# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_jph8 _database_code_depnum_ccdc_archive 'CCDC 893592' #TrackingRef 'web_deposit_cif_file_0_JonathanP.HIll_1343194096.1a_Hill.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C59 H64 Mn2 N2 O12 3-, C3 H18 O6 Mn 3+, 2(C H4 O), H2 O' _chemical_formula_sum 'C64 H92 Mn3 N2 O21' _chemical_formula_weight 1390.22 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.172(3) _cell_length_b 15.897(3) _cell_length_c 19.059(4) _cell_angle_alpha 70.363(4) _cell_angle_beta 83.939(4) _cell_angle_gamma 67.134(3) _cell_volume 3461.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 832 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 16.14 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1466 _exptl_absorpt_coefficient_mu 0.611 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.909 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details 'SADABS v2008/1, Sheldrick, G.M., (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX 2 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31865 _diffrn_reflns_av_R_equivalents 0.1734 _diffrn_reflns_av_sigmaI/netI 0.1950 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 23.37 _reflns_number_total 10045 _reflns_number_gt 4622 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0810P)^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, but OH coords other than H18 refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10045 _refine_ls_number_parameters 865 _refine_ls_number_restraints 197 _refine_ls_R_factor_all 0.1827 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.2054 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 0.74334(10) 0.38189(9) 0.30888(7) 0.0251(4) Uani 1 1 d D . . Mn2 Mn 0.65155(10) 0.58662(9) 0.30618(7) 0.0251(4) Uani 1 1 d D . . O1 O 0.6942(4) 0.5115(4) 0.2399(3) 0.0253(14) Uani 1 1 d . . . C1 C 0.6321(8) 0.5431(7) 0.1715(5) 0.045(3) Uani 1 1 d . . . H1A H 0.5555 0.5500 0.1830 0.068 Uiso 1 1 calc R . . H1B H 0.6646 0.4954 0.1455 0.068 Uiso 1 1 calc R . . H1C H 0.6339 0.6054 0.1397 0.068 Uiso 1 1 calc R . . O2 O 0.6984(4) 0.4569(4) 0.3773(3) 0.0272(14) Uani 1 1 d D . . H2 H 0.748(4) 0.446(2) 0.405(4) 0.033 Uiso 1 1 d D . . O3 O 0.7826(4) 0.3262(4) 0.2333(3) 0.0284(14) Uani 1 1 d . . . C2 C 0.8760(7) 0.2462(6) 0.2414(5) 0.031(2) Uani 1 1 d . . . C3 C 0.8909(7) 0.1660(6) 0.3041(5) 0.029(2) Uani 1 1 d . . . C4 C 0.9835(7) 0.0828(7) 0.3138(5) 0.039(2) Uani 1 1 d . . . H4 H 0.9917 0.0287 0.3572 0.046 Uiso 1 1 calc R . . C5 C 1.0657(7) 0.0769(7) 0.2603(6) 0.041(2) Uani 1 1 d U . . C6 C 1.0479(7) 0.1571(7) 0.1988(5) 0.038(2) Uani 1 1 d . . . H6 H 1.1016 0.1537 0.1613 0.046 Uiso 1 1 calc R . . C7 C 0.9571(7) 0.2429(7) 0.1872(5) 0.033(2) Uani 1 1 d . . . C8 C 0.7999(7) 0.1706(6) 0.3591(5) 0.030(2) Uani 1 1 d . . . H8A H 0.8179 0.1069 0.3981 0.036 Uiso 1 1 calc R . . H8B H 0.7305 0.1858 0.3332 0.036 Uiso 1 1 calc R . . N1 N 0.7832(5) 0.2458(5) 0.3952(4) 0.0247(17) Uani 1 1 d . . . C9 C 0.8843(6) 0.2222(6) 0.4372(4) 0.028(2) Uani 1 1 d . . . H9A H 0.9273 0.1519 0.4515 0.034 Uiso 1 1 calc R . . H9B H 0.8633 0.2392 0.4836 0.034 Uiso 1 1 calc R . . C10 C 0.9555(8) 0.2750(6) 0.3930(5) 0.030(2) Uani 1 1 d . . . O4 O 0.9128(4) 0.3467(4) 0.3362(3) 0.0310(15) Uani 1 1 d . . . O5 O 1.0511(5) 0.2458(4) 0.4174(4) 0.0445(17) Uani 1 1 d . . . C11 C 0.6859(6) 0.2523(6) 0.4424(4) 0.026(2) Uani 1 1 d . . . H11A H 0.6881 0.2831 0.4793 0.032 Uiso 1 1 calc R . . H11B H 0.6882 0.1865 0.4701 0.032 Uiso 1 1 calc R . . C12 C 0.5794(7) 0.3101(6) 0.3965(5) 0.027(2) Uani 1 1 d . . . O6 O 0.5870(4) 0.3608(4) 0.3291(3) 0.0258(14) Uani 1 1 d . . . O7 O 0.4920(5) 0.3056(4) 0.4266(3) 0.0380(16) Uani 1 1 d . . . C13 C 1.1654(9) -0.0162(8) 0.2645(7) 0.070(3) Uani 1 1 d U . . C14 C 1.2728(9) 0.0052(9) 0.2499(9) 0.119(5) Uani 1 1 d U . . H14D H 1.2876 0.0228 0.2912 0.179 Uiso 1 1 calc R . . H14E H 1.2637 0.0587 0.2033 0.179 Uiso 1 1 calc R . . H14F H 1.3346 -0.0523 0.2459 0.179 Uiso 1 1 calc R . . C15 C 1.1793(9) -0.0944(8) 0.3403(7) 0.084(4) Uani 1 1 d U . . H15C H 1.1867 -0.0697 0.3795 0.127 Uiso 1 1 calc R . . H15D H 1.2456 -0.1511 0.3408 0.127 Uiso 1 1 calc R . . H15E H 1.1147 -0.1123 0.3493 0.127 Uiso 1 1 calc R . . C16 C 1.1426(11) -0.0510(8) 0.2029(7) 0.089(4) Uani 1 1 d DU . . C17 C 1.1922(13) -0.0503(11) 0.1371(8) 0.169(6) Uani 1 1 d DU . . H17A H 1.2546 -0.0327 0.1276 0.203 Uiso 1 1 calc R . . C18 C 1.1566(14) -0.0744(13) 0.0811(9) 0.176(7) Uani 1 1 d DU . . H18 H 1.1965 -0.0736 0.0365 0.212 Uiso 1 1 calc R . . C19 C 1.0660(14) -0.0989(13) 0.0900(9) 0.155(6) Uani 1 1 d DU . . H19A H 1.0382 -0.1114 0.0521 0.186 Uiso 1 1 calc R . . C20 C 1.0201(14) -0.1037(12) 0.1563(8) 0.139(5) Uani 1 1 d DU . . H20 H 0.9626 -0.1278 0.1687 0.166 Uiso 1 1 calc R . . C21 C 1.0539(12) -0.0743(10) 0.2084(8) 0.113(5) Uani 1 1 d DU . . H21A H 1.0103 -0.0705 0.2511 0.135 Uiso 1 1 calc R . . C22 C 0.9396(7) 0.3291(7) 0.1158(5) 0.039(2) Uani 1 1 d . . . C23 C 1.0359(8) 0.3094(8) 0.0613(5) 0.056(3) Uani 1 1 d . . . H23A H 1.1054 0.2927 0.0867 0.083 Uiso 1 1 calc R . . H23B H 1.0231 0.3673 0.0177 0.083 Uiso 1 1 calc R . . H23C H 1.0399 0.2557 0.0453 0.083 Uiso 1 1 calc R . . C24 C 0.9350(7) 0.4170(6) 0.1346(5) 0.044(3) Uani 1 1 d . . . H24A H 0.8697 0.4377 0.1638 0.066 Uiso 1 1 calc R . . H24B H 0.9310 0.4697 0.0883 0.066 Uiso 1 1 calc R . . H24C H 1.0015 0.3998 0.1636 0.066 Uiso 1 1 calc R . . C25 C 0.8369(7) 0.3472(6) 0.0731(5) 0.037(2) Uani 1 1 d D . . C26 C 0.7636(8) 0.4367(7) 0.0380(5) 0.051(3) Uani 1 1 d D . . H26 H 0.7767 0.4909 0.0392 0.061 Uiso 1 1 calc R . . C27 C 0.6693(8) 0.4525(8) -0.0001(6) 0.063(3) Uani 1 1 d D . . H27 H 0.6172 0.5163 -0.0207 0.076 Uiso 1 1 calc R . . C28 C 0.6518(9) 0.3768(8) -0.0078(6) 0.058(3) Uani 1 1 d D . . H28 H 0.5897 0.3868 -0.0354 0.070 Uiso 1 1 calc R . . C29 C 0.7269(9) 0.2861(9) 0.0255(6) 0.065(3) Uani 1 1 d D . . H29 H 0.7172 0.2321 0.0207 0.078 Uiso 1 1 calc R . . C30 C 0.8173(8) 0.2715(7) 0.0663(5) 0.049(3) Uani 1 1 d D . . H30 H 0.8667 0.2075 0.0901 0.059 Uiso 1 1 calc R . . O8 O 0.6163(4) 0.7027(4) 0.2291(3) 0.0296(14) Uani 1 1 d . . . C31 C 0.6240(7) 0.7825(6) 0.2367(5) 0.033(2) Uani 1 1 d . . . C32 C 0.5770(7) 0.8114(6) 0.2984(5) 0.027(2) Uani 1 1 d . . . C33 C 0.5819(7) 0.8926(6) 0.3067(5) 0.035(2) Uani 1 1 d . . . H33 H 0.5499 0.9115 0.3487 0.042 Uiso 1 1 calc R . . C34 C 0.6325(7) 0.9468(6) 0.2547(5) 0.036(2) Uani 1 1 d . . . C35 C 0.6793(7) 0.9172(7) 0.1932(5) 0.040(2) Uani 1 1 d . . . H35 H 0.7140 0.9545 0.1571 0.049 Uiso 1 1 calc R . . C36 C 0.6770(7) 0.8354(6) 0.1828(5) 0.037(2) Uani 1 1 d . . . C37 C 0.5170(7) 0.7566(6) 0.3523(5) 0.033(2) Uani 1 1 d . . . H37A H 0.4546 0.7591 0.3259 0.040 Uiso 1 1 calc R . . H37B H 0.4864 0.7877 0.3910 0.040 Uiso 1 1 calc R . . N2 N 0.5893(5) 0.6530(5) 0.3892(3) 0.0232(16) Uani 1 1 d . . . C38 C 0.6770(6) 0.6438(6) 0.4360(4) 0.022(2) Uani 1 1 d . . . H38A H 0.6833 0.5918 0.4839 0.027 Uiso 1 1 calc R . . H38B H 0.6576 0.7048 0.4470 0.027 Uiso 1 1 calc R . . C39 C 0.7879(7) 0.6212(6) 0.3979(5) 0.031(2) Uani 1 1 d . . . O9 O 0.7960(4) 0.5997(4) 0.3392(3) 0.0270(14) Uani 1 1 d . . . O10 O 0.8666(5) 0.6212(5) 0.4300(3) 0.0433(17) Uani 1 1 d . . . C40 C 0.5162(7) 0.6044(6) 0.4339(4) 0.030(2) Uani 1 1 d . . . H40A H 0.4680 0.6433 0.4643 0.036 Uiso 1 1 calc R . . H40B H 0.5614 0.5404 0.4681 0.036 Uiso 1 1 calc R . . C41 C 0.4458(7) 0.5922(6) 0.3826(5) 0.027(2) Uani 1 1 d . . . O11 O 0.4826(4) 0.5899(4) 0.3198(3) 0.0282(14) Uani 1 1 d . . . O12 O 0.3564(5) 0.5839(4) 0.4075(3) 0.0371(16) Uani 1 1 d . . . C42 C 0.6275(8) 1.0429(6) 0.2642(5) 0.039(2) Uani 1 1 d . . . C43 C 0.7086(8) 1.0828(7) 0.2137(5) 0.052(3) Uani 1 1 d . . . H43A H 0.7018 1.1431 0.2207 0.078 Uiso 1 1 calc R . . H43B H 0.6914 1.0952 0.1615 0.078 Uiso 1 1 calc R . . H43C H 0.7841 1.0356 0.2267 0.078 Uiso 1 1 calc R . . C44 C 0.5121(8) 1.1153(7) 0.2430(6) 0.067(3) Uani 1 1 d . . . H44A H 0.4602 1.0920 0.2766 0.100 Uiso 1 1 calc R . . H44B H 0.4946 1.1243 0.1916 0.100 Uiso 1 1 calc R . . H44C H 0.5061 1.1769 0.2470 0.100 Uiso 1 1 calc R . . C45 C 0.6604(9) 1.0189(7) 0.3458(6) 0.046(2) Uani 1 1 d U . . C46 C 0.5937(11) 1.0636(9) 0.3941(7) 0.071(3) Uani 1 1 d U . . H46 H 0.5251 1.1148 0.3761 0.085 Uiso 1 1 calc R . . C47 C 0.6257(14) 1.0345(11) 0.4703(8) 0.100(4) Uani 1 1 d U . . H47 H 0.5793 1.0644 0.5038 0.120 Uiso 1 1 calc R . . C48 C 0.7304(17) 0.9584(13) 0.4943(9) 0.121(6) Uani 1 1 d U . . H48 H 0.7552 0.9366 0.5447 0.145 Uiso 1 1 calc R . . C49 C 0.7928(14) 0.9184(10) 0.4459(8) 0.103(5) Uani 1 1 d U . . H49 H 0.8625 0.8685 0.4632 0.124 Uiso 1 1 calc R . . C50 C 0.7636(10) 0.9441(8) 0.3731(7) 0.075(3) Uani 1 1 d U . . H50 H 0.8115 0.9125 0.3410 0.089 Uiso 1 1 calc R . . C51 C 0.7338(7) 0.8019(6) 0.1172(5) 0.035(2) Uani 1 1 d . . . C52 C 0.7801(9) 0.8730(7) 0.0626(6) 0.062(3) Uani 1 1 d . . . H52A H 0.7205 0.9364 0.0439 0.093 Uiso 1 1 calc R . . H52B H 0.8126 0.8497 0.0208 0.093 Uiso 1 1 calc R . . H52C H 0.8368 0.8786 0.0882 0.093 Uiso 1 1 calc R . . C53 C 0.8313(7) 0.7048(7) 0.1482(5) 0.051(3) Uani 1 1 d . . . H53A H 0.8788 0.7116 0.1805 0.076 Uiso 1 1 calc R . . H53B H 0.8739 0.6863 0.1068 0.076 Uiso 1 1 calc R . . H53C H 0.8030 0.6551 0.1770 0.076 Uiso 1 1 calc R . . C54 C 0.6534(8) 0.7944(7) 0.0690(5) 0.037(2) Uani 1 1 d . . . C55 C 0.6916(9) 0.7336(8) 0.0264(6) 0.056(3) Uani 1 1 d . . . H55 H 0.7675 0.6931 0.0303 0.067 Uiso 1 1 calc R . . C56 C 0.6234(10) 0.7299(9) -0.0215(6) 0.062(3) Uani 1 1 d . . . H56 H 0.6535 0.6880 -0.0505 0.074 Uiso 1 1 calc R . . C57 C 0.5147(11) 0.7844(10) -0.0282(6) 0.075(4) Uani 1 1 d . . . H57 H 0.4679 0.7827 -0.0619 0.090 Uiso 1 1 calc R . . C58 C 0.4743(10) 0.8429(10) 0.0161(7) 0.085(4) Uani 1 1 d . . . H58 H 0.3975 0.8800 0.0142 0.102 Uiso 1 1 calc R . . C59 C 0.5438(10) 0.8494(8) 0.0641(6) 0.074(4) Uani 1 1 d . . . H59 H 0.5142 0.8918 0.0927 0.089 Uiso 1 1 calc R . . Mn3 Mn 0.15131(11) 0.47086(10) 0.32876(7) 0.0316(4) Uani 1 1 d . . . O13 O -0.0076(4) 0.4901(4) 0.2887(3) 0.0334(15) Uani 1 1 d D . . H13A H -0.061(5) 0.530(4) 0.302(5) 0.050 Uiso 1 1 d D . . H13B H -0.015(6) 0.438(3) 0.303(5) 0.050 Uiso 1 1 d D . . O14 O 0.1330(7) 0.3707(6) 0.4302(4) 0.069(2) Uani 1 1 d D . . H14A H 0.105(9) 0.332(7) 0.429(5) 0.103 Uiso 1 1 d D . . H14B H 0.134(10) 0.369(8) 0.475(2) 0.103 Uiso 1 1 d D . . O15 O 0.3043(5) 0.4579(4) 0.3678(3) 0.0350(16) Uani 1 1 d D . . H15A H 0.364(5) 0.401(4) 0.385(5) 0.052 Uiso 1 1 d D . . H15B H 0.324(7) 0.505(5) 0.372(5) 0.052 Uiso 1 1 d D . . O16 O 0.2428(5) 0.3603(5) 0.2777(4) 0.063(2) Uani 1 1 d DU . . H16 H 0.308(4) 0.361(8) 0.259(5) 0.094 Uiso 1 1 d D . . C60 C 0.2297(13) 0.2695(11) 0.2832(9) 0.138(6) Uani 1 1 d U . . H60A H 0.2935 0.2140 0.3103 0.207 Uiso 1 1 calc R . . H60B H 0.2243 0.2671 0.2331 0.207 Uiso 1 1 calc R . . H60C H 0.1625 0.2674 0.3100 0.207 Uiso 1 1 calc R . . O17 O 0.1683(5) 0.5731(5) 0.2244(4) 0.0529(19) Uani 1 1 d D . . H17 H 0.232(6) 0.587(7) 0.219(5) 0.079 Uiso 1 1 d D . . C61 C 0.1387(9) 0.5781(9) 0.1535(6) 0.081(4) Uani 1 1 d . . . H61A H 0.2005 0.5336 0.1344 0.122 Uiso 1 1 calc R . . H61B H 0.1207 0.6440 0.1192 0.122 Uiso 1 1 calc R . . H61C H 0.0744 0.5603 0.1578 0.122 Uiso 1 1 calc R . . O18 O 0.0627(5) 0.5948(4) 0.3730(3) 0.0429(17) Uani 1 1 d . . . H18A H 0.0324 0.5823 0.4211 0.064 Uiso 1 1 calc R . . C62 C 0.0504(9) 0.6924(7) 0.3309(6) 0.062(3) Uani 1 1 d . . . H62A H 0.1234 0.6956 0.3195 0.093 Uiso 1 1 calc R . . H62B H 0.0106 0.7349 0.3603 0.093 Uiso 1 1 calc R . . H62C H 0.0089 0.7131 0.2844 0.093 Uiso 1 1 calc R . . O19 O 0.4459(6) 0.3590(7) 0.2375(4) 0.075(2) Uani 1 1 d D . . H19 H 0.482(9) 0.384(8) 0.261(6) 0.112 Uiso 1 1 d D . . O20 O 0.1784(6) 0.6006(5) 0.4968(4) 0.0501(18) Uani 1 1 d D . . H20A H 0.133(7) 0.579(7) 0.523(4) 0.075 Uiso 1 1 d D . . H20B H 0.182(8) 0.588(7) 0.457(3) 0.075 Uiso 1 1 d D . . C63 C 0.4988(10) 0.3718(8) 0.1685(6) 0.071(4) Uani 1 1 d . . . H63A H 0.4831 0.4406 0.1435 0.107 Uiso 1 1 calc R . . H63B H 0.4714 0.3470 0.1370 0.107 Uiso 1 1 calc R . . H63C H 0.5786 0.3367 0.1769 0.107 Uiso 1 1 calc R . . O21 O 0.3493(6) 0.6063(6) 0.2102(4) 0.070(2) Uani 1 1 d D . . H21 H 0.407(7) 0.577(8) 0.246(5) 0.105 Uiso 1 1 d D . . C64 C 0.3220(14) 0.7172(13) 0.1779(9) 0.153(7) Uani 1 1 d . . . H64A H 0.3006 0.7452 0.2184 0.229 Uiso 1 1 calc R . . H64B H 0.2612 0.7472 0.1410 0.229 Uiso 1 1 calc R . . H64C H 0.3872 0.7287 0.1540 0.229 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 0.0227(8) 0.0262(8) 0.0320(8) -0.0143(7) 0.0026(6) -0.0113(6) Mn2 0.0237(8) 0.0267(8) 0.0303(8) -0.0137(7) 0.0017(6) -0.0114(6) O1 0.028(3) 0.031(3) 0.026(3) -0.014(3) -0.001(3) -0.015(3) C1 0.048(6) 0.045(6) 0.051(7) -0.025(5) -0.006(5) -0.016(5) O2 0.032(4) 0.033(4) 0.023(4) -0.014(3) -0.002(3) -0.015(3) O3 0.030(4) 0.030(4) 0.030(4) -0.017(3) 0.001(3) -0.009(3) C2 0.031(6) 0.029(6) 0.040(6) -0.017(5) -0.002(5) -0.014(5) C3 0.041(6) 0.020(5) 0.031(6) -0.010(5) -0.002(5) -0.014(5) C4 0.037(6) 0.030(6) 0.050(7) -0.016(5) -0.007(5) -0.008(5) C5 0.025(5) 0.045(6) 0.063(7) -0.027(5) -0.002(5) -0.015(4) C6 0.040(6) 0.037(6) 0.045(6) -0.025(5) 0.004(5) -0.011(5) C7 0.037(6) 0.037(6) 0.038(6) -0.024(5) 0.004(5) -0.017(5) C8 0.039(6) 0.032(5) 0.030(5) -0.010(5) 0.001(4) -0.024(5) N1 0.020(4) 0.030(4) 0.030(4) -0.013(4) 0.004(3) -0.012(3) C9 0.031(5) 0.022(5) 0.028(5) -0.008(4) -0.005(4) -0.006(4) C10 0.030(6) 0.021(5) 0.044(6) -0.018(5) 0.005(5) -0.010(5) O4 0.022(3) 0.029(4) 0.045(4) -0.012(3) -0.004(3) -0.012(3) O5 0.029(4) 0.034(4) 0.070(5) -0.011(4) -0.012(3) -0.014(3) C11 0.025(5) 0.026(5) 0.028(5) -0.012(4) 0.004(4) -0.008(4) C12 0.020(5) 0.036(6) 0.035(6) -0.022(5) 0.005(4) -0.013(5) O6 0.022(3) 0.033(4) 0.029(4) -0.015(3) 0.003(3) -0.013(3) O7 0.022(4) 0.041(4) 0.051(4) -0.016(3) 0.007(3) -0.012(3) C13 0.050(6) 0.045(6) 0.098(8) -0.024(5) 0.017(6) -0.004(5) C14 0.033(6) 0.080(10) 0.204(16) -0.013(9) 0.003(8) -0.006(6) C15 0.050(7) 0.060(7) 0.102(8) -0.021(6) 0.003(7) 0.018(6) C16 0.120(10) 0.056(7) 0.104(8) -0.053(7) 0.062(7) -0.037(7) C17 0.216(15) 0.232(16) 0.173(13) -0.156(13) 0.101(11) -0.150(13) C18 0.189(16) 0.269(18) 0.201(14) -0.189(14) 0.096(12) -0.147(14) C19 0.194(16) 0.215(16) 0.127(12) -0.080(13) 0.069(11) -0.146(13) C20 0.198(15) 0.157(13) 0.118(12) -0.092(11) 0.047(10) -0.096(12) C21 0.117(11) 0.121(12) 0.125(11) -0.080(10) 0.018(9) -0.040(9) C22 0.031(6) 0.045(6) 0.047(6) -0.026(6) 0.013(5) -0.017(5) C23 0.048(7) 0.082(8) 0.049(7) -0.035(6) 0.026(5) -0.031(6) C24 0.040(6) 0.049(7) 0.044(6) -0.013(5) 0.011(5) -0.024(5) C25 0.040(6) 0.033(6) 0.032(6) -0.015(5) 0.007(5) -0.007(5) C26 0.056(7) 0.067(8) 0.053(7) -0.040(7) 0.012(6) -0.032(7) C27 0.049(7) 0.080(9) 0.053(8) -0.026(7) -0.001(6) -0.013(7) C28 0.057(8) 0.085(10) 0.042(7) -0.031(7) -0.002(6) -0.028(8) C29 0.067(8) 0.093(10) 0.058(8) -0.035(8) -0.005(7) -0.043(8) C30 0.065(8) 0.049(7) 0.045(7) -0.024(6) 0.006(6) -0.027(6) O8 0.031(3) 0.028(4) 0.035(4) -0.011(3) 0.004(3) -0.017(3) C31 0.037(6) 0.018(5) 0.042(6) -0.004(5) -0.010(5) -0.011(5) C32 0.029(5) 0.024(5) 0.035(6) -0.020(5) 0.003(4) -0.009(4) C33 0.041(6) 0.031(6) 0.036(6) -0.014(5) 0.007(5) -0.014(5) C34 0.037(6) 0.030(6) 0.044(6) -0.014(5) 0.000(5) -0.014(5) C35 0.033(6) 0.042(6) 0.050(7) -0.013(5) 0.009(5) -0.023(5) C36 0.047(6) 0.023(5) 0.048(6) -0.013(5) 0.001(5) -0.021(5) C37 0.030(5) 0.034(6) 0.044(6) -0.026(5) 0.011(5) -0.012(5) N2 0.022(4) 0.027(4) 0.024(4) -0.009(3) 0.000(3) -0.013(3) C38 0.016(5) 0.028(5) 0.028(5) -0.015(4) 0.007(4) -0.008(4) C39 0.035(6) 0.035(6) 0.033(6) -0.019(5) 0.009(5) -0.019(5) O9 0.024(3) 0.033(4) 0.034(4) -0.018(3) 0.005(3) -0.016(3) O10 0.028(4) 0.075(5) 0.048(4) -0.035(4) 0.000(3) -0.027(4) C40 0.028(5) 0.035(6) 0.030(5) -0.016(5) 0.002(4) -0.010(5) C41 0.028(6) 0.021(5) 0.033(6) -0.009(4) 0.001(5) -0.012(4) O11 0.027(3) 0.035(4) 0.035(4) -0.019(3) 0.006(3) -0.018(3) O12 0.027(4) 0.051(4) 0.049(4) -0.030(3) 0.014(3) -0.022(3) C42 0.047(6) 0.033(6) 0.051(7) -0.019(5) 0.008(5) -0.027(5) C43 0.076(8) 0.044(7) 0.057(7) -0.021(6) 0.001(6) -0.040(6) C44 0.063(8) 0.043(7) 0.102(10) -0.035(7) 0.000(7) -0.017(6) C45 0.075(7) 0.035(6) 0.044(6) -0.007(5) 0.001(5) -0.042(5) C46 0.106(9) 0.075(8) 0.073(7) -0.035(6) 0.027(6) -0.075(6) C47 0.193(13) 0.117(11) 0.073(8) -0.052(8) 0.040(8) -0.134(9) C48 0.229(17) 0.116(13) 0.060(9) 0.009(8) -0.029(9) -0.133(11) C49 0.166(12) 0.064(9) 0.094(10) 0.012(7) -0.061(9) -0.073(8) C50 0.094(8) 0.050(7) 0.091(8) -0.012(7) -0.042(7) -0.036(6) C51 0.034(6) 0.039(6) 0.038(6) -0.018(5) 0.015(5) -0.020(5) C52 0.087(9) 0.071(8) 0.059(7) -0.041(7) 0.035(6) -0.053(7) C53 0.033(6) 0.078(8) 0.046(7) -0.031(6) 0.012(5) -0.020(6) C54 0.039(6) 0.039(6) 0.027(6) -0.006(5) 0.001(5) -0.013(5) C55 0.054(7) 0.062(8) 0.052(7) -0.018(6) 0.007(6) -0.025(6) C56 0.064(9) 0.076(9) 0.057(8) -0.028(7) 0.000(6) -0.032(7) C57 0.083(10) 0.097(11) 0.058(8) -0.036(8) -0.011(7) -0.034(9) C58 0.056(8) 0.095(11) 0.093(11) -0.025(9) -0.029(8) -0.013(8) C59 0.075(9) 0.069(9) 0.081(9) -0.039(8) -0.016(7) -0.011(8) Mn3 0.0260(8) 0.0386(9) 0.0392(9) -0.0171(7) 0.0002(6) -0.0173(7) O13 0.022(4) 0.033(4) 0.049(4) -0.019(4) 0.004(3) -0.010(3) O14 0.109(7) 0.074(6) 0.049(5) -0.010(5) -0.017(5) -0.064(5) O15 0.024(4) 0.043(4) 0.048(4) -0.023(4) -0.003(3) -0.015(3) O16 0.040(4) 0.069(5) 0.097(6) -0.055(5) 0.014(4) -0.019(4) C60 0.128(14) 0.119(12) 0.205(18) -0.118(14) 0.039(12) -0.040(11) O17 0.044(4) 0.084(6) 0.040(4) -0.017(4) 0.002(4) -0.037(4) C61 0.058(8) 0.132(12) 0.057(8) -0.014(8) -0.010(6) -0.050(8) O18 0.044(4) 0.043(4) 0.052(4) -0.020(4) 0.007(3) -0.024(3) C62 0.057(8) 0.050(8) 0.080(9) -0.025(7) 0.013(6) -0.019(6) O19 0.050(5) 0.135(8) 0.071(6) -0.071(6) 0.013(4) -0.039(5) O20 0.052(5) 0.059(5) 0.044(5) -0.026(4) -0.004(4) -0.017(4) C63 0.117(11) 0.056(8) 0.043(7) -0.008(6) -0.011(7) -0.038(8) O21 0.065(6) 0.096(7) 0.055(5) 0.005(5) -0.013(4) -0.057(5) C64 0.146(17) 0.20(2) 0.131(16) -0.050(15) -0.002(12) -0.083(16) _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 O3 1.862(5) . ? Mn1 O1 1.927(5) . ? Mn1 O2 1.952(5) . ? Mn1 N1 2.137(7) . ? Mn1 O4 2.155(5) . ? Mn1 O6 2.187(5) . ? Mn1 Mn2 2.9832(18) . ? Mn2 O8 1.853(5) . ? Mn2 O1 1.919(5) . ? Mn2 O2 1.944(6) . ? Mn2 N2 2.113(6) . ? Mn2 O9 2.170(5) . ? Mn2 O11 2.195(5) . ? O1 C1 1.444(9) . ? O3 C2 1.359(9) . ? C2 C3 1.386(11) . ? C2 C7 1.405(11) . ? C3 C4 1.379(11) . ? C3 C8 1.504(11) . ? C4 C5 1.404(12) . ? C5 C6 1.371(12) . ? C5 C13 1.535(13) . ? C6 C7 1.387(11) . ? C7 C22 1.533(12) . ? C8 N1 1.505(9) . ? N1 C11 1.477(9) . ? N1 C9 1.481(9) . ? C9 C10 1.503(11) . ? C10 O5 1.243(10) . ? C10 O4 1.260(10) . ? C11 C12 1.515(11) . ? C12 O7 1.247(9) . ? C12 O6 1.284(9) . ? C13 C15 1.529(15) . ? C13 C16 1.554(16) . ? C13 C14 1.556(15) . ? C16 C21 1.340(12) . ? C16 C17 1.349(12) . ? C17 C18 1.424(13) . ? C18 C19 1.369(13) . ? C19 C20 1.334(13) . ? C20 C21 1.403(13) . ? C22 C25 1.532(12) . ? C22 C24 1.534(12) . ? C22 C23 1.554(11) . ? C25 C26 1.354(10) . ? C25 C30 1.373(10) . ? C26 C27 1.399(11) . ? C27 C28 1.366(11) . ? C28 C29 1.368(11) . ? C29 C30 1.391(11) . ? O8 C31 1.367(9) . ? C31 C32 1.403(11) . ? C31 C36 1.404(12) . ? C32 C33 1.378(11) . ? C32 C37 1.483(11) . ? C33 C34 1.378(11) . ? C34 C35 1.404(12) . ? C34 C42 1.572(11) . ? C35 C36 1.392(12) . ? C36 C51 1.531(12) . ? C37 N2 1.502(10) . ? N2 C38 1.467(9) . ? N2 C40 1.489(10) . ? C38 C39 1.528(10) . ? C39 O9 1.257(9) . ? C39 O10 1.259(9) . ? C40 C41 1.520(11) . ? C41 O11 1.250(9) . ? C41 O12 1.261(9) . ? C42 C44 1.503(13) . ? C42 C45 1.539(13) . ? C42 C43 1.540(12) . ? C45 C46 1.380(13) . ? C45 C50 1.417(14) . ? C46 C47 1.424(16) . ? C47 C48 1.43(2) . ? C48 C49 1.33(2) . ? C49 C50 1.361(16) . ? C51 C52 1.532(12) . ? C51 C54 1.536(12) . ? C51 C53 1.545(12) . ? C54 C59 1.359(13) . ? C54 C55 1.381(12) . ? C55 C56 1.378(13) . ? C56 C57 1.347(14) . ? C57 C58 1.382(15) . ? C58 C59 1.413(15) . ? Mn3 O14 2.113(7) . ? Mn3 O15 2.133(6) . ? Mn3 O17 2.159(7) . ? Mn3 O13 2.178(6) . ? Mn3 O16 2.178(7) . ? Mn3 O18 2.253(6) . ? O16 C60 1.488(15) . ? O17 C61 1.414(11) . ? O18 C62 1.439(11) . ? O19 C63 1.413(12) . ? O21 C64 1.561(18) . ? 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 Mn1 O1 93.3(2) . . ? O3 Mn1 O2 172.2(2) . . ? O1 Mn1 O2 79.0(2) . . ? O3 Mn1 N1 93.3(2) . . ? O1 Mn1 N1 172.6(2) . . ? O2 Mn1 N1 94.5(2) . . ? O3 Mn1 O4 92.5(2) . . ? O1 Mn1 O4 105.2(2) . . ? O2 Mn1 O4 88.7(2) . . ? N1 Mn1 O4 77.8(2) . . ? O3 Mn1 O6 94.2(2) . . ? O1 Mn1 O6 100.3(2) . . ? O2 Mn1 O6 88.1(2) . . ? N1 Mn1 O6 75.9(2) . . ? O4 Mn1 O6 153.1(2) . . ? O3 Mn1 Mn2 132.33(18) . . ? O1 Mn1 Mn2 39.04(15) . . ? O2 Mn1 Mn2 39.93(16) . . ? N1 Mn1 Mn2 134.35(18) . . ? O4 Mn1 Mn2 98.58(15) . . ? O6 Mn1 Mn2 95.97(14) . . ? O8 Mn2 O1 93.4(2) . . ? O8 Mn2 O2 172.5(2) . . ? O1 Mn2 O2 79.4(2) . . ? O8 Mn2 N2 93.9(2) . . ? O1 Mn2 N2 169.7(2) . . ? O2 Mn2 N2 93.6(2) . . ? O8 Mn2 O9 91.9(2) . . ? O1 Mn2 O9 109.2(2) . . ? O2 Mn2 O9 88.7(2) . . ? N2 Mn2 O9 77.8(2) . . ? O8 Mn2 O11 95.5(2) . . ? O1 Mn2 O11 95.6(2) . . ? O2 Mn2 O11 87.2(2) . . ? N2 Mn2 O11 76.5(2) . . ? O9 Mn2 O11 153.6(2) . . ? O8 Mn2 Mn1 132.55(17) . . ? O1 Mn2 Mn1 39.23(16) . . ? O2 Mn2 Mn1 40.13(15) . . ? N2 Mn2 Mn1 133.34(18) . . ? O9 Mn2 Mn1 101.12(15) . . ? O11 Mn2 Mn1 92.38(14) . . ? C1 O1 Mn2 120.8(5) . . ? C1 O1 Mn1 124.5(5) . . ? Mn2 O1 Mn1 101.7(2) . . ? Mn2 O2 Mn1 99.9(2) . . ? C2 O3 Mn1 119.6(5) . . ? O3 C2 C3 119.3(8) . . ? O3 C2 C7 121.2(8) . . ? C3 C2 C7 119.4(8) . . ? C4 C3 C2 121.2(8) . . ? C4 C3 C8 120.9(8) . . ? C2 C3 C8 117.8(8) . . ? C3 C4 C5 120.8(9) . . ? C6 C5 C4 116.5(9) . . ? C6 C5 C13 120.0(9) . . ? C4 C5 C13 123.3(10) . . ? C5 C6 C7 124.8(9) . . ? C6 C7 C2 117.3(9) . . ? C6 C7 C22 122.3(8) . . ? C2 C7 C22 120.2(8) . . ? C3 C8 N1 111.7(6) . . ? C11 N1 C9 112.9(6) . . ? C11 N1 C8 108.2(6) . . ? C9 N1 C8 110.4(6) . . ? C11 N1 Mn1 106.8(5) . . ? C9 N1 Mn1 110.7(5) . . ? C8 N1 Mn1 107.8(5) . . ? N1 C9 C10 112.4(7) . . ? O5 C10 O4 125.3(8) . . ? O5 C10 C9 116.6(8) . . ? O4 C10 C9 118.0(8) . . ? C10 O4 Mn1 116.9(5) . . ? N1 C11 C12 111.6(7) . . ? O7 C12 O6 125.3(8) . . ? O7 C12 C11 118.2(8) . . ? O6 C12 C11 116.5(7) . . ? C12 O6 Mn1 113.0(5) . . ? C15 C13 C5 112.7(9) . . ? C15 C13 C16 109.9(10) . . ? C5 C13 C16 105.2(9) . . ? C15 C13 C14 107.9(10) . . ? C5 C13 C14 109.9(9) . . ? C16 C13 C14 111.4(11) . . ? C21 C16 C17 112.1(14) . . ? C21 C16 C13 118.5(11) . . ? C17 C16 C13 128.8(12) . . ? C16 C17 C18 124.0(14) . . ? C19 C18 C17 121.5(14) . . ? C20 C19 C18 114.4(15) . . ? C19 C20 C21 122.1(14) . . ? C16 C21 C20 125.4(13) . . ? C25 C22 C7 109.3(7) . . ? C25 C22 C24 113.7(8) . . ? C7 C22 C24 110.1(7) . . ? C25 C22 C23 105.4(7) . . ? C7 C22 C23 112.3(8) . . ? C24 C22 C23 106.1(7) . . ? C26 C25 C30 116.4(9) . . ? C26 C25 C22 123.0(8) . . ? C30 C25 C22 120.6(8) . . ? C25 C26 C27 122.6(9) . . ? C28 C27 C26 120.4(10) . . ? C27 C28 C29 117.5(10) . . ? C28 C29 C30 121.2(10) . . ? C25 C30 C29 121.7(9) . . ? C31 O8 Mn2 122.6(5) . . ? O8 C31 C32 119.1(8) . . ? O8 C31 C36 120.3(8) . . ? C32 C31 C36 120.6(8) . . ? C33 C32 C31 120.2(8) . . ? C33 C32 C37 120.6(8) . . ? C31 C32 C37 119.2(7) . . ? C32 C33 C34 121.0(8) . . ? C33 C34 C35 118.4(8) . . ? C33 C34 C42 118.4(8) . . ? C35 C34 C42 123.1(8) . . ? C36 C35 C34 122.6(9) . . ? C35 C36 C31 117.2(8) . . ? C35 C36 C51 121.5(8) . . ? C31 C36 C51 121.3(7) . . ? C32 C37 N2 112.7(6) . . ? C38 N2 C40 111.3(6) . . ? C38 N2 C37 111.9(6) . . ? C40 N2 C37 106.8(6) . . ? C38 N2 Mn2 112.5(5) . . ? C40 N2 Mn2 105.3(5) . . ? C37 N2 Mn2 108.7(5) . . ? N2 C38 C39 111.5(6) . . ? O9 C39 O10 124.6(8) . . ? O9 C39 C38 118.7(8) . . ? O10 C39 C38 116.7(7) . . ? C39 O9 Mn2 115.7(5) . . ? N2 C40 C41 110.1(7) . . ? O11 C41 O12 125.9(8) . . ? O11 C41 C40 116.9(7) . . ? O12 C41 C40 117.2(8) . . ? C41 O11 Mn2 113.2(5) . . ? C44 C42 C45 113.5(8) . . ? C44 C42 C43 108.9(8) . . ? C45 C42 C43 108.3(7) . . ? C44 C42 C34 107.0(8) . . ? C45 C42 C34 107.0(7) . . ? C43 C42 C34 112.2(7) . . ? C46 C45 C50 118.7(11) . . ? C46 C45 C42 123.8(10) . . ? C50 C45 C42 117.5(10) . . ? C45 C46 C47 121.3(13) . . ? C46 C47 C48 117.2(15) . . ? C49 C48 C47 119.6(16) . . ? C48 C49 C50 124.3(17) . . ? C49 C50 C45 118.8(14) . . ? C36 C51 C52 112.8(7) . . ? C36 C51 C54 112.1(7) . . ? C52 C51 C54 104.0(7) . . ? C36 C51 C53 108.5(7) . . ? C52 C51 C53 107.6(8) . . ? C54 C51 C53 111.8(7) . . ? C59 C54 C55 117.7(10) . . ? C59 C54 C51 121.8(9) . . ? C55 C54 C51 120.4(9) . . ? C56 C55 C54 122.2(10) . . ? C57 C56 C55 121.4(11) . . ? C56 C57 C58 117.1(11) . . ? C57 C58 C59 122.0(12) . . ? C54 C59 C58 119.5(11) . . ? O14 Mn3 O15 91.1(3) . . ? O14 Mn3 O17 179.3(3) . . ? O15 Mn3 O17 89.6(2) . . ? O14 Mn3 O13 89.9(3) . . ? O15 Mn3 O13 177.7(2) . . ? O17 Mn3 O13 89.4(2) . . ? O14 Mn3 O16 93.8(3) . . ? O15 Mn3 O16 88.6(2) . . ? O17 Mn3 O16 86.1(3) . . ? O13 Mn3 O16 93.4(2) . . ? O14 Mn3 O18 91.4(3) . . ? O15 Mn3 O18 89.7(2) . . ? O17 Mn3 O18 88.7(3) . . ? O13 Mn3 O18 88.2(2) . . ? O16 Mn3 O18 174.5(3) . . ? C60 O16 Mn3 130.6(7) . . ? C61 O17 Mn3 125.0(6) . . ? C62 O18 Mn3 122.4(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mn1 Mn2 O8 -1.5(3) . . . . ? O1 Mn1 Mn2 O8 -3.7(3) . . . . ? O2 Mn1 Mn2 O8 177.5(3) . . . . ? N1 Mn1 Mn2 O8 -178.8(3) . . . . ? O4 Mn1 Mn2 O8 99.9(3) . . . . ? O6 Mn1 Mn2 O8 -102.7(3) . . . . ? O3 Mn1 Mn2 O1 2.3(3) . . . . ? O2 Mn1 Mn2 O1 -178.8(4) . . . . ? N1 Mn1 Mn2 O1 -175.1(3) . . . . ? O4 Mn1 Mn2 O1 103.7(3) . . . . ? O6 Mn1 Mn2 O1 -99.0(3) . . . . ? O3 Mn1 Mn2 O2 -179.0(3) . . . . ? O1 Mn1 Mn2 O2 178.8(4) . . . . ? N1 Mn1 Mn2 O2 3.7(3) . . . . ? O4 Mn1 Mn2 O2 -77.6(3) . . . . ? O6 Mn1 Mn2 O2 79.8(3) . . . . ? O3 Mn1 Mn2 N2 171.7(3) . . . . ? O1 Mn1 Mn2 N2 169.5(3) . . . . ? O2 Mn1 Mn2 N2 -9.3(3) . . . . ? N1 Mn1 Mn2 N2 -5.6(3) . . . . ? O4 Mn1 Mn2 N2 -86.9(3) . . . . ? O6 Mn1 Mn2 N2 70.5(3) . . . . ? O3 Mn1 Mn2 O9 -104.6(3) . . . . ? O1 Mn1 Mn2 O9 -106.9(3) . . . . ? O2 Mn1 Mn2 O9 74.4(3) . . . . ? N1 Mn1 Mn2 O9 78.1(3) . . . . ? O4 Mn1 Mn2 O9 -3.2(2) . . . . ? O6 Mn1 Mn2 O9 154.2(2) . . . . ? O3 Mn1 Mn2 O11 98.2(3) . . . . ? O1 Mn1 Mn2 O11 95.9(3) . . . . ? O2 Mn1 Mn2 O11 -82.8(3) . . . . ? N1 Mn1 Mn2 O11 -79.2(3) . . . . ? O4 Mn1 Mn2 O11 -160.4(2) . . . . ? O6 Mn1 Mn2 O11 -3.1(2) . . . . ? O8 Mn2 O1 C1 -39.9(6) . . . . ? O2 Mn2 O1 C1 142.0(6) . . . . ? N2 Mn2 O1 C1 94.8(14) . . . . ? O9 Mn2 O1 C1 -133.2(6) . . . . ? O11 Mn2 O1 C1 55.9(6) . . . . ? Mn1 Mn2 O1 C1 142.8(7) . . . . ? O8 Mn2 O1 Mn1 177.2(2) . . . . ? O2 Mn2 O1 Mn1 -0.8(2) . . . . ? N2 Mn2 O1 Mn1 -48.0(14) . . . . ? O9 Mn2 O1 Mn1 84.0(3) . . . . ? O11 Mn2 O1 Mn1 -86.9(2) . . . . ? O3 Mn1 O1 C1 40.7(6) . . . . ? O2 Mn1 O1 C1 -140.1(6) . . . . ? N1 Mn1 O1 C1 -112.4(18) . . . . ? O4 Mn1 O1 C1 134.3(6) . . . . ? O6 Mn1 O1 C1 -54.1(6) . . . . ? Mn2 Mn1 O1 C1 -140.9(7) . . . . ? O3 Mn1 O1 Mn2 -178.3(2) . . . . ? O2 Mn1 O1 Mn2 0.8(2) . . . . ? N1 Mn1 O1 Mn2 28.5(19) . . . . ? O4 Mn1 O1 Mn2 -84.8(2) . . . . ? O6 Mn1 O1 Mn2 86.8(2) . . . . ? O8 Mn2 O2 Mn1 -14.2(19) . . . . ? O1 Mn2 O2 Mn1 0.8(2) . . . . ? N2 Mn2 O2 Mn1 173.2(2) . . . . ? O9 Mn2 O2 Mn1 -109.1(2) . . . . ? O11 Mn2 O2 Mn1 97.0(2) . . . . ? O3 Mn1 O2 Mn2 5.6(19) . . . . ? O1 Mn1 O2 Mn2 -0.8(2) . . . . ? N1 Mn1 O2 Mn2 -177.4(2) . . . . ? O4 Mn1 O2 Mn2 105.0(3) . . . . ? O6 Mn1 O2 Mn2 -101.7(2) . . . . ? O1 Mn1 O3 C2 140.4(6) . . . . ? O2 Mn1 O3 C2 134.1(16) . . . . ? N1 Mn1 O3 C2 -42.9(6) . . . . ? O4 Mn1 O3 C2 35.0(6) . . . . ? O6 Mn1 O3 C2 -119.0(6) . . . . ? Mn2 Mn1 O3 C2 139.0(5) . . . . ? Mn1 O3 C2 C3 54.3(9) . . . . ? Mn1 O3 C2 C7 -126.3(7) . . . . ? O3 C2 C3 C4 178.7(7) . . . . ? C7 C2 C3 C4 -0.6(12) . . . . ? O3 C2 C3 C8 2.2(11) . . . . ? C7 C2 C3 C8 -177.2(7) . . . . ? C2 C3 C4 C5 0.1(13) . . . . ? C8 C3 C4 C5 176.6(8) . . . . ? C3 C4 C5 C6 -0.7(13) . . . . ? C3 C4 C5 C13 -174.5(9) . . . . ? C4 C5 C6 C7 1.9(13) . . . . ? C13 C5 C6 C7 175.9(9) . . . . ? C5 C6 C7 C2 -2.4(13) . . . . ? C5 C6 C7 C22 -177.7(8) . . . . ? O3 C2 C7 C6 -177.7(7) . . . . ? C3 C2 C7 C6 1.6(12) . . . . ? O3 C2 C7 C22 -2.3(12) . . . . ? C3 C2 C7 C22 177.1(7) . . . . ? C4 C3 C8 N1 118.8(8) . . . . ? C2 C3 C8 N1 -64.7(9) . . . . ? C3 C8 N1 C11 174.5(7) . . . . ? C3 C8 N1 C9 -61.5(8) . . . . ? C3 C8 N1 Mn1 59.4(7) . . . . ? O3 Mn1 N1 C11 -128.0(5) . . . . ? O1 Mn1 N1 C11 25(2) . . . . ? O2 Mn1 N1 C11 52.4(5) . . . . ? O4 Mn1 N1 C11 140.1(5) . . . . ? O6 Mn1 N1 C11 -34.5(5) . . . . ? Mn2 Mn1 N1 C11 50.0(5) . . . . ? O3 Mn1 N1 C9 108.8(5) . . . . ? O1 Mn1 N1 C9 -98.1(18) . . . . ? O2 Mn1 N1 C9 -70.8(5) . . . . ? O4 Mn1 N1 C9 16.9(5) . . . . ? O6 Mn1 N1 C9 -157.7(5) . . . . ? Mn2 Mn1 N1 C9 -73.2(5) . . . . ? O3 Mn1 N1 C8 -12.0(5) . . . . ? O1 Mn1 N1 C8 141.2(17) . . . . ? O2 Mn1 N1 C8 168.4(5) . . . . ? O4 Mn1 N1 C8 -103.8(5) . . . . ? O6 Mn1 N1 C8 81.5(5) . . . . ? Mn2 Mn1 N1 C8 166.1(4) . . . . ? C11 N1 C9 C10 -142.4(7) . . . . ? C8 N1 C9 C10 96.5(7) . . . . ? Mn1 N1 C9 C10 -22.7(8) . . . . ? N1 C9 C10 O5 -166.1(7) . . . . ? N1 C9 C10 O4 16.5(10) . . . . ? O5 C10 O4 Mn1 -178.6(7) . . . . ? C9 C10 O4 Mn1 -1.4(9) . . . . ? O3 Mn1 O4 C10 -101.9(6) . . . . ? O1 Mn1 O4 C10 164.0(5) . . . . ? O2 Mn1 O4 C10 85.8(6) . . . . ? N1 Mn1 O4 C10 -9.0(6) . . . . ? O6 Mn1 O4 C10 2.6(8) . . . . ? Mn2 Mn1 O4 C10 124.6(5) . . . . ? C9 N1 C11 C12 159.2(6) . . . . ? C8 N1 C11 C12 -78.4(8) . . . . ? Mn1 N1 C11 C12 37.4(7) . . . . ? N1 C11 C12 O7 166.0(7) . . . . ? N1 C11 C12 O6 -14.4(10) . . . . ? O7 C12 O6 Mn1 163.1(7) . . . . ? C11 C12 O6 Mn1 -16.4(8) . . . . ? O3 Mn1 O6 C12 121.7(5) . . . . ? O1 Mn1 O6 C12 -144.1(5) . . . . ? O2 Mn1 O6 C12 -65.7(5) . . . . ? N1 Mn1 O6 C12 29.4(5) . . . . ? O4 Mn1 O6 C12 17.7(8) . . . . ? Mn2 Mn1 O6 C12 -104.9(5) . . . . ? C6 C5 C13 C15 173.6(9) . . . . ? C4 C5 C13 C15 -12.8(15) . . . . ? C6 C5 C13 C16 -66.7(12) . . . . ? C4 C5 C13 C16 106.9(11) . . . . ? C6 C5 C13 C14 53.3(14) . . . . ? C4 C5 C13 C14 -133.1(11) . . . . ? C15 C13 C16 C21 59.2(15) . . . . ? C5 C13 C16 C21 -62.3(14) . . . . ? C14 C13 C16 C21 178.7(12) . . . . ? C15 C13 C16 C17 -130.2(13) . . . . ? C5 C13 C16 C17 108.3(14) . . . . ? C14 C13 C16 C17 -10.7(17) . . . . ? C21 C16 C17 C18 -1.9(15) . . . . ? C13 C16 C17 C18 -172.9(14) . . . . ? C16 C17 C18 C19 1.2(18) . . . . ? C17 C18 C19 C20 -4(3) . . . . ? C18 C19 C20 C21 8(3) . . . . ? C17 C16 C21 C20 6(2) . . . . ? C13 C16 C21 C20 177.8(14) . . . . ? C19 C20 C21 C16 -9(3) . . . . ? C6 C7 C22 C25 114.5(9) . . . . ? C2 C7 C22 C25 -60.6(10) . . . . ? C6 C7 C22 C24 -120.0(9) . . . . ? C2 C7 C22 C24 64.9(10) . . . . ? C6 C7 C22 C23 -2.0(12) . . . . ? C2 C7 C22 C23 -177.2(8) . . . . ? C7 C22 C25 C26 140.3(9) . . . . ? C24 C22 C25 C26 16.9(12) . . . . ? C23 C22 C25 C26 -98.9(10) . . . . ? C7 C22 C25 C30 -42.4(11) . . . . ? C24 C22 C25 C30 -165.8(8) . . . . ? C23 C22 C25 C30 78.5(10) . . . . ? C30 C25 C26 C27 3.3(14) . . . . ? C22 C25 C26 C27 -179.2(9) . . . . ? C25 C26 C27 C28 -4.8(16) . . . . ? C26 C27 C28 C29 2.7(16) . . . . ? C27 C28 C29 C30 0.6(16) . . . . ? C26 C25 C30 C29 0.0(14) . . . . ? C22 C25 C30 C29 -177.5(9) . . . . ? C28 C29 C30 C25 -2.0(16) . . . . ? O1 Mn2 O8 C31 -151.1(6) . . . . ? O2 Mn2 O8 C31 -136.4(17) . . . . ? N2 Mn2 O8 C31 36.2(6) . . . . ? O9 Mn2 O8 C31 -41.7(6) . . . . ? O11 Mn2 O8 C31 112.9(6) . . . . ? Mn1 Mn2 O8 C31 -148.8(5) . . . . ? Mn2 O8 C31 C32 -48.8(10) . . . . ? Mn2 O8 C31 C36 132.0(7) . . . . ? O8 C31 C32 C33 -178.8(8) . . . . ? C36 C31 C32 C33 0.4(13) . . . . ? O8 C31 C32 C37 -2.1(12) . . . . ? C36 C31 C32 C37 177.1(8) . . . . ? C31 C32 C33 C34 0.1(13) . . . . ? C37 C32 C33 C34 -176.6(8) . . . . ? C32 C33 C34 C35 -0.2(13) . . . . ? C32 C33 C34 C42 175.5(8) . . . . ? C33 C34 C35 C36 -0.3(14) . . . . ? C42 C34 C35 C36 -175.7(8) . . . . ? C34 C35 C36 C31 0.7(14) . . . . ? C34 C35 C36 C51 -176.9(8) . . . . ? O8 C31 C36 C35 178.4(8) . . . . ? C32 C31 C36 C35 -0.7(13) . . . . ? O8 C31 C36 C51 -4.0(13) . . . . ? C32 C31 C36 C51 176.8(8) . . . . ? C33 C32 C37 N2 -122.1(8) . . . . ? C31 C32 C37 N2 61.2(10) . . . . ? C32 C37 N2 C38 64.9(8) . . . . ? C32 C37 N2 C40 -173.0(6) . . . . ? C32 C37 N2 Mn2 -59.9(7) . . . . ? O8 Mn2 N2 C38 -108.4(5) . . . . ? O1 Mn2 N2 C38 116.9(13) . . . . ? O2 Mn2 N2 C38 70.7(5) . . . . ? O9 Mn2 N2 C38 -17.2(5) . . . . ? O11 Mn2 N2 C38 156.9(5) . . . . ? Mn1 Mn2 N2 C38 76.7(5) . . . . ? O8 Mn2 N2 C40 130.2(5) . . . . ? O1 Mn2 N2 C40 -4.5(16) . . . . ? O2 Mn2 N2 C40 -50.7(5) . . . . ? O9 Mn2 N2 C40 -138.6(5) . . . . ? O11 Mn2 N2 C40 35.5(5) . . . . ? Mn1 Mn2 N2 C40 -44.8(5) . . . . ? O8 Mn2 N2 C37 16.1(5) . . . . ? O1 Mn2 N2 C37 -118.6(13) . . . . ? O2 Mn2 N2 C37 -164.8(5) . . . . ? O9 Mn2 N2 C37 107.3(5) . . . . ? O11 Mn2 N2 C37 -78.6(5) . . . . ? Mn1 Mn2 N2 C37 -158.8(4) . . . . ? C40 N2 C38 C39 137.7(7) . . . . ? C37 N2 C38 C39 -102.9(7) . . . . ? Mn2 N2 C38 C39 19.8(8) . . . . ? N2 C38 C39 O9 -9.9(11) . . . . ? N2 C38 C39 O10 173.2(7) . . . . ? O10 C39 O9 Mn2 171.6(7) . . . . ? C38 C39 O9 Mn2 -5.0(10) . . . . ? O8 Mn2 O9 C39 106.1(6) . . . . ? O1 Mn2 O9 C39 -159.6(6) . . . . ? O2 Mn2 O9 C39 -81.4(6) . . . . ? N2 Mn2 O9 C39 12.5(6) . . . . ? O11 Mn2 O9 C39 -0.3(8) . . . . ? Mn1 Mn2 O9 C39 -119.8(6) . . . . ? C38 N2 C40 C41 -165.4(6) . . . . ? C37 N2 C40 C41 72.2(8) . . . . ? Mn2 N2 C40 C41 -43.3(7) . . . . ? N2 C40 C41 O11 24.8(10) . . . . ? N2 C40 C41 O12 -156.2(7) . . . . ? O12 C41 O11 Mn2 -171.8(7) . . . . ? C40 C41 O11 Mn2 7.1(9) . . . . ? O8 Mn2 O11 C41 -118.0(5) . . . . ? O1 Mn2 O11 C41 148.1(5) . . . . ? O2 Mn2 O11 C41 69.1(5) . . . . ? N2 Mn2 O11 C41 -25.3(5) . . . . ? O9 Mn2 O11 C41 -12.3(8) . . . . ? Mn1 Mn2 O11 C41 108.9(5) . . . . ? C33 C34 C42 C44 -73.7(11) . . . . ? C35 C34 C42 C44 101.7(10) . . . . ? C33 C34 C42 C45 48.3(11) . . . . ? C35 C34 C42 C45 -136.3(9) . . . . ? C33 C34 C42 C43 166.9(8) . . . . ? C35 C34 C42 C43 -17.7(12) . . . . ? C44 C42 C45 C46 -4.0(12) . . . . ? C43 C42 C45 C46 117.1(10) . . . . ? C34 C42 C45 C46 -121.8(9) . . . . ? C44 C42 C45 C50 173.8(9) . . . . ? C43 C42 C45 C50 -65.2(10) . . . . ? C34 C42 C45 C50 55.9(11) . . . . ? C50 C45 C46 C47 -1.5(14) . . . . ? C42 C45 C46 C47 176.2(9) . . . . ? C45 C46 C47 C48 1.1(16) . . . . ? C46 C47 C48 C49 0(2) . . . . ? C47 C48 C49 C50 -1(2) . . . . ? C48 C49 C50 C45 0(2) . . . . ? C46 C45 C50 C49 0.7(15) . . . . ? C42 C45 C50 C49 -177.2(9) . . . . ? C35 C36 C51 C52 -6.1(13) . . . . ? C31 C36 C51 C52 176.5(9) . . . . ? C35 C36 C51 C54 -123.0(9) . . . . ? C31 C36 C51 C54 59.5(11) . . . . ? C35 C36 C51 C53 113.0(9) . . . . ? C31 C36 C51 C53 -64.4(11) . . . . ? C36 C51 C54 C59 27.3(13) . . . . ? C52 C51 C54 C59 -94.9(11) . . . . ? C53 C51 C54 C59 149.3(10) . . . . ? C36 C51 C54 C55 -155.4(8) . . . . ? C52 C51 C54 C55 82.4(10) . . . . ? C53 C51 C54 C55 -33.4(11) . . . . ? C59 C54 C55 C56 2.1(15) . . . . ? C51 C54 C55 C56 -175.3(9) . . . . ? C54 C55 C56 C57 -1.3(17) . . . . ? C55 C56 C57 C58 -1.1(18) . . . . ? C56 C57 C58 C59 2.8(19) . . . . ? C55 C54 C59 C58 -0.4(16) . . . . ? C51 C54 C59 C58 177.0(10) . . . . ? C57 C58 C59 C54 -2.1(19) . . . . ? O14 Mn3 O16 C60 37.5(11) . . . . ? O15 Mn3 O16 C60 128.5(11) . . . . ? O17 Mn3 O16 C60 -141.8(11) . . . . ? O13 Mn3 O16 C60 -52.7(11) . . . . ? O18 Mn3 O16 C60 -159(2) . . . . ? O14 Mn3 O17 C61 -26(28) . . . . ? O15 Mn3 O17 C61 141.3(8) . . . . ? O13 Mn3 O17 C61 -40.7(8) . . . . ? O16 Mn3 O17 C61 52.7(8) . . . . ? O18 Mn3 O17 C61 -129.0(8) . . . . ? O14 Mn3 O18 C62 175.9(7) . . . . ? O15 Mn3 O18 C62 84.8(7) . . . . ? O17 Mn3 O18 C62 -4.8(7) . . . . ? O13 Mn3 O18 C62 -94.2(7) . . . . ? O16 Mn3 O18 C62 13(3) . . . . ? 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 O13 H13B O4 0.83(2) 1.93(4) 2.718(8) 159(7) 1_455 O13 H13A O9 0.84(2) 1.97(3) 2.784(7) 166(7) 1_455 O14 H14A O5 0.83(2) 1.86(2) 2.685(9) 174(10) 1_455 O14 H14B O10 0.84(2) 1.88(2) 2.710(9) 174(11) 2_666 O15 H15A O7 0.92(5) 1.81(5) 2.709(8) 167(8) . O15 H15B O12 0.92(5) 1.80(5) 2.693(8) 164(8) . O16 H16 O19 0.902(17) 1.803(17) 2.698(9) 171(9) . O17 H17 O21 0.93(5) 1.67(5) 2.605(9) 177(10) . O18 H18A O10 0.95 2.03 2.627(8) 119.1 1_455 O19 H19 O6 0.93(5) 1.85(8) 2.695(8) 149(11) . O20 H20B O12 0.84(2) 2.38(8) 2.727(9) 106(7) . O20 H20B O18 0.84(2) 2.31(7) 2.986(8) 138(8) . O21 H21 O11 0.94(5) 1.91(8) 2.750(9) 147(10) . O2 H2 O20 0.81(2) 1.97(4) 2.722(8) 154(8) 2_666 O2 H2 O9 0.81(2) 2.63(6) 2.880(7) 100(4) . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.961 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.092 data_jon59 _database_code_depnum_ccdc_archive 'CCDC 893593' #TrackingRef 'web_deposit_cif_file_0_JonathanP.Hill_1343194442.1b_Hill.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C60.5 H69 Mn3 N2 O16), 2.5(C H4 O), 0.5(H2 O)' _chemical_formula_sum 'C63 H86 Mn3 N2 O19' _chemical_formula_weight 1340.16 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.7606(8) _cell_length_b 21.3505(8) _cell_length_c 26.7827(17) _cell_angle_alpha 90.00 _cell_angle_beta 91.494(8) _cell_angle_gamma 90.00 _cell_volume 6722.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 23.08 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2820 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.859 _exptl_absorpt_correction_T_max 0.901 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; Crystals were generally weakly diffracting to higher angles, resulting in the rather high R(int). The data from the measurement were truncated at resolution 0.90 Angstrom, as there was no significant intensity to higher resolutions. ; _diffrn_ambient_temperature 200(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 'Stoe IPDS' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39608 _diffrn_reflns_av_R_equivalents 0.0968 _diffrn_reflns_av_sigmaI/netI 0.1386 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 23.26 _reflns_number_total 9629 _reflns_number_gt 4888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_cell_refinement 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_data_reduction 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. One of the terminal ligands on Mn(3) (involving O(16)) was a disordered mixture of methanol and water. The methyl group was refined with 50% occupancy. No attempt was made to locate the half-hydrogen on O(16) (corresponding to the water ligand) that would have been lying under the O-C bond. This ligand disorder then resulted in disorder of the lattice solvent molecules, and similarity restraints were applied to methanol C-O bond lengths. O-H bond lengths were restrained to 0.92(4) Ang. ; _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^)+(0.0321P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9629 _refine_ls_number_parameters 800 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.014 _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 0.09408(8) 0.29496(4) 0.44167(3) 0.0309(2) Uani 1 1 d . . . Mn2 Mn 0.15020(7) 0.42070(4) 0.40218(3) 0.0296(2) Uani 1 1 d . . . Mn3 Mn 0.55918(8) 0.32160(5) 0.46600(4) 0.0388(3) Uani 1 1 d D A . O1 O 0.1062(3) 0.33812(18) 0.37872(15) 0.0344(10) Uani 1 1 d . . . C1 C 0.1583(6) 0.3089(3) 0.3374(2) 0.0476(18) Uani 1 1 d . . . H1A H 0.1178 0.2700 0.3290 0.071 Uiso 1 1 calc R . . H1B H 0.2379 0.2993 0.3461 0.071 Uiso 1 1 calc R . . H1C H 0.1552 0.3372 0.3086 0.071 Uiso 1 1 calc R . . O2 O 0.1371(3) 0.3778(2) 0.46565(15) 0.0358(11) Uani 1 1 d D . . H2 H 0.100(5) 0.391(3) 0.4910(18) 0.043 Uiso 1 1 d D . . N1 N 0.1211(4) 0.2511(2) 0.51219(18) 0.0320(13) Uani 1 1 d . . . C3 C 0.2350(5) 0.2692(3) 0.5296(2) 0.0342(15) Uani 1 1 d . . . H3A H 0.2630 0.2387 0.5549 0.041 Uiso 1 1 calc R . . H3B H 0.2317 0.3109 0.5457 0.041 Uiso 1 1 calc R . . C4 C 0.3175(5) 0.2715(3) 0.4870(3) 0.0368(16) Uani 1 1 d . . . O3 O 0.2764(3) 0.2703(2) 0.44344(17) 0.0382(11) Uani 1 1 d . . . O4 O 0.4193(4) 0.2773(2) 0.49866(18) 0.0541(14) Uani 1 1 d . . . C5 C 0.0320(5) 0.2702(3) 0.5459(2) 0.0351(16) Uani 1 1 d . . . H5A H 0.0591 0.3068 0.5655 0.042 Uiso 1 1 calc R . . H5B H 0.0181 0.2356 0.5696 0.042 Uiso 1 1 calc R . . C6 C -0.0777(5) 0.2868(3) 0.5198(3) 0.0368(16) Uani 1 1 d . . . O5 O -0.0733(3) 0.3047(2) 0.47478(16) 0.0357(10) Uani 1 1 d . . . O6 O -0.1653(4) 0.2851(2) 0.54404(18) 0.0580(14) Uani 1 1 d . . . C7 C 0.1177(5) 0.1814(3) 0.5042(2) 0.0365(16) Uani 1 1 d . . . H7A H 0.1823 0.1693 0.4833 0.044 Uiso 1 1 calc R . . H7B H 0.1280 0.1603 0.5369 0.044 Uiso 1 1 calc R . . C8 C 0.0094(5) 0.1583(3) 0.4796(2) 0.0321(15) Uani 1 1 d . . . C9 C -0.0558(5) 0.1129(3) 0.5015(2) 0.0374(16) Uani 1 1 d . . . H9A H -0.0354 0.0987 0.5341 0.045 Uiso 1 1 calc R . . C10 C -0.1490(5) 0.0876(3) 0.4775(2) 0.0317(15) Uani 1 1 d . . . C11 C -0.1749(5) 0.1097(3) 0.4294(2) 0.0377(16) Uani 1 1 d . . . H11A H -0.2402 0.0931 0.4124 0.045 Uiso 1 1 calc R . . C12 C -0.1109(5) 0.1544(3) 0.4048(2) 0.0325(15) Uani 1 1 d . . . C13 C -0.0167(5) 0.1793(3) 0.4312(2) 0.0307(15) Uani 1 1 d . . . O7 O 0.0523(3) 0.22143(19) 0.41031(15) 0.0370(11) Uani 1 1 d . . . C14 C -0.2249(5) 0.0368(3) 0.5005(2) 0.0410(17) Uani 1 1 d . . . C15 C -0.1627(6) 0.0036(3) 0.5437(3) 0.051(2) Uani 1 1 d . . . H15A H -0.2127 -0.0281 0.5579 0.077 Uiso 1 1 calc R . . H15B H -0.1414 0.0343 0.5695 0.077 Uiso 1 1 calc R . . H15C H -0.0940 -0.0166 0.5315 0.077 Uiso 1 1 calc R . . C16 C -0.3283(6) 0.0700(4) 0.5202(3) 0.058(2) Uani 1 1 d . . . H16A H -0.3786 0.0394 0.5356 0.087 Uiso 1 1 calc R . . H16B H -0.3692 0.0910 0.4926 0.087 Uiso 1 1 calc R . . H16C H -0.3040 0.1011 0.5452 0.087 Uiso 1 1 calc R . . C17 C -0.2567(6) -0.0136(3) 0.4624(3) 0.0420(17) Uani 1 1 d . . . C18 C -0.3567(7) -0.0459(4) 0.4645(4) 0.077(3) Uani 1 1 d . . . H18A H -0.4072 -0.0364 0.4906 0.092 Uiso 1 1 calc R . . C19 C -0.3879(8) -0.0924(4) 0.4299(4) 0.089(3) Uani 1 1 d . . . H19A H -0.4595 -0.1128 0.4319 0.107 Uiso 1 1 calc R . . C20 C -0.3160(8) -0.1077(4) 0.3941(3) 0.070(2) Uani 1 1 d . . . H20A H -0.3363 -0.1391 0.3704 0.084 Uiso 1 1 calc R . . C21 C -0.2126(7) -0.0781(4) 0.3916(3) 0.059(2) Uani 1 1 d . . . H21A H -0.1612 -0.0893 0.3664 0.070 Uiso 1 1 calc R . . C22 C -0.1836(6) -0.0321(3) 0.4257(3) 0.0484(18) Uani 1 1 d . . . H22A H -0.1113 -0.0126 0.4240 0.058 Uiso 1 1 calc R . . C23 C -0.1347(5) 0.1716(3) 0.3501(2) 0.0397(17) Uani 1 1 d . . . C24 C -0.2382(6) 0.1395(4) 0.3284(3) 0.059(2) Uani 1 1 d . . . H24A H -0.2278 0.0940 0.3302 0.089 Uiso 1 1 calc R . . H24B H -0.2493 0.1520 0.2934 0.089 Uiso 1 1 calc R . . H24C H -0.3050 0.1515 0.3472 0.089 Uiso 1 1 calc R . . C25 C -0.1565(6) 0.2417(3) 0.3458(3) 0.0518(19) Uani 1 1 d . . . H25A H -0.1707 0.2527 0.3106 0.078 Uiso 1 1 calc R . . H25B H -0.0899 0.2647 0.3587 0.078 Uiso 1 1 calc R . . H25C H -0.2231 0.2529 0.3652 0.078 Uiso 1 1 calc R . . C26 C -0.0321(6) 0.1512(3) 0.3196(3) 0.0485(19) Uani 1 1 d . . . C27 C -0.0031(7) 0.1791(4) 0.2760(3) 0.062(2) Uani 1 1 d . . . H27A H -0.0446 0.2147 0.2647 0.074 Uiso 1 1 calc R . . C28 C 0.0850(9) 0.1571(5) 0.2476(3) 0.078(3) Uani 1 1 d . . . H28A H 0.0997 0.1767 0.2166 0.093 Uiso 1 1 calc R . . C29 C 0.1496(10) 0.1091(5) 0.2626(4) 0.106(4) Uani 1 1 d . . . H29A H 0.2088 0.0939 0.2424 0.127 Uiso 1 1 calc R . . C30 C 0.1282(10) 0.0818(6) 0.3087(4) 0.119(4) Uani 1 1 d . . . H30A H 0.1760 0.0495 0.3217 0.143 Uiso 1 1 calc R . . C31 C 0.0373(9) 0.1021(5) 0.3348(3) 0.093(3) Uani 1 1 d . . . H31A H 0.0207 0.0815 0.3652 0.112 Uiso 1 1 calc R . . N2 N 0.2277(4) 0.5039(2) 0.43229(17) 0.0306(12) Uani 1 1 d . . . C32 C 0.3249(5) 0.4840(3) 0.4644(2) 0.0363(16) Uani 1 1 d . . . H32A H 0.2974 0.4736 0.4981 0.044 Uiso 1 1 calc R . . H32B H 0.3795 0.5191 0.4681 0.044 Uiso 1 1 calc R . . C33 C 0.3849(5) 0.4283(3) 0.4438(2) 0.0327(15) Uani 1 1 d . . . O8 O 0.3362(3) 0.40018(19) 0.40750(16) 0.0360(11) Uani 1 1 d . . . O9 O 0.4768(3) 0.4122(2) 0.46451(17) 0.0477(12) Uani 1 1 d . . . C34 C 0.1439(5) 0.5411(3) 0.4589(2) 0.0366(16) Uani 1 1 d . . . H34A H 0.1608 0.5861 0.4543 0.044 Uiso 1 1 calc R . . H34B H 0.1514 0.5318 0.4951 0.044 Uiso 1 1 calc R . . C35 C 0.0225(5) 0.5285(3) 0.4416(2) 0.0322(15) Uani 1 1 d . . . O10 O 0.0041(3) 0.4768(2) 0.41842(15) 0.0355(10) Uani 1 1 d . . . O11 O -0.0535(4) 0.5657(2) 0.45245(15) 0.0419(11) Uani 1 1 d . . . C36 C 0.2707(5) 0.5410(3) 0.3888(2) 0.0316(15) Uani 1 1 d . . . H36A H 0.3065 0.5800 0.4015 0.038 Uiso 1 1 calc R . . H36B H 0.3300 0.5163 0.3721 0.038 Uiso 1 1 calc R . . C37 C 0.1793(5) 0.5574(3) 0.3513(2) 0.0284(14) Uani 1 1 d . . . C38 C 0.1520(5) 0.6194(3) 0.3410(2) 0.0366(16) Uani 1 1 d . . . H38A H 0.1892 0.6519 0.3594 0.044 Uiso 1 1 calc R . . C39 C 0.0713(5) 0.6345(3) 0.3044(2) 0.0365(16) Uani 1 1 d . . . C40 C 0.0168(5) 0.5854(3) 0.2796(2) 0.0393(16) Uani 1 1 d . . . H40A H -0.0381 0.5956 0.2542 0.047 Uiso 1 1 calc R . . C41 C 0.0371(5) 0.5225(3) 0.2893(2) 0.0312(15) Uani 1 1 d . . . C42 C 0.1229(5) 0.5093(3) 0.3256(2) 0.0303(15) Uani 1 1 d . . . O12 O 0.1526(3) 0.44982(19) 0.33678(14) 0.0328(10) Uani 1 1 d . . . C43 C 0.0395(6) 0.7021(3) 0.2907(2) 0.0394(16) Uani 1 1 d . . . C44 C 0.1136(6) 0.7494(3) 0.3191(3) 0.057(2) Uani 1 1 d . . . H44A H 0.1028 0.7445 0.3550 0.086 Uiso 1 1 calc R . . H44B H 0.0921 0.7919 0.3088 0.086 Uiso 1 1 calc R . . H44C H 0.1937 0.7421 0.3116 0.086 Uiso 1 1 calc R . . C45 C 0.0610(7) 0.7115(4) 0.2348(3) 0.061(2) Uani 1 1 d . . . H45A H 0.0143 0.6819 0.2152 0.092 Uiso 1 1 calc R . . H45B H 0.1415 0.7041 0.2284 0.092 Uiso 1 1 calc R . . H45C H 0.0407 0.7544 0.2251 0.092 Uiso 1 1 calc R . . C46 C -0.0861(6) 0.7154(3) 0.3019(2) 0.0397(17) Uani 1 1 d . . . C47 C -0.1524(6) 0.6773(3) 0.3301(3) 0.0461(18) Uani 1 1 d . . . H47A H -0.1201 0.6401 0.3437 0.055 Uiso 1 1 calc R . . C48 C -0.2637(6) 0.6910(4) 0.3393(3) 0.055(2) Uani 1 1 d . . . H48A H -0.3074 0.6624 0.3581 0.066 Uiso 1 1 calc R . . C49 C -0.3124(7) 0.7446(4) 0.3222(3) 0.064(2) Uani 1 1 d . . . H49A H -0.3889 0.7545 0.3295 0.076 Uiso 1 1 calc R . . C50 C -0.2489(8) 0.7838(4) 0.2942(3) 0.072(3) Uani 1 1 d . . . H50A H -0.2816 0.8214 0.2814 0.087 Uiso 1 1 calc R . . C51 C -0.1364(7) 0.7692(4) 0.2841(3) 0.062(2) Uani 1 1 d . . . H51A H -0.0935 0.7972 0.2644 0.075 Uiso 1 1 calc R . . C52 C -0.0293(5) 0.4710(3) 0.2623(2) 0.0392(16) Uani 1 1 d . . . C53 C -0.0891(5) 0.4303(3) 0.3006(2) 0.0468(18) Uani 1 1 d . . . H53A H -0.0324 0.4117 0.3236 0.070 Uiso 1 1 calc R . . H53B H -0.1314 0.3968 0.2832 0.070 Uiso 1 1 calc R . . H53C H -0.1419 0.4561 0.3194 0.070 Uiso 1 1 calc R . . C54 C -0.1242(6) 0.4991(3) 0.2275(3) 0.058(2) Uani 1 1 d . . . H54A H -0.0897 0.5256 0.2022 0.087 Uiso 1 1 calc R . . H54B H -0.1760 0.5242 0.2474 0.087 Uiso 1 1 calc R . . H54C H -0.1667 0.4650 0.2111 0.087 Uiso 1 1 calc R . . C55 C 0.0469(6) 0.4333(3) 0.2283(2) 0.0398(17) Uani 1 1 d . . . C56 C 0.0407(6) 0.3690(4) 0.2230(3) 0.0509(19) Uani 1 1 d . . . H56A H -0.0092 0.3461 0.2434 0.061 Uiso 1 1 calc R . . C57 C 0.1038(7) 0.3377(4) 0.1893(3) 0.062(2) Uani 1 1 d . . . H57A H 0.0978 0.2934 0.1870 0.074 Uiso 1 1 calc R . . C58 C 0.1759(7) 0.3690(4) 0.1589(3) 0.065(2) Uani 1 1 d . . . H58A H 0.2204 0.3468 0.1356 0.079 Uiso 1 1 calc R . . C59 C 0.1828(8) 0.4318(5) 0.1623(3) 0.080(3) Uani 1 1 d . . . H59A H 0.2305 0.4544 0.1406 0.096 Uiso 1 1 calc R . . C60 C 0.1196(7) 0.4642(4) 0.1980(3) 0.065(2) Uani 1 1 d . . . H60A H 0.1278 0.5083 0.2011 0.078 Uiso 1 1 calc R . . O13 O 0.7207(4) 0.3583(3) 0.4448(2) 0.0565(14) Uani 1 1 d D . . H131 H 0.789(4) 0.343(3) 0.457(3) 0.085 Uiso 1 1 d D . . H132 H 0.732(6) 0.395(3) 0.424(2) 0.085 Uiso 1 1 d D . . O14 O 0.6404(4) 0.2274(3) 0.4617(3) 0.0762(17) Uani 1 1 d D . . H141 H 0.599(5) 0.198(3) 0.446(3) 0.114 Uiso 1 1 d D . . H142 H 0.715(3) 0.226(3) 0.464(4) 0.114 Uiso 1 1 d D . . O15 O 0.6280(3) 0.3269(2) 0.54360(16) 0.0451(12) Uani 1 1 d D . . H15 H 0.702(4) 0.314(3) 0.537(2) 0.054 Uiso 1 1 d D . . C61 C 0.5802(6) 0.2951(4) 0.5852(3) 0.072(3) Uani 1 1 d D . . H61A H 0.6255 0.3044 0.6155 0.108 Uiso 1 1 calc R . . H61B H 0.5804 0.2499 0.5791 0.108 Uiso 1 1 calc R . . H61C H 0.5018 0.3094 0.5895 0.108 Uiso 1 1 calc R . . O16 O 0.4904(4) 0.3074(3) 0.3885(2) 0.0707(16) Uani 1 1 d D . . H16 H 0.467(7) 0.2688(16) 0.398(3) 0.085 Uiso 1 1 d D . . C62A C 0.556(2) 0.3377(12) 0.3481(9) 0.146(10) Uiso 0.50 1 d PD A 1 H62A H 0.5191 0.3289 0.3157 0.219 Uiso 0.50 1 calc PR A 1 H62B H 0.6337 0.3210 0.3486 0.219 Uiso 0.50 1 calc PR A 1 H62C H 0.5586 0.3831 0.3536 0.219 Uiso 0.50 1 calc PR A 1 O71 O -0.2367(5) 0.4744(3) 0.4118(3) 0.0866(19) Uani 1 1 d D . . H71 H -0.1672 0.4830 0.4149 0.130 Uiso 1 1 calc R . . C71 C -0.2986(10) 0.5295(6) 0.3956(4) 0.116(4) Uani 1 1 d D . . H71A H -0.3792 0.5246 0.4031 0.174 Uiso 1 1 calc R . . H71B H -0.2905 0.5351 0.3595 0.174 Uiso 1 1 calc R . . H71C H -0.2680 0.5663 0.4132 0.174 Uiso 1 1 calc R . . O72A O 0.5150(13) 0.1539(9) 0.4034(7) 0.124(6) Uiso 0.50 1 d PD B 1 O72B O 0.4725(15) 0.1804(7) 0.3976(6) 0.118(6) Uiso 0.50 1 d PD B 2 C72 C 0.4026(14) 0.1249(8) 0.4014(6) 0.185(6) Uiso 1 1 d D . . O73B O 0.5483(15) 0.3821(9) 0.3065(7) 0.144(6) Uiso 0.50 1 d PD C 2 C73B C 0.523(4) 0.4330(19) 0.2674(15) 0.27(2) Uiso 0.50 1 d PD C 2 O74A O 0.3653(10) 0.4233(6) 0.2735(5) 0.093(4) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0300(5) 0.0291(6) 0.0333(5) 0.0027(5) -0.0016(4) -0.0013(4) Mn2 0.0291(5) 0.0281(6) 0.0316(5) 0.0009(5) -0.0012(4) 0.0004(4) Mn3 0.0285(5) 0.0410(6) 0.0468(6) 0.0023(5) -0.0015(4) 0.0004(5) O1 0.038(2) 0.030(3) 0.035(2) -0.002(2) 0.001(2) 0.0007(19) C1 0.063(5) 0.037(4) 0.043(4) 0.001(4) 0.003(4) 0.005(4) O2 0.037(3) 0.037(3) 0.033(3) -0.001(2) 0.000(2) 0.000(2) N1 0.024(3) 0.031(3) 0.041(3) 0.000(3) 0.002(2) -0.002(2) C3 0.027(3) 0.032(4) 0.044(4) 0.003(3) -0.004(3) -0.002(3) C4 0.029(4) 0.034(4) 0.048(5) 0.011(3) -0.003(3) 0.000(3) O3 0.030(2) 0.041(3) 0.044(3) 0.005(2) 0.002(2) 0.000(2) O4 0.027(3) 0.073(4) 0.062(3) 0.015(3) -0.008(2) -0.006(2) C5 0.034(4) 0.035(4) 0.036(4) 0.002(3) -0.001(3) 0.001(3) C6 0.034(4) 0.032(4) 0.044(4) 0.003(4) 0.001(3) 0.004(3) O5 0.030(2) 0.041(3) 0.036(3) 0.008(2) -0.0029(19) 0.0023(19) O6 0.030(3) 0.084(4) 0.061(3) 0.020(3) 0.012(2) 0.010(3) C7 0.028(3) 0.036(4) 0.044(4) 0.005(3) -0.005(3) -0.002(3) C8 0.032(3) 0.024(4) 0.041(4) 0.003(3) 0.000(3) 0.001(3) C9 0.039(4) 0.036(4) 0.037(4) 0.004(3) -0.004(3) -0.004(3) C10 0.028(3) 0.026(4) 0.042(4) 0.001(3) 0.006(3) -0.002(3) C11 0.032(4) 0.035(4) 0.046(4) -0.007(4) 0.001(3) -0.006(3) C12 0.030(4) 0.027(4) 0.040(4) -0.004(3) 0.002(3) -0.003(3) C13 0.029(3) 0.026(4) 0.038(4) -0.001(3) 0.003(3) -0.003(3) O7 0.036(2) 0.040(3) 0.036(2) 0.005(2) 0.004(2) -0.004(2) C14 0.039(4) 0.041(4) 0.043(4) 0.000(4) 0.003(3) -0.009(3) C15 0.057(5) 0.051(5) 0.046(4) 0.004(4) 0.005(4) -0.021(4) C16 0.045(4) 0.058(5) 0.072(5) -0.002(5) 0.018(4) -0.008(4) C17 0.042(4) 0.036(4) 0.048(4) 0.005(4) 0.000(3) -0.007(3) C18 0.053(5) 0.079(7) 0.099(7) -0.028(6) 0.016(5) -0.025(5) C19 0.068(6) 0.078(7) 0.122(8) -0.040(7) 0.007(6) -0.026(5) C20 0.093(7) 0.051(6) 0.065(6) -0.008(5) -0.025(5) -0.007(5) C21 0.078(6) 0.051(5) 0.047(5) 0.002(4) -0.006(4) 0.004(5) C22 0.058(5) 0.038(4) 0.049(5) 0.001(4) -0.011(4) -0.004(4) C23 0.047(4) 0.034(4) 0.038(4) 0.000(3) -0.002(3) -0.005(3) C24 0.071(5) 0.070(6) 0.037(4) 0.005(4) -0.016(4) -0.018(4) C25 0.055(5) 0.056(5) 0.044(4) 0.005(4) -0.001(4) 0.000(4) C26 0.065(5) 0.038(5) 0.043(4) 0.002(4) 0.009(4) -0.005(4) C27 0.082(6) 0.056(5) 0.047(5) 0.008(4) 0.004(4) 0.005(5) C28 0.109(8) 0.069(7) 0.055(6) 0.011(5) 0.026(5) -0.003(6) C29 0.130(9) 0.101(9) 0.089(8) -0.005(7) 0.071(7) 0.012(7) C30 0.137(10) 0.125(10) 0.099(8) 0.028(8) 0.049(7) 0.068(8) C31 0.118(8) 0.091(8) 0.074(6) 0.013(6) 0.054(6) 0.031(6) N2 0.031(3) 0.029(3) 0.031(3) 0.005(2) -0.003(2) 0.002(2) C32 0.034(4) 0.036(4) 0.038(4) 0.000(3) -0.007(3) 0.003(3) C33 0.031(4) 0.037(4) 0.031(4) 0.007(3) -0.005(3) -0.003(3) O8 0.027(2) 0.036(3) 0.044(3) 0.000(2) -0.003(2) 0.0047(19) O9 0.034(3) 0.048(3) 0.060(3) 0.002(3) -0.017(2) 0.003(2) C34 0.038(4) 0.036(4) 0.036(4) 0.001(3) 0.003(3) -0.001(3) C35 0.039(4) 0.033(4) 0.025(4) 0.010(3) 0.001(3) 0.001(3) O10 0.031(2) 0.038(3) 0.037(3) -0.002(2) -0.0007(19) 0.003(2) O11 0.041(3) 0.040(3) 0.045(3) 0.000(2) 0.004(2) 0.016(2) C36 0.031(3) 0.025(4) 0.038(4) 0.000(3) 0.000(3) -0.003(3) C37 0.032(3) 0.025(4) 0.029(3) 0.003(3) 0.004(3) -0.002(3) C38 0.043(4) 0.033(4) 0.034(4) -0.003(3) 0.002(3) -0.008(3) C39 0.043(4) 0.034(4) 0.032(4) 0.005(3) 0.006(3) -0.001(3) C40 0.046(4) 0.037(5) 0.035(4) -0.001(3) -0.004(3) 0.007(3) C41 0.032(4) 0.031(4) 0.030(4) -0.003(3) -0.002(3) 0.005(3) C42 0.032(4) 0.028(4) 0.030(4) 0.002(3) 0.006(3) 0.004(3) O12 0.037(2) 0.026(2) 0.036(2) -0.003(2) 0.0027(19) 0.0003(19) C43 0.055(4) 0.030(4) 0.033(4) 0.003(3) 0.000(3) 0.000(3) C44 0.064(5) 0.033(4) 0.074(5) 0.013(4) -0.003(4) 0.003(4) C45 0.082(6) 0.054(5) 0.049(5) 0.014(4) 0.009(4) 0.012(4) C46 0.052(4) 0.028(4) 0.039(4) -0.001(3) -0.005(3) 0.003(3) C47 0.052(4) 0.038(4) 0.048(4) 0.001(4) -0.004(4) 0.006(4) C48 0.050(5) 0.058(6) 0.058(5) -0.004(4) 0.003(4) 0.002(4) C49 0.057(5) 0.075(7) 0.060(6) -0.008(5) -0.003(4) 0.017(5) C50 0.078(6) 0.067(6) 0.071(6) -0.002(5) -0.013(5) 0.038(5) C51 0.072(6) 0.061(6) 0.054(5) 0.013(4) 0.003(4) 0.017(4) C52 0.047(4) 0.037(4) 0.033(4) 0.002(3) -0.004(3) 0.005(3) C53 0.038(4) 0.052(5) 0.050(4) -0.003(4) -0.003(3) -0.003(4) C54 0.058(5) 0.049(5) 0.067(5) -0.008(4) -0.026(4) 0.009(4) C55 0.053(4) 0.032(4) 0.034(4) -0.003(3) -0.007(3) 0.002(3) C56 0.052(4) 0.047(5) 0.054(5) -0.005(4) 0.000(4) 0.003(4) C57 0.065(5) 0.045(5) 0.074(6) -0.020(5) -0.009(5) 0.011(4) C58 0.079(6) 0.064(6) 0.054(5) -0.013(5) 0.010(5) 0.022(5) C59 0.107(7) 0.073(7) 0.061(6) -0.001(5) 0.040(5) -0.006(6) C60 0.095(6) 0.043(5) 0.059(5) -0.006(4) 0.019(5) -0.006(5) O13 0.029(3) 0.065(4) 0.075(4) 0.021(3) -0.004(2) -0.002(2) O14 0.059(4) 0.048(4) 0.122(5) -0.005(4) 0.011(4) 0.004(3) O15 0.030(2) 0.058(3) 0.047(3) 0.002(3) 0.004(2) -0.001(2) C61 0.058(5) 0.108(7) 0.051(5) 0.017(5) 0.001(4) -0.028(5) O16 0.055(3) 0.102(5) 0.054(3) -0.017(4) -0.005(3) 0.016(3) O71 0.074(4) 0.097(5) 0.088(4) 0.014(4) -0.005(4) -0.025(4) C71 0.125(9) 0.132(11) 0.089(8) 0.038(7) -0.023(7) 0.019(8) _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 O7 1.841(4) . ? Mn1 O1 1.930(4) . ? Mn1 O2 1.944(5) . ? Mn1 N1 2.125(5) . ? Mn1 O5 2.190(4) . ? Mn1 O3 2.207(4) . ? Mn1 Mn2 2.9661(13) . ? Mn2 O12 1.860(4) . ? Mn2 O1 1.938(4) . ? Mn2 O2 1.941(4) . ? Mn2 N2 2.145(5) . ? Mn2 O10 2.148(4) . ? Mn2 O8 2.232(4) . ? Mn3 O4 2.107(5) . ? Mn3 O13 2.145(5) . ? Mn3 O9 2.163(5) . ? Mn3 O15 2.213(4) . ? Mn3 O16 2.228(5) . ? Mn3 O14 2.230(5) . ? O1 C1 1.424(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 H2 0.86(3) . ? N1 C5 1.459(7) . ? N1 C3 1.460(7) . ? N1 C7 1.503(8) . ? C3 C4 1.517(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O4 1.236(7) . ? C4 O3 1.252(7) . ? C5 C6 1.494(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O6 1.233(7) . ? C6 O5 1.267(7) . ? C7 C8 1.501(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.376(8) . ? C8 C13 1.399(8) . ? C9 C10 1.367(8) . ? C9 H9A 0.9500 . ? C10 C11 1.398(8) . ? C10 C14 1.544(8) . ? C11 C12 1.392(8) . ? C11 H11A 0.9500 . ? C12 C13 1.403(8) . ? C12 C23 1.529(9) . ? C13 O7 1.342(7) . ? C14 C16 1.514(9) . ? C14 C17 1.523(9) . ? C14 C15 1.527(9) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.366(9) . ? C17 C22 1.379(9) . ? C18 C19 1.401(11) . ? C18 H18A 0.9500 . ? C19 C20 1.336(11) . ? C19 H19A 0.9500 . ? C20 C21 1.373(11) . ? C20 H20A 0.9500 . ? C21 C22 1.378(10) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.501(9) . ? C23 C25 1.524(9) . ? C23 C26 1.537(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.363(10) . ? C26 C31 1.383(11) . ? C27 C28 1.382(11) . ? C27 H27A 0.9500 . ? C28 C29 1.332(13) . ? C28 H28A 0.9500 . ? C29 C30 1.395(13) . ? C29 H29A 0.9500 . ? C30 C31 1.364(12) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? N2 C34 1.466(7) . ? N2 C32 1.476(7) . ? N2 C36 1.507(7) . ? C32 C33 1.496(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O9 1.251(7) . ? C33 O8 1.266(7) . ? C34 C35 1.514(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O11 1.237(7) . ? C35 O10 1.281(7) . ? C36 C37 1.494(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.388(8) . ? C37 C42 1.395(8) . ? C38 C39 1.385(9) . ? C38 H38A 0.9500 . ? C39 C40 1.390(9) . ? C39 C43 1.533(9) . ? C40 C41 1.387(8) . ? C40 H40A 0.9500 . ? C41 C42 1.411(8) . ? C41 C52 1.521(9) . ? C42 O12 1.349(7) . ? C43 C44 1.524(9) . ? C43 C45 1.537(9) . ? C43 C46 1.541(9) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.367(9) . ? C46 C51 1.373(9) . ? C47 C48 1.370(9) . ? C47 H47A 0.9500 . ? C48 C49 1.354(10) . ? C48 H48A 0.9500 . ? C49 C50 1.360(11) . ? C49 H49A 0.9500 . ? C50 C51 1.392(10) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C55 1.524(9) . ? C52 C53 1.529(9) . ? C52 C54 1.555(9) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C60 1.364(9) . ? C55 C56 1.381(9) . ? C56 C57 1.358(10) . ? C56 H56A 0.9500 . ? C57 C58 1.366(11) . ? C57 H57A 0.9500 . ? C58 C59 1.347(11) . ? C58 H58A 0.9500 . ? C59 C60 1.408(11) . ? C59 H59A 0.9500 . ? C60 H60A 0.9500 . ? O13 H131 0.92(4) . ? O13 H132 0.97(4) . ? O14 H141 0.89(4) . ? O14 H142 0.88(4) . ? O15 C61 1.432(8) . ? O15 H15 0.93(4) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? O16 C62A 1.493(17) . ? O16 H16 0.91(3) . ? C62A H62A 0.9800 . ? C62A H62B 0.9800 . ? C62A H62C 0.9800 . ? O71 C71 1.444(10) . ? O71 H71 0.8400 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? O72A C72 1.461(16) . ? O72B C72 1.448(16) . ? O73B C73B 1.532(19) . ? C73B O74A 1.88(5) . ? 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 O7 Mn1 O1 91.93(17) . . ? O7 Mn1 O2 172.09(18) . . ? O1 Mn1 O2 80.20(17) . . ? O7 Mn1 N1 93.52(19) . . ? O1 Mn1 N1 167.00(18) . . ? O2 Mn1 N1 94.35(19) . . ? O7 Mn1 O5 91.90(17) . . ? O1 Mn1 O5 113.34(16) . . ? O2 Mn1 O5 90.51(16) . . ? N1 Mn1 O5 78.28(17) . . ? O7 Mn1 O3 93.11(17) . . ? O1 Mn1 O3 92.22(17) . . ? O2 Mn1 O3 88.03(17) . . ? N1 Mn1 O3 75.71(17) . . ? O5 Mn1 O3 153.76(16) . . ? O12 Mn2 O1 90.53(17) . . ? O12 Mn2 O2 170.54(18) . . ? O1 Mn2 O2 80.09(17) . . ? O12 Mn2 N2 93.46(18) . . ? O1 Mn2 N2 169.44(18) . . ? O2 Mn2 N2 95.99(18) . . ? O12 Mn2 O10 92.08(16) . . ? O1 Mn2 O10 111.40(17) . . ? O2 Mn2 O10 90.19(17) . . ? N2 Mn2 O10 78.25(17) . . ? O12 Mn2 O8 94.97(16) . . ? O1 Mn2 O8 95.45(16) . . ? O2 Mn2 O8 87.24(16) . . ? N2 Mn2 O8 74.48(17) . . ? O10 Mn2 O8 152.16(17) . . ? O4 Mn3 O13 168.59(19) . . ? O4 Mn3 O9 93.14(18) . . ? O13 Mn3 O9 93.87(19) . . ? O4 Mn3 O15 84.45(17) . . ? O13 Mn3 O15 85.75(18) . . ? O9 Mn3 O15 97.13(17) . . ? O4 Mn3 O16 93.3(2) . . ? O13 Mn3 O16 96.0(2) . . ? O9 Mn3 O16 87.28(19) . . ? O15 Mn3 O16 175.1(2) . . ? O4 Mn3 O14 87.5(2) . . ? O13 Mn3 O14 86.1(2) . . ? O9 Mn3 O14 175.9(2) . . ? O15 Mn3 O14 87.0(2) . . ? O16 Mn3 O14 88.6(2) . . ? C1 O1 Mn1 120.9(4) . . ? C1 O1 Mn2 122.3(4) . . ? Mn1 O1 Mn2 100.16(18) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Mn2 O2 Mn1 99.55(19) . . ? Mn2 O2 H2 126(4) . . ? Mn1 O2 H2 115(4) . . ? C5 N1 C3 113.4(5) . . ? C5 N1 C7 110.4(5) . . ? C3 N1 C7 109.2(5) . . ? C5 N1 Mn1 109.5(4) . . ? C3 N1 Mn1 106.4(4) . . ? C7 N1 Mn1 107.8(4) . . ? N1 C3 C4 111.6(5) . . ? N1 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? O4 C4 O3 125.9(6) . . ? O4 C4 C3 116.6(6) . . ? O3 C4 C3 117.5(5) . . ? C4 O3 Mn1 111.5(4) . . ? C4 O4 Mn3 134.6(4) . . ? N1 C5 C6 113.7(5) . . ? 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 . . ? O6 C6 O5 124.5(6) . . ? O6 C6 C5 118.0(6) . . ? O5 C6 C5 117.4(6) . . ? C6 O5 Mn1 114.6(4) . . ? C8 C7 N1 114.0(5) . . ? C8 C7 H7A 108.8 . . ? N1 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? N1 C7 H7B 108.8 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C13 120.6(6) . . ? C9 C8 C7 121.4(6) . . ? C13 C8 C7 117.6(5) . . ? C10 C9 C8 121.8(6) . . ? C10 C9 H9A 119.1 . . ? C8 C9 H9A 119.1 . . ? C9 C10 C11 117.0(6) . . ? C9 C10 C14 123.7(6) . . ? C11 C10 C14 119.3(5) . . ? C12 C11 C10 123.9(6) . . ? C12 C11 H11A 118.0 . . ? C10 C11 H11A 118.0 . . ? C11 C12 C13 116.9(6) . . ? C11 C12 C23 121.9(6) . . ? C13 C12 C23 120.9(5) . . ? O7 C13 C8 118.7(5) . . ? O7 C13 C12 121.5(6) . . ? C8 C13 C12 119.7(5) . . ? C13 O7 Mn1 122.6(4) . . ? C16 C14 C17 112.3(6) . . ? C16 C14 C15 109.0(6) . . ? C17 C14 C15 106.6(5) . . ? C16 C14 C10 106.7(5) . . ? C17 C14 C10 111.3(5) . . ? C15 C14 C10 111.0(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 116.0(7) . . ? C18 C17 C14 121.7(7) . . ? C22 C17 C14 122.2(6) . . ? C17 C18 C19 122.8(8) . . ? C17 C18 H18A 118.6 . . ? C19 C18 H18A 118.6 . . ? C20 C19 C18 119.2(8) . . ? C20 C19 H19A 120.4 . . ? C18 C19 H19A 120.4 . . ? C19 C20 C21 120.1(8) . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C20 C21 C22 120.0(8) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C21 C22 C17 121.9(7) . . ? C21 C22 H22A 119.1 . . ? C17 C22 H22A 119.1 . . ? C24 C23 C25 106.6(6) . . ? C24 C23 C12 112.9(5) . . ? C25 C23 C12 109.6(5) . . ? C24 C23 C26 107.7(6) . . ? C25 C23 C26 111.7(6) . . ? C12 C23 C26 108.3(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 115.1(7) . . ? C27 C26 C23 123.4(7) . . ? C31 C26 C23 121.5(6) . . ? C26 C27 C28 122.1(8) . . ? C26 C27 H27A 119.0 . . ? C28 C27 H27A 119.0 . . ? C29 C28 C27 121.7(8) . . ? C29 C28 H28A 119.1 . . ? C27 C28 H28A 119.1 . . ? C28 C29 C30 118.3(9) . . ? C28 C29 H29A 120.9 . . ? C30 C29 H29A 120.9 . . ? C31 C30 C29 118.9(10) . . ? C31 C30 H30A 120.5 . . ? C29 C30 H30A 120.5 . . ? C30 C31 C26 123.7(9) . . ? C30 C31 H31A 118.2 . . ? C26 C31 H31A 118.2 . . ? C34 N2 C32 113.1(5) . . ? C34 N2 C36 109.6(5) . . ? C32 N2 C36 109.4(4) . . ? C34 N2 Mn2 110.3(4) . . ? C32 N2 Mn2 107.2(4) . . ? C36 N2 Mn2 107.0(3) . . ? N2 C32 C33 112.3(5) . . ? N2 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? N2 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? O9 C33 O8 125.4(6) . . ? O9 C33 C32 117.6(6) . . ? O8 C33 C32 116.9(5) . . ? C33 O8 Mn2 112.3(4) . . ? C33 O9 Mn3 129.4(4) . . ? N2 C34 C35 113.2(5) . . ? N2 C34 H34A 108.9 . . ? C35 C34 H34A 108.9 . . ? N2 C34 H34B 108.9 . . ? C35 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? O11 C35 O10 123.6(6) . . ? O11 C35 C34 119.6(6) . . ? O10 C35 C34 116.6(6) . . ? C35 O10 Mn2 116.9(4) . . ? C37 C36 N2 113.2(5) . . ? C37 C36 H36A 108.9 . . ? N2 C36 H36A 108.9 . . ? C37 C36 H36B 108.9 . . ? N2 C36 H36B 108.9 . . ? H36A C36 H36B 107.8 . . ? C38 C37 C42 120.0(6) . . ? C38 C37 C36 121.1(6) . . ? C42 C37 C36 118.9(5) . . ? C39 C38 C37 120.9(6) . . ? C39 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C38 C39 C40 117.5(6) . . ? C38 C39 C43 123.2(6) . . ? C40 C39 C43 119.2(6) . . ? C41 C40 C39 124.5(6) . . ? C41 C40 H40A 117.8 . . ? C39 C40 H40A 117.8 . . ? C40 C41 C42 116.1(6) . . ? C40 C41 C52 121.8(5) . . ? C42 C41 C52 122.1(6) . . ? O12 C42 C37 117.8(5) . . ? O12 C42 C41 121.2(6) . . ? C37 C42 C41 121.0(6) . . ? C42 O12 Mn2 120.9(4) . . ? C44 C43 C39 111.7(5) . . ? C44 C43 C45 107.1(6) . . ? C39 C43 C45 108.1(5) . . ? C44 C43 C46 108.6(5) . . ? C39 C43 C46 110.8(5) . . ? C45 C43 C46 110.4(5) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C51 116.3(7) . . ? C47 C46 C43 124.1(6) . . ? C51 C46 C43 119.5(6) . . ? C46 C47 C48 122.3(7) . . ? C46 C47 H47A 118.9 . . ? C48 C47 H47A 118.9 . . ? C49 C48 C47 121.1(8) . . ? C49 C48 H48A 119.4 . . ? C47 C48 H48A 119.4 . . ? C48 C49 C50 118.2(8) . . ? C48 C49 H49A 120.9 . . ? C50 C49 H49A 120.9 . . ? C49 C50 C51 120.6(8) . . ? C49 C50 H50A 119.7 . . ? C51 C50 H50A 119.7 . . ? C46 C51 C50 121.5(8) . . ? C46 C51 H51A 119.3 . . ? C50 C51 H51A 119.3 . . ? C41 C52 C55 111.3(5) . . ? C41 C52 C53 109.4(5) . . ? C55 C52 C53 112.8(5) . . ? C41 C52 C54 111.0(5) . . ? C55 C52 C54 105.6(5) . . ? C53 C52 C54 106.6(6) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C60 C55 C56 116.8(7) . . ? C60 C55 C52 119.1(6) . . ? C56 C55 C52 123.8(6) . . ? C57 C56 C55 122.0(7) . . ? C57 C56 H56A 119.0 . . ? C55 C56 H56A 119.0 . . ? C56 C57 C58 120.9(8) . . ? C56 C57 H57A 119.6 . . ? C58 C57 H57A 119.6 . . ? C59 C58 C57 118.9(8) . . ? C59 C58 H58A 120.6 . . ? C57 C58 H58A 120.6 . . ? C58 C59 C60 120.3(8) . . ? C58 C59 H59A 119.9 . . ? C60 C59 H59A 119.9 . . ? C55 C60 C59 121.1(8) . . ? C55 C60 H60A 119.5 . . ? C59 C60 H60A 119.5 . . ? Mn3 O13 H131 123(5) . . ? Mn3 O13 H132 126(4) . . ? H131 O13 H132 111(6) . . ? Mn3 O14 H141 116(4) . . ? Mn3 O14 H142 117(4) . . ? H141 O14 H142 122(7) . . ? C61 O15 Mn3 124.4(4) . . ? C61 O15 H15 113(4) . . ? Mn3 O15 H15 98(4) . . ? O15 C61 H61A 109.5 . . ? O15 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O15 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C62A O16 Mn3 115.7(11) . . ? C62A O16 H16 140(5) . . ? Mn3 O16 H16 88(6) . . ? O16 C62A H62A 109.5 . . ? O16 C62A H62B 109.5 . . ? H62A C62A H62B 109.5 . . ? O16 C62A H62C 109.5 . . ? H62A C62A H62C 109.5 . . ? H62B C62A H62C 109.5 . . ? C71 O71 H71 109.5 . . ? O71 C71 H71A 109.5 . . ? O71 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? O71 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 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 O2 H2 O11 0.86(3) 1.87(4) 2.710(6) 164(6) 3_566 O13 H131 O5 0.92(4) 1.87(4) 2.780(6) 173(8) 1_655 O13 H132 O71 0.97(4) 1.77(5) 2.684(8) 155(7) 1_655 O14 H141 O72A 0.89(4) 1.77(5) 2.637(17) 165(9) . O14 H141 O72B 0.89(4) 1.99(6) 2.772(17) 145(7) . O15 H15 O6 0.93(4) 1.69(4) 2.589(6) 163(6) 1_655 O16 H16 O72B 0.91(3) 1.89(3) 2.732(17) 154(7) . O71 H71 O10 0.84 2.02 2.834(7) 163.3 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.927 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.087 data_ns291 _database_code_depnum_ccdc_archive 'CCDC 893594' #TrackingRef 'web_deposit_cif_file_0_JonathanP.Hill_1343194688.2a_Hill_new.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H36 Fe N O6, H2 O' _chemical_formula_sum 'C31 H38 Fe N O7' _chemical_formula_weight 592.47 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 orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.411(5) _cell_length_b 16.390(8) _cell_length_c 37.968(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5856(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 259 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 12.58 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 0.562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 0.983 _exptl_absorpt_process_details 'SADABS v2004/1, Sheldrick, G.M., (2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43338 _diffrn_reflns_av_R_equivalents 0.1358 _diffrn_reflns_av_sigmaI/netI 0.1115 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.18 _reflns_number_total 6102 _reflns_number_gt 3625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0643P)^2^+2.0071P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6102 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1320 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1266 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.52880(5) 0.20388(3) 0.295832(13) 0.01917(16) Uani 1 1 d . . . O1 O 0.5547(3) 0.32201(17) 0.28227(8) 0.0345(7) Uani 1 1 d . . . C1 C 0.4498(4) 0.3697(3) 0.28483(11) 0.0318(10) Uani 1 1 d . . . C2 C 0.3193(5) 0.3394(3) 0.30405(11) 0.0358(11) Uani 1 1 d . . . H2A H 0.3144 0.3661 0.3268 0.043 Uiso 1 1 calc R . . H2B H 0.2356 0.3553 0.2908 0.043 Uiso 1 1 calc R . . O2 O 0.4481(3) 0.44112(19) 0.27384(9) 0.0508(9) Uani 1 1 d . . . O3 O 0.4227(3) 0.19105(16) 0.24954(6) 0.0269(6) Uani 1 1 d . . . C3 C 0.2174(4) 0.2101(3) 0.28478(9) 0.0318(10) Uani 1 1 d . . . H3A H 0.1357 0.2450 0.2809 0.038 Uiso 1 1 calc R . . H3B H 0.1840 0.1592 0.2949 0.038 Uiso 1 1 calc R . . C4 C 0.2897(4) 0.1931(2) 0.24996(9) 0.0232(8) Uani 1 1 d . . . O4 O 0.2167(3) 0.17931(16) 0.22303(6) 0.0273(6) Uani 1 1 d . . . O5 O 0.4699(3) 0.08494(17) 0.30273(7) 0.0348(7) Uani 1 1 d . . . C5 C 0.5329(5) 0.0273(3) 0.32718(12) 0.0469(12) Uani 1 1 d . . . H5A H 0.6168 0.0514 0.3378 0.056 Uiso 1 1 calc R . . H5B H 0.5620 -0.0213 0.3145 0.056 Uiso 1 1 calc R . . C6 C 0.4320(6) 0.0048(3) 0.35483(13) 0.0710(18) Uani 1 1 d . . . H6A H 0.4098 0.0520 0.3688 0.107 Uiso 1 1 calc R . . H6B H 0.4733 -0.0364 0.3696 0.107 Uiso 1 1 calc R . . H6C H 0.3466 -0.0159 0.3443 0.107 Uiso 1 1 calc R . . N1 N 0.3160(3) 0.2500(2) 0.30951(7) 0.0238(8) Uani 1 1 d . . . C7 C 0.2783(4) 0.2298(2) 0.34653(9) 0.0213(9) Uani 1 1 d . . . H7A H 0.2741 0.1709 0.3489 0.026 Uiso 1 1 calc R . . H7B H 0.1840 0.2509 0.3514 0.026 Uiso 1 1 calc R . . C8 C 0.3789(4) 0.2625(2) 0.37390(9) 0.0195(8) Uani 1 1 d . . . C9 C 0.5260(4) 0.2495(2) 0.37052(8) 0.0182(8) Uani 1 1 d . . . O6 O 0.5797(3) 0.21199(16) 0.34247(6) 0.0254(6) Uani 1 1 d . . . C10 C 0.6187(4) 0.2753(2) 0.39742(9) 0.0187(8) Uani 1 1 d . . . C11 C 0.5613(4) 0.3104(2) 0.42727(9) 0.0227(9) Uani 1 1 d . . . H11 H 0.6217 0.3258 0.4455 0.027 Uiso 1 1 calc R . . C12 C 0.4143(4) 0.3237(2) 0.43105(9) 0.0199(8) Uani 1 1 d . . . C13 C 0.3262(4) 0.3010(2) 0.40365(9) 0.0209(8) Uani 1 1 d . . . C14 C 0.7805(4) 0.2652(2) 0.39133(9) 0.0220(9) Uani 1 1 d . . . C15 C 0.8256(4) 0.3227(2) 0.36168(11) 0.0318(10) Uani 1 1 d . . . H15A H 0.9257 0.3171 0.3575 0.048 Uiso 1 1 calc R . . H15B H 0.8049 0.3780 0.3683 0.048 Uiso 1 1 calc R . . H15C H 0.7744 0.3093 0.3406 0.048 Uiso 1 1 calc R . . C16 C 0.8662(4) 0.2900(3) 0.42413(10) 0.0337(10) Uani 1 1 d . . . H16A H 0.8382 0.2567 0.4437 0.051 Uiso 1 1 calc R . . H16B H 0.8482 0.3463 0.4295 0.051 Uiso 1 1 calc R . . H16C H 0.9658 0.2825 0.4196 0.051 Uiso 1 1 calc R . . C17 C 0.8169(4) 0.1760(2) 0.38361(9) 0.0217(9) Uani 1 1 d . . . C18 C 0.8949(4) 0.1519(2) 0.35425(10) 0.0289(10) Uani 1 1 d . . . H18 H 0.9224 0.1910 0.3378 0.035 Uiso 1 1 calc R . . C19 C 0.9325(4) 0.0715(3) 0.34892(12) 0.0364(11) Uani 1 1 d . . . H19 H 0.9841 0.0571 0.3290 0.044 Uiso 1 1 calc R . . C20 C 0.8943(5) 0.0120(3) 0.37295(13) 0.0398(11) Uani 1 1 d . . . H20 H 0.9214 -0.0420 0.3696 0.048 Uiso 1 1 calc R . . C21 C 0.8151(4) 0.0345(3) 0.40198(12) 0.0390(11) Uani 1 1 d . . . H21 H 0.7875 -0.0049 0.4182 0.047 Uiso 1 1 calc R . . C22 C 0.7761(4) 0.1154(3) 0.40720(10) 0.0307(10) Uani 1 1 d . . . H22 H 0.7219 0.1292 0.4268 0.037 Uiso 1 1 calc R . . C23 C 0.3474(4) 0.3594(2) 0.46493(9) 0.0232(9) Uani 1 1 d . . . C24 C 0.2509(4) 0.2936(2) 0.48082(9) 0.0302(9) Uani 1 1 d . . . H24A H 0.2081 0.3140 0.5020 0.045 Uiso 1 1 calc R . . H24B H 0.3062 0.2460 0.4862 0.045 Uiso 1 1 calc R . . H24C H 0.1778 0.2797 0.4642 0.045 Uiso 1 1 calc R . . C25 C 0.4592(4) 0.3811(3) 0.49277(10) 0.0340(10) Uani 1 1 d . . . H25A H 0.4127 0.4018 0.5134 0.051 Uiso 1 1 calc R . . H25B H 0.5221 0.4220 0.4835 0.051 Uiso 1 1 calc R . . H25C H 0.5127 0.3333 0.4988 0.051 Uiso 1 1 calc R . . C26 C 0.2663(4) 0.4374(2) 0.45585(9) 0.0229(9) Uani 1 1 d . . . C27 C 0.3381(5) 0.5022(2) 0.44056(11) 0.0323(10) Uani 1 1 d . . . H27 H 0.4337 0.4963 0.4350 0.039 Uiso 1 1 calc R . . C28 C 0.2713(5) 0.5754(3) 0.43342(11) 0.0408(12) Uani 1 1 d . . . H28 H 0.3225 0.6182 0.4236 0.049 Uiso 1 1 calc R . . C29 C 0.1301(5) 0.5850(3) 0.44072(12) 0.0438(12) Uani 1 1 d . . . H29 H 0.0852 0.6343 0.4360 0.053 Uiso 1 1 calc R . . C30 C 0.0548(5) 0.5215(3) 0.45503(11) 0.0408(12) Uani 1 1 d . . . H30 H -0.0417 0.5275 0.4596 0.049 Uiso 1 1 calc R . . C31 C 0.1226(4) 0.4482(3) 0.46267(10) 0.0317(10) Uani 1 1 d . . . H31 H 0.0707 0.4057 0.4725 0.038 Uiso 1 1 calc R . . O7 O 0.6815(4) 0.5082(2) 0.24140(10) 0.0495(9) Uani 1 1 d . . . H7Y H 0.755(5) 0.483(3) 0.2403(11) 0.034(14) Uiso 1 1 d . . . H7X H 0.639(7) 0.475(4) 0.2586(17) 0.11(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0129(3) 0.0283(3) 0.0163(3) -0.0002(2) 0.0003(2) 0.0016(2) O1 0.0219(16) 0.0295(17) 0.0523(18) 0.0106(14) 0.0001(13) 0.0000(13) C1 0.028(3) 0.032(3) 0.035(2) 0.0026(19) -0.0099(19) -0.001(2) C2 0.035(3) 0.039(3) 0.033(2) 0.009(2) 0.0005(19) 0.013(2) O2 0.041(2) 0.033(2) 0.079(2) 0.0120(17) 0.0012(17) 0.0004(15) O3 0.0148(14) 0.0452(18) 0.0209(13) 0.0001(12) -0.0002(11) 0.0010(13) C3 0.014(2) 0.060(3) 0.021(2) -0.004(2) -0.0044(15) 0.004(2) C4 0.019(2) 0.032(2) 0.0185(18) 0.0016(18) -0.0036(16) 0.0035(19) O4 0.0173(14) 0.0460(18) 0.0187(14) -0.0025(12) -0.0030(12) 0.0042(12) O5 0.0334(16) 0.0310(16) 0.0400(17) 0.0063(13) -0.0060(14) -0.0013(14) C5 0.049(3) 0.036(3) 0.056(3) 0.013(2) -0.012(3) -0.002(2) C6 0.092(5) 0.072(4) 0.049(3) 0.017(3) 0.014(3) 0.035(3) N1 0.0154(17) 0.036(2) 0.0197(16) 0.0004(14) -0.0015(14) 0.0014(15) C7 0.012(2) 0.030(2) 0.0217(19) -0.0008(16) 0.0011(15) 0.0021(16) C8 0.016(2) 0.022(2) 0.021(2) 0.0026(16) -0.0003(15) -0.0012(16) C9 0.0204(19) 0.020(2) 0.0139(17) 0.0003(15) 0.0018(16) 0.0024(17) O6 0.0155(13) 0.0421(17) 0.0185(13) -0.0039(12) -0.0010(10) 0.0056(12) C10 0.0136(19) 0.022(2) 0.0208(19) 0.0028(15) -0.0008(15) 0.0004(16) C11 0.025(2) 0.022(2) 0.0211(19) -0.0017(16) -0.0060(16) -0.0004(17) C12 0.022(2) 0.019(2) 0.0185(19) -0.0020(15) 0.0006(16) -0.0020(16) C13 0.021(2) 0.025(2) 0.0168(18) -0.0011(16) -0.0002(15) -0.0019(18) C14 0.016(2) 0.025(2) 0.025(2) -0.0028(16) 0.0008(16) -0.0004(17) C15 0.021(2) 0.033(2) 0.042(3) 0.0001(19) 0.0051(19) -0.0031(18) C16 0.020(2) 0.042(3) 0.039(2) -0.008(2) -0.0051(18) -0.003(2) C17 0.0123(19) 0.029(2) 0.024(2) 0.0035(17) -0.0084(16) -0.0011(16) C18 0.021(2) 0.032(3) 0.033(2) -0.0025(19) -0.0008(18) -0.0023(19) C19 0.026(2) 0.038(3) 0.045(3) -0.009(2) 0.003(2) 0.002(2) C20 0.027(3) 0.030(3) 0.062(3) -0.004(2) -0.008(2) 0.006(2) C21 0.030(3) 0.035(3) 0.053(3) 0.012(2) -0.007(2) -0.003(2) C22 0.025(2) 0.037(3) 0.030(2) 0.0025(19) -0.0027(18) 0.002(2) C23 0.021(2) 0.027(2) 0.021(2) -0.0034(16) -0.0013(16) -0.0007(18) C24 0.038(2) 0.030(2) 0.023(2) -0.0032(18) 0.0026(18) 0.003(2) C25 0.036(3) 0.043(3) 0.024(2) -0.0077(19) -0.0042(19) 0.007(2) C26 0.021(2) 0.031(2) 0.0172(19) -0.0064(16) -0.0007(16) 0.0019(18) C27 0.029(2) 0.032(3) 0.035(2) -0.0006(19) 0.002(2) -0.002(2) C28 0.050(3) 0.030(3) 0.043(3) -0.002(2) 0.000(2) -0.006(2) C29 0.060(3) 0.033(3) 0.038(3) -0.002(2) -0.006(2) 0.013(3) C30 0.028(3) 0.051(3) 0.043(3) -0.002(2) 0.001(2) 0.014(2) C31 0.032(3) 0.030(3) 0.033(2) -0.0003(19) 0.0026(19) 0.002(2) O7 0.043(2) 0.044(2) 0.062(2) 0.0156(18) 0.0028(18) 0.0166(19) _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 O6 1.839(2) . ? Fe1 O4 1.950(3) 6_656 ? Fe1 O1 2.018(3) . ? Fe1 O3 2.032(3) . ? Fe1 O5 2.044(3) . ? Fe1 N1 2.202(3) . ? O1 C1 1.263(5) . ? C1 O2 1.243(5) . ? C1 C2 1.512(6) . ? C2 N1 1.481(5) . ? O3 C4 1.252(4) . ? C3 N1 1.473(5) . ? C3 C4 1.512(5) . ? C4 O4 1.252(4) . ? O4 Fe1 1.950(3) 6_556 ? O5 C5 1.451(5) . ? C5 C6 1.463(7) . ? N1 C7 1.487(4) . ? C7 C8 1.505(5) . ? C8 C13 1.386(5) . ? C8 C9 1.406(5) . ? C9 O6 1.330(4) . ? C9 C10 1.408(5) . ? C10 C11 1.382(5) . ? C10 C14 1.549(5) . ? C11 C12 1.407(5) . ? C12 C13 1.382(5) . ? C12 C23 1.547(5) . ? C14 C15 1.528(5) . ? C14 C17 1.529(5) . ? C14 C16 1.539(5) . ? C17 C22 1.392(5) . ? C17 C18 1.392(5) . ? C18 C19 1.380(6) . ? C19 C20 1.383(6) . ? C20 C21 1.381(6) . ? C21 C22 1.390(6) . ? C23 C26 1.529(5) . ? C23 C25 1.533(5) . ? C23 C24 1.533(5) . ? C26 C27 1.386(5) . ? C26 C31 1.388(5) . ? C27 C28 1.380(6) . ? C28 C29 1.367(6) . ? C29 C30 1.370(6) . ? C30 C31 1.391(6) . ? 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 O6 Fe1 O4 97.59(11) . 6_656 ? O6 Fe1 O1 98.33(12) . . ? O4 Fe1 O1 89.70(11) 6_656 . ? O6 Fe1 O3 165.49(11) . . ? O4 Fe1 O3 96.12(10) 6_656 . ? O1 Fe1 O3 86.45(11) . . ? O6 Fe1 O5 90.93(11) . . ? O4 Fe1 O5 95.49(12) 6_656 . ? O1 Fe1 O5 168.71(11) . . ? O3 Fe1 O5 83.04(11) . . ? O6 Fe1 N1 89.15(11) . . ? O4 Fe1 N1 169.13(11) 6_656 . ? O1 Fe1 N1 80.86(11) . . ? O3 Fe1 N1 78.03(11) . . ? O5 Fe1 N1 92.90(12) . . ? C1 O1 Fe1 118.6(3) . . ? O2 C1 O1 124.5(4) . . ? O2 C1 C2 117.4(4) . . ? O1 C1 C2 118.0(4) . . ? N1 C2 C1 114.1(3) . . ? C4 O3 Fe1 118.5(2) . . ? N1 C3 C4 110.8(3) . . ? O3 C4 O4 122.2(3) . . ? O3 C4 C3 117.7(3) . . ? O4 C4 C3 120.0(3) . . ? C4 O4 Fe1 139.4(2) . 6_556 ? C5 O5 Fe1 126.3(3) . . ? O5 C5 C6 111.0(4) . . ? C3 N1 C2 111.3(3) . . ? C3 N1 C7 110.7(3) . . ? C2 N1 C7 111.0(3) . . ? C3 N1 Fe1 105.7(2) . . ? C2 N1 Fe1 106.7(2) . . ? C7 N1 Fe1 111.3(2) . . ? N1 C7 C8 115.0(3) . . ? C13 C8 C9 119.7(3) . . ? C13 C8 C7 120.0(3) . . ? C9 C8 C7 120.2(3) . . ? O6 C9 C8 121.2(3) . . ? O6 C9 C10 118.9(3) . . ? C8 C9 C10 119.9(3) . . ? C9 O6 Fe1 134.9(2) . . ? C11 C10 C9 118.5(3) . . ? C11 C10 C14 123.5(3) . . ? C9 C10 C14 118.0(3) . . ? C10 C11 C12 122.2(3) . . ? C13 C12 C11 118.1(3) . . ? C13 C12 C23 118.9(3) . . ? C11 C12 C23 122.9(3) . . ? C12 C13 C8 121.4(3) . . ? C15 C14 C17 112.7(3) . . ? C15 C14 C16 106.7(3) . . ? C17 C14 C16 106.9(3) . . ? C15 C14 C10 108.5(3) . . ? C17 C14 C10 110.5(3) . . ? C16 C14 C10 111.5(3) . . ? C22 C17 C18 117.2(4) . . ? C22 C17 C14 119.8(3) . . ? C18 C17 C14 122.9(3) . . ? C19 C18 C17 121.6(4) . . ? C18 C19 C20 120.7(4) . . ? C21 C20 C19 118.6(4) . . ? C20 C21 C22 120.7(4) . . ? C21 C22 C17 121.1(4) . . ? C26 C23 C25 107.6(3) . . ? C26 C23 C24 112.4(3) . . ? C25 C23 C24 107.4(3) . . ? C26 C23 C12 109.4(3) . . ? C25 C23 C12 112.4(3) . . ? C24 C23 C12 107.6(3) . . ? C27 C26 C31 117.0(4) . . ? C27 C26 C23 119.5(3) . . ? C31 C26 C23 123.4(4) . . ? C28 C27 C26 121.7(4) . . ? C29 C28 C27 120.2(4) . . ? C28 C29 C30 119.7(4) . . ? C29 C30 C31 120.1(4) . . ? C26 C31 C30 121.2(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7X O2 0.94(7) 1.97(7) 2.748(5) 139(6) . O7 H7Y O2 0.81(5) 2.01(5) 2.800(5) 164(4) 6_656 _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 27.18 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.777 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.078 data_ns324 _database_code_depnum_ccdc_archive 'CCDC 893595' #TrackingRef 'web_deposit_cif_file_0_JonathanP.Hill_1343194833.2b_Hill.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 Fe N O7' _chemical_formula_weight 606.50 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.556(2) _cell_length_b 16.496(4) _cell_length_c 38.041(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5996(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.848 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details 'SADABS v2004/1, Sheldrick, G.M., (2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 43888 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.02 _reflns_number_total 6245 _reflns_number_gt 5318 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0474P)^2^+5.3056P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6245 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.002 _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 1.03420(3) 0.208077(18) 0.205058(7) 0.01598(10) Uani 1 1 d . . . O1 O 1.08442(15) 0.21975(9) 0.15829(4) 0.0196(3) Uani 1 1 d . . . C1 C 0.8258(3) 0.34060(14) 0.19629(6) 0.0277(5) Uani 1 1 d . . . H1A H 0.7411 0.3563 0.2086 0.033 Uiso 1 1 calc R . . H1B H 0.8247 0.3670 0.1735 0.033 Uiso 1 1 calc R . . O2 O 0.9446(2) 0.44153(11) 0.22841(6) 0.0469(5) Uani 1 1 d . . . C2 C 0.9513(3) 0.37113(14) 0.21691(6) 0.0283(5) Uani 1 1 d . . . O3 O 1.05526(16) 0.32461(10) 0.22011(4) 0.0284(4) Uani 1 1 d . . . O4 O 1.22254(15) 0.18325(10) 0.22251(4) 0.0234(3) Uani 1 1 d . . . C3 C 0.7258(2) 0.21146(16) 0.21566(5) 0.0254(5) Uani 1 1 d . . . H3A H 0.6941 0.1606 0.2056 0.030 Uiso 1 1 calc R . . H3B H 0.6446 0.2458 0.2192 0.030 Uiso 1 1 calc R . . N1 N 0.82372(18) 0.25159(11) 0.19091(4) 0.0200(4) Uani 1 1 d . . . C4 C 1.2963(2) 0.19527(13) 0.24911(5) 0.0194(4) Uani 1 1 d . . . O5 O 0.92716(15) 0.19218(9) 0.25135(4) 0.0219(3) Uani 1 1 d . . . O6 O 0.98355(18) 0.08975(10) 0.19703(4) 0.0259(4) Uani 1 1 d . . . H6 H 0.931(3) 0.0613(18) 0.2084(7) 0.035(8) Uiso 1 1 d . . . C5 C 1.0637(3) 0.03735(15) 0.17368(6) 0.0301(5) Uani 1 1 d . . . H5A H 1.0761 -0.0153 0.1846 0.036 Uiso 1 1 calc R . . H5B H 1.1556 0.0607 0.1698 0.036 Uiso 1 1 calc R . . C6 C 0.9901(3) 0.02707(15) 0.13888(6) 0.0303(5) Uani 1 1 d . . . H6A H 1.0521 -0.0008 0.1227 0.036 Uiso 1 1 calc R . . H6B H 0.9703 0.0802 0.1291 0.036 Uiso 1 1 calc R . . C7 C 0.8541(3) -0.02030(17) 0.14173(7) 0.0380(6) Uani 1 1 d . . . H7A H 0.8733 -0.0739 0.1503 0.057 Uiso 1 1 calc R . . H7B H 0.8110 -0.0239 0.1190 0.057 Uiso 1 1 calc R . . H7C H 0.7920 0.0069 0.1577 0.057 Uiso 1 1 calc R . . C8 C 0.7863(2) 0.22981(14) 0.15394(5) 0.0200(4) Uani 1 1 d . . . H8A H 0.6922 0.2490 0.1492 0.024 Uiso 1 1 calc R . . H8B H 0.7854 0.1712 0.1518 0.024 Uiso 1 1 calc R . . C9 C 0.8838(2) 0.26399(13) 0.12635(5) 0.0183(4) Uani 1 1 d . . . C10 C 1.0296(2) 0.25446(12) 0.12991(5) 0.0168(4) Uani 1 1 d . . . C11 C 1.1199(2) 0.28133(12) 0.10286(5) 0.0192(4) Uani 1 1 d . . . C12 C 1.0594(2) 0.31404(13) 0.07250(5) 0.0207(4) Uani 1 1 d . . . H12 H 1.1180 0.3302 0.0543 0.025 Uiso 1 1 calc R . . C13 C 0.9153(2) 0.32345(13) 0.06832(5) 0.0203(4) Uani 1 1 d . . . C14 C 0.8299(2) 0.29937(13) 0.09617(5) 0.0198(4) Uani 1 1 d . . . H14 H 0.7337 0.3073 0.0944 0.024 Uiso 1 1 calc R . . C15 C 1.2786(2) 0.27508(14) 0.10888(6) 0.0228(5) Uani 1 1 d . . . C16 C 1.3622(3) 0.30350(17) 0.07648(7) 0.0351(6) Uani 1 1 d . . . H16A H 1.3385 0.2703 0.0566 0.053 Uiso 1 1 calc R . . H16B H 1.4605 0.2989 0.0812 0.053 Uiso 1 1 calc R . . H16C H 1.3395 0.3590 0.0714 0.053 Uiso 1 1 calc R . . C17 C 1.3177(3) 0.33187(14) 0.13941(7) 0.0299(5) Uani 1 1 d . . . H17A H 1.2870 0.3859 0.1341 0.045 Uiso 1 1 calc R . . H17B H 1.4173 0.3316 0.1426 0.045 Uiso 1 1 calc R . . H17C H 1.2731 0.3135 0.1606 0.045 Uiso 1 1 calc R . . C18 C 1.3213(2) 0.18685(14) 0.11605(6) 0.0229(5) Uani 1 1 d . . . C19 C 1.4003(2) 0.16348(15) 0.14519(6) 0.0286(5) Uani 1 1 d . . . H19 H 1.4246 0.2019 0.1620 0.034 Uiso 1 1 calc R . . C20 C 1.4432(3) 0.08367(17) 0.14948(7) 0.0373(6) Uani 1 1 d . . . H20 H 1.4957 0.0693 0.1691 0.045 Uiso 1 1 calc R . . C21 C 1.4084(3) 0.02554(17) 0.12490(8) 0.0415(7) Uani 1 1 d . . . H21 H 1.4394 -0.0276 0.1275 0.050 Uiso 1 1 calc R . . C22 C 1.3276(3) 0.04718(16) 0.09655(7) 0.0383(6) Uani 1 1 d . . . H22 H 1.3014 0.0080 0.0802 0.046 Uiso 1 1 calc R . . C23 C 1.2845(2) 0.12668(15) 0.09202(6) 0.0297(5) Uani 1 1 d . . . H23 H 1.2302 0.1402 0.0726 0.036 Uiso 1 1 calc R . . C24 C 0.8475(2) 0.35682(14) 0.03441(5) 0.0230(5) Uani 1 1 d . . . C25 C 0.9571(3) 0.37557(17) 0.00584(6) 0.0332(6) Uani 1 1 d . . . H25A H 0.9110 0.3967 -0.0146 0.050 Uiso 1 1 calc R . . H25B H 1.0061 0.3267 -0.0002 0.050 Uiso 1 1 calc R . . H25C H 1.0224 0.4149 0.0146 0.050 Uiso 1 1 calc R . . C26 C 0.7498(3) 0.29113(15) 0.01941(6) 0.0304(5) Uani 1 1 d . . . H26A H 0.6782 0.2788 0.0363 0.046 Uiso 1 1 calc R . . H26B H 0.8028 0.2431 0.0145 0.046 Uiso 1 1 calc R . . H26C H 0.7073 0.3106 -0.0018 0.046 Uiso 1 1 calc R . . C27 C 0.7684(2) 0.43571(14) 0.04263(5) 0.0231(5) Uani 1 1 d . . . C28 C 0.6257(3) 0.44584(16) 0.03716(6) 0.0302(5) Uani 1 1 d . . . H28 H 0.5729 0.4027 0.0287 0.036 Uiso 1 1 calc R . . C29 C 0.5608(3) 0.51941(17) 0.04419(7) 0.0396(6) Uani 1 1 d . . . H29 H 0.4651 0.5249 0.0404 0.048 Uiso 1 1 calc R . . C30 C 0.6364(3) 0.58448(17) 0.05676(7) 0.0444(7) Uani 1 1 d . . . H30 H 0.5926 0.6337 0.0613 0.053 Uiso 1 1 calc R . . C31 C 0.7782(3) 0.57532(17) 0.06244(7) 0.0434(7) Uani 1 1 d . . . H31 H 0.8306 0.6187 0.0709 0.052 Uiso 1 1 calc R . . C32 C 0.8427(3) 0.50195(15) 0.05565(6) 0.0325(6) Uani 1 1 d . . . H32 H 0.9382 0.4967 0.0599 0.039 Uiso 1 1 calc R . . O7 O 0.8242(2) 0.00980(12) 0.23908(6) 0.0403(5) Uani 1 1 d . . . H7E H 0.878(5) -0.014(2) 0.2533(11) 0.084(14) Uiso 1 1 d . . . H7D H 0.748(4) -0.009(2) 0.2384(9) 0.063(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01196(16) 0.02220(17) 0.01379(15) 0.00018(11) -0.00027(11) 0.00114(12) O1 0.0153(7) 0.0290(8) 0.0146(7) 0.0036(6) 0.0021(6) 0.0024(6) C1 0.0284(13) 0.0284(13) 0.0262(11) -0.0028(9) -0.0015(10) 0.0107(10) O2 0.0363(11) 0.0286(10) 0.0759(15) -0.0165(10) -0.0062(10) 0.0049(8) C2 0.0287(13) 0.0257(12) 0.0306(12) -0.0020(10) 0.0011(10) 0.0011(10) O3 0.0191(8) 0.0272(9) 0.0388(9) -0.0067(7) -0.0012(7) -0.0003(7) O4 0.0150(7) 0.0381(9) 0.0172(7) -0.0028(6) -0.0033(6) 0.0057(7) C3 0.0133(10) 0.0448(14) 0.0180(10) 0.0055(10) 0.0024(8) -0.0006(10) N1 0.0158(9) 0.0284(10) 0.0159(8) 0.0015(7) 0.0016(7) 0.0003(8) C4 0.0193(11) 0.0223(11) 0.0164(9) 0.0010(8) 0.0006(8) 0.0019(9) O5 0.0140(7) 0.0356(9) 0.0160(7) 0.0002(6) -0.0001(6) 0.0017(6) O6 0.0275(9) 0.0225(8) 0.0276(8) -0.0007(7) 0.0073(7) -0.0038(7) C5 0.0247(12) 0.0276(12) 0.0381(13) -0.0039(10) 0.0030(10) 0.0023(10) C6 0.0356(14) 0.0238(12) 0.0314(12) -0.0016(10) 0.0061(10) -0.0014(10) C7 0.0389(15) 0.0397(15) 0.0355(14) -0.0007(11) -0.0035(12) -0.0091(12) C8 0.0138(10) 0.0311(12) 0.0151(9) 0.0024(8) -0.0013(8) -0.0002(9) C9 0.0180(10) 0.0209(10) 0.0160(9) 0.0006(8) -0.0003(8) -0.0007(8) C10 0.0180(10) 0.0172(10) 0.0154(9) -0.0003(8) 0.0000(8) -0.0001(8) C11 0.0172(10) 0.0198(11) 0.0205(10) -0.0002(8) 0.0014(8) -0.0005(8) C12 0.0209(11) 0.0229(11) 0.0183(10) 0.0029(8) 0.0039(8) -0.0017(9) C13 0.0239(11) 0.0209(11) 0.0160(10) 0.0015(8) -0.0013(8) 0.0012(9) C14 0.0166(10) 0.0245(11) 0.0182(10) -0.0009(8) -0.0007(8) 0.0015(9) C15 0.0152(11) 0.0279(12) 0.0252(11) 0.0044(9) 0.0008(9) -0.0031(9) C16 0.0195(12) 0.0470(16) 0.0388(14) 0.0152(12) 0.0059(10) -0.0029(11) C17 0.0229(12) 0.0252(12) 0.0416(14) 0.0008(10) -0.0055(10) -0.0057(10) C18 0.0124(10) 0.0307(12) 0.0257(11) 0.0007(9) 0.0074(8) -0.0005(9) C19 0.0177(11) 0.0339(13) 0.0342(12) 0.0030(10) -0.0001(10) -0.0013(10) C20 0.0231(13) 0.0423(15) 0.0466(15) 0.0120(12) -0.0013(11) 0.0045(11) C21 0.0269(14) 0.0316(14) 0.0661(19) 0.0041(13) 0.0105(13) 0.0074(11) C22 0.0307(14) 0.0343(14) 0.0501(16) -0.0120(12) 0.0111(12) 0.0010(11) C23 0.0242(12) 0.0367(14) 0.0283(12) -0.0035(10) 0.0048(10) 0.0000(10) C24 0.0234(12) 0.0283(12) 0.0172(10) 0.0041(9) 0.0000(9) 0.0013(9) C25 0.0340(14) 0.0471(15) 0.0184(11) 0.0111(10) 0.0045(10) 0.0081(12) C26 0.0405(14) 0.0310(13) 0.0196(10) 0.0004(9) -0.0067(10) 0.0003(11) C27 0.0283(12) 0.0256(12) 0.0152(9) 0.0079(8) -0.0007(9) -0.0005(9) C28 0.0287(13) 0.0349(14) 0.0271(12) 0.0037(10) -0.0026(10) -0.0005(11) C29 0.0371(15) 0.0480(17) 0.0338(13) 0.0064(12) -0.0003(11) 0.0152(13) C30 0.064(2) 0.0321(15) 0.0375(14) 0.0076(12) 0.0074(14) 0.0174(14) C31 0.061(2) 0.0285(14) 0.0411(15) 0.0017(11) 0.0020(14) -0.0065(13) C32 0.0307(13) 0.0334(14) 0.0334(13) 0.0034(10) -0.0012(10) -0.0047(11) O7 0.0328(11) 0.0411(11) 0.0471(12) 0.0130(9) -0.0006(9) -0.0118(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.8528(14) . ? Fe1 O4 1.9615(15) . ? Fe1 O3 2.0158(17) . ? Fe1 O6 2.0340(17) . ? Fe1 O5 2.0533(15) . ? Fe1 N1 2.2024(18) . ? O1 C10 1.330(2) . ? C1 N1 1.483(3) . ? C1 C2 1.519(3) . ? O2 C2 1.243(3) . ? C2 O3 1.261(3) . ? O4 C4 1.249(2) . ? C3 N1 1.483(3) . ? C3 C4 1.523(3) 6_556 ? N1 C8 1.495(3) . ? C4 O5 1.252(3) 6_656 ? C4 C3 1.523(3) 6_656 ? O5 C4 1.252(3) 6_556 ? O6 C5 1.457(3) . ? C5 C6 1.508(3) . ? C6 C7 1.520(4) . ? C8 C9 1.513(3) . ? C9 C14 1.387(3) . ? C9 C10 1.408(3) . ? C10 C11 1.414(3) . ? C11 C12 1.400(3) . ? C11 C15 1.538(3) . ? C12 C13 1.395(3) . ? C13 C14 1.395(3) . ? C13 C24 1.545(3) . ? C15 C18 1.536(3) . ? C15 C17 1.538(3) . ? C15 C16 1.541(3) . ? C18 C23 1.394(3) . ? C18 C19 1.396(3) . ? C19 C20 1.388(4) . ? C20 C21 1.380(4) . ? C21 C22 1.374(4) . ? C22 C23 1.385(4) . ? C24 C27 1.537(3) . ? C24 C25 1.540(3) . ? C24 C26 1.540(3) . ? C27 C28 1.390(3) . ? C27 C32 1.394(3) . ? C28 C29 1.389(4) . ? C29 C30 1.380(4) . ? C30 C31 1.380(4) . ? C31 C32 1.383(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O4 96.26(6) . . ? O1 Fe1 O3 98.50(7) . . ? O4 Fe1 O3 90.65(7) . . ? O1 Fe1 O6 90.99(7) . . ? O4 Fe1 O6 93.94(7) . . ? O3 Fe1 O6 168.95(7) . . ? O1 Fe1 O5 164.99(6) . . ? O4 Fe1 O5 98.05(6) . . ? O3 Fe1 O5 85.86(7) . . ? O6 Fe1 O5 83.55(6) . . ? O1 Fe1 N1 88.16(6) . . ? O4 Fe1 N1 171.38(7) . . ? O3 Fe1 N1 81.36(7) . . ? O6 Fe1 N1 93.37(7) . . ? O5 Fe1 N1 78.25(6) . . ? C10 O1 Fe1 136.24(13) . . ? N1 C1 C2 114.20(19) . . ? O2 C2 O3 125.1(2) . . ? O2 C2 C1 116.8(2) . . ? O3 C2 C1 118.0(2) . . ? C2 O3 Fe1 118.31(15) . . ? C4 O4 Fe1 139.35(14) . . ? N1 C3 C4 110.97(18) . 6_556 ? C1 N1 C3 111.26(18) . . ? C1 N1 C8 111.78(17) . . ? C3 N1 C8 109.81(17) . . ? C1 N1 Fe1 106.08(13) . . ? C3 N1 Fe1 105.99(13) . . ? C8 N1 Fe1 111.73(13) . . ? O4 C4 O5 123.07(19) . 6_656 ? O4 C4 C3 119.42(18) . 6_656 ? O5 C4 C3 117.47(18) 6_656 6_656 ? C4 O5 Fe1 118.70(13) 6_556 . ? C5 O6 Fe1 122.39(14) . . ? O6 C5 C6 110.89(19) . . ? C5 C6 C7 113.2(2) . . ? N1 C8 C9 114.55(17) . . ? C14 C9 C10 119.62(19) . . ? C14 C9 C8 120.12(19) . . ? C10 C9 C8 120.07(18) . . ? O1 C10 C9 121.08(18) . . ? O1 C10 C11 119.02(18) . . ? C9 C10 C11 119.90(18) . . ? C12 C11 C10 117.99(19) . . ? C12 C11 C15 123.77(19) . . ? C10 C11 C15 118.21(18) . . ? C13 C12 C11 122.99(19) . . ? C12 C13 C14 117.36(19) . . ? C12 C13 C24 123.27(19) . . ? C14 C13 C24 119.35(19) . . ? C9 C14 C13 122.0(2) . . ? C18 C15 C11 110.59(17) . . ? C18 C15 C17 112.26(18) . . ? C11 C15 C17 108.11(18) . . ? C18 C15 C16 107.03(18) . . ? C11 C15 C16 111.82(18) . . ? C17 C15 C16 107.02(19) . . ? C23 C18 C19 117.4(2) . . ? C23 C18 C15 119.4(2) . . ? C19 C18 C15 123.1(2) . . ? C20 C19 C18 121.0(2) . . ? C21 C20 C19 120.6(3) . . ? C22 C21 C20 119.1(2) . . ? C21 C22 C23 120.7(3) . . ? C22 C23 C18 121.2(2) . . ? C27 C24 C25 107.92(18) . . ? C27 C24 C26 111.88(19) . . ? C25 C24 C26 107.00(19) . . ? C27 C24 C13 109.75(17) . . ? C25 C24 C13 112.08(19) . . ? C26 C24 C13 108.23(18) . . ? C28 C27 C32 117.3(2) . . ? C28 C27 C24 123.6(2) . . ? C32 C27 C24 119.0(2) . . ? C29 C28 C27 121.0(2) . . ? C30 C29 C28 120.8(3) . . ? C29 C30 C31 118.9(3) . . ? C30 C31 C32 120.3(3) . . ? C31 C32 C27 121.7(3) . . ? 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 O7 H7D O2 0.80(4) 2.05(4) 2.834(3) 171(4) 8_755 O6 H6 O7 0.81(3) 1.77(3) 2.572(3) 171(3) . O7 H7E O2 0.85(4) 1.97(4) 2.771(3) 158(4) 3_745 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.02 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.506 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.065 data_ns443_patterson _database_code_depnum_ccdc_archive 'CCDC 906345' #TrackingRef 'web_deposit_cif_file_0_JonathanP.Hill_1350463268.7_Hill.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H37 Fe N O8' _chemical_formula_weight 607.47 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.4671(10) _cell_length_b 16.4024(17) _cell_length_c 37.998(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5900.4(11) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.869 _exptl_absorpt_correction_T_max 0.972 _exptl_absorpt_process_details 'SADABS v2004/1, Sheldrick, G.M., (2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 32741 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 26.73 _reflns_number_total 6245 _reflns_number_gt 4108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0475P)^2^+5.8273P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6245 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _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 0.52191(4) 0.30033(3) 0.795302(11) 0.02959(13) Uani 1 1 d . . . O1 O 0.5746(2) 0.29324(13) 0.84211(5) 0.0339(5) Uani 1 1 d . . . C1 C 0.2753(3) 0.2737(2) 0.84659(8) 0.0351(7) Uani 1 1 d . . . H1A H 0.1820 0.2523 0.8516 0.042 Uiso 1 1 calc R . . H1B H 0.2712 0.3325 0.8493 0.042 Uiso 1 1 calc R . . C2 C 0.3117(4) 0.1660(2) 0.80248(10) 0.0494(9) Uani 1 1 d . . . H2A H 0.2313 0.1527 0.7877 0.059 Uiso 1 1 calc R . . H2B H 0.2996 0.1376 0.8247 0.059 Uiso 1 1 calc R . . N1 N 0.3114(3) 0.25460(16) 0.80931(6) 0.0330(6) Uani 1 1 d . . . C3 C 0.4438(4) 0.1347(2) 0.78495(10) 0.0472(9) Uani 1 1 d . . . O2 O 0.5492(2) 0.18264(14) 0.78281(7) 0.0476(6) Uani 1 1 d . . . O3 O 0.4438(3) 0.06438(17) 0.77387(9) 0.0798(10) Uani 1 1 d . . . C4 C 0.2131(3) 0.2970(2) 0.78529(8) 0.0426(8) Uani 1 1 d . . . H4A H 0.1854 0.3488 0.7955 0.051 Uiso 1 1 calc R . . H4B H 0.1286 0.2643 0.7822 0.051 Uiso 1 1 calc R . . C5 C 0.2821(3) 0.31159(19) 0.74990(8) 0.0338(7) Uani 1 1 d . . . O4 O 0.4138(2) 0.31250(13) 0.74906(5) 0.0375(5) Uani 1 1 d . . . O5 O 0.4656(2) 0.42024(13) 0.80177(6) 0.0436(6) Uani 1 1 d . . . C6 C 0.5352(4) 0.4778(2) 0.82475(10) 0.0562(10) Uani 1 1 d . . . H6A H 0.5368 0.5309 0.8135 0.067 Uiso 1 1 calc R . . H6B H 0.6321 0.4607 0.8284 0.067 Uiso 1 1 calc R . . C7 C 0.4638(5) 0.4844(3) 0.85891(11) 0.0648(12) Uani 1 1 d . . . H7A H 0.4562 0.4309 0.8696 0.078 Uiso 1 1 calc R . . H7B H 0.5184 0.5190 0.8745 0.078 Uiso 1 1 calc R . . O6 O 0.3280(4) 0.5177(3) 0.85416(9) 0.1082(14) Uani 1 1 d . . . H6 H 0.2846 0.5160 0.8728 0.162 Uiso 1 1 calc R . . O7 O 0.7080(2) 0.32582(14) 0.77644(5) 0.0392(5) Uani 1 1 d . . . C8 C 0.3777(3) 0.23995(18) 0.87340(7) 0.0294(7) Uani 1 1 d . . . C9 C 0.5238(3) 0.25337(17) 0.86973(7) 0.0294(6) Uani 1 1 d . . . C10 C 0.6176(3) 0.22671(18) 0.89609(8) 0.0297(7) Uani 1 1 d . . . C11 C 0.5602(3) 0.19046(19) 0.92613(8) 0.0350(7) Uani 1 1 d . . . H11 H 0.6210 0.1740 0.9440 0.042 Uiso 1 1 calc R . . C12 C 0.4156(3) 0.17783(18) 0.93047(8) 0.0327(7) Uani 1 1 d . . . C13 C 0.3269(3) 0.20097(19) 0.90308(8) 0.0338(7) Uani 1 1 d . . . H13 H 0.2307 0.1899 0.9048 0.041 Uiso 1 1 calc R . . C14 C 0.7766(3) 0.23610(19) 0.88976(8) 0.0351(7) Uani 1 1 d . . . C15 C 0.8180(4) 0.1800(2) 0.85874(10) 0.0484(9) Uani 1 1 d . . . H15A H 0.7703 0.1977 0.8378 0.073 Uiso 1 1 calc R . . H15B H 0.7912 0.1249 0.8640 0.073 Uiso 1 1 calc R . . H15C H 0.9183 0.1826 0.8551 0.073 Uiso 1 1 calc R . . C16 C 0.8639(4) 0.2085(2) 0.92189(10) 0.0561(10) Uani 1 1 d . . . H16A H 0.9626 0.2167 0.9172 0.084 Uiso 1 1 calc R . . H16B H 0.8468 0.1518 0.9263 0.084 Uiso 1 1 calc R . . H16C H 0.8368 0.2399 0.9421 0.084 Uiso 1 1 calc R . . C17 C 0.8159(3) 0.3253(2) 0.88265(9) 0.0366(7) Uani 1 1 d . . . C18 C 0.8933(4) 0.3502(2) 0.85365(10) 0.0474(9) Uani 1 1 d . . . H18 H 0.9188 0.3120 0.8367 0.057 Uiso 1 1 calc R . . C19 C 0.9337(4) 0.4309(3) 0.84930(12) 0.0630(11) Uani 1 1 d . . . H19 H 0.9860 0.4460 0.8296 0.076 Uiso 1 1 calc R . . C20 C 0.8972(4) 0.4879(3) 0.87365(14) 0.0678(13) Uani 1 1 d . . . H20 H 0.9261 0.5418 0.8709 0.081 Uiso 1 1 calc R . . C21 C 0.8172(4) 0.4655(2) 0.90234(12) 0.0637(12) Uani 1 1 d . . . H21 H 0.7900 0.5044 0.9188 0.076 Uiso 1 1 calc R . . C22 C 0.7771(4) 0.3847(2) 0.90665(10) 0.0488(9) Uani 1 1 d . . . H22 H 0.7231 0.3701 0.9261 0.059 Uiso 1 1 calc R . . C23 C 0.3499(3) 0.14243(19) 0.96435(8) 0.0369(7) Uani 1 1 d . . . C24 C 0.4617(4) 0.1210(3) 0.99202(9) 0.0552(10) Uani 1 1 d . . . H24A H 0.5105 0.1696 0.9991 0.083 Uiso 1 1 calc R . . H24B H 0.5281 0.0830 0.9822 0.083 Uiso 1 1 calc R . . H24C H 0.4167 0.0969 1.0121 0.083 Uiso 1 1 calc R . . C25 C 0.2539(4) 0.2085(2) 0.98052(9) 0.0530(10) Uani 1 1 d . . . H25A H 0.1809 0.2225 0.9641 0.079 Uiso 1 1 calc R . . H25B H 0.3091 0.2561 0.9858 0.079 Uiso 1 1 calc R . . H25C H 0.2119 0.1881 1.0018 0.079 Uiso 1 1 calc R . . C26 C 0.2680(4) 0.0644(2) 0.95535(8) 0.0375(8) Uani 1 1 d . . . C27 C 0.3379(4) -0.0004(2) 0.94020(10) 0.0540(10) Uani 1 1 d . . . H27 H 0.4329 0.0054 0.9345 0.065 Uiso 1 1 calc R . . C28 C 0.2715(6) -0.0735(3) 0.93318(11) 0.0681(12) Uani 1 1 d . . . H28 H 0.3222 -0.1163 0.9232 0.082 Uiso 1 1 calc R . . C29 C 0.1312(6) -0.0833(3) 0.94092(12) 0.0721(13) Uani 1 1 d . . . H29 H 0.0860 -0.1327 0.9366 0.087 Uiso 1 1 calc R . . C30 C 0.0590(5) -0.0192(3) 0.95502(11) 0.0699(13) Uani 1 1 d . . . H30 H -0.0369 -0.0247 0.9597 0.084 Uiso 1 1 calc R . . C31 C 0.1259(4) 0.0540(2) 0.96247(10) 0.0543(10) Uani 1 1 d . . . H31 H 0.0746 0.0966 0.9724 0.065 Uiso 1 1 calc R . . O8 O 0.3188(4) 0.49580(19) 0.75646(10) 0.0678(9) Uani 1 1 d . . . H8B H 0.372(8) 0.524(4) 0.7346(19) 0.18(3) Uiso 1 1 d . . . H8A H 0.247(7) 0.514(4) 0.7609(16) 0.12(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0232(2) 0.0403(2) 0.0253(2) 0.00095(19) 0.00087(18) -0.00100(19) O1 0.0268(11) 0.0513(13) 0.0235(11) 0.0063(10) -0.0009(8) -0.0045(10) C1 0.0230(16) 0.053(2) 0.0289(17) 0.0036(14) 0.0032(12) 0.0035(14) C2 0.050(2) 0.050(2) 0.048(2) -0.0051(17) 0.0044(17) -0.0155(17) N1 0.0267(13) 0.0452(16) 0.0271(13) 0.0018(12) -0.0023(11) -0.0003(11) C3 0.045(2) 0.041(2) 0.055(2) -0.0033(17) -0.0056(17) 0.0005(16) O2 0.0349(13) 0.0417(14) 0.0663(17) -0.0095(12) 0.0001(11) 0.0008(10) O3 0.063(2) 0.0455(17) 0.131(3) -0.0266(17) 0.0095(19) -0.0057(14) C4 0.0240(15) 0.074(2) 0.0295(17) 0.0078(16) -0.0031(12) -0.0010(17) C5 0.0292(16) 0.0431(18) 0.0290(16) -0.0003(15) -0.0017(13) -0.0026(14) O4 0.0281(12) 0.0581(14) 0.0262(11) 0.0023(10) -0.0006(9) -0.0013(10) O5 0.0501(14) 0.0378(12) 0.0429(14) -0.0052(10) -0.0054(11) 0.0020(11) C6 0.058(2) 0.049(2) 0.061(3) -0.0074(19) -0.006(2) -0.0033(19) C7 0.084(3) 0.053(2) 0.058(3) -0.008(2) -0.007(2) -0.001(2) O6 0.111(3) 0.133(3) 0.080(3) 0.022(2) 0.031(2) 0.063(3) O7 0.0285(11) 0.0633(15) 0.0257(11) -0.0045(10) 0.0066(9) -0.0067(10) C8 0.0268(15) 0.0369(16) 0.0244(16) 0.0014(13) -0.0027(12) 0.0017(13) C9 0.0332(15) 0.0319(16) 0.0229(15) 0.0016(12) -0.0009(13) -0.0002(13) C10 0.0275(16) 0.0338(16) 0.0278(16) -0.0009(13) -0.0005(12) 0.0033(12) C11 0.0382(18) 0.0350(17) 0.0319(17) 0.0041(14) -0.0090(13) 0.0022(14) C12 0.0364(17) 0.0352(17) 0.0264(16) 0.0041(13) -0.0001(13) -0.0009(13) C13 0.0274(16) 0.0456(18) 0.0284(16) 0.0021(14) -0.0003(12) -0.0021(14) C14 0.0276(16) 0.0417(18) 0.0359(18) 0.0031(14) -0.0013(13) 0.0043(14) C15 0.0349(19) 0.044(2) 0.066(3) -0.0051(18) 0.0088(17) 0.0047(15) C16 0.0312(19) 0.073(3) 0.064(3) 0.018(2) -0.0127(17) 0.0049(18) C17 0.0252(16) 0.0429(19) 0.0417(19) -0.0011(15) -0.0074(14) 0.0009(13) C18 0.037(2) 0.053(2) 0.052(2) 0.0013(17) 0.0042(17) 0.0016(17) C19 0.046(2) 0.058(3) 0.085(3) 0.018(2) 0.005(2) -0.0045(19) C20 0.050(3) 0.044(2) 0.109(4) 0.006(2) -0.015(3) -0.0080(19) C21 0.054(3) 0.052(2) 0.085(3) -0.022(2) -0.011(2) 0.001(2) C22 0.041(2) 0.055(2) 0.050(2) -0.0097(18) -0.0035(17) -0.0016(17) C23 0.0410(19) 0.0412(18) 0.0285(17) 0.0069(14) 0.0013(14) -0.0015(15) C24 0.059(2) 0.072(3) 0.034(2) 0.0188(18) -0.0091(18) -0.012(2) C25 0.072(3) 0.052(2) 0.035(2) -0.0008(17) 0.0121(18) -0.0022(19) C26 0.044(2) 0.0428(19) 0.0258(16) 0.0092(14) -0.0018(14) -0.0018(15) C27 0.054(2) 0.053(2) 0.055(2) 0.0007(19) 0.0011(19) 0.0028(19) C28 0.092(4) 0.048(2) 0.064(3) -0.003(2) -0.005(3) 0.006(2) C29 0.100(4) 0.054(3) 0.063(3) 0.005(2) -0.007(3) -0.022(3) C30 0.062(3) 0.086(3) 0.062(3) 0.006(2) 0.005(2) -0.028(3) C31 0.052(2) 0.062(3) 0.050(2) 0.0015(19) 0.0051(18) -0.0073(19) O8 0.070(2) 0.0592(19) 0.075(2) 0.0104(16) -0.0033(18) 0.0191(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.851(2) . ? Fe1 O7 1.948(2) . ? Fe1 O2 2.005(2) . ? Fe1 O4 2.043(2) . ? Fe1 O5 2.053(2) . ? Fe1 N1 2.195(3) . ? O1 C9 1.327(3) . ? C1 N1 1.490(4) . ? C1 C8 1.511(4) . ? C2 N1 1.477(4) . ? C2 C3 1.506(5) . ? N1 C4 1.477(4) . ? C3 O3 1.229(4) . ? C3 O2 1.273(4) . ? C4 C5 1.514(4) . ? C5 O7 1.244(3) 6_557 ? C5 O4 1.247(4) . ? O5 C6 1.444(4) . ? C6 C7 1.468(6) . ? C7 O6 1.408(5) . ? O7 C5 1.244(3) 6_657 ? C8 C13 1.383(4) . ? C8 C9 1.407(4) . ? C9 C10 1.409(4) . ? C10 C11 1.397(4) . ? C10 C14 1.532(4) . ? C11 C12 1.394(4) . ? C12 C13 1.390(4) . ? C12 C23 1.543(4) . ? C14 C17 1.534(4) . ? C14 C16 1.542(4) . ? C14 C15 1.546(5) . ? C17 C22 1.384(5) . ? C17 C18 1.385(5) . ? C18 C19 1.388(5) . ? C19 C20 1.361(6) . ? C20 C21 1.377(6) . ? C21 C22 1.388(5) . ? C23 C24 1.533(5) . ? C23 C26 1.536(4) . ? C23 C25 1.542(5) . ? C26 C27 1.377(5) . ? C26 C31 1.383(5) . ? C27 C28 1.381(5) . ? C28 C29 1.370(6) . ? C29 C30 1.363(6) . ? C30 C31 1.387(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O7 97.08(9) . . ? O1 Fe1 O2 97.61(10) . . ? O7 Fe1 O2 90.18(10) . . ? O1 Fe1 O4 165.35(9) . . ? O7 Fe1 O4 96.65(9) . . ? O2 Fe1 O4 87.42(10) . . ? O1 Fe1 O5 90.86(9) . . ? O7 Fe1 O5 94.20(10) . . ? O2 Fe1 O5 169.92(10) . . ? O4 Fe1 O5 83.07(9) . . ? O1 Fe1 N1 89.43(9) . . ? O7 Fe1 N1 169.76(9) . . ? O2 Fe1 N1 81.10(10) . . ? O4 Fe1 N1 77.71(9) . . ? O5 Fe1 N1 93.59(10) . . ? C9 O1 Fe1 133.90(19) . . ? N1 C1 C8 114.6(2) . . ? N1 C2 C3 114.5(3) . . ? C2 N1 C4 110.9(3) . . ? C2 N1 C1 112.0(3) . . ? C4 N1 C1 110.1(2) . . ? C2 N1 Fe1 106.95(19) . . ? C4 N1 Fe1 105.15(18) . . ? C1 N1 Fe1 111.49(18) . . ? O3 C3 O2 123.9(4) . . ? O3 C3 C2 118.1(3) . . ? O2 C3 C2 118.0(3) . . ? C3 O2 Fe1 118.6(2) . . ? N1 C4 C5 110.6(3) . . ? O7 C5 O4 122.7(3) 6_557 . ? O7 C5 C4 120.1(3) 6_557 . ? O4 C5 C4 117.1(3) . . ? C5 O4 Fe1 118.5(2) . . ? C6 O5 Fe1 125.5(2) . . ? O5 C6 C7 111.9(3) . . ? O6 C7 C6 109.6(4) . . ? C5 O7 Fe1 140.0(2) 6_657 . ? C13 C8 C9 119.7(3) . . ? C13 C8 C1 119.8(3) . . ? C9 C8 C1 120.4(3) . . ? O1 C9 C8 120.8(3) . . ? O1 C9 C10 119.1(3) . . ? C8 C9 C10 120.1(3) . . ? C11 C10 C9 117.9(3) . . ? C11 C10 C14 123.6(3) . . ? C9 C10 C14 118.5(3) . . ? C12 C11 C10 122.8(3) . . ? C13 C12 C11 117.7(3) . . ? C13 C12 C23 118.9(3) . . ? C11 C12 C23 123.4(3) . . ? C8 C13 C12 121.8(3) . . ? C10 C14 C17 111.2(2) . . ? C10 C14 C16 111.9(3) . . ? C17 C14 C16 106.8(3) . . ? C10 C14 C15 108.0(3) . . ? C17 C14 C15 111.8(3) . . ? C16 C14 C15 107.1(3) . . ? C22 C17 C18 117.2(3) . . ? C22 C17 C14 119.4(3) . . ? C18 C17 C14 123.3(3) . . ? C17 C18 C19 121.4(4) . . ? C20 C19 C18 120.3(4) . . ? C19 C20 C21 119.6(4) . . ? C20 C21 C22 119.9(4) . . ? C17 C22 C21 121.5(4) . . ? C24 C23 C26 108.1(3) . . ? C24 C23 C25 107.2(3) . . ? C26 C23 C25 112.1(3) . . ? C24 C23 C12 112.4(3) . . ? C26 C23 C12 109.4(3) . . ? C25 C23 C12 107.8(3) . . ? C27 C26 C31 117.0(3) . . ? C27 C26 C23 119.6(3) . . ? C31 C26 C23 123.4(3) . . ? C26 C27 C28 122.2(4) . . ? C29 C28 C27 120.1(4) . . ? C30 C29 C28 118.7(4) . . ? C29 C30 C31 121.3(4) . . ? C26 C31 C30 120.7(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8B O3 1.08(8) 1.89(7) 2.766(5) 136(5) 3_656 O8 H8A O3 0.76(6) 2.05(6) 2.807(5) 179(7) 8_665 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.467 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.060