_publ_contact_author ; 'Annie K. Powell' ; _publ_contact_author_email powell@aoc.uni-karlsruhe.de _publ_contact_author_phone '+49 721 608 2135' _publ_requested_journal 'Cryst. Growth Design' _publ_section_title ; Influence of Water Ligands on Structural Diversity: From a 1D Linear Coordination Polymer to 3D Ferrimagnetic Diamondoid Metal-Organic Frameworks ; loop_ _publ_author_name _publ_author_address 'Sudarshana Mukherjee' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Yanhua Lan' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'George E. Kostakis' ; 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 Avenue 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 ; 'Annie K. Powell' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; data_msa441 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H44 Mn3 N4 O12' _chemical_formula_weight 1081.73 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 tetragonal _symmetry_space_group_name_H-M 'P 43' _symmetry_space_group_name_Hall 'P 4cw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 18.7991(2) _cell_length_b 18.7991(2) _cell_length_c 13.8136(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4881.81(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18760 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.03 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2220 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.796 _exptl_absorpt_correction_T_max 0.879 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2005)' _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 34044 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.14 _reflns_number_total 11063 _reflns_number_gt 10556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. The structure possesses non-crystallographic inversion symmetry, but close investigation using PLATON showed that P43 is the correct space group. Potential higher-symmetry space groups all gave very high R(int) values. ; _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^)+(0.0538P)^2^+1.5612P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 4855 Friedel pairs' _refine_ls_abs_structure_Flack 0.478(10) _refine_ls_number_reflns 11063 _refine_ls_number_parameters 645 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 -0.003872(17) 0.247051(19) 0.39332(2) 0.02339(8) Uani 1 1 d . . . Mn2 Mn 0.494593(17) 0.247591(18) 0.42784(2) 0.02223(8) Uani 1 1 d . . . Mn3 Mn 0.262543(18) 0.260143(19) 0.53474(3) 0.02577(8) Uani 1 1 d . . . O1 O -0.05547(8) 0.26274(9) 0.50547(12) 0.0264(3) Uani 1 1 d . . . C1 C -0.03302(12) 0.27198(11) 0.59493(17) 0.0237(4) Uani 1 1 d . . . C2 C 0.03930(12) 0.27364(11) 0.62339(17) 0.0228(4) Uani 1 1 d . . . C3 C 0.05689(14) 0.28837(13) 0.72004(19) 0.0316(5) Uani 1 1 d . . . H3A H 0.1055 0.2902 0.7388 0.038 Uiso 1 1 calc R . . C4 C 0.00450(14) 0.30021(14) 0.7885(2) 0.0377(6) Uani 1 1 d . . . H4A H 0.0169 0.3117 0.8533 0.045 Uiso 1 1 calc R . . C5 C -0.06639(14) 0.29515(14) 0.76145(19) 0.0356(6) Uani 1 1 d . . . H5A H -0.1022 0.3017 0.8091 0.043 Uiso 1 1 calc R . . C6 C -0.08637(12) 0.28079(12) 0.66692(17) 0.0274(5) Uani 1 1 d . . . C7 C 0.09879(11) 0.26032(11) 0.55529(18) 0.0244(5) Uani 1 1 d . . . O2 O 0.08742(8) 0.24579(9) 0.46646(12) 0.0264(3) Uani 1 1 d . . . O3 O 0.16118(8) 0.26341(10) 0.58936(13) 0.0323(4) Uani 1 1 d . . . C8 C -0.16286(13) 0.27263(14) 0.6380(2) 0.0344(5) Uani 1 1 d . . . H8A H -0.1727 0.2226 0.6233 0.052 Uiso 1 1 calc R . . H8B H -0.1723 0.3017 0.5805 0.052 Uiso 1 1 calc R . . H8C H -0.1935 0.2883 0.6912 0.052 Uiso 1 1 calc R . . O4 O 0.04589(8) 0.23031(9) 0.27866(12) 0.0272(3) Uani 1 1 d . . . C9 C 0.02131(11) 0.22537(11) 0.18959(16) 0.0218(4) Uani 1 1 d . . . C10 C -0.05129(11) 0.23044(11) 0.16258(16) 0.0223(4) Uani 1 1 d . . . C11 C -0.07114(12) 0.22024(12) 0.06577(18) 0.0286(5) Uani 1 1 d . . . H11A H -0.1200 0.2230 0.0486 0.034 Uiso 1 1 calc R . . C12 C -0.02179(13) 0.20629(13) -0.00485(19) 0.0323(5) Uani 1 1 d . . . H12A H -0.0363 0.1980 -0.0698 0.039 Uiso 1 1 calc R . . C13 C 0.05034(12) 0.20448(12) 0.02033(18) 0.0283(5) Uani 1 1 d . . . H13A H 0.0848 0.1968 -0.0289 0.034 Uiso 1 1 calc R . . C14 C 0.07272(11) 0.21355(11) 0.11444(17) 0.0239(4) Uani 1 1 d . . . C15 C -0.10846(12) 0.24678(11) 0.23292(17) 0.0236(4) Uani 1 1 d . . . O5 O -0.09575(8) 0.25203(9) 0.32349(12) 0.0276(3) Uani 1 1 d . . . O6 O -0.17051(8) 0.25588(8) 0.19994(12) 0.0267(3) Uani 1 1 d . . . C16 C 0.14966(12) 0.21004(14) 0.14271(18) 0.0323(5) Uani 1 1 d . . . H16A H 0.1577 0.1680 0.1833 0.048 Uiso 1 1 calc R . . H16B H 0.1624 0.2530 0.1790 0.048 Uiso 1 1 calc R . . H16C H 0.1791 0.2068 0.0843 0.048 Uiso 1 1 calc R . . O7 O 0.54994(8) 0.22190(9) 0.53421(13) 0.0282(3) Uani 1 1 d . . . C17 C 0.53227(12) 0.21876(11) 0.62715(16) 0.0233(4) Uani 1 1 d . . . C18 C 0.46259(12) 0.22548(11) 0.66449(17) 0.0240(4) Uani 1 1 d . . . C19 C 0.45086(13) 0.21631(12) 0.76435(19) 0.0310(5) Uani 1 1 d . . . H19A H 0.4038 0.2198 0.7890 0.037 Uiso 1 1 calc R . . C20 C 0.50600(14) 0.20245(14) 0.82703(19) 0.0345(5) Uani 1 1 d . . . H20A H 0.4971 0.1957 0.8941 0.041 Uiso 1 1 calc R . . C21 C 0.57495(13) 0.19850(12) 0.79086(19) 0.0319(5) Uani 1 1 d . . . H21A H 0.6132 0.1899 0.8343 0.038 Uiso 1 1 calc R . . C22 C 0.58929(12) 0.20671(12) 0.69343(18) 0.0269(5) Uani 1 1 d . . . C23 C 0.39979(12) 0.24090(11) 0.60254(17) 0.0236(4) Uani 1 1 d . . . O8 O 0.40551(8) 0.24478(9) 0.51054(12) 0.0261(3) Uani 1 1 d . . . O9 O 0.34005(8) 0.24949(9) 0.64277(13) 0.0292(3) Uani 1 1 d . . . C24 C 0.66324(13) 0.20259(17) 0.6545(2) 0.0411(6) Uani 1 1 d . . . H24A H 0.6970 0.1988 0.7084 0.062 Uiso 1 1 calc R . . H24B H 0.6736 0.2456 0.6169 0.062 Uiso 1 1 calc R . . H24C H 0.6677 0.1607 0.6127 0.062 Uiso 1 1 calc R . . O10 O 0.43646(8) 0.27226(9) 0.32546(12) 0.0267(3) Uani 1 1 d . . . C25 C 0.45185(12) 0.27918(11) 0.23244(17) 0.0237(5) Uani 1 1 d . . . C26 C 0.52073(12) 0.28016(11) 0.19276(17) 0.0248(4) Uani 1 1 d . . . C27 C 0.52941(14) 0.29420(13) 0.09294(19) 0.0337(5) Uani 1 1 d . . . H27A H 0.5759 0.2959 0.0659 0.040 Uiso 1 1 calc R . . C28 C 0.47114(16) 0.30545(14) 0.0345(2) 0.0412(6) Uani 1 1 d . . . H28A H 0.4775 0.3156 -0.0323 0.049 Uiso 1 1 calc R . . C29 C 0.40294(14) 0.30189(13) 0.0732(2) 0.0369(6) Uani 1 1 d . . . H29A H 0.3631 0.3088 0.0319 0.044 Uiso 1 1 calc R . . C30 C 0.39191(13) 0.28853(12) 0.16985(18) 0.0295(5) Uani 1 1 d . . . C31 C 0.58614(12) 0.26789(11) 0.25183(18) 0.0244(4) Uani 1 1 d . . . O11 O 0.58231(8) 0.25522(8) 0.34214(12) 0.0255(3) Uani 1 1 d . . . O12 O 0.64564(8) 0.27117(9) 0.20881(13) 0.0303(4) Uani 1 1 d . . . C32 C 0.31820(13) 0.28228(15) 0.2131(2) 0.0398(6) Uani 1 1 d . . . H32A H 0.2831 0.3007 0.1670 0.060 Uiso 1 1 calc R . . H32B H 0.3159 0.3099 0.2731 0.060 Uiso 1 1 calc R . . H32C H 0.3079 0.2322 0.2270 0.060 Uiso 1 1 calc R . . N1 N 0.01420(10) 0.36537(11) 0.37118(15) 0.0287(4) Uani 1 1 d . . . C33 C 0.08047(12) 0.39123(14) 0.35918(19) 0.0331(5) Uani 1 1 d . . . H33A H 0.1196 0.3593 0.3633 0.040 Uiso 1 1 calc R . . C34 C 0.09386(14) 0.46250(15) 0.3411(2) 0.0372(6) Uani 1 1 d . . . H34A H 0.1412 0.4791 0.3331 0.045 Uiso 1 1 calc R . . C35 C 0.03683(15) 0.50914(15) 0.3349(2) 0.0401(6) Uani 1 1 d . . . H35A H 0.0444 0.5582 0.3221 0.048 Uiso 1 1 calc R . . C36 C -0.03135(14) 0.48292(14) 0.3477(2) 0.0357(6) Uani 1 1 d . . . H36A H -0.0713 0.5137 0.3442 0.043 Uiso 1 1 calc R . . C37 C -0.04020(12) 0.41105(13) 0.36588(18) 0.0299(5) Uani 1 1 d . . . H37A H -0.0871 0.3934 0.3750 0.036 Uiso 1 1 calc R . . N2 N -0.01764(10) 0.12985(11) 0.41849(15) 0.0274(4) Uani 1 1 d . . . C38 C -0.08241(12) 0.10119(13) 0.43262(19) 0.0304(5) Uani 1 1 d . . . H38A H -0.1230 0.1312 0.4287 0.036 Uiso 1 1 calc R . . C39 C -0.09213(13) 0.02986(14) 0.4527(2) 0.0355(6) Uani 1 1 d . . . H39A H -0.1385 0.0110 0.4619 0.043 Uiso 1 1 calc R . . C40 C -0.03314(14) -0.01350(15) 0.4590(2) 0.0383(6) Uani 1 1 d . . . H40A H -0.0384 -0.0626 0.4734 0.046 Uiso 1 1 calc R . . C41 C 0.03397(13) 0.01530(14) 0.4441(2) 0.0359(6) Uani 1 1 d . . . H41A H 0.0752 -0.0137 0.4475 0.043 Uiso 1 1 calc R . . C42 C 0.03941(12) 0.08684(14) 0.42427(19) 0.0314(5) Uani 1 1 d . . . H42A H 0.0853 0.1067 0.4143 0.038 Uiso 1 1 calc R . . N3 N 0.51173(10) 0.36022(11) 0.46798(15) 0.0280(4) Uani 1 1 d . . . C43 C 0.45680(12) 0.40588(13) 0.47598(19) 0.0306(5) Uani 1 1 d . . . H43A H 0.4101 0.3889 0.4632 0.037 Uiso 1 1 calc R . . C44 C 0.46544(14) 0.47633(14) 0.5020(2) 0.0357(6) Uani 1 1 d . . . H44A H 0.4255 0.5071 0.5071 0.043 Uiso 1 1 calc R . . C45 C 0.53346(14) 0.50126(14) 0.5204(2) 0.0382(6) Uani 1 1 d . . . H45A H 0.5409 0.5494 0.5388 0.046 Uiso 1 1 calc R . . C46 C 0.59047(13) 0.45487(14) 0.5117(2) 0.0362(6) Uani 1 1 d . . . H46A H 0.6376 0.4709 0.5233 0.043 Uiso 1 1 calc R . . C47 C 0.57763(12) 0.38516(14) 0.48586(19) 0.0325(5) Uani 1 1 d . . . H47A H 0.6168 0.3535 0.4805 0.039 Uiso 1 1 calc R . . N4 N 0.48372(9) 0.13533(10) 0.38423(14) 0.0247(4) Uani 1 1 d . . . C48 C 0.41964(12) 0.10647(12) 0.36540(17) 0.0272(5) Uani 1 1 d . . . H48A H 0.3786 0.1357 0.3703 0.033 Uiso 1 1 calc R . . C49 C 0.41122(13) 0.03630(14) 0.33930(19) 0.0328(5) Uani 1 1 d . . . H49A H 0.3653 0.0174 0.3266 0.039 Uiso 1 1 calc R . . C50 C 0.47139(13) -0.00631(14) 0.3319(2) 0.0335(5) Uani 1 1 d . . . H50A H 0.4672 -0.0550 0.3146 0.040 Uiso 1 1 calc R . . C51 C 0.53712(13) 0.02306(13) 0.3500(2) 0.0327(5) Uani 1 1 d . . . H51A H 0.5790 -0.0050 0.3450 0.039 Uiso 1 1 calc R . . C52 C 0.54141(12) 0.09373(12) 0.37564(17) 0.0269(5) Uani 1 1 d . . . H52A H 0.5869 0.1138 0.3877 0.032 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 0.01565(14) 0.02955(18) 0.02495(17) 0.00116(13) -0.00022(13) 0.00189(12) Mn2 0.01543(14) 0.02672(17) 0.02455(17) -0.00201(13) -0.00217(13) 0.00174(12) Mn3 0.02454(17) 0.02811(17) 0.02466(15) -0.00078(14) -0.00060(14) -0.00153(13) O1 0.0186(7) 0.0346(9) 0.0260(8) -0.0013(7) 0.0018(6) 0.0027(6) C1 0.0237(10) 0.0143(9) 0.0330(12) 0.0031(8) 0.0044(9) 0.0000(8) C2 0.0239(10) 0.0173(9) 0.0273(11) 0.0026(8) -0.0011(8) -0.0044(8) C3 0.0323(12) 0.0311(12) 0.0314(12) 0.0005(10) -0.0005(10) -0.0072(10) C4 0.0474(15) 0.0396(14) 0.0261(12) -0.0034(11) 0.0018(11) -0.0072(11) C5 0.0395(14) 0.0341(13) 0.0331(13) 0.0019(10) 0.0110(11) -0.0018(10) C6 0.0282(11) 0.0223(10) 0.0318(12) 0.0053(9) 0.0063(9) 0.0011(8) C7 0.0215(10) 0.0170(9) 0.0348(13) 0.0025(9) -0.0014(9) -0.0012(8) O2 0.0196(7) 0.0319(9) 0.0277(8) -0.0002(7) -0.0019(6) 0.0008(6) O3 0.0201(8) 0.0421(10) 0.0346(9) -0.0038(8) -0.0050(7) -0.0037(7) C8 0.0271(12) 0.0366(13) 0.0395(14) 0.0081(11) 0.0108(10) 0.0029(10) O4 0.0181(7) 0.0387(9) 0.0250(8) 0.0016(7) -0.0006(6) 0.0036(6) C9 0.0233(10) 0.0168(9) 0.0254(11) 0.0039(8) -0.0014(9) -0.0001(8) C10 0.0213(10) 0.0166(9) 0.0289(12) 0.0021(8) -0.0030(8) -0.0014(8) C11 0.0256(11) 0.0264(11) 0.0338(12) 0.0005(9) -0.0049(9) -0.0038(9) C12 0.0353(13) 0.0327(12) 0.0289(12) -0.0043(10) -0.0043(10) -0.0038(10) C13 0.0283(11) 0.0272(11) 0.0293(12) 0.0012(9) 0.0053(9) -0.0021(9) C14 0.0221(10) 0.0192(10) 0.0305(12) 0.0068(8) 0.0023(9) -0.0012(8) C15 0.0214(10) 0.0172(10) 0.0321(12) 0.0010(8) -0.0038(9) -0.0021(8) O5 0.0180(7) 0.0327(9) 0.0319(9) 0.0004(7) 0.0012(6) 0.0026(6) O6 0.0181(7) 0.0275(8) 0.0345(9) -0.0019(7) -0.0034(6) -0.0008(6) C16 0.0217(11) 0.0456(14) 0.0295(12) 0.0105(11) 0.0044(9) 0.0028(10) O7 0.0184(7) 0.0383(9) 0.0280(8) -0.0045(7) -0.0035(6) 0.0049(6) C17 0.0232(10) 0.0196(10) 0.0272(11) -0.0028(8) -0.0054(9) -0.0015(8) C18 0.0240(11) 0.0199(10) 0.0282(12) -0.0021(8) -0.0021(9) -0.0005(8) C19 0.0305(12) 0.0267(11) 0.0358(13) 0.0033(10) 0.0040(10) -0.0009(9) C20 0.0407(14) 0.0339(13) 0.0289(12) 0.0026(10) -0.0005(10) 0.0022(10) C21 0.0348(12) 0.0289(11) 0.0320(12) -0.0028(10) -0.0103(10) 0.0009(9) C22 0.0253(11) 0.0251(11) 0.0303(12) -0.0041(9) -0.0067(9) 0.0017(9) C23 0.0218(10) 0.0179(10) 0.0311(11) -0.0026(9) -0.0018(9) -0.0016(8) O8 0.0171(7) 0.0315(8) 0.0295(9) -0.0017(7) -0.0027(6) 0.0013(6) O9 0.0201(8) 0.0352(9) 0.0322(9) -0.0004(7) 0.0007(7) -0.0001(7) C24 0.0222(12) 0.0636(18) 0.0376(14) -0.0063(13) -0.0088(10) 0.0067(12) O10 0.0182(7) 0.0333(9) 0.0288(8) 0.0020(7) -0.0048(6) 0.0017(6) C25 0.0240(10) 0.0147(9) 0.0324(12) -0.0018(8) -0.0064(9) -0.0008(8) C26 0.0281(11) 0.0165(9) 0.0299(12) -0.0001(8) -0.0031(9) 0.0008(8) C27 0.0377(13) 0.0294(12) 0.0341(13) 0.0009(10) 0.0012(11) 0.0009(10) C28 0.0572(17) 0.0384(14) 0.0281(12) 0.0040(11) -0.0046(12) 0.0046(12) C29 0.0405(14) 0.0319(12) 0.0384(14) 0.0017(11) -0.0160(11) 0.0000(11) C30 0.0327(12) 0.0227(10) 0.0330(12) -0.0013(9) -0.0113(10) -0.0028(9) C31 0.0232(10) 0.0172(10) 0.0327(12) -0.0017(8) 0.0005(9) -0.0017(8) O11 0.0206(7) 0.0290(8) 0.0269(8) -0.0020(6) -0.0023(6) 0.0004(6) O12 0.0234(8) 0.0330(9) 0.0345(9) 0.0051(7) 0.0040(7) -0.0022(7) C32 0.0251(12) 0.0414(14) 0.0531(16) 0.0034(13) -0.0136(11) -0.0018(11) N1 0.0208(9) 0.0352(11) 0.0302(10) 0.0025(8) -0.0003(8) 0.0004(8) C33 0.0215(11) 0.0398(13) 0.0381(13) 0.0074(11) 0.0001(10) 0.0012(9) C34 0.0275(12) 0.0439(15) 0.0402(15) 0.0120(11) -0.0015(10) -0.0062(10) C35 0.0427(15) 0.0336(13) 0.0439(16) 0.0098(12) -0.0070(12) -0.0026(11) C36 0.0279(12) 0.0386(14) 0.0407(14) 0.0034(11) -0.0056(10) 0.0052(10) C37 0.0215(10) 0.0341(12) 0.0340(13) -0.0003(10) -0.0028(9) 0.0020(9) N2 0.0201(9) 0.0313(10) 0.0306(10) -0.0005(8) -0.0032(7) 0.0025(8) C38 0.0196(10) 0.0343(12) 0.0373(13) 0.0047(10) -0.0027(10) 0.0034(9) C39 0.0234(11) 0.0379(14) 0.0451(15) 0.0066(11) -0.0040(10) -0.0030(10) C40 0.0364(14) 0.0307(13) 0.0478(15) 0.0046(11) -0.0059(12) 0.0004(11) C41 0.0289(12) 0.0357(13) 0.0431(15) -0.0023(11) -0.0043(11) 0.0087(10) C42 0.0210(10) 0.0384(13) 0.0347(12) -0.0018(11) -0.0013(10) 0.0035(9) N3 0.0192(9) 0.0328(10) 0.0322(10) -0.0038(8) 0.0009(8) 0.0005(7) C43 0.0194(10) 0.0342(12) 0.0381(13) 0.0007(10) 0.0021(9) -0.0001(9) C44 0.0274(12) 0.0344(13) 0.0454(15) -0.0033(11) 0.0010(11) 0.0055(10) C45 0.0356(13) 0.0325(13) 0.0466(16) -0.0030(12) 0.0009(12) -0.0062(11) C46 0.0232(11) 0.0425(14) 0.0428(15) -0.0083(12) 0.0002(10) -0.0063(10) C47 0.0191(11) 0.0423(14) 0.0361(13) -0.0067(11) -0.0012(9) 0.0010(10) N4 0.0185(8) 0.0286(10) 0.0270(10) 0.0007(8) 0.0009(7) 0.0014(7) C48 0.0195(10) 0.0307(11) 0.0313(12) -0.0019(9) 0.0020(9) 0.0016(8) C49 0.0251(11) 0.0368(13) 0.0364(14) -0.0028(10) 0.0013(10) -0.0045(10) C50 0.0308(12) 0.0273(12) 0.0423(14) -0.0041(10) 0.0030(11) 0.0006(10) C51 0.0242(11) 0.0329(13) 0.0412(14) 0.0011(11) 0.0039(10) 0.0062(9) C52 0.0197(10) 0.0303(11) 0.0307(12) 0.0024(9) 0.0017(9) 0.0027(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 O1 1.8514(16) . ? Mn1 O4 1.8663(17) . ? Mn1 O5 1.9807(16) . ? Mn1 O2 1.9916(16) . ? Mn1 N2 2.245(2) . ? Mn1 N1 2.271(2) . ? Mn2 O10 1.8465(16) . ? Mn2 O7 1.8641(17) . ? Mn2 O8 2.0279(16) . ? Mn2 O11 2.0350(16) . ? Mn2 N4 2.204(2) . ? Mn2 N3 2.212(2) . ? Mn3 O3 2.0505(17) . ? Mn3 O6 2.0560(16) 4 ? Mn3 O12 2.0648(17) 4_565 ? Mn3 O9 2.0953(17) . ? O1 C1 1.317(3) . ? C1 C2 1.415(3) . ? C1 C6 1.422(3) . ? C2 C3 1.403(3) . ? C2 C7 1.483(3) . ? C3 C4 1.383(4) . ? C3 H3A 0.9500 . ? C4 C5 1.387(4) . ? C4 H4A 0.9500 . ? C5 C6 1.385(4) . ? C5 H5A 0.9500 . ? C6 C8 1.500(3) . ? C7 O3 1.265(3) . ? C7 O2 1.275(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O4 C9 1.317(3) . ? C9 C10 1.418(3) . ? C9 C14 1.436(3) . ? C10 C11 1.402(3) . ? C10 C15 1.481(3) . ? C11 C12 1.372(4) . ? C11 H11A 0.9500 . ? C12 C13 1.400(3) . ? C12 H12A 0.9500 . ? C13 C14 1.377(3) . ? C13 H13A 0.9500 . ? C14 C16 1.500(3) . ? C15 O6 1.264(3) . ? C15 O5 1.277(3) . ? O6 Mn3 2.0559(16) 3_554 ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O7 C17 1.327(3) . ? C17 C18 1.413(3) . ? C17 C22 1.428(3) . ? C18 C19 1.407(3) . ? C18 C23 1.487(3) . ? C19 C20 1.376(4) . ? C19 H19A 0.9500 . ? C20 C21 1.391(4) . ? C20 H20A 0.9500 . ? C21 C22 1.381(4) . ? C21 H21A 0.9500 . ? C22 C24 1.492(3) . ? C23 O9 1.263(3) . ? C23 O8 1.278(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? O10 C25 1.324(3) . ? C25 C26 1.406(3) . ? C25 C30 1.431(3) . ? C26 C27 1.413(3) . ? C26 C31 1.494(3) . ? C27 C28 1.377(4) . ? C27 H27A 0.9500 . ? C28 C29 1.391(4) . ? C28 H28A 0.9500 . ? C29 C30 1.375(4) . ? C29 H29A 0.9500 . ? C30 C32 1.513(4) . ? C31 O12 1.268(3) . ? C31 O11 1.272(3) . ? O12 Mn3 2.0648(17) 3_654 ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N1 C37 1.337(3) . ? N1 C33 1.348(3) . ? C33 C34 1.386(4) . ? C33 H33A 0.9500 . ? C34 C35 1.388(4) . ? C34 H34A 0.9500 . ? C35 C36 1.385(4) . ? C35 H35A 0.9500 . ? C36 C37 1.384(4) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? N2 C38 1.346(3) . ? N2 C42 1.346(3) . ? C38 C39 1.381(3) . ? C38 H38A 0.9500 . ? C39 C40 1.379(4) . ? C39 H39A 0.9500 . ? C40 C41 1.388(3) . ? C40 H40A 0.9500 . ? C41 C42 1.376(4) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? N3 C43 1.347(3) . ? N3 C47 1.348(3) . ? C43 C44 1.382(4) . ? C43 H43A 0.9500 . ? C44 C45 1.386(3) . ? C44 H44A 0.9500 . ? C45 C46 1.387(4) . ? C45 H45A 0.9500 . ? C46 C47 1.379(4) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? N4 C52 1.342(3) . ? N4 C48 1.347(3) . ? C48 C49 1.377(3) . ? C48 H48A 0.9500 . ? C49 C50 1.390(3) . ? C49 H49A 0.9500 . ? C50 C51 1.377(3) . ? C50 H50A 0.9500 . ? C51 C52 1.377(3) . ? C51 H51A 0.9500 . ? C52 H52A 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 O1 Mn1 O4 178.44(7) . . ? O1 Mn1 O5 86.74(7) . . ? O4 Mn1 O5 91.82(7) . . ? O1 Mn1 O2 91.65(7) . . ? O4 Mn1 O2 89.81(7) . . ? O5 Mn1 O2 177.59(7) . . ? O1 Mn1 N2 88.07(7) . . ? O4 Mn1 N2 91.36(7) . . ? O5 Mn1 N2 91.21(7) . . ? O2 Mn1 N2 90.52(7) . . ? O1 Mn1 N1 92.01(7) . . ? O4 Mn1 N1 88.62(7) . . ? O5 Mn1 N1 91.06(7) . . ? O2 Mn1 N1 87.20(7) . . ? N2 Mn1 N1 177.72(7) . . ? O10 Mn2 O7 177.64(7) . . ? O10 Mn2 O8 87.09(7) . . ? O7 Mn2 O8 90.59(7) . . ? O10 Mn2 O11 90.94(7) . . ? O7 Mn2 O11 91.40(7) . . ? O8 Mn2 O11 177.10(7) . . ? O10 Mn2 N4 88.64(7) . . ? O7 Mn2 N4 91.10(7) . . ? O8 Mn2 N4 93.01(7) . . ? O11 Mn2 N4 89.06(7) . . ? O10 Mn2 N3 92.17(8) . . ? O7 Mn2 N3 88.23(7) . . ? O8 Mn2 N3 90.23(7) . . ? O11 Mn2 N3 87.73(7) . . ? N4 Mn2 N3 176.71(7) . . ? O3 Mn3 O6 100.22(7) . 4 ? O3 Mn3 O12 103.55(7) . 4_565 ? O6 Mn3 O12 114.73(7) 4 4_565 ? O3 Mn3 O9 112.77(7) . . ? O6 Mn3 O9 111.71(7) 4 . ? O12 Mn3 O9 112.91(7) 4_565 . ? C1 O1 Mn1 129.65(14) . . ? O1 C1 C2 124.8(2) . . ? O1 C1 C6 116.4(2) . . ? C2 C1 C6 118.7(2) . . ? C3 C2 C1 119.7(2) . . ? C3 C2 C7 117.3(2) . . ? C1 C2 C7 123.0(2) . . ? C4 C3 C2 121.0(2) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C3 C4 C5 119.3(2) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C6 C5 C4 121.8(2) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C5 C6 C1 119.4(2) . . ? C5 C6 C8 122.1(2) . . ? C1 C6 C8 118.5(2) . . ? O3 C7 O2 121.6(2) . . ? O3 C7 C2 117.1(2) . . ? O2 C7 C2 121.34(19) . . ? C7 O2 Mn1 129.06(15) . . ? C7 O3 Mn3 136.33(17) . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 O4 Mn1 128.95(14) . . ? O4 C9 C10 125.4(2) . . ? O4 C9 C14 116.74(19) . . ? C10 C9 C14 117.9(2) . . ? C11 C10 C9 119.9(2) . . ? C11 C10 C15 117.5(2) . . ? C9 C10 C15 122.7(2) . . ? C12 C11 C10 121.6(2) . . ? C12 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C11 C12 C13 118.9(2) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C14 C13 C12 121.8(2) . . ? C14 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? C13 C14 C9 119.8(2) . . ? C13 C14 C16 122.3(2) . . ? C9 C14 C16 117.9(2) . . ? O6 C15 O5 121.0(2) . . ? O6 C15 C10 117.5(2) . . ? O5 C15 C10 121.5(2) . . ? C15 O5 Mn1 129.53(15) . . ? C15 O6 Mn3 124.01(15) . 3_554 ? 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 . . ? C17 O7 Mn2 129.35(14) . . ? O7 C17 C18 125.5(2) . . ? O7 C17 C22 116.1(2) . . ? C18 C17 C22 118.4(2) . . ? C19 C18 C17 119.5(2) . . ? C19 C18 C23 117.6(2) . . ? C17 C18 C23 122.9(2) . . ? C20 C19 C18 121.5(2) . . ? C20 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? C19 C20 C21 119.1(2) . . ? C19 C20 H20A 120.5 . . ? C21 C20 H20A 120.5 . . ? C22 C21 C20 121.7(2) . . ? C22 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? C21 C22 C17 119.7(2) . . ? C21 C22 C24 121.8(2) . . ? C17 C22 C24 118.5(2) . . ? O9 C23 O8 120.3(2) . . ? O9 C23 C18 118.5(2) . . ? O8 C23 C18 121.1(2) . . ? C23 O8 Mn2 129.15(15) . . ? C23 O9 Mn3 108.49(15) . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 O10 Mn2 129.70(15) . . ? O10 C25 C26 125.5(2) . . ? O10 C25 C30 115.2(2) . . ? C26 C25 C30 119.2(2) . . ? C25 C26 C27 119.3(2) . . ? C25 C26 C31 122.9(2) . . ? C27 C26 C31 117.8(2) . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27A 119.7 . . ? C26 C27 H27A 119.7 . . ? C27 C28 C29 120.0(3) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 121.4(2) . . ? C30 C29 H29A 119.3 . . ? C28 C29 H29A 119.3 . . ? C29 C30 C25 119.4(2) . . ? C29 C30 C32 122.4(2) . . ? C25 C30 C32 118.2(2) . . ? O12 C31 O11 121.2(2) . . ? O12 C31 C26 117.6(2) . . ? O11 C31 C26 121.2(2) . . ? C31 O11 Mn2 129.02(15) . . ? C31 O12 Mn3 120.98(16) . 3_654 ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C37 N1 C33 117.9(2) . . ? C37 N1 Mn1 121.47(16) . . ? C33 N1 Mn1 120.54(16) . . ? N1 C33 C34 122.6(2) . . ? N1 C33 H33A 118.7 . . ? C34 C33 H33A 118.7 . . ? C33 C34 C35 118.8(2) . . ? C33 C34 H34A 120.6 . . ? C35 C34 H34A 120.6 . . ? C36 C35 C34 118.8(2) . . ? C36 C35 H35A 120.6 . . ? C34 C35 H35A 120.6 . . ? C37 C36 C35 118.8(2) . . ? C37 C36 H36A 120.6 . . ? C35 C36 H36A 120.6 . . ? N1 C37 C36 123.0(2) . . ? N1 C37 H37A 118.5 . . ? C36 C37 H37A 118.5 . . ? C38 N2 C42 118.2(2) . . ? C38 N2 Mn1 121.31(16) . . ? C42 N2 Mn1 120.46(16) . . ? N2 C38 C39 122.5(2) . . ? N2 C38 H38A 118.7 . . ? C39 C38 H38A 118.7 . . ? C40 C39 C38 118.7(2) . . ? C40 C39 H39A 120.7 . . ? C38 C39 H39A 120.7 . . ? C39 C40 C41 119.4(2) . . ? C39 C40 H40A 120.3 . . ? C41 C40 H40A 120.3 . . ? C42 C41 C40 118.6(2) . . ? C42 C41 H41A 120.7 . . ? C40 C41 H41A 120.7 . . ? N2 C42 C41 122.7(2) . . ? N2 C42 H42A 118.7 . . ? C41 C42 H42A 118.7 . . ? C43 N3 C47 117.9(2) . . ? C43 N3 Mn2 121.25(16) . . ? C47 N3 Mn2 120.85(16) . . ? N3 C43 C44 122.8(2) . . ? N3 C43 H43A 118.6 . . ? C44 C43 H43A 118.6 . . ? C43 C44 C45 118.7(2) . . ? C43 C44 H44A 120.6 . . ? C45 C44 H44A 120.6 . . ? C44 C45 C46 119.0(2) . . ? C44 C45 H45A 120.5 . . ? C46 C45 H45A 120.5 . . ? C47 C46 C45 119.0(2) . . ? C47 C46 H46A 120.5 . . ? C45 C46 H46A 120.5 . . ? N3 C47 C46 122.6(2) . . ? N3 C47 H47A 118.7 . . ? C46 C47 H47A 118.7 . . ? C52 N4 C48 118.1(2) . . ? C52 N4 Mn2 120.46(15) . . ? C48 N4 Mn2 121.44(15) . . ? N4 C48 C49 122.7(2) . . ? N4 C48 H48A 118.7 . . ? C49 C48 H48A 118.7 . . ? C48 C49 C50 118.5(2) . . ? C48 C49 H49A 120.7 . . ? C50 C49 H49A 120.7 . . ? C51 C50 C49 119.1(2) . . ? C51 C50 H50A 120.5 . . ? C49 C50 H50A 120.5 . . ? C52 C51 C50 119.1(2) . . ? C52 C51 H51A 120.5 . . ? C50 C51 H51A 120.5 . . ? N4 C52 C51 122.5(2) . . ? N4 C52 H52A 118.7 . . ? C51 C52 H52A 118.7 . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.024 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.084 ################################################################### data_msa262 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H51 Mn3 N4 O14' _chemical_formula_weight 1132.80 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 tetragonal _symmetry_space_group_name_H-M 'I 41' _symmetry_space_group_name_Hall 'I 4bw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-y, x+1/2, z+1/4' 'y+1/2, -x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1, z+1' '-y+1/2, x+1, z+3/4' 'y+1, -x+1/2, z+5/4' _cell_length_a 18.9660(7) _cell_length_b 18.9660(7) _cell_length_c 13.9262(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5009.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9359 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 27.99 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8218 _exptl_absorpt_correction_T_max 0.9155 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2005)' _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 13860 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.64 _reflns_number_total 4687 _reflns_number_gt 4452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. The large residual electron density peak is either side of Mn(2), which lies on a two-fold axis and is ligated by a methanol oxygen which is disordered either side of the axis. Mn(2) is therefore itself probably slightly displaced from the axis, and the large difference peak reflects this. Attempts to refine Mn(2) slightly off the twofold axis were unsuccessful. ; _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^)+(0.0737P)^2^+17.4900P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.31(3) _refine_ls_number_reflns 4687 _refine_ls_number_parameters 348 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1424 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.50144(4) 0.24147(4) 0.33684(6) 0.03191(19) Uani 1 1 d . . . Mn2 Mn 0.5000 0.5000 0.18168(8) 0.0378(3) Uani 1 2 d S . . O1 O 0.47212(19) 0.18628(18) 0.2306(2) 0.0364(8) Uani 1 1 d . . . C1 C 0.4653(2) 0.2071(3) 0.1402(3) 0.0303(10) Uani 1 1 d . . . C2 C 0.4694(2) 0.2777(3) 0.1089(3) 0.0330(11) Uani 1 1 d . A . C3 C 0.4576(3) 0.2920(3) 0.0120(4) 0.0434(13) Uani 1 1 d . . . H3A H 0.4589 0.3396 -0.0091 0.052 Uiso 1 1 calc R . . C4 C 0.4442(3) 0.2400(3) -0.0541(4) 0.0466(14) Uani 1 1 d . . . H4A H 0.4371 0.2517 -0.1198 0.056 Uiso 1 1 calc R . . C5 C 0.4412(3) 0.1702(3) -0.0244(4) 0.0459(13) Uani 1 1 d . . . C6 C 0.4513(3) 0.1549(3) 0.0716(4) 0.0416(12) Uani 1 1 d . . . H6A H 0.4487 0.1072 0.0919 0.050 Uiso 1 1 calc R . . C7 C 0.4848(2) 0.3375(3) 0.1751(4) 0.0342(10) Uani 1 1 d . . . O2 O 0.49811(18) 0.32781(17) 0.2627(3) 0.0368(8) Uani 1 1 d . A . O3 O 0.4845(3) 0.3983(2) 0.1396(3) 0.0611(12) Uani 1 1 d . A . C8 C 0.4264(4) 0.1120(4) -0.0971(5) 0.069(2) Uani 1 1 d . . . H8A H 0.4261 0.0663 -0.0644 0.104 Uiso 1 1 calc R . . H8B H 0.4632 0.1122 -0.1465 0.104 Uiso 1 1 calc R . . H8C H 0.3804 0.1202 -0.1272 0.104 Uiso 1 1 calc R . . O4 O 0.53011(18) 0.29450(18) 0.4426(3) 0.0382(8) Uani 1 1 d . . . C9 C 0.5351(2) 0.2740(3) 0.5338(4) 0.0345(11) Uani 1 1 d . . . C10 C 0.5297(2) 0.2037(3) 0.5654(4) 0.0353(11) Uani 1 1 d . . . C11 C 0.5401(2) 0.1890(3) 0.6643(4) 0.0384(11) Uani 1 1 d . . . H11A H 0.5379 0.1415 0.6855 0.046 Uiso 1 1 calc R . . C12 C 0.5531(3) 0.2403(3) 0.7293(4) 0.0470(14) Uani 1 1 d . . . H12A H 0.5598 0.2285 0.7950 0.056 Uiso 1 1 calc R . . C13 C 0.5564(3) 0.3106(3) 0.6999(4) 0.0457(14) Uani 1 1 d . . . C14 C 0.5486(3) 0.3271(3) 0.6030(4) 0.0426(13) Uani 1 1 d . . . H14A H 0.5523 0.3748 0.5829 0.051 Uiso 1 1 calc R . . C15 C 0.5149(2) 0.1438(3) 0.5004(4) 0.0347(11) Uani 1 1 d . . . O5 O 0.50550(18) 0.15413(17) 0.4101(3) 0.0353(8) Uani 1 1 d . . . O6 O 0.5131(2) 0.08233(19) 0.5330(3) 0.0438(9) Uani 1 1 d . . . C16 C 0.5693(4) 0.3690(4) 0.7719(5) 0.0660(19) Uani 1 1 d . . . H16A H 0.5699 0.4145 0.7386 0.099 Uiso 1 1 calc R . . H16B H 0.6148 0.3614 0.8036 0.099 Uiso 1 1 calc R . . H16C H 0.5316 0.3689 0.8200 0.099 Uiso 1 1 calc R . . N1 N 0.6167(2) 0.2277(2) 0.2902(3) 0.0352(9) Uani 1 1 d . . . C17 C 0.6467(3) 0.1645(3) 0.2772(4) 0.0380(11) Uani 1 1 d . . . H17A H 0.6189 0.1237 0.2884 0.046 Uiso 1 1 calc R . . C18 C 0.7153(3) 0.1554(3) 0.2485(4) 0.0406(12) Uani 1 1 d . . . H18A H 0.7345 0.1095 0.2411 0.049 Uiso 1 1 calc R . . C19 C 0.7562(3) 0.2149(3) 0.2305(4) 0.0406(12) Uani 1 1 d . . . H19A H 0.8034 0.2106 0.2084 0.049 Uiso 1 1 calc R . . C20 C 0.7264(3) 0.2807(3) 0.2457(4) 0.0364(11) Uani 1 1 d . . . H20A H 0.7533 0.3224 0.2360 0.044 Uiso 1 1 calc R . . C21 C 0.6571(3) 0.2847(3) 0.2751(4) 0.0339(10) Uani 1 1 d . . . H21A H 0.6371 0.3300 0.2852 0.041 Uiso 1 1 calc R . . N2 N 0.3869(2) 0.2622(2) 0.3822(3) 0.0334(9) Uani 1 1 d . . . C22 C 0.3413(3) 0.2087(2) 0.3954(3) 0.0335(10) Uani 1 1 d . . . H22A H 0.3574 0.1619 0.3847 0.040 Uiso 1 1 calc R . . C23 C 0.2720(3) 0.2188(2) 0.4240(3) 0.0336(11) Uani 1 1 d . . . H23A H 0.2416 0.1796 0.4336 0.040 Uiso 1 1 calc R . . C24 C 0.2482(3) 0.2857(3) 0.4380(4) 0.0394(11) Uani 1 1 d . . . H24A H 0.2008 0.2939 0.4568 0.047 Uiso 1 1 calc R . . C25 C 0.2942(3) 0.3419(3) 0.4245(4) 0.0383(11) Uani 1 1 d . . . H25A H 0.2791 0.3890 0.4347 0.046 Uiso 1 1 calc R . . C26 C 0.3622(3) 0.3273(3) 0.3959(4) 0.0387(12) Uani 1 1 d . . . H26A H 0.3933 0.3658 0.3853 0.046 Uiso 1 1 calc R . . O7 O 0.4567(3) 0.5120(4) 0.0301(5) 0.0377(16) Uani 0.50 1 d PD A -1 H7 H 0.411(2) 0.491(3) 0.009(4) 0.045 Uiso 1 1 d D B -1 C27 C 0.5000 0.5000 -0.0416(5) 0.058(3) Uani 1 2 d S . . H27A H 0.5268 0.4568 -0.0290 0.087 Uiso 0.50 1 calc PR A . H27B H 0.5326 0.5398 -0.0482 0.087 Uiso 0.50 1 calc PR . . H27C H 0.4729 0.4945 -0.1011 0.087 Uiso 0.50 1 calc PR . . O21 O 0.4988(5) 0.4506(6) 0.4612(7) 0.077(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0354(4) 0.0333(4) 0.0270(3) -0.0043(3) -0.0015(3) -0.0061(3) Mn2 0.0399(6) 0.0337(6) 0.0398(6) 0.000 0.000 0.0053(5) O1 0.046(2) 0.0310(18) 0.0322(18) -0.0072(14) -0.0058(15) -0.0056(15) C1 0.020(2) 0.047(3) 0.024(2) -0.007(2) -0.0005(17) -0.0044(19) C2 0.018(2) 0.054(3) 0.027(3) -0.008(2) 0.0000(17) 0.0044(19) C3 0.030(3) 0.055(3) 0.045(3) 0.001(3) 0.002(2) -0.001(2) C4 0.037(3) 0.076(4) 0.027(3) -0.005(3) -0.008(2) -0.004(3) C5 0.039(3) 0.061(4) 0.037(3) -0.018(3) -0.003(2) -0.001(3) C6 0.040(3) 0.044(3) 0.041(3) -0.009(2) -0.002(2) 0.003(2) C7 0.022(2) 0.042(3) 0.038(3) -0.002(2) 0.000(2) 0.0007(18) O2 0.043(2) 0.0290(17) 0.039(2) -0.0025(14) 0.0009(16) -0.0020(14) O3 0.086(3) 0.044(2) 0.053(3) 0.0033(19) -0.025(2) 0.007(2) C8 0.091(5) 0.076(5) 0.040(3) -0.018(3) -0.018(3) 0.002(4) O4 0.0411(19) 0.0392(19) 0.0342(18) -0.0129(16) -0.0006(15) -0.0098(15) C9 0.023(2) 0.050(3) 0.031(3) -0.013(2) -0.0003(19) 0.003(2) C10 0.017(2) 0.049(3) 0.040(3) -0.010(2) -0.0001(18) 0.0014(19) C11 0.028(2) 0.057(3) 0.029(3) -0.003(2) -0.0009(19) 0.003(2) C12 0.044(3) 0.063(4) 0.033(3) -0.008(3) -0.003(2) 0.008(3) C13 0.035(3) 0.064(4) 0.038(3) -0.027(3) -0.009(2) 0.011(2) C14 0.032(3) 0.045(3) 0.050(3) -0.015(2) -0.002(2) 0.005(2) C15 0.021(2) 0.047(3) 0.036(3) -0.001(2) -0.0052(18) -0.0005(19) O5 0.0392(18) 0.0336(17) 0.0331(18) -0.0012(14) -0.0033(14) -0.0044(14) O6 0.057(2) 0.038(2) 0.0369(19) 0.0044(16) -0.0092(17) -0.0042(17) C16 0.075(4) 0.074(4) 0.048(4) -0.035(3) -0.017(3) 0.020(4) N1 0.038(2) 0.034(2) 0.034(2) -0.0045(17) -0.0022(18) -0.0083(17) C17 0.048(3) 0.033(2) 0.033(3) -0.005(2) 0.003(2) -0.014(2) C18 0.052(3) 0.032(3) 0.038(3) -0.003(2) 0.005(2) -0.002(2) C19 0.033(3) 0.048(3) 0.040(3) -0.004(2) 0.009(2) -0.002(2) C20 0.038(3) 0.030(2) 0.041(3) 0.005(2) -0.001(2) -0.009(2) C21 0.040(3) 0.033(2) 0.030(2) 0.0028(19) -0.007(2) -0.003(2) N2 0.043(2) 0.029(2) 0.028(2) -0.0024(16) -0.0009(18) -0.0034(17) C22 0.039(3) 0.027(2) 0.034(3) -0.0037(19) -0.002(2) -0.0008(19) C23 0.045(3) 0.031(2) 0.025(2) 0.0035(19) -0.004(2) -0.011(2) C24 0.042(3) 0.046(3) 0.030(2) 0.006(2) 0.004(2) 0.001(2) C25 0.053(3) 0.032(2) 0.031(3) -0.005(2) 0.006(2) 0.000(2) C26 0.048(3) 0.032(2) 0.036(3) 0.000(2) 0.003(2) -0.011(2) O7 0.029(4) 0.054(4) 0.030(4) 0.009(3) 0.000(3) 0.004(3) C27 0.104(8) 0.042(5) 0.027(4) 0.000 0.000 -0.011(5) O21 0.065(6) 0.109(8) 0.056(6) 0.010(5) -0.008(5) -0.012(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 1.864(3) . ? Mn1 O1 1.896(3) . ? Mn1 O2 1.937(3) . ? Mn1 O5 1.947(3) . ? Mn1 N1 2.295(4) . ? Mn1 N2 2.296(4) . ? Mn2 O3 2.037(4) . ? Mn2 O3 2.037(4) 6_554 ? Mn2 O6 2.119(4) 7_544 ? Mn2 O6 2.119(4) 4_564 ? Mn2 O7 2.277(7) . ? Mn2 O7 2.277(7) 6_554 ? O1 C1 1.326(6) . ? C1 C6 1.401(7) . ? C1 C2 1.410(7) . ? C2 C3 1.394(8) . ? C2 C7 1.492(7) . ? C3 C4 1.372(8) . ? C3 H3A 0.9500 . ? C4 C5 1.389(9) . ? C4 H4A 0.9500 . ? C5 C6 1.381(8) . ? C5 C8 1.524(8) . ? C6 H6A 0.9500 . ? C7 O3 1.255(7) . ? C7 O2 1.259(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O4 C9 1.332(7) . ? C9 C10 1.408(7) . ? C9 C14 1.416(7) . ? C10 C11 1.419(7) . ? C10 C15 1.479(7) . ? C11 C12 1.351(8) . ? C11 H11A 0.9500 . ? C12 C13 1.397(9) . ? C12 H12A 0.9500 . ? C13 C14 1.394(9) . ? C13 C16 1.513(7) . ? C14 H14A 0.9500 . ? C15 O6 1.252(6) . ? C15 O5 1.285(6) . ? O6 Mn2 2.119(4) 3_645 ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N1 C17 1.339(7) . ? N1 C21 1.343(6) . ? C17 C18 1.372(7) . ? C17 H17A 0.9500 . ? C18 C19 1.392(7) . ? C18 H18A 0.9500 . ? C19 C20 1.386(7) . ? C19 H19A 0.9500 . ? C20 C21 1.378(7) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? N2 C26 1.333(6) . ? N2 C22 1.346(6) . ? C22 C23 1.387(7) . ? C22 H22A 0.9500 . ? C23 C24 1.362(7) . ? C23 H23A 0.9500 . ? C24 C25 1.388(7) . ? C24 H24A 0.9500 . ? C25 C26 1.378(7) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? O7 C27 1.313(9) . ? O7 H7 0.99(3) . ? C27 O7 1.313(9) 6_554 ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 O4 Mn1 O1 179.08(17) . . ? O4 Mn1 O2 88.54(16) . . ? O1 Mn1 O2 92.36(16) . . ? O4 Mn1 O5 91.92(16) . . ? O1 Mn1 O5 87.17(15) . . ? O2 Mn1 O5 179.27(17) . . ? O4 Mn1 N1 90.41(15) . . ? O1 Mn1 N1 89.75(15) . . ? O2 Mn1 N1 88.64(15) . . ? O5 Mn1 N1 90.79(15) . . ? O4 Mn1 N2 88.07(15) . . ? O1 Mn1 N2 91.82(15) . . ? O2 Mn1 N2 88.33(15) . . ? O5 Mn1 N2 92.24(14) . . ? N1 Mn1 N2 176.65(15) . . ? O3 Mn2 O3 146.5(3) . 6_554 ? O3 Mn2 O6 101.33(19) . 7_544 ? O3 Mn2 O6 100.79(17) 6_554 7_544 ? O3 Mn2 O6 100.79(17) . 4_564 ? O3 Mn2 O6 101.32(19) 6_554 4_564 ? O6 Mn2 O6 96.5(2) 7_544 4_564 ? O3 Mn2 O7 77.0(2) . . ? O3 Mn2 O7 72.0(2) 6_554 . ? O6 Mn2 O7 109.9(2) 7_544 . ? O6 Mn2 O7 153.52(19) 4_564 . ? O3 Mn2 O7 72.0(2) . 6_554 ? O3 Mn2 O7 77.0(2) 6_554 6_554 ? O6 Mn2 O7 153.52(19) 7_544 6_554 ? O6 Mn2 O7 109.9(2) 4_564 6_554 ? O7 Mn2 O7 44.0(3) . 6_554 ? C1 O1 Mn1 127.3(3) . . ? O1 C1 C6 117.1(5) . . ? O1 C1 C2 124.8(4) . . ? C6 C1 C2 118.0(4) . . ? C3 C2 C1 118.4(5) . . ? C3 C2 C7 118.8(5) . . ? C1 C2 C7 122.8(4) . . ? C4 C3 C2 122.7(6) . . ? C4 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? C3 C4 C5 119.5(5) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 118.8(5) . . ? C6 C5 C8 121.1(6) . . ? C4 C5 C8 120.0(5) . . ? C5 C6 C1 122.6(5) . . ? C5 C6 H6A 118.7 . . ? C1 C6 H6A 118.7 . . ? O3 C7 O2 121.2(5) . . ? O3 C7 C2 117.0(5) . . ? O2 C7 C2 121.8(4) . . ? C7 O2 Mn1 130.3(3) . . ? C7 O3 Mn2 139.1(4) . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 O4 Mn1 128.1(3) . . ? O4 C9 C10 124.7(4) . . ? O4 C9 C14 117.0(5) . . ? C10 C9 C14 118.3(5) . . ? C9 C10 C11 118.6(5) . . ? C9 C10 C15 123.4(5) . . ? C11 C10 C15 118.0(5) . . ? C12 C11 C10 122.3(5) . . ? C12 C11 H11A 118.8 . . ? C10 C11 H11A 118.8 . . ? C11 C12 C13 119.9(5) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 119.5(5) . . ? C14 C13 C16 119.7(6) . . ? C12 C13 C16 120.8(5) . . ? C13 C14 C9 121.3(5) . . ? C13 C14 H14A 119.4 . . ? C9 C14 H14A 119.4 . . ? O6 C15 O5 119.6(5) . . ? O6 C15 C10 119.9(5) . . ? O5 C15 C10 120.5(5) . . ? C15 O5 Mn1 130.4(3) . . ? C15 O6 Mn2 116.6(3) . 3_645 ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 N1 C21 117.2(4) . . ? C17 N1 Mn1 123.0(3) . . ? C21 N1 Mn1 119.8(3) . . ? N1 C17 C18 123.7(5) . . ? N1 C17 H17A 118.2 . . ? C18 C17 H17A 118.2 . . ? C17 C18 C19 118.6(5) . . ? C17 C18 H18A 120.7 . . ? C19 C18 H18A 120.7 . . ? C20 C19 C18 118.4(5) . . ? C20 C19 H19A 120.8 . . ? C18 C19 H19A 120.8 . . ? C21 C20 C19 119.0(5) . . ? C21 C20 H20A 120.5 . . ? C19 C20 H20A 120.5 . . ? N1 C21 C20 123.1(5) . . ? N1 C21 H21A 118.4 . . ? C20 C21 H21A 118.4 . . ? C26 N2 C22 116.9(4) . . ? C26 N2 Mn1 122.0(3) . . ? C22 N2 Mn1 121.1(3) . . ? N2 C22 C23 123.0(4) . . ? N2 C22 H22A 118.5 . . ? C23 C22 H22A 118.5 . . ? C24 C23 C22 118.9(4) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? C23 C24 C25 119.2(5) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C26 C25 C24 118.2(5) . . ? C26 C25 H25A 120.9 . . ? C24 C25 H25A 120.9 . . ? N2 C26 C25 123.8(4) . . ? N2 C26 H26A 118.1 . . ? C25 C26 H26A 118.1 . . ? C27 O7 Mn2 117.5(4) . . ? C27 O7 H7 104(4) . . ? Mn2 O7 H7 123(4) . . ? O7 C27 O7 81.0(7) . 6_554 ? O7 C27 H27A 109.5 . . ? O7 C27 H27A 52.7 6_554 . ? O7 C27 H27B 109.5 . . ? O7 C27 H27B 79.0 6_554 . ? H27A C27 H27B 109.5 . . ? O7 C27 H27C 109.5 . . ? O7 C27 H27C 162.2 6_554 . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 O7 H7 O1 0.99(3) 1.93(4) 2.898(8) 165(5) 7_544 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.411 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.098 ################################################################# data_msa538 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H52 Mn3 N4 O15' _chemical_formula_weight 1149.81 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/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 18.888(3) _cell_length_b 13.7658(14) _cell_length_c 20.054(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.780(12) _cell_angle_gamma 90.00 _cell_volume 5203.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9781 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 24.76 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2372 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Crystals were small and poorly-diffracting. No significant intensity was measureable at a resolution higher than 1.05 \%A, even using a rotating anode, and the data were truncated at this resolution. The low data . parameter ratio (6.8 : 1) is a result of this. The weak diffraction also resulted in the rather high R(int). ; _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 17781 _diffrn_reflns_av_R_equivalents 0.1682 _diffrn_reflns_av_sigmaI/netI 0.1283 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 19.78 _reflns_number_total 4704 _reflns_number_gt 2867 _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 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. ; _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^)+(0.1007P)^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 4704 _refine_ls_number_parameters 693 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1384 _refine_ls_R_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.2082 _refine_ls_wR_factor_gt 0.1808 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.27196(9) 0.25334(13) 0.26402(8) 0.0392(5) Uani 1 1 d . . . Mn2 Mn 0.5000 0.0000 0.5000 0.0593(9) Uani 1 2 d S . . Mn3 Mn 0.0000 0.0000 0.5000 0.0427(7) Uani 1 2 d S . . Mn4 Mn 0.26808(10) 0.23916(14) 0.51201(10) 0.0528(6) Uani 1 1 d D . . O1 O 0.2567(4) 0.3851(6) 0.2363(4) 0.048(2) Uani 1 1 d . . . C1 C 0.2323(6) 0.4562(8) 0.2776(7) 0.041(3) Uani 1 1 d . . . C2 C 0.2275(6) 0.4488(8) 0.3451(6) 0.035(3) Uani 1 1 d . . . C3 C 0.2037(6) 0.5317(9) 0.3807(6) 0.044(3) Uani 1 1 d . . . H3A H 0.1994 0.5268 0.4265 0.053 Uiso 1 1 calc R . . C4 C 0.1870(6) 0.6182(9) 0.3490(6) 0.039(3) Uani 1 1 d . . . C5 C 0.1910(6) 0.6197(9) 0.2790(7) 0.048(3) Uani 1 1 d . . . H5A H 0.1769 0.6760 0.2561 0.058 Uiso 1 1 calc R . . C6 C 0.2145(6) 0.5426(8) 0.2426(6) 0.038(3) Uani 1 1 d . . . H6A H 0.2185 0.5474 0.1968 0.045 Uiso 1 1 calc R . . C7 C 0.2459(6) 0.3608(10) 0.3848(7) 0.039(3) Uani 1 1 d . . . O2 O 0.2648(4) 0.2832(6) 0.3557(4) 0.045(2) Uani 1 1 d . . . O3 O 0.2418(4) 0.3620(5) 0.4473(4) 0.050(2) Uani 1 1 d . . . C8 C 0.1623(7) 0.7054(9) 0.3871(6) 0.059(4) Uani 1 1 d . . . H8A H 0.1629 0.6900 0.4338 0.088 Uiso 1 1 calc R . . H8B H 0.1149 0.7222 0.3710 0.088 Uiso 1 1 calc R . . H8C H 0.1933 0.7593 0.3807 0.088 Uiso 1 1 calc R . . O4 O 0.2843(4) 0.1222(5) 0.2923(4) 0.042(2) Uani 1 1 d . . . C9 C 0.2803(6) 0.0431(9) 0.2512(7) 0.047(3) Uani 1 1 d . . . C10 C 0.2758(6) 0.0488(9) 0.1814(6) 0.040(3) Uani 1 1 d . . . C11 C 0.2728(6) -0.0408(10) 0.1461(7) 0.048(3) Uani 1 1 d . . . H11A H 0.2681 -0.0386 0.0996 0.058 Uiso 1 1 calc R . . C12 C 0.2764(6) -0.1297(9) 0.1760(7) 0.046(3) Uani 1 1 d . . . C13 C 0.2816(6) -0.1314(9) 0.2459(7) 0.049(3) Uani 1 1 d . . . H13A H 0.2827 -0.1913 0.2674 0.059 Uiso 1 1 calc R . . C14 C 0.2851(6) -0.0476(9) 0.2845(6) 0.042(3) Uani 1 1 d . . . H14A H 0.2904 -0.0510 0.3309 0.051 Uiso 1 1 calc R . . C15 C 0.2739(6) 0.1394(10) 0.1423(8) 0.046(3) Uani 1 1 d . . . O5 O 0.2804(4) 0.2209(6) 0.1733(4) 0.048(2) Uani 1 1 d . . . O6 O 0.2667(5) 0.1372(6) 0.0808(5) 0.055(2) Uani 1 1 d . . . C16 C 0.2774(7) -0.2235(9) 0.1361(7) 0.062(4) Uani 1 1 d . . . H16A H 0.2732 -0.2088 0.0892 0.093 Uiso 1 1 calc R . . H16B H 0.2383 -0.2638 0.1472 0.093 Uiso 1 1 calc R . . H16C H 0.3212 -0.2572 0.1468 0.093 Uiso 1 1 calc R . . O7 O 0.5721(4) 0.0831(6) 0.5266(5) 0.059(3) Uani 1 1 d . . . C17 C 0.5699(6) 0.1801(11) 0.5405(7) 0.056(4) Uani 1 1 d . . . C18 C 0.5070(6) 0.2346(9) 0.5347(6) 0.044(3) Uani 1 1 d . . . C19 C 0.5119(7) 0.3353(10) 0.5490(6) 0.053(4) Uani 1 1 d . . . H19A H 0.4708 0.3725 0.5454 0.064 Uiso 1 1 calc R . . C20 C 0.5733(8) 0.3789(10) 0.5674(8) 0.068(4) Uani 1 1 d . . . C21 C 0.6346(8) 0.3242(12) 0.5748(8) 0.077(5) Uani 1 1 d . . . H21A H 0.6775 0.3541 0.5876 0.093 Uiso 1 1 calc R . . C22 C 0.6324(7) 0.2217(10) 0.5629(7) 0.063(4) Uani 1 1 d . . . H22A H 0.6730 0.1841 0.5704 0.075 Uiso 1 1 calc R . . C23 C 0.4356(7) 0.1977(10) 0.5150(6) 0.048(3) Uani 1 1 d . . . O8 O 0.4274(4) 0.1081(6) 0.4967(5) 0.062(3) Uani 1 1 d . . . O9 O 0.3824(4) 0.2512(6) 0.5131(5) 0.062(2) Uani 1 1 d . . . C24 C 0.5806(9) 0.4920(11) 0.5786(9) 0.096(5) Uani 1 1 d . . . H24A H 0.5347 0.5218 0.5722 0.143 Uiso 1 1 calc R . . H24B H 0.6115 0.5185 0.5471 0.143 Uiso 1 1 calc R . . H24C H 0.6000 0.5045 0.6232 0.143 Uiso 1 1 calc R . . O10 O -0.0564(4) 0.1081(6) 0.4798(4) 0.044(2) Uani 1 1 d . . . C25 C -0.0333(6) 0.1984(9) 0.4645(5) 0.038(3) Uani 1 1 d . . . C26 C 0.0365(6) 0.2298(9) 0.4740(5) 0.040(3) Uani 1 1 d . . . C27 C 0.0517(6) 0.3276(9) 0.4560(6) 0.042(3) Uani 1 1 d . . . H27A H 0.0984 0.3494 0.4607 0.050 Uiso 1 1 calc R . . C28 C -0.0002(7) 0.3905(9) 0.4318(6) 0.046(3) Uani 1 1 d . . . C29 C -0.0689(7) 0.3593(9) 0.4230(6) 0.049(3) Uani 1 1 d . . . H29A H -0.1043 0.4017 0.4068 0.059 Uiso 1 1 calc R . . C30 C -0.0858(6) 0.2626(10) 0.4385(6) 0.050(3) Uani 1 1 d . . . H30A H -0.1324 0.2410 0.4315 0.060 Uiso 1 1 calc R . . C31 C 0.0957(7) 0.1709(10) 0.4993(6) 0.046(3) Uani 1 1 d . . . O11 O 0.0867(4) 0.0767(6) 0.5102(4) 0.046(2) Uani 1 1 d . . . O12 O 0.1557(5) 0.2060(6) 0.5098(5) 0.064(3) Uani 1 1 d . . . C32 C 0.0190(7) 0.4962(9) 0.4135(7) 0.061(4) Uani 1 1 d . . . H32A H -0.0232 0.5300 0.3973 0.091 Uiso 1 1 calc R . . H32B H 0.0524 0.4955 0.3794 0.091 Uiso 1 1 calc R . . H32C H 0.0396 0.5287 0.4524 0.091 Uiso 1 1 calc R . . O13 O 0.2807(5) 0.1221(7) 0.5869(4) 0.060(3) Uani 1 1 d D . . H131 H 0.283(8) 0.131(11) 0.632(2) 0.090 Uiso 1 1 d D . . H132 H 0.253(5) 0.074(7) 0.593(6) 0.090 Uiso 1 1 d D . . O14 O 0.2855(6) 0.1156(7) 0.4421(5) 0.071(3) Uani 1 1 d D . . H141 H 0.300(8) 0.063(7) 0.463(6) 0.106 Uiso 1 1 d D . . H142 H 0.289(8) 0.120(10) 0.398(2) 0.106 Uiso 1 1 d D . . N1 N 0.3936(5) 0.2808(6) 0.2738(5) 0.038(2) Uani 1 1 d . . . C41 C 0.4316(7) 0.2913(8) 0.2198(6) 0.046(3) Uani 1 1 d . . . H41A H 0.4088 0.2879 0.1774 0.056 Uiso 1 1 calc R . . C42 C 0.5040(8) 0.3073(10) 0.2263(8) 0.059(4) Uani 1 1 d . . . H42A H 0.5292 0.3134 0.1882 0.071 Uiso 1 1 calc R . . C43 C 0.5385(7) 0.3139(10) 0.2870(8) 0.059(4) Uani 1 1 d . . . H43A H 0.5869 0.3268 0.2914 0.071 Uiso 1 1 calc R . . C44 C 0.5003(7) 0.3012(10) 0.3423(7) 0.057(4) Uani 1 1 d . . . H44A H 0.5227 0.3035 0.3850 0.068 Uiso 1 1 calc R . . C45 C 0.4280(7) 0.2848(8) 0.3332(7) 0.046(3) Uani 1 1 d . . . H45A H 0.4023 0.2762 0.3708 0.055 Uiso 1 1 calc R . . N2 N 0.1482(5) 0.2302(7) 0.2462(5) 0.045(3) Uani 1 1 d . . . C46 C 0.1088(7) 0.2139(8) 0.2979(7) 0.050(3) Uani 1 1 d . . . H46A H 0.1315 0.2109 0.3405 0.060 Uiso 1 1 calc R . . C47 C 0.0353(7) 0.2012(9) 0.2915(6) 0.049(3) Uani 1 1 d . . . H47A H 0.0083 0.1930 0.3282 0.058 Uiso 1 1 calc R . . C48 C 0.0060(7) 0.2015(9) 0.2278(7) 0.054(4) Uani 1 1 d . . . H48A H -0.0426 0.1910 0.2205 0.064 Uiso 1 1 calc R . . C49 C 0.0456(7) 0.2168(8) 0.1739(7) 0.046(3) Uani 1 1 d . . . H49A H 0.0244 0.2174 0.1307 0.055 Uiso 1 1 calc R . . C50 C 0.1163(7) 0.2311(8) 0.1851(6) 0.045(3) Uani 1 1 d . . . H50A H 0.1434 0.2420 0.1488 0.054 Uiso 1 1 calc R . . N3 N 0.4822(7) -0.0277(7) 0.6082(6) 0.061(3) Uani 1 1 d . . . C51 C 0.5363(8) -0.0384(9) 0.6545(10) 0.064(4) Uani 1 1 d . . . H51A H 0.5822 -0.0318 0.6409 0.077 Uiso 1 1 calc R . . C52 C 0.5282(8) -0.0587(9) 0.7210(10) 0.070(4) Uani 1 1 d . . . H52A H 0.5677 -0.0682 0.7503 0.084 Uiso 1 1 calc R . . C53 C 0.4617(10) -0.0649(10) 0.7432(8) 0.073(4) Uani 1 1 d . . . H53A H 0.4542 -0.0796 0.7874 0.087 Uiso 1 1 calc R . . C54 C 0.4060(8) -0.0480(11) 0.6963(11) 0.080(5) Uani 1 1 d . . . H54A H 0.3599 -0.0482 0.7099 0.096 Uiso 1 1 calc R . . C55 C 0.4166(8) -0.0315(11) 0.6320(10) 0.073(4) Uani 1 1 d . . . H55A H 0.3773 -0.0223 0.6023 0.088 Uiso 1 1 calc R . . N4 N -0.0160(6) 0.0201(7) 0.6111(6) 0.054(3) Uani 1 1 d . . . C56 C 0.0378(7) 0.0231(9) 0.6573(8) 0.054(4) Uani 1 1 d . . . H56A H 0.0831 0.0107 0.6440 0.065 Uiso 1 1 calc R . . C57 C 0.0303(7) 0.0440(9) 0.7253(7) 0.046(3) Uani 1 1 d . . . H57A H 0.0697 0.0475 0.7555 0.056 Uiso 1 1 calc R . . C58 C -0.0358(8) 0.0587(9) 0.7454(7) 0.053(4) Uani 1 1 d . . . H58A H -0.0429 0.0726 0.7899 0.064 Uiso 1 1 calc R . . C59 C -0.0926(8) 0.0527(10) 0.6986(8) 0.060(4) Uani 1 1 d . . . H59A H -0.1385 0.0614 0.7116 0.072 Uiso 1 1 calc R . . C60 C -0.0815(7) 0.0340(9) 0.6330(7) 0.052(4) Uani 1 1 d . . . H60A H -0.1205 0.0308 0.6023 0.062 Uiso 1 1 calc R . . O61 O 0.2035(5) -0.0427(8) 0.5643(5) 0.074(3) Uani 1 1 d . . . H61 H 0.1609 -0.0356 0.5547 0.111 Uiso 1 1 calc R . . C61 C 0.2333(8) -0.0894(12) 0.5140(8) 0.083(5) Uani 1 1 d . . . H61A H 0.2509 -0.0426 0.4837 0.124 Uiso 1 1 calc R . . H61B H 0.1983 -0.1296 0.4906 0.124 Uiso 1 1 calc R . . H61C H 0.2717 -0.1291 0.5319 0.124 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 0.0516(11) 0.0267(11) 0.0397(10) 0.0027(8) 0.0049(8) 0.0013(9) Mn2 0.0389(16) 0.0337(18) 0.103(2) -0.0224(16) -0.0162(15) 0.0084(14) Mn3 0.0318(14) 0.0384(17) 0.0578(17) 0.0102(13) 0.0027(12) -0.0001(13) Mn4 0.0471(12) 0.0321(12) 0.0785(14) -0.0009(11) -0.0024(10) 0.0022(10) O1 0.061(5) 0.023(5) 0.060(5) 0.014(4) 0.004(4) 0.002(4) C1 0.041(7) 0.013(8) 0.069(10) -0.008(7) -0.006(7) 0.002(6) C2 0.044(7) 0.029(8) 0.032(8) 0.005(6) -0.006(6) -0.007(6) C3 0.052(8) 0.051(10) 0.030(7) -0.007(7) 0.005(6) -0.008(7) C4 0.039(7) 0.031(8) 0.047(9) 0.002(7) 0.005(6) -0.001(6) C5 0.034(7) 0.033(9) 0.075(11) 0.005(7) -0.005(7) -0.013(6) C6 0.050(8) 0.013(7) 0.051(8) 0.003(6) 0.005(6) 0.000(6) C7 0.025(7) 0.045(10) 0.047(9) 0.009(8) 0.006(6) -0.011(6) O2 0.058(5) 0.031(5) 0.048(5) 0.000(4) 0.011(4) 0.003(4) O3 0.074(6) 0.028(5) 0.049(6) -0.002(4) 0.012(5) -0.005(4) C8 0.077(10) 0.031(8) 0.068(9) -0.006(7) 0.001(7) 0.006(7) O4 0.056(5) 0.021(5) 0.048(5) 0.011(4) -0.001(4) 0.007(4) C9 0.029(7) 0.044(10) 0.067(10) -0.005(8) 0.001(6) 0.000(6) C10 0.042(7) 0.038(9) 0.042(9) -0.011(7) 0.003(6) -0.006(6) C11 0.027(7) 0.057(11) 0.060(9) 0.001(8) 0.000(6) 0.001(6) C12 0.042(8) 0.040(10) 0.056(10) 0.006(7) -0.004(6) 0.011(6) C13 0.038(8) 0.030(9) 0.079(11) 0.006(8) 0.000(7) 0.006(6) C14 0.052(8) 0.026(8) 0.049(8) 0.012(7) 0.000(6) -0.003(6) C15 0.043(8) 0.040(10) 0.056(10) 0.005(9) 0.008(7) 0.001(7) O5 0.055(5) 0.035(6) 0.053(5) 0.008(5) 0.004(4) -0.008(4) O6 0.070(6) 0.055(6) 0.040(6) -0.001(5) 0.007(5) 0.002(5) C16 0.069(9) 0.038(9) 0.077(9) -0.015(7) -0.009(7) -0.010(7) O7 0.041(5) 0.030(6) 0.105(7) -0.027(5) -0.018(5) 0.004(4) C17 0.029(8) 0.063(11) 0.076(10) -0.011(8) -0.007(7) -0.003(8) C18 0.038(8) 0.031(9) 0.062(8) -0.007(6) 0.003(6) -0.006(7) C19 0.045(9) 0.043(10) 0.069(9) 0.001(7) -0.006(7) 0.010(7) C20 0.051(10) 0.036(9) 0.114(13) 0.001(8) -0.002(9) 0.000(9) C21 0.048(10) 0.073(13) 0.110(13) -0.020(9) -0.008(8) -0.025(9) C22 0.044(9) 0.039(10) 0.103(11) -0.019(8) -0.012(8) 0.000(7) C23 0.045(9) 0.043(10) 0.058(9) 0.000(7) 0.006(7) 0.013(8) O8 0.044(5) 0.026(6) 0.112(8) -0.023(5) -0.018(5) 0.026(4) O9 0.046(5) 0.021(5) 0.119(8) -0.004(5) 0.000(5) 0.014(5) C24 0.090(12) 0.043(10) 0.150(16) -0.001(10) -0.015(11) -0.011(9) O10 0.025(4) 0.036(6) 0.071(6) 0.018(4) 0.008(4) 0.011(4) C25 0.039(8) 0.040(9) 0.033(7) 0.004(6) -0.001(6) 0.002(7) C26 0.024(7) 0.053(10) 0.044(7) 0.009(6) 0.002(6) 0.009(7) C27 0.039(7) 0.041(9) 0.048(8) -0.010(6) 0.021(6) -0.003(7) C28 0.040(8) 0.036(8) 0.063(9) 0.006(6) 0.016(7) 0.008(7) C29 0.052(10) 0.039(9) 0.059(9) 0.012(7) 0.014(7) 0.014(7) C30 0.041(8) 0.062(11) 0.048(8) 0.003(7) 0.010(6) 0.002(8) C31 0.029(8) 0.042(10) 0.069(9) -0.007(7) 0.005(7) -0.014(7) O11 0.032(5) 0.033(6) 0.072(6) 0.007(4) 0.003(4) 0.001(4) O12 0.048(6) 0.037(6) 0.103(8) 0.019(5) -0.020(5) -0.002(5) C32 0.059(8) 0.035(8) 0.087(10) 0.012(7) -0.004(7) 0.006(7) O13 0.088(7) 0.047(6) 0.043(5) 0.005(5) -0.014(5) 0.003(5) O14 0.102(8) 0.053(7) 0.057(6) -0.001(5) 0.003(6) -0.008(6) N1 0.050(6) 0.028(6) 0.037(6) 0.004(4) 0.002(6) -0.003(5) C41 0.067(10) 0.026(7) 0.048(9) 0.000(6) 0.014(8) -0.009(6) C42 0.057(10) 0.053(9) 0.070(11) 0.027(8) 0.015(8) -0.006(7) C43 0.048(9) 0.059(10) 0.071(11) 0.001(8) 0.001(9) -0.014(7) C44 0.044(9) 0.054(9) 0.069(11) 0.009(7) -0.022(8) 0.000(7) C45 0.068(10) 0.023(7) 0.048(9) 0.005(6) 0.013(7) 0.003(6) N2 0.057(6) 0.032(6) 0.049(7) -0.006(5) 0.016(7) -0.005(5) C46 0.066(10) 0.031(8) 0.052(9) -0.001(6) -0.001(8) -0.005(7) C47 0.062(10) 0.053(9) 0.031(8) 0.009(6) 0.003(7) -0.008(7) C48 0.051(8) 0.042(9) 0.069(11) 0.009(7) 0.008(9) -0.007(7) C49 0.045(9) 0.038(8) 0.053(9) -0.003(6) -0.009(7) 0.006(6) C50 0.062(10) 0.042(8) 0.031(8) 0.001(6) 0.003(7) 0.005(7) N3 0.046(7) 0.034(7) 0.103(10) -0.023(6) -0.009(8) 0.004(5) C51 0.057(10) 0.033(9) 0.102(13) -0.016(8) 0.007(11) 0.004(7) C52 0.063(12) 0.026(8) 0.120(16) -0.008(9) -0.001(10) -0.003(7) C53 0.087(13) 0.048(10) 0.083(11) -0.016(8) 0.006(12) 0.009(9) C54 0.048(10) 0.064(11) 0.129(17) -0.020(11) 0.014(12) 0.006(8) C55 0.053(12) 0.067(11) 0.099(15) -0.007(9) 0.001(10) 0.011(8) N4 0.039(7) 0.039(7) 0.081(8) 0.011(6) -0.004(7) -0.002(5) C56 0.045(9) 0.037(8) 0.082(12) 0.022(7) 0.015(9) 0.012(7) C57 0.041(9) 0.048(9) 0.050(9) 0.017(6) 0.000(7) -0.002(6) C58 0.059(10) 0.035(8) 0.067(9) -0.004(7) 0.006(9) 0.007(7) C59 0.057(10) 0.050(9) 0.076(11) 0.013(8) 0.016(9) 0.011(7) C60 0.048(10) 0.045(9) 0.060(10) 0.017(7) -0.005(7) -0.005(7) O61 0.049(6) 0.092(8) 0.082(7) -0.005(6) 0.001(5) -0.006(6) C61 0.082(12) 0.076(12) 0.088(13) 0.011(10) -0.013(10) -0.007(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 Mn1 O5 1.891(9) . ? Mn1 O2 1.897(8) . ? Mn1 O4 1.901(7) . ? Mn1 O1 1.913(8) . ? Mn1 N1 2.324(9) . ? Mn1 N2 2.363(10) . ? Mn2 O7 1.831(8) . ? Mn2 O7 1.831(8) 3_656 ? Mn2 O8 2.022(7) . ? Mn2 O8 2.022(7) 3_656 ? Mn2 N3 2.250(13) 3_656 ? Mn2 N3 2.250(13) . ? Mn3 O10 1.860(7) . ? Mn3 O10 1.860(7) 3_556 ? Mn3 O11 1.948(8) . ? Mn3 O11 1.948(8) 3_556 ? Mn3 N4 2.285(11) . ? Mn3 N4 2.286(11) 3_556 ? Mn4 O9 2.164(8) . ? Mn4 O12 2.168(9) . ? Mn4 O3 2.169(8) . ? Mn4 O6 2.192(9) 4_566 ? Mn4 O13 2.205(9) . ? Mn4 O14 2.242(9) . ? O1 C1 1.381(14) . ? C1 C2 1.367(15) . ? C1 C6 1.410(16) . ? C2 C3 1.432(16) . ? C2 C7 1.479(16) . ? C3 C4 1.378(16) . ? C3 H3A 0.9300 . ? C4 C5 1.409(16) . ? C4 C8 1.514(17) . ? C5 C6 1.379(16) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O3 1.261(13) . ? C7 O2 1.280(14) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? O4 C9 1.365(14) . ? C9 C10 1.400(16) . ? C9 C14 1.415(17) . ? C10 C11 1.422(17) . ? C10 C15 1.472(18) . ? C11 C12 1.363(17) . ? C11 H11A 0.9300 . ? C12 C13 1.398(17) . ? C12 C16 1.520(17) . ? C13 C14 1.389(17) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 O6 1.232(14) . ? C15 O5 1.284(15) . ? O6 Mn4 2.192(9) 4_565 ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? O7 C17 1.365(16) . ? C17 C22 1.362(17) . ? C17 C18 1.403(17) . ? C18 C19 1.417(17) . ? C18 C23 1.469(17) . ? C19 C20 1.335(18) . ? C19 H19A 0.9300 . ? C20 C21 1.381(19) . ? C20 C24 1.58(2) . ? C21 C22 1.431(19) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 O9 1.245(14) . ? C23 O8 1.294(15) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? O10 C25 1.359(14) . ? C25 C26 1.387(16) . ? C25 C30 1.404(16) . ? C26 C27 1.429(17) . ? C26 C31 1.446(17) . ? C27 C28 1.372(16) . ? C27 H27A 0.9300 . ? C28 C29 1.368(17) . ? C28 C32 1.550(17) . ? C29 C30 1.409(17) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 O12 1.238(13) . ? C31 O11 1.328(14) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? O13 H131 0.91(4) . ? O13 H132 0.85(4) . ? O14 H141 0.88(4) . ? O14 H142 0.89(4) . ? N1 C45 1.320(14) . ? N1 C41 1.345(14) . ? C41 C42 1.382(18) . ? C41 H41A 0.9300 . ? C42 C43 1.345(18) . ? C42 H42A 0.9300 . ? C43 C44 1.372(18) . ? C43 H43A 0.9300 . ? C44 C45 1.386(17) . ? C44 H44A 0.9300 . ? C45 H45A 0.9300 . ? N2 C50 1.330(14) . ? N2 C46 1.335(15) . ? C46 C47 1.397(17) . ? C46 H46A 0.9300 . ? C47 C48 1.358(16) . ? C47 H47A 0.9300 . ? C48 C49 1.371(17) . ? C48 H48A 0.9300 . ? C49 C50 1.354(16) . ? C49 H49A 0.9300 . ? C50 H50A 0.9300 . ? N3 C51 1.342(17) . ? N3 C55 1.357(18) . ? C51 C52 1.38(2) . ? C51 H51A 0.9300 . ? C52 C53 1.36(2) . ? C52 H52A 0.9300 . ? C53 C54 1.38(2) . ? C53 H53A 0.9300 . ? C54 C55 1.34(2) . ? C54 H54A 0.9300 . ? C55 H55A 0.9300 . ? N4 C56 1.330(16) . ? N4 C60 1.353(16) . ? C56 C57 1.409(17) . ? C56 H56A 0.9300 . ? C57 C58 1.353(16) . ? C57 H57A 0.9300 . ? C58 C59 1.380(18) . ? C58 H58A 0.9300 . ? C59 C60 1.371(17) . ? C59 H59A 0.9300 . ? C60 H60A 0.9300 . ? O61 C61 1.349(17) . ? O61 H61 0.8200 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mn1 O2 178.6(4) . . ? O5 Mn1 O4 92.7(3) . . ? O2 Mn1 O4 86.1(3) . . ? O5 Mn1 O1 88.0(4) . . ? O2 Mn1 O1 93.3(4) . . ? O4 Mn1 O1 178.3(3) . . ? O5 Mn1 N1 88.5(3) . . ? O2 Mn1 N1 90.9(3) . . ? O4 Mn1 N1 91.6(3) . . ? O1 Mn1 N1 90.0(3) . . ? O5 Mn1 N2 88.2(3) . . ? O2 Mn1 N2 92.5(3) . . ? O4 Mn1 N2 91.0(3) . . ? O1 Mn1 N2 87.4(3) . . ? N1 Mn1 N2 175.9(4) . . ? O7 Mn2 O7 179.999(1) . 3_656 ? O7 Mn2 O8 92.3(4) . . ? O7 Mn2 O8 87.7(4) 3_656 . ? O7 Mn2 O8 87.7(4) . 3_656 ? O7 Mn2 O8 92.3(4) 3_656 3_656 ? O8 Mn2 O8 179.999(1) . 3_656 ? O7 Mn2 N3 91.1(4) . 3_656 ? O7 Mn2 N3 88.9(4) 3_656 3_656 ? O8 Mn2 N3 89.3(4) . 3_656 ? O8 Mn2 N3 90.7(4) 3_656 3_656 ? O7 Mn2 N3 88.9(4) . . ? O7 Mn2 N3 91.1(4) 3_656 . ? O8 Mn2 N3 90.7(4) . . ? O8 Mn2 N3 89.3(4) 3_656 . ? N3 Mn2 N3 179.998(2) 3_656 . ? O10 Mn3 O10 179.998(2) . 3_556 ? O10 Mn3 O11 93.2(3) . . ? O10 Mn3 O11 86.8(3) 3_556 . ? O10 Mn3 O11 86.8(3) . 3_556 ? O10 Mn3 O11 93.2(3) 3_556 3_556 ? O11 Mn3 O11 179.997(1) . 3_556 ? O10 Mn3 N4 90.2(4) . . ? O10 Mn3 N4 89.8(4) 3_556 . ? O11 Mn3 N4 89.8(4) . . ? O11 Mn3 N4 90.2(4) 3_556 . ? O10 Mn3 N4 89.8(4) . 3_556 ? O10 Mn3 N4 90.2(4) 3_556 3_556 ? O11 Mn3 N4 90.2(4) . 3_556 ? O11 Mn3 N4 89.8(4) 3_556 3_556 ? N4 Mn3 N4 180.0(5) . 3_556 ? O9 Mn4 O12 172.2(3) . . ? O9 Mn4 O3 97.7(3) . . ? O12 Mn4 O3 88.1(3) . . ? O9 Mn4 O6 89.3(3) . 4_566 ? O12 Mn4 O6 97.1(3) . 4_566 ? O3 Mn4 O6 76.1(3) . 4_566 ? O9 Mn4 O13 89.3(3) . . ? O12 Mn4 O13 85.5(3) . . ? O3 Mn4 O13 170.9(4) . . ? O6 Mn4 O13 98.3(3) 4_566 . ? O9 Mn4 O14 82.9(4) . . ? O12 Mn4 O14 90.6(4) . . ? O3 Mn4 O14 104.7(3) . . ? O6 Mn4 O14 172.2(4) 4_566 . ? O13 Mn4 O14 81.9(3) . . ? C1 O1 Mn1 123.2(7) . . ? C2 C1 O1 126.0(10) . . ? C2 C1 C6 121.7(11) . . ? O1 C1 C6 112.2(11) . . ? C1 C2 C3 118.5(10) . . ? C1 C2 C7 124.4(11) . . ? C3 C2 C7 117.1(11) . . ? C4 C3 C2 121.9(10) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C3 C4 C5 116.5(11) . . ? C3 C4 C8 121.4(11) . . ? C5 C4 C8 122.0(11) . . ? C6 C5 C4 123.8(12) . . ? C6 C5 H5A 118.1 . . ? C4 C5 H5A 118.1 . . ? C5 C6 C1 117.4(11) . . ? C5 C6 H6A 121.3 . . ? C1 C6 H6A 121.3 . . ? O3 C7 O2 120.1(11) . . ? O3 C7 C2 119.8(12) . . ? O2 C7 C2 120.1(11) . . ? C7 O2 Mn1 131.5(8) . . ? C7 O3 Mn4 123.9(8) . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 O4 Mn1 125.3(7) . . ? O4 C9 C10 123.7(11) . . ? O4 C9 C14 114.9(11) . . ? C10 C9 C14 121.3(12) . . ? C9 C10 C11 116.6(12) . . ? C9 C10 C15 125.4(12) . . ? C11 C10 C15 118.1(12) . . ? C12 C11 C10 124.1(12) . . ? C12 C11 H11A 118.0 . . ? C10 C11 H11A 118.0 . . ? C11 C12 C13 117.0(12) . . ? C11 C12 C16 122.2(12) . . ? C13 C12 C16 120.7(12) . . ? C14 C13 C12 122.9(12) . . ? C14 C13 H13A 118.6 . . ? C12 C13 H13A 118.6 . . ? C13 C14 C9 118.1(11) . . ? C13 C14 H14A 121.0 . . ? C9 C14 H14A 121.0 . . ? O6 C15 O5 120.4(11) . . ? O6 C15 C10 120.7(12) . . ? O5 C15 C10 118.9(12) . . ? C15 O5 Mn1 131.3(8) . . ? C15 O6 Mn4 127.3(8) . 4_565 ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 O7 Mn2 129.6(7) . . ? C22 C17 O7 116.2(11) . . ? C22 C17 C18 120.8(13) . . ? O7 C17 C18 122.9(11) . . ? C17 C18 C19 117.5(11) . . ? C17 C18 C23 126.4(12) . . ? C19 C18 C23 116.0(11) . . ? C20 C19 C18 122.7(12) . . ? C20 C19 H19A 118.6 . . ? C18 C19 H19A 118.6 . . ? C19 C20 C21 119.4(13) . . ? C19 C20 C24 123.3(13) . . ? C21 C20 C24 117.3(13) . . ? C20 C21 C22 120.3(13) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C17 C22 C21 119.1(13) . . ? C17 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? O9 C23 O8 118.2(11) . . ? O9 C23 C18 121.9(12) . . ? O8 C23 C18 119.8(11) . . ? C23 O8 Mn2 128.6(8) . . ? C23 O9 Mn4 139.3(8) . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 O10 Mn3 126.3(7) . . ? O10 C25 C26 124.8(11) . . ? O10 C25 C30 115.4(10) . . ? C26 C25 C30 119.8(12) . . ? C25 C26 C27 117.7(11) . . ? C25 C26 C31 125.4(12) . . ? C27 C26 C31 116.9(11) . . ? C28 C27 C26 122.2(11) . . ? C28 C27 H27A 118.9 . . ? C26 C27 H27A 118.9 . . ? C29 C28 C27 119.8(12) . . ? C29 C28 C32 119.9(11) . . ? C27 C28 C32 120.3(11) . . ? C28 C29 C30 119.7(12) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C25 C30 C29 120.8(11) . . ? C25 C30 H30A 119.6 . . ? C29 C30 H30A 119.6 . . ? O12 C31 O11 118.6(11) . . ? O12 C31 C26 121.3(12) . . ? O11 C31 C26 120.1(11) . . ? C31 O11 Mn3 128.9(7) . . ? C31 O12 Mn4 166.0(9) . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Mn4 O13 H131 125(10) . . ? Mn4 O13 H132 128(5) . . ? H131 O13 H132 88(10) . . ? Mn4 O14 H141 112(9) . . ? Mn4 O14 H142 126(9) . . ? H141 O14 H142 120(8) . . ? C45 N1 C41 117.7(11) . . ? C45 N1 Mn1 120.5(8) . . ? C41 N1 Mn1 121.8(8) . . ? N1 C41 C42 121.2(12) . . ? N1 C41 H41A 119.4 . . ? C42 C41 H41A 119.4 . . ? C43 C42 C41 120.9(13) . . ? C43 C42 H42A 119.6 . . ? C41 C42 H42A 119.6 . . ? C42 C43 C44 118.3(13) . . ? C42 C43 H43A 120.9 . . ? C44 C43 H43A 120.9 . . ? C43 C44 C45 118.8(13) . . ? C43 C44 H44A 120.6 . . ? C45 C44 H44A 120.6 . . ? N1 C45 C44 123.1(12) . . ? N1 C45 H45A 118.4 . . ? C44 C45 H45A 118.4 . . ? C50 N2 C46 118.4(10) . . ? C50 N2 Mn1 121.5(8) . . ? C46 N2 Mn1 120.1(9) . . ? N2 C46 C47 123.4(12) . . ? N2 C46 H46A 118.3 . . ? C47 C46 H46A 118.3 . . ? C48 C47 C46 115.4(12) . . ? C48 C47 H47A 122.3 . . ? C46 C47 H47A 122.3 . . ? C47 C48 C49 122.2(12) . . ? C47 C48 H48A 118.9 . . ? C49 C48 H48A 118.9 . . ? C50 C49 C48 118.4(12) . . ? C50 C49 H49A 120.8 . . ? C48 C49 H49A 120.8 . . ? N2 C50 C49 122.3(11) . . ? N2 C50 H50A 118.9 . . ? C49 C50 H50A 118.9 . . ? C51 N3 C55 115.0(13) . . ? C51 N3 Mn2 122.0(11) . . ? C55 N3 Mn2 122.9(11) . . ? N3 C51 C52 124.2(14) . . ? N3 C51 H51A 117.9 . . ? C52 C51 H51A 117.9 . . ? C53 C52 C51 119.5(15) . . ? C53 C52 H52A 120.3 . . ? C51 C52 H52A 120.3 . . ? C52 C53 C54 116.3(16) . . ? C52 C53 H53A 121.8 . . ? C54 C53 H53A 121.8 . . ? C55 C54 C53 121.9(15) . . ? C55 C54 H54A 119.1 . . ? C53 C54 H54A 119.1 . . ? C54 C55 N3 123.0(15) . . ? C54 C55 H55A 118.5 . . ? N3 C55 H55A 118.5 . . ? C56 N4 C60 116.3(11) . . ? C56 N4 Mn3 122.6(9) . . ? C60 N4 Mn3 121.0(9) . . ? N4 C56 C57 124.0(11) . . ? N4 C56 H56A 118.0 . . ? C57 C56 H56A 118.0 . . ? C58 C57 C56 118.2(12) . . ? C58 C57 H57A 120.9 . . ? C56 C57 H57A 120.9 . . ? C57 C58 C59 118.6(13) . . ? C57 C58 H58A 120.7 . . ? C59 C58 H58A 120.7 . . ? C60 C59 C58 120.2(12) . . ? C60 C59 H59A 119.9 . . ? C58 C59 H59A 119.9 . . ? N4 C60 C59 122.6(12) . . ? N4 C60 H60A 118.7 . . ? C59 C60 H60A 118.7 . . ? C61 O61 H61 109.5 . . ? O61 C61 H61A 109.5 . . ? O61 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O61 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 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 O13 H131 O5 0.91(4) 2.20(13) 2.770(12) 120(12) 4_566 O13 H131 O1 0.91(4) 2.19(7) 3.061(12) 159(13) 4_566 O13 H132 O61 0.85(4) 1.93(8) 2.719(14) 153(14) . O14 H141 O8 0.88(4) 2.53(17) 2.829(13) 101(12) . O14 H142 O4 0.89(4) 2.12(5) 3.003(12) 173(15) . O61 H61 O11 0.82 2.23 2.903(13) 139.1 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 19.78 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.710 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.112 #################################################################### data_msa298 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H64 Mn3 N4 O16' _chemical_formula_weight 1237.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8534(12) _cell_length_b 12.5635(14) _cell_length_c 19.530(2) _cell_angle_alpha 82.457(9) _cell_angle_beta 83.345(8) _cell_angle_gamma 85.861(8) _cell_volume 2859.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17867 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 27.18 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1286 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _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 21350 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.84 _reflns_number_total 12060 _reflns_number_gt 7513 _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 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. ; _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^)+(0.1190P)^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 12060 _refine_ls_number_parameters 780 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1198 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1974 _refine_ls_wR_factor_gt 0.1713 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.978 _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 0.48676(5) 0.01344(5) 0.24988(3) 0.04119(17) Uani 1 1 d . . . Mn2 Mn 0.5000 0.0000 0.5000 0.0368(2) Uani 1 2 d S . . Mn3 Mn 0.5000 0.0000 0.0000 0.0616(3) Uani 1 2 d S . . O1 O 0.6070(3) 0.0919(2) 0.20195(15) 0.0456(7) Uani 1 1 d . . . C1 C 0.6768(3) 0.1494(3) 0.2306(2) 0.0383(8) Uani 1 1 d . . . C2 C 0.7547(4) 0.2103(3) 0.1844(2) 0.0420(9) Uani 1 1 d . . . H2A H 0.7528 0.2115 0.1359 0.050 Uiso 1 1 calc R . . C3 C 0.8342(4) 0.2686(3) 0.2079(2) 0.0460(10) Uani 1 1 d . . . C4 C 0.8350(4) 0.2686(4) 0.2794(3) 0.0502(10) Uani 1 1 d . . . H4A H 0.8887 0.3085 0.2963 0.060 Uiso 1 1 calc R . . C5 C 0.7578(4) 0.2106(3) 0.3255(2) 0.0459(10) Uani 1 1 d . . . H5A H 0.7587 0.2117 0.3740 0.055 Uiso 1 1 calc R . . C6 C 0.6779(3) 0.1499(3) 0.3023(2) 0.0394(9) Uani 1 1 d . . . C7 C 0.6044(3) 0.0861(3) 0.3559(2) 0.0383(8) Uani 1 1 d . . . O2 O 0.5313(2) 0.0261(2) 0.33857(14) 0.0436(6) Uani 1 1 d . . . O3 O 0.6122(3) 0.0878(2) 0.41878(14) 0.0443(7) Uani 1 1 d . . . C8 C 0.9195(5) 0.3282(4) 0.1567(3) 0.0610(13) Uani 1 1 d . . . H8A H 0.8855 0.3526 0.1135 0.091 Uiso 1 1 calc R . . H8B H 0.9868 0.2803 0.1469 0.091 Uiso 1 1 calc R . . H8C H 0.9418 0.3906 0.1762 0.091 Uiso 1 1 calc R . . O4 O 0.3648(3) -0.0641(2) 0.29744(14) 0.0447(7) Uani 1 1 d . . . C9 C 0.2944(3) -0.1207(3) 0.2691(2) 0.0389(8) Uani 1 1 d . . . C10 C 0.2160(4) -0.1799(3) 0.3154(2) 0.0409(9) Uani 1 1 d . . . H10A H 0.2164 -0.1787 0.3639 0.049 Uiso 1 1 calc R . . C11 C 0.1373(4) -0.2406(3) 0.2922(2) 0.0445(9) Uani 1 1 d . . . C12 C 0.1389(4) -0.2432(4) 0.2206(2) 0.0467(10) Uani 1 1 d . . . H12A H 0.0857 -0.2838 0.2039 0.056 Uiso 1 1 calc R . . C13 C 0.2173(4) -0.1870(3) 0.1739(2) 0.0442(9) Uani 1 1 d . . . H13A H 0.2179 -0.1906 0.1255 0.053 Uiso 1 1 calc R . . C14 C 0.2963(4) -0.1246(3) 0.1971(2) 0.0412(9) Uani 1 1 d . A . C15 C 0.3746(4) -0.0666(4) 0.1439(2) 0.0474(10) Uani 1 1 d . . . O5 O 0.4444(3) -0.0026(2) 0.16123(15) 0.0488(7) Uani 1 1 d . A . O6 O 0.3767(3) -0.0783(3) 0.08100(16) 0.0634(9) Uani 1 1 d . A . C16 C 0.0512(4) -0.2990(4) 0.3432(2) 0.0527(11) Uani 1 1 d . . . H16A H 0.0157 -0.3507 0.3202 0.079 Uiso 1 1 calc R . . H16B H -0.0073 -0.2472 0.3607 0.079 Uiso 1 1 calc R . . H16C H 0.0890 -0.3373 0.3821 0.079 Uiso 1 1 calc R . . N1 N 0.6032(4) -0.1467(3) 0.2485(2) 0.0536(9) Uani 1 1 d . . . C17 C 0.6292(5) -0.1970(4) 0.1914(3) 0.0639(13) Uani 1 1 d . . . H17A H 0.5977 -0.1672 0.1501 0.077 Uiso 1 1 calc R . . C18 C 0.6992(5) -0.2895(5) 0.1898(3) 0.0698(15) Uani 1 1 d . . . H18A H 0.7152 -0.3219 0.1481 0.084 Uiso 1 1 calc R . . C19 C 0.7460(5) -0.3348(4) 0.2495(3) 0.0631(13) Uani 1 1 d . . . C20 C 0.7196(5) -0.2831(4) 0.3083(3) 0.0643(14) Uani 1 1 d . . . H20A H 0.7510 -0.3106 0.3501 0.077 Uiso 1 1 calc R . . C21 C 0.6474(5) -0.1911(4) 0.3060(3) 0.0577(12) Uani 1 1 d . . . H21A H 0.6285 -0.1584 0.3473 0.069 Uiso 1 1 calc R . . C22 C 0.8225(5) -0.4377(5) 0.2501(4) 0.0835(19) Uani 1 1 d . . . H22A H 0.8457 -0.4586 0.2968 0.125 Uiso 1 1 calc R . . H22B H 0.8901 -0.4254 0.2168 0.125 Uiso 1 1 calc R . . H22C H 0.7807 -0.4953 0.2372 0.125 Uiso 1 1 calc R . . N2 N 0.3773(3) 0.1737(3) 0.25374(19) 0.0472(8) Uani 1 1 d . . . C23 C 0.3384(4) 0.2112(4) 0.3144(2) 0.0478(10) Uani 1 1 d . . . H23A H 0.3616 0.1731 0.3562 0.057 Uiso 1 1 calc R . . C24 C 0.2670(4) 0.3020(4) 0.3185(3) 0.0518(11) Uani 1 1 d . . . H24A H 0.2426 0.3255 0.3624 0.062 Uiso 1 1 calc R . . C25 C 0.2304(4) 0.3593(4) 0.2583(3) 0.0548(11) Uani 1 1 d . . . C26 C 0.2705(4) 0.3207(4) 0.1962(3) 0.0587(12) Uani 1 1 d . . . H26A H 0.2476 0.3569 0.1538 0.070 Uiso 1 1 calc R . . C27 C 0.3432(4) 0.2302(4) 0.1957(2) 0.0551(11) Uani 1 1 d . . . H27A H 0.3707 0.2066 0.1522 0.066 Uiso 1 1 calc R . . C28 C 0.1508(5) 0.4573(4) 0.2615(3) 0.0681(15) Uani 1 1 d . . . H28A H 0.1245 0.4796 0.2158 0.102 Uiso 1 1 calc R . . H28B H 0.1905 0.5157 0.2751 0.102 Uiso 1 1 calc R . . H28C H 0.0853 0.4406 0.2958 0.102 Uiso 1 1 calc R . . O7 O 0.5932(3) -0.1547(2) 0.48472(18) 0.0475(7) Uani 1 1 d . . . H7 H 0.662(5) -0.169(4) 0.493(3) 0.057 Uiso 1 1 d . . . C29 C 0.5360(4) -0.2524(4) 0.4905(3) 0.0629(14) Uani 1 1 d . . . H29A H 0.5918 -0.3121 0.4822 0.094 Uiso 1 1 calc R . . H29B H 0.4811 -0.2456 0.4561 0.094 Uiso 1 1 calc R . . H29C H 0.4959 -0.2666 0.5373 0.094 Uiso 1 1 calc R . . O8 O 0.3573(3) -0.0388(3) 0.44357(15) 0.0450(7) Uani 1 1 d D . . H81 H 0.362(5) -0.042(5) 0.402(2) 0.067 Uiso 1 1 d D . . H82 H 0.288(4) -0.055(4) 0.464(3) 0.067 Uiso 1 1 d D . . O9A O 0.4284(6) 0.1678(7) 0.0037(4) 0.071(2) Uani 0.50 1 d P A 1 O10A O 0.6316(5) 0.0322(8) 0.0648(3) 0.071(2) Uani 0.50 1 d P A 1 H10B H 0.6061 0.0682 0.1041 0.085 Uiso 0.50 1 calc PR A 1 C30A C 0.7505(13) 0.0048(15) 0.0540(8) 0.077(5) Uani 0.50 1 d PU A 1 H30A H 0.7886 0.0292 0.0906 0.115 Uiso 0.50 1 calc PR A 1 H30B H 0.7816 0.0396 0.0086 0.115 Uiso 0.50 1 calc PR A 1 H30C H 0.7630 -0.0734 0.0555 0.115 Uiso 0.50 1 calc PR A 1 O9B O 0.5497(7) 0.1365(7) 0.0539(4) 0.072(2) Uani 0.50 1 d P A 2 O10B O 0.3507(6) 0.1029(7) -0.0251(4) 0.072(2) Uani 0.50 1 d P A 2 H10C H 0.3518 0.1791 -0.0298 0.086 Uiso 0.50 1 calc PR A 2 C30B C 0.2459(13) 0.0484(15) -0.0347(11) 0.091(5) Uani 0.50 1 d PU A 2 H30D H 0.1849 0.1028 -0.0453 0.136 Uiso 0.50 1 calc PR A 2 H30E H 0.2217 0.0021 0.0081 0.136 Uiso 0.50 1 calc PR A 2 H30F H 0.2628 0.0047 -0.0731 0.136 Uiso 0.50 1 calc PR A 2 Mn4 Mn 0.0000 0.0000 0.5000 0.0395(2) Uani 1 2 d S . . O11 O -0.1127(2) 0.1121(2) 0.50970(15) 0.0415(6) Uani 1 1 d . . . C31 C -0.0979(3) 0.2173(3) 0.4900(2) 0.0363(8) Uani 1 1 d . . . C32 C -0.1966(4) 0.2855(3) 0.4870(2) 0.0397(9) Uani 1 1 d . . . H32A H -0.2689 0.2560 0.4991 0.048 Uiso 1 1 calc R . . C33 C -0.1910(4) 0.3948(3) 0.4667(2) 0.0431(9) Uani 1 1 d . . . C34 C -0.0850(4) 0.4381(3) 0.4493(2) 0.0468(10) Uani 1 1 d . . . H34A H -0.0802 0.5126 0.4337 0.056 Uiso 1 1 calc R . . C35 C 0.0122(4) 0.3730(3) 0.4546(2) 0.0432(9) Uani 1 1 d . . . H35A H 0.0838 0.4042 0.4440 0.052 Uiso 1 1 calc R . . C36 C 0.0095(3) 0.2612(3) 0.4754(2) 0.0373(8) Uani 1 1 d . . . C37 C 0.1187(3) 0.1992(3) 0.4852(2) 0.0397(9) Uani 1 1 d . . . O12 O 0.1222(2) 0.0948(2) 0.49129(16) 0.0427(6) Uani 1 1 d . . . O13 O 0.2063(2) 0.2472(2) 0.48804(17) 0.0482(7) Uani 1 1 d . . . C38 C -0.2987(4) 0.4669(4) 0.4639(3) 0.0590(13) Uani 1 1 d . . . H38A H -0.2868 0.5351 0.4805 0.088 Uiso 1 1 calc R . . H38B H -0.3611 0.4315 0.4935 0.088 Uiso 1 1 calc R . . H38C H -0.3179 0.4808 0.4160 0.088 Uiso 1 1 calc R . . N3 N -0.0048(3) 0.0206(3) 0.37944(19) 0.0450(8) Uani 1 1 d . . . C39 C -0.0844(4) -0.0214(4) 0.3485(3) 0.0523(11) Uani 1 1 d . . . H39A H -0.1461 -0.0540 0.3771 0.063 Uiso 1 1 calc R . . C40 C -0.0805(5) -0.0191(4) 0.2770(3) 0.0572(12) Uani 1 1 d . . . H40A H -0.1380 -0.0517 0.2584 0.069 Uiso 1 1 calc R . . C41 C 0.0059(5) 0.0297(4) 0.2322(3) 0.0591(12) Uani 1 1 d . . . C42 C 0.0859(4) 0.0739(4) 0.2644(3) 0.0574(12) Uani 1 1 d . . . H42A H 0.1467 0.1096 0.2369 0.069 Uiso 1 1 calc R . . C43 C 0.0788(4) 0.0671(4) 0.3360(2) 0.0492(10) Uani 1 1 d . . . H43A H 0.1369 0.0973 0.3558 0.059 Uiso 1 1 calc R . . C44 C 0.0114(6) 0.0340(5) 0.1560(3) 0.0750(17) Uani 1 1 d . . . H44A H 0.0909 0.0367 0.1357 0.113 Uiso 1 1 calc R . . H44B H -0.0322 0.0984 0.1372 0.113 Uiso 1 1 calc R . . H44C H -0.0209 -0.0302 0.1444 0.113 Uiso 1 1 calc R . . Mn5 Mn 0.5000 0.5000 0.0000 0.0848(5) Uani 1 2 d S . . O14 O 0.3819(3) 0.6069(5) -0.0094(2) 0.0890(14) Uani 1 1 d . . . C45 C 0.2720(5) 0.5918(7) 0.0116(3) 0.082(2) Uani 1 1 d . . . C46 C 0.2021(5) 0.6860(7) 0.0176(3) 0.085(2) Uani 1 1 d . . . H46A H 0.2332 0.7544 0.0059 0.102 Uiso 1 1 calc R . . C47 C 0.0858(5) 0.6786(7) 0.0411(3) 0.0817(19) Uani 1 1 d . . . C48 C 0.0455(6) 0.5762(7) 0.0584(3) 0.0850(19) Uani 1 1 d . . . H48A H -0.0320 0.5700 0.0766 0.102 Uiso 1 1 calc R . . C49 C 0.1120(5) 0.4839(7) 0.0505(3) 0.086(2) Uani 1 1 d . . . H49A H 0.0791 0.4162 0.0619 0.103 Uiso 1 1 calc R . . C50 C 0.2276(5) 0.4876(6) 0.0260(3) 0.0770(18) Uani 1 1 d . . . C51 C 0.2911(5) 0.3845(7) 0.0176(3) 0.085(2) Uani 1 1 d . . . O15 O 0.4004(4) 0.3837(5) 0.0106(2) 0.0916(14) Uani 1 1 d . . . O16 O 0.2413(4) 0.3003(5) 0.0182(3) 0.0974(15) Uani 1 1 d . . . C52 C 0.0122(6) 0.7802(7) 0.0450(4) 0.098(2) Uani 1 1 d . . . H52A H -0.0493 0.7808 0.0154 0.147 Uiso 1 1 calc R . . H52B H 0.0581 0.8423 0.0289 0.147 Uiso 1 1 calc R . . H52C H -0.0203 0.7840 0.0931 0.147 Uiso 1 1 calc R . . N4 N 0.4848(4) 0.5066(4) 0.1205(2) 0.0687(12) Uani 1 1 d . . . C53 C 0.4270(5) 0.5872(5) 0.1500(3) 0.0678(14) Uani 1 1 d . . . H53A H 0.3903 0.6424 0.1209 0.081 Uiso 1 1 calc R . . C54 C 0.4175(5) 0.5946(4) 0.2204(3) 0.0612(13) Uani 1 1 d . . . H54A H 0.3753 0.6537 0.2386 0.073 Uiso 1 1 calc R . . C55 C 0.4698(4) 0.5152(4) 0.2644(3) 0.0575(12) Uani 1 1 d . . . C56 C 0.5326(5) 0.4329(5) 0.2330(3) 0.0663(14) Uani 1 1 d . . . H56A H 0.5726 0.3779 0.2604 0.080 Uiso 1 1 calc R . . C57 C 0.5366(5) 0.4316(5) 0.1619(3) 0.0713(15) Uani 1 1 d . . . H57A H 0.5786 0.3739 0.1420 0.086 Uiso 1 1 calc R . . C58 C 0.4581(6) 0.5210(5) 0.3412(3) 0.0751(16) Uani 1 1 d . . . H58A H 0.3800 0.5456 0.3565 0.113 Uiso 1 1 calc R . . H58B H 0.5111 0.5716 0.3515 0.113 Uiso 1 1 calc R . . H58C H 0.4754 0.4496 0.3657 0.113 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 0.0433(4) 0.0493(3) 0.0301(3) 0.0002(2) -0.0020(2) -0.0089(3) Mn2 0.0377(4) 0.0375(4) 0.0333(4) 0.0017(3) -0.0042(3) -0.0005(3) Mn3 0.0506(6) 0.0941(8) 0.0377(5) 0.0095(5) -0.0051(4) -0.0194(6) O1 0.0469(17) 0.0574(17) 0.0320(14) 0.0005(12) -0.0041(12) -0.0103(13) C1 0.039(2) 0.0401(19) 0.035(2) -0.0005(16) -0.0068(16) -0.0034(16) C2 0.047(2) 0.042(2) 0.036(2) 0.0006(16) -0.0017(17) -0.0059(17) C3 0.052(3) 0.042(2) 0.041(2) -0.0009(17) 0.0009(19) -0.0057(18) C4 0.054(3) 0.045(2) 0.051(3) -0.0016(19) -0.004(2) -0.0146(19) C5 0.053(3) 0.044(2) 0.040(2) -0.0005(17) -0.0038(18) -0.0094(18) C6 0.042(2) 0.0373(19) 0.038(2) 0.0003(16) -0.0043(16) -0.0023(16) C7 0.041(2) 0.0389(19) 0.033(2) 0.0005(15) -0.0050(16) 0.0001(16) O2 0.0434(16) 0.0494(15) 0.0364(15) 0.0020(12) -0.0016(12) -0.0108(13) O3 0.0485(17) 0.0539(16) 0.0293(14) 0.0018(12) -0.0021(12) -0.0101(13) C8 0.069(3) 0.062(3) 0.052(3) -0.003(2) 0.006(2) -0.025(2) O4 0.0509(17) 0.0523(16) 0.0315(14) -0.0035(12) -0.0026(12) -0.0131(13) C9 0.038(2) 0.0411(19) 0.037(2) -0.0023(16) -0.0070(16) -0.0048(16) C10 0.047(2) 0.0389(19) 0.035(2) 0.0015(16) -0.0042(17) -0.0029(17) C11 0.048(2) 0.043(2) 0.041(2) 0.0002(17) -0.0034(18) -0.0042(18) C12 0.045(2) 0.052(2) 0.042(2) -0.0002(19) -0.0060(18) -0.0103(19) C13 0.046(2) 0.050(2) 0.036(2) -0.0015(17) -0.0045(17) -0.0084(18) C14 0.045(2) 0.044(2) 0.034(2) -0.0002(16) -0.0034(16) -0.0052(17) C15 0.046(2) 0.060(3) 0.035(2) -0.0012(19) -0.0020(18) -0.008(2) O5 0.0532(18) 0.0577(17) 0.0363(16) -0.0022(13) -0.0017(13) -0.0194(14) O6 0.071(2) 0.091(2) 0.0308(16) -0.0055(16) 0.0003(15) -0.0356(19) C16 0.057(3) 0.057(3) 0.044(2) 0.000(2) 0.000(2) -0.016(2) N1 0.060(2) 0.052(2) 0.044(2) 0.0015(17) 0.0041(18) 0.0006(18) C17 0.064(3) 0.070(3) 0.054(3) -0.008(2) 0.001(2) 0.009(3) C18 0.068(4) 0.073(3) 0.067(4) -0.017(3) 0.004(3) 0.006(3) C19 0.053(3) 0.053(3) 0.082(4) -0.010(3) 0.001(3) -0.001(2) C20 0.070(3) 0.050(3) 0.069(3) 0.003(2) -0.008(3) 0.000(2) C21 0.067(3) 0.050(2) 0.051(3) 0.001(2) 0.003(2) -0.001(2) C22 0.068(4) 0.066(3) 0.116(6) -0.019(4) -0.008(4) 0.014(3) N2 0.047(2) 0.051(2) 0.041(2) 0.0035(16) -0.0034(16) -0.0026(16) C23 0.051(3) 0.050(2) 0.041(2) 0.0001(18) -0.0058(19) -0.0027(19) C24 0.053(3) 0.049(2) 0.050(3) 0.000(2) 0.001(2) -0.005(2) C25 0.051(3) 0.052(2) 0.058(3) 0.007(2) -0.004(2) -0.005(2) C26 0.061(3) 0.060(3) 0.051(3) 0.012(2) -0.011(2) -0.001(2) C27 0.066(3) 0.059(3) 0.037(2) 0.002(2) -0.004(2) -0.002(2) C28 0.066(3) 0.055(3) 0.078(4) 0.004(3) -0.002(3) 0.002(2) O7 0.0366(16) 0.0397(15) 0.066(2) -0.0035(14) -0.0113(14) -0.0005(12) C29 0.048(3) 0.044(2) 0.097(4) -0.009(3) -0.007(3) -0.004(2) O8 0.0401(16) 0.0641(18) 0.0300(14) -0.0012(13) -0.0041(12) -0.0063(13) O9A 0.053(4) 0.093(5) 0.063(5) 0.012(4) -0.006(3) -0.016(4) O10A 0.038(3) 0.146(7) 0.031(3) -0.016(4) 0.000(3) -0.011(4) C30A 0.046(6) 0.136(15) 0.054(7) -0.040(8) 0.004(5) -0.012(8) O9B 0.072(5) 0.104(6) 0.037(4) 0.000(4) 0.002(3) -0.010(4) O10B 0.055(4) 0.091(5) 0.066(5) 0.006(4) -0.008(4) -0.008(4) C30B 0.041(7) 0.114(13) 0.117(16) -0.008(10) -0.016(8) -0.003(8) Mn4 0.0343(4) 0.0330(4) 0.0484(5) 0.0028(4) -0.0022(4) 0.0006(3) O11 0.0387(15) 0.0318(13) 0.0509(17) 0.0035(12) -0.0007(12) -0.0027(11) C31 0.042(2) 0.0318(17) 0.0343(19) 0.0004(15) -0.0056(16) 0.0001(15) C32 0.038(2) 0.040(2) 0.039(2) -0.0012(16) -0.0045(16) 0.0013(16) C33 0.044(2) 0.039(2) 0.045(2) 0.0009(17) -0.0065(18) 0.0015(17) C34 0.048(2) 0.0357(19) 0.054(3) 0.0033(18) -0.0089(19) 0.0021(17) C35 0.044(2) 0.0378(19) 0.047(2) 0.0002(17) -0.0079(18) -0.0041(17) C36 0.041(2) 0.0340(18) 0.036(2) -0.0001(15) -0.0076(16) -0.0017(15) C37 0.042(2) 0.042(2) 0.034(2) 0.0016(16) -0.0039(16) -0.0033(17) O12 0.0384(15) 0.0347(13) 0.0522(17) 0.0027(12) -0.0028(12) -0.0017(11) O13 0.0406(16) 0.0429(15) 0.062(2) -0.0002(14) -0.0126(14) -0.0058(12) C38 0.047(3) 0.049(2) 0.077(3) 0.003(2) -0.010(2) 0.007(2) N3 0.0420(19) 0.0400(18) 0.051(2) 0.0004(15) -0.0050(16) 0.0027(15) C39 0.049(3) 0.047(2) 0.060(3) 0.004(2) -0.015(2) 0.0003(19) C40 0.065(3) 0.050(2) 0.059(3) -0.005(2) -0.023(2) 0.001(2) C41 0.065(3) 0.056(3) 0.053(3) 0.005(2) -0.011(2) 0.009(2) C42 0.054(3) 0.060(3) 0.053(3) 0.005(2) -0.005(2) 0.003(2) C43 0.048(2) 0.050(2) 0.047(2) 0.0009(19) -0.0027(19) -0.0058(19) C44 0.085(4) 0.087(4) 0.052(3) -0.009(3) -0.015(3) 0.021(3) Mn5 0.0531(7) 0.1498(14) 0.0524(7) -0.0061(8) -0.0002(5) -0.0328(8) O14 0.049(2) 0.164(4) 0.055(2) -0.012(3) 0.0026(17) -0.028(2) C45 0.056(3) 0.161(7) 0.032(2) -0.011(3) -0.002(2) -0.030(4) C46 0.062(4) 0.155(7) 0.040(3) -0.017(3) -0.004(2) -0.023(4) C47 0.065(4) 0.136(6) 0.045(3) -0.015(3) -0.003(3) -0.016(4) C48 0.064(4) 0.129(6) 0.062(4) -0.003(4) -0.001(3) -0.032(4) C49 0.060(4) 0.131(6) 0.065(4) 0.002(4) -0.003(3) -0.024(4) C50 0.048(3) 0.139(6) 0.044(3) 0.003(3) -0.005(2) -0.033(4) C51 0.053(3) 0.144(6) 0.055(3) 0.006(4) -0.005(3) -0.028(4) O15 0.058(2) 0.155(4) 0.064(3) -0.012(3) -0.0012(19) -0.032(3) O16 0.065(3) 0.133(4) 0.094(4) 0.006(3) -0.010(2) -0.036(3) C52 0.080(5) 0.153(7) 0.067(4) -0.031(4) -0.014(3) -0.020(5) N4 0.051(2) 0.100(4) 0.053(3) 0.000(2) -0.004(2) -0.009(2) C53 0.059(3) 0.084(4) 0.056(3) 0.013(3) -0.012(2) -0.005(3) C54 0.060(3) 0.069(3) 0.051(3) 0.002(2) -0.011(2) 0.002(2) C55 0.054(3) 0.066(3) 0.052(3) 0.002(2) -0.013(2) -0.010(2) C56 0.066(3) 0.069(3) 0.062(3) 0.002(3) -0.017(3) 0.000(3) C57 0.058(3) 0.093(4) 0.060(3) -0.001(3) -0.006(3) 0.001(3) C58 0.090(4) 0.084(4) 0.053(3) 0.003(3) -0.024(3) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.879(3) . ? Mn1 O4 1.886(3) . ? Mn1 O5 1.897(3) . ? Mn1 O2 1.897(3) . ? Mn1 N2 2.320(4) . ? Mn1 N1 2.357(4) . ? Mn2 O3 2.183(3) . ? Mn2 O3 2.183(3) 2_656 ? Mn2 O7 2.204(3) 2_656 ? Mn2 O7 2.204(3) . ? Mn2 O8 2.237(3) 2_656 ? Mn2 O8 2.237(3) . ? Mn3 O10B 2.179(8) 2_655 ? Mn3 O10B 2.179(8) . ? Mn3 O6 2.207(3) 2_655 ? Mn3 O6 2.207(3) . ? Mn3 O10A 2.209(7) 2_655 ? Mn3 O10A 2.209(7) . ? Mn3 O9A 2.222(8) . ? Mn3 O9A 2.222(8) 2_655 ? Mn3 O9B 2.272(9) 2_655 ? Mn3 O9B 2.272(9) . ? O1 C1 1.349(5) . ? C1 C6 1.403(6) . ? C1 C2 1.406(6) . ? C2 C3 1.387(6) . ? C2 H2A 0.9500 . ? C3 C4 1.396(7) . ? C3 C8 1.504(6) . ? C4 C5 1.384(6) . ? C4 H4A 0.9500 . ? C5 C6 1.407(6) . ? C5 H5A 0.9500 . ? C6 C7 1.472(5) . ? C7 O3 1.245(5) . ? C7 O2 1.290(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O4 C9 1.344(5) . ? C9 C10 1.400(6) . ? C9 C14 1.412(6) . ? C10 C11 1.395(6) . ? C10 H10A 0.9500 . ? C11 C12 1.400(6) . ? C11 C16 1.502(6) . ? C12 C13 1.387(6) . ? C12 H12A 0.9500 . ? C13 C14 1.413(6) . ? C13 H13A 0.9500 . ? C14 C15 1.465(6) . ? C15 O6 1.253(5) . ? C15 O5 1.295(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N1 C21 1.332(6) . ? N1 C17 1.348(6) . ? C17 C18 1.380(7) . ? C17 H17A 0.9500 . ? C18 C19 1.386(8) . ? C18 H18A 0.9500 . ? C19 C20 1.385(8) . ? C19 C22 1.524(7) . ? C20 C21 1.386(7) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N2 C27 1.344(6) . ? N2 C23 1.352(6) . ? C23 C24 1.375(6) . ? C23 H23A 0.9500 . ? C24 C25 1.392(7) . ? C24 H24A 0.9500 . ? C25 C26 1.386(7) . ? C25 C28 1.500(7) . ? C26 C27 1.377(7) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O7 C29 1.430(5) . ? O7 H7 0.84(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? O8 H81 0.81(4) . ? O8 H82 0.89(4) . ? O10A C30A 1.424(16) . ? O10A H10B 0.9500 . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? O10B C30B 1.502(17) . ? O10B H10C 0.9500 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? Mn4 O11 1.883(3) 2_556 ? Mn4 O11 1.883(3) . ? Mn4 O12 1.919(3) . ? Mn4 O12 1.919(3) 2_556 ? Mn4 N3 2.342(4) . ? Mn4 N3 2.342(4) 2_556 ? O11 C31 1.345(4) . ? C31 C32 1.402(5) . ? C31 C36 1.408(6) . ? C32 C33 1.382(6) . ? C32 H32A 0.9500 . ? C33 C34 1.393(6) . ? C33 C38 1.513(6) . ? C34 C35 1.370(6) . ? C34 H34A 0.9500 . ? C35 C36 1.412(5) . ? C35 H35A 0.9500 . ? C36 C37 1.481(5) . ? C37 O13 1.249(5) . ? C37 O12 1.299(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? N3 C43 1.342(6) . ? N3 C39 1.350(6) . ? C39 C40 1.388(7) . ? C39 H39A 0.9500 . ? C40 C41 1.390(8) . ? C40 H40A 0.9500 . ? C41 C42 1.382(8) . ? C41 C44 1.477(7) . ? C42 C43 1.384(7) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? Mn5 O14 1.876(5) 2_665 ? Mn5 O14 1.876(5) . ? Mn5 O15 1.920(5) 2_665 ? Mn5 O15 1.920(5) . ? Mn5 N4 2.350(5) 2_665 ? Mn5 N4 2.350(5) . ? O14 C45 1.339(7) . ? C45 C46 1.404(10) . ? C45 C50 1.428(10) . ? C46 C47 1.408(9) . ? C46 H46A 0.9500 . ? C47 C48 1.391(10) . ? C47 C52 1.499(10) . ? C48 C49 1.371(10) . ? C48 H48A 0.9500 . ? C49 C50 1.400(8) . ? C49 H49A 0.9500 . ? C50 C51 1.468(10) . ? C51 O16 1.247(9) . ? C51 O15 1.286(7) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? N4 C57 1.324(7) . ? N4 C53 1.338(7) . ? C53 C54 1.381(8) . ? C53 H53A 0.9500 . ? C54 C55 1.390(7) . ? C54 H54A 0.9500 . ? C55 C56 1.395(8) . ? C55 C58 1.500(7) . ? C56 C57 1.386(8) . ? C56 H56A 0.9500 . ? C57 H57A 0.9500 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 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 O1 Mn1 O4 179.28(14) . . ? O1 Mn1 O5 86.47(13) . . ? O4 Mn1 O5 93.16(13) . . ? O1 Mn1 O2 93.63(13) . . ? O4 Mn1 O2 86.76(12) . . ? O5 Mn1 O2 178.55(14) . . ? O1 Mn1 N2 88.75(13) . . ? O4 Mn1 N2 90.64(13) . . ? O5 Mn1 N2 91.85(14) . . ? O2 Mn1 N2 89.60(13) . . ? O1 Mn1 N1 90.13(14) . . ? O4 Mn1 N1 90.49(14) . . ? O5 Mn1 N1 90.10(14) . . ? O2 Mn1 N1 88.46(14) . . ? N2 Mn1 N1 177.69(15) . . ? O3 Mn2 O3 180.00(12) . 2_656 ? O3 Mn2 O7 87.76(12) . 2_656 ? O3 Mn2 O7 92.24(12) 2_656 2_656 ? O3 Mn2 O7 92.24(12) . . ? O3 Mn2 O7 87.76(12) 2_656 . ? O7 Mn2 O7 180.0 2_656 . ? O3 Mn2 O8 76.53(11) . 2_656 ? O3 Mn2 O8 103.47(11) 2_656 2_656 ? O7 Mn2 O8 92.04(12) 2_656 2_656 ? O7 Mn2 O8 87.96(12) . 2_656 ? O3 Mn2 O8 103.47(11) . . ? O3 Mn2 O8 76.53(11) 2_656 . ? O7 Mn2 O8 87.96(12) 2_656 . ? O7 Mn2 O8 92.04(12) . . ? O8 Mn2 O8 179.999(1) 2_656 . ? O10B Mn3 O10B 180.0 2_655 . ? O10B Mn3 O6 82.6(2) 2_655 2_655 ? O10B Mn3 O6 97.4(2) . 2_655 ? O10B Mn3 O6 97.4(2) 2_655 . ? O10B Mn3 O6 82.6(2) . . ? O6 Mn3 O6 180.0 2_655 . ? O10B Mn3 O10A 127.4(3) 2_655 2_655 ? O10B Mn3 O10A 52.6(3) . 2_655 ? O6 Mn3 O10A 99.9(2) 2_655 2_655 ? O6 Mn3 O10A 80.1(2) . 2_655 ? O10B Mn3 O10A 52.6(3) 2_655 . ? O10B Mn3 O10A 127.4(3) . . ? O6 Mn3 O10A 80.1(2) 2_655 . ? O6 Mn3 O10A 99.9(2) . . ? O10A Mn3 O10A 180.0 2_655 . ? O10B Mn3 O9A 140.8(3) 2_655 . ? O10B Mn3 O9A 39.2(3) . . ? O6 Mn3 O9A 82.7(2) 2_655 . ? O6 Mn3 O9A 97.3(2) . . ? O10A Mn3 O9A 90.9(3) 2_655 . ? O10A Mn3 O9A 89.1(3) . . ? O10B Mn3 O9A 39.2(3) 2_655 2_655 ? O10B Mn3 O9A 140.8(3) . 2_655 ? O6 Mn3 O9A 97.3(2) 2_655 2_655 ? O6 Mn3 O9A 82.7(2) . 2_655 ? O10A Mn3 O9A 89.1(3) 2_655 2_655 ? O10A Mn3 O9A 90.9(3) . 2_655 ? O9A Mn3 O9A 180.0 . 2_655 ? O10B Mn3 O9B 86.4(3) 2_655 2_655 ? O10B Mn3 O9B 93.6(3) . 2_655 ? O6 Mn3 O9B 101.0(2) 2_655 2_655 ? O6 Mn3 O9B 79.0(2) . 2_655 ? O10A Mn3 O9B 41.3(3) 2_655 2_655 ? O10A Mn3 O9B 138.7(3) . 2_655 ? O9A Mn3 O9B 132.1(3) . 2_655 ? O9A Mn3 O9B 47.9(3) 2_655 2_655 ? O10B Mn3 O9B 93.6(3) 2_655 . ? O10B Mn3 O9B 86.4(3) . . ? O6 Mn3 O9B 79.0(2) 2_655 . ? O6 Mn3 O9B 101.0(2) . . ? O10A Mn3 O9B 138.7(3) 2_655 . ? O10A Mn3 O9B 41.3(3) . . ? O9A Mn3 O9B 47.9(3) . . ? O9A Mn3 O9B 132.1(3) 2_655 . ? O9B Mn3 O9B 180.0 2_655 . ? C1 O1 Mn1 125.9(3) . . ? O1 C1 C6 124.3(4) . . ? O1 C1 C2 116.7(4) . . ? C6 C1 C2 119.0(4) . . ? C3 C2 C1 121.8(4) . . ? C3 C2 H2A 119.1 . . ? C1 C2 H2A 119.1 . . ? C2 C3 C4 118.9(4) . . ? C2 C3 C8 119.9(4) . . ? C4 C3 C8 121.1(4) . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 121.5(4) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C1 C6 C5 118.7(4) . . ? C1 C6 C7 124.3(4) . . ? C5 C6 C7 116.9(4) . . ? O3 C7 O2 118.6(4) . . ? O3 C7 C6 121.0(4) . . ? O2 C7 C6 120.5(4) . . ? C7 O2 Mn1 130.1(3) . . ? C7 O3 Mn2 122.1(3) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 O4 Mn1 126.5(3) . . ? O4 C9 C10 116.5(4) . . ? O4 C9 C14 124.2(4) . . ? C10 C9 C14 119.3(4) . . ? C11 C10 C9 121.8(4) . . ? C11 C10 H10A 119.1 . . ? C9 C10 H10A 119.1 . . ? C10 C11 C12 118.6(4) . . ? C10 C11 C16 120.2(4) . . ? C12 C11 C16 121.2(4) . . ? C13 C12 C11 120.7(4) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C12 C13 C14 121.0(4) . . ? C12 C13 H13A 119.5 . . ? C14 C13 H13A 119.5 . . ? C9 C14 C13 118.6(4) . . ? C9 C14 C15 124.2(4) . . ? C13 C14 C15 117.2(4) . . ? O6 C15 O5 118.5(4) . . ? O6 C15 C14 121.1(4) . . ? O5 C15 C14 120.4(4) . . ? C15 O5 Mn1 130.1(3) . . ? C15 O6 Mn3 122.3(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C21 N1 C17 116.9(4) . . ? C21 N1 Mn1 120.0(3) . . ? C17 N1 Mn1 123.1(3) . . ? N1 C17 C18 123.5(5) . . ? N1 C17 H17A 118.2 . . ? C18 C17 H17A 118.2 . . ? C17 C18 C19 119.3(5) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? C18 C19 C20 117.3(5) . . ? C18 C19 C22 121.0(6) . . ? C20 C19 C22 121.8(6) . . ? C19 C20 C21 120.0(5) . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? N1 C21 C20 123.0(5) . . ? N1 C21 H21A 118.5 . . ? C20 C21 H21A 118.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C27 N2 C23 116.7(4) . . ? C27 N2 Mn1 121.2(3) . . ? C23 N2 Mn1 122.0(3) . . ? N2 C23 C24 123.2(4) . . ? N2 C23 H23A 118.4 . . ? C24 C23 H23A 118.4 . . ? C23 C24 C25 120.0(5) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C26 C25 C24 116.6(4) . . ? C26 C25 C28 122.3(5) . . ? C24 C25 C28 121.1(5) . . ? C27 C26 C25 120.4(4) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? N2 C27 C26 123.1(5) . . ? N2 C27 H27A 118.5 . . ? C26 C27 H27A 118.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C29 O7 Mn2 121.7(3) . . ? C29 O7 H7 110(4) . . ? Mn2 O7 H7 123(4) . . ? O7 C29 H29A 109.5 . . ? O7 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O7 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Mn2 O8 H81 125(4) . . ? Mn2 O8 H82 124(4) . . ? H81 O8 H82 112(5) . . ? C30A O10A Mn3 127.0(7) . . ? C30A O10A H10B 116.5 . . ? Mn3 O10A H10B 116.5 . . ? O10A C30A H30A 109.5 . . ? O10A C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? O10A C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C30B O10B Mn3 117.2(8) . . ? C30B O10B H10C 121.4 . . ? Mn3 O10B H10C 121.4 . . ? O10B C30B H30D 109.5 . . ? O10B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? O10B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? O11 Mn4 O11 180.00(18) 2_556 . ? O11 Mn4 O12 86.83(11) 2_556 . ? O11 Mn4 O12 93.17(11) . . ? O11 Mn4 O12 93.17(11) 2_556 2_556 ? O11 Mn4 O12 86.83(11) . 2_556 ? O12 Mn4 O12 179.999(1) . 2_556 ? O11 Mn4 N3 88.67(12) 2_556 . ? O11 Mn4 N3 91.33(12) . . ? O12 Mn4 N3 91.50(13) . . ? O12 Mn4 N3 88.50(13) 2_556 . ? O11 Mn4 N3 91.33(12) 2_556 2_556 ? O11 Mn4 N3 88.67(12) . 2_556 ? O12 Mn4 N3 88.50(13) . 2_556 ? O12 Mn4 N3 91.50(13) 2_556 2_556 ? N3 Mn4 N3 180.00(17) . 2_556 ? C31 O11 Mn4 125.5(2) . . ? O11 C31 C32 116.7(4) . . ? O11 C31 C36 123.7(3) . . ? C32 C31 C36 119.6(3) . . ? C33 C32 C31 121.3(4) . . ? C33 C32 H32A 119.3 . . ? C31 C32 H32A 119.3 . . ? C32 C33 C34 119.3(4) . . ? C32 C33 C38 120.4(4) . . ? C34 C33 C38 120.3(4) . . ? C35 C34 C33 119.9(4) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 122.1(4) . . ? C34 C35 H35A 118.9 . . ? C36 C35 H35A 118.9 . . ? C31 C36 C35 117.6(3) . . ? C31 C36 C37 124.2(3) . . ? C35 C36 C37 118.1(4) . . ? O13 C37 O12 120.6(4) . . ? O13 C37 C36 120.0(3) . . ? O12 C37 C36 119.5(4) . . ? C37 O12 Mn4 129.6(3) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C43 N3 C39 115.3(4) . . ? C43 N3 Mn4 121.3(3) . . ? C39 N3 Mn4 123.1(3) . . ? N3 C39 C40 123.1(5) . . ? N3 C39 H39A 118.4 . . ? C40 C39 H39A 118.4 . . ? C39 C40 C41 121.4(5) . . ? C39 C40 H40A 119.3 . . ? C41 C40 H40A 119.3 . . ? C42 C41 C40 114.9(5) . . ? C42 C41 C44 122.6(5) . . ? C40 C41 C44 122.4(5) . . ? C43 C42 C41 121.0(5) . . ? C43 C42 H42A 119.5 . . ? C41 C42 H42A 119.5 . . ? N3 C43 C42 124.2(5) . . ? N3 C43 H43A 117.9 . . ? C42 C43 H43A 117.9 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O14 Mn5 O14 180.0 2_665 . ? O14 Mn5 O15 94.0(2) 2_665 2_665 ? O14 Mn5 O15 86.0(2) . 2_665 ? O14 Mn5 O15 86.0(2) 2_665 . ? O14 Mn5 O15 94.0(2) . . ? O15 Mn5 O15 180.0 2_665 . ? O14 Mn5 N4 90.80(17) 2_665 2_665 ? O14 Mn5 N4 89.21(17) . 2_665 ? O15 Mn5 N4 92.35(18) 2_665 2_665 ? O15 Mn5 N4 87.65(18) . 2_665 ? O14 Mn5 N4 89.20(17) 2_665 . ? O14 Mn5 N4 90.80(17) . . ? O15 Mn5 N4 87.65(18) 2_665 . ? O15 Mn5 N4 92.35(18) . . ? N4 Mn5 N4 180.0 2_665 . ? C45 O14 Mn5 124.6(5) . . ? O14 C45 C46 115.4(7) . . ? O14 C45 C50 122.7(7) . . ? C46 C45 C50 121.8(6) . . ? C45 C46 C47 119.8(7) . . ? C45 C46 H46A 120.1 . . ? C47 C46 H46A 120.1 . . ? C48 C47 C46 117.5(7) . . ? C48 C47 C52 123.7(6) . . ? C46 C47 C52 118.8(7) . . ? C49 C48 C47 123.2(6) . . ? C49 C48 H48A 118.4 . . ? C47 C48 H48A 118.4 . . ? C48 C49 C50 121.1(7) . . ? C48 C49 H49A 119.4 . . ? C50 C49 H49A 119.4 . . ? C49 C50 C45 116.4(7) . . ? C49 C50 C51 117.1(7) . . ? C45 C50 C51 126.5(6) . . ? O16 C51 O15 121.0(8) . . ? O16 C51 C50 121.4(6) . . ? O15 C51 C50 117.6(7) . . ? C51 O15 Mn5 130.5(6) . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C57 N4 C53 117.0(5) . . ? C57 N4 Mn5 121.0(4) . . ? C53 N4 Mn5 122.0(4) . . ? N4 C53 C54 123.7(5) . . ? N4 C53 H53A 118.2 . . ? C54 C53 H53A 118.2 . . ? C53 C54 C55 119.7(5) . . ? C53 C54 H54A 120.2 . . ? C55 C54 H54A 120.2 . . ? C54 C55 C56 116.3(5) . . ? C54 C55 C58 120.2(5) . . ? C56 C55 C58 123.5(5) . . ? C57 C56 C55 120.0(5) . . ? C57 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? N4 C57 C56 123.3(6) . . ? N4 C57 H57A 118.3 . . ? C56 C57 H57A 118.3 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 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 O7 H7 O13 0.84(5) 1.84(5) 2.647(4) 160(5) 2_656 O8 H81 O4 0.81(4) 2.10(4) 2.903(4) 174(6) . O8 H82 O11 0.89(4) 2.23(4) 3.105(4) 165(5) 2_556 O10A H10B O1 0.95 1.97 2.852(7) 152.9 . O10B H10C O16 0.95 2.17 2.895(11) 131.9 . _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.769 _refine_diff_density_min -1.010 _refine_diff_density_rms 0.106