Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Cameron Jones' 'Robert J. Baker' 'Marc Kloth' _publ_contact_author_name 'Prof Cameron Jones' _publ_contact_author_address ; Chemistry Department Cardiff University Main Building Cardiff University Cardiff CF10 3AT UNITED KINGDOM ; _publ_contact_author_email JONESCA6@CARDIFF.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Oxidation Reactions of an Anionic Gallium(I) N-Heterocyclic Carbene Analogue with Group 16 Compounds ; data_compound5 _database_code_depnum_ccdc_archive 'CCDC 268557' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H76 Ga K N2 O3 Te2' _chemical_formula_weight 1117.15 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.690(2) _cell_length_b 23.912(5) _cell_length_c 19.616(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.19(3) _cell_angle_gamma 90.00 _cell_volume 5359.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.673 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51522 _diffrn_reflns_av_R_equivalents 0.0942 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.02 _reflns_number_total 10484 _reflns_number_gt 7500 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. During the course of the refinement it was found that the molecule of diethyl ether containing the oxygen centre, O(3), was severely disordered. This disorder was modelled but the displacement parameters of the two disordered diethyl ether 'parts' were found to be relatively high so both were subsequently refined isotropically. In addition, a relatively large peak of electron density was found 1.10 angstroms from K1. This is believed to arise from significant thermal motion for this atom. Attempts to model a disorder of this atom over two sites met with failure. Despite the problems associated with disorder in the crystal structure, the molecular connectivity of the molecule is unambiguous and fully supported by its spectroscopic data. ; _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^)+(0.0766P)^2^+35.5694P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10484 _refine_ls_number_parameters 545 _refine_ls_number_restraints 118 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1830 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.36685(4) 0.40367(2) 0.40871(3) 0.04223(19) Uani 1 1 d . A . Te2 Te 0.26633(4) 0.32112(2) 0.23532(3) 0.03633(18) Uani 1 1 d . A . Ga1 Ga 0.17327(6) 0.38418(3) 0.32112(4) 0.0251(2) Uani 1 1 d . . . K1 K 0.4044(3) 0.24288(11) 0.39491(13) 0.0750(7) Uani 1 1 d U . . O1 O 0.3478(6) 0.1532(3) 0.3017(4) 0.076(2) Uani 1 1 d DU A . O2 O 0.6377(10) 0.2701(5) 0.4186(6) 0.126(4) Uani 1 1 d DU A . O3 O 0.4205(14) 0.1643(8) 0.4953(9) 0.111(6) Uiso 0.64(2) 1 d PD A 1 O3A O 0.4128(19) 0.1941(9) 0.5214(12) 0.079(8) Uiso 0.36(2) 1 d PD A 2 N1 N 0.0705(5) 0.4429(2) 0.2829(3) 0.0276(13) Uani 1 1 d . . . N2 N 0.0464(5) 0.3515(2) 0.3535(3) 0.0323(14) Uani 1 1 d . . . C1 C -0.0408(6) 0.4308(3) 0.2954(4) 0.0346(17) Uani 1 1 d . . . H1 H -0.1055 0.4547 0.2786 0.042 Uiso 1 1 calc R . . C2 C -0.0532(7) 0.3847(3) 0.3317(4) 0.0377(18) Uani 1 1 d . . . H2 H -0.1264 0.3750 0.3422 0.045 Uiso 1 1 calc R . . C3 C 0.0832(7) 0.4796(3) 0.2285(4) 0.0392(19) Uani 1 1 d . . . C4 C 0.1501(8) 0.5278(4) 0.2454(5) 0.049(2) Uani 1 1 d . . . C5 C 0.1713(11) 0.5619(4) 0.1901(8) 0.080(4) Uani 1 1 d . . . H5 H 0.2199 0.5940 0.2007 0.096 Uiso 1 1 calc R . . C6 C 0.1243(14) 0.5498(7) 0.1228(8) 0.102(5) Uani 1 1 d . . . H6 H 0.1394 0.5734 0.0867 0.123 Uiso 1 1 calc R . . C7 C 0.0530(12) 0.5024(7) 0.1061(6) 0.090(4) Uani 1 1 d . . . H7 H 0.0185 0.4948 0.0586 0.108 Uiso 1 1 calc R . . C8 C 0.0319(8) 0.4665(4) 0.1572(5) 0.054(2) Uani 1 1 d . . . C9 C 0.1974(7) 0.5431(3) 0.3195(5) 0.047(2) Uani 1 1 d . . . H9 H 0.2238 0.5076 0.3450 0.057 Uiso 1 1 calc R . . C10 C 0.0983(9) 0.5679(4) 0.3527(6) 0.064(3) Uani 1 1 d . . . H10A H 0.0666 0.6016 0.3271 0.095 Uiso 1 1 calc R . . H10B H 0.1302 0.5775 0.4016 0.095 Uiso 1 1 calc R . . H10C H 0.0357 0.5402 0.3502 0.095 Uiso 1 1 calc R . . C11 C 0.3030(10) 0.5834(5) 0.3332(8) 0.091(4) Uani 1 1 d . . . H11A H 0.3626 0.5699 0.3088 0.136 Uiso 1 1 calc R . . H11B H 0.3362 0.5852 0.3834 0.136 Uiso 1 1 calc R . . H11C H 0.2771 0.6208 0.3161 0.136 Uiso 1 1 calc R . . C12 C -0.0398(9) 0.4146(5) 0.1372(5) 0.060(3) Uani 1 1 d . . . H12 H -0.0311 0.3904 0.1796 0.072 Uiso 1 1 calc R . . C13 C 0.0025(11) 0.3809(6) 0.0806(6) 0.089(4) Uani 1 1 d . . . H13A H -0.0134 0.4021 0.0368 0.134 Uiso 1 1 calc R . . H13B H -0.0390 0.3451 0.0736 0.134 Uiso 1 1 calc R . . H13C H 0.0868 0.3741 0.0952 0.134 Uiso 1 1 calc R . . C14 C -0.1706(10) 0.4290(7) 0.1128(7) 0.095(4) Uani 1 1 d . . . H14A H -0.1977 0.4491 0.1500 0.143 Uiso 1 1 calc R . . H14B H -0.2158 0.3945 0.1017 0.143 Uiso 1 1 calc R . . H14C H -0.1814 0.4527 0.0712 0.143 Uiso 1 1 calc R . . C15 C 0.0348(8) 0.2940(3) 0.3710(5) 0.044(2) Uani 1 1 d . . . C16 C -0.0207(9) 0.2553(3) 0.3203(6) 0.060(3) Uani 1 1 d . . . C17 C -0.0267(12) 0.1998(5) 0.3394(7) 0.081(3) Uani 1 1 d U . . H17 H -0.0669 0.1737 0.3064 0.097 Uiso 1 1 calc R . . C18 C 0.0237(13) 0.1823(5) 0.4040(8) 0.091(4) Uani 1 1 d U . . H18 H 0.0227 0.1435 0.4145 0.109 Uiso 1 1 calc R . . C19 C 0.0773(13) 0.2193(5) 0.4561(7) 0.091(4) Uani 1 1 d . . . H19 H 0.1106 0.2061 0.5016 0.109 Uiso 1 1 calc R . . C20 C 0.0809(9) 0.2775(4) 0.4395(5) 0.059(3) Uani 1 1 d . . . C21 C -0.0758(9) 0.2721(4) 0.2462(6) 0.067(3) Uani 1 1 d . . . H21 H -0.0537 0.3119 0.2400 0.080 Uiso 1 1 calc R . . C22 C -0.0322(12) 0.2370(5) 0.1909(7) 0.089(4) Uani 1 1 d . . . H22A H -0.0683 0.1999 0.1879 0.133 Uiso 1 1 calc R . . H22B H 0.0531 0.2332 0.2041 0.133 Uiso 1 1 calc R . . H22C H -0.0535 0.2556 0.1455 0.133 Uiso 1 1 calc R . . C23 C -0.2084(12) 0.2696(7) 0.2342(9) 0.112(5) Uani 1 1 d U . . H23A H -0.2329 0.2310 0.2404 0.167 Uiso 1 1 calc R . . H23B H -0.2427 0.2821 0.1868 0.167 Uiso 1 1 calc R . . H23C H -0.2352 0.2939 0.2679 0.167 Uiso 1 1 calc R . . C24 C 0.1301(9) 0.3201(4) 0.4954(5) 0.059(3) Uani 1 1 d . . . H24 H 0.1667 0.3507 0.4725 0.071 Uiso 1 1 calc R . . C25 C 0.0272(11) 0.3465(5) 0.5240(7) 0.081(4) Uani 1 1 d . . . H25A H -0.0176 0.3168 0.5408 0.122 Uiso 1 1 calc R . . H25B H -0.0243 0.3673 0.4866 0.122 Uiso 1 1 calc R . . H25C H 0.0588 0.3720 0.5625 0.122 Uiso 1 1 calc R . . C26 C 0.2218(14) 0.2978(7) 0.5537(7) 0.109(5) Uani 1 1 d U . . H26A H 0.1854 0.2732 0.5830 0.164 Uiso 1 1 calc R . . H26B H 0.2607 0.3290 0.5818 0.164 Uiso 1 1 calc R . . H26C H 0.2795 0.2766 0.5345 0.164 Uiso 1 1 calc R . . C27 C 0.3143(7) 0.4487(4) 0.4903(4) 0.0387(18) Uani 1 1 d . . . C28 C 0.1999(7) 0.4656(4) 0.4885(4) 0.045(2) Uani 1 1 d . A . H28 H 0.1400 0.4570 0.4491 0.053 Uiso 1 1 calc R . . C29 C 0.1727(8) 0.4952(4) 0.5440(5) 0.050(2) Uani 1 1 d . . . H29 H 0.0943 0.5066 0.5425 0.061 Uiso 1 1 calc R A . C30 C 0.2585(8) 0.5077(4) 0.6006(5) 0.050(2) Uani 1 1 d . A . H30 H 0.2394 0.5274 0.6387 0.060 Uiso 1 1 calc R . . C31 C 0.3717(8) 0.4921(5) 0.6031(5) 0.058(3) Uani 1 1 d . . . H31 H 0.4309 0.5014 0.6426 0.070 Uiso 1 1 calc R A . C32 C 0.4003(7) 0.4628(4) 0.5485(5) 0.054(2) Uani 1 1 d . A . H32 H 0.4792 0.4522 0.5505 0.065 Uiso 1 1 calc R . . C33 C 0.3993(6) 0.3802(3) 0.2257(4) 0.0357(18) Uani 1 1 d . . . C34 C 0.5157(7) 0.3653(4) 0.2406(5) 0.048(2) Uani 1 1 d . A . H34 H 0.5383 0.3288 0.2571 0.057 Uiso 1 1 calc R . . C35 C 0.5998(8) 0.4040(5) 0.2315(6) 0.064(3) Uani 1 1 d . . . H35 H 0.6800 0.3934 0.2413 0.077 Uiso 1 1 calc R A . C36 C 0.5696(9) 0.4561(5) 0.2089(6) 0.064(3) Uani 1 1 d . A . H36 H 0.6283 0.4820 0.2029 0.077 Uiso 1 1 calc R . . C37 C 0.4538(10) 0.4722(5) 0.1946(6) 0.069(3) Uani 1 1 d . . . H37 H 0.4327 0.5093 0.1795 0.083 Uiso 1 1 calc R A . C38 C 0.3685(8) 0.4339(4) 0.2023(5) 0.051(2) Uani 1 1 d . A . H38 H 0.2884 0.4446 0.1914 0.061 Uiso 1 1 calc R . . C39 C 0.4913(14) 0.1796(7) 0.2380(9) 0.120(5) Uani 1 1 d DU A . H39A H 0.4612 0.2178 0.2307 0.180 Uiso 1 1 calc R . . H39B H 0.5253 0.1684 0.1985 0.180 Uiso 1 1 calc R . . H39C H 0.5515 0.1779 0.2811 0.180 Uiso 1 1 calc R . . C40 C 0.3972(15) 0.1423(7) 0.2434(9) 0.130(6) Uani 1 1 d DU . . H40A H 0.3353 0.1454 0.2005 0.156 Uiso 1 1 calc R A . H40B H 0.4268 0.1034 0.2464 0.156 Uiso 1 1 calc R . . C41 C 0.2238(13) 0.1464(7) 0.2887(11) 0.149(7) Uani 1 1 d DU . . H41A H 0.1886 0.1599 0.2411 0.179 Uiso 1 1 calc R A . H41B H 0.1914 0.1691 0.3224 0.179 Uiso 1 1 calc R . . C42 C 0.1925(12) 0.0857(6) 0.2954(8) 0.105(4) Uani 1 1 d DU A . H42A H 0.2041 0.0651 0.2542 0.157 Uiso 1 1 calc R . . H42B H 0.1104 0.0828 0.2990 0.157 Uiso 1 1 calc R . . H42C H 0.2426 0.0698 0.3373 0.157 Uiso 1 1 calc R . . C43 C 0.6838(19) 0.3501(9) 0.4950(10) 0.170(8) Uani 1 1 d DU A . H43A H 0.6061 0.3493 0.5065 0.255 Uiso 1 1 calc R . . H43B H 0.7129 0.3887 0.4980 0.255 Uiso 1 1 calc R . . H43C H 0.7376 0.3267 0.5281 0.255 Uiso 1 1 calc R . . C44 C 0.6756(13) 0.3285(6) 0.4229(8) 0.104(4) Uani 1 1 d DU . . H44A H 0.6190 0.3513 0.3895 0.124 Uiso 1 1 calc R A . H44B H 0.7529 0.3315 0.4101 0.124 Uiso 1 1 calc R . . C45 C 0.7298(16) 0.2352(7) 0.4443(11) 0.149(7) Uani 1 1 d DU . . H45A H 0.7567 0.2421 0.4949 0.179 Uiso 1 1 calc R A . H45B H 0.7954 0.2441 0.4214 0.179 Uiso 1 1 calc R . . C46 C 0.6986(16) 0.1736(6) 0.4328(10) 0.133(6) Uani 1 1 d DU A . H46A H 0.6259 0.1658 0.4484 0.200 Uiso 1 1 calc R . . H46B H 0.7618 0.1506 0.4595 0.200 Uiso 1 1 calc R . . H46C H 0.6878 0.1647 0.3831 0.200 Uiso 1 1 calc R . . C47 C 0.533(2) 0.2329(10) 0.5767(14) 0.115(9) Uiso 0.64(2) 1 d PD A 1 H47A H 0.5824 0.2347 0.5421 0.173 Uiso 0.64(2) 1 calc PR A 1 H47B H 0.5825 0.2354 0.6236 0.173 Uiso 0.64(2) 1 calc PR A 1 H47C H 0.4774 0.2640 0.5693 0.173 Uiso 0.64(2) 1 calc PR A 1 C47A C 0.540(3) 0.2719(14) 0.565(2) 0.107(15) Uiso 0.36(2) 1 d PD A 2 H47D H 0.5726 0.2679 0.5234 0.160 Uiso 0.36(2) 1 calc PR A 2 H47E H 0.6014 0.2846 0.6042 0.160 Uiso 0.36(2) 1 calc PR A 2 H47F H 0.4763 0.2994 0.5564 0.160 Uiso 0.36(2) 1 calc PR A 2 C48 C 0.466(2) 0.1775(11) 0.5691(11) 0.113(9) Uiso 0.64(2) 1 d PD A 1 H48A H 0.5194 0.1471 0.5909 0.135 Uiso 0.64(2) 1 calc PR A 1 H48B H 0.4009 0.1799 0.5937 0.135 Uiso 0.64(2) 1 calc PR A 1 C48A C 0.493(2) 0.2157(11) 0.5834(12) 0.051(8) Uiso 0.36(2) 1 d PD A 2 H48C H 0.5580 0.1891 0.5987 0.061 Uiso 0.36(2) 1 calc PR A 2 H48D H 0.4507 0.2203 0.6219 0.061 Uiso 0.36(2) 1 calc PR A 2 C49 C 0.341(2) 0.1144(11) 0.4924(18) 0.148(12) Uiso 0.64(2) 1 d PD A 1 H49A H 0.2722 0.1170 0.4531 0.177 Uiso 0.64(2) 1 calc PR A 1 H49B H 0.3136 0.1094 0.5366 0.177 Uiso 0.64(2) 1 calc PR A 1 C49A C 0.364(4) 0.1389(13) 0.534(2) 0.14(2) Uiso 0.36(2) 1 d PD A 2 H49C H 0.2782 0.1395 0.5284 0.172 Uiso 0.36(2) 1 calc PR A 2 H49D H 0.4013 0.1230 0.5799 0.172 Uiso 0.36(2) 1 calc PR A 2 C50 C 0.425(5) 0.0679(16) 0.481(4) 0.35(4) Uiso 0.64(2) 1 d PD A 1 H50A H 0.4476 0.0736 0.4365 0.526 Uiso 0.64(2) 1 calc PR A 1 H50B H 0.3857 0.0316 0.4810 0.526 Uiso 0.64(2) 1 calc PR A 1 H50C H 0.4944 0.0687 0.5190 0.526 Uiso 0.64(2) 1 calc PR A 1 C50A C 0.403(3) 0.1089(12) 0.4730(16) 0.066(9) Uiso 0.36(2) 1 d PD A 2 H50D H 0.3593 0.1239 0.4287 0.100 Uiso 0.36(2) 1 calc PR A 2 H50E H 0.3881 0.0687 0.4754 0.100 Uiso 0.36(2) 1 calc PR A 2 H50F H 0.4871 0.1151 0.4764 0.100 Uiso 0.36(2) 1 calc PR A 2 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 Te1 0.0275(3) 0.0606(4) 0.0373(3) -0.0138(3) 0.0039(2) 0.0085(2) Te2 0.0373(3) 0.0359(3) 0.0389(3) -0.0082(2) 0.0150(2) 0.0048(2) Ga1 0.0274(4) 0.0228(4) 0.0268(4) 0.0011(3) 0.0098(3) 0.0025(3) K1 0.1030(18) 0.0657(14) 0.0538(14) 0.0068(11) 0.0111(12) 0.0178(13) O1 0.062(4) 0.076(4) 0.090(5) 0.016(4) 0.021(3) -0.002(3) O2 0.117(6) 0.137(6) 0.120(6) 0.001(5) 0.019(5) -0.001(5) N1 0.027(3) 0.026(3) 0.031(3) 0.003(3) 0.011(2) 0.001(2) N2 0.040(4) 0.025(3) 0.035(4) 0.001(3) 0.016(3) -0.002(3) C1 0.024(4) 0.047(5) 0.033(4) -0.005(4) 0.007(3) 0.011(3) C2 0.031(4) 0.044(5) 0.042(5) 0.000(4) 0.015(3) -0.004(3) C3 0.038(4) 0.040(5) 0.042(5) 0.016(4) 0.015(4) 0.017(3) C4 0.048(5) 0.040(5) 0.065(6) 0.020(4) 0.027(4) 0.015(4) C5 0.086(8) 0.045(6) 0.119(11) 0.047(7) 0.043(8) 0.017(5) C6 0.118(11) 0.115(12) 0.084(10) 0.074(9) 0.044(9) 0.026(9) C7 0.105(10) 0.127(12) 0.042(6) 0.041(7) 0.026(6) 0.048(9) C8 0.060(6) 0.064(6) 0.039(5) 0.015(4) 0.015(4) 0.020(5) C9 0.039(5) 0.020(4) 0.084(7) 0.008(4) 0.018(4) 0.003(3) C10 0.069(7) 0.037(5) 0.088(8) -0.007(5) 0.024(6) 0.005(4) C11 0.069(8) 0.049(6) 0.156(13) 0.011(7) 0.026(8) -0.012(5) C12 0.062(6) 0.080(7) 0.035(5) -0.003(5) 0.003(4) 0.017(5) C13 0.080(8) 0.140(12) 0.043(6) -0.021(7) 0.004(5) 0.040(8) C14 0.073(8) 0.136(12) 0.073(8) -0.011(8) 0.006(6) 0.033(8) C15 0.056(5) 0.030(4) 0.057(6) 0.007(4) 0.035(4) 0.001(4) C16 0.085(7) 0.018(4) 0.093(8) -0.013(4) 0.055(6) -0.011(4) C17 0.102(7) 0.058(6) 0.096(7) -0.014(5) 0.052(6) -0.013(5) C18 0.115(8) 0.052(6) 0.117(8) -0.004(6) 0.048(7) 0.008(6) C19 0.135(11) 0.063(7) 0.095(10) 0.037(7) 0.072(9) 0.021(7) C20 0.085(7) 0.040(5) 0.068(7) 0.022(5) 0.053(6) 0.017(5) C21 0.074(7) 0.052(6) 0.077(8) -0.030(6) 0.022(6) -0.017(5) C22 0.100(9) 0.060(7) 0.114(11) -0.036(7) 0.042(8) -0.023(6) C23 0.100(8) 0.105(8) 0.130(9) -0.021(7) 0.024(7) -0.017(7) C24 0.077(7) 0.069(7) 0.041(5) 0.022(5) 0.032(5) 0.015(5) C25 0.099(9) 0.077(8) 0.088(9) 0.002(7) 0.066(7) 0.001(7) C26 0.120(8) 0.125(8) 0.082(7) 0.020(7) 0.023(6) 0.026(7) C27 0.034(4) 0.053(5) 0.031(4) -0.012(4) 0.011(3) 0.001(3) C28 0.039(5) 0.053(5) 0.041(5) -0.012(4) 0.007(4) 0.005(4) C29 0.043(5) 0.058(6) 0.050(5) -0.014(4) 0.010(4) 0.007(4) C30 0.049(5) 0.059(6) 0.046(5) -0.020(4) 0.018(4) -0.007(4) C31 0.039(5) 0.094(8) 0.043(5) -0.023(5) 0.009(4) -0.013(5) C32 0.032(5) 0.084(7) 0.046(5) -0.019(5) 0.010(4) 0.000(4) C33 0.032(4) 0.045(5) 0.035(4) -0.016(4) 0.019(3) -0.002(3) C34 0.035(5) 0.058(6) 0.052(5) -0.013(4) 0.013(4) -0.004(4) C35 0.035(5) 0.086(8) 0.074(7) -0.024(6) 0.018(5) -0.004(5) C36 0.049(6) 0.075(8) 0.078(7) -0.017(6) 0.035(5) -0.026(5) C37 0.076(7) 0.057(6) 0.087(8) -0.005(6) 0.045(6) -0.012(5) C38 0.046(5) 0.051(5) 0.062(6) 0.002(5) 0.025(4) -0.002(4) C39 0.121(7) 0.120(8) 0.130(8) -0.001(6) 0.048(6) 0.019(6) C40 0.141(8) 0.121(8) 0.126(8) -0.022(6) 0.024(6) 0.002(6) C41 0.138(9) 0.147(9) 0.157(9) 0.000(6) 0.020(6) 0.002(6) C42 0.092(6) 0.096(7) 0.121(7) -0.016(6) 0.013(5) -0.009(5) C43 0.165(10) 0.173(10) 0.169(10) -0.001(7) 0.030(7) -0.002(7) C44 0.100(7) 0.105(7) 0.111(7) 0.004(6) 0.033(6) -0.001(5) C45 0.153(9) 0.157(9) 0.144(9) -0.005(6) 0.048(6) 0.017(6) C46 0.131(8) 0.132(8) 0.136(8) -0.005(6) 0.027(6) 0.019(6) _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 Te1 C27 2.125(7) . ? Te1 Ga1 2.5785(12) . ? Te1 K1 3.886(3) . ? Te2 C33 2.139(8) . ? Te2 Ga1 2.6577(10) . ? Te2 K1 3.711(3) . ? Ga1 N1 1.896(6) . ? Ga1 N2 1.900(6) . ? K1 O3 2.700(16) . ? K1 O3A 2.72(2) . ? K1 O2 2.747(12) . ? K1 O1 2.805(9) . ? O1 C40 1.410(13) . ? O1 C41 1.427(14) . ? O2 C45 1.371(14) . ? O2 C44 1.463(13) . ? O3 C48 1.467(17) . ? O3 C49 1.509(17) . ? O3A C48A 1.462(18) . ? O3A C49A 1.478(19) . ? N1 C1 1.405(9) . ? N1 C3 1.413(9) . ? N2 C2 1.401(10) . ? N2 C15 1.429(10) . ? C1 C2 1.335(11) . ? C3 C4 1.393(12) . ? C3 C8 1.436(12) . ? C4 C5 1.420(14) . ? C4 C9 1.487(14) . ? C5 C6 1.35(2) . ? C6 C7 1.41(2) . ? C7 C8 1.380(15) . ? C8 C12 1.503(15) . ? C9 C11 1.545(13) . ? C9 C10 1.561(13) . ? C12 C13 1.535(14) . ? C12 C14 1.542(14) . ? C15 C20 1.395(13) . ? C15 C16 1.412(13) . ? C16 C17 1.385(14) . ? C16 C21 1.515(16) . ? C17 C18 1.347(19) . ? C18 C19 1.395(19) . ? C19 C20 1.433(14) . ? C20 C24 1.518(15) . ? C21 C23 1.519(17) . ? C21 C22 1.542(15) . ? C24 C26 1.490(16) . ? C24 C25 1.564(13) . ? C27 C28 1.391(11) . ? C27 C32 1.393(11) . ? C28 C29 1.389(12) . ? C29 C30 1.364(12) . ? C30 C31 1.366(13) . ? C31 C32 1.380(12) . ? C33 C34 1.377(11) . ? C33 C38 1.386(12) . ? C34 C35 1.389(13) . ? C35 C36 1.345(15) . ? C36 C37 1.377(15) . ? C37 C38 1.386(13) . ? C39 C40 1.437(15) . ? C41 C42 1.510(15) . ? C43 C44 1.491(15) . ? C45 C46 1.523(15) . ? C47 C48 1.529(18) . ? C47A C48A 1.524(19) . ? C49 C50 1.53(2) . ? C49A C50A 1.54(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 Te1 Ga1 103.9(2) . . ? C27 Te1 K1 127.5(2) . . ? Ga1 Te1 K1 82.57(5) . . ? C33 Te2 Ga1 94.77(18) . . ? C33 Te2 K1 102.3(2) . . ? Ga1 Te2 K1 85.12(5) . . ? N1 Ga1 N2 87.9(2) . . ? N1 Ga1 Te1 121.56(18) . . ? N2 Ga1 Te1 119.27(19) . . ? N1 Ga1 Te2 118.63(18) . . ? N2 Ga1 Te2 115.50(18) . . ? Te1 Ga1 Te2 96.06(3) . . ? O3 K1 O3A 18.9(5) . . ? O3 K1 O2 97.3(4) . . ? O3A K1 O2 95.9(5) . . ? O3 K1 O1 85.1(4) . . ? O3A K1 O1 103.0(5) . . ? O2 K1 O1 112.3(3) . . ? O3 K1 Te2 156.5(4) . . ? O3A K1 Te2 155.5(5) . . ? O2 K1 Te2 105.2(3) . . ? O1 K1 Te2 80.47(17) . . ? O3 K1 Te1 129.0(4) . . ? O3A K1 Te1 110.1(5) . . ? O2 K1 Te1 82.9(3) . . ? O1 K1 Te1 141.91(18) . . ? Te2 K1 Te1 61.62(4) . . ? C40 O1 C41 114.1(12) . . ? C40 O1 K1 126.2(8) . . ? C41 O1 K1 107.1(9) . . ? C45 O2 C44 110.8(12) . . ? C45 O2 K1 126.3(11) . . ? C44 O2 K1 120.9(9) . . ? C48 O3 C49 107.6(17) . . ? C48 O3 K1 121.6(12) . . ? C49 O3 K1 125.1(15) . . ? C48A O3A C49A 112(2) . . ? C48A O3A K1 120.0(14) . . ? C49A O3A K1 126.3(18) . . ? C1 N1 C3 120.6(6) . . ? C1 N1 Ga1 108.1(5) . . ? C3 N1 Ga1 126.9(5) . . ? C2 N2 C15 120.3(6) . . ? C2 N2 Ga1 108.8(5) . . ? C15 N2 Ga1 126.6(5) . . ? C2 C1 N1 118.2(7) . . ? C1 C2 N2 117.0(6) . . ? C4 C3 N1 118.6(7) . . ? C4 C3 C8 120.7(8) . . ? N1 C3 C8 120.7(8) . . ? C3 C4 C5 118.2(10) . . ? C3 C4 C9 120.6(7) . . ? C5 C4 C9 121.2(10) . . ? C6 C5 C4 121.6(12) . . ? C5 C6 C7 120.0(11) . . ? C8 C7 C6 121.3(12) . . ? C7 C8 C3 118.0(11) . . ? C7 C8 C12 119.9(10) . . ? C3 C8 C12 122.0(8) . . ? C4 C9 C11 116.2(9) . . ? C4 C9 C10 110.2(7) . . ? C11 C9 C10 109.0(8) . . ? C8 C12 C13 112.0(10) . . ? C8 C12 C14 110.9(9) . . ? C13 C12 C14 110.0(9) . . ? C20 C15 C16 121.3(8) . . ? C20 C15 N2 117.9(8) . . ? C16 C15 N2 120.9(8) . . ? C17 C16 C15 118.7(11) . . ? C17 C16 C21 118.5(10) . . ? C15 C16 C21 122.7(8) . . ? C18 C17 C16 121.0(12) . . ? C17 C18 C19 122.1(12) . . ? C18 C19 C20 118.7(12) . . ? C15 C20 C19 118.0(11) . . ? C15 C20 C24 121.1(8) . . ? C19 C20 C24 120.9(10) . . ? C16 C21 C23 110.5(10) . . ? C16 C21 C22 113.2(10) . . ? C23 C21 C22 110.4(10) . . ? C26 C24 C20 114.6(10) . . ? C26 C24 C25 110.7(10) . . ? C20 C24 C25 109.1(9) . . ? C28 C27 C32 118.2(7) . . ? C28 C27 Te1 124.0(6) . . ? C32 C27 Te1 117.8(6) . . ? C29 C28 C27 120.5(8) . . ? C30 C29 C28 119.9(8) . . ? C29 C30 C31 120.7(8) . . ? C30 C31 C32 120.1(8) . . ? C31 C32 C27 120.6(8) . . ? C34 C33 C38 119.1(8) . . ? C34 C33 Te2 121.0(6) . . ? C38 C33 Te2 119.9(6) . . ? C33 C34 C35 119.7(9) . . ? C36 C35 C34 121.0(9) . . ? C35 C36 C37 120.3(9) . . ? C36 C37 C38 119.5(10) . . ? C37 C38 C33 120.4(9) . . ? O1 C40 C39 113.3(13) . . ? O1 C41 C42 110.5(12) . . ? O2 C44 C43 110.1(13) . . ? O2 C45 C46 112.9(15) . . ? O3 C48 C47 110.8(18) . . ? O3A C48A C47A 108(2) . . ? O3 C49 C50 100(2) . . ? O3A C49A C50A 95.7(19) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.883 #(1.10 angstrom from K1) _refine_diff_density_min -1.526 #(near Ga1) _refine_diff_density_rms 0.148 data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 268558' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H88 Ga2 K2 N4 O2 Te2' _chemical_formula_weight 1370.18 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 12.084(2) _cell_length_b 21.762(4) _cell_length_c 12.374(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.22(3) _cell_angle_gamma 90.00 _cell_volume 3167.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 1.926 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.504 _exptl_absorpt_correction_T_max 0.714 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19176 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5675 _reflns_number_gt 4518 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+4.8876P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5675 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _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 Te1 Te 0.83984(3) 0.026097(14) 0.48652(3) 0.03897(15) Uani 1 1 d . . . Ga1 Ga 0.99255(4) 0.02218(2) 0.36647(4) 0.03367(16) Uani 1 1 d . . . K1 K 0.72804(11) -0.11801(6) 0.38920(10) 0.0537(3) Uani 1 1 d . . . O1 O 0.5065(4) -0.1453(2) 0.3583(4) 0.0766(13) Uani 1 1 d . . . N1 N 1.0455(3) 0.09245(17) 0.2973(3) 0.0370(9) Uani 1 1 d . . . N2 N 0.9419(3) -0.01219(16) 0.2207(3) 0.0348(9) Uani 1 1 d . . . C1 C 1.0292(4) 0.0805(2) 0.1843(4) 0.0385(11) Uani 1 1 d . . . H1 H 1.0570 0.1079 0.1369 0.046 Uiso 1 1 calc R . . C2 C 0.9734(4) 0.0294(2) 0.1442(4) 0.0396(11) Uani 1 1 d . . . H2 H 0.9552 0.0211 0.0668 0.048 Uiso 1 1 calc R . . C3 C 1.1130(4) 0.1415(2) 0.3480(4) 0.0372(11) Uani 1 1 d . . . C4 C 1.2290(4) 0.1472(2) 0.3451(4) 0.0416(12) Uani 1 1 d . . . C5 C 1.2909(5) 0.1971(2) 0.3988(5) 0.0492(13) Uani 1 1 d . . . H5 H 1.3682 0.2017 0.3953 0.059 Uiso 1 1 calc R . . C6 C 1.2425(5) 0.2401(2) 0.4571(4) 0.0493(13) Uani 1 1 d . . . H6 H 1.2869 0.2727 0.4955 0.059 Uiso 1 1 calc R . . C7 C 1.1283(5) 0.2346(2) 0.4585(4) 0.0469(12) Uani 1 1 d . . . H7 H 1.0947 0.2640 0.4980 0.056 Uiso 1 1 calc R . . C8 C 1.0623(4) 0.1871(2) 0.4035(4) 0.0421(12) Uani 1 1 d . . . C9 C 1.2870(4) 0.1005(2) 0.2856(5) 0.0475(13) Uani 1 1 d . . . H9 H 1.2329 0.0656 0.2623 0.057 Uiso 1 1 calc R . . C10 C 1.3941(5) 0.0746(3) 0.3606(6) 0.0637(16) Uani 1 1 d . . . H10A H 1.4456 0.1084 0.3909 0.096 Uiso 1 1 calc R . . H10B H 1.4318 0.0470 0.3177 0.096 Uiso 1 1 calc R . . H10C H 1.3740 0.0517 0.4216 0.096 Uiso 1 1 calc R . . C11 C 1.3134(5) 0.1287(3) 0.1794(5) 0.0639(16) Uani 1 1 d . . . H11A H 1.2440 0.1466 0.1336 0.096 Uiso 1 1 calc R . . H11B H 1.3417 0.0965 0.1372 0.096 Uiso 1 1 calc R . . H11C H 1.3713 0.1607 0.2002 0.096 Uiso 1 1 calc R . . C12 C 0.9328(4) 0.1864(2) 0.3889(4) 0.0460(12) Uani 1 1 d . . . H12 H 0.9090 0.1423 0.3862 0.055 Uiso 1 1 calc R . . C13 C 0.8782(5) 0.2145(3) 0.2759(5) 0.0552(14) Uani 1 1 d . . . H13A H 0.7952 0.2135 0.2647 0.083 Uiso 1 1 calc R . . H13B H 0.9008 0.1909 0.2171 0.083 Uiso 1 1 calc R . . H13C H 0.9035 0.2572 0.2735 0.083 Uiso 1 1 calc R . . C14 C 0.8911(5) 0.2162(3) 0.4831(5) 0.0560(14) Uani 1 1 d . . . H14A H 0.9241 0.1948 0.5527 0.084 Uiso 1 1 calc R . . H14B H 0.8080 0.2135 0.4679 0.084 Uiso 1 1 calc R . . H14C H 0.9142 0.2594 0.4894 0.084 Uiso 1 1 calc R . . C15 C 0.8385(4) -0.0447(2) 0.1832(4) 0.0354(10) Uani 1 1 d . . . C16 C 0.8432(4) -0.1095(2) 0.1777(4) 0.0392(11) Uani 1 1 d . . . C17 C 0.7413(4) -0.1422(2) 0.1424(4) 0.0459(12) Uani 1 1 d . . . H17 H 0.7436 -0.1858 0.1382 0.055 Uiso 1 1 calc R . . C18 C 0.6376(5) -0.1125(3) 0.1135(5) 0.0536(14) Uani 1 1 d . . . H18 H 0.5693 -0.1354 0.0911 0.064 Uiso 1 1 calc R . . C19 C 0.6343(4) -0.0489(2) 0.1178(5) 0.0480(13) Uani 1 1 d . . . H19 H 0.5631 -0.0285 0.0964 0.058 Uiso 1 1 calc R . . C20 C 0.7329(4) -0.0141(2) 0.1527(4) 0.0424(12) Uani 1 1 d . . . C21 C 0.9562(4) -0.1431(2) 0.2039(4) 0.0429(12) Uani 1 1 d . . . H21 H 1.0053 -0.1234 0.2710 0.052 Uiso 1 1 calc R . . C22 C 1.0158(5) -0.1358(3) 0.1076(5) 0.0595(15) Uani 1 1 d . . . H22A H 0.9679 -0.1533 0.0399 0.089 Uiso 1 1 calc R . . H22B H 1.0889 -0.1574 0.1255 0.089 Uiso 1 1 calc R . . H22C H 1.0286 -0.0921 0.0958 0.089 Uiso 1 1 calc R . . C23 C 0.9486(5) -0.2117(2) 0.2285(5) 0.0551(14) Uani 1 1 d . . . H23A H 0.9057 -0.2174 0.2860 0.083 Uiso 1 1 calc R . . H23B H 1.0254 -0.2285 0.2545 0.083 Uiso 1 1 calc R . . H23C H 0.9100 -0.2332 0.1607 0.083 Uiso 1 1 calc R . . C24 C 0.7238(4) 0.0554(2) 0.1525(5) 0.0461(12) Uani 1 1 d . . . H24 H 0.7976 0.0721 0.1963 0.055 Uiso 1 1 calc R . . C25 C 0.7054(5) 0.0803(3) 0.0337(5) 0.0618(16) Uani 1 1 d . . . H25A H 0.7665 0.0657 0.0000 0.093 Uiso 1 1 calc R . . H25B H 0.7059 0.1254 0.0355 0.093 Uiso 1 1 calc R . . H25C H 0.6320 0.0659 -0.0104 0.093 Uiso 1 1 calc R . . C26 C 0.6292(5) 0.0787(3) 0.2061(5) 0.0594(15) Uani 1 1 d . . . H26A H 0.5557 0.0632 0.1643 0.089 Uiso 1 1 calc R . . H26B H 0.6284 0.1237 0.2053 0.089 Uiso 1 1 calc R . . H26C H 0.6431 0.0641 0.2830 0.089 Uiso 1 1 calc R . . C27 C 0.4347(7) -0.0938(4) 0.3240(7) 0.092(2) Uani 1 1 d . . . H27A H 0.4618 -0.0700 0.2669 0.111 Uiso 1 1 calc R . . H27B H 0.4348 -0.0665 0.3880 0.111 Uiso 1 1 calc R . . C28 C 0.3193(7) -0.1173(5) 0.2781(8) 0.106(3) Uani 1 1 d . . . H28A H 0.2607 -0.0888 0.2929 0.127 Uiso 1 1 calc R . . H28B H 0.3061 -0.1245 0.1972 0.127 Uiso 1 1 calc R . . C29 C 0.3201(8) -0.1751(6) 0.3388(9) 0.132(4) Uani 1 1 d . . . H29A H 0.2853 -0.1688 0.4031 0.159 Uiso 1 1 calc R . . H29B H 0.2752 -0.2065 0.2898 0.159 Uiso 1 1 calc R . . C30 C 0.4351(7) -0.1954(4) 0.3764(9) 0.103(3) Uani 1 1 d . . . H30A H 0.4491 -0.2321 0.3341 0.123 Uiso 1 1 calc R . . H30B H 0.4509 -0.2061 0.4562 0.123 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 Te1 0.0399(2) 0.0369(2) 0.0439(2) 0.00712(14) 0.01742(14) 0.00388(15) Ga1 0.0382(3) 0.0280(3) 0.0374(3) 0.0018(2) 0.0142(2) -0.0019(2) K1 0.0574(7) 0.0508(7) 0.0557(8) 0.0019(6) 0.0184(6) -0.0109(6) O1 0.055(2) 0.061(3) 0.117(4) 0.008(3) 0.026(3) -0.001(2) N1 0.043(2) 0.034(2) 0.038(2) 0.0026(17) 0.0159(18) -0.0050(18) N2 0.039(2) 0.032(2) 0.036(2) -0.0009(16) 0.0122(17) -0.0016(17) C1 0.049(3) 0.036(3) 0.033(3) 0.004(2) 0.016(2) -0.004(2) C2 0.043(3) 0.043(3) 0.037(3) 0.000(2) 0.018(2) -0.001(2) C3 0.051(3) 0.027(2) 0.036(3) 0.0043(19) 0.017(2) -0.003(2) C4 0.049(3) 0.036(3) 0.045(3) 0.003(2) 0.021(2) -0.006(2) C5 0.049(3) 0.040(3) 0.062(4) 0.004(3) 0.019(3) -0.011(2) C6 0.063(3) 0.035(3) 0.050(3) -0.003(2) 0.012(3) -0.009(3) C7 0.065(3) 0.033(3) 0.046(3) -0.001(2) 0.019(3) -0.001(3) C8 0.056(3) 0.029(2) 0.045(3) 0.005(2) 0.020(2) -0.002(2) C9 0.049(3) 0.046(3) 0.054(3) -0.006(2) 0.024(3) -0.004(2) C10 0.059(4) 0.060(4) 0.081(4) 0.001(3) 0.032(3) 0.002(3) C11 0.067(4) 0.082(4) 0.053(4) -0.006(3) 0.034(3) -0.006(3) C12 0.056(3) 0.030(2) 0.056(3) 0.003(2) 0.021(3) 0.008(2) C13 0.059(3) 0.051(3) 0.052(3) -0.001(3) 0.006(3) 0.009(3) C14 0.062(4) 0.055(3) 0.054(4) 0.007(3) 0.019(3) 0.015(3) C15 0.039(3) 0.036(2) 0.031(3) 0.0020(19) 0.008(2) -0.003(2) C16 0.046(3) 0.039(3) 0.033(3) 0.001(2) 0.010(2) -0.002(2) C17 0.054(3) 0.034(3) 0.049(3) 0.002(2) 0.009(3) -0.007(2) C18 0.039(3) 0.056(3) 0.063(4) 0.005(3) 0.005(3) -0.011(3) C19 0.039(3) 0.047(3) 0.056(3) 0.005(2) 0.006(2) -0.001(2) C20 0.047(3) 0.037(3) 0.045(3) 0.006(2) 0.015(2) 0.001(2) C21 0.051(3) 0.039(3) 0.038(3) -0.001(2) 0.009(2) 0.004(2) C22 0.069(4) 0.061(4) 0.055(4) 0.007(3) 0.027(3) 0.017(3) C23 0.059(3) 0.037(3) 0.064(4) -0.001(3) 0.004(3) 0.005(3) C24 0.039(3) 0.038(3) 0.063(4) 0.003(2) 0.017(2) 0.002(2) C25 0.058(3) 0.049(3) 0.077(4) 0.018(3) 0.014(3) 0.003(3) C26 0.053(3) 0.054(3) 0.074(4) 0.000(3) 0.020(3) 0.012(3) C27 0.087(5) 0.083(5) 0.109(6) 0.010(5) 0.025(5) 0.007(5) C28 0.070(5) 0.153(9) 0.097(6) 0.000(6) 0.023(5) 0.017(6) C29 0.096(7) 0.199(12) 0.104(7) 0.009(8) 0.027(6) -0.063(8) C30 0.077(5) 0.070(5) 0.169(9) 0.006(5) 0.046(6) -0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Ga1 2.6135(10) 3_756 ? Te1 Ga1 2.6217(9) . ? Te1 K1 3.5166(14) . ? Ga1 N2 1.919(4) . ? Ga1 N1 1.932(4) . ? Ga1 Te1 2.6135(10) 3_756 ? K1 O1 2.683(4) . ? K1 C17 3.139(5) . ? K1 C5 3.189(5) 3_756 ? K1 C16 3.238(5) . ? K1 C6 3.239(5) 3_756 ? K1 C4 3.272(5) 3_756 ? K1 C18 3.337(6) . ? K1 C7 3.392(5) 3_756 ? K1 C3 3.416(5) 3_756 ? K1 C8 3.505(5) 3_756 ? K1 C15 3.519(5) . ? O1 C27 1.421(9) . ? O1 C30 1.439(8) . ? N1 C1 1.392(6) . ? N1 C3 1.402(6) . ? N2 C15 1.418(6) . ? N2 C2 1.424(6) . ? C1 C2 1.335(7) . ? C3 C4 1.415(7) . ? C3 C8 1.423(7) . ? C3 K1 3.416(5) 3_756 ? C4 C5 1.397(7) . ? C4 C9 1.517(7) . ? C4 K1 3.272(5) 3_756 ? C5 C6 1.390(7) . ? C5 K1 3.189(5) 3_756 ? C6 C7 1.390(7) . ? C6 K1 3.239(5) 3_756 ? C7 C8 1.384(7) . ? C7 K1 3.392(5) 3_756 ? C8 C12 1.534(7) . ? C8 K1 3.505(5) 3_756 ? C9 C10 1.518(8) . ? C9 C11 1.548(8) . ? C12 C14 1.516(7) . ? C12 C13 1.531(8) . ? C15 C20 1.412(7) . ? C15 C16 1.414(7) . ? C16 C17 1.402(7) . ? C16 C21 1.517(7) . ? C17 C18 1.383(7) . ? C18 C19 1.385(8) . ? C19 C20 1.396(7) . ? C20 C24 1.515(7) . ? C21 C23 1.530(7) . ? C21 C22 1.536(7) . ? C24 C26 1.534(7) . ? C24 C25 1.535(8) . ? C27 C28 1.472(11) . ? C28 C29 1.463(14) . ? C29 C30 1.431(13) . ? 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 Ga1 Te1 Ga1 81.23(2) 3_756 . ? Ga1 Te1 K1 93.19(3) 3_756 . ? Ga1 Te1 K1 92.41(3) . . ? N2 Ga1 N1 87.66(16) . . ? N2 Ga1 Te1 121.84(11) . 3_756 ? N1 Ga1 Te1 110.11(12) . 3_756 ? N2 Ga1 Te1 115.50(11) . . ? N1 Ga1 Te1 124.95(11) . . ? Te1 Ga1 Te1 98.77(2) 3_756 . ? O1 K1 C17 95.48(15) . . ? O1 K1 C5 74.99(15) . 3_756 ? C17 K1 C5 137.66(14) . 3_756 ? O1 K1 C16 119.76(15) . . ? C17 K1 C16 25.33(12) . . ? C5 K1 C16 145.16(14) 3_756 . ? O1 K1 C6 82.80(15) . 3_756 ? C17 K1 C6 114.24(14) . 3_756 ? C5 K1 C6 24.97(13) 3_756 3_756 ? C16 K1 C6 120.77(13) . 3_756 ? O1 K1 C4 91.40(15) . 3_756 ? C17 K1 C4 156.00(14) . 3_756 ? C5 K1 C4 24.94(13) 3_756 3_756 ? C16 K1 C4 145.55(13) . 3_756 ? C6 K1 C4 43.93(13) 3_756 3_756 ? O1 K1 C18 77.25(15) . . ? C17 K1 C18 24.41(13) . . ? C5 K1 C18 142.37(14) 3_756 . ? C16 K1 C18 43.33(13) . . ? C6 K1 C18 126.59(14) 3_756 . ? C4 K1 C18 166.86(13) 3_756 . ? O1 K1 C7 106.34(14) . 3_756 ? C17 K1 C7 106.35(14) . 3_756 ? C5 K1 C7 42.56(13) 3_756 3_756 ? C16 K1 C7 103.40(13) . 3_756 ? C6 K1 C7 24.06(13) 3_756 3_756 ? C4 K1 C7 49.69(13) 3_756 3_756 ? C18 K1 C7 126.96(14) . 3_756 ? O1 K1 C3 115.36(14) . 3_756 ? C17 K1 C3 139.31(13) . 3_756 ? C5 K1 C3 42.82(12) 3_756 3_756 ? C16 K1 C3 121.74(12) . 3_756 ? C6 K1 C3 49.89(12) 3_756 3_756 ? C4 K1 C3 24.31(11) 3_756 3_756 ? C18 K1 C3 163.68(13) . 3_756 ? C7 K1 C3 41.76(12) 3_756 3_756 ? O1 K1 C8 122.70(13) . 3_756 ? C17 K1 C8 116.78(13) . 3_756 ? C5 K1 C8 48.89(13) 3_756 3_756 ? C16 K1 C8 104.10(12) . 3_756 ? C6 K1 C8 41.79(13) 3_756 3_756 ? C4 K1 C8 42.21(12) 3_756 3_756 ? C18 K1 C8 140.92(13) . 3_756 ? C7 K1 C8 23.08(12) 3_756 3_756 ? C3 K1 C8 23.68(11) 3_756 3_756 ? O1 K1 Te1 122.59(11) . . ? C17 K1 Te1 112.43(10) . . ? C5 K1 Te1 107.08(10) 3_756 . ? C16 K1 Te1 91.35(9) . . ? C6 K1 Te1 123.25(10) 3_756 . ? C4 K1 Te1 82.45(9) 3_756 . ? C18 K1 Te1 109.15(10) . . ? C7 K1 Te1 111.65(10) 3_756 . ? C3 K1 Te1 73.70(8) 3_756 . ? C8 K1 Te1 88.59(9) 3_756 . ? O1 K1 C15 121.89(14) . . ? C17 K1 C15 42.17(12) . . ? C5 K1 C15 162.01(13) 3_756 . ? C16 K1 C15 23.69(11) . . ? C6 K1 C15 142.02(13) 3_756 . ? C4 K1 C15 144.77(12) 3_756 . ? C18 K1 C15 48.16(12) . . ? C7 K1 C15 120.71(12) 3_756 . ? C3 K1 C15 122.26(11) 3_756 . ? C8 K1 C15 113.22(11) 3_756 . ? Te1 K1 C15 70.37(8) . . ? C27 O1 C30 107.3(5) . . ? C27 O1 K1 112.9(4) . . ? C30 O1 K1 139.4(4) . . ? C1 N1 C3 121.8(4) . . ? C1 N1 Ga1 108.2(3) . . ? C3 N1 Ga1 128.5(3) . . ? C15 N2 C2 116.7(4) . . ? C15 N2 Ga1 124.8(3) . . ? C2 N2 Ga1 107.5(3) . . ? C2 C1 N1 118.2(4) . . ? C1 C2 N2 118.2(4) . . ? N1 C3 C4 122.2(4) . . ? N1 C3 C8 118.5(4) . . ? C4 C3 C8 119.3(4) . . ? N1 C3 K1 117.0(3) . 3_756 ? C4 C3 K1 72.1(3) . 3_756 ? C8 C3 K1 81.7(3) . 3_756 ? C5 C4 C3 118.8(5) . . ? C5 C4 C9 119.6(4) . . ? C3 C4 C9 121.6(4) . . ? C5 C4 K1 74.2(3) . 3_756 ? C3 C4 K1 83.6(3) . 3_756 ? C9 C4 K1 111.9(3) . 3_756 ? C6 C5 C4 121.8(5) . . ? C6 C5 K1 79.5(3) . 3_756 ? C4 C5 K1 80.8(3) . 3_756 ? C7 C6 C5 119.1(5) . . ? C7 C6 K1 84.2(3) . 3_756 ? C5 C6 K1 75.5(3) . 3_756 ? C8 C7 C6 121.3(5) . . ? C8 C7 K1 83.1(3) . 3_756 ? C6 C7 K1 71.8(3) . 3_756 ? C7 C8 C3 119.6(5) . . ? C7 C8 C12 121.5(4) . . ? C3 C8 C12 118.5(4) . . ? C7 C8 K1 73.9(3) . 3_756 ? C3 C8 K1 74.6(3) . 3_756 ? C12 C8 K1 129.0(3) . 3_756 ? C4 C9 C10 112.1(5) . . ? C4 C9 C11 110.8(4) . . ? C10 C9 C11 110.7(4) . . ? C14 C12 C13 112.4(4) . . ? C14 C12 C8 114.5(5) . . ? C13 C12 C8 108.6(4) . . ? C20 C15 C16 120.1(4) . . ? C20 C15 N2 121.7(4) . . ? C16 C15 N2 118.1(4) . . ? C20 C15 K1 86.5(3) . . ? C16 C15 K1 67.0(3) . . ? N2 C15 K1 116.1(3) . . ? C17 C16 C15 118.6(5) . . ? C17 C16 C21 120.4(4) . . ? C15 C16 C21 120.9(4) . . ? C17 C16 K1 73.4(3) . . ? C15 C16 K1 89.3(3) . . ? C21 C16 K1 109.4(3) . . ? C18 C17 C16 121.5(5) . . ? C18 C17 K1 85.8(3) . . ? C16 C17 K1 81.3(3) . . ? C17 C18 C19 119.4(5) . . ? C17 C18 K1 69.7(3) . . ? C19 C18 K1 90.2(4) . . ? C18 C19 C20 121.6(5) . . ? C19 C20 C15 118.8(4) . . ? C19 C20 C24 119.0(5) . . ? C15 C20 C24 122.2(4) . . ? C16 C21 C23 114.9(4) . . ? C16 C21 C22 110.1(4) . . ? C23 C21 C22 108.3(4) . . ? C20 C24 C26 113.0(4) . . ? C20 C24 C25 110.5(5) . . ? C26 C24 C25 109.7(5) . . ? O1 C27 C28 107.4(7) . . ? C29 C28 C27 102.0(7) . . ? C30 C29 C28 108.8(7) . . ? C29 C30 O1 106.8(7) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.772 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.083 data_compound4 _database_code_depnum_ccdc_archive 'CCDC 268559' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H46 Ga K N2 Se2' _chemical_formula_weight 797.51 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.231(2) _cell_length_b 16.360(3) _cell_length_c 22.088(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.33(3) _cell_angle_gamma 90.00 _cell_volume 3949.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 2.671 _exptl_absorpt_correction_type milti-scan _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.771 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24621 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.41 _reflns_number_total 7200 _reflns_number_gt 5425 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+1.1455P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00088(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7200 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Se1 Se 1.12890(4) 0.75837(2) 0.325483(17) 0.03283(12) Uani 1 1 d . . . Se2 Se 0.93718(3) 0.91916(2) 0.222199(15) 0.02716(11) Uani 1 1 d . . . Ga1 Ga 1.14411(3) 0.86557(2) 0.253305(16) 0.02108(11) Uani 1 1 d . . . K1 K 0.95666(8) 1.10446(5) 0.28546(4) 0.0335(2) Uani 1 1 d . . . N1 N 1.2142(3) 0.82625(15) 0.18778(12) 0.0227(6) Uani 1 1 d . . . N2 N 1.2648(3) 0.94894(15) 0.26922(11) 0.0207(6) Uani 1 1 d . . . C1 C 1.3254(3) 0.86858(19) 0.19243(15) 0.0252(8) Uani 1 1 d . . . H1 H 1.3820 0.8525 0.1687 0.030 Uiso 1 1 calc R . . C2 C 1.3483(3) 0.93214(19) 0.23136(15) 0.0229(8) Uani 1 1 d . . . H2 H 1.4187 0.9653 0.2337 0.028 Uiso 1 1 calc R . . C3 C 1.1850(3) 0.75562(18) 0.15042(15) 0.0222(8) Uani 1 1 d . . . C4 C 1.2553(3) 0.68324(19) 0.16325(15) 0.0232(8) Uani 1 1 d . . . C5 C 1.2192(3) 0.6148(2) 0.12543(16) 0.0281(8) Uani 1 1 d . . . H5 H 1.2673 0.5665 0.1327 0.034 Uiso 1 1 calc R . . C6 C 1.1154(4) 0.6161(2) 0.07791(16) 0.0319(9) Uani 1 1 d . . . H6 H 1.0910 0.5686 0.0535 0.038 Uiso 1 1 calc R . . C7 C 1.0463(4) 0.6876(2) 0.06597(16) 0.0327(9) Uani 1 1 d . . . H7 H 0.9736 0.6880 0.0339 0.039 Uiso 1 1 calc R . . C8 C 1.0820(3) 0.7578(2) 0.10010(15) 0.0252(8) Uani 1 1 d . . . C9 C 1.3688(3) 0.6780(2) 0.21598(16) 0.0291(8) Uani 1 1 d . . . H9 H 1.3735 0.7296 0.2407 0.035 Uiso 1 1 calc R . . C10 C 1.3636(4) 0.6065(2) 0.26007(17) 0.0396(10) Uani 1 1 d . . . H10A H 1.2939 0.6139 0.2793 0.059 Uiso 1 1 calc R . . H10B H 1.4395 0.6047 0.2925 0.059 Uiso 1 1 calc R . . H10C H 1.3540 0.5552 0.2366 0.059 Uiso 1 1 calc R . . C11 C 1.4843(4) 0.6733(3) 0.1904(2) 0.0523(12) Uani 1 1 d . . . H11A H 1.4845 0.6218 0.1678 0.078 Uiso 1 1 calc R . . H11B H 1.5568 0.6759 0.2249 0.078 Uiso 1 1 calc R . . H11C H 1.4853 0.7192 0.1620 0.078 Uiso 1 1 calc R . . C12 C 1.0166(4) 0.8385(2) 0.07941(16) 0.0362(10) Uani 1 1 d . . . H12 H 1.0139 0.8700 0.1179 0.043 Uiso 1 1 calc R . . C13 C 1.0968(4) 0.8875(2) 0.04418(17) 0.0457(11) Uani 1 1 d . . . H13A H 1.1787 0.8947 0.0710 0.069 Uiso 1 1 calc R . . H13B H 1.0597 0.9412 0.0327 0.069 Uiso 1 1 calc R . . H13C H 1.1029 0.8578 0.0065 0.069 Uiso 1 1 calc R . . C14 C 0.8857(4) 0.8306(3) 0.04152(19) 0.0555(13) Uani 1 1 d . . . H14A H 0.8857 0.8063 0.0010 0.083 Uiso 1 1 calc R . . H14B H 0.8477 0.8848 0.0354 0.083 Uiso 1 1 calc R . . H14C H 0.8392 0.7956 0.0637 0.083 Uiso 1 1 calc R . . C15 C 1.2404(3) 1.03199(18) 0.28172(14) 0.0194(7) Uani 1 1 d . . . C16 C 1.2499(3) 1.05561(19) 0.34394(14) 0.0210(7) Uani 1 1 d . . . C17 C 1.2296(3) 1.13720(19) 0.35689(15) 0.0248(8) Uani 1 1 d . . . H17 H 1.2357 1.1534 0.3988 0.030 Uiso 1 1 calc R . . C18 C 1.2008(3) 1.1951(2) 0.31015(15) 0.0268(8) Uani 1 1 d . . . H18 H 1.1896 1.2507 0.3199 0.032 Uiso 1 1 calc R . . C19 C 1.1886(3) 1.17106(19) 0.24912(16) 0.0258(8) Uani 1 1 d . . . H19 H 1.1683 1.2108 0.2171 0.031 Uiso 1 1 calc R . . C20 C 1.2053(3) 1.09013(18) 0.23317(14) 0.0202(7) Uani 1 1 d . . . C21 C 1.2915(3) 0.9939(2) 0.39616(14) 0.0250(8) Uani 1 1 d . . . H21 H 1.2544 0.9400 0.3808 0.030 Uiso 1 1 calc R . . C22 C 1.4289(3) 0.9837(2) 0.41018(17) 0.0364(9) Uani 1 1 d . . . H22A H 1.4542 0.9699 0.3718 0.055 Uiso 1 1 calc R . . H22B H 1.4534 0.9396 0.4406 0.055 Uiso 1 1 calc R . . H22C H 1.4684 1.0348 0.4272 0.055 Uiso 1 1 calc R . . C23 C 1.2493(4) 1.0145(2) 0.45587(16) 0.0401(10) Uani 1 1 d . . . H23A H 1.2926 1.0632 0.4753 0.060 Uiso 1 1 calc R . . H23B H 1.2674 0.9684 0.4849 0.060 Uiso 1 1 calc R . . H23C H 1.1610 1.0250 0.4455 0.060 Uiso 1 1 calc R . . C24 C 1.1825(3) 1.0669(2) 0.16436(15) 0.0278(8) Uani 1 1 d . . . H24 H 1.1887 1.0060 0.1620 0.033 Uiso 1 1 calc R . . C25 C 1.0555(3) 1.0912(2) 0.12813(15) 0.0344(9) Uani 1 1 d . . . H25A H 0.9942 1.0697 0.1492 0.052 Uiso 1 1 calc R . . H25B H 1.0408 1.0686 0.0860 0.052 Uiso 1 1 calc R . . H25C H 1.0494 1.1509 0.1259 0.052 Uiso 1 1 calc R . . C26 C 1.2796(4) 1.1034(3) 0.13432(17) 0.0444(11) Uani 1 1 d . . . H26A H 1.2618 1.0884 0.0902 0.067 Uiso 1 1 calc R . . H26B H 1.3602 1.0821 0.1552 0.067 Uiso 1 1 calc R . . H26C H 1.2792 1.1630 0.1383 0.067 Uiso 1 1 calc R . . C27 C 1.2739(4) 0.7655(2) 0.39156(16) 0.0312(9) Uani 1 1 d . . . C28 C 1.2565(4) 0.7761(2) 0.45155(18) 0.0446(11) Uani 1 1 d . . . H28 H 1.1763 0.7834 0.4579 0.053 Uiso 1 1 calc R . . C29 C 1.3567(5) 0.7760(3) 0.5022(2) 0.0607(14) Uani 1 1 d . . . H29 H 1.3443 0.7837 0.5429 0.073 Uiso 1 1 calc R . . C30 C 1.4732(5) 0.7649(3) 0.4942(2) 0.0527(12) Uani 1 1 d . . . H30 H 1.5409 0.7638 0.5291 0.063 Uiso 1 1 calc R . . C31 C 1.4907(4) 0.7555(2) 0.4343(2) 0.0471(11) Uani 1 1 d . . . H31 H 1.5710 0.7484 0.4281 0.057 Uiso 1 1 calc R . . C32 C 1.3910(4) 0.7564(2) 0.38346(18) 0.0374(10) Uani 1 1 d . . . H32 H 1.4039 0.7506 0.3427 0.045 Uiso 1 1 calc R . . C33 C 0.8637(3) 0.90086(19) 0.29177(15) 0.0262(8) Uani 1 1 d . . . C34 C 0.7398(4) 0.8813(2) 0.27856(18) 0.0323(9) Uani 1 1 d . . . H34 H 0.6958 0.8751 0.2366 0.039 Uiso 1 1 calc R . . C35 C 0.6802(4) 0.8709(2) 0.3266(2) 0.0439(11) Uani 1 1 d . . . H35 H 0.5955 0.8578 0.3175 0.053 Uiso 1 1 calc R . . C36 C 0.7444(5) 0.8794(2) 0.3877(2) 0.0463(12) Uani 1 1 d . . . H36 H 0.7039 0.8714 0.4206 0.056 Uiso 1 1 calc R . . C37 C 0.8663(4) 0.8996(2) 0.40100(18) 0.0427(11) Uani 1 1 d . . . H37 H 0.9098 0.9058 0.4431 0.051 Uiso 1 1 calc R . . C38 C 0.9263(4) 0.9108(2) 0.35342(16) 0.0320(9) Uani 1 1 d . . . H38 H 1.0105 0.9254 0.3629 0.038 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 Se1 0.0370(3) 0.02387(19) 0.0396(2) 0.00721(16) 0.01279(18) -0.00447(16) Se2 0.0251(2) 0.0313(2) 0.0264(2) 0.00101(15) 0.00874(16) -0.00023(15) Ga1 0.0247(2) 0.01702(19) 0.0234(2) -0.00149(15) 0.00955(16) -0.00154(15) K1 0.0283(5) 0.0316(4) 0.0421(5) -0.0005(4) 0.0113(4) 0.0031(3) N1 0.0229(17) 0.0233(14) 0.0250(15) -0.0032(12) 0.0118(13) 0.0013(12) N2 0.0234(17) 0.0181(13) 0.0214(14) -0.0017(11) 0.0068(13) 0.0014(11) C1 0.024(2) 0.0259(18) 0.0280(18) 0.0025(16) 0.0118(16) 0.0052(15) C2 0.019(2) 0.0205(17) 0.0309(19) 0.0024(15) 0.0083(16) -0.0010(14) C3 0.024(2) 0.0189(16) 0.0262(18) -0.0043(14) 0.0114(16) -0.0003(14) C4 0.021(2) 0.0236(17) 0.0261(18) -0.0018(15) 0.0090(16) -0.0015(14) C5 0.033(2) 0.0194(17) 0.034(2) -0.0017(15) 0.0115(18) 0.0051(15) C6 0.039(3) 0.0290(19) 0.0278(19) -0.0103(16) 0.0086(18) -0.0055(17) C7 0.035(2) 0.038(2) 0.0245(19) -0.0064(17) 0.0034(17) -0.0006(17) C8 0.029(2) 0.0264(18) 0.0214(18) -0.0003(15) 0.0077(16) 0.0060(15) C9 0.026(2) 0.0261(18) 0.035(2) -0.0018(16) 0.0054(17) 0.0021(15) C10 0.041(3) 0.029(2) 0.041(2) 0.0048(18) -0.0050(19) 0.0046(18) C11 0.029(3) 0.064(3) 0.065(3) -0.004(2) 0.010(2) 0.008(2) C12 0.048(3) 0.038(2) 0.0197(18) -0.0025(16) 0.0023(18) 0.0158(19) C13 0.067(3) 0.033(2) 0.032(2) 0.0012(18) 0.002(2) 0.011(2) C14 0.053(3) 0.070(3) 0.038(2) 0.009(2) 0.000(2) 0.023(2) C15 0.0164(19) 0.0178(16) 0.0240(17) -0.0007(14) 0.0047(15) -0.0021(13) C16 0.0167(19) 0.0229(17) 0.0237(18) -0.0002(14) 0.0051(15) 0.0006(14) C17 0.025(2) 0.0249(18) 0.0235(18) -0.0059(15) 0.0043(15) -0.0006(15) C18 0.028(2) 0.0194(17) 0.034(2) -0.0032(16) 0.0079(17) 0.0001(15) C19 0.023(2) 0.0236(18) 0.031(2) 0.0028(15) 0.0071(16) 0.0019(15) C20 0.0181(19) 0.0213(17) 0.0226(17) -0.0011(14) 0.0074(15) -0.0023(14) C21 0.031(2) 0.0236(17) 0.0208(17) 0.0006(14) 0.0059(16) -0.0016(15) C22 0.036(3) 0.040(2) 0.031(2) 0.0085(17) 0.0022(18) 0.0031(18) C23 0.053(3) 0.042(2) 0.027(2) 0.0032(18) 0.0127(19) 0.001(2) C24 0.033(2) 0.0292(19) 0.0214(18) 0.0005(15) 0.0066(16) 0.0053(16) C25 0.036(2) 0.045(2) 0.0209(18) -0.0007(17) 0.0039(17) 0.0044(18) C26 0.040(3) 0.066(3) 0.031(2) 0.003(2) 0.015(2) 0.002(2) C27 0.042(3) 0.0215(18) 0.032(2) 0.0074(16) 0.0126(18) -0.0003(16) C28 0.056(3) 0.045(2) 0.038(2) 0.0121(19) 0.023(2) 0.007(2) C29 0.090(4) 0.061(3) 0.031(2) 0.007(2) 0.016(3) 0.006(3) C30 0.058(3) 0.053(3) 0.041(3) 0.009(2) -0.002(2) -0.003(2) C31 0.039(3) 0.044(2) 0.057(3) -0.001(2) 0.010(2) -0.001(2) C32 0.039(3) 0.039(2) 0.036(2) -0.0040(18) 0.013(2) -0.0059(18) C33 0.030(2) 0.0196(17) 0.032(2) -0.0039(15) 0.0141(17) 0.0011(15) C34 0.034(2) 0.0263(18) 0.041(2) -0.0020(17) 0.0157(19) 0.0009(16) C35 0.039(3) 0.038(2) 0.063(3) -0.005(2) 0.030(2) -0.0008(19) C36 0.070(4) 0.029(2) 0.052(3) 0.0047(19) 0.039(3) 0.000(2) C37 0.072(4) 0.029(2) 0.030(2) 0.0011(17) 0.017(2) 0.007(2) C38 0.035(2) 0.0291(19) 0.031(2) -0.0025(16) 0.0068(18) 0.0063(17) _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 Se1 C27 1.923(4) . ? Se1 Ga1 2.4026(6) . ? Se1 K1 3.4903(11) 2_745 ? Se2 C33 1.928(3) . ? Se2 Ga1 2.4301(7) . ? Se2 K1 3.3241(10) . ? Ga1 N2 1.898(3) . ? Ga1 N1 1.912(3) . ? K1 C18 3.054(4) . ? K1 C19 3.095(4) . ? K1 C5 3.098(4) 2_755 ? K1 C4 3.140(3) 2_755 ? K1 C17 3.153(4) . ? K1 C20 3.267(3) . ? K1 C6 3.305(4) 2_755 ? K1 C16 3.345(4) . ? K1 C15 3.419(3) . ? K1 C3 3.419(3) 2_755 ? K1 Se1 3.4903(11) 2_755 ? N1 C1 1.410(4) . ? N1 C3 1.414(4) . ? N2 C2 1.420(4) . ? N2 C15 1.426(4) . ? C1 C2 1.336(4) . ? C3 C8 1.408(5) . ? C3 C4 1.415(4) . ? C3 K1 3.419(3) 2_745 ? C4 C5 1.400(5) . ? C4 C9 1.518(5) . ? C4 K1 3.140(3) 2_745 ? C5 C6 1.378(5) . ? C5 K1 3.098(4) 2_745 ? C6 C7 1.394(5) . ? C6 K1 3.305(4) 2_745 ? C7 C8 1.383(5) . ? C8 C12 1.528(5) . ? C9 C11 1.532(5) . ? C9 C10 1.532(5) . ? C12 C14 1.521(6) . ? C12 C13 1.544(6) . ? C15 C16 1.408(4) . ? C15 C20 1.419(4) . ? C16 C17 1.395(4) . ? C16 C21 1.523(4) . ? C17 C18 1.383(5) . ? C18 C19 1.380(4) . ? C19 C20 1.394(4) . ? C20 C24 1.530(4) . ? C21 C22 1.512(5) . ? C21 C23 1.538(5) . ? C24 C25 1.519(5) . ? C24 C26 1.523(5) . ? C27 C32 1.376(5) . ? C27 C28 1.394(5) . ? C28 C29 1.392(6) . ? C29 C30 1.371(7) . ? C30 C31 1.389(6) . ? C31 C32 1.392(6) . ? C33 C38 1.391(5) . ? C33 C34 1.391(5) . ? C34 C35 1.390(5) . ? C35 C36 1.383(6) . ? C36 C37 1.373(6) . ? C37 C38 1.385(5) . ? 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 C27 Se1 Ga1 106.39(10) . . ? C27 Se1 K1 128.64(11) . 2_745 ? Ga1 Se1 K1 96.37(3) . 2_745 ? C33 Se2 Ga1 106.01(11) . . ? C33 Se2 K1 78.78(10) . . ? Ga1 Se2 K1 104.13(3) . . ? N2 Ga1 N1 88.91(11) . . ? N2 Ga1 Se1 123.97(8) . . ? N1 Ga1 Se1 111.19(8) . . ? N2 Ga1 Se2 112.87(8) . . ? N1 Ga1 Se2 116.19(9) . . ? Se1 Ga1 Se2 103.96(3) . . ? C18 K1 C19 25.93(8) . . ? C18 K1 C5 122.54(9) . 2_755 ? C19 K1 C5 147.51(9) . 2_755 ? C18 K1 C4 117.44(9) . 2_755 ? C19 K1 C4 134.64(9) . 2_755 ? C5 K1 C4 25.92(8) 2_755 2_755 ? C18 K1 C17 25.68(8) . . ? C19 K1 C17 44.83(9) . . ? C5 K1 C17 111.19(10) 2_755 . ? C4 K1 C17 118.70(9) 2_755 . ? C18 K1 C20 44.96(8) . . ? C19 K1 C20 25.12(8) . . ? C5 K1 C20 161.93(9) 2_755 . ? C4 K1 C20 159.74(8) 2_755 . ? C17 K1 C20 51.51(8) . . ? C18 K1 C6 101.99(10) . 2_755 ? C19 K1 C6 127.90(10) . 2_755 ? C5 K1 C6 24.58(9) 2_755 2_755 ? C4 K1 C6 44.05(9) 2_755 2_755 ? C17 K1 C6 87.00(10) . 2_755 ? C20 K1 C6 137.39(9) . 2_755 ? C18 K1 Se2 119.15(7) . . ? C19 K1 Se2 100.94(6) . . ? C5 K1 Se2 109.10(7) 2_755 . ? C4 K1 Se2 122.97(7) 2_755 . ? C17 K1 Se2 109.12(6) . . ? C20 K1 Se2 76.39(6) . . ? C6 K1 Se2 115.47(7) 2_755 . ? C18 K1 C16 44.23(8) . . ? C19 K1 C16 51.09(8) . . ? C5 K1 C16 118.87(9) 2_755 . ? C4 K1 C16 136.03(8) 2_755 . ? C17 K1 C16 24.56(8) . . ? C20 K1 C16 43.43(8) . . ? C6 K1 C16 95.02(9) 2_755 . ? Se2 K1 C16 84.72(6) . . ? C18 K1 C15 50.87(8) . . ? C19 K1 C15 43.20(8) . . ? C5 K1 C15 140.24(9) 2_755 . ? C4 K1 C15 160.00(9) 2_755 . ? C17 K1 C15 42.87(8) . . ? C20 K1 C15 24.38(7) . . ? C6 K1 C15 117.88(9) 2_755 . ? Se2 K1 C15 69.20(5) . . ? C16 K1 C15 23.99(7) . . ? C18 K1 C3 93.41(9) . 2_755 ? C19 K1 C3 110.65(8) . 2_755 ? C5 K1 C3 43.24(8) 2_755 2_755 ? C4 K1 C3 24.45(8) 2_755 2_755 ? C17 K1 C3 99.28(9) . 2_755 ? C20 K1 C3 135.69(8) . 2_755 ? C6 K1 C3 49.08(8) 2_755 2_755 ? Se2 K1 C3 147.34(6) . 2_755 ? C16 K1 C3 121.57(8) . 2_755 ? C15 K1 C3 141.82(8) . 2_755 ? C18 K1 Se1 82.29(7) . 2_755 ? C19 K1 Se1 71.09(7) . 2_755 ? C5 K1 Se1 107.09(7) 2_755 2_755 ? C4 K1 Se1 81.27(6) 2_755 2_755 ? C17 K1 Se1 107.90(7) . 2_755 ? C20 K1 Se1 85.58(6) . 2_755 ? C6 K1 Se1 120.92(7) 2_755 2_755 ? Se2 K1 Se1 112.46(3) . 2_755 ? C16 K1 Se1 122.05(6) . 2_755 ? C15 K1 Se1 109.91(6) . 2_755 ? C3 K1 Se1 71.94(6) 2_755 2_755 ? C1 N1 C3 121.8(3) . . ? C1 N1 Ga1 107.0(2) . . ? C3 N1 Ga1 129.5(2) . . ? C2 N2 C15 118.8(3) . . ? C2 N2 Ga1 106.99(19) . . ? C15 N2 Ga1 124.0(2) . . ? C2 C1 N1 117.7(3) . . ? C1 C2 N2 118.3(3) . . ? C8 C3 N1 118.5(3) . . ? C8 C3 C4 119.9(3) . . ? N1 C3 C4 121.6(3) . . ? C8 C3 K1 88.3(2) . 2_745 ? N1 C3 K1 114.64(19) . 2_745 ? C4 C3 K1 66.64(18) . 2_745 ? C5 C4 C3 118.6(3) . . ? C5 C4 C9 119.3(3) . . ? C3 C4 C9 122.1(3) . . ? C5 C4 K1 75.4(2) . 2_745 ? C3 C4 K1 88.9(2) . 2_745 ? C9 C4 K1 105.8(2) . 2_745 ? C6 C5 C4 121.4(3) . . ? C6 C5 K1 86.2(2) . 2_745 ? C4 C5 K1 78.70(19) . 2_745 ? C5 C6 C7 119.5(3) . . ? C5 C6 K1 69.26(19) . 2_745 ? C7 C6 K1 88.8(2) . 2_745 ? C8 C7 C6 121.0(3) . . ? C7 C8 C3 119.4(3) . . ? C7 C8 C12 119.7(3) . . ? C3 C8 C12 120.6(3) . . ? C4 C9 C11 110.6(3) . . ? C4 C9 C10 112.5(3) . . ? C11 C9 C10 110.9(3) . . ? C14 C12 C8 115.4(3) . . ? C14 C12 C13 111.7(3) . . ? C8 C12 C13 107.7(3) . . ? C16 C15 C20 119.9(3) . . ? C16 C15 N2 118.4(3) . . ? C20 C15 N2 121.7(3) . . ? C16 C15 K1 75.08(19) . . ? C20 C15 K1 71.81(18) . . ? N2 C15 K1 123.9(2) . . ? C17 C16 C15 118.9(3) . . ? C17 C16 C21 121.0(3) . . ? C15 C16 C21 119.9(3) . . ? C17 C16 K1 69.98(19) . . ? C15 C16 K1 80.92(19) . . ? C21 C16 K1 123.6(2) . . ? C18 C17 C16 121.5(3) . . ? C18 C17 K1 73.1(2) . . ? C16 C17 K1 85.5(2) . . ? C19 C18 C17 119.2(3) . . ? C19 C18 K1 78.7(2) . . ? C17 C18 K1 81.2(2) . . ? C18 C19 C20 121.9(3) . . ? C18 C19 K1 75.3(2) . . ? C20 C19 K1 84.3(2) . . ? C19 C20 C15 118.4(3) . . ? C19 C20 C24 119.1(3) . . ? C15 C20 C24 122.5(3) . . ? C19 C20 K1 70.55(19) . . ? C15 C20 K1 83.81(19) . . ? C24 C20 K1 114.1(2) . . ? C22 C21 C16 110.4(3) . . ? C22 C21 C23 110.5(3) . . ? C16 C21 C23 113.8(3) . . ? C25 C24 C26 110.3(3) . . ? C25 C24 C20 112.3(3) . . ? C26 C24 C20 111.3(3) . . ? C32 C27 C28 119.0(4) . . ? C32 C27 Se1 124.2(3) . . ? C28 C27 Se1 116.7(3) . . ? C29 C28 C27 119.9(4) . . ? C30 C29 C28 121.0(4) . . ? C29 C30 C31 119.1(4) . . ? C30 C31 C32 120.2(4) . . ? C27 C32 C31 120.8(4) . . ? C38 C33 C34 119.2(3) . . ? C38 C33 Se2 123.3(3) . . ? C34 C33 Se2 117.4(3) . . ? C35 C34 C33 120.2(4) . . ? C36 C35 C34 119.9(4) . . ? C37 C36 C35 120.2(4) . . ? C36 C37 C38 120.4(4) . . ? C37 C38 C33 120.2(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.41 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.392 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.080 data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 268560' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H104 Ga2 K2 N8 O2' _chemical_formula_weight 1235.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 12.498(3) _cell_length_b 12.816(3) _cell_length_c 12.885(3) _cell_angle_alpha 83.87(3) _cell_angle_beta 65.85(3) _cell_angle_gamma 64.02(3) _cell_volume 1686.3(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 0.968 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.798 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17102 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0800 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _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 3.05 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5836 _reflns_number_gt 4475 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+4.3510P] 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 5836 _refine_ls_number_parameters 364 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1670 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.37424(5) 0.54543(4) 0.03171(4) 0.02898(18) Uani 1 1 d . . . K1 K 0.34752(12) 0.71759(10) -0.15840(10) 0.0493(3) Uani 1 1 d . . . O1 O 0.4844(3) 0.4344(3) 0.0868(3) 0.0337(8) Uani 1 1 d . . . N1 N 0.2664(4) 0.5284(3) -0.0310(3) 0.0344(9) Uani 1 1 d . . . N2 N 0.2321(4) 0.6932(3) 0.1050(3) 0.0296(8) Uani 1 1 d . . . N3 N 0.4619(6) 0.8579(5) -0.3283(5) 0.0728(16) Uani 1 1 d . . . N4 N 0.1981(5) 0.8716(5) -0.2794(4) 0.0616(14) Uani 1 1 d . . . C1 C 0.1428(5) 0.6238(4) 0.0144(4) 0.0340(11) Uani 1 1 d . . . H1 H 0.0735 0.6291 -0.0025 0.041 Uiso 1 1 calc R . . C2 C 0.1259(4) 0.7073(4) 0.0827(4) 0.0318(10) Uani 1 1 d . . . H2 H 0.0445 0.7737 0.1147 0.038 Uiso 1 1 calc R . . C3 C 0.2044(4) 0.7620(4) 0.2017(4) 0.0306(10) Uani 1 1 d . . . C4 C 0.1242(5) 0.7528(4) 0.3123(4) 0.0365(11) Uani 1 1 d . . . C5 C 0.0968(5) 0.8261(5) 0.4013(5) 0.0480(14) Uani 1 1 d . . . H5 H 0.0414 0.8210 0.4766 0.058 Uiso 1 1 calc R . . C6 C 0.1472(5) 0.9050(5) 0.3837(5) 0.0519(15) Uani 1 1 d . . . H6 H 0.1254 0.9550 0.4458 0.062 Uiso 1 1 calc R . . C7 C 0.2300(5) 0.9115(5) 0.2751(5) 0.0485(14) Uani 1 1 d . . . H7 H 0.2665 0.9653 0.2630 0.058 Uiso 1 1 calc R . . C8 C 0.2609(5) 0.8403(4) 0.1826(4) 0.0370(11) Uani 1 1 d . . . C9 C 0.0726(5) 0.6605(5) 0.3387(5) 0.0461(13) Uani 1 1 d . . . H9 H 0.0958 0.6215 0.2643 0.055 Uiso 1 1 calc R . . C10 C 0.1412(8) 0.5680(6) 0.4041(7) 0.085(2) Uani 1 1 d . . . H10A H 0.2354 0.5331 0.3585 0.128 Uiso 1 1 calc R . . H10B H 0.1102 0.5074 0.4189 0.128 Uiso 1 1 calc R . . H10C H 0.1218 0.6043 0.4767 0.128 Uiso 1 1 calc R . . C11 C -0.0745(6) 0.7120(6) 0.4028(7) 0.075(2) Uani 1 1 d . . . H11A H -0.0997 0.7480 0.4776 0.113 Uiso 1 1 calc R . . H11B H -0.1031 0.6502 0.4131 0.113 Uiso 1 1 calc R . . H11C H -0.1154 0.7712 0.3590 0.113 Uiso 1 1 calc R . . C12 C 0.3458(5) 0.8526(5) 0.0627(5) 0.0472(14) Uani 1 1 d . . . H12 H 0.3932 0.7746 0.0186 0.057 Uiso 1 1 calc R . . C13 C 0.2595(7) 0.9372(5) 0.0057(6) 0.071(2) Uani 1 1 d U . . H13A H 0.1929 0.9130 0.0120 0.107 Uiso 1 1 calc R . . H13B H 0.3129 0.9372 -0.0751 0.107 Uiso 1 1 calc R . . H13C H 0.2172 1.0159 0.0436 0.107 Uiso 1 1 calc R . . C14 C 0.4480(7) 0.8904(6) 0.0595(7) 0.081(2) Uani 1 1 d U . . H14A H 0.4043 0.9705 0.0942 0.121 Uiso 1 1 calc R . . H14B H 0.5079 0.8863 -0.0199 0.121 Uiso 1 1 calc R . . H14C H 0.4970 0.8384 0.1022 0.121 Uiso 1 1 calc R . . C15 C 0.2689(5) 0.4255(4) -0.0659(4) 0.0394(12) Uani 1 1 d . . . C16 C 0.2025(5) 0.3668(4) 0.0142(5) 0.0412(12) Uani 1 1 d . . . C17 C 0.1985(6) 0.2726(5) -0.0257(6) 0.0528(15) Uani 1 1 d . . . H17 H 0.1521 0.2339 0.0272 0.063 Uiso 1 1 calc R . . C18 C 0.2599(7) 0.2337(5) -0.1398(6) 0.0643(18) Uani 1 1 d . . . H18 H 0.2528 0.1711 -0.1653 0.077 Uiso 1 1 calc R . . C19 C 0.3317(8) 0.2862(5) -0.2165(6) 0.070(2) Uani 1 1 d . . . H19 H 0.3767 0.2571 -0.2946 0.084 Uiso 1 1 calc R . . C20 C 0.3399(6) 0.3814(5) -0.1821(5) 0.0524(15) Uani 1 1 d . . . C21 C 0.4247(8) 0.4383(5) -0.2663(5) 0.073(2) Uani 1 1 d . . . H21 H 0.4485 0.4761 -0.2207 0.087 Uiso 1 1 calc R . . C22 C 0.3412(7) 0.5312(7) -0.3134(7) 0.091(2) Uani 1 1 d . . . H22A H 0.3846 0.5803 -0.3541 0.136 Uiso 1 1 calc R . . H22B H 0.2583 0.5788 -0.2512 0.136 Uiso 1 1 calc R . . H22C H 0.3250 0.4967 -0.3664 0.136 Uiso 1 1 calc R . . C23 C 0.5498(7) 0.3555(7) -0.3586(7) 0.090(2) Uani 1 1 d . . . H23A H 0.5296 0.3226 -0.4096 0.135 Uiso 1 1 calc R . . H23B H 0.6002 0.2926 -0.3237 0.135 Uiso 1 1 calc R . . H23C H 0.6007 0.3978 -0.4026 0.135 Uiso 1 1 calc R . . C24 C 0.1415(5) 0.4013(5) 0.1410(4) 0.0428(12) Uani 1 1 d . . . H24 H 0.1546 0.4707 0.1505 0.051 Uiso 1 1 calc R . . C25 C 0.2141(8) 0.3049(6) 0.2004(6) 0.086(2) Uani 1 1 d . . . H25A H 0.2013 0.2357 0.1953 0.129 Uiso 1 1 calc R . . H25B H 0.1804 0.3315 0.2808 0.129 Uiso 1 1 calc R . . H25C H 0.3072 0.2855 0.1632 0.129 Uiso 1 1 calc R . . C26 C -0.0037(6) 0.4381(6) 0.1952(6) 0.0659(18) Uani 1 1 d . . . H26A H -0.0209 0.3725 0.1870 0.099 Uiso 1 1 calc R . . H26B H -0.0463 0.5035 0.1572 0.099 Uiso 1 1 calc R . . H26C H -0.0378 0.4621 0.2764 0.099 Uiso 1 1 calc R . . C27 C 0.1235(8) 0.8259(8) -0.3056(8) 0.094(3) Uani 1 1 d U . . H27A H 0.0636 0.8871 -0.3342 0.140 Uiso 1 1 calc R . . H27B H 0.0736 0.7998 -0.2364 0.140 Uiso 1 1 calc R . . H27C H 0.1828 0.7600 -0.3640 0.140 Uiso 1 1 calc R . . C28 C 0.1076(8) 0.9678(7) -0.1951(7) 0.096(3) Uani 1 1 d U . . H28A H 0.1551 0.9971 -0.1712 0.144 Uiso 1 1 calc R . . H28B H 0.0528 0.9424 -0.1290 0.144 Uiso 1 1 calc R . . H28C H 0.0527 1.0299 -0.2273 0.144 Uiso 1 1 calc R . . C29 C 0.2727(8) 0.9094(7) -0.3798(7) 0.080(2) Uani 1 1 d U . . H29A H 0.2115 0.9788 -0.4015 0.096 Uiso 1 1 calc R . . H29B H 0.3179 0.8471 -0.4426 0.096 Uiso 1 1 calc R . . C30 C 0.3726(8) 0.9396(8) -0.3715(7) 0.086(2) Uani 1 1 d U . . H30A H 0.4236 0.9543 -0.4488 0.103 Uiso 1 1 calc R . . H30B H 0.3256 1.0138 -0.3228 0.103 Uiso 1 1 calc R . . C31 C 0.5525(8) 0.7575(8) -0.4026(8) 0.101(3) Uani 1 1 d U . . H31A H 0.5068 0.7170 -0.4141 0.152 Uiso 1 1 calc R . . H31B H 0.6134 0.7059 -0.3697 0.152 Uiso 1 1 calc R . . H31C H 0.6006 0.7792 -0.4761 0.152 Uiso 1 1 calc R . . C32 C 0.5349(8) 0.9109(8) -0.3076(7) 0.091(2) Uani 1 1 d U . . H32A H 0.5893 0.8571 -0.2700 0.136 Uiso 1 1 calc R . . H32B H 0.4739 0.9837 -0.2584 0.136 Uiso 1 1 calc R . . H32C H 0.5903 0.9274 -0.3805 0.136 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 0.0269(3) 0.0256(3) 0.0318(3) 0.0017(2) -0.0103(2) -0.0104(2) K1 0.0482(7) 0.0447(7) 0.0444(7) 0.0157(5) -0.0194(6) -0.0133(6) O1 0.0297(17) 0.0324(18) 0.0338(18) 0.0069(14) -0.0102(14) -0.0125(14) N1 0.029(2) 0.032(2) 0.039(2) -0.0038(17) -0.0121(18) -0.0110(18) N2 0.029(2) 0.0253(19) 0.031(2) 0.0028(16) -0.0110(17) -0.0097(16) N3 0.069(4) 0.074(4) 0.074(4) 0.010(3) -0.027(3) -0.033(3) N4 0.063(3) 0.061(3) 0.058(3) 0.006(3) -0.026(3) -0.024(3) C1 0.033(3) 0.034(3) 0.038(3) 0.006(2) -0.017(2) -0.016(2) C2 0.025(2) 0.029(2) 0.034(3) 0.005(2) -0.010(2) -0.008(2) C3 0.028(2) 0.022(2) 0.033(3) -0.0019(19) -0.009(2) -0.0051(19) C4 0.032(3) 0.033(3) 0.036(3) 0.002(2) -0.010(2) -0.009(2) C5 0.042(3) 0.055(3) 0.034(3) -0.004(2) -0.010(2) -0.013(3) C6 0.042(3) 0.052(3) 0.050(4) -0.018(3) -0.017(3) -0.008(3) C7 0.041(3) 0.038(3) 0.064(4) -0.012(3) -0.018(3) -0.013(2) C8 0.030(3) 0.030(3) 0.043(3) -0.004(2) -0.009(2) -0.010(2) C9 0.048(3) 0.043(3) 0.039(3) 0.009(2) -0.007(3) -0.022(3) C10 0.104(6) 0.065(5) 0.102(6) 0.049(4) -0.054(5) -0.047(5) C11 0.056(4) 0.073(5) 0.085(5) 0.007(4) -0.009(4) -0.037(4) C12 0.043(3) 0.034(3) 0.052(3) -0.001(2) -0.001(3) -0.022(2) C13 0.072(4) 0.046(3) 0.058(4) 0.017(3) -0.004(3) -0.018(3) C14 0.071(4) 0.070(4) 0.097(5) -0.014(4) -0.001(4) -0.052(4) C15 0.041(3) 0.036(3) 0.049(3) 0.001(2) -0.027(3) -0.014(2) C16 0.042(3) 0.037(3) 0.052(3) 0.005(2) -0.026(3) -0.018(2) C17 0.056(4) 0.045(3) 0.076(4) 0.009(3) -0.035(3) -0.030(3) C18 0.082(5) 0.044(3) 0.082(5) -0.008(3) -0.041(4) -0.029(3) C19 0.105(6) 0.048(4) 0.057(4) -0.008(3) -0.035(4) -0.029(4) C20 0.066(4) 0.041(3) 0.047(3) -0.001(3) -0.020(3) -0.022(3) C21 0.116(6) 0.043(4) 0.038(3) -0.007(3) -0.016(4) -0.030(4) C22 0.062(5) 0.094(6) 0.096(6) 0.012(5) -0.023(4) -0.026(4) C23 0.072(5) 0.089(6) 0.081(5) 0.007(4) -0.024(4) -0.018(4) C24 0.049(3) 0.042(3) 0.045(3) 0.009(2) -0.021(3) -0.025(3) C25 0.106(6) 0.068(5) 0.067(5) 0.013(4) -0.047(5) -0.014(4) C26 0.057(4) 0.083(5) 0.060(4) 0.005(3) -0.017(3) -0.039(4) C27 0.088(5) 0.097(5) 0.113(6) 0.026(4) -0.055(5) -0.045(4) C28 0.077(5) 0.095(5) 0.083(5) -0.007(4) -0.032(4) -0.006(4) C29 0.089(5) 0.086(5) 0.090(5) 0.030(4) -0.047(4) -0.053(4) C30 0.093(5) 0.108(5) 0.087(5) 0.046(4) -0.055(4) -0.060(4) C31 0.076(5) 0.108(6) 0.097(6) 0.001(5) -0.017(4) -0.036(5) C32 0.083(5) 0.111(6) 0.094(5) 0.030(4) -0.043(4) -0.053(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 O1 1.814(3) . ? Ga1 O1 1.905(3) 2_665 ? Ga1 N2 1.923(4) . ? Ga1 N1 1.924(4) . ? Ga1 K1 3.1383(16) . ? K1 O1 2.584(3) 2_665 ? K1 N4 2.883(5) . ? K1 N3 2.987(6) . ? K1 N1 3.088(4) . ? K1 N2 3.140(4) . ? K1 C1 3.226(5) . ? K1 C2 3.245(5) . ? O1 Ga1 1.905(3) 2_665 ? O1 K1 2.584(3) 2_665 ? N1 C1 1.408(6) . ? N1 C15 1.423(6) . ? N2 C2 1.403(6) . ? N2 C3 1.437(6) . ? N3 C31 1.398(10) . ? N3 C30 1.419(9) . ? N3 C32 1.465(9) . ? N4 C28 1.427(9) . ? N4 C29 1.433(9) . ? N4 C27 1.451(9) . ? C1 C2 1.346(7) . ? C3 C4 1.396(7) . ? C3 C8 1.411(7) . ? C4 C5 1.393(7) . ? C4 C9 1.529(7) . ? C5 C6 1.364(8) . ? C6 C7 1.379(8) . ? C7 C8 1.395(7) . ? C8 C12 1.513(7) . ? C9 C11 1.519(8) . ? C9 C10 1.528(8) . ? C12 C13 1.528(9) . ? C12 C14 1.538(8) . ? C15 C16 1.413(8) . ? C15 C20 1.416(8) . ? C16 C17 1.389(7) . ? C16 C24 1.513(7) . ? C17 C18 1.377(9) . ? C18 C19 1.377(10) . ? C19 C20 1.399(8) . ? C20 C21 1.549(9) . ? C21 C22 1.466(10) . ? C21 C23 1.510(9) . ? C24 C26 1.512(8) . ? C24 C25 1.522(8) . ? C29 C30 1.503(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga1 O1 91.00(14) . 2_665 ? O1 Ga1 N2 129.19(15) . . ? O1 Ga1 N2 111.07(15) 2_665 . ? O1 Ga1 N1 128.02(16) . . ? O1 Ga1 N1 110.00(16) 2_665 . ? N2 Ga1 N1 87.67(16) . . ? O1 Ga1 K1 146.30(10) . . ? O1 Ga1 K1 55.33(10) 2_665 . ? N2 Ga1 K1 72.23(12) . . ? N1 Ga1 K1 70.59(13) . . ? O1 K1 N4 169.46(14) 2_665 . ? O1 K1 N3 111.21(14) 2_665 . ? N4 K1 N3 61.90(16) . . ? O1 K1 N1 66.46(10) 2_665 . ? N4 K1 N1 118.14(14) . . ? N3 K1 N1 166.46(15) . . ? O1 K1 Ga1 37.33(7) 2_665 . ? N4 K1 Ga1 150.89(12) . . ? N3 K1 Ga1 146.88(13) . . ? N1 K1 Ga1 35.99(7) . . ? O1 K1 N2 66.09(10) 2_665 . ? N4 K1 N2 124.38(14) . . ? N3 K1 N2 141.92(15) . . ? N1 K1 N2 50.65(10) . . ? Ga1 K1 N2 35.67(7) . . ? O1 K1 C1 86.81(12) 2_665 . ? N4 K1 C1 100.50(15) . . ? N3 K1 C1 161.91(15) . . ? N1 K1 C1 25.64(11) . . ? Ga1 K1 C1 50.42(9) . . ? N2 K1 C1 43.43(11) . . ? O1 K1 C2 86.51(11) 2_665 . ? N4 K1 C2 103.26(14) . . ? N3 K1 C2 149.32(15) . . ? N1 K1 C2 43.67(11) . . ? Ga1 K1 C2 50.23(9) . . ? N2 K1 C2 25.32(11) . . ? C1 K1 C2 24.01(12) . . ? Ga1 O1 Ga1 89.00(14) . 2_665 ? Ga1 O1 K1 176.04(17) . 2_665 ? Ga1 O1 K1 87.34(12) 2_665 2_665 ? C1 N1 C15 115.6(4) . . ? C1 N1 Ga1 108.0(3) . . ? C15 N1 Ga1 129.6(3) . . ? C1 N1 K1 82.7(3) . . ? C15 N1 K1 134.5(3) . . ? Ga1 N1 K1 73.42(12) . . ? C2 N2 C3 117.2(4) . . ? C2 N2 Ga1 108.2(3) . . ? C3 N2 Ga1 130.4(3) . . ? C2 N2 K1 81.5(2) . . ? C3 N2 K1 131.8(3) . . ? Ga1 N2 K1 72.11(12) . . ? C31 N3 C30 113.1(7) . . ? C31 N3 C32 107.5(7) . . ? C30 N3 C32 110.0(6) . . ? C31 N3 K1 90.4(5) . . ? C30 N3 K1 112.2(4) . . ? C32 N3 K1 122.0(4) . . ? C28 N4 C29 110.0(6) . . ? C28 N4 C27 107.4(6) . . ? C29 N4 C27 110.5(6) . . ? C28 N4 K1 100.9(4) . . ? C29 N4 K1 114.0(4) . . ? C27 N4 K1 113.5(4) . . ? C2 C1 N1 118.0(4) . . ? C2 C1 K1 78.8(3) . . ? N1 C1 K1 71.7(3) . . ? C1 C2 N2 118.0(4) . . ? C1 C2 K1 77.2(3) . . ? N2 C2 K1 73.2(2) . . ? C4 C3 C8 120.0(4) . . ? C4 C3 N2 121.7(4) . . ? C8 C3 N2 118.3(4) . . ? C5 C4 C3 118.6(5) . . ? C5 C4 C9 119.5(5) . . ? C3 C4 C9 121.8(4) . . ? C6 C5 C4 122.1(5) . . ? C5 C6 C7 119.4(5) . . ? C6 C7 C8 121.0(5) . . ? C7 C8 C3 118.8(5) . . ? C7 C8 C12 120.8(5) . . ? C3 C8 C12 120.3(4) . . ? C11 C9 C10 111.5(5) . . ? C11 C9 C4 112.7(5) . . ? C10 C9 C4 109.3(5) . . ? C8 C12 C13 109.3(5) . . ? C8 C12 C14 112.8(5) . . ? C13 C12 C14 111.3(5) . . ? C16 C15 C20 120.1(5) . . ? C16 C15 N1 120.8(5) . . ? C20 C15 N1 119.1(5) . . ? C17 C16 C15 118.5(5) . . ? C17 C16 C24 120.0(5) . . ? C15 C16 C24 121.5(5) . . ? C18 C17 C16 121.9(6) . . ? C17 C18 C19 119.4(6) . . ? C18 C19 C20 121.6(6) . . ? C19 C20 C15 118.2(6) . . ? C19 C20 C21 122.3(5) . . ? C15 C20 C21 119.6(5) . . ? C22 C21 C23 112.2(6) . . ? C22 C21 C20 106.8(7) . . ? C23 C21 C20 115.4(6) . . ? C26 C24 C16 113.4(5) . . ? C26 C24 C25 112.7(5) . . ? C16 C24 C25 110.0(5) . . ? N4 C29 C30 116.8(6) . . ? N3 C30 C29 118.2(7) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.730 #(near Ga1) _refine_diff_density_min -0.595 _refine_diff_density_rms 0.092