Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Cameron Jones' 'Robert J. Baker' 'James Platts' _publ_contact_author_name 'Prof Cameron Jones' _publ_contact_author_address ; Department of Chemistry Cardiff University P.O. Box 912, Park Place Cardiff CF10 3TB UNITED KINGDOM ; _publ_contact_author_email JONESCA6@CARDIFF.AC.UK _publ_section_title ; Synthesis, Structural and Theoretical Studies of an Iron-Gallium(I) Heterocycle Complex: Analogies with N-Heterocyclic Carbene Chemistry ; data_compound_5 _database_code_CSD 211975 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H52 Fe Ga K N4 O4' _chemical_formula_weight 769.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' K K 0.2009 0.2494 '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 14.558(3) _cell_length_b 14.257(3) _cell_length_c 19.171(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.50(3) _cell_angle_gamma 90.00 _cell_volume 3966.7(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 prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7969 _exptl_absorpt_correction_T_max 0.9003 _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 27550 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.02 _reflns_number_total 7785 _reflns_number_gt 5675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT (Hooft, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+6.3350P] 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 'calculated (riding model)' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7785 _refine_ls_number_parameters 438 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.051 _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 Ga1 Ga 0.95342(3) 0.27657(3) 0.13735(2) 0.02123(14) Uani 1 1 d . . . Fe1 Fe 0.83468(3) 0.18412(4) 0.08940(3) 0.02342(16) Uani 1 1 d . . . K1 K 0.60980(7) 0.42835(7) 0.21562(6) 0.0463(3) Uani 1 1 d . . . O1 O 0.6825(2) 0.0803(2) 0.01622(17) 0.0490(8) Uani 1 1 d . . . O2 O 0.9203(2) 0.0245(2) 0.16460(16) 0.0444(8) Uani 1 1 d . . . O3 O 0.9026(2) 0.2546(3) -0.04078(16) 0.0583(10) Uani 1 1 d . . . O4 O 0.7241(2) 0.2994(2) 0.17668(18) 0.0502(9) Uani 1 1 d . . . N1 N 0.96021(19) 0.4052(2) 0.15917(16) 0.0245(7) Uani 1 1 d . . . N2 N 1.08064(19) 0.2693(2) 0.16028(15) 0.0221(6) Uani 1 1 d . . . N3 N 0.4989(3) 0.3402(3) 0.1052(2) 0.0535(11) Uani 1 1 d . . . N4 N 0.4765(3) 0.3049(3) 0.2597(2) 0.0471(10) Uani 1 1 d . . . C1 C 1.0520(2) 0.4281(3) 0.18034(19) 0.0240(8) Uani 1 1 d . . . H1 H 1.0696 0.4901 0.1937 0.029 Uiso 1 1 calc R . . C2 C 1.1137(2) 0.3581(3) 0.18072(19) 0.0254(8) Uani 1 1 d . . . H2 H 1.1771 0.3684 0.1943 0.030 Uiso 1 1 calc R . . C3 C 0.8897(2) 0.4684(3) 0.17556(19) 0.0247(8) Uani 1 1 d . . . C4 C 0.8378(2) 0.5146(3) 0.1213(2) 0.0272(8) Uani 1 1 d . . . C5 C 0.7701(3) 0.5782(3) 0.1388(2) 0.0347(10) Uani 1 1 d . . . H5 H 0.7345 0.6103 0.1026 0.042 Uiso 1 1 calc R . . C6 C 0.7541(3) 0.5953(3) 0.2080(2) 0.0386(11) Uani 1 1 d . . . H6 H 0.7090 0.6400 0.2191 0.046 Uiso 1 1 calc R . . C7 C 0.8036(3) 0.5473(3) 0.2604(2) 0.0359(10) Uani 1 1 d . . . H7 H 0.7915 0.5585 0.3077 0.043 Uiso 1 1 calc R . . C8 C 0.8713(3) 0.4826(3) 0.2460(2) 0.0287(9) Uani 1 1 d . . . C9 C 0.8586(3) 0.5025(3) 0.0452(2) 0.0325(9) Uani 1 1 d . . . H9 H 0.8970 0.4447 0.0423 0.039 Uiso 1 1 calc R . . C10 C 0.7727(4) 0.4895(6) -0.0040(3) 0.083(2) Uani 1 1 d . . . H10A H 0.7362 0.5473 -0.0054 0.125 Uiso 1 1 calc R . . H10B H 0.7359 0.4377 0.0127 0.125 Uiso 1 1 calc R . . H10C H 0.7905 0.4750 -0.0511 0.125 Uiso 1 1 calc R . . C11 C 0.9157(4) 0.5850(4) 0.0228(3) 0.0590(14) Uani 1 1 d . . . H11A H 0.9292 0.5768 -0.0261 0.088 Uiso 1 1 calc R . . H11B H 0.9736 0.5879 0.0525 0.088 Uiso 1 1 calc R . . H11C H 0.8812 0.6433 0.0276 0.088 Uiso 1 1 calc R . . C12 C 0.9201(3) 0.4267(3) 0.3050(2) 0.0348(10) Uani 1 1 d . . . H12 H 0.9614 0.3806 0.2836 0.042 Uiso 1 1 calc R . . C13 C 0.9806(3) 0.4884(4) 0.3555(2) 0.0515(12) Uani 1 1 d . . . H13A H 1.0271 0.5203 0.3298 0.077 Uiso 1 1 calc R . . H13B H 1.0112 0.4491 0.3923 0.077 Uiso 1 1 calc R . . H13C H 0.9421 0.5352 0.3767 0.077 Uiso 1 1 calc R . . C14 C 0.8509(4) 0.3708(4) 0.3451(3) 0.0533(13) Uani 1 1 d . . . H14A H 0.8092 0.4142 0.3665 0.080 Uiso 1 1 calc R . . H14B H 0.8843 0.3332 0.3816 0.080 Uiso 1 1 calc R . . H14C H 0.8151 0.3292 0.3126 0.080 Uiso 1 1 calc R . . C15 C 1.1399(2) 0.1910(3) 0.17526(19) 0.0231(8) Uani 1 1 d . . . C16 C 1.1758(2) 0.1409(3) 0.1200(2) 0.0258(8) Uani 1 1 d . . . C17 C 1.2362(3) 0.0667(3) 0.1368(2) 0.0339(10) Uani 1 1 d . . . H17 H 1.2610 0.0321 0.1003 0.041 Uiso 1 1 calc R . . C18 C 1.2606(3) 0.0427(3) 0.2056(2) 0.0373(10) Uani 1 1 d . . . H18 H 1.3036 -0.0064 0.2160 0.045 Uiso 1 1 calc R . . C19 C 1.2227(3) 0.0897(3) 0.2591(2) 0.0362(10) Uani 1 1 d . . . H19 H 1.2388 0.0715 0.3062 0.043 Uiso 1 1 calc R . . C20 C 1.1613(3) 0.1635(3) 0.2455(2) 0.0292(9) Uani 1 1 d . . . C21 C 1.1488(3) 0.1634(3) 0.0441(2) 0.0287(9) Uani 1 1 d . . . H21 H 1.1105 0.2217 0.0429 0.034 Uiso 1 1 calc R . . C22 C 1.0895(3) 0.0851(3) 0.0106(2) 0.0416(11) Uani 1 1 d . . . H22A H 1.1250 0.0267 0.0117 0.062 Uiso 1 1 calc R . . H22B H 1.0705 0.1017 -0.0380 0.062 Uiso 1 1 calc R . . H22C H 1.0347 0.0766 0.0366 0.062 Uiso 1 1 calc R . . C23 C 1.2317(3) 0.1823(4) 0.0017(2) 0.0456(11) Uani 1 1 d . . . H23A H 1.2666 0.2358 0.0219 0.068 Uiso 1 1 calc R . . H23B H 1.2102 0.1963 -0.0468 0.068 Uiso 1 1 calc R . . H23C H 1.2715 0.1267 0.0030 0.068 Uiso 1 1 calc R . . C24 C 1.1132(3) 0.2089(3) 0.3044(2) 0.0365(10) Uani 1 1 d . . . H24 H 1.0860 0.2693 0.2861 0.044 Uiso 1 1 calc R . . C25 C 1.1758(4) 0.2317(5) 0.3696(3) 0.0778(19) Uani 1 1 d . . . H25A H 1.1998 0.1734 0.3910 0.117 Uiso 1 1 calc R . . H25B H 1.1406 0.2657 0.4030 0.117 Uiso 1 1 calc R . . H25C H 1.2271 0.2708 0.3566 0.117 Uiso 1 1 calc R . . C26 C 1.0340(4) 0.1470(4) 0.3236(3) 0.0743(18) Uani 1 1 d . . . H26A H 0.9940 0.1328 0.2815 0.111 Uiso 1 1 calc R . . H26B H 0.9984 0.1798 0.3575 0.111 Uiso 1 1 calc R . . H26C H 1.0586 0.0884 0.3444 0.111 Uiso 1 1 calc R . . C27 C 0.7424(3) 0.1210(3) 0.0451(2) 0.0316(9) Uani 1 1 d . . . C28 C 0.8895(3) 0.0887(3) 0.1333(2) 0.0311(9) Uani 1 1 d . . . C29 C 0.8765(3) 0.2275(3) 0.0106(2) 0.0345(10) Uani 1 1 d . . . C30 C 0.7687(3) 0.2549(3) 0.1411(2) 0.0325(9) Uani 1 1 d . . . C31 C 0.4686(7) 0.4069(7) 0.0535(5) 0.151(4) Uani 1 1 d U . . H31A H 0.5199 0.4482 0.0439 0.226 Uiso 1 1 calc R . . H31B H 0.4184 0.4444 0.0704 0.226 Uiso 1 1 calc R . . H31C H 0.4464 0.3741 0.0105 0.226 Uiso 1 1 calc R . . C32 C 0.5425(6) 0.2681(6) 0.0693(5) 0.117(3) Uani 1 1 d U . . H32A H 0.4959 0.2314 0.0415 0.176 Uiso 1 1 calc R . . H32B H 0.5764 0.2269 0.1033 0.176 Uiso 1 1 calc R . . H32C H 0.5855 0.2959 0.0383 0.176 Uiso 1 1 calc R . . C33 C 0.4174(7) 0.3131(8) 0.1363(5) 0.138(3) Uani 1 1 d U . . H33A H 0.3784 0.2772 0.1010 0.166 Uiso 1 1 calc R . . H33B H 0.3832 0.3708 0.1466 0.166 Uiso 1 1 calc R . . C34 C 0.4277(5) 0.2569(5) 0.2005(4) 0.0827(19) Uani 1 1 d U . . H34A H 0.3657 0.2388 0.2137 0.099 Uiso 1 1 calc R . . H34B H 0.4613 0.1985 0.1908 0.099 Uiso 1 1 calc R . . C35 C 0.4145(4) 0.3608(4) 0.2981(3) 0.0719(17) Uani 1 1 d U . . H35A H 0.3654 0.3208 0.3138 0.108 Uiso 1 1 calc R . . H35B H 0.3873 0.4105 0.2678 0.108 Uiso 1 1 calc R . . H35C H 0.4488 0.3891 0.3389 0.108 Uiso 1 1 calc R . . C36 C 0.5211(6) 0.2373(6) 0.3079(4) 0.107(2) Uani 1 1 d U . . H36A H 0.5575 0.2706 0.3453 0.160 Uiso 1 1 calc R . . H36B H 0.5618 0.1969 0.2827 0.160 Uiso 1 1 calc R . . H36C H 0.4742 0.1988 0.3282 0.160 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 0.0202(2) 0.0199(2) 0.0236(2) -0.00212(17) 0.00142(15) -0.00042(17) Fe1 0.0215(3) 0.0219(3) 0.0269(3) -0.0022(2) 0.0024(2) -0.0026(2) K1 0.0358(5) 0.0435(6) 0.0607(7) -0.0223(5) 0.0114(5) -0.0053(4) O1 0.0378(17) 0.054(2) 0.054(2) -0.0141(17) -0.0040(15) -0.0140(16) O2 0.0552(19) 0.0342(18) 0.0442(18) 0.0129(15) 0.0066(15) 0.0085(16) O3 0.063(2) 0.082(3) 0.0295(18) 0.0091(17) 0.0038(16) -0.026(2) O4 0.0373(17) 0.047(2) 0.069(2) -0.0232(17) 0.0169(16) 0.0005(15) N1 0.0216(15) 0.0227(17) 0.0293(17) -0.0024(13) 0.0035(13) 0.0008(13) N2 0.0216(15) 0.0207(16) 0.0236(16) -0.0022(13) -0.0007(12) 0.0003(13) N3 0.046(2) 0.065(3) 0.048(2) 0.002(2) -0.0067(19) 0.007(2) N4 0.047(2) 0.041(2) 0.054(2) -0.0012(19) 0.0106(19) 0.0048(19) C1 0.0252(19) 0.0206(19) 0.026(2) -0.0039(16) 0.0031(15) -0.0056(16) C2 0.0230(18) 0.028(2) 0.025(2) -0.0011(16) -0.0002(15) -0.0019(17) C3 0.0249(18) 0.0165(19) 0.034(2) -0.0019(16) 0.0087(16) -0.0031(16) C4 0.0248(19) 0.020(2) 0.037(2) 0.0007(17) 0.0047(16) -0.0028(16) C5 0.027(2) 0.024(2) 0.054(3) 0.0051(19) 0.0057(19) 0.0021(17) C6 0.031(2) 0.026(2) 0.061(3) -0.004(2) 0.018(2) 0.0030(18) C7 0.037(2) 0.029(2) 0.044(3) -0.007(2) 0.018(2) -0.0022(19) C8 0.0283(19) 0.023(2) 0.036(2) -0.0034(17) 0.0107(17) -0.0053(17) C9 0.036(2) 0.029(2) 0.033(2) 0.0015(18) 0.0006(18) 0.0046(18) C10 0.055(3) 0.138(6) 0.054(4) -0.022(4) -0.009(3) 0.002(4) C11 0.084(4) 0.043(3) 0.054(3) 0.005(2) 0.034(3) -0.005(3) C12 0.044(2) 0.030(2) 0.031(2) -0.0022(18) 0.0135(19) 0.0021(19) C13 0.051(3) 0.056(3) 0.046(3) -0.003(2) 0.001(2) -0.004(3) C14 0.069(3) 0.050(3) 0.043(3) 0.012(2) 0.013(2) -0.009(3) C15 0.0187(17) 0.022(2) 0.028(2) 0.0002(16) 0.0001(15) -0.0026(15) C16 0.0234(18) 0.021(2) 0.033(2) 0.0002(17) -0.0010(16) -0.0012(16) C17 0.030(2) 0.026(2) 0.046(3) -0.0037(19) 0.0043(18) 0.0043(18) C18 0.029(2) 0.031(2) 0.051(3) 0.010(2) -0.0032(19) 0.0065(18) C19 0.033(2) 0.037(2) 0.038(2) 0.011(2) -0.0054(18) 0.0007(19) C20 0.0263(19) 0.031(2) 0.029(2) 0.0036(17) -0.0023(16) -0.0053(17) C21 0.030(2) 0.027(2) 0.028(2) -0.0025(17) 0.0025(16) 0.0081(17) C22 0.041(2) 0.044(3) 0.038(2) -0.008(2) -0.002(2) 0.002(2) C23 0.047(3) 0.055(3) 0.036(2) 0.002(2) 0.008(2) -0.003(2) C24 0.038(2) 0.045(3) 0.026(2) 0.0032(19) -0.0016(17) -0.002(2) C25 0.061(3) 0.128(6) 0.043(3) -0.029(3) -0.006(3) -0.003(4) C26 0.071(4) 0.085(5) 0.073(4) -0.018(3) 0.041(3) -0.022(3) C27 0.031(2) 0.029(2) 0.035(2) -0.0011(18) 0.0073(18) 0.0004(19) C28 0.034(2) 0.032(2) 0.028(2) -0.0020(19) 0.0063(17) -0.0072(19) C29 0.030(2) 0.039(2) 0.034(2) 0.000(2) -0.0047(18) -0.0094(19) C30 0.0219(19) 0.031(2) 0.044(2) -0.0066(19) 0.0013(18) -0.0065(18) C31 0.165(5) 0.142(5) 0.140(5) 0.001(4) -0.024(4) 0.021(4) C32 0.105(4) 0.124(5) 0.120(4) -0.038(4) -0.009(4) 0.008(4) C33 0.125(5) 0.164(5) 0.124(5) -0.019(4) 0.000(4) -0.033(4) C34 0.088(4) 0.074(3) 0.087(4) -0.001(3) 0.009(3) -0.032(3) C35 0.061(3) 0.069(3) 0.088(3) 0.001(3) 0.020(3) 0.006(3) C36 0.124(4) 0.098(4) 0.100(4) 0.013(3) 0.013(4) 0.040(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 N2 1.872(3) . ? Ga1 N1 1.882(3) . ? Ga1 Fe1 2.3068(8) . ? Fe1 C30 1.753(4) . ? Fe1 C28 1.758(4) . ? Fe1 C27 1.777(4) . ? Fe1 C29 1.783(4) . ? K1 O4 2.626(3) . ? K1 O2 2.739(3) 2_655 ? K1 N4 2.798(4) . ? K1 N3 2.851(4) . ? K1 C6 3.185(4) . ? K1 C7 3.346(4) . ? O1 C27 1.152(5) . ? O2 C28 1.165(5) . ? O2 K1 2.739(3) 2_645 ? O3 C29 1.150(5) . ? O4 C30 1.166(5) . ? N1 C1 1.405(4) . ? N1 C3 1.420(5) . ? N2 C2 1.399(5) . ? N2 C15 1.426(5) . ? N3 C32 1.416(8) . ? N3 C31 1.419(10) . ? N3 C33 1.422(10) . ? N4 C35 1.449(6) . ? N4 C36 1.453(8) . ? N4 C34 1.462(7) . ? C1 C2 1.342(5) . ? C3 C4 1.400(5) . ? C3 C8 1.411(5) . ? C4 C5 1.399(5) . ? C4 C9 1.524(5) . ? C5 C6 1.388(6) . ? C6 C7 1.372(6) . ? C7 C8 1.394(5) . ? C8 C12 1.514(6) . ? C9 C10 1.518(6) . ? C9 C11 1.521(6) . ? C12 C13 1.534(6) . ? C12 C14 1.538(6) . ? C15 C16 1.412(5) . ? C15 C20 1.413(5) . ? C16 C17 1.397(5) . ? C16 C21 1.510(5) . ? C17 C18 1.382(6) . ? C18 C19 1.376(6) . ? C19 C20 1.392(6) . ? C20 C24 1.519(6) . ? C21 C22 1.523(6) . ? C21 C23 1.531(6) . ? C24 C26 1.519(7) . ? C24 C25 1.522(6) . ? C33 C34 1.466(11) . ? 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 N2 Ga1 N1 88.17(13) . . ? N2 Ga1 Fe1 139.33(9) . . ? N1 Ga1 Fe1 132.07(9) . . ? C30 Fe1 C28 114.99(19) . . ? C30 Fe1 C27 97.74(17) . . ? C28 Fe1 C27 97.76(19) . . ? C30 Fe1 C29 121.2(2) . . ? C28 Fe1 C29 120.12(19) . . ? C27 Fe1 C29 93.81(18) . . ? C30 Fe1 Ga1 82.66(12) . . ? C28 Fe1 Ga1 87.33(13) . . ? C27 Fe1 Ga1 174.13(13) . . ? C29 Fe1 Ga1 81.04(13) . . ? O4 K1 O2 137.33(11) . 2_655 ? O4 K1 N4 96.63(11) . . ? O2 K1 N4 84.33(11) 2_655 . ? O4 K1 N3 79.34(11) . . ? O2 K1 N3 136.41(11) 2_655 . ? N4 K1 N3 65.24(12) . . ? O4 K1 C6 94.32(10) . . ? O2 K1 C6 79.28(10) 2_655 . ? N4 K1 C6 163.53(12) . . ? N3 K1 C6 129.22(13) . . ? O4 K1 C7 83.54(10) . . ? O2 K1 C7 73.65(10) 2_655 . ? N4 K1 C7 146.31(12) . . ? N3 K1 C7 146.19(12) . . ? C6 K1 C7 24.10(11) . . ? C28 O2 K1 138.1(3) . 2_645 ? C30 O4 K1 160.4(3) . . ? C1 N1 C3 118.5(3) . . ? C1 N1 Ga1 108.8(2) . . ? C3 N1 Ga1 129.9(2) . . ? C2 N2 C15 117.6(3) . . ? C2 N2 Ga1 109.1(2) . . ? C15 N2 Ga1 131.4(2) . . ? C32 N3 C31 105.9(6) . . ? C32 N3 C33 115.2(7) . . ? C31 N3 C33 104.5(7) . . ? C32 N3 K1 115.6(4) . . ? C31 N3 K1 110.5(5) . . ? C33 N3 K1 104.6(4) . . ? C35 N4 C36 107.8(5) . . ? C35 N4 C34 111.6(5) . . ? C36 N4 C34 110.4(5) . . ? C35 N4 K1 106.4(3) . . ? C36 N4 K1 108.9(4) . . ? C34 N4 K1 111.5(3) . . ? C2 C1 N1 116.7(3) . . ? C1 C2 N2 117.2(3) . . ? C4 C3 C8 120.8(3) . . ? C4 C3 N1 119.4(3) . . ? C8 C3 N1 119.8(3) . . ? C5 C4 C3 118.5(4) . . ? C5 C4 C9 119.9(4) . . ? C3 C4 C9 121.4(3) . . ? C6 C5 C4 121.1(4) . . ? C7 C6 C5 119.6(4) . . ? C7 C6 K1 84.5(2) . . ? C5 C6 K1 94.2(3) . . ? C6 C7 C8 121.6(4) . . ? C6 C7 K1 71.4(2) . . ? C8 C7 K1 102.1(2) . . ? C7 C8 C3 118.3(4) . . ? C7 C8 C12 119.9(4) . . ? C3 C8 C12 121.8(3) . . ? C10 C9 C11 111.2(4) . . ? C10 C9 C4 113.2(4) . . ? C11 C9 C4 109.6(3) . . ? C8 C12 C13 112.5(4) . . ? C8 C12 C14 111.0(4) . . ? C13 C12 C14 110.3(4) . . ? C16 C15 C20 120.5(3) . . ? C16 C15 N2 119.9(3) . . ? C20 C15 N2 119.6(3) . . ? C17 C16 C15 118.3(4) . . ? C17 C16 C21 119.6(3) . . ? C15 C16 C21 122.1(3) . . ? C18 C17 C16 121.1(4) . . ? C19 C18 C17 120.2(4) . . ? C18 C19 C20 121.2(4) . . ? C19 C20 C15 118.6(4) . . ? C19 C20 C24 120.6(4) . . ? C15 C20 C24 120.7(3) . . ? C16 C21 C22 110.3(3) . . ? C16 C21 C23 113.1(3) . . ? C22 C21 C23 110.4(3) . . ? C20 C24 C26 109.6(4) . . ? C20 C24 C25 114.8(4) . . ? C26 C24 C25 110.0(4) . . ? O1 C27 Fe1 179.8(4) . . ? O2 C28 Fe1 175.3(4) . . ? O3 C29 Fe1 179.0(4) . . ? O4 C30 Fe1 177.9(4) . . ? N3 C33 C34 117.8(8) . . ? N4 C34 C33 114.0(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.288 #(near K1) _refine_diff_density_min -0.617 #(near Fe1) _refine_diff_density_rms 0.084