# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_shelxl _database_code_depnum_ccdc_archive 'CCDC 895358' #TrackingRef 'holm41_fertig_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H28 N6 Zn, 2(F6 P), C2 H3 N' _chemical_formula_sum 'C36 H31 F12 N7 P2 Zn' _chemical_formula_weight 916.99 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 15.4044(4) _cell_length_b 15.0872(2) _cell_length_c 17.6485(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.232(3) _cell_angle_gamma 90.00 _cell_volume 3710.33(15) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11321 _cell_measurement_theta_min 2.9435 _cell_measurement_theta_max 28.1828 _exptl_absorpt_correction_T_min 0.84795 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET) (compiled Mar 22 2010,13:57:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.848 _diffrn_ambient_temperature 113(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 ? _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 20450 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6506 _reflns_number_gt 5065 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6506 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 C1 C 0.07551(14) 0.60321(14) 0.40835(14) 0.0210(5) Uani 1 1 d . . . C1A C 0.4371(2) 0.60183(18) 0.0495(2) 0.0577(8) Uani 1 1 d . . . H1A1 H 0.4365 0.5922 -0.0056 0.087 Uiso 1 1 calc R . . H1A2 H 0.3723 0.5930 0.0457 0.087 Uiso 1 1 calc R . . H1A3 H 0.4813 0.5596 0.0898 0.087 Uiso 1 1 calc R . . C2 C 0.01466(14) 0.66944(15) 0.41401(15) 0.0284(5) Uani 1 1 d . . . H2 H 0.0373 0.7288 0.4250 0.034 Uiso 1 1 calc R . . C2A C 0.46885(19) 0.69253(19) 0.07755(17) 0.0433(7) Uani 1 1 d . . . C3 C -0.07705(15) 0.65061(16) 0.40404(15) 0.0319(6) Uani 1 1 d . . . H3 H -0.1174 0.6968 0.4070 0.038 Uiso 1 1 calc R . . C4 C -0.11000(15) 0.56456(15) 0.38983(15) 0.0279(5) Uani 1 1 d . . . H4 H -0.1737 0.5515 0.3817 0.033 Uiso 1 1 calc R . . C5 C -0.05073(14) 0.49763(15) 0.38747(13) 0.0235(5) Uani 1 1 d . . . H5 H -0.0731 0.4381 0.3795 0.028 Uiso 1 1 calc R . . C6 C 0.04187(14) 0.51620(14) 0.39659(13) 0.0201(5) Uani 1 1 d . . . C7 C 0.17145(14) 0.62923(13) 0.41295(14) 0.0204(5) Uani 1 1 d . . . C8 C 0.24356(15) 0.65655(13) 0.48955(15) 0.0250(5) Uani 1 1 d . . . H8 H 0.2301 0.6598 0.5373 0.030 Uiso 1 1 calc R . . C9 C 0.33443(15) 0.67899(14) 0.49741(15) 0.0280(5) Uani 1 1 d . . . H9 H 0.3829 0.6962 0.5503 0.034 Uiso 1 1 calc R . . C10 C 0.35400(14) 0.67623(13) 0.42820(15) 0.0258(5) Uani 1 1 d . . . H10 H 0.4162 0.6914 0.4334 0.031 Uiso 1 1 calc R . . C11 C 0.28330(14) 0.65140(12) 0.35105(15) 0.0216(5) Uani 1 1 d . . . H11 H 0.2968 0.6504 0.3033 0.026 Uiso 1 1 calc R . . C12 C 0.19208(13) 0.62778(12) 0.34322(14) 0.0195(5) Uani 1 1 d . . . C13 C 0.19678(13) 0.43140(13) 0.45098(14) 0.0204(5) Uani 1 1 d . . . H13A H 0.2007 0.3749 0.4808 0.025 Uiso 1 1 calc R . . H13B H 0.2136 0.4800 0.4925 0.025 Uiso 1 1 calc R . . C14 C 0.26835(14) 0.42976(12) 0.41319(14) 0.0184(5) Uani 1 1 d . . . C15 C 0.36675(14) 0.43164(13) 0.46268(15) 0.0231(5) Uani 1 1 d . . . H15 H 0.3917 0.4357 0.5219 0.028 Uiso 1 1 calc R . . C16 C 0.42724(15) 0.42747(14) 0.42343(15) 0.0260(5) Uani 1 1 d . . . H16 H 0.4948 0.4287 0.4560 0.031 Uiso 1 1 calc R . . C17 C 0.39076(14) 0.42162(13) 0.33761(15) 0.0240(5) Uani 1 1 d . . . H17 H 0.4324 0.4194 0.3105 0.029 Uiso 1 1 calc R . . C18 C 0.29218(14) 0.41906(12) 0.29155(14) 0.0188(5) Uani 1 1 d . . . C19 C 0.24249(14) 0.41150(13) 0.19923(14) 0.0196(5) Uani 1 1 d . . . C20 C 0.28943(15) 0.39278(14) 0.14926(15) 0.0262(5) Uani 1 1 d . . . H20 H 0.3568 0.3834 0.1733 0.031 Uiso 1 1 calc R . . C21 C 0.23575(17) 0.38813(14) 0.06379(16) 0.0310(6) Uani 1 1 d . . . H21 H 0.2664 0.3765 0.0281 0.037 Uiso 1 1 calc R . . C22 C 0.13804(16) 0.40029(14) 0.03003(15) 0.0288(5) Uani 1 1 d . . . H22 H 0.1006 0.3970 -0.0288 0.035 Uiso 1 1 calc R . . C23 C 0.09557(16) 0.41734(13) 0.08315(15) 0.0249(5) Uani 1 1 d . . . H23 H 0.0279 0.4249 0.0602 0.030 Uiso 1 1 calc R . . C24 C 0.03187(13) 0.65022(13) 0.22539(14) 0.0209(5) Uani 1 1 d . . . H24A H 0.0293 0.6818 0.1753 0.025 Uiso 1 1 calc R . . H24B H 0.0317 0.6953 0.2661 0.025 Uiso 1 1 calc R . . C25 C -0.05633(14) 0.59273(14) 0.20031(14) 0.0201(5) Uani 1 1 d . . . C26 C -0.14675(14) 0.62957(15) 0.17658(14) 0.0252(5) Uani 1 1 d . . . H26 H -0.1550 0.6920 0.1760 0.030 Uiso 1 1 calc R . . C27 C -0.22399(15) 0.57360(15) 0.15401(15) 0.0273(5) Uani 1 1 d . . . H27 H -0.2866 0.5973 0.1374 0.033 Uiso 1 1 calc R . . C28 C -0.21107(14) 0.48305(16) 0.15528(14) 0.0273(5) Uani 1 1 d . . . H28 H -0.2643 0.4440 0.1398 0.033 Uiso 1 1 calc R . . C29 C -0.11940(14) 0.45010(14) 0.17946(14) 0.0213(5) Uani 1 1 d . . . C30 C -0.09495(15) 0.35417(14) 0.18706(14) 0.0238(5) Uani 1 1 d . . . C31 C -0.16199(16) 0.28684(15) 0.16402(16) 0.0340(6) Uani 1 1 d . . . H31 H -0.2285 0.3002 0.1422 0.041 Uiso 1 1 calc R . . C32 C -0.13150(17) 0.20054(16) 0.17297(17) 0.0392(6) Uani 1 1 d . . . H32 H -0.1770 0.1537 0.1581 0.047 Uiso 1 1 calc R . . C33 C -0.03539(17) 0.18147(15) 0.20334(16) 0.0344(6) Uani 1 1 d . . . H33 H -0.0135 0.1219 0.2086 0.041 Uiso 1 1 calc R . . C34 C 0.02841(16) 0.25125(14) 0.22599(15) 0.0282(5) Uani 1 1 d . . . H34 H 0.0951 0.2387 0.2477 0.034 Uiso 1 1 calc R . . N1 N 0.09710(12) 0.44427(12) 0.38665(12) 0.0199(4) Uani 1 1 d . . . N1A N 0.49309(17) 0.76357(15) 0.09946(15) 0.0492(6) Uani 1 1 d . . . N2 N 0.23365(11) 0.42327(10) 0.33071(11) 0.0173(4) Uani 1 1 d . . . N3 N 0.14668(11) 0.42356(10) 0.16623(12) 0.0201(4) Uani 1 1 d . . . N4 N 0.12227(12) 0.59882(11) 0.26314(12) 0.0197(4) Uani 1 1 d . . . F1 F 0.10119(9) 0.72655(9) 0.00468(9) 0.0422(4) Uani 1 1 d . . . F2 F 0.26342(10) 0.72682(9) 0.06475(10) 0.0463(4) Uani 1 1 d . . . F3 F 0.18295(9) 0.73391(8) 0.14600(9) 0.0377(3) Uani 1 1 d . . . F4 F 0.18209(10) 0.60192(9) 0.00437(9) 0.0441(4) Uani 1 1 d . . . F5 F 0.10120(9) 0.61021(8) 0.08538(9) 0.0378(3) Uani 1 1 d . . . F6 F 0.26297(9) 0.60985(8) 0.14499(9) 0.0432(4) Uani 1 1 d . . . F7 F 0.64804(9) 0.51637(9) 0.23325(10) 0.0436(4) Uani 1 1 d . . . F8 F 0.71529(10) 0.38906(10) 0.29809(11) 0.0591(5) Uani 1 1 d . . . F9 F 0.62213(11) 0.46851(9) 0.34283(10) 0.0473(4) Uani 1 1 d . . . F10 F 0.56892(11) 0.33859(9) 0.27769(11) 0.0553(5) Uani 1 1 d . . . F11 F 0.50404(9) 0.46737(10) 0.21416(11) 0.0505(4) Uani 1 1 d . . . F12 F 0.59630(11) 0.38631(10) 0.16796(11) 0.0593(5) Uani 1 1 d . . . N5 N -0.04400(11) 0.50523(11) 0.20052(11) 0.0187(4) Uani 1 1 d . . . N6 N 0.00018(12) 0.33571(11) 0.21861(11) 0.0222(4) Uani 1 1 d . . . P1 P 0.18267(4) 0.66872(4) 0.07429(4) 0.02874(15) Uani 1 1 d . . . P2 P 0.60958(4) 0.42666(4) 0.25520(4) 0.02963(16) Uani 1 1 d . . . Zn01 Zn 0.090947(15) 0.448374(15) 0.255339(16) 0.01813(8) Uani 1 1 d . . . H1N1 H 0.0674(14) 0.3944(14) 0.3821(14) 0.023(6) Uiso 1 1 d . . . H1N4 H 0.1470(13) 0.5983(13) 0.2309(14) 0.013(6) Uiso 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 C1 0.0182(10) 0.0288(11) 0.0160(13) -0.0004(10) 0.0072(9) 0.0041(9) C1A 0.073(2) 0.0427(16) 0.053(2) -0.0010(15) 0.0221(17) 0.0125(15) C2 0.0284(12) 0.0316(12) 0.0229(14) -0.0063(11) 0.0086(11) 0.0050(10) C2A 0.0562(17) 0.0475(17) 0.0286(17) 0.0100(14) 0.0203(14) 0.0189(14) C3 0.0248(12) 0.0467(15) 0.0253(15) -0.0050(12) 0.0116(11) 0.0135(11) C4 0.0172(11) 0.0459(14) 0.0215(14) -0.0010(11) 0.0091(10) 0.0038(10) C5 0.0221(11) 0.0352(13) 0.0144(13) -0.0013(10) 0.0088(10) -0.0025(10) C6 0.0202(11) 0.0288(11) 0.0130(12) -0.0006(9) 0.0087(9) 0.0043(9) C7 0.0216(11) 0.0164(10) 0.0217(13) -0.0014(9) 0.0080(10) 0.0026(9) C8 0.0286(12) 0.0212(11) 0.0227(14) -0.0022(10) 0.0086(11) 0.0026(9) C9 0.0246(12) 0.0227(11) 0.0266(15) -0.0047(10) 0.0012(10) -0.0019(9) C10 0.0175(11) 0.0231(11) 0.0313(15) 0.0011(10) 0.0050(10) -0.0009(9) C11 0.0218(11) 0.0177(10) 0.0260(14) 0.0018(10) 0.0108(10) -0.0003(9) C12 0.0176(10) 0.0148(10) 0.0216(13) -0.0008(9) 0.0041(9) 0.0020(8) C13 0.0198(11) 0.0229(11) 0.0180(13) 0.0026(9) 0.0075(9) 0.0021(9) C14 0.0191(10) 0.0149(10) 0.0205(13) 0.0018(9) 0.0078(10) 0.0013(8) C15 0.0192(11) 0.0243(11) 0.0199(13) 0.0016(10) 0.0026(10) 0.0013(9) C16 0.0157(10) 0.0261(12) 0.0323(15) 0.0011(10) 0.0066(10) 0.0013(9) C17 0.0202(11) 0.0227(11) 0.0319(15) -0.0009(10) 0.0138(10) 0.0001(9) C18 0.0193(11) 0.0136(9) 0.0247(13) 0.0011(9) 0.0105(10) -0.0009(8) C19 0.0240(11) 0.0138(10) 0.0246(14) -0.0010(9) 0.0138(10) -0.0031(8) C20 0.0268(12) 0.0258(12) 0.0319(16) -0.0024(10) 0.0182(11) -0.0026(9) C21 0.0434(14) 0.0277(12) 0.0347(17) -0.0065(11) 0.0290(13) -0.0071(11) C22 0.0443(14) 0.0254(12) 0.0183(14) -0.0023(10) 0.0148(11) -0.0041(10) C23 0.0289(12) 0.0216(11) 0.0228(14) 0.0008(10) 0.0098(11) 0.0010(9) C24 0.0196(11) 0.0207(10) 0.0207(13) 0.0009(9) 0.0071(10) 0.0035(9) C25 0.0197(11) 0.0267(11) 0.0142(12) 0.0016(9) 0.0073(9) 0.0010(9) C26 0.0227(11) 0.0332(12) 0.0213(13) 0.0045(10) 0.0112(10) 0.0060(10) C27 0.0161(11) 0.0406(14) 0.0255(14) 0.0057(11) 0.0092(10) 0.0049(10) C28 0.0182(11) 0.0434(13) 0.0209(14) -0.0023(11) 0.0089(10) -0.0062(10) C29 0.0190(11) 0.0303(12) 0.0135(12) -0.0018(10) 0.0058(9) -0.0039(9) C30 0.0256(12) 0.0300(12) 0.0173(13) -0.0028(10) 0.0104(10) -0.0070(10) C31 0.0270(12) 0.0372(14) 0.0306(16) 0.0005(12) 0.0052(11) -0.0118(11) C32 0.0422(15) 0.0337(14) 0.0336(16) -0.0061(12) 0.0084(12) -0.0200(12) C33 0.0508(16) 0.0237(12) 0.0281(16) -0.0021(11) 0.0160(13) -0.0064(11) C34 0.0325(13) 0.0302(13) 0.0250(14) -0.0031(11) 0.0152(11) -0.0017(10) N1 0.0167(9) 0.0217(9) 0.0207(11) -0.0007(8) 0.0073(8) -0.0018(8) N1A 0.0745(17) 0.0419(14) 0.0405(16) 0.0068(12) 0.0334(14) 0.0106(12) N2 0.0170(8) 0.0167(9) 0.0190(11) 0.0003(7) 0.0084(8) 0.0013(7) N3 0.0220(9) 0.0179(9) 0.0209(11) -0.0004(8) 0.0098(8) -0.0002(7) N4 0.0174(9) 0.0240(9) 0.0195(11) -0.0003(8) 0.0098(9) 0.0013(7) F1 0.0507(8) 0.0354(8) 0.0335(9) 0.0080(7) 0.0112(7) 0.0044(6) F2 0.0497(9) 0.0348(8) 0.0642(12) 0.0027(8) 0.0337(8) -0.0064(7) F3 0.0537(9) 0.0254(7) 0.0341(9) -0.0059(6) 0.0189(7) -0.0034(6) F4 0.0746(10) 0.0321(8) 0.0351(9) -0.0034(7) 0.0325(8) -0.0025(7) F5 0.0525(8) 0.0314(7) 0.0328(9) -0.0038(6) 0.0213(7) -0.0129(6) F6 0.0516(9) 0.0313(8) 0.0387(10) 0.0055(7) 0.0115(7) 0.0075(6) F7 0.0468(8) 0.0346(7) 0.0657(12) 0.0036(8) 0.0395(8) -0.0049(6) F8 0.0432(9) 0.0644(11) 0.0755(13) 0.0149(9) 0.0308(9) 0.0223(8) F9 0.0606(9) 0.0451(9) 0.0434(10) -0.0012(7) 0.0291(8) 0.0033(7) F10 0.0779(11) 0.0283(8) 0.0841(14) 0.0023(8) 0.0580(10) -0.0095(7) F11 0.0292(7) 0.0639(10) 0.0626(12) 0.0184(9) 0.0236(8) 0.0039(7) F12 0.0740(11) 0.0616(11) 0.0558(12) -0.0232(9) 0.0407(9) -0.0290(9) N5 0.0161(8) 0.0247(9) 0.0141(10) 0.0006(8) 0.0052(7) -0.0020(7) N6 0.0253(10) 0.0238(10) 0.0184(11) -0.0019(8) 0.0103(8) -0.0032(8) P1 0.0410(4) 0.0206(3) 0.0259(4) 0.0010(3) 0.0154(3) -0.0023(3) P2 0.0280(3) 0.0278(3) 0.0399(4) 0.0028(3) 0.0210(3) -0.0013(2) Zn01 0.01515(13) 0.02078(13) 0.01812(15) -0.00141(11) 0.00679(10) 0.00011(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.394(3) . ? C1 C2 1.402(3) . ? C1 C7 1.498(3) . ? C1A C2A 1.466(4) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2 C3 1.377(3) . ? C2 H2 0.9500 . ? C2A N1A 1.147(3) . ? C3 C4 1.378(3) . ? C3 H3 0.9500 . ? C4 C5 1.374(3) . ? C4 H4 0.9500 . ? C5 C6 1.394(3) . ? C5 H5 0.9500 . ? C6 N1 1.435(3) . ? C7 C12 1.396(3) . ? C7 C8 1.397(3) . ? C8 C9 1.388(3) . ? C8 H8 0.9500 . ? C9 C10 1.378(3) . ? C9 H9 0.9500 . ? C10 C11 1.384(3) . ? C10 H10 0.9500 . ? C11 C12 1.398(3) . ? C11 H11 0.9500 . ? C12 N4 1.431(3) . ? C13 N1 1.483(3) . ? C13 C14 1.513(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N2 1.323(3) . ? C14 C15 1.390(3) . ? C15 C16 1.379(3) . ? C15 H15 0.9500 . ? C16 C17 1.375(3) . ? C16 H16 0.9500 . ? C17 C18 1.384(3) . ? C17 H17 0.9500 . ? C18 N2 1.351(3) . ? C18 C19 1.480(3) . ? C19 N3 1.348(3) . ? C19 C20 1.387(3) . ? C20 C21 1.379(3) . ? C20 H20 0.9500 . ? C21 C22 1.375(3) . ? C21 H21 0.9500 . ? C22 C23 1.377(3) . ? C22 H22 0.9500 . ? C23 N3 1.340(3) . ? C23 H23 0.9500 . ? C24 N4 1.481(3) . ? C24 C25 1.510(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N5 1.334(3) . ? C25 C26 1.388(3) . ? C26 C27 1.372(3) . ? C26 H26 0.9500 . ? C27 C28 1.379(3) . ? C27 H27 0.9500 . ? C28 C29 1.382(3) . ? C28 H28 0.9500 . ? C29 N5 1.346(2) . ? C29 C30 1.487(3) . ? C30 N6 1.356(3) . ? C30 C31 1.381(3) . ? C31 C32 1.370(3) . ? C31 H31 0.9500 . ? C32 C33 1.373(3) . ? C32 H32 0.9500 . ? C33 C34 1.378(3) . ? C33 H33 0.9500 . ? C34 N6 1.335(3) . ? C34 H34 0.9500 . ? N1 Zn01 2.2795(18) . ? N1 H1N1 0.87(2) . ? N2 Zn01 2.0621(16) . ? N3 Zn01 2.1217(18) . ? N4 Zn01 2.3123(17) . ? N4 H1N4 0.81(2) . ? F1 P1 1.5910(14) . ? F2 P1 1.5883(14) . ? F3 P1 1.6014(14) . ? F4 P1 1.5903(15) . ? F5 P1 1.6130(13) . ? F6 P1 1.6000(14) . ? F7 P2 1.5902(14) . ? F8 P2 1.5797(15) . ? F9 P2 1.6041(16) . ? F10 P2 1.5898(14) . ? F11 P2 1.5941(14) . ? F12 P2 1.5858(17) . ? N5 Zn01 2.0684(16) . ? N6 Zn01 2.1193(16) . ? 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 C6 C1 C2 117.66(18) . . ? C6 C1 C7 123.40(17) . . ? C2 C1 C7 118.92(19) . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C3 C2 C1 121.6(2) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? N1A C2A C1A 179.6(3) . . ? C2 C3 C4 119.7(2) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.01(19) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 120.24(18) . . ? C1 C6 N1 121.89(17) . . ? C5 C6 N1 117.69(19) . . ? C12 C7 C8 118.15(18) . . ? C12 C7 C1 122.56(19) . . ? C8 C7 C1 119.29(19) . . ? C9 C8 C7 121.4(2) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 119.8(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.16(19) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 120.4(2) . . ? C7 C12 N4 121.17(17) . . ? C11 C12 N4 118.4(2) . . ? N1 C13 C14 112.09(18) . . ? N1 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? N1 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N2 C14 C15 120.91(19) . . ? N2 C14 C13 117.24(17) . . ? C15 C14 C13 121.8(2) . . ? C16 C15 C14 118.2(2) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C17 C16 C15 120.6(2) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 118.7(2) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? N2 C18 C17 120.2(2) . . ? N2 C18 C19 114.96(17) . . ? C17 C18 C19 124.87(19) . . ? N3 C19 C20 121.6(2) . . ? N3 C19 C18 114.98(18) . . ? C20 C19 C18 123.41(19) . . ? C21 C20 C19 118.3(2) . . ? C21 C20 H20 120.9 . . ? C19 C20 H20 120.9 . . ? C22 C21 C20 120.2(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 118.7(2) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? N3 C23 C22 122.0(2) . . ? N3 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? N4 C24 C25 112.77(16) . . ? N4 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? N4 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? N5 C25 C26 121.37(18) . . ? N5 C25 C24 117.28(16) . . ? C26 C25 C24 121.34(18) . . ? C27 C26 C25 118.4(2) . . ? C27 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? C26 C27 C28 120.23(19) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C29 118.86(19) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? N5 C29 C28 120.73(19) . . ? N5 C29 C30 114.90(17) . . ? C28 C29 C30 124.35(18) . . ? N6 C30 C31 120.8(2) . . ? N6 C30 C29 115.13(17) . . ? C31 C30 C29 124.10(19) . . ? C32 C31 C30 119.2(2) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? C31 C32 C33 120.2(2) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C34 118.0(2) . . ? C32 C33 H33 121.0 . . ? C34 C33 H33 121.0 . . ? N6 C34 C33 122.6(2) . . ? N6 C34 H34 118.7 . . ? C33 C34 H34 118.7 . . ? C6 N1 C13 118.67(17) . . ? C6 N1 Zn01 109.50(13) . . ? C13 N1 Zn01 111.27(12) . . ? C6 N1 H1N1 110.6(13) . . ? C13 N1 H1N1 106.9(14) . . ? Zn01 N1 H1N1 97.9(15) . . ? C14 N2 C18 121.43(17) . . ? C14 N2 Zn01 121.04(13) . . ? C18 N2 Zn01 116.03(15) . . ? C23 N3 C19 119.20(19) . . ? C23 N3 Zn01 126.08(14) . . ? C19 N3 Zn01 114.71(14) . . ? C12 N4 C24 116.80(16) . . ? C12 N4 Zn01 114.10(13) . . ? C24 N4 Zn01 110.79(12) . . ? C12 N4 H1N4 108.5(15) . . ? C24 N4 H1N4 108.9(14) . . ? Zn01 N4 H1N4 95.6(14) . . ? C25 N5 C29 120.40(17) . . ? C25 N5 Zn01 121.70(13) . . ? C29 N5 Zn01 116.73(13) . . ? C34 N6 C30 119.09(18) . . ? C34 N6 Zn01 126.21(14) . . ? C30 N6 Zn01 114.67(13) . . ? F2 P1 F4 90.75(8) . . ? F2 P1 F1 90.64(8) . . ? F4 P1 F1 90.39(8) . . ? F2 P1 F6 90.52(8) . . ? F4 P1 F6 90.00(8) . . ? F1 P1 F6 178.78(8) . . ? F2 P1 F3 90.37(8) . . ? F4 P1 F3 178.56(8) . . ? F1 P1 F3 90.51(8) . . ? F6 P1 F3 89.08(8) . . ? F2 P1 F5 179.15(9) . . ? F4 P1 F5 90.01(7) . . ? F1 P1 F5 89.73(7) . . ? F6 P1 F5 89.11(8) . . ? F3 P1 F5 88.87(7) . . ? F8 P2 F12 90.42(9) . . ? F8 P2 F10 90.90(9) . . ? F12 P2 F10 91.15(9) . . ? F8 P2 F7 90.42(8) . . ? F12 P2 F7 89.85(8) . . ? F10 P2 F7 178.33(8) . . ? F8 P2 F11 178.02(10) . . ? F12 P2 F11 91.27(9) . . ? F10 P2 F11 90.08(8) . . ? F7 P2 F11 88.57(8) . . ? F8 P2 F9 90.20(9) . . ? F12 P2 F9 179.26(10) . . ? F10 P2 F9 89.24(9) . . ? F7 P2 F9 89.75(8) . . ? F11 P2 F9 88.10(9) . . ? N2 Zn01 N5 163.81(7) . . ? N2 Zn01 N6 115.65(6) . . ? N5 Zn01 N6 77.82(6) . . ? N2 Zn01 N3 77.81(7) . . ? N5 Zn01 N3 111.72(7) . . ? N6 Zn01 N3 93.12(6) . . ? N2 Zn01 N1 76.60(6) . . ? N5 Zn01 N1 94.86(6) . . ? N6 Zn01 N1 91.45(7) . . ? N3 Zn01 N1 153.40(6) . . ? N2 Zn01 N4 90.22(6) . . ? N5 Zn01 N4 76.31(6) . . ? N6 Zn01 N4 154.05(6) . . ? N3 Zn01 N4 94.43(6) . . ? N1 Zn01 N4 92.80(7) . . ? 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 C6 C1 C2 C3 -3.3(3) . . . . ? C7 C1 C2 C3 175.1(2) . . . . ? C1 C2 C3 C4 1.4(4) . . . . ? C2 C3 C4 C5 1.4(4) . . . . ? C3 C4 C5 C6 -2.1(3) . . . . ? C2 C1 C6 C5 2.6(3) . . . . ? C7 C1 C6 C5 -175.8(2) . . . . ? C2 C1 C6 N1 177.4(2) . . . . ? C7 C1 C6 N1 -1.0(3) . . . . ? C4 C5 C6 C1 0.1(3) . . . . ? C4 C5 C6 N1 -175.0(2) . . . . ? C6 C1 C7 C12 70.7(3) . . . . ? C2 C1 C7 C12 -107.7(2) . . . . ? C6 C1 C7 C8 -109.6(2) . . . . ? C2 C1 C7 C8 72.0(3) . . . . ? C12 C7 C8 C9 -2.1(3) . . . . ? C1 C7 C8 C9 178.22(18) . . . . ? C7 C8 C9 C10 1.4(3) . . . . ? C8 C9 C10 C11 0.2(3) . . . . ? C9 C10 C11 C12 -0.9(3) . . . . ? C8 C7 C12 C11 1.3(3) . . . . ? C1 C7 C12 C11 -179.01(18) . . . . ? C8 C7 C12 N4 178.72(17) . . . . ? C1 C7 C12 N4 -1.6(3) . . . . ? C10 C11 C12 C7 0.2(3) . . . . ? C10 C11 C12 N4 -177.32(18) . . . . ? N1 C13 C14 N2 -12.0(2) . . . . ? N1 C13 C14 C15 170.30(17) . . . . ? N2 C14 C15 C16 0.7(3) . . . . ? C13 C14 C15 C16 178.24(18) . . . . ? C14 C15 C16 C17 0.0(3) . . . . ? C15 C16 C17 C18 -0.7(3) . . . . ? C16 C17 C18 N2 0.7(3) . . . . ? C16 C17 C18 C19 -179.04(19) . . . . ? N2 C18 C19 N3 9.8(2) . . . . ? C17 C18 C19 N3 -170.45(18) . . . . ? N2 C18 C19 C20 -169.75(18) . . . . ? C17 C18 C19 C20 10.0(3) . . . . ? N3 C19 C20 C21 1.1(3) . . . . ? C18 C19 C20 C21 -179.42(19) . . . . ? C19 C20 C21 C22 -1.2(3) . . . . ? C20 C21 C22 C23 0.2(3) . . . . ? C21 C22 C23 N3 0.9(3) . . . . ? N4 C24 C25 N5 -11.7(3) . . . . ? N4 C24 C25 C26 169.42(19) . . . . ? N5 C25 C26 C27 0.8(3) . . . . ? C24 C25 C26 C27 179.6(2) . . . . ? C25 C26 C27 C28 0.1(3) . . . . ? C26 C27 C28 C29 -0.1(3) . . . . ? C27 C28 C29 N5 -0.8(3) . . . . ? C27 C28 C29 C30 177.3(2) . . . . ? N5 C29 C30 N6 3.6(3) . . . . ? C28 C29 C30 N6 -174.6(2) . . . . ? N5 C29 C30 C31 -176.1(2) . . . . ? C28 C29 C30 C31 5.8(4) . . . . ? N6 C30 C31 C32 -0.3(4) . . . . ? C29 C30 C31 C32 179.4(2) . . . . ? C30 C31 C32 C33 -1.0(4) . . . . ? C31 C32 C33 C34 1.5(4) . . . . ? C32 C33 C34 N6 -0.7(4) . . . . ? C1 C6 N1 C13 53.6(3) . . . . ? C5 C6 N1 C13 -131.4(2) . . . . ? C1 C6 N1 Zn01 -75.6(2) . . . . ? C5 C6 N1 Zn01 99.37(19) . . . . ? C14 C13 N1 C6 -125.09(19) . . . . ? C14 C13 N1 Zn01 3.3(2) . . . . ? C15 C14 N2 C18 -0.6(3) . . . . ? C13 C14 N2 C18 -178.30(16) . . . . ? C15 C14 N2 Zn01 -166.13(14) . . . . ? C13 C14 N2 Zn01 16.2(2) . . . . ? C17 C18 N2 C14 -0.1(3) . . . . ? C19 C18 N2 C14 179.70(17) . . . . ? C17 C18 N2 Zn01 166.12(14) . . . . ? C19 C18 N2 Zn01 -14.1(2) . . . . ? C22 C23 N3 C19 -1.0(3) . . . . ? C22 C23 N3 Zn01 -179.46(15) . . . . ? C20 C19 N3 C23 0.0(3) . . . . ? C18 C19 N3 C23 -179.55(17) . . . . ? C20 C19 N3 Zn01 178.61(15) . . . . ? C18 C19 N3 Zn01 -0.9(2) . . . . ? C7 C12 N4 C24 61.1(3) . . . . ? C11 C12 N4 C24 -121.4(2) . . . . ? C7 C12 N4 Zn01 -70.3(2) . . . . ? C11 C12 N4 Zn01 107.19(18) . . . . ? C25 C24 N4 C12 -126.84(19) . . . . ? C25 C24 N4 Zn01 6.1(2) . . . . ? C26 C25 N5 C29 -1.6(3) . . . . ? C24 C25 N5 C29 179.50(19) . . . . ? C26 C25 N5 Zn01 -168.83(16) . . . . ? C24 C25 N5 Zn01 12.3(3) . . . . ? C28 C29 N5 C25 1.6(3) . . . . ? C30 C29 N5 C25 -176.60(19) . . . . ? C28 C29 N5 Zn01 169.44(16) . . . . ? C30 C29 N5 Zn01 -8.8(2) . . . . ? C33 C34 N6 C30 -0.5(3) . . . . ? C33 C34 N6 Zn01 177.53(17) . . . . ? C31 C30 N6 C34 1.0(3) . . . . ? C29 C30 N6 C34 -178.66(19) . . . . ? C31 C30 N6 Zn01 -177.21(18) . . . . ? C29 C30 N6 Zn01 3.1(2) . . . . ? C14 N2 Zn01 N5 48.8(3) . . . . ? C18 N2 Zn01 N5 -117.4(2) . . . . ? C14 N2 Zn01 N6 -95.72(15) . . . . ? C18 N2 Zn01 N6 98.02(14) . . . . ? C14 N2 Zn01 N3 176.68(16) . . . . ? C18 N2 Zn01 N3 10.42(13) . . . . ? C14 N2 Zn01 N1 -10.63(14) . . . . ? C18 N2 Zn01 N1 -176.90(14) . . . . ? C14 N2 Zn01 N4 82.20(15) . . . . ? C18 N2 Zn01 N4 -84.07(14) . . . . ? C25 N5 Zn01 N2 28.0(3) . . . . ? C29 N5 Zn01 N2 -139.7(2) . . . . ? C25 N5 Zn01 N6 175.65(17) . . . . ? C29 N5 Zn01 N6 7.99(15) . . . . ? C25 N5 Zn01 N3 -95.83(16) . . . . ? C29 N5 Zn01 N3 96.51(15) . . . . ? C25 N5 Zn01 N1 85.22(16) . . . . ? C29 N5 Zn01 N1 -82.44(15) . . . . ? C25 N5 Zn01 N4 -6.49(15) . . . . ? C29 N5 Zn01 N4 -174.15(16) . . . . ? C34 N6 Zn01 N2 -13.4(2) . . . . ? C30 N6 Zn01 N2 164.68(14) . . . . ? C34 N6 Zn01 N5 176.09(19) . . . . ? C30 N6 Zn01 N5 -5.80(15) . . . . ? C34 N6 Zn01 N3 64.54(19) . . . . ? C30 N6 Zn01 N3 -117.36(15) . . . . ? C34 N6 Zn01 N1 -89.25(18) . . . . ? C30 N6 Zn01 N1 88.86(15) . . . . ? C34 N6 Zn01 N4 171.33(17) . . . . ? C30 N6 Zn01 N4 -10.6(3) . . . . ? C23 N3 Zn01 N2 173.69(17) . . . . ? C19 N3 Zn01 N2 -4.83(13) . . . . ? C23 N3 Zn01 N5 -20.02(18) . . . . ? C19 N3 Zn01 N5 161.46(13) . . . . ? C23 N3 Zn01 N6 58.11(17) . . . . ? C19 N3 Zn01 N6 -120.41(14) . . . . ? C23 N3 Zn01 N1 157.63(16) . . . . ? C19 N3 Zn01 N1 -20.9(2) . . . . ? C23 N3 Zn01 N4 -97.04(17) . . . . ? C19 N3 Zn01 N4 84.44(14) . . . . ? C6 N1 Zn01 N2 136.20(14) . . . . ? C13 N1 Zn01 N2 3.04(12) . . . . ? C6 N1 Zn01 N5 -29.85(14) . . . . ? C13 N1 Zn01 N5 -163.01(13) . . . . ? C6 N1 Zn01 N6 -107.75(13) . . . . ? C13 N1 Zn01 N6 119.09(13) . . . . ? C6 N1 Zn01 N3 152.34(14) . . . . ? C13 N1 Zn01 N3 19.2(2) . . . . ? C6 N1 Zn01 N4 46.64(13) . . . . ? C13 N1 Zn01 N4 -86.52(13) . . . . ? C12 N4 Zn01 N2 -37.11(14) . . . . ? C24 N4 Zn01 N2 -171.38(14) . . . . ? C12 N4 Zn01 N5 133.81(15) . . . . ? C24 N4 Zn01 N5 -0.46(14) . . . . ? C12 N4 Zn01 N6 138.60(16) . . . . ? C24 N4 Zn01 N6 4.3(2) . . . . ? C12 N4 Zn01 N3 -114.89(14) . . . . ? C24 N4 Zn01 N3 110.84(14) . . . . ? C12 N4 Zn01 N1 39.49(14) . . . . ? C24 N4 Zn01 N1 -94.78(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N1 N1A 0.87(2) 2.26(2) 3.117(3) 168(2) 2_545 N4 H1N4 F5 0.81(2) 2.36(2) 3.018(2) 138.8(18) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.439 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.050 data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 895359' #TrackingRef 'holm71_fertig.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H26 Fe N8, 2(Cl O4)' _chemical_formula_sum 'C30 H26 Cl2 Fe N8 O8' _chemical_formula_weight 753.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 20.6794(5) _cell_length_b 13.0498(2) _cell_length_c 23.5787(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.980(2) _cell_angle_gamma 90.00 _cell_volume 6117.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8154 _cell_measurement_theta_min 3.3334 _cell_measurement_theta_max 61.9999 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 6.148 _exptl_absorpt_correction_T_min 0.65644 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET) (compiled Mar 22 2010,13:57:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_detector_area_resol_mean 16.2879 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19707 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 62.09 _reflns_number_total 9577 _reflns_number_gt 6365 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9577 _refine_ls_number_parameters 887 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.912 _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 C1 C 0.92115(19) 0.0020(3) 0.60271(16) 0.0223(8) Uani 1 1 d . . . C2 C 0.8863(2) -0.0786(3) 0.56832(16) 0.0258(9) Uani 1 1 d . . . H2 H 0.9102 -0.1247 0.5504 0.031 Uiso 1 1 calc R . . C3 C 0.8180(2) -0.0930(3) 0.55969(17) 0.0295(9) Uani 1 1 d . . . H3 H 0.7955 -0.1482 0.5361 0.035 Uiso 1 1 calc R . . C4 C 0.7830(2) -0.0264(3) 0.58573(17) 0.0303(9) Uani 1 1 d . . . H4 H 0.7361 -0.0359 0.5801 0.036 Uiso 1 1 calc R . . C5 C 0.81562(19) 0.0542(3) 0.62003(16) 0.0267(9) Uani 1 1 d . . . H5 H 0.7911 0.0996 0.6378 0.032 Uiso 1 1 calc R . . C6 C 0.88437(18) 0.0688(3) 0.62855(15) 0.0206(8) Uani 1 1 d . . . C7 C 0.99540(18) 0.0084(3) 0.61287(15) 0.0211(8) Uani 1 1 d . . . C8 C 1.0342(2) -0.0769(3) 0.63773(16) 0.0281(9) Uani 1 1 d . . . H8 H 1.0122 -0.1382 0.6438 0.034 Uiso 1 1 calc R . . C9 C 1.1041(2) -0.0738(3) 0.65371(17) 0.0302(10) Uani 1 1 d . . . H9 H 1.1294 -0.1323 0.6707 0.036 Uiso 1 1 calc R . . C10 C 1.1364(2) 0.0151(3) 0.64479(17) 0.0304(9) Uani 1 1 d . . . H10 H 1.1841 0.0185 0.6571 0.037 Uiso 1 1 calc R . . C11 C 1.09968(18) 0.0988(3) 0.61808(16) 0.0256(9) Uani 1 1 d . . . H11 H 1.1223 0.1584 0.6105 0.031 Uiso 1 1 calc R . . C12 C 1.02958(19) 0.0965(3) 0.60208(16) 0.0227(9) Uani 1 1 d . . . C13 C 0.96887(19) 0.1257(3) 0.72020(16) 0.0250(9) Uani 1 1 d . . . H13A H 0.9476 0.1156 0.7526 0.030 Uiso 1 1 calc R . . H13B H 0.9902 0.0603 0.7139 0.030 Uiso 1 1 calc R . . C14 C 1.02145(19) 0.2076(3) 0.73707(16) 0.0241(9) Uani 1 1 d . . . C15 C 1.07072(19) 0.2140(3) 0.79046(17) 0.0279(9) Uani 1 1 d . . . H15 H 1.0719 0.1664 0.8212 0.033 Uiso 1 1 calc R . . C16 C 1.11849(19) 0.2921(3) 0.79786(17) 0.0292(9) Uani 1 1 d . . . H16 H 1.1531 0.2969 0.8339 0.035 Uiso 1 1 calc R . . C17 C 1.11619(19) 0.3618(3) 0.75400(17) 0.0291(9) Uani 1 1 d . . . H17 H 1.1489 0.4145 0.7586 0.035 Uiso 1 1 calc R . . C18 C 1.06449(19) 0.3525(3) 0.70274(16) 0.0245(9) Uani 1 1 d . . . C19 C 1.0815(2) 0.5082(3) 0.64418(18) 0.0283(9) Uani 1 1 d . . . H19 H 1.1215 0.5376 0.6687 0.034 Uiso 1 1 calc R . . C20 C 1.0427(2) 0.5475(3) 0.59294(18) 0.0310(10) Uani 1 1 d . . . H20 H 1.0497 0.6099 0.5747 0.037 Uiso 1 1 calc R . . C21 C 0.9899(2) 0.4773(3) 0.57222(17) 0.0268(9) Uani 1 1 d . . . H21 H 0.9550 0.4850 0.5366 0.032 Uiso 1 1 calc R . . C22 C 0.94695(18) 0.1659(3) 0.51382(15) 0.0227(8) Uani 1 1 d . . . H22A H 0.9344 0.0925 0.5104 0.027 Uiso 1 1 calc R . . H22B H 0.9706 0.1815 0.4836 0.027 Uiso 1 1 calc R . . C23 C 0.88447(18) 0.2302(3) 0.50283(16) 0.0202(8) Uani 1 1 d . . . C24 C 0.83701(19) 0.2414(3) 0.44922(16) 0.0254(9) Uani 1 1 d . . . H24 H 0.8431 0.2089 0.4150 0.030 Uiso 1 1 calc R . . C25 C 0.78018(19) 0.3005(3) 0.44577(18) 0.0284(9) Uani 1 1 d . . . H25 H 0.7467 0.3076 0.4092 0.034 Uiso 1 1 calc R . . C26 C 0.77255(19) 0.3490(3) 0.49568(17) 0.0271(9) Uani 1 1 d . . . H26 H 0.7342 0.3900 0.4942 0.033 Uiso 1 1 calc R . . C27 C 0.82229(19) 0.3360(3) 0.54753(16) 0.0236(8) Uani 1 1 d . . . C28 C 0.7822(2) 0.4470(3) 0.61873(18) 0.0290(9) Uani 1 1 d . . . H28 H 0.7393 0.4689 0.5953 0.035 Uiso 1 1 calc R . . C29 C 0.8120(2) 0.4747(3) 0.67508(18) 0.0311(10) Uani 1 1 d . . . H29 H 0.7946 0.5197 0.6990 0.037 Uiso 1 1 calc R . . C30 C 0.8739(2) 0.4230(3) 0.69092(17) 0.0269(9) Uani 1 1 d . . . H30 H 0.9058 0.4280 0.7285 0.032 Uiso 1 1 calc R . . C31 C 1.01110(19) 0.4955(3) 0.88810(16) 0.0229(8) Uani 1 1 d . . . C32 C 0.9820(2) 0.4015(3) 0.86619(16) 0.0283(9) Uani 1 1 d . . . H32 H 1.0105 0.3446 0.8654 0.034 Uiso 1 1 calc R . . C33 C 0.9132(2) 0.3891(3) 0.84578(17) 0.0319(10) Uani 1 1 d . . . H33 H 0.8948 0.3246 0.8310 0.038 Uiso 1 1 calc R . . C34 C 0.8714(2) 0.4708(3) 0.84694(17) 0.0330(10) Uani 1 1 d . . . H34 H 0.8242 0.4635 0.8312 0.040 Uiso 1 1 calc R . . C35 C 0.89825(19) 0.5642(3) 0.87121(16) 0.0271(9) Uani 1 1 d . . . H35 H 0.8692 0.6195 0.8734 0.033 Uiso 1 1 calc R . . C36 C 0.96752(19) 0.5764(3) 0.89224(16) 0.0231(9) Uani 1 1 d . . . C37 C 1.08612(18) 0.5038(3) 0.90420(16) 0.0223(8) Uani 1 1 d . . . C38 C 1.1239(2) 0.4328(3) 0.94387(17) 0.0286(9) Uani 1 1 d . . . H38 H 1.1015 0.3839 0.9616 0.034 Uiso 1 1 calc R . . C39 C 1.1940(2) 0.4322(3) 0.95803(18) 0.0336(10) Uani 1 1 d . . . H39 H 1.2191 0.3834 0.9852 0.040 Uiso 1 1 calc R . . C40 C 1.2264(2) 0.5030(3) 0.93234(17) 0.0338(10) Uani 1 1 d . . . H40 H 1.2741 0.5027 0.9418 0.041 Uiso 1 1 calc R . . C41 C 1.19028(19) 0.5742(3) 0.89297(17) 0.0283(9) Uani 1 1 d . . . H41 H 1.2133 0.6231 0.8759 0.034 Uiso 1 1 calc R . . C42 C 1.12041(18) 0.5746(3) 0.87820(16) 0.0217(8) Uani 1 1 d . . . C43 C 1.0401(2) 0.6058(3) 0.78102(16) 0.0268(9) Uani 1 1 d . . . H43A H 1.0215 0.5398 0.7901 0.032 Uiso 1 1 calc R . . H43B H 1.0666 0.5924 0.7526 0.032 Uiso 1 1 calc R . . C44 C 0.98345(19) 0.6781(3) 0.75392(16) 0.0232(8) Uani 1 1 d . . . C45 C 0.9419(2) 0.6722(3) 0.69721(17) 0.0282(9) Uani 1 1 d . . . H45 H 0.9490 0.6213 0.6707 0.034 Uiso 1 1 calc R . . C46 C 0.8895(2) 0.7421(3) 0.67943(18) 0.0316(10) Uani 1 1 d . . . H46 H 0.8603 0.7387 0.6406 0.038 Uiso 1 1 calc R . . C47 C 0.87970(19) 0.8163(3) 0.71778(17) 0.0286(9) Uani 1 1 d . . . H47 H 0.8440 0.8644 0.7063 0.034 Uiso 1 1 calc R . . C48 C 0.92389(18) 0.8176(3) 0.77355(16) 0.0239(8) Uani 1 1 d . . . C49 C 0.8836(2) 0.9715(3) 0.81992(19) 0.0326(10) Uani 1 1 d . . . H49 H 0.8454 0.9934 0.7897 0.039 Uiso 1 1 calc R . . C50 C 0.9092(2) 1.0168(3) 0.87280(18) 0.0344(10) Uani 1 1 d . . . H50 H 0.8928 1.0771 0.8868 0.041 Uiso 1 1 calc R . . C51 C 0.9647(2) 0.9575(3) 0.90312(18) 0.0303(9) Uani 1 1 d . . . H51 H 0.9921 0.9715 0.9418 0.036 Uiso 1 1 calc R . . C52 C 1.03832(18) 0.6640(3) 0.98000(16) 0.0238(8) Uani 1 1 d . . . H52A H 1.0120 0.6809 1.0080 0.029 Uiso 1 1 calc R . . H52B H 1.0541 0.5923 0.9874 0.029 Uiso 1 1 calc R . . C53 C 1.09782(18) 0.7341(3) 0.99042(16) 0.0215(8) Uani 1 1 d . . . C54 C 1.14550(19) 0.7471(3) 1.04357(16) 0.0253(9) Uani 1 1 d . . . H54 H 1.1417 0.7113 1.0776 0.030 Uiso 1 1 calc R . . C55 C 1.19927(19) 0.8130(3) 1.04709(17) 0.0266(9) Uani 1 1 d . . . H55 H 1.2323 0.8231 1.0836 0.032 Uiso 1 1 calc R . . C56 C 1.20434(19) 0.8639(3) 0.99706(16) 0.0245(9) Uani 1 1 d . . . H56 H 1.2410 0.9086 0.9982 0.029 Uiso 1 1 calc R . . C57 C 1.15436(18) 0.8475(3) 0.94535(15) 0.0212(8) Uani 1 1 d . . . C58 C 1.1939(2) 0.9560(3) 0.87220(17) 0.0276(9) Uani 1 1 d . . . H58 H 1.2354 0.9825 0.8957 0.033 Uiso 1 1 calc R . . C59 C 1.1652(2) 0.9757(3) 0.81431(17) 0.0308(9) Uani 1 1 d . . . H59 H 1.1823 1.0192 0.7895 0.037 Uiso 1 1 calc R . . C60 C 1.1054(2) 0.9188(3) 0.79842(17) 0.0265(9) Uani 1 1 d . . . H60 H 1.0749 0.9176 0.7600 0.032 Uiso 1 1 calc R . . N1 N 0.91582(15) 0.1547(2) 0.66458(13) 0.0222(7) Uani 1 1 d . . . H1 H 0.8820(14) 0.1816(12) 0.6780(6) 0.027 Uiso 1 1 calc R . . N2 N 1.01848(15) 0.2776(2) 0.69508(13) 0.0225(7) Uani 1 1 d . . . N3 N 1.05208(15) 0.4177(2) 0.65413(13) 0.0236(7) Uani 1 1 d . . . N4 N 0.99528(16) 0.3992(2) 0.60877(13) 0.0249(7) Uani 1 1 d . . . N5 N 0.99321(15) 0.1863(2) 0.57407(12) 0.0217(7) Uani 1 1 d . . . H5A H 1.0231(14) 0.2242(18) 0.5677(3) 0.026 Uiso 1 1 calc R . . N6 N 0.87736(14) 0.2787(2) 0.55099(12) 0.0189(7) Uani 1 1 d . . . N7 N 0.82480(15) 0.3819(2) 0.60147(13) 0.0239(7) Uani 1 1 d . . . N8 N 0.88222(16) 0.3668(2) 0.64710(13) 0.0240(7) Uani 1 1 d . . . N9 N 0.99402(16) 0.6735(2) 0.91785(13) 0.0229(7) Uani 1 1 d . . . H9A H 0.9596(16) 0.7065(16) 0.9212(2) 0.027 Uiso 1 1 calc R . . N10 N 1.10245(14) 0.7848(2) 0.94224(13) 0.0196(7) Uani 1 1 d . . . N11 N 1.09726(15) 0.8672(2) 0.84419(13) 0.0238(7) Uani 1 1 d . . . N12 N 1.15191(15) 0.8911(2) 0.89050(13) 0.0228(7) Uani 1 1 d . . . N13 N 1.08476(15) 0.6504(2) 0.83634(13) 0.0219(7) Uani 1 1 d . . . H13 H 1.1208(14) 0.6856(14) 0.8232(5) 0.026 Uiso 1 1 calc R . . N14 N 0.97426(15) 0.7511(2) 0.79106(13) 0.0220(7) Uani 1 1 d . . . N15 N 0.92297(16) 0.8881(2) 0.81806(14) 0.0260(7) Uani 1 1 d . . . N16 N 0.97330(16) 0.8800(2) 0.87044(13) 0.0250(7) Uani 1 1 d . . . Fe1 Fe 0.94717(3) 0.27627(4) 0.62351(2) 0.01993(15) Uani 1 1 d . . . Fe2 Fe 1.03690(3) 0.76781(4) 0.86763(2) 0.01992(15) Uani 1 1 d . . . Cl2 Cl 1.13130(5) 0.34195(7) 0.51060(4) 0.0277(2) Uani 1 1 d . . . O5 O 1.17636(14) 0.2673(2) 0.54503(12) 0.0395(7) Uani 1 1 d . . . O6 O 1.06335(14) 0.3202(2) 0.51288(14) 0.0422(8) Uani 1 1 d . . . O7 O 1.13353(14) 0.3377(2) 0.45072(11) 0.0354(7) Uani 1 1 d . . . O8 O 1.14975(14) 0.4427(2) 0.53348(13) 0.0388(7) Uani 1 1 d . . . Cl1 Cl 0.77275(5) 0.20915(7) 0.75192(4) 0.0289(2) Uani 1 1 d . . . O1 O 0.74748(19) 0.1095(3) 0.73287(16) 0.0689(11) Uani 1 1 d . . . O2 O 0.83941(14) 0.2159(2) 0.74445(12) 0.0372(7) Uani 1 1 d . . . O3 O 0.7307(2) 0.2810(3) 0.7155(2) 0.0961(16) Uani 1 1 d . . . O4 O 0.77500(16) 0.2207(3) 0.81143(13) 0.0576(10) Uani 1 1 d . . . Cl3 Cl 0.90796(5) 0.84518(7) 1.01823(4) 0.0295(2) Uani 1 1 d . . . O9 O 0.88326(14) 0.7743(2) 0.97089(12) 0.0358(7) Uani 1 1 d . . . O10 O 0.88697(15) 0.8139(2) 1.06833(12) 0.0376(7) Uani 1 1 d . . . O11 O 0.88176(14) 0.94605(19) 1.00007(13) 0.0389(7) Uani 1 1 d . . . O12 O 0.98021(14) 0.8470(2) 1.03246(14) 0.0480(8) Uani 1 1 d . . . Cl4 Cl 1.21696(5) 0.69047(7) 0.74637(4) 0.0296(2) Uani 1 1 d . . . O13 O 1.21655(16) 0.5804(2) 0.74761(15) 0.0514(9) Uani 1 1 d . . . O14 O 1.2675(2) 0.7263(3) 0.79536(15) 0.0774(13) Uani 1 1 d . . . O15 O 1.22823(16) 0.7264(3) 0.69348(14) 0.0595(10) Uani 1 1 d . . . O16 O 1.15281(18) 0.7256(2) 0.74944(17) 0.0634(11) 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 C1 0.027(2) 0.0210(19) 0.021(2) 0.0034(16) 0.0099(16) 0.0004(16) C2 0.035(2) 0.0210(19) 0.024(2) -0.0013(17) 0.0119(18) 0.0015(17) C3 0.032(2) 0.026(2) 0.029(2) -0.0054(18) 0.0063(18) -0.0061(18) C4 0.022(2) 0.034(2) 0.036(2) -0.003(2) 0.0086(18) -0.0066(18) C5 0.027(2) 0.028(2) 0.027(2) -0.0012(18) 0.0109(18) 0.0012(17) C6 0.024(2) 0.0197(18) 0.019(2) 0.0011(16) 0.0069(16) 0.0015(15) C7 0.024(2) 0.0213(19) 0.020(2) -0.0031(16) 0.0089(16) 0.0026(16) C8 0.041(3) 0.022(2) 0.023(2) 0.0008(17) 0.0125(19) 0.0034(18) C9 0.037(3) 0.031(2) 0.023(2) 0.0030(18) 0.0092(19) 0.0156(19) C10 0.023(2) 0.042(2) 0.026(2) 0.0018(19) 0.0064(17) 0.0054(19) C11 0.022(2) 0.028(2) 0.026(2) 0.0005(17) 0.0068(17) 0.0008(16) C12 0.027(2) 0.0232(19) 0.019(2) 0.0006(16) 0.0081(17) 0.0018(16) C13 0.032(2) 0.024(2) 0.021(2) 0.0051(17) 0.0102(18) 0.0030(17) C14 0.029(2) 0.0217(19) 0.022(2) -0.0020(17) 0.0086(17) 0.0068(16) C15 0.031(2) 0.029(2) 0.023(2) 0.0017(18) 0.0065(17) 0.0094(18) C16 0.025(2) 0.033(2) 0.025(2) -0.0089(19) -0.0009(17) 0.0069(18) C17 0.022(2) 0.032(2) 0.030(2) -0.0047(19) 0.0005(18) 0.0037(17) C18 0.024(2) 0.0242(19) 0.026(2) -0.0055(17) 0.0074(17) 0.0046(17) C19 0.031(2) 0.0195(19) 0.037(2) -0.0060(18) 0.0131(19) -0.0063(17) C20 0.039(2) 0.023(2) 0.035(2) 0.0022(19) 0.018(2) -0.0047(18) C21 0.033(2) 0.026(2) 0.023(2) 0.0001(18) 0.0109(18) 0.0016(17) C22 0.029(2) 0.0220(19) 0.0185(19) -0.0012(17) 0.0094(17) -0.0009(16) C23 0.024(2) 0.0158(18) 0.021(2) 0.0015(16) 0.0066(16) -0.0019(15) C24 0.031(2) 0.0237(19) 0.021(2) -0.0031(17) 0.0070(17) -0.0022(17) C25 0.026(2) 0.025(2) 0.030(2) 0.0012(18) 0.0012(17) 0.0013(17) C26 0.023(2) 0.0231(19) 0.033(2) 0.0022(18) 0.0050(18) 0.0040(16) C27 0.029(2) 0.0193(19) 0.025(2) 0.0007(17) 0.0114(17) -0.0006(16) C28 0.030(2) 0.026(2) 0.035(2) 0.0016(19) 0.0161(19) 0.0082(18) C29 0.043(3) 0.023(2) 0.036(3) -0.0024(19) 0.024(2) 0.0023(19) C30 0.037(2) 0.0209(19) 0.024(2) -0.0017(17) 0.0104(18) -0.0055(17) C31 0.029(2) 0.0198(19) 0.020(2) 0.0021(16) 0.0081(17) -0.0011(16) C32 0.041(3) 0.022(2) 0.025(2) -0.0011(17) 0.0152(19) -0.0033(18) C33 0.044(3) 0.027(2) 0.025(2) -0.0039(18) 0.011(2) -0.0137(19) C34 0.026(2) 0.043(2) 0.027(2) 0.004(2) 0.0012(18) -0.0128(19) C35 0.026(2) 0.030(2) 0.027(2) 0.0048(18) 0.0093(17) -0.0002(17) C36 0.029(2) 0.0208(19) 0.021(2) 0.0030(16) 0.0091(17) -0.0008(16) C37 0.026(2) 0.0199(19) 0.022(2) -0.0016(16) 0.0082(17) 0.0033(16) C38 0.038(3) 0.0209(19) 0.030(2) -0.0003(18) 0.0142(19) 0.0011(17) C39 0.037(3) 0.032(2) 0.033(2) 0.008(2) 0.011(2) 0.0137(19) C40 0.023(2) 0.046(3) 0.032(2) 0.003(2) 0.0066(19) 0.0079(19) C41 0.024(2) 0.033(2) 0.030(2) 0.0026(19) 0.0109(18) -0.0011(17) C42 0.026(2) 0.0199(18) 0.019(2) -0.0014(16) 0.0071(17) 0.0030(16) C43 0.034(2) 0.0225(19) 0.025(2) -0.0011(17) 0.0098(18) 0.0029(17) C44 0.027(2) 0.0208(19) 0.024(2) 0.0000(17) 0.0118(17) -0.0059(16) C45 0.034(2) 0.026(2) 0.024(2) -0.0030(18) 0.0078(18) -0.0082(18) C46 0.030(2) 0.038(2) 0.025(2) 0.0052(19) 0.0048(18) -0.0082(19) C47 0.024(2) 0.029(2) 0.031(2) 0.0100(19) 0.0058(18) -0.0005(17) C48 0.025(2) 0.0240(19) 0.027(2) 0.0006(17) 0.0131(17) -0.0028(16) C49 0.029(2) 0.025(2) 0.045(3) 0.006(2) 0.013(2) 0.0084(18) C50 0.044(3) 0.021(2) 0.042(3) -0.004(2) 0.018(2) 0.0062(19) C51 0.041(3) 0.022(2) 0.031(2) -0.0042(18) 0.015(2) -0.0034(18) C52 0.031(2) 0.0167(18) 0.027(2) -0.0010(17) 0.0123(17) -0.0011(16) C53 0.027(2) 0.0183(18) 0.022(2) 0.0008(16) 0.0113(17) 0.0049(16) C54 0.032(2) 0.0226(19) 0.022(2) 0.0039(17) 0.0100(17) 0.0058(17) C55 0.025(2) 0.027(2) 0.026(2) -0.0021(18) 0.0029(17) 0.0052(17) C56 0.025(2) 0.0225(19) 0.026(2) -0.0014(17) 0.0074(17) -0.0003(16) C57 0.027(2) 0.0163(18) 0.021(2) 0.0009(16) 0.0086(17) 0.0035(16) C58 0.028(2) 0.023(2) 0.035(2) 0.0005(18) 0.0145(19) -0.0040(17) C59 0.044(3) 0.023(2) 0.029(2) 0.0046(18) 0.017(2) -0.0007(18) C60 0.035(2) 0.025(2) 0.022(2) 0.0062(17) 0.0111(18) 0.0063(17) N1 0.0243(17) 0.0201(15) 0.0229(17) -0.0014(14) 0.0079(14) 0.0026(13) N2 0.0238(17) 0.0205(16) 0.0251(17) -0.0005(14) 0.0098(14) 0.0008(13) N3 0.0240(18) 0.0230(16) 0.0233(17) -0.0011(14) 0.0059(14) -0.0017(13) N4 0.0293(19) 0.0240(16) 0.0222(17) -0.0005(14) 0.0084(15) 0.0018(14) N5 0.0242(17) 0.0199(15) 0.0211(17) 0.0017(13) 0.0063(14) -0.0005(13) N6 0.0215(16) 0.0167(15) 0.0205(16) 0.0021(13) 0.0089(13) 0.0010(13) N7 0.0250(18) 0.0226(16) 0.0258(18) 0.0015(14) 0.0097(15) 0.0048(13) N8 0.0328(19) 0.0189(15) 0.0209(17) 0.0004(14) 0.0083(15) -0.0034(13) N9 0.0233(17) 0.0219(16) 0.0247(17) -0.0004(14) 0.0088(14) 0.0027(13) N10 0.0216(17) 0.0174(15) 0.0223(17) 0.0018(13) 0.0103(13) 0.0001(13) N11 0.0283(18) 0.0224(16) 0.0199(17) 0.0019(14) 0.0052(14) 0.0045(14) N12 0.0253(18) 0.0195(15) 0.0239(18) 0.0027(14) 0.0072(14) -0.0011(13) N13 0.0245(17) 0.0201(15) 0.0230(17) 0.0000(14) 0.0096(14) -0.0015(13) N14 0.0224(17) 0.0202(15) 0.0258(17) 0.0028(14) 0.0106(14) -0.0003(13) N15 0.0262(18) 0.0226(16) 0.0289(19) 0.0021(15) 0.0069(15) 0.0017(14) N16 0.0280(18) 0.0245(17) 0.0242(18) -0.0031(15) 0.0100(15) -0.0043(14) Fe1 0.0239(3) 0.0174(3) 0.0196(3) -0.0003(2) 0.0078(3) 0.0000(2) Fe2 0.0232(3) 0.0168(3) 0.0207(3) 0.0006(2) 0.0076(3) 0.0010(2) Cl2 0.0299(5) 0.0245(5) 0.0325(5) -0.0003(4) 0.0148(4) -0.0009(4) O5 0.0410(18) 0.0366(16) 0.0423(18) 0.0127(14) 0.0135(14) 0.0052(14) O6 0.0293(17) 0.0405(17) 0.061(2) 0.0078(15) 0.0196(15) -0.0014(13) O7 0.0379(17) 0.0422(17) 0.0277(15) 0.0011(13) 0.0117(13) 0.0030(13) O8 0.0359(17) 0.0272(14) 0.0527(19) -0.0109(14) 0.0110(14) -0.0010(13) Cl1 0.0284(5) 0.0286(5) 0.0317(5) 0.0039(4) 0.0116(4) -0.0028(4) O1 0.080(3) 0.072(2) 0.066(2) -0.023(2) 0.040(2) -0.048(2) O2 0.0329(16) 0.0444(17) 0.0403(17) -0.0147(14) 0.0199(13) -0.0071(13) O3 0.077(3) 0.111(3) 0.118(4) 0.086(3) 0.058(3) 0.049(3) O4 0.0400(19) 0.101(3) 0.0376(18) -0.0227(19) 0.0197(15) -0.0158(19) Cl3 0.0305(5) 0.0212(4) 0.0380(6) -0.0012(4) 0.0115(4) 0.0004(4) O9 0.0439(18) 0.0322(15) 0.0310(16) -0.0036(13) 0.0099(13) -0.0024(13) O10 0.0484(19) 0.0358(15) 0.0299(16) 0.0019(13) 0.0129(14) 0.0008(14) O11 0.0456(18) 0.0220(14) 0.0544(19) 0.0065(14) 0.0228(15) 0.0047(13) O12 0.0267(16) 0.0338(16) 0.083(2) -0.0117(17) 0.0132(16) 0.0015(13) Cl4 0.0337(5) 0.0303(5) 0.0267(5) -0.0009(4) 0.0114(4) -0.0002(4) O13 0.0474(19) 0.0266(15) 0.069(2) -0.0104(16) -0.0030(17) 0.0073(14) O14 0.111(3) 0.048(2) 0.050(2) 0.0029(18) -0.017(2) -0.030(2) O15 0.049(2) 0.099(3) 0.0369(18) 0.0227(19) 0.0221(16) 0.0161(19) O16 0.072(2) 0.0443(19) 0.100(3) 0.0296(19) 0.068(2) 0.0252(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.400(5) . ? C1 C6 1.402(5) . ? C1 C7 1.490(5) . ? C2 C3 1.382(6) . ? C2 H2 0.9500 . ? C3 C4 1.379(5) . ? C3 H3 0.9500 . ? C4 C5 1.383(5) . ? C4 H4 0.9500 . ? C5 C6 1.393(5) . ? C5 H5 0.9500 . ? C6 N1 1.448(4) . ? C7 C8 1.402(5) . ? C7 C12 1.409(5) . ? C8 C9 1.389(6) . ? C8 H8 0.9500 . ? C9 C10 1.383(6) . ? C9 H9 0.9500 . ? C10 C11 1.379(5) . ? C10 H10 0.9500 . ? C11 C12 1.394(5) . ? C11 H11 0.9500 . ? C12 N5 1.450(4) . ? C13 C14 1.498(5) . ? C13 N1 1.508(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N2 1.336(5) . ? C14 C15 1.387(5) . ? C15 C16 1.396(6) . ? C15 H15 0.9500 . ? C16 C17 1.368(5) . ? C16 H16 0.9500 . ? C17 C18 1.381(5) . ? C17 H17 0.9500 . ? C18 N2 1.341(5) . ? C18 N3 1.393(5) . ? C19 C20 1.354(6) . ? C19 N3 1.378(5) . ? C19 H19 0.9500 . ? C20 C21 1.407(5) . ? C20 H20 0.9500 . ? C21 N4 1.320(5) . ? C21 H21 0.9500 . ? C22 N5 1.502(4) . ? C22 C23 1.502(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N6 1.343(4) . ? C23 C24 1.378(5) . ? C24 C25 1.390(5) . ? C24 H24 0.9500 . ? C25 C26 1.383(5) . ? C25 H25 0.9500 . ? C26 C27 1.374(5) . ? C26 H26 0.9500 . ? C27 N6 1.346(5) . ? C27 N7 1.394(5) . ? C28 C29 1.351(5) . ? C28 N7 1.365(5) . ? C28 H28 0.9500 . ? C29 C30 1.404(6) . ? C29 H29 0.9500 . ? C30 N8 1.316(5) . ? C30 H30 0.9500 . ? C31 C32 1.402(5) . ? C31 C36 1.408(5) . ? C31 C37 1.496(5) . ? C32 C33 1.380(6) . ? C32 H32 0.9500 . ? C33 C34 1.377(6) . ? C33 H33 0.9500 . ? C34 C35 1.395(5) . ? C34 H34 0.9500 . ? C35 C36 1.390(5) . ? C35 H35 0.9500 . ? C36 N9 1.445(5) . ? C37 C38 1.393(5) . ? C37 C42 1.405(5) . ? C38 C39 1.395(6) . ? C38 H38 0.9500 . ? C39 C40 1.376(6) . ? C39 H39 0.9500 . ? C40 C41 1.379(5) . ? C40 H40 0.9500 . ? C41 C42 1.390(5) . ? C41 H41 0.9500 . ? C42 N13 1.448(4) . ? C43 N13 1.494(5) . ? C43 C44 1.503(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N14 1.342(5) . ? C44 C45 1.378(5) . ? C45 C46 1.390(5) . ? C45 H45 0.9500 . ? C46 C47 1.377(5) . ? C46 H46 0.9500 . ? C47 C48 1.379(5) . ? C47 H47 0.9500 . ? C48 N14 1.331(5) . ? C48 N15 1.400(5) . ? C49 C50 1.349(6) . ? C49 N15 1.368(5) . ? C49 H49 0.9500 . ? C50 C51 1.406(6) . ? C50 H50 0.9500 . ? C51 N16 1.313(5) . ? C51 H51 0.9500 . ? C52 C53 1.498(5) . ? C52 N9 1.504(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 N10 1.340(4) . ? C53 C54 1.375(5) . ? C54 C55 1.390(5) . ? C54 H54 0.9500 . ? C55 C56 1.383(5) . ? C55 H55 0.9500 . ? C56 C57 1.381(5) . ? C56 H56 0.9500 . ? C57 N10 1.336(5) . ? C57 N12 1.400(4) . ? C58 C59 1.354(5) . ? C58 N12 1.365(5) . ? C58 H58 0.9500 . ? C59 C60 1.402(6) . ? C59 H59 0.9500 . ? C60 N11 1.321(5) . ? C60 H60 0.9500 . ? N1 Fe1 2.054(3) . ? N1 H1 0.9124 . ? N2 Fe1 1.911(3) . ? N3 N4 1.375(4) . ? N4 Fe1 1.968(3) . ? N5 Fe1 2.063(3) . ? N5 H5A 0.8363 . ? N6 Fe1 1.911(3) . ? N7 N8 1.379(4) . ? N8 Fe1 1.980(3) . ? N9 Fe2 2.069(3) . ? N9 H9A 0.8547 . ? N10 Fe2 1.915(3) . ? N11 N12 1.374(4) . ? N11 Fe2 1.982(3) . ? N13 Fe2 2.067(3) . ? N13 H13 0.9942 . ? N14 Fe2 1.923(3) . ? N15 N16 1.383(4) . ? N16 Fe2 1.982(3) . ? Cl2 O7 1.426(3) . ? Cl2 O8 1.432(3) . ? Cl2 O5 1.435(3) . ? Cl2 O6 1.449(3) . ? Cl1 O4 1.399(3) . ? Cl1 O3 1.401(4) . ? Cl1 O1 1.427(3) . ? Cl1 O2 1.440(3) . ? Cl3 O10 1.426(3) . ? Cl3 O9 1.431(3) . ? Cl3 O12 1.439(3) . ? Cl3 O11 1.443(3) . ? Cl4 O14 1.407(3) . ? Cl4 O15 1.410(3) . ? Cl4 O16 1.424(3) . ? Cl4 O13 1.436(3) . ? 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 C2 C1 C6 117.7(3) . . ? C2 C1 C7 118.6(3) . . ? C6 C1 C7 123.6(3) . . ? C3 C2 C1 122.0(4) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C4 C3 C2 119.2(4) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 120.6(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 120.1(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.4(3) . . ? C5 C6 N1 117.8(3) . . ? C1 C6 N1 121.8(3) . . ? C8 C7 C12 117.7(3) . . ? C8 C7 C1 118.0(3) . . ? C12 C7 C1 124.2(3) . . ? C9 C8 C7 121.5(4) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119.5(4) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 120.3(3) . . ? C11 C12 N5 118.4(3) . . ? C7 C12 N5 121.3(3) . . ? C14 C13 N1 110.7(3) . . ? C14 C13 H13A 109.5 . . ? N1 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? N1 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N2 C14 C15 120.3(3) . . ? N2 C14 C13 114.2(3) . . ? C15 C14 C13 125.6(3) . . ? C14 C15 C16 118.3(4) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C17 C16 C15 121.0(4) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 117.4(4) . . ? C16 C17 H17 121.3 . . ? C18 C17 H17 121.3 . . ? N2 C18 C17 122.1(4) . . ? N2 C18 N3 111.8(3) . . ? C17 C18 N3 126.1(4) . . ? C20 C19 N3 107.2(3) . . ? C20 C19 H19 126.4 . . ? N3 C19 H19 126.4 . . ? C19 C20 C21 106.0(3) . . ? C19 C20 H20 127.0 . . ? C21 C20 H20 127.0 . . ? N4 C21 C20 111.0(3) . . ? N4 C21 H21 124.5 . . ? C20 C21 H21 124.5 . . ? N5 C22 C23 111.0(3) . . ? N5 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? N5 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? N6 C23 C24 120.7(3) . . ? N6 C23 C22 114.0(3) . . ? C24 C23 C22 125.4(3) . . ? C23 C24 C25 119.3(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 119.8(4) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C27 C26 C25 117.9(4) . . ? C27 C26 H26 121.1 . . ? C25 C26 H26 121.1 . . ? N6 C27 C26 122.4(3) . . ? N6 C27 N7 111.4(3) . . ? C26 C27 N7 126.1(3) . . ? C29 C28 N7 107.6(4) . . ? C29 C28 H28 126.2 . . ? N7 C28 H28 126.2 . . ? C28 C29 C30 105.6(3) . . ? C28 C29 H29 127.2 . . ? C30 C29 H29 127.2 . . ? N8 C30 C29 111.4(3) . . ? N8 C30 H30 124.3 . . ? C29 C30 H30 124.3 . . ? C32 C31 C36 117.6(3) . . ? C32 C31 C37 117.8(3) . . ? C36 C31 C37 124.6(3) . . ? C33 C32 C31 121.8(4) . . ? C33 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? C34 C33 C32 119.7(4) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.2(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.1(4) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C31 120.4(3) . . ? C35 C36 N9 119.0(3) . . ? C31 C36 N9 120.6(3) . . ? C38 C37 C42 118.3(3) . . ? C38 C37 C31 118.3(3) . . ? C42 C37 C31 123.3(3) . . ? C37 C38 C39 121.2(4) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C40 C39 C38 119.4(4) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C39 C40 C41 120.7(4) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C40 C41 C42 120.3(4) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C37 120.2(3) . . ? C41 C42 N13 118.2(3) . . ? C37 C42 N13 121.6(3) . . ? N13 C43 C44 110.4(3) . . ? N13 C43 H43A 109.6 . . ? C44 C43 H43A 109.6 . . ? N13 C43 H43B 109.6 . . ? C44 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? N14 C44 C45 120.7(3) . . ? N14 C44 C43 113.7(3) . . ? C45 C44 C43 125.6(3) . . ? C44 C45 C46 118.8(4) . . ? C44 C45 H45 120.6 . . ? C46 C45 H45 120.6 . . ? C47 C46 C45 120.5(4) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 117.1(4) . . ? C46 C47 H47 121.4 . . ? C48 C47 H47 121.4 . . ? N14 C48 C47 123.0(4) . . ? N14 C48 N15 111.5(3) . . ? C47 C48 N15 125.5(3) . . ? C50 C49 N15 107.0(4) . . ? C50 C49 H49 126.5 . . ? N15 C49 H49 126.5 . . ? C49 C50 C51 106.6(3) . . ? C49 C50 H50 126.7 . . ? C51 C50 H50 126.7 . . ? N16 C51 C50 110.5(4) . . ? N16 C51 H51 124.8 . . ? C50 C51 H51 124.8 . . ? C53 C52 N9 111.2(3) . . ? C53 C52 H52A 109.4 . . ? N9 C52 H52A 109.4 . . ? C53 C52 H52B 109.4 . . ? N9 C52 H52B 109.4 . . ? H52A C52 H52B 108.0 . . ? N10 C53 C54 120.7(3) . . ? N10 C53 C52 114.2(3) . . ? C54 C53 C52 125.1(3) . . ? C53 C54 C55 119.5(4) . . ? C53 C54 H54 120.3 . . ? C55 C54 H54 120.3 . . ? C56 C55 C54 119.6(4) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C57 C56 C55 117.7(4) . . ? C57 C56 H56 121.1 . . ? C55 C56 H56 121.1 . . ? N10 C57 C56 122.5(3) . . ? N10 C57 N12 111.9(3) . . ? C56 C57 N12 125.5(3) . . ? C59 C58 N12 107.2(3) . . ? C59 C58 H58 126.4 . . ? N12 C58 H58 126.4 . . ? C58 C59 C60 106.1(3) . . ? C58 C59 H59 126.9 . . ? C60 C59 H59 126.9 . . ? N11 C60 C59 110.6(3) . . ? N11 C60 H60 124.7 . . ? C59 C60 H60 124.7 . . ? C6 N1 C13 114.7(3) . . ? C6 N1 Fe1 118.0(2) . . ? C13 N1 Fe1 110.8(2) . . ? C6 N1 H1 103.8 . . ? C13 N1 H1 103.8 . . ? Fe1 N1 H1 103.8 . . ? C14 N2 C18 120.8(3) . . ? C14 N2 Fe1 121.0(2) . . ? C18 N2 Fe1 118.2(2) . . ? N4 N3 C19 109.9(3) . . ? N4 N3 C18 117.2(3) . . ? C19 N3 C18 132.3(3) . . ? C21 N4 N3 105.8(3) . . ? C21 N4 Fe1 142.1(3) . . ? N3 N4 Fe1 111.8(2) . . ? C12 N5 C22 113.8(3) . . ? C12 N5 Fe1 117.7(2) . . ? C22 N5 Fe1 111.3(2) . . ? C12 N5 H5A 104.1 . . ? C22 N5 H5A 104.1 . . ? Fe1 N5 H5A 104.1 . . ? C23 N6 C27 119.9(3) . . ? C23 N6 Fe1 121.2(2) . . ? C27 N6 Fe1 118.8(2) . . ? C28 N7 N8 110.1(3) . . ? C28 N7 C27 132.4(3) . . ? N8 N7 C27 117.3(3) . . ? C30 N8 N7 105.2(3) . . ? C30 N8 Fe1 143.0(3) . . ? N7 N8 Fe1 111.7(2) . . ? C36 N9 C52 113.2(3) . . ? C36 N9 Fe2 117.1(2) . . ? C52 N9 Fe2 111.4(2) . . ? C36 N9 H9A 104.6 . . ? C52 N9 H9A 104.6 . . ? Fe2 N9 H9A 104.6 . . ? C57 N10 C53 120.0(3) . . ? C57 N10 Fe2 118.4(2) . . ? C53 N10 Fe2 121.6(2) . . ? C60 N11 N12 105.8(3) . . ? C60 N11 Fe2 142.5(3) . . ? N12 N11 Fe2 111.7(2) . . ? C58 N12 N11 110.2(3) . . ? C58 N12 C57 132.8(3) . . ? N11 N12 C57 117.1(3) . . ? C42 N13 C43 113.9(3) . . ? C42 N13 Fe2 117.8(2) . . ? C43 N13 Fe2 111.0(2) . . ? C42 N13 H13 104.1 . . ? C43 N13 H13 104.1 . . ? Fe2 N13 H13 104.1 . . ? C48 N14 C44 120.0(3) . . ? C48 N14 Fe2 119.0(2) . . ? C44 N14 Fe2 120.9(2) . . ? C49 N15 N16 109.9(3) . . ? C49 N15 C48 132.7(3) . . ? N16 N15 C48 117.2(3) . . ? C51 N16 N15 106.0(3) . . ? C51 N16 Fe2 142.0(3) . . ? N15 N16 Fe2 111.7(2) . . ? N6 Fe1 N2 178.04(13) . . ? N6 Fe1 N4 97.04(12) . . ? N2 Fe1 N4 81.01(13) . . ? N6 Fe1 N8 80.66(12) . . ? N2 Fe1 N8 99.47(13) . . ? N4 Fe1 N8 88.75(12) . . ? N6 Fe1 N1 100.13(12) . . ? N2 Fe1 N1 81.83(12) . . ? N4 Fe1 N1 162.37(12) . . ? N8 Fe1 N1 90.11(12) . . ? N6 Fe1 N5 81.73(12) . . ? N2 Fe1 N5 98.07(12) . . ? N4 Fe1 N5 91.70(12) . . ? N8 Fe1 N5 162.31(12) . . ? N1 Fe1 N5 94.68(12) . . ? N10 Fe2 N14 177.46(13) . . ? N10 Fe2 N16 101.09(13) . . ? N14 Fe2 N16 80.41(13) . . ? N10 Fe2 N11 80.78(12) . . ? N14 Fe2 N11 97.21(12) . . ? N16 Fe2 N11 90.01(12) . . ? N10 Fe2 N13 97.24(12) . . ? N14 Fe2 N13 81.13(12) . . ? N16 Fe2 N13 161.27(12) . . ? N11 Fe2 N13 89.16(12) . . ? N10 Fe2 N9 81.35(12) . . ? N14 Fe2 N9 100.71(12) . . ? N16 Fe2 N9 91.59(12) . . ? N11 Fe2 N9 162.02(12) . . ? N13 Fe2 N9 94.94(12) . . ? O7 Cl2 O8 109.29(17) . . ? O7 Cl2 O5 109.94(17) . . ? O8 Cl2 O5 110.23(17) . . ? O7 Cl2 O6 108.96(17) . . ? O8 Cl2 O6 109.06(17) . . ? O5 Cl2 O6 109.34(17) . . ? O4 Cl1 O3 112.7(2) . . ? O4 Cl1 O1 108.8(2) . . ? O3 Cl1 O1 107.8(3) . . ? O4 Cl1 O2 110.33(18) . . ? O3 Cl1 O2 109.8(2) . . ? O1 Cl1 O2 107.30(19) . . ? O10 Cl3 O9 109.65(17) . . ? O10 Cl3 O12 110.18(19) . . ? O9 Cl3 O12 108.51(17) . . ? O10 Cl3 O11 109.40(17) . . ? O9 Cl3 O11 109.51(17) . . ? O12 Cl3 O11 109.57(17) . . ? O14 Cl4 O15 110.4(2) . . ? O14 Cl4 O16 110.1(3) . . ? O15 Cl4 O16 108.71(19) . . ? O14 Cl4 O13 108.8(2) . . ? O15 Cl4 O13 110.7(2) . . ? O16 Cl4 O13 108.1(2) . . ? 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 C6 C1 C2 C3 -0.1(5) . . . . ? C7 C1 C2 C3 176.3(4) . . . . ? C1 C2 C3 C4 -0.1(6) . . . . ? C2 C3 C4 C5 0.1(6) . . . . ? C3 C4 C5 C6 0.1(6) . . . . ? C4 C5 C6 C1 -0.3(5) . . . . ? C4 C5 C6 N1 179.6(3) . . . . ? C2 C1 C6 C5 0.3(5) . . . . ? C7 C1 C6 C5 -175.9(3) . . . . ? C2 C1 C6 N1 -179.7(3) . . . . ? C7 C1 C6 N1 4.2(5) . . . . ? C2 C1 C7 C8 -56.0(5) . . . . ? C6 C1 C7 C8 120.1(4) . . . . ? C2 C1 C7 C12 127.6(4) . . . . ? C6 C1 C7 C12 -56.3(5) . . . . ? C12 C7 C8 C9 2.8(5) . . . . ? C1 C7 C8 C9 -173.9(3) . . . . ? C7 C8 C9 C10 -0.3(6) . . . . ? C8 C9 C10 C11 -2.6(6) . . . . ? C9 C10 C11 C12 2.8(6) . . . . ? C10 C11 C12 C7 -0.2(6) . . . . ? C10 C11 C12 N5 -180.0(3) . . . . ? C8 C7 C12 C11 -2.5(5) . . . . ? C1 C7 C12 C11 173.9(3) . . . . ? C8 C7 C12 N5 177.2(3) . . . . ? C1 C7 C12 N5 -6.3(6) . . . . ? N1 C13 C14 N2 -12.2(4) . . . . ? N1 C13 C14 C15 168.5(3) . . . . ? N2 C14 C15 C16 -3.0(5) . . . . ? C13 C14 C15 C16 176.3(3) . . . . ? C14 C15 C16 C17 1.1(6) . . . . ? C15 C16 C17 C18 0.8(6) . . . . ? C16 C17 C18 N2 -1.0(6) . . . . ? C16 C17 C18 N3 177.5(3) . . . . ? N3 C19 C20 C21 -0.8(4) . . . . ? C19 C20 C21 N4 0.5(5) . . . . ? N5 C22 C23 N6 -10.4(4) . . . . ? N5 C22 C23 C24 169.7(3) . . . . ? N6 C23 C24 C25 -2.3(5) . . . . ? C22 C23 C24 C25 177.7(3) . . . . ? C23 C24 C25 C26 1.3(6) . . . . ? C24 C25 C26 C27 -0.3(6) . . . . ? C25 C26 C27 N6 0.3(6) . . . . ? C25 C26 C27 N7 177.1(3) . . . . ? N7 C28 C29 C30 -0.4(4) . . . . ? C28 C29 C30 N8 0.1(4) . . . . ? C36 C31 C32 C33 4.0(6) . . . . ? C37 C31 C32 C33 -174.7(3) . . . . ? C31 C32 C33 C34 -0.2(6) . . . . ? C32 C33 C34 C35 -3.1(6) . . . . ? C33 C34 C35 C36 2.5(6) . . . . ? C34 C35 C36 C31 1.3(6) . . . . ? C34 C35 C36 N9 -179.2(3) . . . . ? C32 C31 C36 C35 -4.5(5) . . . . ? C37 C31 C36 C35 174.1(3) . . . . ? C32 C31 C36 N9 176.1(3) . . . . ? C37 C31 C36 N9 -5.3(6) . . . . ? C32 C31 C37 C38 -54.7(5) . . . . ? C36 C31 C37 C38 126.8(4) . . . . ? C32 C31 C37 C42 120.6(4) . . . . ? C36 C31 C37 C42 -58.0(5) . . . . ? C42 C37 C38 C39 0.5(5) . . . . ? C31 C37 C38 C39 176.1(4) . . . . ? C37 C38 C39 C40 0.0(6) . . . . ? C38 C39 C40 C41 0.1(6) . . . . ? C39 C40 C41 C42 -0.7(6) . . . . ? C40 C41 C42 C37 1.3(6) . . . . ? C40 C41 C42 N13 -179.6(3) . . . . ? C38 C37 C42 C41 -1.2(5) . . . . ? C31 C37 C42 C41 -176.4(3) . . . . ? C38 C37 C42 N13 179.7(3) . . . . ? C31 C37 C42 N13 4.4(5) . . . . ? N13 C43 C44 N14 -16.7(4) . . . . ? N13 C43 C44 C45 165.1(3) . . . . ? N14 C44 C45 C46 -1.2(5) . . . . ? C43 C44 C45 C46 176.9(3) . . . . ? C44 C45 C46 C47 0.4(6) . . . . ? C45 C46 C47 C48 0.2(5) . . . . ? C46 C47 C48 N14 -0.1(6) . . . . ? C46 C47 C48 N15 178.6(3) . . . . ? N15 C49 C50 C51 -0.7(5) . . . . ? C49 C50 C51 N16 0.5(5) . . . . ? N9 C52 C53 N10 -4.6(4) . . . . ? N9 C52 C53 C54 176.4(3) . . . . ? N10 C53 C54 C55 -0.4(5) . . . . ? C52 C53 C54 C55 178.6(3) . . . . ? C53 C54 C55 C56 -0.5(5) . . . . ? C54 C55 C56 C57 0.9(5) . . . . ? C55 C56 C57 N10 -0.4(5) . . . . ? C55 C56 C57 N12 -178.9(3) . . . . ? N12 C58 C59 C60 -1.0(4) . . . . ? C58 C59 C60 N11 0.4(4) . . . . ? C5 C6 N1 C13 117.0(4) . . . . ? C1 C6 N1 C13 -63.1(4) . . . . ? C5 C6 N1 Fe1 -109.5(3) . . . . ? C1 C6 N1 Fe1 70.4(4) . . . . ? C14 C13 N1 C6 150.0(3) . . . . ? C14 C13 N1 Fe1 13.3(4) . . . . ? C15 C14 N2 C18 2.8(5) . . . . ? C13 C14 N2 C18 -176.5(3) . . . . ? C15 C14 N2 Fe1 -175.3(3) . . . . ? C13 C14 N2 Fe1 5.3(4) . . . . ? C17 C18 N2 C14 -0.8(5) . . . . ? N3 C18 N2 C14 -179.5(3) . . . . ? C17 C18 N2 Fe1 177.4(3) . . . . ? N3 C18 N2 Fe1 -1.3(4) . . . . ? C20 C19 N3 N4 0.8(4) . . . . ? C20 C19 N3 C18 -170.3(4) . . . . ? N2 C18 N3 N4 2.8(4) . . . . ? C17 C18 N3 N4 -175.8(3) . . . . ? N2 C18 N3 C19 173.4(4) . . . . ? C17 C18 N3 C19 -5.3(6) . . . . ? C20 C21 N4 N3 0.0(4) . . . . ? C20 C21 N4 Fe1 172.6(3) . . . . ? C19 N3 N4 C21 -0.5(4) . . . . ? C18 N3 N4 C21 172.1(3) . . . . ? C19 N3 N4 Fe1 -175.6(2) . . . . ? C18 N3 N4 Fe1 -3.0(4) . . . . ? C11 C12 N5 C22 120.8(4) . . . . ? C7 C12 N5 C22 -59.0(4) . . . . ? C11 C12 N5 Fe1 -106.5(3) . . . . ? C7 C12 N5 Fe1 73.8(4) . . . . ? C23 C22 N5 C12 145.0(3) . . . . ? C23 C22 N5 Fe1 9.2(3) . . . . ? C24 C23 N6 C27 2.3(5) . . . . ? C22 C23 N6 C27 -177.7(3) . . . . ? C24 C23 N6 Fe1 -173.1(3) . . . . ? C22 C23 N6 Fe1 7.0(4) . . . . ? C26 C27 N6 C23 -1.3(5) . . . . ? N7 C27 N6 C23 -178.6(3) . . . . ? C26 C27 N6 Fe1 174.2(3) . . . . ? N7 C27 N6 Fe1 -3.1(4) . . . . ? C29 C28 N7 N8 0.5(4) . . . . ? C29 C28 N7 C27 -174.9(4) . . . . ? N6 C27 N7 C28 178.4(3) . . . . ? C26 C27 N7 C28 1.2(6) . . . . ? N6 C27 N7 N8 3.3(4) . . . . ? C26 C27 N7 N8 -173.9(3) . . . . ? C29 C30 N8 N7 0.2(4) . . . . ? C29 C30 N8 Fe1 176.7(3) . . . . ? C28 N7 N8 C30 -0.4(4) . . . . ? C27 N7 N8 C30 175.7(3) . . . . ? C28 N7 N8 Fe1 -178.2(2) . . . . ? C27 N7 N8 Fe1 -2.0(4) . . . . ? C35 C36 N9 C52 123.1(4) . . . . ? C31 C36 N9 C52 -57.5(4) . . . . ? C35 C36 N9 Fe2 -105.3(3) . . . . ? C31 C36 N9 Fe2 74.1(4) . . . . ? C53 C52 N9 C36 140.5(3) . . . . ? C53 C52 N9 Fe2 6.1(4) . . . . ? C56 C57 N10 C53 -0.6(5) . . . . ? N12 C57 N10 C53 178.1(3) . . . . ? C56 C57 N10 Fe2 -179.4(3) . . . . ? N12 C57 N10 Fe2 -0.8(4) . . . . ? C54 C53 N10 C57 1.0(5) . . . . ? C52 C53 N10 C57 -178.1(3) . . . . ? C54 C53 N10 Fe2 179.8(3) . . . . ? C52 C53 N10 Fe2 0.7(4) . . . . ? C59 C60 N11 N12 0.4(4) . . . . ? C59 C60 N11 Fe2 -177.1(3) . . . . ? C59 C58 N12 N11 1.3(4) . . . . ? C59 C58 N12 C57 -178.0(4) . . . . ? C60 N11 N12 C58 -1.1(4) . . . . ? Fe2 N11 N12 C58 177.3(2) . . . . ? C60 N11 N12 C57 178.4(3) . . . . ? Fe2 N11 N12 C57 -3.2(4) . . . . ? N10 C57 N12 C58 -178.0(3) . . . . ? C56 C57 N12 C58 0.6(6) . . . . ? N10 C57 N12 N11 2.7(4) . . . . ? C56 C57 N12 N11 -178.7(3) . . . . ? C41 C42 N13 C43 117.8(4) . . . . ? C37 C42 N13 C43 -63.0(4) . . . . ? C41 C42 N13 Fe2 -109.5(3) . . . . ? C37 C42 N13 Fe2 69.7(4) . . . . ? C44 C43 N13 C42 153.8(3) . . . . ? C44 C43 N13 Fe2 17.9(4) . . . . ? C47 C48 N14 C44 -0.6(5) . . . . ? N15 C48 N14 C44 -179.4(3) . . . . ? C47 C48 N14 Fe2 174.9(3) . . . . ? N15 C48 N14 Fe2 -4.0(4) . . . . ? C45 C44 N14 C48 1.2(5) . . . . ? C43 C44 N14 C48 -177.1(3) . . . . ? C45 C44 N14 Fe2 -174.1(3) . . . . ? C43 C44 N14 Fe2 7.6(4) . . . . ? C50 C49 N15 N16 0.7(4) . . . . ? C50 C49 N15 C48 -174.5(4) . . . . ? N14 C48 N15 C49 176.6(4) . . . . ? C47 C48 N15 C49 -2.2(6) . . . . ? N14 C48 N15 N16 1.6(4) . . . . ? C47 C48 N15 N16 -177.2(3) . . . . ? C50 C51 N16 N15 -0.1(4) . . . . ? C50 C51 N16 Fe2 171.6(3) . . . . ? C49 N15 N16 C51 -0.4(4) . . . . ? C48 N15 N16 C51 175.7(3) . . . . ? C49 N15 N16 Fe2 -174.9(2) . . . . ? C48 N15 N16 Fe2 1.2(4) . . . . ? C23 N6 Fe1 N2 83(4) . . . . ? C27 N6 Fe1 N2 -92(4) . . . . ? C23 N6 Fe1 N4 89.5(3) . . . . ? C27 N6 Fe1 N4 -85.9(3) . . . . ? C23 N6 Fe1 N8 177.1(3) . . . . ? C27 N6 Fe1 N8 1.6(3) . . . . ? C23 N6 Fe1 N1 -94.5(3) . . . . ? C27 N6 Fe1 N1 90.1(3) . . . . ? C23 N6 Fe1 N5 -1.2(3) . . . . ? C27 N6 Fe1 N5 -176.6(3) . . . . ? C14 N2 Fe1 N6 -176(46) . . . . ? C18 N2 Fe1 N6 6(4) . . . . ? C14 N2 Fe1 N4 178.0(3) . . . . ? C18 N2 Fe1 N4 -0.2(3) . . . . ? C14 N2 Fe1 N8 90.8(3) . . . . ? C18 N2 Fe1 N8 -87.4(3) . . . . ? C14 N2 Fe1 N1 2.1(3) . . . . ? C18 N2 Fe1 N1 -176.2(3) . . . . ? C14 N2 Fe1 N5 -91.5(3) . . . . ? C18 N2 Fe1 N5 90.2(3) . . . . ? C21 N4 Fe1 N6 9.6(4) . . . . ? N3 N4 Fe1 N6 -178.1(2) . . . . ? C21 N4 Fe1 N2 -170.6(4) . . . . ? N3 N4 Fe1 N2 1.7(2) . . . . ? C21 N4 Fe1 N8 -70.8(4) . . . . ? N3 N4 Fe1 N8 101.5(2) . . . . ? C21 N4 Fe1 N1 -157.2(4) . . . . ? N3 N4 Fe1 N1 15.1(6) . . . . ? C21 N4 Fe1 N5 91.5(4) . . . . ? N3 N4 Fe1 N5 -96.2(2) . . . . ? C30 N8 Fe1 N6 -176.2(4) . . . . ? N7 N8 Fe1 N6 0.2(2) . . . . ? C30 N8 Fe1 N2 1.8(4) . . . . ? N7 N8 Fe1 N2 178.3(2) . . . . ? C30 N8 Fe1 N4 -78.8(4) . . . . ? N7 N8 Fe1 N4 97.6(2) . . . . ? C30 N8 Fe1 N1 83.6(4) . . . . ? N7 N8 Fe1 N1 -100.0(2) . . . . ? C30 N8 Fe1 N5 -170.5(4) . . . . ? N7 N8 Fe1 N5 5.9(5) . . . . ? C6 N1 Fe1 N6 36.1(3) . . . . ? C13 N1 Fe1 N6 171.3(2) . . . . ? C6 N1 Fe1 N2 -143.8(3) . . . . ? C13 N1 Fe1 N2 -8.7(2) . . . . ? C6 N1 Fe1 N4 -157.1(4) . . . . ? C13 N1 Fe1 N4 -22.0(6) . . . . ? C6 N1 Fe1 N8 116.7(3) . . . . ? C13 N1 Fe1 N8 -108.2(2) . . . . ? C6 N1 Fe1 N5 -46.3(3) . . . . ? C13 N1 Fe1 N5 88.8(2) . . . . ? C12 N5 Fe1 N6 -138.6(3) . . . . ? C22 N5 Fe1 N6 -4.8(2) . . . . ? C12 N5 Fe1 N2 43.4(3) . . . . ? C22 N5 Fe1 N2 177.2(2) . . . . ? C12 N5 Fe1 N4 124.5(3) . . . . ? C22 N5 Fe1 N4 -101.6(2) . . . . ? C12 N5 Fe1 N8 -144.3(4) . . . . ? C22 N5 Fe1 N8 -10.4(5) . . . . ? C12 N5 Fe1 N1 -39.0(3) . . . . ? C22 N5 Fe1 N1 94.8(2) . . . . ? C57 N10 Fe2 N14 37(3) . . . . ? C53 N10 Fe2 N14 -142(3) . . . . ? C57 N10 Fe2 N16 -88.9(3) . . . . ? C53 N10 Fe2 N16 92.2(3) . . . . ? C57 N10 Fe2 N11 -0.8(3) . . . . ? C53 N10 Fe2 N11 -179.6(3) . . . . ? C57 N10 Fe2 N13 87.2(3) . . . . ? C53 N10 Fe2 N13 -91.6(3) . . . . ? C57 N10 Fe2 N9 -178.9(3) . . . . ? C53 N10 Fe2 N9 2.3(3) . . . . ? C48 N14 Fe2 N10 -123(3) . . . . ? C44 N14 Fe2 N10 53(3) . . . . ? C48 N14 Fe2 N16 3.7(3) . . . . ? C44 N14 Fe2 N16 179.1(3) . . . . ? C48 N14 Fe2 N11 -85.1(3) . . . . ? C44 N14 Fe2 N11 90.3(3) . . . . ? C48 N14 Fe2 N13 -173.1(3) . . . . ? C44 N14 Fe2 N13 2.3(3) . . . . ? C48 N14 Fe2 N9 93.5(3) . . . . ? C44 N14 Fe2 N9 -91.1(3) . . . . ? C51 N16 Fe2 N10 4.0(4) . . . . ? N15 N16 Fe2 N10 175.4(2) . . . . ? C51 N16 Fe2 N14 -173.9(4) . . . . ? N15 N16 Fe2 N14 -2.5(2) . . . . ? C51 N16 Fe2 N11 -76.6(4) . . . . ? N15 N16 Fe2 N11 94.8(2) . . . . ? C51 N16 Fe2 N13 -164.0(4) . . . . ? N15 N16 Fe2 N13 7.4(5) . . . . ? C51 N16 Fe2 N9 85.5(4) . . . . ? N15 N16 Fe2 N9 -103.1(2) . . . . ? C60 N11 Fe2 N10 179.6(4) . . . . ? N12 N11 Fe2 N10 2.1(2) . . . . ? C60 N11 Fe2 N14 1.2(4) . . . . ? N12 N11 Fe2 N14 -176.3(2) . . . . ? C60 N11 Fe2 N16 -79.2(4) . . . . ? N12 N11 Fe2 N16 103.3(2) . . . . ? C60 N11 Fe2 N13 82.1(4) . . . . ? N12 N11 Fe2 N13 -95.4(2) . . . . ? C60 N11 Fe2 N9 -174.4(4) . . . . ? N12 N11 Fe2 N9 8.2(5) . . . . ? C42 N13 Fe2 N10 36.5(3) . . . . ? C43 N13 Fe2 N10 170.5(2) . . . . ? C42 N13 Fe2 N14 -145.5(3) . . . . ? C43 N13 Fe2 N14 -11.5(2) . . . . ? C42 N13 Fe2 N16 -155.3(3) . . . . ? C43 N13 Fe2 N16 -21.4(5) . . . . ? C42 N13 Fe2 N11 117.1(3) . . . . ? C43 N13 Fe2 N11 -108.9(2) . . . . ? C42 N13 Fe2 N9 -45.4(3) . . . . ? C43 N13 Fe2 N9 88.6(2) . . . . ? C36 N9 Fe2 N10 -137.1(3) . . . . ? C52 N9 Fe2 N10 -4.6(2) . . . . ? C36 N9 Fe2 N14 41.4(3) . . . . ? C52 N9 Fe2 N14 173.9(2) . . . . ? C36 N9 Fe2 N16 121.9(3) . . . . ? C52 N9 Fe2 N16 -105.6(2) . . . . ? C36 N9 Fe2 N11 -143.1(4) . . . . ? C52 N9 Fe2 N11 -10.6(5) . . . . ? C36 N9 Fe2 N13 -40.5(3) . . . . ? C52 N9 Fe2 N13 92.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 62.09 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.816 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.085 data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 895360' #TrackingRef 'holm71rt_fertig.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C30 H26 Fe N8)(Cl O4)(Cl O4)' _chemical_formula_sum 'C30 H26 Cl2 Fe N8 O8' _chemical_formula_weight 753.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 10.6583(5) _cell_length_b 13.0183(6) _cell_length_c 23.5210(14) _cell_angle_alpha 90.00 _cell_angle_beta 102.085(5) _cell_angle_gamma 90.00 _cell_volume 3191.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_oxdiff_measurement_reflns_used 3054 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 5.892 _exptl_absorpt_correction_T_min 0.74156 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET) (compiled Mar 22 2010,13:57:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _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 9664 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 62.71 _reflns_number_total 5030 _reflns_number_gt 3295 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1151P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5030 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1793 _refine_ls_wR_factor_gt 0.1708 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1514(5) 0.4837(4) 0.8976(2) 0.0552(12) Uani 1 1 d . . . C2 C 0.2132(5) 0.5583(4) 0.9349(3) 0.0705(15) Uani 1 1 d . . . H2 H 0.1642 0.6039 0.9516 0.085 Uiso 1 1 calc R . . C3 C 0.3441(6) 0.5677(5) 0.9481(3) 0.0865(18) Uani 1 1 d . . . H3 H 0.3830 0.6179 0.9740 0.104 Uiso 1 1 calc R . . C4 C 0.4176(6) 0.5019(5) 0.9225(3) 0.0883(19) Uani 1 1 d . . . H4 H 0.5066 0.5075 0.9312 0.106 Uiso 1 1 calc R . . C5 C 0.3592(5) 0.4283(4) 0.8843(3) 0.0689(15) Uani 1 1 d . . . H5 H 0.4091 0.3845 0.8669 0.083 Uiso 1 1 calc R . . C6 C 0.2274(5) 0.4183(4) 0.8712(2) 0.0539(12) Uani 1 1 d . . . C7 C 0.0077(4) 0.4795(4) 0.8834(2) 0.0538(12) Uani 1 1 d . . . C8 C -0.0581(5) 0.5638(4) 0.8547(2) 0.0680(14) Uani 1 1 d . . . H8 H -0.0117 0.6209 0.8471 0.082 Uiso 1 1 calc R . . C9 C -0.1881(6) 0.5644(5) 0.8376(3) 0.0784(17) Uani 1 1 d . . . H9 H -0.2296 0.6212 0.8182 0.094 Uiso 1 1 calc R . . C10 C -0.2580(5) 0.4814(6) 0.8488(3) 0.0811(18) Uani 1 1 d . . . H10 H -0.3466 0.4808 0.8360 0.097 Uiso 1 1 calc R . . C11 C -0.1966(5) 0.3985(5) 0.8793(3) 0.0708(15) Uani 1 1 d . . . H11 H -0.2443 0.3426 0.8874 0.085 Uiso 1 1 calc R . . C12 C -0.0642(4) 0.3981(4) 0.8979(2) 0.0545(12) Uani 1 1 d . . . C13 C 0.0883(5) 0.3759(4) 0.7764(2) 0.0639(13) Uani 1 1 d . . . H13A H 0.1401 0.3830 0.7473 0.077 Uiso 1 1 calc R . . H13B H 0.0554 0.4434 0.7830 0.077 Uiso 1 1 calc R . . C14 C -0.0218(5) 0.3060(4) 0.7536(2) 0.0523(12) Uani 1 1 d . . . C15 C -0.0988(6) 0.3173(4) 0.6993(2) 0.0668(14) Uani 1 1 d . . . H15 H -0.0814 0.3675 0.6739 0.080 Uiso 1 1 calc R . . C16 C -0.2030(6) 0.2521(5) 0.6834(3) 0.0799(17) Uani 1 1 d . . . H16 H -0.2570 0.2592 0.6470 0.096 Uiso 1 1 calc R . . C17 C -0.2271(5) 0.1775(5) 0.7204(2) 0.0673(15) Uani 1 1 d . . . H17 H -0.2964 0.1330 0.7100 0.081 Uiso 1 1 calc R . . C18 C -0.1445(4) 0.1709(4) 0.7738(2) 0.0527(12) Uani 1 1 d . . . C19 C -0.2497(5) 0.0266(5) 0.8159(3) 0.0739(16) Uani 1 1 d . . . H19 H -0.3255 0.0194 0.7882 0.089 Uiso 1 1 calc R . . C20 C -0.2122(6) -0.0314(5) 0.8636(3) 0.0848(19) Uani 1 1 d . . . H20 H -0.2556 -0.0870 0.8752 0.102 Uiso 1 1 calc R . . C21 C -0.0944(6) 0.0089(4) 0.8923(3) 0.0763(16) Uani 1 1 d . . . H21 H -0.0469 -0.0160 0.9273 0.092 Uiso 1 1 calc R . . C22 C 0.0800(5) 0.3313(4) 0.9868(2) 0.0621(13) Uani 1 1 d . . . H22A H 0.0356 0.3123 1.0173 0.075 Uiso 1 1 calc R . . H22B H 0.0979 0.4044 0.9903 0.075 Uiso 1 1 calc R . . C23 C 0.2044(5) 0.2736(4) 0.9954(2) 0.0582(13) Uani 1 1 d . . . C24 C 0.2965(6) 0.2791(5) 1.0456(2) 0.0736(16) Uani 1 1 d . . . H24 H 0.2827 0.3181 1.0768 0.088 Uiso 1 1 calc R . . C25 C 0.4097(6) 0.2259(5) 1.0493(3) 0.0825(18) Uani 1 1 d . . . H25 H 0.4732 0.2305 1.0829 0.099 Uiso 1 1 calc R . . C26 C 0.4300(5) 0.1669(5) 1.0044(3) 0.0721(15) Uani 1 1 d . . . H26 H 0.5057 0.1300 1.0068 0.087 Uiso 1 1 calc R . . C27 C 0.3327(5) 0.1638(4) 0.9546(2) 0.0533(12) Uani 1 1 d . . . C28 C 0.4354(6) 0.0485(4) 0.8932(3) 0.0760(17) Uani 1 1 d . . . H28 H 0.5163 0.0395 0.9167 0.091 Uiso 1 1 calc R . . C29 C 0.3927(6) 0.0050(5) 0.8406(3) 0.0797(17) Uani 1 1 d . . . H29 H 0.4363 -0.0406 0.8213 0.096 Uiso 1 1 calc R . . C30 C 0.2705(6) 0.0429(4) 0.8219(3) 0.0694(15) Uani 1 1 d . . . H30 H 0.2180 0.0270 0.7862 0.083 Uiso 1 1 calc R . . N1 N 0.1710(4) 0.3387(3) 0.83147(18) 0.0538(10) Uani 1 1 d . . . N2 N -0.0438(4) 0.2329(3) 0.79009(16) 0.0494(9) Uani 1 1 d . . . N3 N -0.1566(4) 0.0977(3) 0.81536(18) 0.0572(10) Uani 1 1 d . . . N4 N -0.0596(4) 0.0865(3) 0.86352(18) 0.0584(10) Uani 1 1 d . . . N5 N -0.0056(4) 0.3106(3) 0.92912(19) 0.0559(11) Uani 1 1 d . . . N6 N 0.2220(4) 0.2152(3) 0.95090(16) 0.0501(9) Uani 1 1 d . . . N7 N 0.3404(4) 0.1072(3) 0.90554(18) 0.0557(10) Uani 1 1 d . . . N8 N 0.2370(4) 0.1043(3) 0.86073(17) 0.0558(10) Uani 1 1 d . . . Fe1 Fe 0.08400(7) 0.20744(6) 0.87184(3) 0.0500(3) Uani 1 1 d . . . Cl2 Cl -0.20802(14) 0.13778(11) 1.00975(6) 0.0735(4) Uani 1 1 d . . . Cl1 Cl 0.45387(13) 0.26188(12) 0.74755(7) 0.0731(4) Uani 1 1 d . . . O6 O -0.0802(5) 0.1484(6) 1.0146(4) 0.184(4) Uani 1 1 d . . . O5 O -0.2479(8) 0.0388(4) 1.0001(3) 0.165(3) Uani 1 1 d . . . O8 O -0.2520(8) 0.1694(7) 1.0568(3) 0.176(3) Uani 1 1 d . . . O7 O -0.2615(7) 0.1989(5) 0.9616(3) 0.153(3) Uani 1 1 d . . . O3 O 0.5448(9) 0.2411(8) 0.7942(3) 0.204(4) Uani 1 1 d . . . O1 O 0.4662(7) 0.2075(14) 0.7052(5) 0.374(11) Uani 1 1 d . . . O2 O 0.4763(10) 0.3548(10) 0.7404(7) 0.348(10) Uani 1 1 d . . . O4 O 0.3294(5) 0.2512(4) 0.7569(3) 0.130(2) Uani 1 1 d . . . H1N1 H 0.229(5) 0.305(4) 0.825(2) 0.053(16) Uiso 1 1 d . . . H1N5 H -0.057(4) 0.269(4) 0.9315(19) 0.039(13) Uiso 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 C1 0.058(3) 0.050(3) 0.059(3) -0.003(2) 0.016(2) -0.001(2) C2 0.065(3) 0.056(3) 0.092(4) -0.011(3) 0.019(3) -0.007(3) C3 0.084(4) 0.077(4) 0.096(5) -0.025(4) 0.012(4) -0.023(3) C4 0.056(3) 0.100(5) 0.107(5) -0.011(4) 0.014(3) -0.018(3) C5 0.050(3) 0.073(4) 0.089(4) -0.008(3) 0.025(3) -0.004(3) C6 0.056(3) 0.049(3) 0.058(3) 0.002(2) 0.015(2) -0.005(2) C7 0.053(3) 0.049(3) 0.061(3) -0.002(2) 0.017(2) 0.003(2) C8 0.071(4) 0.059(3) 0.077(4) 0.008(3) 0.022(3) 0.006(3) C9 0.076(4) 0.082(4) 0.073(4) 0.005(3) 0.006(3) 0.024(3) C10 0.050(3) 0.102(5) 0.088(4) -0.005(4) 0.006(3) 0.015(3) C11 0.053(3) 0.076(4) 0.086(4) -0.013(3) 0.021(3) -0.007(3) C12 0.050(3) 0.056(3) 0.060(3) -0.003(2) 0.016(2) 0.006(2) C13 0.081(4) 0.057(3) 0.057(3) 0.011(3) 0.022(3) 0.000(3) C14 0.058(3) 0.052(3) 0.049(3) 0.002(2) 0.017(2) 0.011(2) C15 0.074(4) 0.074(4) 0.051(3) 0.013(3) 0.011(3) 0.018(3) C16 0.073(4) 0.105(5) 0.055(3) 0.006(3) -0.001(3) 0.021(4) C17 0.049(3) 0.086(4) 0.063(4) -0.013(3) 0.004(3) 0.005(3) C18 0.046(3) 0.056(3) 0.059(3) -0.001(2) 0.015(2) 0.004(2) C19 0.058(3) 0.078(4) 0.091(4) -0.014(4) 0.029(3) -0.023(3) C20 0.092(5) 0.062(4) 0.113(5) -0.007(4) 0.050(4) -0.023(3) C21 0.102(5) 0.062(3) 0.073(4) 0.011(3) 0.036(3) 0.004(3) C22 0.077(3) 0.061(3) 0.053(3) -0.003(2) 0.023(3) 0.002(3) C23 0.070(3) 0.053(3) 0.055(3) 0.004(2) 0.021(3) -0.010(2) C24 0.085(4) 0.083(4) 0.050(3) -0.014(3) 0.009(3) -0.017(3) C25 0.071(4) 0.104(5) 0.066(4) -0.007(4) -0.001(3) -0.019(4) C26 0.054(3) 0.081(4) 0.076(4) 0.008(3) 0.002(3) -0.007(3) C27 0.051(3) 0.051(3) 0.056(3) 0.011(2) 0.010(2) -0.005(2) C28 0.065(3) 0.067(4) 0.102(5) 0.010(3) 0.031(3) 0.015(3) C29 0.090(4) 0.063(4) 0.097(5) -0.001(3) 0.043(4) 0.009(3) C30 0.090(4) 0.058(3) 0.066(4) -0.003(3) 0.029(3) -0.001(3) N1 0.056(3) 0.049(2) 0.060(3) 0.002(2) 0.019(2) 0.000(2) N2 0.054(2) 0.050(2) 0.046(2) 0.0040(18) 0.0144(18) 0.0042(18) N3 0.053(2) 0.055(2) 0.064(3) -0.006(2) 0.014(2) -0.0039(19) N4 0.062(3) 0.055(2) 0.060(3) 0.008(2) 0.018(2) -0.002(2) N5 0.056(3) 0.050(3) 0.066(3) 0.002(2) 0.023(2) -0.007(2) N6 0.057(2) 0.049(2) 0.046(2) 0.0053(18) 0.0135(18) -0.0009(18) N7 0.058(2) 0.052(2) 0.059(3) 0.002(2) 0.015(2) 0.0045(19) N8 0.066(3) 0.052(2) 0.052(2) -0.0013(19) 0.018(2) 0.000(2) Fe1 0.0531(4) 0.0514(5) 0.0449(4) 0.0018(3) 0.0087(3) 0.0002(3) Cl2 0.0760(9) 0.0699(9) 0.0783(10) 0.0004(7) 0.0245(7) -0.0053(7) Cl1 0.0633(8) 0.0816(10) 0.0779(10) 0.0131(8) 0.0226(7) -0.0053(7) O6 0.082(4) 0.178(6) 0.282(9) 0.112(7) 0.014(4) -0.016(4) O5 0.274(8) 0.084(4) 0.169(6) -0.017(4) 0.119(6) -0.060(5) O8 0.223(8) 0.209(7) 0.104(5) -0.060(5) 0.051(5) 0.007(6) O7 0.166(6) 0.161(6) 0.127(5) 0.064(4) 0.021(4) 0.007(5) O3 0.178(8) 0.282(11) 0.136(6) 0.035(7) -0.005(5) 0.054(7) O1 0.086(4) 0.75(3) 0.312(12) -0.394(17) 0.096(6) -0.114(9) O2 0.192(9) 0.316(14) 0.53(2) 0.302(16) 0.049(11) -0.060(9) O4 0.111(4) 0.127(4) 0.179(5) -0.060(4) 0.091(4) -0.033(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 C1 C2 1.380(7) . ? C1 C6 1.406(7) . ? C1 C7 1.499(7) . ? C2 C3 1.370(8) . ? C3 C4 1.382(9) . ? C4 C5 1.371(8) . ? C5 C6 1.380(7) . ? C6 N1 1.440(6) . ? C7 C12 1.390(7) . ? C7 C8 1.399(7) . ? C8 C9 1.360(8) . ? C9 C10 1.369(9) . ? C10 C11 1.382(8) . ? C11 C12 1.387(7) . ? C12 N5 1.427(6) . ? C13 N1 1.487(7) . ? C13 C14 1.494(7) . ? C14 N2 1.334(6) . ? C14 C15 1.374(7) . ? C15 C16 1.386(9) . ? C16 C17 1.365(9) . ? C17 C18 1.377(7) . ? C18 N2 1.334(6) . ? C18 N3 1.391(6) . ? C19 C20 1.342(9) . ? C19 N3 1.359(6) . ? C20 C21 1.397(9) . ? C21 N4 1.312(7) . ? C22 N5 1.492(7) . ? C22 C23 1.501(7) . ? C23 N6 1.338(6) . ? C23 C24 1.371(8) . ? C24 C25 1.378(9) . ? C25 C26 1.359(9) . ? C26 C27 1.393(7) . ? C27 N6 1.343(6) . ? C27 N7 1.387(6) . ? C28 N7 1.347(7) . ? C28 C29 1.348(9) . ? C29 C30 1.375(8) . ? C30 N8 1.317(6) . ? N1 Fe1 2.247(4) . ? N2 Fe1 2.137(4) . ? N3 N4 1.372(6) . ? N4 Fe1 2.176(4) . ? N5 Fe1 2.252(4) . ? N6 Fe1 2.118(4) . ? N7 N8 1.357(6) . ? N8 Fe1 2.170(4) . ? Cl2 O6 1.350(6) . ? Cl2 O8 1.353(6) . ? Cl2 O5 1.361(6) . ? Cl2 O7 1.403(6) . ? Cl1 O2 1.251(11) . ? Cl1 O1 1.251(7) . ? Cl1 O3 1.331(8) . ? Cl1 O4 1.396(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.7(5) . . ? C2 C1 C7 119.8(4) . . ? C6 C1 C7 122.4(4) . . ? C3 C2 C1 122.3(5) . . ? C2 C3 C4 119.3(6) . . ? C5 C4 C3 119.9(6) . . ? C4 C5 C6 120.9(5) . . ? C5 C6 C1 119.9(5) . . ? C5 C6 N1 118.7(5) . . ? C1 C6 N1 121.4(4) . . ? C12 C7 C8 118.0(4) . . ? C12 C7 C1 124.3(4) . . ? C8 C7 C1 117.7(4) . . ? C9 C8 C7 121.6(5) . . ? C8 C9 C10 120.0(6) . . ? C9 C10 C11 119.9(5) . . ? C10 C11 C12 120.4(5) . . ? C11 C12 C7 119.8(5) . . ? C11 C12 N5 118.2(5) . . ? C7 C12 N5 122.0(4) . . ? N1 C13 C14 113.0(4) . . ? N2 C14 C15 121.5(5) . . ? N2 C14 C13 115.8(4) . . ? C15 C14 C13 122.7(5) . . ? C14 C15 C16 118.3(5) . . ? C17 C16 C15 120.7(5) . . ? C16 C17 C18 117.1(5) . . ? N2 C18 C17 123.2(5) . . ? N2 C18 N3 113.5(4) . . ? C17 C18 N3 123.2(5) . . ? C20 C19 N3 107.5(5) . . ? C19 C20 C21 105.8(5) . . ? N4 C21 C20 111.3(6) . . ? N5 C22 C23 112.7(4) . . ? N6 C23 C24 120.8(5) . . ? N6 C23 C22 116.4(5) . . ? C24 C23 C22 122.9(5) . . ? C23 C24 C25 119.1(5) . . ? C26 C25 C24 121.0(6) . . ? C25 C26 C27 117.2(6) . . ? N6 C27 N7 114.5(4) . . ? N6 C27 C26 122.0(5) . . ? N7 C27 C26 123.4(5) . . ? N7 C28 C29 108.1(6) . . ? C28 C29 C30 105.0(5) . . ? N8 C30 C29 111.8(6) . . ? C6 N1 C13 114.9(4) . . ? C6 N1 Fe1 115.3(3) . . ? C13 N1 Fe1 113.2(3) . . ? C18 N2 C14 119.0(4) . . ? C18 N2 Fe1 119.2(3) . . ? C14 N2 Fe1 121.6(3) . . ? C19 N3 N4 110.2(4) . . ? C19 N3 C18 130.4(5) . . ? N4 N3 C18 119.3(4) . . ? C21 N4 N3 105.2(5) . . ? C21 N4 Fe1 141.3(4) . . ? N3 N4 Fe1 113.0(3) . . ? C12 N5 C22 116.3(4) . . ? C12 N5 Fe1 111.3(3) . . ? C22 N5 Fe1 113.4(3) . . ? C23 N6 C27 119.8(4) . . ? C23 N6 Fe1 121.9(3) . . ? C27 N6 Fe1 118.2(3) . . ? C28 N7 N8 109.9(5) . . ? C28 N7 C27 131.3(5) . . ? N8 N7 C27 118.8(4) . . ? C30 N8 N7 105.1(4) . . ? C30 N8 Fe1 141.1(4) . . ? N7 N8 Fe1 113.5(3) . . ? N6 Fe1 N2 167.78(15) . . ? N6 Fe1 N8 74.58(15) . . ? N2 Fe1 N8 109.94(15) . . ? N6 Fe1 N4 117.34(15) . . ? N2 Fe1 N4 74.19(15) . . ? N8 Fe1 N4 94.22(16) . . ? N6 Fe1 N1 93.61(15) . . ? N2 Fe1 N1 75.12(15) . . ? N8 Fe1 N1 91.88(16) . . ? N4 Fe1 N1 148.97(16) . . ? N6 Fe1 N5 75.51(16) . . ? N2 Fe1 N5 100.12(15) . . ? N8 Fe1 N5 149.85(16) . . ? N4 Fe1 N5 96.14(17) . . ? N1 Fe1 N5 93.64(17) . . ? O6 Cl2 O8 114.6(6) . . ? O6 Cl2 O5 112.7(5) . . ? O8 Cl2 O5 106.0(5) . . ? O6 Cl2 O7 104.0(4) . . ? O8 Cl2 O7 109.6(5) . . ? O5 Cl2 O7 110.0(5) . . ? O2 Cl1 O1 112.7(10) . . ? O2 Cl1 O3 100.4(8) . . ? O1 Cl1 O3 111.2(8) . . ? O2 Cl1 O4 109.4(6) . . ? O1 Cl1 O4 109.3(4) . . ? O3 Cl1 O4 113.7(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 62.71 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.814 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.080 data_sh18190 _database_code_depnum_ccdc_archive 'CCDC 895361' #TrackingRef 'sh18190.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H26 Fe N8), 0.5(B2 F8), 3(B F4) ' _chemical_formula_sum 'C60 H52 B4 F16 Fe2 N16' _chemical_formula_weight 1456.12 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' 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 20.4210(9) _cell_length_b 13.0531(4) _cell_length_c 23.2971(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.612(4) _cell_angle_gamma 90.00 _cell_volume 5980.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 91.2(3) _cell_measurement_reflns_used 6252 _cell_measurement_theta_min 2.9389 _cell_measurement_theta_max 24.9922 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_T_min 0.44334 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 91.2(3) _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 'oxford gemini s' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time 5 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25047 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0775 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10501 _reflns_number_gt 5945 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1072P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10501 _refine_ls_number_parameters 929 _refine_ls_number_restraints 336 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1724 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.878 _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 C30 C 0.8702(2) 0.0767(3) 0.69041(19) 0.0343(10) Uani 1 1 d . . . H30 H 0.9014 0.0712 0.7276 0.041 Uiso 1 1 calc R . . C29 C 0.8083(2) 0.0271(3) 0.67453(19) 0.0385(11) Uani 1 1 d . . . H29 H 0.7908 -0.0171 0.6981 0.046 Uiso 1 1 calc R . . C28 C 0.7781(2) 0.0558(3) 0.61779(19) 0.0345(10) Uani 1 1 d . . . H28 H 0.7353 0.0357 0.5949 0.041 Uiso 1 1 calc R . . C27 C 0.8205(2) 0.1642(3) 0.54510(18) 0.0294(10) Uani 1 1 d . . . C26 C 0.7702(2) 0.1508(3) 0.49320(18) 0.0346(10) Uani 1 1 d . . . H26 H 0.7316 0.1121 0.4919 0.042 Uiso 1 1 calc R . . C25 C 0.7798(2) 0.1978(3) 0.44293(19) 0.0345(10) Uani 1 1 d . . . H25 H 0.7475 0.1900 0.4065 0.041 Uiso 1 1 calc R . . C24 C 0.8377(2) 0.2567(3) 0.44635(18) 0.0308(10) Uani 1 1 d . . . H24 H 0.8443 0.2877 0.4124 0.037 Uiso 1 1 calc R . . C23 C 0.8851(2) 0.2686(3) 0.50081(17) 0.0271(9) Uani 1 1 d . . . C22 C 0.9478(2) 0.3328(3) 0.51217(16) 0.0285(9) Uani 1 1 d . . . H22A H 0.9352 0.4047 0.5093 0.034 Uiso 1 1 calc R . . H22B H 0.9715 0.3184 0.4822 0.034 Uiso 1 1 calc R . . C12 C 1.0320(2) 0.4003(3) 0.60169(16) 0.0269(9) Uani 1 1 d . . . C11 C 1.1023(2) 0.3932(4) 0.61814(17) 0.0340(10) Uani 1 1 d . . . H11 H 1.1233 0.3337 0.6101 0.041 Uiso 1 1 calc R . . C10 C 1.1409(2) 0.4741(4) 0.64637(18) 0.0381(11) Uani 1 1 d . . . H10 H 1.1880 0.4680 0.6593 0.046 Uiso 1 1 calc R . . C9 C 1.1098(2) 0.5648(4) 0.65558(17) 0.0400(12) Uani 1 1 d . . . H9 H 1.1361 0.6206 0.6729 0.048 Uiso 1 1 calc R . . C8 C 1.0399(2) 0.5722(3) 0.63908(17) 0.0330(10) Uani 1 1 d . . . H8 H 1.0195 0.6335 0.6452 0.040 Uiso 1 1 calc R . . C7 C 0.9989(2) 0.4890(3) 0.61328(16) 0.0258(9) Uani 1 1 d . . . C1 C 0.9244(2) 0.4975(3) 0.60228(17) 0.0281(9) Uani 1 1 d . . . C2 C 0.8900(2) 0.5792(3) 0.56749(17) 0.0298(10) Uani 1 1 d . . . H2 H 0.9146 0.6248 0.5507 0.036 Uiso 1 1 calc R . . C3 C 0.8213(2) 0.5935(4) 0.55761(19) 0.0379(11) Uani 1 1 d . . . H3 H 0.7999 0.6475 0.5338 0.045 Uiso 1 1 calc R . . C4 C 0.7840(2) 0.5280(4) 0.58283(19) 0.0394(11) Uani 1 1 d . . . H4 H 0.7375 0.5383 0.5765 0.047 Uiso 1 1 calc R . . C5 C 0.8157(2) 0.4470(3) 0.61754(18) 0.0321(10) Uani 1 1 d . . . H5 H 0.7905 0.4028 0.6345 0.039 Uiso 1 1 calc R . . C6 C 0.8848(2) 0.4314(3) 0.62714(16) 0.0257(9) Uani 1 1 d . . . C13 C 0.9676(2) 0.3740(3) 0.72045(17) 0.0290(10) Uani 1 1 d . . . H13A H 0.9453 0.3831 0.7520 0.035 Uiso 1 1 calc R . . H13B H 0.9888 0.4385 0.7150 0.035 Uiso 1 1 calc R . . C14 C 1.0210(2) 0.2924(3) 0.73797(18) 0.0305(10) Uani 1 1 d . . . C15 C 1.0710(2) 0.2850(4) 0.79160(19) 0.0401(12) Uani 1 1 d . . . H15 H 1.0725 0.3313 0.8223 0.048 Uiso 1 1 calc R . . C16 C 1.1191(2) 0.2064(4) 0.7984(2) 0.0406(12) Uani 1 1 d . . . H16 H 1.1533 0.2008 0.8339 0.049 Uiso 1 1 calc R . . C17 C 1.1163(2) 0.1377(4) 0.7536(2) 0.0410(12) Uani 1 1 d . . . H17 H 1.1487 0.0861 0.7578 0.049 Uiso 1 1 calc R . . C18 C 1.0651(2) 0.1465(4) 0.70248(18) 0.0320(10) Uani 1 1 d . . . C19 C 1.0816(2) -0.0093(4) 0.6431(2) 0.0389(11) Uani 1 1 d . . . H19 H 1.1212 -0.0380 0.6671 0.047 Uiso 1 1 calc R . . C20 C 1.0415(2) -0.0483(4) 0.59133(19) 0.0393(11) Uani 1 1 d . . . H20 H 1.0483 -0.1092 0.5730 0.047 Uiso 1 1 calc R . . C21 C 0.9883(2) 0.0208(4) 0.57106(19) 0.0395(11) Uani 1 1 d . . . H21 H 0.9532 0.0125 0.5365 0.047 Uiso 1 1 calc R . . C51 C 0.4735(3) 0.9635(4) 0.4072(2) 0.0485(13) Uani 1 1 d . . . H51 H 0.5024 0.9785 0.4445 0.058 Uiso 1 1 calc R . . C50 C 0.4168(3) 1.0217(4) 0.3766(2) 0.0526(14) Uani 1 1 d . . . H50 H 0.4018 1.0819 0.3903 0.063 Uiso 1 1 calc R . . C49 C 0.3880(3) 0.9754(4) 0.3240(2) 0.0477(13) Uani 1 1 d . . . H49 H 0.3494 0.9965 0.2950 0.057 Uiso 1 1 calc R . . C48 C 0.4253(2) 0.8221(4) 0.27715(19) 0.0356(11) Uani 1 1 d . . . C47 C 0.3795(2) 0.8184(4) 0.2209(2) 0.0472(14) Uani 1 1 d . . . H47 H 0.3439 0.8651 0.2099 0.057 Uiso 1 1 calc R . . C46 C 0.3884(3) 0.7439(4) 0.1822(2) 0.0486(13) Uani 1 1 d . . . H46 H 0.3584 0.7394 0.1444 0.058 Uiso 1 1 calc R . . C45 C 0.4411(2) 0.6764(4) 0.19893(19) 0.0428(12) Uani 1 1 d . . . H45 H 0.4480 0.6269 0.1724 0.051 Uiso 1 1 calc R . . C44 C 0.4838(2) 0.6824(4) 0.25540(18) 0.0316(10) Uani 1 1 d . . . C43 C 0.5409(2) 0.6101(3) 0.28128(17) 0.0317(10) Uani 1 1 d . . . H43A H 0.5225 0.5445 0.2889 0.038 Uiso 1 1 calc R . . H43B H 0.5672 0.5992 0.2528 0.038 Uiso 1 1 calc R . . C36 C 0.6203(2) 0.5712(3) 0.37904(17) 0.0278(9) Uani 1 1 d . . . C35 C 0.6901(2) 0.5666(4) 0.39383(18) 0.0338(10) Uani 1 1 d . . . H35 H 0.7143 0.6135 0.3775 0.041 Uiso 1 1 calc R . . C34 C 0.7245(2) 0.4927(4) 0.43292(19) 0.0418(12) Uani 1 1 d . . . H34 H 0.7718 0.4902 0.4430 0.050 Uiso 1 1 calc R . . C33 C 0.6890(2) 0.4225(4) 0.4570(2) 0.0434(12) Uani 1 1 d . . . H33 H 0.7121 0.3723 0.4830 0.052 Uiso 1 1 calc R . . C32 C 0.6191(2) 0.4269(3) 0.44250(18) 0.0336(10) Uani 1 1 d . . . H32 H 0.5953 0.3791 0.4586 0.040 Uiso 1 1 calc R . . C31 C 0.5832(2) 0.5026(3) 0.40369(16) 0.0266(9) Uani 1 1 d . . . C37 C 0.5070(2) 0.5001(3) 0.38754(16) 0.0280(10) Uani 1 1 d . . . C38 C 0.4743(2) 0.4094(4) 0.36354(17) 0.0354(11) Uani 1 1 d . . . H38 H 0.5006 0.3522 0.3612 0.042 Uiso 1 1 calc R . . C39 C 0.4052(3) 0.4018(4) 0.34345(18) 0.0439(12) Uani 1 1 d . . . H39 H 0.3851 0.3404 0.3277 0.053 Uiso 1 1 calc R . . C40 C 0.3652(2) 0.4863(5) 0.34665(19) 0.0476(14) Uani 1 1 d . . . H40 H 0.3182 0.4828 0.3313 0.057 Uiso 1 1 calc R . . C41 C 0.3957(2) 0.5768(4) 0.37304(18) 0.0401(12) Uani 1 1 d . . . H41 H 0.3688 0.6326 0.3767 0.048 Uiso 1 1 calc R . . C42 C 0.4664(2) 0.5835(3) 0.39396(17) 0.0272(9) Uani 1 1 d . . . C52 C 0.5408(2) 0.6655(3) 0.48272(17) 0.0299(10) Uani 1 1 d . . . H52A H 0.5149 0.6816 0.5108 0.036 Uiso 1 1 calc R . . H52B H 0.5555 0.5947 0.4890 0.036 Uiso 1 1 calc R . . C53 C 0.6016(2) 0.7332(3) 0.49420(17) 0.0260(9) Uani 1 1 d . . . C54 C 0.6494(2) 0.7476(3) 0.54790(18) 0.0295(10) Uani 1 1 d . . . H54 H 0.6451 0.7137 0.5818 0.035 Uiso 1 1 calc R . . C55 C 0.7037(2) 0.8121(3) 0.55150(18) 0.0315(10) Uani 1 1 d . . . H55 H 0.7359 0.8222 0.5878 0.038 Uiso 1 1 calc R . . C56 C 0.7105(2) 0.8622(3) 0.50089(17) 0.0296(10) Uani 1 1 d . . . H56 H 0.7471 0.9054 0.5023 0.036 Uiso 1 1 calc R . . C57 C 0.6610(2) 0.8456(3) 0.44874(17) 0.0290(10) Uani 1 1 d . . . C58 C 0.7021(2) 0.9533(3) 0.37543(18) 0.0352(11) Uani 1 1 d . . . H58 H 0.7433 0.9780 0.3990 0.042 Uiso 1 1 calc R . . C59 C 0.6736(2) 0.9751(3) 0.31644(18) 0.0354(11) Uani 1 1 d . . . H59 H 0.6909 1.0177 0.2921 0.043 Uiso 1 1 calc R . . C60 C 0.6128(2) 0.9195(3) 0.30081(18) 0.0327(10) Uani 1 1 d . . . H60 H 0.5825 0.9194 0.2630 0.039 Uiso 1 1 calc R . . N8 N 0.87966(17) 0.1335(3) 0.64572(14) 0.0293(8) Uani 1 1 d . . . N7 N 0.82174(18) 0.1195(3) 0.60038(14) 0.0329(9) Uani 1 1 d . . . N6 N 0.87640(17) 0.2207(3) 0.54935(14) 0.0270(8) Uani 1 1 d . . . N1 N 0.91603(16) 0.3452(3) 0.66387(13) 0.0265(8) Uani 1 1 d . . . H1N H 0.8813 0.3191 0.6769 0.032 Uiso 1 1 calc R . . N4 N 0.99475(17) 0.1010(3) 0.60819(15) 0.0312(8) Uani 1 1 d . . . N3 N 1.05149(17) 0.0813(3) 0.65270(15) 0.0322(8) Uani 1 1 d . . . N2 N 1.01740(17) 0.2213(3) 0.69473(15) 0.0298(8) Uani 1 1 d . . . N5 N 0.99400(17) 0.3112(3) 0.57295(14) 0.0279(8) Uani 1 1 d . . . H5N H 1.0264 0.2690 0.5658 0.034 Uiso 1 1 calc R . . N12 N 0.47846(18) 0.8842(3) 0.37389(15) 0.0345(9) Uani 1 1 d . . . N11 N 0.42706(18) 0.8918(3) 0.32204(17) 0.0399(10) Uani 1 1 d . . . N10 N 0.47715(17) 0.7555(3) 0.29401(15) 0.0304(8) Uani 1 1 d . . . N9 N 0.58605(16) 0.6508(3) 0.33772(13) 0.0266(8) Uani 1 1 d . . . H9N H 0.6205 0.6811 0.3260 0.032 Uiso 1 1 calc R . . N16 N 0.60382(17) 0.8669(3) 0.34685(14) 0.0280(8) Uani 1 1 d . . . N15 N 0.65937(18) 0.8893(3) 0.39283(14) 0.0294(8) Uani 1 1 d . . . N14 N 0.60753(17) 0.7846(3) 0.44496(14) 0.0262(8) Uani 1 1 d . . . N13 N 0.49665(17) 0.6779(3) 0.42083(14) 0.0310(8) Uani 1 1 d . . . H13N H 0.4608 0.7155 0.4253 0.037 Uiso 1 1 calc R . . F1 F 0.84106(13) 0.2788(2) 0.74463(11) 0.0439(7) Uani 1 1 d U . . F2 F 0.72944(17) 0.2443(3) 0.70800(15) 0.0821(11) Uani 1 1 d U . . F3 F 0.76299(16) 0.4013(2) 0.74006(13) 0.0670(9) Uani 1 1 d U . . F4 F 0.77373(14) 0.2735(3) 0.80684(12) 0.0584(9) Uani 1 1 d U . . F5 F 0.82742(14) 0.7722(2) 0.45720(11) 0.0481(7) Uani 1 1 d U . . F6 F 0.93731(13) 0.8227(2) 0.48875(12) 0.0514(7) Uani 1 1 d U . . F7 F 0.85287(13) 0.9417(2) 0.47221(11) 0.0463(7) Uani 1 1 d U . . F8 F 0.87070(12) 0.8348(2) 0.55187(10) 0.0432(7) Uani 1 1 d U . . F9 F 0.38019(17) 0.7758(2) 0.46954(12) 0.0614(9) Uani 1 1 d U . . F10 F 0.38844(13) 0.8162(2) 0.56608(11) 0.0456(7) Uani 1 1 d U . . F11 F 0.37892(13) 0.9412(2) 0.49777(12) 0.0481(7) Uani 1 1 d U . . F12 F 0.47680(14) 0.8459(2) 0.52569(14) 0.0634(9) Uani 1 1 d U . . B4 B 0.2170(9) 0.8049(17) 0.7457(9) 0.038(5) Uani 0.50(3) 1 d PDU A 1 F13 F 0.2332(6) 0.7596(17) 0.6985(7) 0.057(4) Uani 0.50(3) 1 d PDU A 1 F14 F 0.1537(8) 0.7747(7) 0.7501(7) 0.054(4) Uani 0.50(3) 1 d PDU A 1 F15 F 0.2186(11) 0.9096(13) 0.7443(10) 0.054(5) Uani 0.50(3) 1 d PDU A 1 F16 F 0.2649(9) 0.7706(7) 0.7938(4) 0.071(4) Uani 0.50(3) 1 d PDU A 1 B4' B 0.2012(10) 0.8082(18) 0.7416(10) 0.032(4) Uani 0.50(3) 1 d PU A 2 F13' F 0.2320(9) 0.7816(18) 0.7018(8) 0.080(5) Uani 0.50(3) 1 d PDU A 2 F14' F 0.1331(4) 0.7836(6) 0.7154(9) 0.057(4) Uani 0.50(3) 1 d PDU A 2 F15' F 0.2043(10) 0.9192(11) 0.7478(8) 0.036(3) Uani 0.50(3) 1 d PDU A 2 F16' F 0.2180(11) 0.7719(5) 0.7971(3) 0.061(5) Uani 0.50(3) 1 d PDU A 2 Fe1 Fe 0.94654(3) 0.22344(5) 0.62294(2) 0.02611(18) Uani 1 1 d . . . Fe2 Fe 0.54135(3) 0.76996(5) 0.37017(2) 0.02620(18) Uani 1 1 d . . . B1 B 0.7759(3) 0.2965(4) 0.7502(2) 0.0379(13) Uani 1 1 d U . . B2 B 0.4053(3) 0.8441(4) 0.5151(3) 0.0425(13) Uani 1 1 d U . . B3 B 0.8724(3) 0.8424(4) 0.4921(2) 0.0363(12) Uani 1 1 d U . . 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 C30 0.055(3) 0.022(2) 0.031(2) 0.0021(19) 0.019(2) 0.008(2) C29 0.065(3) 0.019(2) 0.039(3) -0.002(2) 0.027(2) -0.004(2) C28 0.047(3) 0.023(2) 0.037(3) -0.002(2) 0.018(2) -0.009(2) C27 0.041(2) 0.020(2) 0.029(2) -0.0006(18) 0.0129(19) -0.003(2) C26 0.045(3) 0.021(2) 0.035(2) -0.0030(19) 0.006(2) -0.007(2) C25 0.043(3) 0.025(3) 0.030(2) 0.0027(19) 0.0019(19) -0.002(2) C24 0.043(3) 0.022(2) 0.028(2) 0.0006(18) 0.0105(19) 0.001(2) C23 0.036(2) 0.017(2) 0.029(2) 0.0014(18) 0.0102(18) 0.0027(19) C22 0.044(2) 0.020(2) 0.021(2) -0.0009(17) 0.0076(18) -0.001(2) C12 0.037(2) 0.024(2) 0.021(2) 0.0007(17) 0.0096(18) -0.0038(19) C11 0.040(3) 0.035(3) 0.028(2) 0.001(2) 0.0116(19) 0.002(2) C10 0.037(3) 0.051(3) 0.029(2) 0.003(2) 0.0118(19) -0.005(2) C9 0.049(3) 0.052(3) 0.019(2) -0.001(2) 0.009(2) -0.027(3) C8 0.050(3) 0.026(2) 0.024(2) -0.0013(19) 0.0117(19) -0.010(2) C7 0.036(2) 0.021(2) 0.021(2) 0.0004(17) 0.0089(17) -0.0049(19) C1 0.041(2) 0.017(2) 0.027(2) -0.0038(18) 0.0108(18) -0.0011(19) C2 0.045(3) 0.018(2) 0.031(2) 0.0021(18) 0.0182(19) 0.000(2) C3 0.047(3) 0.031(3) 0.037(3) 0.009(2) 0.013(2) 0.007(2) C4 0.034(2) 0.039(3) 0.045(3) 0.005(2) 0.010(2) 0.007(2) C5 0.038(3) 0.023(2) 0.037(2) 0.0047(19) 0.013(2) -0.003(2) C6 0.038(2) 0.017(2) 0.022(2) -0.0006(17) 0.0074(17) 0.0050(18) C13 0.039(2) 0.026(2) 0.025(2) -0.0019(18) 0.0135(18) -0.006(2) C14 0.036(2) 0.028(3) 0.026(2) 0.0080(19) 0.0049(18) -0.006(2) C15 0.053(3) 0.040(3) 0.027(2) -0.003(2) 0.009(2) -0.017(2) C16 0.039(3) 0.038(3) 0.037(3) 0.014(2) -0.002(2) -0.010(2) C17 0.043(3) 0.035(3) 0.044(3) 0.004(2) 0.009(2) -0.008(2) C18 0.032(2) 0.032(3) 0.031(2) 0.010(2) 0.0075(19) -0.003(2) C19 0.046(3) 0.025(3) 0.051(3) 0.010(2) 0.022(2) 0.009(2) C20 0.059(3) 0.027(3) 0.036(3) -0.002(2) 0.020(2) 0.006(2) C21 0.064(3) 0.027(3) 0.032(2) -0.002(2) 0.020(2) 0.007(2) C51 0.084(4) 0.027(3) 0.047(3) 0.005(2) 0.039(3) 0.010(3) C50 0.075(4) 0.025(3) 0.070(4) 0.012(3) 0.041(3) 0.020(3) C49 0.056(3) 0.038(3) 0.055(3) 0.021(3) 0.026(3) 0.017(3) C48 0.040(3) 0.038(3) 0.033(3) 0.009(2) 0.018(2) 0.003(2) C47 0.034(3) 0.048(3) 0.056(3) 0.032(3) 0.006(2) -0.005(2) C46 0.055(3) 0.054(4) 0.033(3) 0.004(3) 0.006(2) -0.018(3) C45 0.045(3) 0.049(3) 0.030(3) 0.007(2) 0.004(2) -0.012(3) C44 0.038(2) 0.030(3) 0.029(2) 0.002(2) 0.0125(19) -0.011(2) C43 0.046(3) 0.026(2) 0.024(2) 0.0011(18) 0.0118(19) -0.007(2) C36 0.039(2) 0.020(2) 0.027(2) -0.0016(18) 0.0124(18) 0.0048(19) C35 0.040(3) 0.028(3) 0.036(2) 0.001(2) 0.016(2) 0.002(2) C34 0.039(3) 0.047(3) 0.039(3) 0.004(2) 0.011(2) 0.010(2) C33 0.058(3) 0.034(3) 0.042(3) 0.009(2) 0.020(2) 0.014(2) C32 0.050(3) 0.019(2) 0.037(2) 0.0040(19) 0.022(2) 0.002(2) C31 0.040(2) 0.017(2) 0.024(2) 0.0003(17) 0.0119(18) 0.0017(19) C37 0.041(2) 0.023(2) 0.022(2) 0.0015(18) 0.0119(18) -0.005(2) C38 0.057(3) 0.028(3) 0.026(2) -0.0018(19) 0.019(2) -0.013(2) C39 0.060(3) 0.046(3) 0.027(2) -0.001(2) 0.012(2) -0.022(3) C40 0.042(3) 0.065(4) 0.034(3) 0.014(3) 0.006(2) -0.023(3) C41 0.042(3) 0.051(3) 0.031(2) 0.016(2) 0.016(2) 0.010(2) C42 0.035(2) 0.023(2) 0.024(2) 0.0033(18) 0.0075(18) -0.0022(19) C52 0.048(3) 0.017(2) 0.028(2) -0.0020(18) 0.0145(19) 0.001(2) C53 0.042(2) 0.014(2) 0.027(2) -0.0024(17) 0.0169(19) 0.0008(19) C54 0.046(3) 0.021(2) 0.025(2) 0.0020(17) 0.0159(19) 0.005(2) C55 0.044(3) 0.028(2) 0.022(2) -0.0019(19) 0.0092(18) 0.002(2) C56 0.039(2) 0.023(2) 0.027(2) 0.0014(18) 0.0101(19) 0.0010(19) C57 0.046(3) 0.019(2) 0.026(2) 0.0007(18) 0.0150(19) -0.001(2) C58 0.051(3) 0.026(3) 0.032(2) -0.002(2) 0.016(2) -0.005(2) C59 0.061(3) 0.022(2) 0.030(2) 0.0002(19) 0.023(2) -0.005(2) C60 0.049(3) 0.023(2) 0.029(2) 0.0079(19) 0.016(2) 0.007(2) N8 0.046(2) 0.0155(18) 0.0291(19) 0.0028(15) 0.0154(16) 0.0009(16) N7 0.047(2) 0.026(2) 0.0256(19) -0.0003(16) 0.0082(17) -0.0056(17) N6 0.042(2) 0.0155(18) 0.0264(18) -0.0008(15) 0.0143(15) -0.0003(16) N1 0.0369(19) 0.0170(19) 0.0267(18) 0.0013(14) 0.0105(15) -0.0034(15) N4 0.040(2) 0.023(2) 0.033(2) 0.0032(16) 0.0134(17) -0.0007(17) N3 0.039(2) 0.027(2) 0.033(2) 0.0016(17) 0.0130(16) 0.0023(17) N2 0.039(2) 0.025(2) 0.0298(19) 0.0060(16) 0.0167(16) 0.0037(17) N5 0.040(2) 0.0177(18) 0.0240(18) 0.0000(14) 0.0059(15) 0.0011(16) N12 0.051(2) 0.025(2) 0.034(2) 0.0013(17) 0.0231(18) 0.0014(18) N11 0.039(2) 0.033(2) 0.051(2) 0.019(2) 0.0173(19) 0.0087(19) N10 0.0333(19) 0.031(2) 0.032(2) 0.0102(17) 0.0169(16) 0.0001(17) N9 0.0394(19) 0.0179(19) 0.0223(18) -0.0014(14) 0.0082(15) -0.0015(15) N16 0.042(2) 0.0183(19) 0.0219(18) -0.0001(15) 0.0061(15) -0.0001(16) N15 0.050(2) 0.0185(19) 0.0220(18) 0.0044(15) 0.0126(16) -0.0017(17) N14 0.041(2) 0.0161(18) 0.0247(18) -0.0033(14) 0.0143(15) -0.0023(16) N13 0.042(2) 0.023(2) 0.031(2) 0.0038(16) 0.0150(16) 0.0044(17) F1 0.0514(15) 0.0339(16) 0.0555(17) 0.0132(13) 0.0300(13) 0.0106(13) F2 0.077(2) 0.087(3) 0.073(2) -0.034(2) 0.0030(18) -0.002(2) F3 0.096(2) 0.0415(19) 0.071(2) 0.0088(16) 0.0347(17) 0.0310(17) F4 0.0525(17) 0.089(3) 0.0396(15) 0.0186(15) 0.0232(13) 0.0127(16) F5 0.0659(18) 0.0368(16) 0.0429(15) -0.0097(13) 0.0167(13) -0.0086(14) F6 0.0555(17) 0.0395(17) 0.0673(19) -0.0026(15) 0.0303(14) 0.0062(14) F7 0.0573(17) 0.0249(15) 0.0612(17) 0.0083(13) 0.0239(13) 0.0014(13) F8 0.0543(16) 0.0432(17) 0.0360(14) -0.0059(12) 0.0189(12) -0.0068(13) F9 0.112(3) 0.0317(17) 0.0397(16) -0.0043(13) 0.0183(16) 0.0028(16) F10 0.0655(18) 0.0378(16) 0.0371(15) -0.0021(12) 0.0198(13) -0.0047(14) F11 0.0636(17) 0.0223(15) 0.0690(18) 0.0065(13) 0.0360(14) 0.0072(13) F12 0.0592(18) 0.0417(19) 0.098(2) 0.0056(17) 0.0360(16) 0.0127(15) B4 0.055(9) 0.030(7) 0.035(8) -0.003(7) 0.021(7) -0.003(8) F13 0.037(5) 0.080(10) 0.056(6) -0.036(5) 0.017(4) 0.001(4) F14 0.075(7) 0.037(4) 0.068(9) -0.020(5) 0.052(7) -0.020(5) F15 0.053(10) 0.028(5) 0.090(8) 0.012(4) 0.036(6) 0.000(5) F16 0.086(9) 0.053(5) 0.057(4) -0.003(3) -0.012(5) 0.019(5) B4' 0.041(7) 0.022(7) 0.038(7) 0.006(6) 0.019(6) 0.010(6) F13' 0.121(9) 0.070(9) 0.078(7) -0.031(6) 0.078(8) -0.019(6) F14' 0.039(4) 0.025(4) 0.098(10) -0.019(5) 0.005(4) -0.003(3) F15' 0.024(6) 0.021(4) 0.054(6) 0.008(3) -0.003(5) 0.002(4) F16' 0.128(14) 0.023(3) 0.033(3) 0.008(3) 0.021(5) 0.005(5) Fe1 0.0402(4) 0.0175(3) 0.0223(3) 0.0004(2) 0.0113(3) 0.0007(3) Fe2 0.0398(4) 0.0172(3) 0.0238(3) 0.0016(2) 0.0123(3) 0.0023(3) B1 0.051(3) 0.030(3) 0.034(3) 0.000(2) 0.014(2) 0.013(3) B2 0.061(3) 0.024(3) 0.046(3) 0.003(2) 0.020(3) 0.001(3) B3 0.043(3) 0.023(3) 0.045(3) 0.002(2) 0.017(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C30 N8 1.334(5) . ? C30 C29 1.380(6) . ? C30 H30 0.9300 . ? C29 C28 1.353(6) . ? C29 H29 0.9300 . ? C28 N7 1.358(5) . ? C28 H28 0.9300 . ? C27 N6 1.340(5) . ? C27 C26 1.371(6) . ? C27 N7 1.408(5) . ? C26 C25 1.383(6) . ? C26 H26 0.9300 . ? C25 C24 1.395(6) . ? C25 H25 0.9300 . ? C24 C23 1.382(6) . ? C24 H24 0.9300 . ? C23 N6 1.345(5) . ? C23 C22 1.492(6) . ? C22 N5 1.502(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C12 C11 1.385(6) . ? C12 C7 1.403(6) . ? C12 N5 1.457(5) . ? C11 C10 1.376(6) . ? C11 H11 0.9300 . ? C10 C9 1.387(7) . ? C10 H10 0.9300 . ? C9 C8 1.379(6) . ? C9 H9 0.9300 . ? C8 C7 1.404(6) . ? C8 H8 0.9300 . ? C7 C1 1.477(5) . ? C1 C2 1.407(6) . ? C1 C6 1.408(6) . ? C2 C3 1.372(6) . ? C2 H2 0.9300 . ? C3 C4 1.378(6) . ? C3 H3 0.9300 . ? C4 C5 1.382(6) . ? C4 H4 0.9300 . ? C5 C6 1.383(5) . ? C5 H5 0.9300 . ? C6 N1 1.453(5) . ? C13 N1 1.497(5) . ? C13 C14 1.500(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N2 1.357(5) . ? C14 C15 1.387(6) . ? C15 C16 1.401(7) . ? C15 H15 0.9300 . ? C16 C17 1.367(7) . ? C16 H16 0.9300 . ? C17 C18 1.361(6) . ? C17 H17 0.9300 . ? C18 N2 1.357(5) . ? C18 N3 1.405(5) . ? C19 C20 1.360(6) . ? C19 N3 1.379(6) . ? C19 H19 0.9300 . ? C20 C21 1.393(6) . ? C20 H20 0.9300 . ? C21 N4 1.341(5) . ? C21 H21 0.9300 . ? C51 N12 1.314(6) . ? C51 C50 1.408(7) . ? C51 H51 0.9300 . ? C50 C49 1.352(7) . ? C50 H50 0.9300 . ? C49 N11 1.360(6) . ? C49 H49 0.9300 . ? C48 N10 1.345(6) . ? C48 N11 1.379(6) . ? C48 C47 1.390(6) . ? C47 C46 1.372(7) . ? C47 H47 0.9300 . ? C46 C45 1.364(7) . ? C46 H46 0.9300 . ? C45 C44 1.371(6) . ? C45 H45 0.9300 . ? C44 N10 1.343(5) . ? C44 C43 1.496(6) . ? C43 N9 1.486(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C36 C35 1.375(5) . ? C36 C31 1.393(6) . ? C36 N9 1.460(5) . ? C35 C34 1.382(6) . ? C35 H35 0.9300 . ? C34 C33 1.378(6) . ? C34 H34 0.9300 . ? C33 C32 1.376(6) . ? C33 H33 0.9300 . ? C32 C31 1.405(6) . ? C32 H32 0.9300 . ? C31 C37 1.501(5) . ? C37 C38 1.399(6) . ? C37 C42 1.400(6) . ? C38 C39 1.366(6) . ? C38 H38 0.9300 . ? C39 C40 1.386(7) . ? C39 H39 0.9300 . ? C40 C41 1.398(7) . ? C40 H40 0.9300 . ? C41 C42 1.397(6) . ? C41 H41 0.9300 . ? C42 N13 1.444(5) . ? C52 C53 1.488(6) . ? C52 N13 1.490(5) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 N14 1.362(5) . ? C53 C54 1.377(6) . ? C54 C55 1.377(6) . ? C54 H54 0.9300 . ? C55 C56 1.387(5) . ? C55 H55 0.9300 . ? C56 C57 1.372(5) . ? C56 H56 0.9300 . ? C57 N14 1.336(5) . ? C57 N15 1.414(5) . ? C58 N15 1.347(5) . ? C58 C59 1.370(6) . ? C58 H58 0.9300 . ? C59 C60 1.399(6) . ? C59 H59 0.9300 . ? C60 N16 1.327(5) . ? C60 H60 0.9300 . ? N8 N7 1.370(5) . ? N8 Fe1 1.979(3) . ? N6 Fe1 1.916(3) . ? N1 Fe1 2.035(3) . ? N1 H1N 0.9100 . ? N4 N3 1.355(5) . ? N4 Fe1 1.955(4) . ? N2 Fe1 1.895(3) . ? N5 Fe1 2.053(3) . ? N5 H5N 0.9100 . ? N12 N11 1.374(5) . ? N12 Fe2 1.985(4) . ? N10 Fe2 1.911(3) . ? N9 Fe2 2.049(3) . ? N9 H9N 0.9100 . ? N16 N15 1.366(4) . ? N16 Fe2 1.974(3) . ? N14 Fe2 1.906(3) . ? N13 Fe2 2.061(3) . ? N13 H13N 0.9100 . ? F1 B1 1.392(6) . ? F2 B1 1.353(6) . ? F3 B1 1.400(6) . ? F4 B1 1.364(6) . ? F5 B3 1.393(6) . ? F6 B3 1.374(6) . ? F7 B3 1.398(6) . ? F8 B3 1.405(6) . ? F9 B2 1.374(6) . ? F10 B2 1.372(6) . ? F11 B2 1.394(6) . ? F12 B2 1.415(6) . ? B4 F16 1.351(16) . ? B4 F13 1.367(17) . ? B4 F15 1.367(18) . ? B4 F14 1.381(16) . ? B4' F13' 1.30(2) . ? B4' F16' 1.33(2) . ? B4' F14' 1.40(2) . ? B4' F15' 1.46(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 C30 C29 111.5(4) . . ? N8 C30 H30 124.2 . . ? C29 C30 H30 124.2 . . ? C28 C29 C30 106.0(4) . . ? C28 C29 H29 127.0 . . ? C30 C29 H29 127.0 . . ? C29 C28 N7 107.4(4) . . ? C29 C28 H28 126.3 . . ? N7 C28 H28 126.3 . . ? N6 C27 C26 123.9(4) . . ? N6 C27 N7 110.8(3) . . ? C26 C27 N7 125.3(4) . . ? C27 C26 C25 116.5(4) . . ? C27 C26 H26 121.8 . . ? C25 C26 H26 121.8 . . ? C26 C25 C24 120.6(4) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C23 C24 C25 119.2(4) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? N6 C23 C24 120.1(4) . . ? N6 C23 C22 114.4(3) . . ? C24 C23 C22 125.5(4) . . ? C23 C22 N5 110.7(3) . . ? C23 C22 H22A 109.5 . . ? N5 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C11 C12 C7 121.3(4) . . ? C11 C12 N5 117.2(4) . . ? C7 C12 N5 121.5(3) . . ? C10 C11 C12 120.0(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C10 C9 120.1(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C8 C9 C10 120.0(4) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C8 C7 121.2(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C12 C7 C8 117.3(4) . . ? C12 C7 C1 123.7(4) . . ? C8 C7 C1 118.9(4) . . ? C2 C1 C6 116.7(4) . . ? C2 C1 C7 119.2(4) . . ? C6 C1 C7 124.1(4) . . ? C3 C2 C1 121.9(4) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C2 C3 C4 120.2(4) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 121.1(4) . . ? C5 C6 N1 118.4(3) . . ? C1 C6 N1 120.5(3) . . ? N1 C13 C14 110.4(3) . . ? N1 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N1 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N2 C14 C15 120.0(4) . . ? N2 C14 C13 113.2(3) . . ? C15 C14 C13 126.8(4) . . ? C14 C15 C16 118.5(4) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C17 C16 C15 120.7(4) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C18 C17 C16 118.5(5) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? N2 C18 C17 122.1(4) . . ? N2 C18 N3 110.5(3) . . ? C17 C18 N3 127.3(4) . . ? C20 C19 N3 106.1(4) . . ? C20 C19 H19 127.0 . . ? N3 C19 H19 127.0 . . ? C19 C20 C21 106.7(4) . . ? C19 C20 H20 126.7 . . ? C21 C20 H20 126.7 . . ? N4 C21 C20 110.8(4) . . ? N4 C21 H21 124.6 . . ? C20 C21 H21 124.6 . . ? N12 C51 C50 108.0(5) . . ? N12 C51 H51 126.0 . . ? C50 C51 H51 126.0 . . ? C49 C50 C51 108.4(5) . . ? C49 C50 H50 125.8 . . ? C51 C50 H50 125.8 . . ? C50 C49 N11 105.8(4) . . ? C50 C49 H49 127.1 . . ? N11 C49 H49 127.1 . . ? N10 C48 N11 110.3(4) . . ? N10 C48 C47 122.0(5) . . ? N11 C48 C47 127.7(5) . . ? C46 C47 C48 118.0(5) . . ? C46 C47 H47 121.0 . . ? C48 C47 H47 121.0 . . ? C45 C46 C47 120.3(5) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C46 C45 C44 119.1(5) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? N10 C44 C45 122.1(4) . . ? N10 C44 C43 112.8(3) . . ? C45 C44 C43 125.2(4) . . ? N9 C43 C44 111.2(3) . . ? N9 C43 H43A 109.4 . . ? C44 C43 H43A 109.4 . . ? N9 C43 H43B 109.4 . . ? C44 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? C35 C36 C31 120.7(4) . . ? C35 C36 N9 118.5(4) . . ? C31 C36 N9 120.8(3) . . ? C36 C35 C34 120.3(4) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C33 C34 C35 120.2(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C32 C33 C34 119.8(4) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C33 C32 C31 121.0(4) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C36 C31 C32 118.0(4) . . ? C36 C31 C37 123.6(3) . . ? C32 C31 C37 118.2(4) . . ? C38 C37 C42 117.9(4) . . ? C38 C37 C31 118.0(4) . . ? C42 C37 C31 124.1(4) . . ? C39 C38 C37 122.4(5) . . ? C39 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? C38 C39 C40 119.5(5) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C39 C40 C41 119.8(4) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C42 C41 C40 120.2(5) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C37 120.0(4) . . ? C41 C42 N13 119.1(4) . . ? C37 C42 N13 120.9(3) . . ? C53 C52 N13 111.6(3) . . ? C53 C52 H52A 109.3 . . ? N13 C52 H52A 109.3 . . ? C53 C52 H52B 109.3 . . ? N13 C52 H52B 109.3 . . ? H52A C52 H52B 108.0 . . ? N14 C53 C54 119.8(4) . . ? N14 C53 C52 113.6(3) . . ? C54 C53 C52 126.7(4) . . ? C55 C54 C53 120.1(4) . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C54 C55 C56 119.9(4) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C57 C56 C55 117.4(4) . . ? C57 C56 H56 121.3 . . ? C55 C56 H56 121.3 . . ? N14 C57 C56 123.1(4) . . ? N14 C57 N15 111.3(3) . . ? C56 C57 N15 125.5(4) . . ? N15 C58 C59 107.2(4) . . ? N15 C58 H58 126.4 . . ? C59 C58 H58 126.4 . . ? C58 C59 C60 105.2(4) . . ? C58 C59 H59 127.4 . . ? C60 C59 H59 127.4 . . ? N16 C60 C59 111.3(4) . . ? N16 C60 H60 124.3 . . ? C59 C60 H60 124.3 . . ? C30 N8 N7 104.6(3) . . ? C30 N8 Fe1 142.6(3) . . ? N7 N8 Fe1 112.8(2) . . ? C28 N7 N8 110.6(3) . . ? C28 N7 C27 132.5(4) . . ? N8 N7 C27 116.7(3) . . ? C27 N6 C23 119.7(3) . . ? C27 N6 Fe1 119.6(3) . . ? C23 N6 Fe1 120.5(3) . . ? C6 N1 C13 114.6(3) . . ? C6 N1 Fe1 118.0(2) . . ? C13 N1 Fe1 112.2(2) . . ? C6 N1 H1N 103.2 . . ? C13 N1 H1N 103.2 . . ? Fe1 N1 H1N 103.2 . . ? C21 N4 N3 105.1(4) . . ? C21 N4 Fe1 141.7(3) . . ? N3 N4 Fe1 112.8(3) . . ? N4 N3 C19 111.4(4) . . ? N4 N3 C18 117.1(3) . . ? C19 N3 C18 131.0(4) . . ? C14 N2 C18 120.0(4) . . ? C14 N2 Fe1 121.4(3) . . ? C18 N2 Fe1 118.6(3) . . ? C12 N5 C22 113.9(3) . . ? C12 N5 Fe1 117.3(2) . . ? C22 N5 Fe1 111.5(2) . . ? C12 N5 H5N 104.1 . . ? C22 N5 H5N 104.1 . . ? Fe1 N5 H5N 104.1 . . ? C51 N12 N11 107.5(4) . . ? C51 N12 Fe2 140.5(4) . . ? N11 N12 Fe2 111.5(3) . . ? C49 N11 N12 110.2(4) . . ? C49 N11 C48 131.2(4) . . ? N12 N11 C48 118.5(4) . . ? C44 N10 C48 118.5(4) . . ? C44 N10 Fe2 121.6(3) . . ? C48 N10 Fe2 119.8(3) . . ? C36 N9 C43 113.7(3) . . ? C36 N9 Fe2 118.6(2) . . ? C43 N9 Fe2 111.5(2) . . ? C36 N9 H9N 103.6 . . ? C43 N9 H9N 103.6 . . ? Fe2 N9 H9N 103.6 . . ? C60 N16 N15 104.9(3) . . ? C60 N16 Fe2 142.6(3) . . ? N15 N16 Fe2 112.5(2) . . ? C58 N15 N16 111.5(3) . . ? C58 N15 C57 132.1(4) . . ? N16 N15 C57 116.4(3) . . ? C57 N14 C53 119.6(3) . . ? C57 N14 Fe2 119.1(3) . . ? C53 N14 Fe2 121.3(3) . . ? C42 N13 C52 113.8(3) . . ? C42 N13 Fe2 116.9(2) . . ? C52 N13 Fe2 111.8(2) . . ? C42 N13 H13N 104.2 . . ? C52 N13 H13N 104.2 . . ? Fe2 N13 H13N 104.2 . . ? F16 B4 F13 104.2(15) . . ? F16 B4 F15 109.6(16) . . ? F13 B4 F15 113.6(17) . . ? F16 B4 F14 109.1(14) . . ? F13 B4 F14 111.8(15) . . ? F15 B4 F14 108.5(16) . . ? F13' B4' F16' 123.4(19) . . ? F13' B4' F14' 104.1(17) . . ? F16' B4' F14' 107.9(15) . . ? F13' B4' F15' 108.7(17) . . ? F16' B4' F15' 105.3(17) . . ? F14' B4' F15' 106.4(15) . . ? N2 Fe1 N6 177.69(15) . . ? N2 Fe1 N4 80.92(15) . . ? N6 Fe1 N4 96.78(14) . . ? N2 Fe1 N8 99.96(14) . . ? N6 Fe1 N8 79.93(14) . . ? N4 Fe1 N8 88.79(14) . . ? N2 Fe1 N1 81.67(14) . . ? N6 Fe1 N1 100.63(13) . . ? N4 Fe1 N1 162.28(13) . . ? N8 Fe1 N1 90.98(13) . . ? N2 Fe1 N5 98.27(13) . . ? N6 Fe1 N5 81.74(13) . . ? N4 Fe1 N5 91.13(14) . . ? N8 Fe1 N5 161.53(13) . . ? N1 Fe1 N5 94.62(13) . . ? N14 Fe2 N10 178.27(13) . . ? N14 Fe2 N16 80.54(13) . . ? N10 Fe2 N16 98.09(13) . . ? N14 Fe2 N12 101.13(14) . . ? N10 Fe2 N12 79.90(15) . . ? N16 Fe2 N12 90.23(14) . . ? N14 Fe2 N9 97.84(13) . . ? N10 Fe2 N9 81.06(14) . . ? N16 Fe2 N9 90.01(14) . . ? N12 Fe2 N9 160.81(14) . . ? N14 Fe2 N13 81.32(13) . . ? N10 Fe2 N13 100.08(14) . . ? N16 Fe2 N13 161.75(13) . . ? N12 Fe2 N13 91.23(14) . . ? N9 Fe2 N13 94.51(14) . . ? F2 B1 F4 113.2(5) . . ? F2 B1 F1 110.4(4) . . ? F4 B1 F1 109.5(4) . . ? F2 B1 F3 107.8(4) . . ? F4 B1 F3 109.0(4) . . ? F1 B1 F3 106.7(4) . . ? F10 B2 F9 111.6(4) . . ? F10 B2 F11 108.9(4) . . ? F9 B2 F11 109.4(4) . . ? F10 B2 F12 109.9(4) . . ? F9 B2 F12 107.4(4) . . ? F11 B2 F12 109.6(4) . . ? F6 B3 F5 109.7(4) . . ? F6 B3 F7 110.3(4) . . ? F5 B3 F7 109.4(4) . . ? F6 B3 F8 108.9(4) . . ? F5 B3 F8 110.2(4) . . ? F7 B3 F8 108.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 C30 C29 C28 -0.8(5) . . . . ? C30 C29 C28 N7 1.0(5) . . . . ? N6 C27 C26 C25 1.2(7) . . . . ? N7 C27 C26 C25 -177.2(4) . . . . ? C27 C26 C25 C24 -1.0(6) . . . . ? C26 C25 C24 C23 -0.7(6) . . . . ? C25 C24 C23 N6 2.3(6) . . . . ? C25 C24 C23 C22 -177.1(4) . . . . ? N6 C23 C22 N5 11.9(5) . . . . ? C24 C23 C22 N5 -168.7(4) . . . . ? C7 C12 C11 C10 0.0(6) . . . . ? N5 C12 C11 C10 -178.9(4) . . . . ? C12 C11 C10 C9 -3.4(6) . . . . ? C11 C10 C9 C8 3.2(6) . . . . ? C10 C9 C8 C7 0.5(6) . . . . ? C11 C12 C7 C8 3.6(6) . . . . ? N5 C12 C7 C8 -177.7(3) . . . . ? C11 C12 C7 C1 -173.7(4) . . . . ? N5 C12 C7 C1 5.1(6) . . . . ? C9 C8 C7 C12 -3.8(5) . . . . ? C9 C8 C7 C1 173.6(3) . . . . ? C12 C7 C1 C2 -126.8(4) . . . . ? C8 C7 C1 C2 55.9(5) . . . . ? C12 C7 C1 C6 56.7(5) . . . . ? C8 C7 C1 C6 -120.5(4) . . . . ? C6 C1 C2 C3 -0.7(6) . . . . ? C7 C1 C2 C3 -177.4(4) . . . . ? C1 C2 C3 C4 1.2(6) . . . . ? C2 C3 C4 C5 -0.8(7) . . . . ? C3 C4 C5 C6 0.1(7) . . . . ? C4 C5 C6 C1 0.4(6) . . . . ? C4 C5 C6 N1 -179.9(4) . . . . ? C2 C1 C6 C5 -0.1(6) . . . . ? C7 C1 C6 C5 176.5(4) . . . . ? C2 C1 C6 N1 -179.8(3) . . . . ? C7 C1 C6 N1 -3.2(6) . . . . ? N1 C13 C14 N2 10.5(5) . . . . ? N1 C13 C14 C15 -170.0(4) . . . . ? N2 C14 C15 C16 3.4(6) . . . . ? C13 C14 C15 C16 -176.2(4) . . . . ? C14 C15 C16 C17 -0.8(7) . . . . ? C15 C16 C17 C18 -1.1(7) . . . . ? C16 C17 C18 N2 0.5(7) . . . . ? C16 C17 C18 N3 -176.7(4) . . . . ? N3 C19 C20 C21 0.3(5) . . . . ? C19 C20 C21 N4 0.6(5) . . . . ? N12 C51 C50 C49 -0.1(6) . . . . ? C51 C50 C49 N11 -1.1(5) . . . . ? N10 C48 C47 C46 0.1(7) . . . . ? N11 C48 C47 C46 177.9(4) . . . . ? C48 C47 C46 C45 -0.3(7) . . . . ? C47 C46 C45 C44 1.7(7) . . . . ? C46 C45 C44 N10 -2.9(7) . . . . ? C46 C45 C44 C43 176.1(4) . . . . ? N10 C44 C43 N9 -13.5(5) . . . . ? C45 C44 C43 N9 167.5(4) . . . . ? C31 C36 C35 C34 0.9(6) . . . . ? N9 C36 C35 C34 179.8(4) . . . . ? C36 C35 C34 C33 0.4(7) . . . . ? C35 C34 C33 C32 -0.6(7) . . . . ? C34 C33 C32 C31 -0.5(7) . . . . ? C35 C36 C31 C32 -1.9(6) . . . . ? N9 C36 C31 C32 179.1(4) . . . . ? C35 C36 C31 C37 -177.2(4) . . . . ? N9 C36 C31 C37 3.9(6) . . . . ? C33 C32 C31 C36 1.7(6) . . . . ? C33 C32 C31 C37 177.2(4) . . . . ? C36 C31 C37 C38 120.5(4) . . . . ? C32 C31 C37 C38 -54.7(5) . . . . ? C36 C31 C37 C42 -58.3(5) . . . . ? C32 C31 C37 C42 126.5(4) . . . . ? C42 C37 C38 C39 3.7(6) . . . . ? C31 C37 C38 C39 -175.1(3) . . . . ? C37 C38 C39 C40 0.0(6) . . . . ? C38 C39 C40 C41 -3.2(6) . . . . ? C39 C40 C41 C42 2.6(6) . . . . ? C40 C41 C42 C37 1.2(6) . . . . ? C40 C41 C42 N13 179.8(4) . . . . ? C38 C37 C42 C41 -4.2(6) . . . . ? C31 C37 C42 C41 174.6(3) . . . . ? C38 C37 C42 N13 177.2(3) . . . . ? C31 C37 C42 N13 -4.0(6) . . . . ? N13 C52 C53 N14 -5.7(5) . . . . ? N13 C52 C53 C54 173.8(4) . . . . ? N14 C53 C54 C55 -1.3(6) . . . . ? C52 C53 C54 C55 179.2(4) . . . . ? C53 C54 C55 C56 -0.4(6) . . . . ? C54 C55 C56 C57 0.9(6) . . . . ? C55 C56 C57 N14 0.3(6) . . . . ? C55 C56 C57 N15 -179.7(4) . . . . ? N15 C58 C59 C60 -0.7(5) . . . . ? C58 C59 C60 N16 0.2(5) . . . . ? C29 C30 N8 N7 0.2(5) . . . . ? C29 C30 N8 Fe1 -177.4(3) . . . . ? C29 C28 N7 N8 -0.9(5) . . . . ? C29 C28 N7 C27 173.0(4) . . . . ? C30 N8 N7 C28 0.4(4) . . . . ? Fe1 N8 N7 C28 178.8(3) . . . . ? C30 N8 N7 C27 -174.5(3) . . . . ? Fe1 N8 N7 C27 3.9(4) . . . . ? N6 C27 N7 C28 -178.6(4) . . . . ? C26 C27 N7 C28 -0.1(7) . . . . ? N6 C27 N7 N8 -5.1(5) . . . . ? C26 C27 N7 N8 173.5(4) . . . . ? C26 C27 N6 C23 0.4(6) . . . . ? N7 C27 N6 C23 179.0(3) . . . . ? C26 C27 N6 Fe1 -174.6(3) . . . . ? N7 C27 N6 Fe1 4.0(5) . . . . ? C24 C23 N6 C27 -2.2(6) . . . . ? C22 C23 N6 C27 177.3(4) . . . . ? C24 C23 N6 Fe1 172.7(3) . . . . ? C22 C23 N6 Fe1 -7.8(5) . . . . ? C5 C6 N1 C13 -116.2(4) . . . . ? C1 C6 N1 C13 63.5(4) . . . . ? C5 C6 N1 Fe1 108.3(3) . . . . ? C1 C6 N1 Fe1 -72.0(4) . . . . ? C14 C13 N1 C6 -149.8(3) . . . . ? C14 C13 N1 Fe1 -11.6(4) . . . . ? C20 C21 N4 N3 -1.2(5) . . . . ? C20 C21 N4 Fe1 -172.6(3) . . . . ? C21 N4 N3 C19 1.4(5) . . . . ? Fe1 N4 N3 C19 175.7(3) . . . . ? C21 N4 N3 C18 -171.3(4) . . . . ? Fe1 N4 N3 C18 2.9(4) . . . . ? C20 C19 N3 N4 -1.1(5) . . . . ? C20 C19 N3 C18 170.3(4) . . . . ? N2 C18 N3 N4 -1.8(5) . . . . ? C17 C18 N3 N4 175.7(4) . . . . ? N2 C18 N3 C19 -172.9(4) . . . . ? C17 C18 N3 C19 4.6(7) . . . . ? C15 C14 N2 C18 -4.0(6) . . . . ? C13 C14 N2 C18 175.6(3) . . . . ? C15 C14 N2 Fe1 175.9(3) . . . . ? C13 C14 N2 Fe1 -4.5(5) . . . . ? C17 C18 N2 C14 2.0(6) . . . . ? N3 C18 N2 C14 179.7(3) . . . . ? C17 C18 N2 Fe1 -177.8(3) . . . . ? N3 C18 N2 Fe1 -0.2(4) . . . . ? C11 C12 N5 C22 -121.9(4) . . . . ? C7 C12 N5 C22 59.3(5) . . . . ? C11 C12 N5 Fe1 105.2(3) . . . . ? C7 C12 N5 Fe1 -73.6(4) . . . . ? C23 C22 N5 C12 -146.3(3) . . . . ? C23 C22 N5 Fe1 -10.7(4) . . . . ? C50 C51 N12 N11 1.3(5) . . . . ? C50 C51 N12 Fe2 171.1(4) . . . . ? C50 C49 N11 N12 2.0(5) . . . . ? C50 C49 N11 C48 -173.6(4) . . . . ? C51 N12 N11 C49 -2.1(5) . . . . ? Fe2 N12 N11 C49 -175.2(3) . . . . ? C51 N12 N11 C48 174.1(4) . . . . ? Fe2 N12 N11 C48 1.0(5) . . . . ? N10 C48 N11 C49 175.7(4) . . . . ? C47 C48 N11 C49 -2.3(8) . . . . ? N10 C48 N11 N12 0.5(5) . . . . ? C47 C48 N11 N12 -177.6(4) . . . . ? C45 C44 N10 C48 2.6(6) . . . . ? C43 C44 N10 C48 -176.5(4) . . . . ? C45 C44 N10 Fe2 -174.8(3) . . . . ? C43 C44 N10 Fe2 6.2(5) . . . . ? N11 C48 N10 C44 -179.3(3) . . . . ? C47 C48 N10 C44 -1.1(6) . . . . ? N11 C48 N10 Fe2 -1.9(5) . . . . ? C47 C48 N10 Fe2 176.2(3) . . . . ? C35 C36 N9 C43 117.3(4) . . . . ? C31 C36 N9 C43 -63.8(5) . . . . ? C35 C36 N9 Fe2 -108.7(4) . . . . ? C31 C36 N9 Fe2 70.3(4) . . . . ? C44 C43 N9 C36 151.9(3) . . . . ? C44 C43 N9 Fe2 14.5(4) . . . . ? C59 C60 N16 N15 0.3(5) . . . . ? C59 C60 N16 Fe2 -178.2(4) . . . . ? C59 C58 N15 N16 0.9(5) . . . . ? C59 C58 N15 C57 -176.9(4) . . . . ? C60 N16 N15 C58 -0.8(4) . . . . ? Fe2 N16 N15 C58 178.3(3) . . . . ? C60 N16 N15 C57 177.4(3) . . . . ? Fe2 N16 N15 C57 -3.5(4) . . . . ? N14 C57 N15 C58 -179.1(4) . . . . ? C56 C57 N15 C58 0.9(7) . . . . ? N14 C57 N15 N16 3.1(5) . . . . ? C56 C57 N15 N16 -176.9(4) . . . . ? C56 C57 N14 C53 -2.0(6) . . . . ? N15 C57 N14 C53 178.0(3) . . . . ? C56 C57 N14 Fe2 178.7(3) . . . . ? N15 C57 N14 Fe2 -1.2(4) . . . . ? C54 C53 N14 C57 2.4(6) . . . . ? C52 C53 N14 C57 -178.0(4) . . . . ? C54 C53 N14 Fe2 -178.3(3) . . . . ? C52 C53 N14 Fe2 1.3(5) . . . . ? C41 C42 N13 C52 122.9(4) . . . . ? C37 C42 N13 C52 -58.5(5) . . . . ? C41 C42 N13 Fe2 -104.3(4) . . . . ? C37 C42 N13 Fe2 74.3(4) . . . . ? C53 C52 N13 C42 142.5(3) . . . . ? C53 C52 N13 Fe2 7.3(4) . . . . ? C14 N2 Fe1 N6 -178(100) . . . . ? C18 N2 Fe1 N6 1(4) . . . . ? C14 N2 Fe1 N4 -178.5(3) . . . . ? C18 N2 Fe1 N4 1.3(3) . . . . ? C14 N2 Fe1 N8 -91.3(3) . . . . ? C18 N2 Fe1 N8 88.5(3) . . . . ? C14 N2 Fe1 N1 -1.8(3) . . . . ? C18 N2 Fe1 N1 178.0(3) . . . . ? C14 N2 Fe1 N5 91.7(3) . . . . ? C18 N2 Fe1 N5 -88.5(3) . . . . ? C27 N6 Fe1 N2 86(4) . . . . ? C23 N6 Fe1 N2 -89(4) . . . . ? C27 N6 Fe1 N4 85.9(3) . . . . ? C23 N6 Fe1 N4 -89.0(3) . . . . ? C27 N6 Fe1 N8 -1.6(3) . . . . ? C23 N6 Fe1 N8 -176.6(3) . . . . ? C27 N6 Fe1 N1 -90.7(3) . . . . ? C23 N6 Fe1 N1 94.3(3) . . . . ? C27 N6 Fe1 N5 176.1(3) . . . . ? C23 N6 Fe1 N5 1.1(3) . . . . ? C21 N4 Fe1 N2 168.7(5) . . . . ? N3 N4 Fe1 N2 -2.2(3) . . . . ? C21 N4 Fe1 N6 -11.3(5) . . . . ? N3 N4 Fe1 N6 177.8(3) . . . . ? C21 N4 Fe1 N8 68.4(5) . . . . ? N3 N4 Fe1 N8 -102.5(3) . . . . ? C21 N4 Fe1 N1 157.9(5) . . . . ? N3 N4 Fe1 N1 -13.1(6) . . . . ? C21 N4 Fe1 N5 -93.1(5) . . . . ? N3 N4 Fe1 N5 95.9(3) . . . . ? C30 N8 Fe1 N2 -1.5(5) . . . . ? N7 N8 Fe1 N2 -178.9(3) . . . . ? C30 N8 Fe1 N6 176.2(5) . . . . ? N7 N8 Fe1 N6 -1.3(3) . . . . ? C30 N8 Fe1 N4 79.1(5) . . . . ? N7 N8 Fe1 N4 -98.4(3) . . . . ? C30 N8 Fe1 N1 -83.2(5) . . . . ? N7 N8 Fe1 N1 99.3(3) . . . . ? C30 N8 Fe1 N5 169.0(4) . . . . ? N7 N8 Fe1 N5 -8.4(6) . . . . ? C6 N1 Fe1 N2 144.2(3) . . . . ? C13 N1 Fe1 N2 7.6(3) . . . . ? C6 N1 Fe1 N6 -35.9(3) . . . . ? C13 N1 Fe1 N6 -172.5(2) . . . . ? C6 N1 Fe1 N4 155.1(4) . . . . ? C13 N1 Fe1 N4 18.5(6) . . . . ? C6 N1 Fe1 N8 -115.8(3) . . . . ? C13 N1 Fe1 N8 107.6(3) . . . . ? C6 N1 Fe1 N5 46.5(3) . . . . ? C13 N1 Fe1 N5 -90.1(3) . . . . ? C12 N5 Fe1 N2 -42.7(3) . . . . ? C22 N5 Fe1 N2 -176.7(3) . . . . ? C12 N5 Fe1 N6 139.6(3) . . . . ? C22 N5 Fe1 N6 5.7(3) . . . . ? C12 N5 Fe1 N4 -123.7(3) . . . . ? C22 N5 Fe1 N4 102.3(3) . . . . ? C12 N5 Fe1 N8 146.7(4) . . . . ? C22 N5 Fe1 N8 12.8(6) . . . . ? C12 N5 Fe1 N1 39.5(3) . . . . ? C22 N5 Fe1 N1 -94.4(3) . . . . ? C57 N14 Fe2 N10 37(5) . . . . ? C53 N14 Fe2 N10 -142(5) . . . . ? C57 N14 Fe2 N16 -0.5(3) . . . . ? C53 N14 Fe2 N16 -179.7(3) . . . . ? C57 N14 Fe2 N12 -88.8(3) . . . . ? C53 N14 Fe2 N12 91.9(3) . . . . ? C57 N14 Fe2 N9 88.2(3) . . . . ? C53 N14 Fe2 N9 -91.0(3) . . . . ? C57 N14 Fe2 N13 -178.4(3) . . . . ? C53 N14 Fe2 N13 2.4(3) . . . . ? C44 N10 Fe2 N14 53(5) . . . . ? C48 N10 Fe2 N14 -124(5) . . . . ? C44 N10 Fe2 N16 90.5(3) . . . . ? C48 N10 Fe2 N16 -86.8(3) . . . . ? C44 N10 Fe2 N12 179.3(3) . . . . ? C48 N10 Fe2 N12 2.0(3) . . . . ? C44 N10 Fe2 N9 1.8(3) . . . . ? C48 N10 Fe2 N9 -175.5(3) . . . . ? C44 N10 Fe2 N13 -91.2(3) . . . . ? C48 N10 Fe2 N13 91.5(3) . . . . ? C60 N16 Fe2 N14 -179.4(5) . . . . ? N15 N16 Fe2 N14 2.1(3) . . . . ? C60 N16 Fe2 N10 1.7(5) . . . . ? N15 N16 Fe2 N10 -176.8(3) . . . . ? C60 N16 Fe2 N12 -78.1(5) . . . . ? N15 N16 Fe2 N12 103.4(3) . . . . ? C60 N16 Fe2 N9 82.7(5) . . . . ? N15 N16 Fe2 N9 -95.8(3) . . . . ? C60 N16 Fe2 N13 -172.8(4) . . . . ? N15 N16 Fe2 N13 8.7(6) . . . . ? C51 N12 Fe2 N14 7.5(5) . . . . ? N11 N12 Fe2 N14 177.0(3) . . . . ? C51 N12 Fe2 N10 -171.1(5) . . . . ? N11 N12 Fe2 N10 -1.5(3) . . . . ? C51 N12 Fe2 N16 -72.9(5) . . . . ? N11 N12 Fe2 N16 96.6(3) . . . . ? C51 N12 Fe2 N9 -163.6(4) . . . . ? N11 N12 Fe2 N9 5.9(6) . . . . ? C51 N12 Fe2 N13 88.9(5) . . . . ? N11 N12 Fe2 N13 -101.6(3) . . . . ? C36 N9 Fe2 N14 37.1(3) . . . . ? C43 N9 Fe2 N14 172.1(3) . . . . ? C36 N9 Fe2 N10 -144.2(3) . . . . ? C43 N9 Fe2 N10 -9.2(3) . . . . ? C36 N9 Fe2 N16 117.6(3) . . . . ? C43 N9 Fe2 N16 -107.4(3) . . . . ? C36 N9 Fe2 N12 -151.7(4) . . . . ? C43 N9 Fe2 N12 -16.7(6) . . . . ? C36 N9 Fe2 N13 -44.7(3) . . . . ? C43 N9 Fe2 N13 90.3(3) . . . . ? C42 N13 Fe2 N14 -139.1(3) . . . . ? C52 N13 Fe2 N14 -5.3(3) . . . . ? C42 N13 Fe2 N10 39.9(3) . . . . ? C52 N13 Fe2 N10 173.6(3) . . . . ? C42 N13 Fe2 N16 -145.6(4) . . . . ? C52 N13 Fe2 N16 -11.9(6) . . . . ? C42 N13 Fe2 N12 119.9(3) . . . . ? C52 N13 Fe2 N12 -106.4(3) . . . . ? C42 N13 Fe2 N9 -41.8(3) . . . . ? C52 N13 Fe2 N9 91.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.714 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.111 data_sh181rt _database_code_depnum_ccdc_archive 'CCDC 895362' #TrackingRef 'sh181rt.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H26 Fe N8, 2(B F4)' _chemical_formula_sum 'C60 H52 B4 F16 Fe2 N16' _chemical_formula_weight 1456.12 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' 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 10.5414(3) _cell_length_b 13.0245(4) _cell_length_c 23.2290(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.677(3) _cell_angle_gamma 90.00 _cell_volume 3123.25(16) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5301 _cell_measurement_theta_min 2.9149 _cell_measurement_theta_max 24.9996 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_T_min 0.84846 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'oxford gemini s' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time 25 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13036 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5517 _reflns_number_gt 3981 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5517 _refine_ls_number_parameters 542 _refine_ls_number_restraints 298 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 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 C21 C 0.5971(3) 0.0055(2) 0.60697(13) 0.0759(8) Uani 1 1 d . . . H21 H 0.5492 -0.0201 0.5719 0.091 Uiso 1 1 calc R . . C20 C 0.7155(3) -0.0327(3) 0.63523(16) 0.0861(9) Uani 1 1 d . . . H20 H 0.7603 -0.0874 0.6229 0.103 Uiso 1 1 calc R . . C19 C 0.7534(3) 0.0239(2) 0.68371(14) 0.0767(8) Uani 1 1 d . . . H19 H 0.8296 0.0164 0.7117 0.092 Uiso 1 1 calc R . . C18 C 0.6463(2) 0.1669(2) 0.72644(10) 0.0520(6) Uani 1 1 d . . . C17 C 0.7309(2) 0.1755(2) 0.78027(12) 0.0680(7) Uani 1 1 d . . . H17 H 0.8025 0.1327 0.7902 0.082 Uiso 1 1 calc R . . C16 C 0.7056(3) 0.2485(3) 0.81772(12) 0.0782(9) Uani 1 1 d . . . H16 H 0.7602 0.2556 0.8543 0.094 Uiso 1 1 calc R . . C15 C 0.6004(3) 0.3124(2) 0.80244(11) 0.0650(7) Uani 1 1 d . . . H15 H 0.5826 0.3620 0.8285 0.078 Uiso 1 1 calc R . . C14 C 0.5219(2) 0.30114(18) 0.74753(9) 0.0495(5) Uani 1 1 d . . . C13 C 0.4103(2) 0.3713(2) 0.72531(10) 0.0581(6) Uani 1 1 d . . . H13A H 0.3574 0.3770 0.7548 0.070 Uiso 1 1 calc R . . H13B H 0.4432 0.4392 0.7193 0.070 Uiso 1 1 calc R . . C6 C 0.2724(2) 0.41475(18) 0.62955(10) 0.0503(5) Uani 1 1 d . . . C5 C 0.1395(2) 0.4248(2) 0.61643(12) 0.0648(7) Uani 1 1 d . . . H5 H 0.0886 0.3808 0.6337 0.078 Uiso 1 1 calc R . . C4 C 0.0814(2) 0.4994(3) 0.57792(13) 0.0793(9) Uani 1 1 d . . . H4 H -0.0084 0.5050 0.5689 0.095 Uiso 1 1 calc R . . C3 C 0.1556(3) 0.5652(2) 0.55301(13) 0.0805(8) Uani 1 1 d . . . H3 H 0.1164 0.6164 0.5276 0.097 Uiso 1 1 calc R . . C2 C 0.2879(2) 0.5557(2) 0.56546(12) 0.0663(7) Uani 1 1 d . . . H2 H 0.3377 0.6010 0.5483 0.080 Uiso 1 1 calc R . . C1 C 0.3491(2) 0.47963(18) 0.60325(10) 0.0514(6) Uani 1 1 d . . . C7 C 0.4947(2) 0.47567(18) 0.61660(10) 0.0513(6) Uani 1 1 d . . . C8 C 0.5615(2) 0.5594(2) 0.64552(11) 0.0643(7) Uani 1 1 d . . . H8 H 0.5147 0.6165 0.6531 0.077 Uiso 1 1 calc R . . C9 C 0.6940(3) 0.5606(2) 0.66315(12) 0.0733(8) Uani 1 1 d . . . H9 H 0.7361 0.6175 0.6823 0.088 Uiso 1 1 calc R . . C10 C 0.7629(2) 0.4764(3) 0.65204(12) 0.0746(8) Uani 1 1 d . . . H10 H 0.8522 0.4749 0.6653 0.089 Uiso 1 1 calc R . . C11 C 0.7014(2) 0.3938(2) 0.62149(11) 0.0658(7) Uani 1 1 d . . . H11 H 0.7495 0.3378 0.6133 0.079 Uiso 1 1 calc R . . C12 C 0.5677(2) 0.39387(19) 0.60286(9) 0.0502(6) Uani 1 1 d . . . C22 C 0.4234(2) 0.3259(2) 0.51280(10) 0.0591(6) Uani 1 1 d . . . H22A H 0.4680 0.3046 0.4821 0.071 Uiso 1 1 calc R . . H22B H 0.4077 0.3991 0.5086 0.071 Uiso 1 1 calc R . . C23 C 0.2967(2) 0.27114(18) 0.50485(9) 0.0501(5) Uani 1 1 d . . . C24 C 0.2026(3) 0.2797(2) 0.45389(11) 0.0679(7) Uani 1 1 d . . . H24 H 0.2164 0.3205 0.4228 0.081 Uiso 1 1 calc R . . C25 C 0.0879(3) 0.2265(2) 0.45024(12) 0.0741(8) Uani 1 1 d . . . H25 H 0.0245 0.2304 0.4160 0.089 Uiso 1 1 calc R . . C26 C 0.0663(2) 0.1681(2) 0.49625(12) 0.0671(7) Uani 1 1 d . . . H26 H -0.0118 0.1339 0.4948 0.081 Uiso 1 1 calc R . . C27 C 0.1659(2) 0.16242(18) 0.54500(10) 0.0505(5) Uani 1 1 d . . . C28 C 0.0598(3) 0.0450(2) 0.60669(13) 0.0696(7) Uani 1 1 d . . . H28 H -0.0213 0.0358 0.5826 0.083 Uiso 1 1 calc R . . C29 C 0.1028(3) 0.0014(2) 0.65958(14) 0.0762(8) Uani 1 1 d . . . H29 H 0.0581 -0.0440 0.6791 0.091 Uiso 1 1 calc R . . C30 C 0.2271(3) 0.0380(2) 0.67887(11) 0.0675(7) Uani 1 1 d . . . H30 H 0.2797 0.0207 0.7147 0.081 Uiso 1 1 calc R . . N4 N 0.56064(19) 0.08384(16) 0.63651(9) 0.0597(5) Uani 1 1 d . . . N3 N 0.65901(17) 0.09423(16) 0.68408(9) 0.0573(5) Uani 1 1 d . . . N2 N 0.54380(16) 0.22780(14) 0.71043(7) 0.0459(4) Uani 1 1 d . . . N1 N 0.32893(19) 0.33494(15) 0.66971(8) 0.0508(5) Uani 1 1 d D . . N8 N 0.26222(18) 0.10127(15) 0.63979(8) 0.0530(5) Uani 1 1 d . . . N7 N 0.15693(17) 0.10496(15) 0.59519(8) 0.0534(5) Uani 1 1 d . . . N6 N 0.27732(16) 0.21158(14) 0.54931(7) 0.0454(4) Uani 1 1 d . . . N5 N 0.50782(19) 0.30529(16) 0.57103(9) 0.0531(5) Uani 1 1 d D . . B1 B 0.0554(12) 0.2674(9) 0.7550(4) 0.072(3) Uani 0.555(7) 1 d PDU A 1 F1 F 0.0389(5) 0.2358(9) 0.8069(3) 0.164(5) Uani 0.555(7) 1 d PDU A 1 F2 F -0.0302(8) 0.2260(6) 0.7080(3) 0.169(4) Uani 0.555(7) 1 d PDU A 1 F3 F 0.0374(6) 0.3713(4) 0.7460(3) 0.134(2) Uani 0.555(7) 1 d PDU A 1 F4 F 0.1761(6) 0.2522(8) 0.7477(4) 0.101(2) Uani 0.555(7) 1 d PDU A 1 B1' B 0.0452(12) 0.2516(11) 0.7541(6) 0.072(4) Uani 0.445(7) 1 d PDU A 2 F1' F 0.0202(4) 0.1540(4) 0.7689(4) 0.115(3) Uani 0.445(7) 1 d PDU A 2 F2' F -0.0580(8) 0.2855(10) 0.7190(5) 0.191(5) Uani 0.445(7) 1 d PDU A 2 F3' F 0.0556(11) 0.3040(9) 0.8019(5) 0.197(6) Uani 0.445(7) 1 d PDU A 2 F4' F 0.1484(12) 0.2396(12) 0.7319(7) 0.174(6) Uani 0.445(7) 1 d PDU A 2 Fe1 Fe 0.41548(3) 0.20404(3) 0.628607(12) 0.04633(13) Uani 1 1 d . . . B2 B 0.2899(12) 0.8616(10) 0.5104(6) 0.102(5) Uani 0.393(18) 1 d PDU B 1 F5 F 0.2287(10) 0.8116(11) 0.5502(6) 0.127(4) Uani 0.393(18) 1 d PDU B 1 F6 F 0.244(2) 0.8279(14) 0.4564(6) 0.136(4) Uani 0.393(18) 1 d PDU B 1 F7 F 0.4154(9) 0.8365(14) 0.5332(12) 0.175(6) Uani 0.393(18) 1 d PDU B 1 F8 F 0.286(2) 0.9653(8) 0.5129(7) 0.145(5) Uani 0.393(18) 1 d PDU B 1 B2' B 0.2905(7) 0.8603(6) 0.5092(3) 0.070(3) Uani 0.607(18) 1 d PDU B 2 F5' F 0.2707(13) 0.8343(10) 0.5601(3) 0.185(4) Uani 0.607(18) 1 d PDU B 2 F6' F 0.2405(11) 0.7884(7) 0.4676(5) 0.128(3) Uani 0.607(18) 1 d PDU B 2 F7' F 0.4178(6) 0.8667(6) 0.5042(3) 0.106(2) Uani 0.607(18) 1 d PDU B 2 F8' F 0.2264(5) 0.9495(5) 0.4954(4) 0.0991(18) Uani 0.607(18) 1 d PDU B 2 H1N H 0.262(2) 0.300(2) 0.6796(12) 0.077(9) Uiso 1 1 d D . . H5N H 0.565(2) 0.2610(16) 0.5641(10) 0.057(7) Uiso 1 1 d 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 C21 0.094(2) 0.0646(19) 0.0772(18) -0.0134(15) 0.0371(16) -0.0081(16) C20 0.095(2) 0.063(2) 0.111(2) 0.0046(19) 0.0480(19) 0.0193(17) C19 0.0662(16) 0.079(2) 0.093(2) 0.0114(18) 0.0354(15) 0.0193(16) C18 0.0475(12) 0.0555(15) 0.0564(13) 0.0057(11) 0.0188(10) -0.0055(11) C17 0.0462(13) 0.083(2) 0.0691(17) 0.0143(15) -0.0011(12) -0.0042(13) C16 0.0741(18) 0.100(2) 0.0538(15) -0.0005(16) -0.0020(14) -0.0221(18) C15 0.0756(17) 0.0694(19) 0.0490(14) -0.0087(12) 0.0104(12) -0.0203(15) C14 0.0588(13) 0.0484(14) 0.0436(11) -0.0029(10) 0.0161(10) -0.0107(11) C13 0.0728(14) 0.0538(15) 0.0517(13) -0.0067(11) 0.0221(11) 0.0001(13) C6 0.0508(11) 0.0449(14) 0.0570(13) -0.0040(10) 0.0149(10) 0.0055(11) C5 0.0506(13) 0.0687(18) 0.0784(17) 0.0038(14) 0.0210(12) 0.0039(13) C4 0.0491(13) 0.092(2) 0.096(2) 0.0090(18) 0.0109(14) 0.0120(15) C3 0.0758(17) 0.077(2) 0.0848(19) 0.0166(16) 0.0079(15) 0.0266(17) C2 0.0711(15) 0.0525(16) 0.0781(17) 0.0110(13) 0.0214(13) 0.0068(14) C1 0.0501(12) 0.0468(14) 0.0581(13) -0.0029(11) 0.0130(10) 0.0029(11) C7 0.0505(12) 0.0476(14) 0.0584(13) 0.0018(11) 0.0174(10) -0.0022(11) C8 0.0693(15) 0.0558(17) 0.0714(16) -0.0070(13) 0.0226(13) -0.0084(13) C9 0.0737(17) 0.080(2) 0.0655(16) -0.0071(15) 0.0132(13) -0.0255(17) C10 0.0504(13) 0.100(3) 0.0709(17) 0.0058(16) 0.0061(12) -0.0155(16) C11 0.0505(13) 0.077(2) 0.0736(16) 0.0069(14) 0.0202(12) 0.0031(13) C12 0.0493(12) 0.0531(15) 0.0512(12) 0.0037(11) 0.0171(10) -0.0050(11) C22 0.0736(15) 0.0571(16) 0.0512(13) 0.0034(11) 0.0236(11) -0.0003(13) C23 0.0603(13) 0.0485(15) 0.0434(12) -0.0017(10) 0.0148(10) 0.0079(11) C24 0.0807(17) 0.073(2) 0.0474(14) 0.0083(12) 0.0072(12) 0.0109(15) C25 0.0663(16) 0.089(2) 0.0595(16) 0.0016(15) -0.0052(13) 0.0134(16) C26 0.0530(13) 0.0750(19) 0.0690(17) -0.0097(14) 0.0019(12) 0.0016(13) C27 0.0542(12) 0.0458(13) 0.0518(13) -0.0067(10) 0.0115(10) 0.0032(11) C28 0.0645(14) 0.0613(18) 0.0894(19) -0.0085(15) 0.0310(14) -0.0150(14) C29 0.0863(19) 0.0571(18) 0.097(2) 0.0021(16) 0.0458(17) -0.0095(15) C30 0.0877(18) 0.0570(17) 0.0648(15) 0.0084(13) 0.0322(14) 0.0087(15) N4 0.0680(12) 0.0534(13) 0.0628(12) -0.0110(10) 0.0253(10) -0.0011(10) N3 0.0511(10) 0.0565(13) 0.0673(13) 0.0071(10) 0.0191(10) 0.0057(10) N2 0.0475(9) 0.0486(12) 0.0430(9) 0.0016(8) 0.0125(8) -0.0034(9) N1 0.0557(11) 0.0427(11) 0.0562(11) -0.0020(9) 0.0165(9) -0.0006(10) N8 0.0627(11) 0.0475(12) 0.0515(10) 0.0028(9) 0.0182(9) 0.0015(9) N7 0.0538(10) 0.0500(12) 0.0584(11) -0.0049(9) 0.0159(9) -0.0037(9) N6 0.0507(10) 0.0434(11) 0.0431(9) -0.0035(8) 0.0118(8) 0.0008(9) N5 0.0571(11) 0.0465(12) 0.0590(12) -0.0001(9) 0.0196(9) 0.0023(10) B1 0.091(7) 0.076(6) 0.058(5) -0.003(4) 0.034(5) 0.017(6) F1 0.088(3) 0.323(13) 0.092(4) 0.086(6) 0.046(3) 0.030(5) F2 0.162(6) 0.172(7) 0.153(5) -0.091(5) -0.014(4) 0.005(5) F3 0.160(4) 0.090(3) 0.146(5) -0.026(3) 0.019(3) 0.048(3) F4 0.074(2) 0.098(5) 0.142(4) 0.055(4) 0.051(2) 0.015(2) B1' 0.039(5) 0.065(7) 0.109(11) -0.023(6) 0.006(5) -0.010(5) F1' 0.076(3) 0.086(4) 0.191(7) 0.015(4) 0.047(4) -0.004(2) F2' 0.123(5) 0.244(13) 0.192(9) 0.131(8) 0.002(6) 0.050(7) F3' 0.276(10) 0.180(9) 0.161(9) -0.100(8) 0.107(7) -0.039(7) F4' 0.201(9) 0.117(7) 0.268(13) 0.022(8) 0.200(10) 0.033(8) Fe1 0.05090(19) 0.0488(2) 0.03876(18) -0.00200(14) 0.00781(13) -0.00089(15) B2 0.097(8) 0.085(8) 0.097(8) 0.057(7) -0.048(7) -0.059(7) F5 0.096(5) 0.147(8) 0.132(7) 0.067(6) 0.014(4) -0.008(5) F6 0.186(8) 0.121(10) 0.098(5) -0.008(6) 0.022(4) -0.030(9) F7 0.064(4) 0.163(10) 0.289(16) -0.054(11) 0.012(6) 0.006(4) F8 0.216(14) 0.081(5) 0.158(9) -0.025(5) 0.082(9) 0.029(7) B2' 0.073(5) 0.084(6) 0.066(5) -0.020(4) 0.044(4) 0.024(5) F5' 0.257(10) 0.234(8) 0.073(3) 0.028(4) 0.053(5) -0.055(7) F6' 0.139(4) 0.092(5) 0.149(6) -0.062(5) 0.022(4) -0.006(4) F7' 0.078(2) 0.121(4) 0.120(4) -0.025(3) 0.025(2) 0.011(2) F8' 0.095(3) 0.067(3) 0.138(4) 0.001(3) 0.031(3) 0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C21 N4 1.329(3) . ? C21 C20 1.380(4) . ? C21 H21 0.9300 . ? C20 C19 1.338(4) . ? C20 H20 0.9300 . ? C19 N3 1.354(3) . ? C19 H19 0.9300 . ? C18 N2 1.331(3) . ? C18 C17 1.386(3) . ? C18 N3 1.392(3) . ? C17 C16 1.351(4) . ? C17 H17 0.9300 . ? C16 C15 1.374(4) . ? C16 H16 0.9300 . ? C15 C14 1.381(3) . ? C15 H15 0.9300 . ? C14 N2 1.338(3) . ? C14 C13 1.496(3) . ? C13 N1 1.476(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C6 C5 1.379(3) . ? C6 C1 1.393(3) . ? C6 N1 1.442(3) . ? C5 C4 1.378(4) . ? C5 H5 0.9300 . ? C4 C3 1.365(4) . ? C4 H4 0.9300 . ? C3 C2 1.371(4) . ? C3 H3 0.9300 . ? C2 C1 1.393(3) . ? C2 H2 0.9300 . ? C1 C7 1.504(3) . ? C7 C12 1.388(3) . ? C7 C8 1.394(3) . ? C8 C9 1.373(4) . ? C8 H8 0.9300 . ? C9 C10 1.368(4) . ? C9 H9 0.9300 . ? C10 C11 1.377(4) . ? C10 H10 0.9300 . ? C11 C12 1.388(3) . ? C11 H11 0.9300 . ? C12 N5 1.445(3) . ? C22 N5 1.485(3) . ? C22 C23 1.492(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N6 1.340(3) . ? C23 C24 1.387(3) . ? C24 C25 1.381(4) . ? C24 H24 0.9300 . ? C25 C26 1.368(4) . ? C25 H25 0.9300 . ? C26 C27 1.382(3) . ? C26 H26 0.9300 . ? C27 N6 1.324(3) . ? C27 N7 1.404(3) . ? C28 C29 1.346(4) . ? C28 N7 1.356(3) . ? C28 H28 0.9300 . ? C29 C30 1.380(4) . ? C29 H29 0.9300 . ? C30 N8 1.333(3) . ? C30 H30 0.9300 . ? N4 N3 1.360(3) . ? N4 Fe1 2.171(2) . ? N2 Fe1 2.1207(17) . ? N1 Fe1 2.2368(19) . ? N1 H1N 0.905(17) . ? N8 N7 1.357(2) . ? N8 Fe1 2.1539(19) . ? N6 Fe1 2.1065(17) . ? N5 Fe1 2.237(2) . ? N5 H5N 0.871(16) . ? B1 F1 1.319(10) . ? B1 F4 1.331(11) . ? B1 F3 1.376(12) . ? B1 F2 1.377(11) . ? B1' F3' 1.290(14) . ? B1' F2' 1.297(13) . ? B1' F4' 1.303(14) . ? B1' F1' 1.356(14) . ? B2 F6 1.324(14) . ? B2 F8 1.353(13) . ? B2 F7 1.362(14) . ? B2 F5 1.392(14) . ? B2' F5' 1.286(9) . ? B2' F8' 1.350(9) . ? B2' F6' 1.372(9) . ? B2' F7' 1.374(9) . ? 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 N4 C21 C20 111.1(3) . . ? N4 C21 H21 124.5 . . ? C20 C21 H21 124.5 . . ? C19 C20 C21 106.8(3) . . ? C19 C20 H20 126.6 . . ? C21 C20 H20 126.6 . . ? C20 C19 N3 106.5(3) . . ? C20 C19 H19 126.8 . . ? N3 C19 H19 126.8 . . ? N2 C18 C17 122.8(2) . . ? N2 C18 N3 113.36(19) . . ? C17 C18 N3 123.8(2) . . ? C16 C17 C18 117.6(3) . . ? C16 C17 H17 121.2 . . ? C18 C17 H17 121.2 . . ? C17 C16 C15 120.9(2) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C15 C14 118.4(3) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? N2 C14 C15 121.4(2) . . ? N2 C14 C13 116.09(19) . . ? C15 C14 C13 122.5(2) . . ? N1 C13 C14 112.52(19) . . ? N1 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N1 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C5 C6 C1 120.0(2) . . ? C5 C6 N1 118.7(2) . . ? C1 C6 N1 121.38(19) . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C3 C4 C5 120.0(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C2 C1 121.2(3) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C6 C1 C2 118.2(2) . . ? C6 C1 C7 123.2(2) . . ? C2 C1 C7 118.5(2) . . ? C12 C7 C8 117.5(2) . . ? C12 C7 C1 124.6(2) . . ? C8 C7 C1 117.9(2) . . ? C9 C8 C7 122.4(3) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C10 C9 C8 118.8(3) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 120.7(2) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 120.2(2) . . ? C11 C12 N5 118.0(2) . . ? C7 C12 N5 121.71(19) . . ? N5 C22 C23 112.51(19) . . ? N5 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? N5 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? N6 C23 C24 120.7(2) . . ? N6 C23 C22 116.98(19) . . ? C24 C23 C22 122.4(2) . . ? C25 C24 C23 118.6(2) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C26 C25 C24 120.9(2) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 116.8(2) . . ? C25 C26 H26 121.6 . . ? C27 C26 H26 121.6 . . ? N6 C27 C26 123.5(2) . . ? N6 C27 N7 113.75(18) . . ? C26 C27 N7 122.8(2) . . ? C29 C28 N7 107.1(2) . . ? C29 C28 H28 126.5 . . ? N7 C28 H28 126.5 . . ? C28 C29 C30 105.8(3) . . ? C28 C29 H29 127.1 . . ? C30 C29 H29 127.1 . . ? N8 C30 C29 111.6(2) . . ? N8 C30 H30 124.2 . . ? C29 C30 H30 124.2 . . ? C21 N4 N3 104.1(2) . . ? C21 N4 Fe1 141.5(2) . . ? N3 N4 Fe1 113.92(14) . . ? C19 N3 N4 111.6(2) . . ? C19 N3 C18 129.9(2) . . ? N4 N3 C18 118.39(18) . . ? C18 N2 C14 118.78(19) . . ? C18 N2 Fe1 119.87(15) . . ? C14 N2 Fe1 121.32(15) . . ? C6 N1 C13 115.17(19) . . ? C6 N1 Fe1 115.08(14) . . ? C13 N1 Fe1 113.76(14) . . ? C6 N1 H1N 106.6(17) . . ? C13 N1 H1N 106.4(17) . . ? Fe1 N1 H1N 97.5(18) . . ? C30 N8 N7 104.2(2) . . ? C30 N8 Fe1 141.73(18) . . ? N7 N8 Fe1 113.79(13) . . ? C28 N7 N8 111.3(2) . . ? C28 N7 C27 130.6(2) . . ? N8 N7 C27 118.06(18) . . ? C27 N6 C23 119.56(19) . . ? C27 N6 Fe1 119.30(15) . . ? C23 N6 Fe1 120.96(15) . . ? C12 N5 C22 116.17(19) . . ? C12 N5 Fe1 111.28(14) . . ? C22 N5 Fe1 113.45(14) . . ? C12 N5 H5N 112.2(16) . . ? C22 N5 H5N 105.0(16) . . ? Fe1 N5 H5N 96.8(17) . . ? F1 B1 F4 112.1(9) . . ? F1 B1 F3 113.9(9) . . ? F4 B1 F3 103.5(9) . . ? F1 B1 F2 114.5(10) . . ? F4 B1 F2 109.3(9) . . ? F3 B1 F2 102.6(8) . . ? F3' B1' F2' 106.0(13) . . ? F3' B1' F4' 118.1(12) . . ? F2' B1' F4' 117.0(14) . . ? F3' B1' F1' 105.3(12) . . ? F2' B1' F1' 107.3(10) . . ? F4' B1' F1' 102.0(12) . . ? N6 Fe1 N2 168.39(7) . . ? N6 Fe1 N8 74.44(7) . . ? N2 Fe1 N8 109.91(7) . . ? N6 Fe1 N4 117.28(7) . . ? N2 Fe1 N4 73.66(7) . . ? N8 Fe1 N4 94.28(8) . . ? N6 Fe1 N5 75.95(7) . . ? N2 Fe1 N5 100.02(7) . . ? N8 Fe1 N5 150.04(7) . . ? N4 Fe1 N5 95.23(8) . . ? N6 Fe1 N1 93.91(7) . . ? N2 Fe1 N1 75.37(7) . . ? N8 Fe1 N1 92.38(7) . . ? N4 Fe1 N1 148.76(7) . . ? N5 Fe1 N1 94.03(8) . . ? F6 B2 F8 111.3(11) . . ? F6 B2 F7 115.4(17) . . ? F8 B2 F7 104.8(11) . . ? F6 B2 F5 110.2(11) . . ? F8 B2 F5 114.7(15) . . ? F7 B2 F5 100.0(13) . . ? F5' B2' F8' 106.2(7) . . ? F5' B2' F6' 110.9(9) . . ? F8' B2' F6' 108.5(7) . . ? F5' B2' F7' 115.9(8) . . ? F8' B2' F7' 112.2(7) . . ? F6' B2' F7' 103.0(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 N4 C21 C20 C19 -0.1(4) . . . . ? C21 C20 C19 N3 0.0(3) . . . . ? N2 C18 C17 C16 0.8(4) . . . . ? N3 C18 C17 C16 -178.8(2) . . . . ? C18 C17 C16 C15 -0.7(4) . . . . ? C17 C16 C15 C14 -0.8(4) . . . . ? C16 C15 C14 N2 2.4(4) . . . . ? C16 C15 C14 C13 -175.9(2) . . . . ? N2 C14 C13 N1 10.5(3) . . . . ? C15 C14 C13 N1 -171.2(2) . . . . ? C1 C6 C5 C4 -0.8(4) . . . . ? N1 C6 C5 C4 -179.5(2) . . . . ? C6 C5 C4 C3 -0.9(4) . . . . ? C5 C4 C3 C2 1.2(5) . . . . ? C4 C3 C2 C1 0.1(4) . . . . ? C5 C6 C1 C2 2.1(3) . . . . ? N1 C6 C1 C2 -179.3(2) . . . . ? C5 C6 C1 C7 178.1(2) . . . . ? N1 C6 C1 C7 -3.2(3) . . . . ? C3 C2 C1 C6 -1.8(4) . . . . ? C3 C2 C1 C7 -178.0(2) . . . . ? C6 C1 C7 C12 66.2(3) . . . . ? C2 C1 C7 C12 -117.8(3) . . . . ? C6 C1 C7 C8 -113.0(3) . . . . ? C2 C1 C7 C8 63.1(3) . . . . ? C12 C7 C8 C9 -3.6(4) . . . . ? C1 C7 C8 C9 175.6(2) . . . . ? C7 C8 C9 C10 -0.1(4) . . . . ? C8 C9 C10 C11 2.8(4) . . . . ? C9 C10 C11 C12 -1.7(4) . . . . ? C10 C11 C12 C7 -2.2(4) . . . . ? C10 C11 C12 N5 -179.9(2) . . . . ? C8 C7 C12 C11 4.6(3) . . . . ? C1 C7 C12 C11 -174.5(2) . . . . ? C8 C7 C12 N5 -177.7(2) . . . . ? C1 C7 C12 N5 3.2(3) . . . . ? N5 C22 C23 N6 -1.0(3) . . . . ? N5 C22 C23 C24 179.6(2) . . . . ? N6 C23 C24 C25 0.7(4) . . . . ? C22 C23 C24 C25 -179.9(2) . . . . ? C23 C24 C25 C26 1.3(4) . . . . ? C24 C25 C26 C27 -2.3(4) . . . . ? C25 C26 C27 N6 1.4(4) . . . . ? C25 C26 C27 N7 -179.7(2) . . . . ? N7 C28 C29 C30 0.5(3) . . . . ? C28 C29 C30 N8 -0.6(3) . . . . ? C20 C21 N4 N3 0.1(3) . . . . ? C20 C21 N4 Fe1 170.6(2) . . . . ? C20 C19 N3 N4 0.0(3) . . . . ? C20 C19 N3 C18 175.3(2) . . . . ? C21 N4 N3 C19 -0.1(3) . . . . ? Fe1 N4 N3 C19 -173.61(17) . . . . ? C21 N4 N3 C18 -176.0(2) . . . . ? Fe1 N4 N3 C18 10.5(2) . . . . ? N2 C18 N3 C19 176.4(2) . . . . ? C17 C18 N3 C19 -4.0(4) . . . . ? N2 C18 N3 N4 -8.6(3) . . . . ? C17 C18 N3 N4 171.0(2) . . . . ? C17 C18 N2 C14 0.7(3) . . . . ? N3 C18 N2 C14 -179.67(19) . . . . ? C17 C18 N2 Fe1 -177.28(17) . . . . ? N3 C18 N2 Fe1 2.4(3) . . . . ? C15 C14 N2 C18 -2.3(3) . . . . ? C13 C14 N2 C18 176.1(2) . . . . ? C15 C14 N2 Fe1 175.63(17) . . . . ? C13 C14 N2 Fe1 -6.0(3) . . . . ? C5 C6 N1 C13 -115.6(2) . . . . ? C1 C6 N1 C13 65.7(3) . . . . ? C5 C6 N1 Fe1 109.0(2) . . . . ? C1 C6 N1 Fe1 -69.7(2) . . . . ? C14 C13 N1 C6 -146.0(2) . . . . ? C14 C13 N1 Fe1 -10.1(2) . . . . ? C29 C30 N8 N7 0.5(3) . . . . ? C29 C30 N8 Fe1 173.0(2) . . . . ? C29 C28 N7 N8 -0.2(3) . . . . ? C29 C28 N7 C27 175.9(2) . . . . ? C30 N8 N7 C28 -0.2(3) . . . . ? Fe1 N8 N7 C28 -175.11(16) . . . . ? C30 N8 N7 C27 -176.9(2) . . . . ? Fe1 N8 N7 C27 8.2(2) . . . . ? N6 C27 N7 C28 -179.5(2) . . . . ? C26 C27 N7 C28 1.6(4) . . . . ? N6 C27 N7 N8 -3.6(3) . . . . ? C26 C27 N7 N8 177.5(2) . . . . ? C26 C27 N6 C23 0.5(3) . . . . ? N7 C27 N6 C23 -178.42(19) . . . . ? C26 C27 N6 Fe1 175.75(19) . . . . ? N7 C27 N6 Fe1 -3.2(2) . . . . ? C24 C23 N6 C27 -1.6(3) . . . . ? C22 C23 N6 C27 179.0(2) . . . . ? C24 C23 N6 Fe1 -176.76(18) . . . . ? C22 C23 N6 Fe1 3.8(3) . . . . ? C11 C12 N5 C22 -125.5(2) . . . . ? C7 C12 N5 C22 56.8(3) . . . . ? C11 C12 N5 Fe1 102.6(2) . . . . ? C7 C12 N5 Fe1 -75.1(2) . . . . ? C23 C22 N5 C12 -132.8(2) . . . . ? C23 C22 N5 Fe1 -2.0(2) . . . . ? C27 N6 Fe1 N2 -108.0(3) . . . . ? C23 N6 Fe1 N2 67.2(4) . . . . ? C27 N6 Fe1 N8 5.65(16) . . . . ? C23 N6 Fe1 N8 -179.16(17) . . . . ? C27 N6 Fe1 N4 92.42(17) . . . . ? C23 N6 Fe1 N4 -92.39(17) . . . . ? C27 N6 Fe1 N5 -178.92(17) . . . . ? C23 N6 Fe1 N5 -3.73(16) . . . . ? C27 N6 Fe1 N1 -85.73(17) . . . . ? C23 N6 Fe1 N1 89.45(17) . . . . ? C18 N2 Fe1 N6 -158.9(3) . . . . ? C14 N2 Fe1 N6 23.2(4) . . . . ? C18 N2 Fe1 N8 90.91(17) . . . . ? C14 N2 Fe1 N8 -86.98(17) . . . . ? C18 N2 Fe1 N4 2.25(16) . . . . ? C14 N2 Fe1 N4 -175.64(18) . . . . ? C18 N2 Fe1 N5 -90.31(17) . . . . ? C14 N2 Fe1 N5 91.80(17) . . . . ? C18 N2 Fe1 N1 178.11(17) . . . . ? C14 N2 Fe1 N1 0.21(16) . . . . ? C30 N8 Fe1 N6 -179.1(3) . . . . ? N7 N8 Fe1 N6 -7.11(14) . . . . ? C30 N8 Fe1 N2 -10.4(3) . . . . ? N7 N8 Fe1 N2 161.59(14) . . . . ? C30 N8 Fe1 N4 63.7(3) . . . . ? N7 N8 Fe1 N4 -124.25(14) . . . . ? C30 N8 Fe1 N5 172.0(2) . . . . ? N7 N8 Fe1 N5 -16.0(2) . . . . ? C30 N8 Fe1 N1 -85.7(3) . . . . ? N7 N8 Fe1 N1 86.29(15) . . . . ? C21 N4 Fe1 N6 -0.7(3) . . . . ? N3 N4 Fe1 N6 169.24(14) . . . . ? C21 N4 Fe1 N2 -176.5(3) . . . . ? N3 N4 Fe1 N2 -6.56(14) . . . . ? C21 N4 Fe1 N8 74.0(3) . . . . ? N3 N4 Fe1 N8 -116.07(15) . . . . ? C21 N4 Fe1 N5 -77.5(3) . . . . ? N3 N4 Fe1 N5 92.37(16) . . . . ? C21 N4 Fe1 N1 175.8(2) . . . . ? N3 N4 Fe1 N1 -14.3(2) . . . . ? C12 N5 Fe1 N6 136.10(16) . . . . ? C22 N5 Fe1 N6 2.88(15) . . . . ? C12 N5 Fe1 N2 -32.76(16) . . . . ? C22 N5 Fe1 N2 -165.99(16) . . . . ? C12 N5 Fe1 N8 144.95(15) . . . . ? C22 N5 Fe1 N8 11.7(3) . . . . ? C12 N5 Fe1 N4 -107.05(15) . . . . ? C22 N5 Fe1 N4 119.72(16) . . . . ? C12 N5 Fe1 N1 43.08(15) . . . . ? C22 N5 Fe1 N1 -90.15(16) . . . . ? C6 N1 Fe1 N6 -33.92(16) . . . . ? C13 N1 Fe1 N6 -169.90(16) . . . . ? C6 N1 Fe1 N2 141.56(16) . . . . ? C13 N1 Fe1 N2 5.58(15) . . . . ? C6 N1 Fe1 N8 -108.48(16) . . . . ? C13 N1 Fe1 N8 115.55(16) . . . . ? C6 N1 Fe1 N4 149.24(16) . . . . ? C13 N1 Fe1 N4 13.3(2) . . . . ? C6 N1 Fe1 N5 42.24(16) . . . . ? C13 N1 Fe1 N5 -93.73(16) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.306 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.045 data_sh264 _database_code_depnum_ccdc_archive 'CCDC 895363' #TrackingRef 'sh264.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H26 N8 Zn, 2(B F4)' _chemical_formula_sum 'C30 H26 B2 F8 N8 Zn' _chemical_formula_weight 737.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 20.6854(5) _cell_length_b 12.8812(2) _cell_length_c 23.2003(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.953(2) _cell_angle_gamma 90.00 _cell_volume 6069.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100 _cell_measurement_reflns_used 7533 _cell_measurement_theta_min 2.9244 _cell_measurement_theta_max 28.0702 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_T_min 0.88638 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _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 'oxford gemini s' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time 5 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25179 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10665 _reflns_number_gt 8172 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.6856P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10665 _refine_ls_number_parameters 899 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.013 _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 C21 C 1.03733(15) 0.0074(2) 0.09480(13) 0.0285(7) Uani 1 1 d . . . H1 H 1.0102 -0.0087 0.0591 0.034 Uiso 1 1 calc R . . C20 C 1.09461(16) -0.0474(2) 0.11910(15) 0.0377(8) Uani 1 1 d . . . H2 H 1.1121 -0.1049 0.1033 0.045 Uiso 1 1 calc R . . C19 C 1.11926(15) 0.0010(2) 0.17055(15) 0.0335(8) Uani 1 1 d . . . H3 H 1.1572 -0.0172 0.1970 0.040 Uiso 1 1 calc R . . C18 C 1.07747(13) 0.14990(19) 0.22329(12) 0.0214(6) Uani 1 1 d . . . C17 C 1.12256(14) 0.1454(2) 0.27566(13) 0.0277(7) Uani 1 1 d . . . H5 H 1.1563 0.0965 0.2819 0.033 Uiso 1 1 calc R . . C16 C 1.11510(15) 0.2168(2) 0.31807(13) 0.0320(8) Uani 1 1 d . . . H6 H 1.1440 0.2162 0.3540 0.038 Uiso 1 1 calc R . . C15 C 1.06497(14) 0.2896(2) 0.30770(12) 0.0260(7) Uani 1 1 d . . . H7 H 1.0596 0.3372 0.3365 0.031 Uiso 1 1 calc R . . C14 C 1.02297(14) 0.28996(19) 0.25353(12) 0.0222(6) Uani 1 1 d . . . C13 C 0.96917(14) 0.36887(19) 0.23643(12) 0.0235(6) Uani 1 1 d . . . H9A H 0.9451 0.3765 0.2682 0.028 Uiso 1 1 calc R . . H9B H 0.9887 0.4355 0.2304 0.028 Uiso 1 1 calc R . . C6 C 0.89284(13) 0.42219(19) 0.14486(12) 0.0193(6) Uani 1 1 d . . . C5 C 0.82464(13) 0.4310(2) 0.13447(13) 0.0257(7) Uani 1 1 d . . . H11 H 0.7999 0.3854 0.1526 0.031 Uiso 1 1 calc R . . C4 C 0.79341(14) 0.5075(2) 0.09721(13) 0.0282(7) Uani 1 1 d . . . H12 H 0.7477 0.5121 0.0897 0.034 Uiso 1 1 calc R . . C3 C 0.82988(14) 0.5770(2) 0.07124(13) 0.0266(7) Uani 1 1 d . . . H13 H 0.8090 0.6290 0.0467 0.032 Uiso 1 1 calc R . . C2 C 0.89780(13) 0.5684(2) 0.08214(12) 0.0235(6) Uani 1 1 d . . . H14 H 0.9223 0.6159 0.0650 0.028 Uiso 1 1 calc R . . C1 C 0.93053(13) 0.49058(18) 0.11801(12) 0.0198(6) Uani 1 1 d . . . C7 C 1.00439(13) 0.48852(19) 0.12838(12) 0.0208(6) Uani 1 1 d . . . C8 C 1.03858(14) 0.5736(2) 0.15730(12) 0.0235(6) Uani 1 1 d . . . H17 H 1.0149 0.6298 0.1675 0.028 Uiso 1 1 calc R . . C9 C 1.10673(14) 0.5759(2) 0.17108(12) 0.0268(7) Uani 1 1 d . . . H18 H 1.1284 0.6333 0.1899 0.032 Uiso 1 1 calc R . . C10 C 1.14219(14) 0.4920(2) 0.15661(13) 0.0295(7) Uani 1 1 d . . . H19 H 1.1878 0.4914 0.1675 0.035 Uiso 1 1 calc R . . C11 C 1.11010(14) 0.4096(2) 0.12623(12) 0.0251(7) Uani 1 1 d . . . H20 H 1.1345 0.3546 0.1156 0.030 Uiso 1 1 calc R . . C12 C 1.04189(13) 0.40701(19) 0.11113(12) 0.0201(6) Uani 1 1 d . . . C22 C 0.96750(14) 0.3452(2) 0.02129(12) 0.0251(7) Uani 1 1 d . . . H22A H 0.9910 0.3292 -0.0100 0.030 Uiso 1 1 calc R . . H22B H 0.9585 0.4191 0.0200 0.030 Uiso 1 1 calc R . . C23 C 0.90361(14) 0.28730(19) 0.01079(12) 0.0222(6) Uani 1 1 d . . . C24 C 0.85748(14) 0.2962(2) -0.04085(12) 0.0269(7) Uani 1 1 d . . . H24 H 0.8657 0.3388 -0.0710 0.032 Uiso 1 1 calc R . . C25 C 0.79950(15) 0.2415(2) -0.04714(13) 0.0303(7) Uani 1 1 d . . . H25 H 0.7685 0.2471 -0.0817 0.036 Uiso 1 1 calc R . . C26 C 0.78689(14) 0.1780(2) -0.00210(12) 0.0258(7) Uani 1 1 d . . . H26 H 0.7477 0.1410 -0.0053 0.031 Uiso 1 1 calc R . . C27 C 0.83604(13) 0.17253(19) 0.04801(12) 0.0204(6) Uani 1 1 d . . . C28 C 0.78071(14) 0.0485(2) 0.10635(13) 0.0259(7) Uani 1 1 d . . . H28 H 0.7410 0.0369 0.0808 0.031 Uiso 1 1 calc R . . C29 C 0.80037(14) 0.0045(2) 0.16013(13) 0.0261(7) Uani 1 1 d . . . H29 H 0.7773 -0.0432 0.1786 0.031 Uiso 1 1 calc R . . C30 C 0.86225(14) 0.04579(19) 0.18160(12) 0.0229(6) Uani 1 1 d . . . H30 H 0.8875 0.0294 0.2180 0.027 Uiso 1 1 calc R . . C60 C 0.94398(13) -0.49722(19) 0.39137(12) 0.0233(6) Uani 1 1 d . . . H31 H 0.9658 -0.5258 0.4265 0.028 Uiso 1 1 calc R . . C59 C 0.88309(13) -0.5325(2) 0.35985(13) 0.0247(7) Uani 1 1 d . . . H32 H 0.8579 -0.5871 0.3698 0.030 Uiso 1 1 calc R . . C58 C 0.86885(13) -0.47009(19) 0.31179(12) 0.0213(6) Uani 1 1 d . . . H33 H 0.8316 -0.4736 0.2823 0.026 Uiso 1 1 calc R . . C57 C 0.93063(13) -0.32344(18) 0.27541(12) 0.0174(6) Uani 1 1 d . . . C56 C 0.88895(13) -0.3069(2) 0.22196(12) 0.0221(6) Uani 1 1 d . . . H35 H 0.8516 -0.3474 0.2098 0.027 Uiso 1 1 calc R . . C55 C 0.90567(14) -0.22732(19) 0.18768(12) 0.0236(6) Uani 1 1 d . . . H36 H 0.8792 -0.2132 0.1515 0.028 Uiso 1 1 calc R . . C54 C 0.96152(13) -0.16855(19) 0.20684(12) 0.0220(6) Uani 1 1 d . . . H37 H 0.9731 -0.1157 0.1835 0.026 Uiso 1 1 calc R . . C53 C 0.99988(13) -0.18935(18) 0.26112(12) 0.0181(6) Uani 1 1 d . . . C52 C 1.05937(13) -0.12603(19) 0.28617(12) 0.0228(6) Uani 1 1 d . . . H39A H 1.0886 -0.1239 0.2581 0.027 Uiso 1 1 calc R . . H39B H 1.0457 -0.0554 0.2921 0.027 Uiso 1 1 calc R . . C42 C 1.12297(13) -0.08997(18) 0.38563(11) 0.0185(6) Uani 1 1 d . . . C41 C 1.19088(13) -0.0829(2) 0.40275(12) 0.0234(6) Uani 1 1 d . . . H41 H 1.2179 -0.1283 0.3871 0.028 Uiso 1 1 calc R . . C40 C 1.21850(14) -0.0085(2) 0.44302(13) 0.0273(7) Uani 1 1 d . . . H42 H 1.2640 -0.0039 0.4542 0.033 Uiso 1 1 calc R . . C39 C 1.17862(14) 0.0589(2) 0.46660(12) 0.0262(7) Uani 1 1 d . . . H43 H 1.1971 0.1092 0.4935 0.031 Uiso 1 1 calc R . . C38 C 1.11111(14) 0.05117(19) 0.44988(12) 0.0235(6) Uani 1 1 d . . . H44 H 1.0845 0.0972 0.4656 0.028 Uiso 1 1 calc R . . C37 C 1.08171(13) -0.02378(19) 0.41002(12) 0.0186(6) Uani 1 1 d . . . C31 C 1.00830(13) -0.02607(19) 0.39206(11) 0.0188(6) Uani 1 1 d . . . C32 C 0.97763(14) 0.0611(2) 0.36241(12) 0.0234(6) Uani 1 1 d . . . H47 H 1.0030 0.1192 0.3582 0.028 Uiso 1 1 calc R . . C33 C 0.91077(14) 0.0635(2) 0.33927(12) 0.0245(6) Uani 1 1 d . . . H48 H 0.8917 0.1222 0.3197 0.029 Uiso 1 1 calc R . . C34 C 0.87272(14) -0.0229(2) 0.34572(12) 0.0249(7) Uani 1 1 d . . . H49 H 0.8281 -0.0235 0.3290 0.030 Uiso 1 1 calc R . . C35 C 0.90093(13) -0.1079(2) 0.37690(12) 0.0227(6) Uani 1 1 d . . . H50 H 0.8749 -0.1649 0.3819 0.027 Uiso 1 1 calc R . . C36 C 0.96785(13) -0.10942(19) 0.40096(11) 0.0182(6) Uani 1 1 d . . . C43 C 1.03594(12) -0.18491(19) 0.49183(11) 0.0188(6) Uani 1 1 d . . . H52A H 1.0127 -0.2112 0.5214 0.023 Uiso 1 1 calc R . . H52B H 1.0428 -0.1111 0.4986 0.023 Uiso 1 1 calc R . . C44 C 1.10159(13) -0.23760(18) 0.49892(11) 0.0180(6) Uani 1 1 d . . . C45 C 1.14995(13) -0.22592(19) 0.54884(12) 0.0212(6) Uani 1 1 d . . . H54 H 1.1426 -0.1846 0.5798 0.025 Uiso 1 1 calc R . . C46 C 1.20923(14) -0.27695(19) 0.55156(12) 0.0238(7) Uani 1 1 d . . . H55 H 1.2420 -0.2702 0.5848 0.029 Uiso 1 1 calc R . . C47 C 1.22038(13) -0.33801(19) 0.50529(12) 0.0205(6) Uani 1 1 d . . . H56 H 1.2602 -0.3721 0.5064 0.025 Uiso 1 1 calc R . . C48 C 1.16933(13) -0.34585(18) 0.45726(12) 0.0185(6) Uani 1 1 d . . . C49 C 1.22354(14) -0.46398(19) 0.39522(13) 0.0244(6) Uani 1 1 d . . . H58 H 1.2649 -0.4723 0.4189 0.029 Uiso 1 1 calc R . . C50 C 1.20161(14) -0.5095(2) 0.34206(13) 0.0266(7) Uani 1 1 d . . . H59 H 1.2244 -0.5554 0.3223 0.032 Uiso 1 1 calc R . . C51 C 1.13764(14) -0.47257(19) 0.32364(12) 0.0223(6) Uani 1 1 d . . . H60 H 1.1107 -0.4905 0.2882 0.027 Uiso 1 1 calc R . . B1 B 0.77250(16) 0.2384(2) 0.26018(14) 0.0234(7) Uani 1 1 d . . . B2 B 1.10513(17) 0.1471(2) -0.00454(15) 0.0246(7) Uani 1 1 d . . . B3 B 1.23123(17) -0.2140(3) 0.25904(15) 0.0268(8) Uani 1 1 d . . . B4 B 1.11002(16) -0.6385(2) 0.49174(15) 0.0236(7) Uani 1 1 d . . . N4 N 1.02696(11) 0.08472(16) 0.12920(10) 0.0225(5) Uani 1 1 d . . . N3 N 1.07823(11) 0.08101(16) 0.17633(10) 0.0227(5) Uani 1 1 d . . . N2 N 1.02954(11) 0.21956(15) 0.21253(10) 0.0191(5) Uani 1 1 d . . . N1 N 0.92265(11) 0.33880(16) 0.18209(10) 0.0201(5) Uani 1 1 d D . . N5 N 1.01019(11) 0.31947(16) 0.07856(10) 0.0211(5) Uani 1 1 d D . . N6 N 0.89212(11) 0.22457(15) 0.05391(9) 0.0190(5) Uani 1 1 d . . . N7 N 0.82986(11) 0.11254(15) 0.09698(9) 0.0195(5) Uani 1 1 d . . . N8 N 0.88086(11) 0.11115(16) 0.14411(10) 0.0211(5) Uani 1 1 d . . . N16 N 0.96609(10) -0.41823(15) 0.36446(9) 0.0186(5) Uani 1 1 d . . . N15 N 0.91929(10) -0.40166(15) 0.31496(9) 0.0178(5) Uani 1 1 d . . . N14 N 0.98448(10) -0.26758(15) 0.29431(9) 0.0178(5) Uani 1 1 d . . . N13 N 1.09597(11) -0.16750(16) 0.34261(10) 0.0195(5) Uani 1 1 d D . . N9 N 0.99409(11) -0.20088(16) 0.43257(10) 0.0174(5) Uani 1 1 d D . . N10 N 1.11146(10) -0.29871(15) 0.45483(9) 0.0172(5) Uani 1 1 d . . . N11 N 1.17366(11) -0.40422(15) 0.40708(9) 0.0193(5) Uani 1 1 d . . . N12 N 1.11993(11) -0.40924(15) 0.36246(9) 0.0188(5) Uani 1 1 d . . . F1 F 0.83827(8) 0.25144(12) 0.25297(7) 0.0334(4) Uani 1 1 d . . . F2 F 0.73037(10) 0.26843(17) 0.21047(9) 0.0630(6) Uani 1 1 d . . . F3 F 0.76191(8) 0.13355(12) 0.27066(8) 0.0384(5) Uani 1 1 d . . . F4 F 0.76310(10) 0.29312(14) 0.30827(9) 0.0536(5) Uani 1 1 d . . . F5 F 1.12520(9) 0.04447(12) -0.00079(8) 0.0417(5) Uani 1 1 d . . . F6 F 1.12536(9) 0.19238(13) -0.05147(8) 0.0457(5) Uani 1 1 d . . . F7 F 1.13318(9) 0.19827(15) 0.04689(8) 0.0532(6) Uani 1 1 d . . . F8 F 1.03737(8) 0.15476(13) -0.00980(8) 0.0406(5) Uani 1 1 d . . . F9 F 1.22053(8) -0.10805(11) 0.26781(7) 0.0366(4) Uani 1 1 d . . . F10 F 1.18038(9) -0.26877(12) 0.27681(9) 0.0450(5) Uani 1 1 d . . . F11 F 1.29002(10) -0.24316(16) 0.29212(9) 0.0627(6) Uani 1 1 d . . . F12 F 1.22933(9) -0.23289(14) 0.19990(8) 0.0467(5) Uani 1 1 d . . . F13 F 1.04291(8) -0.62199(13) 0.48797(9) 0.0442(5) Uani 1 1 d . . . F14 F 1.13010(8) -0.70985(12) 0.53665(8) 0.0360(4) Uani 1 1 d . . . F15 F 1.12320(10) -0.67725(15) 0.44018(8) 0.0554(6) Uani 1 1 d . . . F16 F 1.14388(8) -0.54639(11) 0.50506(8) 0.0349(4) Uani 1 1 d . . . Zn1 Zn 0.961130(15) 0.21163(2) 0.132544(13) 0.01816(9) Uani 1 1 d . . . Zn2 Zn 1.043272(15) -0.30387(2) 0.375957(13) 0.01726(9) Uani 1 1 d . . . H9N H 0.9619(10) -0.2401(17) 0.4386(11) 0.016(7) Uiso 1 1 d D . . H5N H 1.0410(11) 0.2755(17) 0.0723(12) 0.021(8) Uiso 1 1 d D . . H13N H 1.1294(10) -0.2034(17) 0.3335(11) 0.019(8) Uiso 1 1 d D . . H1N H 0.8900(11) 0.3010(17) 0.1937(11) 0.022(8) Uiso 1 1 d 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 C21 0.042(2) 0.0203(14) 0.0270(17) -0.0012(13) 0.0167(14) -0.0016(14) C20 0.052(2) 0.0253(15) 0.045(2) 0.0060(15) 0.0324(17) 0.0095(16) C19 0.0349(19) 0.0299(15) 0.042(2) 0.0163(15) 0.0227(15) 0.0145(15) C18 0.0150(15) 0.0218(13) 0.0279(16) 0.0050(12) 0.0053(12) -0.0035(12) C17 0.0165(16) 0.0325(15) 0.0329(18) 0.0106(14) 0.0021(12) -0.0034(13) C16 0.0258(17) 0.0411(17) 0.0258(17) 0.0086(15) -0.0035(13) -0.0134(15) C15 0.0338(18) 0.0264(14) 0.0183(15) -0.0012(12) 0.0062(13) -0.0130(14) C14 0.0254(16) 0.0206(13) 0.0217(15) 0.0001(12) 0.0070(12) -0.0088(12) C13 0.0293(17) 0.0209(13) 0.0210(15) -0.0024(12) 0.0071(12) -0.0027(13) C6 0.0172(15) 0.0183(13) 0.0231(15) -0.0028(12) 0.0058(11) 0.0019(12) C5 0.0202(16) 0.0262(14) 0.0322(17) -0.0021(13) 0.0088(13) -0.0019(13) C4 0.0188(16) 0.0346(16) 0.0315(18) -0.0024(14) 0.0058(13) 0.0033(13) C3 0.0243(17) 0.0257(14) 0.0301(17) 0.0032(13) 0.0055(13) 0.0056(13) C2 0.0249(17) 0.0212(13) 0.0267(16) 0.0007(12) 0.0104(12) 0.0000(13) C1 0.0205(15) 0.0163(12) 0.0238(16) -0.0041(12) 0.0072(12) 0.0028(12) C7 0.0202(16) 0.0225(13) 0.0219(15) 0.0055(12) 0.0090(12) 0.0002(12) C8 0.0269(17) 0.0205(13) 0.0249(16) 0.0021(12) 0.0097(12) 0.0015(13) C9 0.0250(17) 0.0298(15) 0.0253(17) 0.0048(13) 0.0045(12) -0.0068(13) C10 0.0156(16) 0.0382(17) 0.0329(18) 0.0098(14) 0.0004(13) 0.0006(14) C11 0.0218(16) 0.0256(14) 0.0301(17) 0.0056(13) 0.0105(12) 0.0082(13) C12 0.0184(15) 0.0219(13) 0.0216(15) 0.0058(12) 0.0078(11) 0.0028(12) C22 0.0347(18) 0.0241(14) 0.0188(15) 0.0028(12) 0.0108(12) 0.0014(13) C23 0.0286(17) 0.0213(13) 0.0191(15) -0.0004(12) 0.0105(12) 0.0088(13) C24 0.0336(18) 0.0295(15) 0.0182(15) 0.0068(13) 0.0067(13) 0.0098(14) C25 0.0321(19) 0.0355(16) 0.0218(16) -0.0002(13) 0.0010(13) 0.0150(15) C26 0.0191(16) 0.0298(15) 0.0276(17) -0.0044(13) 0.0019(12) 0.0070(13) C27 0.0226(16) 0.0190(13) 0.0200(15) -0.0020(12) 0.0051(12) 0.0051(12) C28 0.0191(16) 0.0269(14) 0.0319(18) -0.0059(13) 0.0053(13) -0.0036(13) C29 0.0274(17) 0.0212(14) 0.0333(18) -0.0018(13) 0.0148(13) -0.0042(13) C30 0.0299(17) 0.0190(13) 0.0209(15) 0.0017(12) 0.0077(12) 0.0020(13) C60 0.0260(17) 0.0211(13) 0.0236(16) 0.0038(12) 0.0070(12) 0.0036(13) C59 0.0222(16) 0.0193(13) 0.0343(18) 0.0008(13) 0.0094(13) -0.0041(12) C58 0.0148(15) 0.0221(13) 0.0271(16) -0.0005(12) 0.0039(12) -0.0048(12) C57 0.0161(15) 0.0169(12) 0.0203(15) -0.0013(11) 0.0063(11) 0.0011(11) C56 0.0200(15) 0.0257(14) 0.0197(15) -0.0012(12) 0.0016(11) 0.0006(12) C55 0.0250(16) 0.0269(14) 0.0177(15) -0.0002(12) 0.0011(12) 0.0073(13) C54 0.0259(17) 0.0209(13) 0.0199(15) 0.0030(12) 0.0064(12) 0.0029(13) C53 0.0193(15) 0.0155(12) 0.0217(15) 0.0011(11) 0.0095(11) 0.0035(11) C52 0.0264(17) 0.0217(14) 0.0210(15) 0.0023(12) 0.0065(12) -0.0009(12) C42 0.0182(15) 0.0174(12) 0.0204(15) 0.0031(11) 0.0049(11) -0.0045(12) C41 0.0212(16) 0.0229(14) 0.0273(17) 0.0024(12) 0.0074(12) 0.0016(12) C40 0.0181(16) 0.0346(16) 0.0282(17) 0.0006(14) 0.0017(12) -0.0071(13) C39 0.0287(17) 0.0239(14) 0.0249(17) -0.0057(13) 0.0023(13) -0.0075(13) C38 0.0274(17) 0.0182(13) 0.0265(16) -0.0014(12) 0.0095(12) 0.0031(12) C37 0.0168(15) 0.0186(13) 0.0210(15) 0.0017(11) 0.0054(11) -0.0016(12) C31 0.0196(15) 0.0211(13) 0.0171(15) -0.0025(11) 0.0073(11) 0.0011(12) C32 0.0269(17) 0.0211(13) 0.0235(16) 0.0013(12) 0.0081(12) -0.0006(13) C33 0.0279(17) 0.0250(14) 0.0216(16) 0.0031(12) 0.0070(12) 0.0075(13) C34 0.0180(15) 0.0352(16) 0.0216(16) -0.0017(13) 0.0039(12) 0.0047(13) C35 0.0216(16) 0.0250(14) 0.0228(15) -0.0014(12) 0.0075(12) -0.0036(12) C36 0.0200(15) 0.0197(13) 0.0154(14) 0.0002(11) 0.0043(11) 0.0030(12) C43 0.0211(15) 0.0206(13) 0.0159(14) 0.0000(11) 0.0065(11) 0.0002(12) C44 0.0217(15) 0.0167(12) 0.0164(14) 0.0048(11) 0.0058(11) -0.0030(11) C45 0.0238(16) 0.0206(13) 0.0194(15) -0.0033(12) 0.0045(12) -0.0031(12) C46 0.0219(16) 0.0253(14) 0.0219(16) 0.0021(12) -0.0018(12) -0.0074(13) C47 0.0147(15) 0.0210(13) 0.0258(16) 0.0021(12) 0.0039(11) -0.0005(12) C48 0.0191(15) 0.0158(12) 0.0218(15) 0.0020(11) 0.0066(11) -0.0030(12) C49 0.0187(16) 0.0231(13) 0.0331(18) 0.0033(13) 0.0093(13) 0.0030(12) C50 0.0287(18) 0.0232(14) 0.0317(18) -0.0041(13) 0.0154(13) 0.0011(13) C51 0.0284(17) 0.0186(13) 0.0227(16) -0.0024(12) 0.0114(12) -0.0038(12) B1 0.0212(18) 0.0278(17) 0.0213(18) -0.0010(14) 0.0043(14) 0.0026(15) B2 0.026(2) 0.0241(16) 0.0244(19) 0.0028(14) 0.0060(14) 0.0025(15) B3 0.0226(19) 0.0320(18) 0.0268(19) 0.0021(15) 0.0073(14) -0.0039(15) B4 0.0202(18) 0.0243(16) 0.0248(19) -0.0006(14) 0.0006(14) -0.0026(14) N4 0.0247(14) 0.0201(11) 0.0236(13) 0.0024(10) 0.0068(10) -0.0006(10) N3 0.0219(13) 0.0228(11) 0.0251(14) 0.0052(10) 0.0090(10) 0.0027(10) N2 0.0179(13) 0.0203(11) 0.0198(13) 0.0015(10) 0.0056(9) -0.0034(10) N1 0.0214(14) 0.0181(11) 0.0224(13) -0.0001(10) 0.0081(10) -0.0026(10) N5 0.0227(14) 0.0189(11) 0.0230(13) 0.0039(10) 0.0074(10) 0.0041(11) N6 0.0235(13) 0.0171(10) 0.0171(12) 0.0011(9) 0.0057(10) 0.0023(10) N7 0.0193(13) 0.0206(11) 0.0185(13) -0.0024(10) 0.0034(10) -0.0012(10) N8 0.0229(13) 0.0216(11) 0.0180(13) -0.0020(10) 0.0018(10) -0.0034(10) N16 0.0178(12) 0.0183(11) 0.0184(12) 0.0021(9) 0.0005(9) -0.0018(10) N15 0.0172(12) 0.0183(11) 0.0177(12) 0.0007(9) 0.0028(9) 0.0004(10) N14 0.0190(13) 0.0179(10) 0.0172(12) 0.0009(9) 0.0053(9) 0.0007(10) N13 0.0220(13) 0.0188(11) 0.0179(13) -0.0002(10) 0.0039(10) 0.0008(10) N9 0.0155(13) 0.0183(11) 0.0194(12) -0.0009(10) 0.0060(9) -0.0036(10) N10 0.0181(13) 0.0151(10) 0.0194(12) 0.0015(9) 0.0059(9) -0.0014(9) N11 0.0186(13) 0.0187(11) 0.0206(13) -0.0014(10) 0.0036(10) 0.0001(10) N12 0.0203(13) 0.0180(11) 0.0176(12) 0.0008(9) 0.0027(9) -0.0001(10) F1 0.0274(10) 0.0353(9) 0.0408(11) 0.0111(8) 0.0150(8) 0.0017(8) F2 0.0421(13) 0.0896(15) 0.0507(14) 0.0377(12) -0.0079(10) 0.0000(11) F3 0.0311(11) 0.0288(9) 0.0570(13) 0.0014(8) 0.0130(8) -0.0018(8) F4 0.0515(13) 0.0565(12) 0.0595(14) -0.0305(11) 0.0279(10) -0.0089(10) F5 0.0531(13) 0.0265(8) 0.0523(13) 0.0098(8) 0.0274(9) 0.0122(8) F6 0.0510(13) 0.0486(11) 0.0409(12) 0.0209(9) 0.0175(9) 0.0093(9) F7 0.0448(13) 0.0659(13) 0.0447(13) -0.0269(10) -0.0021(9) 0.0013(10) F8 0.0245(10) 0.0457(10) 0.0515(12) -0.0102(9) 0.0070(8) 0.0031(8) F9 0.0402(11) 0.0272(8) 0.0397(11) 0.0039(8) 0.0008(8) -0.0082(8) F10 0.0630(14) 0.0271(8) 0.0578(13) -0.0109(9) 0.0441(10) -0.0135(9) F11 0.0458(13) 0.0784(14) 0.0559(14) -0.0231(12) -0.0110(10) 0.0266(12) F12 0.0528(13) 0.0621(12) 0.0278(11) -0.0072(9) 0.0141(9) -0.0248(10) F13 0.0221(10) 0.0423(10) 0.0645(14) 0.0160(9) -0.0008(9) 0.0007(8) F14 0.0305(10) 0.0344(9) 0.0423(11) 0.0203(8) 0.0050(8) 0.0008(8) F15 0.0746(16) 0.0617(12) 0.0294(11) -0.0134(10) 0.0085(10) -0.0030(11) F16 0.0354(11) 0.0260(8) 0.0430(11) 0.0026(8) 0.0066(8) -0.0097(8) Zn1 0.01975(18) 0.01847(16) 0.01618(17) 0.00084(13) 0.00319(13) 0.00010(13) Zn2 0.01750(18) 0.01808(15) 0.01583(17) 0.00072(13) 0.00226(12) -0.00082(13) _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 C21 N4 1.319(3) . ? C21 C20 1.402(4) . ? C21 H1 0.9300 . ? C20 C19 1.358(4) . ? C20 H2 0.9300 . ? C19 N3 1.358(3) . ? C19 H3 0.9300 . ? C18 N2 1.325(3) . ? C18 C17 1.385(4) . ? C18 N3 1.408(3) . ? C17 C16 1.377(4) . ? C17 H5 0.9300 . ? C16 C15 1.384(4) . ? C16 H6 0.9300 . ? C15 C14 1.385(4) . ? C15 H7 0.9300 . ? C14 N2 1.340(3) . ? C14 C13 1.504(4) . ? C13 N1 1.485(3) . ? C13 H9A 0.9700 . ? C13 H9B 0.9700 . ? C6 C5 1.390(4) . ? C6 C1 1.399(4) . ? C6 N1 1.441(3) . ? C5 C4 1.387(4) . ? C5 H11 0.9300 . ? C4 C3 1.380(4) . ? C4 H12 0.9300 . ? C3 C2 1.384(4) . ? C3 H13 0.9300 . ? C2 C1 1.393(4) . ? C2 H14 0.9300 . ? C1 C7 1.501(4) . ? C7 C8 1.404(4) . ? C7 C12 1.408(4) . ? C8 C9 1.385(4) . ? C8 H17 0.9300 . ? C9 C10 1.382(4) . ? C9 H18 0.9300 . ? C10 C11 1.373(4) . ? C10 H19 0.9300 . ? C11 C12 1.388(4) . ? C11 H20 0.9300 . ? C12 N5 1.444(3) . ? C22 N5 1.486(3) . ? C22 C23 1.497(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N6 1.342(3) . ? C23 C24 1.387(4) . ? C24 C25 1.374(4) . ? C24 H24 0.9300 . ? C25 C26 1.391(4) . ? C25 H25 0.9300 . ? C26 C27 1.393(4) . ? C26 H26 0.9300 . ? C27 N6 1.324(3) . ? C27 N7 1.400(3) . ? C28 N7 1.358(3) . ? C28 C29 1.361(4) . ? C28 H28 0.9300 . ? C29 C30 1.388(4) . ? C29 H29 0.9300 . ? C30 N8 1.319(3) . ? C30 H30 0.9300 . ? C60 N16 1.320(3) . ? C60 C59 1.406(4) . ? C60 H31 0.9300 . ? C59 C58 1.361(4) . ? C59 H32 0.9300 . ? C58 N15 1.357(3) . ? C58 H33 0.9300 . ? C57 N14 1.329(3) . ? C57 C56 1.386(4) . ? C57 N15 1.412(3) . ? C56 C55 1.381(4) . ? C56 H35 0.9300 . ? C55 C54 1.382(4) . ? C55 H36 0.9300 . ? C54 C53 1.381(4) . ? C54 H37 0.9300 . ? C53 N14 1.343(3) . ? C53 C52 1.499(3) . ? C52 N13 1.482(3) . ? C52 H39A 0.9700 . ? C52 H39B 0.9700 . ? C42 C41 1.388(4) . ? C42 C37 1.400(4) . ? C42 N13 1.447(3) . ? C41 C40 1.383(4) . ? C41 H41 0.9300 . ? C40 C39 1.381(4) . ? C40 H42 0.9300 . ? C39 C38 1.380(4) . ? C39 H43 0.9300 . ? C38 C37 1.394(4) . ? C38 H44 0.9300 . ? C37 C31 1.497(4) . ? C31 C36 1.400(4) . ? C31 C32 1.404(4) . ? C32 C33 1.386(4) . ? C32 H47 0.9300 . ? C33 C34 1.387(4) . ? C33 H48 0.9300 . ? C34 C35 1.380(4) . ? C34 H49 0.9300 . ? C35 C36 1.391(4) . ? C35 H50 0.9300 . ? C36 N9 1.438(3) . ? C43 N9 1.493(3) . ? C43 C44 1.499(4) . ? C43 H52A 0.9700 . ? C43 H52B 0.9700 . ? C44 N10 1.337(3) . ? C44 C45 1.387(4) . ? C45 C46 1.382(4) . ? C45 H54 0.9300 . ? C46 C47 1.385(4) . ? C46 H55 0.9300 . ? C47 C48 1.386(4) . ? C47 H56 0.9300 . ? C48 N10 1.334(3) . ? C48 N11 1.403(3) . ? C49 N11 1.357(3) . ? C49 C50 1.363(4) . ? C49 H58 0.9300 . ? C50 C51 1.395(4) . ? C50 H59 0.9300 . ? C51 N12 1.318(3) . ? C51 H60 0.9300 . ? B1 F2 1.363(4) . ? B1 F4 1.364(4) . ? B1 F3 1.397(3) . ? B1 F1 1.412(4) . ? B2 F6 1.369(4) . ? B2 F5 1.383(3) . ? B2 F8 1.387(4) . ? B2 F7 1.390(4) . ? B3 F11 1.362(4) . ? B3 F12 1.387(4) . ? B3 F10 1.392(4) . ? B3 F9 1.404(4) . ? B4 F15 1.370(4) . ? B4 F16 1.383(3) . ? B4 F13 1.391(4) . ? B4 F14 1.392(3) . ? N4 N3 1.372(3) . ? N4 Zn1 2.138(2) . ? N2 Zn1 2.112(2) . ? N1 Zn1 2.233(2) . ? N1 H1N 0.915(17) . ? N5 Zn1 2.239(2) . ? N5 H5N 0.885(17) . ? N6 Zn1 2.099(2) . ? N7 N8 1.368(3) . ? N8 Zn1 2.162(2) . ? N16 N15 1.371(3) . ? N16 Zn2 2.151(2) . ? N14 Zn2 2.100(2) . ? N13 Zn2 2.279(2) . ? N13 H13N 0.890(17) . ? N9 Zn2 2.242(2) . ? N9 H9N 0.868(16) . ? N10 Zn2 2.089(2) . ? N11 N12 1.369(3) . ? N12 Zn2 2.155(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 C21 C20 111.0(3) . . ? N4 C21 H1 124.5 . . ? C20 C21 H1 124.5 . . ? C19 C20 C21 105.7(3) . . ? C19 C20 H2 127.2 . . ? C21 C20 H2 127.2 . . ? C20 C19 N3 107.3(3) . . ? C20 C19 H3 126.3 . . ? N3 C19 H3 126.3 . . ? N2 C18 C17 123.3(3) . . ? N2 C18 N3 113.5(2) . . ? C17 C18 N3 123.2(3) . . ? C16 C17 C18 116.8(3) . . ? C16 C17 H5 121.6 . . ? C18 C17 H5 121.6 . . ? C17 C16 C15 120.7(3) . . ? C17 C16 H6 119.7 . . ? C15 C16 H6 119.7 . . ? C16 C15 C14 118.7(3) . . ? C16 C15 H7 120.6 . . ? C14 C15 H7 120.6 . . ? N2 C14 C15 120.7(3) . . ? N2 C14 C13 116.1(2) . . ? C15 C14 C13 123.2(3) . . ? N1 C13 C14 112.0(2) . . ? N1 C13 H9A 109.2 . . ? C14 C13 H9A 109.2 . . ? N1 C13 H9B 109.2 . . ? C14 C13 H9B 109.2 . . ? H9A C13 H9B 107.9 . . ? C5 C6 C1 120.3(2) . . ? C5 C6 N1 118.0(2) . . ? C1 C6 N1 121.7(2) . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H11 119.9 . . ? C6 C5 H11 119.9 . . ? C3 C4 C5 120.3(3) . . ? C3 C4 H12 119.9 . . ? C5 C4 H12 119.9 . . ? C4 C3 C2 119.2(3) . . ? C4 C3 H13 120.4 . . ? C2 C3 H13 120.4 . . ? C3 C2 C1 121.9(3) . . ? C3 C2 H14 119.1 . . ? C1 C2 H14 119.1 . . ? C2 C1 C6 118.1(2) . . ? C2 C1 C7 118.2(2) . . ? C6 C1 C7 123.6(2) . . ? C8 C7 C12 117.6(2) . . ? C8 C7 C1 117.9(2) . . ? C12 C7 C1 124.5(2) . . ? C9 C8 C7 121.7(3) . . ? C9 C8 H17 119.2 . . ? C7 C8 H17 119.2 . . ? C10 C9 C8 119.4(3) . . ? C10 C9 H18 120.3 . . ? C8 C9 H18 120.3 . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H19 120.0 . . ? C9 C10 H19 120.0 . . ? C10 C11 C12 121.2(3) . . ? C10 C11 H20 119.4 . . ? C12 C11 H20 119.4 . . ? C11 C12 C7 119.9(2) . . ? C11 C12 N5 119.3(2) . . ? C7 C12 N5 120.8(2) . . ? N5 C22 C23 113.0(2) . . ? N5 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? N5 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? N6 C23 C24 120.2(3) . . ? N6 C23 C22 117.0(2) . . ? C24 C23 C22 122.7(3) . . ? C25 C24 C23 119.5(3) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.4(3) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 116.4(3) . . ? C25 C26 H26 121.8 . . ? C27 C26 H26 121.8 . . ? N6 C27 C26 123.1(3) . . ? N6 C27 N7 114.1(2) . . ? C26 C27 N7 122.7(3) . . ? N7 C28 C29 107.3(2) . . ? N7 C28 H28 126.3 . . ? C29 C28 H28 126.3 . . ? C28 C29 C30 105.3(2) . . ? C28 C29 H29 127.4 . . ? C30 C29 H29 127.4 . . ? N8 C30 C29 111.9(2) . . ? N8 C30 H30 124.1 . . ? C29 C30 H30 124.1 . . ? N16 C60 C59 111.1(2) . . ? N16 C60 H31 124.4 . . ? C59 C60 H31 124.4 . . ? C58 C59 C60 105.5(2) . . ? C58 C59 H32 127.2 . . ? C60 C59 H32 127.2 . . ? N15 C58 C59 107.2(2) . . ? N15 C58 H33 126.4 . . ? C59 C58 H33 126.4 . . ? N14 C57 C56 123.5(2) . . ? N14 C57 N15 113.9(2) . . ? C56 C57 N15 122.6(2) . . ? C55 C56 C57 116.6(3) . . ? C55 C56 H35 121.7 . . ? C57 C56 H35 121.7 . . ? C56 C55 C54 120.4(2) . . ? C56 C55 H36 119.8 . . ? C54 C55 H36 119.8 . . ? C53 C54 C55 119.2(3) . . ? C53 C54 H37 120.4 . . ? C55 C54 H37 120.4 . . ? N14 C53 C54 120.7(2) . . ? N14 C53 C52 116.9(2) . . ? C54 C53 C52 122.4(2) . . ? N13 C52 C53 113.0(2) . . ? N13 C52 H39A 109.0 . . ? C53 C52 H39A 109.0 . . ? N13 C52 H39B 109.0 . . ? C53 C52 H39B 109.0 . . ? H39A C52 H39B 107.8 . . ? C41 C42 C37 120.4(2) . . ? C41 C42 N13 118.7(2) . . ? C37 C42 N13 120.9(2) . . ? C40 C41 C42 120.3(3) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C39 C40 C41 120.1(3) . . ? C39 C40 H42 119.9 . . ? C41 C40 H42 119.9 . . ? C38 C39 C40 119.5(3) . . ? C38 C39 H43 120.3 . . ? C40 C39 H43 120.3 . . ? C39 C38 C37 121.8(3) . . ? C39 C38 H44 119.1 . . ? C37 C38 H44 119.1 . . ? C38 C37 C42 117.9(2) . . ? C38 C37 C31 119.3(2) . . ? C42 C37 C31 122.7(2) . . ? C36 C31 C32 117.3(2) . . ? C36 C31 C37 125.2(2) . . ? C32 C31 C37 117.4(2) . . ? C33 C32 C31 122.2(3) . . ? C33 C32 H47 118.9 . . ? C31 C32 H47 118.9 . . ? C32 C33 C34 119.0(3) . . ? C32 C33 H48 120.5 . . ? C34 C33 H48 120.5 . . ? C35 C34 C33 120.1(3) . . ? C35 C34 H49 120.0 . . ? C33 C34 H49 120.0 . . ? C34 C35 C36 120.7(3) . . ? C34 C35 H50 119.6 . . ? C36 C35 H50 119.6 . . ? C35 C36 C31 120.5(2) . . ? C35 C36 N9 117.8(2) . . ? C31 C36 N9 121.7(2) . . ? N9 C43 C44 113.2(2) . . ? N9 C43 H52A 108.9 . . ? C44 C43 H52A 108.9 . . ? N9 C43 H52B 108.9 . . ? C44 C43 H52B 108.9 . . ? H52A C43 H52B 107.8 . . ? N10 C44 C45 120.8(2) . . ? N10 C44 C43 116.7(2) . . ? C45 C44 C43 122.5(2) . . ? C46 C45 C44 118.6(3) . . ? C46 C45 H54 120.7 . . ? C44 C45 H54 120.7 . . ? C45 C46 C47 120.8(2) . . ? C45 C46 H55 119.6 . . ? C47 C46 H55 119.6 . . ? C46 C47 C48 116.8(3) . . ? C46 C47 H56 121.6 . . ? C48 C47 H56 121.6 . . ? N10 C48 C47 122.8(3) . . ? N10 C48 N11 114.0(2) . . ? C47 C48 N11 123.2(2) . . ? N11 C49 C50 107.0(2) . . ? N11 C49 H58 126.5 . . ? C50 C49 H58 126.5 . . ? C49 C50 C51 105.3(2) . . ? C49 C50 H59 127.4 . . ? C51 C50 H59 127.4 . . ? N12 C51 C50 111.9(2) . . ? N12 C51 H60 124.1 . . ? C50 C51 H60 124.1 . . ? F2 B1 F4 112.2(3) . . ? F2 B1 F3 109.0(2) . . ? F4 B1 F3 107.8(3) . . ? F2 B1 F1 110.0(3) . . ? F4 B1 F1 109.0(2) . . ? F3 B1 F1 108.8(2) . . ? F6 B2 F5 108.9(3) . . ? F6 B2 F8 110.9(2) . . ? F5 B2 F8 111.1(2) . . ? F6 B2 F7 109.9(3) . . ? F5 B2 F7 109.1(2) . . ? F8 B2 F7 107.0(3) . . ? F11 B3 F12 111.3(3) . . ? F11 B3 F10 109.7(3) . . ? F12 B3 F10 108.9(2) . . ? F11 B3 F9 109.6(2) . . ? F12 B3 F9 109.8(2) . . ? F10 B3 F9 107.5(3) . . ? F15 B4 F16 109.3(3) . . ? F15 B4 F13 111.3(2) . . ? F16 B4 F13 109.9(2) . . ? F15 B4 F14 109.4(2) . . ? F16 B4 F14 109.4(2) . . ? F13 B4 F14 107.5(3) . . ? C21 N4 N3 105.4(2) . . ? C21 N4 Zn1 141.0(2) . . ? N3 N4 Zn1 113.51(16) . . ? C19 N3 N4 110.5(2) . . ? C19 N3 C18 130.8(2) . . ? N4 N3 C18 118.3(2) . . ? C18 N2 C14 119.8(2) . . ? C18 N2 Zn1 119.03(18) . . ? C14 N2 Zn1 121.01(18) . . ? C6 N1 C13 116.7(2) . . ? C6 N1 Zn1 113.08(17) . . ? C13 N1 Zn1 113.06(16) . . ? C6 N1 H1N 108.5(16) . . ? C13 N1 H1N 106.5(17) . . ? Zn1 N1 H1N 96.7(16) . . ? C12 N5 C22 115.3(2) . . ? C12 N5 Zn1 113.63(17) . . ? C22 N5 Zn1 112.52(16) . . ? C12 N5 H5N 108.4(17) . . ? C22 N5 H5N 108.7(18) . . ? Zn1 N5 H5N 96.4(17) . . ? C27 N6 C23 120.2(2) . . ? C27 N6 Zn1 119.17(17) . . ? C23 N6 Zn1 120.56(18) . . ? C28 N7 N8 110.6(2) . . ? C28 N7 C27 130.7(2) . . ? N8 N7 C27 118.7(2) . . ? C30 N8 N7 105.0(2) . . ? C30 N8 Zn1 142.29(18) . . ? N7 N8 Zn1 112.76(16) . . ? C60 N16 N15 105.3(2) . . ? C60 N16 Zn2 141.71(18) . . ? N15 N16 Zn2 112.74(15) . . ? C58 N15 N16 110.9(2) . . ? C58 N15 C57 130.5(2) . . ? N16 N15 C57 118.5(2) . . ? C57 N14 C53 119.5(2) . . ? C57 N14 Zn2 118.86(17) . . ? C53 N14 Zn2 121.63(17) . . ? C42 N13 C52 115.22(19) . . ? C42 N13 Zn2 116.40(17) . . ? C52 N13 Zn2 112.38(15) . . ? C42 N13 H13N 107.9(17) . . ? C52 N13 H13N 105.4(17) . . ? Zn2 N13 H13N 97.1(16) . . ? C36 N9 C43 116.95(19) . . ? C36 N9 Zn2 110.80(16) . . ? C43 N9 Zn2 111.88(15) . . ? C36 N9 H9N 109.5(17) . . ? C43 N9 H9N 105.0(18) . . ? Zn2 N9 H9N 101.4(17) . . ? C48 N10 C44 120.1(2) . . ? C48 N10 Zn2 118.28(17) . . ? C44 N10 Zn2 120.88(17) . . ? C49 N11 N12 111.1(2) . . ? C49 N11 C48 130.0(2) . . ? N12 N11 C48 118.8(2) . . ? C51 N12 N11 104.8(2) . . ? C51 N12 Zn2 142.86(19) . . ? N11 N12 Zn2 111.99(16) . . ? N6 Zn1 N2 172.62(8) . . ? N6 Zn1 N4 111.21(8) . . ? N2 Zn1 N4 75.16(8) . . ? N6 Zn1 N8 75.16(8) . . ? N2 Zn1 N8 108.79(8) . . ? N4 Zn1 N8 93.22(8) . . ? N6 Zn1 N1 98.00(8) . . ? N2 Zn1 N1 75.94(8) . . ? N4 Zn1 N1 150.60(8) . . ? N8 Zn1 N1 91.03(8) . . ? N6 Zn1 N5 76.71(8) . . ? N2 Zn1 N5 99.34(8) . . ? N4 Zn1 N5 95.42(9) . . ? N8 Zn1 N5 151.83(8) . . ? N1 Zn1 N5 94.40(8) . . ? N10 Zn2 N14 164.20(8) . . ? N10 Zn2 N16 119.48(8) . . ? N14 Zn2 N16 75.62(8) . . ? N10 Zn2 N12 75.77(8) . . ? N14 Zn2 N12 108.97(8) . . ? N16 Zn2 N12 95.73(8) . . ? N10 Zn2 N9 76.94(8) . . ? N14 Zn2 N9 98.47(8) . . ? N16 Zn2 N9 93.96(8) . . ? N12 Zn2 N9 152.39(8) . . ? N10 Zn2 N13 89.19(8) . . ? N14 Zn2 N13 75.80(8) . . ? N16 Zn2 N13 151.33(8) . . ? N12 Zn2 N13 91.34(8) . . ? N9 Zn2 N13 92.43(8) . . ? 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 N4 C21 C20 C19 -0.3(3) . . . . ? C21 C20 C19 N3 0.0(3) . . . . ? N2 C18 C17 C16 1.2(4) . . . . ? N3 C18 C17 C16 -179.0(2) . . . . ? C18 C17 C16 C15 -0.6(4) . . . . ? C17 C16 C15 C14 -0.8(4) . . . . ? C16 C15 C14 N2 1.8(4) . . . . ? C16 C15 C14 C13 -176.7(3) . . . . ? N2 C14 C13 N1 13.9(3) . . . . ? C15 C14 C13 N1 -167.5(3) . . . . ? C1 C6 C5 C4 0.2(4) . . . . ? N1 C6 C5 C4 -177.6(2) . . . . ? C6 C5 C4 C3 -1.5(4) . . . . ? C5 C4 C3 C2 0.9(4) . . . . ? C4 C3 C2 C1 0.9(4) . . . . ? C3 C2 C1 C6 -2.1(4) . . . . ? C3 C2 C1 C7 -178.8(2) . . . . ? C5 C6 C1 C2 1.6(4) . . . . ? N1 C6 C1 C2 179.3(2) . . . . ? C5 C6 C1 C7 178.0(2) . . . . ? N1 C6 C1 C7 -4.3(4) . . . . ? C2 C1 C7 C8 63.0(3) . . . . ? C6 C1 C7 C8 -113.4(3) . . . . ? C2 C1 C7 C12 -117.1(3) . . . . ? C6 C1 C7 C12 66.5(4) . . . . ? C12 C7 C8 C9 -3.0(4) . . . . ? C1 C7 C8 C9 176.9(2) . . . . ? C7 C8 C9 C10 -0.7(4) . . . . ? C8 C9 C10 C11 3.2(4) . . . . ? C9 C10 C11 C12 -2.1(4) . . . . ? C10 C11 C12 C7 -1.7(4) . . . . ? C10 C11 C12 N5 179.2(3) . . . . ? C8 C7 C12 C11 4.2(4) . . . . ? C1 C7 C12 C11 -175.8(2) . . . . ? C8 C7 C12 N5 -176.8(2) . . . . ? C1 C7 C12 N5 3.2(4) . . . . ? N5 C22 C23 N6 2.4(3) . . . . ? N5 C22 C23 C24 -177.3(2) . . . . ? N6 C23 C24 C25 1.0(4) . . . . ? C22 C23 C24 C25 -179.2(2) . . . . ? C23 C24 C25 C26 0.2(4) . . . . ? C24 C25 C26 C27 -0.8(4) . . . . ? C25 C26 C27 N6 0.3(4) . . . . ? C25 C26 C27 N7 179.3(2) . . . . ? N7 C28 C29 C30 0.4(3) . . . . ? C28 C29 C30 N8 -0.3(3) . . . . ? N16 C60 C59 C58 -0.2(3) . . . . ? C60 C59 C58 N15 0.3(3) . . . . ? N14 C57 C56 C55 -0.2(4) . . . . ? N15 C57 C56 C55 179.6(2) . . . . ? C57 C56 C55 C54 0.1(4) . . . . ? C56 C55 C54 C53 -1.0(4) . . . . ? C55 C54 C53 N14 2.0(4) . . . . ? C55 C54 C53 C52 -177.1(2) . . . . ? N14 C53 C52 N13 5.5(3) . . . . ? C54 C53 C52 N13 -175.3(2) . . . . ? C37 C42 C41 C40 -1.6(4) . . . . ? N13 C42 C41 C40 178.9(2) . . . . ? C42 C41 C40 C39 0.2(4) . . . . ? C41 C40 C39 C38 0.3(4) . . . . ? C40 C39 C38 C37 0.6(4) . . . . ? C39 C38 C37 C42 -1.9(4) . . . . ? C39 C38 C37 C31 -178.0(2) . . . . ? C41 C42 C37 C38 2.4(4) . . . . ? N13 C42 C37 C38 -178.1(2) . . . . ? C41 C42 C37 C31 178.3(2) . . . . ? N13 C42 C37 C31 -2.2(4) . . . . ? C38 C37 C31 C36 -119.3(3) . . . . ? C42 C37 C31 C36 64.9(4) . . . . ? C38 C37 C31 C32 62.7(3) . . . . ? C42 C37 C31 C32 -113.2(3) . . . . ? C36 C31 C32 C33 -4.1(4) . . . . ? C37 C31 C32 C33 174.2(2) . . . . ? C31 C32 C33 C34 0.2(4) . . . . ? C32 C33 C34 C35 2.7(4) . . . . ? C33 C34 C35 C36 -1.6(4) . . . . ? C34 C35 C36 C31 -2.4(4) . . . . ? C34 C35 C36 N9 -179.6(2) . . . . ? C32 C31 C36 C35 5.1(4) . . . . ? C37 C31 C36 C35 -173.0(2) . . . . ? C32 C31 C36 N9 -177.9(2) . . . . ? C37 C31 C36 N9 4.1(4) . . . . ? N9 C43 C44 N10 -6.3(3) . . . . ? N9 C43 C44 C45 174.8(2) . . . . ? N10 C44 C45 C46 1.5(4) . . . . ? C43 C44 C45 C46 -179.7(2) . . . . ? C44 C45 C46 C47 0.4(4) . . . . ? C45 C46 C47 C48 -0.7(4) . . . . ? C46 C47 C48 N10 -0.8(4) . . . . ? C46 C47 C48 N11 179.5(2) . . . . ? N11 C49 C50 C51 0.7(3) . . . . ? C49 C50 C51 N12 -0.7(3) . . . . ? C20 C21 N4 N3 0.4(3) . . . . ? C20 C21 N4 Zn1 176.8(2) . . . . ? C20 C19 N3 N4 0.2(3) . . . . ? C20 C19 N3 C18 173.8(3) . . . . ? C21 N4 N3 C19 -0.4(3) . . . . ? Zn1 N4 N3 C19 -177.93(17) . . . . ? C21 N4 N3 C18 -174.8(2) . . . . ? Zn1 N4 N3 C18 7.6(3) . . . . ? N2 C18 N3 C19 179.4(3) . . . . ? C17 C18 N3 C19 -0.4(5) . . . . ? N2 C18 N3 N4 -7.5(3) . . . . ? C17 C18 N3 N4 172.7(2) . . . . ? C17 C18 N2 C14 -0.2(4) . . . . ? N3 C18 N2 C14 179.9(2) . . . . ? C17 C18 N2 Zn1 -176.5(2) . . . . ? N3 C18 N2 Zn1 3.6(3) . . . . ? C15 C14 N2 C18 -1.3(4) . . . . ? C13 C14 N2 C18 177.3(2) . . . . ? C15 C14 N2 Zn1 174.9(2) . . . . ? C13 C14 N2 Zn1 -6.5(3) . . . . ? C5 C6 N1 C13 -119.4(3) . . . . ? C1 C6 N1 C13 62.8(3) . . . . ? C5 C6 N1 Zn1 106.9(2) . . . . ? C1 C6 N1 Zn1 -70.9(3) . . . . ? C14 C13 N1 C6 -148.2(2) . . . . ? C14 C13 N1 Zn1 -14.6(3) . . . . ? C11 C12 N5 C22 -121.7(3) . . . . ? C7 C12 N5 C22 59.3(3) . . . . ? C11 C12 N5 Zn1 106.3(2) . . . . ? C7 C12 N5 Zn1 -72.7(3) . . . . ? C23 C22 N5 C12 -136.8(2) . . . . ? C23 C22 N5 Zn1 -4.3(3) . . . . ? C26 C27 N6 C23 0.9(4) . . . . ? N7 C27 N6 C23 -178.2(2) . . . . ? C26 C27 N6 Zn1 178.7(2) . . . . ? N7 C27 N6 Zn1 -0.3(3) . . . . ? C24 C23 N6 C27 -1.6(4) . . . . ? C22 C23 N6 C27 178.7(2) . . . . ? C24 C23 N6 Zn1 -179.40(19) . . . . ? C22 C23 N6 Zn1 0.9(3) . . . . ? C29 C28 N7 N8 -0.4(3) . . . . ? C29 C28 N7 C27 176.9(3) . . . . ? N6 C27 N7 C28 -178.6(2) . . . . ? C26 C27 N7 C28 2.3(4) . . . . ? N6 C27 N7 N8 -1.4(3) . . . . ? C26 C27 N7 N8 179.5(2) . . . . ? C29 C30 N8 N7 0.0(3) . . . . ? C29 C30 N8 Zn1 -179.8(2) . . . . ? C28 N7 N8 C30 0.3(3) . . . . ? C27 N7 N8 C30 -177.4(2) . . . . ? C28 N7 N8 Zn1 -179.89(16) . . . . ? C27 N7 N8 Zn1 2.4(3) . . . . ? C59 C60 N16 N15 0.0(3) . . . . ? C59 C60 N16 Zn2 172.8(2) . . . . ? C59 C58 N15 N16 -0.2(3) . . . . ? C59 C58 N15 C57 177.0(3) . . . . ? C60 N16 N15 C58 0.1(3) . . . . ? Zn2 N16 N15 C58 -175.00(16) . . . . ? C60 N16 N15 C57 -177.5(2) . . . . ? Zn2 N16 N15 C57 7.4(3) . . . . ? N14 C57 N15 C58 177.2(2) . . . . ? C56 C57 N15 C58 -2.6(4) . . . . ? N14 C57 N15 N16 -5.8(3) . . . . ? C56 C57 N15 N16 174.4(2) . . . . ? C56 C57 N14 C53 1.2(4) . . . . ? N15 C57 N14 C53 -178.6(2) . . . . ? C56 C57 N14 Zn2 -179.1(2) . . . . ? N15 C57 N14 Zn2 1.1(3) . . . . ? C54 C53 N14 C57 -2.1(4) . . . . ? C52 C53 N14 C57 177.1(2) . . . . ? C54 C53 N14 Zn2 178.24(19) . . . . ? C52 C53 N14 Zn2 -2.6(3) . . . . ? C41 C42 N13 C52 -115.7(3) . . . . ? C37 C42 N13 C52 64.8(3) . . . . ? C41 C42 N13 Zn2 109.6(2) . . . . ? C37 C42 N13 Zn2 -69.9(3) . . . . ? C53 C52 N13 C42 -142.1(2) . . . . ? C53 C52 N13 Zn2 -5.6(3) . . . . ? C35 C36 N9 C43 -130.8(3) . . . . ? C31 C36 N9 C43 52.1(3) . . . . ? C35 C36 N9 Zn2 99.4(2) . . . . ? C31 C36 N9 Zn2 -77.7(3) . . . . ? C44 C43 N9 C36 -127.1(2) . . . . ? C44 C43 N9 Zn2 2.2(3) . . . . ? C47 C48 N10 C44 2.7(4) . . . . ? N11 C48 N10 C44 -177.6(2) . . . . ? C47 C48 N10 Zn2 173.1(2) . . . . ? N11 C48 N10 Zn2 -7.1(3) . . . . ? C45 C44 N10 C48 -3.0(4) . . . . ? C43 C44 N10 C48 178.1(2) . . . . ? C45 C44 N10 Zn2 -173.20(19) . . . . ? C43 C44 N10 Zn2 7.9(3) . . . . ? C50 C49 N11 N12 -0.6(3) . . . . ? C50 C49 N11 C48 176.1(3) . . . . ? N10 C48 N11 C49 -177.8(2) . . . . ? C47 C48 N11 C49 2.0(4) . . . . ? N10 C48 N11 N12 -1.3(3) . . . . ? C47 C48 N11 N12 178.4(2) . . . . ? C50 C51 N12 N11 0.3(3) . . . . ? C50 C51 N12 Zn2 172.0(2) . . . . ? C49 N11 N12 C51 0.1(3) . . . . ? C48 N11 N12 C51 -177.0(2) . . . . ? C49 N11 N12 Zn2 -174.46(16) . . . . ? C48 N11 N12 Zn2 8.5(3) . . . . ? C27 N6 Zn1 N2 -122.1(6) . . . . ? C23 N6 Zn1 N2 55.8(8) . . . . ? C27 N6 Zn1 N4 88.9(2) . . . . ? C23 N6 Zn1 N4 -93.2(2) . . . . ? C27 N6 Zn1 N8 1.22(18) . . . . ? C23 N6 Zn1 N8 179.1(2) . . . . ? C27 N6 Zn1 N1 -87.73(19) . . . . ? C23 N6 Zn1 N1 90.1(2) . . . . ? C27 N6 Zn1 N5 179.6(2) . . . . ? C23 N6 Zn1 N5 -2.52(19) . . . . ? C18 N2 Zn1 N6 -150.0(6) . . . . ? C14 N2 Zn1 N6 33.7(8) . . . . ? C18 N2 Zn1 N4 0.23(19) . . . . ? C14 N2 Zn1 N4 -176.0(2) . . . . ? C18 N2 Zn1 N8 88.6(2) . . . . ? C14 N2 Zn1 N8 -87.7(2) . . . . ? C18 N2 Zn1 N1 174.8(2) . . . . ? C14 N2 Zn1 N1 -1.44(19) . . . . ? C18 N2 Zn1 N5 -92.9(2) . . . . ? C14 N2 Zn1 N5 90.8(2) . . . . ? C21 N4 Zn1 N6 -4.2(3) . . . . ? N3 N4 Zn1 N6 171.97(16) . . . . ? C21 N4 Zn1 N2 179.7(3) . . . . ? N3 N4 Zn1 N2 -4.11(17) . . . . ? C21 N4 Zn1 N8 71.1(3) . . . . ? N3 N4 Zn1 N8 -112.70(18) . . . . ? C21 N4 Zn1 N1 168.9(3) . . . . ? N3 N4 Zn1 N1 -14.8(3) . . . . ? C21 N4 Zn1 N5 -82.1(3) . . . . ? N3 N4 Zn1 N5 94.15(18) . . . . ? C30 N8 Zn1 N6 177.9(3) . . . . ? N7 N8 Zn1 N6 -1.85(16) . . . . ? C30 N8 Zn1 N2 -8.6(3) . . . . ? N7 N8 Zn1 N2 171.64(16) . . . . ? C30 N8 Zn1 N4 66.8(3) . . . . ? N7 N8 Zn1 N4 -112.95(17) . . . . ? C30 N8 Zn1 N1 -84.1(3) . . . . ? N7 N8 Zn1 N1 96.15(17) . . . . ? C30 N8 Zn1 N5 174.6(3) . . . . ? N7 N8 Zn1 N5 -5.2(3) . . . . ? C6 N1 Zn1 N6 -31.41(18) . . . . ? C13 N1 Zn1 N6 -166.78(18) . . . . ? C6 N1 Zn1 N2 144.31(18) . . . . ? C13 N1 Zn1 N2 8.94(17) . . . . ? C6 N1 Zn1 N4 155.01(17) . . . . ? C13 N1 Zn1 N4 19.6(3) . . . . ? C6 N1 Zn1 N8 -106.56(18) . . . . ? C13 N1 Zn1 N8 118.06(18) . . . . ? C6 N1 Zn1 N5 45.77(18) . . . . ? C13 N1 Zn1 N5 -89.60(18) . . . . ? C12 N5 Zn1 N6 136.94(18) . . . . ? C22 N5 Zn1 N6 3.60(17) . . . . ? C12 N5 Zn1 N2 -36.70(18) . . . . ? C22 N5 Zn1 N2 -170.05(18) . . . . ? C12 N5 Zn1 N4 -112.51(17) . . . . ? C22 N5 Zn1 N4 114.14(18) . . . . ? C12 N5 Zn1 N8 140.22(18) . . . . ? C22 N5 Zn1 N8 6.9(3) . . . . ? C12 N5 Zn1 N1 39.74(18) . . . . ? C22 N5 Zn1 N1 -93.60(18) . . . . ? C48 N10 Zn2 N14 -100.8(3) . . . . ? C44 N10 Zn2 N14 69.7(4) . . . . ? C48 N10 Zn2 N16 97.44(19) . . . . ? C44 N10 Zn2 N16 -92.14(19) . . . . ? C48 N10 Zn2 N12 8.87(17) . . . . ? C44 N10 Zn2 N12 179.3(2) . . . . ? C48 N10 Zn2 N9 -175.41(19) . . . . ? C44 N10 Zn2 N9 -4.99(18) . . . . ? C48 N10 Zn2 N13 -82.72(18) . . . . ? C44 N10 Zn2 N13 87.70(19) . . . . ? C57 N14 Zn2 N10 -161.6(3) . . . . ? C53 N14 Zn2 N10 18.1(4) . . . . ? C57 N14 Zn2 N16 2.12(18) . . . . ? C53 N14 Zn2 N16 -178.2(2) . . . . ? C57 N14 Zn2 N12 93.3(2) . . . . ? C53 N14 Zn2 N12 -87.0(2) . . . . ? C57 N14 Zn2 N9 -89.83(19) . . . . ? C53 N14 Zn2 N9 89.9(2) . . . . ? C57 N14 Zn2 N13 179.8(2) . . . . ? C53 N14 Zn2 N13 -0.50(19) . . . . ? C60 N16 Zn2 N10 -2.4(3) . . . . ? N15 N16 Zn2 N10 170.04(16) . . . . ? C60 N16 Zn2 N14 -177.3(3) . . . . ? N15 N16 Zn2 N14 -4.92(16) . . . . ? C60 N16 Zn2 N12 74.5(3) . . . . ? N15 N16 Zn2 N12 -113.07(17) . . . . ? C60 N16 Zn2 N9 -79.6(3) . . . . ? N15 N16 Zn2 N9 92.82(17) . . . . ? C60 N16 Zn2 N13 178.0(3) . . . . ? N15 N16 Zn2 N13 -9.6(3) . . . . ? C51 N12 Zn2 N10 179.9(3) . . . . ? N11 N12 Zn2 N10 -8.79(16) . . . . ? C51 N12 Zn2 N14 -15.8(3) . . . . ? N11 N12 Zn2 N14 155.47(16) . . . . ? C51 N12 Zn2 N16 60.9(3) . . . . ? N11 N12 Zn2 N16 -127.79(16) . . . . ? C51 N12 Zn2 N9 170.9(3) . . . . ? N11 N12 Zn2 N9 -17.8(3) . . . . ? C51 N12 Zn2 N13 -91.3(3) . . . . ? N11 N12 Zn2 N13 80.03(17) . . . . ? C36 N9 Zn2 N10 133.56(17) . . . . ? C43 N9 Zn2 N10 1.11(16) . . . . ? C36 N9 Zn2 N14 -31.04(17) . . . . ? C43 N9 Zn2 N14 -163.50(17) . . . . ? C36 N9 Zn2 N16 -107.08(16) . . . . ? C43 N9 Zn2 N16 120.47(17) . . . . ? C36 N9 Zn2 N12 142.53(18) . . . . ? C43 N9 Zn2 N12 10.1(3) . . . . ? C36 N9 Zn2 N13 44.95(17) . . . . ? C43 N9 Zn2 N13 -87.50(17) . . . . ? C42 N13 Zn2 N10 -35.63(18) . . . . ? C52 N13 Zn2 N10 -171.59(18) . . . . ? C42 N13 Zn2 N14 139.39(19) . . . . ? C52 N13 Zn2 N14 3.42(17) . . . . ? C42 N13 Zn2 N16 144.08(18) . . . . ? C52 N13 Zn2 N16 8.1(3) . . . . ? C42 N13 Zn2 N12 -111.38(18) . . . . ? C52 N13 Zn2 N12 112.66(18) . . . . ? C42 N13 Zn2 N9 41.26(18) . . . . ? C52 N13 Zn2 N9 -94.70(18) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.538 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.063