Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'William E. Buhro' 'Sean D. Dingman' 'Nigam Rath' _publ_contact_author_name 'Prof William E. Buhro' _publ_contact_author_address ; Department of Chemistry Washington University 1 Brookings Drive St. Louis Missouri 63130-4899 UNITED STATES OF AMERICA ; _publ_contact_author_email BUHRO@WUCHEM.WUSTL.EDU _publ_section_title ; Oligimerization of Dialkylazidogallium Compounds: A Structural and Solution-Phase Study ; data_e1399 _database_code_CSD 214951 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H66 Ga3 N9 Si6' _chemical_formula_weight 858.56 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' Si Si 0.0817 0.0704 '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 12.3854(1) _cell_length_b 13.5088(2) _cell_length_c 15.2823(2) _cell_angle_alpha 86.595(1) _cell_angle_beta 67.665(1) _cell_angle_gamma 87.91 _cell_volume 2360.64(5) _cell_formula_units_Z 2 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 1.877 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.6029 _exptl_absorpt_correction_T_max 0.7053 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'long 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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38359 _diffrn_reflns_av_R_equivalents 0.14 _diffrn_reflns_av_sigmaI/netI 0.1380 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8268 _reflns_number_gt 4153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL (Sheldrick, 1999)' _computing_structure_refinement 'Bruker SHELXTL (Sheldrick, 1999)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 1999)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 1999)' _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^)+(0.0400P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8268 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1369 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.91149(6) 0.73724(5) 0.28208(5) 0.0460(2) Uani 1 1 d . . . Ga2 Ga 0.72725(6) 0.68798(5) 0.14656(5) 0.0449(2) Uani 1 1 d . . . Ga3 Ga 0.70562(6) 0.92747(5) 0.25564(5) 0.0454(2) Uani 1 1 d . . . Si1 Si 0.9559(2) 0.70720(19) 0.48033(16) 0.0725(7) Uani 1 1 d . . . Si2 Si 1.16613(18) 0.76741(16) 0.10798(16) 0.0618(6) Uani 1 1 d . . . Si3 Si 0.71810(19) 0.67867(17) -0.06458(15) 0.0643(6) Uani 1 1 d . . . Si4 Si 0.5401(2) 0.52937(17) 0.29239(16) 0.0691(7) Uani 1 1 d . . . Si5 Si 0.45472(17) 1.00546(15) 0.25607(15) 0.0557(6) Uani 1 1 d . . . Si6 Si 0.8250(2) 1.11595(17) 0.30751(18) 0.0730(7) Uani 1 1 d . . . N1 N 0.8484(5) 0.6505(4) 0.2058(4) 0.0460(14) Uani 1 1 d . . . N2 N 0.8925(5) 0.5671(6) 0.1895(4) 0.0614(18) Uani 1 1 d . . . N3 N 0.9339(6) 0.4909(5) 0.1732(5) 0.086(2) Uani 1 1 d . . . N4 N 0.7545(5) 0.8374(4) 0.1444(4) 0.0462(15) Uani 1 1 d . . . N5 N 0.8336(6) 0.8698(4) 0.0711(5) 0.0539(16) Uani 1 1 d . . . N6 N 0.9065(6) 0.8996(5) 0.0032(5) 0.083(2) Uani 1 1 d . . . N7 N 0.7619(5) 0.8212(4) 0.3320(4) 0.0489(15) Uani 1 1 d . . . N8 N 0.6853(6) 0.7886(5) 0.4056(5) 0.0646(18) Uani 1 1 d . . . N9 N 0.6169(6) 0.7597(6) 0.4733(5) 0.102(3) Uani 1 1 d . . . C1 C 0.9185(6) 0.6508(5) 0.3868(5) 0.0557(19) Uani 1 1 d . . . H1A H 0.8423 0.6193 0.4178 0.067 Uiso 1 1 calc R . . H1B H 0.9759 0.5980 0.3598 0.067 Uiso 1 1 calc R . . C2 C 1.0306(5) 0.8229(5) 0.1922(4) 0.0506(18) Uani 1 1 d . . . H2A H 0.9938 0.8623 0.1549 0.061 Uiso 1 1 calc R . . H2B H 1.0533 0.8694 0.2288 0.061 Uiso 1 1 calc R . . C3 C 0.7950(6) 0.6456(5) 0.0185(5) 0.0547(19) Uani 1 1 d . . . H3A H 0.8739 0.6726 -0.0103 0.066 Uiso 1 1 calc R . . H3B H 0.8035 0.5733 0.0217 0.066 Uiso 1 1 calc R . . C4 C 0.5747(5) 0.6590(5) 0.2450(5) 0.0556(19) Uani 1 1 d . . . H4A H 0.5654 0.6996 0.2985 0.067 Uiso 1 1 calc R . . H4B H 0.5154 0.6818 0.2201 0.067 Uiso 1 1 calc R . . C5 C 0.5357(5) 0.9315(5) 0.3188(4) 0.0484(18) Uani 1 1 d . . . H5A H 0.5076 0.8632 0.3290 0.058 Uiso 1 1 calc R . . H5B H 0.5160 0.9583 0.3814 0.058 Uiso 1 1 calc R . . C6 C 0.8083(6) 1.0422(4) 0.2147(5) 0.0542(19) Uani 1 1 d . . . H6A H 0.8861 1.0188 0.1741 0.065 Uiso 1 1 calc R . . H6B H 0.7796 1.0871 0.1753 0.065 Uiso 1 1 calc R . . C11 C 0.8387(10) 0.7797(10) 0.5538(8) 0.198(7) Uani 1 1 d . . . H11A H 0.8231 0.8348 0.5163 0.297 Uiso 1 1 calc R . . H11B H 0.8588 0.8049 0.6036 0.297 Uiso 1 1 calc R . . H11C H 0.7697 0.7392 0.5817 0.297 Uiso 1 1 calc R . . C12 C 0.9791(11) 0.6057(8) 0.5639(8) 0.182(6) Uani 1 1 d . . . H12A H 0.9985 0.6355 0.6122 0.273 Uiso 1 1 calc R . . H12B H 1.0424 0.5619 0.5283 0.273 Uiso 1 1 calc R . . H12C H 0.9081 0.5679 0.5938 0.273 Uiso 1 1 calc R . . C13 C 1.0954(10) 0.7657(10) 0.4293(7) 0.193(7) Uani 1 1 d . . . H13A H 1.0920 0.8197 0.3856 0.289 Uiso 1 1 calc R . . H13B H 1.1543 0.7175 0.3955 0.289 Uiso 1 1 calc R . . H13C H 1.1152 0.7914 0.4791 0.289 Uiso 1 1 calc R . . C21 C 1.2404(7) 0.6942(7) 0.1747(6) 0.125(4) Uani 1 1 d . . . H21A H 1.3113 0.6644 0.1308 0.188 Uiso 1 1 calc R . . H21B H 1.1891 0.6424 0.2135 0.188 Uiso 1 1 calc R . . H21C H 1.2599 0.7372 0.2150 0.188 Uiso 1 1 calc R . . C22 C 1.2644(7) 0.8680(6) 0.0361(6) 0.095(3) Uani 1 1 d . . . H22A H 1.3358 0.8391 -0.0079 0.143 Uiso 1 1 calc R . . H22B H 1.2829 0.9101 0.0776 0.143 Uiso 1 1 calc R . . H22C H 1.2258 0.9073 0.0010 0.143 Uiso 1 1 calc R . . C23 C 1.1370(8) 0.6917(7) 0.0229(7) 0.133(4) Uani 1 1 d . . . H23A H 1.2097 0.6630 -0.0194 0.199 Uiso 1 1 calc R . . H23B H 1.1022 0.7333 -0.0136 0.199 Uiso 1 1 calc R . . H23C H 1.0837 0.6391 0.0571 0.199 Uiso 1 1 calc R . . C31 C 0.5604(7) 0.6583(9) -0.0036(6) 0.141(4) Uani 1 1 d . . . H31A H 0.5212 0.6771 -0.0463 0.212 Uiso 1 1 calc R . . H31B H 0.5300 0.6982 0.0515 0.212 Uiso 1 1 calc R . . H31C H 0.5470 0.5887 0.0162 0.212 Uiso 1 1 calc R . . C32 C 0.7314(10) 0.8128(7) -0.0991(7) 0.149(5) Uani 1 1 d . . . H32A H 0.6897 0.8289 -0.1405 0.224 Uiso 1 1 calc R . . H32B H 0.8132 0.8289 -0.1320 0.224 Uiso 1 1 calc R . . H32C H 0.6985 0.8509 -0.0428 0.224 Uiso 1 1 calc R . . C33 C 0.7812(9) 0.6086(7) -0.1725(6) 0.129(4) Uani 1 1 d . . . H33A H 0.7405 0.6267 -0.2144 0.193 Uiso 1 1 calc R . . H33B H 0.7730 0.5381 -0.1557 0.193 Uiso 1 1 calc R . . H33C H 0.8632 0.6240 -0.2043 0.193 Uiso 1 1 calc R . . C41 C 0.5833(9) 0.4421(6) 0.1951(6) 0.129(4) Uani 1 1 d . . . H41A H 0.6666 0.4464 0.1589 0.194 Uiso 1 1 calc R . . H41B H 0.5414 0.4593 0.1539 0.194 Uiso 1 1 calc R . . H41C H 0.5644 0.3749 0.2216 0.194 Uiso 1 1 calc R . . C42 C 0.3809(7) 0.5190(7) 0.3612(6) 0.109(3) Uani 1 1 d . . . H42A H 0.3389 0.5387 0.3207 0.164 Uiso 1 1 calc R . . H42B H 0.3580 0.5619 0.4141 0.164 Uiso 1 1 calc R . . H42C H 0.3627 0.4509 0.3847 0.164 Uiso 1 1 calc R . . C43 C 0.6194(7) 0.4915(6) 0.3707(6) 0.092(3) Uani 1 1 d . . . H43A H 0.7028 0.4965 0.3351 0.138 Uiso 1 1 calc R . . H43B H 0.6006 0.4235 0.3945 0.138 Uiso 1 1 calc R . . H43C H 0.5963 0.5347 0.4235 0.138 Uiso 1 1 calc R . . C51 C 0.5012(7) 0.9650(6) 0.1340(5) 0.082(3) Uani 1 1 d . . . H51A H 0.5843 0.9752 0.1012 0.123 Uiso 1 1 calc R . . H51B H 0.4591 1.0033 0.1010 0.123 Uiso 1 1 calc R . . H51C H 0.4845 0.8952 0.1354 0.123 Uiso 1 1 calc R . . C52 C 0.2950(6) 0.9853(6) 0.3203(6) 0.094(3) Uani 1 1 d . . . H52A H 0.2785 0.9155 0.3214 0.141 Uiso 1 1 calc R . . H52B H 0.2521 1.0239 0.2882 0.141 Uiso 1 1 calc R . . H52C H 0.2713 1.0062 0.3847 0.141 Uiso 1 1 calc R . . C53 C 0.4871(6) 1.1396(5) 0.2536(6) 0.075(2) Uani 1 1 d . . . H53A H 0.5704 1.1496 0.2211 0.113 Uiso 1 1 calc R . . H53B H 0.4623 1.1609 0.3179 0.113 Uiso 1 1 calc R . . H53C H 0.4456 1.1781 0.2203 0.113 Uiso 1 1 calc R . . C61 C 0.6943(8) 1.1149(8) 0.4146(6) 0.136(4) Uani 1 1 d . . . H61A H 0.6297 1.1439 0.4004 0.203 Uiso 1 1 calc R . . H61B H 0.7071 1.1532 0.4615 0.203 Uiso 1 1 calc R . . H61C H 0.6762 1.0471 0.4393 0.203 Uiso 1 1 calc R . . C62 C 0.9466(9) 1.0601(9) 0.3406(9) 0.202(8) Uani 1 1 d . . . H62A H 0.9549 1.0976 0.3898 0.303 Uiso 1 1 calc R . . H62B H 1.0190 1.0620 0.2854 0.303 Uiso 1 1 calc R . . H62C H 0.9285 0.9918 0.3637 0.303 Uiso 1 1 calc R . . C63 C 0.8580(13) 1.2462(7) 0.2641(8) 0.207(7) Uani 1 1 d . . . H63A H 0.7956 1.2743 0.2463 0.311 Uiso 1 1 calc R . . H63B H 0.9310 1.2488 0.2094 0.311 Uiso 1 1 calc R . . H63C H 0.8648 1.2840 0.3138 0.311 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 0.0389(5) 0.0556(5) 0.0517(5) -0.0016(4) -0.0266(4) -0.0001(4) Ga2 0.0412(5) 0.0507(5) 0.0501(5) -0.0016(4) -0.0253(4) -0.0062(4) Ga3 0.0400(5) 0.0484(5) 0.0520(5) -0.0023(4) -0.0221(4) -0.0010(4) Si1 0.0671(16) 0.104(2) 0.0626(16) -0.0064(13) -0.0430(14) -0.0002(14) Si2 0.0438(13) 0.0676(15) 0.0700(16) 0.0012(12) -0.0176(12) -0.0036(11) Si3 0.0595(15) 0.0893(18) 0.0560(15) -0.0075(12) -0.0342(12) -0.0037(13) Si4 0.0700(16) 0.0752(16) 0.0661(16) 0.0097(12) -0.0300(13) -0.0282(13) Si5 0.0410(12) 0.0612(14) 0.0696(15) 0.0048(11) -0.0272(11) -0.0016(10) Si6 0.0668(16) 0.0670(16) 0.0913(19) -0.0226(13) -0.0335(15) -0.0091(13) N1 0.049(4) 0.044(4) 0.054(4) -0.003(3) -0.029(3) -0.005(3) N2 0.052(5) 0.049(5) 0.092(5) -0.007(4) -0.037(4) -0.005(4) N3 0.077(5) 0.054(5) 0.137(7) -0.018(5) -0.050(5) 0.016(4) N4 0.034(3) 0.053(4) 0.047(4) 0.008(3) -0.012(3) -0.003(3) N5 0.056(5) 0.051(4) 0.066(5) -0.009(4) -0.035(4) 0.002(4) N6 0.077(5) 0.092(6) 0.069(5) -0.004(4) -0.012(4) -0.022(4) N7 0.046(4) 0.062(4) 0.047(4) 0.000(3) -0.028(3) 0.001(3) N8 0.052(5) 0.091(5) 0.053(5) 0.008(4) -0.024(4) 0.002(4) N9 0.068(5) 0.153(8) 0.071(6) 0.031(5) -0.017(4) 0.019(5) C1 0.060(5) 0.063(5) 0.059(5) -0.002(4) -0.039(4) -0.003(4) C2 0.046(4) 0.055(5) 0.058(5) -0.012(4) -0.026(4) -0.005(4) C3 0.051(5) 0.050(5) 0.069(5) 0.002(4) -0.030(4) -0.007(4) C4 0.046(4) 0.060(5) 0.064(5) 0.002(4) -0.026(4) -0.007(4) C5 0.043(4) 0.055(5) 0.046(4) -0.012(3) -0.016(4) 0.009(4) C6 0.049(5) 0.042(4) 0.067(5) -0.001(4) -0.019(4) -0.001(3) C11 0.178(13) 0.285(17) 0.186(13) -0.149(13) -0.116(11) 0.062(12) C12 0.305(18) 0.152(11) 0.157(12) 0.016(9) -0.166(13) -0.001(11) C13 0.157(11) 0.335(18) 0.088(9) -0.039(10) -0.032(8) -0.145(11) C21 0.066(6) 0.143(9) 0.135(9) 0.039(7) -0.013(6) 0.047(6) C22 0.065(6) 0.109(7) 0.094(7) 0.010(5) -0.011(5) -0.026(5) C23 0.087(7) 0.160(10) 0.125(9) -0.073(8) 0.002(7) -0.034(7) C31 0.071(7) 0.278(14) 0.091(8) 0.020(8) -0.050(6) -0.035(8) C32 0.240(14) 0.116(9) 0.174(11) 0.030(7) -0.175(11) -0.027(8) C33 0.155(10) 0.172(10) 0.094(8) -0.063(7) -0.081(8) 0.050(8) C41 0.206(12) 0.072(7) 0.111(8) -0.010(6) -0.057(8) -0.045(7) C42 0.074(6) 0.130(8) 0.121(8) 0.048(6) -0.039(6) -0.039(6) C43 0.088(7) 0.093(7) 0.089(7) 0.025(5) -0.031(6) -0.012(5) C51 0.079(6) 0.102(7) 0.076(6) 0.005(5) -0.042(5) -0.008(5) C52 0.042(5) 0.121(8) 0.114(8) 0.018(6) -0.027(5) -0.003(5) C53 0.074(6) 0.060(5) 0.108(7) 0.007(5) -0.054(5) 0.005(4) C61 0.106(8) 0.210(12) 0.093(8) -0.079(8) -0.030(7) -0.007(8) C62 0.132(10) 0.274(15) 0.287(16) -0.223(14) -0.160(11) 0.126(11) C63 0.36(2) 0.085(9) 0.185(13) -0.013(8) -0.110(14) -0.095(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 Ga1 C2 1.950(6) . ? Ga1 C1 1.951(6) . ? Ga1 N7 2.043(5) . ? Ga1 N1 2.064(5) . ? Ga2 C3 1.927(7) . ? Ga2 C4 1.951(6) . ? Ga2 N4 2.055(5) . ? Ga2 N1 2.062(5) . ? Ga3 C5 1.954(6) . ? Ga3 C6 1.959(6) . ? Ga3 N4 2.036(5) . ? Ga3 N7 2.063(5) . ? Si1 C11 1.765(10) . ? Si1 C13 1.793(10) . ? Si1 C1 1.871(6) . ? Si1 C12 1.907(9) . ? Si2 C21 1.842(8) . ? Si2 C23 1.846(8) . ? Si2 C2 1.848(6) . ? Si2 C22 1.861(8) . ? Si3 C33 1.838(8) . ? Si3 C31 1.839(8) . ? Si3 C32 1.853(9) . ? Si3 C3 1.881(6) . ? Si4 C43 1.855(8) . ? Si4 C42 1.854(8) . ? Si4 C41 1.856(8) . ? Si4 C4 1.856(7) . ? Si5 C51 1.842(7) . ? Si5 C5 1.863(6) . ? Si5 C52 1.866(7) . ? Si5 C53 1.866(7) . ? Si6 C61 1.813(9) . ? Si6 C63 1.847(10) . ? Si6 C6 1.858(7) . ? Si6 C62 1.882(9) . ? N1 N2 1.230(7) . ? N2 N3 1.132(7) . ? N4 N5 1.243(8) . ? N5 N6 1.148(8) . ? N7 N8 1.233(8) . ? N8 N9 1.119(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ga1 C1 129.6(3) . . ? C2 Ga1 N7 106.5(2) . . ? C1 Ga1 N7 107.9(3) . . ? C2 Ga1 N1 107.9(2) . . ? C1 Ga1 N1 105.5(2) . . ? N7 Ga1 N1 93.6(2) . . ? C3 Ga2 C4 129.6(3) . . ? C3 Ga2 N4 108.4(3) . . ? C4 Ga2 N4 107.8(2) . . ? C3 Ga2 N1 105.6(2) . . ? C4 Ga2 N1 106.2(2) . . ? N4 Ga2 N1 93.2(2) . . ? C5 Ga3 C6 126.2(3) . . ? C5 Ga3 N4 110.3(2) . . ? C6 Ga3 N4 106.8(2) . . ? C5 Ga3 N7 105.3(2) . . ? C6 Ga3 N7 112.3(2) . . ? N4 Ga3 N7 90.0(2) . . ? C11 Si1 C13 116.6(6) . . ? C11 Si1 C1 111.2(4) . . ? C13 Si1 C1 110.6(4) . . ? C11 Si1 C12 104.5(6) . . ? C13 Si1 C12 103.3(6) . . ? C1 Si1 C12 110.0(4) . . ? C21 Si2 C23 111.5(5) . . ? C21 Si2 C2 109.2(4) . . ? C23 Si2 C2 111.8(3) . . ? C21 Si2 C22 108.9(4) . . ? C23 Si2 C22 106.1(4) . . ? C2 Si2 C22 109.3(3) . . ? C33 Si3 C31 112.0(5) . . ? C33 Si3 C32 108.5(5) . . ? C31 Si3 C32 105.1(5) . . ? C33 Si3 C3 110.7(4) . . ? C31 Si3 C3 110.0(4) . . ? C32 Si3 C3 110.5(3) . . ? C43 Si4 C42 109.0(4) . . ? C43 Si4 C41 107.8(4) . . ? C42 Si4 C41 108.7(4) . . ? C43 Si4 C4 110.7(3) . . ? C42 Si4 C4 109.6(4) . . ? C41 Si4 C4 111.0(4) . . ? C51 Si5 C5 109.2(3) . . ? C51 Si5 C52 109.9(4) . . ? C5 Si5 C52 109.0(3) . . ? C51 Si5 C53 109.6(4) . . ? C5 Si5 C53 109.4(3) . . ? C52 Si5 C53 109.7(4) . . ? C61 Si6 C63 108.1(5) . . ? C61 Si6 C6 112.1(4) . . ? C63 Si6 C6 110.5(4) . . ? C61 Si6 C62 107.1(5) . . ? C63 Si6 C62 109.9(6) . . ? C6 Si6 C62 109.1(4) . . ? N2 N1 Ga2 115.3(4) . . ? N2 N1 Ga1 116.2(4) . . ? Ga2 N1 Ga1 128.4(3) . . ? N3 N2 N1 179.0(8) . . ? N5 N4 Ga3 115.2(4) . . ? N5 N4 Ga2 114.0(4) . . ? Ga3 N4 Ga2 128.3(3) . . ? N6 N5 N4 179.7(8) . . ? N8 N7 Ga1 115.8(4) . . ? N8 N7 Ga3 114.9(4) . . ? Ga1 N7 Ga3 126.5(3) . . ? N9 N8 N7 178.6(9) . . ? Si1 C1 Ga1 118.2(3) . . ? Si2 C2 Ga1 119.6(3) . . ? Si3 C3 Ga2 119.0(3) . . ? Si4 C4 Ga2 119.3(3) . . ? Si5 C5 Ga3 116.3(3) . . ? Si6 C6 Ga3 118.0(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.885 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.113