# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mallayan Andavar' _publ_contact_author_email PALANIM51@YAHOO.COM loop_ _publ_author_name M.Andavar E.Suresh K.Visvaganesan data_12mpkvm _database_code_depnum_ccdc_archive 'CCDC 683417' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H52 Cl2 Fe2 N6 O13' _chemical_formula_weight 1079.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2855(17) _cell_length_b 19.283(3) _cell_length_c 21.682(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.900(3) _cell_angle_gamma 90.00 _cell_volume 4986.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATES _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'BRUKER SAMRT APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29731 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.28 _reflns_number_total 11534 _reflns_number_gt 6587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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 w=1/[\s^2^(Fo^2^)+(0.0881P)^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 11534 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1778 _refine_ls_wR_factor_gt 0.1523 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O7 O 0.0864(5) 0.2309(2) 1.0022(2) 0.168(2) Uani 1 d . . . Fe1 Fe 0.39665(4) 0.07299(3) 0.19516(2) 0.04419(16) Uani 1 d . . . Fe2 Fe 0.57141(4) 0.00513(3) 0.30544(2) 0.04489(17) Uani 1 d . . . Cl1 Cl 0.00931(12) 0.20245(8) 0.94965(7) 0.0890(4) Uani 1 d . . . O3 O 0.5191(2) -0.07898(13) 0.25128(12) 0.0532(6) Uani 1 d . . . C33 C 0.4601(3) -0.0786(2) 0.19451(17) 0.0466(9) Uani 1 d . . . O1 O 0.4504(2) 0.05929(13) 0.27877(11) 0.0498(6) Uani 1 d . . . O4 O 0.66007(19) 0.03879(14) 0.24250(11) 0.0495(6) Uani 1 d . . . O2 O 0.4221(2) -0.02377(13) 0.16433(11) 0.0524(6) Uani 1 d . . . N2 N 0.3121(2) 0.10442(16) 0.09325(13) 0.0445(7) Uani 1 d . . . N6 N 0.5126(2) -0.04076(17) 0.38118(13) 0.0495(8) Uani 1 d . . . O5 O 0.54067(19) 0.10649(13) 0.17447(11) 0.0501(6) Uani 1 d . . . N5 N 0.7162(2) -0.06663(16) 0.35480(14) 0.0489(7) Uani 1 d . . . N4 N 0.6768(3) 0.07321(17) 0.36932(14) 0.0500(8) Uani 1 d . . . N1 N 0.3423(2) 0.17662(16) 0.20344(14) 0.0507(8) Uani 1 d . . . C40 C 0.6385(3) 0.08521(19) 0.20043(16) 0.0430(8) Uani 1 d . . . C41 C 0.7343(3) 0.11700(19) 0.18001(16) 0.0445(8) Uani 1 d . . . N3 N 0.2291(2) 0.03600(17) 0.18411(15) 0.0500(8) Uani 1 d . . . C8 C 0.1581(3) 0.0423(2) 0.12736(18) 0.0495(9) Uani 1 d . . . C34 C 0.4343(3) -0.1460(2) 0.16199(17) 0.0488(9) Uani 1 d . . . C21 C 0.7700(3) 0.0483(2) 0.40722(17) 0.0504(9) Uani 1 d . . . C6 C 0.3349(3) 0.1799(2) 0.09185(17) 0.0530(10) Uani 1 d . . . H6A H 0.2876 0.2002 0.0538 0.064 Uiso 1 calc R . . H6B H 0.4125 0.1872 0.0907 0.064 Uiso 1 calc R . . C46 C 0.8424(3) 0.1084(2) 0.2165(2) 0.0641(11) Uani 1 d . . . H46 H 0.8547 0.0833 0.2542 0.077 Uiso 1 calc R . . C13 C 0.3591(3) 0.0646(2) 0.04690(16) 0.0561(10) Uani 1 d . . . H13A H 0.3390 0.0162 0.0498 0.067 Uiso 1 calc R . . H13B H 0.4402 0.0675 0.0602 0.067 Uiso 1 calc R . . C42 C 0.7183(3) 0.1544(2) 0.12445(18) 0.0573(10) Uani 1 d . . . H42 H 0.6460 0.1607 0.0994 0.069 Uiso 1 calc R . . C5 C 0.3124(3) 0.2140(2) 0.14925(19) 0.0565(10) Uani 1 d . . . C23 C 0.6574(3) -0.1241(2) 0.37910(19) 0.0565(10) Uani 1 d . . . H23A H 0.7113 -0.1507 0.4102 0.068 Uiso 1 calc R . . H23B H 0.6238 -0.1548 0.3443 0.068 Uiso 1 calc R . . C35 C 0.3457(3) -0.1524(2) 0.10888(19) 0.0629(11) Uani 1 d . . . H35 H 0.3018 -0.1139 0.0936 0.075 Uiso 1 calc R . . C28 C 0.4268(3) -0.0172(2) 0.40285(19) 0.0590(11) Uani 1 d . . . H28 H 0.3882 0.0217 0.3839 0.071 Uiso 1 calc R . . C39 C 0.4989(4) -0.2039(2) 0.1833(2) 0.0693(12) Uani 1 d . . . H39 H 0.5582 -0.2011 0.2191 0.083 Uiso 1 calc R . . C29 C 0.7789(3) -0.0933(2) 0.30825(19) 0.0558(10) Uani 1 d . . . H29A H 0.8337 -0.0585 0.3042 0.067 Uiso 1 calc R . . H29B H 0.7260 -0.0970 0.2672 0.067 Uiso 1 calc R . . C43 C 0.8077(4) 0.1824(3) 0.1056(2) 0.0736(13) Uani 1 d . . . H43 H 0.7956 0.2070 0.0677 0.088 Uiso 1 calc R . . C24 C 0.5686(3) -0.0972(2) 0.40895(18) 0.0550(10) Uani 1 d . . . C4 C 0.2651(4) 0.2783(3) 0.1482(2) 0.0821(15) Uani 1 d . . . H4 H 0.2448 0.3033 0.1105 0.099 Uiso 1 calc R . . O6 O -0.0556(3) 0.2561(2) 0.91688(18) 0.1171(14) Uani 1 d . . . C1 C 0.3266(4) 0.2048(2) 0.2575(2) 0.0687(12) Uani 1 d . . . H1 H 0.3484 0.1797 0.2951 0.082 Uiso 1 calc R . . C44 C 0.9140(4) 0.1746(3) 0.1420(3) 0.0798(14) Uani 1 d . . . H44 H 0.9742 0.1946 0.1295 0.096 Uiso 1 calc R . . C30 C 0.8401(4) -0.1628(2) 0.3218(2) 0.0732(13) Uani 1 d . . . H30 H 0.7843 -0.1983 0.3245 0.088 Uiso 1 calc R . . C17 C 0.6581(4) 0.1420(2) 0.3685(2) 0.0668(12) Uani 1 d . . . H17 H 0.5924 0.1594 0.3424 0.080 Uiso 1 calc R . . C25 C 0.5392(4) -0.1302(2) 0.4591(2) 0.0693(12) Uani 1 d . . . H25 H 0.5788 -0.1688 0.4780 0.083 Uiso 1 calc R . . C26 C 0.4508(4) -0.1050(3) 0.4806(2) 0.0782(14) Uani 1 d . . . H26 H 0.4301 -0.1264 0.5145 0.094 Uiso 1 calc R . . C19 C 0.8273(4) 0.1601(3) 0.4449(3) 0.0897(16) Uani 1 d . . . H19 H 0.8776 0.1896 0.4714 0.108 Uiso 1 calc R . . C20 C 0.8476(4) 0.0915(3) 0.4460(2) 0.0747(13) Uani 1 d . . . H20 H 0.9124 0.0733 0.4724 0.090 Uiso 1 calc R . . C14 C 0.3235(4) 0.0862(3) -0.02348(19) 0.0720(13) Uani 1 d . . . H14 H 0.2518 0.1108 -0.0305 0.086 Uiso 1 calc R . . C22 C 0.7900(4) -0.0281(2) 0.4089(2) 0.0652(11) Uani 1 d . . . H22A H 0.7781 -0.0464 0.4485 0.078 Uiso 1 calc R . . H22B H 0.8677 -0.0365 0.4086 0.078 Uiso 1 calc R . . C3 C 0.2479(5) 0.3058(3) 0.2042(3) 0.1035(19) Uani 1 d . . . H3 H 0.2146 0.3491 0.2042 0.124 Uiso 1 calc R . . C12 C 0.2010(4) -0.0039(2) 0.2278(2) 0.0699(12) Uani 1 d . . . H12 H 0.2512 -0.0087 0.2672 0.084 Uiso 1 calc R . . C9 C 0.0573(4) 0.0081(3) 0.1122(2) 0.0737(13) Uani 1 d . . . H9 H 0.0089 0.0128 0.0722 0.088 Uiso 1 calc R . . C27 C 0.3931(4) -0.0484(3) 0.4523(2) 0.0704(13) Uani 1 d . . . H27 H 0.3322 -0.0313 0.4661 0.084 Uiso 1 calc R . . C18 C 0.7321(4) 0.1867(3) 0.4046(2) 0.0828(14) Uani 1 d . . . H18 H 0.7189 0.2343 0.4022 0.099 Uiso 1 calc R . . C31 C 0.8871(5) -0.1798(3) 0.2644(3) 0.111(2) Uani 1 d . . . H31A H 0.9455 -0.1475 0.2623 0.167 Uiso 1 calc R . . H31B H 0.8282 -0.1764 0.2263 0.167 Uiso 1 calc R . . H31C H 0.9169 -0.2260 0.2685 0.167 Uiso 1 calc R . . C15 C 0.4074(6) 0.1333(4) -0.0422(3) 0.129(2) Uani 1 d . . . H15A H 0.4767 0.1088 -0.0386 0.193 Uiso 1 calc R . . H15B H 0.4201 0.1729 -0.0146 0.193 Uiso 1 calc R . . H15C H 0.3791 0.1483 -0.0853 0.193 Uiso 1 calc R . . C2 C 0.2802(4) 0.2687(3) 0.2592(2) 0.0923(17) Uani 1 d . . . H2 H 0.2707 0.2868 0.2973 0.111 Uiso 1 calc R . . C11 C 0.1005(5) -0.0381(3) 0.2166(3) 0.0938(17) Uani 1 d . . . H11 H 0.0809 -0.0640 0.2485 0.113 Uiso 1 calc R . . C10 C 0.0297(5) -0.0334(3) 0.1578(3) 0.0990(18) Uani 1 d . . . H10 H -0.0372 -0.0582 0.1485 0.119 Uiso 1 calc R . . C45 C 0.9314(4) 0.1367(3) 0.1976(2) 0.0794(14) Uani 1 d . . . H45 H 1.0038 0.1303 0.2222 0.095 Uiso 1 calc R . . C36 C 0.3225(5) -0.2146(3) 0.0789(2) 0.0898(16) Uani 1 d . . . H36 H 0.2623 -0.2185 0.0437 0.108 Uiso 1 calc R . . C32 C 0.9317(4) -0.1657(3) 0.3832(3) 0.0991(18) Uani 1 d . . . H32A H 0.9668 -0.2105 0.3872 0.149 Uiso 1 calc R . . H32B H 0.8992 -0.1579 0.4187 0.149 Uiso 1 calc R . . H32C H 0.9866 -0.1305 0.3824 0.149 Uiso 1 calc R . . O9 O -0.0530(4) 0.1493(3) 0.9682(3) 0.1487(18) Uani 1 d . . . C38 C 0.4751(5) -0.2658(3) 0.1511(3) 0.0939(17) Uani 1 d . . . H38 H 0.5202 -0.3043 0.1646 0.113 Uiso 1 calc R . . O8 O 0.0736(4) 0.1719(3) 0.9131(3) 0.180(3) Uani 1 d . . . Cl2 Cl 0.39000(11) 0.52702(8) 0.11845(7) 0.0855(4) Uani 1 d . . . O10 O 0.3592(3) 0.4572(2) 0.1286(2) 0.1223(14) Uani 1 d . . . O12 O 0.4971(3) 0.5430(3) 0.1542(2) 0.1321(16) Uani 1 d . . . O11 O 0.3834(5) 0.5407(4) 0.0566(2) 0.183(3) Uani 1 d . . . O13 O 0.3139(4) 0.5701(3) 0.1403(3) 0.162(2) Uani 1 d . . . C7 C 0.1889(3) 0.0928(2) 0.08184(19) 0.0612(11) Uani 1 d . . . H7A H 0.1607 0.0758 0.0389 0.073 Uiso 1 calc R . . H7B H 0.1525 0.1368 0.0853 0.073 Uiso 1 calc R . . C37 C 0.3869(6) -0.2714(3) 0.1002(3) 0.0991(18) Uani 1 d . . . H37 H 0.3703 -0.3138 0.0798 0.119 Uiso 1 calc R . . C16 C 0.3069(6) 0.0221(3) -0.0653(3) 0.131(3) Uani 1 d . . . H16A H 0.2823 0.0357 -0.1090 0.196 Uiso 1 calc R . . H16B H 0.2514 -0.0073 -0.0542 0.196 Uiso 1 calc R . . H16C H 0.3765 -0.0027 -0.0590 0.196 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O7 0.213(5) 0.091(3) 0.137(4) -0.020(3) -0.083(4) 0.037(3) Fe1 0.0457(3) 0.0452(3) 0.0408(3) 0.0057(2) 0.0087(2) 0.0058(2) Fe2 0.0497(3) 0.0472(3) 0.0365(3) 0.0076(2) 0.0078(2) 0.0029(2) Cl1 0.0818(9) 0.0801(10) 0.0948(9) -0.0116(8) 0.0012(8) 0.0183(8) O3 0.0625(16) 0.0452(16) 0.0469(15) 0.0054(12) 0.0036(13) 0.0033(12) C33 0.046(2) 0.050(2) 0.047(2) 0.0075(18) 0.0180(17) 0.0008(17) O1 0.0526(14) 0.0569(17) 0.0404(13) 0.0053(11) 0.0124(11) 0.0073(12) O4 0.0491(14) 0.0562(17) 0.0455(14) 0.0156(12) 0.0159(11) 0.0095(12) O2 0.0642(16) 0.0461(16) 0.0441(14) 0.0065(12) 0.0076(12) 0.0118(13) N2 0.0447(16) 0.050(2) 0.0393(16) 0.0021(13) 0.0107(13) 0.0051(14) N6 0.0497(18) 0.059(2) 0.0399(17) 0.0085(15) 0.0102(14) 0.0002(16) O5 0.0459(14) 0.0498(16) 0.0527(15) 0.0138(12) 0.0085(12) 0.0050(12) N5 0.0551(18) 0.0435(19) 0.0465(18) 0.0059(14) 0.0090(15) 0.0021(15) N4 0.0551(18) 0.048(2) 0.0478(18) 0.0067(14) 0.0144(15) 0.0018(15) N1 0.0569(19) 0.047(2) 0.0461(18) -0.0040(15) 0.0081(15) 0.0069(15) C40 0.050(2) 0.040(2) 0.0363(19) 0.0017(15) 0.0064(16) 0.0027(17) C41 0.050(2) 0.044(2) 0.0410(19) -0.0019(16) 0.0137(17) 0.0028(17) N3 0.0497(18) 0.050(2) 0.0518(19) 0.0064(15) 0.0147(15) 0.0004(15) C8 0.051(2) 0.047(2) 0.051(2) -0.0106(18) 0.0142(18) -0.0008(18) C34 0.058(2) 0.046(2) 0.043(2) 0.0042(17) 0.0154(18) -0.0059(19) C21 0.048(2) 0.060(3) 0.043(2) 0.0007(18) 0.0117(17) 0.0024(19) C6 0.065(2) 0.042(2) 0.051(2) 0.0068(17) 0.0099(19) 0.0096(19) C46 0.055(2) 0.079(3) 0.058(3) 0.008(2) 0.012(2) -0.002(2) C13 0.071(3) 0.054(3) 0.043(2) -0.0012(18) 0.0127(19) 0.015(2) C42 0.060(2) 0.058(3) 0.054(2) 0.0091(19) 0.013(2) -0.004(2) C5 0.061(2) 0.049(3) 0.057(2) -0.0010(19) 0.008(2) 0.007(2) C23 0.068(2) 0.049(3) 0.056(2) 0.0144(19) 0.021(2) 0.005(2) C35 0.067(3) 0.062(3) 0.058(3) 0.003(2) 0.012(2) -0.006(2) C28 0.051(2) 0.076(3) 0.049(2) 0.003(2) 0.0098(19) 0.002(2) C39 0.091(3) 0.055(3) 0.058(3) 0.003(2) 0.010(2) 0.007(2) C29 0.054(2) 0.054(3) 0.064(3) 0.0093(19) 0.022(2) 0.0006(19) C43 0.091(3) 0.073(3) 0.064(3) 0.018(2) 0.032(3) 0.001(3) C24 0.063(3) 0.055(3) 0.046(2) 0.0061(18) 0.0127(19) -0.003(2) C4 0.110(4) 0.061(3) 0.067(3) 0.000(2) 0.005(3) 0.031(3) O6 0.109(3) 0.118(3) 0.100(3) 0.022(2) -0.024(2) 0.025(2) C1 0.075(3) 0.078(3) 0.051(2) -0.010(2) 0.011(2) 0.013(2) C44 0.082(3) 0.076(4) 0.095(4) 0.002(3) 0.049(3) -0.011(3) C30 0.074(3) 0.058(3) 0.095(3) 0.012(2) 0.033(3) 0.012(2) C17 0.073(3) 0.057(3) 0.070(3) 0.003(2) 0.016(2) 0.006(2) C25 0.092(3) 0.059(3) 0.064(3) 0.015(2) 0.034(3) -0.002(2) C26 0.103(4) 0.080(4) 0.058(3) 0.011(3) 0.032(3) -0.017(3) C19 0.076(3) 0.071(4) 0.110(4) -0.026(3) -0.003(3) -0.009(3) C20 0.061(3) 0.068(3) 0.086(3) -0.017(3) 0.001(2) 0.001(2) C14 0.082(3) 0.091(4) 0.045(2) 0.008(2) 0.020(2) 0.034(3) C22 0.064(3) 0.058(3) 0.064(3) 0.005(2) -0.002(2) 0.003(2) C3 0.132(5) 0.076(4) 0.092(4) -0.021(3) 0.005(4) 0.047(4) C12 0.069(3) 0.069(3) 0.073(3) 0.016(2) 0.020(2) -0.009(2) C9 0.069(3) 0.084(4) 0.068(3) -0.009(3) 0.014(2) -0.022(3) C27 0.068(3) 0.094(4) 0.057(3) -0.004(3) 0.030(2) -0.008(3) C18 0.096(4) 0.052(3) 0.097(4) -0.011(3) 0.018(3) -0.004(3) C31 0.116(4) 0.083(4) 0.161(6) 0.008(4) 0.085(4) 0.022(3) C15 0.179(6) 0.146(6) 0.083(4) 0.042(4) 0.071(4) 0.010(5) C2 0.112(4) 0.087(4) 0.073(3) -0.031(3) 0.012(3) 0.039(3) C11 0.098(4) 0.092(4) 0.094(4) 0.013(3) 0.027(3) -0.038(3) C10 0.087(4) 0.096(5) 0.112(5) -0.011(4) 0.022(4) -0.048(3) C45 0.052(3) 0.097(4) 0.092(4) 0.003(3) 0.022(2) -0.001(3) C36 0.112(4) 0.083(4) 0.064(3) -0.008(3) 0.001(3) -0.025(3) C32 0.076(3) 0.072(4) 0.141(5) 0.023(3) 0.008(3) 0.028(3) O9 0.129(4) 0.130(4) 0.183(5) 0.033(4) 0.029(3) 0.000(3) C38 0.149(5) 0.046(3) 0.084(4) -0.001(3) 0.024(4) 0.014(3) O8 0.128(4) 0.145(5) 0.292(7) -0.101(5) 0.097(4) -0.019(3) Cl2 0.0683(8) 0.0934(11) 0.0893(10) -0.0069(8) 0.0080(7) -0.0104(7) O10 0.128(3) 0.074(3) 0.150(4) -0.008(3) 0.004(3) -0.008(2) O12 0.088(3) 0.186(5) 0.106(3) -0.035(3) -0.009(2) -0.033(3) O11 0.211(6) 0.247(7) 0.070(3) 0.001(3) -0.007(3) -0.098(5) O13 0.123(4) 0.099(4) 0.291(7) 0.024(4) 0.100(4) 0.013(3) C7 0.051(2) 0.077(3) 0.056(2) 0.011(2) 0.0123(19) -0.001(2) C37 0.158(6) 0.060(4) 0.076(4) -0.016(3) 0.021(4) -0.018(4) C16 0.189(7) 0.130(6) 0.060(3) -0.023(4) 0.005(4) 0.032(5) _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 O7 Cl1 1.405(4) . ? Fe1 O1 1.794(2) . ? Fe1 O2 2.031(3) . ? Fe1 O5 2.032(2) . ? Fe1 N1 2.128(3) . ? Fe1 N3 2.137(3) . ? Fe1 N2 2.286(3) . ? Fe2 O1 1.795(2) . ? Fe2 O3 2.015(3) . ? Fe2 O4 2.046(2) . ? Fe2 N4 2.111(3) . ? Fe2 N6 2.138(3) . ? Fe2 N5 2.305(3) . ? Cl1 O8 1.378(5) . ? Cl1 O6 1.392(4) . ? Cl1 O9 1.396(5) . ? O3 C33 1.269(4) . ? C33 O2 1.272(4) . ? C33 C34 1.475(5) . ? O4 C40 1.260(4) . ? N2 C6 1.483(5) . ? N2 C13 1.488(4) . ? N2 C7 1.490(5) . ? N6 C28 1.333(5) . ? N6 C24 1.350(5) . ? O5 C40 1.267(4) . ? N5 C23 1.487(5) . ? N5 C22 1.496(5) . ? N5 C29 1.500(5) . ? N4 C21 1.328(4) . ? N4 C17 1.345(5) . ? N1 C1 1.347(5) . ? N1 C5 1.352(5) . ? C40 C41 1.485(5) . ? C41 C42 1.377(5) . ? C41 C46 1.383(5) . ? N3 C12 1.329(5) . ? N3 C8 1.332(5) . ? C8 C9 1.371(5) . ? C8 C7 1.499(5) . ? C34 C39 1.385(6) . ? C34 C35 1.387(5) . ? C21 C20 1.388(6) . ? C21 C22 1.492(6) . ? C6 C5 1.492(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C46 C45 1.370(6) . ? C46 H46 0.9300 . ? C13 C14 1.540(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C42 C43 1.371(6) . ? C42 H42 0.9300 . ? C5 C4 1.367(6) . ? C23 C24 1.489(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C35 C36 1.362(7) . ? C35 H35 0.9300 . ? C28 C27 1.377(6) . ? C28 H28 0.9300 . ? C39 C38 1.377(6) . ? C39 H39 0.9300 . ? C29 C30 1.530(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C43 C44 1.361(6) . ? C43 H43 0.9300 . ? C24 C25 1.381(5) . ? C4 C3 1.386(7) . ? C4 H4 0.9300 . ? C1 C2 1.362(6) . ? C1 H1 0.9300 . ? C44 C45 1.382(7) . ? C44 H44 0.9300 . ? C30 C32 1.523(6) . ? C30 C31 1.528(7) . ? C30 H30 0.9800 . ? C17 C18 1.357(6) . ? C17 H17 0.9300 . ? C25 C26 1.370(6) . ? C25 H25 0.9300 . ? C26 C27 1.363(7) . ? C26 H26 0.9300 . ? C19 C20 1.344(6) . ? C19 C18 1.382(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C14 C15 1.501(7) . ? C14 C16 1.517(7) . ? C14 H14 0.9800 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C3 C2 1.367(7) . ? C3 H3 0.9300 . ? C12 C11 1.369(6) . ? C12 H12 0.9300 . ? C9 C10 1.376(7) . ? C9 H9 0.9300 . ? C27 H27 0.9300 . ? C18 H18 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C2 H2 0.9300 . ? C11 C10 1.363(7) . ? C11 H11 0.9300 . ? C10 H10 0.9300 . ? C45 H45 0.9300 . ? C36 C37 1.364(8) . ? C36 H36 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C38 C37 1.352(7) . ? C38 H38 0.9300 . ? Cl2 O11 1.350(5) . ? Cl2 O12 1.392(4) . ? Cl2 O13 1.414(5) . ? Cl2 O10 1.431(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C37 H37 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 98.57(11) . . ? O1 Fe1 O5 98.13(10) . . ? O2 Fe1 O5 90.48(11) . . ? O1 Fe1 N1 95.73(12) . . ? O2 Fe1 N1 165.12(10) . . ? O5 Fe1 N1 91.58(11) . . ? O1 Fe1 N3 100.07(11) . . ? O2 Fe1 N3 82.93(11) . . ? O5 Fe1 N3 161.37(11) . . ? N1 Fe1 N3 90.54(12) . . ? O1 Fe1 N2 170.90(11) . . ? O2 Fe1 N2 89.75(10) . . ? O5 Fe1 N2 85.41(10) . . ? N1 Fe1 N2 75.73(11) . . ? N3 Fe1 N2 77.18(11) . . ? O1 Fe2 O3 99.04(11) . . ? O1 Fe2 O4 97.65(10) . . ? O3 Fe2 O4 90.74(11) . . ? O1 Fe2 N4 100.35(12) . . ? O3 Fe2 N4 160.45(11) . . ? O4 Fe2 N4 84.23(11) . . ? O1 Fe2 N6 94.69(11) . . ? O3 Fe2 N6 89.73(11) . . ? O4 Fe2 N6 167.42(10) . . ? N4 Fe2 N6 91.18(12) . . ? O1 Fe2 N5 170.47(11) . . ? O3 Fe2 N5 83.67(10) . . ? O4 Fe2 N5 91.43(10) . . ? N4 Fe2 N5 77.61(12) . . ? N6 Fe2 N5 76.13(11) . . ? O8 Cl1 O6 111.2(4) . . ? O8 Cl1 O9 106.4(4) . . ? O6 Cl1 O9 113.9(3) . . ? O8 Cl1 O7 105.3(4) . . ? O6 Cl1 O7 108.4(3) . . ? O9 Cl1 O7 111.2(4) . . ? C33 O3 Fe2 126.0(2) . . ? O3 C33 O2 123.8(4) . . ? O3 C33 C34 117.8(3) . . ? O2 C33 C34 118.4(3) . . ? Fe1 O1 Fe2 119.11(13) . . ? C40 O4 Fe2 130.9(2) . . ? C33 O2 Fe1 131.4(2) . . ? C6 N2 C13 112.7(3) . . ? C6 N2 C7 109.5(3) . . ? C13 N2 C7 110.7(3) . . ? C6 N2 Fe1 103.6(2) . . ? C13 N2 Fe1 110.8(2) . . ? C7 N2 Fe1 109.2(2) . . ? C28 N6 C24 118.6(3) . . ? C28 N6 Fe2 124.9(3) . . ? C24 N6 Fe2 116.5(2) . . ? C40 O5 Fe1 125.6(2) . . ? C23 N5 C22 110.3(3) . . ? C23 N5 C29 110.7(3) . . ? C22 N5 C29 112.7(3) . . ? C23 N5 Fe2 103.0(2) . . ? C22 N5 Fe2 108.7(2) . . ? C29 N5 Fe2 110.9(2) . . ? C21 N4 C17 118.9(4) . . ? C21 N4 Fe2 118.8(3) . . ? C17 N4 Fe2 121.9(3) . . ? C1 N1 C5 118.4(4) . . ? C1 N1 Fe1 124.5(3) . . ? C5 N1 Fe1 116.9(2) . . ? O4 C40 O5 124.3(3) . . ? O4 C40 C41 117.7(3) . . ? O5 C40 C41 118.0(3) . . ? C42 C41 C46 118.6(4) . . ? C42 C41 C40 121.3(3) . . ? C46 C41 C40 120.0(3) . . ? C12 N3 C8 119.2(3) . . ? C12 N3 Fe1 121.4(3) . . ? C8 N3 Fe1 118.2(2) . . ? N3 C8 C9 122.1(4) . . ? N3 C8 C7 117.0(3) . . ? C9 C8 C7 120.7(4) . . ? C39 C34 C35 118.5(4) . . ? C39 C34 C33 120.7(4) . . ? C35 C34 C33 120.8(4) . . ? N4 C21 C20 121.5(4) . . ? N4 C21 C22 119.0(3) . . ? C20 C21 C22 119.5(4) . . ? N2 C6 C5 110.0(3) . . ? N2 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N2 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C45 C46 C41 120.4(4) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? N2 C13 C14 117.8(3) . . ? N2 C13 H13A 107.9 . . ? C14 C13 H13A 107.9 . . ? N2 C13 H13B 107.9 . . ? C14 C13 H13B 107.9 . . ? H13A C13 H13B 107.2 . . ? C43 C42 C41 120.7(4) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? N1 C5 C4 121.6(4) . . ? N1 C5 C6 115.1(3) . . ? C4 C5 C6 123.4(4) . . ? N5 C23 C24 111.4(3) . . ? N5 C23 H23A 109.4 . . ? C24 C23 H23A 109.4 . . ? N5 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C36 C35 C34 120.5(4) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? N6 C28 C27 122.5(4) . . ? N6 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? C38 C39 C34 119.7(4) . . ? C38 C39 H39 120.2 . . ? C34 C39 H39 120.2 . . ? N5 C29 C30 118.6(3) . . ? N5 C29 H29A 107.7 . . ? C30 C29 H29A 107.7 . . ? N5 C29 H29B 107.7 . . ? C30 C29 H29B 107.7 . . ? H29A C29 H29B 107.1 . . ? C44 C43 C42 120.6(4) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? N6 C24 C25 121.4(4) . . ? N6 C24 C23 115.8(3) . . ? C25 C24 C23 122.7(4) . . ? C5 C4 C3 119.1(5) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C1 C2 122.5(4) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C43 C44 C45 119.3(4) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C32 C30 C31 111.1(4) . . ? C32 C30 C29 115.2(4) . . ? C31 C30 C29 107.1(4) . . ? C32 C30 H30 107.7 . . ? C31 C30 H30 107.7 . . ? C29 C30 H30 107.7 . . ? N4 C17 C18 122.1(4) . . ? N4 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C26 C25 C24 118.9(4) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C27 C26 C25 120.0(4) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C20 C19 C18 120.2(5) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 118.9(4) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C15 C14 C16 109.6(5) . . ? C15 C14 C13 112.4(4) . . ? C16 C14 C13 109.7(4) . . ? C15 C14 H14 108.4 . . ? C16 C14 H14 108.4 . . ? C13 C14 H14 108.4 . . ? C21 C22 N5 113.9(3) . . ? C21 C22 H22A 108.8 . . ? N5 C22 H22A 108.8 . . ? C21 C22 H22B 108.8 . . ? N5 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C2 C3 C4 119.4(5) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? N3 C12 C11 122.0(5) . . ? N3 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C8 C9 C10 118.1(5) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? C26 C27 C28 118.6(4) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C17 C18 C19 118.4(5) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C1 C2 C3 119.0(5) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C10 C11 C12 118.7(5) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C11 C10 C9 119.9(5) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C46 C45 C44 120.3(4) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C35 C36 C37 120.5(5) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C37 C38 C39 120.9(5) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? O11 Cl2 O12 109.5(3) . . ? O11 Cl2 O13 109.4(4) . . ? O12 Cl2 O13 107.2(3) . . ? O11 Cl2 O10 112.4(3) . . ? O12 Cl2 O10 111.9(3) . . ? O13 Cl2 O10 106.3(3) . . ? N2 C7 C8 113.3(3) . . ? N2 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N2 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C38 C37 C36 119.9(5) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 0.643 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.079 # Attachment '4.cif' data_14mpkvm _database_code_depnum_ccdc_archive 'CCDC 683418' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H48 Cl2 Fe2 N6 O13' _chemical_formula_weight 1147.56 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 TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1543(10) _cell_length_b 14.4925(12) _cell_length_c 15.7642(13) _cell_angle_alpha 82.9990(10) _cell_angle_beta 87.5060(10) _cell_angle_gamma 68.9290(10) _cell_volume 2571.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATES _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type 'SADABS MULTI-SCAN' _exptl_absorpt_correction_T_min 0.6654 _exptl_absorpt_correction_T_max 0.9036 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22194 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 28.25 _reflns_number_total 11641 _reflns_number_gt 9988 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP, PLATON' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+1.6796P] 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 11641 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.38093(3) 0.32081(2) 0.26112(2) 0.01352(8) Uani 1 d . . . Fe2 Fe 0.59080(3) 0.15581(2) 0.193345(19) 0.01313(8) Uani 1 d . . . Cl1 Cl 0.12159(5) 0.18609(4) 0.02524(4) 0.02190(13) Uani 1 d . . . Cl2 Cl 0.85199(5) 0.70080(4) 0.37342(4) 0.02207(13) Uani 1 d . . . O1 O 0.43800(13) 0.23266(11) 0.18477(10) 0.0162(3) Uani 1 d . . . O3 O 0.65790(13) 0.26073(11) 0.21937(10) 0.0167(3) Uani 1 d . . . O2 O 0.49523(13) 0.39375(11) 0.23532(10) 0.0169(3) Uani 1 d . . . O4 O 0.60040(13) 0.10429(11) 0.31817(10) 0.0163(3) Uani 1 d . . . O5 O 0.46059(14) 0.23535(11) 0.36761(10) 0.0175(3) Uani 1 d . . . O6 O 0.1786(2) 0.25729(16) 0.02146(15) 0.0488(6) Uani 1 d . . . O7 O 0.20383(16) 0.08899(13) 0.05588(12) 0.0297(4) Uani 1 d . . . O8 O 0.08168(15) 0.18433(13) -0.05873(11) 0.0240(4) Uani 1 d . . . O9 O 0.02187(18) 0.21294(16) 0.08181(12) 0.0447(6) Uani 1 d . . . O10 O 0.73841(17) 0.69024(15) 0.37573(13) 0.0367(5) Uani 1 d . . . O11 O 0.8451(2) 0.78070(15) 0.42161(13) 0.0388(5) Uani 1 d . . . O12 O 0.88227(18) 0.72282(14) 0.28620(11) 0.0338(5) Uani 1 d . . . O13 O 0.93840(18) 0.60983(15) 0.41038(13) 0.0427(5) Uani 1 d . . . N6 N 0.64188(17) 0.19636(14) 0.06674(12) 0.0168(4) Uani 1 d . . . N5 N 0.77689(16) 0.04645(13) 0.18594(11) 0.0142(4) Uani 1 d . . . N4 N 0.57033(16) 0.02550(13) 0.15796(11) 0.0149(4) Uani 1 d . . . N2 N 0.29239(16) 0.43640(13) 0.35159(12) 0.0156(4) Uani 1 d . . . N3 N 0.25922(16) 0.43547(14) 0.17875(12) 0.0162(4) Uani 1 d . . . N1 N 0.22703(16) 0.28901(13) 0.29737(12) 0.0159(4) Uani 1 d . . . C1 C 0.5776(2) 0.28122(18) 0.01952(15) 0.0228(5) Uani 1 d . . . H1 H 0.5010 0.3157 0.0366 0.027 Uiso 1 calc R . . C2 C 0.6217(3) 0.3189(2) -0.05351(17) 0.0308(6) Uani 1 d . . . H2 H 0.5755 0.3771 -0.0857 0.037 Uiso 1 calc R . . C3 C 0.7364(3) 0.2674(2) -0.07739(17) 0.0330(6) Uani 1 d . . . H3 H 0.7681 0.2907 -0.1264 0.040 Uiso 1 calc R . . C4 C 0.8034(2) 0.1817(2) -0.02846(16) 0.0254(5) Uani 1 d . . . H4 H 0.8810 0.1475 -0.0433 0.030 Uiso 1 calc R . . C5 C 0.7532(2) 0.14713(17) 0.04351(14) 0.0173(5) Uani 1 d . . . C6 C 0.8168(2) 0.04937(17) 0.09539(14) 0.0185(5) Uani 1 d . . . H6A H 0.8044 -0.0035 0.0696 0.022 Uiso 1 calc R . . H6B H 0.9007 0.0371 0.0940 0.022 Uiso 1 calc R . . C7 C 0.85846(19) 0.06755(17) 0.24332(15) 0.0174(5) Uani 1 d . . . H7A H 0.8198 0.0802 0.2981 0.021 Uiso 1 calc R . . H7B H 0.8700 0.1281 0.2187 0.021 Uiso 1 calc R . . C8 C 0.9783(2) -0.01324(17) 0.25905(15) 0.0184(5) Uani 1 d . . . C9 C 0.9957(2) -0.0883(2) 0.32610(18) 0.0284(6) Uani 1 d . . . H9 H 0.9327 -0.0891 0.3615 0.034 Uiso 1 calc R . . C10 C 1.1053(2) -0.1620(2) 0.3413(2) 0.0357(7) Uani 1 d . . . H10 H 1.1152 -0.2128 0.3857 0.043 Uiso 1 calc R . . C11 C 1.1998(2) -0.1600(2) 0.2903(2) 0.0367(7) Uani 1 d . . . H11 H 1.2739 -0.2087 0.3010 0.044 Uiso 1 calc R . . C12 C 1.1840(2) -0.0856(2) 0.22366(18) 0.0305(6) Uani 1 d . . . H12 H 1.2476 -0.0844 0.1892 0.037 Uiso 1 calc R . . C13 C 1.0742(2) -0.01265(18) 0.20761(16) 0.0221(5) Uani 1 d . . . H13 H 1.0643 0.0370 0.1622 0.026 Uiso 1 calc R . . C14 C 0.76824(19) -0.05239(16) 0.21444(14) 0.0160(4) Uani 1 d . . . H14A H 0.7598 -0.0604 0.2761 0.019 Uiso 1 calc R . . H14B H 0.8396 -0.1048 0.1990 0.019 Uiso 1 calc R . . C15 C 0.66342(19) -0.06012(16) 0.17274(14) 0.0157(4) Uani 1 d . . . C16 C 0.6607(2) -0.14922(17) 0.15205(15) 0.0197(5) Uani 1 d . . . H16 H 0.7254 -0.2077 0.1632 0.024 Uiso 1 calc R . . C17 C 0.5603(2) -0.15017(18) 0.11451(16) 0.0222(5) Uani 1 d . . . H17 H 0.5569 -0.2094 0.1000 0.027 Uiso 1 calc R . . C18 C 0.4647(2) -0.06186(18) 0.09876(15) 0.0207(5) Uani 1 d . . . H18 H 0.3965 -0.0609 0.0736 0.025 Uiso 1 calc R . . C19 C 0.4731(2) 0.02448(17) 0.12122(14) 0.0172(5) Uani 1 d . . . H19 H 0.4094 0.0839 0.1106 0.021 Uiso 1 calc R . . C20 C 0.6043(2) 0.35331(16) 0.22076(13) 0.0152(4) Uani 1 d . . . C21 C 0.6751(2) 0.41961(17) 0.20639(14) 0.0170(5) Uani 1 d . . . C22 C 0.7920(2) 0.38198(17) 0.18077(15) 0.0197(5) Uani 1 d . . . H22 H 0.8247 0.3170 0.1671 0.024 Uiso 1 calc R . . C23 C 0.8602(2) 0.44161(19) 0.17561(17) 0.0264(5) Uani 1 d . . . H23 H 0.9386 0.4168 0.1584 0.032 Uiso 1 calc R . . C24 C 0.8105(2) 0.5389(2) 0.19643(17) 0.0287(6) Uani 1 d . . . H24 H 0.8564 0.5784 0.1945 0.034 Uiso 1 calc R . . C25 C 0.6931(2) 0.57687(18) 0.22000(16) 0.0262(5) Uani 1 d . . . H25 H 0.6601 0.6421 0.2330 0.031 Uiso 1 calc R . . C26 C 0.6254(2) 0.51828(17) 0.22425(15) 0.0209(5) Uani 1 d . . . H26 H 0.5461 0.5444 0.2391 0.025 Uiso 1 calc R . . C27 C 0.54012(19) 0.14944(16) 0.37803(14) 0.0150(4) Uani 1 d . . . C28 C 0.56480(19) 0.10004(16) 0.46753(14) 0.0154(4) Uani 1 d . . . C29 C 0.6628(2) 0.01339(18) 0.48462(15) 0.0224(5) Uani 1 d . . . H29 H 0.7107 -0.0149 0.4400 0.027 Uiso 1 calc R . . C30 C 0.6894(2) -0.0308(2) 0.56753(17) 0.0292(6) Uani 1 d . . . H30 H 0.7554 -0.0883 0.5788 0.035 Uiso 1 calc R . . C31 C 0.6170(2) 0.0109(2) 0.63411(16) 0.0270(6) Uani 1 d . . . H31 H 0.6352 -0.0183 0.6901 0.032 Uiso 1 calc R . . C32 C 0.5179(2) 0.09572(19) 0.61724(15) 0.0241(5) Uani 1 d . . . H32 H 0.4687 0.1227 0.6617 0.029 Uiso 1 calc R . . C33 C 0.4920(2) 0.14043(17) 0.53405(15) 0.0203(5) Uani 1 d . . . H33 H 0.4257 0.1977 0.5228 0.024 Uiso 1 calc R . . C34 C 0.2328(2) 0.42093(17) 0.10116(15) 0.0195(5) Uani 1 d . . . H34 H 0.2787 0.3629 0.0785 0.023 Uiso 1 calc R . . C35 C 0.1399(2) 0.48905(19) 0.05354(16) 0.0262(5) Uani 1 d . . . H35 H 0.1244 0.4784 -0.0010 0.031 Uiso 1 calc R . . C36 C 0.0703(2) 0.57370(18) 0.08924(17) 0.0274(6) Uani 1 d . . . H36 H 0.0065 0.6205 0.0589 0.033 Uiso 1 calc R . . C37 C 0.0958(2) 0.58868(17) 0.16995(16) 0.0218(5) Uani 1 d . . . H37 H 0.0494 0.6450 0.1947 0.026 Uiso 1 calc R . . C38 C 0.19227(19) 0.51773(16) 0.21312(15) 0.0163(4) Uani 1 d . . . C39 C 0.2317(2) 0.53179(16) 0.29838(15) 0.0203(5) Uani 1 d . . . H39A H 0.2847 0.5686 0.2890 0.024 Uiso 1 calc R . . H39B H 0.1635 0.5712 0.3292 0.024 Uiso 1 calc R . . C40 C 0.3841(2) 0.44625(17) 0.40744(15) 0.0183(5) Uani 1 d . . . H40A H 0.4484 0.4520 0.3712 0.022 Uiso 1 calc R . . H40B H 0.4154 0.3852 0.4459 0.022 Uiso 1 calc R . . C41 C 0.3438(2) 0.53257(17) 0.46041(15) 0.0177(5) Uani 1 d . . . C42 C 0.3736(2) 0.61585(18) 0.43606(15) 0.0209(5) Uani 1 d . . . H42 H 0.4157 0.6190 0.3857 0.025 Uiso 1 calc R . . C43 C 0.3419(2) 0.69454(18) 0.48543(16) 0.0239(5) Uani 1 d . . . H43 H 0.3617 0.7502 0.4679 0.029 Uiso 1 calc R . . C44 C 0.2810(2) 0.68943(18) 0.56048(16) 0.0246(5) Uani 1 d . . . H44 H 0.2597 0.7417 0.5940 0.030 Uiso 1 calc R . . C45 C 0.2513(2) 0.60662(19) 0.58609(15) 0.0235(5) Uani 1 d . . . H45 H 0.2100 0.6035 0.6368 0.028 Uiso 1 calc R . . C46 C 0.2826(2) 0.52847(18) 0.53668(15) 0.0205(5) Uani 1 d . . . H46 H 0.2626 0.4729 0.5545 0.025 Uiso 1 calc R . . C47 C 0.2073(2) 0.40117(17) 0.40460(15) 0.0193(5) Uani 1 d . . . H47A H 0.1415 0.4586 0.4196 0.023 Uiso 1 calc R . . H47B H 0.2460 0.3642 0.4572 0.023 Uiso 1 calc R . . C48 C 0.1609(2) 0.33629(16) 0.36061(15) 0.0174(5) Uani 1 d . . . C49 C 0.0584(2) 0.32003(18) 0.38801(16) 0.0222(5) Uani 1 d . . . H49 H 0.0130 0.3533 0.4316 0.027 Uiso 1 calc R . . C50 C 0.0254(2) 0.25349(19) 0.34922(17) 0.0252(5) Uani 1 d . . . H50 H -0.0413 0.2397 0.3679 0.030 Uiso 1 calc R . . C51 C 0.0918(2) 0.20763(18) 0.28256(16) 0.0222(5) Uani 1 d . . . H51 H 0.0694 0.1641 0.2549 0.027 Uiso 1 calc R . . C52 C 0.1915(2) 0.22733(17) 0.25786(15) 0.0195(5) Uani 1 d . . . H52 H 0.2358 0.1972 0.2125 0.023 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01186(16) 0.01226(16) 0.01474(16) -0.00279(12) -0.00072(12) -0.00179(12) Fe2 0.01280(16) 0.01187(15) 0.01367(16) -0.00268(11) 0.00022(12) -0.00276(12) Cl1 0.0231(3) 0.0182(3) 0.0207(3) -0.0045(2) -0.0042(2) -0.0018(2) Cl2 0.0252(3) 0.0179(3) 0.0205(3) -0.0012(2) 0.0032(2) -0.0052(2) O1 0.0150(8) 0.0150(8) 0.0165(8) -0.0044(6) -0.0018(6) -0.0019(6) O3 0.0167(8) 0.0133(8) 0.0196(8) -0.0031(6) -0.0014(6) -0.0043(6) O2 0.0144(8) 0.0146(8) 0.0216(8) -0.0040(6) 0.0006(6) -0.0044(6) O4 0.0165(8) 0.0150(8) 0.0144(8) -0.0018(6) 0.0009(6) -0.0018(6) O5 0.0187(8) 0.0147(8) 0.0157(8) -0.0019(6) -0.0019(6) -0.0017(6) O6 0.0625(15) 0.0331(12) 0.0590(15) -0.0047(10) -0.0231(12) -0.0245(11) O7 0.0246(9) 0.0251(9) 0.0307(10) 0.0037(8) -0.0052(8) 0.0000(8) O8 0.0229(9) 0.0257(9) 0.0206(9) -0.0070(7) -0.0017(7) -0.0039(7) O9 0.0372(12) 0.0498(13) 0.0236(10) -0.0065(9) 0.0042(9) 0.0131(10) O10 0.0295(11) 0.0395(11) 0.0453(12) -0.0114(9) 0.0061(9) -0.0161(9) O11 0.0575(14) 0.0349(11) 0.0321(11) -0.0134(9) 0.0093(10) -0.0241(10) O12 0.0468(12) 0.0295(10) 0.0218(10) 0.0000(8) 0.0105(8) -0.0120(9) O13 0.0389(12) 0.0317(11) 0.0380(12) 0.0067(9) -0.0007(9) 0.0073(9) N6 0.0188(10) 0.0159(9) 0.0165(10) -0.0023(7) -0.0013(7) -0.0069(8) N5 0.0141(9) 0.0135(9) 0.0148(9) -0.0015(7) -0.0003(7) -0.0046(7) N4 0.0144(9) 0.0155(9) 0.0141(9) -0.0027(7) 0.0012(7) -0.0043(7) N2 0.0145(9) 0.0148(9) 0.0159(9) -0.0018(7) -0.0021(7) -0.0031(7) N3 0.0153(9) 0.0169(9) 0.0163(9) -0.0027(7) -0.0007(7) -0.0052(8) N1 0.0149(9) 0.0142(9) 0.0155(9) -0.0013(7) -0.0008(7) -0.0014(7) C1 0.0227(12) 0.0215(12) 0.0218(12) -0.0011(10) -0.0031(10) -0.0049(10) C2 0.0394(16) 0.0260(14) 0.0255(14) 0.0070(11) -0.0065(12) -0.0121(12) C3 0.0406(16) 0.0367(16) 0.0252(14) 0.0078(12) 0.0012(12) -0.0218(13) C4 0.0214(13) 0.0338(14) 0.0233(13) -0.0022(11) 0.0028(10) -0.0135(11) C5 0.0182(11) 0.0208(12) 0.0163(11) -0.0048(9) -0.0004(9) -0.0102(9) C6 0.0166(11) 0.0194(11) 0.0184(11) -0.0038(9) 0.0033(9) -0.0049(9) C7 0.0162(11) 0.0176(11) 0.0194(11) -0.0046(9) -0.0005(9) -0.0065(9) C8 0.0152(11) 0.0180(11) 0.0231(12) -0.0041(9) -0.0033(9) -0.0064(9) C9 0.0223(13) 0.0314(14) 0.0326(15) 0.0045(11) -0.0048(11) -0.0130(11) C10 0.0278(14) 0.0325(15) 0.0435(17) 0.0115(13) -0.0123(12) -0.0103(12) C11 0.0222(14) 0.0312(15) 0.0501(18) -0.0033(13) -0.0112(12) -0.0005(11) C12 0.0170(12) 0.0396(16) 0.0338(15) -0.0124(12) 0.0011(11) -0.0064(11) C13 0.0199(12) 0.0234(12) 0.0242(13) -0.0036(10) -0.0016(10) -0.0087(10) C14 0.0142(11) 0.0136(10) 0.0195(11) -0.0021(8) -0.0003(8) -0.0038(9) C15 0.0151(11) 0.0159(11) 0.0155(11) -0.0011(8) 0.0015(8) -0.0051(9) C16 0.0174(11) 0.0159(11) 0.0240(12) -0.0034(9) 0.0012(9) -0.0036(9) C17 0.0237(12) 0.0186(12) 0.0285(13) -0.0079(10) 0.0007(10) -0.0109(10) C18 0.0192(12) 0.0244(12) 0.0214(12) -0.0040(9) -0.0008(9) -0.0108(10) C19 0.0145(11) 0.0191(11) 0.0157(11) -0.0030(9) 0.0011(8) -0.0030(9) C20 0.0182(11) 0.0164(11) 0.0103(10) -0.0015(8) -0.0017(8) -0.0052(9) C21 0.0213(12) 0.0176(11) 0.0131(11) -0.0011(8) -0.0019(9) -0.0082(9) C22 0.0218(12) 0.0180(11) 0.0187(12) -0.0024(9) 0.0011(9) -0.0062(9) C23 0.0231(13) 0.0295(14) 0.0285(14) -0.0007(11) 0.0035(10) -0.0129(11) C24 0.0315(14) 0.0282(14) 0.0344(15) -0.0006(11) -0.0030(11) -0.0208(12) C25 0.0334(14) 0.0166(12) 0.0287(14) -0.0027(10) 0.0004(11) -0.0090(11) C26 0.0222(12) 0.0163(11) 0.0224(12) -0.0003(9) -0.0013(9) -0.0050(9) C27 0.0119(10) 0.0168(11) 0.0177(11) -0.0040(8) 0.0000(8) -0.0062(9) C28 0.0154(11) 0.0171(11) 0.0151(11) -0.0011(8) -0.0019(8) -0.0074(9) C29 0.0219(12) 0.0213(12) 0.0195(12) -0.0016(9) 0.0016(9) -0.0028(10) C30 0.0239(13) 0.0277(14) 0.0269(14) 0.0036(11) -0.0048(11) 0.0000(11) C31 0.0323(14) 0.0325(14) 0.0144(12) 0.0033(10) -0.0031(10) -0.0111(12) C32 0.0307(14) 0.0263(13) 0.0175(12) -0.0050(10) 0.0031(10) -0.0124(11) C33 0.0216(12) 0.0189(12) 0.0192(12) -0.0019(9) 0.0004(9) -0.0058(10) C34 0.0192(12) 0.0197(12) 0.0192(12) -0.0028(9) -0.0017(9) -0.0063(9) C35 0.0303(14) 0.0254(13) 0.0224(13) 0.0013(10) -0.0089(10) -0.0095(11) C36 0.0256(13) 0.0196(12) 0.0340(15) 0.0030(10) -0.0126(11) -0.0048(10) C37 0.0176(12) 0.0140(11) 0.0303(13) 0.0000(10) -0.0024(10) -0.0021(9) C38 0.0138(11) 0.0142(11) 0.0207(12) -0.0002(9) 0.0000(9) -0.0051(9) C39 0.0236(12) 0.0125(11) 0.0226(12) -0.0051(9) -0.0019(10) -0.0025(9) C40 0.0146(11) 0.0200(11) 0.0201(12) -0.0078(9) -0.0023(9) -0.0038(9) C41 0.0141(11) 0.0188(11) 0.0190(11) -0.0045(9) -0.0040(9) -0.0033(9) C42 0.0184(12) 0.0256(13) 0.0207(12) -0.0053(10) -0.0007(9) -0.0092(10) C43 0.0244(13) 0.0217(12) 0.0294(14) -0.0051(10) -0.0071(10) -0.0114(10) C44 0.0214(12) 0.0241(13) 0.0276(13) -0.0132(10) -0.0061(10) -0.0033(10) C45 0.0200(12) 0.0315(14) 0.0182(12) -0.0083(10) -0.0015(9) -0.0065(10) C46 0.0211(12) 0.0202(12) 0.0200(12) -0.0041(9) -0.0032(9) -0.0063(10) C47 0.0206(12) 0.0203(12) 0.0178(11) -0.0051(9) 0.0017(9) -0.0075(10) C48 0.0165(11) 0.0155(11) 0.0179(11) -0.0018(9) -0.0024(9) -0.0026(9) C49 0.0174(12) 0.0261(13) 0.0222(12) -0.0061(10) 0.0027(9) -0.0058(10) C50 0.0175(12) 0.0295(14) 0.0301(14) -0.0033(11) 0.0001(10) -0.0103(10) C51 0.0212(12) 0.0207(12) 0.0265(13) -0.0041(10) -0.0038(10) -0.0086(10) C52 0.0199(12) 0.0178(11) 0.0191(12) -0.0028(9) -0.0019(9) -0.0043(9) _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 O1 1.7963(15) . ? Fe1 O5 2.0153(16) . ? Fe1 O2 2.0284(16) . ? Fe1 N1 2.1215(19) . ? Fe1 N3 2.1236(19) . ? Fe1 N2 2.2695(18) . ? Fe2 O1 1.7905(15) . ? Fe2 O4 2.0107(15) . ? Fe2 O3 2.0538(15) . ? Fe2 N4 2.1323(18) . ? Fe2 N6 2.1407(19) . ? Fe2 N5 2.2552(18) . ? Cl1 O6 1.430(2) . ? Cl1 O8 1.4356(17) . ? Cl1 O9 1.438(2) . ? Cl1 O7 1.4414(18) . ? Cl2 O13 1.4321(19) . ? Cl2 O12 1.4357(18) . ? Cl2 O11 1.4365(19) . ? Cl2 O10 1.441(2) . ? O3 C20 1.266(3) . ? O2 C20 1.265(3) . ? O4 C27 1.265(3) . ? O5 C27 1.269(3) . ? N6 C5 1.342(3) . ? N6 C1 1.347(3) . ? N5 C14 1.487(3) . ? N5 C6 1.488(3) . ? N5 C7 1.503(3) . ? N4 C19 1.344(3) . ? N4 C15 1.348(3) . ? N2 C39 1.482(3) . ? N2 C47 1.493(3) . ? N2 C40 1.506(3) . ? N3 C34 1.338(3) . ? N3 C38 1.341(3) . ? N1 C48 1.345(3) . ? N1 C52 1.346(3) . ? C1 C2 1.383(4) . ? C1 H1 0.9300 . ? C2 C3 1.384(4) . ? C2 H2 0.9300 . ? C3 C4 1.376(4) . ? C3 H3 0.9300 . ? C4 C5 1.390(3) . ? C4 H4 0.9300 . ? C5 C6 1.503(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.513(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.385(3) . ? C8 C13 1.392(3) . ? C9 C10 1.384(4) . ? C9 H9 0.9300 . ? C10 C11 1.380(4) . ? C10 H10 0.9300 . ? C11 C12 1.377(4) . ? C11 H11 0.9300 . ? C12 C13 1.383(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.504(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.382(3) . ? C16 C17 1.384(3) . ? C16 H16 0.9300 . ? C17 C18 1.389(3) . ? C17 H17 0.9300 . ? C18 C19 1.380(3) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.496(3) . ? C21 C22 1.389(3) . ? C21 C26 1.397(3) . ? C22 C23 1.390(3) . ? C22 H22 0.9300 . ? C23 C24 1.394(4) . ? C23 H23 0.9300 . ? C24 C25 1.384(4) . ? C24 H24 0.9300 . ? C25 C26 1.374(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.493(3) . ? C28 C33 1.386(3) . ? C28 C29 1.392(3) . ? C29 C30 1.381(3) . ? C29 H29 0.9300 . ? C30 C31 1.390(4) . ? C30 H30 0.9300 . ? C31 C32 1.384(4) . ? C31 H31 0.9300 . ? C32 C33 1.386(3) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.381(3) . ? C34 H34 0.9300 . ? C35 C36 1.385(4) . ? C35 H35 0.9300 . ? C36 C37 1.383(4) . ? C36 H36 0.9300 . ? C37 C38 1.388(3) . ? C37 H37 0.9300 . ? C38 C39 1.507(3) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.510(3) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.388(3) . ? C41 C46 1.393(3) . ? C42 C43 1.389(3) . ? C42 H42 0.9300 . ? C43 C44 1.377(4) . ? C43 H43 0.9300 . ? C44 C45 1.384(4) . ? C44 H44 0.9300 . ? C45 C46 1.383(3) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.503(3) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.391(3) . ? C49 C50 1.382(3) . ? C49 H49 0.9300 . ? C50 C51 1.382(3) . ? C50 H50 0.9300 . ? C51 C52 1.371(3) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O5 99.54(7) . . ? O1 Fe1 O2 97.07(7) . . ? O5 Fe1 O2 97.53(6) . . ? O1 Fe1 N1 98.43(7) . . ? O5 Fe1 N1 88.68(7) . . ? O2 Fe1 N1 162.10(7) . . ? O1 Fe1 N3 97.46(7) . . ? O5 Fe1 N3 161.55(7) . . ? O2 Fe1 N3 87.40(7) . . ? N1 Fe1 N3 81.77(7) . . ? O1 Fe1 N2 174.70(7) . . ? O5 Fe1 N2 84.38(6) . . ? O2 Fe1 N2 85.90(6) . . ? N1 Fe1 N2 77.99(7) . . ? N3 Fe1 N2 78.23(7) . . ? O1 Fe2 O4 100.39(7) . . ? O1 Fe2 O3 98.96(7) . . ? O4 Fe2 O3 89.85(6) . . ? O1 Fe2 N4 96.05(7) . . ? O4 Fe2 N4 92.07(7) . . ? O3 Fe2 N4 164.27(7) . . ? O1 Fe2 N6 97.43(7) . . ? O4 Fe2 N6 161.02(7) . . ? O3 Fe2 N6 80.94(7) . . ? N4 Fe2 N6 92.50(7) . . ? O1 Fe2 N5 170.27(7) . . ? O4 Fe2 N5 85.35(6) . . ? O2 Fe2 N3 88.84(6) . . ? N4 Fe2 N5 75.76(7) . . ? N6 Fe2 N5 77.96(7) . . ? O6 Cl1 O8 109.20(12) . . ? O6 Cl1 O9 110.06(15) . . ? O8 Cl1 O9 109.05(12) . . ? O6 Cl1 O7 109.40(12) . . ? O8 Cl1 O7 109.60(11) . . ? O9 Cl1 O7 109.50(12) . . ? O13 Cl2 O12 109.88(12) . . ? O13 Cl2 O11 109.97(13) . . ? O12 Cl2 O11 110.12(12) . . ? O13 Cl2 O10 109.25(13) . . ? O12 Cl2 O10 109.05(12) . . ? O11 Cl2 O10 108.53(12) . . ? Fe2 O1 Fe1 117.13(8) . . ? C20 O3 Fe2 128.40(14) . . ? C20 O2 Fe1 125.44(14) . . ? C27 O4 Fe2 126.69(14) . . ? C27 O5 Fe1 131.31(14) . . ? C5 N6 C1 119.3(2) . . ? C5 N6 Fe2 116.87(15) . . ? C1 N6 Fe2 122.02(16) . . ? C14 N5 C6 109.45(17) . . ? C14 N5 C7 110.53(17) . . ? C6 N5 C7 111.50(17) . . ? C14 N5 Fe2 104.74(13) . . ? C6 N5 Fe2 108.90(13) . . ? C7 N5 Fe2 111.48(13) . . ? C19 N4 C15 119.27(19) . . ? C19 N4 Fe2 124.38(15) . . ? C15 N4 Fe2 116.34(15) . . ? C39 N2 C47 111.73(18) . . ? C39 N2 C40 110.51(17) . . ? C47 N2 C40 110.47(17) . . ? C39 N2 Fe1 107.24(13) . . ? C47 N2 Fe1 107.22(13) . . ? C40 N2 Fe1 109.55(13) . . ? C34 N3 C38 119.6(2) . . ? C34 N3 Fe1 122.24(15) . . ? C38 N3 Fe1 117.01(15) . . ? C48 N1 C52 119.5(2) . . ? C48 N1 Fe1 117.56(15) . . ? C52 N1 Fe1 122.88(15) . . ? N6 C1 C2 122.2(2) . . ? N6 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C1 C2 C3 118.2(2) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C4 C3 C2 119.9(2) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.0(2) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N6 C5 C4 121.3(2) . . ? N6 C5 C6 116.4(2) . . ? C4 C5 C6 122.1(2) . . ? N5 C6 C5 112.83(18) . . ? N5 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N5 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N5 C7 C8 116.14(18) . . ? N5 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? N5 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C9 C8 C13 118.5(2) . . ? C9 C8 C7 120.7(2) . . ? C13 C8 C7 120.8(2) . . ? C10 C9 C8 121.0(3) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C11 C10 C9 119.8(3) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.5(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 120.3(2) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? N5 C14 C15 109.49(18) . . ? N5 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? N5 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? N4 C15 C16 121.5(2) . . ? N4 C15 C14 115.79(19) . . ? C16 C15 C14 122.7(2) . . ? C15 C16 C17 119.1(2) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C18 119.4(2) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 118.6(2) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? N4 C19 C18 122.1(2) . . ? N4 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? O2 C20 O2 124.6(2) . . ? O2 C20 C21 117.47(19) . . ? O3 C20 C21 117.9(2) . . ? C22 C21 C26 119.8(2) . . ? C22 C21 C20 120.4(2) . . ? C26 C21 C20 119.7(2) . . ? C21 C22 C23 119.9(2) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 119.6(2) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 120.3(2) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C24 120.1(2) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 120.2(2) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? O4 C27 O5 124.4(2) . . ? O4 C27 C28 118.44(19) . . ? O5 C27 C28 117.10(19) . . ? C33 C28 C29 119.6(2) . . ? C33 C28 C27 120.6(2) . . ? C29 C28 C27 119.7(2) . . ? C30 C29 C28 120.3(2) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 119.7(2) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 120.1(2) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 120.0(2) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 120.1(2) . . ? C32 C33 H33 119.9 . . ? C28 C33 H33 119.9 . . ? N3 C34 C35 122.3(2) . . ? N3 C34 H34 118.8 . . ? C35 C34 H34 118.8 . . ? C34 C35 C36 118.1(2) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? C37 C36 C35 120.0(2) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 118.5(2) . . ? C36 C37 H37 120.8 . . ? C38 C37 H37 120.8 . . ? N3 C38 C37 121.5(2) . . ? N3 C38 C39 116.43(19) . . ? C37 C38 C39 122.0(2) . . ? N2 C39 C38 112.92(18) . . ? N2 C39 H39A 109.0 . . ? C38 C39 H39A 109.0 . . ? N2 C39 H39B 109.0 . . ? C38 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? N2 C40 C41 116.48(18) . . ? N4 C40 H40A 108.2 . . ? C41 C40 H40A 108.2 . . ? N2 C40 H40B 108.2 . . ? C41 C40 H40B 108.2 . . ? H40A C40 H40B 107.3 . . ? C42 C41 C46 118.5(2) . . ? C42 C41 C40 120.0(2) . . ? C46 C41 C40 121.4(2) . . ? C41 C42 C43 121.2(2) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C44 C43 C42 119.5(2) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C45 120.1(2) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.4(2) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C41 120.3(2) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? N2 C47 C48 113.52(18) . . ? N2 C47 H47A 108.9 . . ? C48 C47 H47A 108.9 . . ? N2 C47 H47B 108.9 . . ? C48 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? N1 C48 C49 121.2(2) . . ? N1 C48 C47 117.1(2) . . ? C49 C48 C47 121.5(2) . . ? C50 C49 C48 118.7(2) . . ? C50 C49 H49 120.7 . . ? C48 C49 H49 120.7 . . ? C49 C50 C51 119.7(2) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C52 C51 C50 119.0(2) . . ? C52 C51 H51 120.5 . . ? C50 C51 H51 120.5 . . ? N1 C52 C51 121.9(2) . . ? N1 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.552 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.076