# Copyright TheRoyal Society of Chemistry, 1998 # CCDC Number: 186/1222 data_global _publ_contact_autor ; Martin Nieger Institut f\"ur Anorganische Chemie Universit\"at Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; _publ_contact_author_phone '049 228 73-5823' _publ_contact_author_fax '049 228 73-5327' _publ_contact_author_email 'NIEGER@OC3062.CHEMIE.UNI-BONN.DE' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; enclosed you will fond the necessary data for our publication in J. Chem. Soc., Dalton Trans. ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Simple Synthesis of Organogallium Azides - Structural Characterization of [Mes~2~GaN~3~]~2~ ; loop_ _publ_author_name _publ_author_address 'Schulz, Stephan' ; Institut f\"ur Anorganische Chemie Universit\"at Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; 'Nieger, Martin' ; Institut f\"ur Anorganische Chemie Universit\"at Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; #============================================================================== data_schulz03_compound_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bismesitylgallium azide [Mes~2~GaN~3~]~2~ ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 Ga2 N6' _chemical_formula_weight 700.21 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' '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 (no.2)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2385(4) _cell_length_b 13.6773(4) _cell_length_c 14.0356(5) _cell_angle_alpha 69.309(2) _cell_angle_beta 74.268(2) _cell_angle_gamma 75.279(2) _cell_volume 1742.26(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 27521 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.579 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min '0.5707 (theor.)' _exptl_absorpt_correction_T_max '0.7430 (theor.)' _exptl_special_details ; dx = 28.893(1) mm; mos.= 0.785(2); scan 120 sec., 200 frames, 2 deg. ; _diffrn_ambient_temperature 123(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 Kappa-CCD' _diffrn_measurement_method 'rotation in phi, 2 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27441 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6472 _reflns_number_gt 5615 _reflns_threshold_expression >2sigma(I) _computing_data_collection Kappa-CCD _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+1.0576P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0110(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6472 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.72175(2) 0.797499(17) 0.859960(16) 0.02075(8) Uani 1 d . . . Ga2 Ga 0.76445(2) 0.652235(17) 0.715673(16) 0.02094(8) Uani 1 d . . . N1 N 0.61555(18) 0.71735(14) 0.81696(14) 0.0245(4) Uani 1 d . . . N2 N 0.4925(2) 0.71241(16) 0.84030(14) 0.0308(4) Uani 1 d . . . N3 N 0.3788(2) 0.7077(2) 0.86135(18) 0.0498(6) Uani 1 d . . . N4 N 0.87430(18) 0.70953(13) 0.78001(13) 0.0229(4) Uani 1 d . . . N5 N 0.9970(2) 0.68799(15) 0.78125(15) 0.0308(4) Uani 1 d . . . N6 N 1.1114(2) 0.6685(2) 0.7821(2) 0.0544(6) Uani 1 d . . . C1 C 0.7395(2) 0.74218(16) 1.00701(16) 0.0219(4) Uani 1 d . . . C2 C 0.6731(2) 0.66160(16) 1.08415(16) 0.0245(4) Uani 1 d . . . C3 C 0.7015(2) 0.62575(17) 1.18435(17) 0.0282(5) Uani 1 d . . . H3 H 0.6576 0.5707 1.2357 0.034 Uiso 1 calc R . . C4 C 0.7906(2) 0.66718(17) 1.21145(16) 0.0283(5) Uani 1 d . . . C5 C 0.8522(2) 0.74933(17) 1.13557(17) 0.0269(5) Uani 1 d . . . H5 H 0.9105 0.7815 1.1533 0.032 Uiso 1 calc R . . C6 C 0.8299(2) 0.78509(16) 1.03426(16) 0.0234(4) Uani 1 d . . . C7 C 0.5691(3) 0.6143(2) 1.06464(18) 0.0346(5) Uani 1 d . . . H7A H 0.5313 0.5634 1.1294 0.052 Uiso 1 calc R . . H7B H 0.6138 0.5779 1.0122 0.052 Uiso 1 calc R . . H7C H 0.4944 0.6709 1.0396 0.052 Uiso 1 calc R . . C8 C 0.8231(3) 0.6260(2) 1.31902(18) 0.0392(6) Uani 1 d . . . H8A H 0.7797 0.5638 1.3600 0.059 Uiso 1 calc R . . H8B H 0.7875 0.6816 1.3531 0.059 Uiso 1 calc R . . H8C H 0.9232 0.6061 1.3137 0.059 Uiso 1 calc R . . C9 C 0.9091(2) 0.86856(18) 0.95434(18) 0.0318(5) Uani 1 d . . . H9A H 0.9496 0.9002 0.9897 0.048 Uiso 1 calc R . . H9B H 0.8464 0.9239 0.9135 0.048 Uiso 1 calc R . . H9C H 0.9826 0.8356 0.9081 0.048 Uiso 1 calc R . . C10 C 0.6806(2) 0.94640(16) 0.77218(16) 0.0236(4) Uani 1 d . . . C11 C 0.7683(2) 0.99652(17) 0.68189(16) 0.0256(5) Uani 1 d . . . C12 C 0.7218(2) 1.10049(17) 0.62253(17) 0.0290(5) Uani 1 d . . . H12 H 0.7810 1.1334 0.5606 0.035 Uiso 1 calc R . . C13 C 0.5930(2) 1.15633(17) 0.65127(18) 0.0308(5) Uani 1 d . . . C14 C 0.5080(2) 1.10805(17) 0.74337(18) 0.0307(5) Uani 1 d . . . H14 H 0.4205 1.1464 0.7659 0.037 Uiso 1 calc R . . C15 C 0.5498(2) 1.00434(17) 0.80282(17) 0.0259(5) Uani 1 d . . . C16 C 0.9125(2) 0.94315(18) 0.64505(18) 0.0320(5) Uani 1 d . . . H16A H 0.9080 0.8934 0.6106 0.048 Uiso 1 calc R . . H16B H 0.9569 0.9045 0.7048 0.048 Uiso 1 calc R . . H16C H 0.9661 0.9970 0.5959 0.048 Uiso 1 calc R . . C17 C 0.5439(3) 1.26770(18) 0.5853(2) 0.0383(6) Uani 1 d . . . H17A H 0.6211 1.2941 0.5310 0.058 Uiso 1 calc R . . H17B H 0.5081 1.3145 0.6293 0.058 Uiso 1 calc R . . H17C H 0.4707 1.2666 0.5531 0.058 Uiso 1 calc R . . C18 C 0.4515(2) 0.95534(18) 0.90094(18) 0.0326(5) Uani 1 d . . . H18A H 0.3798 1.0115 0.9208 0.049 Uiso 1 calc R . . H18B H 0.5025 0.9171 0.9571 0.049 Uiso 1 calc R . . H18C H 0.4088 0.9058 0.8883 0.049 Uiso 1 calc R . . C19 C 0.7774(2) 0.75047(16) 0.57261(16) 0.0239(4) Uani 1 d . . . C20 C 0.6653(2) 0.82481(17) 0.53491(17) 0.0281(5) Uani 1 d . . . C21 C 0.6873(3) 0.89432(17) 0.43379(18) 0.0324(5) Uani 1 d . . . H21 H 0.6111 0.9439 0.4088 0.039 Uiso 1 calc R . . C22 C 0.8144(3) 0.89383(18) 0.36919(18) 0.0344(6) Uani 1 d . . . C23 C 0.9244(3) 0.81851(18) 0.40537(17) 0.0325(5) Uani 1 d . . . H23 H 1.0130 0.8155 0.3611 0.039 Uiso 1 calc R . . C24 C 0.9063(2) 0.74703(17) 0.50625(17) 0.0271(5) Uani 1 d . . . C25 C 0.5221(2) 0.8318(2) 0.59993(19) 0.0366(6) Uani 1 d . . . H25A H 0.5167 0.8657 0.6522 0.055 Uiso 1 calc R . . H25B H 0.5003 0.7603 0.6348 0.055 Uiso 1 calc R . . H25C H 0.4560 0.8740 0.5553 0.055 Uiso 1 calc R . . C26 C 0.8334(3) 0.9714(2) 0.26030(19) 0.0469(7) Uani 1 d . . . H26A H 0.7775 0.9591 0.2203 0.070 Uiso 1 calc R . . H26B H 0.9307 0.9610 0.2262 0.070 Uiso 1 calc R . . H26C H 0.8041 1.0442 0.2640 0.070 Uiso 1 calc R . . C27 C 1.0298(3) 0.6662(2) 0.53961(19) 0.0400(6) Uani 1 d . . . H27A H 1.0773 0.6949 0.5730 0.060 Uiso 1 calc R . . H27B H 1.0930 0.6503 0.4786 0.060 Uiso 1 calc R . . H27C H 0.9991 0.6010 0.5889 0.060 Uiso 1 calc R . . C28 C 0.7727(2) 0.49755(16) 0.76492(15) 0.0220(4) Uani 1 d . . . C29 C 0.7290(2) 0.45259(17) 0.70565(16) 0.0260(5) Uani 1 d . . . C30 C 0.7317(2) 0.34354(17) 0.73648(17) 0.0283(5) Uani 1 d . . . H30 H 0.7048 0.3144 0.6941 0.034 Uiso 1 calc R . . C31 C 0.7730(2) 0.27643(16) 0.82797(16) 0.0261(5) Uani 1 d . . . C32 C 0.8131(2) 0.32098(16) 0.88719(16) 0.0242(4) Uani 1 d . . . H32 H 0.8395 0.2763 0.9507 0.029 Uiso 1 calc R . . C33 C 0.8164(2) 0.42944(16) 0.85749(16) 0.0228(4) Uani 1 d . . . C34 C 0.6751(3) 0.52023(19) 0.60772(18) 0.0399(6) Uani 1 d . . . H34A H 0.6575 0.4741 0.5744 0.060 Uiso 1 calc R . . H34B H 0.7437 0.5628 0.5597 0.060 Uiso 1 calc R . . H34C H 0.5892 0.5674 0.6258 0.060 Uiso 1 calc R . . C35 C 0.7717(3) 0.15942(17) 0.86124(18) 0.0359(6) Uani 1 d . . . H35A H 0.8157 0.1234 0.9215 0.054 Uiso 1 calc R . . H35B H 0.8223 0.1309 0.8039 0.054 Uiso 1 calc R . . H35C H 0.6763 0.1477 0.8800 0.054 Uiso 1 calc R . . C36 C 0.8725(3) 0.46623(18) 0.92544(17) 0.0319(5) Uani 1 d . . . H36A H 0.8540 0.4199 0.9973 0.048 Uiso 1 calc R . . H36B H 0.8277 0.5394 0.9225 0.048 Uiso 1 calc R . . H36C H 0.9721 0.4633 0.9007 0.048 Uiso 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 0.02499(14) 0.01862(13) 0.01837(13) -0.00403(10) -0.00441(9) -0.00562(9) Ga2 0.02668(14) 0.01715(13) 0.01820(13) -0.00348(10) -0.00544(9) -0.00422(9) N1 0.0243(10) 0.0261(9) 0.0251(9) -0.0098(8) -0.0030(7) -0.0069(7) N2 0.0316(12) 0.0381(11) 0.0263(10) -0.0124(9) -0.0038(8) -0.0108(8) N3 0.0307(13) 0.0850(19) 0.0444(13) -0.0295(13) 0.0003(10) -0.0227(12) N4 0.0239(10) 0.0222(9) 0.0230(9) -0.0070(8) -0.0042(7) -0.0049(7) N5 0.0322(12) 0.0315(10) 0.0321(10) -0.0133(9) -0.0075(8) -0.0054(8) N6 0.0306(13) 0.0723(17) 0.0727(17) -0.0381(15) -0.0170(12) -0.0003(11) C1 0.0240(11) 0.0185(10) 0.0206(10) -0.0066(9) -0.0031(8) 0.0000(8) C2 0.0258(11) 0.0219(10) 0.0239(11) -0.0076(9) -0.0024(9) -0.0028(8) C3 0.0331(12) 0.0234(11) 0.0213(11) -0.0028(9) -0.0002(9) -0.0047(9) C4 0.0328(12) 0.0260(11) 0.0218(11) -0.0069(10) -0.0060(9) 0.0024(9) C5 0.0307(12) 0.0244(11) 0.0263(11) -0.0084(10) -0.0101(9) -0.0006(9) C6 0.0271(11) 0.0175(10) 0.0234(10) -0.0049(9) -0.0070(9) -0.0002(8) C7 0.0401(14) 0.0381(13) 0.0249(11) -0.0045(11) -0.0003(10) -0.0196(11) C8 0.0468(15) 0.0415(14) 0.0256(12) -0.0038(11) -0.0121(11) -0.0052(11) C9 0.0409(14) 0.0263(11) 0.0301(12) -0.0004(10) -0.0144(10) -0.0135(10) C10 0.0315(12) 0.0200(10) 0.0211(10) -0.0030(9) -0.0098(9) -0.0077(8) C11 0.0363(12) 0.0223(10) 0.0220(10) -0.0077(9) -0.0075(9) -0.0084(9) C12 0.0400(13) 0.0267(11) 0.0227(11) -0.0022(10) -0.0088(10) -0.0151(10) C13 0.0399(13) 0.0238(11) 0.0322(12) -0.0028(10) -0.0174(10) -0.0088(10) C14 0.0326(12) 0.0250(11) 0.0346(12) -0.0056(10) -0.0116(10) -0.0047(9) C15 0.0297(12) 0.0232(11) 0.0255(11) -0.0052(10) -0.0089(9) -0.0054(9) C16 0.0374(13) 0.0274(12) 0.0282(12) -0.0063(10) 0.0024(10) -0.0135(10) C17 0.0466(15) 0.0259(12) 0.0419(14) 0.0017(11) -0.0218(12) -0.0089(10) C18 0.0314(13) 0.0291(12) 0.0309(12) -0.0056(11) -0.0029(10) -0.0030(9) C19 0.0346(12) 0.0181(10) 0.0203(10) -0.0016(9) -0.0094(9) -0.0089(8) C20 0.0414(13) 0.0195(10) 0.0272(11) -0.0072(10) -0.0132(10) -0.0051(9) C21 0.0467(15) 0.0201(11) 0.0315(12) -0.0022(10) -0.0188(11) -0.0043(10) C22 0.0544(16) 0.0246(12) 0.0265(12) 0.0032(10) -0.0175(11) -0.0169(11) C23 0.0399(14) 0.0332(12) 0.0238(11) -0.0020(10) -0.0045(10) -0.0168(10) C24 0.0356(12) 0.0230(11) 0.0225(11) -0.0022(9) -0.0085(9) -0.0086(9) C25 0.0389(14) 0.0353(13) 0.0332(13) -0.0088(11) -0.0160(11) 0.0049(10) C26 0.0666(19) 0.0402(15) 0.0293(13) 0.0090(12) -0.0167(13) -0.0223(13) C27 0.0335(13) 0.0452(15) 0.0273(12) -0.0003(11) -0.0013(10) -0.0033(11) C28 0.0247(11) 0.0196(10) 0.0182(10) -0.0027(9) -0.0024(8) -0.0043(8) C29 0.0346(12) 0.0223(11) 0.0194(10) -0.0033(9) -0.0052(9) -0.0066(9) C30 0.0416(13) 0.0235(11) 0.0220(11) -0.0064(10) -0.0067(9) -0.0100(9) C31 0.0302(12) 0.0206(10) 0.0222(11) -0.0022(9) -0.0004(9) -0.0068(8) C32 0.0274(11) 0.0212(10) 0.0183(10) -0.0016(9) -0.0031(8) -0.0022(8) C33 0.0254(11) 0.0222(10) 0.0185(10) -0.0044(9) -0.0028(8) -0.0044(8) C34 0.0708(18) 0.0267(12) 0.0286(12) -0.0015(11) -0.0247(12) -0.0138(12) C35 0.0547(16) 0.0212(11) 0.0279(12) -0.0031(10) -0.0047(11) -0.0104(10) C36 0.0439(14) 0.0257(11) 0.0262(11) -0.0021(10) -0.0160(10) -0.0052(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 C1 1.974(2) . ? Ga1 C10 1.979(2) . ? Ga1 N1 2.0439(18) . ? Ga1 N4 2.0481(18) . ? Ga2 C28 1.967(2) . ? Ga2 C19 1.973(2) . ? Ga2 N1 2.0415(18) . ? Ga2 N4 2.0477(18) . ? N1 N2 1.226(3) . ? N2 N3 1.133(3) . ? N4 N5 1.219(3) . ? N5 N6 1.136(3) . ? C1 C6 1.405(3) . ? C1 C2 1.409(3) . ? C2 C3 1.402(3) . ? C2 C7 1.503(3) . ? C3 C4 1.379(3) . ? C4 C5 1.395(3) . ? C4 C8 1.511(3) . ? C5 C6 1.393(3) . ? C6 C9 1.514(3) . ? C10 C11 1.401(3) . ? C10 C15 1.413(3) . ? C11 C12 1.406(3) . ? C11 C16 1.512(3) . ? C12 C13 1.379(3) . ? C13 C14 1.394(3) . ? C13 C17 1.516(3) . ? C14 C15 1.393(3) . ? C15 C18 1.515(3) . ? C19 C24 1.394(3) . ? C19 C20 1.410(3) . ? C20 C21 1.397(3) . ? C20 C25 1.502(3) . ? C21 C22 1.370(4) . ? C22 C23 1.393(3) . ? C22 C26 1.515(3) . ? C23 C24 1.402(3) . ? C24 C27 1.512(3) . ? C28 C29 1.404(3) . ? C28 C33 1.416(3) . ? C29 C30 1.394(3) . ? C29 C34 1.518(3) . ? C30 C31 1.391(3) . ? C31 C32 1.379(3) . ? C31 C35 1.503(3) . ? C32 C33 1.399(3) . ? C33 C36 1.508(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ga1 C10 129.18(9) . . ? C1 Ga1 N1 115.42(8) . . ? C10 Ga1 N1 104.34(8) . . ? C1 Ga1 N4 107.82(7) . . ? C10 Ga1 N4 111.20(8) . . ? N1 Ga1 N4 76.72(7) . . ? C28 Ga2 C19 129.21(9) . . ? C28 Ga2 N1 108.73(8) . . ? C19 Ga2 N1 110.74(8) . . ? C28 Ga2 N4 116.22(8) . . ? C19 Ga2 N4 102.98(8) . . ? N1 Ga2 N4 76.78(7) . . ? N2 N1 Ga2 127.26(15) . . ? N2 N1 Ga1 130.07(15) . . ? Ga2 N1 Ga1 102.57(8) . . ? N3 N2 N1 179.6(2) . . ? N5 N4 Ga2 129.49(15) . . ? N5 N4 Ga1 127.82(15) . . ? Ga2 N4 Ga1 102.21(7) . . ? N6 N5 N4 179.6(2) . . ? C6 C1 C2 118.50(18) . . ? C6 C1 Ga1 116.21(15) . . ? C2 C1 Ga1 125.24(16) . . ? C3 C2 C1 119.1(2) . . ? C3 C2 C7 118.15(19) . . ? C1 C2 C7 122.75(19) . . ? C4 C3 C2 122.7(2) . . ? C3 C4 C5 117.83(19) . . ? C3 C4 C8 122.2(2) . . ? C5 C4 C8 120.0(2) . . ? C6 C5 C4 121.2(2) . . ? C5 C6 C1 120.61(19) . . ? C5 C6 C9 118.1(2) . . ? C1 C6 C9 121.31(18) . . ? C11 C10 C15 118.41(19) . . ? C11 C10 Ga1 125.39(16) . . ? C15 C10 Ga1 116.16(15) . . ? C10 C11 C12 119.4(2) . . ? C10 C11 C16 122.52(19) . . ? C12 C11 C16 118.06(19) . . ? C13 C12 C11 122.2(2) . . ? C12 C13 C14 118.4(2) . . ? C12 C13 C17 121.4(2) . . ? C14 C13 C17 120.2(2) . . ? C15 C14 C13 120.8(2) . . ? C14 C15 C10 120.7(2) . . ? C14 C15 C18 118.4(2) . . ? C10 C15 C18 120.93(18) . . ? C24 C19 C20 118.59(19) . . ? C24 C19 Ga2 117.51(15) . . ? C20 C19 Ga2 123.89(17) . . ? C21 C20 C19 119.2(2) . . ? C21 C20 C25 118.6(2) . . ? C19 C20 C25 122.15(19) . . ? C22 C21 C20 122.6(2) . . ? C21 C22 C23 118.2(2) . . ? C21 C22 C26 120.7(2) . . ? C23 C22 C26 121.1(2) . . ? C22 C23 C24 120.9(2) . . ? C19 C24 C23 120.5(2) . . ? C19 C24 C27 121.55(19) . . ? C23 C24 C27 118.0(2) . . ? C29 C28 C33 118.18(18) . . ? C29 C28 Ga2 117.71(14) . . ? C33 C28 Ga2 124.09(16) . . ? C30 C29 C28 120.58(19) . . ? C30 C29 C34 117.7(2) . . ? C28 C29 C34 121.70(19) . . ? C31 C30 C29 121.5(2) . . ? C32 C31 C30 117.87(19) . . ? C32 C31 C35 121.48(19) . . ? C30 C31 C35 120.6(2) . . ? C31 C32 C33 122.59(19) . . ? C32 C33 C28 119.26(19) . . ? C32 C33 C36 117.03(18) . . ? C28 C33 C36 123.67(19) . . ? 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 C28 Ga2 N1 N2 -59.7(2) . . . . ? C19 Ga2 N1 N2 87.72(19) . . . . ? N4 Ga2 N1 N2 -173.2(2) . . . . ? C28 Ga2 N1 Ga1 123.60(8) . . . . ? C19 Ga2 N1 Ga1 -89.02(9) . . . . ? N4 Ga2 N1 Ga1 10.06(7) . . . . ? C1 Ga1 N1 N2 69.7(2) . . . . ? C10 Ga1 N1 N2 -77.8(2) . . . . ? N4 Ga1 N1 N2 173.3(2) . . . . ? C1 Ga1 N1 Ga2 -113.70(8) . . . . ? C10 Ga1 N1 Ga2 98.80(9) . . . . ? N4 Ga1 N1 Ga2 -10.06(7) . . . . ? Ga2 N1 N2 N3 -20(33) . . . . ? Ga1 N1 N2 N3 156(100) . . . . ? C28 Ga2 N4 N5 57.8(2) . . . . ? C19 Ga2 N4 N5 -89.0(2) . . . . ? N1 Ga2 N4 N5 162.4(2) . . . . ? C28 Ga2 N4 Ga1 -114.62(8) . . . . ? C19 Ga2 N4 Ga1 98.59(9) . . . . ? N1 Ga2 N4 Ga1 -10.02(7) . . . . ? C1 Ga1 N4 N5 -49.8(2) . . . . ? C10 Ga1 N4 N5 96.95(19) . . . . ? N1 Ga1 N4 N5 -162.6(2) . . . . ? C1 Ga1 N4 Ga2 122.80(8) . . . . ? C10 Ga1 N4 Ga2 -90.44(9) . . . . ? N1 Ga1 N4 Ga2 10.01(7) . . . . ? Ga2 N4 N5 N6 120(39) . . . . ? Ga1 N4 N5 N6 -70(39) . . . . ? C10 Ga1 C1 C6 -51.90(19) . . . . ? N1 Ga1 C1 C6 170.28(14) . . . . ? N4 Ga1 C1 C6 86.85(16) . . . . ? C10 Ga1 C1 C2 130.53(17) . . . . ? N1 Ga1 C1 C2 -7.3(2) . . . . ? N4 Ga1 C1 C2 -90.72(18) . . . . ? C6 C1 C2 C3 -1.2(3) . . . . ? Ga1 C1 C2 C3 176.29(16) . . . . ? C6 C1 C2 C7 176.8(2) . . . . ? Ga1 C1 C2 C7 -5.7(3) . . . . ? C1 C2 C3 C4 1.0(3) . . . . ? C7 C2 C3 C4 -177.1(2) . . . . ? C2 C3 C4 C5 1.1(3) . . . . ? C2 C3 C4 C8 -178.5(2) . . . . ? C3 C4 C5 C6 -3.0(3) . . . . ? C8 C4 C5 C6 176.6(2) . . . . ? C4 C5 C6 C1 2.8(3) . . . . ? C4 C5 C6 C9 -175.3(2) . . . . ? C2 C1 C6 C5 -0.6(3) . . . . ? Ga1 C1 C6 C5 -178.36(16) . . . . ? C2 C1 C6 C9 177.4(2) . . . . ? Ga1 C1 C6 C9 -0.3(3) . . . . ? C1 Ga1 C10 C11 118.08(18) . . . . ? N1 Ga1 C10 C11 -100.68(18) . . . . ? N4 Ga1 C10 C11 -19.6(2) . . . . ? C1 Ga1 C10 C15 -64.0(2) . . . . ? N1 Ga1 C10 C15 77.23(17) . . . . ? N4 Ga1 C10 C15 158.30(15) . . . . ? C15 C10 C11 C12 -2.6(3) . . . . ? Ga1 C10 C11 C12 175.25(16) . . . . ? C15 C10 C11 C16 177.3(2) . . . . ? Ga1 C10 C11 C16 -4.8(3) . . . . ? C10 C11 C12 C13 1.4(3) . . . . ? C16 C11 C12 C13 -178.5(2) . . . . ? C11 C12 C13 C14 1.2(3) . . . . ? C11 C12 C13 C17 -179.0(2) . . . . ? C12 C13 C14 C15 -2.6(3) . . . . ? C17 C13 C14 C15 177.6(2) . . . . ? C13 C14 C15 C10 1.3(3) . . . . ? C13 C14 C15 C18 -178.7(2) . . . . ? C11 C10 C15 C14 1.3(3) . . . . ? Ga1 C10 C15 C14 -176.75(17) . . . . ? C11 C10 C15 C18 -178.7(2) . . . . ? Ga1 C10 C15 C18 3.2(3) . . . . ? C28 Ga2 C19 C24 -72.5(2) . . . . ? N1 Ga2 C19 C24 148.75(16) . . . . ? N4 Ga2 C19 C24 68.17(18) . . . . ? C28 Ga2 C19 C20 108.98(19) . . . . ? N1 Ga2 C19 C20 -29.8(2) . . . . ? N4 Ga2 C19 C20 -110.38(18) . . . . ? C24 C19 C20 C21 -1.7(3) . . . . ? Ga2 C19 C20 C21 176.80(16) . . . . ? C24 C19 C20 C25 178.1(2) . . . . ? Ga2 C19 C20 C25 -3.3(3) . . . . ? C19 C20 C21 C22 -0.4(3) . . . . ? C25 C20 C21 C22 179.7(2) . . . . ? C20 C21 C22 C23 2.1(4) . . . . ? C20 C21 C22 C26 -179.6(2) . . . . ? C21 C22 C23 C24 -1.7(3) . . . . ? C26 C22 C23 C24 179.9(2) . . . . ? C20 C19 C24 C23 2.1(3) . . . . ? Ga2 C19 C24 C23 -176.55(17) . . . . ? C20 C19 C24 C27 -177.2(2) . . . . ? Ga2 C19 C24 C27 4.2(3) . . . . ? C22 C23 C24 C19 -0.4(3) . . . . ? C22 C23 C24 C27 178.9(2) . . . . ? C19 Ga2 C28 C29 -27.9(2) . . . . ? N1 Ga2 C28 C29 111.56(16) . . . . ? N4 Ga2 C28 C29 -164.31(15) . . . . ? C19 Ga2 C28 C33 153.80(16) . . . . ? N1 Ga2 C28 C33 -66.79(19) . . . . ? N4 Ga2 C28 C33 17.3(2) . . . . ? C33 C28 C29 C30 -1.3(3) . . . . ? Ga2 C28 C29 C30 -179.74(17) . . . . ? C33 C28 C29 C34 177.5(2) . . . . ? Ga2 C28 C29 C34 -0.9(3) . . . . ? C28 C29 C30 C31 2.1(3) . . . . ? C34 C29 C30 C31 -176.7(2) . . . . ? C29 C30 C31 C32 -0.8(3) . . . . ? C29 C30 C31 C35 178.4(2) . . . . ? C30 C31 C32 C33 -1.4(3) . . . . ? C35 C31 C32 C33 179.4(2) . . . . ? C31 C32 C33 C28 2.2(3) . . . . ? C31 C32 C33 C36 -175.5(2) . . . . ? C29 C28 C33 C32 -0.8(3) . . . . ? Ga2 C28 C33 C32 177.54(15) . . . . ? C29 C28 C33 C36 176.8(2) . . . . ? Ga2 C28 C33 C36 -4.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.748 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.748 _refine_diff_density_max 0.316 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.054 #==============================================================================