Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_xekb35 _database_code_CSD 189138 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Brechin, Euan Kenneth' 'Christou, George' 'Davidson, James' 'Parsons, S.' 'Soler, Monica' _publ_contact_author_name 'Dr Euan Kenneth Brechin' _publ_contact_author_address ; Chemistry Manchester University Oxford Road Manchester M13 9PL UNITED KINGDOM ; _publ_contact_author_email 'EUAN.K.BRECHIN@MAN.AC.UK' _publ_requested_journal 'Chemical Communications' _publ_section_title ; A new class of single-molecule magnet: [Mn9O7(OAc)11(thme)(py)3(H2O)2] with an S = 17/2 ground state ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Mn9O7(H2O)2(OAc)11(pyr)3(MeC(CH2O)3)].3MeCN.Et2O' _chemical_formula_sum 'C52 H80 Mn9 N6 O35' _chemical_formula_weight 1843.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.745(3) _cell_length_b 23.688(5) _cell_length_c 23.259(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.49(3) _cell_angle_gamma 90.00 _cell_volume 7524(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6826 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26.5 _exptl_crystal_description block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3756 _exptl_absorpt_coefficient_mu 1.546 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BrukerSmart APEX CCD' _diffrn_measurement_method 'Omega at different phi settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42819 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.42 _reflns_number_total 15403 _reflns_number_gt 13552 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution DIRDIF _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; This section contains -a short description of refinement problems -Xprep output (reciprocal space exploration) -the final shelx .res file -a set of coordinates in shelx format of the disordered solvent region before we gave up and used squeeze. -the checkcif output. A cluster of difference map peaks in the region of the hexagon of oxygen atoms attached to Mn4-9 were interpreted as part-weight acetates. Refinement of C-atom occupancies with the constraint that chemically equivalent C-atoms had equal isotropic displacement parameters suggested that opposite edges of the oxygen hexagon were equally occupied by acetate, with a strong preference for the sites labelled C110, C210, C111 and C211 in this cif. This is inconsistent with occupancy of this site by three acetates, and so the total acetate occupancy in this region was restrained to be 2, with opposite actates having equal occupancy. In the three possible configurations the oxygen atoms not attached to C were assumed to be H2O. Part weight H-atoms have not been placed on these sites. This interpretation is consistent with the chemical analysis results. The acetates were restrained to be geometrically similar; the major component C-atoms were refined with adps the minor component only isotropically. The lattice contains four solvent regions: two of these are occupied by well-behaved MeCN. Of the other two sites, one contains disodered MeCN, the other seemed to contain mostly Et2O, but was very badly disordered. These two regions were treated in the manner described by van der Sluis and Spek. This treated 276 e per cell, or 69 e per formula unit. This fits quite well with 1MeCN and 1Et2O (=66e) for formula unit. The values of F(000), the density, mu etc reflect this assumption. Xprep output follows: ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + xehb35 started at 12:25:32 on 27-Jun-2002 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.745 23.688 23.259 90.00 96.49 90.00 43450 Reflections read from file xehb35.hkl; mean (I/sigma) = 13.67 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 21729 21708 21701 21718 32569 28974 28941 43450 N (int>3sigma) = 0 16807 16526 16809 16663 25071 22460 22455 33695 Mean intensity = 0.0 200.1 181.1 195.9 193.8 192.3 195.3 194.6 194.4 Mean int/sigma = 0.0 13.9 13.1 13.7 13.5 13.6 13.7 13.7 13.7 Lattice type: P chosen Volume: 7524.21 #------------------------------------------------------------------------------ DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 13.745 23.259 23.688 90.00 90.00 96.49 Niggli form: a.a = 188.91 b.b = 541.00 c.c = 561.13 b.c = 0.00 a.c = 0.00 a.b = -36.15 #------------------------------------------------------------------------------ Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) #----------------------------------------------------------------------------- Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.023 [ 14481] Cell: 13.745 23.688 23.259 90.00 96.49 90.00 Volume: 7524.21 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected #------------------------------------------------------------------------------ SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 21729 21708 21701 21718 32569 28974 28941 43450 N (int>3sigma) = 0 16807 16526 16809 16663 25071 22460 22455 33695 Mean intensity = 0.0 200.1 181.1 195.9 193.8 192.3 195.3 194.6 194.4 Mean int/sigma = 0.0 13.9 13.1 13.7 13.5 13.6 13.7 13.7 13.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.947 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 24 607 604 605 N I>3s 1 274 273 17 2.0 284.1 285.5 1.9 1.2 13.6 13.6 1.0 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.023 14481 1.2 / 13.6 0.84 Option [A] chosen #------------------------------------------------------------------------------ INTENSITY STATISTICS FOR DATASET # 1 xehb35.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 798 799 99.9 3.75 678.2 78.30 0.0152 0.0079 2.20 - 1.70 893 893 100.0 3.85 428.9 51.90 0.0182 0.0121 1.70 - 1.45 1016 1016 100.0 3.76 355.4 41.74 0.0232 0.0156 1.45 - 1.30 1033 1036 99.7 3.40 247.0 29.28 0.0340 0.0223 1.30 - 1.20 1010 1011 99.9 3.16 147.5 20.53 0.0365 0.0330 1.20 - 1.10 1384 1385 99.9 2.92 127.3 17.24 0.0383 0.0391 1.10 - 1.05 894 896 99.8 2.76 109.0 14.72 0.0390 0.0462 1.05 - 1.00 1105 1105 100.0 2.62 102.3 13.63 0.0425 0.0505 1.00 - 0.95 1340 1343 99.8 2.49 83.8 11.45 0.0478 0.0593 0.95 - 0.90 1641 1647 99.6 2.33 70.7 10.20 0.0543 0.0691 0.90 - 0.85 2045 2049 99.8 2.20 70.7 9.48 0.0531 0.0719 0.85 - 0.80 2600 2619 99.3 2.02 59.3 8.29 0.0581 0.0841 0.80 - 0.80 42 88 47.7 0.70 42.1 5.46 0.1329 0.1295 #----------------------------------------------------------------------------- 0.90 - 0.80 4687 4756 98.5 2.08 64.1 8.78 0.0558 0.0785 Inf - 0.80 15801 15887 99.5 2.73 164.9 20.73 0.0285 0.0309 Merged [A], lowest resolution = 23.69 Angstroms, 818 outliers downweighted #------------------------------------------------------------------------------ #The final shelxl .res file follows: #TITL XEHB35 in P21/n solved dirdif #REM Simon Parsons & James Davidson (Edinburgh) for Euan Brechin (Manchester) #REM [Mn9O7(OAc)11(pyr)3(MeC(CH2O)3)].3MeCN.Et2O #REM 276 e/cell corrected with van der Sluis & Spek method #REM (=1MeCN and 1Et2O per form. unit) SFAC & UNIT include this. #CELL 0.71073 13.74450 23.68810 23.25930 90.0000 96.4930 90.0000 #ZERR 4.000 0.00270 0.00470 0.00470 0.0000 0.0300 0.0000 #LATT +1 #SYMM 1/2-X , 1/2+Y , 1/2-Z #SFAC C H N O MN #UNIT 208 320 24 140 36 #OMIT 0 1 1 #TEMP -123 #L.S. 4 #ACTA #FMAP 2 #PLAN 10 #SUMP 1 0.0001 1 2 1 3 1 4 #WGHT 0.045500 3.770000 #EXTI 0.000200 #FVAR 0.60487 0.59278 0.18964 0.21759 #MN1 5 0.115808 -0.203895 0.757796 11.00000 0.01320 0.01499 = #0.01672 0.00067 -0.00055 -0.00056 #MN2 5 -0.048302 -0.272683 0.779568 11.00000 0.01441 0.01484 = #0.01699 0.00053 0.00000 -0.00062 #MN3 5 -0.074319 -0.184104 0.690680 11.00000 0.01416 0.01525 = #0.01684 0.00059 -0.00105 0.00025 #MN4 5 0.066971 -0.059963 0.720908 11.00000 0.01961 0.01697 = #0.03536 0.00422 -0.00634 -0.00166 #MN5 5 0.212649 -0.130453 0.835774 11.00000 0.02156 0.01771 = #0.01966 0.00229 -0.00473 -0.00534 #MN6 5 0.112087 -0.243319 0.899406 11.00000 0.01631 0.01947 = #0.01630 0.00179 -0.00111 -0.00188 #MN7 5 -0.132179 -0.279068 0.881677 11.00000 0.01601 0.02272 = #0.01956 0.00391 0.00168 -0.00104 #MN8 5 -0.278292 -0.204517 0.769181 11.00000 0.01534 0.02823 = #0.02743 0.00587 0.00159 0.00241 #MN9 5 -0.189455 -0.090216 0.691158 11.00000 0.01529 0.01541 = #0.02537 0.00211 0.00069 0.00147 #REM OXIDE #O1 4 -0.018276 -0.195198 0.769544 11.00000 0.01407 0.01337 = #0.01652 0.00098 -0.00031 -0.00078 #O2 4 0.143619 -0.129065 0.762415 11.00000 0.01895 0.01634 = #0.01819 0.00160 -0.00118 -0.00224 #O3 4 0.155558 -0.203795 0.836916 11.00000 0.01794 0.01799 = #0.01788 0.00092 -0.00227 -0.00347 #O4 4 -0.003687 -0.271837 0.858554 11.00000 0.01684 0.02156 = #0.01682 0.00163 0.00023 -0.00229 #O5 4 -0.166882 -0.260139 0.804449 11.00000 0.01417 0.02192 = #0.01884 0.00005 0.00116 0.00005 #O6 4 -0.195998 -0.167584 0.707402 11.00000 0.01430 0.01771 = #0.02428 0.00268 0.00115 0.00024 #O7 4 -0.056459 -0.108525 0.691495 11.00000 0.01731 0.01478 = #0.02264 0.00328 -0.00078 0.00021 #REM ACETATE numbered 1-11 #O11 4 0.242930 -0.224723 0.736772 11.00000 0.01561 0.02297 = #0.02535 0.00017 0.00144 -0.00030 #O21 4 0.338207 -0.171719 0.800092 11.00000 0.01912 0.02871 = #0.03850 -0.00123 -0.00393 -0.00363 #C11 1 0.326773 -0.207841 0.761291 11.00000 0.01555 0.02412 = #0.03144 0.00722 0.00004 -0.00200 #C21 1 0.414274 -0.235734 0.739582 11.00000 0.01507 0.03771 = #0.06633 -0.00396 0.00563 -0.00074 #AFIX 137 #H21A 2 0.468498 -0.208711 0.741138 11.00000 -1.50000 #H21B 2 0.397003 -0.248196 0.699553 11.00000 -1.50000 #H21C 2 0.434171 -0.268416 0.763953 11.00000 -1.50000 #AFIX 0 #O12 4 -0.065345 -0.353502 0.775258 11.00000 0.02215 0.01560 = #0.02836 0.00052 0.00108 -0.00269 #O22 4 -0.134592 -0.369493 0.856723 11.00000 0.03004 0.02190 = #0.03676 0.00700 0.00887 -0.00211 #C12 1 -0.104315 -0.385749 0.811070 11.00000 0.02549 0.01908 = #0.04006 0.00188 0.00505 -0.00196 #C22 1 -0.111467 -0.446708 0.793970 11.00000 0.07857 0.02269 = #0.07728 -0.00250 0.04235 -0.01006 #AFIX 137 #H22A 2 -0.059497 -0.468096 0.816671 11.00000 -1.50000 #H22B 2 -0.104160 -0.450323 0.752705 11.00000 -1.50000 #H22C 2 -0.175421 -0.461584 0.801347 11.00000 -1.50000 #AFIX 0 #O13 4 -0.110023 -0.187700 0.607899 11.00000 0.02303 0.02140 = #0.01918 0.00123 -0.00308 0.00259 #O23 4 -0.205631 -0.110273 0.596582 11.00000 0.02934 0.02642 = #0.02464 0.00134 -0.00505 0.00817 #C13 1 -0.162534 -0.150628 0.577003 11.00000 0.02243 0.02212 = #0.02213 0.00109 -0.00339 -0.00501 #C23 1 -0.169236 -0.159849 0.512794 11.00000 0.04966 0.03358 = #0.02184 0.00053 -0.01041 0.00560 #AFIX 137 #H23A 2 -0.220539 -0.187635 0.501170 11.00000 -1.50000 #H23B 2 -0.106313 -0.173834 0.502594 11.00000 -1.50000 #H23C 2 -0.185230 -0.124096 0.492719 11.00000 -1.50000 #AFIX 0 #O14 4 0.198869 -0.014406 0.751058 11.00000 0.03436 0.02752 = #0.05238 0.01455 -0.01749 -0.01118 #O24 4 0.277984 -0.058319 0.827806 11.00000 0.03536 0.02228 = #0.02772 0.00427 -0.00832 -0.01121 #C14 1 0.267298 -0.018942 0.790551 11.00000 0.02396 0.01927 = #0.03611 -0.00253 -0.00085 -0.00675 #C24 1 0.344785 0.026100 0.796138 11.00000 0.04132 0.03392 = #0.05201 0.01307 -0.01201 -0.01918 #AFIX 137 #H24A 2 0.347690 0.044192 0.758479 11.00000 -1.50000 #H24B 2 0.408411 0.009065 0.809261 11.00000 -1.50000 #H24C 2 0.328784 0.054415 0.824316 11.00000 -1.50000 #AFIX 0 #O15 4 0.289590 -0.140396 0.912239 11.00000 0.03575 0.02527 = #0.02606 0.00403 -0.01312 -0.01159 #O25 4 0.232286 -0.220495 0.948340 11.00000 0.02143 0.02748 = #0.02324 0.00349 -0.00444 -0.00457 #C15 1 0.290968 -0.179600 0.948833 11.00000 0.02169 0.02352 = #0.02187 -0.00282 -0.00353 -0.00022 #C25 1 0.370384 -0.177457 0.998740 11.00000 0.03364 0.04079 = #0.02780 0.00589 -0.01292 -0.00942 #AFIX 137 #H25A 2 0.352434 -0.150310 1.027536 11.00000 -1.50000 #H25B 2 0.431951 -0.165719 0.984808 11.00000 -1.50000 #H25C 2 0.378596 -0.214945 1.016446 11.00000 -1.50000 #AFIX 0 #O16 4 0.080960 -0.285037 0.968092 11.00000 0.02528 0.03794 = #0.01916 0.00722 -0.00103 -0.00729 #O26 4 -0.079439 -0.306282 0.959642 11.00000 0.02093 0.04339 = #0.02365 0.01129 0.00143 -0.00107 #C16 1 0.006899 -0.309817 0.983871 11.00000 0.02587 0.02828 = #0.02012 0.00297 0.00310 0.00040 #C26 1 0.023500 -0.345931 1.037313 11.00000 0.03234 0.05053 = #0.03238 0.02005 -0.00403 -0.00498 #AFIX 137 #H26A 2 0.092693 -0.356706 1.044022 11.00000 -1.50000 #H26B 2 -0.017035 -0.379976 1.032033 11.00000 -1.50000 #H26C 2 0.005651 -0.324627 1.070684 11.00000 -1.50000 #AFIX 0 #O17 4 -0.266193 -0.287295 0.901985 11.00000 0.01892 0.03282 = #0.02885 0.00531 0.00520 -0.00005 #O27 4 -0.361775 -0.240337 0.834065 11.00000 0.02125 0.07090 = #0.04488 0.02483 0.00827 0.00914 #C17 1 -0.347150 -0.265706 0.880523 11.00000 0.01948 0.02676 = #0.03373 -0.00037 0.00655 -0.00467 #C27 1 -0.430738 -0.271039 0.916905 11.00000 0.02635 0.03806 = #0.04142 0.00126 0.01220 -0.00035 #AFIX 137 #H27A 2 -0.415419 -0.249777 0.952935 11.00000 -1.50000 #H27B 2 -0.440559 -0.310901 0.925938 11.00000 -1.50000 #H27C 2 -0.490584 -0.255906 0.895496 11.00000 -1.50000 #AFIX 0 #O18 4 -0.391909 -0.149571 0.733004 11.00000 0.01806 0.03767 = #0.05291 0.01651 0.00602 0.00352 #O28 4 -0.332975 -0.079127 0.682975 11.00000 0.01786 0.02292 = #0.04359 0.00402 0.00238 0.00275 #C18 1 -0.401557 -0.106884 0.701851 11.00000 0.01946 0.02434 = #0.03014 -0.00179 -0.00091 0.00261 #C28 1 -0.504412 -0.085721 0.684979 11.00000 0.01880 0.03876 = #0.05990 0.01084 0.00101 0.00505 #AFIX 137 #H28A 2 -0.547800 -0.117794 0.674376 11.00000 -1.50000 #H28B 2 -0.504911 -0.060057 0.651900 11.00000 -1.50000 #H28C 2 -0.527306 -0.065573 0.717706 11.00000 -1.50000 #AFIX 0 #O19 4 -0.172624 -0.010103 0.669504 11.00000 0.02162 0.01807 = #0.03761 0.00494 0.00232 0.00130 #O29 4 -0.012127 0.009851 0.679076 11.00000 0.02519 0.02385 = #0.06899 0.01626 -0.00759 -0.00198 #C19 1 -0.099917 0.022136 0.666329 11.00000 0.02560 0.02104 = #0.02410 0.00154 0.00033 0.00201 #C29 1 -0.123202 0.080947 0.643802 11.00000 0.03016 0.02543 = #0.05718 0.01454 0.00093 0.00071 #AFIX 137 #H29A 2 -0.087309 0.108593 0.669403 11.00000 -1.50000 #H29B 2 -0.193699 0.087843 0.642659 11.00000 -1.50000 #H29C 2 -0.103712 0.084575 0.604723 11.00000 -1.50000 #AFIX 0 #REM disordered H2O/OAc starts here #SAME O210 O110 C110 C210 #SAME O111 O211 C111 C211 #SAME O1W O210 C310 C410 #SAME O2W O211 C311 C411 #SAME O110 O2W C510 C610 #SAME O111 O1W C511 C611 #O110 4 -0.236812 -0.137626 0.834274 11.00000 0.04298 0.04921 = #0.04241 -0.01595 0.00120 0.01367 #O210 4 -0.181651 -0.059261 0.780601 11.00000 0.03453 0.03006 = #0.02910 -0.00289 0.00587 -0.00311 #PART 1 #C110 1 -0.205408 -0.083377 0.826300 21.00000 0.02207 0.02070 = #0.02706 -0.00709 -0.00020 0.00208 #C210 1 -0.199700 -0.046090 0.880140 21.00000 0.05956 0.03831 = #0.03277 -0.00993 0.01715 -0.01507 #AFIX 137 #H21D 2 -0.141198 -0.022226 0.881881 21.00000 -1.50000 #H21E 2 -0.196083 -0.069934 0.914748 21.00000 -1.50000 #H21F 2 -0.258158 -0.022184 0.878340 21.00000 -1.50000 #AFIX 0 #PART 2 #C310 1 -0.093417 -0.039607 0.810887 31.00000 0.03062 #C410 1 -0.113467 -0.016129 0.870522 31.00000 0.05111 #AFIX 137 #H41A 2 -0.150282 0.019262 0.865082 31.00000 -1.50000 #H41B 2 -0.051113 -0.009102 0.894277 31.00000 -1.50000 #H41C 2 -0.151699 -0.043683 0.889964 31.00000 -1.50000 #AFIX 0 #PART 3 #C510 1 -0.186468 -0.148682 0.890231 41.00000 0.03413 #C610 1 -0.183243 -0.096226 0.929491 41.00000 0.05192 #AFIX 137 #H61A 2 -0.217327 -0.104375 0.963351 41.00000 -1.50000 #H61B 2 -0.215411 -0.064542 0.907918 41.00000 -1.50000 #H61C 2 -0.114938 -0.086374 0.942193 41.00000 -1.50000 #AFIX 0 #PART 0 #O111 4 0.105990 -0.087762 0.883400 11.00000 0.04274 0.03471 = #0.03023 -0.00364 0.00562 0.00438 #O211 4 0.048397 -0.166706 0.936733 11.00000 0.03049 0.03928 = #0.04168 -0.01056 0.00604 0.00657 #PART 1 #C111 1 0.064754 -0.111832 0.926545 21.00000 0.02003 0.02477 = #0.02358 -0.00459 -0.00296 0.00097 #C211 1 0.034582 -0.070319 0.970860 21.00000 0.07047 0.02950 = #0.04072 -0.00572 0.02302 0.00483 #AFIX 137 #H21G 2 0.076910 -0.075074 1.007366 21.00000 -1.50000 #H21H 2 -0.033634 -0.077330 0.977260 21.00000 -1.50000 #H21I 2 0.040966 -0.031717 0.956602 21.00000 -1.50000 #AFIX 0 #PART 2 #C311 1 -0.051742 -0.166464 0.940531 31.00000 0.02633 #C411 1 -0.073353 -0.119955 0.983858 31.00000 0.03626 #AFIX 137 #H41D 2 -0.129388 -0.097382 0.967296 31.00000 -1.50000 #H41E 2 -0.015841 -0.095540 0.991794 31.00000 -1.50000 #H41F 2 -0.088542 -0.137433 1.019976 31.00000 -1.50000 #AFIX 0 #PART 3 #C511 1 0.039951 -0.045059 0.858829 41.00000 0.03273 #C611 1 0.009948 -0.004344 0.905275 41.00000 0.05237 #AFIX 137 #H61D 2 -0.015337 -0.026019 0.936258 41.00000 -1.50000 #H61E 2 -0.041014 0.021305 0.887812 41.00000 -1.50000 #H61F 2 0.067086 0.017612 0.921332 41.00000 -1.50000 #AFIX 0 #PART 0 #O1W 4 0.006502 -0.030975 0.800269 11.00000 0.04073 0.04455 = #0.05259 -0.01859 -0.00021 0.00981 #O2W 4 -0.137638 -0.193463 0.917512 11.00000 0.03353 0.03007 = #0.03294 -0.00445 0.00555 -0.00033 #REM Pyridine numbered A, B, C #N1A 3 0.129509 -0.078598 0.636128 11.00000 0.02894 0.03453 = #0.03311 0.00952 0.00226 -0.00503 #C2A 1 0.218248 -0.101603 0.636402 11.00000 0.02736 0.06549 = #0.04352 0.00752 0.00173 -0.00032 #AFIX 43 #H2A 2 0.259562 -0.103318 0.671977 11.00000 -1.20000 #AFIX 0 #C3A 1 0.252929 -0.123161 0.586985 11.00000 0.03815 0.08228 = #0.06021 -0.00333 0.01455 0.00090 #AFIX 43 #H3A 2 0.316608 -0.139176 0.589165 11.00000 -1.20000 #AFIX 0 #C4A 1 0.195002 -0.121199 0.535299 11.00000 0.05556 0.07603 = #0.04778 -0.00812 0.01635 -0.00993 #AFIX 43 #H4A 2 0.217225 -0.135345 0.500861 11.00000 -1.20000 #AFIX 0 #C5A 1 0.102318 -0.097722 0.535012 11.00000 0.06265 0.08727 = #0.03362 0.00050 -0.00361 -0.00373 #AFIX 43 #H5A 2 0.059533 -0.095809 0.500007 11.00000 -1.20000 #AFIX 0 #C6A 1 0.072442 -0.077077 0.586016 11.00000 0.03801 0.05906 = #0.03881 0.00774 -0.00226 0.00242 #AFIX 43 #H6A 2 0.008778 -0.061249 0.585101 11.00000 -1.20000 #AFIX 0 #N1B 3 0.198132 -0.320715 0.877003 11.00000 0.02413 0.02470 = #0.01796 0.00181 -0.00433 0.00183 #C2B 1 0.288146 -0.314544 0.860709 11.00000 0.02274 0.03170 = #0.03033 0.00109 -0.00164 0.00221 #AFIX 43 #H2B 2 0.314365 -0.277550 0.859034 11.00000 -1.20000 #AFIX 0 #C3B 1 0.344272 -0.359581 0.846284 11.00000 0.02809 0.04620 = #0.04563 -0.00643 0.00662 0.01051 #AFIX 43 #H3B 2 0.407983 -0.353539 0.835340 11.00000 -1.20000 #AFIX 0 #C4B 1 0.306609 -0.413631 0.847957 11.00000 0.05186 0.03660 = #0.04983 -0.01592 -0.00005 0.01865 #AFIX 43 #H4B 2 0.344074 -0.445302 0.838461 11.00000 -1.20000 #AFIX 0 #C5B 1 0.214492 -0.420554 0.863532 11.00000 0.05602 0.02428 = #0.04308 -0.00727 -0.00444 0.00080 #AFIX 43 #H5B 2 0.186592 -0.457181 0.864573 11.00000 -1.20000 #AFIX 0 #C6B 1 0.161939 -0.373373 0.877864 11.00000 0.03388 0.02631 = #0.02936 -0.00103 -0.00259 -0.00099 #AFIX 43 #H6B 2 0.097940 -0.378593 0.888685 11.00000 -1.20000 #AFIX 0 #N1C 3 -0.324254 -0.272926 0.702584 11.00000 0.02258 0.03453 = #0.03942 0.00308 -0.00384 -0.00611 #C2C 1 -0.314303 -0.326955 0.716951 11.00000 0.04898 0.03853 = #0.05928 0.00185 -0.00890 -0.01091 #AFIX 43 #H2C 2 -0.305777 -0.336679 0.756828 11.00000 -1.20000 #AFIX 0 #C3C 1 -0.315793 -0.369882 0.676346 11.00000 0.08747 0.04379 = #0.09443 -0.01096 -0.02006 -0.00492 #AFIX 43 #H3C 2 -0.307517 -0.408144 0.688130 11.00000 -1.20000 #AFIX 0 #C4C 1 -0.329611 -0.355744 0.618243 11.00000 0.08103 0.08036 = #0.07051 -0.03797 -0.00706 -0.00451 #AFIX 43 #H4C 2 -0.330503 -0.384191 0.589398 11.00000 -1.20000 #AFIX 0 #C5C 1 -0.342049 -0.299824 0.602857 11.00000 0.05297 0.07838 = #0.04544 -0.01020 -0.00477 -0.00766 #AFIX 43 #H5C 2 -0.354160 -0.288989 0.563370 11.00000 -1.20000 #AFIX 0 #C6C 1 -0.336477 -0.260357 0.645994 11.00000 0.03401 0.04863 = #0.03788 0.00061 -0.00680 -0.00520 #AFIX 43 #H6C 2 -0.341570 -0.221690 0.635239 11.00000 -1.20000 #AFIX 0 #REM trihydroxymethylethane starts here #O1T 4 0.084210 -0.283915 0.760290 11.00000 0.01443 0.01432 = #0.01971 -0.00087 0.00061 0.00136 #C1T 1 0.103435 -0.321022 0.714633 11.00000 0.01931 0.01673 = #0.02428 -0.00257 0.00234 0.00313 #AFIX 23 #H1T1 2 0.082744 -0.359678 0.723939 11.00000 -1.20000 #H1T2 2 0.174838 -0.321876 0.712102 11.00000 -1.20000 #AFIX 0 #O2T 4 -0.095433 -0.266654 0.698533 11.00000 0.01632 0.01690 = #0.01702 -0.00176 -0.00024 -0.00106 #C2T 1 -0.060467 -0.304890 0.657311 11.00000 0.02157 0.01862 = #0.01928 -0.00390 -0.00220 0.00171 #AFIX 23 #H2T1 2 -0.092935 -0.295559 0.618291 11.00000 -1.20000 #H2T2 2 -0.080041 -0.343760 0.666607 11.00000 -1.20000 #AFIX 0 #O3T 4 0.063715 -0.200312 0.677743 11.00000 0.01407 0.01880 = #0.01618 0.00029 -0.00039 0.00115 #C3T 1 0.085015 -0.244446 0.638770 11.00000 0.02237 0.02228 = #0.01642 -0.00070 0.00173 0.00136 #AFIX 23 #H3T1 2 0.156620 -0.245594 0.637011 11.00000 -1.20000 #H3T2 2 0.053400 -0.235169 0.599538 11.00000 -1.20000 #AFIX 0 #C4T 1 0.050523 -0.303607 0.655683 11.00000 0.02014 0.01998 = #0.02003 -0.00389 0.00152 0.00105 #C5T 1 0.076394 -0.346222 0.610247 11.00000 0.02863 0.02844 = #0.02385 -0.00557 0.00184 0.00424 #AFIX 137 #H5T1 2 0.147637 -0.350865 0.613215 11.00000 -1.50000 #H5T2 2 0.052299 -0.332413 0.571524 11.00000 -1.50000 #H5T3 2 0.045796 -0.382648 0.616937 11.00000 -1.50000 #AFIX 0 #REM Two MeCN's of solvation. One MeCN and one Et2O squeezed out. #N1Y 3 0.621987 0.038441 0.930039 11.00000 0.30448 0.07410 = #0.13138 -0.00319 0.05956 0.05221 #C2Y 1 0.642488 0.022744 0.978745 11.00000 0.22657 0.05194 = #0.09659 -0.01561 0.04806 0.01380 #C3Y 1 0.659401 0.003472 1.035900 11.00000 0.18015 0.08031 = #0.06767 -0.02467 0.01148 -0.01954 #AFIX 137 #H3Y1 2 0.597737 -0.009832 1.048537 11.00000 -1.50000 #H3Y2 2 0.685611 0.034387 1.061042 11.00000 -1.50000 #H3Y3 2 0.706695 -0.027630 1.038130 11.00000 -1.50000 #AFIX 0 #N1Z 3 0.394622 0.123041 0.037667 11.00000 0.11314 0.09334 = #0.04992 0.00461 0.01206 -0.02345 #C2Z 1 0.427058 0.112300 0.083549 11.00000 0.05230 0.04927 = #0.05657 -0.00928 0.02082 -0.01349 #C3Z 1 0.469200 0.098354 0.141032 11.00000 0.03081 0.06992 = #0.05584 -0.01310 -0.00005 0.00166 #AFIX 137 #H3Z1 2 0.452391 0.059348 0.149897 11.00000 -1.50000 #H3Z2 2 0.443449 0.123940 0.168767 11.00000 -1.50000 #H3Z3 2 0.540555 0.102244 0.143710 11.00000 -1.50000 #HKLF 4 #REM XEHB35 in P21/n solved dirdif #REM R1 = 0.0376 for 13552 Fo > 4sig(Fo) and 0.0437 for all 15403 data #REM 901 parameters refined using 163 restraints #END #WGHT 0.0455 3.7853 #REM Highest difference peak 0.632, deepest hole -0.338, 1-sigma level 0.079 #Q1 1 0.3855 -0.2573 0.6001 11.00000 0.05 0.63 #Q2 1 -0.0437 -0.0449 0.7990 11.00000 0.05 0.47 #Q3 1 0.0222 -0.0572 0.7400 11.00000 0.05 0.46 #Q4 1 0.0959 0.0601 0.9226 11.00000 0.05 0.45 #Q5 1 -0.1194 -0.1581 1.0453 11.00000 0.05 0.44 #Q6 1 -0.3565 -0.2697 0.8213 11.00000 0.05 0.41 #Q7 1 -0.0818 -0.1901 0.9236 11.00000 0.05 0.41 #Q8 1 0.0102 -0.0300 0.7833 11.00000 0.05 0.41 #Q9 1 0.1606 -0.0376 1.0030 11.00000 0.05 0.40 #Q10 1 0.0007 -0.0108 0.8008 11.00000 0.05 0.40 #The following is an attaempt to model the disordered #solvent region with discrete part weight atoms. Note that #some atoms have been renamed in the final model. #N1X 3 0.619556 0.037663 0.930275 11.00000 0.32256 0.07357 = #0.12698 -0.00585 0.05436 0.05775 #C2X 1 0.640407 0.022446 0.978415 11.00000 0.22116 0.05152 = #0.09123 -0.01399 0.04238 0.01685 #C3X 1 0.658466 0.003721 1.035477 11.00000 0.19225 0.07878 = #0.06663 -0.02547 0.01011 -0.01806 #AFIX 137 #H3X1 2 0.598163 -0.011934 1.047803 11.00000 -1.50000 #H3X2 2 0.680729 0.035472 1.060602 11.00000 -1.50000 #H3X3 2 0.709193 -0.025532 1.038119 11.00000 -1.50000 #AFIX 0 #PART 1 #N1Y 3 0.661123 0.008951 0.553058 10.80000 0.05623 0.07485 = #0.04573 0.00180 -0.01533 0.00324 #C2Y 1 0.620204 0.002004 0.490954 10.80000 0.06138 0.06203 = #0.08858 0.01452 0.03616 0.01642 #C3Y 1 0.574528 -0.004020 0.440584 10.80000 0.15760 0.09305 = #0.04410 0.02938 0.06163 0.06691 #AFIX 137 #H3Y1 2 0.511251 -0.022204 0.443567 10.80000 -1.50000 #H3Y2 2 0.613393 -0.027562 0.417110 10.80000 -1.50000 #H3Y3 2 0.563778 0.033070 0.422300 10.80000 -1.50000 #AFIX 0 #PART 2 #O1Y 4 0.555914 0.014621 0.566903 10.20000 0.04485 #PART 0 #N1Z 3 0.393914 0.123186 0.037862 11.00000 0.11076 0.09330 = #0.04850 0.00398 0.01147 -0.02375 #C2Z 1 0.426672 0.112289 0.083461 11.00000 0.05301 0.05007 = #0.05445 -0.00980 0.02051 -0.01554 #C3Z 1 0.468833 0.097993 0.140848 11.00000 0.03199 0.06963 = #0.05675 -0.01487 0.00026 0.00249 #AFIX 137 #H3Z1 2 0.453637 0.058585 0.149043 11.00000 -1.50000 #H3Z2 2 0.441653 0.122671 0.168847 11.00000 -1.50000 #H3Z3 2 0.540015 0.102956 0.143866 11.00000 -1.50000 #AFIX 0 #N1U 3 0.906665 -0.235610 1.099033 10.20000 0.04187 #C3U 1 0.767961 -0.219231 1.034278 10.20000 0.00104 #N4U 3 0.940027 -0.106996 1.197512 10.20000 0.03673 #C5U 1 0.903663 -0.104952 1.182184 10.20000 0.03316 #N6U 3 0.857571 -0.073807 1.094890 10.20000 0.07540 #C7U 1 0.830065 -0.108772 1.103951 10.20000 0.06913 #C1V 1 0.905815 -0.106479 1.204335 10.40000 0.04375 #C2V 1 0.886817 -0.096235 1.140282 10.60000 0.07785 #O3V 4 0.854195 -0.161506 1.118844 10.60000 0.10347 #C4V 1 0.851141 -0.176244 1.061640 10.40000 0.07014 #C5V 1 0.822693 -0.226272 1.059304 10.60000 0.07322 #Q1 1 0.8551 -0.2272 1.0773 11.00000 0.05 1.49 #Q2 1 0.7438 -0.2115 1.0236 11.00000 0.05 1.35 #Q3 1 0.7759 -0.2361 1.0411 11.00000 0.05 1.34 #Q4 1 0.7870 -0.2058 1.0396 11.00000 0.05 1.14 #Q5 1 0.5155 -0.0139 0.4199 11.00000 0.05 1.13 #Q6 1 0.9132 -0.1270 1.1394 11.00000 0.05 0.79 #Q7 1 0.6008 0.0020 0.4384 11.00000 0.05 0.78 #Q8 1 0.8251 -0.0815 1.1163 11.00000 0.05 0.73 #Q9 1 0.9120 -0.2576 1.1013 11.00000 0.05 0.68 #Q10 1 0.8575 -0.0962 1.1602 11.00000 0.05 0.64 #checkcif output: #=============================================================================== # PLATON/CHECK-(191101) versus check.def version of 16/11/01 for entry: xehb35 # Data From: xehb35.cif - Data Type: CIF Bond Precision C-C = 0.0052 A # # CELL 0.71073 13.745 23.688 23.259 90.00 96.49 90.00 7524.00 # SpaceGroup from Symmetry P21/n Hall: -P 2yn # Reported P21/n ? # MoietyFormula C42 H57 Mn9 N3 O34, 2(C2 H3 N) # Reported [MN9O7(H2O)2(OAC)11(PYR)3(MEC(CH2O)3)].3MECN.ET2O # SumFormula C46 H63 Mn9 N5 O34 # Reported C52 H80 MN9 N6 O35 # Mr = 1724.48[Calc], 1843.68[Rep] # Dx,gcm-3 = 1.522[Calc], 1.628[Rep] # Z = 4[Calc], 4[Rep] # Mu (mm-1) = 1.539[Calc], 1.546[Rep] # F000 = 3484.0[Calc], 3756.0[Rep] # Reported T limits: Tmin=0.788 Tmax=0.928 'MULTISCAN' # Calculated T limits: Tmin=0.659 Tmin'=0.655 Tmax=0.831 # Reported Hmax= 17, Kmax= 29, Lmax= 29, Nref=15403 , Th(max)= 26.42 # Calculated Hmax= 17, Kmax= 29, Lmax= 29, Nref=15474(15474), Ratio= 1.00( 1.00) # R= 0.0376(13552), wR2= 0.0939(15403), S = 1.075, Npar= 901 #=============================================================================== #>>> The Following ALERTS were generated <<< #221_ALERT A Large Solvent/Anion C Ueq(max)/Ueq(min) . 6.12 Ratio #221_ALERT A Large Solvent/Anion N Ueq(max)/Ueq(min) . 7.32 Ratio #223_ALERT A Large Solvent/Anion H Ueq(max)/Ueq(min) . 6.83 Ratio #These are high, not not high enough to justify modelling this MeCN as #being disordered. The eigenvalues of the relevant tensors are: #0.3184 0.1240 0.0595 N1Y #0.2309 0.0946 0.0428 C2Y #0.1840 0.0966 0.0481 C3Y #761_ALERT A CIF Contains no X-H Bonds .................... ? #762_ALERT A CIF Contains no X-Y-H or H-Y-H Angles ........ ? #The H's are all calculated. #601_ALERT A Structure Contains Solvent Accessible VOIDS of 225.00 A**3 #043_ALERT B Check Reported Molecular Weight .............. 1843.68 #044_ALERT B Calculated and Reported Dx Differ ............ ? #041_ALERT C Calc. and Rep. SumFormula Strings Differ .. ? #042_ALERT C Calc. and Rep. MoietyFormula Strings Differ .. ? #068_ALERT C Reported F000 Differs from Calcd (or Missing). ? #These alerts arise from the use of the squeeze correction #062_ALERT C Rescale T(min) & T(max) by ................... 0.89 #125_ALERT C No _symmetry_space_group_name_Hall given ..... ? #128_ALERT C Non-standard setting of space group P21/c .. P21/n #221_ALERT C Large Solvent/Anion O Ueq(max)/Ueq(min) . 3.13 Ratio #241_ALERT C Check High U(eq) as Compared to Neighbors .... O(1W) #241_ALERT C Check High U(eq) as Compared to Neighbors .... O(27) #241_ALERT C Check High U(eq) as Compared to Neighbors .... O(29) #241_ALERT C Check High U(eq) as Compared to Neighbors .... O(110) #242_ALERT C Check Low U(eq) as Compared to Neighbors .... >C(110) #242_ALERT C Check Low U(eq) as Compared to Neighbors .... >C(111) #244_ALERT C Low Solvent U(eq) as Compared to Neighbors ... C(2Y) #244_ALERT C Low Solvent U(eq) as Compared to Neighbors ... C(2Z) #301_ALERT C Main Residue Disorder ........................ 4.00 Perc. #732_ALERT C Angle Calc 127.97(4), Rep 127.97(2) .... 2.11 s.u-Ratio #MN7 -MN2 -MN3 1.555 1.555 1.555 #732_ALERT C Angle Calc 127.69(4), Rep 127.69(2) .... 2.11 s.u-Ratio #MN9 -MN3 -MN1 1.555 1.555 1.555 #The s.u.s are calculated by shelx using the full l.s. matrix. #790_ALERT C Centre of Gravity not Within Unit Cell: Resd.# 1 #C42 H57 Mn9 N3 O34 #ALERT Level Summary #6 ALERT Level A = In General: Serious Problem #2 ALERT Level B = Potentially Serious Problem #19 ALERT Level C = Check & Explain #=============================================================================== ; _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^)+(0.0455P)^2^+3.7700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometric, not placed on part weight water' _refine_ls_hydrogen_treatment 'riding or rotating group' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00020(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 15403 _refine_ls_number_parameters 901 _refine_ls_number_restraints 163 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.001 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 0.11581(3) -0.203895(16) 0.757796(17) 0.01514(9) Uani 1 1 d . . . Mn2 Mn -0.04830(3) -0.272683(16) 0.779568(17) 0.01555(9) Uani 1 1 d . . . Mn3 Mn -0.07432(3) -0.184104(16) 0.690680(17) 0.01563(9) Uani 1 1 d . . . Mn4 Mn 0.06697(3) -0.059963(17) 0.72091(2) 0.02470(10) Uani 1 1 d . A . Mn5 Mn 0.21265(3) -0.130453(17) 0.835774(18) 0.02018(9) Uani 1 1 d . A . Mn6 Mn 0.11209(3) -0.243319(16) 0.899406(17) 0.01758(9) Uani 1 1 d . A . Mn7 Mn -0.13218(3) -0.279068(17) 0.881677(18) 0.01945(9) Uani 1 1 d . A . Mn8 Mn -0.27829(3) -0.204517(18) 0.769181(19) 0.02373(10) Uani 1 1 d . A . Mn9 Mn -0.18946(3) -0.090216(16) 0.691158(18) 0.01881(9) Uani 1 1 d . A . O1 O -0.01828(12) -0.19520(7) 0.76954(7) 0.0148(3) Uani 1 1 d . . . O2 O 0.14362(12) -0.12906(7) 0.76242(8) 0.0181(4) Uani 1 1 d . . . O3 O 0.15556(12) -0.20379(7) 0.83692(8) 0.0183(4) Uani 1 1 d . . . O4 O -0.00369(12) -0.27184(7) 0.85855(8) 0.0185(4) Uani 1 1 d . . . O5 O -0.16688(12) -0.26014(7) 0.80445(8) 0.0184(4) Uani 1 1 d . . . O6 O -0.19600(12) -0.16758(7) 0.70740(8) 0.0188(4) Uani 1 1 d . . . O7 O -0.05646(12) -0.10852(7) 0.69150(8) 0.0185(4) Uani 1 1 d . . . O11 O 0.24293(13) -0.22472(8) 0.73677(8) 0.0214(4) Uani 1 1 d . . . O21 O 0.33821(14) -0.17172(8) 0.80009(9) 0.0293(5) Uani 1 1 d . . . C11 C 0.32677(19) -0.20784(12) 0.76129(13) 0.0239(6) Uani 1 1 d . . . C21 C 0.4143(2) -0.23573(14) 0.73958(17) 0.0396(8) Uani 1 1 d . . . H21A H 0.4685 -0.2087 0.7411 0.059 Uiso 1 1 calc R . . H21B H 0.3970 -0.2482 0.6996 0.059 Uiso 1 1 calc R . . H21C H 0.4342 -0.2684 0.7640 0.059 Uiso 1 1 calc R . . O12 O -0.06534(13) -0.35350(7) 0.77526(8) 0.0222(4) Uani 1 1 d . . . O22 O -0.13459(14) -0.36949(8) 0.85672(9) 0.0292(5) Uani 1 1 d . . . C12 C -0.1043(2) -0.38575(12) 0.81107(14) 0.0281(6) Uani 1 1 d . . . C22 C -0.1115(3) -0.44671(14) 0.79397(19) 0.0570(11) Uani 1 1 d . . . H22A H -0.0595 -0.4681 0.8167 0.085 Uiso 1 1 calc R . . H22B H -0.1042 -0.4503 0.7527 0.085 Uiso 1 1 calc R . . H22C H -0.1754 -0.4616 0.8013 0.085 Uiso 1 1 calc R . . O13 O -0.11002(13) -0.18770(8) 0.60790(8) 0.0216(4) Uani 1 1 d . . . O23 O -0.20563(14) -0.11027(8) 0.59658(8) 0.0274(4) Uani 1 1 d . . . C13 C -0.16253(19) -0.15063(11) 0.57700(12) 0.0227(6) Uani 1 1 d . . . C23 C -0.1692(3) -0.15985(14) 0.51279(13) 0.0361(7) Uani 1 1 d . . . H23A H -0.2205 -0.1876 0.5012 0.054 Uiso 1 1 calc R . . H23B H -0.1063 -0.1738 0.5026 0.054 Uiso 1 1 calc R . . H23C H -0.1852 -0.1241 0.4927 0.054 Uiso 1 1 calc R . . O14 O 0.19887(16) -0.01441(9) 0.75106(10) 0.0398(6) Uani 1 1 d . . . O24 O 0.27798(15) -0.05832(8) 0.82781(9) 0.0294(5) Uani 1 1 d . . . C14 C 0.2673(2) -0.01894(12) 0.79055(13) 0.0268(6) Uani 1 1 d . . . C24 C 0.3448(3) 0.02610(14) 0.79614(16) 0.0437(9) Uani 1 1 d . . . H24A H 0.3477 0.0442 0.7585 0.066 Uiso 1 1 calc R . . H24B H 0.4084 0.0091 0.8093 0.066 Uiso 1 1 calc R . . H24C H 0.3288 0.0544 0.8243 0.066 Uiso 1 1 calc R . . O15 O 0.28959(15) -0.14040(8) 0.91224(9) 0.0303(5) Uani 1 1 d . . . O25 O 0.23229(13) -0.22050(8) 0.94834(8) 0.0246(4) Uani 1 1 d . . . C15 C 0.29097(19) -0.17960(11) 0.94883(12) 0.0228(6) Uani 1 1 d . . . C25 C 0.3704(2) -0.17746(14) 0.99874(14) 0.0353(7) Uani 1 1 d . . . H25A H 0.3524 -0.1503 1.0275 0.053 Uiso 1 1 calc R . . H25B H 0.4320 -0.1657 0.9848 0.053 Uiso 1 1 calc R . . H25C H 0.3786 -0.2149 1.0164 0.053 Uiso 1 1 calc R . . O16 O 0.08096(14) -0.28504(9) 0.96809(8) 0.0277(4) Uani 1 1 d . . . O26 O -0.07944(14) -0.30628(9) 0.95964(9) 0.0294(5) Uani 1 1 d . . . C16 C 0.0069(2) -0.30982(12) 0.98387(12) 0.0247(6) Uani 1 1 d . . . C26 C 0.0235(2) -0.34593(15) 1.03731(14) 0.0390(8) Uani 1 1 d . . . H26A H 0.0927 -0.3567 1.0440 0.059 Uiso 1 1 calc R . . H26B H -0.0170 -0.3800 1.0320 0.059 Uiso 1 1 calc R . . H26C H 0.0057 -0.3246 1.0707 0.059 Uiso 1 1 calc R . . O17 O -0.26619(13) -0.28729(9) 0.90199(9) 0.0267(4) Uani 1 1 d . . . O27 O -0.36177(15) -0.24034(11) 0.83406(11) 0.0453(6) Uani 1 1 d . . . C17 C -0.3471(2) -0.26571(12) 0.88052(13) 0.0264(6) Uani 1 1 d . . . C27 C -0.4307(2) -0.27104(14) 0.91690(15) 0.0346(7) Uani 1 1 d . . . H27A H -0.4154 -0.2498 0.9529 0.052 Uiso 1 1 calc R . . H27B H -0.4406 -0.3109 0.9259 0.052 Uiso 1 1 calc R . . H27C H -0.4906 -0.2559 0.8955 0.052 Uiso 1 1 calc R . . O18 O -0.39191(14) -0.14957(9) 0.73300(10) 0.0361(5) Uani 1 1 d . . . O28 O -0.33298(13) -0.07913(8) 0.68298(9) 0.0282(5) Uani 1 1 d . . . C18 C -0.40156(19) -0.10688(12) 0.70185(13) 0.0249(6) Uani 1 1 d . . . C28 C -0.5044(2) -0.08572(14) 0.68498(17) 0.0394(8) Uani 1 1 d . . . H28A H -0.5478 -0.1178 0.6744 0.059 Uiso 1 1 calc R . . H28B H -0.5049 -0.0601 0.6519 0.059 Uiso 1 1 calc R . . H28C H -0.5273 -0.0656 0.7177 0.059 Uiso 1 1 calc R . . O19 O -0.17262(13) -0.01010(8) 0.66950(9) 0.0258(4) Uani 1 1 d . . . O29 O -0.01213(15) 0.00985(9) 0.67908(11) 0.0403(6) Uani 1 1 d . . . C19 C -0.0999(2) 0.02214(11) 0.66633(12) 0.0238(6) Uani 1 1 d . . . C29 C -0.1232(2) 0.08095(13) 0.64380(16) 0.0379(8) Uani 1 1 d . . . H29A H -0.0873 0.1086 0.6694 0.057 Uiso 1 1 calc R . . H29B H -0.1937 0.0878 0.6427 0.057 Uiso 1 1 calc R . . H29C H -0.1037 0.0846 0.6047 0.057 Uiso 1 1 calc R . . O110 O -0.23681(17) -0.13763(10) 0.83427(11) 0.0451(6) Uani 1 1 d D . . O210 O -0.18165(15) -0.05926(9) 0.78060(9) 0.0311(5) Uani 1 1 d D . . C110 C -0.2054(3) -0.08338(18) 0.8263(2) 0.0235(10) Uani 0.593(3) 1 d PD A 1 C210 C -0.1997(5) -0.0461(2) 0.8801(2) 0.0426(15) Uani 0.593(3) 1 d PD A 1 H21D H -0.1412 -0.0222 0.8819 0.064 Uiso 0.593(3) 1 calc PR A 1 H21E H -0.1961 -0.0699 0.9147 0.064 Uiso 0.593(3) 1 calc PR A 1 H21F H -0.2582 -0.0222 0.8783 0.064 Uiso 0.593(3) 1 calc PR A 1 C310 C -0.0934(7) -0.0396(7) 0.8109(6) 0.031(4) Uiso 0.190(4) 1 d PD A 2 C410 C -0.1135(14) -0.0161(9) 0.8705(7) 0.051(5) Uiso 0.190(4) 1 d PD A 2 H41A H -0.1503 0.0193 0.8651 0.077 Uiso 0.190(4) 1 calc PR A 2 H41B H -0.0511 -0.0091 0.8943 0.077 Uiso 0.190(4) 1 calc PR A 2 H41C H -0.1517 -0.0437 0.8900 0.077 Uiso 0.190(4) 1 calc PR A 2 C510 C -0.1865(10) -0.1487(5) 0.8902(5) 0.034(3) Uiso 0.218(4) 1 d PD A 3 C610 C -0.1832(14) -0.0962(6) 0.9295(7) 0.052(5) Uiso 0.218(4) 1 d PD A 3 H61A H -0.2173 -0.1044 0.9634 0.078 Uiso 0.218(4) 1 calc PR A 3 H61B H -0.2154 -0.0645 0.9079 0.078 Uiso 0.218(4) 1 calc PR A 3 H61C H -0.1149 -0.0864 0.9422 0.078 Uiso 0.218(4) 1 calc PR A 3 O111 O 0.10599(16) -0.08776(9) 0.88340(9) 0.0358(5) Uani 1 1 d D . . O211 O 0.04840(15) -0.16671(9) 0.93673(10) 0.0370(5) Uani 1 1 d D . . C111 C 0.0648(3) -0.11183(19) 0.9265(2) 0.0232(10) Uani 0.593(3) 1 d PD A 1 C211 C 0.0346(5) -0.0703(2) 0.9709(3) 0.0456(16) Uani 0.593(3) 1 d PD A 1 H21G H 0.0769 -0.0751 1.0074 0.068 Uiso 0.593(3) 1 calc PR A 1 H21H H -0.0336 -0.0773 0.9773 0.068 Uiso 0.593(3) 1 calc PR A 1 H21I H 0.0410 -0.0317 0.9566 0.068 Uiso 0.593(3) 1 calc PR A 1 C311 C -0.0517(7) -0.1665(6) 0.9405(6) 0.026(3) Uiso 0.190(4) 1 d PD A 2 C411 C -0.0734(11) -0.1200(6) 0.9839(7) 0.036(4) Uiso 0.190(4) 1 d PD A 2 H41D H -0.1294 -0.0974 0.9673 0.054 Uiso 0.190(4) 1 calc PR A 2 H41E H -0.0158 -0.0955 0.9918 0.054 Uiso 0.190(4) 1 calc PR A 2 H41F H -0.0885 -0.1374 1.0200 0.054 Uiso 0.190(4) 1 calc PR A 2 C511 C 0.0400(9) -0.0451(5) 0.8588(5) 0.033(3) Uiso 0.218(4) 1 d PD A 3 C611 C 0.0099(13) -0.0043(7) 0.9053(7) 0.052(5) Uiso 0.218(4) 1 d PD A 3 H61D H -0.0153 -0.0260 0.9363 0.079 Uiso 0.218(4) 1 calc PR A 3 H61E H -0.0410 0.0213 0.8878 0.079 Uiso 0.218(4) 1 calc PR A 3 H61F H 0.0671 0.0176 0.9213 0.079 Uiso 0.218(4) 1 calc PR A 3 O1W O 0.00650(17) -0.03097(10) 0.80027(11) 0.0464(6) Uani 1 1 d D . . O2W O -0.13764(15) -0.19346(9) 0.91751(9) 0.0320(5) Uani 1 1 d D . . N1A N 0.12951(18) -0.07860(11) 0.63613(11) 0.0323(6) Uani 1 1 d . . . C2A C 0.2182(2) -0.10160(17) 0.63640(16) 0.0456(9) Uani 1 1 d . A . H2A H 0.2596 -0.1033 0.6720 0.055 Uiso 1 1 calc R . . C3A C 0.2529(3) -0.1232(2) 0.58699(19) 0.0595(11) Uani 1 1 d . . . H3A H 0.3166 -0.1392 0.5892 0.071 Uiso 1 1 calc R A . C4A C 0.1950(3) -0.1212(2) 0.53530(19) 0.0590(11) Uani 1 1 d . A . H4A H 0.2172 -0.1353 0.5009 0.071 Uiso 1 1 calc R . . C5A C 0.1023(3) -0.0977(2) 0.53501(18) 0.0619(12) Uani 1 1 d . . . H5A H 0.0595 -0.0958 0.5000 0.074 Uiso 1 1 calc R A . C6A C 0.0724(3) -0.07708(17) 0.58602(16) 0.0458(9) Uani 1 1 d . A . H6A H 0.0088 -0.0612 0.5851 0.055 Uiso 1 1 calc R . . N1B N 0.19813(16) -0.32072(10) 0.87700(10) 0.0228(5) Uani 1 1 d . . . C2B C 0.2881(2) -0.31454(13) 0.86071(13) 0.0286(6) Uani 1 1 d . A . H2B H 0.3144 -0.2776 0.8590 0.034 Uiso 1 1 calc R . . C3B C 0.3443(2) -0.35958(15) 0.84628(15) 0.0398(8) Uani 1 1 d . . . H3B H 0.4080 -0.3535 0.8353 0.048 Uiso 1 1 calc R A . C4B C 0.3066(3) -0.41363(15) 0.84796(16) 0.0465(9) Uani 1 1 d . A . H4B H 0.3441 -0.4453 0.8385 0.056 Uiso 1 1 calc R . . C5B C 0.2145(3) -0.42055(14) 0.86353(16) 0.0419(8) Uani 1 1 d . . . H5B H 0.1866 -0.4572 0.8646 0.050 Uiso 1 1 calc R A . C6B C 0.1619(2) -0.37337(12) 0.87786(13) 0.0303(7) Uani 1 1 d . A . H6B H 0.0979 -0.3786 0.8887 0.036 Uiso 1 1 calc R . . N1C N -0.32425(18) -0.27293(11) 0.70258(12) 0.0327(6) Uani 1 1 d . . . C2C C -0.3143(3) -0.32695(15) 0.71695(19) 0.0501(10) Uani 1 1 d . A . H2C H -0.3058 -0.3367 0.7568 0.060 Uiso 1 1 calc R . . C3C C -0.3158(4) -0.3699(2) 0.6763(2) 0.0775(15) Uani 1 1 d . . . H3C H -0.3075 -0.4081 0.6881 0.093 Uiso 1 1 calc R A . C4C C -0.3296(4) -0.3557(2) 0.6182(2) 0.0785(15) Uani 1 1 d . A . H4C H -0.3305 -0.3842 0.5894 0.094 Uiso 1 1 calc R . . C5C C -0.3420(3) -0.2998(2) 0.60286(19) 0.0597(11) Uani 1 1 d . . . H5C H -0.3542 -0.2890 0.5634 0.072 Uiso 1 1 calc R A . C6C C -0.3365(2) -0.26036(16) 0.64599(15) 0.0410(8) Uani 1 1 d . A . H6C H -0.3416 -0.2217 0.6352 0.049 Uiso 1 1 calc R . . O1T O 0.08421(12) -0.28391(7) 0.76029(8) 0.0163(4) Uani 1 1 d . . . C1T C 0.10343(19) -0.32102(11) 0.71463(12) 0.0201(5) Uani 1 1 d . . . H1T1 H 0.0827 -0.3597 0.7239 0.024 Uiso 1 1 calc R . . H1T2 H 0.1748 -0.3219 0.7121 0.024 Uiso 1 1 calc R . . O2T O -0.09543(12) -0.26665(7) 0.69853(7) 0.0169(4) Uani 1 1 d . . . C2T C -0.06047(19) -0.30489(11) 0.65731(12) 0.0202(5) Uani 1 1 d . . . H2T1 H -0.0929 -0.2956 0.6183 0.024 Uiso 1 1 calc R . . H2T2 H -0.0800 -0.3438 0.6666 0.024 Uiso 1 1 calc R . . O3T O 0.06371(12) -0.20031(7) 0.67774(7) 0.0165(4) Uani 1 1 d . . . C3T C 0.08502(19) -0.24445(11) 0.63877(11) 0.0204(5) Uani 1 1 d . . . H3T1 H 0.1566 -0.2456 0.6370 0.024 Uiso 1 1 calc R . . H3T2 H 0.0534 -0.2352 0.5995 0.024 Uiso 1 1 calc R . . C4T C 0.05052(19) -0.30361(11) 0.65568(12) 0.0201(5) Uani 1 1 d . . . C5T C 0.0764(2) -0.34622(12) 0.61025(12) 0.0271(6) Uani 1 1 d . . . H5T1 H 0.1476 -0.3509 0.6132 0.041 Uiso 1 1 calc R . . H5T2 H 0.0523 -0.3324 0.5715 0.041 Uiso 1 1 calc R . . H5T3 H 0.0458 -0.3826 0.6169 0.041 Uiso 1 1 calc R . . N1Y N 0.6220(7) 0.0384(3) 0.9300(3) 0.167(3) Uani 1 1 d . . . C2Y C 0.6425(7) 0.0227(3) 0.9787(4) 0.123(3) Uani 1 1 d . . . C3Y C 0.6594(6) 0.0035(3) 1.0359(3) 0.110(2) Uani 1 1 d . . . H3Y1 H 0.5977 -0.0098 1.0485 0.164 Uiso 1 1 calc R . . H3Y2 H 0.6856 0.0344 1.0610 0.164 Uiso 1 1 calc R . . H3Y3 H 0.7067 -0.0276 1.0381 0.164 Uiso 1 1 calc R . . N1Z N 0.3946(4) 0.1230(2) 0.03767(18) 0.0852(13) Uani 1 1 d . . . C2Z C 0.4271(3) 0.11230(17) 0.08355(19) 0.0516(10) Uani 1 1 d . . . C3Z C 0.4692(3) 0.09835(18) 0.14103(17) 0.0526(10) Uani 1 1 d . . . H3Z1 H 0.4524 0.0593 0.1499 0.079 Uiso 1 1 calc R . . H3Z2 H 0.4434 0.1239 0.1688 0.079 Uiso 1 1 calc R . . H3Z3 H 0.5406 0.1022 0.1437 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01320(18) 0.01499(19) 0.0167(2) 0.00067(14) -0.00055(14) -0.00056(14) Mn2 0.01441(18) 0.01484(19) 0.0170(2) 0.00053(14) 0.00000(14) -0.00062(14) Mn3 0.01416(18) 0.01525(19) 0.0168(2) 0.00059(14) -0.00105(14) 0.00025(14) Mn4 0.0196(2) 0.0170(2) 0.0354(3) 0.00422(17) -0.00634(18) -0.00166(16) Mn5 0.0216(2) 0.0177(2) 0.0197(2) 0.00229(15) -0.00473(16) -0.00534(16) Mn6 0.01631(19) 0.0195(2) 0.0163(2) 0.00179(15) -0.00111(15) -0.00188(15) Mn7 0.01601(19) 0.0227(2) 0.0196(2) 0.00391(16) 0.00168(15) -0.00104(15) Mn8 0.0153(2) 0.0282(2) 0.0274(2) 0.00587(18) 0.00159(16) 0.00241(16) Mn9 0.01529(19) 0.01541(19) 0.0254(2) 0.00211(15) 0.00069(16) 0.00147(15) O1 0.0141(8) 0.0134(8) 0.0165(9) 0.0010(7) -0.0003(7) -0.0008(7) O2 0.0189(9) 0.0163(9) 0.0182(9) 0.0016(7) -0.0012(7) -0.0022(7) O3 0.0179(9) 0.0180(9) 0.0179(9) 0.0009(7) -0.0023(7) -0.0035(7) O4 0.0168(9) 0.0216(9) 0.0168(9) 0.0016(7) 0.0002(7) -0.0023(7) O5 0.0142(8) 0.0219(9) 0.0188(9) 0.0001(7) 0.0012(7) 0.0001(7) O6 0.0143(8) 0.0177(9) 0.0243(10) 0.0027(7) 0.0012(7) 0.0002(7) O7 0.0173(9) 0.0148(9) 0.0226(10) 0.0033(7) -0.0008(7) 0.0002(7) O11 0.0156(9) 0.0230(10) 0.0253(10) 0.0002(8) 0.0014(7) -0.0003(7) O21 0.0191(10) 0.0287(11) 0.0385(12) -0.0012(9) -0.0039(9) -0.0036(8) C11 0.0156(13) 0.0241(14) 0.0314(16) 0.0072(12) 0.0000(11) -0.0020(11) C21 0.0151(14) 0.0377(18) 0.066(2) -0.0040(16) 0.0056(14) -0.0007(13) O12 0.0221(9) 0.0156(9) 0.0284(11) 0.0005(8) 0.0011(8) -0.0027(7) O22 0.0300(11) 0.0219(10) 0.0368(12) 0.0070(9) 0.0089(9) -0.0021(8) C12 0.0255(14) 0.0191(14) 0.0401(18) 0.0019(12) 0.0050(13) -0.0020(11) C22 0.079(3) 0.0227(17) 0.077(3) -0.0025(17) 0.042(2) -0.0101(18) O13 0.0230(9) 0.0214(9) 0.0192(10) 0.0012(7) -0.0031(7) 0.0026(8) O23 0.0293(10) 0.0264(10) 0.0246(11) 0.0013(8) -0.0050(8) 0.0082(8) C13 0.0224(13) 0.0221(14) 0.0221(14) 0.0011(11) -0.0034(11) -0.0050(11) C23 0.050(2) 0.0336(17) 0.0218(16) 0.0005(13) -0.0104(14) 0.0056(15) O14 0.0344(12) 0.0275(11) 0.0524(15) 0.0146(10) -0.0175(11) -0.0112(9) O24 0.0354(11) 0.0223(10) 0.0277(11) 0.0043(8) -0.0083(9) -0.0112(9) C14 0.0240(14) 0.0193(14) 0.0361(17) -0.0025(12) -0.0009(12) -0.0068(11) C24 0.0413(19) 0.0339(18) 0.052(2) 0.0131(16) -0.0120(16) -0.0192(15) O15 0.0357(11) 0.0253(10) 0.0261(11) 0.0040(8) -0.0131(9) -0.0116(9) O25 0.0214(9) 0.0275(10) 0.0232(10) 0.0035(8) -0.0044(8) -0.0046(8) C15 0.0217(13) 0.0235(14) 0.0219(14) -0.0028(11) -0.0035(11) -0.0002(11) C25 0.0336(17) 0.0408(18) 0.0278(17) 0.0059(14) -0.0129(13) -0.0094(14) O16 0.0253(10) 0.0379(12) 0.0192(10) 0.0072(9) -0.0010(8) -0.0073(9) O26 0.0209(10) 0.0434(12) 0.0236(11) 0.0113(9) 0.0014(8) -0.0011(9) C16 0.0259(14) 0.0283(15) 0.0201(14) 0.0030(11) 0.0031(11) 0.0004(12) C26 0.0323(17) 0.051(2) 0.0324(18) 0.0200(15) -0.0040(14) -0.0050(15) O17 0.0189(10) 0.0328(11) 0.0289(11) 0.0053(9) 0.0052(8) -0.0001(8) O27 0.0213(11) 0.0709(17) 0.0449(15) 0.0248(13) 0.0083(10) 0.0091(11) C17 0.0195(14) 0.0268(15) 0.0337(17) -0.0004(12) 0.0066(12) -0.0047(11) C27 0.0263(15) 0.0381(18) 0.0414(19) 0.0013(14) 0.0122(14) -0.0003(13) O18 0.0181(10) 0.0377(12) 0.0529(15) 0.0165(11) 0.0060(9) 0.0035(9) O28 0.0179(9) 0.0229(10) 0.0436(13) 0.0040(9) 0.0024(9) 0.0027(8) C18 0.0195(13) 0.0243(14) 0.0301(16) -0.0018(12) -0.0009(11) 0.0026(11) C28 0.0188(15) 0.0388(18) 0.060(2) 0.0108(16) 0.0010(14) 0.0050(13) O19 0.0216(10) 0.0181(9) 0.0376(12) 0.0049(8) 0.0023(8) 0.0013(8) O29 0.0252(11) 0.0238(11) 0.0690(17) 0.0163(11) -0.0076(11) -0.0020(9) C19 0.0256(14) 0.0210(14) 0.0241(15) 0.0015(11) 0.0003(11) 0.0020(11) C29 0.0302(16) 0.0254(16) 0.057(2) 0.0145(15) 0.0009(15) 0.0007(13) O110 0.0430(14) 0.0492(15) 0.0424(14) -0.0159(11) 0.0012(11) 0.0137(11) O210 0.0345(11) 0.0301(11) 0.0291(12) -0.0029(9) 0.0059(9) -0.0031(9) C110 0.022(2) 0.021(2) 0.027(3) -0.0071(19) -0.0002(19) 0.0021(18) C210 0.060(4) 0.038(3) 0.033(3) -0.010(2) 0.017(3) -0.015(3) O111 0.0427(13) 0.0347(12) 0.0302(12) -0.0036(9) 0.0056(10) 0.0044(10) O211 0.0305(12) 0.0393(13) 0.0417(14) -0.0106(10) 0.0060(10) 0.0066(10) C111 0.020(2) 0.025(2) 0.024(2) -0.0046(19) -0.0030(18) 0.0010(18) C211 0.070(4) 0.030(3) 0.041(4) -0.006(2) 0.023(3) 0.005(3) O1W 0.0407(13) 0.0445(14) 0.0526(16) -0.0186(12) -0.0002(11) 0.0098(11) O2W 0.0335(11) 0.0301(11) 0.0329(12) -0.0044(9) 0.0055(9) -0.0003(9) N1A 0.0289(13) 0.0345(14) 0.0331(15) 0.0095(11) 0.0023(11) -0.0050(11) C2A 0.0274(17) 0.065(2) 0.044(2) 0.0075(18) 0.0017(15) -0.0003(16) C3A 0.038(2) 0.082(3) 0.060(3) -0.003(2) 0.0145(19) 0.001(2) C4A 0.056(2) 0.076(3) 0.048(2) -0.008(2) 0.016(2) -0.010(2) C5A 0.063(3) 0.087(3) 0.034(2) 0.000(2) -0.0036(19) -0.004(2) C6A 0.0380(19) 0.059(2) 0.039(2) 0.0077(17) -0.0023(16) 0.0024(17) N1B 0.0241(12) 0.0247(12) 0.0180(12) 0.0018(9) -0.0043(9) 0.0018(9) C2B 0.0227(14) 0.0317(16) 0.0303(16) 0.0011(12) -0.0016(12) 0.0022(12) C3B 0.0281(16) 0.046(2) 0.046(2) -0.0064(16) 0.0066(14) 0.0105(14) C4B 0.052(2) 0.0366(19) 0.050(2) -0.0159(16) -0.0001(17) 0.0187(16) C5B 0.056(2) 0.0243(16) 0.043(2) -0.0073(14) -0.0044(17) 0.0008(15) C6B 0.0339(16) 0.0263(15) 0.0294(16) -0.0010(12) -0.0026(13) -0.0010(12) N1C 0.0226(12) 0.0345(14) 0.0394(16) 0.0031(12) -0.0038(11) -0.0061(11) C2C 0.049(2) 0.039(2) 0.059(3) 0.0018(17) -0.0089(18) -0.0109(17) C3C 0.087(4) 0.044(3) 0.094(4) -0.011(2) -0.020(3) -0.005(2) C4C 0.081(3) 0.080(4) 0.071(3) -0.038(3) -0.007(3) -0.005(3) C5C 0.053(2) 0.078(3) 0.045(2) -0.010(2) -0.0048(19) -0.008(2) C6C 0.0340(18) 0.049(2) 0.0379(19) 0.0006(16) -0.0068(14) -0.0052(15) O1T 0.0144(8) 0.0143(8) 0.0197(9) -0.0009(7) 0.0006(7) 0.0014(7) C1T 0.0193(13) 0.0167(13) 0.0243(14) -0.0026(10) 0.0023(11) 0.0031(10) O2T 0.0163(8) 0.0169(9) 0.0170(9) -0.0018(7) -0.0002(7) -0.0011(7) C2T 0.0216(13) 0.0186(13) 0.0193(14) -0.0039(10) -0.0022(10) 0.0017(10) O3T 0.0141(8) 0.0188(9) 0.0162(9) 0.0003(7) -0.0004(7) 0.0011(7) C3T 0.0224(13) 0.0223(13) 0.0164(13) -0.0007(10) 0.0017(10) 0.0014(10) C4T 0.0201(13) 0.0200(13) 0.0200(14) -0.0039(10) 0.0015(10) 0.0011(10) C5T 0.0286(15) 0.0284(15) 0.0239(15) -0.0056(12) 0.0018(12) 0.0042(12) N1Y 0.304(11) 0.074(4) 0.131(6) -0.003(4) 0.060(7) 0.052(5) C2Y 0.227(9) 0.052(3) 0.097(5) -0.016(3) 0.048(6) 0.014(4) C3Y 0.180(7) 0.080(4) 0.068(4) -0.025(3) 0.011(4) -0.020(4) N1Z 0.113(4) 0.093(3) 0.050(3) 0.005(2) 0.012(2) -0.023(3) C2Z 0.052(2) 0.049(2) 0.057(3) -0.0093(19) 0.021(2) -0.0135(18) C3Z 0.0308(18) 0.070(3) 0.056(3) -0.013(2) -0.0001(17) 0.0017(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 1.8139(18) . ? Mn1 O3 1.8595(18) . ? Mn1 O1 1.9046(17) . ? Mn1 O3T 1.9197(18) . ? Mn1 O11 1.9309(18) . ? Mn1 O1T 1.9470(18) . ? Mn1 Mn5 2.7462(8) . ? Mn1 Mn2 2.8736(7) . ? Mn1 Mn3 2.9263(10) . ? Mn2 O5 1.8146(18) . ? Mn2 O4 1.8700(18) . ? Mn2 O1 1.9014(17) . ? Mn2 O2T 1.9278(18) . ? Mn2 O12 1.9300(18) . ? Mn2 O1T 1.9426(17) . ? Mn2 Mn7 2.7589(9) . ? Mn2 Mn3 2.9390(7) . ? Mn3 O6 1.8024(18) . ? Mn3 O7 1.8069(18) . ? Mn3 O1 1.9255(18) . ? Mn3 O13 1.9343(19) . ? Mn3 O2T 1.9883(18) . ? Mn3 O3T 1.9916(17) . ? Mn3 Mn9 2.7303(7) . ? Mn4 O7 2.0992(18) . ? Mn4 O2 2.1193(18) . ? Mn4 O29 2.150(2) . ? Mn4 O14 2.158(2) . ? Mn4 O1W 2.217(3) . ? Mn4 N1A 2.282(3) . ? Mn5 O2 1.8565(18) . ? Mn5 O3 1.9077(18) . ? Mn5 O24 1.9489(19) . ? Mn5 O15 1.978(2) . ? Mn5 O111 2.183(2) . ? Mn5 O21 2.224(2) . ? Mn6 O3 1.8822(19) . ? Mn6 O4 1.8840(18) . ? Mn6 O16 1.966(2) . ? Mn6 O25 1.9728(19) . ? Mn6 O211 2.233(2) . ? Mn6 N1B 2.274(2) . ? Mn7 O5 1.8605(18) . ? Mn7 O4 1.9111(18) . ? Mn7 O17 1.9623(19) . ? Mn7 O26 1.983(2) . ? Mn7 O2W 2.197(2) . ? Mn7 O22 2.219(2) . ? Mn8 O5 2.1142(18) . ? Mn8 O6 2.1159(19) . ? Mn8 O18 2.132(2) . ? Mn8 O27 2.169(2) . ? Mn8 O110 2.221(2) . ? Mn8 N1C 2.281(3) . ? Mn9 O6 1.8755(18) . ? Mn9 O7 1.8779(18) . ? Mn9 O28 1.9778(19) . ? Mn9 O19 1.9837(19) . ? Mn9 O210 2.197(2) . ? Mn9 O23 2.237(2) . ? O11 C11 1.290(3) . ? O21 C11 1.241(3) . ? C11 C21 1.508(4) . ? O12 C12 1.290(3) . ? O22 C12 1.245(4) . ? C12 C22 1.498(4) . ? O13 C13 1.300(3) . ? O23 C13 1.238(3) . ? C13 C23 1.502(4) . ? O14 C14 1.243(3) . ? O24 C14 1.270(3) . ? C14 C24 1.503(4) . ? O15 C15 1.258(3) . ? O25 C15 1.260(3) . ? C15 C25 1.502(4) . ? O16 C16 1.265(3) . ? O26 C16 1.258(3) . ? C16 C26 1.505(4) . ? O17 C17 1.274(3) . ? O27 C17 1.233(4) . ? C17 C27 1.507(4) . ? O18 C18 1.242(3) . ? O28 C18 1.268(3) . ? C18 C28 1.509(4) . ? O19 C19 1.266(3) . ? O29 C19 1.244(3) . ? C19 C29 1.510(4) . ? O110 C110 1.375(5) . ? O110 C510 1.427(10) . ? O210 C110 1.281(5) . ? O210 C310 1.411(10) . ? C110 C210 1.527(6) . ? C310 O1W 1.437(10) . ? C310 C410 1.548(14) . ? C510 O2W 1.372(10) . ? C510 C610 1.540(13) . ? O111 C111 1.335(5) . ? O111 C511 1.434(10) . ? O211 C111 1.345(5) . ? O211 C311 1.389(10) . ? C111 C211 1.516(6) . ? C311 O2W 1.395(9) . ? C311 C411 1.544(13) . ? C511 O1W 1.427(10) . ? C511 C611 1.539(13) . ? N1A C6A 1.330(4) . ? N1A C2A 1.335(4) . ? C2A C3A 1.390(5) . ? C3A C4A 1.366(6) . ? C4A C5A 1.389(6) . ? C5A C6A 1.388(6) . ? N1B C2B 1.342(4) . ? N1B C6B 1.344(4) . ? C2B C3B 1.380(4) . ? C3B C4B 1.383(5) . ? C4B C5B 1.366(5) . ? C5B C6B 1.392(4) . ? N1C C2C 1.326(4) . ? N1C C6C 1.341(4) . ? C2C C3C 1.386(6) . ? C3C C4C 1.384(7) . ? C4C C5C 1.378(7) . ? C5C C6C 1.367(5) . ? O1T C1T 1.426(3) . ? C1T C4T 1.534(4) . ? O2T C2T 1.440(3) . ? C2T C4T 1.531(4) . ? O3T C3T 1.435(3) . ? C3T C4T 1.545(4) . ? C4T C5T 1.532(4) . ? N1Y C2Y 1.195(9) . ? C2Y C3Y 1.400(9) . ? N1Z C2Z 1.138(5) . ? C2Z C3Z 1.434(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 O2 Mn1 O3 84.48(8) . . ? O2 Mn1 O1 94.97(8) . . ? O3 Mn1 O1 92.22(8) . . ? O2 Mn1 O3T 93.85(8) . . ? O3 Mn1 O3T 174.54(8) . . ? O1 Mn1 O3T 82.74(8) . . ? O2 Mn1 O11 94.25(8) . . ? O3 Mn1 O11 94.47(8) . . ? O1 Mn1 O11 169.09(8) . . ? O3T Mn1 O11 90.84(8) . . ? O2 Mn1 O1T 174.77(8) . . ? O3 Mn1 O1T 90.76(8) . . ? O1 Mn1 O1T 83.01(7) . . ? O3T Mn1 O1T 90.69(7) . . ? O11 Mn1 O1T 88.29(8) . . ? O2 Mn1 Mn5 42.16(6) . . ? O3 Mn1 Mn5 43.89(6) . . ? O1 Mn1 Mn5 103.96(6) . . ? O3T Mn1 Mn5 135.42(6) . . ? O11 Mn1 Mn5 86.80(6) . . ? O1T Mn1 Mn5 133.64(5) . . ? O2 Mn1 Mn2 135.07(6) . . ? O3 Mn1 Mn2 88.56(6) . . ? O1 Mn1 Mn2 40.93(5) . . ? O3T Mn1 Mn2 88.96(6) . . ? O11 Mn1 Mn2 130.58(6) . . ? O1T Mn1 Mn2 42.31(5) . . ? Mn5 Mn1 Mn2 125.05(2) . . ? O2 Mn1 Mn3 92.55(6) . . ? O3 Mn1 Mn3 132.26(6) . . ? O1 Mn1 Mn3 40.45(5) . . ? O3T Mn1 Mn3 42.51(5) . . ? O11 Mn1 Mn3 133.23(6) . . ? O1T Mn1 Mn3 89.03(5) . . ? Mn5 Mn1 Mn3 126.00(2) . . ? Mn2 Mn1 Mn3 60.885(17) . . ? O5 Mn2 O4 83.77(8) . . ? O5 Mn2 O1 95.52(8) . . ? O4 Mn2 O1 93.35(8) . . ? O5 Mn2 O2T 94.88(8) . . ? O4 Mn2 O2T 175.11(8) . . ? O1 Mn2 O2T 82.08(7) . . ? O5 Mn2 O12 94.06(8) . . ? O4 Mn2 O12 94.94(8) . . ? O1 Mn2 O12 167.94(8) . . ? O2T Mn2 O12 89.85(8) . . ? O5 Mn2 O1T 174.49(8) . . ? O4 Mn2 O1T 90.94(8) . . ? O1 Mn2 O1T 83.21(7) . . ? O2T Mn2 O1T 90.27(8) . . ? O12 Mn2 O1T 87.91(7) . . ? O5 Mn2 Mn7 41.98(6) . . ? O4 Mn2 Mn7 43.73(5) . . ? O1 Mn2 Mn7 106.03(5) . . ? O2T Mn2 Mn7 135.95(5) . . ? O12 Mn2 Mn7 86.00(6) . . ? O1T Mn2 Mn7 133.25(6) . . ? O5 Mn2 Mn1 135.61(6) . . ? O4 Mn2 Mn1 89.45(6) . . ? O1 Mn2 Mn1 41.01(5) . . ? O2T Mn2 Mn1 88.24(6) . . ? O12 Mn2 Mn1 130.27(6) . . ? O1T Mn2 Mn1 42.43(5) . . ? Mn7 Mn2 Mn1 126.55(2) . . ? O5 Mn2 Mn3 93.74(6) . . ? O4 Mn2 Mn3 133.14(6) . . ? O1 Mn2 Mn3 40.13(5) . . ? O2T Mn2 Mn3 42.15(5) . . ? O12 Mn2 Mn3 131.86(6) . . ? O1T Mn2 Mn3 88.74(6) . . ? Mn7 Mn2 Mn3 127.970(19) . . ? Mn1 Mn2 Mn3 60.44(2) . . ? O6 Mn3 O7 84.89(8) . . ? O6 Mn3 O1 96.03(8) . . ? O7 Mn3 O1 94.93(8) . . ? O6 Mn3 O13 95.00(8) . . ? O7 Mn3 O13 94.18(8) . . ? O1 Mn3 O13 166.26(8) . . ? O6 Mn3 O2T 92.58(8) . . ? O7 Mn3 O2T 174.02(8) . . ? O1 Mn3 O2T 79.93(7) . . ? O13 Mn3 O2T 91.43(8) . . ? O6 Mn3 O3T 175.94(8) . . ? O7 Mn3 O3T 93.55(8) . . ? O1 Mn3 O3T 80.35(7) . . ? O13 Mn3 O3T 88.85(8) . . ? O2T Mn3 O3T 88.61(7) . . ? O6 Mn3 Mn9 43.10(6) . . ? O7 Mn3 Mn9 43.20(6) . . ? O1 Mn3 Mn9 106.08(5) . . ? O13 Mn3 Mn9 87.59(6) . . ? O2T Mn3 Mn9 135.24(5) . . ? O3T Mn3 Mn9 136.06(5) . . ? O6 Mn3 Mn1 135.57(6) . . ? O7 Mn3 Mn1 92.35(6) . . ? O1 Mn3 Mn1 39.92(5) . . ? O13 Mn3 Mn1 129.40(6) . . ? O2T Mn3 Mn1 85.66(5) . . ? O3T Mn3 Mn1 40.64(5) . . ? Mn9 Mn3 Mn1 127.688(19) . . ? O6 Mn3 Mn2 92.59(6) . . ? O7 Mn3 Mn2 133.98(6) . . ? O1 Mn3 Mn2 39.53(5) . . ? O13 Mn3 Mn2 131.74(6) . . ? O2T Mn3 Mn2 40.59(5) . . ? O3T Mn3 Mn2 85.78(6) . . ? Mn9 Mn3 Mn2 127.10(2) . . ? Mn1 Mn3 Mn2 58.673(19) . . ? O7 Mn4 O2 93.84(7) . . ? O7 Mn4 O29 85.72(8) . . ? O2 Mn4 O29 179.43(8) . . ? O7 Mn4 O14 176.70(8) . . ? O2 Mn4 O14 83.23(8) . . ? O29 Mn4 O14 97.22(8) . . ? O7 Mn4 O1W 94.35(8) . . ? O2 Mn4 O1W 94.23(8) . . ? O29 Mn4 O1W 85.45(10) . . ? O14 Mn4 O1W 87.41(10) . . ? O7 Mn4 N1A 88.96(8) . . ? O2 Mn4 N1A 91.60(8) . . ? O29 Mn4 N1A 88.76(10) . . ? O14 Mn4 N1A 89.59(10) . . ? O1W Mn4 N1A 173.09(10) . . ? O2 Mn5 O3 81.99(8) . . ? O2 Mn5 O24 95.17(8) . . ? O3 Mn5 O24 173.96(9) . . ? O2 Mn5 O15 173.90(8) . . ? O3 Mn5 O15 93.32(8) . . ? O24 Mn5 O15 89.12(8) . . ? O2 Mn5 O111 98.94(8) . . ? O3 Mn5 O111 96.54(8) . . ? O24 Mn5 O111 89.15(9) . . ? O15 Mn5 O111 85.43(9) . . ? O2 Mn5 O21 90.13(8) . . ? O3 Mn5 O21 86.71(8) . . ? O24 Mn5 O21 87.97(9) . . ? O15 Mn5 O21 85.68(9) . . ? O111 Mn5 O21 170.69(8) . . ? O2 Mn5 Mn1 40.98(5) . . ? O3 Mn5 Mn1 42.52(5) . . ? O24 Mn5 Mn1 133.37(6) . . ? O15 Mn5 Mn1 133.50(6) . . ? O111 Mn5 Mn1 108.99(6) . . ? O21 Mn5 Mn1 79.26(5) . . ? O3 Mn6 O4 96.47(8) . . ? O3 Mn6 O16 174.07(8) . . ? O4 Mn6 O16 88.89(8) . . ? O3 Mn6 O25 89.48(8) . . ? O4 Mn6 O25 173.57(8) . . ? O16 Mn6 O25 85.06(8) . . ? O3 Mn6 O211 93.93(9) . . ? O4 Mn6 O211 98.14(8) . . ? O16 Mn6 O211 87.80(9) . . ? O25 Mn6 O211 83.83(8) . . ? O3 Mn6 N1B 90.31(8) . . ? O4 Mn6 N1B 91.54(8) . . ? O16 Mn6 N1B 86.99(9) . . ? O25 Mn6 N1B 85.98(8) . . ? O211 Mn6 N1B 168.92(8) . . ? O5 Mn7 O4 81.42(8) . . ? O5 Mn7 O17 96.38(8) . . ? O4 Mn7 O17 177.55(8) . . ? O5 Mn7 O26 171.33(8) . . ? O4 Mn7 O26 91.87(8) . . ? O17 Mn7 O26 90.21(8) . . ? O5 Mn7 O2W 97.34(8) . . ? O4 Mn7 O2W 95.53(8) . . ? O17 Mn7 O2W 85.82(8) . . ? O26 Mn7 O2W 88.73(9) . . ? O5 Mn7 O22 89.17(8) . . ? O4 Mn7 O22 89.99(8) . . ? O17 Mn7 O22 88.88(8) . . ? O26 Mn7 O22 85.32(9) . . ? O2W Mn7 O22 172.01(8) . . ? O5 Mn7 Mn2 40.72(5) . . ? O4 Mn7 Mn2 42.56(6) . . ? O17 Mn7 Mn2 135.04(6) . . ? O26 Mn7 Mn2 131.29(6) . . ? O2W Mn7 Mn2 108.15(6) . . ? O22 Mn7 Mn2 79.81(5) . . ? O5 Mn8 O6 95.84(7) . . ? O5 Mn8 O18 179.07(8) . . ? O6 Mn8 O18 84.46(8) . . ? O5 Mn8 O27 84.44(8) . . ? O6 Mn8 O27 178.40(10) . . ? O18 Mn8 O27 95.28(8) . . ? O5 Mn8 O110 93.51(8) . . ? O6 Mn8 O110 92.99(9) . . ? O18 Mn8 O110 87.34(9) . . ? O27 Mn8 O110 85.41(10) . . ? O5 Mn8 N1C 87.34(8) . . ? O6 Mn8 N1C 87.75(8) . . ? O18 Mn8 N1C 91.80(10) . . ? O27 Mn8 N1C 93.84(10) . . ? O110 Mn8 N1C 178.80(9) . . ? O6 Mn9 O7 80.93(7) . . ? O6 Mn9 O28 94.54(8) . . ? O7 Mn9 O28 172.27(8) . . ? O6 Mn9 O19 174.65(8) . . ? O7 Mn9 O19 94.62(8) . . ? O28 Mn9 O19 89.55(8) . . ? O6 Mn9 O210 97.68(8) . . ? O7 Mn9 O210 97.46(8) . . ? O28 Mn9 O210 89.32(9) . . ? O19 Mn9 O210 85.79(8) . . ? O6 Mn9 O23 89.36(8) . . ? O7 Mn9 O23 86.76(8) . . ? O28 Mn9 O23 86.93(9) . . ? O19 Mn9 O23 87.42(8) . . ? O210 Mn9 O23 172.26(8) . . ? O6 Mn9 Mn3 41.05(5) . . ? O7 Mn9 Mn3 41.19(5) . . ? O28 Mn9 Mn3 132.85(6) . . ? O19 Mn9 Mn3 133.94(6) . . ? O210 Mn9 Mn3 108.03(6) . . ? O23 Mn9 Mn3 79.41(5) . . ? Mn2 O1 Mn1 98.06(8) . . ? Mn2 O1 Mn3 100.34(8) . . ? Mn1 O1 Mn3 99.64(8) . . ? Mn1 O2 Mn5 96.86(8) . . ? Mn1 O2 Mn4 129.58(9) . . ? Mn5 O2 Mn4 127.48(9) . . ? Mn1 O3 Mn6 132.86(10) . . ? Mn1 O3 Mn5 93.59(8) . . ? Mn6 O3 Mn5 129.11(10) . . ? Mn2 O4 Mn6 131.59(10) . . ? Mn2 O4 Mn7 93.71(8) . . ? Mn6 O4 Mn7 130.16(10) . . ? Mn2 O5 Mn7 97.30(8) . . ? Mn2 O5 Mn8 127.99(10) . . ? Mn7 O5 Mn8 128.33(9) . . ? Mn3 O6 Mn9 95.85(8) . . ? Mn3 O6 Mn8 129.58(9) . . ? Mn9 O6 Mn8 125.62(9) . . ? Mn3 O7 Mn9 95.61(8) . . ? Mn3 O7 Mn4 130.56(9) . . ? Mn9 O7 Mn4 128.70(9) . . ? C11 O11 Mn1 126.69(18) . . ? C11 O21 Mn5 122.33(17) . . ? O21 C11 O11 124.7(3) . . ? O21 C11 C21 120.4(3) . . ? O11 C11 C21 115.0(3) . . ? C12 O12 Mn2 127.62(19) . . ? C12 O22 Mn7 121.69(18) . . ? O22 C12 O12 124.8(3) . . ? O22 C12 C22 120.4(3) . . ? O12 C12 C22 114.8(3) . . ? C13 O13 Mn3 125.65(18) . . ? C13 O23 Mn9 121.82(17) . . ? O23 C13 O13 125.2(3) . . ? O23 C13 C23 120.0(3) . . ? O13 C13 C23 114.8(2) . . ? C14 O14 Mn4 137.29(19) . . ? C14 O24 Mn5 133.61(18) . . ? O14 C14 O24 126.0(3) . . ? O14 C14 C24 118.2(3) . . ? O24 C14 C24 115.9(3) . . ? C15 O15 Mn5 131.43(17) . . ? C15 O25 Mn6 135.20(18) . . ? O15 C15 O25 126.9(2) . . ? O15 C15 C25 116.9(2) . . ? O25 C15 C25 116.2(2) . . ? C16 O16 Mn6 136.48(18) . . ? C16 O26 Mn7 131.32(18) . . ? O26 C16 O16 126.1(3) . . ? O26 C16 C26 117.1(3) . . ? O16 C16 C26 116.8(3) . . ? C17 O17 Mn7 131.90(18) . . ? C17 O27 Mn8 138.92(19) . . ? O27 C17 O17 126.0(3) . . ? O27 C17 C27 118.3(3) . . ? O17 C17 C27 115.7(3) . . ? C18 O18 Mn8 138.80(19) . . ? C18 O28 Mn9 132.10(18) . . ? O18 C18 O28 126.1(3) . . ? O18 C18 C28 117.2(3) . . ? O28 C18 C28 116.7(3) . . ? C19 O19 Mn9 135.00(18) . . ? C19 O29 Mn4 135.63(19) . . ? O29 C19 O19 126.5(3) . . ? O29 C19 C29 117.4(3) . . ? O19 C19 C29 116.0(2) . . ? C110 O110 C510 99.6(6) . . ? C110 O110 Mn8 129.4(2) . . ? C510 O110 Mn8 123.5(5) . . ? C110 O210 C310 91.0(6) . . ? C110 O210 Mn9 130.3(2) . . ? C310 O210 Mn9 122.0(5) . . ? O210 C110 O110 129.9(4) . . ? O210 C110 C210 115.4(4) . . ? O110 C110 C210 114.7(4) . . ? O210 C310 O1W 138.2(10) . . ? O210 C310 C410 109.6(10) . . ? O1W C310 C410 111.9(10) . . ? O2W C510 O110 136.5(9) . . ? O2W C510 C610 111.7(9) . . ? O110 C510 C610 111.8(9) . . ? C111 O111 C511 107.3(6) . . ? C111 O111 Mn5 123.4(2) . . ? C511 O111 Mn5 123.8(5) . . ? C111 O211 C311 101.2(6) . . ? C111 O211 Mn6 129.5(2) . . ? C311 O211 Mn6 117.6(5) . . ? O111 C111 O211 129.7(4) . . ? O111 C111 C211 114.0(4) . . ? O211 C111 C211 116.3(4) . . ? O211 C311 O2W 140.8(10) . . ? O211 C311 C411 108.0(9) . . ? O2W C311 C411 111.1(9) . . ? O1W C511 O111 131.8(9) . . ? O1W C511 C611 116.1(9) . . ? O111 C511 C611 111.7(9) . . ? C511 O1W C310 90.8(8) . . ? C511 O1W Mn4 127.7(5) . . ? C310 O1W Mn4 123.7(5) . . ? C510 O2W C311 99.9(8) . . ? C510 O2W Mn7 125.0(5) . . ? C311 O2W Mn7 120.3(5) . . ? C6A N1A C2A 117.6(3) . . ? C6A N1A Mn4 120.6(2) . . ? C2A N1A Mn4 120.5(2) . . ? N1A C2A C3A 123.0(3) . . ? C4A C3A C2A 119.7(4) . . ? C3A C4A C5A 117.4(4) . . ? C6A C5A C4A 119.8(4) . . ? N1A C6A C5A 122.5(4) . . ? C2B N1B C6B 117.4(3) . . ? C2B N1B Mn6 119.79(19) . . ? C6B N1B Mn6 122.8(2) . . ? N1B C2B C3B 122.9(3) . . ? C2B C3B C4B 119.2(3) . . ? C5B C4B C3B 118.7(3) . . ? C4B C5B C6B 119.3(3) . . ? N1B C6B C5B 122.6(3) . . ? C2C N1C C6C 117.4(3) . . ? C2C N1C Mn8 120.1(2) . . ? C6C N1C Mn8 120.2(2) . . ? N1C C2C C3C 122.9(4) . . ? C4C C3C C2C 118.5(4) . . ? C5C C4C C3C 119.0(4) . . ? C6C C5C C4C 118.2(4) . . ? N1C C6C C5C 124.0(4) . . ? C1T O1T Mn2 120.92(15) . . ? C1T O1T Mn1 121.14(15) . . ? Mn2 O1T Mn1 95.26(7) . . ? O1T C1T C4T 113.0(2) . . ? C2T O2T Mn2 120.24(15) . . ? C2T O2T Mn3 119.61(15) . . ? Mn2 O2T Mn3 97.25(7) . . ? O2T C2T C4T 114.4(2) . . ? C3T O3T Mn1 120.00(15) . . ? C3T O3T Mn3 120.11(15) . . ? Mn1 O3T Mn3 96.84(8) . . ? O3T C3T C4T 114.2(2) . . ? C2T C4T C5T 108.3(2) . . ? C2T C4T C1T 110.2(2) . . ? C5T C4T C1T 108.4(2) . . ? C2T C4T C3T 111.1(2) . . ? C5T C4T C3T 108.7(2) . . ? C1T C4T C3T 110.1(2) . . ? N1Y C2Y C3Y 175.9(11) . . ? N1Z C2Z C3Z 179.1(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.632 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.079