# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name C.Bielawski V.Lynch C.D.V.Junior _publ_contact_author_name 'Christopher Bielawski' _publ_contact_author_email BIELAWSKI@CM.UTEXAS.EDU data_bisfc _database_code_depnum_ccdc_archive 'CCDC 729832' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common N,N'-diethyl-benzazolium-Fc _chemical_melting_point ? _chemical_formula_moiety '2 C14 H14 N2, Fe 2+, 2 B F4 1-' _chemical_formula_sum 'C28 H28 B2 F8 Fe N4' _chemical_formula_weight 650.01 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.853(2) _cell_length_b 9.4328(12) _cell_length_c 20.816(2) _cell_angle_alpha 90.000(5) _cell_angle_beta 98.506(2) _cell_angle_gamma 90.000(5) _cell_volume 5603.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6757 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description laths _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.737 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _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 \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9421 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4933 _reflns_number_gt 4122 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. One of the tetrafluoroborate anions was disordered. The disorder was modeled by assigning the variable x to the site occupancy factor of one arrangement of fluorine atoms, F5, F6, F7 and F8, and (1-x) to the site occupancy factor of the alternate arrangement, F5a, F6a, F7a and F8a. The geometry of the two components were restrained to be equal throughout the refinement. The site occupancy factor for the major component, F5, F6, F7 and F8 refined to 64(2)%. The fluorine atoms of the disordered anion were refined anisotropically with their displacement parameters restrained to be approximately isotropic. ; _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^)+(0.0596P)^2^+8.1926P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4933 _refine_ls_number_parameters 428 _refine_ls_number_restraints 309 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1530 _refine_ls_goodness_of_fit_ref 1.452 _refine_ls_restrained_S_all 1.575 _refine_ls_shift/su_max 0.003 _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 Fe1 Fe 0.809191(17) 0.45470(6) -0.04442(3) 0.0271(2) Uani 1 1 d . . . N1 N 0.73292(11) 0.5779(4) -0.15121(16) 0.0366(8) Uani 1 1 d . . . N2 N 0.66652(14) 0.6889(5) -0.18003(19) 0.0543(11) Uani 1 1 d . . . N3 N 0.91112(11) 0.4091(4) 0.02573(18) 0.0357(8) Uani 1 1 d . . . N4 N 0.97124(13) 0.2828(4) 0.0701(2) 0.0540(11) Uani 1 1 d . . . C1 C 0.68578(15) 0.5649(6) -0.1616(2) 0.0471(12) Uani 1 1 d . . . H1 H 0.6690 0.4800 -0.1565 0.057 Uiso 1 1 calc R . . C2 C 0.74469(15) 0.7182(5) -0.16398(18) 0.0391(11) Uani 1 1 d . . . C3 C 0.78724(17) 0.7855(5) -0.1597(2) 0.0447(11) Uani 1 1 d . . . H3 H 0.8160 0.7371 -0.1472 0.054 Uiso 1 1 calc R . . C4 C 0.7855(2) 0.9291(5) -0.1749(2) 0.0543(13) Uani 1 1 d . . . H4 H 0.8139 0.9810 -0.1727 0.065 Uiso 1 1 calc R . . C5 C 0.7426(3) 0.9991(6) -0.1934(2) 0.0628(16) Uani 1 1 d . . . H5 H 0.7430 1.0971 -0.2038 0.075 Uiso 1 1 calc R . . C6 C 0.7004(2) 0.9314(6) -0.1971(2) 0.0586(15) Uani 1 1 d . . . H6 H 0.6716 0.9801 -0.2089 0.070 Uiso 1 1 calc R . . C7 C 0.70199(18) 0.7879(5) -0.1825(2) 0.0476(12) Uani 1 1 d . . . C8 C 0.61518(19) 0.7140(9) -0.1938(3) 0.086(2) Uani 1 1 d . . . H8A H 0.5992 0.6449 -0.1688 0.103 Uiso 1 1 calc R . . H8B H 0.6084 0.8101 -0.1785 0.103 Uiso 1 1 calc R . . C9 C 0.5965(2) 0.7018(11) -0.2608(4) 0.113(3) Uani 1 1 d . . . H9A H 0.6106 0.7743 -0.2856 0.170 Uiso 1 1 calc R . . H9B H 0.5625 0.7154 -0.2664 0.170 Uiso 1 1 calc R . . H9C H 0.6036 0.6076 -0.2766 0.170 Uiso 1 1 calc R . . C10 C 0.76292(13) 0.4637(5) -0.12751(18) 0.0326(9) Uani 1 1 d . . . C11 C 0.74952(13) 0.3552(4) -0.08663(19) 0.0344(9) Uani 1 1 d . . . H11 H 0.7209 0.3497 -0.0692 0.041 Uiso 1 1 calc R . . C12 C 0.78692(13) 0.2573(4) -0.0769(2) 0.0349(9) Uani 1 1 d . . . H12 H 0.7876 0.1726 -0.0521 0.042 Uiso 1 1 calc R . . C13 C 0.82313(14) 0.3061(5) -0.1101(2) 0.0358(10) Uani 1 1 d . . . H13 H 0.8524 0.2605 -0.1108 0.043 Uiso 1 1 calc R . . C14 C 0.80849(13) 0.4340(4) -0.14223(18) 0.0320(9) Uani 1 1 d . . . H14 H 0.8258 0.4894 -0.1686 0.038 Uiso 1 1 calc R . . C15 C 0.93101(14) 0.3405(5) 0.0789(2) 0.0439(11) Uani 1 1 d . . . H15 H 0.9178 0.3341 0.1180 0.053 Uiso 1 1 calc R . . C16 C 0.94039(13) 0.3954(5) -0.0219(2) 0.0413(11) Uani 1 1 d . . . C17 C 0.93687(15) 0.4475(5) -0.0840(3) 0.0486(12) Uani 1 1 d . . . H17 H 0.9107 0.5023 -0.1028 0.058 Uiso 1 1 calc R . . C18 C 0.97371(18) 0.4155(6) -0.1180(3) 0.0655(16) Uani 1 1 d . . . H18 H 0.9735 0.4498 -0.1610 0.079 Uiso 1 1 calc R . . C19 C 1.01211(17) 0.3298(6) -0.0874(4) 0.0680(19) Uani 1 1 d . . . H19 H 1.0365 0.3068 -0.1117 0.082 Uiso 1 1 calc R . . C20 C 1.01515(17) 0.2809(6) -0.0261(4) 0.0649(17) Uani 1 1 d . . . H20 H 1.0412 0.2262 -0.0069 0.078 Uiso 1 1 calc R . . C21 C 0.97841(13) 0.3141(5) 0.0077(3) 0.0512(14) Uani 1 1 d . . . C22 C 1.00319(18) 0.2035(6) 0.1205(3) 0.0736(18) Uani 1 1 d . . . H22A H 1.0356 0.2378 0.1206 0.088 Uiso 1 1 calc R . . H22B H 0.9943 0.2243 0.1637 0.088 Uiso 1 1 calc R . . C23 C 1.0021(2) 0.0504(7) 0.1104(4) 0.095(2) Uani 1 1 d . . . H23A H 0.9700 0.0156 0.1097 0.142 Uiso 1 1 calc R . . H23B H 1.0229 0.0043 0.1458 0.142 Uiso 1 1 calc R . . H23C H 1.0127 0.0284 0.0689 0.142 Uiso 1 1 calc R . . C24 C 0.86770(13) 0.4814(4) 0.02145(19) 0.0314(9) Uani 1 1 d . . . C25 C 0.82967(13) 0.4365(4) 0.05328(18) 0.0317(9) Uani 1 1 d . . . H25 H 0.8283 0.3529 0.0784 0.038 Uiso 1 1 calc R . . C26 C 0.79440(13) 0.5409(4) 0.04006(18) 0.0327(9) Uani 1 1 d . . . H26 H 0.7649 0.5394 0.0551 0.039 Uiso 1 1 calc R . . C27 C 0.81016(13) 0.6476(4) 0.00100(19) 0.0339(9) Uani 1 1 d . . . H27 H 0.7930 0.7296 -0.0147 0.041 Uiso 1 1 calc R . . C28 C 0.85602(13) 0.6117(4) -0.01096(19) 0.0321(9) Uani 1 1 d . . . H28 H 0.8751 0.6647 -0.0358 0.039 Uiso 1 1 calc R . . B1 B 0.87259(14) 0.0081(5) 0.0218(2) 0.0453(13) Uani 1 1 d DU . . F1 F 0.82806(10) -0.0290(3) -0.00518(19) 0.0850(12) Uani 1 1 d DU . . F2 F 0.86846(11) 0.1083(3) 0.06963(17) 0.0787(10) Uani 1 1 d DU . . F3 F 0.89524(10) -0.1071(3) 0.05129(17) 0.0746(10) Uani 1 1 d DU . . F4 F 0.89690(14) 0.0697(4) -0.02154(19) 0.1059(14) Uani 1 1 d DU . . B2 B 0.89325(15) 0.2803(5) 0.2469(2) 0.0573(16) Uani 1 1 d DU . . F5 F 0.8505(2) 0.2466(9) 0.2122(4) 0.078(2) Uani 0.64 1 d PDU A 1 F6 F 0.8886(3) 0.3107(8) 0.3097(2) 0.080(3) Uani 0.64 1 d PDU A 1 F7 F 0.9240(2) 0.1733(7) 0.2452(3) 0.110(2) Uani 0.64 1 d PDU A 1 F8 F 0.9104(2) 0.3998(7) 0.2194(3) 0.107(2) Uani 0.64 1 d PDU A 1 F5A F 0.8571(4) 0.2770(15) 0.1965(5) 0.081(4) Uani 0.36 1 d PDU A 2 F6A F 0.8999(4) 0.1447(8) 0.2723(6) 0.126(4) Uani 0.36 1 d PDU A 2 F7A F 0.9336(3) 0.3209(14) 0.2254(6) 0.112(3) Uani 0.36 1 d PDU A 2 F8A F 0.8834(5) 0.3693(12) 0.2943(5) 0.078(4) Uani 0.36 1 d PDU 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 Fe1 0.0214(3) 0.0313(3) 0.0287(3) -0.0013(2) 0.0044(2) -0.0007(2) N1 0.0324(18) 0.047(2) 0.0303(18) 0.0013(16) 0.0033(14) 0.0076(16) N2 0.041(2) 0.075(3) 0.045(2) -0.004(2) -0.0002(18) 0.019(2) N3 0.0229(16) 0.0290(18) 0.053(2) -0.0055(16) -0.0031(15) -0.0032(14) N4 0.030(2) 0.042(2) 0.085(3) -0.003(2) -0.010(2) -0.0025(17) C1 0.031(2) 0.065(3) 0.044(3) 0.002(2) -0.0001(19) 0.009(2) C2 0.047(3) 0.051(3) 0.019(2) 0.0022(19) 0.0051(17) 0.013(2) C3 0.057(3) 0.044(3) 0.033(2) 0.005(2) 0.011(2) 0.006(2) C4 0.083(4) 0.042(3) 0.039(3) 0.005(2) 0.014(2) -0.002(3) C5 0.120(5) 0.047(3) 0.023(2) 0.009(2) 0.016(3) 0.022(3) C6 0.083(4) 0.065(4) 0.028(2) 0.002(2) 0.006(2) 0.031(3) C7 0.062(3) 0.059(3) 0.022(2) 0.000(2) 0.004(2) 0.027(3) C8 0.044(3) 0.130(6) 0.081(4) 0.009(4) 0.003(3) 0.041(4) C9 0.045(3) 0.170(9) 0.117(6) -0.018(6) -0.016(4) 0.007(4) C10 0.0268(19) 0.043(2) 0.027(2) -0.0051(19) -0.0018(16) 0.0032(18) C11 0.0254(19) 0.042(2) 0.035(2) -0.0041(19) 0.0029(16) -0.0088(18) C12 0.036(2) 0.025(2) 0.042(2) -0.0057(18) 0.0007(18) -0.0084(18) C13 0.031(2) 0.040(2) 0.036(2) -0.0145(19) 0.0036(17) 0.0057(18) C14 0.030(2) 0.045(3) 0.0216(19) -0.0059(18) 0.0064(15) -0.0033(18) C15 0.026(2) 0.038(2) 0.063(3) -0.001(2) -0.007(2) -0.0053(19) C16 0.022(2) 0.038(2) 0.065(3) -0.015(2) 0.0081(19) -0.0094(18) C17 0.030(2) 0.049(3) 0.069(3) -0.023(3) 0.015(2) -0.009(2) C18 0.051(3) 0.065(3) 0.088(4) -0.032(3) 0.034(3) -0.024(3) C19 0.033(3) 0.055(3) 0.123(6) -0.048(4) 0.036(3) -0.014(2) C20 0.032(3) 0.049(3) 0.115(5) -0.029(3) 0.014(3) -0.005(2) C21 0.018(2) 0.031(2) 0.103(4) -0.026(3) 0.003(2) -0.0042(18) C22 0.039(3) 0.056(3) 0.115(5) 0.005(3) -0.026(3) 0.001(2) C23 0.072(4) 0.064(4) 0.131(6) 0.011(4) -0.039(4) -0.002(3) C24 0.0220(19) 0.035(2) 0.035(2) -0.0056(18) -0.0018(16) -0.0044(17) C25 0.033(2) 0.034(2) 0.027(2) -0.0001(17) -0.0005(16) -0.0034(18) C26 0.028(2) 0.044(2) 0.028(2) -0.0099(19) 0.0084(16) 0.0011(19) C27 0.032(2) 0.033(2) 0.037(2) -0.0078(18) 0.0031(17) 0.0033(18) C28 0.028(2) 0.029(2) 0.040(2) -0.0046(18) 0.0067(17) -0.0087(17) B1 0.027(2) 0.039(3) 0.070(4) -0.004(3) 0.007(2) 0.002(2) F1 0.0486(17) 0.0470(18) 0.144(3) 0.0076(19) -0.0351(19) -0.0050(14) F2 0.073(2) 0.0526(18) 0.117(3) -0.0245(19) 0.0351(19) -0.0047(16) F3 0.0496(17) 0.0512(18) 0.114(3) -0.0117(18) -0.0186(16) 0.0138(15) F4 0.110(3) 0.117(3) 0.100(3) -0.011(2) 0.045(2) -0.034(3) B2 0.049(3) 0.066(4) 0.057(4) 0.007(3) 0.009(3) 0.017(3) F5 0.087(4) 0.072(4) 0.068(4) 0.003(3) -0.012(3) -0.002(3) F6 0.054(3) 0.124(6) 0.063(4) -0.023(4) 0.013(3) 0.008(4) F7 0.098(4) 0.120(5) 0.115(5) -0.003(4) 0.022(3) 0.069(4) F8 0.100(5) 0.113(5) 0.113(4) 0.027(4) 0.027(4) -0.001(4) F5A 0.100(7) 0.078(7) 0.057(7) 0.014(6) -0.016(6) 0.035(6) F6A 0.109(8) 0.106(7) 0.153(9) 0.034(7) -0.011(7) 0.055(7) F7A 0.084(6) 0.148(7) 0.116(6) 0.003(6) 0.052(5) 0.021(6) F8A 0.061(6) 0.102(9) 0.074(6) -0.035(7) 0.015(5) 0.021(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 Fe1 C10 2.024(4) . ? Fe1 C24 2.027(4) . ? Fe1 C26 2.039(4) . ? Fe1 C25 2.039(4) . ? Fe1 C13 2.040(4) . ? Fe1 C11 2.042(4) . ? Fe1 C14 2.042(4) . ? Fe1 C27 2.049(4) . ? Fe1 C12 2.052(4) . ? Fe1 C28 2.056(4) . ? N1 C1 1.351(5) . ? N1 C2 1.401(6) . ? N1 C10 1.424(5) . ? N2 C1 1.327(6) . ? N2 C7 1.392(7) . ? N2 C8 1.486(6) . ? N3 C15 1.336(6) . ? N3 C16 1.400(6) . ? N3 C24 1.418(5) . ? N4 C15 1.319(6) . ? N4 C21 1.377(7) . ? N4 C22 1.491(7) . ? C1 H1 0.9500 . ? C2 C3 1.373(6) . ? C2 C7 1.400(6) . ? C3 C4 1.390(7) . ? C3 H3 0.9500 . ? C4 C5 1.404(8) . ? C4 H4 0.9500 . ? C5 C6 1.367(8) . ? C5 H5 0.9500 . ? C6 C7 1.386(7) . ? C6 H6 0.9500 . ? C8 C9 1.424(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.420(6) . ? C10 C14 1.422(5) . ? C11 C12 1.412(6) . ? C11 H11 0.9500 . ? C12 C13 1.413(6) . ? C12 H12 0.9500 . ? C13 C14 1.413(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.373(7) . ? C16 C21 1.404(7) . ? C17 C18 1.395(7) . ? C17 H17 0.9500 . ? C18 C19 1.441(9) . ? C18 H18 0.9500 . ? C19 C20 1.348(9) . ? C19 H19 0.9500 . ? C20 C21 1.393(7) . ? C20 H20 0.9500 . ? C22 C23 1.459(8) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C28 1.419(6) . ? C24 C25 1.427(5) . ? C25 C26 1.414(6) . ? C25 H25 0.9500 . ? C26 C27 1.411(6) . ? C26 H26 0.9500 . ? C27 C28 1.423(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? B1 F4 1.353(5) . ? B1 F3 1.366(5) . ? B1 F1 1.369(5) . ? B1 F2 1.391(5) . ? B2 F7 1.349(5) . ? B2 F8A 1.357(6) . ? B2 F7A 1.362(6) . ? B2 F6 1.364(6) . ? B2 F5A 1.364(6) . ? B2 F5 1.372(6) . ? B2 F6A 1.387(6) . ? B2 F8 1.387(6) . ? 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 C10 Fe1 C24 161.95(16) . . ? C10 Fe1 C26 121.63(16) . . ? C24 Fe1 C26 68.07(16) . . ? C10 Fe1 C25 155.88(16) . . ? C24 Fe1 C25 41.10(16) . . ? C26 Fe1 C25 40.56(16) . . ? C10 Fe1 C13 68.07(16) . . ? C24 Fe1 C13 108.17(16) . . ? C26 Fe1 C13 159.97(18) . . ? C25 Fe1 C13 123.64(17) . . ? C10 Fe1 C11 40.89(17) . . ? C24 Fe1 C11 155.94(17) . . ? C26 Fe1 C11 106.48(16) . . ? C25 Fe1 C11 119.47(16) . . ? C13 Fe1 C11 68.47(16) . . ? C10 Fe1 C14 40.92(15) . . ? C24 Fe1 C14 124.79(16) . . ? C26 Fe1 C14 157.73(17) . . ? C25 Fe1 C14 160.85(16) . . ? C13 Fe1 C14 40.52(17) . . ? C11 Fe1 C14 69.13(16) . . ? C10 Fe1 C27 108.62(17) . . ? C24 Fe1 C27 67.92(16) . . ? C26 Fe1 C27 40.38(16) . . ? C25 Fe1 C27 68.43(16) . . ? C13 Fe1 C27 158.32(17) . . ? C11 Fe1 C27 124.04(16) . . ? C14 Fe1 C27 122.85(17) . . ? C10 Fe1 C12 67.78(17) . . ? C24 Fe1 C12 121.65(16) . . ? C26 Fe1 C12 123.41(17) . . ? C25 Fe1 C12 106.41(16) . . ? C13 Fe1 C12 40.41(17) . . ? C11 Fe1 C12 40.36(16) . . ? C14 Fe1 C12 68.19(17) . . ? C27 Fe1 C12 160.11(16) . . ? C10 Fe1 C28 125.21(17) . . ? C24 Fe1 C28 40.66(16) . . ? C26 Fe1 C28 68.37(16) . . ? C25 Fe1 C28 69.14(16) . . ? C13 Fe1 C28 122.51(16) . . ? C11 Fe1 C28 161.26(17) . . ? C14 Fe1 C28 108.40(16) . . ? C27 Fe1 C28 40.56(15) . . ? C12 Fe1 C28 157.48(16) . . ? C1 N1 C2 108.8(4) . . ? C1 N1 C10 122.2(4) . . ? C2 N1 C10 128.9(3) . . ? C1 N2 C7 108.9(4) . . ? C1 N2 C8 124.0(5) . . ? C7 N2 C8 127.1(5) . . ? C15 N3 C16 108.2(4) . . ? C15 N3 C24 123.5(4) . . ? C16 N3 C24 128.3(4) . . ? C15 N4 C21 107.4(4) . . ? C15 N4 C22 125.1(5) . . ? C21 N4 C22 127.4(5) . . ? N2 C1 N1 109.6(4) . . ? N2 C1 H1 125.2 . . ? N1 C1 H1 125.2 . . ? C3 C2 C7 122.9(5) . . ? C3 C2 N1 131.6(4) . . ? C7 C2 N1 105.5(4) . . ? C2 C3 C4 115.7(5) . . ? C2 C3 H3 122.2 . . ? C4 C3 H3 122.2 . . ? C3 C4 C5 121.5(5) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 122.4(5) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C7 116.4(5) . . ? C5 C6 H6 121.8 . . ? C7 C6 H6 121.8 . . ? C6 C7 N2 131.6(5) . . ? C6 C7 C2 121.2(5) . . ? N2 C7 C2 107.2(4) . . ? C9 C8 N2 113.4(5) . . ? C9 C8 H8A 108.9 . . ? N2 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? N2 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C14 109.2(4) . . ? C11 C10 N1 123.2(3) . . ? C14 C10 N1 127.5(4) . . ? C11 C10 Fe1 70.2(2) . . ? C14 C10 Fe1 70.2(2) . . ? N1 C10 Fe1 128.2(3) . . ? C12 C11 C10 106.7(3) . . ? C12 C11 Fe1 70.2(2) . . ? C10 C11 Fe1 68.9(2) . . ? C12 C11 H11 126.6 . . ? C10 C11 H11 126.6 . . ? Fe1 C11 H11 125.8 . . ? C11 C12 C13 108.7(4) . . ? C11 C12 Fe1 69.4(2) . . ? C13 C12 Fe1 69.3(2) . . ? C11 C12 H12 125.6 . . ? C13 C12 H12 125.6 . . ? Fe1 C12 H12 127.2 . . ? C12 C13 C14 108.6(4) . . ? C12 C13 Fe1 70.3(2) . . ? C14 C13 Fe1 69.9(2) . . ? C12 C13 H13 125.7 . . ? C14 C13 H13 125.7 . . ? Fe1 C13 H13 125.8 . . ? C13 C14 C10 106.7(4) . . ? C13 C14 Fe1 69.6(2) . . ? C10 C14 Fe1 68.9(2) . . ? C13 C14 H14 126.6 . . ? C10 C14 H14 126.6 . . ? Fe1 C14 H14 126.4 . . ? N4 C15 N3 111.4(5) . . ? N4 C15 H15 124.3 . . ? N3 C15 H15 124.3 . . ? C17 C16 N3 131.7(4) . . ? C17 C16 C21 123.6(4) . . ? N3 C16 C21 104.7(4) . . ? C16 C17 C18 116.4(5) . . ? C16 C17 H17 121.8 . . ? C18 C17 H17 121.8 . . ? C17 C18 C19 119.4(6) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 123.3(5) . . ? C20 C19 H19 118.4 . . ? C18 C19 H19 118.4 . . ? C19 C20 C21 117.0(5) . . ? C19 C20 H20 121.5 . . ? C21 C20 H20 121.5 . . ? N4 C21 C20 131.4(5) . . ? N4 C21 C16 108.4(4) . . ? C20 C21 C16 120.3(6) . . ? C23 C22 N4 113.4(5) . . ? C23 C22 H22A 108.9 . . ? N4 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? N4 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N3 C24 C28 126.3(4) . . ? N3 C24 C25 124.1(4) . . ? C28 C24 C25 109.5(3) . . ? N3 C24 Fe1 128.5(3) . . ? C28 C24 Fe1 70.8(2) . . ? C25 C24 Fe1 69.9(2) . . ? C26 C25 C24 106.5(3) . . ? C26 C25 Fe1 69.7(2) . . ? C24 C25 Fe1 69.0(2) . . ? C26 C25 H25 126.8 . . ? C24 C25 H25 126.8 . . ? Fe1 C25 H25 126.1 . . ? C27 C26 C25 109.0(3) . . ? C27 C26 Fe1 70.2(2) . . ? C25 C26 Fe1 69.7(2) . . ? C27 C26 H26 125.5 . . ? C25 C26 H26 125.5 . . ? Fe1 C26 H26 126.2 . . ? C26 C27 C28 108.6(4) . . ? C26 C27 Fe1 69.4(2) . . ? C28 C27 Fe1 70.0(2) . . ? C26 C27 H27 125.7 . . ? C28 C27 H27 125.7 . . ? Fe1 C27 H27 126.4 . . ? C24 C28 C27 106.5(3) . . ? C24 C28 Fe1 68.6(2) . . ? C27 C28 Fe1 69.4(2) . . ? C24 C28 H28 126.7 . . ? C27 C28 H28 126.7 . . ? Fe1 C28 H28 126.8 . . ? F4 B1 F3 112.4(4) . . ? F4 B1 F1 112.6(4) . . ? F3 B1 F1 109.8(3) . . ? F4 B1 F2 107.1(4) . . ? F3 B1 F2 107.8(4) . . ? F1 B1 F2 107.0(3) . . ? F8A B2 F7A 110.2(6) . . ? F7 B2 F6 110.0(5) . . ? F8A B2 F5A 110.8(6) . . ? F7A B2 F5A 110.3(6) . . ? F7 B2 F5 110.9(5) . . ? F6 B2 F5 110.1(5) . . ? F8A B2 F6A 109.0(6) . . ? F7A B2 F6A 108.0(5) . . ? F5A B2 F6A 108.6(6) . . ? F7 B2 F8 108.7(4) . . ? F6 B2 F8 108.4(5) . . ? F5 B2 F8 108.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N2 C1 N1 0.5(5) . . . . ? C8 N2 C1 N1 -178.2(4) . . . . ? C2 N1 C1 N2 -0.3(5) . . . . ? C10 N1 C1 N2 176.5(4) . . . . ? C1 N1 C2 C3 178.7(4) . . . . ? C10 N1 C2 C3 2.2(7) . . . . ? C1 N1 C2 C7 0.1(4) . . . . ? C10 N1 C2 C7 -176.4(4) . . . . ? C7 C2 C3 C4 0.1(6) . . . . ? N1 C2 C3 C4 -178.4(4) . . . . ? C2 C3 C4 C5 -0.1(7) . . . . ? C3 C4 C5 C6 0.6(7) . . . . ? C4 C5 C6 C7 -1.1(7) . . . . ? C5 C6 C7 N2 178.5(4) . . . . ? C5 C6 C7 C2 1.1(6) . . . . ? C1 N2 C7 C6 -178.1(5) . . . . ? C8 N2 C7 C6 0.5(8) . . . . ? C1 N2 C7 C2 -0.4(5) . . . . ? C8 N2 C7 C2 178.2(5) . . . . ? C3 C2 C7 C6 -0.7(6) . . . . ? N1 C2 C7 C6 178.2(4) . . . . ? C3 C2 C7 N2 -178.6(4) . . . . ? N1 C2 C7 N2 0.2(4) . . . . ? C1 N2 C8 C9 -95.4(8) . . . . ? C7 N2 C8 C9 86.2(8) . . . . ? C1 N1 C10 C11 -29.3(6) . . . . ? C2 N1 C10 C11 146.8(4) . . . . ? C1 N1 C10 C14 147.2(4) . . . . ? C2 N1 C10 C14 -36.6(6) . . . . ? C1 N1 C10 Fe1 -119.3(4) . . . . ? C2 N1 C10 Fe1 56.8(5) . . . . ? C24 Fe1 C10 C11 163.4(5) . . . . ? C26 Fe1 C10 C11 -78.3(3) . . . . ? C25 Fe1 C10 C11 -42.2(5) . . . . ? C13 Fe1 C10 C11 82.0(3) . . . . ? C14 Fe1 C10 C11 120.1(3) . . . . ? C27 Fe1 C10 C11 -120.9(2) . . . . ? C12 Fe1 C10 C11 38.2(2) . . . . ? C28 Fe1 C10 C11 -162.9(2) . . . . ? C24 Fe1 C10 C14 43.3(6) . . . . ? C26 Fe1 C10 C14 161.6(2) . . . . ? C25 Fe1 C10 C14 -162.3(4) . . . . ? C13 Fe1 C10 C14 -38.1(2) . . . . ? C11 Fe1 C10 C14 -120.1(3) . . . . ? C27 Fe1 C10 C14 119.0(3) . . . . ? C12 Fe1 C10 C14 -81.9(3) . . . . ? C28 Fe1 C10 C14 77.0(3) . . . . ? C24 Fe1 C10 N1 -79.4(6) . . . . ? C26 Fe1 C10 N1 38.9(4) . . . . ? C25 Fe1 C10 N1 75.0(6) . . . . ? C13 Fe1 C10 N1 -160.8(4) . . . . ? C11 Fe1 C10 N1 117.2(4) . . . . ? C14 Fe1 C10 N1 -122.7(5) . . . . ? C27 Fe1 C10 N1 -3.7(4) . . . . ? C12 Fe1 C10 N1 155.4(4) . . . . ? C28 Fe1 C10 N1 -45.7(4) . . . . ? C14 C10 C11 C12 -0.7(4) . . . . ? N1 C10 C11 C12 176.3(3) . . . . ? Fe1 C10 C11 C12 -60.3(3) . . . . ? C14 C10 C11 Fe1 59.6(3) . . . . ? N1 C10 C11 Fe1 -123.3(4) . . . . ? C10 Fe1 C11 C12 117.8(3) . . . . ? C24 Fe1 C11 C12 -49.6(5) . . . . ? C26 Fe1 C11 C12 -122.6(3) . . . . ? C25 Fe1 C11 C12 -80.6(3) . . . . ? C13 Fe1 C11 C12 36.9(2) . . . . ? C14 Fe1 C11 C12 80.5(3) . . . . ? C27 Fe1 C11 C12 -163.2(2) . . . . ? C28 Fe1 C11 C12 166.3(4) . . . . ? C24 Fe1 C11 C10 -167.4(4) . . . . ? C26 Fe1 C11 C10 119.6(2) . . . . ? C25 Fe1 C11 C10 161.6(2) . . . . ? C13 Fe1 C11 C10 -80.9(3) . . . . ? C14 Fe1 C11 C10 -37.3(2) . . . . ? C27 Fe1 C11 C10 79.0(3) . . . . ? C12 Fe1 C11 C10 -117.8(3) . . . . ? C28 Fe1 C11 C10 48.5(6) . . . . ? C10 C11 C12 C13 1.2(4) . . . . ? Fe1 C11 C12 C13 -58.3(3) . . . . ? C10 C11 C12 Fe1 59.5(3) . . . . ? C10 Fe1 C12 C11 -38.7(2) . . . . ? C24 Fe1 C12 C11 158.6(2) . . . . ? C26 Fe1 C12 C11 75.4(3) . . . . ? C25 Fe1 C12 C11 116.4(2) . . . . ? C13 Fe1 C12 C11 -120.5(4) . . . . ? C14 Fe1 C12 C11 -83.0(3) . . . . ? C27 Fe1 C12 C11 44.7(6) . . . . ? C28 Fe1 C12 C11 -168.6(4) . . . . ? C10 Fe1 C12 C13 81.8(3) . . . . ? C24 Fe1 C12 C13 -80.9(3) . . . . ? C26 Fe1 C12 C13 -164.0(2) . . . . ? C25 Fe1 C12 C13 -123.0(2) . . . . ? C11 Fe1 C12 C13 120.5(4) . . . . ? C14 Fe1 C12 C13 37.5(2) . . . . ? C27 Fe1 C12 C13 165.2(4) . . . . ? C28 Fe1 C12 C13 -48.0(5) . . . . ? C11 C12 C13 C14 -1.2(4) . . . . ? Fe1 C12 C13 C14 -59.5(3) . . . . ? C11 C12 C13 Fe1 58.4(3) . . . . ? C10 Fe1 C13 C12 -81.0(3) . . . . ? C24 Fe1 C13 C12 117.8(2) . . . . ? C26 Fe1 C13 C12 42.1(6) . . . . ? C25 Fe1 C13 C12 75.0(3) . . . . ? C11 Fe1 C13 C12 -36.8(2) . . . . ? C14 Fe1 C13 C12 -119.5(3) . . . . ? C27 Fe1 C13 C12 -166.4(4) . . . . ? C28 Fe1 C13 C12 160.3(2) . . . . ? C10 Fe1 C13 C14 38.5(2) . . . . ? C24 Fe1 C13 C14 -122.7(2) . . . . ? C26 Fe1 C13 C14 161.6(4) . . . . ? C25 Fe1 C13 C14 -165.5(2) . . . . ? C11 Fe1 C13 C14 82.7(2) . . . . ? C27 Fe1 C13 C14 -46.9(5) . . . . ? C12 Fe1 C13 C14 119.5(3) . . . . ? C28 Fe1 C13 C14 -80.2(3) . . . . ? C12 C13 C14 C10 0.7(4) . . . . ? Fe1 C13 C14 C10 -59.1(3) . . . . ? C12 C13 C14 Fe1 59.8(3) . . . . ? C11 C10 C14 C13 0.0(4) . . . . ? N1 C10 C14 C13 -176.9(4) . . . . ? Fe1 C10 C14 C13 59.6(3) . . . . ? C11 C10 C14 Fe1 -59.6(3) . . . . ? N1 C10 C14 Fe1 123.5(4) . . . . ? C10 Fe1 C14 C13 -118.2(3) . . . . ? C24 Fe1 C14 C13 76.8(3) . . . . ? C26 Fe1 C14 C13 -163.4(4) . . . . ? C25 Fe1 C14 C13 39.6(6) . . . . ? C11 Fe1 C14 C13 -80.9(3) . . . . ? C27 Fe1 C14 C13 161.3(2) . . . . ? C12 Fe1 C14 C13 -37.4(2) . . . . ? C28 Fe1 C14 C13 118.9(2) . . . . ? C24 Fe1 C14 C10 -165.0(2) . . . . ? C26 Fe1 C14 C10 -45.2(5) . . . . ? C25 Fe1 C14 C10 157.8(5) . . . . ? C13 Fe1 C14 C10 118.2(3) . . . . ? C11 Fe1 C14 C10 37.3(2) . . . . ? C27 Fe1 C14 C10 -80.5(3) . . . . ? C12 Fe1 C14 C10 80.8(3) . . . . ? C28 Fe1 C14 C10 -122.9(2) . . . . ? C21 N4 C15 N3 -0.3(5) . . . . ? C22 N4 C15 N3 177.6(4) . . . . ? C16 N3 C15 N4 0.2(5) . . . . ? C24 N3 C15 N4 -179.8(3) . . . . ? C15 N3 C16 C17 -178.5(5) . . . . ? C24 N3 C16 C17 1.5(7) . . . . ? C15 N3 C16 C21 0.0(4) . . . . ? C24 N3 C16 C21 -180.0(4) . . . . ? N3 C16 C17 C18 178.4(4) . . . . ? C21 C16 C17 C18 0.1(7) . . . . ? C16 C17 C18 C19 1.0(7) . . . . ? C17 C18 C19 C20 -1.7(8) . . . . ? C18 C19 C20 C21 1.2(8) . . . . ? C15 N4 C21 C20 179.2(5) . . . . ? C22 N4 C21 C20 1.4(8) . . . . ? C15 N4 C21 C16 0.3(5) . . . . ? C22 N4 C21 C16 -177.5(4) . . . . ? C19 C20 C21 N4 -178.9(5) . . . . ? C19 C20 C21 C16 -0.1(7) . . . . ? C17 C16 C21 N4 178.5(4) . . . . ? N3 C16 C21 N4 -0.2(4) . . . . ? C17 C16 C21 C20 -0.6(7) . . . . ? N3 C16 C21 C20 -179.3(4) . . . . ? C15 N4 C22 C23 105.4(7) . . . . ? C21 N4 C22 C23 -77.2(8) . . . . ? C15 N3 C24 C28 142.0(4) . . . . ? C16 N3 C24 C28 -38.0(6) . . . . ? C15 N3 C24 C25 -33.9(6) . . . . ? C16 N3 C24 C25 146.1(4) . . . . ? C15 N3 C24 Fe1 -124.4(4) . . . . ? C16 N3 C24 Fe1 55.6(5) . . . . ? C10 Fe1 C24 N3 -77.4(7) . . . . ? C26 Fe1 C24 N3 156.5(4) . . . . ? C25 Fe1 C24 N3 118.2(5) . . . . ? C13 Fe1 C24 N3 -2.5(4) . . . . ? C11 Fe1 C24 N3 75.2(6) . . . . ? C14 Fe1 C24 N3 -44.3(4) . . . . ? C27 Fe1 C24 N3 -159.8(4) . . . . ? C12 Fe1 C24 N3 39.8(4) . . . . ? C28 Fe1 C24 N3 -121.6(5) . . . . ? C10 Fe1 C24 C28 44.2(6) . . . . ? C26 Fe1 C24 C28 -81.9(3) . . . . ? C25 Fe1 C24 C28 -120.2(3) . . . . ? C13 Fe1 C24 C28 119.1(2) . . . . ? C11 Fe1 C24 C28 -163.2(4) . . . . ? C14 Fe1 C24 C28 77.3(3) . . . . ? C27 Fe1 C24 C28 -38.2(2) . . . . ? C12 Fe1 C24 C28 161.4(2) . . . . ? C10 Fe1 C24 C25 164.4(5) . . . . ? C26 Fe1 C24 C25 38.3(2) . . . . ? C13 Fe1 C24 C25 -120.7(2) . . . . ? C11 Fe1 C24 C25 -43.0(5) . . . . ? C14 Fe1 C24 C25 -162.4(2) . . . . ? C27 Fe1 C24 C25 82.0(2) . . . . ? C12 Fe1 C24 C25 -78.4(3) . . . . ? C28 Fe1 C24 C25 120.2(3) . . . . ? N3 C24 C25 C26 176.5(3) . . . . ? C28 C24 C25 C26 0.0(4) . . . . ? Fe1 C24 C25 C26 -59.9(3) . . . . ? N3 C24 C25 Fe1 -123.6(4) . . . . ? C28 C24 C25 Fe1 59.9(3) . . . . ? C10 Fe1 C25 C26 -50.5(5) . . . . ? C24 Fe1 C25 C26 117.8(3) . . . . ? C13 Fe1 C25 C26 -163.3(2) . . . . ? C11 Fe1 C25 C26 -80.8(3) . . . . ? C14 Fe1 C25 C26 166.8(5) . . . . ? C27 Fe1 C25 C26 37.1(2) . . . . ? C12 Fe1 C25 C26 -122.6(2) . . . . ? C28 Fe1 C25 C26 80.7(2) . . . . ? C10 Fe1 C25 C24 -168.3(4) . . . . ? C26 Fe1 C25 C24 -117.8(3) . . . . ? C13 Fe1 C25 C24 78.9(3) . . . . ? C11 Fe1 C25 C24 161.4(2) . . . . ? C14 Fe1 C25 C24 49.1(6) . . . . ? C27 Fe1 C25 C24 -80.7(2) . . . . ? C12 Fe1 C25 C24 119.6(2) . . . . ? C28 Fe1 C25 C24 -37.0(2) . . . . ? C24 C25 C26 C27 0.1(4) . . . . ? Fe1 C25 C26 C27 -59.4(3) . . . . ? C24 C25 C26 Fe1 59.5(3) . . . . ? C10 Fe1 C26 C27 -81.6(3) . . . . ? C24 Fe1 C26 C27 81.3(2) . . . . ? C25 Fe1 C26 C27 120.1(3) . . . . ? C13 Fe1 C26 C27 164.2(4) . . . . ? C11 Fe1 C26 C27 -123.6(2) . . . . ? C14 Fe1 C26 C27 -48.5(5) . . . . ? C12 Fe1 C26 C27 -164.4(2) . . . . ? C28 Fe1 C26 C27 37.3(2) . . . . ? C10 Fe1 C26 C25 158.3(2) . . . . ? C24 Fe1 C26 C25 -38.8(2) . . . . ? C13 Fe1 C26 C25 44.1(5) . . . . ? C11 Fe1 C26 C25 116.3(2) . . . . ? C14 Fe1 C26 C25 -168.6(4) . . . . ? C27 Fe1 C26 C25 -120.1(3) . . . . ? C12 Fe1 C26 C25 75.5(3) . . . . ? C28 Fe1 C26 C25 -82.8(2) . . . . ? C25 C26 C27 C28 -0.1(4) . . . . ? Fe1 C26 C27 C28 -59.2(3) . . . . ? C25 C26 C27 Fe1 59.1(3) . . . . ? C10 Fe1 C27 C26 117.3(2) . . . . ? C24 Fe1 C27 C26 -81.7(2) . . . . ? C25 Fe1 C27 C26 -37.2(2) . . . . ? C13 Fe1 C27 C26 -165.4(4) . . . . ? C11 Fe1 C27 C26 74.6(3) . . . . ? C14 Fe1 C27 C26 160.2(2) . . . . ? C12 Fe1 C27 C26 41.2(6) . . . . ? C28 Fe1 C27 C26 -119.9(3) . . . . ? C10 Fe1 C27 C28 -122.8(2) . . . . ? C24 Fe1 C27 C28 38.3(2) . . . . ? C26 Fe1 C27 C28 119.9(3) . . . . ? C25 Fe1 C27 C28 82.7(3) . . . . ? C13 Fe1 C27 C28 -45.5(5) . . . . ? C11 Fe1 C27 C28 -165.5(2) . . . . ? C14 Fe1 C27 C28 -79.8(3) . . . . ? C12 Fe1 C27 C28 161.2(4) . . . . ? N3 C24 C28 C27 -176.5(4) . . . . ? C25 C24 C28 C27 0.0(4) . . . . ? Fe1 C24 C28 C27 59.4(3) . . . . ? N3 C24 C28 Fe1 124.2(4) . . . . ? C25 C24 C28 Fe1 -59.4(3) . . . . ? C26 C27 C28 C24 0.1(4) . . . . ? Fe1 C27 C28 C24 -58.8(3) . . . . ? C26 C27 C28 Fe1 58.9(3) . . . . ? C10 Fe1 C28 C24 -164.7(2) . . . . ? C26 Fe1 C28 C24 81.1(2) . . . . ? C25 Fe1 C28 C24 37.4(2) . . . . ? C13 Fe1 C28 C24 -80.0(3) . . . . ? C11 Fe1 C28 C24 158.4(5) . . . . ? C14 Fe1 C28 C24 -122.4(2) . . . . ? C27 Fe1 C28 C24 118.2(3) . . . . ? C12 Fe1 C28 C24 -45.1(5) . . . . ? C10 Fe1 C28 C27 77.1(3) . . . . ? C24 Fe1 C28 C27 -118.2(3) . . . . ? C26 Fe1 C28 C27 -37.2(2) . . . . ? C25 Fe1 C28 C27 -80.8(3) . . . . ? C13 Fe1 C28 C27 161.8(2) . . . . ? C11 Fe1 C28 C27 40.2(6) . . . . ? C14 Fe1 C28 C27 119.4(2) . . . . ? C12 Fe1 C28 C27 -163.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.820 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.073 #===END data_diirco _database_code_depnum_ccdc_archive 'CCDC 729833' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2 C14 H13 N2, 4 C O, Fe, 2 Ir, 2 Cl, C H Cl3' _chemical_formula_sum 'C33 H27 Cl5 Fe Ir2 N4 O4' _chemical_formula_weight 1161.09 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' Ir Ir -1.4442 7.9887 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 15.8100(2) _cell_length_b 14.5490(2) _cell_length_c 17.1930(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.5520(10) _cell_angle_gamma 90.00 _cell_volume 3703.02(8) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 10829 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 30.0 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 7.959 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.172 _exptl_absorpt_correction_T_max 0.418 _exptl_absorpt_process_details ; (see. N.W. Alcock (1970). Cryst. Computing, p271) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _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 \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53217 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10804 _reflns_number_gt 8188 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. A molecule of chloroform was disordered near a crystallographic inversion at 1/2, 0, 1/2. The contributions to the scattering factors due to this solvent molecule were removed by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). ; _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^)+(0.0432P)^2^+2.2559P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10804 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0913 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Ir1 Ir 0.429143(10) 0.431457(10) 0.742074(9) 0.03275(5) Uani 1 1 d . . . Ir2 Ir 0.026491(12) 0.574717(10) 0.210734(9) 0.03820(6) Uani 1 1 d . . . Fe1 Fe 0.28728(3) 0.38996(4) 0.42626(3) 0.02894(12) Uani 1 1 d . . . Cl1 Cl 0.28954(8) 0.37883(9) 0.74388(8) 0.0621(3) Uani 1 1 d . . . Cl2 Cl 0.15257(9) 0.67194(8) 0.23846(7) 0.0520(3) Uani 1 1 d . . . N1 N 0.3352(2) 0.6149(2) 0.67606(18) 0.0306(6) Uani 1 1 d . . . N2 N 0.3499(2) 0.5369(2) 0.57417(18) 0.0300(6) Uani 1 1 d . . . N3 N 0.0212(2) 0.6298(2) 0.37917(18) 0.0309(6) Uani 1 1 d . . . N4 N 0.10843(19) 0.5103(2) 0.39537(17) 0.0276(6) Uani 1 1 d . . . C1 C 0.3648(2) 0.5337(3) 0.6570(2) 0.0316(8) Uani 1 1 d . . . C2 C 0.3014(2) 0.6709(3) 0.6064(2) 0.0313(8) Uani 1 1 d . . . C3 C 0.2642(3) 0.7585(3) 0.5956(3) 0.0384(9) Uani 1 1 d . . . H3 H 0.2580 0.7920 0.6407 0.046 Uiso 1 1 calc R . . C4 C 0.2368(3) 0.7942(3) 0.5170(3) 0.0397(9) Uani 1 1 d . . . H4 H 0.2113 0.8542 0.5075 0.048 Uiso 1 1 calc R . . C5 C 0.2453(3) 0.7449(3) 0.4504(3) 0.0406(9) Uani 1 1 d . . . H5 H 0.2252 0.7719 0.3967 0.049 Uiso 1 1 calc R . . C6 C 0.2823(3) 0.6575(3) 0.4608(2) 0.0336(8) Uani 1 1 d . . . H6 H 0.2879 0.6238 0.4155 0.040 Uiso 1 1 calc R . . C7 C 0.3108(2) 0.6216(2) 0.5408(2) 0.0313(8) Uani 1 1 d . . . C8 C 0.3347(3) 0.6396(3) 0.7597(2) 0.0391(9) Uani 1 1 d . . . H8A H 0.3406 0.5829 0.7930 0.047 Uiso 1 1 calc R . . H8B H 0.2761 0.6684 0.7538 0.047 Uiso 1 1 calc R . . C9 C 0.4105(4) 0.7051(4) 0.8053(3) 0.0632(14) Uani 1 1 d . . . H9A H 0.4684 0.6791 0.8073 0.095 Uiso 1 1 calc R . . H9B H 0.4113 0.7144 0.8620 0.095 Uiso 1 1 calc R . . H9C H 0.4008 0.7643 0.7762 0.095 Uiso 1 1 calc R . . C10 C 0.3688(3) 0.4629(3) 0.5281(2) 0.0335(8) Uani 1 1 d . . . C11 C 0.3998(3) 0.4725(3) 0.4605(2) 0.0372(9) Uani 1 1 d . . . H11 H 0.4057 0.5283 0.4340 0.045 Uiso 1 1 calc R . . C12 C 0.4204(3) 0.3828(3) 0.4399(3) 0.0423(10) Uani 1 1 d . . . H12 H 0.4434 0.3681 0.3973 0.051 Uiso 1 1 calc R . . C13 C 0.4011(3) 0.3193(3) 0.4933(2) 0.0411(9) Uani 1 1 d . . . H13 H 0.4093 0.2547 0.4930 0.049 Uiso 1 1 calc R . . C14 C 0.3673(3) 0.3685(3) 0.5480(2) 0.0365(9) Uani 1 1 d . . . H14 H 0.3476 0.3430 0.5896 0.044 Uiso 1 1 calc R . . C15 C 0.1554(3) 0.4348(2) 0.3755(2) 0.0291(8) Uani 1 1 d . . . C16 C 0.1983(3) 0.4375(3) 0.3151(2) 0.0334(8) Uani 1 1 d . . . H16 H 0.2068 0.4901 0.2859 0.040 Uiso 1 1 calc R . . C17 C 0.2258(3) 0.3467(3) 0.3071(2) 0.0380(9) Uani 1 1 d . . . H17 H 0.2558 0.3275 0.2707 0.046 Uiso 1 1 calc R . . C18 C 0.2016(3) 0.2896(3) 0.3615(3) 0.0398(9) Uani 1 1 d . . . H18 H 0.2124 0.2253 0.3679 0.048 Uiso 1 1 calc R . . C19 C 0.1585(3) 0.3433(2) 0.4050(2) 0.0339(8) Uani 1 1 d . . . H19 H 0.1360 0.3222 0.4463 0.041 Uiso 1 1 calc R . . C20 C 0.0549(3) 0.5693(2) 0.3380(2) 0.0307(8) Uani 1 1 d . . . C21 C 0.0539(2) 0.6100(2) 0.4638(2) 0.0292(7) Uani 1 1 d . . . C22 C 0.0392(3) 0.6530(3) 0.5303(2) 0.0339(8) Uani 1 1 d . . . H22 H 0.0031 0.7068 0.5228 0.041 Uiso 1 1 calc R . . C23 C 0.0795(3) 0.6138(3) 0.6076(2) 0.0357(8) Uani 1 1 d . . . H23 H 0.0718 0.6419 0.6545 0.043 Uiso 1 1 calc R . . C24 C 0.1314(2) 0.5340(3) 0.6186(2) 0.0329(8) Uani 1 1 d . . . H24 H 0.1567 0.5080 0.6725 0.039 Uiso 1 1 calc R . . C25 C 0.1467(2) 0.4918(3) 0.5523(2) 0.0306(8) Uani 1 1 d . . . H25 H 0.1822 0.4376 0.5595 0.037 Uiso 1 1 calc R . . C26 C 0.1077(2) 0.5327(2) 0.4750(2) 0.0272(7) Uani 1 1 d . . . C27 C -0.0448(3) 0.7036(3) 0.3406(3) 0.0405(9) Uani 1 1 d . . . H27A H -0.0887 0.7081 0.3697 0.049 Uiso 1 1 calc R . . H27B H -0.0785 0.6878 0.2818 0.049 Uiso 1 1 calc R . . C28 C 0.0012(3) 0.7950(3) 0.3447(3) 0.0473(11) Uani 1 1 d . . . H28A H 0.0344 0.8109 0.4029 0.071 Uiso 1 1 calc R . . H28B H -0.0443 0.8424 0.3195 0.071 Uiso 1 1 calc R . . H28C H 0.0433 0.7913 0.3145 0.071 Uiso 1 1 calc R . . O1A O 0.5161(2) 0.2903(3) 0.8748(2) 0.0680(10) Uani 1 1 d . . . C1A C 0.4838(3) 0.3426(3) 0.8241(3) 0.0462(10) Uani 1 1 d . . . O2A O 0.6036(3) 0.4876(4) 0.7315(3) 0.0881(14) Uani 1 1 d . . . C2A C 0.5407(3) 0.4690(4) 0.7362(3) 0.0484(11) Uani 1 1 d . . . O3A O -0.1358(2) 0.4567(3) 0.1787(2) 0.0594(9) Uani 1 1 d . . . C3A C -0.0738(3) 0.5014(3) 0.1905(3) 0.0464(11) Uani 1 1 d . . . O4A O -0.0053(4) 0.6008(3) 0.0286(2) 0.1079(19) Uani 1 1 d . . . C4A C 0.0058(5) 0.5889(3) 0.0971(3) 0.0650(16) Uani 1 1 d . . . 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 Ir1 0.03084(9) 0.03540(9) 0.02997(8) 0.00215(6) 0.00813(6) -0.00008(6) Ir2 0.04880(11) 0.03376(9) 0.02829(8) 0.00505(6) 0.00883(7) 0.00113(7) Fe1 0.0283(3) 0.0279(3) 0.0298(2) -0.0021(2) 0.0092(2) 0.0000(2) Cl1 0.0435(6) 0.0569(8) 0.0807(9) 0.0268(6) 0.0153(6) -0.0026(5) Cl2 0.0666(7) 0.0493(6) 0.0457(5) 0.0061(5) 0.0268(5) -0.0114(6) N1 0.0311(16) 0.0311(16) 0.0289(15) -0.0031(12) 0.0097(12) -0.0041(13) N2 0.0263(15) 0.0293(15) 0.0319(15) -0.0012(13) 0.0071(12) -0.0003(13) N3 0.0266(15) 0.0283(15) 0.0357(16) 0.0022(13) 0.0082(13) 0.0020(12) N4 0.0240(14) 0.0284(15) 0.0290(14) 0.0030(12) 0.0077(12) -0.0024(12) C1 0.0284(18) 0.0325(19) 0.0330(18) -0.0040(15) 0.0096(15) -0.0061(15) C2 0.0278(18) 0.0300(18) 0.0350(18) -0.0014(15) 0.0096(15) -0.0063(15) C3 0.037(2) 0.0306(19) 0.050(2) -0.0021(17) 0.0186(18) -0.0002(17) C4 0.038(2) 0.0284(19) 0.051(2) 0.0034(17) 0.0130(18) 0.0040(17) C5 0.041(2) 0.036(2) 0.041(2) 0.0067(17) 0.0097(18) -0.0041(18) C6 0.035(2) 0.037(2) 0.0314(18) 0.0043(15) 0.0146(16) -0.0031(16) C7 0.0254(17) 0.0280(18) 0.0384(19) -0.0005(15) 0.0086(15) -0.0060(15) C8 0.045(2) 0.040(2) 0.0345(19) -0.0047(17) 0.0167(18) -0.0022(19) C9 0.081(4) 0.064(3) 0.048(3) -0.025(2) 0.026(3) -0.025(3) C10 0.0267(18) 0.036(2) 0.0344(19) -0.0043(16) 0.0069(15) -0.0007(16) C11 0.0275(19) 0.043(2) 0.040(2) -0.0067(17) 0.0113(16) -0.0025(17) C12 0.032(2) 0.046(2) 0.050(2) -0.014(2) 0.0144(18) 0.0032(18) C13 0.038(2) 0.036(2) 0.041(2) -0.0016(17) 0.0028(17) 0.0116(18) C14 0.038(2) 0.034(2) 0.0313(18) 0.0013(15) 0.0047(16) 0.0046(17) C15 0.0264(18) 0.0299(18) 0.0277(17) -0.0020(13) 0.0054(14) -0.0018(14) C16 0.037(2) 0.034(2) 0.0279(18) 0.0031(14) 0.0105(16) 0.0003(16) C17 0.042(2) 0.040(2) 0.0310(18) -0.0090(16) 0.0107(17) 0.0035(18) C18 0.039(2) 0.0310(19) 0.045(2) -0.0091(17) 0.0093(18) -0.0030(17) C19 0.0315(19) 0.0293(19) 0.040(2) 0.0017(16) 0.0107(16) -0.0038(16) C20 0.0311(19) 0.0277(18) 0.0341(19) 0.0043(14) 0.0124(16) -0.0017(14) C21 0.0235(17) 0.0282(18) 0.0352(18) 0.0026(15) 0.0095(14) -0.0054(15) C22 0.0292(19) 0.0319(19) 0.043(2) -0.0003(16) 0.0162(16) -0.0028(16) C23 0.034(2) 0.038(2) 0.0359(19) -0.0111(16) 0.0138(16) -0.0096(17) C24 0.0286(19) 0.039(2) 0.0304(18) -0.0010(16) 0.0100(15) -0.0070(16) C25 0.0228(17) 0.0330(19) 0.0342(18) 0.0015(15) 0.0077(15) -0.0065(15) C26 0.0239(17) 0.0268(17) 0.0304(17) -0.0025(14) 0.0089(14) -0.0063(14) C27 0.033(2) 0.038(2) 0.044(2) 0.0058(17) 0.0058(17) 0.0072(17) C28 0.050(3) 0.034(2) 0.053(3) 0.0092(19) 0.012(2) 0.0085(19) O1A 0.050(2) 0.079(2) 0.076(2) 0.040(2) 0.0219(18) 0.0127(18) C1A 0.035(2) 0.056(3) 0.048(2) 0.010(2) 0.0162(19) 0.005(2) O2A 0.060(3) 0.125(4) 0.083(3) 0.042(3) 0.031(2) 0.004(3) C2A 0.042(3) 0.061(3) 0.038(2) 0.014(2) 0.009(2) 0.007(2) O3A 0.053(2) 0.064(2) 0.0511(19) -0.0079(17) 0.0069(16) -0.0044(18) C3A 0.055(3) 0.039(2) 0.034(2) 0.0023(17) 0.001(2) 0.002(2) O4A 0.193(6) 0.087(3) 0.036(2) 0.003(2) 0.030(3) -0.037(3) C4A 0.107(5) 0.047(3) 0.038(2) 0.000(2) 0.022(3) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C2A 1.883(5) . ? Ir1 C1A 1.885(4) . ? Ir1 C1 2.084(4) . ? Ir1 Cl1 2.3466(12) . ? Ir2 C3A 1.840(5) . ? Ir2 C4A 1.875(5) . ? Ir2 C20 2.075(4) . ? Ir2 Cl2 2.3524(12) . ? Fe1 C17 2.035(4) . ? Fe1 C12 2.037(4) . ? Fe1 C18 2.037(4) . ? Fe1 C13 2.042(4) . ? Fe1 C14 2.054(4) . ? Fe1 C19 2.053(4) . ? Fe1 C11 2.054(4) . ? Fe1 C16 2.055(4) . ? Fe1 C15 2.063(4) . ? Fe1 C10 2.066(4) . ? N1 C1 1.353(5) . ? N1 C2 1.391(5) . ? N1 C8 1.484(5) . ? N2 C1 1.359(5) . ? N2 C7 1.407(5) . ? N2 C10 1.428(5) . ? N3 C20 1.350(5) . ? N3 C21 1.392(5) . ? N3 C27 1.482(5) . ? N4 C20 1.357(5) . ? N4 C26 1.412(4) . ? N4 C15 1.433(5) . ? C2 C7 1.387(5) . ? C2 C3 1.389(5) . ? C3 C4 1.369(6) . ? C3 H3 0.9500 . ? C4 C5 1.397(6) . ? C4 H4 0.9500 . ? C5 C6 1.385(6) . ? C5 H5 0.9500 . ? C6 C7 1.390(5) . ? C6 H6 0.9500 . ? C8 C9 1.517(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C14 1.417(6) . ? C10 C11 1.419(5) . ? C11 C12 1.419(6) . ? C11 H11 0.9500 . ? C12 C13 1.410(6) . ? C12 H12 0.9500 . ? C13 C14 1.426(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C19 1.420(5) . ? C15 C16 1.427(5) . ? C16 C17 1.411(5) . ? C16 H16 0.9500 . ? C17 C18 1.401(6) . ? C17 H17 0.9500 . ? C18 C19 1.412(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C21 C26 1.383(5) . ? C21 C22 1.393(5) . ? C22 C23 1.378(5) . ? C22 H22 0.9500 . ? C23 C24 1.396(6) . ? C23 H23 0.9500 . ? C24 C25 1.389(5) . ? C24 H24 0.9500 . ? C25 C26 1.387(5) . ? C25 H25 0.9500 . ? C27 C28 1.505(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O1A C1A 1.135(5) . ? O2A C2A 1.060(6) . ? O3A C3A 1.134(6) . ? O4A C4A 1.141(6) . ? 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 C2A Ir1 C1A 92.69(19) . . ? C2A Ir1 C1 89.47(17) . . ? C1A Ir1 C1 176.09(17) . . ? C2A Ir1 Cl1 176.93(16) . . ? C1A Ir1 Cl1 87.29(13) . . ? C1 Ir1 Cl1 90.73(11) . . ? C3A Ir2 C4A 92.5(2) . . ? C3A Ir2 C20 91.72(17) . . ? C4A Ir2 C20 175.30(19) . . ? C3A Ir2 Cl2 178.18(15) . . ? C4A Ir2 Cl2 88.31(19) . . ? C20 Ir2 Cl2 87.42(10) . . ? C17 Fe1 C12 102.08(17) . . ? C17 Fe1 C18 40.26(17) . . ? C12 Fe1 C18 119.24(17) . . ? C17 Fe1 C13 115.34(16) . . ? C12 Fe1 C13 40.44(18) . . ? C18 Fe1 C13 103.49(17) . . ? C17 Fe1 C14 152.22(16) . . ? C12 Fe1 C14 68.46(18) . . ? C18 Fe1 C14 120.13(17) . . ? C13 Fe1 C14 40.76(16) . . ? C17 Fe1 C19 68.02(16) . . ? C12 Fe1 C19 157.42(16) . . ? C18 Fe1 C19 40.38(16) . . ? C13 Fe1 C19 123.79(17) . . ? C14 Fe1 C19 110.38(17) . . ? C17 Fe1 C11 121.91(17) . . ? C12 Fe1 C11 40.60(17) . . ? C18 Fe1 C11 156.74(16) . . ? C13 Fe1 C11 68.25(17) . . ? C14 Fe1 C11 68.61(17) . . ? C19 Fe1 C11 161.67(16) . . ? C17 Fe1 C16 40.36(15) . . ? C12 Fe1 C16 117.79(18) . . ? C18 Fe1 C16 68.02(16) . . ? C13 Fe1 C16 150.98(16) . . ? C14 Fe1 C16 167.06(15) . . ? C19 Fe1 C16 68.54(16) . . ? C11 Fe1 C16 108.11(16) . . ? C17 Fe1 C15 67.48(15) . . ? C12 Fe1 C15 156.17(17) . . ? C18 Fe1 C15 67.40(15) . . ? C13 Fe1 C15 163.27(17) . . ? C14 Fe1 C15 130.44(16) . . ? C19 Fe1 C15 40.35(14) . . ? C11 Fe1 C15 125.55(15) . . ? C16 Fe1 C15 40.55(15) . . ? C17 Fe1 C10 161.37(17) . . ? C12 Fe1 C10 67.47(16) . . ? C18 Fe1 C10 158.26(17) . . ? C13 Fe1 C10 67.41(16) . . ? C14 Fe1 C10 40.22(16) . . ? C19 Fe1 C10 127.21(16) . . ? C11 Fe1 C10 40.29(15) . . ? C16 Fe1 C10 129.45(15) . . ? C15 Fe1 C10 115.68(15) . . ? C1 N1 C2 111.3(3) . . ? C1 N1 C8 124.5(3) . . ? C2 N1 C8 124.2(3) . . ? C1 N2 C7 110.3(3) . . ? C1 N2 C10 124.1(3) . . ? C7 N2 C10 125.5(3) . . ? C20 N3 C21 110.1(3) . . ? C20 N3 C27 125.7(3) . . ? C21 N3 C27 124.1(3) . . ? C20 N4 C26 110.1(3) . . ? C20 N4 C15 123.7(3) . . ? C26 N4 C15 126.2(3) . . ? N1 C1 N2 106.0(3) . . ? N1 C1 Ir1 125.3(3) . . ? N2 C1 Ir1 128.5(3) . . ? C7 C2 C3 121.8(3) . . ? C7 C2 N1 106.2(3) . . ? C3 C2 N1 132.0(3) . . ? C4 C3 C2 116.9(4) . . ? C4 C3 H3 121.5 . . ? C2 C3 H3 121.5 . . ? C3 C4 C5 121.7(4) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 116.6(4) . . ? C5 C6 H6 121.7 . . ? C7 C6 H6 121.7 . . ? C2 C7 C6 121.3(3) . . ? C2 C7 N2 106.1(3) . . ? C6 C7 N2 132.5(3) . . ? N1 C8 C9 112.5(3) . . ? N1 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C10 C11 109.4(4) . . ? C14 C10 N2 124.9(3) . . ? C11 C10 N2 125.4(4) . . ? C14 C10 Fe1 69.4(2) . . ? C11 C10 Fe1 69.4(2) . . ? N2 C10 Fe1 131.9(3) . . ? C10 C11 C12 106.8(4) . . ? C10 C11 Fe1 70.3(2) . . ? C12 C11 Fe1 69.1(2) . . ? C10 C11 H11 126.6 . . ? C12 C11 H11 126.6 . . ? Fe1 C11 H11 125.6 . . ? C13 C12 C11 108.6(4) . . ? C13 C12 Fe1 70.0(2) . . ? C11 C12 Fe1 70.3(2) . . ? C13 C12 H12 125.7 . . ? C11 C12 H12 125.7 . . ? Fe1 C12 H12 125.6 . . ? C12 C13 C14 108.5(4) . . ? C12 C13 Fe1 69.6(2) . . ? C14 C13 Fe1 70.1(2) . . ? C12 C13 H13 125.8 . . ? C14 C13 H13 125.8 . . ? Fe1 C13 H13 126.2 . . ? C10 C14 C13 106.6(4) . . ? C10 C14 Fe1 70.4(2) . . ? C13 C14 Fe1 69.2(2) . . ? C10 C14 H14 126.7 . . ? C13 C14 H14 126.7 . . ? Fe1 C14 H14 125.4 . . ? C19 C15 C16 108.7(3) . . ? C19 C15 N4 126.1(3) . . ? C16 C15 N4 124.8(3) . . ? C19 C15 Fe1 69.5(2) . . ? C16 C15 Fe1 69.4(2) . . ? N4 C15 Fe1 132.3(2) . . ? C17 C16 C15 106.6(3) . . ? C17 C16 Fe1 69.1(2) . . ? C15 C16 Fe1 70.0(2) . . ? C17 C16 H16 126.7 . . ? C15 C16 H16 126.7 . . ? Fe1 C16 H16 125.8 . . ? C18 C17 C16 108.9(4) . . ? C18 C17 Fe1 69.9(2) . . ? C16 C17 Fe1 70.6(2) . . ? C18 C17 H17 125.5 . . ? C16 C17 H17 125.5 . . ? Fe1 C17 H17 125.5 . . ? C17 C18 C19 108.8(4) . . ? C17 C18 Fe1 69.8(2) . . ? C19 C18 Fe1 70.4(2) . . ? C17 C18 H18 125.6 . . ? C19 C18 H18 125.6 . . ? Fe1 C18 H18 125.7 . . ? C18 C19 C15 106.9(3) . . ? C18 C19 Fe1 69.2(2) . . ? C15 C19 Fe1 70.2(2) . . ? C18 C19 H19 126.5 . . ? C15 C19 H19 126.5 . . ? Fe1 C19 H19 125.7 . . ? N3 C20 N4 106.9(3) . . ? N3 C20 Ir2 123.3(3) . . ? N4 C20 Ir2 129.8(3) . . ? C26 C21 C22 121.5(3) . . ? C26 C21 N3 107.3(3) . . ? C22 C21 N3 131.2(3) . . ? C23 C22 C21 116.9(4) . . ? C23 C22 H22 121.6 . . ? C21 C22 H22 121.6 . . ? C22 C23 C24 121.7(3) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C25 C24 C23 121.4(3) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C26 C25 C24 116.6(4) . . ? C26 C25 H25 121.7 . . ? C24 C25 H25 121.7 . . ? C21 C26 C25 121.9(3) . . ? C21 C26 N4 105.5(3) . . ? C25 C26 N4 132.6(3) . . ? N3 C27 C28 111.5(3) . . ? N3 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? N3 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O1A C1A Ir1 178.3(4) . . ? O2A C2A Ir1 177.6(6) . . ? O3A C3A Ir2 179.3(5) . . ? O4A C4A Ir2 177.4(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 -0.2(4) . . . . ? C8 N1 C1 N2 177.1(3) . . . . ? C2 N1 C1 Ir1 175.5(2) . . . . ? C8 N1 C1 Ir1 -7.2(5) . . . . ? C7 N2 C1 N1 0.3(4) . . . . ? C10 N2 C1 N1 -177.7(3) . . . . ? C7 N2 C1 Ir1 -175.1(3) . . . . ? C10 N2 C1 Ir1 6.9(5) . . . . ? C2A Ir1 C1 N1 -102.4(3) . . . . ? Cl1 Ir1 C1 N1 80.6(3) . . . . ? C2A Ir1 C1 N2 72.2(4) . . . . ? Cl1 Ir1 C1 N2 -104.7(3) . . . . ? C1 N1 C2 C7 0.0(4) . . . . ? C8 N1 C2 C7 -177.4(3) . . . . ? C1 N1 C2 C3 179.8(4) . . . . ? C8 N1 C2 C3 2.5(6) . . . . ? C7 C2 C3 C4 0.1(6) . . . . ? N1 C2 C3 C4 -179.7(4) . . . . ? C2 C3 C4 C5 0.4(6) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? C4 C5 C6 C7 -0.2(6) . . . . ? C3 C2 C7 C6 -0.6(6) . . . . ? N1 C2 C7 C6 179.2(3) . . . . ? C3 C2 C7 N2 -179.6(3) . . . . ? N1 C2 C7 N2 0.2(4) . . . . ? C5 C6 C7 C2 0.7(5) . . . . ? C5 C6 C7 N2 179.3(4) . . . . ? C1 N2 C7 C2 -0.4(4) . . . . ? C10 N2 C7 C2 177.6(3) . . . . ? C1 N2 C7 C6 -179.2(4) . . . . ? C10 N2 C7 C6 -1.2(6) . . . . ? C1 N1 C8 C9 103.7(5) . . . . ? C2 N1 C8 C9 -79.3(5) . . . . ? C1 N2 C10 C14 28.7(5) . . . . ? C7 N2 C10 C14 -149.0(4) . . . . ? C1 N2 C10 C11 -145.1(4) . . . . ? C7 N2 C10 C11 37.2(5) . . . . ? C1 N2 C10 Fe1 121.6(4) . . . . ? C7 N2 C10 Fe1 -56.1(5) . . . . ? C17 Fe1 C10 C14 -141.4(5) . . . . ? C12 Fe1 C10 C14 -82.8(3) . . . . ? C18 Fe1 C10 C14 30.0(5) . . . . ? C13 Fe1 C10 C14 -38.9(2) . . . . ? C19 Fe1 C10 C14 77.3(3) . . . . ? C11 Fe1 C10 C14 -121.4(3) . . . . ? C16 Fe1 C10 C14 169.0(2) . . . . ? C15 Fe1 C10 C14 123.1(2) . . . . ? C17 Fe1 C10 C11 -20.0(6) . . . . ? C12 Fe1 C10 C11 38.6(3) . . . . ? C18 Fe1 C10 C11 151.4(4) . . . . ? C13 Fe1 C10 C11 82.5(3) . . . . ? C14 Fe1 C10 C11 121.4(3) . . . . ? C19 Fe1 C10 C11 -161.3(2) . . . . ? C16 Fe1 C10 C11 -69.6(3) . . . . ? C15 Fe1 C10 C11 -115.5(2) . . . . ? C17 Fe1 C10 N2 99.6(6) . . . . ? C12 Fe1 C10 N2 158.2(4) . . . . ? C18 Fe1 C10 N2 -89.0(6) . . . . ? C13 Fe1 C10 N2 -157.8(4) . . . . ? C14 Fe1 C10 N2 -119.0(5) . . . . ? C19 Fe1 C10 N2 -41.7(4) . . . . ? C11 Fe1 C10 N2 119.6(5) . . . . ? C16 Fe1 C10 N2 50.0(4) . . . . ? C15 Fe1 C10 N2 4.1(4) . . . . ? C14 C10 C11 C12 -1.8(4) . . . . ? N2 C10 C11 C12 172.9(3) . . . . ? Fe1 C10 C11 C12 -59.7(3) . . . . ? C14 C10 C11 Fe1 57.9(3) . . . . ? N2 C10 C11 Fe1 -127.4(4) . . . . ? C17 Fe1 C11 C10 172.6(2) . . . . ? C12 Fe1 C11 C10 -117.7(4) . . . . ? C18 Fe1 C11 C10 -153.3(4) . . . . ? C13 Fe1 C11 C10 -80.3(3) . . . . ? C14 Fe1 C11 C10 -36.3(2) . . . . ? C19 Fe1 C11 C10 54.1(6) . . . . ? C16 Fe1 C11 C10 130.4(2) . . . . ? C15 Fe1 C11 C10 88.9(3) . . . . ? C17 Fe1 C11 C12 -69.7(3) . . . . ? C18 Fe1 C11 C12 -35.5(5) . . . . ? C13 Fe1 C11 C12 37.5(3) . . . . ? C14 Fe1 C11 C12 81.4(3) . . . . ? C19 Fe1 C11 C12 171.8(5) . . . . ? C16 Fe1 C11 C12 -111.9(3) . . . . ? C15 Fe1 C11 C12 -153.4(2) . . . . ? C10 Fe1 C11 C12 117.7(4) . . . . ? C10 C11 C12 C13 0.8(4) . . . . ? Fe1 C11 C12 C13 -59.7(3) . . . . ? C10 C11 C12 Fe1 60.5(3) . . . . ? C17 Fe1 C12 C13 -115.1(2) . . . . ? C18 Fe1 C12 C13 -75.8(3) . . . . ? C14 Fe1 C12 C13 37.6(2) . . . . ? C19 Fe1 C12 C13 -53.9(5) . . . . ? C11 Fe1 C12 C13 119.4(3) . . . . ? C16 Fe1 C12 C13 -154.9(2) . . . . ? C15 Fe1 C12 C13 -176.1(3) . . . . ? C10 Fe1 C12 C13 81.1(3) . . . . ? C17 Fe1 C12 C11 125.5(2) . . . . ? C18 Fe1 C12 C11 164.8(2) . . . . ? C13 Fe1 C12 C11 -119.4(3) . . . . ? C14 Fe1 C12 C11 -81.8(3) . . . . ? C19 Fe1 C12 C11 -173.3(4) . . . . ? C16 Fe1 C12 C11 85.7(3) . . . . ? C15 Fe1 C12 C11 64.5(5) . . . . ? C10 Fe1 C12 C11 -38.3(2) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? Fe1 C12 C13 C14 -59.5(3) . . . . ? C11 C12 C13 Fe1 60.0(3) . . . . ? C17 Fe1 C13 C12 78.5(3) . . . . ? C18 Fe1 C13 C12 119.5(3) . . . . ? C14 Fe1 C13 C12 -119.6(4) . . . . ? C19 Fe1 C13 C12 158.1(2) . . . . ? C11 Fe1 C13 C12 -37.6(2) . . . . ? C16 Fe1 C13 C12 50.7(4) . . . . ? C15 Fe1 C13 C12 174.5(5) . . . . ? C10 Fe1 C13 C12 -81.3(3) . . . . ? C17 Fe1 C13 C14 -161.8(2) . . . . ? C12 Fe1 C13 C14 119.6(4) . . . . ? C18 Fe1 C13 C14 -120.8(3) . . . . ? C19 Fe1 C13 C14 -82.3(3) . . . . ? C11 Fe1 C13 C14 82.0(3) . . . . ? C16 Fe1 C13 C14 170.3(3) . . . . ? C15 Fe1 C13 C14 -65.9(6) . . . . ? C10 Fe1 C13 C14 38.4(2) . . . . ? C11 C10 C14 C13 2.1(4) . . . . ? N2 C10 C14 C13 -172.7(3) . . . . ? Fe1 C10 C14 C13 60.0(3) . . . . ? C11 C10 C14 Fe1 -57.9(3) . . . . ? N2 C10 C14 Fe1 127.4(4) . . . . ? C12 C13 C14 C10 -1.5(4) . . . . ? Fe1 C13 C14 C10 -60.7(2) . . . . ? C12 C13 C14 Fe1 59.2(3) . . . . ? C17 Fe1 C14 C10 154.7(3) . . . . ? C12 Fe1 C14 C10 80.1(2) . . . . ? C18 Fe1 C14 C10 -167.7(2) . . . . ? C13 Fe1 C14 C10 117.4(4) . . . . ? C19 Fe1 C14 C10 -124.0(2) . . . . ? C11 Fe1 C14 C10 36.4(2) . . . . ? C16 Fe1 C14 C10 -41.3(8) . . . . ? C15 Fe1 C14 C10 -82.8(3) . . . . ? C17 Fe1 C14 C13 37.2(5) . . . . ? C12 Fe1 C14 C13 -37.3(3) . . . . ? C18 Fe1 C14 C13 74.9(3) . . . . ? C19 Fe1 C14 C13 118.5(3) . . . . ? C11 Fe1 C14 C13 -81.1(3) . . . . ? C16 Fe1 C14 C13 -158.7(7) . . . . ? C15 Fe1 C14 C13 159.8(2) . . . . ? C10 Fe1 C14 C13 -117.4(4) . . . . ? C20 N4 C15 C19 -133.3(4) . . . . ? C26 N4 C15 C19 44.2(5) . . . . ? C20 N4 C15 C16 39.2(5) . . . . ? C26 N4 C15 C16 -143.3(4) . . . . ? C20 N4 C15 Fe1 132.3(3) . . . . ? C26 N4 C15 Fe1 -50.1(5) . . . . ? C17 Fe1 C15 C19 82.1(2) . . . . ? C12 Fe1 C15 C19 149.9(4) . . . . ? C18 Fe1 C15 C19 38.3(2) . . . . ? C13 Fe1 C15 C19 -21.2(6) . . . . ? C14 Fe1 C15 C19 -72.8(3) . . . . ? C11 Fe1 C15 C19 -163.9(2) . . . . ? C16 Fe1 C15 C19 120.4(3) . . . . ? C10 Fe1 C15 C19 -118.1(2) . . . . ? C17 Fe1 C15 C16 -38.4(2) . . . . ? C12 Fe1 C15 C16 29.4(5) . . . . ? C18 Fe1 C15 C16 -82.1(2) . . . . ? C13 Fe1 C15 C16 -141.7(5) . . . . ? C14 Fe1 C15 C16 166.8(2) . . . . ? C19 Fe1 C15 C16 -120.4(3) . . . . ? C11 Fe1 C15 C16 75.7(3) . . . . ? C10 Fe1 C15 C16 121.5(2) . . . . ? C17 Fe1 C15 N4 -157.3(4) . . . . ? C12 Fe1 C15 N4 -89.5(5) . . . . ? C18 Fe1 C15 N4 159.0(4) . . . . ? C13 Fe1 C15 N4 99.4(6) . . . . ? C14 Fe1 C15 N4 47.9(4) . . . . ? C19 Fe1 C15 N4 120.6(4) . . . . ? C11 Fe1 C15 N4 -43.3(4) . . . . ? C16 Fe1 C15 N4 -118.9(4) . . . . ? C10 Fe1 C15 N4 2.6(4) . . . . ? C19 C15 C16 C17 1.2(4) . . . . ? N4 C15 C16 C17 -172.5(3) . . . . ? Fe1 C15 C16 C17 59.6(3) . . . . ? C19 C15 C16 Fe1 -58.5(3) . . . . ? N4 C15 C16 Fe1 127.9(3) . . . . ? C12 Fe1 C16 C17 75.2(3) . . . . ? C18 Fe1 C16 C17 -37.3(2) . . . . ? C13 Fe1 C16 C17 40.7(4) . . . . ? C14 Fe1 C16 C17 -168.6(7) . . . . ? C19 Fe1 C16 C17 -80.9(3) . . . . ? C11 Fe1 C16 C17 118.3(3) . . . . ? C15 Fe1 C16 C17 -117.7(3) . . . . ? C10 Fe1 C16 C17 157.9(2) . . . . ? C17 Fe1 C16 C15 117.7(3) . . . . ? C12 Fe1 C16 C15 -167.0(2) . . . . ? C18 Fe1 C16 C15 80.5(2) . . . . ? C13 Fe1 C16 C15 158.4(3) . . . . ? C14 Fe1 C16 C15 -50.9(8) . . . . ? C19 Fe1 C16 C15 36.9(2) . . . . ? C11 Fe1 C16 C15 -124.0(2) . . . . ? C10 Fe1 C16 C15 -84.3(3) . . . . ? C15 C16 C17 C18 -0.6(4) . . . . ? Fe1 C16 C17 C18 59.6(3) . . . . ? C15 C16 C17 Fe1 -60.3(3) . . . . ? C12 Fe1 C17 C18 121.3(3) . . . . ? C13 Fe1 C17 C18 80.8(3) . . . . ? C14 Fe1 C17 C18 54.9(5) . . . . ? C19 Fe1 C17 C18 -37.4(2) . . . . ? C11 Fe1 C17 C18 160.0(2) . . . . ? C16 Fe1 C17 C18 -119.7(4) . . . . ? C15 Fe1 C17 C18 -81.1(3) . . . . ? C10 Fe1 C17 C18 175.1(4) . . . . ? C12 Fe1 C17 C16 -119.0(3) . . . . ? C18 Fe1 C17 C16 119.7(4) . . . . ? C13 Fe1 C17 C16 -159.5(2) . . . . ? C14 Fe1 C17 C16 174.6(3) . . . . ? C19 Fe1 C17 C16 82.3(3) . . . . ? C11 Fe1 C17 C16 -80.4(3) . . . . ? C15 Fe1 C17 C16 38.5(2) . . . . ? C10 Fe1 C17 C16 -65.3(6) . . . . ? C16 C17 C18 C19 -0.2(5) . . . . ? Fe1 C17 C18 C19 59.9(3) . . . . ? C16 C17 C18 Fe1 -60.0(3) . . . . ? C12 Fe1 C18 C17 -73.1(3) . . . . ? C13 Fe1 C18 C17 -113.4(3) . . . . ? C14 Fe1 C18 C17 -153.9(2) . . . . ? C19 Fe1 C18 C17 119.6(3) . . . . ? C11 Fe1 C18 C17 -47.5(5) . . . . ? C16 Fe1 C18 C17 37.4(2) . . . . ? C15 Fe1 C18 C17 81.3(3) . . . . ? C10 Fe1 C18 C17 -175.7(4) . . . . ? C17 Fe1 C18 C19 -119.6(3) . . . . ? C12 Fe1 C18 C19 167.2(2) . . . . ? C13 Fe1 C18 C19 126.9(2) . . . . ? C14 Fe1 C18 C19 86.5(3) . . . . ? C11 Fe1 C18 C19 -167.1(4) . . . . ? C16 Fe1 C18 C19 -82.3(2) . . . . ? C15 Fe1 C18 C19 -38.3(2) . . . . ? C10 Fe1 C18 C19 64.6(5) . . . . ? C17 C18 C19 C15 0.9(4) . . . . ? Fe1 C18 C19 C15 60.3(3) . . . . ? C17 C18 C19 Fe1 -59.5(3) . . . . ? C16 C15 C19 C18 -1.2(4) . . . . ? N4 C15 C19 C18 172.3(3) . . . . ? Fe1 C15 C19 C18 -59.7(3) . . . . ? C16 C15 C19 Fe1 58.5(3) . . . . ? N4 C15 C19 Fe1 -128.0(3) . . . . ? C17 Fe1 C19 C18 37.3(2) . . . . ? C12 Fe1 C19 C18 -30.2(5) . . . . ? C13 Fe1 C19 C18 -69.3(3) . . . . ? C14 Fe1 C19 C18 -112.9(2) . . . . ? C11 Fe1 C19 C18 163.7(5) . . . . ? C16 Fe1 C19 C18 80.9(3) . . . . ? C15 Fe1 C19 C18 117.9(3) . . . . ? C10 Fe1 C19 C18 -155.2(2) . . . . ? C17 Fe1 C19 C15 -80.6(2) . . . . ? C12 Fe1 C19 C15 -148.1(4) . . . . ? C18 Fe1 C19 C15 -117.9(3) . . . . ? C13 Fe1 C19 C15 172.8(2) . . . . ? C14 Fe1 C19 C15 129.2(2) . . . . ? C11 Fe1 C19 C15 45.8(6) . . . . ? C16 Fe1 C19 C15 -37.0(2) . . . . ? C10 Fe1 C19 C15 86.9(3) . . . . ? C21 N3 C20 N4 0.5(4) . . . . ? C27 N3 C20 N4 -176.4(3) . . . . ? C21 N3 C20 Ir2 -178.5(2) . . . . ? C27 N3 C20 Ir2 4.6(5) . . . . ? C26 N4 C20 N3 1.1(4) . . . . ? C15 N4 C20 N3 179.0(3) . . . . ? C26 N4 C20 Ir2 180.0(3) . . . . ? C15 N4 C20 Ir2 -2.1(5) . . . . ? C3A Ir2 C20 N3 -89.2(3) . . . . ? Cl2 Ir2 C20 N3 89.2(3) . . . . ? C3A Ir2 C20 N4 92.1(4) . . . . ? Cl2 Ir2 C20 N4 -89.5(3) . . . . ? C20 N3 C21 C26 -1.9(4) . . . . ? C27 N3 C21 C26 175.1(3) . . . . ? C20 N3 C21 C22 179.3(4) . . . . ? C27 N3 C21 C22 -3.7(6) . . . . ? C26 C21 C22 C23 -1.1(5) . . . . ? N3 C21 C22 C23 177.6(4) . . . . ? C21 C22 C23 C24 -1.0(5) . . . . ? C22 C23 C24 C25 1.8(6) . . . . ? C23 C24 C25 C26 -0.3(5) . . . . ? C22 C21 C26 C25 2.6(5) . . . . ? N3 C21 C26 C25 -176.3(3) . . . . ? C22 C21 C26 N4 -178.6(3) . . . . ? N3 C21 C26 N4 2.4(4) . . . . ? C24 C25 C26 C21 -1.8(5) . . . . ? C24 C25 C26 N4 179.8(4) . . . . ? C20 N4 C26 C21 -2.2(4) . . . . ? C15 N4 C26 C21 180.0(3) . . . . ? C20 N4 C26 C25 176.4(4) . . . . ? C15 N4 C26 C25 -1.5(6) . . . . ? C20 N3 C27 C28 -98.6(4) . . . . ? C21 N3 C27 C28 84.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.819 _refine_diff_density_min -1.384 _refine_diff_density_rms 0.134 #===END #===END data_dimer _database_code_depnum_ccdc_archive 'CCDC 729834' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2 C14 H13 N2, 2 C8 H12, 2 Ir, 2Cl, Fe' _chemical_formula_sum 'C44 H50 Cl2 Fe Ir2 N4' _chemical_formula_weight 1146.03 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' Cl Cl 0.1484 0.1585 '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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.6278(6) _cell_length_b 10.6387(4) _cell_length_c 18.5406(6) _cell_angle_alpha 90.00 _cell_angle_beta 120.241(2) _cell_angle_gamma 90.00 _cell_volume 3855.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4552 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prisms _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 7.434 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.428 _exptl_absorpt_correction_T_max 0.708 _exptl_absorpt_process_details ; N. W. Alcock (1970). Cryst. Computing, p271 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _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 \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25726 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4435 _reflns_number_gt 3810 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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^)+(0.0247P)^2^+13.8520P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4435 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 Ir1 Ir 0.386259(7) 0.303993(14) -0.034566(8) 0.02462(6) Uani 1 1 d . . . Fe1 Fe 0.5000 0.50445(7) 0.2500 0.02672(18) Uani 1 2 d S . . Cl1 Cl 0.50006(5) 0.26114(10) -0.00253(6) 0.0338(2) Uani 1 1 d . . . N1 N 0.41340(17) 0.2665(3) 0.14217(19) 0.0241(7) Uani 1 1 d . . . N2 N 0.39787(17) 0.0865(3) 0.07951(19) 0.0269(7) Uani 1 1 d . . . C1 C 0.4013(2) 0.2119(4) 0.0690(2) 0.0266(8) Uani 1 1 d . . . C2 C 0.4071(2) 0.0610(4) 0.1586(2) 0.0282(8) Uani 1 1 d . . . C3 C 0.4097(2) -0.0515(4) 0.1973(3) 0.0364(10) Uani 1 1 d . . . H3 H 0.4038 -0.1298 0.1698 0.044 Uiso 1 1 calc R . . C4 C 0.4214(2) -0.0450(4) 0.2780(3) 0.0374(10) Uani 1 1 d . . . H4 H 0.4230 -0.1204 0.3064 0.045 Uiso 1 1 calc R . . C5 C 0.4309(2) 0.0706(4) 0.3187(2) 0.0324(9) Uani 1 1 d . . . H5 H 0.4386 0.0718 0.3741 0.039 Uiso 1 1 calc R . . C6 C 0.4293(2) 0.1834(4) 0.2802(2) 0.0259(8) Uani 1 1 d . . . H6 H 0.4363 0.2618 0.3079 0.031 Uiso 1 1 calc R . . C7 C 0.4169(2) 0.1758(3) 0.1985(2) 0.0249(8) Uani 1 1 d . . . C8 C 0.3931(2) -0.0091(4) 0.0192(3) 0.0351(10) Uani 1 1 d . . . H8A H 0.4304 -0.0710 0.0488 0.042 Uiso 1 1 calc R . . H8B H 0.4002 0.0323 -0.0237 0.042 Uiso 1 1 calc R . . C9 C 0.3258(3) -0.0780(5) -0.0237(3) 0.0542(13) Uani 1 1 d . . . H9A H 0.3185 -0.1202 0.0181 0.081 Uiso 1 1 calc R . . H9B H 0.3264 -0.1406 -0.0621 0.081 Uiso 1 1 calc R . . H9C H 0.2886 -0.0180 -0.0552 0.081 Uiso 1 1 calc R . . C10 C 0.4228(2) 0.3985(3) 0.1568(2) 0.0256(8) Uani 1 1 d . . . C11 C 0.4535(2) 0.4788(4) 0.1232(2) 0.0273(8) Uani 1 1 d . . . H11 H 0.4758 0.4531 0.0939 0.033 Uiso 1 1 calc R . . C12 C 0.4443(2) 0.6041(4) 0.1416(3) 0.0334(9) Uani 1 1 d . . . H12 H 0.4588 0.6776 0.1258 0.040 Uiso 1 1 calc R . . C13 C 0.4097(2) 0.6010(4) 0.1879(3) 0.0350(10) Uani 1 1 d . . . H13 H 0.3977 0.6721 0.2088 0.042 Uiso 1 1 calc R . . C14 C 0.3962(2) 0.4727(4) 0.1975(2) 0.0309(9) Uani 1 1 d . . . H14 H 0.3737 0.4428 0.2257 0.037 Uiso 1 1 calc R . . C1A C 0.3601(2) 0.3551(4) -0.1612(2) 0.0341(9) Uani 1 1 d . . . H1A H 0.3953 0.2994 -0.1547 0.041 Uiso 1 1 calc R . . C2A C 0.3794(2) 0.4631(4) -0.1126(3) 0.0320(9) Uani 1 1 d . . . H2A H 0.4270 0.4765 -0.0763 0.038 Uiso 1 1 calc R . . C3A C 0.3320(3) 0.5592(4) -0.1126(4) 0.0515(13) Uani 1 1 d . . . H3A1 H 0.3598 0.6274 -0.0740 0.062 Uiso 1 1 calc R . . H3A2 H 0.3064 0.5960 -0.1693 0.062 Uiso 1 1 calc R . . C4A C 0.2825(3) 0.5181(6) -0.0891(5) 0.075(2) Uani 1 1 d . . . H4A1 H 0.2364 0.5184 -0.1395 0.090 Uiso 1 1 calc R . . H4A2 H 0.2821 0.5799 -0.0494 0.090 Uiso 1 1 calc R . . C5A C 0.2960(2) 0.3888(5) -0.0496(3) 0.0415(11) Uani 1 1 d . . . H5A H 0.3169 0.3842 0.0094 0.050 Uiso 1 1 calc R . . C6A C 0.2797(2) 0.2762(6) -0.0939(3) 0.0456(12) Uani 1 1 d . . . H6A H 0.2884 0.2006 -0.0628 0.055 Uiso 1 1 calc R . . C7A C 0.2495(3) 0.2641(9) -0.1871(3) 0.084(2) Uani 1 1 d . . . H7A1 H 0.2436 0.1735 -0.2012 0.101 Uiso 1 1 calc R . . H7A2 H 0.2033 0.3022 -0.2147 0.101 Uiso 1 1 calc R . . C8A C 0.2876(3) 0.3202(5) -0.2234(3) 0.0533(14) Uani 1 1 d . . . H8A1 H 0.2631 0.3966 -0.2547 0.064 Uiso 1 1 calc R . . H8A2 H 0.2879 0.2602 -0.2640 0.064 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 Ir1 0.02775(10) 0.02878(10) 0.02089(9) 0.00140(6) 0.01489(7) 0.00240(6) Fe1 0.0466(5) 0.0177(4) 0.0259(4) 0.000 0.0256(4) 0.000 Cl1 0.0329(5) 0.0408(6) 0.0345(5) 0.0036(4) 0.0221(4) 0.0071(4) N1 0.0321(18) 0.0234(16) 0.0201(15) 0.0024(13) 0.0155(14) 0.0031(14) N2 0.0352(18) 0.0222(16) 0.0250(16) -0.0024(13) 0.0165(14) -0.0011(14) C1 0.029(2) 0.029(2) 0.0252(19) 0.0024(16) 0.0167(17) 0.0041(16) C2 0.029(2) 0.029(2) 0.028(2) -0.0003(17) 0.0151(17) -0.0007(17) C3 0.045(3) 0.021(2) 0.041(2) 0.0024(18) 0.020(2) -0.0020(18) C4 0.046(3) 0.027(2) 0.039(2) 0.0103(19) 0.021(2) -0.0035(19) C5 0.032(2) 0.040(2) 0.026(2) 0.0048(18) 0.0149(17) -0.0026(18) C6 0.028(2) 0.028(2) 0.0245(19) 0.0006(16) 0.0151(17) -0.0011(16) C7 0.028(2) 0.0221(18) 0.028(2) 0.0043(15) 0.0159(17) 0.0006(15) C8 0.050(3) 0.026(2) 0.034(2) -0.0054(18) 0.024(2) 0.0014(19) C9 0.062(3) 0.051(3) 0.049(3) -0.025(3) 0.027(3) -0.012(3) C10 0.037(2) 0.0213(18) 0.0229(18) 0.0023(15) 0.0187(17) 0.0041(16) C11 0.038(2) 0.028(2) 0.0228(19) 0.0023(16) 0.0200(18) -0.0001(17) C12 0.056(3) 0.0224(19) 0.031(2) 0.0072(17) 0.028(2) 0.0043(19) C13 0.059(3) 0.023(2) 0.034(2) 0.0020(18) 0.033(2) 0.007(2) C14 0.045(2) 0.028(2) 0.030(2) 0.0066(17) 0.026(2) 0.0079(18) C1A 0.043(3) 0.039(2) 0.023(2) 0.0035(18) 0.0189(19) 0.000(2) C2A 0.034(2) 0.036(2) 0.029(2) 0.0032(18) 0.0178(18) -0.0019(18) C3A 0.063(3) 0.032(2) 0.073(4) 0.011(2) 0.044(3) 0.009(2) C4A 0.082(4) 0.072(4) 0.104(5) 0.048(4) 0.073(4) 0.046(4) C5A 0.035(2) 0.059(3) 0.041(2) 0.018(2) 0.026(2) 0.019(2) C6A 0.024(2) 0.072(3) 0.036(2) 0.010(2) 0.012(2) 0.001(2) C7A 0.034(3) 0.174(7) 0.034(3) -0.009(4) 0.009(2) -0.030(4) C8A 0.060(3) 0.071(4) 0.023(2) -0.009(2) 0.016(2) -0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 2.026(4) . ? Ir1 C6A 2.106(5) . ? Ir1 C5A 2.119(4) . ? Ir1 C2A 2.181(4) . ? Ir1 C1A 2.182(4) . ? Ir1 Cl1 2.3772(10) . ? Fe1 C13 2.046(4) 2_655 ? Fe1 C13 2.046(4) . ? Fe1 C12 2.049(4) 2_655 ? Fe1 C12 2.049(4) . ? Fe1 C11 2.053(4) . ? Fe1 C11 2.053(4) 2_655 ? Fe1 C10 2.065(4) . ? Fe1 C10 2.065(4) 2_655 ? Fe1 C14 2.068(4) . ? Fe1 C14 2.068(4) 2_655 ? N1 C1 1.371(5) . ? N1 C7 1.395(5) . ? N1 C10 1.426(5) . ? N2 C1 1.355(5) . ? N2 C2 1.400(5) . ? N2 C8 1.475(5) . ? C2 C3 1.381(6) . ? C2 C7 1.386(5) . ? C3 C4 1.384(6) . ? C3 H3 0.9500 . ? C4 C5 1.402(6) . ? C4 H4 0.9500 . ? C5 C6 1.388(5) . ? C5 H5 0.9500 . ? C6 C7 1.397(5) . ? C6 H6 0.9500 . ? C8 C9 1.506(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C14 1.419(5) . ? C10 C11 1.426(5) . ? C11 C12 1.416(6) . ? C11 H11 0.9500 . ? C12 C13 1.425(5) . ? C12 H12 0.9500 . ? C13 C14 1.430(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C1A C2A 1.388(6) . ? C1A C8A 1.502(7) . ? C1A H1A 0.9500 . ? C2A C3A 1.482(6) . ? C2A H2A 0.9500 . ? C3A C4A 1.459(7) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A C5A 1.515(7) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5A C6A 1.393(7) . ? C5A H5A 0.9500 . ? C6A C7A 1.510(7) . ? C6A H6A 0.9500 . ? C7A C8A 1.461(8) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A H8A1 0.9900 . ? C8A H8A2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir1 C6A 91.62(18) . . ? C1 Ir1 C5A 91.19(16) . . ? C6A Ir1 C5A 38.5(2) . . ? C1 Ir1 C2A 157.82(16) . . ? C6A Ir1 C2A 94.71(18) . . ? C5A Ir1 C2A 80.82(16) . . ? C1 Ir1 C1A 164.94(16) . . ? C6A Ir1 C1A 81.62(18) . . ? C5A Ir1 C1A 91.79(17) . . ? C2A Ir1 C1A 37.09(16) . . ? C1 Ir1 Cl1 91.56(11) . . ? C6A Ir1 Cl1 156.10(16) . . ? C5A Ir1 Cl1 164.94(15) . . ? C2A Ir1 Cl1 91.19(11) . . ? C1A Ir1 Cl1 89.39(12) . . ? C13 Fe1 C13 119.7(2) 2_655 . ? C13 Fe1 C12 40.71(16) 2_655 2_655 ? C13 Fe1 C12 103.79(17) . 2_655 ? C13 Fe1 C12 103.79(17) 2_655 . ? C13 Fe1 C12 40.71(16) . . ? C12 Fe1 C12 117.7(2) 2_655 . ? C13 Fe1 C11 120.13(15) 2_655 . ? C13 Fe1 C11 68.37(16) . . ? C12 Fe1 C11 154.02(16) 2_655 . ? C12 Fe1 C11 40.39(15) . . ? C13 Fe1 C11 68.37(16) 2_655 2_655 ? C13 Fe1 C11 120.13(15) . 2_655 ? C12 Fe1 C11 40.39(15) 2_655 2_655 ? C12 Fe1 C11 154.02(16) . 2_655 ? C11 Fe1 C11 164.7(2) . 2_655 ? C13 Fe1 C10 158.24(14) 2_655 . ? C13 Fe1 C10 67.62(16) . . ? C12 Fe1 C10 161.04(15) 2_655 . ? C12 Fe1 C10 67.59(16) . . ? C11 Fe1 C10 40.51(15) . . ? C11 Fe1 C10 127.98(15) 2_655 . ? C13 Fe1 C10 67.62(16) 2_655 2_655 ? C13 Fe1 C10 158.24(14) . 2_655 ? C12 Fe1 C10 67.59(16) 2_655 2_655 ? C12 Fe1 C10 161.04(15) . 2_655 ? C11 Fe1 C10 127.98(15) . 2_655 ? C11 Fe1 C10 40.51(15) 2_655 2_655 ? C10 Fe1 C10 113.9(2) . 2_655 ? C13 Fe1 C14 157.29(17) 2_655 . ? C13 Fe1 C14 40.68(16) . . ? C12 Fe1 C14 122.50(16) 2_655 . ? C12 Fe1 C14 68.39(16) . . ? C11 Fe1 C14 68.51(15) . . ? C11 Fe1 C14 108.85(15) 2_655 . ? C10 Fe1 C14 40.16(15) . . ? C10 Fe1 C14 125.87(15) 2_655 . ? C13 Fe1 C14 40.68(16) 2_655 2_655 ? C13 Fe1 C14 157.29(17) . 2_655 ? C12 Fe1 C14 68.39(16) 2_655 2_655 ? C12 Fe1 C14 122.50(16) . 2_655 ? C11 Fe1 C14 108.85(15) . 2_655 ? C11 Fe1 C14 68.51(15) 2_655 2_655 ? C10 Fe1 C14 125.87(15) . 2_655 ? C10 Fe1 C14 40.16(15) 2_655 2_655 ? C14 Fe1 C14 161.2(2) . 2_655 ? C1 N1 C7 110.8(3) . . ? C1 N1 C10 122.8(3) . . ? C7 N1 C10 126.3(3) . . ? C1 N2 C2 110.6(3) . . ? C1 N2 C8 123.9(3) . . ? C2 N2 C8 125.1(3) . . ? N2 C1 N1 105.8(3) . . ? N2 C1 Ir1 128.1(3) . . ? N1 C1 Ir1 126.0(3) . . ? C3 C2 C7 122.2(4) . . ? C3 C2 N2 131.1(4) . . ? C7 C2 N2 106.7(3) . . ? C2 C3 C4 116.9(4) . . ? C2 C3 H3 121.5 . . ? C4 C3 H3 121.5 . . ? C3 C4 C5 121.3(4) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 116.6(4) . . ? C5 C6 H6 121.7 . . ? C7 C6 H6 121.7 . . ? C2 C7 N1 106.1(3) . . ? C2 C7 C6 121.4(3) . . ? N1 C7 C6 132.6(4) . . ? N2 C8 C9 113.9(4) . . ? N2 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N2 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C10 N1 125.9(3) . . ? C14 C10 C11 109.3(3) . . ? N1 C10 C11 124.5(3) . . ? C14 C10 Fe1 70.0(2) . . ? N1 C10 Fe1 132.8(3) . . ? C11 C10 Fe1 69.3(2) . . ? C12 C11 C10 107.3(3) . . ? C12 C11 Fe1 69.7(2) . . ? C10 C11 Fe1 70.2(2) . . ? C12 C11 H11 126.4 . . ? C10 C11 H11 126.4 . . ? Fe1 C11 H11 125.4 . . ? C11 C12 C13 108.3(3) . . ? C11 C12 Fe1 70.0(2) . . ? C13 C12 Fe1 69.5(2) . . ? C11 C12 H12 125.8 . . ? C13 C12 H12 125.8 . . ? Fe1 C12 H12 126.3 . . ? C12 C13 C14 108.3(3) . . ? C12 C13 Fe1 69.8(2) . . ? C14 C13 Fe1 70.5(2) . . ? C12 C13 H13 125.8 . . ? C14 C13 H13 125.8 . . ? Fe1 C13 H13 125.5 . . ? C10 C14 C13 106.8(3) . . ? C10 C14 Fe1 69.8(2) . . ? C13 C14 Fe1 68.8(3) . . ? C10 C14 H14 126.6 . . ? C13 C14 H14 126.6 . . ? Fe1 C14 H14 126.3 . . ? C2A C1A C8A 124.6(4) . . ? C2A C1A Ir1 71.4(2) . . ? C8A C1A Ir1 111.3(3) . . ? C2A C1A H1A 117.7 . . ? C8A C1A H1A 117.7 . . ? Ir1 C1A H1A 87.2 . . ? C1A C2A C3A 125.5(4) . . ? C1A C2A Ir1 71.5(2) . . ? C3A C2A Ir1 110.2(3) . . ? C1A C2A H2A 117.3 . . ? C3A C2A H2A 117.3 . . ? Ir1 C2A H2A 88.3 . . ? C4A C3A C2A 117.3(4) . . ? C4A C3A H3A1 108.0 . . ? C2A C3A H3A1 108.0 . . ? C4A C3A H3A2 108.0 . . ? C2A C3A H3A2 108.0 . . ? H3A1 C3A H3A2 107.2 . . ? C3A C4A C5A 114.7(4) . . ? C3A C4A H4A1 108.6 . . ? C5A C4A H4A1 108.6 . . ? C3A C4A H4A2 108.6 . . ? C5A C4A H4A2 108.6 . . ? H4A1 C4A H4A2 107.6 . . ? C6A C5A C4A 124.6(5) . . ? C6A C5A Ir1 70.2(3) . . ? C4A C5A Ir1 113.3(3) . . ? C6A C5A H5A 117.7 . . ? C4A C5A H5A 117.7 . . ? Ir1 C5A H5A 86.4 . . ? C5A C6A C7A 125.5(6) . . ? C5A C6A Ir1 71.3(3) . . ? C7A C6A Ir1 110.4(3) . . ? C5A C6A H6A 117.2 . . ? C7A C6A H6A 117.2 . . ? Ir1 C6A H6A 88.2 . . ? C8A C7A C6A 117.4(5) . . ? C8A C7A H7A1 108.0 . . ? C6A C7A H7A1 108.0 . . ? C8A C7A H7A2 108.0 . . ? C6A C7A H7A2 108.0 . . ? H7A1 C7A H7A2 107.2 . . ? C7A C8A C1A 114.6(4) . . ? C7A C8A H8A1 108.6 . . ? C1A C8A H8A1 108.6 . . ? C7A C8A H8A2 108.6 . . ? C1A C8A H8A2 108.6 . . ? H8A1 C8A H8A2 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N2 C1 N1 0.6(4) . . . . ? C8 N2 C1 N1 -172.9(3) . . . . ? C2 N2 C1 Ir1 -176.1(3) . . . . ? C8 N2 C1 Ir1 10.3(6) . . . . ? C7 N1 C1 N2 -0.7(4) . . . . ? C10 N1 C1 N2 177.7(3) . . . . ? C7 N1 C1 Ir1 176.1(3) . . . . ? C10 N1 C1 Ir1 -5.5(5) . . . . ? C6A Ir1 C1 N2 74.3(4) . . . . ? C5A Ir1 C1 N2 112.8(4) . . . . ? C2A Ir1 C1 N2 -179.0(3) . . . . ? C1A Ir1 C1 N2 11.4(9) . . . . ? Cl1 Ir1 C1 N2 -82.0(4) . . . . ? C6A Ir1 C1 N1 -101.8(4) . . . . ? C5A Ir1 C1 N1 -63.3(4) . . . . ? C2A Ir1 C1 N1 4.8(7) . . . . ? C1A Ir1 C1 N1 -164.7(5) . . . . ? Cl1 Ir1 C1 N1 101.8(3) . . . . ? C1 N2 C2 C3 -177.7(4) . . . . ? C8 N2 C2 C3 -4.3(7) . . . . ? C1 N2 C2 C7 -0.3(5) . . . . ? C8 N2 C2 C7 173.1(4) . . . . ? C7 C2 C3 C4 1.3(7) . . . . ? N2 C2 C3 C4 178.4(4) . . . . ? C2 C3 C4 C5 -0.8(7) . . . . ? C3 C4 C5 C6 -0.3(7) . . . . ? C4 C5 C6 C7 0.9(6) . . . . ? C3 C2 C7 N1 177.6(4) . . . . ? N2 C2 C7 N1 -0.1(4) . . . . ? C3 C2 C7 C6 -0.8(6) . . . . ? N2 C2 C7 C6 -178.4(4) . . . . ? C1 N1 C7 C2 0.5(4) . . . . ? C10 N1 C7 C2 -177.8(4) . . . . ? C1 N1 C7 C6 178.6(4) . . . . ? C10 N1 C7 C6 0.3(7) . . . . ? C5 C6 C7 C2 -0.3(6) . . . . ? C5 C6 C7 N1 -178.2(4) . . . . ? C1 N2 C8 C9 -112.6(5) . . . . ? C2 N2 C8 C9 74.7(5) . . . . ? C1 N1 C10 C14 139.5(4) . . . . ? C7 N1 C10 C14 -42.5(6) . . . . ? C1 N1 C10 C11 -32.2(6) . . . . ? C7 N1 C10 C11 145.8(4) . . . . ? C1 N1 C10 Fe1 -125.1(4) . . . . ? C7 N1 C10 Fe1 52.9(5) . . . . ? C13 Fe1 C10 C14 -152.8(4) 2_655 . . . ? C13 Fe1 C10 C14 -38.4(2) . . . . ? C12 Fe1 C10 C14 27.7(6) 2_655 . . . ? C12 Fe1 C10 C14 -82.6(2) . . . . ? C11 Fe1 C10 C14 -120.8(3) . . . . ? C11 Fe1 C10 C14 73.1(3) 2_655 . . . ? C10 Fe1 C10 C14 118.0(2) 2_655 . . . ? C14 Fe1 C10 C14 162.6(2) 2_655 . . . ? C13 Fe1 C10 N1 86.3(6) 2_655 . . . ? C13 Fe1 C10 N1 -159.3(4) . . . . ? C12 Fe1 C10 N1 -93.2(6) 2_655 . . . ? C12 Fe1 C10 N1 156.5(4) . . . . ? C11 Fe1 C10 N1 118.3(4) . . . . ? C11 Fe1 C10 N1 -47.7(4) 2_655 . . . ? C10 Fe1 C10 N1 -2.9(3) 2_655 . . . ? C14 Fe1 C10 N1 -120.9(4) . . . . ? C14 Fe1 C10 N1 41.8(4) 2_655 . . . ? C13 Fe1 C10 C11 -32.0(5) 2_655 . . . ? C13 Fe1 C10 C11 82.4(2) . . . . ? C12 Fe1 C10 C11 148.5(5) 2_655 . . . ? C12 Fe1 C10 C11 38.2(2) . . . . ? C11 Fe1 C10 C11 -166.0(2) 2_655 . . . ? C10 Fe1 C10 C11 -121.2(2) 2_655 . . . ? C14 Fe1 C10 C11 120.8(3) . . . . ? C14 Fe1 C10 C11 -76.5(3) 2_655 . . . ? C14 C10 C11 C12 -1.3(5) . . . . ? N1 C10 C11 C12 171.5(4) . . . . ? Fe1 C10 C11 C12 -60.1(3) . . . . ? C14 C10 C11 Fe1 58.8(3) . . . . ? N1 C10 C11 Fe1 -128.4(4) . . . . ? C13 Fe1 C11 C12 -75.1(3) 2_655 . . . ? C13 Fe1 C11 C12 37.6(2) . . . . ? C12 Fe1 C11 C12 -39.2(6) 2_655 . . . ? C11 Fe1 C11 C12 164.3(2) 2_655 . . . ? C10 Fe1 C11 C12 118.0(3) . . . . ? C10 Fe1 C11 C12 -159.1(2) 2_655 . . . ? C14 Fe1 C11 C12 81.5(3) . . . . ? C14 Fe1 C11 C12 -118.4(3) 2_655 . . . ? C13 Fe1 C11 C10 166.9(2) 2_655 . . . ? C13 Fe1 C11 C10 -80.4(2) . . . . ? C12 Fe1 C11 C10 -157.2(4) 2_655 . . . ? C12 Fe1 C11 C10 -118.0(3) . . . . ? C11 Fe1 C11 C10 46.3(2) 2_655 . . . ? C10 Fe1 C11 C10 82.9(3) 2_655 . . . ? C14 Fe1 C11 C10 -36.5(2) . . . . ? C14 Fe1 C11 C10 123.6(2) 2_655 . . . ? C10 C11 C12 C13 1.3(5) . . . . ? Fe1 C11 C12 C13 -59.1(3) . . . . ? C10 C11 C12 Fe1 60.4(3) . . . . ? C13 Fe1 C12 C11 120.6(2) 2_655 . . . ? C13 Fe1 C12 C11 -119.6(4) . . . . ? C12 Fe1 C12 C11 161.8(3) 2_655 . . . ? C11 Fe1 C12 C11 -170.7(2) 2_655 . . . ? C10 Fe1 C12 C11 -38.3(2) . . . . ? C10 Fe1 C12 C11 60.1(6) 2_655 . . . ? C14 Fe1 C12 C11 -81.8(3) . . . . ? C14 Fe1 C12 C11 80.9(3) 2_655 . . . ? C13 Fe1 C12 C13 -119.8(3) 2_655 . . . ? C12 Fe1 C12 C13 -78.6(2) 2_655 . . . ? C11 Fe1 C12 C13 119.6(4) . . . . ? C11 Fe1 C12 C13 -51.1(5) 2_655 . . . ? C10 Fe1 C12 C13 81.3(3) . . . . ? C10 Fe1 C12 C13 179.7(4) 2_655 . . . ? C14 Fe1 C12 C13 37.8(2) . . . . ? C14 Fe1 C12 C13 -159.5(2) 2_655 . . . ? C11 C12 C13 C14 -0.8(5) . . . . ? Fe1 C12 C13 C14 -60.2(3) . . . . ? C11 C12 C13 Fe1 59.4(3) . . . . ? C13 Fe1 C13 C12 76.0(2) 2_655 . . . ? C12 Fe1 C13 C12 116.6(3) 2_655 . . . ? C11 Fe1 C13 C12 -37.3(2) . . . . ? C11 Fe1 C13 C12 156.8(2) 2_655 . . . ? C10 Fe1 C13 C12 -81.2(3) . . . . ? C10 Fe1 C13 C12 -179.7(4) 2_655 . . . ? C14 Fe1 C13 C12 -119.1(3) . . . . ? C14 Fe1 C13 C12 50.0(5) 2_655 . . . ? C13 Fe1 C13 C14 -164.9(3) 2_655 . . . ? C12 Fe1 C13 C14 -124.3(2) 2_655 . . . ? C12 Fe1 C13 C14 119.1(3) . . . . ? C11 Fe1 C13 C14 81.8(2) . . . . ? C11 Fe1 C13 C14 -84.1(3) 2_655 . . . ? C10 Fe1 C13 C14 37.9(2) . . . . ? C10 Fe1 C13 C14 -60.7(5) 2_655 . . . ? C14 Fe1 C13 C14 169.0(2) 2_655 . . . ? N1 C10 C14 C13 -171.9(4) . . . . ? C11 C10 C14 C13 0.8(5) . . . . ? Fe1 C10 C14 C13 59.1(3) . . . . ? N1 C10 C14 Fe1 129.0(4) . . . . ? C11 C10 C14 Fe1 -58.3(3) . . . . ? C12 C13 C14 C10 0.0(5) . . . . ? Fe1 C13 C14 C10 -59.7(3) . . . . ? C12 C13 C14 Fe1 59.8(3) . . . . ? C13 Fe1 C14 C10 154.0(4) 2_655 . . . ? C13 Fe1 C14 C10 118.2(3) . . . . ? C12 Fe1 C14 C10 -169.7(2) 2_655 . . . ? C12 Fe1 C14 C10 80.4(2) . . . . ? C11 Fe1 C14 C10 36.8(2) . . . . ? C11 Fe1 C14 C10 -127.1(2) 2_655 . . . ? C10 Fe1 C14 C10 -85.3(3) 2_655 . . . ? C14 Fe1 C14 C10 -48.61(19) 2_655 . . . ? C13 Fe1 C14 C13 35.8(6) 2_655 . . . ? C12 Fe1 C14 C13 72.1(3) 2_655 . . . ? C12 Fe1 C14 C13 -37.8(2) . . . . ? C11 Fe1 C14 C13 -81.4(2) . . . . ? C11 Fe1 C14 C13 114.6(2) 2_655 . . . ? C10 Fe1 C14 C13 -118.2(3) . . . . ? C10 Fe1 C14 C13 156.5(2) 2_655 . . . ? C14 Fe1 C14 C13 -166.8(2) 2_655 . . . ? C1 Ir1 C1A C2A 173.5(5) . . . . ? C6A Ir1 C1A C2A 109.4(3) . . . . ? C5A Ir1 C1A C2A 72.2(3) . . . . ? Cl1 Ir1 C1A C2A -92.8(2) . . . . ? C1 Ir1 C1A C8A 52.7(8) . . . . ? C6A Ir1 C1A C8A -11.4(4) . . . . ? C5A Ir1 C1A C8A -48.6(4) . . . . ? C2A Ir1 C1A C8A -120.8(5) . . . . ? Cl1 Ir1 C1A C8A 146.4(3) . . . . ? C8A C1A C2A C3A 1.5(7) . . . . ? Ir1 C1A C2A C3A -102.0(4) . . . . ? C8A C1A C2A Ir1 103.6(4) . . . . ? C1 Ir1 C2A C1A -175.5(4) . . . . ? C6A Ir1 C2A C1A -69.4(3) . . . . ? C5A Ir1 C2A C1A -105.4(3) . . . . ? Cl1 Ir1 C2A C1A 87.4(2) . . . . ? C1 Ir1 C2A C3A -53.6(6) . . . . ? C6A Ir1 C2A C3A 52.5(4) . . . . ? C5A Ir1 C2A C3A 16.5(4) . . . . ? C1A Ir1 C2A C3A 121.9(5) . . . . ? Cl1 Ir1 C2A C3A -150.7(3) . . . . ? C1A C2A C3A C4A 60.4(7) . . . . ? Ir1 C2A C3A C4A -20.8(6) . . . . ? C2A C3A C4A C5A 12.7(9) . . . . ? C3A C4A C5A C6A -79.1(8) . . . . ? C3A C4A C5A Ir1 2.3(8) . . . . ? C1 Ir1 C5A C6A -91.1(3) . . . . ? C2A Ir1 C5A C6A 109.7(3) . . . . ? C1A Ir1 C5A C6A 74.1(3) . . . . ? Cl1 Ir1 C5A C6A 168.4(4) . . . . ? C1 Ir1 C5A C4A 148.8(4) . . . . ? C6A Ir1 C5A C4A -120.1(5) . . . . ? C2A Ir1 C5A C4A -10.4(4) . . . . ? C1A Ir1 C5A C4A -46.0(4) . . . . ? Cl1 Ir1 C5A C4A 48.3(7) . . . . ? C4A C5A C6A C7A 3.1(7) . . . . ? Ir1 C5A C6A C7A -102.2(5) . . . . ? C4A C5A C6A Ir1 105.3(4) . . . . ? C1 Ir1 C6A C5A 89.9(3) . . . . ? C2A Ir1 C6A C5A -68.9(3) . . . . ? C1A Ir1 C6A C5A -103.6(3) . . . . ? Cl1 Ir1 C6A C5A -172.6(2) . . . . ? C1 Ir1 C6A C7A -148.2(5) . . . . ? C5A Ir1 C6A C7A 121.9(6) . . . . ? C2A Ir1 C6A C7A 53.0(5) . . . . ? C1A Ir1 C6A C7A 18.2(5) . . . . ? Cl1 Ir1 C6A C7A -50.7(7) . . . . ? C5A C6A C7A C8A 57.5(9) . . . . ? Ir1 C6A C7A C8A -23.6(9) . . . . ? C6A C7A C8A C1A 14.4(10) . . . . ? C2A C1A C8A C7A -79.8(7) . . . . ? Ir1 C1A C8A C7A 1.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.733 _refine_diff_density_min -1.285 _refine_diff_density_rms 0.130