Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_eva13 _database_code_CSD 154913 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Schier, Annette' 'Schmidbaur, H.' 'Schmidt, Eva Susanne' _publ_contact_author_name 'Prof H Schmidbaur' _publ_contact_author_address ; Prof H Schmidbaur Lehrstuhl fur Anorganische und Anal Technischen Universitat Munchen Lichtenbergstrase 4 Garching D-85747 GERMANY ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H72 Ga2 K2 N8' _chemical_formula_weight 786.62 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' 'K' 'K' 0.2009 0.2494 '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 10.3925(2) _cell_length_b 10.7648(2) _cell_length_c 10.9534(3) _cell_angle_alpha 101.728(1) _cell_angle_beta 92.051(1) _cell_angle_gamma 114.450(1) _cell_volume 1082.28(4) _cell_formula_units_Z 1 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 1.466 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6279 _exptl_absorpt_correction_T_max 0.7580 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius DIP2020' _diffrn_measurement_method 'phi-rotation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4132 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 26.43 _reflns_number_total 4132 _reflns_number_gt 3906 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement SCALEPACK _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELTXT-PLUS _computing_publication_material SHELXL-97 _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. Disorder of C5 and C6 in the ethylenediamine; the two atoms were refined in split positions with SOF 50:50. ; _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^)+(0.0284P)^2^+0.7759P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4132 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga Ga 0.68979(2) 0.54741(2) 0.113921(19) 0.02561(8) Uani 1 1 d . . . K K 0.38524(5) 0.57426(4) 0.20779(4) 0.02696(11) Uani 1 1 d . . . N1 N 0.71717(18) 0.71908(17) 0.24144(15) 0.0255(3) Uani 1 1 d . A . N2 N 0.60598(18) 0.45580(17) 0.25015(15) 0.0258(3) Uani 1 1 d . . . N3 N 0.2331(2) 0.74728(19) 0.2665(2) 0.0406(5) Uani 1 1 d . . . N4 N 0.0990(2) 0.4319(2) 0.2627(2) 0.0381(4) Uani 1 1 d . . . C1 C 0.6759(2) 0.6895(2) 0.35538(18) 0.0286(4) Uani 1 1 d . . . H1A H 0.6881 0.7620 0.4270 0.034 Uiso 1 1 calc R A . C2 C 0.6177(2) 0.5531(2) 0.35975(18) 0.0286(4) Uani 1 1 d . A . H2A H 0.5862 0.5250 0.4343 0.034 Uiso 1 1 calc R . . C3 C 0.7810(2) 0.8673(2) 0.2350(2) 0.0292(4) Uani 1 1 d . . . C4 C 0.5377(2) 0.3063(2) 0.25187(19) 0.0290(4) Uani 1 1 d . A . C5 C 0.0942(5) 0.6631(5) 0.3156(5) 0.0269(10) Uani 0.50 1 d P A 1 H5A H 0.0291 0.7091 0.3151 0.032 Uiso 0.50 1 calc PR A 1 H5B H 0.1152 0.6585 0.4031 0.032 Uiso 0.50 1 calc PR A 1 C6 C 0.0219(5) 0.5097(5) 0.2265(5) 0.0260(10) Uani 0.50 1 d P A 1 H6A H -0.0801 0.4625 0.2369 0.031 Uiso 0.50 1 calc PR A 1 H6B H 0.0284 0.5140 0.1374 0.031 Uiso 0.50 1 calc PR A 1 C5A C 0.0810(6) 0.6498(7) 0.2395(9) 0.0599(18) Uani 0.50 1 d P A 2 H5AA H 0.0248 0.7038 0.2638 0.072 Uiso 0.50 1 calc PR A 2 H5AB H 0.0565 0.6091 0.1476 0.072 Uiso 0.50 1 calc PR A 2 C6A C 0.0410(7) 0.5436(7) 0.2984(8) 0.0529(16) Uani 0.50 1 d P A 2 H6AA H -0.0644 0.4942 0.2837 0.063 Uiso 0.50 1 calc PR A 2 H6AB H 0.0691 0.5857 0.3899 0.063 Uiso 0.50 1 calc PR A 2 C31 C 0.9098(3) 0.9563(2) 0.3373(2) 0.0408(5) Uani 1 1 d . A . H31A H 0.8790 0.9519 0.4204 0.061 Uiso 1 1 calc R . . H31B H 0.9508 1.0541 0.3302 0.061 Uiso 1 1 calc R . . H31C H 0.9818 0.9197 0.3264 0.061 Uiso 1 1 calc R . . C32 C 0.6705(3) 0.9275(3) 0.2505(2) 0.0424(6) Uani 1 1 d . A . H32A H 0.5880 0.8710 0.1855 0.064 Uiso 1 1 calc R . . H32B H 0.7133 1.0248 0.2420 0.064 Uiso 1 1 calc R . . H32C H 0.6397 0.9252 0.3339 0.064 Uiso 1 1 calc R . . C33 C 0.8319(3) 0.8766(2) 0.1071(2) 0.0407(5) Uani 1 1 d . A . H33A H 0.7510 0.8205 0.0405 0.061 Uiso 1 1 calc R . . H33B H 0.9042 0.8403 0.0972 0.061 Uiso 1 1 calc R . . H33C H 0.8733 0.9748 0.1013 0.061 Uiso 1 1 calc R . . C41 C 0.6084(3) 0.2768(2) 0.3609(2) 0.0390(5) Uani 1 1 d . . . H41A H 0.5992 0.3306 0.4410 0.058 Uiso 1 1 calc R . . H41B H 0.7097 0.3046 0.3530 0.058 Uiso 1 1 calc R . . H41C H 0.5616 0.1762 0.3584 0.058 Uiso 1 1 calc R . . C42 C 0.3787(2) 0.2595(2) 0.2635(2) 0.0376(5) Uani 1 1 d . . . H42A H 0.3328 0.2778 0.1939 0.056 Uiso 1 1 calc R A . H42B H 0.3680 0.3120 0.3437 0.056 Uiso 1 1 calc R . . H42C H 0.3336 0.1587 0.2603 0.056 Uiso 1 1 calc R . . C43 C 0.5530(3) 0.2206(2) 0.1284(2) 0.0385(5) Uani 1 1 d . . . H43A H 0.5078 0.2377 0.0576 0.058 Uiso 1 1 calc R A . H43B H 0.5066 0.1204 0.1274 0.058 Uiso 1 1 calc R . . H43C H 0.6544 0.2487 0.1211 0.058 Uiso 1 1 calc R . . C51 C 0.2927(3) 0.8688(3) 0.3711(2) 0.0506(7) Uani 1 1 d . A . H51A H 0.2297 0.9164 0.3792 0.076 Uiso 1 1 calc R . . H51B H 0.3869 0.9335 0.3568 0.076 Uiso 1 1 calc R . . H51C H 0.3018 0.8392 0.4486 0.076 Uiso 1 1 calc R . . C52 C 0.2347(4) 0.7935(4) 0.1522(3) 0.0696(10) Uani 1 1 d . A . H52A H 0.1855 0.8546 0.1586 0.104 Uiso 1 1 calc R . . H52B H 0.1860 0.7117 0.0812 0.104 Uiso 1 1 calc R . . H52C H 0.3336 0.8458 0.1388 0.104 Uiso 1 1 calc R . . C61 C 0.0846(3) 0.3875(3) 0.3797(2) 0.0478(6) Uani 1 1 d . A . H61A H -0.0168 0.3408 0.3886 0.072 Uiso 1 1 calc R . . H61B H 0.1330 0.4697 0.4503 0.072 Uiso 1 1 calc R . . H61C H 0.1277 0.3219 0.3793 0.072 Uiso 1 1 calc R . . C62 C 0.0333(3) 0.3073(3) 0.1597(3) 0.0595(8) Uani 1 1 d . A . H62A H -0.0657 0.2523 0.1714 0.089 Uiso 1 1 calc R . . H62B H 0.0863 0.2502 0.1583 0.089 Uiso 1 1 calc R . . H62C H 0.0347 0.3354 0.0799 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga 0.02548(14) 0.02985(13) 0.02177(12) 0.00290(9) 0.00403(9) 0.01360(10) K 0.0235(2) 0.0306(2) 0.0284(2) 0.00543(17) 0.00487(17) 0.01387(18) N1 0.0258(9) 0.0256(8) 0.0242(8) 0.0037(6) 0.0013(7) 0.0113(7) N2 0.0282(9) 0.0267(8) 0.0235(8) 0.0037(7) 0.0016(7) 0.0141(7) N3 0.0274(10) 0.0273(10) 0.0664(14) 0.0080(9) 0.0047(9) 0.0128(8) N4 0.0270(10) 0.0354(10) 0.0574(12) 0.0203(9) 0.0124(9) 0.0142(8) C1 0.0327(11) 0.0329(11) 0.0191(9) 0.0004(8) 0.0009(8) 0.0158(9) C2 0.0330(11) 0.0352(11) 0.0195(9) 0.0054(8) 0.0028(8) 0.0170(9) C3 0.0271(11) 0.0281(10) 0.0324(11) 0.0047(8) -0.0005(8) 0.0133(8) C4 0.0269(11) 0.0283(10) 0.0330(11) 0.0076(8) 0.0029(8) 0.0129(8) C5 0.029(3) 0.027(2) 0.028(2) 0.007(2) 0.009(2) 0.0149(19) C6 0.017(2) 0.028(2) 0.029(2) 0.002(2) -0.0017(19) 0.0081(17) C5A 0.023(3) 0.044(3) 0.111(6) 0.015(4) 0.004(4) 0.015(2) C6A 0.032(3) 0.053(4) 0.087(5) 0.028(4) 0.028(4) 0.025(3) C31 0.0332(12) 0.0315(12) 0.0485(14) 0.0005(10) -0.0063(10) 0.0103(9) C32 0.0402(14) 0.0398(13) 0.0555(15) 0.0137(11) 0.0053(11) 0.0245(11) C33 0.0432(14) 0.0363(12) 0.0405(13) 0.0138(10) 0.0097(10) 0.0127(10) C41 0.0380(13) 0.0352(12) 0.0463(13) 0.0154(10) -0.0014(10) 0.0163(10) C42 0.0275(11) 0.0354(12) 0.0465(13) 0.0087(10) 0.0030(10) 0.0109(9) C43 0.0399(13) 0.0301(11) 0.0432(13) 0.0017(10) 0.0064(10) 0.0160(10) C51 0.0613(18) 0.0562(16) 0.0457(14) 0.0096(12) 0.0053(12) 0.0376(14) C52 0.089(3) 0.092(2) 0.0467(16) -0.0016(16) -0.0067(16) 0.066(2) C61 0.0361(14) 0.0579(16) 0.0403(13) 0.0066(12) 0.0079(11) 0.0136(12) C62 0.0339(14) 0.085(2) 0.0411(14) 0.0140(14) 0.0044(11) 0.0079(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga N1 1.9834(16) . ? Ga N2 1.9844(17) . ? Ga K 3.4384(5) 2_665 ? Ga K 3.4681(5) . ? K N4 2.8788(19) . ? K N3 2.899(2) . ? K C2 2.996(2) . ? K C1 3.002(2) . ? K N1 3.1128(17) . ? K N2 3.1129(17) . ? K Ga 3.4384(5) 2_665 ? K C52 3.459(3) . ? K C62 3.530(3) . ? K C42 3.537(2) . ? N1 C1 1.389(3) . ? N1 C3 1.471(3) . ? N2 C2 1.388(3) . ? N2 C4 1.470(3) . ? N3 C52 1.436(4) . ? N3 C51 1.442(3) . ? N3 C5A 1.468(6) . ? N3 C5 1.539(5) . ? N4 C61 1.448(3) . ? N4 C62 1.452(4) . ? N4 C6 1.472(5) . ? N4 C6A 1.545(6) . ? C1 C2 1.349(3) . ? C1 H1A 0.9500 . ? C2 H2A 0.9500 . ? C3 C33 1.522(3) . ? C3 C32 1.533(3) . ? C3 C31 1.536(3) . ? C4 C43 1.528(3) . ? C4 C42 1.534(3) . ? C4 C41 1.534(3) . ? C5 C6 1.584(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5A C6A 1.349(9) . ? C5A H5AA 0.9900 . ? C5A H5AB 0.9900 . ? C6A H6AA 0.9900 . ? C6A H6AB 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ga N2 82.05(7) . . ? N1 Ga K 137.69(5) . 2_665 ? N2 Ga K 130.76(5) . 2_665 ? N1 Ga K 62.88(5) . . ? N2 Ga K 62.88(5) . . ? K Ga K 104.802(10) 2_665 . ? N4 K N3 64.44(5) . . ? N4 K C2 116.98(6) . . ? N3 K C2 131.41(6) . . ? N4 K C1 134.09(6) . . ? N3 K C1 115.13(6) . . ? C2 K C1 25.99(6) . . ? N4 K N1 160.22(5) . . ? N3 K N1 118.85(5) . . ? C2 K N1 44.87(5) . . ? C1 K N1 26.18(5) . . ? N4 K N2 119.45(5) . . ? N3 K N2 157.58(5) . . ? C2 K N2 26.17(5) . . ? C1 K N2 44.77(5) . . ? N1 K N2 49.46(4) . . ? N4 K Ga 96.94(4) . 2_665 ? N3 K Ga 103.95(5) . 2_665 ? C2 K Ga 122.81(4) . 2_665 ? C1 K Ga 124.82(4) . 2_665 ? N1 K Ga 100.75(3) . 2_665 ? N2 K Ga 97.56(3) . 2_665 ? N4 K C52 77.96(8) . . ? N3 K C52 24.11(7) . . ? C2 K C52 145.28(7) . . ? C1 K C52 121.31(7) . . ? N1 K C52 112.91(8) . . ? N2 K C52 162.23(8) . . ? Ga K C52 82.74(5) 2_665 . ? N4 K Ga 147.30(4) . . ? N3 K Ga 148.10(4) . . ? C2 K Ga 51.01(4) . . ? C1 K Ga 50.95(4) . . ? N1 K Ga 34.55(3) . . ? N2 K Ga 34.57(3) . . ? Ga K Ga 75.198(10) 2_665 . ? C52 K Ga 130.68(7) . . ? N4 K C62 23.50(6) . . ? N3 K C62 80.65(7) . . ? C2 K C62 120.20(7) . . ? C1 K C62 144.72(7) . . ? N1 K C62 160.13(7) . . ? N2 K C62 110.99(7) . . ? Ga K C62 76.24(5) 2_665 . ? C52 K C62 86.42(9) . . ? Ga K C62 128.29(6) . . ? N4 K C42 77.43(5) . . ? N3 K C42 138.91(6) . . ? C2 K C42 54.67(5) . . ? C1 K C42 80.54(5) . . ? N1 K C42 92.21(5) . . ? N2 K C42 42.96(5) . . ? Ga K C42 94.93(4) 2_665 . ? C52 K C42 154.80(8) . . ? Ga K C42 71.84(4) . . ? C62 K C42 68.75(7) . . ? C1 N1 C3 117.70(16) . . ? C1 N1 Ga 111.93(13) . . ? C3 N1 Ga 130.24(13) . . ? C1 N1 K 72.44(11) . . ? C3 N1 K 115.13(12) . . ? Ga N1 K 82.57(5) . . ? C2 N2 C4 117.49(17) . . ? C2 N2 Ga 112.03(13) . . ? C4 N2 Ga 130.48(13) . . ? C2 N2 K 72.22(11) . . ? C4 N2 K 112.53(12) . . ? Ga N2 K 82.56(5) . . ? C52 N3 C51 108.8(2) . . ? C52 N3 C5A 94.2(4) . . ? C51 N3 C5A 123.6(4) . . ? C52 N3 C5 122.8(3) . . ? C51 N3 C5 98.6(3) . . ? C5A N3 C5 31.3(3) . . ? C52 N3 K 100.34(16) . . ? C51 N3 K 118.90(15) . . ? C5A N3 K 105.7(3) . . ? C5 N3 K 108.8(2) . . ? C61 N4 C62 108.1(2) . . ? C61 N4 C6 121.6(3) . . ? C62 N4 C6 97.9(3) . . ? C61 N4 C6A 97.0(3) . . ? C62 N4 C6A 124.4(4) . . ? C6 N4 C6A 29.8(3) . . ? C61 N4 K 116.53(15) . . ? C62 N4 K 104.28(15) . . ? C6 N4 K 105.5(2) . . ? C6A N4 K 107.2(2) . . ? C2 C1 N1 116.96(18) . . ? C2 C1 K 76.79(12) . . ? N1 C1 K 81.37(11) . . ? C2 C1 H1A 121.5 . . ? N1 C1 H1A 121.5 . . ? K C1 H1A 111.2 . . ? C1 C2 N2 116.81(18) . . ? C1 C2 K 77.23(12) . . ? N2 C2 K 81.60(11) . . ? C1 C2 H2A 121.6 . . ? N2 C2 H2A 121.6 . . ? K C2 H2A 110.5 . . ? N1 C3 C33 108.81(17) . . ? N1 C3 C32 110.47(18) . . ? C33 C3 C32 108.89(19) . . ? N1 C3 C31 111.20(17) . . ? C33 C3 C31 108.28(19) . . ? C32 C3 C31 109.14(19) . . ? N2 C4 C43 108.38(17) . . ? N2 C4 C42 110.38(17) . . ? C43 C4 C42 109.00(18) . . ? N2 C4 C41 111.61(17) . . ? C43 C4 C41 108.35(18) . . ? C42 C4 C41 109.07(18) . . ? N3 C5 C6 108.0(3) . . ? N3 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? N3 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N4 C6 C5 107.1(3) . . ? N4 C6 H6A 110.3 . . ? C5 C6 H6A 110.3 . . ? N4 C6 H6B 110.3 . . ? C5 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? C6A C5A N3 115.1(6) . . ? C6A C5A H5AA 108.5 . . ? N3 C5A H5AA 108.5 . . ? C6A C5A H5AB 108.5 . . ? N3 C5A H5AB 108.5 . . ? H5AA C5A H5AB 107.5 . . ? C5A C6A N4 118.6(6) . . ? C5A C6A H6AA 107.7 . . ? N4 C6A H6AA 107.7 . . ? C5A C6A H6AB 107.7 . . ? N4 C6A H6AB 107.7 . . ? H6AA C6A H6AB 107.1 . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C3 C32 H32A 109.5 . . ? C3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C3 C33 H33A 109.5 . . ? C3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 K 92.61(12) . . ? C4 C42 H42A 109.5 . . ? K C42 H42A 48.3 . . ? C4 C42 H42B 109.5 . . ? K C42 H42B 73.7 . . ? H42A C42 H42B 109.5 . . ? C4 C42 H42C 109.5 . . ? K C42 H42C 154.2 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C4 C43 H43A 109.5 . . ? C4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N3 C51 H51A 109.5 . . ? N3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N3 C52 K 55.55(13) . . ? N3 C52 H52A 109.5 . . ? K C52 H52A 165.0 . . ? N3 C52 H52B 109.5 . . ? K C52 H52B 78.4 . . ? H52A C52 H52B 109.5 . . ? N3 C52 H52C 109.5 . . ? K C52 H52C 78.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N4 C61 H61A 109.5 . . ? N4 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N4 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N4 C62 K 52.22(11) . . ? N4 C62 H62A 109.5 . . ? K C62 H62A 161.7 . . ? N4 C62 H62B 109.5 . . ? K C62 H62B 80.3 . . ? H62A C62 H62B 109.5 . . ? N4 C62 H62C 109.5 . . ? K C62 H62C 80.3 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ga K N4 -144.00(10) . . . . ? N2 Ga K N4 -48.96(10) . . . . ? K Ga K N4 79.61(8) 2_665 . . . ? N1 Ga K N3 43.68(10) . . . . ? N2 Ga K N3 138.72(10) . . . . ? K Ga K N3 -92.72(9) 2_665 . . . ? N1 Ga K C2 -64.39(7) . . . . ? N2 Ga K C2 30.65(7) . . . . ? K Ga K C2 159.22(5) 2_665 . . . ? N1 Ga K C1 -30.75(7) . . . . ? N2 Ga K C1 64.30(7) . . . . ? K Ga K C1 -167.14(5) 2_665 . . . ? N2 Ga K N1 95.04(7) . . . . ? K Ga K N1 -136.39(5) 2_665 . . . ? N1 Ga K N2 -95.04(7) . . . . ? K Ga K N2 128.57(5) 2_665 . . . ? N1 Ga K Ga 136.39(5) . . . 2_665 ? N2 Ga K Ga -128.57(5) . . . 2_665 ? K Ga K Ga 0.0 2_665 . . 2_665 ? N1 Ga K C52 69.93(9) . . . . ? N2 Ga K C52 164.97(9) . . . . ? K Ga K C52 -66.46(7) 2_665 . . . ? N1 Ga K C62 -165.08(8) . . . . ? N2 Ga K C62 -70.04(8) . . . . ? K Ga K C62 58.53(6) 2_665 . . . ? N1 Ga K C42 -123.22(7) . . . . ? N2 Ga K C42 -28.18(7) . . . . ? K Ga K C42 100.38(4) 2_665 . . . ? N2 Ga N1 C1 4.11(14) . . . . ? K Ga N1 C1 149.81(11) 2_665 . . . ? K Ga N1 C1 67.64(13) . . . . ? N2 Ga N1 C3 179.67(17) . . . . ? K Ga N1 C3 -34.6(2) 2_665 . . . ? K Ga N1 C3 -116.80(17) . . . . ? N2 Ga N1 K -63.53(5) . . . . ? K Ga N1 K 82.16(7) 2_665 . . . ? N4 K N1 C1 -5.6(2) . . . . ? N3 K N1 C1 88.76(12) . . . . ? C2 K N1 C1 -32.37(11) . . . . ? N2 K N1 C1 -67.82(11) . . . . ? Ga K N1 C1 -158.61(11) 2_665 . . . ? C52 K N1 C1 114.79(12) . . . . ? Ga K N1 C1 -115.86(13) . . . . ? C62 K N1 C1 -79.4(2) . . . . ? C42 K N1 C1 -63.16(12) . . . . ? N4 K N1 C3 -118.55(18) . . . . ? N3 K N1 C3 -24.20(15) . . . . ? C2 K N1 C3 -145.34(15) . . . . ? C1 K N1 C3 -112.96(18) . . . . ? N2 K N1 C3 179.22(15) . . . . ? Ga K N1 C3 88.43(13) 2_665 . . . ? C52 K N1 C3 1.83(14) . . . . ? Ga K N1 C3 131.18(15) . . . . ? C62 K N1 C3 167.66(16) . . . . ? C42 K N1 C3 -176.12(13) . . . . ? N4 K N1 Ga 110.27(15) . . . . ? N3 K N1 Ga -155.38(6) . . . . ? C2 K N1 Ga 83.49(7) . . . . ? C1 K N1 Ga 115.86(13) . . . . ? N2 K N1 Ga 48.05(5) . . . . ? Ga K N1 Ga -42.75(5) 2_665 . . . ? C52 K N1 Ga -129.34(7) . . . . ? C62 K N1 Ga 36.48(18) . . . . ? C42 K N1 Ga 52.70(6) . . . . ? N1 Ga N2 C2 -3.83(14) . . . . ? K Ga N2 C2 -153.77(11) 2_665 . . . ? K Ga N2 C2 -67.36(13) . . . . ? N1 Ga N2 C4 176.89(18) . . . . ? K Ga N2 C4 26.9(2) 2_665 . . . ? K Ga N2 C4 113.35(17) . . . . ? N1 Ga N2 K 63.53(5) . . . . ? K Ga N2 K -86.41(5) 2_665 . . . ? N4 K N2 C2 -91.85(13) . . . . ? N3 K N2 C2 2.1(2) . . . . ? C1 K N2 C2 32.57(12) . . . . ? N1 K N2 C2 68.03(12) . . . . ? Ga K N2 C2 165.74(11) 2_665 . . . ? C52 K N2 C2 75.9(2) . . . . ? Ga K N2 C2 116.05(13) . . . . ? C62 K N2 C2 -116.16(12) . . . . ? C42 K N2 C2 -105.14(14) . . . . ? N4 K N2 C4 21.22(14) . . . . ? N3 K N2 C4 115.19(16) . . . . ? C2 K N2 C4 113.07(18) . . . . ? C1 K N2 C4 145.64(15) . . . . ? N1 K N2 C4 -178.90(14) . . . . ? Ga K N2 C4 -81.19(12) 2_665 . . . ? C52 K N2 C4 -171.00(19) . . . . ? Ga K N2 C4 -130.88(14) . . . . ? C62 K N2 C4 -3.09(14) . . . . ? C42 K N2 C4 7.93(12) . . . . ? N4 K N2 Ga 152.10(6) . . . . ? N3 K N2 Ga -113.92(13) . . . . ? C2 K N2 Ga -116.05(13) . . . . ? C1 K N2 Ga -83.47(8) . . . . ? N1 K N2 Ga -48.02(5) . . . . ? Ga K N2 Ga 49.69(5) 2_665 . . . ? C52 K N2 Ga -40.1(2) . . . . ? C62 K N2 Ga 127.80(6) . . . . ? C42 K N2 Ga 138.81(9) . . . . ? N4 K N3 C52 -120.20(19) . . . . ? C2 K N3 C52 135.40(18) . . . . ? C1 K N3 C52 110.93(18) . . . . ? N1 K N3 C52 81.78(18) . . . . ? N2 K N3 C52 134.2(2) . . . . ? Ga K N3 C52 -29.10(18) 2_665 . . . ? Ga K N3 C52 55.2(2) . . . . ? C62 K N3 C52 -102.28(18) . . . . ? C42 K N3 C52 -143.91(18) . . . . ? N4 K N3 C51 121.49(19) . . . . ? C2 K N3 C51 17.1(2) . . . . ? C1 K N3 C51 -7.4(2) . . . . ? N1 K N3 C51 -36.5(2) . . . . ? N2 K N3 C51 15.8(3) . . . . ? Ga K N3 C51 -147.41(17) 2_665 . . . ? C52 K N3 C51 -118.3(3) . . . . ? Ga K N3 C51 -63.1(2) . . . . ? C62 K N3 C51 139.41(19) . . . . ? C42 K N3 C51 97.78(19) . . . . ? N4 K N3 C5A -22.8(4) . . . . ? C2 K N3 C5A -127.2(4) . . . . ? C1 K N3 C5A -151.7(4) . . . . ? N1 K N3 C5A 179.2(4) . . . . ? N2 K N3 C5A -128.5(4) . . . . ? Ga K N3 C5A 68.3(4) 2_665 . . . ? C52 K N3 C5A 97.4(4) . . . . ? Ga K N3 C5A 152.6(4) . . . . ? C62 K N3 C5A -4.9(4) . . . . ? C42 K N3 C5A -46.5(4) . . . . ? N4 K N3 C5 9.8(2) . . . . ? C2 K N3 C5 -94.6(2) . . . . ? C1 K N3 C5 -119.0(2) . . . . ? N1 K N3 C5 -148.2(2) . . . . ? N2 K N3 C5 -95.8(2) . . . . ? Ga K N3 C5 100.9(2) 2_665 . . . ? C52 K N3 C5 130.0(3) . . . . ? Ga K N3 C5 -174.7(2) . . . . ? C62 K N3 C5 27.8(2) . . . . ? C42 K N3 C5 -13.9(3) . . . . ? N3 K N4 C61 -110.46(18) . . . . ? C2 K N4 C61 14.94(19) . . . . ? C1 K N4 C61 -9.4(2) . . . . ? N1 K N4 C61 -6.0(3) . . . . ? N2 K N4 C61 44.59(19) . . . . ? Ga K N4 C61 147.36(17) 2_665 . . . ? C52 K N4 C61 -131.62(18) . . . . ? Ga K N4 C61 74.0(2) . . . . ? C62 K N4 C61 119.1(2) . . . . ? C42 K N4 C61 53.83(17) . . . . ? N3 K N4 C62 130.44(18) . . . . ? C2 K N4 C62 -104.16(17) . . . . ? C1 K N4 C62 -128.49(17) . . . . ? N1 K N4 C62 -125.1(2) . . . . ? N2 K N4 C62 -74.50(17) . . . . ? Ga K N4 C62 28.26(16) 2_665 . . . ? C52 K N4 C62 109.28(17) . . . . ? Ga K N4 C62 -45.1(2) . . . . ? C42 K N4 C62 -65.27(16) . . . . ? N3 K N4 C6 27.9(2) . . . . ? C2 K N4 C6 153.3(2) . . . . ? C1 K N4 C6 128.9(2) . . . . ? N1 K N4 C6 132.4(2) . . . . ? N2 K N4 C6 -177.1(2) . . . . ? Ga K N4 C6 -74.3(2) 2_665 . . . ? C52 K N4 C6 6.7(2) . . . . ? Ga K N4 C6 -147.7(2) . . . . ? C62 K N4 C6 -102.6(3) . . . . ? C42 K N4 C6 -167.9(2) . . . . ? N3 K N4 C6A -3.1(3) . . . . ? C2 K N4 C6A 122.3(3) . . . . ? C1 K N4 C6A 97.9(3) . . . . ? N1 K N4 C6A 101.4(4) . . . . ? N2 K N4 C6A 151.9(3) . . . . ? Ga K N4 C6A -105.3(3) 2_665 . . . ? C52 K N4 C6A -24.3(3) . . . . ? Ga K N4 C6A -178.7(3) . . . . ? C62 K N4 C6A -133.6(4) . . . . ? C42 K N4 C6A 161.1(4) . . . . ? C3 N1 C1 C2 -179.97(18) . . . . ? Ga N1 C1 C2 -3.8(2) . . . . ? K N1 C1 C2 70.34(17) . . . . ? C3 N1 C1 K 109.70(15) . . . . ? Ga N1 C1 K -74.13(9) . . . . ? N4 K C1 C2 56.93(15) . . . . ? N3 K C1 C2 134.85(12) . . . . ? N1 K C1 C2 -120.44(18) . . . . ? N2 K C1 C2 -32.82(11) . . . . ? Ga K C1 C2 -94.56(12) 2_665 . . . ? C52 K C1 C2 161.37(12) . . . . ? Ga K C1 C2 -79.36(12) . . . . ? C62 K C1 C2 24.22(18) . . . . ? C42 K C1 C2 -5.12(12) . . . . ? N4 K C1 N1 177.37(10) . . . . ? N3 K C1 N1 -104.71(11) . . . . ? C2 K C1 N1 120.44(18) . . . . ? N2 K C1 N1 87.62(12) . . . . ? Ga K C1 N1 25.88(13) 2_665 . . . ? C52 K C1 N1 -78.19(13) . . . . ? Ga K C1 N1 41.08(9) . . . . ? C62 K C1 N1 144.66(13) . . . . ? C42 K C1 N1 115.32(12) . . . . ? N1 C1 C2 N2 0.6(3) . . . . ? K C1 C2 N2 73.60(17) . . . . ? N1 C1 C2 K -73.01(17) . . . . ? C4 N2 C2 C1 -177.69(18) . . . . ? Ga N2 C2 C1 2.9(2) . . . . ? K N2 C2 C1 -71.03(17) . . . . ? C4 N2 C2 K -106.66(15) . . . . ? Ga N2 C2 K 73.95(10) . . . . ? N4 K C2 C1 -137.52(12) . . . . ? N3 K C2 C1 -58.85(15) . . . . ? N1 K C2 C1 32.63(11) . . . . ? N2 K C2 C1 120.07(18) . . . . ? Ga K C2 C1 103.17(12) 2_665 . . . ? C52 K C2 C1 -28.62(19) . . . . ? Ga K C2 C1 79.09(12) . . . . ? C62 K C2 C1 -164.09(12) . . . . ? C42 K C2 C1 173.81(15) . . . . ? N4 K C2 N2 102.42(12) . . . . ? N3 K C2 N2 -178.92(10) . . . . ? C1 K C2 N2 -120.07(18) . . . . ? N1 K C2 N2 -87.44(12) . . . . ? Ga K C2 N2 -16.89(13) 2_665 . . . ? C52 K C2 N2 -148.69(14) . . . . ? Ga K C2 N2 -40.98(10) . . . . ? C62 K C2 N2 75.84(13) . . . . ? C42 K C2 N2 53.74(11) . . . . ? C1 N1 C3 C33 174.16(18) . . . . ? Ga N1 C3 C33 -1.2(2) . . . . ? K N1 C3 C33 -103.31(16) . . . . ? C1 N1 C3 C32 -66.4(2) . . . . ? Ga N1 C3 C32 118.29(19) . . . . ? K N1 C3 C32 16.2(2) . . . . ? C1 N1 C3 C31 55.0(2) . . . . ? Ga N1 C3 C31 -120.37(19) . . . . ? K N1 C3 C31 137.51(15) . . . . ? C2 N2 C4 C43 -173.09(18) . . . . ? Ga N2 C4 C43 6.2(2) . . . . ? K N2 C4 C43 105.93(16) . . . . ? C2 N2 C4 C42 67.6(2) . . . . ? Ga N2 C4 C42 -113.13(19) . . . . ? K N2 C4 C42 -13.37(19) . . . . ? C2 N2 C4 C41 -53.9(2) . . . . ? Ga N2 C4 C41 125.41(18) . . . . ? K N2 C4 C41 -134.83(15) . . . . ? C52 N3 C5 C6 71.4(4) . . . . ? C51 N3 C5 C6 -169.6(3) . . . . ? C5A N3 C5 C6 44.5(6) . . . . ? K N3 C5 C6 -45.0(4) . . . . ? C61 N4 C6 C5 71.6(4) . . . . ? C62 N4 C6 C5 -171.3(3) . . . . ? C6A N4 C6 C5 33.5(5) . . . . ? K N4 C6 C5 -64.1(4) . . . . ? N3 C5 C6 N4 78.2(4) . . . . ? C52 N3 C5A C6A 156.4(7) . . . . ? C51 N3 C5A C6A -87.7(7) . . . . ? C5 N3 C5A C6A -46.0(7) . . . . ? K N3 C5A C6A 54.4(8) . . . . ? N3 C5A C6A N4 -66.1(10) . . . . ? C61 N4 C6A C5A 155.6(7) . . . . ? C62 N4 C6A C5A -86.7(7) . . . . ? C6 N4 C6A C5A -56.4(8) . . . . ? K N4 C6A C5A 35.0(8) . . . . ? N2 C4 C42 K 10.85(16) . . . . ? C43 C4 C42 K -108.07(15) . . . . ? C41 C4 C42 K 133.81(15) . . . . ? N4 K C42 C4 -175.19(14) . . . . ? N3 K C42 C4 -153.37(12) . . . . ? C2 K C42 C4 -38.48(12) . . . . ? C1 K C42 C4 -35.74(12) . . . . ? N1 K C42 C4 -12.21(13) . . . . ? N2 K C42 C4 -7.02(10) . . . . ? Ga K C42 C4 88.78(12) 2_665 . . . ? C52 K C42 C4 172.21(14) . . . . ? Ga K C42 C4 16.13(11) . . . . ? C62 K C42 C4 161.94(14) . . . . ? C51 N3 C52 K 125.5(2) . . . . ? C5A N3 C52 K -106.9(3) . . . . ? C5 N3 C52 K -120.5(3) . . . . ? N4 K C52 N3 52.87(17) . . . . ? C2 K C52 N3 -67.6(2) . . . . ? C1 K C52 N3 -81.80(19) . . . . ? N1 K C52 N3 -109.76(17) . . . . ? N2 K C52 N3 -116.3(2) . . . . ? Ga K C52 N3 151.59(18) 2_665 . . . ? Ga K C52 N3 -145.09(14) . . . . ? C62 K C52 N3 75.02(17) . . . . ? C42 K C52 N3 65.4(2) . . . . ? C61 N4 C62 K -124.6(2) . . . . ? C6 N4 C62 K 108.3(2) . . . . ? C6A N4 C62 K 122.9(3) . . . . ? N3 K C62 N4 -44.09(16) . . . . ? C2 K C62 N4 88.74(17) . . . . ? C1 K C62 N4 76.7(2) . . . . ? N1 K C62 N4 125.40(19) . . . . ? N2 K C62 N4 116.01(16) . . . . ? Ga K C62 N4 -151.06(17) 2_665 . . . ? C52 K C62 N4 -67.66(16) . . . . ? Ga K C62 N4 150.84(14) . . . . ? C42 K C62 N4 107.98(16) . . . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.298 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.052