_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 'Inorg. Chem.' _publ_section_title ; In Situ Ligand Transformation as a Synthetic Strategy for Transition Metal Complexes: The Structure of a Barrel-shaped Mn(II)14 Aggregate ; loop_ _publ_author_name _publ_author_address 'Muhammad Usman Anwar' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Lianne M.C. Beltran' ; 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 ; 'Sven Pfirrmann' ; 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_dhb130 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H16 Cl Mn N6 O3' _chemical_formula_weight 394.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.9857(4) _cell_length_b 11.7814(7) _cell_length_c 18.9519(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1559.77(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7740 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 27.95 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 0.894 _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 7872 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.96 _reflns_number_total 3473 _reflns_number_gt 3412 _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. ; _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^)+(0.0329P)^2^+1.5273P] 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 0.004(18) _refine_ls_number_reflns 3473 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.21011(5) 0.50846(3) 0.120507(16) 0.01297(9) Uani 1 1 d . . . Cl1 Cl -0.12884(8) 0.57869(5) 0.08612(3) 0.01805(12) Uani 1 1 d . . . O1 O 0.1234(3) 0.43523(14) 0.20231(8) 0.0169(3) Uani 1 1 d . . . O2 O 0.0643(3) 0.30303(15) 0.28037(9) 0.0206(4) Uani 1 1 d . . . C1 C 0.1071(3) 0.3298(2) 0.21950(12) 0.0147(4) Uani 1 1 d . . . C2 C 0.1411(4) 0.2396(2) 0.16509(12) 0.0162(5) Uani 1 1 d . . . C3 C 0.1328(4) 0.1274(2) 0.18974(12) 0.0183(5) Uani 1 1 d . . . H3A H 0.1092 0.1141 0.2384 0.022 Uiso 1 1 calc R . . C4 C 0.1579(4) 0.0358(2) 0.14541(13) 0.0197(5) Uani 1 1 d . . . H4A H 0.1483 -0.0395 0.1630 0.024 Uiso 1 1 calc R . . C5 C 0.1980(4) 0.0554(2) 0.07394(13) 0.0208(5) Uani 1 1 d . . . H5A H 0.2175 -0.0069 0.0430 0.025 Uiso 1 1 calc R . . C6 C 0.2092(4) 0.1648(2) 0.04851(12) 0.0177(4) Uani 1 1 d . . . H6A H 0.2385 0.1769 0.0001 0.021 Uiso 1 1 calc R . . C7 C 0.1781(3) 0.25881(19) 0.09260(12) 0.0145(4) Uani 1 1 d . . . N1 N 0.1886(3) 0.37074(16) 0.06303(10) 0.0139(4) Uani 1 1 d . . . N2 N 0.1795(3) 0.36999(17) -0.00587(10) 0.0156(4) Uani 1 1 d . . . C8 C 0.2112(4) 0.46037(19) -0.04554(11) 0.0158(4) Uani 1 1 d . . . C9 C 0.1750(3) 0.43875(19) -0.11930(13) 0.0184(5) Uani 1 1 d . . . N3 N 0.1426(4) 0.4223(2) -0.17745(11) 0.0260(5) Uani 1 1 d . . . C10 C 0.2791(4) 0.5737(2) -0.02597(11) 0.0153(4) Uani 1 1 d . . . N4 N 0.3133(3) 0.64719(18) -0.07859(11) 0.0181(4) Uani 1 1 d . . . H41 H 0.308(4) 0.623(3) -0.1203(16) 0.022 Uiso 1 1 d . . . H42 H 0.354(5) 0.708(3) -0.0699(16) 0.022 Uiso 1 1 d . . . N5 N 0.3066(3) 0.59869(16) 0.04076(10) 0.0155(4) Uani 1 1 d . . . C11 C 0.3610(4) 0.7165(2) 0.05903(12) 0.0175(5) Uani 1 1 d . . . H11A H 0.2549 0.7689 0.0474 0.021 Uiso 1 1 calc R . . H11B H 0.4751 0.7395 0.0316 0.021 Uiso 1 1 calc R . . C12 C 0.4046(4) 0.7220(2) 0.13748(12) 0.0171(5) Uani 1 1 d . . . H12A H 0.5336 0.6906 0.1469 0.020 Uiso 1 1 calc R . . H12B H 0.4022 0.8019 0.1537 0.020 Uiso 1 1 calc R . . N6 N 0.2581(3) 0.65516(17) 0.17561(10) 0.0161(4) Uani 1 1 d . . . H61 H 0.295(5) 0.638(2) 0.2165(16) 0.019 Uiso 1 1 d . . . H62 H 0.153(5) 0.694(3) 0.1798(16) 0.019 Uiso 1 1 d . . . O3 O 0.5162(3) 0.46054(17) 0.14760(10) 0.0245(4) Uani 1 1 d . . . H3 H 0.597(5) 0.486(3) 0.1294(18) 0.037 Uiso 1 1 d . . . C13 C 0.5918(5) 0.3848(3) 0.19729(19) 0.0414(8) Uani 1 1 d . . . H13A H 0.5002 0.3748 0.2360 0.062 Uiso 1 1 calc R . . H13B H 0.7121 0.4152 0.2160 0.062 Uiso 1 1 calc R . . H13C H 0.6159 0.3114 0.1747 0.062 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 0.01806(16) 0.01207(15) 0.00877(14) 0.00055(13) 0.00146(13) -0.00112(14) Cl1 0.0175(2) 0.0178(3) 0.0189(3) 0.0008(2) 0.0001(2) 0.0007(2) O1 0.0234(8) 0.0151(8) 0.0121(7) 0.0005(6) 0.0030(7) -0.0012(7) O2 0.0337(10) 0.0170(8) 0.0113(7) 0.0004(6) 0.0018(7) -0.0020(7) C1 0.0132(11) 0.0179(11) 0.0131(10) -0.0001(9) -0.0008(9) -0.0002(9) C2 0.0158(11) 0.0172(11) 0.0155(11) -0.0006(9) 0.0007(9) -0.0004(9) C3 0.0203(11) 0.0191(11) 0.0155(10) 0.0021(9) 0.0022(10) -0.0015(10) C4 0.0235(13) 0.0136(10) 0.0221(11) 0.0024(9) 0.0007(9) 0.0007(9) C5 0.0245(12) 0.0168(11) 0.0211(11) -0.0044(9) 0.0034(10) -0.0010(10) C6 0.0203(11) 0.0182(11) 0.0145(10) -0.0032(8) 0.0023(10) 0.0017(10) C7 0.0108(11) 0.0158(10) 0.0169(10) 0.0011(9) 0.0000(9) -0.0003(8) N1 0.0158(10) 0.0150(9) 0.0110(8) -0.0005(7) 0.0024(7) -0.0016(8) N2 0.0160(10) 0.0193(9) 0.0116(8) -0.0003(7) 0.0015(7) 0.0010(8) C8 0.0180(10) 0.0183(10) 0.0112(9) -0.0010(8) 0.0027(9) -0.0007(10) C9 0.0204(12) 0.0178(10) 0.0171(11) 0.0032(9) 0.0019(9) -0.0018(9) N3 0.0321(12) 0.0307(12) 0.0152(10) -0.0008(9) -0.0003(9) -0.0038(10) C10 0.0130(10) 0.0193(11) 0.0135(10) 0.0010(8) 0.0001(9) 0.0011(10) N4 0.0274(11) 0.0156(9) 0.0114(9) 0.0002(7) 0.0014(8) -0.0023(9) N5 0.0194(10) 0.0147(9) 0.0124(8) 0.0016(7) -0.0006(8) -0.0026(8) C11 0.0215(11) 0.0165(11) 0.0147(11) 0.0011(9) 0.0006(9) -0.0028(10) C12 0.0209(12) 0.0158(10) 0.0146(11) -0.0003(8) 0.0004(9) -0.0026(9) N6 0.0228(12) 0.0152(9) 0.0104(8) 0.0004(7) 0.0008(8) 0.0005(8) O3 0.0206(9) 0.0277(10) 0.0252(9) 0.0106(8) -0.0005(8) 0.0007(8) C13 0.0276(16) 0.0443(19) 0.052(2) 0.0289(16) -0.0106(14) -0.0009(14) _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 1.8747(16) . ? Mn1 N1 1.9601(19) . ? Mn1 N5 1.9668(19) . ? Mn1 N6 2.047(2) . ? Mn1 O3 2.2702(19) . ? Mn1 Cl1 2.5915(7) . ? O1 C1 1.289(3) . ? O2 C1 1.233(3) . ? C1 C2 1.500(3) . ? C2 C3 1.404(3) . ? C2 C7 1.416(3) . ? C3 C4 1.378(3) . ? C3 H3A 0.9500 . ? C4 C5 1.402(3) . ? C4 H4A 0.9500 . ? C5 C6 1.378(3) . ? C5 H5A 0.9500 . ? C6 C7 1.404(3) . ? C6 H6A 0.9500 . ? C7 N1 1.435(3) . ? N1 N2 1.307(3) . ? N2 C8 1.322(3) . ? C8 C9 1.443(3) . ? C8 C10 1.464(3) . ? C9 N3 1.141(3) . ? C10 N5 1.313(3) . ? C10 N4 1.342(3) . ? N4 H41 0.84(3) . ? N4 H42 0.79(3) . ? N5 C11 1.480(3) . ? C11 C12 1.519(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N6 1.480(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N6 H61 0.84(3) . ? N6 H62 0.87(3) . ? O3 C13 1.401(3) . ? O3 H3 0.73(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 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 N1 93.09(7) . . ? O1 Mn1 N5 174.19(8) . . ? N1 Mn1 N5 92.68(8) . . ? O1 Mn1 N6 91.12(7) . . ? N1 Mn1 N6 174.30(9) . . ? N5 Mn1 N6 83.08(8) . . ? O1 Mn1 O3 90.17(7) . . ? N1 Mn1 O3 89.55(8) . . ? N5 Mn1 O3 89.17(8) . . ? N6 Mn1 O3 86.58(8) . . ? O1 Mn1 Cl1 93.42(6) . . ? N1 Mn1 Cl1 93.12(6) . . ? N5 Mn1 Cl1 86.97(6) . . ? N6 Mn1 Cl1 90.47(6) . . ? O3 Mn1 Cl1 175.41(5) . . ? C1 O1 Mn1 132.92(15) . . ? O2 C1 O1 120.3(2) . . ? O2 C1 C2 120.0(2) . . ? O1 C1 C2 119.7(2) . . ? C3 C2 C7 118.7(2) . . ? C3 C2 C1 115.6(2) . . ? C7 C2 C1 125.6(2) . . ? C4 C3 C2 122.0(2) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C3 C4 C5 119.1(2) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? C6 C5 C4 120.2(2) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 C7 121.4(2) . . ? C5 C6 H6A 119.3 . . ? C7 C6 H6A 119.3 . . ? C6 C7 C2 118.7(2) . . ? C6 C7 N1 119.0(2) . . ? C2 C7 N1 122.3(2) . . ? N2 N1 C7 112.43(18) . . ? N2 N1 Mn1 124.36(15) . . ? C7 N1 Mn1 123.21(14) . . ? N1 N2 C8 123.7(2) . . ? N2 C8 C9 112.3(2) . . ? N2 C8 C10 130.1(2) . . ? C9 C8 C10 117.57(19) . . ? N3 C9 C8 178.6(3) . . ? N5 C10 N4 123.0(2) . . ? N5 C10 C8 119.7(2) . . ? N4 C10 C8 117.24(19) . . ? C10 N4 H41 118(2) . . ? C10 N4 H42 120(2) . . ? H41 N4 H42 121(3) . . ? C10 N5 C11 118.26(19) . . ? C10 N5 Mn1 124.68(16) . . ? C11 N5 Mn1 114.53(14) . . ? N5 C11 C12 108.73(19) . . ? N5 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? N5 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N6 C12 C11 108.4(2) . . ? N6 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? N6 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? C12 N6 Mn1 108.27(14) . . ? C12 N6 H61 111(2) . . ? Mn1 N6 H61 109(2) . . ? C12 N6 H62 110(2) . . ? Mn1 N6 H62 111(2) . . ? H61 N6 H62 108(3) . . ? C13 O3 Mn1 131.72(18) . . ? C13 O3 H3 107(3) . . ? Mn1 O3 H3 121(3) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 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 N4 H41 O2 0.84(3) 2.26(3) 2.867(3) 129(3) 2_564 N4 H42 Cl1 0.79(3) 2.53(3) 3.258(2) 153(3) 4_565 N6 H61 N3 0.84(3) 2.18(3) 3.012(3) 172(3) 2_565 N6 H62 O2 0.87(3) 2.12(3) 2.967(3) 163(3) 3 O3 H3 Cl1 0.73(4) 2.35(4) 3.073(2) 172(4) 1_655 _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.426 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.064 ############################################################# data_dhb93 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H84 Mn3 N32 O10' _chemical_formula_weight 1626.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 11.3977(5) _cell_length_b 19.3147(9) _cell_length_c 17.6692(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.559(1) _cell_angle_gamma 90.00 _cell_volume 3781.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8719 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.99 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1694 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.894 _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 17303 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.05 _reflns_number_total 7394 _reflns_number_gt 6263 _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. Coordinates of H-atoms bonded to O or N were refined with restrained O-H or N-H distances. ; _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^)+(0.0562P)^2^+7.5878P] 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 7394 _refine_ls_number_parameters 571 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.5000 0.5000 0.5000 0.02281(17) Uani 1 2 d S . . Mn2 Mn 0.34033(4) 0.39674(3) 0.36082(3) 0.02344(14) Uani 1 1 d . . . O1 O 0.4926(2) 0.41034(12) 0.43030(13) 0.0240(5) Uani 1 1 d . . . H1 H 0.545(4) 0.411(2) 0.412(2) 0.029 Uiso 1 1 d . . . O2 O 0.33123(19) 0.47908(12) 0.54063(12) 0.0263(5) Uani 1 1 d . . . O3 O 0.2546(2) 0.39644(13) 0.45493(13) 0.0310(5) Uani 1 1 d . . . C1 C 0.2497(3) 0.43713(17) 0.51006(18) 0.0251(7) Uani 1 1 d . . . C2 C 0.1359(3) 0.43235(17) 0.53928(19) 0.0253(7) Uani 1 1 d . . . C3 C 0.0352(3) 0.40289(18) 0.4891(2) 0.0298(7) Uani 1 1 d . . . H3A H 0.0417 0.3881 0.4389 0.036 Uiso 1 1 calc R . . C4 C -0.0738(3) 0.39456(19) 0.5100(2) 0.0349(8) Uani 1 1 d . . . H4A H -0.1418 0.3756 0.4743 0.042 Uiso 1 1 calc R . . C5 C -0.0812(3) 0.4146(2) 0.5841(2) 0.0372(9) Uani 1 1 d . . . H5A H -0.1542 0.4072 0.6002 0.045 Uiso 1 1 calc R . . C6 C 0.0149(3) 0.44467(19) 0.6347(2) 0.0339(8) Uani 1 1 d . . . H6A H 0.0074 0.4585 0.6849 0.041 Uiso 1 1 calc R . . C7 C 0.1245(3) 0.45535(17) 0.61288(19) 0.0275(7) Uani 1 1 d . . . N1 N 0.2205(3) 0.48883(15) 0.66485(16) 0.0286(6) Uani 1 1 d . . . H11 H 0.282(4) 0.500(2) 0.652(2) 0.034 Uiso 1 1 d . . . N2 N 0.2035(3) 0.50594(16) 0.73412(16) 0.0309(6) Uani 1 1 d . . . C8 C 0.2835(3) 0.53975(19) 0.78561(19) 0.0310(7) Uani 1 1 d . . . C9 C 0.2456(3) 0.5545(2) 0.8564(2) 0.0394(9) Uani 1 1 d . . . N3 N 0.2146(3) 0.5677(2) 0.9118(2) 0.0546(10) Uani 1 1 d . . . C10 C 0.4018(3) 0.56640(17) 0.78056(19) 0.0269(7) Uani 1 1 d . . . N4 N 0.4442(2) 0.56272(15) 0.71671(16) 0.0289(6) Uani 1 1 d . . . N5 N 0.5535(2) 0.59359(14) 0.73778(16) 0.0271(6) Uani 1 1 d . . . N6 N 0.5732(2) 0.61487(15) 0.81055(16) 0.0288(6) Uani 1 1 d . . . N7 N 0.4778(3) 0.59815(16) 0.83952(16) 0.0322(6) Uani 1 1 d . . . O4 O 0.3642(2) 0.29866(12) 0.36105(13) 0.0309(5) Uani 1 1 d . . . O5 O 0.3316(3) 0.18761(16) 0.3438(2) 0.0639(10) Uani 1 1 d . . . C11 C 0.2920(4) 0.2477(2) 0.3379(2) 0.0391(9) Uani 1 1 d . . . C12 C 0.1610(4) 0.2613(2) 0.3058(2) 0.0431(10) Uani 1 1 d . . . C13 C 0.0833(4) 0.2040(3) 0.2987(2) 0.0638(15) Uani 1 1 d . . . H13A H 0.1162 0.1596 0.3138 0.077 Uiso 1 1 calc R . . C14 C -0.0381(5) 0.2108(4) 0.2706(3) 0.079(2) Uani 1 1 d . . . H14A H -0.0892 0.1713 0.2656 0.095 Uiso 1 1 calc R . . C15 C -0.0860(4) 0.2751(4) 0.2497(3) 0.0763(19) Uani 1 1 d . . . H15A H -0.1708 0.2799 0.2307 0.092 Uiso 1 1 calc R . . C16 C -0.0130(4) 0.3332(3) 0.2558(2) 0.0557(12) Uani 1 1 d . . . H16A H -0.0478 0.3775 0.2418 0.067 Uiso 1 1 calc R . . C17 C 0.1126(3) 0.3266(2) 0.28259(19) 0.0397(9) Uani 1 1 d . . . N8 N 0.1852(2) 0.38684(16) 0.28245(16) 0.0318(7) Uani 1 1 d . . . N9 N 0.1326(3) 0.43082(19) 0.22666(18) 0.0420(8) Uani 1 1 d . A . C18 C 0.1692(4) 0.4948(2) 0.2237(2) 0.0459(10) Uani 1 1 d . . . C19A C 0.0910(9) 0.5372(5) 0.1663(6) 0.044(2) Uiso 0.50 1 d P A 1 N10A N 0.0428(15) 0.5734(7) 0.1194(6) 0.070(4) Uani 0.50 1 d PU A 1 C19B C 0.1199(9) 0.5339(5) 0.1488(6) 0.044(2) Uiso 0.50 1 d P A 2 N10B N 0.0700(13) 0.5603(8) 0.0937(6) 0.068(4) Uani 0.50 1 d PU A 2 C20 C 0.2596(3) 0.5308(2) 0.2819(2) 0.0333(8) Uani 1 1 d . A . N11 N 0.3208(2) 0.49897(15) 0.34563(15) 0.0260(6) Uani 1 1 d . . . N12 N 0.3898(2) 0.54809(15) 0.38819(16) 0.0269(6) Uani 1 1 d . A . N13 N 0.3695(3) 0.60735(15) 0.35042(17) 0.0318(6) Uani 1 1 d . . . N14 N 0.2872(3) 0.59789(17) 0.28261(18) 0.0379(7) Uani 1 1 d . A . N21 N 0.5815(3) 0.19906(18) 0.4173(2) 0.0427(8) Uani 1 1 d . C . H21 H 0.504(4) 0.186(2) 0.379(3) 0.051 Uiso 1 1 d . . . C21 C 0.5757(4) 0.2210(3) 0.4989(3) 0.0633(13) Uani 1 1 d . . . H21A H 0.5206 0.2612 0.4947 0.076 Uiso 1 1 calc R . . H21B H 0.5397 0.1826 0.5230 0.076 Uiso 1 1 calc R . . C22 C 0.6926(5) 0.2398(3) 0.5515(3) 0.0730(15) Uani 1 1 d . . . H22A H 0.6795 0.2536 0.6023 0.110 Uiso 1 1 calc R . . H22B H 0.7286 0.2785 0.5290 0.110 Uiso 1 1 calc R . . H22C H 0.7471 0.1999 0.5581 0.110 Uiso 1 1 calc R . . C23 C 0.6427(4) 0.2550(2) 0.3804(3) 0.0527(11) Uani 1 1 d . . . H23A H 0.6202 0.3010 0.3974 0.063 Uiso 1 1 calc R . . H23B H 0.7313 0.2499 0.3983 0.063 Uiso 1 1 calc R . . C24 C 0.6072(5) 0.2510(3) 0.2932(3) 0.0666(14) Uani 1 1 d . . . H24A H 0.6482 0.2877 0.2711 0.100 Uiso 1 1 calc R . . H24B H 0.5196 0.2569 0.2754 0.100 Uiso 1 1 calc R . . H24C H 0.6305 0.2058 0.2762 0.100 Uiso 1 1 calc R . . C25 C 0.6341(5) 0.1295(2) 0.4119(3) 0.0654(14) Uani 1 1 d . . . H25A H 0.7142 0.1261 0.4486 0.078 Uiso 0.50 1 calc PR B 1 H25B H 0.6443 0.1214 0.3585 0.078 Uiso 0.50 1 calc PR B 1 H25C H 0.7082 0.1254 0.4521 0.078 Uiso 0.50 1 d PR B 2 H25D H 0.6545 0.1250 0.3619 0.078 Uiso 0.50 1 d PR B 2 C26A C 0.5445(18) 0.0740(9) 0.4333(7) 0.061(4) Uani 0.58 1 d P C 1 H26A H 0.5773 0.0274 0.4303 0.092 Uiso 0.58 1 calc PR C 1 H26B H 0.4657 0.0777 0.3965 0.092 Uiso 0.58 1 calc PR C 1 H26C H 0.5352 0.0824 0.4862 0.092 Uiso 0.58 1 calc PR C 1 C26B C 0.562(3) 0.0701(14) 0.4012(12) 0.078(7) Uani 0.42 1 d P C 2 H26D H 0.6120 0.0295 0.3977 0.117 Uiso 0.42 1 calc PR C 2 H26E H 0.4991 0.0745 0.3529 0.117 Uiso 0.42 1 calc PR C 2 H26F H 0.5242 0.0647 0.4453 0.117 Uiso 0.42 1 calc PR C 2 N31 N 0.7795(4) 0.6855(2) 0.9254(2) 0.0576(11) Uani 1 1 d . . . H31 H 0.726(5) 0.663(3) 0.879(3) 0.069 Uiso 1 1 d . . . C31A C 0.8869(8) 0.6974(5) 0.9054(5) 0.057(2) Uani 0.58 1 d P D 1 H31A H 0.8833 0.7411 0.8757 0.068 Uiso 0.58 1 calc PR D 1 H31B H 0.9059 0.6590 0.8732 0.068 Uiso 0.58 1 calc PR D 1 C32A C 1.0023(11) 0.7034(7) 0.9988(9) 0.083(4) Uani 0.58 1 d P D 1 H32A H 1.0820 0.7106 0.9881 0.124 Uiso 0.58 1 calc PR D 1 H32B H 1.0027 0.6603 1.0282 0.124 Uiso 0.58 1 calc PR D 1 H32C H 0.9831 0.7423 1.0293 0.124 Uiso 0.58 1 calc PR D 1 C33A C 0.7819(11) 0.6276(5) 0.9891(5) 0.067(3) Uani 0.58 1 d P D 1 H33A H 0.8355 0.6421 1.0391 0.080 Uiso 0.58 1 calc PR D 1 H33B H 0.6997 0.6208 0.9973 0.080 Uiso 0.58 1 calc PR D 1 C34A C 0.8247(9) 0.5644(4) 0.9633(4) 0.062(2) Uani 0.58 1 d P D 1 H34A H 0.8243 0.5280 1.0019 0.094 Uiso 0.58 1 calc PR D 1 H34B H 0.9072 0.5710 0.9570 0.094 Uiso 0.58 1 calc PR D 1 H34C H 0.7721 0.5508 0.9133 0.094 Uiso 0.58 1 calc PR D 1 C35A C 0.7155(8) 0.7507(4) 0.9503(6) 0.063(2) Uani 0.58 1 d P D 1 H35A H 0.6574 0.7353 0.9806 0.075 Uiso 0.58 1 calc PR D 1 H35B H 0.7767 0.7802 0.9845 0.075 Uiso 0.58 1 calc PR D 1 C36A C 0.6531(12) 0.7907(6) 0.8856(7) 0.070(4) Uani 0.58 1 d P D 1 H36A H 0.6169 0.8313 0.9044 0.106 Uiso 0.58 1 calc PR D 1 H36B H 0.5896 0.7625 0.8528 0.106 Uiso 0.58 1 calc PR D 1 H36C H 0.7100 0.8058 0.8551 0.106 Uiso 0.58 1 calc PR D 1 C31B C 0.9355(14) 0.6576(7) 0.9412(8) 0.072(4) Uani 0.42 1 d P D 2 H31C H 0.9537 0.6204 0.9809 0.086 Uiso 0.42 1 calc PR D 2 H31D H 0.9535 0.6406 0.8923 0.086 Uiso 0.42 1 calc PR D 2 C32B C 1.000(2) 0.7166(12) 0.9670(12) 0.090(7) Uiso 0.42 1 d P D 2 H32D H 1.0867 0.7064 0.9775 0.135 Uiso 0.42 1 calc PR D 2 H32E H 0.9799 0.7327 1.0150 0.135 Uiso 0.42 1 calc PR D 2 H32F H 0.9801 0.7526 0.9271 0.135 Uiso 0.42 1 calc PR D 2 C33B C 0.7456(11) 0.6740(9) 0.9881(8) 0.069(4) Uani 0.42 1 d P D 2 H33C H 0.6633 0.6933 0.9814 0.083 Uiso 0.42 1 calc PR D 2 H33D H 0.7992 0.7008 1.0302 0.083 Uiso 0.42 1 calc PR D 2 C34B C 0.7428(12) 0.5986(7) 1.0167(7) 0.065(4) Uani 0.42 1 d P D 2 H34D H 0.7150 0.5980 1.0651 0.098 Uiso 0.42 1 calc PR D 2 H34E H 0.8240 0.5788 1.0260 0.098 Uiso 0.42 1 calc PR D 2 H34F H 0.6875 0.5713 0.9770 0.098 Uiso 0.42 1 calc PR D 2 C35B C 0.7954(12) 0.7577(6) 0.8931(7) 0.064(3) Uani 0.42 1 d P D 2 H35C H 0.8373 0.7875 0.9367 0.076 Uiso 0.42 1 calc PR D 2 H35D H 0.8483 0.7537 0.8562 0.076 Uiso 0.42 1 calc PR D 2 C36B C 0.684(2) 0.7917(14) 0.8538(9) 0.102(9) Uani 0.42 1 d P D 2 H36D H 0.7031 0.8376 0.8361 0.153 Uiso 0.42 1 calc PR D 2 H36E H 0.6314 0.7966 0.8898 0.153 Uiso 0.42 1 calc PR D 2 H36F H 0.6439 0.7639 0.8088 0.153 Uiso 0.42 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0170(3) 0.0301(4) 0.0208(3) -0.0014(3) 0.0034(3) -0.0023(3) Mn2 0.0174(2) 0.0313(3) 0.0202(2) -0.0016(2) 0.00144(18) -0.00128(19) O1 0.0158(10) 0.0310(12) 0.0242(11) -0.0004(9) 0.0026(9) -0.0010(9) O2 0.0210(11) 0.0340(13) 0.0241(11) -0.0023(10) 0.0055(9) -0.0036(9) O3 0.0237(12) 0.0445(14) 0.0255(12) -0.0060(11) 0.0070(9) -0.0077(10) C1 0.0210(15) 0.0316(17) 0.0214(15) 0.0047(13) 0.0022(12) -0.0013(13) C2 0.0197(15) 0.0265(16) 0.0297(16) 0.0038(13) 0.0059(13) 0.0006(13) C3 0.0266(17) 0.0320(18) 0.0316(17) 0.0024(14) 0.0082(14) -0.0032(14) C4 0.0226(17) 0.037(2) 0.044(2) 0.0013(16) 0.0044(15) -0.0061(14) C5 0.0230(17) 0.045(2) 0.048(2) 0.0023(17) 0.0171(16) -0.0048(15) C6 0.0293(18) 0.042(2) 0.0341(18) 0.0008(16) 0.0157(15) -0.0024(15) C7 0.0231(16) 0.0293(17) 0.0310(17) 0.0049(14) 0.0082(13) -0.0020(13) N1 0.0232(14) 0.0379(17) 0.0270(14) -0.0002(12) 0.0103(12) -0.0031(12) N2 0.0280(15) 0.0409(17) 0.0262(14) 0.0023(13) 0.0112(12) 0.0015(13) C8 0.0304(18) 0.039(2) 0.0263(17) 0.0010(15) 0.0112(14) -0.0011(15) C9 0.035(2) 0.053(2) 0.0313(19) -0.0056(17) 0.0106(16) -0.0101(17) N3 0.052(2) 0.079(3) 0.0390(19) -0.0157(18) 0.0234(17) -0.019(2) C10 0.0280(17) 0.0293(17) 0.0246(16) 0.0039(13) 0.0086(13) 0.0053(13) N4 0.0273(14) 0.0339(16) 0.0272(14) -0.0020(12) 0.0097(12) -0.0017(12) N5 0.0212(13) 0.0314(15) 0.0284(14) -0.0029(12) 0.0051(11) -0.0013(11) N6 0.0273(14) 0.0342(16) 0.0247(14) -0.0008(12) 0.0059(11) 0.0021(12) N7 0.0306(15) 0.0408(17) 0.0260(14) 0.0004(13) 0.0086(12) 0.0006(13) O4 0.0287(12) 0.0294(13) 0.0327(12) -0.0047(10) 0.0037(10) -0.0072(10) O5 0.065(2) 0.0360(17) 0.074(2) 0.0058(15) -0.0170(17) -0.0169(15) C11 0.042(2) 0.044(2) 0.0273(18) 0.0041(16) 0.0007(16) -0.0114(18) C12 0.041(2) 0.060(3) 0.0252(18) 0.0067(17) 0.0015(16) -0.0247(19) C13 0.064(3) 0.081(3) 0.036(2) 0.014(2) -0.010(2) -0.044(3) C14 0.063(3) 0.122(5) 0.042(3) 0.020(3) -0.009(2) -0.065(4) C15 0.034(2) 0.144(6) 0.044(3) 0.002(3) -0.003(2) -0.038(3) C16 0.032(2) 0.095(4) 0.037(2) -0.004(2) 0.0002(17) -0.014(2) C17 0.0270(18) 0.072(3) 0.0182(16) -0.0022(17) 0.0026(13) -0.0151(18) N8 0.0234(14) 0.0483(18) 0.0215(13) -0.0002(13) 0.0005(11) -0.0019(13) N9 0.0312(17) 0.056(2) 0.0317(16) -0.0002(15) -0.0060(13) 0.0026(15) C18 0.037(2) 0.055(3) 0.036(2) 0.0027(19) -0.0104(17) 0.0061(19) N10A 0.100(9) 0.065(6) 0.026(6) -0.015(5) -0.025(5) 0.047(6) N10B 0.073(8) 0.089(10) 0.027(6) 0.022(6) -0.019(5) -0.008(7) C20 0.0266(17) 0.040(2) 0.0315(18) 0.0023(16) 0.0030(14) 0.0076(15) N11 0.0189(13) 0.0334(15) 0.0240(13) 0.0010(11) 0.0013(11) 0.0049(11) N12 0.0207(13) 0.0330(15) 0.0276(14) 0.0012(12) 0.0065(11) 0.0021(11) N13 0.0267(15) 0.0342(16) 0.0339(15) 0.0056(13) 0.0057(12) 0.0045(12) N14 0.0313(16) 0.0437(19) 0.0349(16) 0.0078(14) 0.0001(13) 0.0093(14) N21 0.0431(19) 0.0416(19) 0.0417(18) 0.0012(15) 0.0065(15) -0.0011(15) C21 0.053(3) 0.091(4) 0.046(3) -0.004(3) 0.012(2) -0.006(3) C22 0.066(3) 0.084(4) 0.063(3) -0.015(3) 0.002(3) 0.008(3) C23 0.042(2) 0.050(3) 0.069(3) 0.000(2) 0.019(2) 0.003(2) C24 0.079(4) 0.070(3) 0.063(3) 0.019(3) 0.040(3) 0.029(3) C25 0.085(4) 0.045(3) 0.056(3) 0.002(2) -0.003(3) 0.009(3) C26A 0.072(8) 0.045(7) 0.055(8) 0.018(7) -0.009(7) -0.007(5) C26B 0.082(13) 0.055(9) 0.084(16) -0.007(13) -0.005(13) -0.002(8) N31 0.084(3) 0.042(2) 0.038(2) -0.0042(17) -0.002(2) -0.002(2) C31A 0.062(5) 0.053(5) 0.058(5) -0.013(4) 0.021(4) 0.004(4) C32A 0.069(7) 0.081(8) 0.108(11) -0.021(8) 0.039(7) -0.047(6) C33A 0.112(9) 0.057(6) 0.027(4) 0.008(4) 0.006(5) 0.012(6) C34A 0.086(6) 0.060(5) 0.032(4) 0.007(4) -0.006(4) -0.001(5) C35A 0.056(5) 0.044(4) 0.095(7) -0.011(4) 0.031(5) 0.003(4) C36A 0.072(7) 0.041(5) 0.074(8) -0.002(6) -0.032(7) 0.003(5) C31B 0.118(12) 0.039(7) 0.066(8) -0.004(6) 0.038(8) -0.002(7) C33B 0.044(7) 0.097(11) 0.064(8) 0.035(8) 0.010(6) 0.006(7) C34B 0.073(8) 0.081(9) 0.038(6) 0.029(6) 0.006(5) -0.024(7) C35B 0.079(8) 0.063(7) 0.040(6) 0.002(5) -0.005(6) -0.017(6) C36B 0.15(2) 0.112(15) 0.034(8) 0.024(9) -0.009(9) -0.012(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.115(2) 3_666 ? Mn1 O1 2.115(2) . ? Mn1 O2 2.242(2) . ? Mn1 O2 2.242(2) 3_666 ? Mn1 N12 2.276(3) 3_666 ? Mn1 N12 2.276(3) . ? Mn2 O1 1.895(2) . ? Mn2 O4 1.914(2) . ? Mn2 N8 1.983(3) . ? Mn2 N11 1.998(3) . ? Mn2 O3 2.117(2) . ? Mn2 N5 2.350(3) 3_666 ? O1 H1 0.75(4) . ? O2 C1 1.255(4) . ? O3 C1 1.263(4) . ? C1 C2 1.507(4) . ? C2 C3 1.397(5) . ? C2 C7 1.409(5) . ? C3 C4 1.386(5) . ? C3 H3A 0.9500 . ? C4 C5 1.388(5) . ? C4 H4A 0.9500 . ? C5 C6 1.369(5) . ? C5 H5A 0.9500 . ? C6 C7 1.407(4) . ? C6 H6A 0.9500 . ? C7 N1 1.409(4) . ? N1 N2 1.325(4) . ? N1 H11 0.81(4) . ? N2 C8 1.303(4) . ? C8 C9 1.444(5) . ? C8 C10 1.466(5) . ? C9 N3 1.145(5) . ? C10 N4 1.329(4) . ? C10 N7 1.337(4) . ? N4 N5 1.352(4) . ? N5 N6 1.318(4) . ? N5 Mn2 2.350(3) 3_666 ? N6 N7 1.345(4) . ? O4 C11 1.288(4) . ? O5 C11 1.240(5) . ? C11 C12 1.491(6) . ? C12 C17 1.400(6) . ? C12 C13 1.403(5) . ? C13 C14 1.363(7) . ? C13 H13A 0.9500 . ? C14 C15 1.373(9) . ? C14 H14A 0.9500 . ? C15 C16 1.387(7) . ? C15 H15A 0.9500 . ? C16 C17 1.404(5) . ? C16 H16A 0.9500 . ? C17 N8 1.428(5) . ? N8 N9 1.333(4) . ? N9 C18 1.308(5) . ? C18 C19A 1.439(11) . ? C18 C20 1.451(5) . ? C18 C19B 1.514(11) . ? C19A N10A 1.124(15) . ? C19B N10B 1.128(15) . ? C20 N11 1.328(4) . ? C20 N14 1.334(5) . ? N11 N12 1.344(4) . ? N12 N13 1.318(4) . ? N13 N14 1.350(4) . ? N21 C25 1.482(6) . ? N21 C23 1.514(5) . ? N21 C21 1.519(6) . ? N21 H21 1.01(4) . ? C21 C22 1.480(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.500(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26B 1.40(3) . ? C25 C26A 1.587(19) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 H25C 0.9701 . ? C25 H25D 0.9700 . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? N31 C33B 1.275(13) . ? N31 C31A 1.370(9) . ? N31 C35B 1.533(12) . ? N31 C35A 1.568(9) . ? N31 C33A 1.583(10) . ? N31 C31B 1.817(16) . ? N31 H31 0.99(5) . ? C31A C32A 1.857(17) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C33A C34A 1.429(13) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C35A C36A 1.424(14) . ? C35A H35A 0.9900 . ? C35A H35B 0.9900 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C31B C32B 1.38(2) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C33B C34B 1.544(18) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? C35B C36B 1.45(3) . ? C35B H35C 0.9900 . ? C35B H35D 0.9900 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 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 O1 179.998(1) 3_666 . ? O1 Mn1 O2 83.17(8) 3_666 . ? O1 Mn1 O2 96.83(8) . . ? O1 Mn1 O2 96.83(8) 3_666 3_666 ? O1 Mn1 O2 83.17(8) . 3_666 ? O2 Mn1 O2 180.0 . 3_666 ? O1 Mn1 N12 83.70(9) 3_666 3_666 ? O1 Mn1 N12 96.30(9) . 3_666 ? O2 Mn1 N12 89.37(9) . 3_666 ? O2 Mn1 N12 90.63(9) 3_666 3_666 ? O1 Mn1 N12 96.30(9) 3_666 . ? O1 Mn1 N12 83.70(9) . . ? O2 Mn1 N12 90.63(9) . . ? O2 Mn1 N12 89.37(9) 3_666 . ? N12 Mn1 N12 179.998(1) 3_666 . ? O1 Mn2 O4 91.58(10) . . ? O1 Mn2 N8 175.75(11) . . ? O4 Mn2 N8 90.52(12) . . ? O1 Mn2 N11 90.36(10) . . ? O4 Mn2 N11 171.83(11) . . ? N8 Mn2 N11 87.05(12) . . ? O1 Mn2 O3 90.74(9) . . ? O4 Mn2 O3 95.00(10) . . ? N8 Mn2 O3 92.76(10) . . ? N11 Mn2 O3 92.91(10) . . ? O1 Mn2 N5 85.21(10) . 3_666 ? O4 Mn2 N5 89.00(10) . 3_666 ? N8 Mn2 N5 91.13(10) . 3_666 ? N11 Mn2 N5 83.26(10) . 3_666 ? O3 Mn2 N5 174.39(9) . 3_666 ? Mn2 O1 Mn1 113.34(11) . . ? Mn2 O1 H1 115(3) . . ? Mn1 O1 H1 109(3) . . ? C1 O2 Mn1 125.6(2) . . ? C1 O3 Mn2 135.7(2) . . ? O2 C1 O3 124.9(3) . . ? O2 C1 C2 120.1(3) . . ? O3 C1 C2 115.0(3) . . ? C3 C2 C7 118.4(3) . . ? C3 C2 C1 116.9(3) . . ? C7 C2 C1 124.7(3) . . ? C4 C3 C2 122.2(3) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? C3 C4 C5 118.4(3) . . ? C3 C4 H4A 120.8 . . ? C5 C4 H4A 120.8 . . ? C6 C5 C4 121.2(3) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 120.7(3) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C6 C7 C2 119.1(3) . . ? C6 C7 N1 119.5(3) . . ? C2 C7 N1 121.4(3) . . ? N2 N1 C7 117.2(3) . . ? N2 N1 H11 121(3) . . ? C7 N1 H11 122(3) . . ? C8 N2 N1 122.7(3) . . ? N2 C8 C9 113.7(3) . . ? N2 C8 C10 129.6(3) . . ? C9 C8 C10 116.7(3) . . ? N3 C9 C8 178.3(5) . . ? N4 C10 N7 112.8(3) . . ? N4 C10 C8 123.8(3) . . ? N7 C10 C8 123.4(3) . . ? C10 N4 N5 103.7(3) . . ? N6 N5 N4 110.0(3) . . ? N6 N5 Mn2 134.3(2) . 3_666 ? N4 N5 Mn2 115.60(19) . 3_666 ? N5 N6 N7 109.2(3) . . ? C10 N7 N6 104.3(3) . . ? C11 O4 Mn2 132.6(2) . . ? O5 C11 O4 119.7(4) . . ? O5 C11 C12 120.6(4) . . ? O4 C11 C12 119.7(4) . . ? C17 C12 C13 119.2(4) . . ? C17 C12 C11 124.1(3) . . ? C13 C12 C11 116.7(4) . . ? C14 C13 C12 121.6(5) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C15 119.4(5) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C14 C15 C16 121.2(5) . . ? C14 C15 H15A 119.4 . . ? C16 C15 H15A 119.4 . . ? C15 C16 C17 119.9(5) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C12 C17 C16 118.8(4) . . ? C12 C17 N8 123.1(3) . . ? C16 C17 N8 118.1(4) . . ? N9 N8 C17 111.1(3) . . ? N9 N8 Mn2 128.9(2) . . ? C17 N8 Mn2 120.0(2) . . ? C18 N9 N8 122.6(3) . . ? N9 C18 C19A 114.5(5) . . ? N9 C18 C20 127.2(4) . . ? C19A C18 C20 116.5(5) . . ? N9 C18 C19B 116.7(5) . . ? C19A C18 C19B 19.5(5) . . ? C20 C18 C19B 115.9(5) . . ? N10A C19A C18 171.4(14) . . ? N10B C19B C18 171.7(12) . . ? N11 C20 N14 111.4(3) . . ? N11 C20 C18 121.6(3) . . ? N14 C20 C18 126.8(3) . . ? C20 N11 N12 105.7(3) . . ? C20 N11 Mn2 126.2(2) . . ? N12 N11 Mn2 126.2(2) . . ? N13 N12 N11 108.7(3) . . ? N13 N12 Mn1 142.1(2) . . ? N11 N12 Mn1 109.21(19) . . ? N12 N13 N14 109.5(3) . . ? C20 N14 N13 104.7(3) . . ? C25 N21 C23 112.6(4) . . ? C25 N21 C21 114.9(4) . . ? C23 N21 C21 109.7(4) . . ? C25 N21 H21 93(3) . . ? C23 N21 H21 108(2) . . ? C21 N21 H21 118(2) . . ? C22 C21 N21 115.6(4) . . ? C22 C21 H21A 108.4 . . ? N21 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? N21 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 N21 111.4(4) . . ? C24 C23 H23A 109.3 . . ? N21 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? N21 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26B C25 N21 121.2(12) . . ? C26B C25 C26A 24.0(10) . . ? N21 C25 C26A 107.8(8) . . ? C26B C25 H25A 117.1 . . ? N21 C25 H25A 110.1 . . ? C26A C25 H25A 110.1 . . ? C26B C25 H25B 86.3 . . ? N21 C25 H25B 110.1 . . ? C26A C25 H25B 110.1 . . ? H25A C25 H25B 108.5 . . ? C26B C25 H25C 114.5 . . ? N21 C25 H25C 108.9 . . ? C26A C25 H25C 105.6 . . ? H25A C25 H25C 5.9 . . ? H25B C25 H25C 114.0 . . ? C26B C25 H25D 93.5 . . ? N21 C25 H25D 109.1 . . ? C26A C25 H25D 117.4 . . ? H25A C25 H25D 102.1 . . ? H25B C25 H25D 7.9 . . ? H25C C25 H25D 107.8 . . ? C25 C26A H26A 109.5 . . ? C25 C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C25 C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C25 C26B H26D 109.5 . . ? C25 C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C25 C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C33B N31 C31A 136.4(8) . . ? C33B N31 C35B 124.6(10) . . ? C31A N31 C35B 64.0(7) . . ? C33B N31 C35A 68.9(9) . . ? C31A N31 C35A 116.1(6) . . ? C35B N31 C35A 58.5(6) . . ? C33B N31 C33A 38.5(8) . . ? C31A N31 C33A 115.7(7) . . ? C35B N31 C33A 157.5(6) . . ? C35A N31 C33A 107.4(6) . . ? C33B N31 C31B 107.4(8) . . ? C31A N31 C31B 35.7(5) . . ? C35B N31 C31B 97.5(7) . . ? C35A N31 C31B 134.3(6) . . ? C33A N31 C31B 80.0(6) . . ? C33B N31 H31 113(3) . . ? C31A N31 H31 106(3) . . ? C35B N31 H31 101(3) . . ? C35A N31 H31 110(3) . . ? C33A N31 H31 101(3) . . ? C31B N31 H31 113(3) . . ? N31 C31A C32A 105.8(7) . . ? N31 C31A H31A 110.6 . . ? C32A C31A H31A 110.6 . . ? N31 C31A H31B 110.6 . . ? C32A C31A H31B 110.6 . . ? H31A C31A H31B 108.7 . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C34A C33A N31 109.1(7) . . ? C34A C33A H33A 109.9 . . ? N31 C33A H33A 109.9 . . ? C34A C33A H33B 109.9 . . ? N31 C33A H33B 109.9 . . ? H33A C33A H33B 108.3 . . ? C33A C34A H34A 109.5 . . ? C33A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C33A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C36A C35A N31 112.8(8) . . ? C36A C35A H35A 109.0 . . ? N31 C35A H35A 109.0 . . ? C36A C35A H35B 109.0 . . ? N31 C35A H35B 109.0 . . ? H35A C35A H35B 107.8 . . ? C35A C36A H36A 109.5 . . ? C35A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C35A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C32B C31B N31 103.5(13) . . ? C32B C31B H31C 111.1 . . ? N31 C31B H31C 111.1 . . ? C32B C31B H31D 111.1 . . ? N31 C31B H31D 111.1 . . ? H31C C31B H31D 109.0 . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? N31 C33B C34B 118.8(14) . . ? N31 C33B H33C 107.6 . . ? C34B C33B H33C 107.6 . . ? N31 C33B H33D 107.6 . . ? C34B C33B H33D 107.6 . . ? H33C C33B H33D 107.0 . . ? C33B C34B H34D 109.5 . . ? C33B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C33B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C36B C35B N31 115.1(13) . . ? C36B C35B H35C 108.5 . . ? N31 C35B H35C 108.5 . . ? C36B C35B H35D 108.5 . . ? N31 C35B H35D 108.5 . . ? H35C C35B H35D 107.5 . . ? C35B C36B H36D 109.5 . . ? C35B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C35B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 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 O1 H1 N4 0.75(4) 2.36(4) 2.901(4) 130(4) 3_666 N1 H11 O2 0.81(4) 2.21(4) 2.783(3) 128(3) . N1 H11 N4 0.81(4) 2.28(4) 2.878(4) 131(4) . N21 H21 O5 1.01(4) 1.91(5) 2.849(5) 152(4) . N31 H31 N6 0.99(5) 2.10(5) 3.045(5) 159(4) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.526 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.071 ####################################################### data_dhb19s _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C341 H387 Mn14 N150 O57' _chemical_formula_weight 8268.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3 c' _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 33.681(2) _cell_length_b 33.681(2) _cell_length_c 52.778(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 51850(6) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13982 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 26.01 _exptl_crystal_description rhombohedron _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 25734 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 0.745 _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 76533 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 64 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.10 _reflns_number_total 11401 _reflns_number_gt 5584 _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.005 -0.007 -0.001 30212.4 12839.0 _platon_squeeze_details ; P. van der Sluis & A.L. Spek, Acta Cryst. 1990, A46, 194 ; _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^)+(0.0814P)^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 11401 _refine_ls_number_parameters 407 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.6667 0.3333 0.156370(16) 0.0394(2) Uani 1 3 d S . . Mn2 Mn 0.564667(17) 0.304775(19) 0.170125(11) 0.05306(18) Uani 1 1 d . . . Mn3 Mn 0.570341(15) 0.287704(17) 0.107655(10) 0.04304(15) Uani 1 1 d . . . O1 O 0.60889(7) 0.32913(7) 0.13909(4) 0.0466(6) Uani 1 1 d . . . H1 H 0.6157 0.3611 0.1357 0.056 Uiso 1 1 calc R . . C99 C 0.6667 0.3333 0.0833 0.0419(18) Uani 1 6 d S . . O2 O 0.62855(8) 0.3333 0.0833 0.0368(7) Uani 1 2 d S . . O3 O 0.61139(7) 0.28228(8) 0.18179(4) 0.0500(6) Uani 1 1 d . . . O4 O 0.63938(9) 0.24098(8) 0.19757(5) 0.0603(7) Uani 1 1 d . . . C1 C 0.60990(12) 0.25253(13) 0.19746(7) 0.0516(9) Uani 1 1 d . . . C2 C 0.57250(14) 0.23226(14) 0.21624(8) 0.0668(11) Uani 1 1 d . . . C3 C 0.58276(18) 0.21664(18) 0.23850(9) 0.0972(17) Uani 1 1 d . . . H3A H 0.6123 0.2200 0.2406 0.117 Uiso 1 1 calc R A . C4 C 0.55038(19) 0.1965(2) 0.25735(10) 0.111(2) Uani 1 1 d . . . H4A H 0.5575 0.1859 0.2724 0.133 Uiso 1 1 calc R . . C5 C 0.50797(19) 0.1918(2) 0.25426(11) 0.134(3) Uani 1 1 d . . . H5A H 0.4856 0.1776 0.2672 0.160 Uiso 1 1 calc R A . C6 C 0.49738(16) 0.2069(2) 0.23334(10) 0.120(2) Uani 1 1 d . . . H6A H 0.4677 0.2034 0.2318 0.145 Uiso 1 1 calc R . . C7 C 0.52854(14) 0.22745(15) 0.21405(8) 0.0713(12) Uani 1 1 d . . . N2 N 0.51652(10) 0.24070(12) 0.19068(6) 0.0669(9) Uani 1 1 d . . . N3 N 0.47249(11) 0.21943(12) 0.18729(6) 0.0753(10) Uani 1 1 d . . . C8 C 0.45527(12) 0.22386(16) 0.16496(8) 0.0722(12) Uani 1 1 d . . . C9 C 0.47834(12) 0.24063(13) 0.14150(8) 0.0616(10) Uani 1 1 d . . . O5 O 0.52158(7) 0.25701(8) 0.14027(4) 0.0531(6) Uani 1 1 d . . . C10 C 0.40711(14) 0.20489(19) 0.16510(8) 0.0864(15) Uani 1 1 d . . . N5 N 0.38346(15) 0.18837(19) 0.18589(9) 0.1158(17) Uani 1 1 d D . . H5 H 0.3978(19) 0.190(2) 0.1999(8) 0.139 Uiso 1 1 d D . . N12 N 0.45460(9) 0.23498(12) 0.12014(6) 0.0655(10) Uani 1 1 d . . . N6 N 0.38487(12) 0.20323(14) 0.14367(7) 0.0902(13) Uani 1 1 d . . . H6 H 0.3552 0.1930 0.1436 0.108 Uiso 1 1 calc R . . C11 C 0.40940(13) 0.21770(16) 0.12252(8) 0.0736(13) Uani 1 1 d . . . C12 C 0.38486(14) 0.21471(19) 0.09961(10) 0.0904(16) Uani 1 1 d . . . C13 C 0.34048(14) 0.2091(2) 0.10165(9) 0.105(2) Uani 1 1 d . . . N4 N 0.30322(14) 0.2022(2) 0.10194(9) 0.147(2) Uani 1 1 d . . . N7 N 0.39765(10) 0.21628(14) 0.07580(7) 0.0821(12) Uani 1 1 d . . . N8 N 0.43767(10) 0.22202(12) 0.07065(7) 0.0728(10) Uani 1 1 d . . . H8 H 0.4581 0.2286 0.0827 0.087 Uiso 1 1 calc R . . C14 C 0.44774(13) 0.21762(16) 0.04555(9) 0.0785(14) Uani 1 1 d . . . C15 C 0.41501(14) 0.20576(19) 0.02680(10) 0.0964(17) Uani 1 1 d . . . H15A H 0.3854 0.2007 0.0311 0.116 Uiso 1 1 calc R . . C16 C 0.42428(18) 0.2015(2) 0.00323(11) 0.123(2) Uani 1 1 d . . . H16A H 0.4011 0.1934 -0.0092 0.147 Uiso 1 1 calc R A . C17 C 0.46705(16) 0.2083(2) -0.00427(9) 0.108(2) Uani 1 1 d . . . H17A H 0.4729 0.2048 -0.0215 0.129 Uiso 1 1 calc R . . C18 C 0.50063(14) 0.22031(16) 0.01403(8) 0.0772(13) Uani 1 1 d . . . H18A H 0.5299 0.2250 0.0094 0.093 Uiso 1 1 calc R A . C19 C 0.49174(12) 0.22545(14) 0.03871(8) 0.0638(11) Uani 1 1 d . . . C20 C 0.52980(12) 0.24044(11) 0.05740(7) 0.0488(9) Uani 1 1 d . . . O9 O 0.52182(7) 0.24121(8) 0.08066(5) 0.0509(6) Uani 1 1 d . . . O10 O 0.56865(7) 0.25286(8) 0.04862(4) 0.0490(6) Uani 1 1 d . . . O11 O 0.53864(8) 0.33078(8) 0.10424(5) 0.0537(6) Uani 1 1 d . A . C21 C 0.52283(13) 0.3333 0.0833 0.0482(12) Uani 1 2 d S . . C22 C 0.4754(2) 0.3300(4) 0.08149(17) 0.0677(19) Uiso 0.50 1 d PG A -1 C23 C 0.4575(2) 0.3266(3) 0.05734(14) 0.074(3) Uiso 0.50 1 d PG A -1 H23A H 0.4734 0.3244 0.0430 0.088 Uiso 0.50 1 calc PR A -1 C24 C 0.4165(3) 0.3265(3) 0.05417(11) 0.099(3) Uiso 0.50 1 d PG A -1 H24A H 0.4043 0.3243 0.0377 0.119 Uiso 0.50 1 calc PR A -1 C25 C 0.3933(3) 0.3298(5) 0.07516(14) 0.155(6) Uiso 0.50 1 d PG A -1 H25A H 0.3653 0.3297 0.0730 0.186 Uiso 0.50 1 calc PR A -1 C26 C 0.4112(3) 0.3331(4) 0.09931(12) 0.091(3) Uiso 0.50 1 d PG A -1 H26A H 0.3954 0.3353 0.1137 0.109 Uiso 0.50 1 calc PR A -1 C27 C 0.4522(2) 0.3332(3) 0.10248(13) 0.072(3) Uiso 0.50 1 d PG A -1 N9 N 0.4716(3) 0.3410(3) 0.12540(14) 0.076(2) Uiso 0.50 1 d P A -1 H9 H 0.4953 0.3373 0.1280 0.091 Uiso 0.50 1 calc PR A -1 N10 N 0.4548(4) 0.3542(4) 0.1440(2) 0.126(3) Uiso 0.50 1 d P A -1 C28 C 0.4654(5) 0.3523(5) 0.1690(3) 0.123(4) Uiso 0.50 1 d PD A -1 C29 C 0.5039(4) 0.3529(4) 0.1786(2) 0.085(3) Uiso 0.50 1 d P A -1 O12 O 0.52345(15) 0.33617(15) 0.16006(9) 0.0434(11) Uiso 0.50 1 d P A -1 O13 O 0.5163(4) 0.3650(4) 0.2027(2) 0.166(4) Uiso 0.50 1 d P A -1 C30A C 0.4351(11) 0.3563(11) 0.1877(5) 0.144(8) Uiso 0.25 1 d PD A -1 N11A N 0.4149(10) 0.3695(11) 0.2004(5) 0.172(10) Uiso 0.25 1 d PD A -1 C30B C 0.4504(11) 0.3811(11) 0.1836(6) 0.144(8) Uiso 0.25 1 d PD A -1 N11B N 0.4433(13) 0.4090(12) 0.1944(6) 0.219(14) Uiso 0.25 1 d PD A -1 O14 O 0.5168(3) 0.3303(3) 0.17543(17) 0.117(3) Uiso 0.50 1 d P A -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0310(3) 0.0310(3) 0.0561(5) 0.000 0.000 0.01550(14) Mn2 0.0347(3) 0.0544(4) 0.0688(4) 0.0091(3) 0.0051(3) 0.0213(3) Mn3 0.0271(3) 0.0420(3) 0.0571(3) 0.0074(2) 0.0021(2) 0.0150(2) O1 0.0337(12) 0.0389(13) 0.0651(16) 0.0029(11) -0.0028(11) 0.0165(10) C99 0.042(3) 0.042(3) 0.041(5) 0.000 0.000 0.0211(14) O2 0.0248(11) 0.0378(17) 0.0521(19) 0.0061(14) 0.0031(7) 0.0189(8) O3 0.0384(13) 0.0449(14) 0.0684(16) 0.0154(12) 0.0044(11) 0.0219(11) O4 0.0685(18) 0.0468(15) 0.0670(18) 0.0045(12) -0.0132(14) 0.0299(14) C1 0.040(2) 0.044(2) 0.051(2) -0.0017(18) -0.0027(17) 0.0064(18) C2 0.066(3) 0.072(3) 0.061(3) 0.017(2) 0.004(2) 0.033(2) C3 0.083(4) 0.118(4) 0.091(4) 0.046(3) 0.010(3) 0.050(3) C4 0.091(4) 0.156(5) 0.080(4) 0.060(4) 0.019(3) 0.057(4) C5 0.071(4) 0.211(7) 0.107(5) 0.085(5) 0.027(3) 0.062(4) C6 0.047(3) 0.196(6) 0.088(4) 0.051(4) 0.011(3) 0.038(4) C7 0.049(2) 0.086(3) 0.056(3) 0.005(2) -0.007(2) 0.017(2) N2 0.0376(18) 0.078(2) 0.076(2) 0.0143(18) 0.0023(16) 0.0221(17) N3 0.0409(19) 0.086(3) 0.070(2) 0.0174(19) 0.0070(17) 0.0102(18) C8 0.032(2) 0.102(3) 0.062(3) 0.010(2) -0.0005(18) 0.018(2) C9 0.038(2) 0.056(2) 0.074(3) 0.014(2) 0.0118(19) 0.0105(19) O5 0.0290(12) 0.0574(15) 0.0571(15) 0.0136(12) 0.0050(10) 0.0098(12) C10 0.044(2) 0.139(5) 0.054(3) 0.010(3) 0.010(2) 0.029(3) N5 0.064(3) 0.163(5) 0.085(3) 0.017(3) 0.004(2) 0.031(3) N12 0.0278(15) 0.095(3) 0.061(2) 0.0159(18) 0.0013(14) 0.0208(17) N6 0.0380(19) 0.129(4) 0.083(3) 0.016(2) 0.0027(19) 0.027(2) C11 0.038(2) 0.098(3) 0.068(3) 0.021(2) 0.010(2) 0.021(2) C12 0.035(2) 0.136(5) 0.081(4) 0.029(3) 0.008(2) 0.028(3) C13 0.035(2) 0.174(6) 0.082(3) 0.037(3) 0.013(2) 0.034(3) N4 0.057(3) 0.268(7) 0.116(4) 0.062(4) 0.024(2) 0.081(4) N7 0.0290(18) 0.118(3) 0.085(3) 0.020(2) 0.0044(17) 0.0263(19) N8 0.0259(16) 0.101(3) 0.077(2) 0.027(2) 0.0059(15) 0.0209(18) C14 0.035(2) 0.099(4) 0.078(3) 0.016(3) -0.003(2) 0.015(2) C15 0.042(2) 0.143(5) 0.076(3) 0.012(3) -0.014(2) 0.024(3) C16 0.070(4) 0.209(7) 0.080(4) -0.036(4) -0.031(3) 0.063(4) C17 0.061(3) 0.178(6) 0.059(3) -0.008(3) -0.019(2) 0.041(4) C18 0.049(2) 0.094(3) 0.070(3) -0.006(3) -0.013(2) 0.022(2) C19 0.034(2) 0.078(3) 0.060(3) 0.007(2) -0.0041(18) 0.014(2) C20 0.045(2) 0.0324(19) 0.057(3) 0.0100(17) 0.0001(18) 0.0105(17) O9 0.0330(13) 0.0465(14) 0.0557(16) 0.0089(12) -0.0074(11) 0.0067(11) O10 0.0278(12) 0.0477(14) 0.0649(16) 0.0045(12) -0.0011(11) 0.0140(11) O11 0.0438(14) 0.0641(16) 0.0623(16) 0.0099(13) 0.0019(12) 0.0338(13) C21 0.0344(18) 0.072(4) 0.051(3) 0.009(3) 0.0047(13) 0.0358(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.089(2) 3_665 ? Mn1 O1 2.089(2) 2_655 ? Mn1 O1 2.089(2) . ? Mn1 O3 2.241(2) 3_665 ? Mn1 O3 2.241(2) . ? Mn1 O3 2.241(2) 2_655 ? Mn1 Mn2 3.1543(6) 2_655 ? Mn1 Mn2 3.1544(6) 3_665 ? Mn1 Mn2 3.1544(6) . ? Mn2 O1 2.086(2) . ? Mn2 O3 2.150(2) . ? Mn2 O12 2.190(4) . ? Mn2 O14 2.192(9) . ? Mn2 O5 2.201(2) . ? Mn2 O4 2.201(3) 3_665 ? Mn2 N2 2.228(3) . ? Mn3 O1 2.139(2) . ? Mn3 O9 2.143(2) . ? Mn3 O10 2.155(2) 16_544 ? Mn3 O11 2.197(2) . ? Mn3 O2 2.2000(15) . ? Mn3 O5 2.243(2) . ? O1 H1 1.0000 . ? C99 O2 1.284(3) 3_665 ? C99 O2 1.284(3) . ? C99 O2 1.284(3) 2_655 ? O2 Mn3 2.1999(15) 17_554 ? O3 C1 1.281(4) . ? O4 C1 1.234(4) . ? O4 Mn2 2.201(3) 2_655 ? C1 C2 1.475(5) . ? C2 C3 1.399(6) . ? C2 C7 1.411(6) . ? C3 C4 1.378(6) . ? C3 H3A 0.9500 . ? C4 C5 1.367(7) . ? C4 H4A 0.9500 . ? C5 C6 1.336(7) . ? C5 H5A 0.9500 . ? C6 C7 1.375(6) . ? C6 H6A 0.9500 . ? C7 N2 1.437(5) . ? N2 N3 1.297(4) . ? N3 C8 1.354(5) . ? C8 C10 1.415(5) . ? C8 C9 1.420(5) . ? C9 O5 1.275(4) . ? C9 N12 1.340(5) . ? C10 N5 1.306(6) . ? C10 N6 1.342(5) . ? N5 H5 0.87(3) . ? N12 C11 1.336(4) . ? N6 C11 1.328(5) . ? N6 H6 0.8800 . ? C11 C12 1.439(6) . ? C12 N7 1.321(6) . ? C12 C13 1.414(6) . ? C13 N4 1.157(5) . ? N7 N8 1.292(4) . ? N8 C14 1.394(6) . ? N8 H8 0.8800 . ? C14 C15 1.383(6) . ? C14 C19 1.416(5) . ? C15 C16 1.308(7) . ? C15 H15A 0.9500 . ? C16 C17 1.398(7) . ? C16 H16A 0.9500 . ? C17 C18 1.385(5) . ? C17 H17A 0.9500 . ? C18 C19 1.367(5) . ? C18 H18A 0.9500 . ? C19 C20 1.491(5) . ? C20 O10 1.247(4) . ? C20 O9 1.260(4) . ? O10 Mn3 2.154(2) 16_544 ? O11 C21 1.247(3) . ? C21 O11 1.247(3) 17_554 ? C21 C22 1.547(6) 17_554 ? C21 C22 1.547(6) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C23 H23A 0.9500 . ? C24 C25 1.3900 . ? C24 H24A 0.9500 . ? C25 C26 1.3900 . ? C25 H25A 0.9500 . ? C26 C27 1.3900 . ? C26 H26A 0.9500 . ? C27 N9 1.337(10) . ? N9 N10 1.317(11) . ? N9 H9 0.8800 . ? N10 C28 1.378(14) . ? C28 C29 1.383(15) . ? C28 C30A 1.47(2) . ? C28 C30B 1.51(2) . ? C29 O13 1.336(12) . ? C29 O12 1.442(12) . ? C30A C30B 0.76(5) . ? C30A N11A 1.19(2) . ? C30A N11B 1.69(4) . ? N11A N11B 1.23(4) . ? N11A C30B 1.38(3) . ? C30B N11B 1.22(2) . ? 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 O1 102.37(8) 3_665 2_655 ? O1 Mn1 O1 102.37(8) 3_665 . ? O1 Mn1 O1 102.37(8) 2_655 . ? O1 Mn1 O3 79.68(8) 3_665 3_665 ? O1 Mn1 O3 167.29(9) 2_655 3_665 ? O1 Mn1 O3 89.29(8) . 3_665 ? O1 Mn1 O3 167.30(9) 3_665 . ? O1 Mn1 O3 89.29(8) 2_655 . ? O1 Mn1 O3 79.68(8) . . ? O3 Mn1 O3 87.84(9) 3_665 . ? O1 Mn1 O3 89.29(9) 3_665 2_655 ? O1 Mn1 O3 79.67(8) 2_655 2_655 ? O1 Mn1 O3 167.30(9) . 2_655 ? O3 Mn1 O3 87.85(9) 3_665 2_655 ? O3 Mn1 O3 87.84(9) . 2_655 ? O1 Mn1 Mn2 111.78(6) 3_665 2_655 ? O1 Mn1 Mn2 40.89(6) 2_655 2_655 ? O1 Mn1 Mn2 133.34(6) . 2_655 ? O3 Mn1 Mn2 126.59(7) 3_665 2_655 ? O3 Mn1 Mn2 73.89(6) . 2_655 ? O3 Mn1 Mn2 42.93(6) 2_655 2_655 ? O1 Mn1 Mn2 40.90(6) 3_665 3_665 ? O1 Mn1 Mn2 133.34(6) 2_655 3_665 ? O1 Mn1 Mn2 111.78(6) . 3_665 ? O3 Mn1 Mn2 42.94(6) 3_665 3_665 ? O3 Mn1 Mn2 126.59(7) . 3_665 ? O3 Mn1 Mn2 73.89(6) 2_655 3_665 ? Mn2 Mn1 Mn2 114.865(14) 2_655 3_665 ? O1 Mn1 Mn2 133.34(6) 3_665 . ? O1 Mn1 Mn2 111.78(6) 2_655 . ? O1 Mn1 Mn2 40.89(6) . . ? O3 Mn1 Mn2 73.89(6) 3_665 . ? O3 Mn1 Mn2 42.94(6) . . ? O3 Mn1 Mn2 126.60(7) 2_655 . ? Mn2 Mn1 Mn2 114.866(14) 2_655 . ? Mn2 Mn1 Mn2 114.871(14) 3_665 . ? O1 Mn2 O3 81.88(9) . . ? O1 Mn2 O12 96.90(14) . . ? O3 Mn2 O12 172.81(14) . . ? O1 Mn2 O14 117.8(2) . . ? O3 Mn2 O14 156.0(2) . . ? O12 Mn2 O14 22.1(2) . . ? O1 Mn2 O5 78.78(8) . . ? O3 Mn2 O5 106.19(9) . . ? O12 Mn2 O5 80.43(14) . . ? O14 Mn2 O5 91.9(2) . . ? O1 Mn2 O4 101.15(9) . 3_665 ? O3 Mn2 O4 84.96(9) . 3_665 ? O12 Mn2 O4 88.33(14) . 3_665 ? O14 Mn2 O4 78.1(2) . 3_665 ? O5 Mn2 O4 168.64(9) . 3_665 ? O1 Mn2 N2 142.55(11) . . ? O3 Mn2 N2 79.97(10) . . ? O12 Mn2 N2 104.81(15) . . ? O14 Mn2 N2 89.7(2) . . ? O5 Mn2 N2 75.28(11) . . ? O4 Mn2 N2 109.52(11) 3_665 . ? O1 Mn2 Mn1 40.96(6) . . ? O3 Mn2 Mn1 45.24(6) . . ? O12 Mn2 Mn1 130.82(13) . . ? O14 Mn2 Mn1 144.4(2) . . ? O5 Mn2 Mn1 106.12(6) . . ? O4 Mn2 Mn1 80.03(7) 3_665 . ? N2 Mn2 Mn1 124.17(9) . . ? O1 Mn3 O9 169.98(9) . . ? O1 Mn3 O10 91.06(8) . 16_544 ? O9 Mn3 O10 88.94(9) . 16_544 ? O1 Mn3 O11 88.27(9) . . ? O9 Mn3 O11 89.04(9) . . ? O10 Mn3 O11 164.38(9) 16_544 . ? O1 Mn3 O2 87.64(6) . . ? O9 Mn3 O2 102.13(7) . . ? O10 Mn3 O2 102.79(8) 16_544 . ? O11 Mn3 O2 92.77(8) . . ? O1 Mn3 O5 76.76(8) . . ? O9 Mn3 O5 93.34(9) . . ? O10 Mn3 O5 81.45(9) 16_544 . ? O11 Mn3 O5 83.20(9) . . ? O2 Mn3 O5 163.97(7) . . ? Mn2 O1 Mn1 98.15(9) . . ? Mn2 O1 Mn3 105.75(9) . . ? Mn1 O1 Mn3 128.61(11) . . ? Mn2 O1 H1 107.5 . . ? Mn1 O1 H1 107.5 . . ? Mn3 O1 H1 107.5 . . ? O2 C99 O2 120.007(1) 3_665 . ? O2 C99 O2 119.997(1) 3_665 2_655 ? O2 C99 O2 120.0 . 2_655 ? C99 O2 Mn3 122.80(6) . 17_554 ? C99 O2 Mn3 122.81(6) . . ? Mn3 O2 Mn3 114.39(12) 17_554 . ? C1 O3 Mn2 135.3(2) . . ? C1 O3 Mn1 132.8(2) . . ? Mn2 O3 Mn1 91.83(8) . . ? C1 O4 Mn2 127.7(2) . 2_655 ? O4 C1 O3 121.8(3) . . ? O4 C1 C2 119.1(4) . . ? O3 C1 C2 119.1(4) . . ? C3 C2 C7 117.9(4) . . ? C3 C2 C1 115.1(4) . . ? C7 C2 C1 127.0(4) . . ? C4 C3 C2 120.5(5) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C5 C4 C3 119.6(5) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C6 C5 C4 121.2(5) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 121.4(5) . . ? C5 C6 H6A 119.3 . . ? C7 C6 H6A 119.3 . . ? C6 C7 C2 119.4(4) . . ? C6 C7 N2 121.9(4) . . ? C2 C7 N2 118.5(4) . . ? N3 N2 C7 111.7(3) . . ? N3 N2 Mn2 123.0(3) . . ? C7 N2 Mn2 122.5(2) . . ? N2 N3 C8 119.6(3) . . ? N3 C8 C10 113.8(4) . . ? N3 C8 C9 128.6(4) . . ? C10 C8 C9 117.4(4) . . ? O5 C9 N12 119.3(3) . . ? O5 C9 C8 119.7(4) . . ? N12 C9 C8 120.5(3) . . ? C9 O5 Mn2 118.2(2) . . ? C9 O5 Mn3 130.8(2) . . ? Mn2 O5 Mn3 98.59(8) . . ? N5 C10 N6 118.8(4) . . ? N5 C10 C8 120.9(4) . . ? N6 C10 C8 120.3(4) . . ? C10 N5 H5 119(4) . . ? C11 N12 C9 116.8(3) . . ? C11 N6 C10 117.5(4) . . ? C11 N6 H6 121.3 . . ? C10 N6 H6 121.3 . . ? N6 C11 N12 127.1(4) . . ? N6 C11 C12 116.8(4) . . ? N12 C11 C12 116.1(4) . . ? N7 C12 C13 112.3(4) . . ? N7 C12 C11 129.2(4) . . ? C13 C12 C11 118.5(4) . . ? N4 C13 C12 175.2(7) . . ? N8 N7 C12 120.1(4) . . ? N7 N8 C14 118.4(3) . . ? N7 N8 H8 120.8 . . ? C14 N8 H8 120.8 . . ? C15 C14 N8 120.6(4) . . ? C15 C14 C19 118.7(4) . . ? N8 C14 C19 120.7(4) . . ? C16 C15 C14 120.8(5) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 122.3(5) . . ? C15 C16 H16A 118.8 . . ? C17 C16 H16A 118.8 . . ? C18 C17 C16 118.3(5) . . ? C18 C17 H17A 120.8 . . ? C16 C17 H17A 120.8 . . ? C19 C18 C17 120.2(4) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C18 C19 C14 119.6(4) . . ? C18 C19 C20 117.9(4) . . ? C14 C19 C20 122.5(4) . . ? O10 C20 O9 123.6(3) . . ? O10 C20 C19 116.6(3) . . ? O9 C20 C19 119.7(3) . . ? C20 O9 Mn3 124.8(2) . . ? C20 O10 Mn3 132.4(2) . 16_544 ? C21 O11 Mn3 118.9(2) . . ? O11 C21 O11 125.0(4) . 17_554 ? O11 C21 C22 114.1(4) . 17_554 ? O11 C21 C22 120.8(4) 17_554 17_554 ? O11 C21 C22 120.8(4) . . ? O11 C21 C22 114.1(4) 17_554 . ? C23 C22 C27 120.0 . . ? C23 C22 C21 116.9(5) . . ? C27 C22 C21 122.9(5) . . ? C22 C23 C24 120.0 . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? N9 C27 C26 119.7(6) . . ? N9 C27 C22 119.9(6) . . ? C26 C27 C22 120.0 . . ? N10 N9 C27 119.4(8) . . ? N10 N9 H9 120.3 . . ? C27 N9 H9 120.3 . . ? N9 N10 C28 122.2(11) . . ? N10 C28 C29 127.9(13) . . ? N10 C28 C30A 115.3(18) . . ? C29 C28 C30A 116.3(18) . . ? N10 C28 C30B 106.2(16) . . ? C29 C28 C30B 114.7(17) . . ? O13 C29 C28 119.9(11) . . ? O13 C29 O12 129.2(10) . . ? C28 C29 O12 110.7(10) . . ? C29 O12 Mn2 123.2(5) . . ? N11A C30A C28 165(3) . . ? C28 C30A N11B 118(2) . . ? N11B C30B C28 172(4) . . ? N11A C30B C28 132(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.697 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.064