# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/224 data_global _publ-contact_author_name ; A. C. Jones ; _publ_contact_author_name ; Chemistry Department, The University of Liverpool Liverpool L69 7ZD, U.K. ; _publ_section_journal ' Journal of Materials Chemistry ' _publ_section_title ; New Synthesis Routes to Ultra-High Purity Trialkylgallium MOVPE Precursors. Crystal Structures of Triethylgallium and Triisopropylgallium Adducts with Macrocyclic Tertiary Amines. ; data_compound3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H92 Ga4 N4' _chemical_formula_sum 'C38 H92 Ga4 N4' _chemical_formula_weight 884.04 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8976(9) _cell_length_b 11.6366(11) _cell_length_c 11.7629(8) _cell_angle_alpha 83.338(7) _cell_angle_beta 88.446(7) _cell_angle_gamma 82.189(8) _cell_volume 1198.38(18) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.720 _cell_measurement_theta_max 13.979 _exptl_crystal_description 'irregular block' _exptl_crystal_colour white _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 2.251 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.7555 _exptl_absorpt_correction_T_max 0.8841 _exptl_absorpt_process_details ; 12 reflections having 2\q between 7.56 and 35.8 degrees giving 216 \y scans for parameter estimation ; _exptl_special_details ; The crystal was mounted on a glass pin using Fomblin YR-1800 oil (Lancaster Synthesis). ; _diffrn_ambient_temperature 223(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 'Siemens P4' _diffrn_measurement_method 'profile fitting of \q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6506 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5460 _reflns_number_gt 4208 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS v2.20 (Siemens, 1996)' _computing_cell_refinement 'XSCANS v2.20 (Siemens, 1996)' _computing_data_reduction 'XSCANS v2.20 (Siemens, 1996)' _computing_structure_solution 'SHELXTL-PLUS v5.03 (Siemens, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS v5.03 (Siemens, 1995)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.5202P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5460 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.85384(3) 0.82684(2) 0.28388(2) 0.04015(9) Uani 1 1 d . . . C11 C 0.8329(4) 0.6572(3) 0.3026(3) 0.0683(9) Uani 1 1 d . . . H11A H 0.7654 0.6408 0.3680 0.082 Uiso 1 1 calc R . . H11B H 0.7854 0.6383 0.2341 0.082 Uiso 1 1 calc R . . C111 C 0.9805(5) 0.5804(4) 0.3210(5) 0.1102(17) Uani 1 1 d . . . H11C H 0.9656 0.4998 0.3179 0.165 Uiso 1 1 calc R . . H11D H 1.0198 0.5886 0.3953 0.165 Uiso 1 1 calc R . . H11E H 1.0523 0.6028 0.2617 0.165 Uiso 1 1 calc R . . C12 C 0.9016(4) 0.8948(3) 0.4246(2) 0.0572(8) Uani 1 1 d . . . H12A H 1.0108 0.8994 0.4236 0.069 Uiso 1 1 calc R . . H12B H 0.8496 0.9751 0.4193 0.069 Uiso 1 1 calc R . . C121 C 0.8610(4) 0.8326(4) 0.5408(3) 0.0783(11) Uani 1 1 d . . . H12C H 0.7516 0.8382 0.5490 0.117 Uiso 1 1 calc R . . H12D H 0.9014 0.8690 0.6013 0.117 Uiso 1 1 calc R . . H12E H 0.9044 0.7511 0.5457 0.117 Uiso 1 1 calc R . . C13 C 0.9675(4) 0.8864(3) 0.1456(3) 0.0635(9) Uani 1 1 d . . . H13A H 0.9856 0.8246 0.0950 0.076 Uiso 1 1 calc R . . H13B H 0.9027 0.9521 0.1045 0.076 Uiso 1 1 calc R . . C131 C 1.1096(5) 0.9240(6) 0.1660(4) 0.139(3) Uani 1 1 d . . . H13C H 1.0929 0.9901 0.2102 0.208 Uiso 1 1 calc R . . H13D H 1.1576 0.9469 0.0934 0.208 Uiso 1 1 calc R . . H13E H 1.1747 0.8606 0.2082 0.208 Uiso 1 1 calc R . . Ga2 Ga 0.61117(3) 1.32335(2) 0.22027(2) 0.03366(8) Uani 1 1 d . . . C21 C 0.5918(4) 1.2680(2) 0.3864(2) 0.0470(7) Uani 1 1 d . . . H21A H 0.4875 1.2902 0.4125 0.056 Uiso 1 1 calc R . . H21B H 0.6138 1.1826 0.3980 0.056 Uiso 1 1 calc R . . C211 C 0.7002(4) 1.3204(3) 0.4563(3) 0.0742(10) Uani 1 1 d . . . H21C H 0.6887 1.2928 0.5366 0.111 Uiso 1 1 calc R . . H21D H 0.6778 1.4048 0.4453 0.111 Uiso 1 1 calc R . . H21E H 0.8036 1.2971 0.4315 0.111 Uiso 1 1 calc R . . C22 C 0.8129(3) 1.2822(2) 0.1457(2) 0.0463(6) Uani 1 1 d . . . H22A H 0.8906 1.2679 0.2049 0.056 Uiso 1 1 calc R . . H22B H 0.8118 1.2091 0.1121 0.056 Uiso 1 1 calc R . . C221 C 0.8585(4) 1.3732(3) 0.0532(3) 0.0782(11) Uani 1 1 d . . . H22C H 0.7875 1.3833 -0.0095 0.117 Uiso 1 1 calc R . . H22D H 0.9597 1.3478 0.0253 0.117 Uiso 1 1 calc R . . H22E H 0.8575 1.4468 0.0845 0.117 Uiso 1 1 calc R . . C23 C 0.5160(3) 1.4872(2) 0.1753(2) 0.0428(6) Uani 1 1 d . . . H23A H 0.5970 1.5364 0.1599 0.051 Uiso 1 1 calc R . . H23B H 0.4614 1.4894 0.1036 0.051 Uiso 1 1 calc R . . C231 C 0.4062(4) 1.5405(3) 0.2628(3) 0.0645(9) Uani 1 1 d . . . H23C H 0.3624 1.6183 0.2317 0.097 Uiso 1 1 calc R . . H23D H 0.4604 1.5449 0.3323 0.097 Uiso 1 1 calc R . . H23E H 0.3261 1.4921 0.2801 0.097 Uiso 1 1 calc R . . N1 N 0.6173(2) 0.90502(16) 0.24962(15) 0.0322(4) Uani 1 1 d . . . C14 C 0.5394(3) 0.8924(2) 0.36289(19) 0.0404(6) Uani 1 1 d . . . H14A H 0.5573 0.8115 0.3961 0.061 Uiso 1 1 calc R . . H14B H 0.4313 0.9161 0.3533 0.061 Uiso 1 1 calc R . . H14C H 0.5789 0.9413 0.4132 0.061 Uiso 1 1 calc R . . C1 C 0.6147(3) 1.03139(18) 0.20667(19) 0.0328(5) Uani 1 1 d . . . H1A H 0.6579 1.0374 0.1290 0.039 Uiso 1 1 calc R . . H1B H 0.6802 1.0658 0.2552 0.039 Uiso 1 1 calc R . . C2 C 0.4580(3) 1.10238(19) 0.20434(19) 0.0347(5) Uani 1 1 d . . . H2A H 0.3880 1.0608 0.1671 0.042 Uiso 1 1 calc R . . H2B H 0.4221 1.1080 0.2833 0.042 Uiso 1 1 calc R . . N2 N 0.4532(2) 1.22266(15) 0.14343(16) 0.0321(4) Uani 1 1 d . . . C24 C 0.2972(3) 1.2836(2) 0.1589(2) 0.0427(6) Uani 1 1 d . . . H24A H 0.2861 1.3590 0.1130 0.064 Uiso 1 1 calc R . . H24B H 0.2798 1.2945 0.2389 0.064 Uiso 1 1 calc R . . H24C H 0.2240 1.2370 0.1348 0.064 Uiso 1 1 calc R . . C3 C 0.4916(3) 1.2235(2) 0.01934(18) 0.0340(5) Uani 1 1 d . . . H3A H 0.5971 1.1876 0.0122 0.041 Uiso 1 1 calc R . . H3B H 0.4859 1.3050 -0.0145 0.041 Uiso 1 1 calc R . . C4 C 0.3926(3) 1.1612(2) -0.0514(2) 0.0403(6) Uani 1 1 d . . . H4A H 0.3898 1.0810 -0.0161 0.048 Uiso 1 1 calc R . . H4B H 0.2886 1.2020 -0.0544 0.048 Uiso 1 1 calc R . . C5 C 0.4594(3) 1.16045(19) -0.17150(19) 0.0344(5) Uani 1 1 d . . . H5A H 0.4561 1.2414 -0.2063 0.041 Uiso 1 1 calc R . . H5B H 0.5663 1.1266 -0.1658 0.041 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 0.04199(17) 0.04249(16) 0.03835(16) -0.00386(12) -0.00311(12) -0.01419(13) C11 0.0556(19) 0.0469(17) 0.102(3) -0.0054(17) -0.0156(19) -0.0060(15) C111 0.083(3) 0.063(2) 0.179(5) 0.005(3) -0.024(3) 0.001(2) C12 0.0572(18) 0.081(2) 0.0385(15) -0.0062(14) -0.0100(13) -0.0265(16) C121 0.070(2) 0.130(3) 0.0381(16) -0.0010(18) -0.0106(16) -0.028(2) C13 0.059(2) 0.086(2) 0.0501(17) -0.0119(16) 0.0137(15) -0.0263(18) C131 0.076(3) 0.282(8) 0.070(3) 0.024(4) -0.003(2) -0.102(4) Ga2 0.04342(17) 0.03060(13) 0.02857(13) -0.00426(10) -0.00111(11) -0.00978(11) C21 0.0663(19) 0.0468(15) 0.0309(12) -0.0050(11) -0.0040(12) -0.0176(13) C211 0.084(3) 0.102(3) 0.0433(17) -0.0111(17) -0.0138(17) -0.030(2) C22 0.0434(15) 0.0497(15) 0.0464(15) -0.0058(12) -0.0019(12) -0.0081(12) C221 0.067(2) 0.071(2) 0.093(3) 0.003(2) 0.030(2) -0.0128(18) C23 0.0497(16) 0.0321(12) 0.0475(15) -0.0034(11) -0.0016(12) -0.0097(11) C231 0.067(2) 0.0419(16) 0.084(2) -0.0148(15) 0.0167(18) -0.0025(15) N1 0.0439(12) 0.0301(9) 0.0244(9) 0.0005(7) -0.0023(8) -0.0146(8) C14 0.0502(15) 0.0447(14) 0.0270(11) 0.0003(10) 0.0008(11) -0.0125(12) C1 0.0429(13) 0.0279(11) 0.0296(11) -0.0025(9) -0.0014(10) -0.0123(10) C2 0.0450(14) 0.0315(11) 0.0296(11) -0.0013(9) 0.0007(10) -0.0138(10) N2 0.0392(11) 0.0279(9) 0.0301(10) -0.0037(7) -0.0032(8) -0.0069(8) C24 0.0424(15) 0.0391(13) 0.0470(15) -0.0059(11) -0.0034(12) -0.0049(11) C3 0.0451(14) 0.0309(11) 0.0272(11) -0.0012(9) -0.0048(10) -0.0110(10) C4 0.0498(15) 0.0432(13) 0.0318(12) -0.0057(10) -0.0038(11) -0.0190(12) C5 0.0441(14) 0.0287(11) 0.0321(12) -0.0001(9) -0.0041(10) -0.0134(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 C11 1.995(3) . ? Ga1 C12 1.995(3) . ? Ga1 C13 1.997(3) . ? Ga1 N1 2.205(2) . ? C11 C111 1.491(5) . ? C12 C121 1.529(4) . ? C13 C131 1.427(5) . ? Ga2 C21 1.996(2) . ? Ga2 C23 1.996(2) . ? Ga2 C22 2.000(3) . ? Ga2 N2 2.2197(19) . ? C21 C211 1.516(4) . ? C22 C221 1.515(4) . ? C23 C231 1.525(4) . ? N1 C14 1.486(3) . ? N1 C5 1.493(3) 2_675 ? N1 C1 1.496(3) . ? C1 C2 1.520(3) . ? C2 N2 1.492(3) . ? N2 C24 1.487(3) . ? N2 C3 1.489(3) . ? C3 C4 1.532(3) . ? C4 C5 1.518(3) . ? C5 N1 1.493(3) 2_675 ? 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 C11 Ga1 C12 116.50(15) . . ? C11 Ga1 C13 116.87(16) . . ? C12 Ga1 C13 112.95(13) . . ? C11 Ga1 N1 101.09(11) . . ? C12 Ga1 N1 102.83(11) . . ? C13 Ga1 N1 103.65(12) . . ? C111 C11 Ga1 113.2(3) . . ? C121 C12 Ga1 118.2(2) . . ? C131 C13 Ga1 116.2(3) . . ? C21 Ga2 C23 114.59(11) . . ? C21 Ga2 C22 116.90(12) . . ? C23 Ga2 C22 113.93(11) . . ? C21 Ga2 N2 101.55(9) . . ? C23 Ga2 N2 101.48(9) . . ? C22 Ga2 N2 105.73(10) . . ? C211 C21 Ga2 110.8(2) . . ? C221 C22 Ga2 115.4(2) . . ? C231 C23 Ga2 115.69(19) . . ? C14 N1 C5 107.42(18) . 2_675 ? C14 N1 C1 110.18(18) . . ? C5 N1 C1 113.13(17) 2_675 . ? C14 N1 Ga1 104.54(14) . . ? C5 N1 Ga1 112.23(14) 2_675 . ? C1 N1 Ga1 108.98(14) . . ? N1 C1 C2 114.56(19) . . ? N2 C2 C1 113.91(19) . . ? C24 N2 C3 110.18(19) . . ? C24 N2 C2 107.06(19) . . ? C3 N2 C2 112.95(17) . . ? C24 N2 Ga2 107.08(14) . . ? C3 N2 Ga2 107.91(14) . . ? C2 N2 Ga2 111.50(14) . . ? N2 C3 C4 116.61(19) . . ? C5 C4 C3 108.6(2) . . ? N1 C5 C4 115.50(19) 2_675 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.364 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.058 data_compound4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H116 Ga4 N4' _chemical_formula_weight 1052.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 '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' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.1630 1.6090 '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 8.7237(13) _cell_length_b 12.880(2) _cell_length_c 13.649(2) _cell_angle_alpha 101.558(18) _cell_angle_beta 92.290(18) _cell_angle_gamma 105.696(18) _cell_volume 1439.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 1.813 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9194 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.25 _reflns_number_total 4271 _reflns_number_gt 2870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4271 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.877 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.34051(5) 0.17958(4) -0.23534(4) 0.02642(15) Uani 1 d . . . Ga2 Ga 0.86359(5) 0.32250(4) 0.27234(4) 0.02600(15) Uani 1 d . . . N1 N 0.4961(4) 0.0677(3) -0.2101(3) 0.0241(8) Uani 1 d . . . N2 N 0.6443(4) 0.2287(3) 0.1636(3) 0.0229(8) Uani 1 d . . . C1 C 0.3856(4) -0.0396(3) -0.2009(3) 0.0239(9) Uani 1 d . . . H1A H 0.3040 -0.0646 -0.2576 0.029 Uiso 1 calc R . . H1B H 0.3323 -0.0269 -0.1405 0.029 Uiso 1 calc R . . C2 C 0.5820(5) 0.0514(4) -0.3012(3) 0.0323(11) Uani 1 d . . . H2A H 0.6536 0.1208 -0.3064 0.048 Uiso 1 calc R . . H2B H 0.5059 0.0230 -0.3598 0.048 Uiso 1 calc R . . H2C H 0.6419 -0.0002 -0.2964 0.048 Uiso 1 calc R . . C3 C 0.6202(4) 0.1193(4) -0.1228(3) 0.0263(10) Uani 1 d . . . H3A H 0.6902 0.1867 -0.1357 0.032 Uiso 1 calc R . . H3B H 0.6845 0.0694 -0.1181 0.032 Uiso 1 calc R . . C4 C 0.5553(5) 0.1468(4) -0.0228(3) 0.0293(10) Uani 1 d . . . H4A H 0.4852 0.0801 -0.0086 0.035 Uiso 1 calc R . . H4B H 0.4931 0.1984 -0.0257 0.035 Uiso 1 calc R . . C5 C 0.6923(4) 0.1976(3) 0.0607(3) 0.0241(10) Uani 1 d . . . H5A H 0.7541 0.1454 0.0615 0.029 Uiso 1 calc R . . H5B H 0.7620 0.2632 0.0445 0.029 Uiso 1 calc R . . C6 C 0.5377(4) 0.1333(3) 0.1968(3) 0.0253(10) Uani 1 d . . . H6A H 0.4405 0.1039 0.1511 0.030 Uiso 1 calc R . . H6B H 0.5079 0.1593 0.2630 0.030 Uiso 1 calc R . . C7 C 0.5554(5) 0.3124(3) 0.1655(4) 0.0288(10) Uani 1 d . . . H7A H 0.5238 0.3320 0.2316 0.043 Uiso 1 calc R . . H7B H 0.4620 0.2822 0.1179 0.043 Uiso 1 calc R . . H7C H 0.6230 0.3770 0.1481 0.043 Uiso 1 calc R . . C11 C 0.2245(5) 0.1005(4) -0.3721(4) 0.0367(11) Uani 1 d . . . H11 H 0.1895 0.0215 -0.3720 0.044 Uiso 1 calc R . . C12 C 0.3168(7) 0.1123(6) -0.4641(4) 0.0631(17) Uani 1 d . . . H12A H 0.4119 0.0894 -0.4568 0.095 Uiso 1 calc R . . H12B H 0.3457 0.1881 -0.4698 0.095 Uiso 1 calc R . . H12C H 0.2507 0.0667 -0.5234 0.095 Uiso 1 calc R . . C13 C 0.0729(6) 0.1366(5) -0.3870(4) 0.0586(16) Uani 1 d . . . H13A H 0.0118 0.1288 -0.3306 0.088 Uiso 1 calc R . . H13B H 0.0096 0.0912 -0.4474 0.088 Uiso 1 calc R . . H13C H 0.1025 0.2125 -0.3924 0.088 Uiso 1 calc R . . C14 C 0.1926(5) 0.1813(4) -0.1242(4) 0.0321(11) Uani 1 d . . . H14 H 0.2594 0.2010 -0.0601 0.038 Uiso 1 calc R . . C15 C 0.0639(6) 0.0739(4) -0.1259(5) 0.0532(15) Uani 1 d . . . H15A H 0.1133 0.0162 -0.1231 0.080 Uiso 1 calc R . . H15B H -0.0067 0.0540 -0.1866 0.080 Uiso 1 calc R . . H15C H 0.0040 0.0837 -0.0690 0.080 Uiso 1 calc R . . C16 C 0.1140(6) 0.2728(4) -0.1263(4) 0.0478(14) Uani 1 d . . . H16A H 0.1949 0.3408 -0.1246 0.072 Uiso 1 calc R . . H16B H 0.0548 0.2815 -0.0689 0.072 Uiso 1 calc R . . H16C H 0.0427 0.2539 -0.1866 0.072 Uiso 1 calc R . . C17 C 0.5111(5) 0.3227(4) -0.2249(4) 0.0415(13) Uani 1 d . . . H17 H 0.6062 0.3052 -0.2511 0.050 Uiso 1 calc R . . C18 C 0.5609(7) 0.3945(5) -0.1191(5) 0.0638(17) Uani 1 d . . . H18A H 0.5959 0.3529 -0.0762 0.096 Uiso 1 calc R . . H18B H 0.4715 0.4171 -0.0933 0.096 Uiso 1 calc R . . H18C H 0.6469 0.4587 -0.1212 0.096 Uiso 1 calc R . . C19 C 0.4563(7) 0.3925(5) -0.2912(5) 0.0572(16) Uani 1 d . . . H19A H 0.4242 0.3491 -0.3584 0.086 Uiso 1 calc R . . H19B H 0.5431 0.4566 -0.2921 0.086 Uiso 1 calc R . . H19C H 0.3675 0.4152 -0.2644 0.086 Uiso 1 calc R . . C21 C 0.9287(5) 0.4683(4) 0.2311(3) 0.0315(11) Uani 1 d . . . H21 H 0.8367 0.4984 0.2366 0.038 Uiso 1 calc R . . C22 C 0.9816(7) 0.4721(4) 0.1266(4) 0.0518(14) Uani 1 d . . . H22A H 0.8979 0.4243 0.0769 0.078 Uiso 1 calc R . . H22B H 1.0763 0.4479 0.1198 0.078 Uiso 1 calc R . . H22C H 1.0040 0.5464 0.1171 0.078 Uiso 1 calc R . . C23 C 1.0608(7) 0.5455(5) 0.3088(5) 0.0649(18) Uani 1 d . . . H23A H 1.0279 0.5440 0.3749 0.097 Uiso 1 calc R . . H23B H 1.0820 0.6194 0.2983 0.097 Uiso 1 calc R . . H23C H 1.1561 0.5220 0.3024 0.097 Uiso 1 calc R . . C24 C 0.7894(5) 0.3381(4) 0.4103(3) 0.0357(11) Uani 1 d . . . H24 H 0.8866 0.3839 0.4531 0.043 Uiso 1 calc R . . C25 C 0.6706(7) 0.4056(5) 0.4348(4) 0.0621(16) Uani 1 d . . . H25A H 0.7002 0.4701 0.4068 0.093 Uiso 1 calc R . . H25B H 0.6720 0.4277 0.5064 0.093 Uiso 1 calc R . . H25C H 0.5649 0.3613 0.4066 0.093 Uiso 1 calc R . . C26 C 0.7431(6) 0.2351(4) 0.4546(4) 0.0526(14) Uani 1 d . . . H26A H 0.8186 0.1934 0.4395 0.079 Uiso 1 calc R . . H26B H 0.6380 0.1902 0.4259 0.079 Uiso 1 calc R . . H26C H 0.7437 0.2569 0.5261 0.079 Uiso 1 calc R . . C27 C 1.0169(5) 0.2305(4) 0.2554(4) 0.0369(12) Uani 1 d . . . H27 H 0.9558 0.1544 0.2551 0.044 Uiso 1 calc R . . C28 C 1.1044(5) 0.2272(5) 0.1605(4) 0.0458(13) Uani 1 d . . . H28A H 1.0276 0.2030 0.1023 0.069 Uiso 1 calc R . . H28B H 1.1681 0.1767 0.1584 0.069 Uiso 1 calc R . . H28C H 1.1724 0.2997 0.1611 0.069 Uiso 1 calc R . . C29 C 1.1437(6) 0.2694(6) 0.3469(5) 0.0683(19) Uani 1 d . . . H29A H 1.0914 0.2712 0.4076 0.102 Uiso 1 calc R . . H29B H 1.2106 0.3421 0.3470 0.102 Uiso 1 calc R . . H29C H 1.2081 0.2192 0.3433 0.102 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 0.0206(3) 0.0367(3) 0.0227(3) 0.0074(2) 0.00393(19) 0.0085(2) Ga2 0.0190(2) 0.0378(3) 0.0186(3) 0.0030(2) -0.00017(19) 0.0063(2) N1 0.0187(16) 0.037(2) 0.014(2) 0.0017(16) 0.0031(13) 0.0059(14) N2 0.0201(17) 0.0303(19) 0.018(2) 0.0012(15) 0.0008(14) 0.0099(14) C1 0.019(2) 0.031(2) 0.021(3) 0.0046(19) 0.0006(17) 0.0062(17) C2 0.026(2) 0.046(3) 0.025(3) 0.004(2) 0.0086(18) 0.013(2) C3 0.018(2) 0.035(2) 0.022(3) 0.0032(19) -0.0020(17) 0.0036(17) C4 0.019(2) 0.046(3) 0.019(3) 0.002(2) -0.0023(17) 0.0066(18) C5 0.018(2) 0.034(2) 0.018(3) 0.0045(19) -0.0003(16) 0.0057(17) C6 0.0170(19) 0.035(2) 0.023(3) 0.0030(19) 0.0024(16) 0.0089(17) C7 0.025(2) 0.034(2) 0.028(3) 0.002(2) 0.0007(18) 0.0115(18) C11 0.034(2) 0.050(3) 0.030(3) 0.012(2) 0.002(2) 0.016(2) C12 0.060(4) 0.113(5) 0.028(4) 0.020(3) 0.009(3) 0.040(3) C13 0.043(3) 0.098(5) 0.038(4) 0.007(3) -0.011(2) 0.034(3) C14 0.023(2) 0.042(3) 0.033(3) 0.009(2) 0.0050(18) 0.0115(19) C15 0.036(3) 0.060(3) 0.073(5) 0.018(3) 0.032(3) 0.022(3) C16 0.046(3) 0.058(3) 0.048(4) 0.013(3) 0.019(2) 0.025(3) C17 0.030(2) 0.049(3) 0.051(4) 0.014(3) 0.015(2) 0.018(2) C18 0.059(4) 0.046(3) 0.072(5) 0.007(3) -0.007(3) -0.003(3) C19 0.058(3) 0.049(3) 0.077(5) 0.031(3) 0.022(3) 0.021(3) C21 0.024(2) 0.043(3) 0.022(3) -0.002(2) -0.0002(18) 0.0081(19) C22 0.068(4) 0.045(3) 0.042(4) 0.012(3) 0.020(3) 0.012(3) C23 0.068(4) 0.059(4) 0.045(4) 0.011(3) -0.013(3) -0.016(3) C24 0.035(2) 0.048(3) 0.016(3) 0.002(2) -0.0018(19) 0.004(2) C25 0.070(4) 0.092(5) 0.027(4) -0.002(3) 0.015(3) 0.037(3) C26 0.056(3) 0.059(4) 0.029(4) 0.007(3) 0.005(2) -0.004(3) C27 0.024(2) 0.043(3) 0.041(4) 0.010(2) 0.001(2) 0.004(2) C28 0.031(3) 0.065(4) 0.046(4) 0.013(3) 0.008(2) 0.020(2) C29 0.043(3) 0.121(6) 0.051(4) 0.026(4) -0.005(3) 0.036(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 C17 2.007(5) . ? Ga1 C11 2.018(5) . ? Ga1 C14 2.031(4) . ? Ga1 N1 2.293(3) . ? Ga2 C24 2.005(5) . ? Ga2 C27 2.005(4) . ? Ga2 C21 2.010(5) . ? Ga2 N2 2.264(3) . ? N1 C2 1.486(5) . ? N1 C1 1.488(5) . ? N1 C3 1.491(5) . ? N2 C7 1.485(5) . ? N2 C5 1.490(5) . ? N2 C6 1.490(5) . ? C1 C6 1.539(5) 2_655 ? C3 C4 1.512(6) . ? C4 C5 1.525(5) . ? C6 C1 1.539(5) 2_655 ? C11 C12 1.530(7) . ? C11 C13 1.535(6) . ? C14 C16 1.519(6) . ? C14 C15 1.524(6) . ? C17 C18 1.525(8) . ? C17 C19 1.543(7) . ? C21 C23 1.517(7) . ? C21 C22 1.523(7) . ? C24 C26 1.530(7) . ? C24 C25 1.531(7) . ? C27 C28 1.529(7) . ? C27 C29 1.541(7) . ? 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 C17 Ga1 C11 118.0(2) . . ? C17 Ga1 C14 114.21(19) . . ? C11 Ga1 C14 113.20(18) . . ? C17 Ga1 N1 100.01(15) . . ? C11 Ga1 N1 101.50(16) . . ? C14 Ga1 N1 107.50(15) . . ? C24 Ga2 C27 111.4(2) . . ? C24 Ga2 C21 111.79(19) . . ? C27 Ga2 C21 117.25(18) . . ? C24 Ga2 N2 106.46(15) . . ? C27 Ga2 N2 106.72(16) . . ? C21 Ga2 N2 102.05(15) . . ? C2 N1 C1 109.9(3) . . ? C2 N1 C3 107.1(3) . . ? C1 N1 C3 113.4(3) . . ? C2 N1 Ga1 106.6(2) . . ? C1 N1 Ga1 107.0(2) . . ? C3 N1 Ga1 112.7(2) . . ? C7 N2 C5 109.4(3) . . ? C7 N2 C6 107.2(3) . . ? C5 N2 C6 112.9(3) . . ? C7 N2 Ga2 102.5(2) . . ? C5 N2 Ga2 110.1(2) . . ? C6 N2 Ga2 114.1(2) . . ? N1 C1 C6 116.2(3) . 2_655 ? N1 C3 C4 114.9(3) . . ? C3 C4 C5 110.2(3) . . ? N2 C5 C4 115.7(3) . . ? N2 C6 C1 113.6(3) . 2_655 ? C12 C11 C13 107.9(4) . . ? C12 C11 Ga1 118.0(3) . . ? C13 C11 Ga1 109.5(3) . . ? C16 C14 C15 109.3(4) . . ? C16 C14 Ga1 108.2(3) . . ? C15 C14 Ga1 116.8(3) . . ? C18 C17 C19 107.8(4) . . ? C18 C17 Ga1 115.5(4) . . ? C19 C17 Ga1 110.0(3) . . ? C23 C21 C22 109.0(4) . . ? C23 C21 Ga2 107.2(3) . . ? C22 C21 Ga2 119.3(3) . . ? C26 C24 C25 109.8(4) . . ? C26 C24 Ga2 118.1(3) . . ? C25 C24 Ga2 117.8(3) . . ? C28 C27 C29 108.0(4) . . ? C28 C27 Ga2 117.1(3) . . ? C29 C27 Ga2 109.5(4) . . ? 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 C17 Ga1 N1 C2 -70.4(3) . . . . ? C11 Ga1 N1 C2 51.1(3) . . . . ? C14 Ga1 N1 C2 170.1(3) . . . . ? C17 Ga1 N1 C1 172.1(3) . . . . ? C11 Ga1 N1 C1 -66.5(3) . . . . ? C14 Ga1 N1 C1 52.6(3) . . . . ? C17 Ga1 N1 C3 46.7(3) . . . . ? C11 Ga1 N1 C3 168.2(3) . . . . ? C14 Ga1 N1 C3 -72.8(3) . . . . ? C24 Ga2 N2 C7 72.7(3) . . . . ? C27 Ga2 N2 C7 -168.2(3) . . . . ? C21 Ga2 N2 C7 -44.7(3) . . . . ? C24 Ga2 N2 C5 -171.0(3) . . . . ? C27 Ga2 N2 C5 -51.9(3) . . . . ? C21 Ga2 N2 C5 71.7(3) . . . . ? C24 Ga2 N2 C6 -42.9(3) . . . . ? C27 Ga2 N2 C6 76.2(3) . . . . ? C21 Ga2 N2 C6 -160.2(3) . . . . ? C2 N1 C1 C6 57.2(4) . . . 2_655 ? C3 N1 C1 C6 -62.5(4) . . . 2_655 ? Ga1 N1 C1 C6 172.6(3) . . . 2_655 ? C2 N1 C3 C4 177.6(4) . . . . ? C1 N1 C3 C4 -61.0(5) . . . . ? Ga1 N1 C3 C4 60.8(4) . . . . ? N1 C3 C4 C5 179.3(3) . . . . ? C7 N2 C5 C4 -60.6(4) . . . . ? C6 N2 C5 C4 58.7(4) . . . . ? Ga2 N2 C5 C4 -172.5(3) . . . . ? C3 C4 C5 N2 180.0(3) . . . . ? C7 N2 C6 C1 -178.9(3) . . . 2_655 ? C5 N2 C6 C1 60.6(4) . . . 2_655 ? Ga2 N2 C6 C1 -66.1(4) . . . 2_655 ? C17 Ga1 C11 C12 31.5(4) . . . . ? C14 Ga1 C11 C12 168.7(4) . . . . ? N1 Ga1 C11 C12 -76.4(4) . . . . ? C17 Ga1 C11 C13 -92.3(4) . . . . ? C14 Ga1 C11 C13 44.8(4) . . . . ? N1 Ga1 C11 C13 159.7(3) . . . . ? C17 Ga1 C14 C16 58.2(4) . . . . ? C11 Ga1 C14 C16 -80.5(4) . . . . ? N1 Ga1 C14 C16 168.2(3) . . . . ? C17 Ga1 C14 C15 -178.0(3) . . . . ? C11 Ga1 C14 C15 43.2(4) . . . . ? N1 Ga1 C14 C15 -68.1(4) . . . . ? C11 Ga1 C17 C18 163.3(3) . . . . ? C14 Ga1 C17 C18 26.6(4) . . . . ? N1 Ga1 C17 C18 -87.8(4) . . . . ? C11 Ga1 C17 C19 41.0(4) . . . . ? C14 Ga1 C17 C19 -95.7(4) . . . . ? N1 Ga1 C17 C19 149.8(3) . . . . ? C24 Ga2 C21 C23 58.3(4) . . . . ? C27 Ga2 C21 C23 -72.2(4) . . . . ? N2 Ga2 C21 C23 171.7(4) . . . . ? C24 Ga2 C21 C22 -177.3(3) . . . . ? C27 Ga2 C21 C22 52.2(4) . . . . ? N2 Ga2 C21 C22 -63.9(4) . . . . ? C27 Ga2 C24 C26 -43.8(4) . . . . ? C21 Ga2 C24 C26 -177.2(3) . . . . ? N2 Ga2 C24 C26 72.2(4) . . . . ? C27 Ga2 C24 C25 -179.6(4) . . . . ? C21 Ga2 C24 C25 47.0(4) . . . . ? N2 Ga2 C24 C25 -63.6(4) . . . . ? C24 Ga2 C27 C28 -170.2(3) . . . . ? C21 Ga2 C27 C28 -39.6(4) . . . . ? N2 Ga2 C27 C28 73.9(4) . . . . ? C24 Ga2 C27 C29 -46.9(4) . . . . ? C21 Ga2 C27 C29 83.7(4) . . . . ? N2 Ga2 C27 C29 -162.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 24.25 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 0.583 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.089 data_compound5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H102 Ga4 N6' _chemical_formula_weight 970.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 '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' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.1630 1.6090 '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 9.2460(15) _cell_length_b 10.902(2) _cell_length_c 13.421(3) _cell_angle_alpha 74.15(2) _cell_angle_beta 81.74(2) _cell_angle_gamma 85.47(2) _cell_volume 1286.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 2.027 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6480 _diffrn_reflns_av_R_equivalents 0.0948 _diffrn_reflns_av_sigmaI/netI 0.0983 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 24.18 _reflns_number_total 3801 _reflns_number_gt 2671 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3801 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.19209(5) 0.56829(4) 0.76385(4) 0.02267(16) Uani 1 d . . . Ga2 Ga -0.34089(5) 0.09886(4) 0.75477(4) 0.02515(17) Uani 1 d . . . N1 N -0.0167(4) 0.5157(3) 0.7275(3) 0.0197(8) Uani 1 d . . . N2 N -0.1293(4) 0.1657(3) 0.7723(3) 0.0226(9) Uani 1 d . . . N3 N 0.0613(4) 0.2542(3) 0.5375(3) 0.0218(8) Uani 1 d . . . C11 C -0.0380(5) 0.5639(4) 0.6161(4) 0.0237(10) Uani 1 d . . . H11A H -0.1378 0.5440 0.6084 0.028 Uiso 1 calc R . . H11B H 0.0321 0.5168 0.5754 0.028 Uiso 1 calc R . . C12 C -0.0077(5) 0.3725(4) 0.7565(4) 0.0237(10) Uani 1 d . . . H12A H 0.0024 0.3413 0.8318 0.028 Uiso 1 calc R . . H12B H 0.0823 0.3446 0.7175 0.028 Uiso 1 calc R . . C13 C -0.1385(5) 0.5615(4) 0.7958(4) 0.0280(11) Uani 1 d . . . H13A H -0.1215 0.5285 0.8689 0.042 Uiso 1 calc R . . H13B H -0.2312 0.5310 0.7863 0.042 Uiso 1 calc R . . H13C H -0.1429 0.6550 0.7769 0.042 Uiso 1 calc R . . C21 C -0.1365(5) 0.3091(4) 0.7356(4) 0.0238(10) Uani 1 d . . . H21A H -0.2275 0.3413 0.7705 0.029 Uiso 1 calc R . . H21B H -0.1423 0.3348 0.6596 0.029 Uiso 1 calc R . . C22 C -0.0052(5) 0.1059(4) 0.7160(4) 0.0233(10) Uani 1 d . . . H22A H -0.0059 0.0123 0.7464 0.028 Uiso 1 calc R . . H22B H 0.0872 0.1353 0.7290 0.028 Uiso 1 calc R . . C23 C -0.1167(6) 0.1206(4) 0.8855(4) 0.0323(12) Uani 1 d . . . H23A H -0.1127 0.0270 0.9070 0.048 Uiso 1 calc R . . H23B H -0.2017 0.1528 0.9249 0.048 Uiso 1 calc R . . H23C H -0.0272 0.1520 0.8995 0.048 Uiso 1 calc R . . C31 C -0.0050(5) 0.1335(4) 0.5978(4) 0.0231(10) Uani 1 d . . . H31A H 0.0489 0.0625 0.5737 0.028 Uiso 1 calc R . . H31B H -0.1072 0.1357 0.5830 0.028 Uiso 1 calc R . . C32 C 0.0186(5) 0.2931(4) 0.4316(3) 0.0214(10) Uani 1 d . . . H32A H -0.0849 0.2735 0.4344 0.026 Uiso 1 calc R . . H32B H 0.0796 0.2447 0.3872 0.026 Uiso 1 calc R . . C33 C 0.2211(5) 0.2387(5) 0.5318(4) 0.0339(12) Uani 1 d . . . H33A H 0.2489 0.2126 0.6026 0.051 Uiso 1 calc R . . H33B H 0.2650 0.3199 0.4936 0.051 Uiso 1 calc R . . H33C H 0.2562 0.1733 0.4954 0.051 Uiso 1 calc R . . C14 C 0.3286(5) 0.5244(5) 0.6493(4) 0.0344(12) Uani 1 d . . . H14A H 0.3090 0.4373 0.6469 0.041 Uiso 1 calc R . . H14B H 0.3075 0.5839 0.5822 0.041 Uiso 1 calc R . . C15 C 0.4892(6) 0.5292(5) 0.6583(5) 0.0486(16) Uani 1 d . . . H15A H 0.5482 0.5064 0.5987 0.073 Uiso 1 calc R . . H15B H 0.5124 0.4687 0.7233 0.073 Uiso 1 calc R . . H15C H 0.5109 0.6156 0.6586 0.073 Uiso 1 calc R . . C16 C 0.2061(5) 0.4511(4) 0.9063(4) 0.0317(12) Uani 1 d . . . H16A H 0.1209 0.4687 0.9549 0.038 Uiso 1 calc R . . H16B H 0.2021 0.3617 0.9031 0.038 Uiso 1 calc R . . C17 C 0.3463(6) 0.4658(5) 0.9488(5) 0.0441(14) Uani 1 d . . . H17A H 0.3486 0.4058 1.0179 0.066 Uiso 1 calc R . . H17B H 0.3492 0.5533 0.9545 0.066 Uiso 1 calc R . . H17C H 0.4311 0.4479 0.9012 0.066 Uiso 1 calc R . . C18 C 0.1622(6) 0.7521(4) 0.7666(4) 0.0358(13) Uani 1 d . . . H18A H 0.2514 0.7977 0.7307 0.043 Uiso 1 calc R . . H18B H 0.0806 0.7909 0.7264 0.043 Uiso 1 calc R . . C19 C 0.1287(8) 0.7729(5) 0.8752(5) 0.0518(16) Uani 1 d . . . H19A H 0.1176 0.8646 0.8695 0.078 Uiso 1 calc R . . H19B H 0.2092 0.7358 0.9157 0.078 Uiso 1 calc R . . H19C H 0.0379 0.7318 0.9105 0.078 Uiso 1 calc R . . C24 C -0.4718(5) 0.1432(5) 0.8721(4) 0.0364(13) Uani 1 d . . . H24A H -0.4447 0.0880 0.9391 0.044 Uiso 1 calc R . . H24B H -0.4581 0.2329 0.8706 0.044 Uiso 1 calc R . . C25 C -0.6325(6) 0.1266(6) 0.8654(6) 0.0572(18) Uani 1 d . . . H25A H -0.6937 0.1482 0.9247 0.086 Uiso 1 calc R . . H25B H -0.6465 0.0378 0.8673 0.086 Uiso 1 calc R . . H25C H -0.6604 0.1831 0.8001 0.086 Uiso 1 calc R . . C26 C -0.3909(6) 0.1986(5) 0.6143(4) 0.0339(12) Uani 1 d . . . H26A H -0.4870 0.2437 0.6240 0.041 Uiso 1 calc R . . H26B H -0.3174 0.2644 0.5838 0.041 Uiso 1 calc R . . C27 C -0.3978(7) 0.1215(5) 0.5360(5) 0.0478(15) Uani 1 d . . . H27A H -0.4240 0.1787 0.4704 0.072 Uiso 1 calc R . . H27B H -0.4717 0.0571 0.5643 0.072 Uiso 1 calc R . . H27C H -0.3021 0.0793 0.5230 0.072 Uiso 1 calc R . . C28 C -0.2915(6) -0.0877(4) 0.7710(5) 0.0382(13) Uani 1 d . . . H28A H -0.2304 -0.0991 0.7070 0.046 Uiso 1 calc R . . H28B H -0.2341 -0.1209 0.8303 0.046 Uiso 1 calc R . . C29 C -0.4295(6) -0.1632(5) 0.7903(6) 0.0570(19) Uani 1 d . . . H29A H -0.4022 -0.2537 0.7979 0.086 Uiso 1 calc R . . H29B H -0.4856 -0.1313 0.7311 0.086 Uiso 1 calc R . . H29C H -0.4892 -0.1532 0.8543 0.086 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 0.0222(3) 0.0269(3) 0.0206(3) -0.0080(2) -0.0037(2) -0.0039(2) Ga2 0.0241(3) 0.0220(3) 0.0296(3) -0.0068(2) -0.0023(3) -0.0040(2) N1 0.0213(19) 0.0214(18) 0.016(2) -0.0045(16) -0.0019(17) -0.0030(15) N2 0.026(2) 0.0197(18) 0.020(2) -0.0024(17) -0.0007(18) -0.0078(15) N3 0.0184(19) 0.0284(19) 0.017(2) -0.0022(17) -0.0053(17) -0.0034(15) C11 0.030(2) 0.023(2) 0.021(3) -0.007(2) -0.007(2) -0.0013(19) C12 0.027(2) 0.021(2) 0.024(3) -0.006(2) -0.005(2) -0.0039(18) C13 0.028(3) 0.033(2) 0.025(3) -0.012(2) -0.001(2) -0.004(2) C21 0.027(2) 0.021(2) 0.024(3) -0.006(2) -0.006(2) -0.0020(18) C22 0.022(2) 0.023(2) 0.024(3) -0.002(2) -0.004(2) -0.0032(18) C23 0.039(3) 0.032(3) 0.024(3) -0.001(2) -0.008(2) -0.007(2) C31 0.027(2) 0.022(2) 0.022(3) -0.006(2) -0.005(2) -0.0055(18) C32 0.024(2) 0.026(2) 0.016(2) -0.006(2) -0.006(2) -0.0017(18) C33 0.029(3) 0.042(3) 0.029(3) -0.004(2) -0.009(2) -0.006(2) C14 0.029(3) 0.043(3) 0.033(3) -0.013(3) -0.002(2) -0.008(2) C15 0.032(3) 0.057(3) 0.057(4) -0.021(3) 0.007(3) -0.005(3) C16 0.032(3) 0.036(3) 0.031(3) -0.011(2) -0.013(2) -0.002(2) C17 0.036(3) 0.062(3) 0.039(3) -0.018(3) -0.015(3) 0.008(3) C18 0.045(3) 0.028(2) 0.039(3) -0.008(2) -0.017(3) -0.007(2) C19 0.080(5) 0.038(3) 0.045(4) -0.019(3) -0.023(3) 0.009(3) C24 0.034(3) 0.036(3) 0.035(3) -0.006(3) 0.003(3) -0.001(2) C25 0.040(3) 0.056(4) 0.061(5) -0.005(3) 0.017(3) 0.006(3) C26 0.030(3) 0.036(3) 0.039(3) -0.013(3) -0.010(3) 0.001(2) C27 0.053(4) 0.056(3) 0.042(4) -0.020(3) -0.016(3) -0.005(3) C28 0.035(3) 0.028(2) 0.056(4) -0.013(3) -0.019(3) -0.002(2) C29 0.043(3) 0.033(3) 0.095(6) -0.015(3) -0.005(4) -0.008(2) _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 C14 1.984(5) . ? Ga1 C16 2.004(5) . ? Ga1 C18 2.011(4) . ? Ga1 N1 2.212(4) . ? Ga2 C24 1.988(5) . ? Ga2 C26 2.000(5) . ? Ga2 C28 2.008(4) . ? Ga2 N2 2.206(4) . ? N1 C11 1.480(6) . ? N1 C13 1.490(5) . ? N1 C12 1.501(5) . ? N2 C23 1.482(6) . ? N2 C22 1.488(5) . ? N2 C21 1.505(5) . ? N3 C33 1.467(6) . ? N3 C32 1.471(6) . ? N3 C31 1.471(5) . ? C11 C32 1.529(6) 2_566 ? C12 C21 1.518(6) . ? C22 C31 1.531(7) . ? C32 C11 1.529(6) 2_566 ? C14 C15 1.513(7) . ? C16 C17 1.525(7) . ? C18 C19 1.521(8) . ? C24 C25 1.530(8) . ? C26 C27 1.525(7) . ? C28 C29 1.526(7) . ? 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 C14 Ga1 C16 115.2(2) . . ? C14 Ga1 C18 119.0(2) . . ? C16 Ga1 C18 112.2(2) . . ? C14 Ga1 N1 99.90(17) . . ? C16 Ga1 N1 102.09(17) . . ? C18 Ga1 N1 105.50(18) . . ? C24 Ga2 C26 113.1(2) . . ? C24 Ga2 C28 116.2(2) . . ? C26 Ga2 C28 115.8(2) . . ? C24 Ga2 N2 101.75(18) . . ? C26 Ga2 N2 106.66(18) . . ? C28 Ga2 N2 100.87(17) . . ? C11 N1 C13 111.2(3) . . ? C11 N1 C12 109.0(3) . . ? C13 N1 C12 110.0(3) . . ? C11 N1 Ga1 114.0(3) . . ? C13 N1 Ga1 108.3(3) . . ? C12 N1 Ga1 104.2(2) . . ? C23 N2 C22 107.8(3) . . ? C23 N2 C21 111.4(3) . . ? C22 N2 C21 113.3(3) . . ? C23 N2 Ga2 105.3(3) . . ? C22 N2 Ga2 111.3(3) . . ? C21 N2 Ga2 107.4(3) . . ? C33 N3 C32 109.9(4) . . ? C33 N3 C31 109.6(3) . . ? C32 N3 C31 110.6(3) . . ? N1 C11 C32 115.5(4) . 2_566 ? N1 C12 C21 115.8(3) . . ? N2 C21 C12 114.5(4) . . ? N2 C22 C31 115.8(4) . . ? N3 C31 C22 114.1(4) . . ? N3 C32 C11 110.3(3) . 2_566 ? C15 C14 Ga1 115.0(4) . . ? C17 C16 Ga1 112.6(4) . . ? C19 C18 Ga1 114.8(4) . . ? C25 C24 Ga2 111.6(4) . . ? C27 C26 Ga2 115.8(4) . . ? C29 C28 Ga2 111.2(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 C14 Ga1 N1 C11 -46.7(3) . . . . ? C16 Ga1 N1 C11 -165.3(3) . . . . ? C18 Ga1 N1 C11 77.3(3) . . . . ? C14 Ga1 N1 C13 -171.0(3) . . . . ? C16 Ga1 N1 C13 70.4(3) . . . . ? C18 Ga1 N1 C13 -47.0(3) . . . . ? C14 Ga1 N1 C12 72.0(3) . . . . ? C16 Ga1 N1 C12 -46.6(3) . . . . ? C18 Ga1 N1 C12 -164.0(3) . . . . ? C24 Ga2 N2 C23 44.9(3) . . . . ? C26 Ga2 N2 C23 163.6(3) . . . . ? C28 Ga2 N2 C23 -75.1(3) . . . . ? C24 Ga2 N2 C22 161.4(3) . . . . ? C26 Ga2 N2 C22 -79.8(3) . . . . ? C28 Ga2 N2 C22 41.5(3) . . . . ? C24 Ga2 N2 C21 -74.0(3) . . . . ? C26 Ga2 N2 C21 44.7(3) . . . . ? C28 Ga2 N2 C21 166.1(3) . . . . ? C13 N1 C11 C32 70.4(5) . . . 2_566 ? C12 N1 C11 C32 -168.1(4) . . . 2_566 ? Ga1 N1 C11 C32 -52.2(4) . . . 2_566 ? C11 N1 C12 C21 -55.8(5) . . . . ? C13 N1 C12 C21 66.3(5) . . . . ? Ga1 N1 C12 C21 -177.8(3) . . . . ? C23 N2 C21 C12 57.0(5) . . . . ? C22 N2 C21 C12 -64.9(5) . . . . ? Ga2 N2 C21 C12 171.8(3) . . . . ? N1 C12 C21 N2 -175.9(4) . . . . ? C23 N2 C22 C31 175.8(4) . . . . ? C21 N2 C22 C31 -60.3(5) . . . . ? Ga2 N2 C22 C31 60.9(4) . . . . ? C33 N3 C31 C22 76.0(5) . . . . ? C32 N3 C31 C22 -162.7(3) . . . . ? N2 C22 C31 N3 84.6(5) . . . . ? C33 N3 C32 C11 -79.7(4) . . . 2_566 ? C31 N3 C32 C11 159.2(3) . . . 2_566 ? C16 Ga1 C14 C15 -62.5(4) . . . . ? C18 Ga1 C14 C15 75.0(5) . . . . ? N1 Ga1 C14 C15 -171.0(4) . . . . ? C14 Ga1 C16 C17 71.1(4) . . . . ? C18 Ga1 C16 C17 -69.3(4) . . . . ? N1 Ga1 C16 C17 178.3(3) . . . . ? C14 Ga1 C18 C19 -148.7(4) . . . . ? C16 Ga1 C18 C19 -10.0(5) . . . . ? N1 Ga1 C18 C19 100.4(4) . . . . ? C26 Ga2 C24 C25 56.2(4) . . . . ? C28 Ga2 C24 C25 -81.3(4) . . . . ? N2 Ga2 C24 C25 170.2(4) . . . . ? C24 Ga2 C26 C27 -133.2(4) . . . . ? C28 Ga2 C26 C27 4.4(5) . . . . ? N2 Ga2 C26 C27 115.7(4) . . . . ? C24 Ga2 C28 C29 56.1(5) . . . . ? C26 Ga2 C28 C29 -80.2(5) . . . . ? N2 Ga2 C28 C29 165.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 24.18 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.682 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.095 data_compound6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H132 Ga6 N6' _chemical_formula_weight 1284.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 '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' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.1630 1.6090 '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 11.706(4) _cell_length_b 13.370(3) _cell_length_c 23.081(4) _cell_angle_alpha 104.64(2) _cell_angle_beta 90.77(4) _cell_angle_gamma 103.13(4) _cell_volume 3394.2(16) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 2.300 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18258 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 22.49 _reflns_number_total 8421 _reflns_number_gt 6166 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8421 _refine_ls_number_parameters 599 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.39907(4) 0.25504(4) 0.01143(2) 0.03160(14) Uani 1 d . . . C14 C 0.3910(5) 0.1005(4) -0.0189(2) 0.0464(13) Uani 1 d . . . H14A H 0.4188 0.0747 0.0140 0.056 Uiso 1 calc R . . H14B H 0.3079 0.0620 -0.0306 0.056 Uiso 1 calc R . . C15 C 0.4627(7) 0.0736(5) -0.0718(3) 0.080(2) Uani 1 d . . . H15A H 0.4545 -0.0036 -0.0843 0.120 Uiso 1 calc R . . H15B H 0.5456 0.1096 -0.0603 0.120 Uiso 1 calc R . . H15C H 0.4346 0.0971 -0.1050 0.120 Uiso 1 calc R . . C16 C 0.4934(5) 0.3319(5) 0.0892(2) 0.0517(14) Uani 1 d . . . H16A H 0.5531 0.3925 0.0824 0.062 Uiso 1 calc R . . H16B H 0.4403 0.3620 0.1180 0.062 Uiso 1 calc R . . C17 C 0.5546(6) 0.2694(7) 0.1179(4) 0.103(3) Uani 1 d . . . H17A H 0.5979 0.3154 0.1553 0.155 Uiso 1 calc R . . H17B H 0.6098 0.2407 0.0906 0.155 Uiso 1 calc R . . H17C H 0.4968 0.2106 0.1266 0.155 Uiso 1 calc R . . C18 C 0.4232(4) 0.3355(4) -0.0513(2) 0.0396(12) Uani 1 d . . . H18A H 0.3838 0.2888 -0.0901 0.047 Uiso 1 calc R . . H18B H 0.3869 0.3971 -0.0399 0.047 Uiso 1 calc R . . C19 C 0.5540(4) 0.3750(5) -0.0586(3) 0.0593(16) Uani 1 d . . . H19A H 0.5632 0.4141 -0.0896 0.089 Uiso 1 calc R . . H19B H 0.5898 0.3140 -0.0705 0.089 Uiso 1 calc R . . H19C H 0.5929 0.4222 -0.0204 0.089 Uiso 1 calc R . . Ga2 Ga 0.04326(4) 0.33753(4) -0.13569(2) 0.03384(14) Uani 1 d . . . C24 C 0.1592(4) 0.2651(4) -0.1804(2) 0.0427(13) Uani 1 d . . . H24A H 0.1979 0.2329 -0.1539 0.051 Uiso 1 calc R . . H24B H 0.1180 0.2073 -0.2152 0.051 Uiso 1 calc R . . C25 C 0.2511(6) 0.3439(5) -0.2022(3) 0.0695(18) Uani 1 d . . . H25A H 0.3075 0.3074 -0.2241 0.104 Uiso 1 calc R . . H25B H 0.2926 0.4006 -0.1677 0.104 Uiso 1 calc R . . H25C H 0.2128 0.3749 -0.2290 0.104 Uiso 1 calc R . . C26 C 0.1086(5) 0.4710(4) -0.0718(2) 0.0539(15) Uani 1 d . . . H26A H 0.0496 0.4817 -0.0420 0.065 Uiso 1 calc R . . H26B H 0.1791 0.4631 -0.0509 0.065 Uiso 1 calc R . . C27 C 0.1417(6) 0.5674(5) -0.0953(3) 0.0749(19) Uani 1 d . . . H27A H 0.1730 0.6303 -0.0619 0.112 Uiso 1 calc R . . H27B H 0.0721 0.5768 -0.1153 0.112 Uiso 1 calc R . . H27C H 0.2018 0.5584 -0.1240 0.112 Uiso 1 calc R . . C28 C -0.0901(6) 0.3453(6) -0.1880(3) 0.077(2) Uani 1 d . . . H28A H -0.1265 0.2728 -0.2132 0.092 Uiso 1 calc R A 1 H28B H -0.1504 0.3699 -0.1621 0.092 Uiso 1 calc R A 1 C29 C -0.0596(14) 0.4092(14) -0.2234(7) 0.133(7) Uiso 0.640(14) d P B 1 H29A H -0.1293 0.4086 -0.2477 0.199 Uiso 0.640(14) calc PR B 1 H29B H -0.0013 0.3847 -0.2500 0.199 Uiso 0.640(14) calc PR B 1 H29C H -0.0258 0.4818 -0.1989 0.199 Uiso 0.640(14) calc PR B 1 C29' C -0.120(2) 0.249(2) -0.2532(12) 0.137(12) Uiso 0.360(14) d P B 2 H29D H -0.1865 0.2576 -0.2761 0.206 Uiso 0.360(14) calc PR B 2 H29E H -0.1403 0.1789 -0.2446 0.206 Uiso 0.360(14) calc PR B 2 H29F H -0.0509 0.2536 -0.2767 0.206 Uiso 0.360(14) calc PR B 2 Ga3 Ga -0.01602(5) -0.12446(4) -0.18485(2) 0.03799(15) Uani 1 d . . . C34 C -0.0774(6) -0.2809(4) -0.2132(2) 0.0604(17) Uani 1 d . . . H34A H -0.0895 -0.3111 -0.1781 0.072 Uiso 1 calc R . . H34B H -0.1545 -0.2969 -0.2360 0.072 Uiso 1 calc R . . C35 C 0.0074(8) -0.3334(6) -0.2533(3) 0.110(3) Uani 1 d . . . H35A H -0.0256 -0.4104 -0.2668 0.165 Uiso 1 calc R . . H35B H 0.0832 -0.3192 -0.2305 0.165 Uiso 1 calc R . . H35C H 0.0189 -0.3042 -0.2883 0.165 Uiso 1 calc R . . C36 C 0.0085(5) -0.0519(5) -0.2508(2) 0.0576(16) Uani 1 d . . . H36A H -0.0188 0.0148 -0.2383 0.069 Uiso 1 calc R . . H36B H 0.0941 -0.0316 -0.2550 0.069 Uiso 1 calc R . . C37 C -0.0517(6) -0.1139(6) -0.3120(2) 0.080(2) Uani 1 d . . . H37A H -0.0330 -0.0703 -0.3405 0.120 Uiso 1 calc R . . H37B H -0.1370 -0.1323 -0.3092 0.120 Uiso 1 calc R . . H37C H -0.0240 -0.1792 -0.3259 0.120 Uiso 1 calc R . . C38 C 0.1118(4) -0.0689(4) -0.1186(2) 0.0405(12) Uani 1 d . . . H38A H 0.1719 -0.0114 -0.1283 0.049 Uiso 1 calc R . . H38B H 0.0783 -0.0373 -0.0811 0.049 Uiso 1 calc R . . C39 C 0.1715(5) -0.1526(4) -0.1075(2) 0.0550(15) Uani 1 d . . . H39A H 0.2329 -0.1198 -0.0746 0.082 Uiso 1 calc R . . H39B H 0.2069 -0.1831 -0.1440 0.082 Uiso 1 calc R . . H39C H 0.1132 -0.2090 -0.0968 0.082 Uiso 1 calc R . . N1 N 0.2104(3) 0.2547(3) 0.03064(14) 0.0249(8) Uani 1 d . . . C11 C 0.1525(4) 0.1679(4) 0.05836(18) 0.0309(11) Uani 1 d . . . H11A H 0.1318 0.0997 0.0268 0.037 Uiso 1 calc R . . H11B H 0.0785 0.1831 0.0746 0.037 Uiso 1 calc R . . C12 C 0.1455(3) 0.2383(3) -0.02819(17) 0.0240(10) Uani 1 d . . . H12A H 0.1477 0.1674 -0.0540 0.029 Uiso 1 calc R . . H12B H 0.1869 0.2923 -0.0480 0.029 Uiso 1 calc R . . C13 C 0.2121(4) 0.3607(4) 0.07066(18) 0.0335(11) Uani 1 d . . . H13A H 0.2549 0.3695 0.1091 0.050 Uiso 1 calc R . . H13B H 0.1312 0.3668 0.0776 0.050 Uiso 1 calc R . . H13C H 0.2513 0.4160 0.0518 0.050 Uiso 1 calc R . . N2 N -0.0474(3) 0.2287(3) -0.08303(14) 0.0251(8) Uani 1 d . . . C21 C 0.0175(4) 0.2453(4) -0.02410(17) 0.0285(10) Uani 1 d . . . H21A H -0.0239 0.1913 -0.0042 0.034 Uiso 1 calc R . . H21B H 0.0152 0.3162 0.0017 0.034 Uiso 1 calc R . . C22 C -0.0679(4) 0.1186(4) -0.12191(17) 0.0284(10) Uani 1 d . . . H22A H 0.0094 0.1022 -0.1306 0.034 Uiso 1 calc R . . H22B H -0.1079 0.1158 -0.1606 0.034 Uiso 1 calc R . . C23 C -0.1614(4) 0.2594(4) -0.0703(2) 0.0389(12) Uani 1 d . . . H23A H -0.2065 0.2496 -0.1082 0.058 Uiso 1 calc R . . H23B H -0.1459 0.3342 -0.0474 0.058 Uiso 1 calc R . . H23C H -0.2067 0.2145 -0.0469 0.058 Uiso 1 calc R . . N3 N -0.1686(3) -0.0750(3) -0.13944(14) 0.0285(9) Uani 1 d . . . C31 C -0.1404(4) 0.0320(4) -0.09661(18) 0.0299(11) Uani 1 d . . . H31A H -0.0967 0.0289 -0.0603 0.036 Uiso 1 calc R . . H31B H -0.2149 0.0513 -0.0841 0.036 Uiso 1 calc R . . C32 C -0.2299(4) -0.1564(4) -0.10852(18) 0.0324(11) Uani 1 d . . . H32A H -0.2556 -0.2261 -0.1385 0.039 Uiso 1 calc R . . H32B H -0.3010 -0.1358 -0.0917 0.039 Uiso 1 calc R . . C33 C -0.2558(4) -0.0780(4) -0.1879(2) 0.0470(14) Uani 1 d . . . H33A H -0.2743 -0.1487 -0.2164 0.071 Uiso 1 calc R . . H33B H -0.2226 -0.0242 -0.2090 0.071 Uiso 1 calc R . . H33C H -0.3277 -0.0631 -0.1702 0.071 Uiso 1 calc R . . Ga4 Ga 0.47308(5) 0.54257(4) 0.35691(2) 0.03514(15) Uani 1 d . . . C44 C 0.4045(5) 0.4550(4) 0.4118(2) 0.0524(14) Uani 1 d . . . H44A H 0.4683 0.4481 0.4380 0.063 Uiso 1 calc R . . H44B H 0.3511 0.4909 0.4377 0.063 Uiso 1 calc R . . C45 C 0.3375(7) 0.3461(5) 0.3764(3) 0.095(3) Uani 1 d . . . H45A H 0.3043 0.3043 0.4041 0.142 Uiso 1 calc R . . H45B H 0.3907 0.3102 0.3513 0.142 Uiso 1 calc R . . H45C H 0.2737 0.3529 0.3508 0.142 Uiso 1 calc R . . C46 C 0.3594(5) 0.5722(5) 0.3028(2) 0.0514(14) Uani 1 d . . . H46A H 0.2788 0.5404 0.3116 0.062 Uiso 1 calc R . . H46B H 0.3685 0.6502 0.3121 0.062 Uiso 1 calc R . . C47 C 0.3720(7) 0.5309(6) 0.2366(3) 0.094(2) Uani 1 d . . . H47A H 0.3128 0.5492 0.2134 0.141 Uiso 1 calc R . . H47B H 0.3606 0.4534 0.2264 0.141 Uiso 1 calc R . . H47C H 0.4508 0.5633 0.2270 0.141 Uiso 1 calc R . . C48 C 0.6136(6) 0.5058(5) 0.3188(3) 0.0656(17) Uani 1 d . . . H48A H 0.5931 0.4759 0.2751 0.079 Uiso 1 calc R C 1 H48B H 0.6758 0.5722 0.3243 0.079 Uiso 1 calc R C 1 C49 C 0.6628(11) 0.4290(11) 0.3416(6) 0.096(5) Uiso 0.640(16) d PU D 1 H49A H 0.7317 0.4159 0.3200 0.144 Uiso 0.640(16) calc PR D 1 H49B H 0.6031 0.3619 0.3353 0.144 Uiso 0.640(16) calc PR D 1 H49C H 0.6860 0.4584 0.3846 0.144 Uiso 0.640(16) calc PR D 1 C49' C 0.616(2) 0.412(2) 0.2824(13) 0.128(12) Uiso 0.360(16) d PU D 2 H49D H 0.6966 0.4126 0.2713 0.192 Uiso 0.360(16) calc PR D 2 H49E H 0.5642 0.3983 0.2462 0.192 Uiso 0.360(16) calc PR D 2 H49F H 0.5891 0.3562 0.3030 0.192 Uiso 0.360(16) calc PR D 2 Ga5 Ga 0.0942(3) 0.7487(3) 0.45289(13) 0.0363(6) Uani 0.576(8) d PDU E 1 C54 C 0.0701(8) 0.6146(8) 0.3897(4) 0.051(3) Uiso 0.576(8) d PDU E 1 H54A H 0.1340 0.6180 0.3621 0.061 Uiso 0.576(8) calc PR E 1 H54B H 0.0682 0.5542 0.4075 0.061 Uiso 0.576(8) calc PR E 1 C55 C -0.0543(13) 0.6012(16) 0.3548(8) 0.147(7) Uiso 0.576(8) d PDU E 1 H55A H -0.0720 0.5349 0.3226 0.220 Uiso 0.576(8) calc PR E 1 H55B H -0.0507 0.6616 0.3374 0.220 Uiso 0.576(8) calc PR E 1 H55C H -0.1162 0.5991 0.3829 0.220 Uiso 0.576(8) calc PR E 1 C56 C -0.0217(8) 0.7512(7) 0.5134(4) 0.039(3) Uiso 0.576(8) d PDU E 1 H56A H 0.0128 0.8095 0.5493 0.047 Uiso 0.576(8) calc PR E 1 H56B H -0.0910 0.7693 0.4974 0.047 Uiso 0.576(8) calc PR E 1 C57 C -0.0685(14) 0.6413(12) 0.5352(7) 0.124(6) Uiso 0.576(8) d PDU E 1 H57A H -0.1241 0.6532 0.5662 0.186 Uiso 0.576(8) calc PR E 1 H57B H -0.0014 0.6221 0.5517 0.186 Uiso 0.576(8) calc PR E 1 H57C H -0.1078 0.5834 0.5008 0.186 Uiso 0.576(8) calc PR E 1 C58 C 0.1261(11) 0.8796(9) 0.4210(5) 0.059(3) Uiso 0.576(8) d PDU E 1 H58A H 0.0786 0.9291 0.4410 0.071 Uiso 0.576(8) calc PR E 1 H58B H 0.2103 0.9170 0.4292 0.071 Uiso 0.576(8) calc PR E 1 C59 C 0.0916(12) 0.8416(12) 0.3497(5) 0.101(5) Uiso 0.576(8) d PDU E 1 H59A H 0.1065 0.9038 0.3333 0.152 Uiso 0.576(8) calc PR E 1 H59B H 0.0080 0.8052 0.3421 0.152 Uiso 0.576(8) calc PR E 1 H59C H 0.1391 0.7928 0.3304 0.152 Uiso 0.576(8) calc PR E 1 Ga5' Ga 0.1029(5) 0.7348(5) 0.4659(3) 0.0949(19) Uani 0.424(8) d PDU E 2 C54' C 0.0769(10) 0.5889(9) 0.4098(6) 0.048(4) Uiso 0.424(8) d PDU E 2 H54C H 0.1280 0.5911 0.3760 0.058 Uiso 0.424(8) calc PR E 2 H54D H 0.0978 0.5395 0.4313 0.058 Uiso 0.424(8) calc PR E 2 C55' C -0.0593(10) 0.5472(12) 0.3841(6) 0.066(4) Uiso 0.424(8) d PDU E 2 H55D H -0.0714 0.4762 0.3564 0.100 Uiso 0.424(8) calc PR E 2 H55E H -0.0796 0.5963 0.3629 0.100 Uiso 0.424(8) calc PR E 2 H55F H -0.1094 0.5437 0.4176 0.100 Uiso 0.424(8) calc PR E 2 C56' C -0.0041(12) 0.7422(11) 0.5332(6) 0.050(4) Uiso 0.424(8) d PDU E 2 H56C H -0.0633 0.6740 0.5279 0.060 Uiso 0.424(8) calc PR E 2 H56D H 0.0410 0.7599 0.5725 0.060 Uiso 0.424(8) calc PR E 2 C57' C -0.0697(13) 0.8427(12) 0.5277(7) 0.079(5) Uiso 0.424(8) d PDU E 2 H57D H -0.1236 0.8535 0.5596 0.119 Uiso 0.424(8) calc PR E 2 H57E H -0.1138 0.8232 0.4884 0.119 Uiso 0.424(8) calc PR E 2 H57F H -0.0091 0.9086 0.5318 0.119 Uiso 0.424(8) calc PR E 2 C58' C 0.113(2) 0.8493(16) 0.4244(10) 0.108(9) Uiso 0.424(8) d PDU E 2 H58C H 0.1964 0.8892 0.4274 0.129 Uiso 0.424(8) calc PR E 2 H58D H 0.0886 0.8163 0.3813 0.129 Uiso 0.424(8) calc PR E 2 C59' C 0.033(3) 0.933(3) 0.4513(16) 0.28(2) Uiso 0.424(8) d PDU E 2 H59D H 0.0425 0.9866 0.4287 0.421 Uiso 0.424(8) calc PR E 2 H59E H 0.0584 0.9671 0.4937 0.421 Uiso 0.424(8) calc PR E 2 H59F H -0.0496 0.8941 0.4476 0.421 Uiso 0.424(8) calc PR E 2 Ga6 Ga 0.44477(6) 1.02119(5) 0.67729(2) 0.04636(17) Uani 1 d D . . C64 C 0.4629(6) 1.1465(4) 0.7481(2) 0.0589(16) Uani 1 d . . . H64A H 0.4599 1.2103 0.7344 0.071 Uiso 1 calc R . . H64B H 0.3971 1.1338 0.7739 0.071 Uiso 1 calc R . . C65 C 0.5783(7) 1.1659(6) 0.7840(3) 0.091(2) Uani 1 d . . . H65A H 0.5858 1.2278 0.8185 0.137 Uiso 1 calc R . . H65B H 0.6434 1.1795 0.7585 0.137 Uiso 1 calc R . . H65C H 0.5807 1.1032 0.7981 0.137 Uiso 1 calc R . . C66 C 0.5853(5) 1.0231(5) 0.6292(2) 0.0513(14) Uani 1 d . . . H66A H 0.5610 1.0177 0.5870 0.062 Uiso 1 calc R . . H66B H 0.6431 1.0920 0.6449 0.062 Uiso 1 calc R . . C67 C 0.6445(7) 0.9334(7) 0.6303(3) 0.096(3) Uani 1 d . . . H67A H 0.7131 0.9389 0.6065 0.143 Uiso 1 calc R . . H67B H 0.5888 0.8647 0.6134 0.143 Uiso 1 calc R . . H67C H 0.6697 0.9386 0.6719 0.143 Uiso 1 calc R . . C68 C 0.426(2) 0.8895(12) 0.7022(6) 0.050(6) Uiso 0.330(17) d PDU F 1 H68A H 0.3568 0.8402 0.6770 0.060 Uiso 0.330(17) calc PR F 1 H68B H 0.4946 0.8615 0.6876 0.060 Uiso 0.330(17) calc PR F 1 C69 C 0.4142(18) 0.8721(15) 0.7538(6) 0.047(5) Uiso 0.330(17) d PDU F 1 H69A H 0.3945 0.7952 0.7495 0.071 Uiso 0.330(17) calc PR F 1 H69B H 0.3511 0.9027 0.7727 0.071 Uiso 0.330(17) calc PR F 1 H69C H 0.4881 0.9050 0.7789 0.071 Uiso 0.330(17) calc PR F 1 C68' C 0.3544(8) 0.8849(6) 0.6934(3) 0.038(2) Uiso 0.670(17) d PDU F 2 H68C H 0.2716 0.8728 0.6781 0.045 Uiso 0.670(17) calc PR F 2 H68D H 0.3856 0.8262 0.6690 0.045 Uiso 0.670(17) calc PR F 2 C69' C 0.3540(15) 0.8765(11) 0.7496(5) 0.102(4) Uiso 0.670(17) d PDU F 2 H69D H 0.3059 0.8067 0.7504 0.153 Uiso 0.670(17) calc PR F 2 H69E H 0.3212 0.9325 0.7746 0.153 Uiso 0.670(17) calc PR F 2 H69F H 0.4347 0.8841 0.7651 0.153 Uiso 0.670(17) calc PR F 2 N4 N 0.5493(3) 0.6986(3) 0.42247(14) 0.0282(8) Uani 1 d . . . C41 C 0.5802(4) 0.7794(3) 0.38756(18) 0.0264(10) Uani 1 d . . . H41A H 0.5066 0.7857 0.3686 0.032 Uiso 1 calc R . . H41B H 0.6284 0.7530 0.3549 0.032 Uiso 1 calc R . . C42 C 0.4723(4) 0.7272(4) 0.47168(18) 0.0326(11) Uani 1 d . . . H42A H 0.5110 0.7981 0.4981 0.039 Uiso 1 calc R . . H42B H 0.4650 0.6751 0.4961 0.039 Uiso 1 calc R . . C43 C 0.6576(4) 0.6837(4) 0.4504(2) 0.0456(13) Uani 1 d . . . H43A H 0.7108 0.6652 0.4192 0.068 Uiso 1 calc R . . H43B H 0.6363 0.6262 0.4703 0.068 Uiso 1 calc R . . H43C H 0.6969 0.7498 0.4799 0.068 Uiso 1 calc R . . N5 N 0.2752(3) 0.7645(3) 0.50067(16) 0.0377(10) Uani 1 d . . . C51 C 0.3498(4) 0.7299(4) 0.45080(18) 0.0314(11) Uani 1 d . . . H51A H 0.3570 0.7789 0.4245 0.038 Uiso 1 calc R . . H51B H 0.3092 0.6579 0.4264 0.038 Uiso 1 calc R . . C52 C 0.3320(4) 0.8742(4) 0.5351(2) 0.0360(12) Uani 1 d . . . H52A H 0.3631 0.9162 0.5066 0.043 Uiso 1 calc R . . H52B H 0.3995 0.8724 0.5607 0.043 Uiso 1 calc R . . C53 C 0.2593(6) 0.6913(4) 0.5402(2) 0.0625(17) Uani 1 d . . . H53A H 0.2210 0.6191 0.5166 0.094 Uiso 1 calc R . . H53B H 0.2103 0.7149 0.5725 0.094 Uiso 1 calc R . . H53C H 0.3363 0.6915 0.5575 0.094 Uiso 1 calc R . . N6 N 0.3104(3) 1.0358(3) 0.61440(16) 0.0351(10) Uani 1 d . . . C61 C 0.2495(4) 0.9304(4) 0.5747(2) 0.0455(14) Uani 1 d . . . H61A H 0.1871 0.9401 0.5487 0.055 Uiso 1 calc R . . H61B H 0.2110 0.8844 0.5999 0.055 Uiso 1 calc R . . C62 C 0.3529(4) 1.1095(4) 0.57650(19) 0.0323(11) Uani 1 d . . . H62A H 0.2846 1.1161 0.5532 0.039 Uiso 1 calc R . . H62B H 0.4050 1.0783 0.5475 0.039 Uiso 1 calc R . . C63 C 0.2187(5) 1.0756(5) 0.6524(3) 0.0655(19) Uani 1 d . . . H63A H 0.1901 1.0276 0.6777 0.098 Uiso 1 calc R . . H63B H 0.1529 1.0778 0.6264 0.098 Uiso 1 calc R . . H63C H 0.2531 1.1472 0.6779 0.098 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 0.0290(3) 0.0284(3) 0.0369(3) 0.0102(2) 0.0017(2) 0.0039(2) C14 0.051(3) 0.031(3) 0.054(3) 0.007(2) 0.000(3) 0.009(2) C15 0.122(6) 0.045(5) 0.086(5) 0.019(3) 0.047(4) 0.039(4) C16 0.043(3) 0.055(4) 0.052(3) 0.011(3) -0.007(3) 0.004(3) C17 0.068(5) 0.106(7) 0.135(7) 0.059(5) -0.057(5) -0.011(4) C18 0.037(3) 0.035(3) 0.048(3) 0.017(2) 0.011(2) 0.004(2) C19 0.046(3) 0.052(4) 0.073(4) 0.015(3) 0.026(3) -0.003(3) Ga2 0.0358(3) 0.0320(3) 0.0385(3) 0.0197(2) 0.0039(2) 0.0062(2) C24 0.053(3) 0.041(4) 0.034(3) 0.014(2) 0.010(2) 0.007(3) C25 0.082(4) 0.057(5) 0.080(4) 0.031(3) 0.047(4) 0.022(3) C26 0.071(4) 0.030(4) 0.062(3) 0.014(3) 0.018(3) 0.009(3) C27 0.098(5) 0.033(4) 0.096(5) 0.023(3) 0.032(4) 0.010(3) C28 0.065(4) 0.086(6) 0.088(5) 0.059(4) -0.019(4) -0.006(4) Ga3 0.0526(3) 0.0306(4) 0.0271(3) 0.0075(2) 0.0103(2) 0.0022(3) C34 0.101(5) 0.030(4) 0.040(3) 0.004(2) 0.020(3) 0.002(3) C35 0.192(9) 0.042(5) 0.087(5) 0.000(4) 0.071(6) 0.025(5) C36 0.078(4) 0.056(4) 0.029(3) 0.013(2) 0.014(3) -0.005(3) C37 0.101(5) 0.091(6) 0.033(3) 0.020(3) -0.002(3) -0.010(4) C38 0.035(3) 0.039(3) 0.053(3) 0.020(2) 0.013(2) 0.007(2) C39 0.061(4) 0.043(4) 0.067(4) 0.018(3) 0.013(3) 0.018(3) N1 0.0257(19) 0.020(2) 0.0287(18) 0.0117(15) 0.0020(15) -0.0007(15) C11 0.033(3) 0.024(3) 0.032(2) 0.0119(19) -0.003(2) -0.004(2) C12 0.027(2) 0.021(3) 0.025(2) 0.0104(18) 0.0025(18) 0.0047(19) C13 0.035(3) 0.030(3) 0.032(2) 0.007(2) 0.002(2) 0.002(2) N2 0.0231(19) 0.026(2) 0.0295(19) 0.0121(16) 0.0030(15) 0.0064(16) C21 0.027(2) 0.033(3) 0.026(2) 0.0107(19) 0.0033(18) 0.004(2) C22 0.029(2) 0.033(3) 0.023(2) 0.0105(19) 0.0014(19) 0.004(2) C23 0.031(3) 0.044(3) 0.046(3) 0.017(2) 0.006(2) 0.011(2) N3 0.033(2) 0.027(2) 0.0234(18) 0.0110(16) -0.0039(16) -0.0015(17) C31 0.033(3) 0.030(3) 0.027(2) 0.013(2) 0.0024(19) 0.004(2) C32 0.033(3) 0.034(3) 0.027(2) 0.013(2) -0.0029(19) -0.005(2) C33 0.053(3) 0.048(4) 0.038(3) 0.024(2) -0.012(2) -0.005(3) Ga4 0.0471(3) 0.0243(3) 0.0337(3) 0.0060(2) 0.0097(2) 0.0093(2) C44 0.068(4) 0.033(4) 0.052(3) 0.013(2) 0.009(3) 0.004(3) C45 0.142(7) 0.043(5) 0.083(5) 0.013(3) 0.028(5) -0.011(4) C46 0.067(4) 0.043(4) 0.037(3) 0.004(2) -0.006(3) 0.006(3) C47 0.123(6) 0.099(7) 0.050(4) 0.005(4) -0.005(4) 0.023(5) C48 0.082(4) 0.044(4) 0.073(4) 0.003(3) 0.029(3) 0.032(3) Ga5 0.0256(9) 0.0406(11) 0.0371(8) -0.0029(7) 0.0025(6) 0.0115(7) Ga5' 0.033(2) 0.090(3) 0.107(4) -0.043(2) 0.030(2) -0.0211(18) Ga6 0.0793(4) 0.0309(4) 0.0306(3) 0.0092(2) 0.0157(3) 0.0146(3) C64 0.101(5) 0.036(4) 0.038(3) 0.006(2) 0.015(3) 0.015(3) C65 0.117(6) 0.080(6) 0.052(4) -0.007(3) -0.006(4) 0.002(5) C66 0.056(3) 0.054(4) 0.046(3) 0.007(3) -0.003(3) 0.024(3) C67 0.113(6) 0.108(7) 0.094(5) 0.033(4) 0.012(5) 0.075(5) N4 0.034(2) 0.023(2) 0.0288(19) 0.0060(15) 0.0028(16) 0.0102(17) C41 0.027(2) 0.022(3) 0.029(2) 0.0049(18) 0.0052(18) 0.0064(19) C42 0.045(3) 0.028(3) 0.023(2) 0.0054(19) 0.005(2) 0.006(2) C43 0.040(3) 0.050(4) 0.052(3) 0.016(3) -0.006(2) 0.020(3) N5 0.041(2) 0.022(2) 0.041(2) -0.0013(17) 0.0201(18) -0.0020(18) C51 0.031(3) 0.028(3) 0.030(2) 0.0016(19) 0.007(2) 0.004(2) C52 0.035(3) 0.025(3) 0.042(3) 0.003(2) 0.014(2) -0.001(2) C53 0.092(5) 0.032(4) 0.059(3) 0.012(3) 0.042(3) 0.002(3) N6 0.031(2) 0.021(2) 0.043(2) -0.0049(17) 0.0206(17) -0.0015(17) C61 0.035(3) 0.029(3) 0.057(3) -0.005(2) 0.025(2) -0.004(2) C62 0.028(2) 0.028(3) 0.037(2) 0.003(2) 0.004(2) 0.004(2) C63 0.048(3) 0.047(4) 0.078(4) -0.016(3) 0.046(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 C14 1.987(5) . ? Ga1 C18 1.998(5) . ? Ga1 C16 1.999(5) . ? Ga1 N1 2.258(3) . ? C14 C15 1.504(7) . ? C16 C17 1.480(8) . ? C18 C19 1.528(6) . ? Ga2 C26 1.991(5) . ? Ga2 C24 1.994(5) . ? Ga2 C28 1.997(6) . ? Ga2 N2 2.224(3) . ? C24 C25 1.513(7) . ? C26 C27 1.495(8) . ? C28 C29 1.324(15) . ? C28 C29' 1.69(3) . ? Ga3 C34 1.983(5) . ? Ga3 C36 1.993(5) . ? Ga3 C38 1.997(5) . ? Ga3 N3 2.228(4) . ? C34 C35 1.533(9) . ? C36 C37 1.515(7) . ? C38 C39 1.517(7) . ? N1 C13 1.479(6) . ? N1 C12 1.488(5) . ? N1 C11 1.498(5) . ? C11 C32 1.520(6) 2 ? C12 C21 1.525(6) . ? N2 C22 1.482(6) . ? N2 C21 1.490(5) . ? N2 C23 1.495(5) . ? C22 C31 1.520(6) . ? N3 C31 1.481(6) . ? N3 C33 1.491(6) . ? N3 C32 1.504(5) . ? C32 C11 1.520(6) 2 ? Ga4 C48 1.977(6) . ? Ga4 C46 1.983(5) . ? Ga4 C44 1.992(5) . ? Ga4 N4 2.227(4) . ? C44 C45 1.505(8) . ? C46 C47 1.510(7) . ? C48 C49' 1.33(3) . ? C48 C49 1.483(14) . ? Ga5 C56 1.960(8) . ? Ga5 C54 1.964(8) . ? Ga5 C58 2.026(11) . ? C54 C55 1.607(13) . ? C56 C57 1.652(13) . ? C58 C59 1.611(13) . ? Ga5' C58' 1.983(13) . ? Ga5' C54' 2.004(10) . ? Ga5' C56' 2.006(10) . ? Ga5' N5 2.074(8) . ? C54' C55' 1.614(13) . ? C56' C57' 1.722(14) . ? C58' C59' 1.626(16) . ? Ga6 C68 1.955(13) . ? Ga6 C64 1.993(5) . ? Ga6 C66 1.996(5) . ? Ga6 C68' 2.013(7) . ? Ga6 N6 2.200(4) . ? C64 C65 1.510(9) . ? C66 C67 1.521(8) . ? C68 C69 1.272(14) . ? C68' C69' 1.330(10) . ? N4 C42 1.487(5) . ? N4 C41 1.489(5) . ? N4 C43 1.490(6) . ? C41 C62 1.529(6) 2_676 ? C42 C51 1.519(6) . ? N5 C52 1.476(6) . ? N5 C53 1.482(7) . ? N5 C51 1.497(5) . ? C52 C61 1.530(6) . ? N6 C61 1.485(6) . ? N6 C62 1.486(6) . ? N6 C63 1.501(6) . ? C62 C41 1.529(6) 2_676 ? 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 C14 Ga1 C18 114.5(2) . . ? C14 Ga1 C16 117.2(2) . . ? C18 Ga1 C16 113.8(2) . . ? C14 Ga1 N1 101.82(18) . . ? C18 Ga1 N1 101.49(16) . . ? C16 Ga1 N1 105.38(18) . . ? C15 C14 Ga1 113.9(4) . . ? C17 C16 Ga1 117.0(5) . . ? C19 C18 Ga1 111.2(4) . . ? C26 Ga2 C24 116.7(2) . . ? C26 Ga2 C28 114.1(3) . . ? C24 Ga2 C28 114.0(3) . . ? C26 Ga2 N2 102.16(17) . . ? C24 Ga2 N2 105.56(17) . . ? C28 Ga2 N2 101.94(19) . . ? C25 C24 Ga2 110.3(4) . . ? C27 C26 Ga2 113.4(4) . . ? C29 C28 C29' 83.9(12) . . ? C29 C28 Ga2 114.2(8) . . ? C29' C28 Ga2 114.3(11) . . ? C34 Ga3 C36 113.9(2) . . ? C34 Ga3 C38 117.7(2) . . ? C36 Ga3 C38 114.0(2) . . ? C34 Ga3 N3 101.4(2) . . ? C36 Ga3 N3 105.1(2) . . ? C38 Ga3 N3 102.17(16) . . ? C35 C34 Ga3 111.5(4) . . ? C37 C36 Ga3 117.0(4) . . ? C39 C38 Ga3 114.0(4) . . ? C13 N1 C12 110.9(3) . . ? C13 N1 C11 111.0(3) . . ? C12 N1 C11 108.4(3) . . ? C13 N1 Ga1 106.3(2) . . ? C12 N1 Ga1 106.5(2) . . ? C11 N1 Ga1 113.7(3) . . ? N1 C11 C32 113.0(3) . 2 ? N1 C12 C21 114.5(3) . . ? C22 N2 C21 113.9(3) . . ? C22 N2 C23 110.7(3) . . ? C21 N2 C23 107.3(3) . . ? C22 N2 Ga2 107.4(2) . . ? C21 N2 Ga2 112.5(2) . . ? C23 N2 Ga2 104.7(3) . . ? N2 C21 C12 114.4(3) . . ? N2 C22 C31 115.9(3) . . ? C31 N3 C33 109.4(4) . . ? C31 N3 C32 109.7(3) . . ? C33 N3 C32 105.0(3) . . ? C31 N3 Ga3 115.1(3) . . ? C33 N3 Ga3 106.6(3) . . ? C32 N3 Ga3 110.5(3) . . ? N3 C31 C22 113.8(3) . . ? N3 C32 C11 113.0(3) . 2 ? C48 Ga4 C46 114.7(2) . . ? C48 Ga4 C44 114.8(3) . . ? C46 Ga4 C44 116.2(2) . . ? C48 Ga4 N4 102.4(2) . . ? C46 Ga4 N4 105.07(18) . . ? C44 Ga4 N4 100.97(18) . . ? C45 C44 Ga4 110.6(4) . . ? C47 C46 Ga4 115.0(5) . . ? C49' C48 C49 59.9(13) . . ? C49' C48 Ga4 125.1(13) . . ? C49 C48 Ga4 115.6(6) . . ? C56 Ga5 C54 115.2(4) . . ? C56 Ga5 C58 113.3(5) . . ? C54 Ga5 C58 113.6(5) . . ? C55 C54 Ga5 105.4(8) . . ? C57 C56 Ga5 117.3(7) . . ? C59 C58 Ga5 108.1(8) . . ? C58' Ga5' C54' 113.7(8) . . ? C58' Ga5' C56' 114.5(8) . . ? C54' Ga5' C56' 113.3(6) . . ? C58' Ga5' N5 101.5(8) . . ? C54' Ga5' N5 103.1(4) . . ? C56' Ga5' N5 109.3(5) . . ? C55' C54' Ga5' 109.7(8) . . ? C57' C56' Ga5' 103.1(8) . . ? C59' C58' Ga5' 113.9(15) . . ? C68 Ga6 C64 111.1(5) . . ? C68 Ga6 C66 103.3(6) . . ? C64 Ga6 C66 114.1(3) . . ? C68 Ga6 C68' 24.5(6) . . ? C64 Ga6 C68' 112.9(3) . . ? C66 Ga6 C68' 120.7(3) . . ? C68 Ga6 N6 119.5(7) . . ? C64 Ga6 N6 106.1(2) . . ? C66 Ga6 N6 102.66(17) . . ? C68' Ga6 N6 96.9(3) . . ? C65 C64 Ga6 110.6(4) . . ? C67 C66 Ga6 113.2(5) . . ? C69 C68 Ga6 130.8(13) . . ? C69' C68' Ga6 118.8(8) . . ? C42 N4 C41 113.6(3) . . ? C42 N4 C43 107.2(3) . . ? C41 N4 C43 110.5(3) . . ? C42 N4 Ga4 113.5(3) . . ? C41 N4 Ga4 107.2(2) . . ? C43 N4 Ga4 104.5(3) . . ? N4 C41 C62 115.6(3) . 2_676 ? N4 C42 C51 114.7(3) . . ? C52 N5 C53 110.7(4) . . ? C52 N5 C51 108.8(3) . . ? C53 N5 C51 110.5(4) . . ? C52 N5 Ga5' 117.7(4) . . ? C53 N5 Ga5' 99.7(4) . . ? C51 N5 Ga5' 109.1(3) . . ? N5 C51 C42 114.3(3) . . ? N5 C52 C61 113.7(4) . . ? C61 N6 C62 108.7(4) . . ? C61 N6 C63 106.0(3) . . ? C62 N6 C63 108.7(4) . . ? C61 N6 Ga6 111.5(3) . . ? C62 N6 Ga6 115.4(3) . . ? C63 N6 Ga6 105.9(3) . . ? N6 C61 C52 113.3(4) . . ? N6 C62 C41 113.6(3) . 2_676 ? 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 C18 Ga1 C14 C15 30.3(5) . . . . ? C16 Ga1 C14 C15 -106.7(5) . . . . ? N1 Ga1 C14 C15 138.9(4) . . . . ? C14 Ga1 C16 C17 2.2(6) . . . . ? C18 Ga1 C16 C17 -135.1(5) . . . . ? N1 Ga1 C16 C17 114.5(5) . . . . ? C14 Ga1 C18 C19 -88.0(4) . . . . ? C16 Ga1 C18 C19 50.5(4) . . . . ? N1 Ga1 C18 C19 163.2(4) . . . . ? C26 Ga2 C24 C25 -49.7(4) . . . . ? C28 Ga2 C24 C25 86.6(4) . . . . ? N2 Ga2 C24 C25 -162.3(4) . . . . ? C24 Ga2 C26 C27 83.6(5) . . . . ? C28 Ga2 C26 C27 -52.7(5) . . . . ? N2 Ga2 C26 C27 -161.9(4) . . . . ? C26 Ga2 C28 C29 68.8(10) . . . . ? C24 Ga2 C28 C29 -68.7(10) . . . . ? N2 Ga2 C28 C29 178.1(9) . . . . ? C26 Ga2 C28 C29' 163.1(11) . . . . ? C24 Ga2 C28 C29' 25.6(12) . . . . ? N2 Ga2 C28 C29' -87.6(11) . . . . ? C36 Ga3 C34 C35 60.7(6) . . . . ? C38 Ga3 C34 C35 -76.6(5) . . . . ? N3 Ga3 C34 C35 173.0(5) . . . . ? C34 Ga3 C36 C37 16.6(6) . . . . ? C38 Ga3 C36 C37 155.5(5) . . . . ? N3 Ga3 C36 C37 -93.4(5) . . . . ? C34 Ga3 C38 C39 15.3(4) . . . . ? C36 Ga3 C38 C39 -122.0(4) . . . . ? N3 Ga3 C38 C39 125.2(3) . . . . ? C14 Ga1 N1 C13 162.6(3) . . . . ? C18 Ga1 N1 C13 -79.1(3) . . . . ? C16 Ga1 N1 C13 39.8(3) . . . . ? C14 Ga1 N1 C12 -79.0(3) . . . . ? C18 Ga1 N1 C12 39.3(3) . . . . ? C16 Ga1 N1 C12 158.2(3) . . . . ? C14 Ga1 N1 C11 40.2(3) . . . . ? C18 Ga1 N1 C11 158.5(3) . . . . ? C16 Ga1 N1 C11 -82.6(3) . . . . ? C13 N1 C11 C32 -75.0(5) . . . 2 ? C12 N1 C11 C32 163.0(4) . . . 2 ? Ga1 N1 C11 C32 44.8(4) . . . 2 ? C13 N1 C12 C21 -59.6(4) . . . . ? C11 N1 C12 C21 62.4(4) . . . . ? Ga1 N1 C12 C21 -174.9(3) . . . . ? C26 Ga2 N2 C22 -162.7(3) . . . . ? C24 Ga2 N2 C22 -40.3(3) . . . . ? C28 Ga2 N2 C22 79.1(3) . . . . ? C26 Ga2 N2 C21 -36.6(3) . . . . ? C24 Ga2 N2 C21 85.8(3) . . . . ? C28 Ga2 N2 C21 -154.8(3) . . . . ? C26 Ga2 N2 C23 79.5(3) . . . . ? C24 Ga2 N2 C23 -158.0(3) . . . . ? C28 Ga2 N2 C23 -38.7(4) . . . . ? C22 N2 C21 C12 68.2(4) . . . . ? C23 N2 C21 C12 -168.9(4) . . . . ? Ga2 N2 C21 C12 -54.3(4) . . . . ? N1 C12 C21 N2 -179.9(3) . . . . ? C21 N2 C22 C31 60.7(5) . . . . ? C23 N2 C22 C31 -60.3(5) . . . . ? Ga2 N2 C22 C31 -174.0(3) . . . . ? C34 Ga3 N3 C31 161.2(3) . . . . ? C36 Ga3 N3 C31 -80.0(3) . . . . ? C38 Ga3 N3 C31 39.3(3) . . . . ? C34 Ga3 N3 C33 -77.4(3) . . . . ? C36 Ga3 N3 C33 41.5(3) . . . . ? C38 Ga3 N3 C33 160.8(3) . . . . ? C34 Ga3 N3 C32 36.2(3) . . . . ? C36 Ga3 N3 C32 155.0(3) . . . . ? C38 Ga3 N3 C32 -85.7(3) . . . . ? C33 N3 C31 C22 -70.7(4) . . . . ? C32 N3 C31 C22 174.5(3) . . . . ? Ga3 N3 C31 C22 49.2(4) . . . . ? N2 C22 C31 N3 174.2(3) . . . . ? C31 N3 C32 C11 -64.5(5) . . . 2 ? C33 N3 C32 C11 178.0(4) . . . 2 ? Ga3 N3 C32 C11 63.4(4) . . . 2 ? C48 Ga4 C44 C45 -75.7(5) . . . . ? C46 Ga4 C44 C45 62.0(5) . . . . ? N4 Ga4 C44 C45 175.0(5) . . . . ? C48 Ga4 C46 C47 18.4(6) . . . . ? C44 Ga4 C46 C47 -119.4(5) . . . . ? N4 Ga4 C46 C47 129.9(5) . . . . ? C46 Ga4 C48 C49' -77.2(16) . . . . ? C44 Ga4 C48 C49' 61.3(16) . . . . ? N4 Ga4 C48 C49' 169.7(16) . . . . ? C46 Ga4 C48 C49 -147.1(7) . . . . ? C44 Ga4 C48 C49 -8.6(8) . . . . ? N4 Ga4 C48 C49 99.8(7) . . . . ? C56 Ga5 C54 C55 63.2(10) . . . . ? C58 Ga5 C54 C55 -69.9(10) . . . . ? C54 Ga5 C56 C57 38.3(11) . . . . ? C58 Ga5 C56 C57 171.4(9) . . . . ? C56 Ga5 C58 C59 -119.6(8) . . . . ? C54 Ga5 C58 C59 14.3(10) . . . . ? C58' Ga5' C54' C55' -77.6(13) . . . . ? C56' Ga5' C54' C55' 55.4(11) . . . . ? N5 Ga5' C54' C55' 173.5(9) . . . . ? C58' Ga5' C56' C57' 7.0(14) . . . . ? C54' Ga5' C56' C57' -125.6(9) . . . . ? N5 Ga5' C56' C57' 120.1(9) . . . . ? C54' Ga5' C58' C59' 132(2) . . . . ? C56' Ga5' C58' C59' 0(3) . . . . ? N5 Ga5' C58' C59' -118(2) . . . . ? C68 Ga6 C64 C65 67.9(9) . . . . ? C66 Ga6 C64 C65 -48.4(5) . . . . ? C68' Ga6 C64 C65 94.3(5) . . . . ? N6 Ga6 C64 C65 -160.7(4) . . . . ? C68 Ga6 C66 C67 -5.9(8) . . . . ? C64 Ga6 C66 C67 114.8(5) . . . . ? C68' Ga6 C66 C67 -24.7(6) . . . . ? N6 Ga6 C66 C67 -130.8(5) . . . . ? C64 Ga6 C68 C69 7(2) . . . . ? C66 Ga6 C68 C69 129(2) . . . . ? C68' Ga6 C68 C69 -93(2) . . . . ? N6 Ga6 C68 C69 -118(2) . . . . ? C68 Ga6 C68' C69' 65.1(14) . . . . ? C64 Ga6 C68' C69' -25.7(10) . . . . ? C66 Ga6 C68' C69' 114.4(9) . . . . ? N6 Ga6 C68' C69' -136.5(9) . . . . ? C48 Ga4 N4 C42 -159.7(3) . . . . ? C46 Ga4 N4 C42 80.2(3) . . . . ? C44 Ga4 N4 C42 -41.1(3) . . . . ? C48 Ga4 N4 C41 74.0(3) . . . . ? C46 Ga4 N4 C41 -46.1(3) . . . . ? C44 Ga4 N4 C41 -167.4(3) . . . . ? C48 Ga4 N4 C43 -43.3(3) . . . . ? C46 Ga4 N4 C43 -163.4(3) . . . . ? C44 Ga4 N4 C43 75.4(3) . . . . ? C42 N4 C41 C62 60.5(5) . . . 2_676 ? C43 N4 C41 C62 -60.0(5) . . . 2_676 ? Ga4 N4 C41 C62 -173.3(3) . . . 2_676 ? C41 N4 C42 C51 66.1(5) . . . . ? C43 N4 C42 C51 -171.5(4) . . . . ? Ga4 N4 C42 C51 -56.7(4) . . . . ? C58' Ga5' N5 C52 50.4(8) . . . . ? C54' Ga5' N5 C52 168.3(5) . . . . ? C56' Ga5' N5 C52 -71.0(6) . . . . ? C58' Ga5' N5 C53 170.0(7) . . . . ? C54' Ga5' N5 C53 -72.1(5) . . . . ? C56' Ga5' N5 C53 48.7(6) . . . . ? C58' Ga5' N5 C51 -74.2(7) . . . . ? C54' Ga5' N5 C51 43.7(6) . . . . ? C56' Ga5' N5 C51 164.5(5) . . . . ? C52 N5 C51 C42 61.7(5) . . . . ? C53 N5 C51 C42 -60.0(5) . . . . ? Ga5' N5 C51 C42 -168.7(4) . . . . ? N4 C42 C51 N5 -176.8(4) . . . . ? C53 N5 C52 C61 -75.5(5) . . . . ? C51 N5 C52 C61 162.9(4) . . . . ? Ga5' N5 C52 C61 38.2(6) . . . . ? C68 Ga6 N6 C61 -27.7(6) . . . . ? C64 Ga6 N6 C61 -154.2(3) . . . . ? C66 Ga6 N6 C61 85.8(3) . . . . ? C68' Ga6 N6 C61 -37.8(3) . . . . ? C68 Ga6 N6 C62 -152.5(6) . . . . ? C64 Ga6 N6 C62 81.1(3) . . . . ? C66 Ga6 N6 C62 -39.0(3) . . . . ? C68' Ga6 N6 C62 -162.6(3) . . . . ? C68 Ga6 N6 C63 87.1(6) . . . . ? C64 Ga6 N6 C63 -39.3(3) . . . . ? C66 Ga6 N6 C63 -159.4(3) . . . . ? C68' Ga6 N6 C63 77.0(4) . . . . ? C62 N6 C61 C52 66.8(5) . . . . ? C63 N6 C61 C52 -176.4(5) . . . . ? Ga6 N6 C61 C52 -61.6(5) . . . . ? N5 C52 C61 N6 173.3(4) . . . . ? C61 N6 C62 C41 -178.7(4) . . . 2_676 ? C63 N6 C62 C41 66.3(5) . . . 2_676 ? Ga6 N6 C62 C41 -52.5(4) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.777 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.070 data_compound7 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H126 Ga4 N6' _chemical_formula_sum 'C54 H126 Ga4 N6' _chemical_formula_weight 1138.49 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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5918(17) _cell_length_b 22.387(3) _cell_length_c 14.0306(19) _cell_angle_alpha 90.00 _cell_angle_beta 104.297(13) _cell_angle_gamma 90.00 _cell_volume 3223.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 49 _cell_measurement_theta_min 4.738 _cell_measurement_theta_max 14.541 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 1.688 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7976 _exptl_absorpt_correction_T_max 0.9328 _exptl_absorpt_process_details ? ; 12 reflections having 2\q between 5.39 and 36.40 degrees giving 210 \y scans for parameter estimation ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Siemens P4' _diffrn_measurement_method 'profile fitting of \q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10 _diffrn_reflns_number 8915 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7326 _reflns_number_gt 5285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS v2.20 (Siemens, 1996)' _computing_cell_refinement 'XSCANS v2.20 (Siemens, 1996)' _computing_data_reduction 'XSCANS v2.20 (Siemens, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5.03 (Siemens, 1994)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+1.7434P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7326 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.78274(3) 0.058400(14) 0.19158(2) 0.03319(10) Uani 1 1 d . . . C11 C 0.7248(3) 0.00502(14) 0.0724(2) 0.0402(7) Uani 1 1 d . . . H11 H 0.6549 0.0287 0.0286 0.048 Uiso 1 1 calc R . . C111 C 0.6546(3) -0.05273(16) 0.0879(3) 0.0536(9) Uani 1 1 d . . . H11A H 0.5929 -0.0443 0.1271 0.080 Uiso 1 1 calc R . . H11B H 0.7179 -0.0817 0.1219 0.080 Uiso 1 1 calc R . . H11C H 0.6085 -0.0687 0.0246 0.080 Uiso 1 1 calc R . . C112 C 0.8177(3) -0.00827(17) 0.0071(2) 0.0524(9) Uani 1 1 d . . . H11D H 0.8828 -0.0370 0.0397 0.079 Uiso 1 1 calc R . . H11E H 0.8604 0.0284 -0.0047 0.079 Uiso 1 1 calc R . . H11F H 0.7689 -0.0246 -0.0552 0.079 Uiso 1 1 calc R . . C12 C 0.6637(3) 0.05444(15) 0.2836(2) 0.0430(7) Uani 1 1 d . . . H12 H 0.6870 0.0883 0.3299 0.052 Uiso 1 1 calc R . . C121 C 0.6687(4) -0.00215(18) 0.3455(3) 0.0583(9) Uani 1 1 d . . . H12A H 0.7534 -0.0052 0.3916 0.087 Uiso 1 1 calc R . . H12B H 0.6544 -0.0368 0.3028 0.087 Uiso 1 1 calc R . . H12C H 0.6015 -0.0003 0.3815 0.087 Uiso 1 1 calc R . . C122 C 0.5241(3) 0.06501(18) 0.2239(3) 0.0595(10) Uani 1 1 d . . . H12D H 0.5205 0.1014 0.1858 0.089 Uiso 1 1 calc R . . H12E H 0.4672 0.0688 0.2681 0.089 Uiso 1 1 calc R . . H12F H 0.4960 0.0315 0.1798 0.089 Uiso 1 1 calc R . . C13 C 0.8293(3) 0.14259(14) 0.1610(3) 0.0499(8) Uani 1 1 d . . . H13 H 0.9144 0.1516 0.2067 0.060 Uiso 1 1 calc R . . C131 C 0.7335(5) 0.18719(19) 0.1829(7) 0.144(3) Uani 1 1 d . . . H13A H 0.7239 0.1808 0.2492 0.216 Uiso 1 1 calc R . . H13B H 0.6498 0.1821 0.1363 0.216 Uiso 1 1 calc R . . H13C H 0.7653 0.2274 0.1774 0.216 Uiso 1 1 calc R . . C132 C 0.8478(8) 0.1507(2) 0.0567(3) 0.135(3) Uani 1 1 d . . . H13D H 0.7648 0.1456 0.0092 0.203 Uiso 1 1 calc R . . H13E H 0.9091 0.1211 0.0447 0.203 Uiso 1 1 calc R . . H13F H 0.8813 0.1904 0.0502 0.203 Uiso 1 1 calc R . . Ga2 Ga 0.73399(3) 0.187190(14) 0.65460(2) 0.03758(10) Uani 1 1 d . . . C21 C 0.7686(7) 0.27442(18) 0.6453(4) 0.115(2) Uani 1 1 d . . . H21 H 0.8625 0.2688 0.6761 0.138 Uiso 1 1 calc R . . C211 C 0.7549(7) 0.3120(2) 0.7205(5) 0.123(2) Uani 1 1 d . . . H21A H 0.7209 0.2896 0.7679 0.184 Uiso 1 1 calc R . . H21B H 0.6950 0.3441 0.6936 0.184 Uiso 1 1 calc R . . H21C H 0.8390 0.3288 0.7528 0.184 Uiso 1 1 calc R . . C212 C 0.7970(6) 0.2990(2) 0.5538(4) 0.0947(16) Uani 1 1 d . . . H21D H 0.7387 0.2809 0.4968 0.142 Uiso 1 1 calc R . . H21E H 0.8864 0.2900 0.5534 0.142 Uiso 1 1 calc R . . H21F H 0.7843 0.3419 0.5518 0.142 Uiso 1 1 calc R . . C22 C 0.6453(3) 0.14521(18) 0.5286(2) 0.0532(9) Uani 1 1 d . . . H22 H 0.7130 0.1344 0.4940 0.064 Uiso 1 1 calc R . . C221 C 0.5494(6) 0.1864(3) 0.4622(4) 0.131(3) Uani 1 1 d . . . H22A H 0.5961 0.2141 0.4302 0.197 Uiso 1 1 calc R . . H22B H 0.5010 0.2085 0.5009 0.197 Uiso 1 1 calc R . . H22C H 0.4894 0.1630 0.4127 0.197 Uiso 1 1 calc R . . C222 C 0.5735(4) 0.0888(2) 0.5425(3) 0.0766(13) Uani 1 1 d . . . H22D H 0.5099 0.0978 0.5796 0.115 Uiso 1 1 calc R . . H22E H 0.6351 0.0596 0.5780 0.115 Uiso 1 1 calc R . . H22F H 0.5294 0.0727 0.4787 0.115 Uiso 1 1 calc R . . C23 C 0.6603(3) 0.16956(16) 0.7715(2) 0.0486(8) Uani 1 1 d . . . H23 H 0.7140 0.1918 0.8282 0.058 Uiso 1 1 calc R . . C231 C 0.5226(4) 0.1958(2) 0.7504(3) 0.0738(12) Uani 1 1 d . . . H23A H 0.5247 0.2371 0.7300 0.111 Uiso 1 1 calc R . . H23B H 0.4907 0.1939 0.8095 0.111 Uiso 1 1 calc R . . H23C H 0.4653 0.1731 0.6984 0.111 Uiso 1 1 calc R . . C232 C 0.6538(4) 0.10474(18) 0.8047(3) 0.0603(10) Uani 1 1 d . . . H23D H 0.7414 0.0889 0.8271 0.090 Uiso 1 1 calc R . . H23E H 0.6053 0.0810 0.7500 0.090 Uiso 1 1 calc R . . H23F H 0.6107 0.1032 0.8581 0.090 Uiso 1 1 calc R . . C41 C 0.9577(3) -0.04547(12) 0.2708(2) 0.0319(6) Uani 1 1 d . . . H41A H 0.9301 -0.0563 0.2011 0.038 Uiso 1 1 calc R . . H41B H 0.8872 -0.0565 0.3013 0.038 Uiso 1 1 calc R . . N1 N 0.9752(2) 0.02070(10) 0.27807(15) 0.0288(5) Uani 1 1 d . . . C14 C 1.0733(3) 0.04043(14) 0.2253(2) 0.0395(7) Uani 1 1 d . . . H14A H 1.1590 0.0270 0.2609 0.059 Uiso 1 1 calc R . . H14B H 1.0726 0.0837 0.2210 0.059 Uiso 1 1 calc R . . H14C H 1.0522 0.0235 0.1596 0.059 Uiso 1 1 calc R . . C42 C 1.0175(3) 0.03858(12) 0.3830(2) 0.0349(6) Uani 1 1 d . . . H42A H 1.1099 0.0285 0.4077 0.042 Uiso 1 1 calc R . . H42B H 0.9686 0.0150 0.4206 0.042 Uiso 1 1 calc R . . C43 C 0.9996(3) 0.10449(13) 0.4027(2) 0.0367(6) Uani 1 1 d . . . H43A H 1.0385 0.1289 0.3593 0.044 Uiso 1 1 calc R . . H43B H 0.9065 0.1139 0.3887 0.044 Uiso 1 1 calc R . . N3 N 1.0619(2) 0.11845(10) 0.50577(17) 0.0344(5) Uani 1 1 d . . . C34 C 1.2001(3) 0.13067(16) 0.5161(3) 0.0493(8) Uani 1 1 d . . . H34A H 1.2424 0.1376 0.5848 0.074 Uiso 1 1 calc R . . H34B H 1.2094 0.1659 0.4781 0.074 Uiso 1 1 calc R . . H34C H 1.2403 0.0967 0.4923 0.074 Uiso 1 1 calc R . . C44 C 1.0002(3) 0.17029(13) 0.5396(2) 0.0375(7) Uani 1 1 d . . . H44A H 0.9056 0.1672 0.5141 0.045 Uiso 1 1 calc R . . H44B H 1.0289 0.2066 0.5121 0.045 Uiso 1 1 calc R . . C45 C 1.0311(3) 0.17640(13) 0.6515(2) 0.0399(7) Uani 1 1 d . . . H45A H 1.1171 0.1588 0.6794 0.048 Uiso 1 1 calc R . . H45B H 1.0367 0.2190 0.6681 0.048 Uiso 1 1 calc R . . N2 N 0.9351(2) 0.14783(10) 0.69974(16) 0.0318(5) Uani 1 1 d . . . C24 C 0.9800(3) 0.16106(14) 0.8066(2) 0.0421(7) Uani 1 1 d . . . H24A H 0.9682 0.2032 0.8176 0.063 Uiso 1 1 calc R . . H24B H 1.0714 0.1508 0.8296 0.063 Uiso 1 1 calc R . . H24C H 0.9295 0.1377 0.8423 0.063 Uiso 1 1 calc R . . C46 C 0.9218(3) 0.08230(12) 0.6814(2) 0.0307(6) Uani 1 1 d . . . H46A H 0.9009 0.0755 0.6102 0.037 Uiso 1 1 calc R . . H46B H 0.8482 0.0677 0.7055 0.037 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 0.03294(17) 0.03524(17) 0.02923(16) 0.00202(13) 0.00356(12) 0.00392(13) C11 0.0369(16) 0.0516(18) 0.0292(15) -0.0007(13) 0.0025(12) 0.0053(14) C111 0.0445(19) 0.063(2) 0.051(2) -0.0197(17) 0.0080(16) -0.0101(16) C112 0.053(2) 0.072(2) 0.0324(16) -0.0022(16) 0.0107(15) 0.0044(18) C12 0.0358(16) 0.0523(18) 0.0399(17) -0.0097(14) 0.0076(13) 0.0040(14) C121 0.047(2) 0.081(3) 0.051(2) 0.0061(19) 0.0212(17) 0.0051(19) C122 0.0390(18) 0.072(3) 0.066(2) -0.003(2) 0.0098(17) 0.0079(17) C13 0.0490(19) 0.0407(17) 0.0502(19) 0.0119(15) -0.0067(15) -0.0021(15) C131 0.081(4) 0.042(2) 0.322(11) 0.046(4) 0.075(5) 0.024(2) C132 0.253(8) 0.084(4) 0.047(3) 0.024(3) -0.006(4) -0.069(5) Ga2 0.0425(2) 0.03565(18) 0.03393(18) 0.00342(13) 0.00814(14) 0.00864(14) C21 0.225(7) 0.032(2) 0.121(5) 0.013(2) 0.108(5) 0.017(3) C211 0.166(6) 0.052(3) 0.156(6) -0.044(3) 0.052(5) -0.033(3) C212 0.119(4) 0.056(3) 0.101(4) 0.030(3) 0.012(3) -0.011(3) C22 0.0376(18) 0.082(3) 0.0357(17) -0.0027(17) 0.0015(14) 0.0082(17) C221 0.127(5) 0.122(5) 0.095(4) 0.034(4) -0.067(4) -0.005(4) C222 0.069(3) 0.088(3) 0.065(3) -0.027(2) 0.000(2) -0.015(2) C23 0.0473(19) 0.060(2) 0.0386(17) -0.0018(15) 0.0111(15) 0.0017(16) C231 0.052(2) 0.094(3) 0.082(3) 0.005(3) 0.030(2) 0.007(2) C232 0.067(2) 0.070(2) 0.043(2) 0.0055(18) 0.0133(18) -0.013(2) C41 0.0308(14) 0.0336(14) 0.0288(14) 0.0009(11) 0.0024(11) 0.0016(11) N1 0.0301(12) 0.0310(11) 0.0237(11) 0.0025(9) 0.0036(9) 0.0007(9) C14 0.0368(16) 0.0439(16) 0.0393(16) 0.0074(13) 0.0126(13) 0.0007(13) C42 0.0393(16) 0.0357(14) 0.0254(13) 0.0015(11) -0.0003(12) -0.0030(12) C43 0.0407(16) 0.0365(15) 0.0289(14) -0.0009(12) 0.0010(12) -0.0003(13) N3 0.0317(12) 0.0368(13) 0.0319(12) -0.0044(10) 0.0024(10) -0.0027(10) C34 0.0352(17) 0.064(2) 0.0466(19) -0.0090(16) 0.0053(14) -0.0077(15) C44 0.0396(16) 0.0345(15) 0.0367(16) 0.0000(12) 0.0060(13) -0.0053(12) C45 0.0460(17) 0.0363(16) 0.0359(16) -0.0085(13) 0.0071(13) -0.0093(13) N2 0.0377(13) 0.0298(12) 0.0258(11) -0.0038(9) 0.0037(10) -0.0013(10) C24 0.0473(18) 0.0421(16) 0.0321(15) -0.0091(13) 0.0008(13) -0.0013(14) C46 0.0310(14) 0.0294(13) 0.0297(14) -0.0007(11) 0.0038(11) -0.0005(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 C12 2.017(3) . ? Ga1 C13 2.021(3) . ? Ga1 C11 2.023(3) . ? Ga1 N1 2.263(2) . ? C11 C112 1.531(4) . ? C11 C111 1.533(5) . ? C12 C122 1.527(5) . ? C12 C121 1.530(5) . ? C13 C131 1.508(6) . ? C13 C132 1.535(6) . ? Ga2 C21 1.997(4) . ? Ga2 C22 2.018(3) . ? Ga2 C23 2.022(3) . ? Ga2 N2 2.247(2) . ? C21 C211 1.386(7) . ? C21 C212 1.494(6) . ? C22 C221 1.511(6) . ? C22 C222 1.512(6) . ? C23 C232 1.531(5) . ? C23 C231 1.532(5) . ? C41 N1 1.493(3) . ? C41 C46 1.528(4) 3_756 ? N1 C14 1.484(4) . ? N1 C42 1.485(3) . ? C42 C43 1.521(4) . ? C43 N3 1.468(4) . ? N3 C34 1.460(4) . ? N3 C44 1.468(4) . ? C44 C45 1.529(4) . ? C45 N2 1.497(4) . ? N2 C24 1.487(3) . ? N2 C46 1.490(3) . ? C46 C41 1.528(4) 3_756 ? 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 C12 Ga1 C13 113.63(14) . . ? C12 Ga1 C11 113.12(13) . . ? C13 Ga1 C11 114.55(13) . . ? C12 Ga1 N1 105.27(11) . . ? C13 Ga1 N1 103.12(11) . . ? C11 Ga1 N1 105.80(10) . . ? C112 C11 C111 109.1(3) . . ? C112 C11 Ga1 120.0(2) . . ? C111 C11 Ga1 116.1(2) . . ? C122 C12 C121 109.5(3) . . ? C122 C12 Ga1 108.4(2) . . ? C121 C12 Ga1 117.4(2) . . ? C131 C13 C132 111.6(4) . . ? C131 C13 Ga1 111.2(3) . . ? C132 C13 Ga1 114.1(3) . . ? C21 Ga2 C22 116.8(2) . . ? C21 Ga2 C23 110.96(17) . . ? C22 Ga2 C23 115.50(15) . . ? C21 Ga2 N2 103.0(2) . . ? C22 Ga2 N2 105.56(11) . . ? C23 Ga2 N2 102.94(11) . . ? C211 C21 C212 120.8(4) . . ? C211 C21 Ga2 119.3(4) . . ? C212 C21 Ga2 119.7(3) . . ? C221 C22 C222 107.9(4) . . ? C221 C22 Ga2 110.7(3) . . ? C222 C22 Ga2 114.6(3) . . ? C232 C23 C231 108.1(3) . . ? C232 C23 Ga2 119.1(2) . . ? C231 C23 Ga2 107.9(2) . . ? N1 C41 C46 115.4(2) . 3_756 ? C14 N1 C42 109.7(2) . . ? C14 N1 C41 110.6(2) . . ? C42 N1 C41 109.7(2) . . ? C14 N1 Ga1 105.69(16) . . ? C42 N1 Ga1 116.29(17) . . ? C41 N1 Ga1 104.68(15) . . ? N1 C42 C43 114.9(2) . . ? N3 C43 C42 109.8(2) . . ? C34 N3 C44 109.6(2) . . ? C34 N3 C43 109.5(2) . . ? C44 N3 C43 111.1(2) . . ? N3 C44 C45 113.8(2) . . ? N2 C45 C44 115.4(2) . . ? C24 N2 C46 111.3(2) . . ? C24 N2 C45 106.7(2) . . ? C46 N2 C45 112.8(2) . . ? C24 N2 Ga2 104.53(17) . . ? C46 N2 Ga2 107.17(16) . . ? C45 N2 Ga2 114.07(18) . . ? N2 C46 C41 115.0(2) . 3_756 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.432 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.069