# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author 'Annie K. Powell' _publ_contact_author_address ; Inst fuer Anorganische Chemie Universitaet Karlsruhe Engesserstrasse Geb. 30.45 Karlsruhe D76128 GERMANY ; _publ_contact_author_email powell@chemie.uni-karlsruhe.de _publ_contact_author_phone '+44 721 608 2135' _publ_section_title ; Enhancing Single Molecule Magnet Parameters. Synthesis, Crystal structures and Magnetic Properties of Mixed-valent Mn4 SMMs. ; loop_ _publ_author_name _publ_author_address 'Ayuk M. Ako' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Valeriu Mereacre' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Ian J. Hewitt' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Rodolphe Clerac' ; Centre de Recherche Paul Pascal CNRS UPR 8641 Avenur Dr. A. Schweitzer 33600 Pessac France ; 'Lollita Lecren' ; Centre de Recherche Paul Pascal CNRS UPR 8641 Avenur Dr. A. Schweitzer 33600 Pessac France ; 'Christopher E. Anson' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; ; A.K.Powell ; ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; _publ_contact_author_name 'Annie K. Powell' data_a196b _database_code_depnum_ccdc_archive 'CCDC 600737' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H106 Mn4 N4 O16' _chemical_formula_weight 1263.17 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 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2125(7) _cell_length_b 10.9602(6) _cell_length_c 22.4329(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.053(1) _cell_angle_gamma 90.00 _cell_volume 3235.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9992 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.89 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.781 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15880 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.99 _reflns_number_total 7254 _reflns_number_gt 5927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _refine_special_details ; Coordinates of O-H H atoms refined; organic C-H H atoms in calculated positions. 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^)+(0.0476P)^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 7254 _refine_ls_number_parameters 346 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _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 0.386870(15) 0.494138(18) 0.470619(9) 0.01521(6) Uani 1 1 d . . . Mn2 Mn 0.449975(15) 0.379312(19) 0.609594(9) 0.01723(6) Uani 1 1 d . . . N1 N 0.31291(9) 0.30955(11) 0.43212(5) 0.0203(3) Uani 1 1 d . . . C1 C 0.37804(11) 0.21770(13) 0.46557(7) 0.0229(3) Uani 1 1 d . . . H1A H 0.3779 0.1411 0.4421 0.027 Uiso 1 1 calc R . . H1B H 0.3500 0.1995 0.5041 0.027 Uiso 1 1 calc R . . C2 C 0.48646(10) 0.26396(13) 0.47747(6) 0.0203(3) Uani 1 1 d . . . H2A H 0.5277 0.2040 0.5020 0.024 Uiso 1 1 calc R . . H2B H 0.5173 0.2748 0.4392 0.024 Uiso 1 1 calc R . . O1 O 0.48492(7) 0.37789(8) 0.50835(4) 0.0171(2) Uani 1 1 d . . . C3 C 0.33181(11) 0.31014(14) 0.36758(6) 0.0236(3) Uani 1 1 d . . . H3A H 0.2692 0.2859 0.3430 0.028 Uiso 1 1 calc R . . H3B H 0.3858 0.2506 0.3605 0.028 Uiso 1 1 calc R . . C4 C 0.36404(11) 0.43657(14) 0.34964(6) 0.0228(3) Uani 1 1 d . . . H4A H 0.3917 0.4337 0.3101 0.027 Uiso 1 1 calc R . . H4B H 0.3050 0.4925 0.3470 0.027 Uiso 1 1 calc R . . O2 O 0.44018(7) 0.47866(9) 0.39424(4) 0.0182(2) Uani 1 1 d . . . C5 C 0.20485(11) 0.28799(14) 0.44219(7) 0.0251(3) Uani 1 1 d . . . H5A H 0.1987 0.2830 0.4858 0.030 Uiso 1 1 calc R . . H5B H 0.1835 0.2084 0.4244 0.030 Uiso 1 1 calc R . . C6 C 0.13370(11) 0.38580(15) 0.41589(8) 0.0313(4) Uani 1 1 d . . . H6A H 0.1333 0.3841 0.3717 0.038 Uiso 1 1 calc R . . H6B H 0.1594 0.4666 0.4299 0.038 Uiso 1 1 calc R . . C7 C 0.02433(12) 0.36988(16) 0.43307(9) 0.0382(4) Uani 1 1 d . . . H7A H 0.0254 0.3682 0.4773 0.046 Uiso 1 1 calc R . . H7B H -0.0163 0.4415 0.4186 0.046 Uiso 1 1 calc R . . C8 C -0.02750(13) 0.25517(19) 0.40802(11) 0.0540(6) Uani 1 1 d . . . H8A H -0.0963 0.2505 0.4210 0.081 Uiso 1 1 calc R . . H8B H 0.0115 0.1835 0.4226 0.081 Uiso 1 1 calc R . . H8C H -0.0313 0.2573 0.3642 0.081 Uiso 1 1 calc R . . N2 N 0.33574(9) 0.48990(11) 0.66871(5) 0.0208(3) Uani 1 1 d . . . C9 C 0.31077(12) 0.60225(14) 0.63399(7) 0.0248(3) Uani 1 1 d . . . H9A H 0.3725 0.6532 0.6333 0.030 Uiso 1 1 calc R . . H9B H 0.2594 0.6497 0.6537 0.030 Uiso 1 1 calc R . . C10 C 0.26980(11) 0.57230(14) 0.57030(6) 0.0239(3) Uani 1 1 d . . . H10A H 0.2007 0.5371 0.5700 0.029 Uiso 1 1 calc R . . H10B H 0.2656 0.6475 0.5457 0.029 Uiso 1 1 calc R . . O3 O 0.33611(7) 0.48720(8) 0.54628(4) 0.0185(2) Uani 1 1 d . . . C11 C 0.39613(12) 0.51917(14) 0.72545(6) 0.0248(3) Uani 1 1 d . . . H11A H 0.3514 0.5567 0.7535 0.030 Uiso 1 1 calc R . . H11B H 0.4494 0.5792 0.7177 0.030 Uiso 1 1 calc R . . C12 C 0.44527(12) 0.40676(15) 0.75374(7) 0.0281(3) Uani 1 1 d . . . H12A H 0.4911 0.4301 0.7892 0.034 Uiso 1 1 calc R . . H12B H 0.3924 0.3517 0.7671 0.034 Uiso 1 1 calc R . . O4 O 0.50201(8) 0.34485(10) 0.71128(5) 0.0252(2) Uani 1 1 d D . . H4 H 0.4812(13) 0.2718(16) 0.7101(8) 0.030 Uiso 1 1 d D . . C13 C 0.24495(11) 0.41473(14) 0.67733(7) 0.0239(3) Uani 1 1 d . . . H13A H 0.2678 0.3389 0.6984 0.029 Uiso 1 1 calc R . . H13B H 0.2131 0.3910 0.6374 0.029 Uiso 1 1 calc R . . C14 C 0.16366(12) 0.47418(17) 0.71214(8) 0.0347(4) Uani 1 1 d . . . H14A H 0.1956 0.5045 0.7509 0.042 Uiso 1 1 calc R . . H14B H 0.1347 0.5452 0.6893 0.042 Uiso 1 1 calc R . . C15 C 0.07836(13) 0.3862(2) 0.72371(9) 0.0459(5) Uani 1 1 d . . . H15A H 0.0450 0.3579 0.6849 0.055 Uiso 1 1 calc R . . H15B H 0.1075 0.3140 0.7455 0.055 Uiso 1 1 calc R . . C16 C -0.00078(15) 0.4445(3) 0.76003(10) 0.0620(6) Uani 1 1 d . . . H16A H -0.0550 0.3856 0.7654 0.093 Uiso 1 1 calc R . . H16B H -0.0296 0.5165 0.7388 0.093 Uiso 1 1 calc R . . H16C H 0.0312 0.4691 0.7993 0.093 Uiso 1 1 calc R . . O5 O 0.70436(7) 0.37513(9) 0.55709(4) 0.0193(2) Uani 1 1 d . . . O6 O 0.59928(7) 0.26134(9) 0.60855(4) 0.0230(2) Uani 1 1 d . . . C17 C 0.68342(11) 0.28425(13) 0.59126(6) 0.0204(3) Uani 1 1 d . . . C18 C 0.77495(11) 0.20407(14) 0.61273(7) 0.0249(3) Uani 1 1 d . . . C19 C 0.74169(13) 0.07092(15) 0.61305(8) 0.0342(4) Uani 1 1 d . . . H19A H 0.7999 0.0195 0.6267 0.051 Uiso 1 1 calc R . . H19B H 0.7158 0.0466 0.5725 0.051 Uiso 1 1 calc R . . H19C H 0.6880 0.0610 0.6402 0.051 Uiso 1 1 calc R . . C20 C 0.80803(14) 0.24746(17) 0.67677(8) 0.0394(4) Uani 1 1 d . . . H20A H 0.8288 0.3332 0.6758 0.059 Uiso 1 1 calc R . . H20B H 0.8653 0.1978 0.6936 0.059 Uiso 1 1 calc R . . H20C H 0.7511 0.2390 0.7017 0.059 Uiso 1 1 calc R . . C21 C 0.86367(13) 0.21882(18) 0.57366(10) 0.0469(5) Uani 1 1 d . . . H21A H 0.8845 0.3046 0.5735 0.070 Uiso 1 1 calc R . . H21B H 0.8423 0.1928 0.5327 0.070 Uiso 1 1 calc R . . H21C H 0.9209 0.1685 0.5899 0.070 Uiso 1 1 calc R . . O7 O 0.36571(7) 0.21503(9) 0.60867(4) 0.0218(2) Uani 1 1 d . . . O8 O 0.40450(8) 0.13732(10) 0.70024(5) 0.0313(3) Uani 1 1 d . . . C22 C 0.35746(11) 0.13518(13) 0.64930(7) 0.0224(3) Uani 1 1 d . . . C23 C 0.28423(12) 0.02874(14) 0.63305(7) 0.0264(3) Uani 1 1 d . . . C24 C 0.26447(13) -0.04627(16) 0.68868(7) 0.0320(4) Uani 1 1 d . . . H24A H 0.3291 -0.0775 0.7075 0.048 Uiso 1 1 calc R . . H24B H 0.2195 -0.1148 0.6769 0.048 Uiso 1 1 calc R . . H24C H 0.2323 0.0056 0.7171 0.048 Uiso 1 1 calc R . . C25 C 0.18288(13) 0.07889(17) 0.60411(9) 0.0417(5) Uani 1 1 d . . . H25A H 0.1953 0.1271 0.5687 0.063 Uiso 1 1 calc R . . H25B H 0.1514 0.1307 0.6329 0.063 Uiso 1 1 calc R . . H25C H 0.1373 0.0108 0.5923 0.063 Uiso 1 1 calc R . . C26 C 0.33470(15) -0.05258(15) 0.58841(8) 0.0376(4) Uani 1 1 d . . . H26A H 0.3993 -0.0838 0.6072 0.056 Uiso 1 1 calc R . . H26B H 0.3473 -0.0047 0.5529 0.056 Uiso 1 1 calc R . . H26C H 0.2897 -0.1211 0.5766 0.056 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 0.01557(11) 0.01723(11) 0.01314(11) -0.00020(8) 0.00300(8) -0.00048(8) Mn2 0.01784(11) 0.01858(12) 0.01562(11) 0.00093(8) 0.00348(8) -0.00195(8) N1 0.0189(6) 0.0246(6) 0.0177(6) -0.0004(5) 0.0035(5) -0.0035(5) C1 0.0267(8) 0.0197(8) 0.0223(7) -0.0018(6) 0.0020(6) -0.0025(6) C2 0.0217(7) 0.0187(7) 0.0208(7) -0.0036(6) 0.0030(5) 0.0015(6) O1 0.0181(5) 0.0162(5) 0.0173(5) -0.0011(4) 0.0029(4) 0.0005(4) C3 0.0247(7) 0.0284(8) 0.0176(7) -0.0049(6) 0.0016(6) -0.0044(6) C4 0.0224(7) 0.0304(8) 0.0154(7) -0.0031(6) 0.0012(6) -0.0044(6) O2 0.0179(5) 0.0226(5) 0.0141(5) -0.0015(4) 0.0022(4) -0.0033(4) C5 0.0221(7) 0.0277(8) 0.0262(8) -0.0020(6) 0.0052(6) -0.0065(6) C6 0.0228(8) 0.0297(9) 0.0417(10) 0.0001(7) 0.0037(7) -0.0046(7) C7 0.0242(8) 0.0379(10) 0.0532(12) -0.0046(8) 0.0067(8) -0.0003(7) C8 0.0258(9) 0.0455(12) 0.0906(17) -0.0096(11) 0.0048(10) -0.0054(9) N2 0.0231(6) 0.0243(7) 0.0153(6) -0.0005(5) 0.0040(5) -0.0033(5) C9 0.0297(8) 0.0230(8) 0.0227(8) -0.0015(6) 0.0084(6) 0.0029(6) C10 0.0237(7) 0.0277(8) 0.0213(7) 0.0010(6) 0.0079(6) 0.0070(6) O3 0.0198(5) 0.0203(5) 0.0162(5) 0.0000(4) 0.0062(4) 0.0029(4) C11 0.0250(7) 0.0319(9) 0.0182(7) -0.0050(6) 0.0054(6) -0.0053(6) C12 0.0272(8) 0.0400(10) 0.0172(7) 0.0004(6) 0.0034(6) -0.0069(7) O4 0.0277(6) 0.0258(6) 0.0223(5) 0.0017(4) 0.0023(4) -0.0041(5) C13 0.0233(7) 0.0283(8) 0.0206(7) -0.0014(6) 0.0056(6) -0.0035(6) C14 0.0276(9) 0.0430(10) 0.0354(10) -0.0077(8) 0.0134(7) -0.0045(7) C15 0.0316(9) 0.0612(13) 0.0474(11) -0.0122(10) 0.0177(8) -0.0135(9) C16 0.0369(11) 0.0955(19) 0.0558(14) -0.0172(13) 0.0171(10) -0.0162(12) O5 0.0190(5) 0.0201(5) 0.0192(5) 0.0024(4) 0.0030(4) 0.0004(4) O6 0.0213(5) 0.0236(6) 0.0242(5) 0.0034(4) 0.0030(4) -0.0017(4) C17 0.0223(7) 0.0215(8) 0.0172(7) -0.0011(5) 0.0002(5) -0.0003(6) C18 0.0243(8) 0.0230(8) 0.0270(8) 0.0049(6) 0.0006(6) 0.0023(6) C19 0.0395(10) 0.0256(9) 0.0365(9) 0.0005(7) -0.0022(7) 0.0014(7) C20 0.0430(10) 0.0307(9) 0.0409(10) 0.0010(8) -0.0164(8) 0.0009(8) C21 0.0311(9) 0.0467(12) 0.0649(13) 0.0211(10) 0.0146(9) 0.0142(8) O7 0.0241(5) 0.0212(5) 0.0204(5) 0.0023(4) 0.0036(4) -0.0042(4) O8 0.0376(6) 0.0267(6) 0.0280(6) 0.0079(5) -0.0054(5) -0.0076(5) C22 0.0231(7) 0.0193(7) 0.0252(8) 0.0006(6) 0.0049(6) 0.0005(6) C23 0.0302(8) 0.0213(8) 0.0276(8) 0.0020(6) 0.0032(6) -0.0048(6) C24 0.0358(9) 0.0292(9) 0.0316(9) 0.0036(7) 0.0062(7) -0.0085(7) C25 0.0333(9) 0.0352(10) 0.0543(12) 0.0113(9) -0.0096(8) -0.0130(8) C26 0.0570(11) 0.0256(9) 0.0314(9) -0.0053(7) 0.0109(8) -0.0090(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 O3 1.8807(9) . ? Mn1 O2 1.9166(9) . ? Mn1 O5 1.9392(10) 3_666 ? Mn1 O1 1.9557(9) . ? Mn1 O1 2.2177(9) 3_666 ? Mn1 N1 2.3760(12) . ? Mn1 Mn1 3.1618(4) 3_666 ? Mn1 Mn2 3.2391(3) 3_666 ? Mn2 O7 2.1161(10) . ? Mn2 O2 2.1351(10) 3_666 ? Mn2 O3 2.3026(10) . ? Mn2 O4 2.3542(10) . ? Mn2 O1 2.3573(9) . ? Mn2 O6 2.3605(10) . ? Mn2 N2 2.4204(12) . ? Mn2 Mn1 3.2391(3) 3_666 ? N1 C5 1.4839(18) . ? N1 C1 1.4844(18) . ? N1 C3 1.4906(18) . ? C1 C2 1.5208(19) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O1 1.4290(16) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O1 Mn1 2.2177(9) 3_666 ? C3 C4 1.515(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.4312(16) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O2 Mn2 2.1351(9) 3_666 ? C5 C6 1.511(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.538(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.516(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N2 C11 1.4768(18) . ? N2 C9 1.4787(19) . ? N2 C13 1.4819(18) . ? C9 C10 1.519(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O3 1.4181(16) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.507(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O4 1.4338(19) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O4 H4 0.846(17) . ? C13 C14 1.528(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.522(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.522(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O5 C17 1.3014(17) . ? O5 Mn1 1.9392(10) 3_666 ? O6 C17 1.2350(17) . ? C17 C18 1.5376(19) . ? C18 C19 1.524(2) . ? C18 C21 1.533(2) . ? C18 C20 1.540(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O7 C22 1.2752(17) . ? O8 C22 1.2519(18) . ? C22 C23 1.539(2) . ? C23 C24 1.536(2) . ? C23 C26 1.536(2) . ? C23 C25 1.537(2) . ? 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 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 O2 172.57(4) . . ? O3 Mn1 O5 93.34(4) . 3_666 ? O2 Mn1 O5 92.63(4) . 3_666 ? O3 Mn1 O1 81.86(4) . . ? O2 Mn1 O1 92.73(4) . . ? O5 Mn1 O1 171.67(4) 3_666 . ? O3 Mn1 O1 99.20(4) . 3_666 ? O2 Mn1 O1 84.96(4) . 3_666 ? O5 Mn1 O1 92.43(4) 3_666 3_666 ? O1 Mn1 O1 81.69(4) . 3_666 ? O3 Mn1 N1 97.22(4) . . ? O2 Mn1 N1 76.79(4) . . ? O5 Mn1 N1 106.77(4) 3_666 . ? O1 Mn1 N1 80.69(4) . . ? O1 Mn1 N1 153.88(4) 3_666 . ? O3 Mn1 Mn1 91.41(3) . 3_666 ? O2 Mn1 Mn1 88.16(3) . 3_666 ? O5 Mn1 Mn1 129.93(3) 3_666 3_666 ? O1 Mn1 Mn1 43.95(3) . 3_666 ? O1 Mn1 Mn1 37.74(2) 3_666 3_666 ? N1 Mn1 Mn1 121.98(3) . 3_666 ? O3 Mn1 Mn2 145.73(3) . 3_666 ? O2 Mn1 Mn2 39.31(3) . 3_666 ? O5 Mn1 Mn2 86.03(3) 3_666 3_666 ? O1 Mn1 Mn2 94.10(3) . 3_666 ? O1 Mn1 Mn2 46.70(2) 3_666 3_666 ? N1 Mn1 Mn2 115.80(3) . 3_666 ? Mn1 Mn1 Mn2 64.096(8) 3_666 3_666 ? O7 Mn2 O2 168.20(4) . 3_666 ? O7 Mn2 O3 96.68(4) . . ? O2 Mn2 O3 90.59(3) 3_666 . ? O7 Mn2 O4 88.94(4) . . ? O2 Mn2 O4 90.83(4) 3_666 . ? O3 Mn2 O4 143.05(4) . . ? O7 Mn2 O1 97.61(4) . . ? O2 Mn2 O1 76.97(3) 3_666 . ? O3 Mn2 O1 65.28(3) . . ? O4 Mn2 O1 150.14(4) . . ? O7 Mn2 O6 88.47(4) . . ? O2 Mn2 O6 80.06(4) 3_666 . ? O3 Mn2 O6 140.93(3) . . ? O4 Mn2 O6 75.45(4) . . ? O1 Mn2 O6 75.64(3) . . ? O7 Mn2 N2 94.50(4) . . ? O2 Mn2 N2 96.65(4) 3_666 . ? O3 Mn2 N2 71.08(4) . . ? O4 Mn2 N2 72.09(4) . . ? O1 Mn2 N2 135.70(4) . . ? O6 Mn2 N2 147.32(4) . . ? O7 Mn2 Mn1 137.24(3) . 3_666 ? O2 Mn2 Mn1 34.66(2) 3_666 3_666 ? O3 Mn2 Mn1 82.42(2) . 3_666 ? O4 Mn2 Mn1 117.07(3) . 3_666 ? O1 Mn2 Mn1 43.21(2) . 3_666 ? O6 Mn2 Mn1 68.37(3) . 3_666 ? N2 Mn2 Mn1 124.58(3) . 3_666 ? C5 N1 C1 109.75(11) . . ? C5 N1 C3 113.22(11) . . ? C1 N1 C3 110.77(11) . . ? C5 N1 Mn1 116.79(9) . . ? C1 N1 Mn1 101.08(8) . . ? C3 N1 Mn1 104.51(8) . . ? N1 C1 C2 110.97(12) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? O1 C2 C1 108.85(11) . . ? O1 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O1 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 O1 Mn1 113.37(8) . . ? C2 O1 Mn1 127.78(8) . 3_666 ? Mn1 O1 Mn1 98.31(4) . 3_666 ? C2 O1 Mn2 119.03(8) . . ? Mn1 O1 Mn2 103.54(4) . . ? Mn1 O1 Mn2 90.09(3) 3_666 . ? N1 C3 C4 109.71(12) . . ? N1 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N1 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? O2 C4 C3 107.81(11) . . ? O2 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O2 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.5 . . ? C4 O2 Mn1 111.25(8) . . ? C4 O2 Mn2 130.19(8) . 3_666 ? Mn1 O2 Mn2 106.03(4) . 3_666 ? N1 C5 C6 113.67(12) . . ? 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 . . ? C5 C6 C7 112.80(14) . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C6 113.89(15) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 N2 C9 110.59(12) . . ? C11 N2 C13 112.98(11) . . ? C9 N2 C13 112.71(12) . . ? C11 N2 Mn2 105.39(8) . . ? C9 N2 Mn2 104.44(8) . . ? C13 N2 Mn2 110.13(8) . . ? N2 C9 C10 111.11(12) . . ? N2 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? O3 C10 C9 108.58(11) . . ? O3 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? O3 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C10 O3 Mn1 126.70(9) . . ? C10 O3 Mn2 119.70(8) . . ? Mn1 O3 Mn2 108.17(4) . . ? N2 C11 C12 111.44(12) . . ? N2 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N2 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? O4 C12 C11 109.77(12) . . ? O4 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? O4 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C12 O4 Mn2 116.28(9) . . ? C12 O4 H4 106.3(12) . . ? Mn2 O4 H4 93.2(12) . . ? N2 C13 C14 116.30(13) . . ? N2 C13 H13A 108.2 . . ? C14 C13 H13A 108.2 . . ? N2 C13 H13B 108.2 . . ? C14 C13 H13B 108.2 . . ? H13A C13 H13B 107.4 . . ? C15 C14 C13 112.42(14) . . ? C15 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 112.30(17) . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 O5 Mn1 126.58(9) . 3_666 ? C17 O6 Mn2 131.90(10) . . ? O6 C17 O5 125.77(13) . . ? O6 C17 C18 119.36(13) . . ? O5 C17 C18 114.82(12) . . ? C19 C18 C21 109.81(14) . . ? C19 C18 C17 109.24(12) . . ? C21 C18 C17 112.38(13) . . ? C19 C18 C20 110.46(13) . . ? C21 C18 C20 109.42(15) . . ? C17 C18 C20 105.45(12) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 O7 Mn2 130.92(9) . . ? O8 C22 O7 124.94(13) . . ? O8 C22 C23 118.80(13) . . ? O7 C22 C23 116.26(13) . . ? C24 C23 C26 109.50(13) . . ? C24 C23 C25 109.30(13) . . ? C26 C23 C25 110.12(14) . . ? C24 C23 C22 111.20(13) . . ? C26 C23 C22 107.12(12) . . ? C25 C23 C22 109.58(13) . . ? 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 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O8 0.846(17) 1.791(17) 2.6150(15) 164.0(17) . _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.486 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.058 data_197a _database_code_depnum_ccdc_archive 'CCDC 600738' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H88 Mn4 N4 O16' _chemical_formula_weight 1341.10 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 1 21/n 1' 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 16.6894(14) _cell_length_b 8.7360(7) _cell_length_c 21.3378(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.949(2) _cell_angle_gamma 90.00 _cell_volume 3106.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5621 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.81 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.628 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15182 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.03 _reflns_number_total 6997 _reflns_number_gt 5576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _refine_special_details ; Organic C-H in calculated positions; coordinates of O-H H atoms refined. 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^)+(0.0480P)^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 6997 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 0.575614(19) 0.58075(4) 0.472215(15) 0.01413(9) Uani 1 1 d . . . Mn2 Mn 0.42713(2) 0.45471(4) 0.377157(15) 0.01518(9) Uani 1 1 d . . . N1 N 0.67101(11) 0.4488(2) 0.42131(8) 0.0167(4) Uani 1 1 d . . . C1 C 0.63595(13) 0.2940(3) 0.41073(10) 0.0180(5) Uani 1 1 d . . . H1A H 0.6786 0.2162 0.4179 0.022 Uiso 1 1 calc R . . H1B H 0.6154 0.2855 0.3665 0.022 Uiso 1 1 calc R . . C2 C 0.56770(13) 0.2605(3) 0.45385(10) 0.0180(5) Uani 1 1 d . . . H2A H 0.5366 0.1710 0.4378 0.022 Uiso 1 1 calc R . . H2B H 0.5901 0.2356 0.4965 0.022 Uiso 1 1 calc R . . O1 O 0.51638(9) 0.39028(18) 0.45660(7) 0.0150(3) Uani 1 1 d . . . C3 C 0.73863(13) 0.4550(3) 0.46828(10) 0.0195(5) Uani 1 1 d . . . H3A H 0.7635 0.5579 0.4679 0.023 Uiso 1 1 calc R . . H3B H 0.7798 0.3790 0.4576 0.023 Uiso 1 1 calc R . . C4 C 0.71000(13) 0.4214(3) 0.53333(10) 0.0186(5) Uani 1 1 d . . . H4A H 0.7042 0.3095 0.5387 0.022 Uiso 1 1 calc R . . H4B H 0.7503 0.4587 0.5655 0.022 Uiso 1 1 calc R . . O2 O 0.63588(9) 0.49326(19) 0.54175(7) 0.0164(3) Uani 1 1 d . . . C5 C 0.69110(14) 0.5237(3) 0.36175(10) 0.0196(5) Uani 1 1 d . . . H5A H 0.7089 0.6296 0.3713 0.024 Uiso 1 1 calc R . . H5B H 0.6415 0.5305 0.3343 0.024 Uiso 1 1 calc R . . C6 C 0.75565(14) 0.4451(3) 0.32507(11) 0.0218(5) Uani 1 1 d . . . H6A H 0.8059 0.4383 0.3517 0.026 Uiso 1 1 calc R . . H6B H 0.7382 0.3397 0.3142 0.026 Uiso 1 1 calc R . . C7 C 0.77151(15) 0.5328(3) 0.26523(11) 0.0253(6) Uani 1 1 d . . . H7A H 0.7212 0.5383 0.2386 0.030 Uiso 1 1 calc R . . H7B H 0.7878 0.6388 0.2763 0.030 Uiso 1 1 calc R . . C8 C 0.83655(16) 0.4589(3) 0.22802(12) 0.0311(6) Uani 1 1 d . . . H8A H 0.8449 0.5198 0.1903 0.047 Uiso 1 1 calc R . . H8B H 0.8200 0.3551 0.2158 0.047 Uiso 1 1 calc R . . H8C H 0.8867 0.4544 0.2540 0.047 Uiso 1 1 calc R . . N2 N 0.39552(11) 0.6720(2) 0.30991(8) 0.0170(4) Uani 1 1 d . . . C9 C 0.42168(13) 0.8088(3) 0.34631(10) 0.0200(5) Uani 1 1 d . . . H9A H 0.3851 0.8255 0.3808 0.024 Uiso 1 1 calc R . . H9B H 0.4188 0.8999 0.3187 0.024 Uiso 1 1 calc R . . C10 C 0.50719(13) 0.7896(3) 0.37365(10) 0.0194(5) Uani 1 1 d . . . H10A H 0.5457 0.7990 0.3401 0.023 Uiso 1 1 calc R . . H10B H 0.5196 0.8699 0.4054 0.023 Uiso 1 1 calc R . . O3 O 0.51355(9) 0.64326(19) 0.40164(7) 0.0175(3) Uani 1 1 d . . . C11 C 0.30693(13) 0.6676(3) 0.30083(11) 0.0199(5) Uani 1 1 d . . . H11A H 0.2892 0.7450 0.2692 0.024 Uiso 1 1 calc R . . H11B H 0.2826 0.6937 0.3408 0.024 Uiso 1 1 calc R . . C12 C 0.27840(14) 0.5119(3) 0.27945(11) 0.0218(5) Uani 1 1 d . . . H12A H 0.2190 0.5101 0.2757 0.026 Uiso 1 1 calc R . . H12B H 0.2988 0.4888 0.2377 0.026 Uiso 1 1 calc R . . O4 O 0.30681(10) 0.3995(2) 0.32397(7) 0.0200(4) Uani 1 1 d . . . H4 H 0.3280(17) 0.336(4) 0.3055(13) 0.030 Uiso 1 1 d . . . C13 C 0.43565(14) 0.6571(3) 0.25005(10) 0.0212(5) Uani 1 1 d . . . H13A H 0.4769 0.5838 0.2451 0.025 Uiso 1 1 calc R . . C14 C 0.40818(15) 0.7645(3) 0.19635(11) 0.0277(6) Uani 1 1 d . . . H14A H 0.3514 0.7433 0.1836 0.033 Uiso 1 1 calc R . . H14B H 0.4122 0.8721 0.2107 0.033 Uiso 1 1 calc R . . C15 C 0.46041(16) 0.7411(3) 0.14041(11) 0.0319(6) Uani 1 1 d . . . H15A H 0.5124 0.7937 0.1490 0.038 Uiso 1 1 calc R . . H15B H 0.4715 0.6304 0.1359 0.038 Uiso 1 1 calc R . . C16 C 0.42220(19) 0.8009(4) 0.07891(12) 0.0427(8) Uani 1 1 d . . . H16A H 0.4585 0.7827 0.0450 0.064 Uiso 1 1 calc R . . H16B H 0.4122 0.9110 0.0826 0.064 Uiso 1 1 calc R . . H16C H 0.3713 0.7476 0.0695 0.064 Uiso 1 1 calc R . . O5 O 0.36906(9) 0.22585(19) 0.51685(7) 0.0188(3) Uani 1 1 d . . . O6 O 0.38227(9) 0.1987(2) 0.41302(7) 0.0209(4) Uani 1 1 d . . . C17 C 0.34872(13) 0.1703(3) 0.46176(10) 0.0174(5) Uani 1 1 d . . . C18 C 0.27773(13) 0.0646(3) 0.46054(10) 0.0182(5) Uani 1 1 d . . . C19 C 0.23917(14) 0.0301(3) 0.51464(12) 0.0244(5) Uani 1 1 d . . . H19A H 0.2597 0.0682 0.5540 0.029 Uiso 1 1 calc R . . C20 C 0.17045(15) -0.0602(3) 0.51169(12) 0.0289(6) Uani 1 1 d . . . H20A H 0.1443 -0.0840 0.5490 0.035 Uiso 1 1 calc R . . C21 C 0.14003(15) -0.1153(3) 0.45438(12) 0.0290(6) Uani 1 1 d . . . H21A H 0.0928 -0.1763 0.4524 0.035 Uiso 1 1 calc R . . C22 C 0.17850(15) -0.0816(3) 0.40007(12) 0.0269(6) Uani 1 1 d . . . H22A H 0.1580 -0.1204 0.3608 0.032 Uiso 1 1 calc R . . C23 C 0.24678(14) 0.0086(3) 0.40297(11) 0.0233(5) Uani 1 1 d . . . H23A H 0.2727 0.0325 0.3656 0.028 Uiso 1 1 calc R . . O7 O 0.48684(9) 0.3370(2) 0.30692(7) 0.0200(4) Uani 1 1 d . . . O8 O 0.38807(10) 0.2133(2) 0.25253(7) 0.0250(4) Uani 1 1 d . . . C24 C 0.45760(14) 0.2662(3) 0.25901(10) 0.0192(5) Uani 1 1 d . . . C25 C 0.51077(14) 0.2534(3) 0.20415(10) 0.0214(5) Uani 1 1 d . . . C26 C 0.57781(15) 0.3450(4) 0.20104(11) 0.0306(6) Uani 1 1 d . . . H26A H 0.5926 0.4112 0.2350 0.037 Uiso 1 1 calc R . . C27 C 0.62375(15) 0.3411(4) 0.14861(12) 0.0345(7) Uani 1 1 d . . . H27A H 0.6692 0.4061 0.1465 0.041 Uiso 1 1 calc R . . C28 C 0.60362(16) 0.2431(3) 0.09957(12) 0.0311(6) Uani 1 1 d . . . H28A H 0.6350 0.2402 0.0637 0.037 Uiso 1 1 calc R . . C29 C 0.53774(18) 0.1498(3) 0.10310(12) 0.0345(7) Uani 1 1 d . . . H29A H 0.5245 0.0800 0.0700 0.041 Uiso 1 1 calc R . . C30 C 0.49038(17) 0.1566(3) 0.15470(11) 0.0301(6) Uani 1 1 d . . . H30A H 0.4438 0.0944 0.1560 0.036 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 0.01631(17) 0.01522(18) 0.01069(16) 0.00020(14) -0.00076(12) -0.00072(14) Mn2 0.01769(17) 0.01669(19) 0.01103(16) -0.00034(14) -0.00043(13) -0.00015(14) N1 0.0193(9) 0.0186(11) 0.0122(9) -0.0004(8) 0.0003(7) -0.0009(8) C1 0.0207(11) 0.0178(12) 0.0154(11) -0.0015(9) -0.0006(9) 0.0020(10) C2 0.0199(11) 0.0154(12) 0.0185(11) -0.0006(9) -0.0004(9) 0.0017(9) O1 0.0171(7) 0.0146(8) 0.0133(7) -0.0004(6) 0.0004(6) 0.0002(6) C3 0.0186(11) 0.0248(13) 0.0154(11) -0.0005(10) 0.0020(9) 0.0004(10) C4 0.0169(10) 0.0229(13) 0.0158(11) 0.0014(10) -0.0012(9) 0.0026(10) O2 0.0173(7) 0.0199(9) 0.0118(7) 0.0014(7) 0.0000(6) 0.0022(7) C5 0.0237(11) 0.0207(13) 0.0146(11) 0.0003(10) 0.0024(9) 0.0003(10) C6 0.0222(11) 0.0247(14) 0.0191(11) -0.0001(10) 0.0051(9) 0.0002(10) C7 0.0303(13) 0.0274(14) 0.0186(12) -0.0001(11) 0.0062(10) -0.0031(11) C8 0.0377(14) 0.0313(16) 0.0255(13) -0.0014(12) 0.0134(12) -0.0042(12) N2 0.0187(9) 0.0186(10) 0.0136(9) -0.0003(8) -0.0002(7) -0.0011(8) C9 0.0260(12) 0.0164(12) 0.0172(11) 0.0008(10) -0.0030(9) 0.0013(10) C10 0.0247(12) 0.0172(12) 0.0158(11) 0.0033(10) -0.0047(9) -0.0035(10) O3 0.0207(8) 0.0169(9) 0.0143(7) 0.0025(7) -0.0031(6) -0.0008(7) C11 0.0223(11) 0.0201(13) 0.0169(11) 0.0030(10) -0.0023(9) 0.0026(10) C12 0.0230(12) 0.0229(13) 0.0188(11) 0.0040(10) -0.0052(9) -0.0003(10) O4 0.0234(9) 0.0192(9) 0.0173(8) 0.0015(7) -0.0010(7) 0.0014(7) C13 0.0243(12) 0.0238(13) 0.0155(11) 0.0023(10) 0.0021(9) 0.0041(10) C14 0.0364(14) 0.0254(14) 0.0213(12) 0.0045(11) 0.0024(11) 0.0004(12) C15 0.0441(15) 0.0322(16) 0.0197(12) 0.0023(12) 0.0045(11) -0.0049(13) C16 0.0598(19) 0.0435(19) 0.0247(14) 0.0005(14) 0.0015(13) -0.0150(16) O5 0.0228(8) 0.0183(9) 0.0148(8) 0.0000(7) -0.0022(6) -0.0045(7) O6 0.0231(8) 0.0226(9) 0.0170(8) -0.0001(7) 0.0010(7) -0.0018(7) C17 0.0187(10) 0.0157(12) 0.0176(11) -0.0009(9) -0.0021(9) 0.0026(9) C18 0.0205(11) 0.0150(12) 0.0189(11) -0.0003(9) -0.0018(9) 0.0009(9) C19 0.0276(12) 0.0221(14) 0.0229(12) 0.0009(11) -0.0035(10) 0.0015(11) C20 0.0285(13) 0.0310(16) 0.0276(13) 0.0043(12) 0.0038(11) -0.0033(12) C21 0.0227(12) 0.0261(15) 0.0377(15) 0.0013(12) -0.0031(11) -0.0036(11) C22 0.0272(12) 0.0251(14) 0.0277(13) -0.0026(11) -0.0049(11) 0.0010(11) C23 0.0241(12) 0.0233(14) 0.0222(12) 0.0003(11) -0.0018(10) 0.0026(11) O7 0.0240(8) 0.0229(9) 0.0129(7) -0.0021(7) -0.0009(6) 0.0024(7) O8 0.0254(9) 0.0270(10) 0.0225(9) -0.0076(8) 0.0002(7) -0.0024(8) C24 0.0265(12) 0.0152(12) 0.0156(11) 0.0000(9) -0.0005(9) 0.0054(10) C25 0.0269(12) 0.0219(13) 0.0150(11) 0.0009(10) -0.0015(9) 0.0069(10) C26 0.0273(13) 0.0441(18) 0.0201(12) -0.0068(12) -0.0018(10) 0.0018(13) C27 0.0249(13) 0.054(2) 0.0249(13) -0.0017(13) 0.0021(11) -0.0006(13) C28 0.0355(14) 0.0365(17) 0.0218(13) 0.0001(12) 0.0070(11) 0.0096(13) C29 0.0536(17) 0.0276(15) 0.0225(13) -0.0065(12) 0.0049(12) 0.0041(14) C30 0.0431(15) 0.0239(14) 0.0236(13) 0.0000(11) 0.0044(11) 0.0004(12) _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 1.8651(15) . ? Mn1 O2 1.9088(15) . ? Mn1 O5 1.9337(17) 3_666 ? Mn1 O1 1.9552(16) . ? Mn1 O1 2.2290(15) 3_666 ? Mn1 N1 2.2848(19) . ? Mn2 O7 2.1094(16) . ? Mn2 O2 2.1198(15) 3_666 ? Mn2 O3 2.2336(16) . ? Mn2 O1 2.2692(15) . ? Mn2 O4 2.3060(17) . ? Mn2 N2 2.4213(19) . ? Mn2 O6 2.4912(17) . ? N1 C3 1.471(3) . ? N1 C5 1.483(3) . ? N1 C1 1.487(3) . ? C1 C2 1.529(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O1 1.424(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O1 Mn1 2.2290(15) 3_666 ? C3 C4 1.520(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.407(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O2 Mn2 2.1198(15) 3_666 ? C5 C6 1.527(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.524(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.521(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N2 C13 1.478(3) . ? N2 C9 1.479(3) . ? N2 C11 1.482(3) . ? C9 C10 1.523(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O3 1.413(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.504(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O4 1.430(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O4 H4 0.77(3) . ? C13 C14 1.533(3) . ? C13 H13A 0.9500 . ? C14 C15 1.528(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.522(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O5 C17 1.300(3) . ? O5 Mn1 1.9337(16) 3_666 ? O6 C17 1.231(3) . ? C17 C18 1.501(3) . ? C18 C19 1.384(3) . ? C18 C23 1.396(3) . ? C19 C20 1.391(3) . ? C19 H19A 0.9500 . ? C20 C21 1.386(4) . ? C20 H20A 0.9500 . ? C21 C22 1.385(4) . ? C21 H21A 0.9500 . ? C22 C23 1.384(3) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? O7 C24 1.271(3) . ? O8 C24 1.250(3) . ? C24 C25 1.509(3) . ? C25 C26 1.380(4) . ? C25 C30 1.381(3) . ? C26 C27 1.389(3) . ? C26 H26A 0.9500 . ? C27 C28 1.380(4) . ? C27 H27A 0.9500 . ? C28 C29 1.374(4) . ? C28 H28A 0.9500 . ? C29 C30 1.389(4) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? 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 O2 173.41(7) . . ? O3 Mn1 O5 94.79(7) . 3_666 ? O2 Mn1 O5 91.54(7) . 3_666 ? O3 Mn1 O1 81.76(7) . . ? O2 Mn1 O1 91.91(7) . . ? O5 Mn1 O1 176.54(6) 3_666 . ? O3 Mn1 O1 98.26(6) . 3_666 ? O2 Mn1 O1 82.51(6) . 3_666 ? O5 Mn1 O1 99.20(6) 3_666 3_666 ? O1 Mn1 O1 81.54(6) . 3_666 ? O3 Mn1 N1 97.79(7) . . ? O2 Mn1 N1 79.36(6) . . ? O5 Mn1 N1 99.10(7) 3_666 . ? O1 Mn1 N1 81.27(6) . . ? O1 Mn1 N1 154.48(6) 3_666 . ? O7 Mn2 O2 163.09(7) . 3_666 ? O7 Mn2 O3 101.69(6) . . ? O2 Mn2 O3 89.57(6) 3_666 . ? O7 Mn2 O1 95.39(6) . . ? O2 Mn2 O1 77.15(5) 3_666 . ? O3 Mn2 O1 67.48(6) . . ? O7 Mn2 O4 88.84(6) . . ? O2 Mn2 O4 89.46(6) 3_666 . ? O3 Mn2 O4 143.58(6) . . ? O1 Mn2 O4 146.86(6) . . ? O7 Mn2 N2 93.30(6) . . ? O2 Mn2 N2 102.33(6) 3_666 . ? O3 Mn2 N2 71.27(6) . . ? O1 Mn2 N2 138.74(6) . . ? O4 Mn2 N2 73.41(6) . . ? O7 Mn2 O6 86.63(6) . . ? O2 Mn2 O6 76.83(6) 3_666 . ? O3 Mn2 O6 142.26(5) . . ? O1 Mn2 O6 75.16(5) . . ? O4 Mn2 O6 72.29(6) . . ? N2 Mn2 O6 145.70(6) . . ? C3 N1 C5 111.59(17) . . ? C3 N1 C1 114.79(19) . . ? C5 N1 C1 112.08(17) . . ? C3 N1 Mn1 100.74(13) . . ? C5 N1 Mn1 112.24(14) . . ? C1 N1 Mn1 104.64(12) . . ? N1 C1 C2 112.48(18) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? O1 C2 C1 109.91(18) . . ? O1 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O1 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 O1 Mn1 112.63(12) . . ? C2 O1 Mn1 123.72(13) . 3_666 ? Mn1 O1 Mn1 98.46(6) . 3_666 ? C2 O1 Mn2 122.67(13) . . ? Mn1 O1 Mn2 102.88(7) . . ? Mn1 O1 Mn2 91.85(5) 3_666 . ? N1 C3 C4 110.41(18) . . ? N1 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? O2 C4 C3 110.50(18) . . ? O2 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? O2 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 O2 Mn1 120.72(12) . . ? C4 O2 Mn2 132.55(13) . 3_666 ? Mn1 O2 Mn2 106.56(7) . 3_666 ? N1 C5 C6 115.9(2) . . ? N1 C5 H5A 108.3 . . ? C6 C5 H5A 108.3 . . ? N1 C5 H5B 108.3 . . ? C6 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C7 C6 C5 111.2(2) . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 112.5(2) . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C13 N2 C9 112.98(18) . . ? C13 N2 C11 112.22(17) . . ? C9 N2 C11 110.81(18) . . ? C13 N2 Mn2 110.39(14) . . ? C9 N2 Mn2 105.83(13) . . ? C11 N2 Mn2 104.05(13) . . ? N2 C9 C10 110.96(19) . . ? N2 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? O3 C10 C9 108.06(19) . . ? O3 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O3 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 O3 Mn1 129.26(14) . . ? C10 O3 Mn2 122.34(12) . . ? Mn1 O3 Mn2 107.34(7) . . ? N2 C11 C12 111.17(19) . . ? N2 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? N2 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? O4 C12 C11 109.29(18) . . ? O4 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? O4 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? C12 O4 Mn2 115.73(13) . . ? C12 O4 H4 107(2) . . ? Mn2 O4 H4 89(2) . . ? N2 C13 C14 117.4(2) . . ? N2 C13 H13A 121.3 . . ? C14 C13 H13A 121.3 . . ? C15 C14 C13 110.0(2) . . ? C15 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? C15 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C14 113.4(2) . . ? C16 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 . . ? C16 C15 H15B 108.9 . . ? C14 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 O5 Mn1 122.40(15) . 3_666 ? C17 O6 Mn2 126.66(15) . . ? O6 C17 O5 125.4(2) . . ? O6 C17 C18 120.1(2) . . ? O5 C17 C18 114.47(19) . . ? C19 C18 C23 119.4(2) . . ? C19 C18 C17 121.3(2) . . ? C23 C18 C17 119.1(2) . . ? C18 C19 C20 120.3(2) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C21 C20 C19 120.1(2) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C22 120.0(2) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C23 C22 C21 120.0(2) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C18 120.3(2) . . ? C22 C23 H23A 119.8 . . ? C18 C23 H23A 119.8 . . ? C24 O7 Mn2 129.27(14) . . ? O8 C24 O7 125.8(2) . . ? O8 C24 C25 117.8(2) . . ? O7 C24 C25 116.3(2) . . ? C26 C25 C30 119.1(2) . . ? C26 C25 C24 120.3(2) . . ? C30 C25 C24 120.4(2) . . ? C25 C26 C27 120.5(2) . . ? C25 C26 H26A 119.8 . . ? C27 C26 H26A 119.8 . . ? C28 C27 C26 120.2(3) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C29 C28 C27 119.4(2) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C28 C29 C30 120.5(3) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C25 C30 C29 120.3(3) . . ? C25 C30 H30A 119.9 . . ? C29 C30 H30A 119.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O8 0.77(3) 1.89(3) 2.650(2) 169(3) . _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.796 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.079 data_a200a _database_code_depnum_ccdc_archive 'CCDC 600739' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H75.90 Mn4 N4.70 O20.30' _chemical_formula_weight 1335.45 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 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.242(3) _cell_length_b 8.6710(6) _cell_length_c 26.618(3) _cell_angle_alpha 90.00 _cell_angle_beta 119.915(9) _cell_angle_gamma 90.00 _cell_volume 6050.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15801 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 27.21 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2781 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.983 _exptl_absorpt_process_details ; XPREP in SHELXTL 5.1 (Bruker AXS Inc., 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _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 13938 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.85 _reflns_number_total 5810 _reflns_number_gt 4525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.05 (Stoe & Cie GmbH, 2000)' _computing_cell_refinement 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_data_reduction 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _refine_special_details ; The systematic absences for the c-glide were not particularly clean, and a slight improvement in the R-factors was found if the structure was solved and refined in C2. However, correlation between (pseudo)- symmetry related parameters became severe, and we prefer the version of the structure in C2/c. The disordered lattice solvent was refined as superimposed MeCN (70%, lying on the 2-fold axis) and EtOH (30%, disordered across the axis), with atom C31 in common. 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^)+(0.1123P)^2^+44.2229P] 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 5810 _refine_ls_number_parameters 386 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1091 _refine_ls_R_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.2397 _refine_ls_wR_factor_gt 0.2279 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.090 _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 0.45966(4) 0.42538(11) 0.51436(3) 0.0363(3) Uani 1 1 d . . . Mn2 Mn 0.42447(4) 0.47251(11) 0.37808(4) 0.0366(3) Uani 1 1 d . . . O1 O 0.50281(16) 0.6092(5) 0.53975(16) 0.0365(9) Uani 1 1 d . . . O2 O 0.40951(17) 0.5223(6) 0.44477(17) 0.0444(11) Uani 1 1 d . . . O3A O 0.4048(4) 0.6650(12) 0.6526(5) 0.065(3) Uani 0.62 1 d P A 1 H3A H 0.3881 0.7092 0.6659 0.097 Uiso 0.62 1 calc PR A 1 O3B O 0.3804(8) 0.680(3) 0.6260(9) 0.081(6) Uiso 0.38 1 d P A 2 H3B H 0.4104 0.6927 0.6533 0.121 Uiso 0.38 1 calc PR A 2 O4 O 0.48862(16) 0.6486(5) 0.41474(16) 0.0386(9) Uani 1 1 d . . . O5 O 0.33844(19) 0.4431(6) 0.31437(19) 0.0485(11) Uani 1 1 d D . . H5 H 0.329(3) 0.350(5) 0.299(3) 0.058 Uiso 1 1 d D . . O6 O 0.43986(18) 0.4104(7) 0.30899(19) 0.0512(12) Uani 1 1 d D . . H6 H 0.414(2) 0.380(8) 0.275(2) 0.061 Uiso 1 1 d D . . O7 O 0.42223(19) 0.2358(6) 0.49364(19) 0.0571(13) Uani 1 1 d . . . O8 O 0.40271(19) 0.2224(6) 0.3986(2) 0.0540(12) Uani 1 1 d . . . O9 O 0.3703(2) 0.2546(6) 0.2227(2) 0.0571(13) Uani 1 1 d D . . O10 O 0.31411(19) 0.1865(6) 0.25024(19) 0.0523(12) Uani 1 1 d . . . N1 N 0.4133(2) 0.5640(7) 0.5473(2) 0.0437(13) Uani 1 1 d . . . N2 N 0.3970(2) 0.6938(7) 0.3175(2) 0.0454(13) Uani 1 1 d . . . C1 C 0.4442(3) 0.7055(8) 0.5708(3) 0.0425(14) Uani 1 1 d . . . H1A H 0.4677 0.6923 0.6129 0.051 Uiso 1 1 calc R . . H1B H 0.4213 0.7932 0.5655 0.051 Uiso 1 1 calc R . . C2 C 0.4754(2) 0.7431(7) 0.5409(2) 0.0388(13) Uani 1 1 d . . . H2A H 0.4522 0.7785 0.5007 0.047 Uiso 1 1 calc R . . H2B H 0.4998 0.8273 0.5620 0.047 Uiso 1 1 calc R . . C3 C 0.3643(3) 0.5872(14) 0.4942(3) 0.077(3) Uani 1 1 d . . . H3C H 0.3406 0.5048 0.4917 0.092 Uiso 1 1 calc R . . H3D H 0.3498 0.6868 0.4973 0.092 Uiso 1 1 calc R . . C4 C 0.3663(3) 0.5873(15) 0.4423(3) 0.085(4) Uani 1 1 d . . . H4A H 0.3395 0.6296 0.4075 0.102 Uiso 1 1 calc R . . C5 C 0.4067(4) 0.4746(10) 0.5904(4) 0.066(2) Uani 1 1 d . A . H5A H 0.4409 0.4562 0.6243 0.079 Uiso 1 1 calc R . . H5B H 0.3924 0.3726 0.5732 0.079 Uiso 1 1 calc R . . C6 C 0.3735(4) 0.5427(13) 0.6122(4) 0.072(3) Uani 1 1 d . . . H6A H 0.3418 0.5858 0.5798 0.087 Uiso 0.62 1 calc PR A 1 H6B H 0.3645 0.4636 0.6324 0.087 Uiso 0.62 1 calc PR A 1 H6C H 0.3374 0.5291 0.5818 0.087 Uiso 0.38 1 calc PR A 2 H6D H 0.3789 0.4824 0.6464 0.087 Uiso 0.38 1 calc PR A 2 C7 C 0.4247(3) 0.8275(8) 0.3549(3) 0.0562(19) Uani 1 1 d . . . H7A H 0.4112 0.8494 0.3812 0.067 Uiso 1 1 calc R . . H7B H 0.4186 0.9196 0.3303 0.067 Uiso 1 1 calc R . . C8 C 0.4808(3) 0.7975(8) 0.3899(3) 0.0509(17) Uani 1 1 d . . . H8A H 0.4963 0.8039 0.3649 0.061 Uiso 1 1 calc R . . H8B H 0.4971 0.8759 0.4209 0.061 Uiso 1 1 calc R . . C9 C 0.3412(3) 0.7080(10) 0.2949(3) 0.0535(19) Uani 1 1 d . . . H9A H 0.3269 0.7876 0.2642 0.064 Uiso 1 1 calc R . . H9B H 0.3353 0.7415 0.3266 0.064 Uiso 1 1 calc R . . C10 C 0.3146(3) 0.5586(10) 0.2710(3) 0.060(2) Uani 1 1 d . . . H10A H 0.2782 0.5678 0.2595 0.072 Uiso 1 1 calc R . . H10B H 0.3169 0.5304 0.2362 0.072 Uiso 1 1 calc R . . C11 C 0.4085(3) 0.6692(10) 0.2700(3) 0.057(2) Uani 1 1 d . . . H11A H 0.4205 0.7673 0.2619 0.069 Uiso 1 1 calc R . . H11B H 0.3768 0.6386 0.2344 0.069 Uiso 1 1 calc R . . C12 C 0.4491(3) 0.5448(11) 0.2851(3) 0.059(2) Uani 1 1 d . . . H12A H 0.4500 0.5162 0.2496 0.071 Uiso 1 1 calc R . . H12B H 0.4829 0.5874 0.3132 0.071 Uiso 1 1 calc R . . C13 C 0.3968(3) 0.1837(9) 0.4400(3) 0.0514(17) Uani 1 1 d . . . C14 C 0.3538(3) 0.0799(8) 0.4308(3) 0.0503(16) Uani 1 1 d . . . C15 C 0.3440(3) 0.0471(8) 0.4746(3) 0.0510(17) Uani 1 1 d . . . H15A H 0.3662 0.0878 0.5121 0.061 Uiso 1 1 calc R . . C16 C 0.3023(4) -0.0443(10) 0.4668(4) 0.070(2) Uani 1 1 d . . . H16A H 0.2956 -0.0618 0.4976 0.084 Uiso 1 1 calc R . . C17 C 0.2710(3) -0.1085(9) 0.4113(3) 0.0568(19) Uani 1 1 d . . . H17A H 0.2429 -0.1719 0.4043 0.068 Uiso 1 1 calc R . . C18 C 0.2812(3) -0.0795(9) 0.3675(4) 0.060(2) Uani 1 1 d . . . H18A H 0.2601 -0.1244 0.3305 0.072 Uiso 1 1 calc R . . C19 C 0.3223(3) 0.0154(9) 0.3761(3) 0.0541(18) Uani 1 1 d . . . H19A H 0.3285 0.0353 0.3451 0.065 Uiso 1 1 calc R . . C20 C 0.3351(2) 0.1700(8) 0.2200(2) 0.0422(14) Uani 1 1 d . . . C21 C 0.3176(3) 0.0390(7) 0.1772(2) 0.0424(14) Uani 1 1 d . . . C22 C 0.2722(3) -0.0364(9) 0.1617(3) 0.0554(18) Uani 1 1 d . . . H22A H 0.2520 -0.0040 0.1779 0.066 Uiso 1 1 calc R . . C23 C 0.2559(4) -0.1578(10) 0.1232(4) 0.079(3) Uani 1 1 d . . . H23A H 0.2249 -0.2092 0.1134 0.095 Uiso 1 1 calc R . . C24 C 0.2847(5) -0.2048(11) 0.0987(5) 0.095(4) Uani 1 1 d . . . H24A H 0.2734 -0.2884 0.0721 0.114 Uiso 1 1 calc R . . C25 C 0.3302(5) -0.1305(12) 0.1129(5) 0.094(3) Uani 1 1 d . . . H25A H 0.3498 -0.1615 0.0956 0.113 Uiso 1 1 calc R . . C26 C 0.3468(4) -0.0086(10) 0.1531(4) 0.067(2) Uani 1 1 d . . . H26A H 0.3782 0.0414 0.1638 0.081 Uiso 1 1 calc R . . C32A C 0.0000 0.6570(19) 0.2500 0.058(4) Uiso 0.70 2 d SP B 1 H32A H -0.0341 0.6946 0.2217 0.087 Uiso 0.35 1 calc PR B 1 H32B H 0.0249 0.6946 0.2396 0.087 Uiso 0.35 1 calc PR B 1 H32C H 0.0091 0.6946 0.2887 0.087 Uiso 0.35 1 calc PR B 1 C32B C -0.001(2) 0.545(7) 0.197(2) 0.069(14) Uiso 0.15 1 d P B 2 H32D H 0.0115 0.6520 0.2016 0.103 Uiso 0.15 1 calc PR B 2 H32E H -0.0355 0.5387 0.1643 0.103 Uiso 0.15 1 calc PR B 2 H32F H 0.0218 0.4781 0.1901 0.103 Uiso 0.15 1 calc PR B 2 C31 C 0.0000 0.496(2) 0.2500 0.103(5) Uiso 1 2 d S . . N31 N 0.0000 0.357(3) 0.2500 0.110(7) Uiso 0.70 2 d SPU B 1 O31 O 0.0179(15) 0.366(5) 0.2833(17) 0.068(10) Uiso 0.15 1 d PU B 2 H31 H 0.0208 0.2951 0.2638 0.101 Uiso 0.15 1 calc PR B 2 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 0.0425(5) 0.0393(5) 0.0277(4) 0.0007(3) 0.0180(4) 0.0069(4) Mn2 0.0409(5) 0.0387(5) 0.0323(4) -0.0012(3) 0.0198(4) 0.0026(4) O1 0.042(2) 0.038(2) 0.0360(19) 0.0033(16) 0.0243(17) 0.0133(19) O2 0.042(2) 0.063(3) 0.0340(19) 0.0104(19) 0.0234(18) 0.014(2) O3A 0.081(7) 0.074(7) 0.075(6) -0.033(5) 0.065(6) -0.018(6) O4 0.044(2) 0.037(2) 0.0349(19) 0.0039(16) 0.0198(17) 0.0003(19) O5 0.053(3) 0.058(3) 0.041(2) -0.003(2) 0.029(2) 0.001(2) O6 0.048(3) 0.070(3) 0.045(2) -0.013(2) 0.030(2) -0.004(2) O7 0.057(3) 0.049(3) 0.039(2) -0.005(2) 0.005(2) -0.007(2) O8 0.049(3) 0.060(3) 0.050(3) -0.009(2) 0.022(2) 0.000(2) O9 0.069(3) 0.063(3) 0.057(3) -0.020(2) 0.045(3) -0.028(3) O10 0.051(3) 0.071(3) 0.040(2) -0.010(2) 0.027(2) -0.014(3) N1 0.052(3) 0.052(3) 0.038(2) -0.004(2) 0.030(2) -0.007(3) N2 0.045(3) 0.052(3) 0.030(2) 0.004(2) 0.012(2) 0.003(3) C1 0.050(3) 0.039(3) 0.049(3) -0.001(3) 0.032(3) 0.009(3) C2 0.038(3) 0.037(3) 0.041(3) 0.004(2) 0.019(2) 0.012(3) C3 0.041(4) 0.140(9) 0.048(4) -0.021(5) 0.021(3) 0.013(5) C4 0.056(4) 0.164(10) 0.041(4) 0.021(5) 0.028(3) 0.061(6) C5 0.107(7) 0.056(4) 0.075(5) -0.015(4) 0.075(5) -0.023(5) C6 0.076(5) 0.109(8) 0.055(4) -0.011(4) 0.050(4) -0.011(5) C7 0.066(4) 0.040(4) 0.046(3) 0.007(3) 0.015(3) 0.002(3) C8 0.065(4) 0.034(3) 0.041(3) 0.005(2) 0.017(3) -0.001(3) C9 0.047(4) 0.078(5) 0.033(3) 0.008(3) 0.018(3) 0.022(4) C10 0.053(4) 0.085(6) 0.040(3) 0.000(3) 0.022(3) 0.003(4) C11 0.057(4) 0.082(5) 0.034(3) -0.002(3) 0.023(3) -0.017(4) C12 0.054(4) 0.090(6) 0.040(3) -0.017(4) 0.028(3) -0.013(4) C13 0.053(4) 0.061(4) 0.036(3) -0.002(3) 0.019(3) -0.006(4) C14 0.052(4) 0.045(4) 0.049(3) 0.002(3) 0.021(3) 0.005(3) C15 0.049(4) 0.041(4) 0.054(4) 0.002(3) 0.019(3) -0.003(3) C16 0.076(5) 0.059(5) 0.073(5) 0.002(4) 0.035(5) -0.009(4) C17 0.046(4) 0.045(4) 0.065(4) -0.002(3) 0.016(3) -0.006(3) C18 0.046(4) 0.052(4) 0.066(4) -0.007(3) 0.016(3) -0.004(3) C19 0.052(4) 0.050(4) 0.049(3) -0.007(3) 0.017(3) 0.005(3) C20 0.042(3) 0.047(4) 0.034(3) 0.005(2) 0.016(2) -0.002(3) C21 0.053(4) 0.035(3) 0.037(3) 0.002(2) 0.021(3) -0.003(3) C22 0.054(4) 0.055(4) 0.048(4) 0.001(3) 0.019(3) -0.012(4) C23 0.094(7) 0.052(5) 0.065(5) -0.005(4) 0.019(5) -0.023(5) C24 0.131(10) 0.049(5) 0.086(7) -0.017(5) 0.039(7) -0.015(6) C25 0.145(11) 0.057(5) 0.104(8) -0.024(5) 0.080(8) -0.001(7) C26 0.078(5) 0.055(5) 0.078(5) -0.017(4) 0.047(5) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 1.864(4) 5_666 ? Mn1 O2 1.907(4) . ? Mn1 O7 1.914(5) . ? Mn1 O1 1.955(5) . ? Mn1 O1 2.255(4) 5_666 ? Mn1 N1 2.324(6) . ? Mn1 Mn1 3.173(2) 5_666 ? Mn2 O2 2.084(4) . ? Mn2 O6 2.178(4) . ? Mn2 O4 2.271(4) . ? Mn2 O5 2.304(5) . ? Mn2 O1 2.308(4) 5_666 ? Mn2 N2 2.374(5) . ? Mn2 O8 2.407(6) . ? O1 C2 1.435(7) . ? O1 Mn1 2.255(4) 5_666 ? O1 Mn2 2.308(4) 5_666 ? O2 C4 1.396(8) . ? O3A C6 1.470(14) . ? O3A H3A 0.8400 . ? O3B C6 1.23(2) . ? O3B H3B 0.8400 . ? O4 C8 1.415(7) . ? O4 Mn1 1.864(4) 5_666 ? O5 C10 1.424(9) . ? O5 H5 0.89(4) . ? O6 C12 1.421(10) . ? O6 H6 0.90(3) . ? O7 C13 1.319(7) . ? O8 C13 1.246(8) . ? O9 C20 1.266(8) . ? O10 C20 1.257(8) . ? N1 C3 1.465(9) . ? N1 C1 1.478(9) . ? N1 C5 1.480(9) . ? N2 C11 1.483(9) . ? N2 C7 1.485(9) . ? N2 C9 1.486(9) . ? C1 C2 1.544(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.412(10) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 H4A 0.9500 . ? C5 C6 1.507(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 H6C 0.9900 . ? C6 H6D 0.9900 . ? C7 C8 1.496(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.490(12) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.531(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.499(11) . ? C14 C15 1.370(11) . ? C14 C19 1.398(9) . ? C15 C16 1.415(12) . ? C15 H15A 0.9500 . ? C16 C17 1.412(11) . ? C16 H16A 0.9500 . ? C17 C18 1.369(12) . ? C17 H17A 0.9500 . ? C18 C19 1.412(11) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.506(9) . ? C21 C22 1.385(10) . ? C21 C26 1.388(11) . ? C22 C23 1.378(11) . ? C22 H22A 0.9500 . ? C23 C24 1.384(17) . ? C23 H23A 0.9500 . ? C24 C25 1.390(17) . ? C24 H24A 0.9500 . ? C25 C26 1.407(12) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C32A C31 1.39(2) . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B C31 1.46(6) . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C31 N31 1.21(3) . ? C31 O31 1.37(5) 2 ? C31 O31 1.37(5) . ? C31 C32B 1.46(6) 2 ? O31 H31 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O2 174.0(2) 5_666 . ? O4 Mn1 O7 94.20(19) 5_666 . ? O2 Mn1 O7 91.7(2) . . ? O4 Mn1 O1 81.50(17) 5_666 . ? O2 Mn1 O1 92.7(2) . . ? O7 Mn1 O1 175.34(19) . . ? O4 Mn1 O1 99.52(17) 5_666 5_666 ? O2 Mn1 O1 81.26(16) . 5_666 ? O7 Mn1 O1 96.6(2) . 5_666 ? O1 Mn1 O1 82.39(17) . 5_666 ? O4 Mn1 N1 98.95(19) 5_666 . ? O2 Mn1 N1 78.53(19) . . ? O7 Mn1 N1 99.9(2) . . ? O1 Mn1 N1 82.64(18) . . ? O1 Mn1 N1 154.16(18) 5_666 . ? O4 Mn1 Mn1 91.52(14) 5_666 5_666 ? O2 Mn1 Mn1 85.46(14) . 5_666 ? O7 Mn1 Mn1 134.11(18) . 5_666 ? O1 Mn1 Mn1 44.76(12) . 5_666 ? O1 Mn1 Mn1 37.63(11) 5_666 5_666 ? N1 Mn1 Mn1 124.09(15) . 5_666 ? O2 Mn2 O6 177.6(2) . . ? O2 Mn2 O4 89.80(18) . . ? O6 Mn2 O4 91.88(18) . . ? O2 Mn2 O5 90.28(17) . . ? O6 Mn2 O5 89.40(17) . . ? O4 Mn2 O5 143.09(17) . . ? O2 Mn2 O1 76.43(15) . 5_666 ? O6 Mn2 O1 102.73(17) . 5_666 ? O4 Mn2 O1 65.99(15) . 5_666 ? O5 Mn2 O1 148.89(18) . 5_666 ? O2 Mn2 N2 105.08(19) . . ? O6 Mn2 N2 77.1(2) . . ? O4 Mn2 N2 71.54(17) . . ? O5 Mn2 N2 72.85(19) . . ? O1 Mn2 N2 137.51(18) 5_666 . ? O2 Mn2 O8 78.08(19) . . ? O6 Mn2 O8 99.6(2) . . ? O4 Mn2 O8 141.25(15) . . ? O5 Mn2 O8 74.40(18) . . ? O1 Mn2 O8 75.37(16) 5_666 . ? N2 Mn2 O8 147.09(18) . . ? C2 O1 Mn1 112.0(4) . . ? C2 O1 Mn1 126.9(3) . 5_666 ? Mn1 O1 Mn1 97.61(17) . 5_666 ? C2 O1 Mn2 121.1(3) . 5_666 ? Mn1 O1 Mn2 103.50(17) . 5_666 ? Mn1 O1 Mn2 91.10(15) 5_666 5_666 ? C4 O2 Mn1 119.7(4) . . ? C4 O2 Mn2 129.8(4) . . ? Mn1 O2 Mn2 109.3(2) . . ? C6 O3A H3A 109.5 . . ? C6 O3B H3B 109.5 . . ? C8 O4 Mn1 130.3(4) . 5_666 ? C8 O4 Mn2 120.3(4) . . ? Mn1 O4 Mn2 108.02(19) 5_666 . ? C10 O5 Mn2 116.6(5) . . ? C10 O5 H5 110(5) . . ? Mn2 O5 H5 116(5) . . ? C12 O6 Mn2 110.3(4) . . ? C12 O6 H6 93(5) . . ? Mn2 O6 H6 119(5) . . ? C13 O7 Mn1 123.2(5) . . ? C13 O8 Mn2 128.2(5) . . ? C3 N1 C1 114.6(7) . . ? C3 N1 C5 110.8(7) . . ? C1 N1 C5 114.0(5) . . ? C3 N1 Mn1 102.7(4) . . ? C1 N1 Mn1 102.5(4) . . ? C5 N1 Mn1 111.2(5) . . ? C11 N2 C7 112.9(6) . . ? C11 N2 C9 111.6(5) . . ? C7 N2 C9 110.7(6) . . ? C11 N2 Mn2 108.1(5) . . ? C7 N2 Mn2 106.6(3) . . ? C9 N2 Mn2 106.5(4) . . ? N1 C1 C2 112.1(5) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? O1 C2 C1 110.4(5) . . ? O1 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? O1 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C4 C3 N1 115.2(6) . . ? C4 C3 H3C 108.5 . . ? N1 C3 H3C 108.5 . . ? C4 C3 H3D 108.5 . . ? N1 C3 H3D 108.5 . . ? H3C C3 H3D 107.5 . . ? O2 C4 C3 116.8(6) . . ? O2 C4 H4A 121.6 . . ? C3 C4 H4A 121.6 . . ? N1 C5 C6 117.9(8) . . ? N1 C5 H5A 107.8 . . ? C6 C5 H5A 107.8 . . ? N1 C5 H5B 107.8 . . ? C6 C5 H5B 107.8 . . ? H5A C5 H5B 107.2 . . ? O3B C6 O3A 30.0(10) . . ? O3B C6 C5 116.5(13) . . ? O3A C6 C5 104.8(7) . . ? O3B C6 H6A 80.8 . . ? O3A C6 H6A 110.8 . . ? C5 C6 H6A 110.8 . . ? O3B C6 H6B 124.1 . . ? O3A C6 H6B 110.8 . . ? C5 C6 H6B 110.8 . . ? H6A C6 H6B 108.9 . . ? O3B C6 H6C 108.2 . . ? O3A C6 H6C 136.8 . . ? C5 C6 H6C 108.2 . . ? H6A C6 H6C 30.4 . . ? H6B C6 H6C 82.6 . . ? O3B C6 H6D 108.2 . . ? O3A C6 H6D 87.6 . . ? C5 C6 H6D 108.2 . . ? H6A C6 H6D 130.1 . . ? H6B C6 H6D 25.7 . . ? H6C C6 H6D 107.3 . . ? N2 C7 C8 111.6(6) . . ? N2 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N2 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? O4 C8 C7 108.9(6) . . ? O4 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? O4 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? N2 C9 C10 111.2(6) . . ? N2 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? O5 C10 C9 108.5(6) . . ? O5 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? O5 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? N2 C11 C12 112.1(6) . . ? N2 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N2 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? O6 C12 C11 112.6(6) . . ? O6 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? O6 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? O8 C13 O7 127.1(7) . . ? O8 C13 C14 120.8(6) . . ? O7 C13 C14 111.8(6) . . ? C15 C14 C19 118.6(7) . . ? C15 C14 C13 121.7(6) . . ? C19 C14 C13 119.7(7) . . ? C14 C15 C16 123.3(7) . . ? C14 C15 H15A 118.4 . . ? C16 C15 H15A 118.4 . . ? C17 C16 C15 117.2(8) . . ? C17 C16 H16A 121.4 . . ? C15 C16 H16A 121.4 . . ? C18 C17 C16 120.0(8) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C19 121.6(7) . . ? C17 C18 H18A 119.2 . . ? C19 C18 H18A 119.2 . . ? C14 C19 C18 119.3(8) . . ? C14 C19 H19A 120.4 . . ? C18 C19 H19A 120.4 . . ? O10 C20 O9 125.2(6) . . ? O10 C20 C21 118.1(6) . . ? O9 C20 C21 116.6(6) . . ? C22 C21 C26 119.1(7) . . ? C22 C21 C20 120.2(7) . . ? C26 C21 C20 120.7(7) . . ? C23 C22 C21 121.0(9) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C22 C23 C24 120.0(10) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C25 120.4(9) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C24 C25 C26 118.9(11) . . ? C24 C25 H25A 120.5 . . ? C26 C25 H25A 120.5 . . ? C21 C26 C25 120.5(9) . . ? C21 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C31 C32A H32A 109.5 . . ? C31 C32A H32B 109.5 . . ? C31 C32A H32C 109.5 . . ? C31 C32B H32D 109.5 . . ? C31 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? N31 C31 O31 34.6(18) . 2 ? N31 C31 O31 34.6(18) . . ? O31 C31 O31 69(4) 2 . ? N31 C31 C32A 180.000(10) . . ? O31 C31 C32A 145.4(18) 2 . ? O31 C31 C32A 145.4(18) . . ? N31 C31 C32B 107(3) . 2 ? O31 C31 C32B 133(3) 2 2 ? O31 C31 C32B 79(3) . 2 ? C32A C31 C32B 73(3) . 2 ? N31 C31 C32B 107(3) . . ? O31 C31 C32B 79(3) 2 . ? O31 C31 C32B 133(3) . . ? C32A C31 C32B 73(3) . . ? C32B C31 C32B 146(5) 2 . ? C31 O31 H31 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O10 0.89(4) 1.82(5) 2.675(7) 161(8) . O6 H6 O9 0.90(3) 1.74(3) 2.589(7) 158(7) . O3A H3A O9 0.84 1.87 2.645(9) 153.4 6_566 _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 1.361 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.127