# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Yoshiki Ohgo' _publ_contact_author_address ; Department of Chemistry Toho University School of Medicine 5-21-16 omorinishi ota-ku tokyo 143-8540 JAPAN ; _publ_contact_author_email YOHGO@MED.TOHO-U.AC.JP _publ_section_title ; Novel spin transition between S=5/2 and S=3/2 in highly saddled iron(III) porphyrin complexes at extremely low temperature ; loop_ _publ_author_name 'Yoshiki Ohgo' 'Yuya Chiba' 'Daisuke Hashizume' 'Mikio Nakamura' 'Tomoji Ozeki' 'Hidehiro Uekusa' data_[Fe(OMTDMPP)(H2O)]ClO4 _database_code_depnum_ccdc_archive 'CCDC 297040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; aqua[2,3,7,8,12,13,17,18-octamethyl-5,10,15,20- tetrakis(3,5-dimethylphenyl)porphyrinato-\/Yk^4^N]iron(III) perchlorate ; _chemical_name_common porphyrin _chemical_melting_point ? _chemical_formula_moiety 'C60 H62 Fe N4 O, Cl O4' _chemical_formula_sum 'C60 H62 Fe N4 O5 Cl' _chemical_formula_weight 1010.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0019 0.0015 ; International Tables Vol C Tables 6.1.1.4 and S. Sasaki (1989). Numerical Tables of Anomalous Scattering Factors Calculated by the Cromer and Liberman's Method, KEK Report, 88-14, 1-136. ; H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0037 0.0031 ; International Tables Vol C Tables 6.1.1.4 and S. Sasaki (1989). Numerical Tables of Anomalous Scattering Factors Calculated by the Cromer and Liberman's Method, KEK Report, 88-14, 1-136. ; O O 0.0065 0.0057 ; International Tables Vol C Tables 6.1.1.4 and S. Sasaki (1989). Numerical Tables of Anomalous Scattering Factors Calculated by the Cromer and Liberman's Method, KEK Report, 88-14, 1-136. ; Cl Cl 0.1253 0.1495 ; International Tables Vol C Tables 6.1.1.4 and S. Sasaki (1989). Numerical Tables of Anomalous Scattering Factors Calculated by the Cromer and Liberman's Method, KEK Report, 88-14, 1-136. ; Fe Fe 0.2961 0.8004 ; International Tables Vol C Tables 6.1.1.4 and S. Sasaki (1989). Numerical Tables of Anomalous Scattering Factors Calculated by the Cromer and Liberman's Method, KEK Report, 88-14, 1-136. ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 14.4113(3) _cell_length_b 16.9296(4) _cell_length_c 21.1176(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5152.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110 _cell_measurement_reflns_used 184351 _cell_measurement_theta_min 0.93 _cell_measurement_theta_max 32.09 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2132 _exptl_absorpt_coefficient_mu 0.324 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8183 _exptl_absorpt_correction_T_max 0.9686 _exptl_absorpt_process_details ; MULABS, Blessing, R. H., 1995, Acta Cryst. A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.68878 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'KEK PF-AR NW2 Station Undulator' _diffrn_radiation_monochromator Si(111) _diffrn_measurement_device_type 'Rigaku AFC-8 with Mercury CCD detector' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 14.7059 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53820 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.0858 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 32.09 _reflns_number_total 18104 _reflns_number_gt 13222 _reflns_threshold_expression I>2\s(I) _computing_data_collection CrystalClear _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution SIR-2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SV (Nemoto & Ohashi, 1993)' _computing_publication_material SHELXL-97 _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^)+(0.1031P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _publ_section_exptl_refinement ; Positions of hydrogen atoms were constrained to have C-H distances of 0.96 and 0.93 \%A for methyl and aromatic groups, respectively. The hydrogen atoms on the aqua ligand are fixed. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.034(12) _refine_ls_number_reflns 18104 _refine_ls_number_parameters 668 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1663 _refine_ls_wR_factor_gt 0.1560 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.40093(2) 0.602341(17) 0.396426(16) 0.01852(8) Uani 1 1 d . . . Cl1 Cl 0.14968(5) 0.73659(4) 0.51478(4) 0.03485(16) Uani 1 1 d . . . N1 N 0.44098(16) 0.53039(11) 0.46273(11) 0.0219(4) Uani 1 1 d . . . N2 N 0.52938(14) 0.60608(11) 0.36509(10) 0.0197(4) Uani 1 1 d . . . N3 N 0.36037(15) 0.66399(11) 0.32352(10) 0.0209(4) Uani 1 1 d . . . N4 N 0.27176(14) 0.56555(10) 0.40746(10) 0.0197(4) Uani 1 1 d . . . O1 O 0.40029(15) 0.69986(10) 0.45446(10) 0.0305(4) Uani 1 1 d . . . H01 H 0.3379 0.7235 0.4634 0.046 Uiso 1 1 d . . . H02 H 0.4618 0.7085 0.4750 0.046 Uiso 1 1 d . . . O2 O 0.22985(17) 0.76499(14) 0.47943(16) 0.0580(8) Uani 1 1 d . . . O3 O 0.06951(17) 0.77622(15) 0.48865(13) 0.0474(6) Uani 1 1 d . . . O4 O 0.1590(2) 0.7587(2) 0.57874(14) 0.0690(9) Uani 1 1 d . . . O5 O 0.14107(19) 0.65405(13) 0.50569(15) 0.0546(7) Uani 1 1 d . . . C1 C 0.38447(18) 0.51040(13) 0.51288(12) 0.0230(5) Uani 1 1 d . . . C2 C 0.4383(2) 0.50694(14) 0.57029(13) 0.0260(5) Uani 1 1 d . . . C3 C 0.5292(2) 0.51763(14) 0.55384(13) 0.0258(5) Uani 1 1 d . . . C4 C 0.53158(19) 0.52847(13) 0.48585(13) 0.0229(5) Uani 1 1 d . . . C5 C 0.60827(18) 0.52995(12) 0.44640(12) 0.0226(5) Uani 1 1 d . . . C6 C 0.60333(18) 0.55892(12) 0.38453(11) 0.0202(4) Uani 1 1 d . . . C7 C 0.67344(17) 0.55557(13) 0.33615(13) 0.0220(5) Uani 1 1 d . . . C8 C 0.64519(17) 0.60613(13) 0.28875(12) 0.0211(4) Uani 1 1 d . . . C9 C 0.55824(17) 0.64019(12) 0.30914(12) 0.0199(4) Uani 1 1 d . . . C10 C 0.51106(18) 0.70550(12) 0.28294(12) 0.0212(5) Uani 1 1 d . . . C11 C 0.41884(18) 0.72156(13) 0.29782(12) 0.0226(5) Uani 1 1 d . . . C12 C 0.3644(2) 0.79169(13) 0.28369(13) 0.0256(5) Uani 1 1 d . . . C13 C 0.27464(19) 0.77381(13) 0.29568(13) 0.0250(5) Uani 1 1 d . . . C14 C 0.27148(18) 0.69314(13) 0.31830(12) 0.0223(5) Uani 1 1 d . . . C15 C 0.19345(18) 0.64710(13) 0.32956(13) 0.0221(5) Uani 1 1 d . . . C16 C 0.19810(17) 0.57896(13) 0.36684(12) 0.0213(5) Uani 1 1 d . . . C17 C 0.12650(18) 0.52077(14) 0.37780(13) 0.0245(5) Uani 1 1 d . . . C18 C 0.15403(18) 0.47646(13) 0.42860(13) 0.0229(5) Uani 1 1 d . . . C19 C 0.24289(17) 0.50696(12) 0.44902(12) 0.0211(5) Uani 1 1 d . . . C20 C 0.29163(19) 0.48916(13) 0.50431(12) 0.0239(5) Uani 1 1 d . . . C21 C 0.4031(3) 0.50151(19) 0.63692(14) 0.0379(6) Uani 1 1 d . . . H21A H 0.4426 0.5317 0.6644 0.057 Uiso 1 1 calc R . . H21B H 0.4029 0.4473 0.6502 0.057 Uiso 1 1 calc R . . H21C H 0.3411 0.5221 0.6389 0.057 Uiso 1 1 calc R . . C22 C 0.6081(2) 0.52661(19) 0.59953(15) 0.0366(6) Uani 1 1 d . . . H22A H 0.6399 0.4771 0.6038 0.055 Uiso 1 1 calc R . . H22B H 0.5845 0.5427 0.6400 0.055 Uiso 1 1 calc R . . H22C H 0.6505 0.5659 0.5840 0.055 Uiso 1 1 calc R . . C23 C 0.75867(19) 0.50540(15) 0.33407(15) 0.0283(5) Uani 1 1 d . . . H23A H 0.8091 0.5330 0.3538 0.042 Uiso 1 1 calc R . . H23B H 0.7742 0.4941 0.2908 0.042 Uiso 1 1 calc R . . H23C H 0.7474 0.4568 0.3562 0.042 Uiso 1 1 calc R . . C24 C 0.6928(2) 0.61724(16) 0.22654(14) 0.0294(6) Uani 1 1 d . . . H24A H 0.7239 0.5692 0.2149 0.044 Uiso 1 1 calc R . . H24B H 0.7373 0.6592 0.2300 0.044 Uiso 1 1 calc R . . H24C H 0.6477 0.6304 0.1948 0.044 Uiso 1 1 calc R . . C25 C 0.4010(2) 0.87156(14) 0.26409(16) 0.0351(6) Uani 1 1 d . . . H25A H 0.3670 0.9122 0.2858 0.053 Uiso 1 1 calc R . . H25B H 0.3936 0.8780 0.2192 0.053 Uiso 1 1 calc R . . H25C H 0.4655 0.8753 0.2749 0.053 Uiso 1 1 calc R . . C26 C 0.1951(2) 0.83177(15) 0.29328(16) 0.0329(6) Uani 1 1 d . . . H26A H 0.1642 0.8276 0.2531 0.049 Uiso 1 1 calc R . . H26B H 0.2185 0.8845 0.2985 0.049 Uiso 1 1 calc R . . H26C H 0.1520 0.8202 0.3267 0.049 Uiso 1 1 calc R . . C27 C 0.0409(2) 0.50631(16) 0.33855(16) 0.0321(6) Uani 1 1 d . . . H27A H -0.0110 0.5329 0.3575 0.048 Uiso 1 1 calc R . . H27B H 0.0286 0.4506 0.3367 0.048 Uiso 1 1 calc R . . H27C H 0.0506 0.5262 0.2965 0.048 Uiso 1 1 calc R . . C28 C 0.1022(2) 0.40676(14) 0.45440(15) 0.0317(6) Uani 1 1 d . . . H28A H 0.0493 0.3961 0.4281 0.048 Uiso 1 1 calc R . . H28B H 0.0819 0.4181 0.4967 0.048 Uiso 1 1 calc R . . H28C H 0.1422 0.3614 0.4549 0.048 Uiso 1 1 calc R . . C29 C 0.69829(18) 0.50038(13) 0.47316(13) 0.0237(5) Uani 1 1 d . . . C30 C 0.7034(2) 0.42263(13) 0.49632(14) 0.0276(5) Uani 1 1 d . . . H30 H 0.6528 0.3891 0.4915 0.033 Uiso 1 1 calc R . . C31 C 0.7823(2) 0.39549(15) 0.52597(14) 0.0321(6) Uani 1 1 d . . . C32 C 0.8576(2) 0.44587(16) 0.53237(16) 0.0340(6) Uani 1 1 d . . . H32 H 0.9111 0.4276 0.5523 0.041 Uiso 1 1 calc R . . C33 C 0.8552(2) 0.52373(16) 0.50959(15) 0.0315(6) Uani 1 1 d . . . C34 C 0.7747(2) 0.55007(14) 0.47966(14) 0.0281(5) Uani 1 1 d . . . H34 H 0.7721 0.6013 0.4639 0.034 Uiso 1 1 calc R . . C35 C 0.7843(3) 0.31353(17) 0.55331(19) 0.0508(10) Uani 1 1 d . . . H35A H 0.8269 0.3119 0.5882 0.076 Uiso 1 1 calc R . . H35B H 0.8039 0.2768 0.5213 0.076 Uiso 1 1 calc R . . H35C H 0.7233 0.2995 0.5678 0.076 Uiso 1 1 calc R . . C36 C 0.9371(2) 0.57790(19) 0.5174(2) 0.0444(8) Uani 1 1 d . . . H36A H 0.9183 0.6243 0.5402 0.067 Uiso 1 1 calc R . . H36B H 0.9600 0.5929 0.4764 0.067 Uiso 1 1 calc R . . H36C H 0.9851 0.5511 0.5405 0.067 Uiso 1 1 calc R . . C37 C 0.56097(19) 0.75862(13) 0.23842(13) 0.0247(5) Uani 1 1 d . . . C38 C 0.6374(2) 0.80204(15) 0.25937(15) 0.0289(5) Uani 1 1 d . . . H38 H 0.6595 0.7951 0.3004 0.035 Uiso 1 1 calc R . . C39 C 0.6807(2) 0.85591(16) 0.21874(16) 0.0342(6) Uani 1 1 d . . . C40 C 0.6462(2) 0.86559(15) 0.15789(14) 0.0297(6) Uani 1 1 d . . . H40 H 0.6748 0.9014 0.1308 0.036 Uiso 1 1 calc R . . C41 C 0.5706(2) 0.82338(16) 0.13664(14) 0.0318(6) Uani 1 1 d . . . C42 C 0.5288(2) 0.76902(15) 0.17730(14) 0.0285(5) Uani 1 1 d . . . H42 H 0.4786 0.7394 0.1631 0.034 Uiso 1 1 calc R . . C43 C 0.7616(3) 0.9043(2) 0.24115(19) 0.0477(8) Uani 1 1 d . . . H43A H 0.7530 0.9583 0.2286 0.072 Uiso 1 1 calc R . . H43B H 0.8177 0.8842 0.2227 0.072 Uiso 1 1 calc R . . H43C H 0.7657 0.9013 0.2865 0.072 Uiso 1 1 calc R . . C44 C 0.5293(3) 0.8349(2) 0.07175(16) 0.0411(7) Uani 1 1 d . . . H44A H 0.4792 0.8722 0.0742 0.062 Uiso 1 1 calc R . . H44B H 0.5062 0.7853 0.0563 0.062 Uiso 1 1 calc R . . H44C H 0.5760 0.8545 0.0434 0.062 Uiso 1 1 calc R . . C45 C 0.1004(2) 0.67255(14) 0.30385(13) 0.0251(5) Uani 1 1 d . . . C46 C 0.0302(2) 0.69287(17) 0.34529(15) 0.0317(6) Uani 1 1 d . . . H46 H 0.0396 0.6888 0.3887 0.038 Uiso 1 1 calc R . . C47 C -0.0550(2) 0.71952(18) 0.32195(18) 0.0376(7) Uani 1 1 d . . . C48 C -0.0675(2) 0.72316(18) 0.25707(18) 0.0390(7) Uani 1 1 d . . . H48 H -0.1243 0.7404 0.2414 0.047 Uiso 1 1 calc R . . C49 C 0.0016(2) 0.70198(17) 0.21441(17) 0.0360(7) Uani 1 1 d . . . C50 C 0.0874(2) 0.67694(15) 0.23890(14) 0.0305(6) Uani 1 1 d . . . H50 H 0.1354 0.6633 0.2116 0.037 Uiso 1 1 calc R . . C51 C -0.1320(2) 0.7424(3) 0.3672(2) 0.0535(10) Uani 1 1 d . . . H51A H -0.1292 0.7981 0.3754 0.080 Uiso 1 1 calc R . . H51B H -0.1247 0.7140 0.4062 0.080 Uiso 1 1 calc R . . H51C H -0.1909 0.7296 0.3487 0.080 Uiso 1 1 calc R . . C52 C -0.0145(3) 0.7053(2) 0.14375(19) 0.0536(10) Uani 1 1 d . . . H52A H -0.0544 0.6627 0.1313 0.080 Uiso 1 1 calc R . . H52B H 0.0439 0.7007 0.1221 0.080 Uiso 1 1 calc R . . H52C H -0.0430 0.7548 0.1329 0.080 Uiso 1 1 calc R . . C53 C 0.24383(19) 0.44461(14) 0.55545(13) 0.0252(5) Uani 1 1 d . . . C54 C 0.1776(2) 0.48099(15) 0.59344(14) 0.0279(6) Uani 1 1 d . . . H54 H 0.1592 0.5325 0.5846 0.033 Uiso 1 1 calc R . . C55 C 0.1388(2) 0.44139(16) 0.64419(14) 0.0311(6) Uani 1 1 d . . . C56 C 0.1660(2) 0.36281(16) 0.65460(14) 0.0321(6) Uani 1 1 d . . . H56 H 0.1416 0.3360 0.6893 0.039 Uiso 1 1 calc R . . C57 C 0.2275(2) 0.32369(15) 0.61549(13) 0.0308(6) Uani 1 1 d . . . C58 C 0.2687(2) 0.36605(14) 0.56664(13) 0.0280(5) Uani 1 1 d . . . H58 H 0.3131 0.3419 0.5412 0.034 Uiso 1 1 calc R . . C59 C 0.0681(3) 0.47977(19) 0.68562(18) 0.0437(8) Uani 1 1 d . . . H59A H 0.0073 0.4624 0.6735 0.066 Uiso 1 1 calc R . . H59B H 0.0721 0.5361 0.6811 0.066 Uiso 1 1 calc R . . H59C H 0.0795 0.4656 0.7289 0.066 Uiso 1 1 calc R . . C60 C 0.2497(3) 0.23714(16) 0.62464(16) 0.0422(8) Uani 1 1 d . . . H60A H 0.2023 0.2056 0.6051 0.063 Uiso 1 1 calc R . . H60B H 0.2524 0.2254 0.6691 0.063 Uiso 1 1 calc R . . H60C H 0.3086 0.2255 0.6055 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01442(17) 0.01859(11) 0.02255(15) 0.00019(11) -0.00043(14) -0.00019(11) Cl1 0.0227(4) 0.0351(3) 0.0467(4) -0.0134(3) 0.0007(3) 0.0024(2) N1 0.0182(11) 0.0224(8) 0.0252(11) 0.0017(7) -0.0004(8) 0.0007(7) N2 0.0142(10) 0.0213(7) 0.0237(10) 0.0016(7) -0.0030(8) 0.0005(7) N3 0.0146(10) 0.0216(8) 0.0265(10) 0.0022(7) -0.0004(8) 0.0008(7) N4 0.0154(10) 0.0199(7) 0.0239(10) -0.0010(7) -0.0002(8) -0.0017(6) O1 0.0224(10) 0.0308(8) 0.0384(11) -0.0131(7) -0.0010(9) -0.0001(7) O2 0.0296(14) 0.0441(12) 0.100(2) -0.0117(13) 0.0223(14) -0.0013(10) O3 0.0325(14) 0.0587(13) 0.0511(15) -0.0069(12) 0.0000(11) 0.0120(10) O4 0.065(2) 0.096(2) 0.0463(16) -0.0249(16) -0.0130(15) 0.0321(17) O5 0.0495(16) 0.0302(9) 0.084(2) -0.0061(11) 0.0193(15) -0.0027(9) C1 0.0213(14) 0.0235(9) 0.0241(11) 0.0000(8) 0.0006(10) -0.0003(8) C2 0.0281(15) 0.0281(10) 0.0218(12) 0.0010(9) -0.0027(10) -0.0005(9) C3 0.0267(14) 0.0263(10) 0.0244(12) -0.0004(9) -0.0025(11) -0.0021(9) C4 0.0230(13) 0.0207(9) 0.0249(12) 0.0022(8) -0.0059(10) -0.0019(8) C5 0.0199(13) 0.0197(8) 0.0282(12) 0.0004(8) -0.0065(10) -0.0005(8) C6 0.0144(11) 0.0186(7) 0.0275(12) 0.0002(7) -0.0031(10) -0.0008(8) C7 0.0169(12) 0.0207(9) 0.0285(13) -0.0021(8) 0.0000(10) -0.0015(8) C8 0.0134(12) 0.0251(9) 0.0248(11) -0.0013(9) 0.0010(9) -0.0019(8) C9 0.0141(12) 0.0218(9) 0.0239(12) 0.0029(8) 0.0009(9) 0.0002(8) C10 0.0180(13) 0.0233(9) 0.0221(11) 0.0034(8) -0.0003(9) -0.0014(8) C11 0.0180(13) 0.0231(9) 0.0266(12) 0.0017(8) -0.0017(9) -0.0010(8) C12 0.0251(14) 0.0227(9) 0.0290(13) 0.0026(9) -0.0028(11) 0.0011(8) C13 0.0222(14) 0.0237(9) 0.0291(13) 0.0007(9) -0.0016(10) 0.0038(8) C14 0.0176(12) 0.0245(9) 0.0248(12) -0.0005(8) -0.0022(10) 0.0020(8) C15 0.0144(12) 0.0261(9) 0.0259(12) -0.0025(8) -0.0023(10) 0.0022(8) C16 0.0154(12) 0.0245(9) 0.0241(12) -0.0031(8) 0.0000(9) 0.0012(8) C17 0.0164(13) 0.0237(9) 0.0333(13) -0.0054(9) 0.0020(10) -0.0024(8) C18 0.0150(13) 0.0219(9) 0.0318(13) -0.0035(9) 0.0045(10) -0.0013(8) C19 0.0146(12) 0.0201(8) 0.0286(12) -0.0002(8) 0.0027(9) -0.0005(7) C20 0.0247(14) 0.0217(9) 0.0253(12) -0.0008(8) 0.0048(10) 0.0008(8) C21 0.0366(17) 0.0513(15) 0.0258(13) -0.0019(12) 0.0002(14) 0.0000(14) C22 0.0310(17) 0.0497(14) 0.0292(14) -0.0035(12) -0.0080(13) -0.0060(12) C23 0.0179(13) 0.0297(11) 0.0373(15) -0.0014(10) 0.0023(11) 0.0040(9) C24 0.0201(14) 0.0384(13) 0.0298(14) 0.0022(10) 0.0029(11) 0.0023(10) C25 0.0282(15) 0.0229(9) 0.0543(18) 0.0067(10) 0.0014(15) 0.0020(10) C26 0.0236(15) 0.0307(11) 0.0445(17) 0.0011(11) 0.0007(13) 0.0084(10) C27 0.0207(15) 0.0360(12) 0.0395(17) -0.0018(11) -0.0049(12) -0.0034(10) C28 0.0257(14) 0.0255(10) 0.0440(15) 0.0021(10) -0.0007(13) -0.0068(10) C29 0.0174(13) 0.0238(9) 0.0299(13) 0.0024(9) -0.0056(10) 0.0005(8) C30 0.0252(14) 0.0224(9) 0.0353(14) 0.0018(9) -0.0069(11) -0.0019(9) C31 0.0370(17) 0.0240(9) 0.0352(14) 0.0020(10) -0.0134(12) 0.0017(10) C32 0.0237(15) 0.0351(12) 0.0431(17) 0.0009(11) -0.0093(13) 0.0075(11) C33 0.0192(15) 0.0365(12) 0.0387(16) -0.0024(11) -0.0074(12) -0.0028(10) C34 0.0258(15) 0.0238(9) 0.0346(14) 0.0031(9) -0.0059(11) -0.0004(9) C35 0.067(3) 0.0284(12) 0.057(2) 0.0088(13) -0.024(2) 0.0042(14) C36 0.0258(17) 0.0457(15) 0.062(2) 0.0024(15) -0.0152(16) -0.0088(12) C37 0.0187(13) 0.0255(9) 0.0298(13) 0.0073(9) 0.0011(10) -0.0001(9) C38 0.0226(14) 0.0292(10) 0.0349(14) 0.0058(10) 0.0015(11) -0.0028(9) C39 0.0244(16) 0.0310(11) 0.0472(18) 0.0107(11) 0.0036(13) -0.0035(10) C40 0.0236(14) 0.0296(11) 0.0358(15) 0.0114(10) 0.0071(12) 0.0004(10) C41 0.0312(16) 0.0317(11) 0.0325(14) 0.0102(10) 0.0064(12) 0.0092(10) C42 0.0233(14) 0.0305(10) 0.0317(14) 0.0082(10) -0.0011(11) 0.0012(9) C43 0.040(2) 0.0434(15) 0.060(2) 0.0100(16) 0.0025(17) -0.0132(14) C44 0.0351(19) 0.0542(17) 0.0339(16) 0.0161(14) 0.0011(14) 0.0121(14) C45 0.0165(13) 0.0288(9) 0.0300(12) 0.0016(9) -0.0031(11) 0.0020(9) C46 0.0211(15) 0.0381(12) 0.0358(16) 0.0041(11) -0.0016(12) 0.0013(10) C47 0.0180(15) 0.0443(14) 0.0505(19) 0.0055(13) 0.0038(13) 0.0063(11) C48 0.0209(16) 0.0432(14) 0.053(2) 0.0057(14) -0.0140(14) 0.0043(11) C49 0.0266(16) 0.0395(13) 0.0419(17) 0.0004(12) -0.0148(13) 0.0017(11) C50 0.0234(16) 0.0361(12) 0.0321(14) -0.0005(10) -0.0053(11) 0.0040(10) C51 0.0232(18) 0.077(2) 0.060(2) 0.015(2) 0.0146(16) 0.0239(16) C52 0.048(2) 0.067(2) 0.046(2) -0.0003(17) -0.0225(18) 0.0132(18) C53 0.0241(14) 0.0257(10) 0.0257(12) 0.0008(9) 0.0021(10) -0.0046(9) C54 0.0230(14) 0.0274(10) 0.0333(15) 0.0032(10) 0.0038(11) -0.0004(9) C55 0.0292(15) 0.0328(11) 0.0313(14) -0.0028(10) 0.0049(12) -0.0057(10) C56 0.0356(17) 0.0336(12) 0.0272(13) 0.0045(10) 0.0024(12) -0.0059(11) C57 0.0369(17) 0.0271(10) 0.0285(14) 0.0028(9) 0.0004(12) -0.0066(10) C58 0.0310(15) 0.0252(10) 0.0279(13) 0.0029(9) 0.0049(11) -0.0004(9) C59 0.042(2) 0.0418(14) 0.047(2) -0.0015(13) 0.0189(16) -0.0006(13) C60 0.060(2) 0.0286(12) 0.0383(16) 0.0060(11) 0.0024(16) -0.0021(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.944(2) . ? Fe1 N3 1.950(2) . ? Fe1 N2 1.967(2) . ? Fe1 N4 1.977(2) . ? Fe1 O1 2.0561(17) . ? Cl1 O4 1.408(3) . ? Cl1 O5 1.416(2) . ? Cl1 O3 1.445(2) . ? Cl1 O2 1.457(3) . ? N1 C1 1.378(3) . ? N1 C4 1.394(4) . ? N2 C9 1.379(3) . ? N2 C6 1.393(3) . ? N3 C14 1.377(3) . ? N3 C11 1.398(3) . ? N4 C16 1.384(3) . ? N4 C19 1.388(3) . ? O1 H01 1.002 . ? O1 H02 0.998 . ? C1 C20 1.397(4) . ? C1 C2 1.440(4) . ? C2 C3 1.367(4) . ? C2 C21 1.499(4) . ? C3 C4 1.448(4) . ? C3 C22 1.499(4) . ? C4 C5 1.384(4) . ? C5 C6 1.397(3) . ? C5 C29 1.501(4) . ? C6 C7 1.438(4) . ? C7 C8 1.379(3) . ? C7 C23 1.494(4) . ? C8 C9 1.445(3) . ? C8 C24 1.494(4) . ? C9 C10 1.411(3) . ? C10 C11 1.392(4) . ? C10 C37 1.487(3) . ? C11 C12 1.454(3) . ? C12 C13 1.352(4) . ? C12 C25 1.509(3) . ? C13 C14 1.447(3) . ? C13 C26 1.510(4) . ? C14 C15 1.389(4) . ? C15 C16 1.398(3) . ? C15 C45 1.510(4) . ? C16 C17 1.445(3) . ? C17 C18 1.368(4) . ? C17 C27 1.506(4) . ? C18 C19 1.447(4) . ? C18 C28 1.499(3) . ? C19 C20 1.395(4) . ? C20 C53 1.486(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.393(4) . ? C29 C30 1.406(3) . ? C30 C31 1.377(4) . ? C30 H30 0.9300 . ? C31 C32 1.387(4) . ? C31 C35 1.503(4) . ? C32 C33 1.404(4) . ? C32 H32 0.9300 . ? C33 C34 1.394(4) . ? C33 C36 1.503(4) . ? C34 H34 0.9300 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C42 1.383(4) . ? C37 C38 1.396(4) . ? C38 C39 1.399(4) . ? C38 H38 0.9300 . ? C39 C40 1.387(5) . ? C39 C43 1.501(4) . ? C40 C41 1.378(4) . ? C40 H40 0.9300 . ? C41 C42 1.396(4) . ? C41 C44 1.507(4) . ? C42 H42 0.9300 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.381(4) . ? C45 C50 1.386(4) . ? C46 C47 1.398(4) . ? C46 H46 0.9300 . ? C47 C48 1.383(5) . ? C47 C51 1.515(5) . ? C48 C49 1.389(5) . ? C48 H48 0.9300 . ? C49 C50 1.406(4) . ? C49 C52 1.511(5) . ? C50 H50 0.9300 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.391(4) . ? C53 C58 1.398(3) . ? C54 C55 1.382(4) . ? C54 H54 0.9300 . ? C55 C56 1.404(4) . ? C55 C59 1.491(4) . ? C56 C57 1.381(4) . ? C56 H56 0.9300 . ? C57 C58 1.389(4) . ? C57 C60 1.512(4) . ? C58 H58 0.9300 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 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 N1 Fe1 N3 173.42(9) . . ? N1 Fe1 N2 89.03(9) . . ? N3 Fe1 N2 89.96(9) . . ? N1 Fe1 N4 89.84(9) . . ? N3 Fe1 N4 88.83(9) . . ? N2 Fe1 N4 159.41(8) . . ? N1 Fe1 O1 94.31(9) . . ? N3 Fe1 O1 92.27(8) . . ? N2 Fe1 O1 100.30(8) . . ? N4 Fe1 O1 100.29(8) . . ? O4 Cl1 O5 113.6(2) . . ? O4 Cl1 O3 108.61(17) . . ? O5 Cl1 O3 109.65(17) . . ? O4 Cl1 O2 109.2(2) . . ? O5 Cl1 O2 109.00(15) . . ? O3 Cl1 O2 106.56(17) . . ? C1 N1 C4 106.2(2) . . ? C1 N1 Fe1 122.14(17) . . ? C4 N1 Fe1 123.01(16) . . ? C9 N2 C6 105.2(2) . . ? C9 N2 Fe1 125.83(16) . . ? C6 N2 Fe1 127.02(16) . . ? C14 N3 C11 106.25(19) . . ? C14 N3 Fe1 122.26(17) . . ? C11 N3 Fe1 119.94(17) . . ? C16 N4 C19 106.2(2) . . ? C16 N4 Fe1 126.70(16) . . ? C19 N4 Fe1 125.59(17) . . ? Fe1 O1 H01 115.98 . . ? Fe1 O1 H02 111.94 . . ? H01 O1 H02 130.93 . . ? N1 C1 C20 122.0(2) . . ? N1 C1 C2 109.8(2) . . ? C20 C1 C2 127.9(2) . . ? C3 C2 C1 107.3(2) . . ? C3 C2 C21 124.8(3) . . ? C1 C2 C21 127.6(3) . . ? C2 C3 C4 106.9(2) . . ? C2 C3 C22 125.2(3) . . ? C4 C3 C22 127.4(3) . . ? C5 C4 N1 122.5(2) . . ? C5 C4 C3 128.2(2) . . ? N1 C4 C3 109.2(2) . . ? C4 C5 C6 121.9(2) . . ? C4 C5 C29 117.2(2) . . ? C6 C5 C29 120.9(2) . . ? N2 C6 C5 121.0(2) . . ? N2 C6 C7 110.5(2) . . ? C5 C6 C7 127.9(2) . . ? C8 C7 C6 106.5(2) . . ? C8 C7 C23 125.1(2) . . ? C6 C7 C23 128.4(2) . . ? C7 C8 C9 106.7(2) . . ? C7 C8 C24 125.5(2) . . ? C9 C8 C24 127.6(2) . . ? N2 C9 C10 121.2(2) . . ? N2 C9 C8 110.5(2) . . ? C10 C9 C8 127.9(2) . . ? C11 C10 C9 121.6(2) . . ? C11 C10 C37 119.1(2) . . ? C9 C10 C37 119.3(2) . . ? C10 C11 N3 121.8(2) . . ? C10 C11 C12 128.9(2) . . ? N3 C11 C12 108.9(2) . . ? C13 C12 C11 107.2(2) . . ? C13 C12 C25 125.9(2) . . ? C11 C12 C25 126.8(3) . . ? C12 C13 C14 107.6(2) . . ? C12 C13 C26 125.0(2) . . ? C14 C13 C26 126.9(2) . . ? N3 C14 C15 122.6(2) . . ? N3 C14 C13 109.6(2) . . ? C15 C14 C13 127.7(2) . . ? C14 C15 C16 121.4(2) . . ? C14 C15 C45 119.8(2) . . ? C16 C15 C45 118.7(2) . . ? N4 C16 C15 121.4(2) . . ? N4 C16 C17 109.7(2) . . ? C15 C16 C17 128.2(2) . . ? C18 C17 C16 107.0(2) . . ? C18 C17 C27 125.5(2) . . ? C16 C17 C27 127.4(2) . . ? C17 C18 C19 107.2(2) . . ? C17 C18 C28 124.9(2) . . ? C19 C18 C28 127.9(2) . . ? N4 C19 C20 122.2(2) . . ? N4 C19 C18 109.4(2) . . ? C20 C19 C18 128.2(2) . . ? C19 C20 C1 122.3(2) . . ? C19 C20 C53 119.0(2) . . ? C1 C20 C53 118.7(2) . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C3 C22 H22A 109.5 . . ? C3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C7 C23 H23A 109.5 . . ? C7 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C7 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C24 H24A 109.5 . . ? C8 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C8 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C12 C25 H25A 109.5 . . ? C12 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C12 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C13 C26 H26A 109.5 . . ? C13 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C13 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C17 C27 H27A 109.5 . . ? C17 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C17 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 119.3(2) . . ? C34 C29 C5 121.3(2) . . ? C30 C29 C5 119.2(2) . . ? C31 C30 C29 120.9(2) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 119.0(2) . . ? C30 C31 C35 119.9(3) . . ? C32 C31 C35 121.0(3) . . ? C31 C32 C33 121.6(3) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C34 C33 C32 118.5(3) . . ? C34 C33 C36 120.5(3) . . ? C32 C33 C36 121.1(3) . . ? C29 C34 C33 120.6(2) . . ? C29 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C42 C37 C38 119.6(2) . . ? C42 C37 C10 120.3(2) . . ? C38 C37 C10 120.0(2) . . ? C37 C38 C39 120.0(3) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 119.0(3) . . ? C40 C39 C43 120.4(3) . . ? C38 C39 C43 120.6(3) . . ? C41 C40 C39 121.6(3) . . ? C41 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? C40 C41 C42 118.9(3) . . ? C40 C41 C44 122.8(3) . . ? C42 C41 C44 118.3(3) . . ? C37 C42 C41 120.9(3) . . ? C37 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C39 C43 H43A 109.5 . . ? C39 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C39 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 121.0(3) . . ? C46 C45 C15 119.6(2) . . ? C50 C45 C15 119.4(3) . . ? C45 C46 C47 120.0(3) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C48 C47 C46 118.5(3) . . ? C48 C47 C51 121.2(3) . . ? C46 C47 C51 120.2(3) . . ? C47 C48 C49 122.5(3) . . ? C47 C48 H48 118.7 . . ? C49 C48 H48 118.7 . . ? C48 C49 C50 118.0(3) . . ? C48 C49 C52 121.4(3) . . ? C50 C49 C52 120.6(3) . . ? C45 C50 C49 119.9(3) . . ? C45 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C47 C51 H51A 109.5 . . ? C47 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C47 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C58 120.0(2) . . ? C54 C53 C20 120.8(2) . . ? C58 C53 C20 119.1(2) . . ? C55 C54 C53 120.7(2) . . ? C55 C54 H54 119.7 . . ? C53 C54 H54 119.7 . . ? C54 C55 C56 117.9(3) . . ? C54 C55 C59 121.3(3) . . ? C56 C55 C59 120.8(3) . . ? C57 C56 C55 122.7(3) . . ? C57 C56 H56 118.7 . . ? C55 C56 H56 118.7 . . ? C56 C57 C58 118.1(2) . . ? C56 C57 C60 121.6(3) . . ? C58 C57 C60 120.3(3) . . ? C57 C58 C53 120.5(3) . . ? C57 C58 H58 119.8 . . ? C53 C58 H58 119.8 . . ? C55 C59 H59A 109.5 . . ? C55 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C55 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 N1 C1 169.19(19) . . . . ? N4 Fe1 N1 C1 -31.37(19) . . . . ? O1 Fe1 N1 C1 68.93(19) . . . . ? N2 Fe1 N1 C4 26.0(2) . . . . ? N4 Fe1 N1 C4 -174.6(2) . . . . ? O1 Fe1 N1 C4 -74.3(2) . . . . ? N1 Fe1 N2 C9 170.68(19) . . . . ? N3 Fe1 N2 C9 -2.83(19) . . . . ? N4 Fe1 N2 C9 83.7(3) . . . . ? O1 Fe1 N2 C9 -95.12(19) . . . . ? N1 Fe1 N2 C6 9.06(19) . . . . ? N3 Fe1 N2 C6 -164.44(19) . . . . ? N4 Fe1 N2 C6 -77.9(3) . . . . ? O1 Fe1 N2 C6 103.26(19) . . . . ? N2 Fe1 N3 C14 -172.01(18) . . . . ? N4 Fe1 N3 C14 28.55(18) . . . . ? O1 Fe1 N3 C14 -71.70(19) . . . . ? N2 Fe1 N3 C11 -33.82(18) . . . . ? N4 Fe1 N3 C11 166.74(18) . . . . ? O1 Fe1 N3 C11 66.49(19) . . . . ? N1 Fe1 N4 C16 -166.34(19) . . . . ? N3 Fe1 N4 C16 7.22(19) . . . . ? N2 Fe1 N4 C16 -79.5(3) . . . . ? O1 Fe1 N4 C16 99.31(19) . . . . ? N1 Fe1 N4 C19 -2.22(19) . . . . ? N3 Fe1 N4 C19 171.34(19) . . . . ? N2 Fe1 N4 C19 84.6(3) . . . . ? O1 Fe1 N4 C19 -96.57(19) . . . . ? C4 N1 C1 C20 -165.4(2) . . . . ? Fe1 N1 C1 C20 46.1(3) . . . . ? C4 N1 C1 C2 8.3(2) . . . . ? Fe1 N1 C1 C2 -140.15(17) . . . . ? N1 C1 C2 C3 -5.6(3) . . . . ? C20 C1 C2 C3 167.7(2) . . . . ? N1 C1 C2 C21 168.4(2) . . . . ? C20 C1 C2 C21 -18.3(4) . . . . ? C1 C2 C3 C4 0.5(3) . . . . ? C21 C2 C3 C4 -173.7(2) . . . . ? C1 C2 C3 C22 173.4(2) . . . . ? C21 C2 C3 C22 -0.8(4) . . . . ? C1 N1 C4 C5 166.9(2) . . . . ? Fe1 N1 C4 C5 -45.0(3) . . . . ? C1 N1 C4 C3 -8.0(2) . . . . ? Fe1 N1 C4 C3 140.15(17) . . . . ? C2 C3 C4 C5 -169.8(2) . . . . ? C22 C3 C4 C5 17.5(4) . . . . ? C2 C3 C4 N1 4.6(3) . . . . ? C22 C3 C4 N1 -168.0(2) . . . . ? N1 C4 C5 C6 21.5(3) . . . . ? C3 C4 C5 C6 -164.7(2) . . . . ? N1 C4 C5 C29 -159.6(2) . . . . ? C3 C4 C5 C29 14.1(3) . . . . ? C9 N2 C6 C5 164.7(2) . . . . ? Fe1 N2 C6 C5 -30.7(3) . . . . ? C9 N2 C6 C7 -7.7(2) . . . . ? Fe1 N2 C6 C7 156.93(16) . . . . ? C4 C5 C6 N2 17.1(3) . . . . ? C29 C5 C6 N2 -161.7(2) . . . . ? C4 C5 C6 C7 -171.9(2) . . . . ? C29 C5 C6 C7 9.2(3) . . . . ? N2 C6 C7 C8 4.6(3) . . . . ? C5 C6 C7 C8 -167.1(2) . . . . ? N2 C6 C7 C23 -172.7(2) . . . . ? C5 C6 C7 C23 15.6(4) . . . . ? C6 C7 C8 C9 0.4(3) . . . . ? C23 C7 C8 C9 177.8(2) . . . . ? C6 C7 C8 C24 -175.1(2) . . . . ? C23 C7 C8 C24 2.3(4) . . . . ? C6 N2 C9 C10 -165.1(2) . . . . ? Fe1 N2 C9 C10 30.1(3) . . . . ? C6 N2 C9 C8 7.9(2) . . . . ? Fe1 N2 C9 C8 -156.93(16) . . . . ? C7 C8 C9 N2 -5.3(3) . . . . ? C24 C8 C9 N2 170.0(2) . . . . ? C7 C8 C9 C10 167.1(2) . . . . ? C24 C8 C9 C10 -17.5(4) . . . . ? N2 C9 C10 C11 -22.7(4) . . . . ? C8 C9 C10 C11 165.5(2) . . . . ? N2 C9 C10 C37 157.1(2) . . . . ? C8 C9 C10 C37 -14.6(4) . . . . ? C9 C10 C11 N3 -19.0(4) . . . . ? C37 C10 C11 N3 161.1(2) . . . . ? C9 C10 C11 C12 169.3(3) . . . . ? C37 C10 C11 C12 -10.6(4) . . . . ? C14 N3 C11 C10 -166.1(2) . . . . ? Fe1 N3 C11 C10 49.8(3) . . . . ? C14 N3 C11 C12 7.1(3) . . . . ? Fe1 N3 C11 C12 -136.98(19) . . . . ? C10 C11 C12 C13 167.6(3) . . . . ? N3 C11 C12 C13 -5.0(3) . . . . ? C10 C11 C12 C25 -16.6(5) . . . . ? N3 C11 C12 C25 170.8(3) . . . . ? C11 C12 C13 C14 0.8(3) . . . . ? C25 C12 C13 C14 -174.9(3) . . . . ? C11 C12 C13 C26 174.0(3) . . . . ? C25 C12 C13 C26 -1.8(5) . . . . ? C11 N3 C14 C15 169.4(2) . . . . ? Fe1 N3 C14 C15 -47.6(3) . . . . ? C11 N3 C14 C13 -6.6(3) . . . . ? Fe1 N3 C14 C13 136.43(19) . . . . ? C12 C13 C14 N3 3.6(3) . . . . ? C26 C13 C14 N3 -169.4(3) . . . . ? C12 C13 C14 C15 -172.1(3) . . . . ? C26 C13 C14 C15 14.9(5) . . . . ? N3 C14 C15 C16 22.3(4) . . . . ? C13 C14 C15 C16 -162.5(3) . . . . ? N3 C14 C15 C45 -160.6(2) . . . . ? C13 C14 C15 C45 14.6(4) . . . . ? C19 N4 C16 C15 163.5(2) . . . . ? Fe1 N4 C16 C15 -30.0(3) . . . . ? C19 N4 C16 C17 -7.6(3) . . . . ? Fe1 N4 C16 C17 159.01(16) . . . . ? C14 C15 C16 N4 17.6(4) . . . . ? C45 C15 C16 N4 -159.5(2) . . . . ? C14 C15 C16 C17 -173.1(2) . . . . ? C45 C15 C16 C17 9.8(4) . . . . ? N4 C16 C17 C18 4.9(3) . . . . ? C15 C16 C17 C18 -165.4(2) . . . . ? N4 C16 C17 C27 -170.8(2) . . . . ? C15 C16 C17 C27 18.9(4) . . . . ? C16 C17 C18 C19 -0.2(3) . . . . ? C27 C17 C18 C19 175.6(2) . . . . ? C16 C17 C18 C28 -177.0(2) . . . . ? C27 C17 C18 C28 -1.2(4) . . . . ? C16 N4 C19 C20 -166.9(2) . . . . ? Fe1 N4 C19 C20 26.3(3) . . . . ? C16 N4 C19 C18 7.4(2) . . . . ? Fe1 N4 C19 C18 -159.35(16) . . . . ? C17 C18 C19 N4 -4.5(3) . . . . ? C28 C18 C19 N4 172.2(2) . . . . ? C17 C18 C19 C20 169.4(2) . . . . ? C28 C18 C19 C20 -13.9(4) . . . . ? N4 C19 C20 C1 -19.6(4) . . . . ? C18 C19 C20 C1 167.2(2) . . . . ? N4 C19 C20 C53 161.6(2) . . . . ? C18 C19 C20 C53 -11.6(4) . . . . ? N1 C1 C20 C19 -18.0(3) . . . . ? C2 C1 C20 C19 169.4(2) . . . . ? N1 C1 C20 C53 160.7(2) . . . . ? C2 C1 C20 C53 -11.8(4) . . . . ? C4 C5 C29 C34 -117.1(3) . . . . ? C6 C5 C29 C34 61.8(3) . . . . ? C4 C5 C29 C30 58.3(3) . . . . ? C6 C5 C29 C30 -122.8(3) . . . . ? C34 C29 C30 C31 0.9(4) . . . . ? C5 C29 C30 C31 -174.6(3) . . . . ? C29 C30 C31 C32 -0.5(5) . . . . ? C29 C30 C31 C35 176.8(3) . . . . ? C30 C31 C32 C33 0.2(5) . . . . ? C35 C31 C32 C33 -177.1(3) . . . . ? C31 C32 C33 C34 -0.3(5) . . . . ? C31 C32 C33 C36 179.5(3) . . . . ? C30 C29 C34 C33 -1.0(4) . . . . ? C5 C29 C34 C33 174.4(3) . . . . ? C32 C33 C34 C29 0.7(5) . . . . ? C36 C33 C34 C29 -179.1(3) . . . . ? C11 C10 C37 C42 -59.7(3) . . . . ? C9 C10 C37 C42 120.4(3) . . . . ? C11 C10 C37 C38 116.3(3) . . . . ? C9 C10 C37 C38 -63.6(3) . . . . ? C42 C37 C38 C39 0.3(4) . . . . ? C10 C37 C38 C39 -175.8(3) . . . . ? C37 C38 C39 C40 0.3(4) . . . . ? C37 C38 C39 C43 178.6(3) . . . . ? C38 C39 C40 C41 -0.1(4) . . . . ? C43 C39 C40 C41 -178.4(3) . . . . ? C39 C40 C41 C42 -0.8(4) . . . . ? C39 C40 C41 C44 177.5(3) . . . . ? C38 C37 C42 C41 -1.1(4) . . . . ? C10 C37 C42 C41 174.9(2) . . . . ? C40 C41 C42 C37 1.4(4) . . . . ? C44 C41 C42 C37 -176.9(3) . . . . ? C14 C15 C45 C46 -114.8(3) . . . . ? C16 C15 C45 C46 62.4(3) . . . . ? C14 C15 C45 C50 63.7(3) . . . . ? C16 C15 C45 C50 -119.1(3) . . . . ? C50 C45 C46 C47 -1.0(4) . . . . ? C15 C45 C46 C47 177.4(3) . . . . ? C45 C46 C47 C48 1.4(5) . . . . ? C45 C46 C47 C51 -179.6(3) . . . . ? C46 C47 C48 C49 -0.5(5) . . . . ? C51 C47 C48 C49 -179.5(3) . . . . ? C47 C48 C49 C50 -0.8(5) . . . . ? C47 C48 C49 C52 179.0(3) . . . . ? C46 C45 C50 C49 -0.3(4) . . . . ? C15 C45 C50 C49 -178.8(2) . . . . ? C48 C49 C50 C45 1.2(4) . . . . ? C52 C49 C50 C45 -178.6(3) . . . . ? C19 C20 C53 C54 -74.0(3) . . . . ? C1 C20 C53 C54 107.2(3) . . . . ? C19 C20 C53 C58 108.3(3) . . . . ? C1 C20 C53 C58 -70.5(3) . . . . ? C58 C53 C54 C55 2.9(4) . . . . ? C20 C53 C54 C55 -174.7(3) . . . . ? C53 C54 C55 C56 -2.1(4) . . . . ? C53 C54 C55 C59 179.6(3) . . . . ? C54 C55 C56 C57 -1.7(5) . . . . ? C59 C55 C56 C57 176.6(3) . . . . ? C55 C56 C57 C58 4.7(5) . . . . ? C55 C56 C57 C60 -175.0(3) . . . . ? C56 C57 C58 C53 -3.8(4) . . . . ? C60 C57 C58 C53 175.8(3) . . . . ? C54 C53 C58 C57 0.1(4) . . . . ? C20 C53 C58 C57 177.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 32.09 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.217 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.117 data_[Fe(OMTDTBPP)(H2O)]ClO4 _database_code_depnum_ccdc_archive 'CCDC 297041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,3,7,8,12,13,17,18-octamethyl-5,10,15,20-tetrakis (3,5-di-tert-butylphenyl)porphyrinato-\/Yk^4^N]iron(III) perchlorate dichloromethane solvate ; _chemical_name_common ; 2,3,7,8,12,13,17,18-octamethyl-5,10,15,20-tetrakis (3,5-di- tert-butylphenyl)porphyrinato-\/Yk$4!N)iron(iii) perchlorate dichloromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C84 H110 Fe N4 O, Cl O4, C H2 Cl2' _chemical_formula_sum 'C85 H112 Cl3 Fe N4 O5' _chemical_formula_weight 1431.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' O O 0.0106 0.0060 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.160(4) _cell_length_b 15.846(4) _cell_length_c 18.698(5) _cell_angle_alpha 68.533(7) _cell_angle_beta 79.192(9) _cell_angle_gamma 83.227(9) _cell_volume 4100(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 34022 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.3 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1426.0 _exptl_absorpt_coefficient_mu 0.331 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.934 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_process_details ; ABSCOR(Higashi et al., 1968) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 58762 _diffrn_reflns_av_R_equivalents 0.1618 _diffrn_reflns_av_sigmaI/netI 0.1223 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.40 _reflns_number_total 17675 _reflns_number_gt 7444 _reflns_threshold_expression 2\s(I) _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992a) ; _computing_cell_refinement ; MSC/AFC Diffractometer Control Software ; _computing_data_reduction ; MSC/AFC Diffractometer Control Software. Data Reduction: TEXSAN (Molecular Structure Corporation, 1992b) ; _computing_structure_solution 'SIR-97(Altomare, A. et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SV (Nemoto & Ohashi, 1993)' _computing_publication_material SHELXL-97 _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^)+(0.2000P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.018(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 17675 _refine_ls_number_parameters 1249 _refine_ls_number_restraints 190 _refine_ls_R_factor_all 0.2164 _refine_ls_R_factor_gt 0.1312 _refine_ls_wR_factor_ref 0.3835 _refine_ls_wR_factor_gt 0.3254 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.039 _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 0.47296(4) 0.26714(5) 0.45496(4) 0.0824(3) Uani 1 1 d . . . Cl1 Cl 0.3330(4) 0.7473(4) 0.3214(3) 0.294(2) Uani 1 1 d . . . Cl2 Cl 0.5093(3) 0.8092(4) 0.2483(4) 0.303(3) Uani 1 1 d . . . O1 O 0.5105(3) 0.3638(3) 0.4933(2) 0.1092(12) Uani 1 1 d . . . H1 H 0.4660 0.3954 0.5024 0.164 Uiso 1 1 calc R . . H01A H 0.5491 0.4143 0.4587 0.164 Uiso 1 1 d . . . N1 N 0.4506(3) 0.1640(3) 0.5521(2) 0.0837(11) Uani 1 1 d . . . N2 N 0.3456(3) 0.3018(3) 0.4666(2) 0.0883(11) Uani 1 1 d . . . N3 N 0.4827(2) 0.3328(3) 0.3434(2) 0.0793(10) Uani 1 1 d . . . N4 N 0.5954(2) 0.2163(3) 0.4369(2) 0.0794(10) Uani 1 1 d . . . C1 C 0.5092(3) 0.0878(3) 0.5772(3) 0.0821(13) Uani 1 1 d . . . C2 C 0.4605(4) 0.0100(4) 0.6251(3) 0.0867(14) Uani 1 1 d . . . C3 C 0.3712(4) 0.0391(4) 0.6352(3) 0.0906(14) Uani 1 1 d . . . C4 C 0.3664(3) 0.1353(4) 0.5939(3) 0.0894(14) Uani 1 1 d . . . C5 C 0.2955(3) 0.1980(4) 0.5971(3) 0.0915(15) Uani 1 1 d . . . C6 C 0.2924(3) 0.2850(4) 0.5393(3) 0.0932(15) Uani 1 1 d . . . C7 C 0.2338(4) 0.3619(4) 0.5395(3) 0.1014(17) Uani 1 1 d . . . C8 C 0.2459(4) 0.4246(4) 0.4665(4) 0.1056(18) Uani 1 1 d . . . C9 C 0.3124(3) 0.3855(4) 0.4207(3) 0.0904(14) Uani 1 1 d . . . C10 C 0.3358(4) 0.4145(4) 0.3384(3) 0.0957(16) Uani 1 1 d . . . C11 C 0.4098(3) 0.3731(4) 0.3041(3) 0.0851(13) Uani 1 1 d . . . C12 C 0.4308(3) 0.3763(4) 0.2247(3) 0.0899(14) Uani 1 1 d . . . C13 C 0.5176(3) 0.3441(4) 0.2141(3) 0.0912(15) Uani 1 1 d . . . C14 C 0.5493(3) 0.3228(3) 0.2870(3) 0.0803(12) Uani 1 1 d . . . C15 C 0.6398(3) 0.3056(3) 0.3002(3) 0.0852(13) Uani 1 1 d . . . C16 C 0.6597(3) 0.2657(3) 0.3756(3) 0.0824(13) Uani 1 1 d . . . C17 C 0.7436(3) 0.2563(4) 0.4021(3) 0.0885(14) Uani 1 1 d . . . C18 C 0.7325(3) 0.1950(4) 0.4778(3) 0.0905(14) Uani 1 1 d . . . C19 C 0.6412(3) 0.1677(3) 0.4976(3) 0.0781(12) Uani 1 1 d . . . C20 C 0.6020(3) 0.0961(3) 0.5616(3) 0.0809(13) Uani 1 1 d . . . C21 C 0.4947(4) -0.0877(4) 0.6534(4) 0.1059(17) Uani 1 1 d . . . H21A H 0.4991 -0.1068 0.7076 0.159 Uiso 1 1 calc R . . H21B H 0.5529 -0.0940 0.6245 0.159 Uiso 1 1 calc R . . H21C H 0.4538 -0.1247 0.6461 0.159 Uiso 1 1 calc R . . C22 C 0.2944(4) -0.0223(4) 0.6769(4) 0.120(2) Uani 1 1 d . . . H22A H 0.3066 -0.0782 0.6672 0.180 Uiso 1 1 calc R . . H22B H 0.2398 0.0070 0.6584 0.180 Uiso 1 1 calc R . . H22C H 0.2880 -0.0346 0.7318 0.180 Uiso 1 1 calc R . . C23 C 0.1744(5) 0.3780(5) 0.6083(4) 0.134(2) Uani 1 1 d . . . H23A H 0.1807 0.4385 0.6061 0.201 Uiso 1 1 calc R . . H23B H 0.1918 0.3350 0.6556 0.201 Uiso 1 1 calc R . . H23C H 0.1128 0.3707 0.6068 0.201 Uiso 1 1 calc R . . C24 C 0.2077(5) 0.5217(4) 0.4413(4) 0.133(2) Uani 1 1 d . . . H24A H 0.1475 0.5236 0.4313 0.199 Uiso 1 1 calc R . . H24B H 0.2444 0.5577 0.3948 0.199 Uiso 1 1 calc R . . H24C H 0.2070 0.5456 0.4818 0.199 Uiso 1 1 calc R . . C25 C 0.3667(4) 0.3973(5) 0.1674(4) 0.1097(18) Uani 1 1 d . . . H25A H 0.3690 0.4601 0.1346 0.165 Uiso 1 1 calc R . . H25B H 0.3068 0.3852 0.1949 0.165 Uiso 1 1 calc R . . H25C H 0.3835 0.3599 0.1360 0.165 Uiso 1 1 calc R . . C26 C 0.5637(4) 0.3273(5) 0.1421(3) 0.1077(18) Uani 1 1 d . . . H26A H 0.5201 0.3130 0.1177 0.162 Uiso 1 1 calc R . . H26B H 0.6074 0.2773 0.1557 0.162 Uiso 1 1 calc R . . H26C H 0.5933 0.3806 0.1068 0.162 Uiso 1 1 calc R . . C27 C 0.8246(4) 0.3087(4) 0.3618(4) 0.1094(18) Uani 1 1 d . . . H27A H 0.8499 0.3242 0.3985 0.164 Uiso 1 1 calc R . . H27B H 0.8081 0.3633 0.3215 0.164 Uiso 1 1 calc R . . H27C H 0.8682 0.2727 0.3394 0.164 Uiso 1 1 calc R . . C28 C 0.8028(4) 0.1715(5) 0.5305(4) 0.1103(19) Uani 1 1 d . . . H28A H 0.8438 0.1243 0.5212 0.165 Uiso 1 1 calc R . . H28B H 0.7741 0.1510 0.5838 0.165 Uiso 1 1 calc R . . H28C H 0.8352 0.2244 0.5200 0.165 Uiso 1 1 calc R . . C29 C 0.2225(4) 0.1726(4) 0.6656(3) 0.0922(15) Uani 1 1 d . . . C30 C 0.2443(4) 0.1475(4) 0.7407(3) 0.0949(15) Uani 1 1 d . . . H30 H 0.3037 0.1491 0.7463 0.114 Uiso 1 1 calc R . . C31 C 0.1807(4) 0.1209(4) 0.8058(3) 0.0972(16) Uani 1 1 d . A . C32 C 0.0926(4) 0.1212(4) 0.7952(4) 0.1047(17) Uani 1 1 d . . . H32 H 0.0486 0.1042 0.8390 0.126 Uiso 1 1 calc R . . C33 C 0.0669(4) 0.1454(4) 0.7233(4) 0.0994(16) Uani 1 1 d . . . C34 C 0.1335(4) 0.1716(4) 0.6580(3) 0.1020(17) Uani 1 1 d . . . H34 H 0.1178 0.1886 0.6087 0.122 Uiso 1 1 calc R . . C35 C 0.2828(3) 0.4880(4) 0.2848(3) 0.0901(15) Uani 1 1 d . . . C36 C 0.1934(3) 0.4825(4) 0.2860(3) 0.0993(17) Uani 1 1 d . . . H36 H 0.1635 0.4334 0.3234 0.119 Uiso 1 1 calc R . . C37 C 0.1466(4) 0.5469(4) 0.2340(4) 0.1020(17) Uani 1 1 d . . . C38 C 0.1929(4) 0.6174(4) 0.1762(4) 0.1064(18) Uani 1 1 d . . . H38 H 0.1623 0.6600 0.1386 0.128 Uiso 1 1 calc R . . C39 C 0.2834(4) 0.6260(4) 0.1730(3) 0.1008(17) Uani 1 1 d . B . C40 C 0.3279(4) 0.5602(4) 0.2286(3) 0.0984(16) Uani 1 1 d . . . H40 H 0.3886 0.5647 0.2281 0.118 Uiso 1 1 calc R . . C41 C 0.7119(3) 0.3350(4) 0.2315(3) 0.0852(13) Uani 1 1 d . . . C42 C 0.7087(3) 0.4260(4) 0.1824(3) 0.0935(15) Uani 1 1 d . . . H42 H 0.6657 0.4668 0.1959 0.112 Uiso 1 1 calc R . . C43 C 0.7688(3) 0.4561(4) 0.1138(3) 0.0905(14) Uani 1 1 d . C . C44 C 0.8352(4) 0.3937(4) 0.0987(3) 0.0943(15) Uani 1 1 d . . . H44 H 0.8779 0.4134 0.0542 0.113 Uiso 1 1 calc R . . C45 C 0.8406(3) 0.3035(4) 0.1470(3) 0.0951(15) Uani 1 1 d . D . C46 C 0.7777(3) 0.2761(4) 0.2144(3) 0.0875(14) Uani 1 1 d . . . H46 H 0.7808 0.2163 0.2485 0.105 Uiso 1 1 calc R . . C47 C 0.6586(3) 0.0269(3) 0.6141(3) 0.0850(13) Uani 1 1 d . . . C48 C 0.7269(4) -0.0229(4) 0.5869(3) 0.0937(15) Uani 1 1 d . . . H48 H 0.7401 -0.0112 0.5336 0.112 Uiso 1 1 calc R . . C49 C 0.7773(4) -0.0906(4) 0.6361(4) 0.0999(16) Uani 1 1 d . E . C50 C 0.7557(4) -0.1038(4) 0.7139(4) 0.1026(17) Uani 1 1 d . . . H50 H 0.7907 -0.1468 0.7474 0.123 Uiso 1 1 calc R . . C51 C 0.6867(4) -0.0589(4) 0.7460(3) 0.0988(16) Uani 1 1 d . F . C52 C 0.6376(4) 0.0098(4) 0.6937(3) 0.0918(14) Uani 1 1 d . . . H52 H 0.5911 0.0436 0.7126 0.110 Uiso 1 1 calc R . . C53 C 0.2045(5) 0.0952(5) 0.8884(3) 0.122(2) Uani 1 1 d D . . C54A C 0.264(2) 0.1680(15) 0.8838(14) 0.23(3) Uani 0.35 1 d PD A 1 C55A C 0.2575(18) 0.0045(12) 0.9035(17) 0.150 Uiso 0.35 1 d PD A 1 C56A C 0.1220(11) 0.088(2) 0.9494(11) 0.30(4) Uani 0.35 1 d PD A 1 C54B C 0.3026(9) 0.103(2) 0.8926(14) 0.21(2) Uani 0.35 1 d PD A 2 C55B C 0.1761(19) -0.0003(10) 0.9402(14) 0.150 Uiso 0.35 1 d PD A 2 C56B C 0.1458(18) 0.1638(17) 0.9194(19) 0.194(17) Uani 0.35 1 d PD A 2 C54C C 0.2895(12) 0.0327(16) 0.893(2) 0.150 Uiso 0.30 1 d PD A 3 C55C C 0.1295(16) 0.0468(19) 0.9515(17) 0.144(12) Uani 0.30 1 d PD A 3 C56C C 0.222(2) 0.1828(14) 0.896(2) 0.150 Uiso 0.30 1 d PD A 3 C57 C -0.0303(4) 0.1461(6) 0.7104(4) 0.118(2) Uani 1 1 d . . . C58 C -0.0958(5) 0.1307(9) 0.7911(6) 0.183(4) Uani 1 1 d . . . H58A H -0.1563 0.1268 0.7844 0.275 Uiso 1 1 calc R . . H58B H -0.0933 0.1807 0.8079 0.275 Uiso 1 1 calc R . . H58C H -0.0773 0.0753 0.8295 0.275 Uiso 1 1 calc R . . C59 C -0.0603(5) 0.2372(6) 0.6548(6) 0.160(3) Uani 1 1 d . . . H59A H -0.0194 0.2525 0.6066 0.240 Uiso 1 1 calc R . . H59B H -0.0608 0.2829 0.6773 0.240 Uiso 1 1 calc R . . H59C H -0.1197 0.2339 0.6453 0.240 Uiso 1 1 calc R . . C60 C -0.0384(5) 0.0680(6) 0.6836(5) 0.148(3) Uani 1 1 d . . . H60A H -0.0987 0.0687 0.6743 0.222 Uiso 1 1 calc R . . H60B H -0.0245 0.0116 0.7232 0.222 Uiso 1 1 calc R . . H60C H 0.0029 0.0745 0.6365 0.222 Uiso 1 1 calc R . . C61 C 0.0461(4) 0.5358(5) 0.2339(4) 0.1103(19) Uani 1 1 d . . . C62 C -0.0005(4) 0.4821(6) 0.3176(6) 0.156(3) Uani 1 1 d . . . H62A H -0.0645 0.4919 0.3203 0.234 Uiso 1 1 calc R . . H62B H 0.0188 0.5028 0.3542 0.234 Uiso 1 1 calc R . . H62C H 0.0156 0.4185 0.3300 0.234 Uiso 1 1 calc R . . C63 C -0.0059(4) 0.6287(5) 0.2061(5) 0.129(2) Uani 1 1 d . . . H63A H 0.0229 0.6649 0.1555 0.193 Uiso 1 1 calc R . . H63B H -0.0063 0.6593 0.2420 0.193 Uiso 1 1 calc R . . H63C H -0.0666 0.6198 0.2034 0.193 Uiso 1 1 calc R . . C64 C 0.0402(6) 0.4841(8) 0.1822(7) 0.192(5) Uani 1 1 d . . . H64A H -0.0207 0.4684 0.1887 0.289 Uiso 1 1 calc R . . H64B H 0.0786 0.4298 0.1958 0.289 Uiso 1 1 calc R . . H64C H 0.0591 0.5211 0.1290 0.289 Uiso 1 1 calc R . . C65 C 0.3349(4) 0.7034(4) 0.1059(4) 0.121(2) Uani 1 1 d D . . C66A C 0.4264(14) 0.7143(19) 0.122(2) 0.54(8) Uani 0.39 1 d PD B 1 C67A C 0.2794(13) 0.7928(8) 0.0897(11) 0.126(8) Uani 0.39 1 d PD B 1 C68A C 0.344(3) 0.6710(18) 0.0381(12) 0.30(3) Uani 0.39 1 d PD B 1 C66B C 0.3583(18) 0.753(2) 0.1552(16) 0.20(2) Uani 0.30 1 d PD B 2 C67B C 0.2815(16) 0.766(2) 0.0447(11) 0.39(6) Uani 0.30 1 d PD B 2 C68B C 0.4187(11) 0.6630(15) 0.0704(11) 0.105(9) Uani 0.30 1 d PD B 2 C66C C 0.305(2) 0.7929(16) 0.117(2) 0.150 Uiso 0.31 1 d PD B 3 C67C C 0.3109(17) 0.707(2) 0.0291(10) 0.28(4) Uani 0.31 1 d PD B 3 C68C C 0.4345(8) 0.683(2) 0.1066(14) 0.152(15) Uani 0.31 1 d PD B 3 C69 C 0.7630(4) 0.5548(4) 0.0566(3) 0.1032(18) Uani 1 1 d D . . C70A C 0.746(2) 0.540(3) -0.0144(16) 0.150 Uiso 0.22 1 d PD C 1 C71A C 0.8543(13) 0.592(2) 0.0446(19) 0.17(2) Uani 0.22 1 d PD C 1 C72A C 0.6891(19) 0.614(2) 0.084(2) 0.120(15) Uani 0.22 1 d PD C 1 C70B C 0.7918(14) 0.5693(11) -0.0292(6) 0.117(6) Uani 0.44 1 d PD C 2 C71B C 0.823(2) 0.6049(14) 0.0821(12) 0.30(3) Uani 0.44 1 d PD C 2 C72B C 0.6653(11) 0.586(3) 0.0720(17) 0.34(5) Uani 0.44 1 d PD C 2 C70C C 0.8202(19) 0.556(2) -0.0202(9) 0.33(5) Uani 0.34 1 d PD C 3 C71C C 0.801(3) 0.618(3) 0.086(3) 0.25(3) Uiso 0.34 1 d PD C 3 C72C C 0.6663(8) 0.584(3) 0.0444(14) 0.140(12) Uani 0.34 1 d PD C 3 C73 C 0.9175(4) 0.2365(4) 0.1279(3) 0.1070(19) Uani 1 1 d D . . C74A C 0.985(3) 0.300(3) 0.069(4) 0.59(17) Uani 0.18 1 d PD D 1 C75A C 0.875(5) 0.183(4) 0.093(5) 0.39(10) Uiso 0.18 1 d PD D 1 C76A C 0.959(4) 0.176(4) 0.198(2) 0.15(2) Uiso 0.18 1 d PD D 1 C74B C 0.948(2) 0.2754(18) 0.0404(6) 0.151(14) Uani 0.40 1 d PD D 2 C75B C 0.8792(11) 0.1454(7) 0.1518(19) 0.169(14) Uani 0.40 1 d PD D 2 C76B C 0.9939(16) 0.2332(17) 0.1707(18) 0.141(11) Uani 0.40 1 d PD D 2 C74C C 0.922(2) 0.2363(14) 0.0459(6) 0.123(8) Uani 0.42 1 d PD D 3 C75C C 0.9134(12) 0.1383(7) 0.1853(10) 0.114(7) Uani 0.42 1 d PD D 3 C76C C 1.0035(12) 0.2747(14) 0.1330(13) 0.134(9) Uani 0.42 1 d PD D 3 C77 C 0.8557(4) -0.1444(4) 0.6040(4) 0.114(2) Uani 1 1 d D . . C78A C 0.8078(14) -0.2149(14) 0.5908(13) 0.150 Uiso 0.45 1 d PD E 1 C79A C 0.916(2) -0.190(2) 0.6652(17) 0.35(4) Uani 0.45 1 d PD E 1 C80A C 0.9102(14) -0.0860(11) 0.5287(11) 0.134(8) Uani 0.45 1 d PD E 1 C78B C 0.842(2) -0.2439(9) 0.6485(15) 0.205(18) Uani 0.32 1 d PD E 2 C79B C 0.9434(10) -0.119(2) 0.6184(16) 0.145(14) Uani 0.32 1 d PD E 2 C80B C 0.8604(17) -0.1216(16) 0.5170(7) 0.158(13) Uani 0.32 1 d PD E 2 C78C C 0.896(3) -0.2167(17) 0.6699(15) 0.123(14) Uani 0.23 1 d PD E 3 C79C C 0.921(2) -0.0712(19) 0.5576(16) 0.14(2) Uani 0.23 1 d PD E 3 C80C C 0.8267(17) -0.1865(18) 0.5517(13) 0.100 Uiso 0.23 1 d PD E 3 C81 C 0.6627(4) -0.0794(4) 0.8349(3) 0.1118(19) Uani 1 1 d D . . C82A C 0.7514(19) -0.105(4) 0.865(3) 0.15(2) Uiso 0.20 1 d PD F 1 C83A C 0.607(3) -0.161(2) 0.859(3) 0.150 Uiso 0.20 1 d PD F 1 C84A C 0.611(3) -0.004(3) 0.858(4) 0.17(3) Uiso 0.20 1 d PD F 1 C82B C 0.7334(16) -0.1481(16) 0.8753(14) 0.166(16) Uani 0.38 1 d PD F 2 C83B C 0.5712(11) -0.1177(18) 0.8614(16) 0.142(11) Uani 0.38 1 d PD F 2 C84B C 0.6643(18) 0.0094(9) 0.8465(10) 0.110(8) Uani 0.38 1 d PD F 2 C82C C 0.697(4) -0.1709(18) 0.8861(15) 0.24(3) Uani 0.42 1 d PD F 3 C83C C 0.5627(8) -0.076(5) 0.8569(13) 0.31(3) Uani 0.42 1 d PD F 3 C84C C 0.695(4) -0.015(2) 0.8652(17) 0.27(3) Uani 0.42 1 d PD F 3 C85 C 0.4499(11) 0.7308(12) 0.3320(11) 0.262(7) Uani 1 1 d . . . H85A H 0.4582 0.7412 0.3783 0.315 Uiso 1 1 calc R . . H85B H 0.4716 0.6692 0.3367 0.315 Uiso 1 1 calc R . . Cl3 Cl 0.6257(8) 0.5519(5) 0.3428(7) 0.128(4) Uani 0.28 1 d PD G 1 O2 O 0.6509(15) 0.6380(8) 0.3146(19) 0.29(3) Uani 0.28 1 d PD G 1 O3 O 0.6977(16) 0.4946(17) 0.3350(16) 0.38(4) Uani 0.28 1 d PD G 1 O4 O 0.5640(15) 0.543(2) 0.3027(15) 0.20(2) Uani 0.28 1 d PD G 1 O5 O 0.5896(17) 0.5282(18) 0.4189(9) 0.201(13) Uani 0.28 1 d PD G 1 Cl4 Cl 0.5749(8) 0.5796(8) 0.3315(5) 0.087(3) Uani 0.17 1 d PD H 2 O6 O 0.6387(16) 0.5151(16) 0.3611(16) 0.100 Uiso 0.17 1 d PD H 2 O7 O 0.5001(12) 0.5669(14) 0.3854(10) 0.100 Uiso 0.17 1 d PD H 2 O8 O 0.6070(16) 0.6619(12) 0.3133(14) 0.100 Uiso 0.17 1 d PD H 2 O9 O 0.556(2) 0.570(2) 0.2668(9) 0.14(2) Uani 0.17 1 d PD H 2 Cl5 Cl 0.6218(11) 0.5515(12) 0.3430(11) 0.46(2) Uani 0.55 1 d PD I 3 O10 O 0.6067(11) 0.6178(12) 0.3749(10) 0.241(10) Uani 0.55 1 d PD I 3 O11 O 0.6950(14) 0.5699(16) 0.2862(12) 0.260(11) Uani 0.55 1 d PD I 3 O12 O 0.5488(15) 0.547(2) 0.313(2) 0.46(4) Uani 0.55 1 d PD I 3 O13 O 0.637(2) 0.4701(11) 0.3993(14) 0.45(4) Uani 0.55 1 d PD I 3 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 0.0666(5) 0.0926(6) 0.0685(5) -0.0098(3) -0.0152(3) 0.0172(3) Cl1 0.256(5) 0.323(6) 0.321(6) -0.142(5) -0.025(4) -0.025(4) Cl2 0.209(4) 0.321(6) 0.404(8) -0.161(6) -0.056(5) 0.016(4) O1 0.117(3) 0.106(3) 0.094(3) -0.028(2) -0.018(2) 0.014(2) N1 0.058(2) 0.095(3) 0.079(3) -0.014(2) -0.0077(18) 0.0131(18) N2 0.081(3) 0.091(3) 0.069(3) -0.007(2) -0.016(2) 0.022(2) N3 0.057(2) 0.091(3) 0.069(2) -0.0091(18) -0.0119(17) 0.0181(17) N4 0.065(2) 0.086(3) 0.069(2) -0.0071(18) -0.0171(18) 0.0104(18) C1 0.077(3) 0.085(3) 0.066(3) -0.007(2) -0.020(2) 0.015(2) C2 0.085(3) 0.089(3) 0.069(3) -0.008(2) -0.021(2) 0.011(3) C3 0.080(3) 0.095(4) 0.075(3) -0.008(3) -0.012(2) 0.004(3) C4 0.066(3) 0.116(4) 0.071(3) -0.020(3) -0.014(2) 0.016(3) C5 0.068(3) 0.116(4) 0.068(3) -0.012(3) -0.010(2) 0.010(3) C6 0.073(3) 0.120(4) 0.064(3) -0.013(3) -0.010(2) 0.016(3) C7 0.081(3) 0.112(4) 0.080(4) -0.015(3) -0.003(3) 0.033(3) C8 0.085(4) 0.103(4) 0.101(4) -0.019(3) -0.010(3) 0.035(3) C9 0.072(3) 0.097(4) 0.079(3) -0.011(3) -0.010(2) 0.017(2) C10 0.074(3) 0.096(4) 0.088(4) -0.002(3) -0.016(3) 0.018(3) C11 0.072(3) 0.103(4) 0.062(3) -0.012(2) -0.012(2) 0.011(2) C12 0.075(3) 0.094(3) 0.084(4) -0.012(3) -0.021(3) 0.010(2) C13 0.074(3) 0.096(3) 0.077(3) -0.008(3) -0.008(2) 0.012(2) C14 0.065(3) 0.084(3) 0.075(3) -0.011(2) -0.015(2) 0.009(2) C15 0.068(3) 0.091(3) 0.074(3) -0.008(2) -0.011(2) 0.013(2) C16 0.065(3) 0.086(3) 0.071(3) -0.004(2) -0.011(2) 0.013(2) C17 0.064(3) 0.098(3) 0.084(3) -0.011(3) -0.017(2) 0.010(2) C18 0.072(3) 0.100(4) 0.084(4) -0.014(3) -0.024(2) 0.013(2) C19 0.064(3) 0.092(3) 0.068(3) -0.017(2) -0.018(2) 0.010(2) C20 0.074(3) 0.088(3) 0.060(3) -0.004(2) -0.019(2) 0.018(2) C21 0.098(4) 0.099(4) 0.103(4) -0.017(3) -0.023(3) 0.014(3) C22 0.099(4) 0.100(4) 0.126(5) -0.003(3) -0.007(4) -0.012(3) C23 0.115(5) 0.149(6) 0.105(5) -0.030(4) 0.003(4) 0.036(4) C24 0.136(6) 0.106(5) 0.122(5) -0.020(4) -0.015(4) 0.047(4) C25 0.093(4) 0.128(5) 0.096(4) -0.021(3) -0.041(3) 0.020(3) C26 0.092(4) 0.140(5) 0.085(4) -0.034(3) -0.019(3) 0.008(3) C27 0.071(3) 0.128(5) 0.103(4) -0.007(3) -0.017(3) -0.005(3) C28 0.076(3) 0.142(5) 0.092(4) -0.012(3) -0.035(3) 0.014(3) C29 0.075(3) 0.099(4) 0.080(3) -0.014(3) -0.004(3) 0.009(3) C30 0.078(3) 0.112(4) 0.075(3) -0.011(3) -0.024(3) 0.013(3) C31 0.092(4) 0.117(4) 0.063(3) -0.014(3) -0.009(3) 0.005(3) C32 0.083(4) 0.124(5) 0.081(4) -0.018(3) 0.005(3) 0.005(3) C33 0.074(3) 0.119(4) 0.090(4) -0.026(3) -0.006(3) 0.007(3) C34 0.078(3) 0.144(5) 0.070(3) -0.023(3) -0.019(3) 0.013(3) C35 0.065(3) 0.095(3) 0.080(3) -0.004(3) -0.009(2) 0.020(2) C36 0.066(3) 0.098(4) 0.096(4) 0.002(3) -0.007(3) 0.016(2) C37 0.076(3) 0.101(4) 0.108(4) -0.020(3) -0.019(3) 0.027(3) C38 0.080(4) 0.107(4) 0.095(4) -0.001(3) -0.018(3) 0.030(3) C39 0.088(4) 0.096(4) 0.083(4) -0.003(3) -0.007(3) 0.023(3) C40 0.067(3) 0.106(4) 0.092(4) -0.005(3) -0.016(3) 0.020(3) C41 0.072(3) 0.100(4) 0.065(3) -0.010(2) -0.012(2) 0.006(2) C42 0.074(3) 0.113(4) 0.076(3) -0.014(3) -0.022(3) 0.017(3) C43 0.070(3) 0.101(4) 0.073(3) 0.000(2) -0.012(2) 0.004(3) C44 0.079(3) 0.104(4) 0.080(3) -0.015(3) -0.008(3) 0.010(3) C45 0.070(3) 0.105(4) 0.087(4) -0.010(3) -0.014(3) 0.009(3) C46 0.064(3) 0.108(4) 0.074(3) -0.018(3) -0.010(2) 0.013(2) C47 0.072(3) 0.090(3) 0.071(3) -0.005(2) -0.014(2) 0.006(2) C48 0.078(3) 0.106(4) 0.081(3) -0.015(3) -0.024(3) 0.015(3) C49 0.088(4) 0.102(4) 0.093(4) -0.013(3) -0.032(3) 0.016(3) C50 0.106(4) 0.099(4) 0.086(4) -0.009(3) -0.038(3) 0.018(3) C51 0.101(4) 0.103(4) 0.075(3) -0.003(3) -0.032(3) -0.001(3) C52 0.083(3) 0.102(4) 0.071(3) -0.010(3) -0.018(2) 0.011(3) C53 0.135(6) 0.128(5) 0.082(4) -0.015(4) -0.025(4) 0.012(4) C54A 0.42(7) 0.22(3) 0.068(17) -0.004(17) -0.13(3) -0.11(4) C56A 0.15(3) 0.72(12) 0.032(14) -0.12(3) -0.023(16) -0.04(5) C54B 0.091(15) 0.40(6) 0.085(17) -0.02(3) -0.056(12) 0.01(2) C56B 0.15(3) 0.25(4) 0.25(4) -0.19(4) -0.03(2) 0.06(3) C55C 0.15(3) 0.17(2) 0.074(18) -0.005(14) 0.018(17) -0.037(18) C57 0.077(4) 0.155(6) 0.115(5) -0.045(5) -0.007(3) -0.003(4) C58 0.074(4) 0.311(13) 0.167(8) -0.094(9) 0.004(5) -0.019(6) C59 0.103(5) 0.163(7) 0.212(10) -0.051(7) -0.075(6) 0.030(5) C60 0.110(5) 0.156(7) 0.167(8) -0.039(6) -0.043(5) 0.008(5) C61 0.076(4) 0.117(4) 0.132(5) -0.041(4) -0.032(3) 0.035(3) C62 0.061(4) 0.162(7) 0.195(9) -0.014(6) -0.002(4) -0.001(4) C63 0.087(4) 0.133(5) 0.152(6) -0.032(5) -0.052(4) 0.041(4) C64 0.109(6) 0.249(11) 0.281(14) -0.167(11) -0.065(7) 0.048(6) C65 0.113(5) 0.105(5) 0.108(5) 0.001(4) -0.017(4) 0.015(4) C66A 0.21(4) 0.36(6) 0.69(12) 0.41(8) -0.29(6) -0.22(5) C67A 0.20(2) 0.052(7) 0.095(15) 0.013(7) -0.033(13) 0.003(10) C68A 0.55(9) 0.30(5) 0.064(18) -0.09(3) 0.08(3) -0.14(5) C66B 0.081(18) 0.18(3) 0.26(5) 0.03(3) -0.05(2) -0.031(19) C67B 0.22(4) 0.50(9) 0.09(2) 0.17(4) 0.08(3) 0.24(6) C68B 0.060(12) 0.128(19) 0.069(17) 0.025(13) -0.005(10) 0.018(12) C67C 0.17(3) 0.38(7) 0.16(3) 0.15(4) -0.12(3) -0.18(4) C68C 0.09(2) 0.26(4) 0.063(16) -0.010(19) 0.007(13) -0.06(2) C69 0.090(4) 0.102(4) 0.081(4) 0.005(3) -0.012(3) 0.013(3) C71A 0.10(2) 0.18(4) 0.13(3) 0.10(3) -0.09(2) -0.05(2) C72A 0.17(4) 0.071(17) 0.08(3) -0.010(18) 0.02(2) 0.01(2) C70B 0.176(17) 0.084(10) 0.079(10) -0.005(8) -0.067(11) 0.033(10) C71B 0.58(9) 0.044(9) 0.28(4) 0.040(14) -0.27(5) -0.09(2) C72B 0.17(3) 0.24(5) 0.31(6) 0.17(4) 0.09(3) 0.12(3) C70C 0.22(4) 0.26(5) 0.18(4) 0.19(4) 0.10(3) 0.18(4) C72C 0.14(2) 0.16(3) 0.064(13) 0.039(13) -0.039(13) -0.005(18) C73 0.089(4) 0.103(4) 0.101(4) -0.021(3) 0.008(3) 0.016(3) C74A 0.12(5) 0.19(8) 1.2(4) -0.21(16) 0.32(13) 0.01(5) C74B 0.18(3) 0.11(2) 0.123(18) -0.027(12) 0.023(16) 0.05(2) C75B 0.049(10) 0.114(15) 0.33(4) -0.09(2) 0.027(15) 0.026(9) C76B 0.131(19) 0.13(2) 0.18(3) -0.059(19) -0.10(2) 0.078(16) C74C 0.18(2) 0.101(17) 0.080(11) -0.036(9) -0.019(12) 0.039(15) C75C 0.064(11) 0.070(8) 0.158(15) 0.006(8) -0.002(10) 0.018(7) C76C 0.065(10) 0.128(19) 0.16(2) 0.003(13) -0.027(11) 0.033(10) C77 0.098(4) 0.133(5) 0.114(5) -0.048(4) -0.043(4) 0.044(4) C79A 0.24(6) 0.57(11) 0.23(6) -0.15(6) -0.16(5) 0.21(6) C80A 0.124(16) 0.106(13) 0.143(17) -0.048(12) 0.057(14) -0.005(10) C78B 0.20(4) 0.12(2) 0.22(4) -0.01(2) -0.01(3) 0.08(2) C79B 0.042(10) 0.27(4) 0.15(3) -0.12(3) 0.000(14) 0.019(15) C80B 0.115(19) 0.107(19) 0.29(4) -0.11(2) -0.05(2) 0.013(14) C78C 0.08(2) 0.14(3) 0.14(4) -0.05(2) -0.07(2) 0.08(2) C79C 0.10(2) 0.20(4) 0.19(4) -0.17(4) 0.04(3) -0.03(2) C81 0.124(5) 0.110(5) 0.078(4) -0.001(3) -0.029(3) -0.001(4) C82B 0.20(3) 0.19(4) 0.057(14) 0.028(16) -0.062(18) 0.01(2) C83B 0.123(19) 0.16(2) 0.12(2) -0.026(16) 0.026(16) -0.068(16) C84B 0.17(2) 0.117(15) 0.042(10) -0.024(9) -0.032(11) 0.012(13) C82C 0.47(7) 0.086(12) 0.076(15) 0.015(10) 0.04(2) 0.04(2) C83C 0.27(5) 0.56(8) 0.018(9) -0.03(2) 0.009(14) -0.01(5) C84C 0.55(7) 0.16(3) 0.104(19) 0.036(15) -0.16(3) -0.16(4) C85 0.210(16) 0.283(18) 0.269(19) -0.077(15) -0.016(13) -0.021(13) Cl3 0.145(9) 0.096(6) 0.155(10) -0.079(7) 0.041(8) -0.041(6) O2 0.114(18) 0.085(15) 0.54(8) 0.07(3) -0.08(3) 0.001(12) O3 0.51(8) 0.42(7) 0.29(5) -0.29(5) -0.19(5) 0.38(7) O4 0.18(4) 0.13(2) 0.23(4) -0.04(3) 0.07(4) -0.01(2) O5 0.21(3) 0.123(17) 0.23(3) -0.06(2) 0.06(2) -0.045(18) Cl4 0.095(7) 0.108(9) 0.056(5) -0.029(5) -0.014(5) 0.005(6) O9 0.11(3) 0.23(5) 0.033(13) -0.010(17) -0.005(13) 0.04(3) Cl5 0.57(5) 0.52(4) 0.36(3) -0.25(3) 0.14(3) -0.28(4) O10 0.29(2) 0.245(19) 0.190(15) -0.118(15) 0.106(14) -0.120(15) O11 0.24(2) 0.29(3) 0.24(2) -0.12(2) 0.055(18) -0.046(19) O12 0.30(4) 0.38(4) 0.97(11) -0.52(6) -0.27(5) 0.09(3) O13 0.62(6) 0.167(18) 0.43(5) -0.12(2) 0.34(5) -0.10(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 Fe1 N2 1.938(4) . ? Fe1 N3 1.946(4) . ? Fe1 N1 1.952(4) . ? Fe1 N4 1.954(4) . ? Fe1 O1 2.085(4) . ? Cl1 C85 1.798(16) . ? Cl2 C85 1.765(16) . ? O1 H1 0.8200 . ? O1 H01A 0.995 . ? N1 C4 1.397(6) . ? N1 C1 1.399(6) . ? N2 C9 1.386(6) . ? N2 C6 1.394(6) . ? N3 C14 1.358(6) . ? N3 C11 1.402(6) . ? N4 C19 1.377(6) . ? N4 C16 1.409(6) . ? C1 C20 1.394(7) . ? C1 C2 1.423(7) . ? C2 C3 1.379(7) . ? C2 C21 1.502(8) . ? C3 C4 1.434(7) . ? C3 C22 1.511(8) . ? C4 C5 1.383(7) . ? C5 C6 1.408(7) . ? C5 C29 1.492(7) . ? C6 C7 1.422(7) . ? C7 C8 1.356(8) . ? C7 C23 1.510(8) . ? C8 C9 1.433(7) . ? C8 C24 1.513(8) . ? C9 C10 1.422(7) . ? C10 C11 1.402(7) . ? C10 C35 1.495(7) . ? C11 C12 1.441(7) . ? C12 C13 1.359(7) . ? C12 C25 1.503(7) . ? C13 C14 1.440(7) . ? C13 C26 1.496(8) . ? C14 C15 1.417(7) . ? C15 C16 1.392(7) . ? C15 C41 1.489(7) . ? C16 C17 1.423(7) . ? C17 C18 1.385(7) . ? C17 C27 1.484(7) . ? C18 C19 1.438(7) . ? C18 C28 1.509(7) . ? C19 C20 1.404(6) . ? C20 C47 1.486(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.387(8) . ? C29 C30 1.404(8) . ? C30 C31 1.368(7) . ? C30 H30 0.9300 . ? C31 C32 1.385(8) . ? C31 C53 1.547(8) . ? C32 C33 1.376(8) . ? C32 H32 0.9300 . ? C33 C34 1.394(8) . ? C33 C57 1.537(9) . ? C34 H34 0.9300 . ? C35 C36 1.364(7) . ? C35 C40 1.383(7) . ? C36 C37 1.360(8) . ? C36 H36 0.9300 . ? C37 C38 1.388(8) . ? C37 C61 1.555(8) . ? C38 C39 1.383(8) . ? C38 H38 0.9300 . ? C39 C40 1.387(8) . ? C39 C65 1.556(8) . ? C40 H40 0.9300 . ? C41 C46 1.360(7) . ? C41 C42 1.398(7) . ? C42 C43 1.384(7) . ? C42 H42 0.9300 . ? C43 C44 1.391(7) . ? C43 C69 1.542(7) . ? C44 C45 1.385(7) . ? C44 H44 0.9300 . ? C45 C46 1.390(7) . ? C45 C73 1.563(7) . ? C46 H46 0.9300 . ? C47 C48 1.363(7) . ? C47 C52 1.392(7) . ? C48 C49 1.389(7) . ? C48 H48 0.9300 . ? C49 C50 1.372(8) . ? C49 C77 1.538(8) . ? C50 C51 1.365(8) . ? C50 H50 0.9300 . ? C51 C52 1.412(7) . ? C51 C81 1.553(8) . ? C52 H52 0.9300 . ? C53 C56C 1.508(10) . ? C53 C56A 1.511(9) . ? C53 C54A 1.512(9) . ? C53 C55A 1.519(9) . ? C53 C55C 1.521(9) . ? C53 C54C 1.525(10) . ? C53 C54B 1.526(9) . ? C53 C55B 1.530(9) . ? C53 C56B 1.533(9) . ? C57 C59 1.514(11) . ? C57 C60 1.519(11) . ? C57 C58 1.597(10) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C64 1.497(11) . ? C61 C63 1.543(8) . ? C61 C62 1.557(10) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C68B 1.506(9) . ? C65 C68C 1.508(9) . ? C65 C67B 1.510(9) . ? C65 C68A 1.511(9) . ? C65 C66C 1.516(10) . ? C65 C66A 1.517(9) . ? C65 C67A 1.519(8) . ? C65 C66B 1.523(9) . ? C65 C67C 1.528(9) . ? C69 C70A 1.502(10) . ? C69 C71A 1.511(9) . ? C69 C72A 1.512(10) . ? C69 C71B 1.515(9) . ? C69 C72B 1.516(9) . ? C69 C71C 1.517(10) . ? C69 C72C 1.518(9) . ? C69 C70B 1.521(9) . ? C69 C70C 1.528(9) . ? C73 C75B 1.5001(11) . ? C73 C75A 1.5001(11) . ? C73 C74A 1.509(10) . ? C73 C76A 1.509(10) . ? C73 C76B 1.513(8) . ? C73 C74B 1.523(9) . ? C73 C74C 1.523(9) . ? C73 C76C 1.533(9) . ? C73 C75C 1.535(8) . ? C77 C78B 1.509(9) . ? C77 C79C 1.514(9) . ? C77 C78C 1.516(9) . ? C77 C78A 1.516(9) . ? C77 C80C 1.517(9) . ? C77 C79A 1.518(9) . ? C77 C80A 1.520(9) . ? C77 C80B 1.521(9) . ? C77 C79B 1.531(9) . ? C81 C83C 1.494(10) . ? C81 C84B 1.502(9) . ? C81 C83B 1.503(9) . ? C81 C84C 1.504(10) . ? C81 C83A 1.507(10) . ? C81 C84A 1.509(10) . ? C81 C82A 1.510(10) . ? C81 C82C 1.511(10) . ? C81 C82B 1.527(9) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? Cl3 O2 1.345(8) . ? Cl3 O5 1.352(9) . ? Cl3 O4 1.355(9) . ? Cl3 O3 1.356(8) . ? Cl4 O7 1.348(9) . ? Cl4 O8 1.348(9) . ? Cl4 O9 1.353(9) . ? Cl4 O6 1.356(9) . ? Cl5 O12 1.353(9) . ? Cl5 O13 1.360(9) . ? Cl5 O11 1.361(9) . ? Cl5 O10 1.364(8) . ? 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 N2 Fe1 N3 89.54(16) . . ? N2 Fe1 N1 89.01(16) . . ? N3 Fe1 N1 156.60(19) . . ? N2 Fe1 N4 169.94(18) . . ? N3 Fe1 N4 88.42(15) . . ? N1 Fe1 N4 88.95(16) . . ? N2 Fe1 O1 95.47(18) . . ? N3 Fe1 O1 101.65(18) . . ? N1 Fe1 O1 101.74(18) . . ? N4 Fe1 O1 94.60(17) . . ? Fe1 O1 H1 109.5 . . ? Fe1 O1 H01A 122.3 . . ? H1 O1 H01A 97.2 . . ? C4 N1 C1 104.5(4) . . ? C4 N1 Fe1 126.1(3) . . ? C1 N1 Fe1 125.7(3) . . ? C9 N2 C6 104.4(4) . . ? C9 N2 Fe1 121.4(3) . . ? C6 N2 Fe1 122.2(3) . . ? C14 N3 C11 104.3(4) . . ? C14 N3 Fe1 127.3(3) . . ? C11 N3 Fe1 124.8(3) . . ? C19 N4 C16 106.3(4) . . ? C19 N4 Fe1 121.5(3) . . ? C16 N4 Fe1 121.2(3) . . ? C20 C1 N1 120.6(4) . . ? C20 C1 C2 128.2(4) . . ? N1 C1 C2 110.8(4) . . ? C3 C2 C1 106.8(4) . . ? C3 C2 C21 124.5(5) . . ? C1 C2 C21 128.4(5) . . ? C2 C3 C4 107.0(4) . . ? C2 C3 C22 124.9(5) . . ? C4 C3 C22 128.0(5) . . ? C5 C4 N1 120.4(5) . . ? C5 C4 C3 129.1(5) . . ? N1 C4 C3 110.2(4) . . ? C4 C5 C6 121.9(5) . . ? C4 C5 C29 118.1(5) . . ? C6 C5 C29 119.9(5) . . ? N2 C6 C5 120.1(5) . . ? N2 C6 C7 110.3(5) . . ? C5 C6 C7 129.3(5) . . ? C8 C7 C6 107.7(4) . . ? C8 C7 C23 124.2(5) . . ? C6 C7 C23 127.9(5) . . ? C7 C8 C9 106.6(5) . . ? C7 C8 C24 126.6(5) . . ? C9 C8 C24 126.3(5) . . ? N2 C9 C10 119.7(5) . . ? N2 C9 C8 110.7(5) . . ? C10 C9 C8 128.8(5) . . ? C11 C10 C9 120.5(5) . . ? C11 C10 C35 117.1(5) . . ? C9 C10 C35 122.4(5) . . ? C10 C11 N3 121.0(5) . . ? C10 C11 C12 128.3(5) . . ? N3 C11 C12 110.0(4) . . ? C13 C12 C11 107.0(5) . . ? C13 C12 C25 125.2(5) . . ? C11 C12 C25 127.2(5) . . ? C12 C13 C14 106.1(4) . . ? C12 C13 C26 124.5(5) . . ? C14 C13 C26 129.1(5) . . ? N3 C14 C15 120.5(5) . . ? N3 C14 C13 112.0(4) . . ? C15 C14 C13 126.9(4) . . ? C16 C15 C14 120.5(4) . . ? C16 C15 C41 121.6(4) . . ? C14 C15 C41 117.8(4) . . ? C15 C16 N4 120.6(4) . . ? C15 C16 C17 129.1(4) . . ? N4 C16 C17 109.8(4) . . ? C18 C17 C16 106.4(4) . . ? C18 C17 C27 125.4(5) . . ? C16 C17 C27 127.8(5) . . ? C17 C18 C19 107.9(4) . . ? C17 C18 C28 124.0(5) . . ? C19 C18 C28 127.8(5) . . ? N4 C19 C20 121.1(4) . . ? N4 C19 C18 109.1(4) . . ? C20 C19 C18 129.3(4) . . ? C1 C20 C19 121.0(4) . . ? C1 C20 C47 118.3(4) . . ? C19 C20 C47 120.7(4) . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C3 C22 H22A 109.5 . . ? C3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C7 C23 H23A 109.5 . . ? C7 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C7 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C24 H24A 109.5 . . ? C8 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C8 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C12 C25 H25A 109.5 . . ? C12 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C12 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C13 C26 H26A 109.5 . . ? C13 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C13 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C17 C27 H27A 109.5 . . ? C17 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C17 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 118.5(5) . . ? C34 C29 C5 122.2(5) . . ? C30 C29 C5 119.3(5) . . ? C31 C30 C29 121.9(5) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C32 117.5(5) . . ? C30 C31 C53 121.8(6) . . ? C32 C31 C53 120.7(5) . . ? C33 C32 C31 123.4(5) . . ? C33 C32 H32 118.3 . . ? C31 C32 H32 118.3 . . ? C32 C33 C34 117.8(5) . . ? C32 C33 C57 124.2(5) . . ? C34 C33 C57 118.1(6) . . ? C29 C34 C33 121.0(5) . . ? C29 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C36 C35 C40 119.4(5) . . ? C36 C35 C10 122.0(5) . . ? C40 C35 C10 118.4(5) . . ? C37 C36 C35 121.8(5) . . ? C37 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C36 C37 C38 118.5(5) . . ? C36 C37 C61 120.5(6) . . ? C38 C37 C61 120.7(5) . . ? C39 C38 C37 121.6(5) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C38 C39 C40 117.9(5) . . ? C38 C39 C65 120.8(5) . . ? C40 C39 C65 121.2(5) . . ? C35 C40 C39 120.7(5) . . ? C35 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C46 C41 C42 119.9(5) . . ? C46 C41 C15 122.2(5) . . ? C42 C41 C15 117.8(5) . . ? C43 C42 C41 120.8(5) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C42 C43 C44 117.2(5) . . ? C42 C43 C69 121.6(5) . . ? C44 C43 C69 121.1(5) . . ? C45 C44 C43 123.0(5) . . ? C45 C44 H44 118.5 . . ? C43 C44 H44 118.5 . . ? C44 C45 C46 117.6(5) . . ? C44 C45 C73 120.9(5) . . ? C46 C45 C73 121.4(5) . . ? C41 C46 C45 121.2(5) . . ? C41 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C48 C47 C52 119.5(5) . . ? C48 C47 C20 121.9(5) . . ? C52 C47 C20 118.5(5) . . ? C47 C48 C49 122.2(6) . . ? C47 C48 H48 118.9 . . ? C49 C48 H48 118.9 . . ? C50 C49 C48 116.3(6) . . ? C50 C49 C77 122.3(5) . . ? C48 C49 C77 121.4(6) . . ? C51 C50 C49 125.1(5) . . ? C51 C50 H50 117.5 . . ? C49 C50 H50 117.5 . . ? C50 C51 C52 116.6(5) . . ? C50 C51 C81 122.9(5) . . ? C52 C51 C81 120.5(6) . . ? C47 C52 C51 120.3(5) . . ? C47 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C56C C53 C56A 88.1(18) . . ? C56A C53 C54A 111.3(8) . . ? C56C C53 C55A 132.7(17) . . ? C56A C53 C55A 111.2(8) . . ? C54A C53 C55A 110.6(8) . . ? C56C C53 C55C 110.8(9) . . ? C54A C53 C55C 130.8(19) . . ? C55A C53 C55C 88.5(16) . . ? C56C C53 C54C 110.7(9) . . ? C56A C53 C54C 128.7(19) . . ? C54A C53 C54C 86.6(15) . . ? C55C C53 C54C 109.5(9) . . ? C56C C53 C54B 66.5(15) . . ? C56A C53 C54B 129.7(15) . . ? C55A C53 C54B 68.2(13) . . ? C55C C53 C54B 130.3(17) . . ? C56C C53 C55B 139.1(18) . . ? C56A C53 C55B 63.0(13) . . ? C54A C53 C55B 141.4(14) . . ? C55A C53 C55B 50.1(11) . . ? C54C C53 C55B 73.2(13) . . ? C54B C53 C55B 109.0(8) . . ? C56C C53 C56B 46.0(14) . . ? C56A C53 C56B 45.9(14) . . ? C54A C53 C56B 71.8(15) . . ? C55A C53 C56B 149.8(16) . . ? C55C C53 C56B 70.4(14) . . ? C54C C53 C56B 146.9(17) . . ? C54B C53 C56B 109.0(8) . . ? C55B C53 C56B 108.4(8) . . ? C56C C53 C31 106.4(16) . . ? C56A C53 C31 112.5(10) . . ? C54A C53 C31 106.0(9) . . ? C55A C53 C31 105.0(12) . . ? C55C C53 C31 112.2(15) . . ? C54C C53 C31 107.2(15) . . ? C54B C53 C31 116.0(10) . . ? C55B C53 C31 111.2(11) . . ? C56B C53 C31 102.9(13) . . ? C59 C57 C60 112.9(7) . . ? C59 C57 C33 111.7(6) . . ? C60 C57 C33 108.8(6) . . ? C59 C57 C58 106.1(7) . . ? C60 C57 C58 108.3(7) . . ? C33 C57 C58 108.9(6) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C64 C61 C63 109.8(7) . . ? C64 C61 C37 109.3(5) . . ? C63 C61 C37 111.4(6) . . ? C64 C61 C62 108.6(7) . . ? C63 C61 C62 107.2(6) . . ? C37 C61 C62 110.4(5) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C68B C65 C67B 111.8(8) . . ? C68C C65 C67B 132.4(14) . . ? C68B C65 C68A 53.0(15) . . ? C68C C65 C68A 88.6(17) . . ? C67B C65 C68A 69.5(14) . . ? C68B C65 C66C 137.1(17) . . ? C68C C65 C66C 111.2(9) . . ? C67B C65 C66C 67.0(16) . . ? C68A C65 C66C 134.4(17) . . ? C68B C65 C66A 59.5(16) . . ? C67B C65 C66A 129.5(19) . . ? C68A C65 C66A 110.7(9) . . ? C66C C65 C66A 87.5(17) . . ? C68B C65 C67A 139.6(11) . . ? C68C C65 C67A 130.6(16) . . ? C68A C65 C67A 110.4(8) . . ? C66A C65 C67A 110.0(8) . . ? C68B C65 C66B 110.6(8) . . ? C68C C65 C66B 75.3(12) . . ? C67B C65 C66B 110.3(9) . . ? C68A C65 C66B 157.7(18) . . ? C66A C65 C66B 51.1(15) . . ? C67A C65 C66B 71.2(13) . . ? C68B C65 C67C 76.9(11) . . ? C68C C65 C67C 110.3(8) . . ? C66C C65 C67C 109.5(9) . . ? C66A C65 C67C 127(2) . . ? C67A C65 C67C 84.0(14) . . ? C66B C65 C67C 149.3(18) . . ? C68B C65 C39 109.0(9) . . ? C68C C65 C39 108.8(12) . . ? C67B C65 C39 116.7(14) . . ? C68A C65 C39 102.2(13) . . ? C66C C65 C39 108.8(15) . . ? C66A C65 C39 112.5(13) . . ? C67A C65 C39 110.8(8) . . ? C66B C65 C39 97.6(13) . . ? C67C C65 C39 108.1(12) . . ? C70A C69 C71A 111.9(9) . . ? C70A C69 C72A 112.0(9) . . ? C71A C69 C72A 111.3(9) . . ? C70A C69 C71B 141.3(16) . . ? C72A C69 C71B 84(2) . . ? C70A C69 C72B 90(2) . . ? C71A C69 C72B 137(2) . . ? C71B C69 C72B 110.8(9) . . ? C70A C69 C71C 145(2) . . ? C71A C69 C71C 45.2(18) . . ? C72A C69 C71C 69.1(18) . . ? C72B C69 C71C 96(3) . . ? C70A C69 C72C 70.4(16) . . ? C71A C69 C72C 142.3(17) . . ? C71B C69 C72C 125(2) . . ? C71C C69 C72C 110.8(9) . . ? C71A C69 C70B 80.7(14) . . ? C72A C69 C70B 121.3(19) . . ? C71B C69 C70B 109.8(8) . . ? C72B C69 C70B 110.5(8) . . ? C71C C69 C70B 116(2) . . ? C72C C69 C70B 91.3(14) . . ? C71A C69 C70C 67.7(18) . . ? C72A C69 C70C 137.2(18) . . ? C71B C69 C70C 99(2) . . ? C72B C69 C70C 129.0(16) . . ? C71C C69 C70C 109.3(9) . . ? C72C C69 C70C 109.6(9) . . ? C70A C69 C43 100.8(17) . . ? C71A C69 C43 106.2(12) . . ? C72A C69 C43 114.2(16) . . ? C71B C69 C43 104.5(8) . . ? C72B C69 C43 104.5(14) . . ? C71C C69 C43 110(2) . . ? C72C C69 C43 110.2(13) . . ? C70B C69 C43 116.5(8) . . ? C70C C69 C43 106.4(10) . . ? C75B C73 C74A 143(3) . . ? C75A C73 C74A 112.0(9) . . ? C75B C73 C76A 74(2) . . ? C75A C73 C76A 112.0(9) . . ? C74A C73 C76A 111.4(10) . . ? C75B C73 C76B 112.1(7) . . ? C75A C73 C76B 143(3) . . ? C74A C73 C76B 75(3) . . ? C75B C73 C74B 111.3(8) . . ? C75A C73 C74B 73(3) . . ? C76A C73 C74B 136(3) . . ? C76B C73 C74B 110.2(8) . . ? C75B C73 C74C 83.7(13) . . ? C75A C73 C74C 46(4) . . ? C74A C73 C74C 67(4) . . ? C76A C73 C74C 134(2) . . ? C76B C73 C74C 128.7(19) . . ? C75B C73 C76C 137.8(10) . . ? C75A C73 C76C 148(4) . . ? C74A C73 C76C 46(3) . . ? C76A C73 C76C 69(3) . . ? C74B C73 C76C 84.6(16) . . ? C74C C73 C76C 109.1(8) . . ? C75A C73 C75C 72(3) . . ? C74A C73 C75C 139.6(18) . . ? C76B C73 C75C 80.0(9) . . ? C74B C73 C75C 131.5(14) . . ? C74C C73 C75C 108.8(8) . . ? C76C C73 C75C 107.8(7) . . ? C75B C73 C45 108.0(7) . . ? C75A C73 C45 105(3) . . ? C74A C73 C45 103(2) . . ? C76A C73 C45 113(2) . . ? C76B C73 C45 108.8(10) . . ? C74B C73 C45 106.2(13) . . ? C74C C73 C45 111.7(11) . . ? C76C C73 C45 104.0(11) . . ? C75C C73 C45 115.1(7) . . ? C78B C77 C79C 147.6(19) . . ? C78B C77 C78C 45.4(16) . . ? C79C C77 C78C 110.9(9) . . ? C78B C77 C78A 46.6(12) . . ? C79C C77 C78A 138.2(10) . . ? C78C C77 C78A 91.3(16) . . ? C78B C77 C80C 70.6(13) . . ? C79C C77 C80C 110.8(8) . . ? C78C C77 C80C 110.5(9) . . ? C78B C77 C79A 64.9(14) . . ? C79C C77 C79A 93(2) . . ? C78A C77 C79A 110.2(9) . . ? C80C C77 C79A 126(2) . . ? C78B C77 C80A 137.9(13) . . ? C78C C77 C80A 124(2) . . ? C78A C77 C80A 111.1(8) . . ? C80C C77 C80A 83.6(11) . . ? C79A C77 C80A 110.3(9) . . ? C78B C77 C80B 111.4(9) . . ? C79C C77 C80B 68.8(10) . . ? C78C C77 C80B 136.9(16) . . ? C78A C77 C80B 70.9(9) . . ? C79A C77 C80B 137.7(18) . . ? C78B C77 C79B 109.8(8) . . ? C79C C77 C79B 46.3(16) . . ? C78C C77 C79B 65.9(17) . . ? C78A C77 C79B 146.6(14) . . ? C80C C77 C79B 137.8(13) . . ? C79A C77 C79B 46.8(13) . . ? C80A C77 C79B 68.6(11) . . ? C80B C77 C79B 108.6(8) . . ? C78B C77 C49 107.4(12) . . ? C79C C77 C49 102.0(14) . . ? C78C C77 C49 110.6(14) . . ? C78A C77 C49 102.5(10) . . ? C80C C77 C49 111.8(11) . . ? C79A C77 C49 109.5(18) . . ? C80A C77 C49 113.0(8) . . ? C80B C77 C49 111.4(10) . . ? C79B C77 C49 108.2(10) . . ? C83C C81 C84B 89(3) . . ? C84B C81 C83B 112.4(8) . . ? C83C C81 C84C 105(3) . . ? C83B C81 C84C 124(3) . . ? C83C C81 C83A 57(3) . . ? C84B C81 C83A 141.8(19) . . ? C84C C81 C83A 143(3) . . ? C83C C81 C84A 57(3) . . ? C83B C81 C84A 80.9(18) . . ? C84C C81 C84A 51(3) . . ? C83A C81 C84A 111.6(10) . . ? C83C C81 C82A 145(2) . . ? C84B C81 C82A 87(2) . . ? C83B C81 C82A 135(2) . . ? C84C C81 C82A 63(2) . . ? C83A C81 C82A 111.6(10) . . ? C84A C81 C82A 111.5(10) . . ? C83C C81 C82C 107(3) . . ? C84B C81 C82C 126(2) . . ? C83B C81 C82C 86(2) . . ? C84C C81 C82C 103(2) . . ? C83A C81 C82C 60(2) . . ? C84A C81 C82C 129(3) . . ? C82A C81 C82C 52(3) . . ? C83C C81 C82B 130(2) . . ? C84B C81 C82B 110.9(8) . . ? C83B C81 C82B 110.8(8) . . ? C84C C81 C82B 86(2) . . ? C83A C81 C82B 85(2) . . ? C84A C81 C82B 128(3) . . ? C83C C81 C51 109.0(10) . . ? C84B C81 C51 106.3(8) . . ? C83B C81 C51 107.7(12) . . ? C84C C81 C51 116.4(14) . . ? C83A C81 C51 101(2) . . ? C84A C81 C51 115(2) . . ? C82A C81 C51 105(2) . . ? C82C C81 C51 115.7(13) . . ? C82B C81 C51 108.6(11) . . ? Cl2 C85 Cl1 107.3(10) . . ? Cl2 C85 H85A 110.3 . . ? Cl1 C85 H85A 110.3 . . ? Cl2 C85 H85B 110.3 . . ? Cl1 C85 H85B 110.3 . . ? H85A C85 H85B 108.5 . . ? O2 Cl3 O5 110.6(11) . . ? O2 Cl3 O4 110.0(10) . . ? O5 Cl3 O4 108.9(10) . . ? O2 Cl3 O3 110.1(10) . . ? O5 Cl3 O3 109.1(10) . . ? O4 Cl3 O3 108.0(10) . . ? O7 Cl4 O8 111.7(10) . . ? O7 Cl4 O9 109.5(10) . . ? O8 Cl4 O9 109.9(10) . . ? O7 Cl4 O6 108.2(10) . . ? O8 Cl4 O6 108.5(10) . . ? O9 Cl4 O6 109.0(10) . . ? O12 Cl5 O13 108.6(10) . . ? O12 Cl5 O11 109.9(11) . . ? O13 Cl5 O11 109.5(10) . . ? O12 Cl5 O10 109.9(10) . . ? O13 Cl5 O10 109.3(10) . . ? O11 Cl5 O10 109.7(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 N1 C4 8.3(5) . . . . ? N3 Fe1 N1 C4 -78.3(6) . . . . ? N4 Fe1 N1 C4 -161.9(4) . . . . ? O1 Fe1 N1 C4 103.6(4) . . . . ? N2 Fe1 N1 C1 163.0(4) . . . . ? N3 Fe1 N1 C1 76.4(6) . . . . ? N4 Fe1 N1 C1 -7.2(4) . . . . ? O1 Fe1 N1 C1 -101.6(4) . . . . ? N3 Fe1 N2 C9 -35.3(4) . . . . ? N1 Fe1 N2 C9 168.1(5) . . . . ? N4 Fe1 N2 C9 -113.6(9) . . . . ? O1 Fe1 N2 C9 66.4(5) . . . . ? N3 Fe1 N2 C6 -172.0(4) . . . . ? N1 Fe1 N2 C6 31.3(4) . . . . ? N4 Fe1 N2 C6 109.7(10) . . . . ? O1 Fe1 N2 C6 -70.4(4) . . . . ? N2 Fe1 N3 C14 -161.0(4) . . . . ? N1 Fe1 N3 C14 -74.5(6) . . . . ? N4 Fe1 N3 C14 9.2(4) . . . . ? O1 Fe1 N3 C14 103.6(4) . . . . ? N2 Fe1 N3 C11 -6.0(4) . . . . ? N1 Fe1 N3 C11 80.4(5) . . . . ? N4 Fe1 N3 C11 164.1(4) . . . . ? O1 Fe1 N3 C11 -101.5(4) . . . . ? N2 Fe1 N4 C19 -111.0(9) . . . . ? N3 Fe1 N4 C19 170.6(4) . . . . ? N1 Fe1 N4 C19 -32.7(4) . . . . ? O1 Fe1 N4 C19 69.0(4) . . . . ? N2 Fe1 N4 C16 109.9(9) . . . . ? N3 Fe1 N4 C16 31.5(4) . . . . ? N1 Fe1 N4 C16 -171.7(4) . . . . ? O1 Fe1 N4 C16 -70.0(4) . . . . ? C4 N1 C1 C20 -165.3(5) . . . . ? Fe1 N1 C1 C20 35.6(7) . . . . ? C4 N1 C1 C2 8.2(6) . . . . ? Fe1 N1 C1 C2 -151.0(4) . . . . ? C20 C1 C2 C3 168.2(5) . . . . ? N1 C1 C2 C3 -4.7(6) . . . . ? C20 C1 C2 C21 -18.1(9) . . . . ? N1 C1 C2 C21 169.0(5) . . . . ? C1 C2 C3 C4 -0.8(6) . . . . ? C21 C2 C3 C4 -174.8(5) . . . . ? C1 C2 C3 C22 174.9(6) . . . . ? C21 C2 C3 C22 0.9(9) . . . . ? C1 N1 C4 C5 165.6(5) . . . . ? Fe1 N1 C4 C5 -35.4(7) . . . . ? C1 N1 C4 C3 -8.6(6) . . . . ? Fe1 N1 C4 C3 150.4(4) . . . . ? C2 C3 C4 C5 -167.5(6) . . . . ? C22 C3 C4 C5 17.0(10) . . . . ? C2 C3 C4 N1 6.0(6) . . . . ? C22 C3 C4 N1 -169.5(6) . . . . ? N1 C4 C5 C6 23.8(8) . . . . ? C3 C4 C5 C6 -163.2(6) . . . . ? N1 C4 C5 C29 -153.9(5) . . . . ? C3 C4 C5 C29 19.1(9) . . . . ? C9 N2 C6 C5 168.0(5) . . . . ? Fe1 N2 C6 C5 -49.1(7) . . . . ? C9 N2 C6 C7 -5.9(6) . . . . ? Fe1 N2 C6 C7 137.0(4) . . . . ? C4 C5 C6 N2 19.0(8) . . . . ? C29 C5 C6 N2 -163.4(5) . . . . ? C4 C5 C6 C7 -168.4(6) . . . . ? C29 C5 C6 C7 9.3(9) . . . . ? N2 C6 C7 C8 3.7(7) . . . . ? C5 C6 C7 C8 -169.5(6) . . . . ? N2 C6 C7 C23 -171.0(7) . . . . ? C5 C6 C7 C23 15.8(11) . . . . ? C6 C7 C8 C9 0.2(7) . . . . ? C23 C7 C8 C9 175.1(6) . . . . ? C6 C7 C8 C24 -171.1(7) . . . . ? C23 C7 C8 C24 3.9(12) . . . . ? C6 N2 C9 C10 -164.8(5) . . . . ? Fe1 N2 C9 C10 51.9(7) . . . . ? C6 N2 C9 C8 6.1(6) . . . . ? Fe1 N2 C9 C8 -137.2(4) . . . . ? C7 C8 C9 N2 -4.0(7) . . . . ? C24 C8 C9 N2 167.3(7) . . . . ? C7 C8 C9 C10 165.8(6) . . . . ? C24 C8 C9 C10 -22.9(11) . . . . ? N2 C9 C10 C11 -17.8(8) . . . . ? C8 C9 C10 C11 173.1(6) . . . . ? N2 C9 C10 C35 160.9(5) . . . . ? C8 C9 C10 C35 -8.1(10) . . . . ? C9 C10 C11 N3 -27.2(8) . . . . ? C35 C10 C11 N3 154.0(5) . . . . ? C9 C10 C11 C12 163.1(6) . . . . ? C35 C10 C11 C12 -15.8(9) . . . . ? C14 N3 C11 C10 -164.1(5) . . . . ? Fe1 N3 C11 C10 36.2(7) . . . . ? C14 N3 C11 C12 7.4(6) . . . . ? Fe1 N3 C11 C12 -152.3(4) . . . . ? C10 C11 C12 C13 166.6(5) . . . . ? N3 C11 C12 C13 -4.1(6) . . . . ? C10 C11 C12 C25 -21.9(9) . . . . ? N3 C11 C12 C25 167.5(5) . . . . ? C11 C12 C13 C14 -0.8(6) . . . . ? C25 C12 C13 C14 -172.6(5) . . . . ? C11 C12 C13 C26 173.7(5) . . . . ? C25 C12 C13 C26 1.9(9) . . . . ? C11 N3 C14 C15 163.9(5) . . . . ? Fe1 N3 C14 C15 -37.1(6) . . . . ? C11 N3 C14 C13 -8.0(5) . . . . ? Fe1 N3 C14 C13 151.0(4) . . . . ? C12 C13 C14 N3 5.7(6) . . . . ? C26 C13 C14 N3 -168.5(5) . . . . ? C12 C13 C14 C15 -165.6(5) . . . . ? C26 C13 C14 C15 20.2(9) . . . . ? N3 C14 C15 C16 24.2(7) . . . . ? C13 C14 C15 C16 -165.2(5) . . . . ? N3 C14 C15 C41 -153.3(5) . . . . ? C13 C14 C15 C41 17.3(8) . . . . ? C14 C15 C16 N4 20.2(7) . . . . ? C41 C15 C16 N4 -162.4(5) . . . . ? C14 C15 C16 C17 -168.8(5) . . . . ? C41 C15 C16 C17 8.6(9) . . . . ? C19 N4 C16 C15 165.3(5) . . . . ? Fe1 N4 C16 C15 -50.3(6) . . . . ? C19 N4 C16 C17 -7.3(5) . . . . ? Fe1 N4 C16 C17 137.0(4) . . . . ? C15 C16 C17 C18 -166.9(5) . . . . ? N4 C16 C17 C18 4.9(6) . . . . ? C15 C16 C17 C27 19.8(10) . . . . ? N4 C16 C17 C27 -168.4(6) . . . . ? C16 C17 C18 C19 -0.6(6) . . . . ? C27 C17 C18 C19 172.9(5) . . . . ? C16 C17 C18 C28 -174.4(5) . . . . ? C27 C17 C18 C28 -0.9(9) . . . . ? C16 N4 C19 C20 -165.6(4) . . . . ? Fe1 N4 C19 C20 50.2(6) . . . . ? C16 N4 C19 C18 6.9(5) . . . . ? Fe1 N4 C19 C18 -137.4(4) . . . . ? C17 C18 C19 N4 -4.0(6) . . . . ? C28 C18 C19 N4 169.5(5) . . . . ? C17 C18 C19 C20 167.6(5) . . . . ? C28 C18 C19 C20 -18.8(9) . . . . ? N1 C1 C20 C19 -25.5(8) . . . . ? C2 C1 C20 C19 162.3(5) . . . . ? N1 C1 C20 C47 154.8(5) . . . . ? C2 C1 C20 C47 -17.5(8) . . . . ? N4 C19 C20 C1 -18.5(7) . . . . ? C18 C19 C20 C1 170.8(5) . . . . ? N4 C19 C20 C47 161.3(5) . . . . ? C18 C19 C20 C47 -9.5(8) . . . . ? C4 C5 C29 C34 -121.7(6) . . . . ? C6 C5 C29 C34 60.6(8) . . . . ? C4 C5 C29 C30 57.4(8) . . . . ? C6 C5 C29 C30 -120.3(6) . . . . ? C34 C29 C30 C31 1.2(9) . . . . ? C5 C29 C30 C31 -177.9(5) . . . . ? C29 C30 C31 C32 -1.4(9) . . . . ? C29 C30 C31 C53 -178.7(5) . . . . ? C30 C31 C32 C33 1.1(10) . . . . ? C53 C31 C32 C33 178.5(6) . . . . ? C31 C32 C33 C34 -0.6(10) . . . . ? C31 C32 C33 C57 179.9(6) . . . . ? C30 C29 C34 C33 -0.7(9) . . . . ? C5 C29 C34 C33 178.4(6) . . . . ? C32 C33 C34 C29 0.4(9) . . . . ? C57 C33 C34 C29 179.9(6) . . . . ? C11 C10 C35 C36 120.9(6) . . . . ? C9 C10 C35 C36 -57.9(9) . . . . ? C11 C10 C35 C40 -54.2(8) . . . . ? C9 C10 C35 C40 127.0(6) . . . . ? C40 C35 C36 C37 -0.9(10) . . . . ? C10 C35 C36 C37 -175.9(6) . . . . ? C35 C36 C37 C38 3.1(10) . . . . ? C35 C36 C37 C61 176.4(6) . . . . ? C36 C37 C38 C39 -3.5(10) . . . . ? C61 C37 C38 C39 -176.8(6) . . . . ? C37 C38 C39 C40 1.6(10) . . . . ? C37 C38 C39 C65 177.6(6) . . . . ? C36 C35 C40 C39 -1.0(9) . . . . ? C10 C35 C40 C39 174.2(6) . . . . ? C38 C39 C40 C35 0.6(9) . . . . ? C65 C39 C40 C35 -175.3(6) . . . . ? C16 C15 C41 C46 59.2(8) . . . . ? C14 C15 C41 C46 -123.4(6) . . . . ? C16 C15 C41 C42 -123.0(6) . . . . ? C14 C15 C41 C42 54.5(7) . . . . ? C46 C41 C42 C43 3.7(8) . . . . ? C15 C41 C42 C43 -174.2(5) . . . . ? C41 C42 C43 C44 -3.9(8) . . . . ? C41 C42 C43 C69 176.5(5) . . . . ? C42 C43 C44 C45 3.0(9) . . . . ? C69 C43 C44 C45 -177.4(6) . . . . ? C43 C44 C45 C46 -1.9(9) . . . . ? C43 C44 C45 C73 -179.1(5) . . . . ? C42 C41 C46 C45 -2.5(8) . . . . ? C15 C41 C46 C45 175.3(5) . . . . ? C44 C45 C46 C41 1.6(8) . . . . ? C73 C45 C46 C41 178.8(5) . . . . ? C1 C20 C47 C48 123.2(6) . . . . ? C19 C20 C47 C48 -56.5(7) . . . . ? C1 C20 C47 C52 -53.3(7) . . . . ? C19 C20 C47 C52 127.0(5) . . . . ? C52 C47 C48 C49 -0.4(9) . . . . ? C20 C47 C48 C49 -176.9(5) . . . . ? C47 C48 C49 C50 -1.0(9) . . . . ? C47 C48 C49 C77 -178.4(5) . . . . ? C48 C49 C50 C51 3.2(10) . . . . ? C77 C49 C50 C51 -179.5(6) . . . . ? C49 C50 C51 C52 -3.6(9) . . . . ? C49 C50 C51 C81 177.4(6) . . . . ? C48 C47 C52 C51 0.0(8) . . . . ? C20 C47 C52 C51 176.6(5) . . . . ? C50 C51 C52 C47 1.9(8) . . . . ? C81 C51 C52 C47 -179.1(5) . . . . ? C30 C31 C53 C56C 72.4(14) . . . . ? C32 C31 C53 C56C -104.9(14) . . . . ? C30 C31 C53 C56A 167.3(15) . . . . ? C32 C31 C53 C56A -10.0(16) . . . . ? C30 C31 C53 C54A 45.4(15) . . . . ? C32 C31 C53 C54A -131.9(14) . . . . ? C30 C31 C53 C55A -71.7(13) . . . . ? C32 C31 C53 C55A 111.0(13) . . . . ? C30 C31 C53 C55C -166.3(13) . . . . ? C32 C31 C53 C55C 16.4(15) . . . . ? C30 C31 C53 C54C -46.0(13) . . . . ? C32 C31 C53 C54C 136.7(12) . . . . ? C30 C31 C53 C54B 1.0(16) . . . . ? C32 C31 C53 C54B -176.3(15) . . . . ? C30 C31 C53 C55B -124.2(13) . . . . ? C32 C31 C53 C55B 58.5(14) . . . . ? C30 C31 C53 C56B 119.9(13) . . . . ? C32 C31 C53 C56B -57.4(14) . . . . ? C32 C33 C57 C59 126.0(8) . . . . ? C34 C33 C57 C59 -53.5(9) . . . . ? C32 C33 C57 C60 -108.7(7) . . . . ? C34 C33 C57 C60 71.8(8) . . . . ? C32 C33 C57 C58 9.2(10) . . . . ? C34 C33 C57 C58 -170.3(7) . . . . ? C36 C37 C61 C64 -88.6(9) . . . . ? C38 C37 C61 C64 84.6(8) . . . . ? C36 C37 C61 C63 149.8(6) . . . . ? C38 C37 C61 C63 -37.0(9) . . . . ? C36 C37 C61 C62 30.8(9) . . . . ? C38 C37 C61 C62 -156.0(6) . . . . ? C38 C39 C65 C68B -128.9(11) . . . . ? C40 C39 C65 C68B 47.0(12) . . . . ? C38 C39 C65 C68C -166.8(13) . . . . ? C40 C39 C65 C68C 9.1(14) . . . . ? C38 C39 C65 C67B -1.2(15) . . . . ? C40 C39 C65 C67B 174.7(14) . . . . ? C38 C39 C65 C68A -74.1(16) . . . . ? C40 C39 C65 C68A 101.8(15) . . . . ? C38 C39 C65 C66C 71.9(16) . . . . ? C40 C39 C65 C66C -112.2(15) . . . . ? C38 C39 C65 C66A 167.1(17) . . . . ? C40 C39 C65 C66A -17.0(18) . . . . ? C38 C39 C65 C67A 43.5(12) . . . . ? C40 C39 C65 C67A -140.7(11) . . . . ? C38 C39 C65 C66B 116.2(13) . . . . ? C40 C39 C65 C66B -68.0(13) . . . . ? C38 C39 C65 C67C -46.9(15) . . . . ? C40 C39 C65 C67C 128.9(14) . . . . ? C42 C43 C69 C70A -118.4(15) . . . . ? C44 C43 C69 C70A 62.0(16) . . . . ? C42 C43 C69 C71A 124.8(16) . . . . ? C44 C43 C69 C71A -54.8(17) . . . . ? C42 C43 C69 C72A 1.8(18) . . . . ? C44 C43 C69 C72A -177.8(17) . . . . ? C42 C43 C69 C71B 91.1(14) . . . . ? C44 C43 C69 C71B -88.5(15) . . . . ? C42 C43 C69 C72B -25.3(15) . . . . ? C44 C43 C69 C72B 155.1(15) . . . . ? C42 C43 C69 C71C 77.2(17) . . . . ? C44 C43 C69 C71C -102.3(17) . . . . ? C42 C43 C69 C72C -45.5(15) . . . . ? C44 C43 C69 C72C 134.9(14) . . . . ? C42 C43 C69 C70B -147.6(10) . . . . ? C44 C43 C69 C70B 32.8(12) . . . . ? C42 C43 C69 C70C -164.2(15) . . . . ? C44 C43 C69 C70C 16.2(16) . . . . ? C44 C45 C73 C75B -144.0(14) . . . . ? C46 C45 C73 C75B 38.9(14) . . . . ? C44 C45 C73 C75A -101(4) . . . . ? C46 C45 C73 C75A 82(4) . . . . ? C44 C45 C73 C74A 16(4) . . . . ? C46 C45 C73 C74A -161(4) . . . . ? C44 C45 C73 C76A 136(3) . . . . ? C46 C45 C73 C76A -41(3) . . . . ? C44 C45 C73 C76B 94.1(14) . . . . ? C46 C45 C73 C76B -83.0(14) . . . . ? C44 C45 C73 C74B -24.5(15) . . . . ? C46 C45 C73 C74B 158.4(14) . . . . ? C44 C45 C73 C74C -53.6(11) . . . . ? C46 C45 C73 C74C 129.3(10) . . . . ? C44 C45 C73 C76C 63.9(10) . . . . ? C46 C45 C73 C76C -113.2(9) . . . . ? C44 C45 C73 C75C -178.4(10) . . . . ? C46 C45 C73 C75C 4.5(11) . . . . ? C50 C49 C77 C78B 53.5(15) . . . . ? C48 C49 C77 C78B -129.3(15) . . . . ? C50 C49 C77 C79C -112.6(15) . . . . ? C48 C49 C77 C79C 64.6(15) . . . . ? C50 C49 C77 C78C 5.4(16) . . . . ? C48 C49 C77 C78C -177.4(16) . . . . ? C50 C49 C77 C78A 101.6(11) . . . . ? C48 C49 C77 C78A -81.2(12) . . . . ? C50 C49 C77 C80C 129.0(12) . . . . ? C48 C49 C77 C80C -53.8(13) . . . . ? C50 C49 C77 C79A -15.4(14) . . . . ? C48 C49 C77 C79A 161.8(13) . . . . ? C50 C49 C77 C80A -138.8(13) . . . . ? C48 C49 C77 C80A 38.4(14) . . . . ? C50 C49 C77 C80B 175.7(11) . . . . ? C48 C49 C77 C80B -7.1(13) . . . . ? C50 C49 C77 C79B -65.0(14) . . . . ? C48 C49 C77 C79B 112.2(14) . . . . ? C50 C51 C81 C83C -140(3) . . . . ? C52 C51 C81 C83C 41(3) . . . . ? C50 C51 C81 C84B 125.0(12) . . . . ? C52 C51 C81 C84B -54.0(12) . . . . ? C50 C51 C81 C83B -114.4(13) . . . . ? C52 C51 C81 C83B 66.7(13) . . . . ? C50 C51 C81 C84C 101(3) . . . . ? C52 C51 C81 C84C -78(3) . . . . ? C50 C51 C81 C83A -82(2) . . . . ? C52 C51 C81 C83A 99(2) . . . . ? C50 C51 C81 C84A 157(2) . . . . ? C52 C51 C81 C84A -22(2) . . . . ? C50 C51 C81 C82A 34(2) . . . . ? C52 C51 C81 C82A -145(2) . . . . ? C50 C51 C81 C82C -20(3) . . . . ? C52 C51 C81 C82C 161(3) . . . . ? C50 C51 C81 C82B 5.6(14) . . . . ? C52 C51 C81 C82B -173.3(13) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.601 _refine_diff_density_min -0.938 _refine_diff_density_rms 0.093