# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hui-Zhong Kou' _publ_contact_author_email KOUHZ@MAIL.TSINGHUA.EDU.CN _publ_section_title ; Supramolecular metallomacrocycles based on trans-dicyanoferrite(III) building blocks: synthesis, crystal structure and magnetic properties ; loop_ _publ_author_name 'Hui-Zhong Kou' 'Ai-Li Cui' 'Zhong-Hai Ni' 'Jun Tao' 'Wolfgang Wernsdorfer' #===End data_4 _database_code_depnum_ccdc_archive 'CCDC 651026' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H72 Br4 Fe2 Mn2 N16 O16' _chemical_formula_weight 2006.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.960(4) _cell_length_b 15.992(5) _cell_length_c 18.327(5) _cell_angle_alpha 73.085(6) _cell_angle_beta 77.852(5) _cell_angle_gamma 79.133(6) _cell_volume 4334(2) _cell_formula_units_Z 2 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 4282 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2020 _exptl_absorpt_coefficient_mu 2.527 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.612 _exptl_absorpt_correction_T_max 0.739 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23705 _diffrn_reflns_av_R_equivalents 0.1379 _diffrn_reflns_av_sigmaI/netI 0.4262 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15027 _reflns_number_gt 4282 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_data_reduction 'Crystalstructure 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _refine_special_details ; The R1 value is greater than 0.1, which is due to the bad quality of the single crystal used for X-ray diffraction measurement. The high Rint value (0.1379) and low observed reflections show that the single crystal weakly diffracts, giving unsatisfactory data results. 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 [0.00000+1.00000exp(4.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0010P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15027 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.3047 _refine_ls_R_factor_gt 0.1015 _refine_ls_wR_factor_ref 0.3351 _refine_ls_wR_factor_gt 0.2374 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.017 _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 0.88977(11) 0.03169(14) 0.16444(11) 0.0417(6) Uani 1 1 d . . . Fe2 Fe 0.68302(12) 0.39118(16) 0.53611(11) 0.0473(6) Uani 1 1 d . . . Mn1 Mn 1.11121(12) -0.25860(16) 0.16228(11) 0.0447(6) Uani 1 1 d . . . Mn2 Mn 0.68611(13) 0.32110(16) 0.18495(12) 0.0469(6) Uani 1 1 d . . . Br4 Br 0.79649(13) 0.72384(14) 0.21666(14) 0.0891(7) Uani 1 1 d . . . Br3 Br 0.24098(15) 0.3268(3) 0.1427(2) 0.1798(18) Uani 1 1 d . . . Br2 Br 0.98932(17) -0.67737(17) 0.17940(18) 0.1182(9) Uani 1 1 d . . . Br1 Br 1.56805(12) -0.2126(2) 0.07782(18) 0.1389(12) Uani 1 1 d . . . N1 N 1.0142(9) -0.1354(9) 0.1455(7) 0.054(3) Uani 1 1 d . . . N2 N 0.7760(8) 0.2140(9) 0.1529(7) 0.053(3) Uani 1 1 d . . . N3 N 0.7213(11) 0.3984(13) 0.6910(9) 0.100(6) Uani 1 1 d . . . N4 N 0.6114(8) 0.4186(10) 0.3860(8) 0.066(4) Uani 1 1 d . . . N5 N 0.8235(7) 0.0117(8) 0.0912(7) 0.051(3) Uani 1 1 d . . . N6 N 0.8031(8) -0.0274(9) 0.2387(6) 0.057(4) Uani 1 1 d . . . N7 N 0.9350(7) 0.0290(9) 0.2514(7) 0.057(4) Uani 1 1 d . . . N8 N 0.9882(7) 0.0987(8) 0.1114(7) 0.048(3) Uani 1 1 d . . . N9 N 0.6650(7) 0.5214(9) 0.5164(7) 0.054(3) Uani 1 1 d . . . N10 N 0.7951(8) 0.4118(10) 0.4810(7) 0.055(4) Uani 1 1 d . . . N11 N 0.7284(7) 0.2740(10) 0.5448(6) 0.056(4) Uani 1 1 d . . . N12 N 0.5789(7) 0.3377(9) 0.5971(7) 0.049(3) Uani 1 1 d . . . N13 N 1.0274(7) -0.3173(9) 0.2534(7) 0.049(3) Uani 1 1 d . . . N14 N 1.1615(6) -0.2136(9) 0.2302(6) 0.048(3) Uani 1 1 d . . . N15 N 0.6136(7) 0.2286(9) 0.2574(7) 0.057(4) Uani 1 1 d . . . N16 N 0.7545(7) 0.3163(9) 0.2678(6) 0.048(3) Uani 1 1 d . . . O1 O 1.0567(7) 0.0506(9) 0.2915(6) 0.079(4) Uani 1 1 d . . . O2 O 0.6697(7) -0.0713(9) 0.2537(6) 0.083(4) Uani 1 1 d . . . O3 O 0.8772(8) 0.5190(11) 0.4094(8) 0.113(6) Uani 1 1 d . . . O4 O 0.6975(9) 0.1307(10) 0.5923(9) 0.103(5) Uani 1 1 d . . . O5 O 1.0675(6) -0.3084(8) 0.0994(5) 0.050(3) Uani 1 1 d . . . O6 O 1.1911(6) -0.2094(7) 0.0787(5) 0.052(3) Uani 1 1 d . . . O7 O 0.7475(6) 0.4118(8) 0.1204(5) 0.061(3) Uani 1 1 d . . . O8 O 0.6189(6) 0.3395(8) 0.1076(6) 0.067(3) Uani 1 1 d . . . O9 O 0.5863(6) 0.4201(8) 0.2370(6) 0.055(3) Uani 1 1 d . . . C52 C 1.0197(8) -0.4319(9) 0.1946(8) 0.039(3) Uani 1 1 d . . . C47 C 1.2440(9) -0.2005(10) 0.2149(8) 0.046(4) Uani 1 1 d . . . H47A H 1.2649 -0.1842 0.2517 0.056 Uiso 1 1 calc R . . C61 C 0.7858(8) 0.6255(14) 0.1889(9) 0.068(5) Uani 1 1 d . . . C51 C 1.0034(9) -0.3897(12) 0.2544(9) 0.057(5) Uani 1 1 d . . . H51A H 0.9710 -0.4177 0.3004 0.068 Uiso 1 1 calc R . . C56 C 1.0646(10) -0.4342(13) 0.0601(9) 0.059(4) Uani 1 1 d . . . H56A H 1.0846 -0.4063 0.0089 0.070 Uiso 1 1 calc R . . C30 C 0.9060(11) -0.0227(14) 0.3962(9) 0.081(6) Uani 1 1 d . . . H30 H 0.9558 -0.0048 0.4021 0.097 Uiso 1 1 calc R . . C48 C 1.1130(11) -0.1871(11) 0.2986(9) 0.064(5) Uani 1 1 d . . . H48A H 1.0722 -0.1347 0.2828 0.076 Uiso 1 1 calc R . . H48B H 1.1525 -0.1724 0.3251 0.076 Uiso 1 1 calc R . . C2 C 0.8162(8) 0.1465(11) 0.1546(7) 0.039(4) Uani 1 1 d . . . C63 C 0.7731(8) 0.4687(11) 0.2176(8) 0.048(4) Uani 1 1 d . . . C57 C 1.0529(9) -0.3918(13) 0.1178(9) 0.055(4) Uani 1 1 d . . . C62 C 0.7873(7) 0.5407(11) 0.2396(8) 0.046(4) Uani 1 1 d . . . H62A H 0.7980 0.5322 0.2894 0.055 Uiso 1 1 calc R . . C41 C 1.2759(8) -0.2101(11) 0.0785(8) 0.051(4) Uani 1 1 d . . . C39 C 0.7894(13) 0.0076(13) -0.0281(10) 0.079(6) Uani 1 1 d . . . H39A H 0.8047 0.0168 -0.0814 0.094 Uiso 1 1 calc R . . C27 C 1.0410(8) 0.0975(10) 0.1598(8) 0.049(4) Uani 1 1 d . . . C60 C 0.7737(11) 0.6335(13) 0.1132(10) 0.069(5) Uani 1 1 d . . . H60A H 0.7699 0.6890 0.0785 0.082 Uiso 1 1 calc R . . C53 C 1.0030(9) -0.5180(11) 0.2110(10) 0.056(4) Uani 1 1 d . . . H53A H 0.9825 -0.5459 0.2620 0.067 Uiso 1 1 calc R . . C33 C 0.7576(11) -0.0792(12) 0.3818(9) 0.071(5) Uani 1 1 d . . . H33A H 0.7095 -0.1008 0.3769 0.085 Uiso 1 1 calc R . . C36 C 0.7505(9) -0.0227(10) 0.1292(8) 0.049(4) Uani 1 1 d . . . C28 C 1.0119(9) 0.0571(10) 0.2427(8) 0.052(4) Uani 1 1 d . . . C35 C 0.7337(9) -0.0436(12) 0.2127(8) 0.058(4) Uani 1 1 d . . . C64 C 0.7795(8) 0.3832(10) 0.2708(8) 0.045(4) Uani 1 1 d . . . H64A H 0.8058 0.3775 0.3130 0.053 Uiso 1 1 calc R . . C58 C 0.7598(9) 0.4803(10) 0.1422(9) 0.045(4) Uani 1 1 d . . . C37 C 0.6917(10) -0.0395(12) 0.0884(11) 0.070(5) Uani 1 1 d . . . H37A H 0.6399 -0.0601 0.1144 0.085 Uiso 1 1 calc R . . C66 C 0.5365(10) 0.3342(11) 0.1171(9) 0.057(4) Uani 1 1 d . . . C54 C 1.0142(9) -0.5637(15) 0.1582(13) 0.079(6) Uani 1 1 d . . . C46 C 1.3014(9) -0.2092(9) 0.1481(7) 0.042(3) Uani 1 1 d . . . C34 C 0.8115(9) -0.0399(10) 0.3151(8) 0.053(4) Uani 1 1 d . . . C59 C 0.7673(9) 0.5616(15) 0.0891(10) 0.070(6) Uani 1 1 d . . . H59A H 0.7681 0.5675 0.0370 0.084 Uiso 1 1 calc R . . C43 C 1.4238(10) -0.2044(11) 0.0071(10) 0.064(5) Uani 1 1 d . . . H43 H 1.4633 -0.2026 -0.0384 0.076 Uiso 1 1 calc R . . C32 C 0.7725(14) -0.0868(15) 0.4511(11) 0.096(7) Uani 1 1 d . . . H32A H 0.7327 -0.1094 0.4941 0.115 Uiso 1 1 calc R . . C40 C 0.8428(9) 0.0261(11) 0.0133(8) 0.056(4) Uani 1 1 d . . . H40A H 0.8935 0.0491 -0.0128 0.067 Uiso 1 1 calc R . . C65 C 0.4943(10) 0.2862(13) 0.1851(12) 0.077(6) Uani 1 1 d . . . C26 C 1.1146(9) 0.1429(11) 0.1332(9) 0.056(4) Uani 1 1 d . . . H26A H 1.1513 0.1415 0.1669 0.067 Uiso 1 1 calc R . . C25 C 1.1303(11) 0.1880(12) 0.0584(11) 0.075(5) Uani 1 1 d . . . H25A H 1.1789 0.2170 0.0400 0.090 Uiso 1 1 calc R . . C67 C 0.4911(11) 0.3810(11) 0.0592(10) 0.069(5) Uani 1 1 d . . . H67A H 0.5204 0.4155 0.0146 0.083 Uiso 1 1 calc R . . C24 C 1.0727(10) 0.1918(14) 0.0067(10) 0.079(6) Uani 1 1 d . . . H24A H 1.0818 0.2234 -0.0449 0.094 Uiso 1 1 calc R . . C31 C 0.8468(14) -0.0617(16) 0.4611(9) 0.100(8) Uani 1 1 d . . . H31A H 0.8580 -0.0704 0.5108 0.120 Uiso 1 1 calc R . . C55 C 1.0457(10) -0.5183(14) 0.0808(12) 0.073(6) Uani 1 1 d . . . H55A H 1.0538 -0.5478 0.0424 0.088 Uiso 1 1 calc R . . C38 C 0.7136(13) -0.0243(12) 0.0092(11) 0.074(5) Uani 1 1 d . . . H38A H 0.6768 -0.0358 -0.0189 0.089 Uiso 1 1 calc R . . C29 C 0.8863(10) -0.0124(11) 0.3229(8) 0.057(4) Uani 1 1 d . . . C49 C 1.0631(9) -0.2614(12) 0.3548(8) 0.062(5) Uani 1 1 d . . . H49A H 1.1031 -0.3152 0.3675 0.074 Uiso 1 1 calc R . . H49B H 1.0377 -0.2448 0.4024 0.074 Uiso 1 1 calc R . . C1 C 0.9679(9) -0.0745(12) 0.1510(8) 0.048(4) Uani 1 1 d . . . C68 C 0.4026(11) 0.3797(15) 0.0637(13) 0.091(7) Uani 1 1 d . . . H68A H 0.3737 0.4100 0.0226 0.109 Uiso 1 1 calc R . . C23 C 1.0033(9) 0.1459(11) 0.0379(9) 0.058(4) Uani 1 1 d . . . H23A H 0.9645 0.1479 0.0059 0.070 Uiso 1 1 calc R . . C42 C 1.3345(9) -0.2055(11) 0.0114(10) 0.064(5) Uani 1 1 d . . . H42A H 1.3145 -0.2031 -0.0334 0.077 Uiso 1 1 calc R . . C50 C 0.9930(10) -0.2777(12) 0.3192(9) 0.066(5) Uani 1 1 d . . . H50A H 0.9567 -0.3168 0.3584 0.079 Uiso 1 1 calc R . . H50B H 0.9570 -0.2222 0.3015 0.079 Uiso 1 1 calc R . . C70 C 0.5368(11) 0.2272(12) 0.2494(10) 0.070(5) Uani 1 1 d . . . H70A H 0.5052 0.1863 0.2864 0.084 Uiso 1 1 calc R . . C45 C 1.3921(9) -0.2069(12) 0.1469(10) 0.069(5) Uani 1 1 d . . . H45A H 1.4121 -0.2060 0.1907 0.082 Uiso 1 1 calc R . . C44 C 1.4482(11) -0.2060(12) 0.0770(13) 0.075(5) Uani 1 1 d . . . C73 C 0.7738(11) 0.2314(11) 0.3258(9) 0.066(5) Uani 1 1 d . . . H73A H 0.8040 0.2413 0.3626 0.080 Uiso 1 1 calc R . . H73B H 0.8119 0.1902 0.2997 0.080 Uiso 1 1 calc R . . C72 C 0.6936(11) 0.1907(11) 0.3689(8) 0.062(5) Uani 1 1 d . . . H72A H 0.6526 0.2345 0.3896 0.074 Uiso 1 1 calc R . . H72B H 0.7090 0.1424 0.4122 0.074 Uiso 1 1 calc R . . C71 C 0.6508(10) 0.1568(11) 0.3197(9) 0.059(4) Uani 1 1 d . . . H71A H 0.6929 0.1160 0.2961 0.071 Uiso 1 1 calc R . . H71B H 0.6050 0.1245 0.3525 0.071 Uiso 1 1 calc R . . C74 C 0.4052(12) 0.2812(14) 0.1938(13) 0.095(7) Uani 1 1 d . . . H74 H 0.3758 0.2466 0.2383 0.114 Uiso 1 1 calc R . . C75 C 0.3622(12) 0.3330(17) 0.1295(16) 0.111(9) Uani 1 1 d . . . C76 C 0.5520(16) 0.501(2) 0.1915(18) 0.143(11) Uani 1 1 d . . . H76A H 0.5729 0.5010 0.1378 0.171 Uiso 1 1 calc R . . H76B H 0.5760 0.5470 0.2013 0.171 Uiso 1 1 calc R . . C77 C 0.4552(16) 0.525(2) 0.2014(17) 0.161(13) Uani 1 1 d . . . H77A H 0.4409 0.5824 0.1683 0.242 Uiso 1 1 calc R . . H77B H 0.4328 0.5248 0.2542 0.242 Uiso 1 1 calc R . . H77C H 0.4302 0.4824 0.1878 0.242 Uiso 1 1 calc R . . C12 C 0.8590(13) 0.1741(15) 0.5026(10) 0.083(6) Uani 1 1 d . . . H12A H 0.8352 0.1220 0.5255 0.100 Uiso 1 1 calc R . . C11 C 0.8146(11) 0.2564(14) 0.5049(9) 0.069(5) Uani 1 1 d . . . C9 C 0.5899(12) 0.2501(14) 0.6149(10) 0.072(5) Uani 1 1 d . . . C8 C 0.5282(13) 0.1977(15) 0.6595(12) 0.088(7) Uani 1 1 d . . . H8A H 0.5389 0.1365 0.6709 0.106 Uiso 1 1 calc R . . C10 C 0.6778(13) 0.2094(15) 0.5821(11) 0.078(6) Uani 1 1 d . . . C4 C 0.6367(9) 0.4076(10) 0.4427(8) 0.051(4) Uani 1 1 d . . . C3 C 0.7085(9) 0.3925(11) 0.6346(9) 0.059(5) Uani 1 1 d . . . C5 C 0.5009(9) 0.3748(12) 0.6277(9) 0.067(5) Uani 1 1 d . . . H5A H 0.4913 0.4359 0.6181 0.081 Uiso 1 1 calc R . . C6 C 0.4353(11) 0.3293(15) 0.6714(10) 0.078(6) Uani 1 1 d . . . H6A H 0.3826 0.3581 0.6903 0.094 Uiso 1 1 calc R . . C7 C 0.4502(16) 0.2417(18) 0.6857(12) 0.101(8) Uani 1 1 d U . . H7A H 0.4062 0.2091 0.7145 0.121 Uiso 1 1 calc R . . C19 C 0.7380(15) 0.6508(16) 0.4559(14) 0.105(9) Uani 1 1 d U . . H19A H 0.7878 0.6753 0.4294 0.126 Uiso 1 1 calc R . . C18 C 0.7366(10) 0.5624(15) 0.4734(9) 0.077(6) Uani 1 1 d . . . C16 C 0.8488(9) 0.3351(13) 0.4723(8) 0.058(5) Uani 1 1 d . . . C21 C 0.5963(12) 0.6627(14) 0.5232(11) 0.078(6) Uani 1 1 d . . . H21A H 0.5474 0.6962 0.5430 0.094 Uiso 1 1 calc R . . C14 C 0.9831(11) 0.248(2) 0.4249(13) 0.125(12) Uani 1 1 d . . . H14A H 1.0388 0.2437 0.3967 0.150 Uiso 1 1 calc R . . C15 C 0.9352(10) 0.3299(17) 0.4304(10) 0.088(7) Uani 1 1 d . . . H15A H 0.9600 0.3814 0.4067 0.106 Uiso 1 1 calc R . . C17 C 0.8099(10) 0.4924(15) 0.4531(9) 0.070(6) Uani 1 1 d . . . C20 C 0.6632(16) 0.7035(15) 0.4787(12) 0.095(7) Uani 1 1 d . . . H20A H 0.6594 0.7647 0.4638 0.115 Uiso 1 1 calc R . . C13 C 0.9446(11) 0.177(2) 0.4619(11) 0.096(9) Uani 1 1 d . . . H13A H 0.9779 0.1233 0.4611 0.115 Uiso 1 1 calc R . . C22 C 0.5982(12) 0.5762(12) 0.5393(10) 0.068(5) Uani 1 1 d . . . H22A H 0.5492 0.5522 0.5689 0.082 Uiso 1 1 calc R . . H1WB H 1.2274 -0.3873 0.2234 0.065 Uiso 1 1 d R . . H1WA H 1.2436 -0.3825 0.1448 0.065 Uiso 1 1 d R . . H9A H 0.6011 0.4266 0.2777 0.065 Uiso 1 1 d R . . O1W O 1.2038(6) -0.3828(8) 0.1843(5) 0.057(3) Uani 1 1 d . . . O2W O 0.4985(14) 0.0264(15) 0.257(3) 0.31(2) Uani 1 1 d . . . O3W O 1.2810(7) -0.4181(9) 0.0431(7) 0.084(4) Uani 1 1 d . . . O4W O 0.409(3) 1.004(3) 0.407(3) 0.37(3) Uani 1 1 d . . . O5W O 1.2358(14) 0.003(3) 0.288(2) 0.38(3) Uani 1 1 d . . . O6W O 0.4618(19) 0.117(2) 0.479(2) 0.270(15) Uani 1 1 d . . . O7W O 0.393(4) 0.050(3) 0.1589(19) 0.43(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0332(10) 0.0474(14) 0.0417(11) -0.0077(10) -0.0028(8) -0.0086(9) Fe2 0.0362(10) 0.0639(16) 0.0419(11) -0.0101(11) -0.0090(9) -0.0105(10) Mn1 0.0364(11) 0.0608(16) 0.0393(12) -0.0125(11) -0.0069(9) -0.0127(11) Mn2 0.0444(11) 0.0558(16) 0.0452(12) -0.0155(11) -0.0176(10) -0.0033(11) Br4 0.0797(13) 0.0687(14) 0.1213(17) -0.0218(12) -0.0109(12) -0.0271(11) Br2 0.1077(17) 0.0853(18) 0.174(2) -0.0658(17) 0.0129(16) -0.0343(15) Br1 0.0436(10) 0.216(3) 0.182(3) -0.090(2) 0.0034(13) -0.0412(15) Br3 0.0673(14) 0.238(4) 0.221(3) 0.009(3) -0.0698(19) -0.0463(19) N8 0.041(6) 0.051(8) 0.050(7) -0.001(6) -0.012(5) -0.013(6) N5 0.033(6) 0.047(8) 0.067(8) -0.011(6) 0.003(6) -0.012(6) O5 0.039(5) 0.066(8) 0.052(6) -0.011(5) -0.023(4) -0.014(5) O6 0.047(5) 0.068(8) 0.052(6) -0.024(5) -0.010(4) -0.014(5) C52 0.037(7) 0.037(9) 0.047(8) -0.021(7) 0.005(6) -0.008(7) O7 0.053(6) 0.092(10) 0.029(5) -0.017(6) 0.001(4) 0.003(6) N6 0.061(8) 0.065(10) 0.039(7) -0.009(6) -0.007(6) 0.001(7) N16 0.045(7) 0.044(8) 0.047(7) -0.010(6) 0.005(5) -0.008(6) N7 0.037(6) 0.065(10) 0.064(8) -0.006(7) -0.009(6) -0.011(6) C47 0.066(10) 0.049(10) 0.039(8) -0.018(7) -0.023(7) -0.017(8) C61 0.025(7) 0.114(17) 0.052(10) -0.028(10) 0.020(6) -0.002(9) C51 0.038(8) 0.067(13) 0.058(10) -0.008(9) 0.000(7) -0.009(8) O8 0.045(6) 0.094(9) 0.073(7) -0.026(6) -0.029(5) -0.005(6) C56 0.064(10) 0.070(13) 0.044(9) -0.017(9) -0.008(7) -0.012(9) C30 0.059(10) 0.125(18) 0.051(10) -0.006(11) -0.017(8) -0.013(11) C48 0.083(11) 0.061(12) 0.065(11) -0.017(9) -0.039(9) -0.021(10) C2 0.028(6) 0.068(12) 0.031(7) -0.020(7) -0.003(6) -0.022(7) N14 0.029(6) 0.074(10) 0.026(6) -0.002(6) 0.003(4) 0.001(6) N13 0.049(7) 0.047(8) 0.056(8) -0.028(6) 0.001(6) -0.009(7) C63 0.031(7) 0.070(12) 0.047(8) -0.021(8) -0.009(6) -0.009(7) C57 0.031(7) 0.075(13) 0.065(11) -0.027(10) -0.011(7) -0.002(8) N2 0.044(7) 0.048(9) 0.065(8) -0.018(7) -0.014(6) 0.011(7) N15 0.036(6) 0.058(9) 0.081(9) -0.019(7) -0.027(6) 0.006(6) C62 0.026(7) 0.067(12) 0.043(8) -0.015(8) -0.008(6) 0.002(7) C41 0.036(7) 0.059(11) 0.062(9) -0.026(8) 0.003(7) -0.010(7) C39 0.108(15) 0.091(15) 0.052(10) -0.017(10) -0.039(11) -0.025(13) N1 0.062(8) 0.049(9) 0.055(8) -0.012(7) -0.006(6) -0.025(7) C27 0.036(7) 0.054(10) 0.064(10) -0.020(8) -0.011(7) -0.012(7) C60 0.068(11) 0.069(14) 0.068(12) -0.013(10) -0.003(9) -0.025(10) O1 0.058(6) 0.116(11) 0.068(7) -0.010(7) -0.029(6) -0.029(7) C53 0.043(8) 0.060(12) 0.068(11) -0.014(9) -0.002(7) -0.026(8) C33 0.078(11) 0.071(13) 0.053(10) 0.010(9) -0.011(9) -0.025(10) C36 0.062(9) 0.050(10) 0.039(8) -0.009(7) -0.004(7) -0.027(8) C28 0.052(9) 0.052(11) 0.047(9) -0.002(8) -0.010(7) -0.009(8) C35 0.045(8) 0.082(13) 0.050(9) -0.023(9) 0.002(7) -0.019(9) C64 0.039(7) 0.045(10) 0.050(9) -0.007(8) -0.012(6) -0.010(7) C58 0.052(8) 0.031(9) 0.061(10) -0.024(8) -0.011(7) -0.001(7) O2 0.064(7) 0.111(11) 0.071(7) -0.013(7) 0.013(6) -0.048(7) C37 0.050(9) 0.077(14) 0.087(13) -0.009(10) -0.005(9) -0.041(9) C66 0.063(10) 0.050(11) 0.060(10) -0.017(8) -0.013(8) -0.006(9) C54 0.028(8) 0.106(17) 0.097(15) -0.026(14) -0.010(9) 0.003(9) C46 0.053(8) 0.044(9) 0.037(8) -0.011(7) -0.014(6) -0.017(7) C34 0.051(9) 0.029(9) 0.053(9) 0.013(7) -0.004(7) 0.011(7) C59 0.047(9) 0.109(17) 0.055(10) -0.013(11) -0.006(7) -0.030(10) C43 0.058(10) 0.053(11) 0.081(12) -0.020(9) 0.013(9) -0.031(9) C32 0.089(14) 0.12(2) 0.057(12) 0.008(12) 0.006(10) -0.035(14) C40 0.049(8) 0.073(12) 0.042(9) -0.014(8) -0.007(7) -0.006(8) C65 0.043(9) 0.091(15) 0.109(15) -0.025(12) -0.043(10) -0.003(10) C26 0.040(8) 0.061(11) 0.070(11) -0.017(9) -0.005(7) -0.018(8) C25 0.067(11) 0.066(13) 0.089(13) -0.009(10) 0.005(10) -0.040(10) C67 0.075(11) 0.048(11) 0.086(12) 0.001(9) -0.043(10) -0.010(9) C24 0.048(9) 0.103(16) 0.074(12) -0.003(11) -0.010(9) -0.017(10) C31 0.097(15) 0.15(2) 0.033(9) 0.004(11) -0.004(9) -0.018(15) C55 0.046(9) 0.093(17) 0.097(15) -0.052(13) -0.035(10) 0.019(10) C38 0.088(13) 0.068(13) 0.089(14) -0.040(11) -0.023(11) -0.023(11) C29 0.050(9) 0.055(11) 0.052(9) -0.012(8) 0.003(7) 0.009(8) C49 0.045(8) 0.103(15) 0.039(8) -0.024(9) -0.005(7) -0.007(9) C1 0.044(8) 0.047(11) 0.046(9) -0.001(8) 0.001(7) -0.015(8) C68 0.048(10) 0.107(17) 0.125(17) -0.004(14) -0.055(11) -0.025(11) C23 0.051(9) 0.079(13) 0.054(10) -0.017(9) -0.012(7) -0.027(9) C42 0.049(9) 0.074(13) 0.070(11) -0.030(9) 0.010(8) -0.012(9) C50 0.058(9) 0.074(13) 0.052(9) -0.001(9) 0.008(7) -0.014(9) C70 0.069(11) 0.060(12) 0.089(13) -0.033(10) -0.006(10) -0.013(10) C45 0.042(8) 0.103(16) 0.075(11) -0.037(11) -0.006(8) -0.027(9) C44 0.057(10) 0.046(11) 0.125(17) -0.030(11) -0.022(11) 0.003(9) C73 0.098(13) 0.063(12) 0.054(9) -0.026(9) -0.053(10) 0.013(10) C72 0.075(10) 0.056(11) 0.047(9) 0.011(8) -0.016(8) -0.022(9) C71 0.068(10) 0.050(11) 0.058(9) -0.005(8) -0.018(8) -0.007(9) C74 0.073(12) 0.085(15) 0.133(17) -0.006(13) -0.041(12) -0.037(11) C75 0.047(11) 0.11(2) 0.17(2) -0.010(17) -0.050(14) -0.010(12) O9 0.051(6) 0.060(8) 0.060(6) -0.013(6) -0.027(5) -0.004(5) C76 0.106(19) 0.16(3) 0.20(3) -0.07(2) -0.002(19) -0.08(2) C77 0.097(19) 0.21(4) 0.20(3) -0.12(3) -0.007(19) 0.02(2) C4 0.053(8) 0.051(10) 0.039(8) -0.002(7) 0.007(7) -0.014(8) C3 0.042(8) 0.067(12) 0.054(10) 0.002(9) -0.008(7) -0.007(8) C5 0.047(9) 0.057(12) 0.076(11) 0.007(9) 0.012(8) -0.019(8) C12 0.103(15) 0.085(16) 0.063(11) -0.029(10) -0.047(11) 0.035(13) C11 0.064(11) 0.090(16) 0.050(10) -0.008(10) -0.027(8) 0.003(11) C9 0.069(11) 0.067(14) 0.081(12) -0.020(11) -0.027(10) 0.008(11) C8 0.074(13) 0.087(16) 0.108(16) -0.009(13) -0.020(12) -0.042(13) C10 0.101(16) 0.057(14) 0.084(13) -0.024(11) -0.040(12) 0.006(13) C6 0.060(10) 0.098(17) 0.070(12) -0.004(12) -0.009(9) -0.024(11) C7 0.103(17) 0.093(19) 0.091(15) 0.011(14) 0.000(12) -0.049(15) C19 0.087(15) 0.082(17) 0.138(19) 0.030(15) -0.043(14) -0.064(14) C18 0.053(10) 0.103(17) 0.055(10) 0.015(10) -0.011(8) -0.022(11) C16 0.046(9) 0.076(13) 0.044(9) -0.003(9) -0.014(7) -0.005(9) C21 0.062(11) 0.080(16) 0.093(14) -0.019(12) -0.007(10) -0.020(11) C14 0.020(9) 0.25(4) 0.100(17) -0.08(2) -0.005(10) 0.032(15) C15 0.034(9) 0.17(2) 0.070(11) -0.053(13) -0.013(8) 0.000(12) C17 0.047(9) 0.100(17) 0.045(9) 0.009(10) -0.002(7) -0.014(10) C20 0.107(17) 0.063(15) 0.095(15) 0.021(12) -0.021(13) -0.020(14) C13 0.030(10) 0.20(3) 0.072(13) -0.076(16) -0.006(9) 0.023(13) N4 0.061(8) 0.079(11) 0.059(9) -0.024(8) -0.017(7) 0.008(8) O4 0.094(10) 0.066(10) 0.140(13) -0.013(9) -0.027(9) -0.006(9) C22 0.076(12) 0.048(12) 0.085(13) -0.015(10) -0.012(10) -0.023(10) O3 0.075(8) 0.141(14) 0.094(10) 0.013(9) 0.010(7) -0.042(9) N3 0.108(12) 0.141(17) 0.068(10) -0.026(10) -0.057(10) -0.014(12) N12 0.040(7) 0.065(10) 0.055(7) -0.020(7) -0.011(6) -0.024(7) N10 0.051(7) 0.065(10) 0.044(7) -0.008(7) -0.016(6) 0.003(8) N11 0.032(6) 0.081(11) 0.043(7) 0.002(7) -0.002(5) -0.012(7) N9 0.038(6) 0.067(10) 0.061(8) -0.013(7) -0.004(6) -0.023(7) O1W 0.044(5) 0.090(9) 0.043(5) -0.016(5) -0.014(4) -0.015(5) O2W 0.116(15) 0.112(18) 0.64(6) -0.08(3) 0.09(3) -0.051(14) O3W 0.080(8) 0.102(11) 0.075(8) -0.041(7) 0.005(6) -0.016(8) O5W 0.110(16) 0.39(5) 0.50(5) 0.18(4) -0.10(2) -0.15(2) O6W 0.21(3) 0.24(3) 0.36(4) -0.15(3) 0.04(3) -0.01(2) O4W 0.34(4) 0.41(6) 0.44(5) -0.30(5) 0.20(4) -0.21(4) O7W 0.78(11) 0.33(5) 0.20(3) 0.00(3) -0.15(5) -0.19(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N7 1.870(12) . ? Fe1 N6 1.900(12) . ? Fe1 C1 1.953(19) . ? Fe1 C2 1.966(17) . ? Fe1 N8 1.986(11) . ? Fe1 N5 2.000(13) . ? Mn1 O6 1.856(10) . ? Mn1 O5 1.879(10) . ? Mn1 N14 1.968(13) . ? Mn1 N13 2.020(12) . ? Mn1 O1W 2.229(11) . ? Mn1 N1 2.252(16) . ? Mn2 O7 1.874(12) . ? Mn2 O8 1.878(9) . ? Mn2 N16 2.024(12) . ? Mn2 N15 2.037(13) . ? Mn2 N2 2.154(14) . ? Mn2 O9 2.291(11) . ? Br4 C61 1.84(2) . ? Br2 C54 1.85(2) . ? Br1 C44 1.899(16) . ? Br3 C75 1.916(19) . ? N8 C23 1.334(17) . ? N8 C27 1.340(17) . ? N5 C36 1.350(17) . ? N5 C40 1.355(18) . ? O5 C57 1.33(2) . ? O6 C41 1.351(15) . ? C52 C53 1.39(2) . ? C52 C57 1.40(2) . ? C52 C51 1.40(2) . ? O7 C58 1.330(18) . ? N6 C34 1.388(18) . ? N6 C35 1.386(19) . ? N16 C64 1.230(18) . ? N16 C73 1.486(18) . ? N7 C28 1.348(18) . ? N7 C29 1.422(18) . ? C47 N14 1.330(16) . ? C47 C46 1.392(19) . ? C47 H47A 0.9300 . ? O1W H1WB 0.8565 . ? O1W H1WA 0.8572 . ? C61 C62 1.40(2) . ? C61 C60 1.41(2) . ? C51 N13 1.28(2) . ? C51 H51A 0.9300 . ? O8 C66 1.305(18) . ? C56 C55 1.36(2) . ? C56 C57 1.38(2) . ? C56 H56A 0.9300 . ? C30 C29 1.40(2) . ? C30 C31 1.42(2) . ? C30 H30 0.9300 . ? C48 N14 1.46(2) . ? C48 C49 1.55(2) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C2 N2 1.144(17) . ? N13 C50 1.48(2) . ? C63 C62 1.40(2) . ? C63 C58 1.394(19) . ? C63 C64 1.43(2) . ? N15 C70 1.269(19) . ? N15 C71 1.497(17) . ? C62 H62A 0.9300 . ? C41 C42 1.37(2) . ? C41 C46 1.422(19) . ? C39 C38 1.37(2) . ? C39 C40 1.37(2) . ? C39 H39A 0.9300 . ? N1 C1 1.123(18) . ? C27 C26 1.421(19) . ? C27 C28 1.479(19) . ? C60 C59 1.37(3) . ? C60 H60A 0.9300 . ? O1 C28 1.228(16) . ? C53 C54 1.34(3) . ? C53 H53A 0.9300 . ? C33 C32 1.31(2) . ? C33 C34 1.39(2) . ? C33 H33A 0.9300 . ? C36 C37 1.42(2) . ? C36 C35 1.445(19) . ? C35 O2 1.208(16) . ? C64 H64A 0.9300 . ? C58 C59 1.39(2) . ? C37 C38 1.38(2) . ? C37 H37A 0.9300 . ? C66 C67 1.367(19) . ? C66 C65 1.37(2) . ? C54 C55 1.42(2) . ? C46 C45 1.450(19) . ? C34 C29 1.39(2) . ? C59 H59A 0.9300 . ? C43 C44 1.41(2) . ? C43 C42 1.41(2) . ? C43 H43 0.9300 . ? C32 C31 1.38(3) . ? C32 H32A 0.9300 . ? C40 H40A 0.9300 . ? C65 C74 1.41(2) . ? C65 C70 1.48(2) . ? C26 C25 1.35(2) . ? C26 H26A 0.9300 . ? C25 C24 1.43(2) . ? C25 H25A 0.9300 . ? C67 C68 1.40(2) . ? C67 H67A 0.9300 . ? C24 C23 1.37(2) . ? C24 H24A 0.9300 . ? C31 H31A 0.9300 . ? C55 H55A 0.9300 . ? C38 H38A 0.9300 . ? C49 C50 1.50(2) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C68 C75 1.33(3) . ? C68 H68A 0.9300 . ? C23 H23A 0.9300 . ? C42 H42A 0.9300 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C70 H70A 0.9300 . ? C45 C44 1.40(2) . ? C45 H45A 0.9300 . ? C73 C72 1.51(2) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C72 C71 1.50(2) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C74 C75 1.45(3) . ? C74 H74 0.9300 . ? O9 C76 1.40(3) . ? O9 H9A 0.8673 . ? C76 C77 1.51(3) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C4 N4 1.149(17) . ? C4 Fe2 1.935(16) . ? C3 N3 1.13(2) . ? C3 Fe2 1.939(18) . ? C5 N12 1.356(19) . ? C5 C6 1.36(2) . ? C5 H5A 0.9300 . ? C12 C11 1.38(3) . ? C12 C13 1.41(3) . ? C12 H12A 0.9300 . ? C11 C16 1.39(2) . ? C11 N11 1.44(2) . ? C9 N12 1.33(2) . ? C9 C8 1.38(3) . ? C9 C10 1.51(3) . ? C8 C7 1.38(3) . ? C8 H8A 0.9300 . ? C10 O4 1.21(2) . ? C10 N11 1.36(2) . ? C6 C7 1.33(3) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C19 C18 1.36(3) . ? C19 C20 1.39(3) . ? C19 H19A 0.9300 . ? C18 N9 1.400(19) . ? C18 C17 1.53(3) . ? C16 N10 1.39(2) . ? C16 C15 1.43(2) . ? C21 C22 1.32(2) . ? C21 C20 1.35(2) . ? C21 H21A 0.9300 . ? C14 C13 1.32(4) . ? C14 C15 1.41(3) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C17 O3 1.260(18) . ? C17 N10 1.29(2) . ? C20 H20A 0.9300 . ? C13 H13A 0.9300 . ? Fe2 N11 1.850(15) . ? Fe2 N10 1.897(13) . ? Fe2 N9 1.982(14) . ? Fe2 N12 1.985(11) . ? C22 N9 1.32(2) . ? C22 H22A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Fe1 N6 83.9(5) . . ? N7 Fe1 C1 91.0(6) . . ? N6 Fe1 C1 96.3(6) . . ? N7 Fe1 C2 98.2(5) . . ? N6 Fe1 C2 92.1(5) . . ? C1 Fe1 C2 168.2(5) . . ? N7 Fe1 N8 81.3(5) . . ? N6 Fe1 N8 164.9(5) . . ? C1 Fe1 N8 87.1(5) . . ? C2 Fe1 N8 87.0(5) . . ? N7 Fe1 N5 165.2(5) . . ? N6 Fe1 N5 81.8(5) . . ? C1 Fe1 N5 86.9(6) . . ? C2 Fe1 N5 86.0(5) . . ? N8 Fe1 N5 113.1(5) . . ? O6 Mn1 O5 90.6(4) . . ? O6 Mn1 N14 89.8(4) . . ? O5 Mn1 N14 176.4(5) . . ? O6 Mn1 N13 177.5(5) . . ? O5 Mn1 N13 88.7(5) . . ? N14 Mn1 N13 90.8(5) . . ? O6 Mn1 O1W 89.3(4) . . ? O5 Mn1 O1W 86.2(4) . . ? N14 Mn1 O1W 90.3(4) . . ? N13 Mn1 O1W 88.3(4) . . ? O6 Mn1 N1 93.3(4) . . ? O5 Mn1 N1 94.5(5) . . ? N14 Mn1 N1 89.1(5) . . ? N13 Mn1 N1 89.2(5) . . ? O1W Mn1 N1 177.4(4) . . ? O7 Mn2 O8 88.5(5) . . ? O7 Mn2 N16 87.7(5) . . ? O8 Mn2 N16 173.4(5) . . ? O7 Mn2 N15 176.3(5) . . ? O8 Mn2 N15 91.1(5) . . ? N16 Mn2 N15 92.3(5) . . ? O7 Mn2 N2 96.3(5) . . ? O8 Mn2 N2 96.0(5) . . ? N16 Mn2 N2 89.8(5) . . ? N15 Mn2 N2 87.4(5) . . ? O7 Mn2 O9 91.2(4) . . ? O8 Mn2 O9 88.7(4) . . ? N16 Mn2 O9 86.0(4) . . ? N15 Mn2 O9 85.2(5) . . ? N2 Mn2 O9 171.3(4) . . ? C23 N8 C27 119.4(12) . . ? C23 N8 Fe1 128.3(9) . . ? C27 N8 Fe1 112.3(9) . . ? C36 N5 C40 119.2(13) . . ? C36 N5 Fe1 111.2(9) . . ? C40 N5 Fe1 129.6(10) . . ? C57 O5 Mn1 124.7(9) . . ? C41 O6 Mn1 126.4(9) . . ? C53 C52 C57 117.1(15) . . ? C53 C52 C51 119.5(14) . . ? C57 C52 C51 123.4(15) . . ? C58 O7 Mn2 123.8(9) . . ? C34 N6 C35 126.6(12) . . ? C34 N6 Fe1 114.7(10) . . ? C35 N6 Fe1 118.2(9) . . ? C64 N16 C73 119.8(13) . . ? C64 N16 Mn2 120.5(10) . . ? C73 N16 Mn2 119.7(10) . . ? C28 N7 C29 125.5(13) . . ? C28 N7 Fe1 120.1(10) . . ? C29 N7 Fe1 114.1(10) . . ? N14 C47 C46 125.2(12) . . ? N14 C47 H47A 117.4 . . ? C46 C47 H47A 117.4 . . ? Mn1 O1W H1WB 110.2 . . ? Mn1 O1W H1WA 109.8 . . ? H1WB O1W H1WA 108.6 . . ? C62 C61 C60 116.6(18) . . ? C62 C61 Br4 123.8(13) . . ? C60 C61 Br4 119.7(15) . . ? N13 C51 C52 128.1(14) . . ? N13 C51 H51A 115.9 . . ? C52 C51 H51A 115.9 . . ? C66 O8 Mn2 127.3(10) . . ? C55 C56 C57 117.5(16) . . ? C55 C56 H56A 121.3 . . ? C57 C56 H56A 121.3 . . ? C29 C30 C31 117.2(17) . . ? C29 C30 H30 121.4 . . ? C31 C30 H30 121.4 . . ? N14 C48 C49 111.5(14) . . ? N14 C48 H48A 109.3 . . ? C49 C48 H48A 109.3 . . ? N14 C48 H48B 109.3 . . ? C49 C48 H48B 109.3 . . ? H48A C48 H48B 108.0 . . ? N2 C2 Fe1 175.1(12) . . ? C47 N14 C48 113.5(12) . . ? C47 N14 Mn1 121.9(9) . . ? C48 N14 Mn1 124.5(9) . . ? C51 N13 C50 119.3(14) . . ? C51 N13 Mn1 119.7(11) . . ? C50 N13 Mn1 121.0(11) . . ? C62 C63 C58 119.4(14) . . ? C62 C63 C64 119.1(13) . . ? C58 C63 C64 121.3(15) . . ? O5 C57 C56 119.2(15) . . ? O5 C57 C52 118.9(15) . . ? C56 C57 C52 121.7(17) . . ? C2 N2 Mn2 162.7(12) . . ? C70 N15 C71 117.5(14) . . ? C70 N15 Mn2 121.5(11) . . ? C71 N15 Mn2 120.9(9) . . ? C63 C62 C61 121.8(14) . . ? C63 C62 H62A 119.1 . . ? C61 C62 H62A 119.1 . . ? O6 C41 C42 120.4(14) . . ? O6 C41 C46 118.2(12) . . ? C42 C41 C46 121.2(13) . . ? C38 C39 C40 119.9(16) . . ? C38 C39 H39A 120.0 . . ? C40 C39 H39A 120.0 . . ? C1 N1 Mn1 166.6(13) . . ? N8 C27 C26 120.9(13) . . ? N8 C27 C28 116.2(12) . . ? C26 C27 C28 122.4(13) . . ? C59 C60 C61 121.9(17) . . ? C59 C60 H60A 119.1 . . ? C61 C60 H60A 119.1 . . ? C54 C53 C52 124.4(17) . . ? C54 C53 H53A 117.8 . . ? C52 C53 H53A 117.8 . . ? C32 C33 C34 122.2(18) . . ? C32 C33 H33A 118.9 . . ? C34 C33 H33A 118.9 . . ? N5 C36 C37 121.0(13) . . ? N5 C36 C35 118.7(13) . . ? C37 C36 C35 120.3(13) . . ? O1 C28 N7 129.5(13) . . ? O1 C28 C27 121.3(13) . . ? N7 C28 C27 109.1(12) . . ? O2 C35 N6 125.1(14) . . ? O2 C35 C36 125.7(15) . . ? N6 C35 C36 109.2(12) . . ? N16 C64 C63 128.1(14) . . ? N16 C64 H64A 116.0 . . ? C63 C64 H64A 116.0 . . ? O7 C58 C59 120.7(15) . . ? O7 C58 C63 119.8(14) . . ? C59 C58 C63 119.3(16) . . ? C38 C37 C36 118.2(14) . . ? C38 C37 H37A 120.9 . . ? C36 C37 H37A 120.9 . . ? O8 C66 C67 118.9(15) . . ? O8 C66 C65 121.3(13) . . ? C67 C66 C65 119.7(15) . . ? C53 C54 C55 116(2) . . ? C53 C54 Br2 124.5(15) . . ? C55 C54 Br2 119.7(18) . . ? C47 C46 C41 124.2(12) . . ? C47 C46 C45 117.4(12) . . ? C41 C46 C45 118.0(13) . . ? N6 C34 C29 113.3(13) . . ? N6 C34 C33 128.0(16) . . ? C29 C34 C33 118.5(15) . . ? C60 C59 C58 120.3(16) . . ? C60 C59 H59A 119.9 . . ? C58 C59 H59A 119.9 . . ? C44 C43 C42 114.8(15) . . ? C44 C43 H43 122.6 . . ? C42 C43 H43 122.6 . . ? C33 C32 C31 120.7(17) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? N5 C40 C39 121.7(15) . . ? N5 C40 H40A 119.2 . . ? C39 C40 H40A 119.2 . . ? C66 C65 C74 120.2(16) . . ? C66 C65 C70 125.0(14) . . ? C74 C65 C70 114.3(17) . . ? C25 C26 C27 118.9(14) . . ? C25 C26 H26A 120.6 . . ? C27 C26 H26A 120.6 . . ? C26 C25 C24 120.6(15) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C66 C67 C68 123.3(17) . . ? C66 C67 H67A 118.3 . . ? C68 C67 H67A 118.3 . . ? C23 C24 C25 116.2(15) . . ? C23 C24 H24A 121.9 . . ? C25 C24 H24A 121.9 . . ? C32 C31 C30 120.5(17) . . ? C32 C31 H31A 119.8 . . ? C30 C31 H31A 119.8 . . ? C56 C55 C54 123.5(19) . . ? C56 C55 H55A 118.3 . . ? C54 C55 H55A 118.3 . . ? C39 C38 C37 120.0(16) . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C34 C29 C30 120.7(14) . . ? C34 C29 N7 113.8(13) . . ? C30 C29 N7 125.4(16) . . ? C50 C49 C48 110.9(11) . . ? C50 C49 H49A 109.5 . . ? C48 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 108.1 . . ? N1 C1 Fe1 177.4(15) . . ? C75 C68 C67 116.6(16) . . ? C75 C68 H68A 121.7 . . ? C67 C68 H68A 121.7 . . ? N8 C23 C24 124.0(14) . . ? N8 C23 H23A 118.0 . . ? C24 C23 H23A 118.0 . . ? C41 C42 C43 123.1(16) . . ? C41 C42 H42A 118.4 . . ? C43 C42 H42A 118.4 . . ? N13 C50 C49 112.8(12) . . ? N13 C50 H50A 109.0 . . ? C49 C50 H50A 109.0 . . ? N13 C50 H50B 109.0 . . ? C49 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? N15 C70 C65 124.4(16) . . ? N15 C70 H70A 117.8 . . ? C65 C70 H70A 117.8 . . ? C44 C45 C46 117.2(15) . . ? C44 C45 H45A 121.4 . . ? C46 C45 H45A 121.4 . . ? C45 C44 C43 125.6(15) . . ? C45 C44 Br1 117.0(14) . . ? C43 C44 Br1 117.3(14) . . ? N16 C73 C72 112.9(12) . . ? N16 C73 H73A 109.0 . . ? C72 C73 H73A 109.0 . . ? N16 C73 H73B 109.0 . . ? C72 C73 H73B 109.0 . . ? H73A C73 H73B 107.8 . . ? C73 C72 C71 113.5(13) . . ? C73 C72 H72A 108.9 . . ? C71 C72 H72A 108.9 . . ? C73 C72 H72B 108.9 . . ? C71 C72 H72B 108.9 . . ? H72A C72 H72B 107.7 . . ? N15 C71 C72 113.1(13) . . ? N15 C71 H71A 109.0 . . ? C72 C71 H71A 109.0 . . ? N15 C71 H71B 109.0 . . ? C72 C71 H71B 109.0 . . ? H71A C71 H71B 107.8 . . ? C65 C74 C75 116.2(18) . . ? C65 C74 H74 121.9 . . ? C75 C74 H74 121.9 . . ? C68 C75 C74 123.7(17) . . ? C68 C75 Br3 120.4(15) . . ? C74 C75 Br3 115.8(17) . . ? C76 O9 Mn2 122.2(14) . . ? C76 O9 H9A 111.5 . . ? Mn2 O9 H9A 110.9 . . ? O9 C76 C77 118(2) . . ? O9 C76 H76A 107.7 . . ? C77 C76 H76A 107.7 . . ? O9 C76 H76B 107.7 . . ? C77 C76 H76B 107.7 . . ? H76A C76 H76B 107.1 . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? N4 C4 Fe2 177.9(13) . . ? N3 C3 Fe2 175.9(17) . . ? N12 C5 C6 125.0(18) . . ? N12 C5 H5A 117.5 . . ? C6 C5 H5A 117.5 . . ? C11 C12 C13 113(2) . . ? C11 C12 H12A 123.6 . . ? C13 C12 H12A 123.6 . . ? C12 C11 C16 124.8(18) . . ? C12 C11 N11 125.9(19) . . ? C16 C11 N11 109.2(17) . . ? N12 C9 C8 124.9(18) . . ? N12 C9 C10 114.3(18) . . ? C8 C9 C10 121(2) . . ? C9 C8 C7 116(2) . . ? C9 C8 H8A 122.0 . . ? C7 C8 H8A 122.0 . . ? O4 C10 N11 128(2) . . ? O4 C10 C9 122(2) . . ? N11 C10 C9 109.5(18) . . ? C7 C6 C5 117.0(19) . . ? C7 C6 H6A 121.5 . . ? C5 C6 H6A 121.5 . . ? C6 C7 C8 122(2) . . ? C6 C7 H7A 118.8 . . ? C8 C7 H7A 118.8 . . ? C18 C19 C20 118.2(19) . . ? C18 C19 H19A 120.9 . . ? C20 C19 H19A 120.9 . . ? C19 C18 N9 123.5(19) . . ? C19 C18 C17 127.4(18) . . ? N9 C18 C17 109.1(17) . . ? N10 C16 C11 117.1(15) . . ? N10 C16 C15 125.9(18) . . ? C11 C16 C15 116.9(19) . . ? C22 C21 C20 122(2) . . ? C22 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? C13 C14 C15 116.3(18) . . ? C13 C14 H14A 121.9 . . ? C15 C14 H14A 121.9 . . ? C14 C15 C16 121(2) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? O3 C17 N10 126.8(19) . . ? O3 C17 C18 117.2(18) . . ? N10 C17 C18 116.0(15) . . ? C21 C20 C19 118(2) . . ? C21 C20 H20A 121.2 . . ? C19 C20 H20A 121.2 . . ? C14 C13 C12 128(2) . . ? C14 C13 H13A 115.9 . . ? C12 C13 H13A 115.9 . . ? N11 Fe2 N10 83.4(6) . . ? N11 Fe2 C4 95.5(6) . . ? N10 Fe2 C4 93.0(5) . . ? N11 Fe2 C3 94.7(6) . . ? N10 Fe2 C3 94.6(5) . . ? C4 Fe2 C3 167.9(6) . . ? N11 Fe2 N9 165.6(5) . . ? N10 Fe2 N9 82.4(6) . . ? C4 Fe2 N9 87.4(6) . . ? C3 Fe2 N9 84.3(6) . . ? N11 Fe2 N12 82.0(5) . . ? N10 Fe2 N12 165.4(6) . . ? C4 Fe2 N12 89.1(5) . . ? C3 Fe2 N12 85.9(5) . . ? N9 Fe2 N12 112.2(5) . . ? C21 C22 N9 124.6(18) . . ? C21 C22 H22A 117.7 . . ? N9 C22 H22A 117.7 . . ? C9 N12 C5 114.7(14) . . ? C9 N12 Fe2 114.0(12) . . ? C5 N12 Fe2 131.1(12) . . ? C17 N10 C16 128.9(15) . . ? C17 N10 Fe2 117.9(12) . . ? C16 N10 Fe2 113.1(11) . . ? C10 N11 C11 122.7(17) . . ? C10 N11 Fe2 120.0(12) . . ? C11 N11 Fe2 117.0(12) . . ? C22 N9 C18 114.2(16) . . ? C22 N9 Fe2 131.3(11) . . ? C18 N9 Fe2 114.5(12) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WB N3 0.856 1.867 2.724(19) 179.36 2_756 O1W H1WA O3W 0.857 2.044 2.789(16) 145.14 . O9 H9A N4 0.867 1.989 2.835(17) 164.07 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.925 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.117 #===End # Attachment 'dalton-rev3.cif' #=================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 699870' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C38 H32 Fe Mn N8 O5), H2 O, 2(O), O' _chemical_formula_sum 'C38 H34 Fe Mn N8 O6' _chemical_formula_weight 809.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 23.065(3) _cell_length_b 23.065(3) _cell_length_c 15.363(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8174(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 22.45 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.868 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details 'North, et al., 1968' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9187 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4545 _reflns_number_gt 3966 _reflns_threshold_expression i>2\s(I) _computing_data_collection 'XSCANS (Bruker, 1997)' _computing_cell_refinement XSCANS _computing_data_reduction 'SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics xp _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1400P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_number_reflns 4545 _refine_ls_number_parameters 505 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1735 _refine_ls_wR_factor_gt 0.1640 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.187 _refine_ls_shift/su_mean 0.009 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 0.317261(18) 0.055274(17) 0.04655(3) 0.05068(11) Uani 1 1 d . . . Mn1 Mn 0.244460(19) 0.267532(19) -0.02962(3) 0.05046(12) Uani 1 1 d . . . N4 N 0.32223(13) 0.04703(11) -0.07686(19) 0.0589(8) Uani 1 1 d . . . O3 O 0.31472(9) 0.30446(10) -0.05698(16) 0.0604(6) Uani 1 1 d . . . N8 N 0.16500(11) 0.23697(11) 0.00254(18) 0.0547(7) Uani 1 1 d . . . N5 N 0.23875(12) 0.03450(11) 0.0305(2) 0.0674(9) Uani 1 1 d . . . N7 N 0.24138(12) 0.23256(12) -0.15223(19) 0.0589(7) Uani 1 1 d . . . N6 N 0.29160(11) 0.05826(12) 0.1721(2) 0.0580(8) Uani 1 1 d . . . C2 C 0.33760(13) -0.02513(14) 0.0688(2) 0.0542(8) Uani 1 1 d . . . O4 O 0.24834(9) 0.30450(10) 0.08015(16) 0.0615(6) Uani 1 1 d . . . N3 N 0.40237(11) 0.06974(11) 0.03473(18) 0.0517(7) Uani 1 1 d . . . C11 C 0.20671(15) 0.02027(15) 0.1025(3) 0.0736(12) Uani 1 1 d . . . O5 O 0.19612(9) 0.34640(9) -0.08721(18) 0.0624(7) Uani 1 1 d . . . C1 C 0.30041(13) 0.13899(13) 0.0340(2) 0.0538(8) Uani 1 1 d . . . C26 C 0.14186(16) 0.18362(14) -0.0388(3) 0.0661(10) Uani 1 1 d . . . H26A H 0.1634 0.1504 -0.0176 0.079 Uiso 1 1 calc R . . H26B H 0.1017 0.1786 -0.0219 0.079 Uiso 1 1 calc R . . N1 N 0.28664(12) 0.18538(12) 0.0187(2) 0.0645(8) Uani 1 1 d . . . C10 C 0.22252(13) 0.03106(14) -0.0605(3) 0.0735(11) Uani 1 1 d D . . C12 C 0.23850(16) 0.03398(15) 0.1818(3) 0.0689(11) Uani 1 1 d . . . O1 O 0.15752(12) 0.00127(13) 0.1030(3) 0.0999(12) Uani 1 1 d . . . O2 O 0.38429(15) 0.05033(14) -0.19385(17) 0.0900(10) Uani 1 1 d . . . C20 C 0.36645(19) 0.37174(19) -0.2936(3) 0.0814(13) Uani 1 1 d . . . H20A H 0.3792 0.3872 -0.3462 0.098 Uiso 1 1 calc R . . C3 C 0.44251(15) 0.07804(17) 0.0946(3) 0.0664(10) Uani 1 1 d . . . H3A H 0.4311 0.0798 0.1526 0.080 Uiso 1 1 calc R . . N2 N 0.34818(13) -0.07434(12) 0.0796(2) 0.0620(8) Uani 1 1 d . . . C29 C 0.10289(16) 0.34275(16) 0.1538(2) 0.0629(10) Uani 1 1 d . . . H29A H 0.0646 0.3305 0.1490 0.075 Uiso 1 1 calc R . . C7 C 0.41985(15) 0.06598(14) -0.0494(2) 0.0589(9) Uani 1 1 d . . . C28 C 0.14720(13) 0.31289(14) 0.1088(2) 0.0523(8) Uani 1 1 d . . . C33 C 0.20481(14) 0.33215(14) 0.1181(2) 0.0535(8) Uani 1 1 d . . . C9 C 0.26871(15) 0.03735(14) -0.1171(2) 0.0673(10) Uani 1 1 d D . . C24 C 0.20443(19) 0.18150(17) -0.1694(3) 0.0772(12) Uani 1 1 d . . . H24A H 0.2021 0.1757 -0.2319 0.093 Uiso 1 1 calc R . . H24B H 0.2230 0.1476 -0.1446 0.093 Uiso 1 1 calc R . . C17 C 0.32908(14) 0.32643(15) -0.1336(2) 0.0594(9) Uani 1 1 d . . . C8 C 0.37288(17) 0.05352(15) -0.1152(2) 0.0619(10) Uani 1 1 d . . . C16 C 0.31818(17) 0.07710(17) 0.2415(3) 0.0693(11) Uani 1 1 d . . . H16A H 0.3537 0.0957 0.2348 0.083 Uiso 1 1 calc R . . C18 C 0.36648(16) 0.37326(15) -0.1366(3) 0.0667(11) Uani 1 1 d . . . H18A H 0.3803 0.3903 -0.0858 0.080 Uiso 1 1 calc R . . C23 C 0.26948(16) 0.25467(16) -0.2155(2) 0.0634(10) Uani 1 1 d . . . H23A H 0.2636 0.2379 -0.2698 0.076 Uiso 1 1 calc R . . C5 C 0.51798(16) 0.0811(2) -0.0100(3) 0.0806(13) Uani 1 1 d . . . H5A H 0.5570 0.0848 -0.0244 0.097 Uiso 1 1 calc R . . C32 C 0.21527(17) 0.37941(18) 0.1695(2) 0.0687(11) Uani 1 1 d . . . H32A H 0.2534 0.3919 0.1757 0.082 Uiso 1 1 calc R . . C27 C 0.13225(14) 0.26363(14) 0.0589(2) 0.0589(9) Uani 1 1 d . . . H27A H 0.0952 0.2487 0.0671 0.071 Uiso 1 1 calc R . . C4 C 0.50034(16) 0.0842(2) 0.0754(3) 0.0789(13) Uani 1 1 d . . . H4A H 0.5272 0.0903 0.1196 0.095 Uiso 1 1 calc R . . C14 C 0.2428(2) 0.0440(2) 0.3345(3) 0.0999(15) Uani 1 1 d . . . H14A H 0.2267 0.0387 0.3894 0.120 Uiso 1 1 calc R . . C30 C 0.11633(18) 0.39011(19) 0.2048(3) 0.0743(12) Uani 1 1 d . . . H30A H 0.0870 0.4094 0.2345 0.089 Uiso 1 1 calc R . . C25 C 0.14569(17) 0.18553(17) -0.1348(3) 0.0703(11) Uani 1 1 d . . . H25A H 0.1229 0.1539 -0.1585 0.084 Uiso 1 1 calc R . . H25B H 0.1285 0.2215 -0.1550 0.084 Uiso 1 1 calc R . . C6 C 0.47703(17) 0.07236(17) -0.0736(3) 0.0737(11) Uani 1 1 d . . . H6A H 0.4877 0.0708 -0.1319 0.088 Uiso 1 1 calc R . . C19 C 0.3831(2) 0.39440(19) -0.2189(3) 0.0886(15) Uani 1 1 d . . . H19A H 0.4074 0.4265 -0.2207 0.106 Uiso 1 1 calc R . . C15 C 0.2960(2) 0.0706(2) 0.3247(3) 0.0919(14) Uani 1 1 d . . . H15A H 0.3164 0.0839 0.3729 0.110 Uiso 1 1 calc R . . C22 C 0.30957(16) 0.30299(15) -0.2123(3) 0.0612(10) Uani 1 1 d . . . C21 C 0.33040(17) 0.32539(18) -0.2922(3) 0.0735(11) Uani 1 1 d . . . H21A H 0.3192 0.3081 -0.3442 0.088 Uiso 1 1 calc R . . C13 C 0.21498(18) 0.02591(19) 0.2628(3) 0.0880(14) Uani 1 1 d . . . H13A H 0.1792 0.0077 0.2681 0.106 Uiso 1 1 calc R . . C31 C 0.17269(19) 0.40918(18) 0.2123(3) 0.0745(12) Uani 1 1 d . . . H31A H 0.1816 0.4416 0.2457 0.089 Uiso 1 1 calc R . . C34 C 0.25761(18) 0.03448(19) -0.2049(2) 0.0905(14) Uani 1 1 d D . . H34 H 0.2870 0.0383 -0.2460 0.109 Uiso 1 1 calc R . . C37 C 0.16604(16) 0.02363(17) -0.0896(3) 0.0888(14) Uani 1 1 d D . . H37A H 0.1363 0.0209 -0.0490 0.107 Uiso 1 1 calc R . . C36 C 0.1531(2) 0.0202(2) -0.1745(3) 0.1180(19) Uani 1 1 d D . . H36A H 0.1153 0.0147 -0.1943 0.142 Uiso 1 1 calc R . . C35 C 0.19890(17) 0.0253(2) -0.2299(3) 0.1202(17) Uani 1 1 d D . . H35A H 0.1912 0.0226 -0.2892 0.144 Uiso 1 1 calc R . . C38 C 0.2133(2) 0.4015(2) -0.0884(5) 0.118(2) Uani 1 1 d . . . H38A H 0.1842 0.4248 -0.1162 0.176 Uiso 1 1 calc R . . H38B H 0.2490 0.4047 -0.1199 0.176 Uiso 1 1 calc R . . H38C H 0.2189 0.4149 -0.0298 0.176 Uiso 1 1 calc R . . O3W O 0.0504(5) -0.0095(5) 0.1981(9) 0.090(4) Uani 0.25 1 d P . . O2W O 0.3746(4) 0.3384(9) 0.1000(6) 0.304(6) Uani 0.50 1 d P . . O1W O 0.0878(11) -0.0478(9) 0.4034(17) 0.326(13) Uani 0.25 1 d P . . H400 H 0.0794 -0.0380 0.3516 0.489 Uiso 0.25 1 d PR . . H401 H 0.0845 -0.0170 0.4333 0.489 Uiso 0.25 1 d PR . . H5 H 0.1576 0.3463 -0.0900 0.489 Uiso 1 1 d 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 0.04471(19) 0.04111(18) 0.0662(2) 0.0025(2) -0.0071(2) 0.00311(17) Mn1 0.0479(2) 0.0437(2) 0.0598(2) -0.0019(2) -0.0070(2) 0.00275(18) N4 0.0681(16) 0.0451(13) 0.0634(15) 0.0016(13) -0.0118(14) 0.0035(13) O3 0.0480(10) 0.0693(13) 0.0637(13) 0.0014(12) -0.0037(11) -0.0060(11) N8 0.0511(12) 0.0467(12) 0.0662(15) 0.0067(13) -0.0097(12) -0.0007(11) N5 0.0534(13) 0.0446(12) 0.104(2) -0.0013(15) -0.0225(16) 0.0063(12) N7 0.0586(14) 0.0512(13) 0.0669(15) -0.0085(14) -0.0093(14) 0.0085(13) N6 0.0460(12) 0.0516(13) 0.0764(17) 0.0079(14) 0.0065(13) 0.0097(12) C2 0.0439(14) 0.0549(16) 0.0640(18) 0.0037(16) -0.0042(15) -0.0003(13) O4 0.0493(11) 0.0651(13) 0.0701(13) -0.0085(12) -0.0078(11) 0.0039(11) N3 0.0479(12) 0.0477(12) 0.0596(14) 0.0039(13) -0.0024(13) 0.0028(10) C11 0.0556(18) 0.0484(17) 0.117(3) 0.003(2) 0.012(2) 0.0048(15) O5 0.0490(11) 0.0470(11) 0.0913(16) 0.0073(12) -0.0018(12) 0.0047(10) C1 0.0453(13) 0.0490(14) 0.0670(18) 0.0028(16) -0.0112(15) 0.0044(12) C26 0.0655(18) 0.0462(15) 0.087(2) -0.0013(19) -0.013(2) -0.0089(15) N1 0.0637(15) 0.0464(13) 0.0835(18) -0.0014(15) -0.0130(16) 0.0067(12) C10 0.0698(19) 0.0417(14) 0.109(3) -0.0127(19) -0.038(2) 0.0076(15) C12 0.0544(18) 0.0527(17) 0.100(3) 0.0107(19) 0.009(2) 0.0094(16) O1 0.0534(13) 0.0757(16) 0.171(3) -0.013(2) 0.0054(19) -0.0127(13) O2 0.114(2) 0.095(2) 0.0609(14) 0.0032(16) 0.0003(16) -0.0187(19) C20 0.081(2) 0.087(3) 0.076(2) 0.017(2) 0.009(2) 0.010(2) C3 0.0609(18) 0.074(2) 0.064(2) 0.0041(19) -0.0044(18) 0.0095(18) N2 0.0647(15) 0.0465(13) 0.0748(17) 0.0039(14) -0.0002(16) 0.0033(13) C29 0.0577(17) 0.0622(18) 0.069(2) 0.0012(18) 0.0038(18) 0.0012(16) C7 0.0645(17) 0.0518(16) 0.0603(18) 0.0066(16) 0.0025(17) 0.0040(15) C28 0.0471(14) 0.0573(16) 0.0526(15) 0.0011(15) -0.0012(14) 0.0007(14) C33 0.0573(16) 0.0519(16) 0.0512(16) 0.0017(14) 0.0026(15) 0.0004(15) C9 0.0717(19) 0.0442(15) 0.086(2) -0.0065(17) -0.0347(19) 0.0047(16) C24 0.095(3) 0.0611(19) 0.076(2) -0.0170(19) -0.022(2) 0.006(2) C17 0.0453(15) 0.0561(17) 0.077(2) 0.0065(17) 0.0035(16) 0.0124(14) C8 0.079(2) 0.0490(16) 0.0578(17) 0.0014(16) -0.0049(18) 0.0019(17) C16 0.0596(18) 0.077(2) 0.071(2) 0.002(2) -0.0011(19) 0.0194(18) C18 0.066(2) 0.0518(17) 0.082(2) -0.0022(18) 0.007(2) 0.0021(17) C23 0.0655(19) 0.0668(19) 0.0580(17) -0.0062(16) -0.0100(17) 0.0168(18) C5 0.0460(17) 0.100(3) 0.095(3) 0.015(3) -0.0023(19) -0.0028(19) C32 0.069(2) 0.081(2) 0.0565(18) -0.0042(19) -0.0038(18) -0.0137(19) C27 0.0531(15) 0.0499(15) 0.074(2) 0.0064(17) -0.0083(17) 0.0014(14) C4 0.0387(14) 0.107(3) 0.091(2) -0.001(3) -0.009(2) -0.0049(19) C14 0.095(3) 0.097(3) 0.108(3) 0.039(3) 0.036(3) 0.041(2) C30 0.072(2) 0.082(2) 0.069(2) -0.003(2) 0.019(2) 0.011(2) C25 0.073(2) 0.0593(19) 0.079(2) -0.0099(19) -0.0229(19) -0.0070(18) C6 0.072(2) 0.068(2) 0.081(2) 0.012(2) 0.021(2) 0.0042(19) C19 0.078(2) 0.064(2) 0.123(4) 0.018(3) 0.024(3) 0.008(2) C15 0.084(2) 0.115(3) 0.077(2) 0.014(3) 0.009(2) 0.043(3) C22 0.0609(18) 0.0551(17) 0.0675(19) 0.0069(16) -0.0072(17) 0.0139(16) C21 0.074(2) 0.077(2) 0.069(2) 0.011(2) 0.0007(19) 0.020(2) C13 0.063(2) 0.078(2) 0.124(3) 0.031(3) 0.030(2) 0.018(2) C31 0.088(3) 0.068(2) 0.067(2) -0.0202(18) 0.016(2) -0.005(2) C34 0.110(3) 0.069(2) 0.093(3) -0.004(2) -0.043(2) 0.008(3) C37 0.073(2) 0.059(2) 0.135(4) -0.012(2) -0.034(3) -0.0021(19) C36 0.096(3) 0.091(3) 0.167(4) -0.031(3) -0.064(3) 0.001(3) C35 0.171(4) 0.064(2) 0.125(3) -0.007(2) -0.102(3) 0.006(3) C38 0.096(3) 0.068(3) 0.188(6) 0.002(3) 0.004(4) -0.001(3) O3W 0.061(5) 0.076(6) 0.132(10) -0.023(7) 0.011(7) -0.032(5) O2W 0.180(5) 0.574(18) 0.158(6) 0.123(10) -0.125(4) -0.233(8) O1W 0.256(19) 0.165(13) 0.56(4) 0.208(18) -0.24(2) -0.113(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 N5 1.889(3) . ? Fe1 N4 1.909(3) . ? Fe1 C2 1.943(3) . ? Fe1 C1 1.979(3) . ? Fe1 N3 1.999(2) . ? Fe1 N6 2.018(3) . ? Mn1 O3 1.878(2) . ? Mn1 O4 1.892(3) . ? Mn1 N8 2.025(3) . ? Mn1 N7 2.050(3) . ? Mn1 N1 2.256(3) . ? Mn1 O5 2.310(2) . ? N4 C8 1.317(5) . ? N4 C9 1.399(4) . ? O3 C17 1.323(4) . ? N8 C27 1.303(4) . ? N8 C26 1.484(4) . ? N5 C11 1.370(6) . ? N5 C10 1.449(5) . ? N7 C23 1.275(5) . ? N7 C24 1.478(5) . ? N6 C16 1.305(5) . ? N6 C12 1.355(4) . ? C2 N2 1.173(4) . ? O4 C33 1.325(4) . ? N3 C3 1.319(5) . ? N3 C7 1.357(5) . ? C11 O1 1.216(4) . ? C11 C12 1.457(6) . ? O5 C38 1.332(5) . ? O5 H5 0.8901 . ? C1 N1 1.141(4) . ? C26 C25 1.479(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C10 C9 1.384(5) . ? C10 C37 1.388(5) . ? C12 C13 1.370(6) . ? O2 C8 1.238(4) . ? C20 C19 1.318(7) . ? C20 C21 1.354(6) . ? C20 H20A 0.9300 . ? C3 C4 1.373(5) . ? C3 H3A 0.9300 . ? C29 C30 1.379(6) . ? C29 C28 1.414(5) . ? C29 H29A 0.9300 . ? C7 C6 1.378(5) . ? C7 C8 1.510(5) . ? C28 C33 1.408(5) . ? C28 C27 1.413(5) . ? C33 C32 1.368(5) . ? C9 C34 1.375(5) . ? C24 C25 1.458(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C17 C18 1.383(5) . ? C17 C22 1.400(5) . ? C16 C15 1.385(6) . ? C16 H16A 0.9300 . ? C18 C19 1.409(6) . ? C18 H18A 0.9300 . ? C23 C22 1.449(5) . ? C23 H23A 0.9300 . ? C5 C6 1.374(6) . ? C5 C4 1.375(6) . ? C5 H5A 0.9300 . ? C32 C31 1.367(6) . ? C32 H32A 0.9300 . ? C27 H27A 0.9300 . ? C4 H4A 0.9300 . ? C14 C13 1.342(7) . ? C14 C15 1.379(7) . ? C14 H14A 0.9300 . ? C30 C31 1.377(6) . ? C30 H30A 0.9300 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C6 H6A 0.9300 . ? C19 H19A 0.9300 . ? C15 H15A 0.9300 . ? C22 C21 1.415(6) . ? C21 H21A 0.9300 . ? C13 H13A 0.9300 . ? C31 H31A 0.9300 . ? C34 C35 1.423(5) . ? C34 H34 0.9300 . ? C37 C36 1.341(5) . ? C37 H37A 0.9300 . ? C36 C35 1.362(6) . ? C36 H36A 0.9300 . ? C35 H35A 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? O1W H400 0.8500 . ? O1W H401 0.8500 . ? 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 N5 Fe1 N4 84.43(14) . . ? N5 Fe1 C2 90.70(12) . . ? N4 Fe1 C2 93.76(13) . . ? N5 Fe1 C1 92.67(12) . . ? N4 Fe1 C1 90.72(13) . . ? C2 Fe1 C1 174.64(14) . . ? N5 Fe1 N3 166.29(13) . . ? N4 Fe1 N3 82.38(12) . . ? C2 Fe1 N3 86.46(12) . . ? C1 Fe1 N3 91.22(11) . . ? N5 Fe1 N6 81.50(13) . . ? N4 Fe1 N6 165.92(12) . . ? C2 Fe1 N6 86.27(13) . . ? C1 Fe1 N6 90.10(13) . . ? N3 Fe1 N6 111.65(11) . . ? O3 Mn1 O4 87.38(10) . . ? O3 Mn1 N8 173.39(11) . . ? O4 Mn1 N8 88.98(11) . . ? O3 Mn1 N7 90.15(11) . . ? O4 Mn1 N7 176.29(11) . . ? N8 Mn1 N7 93.21(11) . . ? O3 Mn1 N1 94.73(10) . . ? O4 Mn1 N1 93.72(11) . . ? N8 Mn1 N1 91.02(11) . . ? N7 Mn1 N1 89.24(12) . . ? O3 Mn1 O5 88.49(9) . . ? O4 Mn1 O5 90.54(10) . . ? N8 Mn1 O5 86.03(9) . . ? N7 Mn1 O5 86.63(10) . . ? N1 Mn1 O5 174.77(10) . . ? C8 N4 C9 127.1(3) . . ? C8 N4 Fe1 119.1(2) . . ? C9 N4 Fe1 113.7(2) . . ? C17 O3 Mn1 126.1(2) . . ? C27 N8 C26 117.8(3) . . ? C27 N8 Mn1 121.5(2) . . ? C26 N8 Mn1 120.6(2) . . ? C11 N5 C10 128.7(3) . . ? C11 N5 Fe1 118.2(3) . . ? C10 N5 Fe1 112.8(2) . . ? C23 N7 C24 118.4(3) . . ? C23 N7 Mn1 121.7(2) . . ? C24 N7 Mn1 119.9(2) . . ? C16 N6 C12 118.2(3) . . ? C16 N6 Fe1 130.9(2) . . ? C12 N6 Fe1 110.9(3) . . ? N2 C2 Fe1 177.1(3) . . ? C33 O4 Mn1 125.0(2) . . ? C3 N3 C7 117.7(3) . . ? C3 N3 Fe1 130.6(2) . . ? C7 N3 Fe1 111.6(2) . . ? O1 C11 N5 126.5(4) . . ? O1 C11 C12 122.8(4) . . ? N5 C11 C12 110.6(3) . . ? C38 O5 Mn1 127.9(3) . . ? C38 O5 H5 107.3 . . ? Mn1 O5 H5 120.0 . . ? N1 C1 Fe1 171.8(3) . . ? C25 C26 N8 112.4(3) . . ? C25 C26 H26A 109.1 . . ? N8 C26 H26A 109.1 . . ? C25 C26 H26B 109.1 . . ? N8 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? C1 N1 Mn1 167.4(3) . . ? C9 C10 C37 122.2(4) . . ? C9 C10 N5 113.7(3) . . ? C37 C10 N5 124.1(3) . . ? N6 C12 C13 120.9(4) . . ? N6 C12 C11 116.9(4) . . ? C13 C12 C11 122.0(4) . . ? C19 C20 C21 118.5(4) . . ? C19 C20 H20A 120.7 . . ? C21 C20 H20A 120.8 . . ? N3 C3 C4 123.2(4) . . ? N3 C3 H3A 118.4 . . ? C4 C3 H3A 118.4 . . ? C30 C29 C28 120.1(3) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? N3 C7 C6 122.3(3) . . ? N3 C7 C8 115.9(3) . . ? C6 C7 C8 121.8(3) . . ? C33 C28 C27 122.6(3) . . ? C33 C28 C29 118.6(3) . . ? C27 C28 C29 118.7(3) . . ? O4 C33 C32 120.3(3) . . ? O4 C33 C28 121.2(3) . . ? C32 C33 C28 118.5(3) . . ? C34 C9 C10 118.0(3) . . ? C34 C9 N4 127.3(3) . . ? C10 C9 N4 114.7(3) . . ? C25 C24 N7 114.8(3) . . ? C25 C24 H24A 108.6 . . ? N7 C24 H24A 108.6 . . ? C25 C24 H24B 108.6 . . ? N7 C24 H24B 108.6 . . ? H24A C24 H24B 107.5 . . ? O3 C17 C18 119.0(3) . . ? O3 C17 C22 122.7(3) . . ? C18 C17 C22 118.2(4) . . ? O2 C8 N4 128.2(4) . . ? O2 C8 C7 120.8(4) . . ? N4 C8 C7 111.0(3) . . ? N6 C16 C15 123.0(4) . . ? N6 C16 H16A 118.5 . . ? C15 C16 H16A 118.5 . . ? C17 C18 C19 118.0(4) . . ? C17 C18 H18A 121.0 . . ? C19 C18 H18A 121.0 . . ? N7 C23 C22 127.3(3) . . ? N7 C23 H23A 116.3 . . ? C22 C23 H23A 116.3 . . ? C6 C5 C4 118.9(4) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? C31 C32 C33 123.5(4) . . ? C31 C32 H32A 118.3 . . ? C33 C32 H32A 118.3 . . ? N8 C27 C28 126.7(3) . . ? N8 C27 H27A 116.6 . . ? C28 C27 H27A 116.6 . . ? C3 C4 C5 119.1(4) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C13 C14 C15 118.3(5) . . ? C13 C14 H14A 120.8 . . ? C15 C14 H14A 120.8 . . ? C31 C30 C29 120.8(4) . . ? C31 C30 H30A 119.6 . . ? C29 C30 H30A 119.6 . . ? C24 C25 C26 114.6(3) . . ? C24 C25 H25A 108.6 . . ? C26 C25 H25A 108.6 . . ? C24 C25 H25B 108.6 . . ? C26 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? C5 C6 C7 118.8(4) . . ? C5 C6 H6A 120.6 . . ? C7 C6 H6A 120.6 . . ? C20 C19 C18 124.4(4) . . ? C20 C19 H19A 117.8 . . ? C18 C19 H19A 117.8 . . ? C14 C15 C16 118.5(5) . . ? C14 C15 H15A 120.8 . . ? C16 C15 H15A 120.7 . . ? C17 C22 C21 119.9(3) . . ? C17 C22 C23 122.1(3) . . ? C21 C22 C23 117.9(3) . . ? C20 C21 C22 120.7(4) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? C14 C13 C12 120.9(4) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C32 C31 C30 118.5(4) . . ? C32 C31 H31A 120.7 . . ? C30 C31 H31A 120.7 . . ? C9 C34 C35 116.7(4) . . ? C9 C34 H34 121.7 . . ? C35 C34 H34 121.6 . . ? C36 C37 C10 122.1(4) . . ? C36 C37 H37A 119.0 . . ? C10 C37 H37A 118.9 . . ? C37 C36 C35 115.4(4) . . ? C37 C36 H36A 122.3 . . ? C35 C36 H36A 122.3 . . ? C36 C35 C34 125.7(4) . . ? C36 C35 H35A 117.2 . . ? C34 C35 H35A 117.2 . . ? O5 C38 H38A 109.5 . . ? O5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? H400 O1W H401 105.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 N2 0.890 1.927 2.812(3) 172.28 4_555 O1W H400 O3W 0.850 2.535 3.386(4) 177.81 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.896 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.155 # Attachment 'dalton-ESI.cif' #=================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 699871' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H34 Fe Mn N8 O6' _chemical_formula_weight 809.52 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' O O 0.0106 0.0060 '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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 23.047(3) _cell_length_b 23.047(3) _cell_length_c 15.195(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8071(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5994 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.798 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14280 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7099 _reflns_number_gt 5994 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_data_reduction 'Crystalstructure 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.1548P)^2^+12.2474P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.641(19) _refine_ls_number_reflns 7099 _refine_ls_number_parameters 487 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.2367 _refine_ls_wR_factor_gt 0.2304 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.486 _refine_ls_shift/su_mean 0.013 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 0.55901(2) 0.18395(2) -0.04836(5) 0.06132(16) Uani 1 1 d . . . Mn1 Mn 0.77327(2) 0.25658(2) 0.03148(3) 0.03981(11) Uani 1 1 d . . . N1 N 0.69060(12) 0.21454(12) -0.0192(2) 0.0489(8) Uani 1 1 d . . . N2 N 0.42875(13) 0.15000(15) -0.0793(2) 0.0584(9) Uani 1 1 d . . . N3 N 0.57363(12) 0.09958(13) -0.03314(18) 0.0485(8) Uani 1 1 d . . . N4 N 0.55054(16) 0.1829(2) 0.0716(3) 0.1055(15) Uani 1 1 d . . . N5 N 0.53788(14) 0.26366(16) -0.0416(3) 0.184(3) Uani 1 1 d D . . N6 N 0.56304(15) 0.20771(14) -0.1759(3) 0.0845(11) Uani 1 1 d . . . N7 N 0.73993(12) 0.33627(13) -0.00135(19) 0.0478(8) Uani 1 1 d . . . N8 N 0.73883(12) 0.25747(13) 0.15566(19) 0.0481(8) Uani 1 1 d . . . C1 C 0.64358(15) 0.20134(14) -0.0351(3) 0.0475(9) Uani 1 1 d . . . C2 C 0.47792(18) 0.16259(17) -0.0701(3) 0.0625(12) Uani 1 1 d . . . C3 C 0.58410(19) 0.05738(16) -0.0920(3) 0.0554(11) Uani 1 1 d . . . H3A H 0.5876 0.0680 -0.1522 0.066 Uiso 1 1 calc R . . C4 C 0.5900(3) 0.00045(19) -0.0707(3) 0.0942(18) Uani 1 1 d . . . H4B H 0.5965 -0.0274 -0.1157 0.113 Uiso 1 1 calc R . . C5 C 0.5864(3) -0.0169(2) 0.0150(3) 0.0979(18) Uani 1 1 d . . . H5A H 0.5931 -0.0562 0.0307 0.117 Uiso 1 1 calc R . . C6 C 0.5730(2) 0.0241(3) 0.0792(3) 0.0993(17) Uani 1 1 d . . . H6A H 0.5678 0.0127 0.1387 0.119 Uiso 1 1 calc R . . C7 C 0.56711(17) 0.0831(2) 0.0542(3) 0.0700(13) Uani 1 1 d . . . C8 C 0.5546(2) 0.1345(4) 0.1152(3) 0.113(2) Uani 1 1 d . . . C9 C 0.54026(17) 0.24322(17) 0.1055(2) 0.1503(15) Uani 1 1 d D . . C10 C 0.5336(3) 0.28573(16) 0.0446(3) 0.248(5) Uani 1 1 d D . . C11 C 0.52172(18) 0.29377(15) -0.1093(3) 0.221(7) Uani 1 1 d D . . C12 C 0.53758(18) 0.2616(2) -0.1912(3) 0.145(3) Uani 1 1 d D . . C13 C 0.5291(2) 0.2826(2) -0.2749(5) 0.295(2) Uani 1 1 d D . . H13 H 0.5063 0.3163 -0.2845 0.354 Uiso 1 1 calc R . . C14 C 0.5533(3) 0.2549(3) -0.3418(4) 0.230(2) Uani 1 1 d D . . H14A H 0.5528 0.2714 -0.3991 0.276 Uiso 1 1 calc R . . C15 C 0.5792(3) 0.2020(2) -0.3271(4) 0.1870(18) Uani 1 1 d D . . H15 H 0.5930 0.1803 -0.3761 0.224 Uiso 1 1 calc R . . C16 C 0.5857(2) 0.1796(2) -0.2449(3) 0.0962(15) Uani 1 1 d D . . H16A H 0.6062 0.1443 -0.2365 0.115 Uiso 1 1 calc R . . C17 C 0.83670(16) 0.29954(15) -0.1183(2) 0.0451(9) Uani 1 1 d . . . C18 C 0.88681(17) 0.28880(18) -0.1681(2) 0.0543(11) Uani 1 1 d . . . H18A H 0.9023 0.2507 -0.1717 0.065 Uiso 1 1 calc R . . C19 C 0.9141(2) 0.33498(18) -0.2130(3) 0.0633(12) Uani 1 1 d . . . H19A H 0.9479 0.3278 -0.2472 0.076 Uiso 1 1 calc R . . C20 C 0.8918(2) 0.3908(2) -0.2073(3) 0.0667(12) Uani 1 1 d . . . H20A H 0.9096 0.4217 -0.2388 0.080 Uiso 1 1 calc R . . C21 C 0.84321(17) 0.40139(17) -0.1554(2) 0.0519(10) Uani 1 1 d . . . H21A H 0.8287 0.4398 -0.1504 0.062 Uiso 1 1 calc R . . C22 C 0.81474(15) 0.35521(16) -0.1093(2) 0.0478(9) Uani 1 1 d . . . C23 C 0.76490(16) 0.36988(14) -0.0581(2) 0.0490(9) Uani 1 1 d . . . H23A H 0.7487 0.4074 -0.0664 0.059 Uiso 1 1 calc R . . C24 C 0.68912(18) 0.35436(18) 0.1415(3) 0.0615(12) Uani 1 1 d . . . H24A H 0.7255 0.3727 0.1622 0.074 Uiso 1 1 calc R . . H24B H 0.6563 0.3766 0.1664 0.074 Uiso 1 1 calc R . . C25 C 0.68667(15) 0.35823(17) 0.0420(3) 0.0550(10) Uani 1 1 d . . . H25A H 0.6529 0.3356 0.0207 0.066 Uiso 1 1 calc R . . H25B H 0.6806 0.3992 0.0248 0.066 Uiso 1 1 calc R . . C26 C 0.68659(17) 0.29315(19) 0.1761(3) 0.0604(11) Uani 1 1 d . . . H26A H 0.6815 0.2946 0.2407 0.072 Uiso 1 1 calc R . . H26B H 0.6520 0.2737 0.1509 0.072 Uiso 1 1 calc R . . C27 C 0.76142(15) 0.22830(16) 0.2192(2) 0.0515(9) Uani 1 1 d . . . H27A H 0.7439 0.2335 0.2753 0.062 Uiso 1 1 calc R . . C28 C 0.80985(16) 0.18880(16) 0.2164(3) 0.0509(10) Uani 1 1 d . . . C29 C 0.83187(19) 0.16777(18) 0.2975(3) 0.0653(12) Uani 1 1 d . . . H29A H 0.8147 0.1801 0.3512 0.078 Uiso 1 1 calc R . . C30 C 0.87775(19) 0.12971(18) 0.2993(3) 0.0639(12) Uani 1 1 d . . . H30A H 0.8927 0.1157 0.3535 0.077 Uiso 1 1 calc R . . C31 C 0.90236(17) 0.11178(19) 0.2171(3) 0.0656(12) Uani 1 1 d . . . H31A H 0.9350 0.0866 0.2168 0.079 Uiso 1 1 calc R . . C32 C 0.87943(17) 0.13049(17) 0.1395(3) 0.0597(12) Uani 1 1 d . . . H32A H 0.8953 0.1163 0.0859 0.072 Uiso 1 1 calc R . . C33 C 0.83316(15) 0.17005(15) 0.1360(2) 0.0446(9) Uani 1 1 d . . . C34 C 0.5379(3) 0.26206(18) 0.1903(3) 0.133(2) Uani 1 1 d DU . . H34 H 0.5387 0.2349 0.2374 0.160 Uiso 1 1 calc R . . C35 C 0.5345(2) 0.32053(15) 0.2077(4) 0.480(10) Uani 1 1 d D . . H35 H 0.5396 0.3329 0.2668 0.576 Uiso 1 1 calc R . . C36 C 0.5242(3) 0.36187(15) 0.1453(3) 0.515(2) Uani 1 1 d D . . C37 C 0.5288(4) 0.34429(16) 0.0581(3) 0.159(3) Uani 1 1 d DU . . H37A H 0.5287 0.3712 0.0108 0.191 Uiso 1 1 calc R . . C38 C 0.5253(13) 0.42575(16) 0.1659(5) 0.816(17) Uani 1 1 d D . . H38C H 0.4925 0.4449 0.1369 1.225 Uiso 1 1 calc R . . H38B H 0.5617 0.4426 0.1445 1.225 Uiso 1 1 calc R . . H38A H 0.5224 0.4314 0.2297 1.225 Uiso 1 1 calc R . . O1 O 0.54950(18) 0.1205(3) 0.1972(2) 0.157(3) Uani 1 1 d . . . O2 O 0.5028(2) 0.34501(18) -0.1042(5) 0.165(2) Uani 1 1 d DU . . O4 O 0.81159(10) 0.18592(10) 0.05798(15) 0.0469(6) Uani 1 1 d . . . O3 O 0.81035(11) 0.25297(10) -0.08012(16) 0.0492(6) Uani 1 1 d . . . O1W O 0.85067(10) 0.30611(10) 0.09001(16) 0.0480(7) Uani 1 1 d . . . H1B H 0.8668 0.3004 0.1408 0.072 Uiso 1 1 d R . . H1A H 0.8449 0.3410 0.0875 0.072 Uiso 1 1 d R . . O2W O 0.12201(10) 0.15484(10) 0.09415(16) 0.429(5) Uani 0.50 1 d PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0355(2) 0.0526(3) 0.0959(4) -0.0260(3) -0.0071(3) -0.0035(2) Mn1 0.0343(2) 0.0393(2) 0.0459(2) -0.0073(2) -0.0003(2) -0.00052(18) N1 0.0387(13) 0.0473(14) 0.0607(17) -0.0110(13) -0.0050(13) -0.0060(12) N2 0.0368(14) 0.0604(17) 0.078(2) -0.0159(17) -0.0008(15) 0.0040(14) N3 0.0477(14) 0.0641(17) 0.0336(13) 0.0020(14) -0.0018(12) -0.0137(13) N4 0.0420(17) 0.186(4) 0.088(2) -0.083(2) 0.0015(17) -0.001(2) N5 0.0247(15) 0.070(2) 0.456(9) -0.116(3) -0.008(3) 0.0014(15) N6 0.0736(18) 0.0404(15) 0.140(3) 0.0350(17) -0.0664(18) -0.0233(14) N7 0.0411(14) 0.0471(14) 0.0552(15) -0.0145(12) -0.0067(12) 0.0019(12) N8 0.0430(14) 0.0559(16) 0.0454(13) -0.0111(13) -0.0027(12) -0.0084(13) C1 0.0431(16) 0.0411(15) 0.0582(19) -0.0132(16) -0.0021(16) -0.0030(13) C2 0.057(2) 0.057(2) 0.074(2) -0.0285(18) -0.0021(19) -0.0073(18) C3 0.077(2) 0.0454(18) 0.0441(18) 0.0007(16) -0.0070(18) -0.0009(19) C4 0.156(4) 0.0414(19) 0.085(3) 0.014(2) -0.050(3) -0.025(3) C5 0.142(4) 0.074(3) 0.078(3) 0.031(2) -0.038(3) -0.046(3) C6 0.080(3) 0.153(4) 0.065(2) 0.056(3) -0.025(2) -0.040(3) C7 0.053(2) 0.110(3) 0.047(2) 0.020(2) -0.0123(17) -0.021(2) C8 0.041(2) 0.244(7) 0.055(2) -0.051(3) -0.0010(19) 0.010(3) C9 0.0311(18) 0.218(3) 0.202(3) -0.187(2) 0.029(2) -0.024(2) C10 0.046(3) 0.151(4) 0.546(14) -0.212(5) -0.027(5) 0.007(3) C11 0.025(2) 0.035(2) 0.60(2) -0.012(6) 0.030(5) 0.0071(19) C12 0.0496(19) 0.072(2) 0.313(7) 0.089(3) -0.077(3) -0.0363(19) C13 0.092(2) 0.221(3) 0.570(6) 0.339(3) -0.182(3) -0.113(2) C14 0.206(4) 0.232(5) 0.252(5) 0.186(4) -0.174(4) -0.173(4) C15 0.263(4) 0.182(3) 0.115(3) 0.098(3) -0.117(3) -0.196(3) C16 0.136(3) 0.066(2) 0.087(3) 0.028(2) -0.059(2) -0.062(2) C17 0.0526(18) 0.0482(18) 0.0346(15) 0.0017(14) -0.0114(14) -0.0033(15) C18 0.059(2) 0.059(2) 0.0452(18) 0.0045(17) 0.0101(16) 0.0041(18) C19 0.072(2) 0.061(2) 0.057(2) 0.0079(19) 0.008(2) 0.001(2) C20 0.068(2) 0.073(2) 0.059(2) 0.0271(19) 0.003(2) -0.007(2) C21 0.0550(19) 0.0497(19) 0.0510(19) 0.0065(16) -0.0092(17) 0.0036(17) C22 0.0448(17) 0.0527(18) 0.0460(17) -0.0063(15) -0.0158(15) 0.0036(16) C23 0.0527(18) 0.0398(15) 0.0545(18) -0.0054(15) -0.0143(16) -0.0052(15) C24 0.049(2) 0.067(2) 0.068(2) -0.0249(19) -0.0005(19) 0.0056(19) C25 0.0395(16) 0.0609(19) 0.065(2) -0.0213(18) -0.0036(17) 0.0081(16) C26 0.0471(19) 0.070(2) 0.064(2) -0.0200(18) 0.0139(17) 0.0015(19) C27 0.0473(17) 0.0572(18) 0.0500(17) -0.0136(16) -0.0003(15) -0.0158(16) C28 0.0496(18) 0.0460(17) 0.0570(19) -0.0027(16) -0.0069(17) -0.0136(16) C29 0.070(2) 0.063(2) 0.063(2) 0.0049(19) -0.0184(19) -0.0267(19) C30 0.069(2) 0.056(2) 0.066(2) 0.0072(19) -0.017(2) -0.015(2) C31 0.0470(19) 0.065(2) 0.084(3) 0.021(2) -0.0200(19) -0.0106(18) C32 0.052(2) 0.054(2) 0.073(2) 0.0116(19) -0.0035(19) -0.0117(18) C33 0.0476(17) 0.0408(16) 0.0455(17) 0.0002(14) -0.0055(15) -0.0094(14) C34 0.110(4) 0.141(4) 0.150(4) -0.043(4) 0.015(3) -0.020(3) C35 0.028(2) 0.247(8) 1.17(3) -0.352(12) 0.137(7) -0.048(4) C36 0.073(4) 0.630(4) 0.843(5) -0.711(3) 0.123(4) -0.070(4) C37 0.143(5) 0.137(4) 0.197(5) -0.034(4) 0.022(4) 0.008(4) C38 1.52(4) 0.47(3) 0.457(19) 0.074(19) 0.61(2) 0.48(3) O1 0.083(2) 0.346(8) 0.0433(17) -0.023(3) -0.0053(17) 0.052(4) O2 0.104(3) 0.120(3) 0.273(5) 0.021(3) 0.034(3) 0.019(3) O4 0.0505(12) 0.0437(11) 0.0464(12) -0.0022(10) 0.0016(11) 0.0022(11) O3 0.0527(12) 0.0416(11) 0.0533(12) -0.0039(11) 0.0023(11) 0.0001(11) O1W 0.0448(12) 0.0357(11) 0.0636(14) 0.0045(11) -0.0070(11) -0.0012(10) O2W 0.378(7) 0.843(15) 0.065(5) 0.096(8) -0.043(6) -0.501 _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 N4 1.834(4) . ? Fe1 N5 1.903(4) . ? Fe1 C2 1.961(4) . ? Fe1 N3 1.987(3) . ? Fe1 C1 2.000(3) . ? Fe1 N6 2.016(4) . ? Mn1 O4 1.896(2) . ? Mn1 O3 1.901(3) . ? Mn1 N8 2.047(3) . ? Mn1 N7 2.052(3) . ? Mn1 N1 2.272(3) . ? Mn1 O1W 2.297(2) . ? N1 C1 1.151(4) . ? N2 C2 1.178(5) . ? N3 C3 1.343(5) . ? N3 C7 1.388(5) . ? N4 C8 1.301(9) . ? N4 C9 1.501(6) . ? N5 C11 1.296(5) . ? N5 C10 1.409(5) . ? N6 C16 1.338(6) . ? N6 C12 1.394(6) . ? N7 C23 1.294(5) . ? N7 C25 1.482(5) . ? N8 C27 1.287(5) . ? N8 C26 1.491(5) . ? C3 C4 1.358(6) . ? C3 H3A 0.9500 . ? C4 C5 1.365(7) . ? C4 H4B 0.9500 . ? C5 C6 1.391(8) . ? C5 H5A 0.9500 . ? C6 C7 1.420(8) . ? C6 H6A 0.9500 . ? C7 C8 1.531(9) . ? C8 O1 1.292(6) . ? C9 C10 1.356(5) . ? C9 C34 1.361(5) . ? C10 C37 1.369(5) . ? C11 O2 1.261(5) . ? C11 C12 1.493(6) . ? C12 C13 1.374(8) . ? C13 C14 1.323(9) . ? C13 H13 0.9500 . ? C14 C15 1.377(8) . ? C14 H14A 0.9500 . ? C15 C16 1.360(7) . ? C15 H15 0.9500 . ? C16 H16A 0.9500 . ? C17 O3 1.363(4) . ? C17 C22 1.386(5) . ? C17 C18 1.403(5) . ? C18 C19 1.412(6) . ? C18 H18A 0.9500 . ? C19 C20 1.388(6) . ? C19 H19A 0.9500 . ? C20 C21 1.392(6) . ? C20 H20A 0.9500 . ? C21 C22 1.433(5) . ? C21 H21A 0.9500 . ? C22 C23 1.428(5) . ? C23 H23A 0.9500 . ? C24 C26 1.506(6) . ? C24 C25 1.515(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.441(5) . ? C27 H27A 0.9500 . ? C28 C33 1.403(5) . ? C28 C29 1.419(6) . ? C29 C30 1.374(6) . ? C29 H29A 0.9500 . ? C30 C31 1.433(6) . ? C30 H30A 0.9500 . ? C31 C32 1.363(6) . ? C31 H31A 0.9500 . ? C32 C33 1.404(5) . ? C32 H32A 0.9500 . ? C33 O4 1.336(4) . ? C34 C35 1.376(5) . ? C34 H34 0.9500 . ? C35 C36 1.364(5) . ? C35 H35 0.9500 . ? C36 C37 1.391(5) . ? C36 C38 1.505(5) . ? C37 H37A 0.9500 . ? C38 H38C 0.9804 . ? C38 H38B 0.9804 . ? C38 H38A 0.9804 . ? O1W H1B 0.8664 . ? O1W H1A 0.8154 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N5 86.1(2) . . ? N4 Fe1 C2 93.58(18) . . ? N5 Fe1 C2 90.43(16) . . ? N4 Fe1 N3 83.65(19) . . ? N5 Fe1 N3 169.02(15) . . ? C2 Fe1 N3 86.30(15) . . ? N4 Fe1 C1 90.34(16) . . ? N5 Fe1 C1 92.90(14) . . ? C2 Fe1 C1 175.02(16) . . ? N3 Fe1 C1 91.10(13) . . ? N4 Fe1 N6 164.6(2) . . ? N5 Fe1 N6 78.54(15) . . ? C2 Fe1 N6 87.15(16) . . ? N3 Fe1 N6 111.71(13) . . ? C1 Fe1 N6 89.87(15) . . ? O4 Mn1 O3 86.70(10) . . ? O4 Mn1 N8 89.62(11) . . ? O3 Mn1 N8 175.61(11) . . ? O4 Mn1 N7 174.10(11) . . ? O3 Mn1 N7 89.46(11) . . ? N8 Mn1 N7 94.02(12) . . ? O4 Mn1 N1 95.53(10) . . ? O3 Mn1 N1 93.22(11) . . ? N8 Mn1 N1 89.51(11) . . ? N7 Mn1 N1 89.16(11) . . ? O4 Mn1 O1W 89.01(9) . . ? O3 Mn1 O1W 91.03(10) . . ? N8 Mn1 O1W 86.52(10) . . ? N7 Mn1 O1W 86.58(10) . . ? N1 Mn1 O1W 173.95(10) . . ? C1 N1 Mn1 166.7(3) . . ? C3 N3 C7 117.3(3) . . ? C3 N3 Fe1 131.4(2) . . ? C7 N3 Fe1 111.1(3) . . ? C8 N4 C9 129.1(4) . . ? C8 N4 Fe1 120.7(4) . . ? C9 N4 Fe1 110.2(3) . . ? C11 N5 C10 121.6(4) . . ? C11 N5 Fe1 123.2(3) . . ? C10 N5 Fe1 114.6(3) . . ? C16 N6 C12 117.7(4) . . ? C16 N6 Fe1 129.8(3) . . ? C12 N6 Fe1 112.5(3) . . ? C23 N7 C25 117.4(3) . . ? C23 N7 Mn1 122.1(2) . . ? C25 N7 Mn1 120.5(2) . . ? C27 N8 C26 117.3(3) . . ? C27 N8 Mn1 122.0(2) . . ? C26 N8 Mn1 120.7(2) . . ? N1 C1 Fe1 172.5(3) . . ? N2 C2 Fe1 177.1(4) . . ? N3 C3 C4 124.0(4) . . ? N3 C3 H3A 118.0 . . ? C4 C3 H3A 118.0 . . ? C3 C4 C5 120.3(5) . . ? C3 C4 H4B 119.9 . . ? C5 C4 H4B 119.9 . . ? C4 C5 C6 118.9(5) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? C5 C6 C7 119.0(4) . . ? C5 C6 H6A 120.5 . . ? C7 C6 H6A 120.5 . . ? N3 C7 C6 120.4(4) . . ? N3 C7 C8 112.8(4) . . ? C6 C7 C8 126.7(4) . . ? O1 C8 N4 134.4(7) . . ? O1 C8 C7 114.0(7) . . ? N4 C8 C7 111.6(4) . . ? C10 C9 C34 114.3(4) . . ? C10 C9 N4 116.9(3) . . ? C34 C9 N4 128.8(4) . . ? C9 C10 C37 128.2(4) . . ? C9 C10 N5 111.4(3) . . ? C37 C10 N5 120.1(4) . . ? O2 C11 N5 123.5(5) . . ? O2 C11 C12 126.9(5) . . ? N5 C11 C12 109.0(3) . . ? C13 C12 N6 121.8(5) . . ? C13 C12 C11 124.2(4) . . ? N6 C12 C11 114.0(4) . . ? C14 C13 C12 118.8(5) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 119.0(6) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? C16 C15 C14 122.1(6) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? N6 C16 C15 119.6(5) . . ? N6 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? O3 C17 C22 121.6(3) . . ? O3 C17 C18 117.2(3) . . ? C22 C17 C18 121.1(3) . . ? C17 C18 C19 119.7(4) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C20 C19 C18 120.2(4) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C19 C20 C21 119.7(4) . . ? C19 C20 H20A 120.1 . . ? C21 C20 H20A 120.1 . . ? C20 C21 C22 121.0(4) . . ? C20 C21 H21A 119.5 . . ? C22 C21 H21A 119.5 . . ? C17 C22 C23 124.5(3) . . ? C17 C22 C21 118.2(3) . . ? C23 C22 C21 117.3(3) . . ? N7 C23 C22 125.4(3) . . ? N7 C23 H23A 117.3 . . ? C22 C23 H23A 117.3 . . ? C26 C24 C25 113.7(3) . . ? C26 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? C26 C24 H24B 108.8 . . ? C25 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? N7 C25 C24 113.1(3) . . ? N7 C25 H25A 109.0 . . ? C24 C25 H25A 109.0 . . ? N7 C25 H25B 109.0 . . ? C24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? N8 C26 C24 114.4(3) . . ? N8 C26 H26A 108.7 . . ? C24 C26 H26A 108.7 . . ? N8 C26 H26B 108.7 . . ? C24 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? N8 C27 C28 128.4(3) . . ? N8 C27 H27A 115.8 . . ? C28 C27 H27A 115.8 . . ? C33 C28 C29 121.0(3) . . ? C33 C28 C27 121.2(3) . . ? C29 C28 C27 117.8(3) . . ? C30 C29 C28 120.7(4) . . ? C30 C29 H29A 119.6 . . ? C28 C29 H29A 119.6 . . ? C29 C30 C31 118.1(4) . . ? C29 C30 H30A 120.9 . . ? C31 C30 H30A 120.9 . . ? C32 C31 C30 120.6(4) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C31 C32 C33 122.2(4) . . ? C31 C32 H32A 118.9 . . ? C33 C32 H32A 118.9 . . ? O4 C33 C28 123.1(3) . . ? O4 C33 C32 119.6(3) . . ? C28 C33 C32 117.2(3) . . ? C9 C34 C35 119.7(4) . . ? C9 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 124.2(5) . . ? C36 C35 H35 117.9 . . ? C34 C35 H35 117.9 . . ? C35 C36 C37 116.4(4) . . ? C35 C36 C38 122.4(5) . . ? C37 C36 C38 118.8(4) . . ? C10 C37 C36 115.9(4) . . ? C10 C37 H37A 122.1 . . ? C36 C37 H37A 122.1 . . ? C36 C38 H38C 109.5 . . ? C36 C38 H38B 109.5 . . ? H38C C38 H38B 109.4 . . ? C36 C38 H38A 109.5 . . ? H38C C38 H38A 109.4 . . ? H38B C38 H38A 109.4 . . ? C33 O4 Mn1 126.7(2) . . ? C17 O3 Mn1 123.1(2) . . ? Mn1 O1W H1B 127.0 . . ? Mn1 O1W H1A 110.1 . . ? H1B O1W H1A 105.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1A N2 0.815 2.030 2.831(4) 167.16 4_655 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.914 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.109 #===End data_3 _database_code_depnum_ccdc_archive 'CCDC 699872' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H33 Cl Fe Mn N8 O6' _chemical_formula_weight 843.96 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' O O 0.0106 0.0060 '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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 23.16150(10) _cell_length_b 23.16150(10) _cell_length_c 15.18050(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8143.66(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4780 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 32.57 _exptl_crystal_description block _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% ? _diffrn_reflns_number 7548 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 32.57 _reflns_number_total 7548 _reflns_number_gt 4780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_data_reduction 'Crystalstructure 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0928P)^2^+2.0016P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.44(3) _refine_ls_number_reflns 7548 _refine_ls_number_parameters 507 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1777 _refine_ls_wR_factor_gt 0.1594 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.003 _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 0.31646(3) 0.94428(3) -0.04239(6) 0.0589(2) Uani 1 1 d . . . Mn1 Mn 0.24469(3) 0.73122(3) 0.02911(4) 0.04851(17) Uani 1 1 d . . . O1 O 0.3833(4) 0.9489(3) 0.1998(3) 0.128(2) Uani 1 1 d . . . O2 O 0.1574(2) 0.9995(3) -0.0943(7) 0.176(4) Uani 1 1 d . . . O3 O 0.31458(14) 0.69328(16) 0.0556(2) 0.0587(8) Uani 1 1 d . . . O4 O 0.24706(14) 0.69453(15) -0.0821(2) 0.0580(8) Uani 1 1 d . . . O5 O 0.19481(14) 0.65333(14) 0.0872(2) 0.0592(8) Uani 1 1 d . . . H5 H 0.1587 0.6473 0.0947 0.089 Uiso 1 1 d R . . N1 N 0.28561(18) 0.81426(17) -0.0195(3) 0.0612(10) Uani 1 1 d . . . N2 N 0.3482(2) 1.07300(18) -0.0763(3) 0.0655(11) Uani 1 1 d . . . N3 N 0.40052(17) 0.92992(16) -0.0316(3) 0.0530(8) Uani 1 1 d . . . N4 N 0.3231(3) 0.9511(2) 0.0829(4) 0.0854(18) Uani 1 1 d . . . N5 N 0.2385(2) 0.9648(2) -0.0220(6) 0.109(3) Uani 1 1 d . . . N6 N 0.2900(2) 0.9423(2) -0.1675(4) 0.0734(14) Uani 1 1 d . . . N7 N 0.16536(17) 0.76300(16) -0.0022(3) 0.0549(9) Uani 1 1 d . . . N8 N 0.24263(19) 0.76469(17) 0.1536(3) 0.0582(10) Uani 1 1 d . . . C1 C 0.29947(19) 0.86049(19) -0.0316(4) 0.0552(10) Uani 1 1 d . . . C2 C 0.3376(2) 1.0246(2) -0.0652(3) 0.0569(11) Uani 1 1 d . . . C3 C 0.3162(3) 0.9241(3) -0.2394(5) 0.089(2) Uani 1 1 d . . . H3A H 0.3518 0.9059 -0.2343 0.106 Uiso 1 1 calc R . . C4 C 0.2923(4) 0.9314(5) -0.3219(6) 0.128(4) Uani 1 1 d . . . H4A H 0.3115 0.9182 -0.3718 0.153 Uiso 1 1 calc R . . C5 C 0.2397(5) 0.9586(5) -0.3292(9) 0.148(6) Uani 1 1 d . . . H5A H 0.2232 0.9645 -0.3843 0.178 Uiso 1 1 calc R . . C6 C 0.2111(5) 0.9773(4) -0.2532(10) 0.143(5) Uani 1 1 d . . . H6A H 0.1757 0.9961 -0.2562 0.171 Uiso 1 1 calc R . . C7 C 0.2371(3) 0.9668(3) -0.1755(7) 0.103(3) Uani 1 1 d . . . C8 C 0.2055(3) 0.9795(3) -0.0946(11) 0.128(4) Uani 1 1 d . . . C9 C 0.2236(5) 0.9671(3) 0.0674(9) 0.131(5) Uani 1 1 d . . . C10 C 0.1660(5) 0.9731(3) 0.1015(12) 0.181(7) Uani 1 1 d . . . H10A H 0.1359 0.9795 0.0620 0.218 Uiso 1 1 calc R . . C11 C 0.1534(4) 0.9698(6) 0.1884(12) 0.247(14) Uani 1 1 d D . . C12 C 0.2028(6) 0.9677(5) 0.2500(6) 0.220(11) Uani 1 1 d D . . C13 C 0.2590(7) 0.9607(3) 0.2126(8) 0.172(7) Uani 1 1 d . . . H13A H 0.2897 0.9563 0.2515 0.207 Uiso 1 1 calc R . . C14 C 0.2714(5) 0.9599(3) 0.1255(7) 0.116(4) Uani 1 1 d . . . C15 C 0.3738(4) 0.9450(3) 0.1204(4) 0.088(2) Uani 1 1 d . . . C16 C 0.4184(3) 0.9336(2) 0.0546(3) 0.0681(14) Uani 1 1 d . . . C17 C 0.4768(4) 0.9275(3) 0.0769(5) 0.095(2) Uani 1 1 d . . . H17A H 0.4884 0.9297 0.1354 0.113 Uiso 1 1 calc R . . C18 C 0.5159(3) 0.9184(4) 0.0128(6) 0.097(2) Uani 1 1 d . . . H18A H 0.5547 0.9137 0.0271 0.116 Uiso 1 1 calc R . . C19 C 0.4989(3) 0.9161(4) -0.0728(5) 0.0856(19) Uani 1 1 d . . . H19A H 0.5260 0.9115 -0.1173 0.103 Uiso 1 1 calc R . . C20 C 0.4413(2) 0.9207(3) -0.0931(4) 0.0653(13) Uani 1 1 d . . . H20A H 0.4301 0.9173 -0.1517 0.078 Uiso 1 1 calc R . . C21 C 0.3304(2) 0.6720(2) 0.1315(3) 0.0563(11) Uani 1 1 d . . . C22 C 0.3681(3) 0.6255(3) 0.1345(5) 0.0703(14) Uani 1 1 d . . . H22A H 0.3811 0.6095 0.0819 0.084 Uiso 1 1 calc R . . C23 C 0.3868(3) 0.6025(3) 0.2126(6) 0.087(2) Uani 1 1 d . . . H23A H 0.4117 0.5710 0.2117 0.105 Uiso 1 1 calc R . . C24 C 0.3695(3) 0.6251(3) 0.2931(5) 0.089(2) Uani 1 1 d . . . H24A H 0.3821 0.6090 0.3458 0.107 Uiso 1 1 calc R . . C25 C 0.3323(3) 0.6728(3) 0.2923(4) 0.0820(18) Uani 1 1 d . . . H25A H 0.3216 0.6899 0.3453 0.098 Uiso 1 1 calc R . . C26 C 0.3111(2) 0.6953(2) 0.2125(4) 0.0622(12) Uani 1 1 d . . . C27 C 0.2718(2) 0.7419(2) 0.2180(3) 0.0633(12) Uani 1 1 d . . . H27A H 0.2663 0.7580 0.2735 0.076 Uiso 1 1 calc R . . C28 C 0.2065(3) 0.8158(3) 0.1736(4) 0.0740(16) Uani 1 1 d . . . H28A H 0.2250 0.8498 0.1492 0.089 Uiso 1 1 calc R . . H28B H 0.2047 0.8207 0.2370 0.089 Uiso 1 1 calc R . . C29 C 0.1464(3) 0.8123(3) 0.1385(4) 0.0745(15) Uani 1 1 d . . . H29A H 0.1237 0.8434 0.1636 0.089 Uiso 1 1 calc R . . H29B H 0.1293 0.7761 0.1572 0.089 Uiso 1 1 calc R . . C30 C 0.1434(3) 0.8160(2) 0.0402(4) 0.0673(13) Uani 1 1 d . . . H30A H 0.1037 0.8223 0.0224 0.081 Uiso 1 1 calc R . . H30B H 0.1661 0.8488 0.0204 0.081 Uiso 1 1 calc R . . C31 C 0.1325(2) 0.7371(2) -0.0588(3) 0.0583(11) Uani 1 1 d . . . H31A H 0.0959 0.7527 -0.0667 0.070 Uiso 1 1 calc R . . C32 C 0.1459(2) 0.6877(2) -0.1102(3) 0.0554(10) Uani 1 1 d . . . C33 C 0.1012(2) 0.6594(3) -0.1559(4) 0.0648(13) Uani 1 1 d . . . H33A H 0.0637 0.6734 -0.1515 0.078 Uiso 1 1 calc R . . C34 C 0.1120(3) 0.6118(3) -0.2065(4) 0.0783(16) Uani 1 1 d . . . H34A H 0.0820 0.5936 -0.2365 0.094 Uiso 1 1 calc R . . C35 C 0.1680(3) 0.5908(3) -0.2127(4) 0.0778(17) Uani 1 1 d . . . H35A H 0.1752 0.5576 -0.2454 0.093 Uiso 1 1 calc R . . C36 C 0.2133(3) 0.6186(3) -0.1709(3) 0.0677(14) Uani 1 1 d . . . H36A H 0.2507 0.6047 -0.1771 0.081 Uiso 1 1 calc R . . C37 C 0.2027(2) 0.6678(2) -0.1190(3) 0.0534(10) Uani 1 1 d . . . C51 C 0.2117(4) 0.5968(4) 0.0868(8) 0.119(3) Uani 1 1 d . . . H51A H 0.1828 0.5737 0.1154 0.179 Uiso 1 1 calc R . . H51B H 0.2477 0.5930 0.1175 0.179 Uiso 1 1 calc R . . H51C H 0.2163 0.5840 0.0271 0.179 Uiso 1 1 calc R . . Cl1 Cl 0.0734(3) 0.9707(4) 0.1906(8) 0.265(7) Uani 0.50 1 d PD . . Cl1' Cl 0.2075(4) 0.9661(3) 0.3735(4) 0.184(4) Uani 0.50 1 d PD . . O1W O 0.3670(11) 0.3573(6) 0.1090(9) 0.202(11) Uani 0.50 1 d P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0534(4) 0.0421(3) 0.0812(5) 0.0070(3) 0.0163(4) -0.0032(3) Mn1 0.0487(3) 0.0422(3) 0.0546(3) -0.0009(3) 0.0075(3) -0.0024(2) O1 0.231(8) 0.107(4) 0.046(2) 0.004(2) 0.015(3) 0.019(5) O2 0.058(3) 0.082(3) 0.389(14) -0.033(6) -0.022(5) 0.018(2) O3 0.0495(17) 0.068(2) 0.0585(19) 0.0005(16) -0.0007(15) 0.0050(15) O4 0.0505(17) 0.0601(19) 0.0634(18) -0.0100(15) 0.0058(15) -0.0029(15) O5 0.0480(17) 0.0472(17) 0.082(2) 0.0089(16) 0.0040(16) -0.0048(13) N1 0.061(2) 0.049(2) 0.074(3) 0.006(2) 0.010(2) -0.0087(16) N2 0.075(3) 0.048(2) 0.074(3) 0.0012(19) 0.009(2) -0.0029(19) N3 0.061(2) 0.0495(19) 0.0489(19) 0.0042(17) 0.0021(18) -0.0061(15) N4 0.126(5) 0.047(2) 0.083(3) -0.002(2) 0.055(4) -0.012(3) N5 0.063(3) 0.041(2) 0.223(8) 0.013(4) 0.046(4) -0.0018(19) N6 0.060(3) 0.054(2) 0.107(4) 0.027(3) -0.015(3) -0.016(2) N7 0.055(2) 0.0428(18) 0.067(2) 0.0058(17) 0.0131(17) 0.0028(15) N8 0.066(2) 0.049(2) 0.060(2) -0.0098(18) 0.0136(19) -0.0141(18) C1 0.051(2) 0.045(2) 0.070(3) 0.004(2) 0.014(2) -0.0014(16) C2 0.056(2) 0.048(2) 0.067(3) 0.007(2) 0.011(2) -0.0019(18) C3 0.075(4) 0.113(5) 0.078(4) 0.023(4) -0.023(3) -0.043(4) C4 0.125(7) 0.169(9) 0.088(5) 0.046(6) -0.041(5) -0.087(7) C5 0.129(9) 0.132(9) 0.184(10) 0.091(9) -0.101(8) -0.084(7) C6 0.102(7) 0.092(6) 0.235(13) 0.073(8) -0.082(9) -0.038(5) C7 0.065(4) 0.060(3) 0.185(8) 0.039(5) -0.045(5) -0.021(3) C8 0.055(4) 0.050(3) 0.281(14) 0.012(5) -0.006(6) -0.003(3) C9 0.128(7) 0.040(3) 0.226(12) -0.024(5) 0.125(9) -0.014(4) C10 0.139(8) 0.051(4) 0.354(19) -0.003(7) 0.138(11) 0.008(4) C11 0.241(18) 0.083(6) 0.42(3) -0.069(12) 0.25(2) -0.028(10) C12 0.32(2) 0.077(6) 0.259(17) -0.052(9) 0.249(18) -0.061(11) C13 0.293(16) 0.060(4) 0.163(9) -0.023(5) 0.161(11) -0.036(7) C14 0.149(8) 0.048(3) 0.151(8) -0.020(4) 0.097(7) -0.016(4) C15 0.144(7) 0.060(3) 0.061(3) 0.009(3) 0.019(4) 0.005(4) C16 0.101(4) 0.055(3) 0.048(3) 0.008(2) -0.009(3) -0.009(3) C17 0.111(6) 0.092(5) 0.080(4) 0.018(4) -0.044(4) -0.015(4) C18 0.065(4) 0.125(6) 0.101(5) 0.027(5) -0.017(4) -0.009(4) C19 0.053(3) 0.116(5) 0.088(4) 0.014(4) 0.005(3) -0.004(3) C20 0.056(3) 0.085(4) 0.055(3) 0.003(3) 0.003(2) -0.007(3) C21 0.046(2) 0.056(3) 0.067(3) 0.003(2) -0.001(2) -0.0116(19) C22 0.062(3) 0.066(3) 0.083(4) -0.002(3) -0.012(3) 0.000(2) C23 0.077(4) 0.069(4) 0.116(6) 0.029(4) -0.020(4) -0.012(3) C24 0.085(4) 0.096(5) 0.087(5) 0.032(4) -0.011(4) -0.017(4) C25 0.081(4) 0.095(5) 0.070(3) 0.013(3) -0.004(3) -0.036(4) C26 0.064(3) 0.062(3) 0.060(3) 0.008(2) 0.002(2) -0.021(2) C27 0.066(3) 0.069(3) 0.055(3) 0.000(2) 0.009(2) -0.017(2) C28 0.092(4) 0.056(3) 0.074(3) -0.011(3) 0.017(3) -0.002(3) C29 0.085(4) 0.058(3) 0.080(3) -0.005(3) 0.028(3) 0.010(3) C30 0.069(3) 0.049(2) 0.084(3) 0.002(3) 0.019(3) 0.011(2) C31 0.054(2) 0.051(2) 0.070(3) 0.011(2) 0.009(2) 0.0027(19) C32 0.054(2) 0.057(3) 0.056(2) 0.010(2) 0.002(2) -0.001(2) C33 0.057(3) 0.070(3) 0.067(3) 0.008(3) -0.009(2) -0.003(2) C34 0.086(4) 0.082(4) 0.067(3) 0.003(3) -0.022(3) -0.013(3) C35 0.098(5) 0.077(4) 0.058(3) -0.015(3) -0.012(3) 0.000(3) C36 0.076(4) 0.075(3) 0.053(3) -0.012(2) 0.000(2) 0.012(3) C37 0.058(3) 0.056(2) 0.047(2) 0.0061(19) 0.0036(19) -0.002(2) C51 0.086(5) 0.086(5) 0.185(10) 0.013(6) -0.006(6) -0.001(4) Cl1 0.133(5) 0.225(7) 0.438(14) -0.221(9) 0.169(7) -0.085(5) Cl1' 0.261(8) 0.168(5) 0.122(4) -0.051(4) 0.125(5) -0.078(5) O1W 0.40(3) 0.114(10) 0.094(9) -0.006(7) -0.077(13) -0.095(15) _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 N5 1.892(5) . ? Fe1 N4 1.915(6) . ? Fe1 C2 1.954(5) . ? Fe1 N3 1.982(4) . ? Fe1 C1 1.987(4) . ? Fe1 N6 1.996(6) . ? Mn1 O3 1.885(3) . ? Mn1 O4 1.891(3) . ? Mn1 N7 2.035(4) . ? Mn1 N8 2.043(4) . ? Mn1 N1 2.268(4) . ? Mn1 O5 2.317(3) . ? O1 C15 1.229(9) . ? O2 C8 1.208(9) . ? O3 C21 1.306(6) . ? O4 C37 1.324(6) . ? O5 C51 1.366(9) . ? O5 H5 0.8555 . ? N1 C1 1.133(6) . ? N2 C2 1.160(6) . ? N3 C20 1.347(7) . ? N3 C16 1.374(7) . ? N4 C15 1.312(11) . ? N4 C14 1.377(10) . ? N5 C8 1.384(15) . ? N5 C9 1.401(14) . ? N6 C3 1.317(10) . ? N6 C7 1.357(9) . ? N7 C31 1.296(7) . ? N7 C30 1.477(6) . ? N8 C27 1.301(7) . ? N8 C28 1.482(7) . ? C3 C4 1.380(10) . ? C3 H3A 0.9300 . ? C4 C5 1.376(16) . ? C4 H4A 0.9300 . ? C5 C6 1.399(18) . ? C5 H5A 0.9300 . ? C6 C7 1.345(14) . ? C6 H6A 0.9300 . ? C7 C8 1.460(16) . ? C9 C10 1.439(12) . ? C9 C14 1.424(16) . ? C10 C11 1.35(2) . ? C10 H10A 0.9300 . ? C11 C12 1.478(10) . ? C11 Cl1 1.854(9) . ? C12 C13 1.428(18) . ? C12 Cl1' 1.878(9) . ? C13 C14 1.353(13) . ? C13 H13A 0.9300 . ? C15 C16 1.460(10) . ? C16 C17 1.402(10) . ? C17 C18 1.347(11) . ? C17 H17A 0.9300 . ? C18 C19 1.359(10) . ? C18 H18A 0.9300 . ? C19 C20 1.371(9) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.388(8) . ? C21 C26 1.414(8) . ? C22 C23 1.370(9) . ? C22 H22A 0.9300 . ? C23 C24 1.388(12) . ? C23 H23A 0.9300 . ? C24 C25 1.401(11) . ? C24 H24A 0.9300 . ? C25 C26 1.408(9) . ? C25 H25A 0.9300 . ? C26 C27 1.415(8) . ? C27 H27A 0.9300 . ? C28 C29 1.492(10) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.496(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.419(7) . ? C31 H31A 0.9300 . ? C32 C37 1.401(7) . ? C32 C33 1.408(7) . ? C33 C34 1.367(9) . ? C33 H33A 0.9300 . ? C34 C35 1.390(10) . ? C34 H34A 0.9300 . ? C35 C36 1.384(9) . ? C35 H35A 0.9300 . ? C36 C37 1.407(7) . ? C36 H36A 0.9300 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 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 N5 Fe1 N4 83.9(4) . . ? N5 Fe1 C2 91.6(2) . . ? N4 Fe1 C2 94.4(2) . . ? N5 Fe1 N3 164.9(3) . . ? N4 Fe1 N3 81.5(2) . . ? C2 Fe1 N3 85.91(19) . . ? N5 Fe1 C1 92.50(19) . . ? N4 Fe1 C1 90.8(2) . . ? C2 Fe1 C1 173.6(2) . . ? N3 Fe1 C1 91.37(17) . . ? N5 Fe1 N6 82.5(3) . . ? N4 Fe1 N6 166.4(3) . . ? C2 Fe1 N6 86.0(2) . . ? N3 Fe1 N6 112.1(2) . . ? C1 Fe1 N6 89.7(2) . . ? O3 Mn1 O4 87.49(15) . . ? O3 Mn1 N7 173.40(16) . . ? O4 Mn1 N7 88.87(16) . . ? O3 Mn1 N8 89.97(17) . . ? O4 Mn1 N8 175.59(17) . . ? N7 Mn1 N8 93.30(18) . . ? O3 Mn1 N1 96.08(16) . . ? O4 Mn1 N1 94.49(16) . . ? N7 Mn1 N1 89.69(16) . . ? N8 Mn1 N1 89.37(16) . . ? O3 Mn1 O5 89.08(14) . . ? O4 Mn1 O5 90.26(14) . . ? N7 Mn1 O5 85.44(14) . . ? N8 Mn1 O5 86.08(14) . . ? N1 Mn1 O5 173.13(14) . . ? C21 O3 Mn1 127.2(3) . . ? C37 O4 Mn1 124.4(3) . . ? C51 O5 Mn1 127.0(5) . . ? C51 O5 H5 97.1 . . ? Mn1 O5 H5 131.6 . . ? C1 N1 Mn1 166.6(4) . . ? C20 N3 C16 117.3(5) . . ? C20 N3 Fe1 131.2(4) . . ? C16 N3 Fe1 111.3(4) . . ? C15 N4 C14 126.3(8) . . ? C15 N4 Fe1 119.6(4) . . ? C14 N4 Fe1 114.1(7) . . ? C8 N5 C9 128.8(8) . . ? C8 N5 Fe1 117.3(7) . . ? C9 N5 Fe1 113.8(7) . . ? C3 N6 C7 118.4(7) . . ? C3 N6 Fe1 130.9(4) . . ? C7 N6 Fe1 110.7(6) . . ? C31 N7 C30 118.2(4) . . ? C31 N7 Mn1 121.2(3) . . ? C30 N7 Mn1 120.6(4) . . ? C27 N8 C28 117.6(5) . . ? C27 N8 Mn1 122.0(3) . . ? C28 N8 Mn1 120.4(4) . . ? N1 C1 Fe1 173.0(4) . . ? N2 C2 Fe1 177.1(5) . . ? N6 C3 C4 121.9(9) . . ? N6 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C5 C4 C3 118.9(11) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? C4 C5 C6 119.7(9) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C7 C6 C5 117.0(11) . . ? C7 C6 H6A 121.5 . . ? C5 C6 H6A 121.5 . . ? C6 C7 N6 124.0(12) . . ? C6 C7 C8 118.5(10) . . ? N6 C7 C8 117.4(8) . . ? O2 C8 N5 127.0(14) . . ? O2 C8 C7 122.8(13) . . ? N5 C8 C7 110.2(6) . . ? N5 C9 C10 125.5(15) . . ? N5 C9 C14 113.8(7) . . ? C10 C9 C14 120.7(13) . . ? C11 C10 C9 122.9(15) . . ? C11 C10 H10A 118.5 . . ? C9 C10 H10A 118.5 . . ? C10 C11 C12 116.9(10) . . ? C10 C11 Cl1 103.4(11) . . ? C12 C11 Cl1 139.7(14) . . ? C13 C12 C11 117.2(10) . . ? C13 C12 Cl1' 110.0(11) . . ? C11 C12 Cl1' 132.6(12) . . ? C14 C13 C12 125.7(16) . . ? C14 C13 H13A 117.2 . . ? C12 C13 H13A 117.2 . . ? C13 C14 N4 130.2(14) . . ? C13 C14 C9 116.0(11) . . ? N4 C14 C9 113.8(8) . . ? O1 C15 N4 125.2(8) . . ? O1 C15 C16 124.0(9) . . ? N4 C15 C16 110.8(6) . . ? N3 C16 C17 120.9(6) . . ? N3 C16 C15 116.7(6) . . ? C17 C16 C15 122.4(6) . . ? C18 C17 C16 119.5(6) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 120.0(6) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C18 C19 C20 119.7(7) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? N3 C20 C19 122.5(5) . . ? N3 C20 H20A 118.7 . . ? C19 C20 H20A 118.7 . . ? O3 C21 C22 119.9(5) . . ? O3 C21 C26 122.3(5) . . ? C22 C21 C26 117.8(5) . . ? C23 C22 C21 121.9(7) . . ? C23 C22 H22A 119.1 . . ? C21 C22 H22A 119.1 . . ? C22 C23 C24 121.6(7) . . ? C22 C23 H23A 119.2 . . ? C24 C23 H23A 119.2 . . ? C23 C24 C25 117.9(7) . . ? C23 C24 H24A 121.0 . . ? C25 C24 H24A 121.0 . . ? C24 C25 C26 120.9(7) . . ? C24 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C25 C26 C21 119.8(6) . . ? C25 C26 C27 117.1(6) . . ? C21 C26 C27 123.1(5) . . ? N8 C27 C26 126.8(5) . . ? N8 C27 H27A 116.6 . . ? C26 C27 H27A 116.6 . . ? N8 C28 C29 114.1(5) . . ? N8 C28 H28A 108.7 . . ? C29 C28 H28A 108.7 . . ? N8 C28 H28B 108.7 . . ? C29 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C28 C29 C30 113.3(5) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N7 C30 C29 111.7(4) . . ? N7 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? N7 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? N7 C31 C32 127.5(5) . . ? N7 C31 H31A 116.2 . . ? C32 C31 H31A 116.2 . . ? C37 C32 C33 119.4(5) . . ? C37 C32 C31 121.6(5) . . ? C33 C32 C31 119.0(5) . . ? C34 C33 C32 121.2(6) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? C33 C34 C35 119.4(6) . . ? C33 C34 H34A 120.3 . . ? C35 C34 H34A 120.3 . . ? C36 C35 C34 120.9(6) . . ? C36 C35 H35A 119.5 . . ? C34 C35 H35A 119.5 . . ? C35 C36 C37 120.1(6) . . ? C35 C36 H36A 119.9 . . ? C37 C36 H36A 119.9 . . ? O4 C37 C32 122.3(4) . . ? O4 C37 C36 118.7(5) . . ? C32 C37 C36 118.9(5) . . ? O5 C51 H51A 109.5 . . ? O5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 N2 0.856 2.007 2.826(4) 160.10 2_465 _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 32.57 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.595 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.072 #===End data_5 _database_code_depnum_ccdc_archive 'CCDC 699873' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H77 Cl4 Fe2 Mn2 N17 O16' _chemical_formula_weight 1883.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.771(6) _cell_length_b 15.849(5) _cell_length_c 18.403(6) _cell_angle_alpha 77.540(16) _cell_angle_beta 73.189(15) _cell_angle_gamma 78.680(16) _cell_volume 4255(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8568 _cell_measurement_theta_min 3.0043 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8356 _exptl_absorpt_process_details 'CrystalClear (Rigaku Corp., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Saturn70 CCD (4x4 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_decay_% ? _diffrn_reflns_number 28582 _diffrn_reflns_av_R_equivalents 0.0961 _diffrn_reflns_av_sigmaI/netI 0.1495 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14706 _reflns_number_gt 8568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics xp _computing_publication_material xp _refine_special_details ; The atom C84 has been refined isotropically due to the heavy disorder of the atom. The R1 value is greater than 0.1, which is due to the bad quality of the single crystal used for X-ray diffraction measurement. 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^)+(0.1295P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14706 _refine_ls_number_parameters 1091 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1666 _refine_ls_R_factor_gt 0.1081 _refine_ls_wR_factor_ref 0.2869 _refine_ls_wR_factor_gt 0.2467 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.003 _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 0.46530(8) 0.61111(7) 0.33922(6) 0.0276(3) Uani 1 1 d . . . Fe2 Fe 0.11479(8) 0.82006(7) -0.04083(6) 0.0276(3) Uani 1 1 d . . . Mn1 Mn 0.76214(8) 0.38308(7) 0.33953(6) 0.0272(3) Uani 1 1 d . . . Mn2 Mn 0.16653(9) 0.81423(8) 0.31663(7) 0.0337(3) Uani 1 1 d . . . Cl1 Cl 0.1767(2) 1.25303(18) 0.36290(19) 0.0740(9) Uani 1 1 d . . . Cl2 Cl -0.22610(16) 0.69479(15) 0.27211(14) 0.0477(6) Uani 1 1 d . . . Cl3 Cl 1.1802(2) 0.5128(2) 0.3130(2) 0.0815(10) Uani 1 1 d . . . Cl4 Cl 0.7029(2) -0.06789(16) 0.43805(18) 0.0741(9) Uani 1 1 d . . . O1 O 0.4472(4) 0.4431(4) 0.2115(3) 0.0454(16) Uani 1 1 d . . . O2 O 0.5649(4) 0.8366(4) 0.2516(3) 0.0444(16) Uani 1 1 d . . . O3 O -0.0126(5) 0.6216(4) 0.0879(3) 0.0484(17) Uani 1 1 d . . . O4 O 0.3820(4) 0.8092(5) -0.0989(4) 0.0585(19) Uani 1 1 d . . . O5 O 0.8155(4) 0.4260(3) 0.4009(3) 0.0349(14) Uani 1 1 d . . . O6 O 0.7132(4) 0.3026(3) 0.4270(3) 0.0321(13) Uani 1 1 d . . . O7 O 0.1470(4) 0.8838(4) 0.3926(3) 0.0401(15) Uani 1 1 d . . . O8 O 0.0694(4) 0.7570(4) 0.3801(3) 0.0447(16) Uani 1 1 d . . . O9 O 0.0696(4) 0.9173(4) 0.2612(3) 0.0382(14) Uani 1 1 d . . . H9A H 0.0659 0.9020 0.2208 0.046 Uiso 1 1 d R . . H10A H 0.8834 0.2528 0.2874 0.046 Uiso 1 1 d R . . O10 O 0.8870(4) 0.2850(4) 0.3178(3) 0.0337(14) Uani 1 1 d . . . N1 N 0.6390(5) 0.4840(4) 0.3554(4) 0.0298(16) Uani 1 1 d . . . N2 N 0.2771(5) 0.7226(5) 0.3534(4) 0.0388(18) Uani 1 1 d . . . N3 N 0.0832(5) 0.8879(4) 0.1137(4) 0.0363(17) Uani 1 1 d . . . N4 N 0.1070(5) 0.8014(5) -0.2030(4) 0.0422(19) Uani 1 1 d . . . N5 N 0.3962(4) 0.5125(4) 0.3930(3) 0.0256(15) Uani 1 1 d . . . N6 N 0.4690(4) 0.5654(4) 0.2508(3) 0.0287(15) Uani 1 1 d . . . N7 N 0.5236(5) 0.6993(4) 0.2664(4) 0.0339(17) Uani 1 1 d . . . N8 N 0.4867(5) 0.6773(4) 0.4127(4) 0.0314(16) Uani 1 1 d . . . N9 N 0.1665(4) 0.9286(4) -0.0975(3) 0.0283(15) Uani 1 1 d . . . N10 N 0.2376(5) 0.7754(4) -0.0485(3) 0.0290(16) Uani 1 1 d . . . N11 N 0.0974(5) 0.7057(4) 0.0134(4) 0.0321(16) Uani 1 1 d . . . N12 N -0.0179(5) 0.8356(4) -0.0213(3) 0.0283(15) Uani 1 1 d . . . N13 N 0.8206(5) 0.4659(4) 0.2456(4) 0.0308(16) Uani 1 1 d . . . N14 N 0.7076(4) 0.3294(4) 0.2750(3) 0.0287(15) Uani 1 1 d . . . N15 N 0.2611(5) 0.8864(5) 0.2464(4) 0.0382(18) Uani 1 1 d . . . N16 N 0.1779(5) 0.7438(4) 0.2344(4) 0.0313(16) Uani 1 1 d . . . N17 N 0.1054(18) 0.2913(13) 0.1660(12) 0.233(12) Uani 1 1 d D . . C1 C 0.5765(6) 0.5329(5) 0.3496(4) 0.031(2) Uani 1 1 d . . . C2 C 0.3472(6) 0.6814(5) 0.3482(5) 0.033(2) Uani 1 1 d . . . C3 C 0.0963(5) 0.8642(5) 0.0561(5) 0.0294(18) Uani 1 1 d . . . C4 C 0.1131(5) 0.8043(5) -0.1435(5) 0.0317(19) Uani 1 1 d . . . C5 C 0.4741(5) 0.6551(5) 0.4897(5) 0.0301(19) Uani 1 1 d . . . H5A H 0.4524 0.6030 0.5146 0.036 Uiso 1 1 calc R . . C6 C 0.4924(6) 0.7074(6) 0.5326(5) 0.039(2) Uani 1 1 d . . . H6A H 0.4822 0.6912 0.5857 0.046 Uiso 1 1 calc R . . C7 C 0.5268(6) 0.7860(6) 0.4948(6) 0.043(2) Uani 1 1 d . . . H7A H 0.5396 0.8225 0.5224 0.052 Uiso 1 1 calc R . . C8 C 0.5407(6) 0.8071(6) 0.4160(5) 0.041(2) Uani 1 1 d . . . H8A H 0.5632 0.8583 0.3895 0.049 Uiso 1 1 calc R . . C9 C 0.5208(5) 0.7508(5) 0.3762(5) 0.032(2) Uani 1 1 d . . . C10 C 0.5374(6) 0.7680(6) 0.2905(5) 0.035(2) Uani 1 1 d . . . C11 C 0.5391(6) 0.6896(5) 0.1886(5) 0.034(2) Uani 1 1 d . . . C12 C 0.5780(6) 0.7473(6) 0.1232(5) 0.043(2) Uani 1 1 d . . . H12A H 0.5960 0.7979 0.1280 0.052 Uiso 1 1 calc R . . C13 C 0.5887(7) 0.7266(7) 0.0528(6) 0.057(3) Uani 1 1 d . . . H13A H 0.6129 0.7651 0.0091 0.068 Uiso 1 1 calc R . . C14 C 0.5648(7) 0.6503(6) 0.0431(5) 0.050(3) Uani 1 1 d . . . H14A H 0.5748 0.6380 -0.0061 0.060 Uiso 1 1 calc R . . C15 C 0.5263(7) 0.5927(6) 0.1067(5) 0.045(2) Uani 1 1 d . . . H15A H 0.5104 0.5415 0.1009 0.054 Uiso 1 1 calc R . . C16 C 0.5117(6) 0.6136(5) 0.1806(4) 0.0313(19) Uani 1 1 d . . . C17 C 0.4412(5) 0.4886(5) 0.2607(4) 0.0298(19) Uani 1 1 d . . . C18 C 0.3952(6) 0.4596(5) 0.3434(4) 0.0307(19) Uani 1 1 d . . . C19 C 0.3498(6) 0.3888(5) 0.3681(5) 0.037(2) Uani 1 1 d . . . H19A H 0.3529 0.3515 0.3344 0.044 Uiso 1 1 calc R . . C20 C 0.2987(6) 0.3733(5) 0.4445(5) 0.034(2) Uani 1 1 d . . . H20A H 0.2664 0.3264 0.4621 0.040 Uiso 1 1 calc R . . C21 C 0.2973(6) 0.4289(5) 0.4930(5) 0.038(2) Uani 1 1 d . . . H21A H 0.2646 0.4195 0.5442 0.046 Uiso 1 1 calc R . . C22 C 0.3447(6) 0.4982(5) 0.4653(4) 0.033(2) Uani 1 1 d . . . H22A H 0.3408 0.5369 0.4980 0.040 Uiso 1 1 calc R . . C23 C 0.1262(6) 1.0075(5) -0.1225(5) 0.039(2) Uani 1 1 d . . . H23A H 0.0640 1.0176 -0.1084 0.047 Uiso 1 1 calc R . . C24 C 0.1705(7) 1.0744(6) -0.1674(5) 0.044(2) Uani 1 1 d . . . H24A H 0.1387 1.1274 -0.1842 0.053 Uiso 1 1 calc R . . C25 C 0.2637(7) 1.0621(7) -0.1878(5) 0.051(3) Uani 1 1 d . . . H25A H 0.2958 1.1064 -0.2178 0.061 Uiso 1 1 calc R . . C26 C 0.3064(7) 0.9818(6) -0.1617(5) 0.045(2) Uani 1 1 d . . . H26A H 0.3686 0.9709 -0.1742 0.054 Uiso 1 1 calc R . . C27 C 0.2560(6) 0.9158(6) -0.1160(5) 0.034(2) Uani 1 1 d . . . C28 C 0.2974(6) 0.8280(6) -0.0880(5) 0.042(2) Uani 1 1 d . . . C29 C 0.2532(6) 0.6890(5) -0.0112(5) 0.034(2) Uani 1 1 d . . . C30 C 0.3376(6) 0.6402(6) -0.0049(5) 0.042(2) Uani 1 1 d . . . H30A H 0.3902 0.6644 -0.0280 0.050 Uiso 1 1 calc R . . C31 C 0.3397(8) 0.5567(7) 0.0358(6) 0.055(3) Uani 1 1 d . . . H31A H 0.3950 0.5251 0.0398 0.066 Uiso 1 1 calc R . . C32 C 0.2645(9) 0.5173(7) 0.0710(6) 0.059(3) Uani 1 1 d . . . H32A H 0.2687 0.4609 0.0988 0.071 Uiso 1 1 calc R . . C33 C 0.1807(7) 0.5645(5) 0.0642(5) 0.046(3) Uani 1 1 d . . . H33A H 0.1291 0.5387 0.0865 0.055 Uiso 1 1 calc R . . C34 C 0.1753(6) 0.6504(5) 0.0239(4) 0.033(2) Uani 1 1 d . . . C35 C 0.0127(6) 0.6884(6) 0.0442(5) 0.035(2) Uani 1 1 d . . . C36 C -0.0531(6) 0.7641(5) 0.0218(4) 0.033(2) Uani 1 1 d . . . C37 C -0.1448(6) 0.7596(6) 0.0411(5) 0.043(2) Uani 1 1 d . . . H37A H -0.1672 0.7096 0.0710 0.051 Uiso 1 1 calc R . . C38 C -0.2021(6) 0.8309(7) 0.0149(6) 0.052(3) Uani 1 1 d . . . H38A H -0.2634 0.8296 0.0275 0.062 Uiso 1 1 calc R . . C39 C -0.1665(6) 0.9028(6) -0.0295(5) 0.046(2) Uani 1 1 d . . . H39A H -0.2031 0.9515 -0.0477 0.056 Uiso 1 1 calc R . . C40 C -0.0732(6) 0.9019(5) -0.0475(5) 0.037(2) Uani 1 1 d . . . H40A H -0.0492 0.9503 -0.0792 0.044 Uiso 1 1 calc R . . C41 C 0.7103(5) 0.2198(5) 0.4271(5) 0.0306(19) Uani 1 1 d . . . C42 C 0.7080(6) 0.1603(5) 0.4959(5) 0.035(2) Uani 1 1 d . . . H42A H 0.7097 0.1796 0.5396 0.042 Uiso 1 1 calc R . . C43 C 0.7032(6) 0.0733(6) 0.4998(6) 0.044(2) Uani 1 1 d . . . H43A H 0.7005 0.0348 0.5461 0.053 Uiso 1 1 calc R . . C44 C 0.7024(7) 0.0432(6) 0.4344(6) 0.044(2) Uani 1 1 d . . . C45 C 0.7036(6) 0.1003(6) 0.3671(5) 0.044(2) Uani 1 1 d . . . H45A H 0.7024 0.0797 0.3239 0.053 Uiso 1 1 calc R . . C46 C 0.7067(6) 0.1895(5) 0.3615(5) 0.034(2) Uani 1 1 d . . . C47 C 0.6976(6) 0.2492(5) 0.2922(5) 0.033(2) Uani 1 1 d . . . H47A H 0.6826 0.2264 0.2558 0.040 Uiso 1 1 calc R . . C48 C 0.6840(6) 0.3814(5) 0.2044(4) 0.033(2) Uani 1 1 d . . . H48A H 0.6321 0.4243 0.2193 0.040 Uiso 1 1 calc R . . H48B H 0.6676 0.3429 0.1779 0.040 Uiso 1 1 calc R . . C49 C 0.7590(6) 0.4283(6) 0.1489(4) 0.037(2) Uani 1 1 d . . . H49A H 0.8124 0.3860 0.1368 0.044 Uiso 1 1 calc R . . H49B H 0.7420 0.4535 0.1013 0.044 Uiso 1 1 calc R . . C50 C 0.7805(6) 0.4996(5) 0.1805(4) 0.033(2) Uani 1 1 d . . . H50A H 0.8215 0.5329 0.1398 0.040 Uiso 1 1 calc R . . H50B H 0.7260 0.5389 0.1970 0.040 Uiso 1 1 calc R . . C51 C 0.8954(6) 0.4911(5) 0.2415(4) 0.032(2) Uani 1 1 d . . . H51A H 0.9228 0.5235 0.1951 0.039 Uiso 1 1 calc R . . C52 C 0.9402(6) 0.4731(5) 0.3031(5) 0.032(2) Uani 1 1 d . . . C53 C 1.0297(6) 0.4942(5) 0.2818(5) 0.040(2) Uani 1 1 d . . . H53A H 1.0581 0.5135 0.2307 0.048 Uiso 1 1 calc R . . C54 C 1.0717(6) 0.4849(6) 0.3391(6) 0.044(2) Uani 1 1 d . . . C55 C 1.0317(7) 0.4545(6) 0.4151(6) 0.047(3) Uani 1 1 d . . . H55A H 1.0626 0.4473 0.4526 0.056 Uiso 1 1 calc R . . C56 C 0.9471(6) 0.4352(5) 0.4347(5) 0.040(2) Uani 1 1 d . . . H56A H 0.9201 0.4161 0.4862 0.048 Uiso 1 1 calc R . . C57 C 0.8991(6) 0.4432(5) 0.3793(5) 0.033(2) Uani 1 1 d . . . C58 C 0.1548(6) 0.9674(6) 0.3830(5) 0.039(2) Uani 1 1 d . . . C59 C 0.1110(6) 1.0134(6) 0.4449(5) 0.043(2) Uani 1 1 d . . . H59A H 0.0775 0.9845 0.4904 0.051 Uiso 1 1 calc R . . C60 C 0.1172(7) 1.0979(6) 0.4388(6) 0.047(2) Uani 1 1 d . . . H60A H 0.0880 1.1273 0.4798 0.056 Uiso 1 1 calc R . . C61 C 0.1680(7) 1.1423(6) 0.3701(6) 0.051(3) Uani 1 1 d . . . C62 C 0.2130(7) 1.1000(6) 0.3093(6) 0.050(3) Uani 1 1 d . . . H62A H 0.2481 1.1294 0.2649 0.060 Uiso 1 1 calc R . . C63 C 0.2054(6) 1.0108(6) 0.3147(5) 0.038(2) Uani 1 1 d . . . C64 C 0.2624(6) 0.9648(6) 0.2536(5) 0.043(2) Uani 1 1 d . . . H64A H 0.3040 0.9954 0.2158 0.052 Uiso 1 1 calc R . . C65 C 0.3370(6) 0.8503(6) 0.1840(5) 0.041(2) Uani 1 1 d . . . H65A H 0.3806 0.8109 0.2077 0.049 Uiso 1 1 calc R . . H65B H 0.3664 0.8981 0.1505 0.049 Uiso 1 1 calc R . . C66 C 0.3055(6) 0.8012(6) 0.1352(5) 0.046(2) Uani 1 1 d . . . H66A H 0.2619 0.8411 0.1117 0.056 Uiso 1 1 calc R . . H66B H 0.3563 0.7844 0.0940 0.056 Uiso 1 1 calc R . . C67 C 0.2651(6) 0.7223(5) 0.1779(5) 0.036(2) Uani 1 1 d . . . H67A H 0.3062 0.6841 0.2050 0.043 Uiso 1 1 calc R . . H67B H 0.2557 0.6912 0.1415 0.043 Uiso 1 1 calc R . . C68 C 0.1087(6) 0.7153(5) 0.2275(4) 0.034(2) Uani 1 1 d . . . H68A H 0.1176 0.6870 0.1860 0.040 Uiso 1 1 calc R . . C69 C 0.0197(6) 0.7237(5) 0.2786(4) 0.0314(19) Uani 1 1 d . . . C70 C -0.0509(6) 0.7081(5) 0.2547(5) 0.034(2) Uani 1 1 d . . . H70A H -0.0401 0.6951 0.2057 0.040 Uiso 1 1 calc R . . C71 C -0.1373(6) 0.7115(5) 0.3028(5) 0.034(2) Uani 1 1 d . . . C72 C -0.1523(7) 0.7297(5) 0.3768(5) 0.042(2) Uani 1 1 d . . . H72A H -0.2100 0.7334 0.4089 0.051 Uiso 1 1 calc R . . C73 C -0.0848(6) 0.7418(5) 0.4025(5) 0.038(2) Uani 1 1 d . . . H73A H -0.0963 0.7506 0.4530 0.046 Uiso 1 1 calc R . . C74 C 0.0051(6) 0.7413(5) 0.3536(5) 0.036(2) Uani 1 1 d . . . C80 C -0.0161(7) 0.9626(7) 0.2975(5) 0.056(3) Uani 1 1 d . . . H80A H -0.0408 1.0021 0.2589 0.085 Uiso 1 1 calc R . . H80B H -0.0082 0.9948 0.3332 0.085 Uiso 1 1 calc R . . H80C H -0.0561 0.9209 0.3247 0.085 Uiso 1 1 calc R . . C81 C 0.9221(12) 0.2332(12) 0.3758(9) 0.126(6) Uani 1 1 d . . . H81A H 0.9858 0.2313 0.3520 0.152 Uiso 1 1 calc R . . H81B H 0.9094 0.1763 0.3740 0.152 Uiso 1 1 calc R . . C82 C 0.9198(12) 0.2235(10) 0.4588(8) 0.115(6) Uani 1 1 d . . . H82A H 0.9631 0.1749 0.4717 0.173 Uiso 1 1 calc R . . H82B H 0.8612 0.2134 0.4900 0.173 Uiso 1 1 calc R . . H82C H 0.9338 0.2758 0.4681 0.173 Uiso 1 1 calc R . . C83 C 0.0231(15) 0.4188(12) 0.0732(11) 0.152(7) Uani 1 1 d DU . . C84 C 0.061(2) 0.3457(16) 0.1307(17) 0.217(13) Uani 1 1 d DU . . O1W O 0.4637(7) 0.9955(6) 0.2371(8) 0.149(5) Uani 1 1 d . . . O2W O 0.3778(7) 0.0401(8) 0.0211(9) 0.179(7) Uani 1 1 d . . . O3W O 0.4972(10) 0.0818(8) 0.0889(9) 0.176(7) Uani 1 1 d . . . O4W O 0.4537(17) 0.1309(16) 0.3365(11) 0.310(13) Uani 1 1 d . . . O5W O 0.3168(15) 0.2295(14) 0.1468(7) 0.261(11) Uani 1 1 d . . . O6W O 0.4488(17) 0.2788(14) 0.1871(13) 0.093(7) Uani 0.50 1 d P . . O6W' O 0.492(2) 0.2555(16) 0.236(2) 0.153(13) Uani 0.50 1 d P . . 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 0.0184(6) 0.0271(6) 0.0329(7) -0.0062(5) -0.0019(5) 0.0008(5) Fe2 0.0197(7) 0.0301(6) 0.0318(7) -0.0119(5) -0.0003(5) -0.0026(5) Mn1 0.0226(7) 0.0288(7) 0.0297(7) -0.0116(5) -0.0050(5) 0.0022(5) Mn2 0.0208(7) 0.0406(8) 0.0414(8) -0.0212(6) -0.0074(6) 0.0062(6) Cl1 0.073(2) 0.0528(16) 0.105(2) -0.0393(15) -0.0164(18) -0.0102(15) Cl2 0.0284(13) 0.0491(14) 0.0648(15) -0.0160(11) -0.0042(11) -0.0084(11) Cl3 0.0383(17) 0.081(2) 0.127(3) 0.0118(19) -0.0404(18) -0.0147(15) Cl4 0.099(3) 0.0377(14) 0.102(2) -0.0061(14) -0.050(2) -0.0185(15) O1 0.042(4) 0.052(4) 0.045(4) -0.023(3) -0.003(3) -0.009(3) O2 0.042(4) 0.037(4) 0.051(4) 0.000(3) -0.004(3) -0.020(3) O3 0.045(4) 0.043(4) 0.050(4) -0.013(3) 0.009(3) -0.017(3) O4 0.022(4) 0.067(5) 0.085(5) -0.012(4) -0.011(4) -0.007(3) O5 0.024(3) 0.038(3) 0.043(3) -0.016(3) -0.006(3) 0.002(3) O6 0.029(3) 0.033(3) 0.037(3) -0.013(2) -0.010(3) 0.000(3) O7 0.033(4) 0.045(4) 0.047(4) -0.021(3) -0.014(3) 0.003(3) O8 0.040(4) 0.057(4) 0.039(3) -0.022(3) 0.001(3) -0.012(3) O9 0.028(4) 0.048(4) 0.040(3) -0.025(3) -0.010(3) 0.012(3) O10 0.030(4) 0.045(3) 0.029(3) -0.015(3) -0.013(3) 0.006(3) N1 0.021(4) 0.033(4) 0.030(4) -0.009(3) -0.001(3) 0.004(3) N2 0.033(5) 0.043(4) 0.040(4) -0.010(3) -0.014(4) 0.006(4) N3 0.037(5) 0.034(4) 0.039(4) -0.009(3) -0.012(4) -0.001(3) N4 0.034(5) 0.053(5) 0.037(4) -0.019(4) -0.006(4) 0.008(4) N5 0.019(4) 0.022(3) 0.031(4) -0.012(3) -0.002(3) 0.009(3) N6 0.021(4) 0.034(4) 0.028(4) -0.006(3) -0.005(3) 0.002(3) N7 0.017(4) 0.036(4) 0.044(4) -0.006(3) -0.004(3) 0.002(3) N8 0.030(4) 0.032(4) 0.031(4) -0.003(3) -0.010(3) -0.003(3) N9 0.020(4) 0.036(4) 0.028(4) -0.016(3) 0.000(3) 0.000(3) N10 0.028(4) 0.031(4) 0.028(4) -0.011(3) -0.002(3) -0.004(3) N11 0.031(4) 0.038(4) 0.032(4) -0.018(3) -0.005(3) -0.006(3) N12 0.026(4) 0.032(4) 0.029(4) -0.018(3) -0.003(3) -0.001(3) N13 0.028(4) 0.035(4) 0.030(4) -0.018(3) -0.004(3) 0.002(3) N14 0.023(4) 0.035(4) 0.030(4) -0.014(3) -0.006(3) 0.002(3) N15 0.023(4) 0.042(4) 0.057(5) -0.030(4) -0.014(4) 0.009(3) N16 0.024(4) 0.037(4) 0.036(4) -0.018(3) -0.009(3) 0.004(3) N17 0.38(4) 0.183(18) 0.211(19) -0.133(15) -0.20(2) 0.077(19) C1 0.036(6) 0.028(4) 0.026(4) -0.009(3) 0.005(4) -0.009(4) C2 0.032(6) 0.034(5) 0.037(5) -0.007(4) -0.014(4) -0.008(4) C3 0.016(4) 0.035(5) 0.035(5) -0.015(4) 0.003(4) -0.003(3) C4 0.013(4) 0.040(5) 0.040(5) -0.017(4) 0.005(4) -0.004(4) C5 0.022(5) 0.022(4) 0.046(5) -0.008(4) -0.008(4) -0.002(3) C6 0.020(5) 0.047(5) 0.049(5) -0.018(4) -0.010(4) 0.007(4) C7 0.032(6) 0.035(5) 0.068(7) -0.023(5) -0.013(5) -0.004(4) C8 0.027(5) 0.039(5) 0.054(6) -0.010(4) -0.004(4) -0.004(4) C9 0.011(4) 0.019(4) 0.066(6) -0.012(4) -0.007(4) 0.001(3) C10 0.021(5) 0.049(6) 0.032(5) -0.006(4) -0.005(4) -0.005(4) C11 0.018(5) 0.037(5) 0.033(5) 0.001(4) 0.003(4) 0.009(4) C12 0.033(6) 0.058(6) 0.035(5) 0.001(4) -0.004(4) -0.015(5) C13 0.044(7) 0.069(7) 0.046(6) 0.007(5) 0.001(5) -0.023(6) C14 0.053(7) 0.058(6) 0.021(5) -0.003(4) 0.009(4) 0.002(5) C15 0.042(6) 0.046(6) 0.046(6) -0.018(4) -0.005(5) -0.002(5) C16 0.022(5) 0.030(5) 0.034(5) -0.001(4) -0.008(4) 0.008(4) C17 0.020(5) 0.035(5) 0.035(5) -0.014(4) -0.005(4) 0.001(4) C18 0.025(5) 0.033(5) 0.032(5) -0.004(4) -0.006(4) -0.002(4) C19 0.038(6) 0.023(4) 0.051(5) -0.009(4) -0.016(4) -0.002(4) C20 0.027(5) 0.027(4) 0.040(5) 0.006(4) -0.006(4) -0.006(4) C21 0.027(5) 0.042(5) 0.040(5) -0.013(4) 0.001(4) 0.000(4) C22 0.032(5) 0.039(5) 0.031(5) -0.010(4) -0.007(4) -0.007(4) C23 0.032(5) 0.040(5) 0.041(5) -0.009(4) -0.002(4) -0.007(4) C24 0.034(6) 0.027(5) 0.065(6) -0.005(4) -0.006(5) -0.003(4) C25 0.042(7) 0.053(6) 0.054(6) -0.005(5) -0.001(5) -0.018(5) C26 0.027(5) 0.057(6) 0.048(6) -0.011(5) -0.005(4) -0.006(5) C27 0.024(5) 0.043(5) 0.043(5) -0.020(4) -0.006(4) -0.009(4) C28 0.027(5) 0.048(6) 0.051(6) -0.019(4) -0.009(4) 0.001(4) C29 0.028(5) 0.040(5) 0.036(5) -0.025(4) -0.004(4) 0.006(4) C30 0.031(6) 0.055(6) 0.047(5) -0.025(5) -0.015(4) 0.003(4) C31 0.048(7) 0.055(7) 0.061(6) -0.031(5) -0.020(6) 0.028(5) C32 0.076(9) 0.041(6) 0.049(6) -0.012(5) -0.007(6) 0.008(6) C33 0.059(7) 0.031(5) 0.034(5) -0.006(4) 0.001(5) 0.007(5) C34 0.043(6) 0.030(5) 0.031(5) -0.016(4) -0.011(4) -0.002(4) C35 0.038(6) 0.037(5) 0.031(5) -0.018(4) 0.005(4) -0.015(4) C36 0.028(5) 0.038(5) 0.031(5) -0.012(4) 0.005(4) -0.010(4) C37 0.032(6) 0.056(6) 0.037(5) -0.014(4) 0.009(4) -0.019(5) C38 0.013(5) 0.060(7) 0.077(7) -0.023(5) 0.007(5) -0.009(5) C39 0.022(5) 0.055(6) 0.059(6) -0.015(5) -0.006(4) 0.004(5) C40 0.021(5) 0.028(5) 0.059(6) -0.008(4) -0.006(4) -0.004(4) C41 0.018(4) 0.023(4) 0.048(5) -0.012(4) -0.004(4) 0.002(3) C42 0.023(5) 0.034(5) 0.048(5) -0.009(4) -0.012(4) 0.001(4) C43 0.026(5) 0.040(5) 0.064(6) 0.003(5) -0.018(5) -0.004(4) C44 0.035(6) 0.045(6) 0.059(6) -0.008(5) -0.016(5) -0.012(4) C45 0.035(6) 0.053(6) 0.048(6) -0.018(5) -0.010(4) -0.005(5) C46 0.033(5) 0.035(5) 0.039(5) -0.013(4) -0.014(4) -0.004(4) C47 0.023(5) 0.042(5) 0.037(5) -0.018(4) -0.004(4) 0.000(4) C48 0.028(5) 0.037(5) 0.033(5) -0.013(4) -0.008(4) 0.007(4) C49 0.027(5) 0.050(5) 0.031(5) -0.017(4) -0.001(4) 0.002(4) C50 0.032(5) 0.036(5) 0.026(4) -0.005(4) -0.001(4) -0.001(4) C51 0.037(6) 0.028(4) 0.028(4) -0.006(3) -0.001(4) -0.006(4) C52 0.034(5) 0.024(4) 0.040(5) -0.004(4) -0.013(4) -0.002(4) C53 0.028(5) 0.030(5) 0.056(6) 0.001(4) -0.006(4) -0.005(4) C54 0.019(5) 0.036(5) 0.080(7) -0.014(5) -0.018(5) 0.001(4) C55 0.048(7) 0.036(5) 0.071(7) -0.023(5) -0.035(6) 0.005(5) C56 0.040(6) 0.037(5) 0.047(5) -0.020(4) -0.018(5) 0.007(4) C57 0.034(5) 0.025(4) 0.046(5) -0.029(4) -0.009(4) 0.002(4) C58 0.034(6) 0.039(5) 0.051(6) -0.017(4) -0.019(5) 0.000(4) C59 0.023(5) 0.050(6) 0.055(6) -0.024(5) -0.004(4) 0.001(4) C60 0.033(6) 0.055(6) 0.058(6) -0.027(5) -0.013(5) 0.000(5) C61 0.037(6) 0.045(6) 0.078(7) -0.033(5) -0.023(6) 0.013(5) C62 0.035(6) 0.050(6) 0.071(7) -0.015(5) -0.018(5) -0.008(5) C63 0.030(5) 0.044(5) 0.043(5) -0.023(4) -0.012(4) 0.003(4) C64 0.022(5) 0.052(6) 0.054(6) -0.023(5) 0.001(4) -0.003(4) C65 0.013(5) 0.054(6) 0.050(5) -0.019(4) -0.001(4) 0.007(4) C66 0.032(6) 0.050(6) 0.056(6) -0.025(5) -0.005(5) 0.003(5) C67 0.026(5) 0.035(5) 0.047(5) -0.023(4) -0.005(4) 0.005(4) C68 0.037(6) 0.029(4) 0.031(5) -0.012(4) -0.004(4) 0.002(4) C69 0.024(5) 0.038(5) 0.027(4) -0.009(4) 0.001(4) 0.000(4) C70 0.034(5) 0.031(5) 0.034(5) -0.009(4) -0.004(4) -0.001(4) C71 0.037(6) 0.014(4) 0.049(5) 0.000(4) -0.010(4) -0.006(4) C72 0.033(6) 0.034(5) 0.052(6) -0.011(4) 0.006(4) -0.007(4) C73 0.036(6) 0.041(5) 0.031(5) -0.016(4) 0.008(4) -0.006(4) C74 0.038(6) 0.035(5) 0.034(5) -0.010(4) 0.000(4) -0.012(4) C80 0.042(7) 0.073(7) 0.051(6) -0.036(5) -0.004(5) 0.013(5) C81 0.099(15) 0.181(18) 0.103(13) -0.064(12) -0.017(10) 0.002(13) C82 0.128(17) 0.109(12) 0.094(11) -0.027(9) -0.005(10) -0.009(11) C83 0.153(12) 0.170(10) 0.171(10) -0.115(8) -0.030(8) -0.033(8) C84 0.224(16) 0.221(15) 0.212(15) -0.063(10) -0.046(10) -0.034(10) O1W 0.047(6) 0.086(7) 0.288(15) 0.032(9) -0.049(8) -0.014(5) O2W 0.052(7) 0.138(10) 0.313(17) 0.069(11) -0.069(10) -0.022(7) O3W 0.183(15) 0.120(9) 0.276(16) 0.045(10) -0.167(14) -0.061(9) O4W 0.37(3) 0.35(3) 0.240(19) -0.096(19) -0.20(2) 0.11(2) O5W 0.32(3) 0.34(2) 0.099(10) -0.040(12) 0.069(12) -0.18(2) O6W 0.079(18) 0.059(12) 0.119(18) -0.051(12) 0.037(12) -0.016(11) O6W' 0.11(3) 0.072(16) 0.23(4) -0.09(2) 0.07(2) -0.008(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N7 1.892(7) . ? Fe1 N6 1.900(6) . ? Fe1 C2 1.956(9) . ? Fe1 C1 1.971(9) . ? Fe1 N5 1.997(6) . ? Fe1 N8 2.015(7) . ? Fe2 N11 1.902(7) . ? Fe2 N10 1.903(7) . ? Fe2 C4 1.967(9) . ? Fe2 C3 1.979(8) . ? Fe2 N12 1.992(7) . ? Fe2 N9 1.999(7) . ? Mn1 O5 1.884(6) . ? Mn1 O6 1.896(5) . ? Mn1 N13 2.033(7) . ? Mn1 N14 2.047(6) . ? Mn1 N1 2.251(7) . ? Mn1 O10 2.251(6) . ? Mn2 O7 1.884(6) . ? Mn2 O8 1.894(6) . ? Mn2 N16 2.015(6) . ? Mn2 N15 2.029(8) . ? Mn2 N2 2.207(7) . ? Mn2 O9 2.291(6) . ? Cl1 C61 1.761(10) . ? Cl2 C71 1.736(9) . ? Cl3 C54 1.755(9) . ? Cl4 C44 1.746(9) . ? O1 C17 1.247(9) . ? O2 C10 1.245(9) . ? O3 C35 1.240(9) . ? O4 C28 1.274(11) . ? O5 C57 1.327(10) . ? O6 C41 1.321(9) . ? O7 C58 1.323(10) . ? O8 C74 1.329(10) . ? O9 C80 1.446(10) . ? O9 H9A 0.8499 . ? O10 C81 1.381(17) . ? O10 H10A 0.8532 . ? N1 C1 1.145(10) . ? N2 C2 1.157(11) . ? N3 C3 1.149(9) . ? N4 C4 1.139(10) . ? N5 C22 1.341(10) . ? N5 C18 1.371(10) . ? N6 C17 1.333(10) . ? N6 C16 1.408(10) . ? N7 C10 1.336(11) . ? N7 C11 1.420(10) . ? N8 C9 1.340(10) . ? N8 C5 1.349(10) . ? N9 C23 1.336(10) . ? N9 C27 1.338(10) . ? N10 C28 1.328(11) . ? N10 C29 1.402(10) . ? N11 C35 1.348(11) . ? N11 C34 1.398(11) . ? N12 C40 1.329(10) . ? N12 C36 1.351(10) . ? N13 C51 1.295(10) . ? N13 C50 1.466(10) . ? N14 C47 1.271(10) . ? N14 C48 1.483(9) . ? N15 C64 1.282(10) . ? N15 C65 1.516(10) . ? N16 C68 1.307(11) . ? N16 C67 1.494(10) . ? N17 C84 1.195(10) . ? C5 C6 1.379(11) . ? C5 H5A 0.9300 . ? C6 C7 1.416(12) . ? C6 H6A 0.9300 . ? C7 C8 1.377(12) . ? C7 H7A 0.9300 . ? C8 C9 1.400(11) . ? C8 H8A 0.9300 . ? C9 C10 1.494(12) . ? C11 C16 1.405(12) . ? C11 C12 1.407(11) . ? C12 C13 1.360(13) . ? C12 H12A 0.9300 . ? C13 C14 1.396(14) . ? C13 H13A 0.9300 . ? C14 C15 1.385(12) . ? C14 H14A 0.9300 . ? C15 C16 1.412(12) . ? C15 H15A 0.9300 . ? C17 C18 1.498(11) . ? C18 C19 1.373(11) . ? C19 C20 1.400(12) . ? C19 H19A 0.9300 . ? C20 C21 1.377(11) . ? C20 H20A 0.9300 . ? C21 C22 1.372(11) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.369(11) . ? C23 H23A 0.9300 . ? C24 C25 1.393(13) . ? C24 H24A 0.9300 . ? C25 C26 1.375(13) . ? C25 H25A 0.9300 . ? C26 C27 1.411(12) . ? C26 H26A 0.9300 . ? C27 C28 1.469(12) . ? C29 C34 1.402(12) . ? C29 C30 1.425(12) . ? C30 C31 1.373(13) . ? C30 H30A 0.9300 . ? C31 C32 1.374(15) . ? C31 H31A 0.9300 . ? C32 C33 1.410(15) . ? C32 H32A 0.9300 . ? C33 C34 1.403(11) . ? C33 H33A 0.9300 . ? C35 C36 1.494(12) . ? C36 C37 1.398(12) . ? C37 C38 1.395(14) . ? C37 H37A 0.9300 . ? C38 C39 1.366(13) . ? C38 H38A 0.9300 . ? C39 C40 1.409(12) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 C42 1.402(11) . ? C41 C46 1.412(11) . ? C42 C43 1.381(12) . ? C42 H42A 0.9300 . ? C43 C44 1.391(13) . ? C43 H43A 0.9300 . ? C44 C45 1.364(12) . ? C45 C46 1.404(12) . ? C45 H45A 0.9300 . ? C46 C47 1.441(11) . ? C47 H47A 0.9300 . ? C48 C49 1.521(11) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.510(11) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.454(11) . ? C51 H51A 0.9300 . ? C52 C57 1.385(11) . ? C52 C53 1.437(12) . ? C53 C54 1.369(12) . ? C53 H53A 0.9300 . ? C54 C55 1.380(13) . ? C55 C56 1.356(13) . ? C55 H55A 0.9300 . ? C56 C57 1.408(11) . ? C56 H56A 0.9300 . ? C58 C63 1.397(12) . ? C58 C59 1.418(12) . ? C59 C60 1.340(12) . ? C59 H59A 0.9300 . ? C60 C61 1.409(14) . ? C60 H60A 0.9300 . ? C61 C62 1.373(13) . ? C62 C63 1.422(12) . ? C62 H62A 0.9300 . ? C63 C64 1.455(12) . ? C64 H64A 0.9300 . ? C65 C66 1.540(12) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.479(12) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.445(11) . ? C68 H68A 0.9300 . ? C69 C70 1.390(12) . ? C69 C74 1.412(11) . ? C70 C71 1.392(12) . ? C70 H70A 0.9300 . ? C71 C72 1.397(12) . ? C72 C73 1.343(12) . ? C72 H72A 0.9300 . ? C73 C74 1.442(12) . ? C73 H73A 0.9300 . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 C82 1.492(18) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 C84 1.549(10) . ? O6W O6W' 1.23(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Fe1 N6 84.1(3) . . ? N7 Fe1 C2 93.0(3) . . ? N6 Fe1 C2 96.8(3) . . ? N7 Fe1 C1 95.1(3) . . ? N6 Fe1 C1 89.9(3) . . ? C2 Fe1 C1 170.0(3) . . ? N7 Fe1 N5 165.6(3) . . ? N6 Fe1 N5 82.1(3) . . ? C2 Fe1 N5 84.4(3) . . ? C1 Fe1 N5 89.2(3) . . ? N7 Fe1 N8 81.2(3) . . ? N6 Fe1 N8 164.7(3) . . ? C2 Fe1 N8 88.5(3) . . ? C1 Fe1 N8 86.9(3) . . ? N5 Fe1 N8 112.8(3) . . ? N11 Fe2 N10 83.1(3) . . ? N11 Fe2 C4 98.8(3) . . ? N10 Fe2 C4 97.1(3) . . ? N11 Fe2 C3 91.8(3) . . ? N10 Fe2 C3 94.4(3) . . ? C4 Fe2 C3 165.2(3) . . ? N11 Fe2 N12 82.4(3) . . ? N10 Fe2 N12 165.5(3) . . ? C4 Fe2 N12 83.6(3) . . ? C3 Fe2 N12 87.7(3) . . ? N11 Fe2 N9 165.0(3) . . ? N10 Fe2 N9 81.9(3) . . ? C4 Fe2 N9 84.4(3) . . ? C3 Fe2 N9 88.1(3) . . ? N12 Fe2 N9 112.6(3) . . ? O5 Mn1 O6 89.1(2) . . ? O5 Mn1 N13 89.9(3) . . ? O6 Mn1 N13 177.2(3) . . ? O5 Mn1 N14 176.7(2) . . ? O6 Mn1 N14 88.9(2) . . ? N13 Mn1 N14 91.9(3) . . ? O5 Mn1 N1 94.6(2) . . ? O6 Mn1 N1 94.3(2) . . ? N13 Mn1 N1 88.4(3) . . ? N14 Mn1 N1 88.2(3) . . ? O5 Mn1 O10 86.4(2) . . ? O6 Mn1 O10 88.2(2) . . ? N13 Mn1 O10 89.1(2) . . ? N14 Mn1 O10 90.8(2) . . ? N1 Mn1 O10 177.3(2) . . ? O7 Mn2 O8 88.2(3) . . ? O7 Mn2 N16 175.5(3) . . ? O8 Mn2 N16 89.7(3) . . ? O7 Mn2 N15 89.9(3) . . ? O8 Mn2 N15 174.1(3) . . ? N16 Mn2 N15 91.7(3) . . ? O7 Mn2 N2 95.0(3) . . ? O8 Mn2 N2 98.9(3) . . ? N16 Mn2 N2 89.2(3) . . ? N15 Mn2 N2 86.9(3) . . ? O7 Mn2 O9 88.1(2) . . ? O8 Mn2 O9 90.0(3) . . ? N16 Mn2 O9 87.9(2) . . ? N15 Mn2 O9 84.3(3) . . ? N2 Mn2 O9 170.6(3) . . ? C57 O5 Mn1 124.3(5) . . ? C41 O6 Mn1 125.2(5) . . ? C58 O7 Mn2 128.3(5) . . ? C74 O8 Mn2 123.0(5) . . ? C80 O9 Mn2 129.1(5) . . ? C80 O9 H9A 109.3 . . ? Mn2 O9 H9A 109.2 . . ? C81 O10 Mn1 123.4(8) . . ? C81 O10 H10A 108.9 . . ? Mn1 O10 H10A 109.5 . . ? C1 N1 Mn1 166.7(6) . . ? C2 N2 Mn2 158.3(7) . . ? C22 N5 C18 118.0(7) . . ? C22 N5 Fe1 129.5(5) . . ? C18 N5 Fe1 111.9(5) . . ? C17 N6 C16 126.6(7) . . ? C17 N6 Fe1 118.7(5) . . ? C16 N6 Fe1 114.2(5) . . ? C10 N7 C11 126.0(7) . . ? C10 N7 Fe1 119.3(6) . . ? C11 N7 Fe1 114.2(6) . . ? C9 N8 C5 119.4(7) . . ? C9 N8 Fe1 112.0(5) . . ? C5 N8 Fe1 128.6(5) . . ? C23 N9 C27 117.3(7) . . ? C23 N9 Fe2 130.3(6) . . ? C27 N9 Fe2 112.3(5) . . ? C28 N10 C29 128.1(8) . . ? C28 N10 Fe2 117.4(6) . . ? C29 N10 Fe2 114.5(5) . . ? C35 N11 C34 126.5(7) . . ? C35 N11 Fe2 118.1(6) . . ? C34 N11 Fe2 115.1(6) . . ? C40 N12 C36 117.7(7) . . ? C40 N12 Fe2 129.8(6) . . ? C36 N12 Fe2 112.4(5) . . ? C51 N13 C50 117.4(7) . . ? C51 N13 Mn1 120.6(5) . . ? C50 N13 Mn1 122.0(5) . . ? C47 N14 C48 118.4(7) . . ? C47 N14 Mn1 120.6(5) . . ? C48 N14 Mn1 120.9(5) . . ? C64 N15 C65 115.4(8) . . ? C64 N15 Mn2 122.2(6) . . ? C65 N15 Mn2 122.4(5) . . ? C68 N16 C67 116.6(7) . . ? C68 N16 Mn2 121.4(6) . . ? C67 N16 Mn2 122.0(5) . . ? N1 C1 Fe1 176.5(7) . . ? N2 C2 Fe1 179.6(8) . . ? N3 C3 Fe2 177.4(7) . . ? N4 C4 Fe2 174.3(8) . . ? N8 C5 C6 121.9(7) . . ? N8 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C7 119.2(8) . . ? C5 C6 H6A 120.4 . . ? C7 C6 H6A 120.4 . . ? C8 C7 C6 118.2(8) . . ? C8 C7 H7A 120.9 . . ? C6 C7 H7A 120.9 . . ? C7 C8 C9 119.4(8) . . ? C7 C8 H8A 120.3 . . ? C9 C8 H8A 120.3 . . ? N8 C9 C8 121.8(8) . . ? N8 C9 C10 116.0(7) . . ? C8 C9 C10 122.2(7) . . ? O2 C10 N7 128.9(8) . . ? O2 C10 C9 120.9(8) . . ? N7 C10 C9 110.1(7) . . ? C16 C11 C12 120.5(8) . . ? C16 C11 N7 113.4(7) . . ? C12 C11 N7 126.0(8) . . ? C13 C12 C11 117.8(9) . . ? C13 C12 H12A 121.1 . . ? C11 C12 H12A 121.1 . . ? C12 C13 C14 122.9(9) . . ? C12 C13 H13A 118.6 . . ? C14 C13 H13A 118.6 . . ? C15 C14 C13 120.1(9) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 118.4(9) . . ? C14 C15 H15A 120.8 . . ? C16 C15 H15A 120.8 . . ? C11 C16 N6 113.9(7) . . ? C11 C16 C15 120.2(8) . . ? N6 C16 C15 126.0(8) . . ? O1 C17 N6 128.7(7) . . ? O1 C17 C18 120.1(7) . . ? N6 C17 C18 111.1(7) . . ? N5 C18 C19 121.6(7) . . ? N5 C18 C17 115.1(7) . . ? C19 C18 C17 123.2(7) . . ? C18 C19 C20 119.3(8) . . ? C18 C19 H19A 120.3 . . ? C20 C19 H19A 120.3 . . ? C21 C20 C19 118.6(8) . . ? C21 C20 H20A 120.7 . . ? C19 C20 H20A 120.7 . . ? C22 C21 C20 119.5(8) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? N5 C22 C21 122.7(8) . . ? N5 C22 H22A 118.7 . . ? C21 C22 H22A 118.7 . . ? N9 C23 C24 124.3(9) . . ? N9 C23 H23A 117.8 . . ? C24 C23 H23A 117.8 . . ? C23 C24 C25 119.2(9) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C26 C25 C24 117.3(9) . . ? C26 C25 H25A 121.3 . . ? C24 C25 H25A 121.3 . . ? C25 C26 C27 120.1(9) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? N9 C27 C26 121.7(8) . . ? N9 C27 C28 115.4(8) . . ? C26 C27 C28 122.9(8) . . ? O4 C28 N10 126.0(8) . . ? O4 C28 C27 121.1(9) . . ? N10 C28 C27 112.8(8) . . ? N10 C29 C34 114.0(8) . . ? N10 C29 C30 126.7(8) . . ? C34 C29 C30 119.3(8) . . ? C31 C30 C29 118.6(9) . . ? C31 C30 H30A 120.7 . . ? C29 C30 H30A 120.7 . . ? C30 C31 C32 123.4(10) . . ? C30 C31 H31A 118.3 . . ? C32 C31 H31A 118.3 . . ? C31 C32 C33 118.5(9) . . ? C31 C32 H32A 120.8 . . ? C33 C32 H32A 120.8 . . ? C34 C33 C32 120.0(10) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? N11 C34 C33 126.6(9) . . ? N11 C34 C29 113.2(7) . . ? C33 C34 C29 120.2(9) . . ? O3 C35 N11 127.7(9) . . ? O3 C35 C36 121.1(8) . . ? N11 C35 C36 111.1(7) . . ? N12 C36 C37 122.3(8) . . ? N12 C36 C35 115.7(8) . . ? C37 C36 C35 122.0(8) . . ? C38 C37 C36 119.2(8) . . ? C38 C37 H37A 120.4 . . ? C36 C37 H37A 120.4 . . ? C39 C38 C37 118.6(9) . . ? C39 C38 H38A 120.7 . . ? C37 C38 H38A 120.7 . . ? C38 C39 C40 118.9(9) . . ? C38 C39 H39A 120.6 . . ? C40 C39 H39A 120.6 . . ? N12 C40 C39 123.3(8) . . ? N12 C40 H40A 118.3 . . ? C39 C40 H40A 118.3 . . ? O6 C41 C42 118.6(7) . . ? O6 C41 C46 122.7(7) . . ? C42 C41 C46 118.7(7) . . ? C43 C42 C41 121.1(8) . . ? C43 C42 H42A 119.4 . . ? C41 C42 H42A 119.4 . . ? C42 C43 C44 119.9(8) . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C45 C44 C43 119.8(8) . . ? C45 C44 Cl4 120.3(7) . . ? C43 C44 Cl4 119.8(7) . . ? C44 C45 C46 121.7(8) . . ? C44 C45 H45A 119.2 . . ? C46 C45 H45A 119.2 . . ? C45 C46 C41 118.7(7) . . ? C45 C46 C47 119.9(7) . . ? C41 C46 C47 121.2(7) . . ? N14 C47 C46 127.6(7) . . ? N14 C47 H47A 116.2 . . ? C46 C47 H47A 116.2 . . ? N14 C48 C49 113.9(7) . . ? N14 C48 H48A 108.8 . . ? C49 C48 H48A 108.8 . . ? N14 C48 H48B 108.8 . . ? C49 C48 H48B 108.8 . . ? H48A C48 H48B 107.7 . . ? C50 C49 C48 113.1(7) . . ? C50 C49 H49A 109.0 . . ? C48 C49 H49A 109.0 . . ? C50 C49 H49B 109.0 . . ? C48 C49 H49B 109.0 . . ? H49A C49 H49B 107.8 . . ? N13 C50 C49 112.9(7) . . ? N13 C50 H50A 109.0 . . ? C49 C50 H50A 109.0 . . ? N13 C50 H50B 109.0 . . ? C49 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? N13 C51 C52 125.7(8) . . ? N13 C51 H51A 117.2 . . ? C52 C51 H51A 117.2 . . ? C57 C52 C53 120.6(8) . . ? C57 C52 C51 123.4(8) . . ? C53 C52 C51 115.9(7) . . ? C54 C53 C52 117.8(8) . . ? C54 C53 H53A 121.1 . . ? C52 C53 H53A 121.1 . . ? C53 C54 C55 122.1(9) . . ? C53 C54 Cl3 117.7(8) . . ? C55 C54 Cl3 120.2(7) . . ? C56 C55 C54 119.6(8) . . ? C56 C55 H55A 120.2 . . ? C54 C55 H55A 120.2 . . ? C55 C56 C57 121.8(9) . . ? C55 C56 H56A 119.1 . . ? C57 C56 H56A 119.1 . . ? O5 C57 C52 121.7(7) . . ? O5 C57 C56 120.2(8) . . ? C52 C57 C56 118.0(8) . . ? O7 C58 C63 122.2(8) . . ? O7 C58 C59 118.4(8) . . ? C63 C58 C59 119.5(8) . . ? C60 C59 C58 121.1(9) . . ? C60 C59 H59A 119.5 . . ? C58 C59 H59A 119.5 . . ? C59 C60 C61 119.9(9) . . ? C59 C60 H60A 120.0 . . ? C61 C60 H60A 120.0 . . ? C62 C61 C60 121.1(9) . . ? C62 C61 Cl1 119.2(9) . . ? C60 C61 Cl1 119.6(7) . . ? C61 C62 C63 119.3(9) . . ? C61 C62 H62A 120.4 . . ? C63 C62 H62A 120.4 . . ? C58 C63 C62 119.1(8) . . ? C58 C63 C64 122.1(8) . . ? C62 C63 C64 118.0(9) . . ? N15 C64 C63 126.7(9) . . ? N15 C64 H64A 116.7 . . ? C63 C64 H64A 116.7 . . ? N15 C65 C66 113.0(7) . . ? N15 C65 H65A 109.0 . . ? C66 C65 H65A 109.0 . . ? N15 C65 H65B 109.0 . . ? C66 C65 H65B 109.0 . . ? H65A C65 H65B 107.8 . . ? C67 C66 C65 115.1(7) . . ? C67 C66 H66A 108.5 . . ? C65 C66 H66A 108.5 . . ? C67 C66 H66B 108.5 . . ? C65 C66 H66B 108.5 . . ? H66A C66 H66B 107.5 . . ? C66 C67 N16 112.2(7) . . ? C66 C67 H67A 109.2 . . ? N16 C67 H67A 109.2 . . ? C66 C67 H67B 109.2 . . ? N16 C67 H67B 109.2 . . ? H67A C67 H67B 107.9 . . ? N16 C68 C69 125.9(8) . . ? N16 C68 H68A 117.0 . . ? C69 C68 H68A 117.0 . . ? C70 C69 C74 120.1(8) . . ? C70 C69 C68 118.8(8) . . ? C74 C69 C68 120.9(8) . . ? C69 C70 C71 121.3(8) . . ? C69 C70 H70A 119.3 . . ? C71 C70 H70A 119.3 . . ? C70 C71 C72 118.7(8) . . ? C70 C71 Cl2 121.4(7) . . ? C72 C71 Cl2 119.9(7) . . ? C73 C72 C71 121.2(9) . . ? C73 C72 H72A 119.4 . . ? C71 C72 H72A 119.4 . . ? C72 C73 C74 121.5(8) . . ? C72 C73 H73A 119.2 . . ? C74 C73 H73A 119.2 . . ? O8 C74 C69 123.2(8) . . ? O8 C74 C73 119.8(8) . . ? C69 C74 C73 117.0(8) . . ? O9 C80 H80A 109.5 . . ? O9 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? O9 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O10 C81 C82 143.4(15) . . ? O10 C81 H81A 101.1 . . ? C82 C81 H81A 101.1 . . ? O10 C81 H81B 101.1 . . ? C82 C81 H81B 101.1 . . ? H81A C81 H81B 104.5 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N17 C84 C83 168(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10A N4 0.853 1.887 2.725(4) 166.69 2_665 O9 H9A N3 0.850 1.967 2.793(4) 163.94 . _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.237 _refine_diff_density_min -0.856 _refine_diff_density_rms 0.145