# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Mark Murrie' _publ_contact_author_email MARKM@CHEM.GLA.AC.UK _publ_section_title ; Pressure-induced Jahn-Teller switching in a Mn12 single-molecule magnet ; loop_ _publ_author_name 'Mark Murrie' 'Euan K. Brechin' 'Konstantin Kamenev' 'Alistair R Lennie' 'Stephen A Moggach' ; P.Parois ; 'Simon Parsons' 'Javier Sanchez-Benitez' 'John E. Warren' # Attachment 'all_revised.cif' data_sp8038 #TrackingRef 'all_revised.cif' _database_code_depnum_ccdc_archive 'CCDC 755025' #150K/ambient pressure structure _audit_creation_method SHELXL-97 _audit_creation_date 09-06-12 _chemical_compound_source 'Mark Murrie & Pascal Parois, Glasgow University ' _exptl_crystal_recrystallization_method ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn12O12(tBuCH2CO2)16(H2O)4].MeNO2.0.85CH2Cl2' _chemical_formula_sum 'C97.85 H188.70 Cl1.70 Mn12 N O50' _chemical_formula_weight 2898.94 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.8368(4) _cell_length_b 16.4179(5) _cell_length_c 27.3955(7) _cell_angle_alpha 76.817(2) _cell_angle_beta 78.1610(10) _cell_angle_gamma 78.264(2) _cell_volume 6695.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _cell_measurement_reflns_used 9917 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3023 _exptl_absorpt_coefficient_mu 1.203 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_T_max 0.663 _exptl_absorpt_process_details 'Sadabs scaled by 0.89' _exptl_special_details ; Oxford Cryosystems LT device. ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 52152 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.43 _reflns_number_total 26597 _reflns_number_gt 20068 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.229 0.695 0.364 112 30 ' ' 2 0.176 0.962 -0.004 50 4 ' ' 3 0.457 0.710 0.498 45 2 ' ' 4 0.543 0.290 0.502 45 2 ' ' 5 0.771 0.305 0.636 112 30 ' ' 6 0.824 0.038 1.004 50 4 ' ' _platon_squeeze_details ; 0.85CH2Cl2 = 71 electrons ; _refine_special_details ; H-atoms on the water ligands were located in a difference map. The H2O geometry was idealised, and the H-atoms then allowed to ride on their parent O-atoms. In O121 one of the H-atoms is modelled as disordered over two possible sites. A disordered CH2Cl2 molecule was treated with the squeeze procedure. The formula, M, mu etc have been calculated taking this into account. Checkcif output: 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.90 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.50 Ratio 213_ALERT_2_C Atom C512 has ADP max/min Ratio ............. 3.30 prola 220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.65 Ratio 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C312 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C38 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C310 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C212 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C33 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C35 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C36 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C315 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C317 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C318 230_ALERT_2_C Hirshfeld Test Diff for O210 -- C110 .. 6.93 su 230_ALERT_2_C Hirshfeld Test Diff for C315 -- C415 .. 5.57 su 232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn8 -- O25 .. 7.20 su 234_ALERT_4_C Large Hirshfeld Difference C312 -- C512 .. 0.18 Ang. 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbours of N1A The tBu groups show some libration, in some cases diagonalised Uij components reach ca 0.3 Ang**2. At this level experience suggests that there is little point attempting to model disorder, and alternative positions are effectively modelled by the adps. Note that 'pivot' C- atoms of tBu groups will temnd to have smaller adps than the methyl groups. 420_ALERT_2_B D-H Without Acceptor O10 - H101 ... ? 420_ALERT_2_B D-H Without Acceptor O120 - H121 ... ? 420_ALERT_2_B D-H Without Acceptor O121 - *H124 ... ? 420_ALERT_2_B D-H Without Acceptor O121 - *H125 ... ? H-atoms located in a difference map - see above. All waters make at least one H-bond. 910_ALERT_3_B Missing # of FCF Reflections Below Th(Min) ..... 14 029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 646 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 5 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 303 Coverage stats: #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.985 14038 13830 208 23.01 0.550 0.981 18683 18327 356 25.24 0.600 0.973 24220 23560 660 #----------------------------------------------------------- ACTA Min. Res. --- 26.43 0.626 0.965 27560 26597 963 Some strong reflections were obscured by the beam stop and were omitted. 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 7 Not that bad given the size and thermal motion of the structure! 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? No action 063_ALERT_4_B Crystal Size Likely too Large for Beam Size .... 0.66 mm Gorbitz has shown that use of a large crystal does not appear to matter. See C. H. Gorbitz Acta Cryst. (1999). B55, 1090-1098 041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? 042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ? 043_ALERT_1_C Check Reported Molecular Weight ................ 2898.94 044_ALERT_1_C Calculated and Reported Dx Differ .............. ? 051_ALERT_1_C Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 2.87 Perc. 068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? 605_ALERT_4_G Structure Contains Solvent Accessible VOIDS of . 113.00 A**3 Symptoms of Squeeze being used. See above. 125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 3 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? 795_ALERT_4_G C-Atom in CIF Coordinate List out of Sequence .. C14 796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence .. O107 No action. ; _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^)+(0.0740P)^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/difmap _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26597 _refine_ls_number_parameters 1442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1451 _refine_ls_wR_factor_gt 0.1346 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.42239(3) 0.19862(4) 0.231918(18) 0.02024(12) Uani 1 1 d . . . Mn2 Mn 0.29896(3) 0.08530(4) 0.262539(18) 0.02301(13) Uani 1 1 d . . . Mn3 Mn 0.25617(3) 0.23769(4) 0.193387(17) 0.02028(12) Uani 1 1 d . . . Mn4 Mn 0.26098(3) 0.25106(4) 0.292915(18) 0.02453(13) Uani 1 1 d . . . Mn5 Mn 0.23981(3) 0.40663(5) 0.32269(2) 0.03388(16) Uani 1 1 d . . . Mn6 Mn 0.43951(3) 0.29799(4) 0.32636(2) 0.03003(15) Uani 1 1 d . . . Mn7 Mn 0.58747(3) 0.16364(4) 0.259644(19) 0.02365(13) Uani 1 1 d . . . Mn8 Mn 0.52240(3) -0.01141(4) 0.24667(2) 0.02526(13) Uani 1 1 d . . . Mn9 Mn 0.33227(3) -0.07285(4) 0.23968(2) 0.02681(13) Uani 1 1 d . . . Mn10 Mn 0.17881(3) 0.06639(4) 0.176085(18) 0.02183(12) Uani 1 1 d . . . Mn11 Mn 0.09475(3) 0.27154(4) 0.161621(18) 0.02119(12) Uani 1 1 d . . . Mn12 Mn 0.11954(3) 0.40902(4) 0.232105(19) 0.02424(13) Uani 1 1 d . . . O6 O 0.42181(17) 0.1748(2) 0.38081(10) 0.0448(8) Uani 1 1 d . . . H61 H 0.4740 0.1456 0.3794 0.067 Uiso 1 1 d R . . H62 H 0.3901 0.1551 0.3704 0.067 Uiso 1 1 d R . . O10 O 0.29462(17) 0.0520(2) 0.11303(10) 0.0516(9) Uani 1 1 d . . . H101 H 0.3053 0.1008 0.1111 0.077 Uiso 1 1 d R . . H102 H 0.3363 0.0188 0.1252 0.077 Uiso 1 1 d R . . O120 O 0.00765(15) 0.34653(18) 0.28016(9) 0.0327(6) Uani 1 1 d . . . H120 H 0.0030 0.3033 0.2701 0.049 Uiso 1 1 d R . . H121 H 0.0264 0.3278 0.3078 0.049 Uiso 1 1 d R . . O121 O 0.23149(17) 0.4701(2) 0.18741(10) 0.0400(7) Uani 1 1 d . . . H123 H 0.2699 0.4848 0.2023 0.060 Uiso 1 1 d R . . H124 H 0.2697 0.4313 0.1705 0.060 Uiso 0.50 1 d PR . . H125 H 0.2036 0.4991 0.1745 0.060 Uiso 0.50 1 d PR . . O107 O 0.48184(14) 0.24302(16) 0.27009(8) 0.0244(5) Uani 1 1 d . . . O108 O 0.51437(13) 0.10768(16) 0.23652(8) 0.0224(5) Uani 1 1 d . . . O123 O 0.35348(13) 0.14827(15) 0.20029(8) 0.0198(5) Uani 1 1 d . . . O124 O 0.35086(13) 0.15301(17) 0.29345(8) 0.0243(6) Uani 1 1 d . . . O134 O 0.32251(13) 0.28626(16) 0.22705(8) 0.0219(5) Uani 1 1 d . . . O208 O 0.38928(15) -0.00474(16) 0.26313(9) 0.0262(6) Uani 1 1 d . . . O209 O 0.25119(14) 0.02821(16) 0.22626(8) 0.0240(5) Uani 1 1 d . . . O234 O 0.21107(14) 0.18637(17) 0.26011(8) 0.0245(6) Uani 1 1 d . . . O310 O 0.19034(13) 0.18126(15) 0.16670(8) 0.0210(5) Uani 1 1 d . . . O311 O 0.15685(14) 0.32169(16) 0.19579(8) 0.0232(5) Uani 1 1 d . . . O405 O 0.18407(14) 0.35499(17) 0.28458(8) 0.0264(6) Uani 1 1 d . . . O406 O 0.32191(14) 0.30794(18) 0.32180(9) 0.0301(6) Uani 1 1 d . . . O13 O 0.54021(16) -0.13512(18) 0.25372(10) 0.0355(6) Uani 1 1 d . . . O23 O 0.41237(17) -0.17751(17) 0.25896(10) 0.0371(7) Uani 1 1 d . . . C13 C 0.4929(3) -0.1911(3) 0.26138(14) 0.0319(9) Uani 1 1 d . . . C23 C 0.5351(3) -0.2827(3) 0.27307(17) 0.0445(11) Uani 1 1 d . . . H23A H 0.5737 -0.2963 0.2426 0.053 Uiso 1 1 calc R . . H23B H 0.4895 -0.3175 0.2807 0.053 Uiso 1 1 calc R . . C33 C 0.5875(3) -0.3082(3) 0.31674(17) 0.0483(12) Uani 1 1 d . . . C43 C 0.6060(4) -0.4047(3) 0.3290(2) 0.0693(16) Uani 1 1 d . . . H43A H 0.5517 -0.4263 0.3380 0.104 Uiso 1 1 calc R . . H43B H 0.6376 -0.4233 0.3570 0.104 Uiso 1 1 calc R . . H43C H 0.6403 -0.4255 0.2998 0.104 Uiso 1 1 calc R . . C53 C 0.5332(4) -0.2749(4) 0.36318(19) 0.0744(17) Uani 1 1 d . . . H53A H 0.5208 -0.2141 0.3551 0.112 Uiso 1 1 calc R . . H53B H 0.5653 -0.2925 0.3910 0.112 Uiso 1 1 calc R . . H53C H 0.4793 -0.2971 0.3726 0.112 Uiso 1 1 calc R . . C63 C 0.6727(3) -0.2725(4) 0.3023(2) 0.0712(17) Uani 1 1 d . . . H63A H 0.6600 -0.2117 0.2947 0.107 Uiso 1 1 calc R . . H63B H 0.7071 -0.2927 0.2729 0.107 Uiso 1 1 calc R . . H63C H 0.7048 -0.2906 0.3301 0.107 Uiso 1 1 calc R . . O14 O 0.53285(16) -0.00612(18) 0.17348(9) 0.0318(6) Uani 1 1 d . . . O24 O 0.41567(15) -0.05384(16) 0.16417(9) 0.0283(6) Uani 1 1 d . . . C14 C 0.4896(2) -0.0313(2) 0.14812(13) 0.0244(8) Uani 1 1 d . . . C24 C 0.5302(2) -0.0317(2) 0.09307(13) 0.0293(8) Uani 1 1 d . . . H24A H 0.5836 -0.0077 0.0859 0.035 Uiso 1 1 calc R . . H24B H 0.4904 0.0050 0.0717 0.035 Uiso 1 1 calc R . . C34 C 0.5520(2) -0.1202(3) 0.07836(14) 0.0307(9) Uani 1 1 d . . . C44 C 0.6054(3) -0.1833(3) 0.11523(17) 0.0468(11) Uani 1 1 d . . . H44A H 0.5713 -0.1902 0.1488 0.070 Uiso 1 1 calc R . . H44B H 0.6577 -0.1626 0.1155 0.070 Uiso 1 1 calc R . . H44C H 0.6207 -0.2370 0.1046 0.070 Uiso 1 1 calc R . . C54 C 0.6079(3) -0.1089(3) 0.02526(15) 0.0441(11) Uani 1 1 d . . . H54A H 0.5751 -0.0687 0.0018 0.066 Uiso 1 1 calc R . . H54B H 0.6235 -0.1623 0.0144 0.066 Uiso 1 1 calc R . . H54C H 0.6600 -0.0884 0.0263 0.066 Uiso 1 1 calc R . . C64 C 0.4691(3) -0.1524(3) 0.07609(17) 0.0433(11) Uani 1 1 d . . . H64A H 0.4363 -0.1116 0.0529 0.065 Uiso 1 1 calc R . . H64B H 0.4340 -0.1604 0.1093 0.065 Uiso 1 1 calc R . . H64C H 0.4848 -0.2054 0.0647 0.065 Uiso 1 1 calc R . . O15 O 0.69662(15) 0.09330(18) 0.24045(10) 0.0336(6) Uani 1 1 d . . . O25 O 0.66242(17) -0.02527(19) 0.23055(11) 0.0425(7) Uani 1 1 d . . . C15 C 0.7136(2) 0.0270(3) 0.22270(15) 0.0340(9) Uani 1 1 d . . . C25 C 0.8025(3) 0.0145(3) 0.18872(17) 0.0414(10) Uani 1 1 d . . . H25A H 0.7972 0.0507 0.1558 0.050 Uiso 1 1 calc R . . H25B H 0.8433 0.0354 0.2030 0.050 Uiso 1 1 calc R . . C35 C 0.8440(3) -0.0742(3) 0.17970(16) 0.0397(10) Uani 1 1 d . . . C45 C 0.7894(3) -0.1079(4) 0.1522(2) 0.0617(15) Uani 1 1 d . . . H45A H 0.8170 -0.1637 0.1470 0.093 Uiso 1 1 calc R . . H45B H 0.7842 -0.0711 0.1199 0.093 Uiso 1 1 calc R . . H45C H 0.7323 -0.1105 0.1722 0.093 Uiso 1 1 calc R . . C55 C 0.9342(3) -0.0664(4) 0.1463(2) 0.0651(15) Uani 1 1 d . . . H55A H 0.9692 -0.0449 0.1637 0.098 Uiso 1 1 calc R . . H55B H 0.9267 -0.0282 0.1147 0.098 Uiso 1 1 calc R . . H55C H 0.9629 -0.1212 0.1398 0.098 Uiso 1 1 calc R . . C65 C 0.8597(3) -0.1323(3) 0.2289(2) 0.0646(15) Uani 1 1 d . . . H65A H 0.8949 -0.1089 0.2451 0.097 Uiso 1 1 calc R . . H65B H 0.8894 -0.1868 0.2224 0.097 Uiso 1 1 calc R . . H65C H 0.8047 -0.1384 0.2508 0.097 Uiso 1 1 calc R . . O16 O 0.56712(16) 0.08022(18) 0.33475(9) 0.0324(6) Uani 1 1 d . . . O26 O 0.52950(17) -0.03441(18) 0.31909(10) 0.0363(7) Uani 1 1 d . . . C16 C 0.5484(2) 0.0077(3) 0.34815(14) 0.0322(9) Uani 1 1 d . . . C26 C 0.5471(2) -0.0373(3) 0.40313(14) 0.0388(10) Uani 1 1 d . . . H26A H 0.5219 -0.0884 0.4081 0.047 Uiso 1 1 calc R . . H26B H 0.5087 -0.0009 0.4247 0.047 Uiso 1 1 calc R . . C36 C 0.6361(3) -0.0621(3) 0.42095(15) 0.0375(10) Uani 1 1 d . . . C46 C 0.6209(4) -0.1140(4) 0.47495(18) 0.0658(15) Uani 1 1 d . . . H46A H 0.5801 -0.0802 0.4965 0.099 Uiso 1 1 calc R . . H46B H 0.6753 -0.1309 0.4876 0.099 Uiso 1 1 calc R . . H46C H 0.5977 -0.1635 0.4746 0.099 Uiso 1 1 calc R . . C56 C 0.6999(3) -0.1153(3) 0.3868(2) 0.0607(14) Uani 1 1 d . . . H56A H 0.6764 -0.1646 0.3865 0.091 Uiso 1 1 calc R . . H56B H 0.7545 -0.1325 0.3993 0.091 Uiso 1 1 calc R . . H56C H 0.7093 -0.0826 0.3529 0.091 Uiso 1 1 calc R . . C66 C 0.6726(3) 0.0160(3) 0.42176(18) 0.0496(12) Uani 1 1 d . . . H66A H 0.6316 0.0496 0.4434 0.074 Uiso 1 1 calc R . . H66B H 0.6823 0.0489 0.3879 0.074 Uiso 1 1 calc R . . H66C H 0.7269 -0.0010 0.4345 0.074 Uiso 1 1 calc R . . O17 O 0.47685(14) 0.25254(16) 0.16758(8) 0.0237(5) Uani 1 1 d . . . O27 O 0.61463(14) 0.23493(17) 0.18165(9) 0.0271(6) Uani 1 1 d . . . C17 C 0.5588(2) 0.2573(2) 0.15348(13) 0.0233(7) Uani 1 1 d . . . C27 C 0.5847(2) 0.2923(2) 0.09759(12) 0.0264(8) Uani 1 1 d . . . H27A H 0.6385 0.3149 0.0927 0.032 Uiso 1 1 calc R . . H27B H 0.5397 0.3389 0.0869 0.032 Uiso 1 1 calc R . . C37 C 0.5981(2) 0.2263(3) 0.06341(13) 0.0275(8) Uani 1 1 d . . . C47 C 0.6324(3) 0.2683(3) 0.00916(16) 0.0521(13) Uani 1 1 d . . . H47A H 0.5907 0.3169 -0.0020 0.078 Uiso 1 1 calc R . . H47B H 0.6411 0.2286 -0.0130 0.078 Uiso 1 1 calc R . . H47C H 0.6870 0.2860 0.0083 0.078 Uiso 1 1 calc R . . C57 C 0.5122(2) 0.1977(3) 0.06418(15) 0.0354(9) Uani 1 1 d . . . H57A H 0.4903 0.1711 0.0982 0.053 Uiso 1 1 calc R . . H57B H 0.5218 0.1580 0.0420 0.053 Uiso 1 1 calc R . . H57C H 0.4704 0.2460 0.0529 0.053 Uiso 1 1 calc R . . C67 C 0.6651(3) 0.1491(3) 0.08066(17) 0.0428(10) Uani 1 1 d . . . H67A H 0.6444 0.1228 0.1149 0.064 Uiso 1 1 calc R . . H67B H 0.7198 0.1669 0.0792 0.064 Uiso 1 1 calc R . . H67C H 0.6730 0.1093 0.0587 0.064 Uiso 1 1 calc R . . O18 O 0.55675(16) 0.2860(2) 0.33979(10) 0.0458(8) Uani 1 1 d . . . O28 O 0.65715(15) 0.2305(2) 0.28142(10) 0.0370(7) Uani 1 1 d . . . C18 C 0.6316(2) 0.2805(3) 0.31240(16) 0.0426(11) Uani 1 1 d . . . C28 C 0.6930(3) 0.3367(3) 0.31717(17) 0.0489(12) Uani 1 1 d . . . H28A H 0.6683 0.3953 0.3054 0.059 Uiso 1 1 calc R . . H28B H 0.7481 0.3241 0.2949 0.059 Uiso 1 1 calc R . . C38 C 0.7113(3) 0.3271(3) 0.37092(16) 0.0393(10) Uani 1 1 d . . . C48 C 0.6327(4) 0.3585(5) 0.4065(2) 0.086(2) Uani 1 1 d . . . H48A H 0.6103 0.4163 0.3929 0.129 Uiso 1 1 calc R . . H48B H 0.6488 0.3553 0.4389 0.129 Uiso 1 1 calc R . . H48C H 0.5885 0.3240 0.4107 0.129 Uiso 1 1 calc R . . C58 C 0.7816(3) 0.3836(4) 0.3663(2) 0.0716(17) Uani 1 1 d . . . H58A H 0.7576 0.4420 0.3553 0.107 Uiso 1 1 calc R . . H58B H 0.8316 0.3671 0.3420 0.107 Uiso 1 1 calc R . . H58C H 0.7990 0.3764 0.3988 0.107 Uiso 1 1 calc R . . C68 C 0.7524(6) 0.2382(4) 0.3875(4) 0.141(4) Uani 1 1 d . . . H68A H 0.8021 0.2235 0.3626 0.212 Uiso 1 1 calc R . . H68B H 0.7107 0.2012 0.3911 0.212 Uiso 1 1 calc R . . H68C H 0.7709 0.2323 0.4195 0.212 Uiso 1 1 calc R . . O19 O 0.32031(15) 0.47699(19) 0.25924(10) 0.0367(7) Uani 1 1 d . . . O29 O 0.45011(16) 0.42051(19) 0.28292(10) 0.0372(7) Uani 1 1 d . . . C19 C 0.4013(2) 0.4760(3) 0.25741(16) 0.0361(10) Uani 1 1 d . . . C29 C 0.4429(3) 0.5473(3) 0.22255(18) 0.0422(11) Uani 1 1 d . . . H29A H 0.4779 0.5672 0.2412 0.051 Uiso 1 1 calc R . . H29B H 0.3968 0.5939 0.2133 0.051 Uiso 1 1 calc R . . C39 C 0.5015(3) 0.5249(3) 0.17319(18) 0.0427(11) Uani 1 1 d . . . C49 C 0.5296(3) 0.6073(3) 0.1419(2) 0.0625(15) Uani 1 1 d . . . H49A H 0.4787 0.6484 0.1351 0.094 Uiso 1 1 calc R . . H49B H 0.5652 0.5969 0.1104 0.094 Uiso 1 1 calc R . . H49C H 0.5626 0.6286 0.1606 0.094 Uiso 1 1 calc R . . C59 C 0.5824(3) 0.4603(3) 0.1846(2) 0.0590(14) Uani 1 1 d . . . H59A H 0.5648 0.4085 0.2046 0.089 Uiso 1 1 calc R . . H59B H 0.6150 0.4823 0.2031 0.089 Uiso 1 1 calc R . . H59C H 0.6183 0.4493 0.1533 0.089 Uiso 1 1 calc R . . C69 C 0.4498(3) 0.4906(3) 0.14376(18) 0.0510(12) Uani 1 1 d . . . H69A H 0.4319 0.4389 0.1637 0.076 Uiso 1 1 calc R . . H69B H 0.4858 0.4797 0.1124 0.076 Uiso 1 1 calc R . . H69C H 0.3991 0.5316 0.1366 0.076 Uiso 1 1 calc R . . O110 O 0.29072(17) 0.4513(2) 0.36805(12) 0.0523(9) Uani 1 1 d . . . O210 O 0.40710(17) 0.3506(2) 0.38640(10) 0.0478(9) Uani 1 1 d . . . C110 C 0.3531(3) 0.4186(4) 0.39230(16) 0.0550(15) Uani 1 1 d . . . C210 C 0.3650(3) 0.4650(4) 0.43234(17) 0.0545(13) Uani 1 1 d . . . H21A H 0.4246 0.4477 0.4390 0.065 Uiso 1 1 calc R . . H21B H 0.3568 0.5254 0.4187 0.065 Uiso 1 1 calc R . . C310 C 0.3038(4) 0.4487(4) 0.48117(17) 0.0594(14) Uani 1 1 d . . . C410 C 0.3267(4) 0.4861(4) 0.5211(2) 0.0792(19) Uani 1 1 d . . . H41A H 0.2862 0.4746 0.5521 0.119 Uiso 1 1 calc R . . H41B H 0.3233 0.5463 0.5097 0.119 Uiso 1 1 calc R . . H41C H 0.3850 0.4613 0.5269 0.119 Uiso 1 1 calc R . . C510 C 0.3168(8) 0.3529(5) 0.5015(3) 0.160(5) Uani 1 1 d . . . H51A H 0.2771 0.3406 0.5327 0.240 Uiso 1 1 calc R . . H51B H 0.3758 0.3333 0.5075 0.240 Uiso 1 1 calc R . . H51C H 0.3055 0.3247 0.4770 0.240 Uiso 1 1 calc R . . C610 C 0.2098(4) 0.4833(5) 0.4748(2) 0.096(2) Uani 1 1 d . . . H61A H 0.1723 0.4706 0.5069 0.143 Uiso 1 1 calc R . . H61B H 0.1944 0.4575 0.4504 0.143 Uiso 1 1 calc R . . H61C H 0.2032 0.5436 0.4631 0.143 Uiso 1 1 calc R . . O111 O 0.07393(16) 0.50741(18) 0.26336(10) 0.0352(6) Uani 1 1 d . . . O211 O 0.15155(16) 0.5073(2) 0.32280(11) 0.0474(8) Uani 1 1 d . . . C111 C 0.0907(2) 0.5393(3) 0.29776(14) 0.0332(9) Uani 1 1 d . . . C211 C 0.0344(2) 0.6191(3) 0.30938(15) 0.0381(10) Uani 1 1 d . . . H21C H 0.0072 0.6481 0.2801 0.046 Uiso 1 1 calc R . . H21D H 0.0709 0.6557 0.3150 0.046 Uiso 1 1 calc R . . C311 C -0.0378(2) 0.6053(3) 0.35628(17) 0.0432(11) Uani 1 1 d . . . C411 C -0.0899(3) 0.6932(3) 0.36190(19) 0.0581(14) Uani 1 1 d . . . H41D H -0.0515 0.7283 0.3663 0.087 Uiso 1 1 calc R . . H41E H -0.1354 0.6876 0.3910 0.087 Uiso 1 1 calc R . . H41F H -0.1153 0.7187 0.3319 0.087 Uiso 1 1 calc R . . C511 C 0.0021(3) 0.5647(4) 0.40409(18) 0.0604(14) Uani 1 1 d . . . H51D H 0.0407 0.5996 0.4085 0.091 Uiso 1 1 calc R . . H51E H 0.0344 0.5095 0.4007 0.091 Uiso 1 1 calc R . . H51F H -0.0436 0.5595 0.4331 0.091 Uiso 1 1 calc R . . C611 C -0.0981(3) 0.5498(4) 0.3484(2) 0.0710(17) Uani 1 1 d . . . H61D H -0.1220 0.5751 0.3179 0.107 Uiso 1 1 calc R . . H61E H -0.1448 0.5448 0.3769 0.107 Uiso 1 1 calc R . . H61F H -0.0656 0.4945 0.3454 0.107 Uiso 1 1 calc R . . O112 O 0.19650(15) 0.21054(19) 0.35844(9) 0.0354(7) Uani 1 1 d . . . O212 O 0.16798(18) 0.3309(3) 0.38960(10) 0.0475(8) Uani 1 1 d . . . C112 C 0.1665(3) 0.2546(4) 0.39363(15) 0.0466(13) Uani 1 1 d . . . C212 C 0.1299(3) 0.2037(4) 0.44405(16) 0.0696(18) Uani 1 1 d . . . H21E H 0.1281 0.1477 0.4387 0.084 Uiso 1 1 calc R . . H21F H 0.1712 0.1965 0.4670 0.084 Uiso 1 1 calc R . . C312 C 0.0411(3) 0.2367(3) 0.47094(16) 0.0451(11) Uani 1 1 d . . . C412 C -0.0221(4) 0.2604(6) 0.4348(3) 0.124(3) Uani 1 1 d . . . H41G H -0.0018 0.3019 0.4062 0.186 Uiso 1 1 calc R . . H41H H -0.0782 0.2837 0.4516 0.186 Uiso 1 1 calc R . . H41I H -0.0272 0.2110 0.4231 0.186 Uiso 1 1 calc R . . C512 C 0.0422(6) 0.3162(5) 0.4895(3) 0.145(4) Uani 1 1 d . . . H51G H 0.0601 0.3591 0.4611 0.218 Uiso 1 1 calc R . . H51H H 0.0826 0.3039 0.5130 0.218 Uiso 1 1 calc R . . H51I H -0.0153 0.3361 0.5062 0.218 Uiso 1 1 calc R . . C612 C 0.0116(4) 0.1711(4) 0.51584(19) 0.0744(18) Uani 1 1 d . . . H61G H 0.0533 0.1567 0.5387 0.112 Uiso 1 1 calc R . . H61H H 0.0072 0.1213 0.5044 0.112 Uiso 1 1 calc R . . H61I H -0.0445 0.1933 0.5332 0.112 Uiso 1 1 calc R . . O113 O 0.04554(15) 0.46933(17) 0.18230(9) 0.0295(6) Uani 1 1 d . . . O213 O 0.00156(15) 0.36901(17) 0.15433(9) 0.0287(6) Uani 1 1 d . . . C113 C -0.0026(2) 0.4448(3) 0.15897(13) 0.0259(8) Uani 1 1 d . . . C213 C -0.0701(2) 0.5107(3) 0.13443(14) 0.0310(9) Uani 1 1 d . . . H21G H -0.1019 0.4831 0.1181 0.037 Uiso 1 1 calc R . . H21H H -0.0403 0.5506 0.1081 0.037 Uiso 1 1 calc R . . C313 C -0.1363(2) 0.5607(3) 0.17101(15) 0.0340(9) Uani 1 1 d . . . C413 C -0.1726(3) 0.4999(3) 0.21774(17) 0.0485(12) Uani 1 1 d . . . H41J H -0.1979 0.4595 0.2074 0.073 Uiso 1 1 calc R . . H41K H -0.2166 0.5312 0.2392 0.073 Uiso 1 1 calc R . . H41L H -0.1262 0.4706 0.2361 0.073 Uiso 1 1 calc R . . C513 C -0.0964(3) 0.6245(3) 0.1872(2) 0.0522(12) Uani 1 1 d . . . H51J H -0.0741 0.6632 0.1576 0.078 Uiso 1 1 calc R . . H51K H -0.0495 0.5954 0.2052 0.078 Uiso 1 1 calc R . . H51L H -0.1402 0.6555 0.2089 0.078 Uiso 1 1 calc R . . C613 C -0.2120(3) 0.6081(3) 0.14255(18) 0.0451(11) Uani 1 1 d . . . H61J H -0.1898 0.6467 0.1130 0.068 Uiso 1 1 calc R . . H61K H -0.2553 0.6391 0.1646 0.068 Uiso 1 1 calc R . . H61L H -0.2379 0.5679 0.1324 0.068 Uiso 1 1 calc R . . O114 O 0.26539(16) -0.14179(18) 0.21757(10) 0.0352(6) Uani 1 1 d . . . O214 O 0.16179(16) -0.04912(17) 0.18091(10) 0.0314(6) Uani 1 1 d . . . C114 C 0.1960(2) -0.1224(3) 0.19897(13) 0.0267(8) Uani 1 1 d . . . C214 C 0.1505(2) -0.1932(3) 0.19706(14) 0.0324(9) Uani 1 1 d . . . H21I H 0.0885 -0.1716 0.1983 0.039 Uiso 1 1 calc R . . H21J H 0.1573 -0.2371 0.2271 0.039 Uiso 1 1 calc R . . C314 C 0.1843(2) -0.2337(3) 0.14940(17) 0.0384(10) Uani 1 1 d . . . C414 C 0.2758(3) -0.2857(3) 0.1512(3) 0.0720(18) Uani 1 1 d . . . H41M H 0.2744 -0.3292 0.1813 0.108 Uiso 1 1 calc R . . H41N H 0.3158 -0.2493 0.1516 0.108 Uiso 1 1 calc R . . H41O H 0.2944 -0.3114 0.1218 0.108 Uiso 1 1 calc R . . C514 C 0.1221(3) -0.2931(3) 0.1495(2) 0.0502(12) Uani 1 1 d . . . H51M H 0.1215 -0.3360 0.1798 0.075 Uiso 1 1 calc R . . H51N H 0.1412 -0.3193 0.1203 0.075 Uiso 1 1 calc R . . H51O H 0.0642 -0.2614 0.1483 0.075 Uiso 1 1 calc R . . C614 C 0.1862(3) -0.1646(3) 0.10138(16) 0.0489(12) Uani 1 1 d . . . H61M H 0.2257 -0.1276 0.1019 0.073 Uiso 1 1 calc R . . H61N H 0.1286 -0.1325 0.1001 0.073 Uiso 1 1 calc R . . H61O H 0.2056 -0.1903 0.0720 0.073 Uiso 1 1 calc R . . O115 O 0.23757(15) 0.0368(2) 0.32667(9) 0.0341(7) Uani 1 1 d . . . O215 O 0.25943(17) -0.0986(2) 0.31737(10) 0.0389(7) Uani 1 1 d . . . C115 C 0.2330(2) -0.0430(3) 0.34297(14) 0.0358(10) Uani 1 1 d . . . C215 C 0.1934(3) -0.0631(3) 0.39812(14) 0.0442(12) Uani 1 1 d . . . H21K H 0.1656 -0.1127 0.4040 0.053 Uiso 1 1 calc R . . H21L H 0.1482 -0.0161 0.4060 0.053 Uiso 1 1 calc R . . C315 C 0.2599(3) -0.0797(3) 0.43444(14) 0.0415(11) Uani 1 1 d . . . C415 C 0.3262(4) -0.1576(4) 0.4273(2) 0.083(2) Uani 1 1 d . . . H41P H 0.2968 -0.2054 0.4328 0.125 Uiso 1 1 calc R . . H41Q H 0.3657 -0.1681 0.4512 0.125 Uiso 1 1 calc R . . H41R H 0.3585 -0.1491 0.3933 0.125 Uiso 1 1 calc R . . C515 C 0.2077(4) -0.0898(5) 0.48844(16) 0.084(2) Uani 1 1 d . . . H51P H 0.1666 -0.0389 0.4920 0.127 Uiso 1 1 calc R . . H51Q H 0.2469 -0.1002 0.5125 0.127 Uiso 1 1 calc R . . H51R H 0.1768 -0.1367 0.4947 0.127 Uiso 1 1 calc R . . C615 C 0.3073(3) -0.0043(3) 0.42582(15) 0.0440(11) Uani 1 1 d . . . H61P H 0.2653 0.0456 0.4305 0.066 Uiso 1 1 calc R . . H61Q H 0.3394 0.0043 0.3918 0.066 Uiso 1 1 calc R . . H61R H 0.3469 -0.0152 0.4497 0.066 Uiso 1 1 calc R . . O116 O 0.06230(16) 0.08398(18) 0.22828(10) 0.0324(6) Uani 1 1 d . . . O216 O 0.01916(14) 0.21914(17) 0.23397(9) 0.0267(6) Uani 1 1 d . . . C116 C 0.0309(2) 0.1405(3) 0.25335(14) 0.0268(8) Uani 1 1 d . . . C216 C 0.0065(2) 0.1150(3) 0.31068(14) 0.0329(9) Uani 1 1 d . . . H21M H -0.0273 0.1642 0.3236 0.039 Uiso 1 1 calc R . . H21N H 0.0600 0.0997 0.3251 0.039 Uiso 1 1 calc R . . C316 C -0.0460(2) 0.0413(3) 0.33028(14) 0.0352(10) Uani 1 1 d . . . C416 C 0.0082(3) -0.0419(3) 0.32017(19) 0.0513(12) Uani 1 1 d . . . H41S H 0.0268 -0.0382 0.2842 0.077 Uiso 1 1 calc R . . H41T H -0.0263 -0.0864 0.3332 0.077 Uiso 1 1 calc R . . H41U H 0.0586 -0.0542 0.3367 0.077 Uiso 1 1 calc R . . C516 C -0.1265(3) 0.0609(4) 0.30477(17) 0.0541(13) Uani 1 1 d . . . H51S H -0.1606 0.1139 0.3113 0.081 Uiso 1 1 calc R . . H51T H -0.1610 0.0165 0.3181 0.081 Uiso 1 1 calc R . . H51U H -0.1086 0.0646 0.2688 0.081 Uiso 1 1 calc R . . C616 C -0.0741(3) 0.0343(4) 0.38749(16) 0.0571(14) Uani 1 1 d . . . H61S H -0.1082 0.0871 0.3944 0.086 Uiso 1 1 calc R . . H61T H -0.0233 0.0215 0.4036 0.086 Uiso 1 1 calc R . . H61U H -0.1087 -0.0101 0.4005 0.086 Uiso 1 1 calc R . . O117 O 0.11377(15) 0.09295(17) 0.11934(9) 0.0292(6) Uani 1 1 d . . . O217 O 0.03808(14) 0.22337(17) 0.12156(9) 0.0255(5) Uani 1 1 d . . . C117 C 0.0591(2) 0.1559(3) 0.10399(13) 0.0252(8) Uani 1 1 d . . . C217 C 0.0153(2) 0.1496(3) 0.06194(14) 0.0333(9) Uani 1 1 d . . . H21O H -0.0474 0.1655 0.0715 0.040 Uiso 1 1 calc R . . H21P H 0.0265 0.0910 0.0578 0.040 Uiso 1 1 calc R . . C317 C 0.0453(3) 0.2054(4) 0.01092(16) 0.0544(14) Uani 1 1 d . . . C417 C 0.0043(4) 0.1834(5) -0.0293(2) 0.089(2) Uani 1 1 d . . . H41V H 0.0216 0.2180 -0.0618 0.133 Uiso 1 1 calc R . . H41W H -0.0583 0.1937 -0.0203 0.133 Uiso 1 1 calc R . . H41X H 0.0238 0.1247 -0.0311 0.133 Uiso 1 1 calc R . . C517 C 0.1430(4) 0.1919(5) -0.0026(2) 0.092(2) Uani 1 1 d . . . H51V H 0.1599 0.2282 -0.0345 0.138 Uiso 1 1 calc R . . H51W H 0.1643 0.1338 -0.0055 0.138 Uiso 1 1 calc R . . H51X H 0.1674 0.2051 0.0234 0.138 Uiso 1 1 calc R . . C617 C 0.0129(4) 0.3011(4) 0.0121(2) 0.0794(19) Uani 1 1 d . . . H61V H 0.0328 0.3346 -0.0203 0.119 Uiso 1 1 calc R . . H61W H 0.0359 0.3160 0.0381 0.119 Uiso 1 1 calc R . . H61X H -0.0498 0.3117 0.0193 0.119 Uiso 1 1 calc R . . O118 O 0.30211(14) 0.29746(16) 0.12731(8) 0.0247(5) Uani 1 1 d . . . O218 O 0.17881(15) 0.32787(17) 0.09298(9) 0.0277(6) Uani 1 1 d . . . C118 C 0.2564(2) 0.3325(2) 0.09124(13) 0.0276(8) Uani 1 1 d . . . C218 C 0.3060(3) 0.3825(3) 0.04471(15) 0.0437(11) Uani 1 1 d . . . H21Q H 0.3578 0.3933 0.0542 0.052 Uiso 1 1 calc R . . H21R H 0.3257 0.3466 0.0196 0.052 Uiso 1 1 calc R . . C318 C 0.2592(3) 0.4661(3) 0.01934(15) 0.0386(10) Uani 1 1 d . . . C418 C 0.3262(4) 0.5088(4) -0.02167(19) 0.0671(16) Uani 1 1 d . . . H41Y H 0.2980 0.5620 -0.0387 0.101 Uiso 1 1 calc R . . H41Z H 0.3513 0.4727 -0.0458 0.101 Uiso 1 1 calc R . . H411 H 0.3716 0.5184 -0.0062 0.101 Uiso 1 1 calc R . . C518 C 0.1840(4) 0.4574(4) -0.0047(2) 0.080(2) Uani 1 1 d . . . H51Y H 0.1418 0.4305 0.0209 0.120 Uiso 1 1 calc R . . H51Z H 0.2059 0.4236 -0.0304 0.120 Uiso 1 1 calc R . . H511 H 0.1569 0.5126 -0.0199 0.120 Uiso 1 1 calc R . . C618 C 0.2235(4) 0.5237(3) 0.0578(2) 0.0717(17) Uani 1 1 d . . . H61Y H 0.1807 0.4985 0.0839 0.108 Uiso 1 1 calc R . . H61Z H 0.1968 0.5779 0.0410 0.108 Uiso 1 1 calc R . . H611 H 0.2705 0.5311 0.0728 0.108 Uiso 1 1 calc R . . N1A N 0.8080(2) 0.3007(3) 0.13352(15) 0.0444(9) Uani 1 1 d . . . C1A C 0.8255(3) 0.2533(3) 0.18430(18) 0.0518(12) Uani 1 1 d . . . H1A1 H 0.8474 0.2887 0.2006 0.078 Uiso 1 1 calc R . . H1A2 H 0.8681 0.2035 0.1806 0.078 Uiso 1 1 calc R . . H1A3 H 0.7723 0.2371 0.2046 0.078 Uiso 1 1 calc R . . O2A O 0.8160(2) 0.2610(3) 0.10032(15) 0.0791(13) Uani 1 1 d . . . O3A O 0.7857(2) 0.3755(3) 0.12852(17) 0.0747(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0145(2) 0.0348(3) 0.0140(2) -0.0088(2) -0.00167(18) -0.0063(2) Mn2 0.0186(2) 0.0395(4) 0.0132(2) -0.0032(2) -0.00404(19) -0.0105(2) Mn3 0.0154(2) 0.0346(3) 0.0127(2) -0.0063(2) -0.00186(18) -0.0072(2) Mn4 0.0156(2) 0.0469(4) 0.0136(2) -0.0107(2) -0.00059(18) -0.0073(2) Mn5 0.0185(3) 0.0630(5) 0.0281(3) -0.0292(3) -0.0031(2) -0.0025(3) Mn6 0.0176(2) 0.0569(4) 0.0228(3) -0.0222(3) -0.0039(2) -0.0055(3) Mn7 0.0159(2) 0.0366(3) 0.0227(3) -0.0120(2) -0.00471(19) -0.0054(2) Mn8 0.0229(3) 0.0320(3) 0.0247(3) -0.0071(2) -0.0098(2) -0.0055(2) Mn9 0.0255(3) 0.0341(3) 0.0231(3) 0.0026(2) -0.0108(2) -0.0125(2) Mn10 0.0198(2) 0.0325(3) 0.0167(2) -0.0067(2) -0.00695(19) -0.0061(2) Mn11 0.0174(2) 0.0319(3) 0.0170(2) -0.0064(2) -0.00532(19) -0.0060(2) Mn12 0.0193(2) 0.0369(4) 0.0200(3) -0.0118(2) -0.0028(2) -0.0060(2) O6 0.0347(15) 0.074(2) 0.0251(14) -0.0090(15) -0.0056(11) -0.0067(15) O10 0.0350(15) 0.080(2) 0.0255(14) -0.0014(15) -0.0030(12) 0.0115(15) O120 0.0271(13) 0.0477(18) 0.0264(13) -0.0130(13) -0.0003(10) -0.0106(12) O121 0.0367(14) 0.063(2) 0.0287(14) -0.0099(14) -0.0050(11) -0.0255(14) O107 0.0166(11) 0.0392(16) 0.0221(12) -0.0148(11) -0.0050(9) -0.0036(10) O108 0.0163(10) 0.0356(15) 0.0186(11) -0.0086(11) -0.0049(9) -0.0056(10) O123 0.0179(10) 0.0304(14) 0.0138(11) -0.0047(10) -0.0036(8) -0.0085(10) O124 0.0157(10) 0.0454(16) 0.0132(11) -0.0065(11) -0.0027(8) -0.0072(11) O134 0.0167(10) 0.0361(15) 0.0162(11) -0.0104(11) -0.0015(9) -0.0068(10) O208 0.0252(12) 0.0353(15) 0.0209(12) -0.0025(11) -0.0078(10) -0.0106(11) O209 0.0238(11) 0.0375(15) 0.0150(11) -0.0023(11) -0.0073(9) -0.0137(11) O234 0.0163(11) 0.0449(16) 0.0142(11) -0.0063(11) -0.0017(9) -0.0092(11) O310 0.0183(11) 0.0320(15) 0.0145(11) -0.0033(10) -0.0041(9) -0.0085(10) O311 0.0195(11) 0.0352(15) 0.0184(11) -0.0103(11) -0.0039(9) -0.0062(10) O405 0.0186(11) 0.0451(17) 0.0188(12) -0.0143(12) -0.0029(9) -0.0036(11) O406 0.0176(11) 0.0559(19) 0.0236(12) -0.0231(13) -0.0008(9) -0.0064(11) O13 0.0304(13) 0.0359(17) 0.0438(16) -0.0090(13) -0.0142(12) -0.0040(12) O23 0.0343(14) 0.0336(16) 0.0459(16) 0.0037(13) -0.0188(12) -0.0119(12) C13 0.039(2) 0.033(2) 0.0276(19) -0.0057(17) -0.0155(16) -0.0054(18) C23 0.054(3) 0.037(3) 0.047(3) -0.007(2) -0.022(2) -0.007(2) C33 0.052(3) 0.047(3) 0.046(3) 0.000(2) -0.027(2) 0.001(2) C43 0.092(4) 0.043(3) 0.068(4) -0.001(3) -0.037(3) 0.013(3) C53 0.105(5) 0.064(4) 0.046(3) -0.007(3) -0.027(3) 0.014(3) C63 0.056(3) 0.066(4) 0.098(4) -0.015(3) -0.042(3) 0.003(3) O14 0.0292(13) 0.0451(18) 0.0257(13) -0.0121(13) -0.0026(10) -0.0125(12) O24 0.0260(12) 0.0332(16) 0.0269(13) -0.0062(12) -0.0044(10) -0.0074(11) C14 0.0306(18) 0.0151(19) 0.0275(18) -0.0029(15) -0.0077(15) -0.0024(15) C24 0.0319(19) 0.030(2) 0.0257(18) -0.0036(16) -0.0029(15) -0.0089(16) C34 0.0349(19) 0.034(2) 0.0258(19) -0.0078(17) -0.0081(15) -0.0059(17) C44 0.062(3) 0.035(3) 0.047(3) -0.008(2) -0.025(2) -0.002(2) C54 0.044(2) 0.056(3) 0.032(2) -0.015(2) 0.0006(18) -0.007(2) C64 0.046(2) 0.050(3) 0.045(2) -0.023(2) -0.0067(19) -0.019(2) O15 0.0196(12) 0.0447(18) 0.0434(16) -0.0219(14) -0.0091(11) -0.0018(12) O25 0.0355(15) 0.0400(18) 0.0569(19) -0.0181(15) -0.0109(13) -0.0043(13) C15 0.0296(19) 0.039(3) 0.040(2) -0.012(2) -0.0158(17) -0.0057(18) C25 0.032(2) 0.047(3) 0.048(3) -0.015(2) -0.0093(18) -0.0033(19) C35 0.031(2) 0.047(3) 0.045(2) -0.020(2) -0.0116(18) 0.0000(19) C45 0.051(3) 0.074(4) 0.077(4) -0.046(3) -0.015(3) -0.010(3) C55 0.041(3) 0.082(4) 0.079(4) -0.042(3) -0.003(2) -0.002(3) C65 0.065(3) 0.047(3) 0.082(4) -0.009(3) -0.024(3) -0.001(3) O16 0.0348(14) 0.0399(18) 0.0268(13) -0.0051(13) -0.0123(11) -0.0101(13) O26 0.0394(15) 0.0450(18) 0.0296(14) -0.0048(13) -0.0171(12) -0.0100(13) C16 0.0265(18) 0.045(3) 0.0273(19) -0.0065(19) -0.0096(15) -0.0069(18) C26 0.035(2) 0.055(3) 0.029(2) 0.000(2) -0.0095(16) -0.017(2) C36 0.040(2) 0.043(3) 0.034(2) -0.0079(19) -0.0166(17) -0.0056(19) C46 0.085(4) 0.076(4) 0.041(3) 0.008(3) -0.034(3) -0.023(3) C56 0.055(3) 0.061(4) 0.068(3) -0.023(3) -0.023(3) 0.008(3) C66 0.046(2) 0.062(3) 0.051(3) -0.017(3) -0.023(2) -0.012(2) O17 0.0179(11) 0.0365(15) 0.0179(11) -0.0074(11) -0.0002(9) -0.0078(10) O27 0.0194(11) 0.0416(16) 0.0225(12) -0.0101(12) -0.0014(9) -0.0080(11) C17 0.0221(16) 0.027(2) 0.0231(17) -0.0118(15) 0.0022(13) -0.0081(15) C27 0.0255(17) 0.036(2) 0.0208(17) -0.0104(16) 0.0011(14) -0.0122(16) C37 0.0301(18) 0.033(2) 0.0207(17) -0.0123(16) 0.0016(14) -0.0072(16) C47 0.074(3) 0.054(3) 0.030(2) -0.016(2) 0.012(2) -0.027(3) C57 0.036(2) 0.036(2) 0.038(2) -0.0129(19) -0.0050(17) -0.0112(18) C67 0.036(2) 0.045(3) 0.051(3) -0.023(2) -0.0035(19) -0.0053(19) O18 0.0230(13) 0.087(3) 0.0415(16) -0.0425(17) -0.0065(11) -0.0068(14) O28 0.0218(12) 0.059(2) 0.0401(15) -0.0289(15) -0.0044(11) -0.0070(13) C18 0.0270(19) 0.071(3) 0.038(2) -0.025(2) -0.0088(17) -0.009(2) C28 0.046(2) 0.064(3) 0.044(3) -0.024(2) -0.002(2) -0.017(2) C38 0.044(2) 0.036(3) 0.047(2) -0.012(2) -0.0246(19) -0.0050(19) C48 0.075(4) 0.158(7) 0.055(3) -0.056(4) 0.006(3) -0.063(4) C58 0.049(3) 0.100(5) 0.087(4) -0.051(4) -0.014(3) -0.020(3) C68 0.213(10) 0.058(5) 0.191(9) -0.002(5) -0.160(8) -0.004(5) O19 0.0233(13) 0.0508(19) 0.0445(16) -0.0285(15) -0.0044(11) -0.0056(12) O29 0.0279(13) 0.0495(19) 0.0424(16) -0.0243(15) -0.0047(12) -0.0089(13) C19 0.0274(19) 0.045(3) 0.046(2) -0.031(2) -0.0055(17) -0.0030(18) C29 0.031(2) 0.039(3) 0.063(3) -0.027(2) -0.0071(19) -0.0022(18) C39 0.030(2) 0.035(3) 0.063(3) -0.019(2) 0.0037(19) -0.0063(18) C49 0.047(3) 0.048(3) 0.087(4) -0.013(3) 0.010(3) -0.019(2) C59 0.031(2) 0.051(3) 0.086(4) -0.020(3) 0.011(2) 0.000(2) C69 0.049(3) 0.052(3) 0.053(3) -0.025(2) 0.014(2) -0.015(2) O110 0.0287(14) 0.091(3) 0.0525(19) -0.0507(19) -0.0115(13) 0.0028(15) O210 0.0282(14) 0.089(3) 0.0361(16) -0.0416(18) -0.0088(12) 0.0044(15) C110 0.033(2) 0.111(5) 0.034(2) -0.043(3) -0.0055(18) -0.010(3) C210 0.048(3) 0.079(4) 0.047(3) -0.033(3) -0.010(2) -0.008(3) C310 0.074(3) 0.079(4) 0.032(2) -0.026(3) -0.011(2) -0.009(3) C410 0.088(4) 0.117(6) 0.052(3) -0.058(4) -0.012(3) -0.011(4) C510 0.316(14) 0.086(6) 0.066(5) -0.025(5) 0.001(7) -0.027(8) C610 0.066(4) 0.177(8) 0.056(4) -0.058(5) 0.008(3) -0.027(4) O111 0.0359(14) 0.0415(18) 0.0336(14) -0.0187(13) -0.0093(11) -0.0024(13) O211 0.0227(13) 0.078(2) 0.0536(18) -0.0475(18) -0.0081(12) 0.0042(14) C111 0.0255(18) 0.051(3) 0.030(2) -0.0238(19) 0.0049(15) -0.0132(18) C211 0.034(2) 0.051(3) 0.037(2) -0.026(2) -0.0031(17) -0.0057(19) C311 0.0247(19) 0.063(3) 0.046(2) -0.031(2) 0.0042(17) -0.0034(19) C411 0.050(3) 0.066(4) 0.056(3) -0.032(3) 0.002(2) 0.009(2) C511 0.054(3) 0.075(4) 0.045(3) -0.026(3) 0.005(2) 0.008(3) C611 0.040(3) 0.097(5) 0.085(4) -0.051(4) 0.023(3) -0.028(3) O112 0.0244(12) 0.063(2) 0.0172(12) -0.0091(13) 0.0001(10) -0.0058(13) O212 0.0354(16) 0.082(3) 0.0250(15) -0.0238(17) 0.0034(12) -0.0020(17) C112 0.0255(19) 0.090(4) 0.0182(19) -0.010(2) 0.0024(15) -0.002(2) C212 0.059(3) 0.096(5) 0.024(2) 0.006(3) 0.007(2) 0.020(3) C312 0.035(2) 0.063(3) 0.039(2) -0.023(2) 0.0153(18) -0.019(2) C412 0.049(3) 0.194(9) 0.109(6) 0.031(6) -0.016(4) -0.040(5) C512 0.181(8) 0.139(8) 0.115(6) -0.083(6) 0.107(6) -0.091(7) C612 0.072(4) 0.096(5) 0.041(3) -0.013(3) 0.020(3) -0.011(3) O113 0.0284(13) 0.0367(16) 0.0277(13) -0.0096(12) -0.0088(10) -0.0069(11) O213 0.0217(12) 0.0372(17) 0.0294(13) -0.0067(12) -0.0080(10) -0.0054(11) C113 0.0241(17) 0.035(2) 0.0192(17) -0.0072(16) 0.0003(13) -0.0091(16) C213 0.0322(19) 0.034(2) 0.0284(19) -0.0057(17) -0.0106(15) -0.0043(17) C313 0.0294(19) 0.034(2) 0.039(2) -0.0104(19) -0.0080(16) 0.0005(17) C413 0.037(2) 0.057(3) 0.044(3) -0.009(2) 0.0027(19) 0.000(2) C513 0.050(3) 0.043(3) 0.071(3) -0.028(3) -0.018(2) 0.001(2) C613 0.038(2) 0.042(3) 0.055(3) -0.013(2) -0.014(2) 0.004(2) O114 0.0330(14) 0.0381(17) 0.0382(15) 0.0052(13) -0.0188(12) -0.0156(12) O214 0.0328(13) 0.0329(16) 0.0347(14) -0.0100(13) -0.0159(11) -0.0057(12) C114 0.0279(18) 0.035(2) 0.0199(17) -0.0038(16) -0.0048(14) -0.0121(16) C214 0.0278(18) 0.040(2) 0.035(2) -0.0022(18) -0.0136(15) -0.0156(17) C314 0.0289(19) 0.033(2) 0.058(3) -0.014(2) -0.0126(18) -0.0048(17) C414 0.034(2) 0.053(4) 0.132(5) -0.032(4) -0.016(3) 0.003(2) C514 0.043(2) 0.037(3) 0.078(3) -0.021(3) -0.012(2) -0.010(2) C614 0.055(3) 0.064(3) 0.035(2) -0.023(2) 0.002(2) -0.018(2) O115 0.0243(12) 0.064(2) 0.0152(12) -0.0021(13) -0.0017(10) -0.0176(13) O215 0.0374(15) 0.057(2) 0.0238(14) 0.0076(14) -0.0097(11) -0.0241(14) C115 0.0269(19) 0.061(3) 0.0236(19) 0.002(2) -0.0094(15) -0.022(2) C215 0.040(2) 0.075(3) 0.0210(19) 0.007(2) -0.0070(16) -0.033(2) C315 0.048(2) 0.058(3) 0.0215(19) 0.0073(19) -0.0113(17) -0.028(2) C415 0.120(5) 0.072(4) 0.077(4) -0.004(3) -0.070(4) -0.015(4) C515 0.085(4) 0.156(7) 0.023(2) 0.013(3) -0.013(2) -0.073(4) C615 0.036(2) 0.067(3) 0.033(2) -0.008(2) -0.0078(17) -0.017(2) O116 0.0291(13) 0.0410(17) 0.0302(14) -0.0146(13) 0.0053(11) -0.0141(12) O216 0.0208(11) 0.0405(17) 0.0203(12) -0.0061(12) -0.0006(9) -0.0109(11) C116 0.0215(16) 0.035(2) 0.0260(18) -0.0071(17) 0.0004(14) -0.0125(16) C216 0.035(2) 0.036(2) 0.0270(19) -0.0075(18) -0.0001(15) -0.0085(18) C316 0.0280(18) 0.050(3) 0.029(2) -0.0007(19) -0.0047(15) -0.0154(18) C416 0.058(3) 0.036(3) 0.059(3) -0.004(2) -0.005(2) -0.018(2) C516 0.038(2) 0.086(4) 0.039(2) -0.001(3) -0.0056(19) -0.025(2) C616 0.049(3) 0.084(4) 0.032(2) 0.009(2) -0.0001(19) -0.027(3) O117 0.0295(13) 0.0398(17) 0.0222(12) -0.0099(12) -0.0125(10) -0.0019(12) O217 0.0230(12) 0.0354(16) 0.0222(12) -0.0085(11) -0.0091(9) -0.0051(11) C117 0.0225(16) 0.037(2) 0.0189(17) -0.0078(16) -0.0050(13) -0.0065(16) C217 0.0303(19) 0.044(3) 0.032(2) -0.0112(19) -0.0171(16) -0.0036(17) C317 0.055(3) 0.089(4) 0.024(2) -0.011(2) -0.0133(19) -0.017(3) C417 0.120(5) 0.121(6) 0.040(3) -0.024(3) -0.045(3) -0.009(4) C517 0.062(3) 0.150(7) 0.042(3) -0.004(4) 0.009(3) -0.006(4) C617 0.111(5) 0.086(5) 0.044(3) 0.012(3) -0.032(3) -0.033(4) O118 0.0215(11) 0.0369(16) 0.0163(11) -0.0062(11) 0.0011(9) -0.0095(11) O218 0.0253(12) 0.0369(16) 0.0206(12) 0.0000(11) -0.0058(10) -0.0085(11) C118 0.0286(18) 0.034(2) 0.0194(17) -0.0041(16) 0.0010(14) -0.0083(16) C218 0.042(2) 0.050(3) 0.030(2) 0.009(2) 0.0007(17) -0.011(2) C318 0.052(2) 0.036(3) 0.028(2) 0.0062(18) -0.0107(18) -0.015(2) C418 0.084(4) 0.060(4) 0.048(3) 0.015(3) -0.001(3) -0.031(3) C518 0.111(5) 0.070(4) 0.066(4) 0.033(3) -0.055(3) -0.041(4) C618 0.109(5) 0.044(3) 0.054(3) -0.005(3) 0.001(3) -0.013(3) N1A 0.0192(16) 0.063(3) 0.055(2) -0.019(2) -0.0059(15) -0.0080(17) C1A 0.041(2) 0.062(3) 0.053(3) -0.002(3) -0.011(2) -0.019(2) O2A 0.0392(19) 0.142(4) 0.075(3) -0.066(3) 0.0005(17) -0.017(2) O3A 0.059(2) 0.060(3) 0.103(3) 0.000(2) -0.030(2) -0.005(2) _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 O108 1.863(2) . ? Mn1 O107 1.882(2) . ? Mn1 O17 1.900(2) . ? Mn1 O134 1.914(2) . ? Mn1 O124 1.916(2) . ? Mn1 O123 1.925(2) . ? Mn1 Mn7 2.7833(7) . ? Mn1 Mn4 2.8419(7) . ? Mn1 Mn2 2.8428(7) . ? Mn1 Mn3 2.9326(6) . ? Mn2 O208 1.836(3) . ? Mn2 O209 1.860(2) . ? Mn2 O115 1.908(2) . ? Mn2 O123 1.918(2) . ? Mn2 O124 1.927(2) . ? Mn2 O234 1.935(3) . ? Mn2 Mn9 2.7315(8) . ? Mn2 Mn3 2.8254(8) . ? Mn2 Mn4 2.9364(8) . ? Mn3 O310 1.869(2) . ? Mn3 O311 1.870(2) . ? Mn3 O234 1.889(2) . ? Mn3 O123 1.908(2) . ? Mn3 O134 1.914(2) . ? Mn3 O118 1.926(2) . ? Mn3 Mn11 2.7776(7) . ? Mn3 Mn4 2.8024(7) . ? Mn4 O406 1.856(2) . ? Mn4 O405 1.881(3) . ? Mn4 O134 1.890(2) . ? Mn4 O234 1.905(2) . ? Mn4 O124 1.919(3) . ? Mn4 O112 1.920(2) . ? Mn4 Mn5 2.7913(9) . ? Mn5 O406 1.861(3) . ? Mn5 O405 1.917(2) . ? Mn5 O211 1.935(3) . ? Mn5 O110 1.949(3) . ? Mn5 O19 2.181(3) . ? Mn5 O212 2.209(3) . ? Mn6 O406 1.864(2) . ? Mn6 O107 1.899(2) . ? Mn6 O18 1.929(2) . ? Mn6 O210 1.959(3) . ? Mn6 O29 2.111(3) . ? Mn6 O6 2.253(3) . ? Mn7 O108 1.893(2) . ? Mn7 O107 1.915(2) . ? Mn7 O15 1.921(3) . ? Mn7 O28 1.960(3) . ? Mn7 O27 2.193(2) . ? Mn7 O16 2.199(3) . ? Mn8 O108 1.893(3) . ? Mn8 O26 1.956(3) . ? Mn8 O14 1.961(2) . ? Mn8 O13 1.963(3) . ? Mn8 O208 2.049(2) . ? Mn8 O25 2.145(3) . ? Mn9 O208 1.859(2) . ? Mn9 O209 1.894(3) . ? Mn9 O23 1.953(3) . ? Mn9 O114 1.958(3) . ? Mn9 O215 2.195(3) . ? Mn9 O24 2.208(2) . ? Mn10 O310 1.886(2) . ? Mn10 O209 1.886(2) . ? Mn10 O214 1.940(3) . ? Mn10 O117 1.958(2) . ? Mn10 O116 2.103(2) . ? Mn10 O10 2.261(3) . ? Mn11 O311 1.892(2) . ? Mn11 O310 1.894(2) . ? Mn11 O217 1.930(2) . ? Mn11 O213 1.948(3) . ? Mn11 O216 2.184(2) . ? Mn11 O218 2.201(2) . ? Mn12 O311 1.860(2) . ? Mn12 O405 1.884(2) . ? Mn12 O111 1.941(3) . ? Mn12 O113 1.945(2) . ? Mn12 O121 2.219(3) . ? Mn12 O120 2.257(2) . ? O13 C13 1.257(5) . ? O23 C13 1.262(4) . ? C13 C23 1.507(6) . ? C23 C33 1.528(6) . ? C33 C63 1.522(7) . ? C33 C43 1.522(7) . ? C33 C53 1.528(7) . ? O14 C14 1.250(4) . ? O24 C14 1.262(4) . ? C14 C24 1.514(5) . ? C24 C34 1.549(5) . ? C34 C44 1.525(5) . ? C34 C64 1.530(5) . ? C34 C54 1.532(5) . ? O15 C15 1.249(5) . ? O25 C15 1.252(5) . ? C15 C25 1.524(5) . ? C25 C35 1.524(6) . ? C35 C65 1.497(7) . ? C35 C45 1.508(6) . ? C35 C55 1.542(6) . ? O16 C16 1.240(5) . ? O26 C16 1.279(5) . ? C16 C26 1.517(5) . ? C26 C36 1.533(5) . ? C36 C56 1.512(6) . ? C36 C66 1.516(6) . ? C36 C46 1.528(6) . ? O17 C17 1.289(4) . ? O27 C17 1.237(4) . ? C17 C27 1.510(5) . ? C27 C37 1.544(5) . ? C37 C57 1.521(5) . ? C37 C47 1.528(5) . ? C37 C67 1.529(6) . ? O18 C18 1.265(5) . ? O28 C18 1.265(5) . ? C18 C28 1.511(6) . ? C28 C38 1.525(6) . ? C38 C68 1.480(8) . ? C38 C48 1.495(7) . ? C38 C58 1.557(6) . ? O19 C19 1.270(4) . ? O29 C19 1.249(5) . ? C19 C29 1.505(6) . ? C29 C39 1.549(6) . ? C39 C69 1.517(6) . ? C39 C49 1.524(6) . ? C39 C59 1.526(6) . ? O110 C110 1.264(5) . ? O210 C110 1.281(6) . ? C110 C210 1.530(6) . ? C210 C310 1.487(7) . ? C310 C410 1.504(6) . ? C310 C610 1.512(8) . ? C310 C510 1.530(10) . ? O111 C111 1.271(4) . ? O211 C111 1.256(5) . ? C111 C211 1.487(6) . ? C211 C311 1.542(5) . ? C311 C611 1.523(6) . ? C311 C511 1.527(7) . ? C311 C411 1.533(6) . ? O112 C112 1.292(5) . ? O212 C112 1.236(6) . ? C112 C212 1.511(6) . ? C212 C312 1.503(6) . ? C312 C412 1.486(8) . ? C312 C612 1.502(7) . ? C312 C512 1.509(8) . ? O113 C113 1.262(4) . ? O213 C113 1.267(4) . ? C113 C213 1.502(5) . ? C213 C313 1.539(5) . ? C313 C513 1.513(6) . ? C313 C413 1.521(6) . ? C313 C613 1.541(5) . ? O114 C114 1.258(4) . ? O214 C114 1.249(4) . ? C114 C214 1.502(5) . ? C214 C314 1.548(6) . ? C314 C514 1.520(5) . ? C314 C614 1.528(6) . ? C314 C414 1.528(6) . ? O115 C115 1.297(5) . ? O215 C115 1.231(5) . ? C115 C215 1.501(5) . ? C215 C315 1.538(5) . ? C315 C415 1.504(7) . ? C315 C615 1.524(6) . ? C315 C515 1.530(6) . ? O116 C116 1.242(4) . ? O216 C116 1.270(5) . ? C116 C216 1.519(5) . ? C216 C316 1.540(5) . ? C316 C416 1.509(6) . ? C316 C516 1.521(5) . ? C316 C616 1.523(5) . ? O117 C117 1.257(4) . ? O217 C117 1.264(4) . ? C117 C217 1.494(4) . ? C217 C317 1.529(6) . ? C317 C517 1.498(7) . ? C317 C417 1.529(6) . ? C317 C617 1.556(8) . ? O118 C118 1.302(4) . ? O218 C118 1.237(4) . ? C118 C218 1.513(5) . ? C218 C318 1.510(6) . ? C318 C518 1.518(6) . ? C318 C618 1.522(7) . ? C318 C418 1.528(6) . ? N1A O3A 1.192(5) . ? N1A O2A 1.207(5) . ? N1A C1A 1.481(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O108 Mn1 O107 84.32(10) . . ? O108 Mn1 O17 92.69(10) . . ? O107 Mn1 O17 95.23(10) . . ? O108 Mn1 O134 175.77(10) . . ? O107 Mn1 O134 99.31(10) . . ? O17 Mn1 O134 89.13(10) . . ? O108 Mn1 O124 95.12(10) . . ? O107 Mn1 O124 89.63(10) . . ? O17 Mn1 O124 171.17(10) . . ? O134 Mn1 O124 82.81(10) . . ? O108 Mn1 O123 96.31(10) . . ? O107 Mn1 O123 173.32(10) . . ? O17 Mn1 O123 91.39(9) . . ? O134 Mn1 O123 79.83(10) . . ? O124 Mn1 O123 83.68(9) . . ? O108 Mn1 Mn7 42.61(7) . . ? O107 Mn1 Mn7 43.31(7) . . ? O17 Mn1 Mn7 86.20(7) . . ? O134 Mn1 Mn7 141.42(7) . . ? O124 Mn1 Mn7 102.34(7) . . ? O123 Mn1 Mn7 138.50(7) . . ? O108 Mn1 Mn4 137.08(7) . . ? O107 Mn1 Mn4 89.87(7) . . ? O17 Mn1 Mn4 130.21(8) . . ? O134 Mn1 Mn4 41.33(7) . . ? O124 Mn1 Mn4 42.23(8) . . ? O123 Mn1 Mn4 85.13(7) . . ? Mn7 Mn1 Mn4 126.67(2) . . ? O108 Mn1 Mn2 90.66(7) . . ? O107 Mn1 Mn2 131.24(7) . . ? O17 Mn1 Mn2 133.50(7) . . ? O134 Mn1 Mn2 85.33(7) . . ? O124 Mn1 Mn2 42.46(7) . . ? O123 Mn1 Mn2 42.19(6) . . ? Mn7 Mn1 Mn2 124.25(3) . . ? Mn4 Mn1 Mn2 62.202(19) . . ? O108 Mn1 Mn3 136.17(7) . . ? O107 Mn1 Mn3 139.12(8) . . ? O17 Mn1 Mn3 89.07(7) . . ? O134 Mn1 Mn3 40.00(7) . . ? O124 Mn1 Mn3 82.46(6) . . ? O123 Mn1 Mn3 39.86(7) . . ? Mn7 Mn1 Mn3 174.97(2) . . ? Mn4 Mn1 Mn3 58.040(16) . . ? Mn2 Mn1 Mn3 58.554(17) . . ? O208 Mn2 O209 85.30(11) . . ? O208 Mn2 O115 93.41(11) . . ? O209 Mn2 O115 93.67(10) . . ? O208 Mn2 O123 93.23(10) . . ? O209 Mn2 O123 90.52(9) . . ? O115 Mn2 O123 172.42(12) . . ? O208 Mn2 O124 96.62(10) . . ? O209 Mn2 O124 173.88(10) . . ? O115 Mn2 O124 92.01(10) . . ? O123 Mn2 O124 83.58(9) . . ? O208 Mn2 O234 175.20(10) . . ? O209 Mn2 O234 97.89(10) . . ? O115 Mn2 O234 89.97(11) . . ? O123 Mn2 O234 83.19(10) . . ? O124 Mn2 O234 79.84(10) . . ? O208 Mn2 Mn9 42.65(7) . . ? O209 Mn2 Mn9 43.79(8) . . ? O115 Mn2 Mn9 87.05(9) . . ? O123 Mn2 Mn9 100.33(7) . . ? O124 Mn2 Mn9 138.98(7) . . ? O234 Mn2 Mn9 141.12(7) . . ? O208 Mn2 Mn3 135.15(7) . . ? O209 Mn2 Mn3 89.29(8) . . ? O115 Mn2 Mn3 131.40(9) . . ? O123 Mn2 Mn3 42.25(7) . . ? O124 Mn2 Mn3 85.25(7) . . ? O234 Mn2 Mn3 41.73(6) . . ? Mn9 Mn2 Mn3 124.71(2) . . ? O208 Mn2 Mn1 89.61(7) . . ? O209 Mn2 Mn1 132.29(7) . . ? O115 Mn2 Mn1 134.01(8) . . ? O123 Mn2 Mn1 42.39(6) . . ? O124 Mn2 Mn1 42.15(6) . . ? O234 Mn2 Mn1 85.59(7) . . ? Mn9 Mn2 Mn1 122.90(2) . . ? Mn3 Mn2 Mn1 62.313(18) . . ? O208 Mn2 Mn4 136.74(8) . . ? O209 Mn2 Mn4 137.52(8) . . ? O115 Mn2 Mn4 90.02(9) . . ? O123 Mn2 Mn4 82.63(7) . . ? O124 Mn2 Mn4 40.14(7) . . ? O234 Mn2 Mn4 39.74(7) . . ? Mn9 Mn2 Mn4 176.91(2) . . ? Mn3 Mn2 Mn4 58.167(18) . . ? Mn1 Mn2 Mn4 58.885(18) . . ? O310 Mn3 O311 85.15(10) . . ? O310 Mn3 O234 90.45(10) . . ? O311 Mn3 O234 88.16(10) . . ? O310 Mn3 O123 96.94(10) . . ? O311 Mn3 O123 172.56(9) . . ? O234 Mn3 O123 84.70(10) . . ? O310 Mn3 O134 173.92(10) . . ? O311 Mn3 O134 96.96(10) . . ? O234 Mn3 O134 83.94(10) . . ? O123 Mn3 O134 80.27(10) . . ? O310 Mn3 O118 93.06(10) . . ? O311 Mn3 O118 89.69(10) . . ? O234 Mn3 O118 175.71(11) . . ? O123 Mn3 O118 97.31(10) . . ? O134 Mn3 O118 92.65(10) . . ? O310 Mn3 Mn11 42.78(7) . . ? O311 Mn3 Mn11 42.72(7) . . ? O234 Mn3 Mn11 93.37(7) . . ? O123 Mn3 Mn11 139.71(7) . . ? O134 Mn3 Mn11 139.68(7) . . ? O118 Mn3 Mn11 87.56(7) . . ? O310 Mn3 Mn4 132.58(7) . . ? O311 Mn3 Mn4 86.77(7) . . ? O234 Mn3 Mn4 42.60(7) . . ? O123 Mn3 Mn4 86.58(7) . . ? O134 Mn3 Mn4 42.21(6) . . ? O118 Mn3 Mn4 133.55(7) . . ? Mn11 Mn3 Mn4 118.32(2) . . ? O310 Mn3 Mn2 88.49(7) . . ? O311 Mn3 Mn2 130.70(7) . . ? O234 Mn3 Mn2 42.99(8) . . ? O123 Mn3 Mn2 42.52(6) . . ? O134 Mn3 Mn2 85.82(7) . . ? O118 Mn3 Mn2 139.52(8) . . ? Mn11 Mn3 Mn2 118.73(2) . . ? Mn4 Mn3 Mn2 62.900(19) . . ? O310 Mn3 Mn1 137.14(8) . . ? O311 Mn3 Mn1 136.76(7) . . ? O234 Mn3 Mn1 83.84(7) . . ? O123 Mn3 Mn1 40.30(7) . . ? O134 Mn3 Mn1 40.00(7) . . ? O118 Mn3 Mn1 95.22(7) . . ? Mn11 Mn3 Mn1 177.21(2) . . ? Mn4 Mn3 Mn1 59.359(16) . . ? Mn2 Mn3 Mn1 59.134(17) . . ? O406 Mn4 O405 84.13(11) . . ? O406 Mn4 O134 92.10(10) . . ? O405 Mn4 O134 88.72(10) . . ? O406 Mn4 O234 173.49(10) . . ? O405 Mn4 O234 101.07(10) . . ? O134 Mn4 O234 84.17(9) . . ? O406 Mn4 O124 93.49(11) . . ? O405 Mn4 O124 171.66(10) . . ? O134 Mn4 O124 83.37(10) . . ? O234 Mn4 O124 80.80(10) . . ? O406 Mn4 O112 90.95(11) . . ? O405 Mn4 O112 92.52(11) . . ? O134 Mn4 O112 176.82(11) . . ? O234 Mn4 O112 92.72(11) . . ? O124 Mn4 O112 95.52(11) . . ? O406 Mn4 Mn5 41.41(8) . . ? O405 Mn4 Mn5 43.20(7) . . ? O134 Mn4 Mn5 95.57(8) . . ? O234 Mn4 Mn5 144.16(8) . . ? O124 Mn4 Mn5 134.90(7) . . ? O112 Mn4 Mn5 87.33(9) . . ? O406 Mn4 Mn3 134.81(8) . . ? O405 Mn4 Mn3 89.96(7) . . ? O134 Mn4 Mn3 42.89(7) . . ? O234 Mn4 Mn3 42.16(7) . . ? O124 Mn4 Mn3 86.05(7) . . ? O112 Mn4 Mn3 134.14(8) . . ? Mn5 Mn4 Mn3 122.81(3) . . ? O406 Mn4 Mn1 87.50(7) . . ? O405 Mn4 Mn1 129.61(7) . . ? O134 Mn4 Mn1 41.98(7) . . ? O234 Mn4 Mn1 86.16(7) . . ? O124 Mn4 Mn1 42.14(7) . . ? O112 Mn4 Mn1 137.32(9) . . ? Mn5 Mn4 Mn1 117.18(2) . . ? Mn3 Mn4 Mn1 62.602(17) . . ? O406 Mn4 Mn2 133.83(8) . . ? O405 Mn4 Mn2 141.22(7) . . ? O134 Mn4 Mn2 83.09(8) . . ? O234 Mn4 Mn2 40.49(7) . . ? O124 Mn4 Mn2 40.34(7) . . ? O112 Mn4 Mn2 94.12(9) . . ? Mn5 Mn4 Mn2 175.12(2) . . ? Mn3 Mn4 Mn2 58.933(18) . . ? Mn1 Mn4 Mn2 58.913(18) . . ? O406 Mn5 O405 83.00(10) . . ? O406 Mn5 O211 177.90(11) . . ? O405 Mn5 O211 94.96(11) . . ? O406 Mn5 O110 95.97(12) . . ? O405 Mn5 O110 173.75(13) . . ? O211 Mn5 O110 86.01(12) . . ? O406 Mn5 O19 91.70(11) . . ? O405 Mn5 O19 98.45(10) . . ? O211 Mn5 O19 89.09(12) . . ? O110 Mn5 O19 87.73(12) . . ? O406 Mn5 O212 84.95(12) . . ? O405 Mn5 O212 84.33(11) . . ? O211 Mn5 O212 94.36(13) . . ? O110 Mn5 O212 89.44(13) . . ? O19 Mn5 O212 175.37(11) . . ? O406 Mn5 Mn4 41.27(7) . . ? O405 Mn5 Mn4 42.20(8) . . ? O211 Mn5 Mn4 136.64(8) . . ? O110 Mn5 Mn4 135.70(10) . . ? O19 Mn5 Mn4 101.60(7) . . ? O212 Mn5 Mn4 77.95(9) . . ? O406 Mn6 O107 94.85(10) . . ? O406 Mn6 O18 173.13(11) . . ? O107 Mn6 O18 90.87(10) . . ? O406 Mn6 O210 90.49(11) . . ? O107 Mn6 O210 174.40(11) . . ? O18 Mn6 O210 83.70(11) . . ? O406 Mn6 O29 93.54(11) . . ? O107 Mn6 O29 94.34(11) . . ? O18 Mn6 O29 89.83(13) . . ? O210 Mn6 O29 87.01(13) . . ? O406 Mn6 O6 85.73(11) . . ? O107 Mn6 O6 92.54(11) . . ? O18 Mn6 O6 90.21(13) . . ? O210 Mn6 O6 86.16(13) . . ? O29 Mn6 O6 173.12(10) . . ? O108 Mn7 O107 82.63(10) . . ? O108 Mn7 O15 97.60(11) . . ? O107 Mn7 O15 172.42(11) . . ? O108 Mn7 O28 175.22(12) . . ? O107 Mn7 O28 93.31(11) . . ? O15 Mn7 O28 86.10(11) . . ? O108 Mn7 O27 87.87(9) . . ? O107 Mn7 O27 88.50(10) . . ? O15 Mn7 O27 83.95(11) . . ? O28 Mn7 O27 89.51(10) . . ? O108 Mn7 O16 89.58(10) . . ? O107 Mn7 O16 96.54(10) . . ? O15 Mn7 O16 91.04(11) . . ? O28 Mn7 O16 93.40(11) . . ? O27 Mn7 O16 174.02(10) . . ? O108 Mn7 Mn1 41.77(7) . . ? O107 Mn7 Mn1 42.40(7) . . ? O15 Mn7 Mn1 135.64(8) . . ? O28 Mn7 Mn1 133.67(9) . . ? O27 Mn7 Mn1 78.71(6) . . ? O16 Mn7 Mn1 102.87(7) . . ? O108 Mn8 O26 96.19(11) . . ? O108 Mn8 O14 91.35(11) . . ? O26 Mn8 O14 169.45(12) . . ? O108 Mn8 O13 175.32(10) . . ? O26 Mn8 O13 85.56(12) . . ? O14 Mn8 O13 86.39(12) . . ? O108 Mn8 O208 92.69(10) . . ? O26 Mn8 O208 90.80(10) . . ? O14 Mn8 O208 96.22(10) . . ? O13 Mn8 O208 91.63(11) . . ? O108 Mn8 O25 90.20(10) . . ? O26 Mn8 O25 88.49(11) . . ? O14 Mn8 O25 84.10(11) . . ? O13 Mn8 O25 85.51(11) . . ? O208 Mn8 O25 177.09(11) . . ? O208 Mn9 O209 83.73(10) . . ? O208 Mn9 O23 94.99(11) . . ? O209 Mn9 O23 175.69(11) . . ? O208 Mn9 O114 176.40(11) . . ? O209 Mn9 O114 93.89(10) . . ? O23 Mn9 O114 87.19(11) . . ? O208 Mn9 O215 86.69(10) . . ? O209 Mn9 O215 88.82(11) . . ? O23 Mn9 O215 86.99(12) . . ? O114 Mn9 O215 90.57(11) . . ? O208 Mn9 O24 91.68(10) . . ? O209 Mn9 O24 95.72(10) . . ? O23 Mn9 O24 88.43(11) . . ? O114 Mn9 O24 91.25(10) . . ? O215 Mn9 O24 174.98(10) . . ? O208 Mn9 Mn2 42.00(8) . . ? O209 Mn9 Mn2 42.83(7) . . ? O23 Mn9 Mn2 135.00(8) . . ? O114 Mn9 Mn2 135.10(8) . . ? O215 Mn9 Mn2 79.42(9) . . ? O24 Mn9 Mn2 102.49(7) . . ? O310 Mn10 O209 94.70(10) . . ? O310 Mn10 O214 175.20(10) . . ? O209 Mn10 O214 90.07(11) . . ? O310 Mn10 O117 90.67(10) . . ? O209 Mn10 O117 171.81(11) . . ? O214 Mn10 O117 84.53(11) . . ? O310 Mn10 O116 91.56(10) . . ? O209 Mn10 O116 94.72(10) . . ? O214 Mn10 O116 88.66(11) . . ? O117 Mn10 O116 91.31(10) . . ? O310 Mn10 O10 88.14(12) . . ? O209 Mn10 O10 91.73(10) . . ? O214 Mn10 O10 91.10(12) . . ? O117 Mn10 O10 82.25(10) . . ? O116 Mn10 O10 173.55(10) . . ? O311 Mn11 O310 83.85(10) . . ? O311 Mn11 O217 175.15(10) . . ? O310 Mn11 O217 95.22(10) . . ? O311 Mn11 O213 94.16(11) . . ? O310 Mn11 O213 176.49(10) . . ? O217 Mn11 O213 86.52(11) . . ? O311 Mn11 O216 90.61(9) . . ? O310 Mn11 O216 93.90(9) . . ? O217 Mn11 O216 94.20(9) . . ? O213 Mn11 O216 89.00(10) . . ? O311 Mn11 O218 83.95(9) . . ? O310 Mn11 O218 84.70(9) . . ? O217 Mn11 O218 91.23(9) . . ? O213 Mn11 O218 92.23(10) . . ? O216 Mn11 O218 174.50(9) . . ? O311 Mn11 Mn3 42.10(7) . . ? O310 Mn11 Mn3 42.09(7) . . ? O217 Mn11 Mn3 136.27(8) . . ? O213 Mn11 Mn3 135.56(8) . . ? O216 Mn11 Mn3 97.25(6) . . ? O218 Mn11 Mn3 78.14(6) . . ? O311 Mn12 O405 94.29(11) . . ? O311 Mn12 O111 173.31(11) . . ? O405 Mn12 O111 92.37(11) . . ? O311 Mn12 O113 89.98(10) . . ? O405 Mn12 O113 175.04(10) . . ? O111 Mn12 O113 83.40(11) . . ? O311 Mn12 O121 88.70(10) . . ? O405 Mn12 O121 91.46(10) . . ? O111 Mn12 O121 90.47(11) . . ? O113 Mn12 O121 91.15(10) . . ? O311 Mn12 O120 92.31(10) . . ? O405 Mn12 O120 86.64(10) . . ? O111 Mn12 O120 88.74(11) . . ? O113 Mn12 O120 90.68(10) . . ? O121 Mn12 O120 177.91(9) . . ? Mn1 O107 Mn6 130.86(12) . . ? Mn1 O107 Mn7 94.29(11) . . ? Mn6 O107 Mn7 127.30(12) . . ? Mn1 O108 Mn8 134.17(12) . . ? Mn1 O108 Mn7 95.62(11) . . ? Mn8 O108 Mn7 124.92(12) . . ? Mn3 O123 Mn2 95.23(9) . . ? Mn3 O123 Mn1 99.84(11) . . ? Mn2 O123 Mn1 95.42(9) . . ? Mn1 O124 Mn4 95.63(11) . . ? Mn1 O124 Mn2 95.40(10) . . ? Mn4 O124 Mn2 99.52(10) . . ? Mn4 O134 Mn1 96.68(11) . . ? Mn4 O134 Mn3 94.90(10) . . ? Mn1 O134 Mn3 100.00(11) . . ? Mn2 O208 Mn9 95.35(10) . . ? Mn2 O208 Mn8 132.28(14) . . ? Mn9 O208 Mn8 121.93(13) . . ? Mn2 O209 Mn10 132.41(15) . . ? Mn2 O209 Mn9 93.38(10) . . ? Mn10 O209 Mn9 131.00(13) . . ? Mn3 O234 Mn4 95.24(11) . . ? Mn3 O234 Mn2 95.27(10) . . ? Mn4 O234 Mn2 99.77(10) . . ? Mn3 O310 Mn10 133.28(12) . . ? Mn3 O310 Mn11 95.13(11) . . ? Mn10 O310 Mn11 123.22(11) . . ? Mn12 O311 Mn3 132.58(12) . . ? Mn12 O311 Mn11 130.78(12) . . ? Mn3 O311 Mn11 95.18(11) . . ? Mn4 O405 Mn12 130.75(13) . . ? Mn4 O405 Mn5 94.60(10) . . ? Mn12 O405 Mn5 127.81(15) . . ? Mn4 O406 Mn5 97.32(11) . . ? Mn4 O406 Mn6 133.68(14) . . ? Mn5 O406 Mn6 125.31(15) . . ? C13 O13 Mn8 136.8(3) . . ? C13 O23 Mn9 131.6(3) . . ? O13 C13 O23 125.5(4) . . ? O13 C13 C23 118.2(3) . . ? O23 C13 C23 116.3(4) . . ? C13 C23 C33 116.7(4) . . ? C63 C33 C43 110.4(4) . . ? C63 C33 C23 111.4(4) . . ? C43 C33 C23 107.0(4) . . ? C63 C33 C53 108.9(5) . . ? C43 C33 C53 109.6(4) . . ? C23 C33 C53 109.4(4) . . ? C14 O14 Mn8 132.3(2) . . ? C14 O24 Mn9 133.7(2) . . ? O14 C14 O24 125.7(3) . . ? O14 C14 C24 115.7(3) . . ? O24 C14 C24 118.6(3) . . ? C14 C24 C34 114.9(3) . . ? C44 C34 C64 110.8(4) . . ? C44 C34 C54 108.8(3) . . ? C64 C34 C54 109.0(3) . . ? C44 C34 C24 110.6(3) . . ? C64 C34 C24 111.4(3) . . ? C54 C34 C24 106.2(3) . . ? C15 O15 Mn7 131.4(2) . . ? C15 O25 Mn8 132.1(3) . . ? O15 C15 O25 124.2(4) . . ? O15 C15 C25 114.6(3) . . ? O25 C15 C25 121.2(4) . . ? C35 C25 C15 119.2(4) . . ? C65 C35 C45 112.0(4) . . ? C65 C35 C25 110.3(4) . . ? C45 C35 C25 111.2(4) . . ? C65 C35 C55 107.2(4) . . ? C45 C35 C55 109.2(4) . . ? C25 C35 C55 106.6(4) . . ? C16 O16 Mn7 131.8(2) . . ? C16 O26 Mn8 133.8(3) . . ? O16 C16 O26 125.4(4) . . ? O16 C16 C26 119.5(4) . . ? O26 C16 C26 115.2(4) . . ? C16 C26 C36 115.7(3) . . ? C56 C36 C66 109.9(4) . . ? C56 C36 C46 109.6(4) . . ? C66 C36 C46 109.2(4) . . ? C56 C36 C26 110.4(3) . . ? C66 C36 C26 110.9(4) . . ? C46 C36 C26 106.8(3) . . ? C17 O17 Mn1 126.9(2) . . ? C17 O27 Mn7 122.4(2) . . ? O27 C17 O17 125.2(3) . . ? O27 C17 C27 120.2(3) . . ? O17 C17 C27 114.6(3) . . ? C17 C27 C37 113.9(3) . . ? C57 C37 C47 109.0(3) . . ? C57 C37 C67 109.4(3) . . ? C47 C37 C67 109.0(3) . . ? C57 C37 C27 110.9(3) . . ? C47 C37 C27 107.8(3) . . ? C67 C37 C27 110.8(3) . . ? C18 O18 Mn6 133.9(3) . . ? C18 O28 Mn7 127.9(2) . . ? O18 C18 O28 123.1(4) . . ? O18 C18 C28 118.0(4) . . ? O28 C18 C28 118.9(3) . . ? C18 C28 C38 114.6(4) . . ? C68 C38 C48 115.1(6) . . ? C68 C38 C28 108.0(5) . . ? C48 C38 C28 112.8(4) . . ? C68 C38 C58 106.9(5) . . ? C48 C38 C58 107.6(4) . . ? C28 C38 C58 106.0(4) . . ? C19 O19 Mn5 123.4(3) . . ? C19 O29 Mn6 134.4(3) . . ? O29 C19 O19 125.3(4) . . ? O29 C19 C29 116.4(3) . . ? O19 C19 C29 118.4(4) . . ? C19 C29 C39 115.4(4) . . ? C69 C39 C49 109.7(4) . . ? C69 C39 C59 109.8(4) . . ? C49 C39 C59 109.3(4) . . ? C69 C39 C29 110.1(3) . . ? C49 C39 C29 106.4(4) . . ? C59 C39 C29 111.5(4) . . ? C110 O110 Mn5 130.8(3) . . ? C110 O210 Mn6 128.1(3) . . ? O110 C110 O210 126.1(4) . . ? O110 C110 C210 116.7(5) . . ? O210 C110 C210 117.3(4) . . ? C310 C210 C110 113.9(4) . . ? C210 C310 C410 111.2(5) . . ? C210 C310 C610 111.8(4) . . ? C410 C310 C610 109.3(5) . . ? C210 C310 C510 107.8(5) . . ? C410 C310 C510 105.2(5) . . ? C610 C310 C510 111.2(7) . . ? C111 O111 Mn12 137.8(3) . . ? C111 O211 Mn5 133.7(3) . . ? O211 C111 O111 124.1(4) . . ? O211 C111 C211 117.9(3) . . ? O111 C111 C211 118.0(4) . . ? C111 C211 C311 113.9(4) . . ? C611 C311 C511 109.9(5) . . ? C611 C311 C411 109.7(4) . . ? C511 C311 C411 109.4(4) . . ? C611 C311 C211 110.4(4) . . ? C511 C311 C211 110.7(3) . . ? C411 C311 C211 106.7(4) . . ? C112 O112 Mn4 125.0(3) . . ? C112 O212 Mn5 123.1(3) . . ? O212 C112 O112 126.2(4) . . ? O212 C112 C212 119.8(4) . . ? O112 C112 C212 114.0(5) . . ? C312 C212 C112 118.9(4) . . ? C412 C312 C612 110.8(4) . . ? C412 C312 C212 109.5(4) . . ? C612 C312 C212 110.2(4) . . ? C412 C312 C512 106.5(7) . . ? C612 C312 C512 108.5(5) . . ? C212 C312 C512 111.3(5) . . ? C113 O113 Mn12 132.5(3) . . ? C113 O213 Mn11 131.1(2) . . ? O113 C113 O213 125.3(3) . . ? O113 C113 C213 117.6(3) . . ? O213 C113 C213 117.1(3) . . ? C113 C213 C313 114.8(3) . . ? C513 C313 C413 109.7(4) . . ? C513 C313 C213 112.2(3) . . ? C413 C313 C213 110.0(3) . . ? C513 C313 C613 109.0(4) . . ? C413 C313 C613 108.7(3) . . ? C213 C313 C613 107.2(3) . . ? C114 O114 Mn9 131.5(3) . . ? C114 O214 Mn10 137.8(2) . . ? O214 C114 O114 125.8(3) . . ? O214 C114 C214 116.4(3) . . ? O114 C114 C214 117.8(3) . . ? C114 C214 C314 114.6(3) . . ? C514 C314 C614 110.5(4) . . ? C514 C314 C414 108.3(4) . . ? C614 C314 C414 109.6(4) . . ? C514 C314 C214 107.3(3) . . ? C614 C314 C214 110.0(3) . . ? C414 C314 C214 111.2(4) . . ? C115 O115 Mn2 125.8(3) . . ? C115 O215 Mn9 122.1(3) . . ? O215 C115 O115 125.2(3) . . ? O215 C115 C215 121.8(4) . . ? O115 C115 C215 112.9(4) . . ? C115 C215 C315 113.6(3) . . ? C415 C315 C615 109.1(4) . . ? C415 C315 C515 111.3(5) . . ? C615 C315 C515 107.9(4) . . ? C415 C315 C215 110.8(4) . . ? C615 C315 C215 111.0(4) . . ? C515 C315 C215 106.7(3) . . ? C116 O116 Mn10 131.5(2) . . ? C116 O216 Mn11 122.2(2) . . ? O116 C116 O216 123.8(3) . . ? O116 C116 C216 118.6(3) . . ? O216 C116 C216 117.6(3) . . ? C116 C216 C316 116.4(3) . . ? C416 C316 C516 109.9(4) . . ? C416 C316 C616 108.7(4) . . ? C516 C316 C616 109.5(3) . . ? C416 C316 C216 111.8(3) . . ? C516 C316 C216 109.1(4) . . ? C616 C316 C216 107.8(4) . . ? C117 O117 Mn10 132.4(2) . . ? C117 O217 Mn11 132.0(2) . . ? O117 C117 O217 125.2(3) . . ? O117 C117 C217 117.0(3) . . ? O217 C117 C217 117.7(3) . . ? C117 C217 C317 113.9(3) . . ? C517 C317 C417 110.8(5) . . ? C517 C317 C217 111.3(4) . . ? C417 C317 C217 107.6(4) . . ? C517 C317 C617 108.0(5) . . ? C417 C317 C617 107.8(4) . . ? C217 C317 C617 111.2(4) . . ? C118 O118 Mn3 124.8(2) . . ? C118 O218 Mn11 123.9(2) . . ? O218 C118 O118 125.3(3) . . ? O218 C118 C218 120.3(3) . . ? O118 C118 C218 114.4(3) . . ? C318 C218 C118 118.2(4) . . ? C218 C318 C518 113.6(4) . . ? C218 C318 C618 110.0(4) . . ? C518 C318 C618 108.4(5) . . ? C218 C318 C418 107.7(4) . . ? C518 C318 C418 109.2(4) . . ? C618 C318 C418 107.8(4) . . ? O3A N1A O2A 124.5(5) . . ? O3A N1A C1A 117.4(4) . . ? O2A N1A C1A 118.1(5) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.935 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.090 data_mnjtrt #TrackingRef 'all_revised.cif' _database_code_depnum_ccdc_archive 'CCDC 755026' #Crystal at RT before application of high pressure. _audit_creation_method SHELXL-97 _audit_creation_date 09-11-01 _chemical_compound_source 'Pascal Parois & Mark Murrie ' _exptl_crystal_recrystallization_method ; >From MeNO2/CH2Cl2. Crystal at RT before application of high pressure. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn12O12(tBuCH2CO2)16(H2O)4].MeNO2.CH2Cl2' _chemical_formula_sum 'C98 H189 Cl2 Mn12 N O50' _chemical_formula_weight 2911.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0005 0.0007 '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 0.0015 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0034 0.0025 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.2230 0.3472 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.0750 0.0720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.099(4) _cell_length_b 16.702(4) _cell_length_c 27.570(6) _cell_angle_alpha 76.585(4) _cell_angle_beta 78.042(4) _cell_angle_gamma 77.809(4) _cell_volume 6950(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9562 _cell_measurement_theta_min 2 _cell_measurement_theta_max 17 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3036 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5943 _exptl_absorpt_correction_T_max 0.7441 _exptl_absorpt_process_details Sadabs _exptl_special_details ; On Station 9.8 at Daresbury. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.47800 _diffrn_radiation_type ? _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 68279 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 17.33 _reflns_number_total 27434 _reflns_number_gt 19784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex' _computing_cell_refinement 'Bruker Saint' _computing_data_reduction 'Bruker Saint' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.000 0.500 0.000 21 1 ' ' 2 0.208 0.703 0.354 135 40 CH2Cl2 3 0.178 0.905 0.985 7 1 ' ' 4 0.305 0.955 0.023 11 1 ' ' 5 0.440 0.626 0.460 18 7 ' ' 6 0.560 0.374 0.540 18 7 ' ' 7 0.792 0.297 0.646 135 41 CH2Cl2 8 0.695 0.045 0.977 11 1 ' ' 9 0.821 0.095 0.015 7 1 ' ' _platon_squeeze_details ; ; _refine_special_details ; Data set taken before compression. The model is identical to that refined for the data set measured after compression. CH2tBu ligands #5, 8 and 17 are disordered. #5 and 8 have the entire CH2tBu group in two orientations. in #17 the tBu group is in two positions. Occupancies were refined. In the case of ligand #17, where the disorder components are in the occupancy ratio ~80:20, the minor component atoms were refined with a common U[iso]. All carboxylate ligands were restrained to have similar bond distances and angles. The tBu groups were restrained to have local 3-fold symmetry. The displacement ellipsoids of the CH2tBu groups vary between 0.054 (C27) and 0.310 (C65'). and only the Mn and O atoms were refined with adps. The aim of this experiment wass to determine the coordination geometry about Mn8 at RT before compression. 201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 96 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.06 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.17 Ratio 220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.86 Ratio 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbours of N1A See comments above 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C33 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C35' 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C38 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C312 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C318 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C38' 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C36 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C39 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C310 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C311 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C314 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C315 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C316 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C317 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn6 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn8 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn10 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn12 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C13 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C34 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C37 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C217 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C313 C3xx are pivot atoms of tBu groups. 241_ALERT_2_B Check High Ueq as Compared to Neighbors for C212 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O13 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O14 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O18 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O25 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O26 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O110 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O111 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O210 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O211 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O214 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C23 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C29 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C218 These are either O-atoms attached to Mn: even the O-atoms show quite high thermal motion in this structure. C2xx are 'pivot' CH2 groups. These will tend to show higher thermal motion than the attached O-atoms or the pivot C atoms of the tBu groups. 420_ALERT_2_B D-H Without Acceptor O10 - H101 ... ? 420_ALERT_2_B D-H Without Acceptor O120 - H121 ... ? 420_ALERT_2_B D-H Without Acceptor O121 - *H124 ... ? 420_ALERT_2_B D-H Without Acceptor O121 - *H125 ... ? Noted, but no action taken. The H-positions on oxygen are based on those from the LT (150K) structure. 601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 136.00 A**3 See above 084_ALERT_2_C High R2 Value .................................. 0.27 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 11 083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large. 5.54 Not a precise structure. This is because of the high thermal motion. 432_ALERT_2_C Short Inter X...Y Contact C43 .. C58' .. 3.12 Ang. C58' is disordered, and C43 has quite a high thermal parameter, and may be disordered in sympathy with C58'. If present this disorder has not be resolved. 910_ALERT_3_B Missing # of FCF Reflections Below Th(Min) ..... 15 029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 614 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 7 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 74 301_ALERT_3_G Note Main Residue Disorder .................... 8.00 Perc. See above. 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? No action taken. 041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? 043_ALERT_1_C Check Reported Molecular Weight ................ 2887.80 044_ALERT_1_C Calculated and Reported Dx Differ .............. ? The calculated values assume one extra MeNO2 per formula unit. 731_ALERT_1_C Bond Calc 1.523(15), Rep 1.522(7) ...... 2.14 su-Ra C33 -C63 1.555 1.555 731_ALERT_1_C Bond Calc 1.522(15), Rep 1.524(7) ...... 2.14 su-Ra C33 -C53 1.555 1.555 731_ALERT_1_C Bond Calc 1.510(13), Rep 1.511(6) ...... 2.17 su-Ra C36 -C56 1.555 1.555 731_ALERT_1_C Bond Calc 1.513(13), Rep 1.513(6) ...... 2.17 su-Ra C39 -C49 1.555 1.555 731_ALERT_1_C Bond Calc 1.534(15), Rep 1.532(6) ...... 2.50 su-Ra C39 -C69 1.555 1.555 731_ALERT_1_C Bond Calc 1.509(15), Rep 1.510(7) ...... 2.14 su-Ra C310 -C410 1.555 1.555 731_ALERT_1_C Bond Calc 1.514(15), Rep 1.514(7) ...... 2.14 su-Ra C310 -C510 1.555 1.555 731_ALERT_1_C Bond Calc 1.519(15), Rep 1.518(7) ...... 2.14 su-Ra C310 -C610 1.555 1.555 731_ALERT_1_C Bond Calc 1.515(14), Rep 1.516(6) ...... 2.33 su-Ra C311 -C611 1.555 1.555 731_ALERT_1_C Bond Calc 1.517(15), Rep 1.517(7) ...... 2.14 su-Ra C312 -C412 1.555 1.555 731_ALERT_1_C Bond Calc 1.521(15), Rep 1.521(7) ...... 2.14 su-Ra C312 -C512 1.555 1.555 731_ALERT_1_C Bond Calc 1.517(13), Rep 1.516(6) ...... 2.17 su-Ra C313 -C513 1.555 1.555 731_ALERT_1_C Bond Calc 1.513(15), Rep 1.513(7) ...... 2.14 su-Ra C318 -C618 1.555 1.555 731_ALERT_1_C Bond Calc 1.518(13), Rep 1.519(6) ...... 2.17 su-Ra C318 -C418 1.555 1.555 731_ALERT_1_C Bond Calc 1.526(16), Rep 1.526(7) ...... 2.29 su-Ra C318 -C518 1.555 1.555 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 4866 The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif can be badly in error. 926_ALERT_1_C Reported and Calculated R1 * 100.0 Differ by . -0.32 Suspect this is because calculation in Platon used all data. Very low angle data were omitted from refinement to avoid beam-stop problems. 092_ALERT_4_G Check: Wavelength given is not Cu,Mo or Ag Ka .. 0.48 Ang. Synchrotron data. 154_ALERT_1_G The su's on the Cell Angles are Equal (x 10000) 400 Deg. 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 3 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 42.20 Deg. C25' -C15 -C25 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 32.40 Deg. C327 -C217 -C317 1.555 1.555 1.555 795_ALERT_4_G C-Atom in CIF Coordinate List out of Sequence .. C14 796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence .. O107 ; _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^)+(0.1646P)^2^+5.5377P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 27434 _refine_ls_number_parameters 997 _refine_ls_number_restraints 4866 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.2692 _refine_ls_wR_factor_gt 0.2516 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.004 _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 0.41824(4) 0.19963(5) 0.23177(3) 0.03475(18) Uani 1 1 d . . . Mn2 Mn 0.29841(4) 0.08731(5) 0.26212(3) 0.03568(18) Uani 1 1 d . . . Mn3 Mn 0.25336(4) 0.23839(5) 0.19403(3) 0.03449(18) Uani 1 1 d . . . Mn4 Mn 0.25967(5) 0.24967(5) 0.29326(3) 0.03809(19) Uani 1 1 d . . . Mn5 Mn 0.23532(5) 0.40281(6) 0.32338(3) 0.0514(2) Uani 1 1 d . . . Mn6 Mn 0.43584(5) 0.29950(6) 0.32412(3) 0.0528(2) Uani 1 1 d . . . Mn7 Mn 0.57972(5) 0.16135(5) 0.26053(3) 0.0445(2) Uani 1 1 d . . . Mn8 Mn 0.51433(5) -0.00962(5) 0.24769(3) 0.0462(2) Uani 1 1 d . . . Mn9 Mn 0.33204(5) -0.06940(5) 0.23821(3) 0.0440(2) Uani 1 1 d . . . Mn10 Mn 0.17967(5) 0.07008(5) 0.17611(3) 0.04055(19) Uani 1 1 d . . . Mn11 Mn 0.09360(5) 0.27166(5) 0.16232(3) 0.04073(19) Uani 1 1 d . . . Mn12 Mn 0.11522(5) 0.40423(5) 0.23428(3) 0.0477(2) Uani 1 1 d . . . O6 O 0.4196(4) 0.1803(4) 0.38189(18) 0.0858(16) Uani 1 1 d . . . H61 H 0.4718 0.1511 0.3804 0.129 Uiso 1 1 d R . . H62 H 0.3880 0.1605 0.3715 0.129 Uiso 1 1 d R . . O10 O 0.2942(3) 0.0598(4) 0.11312(17) 0.0914(18) Uani 1 1 d . . . H101 H 0.3049 0.1086 0.1112 0.137 Uiso 1 1 d R . . H102 H 0.3358 0.0266 0.1253 0.137 Uiso 1 1 d R . . O120 O 0.0067(3) 0.3407(3) 0.28090(18) 0.0701(12) Uani 1 1 d . . . H120 H 0.0020 0.2974 0.2708 0.105 Uiso 1 1 d R . . H121 H 0.0254 0.3219 0.3086 0.105 Uiso 1 1 d R . . O121 O 0.2212(4) 0.4706(3) 0.18929(19) 0.0833(15) Uani 1 1 d . . . H123 H 0.2596 0.4852 0.2041 0.125 Uiso 1 1 d R . . H124 H 0.2594 0.4318 0.1723 0.125 Uiso 0.50 1 d PR . . H125 H 0.1933 0.4996 0.1764 0.125 Uiso 0.50 1 d PR . . O107 O 0.4770(2) 0.2421(2) 0.27001(13) 0.0428(8) Uani 1 1 d . . . O108 O 0.5082(2) 0.1098(2) 0.23618(13) 0.0406(7) Uani 1 1 d . . . O123 O 0.35023(19) 0.1511(2) 0.20010(11) 0.0332(6) Uani 1 1 d . . . O124 O 0.3485(2) 0.1531(2) 0.29316(11) 0.0367(7) Uani 1 1 d . . . O134 O 0.3182(2) 0.2860(2) 0.22734(12) 0.0359(7) Uani 1 1 d . . . O208 O 0.3885(2) -0.0023(2) 0.26174(13) 0.0413(7) Uani 1 1 d . . . O209 O 0.2521(2) 0.0312(2) 0.22555(12) 0.0399(7) Uani 1 1 d . . . O234 O 0.2110(2) 0.1866(2) 0.26041(12) 0.0373(7) Uani 1 1 d . . . O310 O 0.1889(2) 0.1832(2) 0.16750(12) 0.0381(7) Uani 1 1 d . . . O311 O 0.1538(2) 0.3196(2) 0.19715(13) 0.0403(7) Uani 1 1 d . . . O405 O 0.1819(2) 0.3519(2) 0.28549(13) 0.0447(8) Uani 1 1 d . . . O406 O 0.3189(2) 0.3060(2) 0.32156(13) 0.0456(8) Uani 1 1 d . . . O13 O 0.5320(3) -0.1343(3) 0.2581(2) 0.0817(16) Uani 1 1 d D . . O23 O 0.4087(3) -0.1734(3) 0.25750(19) 0.0646(11) Uani 1 1 d D . . C13 C 0.4852(3) -0.1878(3) 0.2634(2) 0.0623(15) Uiso 1 1 d D . . C23 C 0.5289(5) -0.2784(4) 0.2741(3) 0.096(3) Uiso 1 1 d D . . H23A H 0.4849 -0.3130 0.2803 0.116 Uiso 1 1 calc R . . H23B H 0.5678 -0.2897 0.2436 0.116 Uiso 1 1 calc R . . C33 C 0.5793(5) -0.3067(5) 0.3175(3) 0.098(3) Uiso 1 1 d D . . C43 C 0.6023(9) -0.4013(5) 0.3287(5) 0.166(6) Uiso 1 1 d D . . H43A H 0.5505 -0.4250 0.3377 0.250 Uiso 1 1 calc R . . H43B H 0.6343 -0.4189 0.3562 0.250 Uiso 1 1 calc R . . H43C H 0.6368 -0.4200 0.2992 0.250 Uiso 1 1 calc R . . C53 C 0.5277(9) -0.2775(10) 0.3650(4) 0.211(8) Uiso 1 1 d D . . H53A H 0.5150 -0.2175 0.3586 0.316 Uiso 1 1 calc R . . H53B H 0.5606 -0.2971 0.3921 0.316 Uiso 1 1 calc R . . H53C H 0.4748 -0.2994 0.3744 0.316 Uiso 1 1 calc R . . C63 C 0.6624(7) -0.2707(9) 0.3045(6) 0.193(7) Uiso 1 1 d D . . H63A H 0.6489 -0.2108 0.2971 0.289 Uiso 1 1 calc R . . H63B H 0.6978 -0.2900 0.2755 0.289 Uiso 1 1 calc R . . H63C H 0.6928 -0.2885 0.3327 0.289 Uiso 1 1 calc R . . O14 O 0.5268(3) -0.0085(3) 0.17340(17) 0.0705(12) Uani 1 1 d D . . O24 O 0.4113(2) -0.0516(3) 0.16275(15) 0.0553(9) Uani 1 1 d D . . C14 C 0.4847(3) -0.0320(3) 0.14730(18) 0.0501(12) Uiso 1 1 d D . . C24 C 0.5261(4) -0.0351(3) 0.0933(2) 0.0666(16) Uiso 1 1 d D . . H24A H 0.5765 -0.0083 0.0856 0.080 Uiso 1 1 calc R . . H24B H 0.4859 -0.0022 0.0714 0.080 Uiso 1 1 calc R . . C34 C 0.5535(4) -0.1208(4) 0.0800(2) 0.0702(17) Uiso 1 1 d D . . C44 C 0.6068(6) -0.1797(6) 0.1174(4) 0.118(3) Uiso 1 1 d D . . H44A H 0.5727 -0.1862 0.1506 0.177 Uiso 1 1 calc R . . H44B H 0.6567 -0.1571 0.1176 0.177 Uiso 1 1 calc R . . H44C H 0.6245 -0.2332 0.1077 0.177 Uiso 1 1 calc R . . C54 C 0.6064(6) -0.1109(6) 0.0267(3) 0.100(3) Uiso 1 1 d D . . H54A H 0.5734 -0.0710 0.0037 0.150 Uiso 1 1 calc R . . H54B H 0.6205 -0.1638 0.0162 0.150 Uiso 1 1 calc R . . H54C H 0.6585 -0.0916 0.0267 0.150 Uiso 1 1 calc R . . C64 C 0.4747(5) -0.1572(6) 0.0798(4) 0.112(3) Uiso 1 1 d D . . H64A H 0.4395 -0.1191 0.0573 0.168 Uiso 1 1 calc R . . H64B H 0.4420 -0.1661 0.1134 0.168 Uiso 1 1 calc R . . H64C H 0.4927 -0.2095 0.0687 0.168 Uiso 1 1 calc R . . O15 O 0.6858(3) 0.0867(3) 0.24359(19) 0.0673(12) Uani 1 1 d D A . O25 O 0.6448(3) -0.0264(3) 0.2335(3) 0.0920(18) Uani 1 1 d D A . C15 C 0.7006(4) 0.0172(4) 0.2304(3) 0.0768(19) Uiso 1 1 d D . . C25 C 0.7877(6) 0.0093(7) 0.1955(5) 0.073(5) Uiso 0.433(14) 1 d PD A 1 H25A H 0.7800 0.0453 0.1630 0.088 Uiso 0.433(14) 1 calc PR A 1 H25B H 0.8267 0.0316 0.2093 0.088 Uiso 0.433(14) 1 calc PR A 1 C35 C 0.8318(7) -0.0753(7) 0.1858(5) 0.097(3) Uiso 0.433(14) 1 d PD A 1 C45 C 0.7792(10) -0.1042(11) 0.1555(7) 0.086(6) Uiso 0.433(14) 1 d PD A 1 H45A H 0.8055 -0.1591 0.1499 0.129 Uiso 0.433(14) 1 calc PR A 1 H45B H 0.7771 -0.0662 0.1236 0.129 Uiso 0.433(14) 1 calc PR A 1 H45C H 0.7218 -0.1054 0.1739 0.129 Uiso 0.433(14) 1 calc PR A 1 C55 C 0.9221(8) -0.0722(12) 0.1559(7) 0.090(6) Uiso 0.433(14) 1 d PD A 1 H55A H 0.9544 -0.0500 0.1738 0.136 Uiso 0.433(14) 1 calc PR A 1 H55B H 0.9186 -0.0370 0.1233 0.136 Uiso 0.433(14) 1 calc PR A 1 H55C H 0.9502 -0.1275 0.1520 0.136 Uiso 0.433(14) 1 calc PR A 1 C65 C 0.8365(15) -0.1354(12) 0.2361(6) 0.131(10) Uiso 0.433(14) 1 d PD A 1 H65A H 0.8711 -0.1175 0.2547 0.196 Uiso 0.433(14) 1 calc PR A 1 H65B H 0.8618 -0.1905 0.2303 0.196 Uiso 0.433(14) 1 calc PR A 1 H65C H 0.7795 -0.1361 0.2552 0.196 Uiso 0.433(14) 1 calc PR A 1 C25' C 0.7901(5) -0.0354(7) 0.2315(5) 0.090(5) Uiso 0.567(14) 1 d PD A 2 H25C H 0.8291 -0.0004 0.2344 0.108 Uiso 0.567(14) 1 calc PR A 2 H25D H 0.7877 -0.0793 0.2615 0.108 Uiso 0.567(14) 1 calc PR A 2 C35' C 0.8272(7) -0.0751(8) 0.1858(5) 0.097(3) Uiso 0.567(14) 1 d PD A 2 C45' C 0.7822(13) -0.1480(12) 0.1889(9) 0.160(10) Uiso 0.567(14) 1 d PD A 2 H45D H 0.8052 -0.1730 0.1598 0.240 Uiso 0.567(14) 1 calc PR A 2 H45E H 0.7215 -0.1282 0.1898 0.240 Uiso 0.567(14) 1 calc PR A 2 H45F H 0.7916 -0.1887 0.2190 0.240 Uiso 0.567(14) 1 calc PR A 2 C55' C 0.9222(7) -0.1097(12) 0.1854(8) 0.124(7) Uiso 0.567(14) 1 d PD A 2 H55D H 0.9453 -0.1337 0.1559 0.186 Uiso 0.567(14) 1 calc PR A 2 H55E H 0.9293 -0.1519 0.2152 0.186 Uiso 0.567(14) 1 calc PR A 2 H55F H 0.9522 -0.0654 0.1848 0.186 Uiso 0.567(14) 1 calc PR A 2 C65' C 0.8126(19) -0.0125(15) 0.1376(7) 0.31(3) Uiso 0.567(14) 1 d PD A 2 H65D H 0.8370 -0.0383 0.1090 0.466 Uiso 0.567(14) 1 calc PR A 2 H65E H 0.8397 0.0345 0.1354 0.466 Uiso 0.567(14) 1 calc PR A 2 H65F H 0.7518 0.0060 0.1380 0.466 Uiso 0.567(14) 1 calc PR A 2 O16 O 0.5586(3) 0.0816(3) 0.33609(15) 0.0613(10) Uani 1 1 d D . . O26 O 0.5219(3) -0.0310(3) 0.32157(18) 0.0738(13) Uani 1 1 d D . . C16 C 0.5413(4) 0.0087(3) 0.34977(19) 0.0564(14) Uiso 1 1 d D . . C26 C 0.5437(4) -0.0345(4) 0.4042(2) 0.0701(17) Uiso 1 1 d D . . H26A H 0.5197 -0.0852 0.4101 0.084 Uiso 1 1 calc R . . H26B H 0.5059 0.0014 0.4256 0.084 Uiso 1 1 calc R . . C36 C 0.6306(4) -0.0578(4) 0.4216(2) 0.0716(18) Uiso 1 1 d D . . C46 C 0.6187(6) -0.1103(6) 0.4747(3) 0.108(3) Uiso 1 1 d D . . H46A H 0.5785 -0.0782 0.4969 0.162 Uiso 1 1 calc R . . H46B H 0.6731 -0.1263 0.4864 0.162 Uiso 1 1 calc R . . H46C H 0.5970 -0.1594 0.4743 0.162 Uiso 1 1 calc R . . C56 C 0.6959(6) -0.1053(7) 0.3860(4) 0.132(4) Uiso 1 1 d D . . H56A H 0.6758 -0.1546 0.3842 0.198 Uiso 1 1 calc R . . H56B H 0.7499 -0.1210 0.3981 0.198 Uiso 1 1 calc R . . H56C H 0.7034 -0.0705 0.3529 0.198 Uiso 1 1 calc R . . C66 C 0.6624(6) 0.0210(5) 0.4239(4) 0.115(3) Uiso 1 1 d D . . H66A H 0.6201 0.0522 0.4457 0.173 Uiso 1 1 calc R . . H66B H 0.6715 0.0546 0.3906 0.173 Uiso 1 1 calc R . . H66C H 0.7156 0.0055 0.4370 0.173 Uiso 1 1 calc R . . O17 O 0.4728(2) 0.2535(2) 0.16845(12) 0.0437(8) Uani 1 1 d D . . O27 O 0.6079(2) 0.2320(3) 0.18273(14) 0.0541(9) Uani 1 1 d D . . C17 C 0.5527(3) 0.2562(3) 0.15444(16) 0.0439(11) Uiso 1 1 d D . . C27 C 0.5792(4) 0.2921(3) 0.09905(17) 0.0545(13) Uiso 1 1 d D . . H27A H 0.6320 0.3140 0.0950 0.065 Uiso 1 1 calc R . . H27B H 0.5349 0.3385 0.0885 0.065 Uiso 1 1 calc R . . C37 C 0.5935(3) 0.2298(3) 0.0642(2) 0.0610(15) Uiso 1 1 d D . . C47 C 0.6215(6) 0.2752(6) 0.0108(3) 0.112(3) Uiso 1 1 d D . . H47A H 0.5779 0.3224 0.0019 0.169 Uiso 1 1 calc R . . H47B H 0.6296 0.2380 -0.0123 0.169 Uiso 1 1 calc R . . H47C H 0.6747 0.2940 0.0089 0.169 Uiso 1 1 calc R . . C57 C 0.5108(4) 0.1979(5) 0.0667(3) 0.081(2) Uiso 1 1 d D . . H57A H 0.4912 0.1720 0.1009 0.121 Uiso 1 1 calc R . . H57B H 0.5214 0.1577 0.0453 0.121 Uiso 1 1 calc R . . H57C H 0.4676 0.2438 0.0555 0.121 Uiso 1 1 calc R . . C67 C 0.6616(5) 0.1559(5) 0.0804(4) 0.104(3) Uiso 1 1 d D . . H67A H 0.6424 0.1287 0.1144 0.156 Uiso 1 1 calc R . . H67B H 0.7144 0.1751 0.0790 0.156 Uiso 1 1 calc R . . H67C H 0.6712 0.1171 0.0582 0.156 Uiso 1 1 calc R . . O18 O 0.5517(3) 0.2887(4) 0.3372(2) 0.0943(19) Uani 1 1 d D B . O28 O 0.6494(2) 0.2210(3) 0.28437(18) 0.0689(13) Uani 1 1 d D B . C18 C 0.6281(4) 0.2693(5) 0.3148(3) 0.090(2) Uiso 1 1 d D . . C28 C 0.6912(7) 0.3256(7) 0.3157(4) 0.084(4) Uiso 0.601(13) 1 d PD B 1 H28A H 0.7460 0.3074 0.2956 0.101 Uiso 0.601(13) 1 calc PR B 1 H28B H 0.6695 0.3822 0.2997 0.101 Uiso 0.601(13) 1 calc PR B 1 C38 C 0.7065(6) 0.3269(6) 0.3673(4) 0.058(3) Uiso 0.601(13) 1 d PD B 1 C48 C 0.6260(7) 0.3732(9) 0.3961(5) 0.101(5) Uiso 0.601(13) 1 d PD B 1 H48A H 0.6126 0.4293 0.3775 0.151 Uiso 0.601(13) 1 calc PR B 1 H48B H 0.6365 0.3748 0.4289 0.151 Uiso 0.601(13) 1 calc PR B 1 H48C H 0.5784 0.3448 0.3998 0.151 Uiso 0.601(13) 1 calc PR B 1 C58 C 0.7816(8) 0.3695(11) 0.3657(6) 0.117(6) Uiso 0.601(13) 1 d PD B 1 H58A H 0.7653 0.4288 0.3551 0.176 Uiso 0.601(13) 1 calc PR B 1 H58B H 0.8299 0.3492 0.3422 0.176 Uiso 0.601(13) 1 calc PR B 1 H58C H 0.7972 0.3576 0.3987 0.176 Uiso 0.601(13) 1 calc PR B 1 C68 C 0.7215(16) 0.2377(8) 0.3972(8) 0.251(19) Uiso 0.601(13) 1 d PD B 1 H68A H 0.7698 0.2055 0.3794 0.377 Uiso 0.601(13) 1 calc PR B 1 H68B H 0.6710 0.2133 0.4011 0.377 Uiso 0.601(13) 1 calc PR B 1 H68C H 0.7331 0.2380 0.4299 0.377 Uiso 0.601(13) 1 calc PR B 1 C28' C 0.6969(8) 0.2547(10) 0.3486(6) 0.090(7) Uiso 0.399(13) 1 d PD B 2 H28C H 0.6965 0.2000 0.3702 0.108 Uiso 0.399(13) 1 calc PR B 2 H28D H 0.7528 0.2534 0.3270 0.108 Uiso 0.399(13) 1 calc PR B 2 C38' C 0.6881(8) 0.3176(8) 0.3817(5) 0.062(5) Uiso 0.399(13) 1 d PD B 2 C48' C 0.6258(15) 0.294(2) 0.4297(8) 0.22(2) Uiso 0.399(13) 1 d PD B 2 H48D H 0.6196 0.3334 0.4510 0.325 Uiso 0.399(13) 1 calc PR B 2 H48E H 0.6476 0.2391 0.4471 0.325 Uiso 0.399(13) 1 calc PR B 2 H48F H 0.5708 0.2939 0.4213 0.325 Uiso 0.399(13) 1 calc PR B 2 C58' C 0.6550(18) 0.4047(10) 0.3543(11) 0.171(16) Uiso 0.399(13) 1 d PD B 2 H58D H 0.6490 0.4438 0.3760 0.257 Uiso 0.399(13) 1 calc PR B 2 H58E H 0.6000 0.4058 0.3456 0.257 Uiso 0.399(13) 1 calc PR B 2 H58F H 0.6950 0.4197 0.3241 0.257 Uiso 0.399(13) 1 calc PR B 2 C68' C 0.7767(9) 0.3152(11) 0.3941(7) 0.071(5) Uiso 0.399(13) 1 d PD B 2 H68D H 0.7723 0.3544 0.4155 0.106 Uiso 0.399(13) 1 calc PR B 2 H68E H 0.8159 0.3298 0.3634 0.106 Uiso 0.399(13) 1 calc PR B 2 H68F H 0.7978 0.2600 0.4113 0.106 Uiso 0.399(13) 1 calc PR B 2 O19 O 0.3107(3) 0.4743(3) 0.25945(18) 0.0671(11) Uani 1 1 d D . . O29 O 0.4415(3) 0.4180(3) 0.2791(2) 0.0786(14) Uani 1 1 d D . . C19 C 0.3913(4) 0.4718(4) 0.2553(3) 0.081(2) Uiso 1 1 d D . . C29 C 0.4309(5) 0.5447(5) 0.2220(3) 0.102(3) Uiso 1 1 d D . . H29A H 0.3847 0.5884 0.2109 0.122 Uiso 1 1 calc R . . H29B H 0.4597 0.5668 0.2424 0.122 Uiso 1 1 calc R . . C39 C 0.4948(4) 0.5257(4) 0.1758(3) 0.082(2) Uiso 1 1 d D . . C49 C 0.5224(8) 0.6053(6) 0.1437(4) 0.142(4) Uiso 1 1 d D . . H49A H 0.4723 0.6461 0.1369 0.214 Uiso 1 1 calc R . . H49B H 0.5568 0.5939 0.1124 0.214 Uiso 1 1 calc R . . H49C H 0.5557 0.6265 0.1615 0.214 Uiso 1 1 calc R . . C59 C 0.5723(6) 0.4609(6) 0.1875(4) 0.130(4) Uiso 1 1 d D . . H59A H 0.5537 0.4104 0.2072 0.196 Uiso 1 1 calc R . . H59B H 0.6046 0.4813 0.2062 0.196 Uiso 1 1 calc R . . H59C H 0.6079 0.4495 0.1565 0.196 Uiso 1 1 calc R . . C69 C 0.4443(8) 0.4921(8) 0.1457(5) 0.153(5) Uiso 1 1 d D . . H69A H 0.4268 0.4411 0.1653 0.230 Uiso 1 1 calc R . . H69B H 0.4803 0.4815 0.1146 0.230 Uiso 1 1 calc R . . H69C H 0.3943 0.5326 0.1384 0.230 Uiso 1 1 calc R . . O110 O 0.2842(3) 0.4460(3) 0.36905(19) 0.0779(15) Uani 1 1 d D . . O210 O 0.4051(3) 0.3555(3) 0.3824(2) 0.0829(16) Uani 1 1 d D . . C110 C 0.3513(4) 0.4203(4) 0.3888(3) 0.0736(18) Uiso 1 1 d D . . C210 C 0.3627(5) 0.4676(5) 0.4272(3) 0.087(2) Uiso 1 1 d D . . H21A H 0.4229 0.4554 0.4311 0.104 Uiso 1 1 calc R . . H21B H 0.3488 0.5271 0.4139 0.104 Uiso 1 1 calc R . . C310 C 0.3083(6) 0.4475(6) 0.4788(3) 0.117(3) Uiso 1 1 d D . . C410 C 0.3335(8) 0.4876(8) 0.5161(4) 0.144(4) Uiso 1 1 d D . . H41A H 0.2954 0.4781 0.5479 0.216 Uiso 1 1 calc R . . H41B H 0.3296 0.5466 0.5033 0.216 Uiso 1 1 calc R . . H41C H 0.3916 0.4637 0.5209 0.216 Uiso 1 1 calc R . . C510 C 0.3192(12) 0.3543(6) 0.4993(6) 0.254(11) Uiso 1 1 d D . . H51A H 0.2794 0.3432 0.5302 0.381 Uiso 1 1 calc R . . H51B H 0.3771 0.3338 0.5057 0.381 Uiso 1 1 calc R . . H51C H 0.3081 0.3267 0.4749 0.381 Uiso 1 1 calc R . . C610 C 0.2142(6) 0.4803(9) 0.4742(5) 0.171(6) Uiso 1 1 d D . . H61A H 0.1789 0.4669 0.5065 0.257 Uiso 1 1 calc R . . H61B H 0.1984 0.4548 0.4503 0.257 Uiso 1 1 calc R . . H61C H 0.2060 0.5398 0.4627 0.257 Uiso 1 1 calc R . . O111 O 0.0667(3) 0.4990(3) 0.26725(19) 0.0770(14) Uani 1 1 d D . . O211 O 0.1455(3) 0.5003(3) 0.32434(18) 0.0720(13) Uani 1 1 d D . . C111 C 0.0849(4) 0.5297(4) 0.3003(2) 0.0610(15) Uiso 1 1 d D . . C211 C 0.0256(4) 0.6090(4) 0.3123(2) 0.078(2) Uiso 1 1 d D . . H21C H -0.0029 0.6359 0.2835 0.093 Uiso 1 1 calc R . . H21D H 0.0605 0.6468 0.3166 0.093 Uiso 1 1 calc R . . C311 C -0.0428(4) 0.5954(4) 0.3593(3) 0.085(2) Uiso 1 1 d D . . C411 C -0.0971(6) 0.6806(5) 0.3652(4) 0.125(4) Uiso 1 1 d D . . H41D H -0.0610 0.7166 0.3696 0.188 Uiso 1 1 calc R . . H41E H -0.1416 0.6737 0.3942 0.188 Uiso 1 1 calc R . . H41F H -0.1228 0.7051 0.3355 0.188 Uiso 1 1 calc R . . C511 C -0.0016(7) 0.5577(7) 0.4060(3) 0.136(4) Uiso 1 1 d D . . H51D H 0.0358 0.5932 0.4093 0.204 Uiso 1 1 calc R . . H51E H 0.0312 0.5035 0.4029 0.204 Uiso 1 1 calc R . . H51F H -0.0457 0.5526 0.4353 0.204 Uiso 1 1 calc R . . C611 C -0.1000(7) 0.5379(7) 0.3537(5) 0.148(5) Uiso 1 1 d D . . H61D H -0.1253 0.5609 0.3237 0.221 Uiso 1 1 calc R . . H61E H -0.1448 0.5326 0.3826 0.221 Uiso 1 1 calc R . . H61F H -0.0662 0.4839 0.3510 0.221 Uiso 1 1 calc R . . O112 O 0.1978(3) 0.2080(3) 0.35854(13) 0.0565(10) Uani 1 1 d D . . O212 O 0.1660(3) 0.3246(3) 0.38971(15) 0.0746(14) Uani 1 1 d D . . C112 C 0.1661(4) 0.2489(4) 0.3932(2) 0.0689(17) Uiso 1 1 d D . . C212 C 0.1318(5) 0.1969(5) 0.4432(3) 0.118(3) Uiso 1 1 d D . . H21E H 0.1250 0.1443 0.4365 0.141 Uiso 1 1 calc R . . H21F H 0.1759 0.1841 0.4643 0.141 Uiso 1 1 calc R . . C312 C 0.0487(4) 0.2310(4) 0.4737(2) 0.0739(18) Uiso 1 1 d D . . C412 C -0.0205(8) 0.2620(9) 0.4406(5) 0.188(7) Uiso 1 1 d D . . H41G H -0.0013 0.3031 0.4121 0.282 Uiso 1 1 calc R . . H41H H -0.0724 0.2867 0.4598 0.282 Uiso 1 1 calc R . . H41I H -0.0315 0.2160 0.4289 0.282 Uiso 1 1 calc R . . C512 C 0.0584(10) 0.3054(7) 0.4938(6) 0.209(8) Uiso 1 1 d D . . H51G H 0.0758 0.3483 0.4659 0.314 Uiso 1 1 calc R . . H51H H 0.1013 0.2882 0.5154 0.314 Uiso 1 1 calc R . . H51I H 0.0043 0.3266 0.5126 0.314 Uiso 1 1 calc R . . C612 C 0.0195(7) 0.1631(6) 0.5167(4) 0.130(4) Uiso 1 1 d D . . H61G H 0.0595 0.1475 0.5401 0.194 Uiso 1 1 calc R . . H61H H 0.0171 0.1153 0.5036 0.194 Uiso 1 1 calc R . . H61I H -0.0367 0.1834 0.5338 0.194 Uiso 1 1 calc R . . O113 O 0.0408(3) 0.4651(3) 0.18494(18) 0.0664(12) Uani 1 1 d D . . O213 O 0.0018(2) 0.3678(2) 0.15478(17) 0.0575(10) Uani 1 1 d D . . C113 C -0.0043(4) 0.4411(3) 0.1603(2) 0.0567(14) Uiso 1 1 d D . . C213 C -0.0703(4) 0.5077(4) 0.1350(2) 0.0712(18) Uiso 1 1 d D . . H21G H -0.1041 0.4804 0.1205 0.085 Uiso 1 1 calc R . . H21H H -0.0396 0.5434 0.1072 0.085 Uiso 1 1 calc R . . C313 C -0.1321(4) 0.5628(4) 0.1684(2) 0.0757(19) Uiso 1 1 d D . . C413 C -0.1681(7) 0.5076(6) 0.2170(3) 0.125(4) Uiso 1 1 d D . . H41J H -0.1938 0.4665 0.2089 0.188 Uiso 1 1 calc R . . H41K H -0.2108 0.5413 0.2371 0.188 Uiso 1 1 calc R . . H41L H -0.1223 0.4802 0.2356 0.188 Uiso 1 1 calc R . . C513 C -0.0871(7) 0.6248(6) 0.1809(4) 0.126(4) Uiso 1 1 d D . . H51J H -0.0667 0.6612 0.1504 0.190 Uiso 1 1 calc R . . H51K H -0.0393 0.5951 0.1973 0.190 Uiso 1 1 calc R . . H51L H -0.1270 0.6572 0.2031 0.190 Uiso 1 1 calc R . . C613 C -0.2043(5) 0.6110(5) 0.1397(3) 0.095(3) Uiso 1 1 d D . . H61J H -0.1813 0.6489 0.1106 0.142 Uiso 1 1 calc R . . H61K H -0.2471 0.6419 0.1614 0.142 Uiso 1 1 calc R . . H61L H -0.2301 0.5725 0.1291 0.142 Uiso 1 1 calc R . . O114 O 0.2640(3) -0.1353(2) 0.21778(17) 0.0570(10) Uani 1 1 d D . . O214 O 0.1650(3) -0.0431(2) 0.17898(18) 0.0674(12) Uani 1 1 d D . . C114 C 0.1976(3) -0.1154(3) 0.1975(2) 0.0481(12) Uiso 1 1 d D . . C214 C 0.1545(4) -0.1850(3) 0.1938(2) 0.0624(15) Uiso 1 1 d D . . H21I H 0.0933 -0.1637 0.1952 0.075 Uiso 1 1 calc R . . H21J H 0.1612 -0.2289 0.2234 0.075 Uiso 1 1 calc R . . C314 C 0.1859(4) -0.2238(4) 0.1475(2) 0.0739(18) Uiso 1 1 d D . . C414 C 0.2783(5) -0.2694(7) 0.1471(5) 0.137(4) Uiso 1 1 d D . . H41M H 0.2810 -0.3137 0.1763 0.206 Uiso 1 1 calc R . . H41N H 0.3146 -0.2310 0.1478 0.206 Uiso 1 1 calc R . . H41O H 0.2978 -0.2923 0.1171 0.206 Uiso 1 1 calc R . . C514 C 0.1279(6) -0.2865(6) 0.1495(4) 0.117(3) Uiso 1 1 d D . . H51M H 0.1298 -0.3277 0.1802 0.176 Uiso 1 1 calc R . . H51N H 0.1479 -0.3135 0.1210 0.176 Uiso 1 1 calc R . . H51O H 0.0698 -0.2578 0.1485 0.176 Uiso 1 1 calc R . . C614 C 0.1824(8) -0.1576(6) 0.0998(3) 0.132(4) Uiso 1 1 d D . . H61M H 0.2203 -0.1195 0.0985 0.198 Uiso 1 1 calc R . . H61N H 0.1245 -0.1276 0.0998 0.198 Uiso 1 1 calc R . . H61O H 0.2002 -0.1836 0.0709 0.198 Uiso 1 1 calc R . . O115 O 0.2402(2) 0.0381(2) 0.32592(13) 0.0500(9) Uani 1 1 d D . . O215 O 0.2596(3) -0.0942(2) 0.31624(15) 0.0590(10) Uani 1 1 d D . . C115 C 0.2350(4) -0.0390(3) 0.34167(18) 0.0513(13) Uiso 1 1 d D . . C215 C 0.1958(4) -0.0617(4) 0.39691(18) 0.0643(16) Uiso 1 1 d D . . H21K H 0.1697 -0.1109 0.4016 0.077 Uiso 1 1 calc R . . H21L H 0.1502 -0.0164 0.4051 0.077 Uiso 1 1 calc R . . C315 C 0.2585(4) -0.0790(4) 0.4339(2) 0.0695(17) Uiso 1 1 d D . . C415 C 0.3241(6) -0.1562(6) 0.4261(5) 0.139(4) Uiso 1 1 d D . . H41P H 0.2951 -0.2030 0.4315 0.208 Uiso 1 1 calc R . . H41Q H 0.3634 -0.1673 0.4496 0.208 Uiso 1 1 calc R . . H41R H 0.3554 -0.1474 0.3922 0.208 Uiso 1 1 calc R . . C515 C 0.2055(6) -0.0898(6) 0.4869(3) 0.114(3) Uiso 1 1 d D . . H51P H 0.1649 -0.0395 0.4904 0.171 Uiso 1 1 calc R . . H51Q H 0.2431 -0.1011 0.5114 0.171 Uiso 1 1 calc R . . H51R H 0.1751 -0.1355 0.4923 0.171 Uiso 1 1 calc R . . C615 C 0.3045(5) -0.0053(5) 0.4261(3) 0.091(2) Uiso 1 1 d D . . H61P H 0.2629 0.0438 0.4308 0.136 Uiso 1 1 calc R . . H61Q H 0.3368 0.0035 0.3925 0.136 Uiso 1 1 calc R . . H61R H 0.3430 -0.0168 0.4502 0.136 Uiso 1 1 calc R . . O116 O 0.0653(3) 0.0844(3) 0.22898(17) 0.0648(11) Uani 1 1 d D . . O216 O 0.0185(2) 0.2173(2) 0.23295(14) 0.0529(9) Uani 1 1 d D . . C116 C 0.0308(4) 0.1419(3) 0.2532(2) 0.0668(16) Uiso 1 1 d D . . C216 C 0.0098(5) 0.1172(4) 0.3108(2) 0.082(2) Uiso 1 1 d D . . H21M H 0.0635 0.0976 0.3239 0.099 Uiso 1 1 calc R . . H21N H -0.0190 0.1668 0.3240 0.099 Uiso 1 1 calc R . . C316 C -0.0465(4) 0.0503(4) 0.3305(2) 0.0673(17) Uiso 1 1 d D . . C416 C 0.0040(6) -0.0341(5) 0.3223(4) 0.107(3) Uiso 1 1 d D . . H41S H 0.0234 -0.0323 0.2868 0.161 Uiso 1 1 calc R . . H41T H -0.0323 -0.0757 0.3355 0.161 Uiso 1 1 calc R . . H41U H 0.0528 -0.0479 0.3395 0.161 Uiso 1 1 calc R . . C516 C -0.1238(6) 0.0743(7) 0.3031(4) 0.139(4) Uiso 1 1 d D . . H51S H -0.1564 0.1269 0.3099 0.208 Uiso 1 1 calc R . . H51T H -0.1596 0.0321 0.3148 0.208 Uiso 1 1 calc R . . H51U H -0.1042 0.0792 0.2674 0.208 Uiso 1 1 calc R . . C616 C -0.0784(7) 0.0459(7) 0.3868(3) 0.131(4) Uiso 1 1 d D . . H61S H -0.1116 0.0989 0.3923 0.196 Uiso 1 1 calc R . . H61T H -0.0300 0.0326 0.4042 0.196 Uiso 1 1 calc R . . H61U H -0.1138 0.0035 0.3993 0.196 Uiso 1 1 calc R . . O117 O 0.1142(3) 0.0965(2) 0.12012(15) 0.0586(10) Uani 1 1 d D . . O217 O 0.0388(2) 0.2249(2) 0.12153(15) 0.0533(9) Uani 1 1 d D . . C117 C 0.0592(3) 0.1581(3) 0.10521(19) 0.0494(12) Uiso 1 1 d D C . C217 C 0.0147(4) 0.1504(4) 0.0640(2) 0.0656(16) Uiso 1 1 d D . . H21O H -0.0468 0.1677 0.0736 0.079 Uiso 0.702(14) 1 calc PR C 1 H21P H 0.0245 0.0921 0.0615 0.079 Uiso 0.702(14) 1 calc PR C 1 H21Q H -0.0339 0.1959 0.0615 0.079 Uiso 0.298(14) 1 calc PR C 2 H21R H -0.0084 0.0988 0.0747 0.079 Uiso 0.298(14) 1 calc PR C 2 C317 C 0.0436(6) 0.2014(6) 0.0121(3) 0.091(4) Uiso 0.702(14) 1 d PD C 1 C417 C -0.0004(11) 0.1810(11) -0.0260(5) 0.146(8) Uiso 0.702(14) 1 d PD C 1 H41V H 0.0156 0.2144 -0.0587 0.219 Uiso 0.702(14) 1 calc PR C 1 H41W H -0.0618 0.1928 -0.0159 0.219 Uiso 0.702(14) 1 calc PR C 1 H41X H 0.0171 0.1229 -0.0276 0.219 Uiso 0.702(14) 1 calc PR C 1 C517 C 0.1407(7) 0.1818(11) -0.0027(7) 0.166(9) Uiso 0.702(14) 1 d PD C 1 H51V H 0.1583 0.2173 -0.0344 0.249 Uiso 0.702(14) 1 calc PR C 1 H51W H 0.1575 0.1244 -0.0061 0.249 Uiso 0.702(14) 1 calc PR C 1 H51X H 0.1678 0.1911 0.0229 0.249 Uiso 0.702(14) 1 calc PR C 1 C617 C 0.0154(10) 0.2938(6) 0.0128(5) 0.118(5) Uiso 0.702(14) 1 d PD C 1 H61V H 0.0357 0.3259 -0.0195 0.177 Uiso 0.702(14) 1 calc PR C 1 H61W H 0.0389 0.3075 0.0385 0.177 Uiso 0.702(14) 1 calc PR C 1 H61X H -0.0464 0.3064 0.0199 0.177 Uiso 0.702(14) 1 calc PR C 1 C327 C 0.0668(10) 0.1512(12) 0.0116(4) 0.115(7) Uiso 0.298(14) 1 d PD C 2 C427 C 0.0057(17) 0.154(2) -0.0242(7) 0.115(7) Uiso 0.298(14) 1 d PD C 2 H42A H 0.0374 0.1555 -0.0579 0.173 Uiso 0.298(14) 1 calc PR C 2 H42B H -0.0377 0.2033 -0.0237 0.173 Uiso 0.298(14) 1 calc PR C 2 H42C H -0.0212 0.1054 -0.0138 0.173 Uiso 0.298(14) 1 calc PR C 2 C527 C 0.1116(19) 0.2269(16) -0.0053(9) 0.115(7) Uiso 0.298(14) 1 d PD C 2 H52A H 0.1437 0.2271 -0.0388 0.173 Uiso 0.298(14) 1 calc PR C 2 H52B H 0.1501 0.2245 0.0176 0.173 Uiso 0.298(14) 1 calc PR C 2 H52C H 0.0693 0.2769 -0.0053 0.173 Uiso 0.298(14) 1 calc PR C 2 C627 C 0.1339(15) 0.0723(15) 0.0110(10) 0.115(7) Uiso 0.298(14) 1 d PD C 2 H62A H 0.1665 0.0736 -0.0224 0.173 Uiso 0.298(14) 1 calc PR C 2 H62B H 0.1057 0.0244 0.0209 0.173 Uiso 0.298(14) 1 calc PR C 2 H62C H 0.1719 0.0690 0.0343 0.173 Uiso 0.298(14) 1 calc PR C 2 O118 O 0.2975(2) 0.2971(2) 0.12811(13) 0.0478(8) Uani 1 1 d D . . O218 O 0.1760(3) 0.3288(3) 0.09429(14) 0.0595(10) Uani 1 1 d D . . C118 C 0.2530(3) 0.3326(4) 0.09323(19) 0.0556(14) Uiso 1 1 d D . . C218 C 0.3017(5) 0.3781(4) 0.0456(3) 0.092(2) Uiso 1 1 d D . . H21S H 0.3557 0.3845 0.0534 0.110 Uiso 1 1 calc R . . H21T H 0.3159 0.3421 0.0210 0.110 Uiso 1 1 calc R . . C318 C 0.2602(5) 0.4628(4) 0.0201(3) 0.090(2) Uiso 1 1 d D . . C418 C 0.3266(6) 0.5016(7) -0.0212(4) 0.127(4) Uiso 1 1 d D . . H41Y H 0.2997 0.5544 -0.0386 0.191 Uiso 1 1 calc R . . H41Z H 0.3495 0.4650 -0.0448 0.191 Uiso 1 1 calc R . . H411 H 0.3724 0.5098 -0.0065 0.191 Uiso 1 1 calc R . . C518 C 0.1871(8) 0.4540(10) -0.0047(6) 0.225(9) Uiso 1 1 d D . . H51Y H 0.1453 0.4273 0.0204 0.338 Uiso 1 1 calc R . . H51Z H 0.2099 0.4208 -0.0301 0.338 Uiso 1 1 calc R . . H511 H 0.1602 0.5083 -0.0200 0.338 Uiso 1 1 calc R . . C618 C 0.2203(9) 0.5190(8) 0.0577(5) 0.176(6) Uiso 1 1 d D . . H61Y H 0.1784 0.4929 0.0831 0.264 Uiso 1 1 calc R . . H61Z H 0.1927 0.5715 0.0405 0.264 Uiso 1 1 calc R . . H611 H 0.2644 0.5283 0.0735 0.264 Uiso 1 1 calc R . . N1A N 0.8039(7) 0.3024(7) 0.1356(4) 0.126(3) Uiso 1 1 d . . . C1A C 0.8165(8) 0.2535(7) 0.1829(5) 0.122(4) Uiso 1 1 d . . . H1A1 H 0.7984 0.2876 0.2081 0.183 Uiso 1 1 calc R . . H1A2 H 0.8765 0.2300 0.1821 0.183 Uiso 1 1 calc R . . H1A3 H 0.7833 0.2093 0.1911 0.183 Uiso 1 1 calc R . . O2A O 0.8113(8) 0.2706(8) 0.1001(5) 0.185(4) Uiso 1 1 d . . . O3A O 0.7796(8) 0.3726(9) 0.1294(5) 0.194(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0280(3) 0.0490(4) 0.0291(3) -0.0125(3) -0.0034(3) -0.0066(3) Mn2 0.0338(4) 0.0479(4) 0.0266(3) -0.0064(3) -0.0072(3) -0.0086(3) Mn3 0.0303(4) 0.0456(4) 0.0275(3) -0.0067(3) -0.0049(3) -0.0069(3) Mn4 0.0316(4) 0.0547(4) 0.0291(4) -0.0137(3) -0.0017(3) -0.0071(3) Mn5 0.0402(4) 0.0723(6) 0.0487(5) -0.0345(4) -0.0038(3) -0.0036(4) Mn6 0.0392(4) 0.0809(6) 0.0500(5) -0.0367(5) -0.0113(4) -0.0056(4) Mn7 0.0300(4) 0.0621(5) 0.0470(4) -0.0208(4) -0.0090(3) -0.0067(3) Mn8 0.0376(4) 0.0495(5) 0.0562(5) -0.0169(4) -0.0176(3) -0.0009(3) Mn9 0.0447(4) 0.0454(4) 0.0450(4) -0.0047(3) -0.0171(3) -0.0097(3) Mn10 0.0412(4) 0.0480(4) 0.0369(4) -0.0126(3) -0.0152(3) -0.0043(3) Mn11 0.0357(4) 0.0494(4) 0.0387(4) -0.0098(3) -0.0129(3) -0.0029(3) Mn12 0.0426(4) 0.0548(5) 0.0480(5) -0.0205(4) -0.0114(3) 0.0020(4) O6 0.082(3) 0.107(4) 0.052(3) -0.009(3) -0.009(2) 0.010(3) O10 0.073(3) 0.131(5) 0.043(2) -0.010(3) -0.005(2) 0.028(3) O120 0.055(3) 0.089(3) 0.069(3) -0.031(3) 0.002(2) -0.014(2) O121 0.105(4) 0.091(4) 0.065(3) -0.003(3) -0.020(3) -0.047(3) O107 0.0342(17) 0.062(2) 0.0388(18) -0.0224(16) -0.0079(14) -0.0062(15) O108 0.0281(16) 0.054(2) 0.0421(18) -0.0170(16) -0.0066(13) -0.0045(14) O123 0.0304(15) 0.0433(17) 0.0271(15) -0.0073(13) -0.0064(12) -0.0070(13) O124 0.0320(16) 0.0523(19) 0.0284(15) -0.0114(14) -0.0070(12) -0.0073(14) O134 0.0311(16) 0.0477(18) 0.0316(16) -0.0149(14) -0.0026(12) -0.0070(13) O208 0.0428(18) 0.0458(18) 0.0383(18) -0.0063(15) -0.0160(14) -0.0077(15) O209 0.0407(18) 0.0474(19) 0.0343(17) -0.0049(14) -0.0121(14) -0.0116(14) O234 0.0301(16) 0.0514(19) 0.0307(16) -0.0082(14) -0.0044(12) -0.0081(14) O310 0.0329(16) 0.0469(18) 0.0354(17) -0.0072(14) -0.0109(13) -0.0047(14) O311 0.0347(17) 0.0469(19) 0.0403(18) -0.0129(15) -0.0099(14) -0.0011(14) O405 0.0343(17) 0.062(2) 0.0398(18) -0.0217(16) -0.0038(14) -0.0025(15) O406 0.0385(18) 0.064(2) 0.0398(18) -0.0256(17) -0.0052(14) -0.0062(16) O13 0.067(3) 0.059(3) 0.131(5) -0.028(3) -0.049(3) 0.006(2) O23 0.062(3) 0.051(2) 0.083(3) -0.001(2) -0.032(2) -0.0071(19) O14 0.057(3) 0.090(3) 0.071(3) -0.036(3) 0.005(2) -0.019(2) O24 0.052(2) 0.066(2) 0.051(2) -0.0183(19) -0.0103(18) -0.0087(19) O15 0.039(2) 0.088(3) 0.084(3) -0.039(3) -0.015(2) -0.002(2) O25 0.051(3) 0.084(3) 0.159(6) -0.068(4) -0.030(3) 0.010(2) O16 0.065(3) 0.074(3) 0.049(2) -0.012(2) -0.0200(19) -0.010(2) O26 0.089(3) 0.071(3) 0.070(3) -0.002(2) -0.039(3) -0.021(3) O17 0.0378(18) 0.058(2) 0.0358(17) -0.0106(15) -0.0017(14) -0.0114(15) O27 0.0393(19) 0.077(3) 0.047(2) -0.0167(19) 0.0025(16) -0.0181(18) O18 0.042(2) 0.157(5) 0.115(4) -0.094(4) -0.019(3) -0.004(3) O28 0.037(2) 0.107(4) 0.082(3) -0.054(3) -0.010(2) -0.014(2) O19 0.058(3) 0.073(3) 0.072(3) -0.027(2) 0.001(2) -0.014(2) O29 0.055(3) 0.079(3) 0.108(4) -0.032(3) -0.002(3) -0.019(2) O110 0.062(3) 0.113(4) 0.077(3) -0.066(3) -0.020(2) 0.006(3) O210 0.064(3) 0.121(4) 0.081(3) -0.065(3) -0.029(2) 0.014(3) O111 0.084(3) 0.076(3) 0.082(3) -0.045(3) -0.033(3) 0.014(3) O211 0.052(2) 0.095(3) 0.081(3) -0.059(3) -0.012(2) 0.009(2) O112 0.053(2) 0.078(3) 0.0332(19) -0.0136(18) 0.0067(16) -0.012(2) O212 0.070(3) 0.110(4) 0.037(2) -0.028(2) 0.016(2) -0.009(3) O113 0.072(3) 0.061(3) 0.070(3) -0.022(2) -0.032(2) 0.009(2) O213 0.046(2) 0.059(2) 0.069(3) -0.016(2) -0.0219(19) 0.0024(18) O114 0.057(2) 0.051(2) 0.072(3) -0.0086(19) -0.028(2) -0.0157(18) O214 0.074(3) 0.061(3) 0.084(3) -0.026(2) -0.043(2) -0.005(2) O115 0.047(2) 0.069(2) 0.0333(18) -0.0054(17) -0.0058(15) -0.0151(18) O215 0.065(3) 0.060(2) 0.049(2) 0.0091(19) -0.0138(19) -0.024(2) O116 0.057(2) 0.062(3) 0.071(3) -0.017(2) 0.011(2) -0.019(2) O216 0.041(2) 0.062(2) 0.050(2) -0.0079(18) -0.0019(16) -0.0065(17) O117 0.064(3) 0.067(3) 0.053(2) -0.024(2) -0.030(2) 0.003(2) O217 0.049(2) 0.063(2) 0.053(2) -0.0136(18) -0.0250(18) -0.0017(18) O118 0.0431(19) 0.059(2) 0.0355(18) 0.0004(16) -0.0026(15) -0.0115(16) O218 0.063(3) 0.072(3) 0.039(2) 0.0014(18) -0.0136(18) -0.010(2) _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 O108 1.853(3) . ? Mn1 O107 1.885(3) . ? Mn1 O17 1.897(3) . ? Mn1 O124 1.924(3) . ? Mn1 O134 1.926(3) . ? Mn1 O123 1.928(3) . ? Mn1 Mn7 2.7771(11) . ? Mn1 Mn4 2.8376(11) . ? Mn1 Mn2 2.8412(11) . ? Mn1 Mn3 2.9417(11) . ? Mn2 O208 1.851(4) . ? Mn2 O209 1.869(3) . ? Mn2 O115 1.903(3) . ? Mn2 O124 1.920(3) . ? Mn2 O123 1.922(3) . ? Mn2 O234 1.933(3) . ? Mn2 Mn9 2.7626(12) . ? Mn2 Mn3 2.8304(11) . ? Mn2 Mn4 2.9367(12) . ? Mn3 O310 1.868(3) . ? Mn3 O311 1.870(3) . ? Mn3 O234 1.887(3) . ? Mn3 O123 1.903(3) . ? Mn3 O134 1.911(3) . ? Mn3 O118 1.924(3) . ? Mn3 Mn11 2.7911(11) . ? Mn3 Mn4 2.8094(11) . ? Mn4 O406 1.852(3) . ? Mn4 O405 1.889(4) . ? Mn4 O134 1.892(3) . ? Mn4 O234 1.905(3) . ? Mn4 O124 1.917(3) . ? Mn4 O112 1.919(4) . ? Mn4 Mn5 2.7950(13) . ? Mn5 O406 1.876(4) . ? Mn5 O405 1.910(4) . ? Mn5 O211 1.937(4) . ? Mn5 O110 1.948(4) . ? Mn5 O19 2.181(5) . ? Mn5 O212 2.226(4) . ? Mn6 O406 1.878(4) . ? Mn6 O107 1.890(3) . ? Mn6 O18 1.936(4) . ? Mn6 O210 1.968(4) . ? Mn6 O29 2.087(5) . ? Mn6 O6 2.268(6) . ? Mn7 O108 1.878(3) . ? Mn7 O107 1.913(3) . ? Mn7 O15 1.932(4) . ? Mn7 O28 1.941(4) . ? Mn7 O16 2.200(4) . ? Mn7 O27 2.202(4) . ? Mn8 O108 1.930(4) . ? Mn8 O208 1.964(4) . ? Mn8 O13 2.002(4) . ? Mn8 O26 2.010(4) . ? Mn8 O14 2.012(4) . ? Mn8 O25 2.025(5) . ? Mn9 O208 1.876(3) . ? Mn9 O209 1.898(4) . ? Mn9 O23 1.940(4) . ? Mn9 O114 1.944(4) . ? Mn9 O24 2.195(4) . ? Mn9 O215 2.216(4) . ? Mn10 O310 1.883(4) . ? Mn10 O209 1.889(3) . ? Mn10 O214 1.936(4) . ? Mn10 O117 1.963(4) . ? Mn10 O116 2.106(4) . ? Mn10 O10 2.263(5) . ? Mn11 O311 1.890(3) . ? Mn11 O310 1.895(3) . ? Mn11 O217 1.940(4) . ? Mn11 O213 1.944(4) . ? Mn11 O216 2.178(4) . ? Mn11 O218 2.205(4) . ? Mn12 O311 1.862(3) . ? Mn12 O405 1.888(4) . ? Mn12 O111 1.948(4) . ? Mn12 O113 1.959(4) . ? Mn12 O121 2.227(5) . ? Mn12 O120 2.248(5) . ? O13 C13 1.251(5) . ? O23 C13 1.241(5) . ? C13 C23 1.516(6) . ? C23 C33 1.514(7) . ? C33 C43 1.519(7) . ? C33 C63 1.522(7) . ? C33 C53 1.524(7) . ? O14 C14 1.256(5) . ? O24 C14 1.255(5) . ? C14 C24 1.508(6) . ? C24 C34 1.512(6) . ? C34 C44 1.519(6) . ? C34 C64 1.521(6) . ? C34 C54 1.530(6) . ? O15 C15 1.256(5) . ? O25 C15 1.251(6) . ? C15 C25' 1.524(7) . ? C15 C25 1.527(7) . ? C25 C35 1.499(7) . ? C35 C45 1.515(7) . ? C35 C65 1.517(7) . ? C35 C55 1.519(7) . ? C25' C35' 1.514(7) . ? C35' C65' 1.513(7) . ? C35' C55' 1.516(7) . ? C35' C45' 1.520(7) . ? O16 C16 1.260(5) . ? O26 C16 1.252(5) . ? C16 C26 1.511(6) . ? C26 C36 1.516(6) . ? C36 C56 1.511(6) . ? C36 C46 1.517(6) . ? C36 C66 1.529(6) . ? O17 C17 1.271(5) . ? O27 C17 1.245(5) . ? C17 C27 1.512(5) . ? C27 C37 1.527(6) . ? C37 C47 1.516(6) . ? C37 C67 1.517(6) . ? C37 C57 1.518(6) . ? O18 C18 1.268(6) . ? O28 C18 1.244(6) . ? C18 C28 1.531(7) . ? C18 C28' 1.537(7) . ? C28 C38 1.500(7) . ? C38 C58 1.515(7) . ? C38 C68 1.522(7) . ? C38 C48 1.531(7) . ? C28' C38' 1.511(7) . ? C38' C48' 1.513(7) . ? C38' C58' 1.516(7) . ? C38' C68' 1.526(7) . ? O19 C19 1.272(6) . ? O29 C19 1.236(6) . ? C19 C29 1.516(6) . ? C29 C39 1.514(6) . ? C39 C59 1.505(6) . ? C39 C49 1.513(6) . ? C39 C69 1.532(6) . ? O110 C110 1.260(6) . ? O210 C110 1.258(6) . ? C110 C210 1.519(6) . ? C210 C310 1.515(7) . ? C310 C410 1.510(7) . ? C310 C510 1.514(7) . ? C310 C610 1.518(7) . ? O111 C111 1.253(5) . ? O211 C111 1.244(5) . ? C111 C211 1.519(6) . ? C211 C311 1.524(6) . ? C311 C511 1.514(6) . ? C311 C611 1.516(6) . ? C311 C411 1.530(6) . ? O112 C112 1.263(5) . ? O212 C112 1.245(6) . ? C112 C212 1.513(6) . ? C212 C312 1.502(6) . ? C312 C612 1.510(6) . ? C312 C412 1.517(7) . ? C312 C512 1.521(7) . ? O113 C113 1.267(5) . ? O213 C113 1.249(5) . ? C113 C213 1.517(6) . ? C213 C313 1.521(6) . ? C313 C513 1.516(6) . ? C313 C413 1.520(6) . ? C313 C613 1.521(6) . ? O114 C114 1.256(5) . ? O214 C114 1.246(5) . ? C114 C214 1.507(5) . ? C214 C314 1.510(6) . ? C314 C614 1.511(6) . ? C314 C414 1.521(6) . ? C314 C514 1.528(6) . ? O115 C115 1.275(5) . ? O215 C115 1.237(5) . ? C115 C215 1.515(6) . ? C215 C315 1.519(6) . ? C315 C415 1.511(6) . ? C315 C615 1.519(6) . ? C315 C515 1.525(6) . ? O116 C116 1.263(5) . ? O216 C116 1.246(5) . ? C116 C216 1.529(6) . ? C216 C316 1.520(6) . ? C316 C416 1.512(6) . ? C316 C616 1.519(6) . ? C316 C516 1.522(6) . ? O117 C117 1.258(5) . ? O217 C117 1.253(5) . ? C117 C217 1.504(6) . ? C217 C327 1.511(7) . ? C217 C317 1.521(7) . ? C317 C617 1.516(7) . ? C317 C517 1.517(7) . ? C317 C417 1.518(7) . ? C327 C627 1.518(7) . ? C327 C427 1.519(7) . ? C327 C527 1.520(7) . ? O118 C118 1.278(5) . ? O218 C118 1.248(5) . ? C118 C218 1.510(6) . ? C218 C318 1.508(6) . ? C318 C618 1.513(7) . ? C318 C418 1.519(6) . ? C318 C518 1.526(7) . ? N1A O3A 1.139(14) . ? N1A O2A 1.192(14) . ? N1A C1A 1.400(14) . ? 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 O108 Mn1 O107 84.31(15) . . ? O108 Mn1 O17 92.63(15) . . ? O107 Mn1 O17 94.44(15) . . ? O108 Mn1 O124 94.29(15) . . ? O107 Mn1 O124 89.64(14) . . ? O17 Mn1 O124 172.28(14) . . ? O108 Mn1 O134 174.87(14) . . ? O107 Mn1 O134 99.96(14) . . ? O17 Mn1 O134 89.89(14) . . ? O124 Mn1 O134 82.95(14) . . ? O108 Mn1 O123 96.18(14) . . ? O107 Mn1 O123 173.27(14) . . ? O17 Mn1 O123 92.24(14) . . ? O124 Mn1 O123 83.63(13) . . ? O134 Mn1 O123 79.24(13) . . ? O108 Mn1 Mn7 42.23(10) . . ? O107 Mn1 Mn7 43.42(11) . . ? O17 Mn1 Mn7 86.42(10) . . ? O124 Mn1 Mn7 101.02(10) . . ? O134 Mn1 Mn7 142.53(10) . . ? O123 Mn1 Mn7 138.12(10) . . ? O108 Mn1 Mn4 136.31(11) . . ? O107 Mn1 Mn4 89.94(10) . . ? O17 Mn1 Mn4 131.03(11) . . ? O124 Mn1 Mn4 42.27(10) . . ? O134 Mn1 Mn4 41.52(10) . . ? O123 Mn1 Mn4 85.07(9) . . ? Mn7 Mn1 Mn4 125.95(3) . . ? O108 Mn1 Mn2 89.80(11) . . ? O107 Mn1 Mn2 131.03(11) . . ? O17 Mn1 Mn2 134.45(11) . . ? O124 Mn1 Mn2 42.29(9) . . ? O134 Mn1 Mn2 85.25(10) . . ? O123 Mn1 Mn2 42.35(9) . . ? Mn7 Mn1 Mn2 122.65(4) . . ? Mn4 Mn1 Mn2 62.28(3) . . ? O108 Mn1 Mn3 135.70(11) . . ? O107 Mn1 Mn3 139.48(11) . . ? O17 Mn1 Mn3 90.28(10) . . ? O124 Mn1 Mn3 82.38(10) . . ? O134 Mn1 Mn3 39.74(9) . . ? O123 Mn1 Mn3 39.52(9) . . ? Mn7 Mn1 Mn3 175.90(3) . . ? Mn4 Mn1 Mn3 58.14(3) . . ? Mn2 Mn1 Mn3 58.58(3) . . ? O208 Mn2 O209 84.54(15) . . ? O208 Mn2 O115 92.97(16) . . ? O209 Mn2 O115 94.12(15) . . ? O208 Mn2 O124 97.19(14) . . ? O209 Mn2 O124 173.99(14) . . ? O115 Mn2 O124 91.54(15) . . ? O208 Mn2 O123 93.67(14) . . ? O209 Mn2 O123 90.27(14) . . ? O115 Mn2 O123 172.36(15) . . ? O124 Mn2 O123 83.89(13) . . ? O208 Mn2 O234 175.47(15) . . ? O209 Mn2 O234 98.19(15) . . ? O115 Mn2 O234 90.43(15) . . ? O124 Mn2 O234 79.73(14) . . ? O123 Mn2 O234 82.74(13) . . ? O208 Mn2 Mn9 42.50(10) . . ? O209 Mn2 Mn9 43.25(11) . . ? O115 Mn2 Mn9 86.83(12) . . ? O124 Mn2 Mn9 139.36(10) . . ? O123 Mn2 Mn9 100.63(10) . . ? O234 Mn2 Mn9 140.84(10) . . ? O208 Mn2 Mn3 135.28(11) . . ? O209 Mn2 Mn3 89.18(11) . . ? O115 Mn2 Mn3 131.68(12) . . ? O124 Mn2 Mn3 85.54(10) . . ? O123 Mn2 Mn3 42.01(9) . . ? O234 Mn2 Mn3 41.57(9) . . ? Mn9 Mn2 Mn3 124.49(4) . . ? O208 Mn2 Mn1 90.04(11) . . ? O209 Mn2 Mn1 132.09(11) . . ? O115 Mn2 Mn1 133.75(11) . . ? O124 Mn2 Mn1 42.39(10) . . ? O123 Mn2 Mn1 42.53(9) . . ? O234 Mn2 Mn1 85.45(10) . . ? Mn9 Mn2 Mn1 123.24(3) . . ? Mn3 Mn2 Mn1 62.49(3) . . ? O208 Mn2 Mn4 137.18(11) . . ? O209 Mn2 Mn4 137.81(11) . . ? O115 Mn2 Mn4 90.13(12) . . ? O124 Mn2 Mn4 40.02(10) . . ? O123 Mn2 Mn4 82.43(10) . . ? O234 Mn2 Mn4 39.74(10) . . ? Mn9 Mn2 Mn4 176.89(3) . . ? Mn3 Mn2 Mn4 58.27(3) . . ? Mn1 Mn2 Mn4 58.80(3) . . ? O310 Mn3 O311 84.39(15) . . ? O310 Mn3 O234 90.74(14) . . ? O311 Mn3 O234 88.17(15) . . ? O310 Mn3 O123 97.15(14) . . ? O311 Mn3 O123 172.51(14) . . ? O234 Mn3 O123 84.48(14) . . ? O310 Mn3 O134 174.06(14) . . ? O311 Mn3 O134 97.50(14) . . ? O234 Mn3 O134 83.71(14) . . ? O123 Mn3 O134 80.25(14) . . ? O310 Mn3 O118 92.56(15) . . ? O311 Mn3 O118 90.47(16) . . ? O234 Mn3 O118 176.29(16) . . ? O123 Mn3 O118 96.77(14) . . ? O134 Mn3 O118 93.05(15) . . ? O310 Mn3 Mn11 42.49(10) . . ? O311 Mn3 Mn11 42.35(10) . . ? O234 Mn3 Mn11 94.11(10) . . ? O123 Mn3 Mn11 139.64(10) . . ? O134 Mn3 Mn11 139.83(10) . . ? O118 Mn3 Mn11 87.20(11) . . ? O310 Mn3 Mn4 132.72(11) . . ? O311 Mn3 Mn4 87.25(10) . . ? O234 Mn3 Mn4 42.45(10) . . ? O123 Mn3 Mn4 86.33(9) . . ? O134 Mn3 Mn4 42.10(10) . . ? O118 Mn3 Mn4 134.03(12) . . ? Mn11 Mn3 Mn4 118.99(3) . . ? O310 Mn3 Mn2 88.66(10) . . ? O311 Mn3 Mn2 130.44(11) . . ? O234 Mn3 Mn2 42.82(10) . . ? O123 Mn3 Mn2 42.52(9) . . ? O134 Mn3 Mn2 85.83(10) . . ? O118 Mn3 Mn2 138.93(12) . . ? Mn11 Mn3 Mn2 119.01(3) . . ? Mn4 Mn3 Mn2 62.76(3) . . ? O310 Mn3 Mn1 137.19(11) . . ? O311 Mn3 Mn1 137.38(11) . . ? O234 Mn3 Mn1 83.39(10) . . ? O123 Mn3 Mn1 40.15(9) . . ? O134 Mn3 Mn1 40.13(10) . . ? O118 Mn3 Mn1 95.30(11) . . ? Mn11 Mn3 Mn1 177.50(3) . . ? Mn4 Mn3 Mn1 59.08(2) . . ? Mn2 Mn3 Mn1 58.94(2) . . ? O406 Mn4 O405 84.13(16) . . ? O406 Mn4 O134 92.20(15) . . ? O405 Mn4 O134 88.32(15) . . ? O406 Mn4 O234 173.58(14) . . ? O405 Mn4 O234 100.65(15) . . ? O134 Mn4 O234 83.72(14) . . ? O406 Mn4 O124 94.18(15) . . ? O405 Mn4 O124 172.12(15) . . ? O134 Mn4 O124 84.04(14) . . ? O234 Mn4 O124 80.51(14) . . ? O406 Mn4 O112 91.22(17) . . ? O405 Mn4 O112 92.81(17) . . ? O134 Mn4 O112 176.49(16) . . ? O234 Mn4 O112 92.81(16) . . ? O124 Mn4 O112 94.92(16) . . ? O406 Mn4 Mn5 41.75(11) . . ? O405 Mn4 Mn5 42.92(11) . . ? O134 Mn4 Mn5 95.65(10) . . ? O234 Mn4 Mn5 143.45(11) . . ? O124 Mn4 Mn5 135.92(10) . . ? O112 Mn4 Mn5 87.43(13) . . ? O406 Mn4 Mn3 134.62(12) . . ? O405 Mn4 Mn3 89.52(11) . . ? O134 Mn4 Mn3 42.62(10) . . ? O234 Mn4 Mn3 41.95(10) . . ? O124 Mn4 Mn3 86.20(9) . . ? O112 Mn4 Mn3 134.03(13) . . ? Mn5 Mn4 Mn3 122.41(4) . . ? O406 Mn4 Mn1 87.60(11) . . ? O405 Mn4 Mn1 129.68(11) . . ? O134 Mn4 Mn1 42.45(10) . . ? O234 Mn4 Mn1 86.05(10) . . ? O124 Mn4 Mn1 42.46(10) . . ? O112 Mn4 Mn1 137.00(13) . . ? Mn5 Mn4 Mn1 117.71(3) . . ? Mn3 Mn4 Mn1 62.79(3) . . ? O406 Mn4 Mn2 134.25(12) . . ? O405 Mn4 Mn2 140.75(11) . . ? O134 Mn4 Mn2 83.14(10) . . ? O234 Mn4 Mn2 40.44(10) . . ? O124 Mn4 Mn2 40.10(9) . . ? O112 Mn4 Mn2 93.90(13) . . ? Mn5 Mn4 Mn2 175.88(4) . . ? Mn3 Mn4 Mn2 58.97(2) . . ? Mn1 Mn4 Mn2 58.92(3) . . ? O406 Mn5 O405 82.93(15) . . ? O406 Mn5 O211 177.39(17) . . ? O405 Mn5 O211 94.56(16) . . ? O406 Mn5 O110 95.86(17) . . ? O405 Mn5 O110 173.3(2) . . ? O211 Mn5 O110 86.55(18) . . ? O406 Mn5 O19 91.99(17) . . ? O405 Mn5 O19 97.51(17) . . ? O211 Mn5 O19 89.0(2) . . ? O110 Mn5 O19 89.1(2) . . ? O406 Mn5 O212 84.78(17) . . ? O405 Mn5 O212 83.68(17) . . ? O211 Mn5 O212 94.3(2) . . ? O110 Mn5 O212 89.6(2) . . ? O19 Mn5 O212 176.40(18) . . ? O406 Mn5 Mn4 41.10(11) . . ? O405 Mn5 Mn4 42.35(11) . . ? O211 Mn5 Mn4 136.31(13) . . ? O110 Mn5 Mn4 135.23(15) . . ? O19 Mn5 Mn4 101.44(12) . . ? O212 Mn5 Mn4 77.13(12) . . ? O406 Mn6 O107 94.86(15) . . ? O406 Mn6 O18 171.8(2) . . ? O107 Mn6 O18 91.18(17) . . ? O406 Mn6 O210 90.88(17) . . ? O107 Mn6 O210 174.00(17) . . ? O18 Mn6 O210 82.94(19) . . ? O406 Mn6 O29 93.45(18) . . ? O107 Mn6 O29 94.87(19) . . ? O18 Mn6 O29 91.6(3) . . ? O210 Mn6 O29 86.5(2) . . ? O406 Mn6 O6 84.56(19) . . ? O107 Mn6 O6 93.09(18) . . ? O18 Mn6 O6 89.6(3) . . ? O210 Mn6 O6 85.7(2) . . ? O29 Mn6 O6 171.9(2) . . ? O108 Mn7 O107 82.87(14) . . ? O108 Mn7 O15 96.75(16) . . ? O107 Mn7 O15 173.8(2) . . ? O108 Mn7 O28 176.57(19) . . ? O107 Mn7 O28 94.12(17) . . ? O15 Mn7 O28 86.06(18) . . ? O108 Mn7 O16 91.82(15) . . ? O107 Mn7 O16 96.57(16) . . ? O15 Mn7 O16 89.6(2) . . ? O28 Mn7 O16 90.16(19) . . ? O108 Mn7 O27 86.87(15) . . ? O107 Mn7 O27 87.87(15) . . ? O15 Mn7 O27 85.93(19) . . ? O28 Mn7 O27 91.38(19) . . ? O16 Mn7 O27 175.19(16) . . ? O108 Mn7 Mn1 41.55(10) . . ? O107 Mn7 Mn1 42.62(10) . . ? O15 Mn7 Mn1 135.43(13) . . ? O28 Mn7 Mn1 135.15(14) . . ? O16 Mn7 Mn1 103.68(12) . . ? O27 Mn7 Mn1 78.35(9) . . ? O108 Mn8 O208 93.60(14) . . ? O108 Mn8 O13 174.94(17) . . ? O208 Mn8 O13 91.46(17) . . ? O108 Mn8 O26 95.79(17) . . ? O208 Mn8 O26 92.40(18) . . ? O13 Mn8 O26 84.2(2) . . ? O108 Mn8 O14 92.48(18) . . ? O208 Mn8 O14 95.54(16) . . ? O13 Mn8 O14 86.8(2) . . ? O26 Mn8 O14 168.1(2) . . ? O108 Mn8 O25 90.65(17) . . ? O208 Mn8 O25 175.73(17) . . ? O13 Mn8 O25 84.3(2) . . ? O26 Mn8 O25 87.6(2) . . ? O14 Mn8 O25 83.8(2) . . ? O208 Mn9 O209 83.08(15) . . ? O208 Mn9 O23 95.97(16) . . ? O209 Mn9 O23 174.82(19) . . ? O208 Mn9 O114 174.79(18) . . ? O209 Mn9 O114 93.63(15) . . ? O23 Mn9 O114 86.94(17) . . ? O208 Mn9 O24 92.99(15) . . ? O209 Mn9 O24 95.76(15) . . ? O23 Mn9 O24 89.37(19) . . ? O114 Mn9 O24 91.36(17) . . ? O208 Mn9 O215 86.43(15) . . ? O209 Mn9 O215 88.16(15) . . ? O23 Mn9 O215 86.69(19) . . ? O114 Mn9 O215 89.44(17) . . ? O24 Mn9 O215 175.94(16) . . ? O208 Mn9 Mn2 41.83(11) . . ? O209 Mn9 Mn2 42.43(10) . . ? O23 Mn9 Mn2 135.44(14) . . ? O114 Mn9 Mn2 134.05(12) . . ? O24 Mn9 Mn2 103.59(11) . . ? O215 Mn9 Mn2 78.62(11) . . ? O310 Mn10 O209 95.06(14) . . ? O310 Mn10 O214 174.32(16) . . ? O209 Mn10 O214 90.50(16) . . ? O310 Mn10 O117 90.95(16) . . ? O209 Mn10 O117 171.46(16) . . ? O214 Mn10 O117 83.40(17) . . ? O310 Mn10 O116 91.94(15) . . ? O209 Mn10 O116 94.54(18) . . ? O214 Mn10 O116 88.79(19) . . ? O117 Mn10 O116 91.32(19) . . ? O310 Mn10 O10 87.4(2) . . ? O209 Mn10 O10 91.25(17) . . ? O214 Mn10 O10 91.4(2) . . ? O117 Mn10 O10 82.95(18) . . ? O116 Mn10 O10 174.21(19) . . ? O311 Mn11 O310 83.12(14) . . ? O311 Mn11 O217 175.21(17) . . ? O310 Mn11 O217 95.66(15) . . ? O311 Mn11 O213 94.41(15) . . ? O310 Mn11 O213 175.84(16) . . ? O217 Mn11 O213 86.53(16) . . ? O311 Mn11 O216 91.52(15) . . ? O310 Mn11 O216 93.72(14) . . ? O217 Mn11 O216 93.19(17) . . ? O213 Mn11 O216 89.69(17) . . ? O311 Mn11 O218 84.22(15) . . ? O310 Mn11 O218 84.92(15) . . ? O217 Mn11 O218 91.06(17) . . ? O213 Mn11 O218 91.51(17) . . ? O216 Mn11 O218 175.65(15) . . ? O311 Mn11 Mn3 41.80(10) . . ? O310 Mn11 Mn3 41.76(10) . . ? O217 Mn11 Mn3 136.25(11) . . ? O213 Mn11 Mn3 135.30(12) . . ? O216 Mn11 Mn3 98.24(11) . . ? O218 Mn11 Mn3 77.99(10) . . ? O311 Mn12 O405 94.59(15) . . ? O311 Mn12 O111 173.42(17) . . ? O405 Mn12 O111 91.99(17) . . ? O311 Mn12 O113 90.19(16) . . ? O405 Mn12 O113 175.11(17) . . ? O111 Mn12 O113 83.22(18) . . ? O311 Mn12 O121 89.71(19) . . ? O405 Mn12 O121 91.57(18) . . ? O111 Mn12 O121 90.2(2) . . ? O113 Mn12 O121 89.4(2) . . ? O311 Mn12 O120 92.08(17) . . ? O405 Mn12 O120 88.45(17) . . ? O111 Mn12 O120 88.0(2) . . ? O113 Mn12 O120 90.4(2) . . ? O121 Mn12 O120 178.2(2) . . ? Mn1 O107 Mn6 131.17(18) . . ? Mn1 O107 Mn7 93.96(15) . . ? Mn6 O107 Mn7 128.16(18) . . ? Mn1 O108 Mn7 96.23(16) . . ? Mn1 O108 Mn8 133.55(18) . . ? Mn7 O108 Mn8 123.78(18) . . ? Mn3 O123 Mn2 95.47(14) . . ? Mn3 O123 Mn1 100.33(15) . . ? Mn2 O123 Mn1 95.12(13) . . ? Mn4 O124 Mn2 99.89(14) . . ? Mn4 O124 Mn1 95.28(15) . . ? Mn2 O124 Mn1 95.32(14) . . ? Mn4 O134 Mn3 95.28(14) . . ? Mn4 O134 Mn1 96.03(15) . . ? Mn3 O134 Mn1 100.13(15) . . ? Mn2 O208 Mn9 95.67(15) . . ? Mn2 O208 Mn8 132.62(19) . . ? Mn9 O208 Mn8 122.67(19) . . ? Mn2 O209 Mn10 132.01(19) . . ? Mn2 O209 Mn9 94.32(15) . . ? Mn10 O209 Mn9 130.75(19) . . ? Mn3 O234 Mn4 95.60(15) . . ? Mn3 O234 Mn2 95.61(14) . . ? Mn4 O234 Mn2 99.83(15) . . ? Mn3 O310 Mn10 133.14(18) . . ? Mn3 O310 Mn11 95.75(16) . . ? Mn10 O310 Mn11 123.28(17) . . ? Mn12 O311 Mn3 132.29(18) . . ? Mn12 O311 Mn11 130.49(18) . . ? Mn3 O311 Mn11 95.85(15) . . ? Mn12 O405 Mn4 130.79(19) . . ? Mn12 O405 Mn5 128.4(2) . . ? Mn4 O405 Mn5 94.73(16) . . ? Mn4 O406 Mn5 97.15(16) . . ? Mn4 O406 Mn6 133.96(19) . . ? Mn5 O406 Mn6 124.7(2) . . ? C13 O13 Mn8 135.9(4) . . ? C13 O23 Mn9 131.4(4) . . ? O23 C13 O13 126.1(5) . . ? O23 C13 C23 117.7(5) . . ? O13 C13 C23 116.1(5) . . ? C33 C23 C13 118.1(6) . . ? C23 C33 C43 109.8(7) . . ? C23 C33 C63 110.8(7) . . ? C43 C33 C63 108.5(7) . . ? C23 C33 C53 111.2(7) . . ? C43 C33 C53 109.1(8) . . ? C63 C33 C53 107.3(8) . . ? C14 O14 Mn8 133.9(4) . . ? C14 O24 Mn9 132.0(3) . . ? O24 C14 O14 124.8(5) . . ? O24 C14 C24 118.6(4) . . ? O14 C14 C24 116.5(4) . . ? C14 C24 C34 116.6(5) . . ? C24 C34 C44 111.1(6) . . ? C24 C34 C64 110.0(6) . . ? C44 C34 C64 109.2(6) . . ? C24 C34 C54 107.9(5) . . ? C44 C34 C54 110.2(6) . . ? C64 C34 C54 108.4(6) . . ? C15 O15 Mn7 131.9(4) . . ? C15 O25 Mn8 135.8(4) . . ? O25 C15 O15 124.8(5) . . ? O25 C15 C25' 111.8(6) . . ? O15 C15 C25' 118.5(6) . . ? O25 C15 C25 124.2(6) . . ? O15 C15 C25 108.3(6) . . ? C25' C15 C25 42.2(7) . . ? C35 C25 C15 118.9(7) . . ? C25 C35 C45 108.2(8) . . ? C25 C35 C65 108.9(9) . . ? C45 C35 C65 109.9(9) . . ? C25 C35 C55 111.0(8) . . ? C45 C35 C55 109.1(8) . . ? C65 C35 C55 109.8(9) . . ? C35' C25' C15 114.9(7) . . ? C65' C35' C25' 110.4(9) . . ? C65' C35' C55' 111.2(9) . . ? C25' C35' C55' 110.1(8) . . ? C65' C35' C45' 108.4(9) . . ? C25' C35' C45' 109.2(9) . . ? C55' C35' C45' 107.4(8) . . ? C16 O16 Mn7 130.9(3) . . ? C16 O26 Mn8 135.0(4) . . ? O26 C16 O16 124.8(5) . . ? O26 C16 C26 117.1(5) . . ? O16 C16 C26 118.1(5) . . ? C16 C26 C36 117.6(5) . . ? C56 C36 C26 110.6(6) . . ? C56 C36 C46 110.9(6) . . ? C26 C36 C46 107.9(5) . . ? C56 C36 C66 109.3(6) . . ? C26 C36 C66 110.0(6) . . ? C46 C36 C66 108.0(6) . . ? C17 O17 Mn1 127.4(3) . . ? C17 O27 Mn7 122.5(3) . . ? O27 C17 O17 124.8(4) . . ? O27 C17 C27 120.0(4) . . ? O17 C17 C27 115.3(4) . . ? C17 C27 C37 114.4(4) . . ? C47 C37 C67 111.3(6) . . ? C47 C37 C57 109.4(6) . . ? C67 C37 C57 108.5(5) . . ? C47 C37 C27 107.4(5) . . ? C67 C37 C27 109.6(5) . . ? C57 C37 C27 110.6(5) . . ? C18 O18 Mn6 137.4(4) . . ? C18 O28 Mn7 130.0(4) . . ? O28 C18 O18 124.4(5) . . ? O28 C18 C28 118.1(6) . . ? O18 C18 C28 115.7(6) . . ? O28 C18 C28' 110.2(6) . . ? O18 C18 C28' 113.8(7) . . ? C28 C18 C28' 50.6(8) . . ? C38 C28 C18 115.1(7) . . ? C28 C38 C58 112.8(8) . . ? C28 C38 C68 109.1(9) . . ? C58 C38 C68 110.2(9) . . ? C28 C38 C48 109.7(7) . . ? C58 C38 C48 108.0(7) . . ? C68 C38 C48 106.8(9) . . ? C38' C28' C18 116.8(8) . . ? C28' C38' C48' 108.7(9) . . ? C28' C38' C58' 110.4(9) . . ? C48' C38' C58' 109.8(9) . . ? C28' C38' C68' 108.3(8) . . ? C48' C38' C68' 110.1(9) . . ? C58' C38' C68' 109.5(9) . . ? C19 O19 Mn5 123.4(4) . . ? C19 O29 Mn6 135.3(4) . . ? O29 C19 O19 126.4(6) . . ? O29 C19 C29 114.8(6) . . ? O19 C19 C29 118.6(6) . . ? C39 C29 C19 115.9(6) . . ? C59 C39 C49 110.5(7) . . ? C59 C39 C29 114.1(6) . . ? C49 C39 C29 110.1(6) . . ? C59 C39 C69 108.7(7) . . ? C49 C39 C69 108.2(7) . . ? C29 C39 C69 104.9(6) . . ? C110 O110 Mn5 132.5(4) . . ? C110 O210 Mn6 129.6(4) . . ? O210 C110 O110 125.3(5) . . ? O210 C110 C210 117.9(5) . . ? O110 C110 C210 116.5(5) . . ? C310 C210 C110 114.6(6) . . ? C410 C310 C510 107.8(8) . . ? C410 C310 C210 110.6(7) . . ? C510 C310 C210 111.5(8) . . ? C410 C310 C610 109.7(7) . . ? C510 C310 C610 108.7(8) . . ? C210 C310 C610 108.6(7) . . ? C111 O111 Mn12 136.6(4) . . ? C111 O211 Mn5 133.4(4) . . ? O211 C111 O111 125.8(5) . . ? O211 C111 C211 118.1(5) . . ? O111 C111 C211 116.1(5) . . ? C111 C211 C311 114.6(5) . . ? C511 C311 C611 109.1(7) . . ? C511 C311 C211 110.9(6) . . ? C611 C311 C211 110.4(6) . . ? C511 C311 C411 109.2(7) . . ? C611 C311 C411 109.5(7) . . ? C211 C311 C411 107.7(6) . . ? C112 O112 Mn4 126.1(4) . . ? C112 O212 Mn5 123.6(3) . . ? O212 C112 O112 125.4(5) . . ? O212 C112 C212 120.0(5) . . ? O112 C112 C212 114.4(5) . . ? C312 C212 C112 119.5(6) . . ? C212 C312 C612 109.8(6) . . ? C212 C312 C412 109.9(7) . . ? C612 C312 C412 108.7(7) . . ? C212 C312 C512 111.1(7) . . ? C612 C312 C512 110.5(7) . . ? C412 C312 C512 106.7(7) . . ? C113 O113 Mn12 132.4(4) . . ? C113 O213 Mn11 131.9(3) . . ? O213 C113 O113 125.5(5) . . ? O213 C113 C213 117.8(5) . . ? O113 C113 C213 116.7(5) . . ? C113 C213 C313 116.4(5) . . ? C513 C313 C413 109.5(6) . . ? C513 C313 C213 111.3(6) . . ? C413 C313 C213 108.8(6) . . ? C513 C313 C613 108.7(6) . . ? C413 C313 C613 110.4(6) . . ? C213 C313 C613 108.1(5) . . ? C114 O114 Mn9 132.3(3) . . ? C114 O214 Mn10 137.8(3) . . ? O214 C114 O114 125.9(4) . . ? O214 C114 C214 116.6(4) . . ? O114 C114 C214 117.5(4) . . ? C114 C214 C314 117.2(5) . . ? C214 C314 C614 110.6(6) . . ? C214 C314 C414 110.5(6) . . ? C614 C314 C414 108.5(6) . . ? C214 C314 C514 107.9(6) . . ? C614 C314 C514 110.2(6) . . ? C414 C314 C514 109.1(6) . . ? C115 O115 Mn2 126.6(3) . . ? C115 O215 Mn9 121.7(3) . . ? O215 C115 O115 125.9(4) . . ? O215 C115 C215 119.6(4) . . ? O115 C115 C215 114.6(4) . . ? C115 C215 C315 115.1(5) . . ? C415 C315 C615 109.5(6) . . ? C415 C315 C215 109.6(6) . . ? C615 C315 C215 110.5(5) . . ? C415 C315 C515 111.9(6) . . ? C615 C315 C515 108.3(6) . . ? C215 C315 C515 107.1(5) . . ? C116 O116 Mn10 131.5(4) . . ? C116 O216 Mn11 124.2(4) . . ? O216 C116 O116 123.5(5) . . ? O216 C116 C216 118.8(5) . . ? O116 C116 C216 117.5(5) . . ? C316 C216 C116 115.2(5) . . ? C416 C316 C616 108.8(6) . . ? C416 C316 C216 110.6(6) . . ? C616 C316 C216 109.3(6) . . ? C416 C316 C516 110.7(6) . . ? C616 C316 C516 108.9(6) . . ? C216 C316 C516 108.5(6) . . ? C117 O117 Mn10 132.6(3) . . ? C117 O217 Mn11 131.8(3) . . ? O217 C117 O117 125.7(4) . . ? O217 C117 C217 117.6(4) . . ? O117 C117 C217 116.6(4) . . ? C117 C217 C327 118.1(7) . . ? C117 C217 C317 114.9(5) . . ? C327 C217 C317 32.4(8) . . ? C617 C317 C517 110.0(8) . . ? C617 C317 C417 107.8(8) . . ? C517 C317 C417 110.2(8) . . ? C617 C317 C217 109.6(7) . . ? C517 C317 C217 110.5(8) . . ? C417 C317 C217 108.6(8) . . ? C217 C327 C627 110.4(9) . . ? C217 C327 C427 108.1(9) . . ? C627 C327 C427 108.8(9) . . ? C217 C327 C527 110.3(9) . . ? C627 C327 C527 109.3(9) . . ? C427 C327 C527 110.0(9) . . ? C118 O118 Mn3 125.3(3) . . ? C118 O218 Mn11 123.1(3) . . ? O218 C118 O118 126.0(5) . . ? O218 C118 C218 118.6(5) . . ? O118 C118 C218 115.3(5) . . ? C318 C218 C118 119.2(5) . . ? C218 C318 C618 111.7(7) . . ? C218 C318 C418 109.2(6) . . ? C618 C318 C418 111.7(7) . . ? C218 C318 C518 110.1(7) . . ? C618 C318 C518 106.4(7) . . ? C418 C318 C518 107.6(7) . . ? O3A N1A O2A 116.2(14) . . ? O3A N1A C1A 123.0(14) . . ? O2A N1A C1A 120.5(13) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 17.33 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.985 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.128 data_mn0311 #TrackingRef 'all_revised.cif' _database_code_depnum_ccdc_archive 'CCDC 755027' #1.5 GPa structure #see refine special details for checkcif comments _audit_creation_method SHELXL-97 _chemical_compound_source 'Mark Murrie & Pascal Parois, Glasgow University' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn12O12(tBuCH2CO2)16(H2O)4].0.75MeNO2.0.5CH2Cl2' _chemical_formula_sum 'C97.25 H187.25 Cl Mn12 N0.75 O49.50' _chemical_formula_weight 2853.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0005 0.0007 '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 0.0015 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0034 0.0025 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.2230 0.3472 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.0750 0.0720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3530(11) _cell_length_b 15.5310(11) _cell_length_c 26.7020(12) _cell_angle_alpha 76.669(5) _cell_angle_beta 76.441(5) _cell_angle_gamma 78.069(5) _cell_volume 5943.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3394 _cell_measurement_theta_min 2 _cell_measurement_theta_max 13.5 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2978 _exptl_absorpt_coefficient_mu 0.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6493 _exptl_absorpt_correction_T_max 0.7437 _exptl_absorpt_process_details Sadabs _exptl_special_details ; Station 9.8 at Daresbury SRS ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.47800 _diffrn_radiation_type Xray _diffrn_radiation_source synchtrotron _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'Bruker Apex-II' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32067 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.1038 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 15.46 _reflns_number_total 4879 _reflns_number_gt 3177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex' _computing_cell_refinement 'Bruker Saint' _computing_data_reduction 'Bruker Saint' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Data were collected on Station 9.8 at the Daresbury SRS. The crystal was held in a Merrill-Bassett diamond anvil cell constructed using conically-ground WC backing disks and Boehler-Almax culet-cut diamonds. The body of the pressure cell restricts the volume of reciprocal space which can be sampled during data collection and, taken with the low crystal symmetry (triclinic) the completeness is low. Coverage statistics are: #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 13.83 0.500 0.280 12451 3490 8961 15.24 0.550 0.287 16219 4647 11572 15.46 0.558 0.288 16799 4842 11957 #----------------------------------------------------------- ACTA Min. Res. --- Data were integrated to 0.9 Ang resolution - beyond this the data became very weak and indistinguishable from noise. The structure was solved by direct methods (SIR92) for the Mn atoms. A starting model was generated from the ambient pressure structure by fitting of the Mn positions. Four possible orientations are possible. The one giving the losest R-factor was selected. In view of the low completeness only the Mn atoms were modelled with anisotropic displacement patameters. All other atoms were modelled isotropically. The MeNO2 and CH2Cl2, which is full occupancy at ambient pressure is modelled here with occupancies of 0.75 and 0.5 respectively in order to retain reasonable values of the displacement parameters. tBuCH2COO- ligands carrying the labels 3,5,6,10,12 and 18 are disordered with the tBu groups distributed over two positions. The C-C distances and C-C-C angles involving part-weight atoms were restrained to 1.50(1) Ang and 109.5 deg, respectively. Fully occupied ligands were restrained to be geometrically similar. Within disordered ligands isotropic displacement parameters for chemically equivalent carbon atoms were constrined to be equal. H-atoms were placed in calculated positions; in some cases methyl groups were modelled as being rotationally disordered in order to avoid close contacts with other part-weight H-atoms. H-atoms were not placed on the ligand water molecules (atoms O6, O10, O120 and O121). In the final cycles of refinement robust-resistant weighting scheme was used as described by Prince (Acta A39, 407-410, 1983). This is amongst the largest structures to have been investigated using high-pressure methods at atomic resolution. The low completeness, weak diffraction and disorder made modelling the diffraction data challenging, and there are numerous checkcif alerts: 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.28 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.28 201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 133 023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6].. 15.46 Deg. 088_ALERT_3_B Poor Data / Parameter Ratio .................... 6.30 341_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 30 910_ALERT_3_B Missing # of FCF Reflections Below Th(Min) ..... 15 911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.558 11905 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 30 082_ALERT_2_C High R1 Value .................................. 0.11 084_ALERT_2_C High R2 Value .................................. 0.26 950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 2 951_ALERT_1_C Reported and Calculated Kmax Values Differ by .. 2 See comments above about low completeness and resolution. The high R-value is to be expected for a structure suffering from high libration (particularly in the tBu groups), but for which only isotropic modelling of displacement is possible. 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.00 Ratio 220_ALERT_2_A Large Non-Solvent O Ueq(max)/Ueq(min) ... 5.81 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.29 Ratio +Numerous alerts of the type: 241_ALERT_2_A Check High Ueq as Compared to Neighbors for O13 241_ALERT_2_A Check High Ueq as Compared to Neighbors for C28 241_ALERT_2_A Check High Ueq as Compared to Neighbors for C46 241_ALERT_2_A Check High Ueq as Compared to Neighbors for C56 241_ALERT_2_A Check High Ueq as Compared to Neighbors for C212 241_ALERT_2_B Check High Ueq as Compared to Neighbors for O26 241_ALERT_2_C Check High Ueq as Compared to Neighbors for Mn7 241_ALERT_2_C Check High Ueq as Compared to Neighbors for Mn9 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O14 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O25 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C38 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C312 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for O108 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C36 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C39 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C310 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C316 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C320 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C361 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn8 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O23 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O28 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O107 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O124 ... Disorder modelling was carried out for ligands in which U[iso] for one or more atoms refined to values larger than ca 0.3 Ang**2. Thermal motion still appears to be high elsewhere in the structure, though this is not unexpected for tBuCH2COO- at room temperature. 411_ALERT_2_A Short Inter H...H Contact H1B2 .. H21M .. 1.65 Ang. 412_ALERT_2_A Short Intra XH3 .. XHn H48B .. H62B .. 1.47 Ang. 413_ALERT_2_A Short Inter XH3 .. XHn H51Z .. H414 .. 1.87 Ang. 413_ALERT_2_A Short Inter XH3 .. XHn H1A2 .. H27A .. 1.70 Ang. 411_ALERT_2_B Short Inter H...H Contact H23A .. H29A .. 1.88 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H41M .. H63E .. 1.94 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H48A .. H42A .. 1.95 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H48A .. H92A .. 1.93 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H51M .. H43D .. 2.06 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H51S .. H68A .. 1.90 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H51T .. H61L .. 1.91 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H51W .. H25B .. 1.93 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H61N .. H513 .. 1.94 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H61O .. H513 .. 2.08 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H1A1 .. H21Q .. 2.05 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H1A1 .. H67C .. 2.03 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H1A2 .. H67C .. 2.09 Ang. 431_ALERT_2_A Short Inter HL..A Contact Cl2B .. O23 .. 2.72 Ang. 432_ALERT_2_A Short Inter X...Y Contact Cl1B .. C211 .. 2.84 Ang. 432_ALERT_2_A Short Inter X...Y Contact O215 .. C1B .. 2.68 Ang. 432_ALERT_2_A Short Inter X...Y Contact C511 .. C610 .. 2.70 Ang. 431_ALERT_2_B Short Inter HL..A Contact Cl2B .. O215 .. 2.84 Ang. 432_ALERT_2_B Short Inter X...Y Contact Cl1B .. C511 .. 2.97 Ang. 432_ALERT_2_B Short Inter X...Y Contact C411 .. C510 .. 2.94 Ang. 411_ALERT_2_C Short Inter H...H Contact H29A .. H23C .. 2.03 Ang. 412_ALERT_2_C Short Intra XH3 .. XHn H48B .. H82B .. 1.88 Ang. 413_ALERT_2_C Short Inter XH3 .. XHn H21R .. H45F .. 2.13 Ang. 413_ALERT_2_C Short Inter XH3 .. XHn H42E .. H61V .. 2.12 Ang. 413_ALERT_2_C Short Inter XH3 .. XHn H59C .. H63F .. 2.10 Ang. 431_ALERT_2_C Short Inter HL..A Contact Cl2B .. O114 .. 2.98 Ang. 432_ALERT_2_C Short Inter X...Y Contact Cl1B .. C311 .. 3.18 Ang. 432_ALERT_2_C Short Inter X...Y Contact C518 .. C613 .. 3.13 Ang. Short H....H contacts are to be expected at high pressure. We have shown that 1.7 Ang is an approximate lower limit for H...H contacts at pressures up to 10 GPa. The shortest contacts in the table above all involve part-weight atoms. 245_ALERT_2_C U(iso) H22B Smaller than U(eq) C518 by ... 0.04 AngSq Don't understand this one. H22B is not connected to C518. 250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 3.23 All the Mn adps are oriented in the same direction. This is because the data set is truncated in one direction by the body of the pressure cell. 083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large. 128.07 Mostly likely due to the limitations of the model. 301_ALERT_3_G Note Main Residue Disorder .................... 13.00 Perc. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1849 See above. 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? No action Numerous alerts of the type: 731_ALERT_1_B Bond Calc 1.51(4), Rep 1.508(8) ...... 5.00 su-Ra C38 -C58 1.555 1.555 731_ALERT_1_B Bond Calc 1.51(5), Rep 1.510(8) ...... 6.25 su-Ra C38 -C48 1.555 1.555 731_ALERT_1_B Bond Calc 1.51(4), Rep 1.510(8) ...... 5.00 su-Ra C38 -C68 1.555 1.555 731_ALERT_1_B Bond Calc 1.51(4), Rep 1.510(8) ...... 5.00 su-Ra C39 -C59 1.555 1.555 731_ALERT_1_B Bond Calc 1.26(4), Rep 1.260(9) ...... 4.44 su-Ra O110 -C110 1.555 1.555 731_ALERT_1_B Bond Calc 1.25(4), Rep 1.259(9) ...... 4.44 su-Ra O210 -C110 1.555 1.555 731_ALERT_1_B Bond Calc 1.52(4), Rep 1.510(8) ...... 5.00 su-Ra C311 -C611 1.555 1.555 731_ALERT_1_B Bond Calc 1.51(4), Rep 1.511(8) ...... 5.00 su-Ra C311 -C411 1.555 1.555 731_ALERT_1_B Bond Calc 1.51(4), Rep 1.509(8) ...... 5.00 su-Ra C313 -C413 1.555 1.555 731_ALERT_1_B Bond Calc 1.51(4), Rep 1.510(8) ...... 5.00 su-Ra C313 -C513 1.555 1.555 ... The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif can be badly in error. 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 C H2 Cl2 No action taken. 926_ALERT_1_C Reported and Calculated R1 * 100.0 Differ by . -0.22 927_ALERT_1_C Reported and Calculated wR2 * 100.0 Differ by . -0.26 Rounding error? 092_ALERT_4_G Check: Wavelength given is not Cu,Mo or Ag Ka .. 0.48 Ang. Synchrotron data. 154_ALERT_1_G The su's on the Cell Angles are Equal (x 10000) 500 Deg. 180_ALERT_4_G Check Cell Rounding: # of Values Ending with 0 = 3 302_ALERT_4_G Note Anion/Solvent Disorder .................... 64.00 Perc. 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 5 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 25.00 Deg. C231 -C13 -C23 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 38.00 Deg. C361 -C26 -C36 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 38.00 Deg. C361 -C46 -C36 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 38.00 Deg. C36 -C56 -C361 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 20.00 Deg. C420 -C320 -C920 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 20.00 Deg. C720 -C320 -C520 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 20.00 Deg. C820 -C320 -C620 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 27.00 Deg. C422 -C312 -C612 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 27.00 Deg. C412 -C312 -C622 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 27.00 Deg. C522 -C312 -C512 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 19.00 Deg. C228 -C118 -C218 1.555 1.555 1.555 795_ALERT_4_G C-Atom in CIF Coordinate List out of Sequence .. C14 796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence .. O107 No action. 811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms .... ! The cell can be transformed to monoclinic C, but merging statistics clearly point to triclinic (-1) symmetry: Option A: FOM = 0.727 deg. MONOCLINIC C-lattice R(sym) = 0.596 [ 1654] Cell: 23.990 19.451 26.702 89.95 107.42 89.32 Volume: 11887.63 Matrix:-1.0000 -1.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ; _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^)+(0.0624P)^2^+128.0706P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4879 _refine_ls_number_parameters 775 _refine_ls_number_restraints 1849 _refine_ls_R_factor_all 0.1615 _refine_ls_R_factor_gt 0.1083 _refine_ls_wR_factor_ref 0.2563 _refine_ls_wR_factor_gt 0.2232 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 0.879 _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 0.4156(3) 0.6890(3) 0.73374(14) 0.044(4) Uani 1 1 d . . . Mn2 Mn 0.2912(3) 0.5654(3) 0.76154(15) 0.038(4) Uani 1 1 d . . . Mn3 Mn 0.2543(3) 0.7237(3) 0.68699(15) 0.042(4) Uani 1 1 d . . . Mn4 Mn 0.2405(3) 0.7411(3) 0.79104(15) 0.045(4) Uani 1 1 d . . . Mn5 Mn 0.2117(4) 0.9067(4) 0.82187(16) 0.059(5) Uani 1 1 d . . . Mn6 Mn 0.4156(3) 0.7942(4) 0.83371(16) 0.058(4) Uani 1 1 d . . . Mn7 Mn 0.5786(3) 0.6529(4) 0.76928(16) 0.064(4) Uani 1 1 d . . . Mn8 Mn 0.5137(4) 0.4672(4) 0.75654(18) 0.053(4) Uani 1 1 d . . . Mn9 Mn 0.3346(4) 0.3951(4) 0.73827(16) 0.061(4) Uani 1 1 d . . . Mn10 Mn 0.1752(3) 0.5378(3) 0.67376(14) 0.044(4) Uani 1 1 d . . . Mn11 Mn 0.0914(4) 0.7557(4) 0.65191(17) 0.051(4) Uani 1 1 d . . . Mn12 Mn 0.1077(4) 0.9079(4) 0.72240(18) 0.064(5) Uani 1 1 d . . . O6 O 0.3879(16) 0.6591(16) 0.8869(7) 0.050(4) Uiso 1 1 d . . . O10 O 0.2964(15) 0.5155(16) 0.6080(7) 0.050(4) Uiso 1 1 d . . . O120 O -0.016(2) 0.843(2) 0.7701(10) 0.081(6) Uiso 1 1 d . . . O121 O 0.2283(16) 0.9608(17) 0.6839(7) 0.048(4) Uiso 1 1 d . . . O107 O 0.4709(13) 0.7389(14) 0.7740(6) 0.033(3) Uiso 1 1 d . . . O108 O 0.5134(12) 0.5983(13) 0.7396(6) 0.021(3) Uiso 1 1 d . . . O123 O 0.3507(13) 0.6281(14) 0.6990(6) 0.028(3) Uiso 1 1 d . . . O124 O 0.3387(13) 0.6416(13) 0.7942(6) 0.024(3) Uiso 1 1 d . . . O134 O 0.3122(14) 0.7799(14) 0.7243(6) 0.034(3) Uiso 1 1 d . . . O208 O 0.3840(13) 0.4698(14) 0.7661(6) 0.031(3) Uiso 1 1 d . . . O209 O 0.2508(14) 0.5045(14) 0.7235(6) 0.034(3) Uiso 1 1 d . . . O234 O 0.2016(14) 0.6729(15) 0.7543(7) 0.037(3) Uiso 1 1 d . . . O310 O 0.1921(14) 0.6585(14) 0.6596(6) 0.031(3) Uiso 1 1 d . . . O311 O 0.1488(13) 0.8095(14) 0.6889(6) 0.032(3) Uiso 1 1 d . . . O405 O 0.1604(14) 0.8476(15) 0.7806(7) 0.040(3) Uiso 1 1 d . . . O406 O 0.2956(13) 0.8049(13) 0.8236(6) 0.029(3) Uiso 1 1 d . . . O13 O 0.5233(16) 0.3326(18) 0.7758(10) 0.122(9) Uiso 1 1 d D A . O23 O 0.4092(15) 0.2788(15) 0.7617(7) 0.055(4) Uiso 1 1 d D A . C13 C 0.4865(16) 0.2695(15) 0.7725(13) 0.089(10) Uiso 1 1 d D . . C23 C 0.535(3) 0.1759(18) 0.7876(12) 0.080(8) Uiso 0.75 1 d PD A 1 H23A H 0.4908 0.1354 0.7974 0.096 Uiso 0.75 1 calc PR A 1 H23B H 0.5779 0.1599 0.7569 0.096 Uiso 0.75 1 calc PR A 1 C33 C 0.585(2) 0.160(2) 0.8316(10) 0.080(8) Uiso 0.75 1 d PD A 1 C43 C 0.613(3) 0.061(2) 0.8491(14) 0.116(10) Uiso 0.75 1 d PD A 1 H43A H 0.6609 0.0387 0.8229 0.174 Uiso 0.75 1 calc PR A 1 H43B H 0.5619 0.0314 0.8543 0.174 Uiso 0.75 1 calc PR A 1 H43C H 0.6340 0.0506 0.8815 0.174 Uiso 0.75 1 calc PR A 1 C53 C 0.525(3) 0.199(3) 0.8765(13) 0.116(10) Uiso 0.75 1 d PD A 1 H53A H 0.5545 0.1831 0.9062 0.174 Uiso 0.75 1 calc PR A 1 H53B H 0.4687 0.1765 0.8858 0.174 Uiso 0.75 1 calc PR A 1 H53C H 0.5135 0.2634 0.8664 0.174 Uiso 0.75 1 calc PR A 1 C63 C 0.668(3) 0.204(3) 0.8133(16) 0.116(10) Uiso 0.75 1 d PD A 1 H63A H 0.7068 0.1803 0.7841 0.174 Uiso 0.75 1 calc PR A 1 H63B H 0.7008 0.1931 0.8414 0.174 Uiso 0.75 1 calc PR A 1 H63C H 0.6507 0.2677 0.8027 0.174 Uiso 0.75 1 calc PR A 1 C231 C 0.514(6) 0.185(4) 0.810(3) 0.080(8) Uiso 0.25 1 d PD A 2 H23C H 0.4926 0.1351 0.8033 0.096 Uiso 0.25 1 calc PR A 2 H23D H 0.4881 0.1921 0.8458 0.096 Uiso 0.25 1 calc PR A 2 C331 C 0.616(6) 0.169(5) 0.801(3) 0.080(8) Uiso 0.25 1 d PD A 2 C431 C 0.653(6) 0.215(8) 0.746(4) 0.116(10) Uiso 0.25 1 d PD A 2 H43D H 0.7165 0.1912 0.7370 0.174 Uiso 0.25 1 calc PR A 2 H43E H 0.6462 0.2781 0.7451 0.174 Uiso 0.25 1 calc PR A 2 H43F H 0.6211 0.2042 0.7222 0.174 Uiso 0.25 1 calc PR A 2 C531 C 0.645(8) 0.208(9) 0.840(5) 0.116(10) Uiso 0.25 1 d PD A 2 H53D H 0.6238 0.1766 0.8747 0.174 Uiso 0.25 1 calc PR A 2 H53E H 0.6194 0.2703 0.8369 0.174 Uiso 0.25 1 calc PR A 2 H53F H 0.7099 0.2012 0.8330 0.174 Uiso 0.25 1 calc PR A 2 C631 C 0.650(9) 0.071(6) 0.808(5) 0.116(10) Uiso 0.25 1 d PD A 2 H63D H 0.6300 0.0426 0.8434 0.174 Uiso 0.25 1 calc PR A 2 H63E H 0.7156 0.0609 0.7995 0.174 Uiso 0.25 1 calc PR A 2 H63F H 0.6278 0.0455 0.7847 0.174 Uiso 0.25 1 calc PR A 2 O14 O 0.5412(12) 0.4626(15) 0.6770(7) 0.068(5) Uiso 1 1 d D . . O24 O 0.4209(11) 0.4194(11) 0.6621(5) 0.044(4) Uiso 1 1 d D . . C14 C 0.4976(13) 0.4430(14) 0.6477(5) 0.041(5) Uiso 1 1 d D . . C24 C 0.5384(13) 0.4554(10) 0.5909(5) 0.059(7) Uiso 1 1 d D . . H24A H 0.5901 0.4857 0.5850 0.071 Uiso 1 1 calc R . . H24B H 0.4942 0.4952 0.5720 0.071 Uiso 1 1 calc R . . C34 C 0.5691(11) 0.3738(10) 0.5671(5) 0.033(5) Uiso 1 1 d D . . C44 C 0.6323(14) 0.3065(13) 0.5979(6) 0.034(5) Uiso 1 1 d D . . H44A H 0.6528 0.2545 0.5820 0.051 Uiso 1 1 calc R . . H44B H 0.6008 0.2893 0.6333 0.051 Uiso 1 1 calc R . . H44C H 0.6836 0.3327 0.5981 0.051 Uiso 1 1 calc R . . C54 C 0.6180(14) 0.3978(15) 0.5109(5) 0.053(6) Uiso 1 1 d D . . H54A H 0.6382 0.3446 0.4962 0.079 Uiso 1 1 calc R . . H54B H 0.6695 0.4248 0.5099 0.079 Uiso 1 1 calc R . . H54C H 0.5775 0.4394 0.4908 0.079 Uiso 1 1 calc R . . C64 C 0.4874(13) 0.3334(14) 0.5676(8) 0.056(6) Uiso 1 1 d D . . H64A H 0.5070 0.2809 0.5521 0.084 Uiso 1 1 calc R . . H64B H 0.4474 0.3763 0.5478 0.084 Uiso 1 1 calc R . . H64C H 0.4560 0.3172 0.6031 0.084 Uiso 1 1 calc R . . O15 O 0.6981(14) 0.5775(15) 0.7513(7) 0.058(4) Uiso 1 1 d D B . O25 O 0.6509(16) 0.4511(15) 0.7494(8) 0.089(7) Uiso 1 1 d D B . C15 C 0.7109(15) 0.4979(15) 0.7447(11) 0.078(9) Uiso 1 1 d D . . C25 C 0.796(3) 0.5079(16) 0.704(2) 0.044(4) Uiso 0.25 1 d PD B 1 H25A H 0.7817 0.5493 0.6726 0.052 Uiso 0.25 1 calc PR B 1 H25B H 0.8378 0.5318 0.7173 0.052 Uiso 0.25 1 calc PR B 1 C35 C 0.839(4) 0.418(3) 0.691(2) 0.044(4) Uiso 0.25 1 d PD B 1 C45 C 0.790(7) 0.396(5) 0.654(4) 0.075(6) Uiso 0.25 1 d PD B 1 H45A H 0.8123 0.3351 0.6495 0.112 Uiso 0.25 1 calc PR B 1 H45B H 0.7993 0.4358 0.6212 0.112 Uiso 0.25 1 calc PR B 1 H45C H 0.7261 0.4015 0.6694 0.112 Uiso 0.25 1 calc PR B 1 C55 C 0.937(4) 0.420(7) 0.665(3) 0.075(6) Uiso 0.25 1 d PD B 1 H55A H 0.9708 0.4246 0.6895 0.112 Uiso 0.25 1 calc PR B 1 H55B H 0.9409 0.4706 0.6361 0.112 Uiso 0.25 1 calc PR B 1 H55C H 0.9616 0.3657 0.6512 0.112 Uiso 0.25 1 calc PR B 1 C65 C 0.834(8) 0.348(3) 0.740(3) 0.075(6) Uiso 0.25 1 d PD B 1 H65A H 0.8626 0.3646 0.7644 0.112 Uiso 0.25 1 calc PR B 1 H65B H 0.8654 0.2912 0.7321 0.112 Uiso 0.25 1 calc PR B 1 H65C H 0.7720 0.3441 0.7557 0.112 Uiso 0.25 1 calc PR B 1 C251 C 0.7927(18) 0.426(2) 0.7466(8) 0.044(4) Uiso 0.75 1 d PD B 2 H25C H 0.7739 0.3692 0.7645 0.052 Uiso 0.75 1 calc PR B 2 H25D H 0.8321 0.4404 0.7661 0.052 Uiso 0.75 1 calc PR B 2 C351 C 0.8441(17) 0.4192(17) 0.6911(10) 0.044(4) Uiso 0.75 1 d PD B 2 C451 C 0.865(2) 0.510(2) 0.6630(11) 0.075(6) Uiso 0.75 1 d PD B 2 H45D H 0.9059 0.5277 0.6794 0.112 Uiso 0.75 1 calc PR B 2 H45E H 0.8095 0.5526 0.6648 0.112 Uiso 0.75 1 calc PR B 2 H45F H 0.8920 0.5082 0.6270 0.112 Uiso 0.75 1 calc PR B 2 C551 C 0.785(2) 0.388(2) 0.6640(13) 0.075(6) Uiso 0.75 1 d PD B 2 H55D H 0.7717 0.3298 0.6826 0.112 Uiso 0.75 1 calc PR B 2 H55E H 0.8161 0.3838 0.6287 0.112 Uiso 0.75 1 calc PR B 2 H55F H 0.7295 0.4295 0.6632 0.112 Uiso 0.75 1 calc PR B 2 C651 C 0.930(2) 0.354(3) 0.6942(12) 0.075(6) Uiso 0.75 1 d PD B 2 H65D H 0.9680 0.3763 0.7104 0.112 Uiso 0.75 1 calc PR B 2 H65E H 0.9610 0.3463 0.6595 0.112 Uiso 0.75 1 calc PR B 2 H65F H 0.9159 0.2973 0.7147 0.112 Uiso 0.75 1 calc PR B 2 O16 O 0.5604(12) 0.5714(13) 0.8462(6) 0.050(4) Uiso 1 1 d D . . O26 O 0.5139(17) 0.4517(15) 0.8342(8) 0.099(7) Uiso 1 1 d D . . C16 C 0.5305(17) 0.4982(16) 0.8627(6) 0.060(7) Uiso 1 1 d D D . C26 C 0.5341(14) 0.4550(14) 0.9182(6) 0.073(8) Uiso 1 1 d D . . H26A H 0.5032 0.4035 0.9262 0.088 Uiso 0.50 1 calc PR C 1 H26B H 0.4975 0.4970 0.9398 0.088 Uiso 0.50 1 calc PR C 1 H26C H 0.4731 0.4434 0.9345 0.088 Uiso 0.50 1 calc PR C 2 H26D H 0.5448 0.5008 0.9343 0.088 Uiso 0.50 1 calc PR C 2 C36 C 0.6221(14) 0.4235(18) 0.9371(7) 0.042(8) Uiso 0.50 1 d PD D 1 C361 C 0.5965(17) 0.3717(15) 0.9359(7) 0.042(8) Uiso 0.50 1 d PD D 2 C46 C 0.606(2) 0.367(2) 0.9911(7) 0.096(6) Uiso 1 1 d D . . H46A H 0.6626 0.3365 1.0001 0.144 Uiso 0.50 1 calc PR D 1 H46B H 0.5689 0.3232 0.9917 0.144 Uiso 0.50 1 calc PR D 1 H46C H 0.5746 0.4041 1.0160 0.144 Uiso 0.50 1 calc PR D 1 H46D H 0.6315 0.3069 1.0052 0.144 Uiso 0.50 1 calc PR D 2 H46E H 0.5467 0.3823 1.0120 0.144 Uiso 0.50 1 calc PR D 2 H46F H 0.6442 0.4078 0.9914 0.144 Uiso 0.50 1 calc PR D 2 C56 C 0.6880(16) 0.371(2) 0.9001(9) 0.096(6) Uiso 1 1 d D . . H56A H 0.7384 0.3392 0.9161 0.144 Uiso 0.50 1 calc PR D 1 H56B H 0.7095 0.4105 0.8684 0.144 Uiso 0.50 1 calc PR D 1 H56C H 0.6585 0.3282 0.8920 0.144 Uiso 0.50 1 calc PR D 1 H56D H 0.7238 0.3122 0.9071 0.144 Uiso 0.50 1 calc PR D 2 H56E H 0.7182 0.4145 0.9061 0.144 Uiso 0.50 1 calc PR D 2 H56F H 0.6806 0.3844 0.8643 0.144 Uiso 0.50 1 calc PR D 2 C66 C 0.660(2) 0.504(2) 0.9394(16) 0.096(6) Uiso 0.50 1 d PD D 1 H66A H 0.7159 0.4843 0.9524 0.144 Uiso 0.50 1 calc PR D 1 H66B H 0.6175 0.5387 0.9624 0.144 Uiso 0.50 1 calc PR D 1 H66C H 0.6723 0.5398 0.9049 0.144 Uiso 0.50 1 calc PR D 1 C661 C 0.559(3) 0.2910(16) 0.9338(15) 0.096(6) Uiso 0.50 1 d PD D 2 H66D H 0.5971 0.2374 0.9467 0.144 Uiso 0.50 1 calc PR D 2 H66E H 0.5556 0.2917 0.8982 0.144 Uiso 0.50 1 calc PR D 2 H66F H 0.4987 0.2923 0.9551 0.144 Uiso 0.50 1 calc PR D 2 O17 O 0.4806(9) 0.7463(11) 0.6694(5) 0.031(3) Uiso 1 1 d D . . O27 O 0.6179(11) 0.7228(13) 0.6889(5) 0.042(4) Uiso 1 1 d D . . C17 C 0.5646(10) 0.7486(13) 0.6573(5) 0.033(5) Uiso 1 1 d D . . C27 C 0.6013(12) 0.7809(11) 0.6010(5) 0.047(6) Uiso 1 1 d D . . H27A H 0.6596 0.7985 0.5980 0.057 Uiso 1 1 calc R . . H27B H 0.5609 0.8342 0.5883 0.057 Uiso 1 1 calc R . . C37 C 0.6135(11) 0.7154(11) 0.5658(5) 0.033(5) Uiso 1 1 d D . . C47 C 0.6466(17) 0.7602(16) 0.5099(6) 0.084(9) Uiso 1 1 d D . . H47A H 0.6545 0.7186 0.4870 0.126 Uiso 1 1 calc R . . H47B H 0.7035 0.7791 0.5073 0.126 Uiso 1 1 calc R . . H47C H 0.6027 0.8114 0.5000 0.126 Uiso 1 1 calc R . . C57 C 0.5258(13) 0.6831(14) 0.5689(8) 0.043(5) Uiso 1 1 d D . . H57A H 0.5365 0.6397 0.5468 0.064 Uiso 1 1 calc R . . H57B H 0.4819 0.7330 0.5574 0.064 Uiso 1 1 calc R . . H57C H 0.5034 0.6561 0.6045 0.064 Uiso 1 1 calc R . . C67 C 0.6832(16) 0.6359(14) 0.5815(8) 0.064(7) Uiso 1 1 d D . . H67A H 0.6896 0.5927 0.5598 0.097 Uiso 1 1 calc R . . H67B H 0.6638 0.6091 0.6176 0.097 Uiso 1 1 calc R . . H67C H 0.7404 0.6552 0.5772 0.097 Uiso 1 1 calc R . . O18 O 0.5339(13) 0.7855(15) 0.8517(7) 0.062(5) Uiso 1 1 d D . . O28 O 0.6433(14) 0.7195(15) 0.7949(7) 0.060(4) Uiso 1 1 d D . . C18 C 0.6127(13) 0.7765(17) 0.8239(9) 0.088(10) Uiso 1 1 d D . . C28 C 0.6811(17) 0.8184(18) 0.8373(8) 0.167(19) Uiso 1 1 d D . . H28A H 0.6661 0.8830 0.8274 0.200 Uiso 1 1 calc R . . H28B H 0.7402 0.8001 0.8165 0.200 Uiso 1 1 calc R . . C38 C 0.6877(14) 0.7952(18) 0.8938(8) 0.077(8) Uiso 1 1 d D . . C48 C 0.609(2) 0.850(3) 0.9244(11) 0.126(14) Uiso 1 1 d D . . H48A H 0.6099 0.8315 0.9612 0.189 Uiso 1 1 calc R . . H48B H 0.5533 0.8416 0.9178 0.189 Uiso 1 1 calc R . . H48C H 0.6153 0.9125 0.9136 0.189 Uiso 1 1 calc R . . C58 C 0.7755(18) 0.813(3) 0.9024(14) 0.140(15) Uiso 1 1 d D . . H58A H 0.7777 0.7959 0.9390 0.211 Uiso 1 1 calc R . . H58B H 0.7788 0.8759 0.8909 0.211 Uiso 1 1 calc R . . H58C H 0.8257 0.7791 0.8827 0.211 Uiso 1 1 calc R . . C68 C 0.681(3) 0.697(2) 0.9134(11) 0.150(17) Uiso 1 1 d D . . H68A H 0.6804 0.6819 0.9504 0.225 Uiso 1 1 calc R . . H68B H 0.7320 0.6615 0.8953 0.225 Uiso 1 1 calc R . . H68C H 0.6258 0.6855 0.9070 0.225 Uiso 1 1 calc R . . O19 O 0.2998(11) 0.9847(14) 0.7607(7) 0.058(4) Uiso 1 1 d D . . O29 O 0.4216(14) 0.9255(13) 0.7966(6) 0.062(5) Uiso 1 1 d D . . C19 C 0.3808(12) 0.9812(15) 0.7641(7) 0.077(9) Uiso 1 1 d D . . C29 C 0.4296(14) 1.0536(13) 0.7300(7) 0.079(9) Uiso 1 1 d D . . H29A H 0.4572 1.0778 0.7517 0.095 Uiso 1 1 calc R . . H29B H 0.3853 1.1014 0.7158 0.095 Uiso 1 1 calc R . . C39 C 0.5015(12) 1.0272(14) 0.6854(7) 0.076(8) Uiso 1 1 d D . . C49 C 0.5333(19) 1.1106(19) 0.6503(10) 0.131(15) Uiso 1 1 d D . . H49A H 0.5806 1.0941 0.6219 0.197 Uiso 1 1 calc R . . H49B H 0.5561 1.1420 0.6702 0.197 Uiso 1 1 calc R . . H49C H 0.4833 1.1488 0.6364 0.197 Uiso 1 1 calc R . . C59 C 0.5818(18) 0.965(2) 0.7044(12) 0.134(15) Uiso 1 1 d D . . H59A H 0.6238 0.9447 0.6752 0.201 Uiso 1 1 calc R . . H59B H 0.5613 0.9150 0.7295 0.201 Uiso 1 1 calc R . . H59C H 0.6114 0.9972 0.7206 0.201 Uiso 1 1 calc R . . C69 C 0.4617(18) 0.9806(18) 0.6545(10) 0.083(9) Uiso 1 1 d D . . H69A H 0.5091 0.9563 0.6286 0.124 Uiso 1 1 calc R . . H69B H 0.4175 1.0228 0.6374 0.124 Uiso 1 1 calc R . . H69C H 0.4331 0.9330 0.6778 0.124 Uiso 1 1 calc R . . O110 O 0.2514(16) 0.9477(16) 0.8759(7) 0.055(4) Uiso 1 1 d D . . O210 O 0.3625(15) 0.8378(15) 0.8995(7) 0.049(4) Uiso 1 1 d D . . C110 C 0.300(2) 0.902(2) 0.9080(9) 0.059(7) Uiso 1 1 d D F . C210 C 0.298(3) 0.941(2) 0.9542(11) 0.115(12) Uiso 1 1 d D . . H21A H 0.2784 1.0050 0.9429 0.138 Uiso 0.50 1 calc PR E 1 H21B H 0.3612 0.9348 0.9559 0.138 Uiso 0.50 1 calc PR E 1 H21C H 0.2878 0.8931 0.9843 0.138 Uiso 0.50 1 calc PR E 2 H21D H 0.2424 0.9849 0.9570 0.138 Uiso 0.50 1 calc PR E 2 C310 C 0.251(3) 0.922(3) 1.0106(13) 0.120(19) Uiso 0.50 1 d PD F 1 C410 C 0.292(5) 0.964(5) 1.0427(16) 0.175(19) Uiso 0.50 1 d PD F 1 H41A H 0.2670 0.9466 1.0793 0.263 Uiso 0.50 1 calc PR F 1 H41B H 0.2792 1.0286 1.0328 0.263 Uiso 0.50 1 calc PR F 1 H41C H 0.3566 0.9452 1.0366 0.263 Uiso 0.50 1 calc PR F 1 C510 C 0.261(6) 0.823(4) 1.030(2) 0.175(19) Uiso 0.50 1 d PD F 1 H51A H 0.2331 0.8108 1.0669 0.263 Uiso 0.50 1 calc PR F 1 H51B H 0.3244 0.7980 1.0261 0.263 Uiso 0.50 1 calc PR F 1 H51C H 0.2324 0.7964 1.0108 0.263 Uiso 0.50 1 calc PR F 1 C610 C 0.152(3) 0.961(6) 1.015(2) 0.175(19) Uiso 0.50 1 d PD F 1 H61A H 0.1206 0.9442 1.0507 0.263 Uiso 0.50 1 calc PR F 1 H61B H 0.1264 0.9380 0.9923 0.263 Uiso 0.50 1 calc PR F 1 H61C H 0.1448 1.0250 1.0055 0.263 Uiso 0.50 1 calc PR F 1 C320 C 0.368(3) 0.986(3) 0.9644(18) 0.120(19) Uiso 0.50 1 d PD F 2 C420 C 0.327(5) 1.034(7) 1.009(3) 0.175(19) Uiso 0.25 1 d PD F 2 H42A H 0.3575 1.0846 1.0049 0.263 Uiso 0.25 1 calc PR F 2 H42B H 0.3350 0.9942 1.0416 0.263 Uiso 0.25 1 calc PR F 2 H42C H 0.2639 1.0549 1.0094 0.263 Uiso 0.25 1 calc PR F 2 C520 C 0.400(7) 1.051(6) 0.916(3) 0.175(19) Uiso 0.25 1 d PD F 2 H52A H 0.4208 1.0983 0.9260 0.263 Uiso 0.25 1 calc PR F 2 H52B H 0.3512 1.0769 0.8978 0.263 Uiso 0.25 1 calc PR F 2 H52C H 0.4493 1.0211 0.8937 0.263 Uiso 0.25 1 calc PR F 2 C620 C 0.447(5) 0.916(4) 0.978(5) 0.175(19) Uiso 0.25 1 d PD F 2 H62A H 0.4928 0.9449 0.9833 0.263 Uiso 0.25 1 calc PR F 2 H62B H 0.4711 0.8836 0.9502 0.263 Uiso 0.25 1 calc PR F 2 H62C H 0.4266 0.8756 1.0099 0.263 Uiso 0.25 1 calc PR F 2 C720 C 0.425(7) 1.023(8) 0.913(3) 0.175(19) Uiso 0.25 1 d PD F 2 H72A H 0.4506 1.0715 0.9176 0.263 Uiso 0.25 1 calc PR F 2 H72B H 0.3874 1.0450 0.8873 0.263 Uiso 0.25 1 calc PR F 2 H72C H 0.4725 0.9769 0.9021 0.263 Uiso 0.25 1 calc PR F 2 C820 C 0.427(6) 0.918(5) 0.997(4) 0.175(19) Uiso 0.25 1 d PD F 2 H82A H 0.4586 0.9492 1.0131 0.263 Uiso 0.25 1 calc PR F 2 H82B H 0.4710 0.8821 0.9752 0.263 Uiso 0.25 1 calc PR F 2 H82C H 0.3909 0.8811 1.0240 0.263 Uiso 0.25 1 calc PR F 2 C920 C 0.322(5) 1.060(6) 0.993(5) 0.175(19) Uiso 0.25 1 d PD F 2 H92A H 0.3668 1.0907 0.9984 0.263 Uiso 0.25 1 calc PR F 2 H92B H 0.2877 1.0362 1.0267 0.263 Uiso 0.25 1 calc PR F 2 H92C H 0.2817 1.1022 0.9731 0.263 Uiso 0.25 1 calc PR F 2 O111 O 0.0569(16) 1.0158(16) 0.7522(8) 0.059(4) Uiso 1 1 d D . . O211 O 0.1231(16) 1.0142(17) 0.8184(8) 0.067(5) Uiso 1 1 d D . . C111 C 0.0671(16) 1.0488(17) 0.7888(8) 0.066(7) Uiso 1 1 d D . . C211 C -0.0045(15) 1.1226(15) 0.8058(7) 0.053(6) Uiso 1 1 d D . . H21E H -0.0411 1.1447 0.7790 0.063 Uiso 1 1 calc R . . H21F H 0.0250 1.1713 0.8072 0.063 Uiso 1 1 calc R . . C311 C -0.0664(15) 1.0998(15) 0.8573(7) 0.080(9) Uiso 1 1 d D . . C411 C -0.1310(19) 1.1834(19) 0.8693(9) 0.075(8) Uiso 1 1 d D . . H41D H -0.1711 1.1691 0.9025 0.113 Uiso 0.50 1 calc PR . . H41E H -0.1659 1.2064 0.8422 0.113 Uiso 0.50 1 calc PR . . H41F H -0.0970 1.2278 0.8709 0.113 Uiso 0.50 1 calc PR . . H41G H -0.1182 1.2331 0.8413 0.113 Uiso 0.50 1 calc PR . . H41H H -0.1234 1.1958 0.9015 0.113 Uiso 0.50 1 calc PR . . H41I H -0.1923 1.1744 0.8728 0.113 Uiso 0.50 1 calc PR . . C511 C -0.015(2) 1.062(2) 0.9012(8) 0.079(9) Uiso 1 1 d D . . H51D H -0.0567 1.0490 0.9337 0.118 Uiso 0.50 1 calc PR . . H51E H 0.0196 1.1060 0.9036 0.118 Uiso 0.50 1 calc PR . . H51F H 0.0258 1.0088 0.8942 0.118 Uiso 0.50 1 calc PR . . H51G H 0.0492 1.0602 0.8873 0.118 Uiso 0.50 1 calc PR . . H51H H -0.0271 1.0032 0.9173 0.118 Uiso 0.50 1 calc PR . . H51I H -0.0334 1.1004 0.9268 0.118 Uiso 0.50 1 calc PR . . C611 C -0.121(2) 1.031(2) 0.8540(14) 0.21(3) Uiso 1 1 d D . . H61D H -0.1604 1.0161 0.8871 0.321 Uiso 0.50 1 calc PR . . H61E H -0.0800 0.9783 0.8456 0.321 Uiso 0.50 1 calc PR . . H61F H -0.1558 1.0556 0.8272 0.321 Uiso 0.50 1 calc PR . . H61G H -0.1037 1.0172 0.8195 0.321 Uiso 0.50 1 calc PR . . H61H H -0.1841 1.0550 0.8610 0.321 Uiso 0.50 1 calc PR . . H61I H -0.1083 0.9777 0.8794 0.321 Uiso 0.50 1 calc PR . . O112 O 0.1634(14) 0.6935(14) 0.8561(6) 0.058(4) Uiso 1 1 d D . . O212 O 0.1122(16) 0.8260(14) 0.8809(8) 0.081(6) Uiso 1 1 d D . . C112 C 0.1216(18) 0.7420(14) 0.8889(7) 0.079(9) Uiso 1 1 d D . . C212 C 0.0662(19) 0.6964(19) 0.9374(8) 0.138(15) Uiso 1 1 d D G . H21G H 0.0920 0.6333 0.9438 0.166 Uiso 1 1 calc R . . H21H H 0.0054 0.7008 0.9313 0.166 Uiso 1 1 calc R . . C312 C 0.0592(18) 0.7326(17) 0.9856(7) 0.089(10) Uiso 1 1 d D . . C412 C 0.026(10) 0.832(2) 0.976(2) 0.183(16) Uiso 0.25 1 d PD G 1 H41J H 0.0304 0.8558 1.0050 0.275 Uiso 0.25 1 calc PR G 1 H41K H -0.0355 0.8431 0.9714 0.275 Uiso 0.25 1 calc PR G 1 H41L H 0.0635 0.8597 0.9445 0.275 Uiso 0.25 1 calc PR G 1 C512 C 0.151(3) 0.715(9) 1.000(4) 0.183(16) Uiso 0.25 1 d PD G 1 H51J H 0.1475 0.7403 1.0301 0.275 Uiso 0.25 1 calc PR G 1 H51K H 0.1939 0.7409 0.9711 0.275 Uiso 0.25 1 calc PR G 1 H51L H 0.1710 0.6510 1.0083 0.275 Uiso 0.25 1 calc PR G 1 C612 C -0.006(8) 0.687(8) 1.0302(17) 0.183(16) Uiso 0.25 1 d PD G 1 H61J H -0.0052 0.7060 1.0619 0.275 Uiso 0.25 1 calc PR G 1 H61K H 0.0122 0.6235 1.0344 0.275 Uiso 0.25 1 calc PR G 1 H61L H -0.0659 0.7034 1.0227 0.275 Uiso 0.25 1 calc PR G 1 C422 C 0.036(4) 0.663(3) 1.0335(8) 0.183(16) Uiso 0.75 1 d PD G 2 H42D H 0.0410 0.6825 1.0641 0.275 Uiso 0.75 1 calc PR G 2 H42E H 0.0775 0.6076 1.0303 0.275 Uiso 0.75 1 calc PR G 2 H42F H -0.0248 0.6526 1.0369 0.275 Uiso 0.75 1 calc PR G 2 C522 C 0.148(2) 0.759(3) 0.9852(16) 0.183(16) Uiso 0.75 1 d PD G 2 H52D H 0.1446 0.7799 1.0168 0.275 Uiso 0.75 1 calc PR G 2 H52E H 0.1620 0.8055 0.9554 0.275 Uiso 0.75 1 calc PR G 2 H52F H 0.1955 0.7076 0.9830 0.275 Uiso 0.75 1 calc PR G 2 C622 C -0.014(3) 0.814(3) 0.9868(16) 0.183(16) Uiso 0.75 1 d PD G 2 H62D H -0.0132 0.8410 1.0156 0.275 Uiso 0.75 1 calc PR G 2 H62E H -0.0717 0.7960 0.9913 0.275 Uiso 0.75 1 calc PR G 2 H62F H -0.0024 0.8559 0.9545 0.275 Uiso 0.75 1 calc PR G 2 O113 O 0.0391(12) 0.9674(12) 0.6688(7) 0.052(4) Uiso 1 1 d D . . O213 O -0.0036(13) 0.8601(11) 0.6410(6) 0.047(4) Uiso 1 1 d D . . C113 C -0.0078(15) 0.9399(12) 0.6449(10) 0.067(7) Uiso 1 1 d D . . C213 C -0.0792(15) 1.0080(15) 0.6224(8) 0.084(9) Uiso 1 1 d D . . H21I H -0.0493 1.0509 0.5946 0.101 Uiso 1 1 calc R . . H21J H -0.1117 0.9780 0.6063 0.101 Uiso 1 1 calc R . . C313 C -0.1469(15) 1.0588(17) 0.6594(9) 0.106(12) Uiso 1 1 d D . . C413 C -0.183(2) 0.995(2) 0.7082(10) 0.113(12) Uiso 1 1 d D . . H41M H -0.2242 1.0283 0.7325 0.170 Uiso 1 1 calc R . . H41N H -0.1330 0.9611 0.7241 0.170 Uiso 1 1 calc R . . H41O H -0.2135 0.9547 0.6990 0.170 Uiso 1 1 calc R . . C513 C -0.107(2) 1.127(2) 0.6751(13) 0.115(12) Uiso 1 1 d D . . H51M H -0.1512 1.1555 0.7007 0.173 Uiso 1 1 calc R . . H51N H -0.0893 1.1716 0.6447 0.173 Uiso 1 1 calc R . . H51O H -0.0545 1.0979 0.6898 0.173 Uiso 1 1 calc R . . C613 C -0.225(2) 1.107(2) 0.6329(14) 0.157(18) Uiso 1 1 d D . . H61M H -0.2701 1.1387 0.6566 0.235 Uiso 1 1 calc R . . H61N H -0.2519 1.0634 0.6234 0.235 Uiso 1 1 calc R . . H61O H -0.2037 1.1480 0.6020 0.235 Uiso 1 1 calc R . . O114 O 0.2729(11) 0.3207(12) 0.7133(7) 0.049(4) Uiso 1 1 d D . . O214 O 0.1564(12) 0.4168(10) 0.6847(6) 0.035(3) Uiso 1 1 d D . . C114 C 0.2006(12) 0.3398(10) 0.6958(8) 0.041(5) Uiso 1 1 d D . . C214 C 0.1629(12) 0.2636(11) 0.6889(5) 0.052(6) Uiso 1 1 d D . . H21K H 0.0972 0.2767 0.6983 0.062 Uiso 1 1 calc R . . H21L H 0.1827 0.2107 0.7136 0.062 Uiso 1 1 calc R . . C314 C 0.1878(10) 0.2414(10) 0.6354(5) 0.030(4) Uiso 1 1 d D . . C414 C 0.2849(11) 0.1939(16) 0.6260(8) 0.056(6) Uiso 1 1 d D . . H41P H 0.3026 0.1850 0.5904 0.083 Uiso 1 1 calc R . . H41Q H 0.2898 0.1369 0.6495 0.083 Uiso 1 1 calc R . . H41R H 0.3239 0.2298 0.6322 0.083 Uiso 1 1 calc R . . C514 C 0.1258(13) 0.1820(14) 0.6298(8) 0.054(6) Uiso 1 1 d D . . H51P H 0.1418 0.1693 0.5949 0.081 Uiso 1 1 calc R . . H51Q H 0.0641 0.2119 0.6360 0.081 Uiso 1 1 calc R . . H51R H 0.1321 0.1269 0.6548 0.081 Uiso 1 1 calc R . . C614 C 0.1793(15) 0.3268(12) 0.5949(6) 0.045(5) Uiso 1 1 d D . . H61P H 0.1998 0.3130 0.5604 0.068 Uiso 1 1 calc R . . H61Q H 0.2158 0.3665 0.5996 0.068 Uiso 1 1 calc R . . H61R H 0.1170 0.3552 0.5989 0.068 Uiso 1 1 calc R . . O115 O 0.2241(12) 0.5148(10) 0.8239(5) 0.042(4) Uiso 1 1 d D . . O215 O 0.2546(14) 0.3696(12) 0.8175(6) 0.048(4) Uiso 1 1 d D . . C115 C 0.2260(14) 0.4324(11) 0.8425(5) 0.038(5) Uiso 1 1 d D . . C215 C 0.1814(12) 0.4095(14) 0.8986(5) 0.064(7) Uiso 1 1 d D . . H21M H 0.1574 0.3544 0.9037 0.077 Uiso 1 1 calc R . . H21N H 0.1303 0.4564 0.9058 0.077 Uiso 1 1 calc R . . C315 C 0.2400(13) 0.3980(14) 0.9377(6) 0.062(7) Uiso 1 1 d D . . C415 C 0.3082(19) 0.3132(17) 0.9352(10) 0.083(9) Uiso 1 1 d D . . H41S H 0.3456 0.3057 0.9606 0.124 Uiso 0.50 1 calc PR . . H41T H 0.3456 0.3172 0.9007 0.124 Uiso 0.50 1 calc PR . . H41U H 0.2769 0.2629 0.9427 0.124 Uiso 0.50 1 calc PR . . H41V H 0.2998 0.2848 0.9087 0.124 Uiso 0.50 1 calc PR . . H41W H 0.2998 0.2733 0.9686 0.124 Uiso 0.50 1 calc PR . . H41X H 0.3685 0.3276 0.9267 0.124 Uiso 0.50 1 calc PR . . C515 C 0.1836(19) 0.393(2) 0.9926(6) 0.115(12) Uiso 1 1 d D . . H51S H 0.2225 0.3855 1.0171 0.173 Uiso 1 1 calc R . . H51T H 0.1516 0.3428 1.0010 0.173 Uiso 1 1 calc R . . H51U H 0.1407 0.4473 0.9944 0.173 Uiso 1 1 calc R . . C615 C 0.2896(15) 0.4771(16) 0.9252(9) 0.065(7) Uiso 1 1 d D . . H61S H 0.3276 0.4698 0.9502 0.098 Uiso 1 1 calc R . . H61T H 0.2464 0.5312 0.9268 0.098 Uiso 1 1 calc R . . H61U H 0.3265 0.4806 0.8906 0.098 Uiso 1 1 calc R . . O116 O 0.0520(17) 0.5594(14) 0.7260(7) 0.070(5) Uiso 1 1 d D . . O216 O 0.0072(15) 0.7050(12) 0.7267(6) 0.063(5) Uiso 1 1 d D . . C116 C 0.018(2) 0.6242(12) 0.7491(6) 0.094(10) Uiso 1 1 d D . . C216 C 0.0042(17) 0.6036(15) 0.8073(6) 0.084(9) Uiso 1 1 d D . . H210 H -0.0174 0.6593 0.8202 0.100 Uiso 1 1 calc R . . H21P H 0.0625 0.5786 0.8171 0.100 Uiso 1 1 calc R . . C316 C -0.0608(14) 0.5399(14) 0.8342(6) 0.060(7) Uiso 1 1 d D . . C416 C -0.017(2) 0.4464(15) 0.8268(11) 0.128(14) Uiso 1 1 d D . . H41Y H -0.0567 0.4048 0.8457 0.192 Uiso 1 1 calc R . . H41Z H 0.0390 0.4309 0.8398 0.192 Uiso 1 1 calc R . . H411 H -0.0037 0.4441 0.7901 0.192 Uiso 1 1 calc R . . C516 C -0.1468(17) 0.565(2) 0.8125(11) 0.134(15) Uiso 1 1 d D . . H51V H -0.1861 0.5214 0.8294 0.202 Uiso 1 1 calc R . . H51W H -0.1321 0.5658 0.7754 0.202 Uiso 1 1 calc R . . H51X H -0.1769 0.6230 0.8188 0.202 Uiso 1 1 calc R . . C616 C -0.0837(18) 0.543(2) 0.8920(7) 0.090(10) Uiso 1 1 d D . . H61V H -0.1207 0.4985 0.9105 0.135 Uiso 1 1 calc R . . H61W H -0.1162 0.6014 0.8969 0.135 Uiso 1 1 calc R . . H61X H -0.0287 0.5317 0.9053 0.135 Uiso 1 1 calc R . . O117 O 0.1106(14) 0.5617(12) 0.6160(6) 0.041(3) Uiso 1 1 d D . . O217 O 0.0370(13) 0.7026(11) 0.6126(6) 0.041(4) Uiso 1 1 d D . . C117 C 0.0592(18) 0.6293(12) 0.5968(8) 0.050(6) Uiso 1 1 d D . . C217 C 0.0160(14) 0.6205(16) 0.5544(7) 0.063(7) Uiso 1 1 d D . . H21Q H -0.0349 0.6689 0.5514 0.076 Uiso 1 1 calc R . . H21R H -0.0085 0.5648 0.5650 0.076 Uiso 1 1 calc R . . C317 C 0.0748(16) 0.6214(17) 0.5013(7) 0.135(15) Uiso 1 1 d D . . C417 C 0.016(2) 0.640(2) 0.4607(9) 0.078(8) Uiso 1 1 d D . . H412 H 0.0536 0.6446 0.4263 0.117 Uiso 1 1 calc R . . H413 H -0.0252 0.6952 0.4632 0.117 Uiso 1 1 calc R . . H414 H -0.0181 0.5919 0.4669 0.117 Uiso 1 1 calc R . . C517 C 0.137(2) 0.533(2) 0.4984(12) 0.165(19) Uiso 1 1 d D . . H51Y H 0.1774 0.5369 0.4648 0.247 Uiso 1 1 calc R . . H51Z H 0.1016 0.4865 0.5029 0.247 Uiso 1 1 calc R . . H511 H 0.1718 0.5190 0.5257 0.247 Uiso 1 1 calc R . . C617 C 0.132(2) 0.695(2) 0.4891(11) 0.121(14) Uiso 1 1 d D . . H61Y H 0.1704 0.6946 0.4550 0.182 Uiso 1 1 calc R . . H61Z H 0.1690 0.6841 0.5150 0.182 Uiso 1 1 calc R . . H611 H 0.0932 0.7516 0.4894 0.182 Uiso 1 1 calc R . . O118 O 0.3092(14) 0.7812(16) 0.6170(7) 0.052(4) Uiso 1 1 d D H . O218 O 0.1854(13) 0.8086(16) 0.5820(8) 0.067(5) Uiso 1 1 d D H . C118 C 0.2682(14) 0.8092(17) 0.5792(7) 0.056(5) Uiso 1 1 d D . . C218 C 0.331(2) 0.856(2) 0.5334(12) 0.056(5) Uiso 0.50 1 d PD H 1 H21S H 0.3827 0.8650 0.5448 0.068 Uiso 0.50 1 calc PR H 1 H21T H 0.3521 0.8185 0.5069 0.068 Uiso 0.50 1 calc PR H 1 C318 C 0.280(2) 0.944(2) 0.5106(12) 0.056(5) Uiso 0.50 1 d PD H 1 C418 C 0.346(4) 1.001(2) 0.475(2) 0.104(10) Uiso 0.50 1 d PD H 1 H415 H 0.3134 1.0527 0.4555 0.156 Uiso 0.50 1 calc PR H 1 H416 H 0.3870 0.9670 0.4505 0.156 Uiso 0.50 1 calc PR H 1 H417 H 0.3799 1.0201 0.4950 0.156 Uiso 0.50 1 calc PR H 1 C518 C 0.218(3) 0.927(4) 0.479(2) 0.104(10) Uiso 0.50 1 d PD H 1 H512 H 0.1775 0.8880 0.5015 0.156 Uiso 0.50 1 calc PR H 1 H513 H 0.2537 0.8986 0.4509 0.156 Uiso 0.50 1 calc PR H 1 H514 H 0.1838 0.9825 0.4653 0.156 Uiso 0.50 1 calc PR H 1 C618 C 0.226(4) 0.992(4) 0.5533(19) 0.104(10) Uiso 0.50 1 d PD H 1 H612 H 0.1827 0.9560 0.5758 0.156 Uiso 0.50 1 calc PR H 1 H613 H 0.1942 1.0484 0.5381 0.156 Uiso 0.50 1 calc PR H 1 H614 H 0.2657 1.0022 0.5734 0.156 Uiso 0.50 1 calc PR H 1 C228 C 0.305(3) 0.856(2) 0.5249(10) 0.056(5) Uiso 0.50 1 d PD H 2 H22A H 0.3634 0.8230 0.5116 0.068 Uiso 0.50 1 calc PR H 2 H22B H 0.2641 0.8576 0.5019 0.068 Uiso 0.50 1 calc PR H 2 C328 C 0.316(2) 0.950(2) 0.5237(12) 0.056(5) Uiso 0.50 1 d PD H 2 C428 C 0.225(3) 1.009(4) 0.530(2) 0.104(10) Uiso 0.50 1 d PD H 2 H42G H 0.1884 0.9866 0.5634 0.156 Uiso 0.50 1 calc PR H 2 H42H H 0.1957 1.0091 0.5024 0.156 Uiso 0.50 1 calc PR H 2 H42I H 0.2327 1.0692 0.5298 0.156 Uiso 0.50 1 calc PR H 2 C528 C 0.374(4) 0.986(3) 0.4722(18) 0.104(10) Uiso 0.50 1 d PD H 2 H52G H 0.3774 1.0476 0.4708 0.156 Uiso 0.50 1 calc PR H 2 H52H H 0.3465 0.9822 0.4440 0.156 Uiso 0.50 1 calc PR H 2 H52I H 0.4333 0.9513 0.4690 0.156 Uiso 0.50 1 calc PR H 2 C628 C 0.361(4) 0.952(4) 0.568(2) 0.104(10) Uiso 0.50 1 d PD H 2 H62G H 0.3223 0.9346 0.6006 0.156 Uiso 0.50 1 calc PR H 2 H62H H 0.3731 1.0115 0.5648 0.156 Uiso 0.50 1 calc PR H 2 H62I H 0.4177 0.9110 0.5653 0.156 Uiso 0.50 1 calc PR H 2 N1A N 0.833(3) 0.826(3) 0.6005(15) 0.205(12) Uiso 0.75 1 d PD . . C1A C 0.810(5) 0.736(4) 0.623(3) 0.205(12) Uiso 0.75 1 d PD . . H1A1 H 0.8408 0.6960 0.5990 0.308 Uiso 0.75 1 calc PR . . H1A2 H 0.7456 0.7380 0.6275 0.308 Uiso 0.75 1 calc PR . . H1A3 H 0.8286 0.7139 0.6558 0.308 Uiso 0.75 1 calc PR . . O2A O 0.894(3) 0.834(4) 0.5621(18) 0.205(12) Uiso 0.75 1 d PD . . O3A O 0.790(4) 0.887(4) 0.6217(19) 0.205(12) Uiso 0.75 1 d PD . . C1B C 0.189(3) 1.217(6) 0.863(2) 0.11(2) Uiso 0.50 1 d PD . . H1B1 H 0.1993 1.1770 0.8959 0.130 Uiso 0.50 1 calc PR . . H1B2 H 0.1929 1.2774 0.8666 0.130 Uiso 0.50 1 calc PR . . Cl1B Cl 0.085(3) 1.215(4) 0.8535(19) 0.28(2) Uiso 0.50 1 d PD . . Cl2B Cl 0.272(3) 1.186(4) 0.8129(17) 0.243(17) Uiso 0.50 1 d PD . . 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 0.044(5) 0.063(6) 0.023(3) -0.024(4) -0.014(4) 0.024(6) Mn2 0.046(5) 0.040(6) 0.030(3) -0.012(4) -0.019(4) 0.010(6) Mn3 0.040(5) 0.044(6) 0.035(3) -0.006(4) -0.016(4) 0.014(6) Mn4 0.047(5) 0.047(6) 0.036(3) -0.019(4) -0.009(4) 0.020(6) Mn5 0.077(7) 0.049(7) 0.042(3) -0.022(5) -0.013(5) 0.027(7) Mn6 0.063(5) 0.075(6) 0.045(3) -0.040(4) -0.026(4) 0.018(6) Mn7 0.064(5) 0.085(6) 0.052(3) -0.045(4) -0.038(4) 0.033(6) Mn8 0.053(6) 0.039(6) 0.079(4) -0.026(5) -0.046(5) 0.019(6) Mn9 0.077(6) 0.066(6) 0.042(3) -0.025(4) -0.037(4) 0.027(6) Mn10 0.046(5) 0.059(6) 0.026(3) -0.014(4) -0.019(4) 0.012(5) Mn11 0.047(6) 0.052(6) 0.053(3) -0.003(4) -0.032(4) 0.011(6) Mn12 0.058(7) 0.057(7) 0.069(4) -0.022(5) -0.027(5) 0.036(7) _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 O108 1.844(10) . ? Mn1 O124 1.86(3) . ? Mn1 O107 1.889(17) . ? Mn1 O17 1.898(19) . ? Mn1 O134 1.917(11) . ? Mn1 O123 1.99(2) . ? Mn1 Mn7 2.787(5) . ? Mn1 Mn4 2.822(6) . ? Mn1 Mn2 2.841(9) . ? Mn1 Mn3 2.927(5) . ? Mn2 O209 1.816(18) . ? Mn2 O208 1.837(11) . ? Mn2 O115 1.84(2) . ? Mn2 O123 1.86(3) . ? Mn2 O234 1.935(12) . ? Mn2 O124 1.955(19) . ? Mn2 Mn9 2.768(6) . ? Mn2 Mn3 2.832(6) . ? Mn2 Mn4 2.915(5) . ? Mn3 O234 1.85(3) . ? Mn3 O311 1.872(11) . ? Mn3 O310 1.88(2) . ? Mn3 O123 1.895(11) . ? Mn3 O134 1.92(2) . ? Mn3 O118 1.95(3) . ? Mn3 Mn11 2.784(6) . ? Mn3 Mn4 2.808(4) . ? Mn4 O405 1.853(13) . ? Mn4 O234 1.86(2) . ? Mn4 O406 1.881(19) . ? Mn4 O134 1.90(3) . ? Mn4 O124 1.925(10) . ? Mn4 O112 1.94(3) . ? Mn4 Mn5 2.796(6) . ? Mn5 O406 1.820(11) . ? Mn5 O211 1.922(14) . ? Mn5 O405 1.962(19) . ? Mn5 O110 1.963(16) . ? Mn5 O19 2.17(3) . ? Mn5 O212 2.27(3) . ? Mn6 O406 1.892(19) . ? Mn6 O107 1.922(11) . ? Mn6 O18 1.956(19) . ? Mn6 O210 1.963(13) . ? Mn6 O29 2.06(2) . ? Mn6 O6 2.31(3) . ? Mn7 O108 1.839(19) . ? Mn7 O28 1.90(2) . ? Mn7 O107 1.898(11) . ? Mn7 O15 1.981(16) . ? Mn7 O16 2.140(19) . ? Mn7 O27 2.18(2) . ? Mn8 O208 1.94(2) . ? Mn8 O108 1.98(2) . ? Mn8 O13 2.02(3) . ? Mn8 O26 2.034(17) . ? Mn8 O25 2.04(3) . ? Mn8 O14 2.082(15) . ? Mn9 O208 1.87(2) . ? Mn9 O209 1.929(12) . ? Mn9 O114 1.946(18) . ? Mn9 O23 1.982(17) . ? Mn9 O24 2.151(17) . ? Mn9 O215 2.18(2) . ? Mn10 O209 1.880(11) . ? Mn10 O310 1.89(3) . ? Mn10 O214 1.91(2) . ? Mn10 O117 1.950(11) . ? Mn10 O116 2.09(2) . ? Mn10 O10 2.27(2) . ? Mn11 O311 1.883(18) . ? Mn11 O217 1.891(15) . ? Mn11 O310 1.937(11) . ? Mn11 O213 1.960(12) . ? Mn11 O218 2.18(3) . ? Mn11 O216 2.18(2) . ? Mn12 O311 1.870(13) . ? Mn12 O405 1.884(13) . ? Mn12 O113 1.926(13) . ? Mn12 O111 1.959(14) . ? Mn12 O121 2.12(3) . ? Mn12 O120 2.31(4) . ? O13 C13 1.258(10) . ? O23 C13 1.257(10) . ? C13 C231 1.501(9) . ? C13 C23 1.502(9) . ? C23 C33 1.499(9) . ? C33 C43 1.498(9) . ? C33 C53 1.501(9) . ? C33 C63 1.501(9) . ? C231 C331 1.501(9) . ? C331 C631 1.498(9) . ? C331 C431 1.500(9) . ? C331 C531 1.501(9) . ? O14 C14 1.261(9) . ? O24 C14 1.254(10) . ? C14 C24 1.483(11) . ? C24 C34 1.488(10) . ? C34 C44 1.507(8) . ? C34 C64 1.510(8) . ? C34 C54 1.512(8) . ? O15 C15 1.257(10) . ? O25 C15 1.254(10) . ? C15 C251 1.499(9) . ? C15 C25 1.502(9) . ? C25 C35 1.500(9) . ? C35 C55 1.499(9) . ? C35 C45 1.500(9) . ? C35 C65 1.500(9) . ? C251 C351 1.52(2) . ? C351 C651 1.494(9) . ? C351 C551 1.496(9) . ? C351 C451 1.497(9) . ? O16 C16 1.260(10) . ? O26 C16 1.258(9) . ? C16 C26 1.488(11) . ? C26 C361 1.494(8) . ? C26 C36 1.501(8) . ? C36 C56 1.496(8) . ? C36 C46 1.501(8) . ? C36 C66 1.504(8) . ? C361 C46 1.495(8) . ? C361 C56 1.503(8) . ? C361 C661 1.505(8) . ? O17 C17 1.259(10) . ? O27 C17 1.254(9) . ? C17 C27 1.485(11) . ? C27 C37 1.494(10) . ? C37 C67 1.507(8) . ? C37 C57 1.509(8) . ? C37 C47 1.509(8) . ? O18 C18 1.261(10) . ? O28 C18 1.256(9) . ? C18 C28 1.490(11) . ? C28 C38 1.491(10) . ? C38 C58 1.508(8) . ? C38 C48 1.510(8) . ? C38 C68 1.510(8) . ? O19 C19 1.258(9) . ? O29 C19 1.256(9) . ? C19 C29 1.486(12) . ? C29 C39 1.492(10) . ? C39 C69 1.508(8) . ? C39 C59 1.510(8) . ? C39 C49 1.510(8) . ? O110 C110 1.260(9) . ? O210 C110 1.259(9) . ? C110 C210 1.488(12) . ? C210 C310 1.500(8) . ? C210 C320 1.500(8) . ? C310 C610 1.500(8) . ? C310 C410 1.500(8) . ? C310 C510 1.500(8) . ? C320 C420 1.499(8) . ? C320 C720 1.500(8) . ? C320 C920 1.500(8) . ? C320 C520 1.500(8) . ? C320 C820 1.501(8) . ? C320 C620 1.501(8) . ? O111 C111 1.256(10) . ? O211 C111 1.258(9) . ? C111 C211 1.487(11) . ? C211 C311 1.491(10) . ? C311 C511 1.506(8) . ? C311 C611 1.510(8) . ? C311 C411 1.511(8) . ? O112 C112 1.260(9) . ? O212 C112 1.255(9) . ? C112 C212 1.487(12) . ? C212 C312 1.494(9) . ? C312 C412 1.499(8) . ? C312 C422 1.501(8) . ? C312 C612 1.501(8) . ? C312 C622 1.502(8) . ? C312 C522 1.503(8) . ? C312 C512 1.505(8) . ? O113 C113 1.255(9) . ? O213 C113 1.254(10) . ? C113 C213 1.489(11) . ? C213 C313 1.489(10) . ? C313 C413 1.509(8) . ? C313 C513 1.510(8) . ? C313 C613 1.513(8) . ? O114 C114 1.257(9) . ? O214 C114 1.254(9) . ? C114 C214 1.485(11) . ? C214 C314 1.491(10) . ? C314 C514 1.509(8) . ? C314 C614 1.509(8) . ? C314 C414 1.511(8) . ? O115 C115 1.258(9) . ? O215 C115 1.255(9) . ? C115 C215 1.488(11) . ? C215 C315 1.490(10) . ? C315 C415 1.507(8) . ? C315 C615 1.510(8) . ? C315 C515 1.511(8) . ? O116 C116 1.259(9) . ? O216 C116 1.255(10) . ? C116 C216 1.487(11) . ? C216 C316 1.494(11) . ? C316 C416 1.507(8) . ? C316 C516 1.507(8) . ? C316 C616 1.510(8) . ? O117 C117 1.259(9) . ? O217 C117 1.258(9) . ? C117 C217 1.486(11) . ? C217 C317 1.489(10) . ? C317 C617 1.509(8) . ? C317 C517 1.510(8) . ? C317 C417 1.511(8) . ? O118 C118 1.261(9) . ? O218 C118 1.257(10) . ? C118 C228 1.502(9) . ? C118 C218 1.504(9) . ? C218 C318 1.500(9) . ? C318 C618 1.497(9) . ? C318 C418 1.501(9) . ? C318 C518 1.504(9) . ? C228 C328 1.499(9) . ? C328 C528 1.500(9) . ? C328 C428 1.501(9) . ? C328 C628 1.501(9) . ? N1A O3A 1.214(8) . ? N1A O2A 1.217(9) . ? N1A C1A 1.477(9) . ? C1B Cl1B 1.698(9) . ? C1B Cl2B 1.701(9) . ? 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 O108 Mn1 O124 96.6(8) . . ? O108 Mn1 O107 82.8(6) . . ? O124 Mn1 O107 90.4(9) . . ? O108 Mn1 O17 90.3(8) . . ? O124 Mn1 O17 172.8(5) . . ? O107 Mn1 O17 92.7(9) . . ? O108 Mn1 O134 176.4(6) . . ? O124 Mn1 O134 84.2(9) . . ? O107 Mn1 O134 100.7(6) . . ? O17 Mn1 O134 88.9(9) . . ? O108 Mn1 O123 96.4(6) . . ? O124 Mn1 O123 83.2(9) . . ? O107 Mn1 O123 173.4(11) . . ? O17 Mn1 O123 93.8(8) . . ? O134 Mn1 O123 80.1(7) . . ? O108 Mn1 Mn7 40.8(6) . . ? O124 Mn1 Mn7 100.4(4) . . ? O107 Mn1 Mn7 42.7(3) . . ? O17 Mn1 Mn7 86.3(4) . . ? O134 Mn1 Mn7 142.7(7) . . ? O123 Mn1 Mn7 137.1(3) . . ? O108 Mn1 Mn4 139.1(7) . . ? O124 Mn1 Mn4 42.7(3) . . ? O107 Mn1 Mn4 92.1(5) . . ? O17 Mn1 Mn4 130.6(4) . . ? O134 Mn1 Mn4 42.1(7) . . ? O123 Mn1 Mn4 84.2(5) . . ? Mn7 Mn1 Mn4 126.86(12) . . ? O108 Mn1 Mn2 92.3(8) . . ? O124 Mn1 Mn2 43.2(6) . . ? O107 Mn1 Mn2 132.6(8) . . ? O17 Mn1 Mn2 134.6(4) . . ? O134 Mn1 Mn2 85.8(9) . . ? O123 Mn1 Mn2 40.8(7) . . ? Mn7 Mn1 Mn2 122.7(2) . . ? Mn4 Mn1 Mn2 61.96(18) . . ? O108 Mn1 Mn3 136.2(5) . . ? O124 Mn1 Mn3 84.0(4) . . ? O107 Mn1 Mn3 140.9(4) . . ? O17 Mn1 Mn3 89.5(4) . . ? O134 Mn1 Mn3 40.3(6) . . ? O123 Mn1 Mn3 39.9(3) . . ? Mn7 Mn1 Mn3 174.70(17) . . ? Mn4 Mn1 Mn3 58.44(12) . . ? Mn2 Mn1 Mn3 58.80(18) . . ? O209 Mn2 O208 85.3(6) . . ? O209 Mn2 O115 93.1(10) . . ? O208 Mn2 O115 91.3(9) . . ? O209 Mn2 O123 88.9(9) . . ? O208 Mn2 O123 94.6(9) . . ? O115 Mn2 O123 173.9(5) . . ? O209 Mn2 O234 97.7(7) . . ? O208 Mn2 O234 174.9(14) . . ? O115 Mn2 O234 92.6(9) . . ? O123 Mn2 O234 81.4(9) . . ? O209 Mn2 O124 172.8(11) . . ? O208 Mn2 O124 97.1(7) . . ? O115 Mn2 O124 93.6(8) . . ? O123 Mn2 O124 84.2(9) . . ? O234 Mn2 O124 79.6(7) . . ? O209 Mn2 Mn9 44.0(4) . . ? O208 Mn2 Mn9 42.1(6) . . ? O115 Mn2 Mn9 86.4(5) . . ? O123 Mn2 Mn9 99.0(5) . . ? O234 Mn2 Mn9 141.3(6) . . ? O124 Mn2 Mn9 139.1(3) . . ? O209 Mn2 Mn3 88.6(6) . . ? O208 Mn2 Mn3 135.8(8) . . ? O115 Mn2 Mn3 132.7(4) . . ? O123 Mn2 Mn3 41.5(3) . . ? O234 Mn2 Mn3 40.5(7) . . ? O124 Mn2 Mn3 85.0(5) . . ? Mn9 Mn2 Mn3 123.80(13) . . ? O209 Mn2 Mn1 132.8(9) . . ? O208 Mn2 Mn1 91.4(9) . . ? O115 Mn2 Mn1 134.1(5) . . ? O123 Mn2 Mn1 44.4(6) . . ? O234 Mn2 Mn1 83.6(9) . . ? O124 Mn2 Mn1 40.6(7) . . ? Mn9 Mn2 Mn1 123.5(2) . . ? Mn3 Mn2 Mn1 62.12(19) . . ? O209 Mn2 Mn4 136.5(4) . . ? O208 Mn2 Mn4 138.0(6) . . ? O115 Mn2 Mn4 90.8(4) . . ? O123 Mn2 Mn4 83.8(5) . . ? O234 Mn2 Mn4 38.9(6) . . ? O124 Mn2 Mn4 40.9(3) . . ? Mn9 Mn2 Mn4 177.2(3) . . ? Mn3 Mn2 Mn4 58.47(13) . . ? Mn1 Mn2 Mn4 58.71(18) . . ? O234 Mn3 O311 85.9(8) . . ? O234 Mn3 O310 89.5(10) . . ? O311 Mn3 O310 85.7(7) . . ? O234 Mn3 O123 82.7(8) . . ? O311 Mn3 O123 168.6(10) . . ? O310 Mn3 O123 95.0(7) . . ? O234 Mn3 O134 82.6(9) . . ? O311 Mn3 O134 95.2(6) . . ? O310 Mn3 O134 171.9(11) . . ? O123 Mn3 O134 82.6(7) . . ? O234 Mn3 O118 177.9(9) . . ? O311 Mn3 O118 92.9(8) . . ? O310 Mn3 O118 92.2(8) . . ? O123 Mn3 O118 98.4(8) . . ? O134 Mn3 O118 95.8(10) . . ? O234 Mn3 Mn11 92.5(6) . . ? O311 Mn3 Mn11 42.3(5) . . ? O310 Mn3 Mn11 44.0(4) . . ? O123 Mn3 Mn11 138.9(7) . . ? O134 Mn3 Mn11 137.5(4) . . ? O118 Mn3 Mn11 87.7(5) . . ? O234 Mn3 Mn4 40.9(7) . . ? O311 Mn3 Mn4 84.6(3) . . ? O310 Mn3 Mn4 129.9(8) . . ? O123 Mn3 Mn4 86.3(3) . . ? O134 Mn3 Mn4 42.4(8) . . ? O118 Mn3 Mn4 137.3(7) . . ? Mn11 Mn3 Mn4 116.0(2) . . ? O234 Mn3 Mn2 42.7(4) . . ? O311 Mn3 Mn2 128.2(8) . . ? O310 Mn3 Mn2 87.1(6) . . ? O123 Mn3 Mn2 40.7(8) . . ? O134 Mn3 Mn2 86.0(6) . . ? O118 Mn3 Mn2 138.7(4) . . ? Mn11 Mn3 Mn2 118.1(3) . . ? Mn4 Mn3 Mn2 62.24(13) . . ? O234 Mn3 Mn1 82.5(6) . . ? O311 Mn3 Mn1 134.9(5) . . ? O310 Mn3 Mn1 137.3(4) . . ? O123 Mn3 Mn1 42.5(6) . . ? O134 Mn3 Mn1 40.2(3) . . ? O118 Mn3 Mn1 97.2(6) . . ? Mn11 Mn3 Mn1 174.7(2) . . ? Mn4 Mn3 Mn1 58.91(12) . . ? Mn2 Mn3 Mn1 59.08(17) . . ? O405 Mn4 O234 101.1(7) . . ? O405 Mn4 O406 84.2(7) . . ? O234 Mn4 O406 172.4(8) . . ? O405 Mn4 O134 88.6(9) . . ? O234 Mn4 O134 83.0(9) . . ? O406 Mn4 O134 91.7(10) . . ? O405 Mn4 O124 170.5(13) . . ? O234 Mn4 O124 82.2(6) . . ? O406 Mn4 O124 91.7(6) . . ? O134 Mn4 O124 82.9(8) . . ? O405 Mn4 O112 92.9(9) . . ? O234 Mn4 O112 91.4(11) . . ? O406 Mn4 O112 93.9(9) . . ? O134 Mn4 O112 174.4(9) . . ? O124 Mn4 O112 96.0(8) . . ? O405 Mn4 Mn5 44.4(6) . . ? O234 Mn4 Mn5 145.5(4) . . ? O406 Mn4 Mn5 40.1(3) . . ? O134 Mn4 Mn5 94.5(6) . . ? O124 Mn4 Mn5 131.8(6) . . ? O112 Mn4 Mn5 90.3(6) . . ? O405 Mn4 Mn3 90.5(4) . . ? O234 Mn4 Mn3 40.8(8) . . ? O406 Mn4 Mn3 134.5(8) . . ? O134 Mn4 Mn3 42.9(6) . . ? O124 Mn4 Mn3 86.2(3) . . ? O112 Mn4 Mn3 131.6(7) . . ? Mn5 Mn4 Mn3 123.3(2) . . ? O405 Mn4 Mn1 130.0(9) . . ? O234 Mn4 Mn1 85.4(6) . . ? O406 Mn4 Mn1 86.9(5) . . ? O134 Mn4 Mn1 42.5(4) . . ? O124 Mn4 Mn1 40.9(7) . . ? O112 Mn4 Mn1 136.8(4) . . ? Mn5 Mn4 Mn1 115.6(3) . . ? Mn3 Mn4 Mn1 62.64(13) . . ? O405 Mn4 Mn2 141.7(6) . . ? O234 Mn4 Mn2 40.8(4) . . ? O406 Mn4 Mn2 133.4(3) . . ? O134 Mn4 Mn2 84.0(6) . . ? O124 Mn4 Mn2 41.7(6) . . ? O112 Mn4 Mn2 91.5(6) . . ? Mn5 Mn4 Mn2 173.5(2) . . ? Mn3 Mn4 Mn2 59.29(13) . . ? Mn1 Mn4 Mn2 59.33(17) . . ? O406 Mn5 O211 178.7(5) . . ? O406 Mn5 O405 82.8(6) . . ? O211 Mn5 O405 96.2(7) . . ? O406 Mn5 O110 94.2(5) . . ? O211 Mn5 O110 87.0(6) . . ? O405 Mn5 O110 167.8(13) . . ? O406 Mn5 O19 93.5(9) . . ? O211 Mn5 O19 85.9(11) . . ? O405 Mn5 O19 101.4(9) . . ? O110 Mn5 O19 90.6(11) . . ? O406 Mn5 O212 88.3(10) . . ? O211 Mn5 O212 92.3(12) . . ? O405 Mn5 O212 74.4(9) . . ? O110 Mn5 O212 93.7(11) . . ? O19 Mn5 O212 175.2(6) . . ? O406 Mn5 Mn4 41.7(6) . . ? O211 Mn5 Mn4 137.3(7) . . ? O405 Mn5 Mn4 41.4(4) . . ? O110 Mn5 Mn4 133.3(5) . . ? O19 Mn5 Mn4 104.1(4) . . ? O212 Mn5 Mn4 74.4(5) . . ? O406 Mn6 O107 94.6(6) . . ? O406 Mn6 O18 173.9(6) . . ? O107 Mn6 O18 91.2(7) . . ? O406 Mn6 O210 87.4(7) . . ? O107 Mn6 O210 173.7(9) . . ? O18 Mn6 O210 86.7(7) . . ? O406 Mn6 O29 91.2(8) . . ? O107 Mn6 O29 97.8(9) . . ? O18 Mn6 O29 89.7(9) . . ? O210 Mn6 O29 88.1(9) . . ? O406 Mn6 O6 84.3(9) . . ? O107 Mn6 O6 92.4(9) . . ? O18 Mn6 O6 93.8(8) . . ? O210 Mn6 O6 81.9(9) . . ? O29 Mn6 O6 169.2(6) . . ? O108 Mn7 O28 174.4(9) . . ? O108 Mn7 O107 82.7(7) . . ? O28 Mn7 O107 94.0(7) . . ? O108 Mn7 O15 97.2(7) . . ? O28 Mn7 O15 85.2(8) . . ? O107 Mn7 O15 169.2(10) . . ? O108 Mn7 O16 98.2(9) . . ? O28 Mn7 O16 86.9(9) . . ? O107 Mn7 O16 101.7(8) . . ? O15 Mn7 O16 89.0(7) . . ? O108 Mn7 O27 83.4(7) . . ? O28 Mn7 O27 91.9(9) . . ? O107 Mn7 O27 87.3(7) . . ? O15 Mn7 O27 82.0(7) . . ? O16 Mn7 O27 171.0(5) . . ? O108 Mn7 Mn1 40.9(3) . . ? O28 Mn7 Mn1 135.0(4) . . ? O107 Mn7 Mn1 42.5(5) . . ? O15 Mn7 Mn1 135.0(5) . . ? O16 Mn7 Mn1 109.0(6) . . ? O27 Mn7 Mn1 78.1(4) . . ? O208 Mn8 O108 98.1(8) . . ? O208 Mn8 O13 86.1(10) . . ? O108 Mn8 O13 175.4(8) . . ? O208 Mn8 O26 95.1(9) . . ? O108 Mn8 O26 96.1(7) . . ? O13 Mn8 O26 81.5(9) . . ? O208 Mn8 O25 174.3(10) . . ? O108 Mn8 O25 87.6(9) . . ? O13 Mn8 O25 88.2(9) . . ? O26 Mn8 O25 83.3(9) . . ? O208 Mn8 O14 95.1(6) . . ? O108 Mn8 O14 90.6(8) . . ? O13 Mn8 O14 91.0(9) . . ? O26 Mn8 O14 166.9(7) . . ? O25 Mn8 O14 85.7(8) . . ? O208 Mn9 O209 81.2(7) . . ? O208 Mn9 O114 174.8(7) . . ? O209 Mn9 O114 95.7(7) . . ? O208 Mn9 O23 99.4(7) . . ? O209 Mn9 O23 172.7(11) . . ? O114 Mn9 O23 83.2(7) . . ? O208 Mn9 O24 94.3(9) . . ? O209 Mn9 O24 93.3(8) . . ? O114 Mn9 O24 89.9(7) . . ? O23 Mn9 O24 93.9(8) . . ? O208 Mn9 O215 83.2(8) . . ? O209 Mn9 O215 88.8(7) . . ? O114 Mn9 O215 92.7(8) . . ? O23 Mn9 O215 84.0(7) . . ? O24 Mn9 O215 176.5(6) . . ? O208 Mn9 Mn2 41.2(3) . . ? O209 Mn9 Mn2 40.8(5) . . ? O114 Mn9 Mn2 135.0(4) . . ? O23 Mn9 Mn2 138.2(5) . . ? O24 Mn9 Mn2 101.2(5) . . ? O215 Mn9 Mn2 78.6(5) . . ? O209 Mn10 O310 92.4(9) . . ? O209 Mn10 O214 90.2(8) . . ? O310 Mn10 O214 177.1(5) . . ? O209 Mn10 O117 171.6(5) . . ? O310 Mn10 O117 90.8(7) . . ? O214 Mn10 O117 86.4(7) . . ? O209 Mn10 O116 97.5(7) . . ? O310 Mn10 O116 94.1(8) . . ? O214 Mn10 O116 86.7(9) . . ? O117 Mn10 O116 90.1(7) . . ? O209 Mn10 O10 90.9(7) . . ? O310 Mn10 O10 87.4(9) . . ? O214 Mn10 O10 91.5(8) . . ? O117 Mn10 O10 81.4(7) . . ? O116 Mn10 O10 171.4(6) . . ? O311 Mn11 O217 178.0(11) . . ? O311 Mn11 O310 83.8(6) . . ? O217 Mn11 O310 95.7(6) . . ? O311 Mn11 O213 94.0(6) . . ? O217 Mn11 O213 86.4(5) . . ? O310 Mn11 O213 175.5(12) . . ? O311 Mn11 O218 86.0(9) . . ? O217 Mn11 O218 92.0(9) . . ? O310 Mn11 O218 83.2(9) . . ? O213 Mn11 O218 92.8(8) . . ? O311 Mn11 O216 88.2(9) . . ? O217 Mn11 O216 93.8(9) . . ? O310 Mn11 O216 94.3(9) . . ? O213 Mn11 O216 89.5(8) . . ? O218 Mn11 O216 173.9(7) . . ? O311 Mn11 Mn3 42.0(3) . . ? O217 Mn11 Mn3 137.2(4) . . ? O310 Mn11 Mn3 42.4(6) . . ? O213 Mn11 Mn3 134.8(6) . . ? O218 Mn11 Mn3 77.2(4) . . ? O216 Mn11 Mn3 97.1(5) . . ? O311 Mn12 O405 92.0(6) . . ? O311 Mn12 O113 90.3(5) . . ? O405 Mn12 O113 172.6(11) . . ? O311 Mn12 O111 174.2(5) . . ? O405 Mn12 O111 93.6(6) . . ? O113 Mn12 O111 84.0(5) . . ? O311 Mn12 O121 89.9(10) . . ? O405 Mn12 O121 91.4(10) . . ? O113 Mn12 O121 95.6(9) . . ? O111 Mn12 O121 91.2(11) . . ? O311 Mn12 O120 89.7(11) . . ? O405 Mn12 O120 83.4(10) . . ? O113 Mn12 O120 89.7(9) . . ? O111 Mn12 O120 89.7(11) . . ? O121 Mn12 O120 174.7(6) . . ? Mn1 O107 Mn7 94.8(6) . . ? Mn1 O107 Mn6 128.9(12) . . ? Mn7 O107 Mn6 125.1(6) . . ? Mn7 O108 Mn1 98.4(7) . . ? Mn7 O108 Mn8 122.6(5) . . ? Mn1 O108 Mn8 128.0(13) . . ? Mn2 O123 Mn3 97.8(9) . . ? Mn2 O123 Mn1 94.8(5) . . ? Mn3 O123 Mn1 97.6(8) . . ? Mn1 O124 Mn4 96.4(9) . . ? Mn1 O124 Mn2 96.2(5) . . ? Mn4 O124 Mn2 97.4(7) . . ? Mn4 O134 Mn1 95.4(9) . . ? Mn4 O134 Mn3 94.7(13) . . ? Mn1 O134 Mn3 99.5(7) . . ? Mn2 O208 Mn9 96.6(7) . . ? Mn2 O208 Mn8 130.2(15) . . ? Mn9 O208 Mn8 122.9(6) . . ? Mn2 O209 Mn10 134.1(10) . . ? Mn2 O209 Mn9 95.3(6) . . ? Mn10 O209 Mn9 129.2(8) . . ? Mn3 O234 Mn4 98.3(15) . . ? Mn3 O234 Mn2 96.8(8) . . ? Mn4 O234 Mn2 100.4(7) . . ? Mn3 O310 Mn10 134.5(7) . . ? Mn3 O310 Mn11 93.6(8) . . ? Mn10 O310 Mn11 121.2(13) . . ? Mn12 O311 Mn3 132.5(9) . . ? Mn12 O311 Mn11 131.5(8) . . ? Mn3 O311 Mn11 95.7(6) . . ? Mn4 O405 Mn12 131.4(6) . . ? Mn4 O405 Mn5 94.2(6) . . ? Mn12 O405 Mn5 124.2(13) . . ? Mn5 O406 Mn4 98.1(7) . . ? Mn5 O406 Mn6 125.5(13) . . ? Mn4 O406 Mn6 133.2(6) . . ? C13 O13 Mn8 141.6(15) . . ? C13 O23 Mn9 125.1(14) . . ? O23 C13 O13 124.9(14) . . ? O23 C13 C231 116(4) . . ? O13 C13 C231 111(4) . . ? O23 C13 C23 118(2) . . ? O13 C13 C23 117(2) . . ? C231 C13 C23 25(4) . . ? C33 C23 C13 116.3(18) . . ? C43 C33 C23 109.5(11) . . ? C43 C33 C53 109.7(12) . . ? C23 C33 C53 109.5(11) . . ? C43 C33 C63 109.3(12) . . ? C23 C33 C63 109.9(12) . . ? C53 C33 C63 108.9(12) . . ? C13 C231 C331 107(4) . . ? C631 C331 C431 109.7(12) . . ? C631 C331 C231 109.6(12) . . ? C431 C331 C231 109.5(12) . . ? C631 C331 C531 109.6(12) . . ? C431 C331 C531 109.3(12) . . ? C231 C331 C531 109.1(12) . . ? C14 O14 Mn8 133.3(12) . . ? C14 O24 Mn9 131.4(9) . . ? O24 C14 O14 125.6(11) . . ? O24 C14 C24 117.6(10) . . ? O14 C14 C24 116.6(10) . . ? C14 C24 C34 117.7(10) . . ? C24 C34 C44 109.9(8) . . ? C24 C34 C64 109.2(9) . . ? C44 C34 C64 109.7(9) . . ? C24 C34 C54 110.3(9) . . ? C44 C34 C54 109.1(8) . . ? C64 C34 C54 108.6(8) . . ? C15 O15 Mn7 126.0(13) . . ? C15 O25 Mn8 138.8(13) . . ? O25 C15 O15 126.5(14) . . ? O25 C15 C251 100(2) . . ? O15 C15 C251 131(2) . . ? O25 C15 C25 130(3) . . ? O15 C15 C25 93.9(15) . . ? C251 C15 C25 60(2) . . ? C35 C25 C15 109(3) . . ? C55 C35 C25 109.9(12) . . ? C55 C35 C45 109.5(12) . . ? C25 C35 C45 109.3(12) . . ? C55 C35 C65 109.4(12) . . ? C25 C35 C65 109.3(12) . . ? C45 C35 C65 109.4(12) . . ? C15 C251 C351 109.9(16) . . ? C651 C351 C551 110.5(12) . . ? C651 C351 C451 110.4(13) . . ? C551 C351 C451 110.3(13) . . ? C651 C351 C251 108.8(12) . . ? C551 C351 C251 108.4(13) . . ? C451 C351 C251 108.3(12) . . ? C16 O16 Mn7 130.2(10) . . ? C16 O26 Mn8 135.3(14) . . ? O26 C16 O16 125.2(12) . . ? O26 C16 C26 117.2(11) . . ? O16 C16 C26 116.3(11) . . ? C16 C26 C361 125.7(14) . . ? C16 C26 C36 122.2(15) . . ? C361 C26 C36 38.0(8) . . ? C56 C36 C46 110.0(10) . . ? C56 C36 C26 109.8(8) . . ? C46 C36 C26 109.6(8) . . ? C56 C36 C66 109.4(11) . . ? C46 C36 C66 109.1(11) . . ? C26 C36 C66 108.9(8) . . ? C26 C361 C46 110.3(8) . . ? C26 C361 C56 109.8(8) . . ? C46 C361 C56 110.0(11) . . ? C26 C361 C661 109.4(8) . . ? C46 C361 C661 108.7(11) . . ? C56 C361 C661 108.5(11) . . ? C361 C46 C36 38.0(8) . . ? C36 C56 C361 38.0(8) . . ? C17 O17 Mn1 127.1(8) . . ? C17 O27 Mn7 123.3(12) . . ? O27 C17 O17 124.7(11) . . ? O27 C17 C27 119.3(11) . . ? O17 C17 C27 116.0(9) . . ? C17 C27 C37 115.8(9) . . ? C27 C37 C67 109.2(9) . . ? C27 C37 C57 111.7(9) . . ? C67 C37 C57 108.9(9) . . ? C27 C37 C47 108.9(9) . . ? C67 C37 C47 109.3(8) . . ? C57 C37 C47 108.9(8) . . ? C18 O18 Mn6 130.5(12) . . ? C18 O28 Mn7 128.7(12) . . ? O28 C18 O18 124.9(13) . . ? O28 C18 C28 116.3(11) . . ? O18 C18 C28 116.7(10) . . ? C18 C28 C38 114.5(10) . . ? C28 C38 C58 112.1(11) . . ? C28 C38 C48 109.0(10) . . ? C58 C38 C48 108.8(9) . . ? C28 C38 C68 108.3(10) . . ? C58 C38 C68 109.7(9) . . ? C48 C38 C68 108.9(9) . . ? C19 O19 Mn5 120.1(10) . . ? C19 O29 Mn6 135.3(14) . . ? O29 C19 O19 125.2(12) . . ? O29 C19 C29 117.4(11) . . ? O19 C19 C29 117.2(11) . . ? C19 C29 C39 116.1(11) . . ? C29 C39 C69 108.8(10) . . ? C29 C39 C59 111.6(10) . . ? C69 C39 C59 109.3(9) . . ? C29 C39 C49 109.0(10) . . ? C69 C39 C49 109.2(9) . . ? C59 C39 C49 108.9(9) . . ? C110 O110 Mn5 127.6(15) . . ? C110 O210 Mn6 129.2(11) . . ? O210 C110 O110 125.7(12) . . ? O210 C110 C210 116.2(11) . . ? O110 C110 C210 116.3(11) . . ? C110 C210 C310 133(3) . . ? C110 C210 C320 129(3) . . ? C310 C210 C320 95(2) . . ? C210 C310 C610 109.5(7) . . ? C210 C310 C410 109.5(8) . . ? C610 C310 C410 109.5(7) . . ? C210 C310 C510 109.4(7) . . ? C610 C310 C510 109.5(8) . . ? C410 C310 C510 109.5(7) . . ? C420 C320 C210 109.6(7) . . ? C420 C320 C720 126(5) . . ? C210 C320 C720 109.5(7) . . ? C420 C320 C920 20(8) . . ? C210 C320 C920 109.5(7) . . ? C720 C320 C920 109.5(7) . . ? C420 C320 C520 109.6(7) . . ? C210 C320 C520 109.5(7) . . ? C720 C320 C520 20(8) . . ? C920 C320 C520 91(7) . . ? C420 C320 C820 91(7) . . ? C210 C320 C820 109.4(7) . . ? C720 C320 C820 109.5(7) . . ? C920 C320 C820 109.4(7) . . ? C520 C320 C820 126(6) . . ? C420 C320 C620 109.4(7) . . ? C210 C320 C620 109.4(7) . . ? C720 C320 C620 91(7) . . ? C920 C320 C620 126(6) . . ? C520 C320 C620 109.4(7) . . ? C820 C320 C620 20(8) . . ? C111 O111 Mn12 137.3(10) . . ? C111 O211 Mn5 132.9(11) . . ? O111 C111 O211 124.8(12) . . ? O111 C111 C211 117.2(10) . . ? O211 C111 C211 116.6(10) . . ? C111 C211 C311 116.4(11) . . ? C211 C311 C511 111.8(10) . . ? C211 C311 C611 109.1(10) . . ? C511 C311 C611 109.0(9) . . ? C211 C311 C411 109.1(10) . . ? C511 C311 C411 108.8(8) . . ? C611 C311 C411 108.9(9) . . ? C112 O112 Mn4 121.7(14) . . ? C112 O212 Mn5 123.4(12) . . ? O212 C112 O112 125.7(12) . . ? O212 C112 C212 117.5(11) . . ? O112 C112 C212 116.0(11) . . ? C112 C212 C312 115.2(11) . . ? C212 C312 C412 110.0(8) . . ? C212 C312 C422 109.8(8) . . ? C412 C312 C422 130(4) . . ? C212 C312 C612 109.7(8) . . ? C412 C312 C612 109.5(8) . . ? C422 C312 C612 27(6) . . ? C212 C312 C622 109.6(7) . . ? C412 C312 C622 27(6) . . ? C422 C312 C622 109.4(8) . . ? C612 C312 C622 85(6) . . ? C212 C312 C522 109.5(7) . . ? C412 C312 C522 84(6) . . ? C422 C312 C522 109.3(7) . . ? C612 C312 C522 130(4) . . ? C622 C312 C522 109.2(8) . . ? C212 C312 C512 109.3(8) . . ? C412 C312 C512 109.2(8) . . ? C422 C312 C512 85(6) . . ? C612 C312 C512 109.0(8) . . ? C622 C312 C512 130(4) . . ? C522 C312 C512 27(6) . . ? C113 O113 Mn12 132.6(13) . . ? C113 O213 Mn11 130.7(11) . . ? O213 C113 O113 126.0(11) . . ? O213 C113 C213 117.5(11) . . ? O113 C113 C213 116.3(10) . . ? C313 C213 C113 116.8(10) . . ? C213 C313 C413 109.9(10) . . ? C213 C313 C513 112.0(10) . . ? C413 C313 C513 108.8(9) . . ? C213 C313 C613 108.6(10) . . ? C413 C313 C613 108.5(9) . . ? C513 C313 C613 108.9(9) . . ? C114 O114 Mn9 130.4(10) . . ? C114 O214 Mn10 137.5(12) . . ? O214 C114 O114 126.3(11) . . ? O214 C114 C214 117.0(10) . . ? O114 C114 C214 116.7(10) . . ? C114 C214 C314 116.1(10) . . ? C214 C314 C514 110.4(9) . . ? C214 C314 C614 109.5(9) . . ? C514 C314 C614 109.0(8) . . ? C214 C314 C414 109.7(9) . . ? C514 C314 C414 109.4(8) . . ? C614 C314 C414 108.8(8) . . ? C115 O115 Mn2 126.6(9) . . ? C115 O215 Mn9 119.8(13) . . ? O215 C115 O115 126.6(11) . . ? O215 C115 C215 117.7(11) . . ? O115 C115 C215 115.4(10) . . ? C115 C215 C315 116.1(10) . . ? C215 C315 C415 109.6(9) . . ? C215 C315 C615 109.2(10) . . ? C415 C315 C615 109.3(9) . . ? C215 C315 C515 110.8(10) . . ? C415 C315 C515 109.3(9) . . ? C615 C315 C515 108.6(9) . . ? C116 O116 Mn10 130(2) . . ? C116 O216 Mn11 123.0(12) . . ? O216 C116 O116 124.7(12) . . ? O216 C116 C216 118.0(11) . . ? O116 C116 C216 116.4(11) . . ? C116 C216 C316 115.1(11) . . ? C216 C316 C416 109.2(10) . . ? C216 C316 C516 111.3(10) . . ? C416 C316 C516 109.2(9) . . ? C216 C316 C616 108.2(10) . . ? C416 C316 C616 109.6(9) . . ? C516 C316 C616 109.3(9) . . ? C117 O117 Mn10 132.9(9) . . ? C117 O217 Mn11 131.9(10) . . ? O217 C117 O117 125.5(10) . . ? O217 C117 C217 116.7(10) . . ? O117 C117 C217 117.7(10) . . ? C117 C217 C317 116.8(11) . . ? C217 C317 C617 109.6(10) . . ? C217 C317 C517 111.2(10) . . ? C617 C317 C517 108.6(9) . . ? C217 C317 C417 109.4(10) . . ? C617 C317 C417 108.7(9) . . ? C517 C317 C417 109.2(9) . . ? C118 O118 Mn3 124.3(16) . . ? C118 O218 Mn11 125.7(12) . . ? O218 C118 O118 124.8(14) . . ? O218 C118 C228 108(2) . . ? O118 C118 C228 127(2) . . ? O218 C118 C218 126.0(19) . . ? O118 C118 C218 109(2) . . ? C228 C118 C218 19(2) . . ? C318 C218 C118 109(3) . . ? C618 C318 C218 110.5(12) . . ? C618 C318 C418 109.5(12) . . ? C218 C318 C418 109.9(12) . . ? C618 C318 C518 109.9(12) . . ? C218 C318 C518 108.3(12) . . ? C418 C318 C518 108.7(12) . . ? C328 C228 C118 112(3) . . ? C228 C328 C528 109.8(12) . . ? C228 C328 C428 109.9(12) . . ? C528 C328 C428 109.4(12) . . ? C228 C328 C628 109.9(12) . . ? C528 C328 C628 109.2(12) . . ? C428 C328 C628 108.7(12) . . ? O3A N1A O2A 124.7(15) . . ? O3A N1A C1A 117.8(14) . . ? O2A N1A C1A 117.4(14) . . ? Cl1B C1B Cl2B 111.0(12) . . ? _diffrn_measured_fraction_theta_max 0.282 _diffrn_reflns_theta_full 15.46 _diffrn_measured_fraction_theta_full 0.282 _refine_diff_density_max 0.552 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.078 data_mnjt04 #TrackingRef 'all_revised.cif' _database_code_depnum_ccdc_archive 'CCDC 755028' #2.5 GPa structure #see refine special details for checkcif comments _audit_creation_method SHELXL-97 _chemical_compound_source 'Mark Murrie & Pascal Parois, Glasgow University' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn12O12(tBuCH2CO2)16(H2O)4]' _chemical_formula_sum 'C96 H184 Mn12 N0 O48' _chemical_formula_weight 2765.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0005 0.0007 '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 0.0015 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0034 0.0025 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.2230 0.3472 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.0148(19) _cell_length_b 15.1418(19) _cell_length_c 26.7583(19) _cell_angle_alpha 76.184(9) _cell_angle_beta 76.208(8) _cell_angle_gamma 79.415(8) _cell_volume 5685.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2423 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 13.4 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6459 _exptl_absorpt_correction_T_max 0.7437 _exptl_absorpt_process_details Sadabs _exptl_special_details ; Station 9.8 at Daresbury SRS ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.47800 _diffrn_radiation_type Xray _diffrn_radiation_source synchtrotron _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'Bruker Apex-II' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12135 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.1270 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 13.54 _reflns_number_total 3426 _reflns_number_gt 2067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex' _computing_cell_refinement 'Bruker Saint' _computing_data_reduction 'Bruker Saint' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Data were collected on Station 9.8 at the Daresbury SRS. The crystal was held in a Merrill-Bassett diamond anvil cell constructed using conically-ground WC backing disks and Boehler-Almax culet-cut diamonds. The body of the pressure cell restricts the volume of reciprocal space which can be sampled during data collection and, taken with the low crystal symmetry (triclinic) the completeness is low. Coverage statistics are: Theta sin(th)/Lambda Complete Expected Measured Missing #-------------------------------------------------------------- 13.54 0.490 0.314 10952 3438 7514 Data were integrated to 1 Ang resolution - beyond this the data became very weak and indistinguishable from noise. The 1.5 GPa structure was used as the starting model. In view of the low completeness only the Mn atoms were modelled with anisotropic displacement patameters. All other atoms were modelled isotropically. tBuCH2COO- ligands carrying the labels 3,5,6,10,12 and 18 are disordered with the tBu groups distributed over two positions. The C-C distances and C-C-C angles involving part-weight atoms were restrained to 1.50(1) Ang and 109.5 deg, respectively. Fully occupied ligands were restrained to be geometrically similar. Within disordered ligands isotropic displacement parameters for chemically equivalent carbon atoms were constrined to be equal. H-atoms were placed in calculated positions; in some cases methyl groups were modelled as being rotationally disordered in order to avoid close contacts with other part-weight H-atoms. H-atoms were not placed on the ligand water molecules (atoms O6, O10, O120 and O121). In the final cycles of refinement robust-resistant weighting scheme was used as described by Prince (Acta A39, 407-410, 1983). This is amongst the largest structures to have been investigated using high-pressure methods at atomic resolution. The low completeness, weak diffraction and disorder made modelling the diffraction data challenging, and there are numerous checkcif alerts: 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.31 023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6].. 13.54 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.31 088_ALERT_3_A Poor Data / Parameter Ratio .................... 4.59 201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 133 341_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 36 601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 175.00 A**3 911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.490 7516 082_ALERT_2_C High R1 Value .................................. 0.11 084_ALERT_2_C High R2 Value .................................. 0.29 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 10 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 16 See comments above about low completeness and resolution. The high R-value is to be expected for a structure suffering from high libration (particularly in the tBu groups), but for which only isotropic modelling of displacement is possible. The data:parameter ratio is 4.43; for a fully anisotropic model it would be ca 2. 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 10.00 Ratio 220_ALERT_2_A Large Non-Solvent O Ueq(max)/Ueq(min) ... 4.82 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 8.52 Ratio 250_ALERT_2_B Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.09 +Numerous alerts of the type: 241_ALERT_2_A Check High Ueq as Compared to Neighbors for O26 241_ALERT_2_A Check High Ueq as Compared to Neighbors for C210 241_ALERT_2_B Check High Ueq as Compared to Neighbors for O13 241_ALERT_2_B Check High Ueq as Compared to Neighbors for C26 241_ALERT_2_B Check High Ueq as Compared to Neighbors for C46 241_ALERT_2_B Check High Ueq as Compared to Neighbors for C56 [More C-Alerts - not included] 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C33 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C110 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C310 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C316 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C320 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C331 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for O108 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C13 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C14 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C16 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C36 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C38 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C117 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C311 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C312 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C317 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C318 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C328 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C361 [More C-Alerts - not included] Disorder modelling was carried out for ligands in which U[iso] for one or more atoms refined to values larger than ca 0.3 Ang**2. Thermal motion still appears to be high elsewhere in the structure, though this is not unexpected for tBuCH2COO- at room temperature. 413_ALERT_2_A Short Inter XH3 .. XHn H42E .. H61V .. 1.86 Ang. 413_ALERT_2_A Short Inter XH3 .. XHn H51M .. H65B .. 1.89 Ang. 413_ALERT_2_A Short Inter XH3 .. XHn H51W .. H25B .. 1.78 Ang. 413_ALERT_2_A Short Inter XH3 .. XHn H61V .. H61K .. 1.82 Ang. 413_ALERT_2_A Short Inter XH3 .. XHn H412 .. H45A .. 1.64 Ang. 432_ALERT_2_A Short Inter X...Y Contact C56 .. C510 .. 2.60 Ang. 432_ALERT_2_A Short Inter X...Y Contact C411 .. C510 .. 2.85 Ang. 432_ALERT_2_A Short Inter X...Y Contact C411 .. C610 .. 2.89 Ang. 432_ALERT_2_A Short Inter X...Y Contact C511 .. C610 .. 2.64 Ang. 411_ALERT_2_B Short Inter H...H Contact H27B .. H52G .. 1.91 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H21K .. H55C .. 1.96 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H21M .. H42F .. 2.03 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H41M .. H63E .. 2.00 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H41W .. H58A .. 1.99 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H42F .. H51T .. 2.07 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H48C .. H42A .. 1.91 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H48C .. H82A .. 1.91 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H49A .. H52H .. 2.06 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H51S .. H68A .. 2.02 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H51X .. H68B .. 2.09 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H59C .. H63F .. 2.04 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H61N .. H513 .. 1.93 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H61O .. H513 .. 2.06 Ang. 432_ALERT_2_B Short Inter X...Y Contact C311 .. C610 .. 3.07 Ang. 432_ALERT_2_B Short Inter X...Y Contact C415 .. C520 .. 3.09 Ang. 432_ALERT_2_B Short Inter X...Y Contact C518 .. C613 .. 3.07 Ang. 432_ALERT_2_B Short Inter X...Y Contact C616 .. C612 .. 3.06 Ang. 411_ALERT_2_C Short Inter H...H Contact H23B .. H29A .. 2.01 Ang. 413_ALERT_2_C Short Inter XH3 .. XHn H43B .. H48C .. 2.13 Ang. 413_ALERT_2_C Short Inter XH3 .. XHn H43C .. H48C .. 2.11 Ang. 413_ALERT_2_C Short Inter XH3 .. XHn H51Z .. H414 .. 2.11 Ang. 413_ALERT_2_C Short Inter XH3 .. XHn H61M .. H43D .. 2.12 Ang. 432_ALERT_2_C Short Inter X...Y Contact C46 .. C510 .. 3.10 Ang. 432_ALERT_2_C Short Inter X...Y Contact C410 .. C611 .. 3.13 Ang. Short H....H contacts are to be expected at high pressure. We have shown that 1.7 Ang is an approximate lower limit for H...H contacts at pressures up to 10 GPa. The shortest contacts in the table above all involve part-weight atoms. 213_ALERT_2_C Atom Mn8 has ADP max/min Ratio ............. 3.60 prola All the Mn adps are oriented in the same direction. This is because the data set is truncated in one direction by the body of the pressure cell. 245_ALERT_2_C U(iso) H22A Smaller than U(eq) C518 by ... 0.04 AngSq Don't understand this one. H22A is not connected to C518. 083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large. 135.44 Mostly likely due to the limitations of the model. 301_ALERT_3_G Note Main Residue Disorder .................... 13.00 Perc. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1839 See above 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? No action 731_ALERT_1_B Bond Calc 1.53(4), Rep 1.529(9) ...... 4.44 su-Ra C34 -C64 1.555 1.555 731_ALERT_1_B Bond Calc 1.52(4), Rep 1.528(9) ...... 4.44 su-Ra C37 -C67 1.555 1.555 731_ALERT_1_B Bond Calc 1.54(4), Rep 1.531(9) ...... 4.44 su-Ra C37 -C57 1.555 1.555 731_ALERT_1_B Bond Calc 1.53(4), Rep 1.528(9) ...... 4.44 su-Ra C38 -C48 1.555 1.555 731_ALERT_1_B Bond Calc 1.53(4), Rep 1.530(9) ...... 4.44 su-Ra C38 -C68 1.555 1.555 731_ALERT_1_B Bond Calc 1.53(4), Rep 1.531(9) ...... 4.44 su-Ra C38 -C58 1.555 1.555 ...+ Numerous similar The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif can be badly in error. 041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? 042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ? H's on ligand waters no placed. 125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? -P1 926_ALERT_1_C Reported and Calculated R1 * 100.0 Differ by . -0.19 927_ALERT_1_C Reported and Calculated wR2 * 100.0 Differ by . -0.22 Rounding error?? 092_ALERT_4_G Check: Wavelength given is not Cu,Mo or Ag Ka .. 0.48 Ang. Synchrotron data 153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) 190 Ang. 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 25.00 Deg. C231 -C13 -C23 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 38.70 Deg. C36 -C26 -C361 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 38.70 Deg. C361 -C46 -C36 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 38.70 Deg. C36 -C56 -C361 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 0.00 Deg. C720 -C320 -C620 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 0.00 Deg. C520 -C320 -C920 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 0.00 Deg. C420 -C320 -C820 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 19.00 Deg. C612 -C312 -C422 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 19.00 Deg. C622 -C312 -C412 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 19.00 Deg. C512 -C312 -C522 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 14.00 Deg. C228 -C118 -C218 1.555 1.555 1.555 795_ALERT_4_G C-Atom in CIF Coordinate List out of Sequence .. C14 796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence .. O107 811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms .... ! No action taken. ; _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^)+(0.1111P)^2^+135.4381P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3426 _refine_ls_number_parameters 746 _refine_ls_number_restraints 1839 _refine_ls_R_factor_all 0.1736 _refine_ls_R_factor_gt 0.1102 _refine_ls_wR_factor_ref 0.2860 _refine_ls_wR_factor_gt 0.2441 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 0.813 _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 0.4173(5) 0.6863(5) 0.7331(2) 0.058(6) Uani 1 1 d . . . Mn2 Mn 0.2872(5) 0.5616(5) 0.7614(2) 0.043(6) Uani 1 1 d . . . Mn3 Mn 0.2533(5) 0.7213(5) 0.6866(2) 0.041(6) Uani 1 1 d . . . Mn4 Mn 0.2396(5) 0.7388(5) 0.7902(2) 0.061(6) Uani 1 1 d . . . Mn5 Mn 0.2118(6) 0.9077(6) 0.8228(2) 0.079(7) Uani 1 1 d . . . Mn6 Mn 0.4186(5) 0.7930(5) 0.8325(2) 0.083(6) Uani 1 1 d . . . Mn7 Mn 0.5824(5) 0.6503(5) 0.7681(2) 0.072(6) Uani 1 1 d . . . Mn8 Mn 0.5084(5) 0.4610(5) 0.7630(2) 0.078(6) Uani 1 1 d . . . Mn9 Mn 0.3274(5) 0.3855(5) 0.7410(2) 0.082(6) Uani 1 1 d . . . Mn10 Mn 0.1714(5) 0.5318(5) 0.6732(2) 0.064(6) Uani 1 1 d . . . Mn11 Mn 0.0914(5) 0.7541(5) 0.6499(2) 0.077(6) Uani 1 1 d . . . Mn12 Mn 0.1061(6) 0.9070(6) 0.7215(3) 0.073(7) Uani 1 1 d . . . O6 O 0.380(2) 0.649(2) 0.8886(9) 0.057(5) Uiso 1 1 d . . . O10 O 0.292(2) 0.505(2) 0.6113(9) 0.059(6) Uiso 1 1 d . . . O120 O -0.017(3) 0.835(3) 0.7713(12) 0.089(8) Uiso 1 1 d . . . O121 O 0.230(2) 0.967(2) 0.6823(10) 0.058(6) Uiso 1 1 d . . . O107 O 0.4728(18) 0.7414(19) 0.7729(8) 0.043(5) Uiso 1 1 d . . . O108 O 0.5113(18) 0.5885(18) 0.7418(8) 0.035(4) Uiso 1 1 d . . . O123 O 0.3503(19) 0.628(2) 0.6997(8) 0.038(5) Uiso 1 1 d . . . O124 O 0.3372(18) 0.6357(19) 0.7932(8) 0.034(4) Uiso 1 1 d . . . O134 O 0.310(2) 0.773(2) 0.7240(9) 0.050(5) Uiso 1 1 d . . . O208 O 0.3795(19) 0.4629(19) 0.7680(8) 0.043(5) Uiso 1 1 d . . . O209 O 0.2464(18) 0.4977(18) 0.7241(8) 0.039(5) Uiso 1 1 d . . . O234 O 0.2024(18) 0.6750(18) 0.7514(8) 0.028(4) Uiso 1 1 d . . . O310 O 0.1866(19) 0.649(2) 0.6592(8) 0.037(4) Uiso 1 1 d . . . O311 O 0.148(2) 0.808(2) 0.6866(9) 0.052(5) Uiso 1 1 d . . . O405 O 0.1636(19) 0.850(2) 0.7798(9) 0.049(5) Uiso 1 1 d . . . O406 O 0.2983(19) 0.809(2) 0.8228(9) 0.045(5) Uiso 1 1 d . . . O13 O 0.510(2) 0.335(2) 0.7929(11) 0.104(9) Uiso 1 1 d D A . O23 O 0.4084(18) 0.2768(19) 0.7656(9) 0.065(6) Uiso 1 1 d D A . C13 C 0.4784(19) 0.2670(18) 0.7836(12) 0.055(9) Uiso 1 1 d D . . C23 C 0.515(4) 0.168(2) 0.8026(17) 0.103(14) Uiso 0.75 1 d PD A 1 H23A H 0.4624 0.1354 0.8197 0.123 Uiso 0.75 1 calc PR A 1 H23B H 0.5469 0.1426 0.7723 0.123 Uiso 0.75 1 calc PR A 1 C33 C 0.579(3) 0.152(3) 0.8400(14) 0.103(14) Uiso 0.75 1 d PD A 1 C43 C 0.612(6) 0.051(3) 0.854(2) 0.180(18) Uiso 0.75 1 d PD A 1 H43A H 0.6593 0.0334 0.8253 0.269 Uiso 0.75 1 calc PR A 1 H43B H 0.5608 0.0169 0.8592 0.269 Uiso 0.75 1 calc PR A 1 H43C H 0.6360 0.0375 0.8851 0.269 Uiso 0.75 1 calc PR A 1 C53 C 0.527(4) 0.185(5) 0.8889(17) 0.180(18) Uiso 0.75 1 d PD A 1 H53A H 0.5637 0.1646 0.9156 0.269 Uiso 0.75 1 calc PR A 1 H53B H 0.4695 0.1608 0.9011 0.269 Uiso 0.75 1 calc PR A 1 H53C H 0.5162 0.2508 0.8812 0.269 Uiso 0.75 1 calc PR A 1 C63 C 0.661(4) 0.202(5) 0.815(2) 0.180(18) Uiso 0.75 1 d PD A 1 H63A H 0.6971 0.1768 0.7863 0.269 Uiso 0.75 1 calc PR A 1 H63B H 0.6977 0.1967 0.8411 0.269 Uiso 0.75 1 calc PR A 1 H63C H 0.6395 0.2660 0.8034 0.269 Uiso 0.75 1 calc PR A 1 C231 C 0.506(8) 0.185(7) 0.824(4) 0.103(14) Uiso 0.25 1 d PD A 2 H23C H 0.4958 0.2013 0.8582 0.123 Uiso 0.25 1 calc PR A 2 H23D H 0.4715 0.1354 0.8271 0.123 Uiso 0.25 1 calc PR A 2 C331 C 0.607(8) 0.161(8) 0.802(4) 0.103(14) Uiso 0.25 1 d PD A 2 C431 C 0.628(11) 0.202(13) 0.745(4) 0.180(18) Uiso 0.25 1 d PD A 2 H43D H 0.6915 0.1814 0.7302 0.269 Uiso 0.25 1 calc PR A 2 H43E H 0.6196 0.2680 0.7396 0.269 Uiso 0.25 1 calc PR A 2 H43F H 0.5880 0.1837 0.7274 0.269 Uiso 0.25 1 calc PR A 2 C531 C 0.663(11) 0.199(15) 0.830(8) 0.180(18) Uiso 0.25 1 d PD A 2 H53D H 0.6512 0.1704 0.8668 0.269 Uiso 0.25 1 calc PR A 2 H53E H 0.6454 0.2639 0.8262 0.269 Uiso 0.25 1 calc PR A 2 H53F H 0.7273 0.1857 0.8152 0.269 Uiso 0.25 1 calc PR A 2 C631 C 0.630(13) 0.059(8) 0.811(7) 0.180(18) Uiso 0.25 1 d PD A 2 H63D H 0.6067 0.0321 0.8467 0.269 Uiso 0.25 1 calc PR A 2 H63E H 0.6964 0.0430 0.8027 0.269 Uiso 0.25 1 calc PR A 2 H63F H 0.6031 0.0362 0.7881 0.269 Uiso 0.25 1 calc PR A 2 O14 O 0.5397(16) 0.442(2) 0.6850(8) 0.085(7) Uiso 1 1 d D . . O24 O 0.4134(15) 0.4102(15) 0.6674(7) 0.061(6) Uiso 1 1 d D . . C14 C 0.4922(16) 0.4301(17) 0.6527(6) 0.039(7) Uiso 1 1 d D . . C24 C 0.5326(17) 0.4533(13) 0.5965(6) 0.067(9) Uiso 1 1 d D . . H24A H 0.5834 0.4877 0.5922 0.080 Uiso 1 1 calc R . . H24B H 0.4861 0.4939 0.5791 0.080 Uiso 1 1 calc R . . C34 C 0.5676(15) 0.3762(14) 0.5687(6) 0.051(8) Uiso 1 1 d D . . C44 C 0.6357(19) 0.3063(18) 0.5972(9) 0.057(9) Uiso 1 1 d D . . H44A H 0.6551 0.2548 0.5802 0.085 Uiso 1 1 calc R . . H44B H 0.6061 0.2858 0.6331 0.085 Uiso 1 1 calc R . . H44C H 0.6887 0.3344 0.5961 0.085 Uiso 1 1 calc R . . C54 C 0.6172(18) 0.4092(19) 0.5119(7) 0.047(8) Uiso 1 1 d D . . H54A H 0.6391 0.3575 0.4952 0.071 Uiso 1 1 calc R . . H54B H 0.6688 0.4385 0.5119 0.071 Uiso 1 1 calc R . . H54C H 0.5750 0.4520 0.4931 0.071 Uiso 1 1 calc R . . C64 C 0.4860(18) 0.3294(17) 0.5679(10) 0.060(9) Uiso 1 1 d D . . H64A H 0.5087 0.2770 0.5520 0.091 Uiso 1 1 calc R . . H64B H 0.4451 0.3718 0.5480 0.091 Uiso 1 1 calc R . . H64C H 0.4532 0.3101 0.6032 0.091 Uiso 1 1 calc R . . O15 O 0.7017(17) 0.5753(18) 0.7478(8) 0.069(6) Uiso 1 1 d D B . O25 O 0.647(2) 0.4437(16) 0.7591(8) 0.067(7) Uiso 1 1 d D B . C15 C 0.7120(18) 0.4868(18) 0.7515(12) 0.066(11) Uiso 1 1 d D . . C25 C 0.808(3) 0.490(3) 0.718(3) 0.071(8) Uiso 0.25 1 d PD B 1 H25A H 0.8075 0.5461 0.6917 0.085 Uiso 0.25 1 calc PR B 1 H25B H 0.8493 0.4932 0.7405 0.085 Uiso 0.25 1 calc PR B 1 C35 C 0.845(4) 0.410(3) 0.692(2) 0.071(8) Uiso 0.25 1 d PD B 1 C45 C 0.835(7) 0.437(7) 0.636(2) 0.060(6) Uiso 0.25 1 d PD B 1 H45A H 0.8492 0.3836 0.6205 0.090 Uiso 0.25 1 calc PR B 1 H45B H 0.8757 0.4808 0.6164 0.090 Uiso 0.25 1 calc PR B 1 H45C H 0.7718 0.4639 0.6344 0.090 Uiso 0.25 1 calc PR B 1 C55 C 0.946(4) 0.383(7) 0.694(4) 0.060(6) Uiso 0.25 1 d PD B 1 H55A H 0.9569 0.3939 0.7256 0.090 Uiso 0.25 1 calc PR B 1 H55B H 0.9826 0.4196 0.6641 0.090 Uiso 0.25 1 calc PR B 1 H55C H 0.9634 0.3196 0.6925 0.090 Uiso 0.25 1 calc PR B 1 C65 C 0.794(8) 0.331(3) 0.720(4) 0.060(6) Uiso 0.25 1 d PD B 1 H65A H 0.8008 0.3139 0.7558 0.090 Uiso 0.25 1 calc PR B 1 H65B H 0.8188 0.2795 0.7030 0.090 Uiso 0.25 1 calc PR B 1 H65C H 0.7297 0.3475 0.7186 0.090 Uiso 0.25 1 calc PR B 1 C251 C 0.790(2) 0.409(3) 0.7530(10) 0.071(8) Uiso 0.75 1 d PD B 2 H25C H 0.7661 0.3519 0.7710 0.085 Uiso 0.75 1 calc PR B 2 H25D H 0.8335 0.4195 0.7719 0.085 Uiso 0.75 1 calc PR B 2 C351 C 0.838(2) 0.404(2) 0.6975(12) 0.071(8) Uiso 0.75 1 d PD B 2 C451 C 0.865(3) 0.495(3) 0.6690(13) 0.060(6) Uiso 0.75 1 d PD B 2 H45D H 0.9063 0.5125 0.6861 0.090 Uiso 0.75 1 calc PR B 2 H45E H 0.8104 0.5403 0.6691 0.090 Uiso 0.75 1 calc PR B 2 H45F H 0.8947 0.4925 0.6333 0.090 Uiso 0.75 1 calc PR B 2 C551 C 0.775(2) 0.373(3) 0.6708(14) 0.060(6) Uiso 0.75 1 d PD B 2 H55D H 0.7595 0.3137 0.6892 0.090 Uiso 0.75 1 calc PR B 2 H55E H 0.8054 0.3708 0.6352 0.090 Uiso 0.75 1 calc PR B 2 H55F H 0.7191 0.4164 0.6708 0.090 Uiso 0.75 1 calc PR B 2 C651 C 0.923(2) 0.334(3) 0.6983(14) 0.060(6) Uiso 0.75 1 d PD B 2 H65D H 0.9646 0.3527 0.7145 0.090 Uiso 0.75 1 calc PR B 2 H65E H 0.9526 0.3286 0.6629 0.090 Uiso 0.75 1 calc PR B 2 H65F H 0.9058 0.2753 0.7179 0.090 Uiso 0.75 1 calc PR B 2 O16 O 0.5690(16) 0.5742(18) 0.8451(7) 0.062(6) Uiso 1 1 d D . . O26 O 0.486(2) 0.466(2) 0.8461(11) 0.135(11) Uiso 1 1 d D . . C16 C 0.529(2) 0.501(2) 0.8675(8) 0.052(10) Uiso 1 1 d D D . C26 C 0.5343(19) 0.4630(18) 0.9228(8) 0.081(11) Uiso 1 1 d D . . H26A H 0.4862 0.4235 0.9359 0.098 Uiso 0.50 1 calc PR C 1 H26B H 0.5136 0.5147 0.9402 0.098 Uiso 0.50 1 calc PR C 1 H26C H 0.4714 0.4685 0.9429 0.098 Uiso 0.50 1 calc PR C 2 H26D H 0.5665 0.5033 0.9333 0.098 Uiso 0.50 1 calc PR C 2 C36 C 0.6155(18) 0.411(2) 0.9455(9) 0.047(11) Uiso 0.50 1 d PD D 1 C361 C 0.578(2) 0.3667(18) 0.9408(8) 0.047(11) Uiso 0.50 1 d PD D 2 C46 C 0.581(3) 0.352(2) 0.9978(7) 0.088(7) Uiso 1 1 d D . . H46A H 0.6331 0.3169 1.0120 0.131 Uiso 0.50 1 calc PR D 1 H46B H 0.5436 0.3102 0.9934 0.131 Uiso 0.50 1 calc PR D 1 H46C H 0.5452 0.3896 1.0214 0.131 Uiso 0.50 1 calc PR D 1 H46D H 0.6076 0.2894 1.0096 0.131 Uiso 0.50 1 calc PR D 2 H46E H 0.5197 0.3625 1.0179 0.131 Uiso 0.50 1 calc PR D 2 H46F H 0.6186 0.3930 1.0024 0.131 Uiso 0.50 1 calc PR D 2 C56 C 0.674(2) 0.352(3) 0.9089(10) 0.088(7) Uiso 1 1 d D . . H56A H 0.7264 0.3188 0.9235 0.131 Uiso 0.50 1 calc PR D 1 H56B H 0.6960 0.3901 0.8755 0.131 Uiso 0.50 1 calc PR D 1 H56C H 0.6384 0.3093 0.9043 0.131 Uiso 0.50 1 calc PR D 1 H56D H 0.7022 0.2903 0.9204 0.131 Uiso 0.50 1 calc PR D 2 H56E H 0.7106 0.3943 0.9136 0.131 Uiso 0.50 1 calc PR D 2 H56F H 0.6720 0.3619 0.8725 0.131 Uiso 0.50 1 calc PR D 2 C66 C 0.671(3) 0.478(3) 0.9530(18) 0.088(7) Uiso 0.50 1 d PD D 1 H66A H 0.7240 0.4447 0.9670 0.131 Uiso 0.50 1 calc PR D 1 H66B H 0.6336 0.5142 0.9771 0.131 Uiso 0.50 1 calc PR D 1 H66C H 0.6918 0.5169 0.9198 0.131 Uiso 0.50 1 calc PR D 1 C661 C 0.521(3) 0.301(2) 0.9334(17) 0.088(7) Uiso 0.50 1 d PD D 2 H66D H 0.5485 0.2388 0.9452 0.131 Uiso 0.50 1 calc PR D 2 H66E H 0.5193 0.3101 0.8969 0.131 Uiso 0.50 1 calc PR D 2 H66F H 0.4594 0.3105 0.9535 0.131 Uiso 0.50 1 calc PR D 2 O17 O 0.4825(15) 0.7403(18) 0.6684(8) 0.073(7) Uiso 1 1 d D . . O27 O 0.6218(16) 0.7244(18) 0.6875(7) 0.048(5) Uiso 1 1 d D . . C17 C 0.5708(15) 0.747(2) 0.6558(7) 0.057(9) Uiso 1 1 d D . . C27 C 0.6084(18) 0.7821(15) 0.6000(7) 0.064(9) Uiso 1 1 d D . . H27A H 0.6680 0.8011 0.5971 0.077 Uiso 1 1 calc R . . H27B H 0.5675 0.8362 0.5876 0.077 Uiso 1 1 calc R . . C37 C 0.6203(17) 0.7162(16) 0.5651(7) 0.077(11) Uiso 1 1 d D . . C47 C 0.657(2) 0.763(2) 0.5082(8) 0.120(15) Uiso 1 1 d D . . H47A H 0.6647 0.7202 0.4856 0.180 Uiso 1 1 calc R . . H47B H 0.7153 0.7824 0.5058 0.180 Uiso 1 1 calc R . . H47C H 0.6135 0.8151 0.4977 0.180 Uiso 1 1 calc R . . C57 C 0.529(2) 0.6819(19) 0.5674(11) 0.060(9) Uiso 1 1 d D . . H57A H 0.5404 0.6382 0.5452 0.090 Uiso 1 1 calc R . . H57B H 0.4856 0.7328 0.5557 0.090 Uiso 1 1 calc R . . H57C H 0.5050 0.6532 0.6030 0.090 Uiso 1 1 calc R . . C67 C 0.691(2) 0.635(2) 0.5818(12) 0.094(12) Uiso 1 1 d D . . H67A H 0.6980 0.5904 0.5602 0.142 Uiso 1 1 calc R . . H67B H 0.6699 0.6066 0.6179 0.142 Uiso 1 1 calc R . . H67C H 0.7495 0.6553 0.5778 0.142 Uiso 1 1 calc R . . O18 O 0.5346(15) 0.7813(18) 0.8481(8) 0.069(6) Uiso 1 1 d D . . O28 O 0.6509(18) 0.7203(19) 0.7924(9) 0.069(6) Uiso 1 1 d D . . C18 C 0.6213(16) 0.769(2) 0.8247(9) 0.079(11) Uiso 1 1 d D . . C28 C 0.6861(17) 0.8098(19) 0.8431(7) 0.090(12) Uiso 1 1 d D . . H28A H 0.6737 0.8761 0.8330 0.108 Uiso 1 1 calc R . . H28B H 0.7485 0.7910 0.8252 0.108 Uiso 1 1 calc R . . C38 C 0.6823(14) 0.7848(18) 0.9005(8) 0.056(8) Uiso 1 1 d D . . C48 C 0.5977(19) 0.839(2) 0.9292(11) 0.087(11) Uiso 1 1 d D . . H48A H 0.5956 0.8226 0.9663 0.131 Uiso 1 1 calc R . . H48B H 0.5426 0.8257 0.9220 0.131 Uiso 1 1 calc R . . H48C H 0.6016 0.9037 0.9172 0.131 Uiso 1 1 calc R . . C58 C 0.7689(18) 0.804(2) 0.9147(12) 0.094(12) Uiso 1 1 d D . . H58A H 0.7649 0.7849 0.9520 0.142 Uiso 1 1 calc R . . H58B H 0.7732 0.8686 0.9043 0.142 Uiso 1 1 calc R . . H58C H 0.8228 0.7706 0.8968 0.142 Uiso 1 1 calc R . . C68 C 0.674(2) 0.6823(19) 0.9190(10) 0.092(12) Uiso 1 1 d D . . H68A H 0.6738 0.6645 0.9560 0.138 Uiso 1 1 calc R . . H68B H 0.7262 0.6478 0.9002 0.138 Uiso 1 1 calc R . . H68C H 0.6180 0.6703 0.9124 0.138 Uiso 1 1 calc R . . O19 O 0.2942(15) 0.9869(17) 0.7632(9) 0.070(6) Uiso 1 1 d D . . O29 O 0.4210(17) 0.9319(16) 0.7966(8) 0.061(6) Uiso 1 1 d D . . C19 C 0.3799(15) 0.9871(18) 0.7655(9) 0.074(11) Uiso 1 1 d D . . C29 C 0.4287(16) 1.0588(16) 0.7273(8) 0.070(10) Uiso 1 1 d D . . H29A H 0.4591 1.0882 0.7459 0.084 Uiso 1 1 calc R . . H29B H 0.3835 1.1051 0.7120 0.084 Uiso 1 1 calc R . . C39 C 0.4988(15) 1.0245(18) 0.6844(8) 0.095(13) Uiso 1 1 d D . . C49 C 0.538(2) 1.106(2) 0.6443(11) 0.128(16) Uiso 1 1 d D . . H49A H 0.5847 1.0831 0.6172 0.192 Uiso 1 1 calc R . . H49B H 0.5643 1.1399 0.6616 0.192 Uiso 1 1 calc R . . H49C H 0.4890 1.1444 0.6290 0.192 Uiso 1 1 calc R . . C59 C 0.579(2) 0.959(3) 0.7049(13) 0.109(14) Uiso 1 1 d D . . H59A H 0.6216 0.9373 0.6761 0.164 Uiso 1 1 calc R . . H59B H 0.5547 0.9076 0.7300 0.164 Uiso 1 1 calc R . . H59C H 0.6096 0.9905 0.7214 0.164 Uiso 1 1 calc R . . C69 C 0.451(2) 0.974(2) 0.6576(12) 0.099(13) Uiso 1 1 d D . . H69A H 0.4955 0.9479 0.6310 0.149 Uiso 1 1 calc R . . H69B H 0.4043 1.0162 0.6417 0.149 Uiso 1 1 calc R . . H69C H 0.4221 0.9258 0.6832 0.149 Uiso 1 1 calc R . . O110 O 0.256(2) 0.948(2) 0.8799(10) 0.083(7) Uiso 1 1 d D . . O210 O 0.369(2) 0.836(2) 0.8977(10) 0.068(6) Uiso 1 1 d D . . C110 C 0.308(3) 0.897(2) 0.9111(11) 0.066(9) Uiso 1 1 d D F . C210 C 0.310(3) 0.931(3) 0.9578(14) 0.20(3) Uiso 1 1 d D . . H21A H 0.2952 0.9967 0.9467 0.241 Uiso 0.50 1 calc PR E 1 H21B H 0.3753 0.9208 0.9586 0.241 Uiso 0.50 1 calc PR E 1 H21C H 0.3400 0.8785 0.9794 0.241 Uiso 0.50 1 calc PR E 2 H21D H 0.2455 0.9374 0.9756 0.241 Uiso 0.50 1 calc PR E 2 C310 C 0.265(4) 0.914(4) 1.0149(15) 0.055(12) Uiso 0.50 1 d PD F 1 C410 C 0.296(7) 0.975(6) 1.042(2) 0.24(3) Uiso 0.50 1 d PD F 1 H41A H 0.2716 0.9603 1.0789 0.365 Uiso 0.50 1 calc PR F 1 H41B H 0.2738 1.0381 1.0283 0.365 Uiso 0.50 1 calc PR F 1 H41C H 0.3623 0.9670 1.0354 0.365 Uiso 0.50 1 calc PR F 1 C510 C 0.291(8) 0.815(4) 1.040(2) 0.24(3) Uiso 0.50 1 d PD F 1 H51A H 0.2624 0.8047 1.0764 0.365 Uiso 0.50 1 calc PR F 1 H51B H 0.3571 0.8028 1.0360 0.365 Uiso 0.50 1 calc PR F 1 H51C H 0.2707 0.7759 1.0228 0.365 Uiso 0.50 1 calc PR F 1 C610 C 0.161(4) 0.933(9) 1.020(3) 0.24(3) Uiso 0.50 1 d PD F 1 H61A H 0.1323 0.9168 1.0568 0.365 Uiso 0.50 1 calc PR F 1 H61B H 0.1420 0.8983 1.0004 0.365 Uiso 0.50 1 calc PR F 1 H61C H 0.1440 0.9976 1.0076 0.365 Uiso 0.50 1 calc PR F 1 C320 C 0.346(4) 1.011(3) 0.9666(18) 0.055(12) Uiso 0.50 1 d PD F 2 C420 C 0.359(16) 0.992(8) 1.022(3) 0.24(3) Uiso 0.25 1 d PD F 2 H42A H 0.3796 1.0445 1.0282 0.365 Uiso 0.25 1 calc PR F 2 H42B H 0.4048 0.9395 1.0278 0.365 Uiso 0.25 1 calc PR F 2 H42C H 0.3016 0.9807 1.0460 0.365 Uiso 0.25 1 calc PR F 2 C520 C 0.277(9) 1.096(4) 0.957(9) 0.24(3) Uiso 0.25 1 d PD F 2 H52A H 0.2978 1.1459 0.9652 0.365 Uiso 0.25 1 calc PR F 2 H52B H 0.2179 1.0851 0.9794 0.365 Uiso 0.25 1 calc PR F 2 H52C H 0.2715 1.1101 0.9210 0.365 Uiso 0.25 1 calc PR F 2 C620 C 0.436(9) 1.025(11) 0.929(7) 0.24(3) Uiso 0.25 1 d PD F 2 H62A H 0.4599 1.0754 0.9358 0.365 Uiso 0.25 1 calc PR F 2 H62B H 0.4274 1.0388 0.8939 0.365 Uiso 0.25 1 calc PR F 2 H62C H 0.4797 0.9704 0.9348 0.365 Uiso 0.25 1 calc PR F 2 C720 C 0.436(9) 1.025(12) 0.929(7) 0.24(3) Uiso 0.25 1 d PD F 2 H72A H 0.4574 1.0784 0.9338 0.365 Uiso 0.25 1 calc PR F 2 H72B H 0.4287 1.0335 0.8940 0.365 Uiso 0.25 1 calc PR F 2 H72C H 0.4812 0.9722 0.9369 0.365 Uiso 0.25 1 calc PR F 2 C820 C 0.359(16) 0.992(9) 1.022(3) 0.24(3) Uiso 0.25 1 d PD F 2 H82A H 0.3802 1.0442 1.0281 0.365 Uiso 0.25 1 calc PR F 2 H82B H 0.4039 0.9390 1.0280 0.365 Uiso 0.25 1 calc PR F 2 H82C H 0.3012 0.9818 1.0460 0.365 Uiso 0.25 1 calc PR F 2 C920 C 0.277(10) 1.096(5) 0.957(10) 0.24(3) Uiso 0.25 1 d PD F 2 H92A H 0.3009 1.1473 0.9616 0.365 Uiso 0.25 1 calc PR F 2 H92B H 0.2197 1.0874 0.9817 0.365 Uiso 0.25 1 calc PR F 2 H92C H 0.2670 1.1065 0.9219 0.365 Uiso 0.25 1 calc PR F 2 O111 O 0.050(2) 1.006(2) 0.7561(11) 0.083(7) Uiso 1 1 d D . . O211 O 0.1188(19) 1.010(2) 0.8204(10) 0.066(6) Uiso 1 1 d D . . C111 C 0.0605(19) 1.042(2) 0.7935(10) 0.077(10) Uiso 1 1 d D . . C211 C -0.013(2) 1.115(2) 0.8090(9) 0.087(12) Uiso 1 1 d D . . H21E H -0.0538 1.1303 0.7840 0.104 Uiso 1 1 calc R . . H21F H 0.0149 1.1690 0.8064 0.104 Uiso 1 1 calc R . . C311 C -0.0699(18) 1.092(2) 0.8627(9) 0.078(11) Uiso 1 1 d D . . C411 C -0.137(2) 1.177(2) 0.8745(11) 0.081(11) Uiso 1 1 d D . . H41D H -0.1773 1.1611 0.9082 0.121 Uiso 0.50 1 calc PR . . H41E H -0.1736 1.1979 0.8479 0.121 Uiso 0.50 1 calc PR . . H41F H -0.1030 1.2240 0.8749 0.121 Uiso 0.50 1 calc PR . . H41G H -0.1253 1.2276 0.8458 0.121 Uiso 0.50 1 calc PR . . H41H H -0.1290 1.1907 0.9061 0.121 Uiso 0.50 1 calc PR . . H41I H -0.1996 1.1646 0.8791 0.121 Uiso 0.50 1 calc PR . . C511 C -0.011(2) 1.059(3) 0.9048(11) 0.086(11) Uiso 1 1 d D . . H51D H -0.0510 1.0444 0.9387 0.129 Uiso 0.50 1 calc PR . . H51E H 0.0229 1.1070 0.9044 0.129 Uiso 0.50 1 calc PR . . H51F H 0.0309 1.0056 0.8977 0.129 Uiso 0.50 1 calc PR . . H51G H 0.0529 1.0603 0.8885 0.129 Uiso 0.50 1 calc PR . . H51H H -0.0211 0.9977 0.9228 0.129 Uiso 0.50 1 calc PR . . H51I H -0.0290 1.0990 0.9295 0.129 Uiso 0.50 1 calc PR . . C611 C -0.126(3) 1.016(3) 0.8644(16) 0.20(3) Uiso 1 1 d D . . H61D H -0.1653 1.0022 0.8984 0.299 Uiso 0.50 1 calc PR . . H61E H -0.0843 0.9615 0.8577 0.299 Uiso 0.50 1 calc PR . . H61F H -0.1629 1.0357 0.8380 0.299 Uiso 0.50 1 calc PR . . H61G H -0.1097 0.9974 0.8310 0.299 Uiso 0.50 1 calc PR . . H61H H -0.1907 1.0381 0.8717 0.299 Uiso 0.50 1 calc PR . . H61I H -0.1121 0.9639 0.8914 0.299 Uiso 0.50 1 calc PR . . O112 O 0.1673(17) 0.6953(18) 0.8548(7) 0.055(5) Uiso 1 1 d D . . O212 O 0.114(2) 0.8273(17) 0.8811(9) 0.081(7) Uiso 1 1 d D . . C112 C 0.115(2) 0.7444(17) 0.8873(8) 0.092(13) Uiso 1 1 d D . . C212 C 0.0690(19) 0.694(2) 0.9381(8) 0.090(12) Uiso 1 1 d D G . H21G H 0.0922 0.6288 0.9407 0.108 Uiso 1 1 calc R . . H21H H 0.0032 0.7009 0.9388 0.108 Uiso 1 1 calc R . . C312 C 0.083(2) 0.7227(18) 0.9847(8) 0.098(13) Uiso 1 1 d D . . C412 C 0.014(7) 0.806(7) 0.995(4) 0.147(14) Uiso 0.25 1 d PD G 1 H41J H 0.0206 0.8217 1.0264 0.221 Uiso 0.25 1 calc PR G 1 H41K H -0.0476 0.7918 0.9993 0.221 Uiso 0.25 1 calc PR G 1 H41L H 0.0255 0.8560 0.9658 0.221 Uiso 0.25 1 calc PR G 1 C512 C 0.179(4) 0.747(10) 0.975(3) 0.147(14) Uiso 0.25 1 d PD G 1 H51J H 0.1870 0.7662 1.0051 0.221 Uiso 0.25 1 calc PR G 1 H51K H 0.1884 0.7952 0.9447 0.221 Uiso 0.25 1 calc PR G 1 H51L H 0.2230 0.6936 0.9693 0.221 Uiso 0.25 1 calc PR G 1 C612 C 0.069(11) 0.646(4) 1.0323(16) 0.147(14) Uiso 0.25 1 d PD G 1 H61J H 0.0739 0.6668 1.0626 0.221 Uiso 0.25 1 calc PR G 1 H61K H 0.1150 0.5946 1.0269 0.221 Uiso 0.25 1 calc PR G 1 H61L H 0.0084 0.6285 1.0376 0.221 Uiso 0.25 1 calc PR G 1 C422 C 0.038(4) 0.663(3) 1.0343(8) 0.147(14) Uiso 0.75 1 d PD G 2 H42D H 0.0433 0.6845 1.0642 0.221 Uiso 0.75 1 calc PR G 2 H42E H 0.0675 0.6008 1.0362 0.221 Uiso 0.75 1 calc PR G 2 H42F H -0.0267 0.6652 1.0343 0.221 Uiso 0.75 1 calc PR G 2 C522 C 0.185(2) 0.713(4) 0.9838(17) 0.147(14) Uiso 0.75 1 d PD G 2 H52D H 0.1934 0.7348 1.0131 0.221 Uiso 0.75 1 calc PR G 2 H52E H 0.2145 0.7493 0.9516 0.221 Uiso 0.75 1 calc PR G 2 H52F H 0.2108 0.6501 0.9862 0.221 Uiso 0.75 1 calc PR G 2 C622 C 0.041(4) 0.821(2) 0.9843(17) 0.147(14) Uiso 0.75 1 d PD G 2 H62D H 0.0497 0.8386 1.0147 0.221 Uiso 0.75 1 calc PR G 2 H62E H -0.0238 0.8274 0.9846 0.221 Uiso 0.75 1 calc PR G 2 H62F H 0.0710 0.8595 0.9531 0.221 Uiso 0.75 1 calc PR G 2 O113 O 0.0361(18) 0.9659(18) 0.6698(10) 0.077(7) Uiso 1 1 d D . . O213 O -0.0063(19) 0.8576(15) 0.6403(9) 0.077(7) Uiso 1 1 d D . . C113 C -0.0119(18) 0.9375(17) 0.6437(11) 0.076(11) Uiso 1 1 d D . . C213 C -0.0836(19) 1.0057(19) 0.6220(9) 0.068(9) Uiso 1 1 d D . . H21I H -0.1164 0.9755 0.6052 0.081 Uiso 1 1 calc R . . H21J H -0.0535 1.0523 0.5951 0.081 Uiso 1 1 calc R . . C313 C -0.1522(18) 1.052(2) 0.6609(11) 0.121(16) Uiso 1 1 d D . . C413 C -0.183(3) 0.981(3) 0.7106(12) 0.140(18) Uiso 1 1 d D . . H41M H -0.2250 1.0112 0.7363 0.210 Uiso 1 1 calc R . . H41N H -0.1297 0.9493 0.7247 0.210 Uiso 1 1 calc R . . H41O H -0.2130 0.9372 0.7022 0.210 Uiso 1 1 calc R . . C513 C -0.114(3) 1.126(3) 0.6763(16) 0.125(16) Uiso 1 1 d D . . H51M H -0.1601 1.1527 0.7020 0.187 Uiso 1 1 calc R . . H51N H -0.0972 1.1725 0.6457 0.187 Uiso 1 1 calc R . . H51O H -0.0601 1.0991 0.6908 0.187 Uiso 1 1 calc R . . C613 C -0.237(2) 1.096(3) 0.6367(17) 0.17(2) Uiso 1 1 d D . . H61M H -0.2810 1.1273 0.6610 0.259 Uiso 1 1 calc R . . H61N H -0.2639 1.0488 0.6294 0.259 Uiso 1 1 calc R . . H61O H -0.2176 1.1383 0.6047 0.259 Uiso 1 1 calc R . . O114 O 0.2659(14) 0.3085(16) 0.7159(8) 0.049(5) Uiso 1 1 d D . . O214 O 0.1494(16) 0.4033(14) 0.6855(7) 0.039(5) Uiso 1 1 d D . . C114 C 0.1915(16) 0.3263(14) 0.6964(10) 0.055(8) Uiso 1 1 d D . . C214 C 0.1561(15) 0.2480(14) 0.6877(6) 0.058(9) Uiso 1 1 d D . . H21K H 0.0891 0.2579 0.6966 0.070 Uiso 1 1 calc R . . H21L H 0.1769 0.1930 0.7114 0.070 Uiso 1 1 calc R . . C314 C 0.1855(13) 0.2323(13) 0.6331(7) 0.043(7) Uiso 1 1 d D . . C414 C 0.2876(15) 0.192(2) 0.6237(9) 0.059(9) Uiso 1 1 d D . . H41P H 0.3072 0.1818 0.5883 0.089 Uiso 1 1 calc R . . H41Q H 0.2959 0.1341 0.6479 0.089 Uiso 1 1 calc R . . H41R H 0.3240 0.2333 0.6289 0.089 Uiso 1 1 calc R . . C514 C 0.1279(18) 0.1680(17) 0.6224(10) 0.058(9) Uiso 1 1 d D . . H51P H 0.1492 0.1595 0.5868 0.087 Uiso 1 1 calc R . . H51Q H 0.0640 0.1944 0.6274 0.087 Uiso 1 1 calc R . . H51R H 0.1343 0.1098 0.6461 0.087 Uiso 1 1 calc R . . C614 C 0.1745(19) 0.3248(15) 0.5951(8) 0.050(8) Uiso 1 1 d D . . H61P H 0.1940 0.3159 0.5596 0.074 Uiso 1 1 calc R . . H61Q H 0.2118 0.3650 0.6009 0.074 Uiso 1 1 calc R . . H61R H 0.1107 0.3516 0.6009 0.074 Uiso 1 1 calc R . . O115 O 0.2165(16) 0.5113(14) 0.8243(7) 0.056(6) Uiso 1 1 d D . . O215 O 0.2418(19) 0.3637(16) 0.8202(8) 0.068(6) Uiso 1 1 d D . . C115 C 0.2121(18) 0.4248(15) 0.8450(6) 0.046(8) Uiso 1 1 d D . . C215 C 0.1646(14) 0.4024(17) 0.9002(6) 0.054(8) Uiso 1 1 d D . . H21M H 0.1385 0.3460 0.9058 0.064 Uiso 1 1 calc R . . H21N H 0.1136 0.4507 0.9066 0.064 Uiso 1 1 calc R . . C315 C 0.2230(16) 0.3913(17) 0.9394(7) 0.100(14) Uiso 1 1 d D . . C415 C 0.291(2) 0.303(2) 0.9378(11) 0.077(10) Uiso 1 1 d D . . H41S H 0.3288 0.2953 0.9634 0.116 Uiso 0.50 1 calc PR . . H41T H 0.3301 0.3068 0.9034 0.116 Uiso 0.50 1 calc PR . . H41U H 0.2576 0.2515 0.9457 0.116 Uiso 0.50 1 calc PR . . H41V H 0.2822 0.2738 0.9116 0.116 Uiso 0.50 1 calc PR . . H41W H 0.2809 0.2623 0.9716 0.116 Uiso 0.50 1 calc PR . . H41X H 0.3534 0.3175 0.9293 0.116 Uiso 0.50 1 calc PR . . C515 C 0.165(2) 0.386(2) 0.9951(7) 0.095(12) Uiso 1 1 d D . . H51S H 0.2052 0.3790 1.0193 0.142 Uiso 1 1 calc R . . H51T H 0.1308 0.3352 1.0044 0.142 Uiso 1 1 calc R . . H51U H 0.1229 0.4421 0.9966 0.142 Uiso 1 1 calc R . . C615 C 0.2774(19) 0.473(2) 0.9249(11) 0.070(10) Uiso 1 1 d D . . H61S H 0.3159 0.4663 0.9498 0.105 Uiso 1 1 calc R . . H61T H 0.2350 0.5287 0.9254 0.105 Uiso 1 1 calc R . . H61U H 0.3153 0.4752 0.8903 0.105 Uiso 1 1 calc R . . O116 O 0.036(2) 0.5540(18) 0.7253(9) 0.085(4) Uiso 1 1 d D . . O216 O 0.001(2) 0.7041(16) 0.7219(8) 0.085(4) Uiso 1 1 d D . . C116 C 0.004(2) 0.6249(17) 0.7471(8) 0.085(4) Uiso 1 1 d D . . C216 C -0.001(2) 0.609(2) 0.8042(8) 0.085(4) Uiso 1 1 d D . . H210 H -0.0221 0.6664 0.8157 0.102 Uiso 1 1 calc R . . H21P H 0.0612 0.5877 0.8110 0.102 Uiso 1 1 calc R . . C316 C -0.062(2) 0.5404(19) 0.8360(8) 0.085(4) Uiso 1 1 d D . . C416 C -0.018(3) 0.4450(19) 0.8266(14) 0.141(18) Uiso 1 1 d D . . H41Y H -0.0584 0.4007 0.8461 0.212 Uiso 1 1 calc R . . H41Z H 0.0400 0.4296 0.8379 0.212 Uiso 1 1 calc R . . H411 H -0.0075 0.4448 0.7898 0.212 Uiso 1 1 calc R . . C516 C -0.158(2) 0.561(4) 0.8222(19) 0.36(6) Uiso 1 1 d D . . H51V H -0.1947 0.5140 0.8421 0.545 Uiso 1 1 calc R . . H51W H -0.1520 0.5640 0.7853 0.545 Uiso 1 1 calc R . . H51X H -0.1882 0.6193 0.8304 0.545 Uiso 1 1 calc R . . C616 C -0.073(3) 0.543(3) 0.8940(9) 0.17(2) Uiso 1 1 d D . . H61V H -0.1111 0.4980 0.9154 0.254 Uiso 1 1 calc R . . H61W H -0.1005 0.6027 0.8998 0.254 Uiso 1 1 calc R . . H61X H -0.0127 0.5291 0.9030 0.254 Uiso 1 1 calc R . . O117 O 0.108(2) 0.5538(16) 0.6155(9) 0.062(6) Uiso 1 1 d D . . O217 O 0.0388(18) 0.6984(14) 0.6100(8) 0.053(5) Uiso 1 1 d D . . C117 C 0.0549(19) 0.6251(15) 0.5957(8) 0.028(6) Uiso 1 1 d D . . C217 C 0.0155(16) 0.6164(18) 0.5521(8) 0.069(10) Uiso 1 1 d D . . H21Q H -0.0376 0.6632 0.5491 0.083 Uiso 1 1 calc R . . H21R H -0.0065 0.5571 0.5607 0.083 Uiso 1 1 calc R . . C317 C 0.0808(18) 0.6250(18) 0.5004(8) 0.063(9) Uiso 1 1 d D . . C417 C 0.025(2) 0.654(2) 0.4567(9) 0.070(10) Uiso 1 1 d D . . H412 H 0.0672 0.6580 0.4232 0.105 Uiso 1 1 calc R . . H413 H -0.0104 0.7130 0.4589 0.105 Uiso 1 1 calc R . . H414 H -0.0151 0.6097 0.4606 0.105 Uiso 1 1 calc R . . C517 C 0.144(3) 0.535(2) 0.4945(12) 0.114(15) Uiso 1 1 d D . . H51Y H 0.1828 0.5419 0.4601 0.171 Uiso 1 1 calc R . . H51Z H 0.1062 0.4871 0.4990 0.171 Uiso 1 1 calc R . . H511 H 0.1810 0.5184 0.5207 0.171 Uiso 1 1 calc R . . C617 C 0.141(2) 0.699(2) 0.4958(13) 0.138(18) Uiso 1 1 d D . . H61Y H 0.1827 0.7062 0.4623 0.208 Uiso 1 1 calc R . . H61Z H 0.1754 0.6816 0.5233 0.208 Uiso 1 1 calc R . . H611 H 0.1019 0.7563 0.4989 0.208 Uiso 1 1 calc R . . O118 O 0.311(2) 0.773(2) 0.6171(10) 0.063(6) Uiso 1 1 d D H . O218 O 0.1909(19) 0.808(2) 0.5783(10) 0.085(7) Uiso 1 1 d D H . C118 C 0.2735(19) 0.806(2) 0.5762(9) 0.071(8) Uiso 1 1 d D . . C218 C 0.341(3) 0.847(3) 0.5292(17) 0.071(8) Uiso 0.50 1 d PD H 1 H21S H 0.3990 0.8496 0.5390 0.085 Uiso 0.50 1 calc PR H 1 H21T H 0.3546 0.8108 0.5023 0.085 Uiso 0.50 1 calc PR H 1 C318 C 0.297(3) 0.942(3) 0.5093(15) 0.071(8) Uiso 0.50 1 d PD H 1 C418 C 0.370(6) 1.002(3) 0.481(3) 0.122(14) Uiso 0.50 1 d PD H 1 H415 H 0.3428 1.0563 0.4598 0.184 Uiso 0.50 1 calc PR H 1 H416 H 0.4171 0.9690 0.4580 0.184 Uiso 0.50 1 calc PR H 1 H417 H 0.3972 1.0185 0.5055 0.184 Uiso 0.50 1 calc PR H 1 C518 C 0.237(5) 0.937(6) 0.472(3) 0.122(14) Uiso 0.50 1 d PD H 1 H512 H 0.1915 0.8975 0.4906 0.184 Uiso 0.50 1 calc PR H 1 H513 H 0.2754 0.9127 0.4432 0.184 Uiso 0.50 1 calc PR H 1 H514 H 0.2076 0.9972 0.4600 0.184 Uiso 0.50 1 calc PR H 1 C618 C 0.238(5) 0.982(6) 0.555(2) 0.122(14) Uiso 0.50 1 d PD H 1 H612 H 0.1962 0.9396 0.5755 0.184 Uiso 0.50 1 calc PR H 1 H613 H 0.2032 1.0389 0.5414 0.184 Uiso 0.50 1 calc PR H 1 H614 H 0.2769 0.9920 0.5758 0.184 Uiso 0.50 1 calc PR H 1 C228 C 0.320(4) 0.862(3) 0.5255(16) 0.071(8) Uiso 0.50 1 d PD H 2 H22A H 0.2879 0.8580 0.4987 0.085 Uiso 0.50 1 calc PR H 2 H22B H 0.3822 0.8302 0.5167 0.085 Uiso 0.50 1 calc PR H 2 C328 C 0.329(3) 0.961(3) 0.5193(15) 0.071(8) Uiso 0.50 1 d PD H 2 C428 C 0.234(4) 1.015(5) 0.527(3) 0.122(14) Uiso 0.50 1 d PD H 2 H42G H 0.1987 0.9906 0.5612 0.184 Uiso 0.50 1 calc PR H 2 H42H H 0.2030 1.0117 0.5005 0.184 Uiso 0.50 1 calc PR H 2 H42I H 0.2392 1.0783 0.5255 0.184 Uiso 0.50 1 calc PR H 2 C528 C 0.381(5) 0.996(3) 0.465(2) 0.122(14) Uiso 0.50 1 d PD H 2 H52G H 0.3880 1.0588 0.4611 0.184 Uiso 0.50 1 calc PR H 2 H52H H 0.3476 0.9904 0.4396 0.184 Uiso 0.50 1 calc PR H 2 H52I H 0.4410 0.9599 0.4593 0.184 Uiso 0.50 1 calc PR H 2 C628 C 0.379(5) 0.972(6) 0.559(3) 0.122(14) Uiso 0.50 1 d PD H 2 H62G H 0.3425 0.9549 0.5938 0.184 Uiso 0.50 1 calc PR H 2 H62H H 0.3898 1.0342 0.5530 0.184 Uiso 0.50 1 calc PR H 2 H62I H 0.4373 0.9324 0.5562 0.184 Uiso 0.50 1 calc PR H 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 0.071(9) 0.065(9) 0.036(5) -0.020(7) -0.029(7) 0.033(9) Mn2 0.055(8) 0.043(9) 0.034(5) -0.011(6) -0.025(6) 0.010(9) Mn3 0.038(8) 0.031(8) 0.054(5) 0.002(6) -0.022(6) -0.005(9) Mn4 0.067(8) 0.058(9) 0.065(5) -0.032(6) -0.034(6) 0.028(9) Mn5 0.094(11) 0.067(11) 0.076(6) -0.037(8) -0.034(8) 0.040(11) Mn6 0.107(9) 0.090(9) 0.064(5) -0.045(7) -0.055(7) 0.047(9) Mn7 0.075(8) 0.082(9) 0.070(5) -0.041(7) -0.047(6) 0.035(9) Mn8 0.105(9) 0.048(8) 0.101(6) -0.035(7) -0.081(7) 0.049(9) Mn9 0.098(9) 0.093(9) 0.068(5) -0.047(7) -0.057(7) 0.044(9) Mn10 0.072(8) 0.076(9) 0.049(4) -0.027(6) -0.039(6) 0.030(8) Mn11 0.080(9) 0.081(9) 0.073(5) -0.016(7) -0.056(7) 0.036(9) Mn12 0.072(11) 0.058(11) 0.096(6) -0.029(8) -0.046(8) 0.034(11) _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 O17 1.85(3) . ? Mn1 O124 1.86(4) . ? Mn1 O108 1.860(14) . ? Mn1 O107 1.91(2) . ? Mn1 O134 1.907(16) . ? Mn1 O123 1.93(3) . ? Mn1 Mn7 2.771(7) . ? Mn1 Mn2 2.815(13) . ? Mn1 Mn4 2.819(9) . ? Mn1 Mn3 2.927(7) . ? Mn2 O209 1.81(2) . ? Mn2 O115 1.84(3) . ? Mn2 O208 1.849(15) . ? Mn2 O123 1.85(4) . ? Mn2 O124 1.90(3) . ? Mn2 O234 1.944(15) . ? Mn2 Mn9 2.778(8) . ? Mn2 Mn3 2.799(9) . ? Mn2 Mn4 2.885(8) . ? Mn3 O234 1.75(3) . ? Mn3 O134 1.84(3) . ? Mn3 O311 1.857(17) . ? Mn3 O123 1.871(15) . ? Mn3 O118 1.90(4) . ? Mn3 O310 1.97(3) . ? Mn3 Mn11 2.753(7) . ? Mn3 Mn4 2.802(5) . ? Mn4 O234 1.81(2) . ? Mn4 O134 1.84(4) . ? Mn4 O112 1.85(3) . ? Mn4 O405 1.857(19) . ? Mn4 O124 1.936(14) . ? Mn4 O406 1.96(3) . ? Mn4 Mn5 2.825(9) . ? Mn5 O406 1.786(16) . ? Mn5 O211 1.883(16) . ? Mn5 O405 1.93(2) . ? Mn5 O19 2.05(3) . ? Mn5 O110 2.06(2) . ? Mn5 O212 2.17(3) . ? Mn6 O406 1.85(3) . ? Mn6 O18 1.85(2) . ? Mn6 O107 1.885(15) . ? Mn6 O210 1.940(18) . ? Mn6 O29 2.10(3) . ? Mn6 O6 2.41(4) . ? Mn7 O108 1.88(3) . ? Mn7 O28 1.91(3) . ? Mn7 O107 1.944(15) . ? Mn7 O15 1.97(2) . ? Mn7 O16 2.09(2) . ? Mn7 O27 2.18(3) . ? Mn8 O108 1.88(3) . ? Mn8 O13 1.89(3) . ? Mn8 O208 1.90(3) . ? Mn8 O25 2.03(3) . ? Mn8 O14 2.105(17) . ? Mn8 O26 2.19(2) . ? Mn9 O208 1.87(3) . ? Mn9 O209 1.925(16) . ? Mn9 O114 1.93(2) . ? Mn9 O23 1.94(2) . ? Mn9 O24 2.07(2) . ? Mn9 O215 2.18(3) . ? Mn10 O310 1.77(4) . ? Mn10 O209 1.888(14) . ? Mn10 O117 1.931(14) . ? Mn10 O214 1.97(3) . ? Mn10 O116 2.19(3) . ? Mn10 O10 2.20(3) . ? Mn11 O311 1.84(3) . ? Mn11 O217 1.88(2) . ? Mn11 O310 1.944(16) . ? Mn11 O213 1.953(17) . ? Mn11 O216 2.13(3) . ? Mn11 O218 2.21(4) . ? Mn12 O113 1.891(18) . ? Mn12 O311 1.890(19) . ? Mn12 O111 1.905(18) . ? Mn12 O405 1.909(16) . ? Mn12 O121 2.15(5) . ? Mn12 O120 2.29(6) . ? O13 C13 1.301(11) . ? O23 C13 1.227(11) . ? C13 C231 1.501(9) . ? C13 C23 1.501(9) . ? C23 C33 1.496(8) . ? C33 C43 1.500(8) . ? C33 C63 1.500(8) . ? C33 C53 1.501(8) . ? C231 C331 1.500(8) . ? C331 C431 1.500(8) . ? C331 C631 1.500(8) . ? C331 C531 1.501(8) . ? O14 C14 1.306(11) . ? O24 C14 1.224(11) . ? C14 C24 1.464(13) . ? C24 C34 1.481(11) . ? C34 C64 1.529(9) . ? C34 C44 1.530(9) . ? C34 C54 1.532(9) . ? O15 C15 1.304(11) . ? O25 C15 1.225(11) . ? C15 C251 1.500(9) . ? C15 C25 1.501(9) . ? C25 C35 1.499(8) . ? C35 C45 1.499(8) . ? C35 C65 1.501(8) . ? C35 C55 1.501(8) . ? C251 C351 1.50(2) . ? C351 C451 1.497(9) . ? C351 C551 1.498(9) . ? C351 C651 1.505(9) . ? O16 C16 1.302(11) . ? O26 C16 1.223(11) . ? C16 C26 1.468(13) . ? C26 C36 1.500(8) . ? C26 C361 1.502(8) . ? C36 C56 1.498(8) . ? C36 C46 1.502(8) . ? C36 C66 1.502(8) . ? C361 C46 1.499(8) . ? C361 C56 1.500(8) . ? C361 C661 1.503(8) . ? O17 C17 1.303(11) . ? O27 C17 1.223(11) . ? C17 C27 1.469(13) . ? C27 C37 1.484(11) . ? C37 C67 1.528(9) . ? C37 C57 1.531(9) . ? C37 C47 1.531(9) . ? O18 C18 1.302(11) . ? O28 C18 1.224(11) . ? C18 C28 1.468(13) . ? C28 C38 1.483(11) . ? C38 C48 1.528(9) . ? C38 C68 1.530(9) . ? C38 C58 1.531(9) . ? O19 C19 1.302(11) . ? O29 C19 1.223(11) . ? C19 C29 1.471(13) . ? C29 C39 1.486(11) . ? C39 C49 1.528(9) . ? C39 C69 1.528(9) . ? C39 C59 1.531(9) . ? O110 C110 1.304(11) . ? O210 C110 1.227(11) . ? C110 C210 1.470(13) . ? C210 C310 1.498(8) . ? C210 C320 1.499(7) . ? C310 C610 1.500(8) . ? C310 C510 1.501(8) . ? C310 C410 1.501(8) . ? C320 C720 1.500(8) . ? C320 C620 1.500(8) . ? C320 C520 1.500(8) . ? C320 C920 1.500(8) . ? C320 C420 1.501(8) . ? C320 C820 1.501(8) . ? O111 C111 1.303(11) . ? O211 C111 1.226(11) . ? C111 C211 1.467(13) . ? C211 C311 1.484(11) . ? C311 C511 1.528(9) . ? C311 C611 1.529(10) . ? C311 C411 1.530(9) . ? O112 C112 1.304(11) . ? O212 C112 1.225(11) . ? C112 C212 1.469(13) . ? C212 C312 1.487(9) . ? C312 C622 1.501(8) . ? C312 C612 1.503(8) . ? C312 C422 1.503(8) . ? C312 C412 1.503(8) . ? C312 C512 1.504(8) . ? C312 C522 1.507(8) . ? O113 C113 1.299(11) . ? O213 C113 1.222(11) . ? C113 C213 1.471(13) . ? C213 C313 1.482(11) . ? C313 C513 1.530(9) . ? C313 C413 1.530(10) . ? C313 C613 1.531(10) . ? O114 C114 1.302(11) . ? O214 C114 1.224(11) . ? C114 C214 1.470(13) . ? C214 C314 1.485(11) . ? C314 C514 1.528(9) . ? C314 C414 1.529(9) . ? C314 C614 1.530(9) . ? O115 C115 1.301(11) . ? O215 C115 1.223(10) . ? C115 C215 1.467(13) . ? C215 C315 1.482(11) . ? C315 C615 1.529(9) . ? C315 C515 1.530(9) . ? C315 C415 1.530(9) . ? O116 C116 1.305(11) . ? O216 C116 1.226(11) . ? C116 C216 1.475(13) . ? C216 C316 1.487(11) . ? C316 C516 1.528(9) . ? C316 C416 1.528(9) . ? C316 C616 1.530(9) . ? O117 C117 1.304(11) . ? O217 C117 1.224(11) . ? C117 C217 1.468(13) . ? C217 C317 1.485(11) . ? C317 C417 1.528(9) . ? C317 C617 1.529(10) . ? C317 C517 1.531(9) . ? O118 C118 1.304(11) . ? O218 C118 1.225(11) . ? C118 C228 1.499(9) . ? C118 C218 1.500(9) . ? C218 C318 1.500(8) . ? C318 C418 1.500(8) . ? C318 C618 1.500(8) . ? C318 C518 1.501(8) . ? C228 C328 1.500(8) . ? C328 C628 1.499(8) . ? C328 C528 1.501(8) . ? C328 C428 1.502(8) . ? 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 O17 Mn1 O124 171.6(9) . . ? O17 Mn1 O108 92.6(12) . . ? O124 Mn1 O108 93.3(12) . . ? O17 Mn1 O107 94.9(13) . . ? O124 Mn1 O107 91.5(12) . . ? O108 Mn1 O107 85.9(9) . . ? O17 Mn1 O134 91.1(13) . . ? O124 Mn1 O134 82.3(13) . . ? O108 Mn1 O134 171.5(17) . . ? O107 Mn1 O134 101.4(9) . . ? O17 Mn1 O123 91.2(11) . . ? O124 Mn1 O123 82.3(13) . . ? O108 Mn1 O123 95.7(9) . . ? O107 Mn1 O123 173.6(14) . . ? O134 Mn1 O123 76.5(10) . . ? O17 Mn1 Mn7 87.3(7) . . ? O124 Mn1 Mn7 101.1(6) . . ? O108 Mn1 Mn7 42.6(9) . . ? O107 Mn1 Mn7 44.5(5) . . ? O134 Mn1 Mn7 145.4(10) . . ? O123 Mn1 Mn7 138.0(5) . . ? O17 Mn1 Mn2 132.0(7) . . ? O124 Mn1 Mn2 42.1(8) . . ? O108 Mn1 Mn2 89.7(12) . . ? O107 Mn1 Mn2 133.1(10) . . ? O134 Mn1 Mn2 82.1(14) . . ? O123 Mn1 Mn2 41.0(10) . . ? Mn7 Mn1 Mn2 123.3(3) . . ? O17 Mn1 Mn4 131.1(6) . . ? O124 Mn1 Mn4 43.1(5) . . ? O108 Mn1 Mn4 136.2(11) . . ? O107 Mn1 Mn4 90.9(7) . . ? O134 Mn1 Mn4 40.4(10) . . ? O123 Mn1 Mn4 83.6(7) . . ? Mn7 Mn1 Mn4 127.05(18) . . ? Mn2 Mn1 Mn4 61.6(3) . . ? O17 Mn1 Mn3 88.2(6) . . ? O124 Mn1 Mn3 83.3(7) . . ? O108 Mn1 Mn3 134.7(8) . . ? O107 Mn1 Mn3 139.1(5) . . ? O134 Mn1 Mn3 37.8(8) . . ? O123 Mn1 Mn3 39.0(5) . . ? Mn7 Mn1 Mn3 174.6(2) . . ? Mn2 Mn1 Mn3 58.3(2) . . ? Mn4 Mn1 Mn3 58.35(17) . . ? O209 Mn2 O115 93.8(13) . . ? O209 Mn2 O208 84.8(9) . . ? O115 Mn2 O208 91.0(12) . . ? O209 Mn2 O123 90.3(12) . . ? O115 Mn2 O123 172.3(8) . . ? O208 Mn2 O123 95.8(12) . . ? O209 Mn2 O124 173.5(15) . . ? O115 Mn2 O124 92.7(10) . . ? O208 Mn2 O124 95.7(9) . . ? O123 Mn2 O124 83.2(13) . . ? O209 Mn2 O234 99.6(8) . . ? O115 Mn2 O234 94.3(11) . . ? O208 Mn2 O234 172.8(18) . . ? O123 Mn2 O234 78.5(11) . . ? O124 Mn2 O234 79.3(9) . . ? O209 Mn2 Mn9 43.6(5) . . ? O115 Mn2 Mn9 86.4(7) . . ? O208 Mn2 Mn9 42.1(9) . . ? O123 Mn2 Mn9 101.0(6) . . ? O124 Mn2 Mn9 137.7(5) . . ? O234 Mn2 Mn9 143.0(8) . . ? O209 Mn2 Mn3 88.9(8) . . ? O115 Mn2 Mn3 131.9(6) . . ? O208 Mn2 Mn3 137.0(11) . . ? O123 Mn2 Mn3 41.5(5) . . ? O124 Mn2 Mn3 86.2(8) . . ? O234 Mn2 Mn3 38.2(8) . . ? Mn9 Mn2 Mn3 124.50(18) . . ? O209 Mn2 Mn1 132.7(11) . . ? O115 Mn2 Mn1 133.5(7) . . ? O208 Mn2 Mn1 91.3(12) . . ? O123 Mn2 Mn1 43.1(8) . . ? O124 Mn2 Mn1 40.9(10) . . ? O234 Mn2 Mn1 81.6(11) . . ? Mn9 Mn2 Mn1 123.5(3) . . ? Mn3 Mn2 Mn1 62.8(3) . . ? O209 Mn2 Mn4 137.6(5) . . ? O115 Mn2 Mn4 89.6(6) . . ? O208 Mn2 Mn4 137.4(8) . . ? O123 Mn2 Mn4 83.0(7) . . ? O124 Mn2 Mn4 41.7(4) . . ? O234 Mn2 Mn4 38.1(7) . . ? Mn9 Mn2 Mn4 175.9(4) . . ? Mn3 Mn2 Mn4 59.06(19) . . ? Mn1 Mn2 Mn4 59.3(3) . . ? O234 Mn3 O134 78.5(12) . . ? O234 Mn3 O311 86.5(11) . . ? O134 Mn3 O311 96.9(9) . . ? O234 Mn3 O123 83.2(11) . . ? O134 Mn3 O123 79.7(10) . . ? O311 Mn3 O123 169.6(13) . . ? O234 Mn3 O118 178.1(14) . . ? O134 Mn3 O118 99.7(16) . . ? O311 Mn3 O118 94.0(11) . . ? O123 Mn3 O118 96.3(11) . . ? O234 Mn3 O310 91.1(14) . . ? O134 Mn3 O310 169.1(15) . . ? O311 Mn3 O310 85.7(10) . . ? O123 Mn3 O310 95.9(10) . . ? O118 Mn3 O310 90.7(11) . . ? O234 Mn3 Mn11 94.8(8) . . ? O134 Mn3 Mn11 138.5(5) . . ? O311 Mn3 Mn11 41.6(8) . . ? O123 Mn3 Mn11 140.8(10) . . ? O118 Mn3 Mn11 86.7(7) . . ? O310 Mn3 Mn11 44.9(5) . . ? O234 Mn3 Mn2 43.4(5) . . ? O134 Mn3 Mn2 83.7(10) . . ? O311 Mn3 Mn2 129.1(12) . . ? O123 Mn3 Mn2 41.1(11) . . ? O118 Mn3 Mn2 136.4(6) . . ? O310 Mn3 Mn2 86.4(8) . . ? Mn11 Mn3 Mn2 119.2(4) . . ? O234 Mn3 Mn4 38.8(9) . . ? O134 Mn3 Mn4 40.5(12) . . ? O311 Mn3 Mn4 86.0(5) . . ? O123 Mn3 Mn4 85.1(5) . . ? O118 Mn3 Mn4 139.4(10) . . ? O310 Mn3 Mn4 129.7(10) . . ? Mn11 Mn3 Mn4 117.1(3) . . ? Mn2 Mn3 Mn4 62.00(19) . . ? O234 Mn3 Mn1 81.4(8) . . ? O134 Mn3 Mn1 39.4(5) . . ? O311 Mn3 Mn1 136.1(8) . . ? O123 Mn3 Mn1 40.5(9) . . ? O118 Mn3 Mn1 97.0(8) . . ? O310 Mn3 Mn1 136.2(5) . . ? Mn11 Mn3 Mn1 175.9(3) . . ? Mn2 Mn3 Mn1 58.8(2) . . ? Mn4 Mn3 Mn1 58.90(17) . . ? O234 Mn4 O134 76.9(12) . . ? O234 Mn4 O112 98.4(14) . . ? O134 Mn4 O112 175.0(13) . . ? O234 Mn4 O405 102.2(8) . . ? O134 Mn4 O405 89.3(11) . . ? O112 Mn4 O405 93.5(12) . . ? O234 Mn4 O124 81.8(8) . . ? O134 Mn4 O124 81.8(10) . . ? O112 Mn4 O124 95.8(11) . . ? O405 Mn4 O124 169.2(18) . . ? O234 Mn4 O406 170.4(14) . . ? O134 Mn4 O406 94.0(15) . . ? O112 Mn4 O406 90.5(11) . . ? O405 Mn4 O406 80.6(10) . . ? O124 Mn4 O406 93.9(9) . . ? O234 Mn4 Mn3 37.4(11) . . ? O134 Mn4 Mn3 40.4(10) . . ? O112 Mn4 Mn3 135.2(9) . . ? O405 Mn4 Mn3 91.7(5) . . ? O124 Mn4 Mn3 85.5(4) . . ? O406 Mn4 Mn3 134.1(10) . . ? O234 Mn4 Mn1 83.7(8) . . ? O134 Mn4 Mn1 42.1(5) . . ? O112 Mn4 Mn1 136.3(5) . . ? O405 Mn4 Mn1 129.0(12) . . ? O124 Mn4 Mn1 40.9(10) . . ? O406 Mn4 Mn1 87.4(7) . . ? Mn3 Mn4 Mn1 62.75(17) . . ? O234 Mn4 Mn5 144.9(5) . . ? O134 Mn4 Mn5 98.6(10) . . ? O112 Mn4 Mn5 86.3(8) . . ? O405 Mn4 Mn5 42.6(7) . . ? O124 Mn4 Mn5 132.6(8) . . ? O406 Mn4 Mn5 38.8(5) . . ? Mn3 Mn4 Mn5 124.6(3) . . ? Mn1 Mn4 Mn5 116.5(4) . . ? O234 Mn4 Mn2 41.5(4) . . ? O134 Mn4 Mn2 81.2(9) . . ? O112 Mn4 Mn2 94.1(8) . . ? O405 Mn4 Mn2 143.7(7) . . ? O124 Mn4 Mn2 40.8(8) . . ? O406 Mn4 Mn2 134.7(5) . . ? Mn3 Mn4 Mn2 58.95(18) . . ? Mn1 Mn4 Mn2 59.1(2) . . ? Mn5 Mn4 Mn2 173.4(3) . . ? O406 Mn5 O211 177.4(8) . . ? O406 Mn5 O405 83.3(9) . . ? O211 Mn5 O405 94.1(8) . . ? O406 Mn5 O19 92.4(14) . . ? O211 Mn5 O19 87.4(14) . . ? O405 Mn5 O19 97.6(12) . . ? O406 Mn5 O110 92.5(7) . . ? O211 Mn5 O110 90.1(7) . . ? O405 Mn5 O110 169.1(17) . . ? O19 Mn5 O110 92.6(15) . . ? O406 Mn5 O212 90.9(14) . . ? O211 Mn5 O212 89.2(14) . . ? O405 Mn5 O212 78.1(13) . . ? O19 Mn5 O212 174.3(8) . . ? O110 Mn5 O212 92.0(14) . . ? O406 Mn5 Mn4 43.4(9) . . ? O211 Mn5 Mn4 134.1(9) . . ? O405 Mn5 Mn4 40.8(5) . . ? O19 Mn5 Mn4 103.4(6) . . ? O110 Mn5 Mn4 132.7(6) . . ? O212 Mn5 Mn4 75.9(6) . . ? O406 Mn6 O18 174.4(7) . . ? O406 Mn6 O107 96.0(9) . . ? O18 Mn6 O107 89.6(9) . . ? O406 Mn6 O210 87.5(10) . . ? O18 Mn6 O210 86.8(10) . . ? O107 Mn6 O210 174.4(8) . . ? O406 Mn6 O29 86.5(12) . . ? O18 Mn6 O29 92.7(12) . . ? O107 Mn6 O29 98.6(11) . . ? O210 Mn6 O29 85.8(12) . . ? O406 Mn6 O6 84.7(13) . . ? O18 Mn6 O6 94.9(10) . . ? O107 Mn6 O6 94.4(12) . . ? O210 Mn6 O6 81.7(13) . . ? O29 Mn6 O6 164.9(8) . . ? O108 Mn7 O28 176.3(9) . . ? O108 Mn7 O107 84.2(9) . . ? O28 Mn7 O107 92.8(10) . . ? O108 Mn7 O15 96.3(9) . . ? O28 Mn7 O15 86.2(9) . . ? O107 Mn7 O15 167.3(13) . . ? O108 Mn7 O16 99.5(12) . . ? O28 Mn7 O16 83.2(11) . . ? O107 Mn7 O16 102.3(10) . . ? O15 Mn7 O16 90.2(9) . . ? O108 Mn7 O27 86.4(10) . . ? O28 Mn7 O27 91.2(12) . . ? O107 Mn7 O27 86.0(9) . . ? O15 Mn7 O27 81.4(9) . . ? O16 Mn7 O27 170.2(8) . . ? O108 Mn7 Mn1 41.9(5) . . ? O28 Mn7 Mn1 134.7(6) . . ? O107 Mn7 Mn1 43.4(7) . . ? O15 Mn7 Mn1 133.5(6) . . ? O16 Mn7 Mn1 112.3(8) . . ? O27 Mn7 Mn1 77.3(6) . . ? O108 Mn8 O13 172.0(8) . . ? O108 Mn8 O208 97.6(11) . . ? O13 Mn8 O208 85.8(13) . . ? O108 Mn8 O25 88.7(12) . . ? O13 Mn8 O25 88.0(11) . . ? O208 Mn8 O25 173.7(12) . . ? O108 Mn8 O14 92.9(10) . . ? O13 Mn8 O14 94.2(11) . . ? O208 Mn8 O14 92.0(8) . . ? O25 Mn8 O14 86.9(8) . . ? O108 Mn8 O26 92.4(10) . . ? O13 Mn8 O26 80.2(11) . . ? O208 Mn8 O26 91.3(10) . . ? O25 Mn8 O26 89.2(9) . . ? O14 Mn8 O26 173.3(10) . . ? O208 Mn9 O209 81.0(9) . . ? O208 Mn9 O114 176.2(10) . . ? O209 Mn9 O114 96.7(9) . . ? O208 Mn9 O23 93.8(9) . . ? O209 Mn9 O23 173.4(6) . . ? O114 Mn9 O23 88.3(9) . . ? O208 Mn9 O24 94.1(12) . . ? O209 Mn9 O24 91.9(10) . . ? O114 Mn9 O24 89.0(9) . . ? O23 Mn9 O24 92.6(10) . . ? O208 Mn9 O215 82.7(11) . . ? O209 Mn9 O215 88.2(9) . . ? O114 Mn9 O215 94.3(11) . . ? O23 Mn9 O215 87.0(10) . . ? O24 Mn9 O215 176.7(10) . . ? O208 Mn9 Mn2 41.4(5) . . ? O209 Mn9 Mn2 40.4(7) . . ? O114 Mn9 Mn2 135.8(4) . . ? O23 Mn9 Mn2 133.7(6) . . ? O24 Mn9 Mn2 100.3(7) . . ? O215 Mn9 Mn2 77.7(6) . . ? O310 Mn10 O209 93.9(11) . . ? O310 Mn10 O117 90.4(10) . . ? O209 Mn10 O117 171.2(7) . . ? O310 Mn10 O214 176.3(6) . . ? O209 Mn10 O214 89.8(11) . . ? O117 Mn10 O214 85.9(10) . . ? O310 Mn10 O116 93.2(11) . . ? O209 Mn10 O116 99.1(9) . . ? O117 Mn10 O116 88.4(10) . . ? O214 Mn10 O116 86.2(11) . . ? O310 Mn10 O10 90.5(13) . . ? O209 Mn10 O10 90.5(9) . . ? O117 Mn10 O10 81.7(9) . . ? O214 Mn10 O10 89.5(11) . . ? O116 Mn10 O10 169.4(9) . . ? O311 Mn11 O217 177.3(12) . . ? O311 Mn11 O310 86.9(9) . . ? O217 Mn11 O310 91.6(8) . . ? O311 Mn11 O213 94.4(8) . . ? O217 Mn11 O213 87.1(8) . . ? O310 Mn11 O213 178.5(14) . . ? O311 Mn11 O216 88.9(12) . . ? O217 Mn11 O216 93.4(12) . . ? O310 Mn11 O216 93.5(12) . . ? O213 Mn11 O216 85.9(11) . . ? O311 Mn11 O218 87.4(13) . . ? O217 Mn11 O218 90.2(11) . . ? O310 Mn11 O218 85.4(12) . . ? O213 Mn11 O218 95.3(11) . . ? O216 Mn11 O218 176.3(9) . . ? O311 Mn11 Mn3 42.1(5) . . ? O217 Mn11 Mn3 135.9(5) . . ? O310 Mn11 Mn3 45.6(9) . . ? O213 Mn11 Mn3 135.8(8) . . ? O216 Mn11 Mn3 98.3(7) . . ? O218 Mn11 Mn3 78.4(6) . . ? O113 Mn12 O311 89.8(7) . . ? O113 Mn12 O111 85.9(8) . . ? O311 Mn12 O111 173.5(15) . . ? O113 Mn12 O405 173.2(12) . . ? O311 Mn12 O405 94.6(8) . . ? O111 Mn12 O405 89.2(8) . . ? O113 Mn12 O121 96.2(13) . . ? O311 Mn12 O121 90.2(14) . . ? O111 Mn12 O121 95.1(16) . . ? O405 Mn12 O121 89.1(13) . . ? O113 Mn12 O120 90.5(12) . . ? O311 Mn12 O120 90.2(15) . . ? O111 Mn12 O120 85.0(16) . . ? O405 Mn12 O120 84.2(14) . . ? O121 Mn12 O120 173.3(7) . . ? Mn6 O107 Mn1 129.7(17) . . ? Mn6 O107 Mn7 124.6(8) . . ? Mn1 O107 Mn7 92.1(8) . . ? Mn1 O108 Mn8 131.5(19) . . ? Mn1 O108 Mn7 95.5(11) . . ? Mn8 O108 Mn7 122.4(7) . . ? Mn2 O123 Mn3 97.4(13) . . ? Mn2 O123 Mn1 95.9(7) . . ? Mn3 O123 Mn1 100.5(11) . . ? Mn1 O124 Mn2 97.0(7) . . ? Mn1 O124 Mn4 96.0(13) . . ? Mn2 O124 Mn4 97.5(9) . . ? Mn3 O134 Mn4 99(2) . . ? Mn3 O134 Mn1 102.8(11) . . ? Mn4 O134 Mn1 97.5(12) . . ? Mn2 O208 Mn9 96.5(10) . . ? Mn2 O208 Mn8 130(2) . . ? Mn9 O208 Mn8 125.3(8) . . ? Mn2 O209 Mn10 133.4(13) . . ? Mn2 O209 Mn9 96.0(7) . . ? Mn10 O209 Mn9 129.3(10) . . ? Mn3 O234 Mn4 103.8(19) . . ? Mn3 O234 Mn2 98.3(9) . . ? Mn4 O234 Mn2 100.4(7) . . ? Mn10 O310 Mn11 126.7(19) . . ? Mn10 O310 Mn3 134.2(9) . . ? Mn11 O310 Mn3 89.5(11) . . ? Mn11 O311 Mn3 96.3(10) . . ? Mn11 O311 Mn12 131.9(12) . . ? Mn3 O311 Mn12 131.2(12) . . ? Mn4 O405 Mn12 128.7(9) . . ? Mn4 O405 Mn5 96.6(8) . . ? Mn12 O405 Mn5 128.5(17) . . ? Mn5 O406 Mn6 130.7(18) . . ? Mn5 O406 Mn4 97.8(10) . . ? Mn6 O406 Mn4 129.6(8) . . ? C13 O13 Mn8 134.9(17) . . ? C13 O23 Mn9 131.7(16) . . ? O23 C13 O13 123.3(14) . . ? O23 C13 C231 124(6) . . ? O13 C13 C231 104(6) . . ? O23 C13 C23 114(2) . . ? O13 C13 C23 122(2) . . ? C231 C13 C23 25(5) . . ? C33 C23 C13 116(2) . . ? C23 C33 C43 109.6(11) . . ? C23 C33 C63 110.2(12) . . ? C43 C33 C63 109.4(12) . . ? C23 C33 C53 108.6(11) . . ? C43 C33 C53 109.7(12) . . ? C63 C33 C53 109.4(12) . . ? C331 C231 C13 102(6) . . ? C431 C331 C231 109.7(12) . . ? C431 C331 C631 109.5(12) . . ? C231 C331 C631 109.4(12) . . ? C431 C331 C531 109.3(12) . . ? C231 C331 C531 109.4(12) . . ? C631 C331 C531 109.5(12) . . ? C14 O14 Mn8 135.2(13) . . ? C14 O24 Mn9 132.4(12) . . ? O24 C14 O14 122.5(12) . . ? O24 C14 C24 120.2(12) . . ? O14 C14 C24 116.8(12) . . ? C14 C24 C34 117.2(11) . . ? C24 C34 C64 109.1(10) . . ? C24 C34 C44 110.0(10) . . ? C64 C34 C44 109.1(9) . . ? C24 C34 C54 111.7(10) . . ? C64 C34 C54 108.6(8) . . ? C44 C34 C54 108.3(8) . . ? C15 O15 Mn7 124.1(15) . . ? C15 O25 Mn8 142.0(14) . . ? O25 C15 O15 123.1(14) . . ? O25 C15 C251 100(3) . . ? O15 C15 C251 137(3) . . ? O25 C15 C25 139(3) . . ? O15 C15 C25 90(2) . . ? C251 C15 C25 55(3) . . ? C35 C25 C15 115(3) . . ? C25 C35 C45 109.7(12) . . ? C25 C35 C65 109.6(12) . . ? C45 C35 C65 109.6(12) . . ? C25 C35 C55 109.3(12) . . ? C45 C35 C55 109.6(12) . . ? C65 C35 C55 109.2(12) . . ? C15 C251 C351 108.4(19) . . ? C451 C351 C551 110.9(13) . . ? C451 C351 C251 109.1(12) . . ? C551 C351 C251 110.0(13) . . ? C451 C351 C651 109.4(13) . . ? C551 C351 C651 108.3(12) . . ? C251 C351 C651 109.1(12) . . ? C16 O16 Mn7 130.5(13) . . ? C16 O26 Mn8 128.3(19) . . ? O26 C16 O16 124.2(12) . . ? O26 C16 C26 119.1(12) . . ? O16 C16 C26 116.5(11) . . ? C16 C26 C36 128.9(18) . . ? C16 C26 C361 122.1(16) . . ? C36 C26 C361 38.7(7) . . ? C56 C36 C26 109.7(8) . . ? C56 C36 C46 109.7(10) . . ? C26 C36 C46 109.3(7) . . ? C56 C36 C66 109.8(11) . . ? C26 C36 C66 109.0(8) . . ? C46 C36 C66 109.2(11) . . ? C46 C361 C56 109.8(10) . . ? C46 C361 C26 109.4(7) . . ? C56 C361 C26 109.5(8) . . ? C46 C361 C661 109.5(11) . . ? C56 C361 C661 109.6(11) . . ? C26 C361 C661 109.0(7) . . ? C361 C46 C36 38.7(7) . . ? C36 C56 C361 38.7(7) . . ? C17 O17 Mn1 126.8(12) . . ? C17 O27 Mn7 124.4(15) . . ? O27 C17 O17 123.5(12) . . ? O27 C17 C27 120.1(12) . . ? O17 C17 C27 116.4(11) . . ? C17 C27 C37 115.0(11) . . ? C27 C37 C67 108.5(10) . . ? C27 C37 C57 112.1(10) . . ? C67 C37 C57 109.3(9) . . ? C27 C37 C47 109.5(11) . . ? C67 C37 C47 109.0(9) . . ? C57 C37 C47 108.4(9) . . ? C18 O18 Mn6 138.7(14) . . ? C18 O28 Mn7 127.5(15) . . ? O28 C18 O18 123.3(13) . . ? O28 C18 C28 119.8(12) . . ? O18 C18 C28 116.6(11) . . ? C18 C28 C38 115.2(11) . . ? C28 C38 C48 110.0(10) . . ? C28 C38 C68 108.4(10) . . ? C48 C38 C68 109.1(9) . . ? C28 C38 C58 112.0(11) . . ? C48 C38 C58 108.5(9) . . ? C68 C38 C58 108.9(9) . . ? C19 O19 Mn5 119.9(12) . . ? C19 O29 Mn6 135.4(16) . . ? O29 C19 O19 124.3(12) . . ? O29 C19 C29 119.3(12) . . ? O19 C19 C29 116.5(11) . . ? C19 C29 C39 114.1(11) . . ? C29 C39 C49 109.6(11) . . ? C29 C39 C69 108.0(11) . . ? C49 C39 C69 109.3(9) . . ? C29 C39 C59 112.0(11) . . ? C49 C39 C59 108.9(9) . . ? C69 C39 C59 109.1(9) . . ? C110 O110 Mn5 125.6(17) . . ? C110 O210 Mn6 134.3(13) . . ? O210 C110 O110 123.1(13) . . ? O210 C110 C210 118.6(13) . . ? O110 C110 C210 115.9(13) . . ? C110 C210 C310 137(4) . . ? C110 C210 C320 135(4) . . ? C310 C210 C320 88(3) . . ? C210 C310 C610 109.5(7) . . ? C210 C310 C510 109.6(7) . . ? C610 C310 C510 109.5(7) . . ? C210 C310 C410 109.5(7) . . ? C610 C310 C410 109.4(7) . . ? C510 C310 C410 109.3(7) . . ? C210 C320 C720 109.6(7) . . ? C210 C320 C620 109.6(7) . . ? C720 C320 C620 0(10) . . ? C210 C320 C520 109.5(7) . . ? C720 C320 C520 110(10) . . ? C620 C320 C520 109.5(7) . . ? C210 C320 C920 109.5(7) . . ? C720 C320 C920 109.5(7) . . ? C620 C320 C920 109(10) . . ? C520 C320 C920 0(10) . . ? C210 C320 C420 109.4(7) . . ? C720 C320 C420 109(10) . . ? C620 C320 C420 109.4(7) . . ? C520 C320 C420 109.4(7) . . ? C920 C320 C420 109(10) . . ? C210 C320 C820 109.4(7) . . ? C720 C320 C820 109.4(7) . . ? C620 C320 C820 109(10) . . ? C520 C320 C820 109(10) . . ? C920 C320 C820 109.4(7) . . ? C420 C320 C820 0(10) . . ? C111 O111 Mn12 139.6(12) . . ? C111 O211 Mn5 135.0(12) . . ? O211 C111 O111 123.2(13) . . ? O211 C111 C211 119.8(11) . . ? O111 C111 C211 115.9(11) . . ? C111 C211 C311 115.3(12) . . ? C211 C311 C511 112.6(11) . . ? C211 C311 C611 108.6(11) . . ? C511 C311 C611 109.0(9) . . ? C211 C311 C411 108.9(10) . . ? C511 C311 C411 109.0(9) . . ? C611 C311 C411 108.7(9) . . ? C112 O112 Mn4 126.6(15) . . ? C112 O212 Mn5 125.3(14) . . ? O212 C112 O112 123.2(13) . . ? O212 C112 C212 119.2(11) . . ? O112 C112 C212 116.5(12) . . ? C112 C212 C312 114.5(10) . . ? C212 C312 C622 110.3(7) . . ? C212 C312 C612 110.0(7) . . ? C622 C312 C612 124(5) . . ? C212 C312 C422 110.0(7) . . ? C622 C312 C422 109.3(7) . . ? C612 C312 C422 19(7) . . ? C212 C312 C412 109.9(7) . . ? C622 C312 C412 19(7) . . ? C612 C312 C412 109.1(7) . . ? C422 C312 C412 92(7) . . ? C212 C312 C512 109.9(7) . . ? C622 C312 C512 92(7) . . ? C612 C312 C512 109.0(7) . . ? C422 C312 C512 124(5) . . ? C412 C312 C512 109.0(7) . . ? C212 C312 C522 109.5(7) . . ? C622 C312 C522 109.0(7) . . ? C612 C312 C522 92(7) . . ? C422 C312 C522 108.7(7) . . ? C412 C312 C522 125(5) . . ? C512 C312 C522 19(7) . . ? C113 O113 Mn12 134.2(16) . . ? C113 O213 Mn11 131.5(15) . . ? O213 C113 O113 124.0(12) . . ? O213 C113 C213 119.2(12) . . ? O113 C113 C213 116.5(11) . . ? C113 C213 C313 115.1(11) . . ? C213 C313 C513 112.5(11) . . ? C213 C313 C413 109.9(11) . . ? C513 C313 C413 108.5(9) . . ? C213 C313 C613 108.2(11) . . ? C513 C313 C613 108.9(9) . . ? C413 C313 C613 108.8(9) . . ? C114 O114 Mn9 131.3(11) . . ? C114 O214 Mn10 138.3(15) . . ? O214 C114 O114 124.1(12) . . ? O214 C114 C214 118.7(11) . . ? O114 C114 C214 117.2(11) . . ? C114 C214 C314 114.4(11) . . ? C214 C314 C514 112.2(10) . . ? C214 C314 C414 109.1(10) . . ? C514 C314 C414 109.6(9) . . ? C214 C314 C614 108.5(10) . . ? C514 C314 C614 109.0(8) . . ? C414 C314 C614 108.5(9) . . ? C115 O115 Mn2 128.0(12) . . ? C115 O215 Mn9 123.4(15) . . ? O215 C115 O115 123.2(12) . . ? O215 C115 C215 119.9(12) . . ? O115 C115 C215 116.8(11) . . ? C115 C215 C315 115.5(11) . . ? C215 C315 C615 108.6(11) . . ? C215 C315 C515 111.9(11) . . ? C615 C315 C515 109.2(9) . . ? C215 C315 C415 109.3(10) . . ? C615 C315 C415 109.0(9) . . ? C515 C315 C415 108.9(9) . . ? C116 O116 Mn10 126(2) . . ? C116 O216 Mn11 126.8(16) . . ? O216 C116 O116 122.7(13) . . ? O216 C116 C216 118.6(12) . . ? O116 C116 C216 116.0(12) . . ? C116 C216 C316 114.1(11) . . ? C216 C316 C516 112.2(11) . . ? C216 C316 C416 109.0(11) . . ? C516 C316 C416 109.2(9) . . ? C216 C316 C616 107.8(11) . . ? C516 C316 C616 109.1(9) . . ? C416 C316 C616 109.5(9) . . ? C117 O117 Mn10 131.7(11) . . ? C117 O217 Mn11 135.7(12) . . ? O217 C117 O117 124.0(11) . . ? O217 C117 C217 119.1(11) . . ? O117 C117 C217 116.9(11) . . ? C117 C217 C317 114.5(11) . . ? C217 C317 C417 109.0(10) . . ? C217 C317 C617 108.6(11) . . ? C417 C317 C617 109.0(9) . . ? C217 C317 C517 111.7(11) . . ? C417 C317 C517 109.5(9) . . ? C617 C317 C517 109.0(9) . . ? C118 O118 Mn3 128(2) . . ? C118 O218 Mn11 124.5(15) . . ? O218 C118 O118 122.3(15) . . ? O218 C118 C228 112(3) . . ? O118 C118 C228 125(3) . . ? O218 C118 C218 126(3) . . ? O118 C118 C218 112(3) . . ? C228 C118 C218 14(3) . . ? C318 C218 C118 106(3) . . ? C218 C318 C418 109.6(12) . . ? C218 C318 C618 109.8(12) . . ? C418 C318 C618 109.6(12) . . ? C218 C318 C518 108.8(12) . . ? C418 C318 C518 109.5(12) . . ? C618 C318 C518 109.6(12) . . ? C118 C228 C328 122(4) . . ? C628 C328 C228 109.7(12) . . ? C628 C328 C528 109.8(12) . . ? C228 C328 C528 109.2(12) . . ? C628 C328 C428 109.5(12) . . ? C228 C328 C428 109.4(12) . . ? C528 C328 C428 109.3(12) . . ? _diffrn_measured_fraction_theta_max 0.306 _diffrn_reflns_theta_full 13.54 _diffrn_measured_fraction_theta_full 0.306 _refine_diff_density_max 0.489 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.077 data_mnjt12 #TrackingRef 'all_revised.cif' _database_code_depnum_ccdc_archive 'CCDC 755029' #Crystal at RT and ambient pressure AFTER compression to 1.5 GPa. _audit_creation_method SHELXL-97 _audit_creation_date 09-11-09 _chemical_compound_source 'Pascal Parois & Mark Murrie ' _exptl_crystal_recrystallization_method ; >From MeNO2 and CH2Cl2 Crystal at RT and ambient pressure AFTER compression to 1.5 GPa. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn12O12(tBuCH2CO2)16(H2O)4].2MeNO2' _chemical_formula_sum 'C98 H189 Cl2 Mn12 N O50' _chemical_formula_weight 2911.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0005 0.0007 '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 0.0015 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0034 0.0025 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.2230 0.3472 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.0750 0.0720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.0888(10) _cell_length_b 16.6899(10) _cell_length_c 27.5390(17) _cell_angle_alpha 76.5270(10) _cell_angle_beta 78.0850(10) _cell_angle_gamma 77.7050(10) _cell_volume 6930.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9939 _cell_measurement_theta_min 2 _cell_measurement_theta_max 17 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3036 _exptl_absorpt_coefficient_mu 0.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5986 _exptl_absorpt_correction_T_max 0.7441 _exptl_absorpt_process_details Sadabs _exptl_special_details ; On Station 9.8 at Daresbury. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.47800 _diffrn_radiation_type ? _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 68385 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 17.26 _reflns_number_total 27186 _reflns_number_gt 16773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex' _computing_cell_refinement 'Bruker Saint' _computing_data_reduction 'Bruker Saint' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.000 0.500 0.000 22 1 ' ' 2 0.204 0.706 0.355 136 42 ' ' 3 -0.204 0.295 0.645 137 42 ' ' 4 0.187 0.963 -0.001 51 13 ' ' 5 0.444 0.634 0.468 21 6 ' ' 6 0.556 0.366 0.532 21 6 ' ' 7 0.813 0.037 1.001 51 13 ' ' _platon_squeeze_details ; ; _refine_special_details ; Data set taken after compression. CH2tBu ligands #5, 8 and 17 are disordered. #5 and 8 have the entire CH2tBu group in two orientations. in #17 the tBu group is in two positions. Occupancies were refined. In the case of ligand #17, where the disorder components are in the occupancy ratio ~80:20, the minor component atoms were refined with a common U[iso]. All carboxylate ligands were restrained to have similar bond distances and angles. The tBu groups were restrained to have local 3-fold symmetry. The displacement ellipsoids of the CH2tBu groups vary between 0.054 (C38) and 0.310 (C65'). and only the Mn and O atoms were refined with adps. The aim of this experiment wass to determine the coordination geometry about Mn8 after compression. Checkcif output: 201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 96 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.75 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.44 Ratio 220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.86 Ratio 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbours of N1A See comments above. 241_ALERT_2_A Check High Ueq as Compared to Neighbors for C212 241_ALERT_2_B Check High Ueq as Compared to Neighbors for C29 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O13 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O14 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O18 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O25 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O26 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O111 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O210 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O214 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C216 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C218 These are either O-atoms attached to Mn: even the O-atoms qhow quite high thermal motion in this structure. C2xx are 'pivot' CH2 groups. These will tend to show higher thermal motion than the attached O-atoms or the pivit C atoms of the tBu groups. 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C33 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C35' 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C38 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C39 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C312 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C316 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C318 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C38' 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C34 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C36 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C37 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C310 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C311 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C313 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C314 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C315 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C317 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn6 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn8 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn10 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn12 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C13 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C14 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C112 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C217 C3xx are pivot atoms of tBu groups. 420_ALERT_2_B D-H Without Acceptor O10 - H101 ... ? 420_ALERT_2_B D-H Without Acceptor O120 - H121 ... ? 420_ALERT_2_B D-H Without Acceptor O121 - *H124 ... ? 420_ALERT_2_B D-H Without Acceptor O121 - *H125 ... ? Noted, but no action taken. The H-positions on oxygen are based on those from the LT (150K) structure. 601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 134.00 A**3 See above. 910_ALERT_3_B Missing # of FCF Reflections Below Th(Min) ..... 15 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 207 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 54 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 315 Very low angle data were omitted to avoid beam-stop problems. #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 13.83 0.500 0.986 14516 14315 201 15.24 0.550 0.989 19325 19119 206 16.67 0.600 0.991 25090 24868 222 #----------------------------------------------------------- ACTA Min. Res. --- 17.26 0.621 0.981 27723 27186 537 084_ALERT_2_C High R2 Value .................................. 0.27 232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn8 -- O14 .. 5.32 su 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 12 Not a precise structure. This is becuase of the high thermal motion. 432_ALERT_2_C Short Inter X...Y Contact C43 .. C58' .. 3.14 Ang. C58' is disordered, and C43 has quite a high thermal parameter, and may be disordered in sympathy with C58'. If present this disorder has not be resolved. 301_ALERT_3_G Note Main Residue Disorder .................... 8.00 Perc. See above. 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? No action taken. 041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? 043_ALERT_1_C Check Reported Molecular Weight ................ 2887.80 044_ALERT_1_C Calculated and Reported Dx Differ .............. ? The caluclated values assume one extra MeNO2 per formula unit. 731_ALERT_1_C Bond Calc 1.517(15), Rep 1.518(7) ...... 2.14 su-Ra C33 -C63 1.555 1.555 731_ALERT_1_C Bond Calc 1.520(17), Rep 1.518(7) ...... 2.43 su-Ra C33 -C53 1.555 1.555 731_ALERT_1_C Bond Calc 1.506(13), Rep 1.505(6) ...... 2.17 su-Ra C36 -C56 1.555 1.555 731_ALERT_1_C Bond Calc 1.499(14), Rep 1.499(6) ...... 2.33 su-Ra C39 -C59 1.555 1.555 731_ALERT_1_C Bond Calc 1.510(14), Rep 1.509(6) ...... 2.33 su-Ra C39 -C49 1.555 1.555 731_ALERT_1_C Bond Calc 1.529(16), Rep 1.529(7) ...... 2.29 su-Ra C39 -C69 1.555 1.555 731_ALERT_1_C Bond Calc 1.511(16), Rep 1.511(7) ...... 2.29 su-Ra C310 -C510 1.555 1.555 731_ALERT_1_C Bond Calc 1.510(15), Rep 1.510(7) ...... 2.14 su-Ra C310 -C410 1.555 1.555 731_ALERT_1_C Bond Calc 1.522(16), Rep 1.522(7) ...... 2.29 su-Ra C310 -C610 1.555 1.555 731_ALERT_1_C Bond Calc 1.506(16), Rep 1.505(7) ...... 2.29 su-Ra C312 -C412 1.555 1.555 731_ALERT_1_C Bond Calc 1.511(14), Rep 1.511(6) ...... 2.33 su-Ra C312 -C612 1.555 1.555 731_ALERT_1_C Bond Calc 1.511(16), Rep 1.511(7) ...... 2.29 su-Ra C312 -C512 1.555 1.555 731_ALERT_1_C Bond Calc 1.510(14), Rep 1.510(6) ...... 2.33 su-Ra C313 -C513 1.555 1.555 731_ALERT_1_C Bond Calc 1.528(13), Rep 1.526(6) ...... 2.17 su-Ra C314 -C514 1.555 1.555 731_ALERT_1_C Bond Calc 1.503(13), Rep 1.503(6) ...... 2.17 su-Ra C315 -C415 1.555 1.555 731_ALERT_1_C Bond Calc 1.512(14), Rep 1.512(6) ...... 2.33 su-Ra C316 -C516 1.555 1.555 731_ALERT_1_C Bond Calc 1.509(16), Rep 1.508(7) ...... 2.29 su-Ra C318 -C618 1.555 1.555 731_ALERT_1_C Bond Calc 1.513(17), Rep 1.513(7) ...... 2.43 su-Ra C318 -C518 1.555 1.555 731_ALERT_1_C Bond Calc 1.517(14), Rep 1.516(6) ...... 2.33 su-Ra C318 -C418 1.555 1.555 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 4866 The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif can be badly in error. 926_ALERT_1_C Reported and Calculated R1 * 100.0 Differ by . -0.26 Suspect this is because calculation in Platon used all data. Very low angle data were omitted from refinement to avoid beam-stop problems. 092_ALERT_4_G Check: Wavelength given is not Cu,Mo or Ag Ka .. 0.48 Ang. Synchrotron data. 154_ALERT_1_G The su's on the Cell Angles are Equal (x 10000) 100 Deg. 180_ALERT_4_G Check Cell Rounding: # of Values Ending with 0 = 4 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 3 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 42.60 Deg. C25 -C15 -C25' 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 31.20 Deg. C327 -C217 -C317 1.555 1.555 1.555 795_ALERT_4_G C-Atom in CIF Coordinate List out of Sequence .. C14 796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence .. O107 No action taken. ; _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^)+(0.1628P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 27186 _refine_ls_number_parameters 997 _refine_ls_number_restraints 4866 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.2745 _refine_ls_wR_factor_gt 0.2531 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.004 _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 0.41823(5) 0.19950(5) 0.23192(3) 0.0376(2) Uani 1 1 d . . . Mn2 Mn 0.29835(5) 0.08715(5) 0.26228(3) 0.0383(2) Uani 1 1 d . . . Mn3 Mn 0.25333(5) 0.23851(5) 0.19414(3) 0.0375(2) Uani 1 1 d . . . Mn4 Mn 0.25959(5) 0.24960(6) 0.29351(3) 0.0408(2) Uani 1 1 d . . . Mn5 Mn 0.23519(6) 0.40288(7) 0.32355(4) 0.0552(3) Uani 1 1 d . . . Mn6 Mn 0.43588(6) 0.29973(7) 0.32405(4) 0.0563(3) Uani 1 1 d . . . Mn7 Mn 0.57961(6) 0.16114(6) 0.26066(4) 0.0477(2) Uani 1 1 d . . . Mn8 Mn 0.51417(6) -0.00984(6) 0.24784(4) 0.0494(2) Uani 1 1 d . . . Mn9 Mn 0.33207(6) -0.06959(6) 0.23828(4) 0.0476(2) Uani 1 1 d . . . Mn10 Mn 0.18002(6) 0.07008(6) 0.17610(3) 0.0439(2) Uani 1 1 d . . . Mn11 Mn 0.09356(6) 0.27165(6) 0.16256(3) 0.0440(2) Uani 1 1 d . . . Mn12 Mn 0.11499(6) 0.40407(6) 0.23451(4) 0.0516(3) Uani 1 1 d . . . O6 O 0.4198(4) 0.1802(4) 0.3817(2) 0.0934(19) Uani 1 1 d . . . H61 H 0.4720 0.1509 0.3803 0.140 Uiso 1 1 d R . . H62 H 0.3881 0.1604 0.3713 0.140 Uiso 1 1 d R . . O10 O 0.2947(4) 0.0599(4) 0.11300(19) 0.097(2) Uani 1 1 d . . . H101 H 0.3054 0.1087 0.1111 0.146 Uiso 1 1 d R . . H102 H 0.3363 0.0267 0.1252 0.146 Uiso 1 1 d R . . O120 O 0.0061(3) 0.3404(4) 0.2813(2) 0.0750(14) Uani 1 1 d . . . H120 H 0.0014 0.2972 0.2712 0.113 Uiso 1 1 d R . . H121 H 0.0248 0.3217 0.3090 0.113 Uiso 1 1 d R . . O121 O 0.2206(4) 0.4710(4) 0.1893(2) 0.0887(18) Uani 1 1 d . . . H123 H 0.2590 0.4857 0.2042 0.133 Uiso 1 1 d R . . H124 H 0.2588 0.4322 0.1724 0.133 Uiso 0.50 1 d PR . . H125 H 0.1927 0.5000 0.1765 0.133 Uiso 0.50 1 d PR . . O107 O 0.4768(2) 0.2415(3) 0.27032(15) 0.0456(9) Uani 1 1 d . . . O108 O 0.5082(2) 0.1098(3) 0.23641(15) 0.0448(9) Uani 1 1 d . . . O123 O 0.3502(2) 0.1511(2) 0.20023(13) 0.0361(8) Uani 1 1 d . . . O124 O 0.3487(2) 0.1530(2) 0.29312(13) 0.0393(8) Uani 1 1 d . . . O134 O 0.3180(2) 0.2862(2) 0.22744(13) 0.0382(8) Uani 1 1 d . . . O208 O 0.3888(3) -0.0026(2) 0.26191(15) 0.0448(9) Uani 1 1 d . . . O209 O 0.2521(2) 0.0314(2) 0.22557(14) 0.0424(9) Uani 1 1 d . . . O234 O 0.2112(2) 0.1864(2) 0.26080(14) 0.0397(8) Uani 1 1 d . . . O310 O 0.1896(2) 0.1831(2) 0.16755(14) 0.0413(9) Uani 1 1 d . . . O311 O 0.1539(2) 0.3200(2) 0.19727(15) 0.0445(9) Uani 1 1 d . . . O405 O 0.1819(2) 0.3519(3) 0.28530(15) 0.0476(10) Uani 1 1 d . . . O406 O 0.3190(2) 0.3061(3) 0.32158(15) 0.0490(10) Uani 1 1 d . . . O13 O 0.5315(3) -0.1342(3) 0.2584(2) 0.0851(17) Uani 1 1 d D . . O23 O 0.4085(3) -0.1739(3) 0.2575(2) 0.0678(13) Uani 1 1 d D . . C13 C 0.4850(4) -0.1880(4) 0.2636(3) 0.0664(19) Uiso 1 1 d D . . C23 C 0.5294(6) -0.2784(4) 0.2740(3) 0.102(3) Uiso 1 1 d D . . H23A H 0.4858 -0.3133 0.2799 0.123 Uiso 1 1 calc R . . H23B H 0.5688 -0.2892 0.2436 0.123 Uiso 1 1 calc R . . C33 C 0.5790(5) -0.3067(5) 0.3174(3) 0.107(3) Uiso 1 1 d D . . C43 C 0.6044(9) -0.4012(6) 0.3271(5) 0.180(6) Uiso 1 1 d D . . H43A H 0.5533 -0.4261 0.3362 0.270 Uiso 1 1 calc R . . H43B H 0.6374 -0.4192 0.3542 0.270 Uiso 1 1 calc R . . H43C H 0.6384 -0.4180 0.2970 0.270 Uiso 1 1 calc R . . C53 C 0.5247(10) -0.2802(11) 0.3650(5) 0.241(10) Uiso 1 1 d D . . H53A H 0.5112 -0.2202 0.3594 0.362 Uiso 1 1 calc R . . H53B H 0.5564 -0.3008 0.3926 0.362 Uiso 1 1 calc R . . H53C H 0.4723 -0.3027 0.3729 0.362 Uiso 1 1 calc R . . C63 C 0.6607(7) -0.2695(9) 0.3065(6) 0.185(7) Uiso 1 1 d D . . H63A H 0.6462 -0.2096 0.2993 0.278 Uiso 1 1 calc R . . H63B H 0.6983 -0.2882 0.2779 0.278 Uiso 1 1 calc R . . H63C H 0.6893 -0.2872 0.3355 0.278 Uiso 1 1 calc R . . O14 O 0.5266(3) -0.0096(4) 0.1735(2) 0.0767(15) Uani 1 1 d D . . O24 O 0.4110(3) -0.0514(3) 0.16270(16) 0.0583(11) Uani 1 1 d D . . C14 C 0.4850(3) -0.0330(4) 0.1473(2) 0.0530(15) Uiso 1 1 d D . . C24 C 0.5267(5) -0.0360(4) 0.0932(2) 0.072(2) Uiso 1 1 d D . . H24A H 0.4867 -0.0026 0.0713 0.086 Uiso 1 1 calc R . . H24B H 0.5772 -0.0095 0.0857 0.086 Uiso 1 1 calc R . . C34 C 0.5535(4) -0.1209(4) 0.0799(2) 0.072(2) Uiso 1 1 d D . . C44 C 0.6051(7) -0.1803(6) 0.1178(4) 0.126(4) Uiso 1 1 d D . . H44A H 0.5704 -0.1863 0.1508 0.190 Uiso 1 1 calc R . . H44B H 0.6554 -0.1585 0.1184 0.190 Uiso 1 1 calc R . . H44C H 0.6225 -0.2339 0.1082 0.190 Uiso 1 1 calc R . . C54 C 0.6061(6) -0.1108(6) 0.0267(3) 0.102(3) Uiso 1 1 d D . . H54A H 0.5730 -0.0708 0.0037 0.152 Uiso 1 1 calc R . . H54B H 0.6203 -0.1637 0.0162 0.152 Uiso 1 1 calc R . . H54C H 0.6582 -0.0914 0.0267 0.152 Uiso 1 1 calc R . . C64 C 0.4745(5) -0.1561(6) 0.0795(4) 0.115(3) Uiso 1 1 d D . . H64A H 0.4397 -0.1175 0.0568 0.173 Uiso 1 1 calc R . . H64B H 0.4416 -0.1647 0.1130 0.173 Uiso 1 1 calc R . . H64C H 0.4920 -0.2085 0.0684 0.173 Uiso 1 1 calc R . . O15 O 0.6857(3) 0.0860(3) 0.2440(2) 0.0699(14) Uani 1 1 d D A . O25 O 0.6445(3) -0.0267(3) 0.2336(3) 0.097(2) Uani 1 1 d D A . C15 C 0.7006(4) 0.0163(4) 0.2311(3) 0.084(2) Uiso 1 1 d D . . C25 C 0.7880(7) 0.0073(7) 0.1965(6) 0.083(6) Uiso 0.474(14) 1 d PD A 1 H25A H 0.7810 0.0435 0.1640 0.100 Uiso 0.474(14) 1 calc PR A 1 H25B H 0.8272 0.0289 0.2107 0.100 Uiso 0.474(14) 1 calc PR A 1 C35 C 0.8312(7) -0.0771(8) 0.1870(5) 0.106(3) Uiso 0.474(14) 1 d PD A 1 C45 C 0.7799(11) -0.1051(11) 0.1558(7) 0.093(6) Uiso 0.474(14) 1 d PD A 1 H45A H 0.8063 -0.1602 0.1501 0.140 Uiso 0.474(14) 1 calc PR A 1 H45B H 0.7787 -0.0669 0.1238 0.140 Uiso 0.474(14) 1 calc PR A 1 H45C H 0.7220 -0.1061 0.1735 0.140 Uiso 0.474(14) 1 calc PR A 1 C55 C 0.9220(8) -0.0737(12) 0.1584(7) 0.098(7) Uiso 0.474(14) 1 d PD A 1 H55A H 0.9531 -0.0514 0.1769 0.147 Uiso 0.474(14) 1 calc PR A 1 H55B H 0.9196 -0.0385 0.1256 0.147 Uiso 0.474(14) 1 calc PR A 1 H55C H 0.9508 -0.1291 0.1547 0.147 Uiso 0.474(14) 1 calc PR A 1 C65 C 0.8349(15) -0.1372(12) 0.2372(6) 0.145(11) Uiso 0.474(14) 1 d PD A 1 H65A H 0.8695 -0.1198 0.2561 0.217 Uiso 0.474(14) 1 calc PR A 1 H65B H 0.8600 -0.1924 0.2315 0.217 Uiso 0.474(14) 1 calc PR A 1 H65C H 0.7776 -0.1375 0.2561 0.217 Uiso 0.474(14) 1 calc PR A 1 C25' C 0.7896(6) -0.0382(8) 0.2330(5) 0.082(5) Uiso 0.526(14) 1 d PD A 2 H25C H 0.8291 -0.0045 0.2370 0.099 Uiso 0.526(14) 1 calc PR A 2 H25D H 0.7857 -0.0829 0.2626 0.099 Uiso 0.526(14) 1 calc PR A 2 C35' C 0.8265(8) -0.0761(8) 0.1870(5) 0.106(3) Uiso 0.526(14) 1 d PD A 2 C45' C 0.7825(13) -0.1488(12) 0.1887(9) 0.141(10) Uiso 0.526(14) 1 d PD A 2 H45D H 0.8064 -0.1729 0.1593 0.212 Uiso 0.526(14) 1 calc PR A 2 H45E H 0.7218 -0.1291 0.1892 0.212 Uiso 0.526(14) 1 calc PR A 2 H45F H 0.7915 -0.1903 0.2186 0.212 Uiso 0.526(14) 1 calc PR A 2 C55' C 0.9215(8) -0.1102(13) 0.1868(8) 0.118(8) Uiso 0.526(14) 1 d PD A 2 H55D H 0.9448 -0.1343 0.1573 0.177 Uiso 0.526(14) 1 calc PR A 2 H55E H 0.9288 -0.1523 0.2167 0.177 Uiso 0.526(14) 1 calc PR A 2 H55F H 0.9511 -0.0656 0.1861 0.177 Uiso 0.526(14) 1 calc PR A 2 C65' C 0.8120(19) -0.0126(15) 0.1392(7) 0.31(3) Uiso 0.526(14) 1 d PD A 2 H65D H 0.8361 -0.0379 0.1103 0.464 Uiso 0.526(14) 1 calc PR A 2 H65E H 0.8393 0.0341 0.1373 0.464 Uiso 0.526(14) 1 calc PR A 2 H65F H 0.7512 0.0063 0.1396 0.464 Uiso 0.526(14) 1 calc PR A 2 O16 O 0.5583(3) 0.0813(3) 0.33643(17) 0.0648(12) Uani 1 1 d D . . O26 O 0.5218(4) -0.0313(3) 0.32165(19) 0.0776(15) Uani 1 1 d D . . C16 C 0.5407(4) 0.0084(4) 0.3496(2) 0.0602(17) Uiso 1 1 d D . . C26 C 0.5439(4) -0.0347(5) 0.4043(2) 0.076(2) Uiso 1 1 d D . . H26A H 0.5063 0.0016 0.4256 0.091 Uiso 1 1 calc R . . H26B H 0.5196 -0.0853 0.4105 0.091 Uiso 1 1 calc R . . C36 C 0.6303(4) -0.0583(4) 0.4217(2) 0.075(2) Uiso 1 1 d D . . C46 C 0.6199(7) -0.1102(6) 0.4748(3) 0.116(3) Uiso 1 1 d D . . H46A H 0.5796 -0.0782 0.4970 0.174 Uiso 1 1 calc R . . H46B H 0.6747 -0.1255 0.4862 0.174 Uiso 1 1 calc R . . H46C H 0.5987 -0.1598 0.4748 0.174 Uiso 1 1 calc R . . C56 C 0.6952(6) -0.1048(7) 0.3856(4) 0.135(4) Uiso 1 1 d D . . H56A H 0.6753 -0.1542 0.3838 0.203 Uiso 1 1 calc R . . H56B H 0.7496 -0.1204 0.3974 0.203 Uiso 1 1 calc R . . H56C H 0.7019 -0.0695 0.3526 0.203 Uiso 1 1 calc R . . C66 C 0.6619(7) 0.0207(5) 0.4235(4) 0.124(4) Uiso 1 1 d D . . H66A H 0.6197 0.0522 0.4452 0.186 Uiso 1 1 calc R . . H66B H 0.6706 0.0541 0.3900 0.186 Uiso 1 1 calc R . . H66C H 0.7154 0.0056 0.4363 0.186 Uiso 1 1 calc R . . O17 O 0.4728(2) 0.2536(3) 0.16850(14) 0.0460(9) Uani 1 1 d D . . O27 O 0.6080(2) 0.2316(3) 0.18270(15) 0.0557(11) Uani 1 1 d D . . C17 C 0.5525(3) 0.2558(4) 0.15470(18) 0.0459(13) Uiso 1 1 d D . . C27 C 0.5793(4) 0.2914(4) 0.09896(19) 0.0603(17) Uiso 1 1 d D . . H27A H 0.5352 0.3381 0.0883 0.072 Uiso 1 1 calc R . . H27B H 0.6322 0.3131 0.0950 0.072 Uiso 1 1 calc R . . C37 C 0.5937(4) 0.2298(4) 0.0641(2) 0.0639(18) Uiso 1 1 d D . . C47 C 0.6218(7) 0.2755(6) 0.0109(3) 0.125(4) Uiso 1 1 d D . . H47A H 0.5782 0.3229 0.0020 0.187 Uiso 1 1 calc R . . H47B H 0.6302 0.2385 -0.0123 0.187 Uiso 1 1 calc R . . H47C H 0.6749 0.2943 0.0092 0.187 Uiso 1 1 calc R . . C57 C 0.5115(5) 0.1981(5) 0.0661(3) 0.089(3) Uiso 1 1 d D . . H57A H 0.4915 0.1720 0.1003 0.133 Uiso 1 1 calc R . . H57B H 0.5225 0.1579 0.0446 0.133 Uiso 1 1 calc R . . H57C H 0.4683 0.2441 0.0547 0.133 Uiso 1 1 calc R . . C67 C 0.6617(6) 0.1562(5) 0.0804(4) 0.116(4) Uiso 1 1 d D . . H67A H 0.6426 0.1289 0.1144 0.174 Uiso 1 1 calc R . . H67B H 0.7145 0.1754 0.0789 0.174 Uiso 1 1 calc R . . H67C H 0.6714 0.1174 0.0581 0.174 Uiso 1 1 calc R . . O18 O 0.5514(3) 0.2882(5) 0.3375(2) 0.103(2) Uani 1 1 d D B . O28 O 0.6493(3) 0.2205(3) 0.2846(2) 0.0714(14) Uani 1 1 d D B . C18 C 0.6280(4) 0.2675(5) 0.3160(3) 0.096(3) Uiso 1 1 d D . . C28 C 0.6905(7) 0.3251(7) 0.3163(4) 0.076(4) Uiso 0.562(13) 1 d PD B 1 H28A H 0.7452 0.3075 0.2958 0.092 Uiso 0.562(13) 1 calc PR B 1 H28B H 0.6678 0.3815 0.3004 0.092 Uiso 0.562(13) 1 calc PR B 1 C38 C 0.7067(6) 0.3269(6) 0.3674(4) 0.054(3) Uiso 0.562(13) 1 d PD B 1 C48 C 0.6276(8) 0.3728(10) 0.3971(6) 0.098(6) Uiso 0.562(13) 1 d PD B 1 H48A H 0.6135 0.4290 0.3789 0.147 Uiso 0.562(13) 1 calc PR B 1 H48B H 0.6396 0.3738 0.4297 0.147 Uiso 0.562(13) 1 calc PR B 1 H48C H 0.5797 0.3444 0.4015 0.147 Uiso 0.562(13) 1 calc PR B 1 C58 C 0.7819(9) 0.3697(12) 0.3644(7) 0.119(7) Uiso 0.562(13) 1 d PD B 1 H58A H 0.7651 0.4290 0.3538 0.178 Uiso 0.562(13) 1 calc PR B 1 H58B H 0.8294 0.3493 0.3404 0.178 Uiso 0.562(13) 1 calc PR B 1 H58C H 0.7989 0.3580 0.3971 0.178 Uiso 0.562(13) 1 calc PR B 1 C68 C 0.7243(17) 0.2380(9) 0.3973(8) 0.27(2) Uiso 0.562(13) 1 d PD B 1 H68A H 0.7728 0.2066 0.3791 0.409 Uiso 0.562(13) 1 calc PR B 1 H68B H 0.6745 0.2123 0.4019 0.409 Uiso 0.562(13) 1 calc PR B 1 H68C H 0.7369 0.2390 0.4297 0.409 Uiso 0.562(13) 1 calc PR B 1 C28' C 0.6960(9) 0.2529(11) 0.3504(7) 0.117(9) Uiso 0.438(13) 1 d PD B 2 H28C H 0.6941 0.1989 0.3729 0.140 Uiso 0.438(13) 1 calc PR B 2 H28D H 0.7525 0.2496 0.3293 0.140 Uiso 0.438(13) 1 calc PR B 2 C38' C 0.6877(8) 0.3172(9) 0.3820(6) 0.071(6) Uiso 0.438(13) 1 d PD B 2 C48' C 0.6240(15) 0.298(2) 0.4298(8) 0.24(2) Uiso 0.438(13) 1 d PD B 2 H48D H 0.6194 0.3390 0.4501 0.365 Uiso 0.438(13) 1 calc PR B 2 H48E H 0.6433 0.2435 0.4484 0.365 Uiso 0.438(13) 1 calc PR B 2 H48F H 0.5686 0.3002 0.4212 0.365 Uiso 0.438(13) 1 calc PR B 2 C58' C 0.657(2) 0.4032(11) 0.3521(12) 0.22(2) Uiso 0.438(13) 1 d PD B 2 H58D H 0.6498 0.4442 0.3725 0.337 Uiso 0.438(13) 1 calc PR B 2 H58E H 0.6024 0.4038 0.3426 0.337 Uiso 0.438(13) 1 calc PR B 2 H58F H 0.6983 0.4158 0.3222 0.337 Uiso 0.438(13) 1 calc PR B 2 C68' C 0.7757(9) 0.3158(11) 0.3946(7) 0.075(6) Uiso 0.438(13) 1 d PD B 2 H68D H 0.7706 0.3551 0.4159 0.113 Uiso 0.438(13) 1 calc PR B 2 H68E H 0.8148 0.3307 0.3639 0.113 Uiso 0.438(13) 1 calc PR B 2 H68F H 0.7973 0.2606 0.4118 0.113 Uiso 0.438(13) 1 calc PR B 2 O19 O 0.3106(3) 0.4744(3) 0.25935(19) 0.0697(13) Uani 1 1 d D . . O29 O 0.4412(3) 0.4176(3) 0.2792(2) 0.0832(16) Uani 1 1 d D . . C19 C 0.3912(4) 0.4711(5) 0.2550(3) 0.086(2) Uiso 1 1 d D . . C29 C 0.4321(6) 0.5442(5) 0.2225(3) 0.120(4) Uiso 1 1 d D . . H29A H 0.3865 0.5891 0.2117 0.145 Uiso 1 1 calc R . . H29B H 0.4617 0.5645 0.2433 0.145 Uiso 1 1 calc R . . C39 C 0.4950(5) 0.5249(5) 0.1763(3) 0.084(2) Uiso 1 1 d D . . C49 C 0.5205(8) 0.6044(6) 0.1430(5) 0.164(6) Uiso 1 1 d D . . H49A H 0.4695 0.6445 0.1366 0.246 Uiso 1 1 calc R . . H49B H 0.5537 0.5925 0.1115 0.246 Uiso 1 1 calc R . . H49C H 0.5543 0.6269 0.1598 0.246 Uiso 1 1 calc R . . C59 C 0.5727(6) 0.4614(7) 0.1888(5) 0.142(5) Uiso 1 1 d D . . H59A H 0.5546 0.4107 0.2086 0.213 Uiso 1 1 calc R . . H59B H 0.6038 0.4827 0.2078 0.213 Uiso 1 1 calc R . . H59C H 0.6094 0.4500 0.1581 0.213 Uiso 1 1 calc R . . C69 C 0.4434(8) 0.4895(8) 0.1480(5) 0.175(6) Uiso 1 1 d D . . H69A H 0.4268 0.4387 0.1685 0.262 Uiso 1 1 calc R . . H69B H 0.4782 0.4781 0.1168 0.262 Uiso 1 1 calc R . . H69C H 0.3927 0.5295 0.1409 0.262 Uiso 1 1 calc R . . O110 O 0.2838(3) 0.4467(4) 0.3690(2) 0.0813(17) Uani 1 1 d D . . O210 O 0.4053(3) 0.3564(4) 0.3819(2) 0.0907(19) Uani 1 1 d D . . C110 C 0.3512(4) 0.4208(4) 0.3886(3) 0.079(2) Uiso 1 1 d D . . C210 C 0.3633(6) 0.4678(5) 0.4273(3) 0.097(3) Uiso 1 1 d D . . H21A H 0.4237 0.4553 0.4310 0.117 Uiso 1 1 calc R . . H21B H 0.3492 0.5274 0.4143 0.117 Uiso 1 1 calc R . . C310 C 0.3101(6) 0.4474(6) 0.4785(3) 0.132(4) Uiso 1 1 d D . . C410 C 0.3366(8) 0.4843(8) 0.5169(4) 0.154(5) Uiso 1 1 d D . . H41A H 0.2981 0.4745 0.5485 0.231 Uiso 1 1 calc R . . H41B H 0.3342 0.5435 0.5049 0.231 Uiso 1 1 calc R . . H41C H 0.3944 0.4586 0.5218 0.231 Uiso 1 1 calc R . . C510 C 0.3198(13) 0.3539(7) 0.4974(7) 0.278(12) Uiso 1 1 d D . . H51A H 0.2802 0.3419 0.5283 0.417 Uiso 1 1 calc R . . H51B H 0.3778 0.3318 0.5034 0.417 Uiso 1 1 calc R . . H51C H 0.3076 0.3284 0.4724 0.417 Uiso 1 1 calc R . . C610 C 0.2161(7) 0.4837(10) 0.4744(6) 0.195(7) Uiso 1 1 d D . . H61A H 0.1808 0.4702 0.5068 0.293 Uiso 1 1 calc R . . H61B H 0.1985 0.4603 0.4502 0.293 Uiso 1 1 calc R . . H61C H 0.2096 0.5433 0.4636 0.293 Uiso 1 1 calc R . . O111 O 0.0665(4) 0.4985(3) 0.2674(2) 0.0810(16) Uani 1 1 d D . . O211 O 0.1449(3) 0.5003(3) 0.32475(19) 0.0727(14) Uani 1 1 d D . . C111 C 0.0849(4) 0.5298(4) 0.3003(2) 0.0657(18) Uiso 1 1 d D . . C211 C 0.0251(4) 0.6086(4) 0.3124(3) 0.080(2) Uiso 1 1 d D . . H21C H 0.0597 0.6468 0.3165 0.096 Uiso 1 1 calc R . . H21D H -0.0037 0.6354 0.2836 0.096 Uiso 1 1 calc R . . C311 C -0.0428(5) 0.5958(5) 0.3591(3) 0.091(3) Uiso 1 1 d D . . C411 C -0.0959(7) 0.6810(5) 0.3651(4) 0.127(4) Uiso 1 1 d D . . H41D H -0.0592 0.7163 0.3695 0.190 Uiso 1 1 calc R . . H41E H -0.1404 0.6744 0.3943 0.190 Uiso 1 1 calc R . . H41F H -0.1218 0.7060 0.3355 0.190 Uiso 1 1 calc R . . C511 C -0.0010(7) 0.5581(7) 0.4055(4) 0.136(4) Uiso 1 1 d D . . H51D H 0.0364 0.5937 0.4087 0.204 Uiso 1 1 calc R . . H51E H 0.0321 0.5039 0.4023 0.204 Uiso 1 1 calc R . . H51F H -0.0448 0.5527 0.4350 0.204 Uiso 1 1 calc R . . C611 C -0.1003(7) 0.5379(7) 0.3544(5) 0.154(5) Uiso 1 1 d D . . H61D H -0.1260 0.5603 0.3245 0.231 Uiso 1 1 calc R . . H61E H -0.1447 0.5331 0.3836 0.231 Uiso 1 1 calc R . . H61F H -0.0664 0.4837 0.3521 0.231 Uiso 1 1 calc R . . O112 O 0.1977(3) 0.2078(3) 0.35862(15) 0.0606(12) Uani 1 1 d D . . O212 O 0.1664(3) 0.3248(3) 0.39006(17) 0.0780(15) Uani 1 1 d D . . C112 C 0.1659(5) 0.2493(4) 0.3931(2) 0.071(2) Uiso 1 1 d D . . C212 C 0.1325(6) 0.1974(6) 0.4436(3) 0.129(4) Uiso 1 1 d D . . H21E H 0.1269 0.1441 0.4374 0.154 Uiso 1 1 calc R . . H21F H 0.1769 0.1860 0.4646 0.154 Uiso 1 1 calc R . . C312 C 0.0498(4) 0.2301(5) 0.4741(3) 0.076(2) Uiso 1 1 d D . . C412 C -0.0197(8) 0.2641(10) 0.4418(5) 0.214(8) Uiso 1 1 d D . . H41G H 0.0001 0.3051 0.4134 0.320 Uiso 1 1 calc R . . H41H H -0.0705 0.2896 0.4615 0.320 Uiso 1 1 calc R . . H41I H -0.0328 0.2193 0.4299 0.320 Uiso 1 1 calc R . . C512 C 0.0603(10) 0.3010(8) 0.4966(6) 0.212(8) Uiso 1 1 d D . . H51G H 0.0778 0.3455 0.4699 0.318 Uiso 1 1 calc R . . H51H H 0.1033 0.2813 0.5181 0.318 Uiso 1 1 calc R . . H51I H 0.0063 0.3212 0.5160 0.318 Uiso 1 1 calc R . . C612 C 0.0199(8) 0.1620(7) 0.5168(4) 0.141(5) Uiso 1 1 d D . . H61G H 0.0596 0.1459 0.5405 0.212 Uiso 1 1 calc R . . H61H H 0.0176 0.1144 0.5035 0.212 Uiso 1 1 calc R . . H61I H -0.0364 0.1825 0.5337 0.212 Uiso 1 1 calc R . . O113 O 0.0409(3) 0.4652(3) 0.1850(2) 0.0703(14) Uani 1 1 d D . . O213 O 0.0015(3) 0.3678(3) 0.15505(18) 0.0591(11) Uani 1 1 d D . . C113 C -0.0046(4) 0.4409(3) 0.1604(2) 0.0592(17) Uiso 1 1 d D . . C213 C -0.0703(4) 0.5077(4) 0.1350(3) 0.079(2) Uiso 1 1 d D . . H21G H -0.0394 0.5434 0.1072 0.094 Uiso 1 1 calc R . . H21H H -0.1040 0.4806 0.1204 0.094 Uiso 1 1 calc R . . C313 C -0.1317(4) 0.5627(4) 0.1680(3) 0.080(2) Uiso 1 1 d D . . C413 C -0.1684(7) 0.5084(7) 0.2167(3) 0.132(4) Uiso 1 1 d D . . H41J H -0.1941 0.4672 0.2088 0.199 Uiso 1 1 calc R . . H41K H -0.2113 0.5428 0.2364 0.199 Uiso 1 1 calc R . . H41L H -0.1229 0.4810 0.2357 0.199 Uiso 1 1 calc R . . C513 C -0.0857(7) 0.6238(7) 0.1801(5) 0.139(4) Uiso 1 1 d D . . H51J H -0.0654 0.6601 0.1493 0.209 Uiso 1 1 calc R . . H51K H -0.0376 0.5937 0.1962 0.209 Uiso 1 1 calc R . . H51L H -0.1248 0.6566 0.2023 0.209 Uiso 1 1 calc R . . C613 C -0.2040(5) 0.6110(6) 0.1397(3) 0.099(3) Uiso 1 1 d D . . H61J H -0.1812 0.6490 0.1106 0.149 Uiso 1 1 calc R . . H61K H -0.2466 0.6419 0.1616 0.149 Uiso 1 1 calc R . . H61L H -0.2300 0.5726 0.1291 0.149 Uiso 1 1 calc R . . O114 O 0.2645(3) -0.1358(3) 0.21744(19) 0.0622(12) Uani 1 1 d D . . O214 O 0.1655(3) -0.0430(3) 0.1787(2) 0.0703(14) Uani 1 1 d D . . C114 C 0.1979(4) -0.1156(3) 0.1972(2) 0.0516(15) Uiso 1 1 d D . . C214 C 0.1545(4) -0.1853(4) 0.1935(2) 0.0677(19) Uiso 1 1 d D . . H21I H 0.1613 -0.2293 0.2231 0.081 Uiso 1 1 calc R . . H21J H 0.0933 -0.1638 0.1949 0.081 Uiso 1 1 calc R . . C314 C 0.1857(5) -0.2233(4) 0.1476(2) 0.078(2) Uiso 1 1 d D . . C414 C 0.2785(5) -0.2671(7) 0.1458(5) 0.151(5) Uiso 1 1 d D . . H41M H 0.2829 -0.3120 0.1747 0.226 Uiso 1 1 calc R . . H41N H 0.3141 -0.2280 0.1462 0.226 Uiso 1 1 calc R . . H41O H 0.2972 -0.2893 0.1154 0.226 Uiso 1 1 calc R . . C514 C 0.1287(7) -0.2865(6) 0.1490(4) 0.134(4) Uiso 1 1 d D . . H51M H 0.1304 -0.3278 0.1797 0.202 Uiso 1 1 calc R . . H51N H 0.1495 -0.3133 0.1205 0.202 Uiso 1 1 calc R . . H51O H 0.0705 -0.2581 0.1477 0.202 Uiso 1 1 calc R . . C614 C 0.1804(7) -0.1573(6) 0.0999(3) 0.131(4) Uiso 1 1 d D . . H61M H 0.2180 -0.1187 0.0981 0.196 Uiso 1 1 calc R . . H61N H 0.1222 -0.1278 0.1004 0.196 Uiso 1 1 calc R . . H61O H 0.1976 -0.1834 0.0710 0.196 Uiso 1 1 calc R . . O115 O 0.2405(3) 0.0382(3) 0.32596(15) 0.0519(10) Uani 1 1 d D . . O215 O 0.2598(3) -0.0948(3) 0.31631(16) 0.0624(12) Uani 1 1 d D . . C115 C 0.2350(4) -0.0393(3) 0.3417(2) 0.0562(16) Uiso 1 1 d D . . C215 C 0.1964(4) -0.0616(4) 0.3970(2) 0.0670(19) Uiso 1 1 d D . . H21K H 0.1513 -0.0157 0.4053 0.080 Uiso 1 1 calc R . . H21L H 0.1695 -0.1103 0.4019 0.080 Uiso 1 1 calc R . . C315 C 0.2592(4) -0.0798(4) 0.4337(2) 0.0703(19) Uiso 1 1 d D . . C415 C 0.3240(7) -0.1570(6) 0.4258(5) 0.147(5) Uiso 1 1 d D . . H41P H 0.2947 -0.2035 0.4312 0.221 Uiso 1 1 calc R . . H41Q H 0.3636 -0.1685 0.4493 0.221 Uiso 1 1 calc R . . H41R H 0.3551 -0.1482 0.3918 0.221 Uiso 1 1 calc R . . C515 C 0.2062(7) -0.0921(7) 0.4864(3) 0.132(4) Uiso 1 1 d D . . H51P H 0.1653 -0.0421 0.4904 0.199 Uiso 1 1 calc R . . H51Q H 0.2437 -0.1042 0.5111 0.199 Uiso 1 1 calc R . . H51R H 0.1761 -0.1379 0.4911 0.199 Uiso 1 1 calc R . . C615 C 0.3045(6) -0.0061(5) 0.4265(4) 0.104(3) Uiso 1 1 d D . . H61P H 0.2624 0.0430 0.4312 0.157 Uiso 1 1 calc R . . H61Q H 0.3371 0.0033 0.3929 0.157 Uiso 1 1 calc R . . H61R H 0.3427 -0.0177 0.4508 0.157 Uiso 1 1 calc R . . O116 O 0.0654(3) 0.0836(3) 0.22875(19) 0.0683(13) Uani 1 1 d D . . O216 O 0.0184(3) 0.2171(3) 0.23295(16) 0.0562(11) Uani 1 1 d D . . C116 C 0.0307(5) 0.1417(4) 0.2527(2) 0.072(2) Uiso 1 1 d D . . C216 C 0.0101(6) 0.1157(5) 0.3104(2) 0.096(3) Uiso 1 1 d D . . H21M H 0.0640 0.0951 0.3234 0.115 Uiso 1 1 calc R . . H21N H -0.0180 0.1650 0.3242 0.115 Uiso 1 1 calc R . . C316 C -0.0465(4) 0.0496(4) 0.3297(2) 0.0692(19) Uiso 1 1 d D . . C416 C 0.0040(6) -0.0345(5) 0.3217(4) 0.114(3) Uiso 1 1 d D . . H41S H 0.0235 -0.0328 0.2862 0.171 Uiso 1 1 calc R . . H41T H -0.0322 -0.0762 0.3349 0.171 Uiso 1 1 calc R . . H41U H 0.0528 -0.0482 0.3389 0.171 Uiso 1 1 calc R . . C516 C -0.1233(7) 0.0739(8) 0.3024(5) 0.166(6) Uiso 1 1 d D . . H51S H -0.1559 0.1265 0.3093 0.249 Uiso 1 1 calc R . . H51T H -0.1592 0.0318 0.3140 0.249 Uiso 1 1 calc R . . H51U H -0.1037 0.0790 0.2666 0.249 Uiso 1 1 calc R . . C616 C -0.0782(8) 0.0459(8) 0.3858(3) 0.147(5) Uiso 1 1 d D . . H61S H -0.1114 0.0992 0.3910 0.221 Uiso 1 1 calc R . . H61T H -0.0297 0.0327 0.4032 0.221 Uiso 1 1 calc R . . H61U H -0.1136 0.0036 0.3986 0.221 Uiso 1 1 calc R . . O117 O 0.1142(3) 0.0962(3) 0.12017(17) 0.0623(12) Uani 1 1 d D . . O217 O 0.0389(3) 0.2249(3) 0.12192(16) 0.0546(11) Uani 1 1 d D . . C117 C 0.0592(4) 0.1584(3) 0.1055(2) 0.0553(16) Uiso 1 1 d D C . C217 C 0.0138(4) 0.1504(4) 0.0645(2) 0.0689(19) Uiso 1 1 d D . . H21O H 0.0235 0.0919 0.0623 0.083 Uiso 0.778(14) 1 calc PR C 1 H21P H -0.0477 0.1677 0.0745 0.083 Uiso 0.778(14) 1 calc PR C 1 H21Q H -0.0078 0.0980 0.0747 0.083 Uiso 0.222(14) 1 calc PR C 2 H21R H -0.0357 0.1952 0.0622 0.083 Uiso 0.222(14) 1 calc PR C 2 C317 C 0.0411(7) 0.2003(6) 0.0127(3) 0.112(5) Uiso 0.778(14) 1 d PD C 1 C417 C -0.0032(12) 0.1774(11) -0.0245(5) 0.167(9) Uiso 0.778(14) 1 d PD C 1 H41V H 0.0118 0.2101 -0.0576 0.250 Uiso 0.778(14) 1 calc PR C 1 H41W H -0.0646 0.1887 -0.0140 0.250 Uiso 0.778(14) 1 calc PR C 1 H41X H 0.0150 0.1191 -0.0253 0.250 Uiso 0.778(14) 1 calc PR C 1 C517 C 0.1382(7) 0.1807(12) -0.0029(7) 0.210(11) Uiso 0.778(14) 1 d PD C 1 H51V H 0.1552 0.2165 -0.0346 0.315 Uiso 0.778(14) 1 calc PR C 1 H51W H 0.1549 0.1233 -0.0065 0.315 Uiso 0.778(14) 1 calc PR C 1 H51X H 0.1660 0.1898 0.0226 0.315 Uiso 0.778(14) 1 calc PR C 1 C617 C 0.0140(10) 0.2928(6) 0.0126(5) 0.136(6) Uiso 0.778(14) 1 d PD C 1 H61V H 0.0348 0.3242 -0.0200 0.204 Uiso 0.778(14) 1 calc PR C 1 H61W H 0.0379 0.3067 0.0381 0.204 Uiso 0.778(14) 1 calc PR C 1 H61X H -0.0477 0.3063 0.0195 0.204 Uiso 0.778(14) 1 calc PR C 1 C327 C 0.0675(11) 0.1533(13) 0.0126(4) 0.094(9) Uiso 0.222(14) 1 d PD C 2 C427 C 0.010(2) 0.158(3) -0.0255(7) 0.094(9) Uiso 0.222(14) 1 d PD C 2 H42A H 0.0445 0.1599 -0.0586 0.141 Uiso 0.222(14) 1 calc PR C 2 H42B H -0.0326 0.2082 -0.0257 0.141 Uiso 0.222(14) 1 calc PR C 2 H42C H -0.0176 0.1103 -0.0165 0.141 Uiso 0.222(14) 1 calc PR C 2 C527 C 0.113(2) 0.2286(19) -0.0016(10) 0.094(9) Uiso 0.222(14) 1 d PD C 2 H52A H 0.1455 0.2309 -0.0351 0.141 Uiso 0.222(14) 1 calc PR C 2 H52B H 0.1508 0.2238 0.0220 0.141 Uiso 0.222(14) 1 calc PR C 2 H52C H 0.0706 0.2787 -0.0007 0.141 Uiso 0.222(14) 1 calc PR C 2 C627 C 0.1361(17) 0.0758(18) 0.0119(11) 0.094(9) Uiso 0.222(14) 1 d PD C 2 H62A H 0.1685 0.0776 -0.0217 0.141 Uiso 0.222(14) 1 calc PR C 2 H62B H 0.1093 0.0270 0.0219 0.141 Uiso 0.222(14) 1 calc PR C 2 H62C H 0.1742 0.0737 0.0350 0.141 Uiso 0.222(14) 1 calc PR C 2 O118 O 0.2976(2) 0.2975(3) 0.12820(14) 0.0505(10) Uani 1 1 d D . . O218 O 0.1760(3) 0.3289(3) 0.09425(16) 0.0643(12) Uani 1 1 d D . . C118 C 0.2530(4) 0.3329(4) 0.0933(2) 0.0584(16) Uiso 1 1 d D . . C218 C 0.3021(5) 0.3794(5) 0.0461(3) 0.098(3) Uiso 1 1 d D . . H21S H 0.3556 0.3859 0.0545 0.117 Uiso 1 1 calc R . . H21T H 0.3173 0.3436 0.0213 0.117 Uiso 1 1 calc R . . C318 C 0.2609(5) 0.4636(5) 0.0207(3) 0.094(3) Uiso 1 1 d D . . C418 C 0.3277(7) 0.5030(7) -0.0199(4) 0.133(4) Uiso 1 1 d D . . H41Y H 0.3010 0.5559 -0.0373 0.200 Uiso 1 1 calc R . . H41Z H 0.3517 0.4667 -0.0436 0.200 Uiso 1 1 calc R . . H411 H 0.3728 0.5112 -0.0045 0.200 Uiso 1 1 calc R . . C518 C 0.1885(8) 0.4534(11) -0.0035(6) 0.248(10) Uiso 1 1 d D . . H51Y H 0.1471 0.4266 0.0219 0.372 Uiso 1 1 calc R . . H51Z H 0.2115 0.4196 -0.0287 0.372 Uiso 1 1 calc R . . H511 H 0.1610 0.5073 -0.0191 0.372 Uiso 1 1 calc R . . C618 C 0.2215(9) 0.5198(8) 0.0582(5) 0.188(7) Uiso 1 1 d D . . H61Y H 0.1795 0.4939 0.0836 0.282 Uiso 1 1 calc R . . H61Z H 0.1940 0.5725 0.0409 0.282 Uiso 1 1 calc R . . H611 H 0.2658 0.5288 0.0739 0.282 Uiso 1 1 calc R . . N1A N 0.8046(8) 0.3006(9) 0.1351(5) 0.145(4) Uiso 1 1 d . . . C1A C 0.8159(8) 0.2522(8) 0.1830(5) 0.126(4) Uiso 1 1 d . . . H1A1 H 0.8142 0.2883 0.2059 0.188 Uiso 1 1 calc R . . H1A2 H 0.8707 0.2154 0.1804 0.188 Uiso 1 1 calc R . . H1A3 H 0.7706 0.2197 0.1956 0.188 Uiso 1 1 calc R . . O2A O 0.8128(8) 0.2701(8) 0.1000(5) 0.198(5) Uiso 1 1 d . . . O3A O 0.7797(9) 0.3712(10) 0.1302(5) 0.208(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0306(4) 0.0512(5) 0.0329(4) -0.0129(4) -0.0046(3) -0.0069(3) Mn2 0.0359(4) 0.0501(5) 0.0303(4) -0.0065(4) -0.0085(3) -0.0091(4) Mn3 0.0328(4) 0.0476(5) 0.0320(4) -0.0073(4) -0.0063(3) -0.0067(3) Mn4 0.0339(4) 0.0574(6) 0.0324(4) -0.0146(4) -0.0020(3) -0.0074(4) Mn5 0.0423(5) 0.0763(7) 0.0543(6) -0.0368(5) -0.0043(4) -0.0037(5) Mn6 0.0421(5) 0.0843(7) 0.0550(6) -0.0392(5) -0.0126(4) -0.0054(5) Mn7 0.0327(5) 0.0640(6) 0.0522(6) -0.0215(5) -0.0107(4) -0.0062(4) Mn8 0.0398(5) 0.0518(6) 0.0611(6) -0.0175(4) -0.0188(4) -0.0007(4) Mn9 0.0482(5) 0.0475(5) 0.0506(5) -0.0051(4) -0.0194(4) -0.0100(4) Mn10 0.0447(5) 0.0507(5) 0.0407(5) -0.0139(4) -0.0168(4) -0.0032(4) Mn11 0.0384(5) 0.0517(5) 0.0430(5) -0.0106(4) -0.0135(4) -0.0026(4) Mn12 0.0462(5) 0.0577(6) 0.0537(6) -0.0222(5) -0.0136(4) 0.0026(4) O6 0.085(4) 0.120(5) 0.061(3) -0.013(3) -0.018(3) 0.014(3) O10 0.083(4) 0.132(5) 0.049(3) -0.009(3) -0.008(3) 0.030(4) O120 0.055(3) 0.097(4) 0.079(4) -0.034(3) 0.000(2) -0.017(3) O121 0.114(5) 0.092(4) 0.073(4) -0.002(3) -0.027(3) -0.049(4) O107 0.038(2) 0.063(3) 0.042(2) -0.0227(19) -0.0102(17) -0.0071(18) O108 0.0306(19) 0.060(2) 0.048(2) -0.0175(19) -0.0077(16) -0.0062(17) O123 0.0329(19) 0.047(2) 0.0286(18) -0.0066(15) -0.0061(14) -0.0078(15) O124 0.0317(19) 0.056(2) 0.0318(19) -0.0116(17) -0.0055(15) -0.0068(16) O134 0.0342(19) 0.048(2) 0.0342(19) -0.0142(16) -0.0027(15) -0.0065(16) O208 0.047(2) 0.046(2) 0.044(2) -0.0054(17) -0.0157(18) -0.0080(17) O209 0.042(2) 0.048(2) 0.039(2) -0.0025(17) -0.0146(17) -0.0102(17) O234 0.0308(19) 0.053(2) 0.036(2) -0.0101(17) -0.0067(15) -0.0066(16) O310 0.037(2) 0.049(2) 0.040(2) -0.0089(17) -0.0141(16) -0.0036(16) O311 0.038(2) 0.050(2) 0.047(2) -0.0149(18) -0.0113(17) -0.0001(17) O405 0.036(2) 0.065(3) 0.045(2) -0.024(2) -0.0041(17) -0.0053(18) O406 0.041(2) 0.066(3) 0.047(2) -0.028(2) -0.0090(18) -0.0042(19) O13 0.070(3) 0.063(3) 0.132(5) -0.025(3) -0.050(3) 0.007(3) O23 0.066(3) 0.049(3) 0.091(4) -0.001(2) -0.039(3) -0.007(2) O14 0.064(3) 0.091(4) 0.082(4) -0.037(3) 0.002(3) -0.020(3) O24 0.054(3) 0.069(3) 0.055(3) -0.019(2) -0.015(2) -0.005(2) O15 0.043(3) 0.087(4) 0.090(4) -0.042(3) -0.015(2) -0.003(2) O25 0.052(3) 0.086(4) 0.168(6) -0.066(4) -0.027(3) 0.010(3) O16 0.069(3) 0.074(3) 0.055(3) -0.011(2) -0.022(2) -0.010(2) O26 0.091(4) 0.072(3) 0.078(4) 0.002(3) -0.044(3) -0.019(3) O17 0.038(2) 0.060(3) 0.041(2) -0.0127(18) -0.0031(17) -0.0124(18) O27 0.042(2) 0.074(3) 0.052(3) -0.016(2) 0.0018(19) -0.018(2) O18 0.045(3) 0.175(6) 0.122(5) -0.103(5) -0.014(3) -0.008(3) O28 0.041(2) 0.104(4) 0.087(4) -0.052(3) -0.008(2) -0.017(2) O19 0.061(3) 0.078(3) 0.072(3) -0.026(3) -0.003(2) -0.014(2) O29 0.055(3) 0.084(4) 0.118(5) -0.036(3) -0.003(3) -0.023(3) O110 0.065(3) 0.117(4) 0.083(4) -0.071(3) -0.023(3) 0.007(3) O210 0.075(4) 0.128(5) 0.087(4) -0.070(4) -0.035(3) 0.018(3) O111 0.088(4) 0.077(4) 0.086(4) -0.044(3) -0.034(3) 0.017(3) O211 0.058(3) 0.090(4) 0.082(4) -0.057(3) -0.015(3) 0.008(3) O112 0.056(3) 0.082(3) 0.040(2) -0.017(2) 0.0080(19) -0.012(2) O212 0.077(3) 0.109(4) 0.041(3) -0.028(3) 0.015(2) -0.011(3) O113 0.073(3) 0.064(3) 0.079(3) -0.023(3) -0.034(3) 0.008(2) O213 0.048(2) 0.059(3) 0.073(3) -0.017(2) -0.024(2) 0.002(2) O114 0.063(3) 0.052(3) 0.080(3) -0.006(2) -0.033(2) -0.015(2) O214 0.078(3) 0.059(3) 0.091(4) -0.030(3) -0.046(3) -0.003(2) O115 0.051(2) 0.065(3) 0.038(2) -0.0022(19) -0.0067(18) -0.016(2) O215 0.071(3) 0.065(3) 0.052(3) 0.005(2) -0.018(2) -0.025(2) O116 0.061(3) 0.066(3) 0.074(3) -0.015(3) 0.011(2) -0.020(2) O216 0.046(2) 0.063(3) 0.054(3) -0.008(2) -0.0016(19) -0.008(2) O117 0.067(3) 0.069(3) 0.061(3) -0.024(2) -0.035(2) 0.003(2) O217 0.054(3) 0.058(3) 0.056(3) -0.012(2) -0.026(2) -0.002(2) O118 0.048(2) 0.060(3) 0.038(2) 0.0000(19) -0.0020(18) -0.0100(19) O218 0.065(3) 0.078(3) 0.042(2) 0.002(2) -0.012(2) -0.007(2) _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 O108 1.848(4) . ? Mn1 O107 1.880(4) . ? Mn1 O17 1.899(4) . ? Mn1 O124 1.917(4) . ? Mn1 O123 1.926(4) . ? Mn1 O134 1.927(4) . ? Mn1 Mn7 2.7716(12) . ? Mn1 Mn4 2.8381(11) . ? Mn1 Mn2 2.8423(12) . ? Mn1 Mn3 2.9382(11) . ? Mn2 O208 1.853(4) . ? Mn2 O209 1.867(4) . ? Mn2 O115 1.895(4) . ? Mn2 O124 1.919(4) . ? Mn2 O123 1.923(3) . ? Mn2 O234 1.927(4) . ? Mn2 Mn9 2.7619(13) . ? Mn2 Mn3 2.8284(12) . ? Mn2 Mn4 2.9368(12) . ? Mn3 O310 1.863(4) . ? Mn3 O311 1.868(4) . ? Mn3 O234 1.892(4) . ? Mn3 O123 1.900(4) . ? Mn3 O134 1.909(4) . ? Mn3 O118 1.925(4) . ? Mn3 Mn11 2.7863(11) . ? Mn3 Mn4 2.8091(12) . ? Mn4 O406 1.852(4) . ? Mn4 O405 1.886(4) . ? Mn4 O134 1.894(4) . ? Mn4 O234 1.901(4) . ? Mn4 O112 1.916(4) . ? Mn4 O124 1.917(4) . ? Mn4 Mn5 2.7943(13) . ? Mn5 O406 1.875(4) . ? Mn5 O405 1.916(4) . ? Mn5 O211 1.937(5) . ? Mn5 O110 1.947(4) . ? Mn5 O19 2.184(5) . ? Mn5 O212 2.224(5) . ? Mn6 O406 1.875(4) . ? Mn6 O107 1.888(4) . ? Mn6 O18 1.931(5) . ? Mn6 O210 1.964(5) . ? Mn6 O29 2.073(6) . ? Mn6 O6 2.269(6) . ? Mn7 O108 1.872(4) . ? Mn7 O107 1.909(4) . ? Mn7 O15 1.931(4) . ? Mn7 O28 1.938(4) . ? Mn7 O27 2.202(4) . ? Mn7 O16 2.203(5) . ? Mn8 O108 1.932(4) . ? Mn8 O208 1.956(4) . ? Mn8 O13 1.994(5) . ? Mn8 O26 2.005(5) . ? Mn8 O14 2.015(5) . ? Mn8 O25 2.022(5) . ? Mn9 O208 1.879(4) . ? Mn9 O209 1.898(4) . ? Mn9 O23 1.936(4) . ? Mn9 O114 1.948(4) . ? Mn9 O24 2.194(4) . ? Mn9 O215 2.214(4) . ? Mn10 O209 1.882(4) . ? Mn10 O310 1.882(4) . ? Mn10 O214 1.933(4) . ? Mn10 O117 1.961(4) . ? Mn10 O116 2.103(4) . ? Mn10 O10 2.265(5) . ? Mn11 O311 1.892(4) . ? Mn11 O310 1.900(4) . ? Mn11 O217 1.934(4) . ? Mn11 O213 1.942(4) . ? Mn11 O216 2.174(4) . ? Mn11 O218 2.209(4) . ? Mn12 O311 1.856(4) . ? Mn12 O405 1.878(4) . ? Mn12 O111 1.940(5) . ? Mn12 O113 1.957(5) . ? Mn12 O121 2.230(6) . ? Mn12 O120 2.254(5) . ? O13 C13 1.252(6) . ? O23 C13 1.243(6) . ? C13 C23 1.515(6) . ? C23 C33 1.503(7) . ? C33 C43 1.516(7) . ? C33 C63 1.518(7) . ? C33 C53 1.518(7) . ? O14 C14 1.250(5) . ? O24 C14 1.257(5) . ? C14 C24 1.509(6) . ? C24 C34 1.499(6) . ? C34 C64 1.512(6) . ? C34 C44 1.513(6) . ? C34 C54 1.525(6) . ? O15 C15 1.255(6) . ? O25 C15 1.249(6) . ? C15 C25 1.527(7) . ? C15 C25' 1.528(7) . ? C25 C35 1.489(7) . ? C35 C45 1.512(7) . ? C35 C65 1.512(7) . ? C35 C55 1.516(7) . ? C25' C35' 1.504(7) . ? C35' C65' 1.511(7) . ? C35' C55' 1.511(7) . ? C35' C45' 1.516(7) . ? O16 C16 1.260(5) . ? O26 C16 1.243(6) . ? C16 C26 1.518(6) . ? C26 C36 1.507(6) . ? C36 C56 1.505(6) . ? C36 C46 1.512(6) . ? C36 C66 1.525(6) . ? O17 C17 1.265(5) . ? O27 C17 1.241(5) . ? C17 C27 1.519(6) . ? C27 C37 1.516(6) . ? C37 C67 1.510(6) . ? C37 C47 1.512(6) . ? C37 C57 1.513(6) . ? O18 C18 1.266(6) . ? O28 C18 1.250(6) . ? C18 C28 1.534(7) . ? C18 C28' 1.537(7) . ? C28 C38 1.491(7) . ? C38 C58 1.510(7) . ? C38 C68 1.518(7) . ? C38 C48 1.524(7) . ? C28' C38' 1.502(7) . ? C38' C48' 1.506(7) . ? C38' C58' 1.516(7) . ? C38' C68' 1.519(7) . ? O19 C19 1.269(6) . ? O29 C19 1.235(6) . ? C19 C29 1.520(7) . ? C29 C39 1.506(7) . ? C39 C59 1.499(6) . ? C39 C49 1.509(6) . ? C39 C69 1.529(7) . ? O110 C110 1.258(6) . ? O210 C110 1.255(6) . ? C110 C210 1.528(6) . ? C210 C310 1.496(7) . ? C310 C510 1.511(7) . ? C310 C410 1.510(7) . ? C310 C610 1.522(7) . ? O111 C111 1.256(6) . ? O211 C111 1.242(6) . ? C111 C211 1.516(6) . ? C211 C311 1.513(6) . ? C311 C511 1.510(7) . ? C311 C611 1.514(7) . ? C311 C411 1.521(6) . ? O112 C112 1.266(6) . ? O212 C112 1.244(6) . ? C112 C212 1.516(6) . ? C212 C312 1.489(7) . ? C312 C412 1.505(7) . ? C312 C612 1.511(6) . ? C312 C512 1.511(7) . ? O113 C113 1.271(5) . ? O213 C113 1.245(5) . ? C113 C213 1.514(6) . ? C213 C313 1.509(6) . ? C313 C513 1.510(6) . ? C313 C613 1.515(6) . ? C313 C413 1.516(6) . ? O114 C114 1.258(5) . ? O214 C114 1.246(5) . ? C114 C214 1.509(6) . ? C214 C314 1.492(6) . ? C314 C614 1.510(6) . ? C314 C414 1.512(6) . ? C314 C514 1.526(6) . ? O115 C115 1.281(5) . ? O215 C115 1.238(5) . ? C115 C215 1.513(6) . ? C215 C315 1.510(6) . ? C315 C415 1.503(6) . ? C315 C615 1.515(6) . ? C315 C515 1.517(6) . ? O116 C116 1.267(6) . ? O216 C116 1.240(6) . ? C116 C216 1.531(6) . ? C216 C316 1.512(6) . ? C316 C416 1.504(6) . ? C316 C516 1.512(6) . ? C316 C616 1.513(6) . ? O117 C117 1.259(5) . ? O217 C117 1.250(5) . ? C117 C217 1.509(6) . ? C217 C327 1.506(7) . ? C217 C317 1.506(7) . ? C317 C617 1.511(7) . ? C317 C417 1.516(7) . ? C317 C517 1.517(7) . ? C327 C627 1.512(7) . ? C327 C427 1.511(7) . ? C327 C527 1.519(7) . ? O118 C118 1.275(5) . ? O218 C118 1.251(5) . ? C118 C218 1.511(6) . ? C218 C318 1.496(7) . ? C318 C618 1.508(7) . ? C318 C518 1.513(7) . ? C318 C418 1.516(6) . ? N1A O3A 1.147(15) . ? N1A O2A 1.165(15) . ? N1A C1A 1.404(15) . ? 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 O108 Mn1 O107 84.18(17) . . ? O108 Mn1 O17 92.65(17) . . ? O107 Mn1 O17 94.57(17) . . ? O108 Mn1 O124 94.30(17) . . ? O107 Mn1 O124 89.54(16) . . ? O17 Mn1 O124 172.25(16) . . ? O108 Mn1 O123 96.28(16) . . ? O107 Mn1 O123 173.10(16) . . ? O17 Mn1 O123 92.29(16) . . ? O124 Mn1 O123 83.56(15) . . ? O108 Mn1 O134 174.98(16) . . ? O107 Mn1 O134 99.97(16) . . ? O17 Mn1 O134 89.84(16) . . ? O124 Mn1 O134 82.97(15) . . ? O123 Mn1 O134 79.25(15) . . ? O108 Mn1 Mn7 42.17(12) . . ? O107 Mn1 Mn7 43.39(12) . . ? O17 Mn1 Mn7 86.36(11) . . ? O124 Mn1 Mn7 101.10(11) . . ? O123 Mn1 Mn7 138.16(11) . . ? O134 Mn1 Mn7 142.47(11) . . ? O108 Mn1 Mn4 136.27(13) . . ? O107 Mn1 Mn4 89.83(12) . . ? O17 Mn1 Mn4 131.05(12) . . ? O124 Mn1 Mn4 42.24(11) . . ? O123 Mn1 Mn4 85.08(11) . . ? O134 Mn1 Mn4 41.59(11) . . ? Mn7 Mn1 Mn4 125.93(4) . . ? O108 Mn1 Mn2 89.87(12) . . ? O107 Mn1 Mn2 130.86(13) . . ? O17 Mn1 Mn2 134.49(12) . . ? O124 Mn1 Mn2 42.22(11) . . ? O123 Mn1 Mn2 42.35(10) . . ? O134 Mn1 Mn2 85.28(11) . . ? Mn7 Mn1 Mn2 122.71(4) . . ? Mn4 Mn1 Mn2 62.26(3) . . ? O108 Mn1 Mn3 135.79(12) . . ? O107 Mn1 Mn3 139.51(13) . . ? O17 Mn1 Mn3 90.31(11) . . ? O124 Mn1 Mn3 82.32(11) . . ? O123 Mn1 Mn3 39.51(11) . . ? O134 Mn1 Mn3 39.77(11) . . ? Mn7 Mn1 Mn3 175.89(4) . . ? Mn4 Mn1 Mn3 58.17(3) . . ? Mn2 Mn1 Mn3 58.56(3) . . ? O208 Mn2 O209 84.65(17) . . ? O208 Mn2 O115 93.03(18) . . ? O209 Mn2 O115 94.36(17) . . ? O208 Mn2 O124 97.06(16) . . ? O209 Mn2 O124 173.69(16) . . ? O115 Mn2 O124 91.62(17) . . ? O208 Mn2 O123 93.60(16) . . ? O209 Mn2 O123 90.25(16) . . ? O115 Mn2 O123 172.25(17) . . ? O124 Mn2 O123 83.59(15) . . ? O208 Mn2 O234 175.31(16) . . ? O209 Mn2 O234 98.38(16) . . ? O115 Mn2 O234 90.32(17) . . ? O124 Mn2 O234 79.54(16) . . ? O123 Mn2 O234 82.84(15) . . ? O208 Mn2 Mn9 42.61(12) . . ? O209 Mn2 Mn9 43.27(12) . . ? O115 Mn2 Mn9 86.95(13) . . ? O124 Mn2 Mn9 139.37(12) . . ? O123 Mn2 Mn9 100.65(11) . . ? O234 Mn2 Mn9 141.02(11) . . ? O208 Mn2 Mn3 135.18(13) . . ? O209 Mn2 Mn3 89.15(12) . . ? O115 Mn2 Mn3 131.74(13) . . ? O124 Mn2 Mn3 85.35(12) . . ? O123 Mn2 Mn3 41.97(11) . . ? O234 Mn2 Mn3 41.74(11) . . ? Mn9 Mn2 Mn3 124.48(4) . . ? O208 Mn2 Mn1 89.93(12) . . ? O209 Mn2 Mn1 131.98(12) . . ? O115 Mn2 Mn1 133.61(13) . . ? O124 Mn2 Mn1 42.17(11) . . ? O123 Mn2 Mn1 42.43(10) . . ? O234 Mn2 Mn1 85.38(11) . . ? Mn9 Mn2 Mn1 123.22(4) . . ? Mn3 Mn2 Mn1 62.41(3) . . ? O208 Mn2 Mn4 137.05(12) . . ? O209 Mn2 Mn4 137.81(12) . . ? O115 Mn2 Mn4 90.03(13) . . ? O124 Mn2 Mn4 40.00(11) . . ? O123 Mn2 Mn4 82.38(11) . . ? O234 Mn2 Mn4 39.57(11) . . ? Mn9 Mn2 Mn4 176.91(4) . . ? Mn3 Mn2 Mn4 58.28(3) . . ? Mn1 Mn2 Mn4 58.80(3) . . ? O310 Mn3 O311 84.84(17) . . ? O310 Mn3 O234 90.89(16) . . ? O311 Mn3 O234 88.27(17) . . ? O310 Mn3 O123 96.83(16) . . ? O311 Mn3 O123 172.51(16) . . ? O234 Mn3 O123 84.41(15) . . ? O310 Mn3 O134 174.06(16) . . ? O311 Mn3 O134 97.30(16) . . ? O234 Mn3 O134 83.65(16) . . ? O123 Mn3 O134 80.34(15) . . ? O310 Mn3 O118 92.64(17) . . ? O311 Mn3 O118 90.47(18) . . ? O234 Mn3 O118 176.12(18) . . ? O123 Mn3 O118 96.73(16) . . ? O134 Mn3 O118 92.87(17) . . ? O310 Mn3 Mn11 42.74(11) . . ? O311 Mn3 Mn11 42.52(12) . . ? O234 Mn3 Mn11 94.11(11) . . ? O123 Mn3 Mn11 139.57(11) . . ? O134 Mn3 Mn11 139.80(12) . . ? O118 Mn3 Mn11 87.43(12) . . ? O310 Mn3 Mn4 132.77(12) . . ? O311 Mn3 Mn4 87.15(12) . . ? O234 Mn3 Mn4 42.33(11) . . ? O123 Mn3 Mn4 86.37(11) . . ? O134 Mn3 Mn4 42.18(11) . . ? O118 Mn3 Mn4 133.94(13) . . ? Mn11 Mn3 Mn4 118.89(4) . . ? O310 Mn3 Mn2 88.40(12) . . ? O311 Mn3 Mn2 130.41(13) . . ? O234 Mn3 Mn2 42.71(11) . . ? O123 Mn3 Mn2 42.59(10) . . ? O134 Mn3 Mn2 86.00(12) . . ? O118 Mn3 Mn2 138.96(13) . . ? Mn11 Mn3 Mn2 118.79(4) . . ? Mn4 Mn3 Mn2 62.79(3) . . ? O310 Mn3 Mn1 136.88(12) . . ? O311 Mn3 Mn1 137.27(12) . . ? O234 Mn3 Mn1 83.28(11) . . ? O123 Mn3 Mn1 40.15(11) . . ? O134 Mn3 Mn1 40.22(11) . . ? O118 Mn3 Mn1 95.19(12) . . ? Mn11 Mn3 Mn1 177.39(4) . . ? Mn4 Mn3 Mn1 59.13(3) . . ? Mn2 Mn3 Mn1 59.03(3) . . ? O406 Mn4 O405 84.27(18) . . ? O406 Mn4 O134 91.93(17) . . ? O405 Mn4 O134 87.97(17) . . ? O406 Mn4 O234 173.38(17) . . ? O405 Mn4 O234 100.59(17) . . ? O134 Mn4 O234 83.81(16) . . ? O406 Mn4 O112 91.67(19) . . ? O405 Mn4 O112 93.09(19) . . ? O134 Mn4 O112 176.33(18) . . ? O234 Mn4 O112 92.54(18) . . ? O406 Mn4 O124 94.26(17) . . ? O405 Mn4 O124 171.65(17) . . ? O134 Mn4 O124 83.86(16) . . ? O234 Mn4 O124 80.28(16) . . ? O112 Mn4 O124 95.18(18) . . ? O406 Mn4 Mn5 41.74(13) . . ? O405 Mn4 Mn5 43.13(12) . . ? O134 Mn4 Mn5 95.54(12) . . ? O234 Mn4 Mn5 143.59(12) . . ? O112 Mn4 Mn5 87.61(14) . . ? O124 Mn4 Mn5 136.00(12) . . ? O406 Mn4 Mn3 134.33(14) . . ? O405 Mn4 Mn3 89.20(12) . . ? O134 Mn4 Mn3 42.58(11) . . ? O234 Mn4 Mn3 42.09(11) . . ? O112 Mn4 Mn3 133.88(14) . . ? O124 Mn4 Mn3 85.95(11) . . ? Mn5 Mn4 Mn3 122.35(4) . . ? O406 Mn4 Mn1 87.46(12) . . ? O405 Mn4 Mn1 129.39(13) . . ? O134 Mn4 Mn1 42.47(11) . . ? O234 Mn4 Mn1 85.98(11) . . ? O112 Mn4 Mn1 137.08(15) . . ? O124 Mn4 Mn1 42.26(11) . . ? Mn5 Mn4 Mn1 117.67(4) . . ? Mn3 Mn4 Mn1 62.70(3) . . ? O406 Mn4 Mn2 134.30(13) . . ? O405 Mn4 Mn2 140.46(12) . . ? O134 Mn4 Mn2 83.17(11) . . ? O234 Mn4 Mn2 40.24(11) . . ? O112 Mn4 Mn2 93.81(14) . . ? O124 Mn4 Mn2 40.07(11) . . ? Mn5 Mn4 Mn2 175.91(4) . . ? Mn3 Mn4 Mn2 58.93(3) . . ? Mn1 Mn4 Mn2 58.94(3) . . ? O406 Mn5 O405 82.81(17) . . ? O406 Mn5 O211 177.34(19) . . ? O405 Mn5 O211 94.66(18) . . ? O406 Mn5 O110 96.20(19) . . ? O405 Mn5 O110 173.7(2) . . ? O211 Mn5 O110 86.2(2) . . ? O406 Mn5 O19 91.77(19) . . ? O405 Mn5 O19 97.19(18) . . ? O211 Mn5 O19 89.3(2) . . ? O110 Mn5 O19 89.1(2) . . ? O406 Mn5 O212 84.92(19) . . ? O405 Mn5 O212 84.04(19) . . ? O211 Mn5 O212 94.0(2) . . ? O110 Mn5 O212 89.6(2) . . ? O19 Mn5 O212 176.3(2) . . ? O406 Mn5 Mn4 41.11(12) . . ? O405 Mn5 Mn4 42.28(12) . . ? O211 Mn5 Mn4 136.27(14) . . ? O110 Mn5 Mn4 135.56(17) . . ? O19 Mn5 Mn4 101.35(14) . . ? O212 Mn5 Mn4 77.20(13) . . ? O406 Mn6 O107 94.75(17) . . ? O406 Mn6 O18 171.3(2) . . ? O107 Mn6 O18 91.34(19) . . ? O406 Mn6 O210 91.0(2) . . ? O107 Mn6 O210 174.00(19) . . ? O18 Mn6 O210 82.8(2) . . ? O406 Mn6 O29 93.5(2) . . ? O107 Mn6 O29 95.3(2) . . ? O18 Mn6 O29 92.1(3) . . ? O210 Mn6 O29 86.2(3) . . ? O406 Mn6 O6 84.4(2) . . ? O107 Mn6 O6 92.5(2) . . ? O18 Mn6 O6 89.2(3) . . ? O210 Mn6 O6 86.2(3) . . ? O29 Mn6 O6 172.1(2) . . ? O108 Mn7 O107 82.75(16) . . ? O108 Mn7 O15 96.73(18) . . ? O107 Mn7 O15 174.2(2) . . ? O108 Mn7 O28 176.6(2) . . ? O107 Mn7 O28 94.27(18) . . ? O15 Mn7 O28 86.07(19) . . ? O108 Mn7 O27 86.91(17) . . ? O107 Mn7 O27 88.24(17) . . ? O15 Mn7 O27 86.0(2) . . ? O28 Mn7 O27 91.5(2) . . ? O108 Mn7 O16 91.74(17) . . ? O107 Mn7 O16 96.22(18) . . ? O15 Mn7 O16 89.5(2) . . ? O28 Mn7 O16 90.1(2) . . ? O27 Mn7 O16 175.14(18) . . ? O108 Mn7 Mn1 41.51(12) . . ? O107 Mn7 Mn1 42.59(11) . . ? O15 Mn7 Mn1 135.44(14) . . ? O28 Mn7 Mn1 135.25(16) . . ? O27 Mn7 Mn1 78.48(10) . . ? O16 Mn7 Mn1 103.54(13) . . ? O108 Mn8 O208 93.78(16) . . ? O108 Mn8 O13 175.01(19) . . ? O208 Mn8 O13 91.21(19) . . ? O108 Mn8 O26 95.71(19) . . ? O208 Mn8 O26 92.3(2) . . ? O13 Mn8 O26 84.1(2) . . ? O108 Mn8 O14 93.0(2) . . ? O208 Mn8 O14 95.57(18) . . ? O13 Mn8 O14 86.5(2) . . ? O26 Mn8 O14 167.8(2) . . ? O108 Mn8 O25 90.49(19) . . ? O208 Mn8 O25 175.7(2) . . ? O13 Mn8 O25 84.5(2) . . ? O26 Mn8 O25 87.7(3) . . ? O14 Mn8 O25 83.8(2) . . ? O208 Mn9 O209 83.09(16) . . ? O208 Mn9 O23 96.09(18) . . ? O209 Mn9 O23 174.8(2) . . ? O208 Mn9 O114 175.2(2) . . ? O209 Mn9 O114 93.95(17) . . ? O23 Mn9 O114 86.52(18) . . ? O208 Mn9 O24 92.94(17) . . ? O209 Mn9 O24 95.53(17) . . ? O23 Mn9 O24 89.6(2) . . ? O114 Mn9 O24 91.06(19) . . ? O208 Mn9 O215 86.50(17) . . ? O209 Mn9 O215 88.29(17) . . ? O23 Mn9 O215 86.6(2) . . ? O114 Mn9 O215 89.69(19) . . ? O24 Mn9 O215 176.04(17) . . ? O208 Mn9 Mn2 41.90(12) . . ? O209 Mn9 Mn2 42.39(11) . . ? O23 Mn9 Mn2 135.59(15) . . ? O114 Mn9 Mn2 134.37(14) . . ? O24 Mn9 Mn2 103.47(13) . . ? O215 Mn9 Mn2 78.69(12) . . ? O209 Mn10 O310 94.80(16) . . ? O209 Mn10 O214 90.71(18) . . ? O310 Mn10 O214 174.31(18) . . ? O209 Mn10 O117 171.51(18) . . ? O310 Mn10 O117 91.35(18) . . ? O214 Mn10 O117 83.02(19) . . ? O209 Mn10 O116 94.60(19) . . ? O310 Mn10 O116 92.49(17) . . ? O214 Mn10 O116 88.5(2) . . ? O117 Mn10 O116 91.0(2) . . ? O209 Mn10 O10 91.40(18) . . ? O310 Mn10 O10 87.2(2) . . ? O214 Mn10 O10 91.3(3) . . ? O117 Mn10 O10 83.1(2) . . ? O116 Mn10 O10 174.0(2) . . ? O311 Mn11 O310 83.16(16) . . ? O311 Mn11 O217 175.09(19) . . ? O310 Mn11 O217 95.64(17) . . ? O311 Mn11 O213 94.37(17) . . ? O310 Mn11 O213 175.71(18) . . ? O217 Mn11 O213 86.52(17) . . ? O311 Mn11 O216 91.92(18) . . ? O310 Mn11 O216 94.00(16) . . ? O217 Mn11 O216 92.91(18) . . ? O213 Mn11 O216 89.58(18) . . ? O311 Mn11 O218 84.13(18) . . ? O310 Mn11 O218 84.65(17) . . ? O217 Mn11 O218 91.03(19) . . ? O213 Mn11 O218 91.61(19) . . ? O216 Mn11 O218 175.95(17) . . ? O311 Mn11 Mn3 41.84(11) . . ? O310 Mn11 Mn3 41.73(11) . . ? O217 Mn11 Mn3 136.23(13) . . ? O213 Mn11 Mn3 135.32(13) . . ? O216 Mn11 Mn3 98.51(12) . . ? O218 Mn11 Mn3 77.94(11) . . ? O311 Mn12 O405 94.49(17) . . ? O311 Mn12 O111 173.4(2) . . ? O405 Mn12 O111 92.10(19) . . ? O311 Mn12 O113 90.13(19) . . ? O405 Mn12 O113 175.35(19) . . ? O111 Mn12 O113 83.3(2) . . ? O311 Mn12 O121 89.6(2) . . ? O405 Mn12 O121 91.6(2) . . ? O111 Mn12 O121 90.1(3) . . ? O113 Mn12 O121 89.0(2) . . ? O311 Mn12 O120 92.41(19) . . ? O405 Mn12 O120 88.68(19) . . ? O111 Mn12 O120 87.9(2) . . ? O113 Mn12 O120 90.6(2) . . ? O121 Mn12 O120 178.0(2) . . ? Mn1 O107 Mn6 131.4(2) . . ? Mn1 O107 Mn7 94.02(17) . . ? Mn6 O107 Mn7 128.4(2) . . ? Mn1 O108 Mn7 96.32(19) . . ? Mn1 O108 Mn8 133.4(2) . . ? Mn7 O108 Mn8 124.0(2) . . ? Mn3 O123 Mn2 95.44(15) . . ? Mn3 O123 Mn1 100.35(17) . . ? Mn2 O123 Mn1 95.21(15) . . ? Mn4 O124 Mn1 95.51(17) . . ? Mn4 O124 Mn2 99.92(16) . . ? Mn1 O124 Mn2 95.61(16) . . ? Mn4 O134 Mn3 95.24(16) . . ? Mn4 O134 Mn1 95.94(17) . . ? Mn3 O134 Mn1 100.01(17) . . ? Mn2 O208 Mn9 95.49(17) . . ? Mn2 O208 Mn8 132.6(2) . . ? Mn9 O208 Mn8 122.8(2) . . ? Mn2 O209 Mn10 132.2(2) . . ? Mn2 O209 Mn9 94.34(16) . . ? Mn10 O209 Mn9 130.5(2) . . ? Mn3 O234 Mn4 95.58(17) . . ? Mn3 O234 Mn2 95.55(16) . . ? Mn4 O234 Mn2 100.19(16) . . ? Mn3 O310 Mn10 133.6(2) . . ? Mn3 O310 Mn11 95.53(18) . . ? Mn10 O310 Mn11 122.85(19) . . ? Mn12 O311 Mn3 132.5(2) . . ? Mn12 O311 Mn11 130.4(2) . . ? Mn3 O311 Mn11 95.64(18) . . ? Mn12 O405 Mn4 131.2(2) . . ? Mn12 O405 Mn5 128.4(2) . . ? Mn4 O405 Mn5 94.59(18) . . ? Mn4 O406 Mn5 97.15(18) . . ? Mn4 O406 Mn6 134.1(2) . . ? Mn5 O406 Mn6 124.7(2) . . ? C13 O13 Mn8 136.3(4) . . ? C13 O23 Mn9 130.9(4) . . ? O23 C13 O13 126.1(6) . . ? O23 C13 C23 117.7(6) . . ? O13 C13 C23 116.0(6) . . ? C33 C23 C13 118.0(6) . . ? C23 C33 C43 109.4(7) . . ? C23 C33 C63 111.9(7) . . ? C43 C33 C63 108.1(8) . . ? C23 C33 C53 110.6(8) . . ? C43 C33 C53 109.5(8) . . ? C63 C33 C53 107.4(8) . . ? C14 O14 Mn8 134.5(4) . . ? C14 O24 Mn9 132.1(4) . . ? O14 C14 O24 124.3(5) . . ? O14 C14 C24 116.7(5) . . ? O24 C14 C24 119.0(5) . . ? C34 C24 C14 116.6(5) . . ? C24 C34 C64 109.8(6) . . ? C24 C34 C44 110.9(6) . . ? C64 C34 C44 108.8(6) . . ? C24 C34 C54 107.8(5) . . ? C64 C34 C54 108.4(6) . . ? C44 C34 C54 111.1(6) . . ? C15 O15 Mn7 132.1(4) . . ? C15 O25 Mn8 136.1(4) . . ? O25 C15 O15 124.6(6) . . ? O25 C15 C25 123.8(7) . . ? O15 C15 C25 108.7(6) . . ? O25 C15 C25' 111.3(7) . . ? O15 C15 C25' 119.4(7) . . ? C25 C15 C25' 42.6(7) . . ? C35 C25 C15 119.0(8) . . ? C25 C35 C45 108.8(8) . . ? C25 C35 C65 108.9(9) . . ? C45 C35 C65 110.4(9) . . ? C25 C35 C55 110.1(8) . . ? C45 C35 C55 109.4(8) . . ? C65 C35 C55 109.3(9) . . ? C35' C25' C15 114.3(8) . . ? C25' C35' C65' 110.7(9) . . ? C25' C35' C55' 109.7(8) . . ? C65' C35' C55' 111.1(9) . . ? C25' C35' C45' 109.8(9) . . ? C65' C35' C45' 107.9(9) . . ? C55' C35' C45' 107.5(9) . . ? C16 O16 Mn7 130.2(4) . . ? C16 O26 Mn8 134.7(4) . . ? O26 C16 O16 125.9(5) . . ? O26 C16 C26 117.3(5) . . ? O16 C16 C26 116.9(5) . . ? C36 C26 C16 118.2(5) . . ? C56 C36 C26 110.2(6) . . ? C56 C36 C46 111.5(7) . . ? C26 C36 C46 108.9(6) . . ? C56 C36 C66 108.8(6) . . ? C26 C36 C66 109.4(6) . . ? C46 C36 C66 107.8(6) . . ? C17 O17 Mn1 127.1(3) . . ? C17 O27 Mn7 122.0(3) . . ? O27 C17 O17 125.4(5) . . ? O27 C17 C27 119.4(5) . . ? O17 C17 C27 115.2(4) . . ? C37 C27 C17 115.0(5) . . ? C67 C37 C47 111.3(6) . . ? C67 C37 C57 108.7(6) . . ? C47 C37 C57 109.2(6) . . ? C67 C37 C27 109.4(6) . . ? C47 C37 C27 107.4(6) . . ? C57 C37 C27 110.9(5) . . ? C18 O18 Mn6 137.9(5) . . ? C18 O28 Mn7 129.8(4) . . ? O28 C18 O18 124.3(6) . . ? O28 C18 C28 117.6(6) . . ? O18 C18 C28 115.2(7) . . ? O28 C18 C28' 111.5(7) . . ? O18 C18 C28' 114.0(8) . . ? C28 C18 C28' 51.9(9) . . ? C38 C28 C18 115.1(7) . . ? C28 C38 C58 112.1(8) . . ? C28 C38 C68 109.4(9) . . ? C58 C38 C68 109.3(9) . . ? C28 C38 C48 110.8(8) . . ? C58 C38 C48 107.9(8) . . ? C68 C38 C48 107.1(9) . . ? C38' C28' C18 116.5(8) . . ? C28' C38' C48' 109.7(10) . . ? C28' C38' C58' 109.3(9) . . ? C48' C38' C58' 109.6(9) . . ? C28' C38' C68' 108.8(8) . . ? C48' C38' C68' 110.5(9) . . ? C58' C38' C68' 108.9(9) . . ? C19 O19 Mn5 123.3(5) . . ? C19 O29 Mn6 135.4(5) . . ? O29 C19 O19 126.4(6) . . ? O29 C19 C29 113.8(6) . . ? O19 C19 C29 119.3(6) . . ? C39 C29 C19 115.2(6) . . ? C59 C39 C29 113.1(7) . . ? C59 C39 C49 111.4(7) . . ? C29 C39 C49 110.3(7) . . ? C59 C39 C69 109.5(7) . . ? C29 C39 C69 104.1(7) . . ? C49 C39 C69 108.2(7) . . ? C110 O110 Mn5 131.8(4) . . ? C110 O210 Mn6 129.9(5) . . ? O210 C110 O110 125.7(6) . . ? O210 C110 C210 117.4(6) . . ? O110 C110 C210 116.6(6) . . ? C310 C210 C110 114.7(6) . . ? C210 C310 C510 110.8(8) . . ? C210 C310 C410 111.5(7) . . ? C510 C310 C410 107.8(8) . . ? C210 C310 C610 108.3(7) . . ? C510 C310 C610 109.5(8) . . ? C410 C310 C610 108.9(8) . . ? C111 O111 Mn12 136.9(4) . . ? C111 O211 Mn5 133.0(4) . . ? O211 C111 O111 125.8(6) . . ? O211 C111 C211 117.9(5) . . ? O111 C111 C211 116.2(5) . . ? C311 C211 C111 115.4(5) . . ? C511 C311 C211 110.4(6) . . ? C511 C311 C611 108.5(7) . . ? C211 C311 C611 110.9(7) . . ? C511 C311 C411 108.9(7) . . ? C211 C311 C411 107.8(6) . . ? C611 C311 C411 110.3(7) . . ? C112 O112 Mn4 125.5(4) . . ? C112 O212 Mn5 123.3(4) . . ? O212 C112 O112 126.2(6) . . ? O212 C112 C212 119.3(6) . . ? O112 C112 C212 114.3(6) . . ? C312 C212 C112 119.9(6) . . ? C212 C312 C412 111.2(7) . . ? C212 C312 C612 110.7(6) . . ? C412 C312 C612 108.8(7) . . ? C212 C312 C512 110.6(7) . . ? C412 C312 C512 107.0(8) . . ? C612 C312 C512 108.3(7) . . ? C113 O113 Mn12 132.0(4) . . ? C113 O213 Mn11 131.7(4) . . ? O213 C113 O113 125.6(5) . . ? O213 C113 C213 118.0(5) . . ? O113 C113 C213 116.4(5) . . ? C313 C213 C113 116.4(5) . . ? C213 C313 C513 110.4(6) . . ? C213 C313 C613 108.5(6) . . ? C513 C313 C613 109.0(6) . . ? C213 C313 C413 109.4(6) . . ? C513 C313 C413 109.8(7) . . ? C613 C313 C413 109.7(6) . . ? C114 O114 Mn9 132.0(4) . . ? C114 O214 Mn10 138.1(4) . . ? O214 C114 O114 125.5(5) . . ? O214 C114 C214 117.0(5) . . ? O114 C114 C214 117.5(5) . . ? C314 C214 C114 116.9(5) . . ? C214 C314 C614 110.8(6) . . ? C214 C314 C414 111.4(6) . . ? C614 C314 C414 107.8(7) . . ? C214 C314 C514 108.5(6) . . ? C614 C314 C514 109.0(7) . . ? C414 C314 C514 109.4(7) . . ? C115 O115 Mn2 126.5(4) . . ? C115 O215 Mn9 121.5(4) . . ? O215 C115 O115 126.0(5) . . ? O215 C115 C215 119.8(5) . . ? O115 C115 C215 114.2(5) . . ? C315 C215 C115 115.3(5) . . ? C415 C315 C215 109.7(6) . . ? C415 C315 C615 110.2(6) . . ? C215 C315 C615 110.4(6) . . ? C415 C315 C515 111.2(7) . . ? C215 C315 C515 106.6(6) . . ? C615 C315 C515 108.7(6) . . ? C116 O116 Mn10 130.9(4) . . ? C116 O216 Mn11 124.0(4) . . ? O216 C116 O116 124.3(6) . . ? O216 C116 C216 119.1(6) . . ? O116 C116 C216 116.3(5) . . ? C316 C216 C116 115.3(6) . . ? C416 C316 C216 110.3(6) . . ? C416 C316 C516 111.0(7) . . ? C216 C316 C516 108.8(6) . . ? C416 C316 C616 109.2(6) . . ? C216 C316 C616 108.7(6) . . ? C516 C316 C616 108.9(7) . . ? C117 O117 Mn10 132.0(4) . . ? C117 O217 Mn11 132.0(4) . . ? O217 C117 O117 126.1(5) . . ? O217 C117 C217 117.8(5) . . ? O117 C117 C217 116.1(5) . . ? C327 C217 C317 31.2(9) . . ? C327 C217 C117 115.9(7) . . ? C317 C217 C117 115.5(6) . . ? C217 C317 C617 110.0(7) . . ? C217 C317 C417 108.2(8) . . ? C617 C317 C417 109.1(8) . . ? C217 C317 C517 110.4(8) . . ? C617 C317 C517 109.3(8) . . ? C417 C317 C517 109.8(8) . . ? C217 C327 C627 110.4(10) . . ? C217 C327 C427 109.5(10) . . ? C627 C327 C427 109.3(9) . . ? C217 C327 C527 109.9(9) . . ? C627 C327 C527 107.7(9) . . ? C427 C327 C527 110.0(10) . . ? C118 O118 Mn3 125.2(4) . . ? C118 O218 Mn11 123.0(4) . . ? O218 C118 O118 126.1(5) . . ? O218 C118 C218 119.1(5) . . ? O118 C118 C218 114.8(5) . . ? C318 C218 C118 119.5(6) . . ? C218 C318 C618 111.6(7) . . ? C218 C318 C518 109.1(8) . . ? C618 C318 C518 107.0(8) . . ? C218 C318 C418 109.2(6) . . ? C618 C318 C418 110.5(7) . . ? C518 C318 C418 109.3(7) . . ? O3A N1A O2A 117.6(17) . . ? O3A N1A C1A 120.4(16) . . ? O2A N1A C1A 121.6(15) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 17.26 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.063 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.114