# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Constantinos Milios' _publ_contact_author_email KOMIL@CHEMISTRY.UOC.GR _publ_section_title ; The first amino acid manganese cluster: A [MnIV2MnIII3] DL-valine cage ; loop_ _publ_author_name 'Constantinos Milios' 'Euan Brechin' 'Chrysa Kozoni' 'Tadeusz Lis' 'Milosz Siczek' # Attachment 'xc31grap.cif' data_xc31grap _database_code_depnum_ccdc_archive 'CCDC 734399' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H68 Mn5 N7 O17, C5 H11 N O2, 2.5(H2 O)' _chemical_formula_sum 'C65 H82 Mn5 N8 O20.50' _chemical_formula_weight 1578.09 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 14.331(5) _cell_length_b 22.238(8) _cell_length_c 23.426(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.16(5) _cell_angle_gamma 90.00 _cell_volume 7446(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 14962 _cell_measurement_theta_min 4.5 _cell_measurement_theta_max 38.5 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.395 _exptl_crystal_size_mid 0.167 _exptl_crystal_size_min 0.023 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3268 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur PX KM4CCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61094 _diffrn_reflns_av_R_equivalents 0.1639 _diffrn_reflns_av_sigmaI/netI 0.2820 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.28 _diffrn_reflns_theta_max 26.74 _reflns_number_total 15580 _reflns_number_gt 5211 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0131P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15580 _refine_ls_number_parameters 905 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.2271 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.1047 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.113 _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 Mn2 Mn 0.08064(7) 0.52637(4) 0.22197(4) 0.0426(3) Uani 1 1 d . . . Mn1 Mn 0.16262(7) 0.38877(4) 0.21105(4) 0.0443(3) Uani 1 1 d . . . Mn4 Mn -0.04525(6) 0.42881(4) 0.16076(4) 0.0416(3) Uani 1 1 d . . . Mn3 Mn 0.23437(7) 0.48142(4) 0.31877(4) 0.0487(3) Uani 1 1 d . . . Mn5 Mn 0.25066(7) 0.33842(4) 0.32331(4) 0.0471(3) Uani 1 1 d . . . O1 O 0.0586(2) 0.44099(14) 0.21332(14) 0.0371(11) Uani 1 1 d . . . O2 O 0.1952(3) 0.40631(15) 0.28842(15) 0.0457(11) Uani 1 1 d . . . O11 O 0.2692(3) 0.34056(17) 0.2072(2) 0.0491(13) Uani 1 1 d . . . O21 O 0.2320(3) 0.50585(16) 0.22404(16) 0.0420(11) Uani 1 1 d . . . N11 N 0.2470(4) 0.4561(2) 0.1918(2) 0.0402(15) Uani 1 1 d . . . C11 C 0.3156(5) 0.3425(4) 0.1594(4) 0.052(2) Uani 1 1 d . . . C21 C 0.3356(4) 0.3974(3) 0.1320(3) 0.0453(19) Uani 1 1 d . . . C31 C 0.3828(5) 0.3958(4) 0.0831(3) 0.061(2) Uani 1 1 d . . . H31 H 0.3943 0.4321 0.0635 0.073 Uiso 1 1 calc R . . C41 C 0.4143(5) 0.3409(5) 0.0620(3) 0.083(3) Uani 1 1 d . . . H41 H 0.4480 0.3402 0.0285 0.099 Uiso 1 1 calc R . . C51 C 0.3965(6) 0.2892(4) 0.0892(4) 0.079(3) Uani 1 1 d . . . H51 H 0.4171 0.2520 0.0747 0.095 Uiso 1 1 calc R . . C61 C 0.3498(5) 0.2902(3) 0.1370(4) 0.065(3) Uani 1 1 d . . . H61 H 0.3399 0.2533 0.1562 0.079 Uiso 1 1 calc R . . C71 C 0.3112(5) 0.4556(3) 0.1565(3) 0.046(2) Uani 1 1 d . . . C81 C 0.3617(4) 0.5120(3) 0.1458(3) 0.055(2) Uani 1 1 d . . . H81A H 0.3269 0.5461 0.1611 0.066 Uiso 1 1 calc R . . H81B H 0.3630 0.5178 0.1039 0.066 Uiso 1 1 calc R . . C91 C 0.4607(4) 0.5130(3) 0.1724(3) 0.069(2) Uani 1 1 d . . . H91A H 0.4601 0.5086 0.2140 0.104 Uiso 1 1 calc R . . H91B H 0.4903 0.5513 0.1635 0.104 Uiso 1 1 calc R . . H91C H 0.4961 0.4797 0.1570 0.104 Uiso 1 1 calc R . . O12 O 0.1118(3) 0.60770(16) 0.22236(17) 0.0440(12) Uani 1 1 d . . . O22 O -0.0019(3) 0.48904(16) 0.11246(15) 0.0426(11) Uani 1 1 d . . . N12 N 0.0635(3) 0.5300(2) 0.1373(2) 0.0328(13) Uani 1 1 d . . . C12 C 0.1682(5) 0.6292(3) 0.1850(3) 0.0397(19) Uani 1 1 d . . . C22 C 0.1660(4) 0.6122(3) 0.1277(3) 0.0375(17) Uani 1 1 d . . . C32 C 0.2277(5) 0.6413(3) 0.0931(3) 0.052(2) Uani 1 1 d . . . H32 H 0.2239 0.6328 0.0533 0.062 Uiso 1 1 calc R . . C42 C 0.2933(5) 0.6815(3) 0.1147(3) 0.055(2) Uani 1 1 d . . . H42 H 0.3372 0.6990 0.0911 0.066 Uiso 1 1 calc R . . C52 C 0.2933(5) 0.6956(3) 0.1717(4) 0.063(2) Uani 1 1 d . . . H52 H 0.3370 0.7246 0.1869 0.075 Uiso 1 1 calc R . . C62 C 0.2347(5) 0.6707(3) 0.2070(3) 0.059(2) Uani 1 1 d . . . H62 H 0.2383 0.6811 0.2465 0.071 Uiso 1 1 calc R . . C72 C 0.1008(4) 0.5660(3) 0.1030(3) 0.0317(16) Uani 1 1 d . . . C82 C 0.0874(4) 0.5576(3) 0.0387(2) 0.0424(18) Uani 1 1 d . . . H82A H 0.0215 0.5467 0.0279 0.051 Uiso 1 1 calc R . . H82B H 0.1013 0.5958 0.0194 0.051 Uiso 1 1 calc R . . C92 C 0.1512(4) 0.5087(2) 0.0196(2) 0.0473(18) Uani 1 1 d . . . H92A H 0.2163 0.5191 0.0313 0.071 Uiso 1 1 calc R . . H92B H 0.1436 0.5048 -0.0221 0.071 Uiso 1 1 calc R . . H92C H 0.1352 0.4705 0.0374 0.071 Uiso 1 1 calc R . . O13 O 0.2814(3) 0.55251(18) 0.35071(18) 0.0620(14) Uani 1 1 d . . . O23 O 0.3633(3) 0.38398(18) 0.34273(16) 0.0496(12) Uani 1 1 d . . . N13 N 0.3632(4) 0.4444(2) 0.3327(2) 0.0482(15) Uani 1 1 d . . . C13 C 0.3672(6) 0.5745(3) 0.3424(3) 0.051(2) Uani 1 1 d . . . C23 C 0.4449(6) 0.5390(3) 0.3352(3) 0.053(2) Uani 1 1 d . . . C33 C 0.5278(6) 0.5678(4) 0.3272(3) 0.078(2) Uani 1 1 d . . . H33 H 0.5820 0.5444 0.3220 0.094 Uiso 1 1 calc R . . C43 C 0.5347(7) 0.6298(4) 0.3263(3) 0.090(3) Uani 1 1 d . . . H43 H 0.5919 0.6482 0.3181 0.108 Uiso 1 1 calc R . . C53 C 0.4593(7) 0.6646(4) 0.3373(3) 0.086(3) Uani 1 1 d . . . H53 H 0.4647 0.7071 0.3403 0.103 Uiso 1 1 calc R . . C63 C 0.3782(6) 0.6372(3) 0.3438(3) 0.076(3) Uani 1 1 d . . . H63 H 0.3250 0.6613 0.3496 0.091 Uiso 1 1 calc R . . C73 C 0.4428(5) 0.4722(3) 0.3399(3) 0.0497(19) Uani 1 1 d . . . C83 C 0.5283(5) 0.4350(3) 0.3542(3) 0.068(2) Uani 1 1 d . . . H83A H 0.5834 0.4540 0.3385 0.081 Uiso 1 1 calc R . . H83B H 0.5201 0.3943 0.3373 0.081 Uiso 1 1 calc R . . C93 C 0.5427(6) 0.4306(4) 0.4187(4) 0.145(4) Uani 1 1 d . . . H93A H 0.5060 0.4619 0.4362 0.218 Uiso 1 1 calc R . . H93B H 0.6092 0.4361 0.4305 0.218 Uiso 1 1 calc R . . H93C H 0.5223 0.3909 0.4311 0.218 Uiso 1 1 calc R . . O14 O -0.1391(3) 0.41724(17) 0.10300(15) 0.0461(12) Uani 1 1 d . . . O24 O 0.1250(3) 0.37111(15) 0.13399(15) 0.0421(12) Uani 1 1 d . . . N14 N 0.0294(4) 0.3648(2) 0.1246(2) 0.0413(15) Uani 1 1 d . . . C14 C -0.1642(5) 0.3620(3) 0.0842(2) 0.048(2) Uani 1 1 d . . . C24 C -0.1021(5) 0.3147(3) 0.0781(3) 0.0418(18) Uani 1 1 d . . . C34 C -0.1383(5) 0.2603(3) 0.0572(3) 0.058(2) Uani 1 1 d . . . H34 H -0.0969 0.2275 0.0527 0.070 Uiso 1 1 calc R . . C44 C -0.2330(6) 0.2527(3) 0.0427(3) 0.069(2) Uani 1 1 d . . . H44 H -0.2560 0.2148 0.0293 0.082 Uiso 1 1 calc R . . C54 C -0.2938(5) 0.2998(3) 0.0477(3) 0.063(2) Uani 1 1 d . . . H54 H -0.3586 0.2948 0.0372 0.075 Uiso 1 1 calc R . . C64 C -0.2601(5) 0.3544(3) 0.0680(3) 0.057(2) Uani 1 1 d . . . H64 H -0.3018 0.3872 0.0712 0.069 Uiso 1 1 calc R . . C74 C 0.0017(5) 0.3201(3) 0.0929(3) 0.0445(19) Uani 1 1 d . . . C84 C 0.0685(5) 0.2779(3) 0.0684(3) 0.0498(19) Uani 1 1 d . . . H84A H 0.0415 0.2369 0.0667 0.060 Uiso 1 1 calc R . . H84B H 0.1274 0.2767 0.0933 0.060 Uiso 1 1 calc R . . C94 C 0.0892(5) 0.2975(3) 0.0092(3) 0.077(2) Uani 1 1 d . . . H94A H 0.0310 0.2988 -0.0153 0.116 Uiso 1 1 calc R . . H94B H 0.1326 0.2690 -0.0066 0.116 Uiso 1 1 calc R . . H94C H 0.1177 0.3376 0.0111 0.116 Uiso 1 1 calc R . . O15 O 0.3016(3) 0.26623(17) 0.34764(17) 0.0529(13) Uani 1 1 d . . . O25 O 0.0968(3) 0.32268(16) 0.23858(16) 0.0498(13) Uani 1 1 d . . . N15 N 0.1441(3) 0.2932(2) 0.2841(2) 0.0433(15) Uani 1 1 d . . . C15 C 0.2544(5) 0.2191(3) 0.3639(3) 0.0449(19) Uani 1 1 d . . . C25 C 0.1641(5) 0.2035(3) 0.3398(2) 0.0359(17) Uani 1 1 d . . . C35 C 0.1231(5) 0.1522(3) 0.3591(3) 0.0465(19) Uani 1 1 d . . . H35 H 0.0618 0.1426 0.3437 0.056 Uiso 1 1 calc R . . C45 C 0.1644(5) 0.1145(3) 0.3988(3) 0.063(2) Uani 1 1 d . . . H45 H 0.1336 0.0791 0.4101 0.076 Uiso 1 1 calc R . . C55 C 0.2553(5) 0.1297(3) 0.4229(3) 0.067(2) Uani 1 1 d . . . H55 H 0.2864 0.1049 0.4513 0.081 Uiso 1 1 calc R . . C65 C 0.2963(5) 0.1800(3) 0.4048(3) 0.063(2) Uani 1 1 d . . . H65 H 0.3575 0.1894 0.4206 0.076 Uiso 1 1 calc R . . C75 C 0.1164(4) 0.2392(3) 0.2947(3) 0.0406(18) Uani 1 1 d . . . C85 C 0.0392(5) 0.2134(3) 0.2549(3) 0.064(2) Uani 1 1 d . . . H85A H -0.0065 0.2454 0.2434 0.077 Uiso 1 1 calc R . . H85B H 0.0060 0.1815 0.2748 0.077 Uiso 1 1 calc R . . C95 C 0.0795(5) 0.1875(3) 0.2021(3) 0.083(3) Uani 1 1 d . . . H95A H 0.1159 0.2186 0.1839 0.124 Uiso 1 1 calc R . . H95B H 0.0285 0.1738 0.1751 0.124 Uiso 1 1 calc R . . H95C H 0.1203 0.1535 0.2132 0.124 Uiso 1 1 calc R . . O16 O -0.0958(3) 0.37048(16) 0.20685(16) 0.0420(12) Uani 1 1 d . . . O26 O -0.0651(3) 0.53684(16) 0.22337(16) 0.0428(12) Uani 1 1 d . . . N16 N -0.1134(4) 0.4876(2) 0.2065(2) 0.0415(15) Uani 1 1 d . . . C16 C -0.1887(6) 0.3687(3) 0.2080(2) 0.0417(19) Uani 1 1 d . . . C26 C -0.2413(5) 0.4218(3) 0.2149(2) 0.0441(18) Uani 1 1 d . . . C36 C -0.3378(5) 0.4161(3) 0.2165(3) 0.062(2) Uani 1 1 d . . . H36 H -0.3739 0.4517 0.2196 0.074 Uiso 1 1 calc R . . C46 C -0.3838(5) 0.3617(4) 0.2137(3) 0.069(2) Uani 1 1 d . . . H46 H -0.4498 0.3598 0.2148 0.082 Uiso 1 1 calc R . . C56 C -0.3308(6) 0.3096(3) 0.2091(3) 0.060(2) Uani 1 1 d . . . H56 H -0.3609 0.2715 0.2079 0.072 Uiso 1 1 calc R . . C66 C -0.2354(5) 0.3127(3) 0.2065(3) 0.053(2) Uani 1 1 d . . . H66 H -0.2004 0.2767 0.2035 0.063 Uiso 1 1 calc R . . C76 C -0.1964(5) 0.4792(3) 0.2246(3) 0.0436(19) Uani 1 1 d . . . C86 C -0.2363(4) 0.5271(3) 0.2636(3) 0.064(2) Uani 1 1 d . . . H86A H -0.2830 0.5086 0.2874 0.077 Uiso 1 1 calc R . . H86B H -0.1855 0.5445 0.2893 0.077 Uiso 1 1 calc R . . C96 C -0.2816(5) 0.5752(3) 0.2262(3) 0.092(3) Uani 1 1 d . . . H96A H -0.2350 0.5930 0.2026 0.138 Uiso 1 1 calc R . . H96B H -0.3069 0.6065 0.2502 0.138 Uiso 1 1 calc R . . H96C H -0.3325 0.5577 0.2014 0.138 Uiso 1 1 calc R . . O17 O 0.2032(3) 0.45251(17) 0.40344(17) 0.0565(15) Uani 1 1 d D . . O27 O 0.1884(3) 0.35346(17) 0.40175(16) 0.0571(13) Uani 1 1 d D . . N17 N 0.1407(3) 0.4643(2) 0.50286(19) 0.0665(17) Uani 1 1 d D . . H17A H 0.1778 0.4919 0.4869 0.100 Uiso 1 1 calc R . . H17B H 0.1444 0.4692 0.5415 0.100 Uiso 1 1 calc R . . H17C H 0.0805 0.4694 0.4887 0.100 Uiso 1 1 calc R . . C17 C 0.1878(4) 0.4037(3) 0.4250(3) 0.046(2) Uani 1 1 d D . . C27 C 0.1717(4) 0.4045(3) 0.4893(3) 0.065(2) Uani 1 1 d D . . H27 H 0.1205 0.3754 0.4963 0.077 Uiso 1 1 calc R . . C37 C 0.2593(6) 0.3872(4) 0.5280(3) 0.102(3) Uani 1 1 d D . . H37A H 0.2735 0.3464 0.5132 0.123 Uiso 0.56 1 d P . . H37B H 0.2374 0.3833 0.5658 0.123 Uiso 0.23 1 d P . . H37C H 0.2993 0.4171 0.5277 0.123 Uiso 0.21 1 d P . . C47 C 0.3383(5) 0.4284(5) 0.5243(4) 0.107(4) Uani 0.767(4) 1 d PD . . H47A H 0.3937 0.4117 0.5457 0.160 Uiso 0.767(4) 1 calc PR . . H47B H 0.3228 0.4674 0.5407 0.160 Uiso 0.767(4) 1 calc PR . . H47C H 0.3513 0.4337 0.4841 0.160 Uiso 0.767(4) 1 calc PR . . C67 C 0.2847(10) 0.3270(5) 0.5131(8) 0.184(14) Uiso 0.421(13) 1 d PD . . H67A H 0.3335 0.3283 0.4860 0.276 Uiso 0.421(13) 1 calc PR . . H67B H 0.2296 0.3061 0.4956 0.276 Uiso 0.421(13) 1 calc PR . . H67C H 0.3081 0.3054 0.5477 0.276 Uiso 0.421(13) 1 calc PR . . C57 C 0.2259(7) 0.3745(4) 0.5885(4) 0.104(5) Uani 0.812(12) 1 d P . . H57A H 0.1670 0.3520 0.5848 0.156 Uiso 0.812(12) 1 calc PR . . H57B H 0.2163 0.4127 0.6081 0.156 Uiso 0.812(12) 1 calc PR . . H57C H 0.2734 0.3508 0.6107 0.156 Uiso 0.812(12) 1 calc PR . . O18 O -0.0166(4) 0.4397(3) 0.4316(3) 0.124(3) Uani 1 1 d D . . O28 O -0.1423(4) 0.4848(2) 0.3949(2) 0.116(2) Uani 1 1 d D . . N18 N 0.0038(3) 0.3981(2) 0.32199(19) 0.0580(16) Uani 1 1 d D . . H18A H 0.0005 0.3726 0.2915 0.087 Uiso 1 1 calc R . . H18B H 0.0462 0.3838 0.3495 0.087 Uiso 1 1 calc R . . H18C H 0.0219 0.4351 0.3106 0.087 Uiso 1 1 calc R . . C18 C -0.0780(5) 0.4478(3) 0.3940(3) 0.071(3) Uani 1 1 d D . . C28 C -0.0860(5) 0.4023(3) 0.3445(3) 0.101(3) Uani 1 1 d D . . H28A H -0.1284 0.4210 0.3137 0.121 Uiso 1 1 calc R . . C38 C -0.1293(5) 0.3410(3) 0.3575(3) 0.071(2) Uani 1 1 d D . . H38A H -0.1318 0.3173 0.3211 0.085 Uiso 1 1 calc R . . C48 C -0.0789(5) 0.3044(3) 0.4014(3) 0.101(3) Uani 1 1 d D . . H48A H -0.1148 0.2677 0.4077 0.151 Uiso 1 1 calc R . . H48B H -0.0708 0.3273 0.4371 0.151 Uiso 1 1 calc R . . H48C H -0.0175 0.2935 0.3887 0.151 Uiso 1 1 calc R . . C58 C -0.2245(5) 0.3519(3) 0.3703(3) 0.079(3) Uani 1 1 d D . . H58A H -0.2539 0.3139 0.3802 0.119 Uiso 1 1 calc R . . H58B H -0.2591 0.3696 0.3368 0.119 Uiso 1 1 calc R . . H58C H -0.2253 0.3797 0.4027 0.119 Uiso 1 1 calc R . . O19 O 0.1058(3) 0.51461(16) 0.30528(15) 0.0396(11) Uani 1 1 d . . . C19 C 0.0763(4) 0.5585(2) 0.3431(2) 0.0430(18) Uani 1 1 d . . . H19A H 0.1130 0.5953 0.3392 0.065 Uiso 1 1 calc R . . H19B H 0.0855 0.5436 0.3825 0.065 Uiso 1 1 calc R . . H19C H 0.0099 0.5673 0.3340 0.065 Uiso 1 1 calc R . . O1W O 0.2462(4) 0.5742(2) 0.4680(2) 0.118(2) Uani 1 1 d . . . H1W1 H 0.2553 0.5737 0.4339 0.177 Uiso 1 1 d R . . H2W1 H 0.1973 0.5895 0.4771 0.177 Uiso 1 1 d R . . O2W O -0.0554(8) 0.3842(5) 0.5309(5) 0.131(4) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn2 0.0530(7) 0.0317(6) 0.0410(7) -0.0024(5) -0.0111(5) 0.0052(6) Mn1 0.0527(7) 0.0295(6) 0.0480(7) -0.0027(5) -0.0156(6) 0.0052(6) Mn4 0.0471(7) 0.0326(6) 0.0427(7) 0.0005(5) -0.0123(6) 0.0018(6) Mn3 0.0553(7) 0.0338(6) 0.0537(7) -0.0035(5) -0.0186(6) 0.0008(6) Mn5 0.0526(7) 0.0347(6) 0.0505(7) 0.0005(5) -0.0192(6) 0.0012(6) O1 0.044(3) 0.030(2) 0.035(3) -0.0046(18) -0.013(2) 0.004(2) O2 0.053(3) 0.035(2) 0.047(3) -0.006(2) -0.011(2) 0.013(2) O11 0.043(3) 0.038(3) 0.063(4) 0.002(2) -0.020(3) 0.005(2) O21 0.043(3) 0.031(3) 0.050(3) -0.007(2) -0.008(2) 0.006(2) N11 0.043(4) 0.026(3) 0.048(4) 0.001(3) -0.017(3) 0.015(3) C11 0.034(5) 0.051(5) 0.066(6) -0.003(5) -0.026(4) 0.009(5) C21 0.030(5) 0.067(6) 0.037(5) -0.019(4) -0.008(4) 0.016(4) C31 0.044(5) 0.080(6) 0.055(6) -0.015(5) -0.021(4) 0.023(5) C41 0.085(7) 0.091(7) 0.068(6) -0.018(6) -0.023(5) 0.031(6) C51 0.094(8) 0.067(7) 0.071(7) -0.025(6) -0.029(6) 0.040(6) C61 0.055(6) 0.053(5) 0.083(7) -0.022(5) -0.031(5) 0.025(5) C71 0.035(5) 0.058(6) 0.044(5) -0.001(4) -0.001(4) 0.011(4) C81 0.051(5) 0.048(5) 0.064(5) -0.006(4) -0.011(4) 0.003(4) C91 0.041(5) 0.073(5) 0.089(6) 0.008(4) -0.026(4) -0.003(4) O12 0.062(3) 0.033(3) 0.035(3) 0.002(2) -0.004(2) 0.004(2) O22 0.050(3) 0.038(3) 0.036(3) -0.005(2) -0.018(2) 0.008(2) N12 0.046(4) 0.020(3) 0.031(3) 0.004(2) -0.003(3) 0.006(3) C12 0.048(5) 0.016(4) 0.054(6) -0.004(3) -0.004(4) 0.001(4) C22 0.046(5) 0.024(4) 0.041(5) 0.002(4) -0.003(4) 0.004(4) C32 0.075(6) 0.027(4) 0.049(5) -0.001(3) -0.024(5) -0.005(4) C42 0.072(6) 0.038(4) 0.054(6) -0.006(4) -0.001(4) -0.016(4) C52 0.072(6) 0.044(5) 0.068(7) -0.022(4) -0.021(5) -0.011(4) C62 0.083(6) 0.049(5) 0.043(5) 0.007(4) -0.009(5) -0.015(5) C72 0.042(4) 0.027(4) 0.026(4) -0.006(3) -0.002(3) 0.013(4) C82 0.039(4) 0.043(4) 0.043(5) 0.002(3) -0.008(4) 0.001(4) C92 0.060(5) 0.037(4) 0.043(4) -0.009(3) -0.006(4) 0.001(4) O13 0.066(4) 0.047(3) 0.069(4) -0.019(2) -0.026(3) 0.012(3) O23 0.037(3) 0.040(3) 0.068(3) 0.005(2) -0.021(2) 0.000(2) N13 0.060(4) 0.033(4) 0.049(4) 0.000(3) -0.011(3) 0.000(3) C13 0.046(5) 0.044(5) 0.059(5) -0.009(4) -0.023(4) 0.002(5) C23 0.062(6) 0.047(5) 0.047(5) -0.006(4) -0.013(4) -0.018(5) C33 0.062(6) 0.058(6) 0.114(7) -0.005(5) -0.002(5) -0.015(5) C43 0.091(8) 0.055(6) 0.121(8) 0.005(5) -0.004(6) -0.036(6) C53 0.077(7) 0.048(6) 0.125(8) -0.015(5) -0.048(6) -0.003(6) C63 0.073(7) 0.050(6) 0.097(6) -0.015(4) -0.048(5) -0.009(5) C73 0.037(5) 0.057(5) 0.053(5) 0.001(4) -0.007(4) -0.007(5) C83 0.039(5) 0.084(6) 0.080(6) 0.010(5) -0.001(4) -0.008(5) C93 0.113(8) 0.203(11) 0.115(9) 0.015(7) -0.028(7) 0.074(7) O14 0.047(3) 0.041(3) 0.047(3) 0.006(2) -0.020(2) -0.001(2) O24 0.043(3) 0.033(3) 0.048(3) -0.0109(19) -0.011(2) 0.008(2) N14 0.057(4) 0.032(3) 0.033(4) 0.001(2) -0.010(3) -0.009(3) C14 0.060(6) 0.050(5) 0.031(4) -0.005(3) -0.022(4) -0.005(5) C24 0.047(5) 0.031(4) 0.048(5) -0.002(3) 0.006(4) -0.002(4) C34 0.057(6) 0.042(5) 0.073(6) -0.009(4) -0.014(4) -0.007(4) C44 0.082(7) 0.051(5) 0.070(6) -0.022(4) -0.017(5) -0.030(5) C54 0.057(6) 0.058(5) 0.070(6) -0.009(4) -0.021(5) -0.013(5) C64 0.057(6) 0.062(5) 0.051(5) -0.001(4) -0.015(4) 0.004(4) C74 0.061(6) 0.029(4) 0.041(5) 0.006(3) -0.015(4) 0.004(4) C84 0.051(5) 0.038(4) 0.058(5) -0.013(4) -0.008(4) 0.003(4) C94 0.088(7) 0.087(6) 0.060(6) -0.001(4) 0.025(5) 0.023(5) O15 0.049(3) 0.036(3) 0.070(3) 0.013(2) -0.020(3) -0.001(2) O25 0.055(3) 0.034(3) 0.057(3) 0.004(2) -0.018(3) 0.010(2) N15 0.055(4) 0.028(3) 0.044(4) 0.002(3) -0.011(3) 0.012(3) C15 0.052(5) 0.017(4) 0.064(5) 0.011(3) -0.006(4) 0.006(4) C25 0.053(5) 0.025(4) 0.029(4) -0.001(3) -0.008(4) 0.009(4) C35 0.067(5) 0.028(4) 0.043(5) 0.007(3) -0.007(4) 0.002(4) C45 0.108(7) 0.038(4) 0.041(5) 0.010(4) -0.004(5) -0.020(5) C55 0.091(7) 0.039(5) 0.066(6) 0.010(4) -0.032(5) 0.000(5) C65 0.088(6) 0.031(4) 0.066(5) 0.002(4) -0.029(5) -0.003(4) C75 0.052(5) 0.033(4) 0.035(4) -0.003(3) -0.010(4) 0.007(4) C85 0.062(5) 0.043(5) 0.083(6) 0.034(4) -0.033(5) -0.021(4) C95 0.135(8) 0.049(5) 0.059(6) -0.016(4) -0.028(6) -0.007(5) O16 0.034(3) 0.046(3) 0.044(3) 0.002(2) -0.013(2) 0.010(2) O26 0.041(3) 0.029(3) 0.058(3) -0.001(2) -0.008(2) 0.005(2) N16 0.045(4) 0.031(3) 0.045(4) 0.001(3) -0.016(3) -0.006(3) C16 0.063(6) 0.028(4) 0.032(4) -0.006(3) -0.012(4) 0.003(5) C26 0.038(5) 0.048(5) 0.045(4) 0.008(3) -0.011(4) -0.002(4) C36 0.051(6) 0.042(5) 0.092(6) 0.016(4) -0.008(4) 0.007(5) C46 0.045(5) 0.065(5) 0.092(6) 0.025(5) -0.016(5) 0.000(5) C56 0.066(6) 0.054(5) 0.058(5) 0.012(4) -0.009(5) -0.016(5) C66 0.050(5) 0.052(5) 0.053(5) 0.005(4) -0.012(4) 0.004(5) C76 0.038(5) 0.041(5) 0.049(5) 0.001(4) -0.014(4) 0.000(5) C86 0.039(5) 0.041(5) 0.114(7) 0.021(5) 0.012(5) 0.008(4) C96 0.123(8) 0.071(6) 0.082(6) 0.002(5) 0.012(5) -0.004(6) O17 0.063(3) 0.039(3) 0.064(3) -0.004(2) -0.021(3) 0.011(3) O27 0.071(3) 0.038(3) 0.060(3) -0.003(2) -0.017(3) -0.003(3) N17 0.066(4) 0.079(4) 0.052(4) -0.008(3) -0.021(3) 0.010(4) C17 0.034(4) 0.051(5) 0.051(6) -0.018(4) -0.012(4) 0.006(4) C27 0.077(6) 0.053(5) 0.063(6) -0.018(4) -0.005(5) 0.017(4) C37 0.127(9) 0.129(8) 0.046(7) -0.013(5) -0.019(6) 0.071(7) C47 0.027(7) 0.171(12) 0.119(10) -0.006(9) -0.015(7) -0.012(7) C57 0.155(11) 0.118(9) 0.035(8) 0.016(6) -0.022(7) 0.041(7) O18 0.071(4) 0.137(5) 0.152(6) -0.064(4) -0.058(4) 0.030(4) O28 0.189(7) 0.078(4) 0.081(4) -0.024(3) 0.013(4) 0.012(4) N18 0.077(5) 0.050(4) 0.045(4) -0.006(3) -0.006(3) -0.010(4) C18 0.065(7) 0.079(7) 0.074(7) -0.018(5) 0.041(6) 0.016(5) C28 0.103(8) 0.101(8) 0.102(8) -0.044(6) 0.040(6) 0.003(7) C38 0.091(7) 0.056(5) 0.063(6) 0.015(4) -0.016(5) -0.035(6) C48 0.067(6) 0.132(8) 0.103(7) -0.006(6) 0.000(5) 0.020(6) C58 0.062(6) 0.080(6) 0.095(7) 0.029(5) 0.001(5) -0.002(5) O19 0.047(3) 0.039(3) 0.032(3) -0.010(2) -0.001(2) 0.009(2) C19 0.034(4) 0.045(4) 0.048(5) -0.003(3) -0.010(4) -0.006(4) O1W 0.163(5) 0.085(4) 0.101(4) -0.013(3) -0.023(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn2 O12 1.863(4) . ? Mn2 O1 1.933(3) . ? Mn2 O19 1.976(4) . ? Mn2 N12 1.982(5) . ? Mn2 O26 2.105(4) . ? Mn2 O21 2.214(4) . ? Mn2 Mn4 3.1053(16) . ? Mn2 Mn3 3.205(2) . ? Mn1 O11 1.874(4) . ? Mn1 O2 1.880(3) . ? Mn1 O25 1.885(4) . ? Mn1 O24 1.887(4) . ? Mn1 O1 1.893(3) . ? Mn1 N11 1.996(5) . ? Mn1 Mn5 3.0463(18) . ? Mn4 O14 1.855(4) . ? Mn4 O16 1.867(4) . ? Mn4 O1 1.881(3) . ? Mn4 O22 1.887(4) . ? Mn4 N16 1.991(5) . ? Mn4 N14 2.005(5) . ? Mn3 O13 1.855(4) . ? Mn3 O2 1.885(3) . ? Mn3 O19 1.988(4) . ? Mn3 N13 2.027(5) . ? Mn3 O17 2.162(4) . ? Mn3 O21 2.283(4) . ? Mn3 Mn5 3.1900(17) . ? Mn5 O15 1.837(4) . ? Mn5 O2 1.867(3) . ? Mn5 O23 1.932(4) . ? Mn5 N15 1.995(5) . ? Mn5 O27 2.127(4) . ? O11 C11 1.342(8) . ? O21 N11 1.365(5) . ? N11 C71 1.282(7) . ? C11 C61 1.382(9) . ? C11 C21 1.419(9) . ? C21 C31 1.371(8) . ? C21 C71 1.467(8) . ? C31 C41 1.404(9) . ? C31 H31 0.9500 . ? C41 C51 1.348(9) . ? C41 H41 0.9500 . ? C51 C61 1.346(9) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C71 C81 1.480(8) . ? C81 C91 1.508(6) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? O12 C12 1.323(7) . ? O22 N12 1.403(5) . ? N12 C72 1.277(6) . ? C12 C22 1.393(8) . ? C12 C62 1.399(8) . ? C22 C32 1.400(8) . ? C22 C72 1.477(8) . ? C32 C42 1.366(7) . ? C32 H32 0.9500 . ? C42 C52 1.372(8) . ? C42 H42 0.9500 . ? C52 C62 1.341(8) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? C72 C82 1.516(7) . ? C82 C92 1.510(7) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? O13 C13 1.349(7) . ? O23 N13 1.365(5) . ? N13 C73 1.297(7) . ? C13 C23 1.387(8) . ? C13 C63 1.402(8) . ? C23 C33 1.375(9) . ? C23 C73 1.490(8) . ? C33 C43 1.382(9) . ? C33 H33 0.9500 . ? C43 C53 1.369(9) . ? C43 H43 0.9500 . ? C53 C63 1.331(9) . ? C53 H53 0.9500 . ? C63 H63 0.9500 . ? C73 C83 1.496(8) . ? C83 C93 1.512(9) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? O14 C14 1.345(6) . ? O24 N14 1.379(5) . ? N14 C74 1.286(6) . ? C14 C24 1.391(8) . ? C14 C64 1.409(8) . ? C24 C34 1.392(7) . ? C24 C74 1.508(8) . ? C34 C44 1.386(8) . ? C34 H34 0.9500 . ? C44 C54 1.372(8) . ? C44 H44 0.9500 . ? C54 C64 1.380(8) . ? C54 H54 0.9500 . ? C64 H64 0.9500 . ? C74 C84 1.486(8) . ? C84 C94 1.502(7) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? O15 C15 1.318(6) . ? O25 N15 1.388(5) . ? N15 C75 1.295(6) . ? C15 C65 1.397(7) . ? C15 C25 1.417(7) . ? C25 C35 1.375(7) . ? C25 C75 1.452(7) . ? C35 C45 1.355(7) . ? C35 H35 0.9500 . ? C45 C55 1.422(8) . ? C45 H45 0.9500 . ? C55 C65 1.346(8) . ? C55 H55 0.9500 . ? C65 H65 0.9500 . ? C75 C85 1.508(7) . ? C85 C95 1.515(9) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? O16 C16 1.335(7) . ? O26 N16 1.340(5) . ? N16 C76 1.304(7) . ? C16 C66 1.413(8) . ? C16 C26 1.416(8) . ? C26 C36 1.391(8) . ? C26 C76 1.441(8) . ? C36 C46 1.376(8) . ? C36 H36 0.9500 . ? C46 C56 1.394(8) . ? C46 H46 0.9500 . ? C56 C66 1.374(8) . ? C56 H56 0.9500 . ? C66 H66 0.9500 . ? C76 C86 1.540(8) . ? C86 C96 1.500(7) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? O17 C17 1.225(5) . ? O27 C17 1.243(5) . ? N17 C27 1.446(5) . ? N17 H17A 0.9100 . ? N17 H17B 0.9100 . ? N17 H17C 0.9100 . ? C17 C27 1.539(6) . ? C27 C37 1.544(6) . ? C27 H27 1.0000 . ? C37 C67 1.437(8) . ? C37 C47 1.464(7) . ? C37 C57 1.554(10) . ? C37 H37A 0.996(8) . ? C37 H37B 0.964(8) . ? C37 H37C 0.878(9) . ? C47 H37C 0.623(9) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C67 H37A 0.462(9) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C57 H37B 0.600(9) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? O18 C18 1.213(6) . ? O28 C18 1.237(5) . ? N18 C28 1.429(5) . ? N18 H18A 0.9100 . ? N18 H18B 0.9100 . ? N18 H18C 0.9100 . ? C18 C28 1.538(6) . ? C28 C38 1.536(6) . ? C28 H28A 1.0000 . ? C38 C58 1.439(7) . ? C38 C48 1.461(6) . ? C38 H38A 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? O19 C19 1.404(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O1W H1W1 0.8201 . ? O1W H2W1 0.8200 . ? 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 O12 Mn2 O1 172.51(19) . . ? O12 Mn2 O19 95.57(16) . . ? O1 Mn2 O19 89.45(15) . . ? O12 Mn2 N12 88.70(19) . . ? O1 Mn2 N12 85.87(17) . . ? O19 Mn2 N12 173.70(17) . . ? O12 Mn2 O26 97.49(17) . . ? O1 Mn2 O26 87.45(15) . . ? O19 Mn2 O26 96.30(16) . . ? N12 Mn2 O26 87.71(18) . . ? O12 Mn2 O21 88.04(16) . . ? O1 Mn2 O21 87.26(15) . . ? O19 Mn2 O21 80.94(16) . . ? N12 Mn2 O21 94.61(18) . . ? O26 Mn2 O21 174.06(14) . . ? O12 Mn2 Mn4 144.26(11) . . ? O1 Mn2 Mn4 34.95(9) . . ? O19 Mn2 Mn4 114.96(12) . . ? N12 Mn2 Mn4 62.68(15) . . ? O26 Mn2 Mn4 62.64(11) . . ? O21 Mn2 Mn4 113.68(11) . . ? O12 Mn2 Mn3 98.46(11) . . ? O1 Mn2 Mn3 82.33(10) . . ? O19 Mn2 Mn3 36.19(11) . . ? N12 Mn2 Mn3 138.56(14) . . ? O26 Mn2 Mn3 130.97(11) . . ? O21 Mn2 Mn3 45.41(10) . . ? Mn4 Mn2 Mn3 117.09(5) . . ? O11 Mn1 O2 91.10(18) . . ? O11 Mn1 O25 90.05(18) . . ? O2 Mn1 O25 85.83(16) . . ? O11 Mn1 O24 90.69(18) . . ? O2 Mn1 O24 177.77(18) . . ? O25 Mn1 O24 92.84(17) . . ? O11 Mn1 O1 176.86(18) . . ? O2 Mn1 O1 89.22(15) . . ? O25 Mn1 O1 93.09(17) . . ? O24 Mn1 O1 89.06(16) . . ? O11 Mn1 N11 84.8(2) . . ? O2 Mn1 N11 87.11(19) . . ? O25 Mn1 N11 171.15(17) . . ? O24 Mn1 N11 94.4(2) . . ? O1 Mn1 N11 92.14(19) . . ? O11 Mn1 Mn5 62.84(15) . . ? O2 Mn1 Mn5 35.46(10) . . ? O25 Mn1 Mn5 66.70(11) . . ? O24 Mn1 Mn5 145.17(11) . . ? O1 Mn1 Mn5 118.61(12) . . ? N11 Mn1 Mn5 104.50(13) . . ? O14 Mn4 O16 91.97(17) . . ? O14 Mn4 O1 174.08(18) . . ? O16 Mn4 O1 92.46(16) . . ? O14 Mn4 O22 85.07(16) . . ? O16 Mn4 O22 176.42(17) . . ? O1 Mn4 O22 90.63(16) . . ? O14 Mn4 N16 97.20(19) . . ? O16 Mn4 N16 85.3(2) . . ? O1 Mn4 N16 87.08(18) . . ? O22 Mn4 N16 93.01(19) . . ? O14 Mn4 N14 88.54(19) . . ? O16 Mn4 N14 89.54(19) . . ? O1 Mn4 N14 87.57(18) . . ? O22 Mn4 N14 92.40(18) . . ? N16 Mn4 N14 172.44(19) . . ? O14 Mn4 Mn2 143.12(12) . . ? O16 Mn4 Mn2 117.06(12) . . ? O1 Mn4 Mn2 36.06(10) . . ? O22 Mn4 Mn2 64.88(11) . . ? N16 Mn4 Mn2 65.43(17) . . ? N14 Mn4 Mn2 112.41(16) . . ? O13 Mn3 O2 175.60(18) . . ? O13 Mn3 O19 93.06(18) . . ? O2 Mn3 O19 91.24(15) . . ? O13 Mn3 N13 88.9(2) . . ? O2 Mn3 N13 86.80(19) . . ? O19 Mn3 N13 177.8(2) . . ? O13 Mn3 O17 88.66(18) . . ? O2 Mn3 O17 90.39(16) . . ? O19 Mn3 O17 90.33(17) . . ? N13 Mn3 O17 88.73(19) . . ? O13 Mn3 O21 99.71(17) . . ? O2 Mn3 O21 82.02(15) . . ? O19 Mn3 O21 78.99(15) . . ? N13 Mn3 O21 101.66(18) . . ? O17 Mn3 O21 166.69(15) . . ? O13 Mn3 Mn5 144.35(13) . . ? O2 Mn3 Mn5 31.59(10) . . ? O19 Mn3 Mn5 116.11(11) . . ? N13 Mn3 Mn5 61.72(16) . . ? O17 Mn3 Mn5 72.09(11) . . ? O21 Mn3 Mn5 105.40(10) . . ? O13 Mn3 Mn2 103.35(13) . . ? O2 Mn3 Mn2 80.72(11) . . ? O19 Mn3 Mn2 35.94(11) . . ? N13 Mn3 Mn2 144.32(15) . . ? O17 Mn3 Mn2 124.39(12) . . ? O21 Mn3 Mn2 43.69(10) . . ? Mn5 Mn3 Mn2 112.30(3) . . ? O15 Mn5 O2 171.74(17) . . ? O15 Mn5 O23 94.53(18) . . ? O2 Mn5 O23 90.05(16) . . ? O15 Mn5 N15 88.60(19) . . ? O2 Mn5 N15 85.36(18) . . ? O23 Mn5 N15 166.17(19) . . ? O15 Mn5 O27 92.95(17) . . ? O2 Mn5 O27 93.37(16) . . ? O23 Mn5 O27 96.30(17) . . ? N15 Mn5 O27 96.99(19) . . ? O15 Mn5 Mn1 136.01(13) . . ? O2 Mn5 Mn1 35.74(11) . . ? O23 Mn5 Mn1 107.29(12) . . ? N15 Mn5 Mn1 62.17(15) . . ? O27 Mn5 Mn1 120.97(11) . . ? O15 Mn5 Mn3 155.24(12) . . ? O2 Mn5 Mn3 31.93(10) . . ? O23 Mn5 Mn3 62.79(12) . . ? N15 Mn5 Mn3 115.83(14) . . ? O27 Mn5 Mn3 80.66(11) . . ? Mn1 Mn5 Mn3 65.17(3) . . ? Mn4 O1 Mn1 118.72(17) . . ? Mn4 O1 Mn2 108.99(16) . . ? Mn1 O1 Mn2 118.85(18) . . ? Mn5 O2 Mn1 108.80(17) . . ? Mn5 O2 Mn3 116.47(17) . . ? Mn1 O2 Mn3 126.4(2) . . ? C11 O11 Mn1 118.4(4) . . ? N11 O21 Mn2 110.4(3) . . ? N11 O21 Mn3 110.6(3) . . ? Mn2 O21 Mn3 90.90(16) . . ? C71 N11 O21 120.9(6) . . ? C71 N11 Mn1 127.8(5) . . ? O21 N11 Mn1 111.2(4) . . ? O11 C11 C61 120.0(8) . . ? O11 C11 C21 122.3(7) . . ? C61 C11 C21 117.6(8) . . ? C31 C21 C11 118.9(7) . . ? C31 C21 C71 119.7(8) . . ? C11 C21 C71 121.3(7) . . ? C21 C31 C41 120.6(8) . . ? C21 C31 H31 119.7 . . ? C41 C31 H31 119.7 . . ? C51 C41 C31 119.8(9) . . ? C51 C41 H41 120.1 . . ? C31 C41 H41 120.1 . . ? C61 C51 C41 120.2(9) . . ? C61 C51 H51 119.9 . . ? C41 C51 H51 119.9 . . ? C51 C61 C11 122.7(9) . . ? C51 C61 H61 118.6 . . ? C11 C61 H61 118.6 . . ? N11 C71 C21 117.6(7) . . ? N11 C71 C81 119.0(6) . . ? C21 C71 C81 123.2(7) . . ? C71 C81 C91 113.5(5) . . ? C71 C81 H81A 108.9 . . ? C91 C81 H81A 108.9 . . ? C71 C81 H81B 108.9 . . ? C91 C81 H81B 108.9 . . ? H81A C81 H81B 107.7 . . ? C81 C91 H91A 109.5 . . ? C81 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C81 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C12 O12 Mn2 120.4(4) . . ? N12 O22 Mn4 116.8(3) . . ? C72 N12 O22 116.3(5) . . ? C72 N12 Mn2 128.9(4) . . ? O22 N12 Mn2 114.8(3) . . ? O12 C12 C22 124.6(6) . . ? O12 C12 C62 115.2(7) . . ? C22 C12 C62 120.2(7) . . ? C12 C22 C32 117.4(6) . . ? C12 C22 C72 122.3(6) . . ? C32 C22 C72 120.3(6) . . ? C42 C32 C22 122.4(6) . . ? C42 C32 H32 118.8 . . ? C22 C32 H32 118.8 . . ? C32 C42 C52 117.4(7) . . ? C32 C42 H42 121.3 . . ? C52 C42 H42 121.3 . . ? C62 C52 C42 123.4(7) . . ? C62 C52 H52 118.3 . . ? C42 C52 H52 118.3 . . ? C52 C62 C12 119.0(7) . . ? C52 C62 H62 120.5 . . ? C12 C62 H62 120.5 . . ? N12 C72 C22 118.1(6) . . ? N12 C72 C82 121.2(5) . . ? C22 C72 C82 120.3(6) . . ? C92 C82 C72 110.3(4) . . ? C92 C82 H82A 109.6 . . ? C72 C82 H82A 109.6 . . ? C92 C82 H82B 109.6 . . ? C72 C82 H82B 109.6 . . ? H82A C82 H82B 108.1 . . ? C82 C92 H92A 109.5 . . ? C82 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C82 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C13 O13 Mn3 124.0(4) . . ? N13 O23 Mn5 119.1(3) . . ? C73 N13 O23 117.2(5) . . ? C73 N13 Mn3 127.6(5) . . ? O23 N13 Mn3 114.6(4) . . ? O13 C13 C23 124.0(7) . . ? O13 C13 C63 117.3(7) . . ? C23 C13 C63 118.6(7) . . ? C33 C23 C13 117.4(7) . . ? C33 C23 C73 119.8(8) . . ? C13 C23 C73 122.6(7) . . ? C23 C33 C43 122.0(8) . . ? C23 C33 H33 119.0 . . ? C43 C33 H33 119.0 . . ? C53 C43 C33 120.3(8) . . ? C53 C43 H43 119.9 . . ? C33 C43 H43 119.9 . . ? C63 C53 C43 118.0(8) . . ? C63 C53 H53 121.0 . . ? C43 C53 H53 121.0 . . ? C53 C63 C13 123.4(8) . . ? C53 C63 H63 118.3 . . ? C13 C63 H63 118.3 . . ? N13 C73 C23 119.1(6) . . ? N13 C73 C83 117.7(6) . . ? C23 C73 C83 123.2(6) . . ? C73 C83 C93 108.1(6) . . ? C73 C83 H83A 110.1 . . ? C93 C83 H83A 110.1 . . ? C73 C83 H83B 110.1 . . ? C93 C83 H83B 110.1 . . ? H83A C83 H83B 108.4 . . ? C83 C93 H93A 109.5 . . ? C83 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C83 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C14 O14 Mn4 121.8(4) . . ? N14 O24 Mn1 112.7(3) . . ? C74 N14 O24 115.6(5) . . ? C74 N14 Mn4 129.9(5) . . ? O24 N14 Mn4 114.5(3) . . ? O14 C14 C24 124.5(6) . . ? O14 C14 C64 115.4(6) . . ? C24 C14 C64 120.0(6) . . ? C14 C24 C34 118.0(6) . . ? C14 C24 C74 122.9(6) . . ? C34 C24 C74 119.1(6) . . ? C44 C34 C24 121.6(7) . . ? C44 C34 H34 119.2 . . ? C24 C34 H34 119.2 . . ? C54 C44 C34 120.2(6) . . ? C54 C44 H44 119.9 . . ? C34 C44 H44 119.9 . . ? C44 C54 C64 119.5(7) . . ? C44 C54 H54 120.2 . . ? C64 C54 H54 120.2 . . ? C54 C64 C14 120.6(7) . . ? C54 C64 H64 119.7 . . ? C14 C64 H64 119.7 . . ? N14 C74 C84 122.1(6) . . ? N14 C74 C24 116.8(6) . . ? C84 C74 C24 120.9(5) . . ? C74 C84 C94 110.4(5) . . ? C74 C84 H84A 109.6 . . ? C94 C84 H84A 109.6 . . ? C74 C84 H84B 109.6 . . ? C94 C84 H84B 109.6 . . ? H84A C84 H84B 108.1 . . ? C84 C94 H94A 109.5 . . ? C84 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C84 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C15 O15 Mn5 125.7(4) . . ? N15 O25 Mn1 113.7(3) . . ? C75 N15 O25 116.5(5) . . ? C75 N15 Mn5 128.0(4) . . ? O25 N15 Mn5 115.5(3) . . ? O15 C15 C65 119.3(6) . . ? O15 C15 C25 123.6(5) . . ? C65 C15 C25 117.1(6) . . ? C35 C25 C15 118.2(5) . . ? C35 C25 C75 120.2(6) . . ? C15 C25 C75 121.6(6) . . ? C45 C35 C25 124.2(6) . . ? C45 C35 H35 117.9 . . ? C25 C35 H35 117.9 . . ? C35 C45 C55 117.9(6) . . ? C35 C45 H45 121.1 . . ? C55 C45 H45 121.1 . . ? C65 C55 C45 118.7(6) . . ? C65 C55 H55 120.7 . . ? C45 C55 H55 120.7 . . ? C55 C65 C15 123.9(7) . . ? C55 C65 H65 118.1 . . ? C15 C65 H65 118.1 . . ? N15 C75 C25 120.7(5) . . ? N15 C75 C85 117.1(5) . . ? C25 C75 C85 121.9(5) . . ? C75 C85 C95 110.0(6) . . ? C75 C85 H85A 109.7 . . ? C95 C85 H85A 109.7 . . ? C75 C85 H85B 109.7 . . ? C95 C85 H85B 109.7 . . ? H85A C85 H85B 108.2 . . ? C85 C95 H95A 109.5 . . ? C85 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C85 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C16 O16 Mn4 117.5(4) . . ? N16 O26 Mn2 113.4(3) . . ? C76 N16 O26 119.0(6) . . ? C76 N16 Mn4 125.1(5) . . ? O26 N16 Mn4 115.6(4) . . ? O16 C16 C66 119.8(6) . . ? O16 C16 C26 121.2(6) . . ? C66 C16 C26 118.8(7) . . ? C36 C26 C16 117.8(6) . . ? C36 C26 C76 120.7(7) . . ? C16 C26 C76 121.4(6) . . ? C46 C36 C26 123.4(7) . . ? C46 C36 H36 118.3 . . ? C26 C36 H36 118.3 . . ? C36 C46 C56 118.2(7) . . ? C36 C46 H46 120.9 . . ? C56 C46 H46 120.9 . . ? C66 C56 C46 120.6(7) . . ? C66 C56 H56 119.7 . . ? C46 C56 H56 119.7 . . ? C56 C66 C16 121.0(7) . . ? C56 C66 H66 119.5 . . ? C16 C66 H66 119.5 . . ? N16 C76 C26 118.9(7) . . ? N16 C76 C86 118.8(6) . . ? C26 C76 C86 121.6(7) . . ? C96 C86 C76 108.1(6) . . ? C96 C86 H86A 110.1 . . ? C76 C86 H86A 110.1 . . ? C96 C86 H86B 110.1 . . ? C76 C86 H86B 110.1 . . ? H86A C86 H86B 108.4 . . ? C86 C96 H96A 109.5 . . ? C86 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C86 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C17 O17 Mn3 134.3(4) . . ? C17 O27 Mn5 122.5(4) . . ? C27 N17 H17A 109.5 . . ? C27 N17 H17B 109.5 . . ? H17A N17 H17B 109.5 . . ? C27 N17 H17C 109.5 . . ? H17A N17 H17C 109.5 . . ? H17B N17 H17C 109.5 . . ? O17 C17 O27 127.5(6) . . ? O17 C17 C27 116.0(5) . . ? O27 C17 C27 116.4(6) . . ? N17 C27 C17 107.2(5) . . ? N17 C27 C37 110.4(5) . . ? C17 C27 C37 113.5(5) . . ? N17 C27 H27 108.5 . . ? C17 C27 H27 108.5 . . ? C37 C27 H27 108.5 . . ? C67 C37 C47 111.1(7) . . ? C67 C37 C27 107.4(7) . . ? C47 C37 C27 114.1(6) . . ? C67 C37 C57 98.7(10) . . ? C47 C37 C57 117.3(7) . . ? C27 C37 C57 106.9(6) . . ? C47 C37 H37A 111.8(8) . . ? C27 C37 H37A 101.5(6) . . ? C57 C37 H37A 103.7(7) . . ? C67 C37 H37B 104.2(10) . . ? C27 C37 H37B 104.8(6) . . ? H37A C37 H37B 109.1(8) . . ? C67 C37 H37C 121.9(8) . . ? C27 C37 H37C 108.0(6) . . ? C57 C37 H37C 112.9(7) . . ? H37A C37 H37C 122.5(9) . . ? H37B C37 H37C 109.3(8) . . ? C37 C47 H47A 109.5 . . ? H37C C47 H47A 118.9 . . ? C37 C47 H47B 109.5 . . ? H37C C47 H47B 94.4 . . ? H47A C47 H47B 109.5 . . ? C37 C47 H47C 109.5 . . ? H37C C47 H47C 113.9 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C37 C67 H67A 109.5 . . ? H37A C67 H67A 103.7 . . ? C37 C67 H67B 109.5 . . ? H37A C67 H67B 100.1 . . ? H67A C67 H67B 109.5 . . ? C37 C67 H67C 109.5 . . ? H37A C67 H67C 123.8 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C37 C57 H57A 109.5 . . ? H37B C57 H57A 112.2 . . ? C37 C57 H57B 109.5 . . ? H37B C57 H57B 100.9 . . ? H57A C57 H57B 109.5 . . ? C37 C57 H57C 109.5 . . ? H37B C57 H57C 114.9 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C28 N18 H18A 109.5 . . ? C28 N18 H18B 109.5 . . ? H18A N18 H18B 109.5 . . ? C28 N18 H18C 109.5 . . ? H18A N18 H18C 109.5 . . ? H18B N18 H18C 109.5 . . ? O18 C18 O28 126.1(6) . . ? O18 C18 C28 117.4(5) . . ? O28 C18 C28 115.9(6) . . ? N18 C28 C38 113.8(5) . . ? N18 C28 C18 107.6(5) . . ? C38 C28 C18 116.3(5) . . ? N18 C28 H28A 106.1 . . ? C38 C28 H28A 106.1 . . ? C18 C28 H28A 106.1 . . ? C58 C38 C48 112.0(6) . . ? C58 C38 C28 107.1(6) . . ? C48 C38 C28 116.6(5) . . ? C58 C38 H38A 106.9 . . ? C48 C38 H38A 106.9 . . ? C28 C38 H38A 106.9 . . ? C38 C48 H48A 109.5 . . ? C38 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C38 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C38 C58 H58A 109.5 . . ? C38 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C38 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C19 O19 Mn2 119.3(3) . . ? C19 O19 Mn3 118.4(3) . . ? Mn2 O19 Mn3 107.87(19) . . ? O19 C19 H19A 109.5 . . ? O19 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O19 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? H1W1 O1W H2W1 117.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 C11 C21 C31 -179.6(5) . . . . ? C61 C11 C21 C31 3.7(9) . . . . ? O11 C11 C21 C71 3.6(9) . . . . ? C61 C11 C21 C71 -173.1(6) . . . . ? C11 C21 C31 C41 -2.7(9) . . . . ? C71 C21 C31 C41 174.2(6) . . . . ? C21 C31 C41 C51 1.2(10) . . . . ? C31 C41 C51 C61 -0.8(12) . . . . ? C41 C51 C61 C11 2.0(12) . . . . ? O11 C11 C61 C51 179.8(6) . . . . ? C21 C11 C61 C51 -3.4(10) . . . . ? O21 N11 C71 C21 168.1(4) . . . . ? O21 N11 C71 C81 -7.2(9) . . . . ? C31 C21 C71 N11 161.6(6) . . . . ? C11 C21 C71 N11 -21.6(9) . . . . ? C31 C21 C71 C81 -23.3(9) . . . . ? C11 C21 C71 C81 153.5(6) . . . . ? N11 C71 C81 C91 107.2(7) . . . . ? C21 C71 C81 C91 -67.9(8) . . . . ? O12 C12 C22 C32 177.2(5) . . . . ? C62 C12 C22 C32 -4.4(8) . . . . ? O12 C12 C22 C72 -2.0(9) . . . . ? C62 C12 C22 C72 176.4(5) . . . . ? C12 C22 C32 C42 5.1(9) . . . . ? C72 C22 C32 C42 -175.7(5) . . . . ? C22 C32 C42 C52 -3.9(9) . . . . ? C32 C42 C52 C62 2.2(10) . . . . ? C42 C52 C62 C12 -1.7(11) . . . . ? O12 C12 C62 C52 -178.6(6) . . . . ? C22 C12 C62 C52 2.9(9) . . . . ? O22 N12 C72 C22 176.5(4) . . . . ? O22 N12 C72 C82 -10.0(7) . . . . ? C12 C22 C72 N12 -18.5(8) . . . . ? C32 C22 C72 N12 162.3(5) . . . . ? C12 C22 C72 C82 167.9(5) . . . . ? C32 C22 C72 C82 -11.2(8) . . . . ? N12 C72 C82 C92 -78.9(7) . . . . ? C22 C72 C82 C92 94.4(6) . . . . ? O13 C13 C23 C33 -180.0(6) . . . . ? C63 C13 C23 C33 -3.0(10) . . . . ? O13 C13 C23 C73 -4.3(10) . . . . ? C63 C13 C23 C73 172.7(5) . . . . ? C13 C23 C33 C43 0.2(11) . . . . ? C73 C23 C33 C43 -175.6(6) . . . . ? C23 C33 C43 C53 4.2(12) . . . . ? C33 C43 C53 C63 -5.7(12) . . . . ? C43 C53 C63 C13 2.9(12) . . . . ? O13 C13 C63 C53 178.7(7) . . . . ? C23 C13 C63 C53 1.4(11) . . . . ? O23 N13 C73 C23 -173.9(5) . . . . ? O23 N13 C73 C83 4.5(8) . . . . ? C33 C23 C73 N13 -162.4(6) . . . . ? C13 C23 C73 N13 22.0(9) . . . . ? C33 C23 C73 C83 19.4(10) . . . . ? C13 C23 C73 C83 -156.3(6) . . . . ? N13 C73 C83 C93 -90.7(8) . . . . ? C23 C73 C83 C93 87.6(8) . . . . ? O14 C14 C24 C34 -178.9(6) . . . . ? C64 C14 C24 C34 -1.6(9) . . . . ? O14 C14 C24 C74 0.9(10) . . . . ? C64 C14 C24 C74 178.1(6) . . . . ? C14 C24 C34 C44 0.0(10) . . . . ? C74 C24 C34 C44 -179.7(6) . . . . ? C24 C34 C44 C54 1.3(11) . . . . ? C34 C44 C54 C64 -1.0(11) . . . . ? C44 C54 C64 C14 -0.6(10) . . . . ? O14 C14 C64 C54 179.5(6) . . . . ? C24 C14 C64 C54 2.0(10) . . . . ? O24 N14 C74 C84 0.4(8) . . . . ? O24 N14 C74 C24 -175.5(4) . . . . ? C14 C24 C74 N14 16.9(9) . . . . ? C34 C24 C74 N14 -163.4(6) . . . . ? C14 C24 C74 C84 -159.1(6) . . . . ? C34 C24 C74 C84 20.7(9) . . . . ? N14 C74 C84 C94 -93.6(7) . . . . ? C24 C74 C84 C94 82.1(7) . . . . ? O15 C15 C25 C35 178.0(6) . . . . ? C65 C15 C25 C35 1.7(9) . . . . ? O15 C15 C25 C75 -0.1(10) . . . . ? C65 C15 C25 C75 -176.4(6) . . . . ? C15 C25 C35 C45 -1.8(10) . . . . ? C75 C25 C35 C45 176.4(6) . . . . ? C25 C35 C45 C55 1.5(10) . . . . ? C35 C45 C55 C65 -1.0(10) . . . . ? C45 C55 C65 C15 1.1(11) . . . . ? O15 C15 C65 C55 -177.9(7) . . . . ? C25 C15 C65 C55 -1.4(10) . . . . ? O25 N15 C75 C25 177.2(5) . . . . ? O25 N15 C75 C85 2.8(8) . . . . ? C35 C25 C75 N15 165.8(6) . . . . ? C15 C25 C75 N15 -16.1(9) . . . . ? C35 C25 C75 C85 -20.1(9) . . . . ? C15 C25 C75 C85 158.1(6) . . . . ? N15 C75 C85 C95 83.1(7) . . . . ? C25 C75 C85 C95 -91.2(7) . . . . ? O16 C16 C26 C36 -179.2(5) . . . . ? C66 C16 C26 C36 -3.7(8) . . . . ? O16 C16 C26 C76 -4.0(9) . . . . ? C66 C16 C26 C76 171.5(5) . . . . ? C16 C26 C36 C46 2.4(10) . . . . ? C76 C26 C36 C46 -172.8(6) . . . . ? C26 C36 C46 C56 0.1(10) . . . . ? C36 C46 C56 C66 -1.2(10) . . . . ? C46 C56 C66 C16 -0.2(10) . . . . ? O16 C16 C66 C56 178.3(6) . . . . ? C26 C16 C66 C56 2.7(9) . . . . ? O26 N16 C76 C26 -169.2(4) . . . . ? O26 N16 C76 C86 1.3(8) . . . . ? C36 C26 C76 N16 -159.6(6) . . . . ? C16 C26 C76 N16 25.3(8) . . . . ? C36 C26 C76 C86 30.2(9) . . . . ? C16 C26 C76 C86 -144.9(6) . . . . ? N16 C76 C86 C96 84.8(7) . . . . ? C26 C76 C86 C96 -104.9(7) . . . . ? O17 C17 C27 N17 23.5(7) . . . . ? O27 C17 C27 N17 -160.0(5) . . . . ? O17 C17 C27 C37 -98.7(7) . . . . ? O27 C17 C27 C37 77.8(7) . . . . ? N17 C27 C37 C67 178.6(9) . . . . ? C17 C27 C37 C67 -61.0(10) . . . . ? N17 C27 C37 C47 -57.8(8) . . . . ? C17 C27 C37 C47 62.6(8) . . . . ? N17 C27 C37 C57 73.5(7) . . . . ? C17 C27 C37 C57 -166.1(6) . . . . ? O18 C18 C28 N18 -53.3(8) . . . . ? O28 C18 C28 N18 135.3(7) . . . . ? O18 C18 C28 C38 75.6(8) . . . . ? O28 C18 C28 C38 -95.8(8) . . . . ? N18 C28 C38 C58 -170.5(6) . . . . ? C18 C28 C38 C58 63.7(7) . . . . ? N18 C28 C38 C48 63.2(8) . . . . ? C18 C28 C38 C48 -62.7(8) . . . . ? 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 N17 H17A O1W 0.91 2.14 3.017(7) 162.4 . N17 H17B O28 0.91 1.81 2.647(7) 152.2 3_566 N17 H17C O18 0.91 1.97 2.761(7) 144.1 . N18 H18A O25 0.91 2.22 2.963(6) 138.7 . N18 H18A O16 0.91 2.33 3.021(6) 132.3 . N18 H18B O27 0.91 2.40 3.279(6) 163.5 . N18 H18C O19 0.91 2.15 3.015(6) 159.3 . N18 H18C O1 0.91 2.38 2.881(6) 114.8 . O1W H1W1 O13 0.82 2.06 2.871(7) 167.5 . O1W H2W1 O2W 0.82 2.11 2.888(12) 158.0 3_566 O1W H1W1 O13 0.82 2.06 2.871(7) 167.5 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.750 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.083 _vrf_PLAT220_xc31grap ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.94 Ratio RESPONSE: The terminal C and H atoms of coordinated valine molecule are partially disordered and therefore have larger temperature factors than other atoms. ; _vrf_PLAT222_xc31grap ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.88 Ratio RESPONSE: The terminal C and H atoms of coordinated valine molecule are partially disordered and therefore have larger temperature factors than other atoms. ; _vrf_PLAT601_xc31grap ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 392.00 A**3 RESPONSE: Probably part of solvent molecules (C2H5OH and water) leave from the crystal ; _vrf_PLAT026_xc31grap ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 33 Perc. RESPONSE: Poor diffraction of the crystal ; _vrf_PLAT430_xc31grap ; PROBLEM: Short Inter D...A Contact O2W .. O18 .. 2.75 Ang. RESPONSE: ; _vrf_PLAT231_xc31grap ; PROBLEM: Hirshfeld Test (Solvent) O28 -- C18 .. 13.01 su RESPONSE: ; # end Validation Reply Form