropylaminoxy-dimethylaluminium - Dimer ; _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 0.0033 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9665(4) _cell_length_b 8.2123(4) _cell_length_c 9.4581(4) _cell_angle_alpha 67.0510(10) _cell_angle_beta 85.6550(10) _cell_angle_gamma 69.2640(10) _cell_volume 531.50(4) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4755 _cell_measurement_theta_min 5.482 _cell_measurement_theta_max 59.956 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 192 _exptl_absorpt_coefficient_mu 0.145 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.623724 _exptl_absorpt_correction_T_max 1.000000 _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 'CCD (Bruker AXS)' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 6148 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 29.99 _reflns_number_total 3051 _reflns_number_gt 2693 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS' _computing_cell_refinement SAINT32 _computing_data_reduction SAINT32 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1' _computing_publication_material 'SHELXTL 5.1' _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^)+(0.0683P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3051 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.34678(3) 0.01572(3) 0.59362(3) 0.01858(10) Uani 1 1 d . . . O1 O 0.40254(8) 0.05163(8) 0.39266(6) 0.01758(14) Uani 1 1 d . . . N1 N 0.25921(9) 0.07394(10) 0.29000(8) 0.01960(16) Uani 1 1 d . . . C1 C 0.25949(15) -0.19292(16) 0.69864(12) 0.0311(2) Uani 1 1 d . . . H13 H 0.339(2) -0.315(2) 0.7087(16) 0.043(4) Uiso 1 1 d . . . H12 H 0.151(2) -0.164(2) 0.6425(18) 0.052(4) Uiso 1 1 d . . . H11 H 0.237(2) -0.208(2) 0.8055(19) 0.054(4) Uiso 1 1 d . . . C2 C 0.21054(14) 0.24382(15) 0.63013(13) 0.0299(2) Uani 1 1 d . . . H23 H 0.0809(19) 0.288(2) 0.5968(17) 0.042(4) Uiso 1 1 d . . . H22 H 0.242(2) 0.347(2) 0.5781(19) 0.052(4) Uiso 1 1 d . . . H21 H 0.219(2) 0.221(2) 0.7340(19) 0.054(4) Uiso 1 1 d . . . C3 C 0.20958(13) 0.26530(13) 0.16554(10) 0.02542(19) Uani 1 1 d . . . H3 H 0.1187(18) 0.2640(19) 0.1137(15) 0.035(3) Uiso 1 1 d . . . C4 C 0.32870(13) -0.08137(13) 0.23459(11) 0.02421(19) Uani 1 1 d . . . H4 H 0.4435(17) -0.0850(17) 0.1874(14) 0.027(3) Uiso 1 1 d . . . C5 C 0.35323(17) 0.30103(18) 0.05436(13) 0.0376(3) Uani 1 1 d . . . H53 H 0.304(2) 0.423(2) -0.0282(19) 0.051(4) Uiso 1 1 d . . . H52 H 0.443(2) 0.319(2) 0.1024(17) 0.044(4) Uiso 1 1 d . . . H51 H 0.407(2) 0.212(2) 0.0122(18) 0.053(4) Uiso 1 1 d . . . C6 C 0.13830(17) 0.41461(15) 0.23291(14) 0.0361(2) Uani 1 1 d . . . H63 H 0.230(2) 0.422(2) 0.2870(18) 0.047(4) Uiso 1 1 d . . . H62 H 0.041(2) 0.395(2) 0.3041(18) 0.052(4) Uiso 1 1 d . . . H61 H 0.080(2) 0.534(2) 0.1547(19) 0.055(4) Uiso 1 1 d . . . C7 C 0.19338(16) -0.05372(17) 0.11354(13) 0.0345(2) Uani 1 1 d . . . H73 H 0.070(2) -0.034(2) 0.1516(18) 0.051(4) Uiso 1 1 d . . . H72 H 0.1831(19) 0.050(2) 0.0162(17) 0.040(4) Uiso 1 1 d . . . H71 H 0.233(2) -0.165(2) 0.0895(19) 0.061(5) Uiso 1 1 d . . . C8 C 0.35849(16) -0.27017(14) 0.36686(13) 0.0326(2) Uani 1 1 d . . . H83 H 0.4372(18) -0.2940(18) 0.4488(15) 0.032(3) Uiso 1 1 d . . . H82 H 0.404(2) -0.367(2) 0.3255(19) 0.059(4) Uiso 1 1 d . . . H81 H 0.242(2) -0.277(2) 0.4115(16) 0.041(4) 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 0.01755(14) 0.02012(15) 0.01688(15) -0.00674(10) 0.00064(9) -0.00570(10) O1 0.0173(3) 0.0195(3) 0.0153(3) -0.0064(2) -0.0035(2) -0.0053(2) N1 0.0190(3) 0.0205(3) 0.0183(3) -0.0068(3) -0.0060(3) -0.0051(3) C1 0.0314(5) 0.0339(5) 0.0284(5) -0.0073(4) 0.0049(4) -0.0178(4) C2 0.0258(5) 0.0319(5) 0.0303(5) -0.0167(4) 0.0034(4) -0.0035(4) C3 0.0275(4) 0.0221(4) 0.0201(4) -0.0035(3) -0.0086(3) -0.0046(3) C4 0.0263(4) 0.0256(4) 0.0239(4) -0.0131(4) -0.0025(3) -0.0081(3) C5 0.0443(6) 0.0377(6) 0.0227(5) -0.0005(4) -0.0007(4) -0.0173(5) C6 0.0433(6) 0.0199(4) 0.0351(6) -0.0072(4) -0.0105(5) -0.0010(4) C7 0.0400(6) 0.0404(6) 0.0304(5) -0.0187(5) -0.0072(4) -0.0150(5) C8 0.0413(6) 0.0220(4) 0.0352(5) -0.0112(4) -0.0069(4) -0.0101(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.8505(6) . ? Al1 O1 1.8741(6) 2_656 ? Al1 C2 1.9530(10) . ? Al1 C1 1.9539(10) . ? Al1 Al1 2.9013(5) 2_656 ? O1 N1 1.4701(8) . ? O1 Al1 1.8741(6) 2_656 ? N1 C4 1.4783(11) . ? N1 C3 1.4831(11) . ? C1 H13 0.948(16) . ? C1 H12 0.955(16) . ? C1 H11 0.980(17) . ? C2 H23 0.996(14) . ? C2 H22 0.909(17) . ? C2 H21 0.929(17) . ? C3 C6 1.5143(15) . ? C3 C5 1.5220(15) . ? C3 H3 0.910(13) . ? C4 C8 1.5157(14) . ? C4 C7 1.5282(13) . ? C4 H4 0.983(13) . ? C5 H53 0.962(17) . ? C5 H52 0.955(15) . ? C5 H51 0.928(17) . ? C6 H63 0.954(16) . ? C6 H62 1.005(16) . ? C6 H61 0.942(17) . ? C7 H73 0.999(16) . ? C7 H72 0.964(15) . ? C7 H71 0.969(17) . ? C8 H83 0.949(13) . ? C8 H82 0.965(18) . ? C8 H81 1.000(15) . ? 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 77.67(3) . 2_656 ? O1 Al1 C2 116.02(4) . . ? O1 Al1 C2 115.22(4) 2_656 . ? O1 Al1 C1 114.97(4) . . ? O1 Al1 C1 114.96(4) 2_656 . ? C2 Al1 C1 113.47(5) . . ? O1 Al1 Al1 39.128(18) . 2_656 ? O1 Al1 Al1 38.544(18) 2_656 2_656 ? C2 Al1 Al1 123.72(4) . 2_656 ? C1 Al1 Al1 122.81(4) . 2_656 ? N1 O1 Al1 115.85(4) . . ? N1 O1 Al1 139.47(5) . 2_656 ? Al1 O1 Al1 102.33(3) . 2_656 ? O1 N1 C4 107.26(6) . . ? O1 N1 C3 107.99(6) . . ? C4 N1 C3 113.93(7) . . ? Al1 C1 H13 116.3(9) . . ? Al1 C1 H12 106.9(9) . . ? H13 C1 H12 108.9(12) . . ? Al1 C1 H11 111.3(9) . . ? H13 C1 H11 103.1(12) . . ? H12 C1 H11 110.3(12) . . ? Al1 C2 H23 110.5(8) . . ? Al1 C2 H22 116.1(10) . . ? H23 C2 H22 103.9(12) . . ? Al1 C2 H21 111.0(10) . . ? H23 C2 H21 107.9(12) . . ? H22 C2 H21 106.9(13) . . ? N1 C3 C6 110.13(8) . . ? N1 C3 C5 116.09(8) . . ? C6 C3 C5 111.69(9) . . ? N1 C3 H3 99.8(8) . . ? C6 C3 H3 110.3(8) . . ? C5 C3 H3 108.2(8) . . ? N1 C4 C8 110.37(8) . . ? N1 C4 C7 109.73(8) . . ? C8 C4 C7 108.87(8) . . ? N1 C4 H4 111.5(7) . . ? C8 C4 H4 108.2(7) . . ? C7 C4 H4 108.1(7) . . ? C3 C5 H53 110.0(9) . . ? C3 C5 H52 109.7(9) . . ? H53 C5 H52 100.9(12) . . ? C3 C5 H51 116.3(10) . . ? H53 C5 H51 108.5(13) . . ? H52 C5 H51 110.4(13) . . ? C3 C6 H63 112.7(9) . . ? C3 C6 H62 112.5(9) . . ? H63 C6 H62 108.4(13) . . ? C3 C6 H61 110.2(10) . . ? H63 C6 H61 109.6(13) . . ? H62 C6 H61 102.9(14) . . ? C4 C7 H73 111.3(8) . . ? C4 C7 H72 115.1(8) . . ? H73 C7 H72 107.2(13) . . ? C4 C7 H71 108.5(10) . . ? H73 C7 H71 109.4(13) . . ? H72 C7 H71 105.0(13) . . ? C4 C8 H83 113.4(8) . . ? C4 C8 H82 107.4(10) . . ? H83 C8 H82 111.0(12) . . ? C4 C8 H81 110.8(8) . . ? H83 C8 H81 106.9(11) . . ? H82 C8 H81 107.4(12) . . ? 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 N1 166.02(6) 2_656 . . . ? C2 Al1 O1 N1 -81.73(6) . . . . ? C1 Al1 O1 N1 54.02(6) . . . . ? Al1 Al1 O1 N1 166.02(6) 2_656 . . . ? O1 Al1 O1 Al1 0.0 2_656 . . 2_656 ? C2 Al1 O1 Al1 112.25(4) . . . 2_656 ? C1 Al1 O1 Al1 -112.00(4) . . . 2_656 ? Al1 O1 N1 C4 -119.48(6) . . . . ? Al1 O1 N1 C4 39.23(10) 2_656 . . . ? Al1 O1 N1 C3 117.34(6) . . . . ? Al1 O1 N1 C3 -83.96(9) 2_656 . . . ? O1 N1 C3 C6 -61.56(10) . . . . ? C4 N1 C3 C6 179.41(8) . . . . ? O1 N1 C3 C5 66.59(10) . . . . ? C4 N1 C3 C5 -52.44(11) . . . . ? O1 N1 C4 C8 66.14(9) . . . . ? C3 N1 C4 C8 -174.42(7) . . . . ? O1 N1 C4 C7 -173.88(7) . . . . ? C3 N1 C4 C7 -54.43(10) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.310 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.059 data_lus47_(compound_2) _database_code_depnum_ccdc_archive 'CCDC 204074' _chemical_name_common '(N,N-Dimethylaminoxy)dimethylgallane - Dimer' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (N,N-Dimethylaminoxy)dimethylgallane - Dimer ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H12 Ga N O' _chemical_formula_weight 159.87 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 7.0678(3) _cell_length_b 8.5926(4) _cell_length_c 11.6957(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.516(3) _cell_angle_gamma 90.00 _cell_volume 695.99(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 39416 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 31.85 _exptl_crystal_description 'Hexagonal Prism' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 3.854 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Intensity corrections were applied by SCALEPACK: Z. Otwinowski, W. Minor Methods Enzymol 1997, 276, 307. ; _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 'Nonius DIP 2020' _diffrn_measurement_method 'Phi scans 2.0 deg' _diffrn_detector_area_resol_mean '8 - 0.68' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 39416 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 31.85 _reflns_number_total 2306 _reflns_number_gt 1968 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius-DIP 2020 Software' _computing_cell_refinement SCALEPACK _computing_data_reduction 'SCALEPACK, DIPSHEL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _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^)+(0.0725P)^2^+0.4076P] 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 SHELXL _refine_ls_extinction_coef 0.047(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2306 _refine_ls_number_parameters 85 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 Ga Ga 0.79502(4) 0.12410(3) 0.43599(2) 0.02977(14) Uani 1 1 d . . . C2 C 0.7450(5) 0.3436(3) 0.4662(3) 0.0380(6) Uani 1 1 d . . . H2A H 0.861(4) 0.3920(19) 0.502(3) 0.058(14) Uiso 1 1 calc R . . H2B H 0.656(4) 0.3499(4) 0.516(3) 0.076(16) Uiso 1 1 calc R . . H2C H 0.694(5) 0.3939(18) 0.395(2) 0.060(14) Uiso 1 1 calc R . . C1 C 0.6192(5) 0.0005(4) 0.3195(3) 0.0399(6) Uani 1 1 d . . . H1A H 0.687(2) -0.085(3) 0.2965(19) 0.052(12) Uiso 1 1 calc R . . H1B H 0.571(3) 0.0633(19) 0.254(2) 0.088(17) Uiso 1 1 calc R . . H1C H 0.515(3) -0.036(3) 0.3523(12) 0.053(12) Uiso 1 1 calc R . . N N 0.9412(4) -0.1125(2) 0.6133(2) 0.0310(4) Uani 1 1 d . . . C4 C 0.7981(5) -0.2244(4) 0.5542(3) 0.0378(6) Uani 1 1 d . . . H4A H 0.793(3) -0.220(2) 0.472(2) 0.062(13) Uiso 1 1 calc R . . H4B H 0.674(3) -0.1989(19) 0.5698(19) 0.054(13) Uiso 1 1 calc R . . H4C H 0.834(2) -0.327(3) 0.5823(18) 0.042(10) Uiso 1 1 calc R . . O O 0.8723(3) 0.0433(2) 0.58810(16) 0.0312(4) Uani 1 1 d . . . C3 C 0.9605(6) -0.1284(3) 0.7400(3) 0.0400(6) Uani 1 1 d . . . H3A H 1.044(3) -0.053(3) 0.7773(11) 0.048(11) Uiso 1 1 calc R . . H3B H 1.009(3) -0.226(3) 0.7631(8) 0.048(11) Uiso 1 1 calc R . . H3C H 0.841(3) -0.117(3) 0.7595(6) 0.037(10) 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 Ga 0.02941(19) 0.02671(19) 0.0318(2) -0.00126(9) 0.00276(11) 0.00158(10) C2 0.0428(16) 0.0266(12) 0.0420(15) -0.0033(10) 0.0025(12) 0.0059(10) C1 0.0350(14) 0.0406(15) 0.0399(15) -0.0072(12) -0.0024(11) -0.0011(11) N 0.0334(11) 0.0258(10) 0.0335(12) 0.0011(8) 0.0058(8) -0.0003(8) C4 0.0364(14) 0.0284(12) 0.0480(16) -0.0022(11) 0.0068(11) -0.0047(10) O 0.0366(10) 0.0253(8) 0.0315(9) 0.0022(7) 0.0062(7) 0.0037(7) C3 0.0499(17) 0.0365(15) 0.0340(15) 0.0035(11) 0.0095(12) 0.0016(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 Ga O 1.8862(19) . ? Ga C1 1.962(3) . ? Ga C2 1.964(3) . ? Ga N 2.061(3) 3_756 ? C2 H2A 0.9394 . ? C2 H2B 0.9394 . ? C2 H2C 0.9394 . ? C1 H1A 0.9478 . ? C1 H1B 0.9478 . ? C1 H1C 0.9478 . ? N O 1.435(3) . ? N C4 1.464(4) . ? N C3 1.468(4) . ? N Ga 2.061(3) 3_756 ? C4 H4A 0.9574 . ? C4 H4B 0.9574 . ? C4 H4C 0.9574 . ? C3 H3A 0.9245 . ? C3 H3B 0.9245 . ? C3 H3C 0.9245 . ? 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 O Ga C1 118.66(12) . . ? O Ga C2 102.26(12) . . ? C1 Ga C2 122.20(13) . . ? O Ga N 97.93(9) . 3_756 ? C1 Ga N 105.22(12) . 3_756 ? C2 Ga N 107.58(12) . 3_756 ? Ga C2 H2A 109.5 . . ? Ga C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Ga C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Ga C1 H1A 109.5 . . ? Ga C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Ga C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O N C4 110.0(2) . . ? O N C3 104.7(2) . . ? C4 N C3 109.4(2) . . ? O N Ga 106.05(15) . 3_756 ? C4 N Ga 114.48(19) . 3_756 ? C3 N Ga 111.8(2) . 3_756 ? N C4 H4A 109.5 . . ? N C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N O Ga 124.02(16) . . ? N C3 H3A 109.5 . . ? N C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 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 C4 N O Ga -55.8(3) . . . . ? C3 N O Ga -173.2(2) . . . . ? Ga N O Ga 68.4(2) 3_756 . . . ? C1 Ga O N 47.7(2) . . . . ? C2 Ga O N -174.5(2) . . . . ? N Ga O N -64.5(2) 3_756 . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 31.85 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.762 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.122