# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # 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_[Fe(1)(CH3CN)](ClO4)2 _database_code_depnum_ccdc_archive 'CCDC 822563' #TrackingRef 'Dalton 04-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H24 Fe N6, 2(Cl O4), 0.625(C H2 Cl2)' _chemical_formula_sum 'C25.63 H25.25 Cl3.25 Fe N6 O8' _chemical_formula_weight 716.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2117(3) _cell_length_b 20.6062(4) _cell_length_c 23.4209(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.957(2) _cell_angle_gamma 90.00 _cell_volume 5892.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173 _cell_measurement_reflns_used 13991 _cell_measurement_theta_min 4.1948 _cell_measurement_theta_max 32.3709 _exptl_crystal_description 'platy needles' _exptl_crystal_colour Red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2930 _exptl_absorpt_coefficient_mu 0.866 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76794 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 4.23 _diffrn_reflns_theta_max 32.44 _reflns_number_total 19647 _reflns_number_gt 13208 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0964P)^2^+10.4268P] 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 19647 _refine_ls_number_parameters 980 _refine_ls_number_restraints 731 _refine_ls_R_factor_all 0.1246 _refine_ls_R_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.2354 _refine_ls_wR_factor_gt 0.2159 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.070 _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 Fe1A Fe 0.06350(4) 0.29678(2) 0.441285(18) 0.02981(12) Uani 1 1 d . . . N1A N 0.0645(3) 0.39391(14) 0.44013(12) 0.0428(7) Uani 1 1 d . . . C2A C 0.1057(4) 0.41719(17) 0.38300(15) 0.0471(9) Uani 1 1 d . . . H2AA H 0.0545 0.4501 0.3671 0.057 Uiso 1 1 calc R . . H2AB H 0.1781 0.4381 0.3885 0.057 Uiso 1 1 calc R . . C3A C 0.1156(3) 0.36212(16) 0.34142(14) 0.0355(7) Uani 1 1 d . . . N4A N 0.1050(2) 0.30351(13) 0.36482(11) 0.0301(5) Uani 1 1 d . . . C5A C 0.1147(3) 0.24884(16) 0.33378(13) 0.0319(6) Uani 1 1 d . . . C6A C 0.1404(3) 0.25215(19) 0.27620(14) 0.0400(8) Uani 1 1 d . . . H6AA H 0.1511 0.2138 0.2545 0.048 Uiso 1 1 calc R . . C7A C 0.1501(3) 0.3132(2) 0.25136(15) 0.0450(9) Uani 1 1 d . . . H7AA H 0.1650 0.3168 0.2118 0.054 Uiso 1 1 calc R . . C8A C 0.1383(4) 0.36840(19) 0.28352(15) 0.0444(9) Uani 1 1 d . . . H8AA H 0.1454 0.4101 0.2667 0.053 Uiso 1 1 calc R . . C9A C 0.0927(3) 0.19075(15) 0.36739(14) 0.0325(6) Uani 1 1 d . . . N10A N 0.0712(2) 0.20393(13) 0.42337(11) 0.0316(5) Uani 1 1 d . . . C11A C 0.0488(3) 0.15315(16) 0.45777(15) 0.0369(7) Uani 1 1 d . . . H11A H 0.0388 0.1609 0.4973 0.044 Uiso 1 1 calc R . . C12A C 0.0401(4) 0.09044(18) 0.43755(18) 0.0467(9) Uani 1 1 d . . . H12A H 0.0213 0.0562 0.4627 0.056 Uiso 1 1 calc R . . C13A C 0.0585(4) 0.07771(19) 0.38099(19) 0.0528(10) Uani 1 1 d . . . H13A H 0.0516 0.0349 0.3664 0.063 Uiso 1 1 calc R . . C14A C 0.0876(4) 0.12870(18) 0.34535(17) 0.0469(9) Uani 1 1 d . . . H14A H 0.1037 0.1209 0.3064 0.056 Uiso 1 1 calc R . . C15A C -0.0498(4) 0.4151(2) 0.44973(18) 0.0549(12) Uani 1 1 d . . . H15A H -0.0612 0.4589 0.4334 0.066 Uiso 1 1 calc R . . H15B H -0.0634 0.4173 0.4912 0.066 Uiso 1 1 calc R . . C16A C -0.1285(4) 0.3683(2) 0.42214(17) 0.0524(11) Uani 1 1 d . . . N17A N -0.0914(3) 0.30622(16) 0.41803(12) 0.0405(7) Uani 1 1 d . . . C18A C -0.1605(3) 0.2600(2) 0.39914(15) 0.0457(9) Uani 1 1 d . . . H18A H -0.1346 0.2167 0.3959 0.055 Uiso 1 1 calc R . . C19A C -0.2680(4) 0.2735(3) 0.3843(2) 0.0653(14) Uani 1 1 d . . . H19A H -0.3155 0.2397 0.3716 0.078 Uiso 1 1 calc R . . C20A C -0.3049(5) 0.3352(4) 0.3879(2) 0.085(2) Uani 1 1 d . . . H20A H -0.3788 0.3451 0.3782 0.102 Uiso 1 1 calc R . . C21A C -0.2345(5) 0.3838(3) 0.4059(2) 0.0733(17) Uani 1 1 d . . . H21A H -0.2588 0.4276 0.4071 0.088 Uiso 1 1 calc R . . C22A C 0.1422(4) 0.41421(19) 0.48698(17) 0.0539(11) Uani 1 1 d . . . H22A H 0.1667 0.4594 0.4806 0.065 Uiso 1 1 calc R . . H22B H 0.1054 0.4122 0.5243 0.065 Uiso 1 1 calc R . . C23A C 0.2377(4) 0.3698(2) 0.48705(16) 0.0508(10) Uani 1 1 d . . . N24A N 0.2158(3) 0.30852(15) 0.46811(12) 0.0387(6) Uani 1 1 d . . . C25A C 0.2974(3) 0.2649(2) 0.46734(17) 0.0494(9) Uani 1 1 d . . . H25A H 0.2822 0.2223 0.4541 0.059 Uiso 1 1 calc R . . C26A C 0.4026(4) 0.2800(3) 0.4851(2) 0.0712(14) Uani 1 1 d . . . H26A H 0.4589 0.2482 0.4837 0.085 Uiso 1 1 calc R . . C27A C 0.4251(5) 0.3411(4) 0.5046(3) 0.0840(19) Uani 1 1 d . . . H27A H 0.4970 0.3521 0.5174 0.101 Uiso 1 1 calc R . . C28A C 0.3430(6) 0.3863(3) 0.5056(2) 0.0781(18) Uani 1 1 d . . . H28A H 0.3579 0.4290 0.5190 0.094 Uiso 1 1 calc R . . N30A N 0.0134(3) 0.28869(13) 0.51942(12) 0.0349(6) Uani 1 1 d . . . C31A C -0.0235(3) 0.28554(18) 0.56373(15) 0.0389(7) Uani 1 1 d . . . C32A C -0.0734(4) 0.2809(2) 0.61953(16) 0.0539(10) Uani 1 1 d . . . H32A H -0.1446 0.2593 0.6158 0.081 Uiso 1 1 calc R . . H32B H -0.0836 0.3246 0.6351 0.081 Uiso 1 1 calc R . . H32C H -0.0255 0.2558 0.6453 0.081 Uiso 1 1 calc R . . Fe1B Fe 0.55443(5) 0.37885(3) 0.18401(3) 0.05274(18) Uani 1 1 d D . . N1B N 0.6661(4) 0.4470(3) 0.2020(2) 0.0833(16) Uani 1 1 d . A . C2B C 0.7634(5) 0.4145(4) 0.2307(3) 0.104(3) Uani 1 1 d . . . H2BA H 0.8308 0.4266 0.2104 0.125 Uiso 1 1 calc R A . H2BB H 0.7706 0.4307 0.2704 0.125 Uiso 1 1 calc R . . C3B C 0.7534(4) 0.3444(3) 0.2316(2) 0.0713(16) Uani 1 1 d . A . N4B N 0.6558(3) 0.3215(2) 0.21362(16) 0.0586(10) Uani 1 1 d . A . C5B C 0.6331(4) 0.2581(3) 0.21273(19) 0.0579(12) Uani 1 1 d . . . C6B C 0.7106(5) 0.2129(4) 0.2306(2) 0.0790(17) Uani 1 1 d . A . H6BA H 0.6944 0.1678 0.2306 0.095 Uiso 1 1 calc R . . C7B C 0.8114(5) 0.2355(6) 0.2483(2) 0.112(3) Uani 1 1 d . . . H7BA H 0.8663 0.2054 0.2600 0.134 Uiso 1 1 calc R A . C8B C 0.8351(5) 0.3028(5) 0.2495(2) 0.103(3) Uani 1 1 d . A . H8BA H 0.9046 0.3185 0.2621 0.124 Uiso 1 1 calc R . . C9B C 0.5228(4) 0.2458(2) 0.18958(18) 0.0521(10) Uani 1 1 d . A . N10B N 0.4690(3) 0.29995(18) 0.17282(15) 0.0489(8) Uani 1 1 d . A . C11B C 0.3689(4) 0.2939(2) 0.14848(19) 0.0533(10) Uani 1 1 d . . . H11B H 0.3312 0.3318 0.1361 0.064 Uiso 1 1 calc R A . C12B C 0.3190(4) 0.2337(3) 0.1408(2) 0.0629(13) Uani 1 1 d . A . H12B H 0.2480 0.2305 0.1238 0.075 Uiso 1 1 calc R . . C13B C 0.3741(4) 0.1795(3) 0.1582(2) 0.0681(14) Uani 1 1 d . . . H13B H 0.3413 0.1380 0.1532 0.082 Uiso 1 1 calc R A . C14B C 0.4761(4) 0.1842(3) 0.1829(2) 0.0637(12) Uani 1 1 d . A . H14B H 0.5144 0.1465 0.1952 0.076 Uiso 1 1 calc R . . C15B C 0.6149(5) 0.4943(3) 0.2407(2) 0.0703(15) Uani 1 1 d . . . H15C H 0.5700 0.5256 0.2184 0.084 Uiso 1 1 calc R A . H15D H 0.6722 0.5188 0.2620 0.084 Uiso 1 1 calc R . . C16B C 0.5445(4) 0.4583(2) 0.2814(2) 0.0515(10) Uani 1 1 d . A . N17B N 0.5029(3) 0.40111(17) 0.26062(15) 0.0450(7) Uani 1 1 d . A . C18B C 0.4386(3) 0.3663(2) 0.29479(18) 0.0444(8) Uani 1 1 d . . . H18B H 0.4099 0.3262 0.2812 0.053 Uiso 1 1 calc R A . C19B C 0.4124(3) 0.3868(2) 0.34927(18) 0.0480(9) Uani 1 1 d . A . H19B H 0.3664 0.3608 0.3723 0.058 Uiso 1 1 calc R . . C20B C 0.4524(4) 0.4437(2) 0.3697(2) 0.0572(11) Uani 1 1 d . . . H20B H 0.4333 0.4585 0.4067 0.069 Uiso 1 1 calc R A . C21B C 0.5215(4) 0.4802(2) 0.3359(2) 0.0571(11) Uani 1 1 d . A . H21B H 0.5526 0.5195 0.3498 0.068 Uiso 1 1 calc R . . C22B C 0.6972(6) 0.4752(4) 0.1467(3) 0.105(3) Uani 1 1 d . . . H22C H 0.7702 0.4959 0.1504 0.126 Uiso 1 1 calc R A . H22D H 0.6435 0.5089 0.1350 0.126 Uiso 1 1 calc R . . C23B C 0.7003(5) 0.4219(4) 0.1016(2) 0.085(2) Uani 1 1 d . A . N24B N 0.6310(3) 0.3722(2) 0.11036(17) 0.0667(12) Uani 1 1 d . A . C25B C 0.6295(4) 0.3237(3) 0.0730(2) 0.0653(13) Uani 1 1 d . . . H25B H 0.5813 0.2884 0.0795 0.078 Uiso 1 1 calc R A . C26B C 0.6943(5) 0.3218(3) 0.0253(2) 0.0743(16) Uani 1 1 d . A . H26B H 0.6900 0.2867 -0.0010 0.089 Uiso 1 1 calc R . . C27B C 0.7661(5) 0.3732(4) 0.0172(2) 0.088(2) Uani 1 1 d . . . H27B H 0.8132 0.3732 -0.0146 0.105 Uiso 1 1 calc R A . C28B C 0.7691(6) 0.4236(4) 0.0548(3) 0.104(3) Uani 1 1 d . A . H28B H 0.8171 0.4592 0.0491 0.125 Uiso 1 1 calc R . . N30B N 0.4458(5) 0.4428(3) 0.1543(2) 0.0576(14) Uani 0.770(3) 1 d PDU A 1 C31B C 0.3847(9) 0.4807(4) 0.1400(4) 0.089(3) Uani 0.770(3) 1 d PDU A 1 C32B C 0.3025(12) 0.5333(6) 0.1231(6) 0.138(5) Uani 0.770(3) 1 d PDU A 1 H32D H 0.2636 0.5480 0.1570 0.207 Uiso 0.770(3) 1 calc PR A 1 H32E H 0.2497 0.5157 0.0951 0.207 Uiso 0.770(3) 1 calc PR A 1 H32F H 0.3413 0.5701 0.1062 0.207 Uiso 0.770(3) 1 calc PR A 1 N30" N 0.447(2) 0.4240(14) 0.1323(12) 0.101(8) Uiso 0.230(3) 1 d PDU A 2 C31" C 0.400(3) 0.4654(18) 0.1117(16) 0.109(9) Uiso 0.230(3) 1 d PDU A 2 C32" C 0.318(3) 0.511(2) 0.0840(19) 0.130(10) Uiso 0.230(3) 1 d PDU A 2 H32G H 0.2855 0.4907 0.0501 0.195 Uiso 0.230(3) 1 calc PR A 2 H32H H 0.3551 0.5514 0.0729 0.195 Uiso 0.230(3) 1 calc PR A 2 H32I H 0.2603 0.5214 0.1112 0.195 Uiso 0.230(3) 1 calc PR A 2 Cl1 Cl 0.0743(10) 0.0938(6) 0.6203(5) 0.045(2) Uani 0.353(4) 1 d PDU B 1 O11 O 0.0758(9) 0.0508(5) 0.5728(4) 0.045(3) Uiso 0.353(4) 1 d PDU B 1 O12 O 0.0701(10) 0.1616(4) 0.6045(4) 0.063(3) Uiso 0.353(4) 1 d PDU B 1 O13 O 0.1789(7) 0.0827(4) 0.6516(3) 0.0445(19) Uiso 0.353(4) 1 d PDU B 1 O14 O -0.0093(8) 0.0814(5) 0.6615(4) 0.058(2) Uiso 0.353(4) 1 d PDU B 1 Cl1A Cl 0.0678(8) 0.1010(5) 0.6180(4) 0.0367(17) Uani 0.367(8) 1 d PDU C 2 O11A O 0.0507(12) 0.0584(6) 0.5700(4) 0.045(3) Uiso 0.367(8) 1 d PDU C 2 O12A O 0.1102(7) 0.1627(4) 0.6002(3) 0.0341(18) Uiso 0.367(8) 1 d PDU C 2 O13A O 0.1445(8) 0.0694(4) 0.6573(4) 0.056(3) Uiso 0.367(8) 1 d PDU C 2 O14A O -0.0320(7) 0.1084(5) 0.6483(4) 0.055(2) Uiso 0.367(8) 1 d PDU C 2 Cl1B Cl 0.0327(9) 0.1037(5) 0.6190(4) 0.069(3) Uani 0.280(7) 1 d PDU D 3 O11B O 0.0256(12) 0.0606(6) 0.5710(5) 0.048(4) Uiso 0.280(7) 1 d PDU D 3 O12B O 0.1234(11) 0.1496(7) 0.6114(7) 0.079(5) Uiso 0.280(7) 1 d PDU D 3 O13B O 0.0511(14) 0.0683(7) 0.6707(5) 0.082(5) Uiso 0.280(7) 1 d PDU D 3 O14B O -0.0681(12) 0.1388(9) 0.6198(9) 0.141(9) Uiso 0.280(7) 1 d PD D 3 Cl2 Cl 0.2975(3) 0.59316(15) 0.43550(15) 0.0500(6) Uani 0.881(10) 1 d PDU E 1 O21 O 0.2935(6) 0.6583(2) 0.4567(3) 0.105(2) Uani 0.881(10) 1 d PDU E 1 O22 O 0.3491(6) 0.5939(4) 0.3831(3) 0.145(3) Uani 0.881(10) 1 d PDU E 1 O23 O 0.1890(4) 0.5707(3) 0.4306(3) 0.0928(18) Uani 0.881(10) 1 d PDU E 1 O24 O 0.3544(5) 0.5533(2) 0.4746(3) 0.0897(19) Uani 0.881(10) 1 d PDU E 1 Cl2A Cl 0.3038(15) 0.5997(10) 0.4239(10) 0.044(4) Uani 0.119(10) 1 d PDU E 2 O21A O 0.264(3) 0.6430(16) 0.4650(15) 0.070(9) Uiso 0.119(10) 1 d PDU E 2 O22A O 0.327(3) 0.634(2) 0.3737(13) 0.157(11) Uiso 0.119(10) 1 d PDU E 2 O23A O 0.223(3) 0.5524(16) 0.4116(18) 0.091(9) Uiso 0.119(10) 1 d PDU E 2 O24A O 0.399(2) 0.5681(16) 0.4443(16) 0.076(8) Uiso 0.119(10) 1 d PDU E 2 Cl3 Cl 0.1150(3) 0.43713(15) 0.66573(13) 0.0617(9) Uani 0.833(9) 1 d PDU F 1 O31 O 0.0361(4) 0.4334(2) 0.62048(17) 0.0693(14) Uani 0.833(9) 1 d PD F 1 O32 O 0.2175(5) 0.4569(3) 0.6393(3) 0.103(2) Uani 0.833(9) 1 d PDU F 1 O33 O 0.1305(5) 0.3774(3) 0.6908(3) 0.109(3) Uani 0.833(9) 1 d PD F 1 O34 O 0.0832(6) 0.4863(4) 0.7028(3) 0.134(3) Uani 0.833(9) 1 d PDU F 1 Cl3A Cl 0.1279(11) 0.4393(7) 0.6654(4) 0.047(4) Uani 0.167(9) 1 d PDU F 2 O31A O 0.088(3) 0.3886(13) 0.6320(11) 0.149(17) Uiso 0.167(9) 1 d PD F 2 O32A O 0.208(2) 0.4743(17) 0.6342(12) 0.126(10) Uiso 0.167(9) 1 d PDU F 2 O33A O 0.1814(14) 0.4154(9) 0.7158(6) 0.048(5) Uiso 0.167(9) 1 d PD F 2 O34A O 0.045(2) 0.4827(16) 0.6815(13) 0.145(10) Uiso 0.167(9) 1 d PDU F 2 Cl4 Cl 0.4549(4) 0.16379(18) 0.35137(14) 0.0635(10) Uani 0.706(12) 1 d PDU G 1 O41 O 0.5152(7) 0.1292(5) 0.3101(4) 0.116(3) Uani 0.706(12) 1 d PDU G 1 O42 O 0.4395(12) 0.2267(3) 0.3342(5) 0.171(5) Uani 0.706(12) 1 d PDU G 1 O43 O 0.5215(8) 0.1644(4) 0.4036(3) 0.133(4) Uani 0.706(12) 1 d PD G 1 O44 O 0.3593(7) 0.1321(5) 0.3640(6) 0.159(5) Uani 0.706(12) 1 d PD G 1 Cl4A Cl 0.4384(11) 0.1643(6) 0.3554(6) 0.099(4) Uani 0.294(12) 1 d PDU G 2 O41A O 0.5313(16) 0.1288(13) 0.3336(11) 0.151(9) Uiso 0.294(12) 1 d PDU G 2 O42A O 0.469(2) 0.2296(8) 0.3558(11) 0.141(8) Uiso 0.294(12) 1 d PDU G 2 O43A O 0.4203(18) 0.1408(9) 0.4097(6) 0.108(7) Uiso 0.294(12) 1 d PD G 2 O44A O 0.3504(13) 0.1526(9) 0.3179(7) 0.106(7) Uiso 0.294(12) 1 d PD G 2 C50 C 0.1725(15) 0.5579(11) 0.2807(8) 0.065(5) Uiso 0.361(3) 1 d PDU H 2 H50A H 0.1870 0.5907 0.3107 0.078 Uiso 0.361(3) 1 calc PR H 2 H50B H 0.1201 0.5259 0.2960 0.078 Uiso 0.361(3) 1 calc PR H 2 Cl7 Cl 0.1159(6) 0.5942(4) 0.2238(4) 0.134(2) Uani 0.361(3) 1 d PDU H 2 Cl8 Cl 0.2889(5) 0.5203(3) 0.2655(4) 0.0781(16) Uani 0.361(3) 1 d PDU H 2 C50A C 0.190(4) 0.5378(16) 0.2068(9) 0.136(11) Uiso 0.230(3) 1 d PDU I 3 H50C H 0.1130 0.5241 0.2017 0.163 Uiso 0.230(3) 1 calc PR I 3 H50D H 0.2358 0.5017 0.1926 0.163 Uiso 0.230(3) 1 calc PR I 3 Cl7A Cl 0.2088(11) 0.5994(5) 0.1630(6) 0.149(4) Uani 0.230(3) 1 d PDU I 3 Cl8A Cl 0.2135(16) 0.5422(7) 0.2761(6) 0.145(4) Uani 0.230(3) 1 d PDU I 3 C50B C 0.265(2) 0.521(3) 0.260(4) 0.074(13) Uiso 0.159(4) 1 d PDU J 4 H50E H 0.2866 0.5140 0.3007 0.089 Uiso 0.159(4) 1 calc PR J 4 H50F H 0.2622 0.4784 0.2414 0.089 Uiso 0.159(4) 1 calc PR J 4 Cl7B Cl 0.1402(12) 0.5523(7) 0.2588(8) 0.112(4) Uani 0.159(4) 1 d PDU J 4 Cl8B Cl 0.3624(14) 0.5643(10) 0.2303(9) 0.159(6) Uani 0.159(4) 1 d PDU J 4 C60 C 0.4297(13) 0.4321(13) -0.0071(9) 0.157(10) Uani 0.50 1 d P K -1 H60A H 0.4392 0.4227 -0.0482 0.188 Uiso 0.50 1 calc PR K -1 H60B H 0.4773 0.4019 0.0148 0.188 Uiso 0.50 1 calc PR K -1 Cl5 Cl 0.2960(3) 0.4180(2) 0.0102(2) 0.1148(14) Uani 0.50 1 d P K -1 Cl6 Cl 0.4764(4) 0.5207(2) 0.0084(2) 0.1218(15) Uani 0.50 1 d P K -1 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 Fe1A 0.0390(2) 0.0266(2) 0.0240(2) 0.00162(15) 0.00515(16) 0.00525(17) N1A 0.068(2) 0.0292(13) 0.0319(14) 0.0031(11) 0.0144(14) 0.0082(13) C2A 0.076(3) 0.0303(16) 0.0355(17) 0.0052(13) 0.0180(18) 0.0099(17) C3A 0.0463(18) 0.0322(15) 0.0281(14) 0.0043(12) 0.0072(13) 0.0067(13) N4A 0.0346(13) 0.0299(12) 0.0259(11) 0.0028(9) 0.0029(10) 0.0053(10) C5A 0.0333(15) 0.0359(16) 0.0267(13) -0.0035(11) 0.0048(11) 0.0049(12) C6A 0.047(2) 0.0460(19) 0.0267(15) -0.0051(13) 0.0069(13) 0.0054(15) C7A 0.055(2) 0.054(2) 0.0256(15) 0.0050(14) 0.0085(15) 0.0074(18) C8A 0.060(2) 0.0423(19) 0.0309(16) 0.0102(14) 0.0120(16) 0.0061(17) C9A 0.0352(16) 0.0294(14) 0.0332(15) -0.0010(11) 0.0070(12) 0.0045(12) N10A 0.0339(13) 0.0331(13) 0.0278(12) 0.0002(10) 0.0027(10) 0.0049(11) C11A 0.0467(19) 0.0302(15) 0.0339(15) 0.0031(12) 0.0048(14) 0.0021(13) C12A 0.060(2) 0.0283(16) 0.052(2) 0.0046(15) 0.0105(18) 0.0041(15) C13A 0.069(3) 0.0314(17) 0.058(2) -0.0058(16) 0.017(2) 0.0028(17) C14A 0.066(3) 0.0347(18) 0.0408(19) -0.0081(14) 0.0154(18) 0.0062(17) C15A 0.081(3) 0.040(2) 0.044(2) 0.0050(16) 0.025(2) 0.026(2) C16A 0.059(2) 0.058(2) 0.0401(19) 0.0090(17) 0.0184(18) 0.028(2) N17A 0.0426(16) 0.0513(18) 0.0281(13) 0.0095(12) 0.0113(12) 0.0153(13) C18A 0.0384(18) 0.065(2) 0.0343(17) 0.0057(16) 0.0051(14) 0.0063(17) C19A 0.040(2) 0.110(4) 0.046(2) 0.013(2) 0.0029(18) 0.014(2) C20A 0.053(3) 0.150(6) 0.053(3) 0.019(3) 0.005(2) 0.048(4) C21A 0.070(3) 0.095(4) 0.056(3) 0.015(3) 0.011(2) 0.049(3) C22A 0.088(3) 0.0351(18) 0.0385(19) -0.0052(15) 0.009(2) -0.012(2) C23A 0.068(3) 0.050(2) 0.0336(18) 0.0013(15) 0.0023(17) -0.018(2) N24A 0.0467(17) 0.0412(16) 0.0282(13) 0.0026(11) 0.0021(12) -0.0049(13) C25A 0.043(2) 0.061(3) 0.043(2) 0.0065(18) -0.0046(16) 0.0015(18) C26A 0.050(3) 0.103(4) 0.061(3) 0.012(3) -0.012(2) -0.004(3) C27A 0.057(3) 0.124(6) 0.070(4) 0.010(4) -0.023(3) -0.027(4) C28A 0.099(5) 0.091(4) 0.044(2) -0.001(2) -0.005(3) -0.050(4) N30A 0.0450(16) 0.0307(13) 0.0290(12) 0.0025(10) 0.0033(11) 0.0058(11) C31A 0.0458(19) 0.0399(18) 0.0311(15) 0.0014(13) 0.0035(14) 0.0067(14) C32A 0.066(3) 0.065(3) 0.0309(17) 0.0043(17) 0.0170(18) 0.008(2) Fe1B 0.0448(3) 0.0657(4) 0.0480(3) -0.0104(3) 0.0101(3) -0.0228(3) N1B 0.078(3) 0.102(4) 0.071(3) -0.031(3) 0.030(2) -0.052(3) C2B 0.047(3) 0.164(7) 0.103(5) -0.071(5) 0.022(3) -0.040(4) C3B 0.054(3) 0.115(5) 0.046(2) -0.035(3) 0.017(2) -0.021(3) N4B 0.0359(17) 0.092(3) 0.0479(19) -0.0233(19) 0.0061(14) -0.0086(18) C5B 0.042(2) 0.088(4) 0.044(2) -0.011(2) 0.0059(17) 0.005(2) C6B 0.056(3) 0.128(5) 0.054(3) 0.001(3) 0.008(2) 0.021(3) C7B 0.047(3) 0.244(11) 0.044(3) -0.010(5) -0.001(2) 0.026(5) C8B 0.041(3) 0.224(10) 0.045(3) -0.041(4) 0.005(2) -0.011(4) C9B 0.044(2) 0.066(3) 0.047(2) -0.0140(19) 0.0131(17) -0.0050(19) N10B 0.0437(18) 0.056(2) 0.0478(18) -0.0067(15) 0.0096(14) -0.0090(15) C11B 0.042(2) 0.064(3) 0.054(2) -0.012(2) 0.0023(18) -0.0086(19) C12B 0.046(2) 0.076(3) 0.067(3) -0.025(2) 0.011(2) -0.014(2) C13B 0.060(3) 0.064(3) 0.081(3) -0.028(3) 0.020(3) -0.022(2) C14B 0.062(3) 0.059(3) 0.071(3) -0.014(2) 0.016(2) -0.001(2) C15B 0.077(3) 0.067(3) 0.068(3) -0.016(2) 0.019(3) -0.033(3) C16B 0.048(2) 0.045(2) 0.062(3) -0.0087(18) 0.0081(19) -0.0049(17) N17B 0.0390(16) 0.0467(17) 0.0496(18) -0.0060(14) 0.0058(14) -0.0050(13) C18B 0.0336(17) 0.045(2) 0.054(2) -0.0004(16) 0.0069(16) -0.0001(15) C19B 0.0402(19) 0.054(2) 0.050(2) 0.0004(17) 0.0091(16) 0.0037(17) C20B 0.057(3) 0.054(2) 0.061(3) -0.010(2) 0.017(2) 0.011(2) C21B 0.064(3) 0.042(2) 0.066(3) -0.0113(19) 0.013(2) 0.0030(19) C22B 0.123(6) 0.123(6) 0.070(4) -0.026(4) 0.042(4) -0.085(5) C23B 0.080(4) 0.116(5) 0.060(3) -0.014(3) 0.025(3) -0.051(4) N24B 0.057(2) 0.095(3) 0.049(2) -0.013(2) 0.0081(17) -0.032(2) C25B 0.052(3) 0.097(4) 0.047(2) -0.011(2) 0.005(2) -0.015(3) C26B 0.062(3) 0.116(5) 0.046(2) -0.013(3) 0.008(2) -0.012(3) C27B 0.062(3) 0.147(6) 0.055(3) -0.012(3) 0.023(3) -0.026(4) C28B 0.085(4) 0.152(7) 0.077(4) -0.019(4) 0.038(3) -0.057(5) N30B 0.075(4) 0.050(3) 0.048(3) -0.005(2) 0.003(2) -0.025(3) C31B 0.116(7) 0.067(5) 0.084(6) 0.014(4) -0.030(5) -0.029(5) C32B 0.157(10) 0.102(8) 0.151(10) 0.020(7) -0.077(9) -0.008(7) Cl1 0.058(4) 0.036(3) 0.041(3) 0.001(2) -0.004(3) 0.002(2) Cl1A 0.048(4) 0.027(2) 0.035(3) 0.0000(17) 0.007(3) -0.002(2) Cl1B 0.133(8) 0.042(3) 0.033(3) -0.002(2) 0.006(5) -0.019(5) Cl2 0.0489(9) 0.0411(9) 0.0604(13) -0.0015(9) 0.0114(9) -0.0050(7) O21 0.118(5) 0.038(2) 0.157(6) -0.020(3) -0.051(4) 0.011(3) O22 0.174(6) 0.128(5) 0.136(5) 0.047(4) 0.113(5) 0.033(5) O23 0.075(3) 0.097(4) 0.108(4) -0.007(3) 0.019(3) -0.035(3) O24 0.111(4) 0.063(3) 0.094(4) 0.007(3) -0.020(3) 0.021(3) Cl2A 0.033(6) 0.047(6) 0.053(8) 0.019(5) -0.015(6) 0.000(4) Cl3 0.0644(13) 0.0441(13) 0.0756(18) -0.0028(11) -0.0221(12) 0.0114(9) O31 0.085(3) 0.067(3) 0.056(2) 0.0036(19) -0.015(2) -0.001(2) O32 0.080(4) 0.070(3) 0.158(6) 0.051(4) 0.008(3) 0.000(3) O33 0.104(4) 0.100(4) 0.122(5) 0.077(4) 0.001(4) 0.016(4) O34 0.115(5) 0.148(6) 0.140(6) -0.103(5) -0.022(4) 0.016(4) Cl3A 0.054(6) 0.056(7) 0.030(4) 0.015(4) 0.024(4) 0.006(4) Cl4 0.079(2) 0.0463(15) 0.0658(14) 0.0057(12) 0.0134(12) -0.0078(13) O41 0.115(6) 0.133(6) 0.101(6) -0.016(5) 0.017(5) 0.046(5) O42 0.304(13) 0.056(4) 0.151(9) 0.029(5) -0.014(9) 0.033(6) O43 0.157(9) 0.141(8) 0.100(6) -0.015(5) -0.046(6) 0.002(6) O44 0.089(6) 0.147(8) 0.240(15) 0.016(8) 0.008(7) -0.047(6) Cl4A 0.071(5) 0.066(5) 0.162(9) -0.049(5) 0.031(5) 0.004(4) Cl7 0.102(4) 0.151(6) 0.149(6) 0.004(5) -0.042(4) 0.024(4) Cl8 0.073(3) 0.072(3) 0.090(4) 0.000(2) 0.002(3) 0.007(2) Cl7A 0.154(8) 0.094(6) 0.195(9) 0.038(6) -0.080(7) -0.018(6) Cl8A 0.167(11) 0.094(7) 0.172(10) 0.032(7) -0.032(9) -0.023(8) Cl7B 0.105(8) 0.081(7) 0.150(10) -0.001(7) -0.047(8) 0.009(6) Cl8B 0.151(11) 0.143(10) 0.182(11) -0.003(10) -0.005(10) -0.011(9) C60 0.069(9) 0.26(3) 0.141(15) -0.105(17) -0.017(10) 0.030(13) Cl5 0.090(2) 0.134(3) 0.121(3) -0.034(3) 0.018(2) -0.015(2) Cl6 0.114(4) 0.122(4) 0.129(4) -0.015(3) -0.026(3) 0.007(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 Fe1A N4A 1.875(3) . ? Fe1A N30A 1.946(3) . ? Fe1A N10A 1.962(3) . ? Fe1A N24A 1.968(3) . ? Fe1A N17A 1.969(3) . ? Fe1A N1A 2.002(3) . ? N1A C15A 1.483(5) . ? N1A C22A 1.499(6) . ? N1A C2A 1.515(4) . ? C2A C3A 1.502(5) . ? C3A N4A 1.333(4) . ? C3A C8A 1.395(4) . ? N4A C5A 1.347(4) . ? C5A C6A 1.392(4) . ? C5A C9A 1.460(4) . ? C6A C7A 1.393(5) . ? C7A C8A 1.372(5) . ? C9A N10A 1.369(4) . ? C9A C14A 1.380(5) . ? N10A C11A 1.351(4) . ? C11A C12A 1.380(5) . ? C12A C13A 1.373(6) . ? C13A C14A 1.392(6) . ? C15A C16A 1.499(7) . ? C16A N17A 1.361(5) . ? C16A C21A 1.380(7) . ? N17A C18A 1.343(6) . ? C18A C19A 1.381(6) . ? C19A C20A 1.354(9) . ? C20A C21A 1.381(10) . ? C22A C23A 1.482(7) . ? C23A N24A 1.363(5) . ? C23A C28A 1.393(7) . ? N24A C25A 1.342(5) . ? C25A C26A 1.379(6) . ? C26A C27A 1.366(9) . ? C27A C28A 1.370(10) . ? N30A C31A 1.140(4) . ? C31A C32A 1.454(5) . ? Fe1B N4B 1.839(5) . ? Fe1B N10B 1.947(3) . ? Fe1B N17B 1.966(3) . ? Fe1B N24B 1.980(4) . ? Fe1B N30B 1.987(6) . ? Fe1B N1B 1.997(4) . ? Fe1B N30" 2.002(16) . ? N1B C22B 1.475(7) . ? N1B C15B 1.479(7) . ? N1B C2B 1.512(10) . ? C2B C3B 1.451(10) . ? C3B N4B 1.343(6) . ? C3B C8B 1.375(10) . ? N4B C5B 1.336(7) . ? C5B C6B 1.387(8) . ? C5B C9B 1.466(6) . ? C6B C7B 1.374(10) . ? C7B C8B 1.417(12) . ? C9B N10B 1.350(6) . ? C9B C14B 1.398(7) . ? N10B C11B 1.346(6) . ? C11B C12B 1.392(6) . ? C12B C13B 1.363(8) . ? C13B C14B 1.368(8) . ? C15B C16B 1.492(6) . ? C16B N17B 1.370(5) . ? C16B C21B 1.385(6) . ? N17B C18B 1.339(5) . ? C18B C19B 1.386(6) . ? C19B C20B 1.355(6) . ? C20B C21B 1.389(7) . ? C22B C23B 1.524(9) . ? C23B N24B 1.348(7) . ? C23B C28B 1.394(7) . ? N24B C25B 1.327(7) . ? C25B C26B 1.381(6) . ? C26B C27B 1.390(9) . ? C27B C28B 1.360(9) . ? N30B C31B 1.127(10) . ? C31B C32B 1.527(14) . ? N30" C31" 1.129(17) . ? C31" C32" 1.52(2) . ? Cl1 O11 1.423(11) . ? Cl1 O14 1.439(11) . ? Cl1 O12 1.447(11) . ? Cl1 O13 1.480(11) . ? Cl1A O14A 1.428(9) . ? Cl1A O11A 1.438(10) . ? Cl1A O12A 1.438(10) . ? Cl1A O13A 1.456(11) . ? Cl1B O13B 1.428(11) . ? Cl1B O14B 1.429(12) . ? Cl1B O11B 1.435(10) . ? Cl1B O12B 1.469(11) . ? Cl2 O22 1.390(5) . ? Cl2 O23 1.406(5) . ? Cl2 O24 1.406(5) . ? Cl2 O21 1.432(5) . ? Cl2A O22A 1.403(13) . ? Cl2A O21A 1.405(13) . ? Cl2A O24A 1.408(13) . ? Cl2A O23A 1.416(13) . ? Cl3 O33 1.375(5) . ? Cl3 O34 1.394(5) . ? Cl3 O31 1.422(5) . ? Cl3 O32 1.464(6) . ? Cl3A O31A 1.387(13) . ? Cl3A O34A 1.404(13) . ? Cl3A O33A 1.428(12) . ? Cl3A O32A 1.428(13) . ? Cl4 O42 1.369(7) . ? Cl4 O44 1.374(8) . ? Cl4 O41 1.417(7) . ? Cl4 O43 1.457(8) . ? Cl4A O43A 1.381(12) . ? Cl4A O42A 1.395(12) . ? Cl4A O44A 1.398(12) . ? Cl4A O41A 1.451(12) . ? C50 Cl8 1.663(14) . ? C50 Cl7 1.668(14) . ? C50A Cl8A 1.646(17) . ? C50A Cl7A 1.650(18) . ? C50B Cl8B 1.647(19) . ? C50B Cl7B 1.652(19) . ? C60 Cl5 1.713(18) . ? C60 Cl6 1.95(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 N4A Fe1A N30A 177.28(13) . . ? N4A Fe1A N10A 81.55(11) . . ? N30A Fe1A N10A 97.72(11) . . ? N4A Fe1A N24A 91.52(12) . . ? N30A Fe1A N24A 91.18(12) . . ? N10A Fe1A N24A 98.04(12) . . ? N4A Fe1A N17A 90.13(12) . . ? N30A Fe1A N17A 87.31(12) . . ? N10A Fe1A N17A 94.95(13) . . ? N24A Fe1A N17A 167.01(14) . . ? N4A Fe1A N1A 84.91(11) . . ? N30A Fe1A N1A 95.77(12) . . ? N10A Fe1A N1A 166.45(11) . . ? N24A Fe1A N1A 82.86(14) . . ? N17A Fe1A N1A 84.46(15) . . ? C15A N1A C22A 113.2(3) . . ? C15A N1A C2A 111.6(3) . . ? C22A N1A C2A 110.0(3) . . ? C15A N1A Fe1A 106.6(3) . . ? C22A N1A Fe1A 105.8(2) . . ? C2A N1A Fe1A 109.3(2) . . ? C3A C2A N1A 111.4(3) . . ? N4A C3A C8A 120.4(3) . . ? N4A C3A C2A 114.1(3) . . ? C8A C3A C2A 125.4(3) . . ? C3A N4A C5A 121.7(3) . . ? C3A N4A Fe1A 119.3(2) . . ? C5A N4A Fe1A 118.8(2) . . ? N4A C5A C6A 120.3(3) . . ? N4A C5A C9A 112.1(3) . . ? C6A C5A C9A 127.5(3) . . ? C5A C6A C7A 118.1(3) . . ? C8A C7A C6A 120.6(3) . . ? C7A C8A C3A 118.8(3) . . ? N10A C9A C14A 122.3(3) . . ? N10A C9A C5A 113.2(3) . . ? C14A C9A C5A 124.5(3) . . ? C11A N10A C9A 117.5(3) . . ? C11A N10A Fe1A 128.1(2) . . ? C9A N10A Fe1A 114.1(2) . . ? N10A C11A C12A 122.4(3) . . ? C13A C12A C11A 119.8(3) . . ? C12A C13A C14A 118.8(4) . . ? C9A C14A C13A 119.1(3) . . ? N1A C15A C16A 110.1(3) . . ? N17A C16A C21A 120.6(5) . . ? N17A C16A C15A 115.0(4) . . ? C21A C16A C15A 124.1(4) . . ? C18A N17A C16A 118.8(4) . . ? C18A N17A Fe1A 128.1(3) . . ? C16A N17A Fe1A 113.1(3) . . ? N17A C18A C19A 122.0(5) . . ? C20A C19A C18A 119.3(6) . . ? C19A C20A C21A 119.6(5) . . ? C16A C21A C20A 119.5(5) . . ? C23A C22A N1A 108.5(3) . . ? N24A C23A C28A 120.2(5) . . ? N24A C23A C22A 115.0(4) . . ? C28A C23A C22A 124.8(5) . . ? C25A N24A C23A 118.9(4) . . ? C25A N24A Fe1A 127.7(3) . . ? C23A N24A Fe1A 113.4(3) . . ? N24A C25A C26A 122.3(5) . . ? C27A C26A C25A 119.3(6) . . ? C26A C27A C28A 119.4(5) . . ? C27A C28A C23A 120.0(5) . . ? C31A N30A Fe1A 174.8(3) . . ? N30A C31A C32A 178.4(5) . . ? N4B Fe1B N10B 82.51(17) . . ? N4B Fe1B N17B 91.69(15) . . ? N10B Fe1B N17B 97.98(14) . . ? N4B Fe1B N24B 87.66(19) . . ? N10B Fe1B N24B 94.82(15) . . ? N17B Fe1B N24B 166.99(15) . . ? N4B Fe1B N30B 178.0(2) . . ? N10B Fe1B N30B 98.84(19) . . ? N17B Fe1B N30B 86.74(19) . . ? N24B Fe1B N30B 93.6(2) . . ? N4B Fe1B N1B 85.4(2) . . ? N10B Fe1B N1B 167.9(2) . . ? N17B Fe1B N1B 82.63(16) . . ? N24B Fe1B N1B 84.36(17) . . ? N30B Fe1B N1B 93.3(2) . . ? N4B Fe1B N30" 163.3(9) . . ? N10B Fe1B N30" 87.8(9) . . ? N17B Fe1B N30" 103.1(9) . . ? N24B Fe1B N30" 79.6(10) . . ? N30B Fe1B N30" 18.6(9) . . ? N1B Fe1B N30" 103.9(9) . . ? C22B N1B C15B 113.3(6) . . ? C22B N1B C2B 110.7(5) . . ? C15B N1B C2B 110.8(5) . . ? C22B N1B Fe1B 106.1(3) . . ? C15B N1B Fe1B 107.4(3) . . ? C2B N1B Fe1B 108.2(4) . . ? C3B C2B N1B 112.4(5) . . ? N4B C3B C8B 120.8(6) . . ? N4B C3B C2B 114.8(6) . . ? C8B C3B C2B 124.4(6) . . ? C5B N4B C3B 122.1(5) . . ? C5B N4B Fe1B 119.0(3) . . ? C3B N4B Fe1B 118.7(4) . . ? N4B C5B C6B 120.8(5) . . ? N4B C5B C9B 111.4(4) . . ? C6B C5B C9B 127.8(6) . . ? C7B C6B C5B 117.8(8) . . ? C6B C7B C8B 121.3(8) . . ? C3B C8B C7B 117.2(6) . . ? N10B C9B C14B 121.5(4) . . ? N10B C9B C5B 113.8(4) . . ? C14B C9B C5B 124.7(5) . . ? C11B N10B C9B 118.7(4) . . ? C11B N10B Fe1B 128.0(3) . . ? C9B N10B Fe1B 113.3(3) . . ? N10B C11B C12B 122.0(5) . . ? C13B C12B C11B 118.6(5) . . ? C12B C13B C14B 120.6(5) . . ? C13B C14B C9B 118.6(5) . . ? N1B C15B C16B 108.5(4) . . ? N17B C16B C21B 121.9(4) . . ? N17B C16B C15B 114.5(4) . . ? C21B C16B C15B 123.6(4) . . ? C18B N17B C16B 117.8(4) . . ? C18B N17B Fe1B 128.4(3) . . ? C16B N17B Fe1B 113.8(3) . . ? N17B C18B C19B 122.3(4) . . ? C20B C19B C18B 120.1(4) . . ? C19B C20B C21B 119.1(4) . . ? C16B C21B C20B 118.9(4) . . ? N1B C22B C23B 109.4(5) . . ? N24B C23B C28B 121.8(6) . . ? N24B C23B C22B 114.9(4) . . ? C28B C23B C22B 123.4(5) . . ? C25B N24B C23B 118.3(4) . . ? C25B N24B Fe1B 128.7(3) . . ? C23B N24B Fe1B 112.7(3) . . ? N24B C25B C26B 123.6(5) . . ? C25B C26B C27B 117.4(5) . . ? C28B C27B C26B 120.2(5) . . ? C27B C28B C23B 118.7(6) . . ? C31B N30B Fe1B 176.5(7) . . ? N30B C31B C32B 177.7(11) . . ? C31" N30" Fe1B 158(3) . . ? N30" C31" C32" 168(5) . . ? O11 Cl1 O14 115.6(9) . . ? O11 Cl1 O12 113.7(9) . . ? O14 Cl1 O12 108.8(9) . . ? O11 Cl1 O13 105.6(8) . . ? O14 Cl1 O13 104.9(8) . . ? O12 Cl1 O13 107.6(9) . . ? O14A Cl1A O11A 109.8(8) . . ? O14A Cl1A O12A 111.3(8) . . ? O11A Cl1A O12A 111.1(8) . . ? O14A Cl1A O13A 106.2(7) . . ? O11A Cl1A O13A 107.8(9) . . ? O12A Cl1A O13A 110.4(8) . . ? O13B Cl1B O14B 111.7(10) . . ? O13B Cl1B O11B 110.7(9) . . ? O14B Cl1B O11B 106.4(9) . . ? O13B Cl1B O12B 108.9(10) . . ? O14B Cl1B O12B 109.2(10) . . ? O11B Cl1B O12B 109.9(9) . . ? O22 Cl2 O23 111.8(5) . . ? O22 Cl2 O24 110.8(4) . . ? O23 Cl2 O24 108.5(4) . . ? O22 Cl2 O21 108.3(5) . . ? O23 Cl2 O21 107.4(4) . . ? O24 Cl2 O21 109.9(4) . . ? O22A Cl2A O21A 109.4(12) . . ? O22A Cl2A O24A 109.9(12) . . ? O21A Cl2A O24A 110.6(12) . . ? O22A Cl2A O23A 108.9(12) . . ? O21A Cl2A O23A 109.2(12) . . ? O24A Cl2A O23A 108.8(12) . . ? O33 Cl3 O34 115.0(5) . . ? O33 Cl3 O31 110.9(4) . . ? O34 Cl3 O31 108.2(4) . . ? O33 Cl3 O32 108.4(4) . . ? O34 Cl3 O32 108.1(5) . . ? O31 Cl3 O32 105.9(4) . . ? O31A Cl3A O34A 112.7(12) . . ? O31A Cl3A O33A 110.9(11) . . ? O34A Cl3A O33A 108.5(11) . . ? O31A Cl3A O32A 109.1(11) . . ? O34A Cl3A O32A 108.7(12) . . ? O33A Cl3A O32A 106.7(11) . . ? O42 Cl4 O44 113.6(7) . . ? O42 Cl4 O41 110.2(6) . . ? O44 Cl4 O41 111.2(6) . . ? O42 Cl4 O43 108.1(6) . . ? O44 Cl4 O43 106.7(6) . . ? O41 Cl4 O43 106.7(6) . . ? O43A Cl4A O42A 112.4(11) . . ? O43A Cl4A O44A 112.6(11) . . ? O42A Cl4A O44A 111.9(11) . . ? O43A Cl4A O41A 106.6(11) . . ? O42A Cl4A O41A 106.1(11) . . ? O44A Cl4A O41A 106.7(10) . . ? Cl8 C50 Cl7 112.4(12) . . ? Cl8A C50A Cl7A 123(2) . . ? Cl8B C50B Cl7B 117(2) . . ? Cl5 C60 Cl6 113.1(10) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.455 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.089 data_[{Fe(1)}2O](ClO4)4 _database_code_depnum_ccdc_archive 'CCDC 822564' #TrackingRef 'Dalton 04-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H42 Fe2 N10 O, C2 H3 N, 4(Cl O4), H2 O' _chemical_formula_sum 'C48 H47 Cl4 Fe2 N11 O18' _chemical_formula_weight 1319.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4043(8) _cell_length_b 38.877(2) _cell_length_c 12.3737(10) _cell_angle_alpha 90.00 _cell_angle_beta 117.208(8) _cell_angle_gamma 90.00 _cell_volume 5306.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 3077 _cell_measurement_theta_min 4.0995 _cell_measurement_theta_max 29.1219 _exptl_crystal_description 'thin plates' _exptl_crystal_colour Orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.832 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22265 _diffrn_reflns_av_R_equivalents 0.1065 _diffrn_reflns_av_sigmaI/netI 0.1796 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -52 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 29.19 _reflns_number_total 10488 _reflns_number_gt 5396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0399P)^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 10488 _refine_ls_number_parameters 775 _refine_ls_number_restraints 124 _refine_ls_R_factor_all 0.1683 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.1703 _refine_ls_wR_factor_gt 0.1365 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.977 _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 Fe1 Fe 0.08160(6) 0.40013(2) 0.21029(7) 0.0171(2) Uani 1 1 d . . . Fe2 Fe 0.32948(7) 0.35686(2) 0.19272(8) 0.0197(2) Uani 1 1 d . . . O O 0.2009(3) 0.37673(9) 0.1987(3) 0.0209(9) Uani 1 1 d . . . N1 N 0.1390(4) 0.44841(12) 0.1728(5) 0.0209(11) Uani 1 1 d . . . C2 C 0.1044(5) 0.46123(15) 0.0621(6) 0.0236(14) Uani 1 1 d . . . H2A H 0.0452 0.4491 -0.0056 0.028 Uiso 1 1 calc R . . C3 C 0.1503(5) 0.49124(16) 0.0411(6) 0.0272(15) Uani 1 1 d . . . H3A H 0.1250 0.4995 -0.0391 0.033 Uiso 1 1 calc R . . C4 C 0.2344(6) 0.50900(17) 0.1408(7) 0.0376(18) Uani 1 1 d . . . H4A H 0.2677 0.5299 0.1299 0.045 Uiso 1 1 calc R . . C5 C 0.2696(5) 0.49631(15) 0.2553(6) 0.0309(16) Uani 1 1 d . . . H5A H 0.3261 0.5086 0.3244 0.037 Uiso 1 1 calc R . . C6 C 0.2219(5) 0.46536(14) 0.2697(5) 0.0201(13) Uani 1 1 d . . . C7 C 0.2604(5) 0.44850(15) 0.3879(6) 0.0274(15) Uani 1 1 d . . . H7A H 0.2816 0.4663 0.4516 0.033 Uiso 1 1 calc R . . H7B H 0.3341 0.4347 0.4073 0.033 Uiso 1 1 calc R . . N8 N 0.1652(4) 0.42585(11) 0.3896(4) 0.0185(11) Uani 1 1 d . . . C9 C 0.2154(5) 0.39819(15) 0.4810(5) 0.0245(14) Uani 1 1 d . . . H9A H 0.2269 0.4068 0.5608 0.029 Uiso 1 1 calc R . . H9B H 0.2955 0.3911 0.4893 0.029 Uiso 1 1 calc R . . C10 C 0.1314(4) 0.36784(14) 0.4438(5) 0.0183(13) Uani 1 1 d . . . C11 C 0.1365(5) 0.34325(15) 0.5262(6) 0.0255(14) Uani 1 1 d . . . H11A H 0.1885 0.3463 0.6105 0.031 Uiso 1 1 calc R . . C12 C 0.0658(6) 0.31425(16) 0.4856(7) 0.0348(17) Uani 1 1 d . . . H12A H 0.0705 0.2967 0.5412 0.042 Uiso 1 1 calc R . . C13 C -0.0120(5) 0.31084(16) 0.3634(6) 0.0289(15) Uani 1 1 d . . . H13A H -0.0631 0.2913 0.3334 0.035 Uiso 1 1 calc R . . C14 C -0.0138(5) 0.33647(14) 0.2861(6) 0.0220(14) Uani 1 1 d . . . H14A H -0.0675 0.3343 0.2018 0.026 Uiso 1 1 calc R . . N15 N 0.0572(4) 0.36445(11) 0.3248(4) 0.0183(11) Uani 1 1 d . . . C16 C 0.0726(5) 0.44650(15) 0.4106(5) 0.0267(15) Uani 1 1 d . . . H16A H 0.0611 0.4357 0.4770 0.032 Uiso 1 1 calc R . . H16B H 0.1046 0.4700 0.4371 0.032 Uiso 1 1 calc R . . N17 N -0.0665(4) 0.42855(11) 0.2084(4) 0.0176(11) Uani 1 1 d . . . C18 C -0.0472(5) 0.44892(15) 0.3001(6) 0.0223(14) Uani 1 1 d . . . C19 C -0.1383(5) 0.47112(16) 0.2956(6) 0.0328(16) Uani 1 1 d . . . H19A H -0.1255 0.4860 0.3613 0.039 Uiso 1 1 calc R . . C20 C -0.2476(5) 0.47035(16) 0.1912(6) 0.0318(16) Uani 1 1 d . . . H20A H -0.3109 0.4853 0.1844 0.038 Uiso 1 1 calc R . . C21 C -0.2666(5) 0.44861(16) 0.0978(6) 0.0312(16) Uani 1 1 d . . . H21A H -0.3426 0.4482 0.0269 0.037 Uiso 1 1 calc R . . C22 C -0.1741(5) 0.42732(15) 0.1077(6) 0.0227(14) Uani 1 1 d . . . C23 C -0.1775(4) 0.40252(15) 0.0171(5) 0.0207(14) Uani 1 1 d . . . C24 C -0.2816(5) 0.39453(15) -0.0882(6) 0.0257(15) Uani 1 1 d . . . H24A H -0.3564 0.4053 -0.1052 0.031 Uiso 1 1 calc R . . C25 C -0.2754(5) 0.37076(17) -0.1677(6) 0.0372(18) Uani 1 1 d . . . H25A H -0.3463 0.3648 -0.2396 0.045 Uiso 1 1 calc R . . C26 C -0.1666(5) 0.35579(17) -0.1426(5) 0.0305(15) Uani 1 1 d . . . H26A H -0.1597 0.3399 -0.1973 0.037 Uiso 1 1 calc R . . C27 C -0.0679(5) 0.36452(16) -0.0360(6) 0.0306(16) Uani 1 1 d . . . H27A H 0.0068 0.3534 -0.0168 0.037 Uiso 1 1 calc R . . N28 N -0.0700(4) 0.38738(12) 0.0415(4) 0.0215(11) Uani 1 1 d . . . N31 N 0.4590(4) 0.39195(12) 0.3143(4) 0.0230(12) Uani 1 1 d . . . C32 C 0.5213(5) 0.38788(17) 0.4347(6) 0.0309(16) Uani 1 1 d . . . H32A H 0.5091 0.3675 0.4700 0.037 Uiso 1 1 calc R . . C33 C 0.6020(6) 0.41184(19) 0.5092(7) 0.0404(18) Uani 1 1 d . . . H33A H 0.6421 0.4086 0.5948 0.048 Uiso 1 1 calc R . . C34 C 0.6234(6) 0.44052(19) 0.4577(7) 0.0436(19) Uani 1 1 d . . . H34A H 0.6817 0.4570 0.5072 0.052 Uiso 1 1 calc R . . C35 C 0.5608(6) 0.44546(17) 0.3345(7) 0.0361(17) Uani 1 1 d . . . H35A H 0.5734 0.4656 0.2982 0.043 Uiso 1 1 calc R . . C36 C 0.4786(5) 0.42058(16) 0.2639(6) 0.0276(15) Uani 1 1 d . . . C37 C 0.4022(5) 0.42361(14) 0.1296(6) 0.0279(15) Uani 1 1 d . . . H37A H 0.3257 0.4356 0.1125 0.033 Uiso 1 1 calc R . . H37B H 0.4456 0.4374 0.0946 0.033 Uiso 1 1 calc R . . N38 N 0.3747(4) 0.38966(12) 0.0727(4) 0.0225(12) Uani 1 1 d . . . C39 C 0.2632(5) 0.39038(15) -0.0476(5) 0.0280(15) Uani 1 1 d . . . H39A H 0.2852 0.3971 -0.1121 0.034 Uiso 1 1 calc R . . H39B H 0.2055 0.4076 -0.0454 0.034 Uiso 1 1 calc R . . C40 C 0.2041(5) 0.35535(16) -0.0759(6) 0.0252(15) Uani 1 1 d . . . C41 C 0.1234(5) 0.3462(2) -0.1934(6) 0.0400(18) Uani 1 1 d . . . H41A H 0.1071 0.3612 -0.2597 0.048 Uiso 1 1 calc R . . C42 C 0.0673(6) 0.31459(19) -0.2113(7) 0.0409(18) Uani 1 1 d . . . H42A H 0.0122 0.3077 -0.2914 0.049 Uiso 1 1 calc R . . C43 C 0.0892(6) 0.29318(19) -0.1168(7) 0.0402(18) Uani 1 1 d . . . H43A H 0.0501 0.2715 -0.1294 0.048 Uiso 1 1 calc R . . C44 C 0.1697(5) 0.30393(17) -0.0027(6) 0.0330(16) Uani 1 1 d . . . H44A H 0.1860 0.2892 0.0644 0.040 Uiso 1 1 calc R . . N45 N 0.2263(4) 0.33436(12) 0.0180(4) 0.0225(12) Uani 1 1 d . . . C46 C 0.4820(5) 0.37549(16) 0.0578(6) 0.0329(16) Uani 1 1 d . . . H46A H 0.4581 0.3733 -0.0299 0.039 Uiso 1 1 calc R . . H46B H 0.5497 0.3921 0.0927 0.039 Uiso 1 1 calc R . . N47 N 0.4779(4) 0.33025(12) 0.1882(4) 0.0216(11) Uani 1 1 d . . . C48 C 0.5247(5) 0.34168(14) 0.1169(5) 0.0220(14) Uani 1 1 d . . . C49 C 0.6124(5) 0.32286(17) 0.1033(6) 0.0333(16) Uani 1 1 d . . . H49A H 0.6442 0.3305 0.0507 0.040 Uiso 1 1 calc R . . C50 C 0.6529(5) 0.29222(17) 0.1692(6) 0.0369(18) Uani 1 1 d . . . H50A H 0.7149 0.2792 0.1636 0.044 Uiso 1 1 calc R . . C51 C 0.6040(5) 0.28110(16) 0.2409(6) 0.0311(16) Uani 1 1 d . . . H51A H 0.6312 0.2603 0.2853 0.037 Uiso 1 1 calc R . . C52 C 0.5144(5) 0.30033(15) 0.2489(5) 0.0247(14) Uani 1 1 d . . . C53 C 0.4453(5) 0.29034(15) 0.3145(5) 0.0236(14) Uani 1 1 d . . . C54 C 0.4669(5) 0.26098(16) 0.3832(6) 0.0354(17) Uani 1 1 d . . . H54A H 0.5334 0.2465 0.3964 0.042 Uiso 1 1 calc R . . C55 C 0.3902(6) 0.25287(17) 0.4329(6) 0.0393(18) Uani 1 1 d . . . H55A H 0.4021 0.2323 0.4786 0.047 Uiso 1 1 calc R . . C56 C 0.2970(6) 0.27467(16) 0.4158(6) 0.0378(18) Uani 1 1 d . . . H56A H 0.2437 0.2695 0.4494 0.045 Uiso 1 1 calc R . . C57 C 0.2821(5) 0.30419(15) 0.3491(6) 0.0290(16) Uani 1 1 d . . . H57A H 0.2181 0.3194 0.3384 0.035 Uiso 1 1 calc R . . N58 N 0.3541(4) 0.31241(12) 0.2986(4) 0.0229(12) Uani 1 1 d . . . Cl1 Cl 0.43301(13) 0.45516(4) 0.75277(15) 0.0322(4) Uani 1 1 d . . . O11 O 0.3170(3) 0.46780(12) 0.6681(4) 0.0435(13) Uani 1 1 d . . . O12 O 0.4961(4) 0.48125(13) 0.8400(4) 0.0581(15) Uani 1 1 d . . . O13 O 0.5003(4) 0.44627(13) 0.6920(4) 0.0550(14) Uani 1 1 d . . . O14 O 0.4195(5) 0.42588(14) 0.8138(6) 0.086(2) Uani 1 1 d . . . Cl2 Cl 0.43885(15) 0.18205(5) 0.22045(17) 0.0439(5) Uani 1 1 d . . . O21 O 0.4282(4) 0.15938(13) 0.1238(5) 0.0652(16) Uani 1 1 d . . . O22 O 0.5580(4) 0.19670(15) 0.2763(6) 0.086(2) Uani 1 1 d . . . O23 O 0.4196(6) 0.16328(17) 0.3067(6) 0.100(2) Uani 1 1 d . . . O24 O 0.3510(5) 0.20904(14) 0.1766(5) 0.0803(19) Uani 1 1 d . . . Cl3 Cl -0.1134(5) 0.23747(12) -0.4641(7) 0.0340(14) Uani 0.688(19) 1 d PDU A 1 O31 O -0.1625(10) 0.2058(2) -0.4497(10) 0.051(3) Uani 0.688(19) 1 d PDU A 1 O32 O 0.0142(6) 0.2386(3) -0.3841(9) 0.059(3) Uani 0.688(19) 1 d PDU A 1 O33 O -0.1352(7) 0.2408(3) -0.5887(8) 0.062(3) Uani 0.688(19) 1 d PDU A 1 O34 O -0.1690(9) 0.2658(2) -0.4343(16) 0.084(4) Uani 0.688(19) 1 d PDU A 1 Cl3' Cl -0.1100(15) 0.2372(4) -0.4441(16) 0.063(5) Uani 0.312(19) 1 d PDU A 2 O31' O -0.188(2) 0.2076(5) -0.480(2) 0.039(6) Uiso 0.312(19) 1 d PDU A 2 O32' O 0.0132(15) 0.2265(6) -0.387(2) 0.063(7) Uiso 0.312(19) 1 d PDU A 2 O33' O -0.1364(17) 0.2584(6) -0.5479(19) 0.062(6) Uiso 0.312(19) 1 d PDU A 2 O34' O -0.1346(17) 0.2570(5) -0.360(2) 0.054(6) Uiso 0.312(19) 1 d PDU A 2 Cl4 Cl 0.02787(16) 0.55867(5) 0.30858(17) 0.0432(5) Uani 1 1 d . . . O41 O 0.1075(6) 0.57552(16) 0.2742(6) 0.096(2) Uani 1 1 d . . . O42 O -0.0721(5) 0.54619(18) 0.2068(5) 0.104(2) Uani 1 1 d . . . O43 O 0.0871(5) 0.53214(14) 0.3925(5) 0.0777(18) Uani 1 1 d . . . O44 O -0.0176(7) 0.58311(16) 0.3644(6) 0.107(2) Uani 1 1 d . . . N60 N 0.7576(5) 0.38538(17) 0.3010(7) 0.0584(19) Uani 1 1 d . . . C61 C 0.7821(6) 0.37133(19) 0.3888(8) 0.0404(19) Uani 1 1 d . . . C62 C 0.8117(6) 0.3521(2) 0.5001(7) 0.061(2) Uani 1 1 d . . . H62A H 0.7377 0.3481 0.5081 0.092 Uiso 1 1 calc R . . H62B H 0.8695 0.3653 0.5702 0.092 Uiso 1 1 calc R . . H62C H 0.8479 0.3300 0.4968 0.092 Uiso 1 1 calc R . . O70 O -0.3339(5) 0.31040(16) -0.3940(6) 0.092(2) 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 Fe1 0.0165(4) 0.0216(4) 0.0137(5) -0.0001(4) 0.0074(3) 0.0014(4) Fe2 0.0194(4) 0.0210(5) 0.0213(6) 0.0022(4) 0.0117(4) 0.0035(4) O 0.025(2) 0.017(2) 0.025(3) -0.0023(19) 0.0147(17) 0.0052(17) N1 0.018(2) 0.031(3) 0.018(3) 0.004(3) 0.013(2) 0.004(2) C2 0.013(3) 0.031(4) 0.026(4) -0.003(3) 0.009(3) 0.002(3) C3 0.028(3) 0.035(4) 0.020(4) 0.014(3) 0.011(3) 0.002(3) C4 0.046(4) 0.030(4) 0.047(5) 0.006(4) 0.030(4) -0.004(3) C5 0.036(4) 0.024(3) 0.038(5) -0.006(3) 0.022(3) -0.004(3) C6 0.015(3) 0.025(3) 0.020(4) 0.002(3) 0.008(2) 0.001(2) C7 0.025(3) 0.026(3) 0.030(4) -0.006(3) 0.012(3) -0.009(3) N8 0.020(2) 0.020(3) 0.015(3) -0.001(2) 0.008(2) -0.002(2) C9 0.025(3) 0.029(3) 0.017(4) 0.003(3) 0.008(3) 0.004(3) C10 0.013(3) 0.022(3) 0.023(4) 0.007(3) 0.011(3) 0.004(2) C11 0.031(3) 0.032(4) 0.016(4) 0.001(3) 0.013(3) -0.002(3) C12 0.044(4) 0.025(4) 0.049(5) 0.013(4) 0.033(4) 0.008(3) C13 0.034(4) 0.028(4) 0.026(5) 0.002(3) 0.015(3) -0.005(3) C14 0.023(3) 0.023(3) 0.018(4) 0.003(3) 0.008(3) 0.009(3) N15 0.017(2) 0.019(3) 0.015(3) -0.002(2) 0.004(2) 0.001(2) C16 0.029(3) 0.027(4) 0.026(4) -0.005(3) 0.015(3) 0.000(3) N17 0.014(2) 0.022(3) 0.020(3) 0.000(2) 0.011(2) 0.000(2) C18 0.031(3) 0.025(3) 0.025(4) 0.001(3) 0.024(3) -0.003(3) C19 0.040(4) 0.029(4) 0.042(5) 0.001(4) 0.030(3) 0.007(3) C20 0.033(4) 0.029(4) 0.039(5) 0.008(3) 0.022(3) 0.017(3) C21 0.023(3) 0.036(4) 0.039(5) 0.015(4) 0.018(3) 0.009(3) C22 0.025(3) 0.026(3) 0.021(4) 0.005(3) 0.015(3) 0.000(3) C23 0.013(3) 0.029(3) 0.015(4) 0.011(3) 0.002(2) -0.004(3) C24 0.019(3) 0.030(4) 0.024(4) 0.005(3) 0.007(3) -0.002(3) C25 0.032(4) 0.046(4) 0.020(5) 0.005(4) 0.000(3) -0.016(3) C26 0.035(4) 0.041(4) 0.014(4) -0.006(3) 0.010(3) -0.003(3) C27 0.028(3) 0.039(4) 0.023(4) -0.001(3) 0.010(3) 0.008(3) N28 0.021(2) 0.031(3) 0.014(3) 0.000(2) 0.010(2) -0.003(2) N31 0.017(2) 0.033(3) 0.014(3) 0.003(3) 0.003(2) 0.007(2) C32 0.027(3) 0.032(4) 0.037(5) 0.002(3) 0.018(3) 0.007(3) C33 0.035(4) 0.053(5) 0.030(5) -0.007(4) 0.012(3) -0.001(4) C34 0.041(4) 0.046(5) 0.042(6) -0.017(4) 0.018(4) -0.006(4) C35 0.039(4) 0.032(4) 0.049(5) -0.005(4) 0.030(4) -0.001(3) C36 0.027(3) 0.029(4) 0.034(5) -0.002(3) 0.020(3) 0.003(3) C37 0.032(3) 0.018(3) 0.042(5) 0.003(3) 0.024(3) 0.004(3) N38 0.020(2) 0.032(3) 0.019(3) 0.004(2) 0.012(2) 0.006(2) C39 0.029(3) 0.032(4) 0.021(4) 0.010(3) 0.010(3) 0.003(3) C40 0.025(3) 0.036(4) 0.021(4) 0.004(3) 0.017(3) 0.004(3) C41 0.033(4) 0.065(5) 0.017(5) 0.002(4) 0.007(3) 0.006(4) C42 0.041(4) 0.052(5) 0.022(5) -0.019(4) 0.008(3) -0.002(4) C43 0.041(4) 0.039(4) 0.033(5) -0.015(4) 0.011(3) -0.008(3) C44 0.033(4) 0.039(4) 0.032(5) -0.009(4) 0.018(3) -0.002(3) N45 0.021(2) 0.023(3) 0.026(3) -0.005(3) 0.012(2) -0.001(2) C46 0.030(3) 0.040(4) 0.039(5) -0.003(4) 0.025(3) -0.002(3) N47 0.020(2) 0.026(3) 0.023(3) 0.000(2) 0.013(2) 0.002(2) C48 0.028(3) 0.021(3) 0.025(4) -0.002(3) 0.019(3) -0.002(3) C49 0.027(3) 0.047(4) 0.035(5) 0.002(4) 0.022(3) 0.003(3) C50 0.019(3) 0.042(4) 0.053(5) -0.013(4) 0.019(3) 0.003(3) C51 0.024(3) 0.026(3) 0.041(5) -0.008(3) 0.014(3) 0.007(3) C52 0.020(3) 0.025(3) 0.023(4) 0.002(3) 0.005(3) 0.005(3) C53 0.020(3) 0.032(4) 0.013(4) -0.003(3) 0.003(2) 0.005(3) C54 0.040(4) 0.029(4) 0.037(5) 0.007(4) 0.018(3) 0.014(3) C55 0.051(4) 0.031(4) 0.048(5) 0.018(4) 0.033(4) 0.012(3) C56 0.049(4) 0.036(4) 0.047(5) 0.008(4) 0.037(4) 0.002(3) C57 0.033(3) 0.027(4) 0.034(5) -0.001(3) 0.022(3) 0.005(3) N58 0.025(3) 0.028(3) 0.016(3) 0.004(2) 0.010(2) 0.008(2) Cl1 0.0282(8) 0.0331(9) 0.0329(11) 0.0029(8) 0.0119(7) 0.0075(7) O11 0.025(2) 0.061(3) 0.027(3) -0.010(3) -0.0041(19) 0.013(2) O12 0.044(3) 0.060(3) 0.046(4) -0.022(3) 0.000(2) 0.005(3) O13 0.045(3) 0.077(4) 0.051(4) -0.008(3) 0.029(3) 0.011(3) O14 0.081(4) 0.067(4) 0.131(6) 0.062(4) 0.067(4) 0.023(3) Cl2 0.0397(10) 0.0459(11) 0.0382(13) -0.0032(10) 0.0110(8) -0.0022(9) O21 0.071(4) 0.057(4) 0.057(4) -0.026(3) 0.020(3) 0.008(3) O22 0.040(3) 0.078(4) 0.127(5) -0.057(4) 0.026(3) -0.024(3) O23 0.141(6) 0.113(6) 0.068(5) 0.036(5) 0.067(4) -0.013(5) O24 0.061(4) 0.069(4) 0.070(4) -0.008(4) -0.005(3) 0.032(3) Cl3 0.035(2) 0.024(2) 0.054(3) 0.016(2) 0.029(2) 0.0065(18) O31 0.062(6) 0.036(5) 0.035(7) 0.012(4) 0.006(5) -0.023(4) O32 0.035(4) 0.065(8) 0.070(6) -0.002(6) 0.019(4) 0.005(4) O33 0.076(5) 0.074(8) 0.048(6) 0.036(6) 0.040(4) 0.009(5) O34 0.079(6) 0.048(6) 0.127(11) -0.020(7) 0.050(7) 0.020(5) Cl3' 0.056(8) 0.086(10) 0.063(9) 0.003(7) 0.041(6) -0.011(7) Cl4 0.0499(11) 0.0417(11) 0.0334(13) 0.0068(10) 0.0151(9) -0.0068(9) O41 0.112(5) 0.088(5) 0.127(6) 0.026(5) 0.088(5) -0.014(4) O42 0.099(5) 0.128(6) 0.040(4) 0.014(4) -0.008(3) -0.042(4) O43 0.071(4) 0.060(4) 0.078(5) 0.033(4) 0.013(3) 0.003(3) O44 0.187(7) 0.069(4) 0.112(6) 0.011(5) 0.110(5) 0.025(5) N60 0.066(4) 0.055(5) 0.062(6) 0.006(4) 0.036(4) 0.004(4) C61 0.042(4) 0.040(5) 0.042(6) -0.004(4) 0.021(4) 0.002(4) C62 0.067(5) 0.060(5) 0.067(7) 0.019(5) 0.040(5) 0.033(5) O70 0.095(4) 0.095(5) 0.087(5) -0.024(4) 0.043(4) -0.025(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O 1.798(3) . ? Fe1 N15 2.101(5) . ? Fe1 N1 2.132(5) . ? Fe1 N28 2.134(5) . ? Fe1 N17 2.135(4) . ? Fe1 N8 2.212(5) . ? Fe2 O 1.803(3) . ? Fe2 N58 2.105(5) . ? Fe2 N31 2.120(5) . ? Fe2 N45 2.132(5) . ? Fe2 N47 2.135(4) . ? Fe2 N38 2.215(5) . ? N1 C2 1.332(7) . ? N1 C6 1.342(7) . ? C2 C3 1.374(8) . ? C3 C4 1.382(8) . ? C4 C5 1.370(8) . ? C5 C6 1.388(7) . ? C6 C7 1.469(8) . ? C7 N8 1.481(6) . ? N8 C9 1.476(7) . ? N8 C16 1.518(6) . ? C9 C10 1.501(7) . ? C10 N15 1.339(7) . ? C10 C11 1.378(7) . ? C11 C12 1.375(8) . ? C12 C13 1.379(9) . ? C13 C14 1.375(8) . ? C14 N15 1.343(6) . ? C16 C18 1.494(8) . ? N17 C18 1.313(7) . ? N17 C22 1.347(7) . ? C18 C19 1.403(7) . ? C19 C20 1.380(8) . ? C20 C21 1.363(8) . ? C21 C22 1.374(7) . ? C22 C23 1.465(8) . ? C23 N28 1.359(6) . ? C23 C24 1.387(7) . ? C24 C25 1.377(8) . ? C25 C26 1.370(8) . ? C26 C27 1.370(8) . ? C27 N28 1.317(7) . ? N31 C32 1.337(7) . ? N31 C36 1.351(7) . ? C32 C33 1.370(8) . ? C33 C34 1.370(9) . ? C34 C35 1.371(9) . ? C35 C36 1.387(8) . ? C36 C37 1.495(9) . ? C37 N38 1.461(7) . ? N38 C39 1.499(7) . ? N38 C46 1.527(6) . ? C39 C40 1.510(8) . ? C40 N45 1.341(7) . ? C40 C41 1.383(8) . ? C41 C42 1.380(9) . ? C42 C43 1.358(9) . ? C43 C44 1.370(8) . ? C44 N45 1.339(7) . ? C46 C48 1.480(8) . ? N47 C48 1.334(6) . ? N47 C52 1.346(7) . ? C48 C49 1.384(7) . ? C49 C50 1.401(8) . ? C50 C51 1.354(8) . ? C51 C52 1.380(7) . ? C52 C53 1.477(8) . ? C53 N58 1.361(6) . ? C53 C54 1.374(8) . ? C54 C55 1.384(8) . ? C55 C56 1.369(8) . ? C56 C57 1.376(8) . ? C57 N58 1.342(6) . ? Cl1 O13 1.398(4) . ? Cl1 O14 1.417(5) . ? Cl1 O11 1.425(4) . ? Cl1 O12 1.426(5) . ? Cl2 O23 1.401(5) . ? Cl2 O24 1.429(5) . ? Cl2 O22 1.433(5) . ? Cl2 O21 1.442(5) . ? Cl3 O31 1.420(7) . ? Cl3 O32 1.433(7) . ? Cl3 O34 1.434(7) . ? Cl3 O33 1.444(8) . ? Cl3' O32' 1.422(12) . ? Cl3' O33' 1.433(12) . ? Cl3' O31' 1.434(12) . ? Cl3' O34' 1.439(12) . ? Cl4 O42 1.390(5) . ? Cl4 O41 1.403(5) . ? Cl4 O43 1.409(5) . ? Cl4 O44 1.433(6) . ? N60 C61 1.127(8) . ? C61 C62 1.458(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Fe1 N15 95.59(16) . . ? O Fe1 N1 93.38(16) . . ? N15 Fe1 N1 153.26(18) . . ? O Fe1 N28 101.16(17) . . ? N15 Fe1 N28 99.92(17) . . ? N1 Fe1 N28 102.96(18) . . ? O Fe1 N17 175.31(18) . . ? N15 Fe1 N17 87.73(16) . . ? N1 Fe1 N17 85.04(16) . . ? N28 Fe1 N17 74.95(18) . . ? O Fe1 N8 106.45(16) . . ? N15 Fe1 N8 76.61(17) . . ? N1 Fe1 N8 76.70(18) . . ? N28 Fe1 N8 152.36(16) . . ? N17 Fe1 N8 77.51(17) . . ? O Fe2 N58 101.85(16) . . ? O Fe2 N31 95.31(16) . . ? N58 Fe2 N31 103.85(19) . . ? O Fe2 N45 94.88(16) . . ? N58 Fe2 N45 98.24(19) . . ? N31 Fe2 N45 153.16(18) . . ? O Fe2 N47 176.31(17) . . ? N58 Fe2 N47 74.77(17) . . ? N31 Fe2 N47 87.00(17) . . ? N45 Fe2 N47 84.25(17) . . ? O Fe2 N38 106.28(16) . . ? N58 Fe2 N38 151.75(16) . . ? N31 Fe2 N38 76.31(18) . . ? N45 Fe2 N38 77.01(18) . . ? N47 Fe2 N38 77.04(17) . . ? Fe1 O Fe2 174.5(2) . . ? C2 N1 C6 119.4(5) . . ? C2 N1 Fe1 124.8(4) . . ? C6 N1 Fe1 115.7(4) . . ? N1 C2 C3 123.1(6) . . ? C2 C3 C4 117.7(6) . . ? C5 C4 C3 119.8(6) . . ? C4 C5 C6 119.5(6) . . ? N1 C6 C5 120.6(6) . . ? N1 C6 C7 116.0(5) . . ? C5 C6 C7 123.4(6) . . ? C6 C7 N8 112.4(5) . . ? C9 N8 C7 112.6(4) . . ? C9 N8 C16 109.9(4) . . ? C7 N8 C16 111.0(4) . . ? C9 N8 Fe1 106.2(3) . . ? C7 N8 Fe1 105.4(3) . . ? C16 N8 Fe1 111.5(3) . . ? N8 C9 C10 110.3(4) . . ? N15 C10 C11 121.5(5) . . ? N15 C10 C9 116.5(5) . . ? C11 C10 C9 121.9(5) . . ? C12 C11 C10 119.5(6) . . ? C11 C12 C13 119.3(6) . . ? C14 C13 C12 118.3(6) . . ? N15 C14 C13 122.7(5) . . ? C10 N15 C14 118.7(5) . . ? C10 N15 Fe1 116.0(4) . . ? C14 N15 Fe1 124.6(4) . . ? C18 C16 N8 113.0(5) . . ? C18 N17 C22 122.2(5) . . ? C18 N17 Fe1 119.1(4) . . ? C22 N17 Fe1 118.4(4) . . ? N17 C18 C19 120.7(6) . . ? N17 C18 C16 117.7(5) . . ? C19 C18 C16 121.5(6) . . ? C20 C19 C18 116.9(6) . . ? C21 C20 C19 121.5(6) . . ? C20 C21 C22 119.0(6) . . ? N17 C22 C21 119.6(6) . . ? N17 C22 C23 113.6(5) . . ? C21 C22 C23 126.7(6) . . ? N28 C23 C24 120.7(6) . . ? N28 C23 C22 115.7(5) . . ? C24 C23 C22 123.7(5) . . ? C25 C24 C23 119.3(6) . . ? C26 C25 C24 119.6(6) . . ? C25 C26 C27 117.8(6) . . ? N28 C27 C26 124.3(6) . . ? C27 N28 C23 118.3(5) . . ? C27 N28 Fe1 124.6(4) . . ? C23 N28 Fe1 117.0(4) . . ? C32 N31 C36 118.5(6) . . ? C32 N31 Fe2 125.4(4) . . ? C36 N31 Fe2 116.1(4) . . ? N31 C32 C33 122.8(6) . . ? C32 C33 C34 118.5(7) . . ? C33 C34 C35 120.0(7) . . ? C34 C35 C36 118.8(7) . . ? N31 C36 C35 121.3(6) . . ? N31 C36 C37 114.9(6) . . ? C35 C36 C37 123.7(6) . . ? N38 C37 C36 110.7(5) . . ? C37 N38 C39 111.6(5) . . ? C37 N38 C46 111.1(4) . . ? C39 N38 C46 110.2(5) . . ? C37 N38 Fe2 105.8(3) . . ? C39 N38 Fe2 106.0(3) . . ? C46 N38 Fe2 112.0(3) . . ? N38 C39 C40 110.1(5) . . ? N45 C40 C41 121.2(6) . . ? N45 C40 C39 117.5(5) . . ? C41 C40 C39 121.1(6) . . ? C42 C41 C40 117.8(7) . . ? C43 C42 C41 121.4(6) . . ? C42 C43 C44 117.7(7) . . ? N45 C44 C43 122.5(7) . . ? C44 N45 C40 119.3(5) . . ? C44 N45 Fe2 125.1(4) . . ? C40 N45 Fe2 114.8(4) . . ? C48 C46 N38 113.3(4) . . ? C48 N47 C52 121.3(5) . . ? C48 N47 Fe2 119.8(4) . . ? C52 N47 Fe2 118.6(3) . . ? N47 C48 C49 120.6(5) . . ? N47 C48 C46 117.2(5) . . ? C49 C48 C46 122.2(5) . . ? C48 C49 C50 118.1(5) . . ? C51 C50 C49 120.3(5) . . ? C50 C51 C52 119.3(6) . . ? N47 C52 C51 120.3(5) . . ? N47 C52 C53 113.7(5) . . ? C51 C52 C53 125.8(6) . . ? N58 C53 C54 121.8(5) . . ? N58 C53 C52 114.0(5) . . ? C54 C53 C52 124.2(5) . . ? C53 C54 C55 119.0(6) . . ? C56 C55 C54 119.5(6) . . ? C55 C56 C57 118.8(5) . . ? N58 C57 C56 122.9(5) . . ? C57 N58 C53 118.0(5) . . ? C57 N58 Fe2 123.2(4) . . ? C53 N58 Fe2 118.8(4) . . ? O13 Cl1 O14 109.4(3) . . ? O13 Cl1 O11 109.9(3) . . ? O14 Cl1 O11 110.1(3) . . ? O13 Cl1 O12 109.1(3) . . ? O14 Cl1 O12 109.0(4) . . ? O11 Cl1 O12 109.4(3) . . ? O23 Cl2 O24 107.8(4) . . ? O23 Cl2 O22 109.7(4) . . ? O24 Cl2 O22 109.3(4) . . ? O23 Cl2 O21 109.3(4) . . ? O24 Cl2 O21 111.6(3) . . ? O22 Cl2 O21 109.0(3) . . ? O31 Cl3 O32 110.0(6) . . ? O31 Cl3 O34 110.3(6) . . ? O32 Cl3 O34 108.0(6) . . ? O31 Cl3 O33 109.3(6) . . ? O32 Cl3 O33 110.1(5) . . ? O34 Cl3 O33 109.2(6) . . ? O32' Cl3' O33' 111.3(11) . . ? O32' Cl3' O31' 109.7(11) . . ? O33' Cl3' O31' 109.6(11) . . ? O32' Cl3' O34' 109.5(11) . . ? O33' Cl3' O34' 107.8(10) . . ? O31' Cl3' O34' 108.8(11) . . ? O42 Cl4 O41 110.4(4) . . ? O42 Cl4 O43 111.1(4) . . ? O41 Cl4 O43 111.3(4) . . ? O42 Cl4 O44 106.4(5) . . ? O41 Cl4 O44 108.8(4) . . ? O43 Cl4 O44 108.5(4) . . ? N60 C61 C62 178.0(9) . . ? _diffrn_measured_fraction_theta_max 0.731 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.868 _refine_diff_density_max 0.806 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.104 #===END