# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Paul Kruger' _publ_contact_author_email PAUL.KRUGER@CANTERBURY.AC.NZ _publ_section_title ; Twist and spin: Asymmetric spin crossover behaviour and evidence of light-induced excited spin state trapping in a dinuclear iron(II) helicate ; loop_ _publ_author_name 'Paul Kruger' 'Rodolphe Clerac' 'Etienne Harte' 'Corine Mathoniere' 'Diane Pelleteret' 'Wolfgang Schmitt' # Attachment 'B816196H.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 702672' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H66 Cl4 Fe2 N20 O19' _chemical_formula_weight 1744.93 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 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 21.250(4) _cell_length_b 10.756(2) _cell_length_c 33.469(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.32(3) _cell_angle_gamma 90.00 _cell_volume 7650(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 28.4 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3592 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82388 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 25.50 _reflns_number_total 14219 _reflns_number_gt 11076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Smart' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+8.0151P] 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 14219 _refine_ls_number_parameters 1052 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1637 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 Fe1 Fe 0.78545(2) 0.78938(4) 0.023748(13) 0.02806(13) Uani 1 1 d . . . Fe2 Fe 1.05234(2) 0.79319(5) 0.321956(14) 0.03029(13) Uani 1 1 d . . . Cl1 Cl 1.00723(5) 1.23937(10) 0.42936(3) 0.0525(3) Uani 1 1 d . . . Cl2 Cl 0.79229(5) 0.76813(9) 0.39279(3) 0.0475(2) Uani 1 1 d . . . Cl3 Cl 1.17152(5) 0.36216(10) 0.20841(4) 0.0557(3) Uani 1 1 d . . . Cl4 Cl 1.40981(6) 0.19692(12) 0.47657(4) 0.0720(4) Uani 1 1 d . . . O1 O 1.04141(12) 1.0450(3) 0.13097(8) 0.0548(8) Uani 1 1 d . . . O2 O 0.91551(14) 0.4134(2) 0.17544(7) 0.0486(7) Uani 1 1 d . . . O3 O 0.75306(10) 0.8995(2) 0.23133(7) 0.0366(6) Uani 1 1 d . . . O4 O 1.02976(18) 1.3586(3) 0.41616(11) 0.0798(10) Uani 1 1 d . . . O5 O 0.97284(19) 1.1842(4) 0.39847(11) 0.0942(13) Uani 1 1 d . . . O6 O 0.9652(3) 1.2521(4) 0.46229(11) 0.1070(16) Uani 1 1 d . . . O7 O 1.0579(3) 1.1622(6) 0.4371(2) 0.172(3) Uani 1 1 d . . . O8 O 0.79891(17) 0.8986(3) 0.39324(10) 0.0686(9) Uani 1 1 d . . . O9 O 0.84485(15) 0.7087(3) 0.37448(11) 0.0682(9) Uani 1 1 d . . . O10 O 0.73890(18) 0.7359(4) 0.36887(16) 0.1085(16) Uani 1 1 d . . . O11 O 0.7826(3) 0.7211(4) 0.43080(13) 0.1244(19) Uani 1 1 d . . . O12 O 1.1267(2) 0.3313(4) 0.17766(12) 0.1011(14) Uani 1 1 d . . . O13 O 1.1656(2) 0.4900(3) 0.21634(15) 0.1091(16) Uani 1 1 d . . . O14 O 1.1554(3) 0.2920(5) 0.24194(13) 0.128(2) Uani 1 1 d . . . O15 O 1.2293(2) 0.3336(5) 0.1954(2) 0.172(3) Uani 1 1 d . . . O16 O 1.3595(2) 0.1070(5) 0.47666(15) 0.1109(16) Uani 1 1 d . A . O17 O 1.3817(2) 0.3055(4) 0.46196(17) 0.1168(16) Uani 1 1 d . A . O18A O 1.4568(4) 0.1306(15) 0.4764(9) 0.201(14) Uani 0.56(2) 1 d P A 1 O18B O 1.4493(7) 0.1855(11) 0.4394(4) 0.096(6) Uani 0.44(2) 1 d P A 2 O19 O 1.4263(5) 0.2416(9) 0.5145(3) 0.251(5) Uani 1 1 d . A . N1 N 0.72144(13) 0.9067(3) 0.00324(8) 0.0312(6) Uani 1 1 d . . . N2 N 0.70273(14) 1.0975(3) -0.01737(8) 0.0346(7) Uani 1 1 d . . . N3 N 0.82532(13) 0.9525(3) 0.04063(8) 0.0299(6) Uani 1 1 d . . . N4 N 1.09918(12) 0.7797(3) 0.26956(8) 0.0299(6) Uani 1 1 d . . . N5 N 1.11997(13) 0.6778(3) 0.33728(8) 0.0349(6) Uani 1 1 d . . . N6 N 1.20428(13) 0.5703(3) 0.32084(9) 0.0346(6) Uani 1 1 d . . . N7 N 0.83034(13) 0.7976(3) -0.02716(8) 0.0336(6) Uani 1 1 d . . . N8 N 0.90349(14) 0.7184(3) -0.06625(8) 0.0374(7) Uani 1 1 d . . . N9 N 0.85947(13) 0.6812(2) 0.03701(8) 0.0293(6) Uani 1 1 d . . . N10 N 0.99137(12) 0.6494(3) 0.31611(8) 0.0309(6) Uani 1 1 d . . . N11 N 1.02019(14) 0.7838(3) 0.37665(9) 0.0403(7) Uani 1 1 d . . . N12 N 0.97427(17) 0.6685(4) 0.42288(10) 0.0543(9) Uani 1 1 d . . . N13 N 0.73550(13) 0.6515(3) 0.00156(8) 0.0319(6) Uani 1 1 d . . . N14 N 0.65173(14) 0.5317(3) 0.00735(9) 0.0388(7) Uani 1 1 d . . . N15 N 0.73388(13) 0.7425(3) 0.07281(8) 0.0308(6) Uani 1 1 d . . . N16 N 0.98959(12) 0.9227(3) 0.30487(8) 0.0309(6) Uani 1 1 d . . . N17 N 1.10042(14) 0.9450(3) 0.33519(9) 0.0417(7) Uani 1 1 d . . . N18 N 1.10204(16) 1.1517(3) 0.33565(10) 0.0517(9) Uani 1 1 d . . . N19 N 0.9071(3) 0.2444(8) 0.2763(4) 0.200(6) Uani 1 1 d . . . N20 N 1.2861(2) 0.3032(5) 0.37737(18) 0.0960(17) Uani 1 1 d . . . C1 C 0.66712(16) 0.9060(3) -0.01869(10) 0.0367(8) Uani 1 1 d . . . H1 H 0.6423 0.8367 -0.0240 0.044 Uiso 1 1 calc R . . C2 C 0.65535(16) 1.0245(3) -0.03146(10) 0.0380(8) Uani 1 1 d . . . H2 H 0.6213 1.0503 -0.0469 0.046 Uiso 1 1 calc R . . C3 C 0.7112(2) 1.2302(4) -0.02507(12) 0.0471(10) Uani 1 1 d . . . H3A H 0.7080 1.2754 -0.0004 0.071 Uiso 1 1 calc R . . H3B H 0.6793 1.2584 -0.0433 0.071 Uiso 1 1 calc R . . H3C H 0.7520 1.2440 -0.0365 0.071 Uiso 1 1 calc R . . C4 C 0.74182(16) 1.0237(3) 0.00363(9) 0.0310(7) Uani 1 1 d . . . C5 C 0.79887(15) 1.0490(3) 0.02545(9) 0.0308(7) Uani 1 1 d . . . H5 H 0.8153 1.1287 0.0283 0.037 Uiso 1 1 calc R . . C7 C 0.88139(15) 0.9749(3) 0.06387(9) 0.0294(7) Uani 1 1 d . . . C8 C 0.87636(18) 1.0285(5) 0.10102(12) 0.0566(12) Uani 1 1 d . . . H8 H 0.8371 1.0508 0.1108 0.068 Uiso 1 1 calc R . . C9 C 0.93009(19) 1.0493(5) 0.12382(12) 0.0625(13) Uani 1 1 d . . . H9 H 0.9271 1.0849 0.1491 0.075 Uiso 1 1 calc R . . C10 C 0.98752(16) 1.0167(4) 0.10875(11) 0.0389(9) Uani 1 1 d . . . C11 C 0.99327(17) 0.9694(4) 0.07146(12) 0.0443(9) Uani 1 1 d . . . H11 H 1.0328 0.9515 0.0612 0.053 Uiso 1 1 calc R . . C12 C 0.93935(17) 0.9477(4) 0.04858(11) 0.0416(9) Uani 1 1 d . . . H12 H 0.9428 0.9148 0.0230 0.050 Uiso 1 1 calc R . . C13 C 1.05382(15) 0.9744(4) 0.16480(11) 0.0378(8) Uani 1 1 d . . . C14 C 1.04971(18) 0.8472(4) 0.16483(11) 0.0438(9) Uani 1 1 d . . . H14 H 1.0361 0.8051 0.1421 0.053 Uiso 1 1 calc R . . C15 C 1.06613(17) 0.7818(3) 0.19914(11) 0.0395(8) Uani 1 1 d . . . H15 H 1.0642 0.6954 0.1993 0.047 Uiso 1 1 calc R . . C16 C 1.08537(14) 0.8453(3) 0.23307(10) 0.0305(7) Uani 1 1 d . . . C17 C 1.09048(15) 0.9727(3) 0.23218(10) 0.0355(8) Uani 1 1 d . . . H17 H 1.1047 1.0152 0.2547 0.043 Uiso 1 1 calc R . . C18 C 1.07450(16) 1.0381(3) 0.19794(11) 0.0389(8) Uani 1 1 d . . . H18 H 1.0777 1.1243 0.1974 0.047 Uiso 1 1 calc R . . C19 C 1.14879(15) 0.7106(3) 0.27021(10) 0.0330(7) Uani 1 1 d . . . H19 H 1.1750 0.7004 0.2483 0.040 Uiso 1 1 calc R . . C20 C 1.15989(15) 0.6506(3) 0.30818(10) 0.0317(7) Uani 1 1 d . . . C21 C 1.13983(18) 0.6125(4) 0.36999(11) 0.0427(9) Uani 1 1 d . . . H21 H 1.1208 0.6130 0.3950 0.051 Uiso 1 1 calc R . . C22 C 1.19207(17) 0.5465(4) 0.35994(11) 0.0404(9) Uani 1 1 d . . . H22 H 1.2152 0.4946 0.3767 0.049 Uiso 1 1 calc R . . C23 C 1.25745(17) 0.5214(4) 0.29810(12) 0.0475(10) Uani 1 1 d . . . H23A H 1.2433 0.4544 0.2814 0.071 Uiso 1 1 calc R . . H23B H 1.2892 0.4915 0.3162 0.071 Uiso 1 1 calc R . . H23C H 1.2747 0.5863 0.2818 0.071 Uiso 1 1 calc R . . C24 C 0.82153(18) 0.8420(4) -0.06507(11) 0.0419(9) Uani 1 1 d . . . H24 H 0.7900 0.8968 -0.0730 0.050 Uiso 1 1 calc R . . C25 C 0.86594(18) 0.7933(4) -0.08896(11) 0.0430(9) Uani 1 1 d . . . H25 H 0.8702 0.8081 -0.1162 0.052 Uiso 1 1 calc R . . C26 C 0.95977(19) 0.6501(4) -0.07918(12) 0.0517(10) Uani 1 1 d . . . H26A H 0.9615 0.6495 -0.1078 0.078 Uiso 1 1 calc R . . H26B H 0.9578 0.5662 -0.0695 0.078 Uiso 1 1 calc R . . H26C H 0.9967 0.6900 -0.0687 0.078 Uiso 1 1 calc R . . C27 C 0.88017(16) 0.7230(3) -0.02867(10) 0.0324(7) Uani 1 1 d . . . C28 C 0.89679(15) 0.6589(3) 0.00750(10) 0.0315(7) Uani 1 1 d . . . H28 H 0.9313 0.6060 0.0095 0.038 Uiso 1 1 calc R . . C29 C 0.87290(15) 0.6160(3) 0.07368(9) 0.0286(7) Uani 1 1 d . . . C30 C 0.89955(19) 0.6765(3) 0.10557(11) 0.0443(9) Uani 1 1 d . . . H30 H 0.9079 0.7612 0.1039 0.053 Uiso 1 1 calc R . . C31 C 0.91413(19) 0.6119(3) 0.14043(11) 0.0451(9) Uani 1 1 d . . . H31 H 0.9323 0.6529 0.1621 0.054 Uiso 1 1 calc R . . C32 C 0.90142(16) 0.4867(3) 0.14248(10) 0.0348(8) Uani 1 1 d . . . C33 C 0.8732(2) 0.4272(3) 0.11093(12) 0.0504(11) Uani 1 1 d . . . H33 H 0.8631 0.3433 0.1128 0.060 Uiso 1 1 calc R . . C34 C 0.8597(2) 0.4920(4) 0.07641(12) 0.0506(10) Uani 1 1 d . . . H34 H 0.8415 0.4510 0.0548 0.061 Uiso 1 1 calc R . . C35 C 0.93403(17) 0.4744(3) 0.21038(10) 0.0363(8) Uani 1 1 d . . . C36 C 0.99607(17) 0.4687(3) 0.22181(10) 0.0353(8) Uani 1 1 d . . . H36 H 1.0252 0.4265 0.2062 0.042 Uiso 1 1 calc R . . C37 C 1.01489(15) 0.5265(3) 0.25683(10) 0.0336(8) Uani 1 1 d . . . H37 H 1.0569 0.5238 0.2647 0.040 Uiso 1 1 calc R . . C38 C 0.97164(15) 0.5878(3) 0.28006(10) 0.0299(7) Uani 1 1 d . . . C39 C 0.90849(16) 0.5899(3) 0.26906(12) 0.0394(8) Uani 1 1 d . . . H39 H 0.8790 0.6294 0.2851 0.047 Uiso 1 1 calc R . . C40 C 0.88992(17) 0.5325(3) 0.23386(12) 0.0427(9) Uani 1 1 d . . . H40 H 0.8478 0.5331 0.2261 0.051 Uiso 1 1 calc R . . C41 C 0.96626(17) 0.6131(4) 0.34909(10) 0.0380(8) Uani 1 1 d . . . H41 H 0.9385 0.5464 0.3505 0.046 Uiso 1 1 calc R . . C42 C 0.98456(18) 0.6837(4) 0.38318(10) 0.0420(9) Uani 1 1 d . . . C43 C 1.0332(2) 0.8341(5) 0.41319(12) 0.0540(11) Uani 1 1 d . . . H43 H 1.0573 0.9049 0.4179 0.065 Uiso 1 1 calc R . . C44 C 1.0050(2) 0.7633(5) 0.44156(13) 0.0673(15) Uani 1 1 d . . . H44 H 1.0064 0.7772 0.4690 0.081 Uiso 1 1 calc R . . C45 C 0.9345(3) 0.5749(5) 0.44164(14) 0.0790(17) Uani 1 1 d . . . H45A H 0.8932 0.6086 0.4458 0.119 Uiso 1 1 calc R . . H45B H 0.9525 0.5512 0.4669 0.119 Uiso 1 1 calc R . . H45C H 0.9316 0.5033 0.4246 0.119 Uiso 1 1 calc R . . C46 C 0.72290(18) 0.5982(3) -0.03472(11) 0.0376(8) Uani 1 1 d . . . H46 H 0.7458 0.6108 -0.0580 0.045 Uiso 1 1 calc R . . C47 C 0.67178(18) 0.5243(3) -0.03129(11) 0.0410(9) Uani 1 1 d . . . H47 H 0.6536 0.4771 -0.0515 0.049 Uiso 1 1 calc R . . C48 C 0.59893(19) 0.4651(4) 0.02555(14) 0.0541(11) Uani 1 1 d . . . H48A H 0.6142 0.3912 0.0385 0.081 Uiso 1 1 calc R . . H48B H 0.5690 0.4427 0.0052 0.081 Uiso 1 1 calc R . . H48C H 0.5790 0.5177 0.0449 0.081 Uiso 1 1 calc R . . C49 C 0.69148(16) 0.6092(3) 0.02622(10) 0.0329(7) Uani 1 1 d . . . C50 C 0.69229(16) 0.6570(3) 0.06625(10) 0.0344(8) Uani 1 1 d . . . H50 H 0.6651 0.6287 0.0859 0.041 Uiso 1 1 calc R . . C51 C 0.73856(15) 0.7838(3) 0.11329(10) 0.0318(7) Uani 1 1 d . . . C52 C 0.74995(16) 0.6961(3) 0.14318(10) 0.0364(8) Uani 1 1 d . . . H52 H 0.7545 0.6125 0.1368 0.044 Uiso 1 1 calc R . . C53 C 0.75431(16) 0.7361(3) 0.18257(10) 0.0358(8) Uani 1 1 d . . . H53 H 0.7617 0.6788 0.2029 0.043 Uiso 1 1 calc R . . C54 C 0.74779(15) 0.8598(3) 0.19171(9) 0.0314(7) Uani 1 1 d . . . C55 C 0.73452(16) 0.9464(3) 0.16239(10) 0.0357(8) Uani 1 1 d . . . H55 H 0.7285 1.0295 0.1690 0.043 Uiso 1 1 calc R . . C56 C 0.73034(17) 0.9079(3) 0.12301(10) 0.0361(8) Uani 1 1 d . . . H56 H 0.7220 0.9657 0.1030 0.043 Uiso 1 1 calc R . . C57 C 0.81292(15) 0.8963(3) 0.24847(10) 0.0304(7) Uani 1 1 d . . . C58 C 0.86729(16) 0.8823(4) 0.22629(10) 0.0365(8) Uani 1 1 d . . . H58 H 0.8651 0.8694 0.1988 0.044 Uiso 1 1 calc R . . C59 C 0.92497(16) 0.8878(4) 0.24569(10) 0.0367(8) Uani 1 1 d . . . H59 H 0.9618 0.8780 0.2311 0.044 Uiso 1 1 calc R . . C60 C 0.92861(15) 0.9077(3) 0.28621(10) 0.0302(7) Uani 1 1 d . . . C61 C 0.87431(16) 0.9189(3) 0.30828(10) 0.0336(7) Uani 1 1 d . . . H61 H 0.8766 0.9305 0.3358 0.040 Uiso 1 1 calc R . . C62 C 0.81632(15) 0.9127(3) 0.28926(10) 0.0329(7) Uani 1 1 d . . . H62 H 0.7796 0.9196 0.3041 0.040 Uiso 1 1 calc R . . C63 C 1.00471(16) 1.0356(3) 0.31345(10) 0.0354(8) Uani 1 1 d . . . H63 H 0.9776 1.1025 0.3096 0.043 Uiso 1 1 calc R . . C64 C 1.06706(17) 1.0487(4) 0.32938(11) 0.0408(9) Uani 1 1 d . . . C65 C 1.15936(19) 0.9832(5) 0.34656(14) 0.0609(12) Uani 1 1 d . . . H65 H 1.1930 0.9317 0.3530 0.073 Uiso 1 1 calc R . . C66 C 1.1601(2) 1.1096(5) 0.34674(16) 0.0675(14) Uani 1 1 d . . . H66 H 1.1945 1.1591 0.3533 0.081 Uiso 1 1 calc R . . C67 C 1.0831(2) 1.2807(4) 0.32875(16) 0.0676(14) Uani 1 1 d . . . H67A H 1.1055 1.3341 0.3469 0.101 Uiso 1 1 calc R . . H67B H 1.0387 1.2890 0.3331 0.101 Uiso 1 1 calc R . . H67C H 1.0927 1.3037 0.3018 0.101 Uiso 1 1 calc R . . C68 C 0.8713(3) 0.2196(5) 0.2465(3) 0.099(3) Uani 1 1 d . . . C69 C 0.8283(3) 0.2018(6) 0.2142(2) 0.100(2) Uani 1 1 d . . . C70 C 1.3143(3) 0.2138(6) 0.37782(16) 0.0735(15) Uani 1 1 d . . . C71 C 1.3494(4) 0.0965(6) 0.3795(2) 0.107(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 0.0308(3) 0.0285(2) 0.0248(2) 0.00201(18) -0.00483(18) 0.00304(19) Fe2 0.0250(2) 0.0388(3) 0.0270(3) -0.0021(2) -0.00362(18) 0.0034(2) Cl1 0.0623(6) 0.0523(6) 0.0428(5) -0.0015(4) -0.0149(5) 0.0045(5) Cl2 0.0520(6) 0.0458(5) 0.0446(5) -0.0008(4) 0.0073(4) -0.0107(4) Cl3 0.0496(6) 0.0449(6) 0.0728(7) -0.0113(5) 0.0089(5) 0.0008(4) Cl4 0.0687(8) 0.0617(7) 0.0854(9) 0.0068(6) -0.0182(7) -0.0019(6) O1 0.0372(14) 0.0702(19) 0.0568(17) 0.0368(15) -0.0186(12) -0.0248(13) O2 0.0760(19) 0.0307(13) 0.0387(14) 0.0089(11) -0.0264(13) -0.0092(13) O3 0.0236(11) 0.0584(16) 0.0279(12) -0.0042(11) -0.0004(9) 0.0068(11) O4 0.087(3) 0.064(2) 0.089(3) -0.0035(19) 0.005(2) -0.0164(19) O5 0.094(3) 0.126(4) 0.063(2) -0.017(2) -0.006(2) -0.043(3) O6 0.171(5) 0.098(3) 0.053(2) -0.011(2) 0.038(3) -0.015(3) O7 0.114(4) 0.150(5) 0.252(8) 0.064(5) -0.060(5) 0.044(4) O8 0.089(2) 0.0451(18) 0.072(2) -0.0101(15) 0.0231(18) -0.0142(16) O9 0.0581(19) 0.061(2) 0.086(2) 0.0118(17) 0.0166(17) 0.0127(16) O10 0.062(2) 0.106(3) 0.157(4) -0.063(3) -0.028(3) 0.003(2) O11 0.204(6) 0.099(3) 0.071(3) 0.024(2) 0.058(3) -0.020(3) O12 0.144(4) 0.082(3) 0.077(3) -0.023(2) -0.019(3) -0.025(3) O13 0.117(3) 0.053(2) 0.157(4) -0.042(2) -0.065(3) 0.018(2) O14 0.192(5) 0.133(4) 0.058(2) 0.006(3) 0.017(3) -0.050(4) O15 0.091(3) 0.119(4) 0.308(8) 0.059(5) 0.107(5) 0.046(3) O16 0.084(3) 0.124(4) 0.125(4) 0.045(3) -0.020(3) -0.027(3) O17 0.097(3) 0.090(3) 0.164(5) 0.022(3) 0.016(3) 0.000(3) O18A 0.023(4) 0.140(11) 0.44(4) -0.122(18) -0.027(9) 0.028(5) O18B 0.103(8) 0.066(7) 0.121(10) -0.027(6) 0.088(7) -0.032(5) O19 0.327(12) 0.228(9) 0.197(8) -0.055(7) -0.164(9) 0.031(9) N1 0.0300(14) 0.0358(16) 0.0279(14) 0.0007(12) -0.0064(11) 0.0039(12) N2 0.0403(16) 0.0353(16) 0.0281(14) 0.0005(12) -0.0053(12) 0.0108(13) N3 0.0321(14) 0.0330(15) 0.0245(13) -0.0013(11) -0.0061(11) 0.0045(12) N4 0.0251(14) 0.0359(15) 0.0287(14) 0.0004(12) -0.0034(11) -0.0008(12) N5 0.0308(15) 0.0447(17) 0.0291(15) -0.0017(13) -0.0047(12) 0.0024(13) N6 0.0269(14) 0.0394(16) 0.0374(16) -0.0025(13) -0.0069(12) 0.0026(12) N7 0.0356(15) 0.0354(16) 0.0298(15) 0.0061(12) -0.0060(12) -0.0013(13) N8 0.0365(16) 0.0455(18) 0.0302(15) -0.0004(13) 0.0041(12) -0.0094(13) N9 0.0314(14) 0.0288(14) 0.0276(14) 0.0011(11) -0.0047(11) 0.0000(11) N10 0.0299(14) 0.0339(15) 0.0288(15) 0.0032(12) 0.0001(11) 0.0057(12) N11 0.0338(16) 0.055(2) 0.0322(16) -0.0071(14) -0.0029(12) 0.0101(15) N12 0.058(2) 0.073(2) 0.0313(17) 0.0121(17) 0.0107(16) 0.0269(19) N13 0.0369(15) 0.0285(14) 0.0304(15) 0.0035(12) -0.0038(12) 0.0030(12) N14 0.0426(17) 0.0310(15) 0.0429(18) 0.0017(13) -0.0069(14) -0.0008(13) N15 0.0318(15) 0.0310(15) 0.0295(14) 0.0036(12) -0.0031(11) 0.0067(12) N16 0.0256(14) 0.0382(16) 0.0289(14) -0.0012(12) -0.0001(11) 0.0005(12) N17 0.0296(15) 0.056(2) 0.0397(17) -0.0070(15) -0.0054(13) -0.0031(14) N18 0.048(2) 0.055(2) 0.053(2) -0.0138(17) -0.0001(16) -0.0155(17) N19 0.080(4) 0.159(7) 0.361(14) 0.192(9) -0.004(6) 0.000(5) N20 0.051(3) 0.101(4) 0.136(5) 0.045(3) -0.013(3) 0.016(3) C1 0.0337(18) 0.044(2) 0.0323(18) -0.0033(15) -0.0085(14) 0.0017(16) C2 0.0349(19) 0.048(2) 0.0311(18) -0.0060(16) -0.0091(14) 0.0101(16) C3 0.059(3) 0.038(2) 0.044(2) 0.0053(17) -0.0066(19) 0.0124(18) C4 0.0339(18) 0.0338(18) 0.0252(16) 0.0007(14) -0.0022(13) 0.0075(14) C5 0.0337(17) 0.0315(17) 0.0273(16) 0.0002(14) -0.0004(13) 0.0028(14) C7 0.0297(17) 0.0298(17) 0.0286(17) 0.0046(13) -0.0046(13) 0.0030(13) C8 0.0285(19) 0.101(4) 0.040(2) -0.020(2) -0.0022(16) -0.002(2) C9 0.039(2) 0.119(4) 0.030(2) -0.010(2) -0.0009(17) -0.016(2) C10 0.0295(18) 0.046(2) 0.041(2) 0.0207(17) -0.0076(15) -0.0088(16) C11 0.0285(18) 0.043(2) 0.062(3) -0.0049(19) 0.0065(17) -0.0060(16) C12 0.040(2) 0.046(2) 0.039(2) -0.0071(17) 0.0065(16) -0.0088(17) C13 0.0210(16) 0.051(2) 0.041(2) 0.0158(17) -0.0030(14) -0.0095(15) C14 0.046(2) 0.053(2) 0.0327(19) 0.0076(17) -0.0106(16) -0.0156(18) C15 0.045(2) 0.037(2) 0.0363(19) 0.0068(15) -0.0084(16) -0.0054(16) C16 0.0197(15) 0.0419(19) 0.0299(17) 0.0035(14) -0.0013(12) -0.0015(14) C17 0.0300(18) 0.042(2) 0.0350(18) 0.0028(15) 0.0002(14) -0.0055(15) C18 0.0295(18) 0.038(2) 0.049(2) 0.0096(17) 0.0017(15) -0.0059(15) C19 0.0261(17) 0.0405(19) 0.0322(18) -0.0020(15) -0.0015(13) -0.0016(15) C20 0.0251(16) 0.0367(18) 0.0331(18) -0.0015(14) -0.0061(13) 0.0000(14) C21 0.044(2) 0.059(2) 0.0257(18) 0.0022(16) -0.0088(15) 0.0076(18) C22 0.037(2) 0.046(2) 0.038(2) 0.0053(16) -0.0156(15) -0.0008(17) C23 0.0304(19) 0.056(2) 0.056(2) 0.003(2) -0.0014(17) 0.0088(17) C24 0.045(2) 0.049(2) 0.0317(19) 0.0110(17) -0.0057(16) -0.0009(18) C25 0.050(2) 0.048(2) 0.0313(19) 0.0091(17) -0.0038(16) -0.0143(18) C26 0.051(2) 0.064(3) 0.041(2) -0.006(2) 0.0133(18) -0.003(2) C27 0.0336(18) 0.0336(18) 0.0301(17) 0.0010(14) -0.0016(14) -0.0070(14) C28 0.0267(16) 0.0342(18) 0.0337(18) -0.0009(14) -0.0052(14) 0.0010(14) C29 0.0270(16) 0.0307(17) 0.0280(16) 0.0043(13) -0.0034(13) 0.0029(13) C30 0.062(3) 0.0314(19) 0.040(2) 0.0080(16) -0.0123(18) -0.0113(17) C31 0.059(2) 0.037(2) 0.039(2) 0.0078(16) -0.0203(18) -0.0153(18) C32 0.0394(19) 0.0316(18) 0.0334(18) 0.0049(14) -0.0077(15) 0.0000(15) C33 0.075(3) 0.0262(18) 0.049(2) 0.0053(16) -0.024(2) -0.0111(18) C34 0.073(3) 0.037(2) 0.041(2) -0.0005(17) -0.027(2) -0.0099(19) C35 0.048(2) 0.0274(17) 0.0331(18) 0.0075(14) -0.0123(16) -0.0059(15) C36 0.0378(19) 0.0373(19) 0.0308(18) 0.0019(15) 0.0015(14) -0.0037(15) C37 0.0273(17) 0.041(2) 0.0319(18) 0.0024(15) -0.0032(14) -0.0032(14) C38 0.0280(16) 0.0312(17) 0.0306(17) 0.0060(14) -0.0018(13) 0.0012(13) C39 0.0305(18) 0.0354(19) 0.052(2) 0.0017(16) -0.0029(16) 0.0026(15) C40 0.0354(19) 0.0329(19) 0.059(2) 0.0052(17) -0.0208(18) -0.0030(15) C41 0.0367(19) 0.041(2) 0.0362(19) 0.0066(16) 0.0052(15) 0.0087(16) C42 0.046(2) 0.052(2) 0.0284(18) 0.0051(16) 0.0048(15) 0.0179(18) C43 0.052(2) 0.077(3) 0.033(2) -0.016(2) -0.0070(18) 0.017(2) C44 0.067(3) 0.102(4) 0.033(2) -0.012(2) -0.008(2) 0.041(3) C45 0.098(4) 0.090(4) 0.050(3) 0.028(3) 0.031(3) 0.033(3) C46 0.048(2) 0.0327(19) 0.0325(18) -0.0025(15) -0.0047(15) 0.0036(16) C47 0.054(2) 0.0296(18) 0.039(2) -0.0014(15) -0.0148(17) 0.0055(17) C48 0.047(2) 0.049(2) 0.067(3) -0.002(2) -0.003(2) -0.0135(19) C49 0.0352(18) 0.0265(17) 0.0369(19) 0.0020(14) -0.0040(15) 0.0038(14) C50 0.0360(18) 0.0339(18) 0.0334(18) 0.0057(15) -0.0005(14) 0.0075(15) C51 0.0281(17) 0.0387(19) 0.0285(17) 0.0013(14) 0.0005(13) 0.0041(14) C52 0.0378(19) 0.0349(19) 0.0365(19) 0.0031(15) -0.0007(15) 0.0065(15) C53 0.0359(19) 0.044(2) 0.0277(17) 0.0059(15) -0.0016(14) 0.0064(16) C54 0.0236(16) 0.045(2) 0.0253(16) -0.0020(14) 0.0008(13) 0.0040(14) C55 0.0364(19) 0.0340(18) 0.0368(19) -0.0008(15) 0.0010(15) 0.0052(15) C56 0.041(2) 0.0374(19) 0.0301(18) 0.0056(15) -0.0003(15) 0.0042(15) C57 0.0251(16) 0.0343(18) 0.0318(17) 0.0025(14) -0.0012(13) 0.0027(13) C58 0.0318(18) 0.051(2) 0.0262(17) -0.0013(15) -0.0007(14) 0.0035(16) C59 0.0260(17) 0.051(2) 0.0335(18) -0.0024(16) 0.0047(14) 0.0030(15) C60 0.0290(17) 0.0300(17) 0.0315(17) 0.0029(14) -0.0025(13) 0.0026(13) C61 0.0343(18) 0.0413(19) 0.0251(16) 0.0009(14) 0.0000(14) -0.0020(15) C62 0.0268(17) 0.042(2) 0.0300(17) 0.0012(15) 0.0045(13) -0.0018(14) C63 0.0353(18) 0.0360(19) 0.0350(19) -0.0009(15) -0.0011(14) 0.0004(15) C64 0.037(2) 0.046(2) 0.040(2) -0.0096(17) 0.0019(16) -0.0067(17) C65 0.033(2) 0.082(3) 0.067(3) -0.013(3) -0.012(2) -0.003(2) C66 0.044(2) 0.077(3) 0.082(3) -0.020(3) -0.007(2) -0.022(2) C67 0.078(3) 0.045(3) 0.080(4) -0.013(2) 0.012(3) -0.018(2) C68 0.070(4) 0.052(3) 0.177(8) 0.055(4) 0.040(5) 0.017(3) C69 0.085(5) 0.084(4) 0.133(6) 0.024(4) 0.011(4) 0.006(4) C70 0.057(3) 0.098(4) 0.066(3) 0.013(3) -0.018(2) -0.008(3) C71 0.150(7) 0.076(4) 0.096(5) -0.004(4) -0.006(4) 0.031(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 N7 1.959(3) . ? Fe1 N13 1.967(3) . ? Fe1 N1 1.976(3) . ? Fe1 N9 2.004(3) . ? Fe1 N3 2.028(3) . ? Fe1 N15 2.042(3) . ? Fe2 N11 1.960(3) . ? Fe2 N5 1.965(3) . ? Fe2 N17 1.975(3) . ? Fe2 N16 2.009(3) . ? Fe2 N10 2.026(3) . ? Fe2 N4 2.027(3) . ? Cl1 O7 1.383(5) . ? Cl1 O5 1.395(4) . ? Cl1 O6 1.429(4) . ? Cl1 O4 1.439(4) . ? Cl2 O11 1.386(4) . ? Cl2 O8 1.411(3) . ? Cl2 O9 1.428(3) . ? Cl2 O10 1.428(4) . ? Cl3 O15 1.341(4) . ? Cl3 O14 1.397(4) . ? Cl3 O13 1.406(4) . ? Cl3 O12 1.437(4) . ? Cl4 O18A 1.228(8) . ? Cl4 O17 1.398(5) . ? Cl4 O19 1.400(7) . ? Cl4 O16 1.442(4) . ? Cl4 O18B 1.508(8) . ? O1 C13 1.387(4) . ? O1 C10 1.396(4) . ? O2 C32 1.387(4) . ? O2 C35 1.396(4) . ? O3 C57 1.393(4) . ? O3 C54 1.397(4) . ? N1 C4 1.331(4) . ? N1 C1 1.364(4) . ? N2 C4 1.344(4) . ? N2 C2 1.359(5) . ? N2 C3 1.462(5) . ? N3 C5 1.283(4) . ? N3 C7 1.440(4) . ? N4 C19 1.290(4) . ? N4 C16 1.439(4) . ? N5 C20 1.328(4) . ? N5 C21 1.366(4) . ? N6 C20 1.346(4) . ? N6 C22 1.360(5) . ? N6 C23 1.464(5) . ? N7 C27 1.330(4) . ? N7 C24 1.368(4) . ? N8 C27 1.355(4) . ? N8 C25 1.362(5) . ? N8 C26 1.471(5) . ? N9 C28 1.293(4) . ? N9 C29 1.441(4) . ? N10 C41 1.289(4) . ? N10 C38 1.437(4) . ? N11 C42 1.335(5) . ? N11 C43 1.364(5) . ? N12 C42 1.358(5) . ? N12 C44 1.361(7) . ? N12 C45 1.458(6) . ? N13 C49 1.331(4) . ? N13 C46 1.368(4) . ? N14 C49 1.342(4) . ? N14 C47 1.366(5) . ? N14 C48 1.467(5) . ? N15 C50 1.294(5) . ? N15 C51 1.429(4) . ? N16 C63 1.288(4) . ? N16 C60 1.444(4) . ? N17 C64 1.335(5) . ? N17 C65 1.370(5) . ? N18 C64 1.349(5) . ? N18 C66 1.364(6) . ? N18 C67 1.463(6) . ? N19 C68 1.281(13) . ? N20 C70 1.133(7) . ? C1 C2 1.367(5) . ? C4 C5 1.438(5) . ? C7 C12 1.368(5) . ? C7 C8 1.375(5) . ? C8 C9 1.388(5) . ? C9 C10 1.369(6) . ? C10 C11 1.354(5) . ? C11 C12 1.394(5) . ? C13 C14 1.372(5) . ? C13 C18 1.374(5) . ? C14 C15 1.389(5) . ? C15 C16 1.385(5) . ? C16 C17 1.376(5) . ? C17 C18 1.385(5) . ? C19 C20 1.443(5) . ? C21 C22 1.361(5) . ? C24 C25 1.346(6) . ? C27 C28 1.436(5) . ? C29 C34 1.366(5) . ? C29 C30 1.370(5) . ? C30 C31 1.392(5) . ? C31 C32 1.375(5) . ? C32 C33 1.370(5) . ? C33 C34 1.378(5) . ? C35 C36 1.372(5) . ? C35 C40 1.376(5) . ? C36 C37 1.384(5) . ? C37 C38 1.376(5) . ? C38 C39 1.390(5) . ? C39 C40 1.386(5) . ? C41 C42 1.423(5) . ? C43 C44 1.359(7) . ? C46 C47 1.351(5) . ? C49 C50 1.435(5) . ? C51 C56 1.385(5) . ? C51 C52 1.395(5) . ? C52 C53 1.390(5) . ? C53 C54 1.371(5) . ? C54 C55 1.381(5) . ? C55 C56 1.384(5) . ? C57 C62 1.378(5) . ? C57 C58 1.385(5) . ? C58 C59 1.385(5) . ? C59 C60 1.374(5) . ? C60 C61 1.379(5) . ? C61 C62 1.385(5) . ? C63 C64 1.432(5) . ? C65 C66 1.359(7) . ? C68 C69 1.423(11) . ? C70 C71 1.466(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Fe1 N13 88.28(12) . . ? N7 Fe1 N1 90.38(12) . . ? N13 Fe1 N1 88.93(11) . . ? N7 Fe1 N9 80.41(11) . . ? N13 Fe1 N9 93.86(11) . . ? N1 Fe1 N9 170.28(11) . . ? N7 Fe1 N3 89.91(11) . . ? N13 Fe1 N3 168.96(11) . . ? N1 Fe1 N3 80.19(11) . . ? N9 Fe1 N3 96.57(11) . . ? N7 Fe1 N15 167.50(12) . . ? N13 Fe1 N15 80.02(11) . . ? N1 Fe1 N15 93.76(11) . . ? N9 Fe1 N15 95.90(11) . . ? N3 Fe1 N15 102.41(11) . . ? N11 Fe2 N5 88.96(12) . . ? N11 Fe2 N17 90.91(13) . . ? N5 Fe2 N17 94.99(13) . . ? N11 Fe2 N16 93.87(12) . . ? N5 Fe2 N16 174.57(12) . . ? N17 Fe2 N16 80.35(12) . . ? N11 Fe2 N10 79.90(12) . . ? N5 Fe2 N10 90.54(12) . . ? N17 Fe2 N10 169.20(12) . . ? N16 Fe2 N10 94.51(11) . . ? N11 Fe2 N4 168.49(12) . . ? N5 Fe2 N4 79.53(11) . . ? N17 Fe2 N4 89.86(12) . . ? N16 Fe2 N4 97.58(11) . . ? N10 Fe2 N4 100.29(11) . . ? O7 Cl1 O5 106.7(4) . . ? O7 Cl1 O6 113.7(4) . . ? O5 Cl1 O6 106.6(3) . . ? O7 Cl1 O4 109.4(3) . . ? O5 Cl1 O4 109.0(2) . . ? O6 Cl1 O4 111.2(2) . . ? O11 Cl2 O8 111.7(3) . . ? O11 Cl2 O9 110.6(3) . . ? O8 Cl2 O9 111.8(2) . . ? O11 Cl2 O10 107.7(4) . . ? O8 Cl2 O10 109.1(3) . . ? O9 Cl2 O10 105.8(2) . . ? O15 Cl3 O14 111.5(4) . . ? O15 Cl3 O13 111.6(3) . . ? O14 Cl3 O13 110.7(3) . . ? O15 Cl3 O12 108.5(4) . . ? O14 Cl3 O12 106.6(3) . . ? O13 Cl3 O12 107.6(3) . . ? O18A Cl4 O17 146.0(14) . . ? O18A Cl4 O19 90.3(12) . . ? O17 Cl4 O19 97.7(5) . . ? O18A Cl4 O16 102.4(8) . . ? O17 Cl4 O16 104.2(3) . . ? O19 Cl4 O16 114.2(5) . . ? O18A Cl4 O18B 59.5(11) . . ? O17 Cl4 O18B 91.0(7) . . ? O19 Cl4 O18B 129.7(8) . . ? O16 Cl4 O18B 111.3(5) . . ? C13 O1 C10 117.9(3) . . ? C32 O2 C35 117.2(3) . . ? C57 O3 C54 116.8(2) . . ? C4 N1 C1 106.6(3) . . ? C4 N1 Fe1 112.2(2) . . ? C1 N1 Fe1 139.6(2) . . ? C4 N2 C2 107.2(3) . . ? C4 N2 C3 126.3(3) . . ? C2 N2 C3 126.5(3) . . ? C5 N3 C7 116.0(3) . . ? C5 N3 Fe1 114.1(2) . . ? C7 N3 Fe1 129.7(2) . . ? C19 N4 C16 117.4(3) . . ? C19 N4 Fe2 115.6(2) . . ? C16 N4 Fe2 126.9(2) . . ? C20 N5 C21 106.2(3) . . ? C20 N5 Fe2 114.6(2) . . ? C21 N5 Fe2 139.1(3) . . ? C20 N6 C22 106.7(3) . . ? C20 N6 C23 127.5(3) . . ? C22 N6 C23 125.8(3) . . ? C27 N7 C24 106.3(3) . . ? C27 N7 Fe1 113.4(2) . . ? C24 N7 Fe1 139.3(3) . . ? C27 N8 C25 106.3(3) . . ? C27 N8 C26 126.4(3) . . ? C25 N8 C26 127.3(3) . . ? C28 N9 C29 116.2(3) . . ? C28 N9 Fe1 115.0(2) . . ? C29 N9 Fe1 128.5(2) . . ? C41 N10 C38 117.3(3) . . ? C41 N10 Fe2 114.6(2) . . ? C38 N10 Fe2 128.0(2) . . ? C42 N11 C43 106.6(3) . . ? C42 N11 Fe2 113.3(2) . . ? C43 N11 Fe2 138.3(3) . . ? C42 N12 C44 106.2(4) . . ? C42 N12 C45 127.0(4) . . ? C44 N12 C45 126.6(4) . . ? C49 N13 C46 105.8(3) . . ? C49 N13 Fe1 113.8(2) . . ? C46 N13 Fe1 138.9(2) . . ? C49 N14 C47 106.4(3) . . ? C49 N14 C48 126.1(3) . . ? C47 N14 C48 127.5(3) . . ? C50 N15 C51 115.2(3) . . ? C50 N15 Fe1 114.1(2) . . ? C51 N15 Fe1 130.6(2) . . ? C63 N16 C60 115.1(3) . . ? C63 N16 Fe2 115.2(2) . . ? C60 N16 Fe2 129.6(2) . . ? C64 N17 C65 105.9(4) . . ? C64 N17 Fe2 112.6(2) . . ? C65 N17 Fe2 141.4(3) . . ? C64 N18 C66 105.5(4) . . ? C64 N18 C67 127.1(4) . . ? C66 N18 C67 127.2(4) . . ? N1 C1 C2 108.4(3) . . ? N2 C2 C1 107.2(3) . . ? N1 C4 N2 110.6(3) . . ? N1 C4 C5 117.2(3) . . ? N2 C4 C5 132.1(3) . . ? N3 C5 C4 114.5(3) . . ? C12 C7 C8 120.2(3) . . ? C12 C7 N3 120.4(3) . . ? C8 C7 N3 119.4(3) . . ? C7 C8 C9 119.8(4) . . ? C10 C9 C8 119.3(4) . . ? C11 C10 C9 121.4(3) . . ? C11 C10 O1 119.7(3) . . ? C9 C10 O1 118.6(4) . . ? C10 C11 C12 119.4(3) . . ? C7 C12 C11 119.8(3) . . ? C14 C13 C18 121.1(3) . . ? C14 C13 O1 122.3(3) . . ? C18 C13 O1 116.4(3) . . ? C13 C14 C15 119.3(3) . . ? C16 C15 C14 120.0(3) . . ? C17 C16 C15 119.8(3) . . ? C17 C16 N4 119.4(3) . . ? C15 C16 N4 120.8(3) . . ? C16 C17 C18 120.3(3) . . ? C13 C18 C17 119.4(3) . . ? N4 C19 C20 113.7(3) . . ? N5 C20 N6 111.1(3) . . ? N5 C20 C19 116.5(3) . . ? N6 C20 C19 132.4(3) . . ? C22 C21 N5 108.6(3) . . ? N6 C22 C21 107.4(3) . . ? C25 C24 N7 108.8(3) . . ? C24 C25 N8 108.0(3) . . ? N7 C27 N8 110.7(3) . . ? N7 C27 C28 116.7(3) . . ? N8 C27 C28 132.5(3) . . ? N9 C28 C27 113.9(3) . . ? C34 C29 C30 119.7(3) . . ? C34 C29 N9 119.5(3) . . ? C30 C29 N9 120.8(3) . . ? C29 C30 C31 120.3(3) . . ? C32 C31 C30 119.2(3) . . ? C33 C32 C31 120.3(3) . . ? C33 C32 O2 116.0(3) . . ? C31 C32 O2 123.7(3) . . ? C32 C33 C34 119.9(3) . . ? C29 C34 C33 120.6(3) . . ? C36 C35 C40 121.2(3) . . ? C36 C35 O2 118.6(3) . . ? C40 C35 O2 120.1(3) . . ? C35 C36 C37 119.3(3) . . ? C38 C37 C36 120.2(3) . . ? C37 C38 C39 120.4(3) . . ? C37 C38 N10 120.2(3) . . ? C39 C38 N10 119.4(3) . . ? C40 C39 C38 119.2(3) . . ? C35 C40 C39 119.7(3) . . ? N10 C41 C42 114.4(3) . . ? N11 C42 N12 110.6(4) . . ? N11 C42 C41 116.9(3) . . ? N12 C42 C41 132.5(4) . . ? C44 C43 N11 108.4(4) . . ? C43 C44 N12 108.2(4) . . ? C47 C46 N13 108.9(3) . . ? C46 C47 N14 107.6(3) . . ? N13 C49 N14 111.3(3) . . ? N13 C49 C50 116.9(3) . . ? N14 C49 C50 131.8(3) . . ? N15 C50 C49 114.7(3) . . ? C56 C51 C52 120.3(3) . . ? C56 C51 N15 121.0(3) . . ? C52 C51 N15 118.7(3) . . ? C53 C52 C51 118.8(3) . . ? C54 C53 C52 120.4(3) . . ? C53 C54 C55 121.1(3) . . ? C53 C54 O3 120.1(3) . . ? C55 C54 O3 118.9(3) . . ? C54 C55 C56 119.1(3) . . ? C55 C56 C51 120.3(3) . . ? C62 C57 C58 120.4(3) . . ? C62 C57 O3 116.6(3) . . ? C58 C57 O3 123.0(3) . . ? C57 C58 C59 118.9(3) . . ? C60 C59 C58 120.9(3) . . ? C59 C60 C61 120.0(3) . . ? C59 C60 N16 119.3(3) . . ? C61 C60 N16 120.7(3) . . ? C60 C61 C62 119.7(3) . . ? C57 C62 C61 120.2(3) . . ? N16 C63 C64 113.9(3) . . ? N17 C64 N18 111.8(3) . . ? N17 C64 C63 117.5(3) . . ? N18 C64 C63 130.2(4) . . ? C66 C65 N17 108.2(4) . . ? C65 C66 N18 108.7(4) . . ? N19 C68 C69 174.8(8) . . ? N20 C70 C71 178.0(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.726 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.084