# 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 'Ming-Liang Tong' _publ_contact_author_email TONGML@MAIL.SYSU.EDU.CN _publ_section_title ; High-Spin Tetranuclear MnII2MnIV2 Clusters with Unique Mn(II)-Mn(IV) Magnetic Exchange. Synthesis, Structures and Magnetism of Mn4 and Fe4 Clusters with Tetrakis(2-hydroxyethyl)ethylenediamine ; loop_ _publ_author_name 'Ming-Liang Tong' 'Radovan Herchel' 'Ji-Dong Leng' 'Jun-Liang Liu' 'Ai-Ju Zhou' # Attachment 'CIF_B823042K.cif' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 679168' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H63 Mn4 N5 O14' _chemical_formula_weight 961.63 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' _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 11.7430(8) _cell_length_b 16.1528(11) _cell_length_c 23.0734(16) _cell_angle_alpha 70.345(1) _cell_angle_beta 85.093(1) _cell_angle_gamma 79.832(1) _cell_volume 4055.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5042 _cell_measurement_theta_min 2.416 _cell_measurement_theta_max 26.525 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 1.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7409 _exptl_absorpt_correction_T_max 0.8641 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; Several restraints were employed to fix the geometries of the solvated acetonitrile molecules. The 93.4% data completeness may be due to the irregular shape of the collected crystal. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23165 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14898 _reflns_number_gt 10937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 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^)+(0.0622P)^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 14898 _refine_ls_number_parameters 997 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.67733(4) -0.04388(3) 0.31884(2) 0.02830(13) Uani 1 1 d . . . Mn2 Mn 0.95089(4) -0.03319(3) 0.30606(2) 0.02773(13) Uani 1 1 d . . . Mn3 Mn 0.80653(4) 0.03294(3) 0.17966(2) 0.02757(13) Uani 1 1 d . . . Mn4 Mn 0.53211(4) 0.02369(3) 0.19269(2) 0.02864(13) Uani 1 1 d . . . Mn5 Mn 0.25147(5) 0.53511(3) 0.30539(2) 0.03329(14) Uani 1 1 d . . . Mn6 Mn 0.03246(5) 0.43211(4) 0.31920(2) 0.03425(14) Uani 1 1 d . . . Mn7 Mn 0.19904(5) 0.45229(3) 0.19526(2) 0.03217(14) Uani 1 1 d . . . Mn8 Mn 0.41828(5) 0.55459(3) 0.18161(2) 0.03312(14) Uani 1 1 d . . . O1 O 0.53205(19) 0.04287(15) 0.27115(11) 0.0334(5) Uani 1 1 d . . . O2 O 0.80380(17) 0.04681(14) 0.27292(10) 0.0269(5) Uani 1 1 d . . . O3 O 0.84743(19) -0.12084(14) 0.33802(10) 0.0321(5) Uani 1 1 d . . . O4 O 0.5583(2) -0.15296(17) 0.33440(11) 0.0445(6) Uani 1 1 d . . . H4O H 0.5090 -0.1255 0.3067 0.053 Uiso 1 1 d R . . O5 O 0.67909(17) -0.05726(14) 0.22503(10) 0.0271(5) Uani 1 1 d . . . O6 O 0.95362(19) -0.05262(14) 0.22728(10) 0.0312(5) Uani 1 1 d . . . O7 O 0.9247(2) 0.14289(17) 0.16442(11) 0.0430(6) Uani 1 1 d . . . H7O H 0.9738 0.1182 0.1926 0.052 Uiso 1 1 d R . . O8 O 0.63614(19) 0.11046(14) 0.15927(10) 0.0325(5) Uani 1 1 d . . . O9 O 0.93088(19) -0.00179(16) 0.37683(11) 0.0369(6) Uani 1 1 d . . . O10 O 1.07959(19) -0.11498(15) 0.33454(11) 0.0380(6) Uani 1 1 d . . . O11 O 1.03865(19) 0.05762(15) 0.26764(11) 0.0357(6) Uani 1 1 d . . . O12 O 0.54776(19) -0.00747(16) 0.12194(11) 0.0373(6) Uani 1 1 d . . . O13 O 0.40337(19) 0.10580(15) 0.16524(11) 0.0373(6) Uani 1 1 d . . . O14 O 0.4445(2) -0.06721(16) 0.23236(11) 0.0387(6) Uani 1 1 d . . . O15 O 0.0654(2) 0.54698(15) 0.31511(11) 0.0392(6) Uani 1 1 d . . . O16 O 0.2846(2) 0.68279(16) 0.27349(12) 0.0485(7) Uani 1 1 d . . . H16O H 0.3372 0.6872 0.2454 0.058 Uiso 1 1 d R . . O17 O 0.4245(2) 0.51219(15) 0.27080(10) 0.0371(6) Uani 1 1 d . . . O18 O 0.20115(19) 0.41061(14) 0.29903(10) 0.0321(5) Uani 1 1 d . . . O19 O 0.0256(2) 0.47469(16) 0.23012(10) 0.0386(6) Uani 1 1 d . . . O20 O 0.24920(19) 0.57632(14) 0.20154(10) 0.0319(5) Uani 1 1 d . . . O21 O 0.3850(2) 0.43936(15) 0.18566(11) 0.0360(6) Uani 1 1 d . . . O22 O 0.1664(2) 0.30490(16) 0.22701(11) 0.0440(7) Uani 1 1 d . . . H22O H 0.1143 0.3033 0.2551 0.053 Uiso 1 1 d R . . O23 O 0.0546(2) 0.38599(17) 0.40309(11) 0.0429(6) Uani 1 1 d . . . O24 O -0.1240(2) 0.46231(17) 0.32988(12) 0.0458(7) Uani 1 1 d . . . O25 O 0.0146(2) 0.31955(16) 0.31721(11) 0.0399(6) Uani 1 1 d . . . O26 O 0.3945(2) 0.60152(16) 0.09804(11) 0.0396(6) Uani 1 1 d . . . O27 O 0.5745(2) 0.52323(16) 0.17037(12) 0.0430(6) Uani 1 1 d . . . O28 O 0.4375(2) 0.66679(15) 0.18376(11) 0.0403(6) Uani 1 1 d . . . N1 N 0.6369(2) 0.07413(19) 0.36319(13) 0.0337(7) Uani 1 1 d . . . N2 N 0.6639(2) -0.1197(2) 0.42629(13) 0.0370(7) Uani 1 1 d . . . N3 N 0.8475(2) -0.08550(19) 0.13543(13) 0.0332(7) Uani 1 1 d . . . N4 N 0.8212(2) 0.1078(2) 0.07288(13) 0.0364(7) Uani 1 1 d . . . N5 N 0.2128(3) 0.58592(19) 0.39074(14) 0.0434(8) Uani 1 1 d . . . N6 N 0.3495(3) 0.41672(19) 0.38772(13) 0.0386(7) Uani 1 1 d . . . N7 N 0.0997(3) 0.5713(2) 0.11264(13) 0.0386(7) Uani 1 1 d . . . N8 N 0.2364(3) 0.40220(19) 0.10974(13) 0.0398(7) Uani 1 1 d . . . C1 C 0.6476(3) 0.0339(3) 0.43075(17) 0.0433(9) Uani 1 1 d . . . H1A H 0.6027 0.0742 0.4503 0.052 Uiso 1 1 calc R . . H1B H 0.7280 0.0268 0.4410 0.052 Uiso 1 1 calc R . . C2 C 0.6067(3) -0.0555(3) 0.45616(17) 0.0447(10) Uani 1 1 d . . . H2A H 0.6208 -0.0801 0.4999 0.054 Uiso 1 1 calc R . . H2B H 0.5238 -0.0469 0.4510 0.054 Uiso 1 1 calc R . . C3 C 0.5167(3) 0.1148(3) 0.34617(17) 0.0411(9) Uani 1 1 d . . . H3A H 0.5009 0.1727 0.3517 0.049 Uiso 1 1 calc R . . H3B H 0.4644 0.0779 0.3736 0.049 Uiso 1 1 calc R . . C4 C 0.4930(3) 0.1256(2) 0.28004(17) 0.0388(9) Uani 1 1 d . . . H4A H 0.4108 0.1434 0.2726 0.047 Uiso 1 1 calc R . . H4B H 0.5338 0.1710 0.2518 0.047 Uiso 1 1 calc R . . C5 C 0.7190(3) 0.1369(2) 0.33717(16) 0.0355(8) Uani 1 1 d . . . H5A H 0.7805 0.1235 0.3660 0.043 Uiso 1 1 calc R . . H5B H 0.6793 0.1967 0.3325 0.043 Uiso 1 1 calc R . . C6 C 0.7726(3) 0.1348(2) 0.27511(16) 0.0328(8) Uani 1 1 d . . . H6A H 0.7179 0.1685 0.2431 0.039 Uiso 1 1 calc R . . H6B H 0.8410 0.1635 0.2668 0.039 Uiso 1 1 calc R . . C7 C 0.7857(3) -0.1528(3) 0.44495(17) 0.0442(10) Uani 1 1 d . . . H7A H 0.7878 -0.2011 0.4838 0.053 Uiso 1 1 calc R . . H7B H 0.8185 -0.1053 0.4509 0.053 Uiso 1 1 calc R . . C8 C 0.8582(3) -0.1854(2) 0.39696(17) 0.0423(9) Uani 1 1 d . . . H8A H 0.9388 -0.1997 0.4082 0.051 Uiso 1 1 calc R . . H8B H 0.8339 -0.2393 0.3961 0.051 Uiso 1 1 calc R . . C9 C 0.5986(3) -0.1935(3) 0.43857(17) 0.0449(10) Uani 1 1 d . . . H9A H 0.5651 -0.2070 0.4800 0.054 Uiso 1 1 calc R . . H9B H 0.6510 -0.2460 0.4363 0.054 Uiso 1 1 calc R . . C10 C 0.5032(3) -0.1717(3) 0.39317(17) 0.0439(10) Uani 1 1 d . . . H10A H 0.4622 -0.2218 0.4015 0.053 Uiso 1 1 calc R . . H10B H 0.4484 -0.1204 0.3957 0.053 Uiso 1 1 calc R . . C11 C 0.8410(3) -0.0459(3) 0.06795(16) 0.0420(9) Uani 1 1 d . . . H11A H 0.7616 -0.0389 0.0562 0.050 Uiso 1 1 calc R . . H11B H 0.8880 -0.0863 0.0491 0.050 Uiso 1 1 calc R . . C12 C 0.8819(3) 0.0435(3) 0.04362(17) 0.0428(9) Uani 1 1 d . . . H12A H 0.9642 0.0350 0.0503 0.051 Uiso 1 1 calc R . . H12B H 0.8706 0.0680 -0.0004 0.051 Uiso 1 1 calc R . . C13 C 0.7621(3) -0.1467(2) 0.16022(17) 0.0375(9) Uani 1 1 d . . . H13A H 0.7996 -0.2068 0.1642 0.045 Uiso 1 1 calc R . . H13B H 0.7007 -0.1309 0.1310 0.045 Uiso 1 1 calc R . . C14 C 0.7089(3) -0.1453(2) 0.22253(17) 0.0353(8) Uani 1 1 d . . . H14A H 0.6399 -0.1733 0.2307 0.042 Uiso 1 1 calc R . . H14B H 0.7634 -0.1797 0.2544 0.042 Uiso 1 1 calc R . . C15 C 0.9663(3) -0.1282(2) 0.15438(17) 0.0406(9) Uani 1 1 d . . . H15A H 1.0206 -0.0938 0.1266 0.049 Uiso 1 1 calc R . . H15B H 0.9800 -0.1871 0.1505 0.049 Uiso 1 1 calc R . . C16 C 0.9895(3) -0.1363(2) 0.21991(17) 0.0373(9) Uani 1 1 d . . . H16A H 0.9470 -0.1800 0.2488 0.045 Uiso 1 1 calc R . . H16B H 1.0713 -0.1555 0.2278 0.045 Uiso 1 1 calc R . . C17 C 0.8843(3) 0.1832(2) 0.06021(17) 0.0427(9) Uani 1 1 d . . . H17A H 0.8304 0.2352 0.0622 0.051 Uiso 1 1 calc R . . H17B H 0.9181 0.1967 0.0189 0.051 Uiso 1 1 calc R . . C18 C 0.9785(3) 0.1638(3) 0.10529(17) 0.0437(9) Uani 1 1 d . . . H18A H 1.0357 0.1140 0.1023 0.052 Uiso 1 1 calc R . . H18B H 1.0167 0.2153 0.0970 0.052 Uiso 1 1 calc R . . C19 C 0.6993(3) 0.1389(3) 0.05284(17) 0.0430(9) Uani 1 1 d . . . H19A H 0.6679 0.0899 0.0481 0.052 Uiso 1 1 calc R . . H19B H 0.6973 0.1858 0.0133 0.052 Uiso 1 1 calc R . . C20 C 0.6254(3) 0.1736(2) 0.09974(17) 0.0427(9) Uani 1 1 d . . . H20A H 0.6492 0.2281 0.0997 0.051 Uiso 1 1 calc R . . H20B H 0.5450 0.1872 0.0882 0.051 Uiso 1 1 calc R . . C21 C 1.1382(3) 0.0029(2) 0.36559(16) 0.0351(8) Uani 1 1 d . . . C22 C 1.0289(3) -0.0014(3) 0.40636(17) 0.0407(9) Uani 1 1 d . . . H22A H 1.0408 -0.0548 0.4420 0.049 Uiso 1 1 calc R . . H22B H 1.0157 0.0494 0.4209 0.049 Uiso 1 1 calc R . . C23 C 1.1713(3) -0.0853(2) 0.35300(18) 0.0426(9) Uani 1 1 d . . . H23A H 1.2318 -0.0790 0.3211 0.051 Uiso 1 1 calc R . . H23B H 1.2031 -0.1305 0.3900 0.051 Uiso 1 1 calc R . . C24 C 1.1128(3) 0.0769(2) 0.30432(17) 0.0399(9) Uani 1 1 d . . . H24A H 1.0780 0.1312 0.3124 0.048 Uiso 1 1 calc R . . H24B H 1.1852 0.0875 0.2817 0.048 Uiso 1 1 calc R . . C25 C 1.2370(3) 0.0212(3) 0.3964(2) 0.0543(11) Uani 1 1 d . . . H25A H 1.2471 -0.0216 0.4369 0.081 Uiso 1 1 calc R . . H25B H 1.2186 0.0800 0.3993 0.081 Uiso 1 1 calc R . . H25C H 1.3072 0.0168 0.3723 0.081 Uiso 1 1 calc R . . C26 C 0.3405(3) -0.0123(2) 0.13629(17) 0.0363(8) Uani 1 1 d . . . C27 C 0.4486(3) -0.0104(3) 0.09449(17) 0.0412(9) Uani 1 1 d . . . H27A H 0.4610 -0.0630 0.0819 0.049 Uiso 1 1 calc R . . H27B H 0.4356 0.0412 0.0577 0.049 Uiso 1 1 calc R . . C28 C 0.3104(3) 0.0765(3) 0.1478(2) 0.0471(10) Uani 1 1 d . . . H28A H 0.2788 0.1213 0.1106 0.057 Uiso 1 1 calc R . . H28B H 0.2503 0.0716 0.1798 0.057 Uiso 1 1 calc R . . C29 C 0.3658(3) -0.0848(3) 0.19754(17) 0.0431(9) Uani 1 1 d . . . H29A H 0.2938 -0.0926 0.2212 0.052 Uiso 1 1 calc R . . H29B H 0.3963 -0.1404 0.1901 0.052 Uiso 1 1 calc R . . C30 C 0.2396(3) -0.0299(3) 0.1070(2) 0.0545(11) Uani 1 1 d . . . H30A H 0.1714 -0.0277 0.1329 0.082 Uiso 1 1 calc R . . H30B H 0.2579 -0.0877 0.1023 0.082 Uiso 1 1 calc R . . H30C H 0.2259 0.0146 0.0673 0.082 Uiso 1 1 calc R . . C31 C 0.2970(4) 0.5333(3) 0.43824(18) 0.0539(11) Uani 1 1 d . . . H31A H 0.2695 0.5414 0.4771 0.065 Uiso 1 1 calc R . . H31B H 0.3700 0.5557 0.4273 0.065 Uiso 1 1 calc R . . C32 C 0.3177(4) 0.4346(3) 0.44665(17) 0.0513(11) Uani 1 1 d . . . H32A H 0.3793 0.4049 0.4755 0.062 Uiso 1 1 calc R . . H32B H 0.2482 0.4098 0.4642 0.062 Uiso 1 1 calc R . . C33 C 0.0925(4) 0.5704(3) 0.41113(18) 0.0533(11) Uani 1 1 d . . . H33A H 0.0608 0.6075 0.4359 0.064 Uiso 1 1 calc R . . H33B H 0.0939 0.5087 0.4367 0.064 Uiso 1 1 calc R . . C34 C 0.0154(4) 0.5910(3) 0.35732(19) 0.0501(11) Uani 1 1 d . . . H34A H -0.0588 0.5725 0.3724 0.060 Uiso 1 1 calc R . . H34B H 0.0021 0.6547 0.3362 0.060 Uiso 1 1 calc R . . C35 C 0.2215(4) 0.6818(2) 0.37244(18) 0.0543(12) Uani 1 1 d . . . H35A H 0.2384 0.6958 0.4082 0.065 Uiso 1 1 calc R . . H35B H 0.1479 0.7170 0.3568 0.065 Uiso 1 1 calc R . . C36 C 0.3142(4) 0.7054(3) 0.32411(18) 0.0526(11) Uani 1 1 d . . . H36A H 0.3181 0.7685 0.3117 0.063 Uiso 1 1 calc R . . H36B H 0.3888 0.6722 0.3396 0.063 Uiso 1 1 calc R . . C37 C 0.4737(3) 0.4207(3) 0.37216(17) 0.0453(10) Uani 1 1 d . . . H37A H 0.5190 0.3648 0.3955 0.054 Uiso 1 1 calc R . . H37B H 0.4959 0.4676 0.3841 0.054 Uiso 1 1 calc R . . C38 C 0.5011(3) 0.4380(2) 0.30408(17) 0.0415(9) Uani 1 1 d . . . H38A H 0.5803 0.4490 0.2946 0.050 Uiso 1 1 calc R . . H38B H 0.4928 0.3865 0.2931 0.050 Uiso 1 1 calc R . . C39 C 0.3168(3) 0.3320(2) 0.38985(16) 0.0384(9) Uani 1 1 d . . . H39A H 0.2549 0.3182 0.4205 0.046 Uiso 1 1 calc R . . H39B H 0.3826 0.2853 0.4032 0.046 Uiso 1 1 calc R . . C40 C 0.2773(3) 0.3312(2) 0.32905(17) 0.0385(9) Uani 1 1 d . . . H40A H 0.3444 0.3249 0.3024 0.046 Uiso 1 1 calc R . . H40B H 0.2381 0.2804 0.3365 0.046 Uiso 1 1 calc R . . C41 C 0.1312(4) 0.5532(3) 0.05428(17) 0.0491(10) Uani 1 1 d . . . H41A H 0.2012 0.5775 0.0370 0.059 Uiso 1 1 calc R . . H41B H 0.0700 0.5835 0.0253 0.059 Uiso 1 1 calc R . . C42 C 0.1508(4) 0.4547(3) 0.06198(18) 0.0507(11) Uani 1 1 d . . . H42A H 0.0778 0.4324 0.0732 0.061 Uiso 1 1 calc R . . H42B H 0.1779 0.4468 0.0230 0.061 Uiso 1 1 calc R . . C43 C -0.0237(3) 0.5676(3) 0.12909(17) 0.0469(10) Uani 1 1 d . . . H43A H -0.0469 0.5210 0.1171 0.056 Uiso 1 1 calc R . . H43B H -0.0690 0.6237 0.1061 0.056 Uiso 1 1 calc R . . C44 C -0.0504(3) 0.5498(3) 0.19717(17) 0.0441(9) Uani 1 1 d . . . H44A H -0.0408 0.6008 0.2084 0.053 Uiso 1 1 calc R . . H44B H -0.1298 0.5395 0.2067 0.053 Uiso 1 1 calc R . . C45 C 0.1337(3) 0.6560(2) 0.11054(16) 0.0398(9) Uani 1 1 d . . . H45A H 0.0683 0.7031 0.0973 0.048 Uiso 1 1 calc R . . H45B H 0.1956 0.6695 0.0799 0.048 Uiso 1 1 calc R . . C46 C 0.1737(3) 0.6559(2) 0.17143(16) 0.0384(9) Uani 1 1 d . . . H46A H 0.2134 0.7065 0.1641 0.046 Uiso 1 1 calc R . . H46B H 0.1067 0.6626 0.1981 0.046 Uiso 1 1 calc R . . C47 C 0.3560(4) 0.4177(3) 0.08892(18) 0.0511(11) Uani 1 1 d . . . H47A H 0.3546 0.4795 0.0637 0.061 Uiso 1 1 calc R . . H47B H 0.3871 0.3810 0.0638 0.061 Uiso 1 1 calc R . . C48 C 0.4342(3) 0.3961(2) 0.14296(18) 0.0447(10) Uani 1 1 d . . . H48A H 0.4475 0.3323 0.1637 0.054 Uiso 1 1 calc R . . H48B H 0.5084 0.4147 0.1278 0.054 Uiso 1 1 calc R . . C49 C 0.2278(4) 0.3066(2) 0.12798(18) 0.0470(10) Uani 1 1 d . . . H49A H 0.3015 0.2715 0.1434 0.056 Uiso 1 1 calc R . . H49B H 0.2108 0.2927 0.0922 0.056 Uiso 1 1 calc R . . C50 C 0.1349(4) 0.2822(3) 0.17685(17) 0.0463(10) Uani 1 1 d . . . H50A H 0.0599 0.3153 0.1618 0.056 Uiso 1 1 calc R . . H50B H 0.1313 0.2191 0.1892 0.056 Uiso 1 1 calc R . . C51 C -0.1133(3) 0.3145(3) 0.40725(17) 0.0423(9) Uani 1 1 d . . . C52 C -0.0285(4) 0.3413(3) 0.44019(19) 0.0674(14) Uani 1 1 d . . . H52A H -0.0712 0.3788 0.4625 0.081 Uiso 1 1 calc R . . H52B H 0.0101 0.2881 0.4703 0.081 Uiso 1 1 calc R . . C53 C -0.1856(4) 0.3982(3) 0.3677(2) 0.0643(13) Uani 1 1 d . . . H53A H -0.2334 0.3820 0.3423 0.077 Uiso 1 1 calc R . . H53B H -0.2370 0.4241 0.3944 0.077 Uiso 1 1 calc R . . C54 C -0.0444(4) 0.2668(3) 0.3658(2) 0.0647(14) Uani 1 1 d . . . H54A H 0.0108 0.2185 0.3906 0.078 Uiso 1 1 calc R . . H54B H -0.0971 0.2406 0.3495 0.078 Uiso 1 1 calc R . . C55 C -0.1904(4) 0.2538(3) 0.45312(19) 0.0594(12) Uani 1 1 d . . . H55A H -0.2265 0.2823 0.4819 0.089 Uiso 1 1 calc R . . H55B H -0.1441 0.1984 0.4749 0.089 Uiso 1 1 calc R . . H55C H -0.2490 0.2428 0.4313 0.089 Uiso 1 1 calc R . . C56 C 0.5643(3) 0.6719(2) 0.09288(17) 0.0423(9) Uani 1 1 d . . . C57 C 0.4841(4) 0.6385(3) 0.05988(18) 0.0518(11) Uani 1 1 d . . . H57A H 0.4511 0.6877 0.0251 0.062 Uiso 1 1 calc R . . H57B H 0.5293 0.5940 0.0440 0.062 Uiso 1 1 calc R . . C58 C 0.6371(3) 0.5912(3) 0.1358(2) 0.0514(11) Uani 1 1 d . . . H58A H 0.6971 0.5671 0.1115 0.062 Uiso 1 1 calc R . . H58B H 0.6750 0.6100 0.1639 0.062 Uiso 1 1 calc R . . C59 C 0.4892(4) 0.7227(3) 0.13176(19) 0.0541(11) Uani 1 1 d . . . H59A H 0.5369 0.7560 0.1449 0.065 Uiso 1 1 calc R . . H59B H 0.4291 0.7650 0.1064 0.065 Uiso 1 1 calc R . . C60 C 0.6403(4) 0.7323(3) 0.04661(19) 0.0593(12) Uani 1 1 d . . . H60A H 0.6800 0.7019 0.0196 0.089 Uiso 1 1 calc R . . H60B H 0.6959 0.7470 0.0682 0.089 Uiso 1 1 calc R . . H60C H 0.5928 0.7858 0.0229 0.089 Uiso 1 1 calc R . . N9 N 0.6169(6) 0.5997(4) 0.4063(3) 0.120(2) Uani 1 1 d U . . C61 C 0.6372(5) 0.6114(3) 0.3556(3) 0.0757(15) Uani 1 1 d . . . C62 C 0.6601(5) 0.6225(3) 0.2921(2) 0.0774(15) Uani 1 1 d . . . H62A H 0.6832 0.6796 0.2716 0.116 Uiso 1 1 calc R . . H62B H 0.5914 0.6189 0.2738 0.116 Uiso 1 1 calc R . . H62C H 0.7210 0.5765 0.2879 0.116 Uiso 1 1 calc R . . N10 N -0.1775(6) 0.3889(4) 0.0943(3) 0.124(2) Uani 1 1 d U . . C63 C -0.1936(5) 0.3786(3) 0.1444(3) 0.0719(15) Uani 1 1 d . . . C64 C -0.2105(4) 0.3685(3) 0.2082(2) 0.0725(14) Uani 1 1 d . . . H64A H -0.2642 0.4181 0.2129 0.109 Uiso 1 1 calc R . . H64B H -0.1379 0.3661 0.2253 0.109 Uiso 1 1 calc R . . H64C H -0.2409 0.3144 0.2292 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0287(3) 0.0297(3) 0.0245(3) -0.0065(2) -0.0025(2) -0.0031(2) Mn2 0.0267(3) 0.0296(3) 0.0251(3) -0.0078(2) -0.0040(2) -0.0007(2) Mn3 0.0278(3) 0.0290(3) 0.0241(3) -0.0071(2) -0.0028(2) -0.0020(2) Mn4 0.0271(3) 0.0301(3) 0.0277(3) -0.0093(2) -0.0049(2) -0.0003(2) Mn5 0.0477(3) 0.0273(3) 0.0229(3) -0.0094(2) -0.0034(2) 0.0027(2) Mn6 0.0424(3) 0.0334(3) 0.0237(3) -0.0097(2) -0.0010(2) 0.0033(2) Mn7 0.0430(3) 0.0294(3) 0.0223(3) -0.0097(2) -0.0016(2) 0.0017(2) Mn8 0.0414(3) 0.0294(3) 0.0251(3) -0.0084(2) -0.0017(2) 0.0027(2) O1 0.0356(13) 0.0342(14) 0.0309(14) -0.0142(11) -0.0061(10) 0.0031(10) O2 0.0264(11) 0.0241(12) 0.0291(13) -0.0080(10) -0.0040(10) -0.0007(9) O3 0.0322(12) 0.0297(13) 0.0293(14) -0.0020(11) -0.0057(10) -0.0044(10) O4 0.0416(15) 0.0526(17) 0.0333(15) -0.0022(13) -0.0075(12) -0.0124(12) O5 0.0274(11) 0.0242(12) 0.0298(13) -0.0101(10) -0.0040(10) 0.0001(9) O6 0.0340(13) 0.0303(13) 0.0275(13) -0.0107(11) -0.0057(10) 0.0047(10) O7 0.0438(15) 0.0523(17) 0.0297(15) -0.0059(13) -0.0053(11) -0.0127(12) O8 0.0343(13) 0.0282(13) 0.0300(14) -0.0033(11) -0.0071(10) -0.0012(10) O9 0.0331(13) 0.0511(16) 0.0298(14) -0.0193(12) -0.0030(11) -0.0026(11) O10 0.0336(13) 0.0353(14) 0.0442(16) -0.0135(12) -0.0140(11) 0.0043(11) O11 0.0362(13) 0.0393(14) 0.0299(14) -0.0051(12) -0.0082(11) -0.0107(11) O12 0.0321(13) 0.0500(16) 0.0342(15) -0.0214(13) -0.0040(11) -0.0010(11) O13 0.0334(13) 0.0334(14) 0.0451(16) -0.0149(12) -0.0142(11) 0.0048(10) O14 0.0389(14) 0.0421(15) 0.0341(15) -0.0063(12) -0.0087(11) -0.0125(11) O15 0.0500(15) 0.0331(14) 0.0323(15) -0.0143(12) 0.0023(12) 0.0047(11) O16 0.0710(19) 0.0435(16) 0.0353(16) -0.0212(13) 0.0036(13) -0.0065(14) O17 0.0467(15) 0.0349(14) 0.0230(13) -0.0057(11) -0.0053(11) 0.0057(11) O18 0.0401(13) 0.0275(13) 0.0243(13) -0.0080(11) -0.0049(10) 0.0068(10) O19 0.0444(14) 0.0412(15) 0.0237(14) -0.0065(12) -0.0033(11) 0.0030(12) O20 0.0409(13) 0.0250(12) 0.0244(13) -0.0065(11) -0.0032(10) 0.0064(10) O21 0.0450(14) 0.0303(13) 0.0322(14) -0.0137(11) 0.0029(11) 0.0000(11) O22 0.0625(17) 0.0434(16) 0.0329(15) -0.0209(13) 0.0056(13) -0.0123(13) O23 0.0575(17) 0.0436(15) 0.0260(14) -0.0105(12) -0.0043(12) -0.0042(13) O24 0.0455(15) 0.0456(16) 0.0344(15) -0.0061(13) 0.0017(12) 0.0085(12) O25 0.0503(15) 0.0373(15) 0.0327(15) -0.0142(12) 0.0059(12) -0.0068(12) O26 0.0475(15) 0.0442(15) 0.0237(14) -0.0088(12) -0.0023(11) -0.0028(12) O27 0.0414(14) 0.0385(15) 0.0394(16) -0.0056(13) -0.0017(12) 0.0046(12) O28 0.0545(16) 0.0322(14) 0.0338(15) -0.0127(12) 0.0011(12) -0.0034(12) N1 0.0320(15) 0.0424(18) 0.0299(17) -0.0169(14) -0.0009(13) -0.0043(13) N2 0.0368(16) 0.0432(18) 0.0272(17) -0.0048(14) -0.0024(13) -0.0092(14) N3 0.0316(15) 0.0383(17) 0.0321(17) -0.0158(14) -0.0020(13) -0.0025(13) N4 0.0354(16) 0.0431(18) 0.0282(17) -0.0083(14) -0.0030(13) -0.0052(14) N5 0.072(2) 0.0320(17) 0.0258(17) -0.0115(14) -0.0034(16) -0.0014(16) N6 0.055(2) 0.0315(17) 0.0252(17) -0.0068(14) -0.0053(14) -0.0002(14) N7 0.0489(19) 0.0378(18) 0.0252(17) -0.0084(14) -0.0049(14) 0.0009(14) N8 0.058(2) 0.0348(18) 0.0277(17) -0.0126(15) 0.0005(15) -0.0071(15) C1 0.048(2) 0.054(3) 0.033(2) -0.019(2) -0.0009(17) -0.0107(19) C2 0.046(2) 0.061(3) 0.028(2) -0.015(2) 0.0069(17) -0.0137(19) C3 0.0302(19) 0.054(2) 0.047(2) -0.029(2) 0.0004(17) -0.0011(17) C4 0.0308(19) 0.042(2) 0.045(2) -0.0216(19) -0.0039(17) 0.0046(16) C5 0.0374(19) 0.034(2) 0.039(2) -0.0184(18) -0.0011(16) -0.0024(15) C6 0.0305(18) 0.0273(19) 0.039(2) -0.0108(17) -0.0011(15) -0.0016(14) C7 0.040(2) 0.055(3) 0.026(2) 0.0023(19) -0.0056(16) -0.0078(18) C8 0.038(2) 0.035(2) 0.042(2) 0.0008(18) -0.0038(17) -0.0010(16) C9 0.046(2) 0.050(2) 0.033(2) -0.0026(19) 0.0003(18) -0.0163(19) C10 0.043(2) 0.045(2) 0.042(2) -0.0087(19) 0.0034(18) -0.0150(18) C11 0.047(2) 0.053(2) 0.032(2) -0.0212(19) -0.0010(17) -0.0056(18) C12 0.042(2) 0.060(3) 0.025(2) -0.0155(19) 0.0016(16) -0.0054(19) C13 0.038(2) 0.032(2) 0.046(2) -0.0190(18) -0.0043(17) -0.0003(16) C14 0.0355(19) 0.0280(19) 0.041(2) -0.0097(17) -0.0024(16) -0.0025(15) C15 0.035(2) 0.048(2) 0.044(2) -0.026(2) -0.0042(17) 0.0037(17) C16 0.0324(19) 0.038(2) 0.043(2) -0.0193(18) -0.0040(16) 0.0045(16) C17 0.051(2) 0.042(2) 0.029(2) -0.0018(18) 0.0020(17) -0.0127(18) C18 0.040(2) 0.052(2) 0.038(2) -0.010(2) 0.0016(17) -0.0162(18) C19 0.041(2) 0.054(3) 0.027(2) -0.0033(19) -0.0094(16) -0.0064(18) C20 0.039(2) 0.037(2) 0.041(2) -0.0002(19) -0.0074(17) 0.0025(17) C21 0.0325(18) 0.041(2) 0.032(2) -0.0111(17) -0.0098(15) -0.0035(16) C22 0.043(2) 0.051(2) 0.030(2) -0.0150(19) -0.0037(17) -0.0056(18) C23 0.0326(19) 0.049(2) 0.046(2) -0.019(2) -0.0133(17) 0.0057(17) C24 0.038(2) 0.047(2) 0.036(2) -0.0120(19) -0.0019(17) -0.0152(17) C25 0.045(2) 0.065(3) 0.059(3) -0.025(2) -0.019(2) -0.008(2) C26 0.0296(18) 0.045(2) 0.038(2) -0.0183(19) -0.0092(16) -0.0012(16) C27 0.047(2) 0.045(2) 0.033(2) -0.0139(19) -0.0088(17) -0.0040(18) C28 0.035(2) 0.053(3) 0.056(3) -0.025(2) -0.0164(18) 0.0067(18) C29 0.045(2) 0.047(2) 0.042(2) -0.016(2) -0.0030(18) -0.0150(18) C30 0.045(2) 0.067(3) 0.060(3) -0.027(2) -0.018(2) -0.008(2) C31 0.091(3) 0.042(2) 0.030(2) -0.015(2) -0.012(2) -0.003(2) C32 0.083(3) 0.045(2) 0.023(2) -0.0100(19) -0.008(2) -0.002(2) C33 0.083(3) 0.045(2) 0.034(2) -0.022(2) 0.009(2) -0.003(2) C34 0.059(3) 0.040(2) 0.051(3) -0.025(2) 0.008(2) 0.0068(19) C35 0.093(3) 0.037(2) 0.036(2) -0.020(2) -0.004(2) -0.001(2) C36 0.083(3) 0.041(2) 0.037(2) -0.016(2) -0.003(2) -0.011(2) C37 0.055(2) 0.040(2) 0.034(2) -0.0034(19) -0.0151(18) -0.0007(18) C38 0.044(2) 0.040(2) 0.034(2) -0.0072(18) -0.0071(17) 0.0029(17) C39 0.051(2) 0.029(2) 0.030(2) -0.0071(17) -0.0083(17) 0.0050(16) C40 0.050(2) 0.0261(19) 0.035(2) -0.0097(17) -0.0070(17) 0.0052(16) C41 0.072(3) 0.049(3) 0.023(2) -0.0125(19) -0.0056(19) 0.002(2) C42 0.079(3) 0.046(2) 0.029(2) -0.015(2) -0.004(2) -0.008(2) C43 0.052(2) 0.048(2) 0.031(2) -0.0023(19) -0.0126(18) 0.0018(19) C44 0.042(2) 0.048(2) 0.035(2) -0.0068(19) -0.0070(17) 0.0040(18) C45 0.051(2) 0.029(2) 0.029(2) -0.0030(17) -0.0065(17) 0.0079(17) C46 0.048(2) 0.031(2) 0.031(2) -0.0082(17) -0.0080(17) 0.0068(16) C47 0.072(3) 0.046(2) 0.040(3) -0.024(2) 0.017(2) -0.011(2) C48 0.049(2) 0.036(2) 0.051(3) -0.023(2) 0.005(2) 0.0016(18) C49 0.069(3) 0.041(2) 0.038(2) -0.0217(19) 0.002(2) -0.009(2) C50 0.063(3) 0.042(2) 0.036(2) -0.0159(19) -0.0024(19) -0.0073(19) C51 0.050(2) 0.048(2) 0.026(2) -0.0115(18) 0.0036(17) -0.0044(18) C52 0.075(3) 0.096(4) 0.028(2) -0.010(2) 0.001(2) -0.024(3) C53 0.049(3) 0.056(3) 0.069(3) -0.003(3) 0.007(2) 0.003(2) C54 0.089(3) 0.052(3) 0.058(3) -0.026(2) 0.033(3) -0.025(3) C55 0.071(3) 0.060(3) 0.042(3) -0.011(2) 0.011(2) -0.013(2) C56 0.053(2) 0.039(2) 0.032(2) -0.0095(18) 0.0016(18) -0.0054(18) C57 0.062(3) 0.053(3) 0.031(2) -0.005(2) 0.002(2) -0.004(2) C58 0.044(2) 0.049(3) 0.056(3) -0.013(2) 0.004(2) -0.0048(19) C59 0.073(3) 0.037(2) 0.049(3) -0.014(2) 0.015(2) -0.008(2) C60 0.069(3) 0.054(3) 0.048(3) -0.008(2) 0.011(2) -0.015(2) N9 0.172(5) 0.115(4) 0.083(4) -0.048(4) -0.028(4) -0.003(4) C61 0.104(4) 0.052(3) 0.072(4) -0.023(3) -0.023(3) 0.003(3) C62 0.101(4) 0.058(3) 0.064(4) -0.009(3) -0.007(3) -0.008(3) N10 0.181(5) 0.114(4) 0.077(4) -0.045(3) 0.017(4) -0.009(4) C63 0.099(4) 0.051(3) 0.059(3) -0.017(3) 0.005(3) 0.000(3) C64 0.094(4) 0.049(3) 0.060(3) -0.007(3) -0.003(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.127(2) . ? Mn1 O3 2.153(2) . ? Mn1 O2 2.220(2) . ? Mn1 O5 2.245(2) . ? Mn1 O4 2.355(2) . ? Mn1 N2 2.373(3) . ? Mn1 N1 2.411(3) . ? Mn1 Mn2 3.2305(7) . ? Mn1 Mn4 3.2599(7) . ? Mn1 Mn3 3.3624(7) . ? Mn2 O10 1.828(2) . ? Mn2 O9 1.852(2) . ? Mn2 O11 1.871(2) . ? Mn2 O6 1.943(2) . ? Mn2 O3 1.943(2) . ? Mn2 O2 2.003(2) . ? Mn2 Mn3 3.2606(7) . ? Mn2 Mn4 5.5552(8) . ? Mn3 O6 2.136(2) . ? Mn3 O8 2.162(2) . ? Mn3 O5 2.221(2) . ? Mn3 O2 2.234(2) . ? Mn3 N4 2.358(3) . ? Mn3 O7 2.360(2) . ? Mn3 N3 2.416(3) . ? Mn3 Mn4 3.2359(7) . ? Mn4 O13 1.827(2) . ? Mn4 O12 1.849(2) . ? Mn4 O14 1.876(2) . ? Mn4 O1 1.937(2) . ? Mn4 O8 1.941(2) . ? Mn4 O5 2.003(2) . ? Mn5 O17 2.135(2) . ? Mn5 O15 2.159(2) . ? Mn5 O18 2.247(2) . ? Mn5 O20 2.262(2) . ? Mn5 O16 2.341(2) . ? Mn5 N5 2.358(3) . ? Mn5 N6 2.397(3) . ? Mn5 Mn6 3.2400(8) . ? Mn5 Mn8 3.2786(7) . ? Mn5 Mn7 3.3871(7) . ? Mn6 O24 1.834(2) . ? Mn6 O23 1.848(2) . ? Mn6 O25 1.883(2) . ? Mn6 O15 1.931(2) . ? Mn6 O19 1.940(2) . ? Mn6 O18 1.992(2) . ? Mn6 Mn7 3.2791(7) . ? Mn6 Mn8 5.5677(8) . ? Mn7 O19 2.141(2) . ? Mn7 O21 2.156(2) . ? Mn7 O20 2.238(2) . ? Mn7 O18 2.260(2) . ? Mn7 O22 2.335(2) . ? Mn7 N8 2.354(3) . ? Mn7 N7 2.411(3) . ? Mn7 Mn8 3.2360(8) . ? Mn8 O27 1.835(2) . ? Mn8 O26 1.845(2) . ? Mn8 O28 1.883(2) . ? Mn8 O21 1.939(2) . ? Mn8 O17 1.941(2) . ? Mn8 O20 1.996(2) . ? O1 C4 1.411(4) . ? O2 C6 1.421(4) . ? O3 C8 1.408(4) . ? O4 C10 1.411(4) . ? O4 H4O 0.8501 . ? O5 C14 1.423(4) . ? O6 C16 1.406(4) . ? O7 C18 1.412(4) . ? O7 H7O 0.8500 . ? O8 C20 1.409(4) . ? O9 C22 1.389(4) . ? O10 C23 1.404(4) . ? O11 C24 1.404(4) . ? O12 C27 1.387(4) . ? O13 C28 1.401(4) . ? O14 C29 1.398(4) . ? O15 C34 1.421(4) . ? O16 C36 1.421(4) . ? O16 H16O 0.8502 . ? O17 C38 1.398(4) . ? O18 C40 1.424(4) . ? O19 C44 1.400(4) . ? O20 C46 1.423(4) . ? O21 C48 1.419(4) . ? O22 C50 1.420(4) . ? O22 H22O 0.8501 . ? O23 C52 1.376(5) . ? O24 C53 1.380(5) . ? O25 C54 1.377(4) . ? O26 C57 1.396(4) . ? O27 C58 1.407(4) . ? O28 C59 1.401(4) . ? N1 C5 1.469(4) . ? N1 C3 1.473(4) . ? N1 C1 1.480(4) . ? N2 C9 1.466(4) . ? N2 C2 1.469(4) . ? N2 C7 1.482(4) . ? N3 C11 1.474(4) . ? N3 C15 1.475(4) . ? N3 C13 1.476(4) . ? N4 C17 1.468(4) . ? N4 C12 1.474(4) . ? N4 C19 1.490(4) . ? N5 C31 1.471(5) . ? N5 C35 1.482(4) . ? N5 C33 1.487(5) . ? N6 C39 1.470(4) . ? N6 C37 1.479(5) . ? N6 C32 1.487(4) . ? N7 C43 1.473(5) . ? N7 C41 1.475(4) . ? N7 C45 1.475(4) . ? N8 C49 1.477(4) . ? N8 C47 1.481(5) . ? N8 C42 1.485(5) . ? C1 C2 1.513(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.520(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.523(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.517(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.513(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.512(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.524(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.517(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.503(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.521(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.523(5) . ? C21 C24 1.526(5) . ? C21 C23 1.526(5) . ? C21 C25 1.530(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C29 1.514(5) . ? C26 C28 1.521(5) . ? C26 C30 1.525(5) . ? C26 C27 1.526(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.517(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.510(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.492(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.516(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.519(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.517(5) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.514(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.519(5) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.520(5) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.504(5) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.504(6) . ? C51 C53 1.509(6) . ? C51 C54 1.519(5) . ? C51 C55 1.534(5) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 C58 1.515(5) . ? C56 C60 1.526(5) . ? C56 C57 1.529(5) . ? C56 C59 1.535(5) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? N9 C61 1.133(7) . ? C61 C62 1.423(7) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? N10 C63 1.115(6) . ? C63 C64 1.424(6) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O3 161.85(9) . . ? O1 Mn1 O2 95.05(8) . . ? O3 Mn1 O2 72.93(8) . . ? O1 Mn1 O5 71.85(8) . . ? O3 Mn1 O5 92.66(8) . . ? O2 Mn1 O5 82.04(8) . . ? O1 Mn1 O4 83.05(9) . . ? O3 Mn1 O4 103.24(9) . . ? O2 Mn1 O4 159.09(8) . . ? O5 Mn1 O4 77.57(8) . . ? O1 Mn1 N2 120.63(9) . . ? O3 Mn1 N2 77.49(9) . . ? O2 Mn1 N2 125.10(9) . . ? O5 Mn1 N2 144.93(9) . . ? O4 Mn1 N2 72.28(9) . . ? O1 Mn1 N1 74.90(9) . . ? O3 Mn1 N1 113.58(9) . . ? O2 Mn1 N1 75.09(8) . . ? O5 Mn1 N1 137.40(9) . . ? O4 Mn1 N1 123.84(9) . . ? N2 Mn1 N1 76.04(10) . . ? O1 Mn1 Mn2 132.40(7) . . ? O3 Mn1 Mn2 35.71(6) . . ? O2 Mn1 Mn2 37.67(5) . . ? O5 Mn1 Mn2 91.21(5) . . ? O4 Mn1 Mn2 137.55(7) . . ? N2 Mn1 Mn2 98.98(7) . . ? N1 Mn1 Mn2 91.98(7) . . ? O1 Mn1 Mn4 34.71(6) . . ? O3 Mn1 Mn4 129.60(6) . . ? O2 Mn1 Mn4 90.34(6) . . ? O5 Mn1 Mn4 37.23(5) . . ? O4 Mn1 Mn4 76.21(6) . . ? N2 Mn1 Mn4 142.79(7) . . ? N1 Mn1 Mn4 106.82(7) . . ? Mn2 Mn1 Mn4 117.718(19) . . ? O1 Mn1 Mn3 81.65(6) . . ? O3 Mn1 Mn3 80.39(6) . . ? O2 Mn1 Mn3 41.15(6) . . ? O5 Mn1 Mn3 40.90(5) . . ? O4 Mn1 Mn3 118.31(6) . . ? N2 Mn1 Mn3 157.30(7) . . ? N1 Mn1 Mn3 108.73(7) . . ? Mn2 Mn1 Mn3 59.242(15) . . ? Mn4 Mn1 Mn3 58.478(15) . . ? O10 Mn2 O9 93.01(11) . . ? O10 Mn2 O11 92.52(11) . . ? O9 Mn2 O11 91.62(11) . . ? O10 Mn2 O6 95.13(10) . . ? O9 Mn2 O6 171.83(10) . . ? O11 Mn2 O6 87.33(10) . . ? O10 Mn2 O3 93.05(10) . . ? O9 Mn2 O3 91.83(10) . . ? O11 Mn2 O3 173.28(10) . . ? O6 Mn2 O3 88.44(10) . . ? O10 Mn2 O2 174.25(10) . . ? O9 Mn2 O2 90.65(10) . . ? O11 Mn2 O2 91.80(9) . . ? O6 Mn2 O2 81.29(9) . . ? O3 Mn2 O2 82.40(9) . . ? O10 Mn2 Mn1 133.18(8) . . ? O9 Mn2 Mn1 86.46(7) . . ? O11 Mn2 Mn1 134.29(7) . . ? O6 Mn2 Mn1 88.48(7) . . ? O3 Mn2 Mn1 40.29(7) . . ? O2 Mn2 Mn1 42.65(6) . . ? O10 Mn2 Mn3 134.12(8) . . ? O9 Mn2 Mn3 132.87(8) . . ? O11 Mn2 Mn3 87.42(7) . . ? O6 Mn2 Mn3 39.01(6) . . ? O3 Mn2 Mn3 86.01(7) . . ? O2 Mn2 Mn3 42.36(6) . . ? Mn1 Mn2 Mn3 62.394(15) . . ? O10 Mn2 Mn4 144.06(7) . . ? O9 Mn2 Mn4 111.11(7) . . ? O11 Mn2 Mn4 112.21(7) . . ? O6 Mn2 Mn4 62.05(6) . . ? O3 Mn2 Mn4 61.13(7) . . ? O2 Mn2 Mn4 30.21(6) . . ? Mn1 Mn2 Mn4 31.298(12) . . ? Mn3 Mn2 Mn4 31.098(11) . . ? O6 Mn3 O8 162.77(9) . . ? O6 Mn3 O5 96.19(8) . . ? O8 Mn3 O5 72.88(8) . . ? O6 Mn3 O2 72.02(8) . . ? O8 Mn3 O2 92.96(8) . . ? O5 Mn3 O2 82.25(8) . . ? O6 Mn3 N4 119.89(9) . . ? O8 Mn3 N4 77.25(9) . . ? O5 Mn3 N4 124.95(9) . . ? O2 Mn3 N4 144.85(9) . . ? O6 Mn3 O7 82.51(9) . . ? O8 Mn3 O7 102.82(9) . . ? O5 Mn3 O7 158.92(8) . . ? O2 Mn3 O7 77.32(8) . . ? N4 Mn3 O7 72.29(9) . . ? O6 Mn3 N3 75.24(9) . . ? O8 Mn3 N3 113.32(9) . . ? O5 Mn3 N3 75.08(8) . . ? O2 Mn3 N3 137.51(9) . . ? N4 Mn3 N3 75.97(10) . . ? O7 Mn3 N3 124.25(9) . . ? O6 Mn3 Mn4 133.33(6) . . ? O8 Mn3 Mn4 35.59(6) . . ? O5 Mn3 Mn4 37.58(6) . . ? O2 Mn3 Mn4 90.71(5) . . ? N4 Mn3 Mn4 99.36(7) . . ? O7 Mn3 Mn4 136.72(7) . . ? N3 Mn3 Mn4 92.51(7) . . ? O6 Mn3 Mn2 34.93(6) . . ? O8 Mn3 Mn2 129.88(6) . . ? O5 Mn3 Mn2 90.85(6) . . ? O2 Mn3 Mn2 37.16(5) . . ? N4 Mn3 Mn2 142.48(7) . . ? O7 Mn3 Mn2 75.99(6) . . ? N3 Mn3 Mn2 107.12(7) . . ? Mn4 Mn3 Mn2 117.539(19) . . ? O6 Mn3 Mn1 82.03(6) . . ? O8 Mn3 Mn1 81.02(6) . . ? O5 Mn3 Mn1 41.42(6) . . ? O2 Mn3 Mn1 40.83(5) . . ? N4 Mn3 Mn1 157.70(7) . . ? O7 Mn3 Mn1 118.00(6) . . ? N3 Mn3 Mn1 108.68(7) . . ? Mn4 Mn3 Mn1 59.178(15) . . ? Mn2 Mn3 Mn1 58.364(15) . . ? O13 Mn4 O12 92.61(11) . . ? O13 Mn4 O14 92.71(11) . . ? O12 Mn4 O14 91.51(11) . . ? O13 Mn4 O1 95.02(10) . . ? O12 Mn4 O1 172.28(10) . . ? O14 Mn4 O1 87.02(10) . . ? O13 Mn4 O8 93.18(10) . . ? O12 Mn4 O8 91.71(10) . . ? O14 Mn4 O8 173.15(10) . . ? O1 Mn4 O8 88.98(10) . . ? O13 Mn4 O5 174.41(9) . . ? O12 Mn4 O5 91.18(10) . . ? O14 Mn4 O5 91.29(10) . . ? O1 Mn4 O5 81.28(9) . . ? O8 Mn4 O5 82.60(9) . . ? O13 Mn4 Mn3 133.52(8) . . ? O12 Mn4 Mn3 87.70(7) . . ? O14 Mn4 Mn3 133.77(8) . . ? O1 Mn4 Mn3 87.86(7) . . ? O8 Mn4 Mn3 40.40(7) . . ? O5 Mn4 Mn3 42.55(6) . . ? O13 Mn4 Mn1 133.73(8) . . ? O12 Mn4 Mn1 133.65(8) . . ? O14 Mn4 Mn1 86.51(7) . . ? O1 Mn4 Mn1 38.71(7) . . ? O8 Mn4 Mn1 86.89(7) . . ? O5 Mn4 Mn1 42.68(6) . . ? Mn3 Mn4 Mn1 62.345(15) . . ? O13 Mn4 Mn2 143.49(7) . . ? O12 Mn4 Mn2 112.64(7) . . ? O14 Mn4 Mn2 111.65(7) . . ? O1 Mn4 Mn2 61.15(7) . . ? O8 Mn4 Mn2 61.52(7) . . ? O5 Mn4 Mn2 30.93(6) . . ? Mn3 Mn4 Mn2 31.363(12) . . ? Mn1 Mn4 Mn2 30.984(11) . . ? O17 Mn5 O15 161.47(9) . . ? O17 Mn5 O18 95.37(9) . . ? O15 Mn5 O18 72.19(8) . . ? O17 Mn5 O20 71.19(8) . . ? O15 Mn5 O20 93.12(9) . . ? O18 Mn5 O20 82.33(8) . . ? O17 Mn5 O16 82.86(9) . . ? O15 Mn5 O16 103.58(9) . . ? O18 Mn5 O16 158.48(9) . . ? O20 Mn5 O16 76.79(8) . . ? O17 Mn5 N5 120.66(11) . . ? O15 Mn5 N5 77.85(10) . . ? O18 Mn5 N5 125.31(10) . . ? O20 Mn5 N5 144.63(9) . . ? O16 Mn5 N5 72.42(10) . . ? O17 Mn5 N6 75.30(10) . . ? O15 Mn5 N6 113.16(10) . . ? O18 Mn5 N6 75.19(9) . . ? O20 Mn5 N6 137.30(9) . . ? O16 Mn5 N6 124.41(10) . . ? N5 Mn5 N6 76.22(10) . . ? O17 Mn5 Mn6 132.29(7) . . ? O15 Mn5 Mn6 35.22(6) . . ? O18 Mn5 Mn6 37.33(6) . . ? O20 Mn5 Mn6 91.23(6) . . ? O16 Mn5 Mn6 137.14(7) . . ? N5 Mn5 Mn6 99.55(8) . . ? N6 Mn5 Mn6 92.20(8) . . ? O17 Mn5 Mn8 34.50(6) . . ? O15 Mn5 Mn8 129.53(7) . . ? O18 Mn5 Mn8 90.49(6) . . ? O20 Mn5 Mn8 36.76(6) . . ? O16 Mn5 Mn8 75.87(6) . . ? N5 Mn5 Mn8 142.54(8) . . ? N6 Mn5 Mn8 106.97(7) . . ? Mn6 Mn5 Mn8 117.32(2) . . ? O17 Mn5 Mn7 81.18(7) . . ? O15 Mn5 Mn7 80.45(6) . . ? O18 Mn5 Mn7 41.42(6) . . ? O20 Mn5 Mn7 40.91(6) . . ? O16 Mn5 Mn7 117.52(6) . . ? N5 Mn5 Mn7 157.84(9) . . ? N6 Mn5 Mn7 108.77(7) . . ? Mn6 Mn5 Mn7 59.264(16) . . ? Mn8 Mn5 Mn7 58.058(16) . . ? O24 Mn6 O23 92.41(11) . . ? O24 Mn6 O25 91.61(11) . . ? O23 Mn6 O25 90.86(11) . . ? O24 Mn6 O15 93.82(11) . . ? O23 Mn6 O15 92.20(11) . . ? O25 Mn6 O15 173.65(10) . . ? O24 Mn6 O19 93.40(11) . . ? O23 Mn6 O19 174.06(11) . . ? O25 Mn6 O19 87.72(10) . . ? O15 Mn6 O19 88.67(10) . . ? O24 Mn6 O18 173.70(11) . . ? O23 Mn6 O18 93.06(10) . . ? O25 Mn6 O18 91.45(10) . . ? O15 Mn6 O18 82.84(10) . . ? O19 Mn6 O18 81.22(10) . . ? O24 Mn6 Mn5 133.92(9) . . ? O23 Mn6 Mn5 88.75(8) . . ? O25 Mn6 Mn5 134.45(8) . . ? O15 Mn6 Mn5 40.13(7) . . ? O19 Mn6 Mn5 88.13(7) . . ? O18 Mn6 Mn5 43.15(6) . . ? O24 Mn6 Mn7 132.07(8) . . ? O23 Mn6 Mn7 135.51(8) . . ? O25 Mn6 Mn7 87.43(7) . . ? O15 Mn6 Mn7 86.48(7) . . ? O19 Mn6 Mn7 38.67(7) . . ? O18 Mn6 Mn7 42.62(6) . . ? Mn5 Mn6 Mn7 62.603(16) . . ? O24 Mn6 Mn8 143.03(8) . . ? O23 Mn6 Mn8 113.99(8) . . ? O25 Mn6 Mn8 112.30(7) . . ? O15 Mn6 Mn8 61.35(7) . . ? O19 Mn6 Mn8 61.44(7) . . ? O18 Mn6 Mn8 30.86(6) . . ? Mn5 Mn6 Mn8 31.546(12) . . ? Mn7 Mn6 Mn8 31.057(12) . . ? O19 Mn7 O21 161.70(9) . . ? O19 Mn7 O20 95.59(9) . . ? O21 Mn7 O20 72.60(8) . . ? O19 Mn7 O18 71.07(9) . . ? O21 Mn7 O18 93.14(9) . . ? O20 Mn7 O18 82.58(8) . . ? O19 Mn7 O22 82.74(9) . . ? O21 Mn7 O22 103.04(9) . . ? O20 Mn7 O22 158.52(9) . . ? O18 Mn7 O22 76.61(8) . . ? O19 Mn7 N8 120.27(10) . . ? O21 Mn7 N8 77.96(10) . . ? O20 Mn7 N8 125.25(9) . . ? O18 Mn7 N8 144.74(9) . . ? O22 Mn7 N8 72.47(9) . . ? O19 Mn7 N7 75.27(10) . . ? O21 Mn7 N7 113.65(10) . . ? O20 Mn7 N7 75.25(9) . . ? O18 Mn7 N7 137.29(9) . . ? O22 Mn7 N7 124.34(10) . . ? N8 Mn7 N7 75.95(10) . . ? O19 Mn7 Mn8 132.60(7) . . ? O21 Mn7 Mn8 35.50(6) . . ? O20 Mn7 Mn8 37.46(6) . . ? O18 Mn7 Mn8 91.35(6) . . ? O22 Mn7 Mn8 136.88(7) . . ? N8 Mn7 Mn8 99.70(8) . . ? N7 Mn7 Mn8 92.53(8) . . ? O19 Mn7 Mn6 34.48(6) . . ? O21 Mn7 Mn6 129.49(7) . . ? O20 Mn7 Mn6 90.67(6) . . ? O18 Mn7 Mn6 36.65(6) . . ? O22 Mn7 Mn6 75.80(6) . . ? N8 Mn7 Mn6 142.31(8) . . ? N7 Mn7 Mn6 106.93(7) . . ? Mn8 Mn7 Mn6 117.42(2) . . ? O19 Mn7 Mn5 81.25(7) . . ? O21 Mn7 Mn5 80.70(6) . . ? O20 Mn7 Mn5 41.45(6) . . ? O18 Mn7 Mn5 41.13(6) . . ? O22 Mn7 Mn5 117.55(6) . . ? N8 Mn7 Mn5 158.12(8) . . ? N7 Mn7 Mn5 108.76(7) . . ? Mn8 Mn7 Mn5 59.291(16) . . ? Mn6 Mn7 Mn5 58.134(16) . . ? O27 Mn8 O26 92.70(11) . . ? O27 Mn8 O28 91.88(11) . . ? O26 Mn8 O28 90.75(11) . . ? O27 Mn8 O21 93.17(10) . . ? O26 Mn8 O21 92.39(11) . . ? O28 Mn8 O21 173.92(10) . . ? O27 Mn8 O17 94.03(11) . . ? O26 Mn8 O17 173.10(10) . . ? O28 Mn8 O17 87.54(10) . . ? O21 Mn8 O17 88.73(10) . . ? O27 Mn8 O20 173.75(10) . . ? O26 Mn8 O20 92.22(10) . . ? O28 Mn8 O20 91.89(10) . . ? O21 Mn8 O20 82.78(9) . . ? O17 Mn8 O20 81.16(10) . . ? O27 Mn8 Mn7 133.34(8) . . ? O26 Mn8 Mn7 88.42(8) . . ? O28 Mn8 Mn7 134.77(8) . . ? O21 Mn8 Mn7 40.21(7) . . ? O17 Mn8 Mn7 88.05(7) . . ? O20 Mn8 Mn7 43.00(6) . . ? O27 Mn8 Mn5 132.55(8) . . ? O26 Mn8 Mn5 134.74(8) . . ? O28 Mn8 Mn5 87.47(7) . . ? O21 Mn8 Mn5 86.62(7) . . ? O17 Mn8 Mn5 38.53(7) . . ? O20 Mn8 Mn5 42.72(7) . . ? Mn7 Mn8 Mn5 62.651(16) . . ? O27 Mn8 Mn6 142.79(8) . . ? O26 Mn8 Mn6 113.53(8) . . ? O28 Mn8 Mn6 112.64(7) . . ? O21 Mn8 Mn6 61.30(7) . . ? O17 Mn8 Mn6 61.24(7) . . ? O20 Mn8 Mn6 31.00(6) . . ? Mn7 Mn8 Mn6 31.518(12) . . ? Mn5 Mn8 Mn6 31.132(12) . . ? C4 O1 Mn4 123.9(2) . . ? C4 O1 Mn1 120.6(2) . . ? Mn4 O1 Mn1 106.58(10) . . ? C6 O2 Mn2 123.89(19) . . ? C6 O2 Mn1 114.76(17) . . ? Mn2 O2 Mn1 99.68(9) . . ? C6 O2 Mn3 115.80(19) . . ? Mn2 O2 Mn3 100.48(9) . . ? Mn1 O2 Mn3 98.02(8) . . ? C8 O3 Mn2 122.7(2) . . ? C8 O3 Mn1 114.76(19) . . ? Mn2 O3 Mn1 104.00(10) . . ? C10 O4 Mn1 110.7(2) . . ? C10 O4 H4O 110.1 . . ? Mn1 O4 H4O 100.3 . . ? C14 O5 Mn4 123.86(19) . . ? C14 O5 Mn3 115.10(18) . . ? Mn4 O5 Mn3 99.86(9) . . ? C14 O5 Mn1 115.91(19) . . ? Mn4 O5 Mn1 100.10(9) . . ? Mn3 O5 Mn1 97.69(8) . . ? C16 O6 Mn2 123.2(2) . . ? C16 O6 Mn3 119.70(19) . . ? Mn2 O6 Mn3 106.07(9) . . ? C18 O7 Mn3 111.1(2) . . ? C18 O7 H7O 111.6 . . ? Mn3 O7 H7O 102.8 . . ? C20 O8 Mn4 122.7(2) . . ? C20 O8 Mn3 115.0(2) . . ? Mn4 O8 Mn3 104.00(10) . . ? C22 O9 Mn2 118.2(2) . . ? C23 O10 Mn2 117.5(2) . . ? C24 O11 Mn2 117.7(2) . . ? C27 O12 Mn4 118.7(2) . . ? C28 O13 Mn4 117.5(2) . . ? C29 O14 Mn4 118.0(2) . . ? C34 O15 Mn6 122.6(2) . . ? C34 O15 Mn5 114.4(2) . . ? Mn6 O15 Mn5 104.65(10) . . ? C36 O16 Mn5 110.8(2) . . ? C36 O16 H16O 113.5 . . ? Mn5 O16 H16O 106.1 . . ? C38 O17 Mn8 123.5(2) . . ? C38 O17 Mn5 119.5(2) . . ? Mn8 O17 Mn5 106.98(11) . . ? C40 O18 Mn6 124.1(2) . . ? C40 O18 Mn5 114.3(2) . . ? Mn6 O18 Mn5 99.52(9) . . ? C40 O18 Mn7 116.33(18) . . ? Mn6 O18 Mn7 100.73(9) . . ? Mn5 O18 Mn7 97.46(9) . . ? C44 O19 Mn6 123.3(2) . . ? C44 O19 Mn7 119.1(2) . . ? Mn6 O19 Mn7 106.85(11) . . ? C46 O20 Mn8 124.0(2) . . ? C46 O20 Mn7 114.5(2) . . ? Mn8 O20 Mn7 99.54(9) . . ? C46 O20 Mn5 116.29(18) . . ? Mn8 O20 Mn5 100.52(10) . . ? Mn7 O20 Mn5 97.64(9) . . ? C48 O21 Mn8 122.3(2) . . ? C48 O21 Mn7 114.4(2) . . ? Mn8 O21 Mn7 104.29(10) . . ? C50 O22 Mn7 111.2(2) . . ? C50 O22 H22O 114.7 . . ? Mn7 O22 H22O 102.9 . . ? C52 O23 Mn6 118.4(2) . . ? C53 O24 Mn6 118.7(2) . . ? C54 O25 Mn6 117.8(2) . . ? C57 O26 Mn8 117.9(2) . . ? C58 O27 Mn8 117.4(2) . . ? C59 O28 Mn8 117.2(2) . . ? C5 N1 C3 112.5(3) . . ? C5 N1 C1 110.9(3) . . ? C3 N1 C1 111.6(3) . . ? C5 N1 Mn1 109.35(19) . . ? C3 N1 Mn1 103.95(19) . . ? C1 N1 Mn1 108.3(2) . . ? C9 N2 C2 110.8(3) . . ? C9 N2 C7 111.1(3) . . ? C2 N2 C7 111.8(3) . . ? C9 N2 Mn1 110.3(2) . . ? C2 N2 Mn1 108.2(2) . . ? C7 N2 Mn1 104.4(2) . . ? C11 N3 C15 111.4(3) . . ? C11 N3 C13 110.9(3) . . ? C15 N3 C13 112.6(3) . . ? C11 N3 Mn3 108.6(2) . . ? C15 N3 Mn3 104.05(19) . . ? C13 N3 Mn3 109.01(19) . . ? C17 N4 C12 110.5(3) . . ? C17 N4 C19 111.2(3) . . ? C12 N4 C19 111.4(3) . . ? C17 N4 Mn3 110.8(2) . . ? C12 N4 Mn3 108.0(2) . . ? C19 N4 Mn3 104.8(2) . . ? C31 N5 C35 110.3(3) . . ? C31 N5 C33 112.0(3) . . ? C35 N5 C33 110.9(3) . . ? C31 N5 Mn5 108.3(2) . . ? C35 N5 Mn5 110.6(2) . . ? C33 N5 Mn5 104.6(2) . . ? C39 N6 C37 112.7(3) . . ? C39 N6 C32 110.9(3) . . ? C37 N6 C32 110.5(3) . . ? C39 N6 Mn5 109.2(2) . . ? C37 N6 Mn5 104.2(2) . . ? C32 N6 Mn5 109.2(2) . . ? C43 N7 C41 111.3(3) . . ? C43 N7 C45 112.7(3) . . ? C41 N7 C45 111.0(3) . . ? C43 N7 Mn7 103.9(2) . . ? C41 N7 Mn7 108.9(2) . . ? C45 N7 Mn7 108.7(2) . . ? C49 N8 C47 110.8(3) . . ? C49 N8 C42 109.9(3) . . ? C47 N8 C42 112.0(3) . . ? C49 N8 Mn7 110.4(2) . . ? C47 N8 Mn7 104.8(2) . . ? C42 N8 Mn7 108.7(2) . . ? N1 C1 C2 112.9(3) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N2 C2 C1 113.3(3) . . ? N2 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? N2 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? N1 C3 C4 112.7(3) . . ? N1 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N1 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? O1 C4 C3 107.6(3) . . ? O1 C4 H4A 110.2 . . ? C3 C4 H4A 110.2 . . ? O1 C4 H4B 110.2 . . ? C3 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? N1 C5 C6 113.9(3) . . ? N1 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N1 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? O2 C6 C5 112.5(3) . . ? O2 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? O2 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N2 C7 C8 111.6(3) . . ? N2 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N2 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? O3 C8 C7 111.5(3) . . ? O3 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? O3 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N2 C9 C10 111.8(3) . . ? N2 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N2 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? O4 C10 C9 106.0(3) . . ? O4 C10 H10A 110.5 . . ? C9 C10 H10A 110.5 . . ? O4 C10 H10B 110.5 . . ? C9 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? N3 C11 C12 112.7(3) . . ? N3 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? N3 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N4 C12 C11 113.3(3) . . ? N4 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? N4 C12 H12B 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? N3 C13 C14 113.7(3) . . ? N3 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? N3 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? O5 C14 C13 112.1(3) . . ? O5 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? O5 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? N3 C15 C16 113.3(3) . . ? N3 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? N3 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? O6 C16 C15 108.3(3) . . ? O6 C16 H16A 110.0 . . ? C15 C16 H16A 110.0 . . ? O6 C16 H16B 110.0 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? N4 C17 C18 111.9(3) . . ? N4 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? N4 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? O7 C18 C17 106.6(3) . . ? O7 C18 H18A 110.4 . . ? C17 C18 H18A 110.4 . . ? O7 C18 H18B 110.4 . . ? C17 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? N4 C19 C20 110.7(3) . . ? N4 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? O8 C20 C19 111.1(3) . . ? O8 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? O8 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C22 C21 C24 108.9(3) . . ? C22 C21 C23 108.5(3) . . ? C24 C21 C23 108.3(3) . . ? C22 C21 C25 110.9(3) . . ? C24 C21 C25 109.6(3) . . ? C23 C21 C25 110.7(3) . . ? O9 C22 C21 113.7(3) . . ? O9 C22 H22A 108.8 . . ? C21 C22 H22A 108.8 . . ? O9 C22 H22B 108.8 . . ? C21 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? O10 C23 C21 114.5(3) . . ? O10 C23 H23A 108.6 . . ? C21 C23 H23A 108.6 . . ? O10 C23 H23B 108.6 . . ? C21 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? O11 C24 C21 113.4(3) . . ? O11 C24 H24A 108.9 . . ? C21 C24 H24A 108.9 . . ? O11 C24 H24B 108.9 . . ? C21 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C29 C26 C28 108.2(3) . . ? C29 C26 C30 109.5(3) . . ? C28 C26 C30 110.4(3) . . ? C29 C26 C27 109.2(3) . . ? C28 C26 C27 108.7(3) . . ? C30 C26 C27 110.7(3) . . ? O12 C27 C26 113.7(3) . . ? O12 C27 H27A 108.8 . . ? C26 C27 H27A 108.8 . . ? O12 C27 H27B 108.8 . . ? C26 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? O13 C28 C26 114.8(3) . . ? O13 C28 H28A 108.6 . . ? C26 C28 H28A 108.6 . . ? O13 C28 H28B 108.6 . . ? C26 C28 H28B 108.6 . . ? H28A C28 H28B 107.5 . . ? O14 C29 C26 113.7(3) . . ? O14 C29 H29A 108.8 . . ? C26 C29 H29A 108.8 . . ? O14 C29 H29B 108.8 . . ? C26 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 C32 113.5(3) . . ? N5 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? N5 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? N6 C32 C31 112.3(3) . . ? N6 C32 H32A 109.1 . . ? C31 C32 H32A 109.1 . . ? N6 C32 H32B 109.1 . . ? C31 C32 H32B 109.1 . . ? H32A C32 H32B 107.9 . . ? N5 C33 C34 112.0(3) . . ? N5 C33 H33A 109.2 . . ? C34 C33 H33A 109.2 . . ? N5 C33 H33B 109.2 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? O15 C34 C33 111.6(3) . . ? O15 C34 H34A 109.3 . . ? C33 C34 H34A 109.3 . . ? O15 C34 H34B 109.3 . . ? C33 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? N5 C35 C36 110.9(3) . . ? N5 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? N5 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.0 . . ? O16 C36 C35 106.5(3) . . ? O16 C36 H36A 110.4 . . ? C35 C36 H36A 110.4 . . ? O16 C36 H36B 110.4 . . ? C35 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? N6 C37 C38 112.4(3) . . ? N6 C37 H37A 109.1 . . ? C38 C37 H37A 109.1 . . ? N6 C37 H37B 109.1 . . ? C38 C37 H37B 109.1 . . ? H37A C37 H37B 107.9 . . ? O17 C38 C37 108.4(3) . . ? O17 C38 H38A 110.0 . . ? C37 C38 H38A 110.0 . . ? O17 C38 H38B 110.0 . . ? C37 C38 H38B 110.0 . . ? H38A C38 H38B 108.4 . . ? N6 C39 C40 114.6(3) . . ? N6 C39 H39A 108.6 . . ? C40 C39 H39A 108.6 . . ? N6 C39 H39B 108.6 . . ? C40 C39 H39B 108.6 . . ? H39A C39 H39B 107.6 . . ? O18 C40 C39 111.7(3) . . ? O18 C40 H40A 109.3 . . ? C39 C40 H40A 109.3 . . ? O18 C40 H40B 109.3 . . ? C39 C40 H40B 109.3 . . ? H40A C40 H40B 107.9 . . ? N7 C41 C42 113.1(3) . . ? N7 C41 H41A 109.0 . . ? C42 C41 H41A 109.0 . . ? N7 C41 H41B 109.0 . . ? C42 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? N8 C42 C41 112.4(3) . . ? N8 C42 H42A 109.1 . . ? C41 C42 H42A 109.1 . . ? N8 C42 H42B 109.1 . . ? C41 C42 H42B 109.1 . . ? H42A C42 H42B 107.9 . . ? N7 C43 C44 113.0(3) . . ? N7 C43 H43A 109.0 . . ? C44 C43 H43A 109.0 . . ? N7 C43 H43B 109.0 . . ? C44 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? O19 C44 C43 108.4(3) . . ? O19 C44 H44A 110.0 . . ? C43 C44 H44A 110.0 . . ? O19 C44 H44B 110.0 . . ? C43 C44 H44B 110.0 . . ? H44A C44 H44B 108.4 . . ? N7 C45 C46 114.4(3) . . ? N7 C45 H45A 108.7 . . ? C46 C45 H45A 108.7 . . ? N7 C45 H45B 108.7 . . ? C46 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? O20 C46 C45 112.1(3) . . ? O20 C46 H46A 109.2 . . ? C45 C46 H46A 109.2 . . ? O20 C46 H46B 109.2 . . ? C45 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? N8 C47 C48 111.7(3) . . ? N8 C47 H47A 109.3 . . ? C48 C47 H47A 109.3 . . ? N8 C47 H47B 109.3 . . ? C48 C47 H47B 109.3 . . ? H47A C47 H47B 107.9 . . ? O21 C48 C47 111.6(3) . . ? O21 C48 H48A 109.3 . . ? C47 C48 H48A 109.3 . . ? O21 C48 H48B 109.3 . . ? C47 C48 H48B 109.3 . . ? H48A C48 H48B 108.0 . . ? N8 C49 C50 111.3(3) . . ? N8 C49 H49A 109.4 . . ? C50 C49 H49A 109.4 . . ? N8 C49 H49B 109.4 . . ? C50 C49 H49B 109.4 . . ? H49A C49 H49B 108.0 . . ? O22 C50 C49 105.6(3) . . ? O22 C50 H50A 110.6 . . ? C49 C50 H50A 110.6 . . ? O22 C50 H50B 110.6 . . ? C49 C50 H50B 110.6 . . ? H50A C50 H50B 108.8 . . ? C52 C51 C53 108.0(4) . . ? C52 C51 C54 107.7(4) . . ? C53 C51 C54 108.8(4) . . ? C52 C51 C55 111.1(3) . . ? C53 C51 C55 110.6(3) . . ? C54 C51 C55 110.6(3) . . ? O23 C52 C51 115.3(3) . . ? O23 C52 H52A 108.4 . . ? C51 C52 H52A 108.4 . . ? O23 C52 H52B 108.4 . . ? C51 C52 H52B 108.4 . . ? H52A C52 H52B 107.5 . . ? O24 C53 C51 115.4(3) . . ? O24 C53 H53A 108.4 . . ? C51 C53 H53A 108.4 . . ? O24 C53 H53B 108.4 . . ? C51 C53 H53B 108.4 . . ? H53A C53 H53B 107.5 . . ? O25 C54 C51 115.0(3) . . ? O25 C54 H54A 108.5 . . ? C51 C54 H54A 108.5 . . ? O25 C54 H54B 108.5 . . ? C51 C54 H54B 108.5 . . ? H54A C54 H54B 107.5 . . ? C51 C55 H55A 109.5 . . ? C51 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C51 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C58 C56 C60 111.1(3) . . ? C58 C56 C57 107.6(3) . . ? C60 C56 C57 110.8(3) . . ? C58 C56 C59 108.5(3) . . ? C60 C56 C59 110.5(3) . . ? C57 C56 C59 108.3(3) . . ? O26 C57 C56 113.0(3) . . ? O26 C57 H57A 109.0 . . ? C56 C57 H57A 109.0 . . ? O26 C57 H57B 109.0 . . ? C56 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? O27 C58 C56 114.3(3) . . ? O27 C58 H58A 108.7 . . ? C56 C58 H58A 108.7 . . ? O27 C58 H58B 108.7 . . ? C56 C58 H58B 108.7 . . ? H58A C58 H58B 107.6 . . ? O28 C59 C56 113.2(3) . . ? O28 C59 H59A 108.9 . . ? C56 C59 H59A 108.9 . . ? O28 C59 H59B 108.9 . . ? C56 C59 H59B 108.9 . . ? H59A C59 H59B 107.8 . . ? C56 C60 H60A 109.5 . . ? C56 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C56 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N9 C61 C62 177.3(7) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N10 C63 C64 177.2(7) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 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 O4 H4O O14 0.85 1.81 2.634(3) 162.0 . O7 H7O O11 0.85 1.83 2.655(3) 162.2 . O16 H16O O28 0.85 1.85 2.672(3) 163.1 . O22 H22O O25 0.85 1.83 2.667(3) 168.0 . _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.540 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.077 #===============================END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 679169' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H68 Mn4 N4 O16' _chemical_formula_weight 984.66 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6698(12) _cell_length_b 12.0458(12) _cell_length_c 13.7154(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.795(2) _cell_angle_gamma 90.00 _cell_volume 2085.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2221 _cell_measurement_theta_min 2.335 _cell_measurement_theta_max 24.419 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7892 _exptl_absorpt_correction_T_max 0.8518 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; The 93.4% data completeness may be due to the irregular shape of the collected crystal. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8361 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3830 _reflns_number_gt 3245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 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^)+(0.0431P)^2^+0.7401P] 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 3830 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.42160(3) 0.40327(3) -0.06149(3) 0.02608(14) Uani 1 1 d . . . Mn2 Mn 0.32005(3) 0.61958(3) 0.03306(3) 0.02682(14) Uani 1 1 d . . . O1 O 0.43563(14) 0.58662(15) -0.05159(13) 0.0258(4) Uani 1 1 d . . . O2 O 0.56327(14) 0.38452(16) -0.13231(14) 0.0299(5) Uani 1 1 d . . . O3 O 0.31128(14) 0.45907(16) 0.04008(14) 0.0301(5) Uani 1 1 d . . . O4 O 0.44831(16) 0.21857(17) -0.01568(16) 0.0391(5) Uani 1 1 d . . . H4O H 0.5142 0.2122 -0.0221 0.047 Uiso 1 1 d R . . O5 O 0.34581(15) 0.77224(16) 0.02451(16) 0.0365(5) Uani 1 1 d . . . O6 O 0.21978(15) 0.63942(17) 0.12188(15) 0.0354(5) Uani 1 1 d . . . O7 O 0.21835(15) 0.62570(17) -0.07088(15) 0.0357(5) Uani 1 1 d . . . O8 O 0.1514(2) 0.5075(3) 0.2679(2) 0.0760(9) Uani 1 1 d . . . H8O H 0.1766 0.5467 0.2239 0.091 Uiso 1 1 d R . . N1 N 0.37679(18) 0.4656(2) -0.22699(18) 0.0324(6) Uani 1 1 d . . . N2 N 0.26623(18) 0.3041(2) -0.11432(18) 0.0331(6) Uani 1 1 d . . . C1 C 0.2729(2) 0.4212(3) -0.2634(2) 0.0438(8) Uani 1 1 d . . . H1A H 0.2692 0.4170 -0.3342 0.053 Uiso 1 1 calc R . . H1B H 0.2180 0.4719 -0.2459 0.053 Uiso 1 1 calc R . . C2 C 0.2516(3) 0.3066(3) -0.2225(2) 0.0442(8) Uani 1 1 d . . . H2A H 0.1796 0.2847 -0.2435 0.053 Uiso 1 1 calc R . . H2B H 0.2992 0.2533 -0.2487 0.053 Uiso 1 1 calc R . . C3 C 0.3758(2) 0.5884(2) -0.2259(2) 0.0342(7) Uani 1 1 d . . . H3A H 0.3036 0.6134 -0.2208 0.041 Uiso 1 1 calc R . . H3B H 0.3980 0.6152 -0.2876 0.041 Uiso 1 1 calc R . . C4 C 0.4461(2) 0.6396(3) -0.1435(2) 0.0333(7) Uani 1 1 d . . . H4A H 0.5193 0.6348 -0.1589 0.040 Uiso 1 1 calc R . . H4B H 0.4284 0.7176 -0.1381 0.040 Uiso 1 1 calc R . . C5 C 0.4615(2) 0.4184(3) -0.2823(2) 0.0366(7) Uani 1 1 d . . . H5A H 0.4628 0.4576 -0.3440 0.044 Uiso 1 1 calc R . . H5B H 0.4454 0.3411 -0.2970 0.044 Uiso 1 1 calc R . . C6 C 0.5700(2) 0.4256(3) -0.2273(2) 0.0321(7) Uani 1 1 d . . . H6A H 0.6205 0.3822 -0.2606 0.039 Uiso 1 1 calc R . . H6B H 0.5939 0.5021 -0.2245 0.039 Uiso 1 1 calc R . . C7 C 0.1811(2) 0.3651(3) -0.0707(2) 0.0404(8) Uani 1 1 d . . . H7A H 0.1189 0.3181 -0.0710 0.048 Uiso 1 1 calc R . . H7B H 0.1623 0.4301 -0.1102 0.048 Uiso 1 1 calc R . . C8 C 0.2139(2) 0.4013(3) 0.0338(2) 0.0389(8) Uani 1 1 d . . . H8A H 0.1594 0.4489 0.0568 0.047 Uiso 1 1 calc R . . H8B H 0.2203 0.3365 0.0758 0.047 Uiso 1 1 calc R . . C9 C 0.2737(2) 0.1878(3) -0.0791(3) 0.0415(8) Uani 1 1 d . . . H9A H 0.2275 0.1410 -0.1214 0.050 Uiso 1 1 calc R . . H9B H 0.2505 0.1837 -0.0135 0.050 Uiso 1 1 calc R . . C10 C 0.3857(2) 0.1465(3) -0.0782(3) 0.0425(8) Uani 1 1 d . . . H10A H 0.3908 0.0709 -0.0538 0.051 Uiso 1 1 calc R . . H10B H 0.4093 0.1480 -0.1436 0.051 Uiso 1 1 calc R . . C11 C 0.1538(2) 0.7895(3) 0.0112(2) 0.0380(8) Uani 1 1 d . . . C12 C 0.0666(3) 0.8778(3) 0.0006(3) 0.0562(10) Uani 1 1 d . . . H12A H -0.0014 0.8425 -0.0009 0.084 Uiso 1 1 calc R . . H12B H 0.0719 0.9184 -0.0590 0.084 Uiso 1 1 calc R . . H12C H 0.0748 0.9280 0.0552 0.084 Uiso 1 1 calc R . . C13 C 0.2607(2) 0.8425(3) -0.0015(3) 0.0428(8) Uani 1 1 d . . . H13A H 0.2631 0.8644 -0.0694 0.051 Uiso 1 1 calc R . . H13B H 0.2678 0.9092 0.0382 0.051 Uiso 1 1 calc R . . C14 C 0.1576(3) 0.7364(3) 0.1121(3) 0.0442(8) Uani 1 1 d . . . H14A H 0.1854 0.7902 0.1603 0.053 Uiso 1 1 calc R . . H14B H 0.0859 0.7184 0.1266 0.053 Uiso 1 1 calc R . . C15 C 0.1337(3) 0.6993(3) -0.0655(3) 0.0494(9) Uani 1 1 d . . . H15A H 0.0714 0.6574 -0.0511 0.059 Uiso 1 1 calc R . . H15B H 0.1185 0.7340 -0.1290 0.059 Uiso 1 1 calc R . . C16 C 0.0470(4) 0.4864(5) 0.2388(3) 0.0871(16) Uani 1 1 d . . . H16A H 0.0055 0.5513 0.2492 0.131 Uiso 1 1 calc R . . H16B H 0.0224 0.4258 0.2763 0.131 Uiso 1 1 calc R . . H16C H 0.0402 0.4674 0.1706 0.131 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0259(2) 0.0242(2) 0.0281(3) -0.00115(18) 0.00222(18) -0.00056(16) Mn2 0.0254(2) 0.0254(2) 0.0297(3) -0.00044(18) 0.00254(18) 0.00339(17) O1 0.0290(10) 0.0248(10) 0.0238(11) 0.0027(8) 0.0042(8) 0.0031(8) O2 0.0274(10) 0.0357(11) 0.0265(12) 0.0029(9) 0.0023(8) 0.0036(8) O3 0.0279(10) 0.0274(11) 0.0356(12) -0.0012(9) 0.0058(9) -0.0011(8) O4 0.0333(11) 0.0328(12) 0.0509(15) -0.0025(10) 0.0020(10) -0.0031(9) O5 0.0323(11) 0.0259(11) 0.0510(14) 0.0007(9) 0.0026(10) 0.0038(8) O6 0.0328(11) 0.0395(12) 0.0352(13) 0.0012(10) 0.0103(9) 0.0085(9) O7 0.0318(11) 0.0387(12) 0.0357(13) -0.0034(9) -0.0020(9) 0.0083(9) O8 0.074(2) 0.098(3) 0.0549(18) 0.0306(16) -0.0018(15) -0.0099(17) N1 0.0305(13) 0.0365(14) 0.0295(15) -0.0018(11) -0.0019(11) -0.0004(11) N2 0.0328(13) 0.0324(14) 0.0344(16) -0.0036(11) 0.0033(11) -0.0046(10) C1 0.0377(18) 0.059(2) 0.033(2) 0.0002(16) -0.0062(14) -0.0053(15) C2 0.0396(18) 0.051(2) 0.040(2) -0.0119(16) -0.0072(15) -0.0097(15) C3 0.0382(17) 0.0391(18) 0.0251(18) 0.0040(13) 0.0016(13) 0.0037(13) C4 0.0408(17) 0.0303(16) 0.0295(18) 0.0042(13) 0.0060(13) 0.0001(13) C5 0.0401(17) 0.0435(19) 0.0260(18) -0.0061(14) 0.0023(13) 0.0011(14) C6 0.0323(16) 0.0357(17) 0.0292(18) -0.0012(13) 0.0077(13) 0.0021(12) C7 0.0282(16) 0.0439(19) 0.049(2) -0.0040(15) 0.0011(14) -0.0063(13) C8 0.0344(16) 0.0370(18) 0.047(2) -0.0035(15) 0.0122(15) -0.0045(13) C9 0.0420(18) 0.0335(17) 0.048(2) -0.0026(15) 0.0009(15) -0.0117(14) C10 0.0470(19) 0.0311(17) 0.050(2) -0.0068(15) 0.0051(16) -0.0036(14) C11 0.0360(17) 0.0374(18) 0.041(2) 0.0026(14) 0.0031(14) 0.0138(13) C12 0.048(2) 0.051(2) 0.070(3) 0.0088(19) 0.0075(19) 0.0237(17) C13 0.0429(18) 0.0334(17) 0.052(2) 0.0043(15) 0.0017(16) 0.0098(14) C14 0.0375(18) 0.0417(19) 0.054(2) -0.0011(16) 0.0106(16) 0.0122(14) C15 0.0394(18) 0.051(2) 0.055(2) -0.0080(17) -0.0138(16) 0.0132(16) C16 0.069(3) 0.128(5) 0.066(3) 0.001(3) 0.016(3) -0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 2.1231(18) . ? Mn1 O3 2.1613(18) . ? Mn1 O1 2.2191(18) . ? Mn1 O1 2.2854(19) 3_665 ? Mn1 O4 2.329(2) . ? Mn1 N2 2.364(2) . ? Mn1 N1 2.413(2) . ? Mn1 Mn2 3.2257(6) . ? Mn1 Mn2 3.2755(6) 3_665 ? Mn1 Mn1 3.4151(9) 3_665 ? Mn2 O7 1.841(2) . ? Mn2 O6 1.8476(19) . ? Mn2 O5 1.873(2) . ? Mn2 O2 1.925(2) 3_665 ? Mn2 O3 1.940(2) . ? Mn2 O1 1.9836(18) . ? Mn2 Mn1 3.2755(6) 3_665 ? Mn2 Mn2 5.5323(9) 3_665 ? O1 C4 1.428(3) . ? O1 Mn1 2.2855(19) 3_665 ? O2 C6 1.403(3) . ? O2 Mn2 1.925(2) 3_665 ? O3 C8 1.413(3) . ? O4 C10 1.415(4) . ? O4 H4O 0.8500 . ? O5 C13 1.394(3) . ? O6 C14 1.409(4) . ? O7 C15 1.398(4) . ? O8 C16 1.372(5) . ? O8 H8O 0.8499 . ? N1 C1 1.469(4) . ? N1 C3 1.479(4) . ? N1 C5 1.480(4) . ? N2 C7 1.473(4) . ? N2 C2 1.480(4) . ? N2 C9 1.482(4) . ? C1 C2 1.523(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.512(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.514(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.522(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.503(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C15 1.520(5) . ? C11 C13 1.521(4) . ? C11 C14 1.521(5) . ? C11 C12 1.532(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O3 160.90(7) . . ? O2 Mn1 O1 93.86(7) . . ? O3 Mn1 O1 72.78(7) . . ? O2 Mn1 O1 70.41(7) . 3_665 ? O3 Mn1 O1 93.66(7) . 3_665 ? O1 Mn1 O1 81.41(7) . 3_665 ? O2 Mn1 O4 84.98(7) . . ? O3 Mn1 O4 102.15(7) . . ? O1 Mn1 O4 157.71(7) . . ? O1 Mn1 O4 77.23(7) 3_665 . ? O2 Mn1 N2 121.34(8) . . ? O3 Mn1 N2 77.76(8) . . ? O1 Mn1 N2 125.61(8) . . ? O1 Mn1 N2 145.73(8) 3_665 . ? O4 Mn1 N2 72.44(8) . . ? O2 Mn1 N1 75.18(8) . . ? O3 Mn1 N1 113.29(8) . . ? O1 Mn1 N1 76.06(8) . . ? O1 Mn1 N1 137.08(7) 3_665 . ? O4 Mn1 N1 124.65(8) . . ? N2 Mn1 N1 75.21(8) . . ? O2 Mn1 Mn2 130.59(6) . . ? O3 Mn1 Mn2 35.76(5) . . ? O1 Mn1 Mn2 37.25(5) . . ? O1 Mn1 Mn2 90.22(5) 3_665 . ? O4 Mn1 Mn2 135.82(6) . . ? N2 Mn1 Mn2 100.47(6) . . ? N1 Mn1 Mn2 93.23(6) . . ? O2 Mn1 Mn2 33.99(5) . 3_665 ? O3 Mn1 Mn2 130.02(5) . 3_665 ? O1 Mn1 Mn2 90.12(5) . 3_665 ? O1 Mn1 Mn2 36.61(5) 3_665 3_665 ? O4 Mn1 Mn2 76.49(5) . 3_665 ? N2 Mn1 Mn2 142.39(6) . 3_665 ? N1 Mn1 Mn2 107.00(6) . 3_665 ? Mn2 Mn1 Mn2 116.630(15) . 3_665 ? O2 Mn1 Mn1 79.59(5) . 3_665 ? O3 Mn1 Mn1 81.39(5) . 3_665 ? O1 Mn1 Mn1 41.43(5) . 3_665 ? O1 Mn1 Mn1 39.98(5) 3_665 3_665 ? O4 Mn1 Mn1 116.95(6) . 3_665 ? N2 Mn1 Mn1 158.66(6) . 3_665 ? N1 Mn1 Mn1 109.48(6) . 3_665 ? Mn2 Mn1 Mn1 59.026(15) . 3_665 ? Mn2 Mn1 Mn1 57.604(14) 3_665 3_665 ? O7 Mn2 O6 91.72(9) . . ? O7 Mn2 O5 91.52(9) . . ? O6 Mn2 O5 92.71(9) . . ? O7 Mn2 O2 174.23(9) . 3_665 ? O6 Mn2 O2 93.83(9) . 3_665 ? O5 Mn2 O2 86.67(9) . 3_665 ? O7 Mn2 O3 92.24(9) . . ? O6 Mn2 O3 92.91(9) . . ? O5 Mn2 O3 173.14(8) . . ? O2 Mn2 O3 89.03(8) 3_665 . ? O7 Mn2 O1 93.32(8) . . ? O6 Mn2 O1 173.61(8) . . ? O5 Mn2 O1 91.08(8) . . ? O2 Mn2 O1 81.25(8) 3_665 . ? O3 Mn2 O1 82.97(7) . . ? O7 Mn2 Mn1 89.88(6) . . ? O6 Mn2 Mn1 133.54(7) . . ? O5 Mn2 Mn1 133.66(6) . . ? O2 Mn2 Mn1 87.42(6) 3_665 . ? O3 Mn2 Mn1 40.63(5) . . ? O1 Mn2 Mn1 42.63(5) . . ? O7 Mn2 Mn1 136.31(7) . 3_665 ? O6 Mn2 Mn1 131.89(7) . 3_665 ? O5 Mn2 Mn1 84.97(6) . 3_665 ? O2 Mn2 Mn1 38.07(6) 3_665 3_665 ? O3 Mn2 Mn1 88.35(5) . 3_665 ? O1 Mn2 Mn1 43.41(5) . 3_665 ? Mn1 Mn2 Mn1 63.370(15) . 3_665 ? O7 Mn2 Mn2 115.27(6) . 3_665 ? O6 Mn2 Mn2 142.85(7) . 3_665 ? O5 Mn2 Mn2 110.53(6) . 3_665 ? O2 Mn2 Mn2 60.51(6) 3_665 3_665 ? O3 Mn2 Mn2 62.64(5) . 3_665 ? O1 Mn2 Mn2 30.78(5) . 3_665 ? Mn1 Mn2 Mn2 31.956(9) . 3_665 ? Mn1 Mn2 Mn2 31.414(9) 3_665 3_665 ? C4 O1 Mn2 123.68(17) . . ? C4 O1 Mn1 113.81(16) . . ? Mn2 O1 Mn1 100.12(8) . . ? C4 O1 Mn1 116.62(16) . 3_665 ? Mn2 O1 Mn1 99.98(8) . 3_665 ? Mn1 O1 Mn1 98.59(7) . 3_665 ? C6 O2 Mn2 124.27(16) . 3_665 ? C6 O2 Mn1 120.45(16) . . ? Mn2 O2 Mn1 107.94(9) 3_665 . ? C8 O3 Mn2 122.76(17) . . ? C8 O3 Mn1 114.58(17) . . ? Mn2 O3 Mn1 103.61(8) . . ? C10 O4 Mn1 111.18(19) . . ? C10 O4 H4O 112.7 . . ? Mn1 O4 H4O 100.4 . . ? C13 O5 Mn2 118.50(19) . . ? C14 O6 Mn2 117.02(18) . . ? C15 O7 Mn2 118.37(19) . . ? C16 O8 H8O 107.9 . . ? C1 N1 C3 111.0(2) . . ? C1 N1 C5 110.7(2) . . ? C3 N1 C5 113.4(2) . . ? C1 N1 Mn1 109.89(18) . . ? C3 N1 Mn1 107.63(17) . . ? C5 N1 Mn1 103.84(17) . . ? C7 N2 C2 111.2(3) . . ? C7 N2 C9 111.6(2) . . ? C2 N2 C9 110.3(2) . . ? C7 N2 Mn1 104.03(17) . . ? C2 N2 Mn1 109.15(17) . . ? C9 N2 Mn1 110.40(18) . . ? N1 C1 C2 112.7(3) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? N2 C2 C1 112.2(3) . . ? N2 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? N2 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N1 C3 C4 114.3(2) . . ? N1 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? O1 C4 C3 112.6(2) . . ? O1 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? O1 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? N1 C5 C6 112.9(2) . . ? N1 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? N1 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? O2 C6 C5 108.6(2) . . ? O2 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O2 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.3 . . ? N2 C7 C8 112.0(3) . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? O3 C8 C7 111.5(2) . . ? O3 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? O3 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N2 C9 C10 110.5(2) . . ? N2 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? O4 C10 C9 106.4(3) . . ? O4 C10 H10A 110.4 . . ? C9 C10 H10A 110.4 . . ? O4 C10 H10B 110.4 . . ? C9 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? C15 C11 C13 108.7(3) . . ? C15 C11 C14 108.7(3) . . ? C13 C11 C14 108.7(3) . . ? C15 C11 C12 110.7(3) . . ? C13 C11 C12 109.8(3) . . ? C14 C11 C12 110.2(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O5 C13 C11 113.1(3) . . ? O5 C13 H13A 109.0 . . ? C11 C13 H13A 109.0 . . ? O5 C13 H13B 109.0 . . ? C11 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? O6 C14 C11 114.2(2) . . ? O6 C14 H14A 108.7 . . ? C11 C14 H14A 108.7 . . ? O6 C14 H14B 108.7 . . ? C11 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? O7 C15 C11 113.8(3) . . ? O7 C15 H15A 108.8 . . ? C11 C15 H15A 108.8 . . ? O7 C15 H15B 108.8 . . ? C11 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? O8 C16 H16A 109.5 . . ? O8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 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 O4 H4O O5 0.85 1.79 2.624(3) 167.7 3_665 O8 H8O O6 0.85 1.91 2.753(3) 174.5 . _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.342 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.066 #===============================END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 679170' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H48 Fe4 N24 O8' _chemical_formula_weight 1024.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.1541(10) _cell_length_b 10.5976(10) _cell_length_c 11.1148(10) _cell_angle_alpha 72.778(2) _cell_angle_beta 65.002(2) _cell_angle_gamma 70.456(2) _cell_volume 1004.66(16) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2265 _cell_measurement_theta_min 2.462 _cell_measurement_theta_max 27.122 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 1.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7545 _exptl_absorpt_correction_T_max 0.7962 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5840 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3824 _reflns_number_gt 3252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 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^)+(0.0473P)^2^+0.5462P] 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 3824 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.58106(4) 0.86638(4) 0.09828(4) 0.02313(12) Uani 1 1 d . . . Fe2 Fe 0.49076(5) 0.82102(4) -0.13730(4) 0.02866(13) Uani 1 1 d . . . N1 N 0.8295(3) 0.8389(2) 0.0271(2) 0.0286(5) Uani 1 1 d . . . N2 N 0.6500(3) 0.7444(2) 0.2937(2) 0.0328(6) Uani 1 1 d . . . N3 N 0.6243(4) 0.7317(3) -0.2937(3) 0.0521(8) Uani 1 1 d . . . N4 N 0.7076(4) 0.6294(3) -0.3207(3) 0.0519(8) Uani 1 1 d . . . N5 N 0.7893(6) 0.5301(5) -0.3506(6) 0.1217(19) Uani 1 1 d . . . N6 N 0.4198(3) 0.6595(2) 0.0042(3) 0.0398(6) Uani 1 1 d . . . N7 N 0.3204(3) 0.6148(3) 0.0132(3) 0.0410(7) Uani 1 1 d . . . N8 N 0.2274(4) 0.5705(3) 0.0222(4) 0.0579(9) Uani 1 1 d . . . N9 N 0.3099(3) 0.8658(3) -0.1920(3) 0.0405(6) Uani 1 1 d . . . N10 N 0.2970(3) 0.7989(3) -0.2545(3) 0.0365(6) Uani 1 1 d . . . N11 N 0.2818(4) 0.7372(3) -0.3147(3) 0.0560(8) Uani 1 1 d . . . O1 O 0.6058(2) 1.06151(17) -0.02391(18) 0.0233(4) Uani 1 1 d . . . O2 O 0.6541(2) 0.78145(19) -0.06195(19) 0.0280(4) Uani 1 1 d . . . O3 O 0.4682(2) 0.70696(19) 0.2000(2) 0.0334(5) Uani 1 1 d . . . H3O H 0.4458 0.6866 0.1437 0.040 Uiso 1 1 d R . . O4 O 0.4739(2) 0.99077(18) 0.22687(18) 0.0270(4) Uani 1 1 d . . . C1 C 0.8862(4) 0.8015(3) 0.1402(3) 0.0370(7) Uani 1 1 d . . . H1A H 0.8645 0.8822 0.1761 0.044 Uiso 1 1 calc R . . H1B H 0.9940 0.7662 0.1063 0.044 Uiso 1 1 calc R . . C2 C 0.8146(4) 0.6960(3) 0.2512(3) 0.0401(7) Uani 1 1 d . . . H2A H 0.8472 0.6108 0.2192 0.048 Uiso 1 1 calc R . . H2B H 0.8448 0.6800 0.3275 0.048 Uiso 1 1 calc R . . C3 C 0.5904(4) 0.8472(3) 0.3815(3) 0.0374(7) Uani 1 1 d . . . H3A H 0.6622 0.9011 0.3551 0.045 Uiso 1 1 calc R . . H3B H 0.5731 0.8023 0.4747 0.045 Uiso 1 1 calc R . . C4 C 0.4461(4) 0.9377(3) 0.3675(3) 0.0359(7) Uani 1 1 d . . . H4A H 0.3703 0.8862 0.4040 0.043 Uiso 1 1 calc R . . H4B H 0.4104 1.0117 0.4167 0.043 Uiso 1 1 calc R . . C5 C 0.5766(4) 0.6290(3) 0.3627(3) 0.0396(7) Uani 1 1 d . . . H5A H 0.6404 0.5539 0.4028 0.047 Uiso 1 1 calc R . . H5B H 0.4824 0.6573 0.4340 0.047 Uiso 1 1 calc R . . C6 C 0.5496(4) 0.5851(3) 0.2620(3) 0.0392(7) Uani 1 1 d . . . H6A H 0.6435 0.5472 0.1955 0.047 Uiso 1 1 calc R . . H6B H 0.4911 0.5172 0.3055 0.047 Uiso 1 1 calc R . . C7 C 0.8680(3) 0.9681(3) -0.0601(3) 0.0312(6) Uani 1 1 d . . . H7A H 0.9646 0.9466 -0.1312 0.037 Uiso 1 1 calc R . . H7B H 0.8768 1.0201 -0.0064 0.037 Uiso 1 1 calc R . . C8 C 0.7538(3) 1.0543(3) -0.1230(3) 0.0295(6) Uani 1 1 d . . . H8A H 0.7703 1.1452 -0.1599 0.035 Uiso 1 1 calc R . . H8B H 0.7645 1.0153 -0.1963 0.035 Uiso 1 1 calc R . . C9 C 0.8941(3) 0.7255(3) -0.0500(3) 0.0356(7) Uani 1 1 d . . . H9A H 0.8897 0.6394 0.0123 0.043 Uiso 1 1 calc R . . H9B H 0.9984 0.7235 -0.1051 0.043 Uiso 1 1 calc R . . C10 C 0.8087(3) 0.7439(3) -0.1387(3) 0.0326(7) Uani 1 1 d . . . H10A H 0.8359 0.8143 -0.2170 0.039 Uiso 1 1 calc R . . H10B H 0.8320 0.6598 -0.1696 0.039 Uiso 1 1 calc R . . N12 N 0.9147(6) 0.9234(6) 0.3979(5) 0.1186(19) Uani 1 1 d . . . C11 C 0.9894(5) 0.8410(6) 0.4460(4) 0.0700(12) Uani 1 1 d . . . C12 C 1.0880(6) 0.7331(5) 0.5033(5) 0.0817(14) Uani 1 1 d . . . H12A H 1.0362 0.6643 0.5624 0.123 Uiso 1 1 calc R . . H12B H 1.1203 0.7687 0.5534 0.123 Uiso 1 1 calc R . . H12C H 1.1736 0.6941 0.4323 0.123 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0255(2) 0.0237(2) 0.0223(2) -0.00360(15) -0.00970(17) -0.00750(16) Fe2 0.0353(3) 0.0269(2) 0.0309(2) -0.00682(17) -0.01702(19) -0.00809(18) N1 0.0259(12) 0.0309(12) 0.0309(13) -0.0063(10) -0.0119(10) -0.0062(10) N2 0.0405(15) 0.0327(12) 0.0287(13) 0.0019(10) -0.0177(11) -0.0126(11) N3 0.064(2) 0.0540(18) 0.0423(17) -0.0249(15) -0.0259(16) 0.0035(16) N4 0.0528(19) 0.0569(19) 0.0535(19) -0.0285(16) -0.0129(15) -0.0142(16) N5 0.116(4) 0.088(3) 0.148(5) -0.081(3) -0.028(4) 0.018(3) N6 0.0530(17) 0.0309(13) 0.0502(17) 0.0006(12) -0.0302(14) -0.0197(13) N7 0.0493(18) 0.0288(13) 0.0458(17) -0.0059(12) -0.0208(14) -0.0067(13) N8 0.0526(19) 0.0478(17) 0.083(2) -0.0044(16) -0.0308(18) -0.0215(15) N9 0.0474(17) 0.0361(14) 0.0520(17) -0.0105(13) -0.0302(14) -0.0089(12) N10 0.0399(15) 0.0383(14) 0.0380(15) -0.0027(12) -0.0217(13) -0.0112(12) N11 0.071(2) 0.0574(19) 0.062(2) -0.0161(16) -0.0399(18) -0.0166(17) O1 0.0232(10) 0.0248(9) 0.0227(10) -0.0025(7) -0.0079(8) -0.0087(7) O2 0.0239(10) 0.0340(10) 0.0285(10) -0.0123(8) -0.0093(8) -0.0044(8) O3 0.0479(13) 0.0289(10) 0.0328(11) 0.0031(8) -0.0232(10) -0.0169(9) O4 0.0368(11) 0.0279(10) 0.0193(10) -0.0043(8) -0.0112(8) -0.0101(8) C1 0.0324(17) 0.0428(17) 0.0423(19) -0.0040(14) -0.0230(15) -0.0078(14) C2 0.0449(19) 0.0395(17) 0.0422(19) -0.0014(14) -0.0289(16) -0.0060(14) C3 0.052(2) 0.0413(17) 0.0251(16) -0.0018(13) -0.0202(15) -0.0142(15) C4 0.0462(19) 0.0391(16) 0.0218(15) -0.0064(13) -0.0087(14) -0.0135(14) C5 0.051(2) 0.0348(16) 0.0352(17) 0.0091(13) -0.0218(15) -0.0178(14) C6 0.052(2) 0.0267(15) 0.0418(19) 0.0030(13) -0.0222(16) -0.0137(14) C7 0.0260(15) 0.0350(15) 0.0335(16) -0.0032(13) -0.0093(13) -0.0127(12) C8 0.0265(15) 0.0313(14) 0.0277(15) -0.0015(12) -0.0061(12) -0.0115(12) C9 0.0258(15) 0.0362(16) 0.0446(19) -0.0127(14) -0.0138(14) -0.0011(13) C10 0.0305(16) 0.0344(15) 0.0314(16) -0.0126(13) -0.0069(13) -0.0060(12) N12 0.081(3) 0.163(5) 0.080(3) -0.005(3) -0.027(3) -0.008(3) C11 0.051(3) 0.105(4) 0.050(3) -0.016(3) -0.009(2) -0.025(3) C12 0.075(3) 0.093(4) 0.076(3) -0.029(3) -0.028(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O4 1.9509(18) . ? Fe1 O2 1.9794(18) . ? Fe1 O3 2.1247(19) . ? Fe1 O1 2.1400(18) . ? Fe1 O1 2.2017(18) 2_675 ? Fe1 N1 2.243(2) . ? Fe1 N2 2.428(2) . ? Fe1 Fe2 3.2652(6) 2_675 ? Fe1 Fe2 3.3162(6) . ? Fe1 Fe1 3.4292(8) 2_675 ? Fe2 N3 1.970(3) . ? Fe2 O4 2.0247(18) 2_675 ? Fe2 O2 2.0316(19) . ? Fe2 N9 2.039(3) . ? Fe2 N6 2.049(3) . ? Fe2 O1 2.1774(18) 2_675 ? Fe2 Fe1 3.2652(6) 2_675 ? Fe2 Fe2 5.6177(8) 2_675 ? N1 C9 1.489(4) . ? N1 C7 1.490(3) . ? N1 C1 1.494(4) . ? N2 C2 1.477(4) . ? N2 C3 1.482(4) . ? N2 C5 1.487(4) . ? N3 N4 1.160(4) . ? N4 N5 1.139(5) . ? N6 N7 1.208(4) . ? N7 N8 1.145(4) . ? N9 N10 1.197(3) . ? N10 N11 1.146(4) . ? O1 C8 1.433(3) . ? O1 Fe2 2.1774(18) 2_675 ? O1 Fe1 2.2017(18) 2_675 ? O2 C10 1.415(3) . ? O3 C6 1.437(3) . ? O3 H3O 0.8501 . ? O4 C4 1.432(3) . ? O4 Fe2 2.0247(18) 2_675 ? C1 C2 1.507(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.502(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.483(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.506(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.503(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? N12 C11 1.117(6) . ? C11 C12 1.434(7) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 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 O4 Fe1 O2 163.01(8) . . ? O4 Fe1 O3 100.29(8) . . ? O2 Fe1 O3 84.67(8) . . ? O4 Fe1 O1 76.27(7) . . ? O2 Fe1 O1 92.19(8) . . ? O3 Fe1 O1 154.44(8) . . ? O4 Fe1 O1 89.85(7) . 2_675 ? O2 Fe1 O1 75.04(7) . 2_675 ? O3 Fe1 O1 79.02(7) . 2_675 ? O1 Fe1 O1 75.67(7) . 2_675 ? O4 Fe1 N1 111.25(8) . . ? O2 Fe1 N1 77.94(8) . . ? O3 Fe1 N1 124.81(8) . . ? O1 Fe1 N1 78.86(8) . . ? O1 Fe1 N1 141.75(8) 2_675 . ? O4 Fe1 N2 76.05(8) . . ? O2 Fe1 N2 120.79(8) . . ? O3 Fe1 N2 70.75(8) . . ? O1 Fe1 N2 130.78(8) . . ? O1 Fe1 N2 143.36(8) 2_675 . ? N1 Fe1 N2 74.44(9) . . ? O4 Fe1 Fe2 35.53(5) . 2_675 ? O2 Fe1 Fe2 133.28(6) . 2_675 ? O3 Fe1 Fe2 133.73(6) . 2_675 ? O1 Fe1 Fe2 41.29(5) . 2_675 ? O1 Fe1 Fe2 86.32(5) 2_675 2_675 ? N1 Fe1 Fe2 93.03(6) . 2_675 ? N2 Fe1 Fe2 99.71(6) . 2_675 ? O4 Fe1 Fe2 130.27(6) . . ? O2 Fe1 Fe2 34.74(6) . . ? O3 Fe1 Fe2 77.00(5) . . ? O1 Fe1 Fe2 85.99(5) . . ? O1 Fe1 Fe2 40.50(5) 2_675 . ? N1 Fe1 Fe2 110.16(6) . . ? N2 Fe1 Fe2 142.01(6) . . ? Fe2 Fe1 Fe2 117.201(13) 2_675 . ? O4 Fe1 Fe1 81.39(6) . 2_675 ? O2 Fe1 Fe1 81.85(6) . 2_675 ? O3 Fe1 Fe1 116.15(6) . 2_675 ? O1 Fe1 Fe1 38.47(5) . 2_675 ? O1 Fe1 Fe1 37.20(4) 2_675 2_675 ? N1 Fe1 Fe1 112.56(6) . 2_675 ? N2 Fe1 Fe1 157.34(6) . 2_675 ? Fe2 Fe1 Fe1 59.328(13) 2_675 2_675 ? Fe2 Fe1 Fe1 57.873(14) . 2_675 ? N3 Fe2 O4 96.66(11) . 2_675 ? N3 Fe2 O2 94.07(11) . . ? O4 Fe2 O2 89.59(8) 2_675 . ? N3 Fe2 N9 92.25(12) . . ? O4 Fe2 N9 91.33(9) 2_675 . ? O2 Fe2 N9 173.46(10) . . ? N3 Fe2 N6 100.96(12) . . ? O4 Fe2 N6 162.25(9) 2_675 . ? O2 Fe2 N6 86.99(9) . . ? N9 Fe2 N6 90.18(11) . . ? N3 Fe2 O1 165.04(11) . 2_675 ? O4 Fe2 O1 73.96(7) 2_675 2_675 ? O2 Fe2 O1 74.58(7) . 2_675 ? N9 Fe2 O1 99.47(9) . 2_675 ? N6 Fe2 O1 88.34(9) . 2_675 ? N3 Fe2 Fe1 130.63(10) . 2_675 ? O4 Fe2 Fe1 34.05(5) 2_675 2_675 ? O2 Fe2 Fe1 85.52(5) . 2_675 ? N9 Fe2 Fe1 91.63(7) . 2_675 ? N6 Fe2 Fe1 128.22(8) . 2_675 ? O1 Fe2 Fe1 40.44(5) 2_675 2_675 ? N3 Fe2 Fe1 127.67(9) . . ? O4 Fe2 Fe1 83.44(5) 2_675 . ? O2 Fe2 Fe1 33.73(5) . . ? N9 Fe2 Fe1 140.05(8) . . ? N6 Fe2 Fe1 84.07(7) . . ? O1 Fe2 Fe1 41.05(5) 2_675 . ? Fe1 Fe2 Fe1 62.799(13) 2_675 . ? N3 Fe2 Fe2 137.67(10) . 2_675 ? O4 Fe2 Fe2 56.70(5) 2_675 2_675 ? O2 Fe2 Fe2 57.56(5) . 2_675 ? N9 Fe2 Fe2 117.97(7) . 2_675 ? N6 Fe2 Fe2 107.38(7) . 2_675 ? O1 Fe2 Fe2 27.43(5) 2_675 2_675 ? Fe1 Fe2 Fe2 31.671(8) 2_675 2_675 ? Fe1 Fe2 Fe2 31.128(8) . 2_675 ? C9 N1 C7 111.9(2) . . ? C9 N1 C1 109.6(2) . . ? C7 N1 C1 109.1(2) . . ? C9 N1 Fe1 104.34(16) . . ? C7 N1 Fe1 108.69(16) . . ? C1 N1 Fe1 113.09(18) . . ? C2 N2 C3 111.6(2) . . ? C2 N2 C5 111.1(2) . . ? C3 N2 C5 110.4(2) . . ? C2 N2 Fe1 109.73(18) . . ? C3 N2 Fe1 103.92(16) . . ? C5 N2 Fe1 109.83(17) . . ? N4 N3 Fe2 141.3(3) . . ? N5 N4 N3 178.1(5) . . ? N7 N6 Fe2 124.9(2) . . ? N8 N7 N6 178.9(3) . . ? N10 N9 Fe2 123.4(2) . . ? N11 N10 N9 178.4(3) . . ? C8 O1 Fe1 111.55(15) . . ? C8 O1 Fe2 123.99(15) . 2_675 ? Fe1 O1 Fe2 98.27(7) . 2_675 ? C8 O1 Fe1 117.13(15) . 2_675 ? Fe1 O1 Fe1 104.33(7) . 2_675 ? Fe2 O1 Fe1 98.45(7) 2_675 2_675 ? C10 O2 Fe1 121.38(16) . . ? C10 O2 Fe2 123.34(17) . . ? Fe1 O2 Fe2 111.53(9) . . ? C6 O3 Fe1 115.76(18) . . ? C6 O3 H3O 108.6 . . ? Fe1 O3 H3O 108.2 . . ? C4 O4 Fe1 119.19(17) . . ? C4 O4 Fe2 123.25(16) . 2_675 ? Fe1 O4 Fe2 110.42(9) . 2_675 ? N1 C1 C2 111.1(2) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 109.4(2) . . ? N2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 108.7(2) . . ? N2 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? N2 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.3 . . ? O4 C4 C3 108.0(2) . . ? O4 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O4 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C6 C5 N2 108.7(2) . . ? C6 C5 H5A 110.0 . . ? N2 C5 H5A 110.0 . . ? C6 C5 H5B 110.0 . . ? N2 C5 H5B 110.0 . . ? H5A C5 H5B 108.3 . . ? O3 C6 C5 104.8(2) . . ? O3 C6 H6A 110.8 . . ? C5 C6 H6A 110.8 . . ? O3 C6 H6B 110.8 . . ? C5 C6 H6B 110.8 . . ? H6A C6 H6B 108.9 . . ? N1 C7 C8 113.0(2) . . ? N1 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O1 C8 C7 110.1(2) . . ? O1 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? O1 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? N1 C9 C10 110.2(2) . . ? N1 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? N1 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? O2 C10 C9 107.9(2) . . ? O2 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O2 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N12 C11 C12 177.9(6) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 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 O3 H3O N6 0.85 1.79 2.636(3) 170.5 . _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.493 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.074 #===============================END data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 679171' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H48 Fe4 N16 O10' _chemical_formula_weight 920.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9710(10) _cell_length_b 10.8998(9) _cell_length_c 14.0946(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.7340(10) _cell_angle_gamma 90.00 _cell_volume 1786.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2416 _cell_measurement_theta_min 2.136 _cell_measurement_theta_max 24.428 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5590 _exptl_absorpt_correction_T_max 0.8524 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; Several restraints were employed to fix the geometry of the azide group. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11774 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3800 _reflns_number_gt 3251 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 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^)+(0.0571P)^2^+1.2030P] 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 3800 _refine_ls_number_parameters 236 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.40092(3) 0.38741(3) 0.01466(3) 0.03105(13) Uani 1 1 d . . . Fe2 Fe 0.48562(3) 0.60204(4) 0.17577(3) 0.03652(14) Uani 1 1 d . . . O1 O 0.34854(15) 0.52315(17) 0.08807(13) 0.0359(4) Uani 1 1 d . . . O2 O 0.43875(14) 0.51940(16) -0.09041(12) 0.0308(4) Uani 1 1 d . . . O3 O 0.48654(18) 0.29525(17) -0.06623(14) 0.0393(4) Uani 1 1 d . . . O4 O 0.43789(17) 0.29440(17) 0.14150(14) 0.0402(5) Uani 1 1 d . . . O5 O 0.48619(17) 0.4558(2) 0.26851(13) 0.0445(5) Uani 1 1 d . . . H5O H 0.4696 0.3954 0.2296 0.053 Uiso 1 1 d R . . N1 N 0.22297(19) 0.4326(2) -0.07853(16) 0.0384(5) Uani 1 1 d . . . N2 N 0.3014(2) 0.1945(2) -0.01617(18) 0.0477(6) Uani 1 1 d . . . N3 N 0.6289(2) 0.6679(3) 0.26954(19) 0.0519(7) Uani 1 1 d . . . N4 N 0.6502(3) 0.6492(3) 0.3549(2) 0.0572(7) Uani 1 1 d . . . N5 N 0.6727(4) 0.6339(4) 0.4376(3) 0.0992(14) Uani 1 1 d U . . N6 N 0.3818(2) 0.7156(3) 0.2270(2) 0.0589(8) Uani 1 1 d . . . N7 N 0.4039(2) 0.8131(3) 0.2648(2) 0.0537(7) Uani 1 1 d . . . N8 N 0.4214(3) 0.9073(4) 0.3005(3) 0.0865(12) Uani 1 1 d . . . C1 C 0.1596(3) 0.3221(3) -0.1248(2) 0.0537(8) Uani 1 1 d . . . H1A H 0.1857 0.3007 -0.1828 0.064 Uiso 1 1 calc R . . H1B H 0.0781 0.3407 -0.1448 0.064 Uiso 1 1 calc R . . C2 C 0.1775(3) 0.2146(3) -0.0561(3) 0.0586(9) Uani 1 1 d . . . H2A H 0.1403 0.2303 -0.0032 0.070 Uiso 1 1 calc R . . H2B H 0.1433 0.1418 -0.0906 0.070 Uiso 1 1 calc R . . C3 C 0.1616(2) 0.4863(3) -0.0077(2) 0.0478(7) Uani 1 1 d . . . H3A H 0.1382 0.4210 0.0302 0.057 Uiso 1 1 calc R . . H3B H 0.0929 0.5284 -0.0431 0.057 Uiso 1 1 calc R . . C4 C 0.2373(2) 0.5749(3) 0.0598(2) 0.0410(6) Uani 1 1 d . . . H4A H 0.2403 0.6525 0.0269 0.049 Uiso 1 1 calc R . . H4B H 0.2071 0.5895 0.1169 0.049 Uiso 1 1 calc R . . C5 C 0.2332(2) 0.5217(3) -0.1551(2) 0.0409(6) Uani 1 1 d . . . H5A H 0.1673 0.5762 -0.1671 0.049 Uiso 1 1 calc R . . H5B H 0.2318 0.4777 -0.2152 0.049 Uiso 1 1 calc R . . C6 C 0.3424(2) 0.5977(3) -0.1279(2) 0.0374(6) Uani 1 1 d . . . H6A H 0.3537 0.6410 -0.1850 0.045 Uiso 1 1 calc R . . H6B H 0.3356 0.6580 -0.0789 0.045 Uiso 1 1 calc R . . C7 C 0.3546(4) 0.1315(3) -0.0867(3) 0.0580(9) Uani 1 1 d . . . H7A H 0.3156 0.1550 -0.1527 0.070 Uiso 1 1 calc R . . H7B H 0.3471 0.0434 -0.0806 0.070 Uiso 1 1 calc R . . C8 C 0.4777(3) 0.1651(3) -0.0680(2) 0.0512(8) Uani 1 1 d . . . H8A H 0.5192 0.1314 -0.0060 0.061 Uiso 1 1 calc R . . H8B H 0.5109 0.1320 -0.1190 0.061 Uiso 1 1 calc R . . C9 C 0.3247(4) 0.1265(3) 0.0779(2) 0.0606(10) Uani 1 1 d . . . H9A H 0.2575 0.0793 0.0823 0.073 Uiso 1 1 calc R . . H9B H 0.3882 0.0701 0.0811 0.073 Uiso 1 1 calc R . . C10 C 0.3530(3) 0.2122(4) 0.1579(3) 0.0656(10) Uani 1 1 d . . . H10A H 0.2848 0.2573 0.1629 0.079 Uiso 1 1 calc R . . H10B H 0.3816 0.1683 0.2187 0.079 Uiso 1 1 calc R . . C11 C 0.4101(4) 0.4521(4) 0.3326(3) 0.0691(11) Uani 1 1 d . . . H11A H 0.4073 0.3701 0.3569 0.104 Uiso 1 1 calc R . . H11B H 0.3344 0.4766 0.2977 0.104 Uiso 1 1 calc R . . H11C H 0.4373 0.5070 0.3864 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0327(2) 0.0320(2) 0.0300(2) 0.00061(14) 0.01050(15) 0.00213(15) Fe2 0.0388(2) 0.0412(2) 0.0323(2) -0.00556(16) 0.01384(17) 0.00013(17) O1 0.0319(9) 0.0414(10) 0.0356(10) -0.0049(8) 0.0101(8) 0.0056(8) O2 0.0296(9) 0.0339(9) 0.0302(9) 0.0032(7) 0.0096(7) 0.0059(7) O3 0.0515(11) 0.0306(9) 0.0400(10) -0.0013(8) 0.0192(9) 0.0055(8) O4 0.0457(11) 0.0394(10) 0.0372(10) 0.0083(8) 0.0129(9) -0.0049(9) O5 0.0508(12) 0.0544(13) 0.0316(10) -0.0010(9) 0.0163(9) -0.0003(10) N1 0.0330(12) 0.0472(13) 0.0351(12) 0.0005(10) 0.0081(10) -0.0034(10) N2 0.0557(16) 0.0437(14) 0.0429(14) 0.0003(11) 0.0104(12) -0.0111(12) N3 0.0518(16) 0.0626(17) 0.0412(15) -0.0094(13) 0.0112(12) -0.0101(13) N4 0.074(2) 0.0465(15) 0.0456(18) -0.0104(13) 0.0037(14) -0.0052(14) N5 0.155(4) 0.079(2) 0.049(2) -0.0038(17) -0.006(2) -0.021(2) N6 0.0559(17) 0.0581(18) 0.0705(19) -0.0234(15) 0.0307(15) -0.0006(14) N7 0.0465(15) 0.0649(18) 0.0545(16) -0.0198(15) 0.0213(13) 0.0016(13) N8 0.078(2) 0.085(3) 0.104(3) -0.052(2) 0.035(2) -0.0087(19) C1 0.0472(18) 0.059(2) 0.0493(18) -0.0032(15) -0.0005(14) -0.0111(15) C2 0.056(2) 0.057(2) 0.061(2) -0.0015(17) 0.0107(16) -0.0217(17) C3 0.0314(14) 0.068(2) 0.0473(17) 0.0007(15) 0.0155(13) 0.0024(14) C4 0.0377(15) 0.0468(16) 0.0419(16) 0.0022(13) 0.0164(12) 0.0118(13) C5 0.0339(14) 0.0517(17) 0.0364(15) 0.0066(12) 0.0071(11) 0.0038(12) C6 0.0339(14) 0.0417(15) 0.0377(15) 0.0104(11) 0.0109(11) 0.0086(11) C7 0.085(3) 0.0367(16) 0.053(2) -0.0078(14) 0.0174(18) -0.0099(16) C8 0.070(2) 0.0325(15) 0.0559(19) 0.0000(13) 0.0247(17) 0.0074(15) C9 0.078(3) 0.0505(19) 0.054(2) 0.0096(16) 0.0157(18) -0.0176(18) C10 0.073(2) 0.069(2) 0.057(2) 0.0168(18) 0.0190(18) -0.0151(19) C11 0.079(3) 0.085(3) 0.053(2) 0.009(2) 0.0345(19) 0.005(2) _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 O3 1.9785(19) . ? Fe1 O1 1.9902(18) . ? Fe1 O4 2.0109(19) . ? Fe1 O2 2.1877(18) . ? Fe1 O2 2.2096(18) 3_665 ? Fe1 N1 2.275(2) . ? Fe1 N2 2.405(2) . ? Fe1 Fe2 3.2502(6) . ? Fe1 Fe2 3.2853(6) 3_665 ? Fe1 Fe1 3.5053(8) 3_665 ? Fe2 O3 1.9981(19) 3_665 ? Fe2 O1 1.9992(18) . ? Fe2 N6 2.006(3) . ? Fe2 N3 2.032(3) . ? Fe2 O5 2.060(2) . ? Fe2 O2 2.1300(17) 3_665 ? Fe2 Fe1 3.2853(6) 3_665 ? Fe2 Fe2 5.5160(8) 3_665 ? O1 C4 1.413(3) . ? O2 C6 1.431(3) . ? O2 Fe2 2.1300(17) 3_665 ? O2 Fe1 2.2096(18) 3_665 ? O3 C8 1.422(3) . ? O3 Fe2 1.9981(19) 3_665 ? O4 C10 1.415(4) . ? O5 C11 1.428(4) . ? O5 H5O 0.8500 . ? N1 C5 1.478(4) . ? N1 C1 1.489(4) . ? N1 C3 1.493(4) . ? N2 C2 1.472(4) . ? N2 C7 1.472(4) . ? N2 C9 1.486(4) . ? N3 N4 1.186(4) . ? N4 N5 1.146(4) . ? N6 N7 1.190(4) . ? N7 N8 1.141(4) . ? C1 C2 1.501(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.500(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.518(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.480(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.441(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 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 O3 Fe1 O1 161.32(8) . . ? O3 Fe1 O4 102.80(8) . . ? O1 Fe1 O4 86.71(8) . . ? O3 Fe1 O2 74.04(7) . . ? O1 Fe1 O2 90.25(7) . . ? O4 Fe1 O2 153.64(7) . . ? O3 Fe1 O2 90.14(8) . 3_665 ? O1 Fe1 O2 75.63(7) . 3_665 ? O4 Fe1 O2 79.61(7) . 3_665 ? O2 Fe1 O2 74.29(7) . 3_665 ? O3 Fe1 N1 108.62(9) . . ? O1 Fe1 N1 76.81(8) . . ? O4 Fe1 N1 126.91(8) . . ? O2 Fe1 N1 77.45(7) . . ? O2 Fe1 N1 140.01(8) 3_665 . ? O3 Fe1 N2 75.77(9) . . ? O1 Fe1 N2 122.69(9) . . ? O4 Fe1 N2 73.43(8) . . ? O2 Fe1 N2 128.75(8) . . ? O2 Fe1 N2 145.64(8) 3_665 . ? N1 Fe1 N2 74.29(9) . . ? O3 Fe1 Fe2 130.52(6) . . ? O1 Fe1 Fe2 35.53(5) . . ? O4 Fe1 Fe2 77.03(6) . . ? O2 Fe1 Fe2 85.37(5) . . ? O2 Fe1 Fe2 40.58(4) 3_665 . ? N1 Fe1 Fe2 109.97(6) . . ? N2 Fe1 Fe2 144.54(6) . . ? O3 Fe1 Fe2 34.49(6) . 3_665 ? O1 Fe1 Fe2 129.88(6) . 3_665 ? O4 Fe1 Fe2 134.23(6) . 3_665 ? O2 Fe1 Fe2 39.81(5) . 3_665 ? O2 Fe1 Fe2 84.17(5) 3_665 3_665 ? N1 Fe1 Fe2 91.88(6) . 3_665 ? N2 Fe1 Fe2 99.57(6) . 3_665 ? Fe2 Fe1 Fe2 115.132(14) . 3_665 ? O3 Fe1 Fe1 80.21(6) . 3_665 ? O1 Fe1 Fe1 81.16(6) . 3_665 ? O4 Fe1 Fe1 116.46(6) . 3_665 ? O2 Fe1 Fe1 37.36(5) . 3_665 ? O2 Fe1 Fe1 36.93(4) 3_665 3_665 ? N1 Fe1 Fe1 110.33(6) . 3_665 ? N2 Fe1 Fe1 155.64(7) . 3_665 ? Fe2 Fe1 Fe1 58.050(13) . 3_665 ? Fe2 Fe1 Fe1 57.082(12) 3_665 3_665 ? O3 Fe2 O1 91.51(8) 3_665 . ? O3 Fe2 N6 99.44(11) 3_665 . ? O1 Fe2 N6 90.00(10) . . ? O3 Fe2 N3 91.99(10) 3_665 . ? O1 Fe2 N3 175.17(10) . . ? N6 Fe2 N3 92.71(12) . . ? O3 Fe2 O5 161.38(8) 3_665 . ? O1 Fe2 O5 86.45(8) . . ? N6 Fe2 O5 99.07(11) . . ? N3 Fe2 O5 89.17(10) . . ? O3 Fe2 O2 74.96(7) 3_665 3_665 ? O1 Fe2 O2 77.30(7) . 3_665 ? N6 Fe2 O2 165.83(10) . 3_665 ? N3 Fe2 O2 100.41(9) . 3_665 ? O5 Fe2 O2 86.55(7) . 3_665 ? O3 Fe2 Fe1 86.85(6) 3_665 . ? O1 Fe2 Fe1 35.35(5) . . ? N6 Fe2 Fe1 125.33(9) . . ? N3 Fe2 Fe1 141.63(8) . . ? O5 Fe2 Fe1 80.79(6) . . ? O2 Fe2 Fe1 42.44(5) 3_665 . ? O3 Fe2 Fe1 34.10(5) 3_665 3_665 ? O1 Fe2 Fe1 87.01(5) . 3_665 ? N6 Fe2 Fe1 133.18(10) . 3_665 ? N3 Fe2 Fe1 94.03(8) . 3_665 ? O5 Fe2 Fe1 127.28(6) . 3_665 ? O2 Fe2 Fe1 41.12(5) 3_665 3_665 ? Fe1 Fe2 Fe1 64.868(14) . 3_665 ? O3 Fe2 Fe2 58.30(5) 3_665 3_665 ? O1 Fe2 Fe2 59.22(5) . 3_665 ? N6 Fe2 Fe2 138.45(9) . 3_665 ? N3 Fe2 Fe2 120.25(8) . 3_665 ? O5 Fe2 Fe2 105.45(6) . 3_665 ? O2 Fe2 Fe2 27.93(4) 3_665 3_665 ? Fe1 Fe2 Fe2 32.629(8) . 3_665 ? Fe1 Fe2 Fe2 32.239(8) 3_665 3_665 ? C4 O1 Fe1 122.82(17) . . ? C4 O1 Fe2 125.65(17) . . ? Fe1 O1 Fe2 109.12(8) . . ? C6 O2 Fe2 125.14(16) . 3_665 ? C6 O2 Fe1 111.32(15) . . ? Fe2 O2 Fe1 99.07(7) 3_665 . ? C6 O2 Fe1 115.84(16) . 3_665 ? Fe2 O2 Fe1 96.99(7) 3_665 3_665 ? Fe1 O2 Fe1 105.71(7) . 3_665 ? C8 O3 Fe1 118.04(18) . . ? C8 O3 Fe2 124.78(18) . 3_665 ? Fe1 O3 Fe2 111.41(9) . 3_665 ? C10 O4 Fe1 116.72(19) . . ? C11 O5 Fe2 121.1(2) . . ? C11 O5 H5O 107.5 . . ? Fe2 O5 H5O 103.0 . . ? C5 N1 C1 109.5(2) . . ? C5 N1 C3 111.7(2) . . ? C1 N1 C3 109.3(2) . . ? C5 N1 Fe1 109.57(16) . . ? C1 N1 Fe1 112.79(19) . . ? C3 N1 Fe1 103.92(16) . . ? C2 N2 C7 111.7(3) . . ? C2 N2 C9 112.0(3) . . ? C7 N2 C9 110.5(3) . . ? C2 N2 Fe1 110.45(19) . . ? C7 N2 Fe1 104.74(19) . . ? C9 N2 Fe1 107.12(18) . . ? N4 N3 Fe2 122.9(2) . . ? N5 N4 N3 178.1(4) . . ? N7 N6 Fe2 128.4(2) . . ? N8 N7 N6 177.7(4) . . ? N1 C1 C2 111.6(3) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 109.9(3) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N1 C3 C4 110.9(2) . . ? N1 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.0 . . ? O1 C4 C3 108.0(2) . . ? O1 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O1 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? N1 C5 C6 113.0(2) . . ? N1 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? N1 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? O2 C6 C5 109.8(2) . . ? O2 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? O2 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N2 C7 C8 109.7(3) . . ? N2 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N2 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O3 C8 C7 108.5(3) . . ? O3 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? O3 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C10 C9 N2 109.6(3) . . ? C10 C9 H9A 109.8 . . ? N2 C9 H9A 109.8 . . ? C10 C9 H9B 109.8 . . ? N2 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? O4 C10 C9 109.1(3) . . ? O4 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? O4 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O5 C11 H11A 109.5 . . ? O5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 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 H5O O4 0.85 1.64 2.479(3) 171.3 . _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.949 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.081 #_eof #End of Crystallographic Information File