# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Euan Brechin' _publ_contact_author_email EBRECHIN@STAFFMAIL.ED.AC.UK _publ_section_title ; New Structural Types and Different Oxidation Levels in the Family of Mn6-oxime Single-Molecule Magnets ; loop_ _publ_author_name 'Euan Brechin' 'Martyn E. Cochrane' 'Anna Collins' 'Ross Inglis' 'Leigh F. Jones' 'Kevin Mason' ; S.Parsons ; 'Spyros Perlepes' # Attachment '1.cif' data_EB7205 _database_code_depnum_ccdc_archive 'CCDC 693561' _cell_length_a 12.9999(5) _cell_length_b 11.2786(5) _cell_length_c 25.7117(11) _cell_angle_alpha 90 _cell_angle_beta 102.471(2) _cell_angle_gamma 90 _cell_volume 3680.9(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C40 H50 Br4 Mn6 N8 O20 # Dc = 1.45 Fooo = 1816.00 Mu = 32.28 M = 806.03 # Found Formula = C66 H90 Br2 Mn6 N6 O20 # Dc = 1.60 FOOO = 1816.00 Mu = 21.57 M = 888.42 _chemical_formula_sum 'C66 H90 Br2 Mn6 N6 O20' _chemical_formula_moiety 'C66 H90 Br2 Mn6 N6 O20' _chemical_compound_source ? _chemical_formula_weight 1776.84 _cell_measurement_reflns_used 8028 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 30.36 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_max 0.31 _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 2.157 # Sheldrick geometric approximatio 0.66 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.86 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _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 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 30552 _reflns_number_total 10248 _diffrn_reflns_av_R_equivalents 0.054 # Number of reflections with Friedels Law is 10248 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11250 _diffrn_reflns_theta_min 1.979 _diffrn_reflns_theta_max 30.521 _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 28.079 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _reflns_limit_h_min -17 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 35 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.01 _refine_diff_density_max 1.07 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 10248 _refine_ls_number_restraints 19 _refine_ls_number_parameters 469 _oxford_refine_ls_R_factor_ref 0.0750 _refine_ls_wR_factor_ref 0.1020 _refine_ls_goodness_of_fit_ref 0.8779 _refine_ls_shift/su_max 0.001919 # The values computed from all data _oxford_reflns_number_all 10248 _refine_ls_R_factor_all 0.0750 _refine_ls_wR_factor_all 0.1020 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7474 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_gt 0.0903 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Br1 Br 1.07000(3) 0.26740(3) 0.407516(15) 0.0209 1.0000 Uani . . . . . . . Mn1 Mn 0.86940(4) -0.03649(5) 0.34919(2) 0.0155 1.0000 Uani . . . . . . . Mn2 Mn 0.79337(4) 0.12131(5) 0.43956(2) 0.0137 1.0000 Uani . . . . . . . Mn3 Mn 1.04296(4) 0.05726(4) 0.45205(2) 0.0126 1.0000 Uani . . . . . . . O1 O 0.90297(17) 0.0484(2) 0.41357(9) 0.0134 1.0000 Uani . . . . . . . O2 O 0.8324(2) -0.1228(3) 0.28673(10) 0.0285 1.0000 Uani . . . . . . . O3 O 0.68785(18) 0.0525(2) 0.38489(9) 0.0183 1.0000 Uani . . . . . . . O4 O 0.69223(18) 0.1990(2) 0.46844(10) 0.0182 1.0000 Uani . . . . . . . O5 O 0.99410(18) 0.1283(2) 0.51191(9) 0.0139 1.0000 Uani . . . . . . . O6 O 1.18139(18) 0.0380(2) 0.49522(9) 0.0150 1.0000 Uani . . . . . . . O7 O 1.01036(18) -0.0992(2) 0.36182(9) 0.0176 1.0000 Uani . . . . . . . O8 O 0.9165(2) 0.1264(2) 0.30746(10) 0.0266 1.0000 Uani . . . . . . . O9 O 0.8063(2) -0.1814(2) 0.39669(10) 0.0230 1.0000 Uani . . . . . . . O10 O 0.8128(2) 0.2780(2) 0.38713(10) 0.0237 1.0000 Uani . . . . . . . N1 N 0.7189(2) 0.0205(3) 0.33912(11) 0.0160 1.0000 Uani . . . . . . . N2 N 0.9033(2) 0.1961(2) 0.49601(11) 0.0138 1.0000 Uani . . . . . . . N3 N 1.0874(2) -0.0335(2) 0.39374(11) 0.0149 1.0000 Uani . . . . . . . C4 C 0.9779(3) 0.3819(4) 0.60974(16) 0.0337 1.0000 Uani . . . . . . . C5 C 0.7516(3) 0.3743(4) 0.36078(16) 0.0331 1.0000 Uani . . . . . . . C6 C 0.9508(4) 0.1438(4) 0.25863(17) 0.0400 1.0000 Uani . U . . . . . C7 C 0.7577(4) 0.3813(5) 0.30346(18) 0.0532 1.0000 Uani . . . . . . . C8 C 1.0500(4) 0.0810(5) 0.2576(2) 0.0596 1.0000 Uani . U . . . . . C14 C 0.7033(3) 0.3145(3) 0.47996(13) 0.0163 1.0000 Uani . . . . . . . C15 C 1.2661(3) 0.0571(3) 0.47343(14) 0.0158 1.0000 Uani . . . . . . . C16 C 1.1832(3) -0.0444(3) 0.38674(14) 0.0192 1.0000 Uani . . . . . . . C17 C 0.8026(3) 0.4903(3) 0.51291(15) 0.0218 1.0000 Uani . . . . . . . C18 C 0.8993(3) 0.3004(3) 0.51707(13) 0.0159 1.0000 Uani . . . . . . . C19 C 1.3548(3) 0.1089(3) 0.50504(14) 0.0189 1.0000 Uani . . . . . . . C20 C 0.8012(3) 0.3681(3) 0.50264(13) 0.0165 1.0000 Uani . . . . . . . C21 C 1.3596(3) 0.0494(4) 0.40222(15) 0.0250 1.0000 Uani . . . . . . . C22 C 1.2682(3) 0.0223(3) 0.42091(14) 0.0168 1.0000 Uani . . . . . . . C23 C 1.4437(3) 0.1328(3) 0.48554(16) 0.0238 1.0000 Uani . . . . . . . C24 C 0.6442(3) 0.0118(3) 0.29683(14) 0.0178 1.0000 Uani . . . . . . . C25 C 0.6175(3) 0.5057(3) 0.47918(15) 0.0245 1.0000 Uani . . . . . . . C26 C 0.5326(3) 0.0398(4) 0.30036(15) 0.0265 1.0000 Uani . . . . . . . C27 C 1.4451(3) 0.1047(4) 0.43315(16) 0.0256 1.0000 Uani . . . . . . . C28 C 0.9931(3) 0.3538(3) 0.55390(15) 0.0242 1.0000 Uani . . . . . . . C29 C 0.7131(3) 0.5587(3) 0.50128(15) 0.0246 1.0000 Uani . . . . . . . C30 C 0.6128(3) 0.3857(3) 0.46904(14) 0.0211 1.0000 Uani . . . . . . . C31 C 1.2813(3) -0.2268(4) 0.36797(19) 0.0402 1.0000 Uani . . . . . . . C32 C 0.5977(3) -0.0022(4) 0.19829(15) 0.0283 1.0000 Uani . . . . . . . C34 C 0.5086(3) 0.1723(4) 0.29791(18) 0.0409 1.0000 Uani . . . . . . . C37 C 0.6687(3) -0.0270(3) 0.24637(14) 0.0209 1.0000 Uani . . . . . . . C39 C 0.7608(3) -0.0909(4) 0.24387(15) 0.0255 1.0000 Uani . . . . . . . C40 C 0.7040(4) -0.1007(4) 0.14771(17) 0.0379 1.0000 Uani . . . . . . . C42 C 0.7757(3) -0.1277(4) 0.19374(16) 0.0344 1.0000 Uani . . . . . . . C43 C 1.2078(3) -0.1256(4) 0.34437(15) 0.0263 1.0000 Uani . . . . . . . C58 C 0.6142(4) -0.0372(4) 0.14946(16) 0.0377 1.0000 Uani . . . . . . . C101 C 0.7147(16) -0.2521(17) 0.3789(8) 0.0378 0.2700 Uani D U . 1 1 . . C102 C 0.7043(14) -0.3120(14) 0.3275(6) 0.0374 0.2700 Uani D U . 1 1 . . C201 C 0.7540(5) -0.2914(6) 0.3808(3) 0.0348 0.7300 Uani . U . 1 2 . . C202 C 0.6388(5) -0.2778(6) 0.3579(3) 0.0524 0.7300 Uani . U . 1 2 . . H14 H 0.9608 0.1588 0.3316 0.0425 1.0000 Uiso R . . . . . . H17 H 0.8661 0.5254 0.5281 0.0257 1.0000 Uiso R . . . . . . H19 H 1.3551 0.1266 0.5401 0.0226 1.0000 Uiso R . . . . . . H21 H 1.3623 0.0298 0.3675 0.0308 1.0000 Uiso R . . . . . . H23 H 1.5029 0.1664 0.5076 0.0278 1.0000 Uiso R . . . . . . H25 H 0.5573 0.5509 0.4715 0.0297 1.0000 Uiso R . . . . . . H27 H 1.5039 0.1207 0.4201 0.0317 1.0000 Uiso R . . . . . . H29 H 0.7186 0.6394 0.5088 0.0304 1.0000 Uiso R . . . . . . H30 H 0.5483 0.3518 0.4548 0.0252 1.0000 Uiso R . . . . . . H32 H 0.5383 0.0390 0.1997 0.0330 1.0000 Uiso R . . . . . . H40 H 0.7161 -0.1258 0.1155 0.0448 1.0000 Uiso R . . . . . . H42 H 0.8350 -0.1696 0.1919 0.0410 1.0000 Uiso R . . . . . . H43 H 1.0372 0.4251 0.6296 0.0468 1.0000 Uiso R . . . . . . H44 H 0.9160 0.4273 0.6074 0.0470 1.0000 Uiso R . . . . . . H45 H 0.9704 0.3092 0.6283 0.0469 1.0000 Uiso R . . . . . . H51 H 0.6788 0.3631 0.3631 0.0412 1.0000 Uiso R . . . . . . H52 H 0.7770 0.4487 0.3786 0.0411 1.0000 Uiso R . . . . . . H58 H 0.5656 -0.0185 0.1190 0.0425 1.0000 Uiso R . . . . . . H61 H 0.9615 0.2286 0.2531 0.0470 1.0000 Uiso R . . . . . . H62 H 0.8967 0.1132 0.2299 0.0471 1.0000 Uiso R . . . . . . H71 H 0.7141 0.4458 0.2869 0.0769 1.0000 Uiso R . . . . . . H72 H 0.7328 0.3082 0.2859 0.0769 1.0000 Uiso R . . . . . . H73 H 0.8299 0.3956 0.3007 0.0768 1.0000 Uiso R . . . . . . H81 H 1.1039 0.1036 0.2878 0.0979 1.0000 Uiso R . . . . . . H82 H 1.0721 0.1024 0.2252 0.0979 1.0000 Uiso R . . . . . . H83 H 1.0360 -0.0029 0.2580 0.0979 1.0000 Uiso R . . . . . . H171 H 0.8128 -0.1627 0.4281 0.0334 1.0000 Uiso R . . . . . . H261 H 0.5206 0.0101 0.3335 0.0302 1.0000 Uiso R . . . . . . H262 H 0.4850 0.0014 0.2715 0.0307 1.0000 Uiso R . . . . . . H281 H 1.0097 0.4271 0.5380 0.0277 1.0000 Uiso R . . . . . . H282 H 1.0516 0.3023 0.5564 0.0282 1.0000 Uiso R . . . . . . H311 H 1.2929 -0.2750 0.3393 0.0610 1.0000 Uiso R . . . . . . H312 H 1.2474 -0.2722 0.3909 0.0608 1.0000 Uiso R . . . . . . H313 H 1.3472 -0.1956 0.3877 0.0606 1.0000 Uiso R . . . . . . H341 H 0.5531 0.2123 0.3273 0.0596 1.0000 Uiso R . . . . . . H342 H 0.4368 0.1865 0.2989 0.0599 1.0000 Uiso R . . . . . . H343 H 0.5209 0.2070 0.2657 0.0598 1.0000 Uiso R . . . . . . H351 H 0.8772 0.2901 0.3929 0.0359 1.0000 Uiso R . . . . . . H431 H 1.1429 -0.1567 0.3241 0.0317 1.0000 Uiso R . . . . . . H432 H 1.2404 -0.0791 0.3207 0.0320 1.0000 Uiso R . . . . . . H1011 H 0.7127 -0.3116 0.4059 0.0380 0.2700 Uiso R . . 1 1 . . H1012 H 0.6536 -0.2000 0.3754 0.0381 0.2700 Uiso R . . 1 1 . . H1021 H 0.6475 -0.3680 0.3231 0.0480 0.2700 Uiso R . . 1 1 . . H1022 H 0.7682 -0.3534 0.3261 0.0480 0.2700 Uiso R . . 1 1 . . H1023 H 0.6892 -0.2560 0.2986 0.0479 0.2700 Uiso R . . 1 1 . . H2011 H 0.7635 -0.3445 0.4115 0.0410 0.7300 Uiso R . . 1 2 . . H2012 H 0.7860 -0.3280 0.3540 0.0410 0.7300 Uiso R . . 1 2 . . H2021 H 0.6068 -0.3539 0.3481 0.0737 0.7300 Uiso R . . 1 2 . . H2022 H 0.6042 -0.2403 0.3828 0.0742 0.7300 Uiso R . . 1 2 . . H2023 H 0.6284 -0.2301 0.3262 0.0740 0.7300 Uiso R . . 1 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 Br1 0.02162(18) 0.01601(17) 0.02535(19) 0.00142(15) 0.00593(15) -0.00519(14) Mn1 0.0125(2) 0.0180(3) 0.0151(2) -0.0039(2) 0.00079(19) 0.0014(2) Mn2 0.0112(2) 0.0143(2) 0.0153(2) -0.0019(2) 0.00249(19) 0.0005(2) Mn3 0.0112(2) 0.0135(2) 0.0130(2) -0.00066(19) 0.00230(19) 0.00028(19) O1 0.0136(11) 0.0123(11) 0.0140(11) -0.0026(9) 0.0023(9) 0.0008(9) O2 0.0223(14) 0.0362(16) 0.0235(14) -0.0125(12) -0.0028(11) 0.0105(12) O3 0.0145(12) 0.0259(14) 0.0146(12) -0.0062(10) 0.0034(9) -0.0015(10) O4 0.0147(12) 0.0161(12) 0.0246(13) -0.0063(10) 0.0063(10) 0.0007(10) O5 0.0135(11) 0.0138(11) 0.0140(11) 0.0000(9) 0.0025(9) 0.0028(9) O6 0.0133(11) 0.0171(12) 0.0151(11) 0.0022(9) 0.0044(9) -0.0012(9) O7 0.0132(12) 0.0195(13) 0.0198(13) -0.0055(10) 0.0029(10) -0.0006(10) O8 0.0320(15) 0.0282(15) 0.0213(14) 0.0032(12) 0.0092(12) -0.0004(12) O9 0.0235(14) 0.0196(13) 0.0235(14) -0.0020(11) 0.0001(11) -0.0050(11) O10 0.0202(13) 0.0231(14) 0.0287(15) 0.0074(12) 0.0068(11) 0.0027(11) N1 0.0147(14) 0.0180(15) 0.0156(14) -0.0014(11) 0.0036(11) 0.0004(11) N2 0.0116(13) 0.0157(14) 0.0144(13) 0.0018(11) 0.0037(11) 0.0014(11) N3 0.0148(14) 0.0131(13) 0.0166(14) -0.0008(11) 0.0031(11) -0.0005(11) C4 0.043(3) 0.023(2) 0.028(2) -0.0003(17) -0.0071(19) -0.0029(19) C5 0.038(2) 0.028(2) 0.033(2) 0.0089(18) 0.009(2) 0.0126(19) C6 0.048(3) 0.049(3) 0.026(2) 0.013(2) 0.012(2) 0.002(2) C7 0.057(3) 0.069(4) 0.034(3) 0.026(3) 0.010(2) 0.022(3) C8 0.067(4) 0.076(4) 0.043(3) 0.012(3) 0.030(3) 0.027(3) C14 0.0204(17) 0.0154(16) 0.0150(16) -0.0002(13) 0.0075(14) -0.0006(14) C15 0.0128(15) 0.0162(16) 0.0185(17) 0.0010(13) 0.0035(13) 0.0002(13) C16 0.0176(17) 0.0192(17) 0.0208(17) 0.0005(14) 0.0041(14) -0.0010(14) C17 0.0202(18) 0.0203(18) 0.0239(19) -0.0010(15) 0.0028(15) -0.0009(15) C18 0.0163(16) 0.0162(16) 0.0154(16) -0.0019(13) 0.0038(13) -0.0035(13) C19 0.0177(17) 0.0224(18) 0.0167(16) -0.0008(14) 0.0038(14) -0.0023(14) C20 0.0179(17) 0.0176(17) 0.0143(15) -0.0010(13) 0.0038(13) 0.0036(14) C21 0.0202(18) 0.035(2) 0.0227(19) -0.0025(17) 0.0103(15) -0.0033(17) C22 0.0141(16) 0.0186(17) 0.0181(17) 0.0026(13) 0.0045(13) 0.0008(13) C23 0.0148(17) 0.026(2) 0.031(2) -0.0007(17) 0.0045(15) -0.0045(15) C24 0.0165(17) 0.0172(17) 0.0192(17) 0.0001(14) 0.0026(14) -0.0006(13) C25 0.025(2) 0.0232(19) 0.026(2) 0.0021(16) 0.0070(16) 0.0095(16) C26 0.0145(17) 0.041(2) 0.0232(19) -0.0069(18) 0.0010(15) 0.0054(17) C27 0.0158(17) 0.032(2) 0.031(2) 0.0011(17) 0.0095(16) -0.0043(16) C28 0.0192(18) 0.0186(18) 0.032(2) -0.0051(16) -0.0013(16) 0.0034(15) C29 0.031(2) 0.0176(18) 0.026(2) -0.0036(15) 0.0079(17) 0.0060(16) C30 0.0169(17) 0.0224(19) 0.0242(19) -0.0007(15) 0.0048(15) 0.0032(15) C31 0.036(2) 0.037(3) 0.050(3) -0.014(2) 0.014(2) 0.010(2) C32 0.025(2) 0.036(2) 0.0215(19) -0.0013(17) -0.0024(16) 0.0080(18) C34 0.033(2) 0.047(3) 0.041(3) -0.002(2) 0.005(2) 0.019(2) C37 0.0213(18) 0.0220(19) 0.0180(17) -0.0037(14) 0.0010(14) -0.0024(15) C39 0.0219(19) 0.029(2) 0.024(2) -0.0071(16) 0.0015(16) 0.0003(16) C40 0.041(3) 0.051(3) 0.022(2) -0.012(2) 0.0071(19) -0.004(2) C42 0.029(2) 0.050(3) 0.024(2) -0.015(2) 0.0055(18) 0.004(2) C43 0.0186(18) 0.035(2) 0.027(2) -0.0117(18) 0.0087(16) 0.0002(17) C58 0.039(3) 0.049(3) 0.020(2) -0.002(2) -0.0043(19) 0.004(2) C101 0.040(8) 0.033(8) 0.042(8) -0.006(7) 0.013(7) -0.014(6) C102 0.041(8) 0.029(7) 0.044(8) -0.008(6) 0.012(7) -0.018(6) C201 0.033(4) 0.021(3) 0.046(4) 0.000(3) -0.001(3) -0.008(3) C202 0.039(4) 0.044(4) 0.063(4) -0.015(3) -0.015(3) -0.012(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.30603(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 . Mn3 . 2.6881(6) yes Mn1 . Mn2 . 3.2458(7) yes Mn1 . Mn3 . 3.2598(7) yes Mn1 . O1 . 1.880(2) yes Mn1 . O2 . 1.850(3) yes Mn1 . O7 . 1.925(2) yes Mn1 . O8 . 2.277(3) yes Mn1 . O9 . 2.296(3) yes Mn1 . N1 . 2.022(3) yes Mn2 . O6 2_756 2.432(2) yes Mn2 . O1 . 1.888(2) yes Mn2 . O3 . 1.904(2) yes Mn2 . O4 . 1.862(2) yes Mn2 . O10 . 2.270(2) yes Mn2 . N2 . 1.991(3) yes Mn3 . O5 2_756 2.380(2) yes Mn3 . Mn3 2_756 3.1915(10) yes Mn3 . O1 . 1.877(2) yes Mn3 . O5 . 1.959(2) yes Mn3 . O6 . 1.912(2) yes Mn3 . N3 . 2.001(3) yes O2 . C39 . 1.330(4) yes O3 . N1 . 1.373(3) yes O4 . C14 . 1.337(4) yes O5 . N2 . 1.391(3) yes O6 . C15 . 1.357(4) yes O7 . N3 . 1.368(3) yes O8 . C6 . 1.434(4) yes O8 . H14 . 0.833 no O9 . C101 . 1.424(19) yes O9 . H171 . 0.820 no O9 . C201 . 1.431(7) yes O9 . H171 . 0.820 no O10 . C5 . 1.427(4) yes O10 . H351 . 0.830 no N1 . C24 . 1.296(4) yes N2 . C18 . 1.301(4) yes N3 . C16 . 1.302(4) yes C4 . C28 . 1.524(5) yes C4 . H43 . 0.961 no C4 . H44 . 0.945 no C4 . H45 . 0.963 no C5 . C7 . 1.495(6) yes C5 . H51 . 0.970 no C5 . H52 . 0.978 no C6 . C8 . 1.477(6) yes C6 . H61 . 0.982 no C6 . H62 . 0.967 no C7 . H71 . 0.964 no C7 . H72 . 0.961 no C7 . H73 . 0.969 no C8 . H81 . 0.961 no C8 . H82 . 0.968 no C8 . H83 . 0.964 no C14 . C20 . 1.415(5) yes C14 . C30 . 1.403(5) yes C15 . C19 . 1.388(5) yes C15 . C22 . 1.412(5) yes C16 . C22 . 1.463(5) yes C16 . C43 . 1.509(5) yes C17 . C20 . 1.402(5) yes C17 . C29 . 1.374(5) yes C17 . H17 . 0.923 no C18 . C20 . 1.464(5) yes C18 . C28 . 1.499(5) yes C19 . C23 . 1.382(5) yes C19 . H19 . 0.922 no C21 . C22 . 1.408(5) yes C21 . C27 . 1.369(5) yes C21 . H21 . 0.927 no C23 . C27 . 1.388(5) yes C23 . H23 . 0.933 no C24 . C26 . 1.507(5) yes C24 . C37 . 1.468(5) yes C25 . C29 . 1.386(5) yes C25 . C30 . 1.377(5) yes C25 . H25 . 0.919 no C26 . C34 . 1.525(6) yes C26 . H261 . 0.960 no C26 . H262 . 0.960 no C27 . H27 . 0.918 no C28 . H281 . 0.967 no C28 . H282 . 0.948 no C29 . H29 . 0.929 no C30 . H30 . 0.922 no C31 . C43 . 1.528(5) yes C31 . H311 . 0.955 no C31 . H312 . 0.958 no C31 . H313 . 0.963 no C32 . C37 . 1.401(5) yes C32 . C58 . 1.376(5) yes C32 . H32 . 0.910 no C34 . H341 . 0.960 no C34 . H342 . 0.953 no C34 . H343 . 0.960 no C37 . C39 . 1.411(5) yes C39 . C42 . 1.407(5) yes C40 . C42 . 1.373(6) yes C40 . C58 . 1.379(6) yes C40 . H40 . 0.921 no C42 . H42 . 0.915 no C43 . H431 . 0.958 no C43 . H432 . 0.967 no C58 . H58 . 0.919 no C101 . C102 . 1.47(2) yes C101 . H1011 . 0.970 no C101 . H1012 . 0.976 no C102 . H1021 . 0.959 no C102 . H1022 . 0.960 no C102 . H1023 . 0.962 no C201 . C202 . 1.494(9) yes C201 . H2011 . 0.977 no C201 . H2012 . 0.970 no C202 . H2021 . 0.964 no C202 . H2022 . 0.957 no C202 . H2023 . 0.961 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Mn2 . Mn1 . Mn3 . 60.381(16) yes Mn2 . Mn1 . O1 . 30.59(7) yes Mn3 . Mn1 . O1 . 29.79(7) yes Mn2 . Mn1 . O2 . 147.95(8) yes Mn3 . Mn1 . O2 . 151.55(8) yes O1 . Mn1 . O2 . 177.89(12) yes Mn2 . Mn1 . O7 . 120.43(7) yes Mn3 . Mn1 . O7 . 61.01(7) yes O1 . Mn1 . O7 . 90.40(10) yes O2 . Mn1 . O7 . 90.72(11) yes Mn2 . Mn1 . O8 . 92.83(7) yes Mn3 . Mn1 . O8 . 84.90(7) yes O1 . Mn1 . O8 . 88.22(10) yes O2 . Mn1 . O8 . 93.53(12) yes O7 . Mn1 . O8 . 91.87(10) yes Mn2 . Mn1 . O9 . 79.07(7) yes Mn3 . Mn1 . O9 . 93.65(7) yes O1 . Mn1 . O9 . 86.33(10) yes O2 . Mn1 . O9 . 91.80(11) yes O7 . Mn1 . O9 . 94.90(10) yes Mn2 . Mn1 . N1 . 58.77(8) yes Mn3 . Mn1 . N1 . 118.80(8) yes O1 . Mn1 . N1 . 89.14(11) yes O2 . Mn1 . N1 . 89.62(11) yes O7 . Mn1 . N1 . 176.12(11) yes O8 . Mn1 . O9 . 171.33(10) yes O8 . Mn1 . N1 . 91.96(11) yes O9 . Mn1 . N1 . 81.23(10) yes O6 2_756 Mn2 . Mn1 . 94.12(6) yes O6 2_756 Mn2 . O1 . 85.56(9) yes Mn1 . Mn2 . O1 . 30.46(7) yes O6 2_756 Mn2 . O3 . 100.16(10) yes Mn1 . Mn2 . O3 . 61.99(7) yes O1 . Mn2 . O3 . 92.28(10) yes O6 2_756 Mn2 . O4 . 94.26(10) yes Mn1 . Mn2 . O4 . 153.33(8) yes O1 . Mn2 . O4 . 176.09(10) yes O3 . Mn2 . O4 . 91.60(10) yes O6 2_756 Mn2 . O10 . 165.80(9) yes Mn1 . Mn2 . O10 . 84.95(7) yes O1 . Mn2 . O10 . 86.55(9) yes O3 . Mn2 . O10 . 91.93(10) yes O4 . Mn2 . O10 . 92.81(10) yes O6 2_756 Mn2 . N2 . 80.88(10) yes Mn1 . Mn2 . N2 . 118.18(8) yes O1 . Mn2 . N2 . 87.96(10) yes O3 . Mn2 . N2 . 178.95(11) yes O4 . Mn2 . N2 . 88.15(11) yes O10 . Mn2 . N2 . 87.06(10) yes Br1 . Mn3 . O5 2_756 175.81(6) yes Br1 . Mn3 . Mn3 2_756 141.79(3) yes O5 2_756 Mn3 . Mn3 2_756 37.74(5) yes Br1 . Mn3 . Mn1 . 94.109(19) yes O5 2_756 Mn3 . Mn1 . 82.40(6) yes Mn3 2_756 Mn3 . Mn1 . 101.49(2) yes Br1 . Mn3 . O1 . 91.34(7) yes O5 2_756 Mn3 . O1 . 84.48(9) yes Mn3 2_756 Mn3 . O1 . 85.67(7) yes Mn1 . Mn3 . O1 . 29.85(7) yes Br1 . Mn3 . O5 . 93.93(7) yes O5 2_756 Mn3 . O5 . 85.78(9) yes Mn3 2_756 Mn3 . O5 . 48.05(7) yes Mn1 . Mn3 . O5 . 119.02(7) yes O1 . Mn3 . O5 . 89.65(10) yes Br1 . Mn3 . O6 . 98.86(7) yes O5 2_756 Mn3 . O6 . 85.33(9) yes Mn3 2_756 Mn3 . O6 . 87.03(7) yes Mn1 . Mn3 . O6 . 146.52(7) yes O1 . Mn3 . O6 . 169.73(10) yes Br1 . Mn3 . N3 . 92.65(8) yes O5 2_756 Mn3 . N3 . 87.57(10) yes Mn3 2_756 Mn3 . N3 . 125.30(8) yes Mn1 . Mn3 . N3 . 59.16(8) yes O1 . Mn3 . N3 . 88.96(10) yes O5 . Mn3 . O6 . 90.83(10) yes O5 . Mn3 . N3 . 173.31(11) yes O6 . Mn3 . N3 . 89.38(11) yes Mn2 . O1 . Mn1 . 118.94(12) yes Mn2 . O1 . Mn3 . 120.69(12) yes Mn1 . O1 . Mn3 . 120.35(12) yes Mn1 . O2 . C39 . 125.5(2) yes Mn2 . O3 . N1 . 116.20(19) yes Mn2 . O4 . C14 . 119.7(2) yes Mn3 2_756 O5 . Mn3 . 94.22(9) yes Mn3 2_756 O5 . N2 . 111.56(17) yes Mn3 . O5 . N2 . 113.09(17) yes Mn2 2_756 O6 . Mn3 . 117.01(10) yes Mn2 2_756 O6 . C15 . 113.65(19) yes Mn3 . O6 . C15 . 119.3(2) yes Mn1 . O7 . N3 . 116.69(19) yes Mn1 . O8 . C6 . 133.5(3) yes Mn1 . O8 . H14 . 102.5 no C6 . O8 . H14 . 107.2 no Mn1 . O9 . C101 . 126.7(9) yes Mn1 . O9 . H171 . 111.6 no C101 . O9 . H171 . 111.1 no Mn1 . O9 . C201 . 131.9(4) yes Mn1 . O9 . H171 . 111.6 no C201 . O9 . H171 . 116.4 no Mn2 . O10 . C5 . 138.8(2) yes Mn2 . O10 . H351 . 105.0 no C5 . O10 . H351 . 113.4 no O3 . N1 . Mn1 . 115.4(2) yes O3 . N1 . C24 . 115.7(3) yes Mn1 . N1 . C24 . 127.8(2) yes O5 . N2 . Mn2 . 114.30(19) yes O5 . N2 . C18 . 118.8(3) yes Mn2 . N2 . C18 . 126.8(2) yes O7 . N3 . Mn3 . 115.7(2) yes O7 . N3 . C16 . 117.6(3) yes Mn3 . N3 . C16 . 126.3(2) yes C28 . C4 . H43 . 110.7 no C28 . C4 . H44 . 109.6 no H43 . C4 . H44 . 109.4 no C28 . C4 . H45 . 109.7 no H43 . C4 . H45 . 108.9 no H44 . C4 . H45 . 108.4 no O10 . C5 . C7 . 111.5(4) yes O10 . C5 . H51 . 108.8 no C7 . C5 . H51 . 109.1 no O10 . C5 . H52 . 109.5 no C7 . C5 . H52 . 109.3 no H51 . C5 . H52 . 108.6 no O8 . C6 . C8 . 112.8(4) yes O8 . C6 . H61 . 109.9 no C8 . C6 . H61 . 108.3 no O8 . C6 . H62 . 107.9 no C8 . C6 . H62 . 108.1 no H61 . C6 . H62 . 109.8 no C5 . C7 . H71 . 108.9 no C5 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.5 no C5 . C7 . H73 . 109.8 no H71 . C7 . H73 . 109.2 no H72 . C7 . H73 . 109.9 no C6 . C8 . H81 . 110.2 no C6 . C8 . H82 . 108.5 no H81 . C8 . H82 . 109.2 no C6 . C8 . H83 . 107.6 no H81 . C8 . H83 . 111.0 no H82 . C8 . H83 . 110.3 no O4 . C14 . C20 . 123.5(3) yes O4 . C14 . C30 . 117.9(3) yes C20 . C14 . C30 . 118.6(3) yes O6 . C15 . C19 . 118.1(3) yes O6 . C15 . C22 . 122.4(3) yes C19 . C15 . C22 . 119.5(3) yes N3 . C16 . C22 . 119.3(3) yes N3 . C16 . C43 . 121.0(3) yes C22 . C16 . C43 . 119.7(3) yes C20 . C17 . C29 . 122.4(4) yes C20 . C17 . H17 . 118.4 no C29 . C17 . H17 . 119.2 no N2 . C18 . C20 . 118.5(3) yes N2 . C18 . C28 . 121.7(3) yes C20 . C18 . C28 . 119.7(3) yes C15 . C19 . C23 . 121.6(3) yes C15 . C19 . H19 . 119.4 no C23 . C19 . H19 . 119.0 no C18 . C20 . C14 . 122.6(3) yes C18 . C20 . C17 . 119.3(3) yes C14 . C20 . C17 . 118.1(3) yes C22 . C21 . C27 . 122.6(4) yes C22 . C21 . H21 . 119.1 no C27 . C21 . H21 . 118.3 no C16 . C22 . C15 . 123.3(3) yes C16 . C22 . C21 . 119.3(3) yes C15 . C22 . C21 . 117.3(3) yes C19 . C23 . C27 . 119.7(3) yes C19 . C23 . H23 . 120.2 no C27 . C23 . H23 . 120.1 no N1 . C24 . C26 . 119.4(3) yes N1 . C24 . C37 . 119.9(3) yes C26 . C24 . C37 . 120.7(3) yes C29 . C25 . C30 . 120.1(4) yes C29 . C25 . H25 . 119.7 no C30 . C25 . H25 . 120.2 no C24 . C26 . C34 . 113.2(3) yes C24 . C26 . H261 . 108.9 no C34 . C26 . H261 . 107.9 no C24 . C26 . H262 . 109.1 no C34 . C26 . H262 . 108.5 no H261 . C26 . H262 . 109.1 no C23 . C27 . C21 . 119.3(3) yes C23 . C27 . H27 . 119.8 no C21 . C27 . H27 . 120.9 no C4 . C28 . C18 . 115.2(3) yes C4 . C28 . H281 . 107.8 no C18 . C28 . H281 . 107.6 no C4 . C28 . H282 . 109.2 no C18 . C28 . H282 . 109.1 no H281 . C28 . H282 . 107.7 no C25 . C29 . C17 . 119.3(4) yes C25 . C29 . H29 . 122.0 no C17 . C29 . H29 . 118.8 no C14 . C30 . C25 . 121.6(4) yes C14 . C30 . H30 . 119.6 no C25 . C30 . H30 . 118.9 no C43 . C31 . H311 . 107.9 no C43 . C31 . H312 . 108.3 no H311 . C31 . H312 . 110.1 no C43 . C31 . H313 . 110.2 no H311 . C31 . H313 . 110.2 no H312 . C31 . H313 . 110.2 no C37 . C32 . C58 . 123.1(4) yes C37 . C32 . H32 . 118.0 no C58 . C32 . H32 . 118.9 no C26 . C34 . H341 . 110.2 no C26 . C34 . H342 . 110.9 no H341 . C34 . H342 . 109.0 no C26 . C34 . H343 . 111.4 no H341 . C34 . H343 . 107.7 no H342 . C34 . H343 . 107.6 no C24 . C37 . C32 . 119.6(3) yes C24 . C37 . C39 . 122.7(3) yes C32 . C37 . C39 . 117.7(3) yes C37 . C39 . O2 . 123.4(3) yes C37 . C39 . C42 . 118.6(4) yes O2 . C39 . C42 . 118.0(4) yes C42 . C40 . C58 . 120.6(4) yes C42 . C40 . H40 . 119.5 no C58 . C40 . H40 . 119.9 no C39 . C42 . C40 . 121.5(4) yes C39 . C42 . H42 . 119.1 no C40 . C42 . H42 . 119.5 no C31 . C43 . C16 . 112.2(3) yes C31 . C43 . H431 . 110.1 no C16 . C43 . H431 . 108.5 no C31 . C43 . H432 . 109.5 no C16 . C43 . H432 . 108.3 no H431 . C43 . H432 . 108.1 no C40 . C58 . C32 . 118.6(4) yes C40 . C58 . H58 . 121.5 no C32 . C58 . H58 . 120.0 no O9 . C101 . C102 . 117.1(15) yes O9 . C101 . H1011 . 107.9 no C102 . C101 . H1011 . 108.4 no O9 . C101 . H1012 . 107.5 no C102 . C101 . H1012 . 106.2 no H1011 . C101 . H1012 . 109.6 no C101 . C102 . H1021 . 109.2 no C101 . C102 . H1022 . 110.3 no H1021 . C102 . H1022 . 109.0 no C101 . C102 . H1023 . 110.9 no H1021 . C102 . H1023 . 108.5 no H1022 . C102 . H1023 . 108.9 no O9 . C201 . C202 . 113.4(5) yes O9 . C201 . H2011 . 109.4 no C202 . C201 . H2011 . 108.9 no O9 . C201 . H2012 . 108.7 no C202 . C201 . H2012 . 108.1 no H2011 . C201 . H2012 . 108.3 no C201 . C202 . H2021 . 110.5 no C201 . C202 . H2022 . 111.0 no H2021 . C202 . H2022 . 109.3 no C201 . C202 . H2023 . 109.7 no H2021 . C202 . H2023 . 107.6 no H2022 . C202 . H2023 . 108.7 no _chemical_name_common (Mn6O2(Et-sao)6(EtOH)6(Br)2) # Attachment '2.cif' data_EB8002 _database_code_depnum_ccdc_archive 'CCDC 693562' _cell_length_a 13.6890(3) _cell_length_b 23.0212(4) _cell_length_c 11.0797(2) _cell_angle_alpha 90 _cell_angle_beta 90.6750(10) _cell_angle_gamma 90 _cell_volume 3491.38(12) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C60 H78 I2 Mn6 N6 O20 # Dc = 1.70 Fooo = 1792.00 Mu = 20.10 M = 893.34 # Found Formula = C60 H78 I2 Mn6 N6 O20 # Dc = 1.70 FOOO = 1792.00 Mu = 20.10 M = 893.34 _chemical_formula_sum 'C60 H78 I2 Mn6 N6 O20' _chemical_formula_moiety 'C60 H78 I2 Mn6 N6 O20' _chemical_compound_source ? _chemical_formula_weight 1786.68 _cell_measurement_reflns_used 9270 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.29 _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 2.010 # Sheldrick geometric approximatio 0.61 0.79 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.79 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _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 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 54126 _reflns_number_total 9960 _diffrn_reflns_av_R_equivalents 0.043 # Number of reflections with Friedels Law is 9960 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10652 _diffrn_reflns_theta_min 1.769 _diffrn_reflns_theta_max 30.501 _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 28.366 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 31 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 1.69 _oxford_diffrn_Wilson_scale 476.38 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.92 _refine_diff_density_max 1.45 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 9960 _refine_ls_number_restraints 0 _refine_ls_number_parameters 424 _oxford_refine_ls_R_factor_ref 0.0478 _refine_ls_wR_factor_ref 0.0809 _refine_ls_goodness_of_fit_ref 0.8579 _refine_ls_shift/su_max 0.003142 # The values computed from all data _oxford_reflns_number_all 9960 _refine_ls_R_factor_all 0.0478 _refine_ls_wR_factor_all 0.0809 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7203 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_gt 0.0754 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Mn1 Mn 0.69772(3) 0.613524(17) -0.08241(4) 0.0171 1.0000 Uani . . . . . . . Mn2 Mn 0.50505(3) 0.565032(17) 0.05410(4) 0.0149 1.0000 Uani . . . . . . . Mn3 Mn 0.71585(3) 0.502320(18) 0.09712(4) 0.0168 1.0000 Uani . . . . . . . O4 O 0.64017(12) 0.56298(8) 0.02993(16) 0.0164 1.0000 Uani . . . . . . . O5 O 0.36629(12) 0.56241(8) 0.05590(16) 0.0172 1.0000 Uani . . . . . . . C6 C 0.31665(18) 0.61224(11) 0.0752(2) 0.0176 1.0000 Uani . . . . . . . C7 C 0.2369(2) 0.61112(13) 0.1511(2) 0.0226 1.0000 Uani . . . . . . . C8 C 0.1857(2) 0.66126(14) 0.1756(3) 0.0283 1.0000 Uani . . . . . . . C9 C 0.2107(2) 0.71353(14) 0.1235(3) 0.0288 1.0000 Uani . . . . . . . C10 C 0.2882(2) 0.71461(13) 0.0440(3) 0.0257 1.0000 Uani . . . . . . . C11 C 0.34166(18) 0.66482(12) 0.0181(2) 0.0186 1.0000 Uani . . . . . . . C12 C 0.42286(19) 0.66889(12) -0.0674(3) 0.0208 1.0000 Uani . . . . . . . N13 N 0.49713(15) 0.63444(9) -0.05432(19) 0.0172 1.0000 Uani . . . . . . . O14 O 0.57131(13) 0.64071(8) -0.13553(16) 0.0187 1.0000 Uani . . . . . . . C15 C 0.4204(2) 0.71260(14) -0.1675(3) 0.0318 1.0000 Uani . . . . . . . O16 O 0.76036(13) 0.66152(9) -0.19180(18) 0.0241 1.0000 Uani . . . . . . . C17 C 0.84612(18) 0.68784(12) -0.1741(3) 0.0208 1.0000 Uani . . . . . . . C18 C 0.8633(2) 0.73943(14) -0.2375(3) 0.0348 1.0000 Uani . . . . . . . C19 C 0.9507(2) 0.76826(15) -0.2253(3) 0.0368 1.0000 Uani . . . . . . . C20 C 1.0238(2) 0.74733(14) -0.1493(3) 0.0324 1.0000 Uani . . . . . . . C21 C 1.0085(2) 0.69681(13) -0.0880(3) 0.0253 1.0000 Uani . . . . . . . C22 C 0.92126(19) 0.66525(12) -0.0979(2) 0.0195 1.0000 Uani . . . . . . . C23 C 0.91330(19) 0.60912(12) -0.0377(3) 0.0205 1.0000 Uani . . . . . . . N24 N 0.82850(16) 0.58423(10) -0.0277(2) 0.0190 1.0000 Uani . . . . . . . O25 O 0.82920(13) 0.52842(8) 0.01751(18) 0.0232 1.0000 Uani . . . . . . . C26 C 1.0033(2) 0.57888(14) 0.0080(3) 0.0364 1.0000 Uani . . . . . . . O27 O 0.78347(13) 0.43902(8) 0.15839(18) 0.0229 1.0000 Uani . . . . . . . C28 C 0.7749(2) 0.41903(12) 0.2703(3) 0.0212 1.0000 Uani . . . . . . . C29 C 0.8570(2) 0.39061(13) 0.3210(3) 0.0268 1.0000 Uani . . . . . . . C30 C 0.8546(2) 0.36866(14) 0.4361(3) 0.0325 1.0000 Uani . . . . . . . C31 C 0.7709(2) 0.37313(14) 0.5037(3) 0.0334 1.0000 Uani . . . . . . . C32 C 0.6893(2) 0.40021(13) 0.4556(3) 0.0271 1.0000 Uani . . . . . . . C33 C 0.6886(2) 0.42355(12) 0.3386(2) 0.0198 1.0000 Uani . . . . . . . C34 C 0.5977(2) 0.44821(12) 0.2897(2) 0.0196 1.0000 Uani . . . . . . . N35 N 0.59991(15) 0.47541(9) 0.18640(19) 0.0155 1.0000 Uani . . . . . . . O36 O 0.51021(12) 0.48950(8) 0.13215(16) 0.0148 1.0000 Uani . . . . . . . C37 C 0.5032(2) 0.44285(14) 0.3546(3) 0.0284 1.0000 Uani . . . . . . . O38 O 0.69587(15) 0.68742(9) 0.05811(19) 0.0274 1.0000 Uani . . . . . . . C39 C 0.6749(3) 0.74606(14) 0.0106(3) 0.0361 1.0000 Uani . . . . . . . C40 C 0.6025(3) 0.77685(16) 0.0871(3) 0.0425 1.0000 Uani . . . . . . . O41 O 0.70061(14) 0.53799(9) -0.21197(18) 0.0257 1.0000 Uani . . . . . . . C42 C 0.7448(3) 0.53047(17) -0.3282(3) 0.0403 1.0000 Uani . . . . . . . C43 C 0.8527(3) 0.5341(2) -0.3196(4) 0.0563 1.0000 Uani . . . . . . . O44 O 0.74629(15) 0.55611(9) 0.2663(2) 0.0333 1.0000 Uani . . . . . . . C45 C 0.8271(3) 0.59042(19) 0.2984(4) 0.0579 1.0000 Uani . . . . . . . C46 C 0.9136(3) 0.5528(2) 0.3222(4) 0.0607 1.0000 Uani . . . . . . . I1 I 0.524592(14) 0.627479(8) 0.282315(17) 0.0254 1.0000 Uani . . . . . . . H71 H 0.2190 0.5767 0.1847 0.0273 1.0000 Uiso R . . . . . . H81 H 0.1329 0.6590 0.2274 0.0338 1.0000 Uiso R . . . . . . H91 H 0.1780 0.7465 0.1403 0.0338 1.0000 Uiso R . . . . . . H101 H 0.3051 0.7492 0.0069 0.0302 1.0000 Uiso R . . . . . . H151 H 0.4450 0.6957 -0.2370 0.0487 1.0000 Uiso R . . . . . . H152 H 0.4588 0.7450 -0.1446 0.0484 1.0000 Uiso R . . . . . . H153 H 0.3560 0.7254 -0.1827 0.0483 1.0000 Uiso R . . . . . . H181 H 0.8157 0.7535 -0.2886 0.0414 1.0000 Uiso R . . . . . . H191 H 0.9596 0.8016 -0.2673 0.0438 1.0000 Uiso R . . . . . . H201 H 1.0839 0.7668 -0.1387 0.0389 1.0000 Uiso R . . . . . . H211 H 1.0577 0.6829 -0.0374 0.0302 1.0000 Uiso R . . . . . . H263 H 0.9859 0.5450 0.0512 0.0553 1.0000 Uiso R . . . . . . H262 H 1.0364 0.6035 0.0603 0.0557 1.0000 Uiso R . . . . . . H261 H 1.0437 0.5686 -0.0543 0.0557 1.0000 Uiso R . . . . . . H291 H 0.9125 0.3869 0.2769 0.0320 1.0000 Uiso R . . . . . . H301 H 0.9102 0.3515 0.4697 0.0389 1.0000 Uiso R . . . . . . H311 H 0.7692 0.3575 0.5805 0.0398 1.0000 Uiso R . . . . . . H321 H 0.6339 0.4020 0.5013 0.0324 1.0000 Uiso R . . . . . . H371 H 0.4700 0.4791 0.3546 0.0438 1.0000 Uiso R . . . . . . H372 H 0.5130 0.4326 0.4376 0.0435 1.0000 Uiso R . . . . . . H373 H 0.4612 0.4153 0.3193 0.0439 1.0000 Uiso R . . . . . . H392 H 0.7333 0.7707 0.0127 0.0428 1.0000 Uiso R . . . . . . H391 H 0.6520 0.7442 -0.0734 0.0426 1.0000 Uiso R . . . . . . H402 H 0.5886 0.8146 0.0502 0.0650 1.0000 Uiso R . . . . . . H401 H 0.6290 0.7816 0.1668 0.0636 1.0000 Uiso R . . . . . . H403 H 0.5431 0.7535 0.0898 0.0643 1.0000 Uiso R . . . . . . H421 H 0.7257 0.5607 -0.3873 0.0474 1.0000 Uiso R . . . . . . H422 H 0.7278 0.4929 -0.3573 0.0484 1.0000 Uiso R . . . . . . H431 H 0.8773 0.5244 -0.4000 0.0848 1.0000 Uiso R . . . . . . H432 H 0.8731 0.5731 -0.2990 0.0847 1.0000 Uiso R . . . . . . H433 H 0.8783 0.5080 -0.2610 0.0849 1.0000 Uiso R . . . . . . H451 H 0.8405 0.6184 0.2330 0.0716 1.0000 Uiso R . . . . . . H452 H 0.8174 0.6112 0.3845 0.0683 1.0000 Uiso R . . . . . . H462 H 0.9696 0.5774 0.3465 0.0915 1.0000 Uiso R . . . . . . H463 H 0.9300 0.5296 0.2493 0.0913 1.0000 Uiso R . . . . . . H461 H 0.8944 0.5269 0.3920 0.0919 1.0000 Uiso R . . . . . . H381 H 0.6605 0.6792 0.1094 0.0402 1.0000 Uiso R . . . . . . H441 H 0.6992 0.5742 0.2797 0.0495 1.0000 Uiso R . . . . . . H411 H 0.6622 0.5134 -0.1975 0.0402 1.0000 Uiso 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 0.01272(18) 0.0181(2) 0.0205(2) 0.00426(15) 0.00063(15) -0.00123(14) Mn2 0.01166(17) 0.01403(19) 0.01890(19) 0.00129(15) 0.00150(14) 0.00077(14) Mn3 0.01312(17) 0.0165(2) 0.0209(2) 0.00477(15) 0.00105(15) 0.00151(14) O4 0.0123(8) 0.0159(9) 0.0209(9) 0.0022(7) 0.0018(7) 0.0002(7) O5 0.0125(8) 0.0170(9) 0.0221(9) -0.0011(7) 0.0020(7) 0.0031(7) C6 0.0137(11) 0.0211(13) 0.0180(12) -0.0015(10) -0.0010(10) 0.0009(9) C7 0.0206(13) 0.0257(15) 0.0217(14) 0.0011(11) 0.0041(11) 0.0059(11) C8 0.0200(14) 0.0374(18) 0.0275(15) -0.0015(13) -0.0004(12) 0.0100(12) C9 0.0246(14) 0.0282(16) 0.0336(17) -0.0093(13) -0.0028(13) 0.0154(12) C10 0.0193(13) 0.0207(14) 0.0369(17) -0.0020(12) -0.0038(12) 0.0052(11) C11 0.0159(12) 0.0200(13) 0.0198(13) 0.0027(10) -0.0006(10) 0.0010(10) C12 0.0153(12) 0.0165(13) 0.0307(15) 0.0013(11) -0.0018(11) 0.0024(10) N13 0.0143(10) 0.0173(11) 0.0200(11) 0.0047(9) 0.0008(8) -0.0033(8) O14 0.0131(8) 0.0214(10) 0.0217(9) 0.0053(7) 0.0029(7) 0.0003(7) C15 0.0263(15) 0.0285(16) 0.0405(19) 0.0089(14) 0.0013(14) 0.0074(13) O16 0.0159(9) 0.0307(11) 0.0258(10) 0.0137(9) -0.0008(8) -0.0053(8) C17 0.0133(12) 0.0237(14) 0.0254(14) 0.0007(11) 0.0050(10) 0.0007(10) C18 0.0295(16) 0.0329(18) 0.0421(19) 0.0155(15) -0.0012(14) -0.0021(13) C19 0.0276(16) 0.0304(18) 0.052(2) 0.0163(16) 0.0036(15) -0.0071(13) C20 0.0228(15) 0.0327(18) 0.0419(19) 0.0033(14) 0.0027(13) -0.0113(13) C21 0.0188(13) 0.0309(16) 0.0261(15) 0.0053(12) 0.0006(11) -0.0054(11) C22 0.0155(12) 0.0213(13) 0.0217(13) 0.0022(11) 0.0027(10) -0.0034(10) C23 0.0157(12) 0.0231(14) 0.0227(13) 0.0011(11) 0.0017(10) -0.0006(10) N24 0.0170(11) 0.0185(11) 0.0215(11) 0.0047(9) 0.0029(9) 0.0015(8) O25 0.0130(9) 0.0201(10) 0.0366(12) 0.0089(9) 0.0047(8) 0.0014(7) C26 0.0128(13) 0.0309(17) 0.065(2) 0.0136(16) -0.0008(14) 0.0009(12) O27 0.0191(9) 0.0239(10) 0.0258(10) 0.0071(8) 0.0012(8) 0.0036(8) C28 0.0236(13) 0.0156(13) 0.0244(14) 0.0030(10) -0.0038(11) -0.0026(10) C29 0.0234(14) 0.0262(15) 0.0307(16) 0.0047(12) -0.0030(12) 0.0064(11) C30 0.0353(17) 0.0326(17) 0.0293(16) 0.0005(13) -0.0091(13) 0.0122(14) C31 0.0460(19) 0.0332(17) 0.0209(14) 0.0094(13) -0.0084(13) 0.0032(15) C32 0.0310(16) 0.0305(16) 0.0197(14) -0.0004(12) 0.0001(12) 0.0013(13) C33 0.0230(13) 0.0184(13) 0.0180(13) -0.0027(10) -0.0025(10) 0.0019(10) C34 0.0216(13) 0.0187(13) 0.0183(13) 0.0034(10) -0.0002(10) -0.0044(10) N35 0.0145(10) 0.0153(10) 0.0167(10) 0.0001(8) -0.0005(8) -0.0013(8) O36 0.0106(8) 0.0143(9) 0.0195(9) 0.0012(7) -0.0002(7) -0.0005(6) C37 0.0239(15) 0.0380(18) 0.0233(15) 0.0081(13) -0.0005(12) -0.0034(13) O38 0.0297(11) 0.0210(10) 0.0314(11) 0.0019(9) 0.0003(9) -0.0018(9) C39 0.0423(19) 0.0286(17) 0.0376(19) -0.0021(14) 0.0006(15) 0.0017(14) C40 0.057(2) 0.037(2) 0.0333(19) -0.0051(15) -0.0010(17) 0.0097(17) O41 0.0218(10) 0.0268(11) 0.0287(11) -0.0048(9) 0.0055(8) -0.0040(8) C42 0.0385(19) 0.053(2) 0.0292(17) -0.0048(16) 0.0095(15) -0.0029(17) C43 0.042(2) 0.075(3) 0.053(3) -0.014(2) 0.0168(19) -0.006(2) O44 0.0237(11) 0.0323(12) 0.0437(14) -0.0115(10) -0.0077(10) 0.0033(9) C45 0.041(2) 0.055(3) 0.078(3) -0.021(2) -0.014(2) -0.0030(19) C46 0.048(2) 0.074(3) 0.060(3) 0.000(2) -0.016(2) -0.002(2) I1 0.02848(10) 0.02528(10) 0.02249(9) -0.00582(8) 0.00157(7) 0.00284(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.066818(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mn1 . Mn2 . 3.2534(5) yes Mn1 . Mn3 . 3.2497(6) yes Mn1 . O4 . 1.8833(18) yes Mn1 . O14 . 1.9258(18) yes Mn1 . O16 . 1.8573(19) yes Mn1 . N24 . 2.000(2) yes Mn1 . O38 . 2.307(2) yes Mn1 . O41 . 2.255(2) yes Mn2 . O36 2_665 2.4224(18) yes Mn2 . Mn2 2_665 3.2277(8) yes Mn2 . Mn3 . 3.2567(5) yes Mn2 . O4 . 1.8727(17) yes Mn2 . O5 . 1.9008(17) yes Mn2 . N13 . 2.001(2) yes Mn2 . O36 . 1.9430(18) yes Mn2 . I1 . 2.9182(4) yes Mn3 . O5 2_665 2.5129(18) yes Mn3 . O4 . 1.8867(18) yes Mn3 . O25 . 1.8918(18) yes Mn3 . O27 . 1.8510(19) yes Mn3 . N35 . 1.979(2) yes Mn3 . O44 . 2.281(2) yes O5 . C6 . 1.352(3) yes C6 . C7 . 1.386(4) yes C6 . C11 . 1.410(4) yes C7 . C8 . 1.379(4) yes C7 . H71 . 0.910 no C8 . C9 . 1.380(4) yes C8 . H81 . 0.930 no C9 . C10 . 1.387(4) yes C9 . H91 . 0.902 no C10 . C11 . 1.392(4) yes C10 . H101 . 0.927 no C11 . C12 . 1.472(4) yes C12 . N13 . 1.296(3) yes C12 . C15 . 1.498(4) yes N13 . O14 . 1.372(3) yes C15 . H151 . 0.929 no C15 . H152 . 0.946 no C15 . H153 . 0.943 no O16 . C17 . 1.334(3) yes C17 . C18 . 1.402(4) yes C17 . C22 . 1.421(4) yes C18 . C19 . 1.373(4) yes C18 . H181 . 0.917 no C19 . C20 . 1.387(4) yes C19 . H191 . 0.907 no C20 . C21 . 1.365(4) yes C20 . H201 . 0.944 no C21 . C22 . 1.401(4) yes C21 . H211 . 0.929 no C22 . C23 . 1.459(4) yes C23 . N24 . 1.300(3) yes C23 . C26 . 1.498(4) yes N24 . O25 . 1.379(3) yes C26 . H263 . 0.947 no C26 . H262 . 0.926 no C26 . H261 . 0.921 no O27 . C28 . 1.329(3) yes C28 . C29 . 1.412(4) yes C28 . C33 . 1.414(4) yes C29 . C30 . 1.373(4) yes C29 . H291 . 0.913 no C30 . C31 . 1.380(5) yes C30 . H301 . 0.931 no C31 . C32 . 1.380(4) yes C31 . H311 . 0.925 no C32 . C33 . 1.404(4) yes C32 . H321 . 0.918 no C33 . C34 . 1.465(4) yes C34 . N35 . 1.305(3) yes C34 . C37 . 1.493(4) yes N35 . O36 . 1.399(3) yes C37 . H371 . 0.950 no C37 . H372 . 0.958 no C37 . H373 . 0.938 no O38 . C39 . 1.475(4) yes O38 . H381 . 0.774 no C39 . C40 . 1.491(4) yes C39 . H392 . 0.980 no C39 . H391 . 0.980 no C40 . H402 . 0.977 no C40 . H401 . 0.957 no C40 . H403 . 0.975 no O41 . C42 . 1.440(4) yes O41 . H411 . 0.790 no C42 . C43 . 1.481(5) yes C42 . H421 . 0.988 no C42 . H422 . 0.952 no C43 . H431 . 0.982 no C43 . H432 . 0.966 no C43 . H433 . 0.948 no O44 . C45 . 1.401(4) yes O44 . H441 . 0.784 no C45 . C46 . 1.489(5) yes C45 . H451 . 0.989 no C45 . H452 . 1.077 no C46 . H462 . 0.988 no C46 . H463 . 0.996 no C46 . H461 . 1.013 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Mn2 . Mn1 . Mn3 . 60.106(12) yes Mn2 . Mn1 . O4 . 29.89(5) yes Mn3 . Mn1 . O4 . 30.49(5) yes Mn2 . Mn1 . O14 . 61.52(5) yes Mn3 . Mn1 . O14 . 120.33(6) yes O4 . Mn1 . O14 . 91.23(7) yes Mn2 . Mn1 . O16 . 152.94(6) yes Mn3 . Mn1 . O16 . 146.68(6) yes O4 . Mn1 . O16 . 177.15(8) yes O14 . Mn1 . O16 . 91.57(8) yes Mn2 . Mn1 . N24 . 118.10(6) yes Mn3 . Mn1 . N24 . 59.16(6) yes O4 . Mn1 . N24 . 88.36(8) yes O14 . Mn1 . N24 . 179.26(9) yes O16 . Mn1 . N24 . 88.84(9) yes Mn2 . Mn1 . O38 . 85.63(5) yes Mn3 . Mn1 . O38 . 99.74(5) yes O4 . Mn1 . O38 . 90.09(8) yes O14 . Mn1 . O38 . 87.11(8) yes O16 . Mn1 . O38 . 90.60(9) yes Mn2 . Mn1 . O41 . 92.97(5) yes Mn3 . Mn1 . O41 . 77.32(5) yes O4 . Mn1 . O41 . 87.42(8) yes O14 . Mn1 . O41 . 94.50(8) yes O16 . Mn1 . O41 . 91.82(8) yes N24 . Mn1 . O38 . 93.51(8) yes N24 . Mn1 . O41 . 84.86(8) yes O38 . Mn1 . O41 . 177.06(8) yes O36 2_665 Mn2 . Mn2 2_665 36.86(4) yes O36 2_665 Mn2 . Mn1 . 81.03(4) yes Mn2 2_665 Mn2 . Mn1 . 100.197(18) yes O36 2_665 Mn2 . Mn3 . 87.84(4) yes Mn2 2_665 Mn2 . Mn3 . 71.163(15) yes Mn1 . Mn2 . Mn3 . 59.892(12) yes O36 2_665 Mn2 . O4 . 86.59(7) yes Mn2 2_665 Mn2 . O4 . 87.80(6) yes Mn1 . Mn2 . O4 . 30.08(5) yes Mn3 . Mn2 . O4 . 30.09(5) yes O36 2_665 Mn2 . O5 . 85.20(7) yes Mn2 2_665 Mn2 . O5 . 86.33(6) yes Mn1 . Mn2 . O5 . 146.25(6) yes Mn3 . Mn2 . O5 . 150.25(6) yes O4 . Mn2 . O5 . 171.71(8) yes O36 2_665 Mn2 . N13 . 84.20(8) yes Mn2 2_665 Mn2 . N13 . 121.06(7) yes Mn1 . Mn2 . N13 . 59.03(6) yes Mn3 . Mn2 . N13 . 118.91(6) yes O4 . Mn2 . N13 . 88.91(8) yes O36 2_665 Mn2 . O36 . 85.28(7) yes Mn2 2_665 Mn2 . O36 . 48.41(5) yes Mn1 . Mn2 . O36 . 119.25(5) yes Mn3 . Mn2 . O36 . 60.70(5) yes O4 . Mn2 . O36 . 90.59(7) yes O36 2_665 Mn2 . I1 . 178.29(4) yes Mn2 2_665 Mn2 . I1 . 141.44(2) yes Mn1 . Mn2 . I1 . 99.628(14) yes Mn3 . Mn2 . I1 . 91.120(13) yes O4 . Mn2 . I1 . 93.19(6) yes O5 . Mn2 . N13 . 89.12(8) yes O5 . Mn2 . O36 . 89.89(7) yes N13 . Mn2 . O36 . 169.47(8) yes O5 . Mn2 . I1 . 95.05(6) yes N13 . Mn2 . I1 . 97.50(6) yes O36 . Mn2 . I1 . 93.03(5) yes O5 2_665 Mn3 . Mn1 . 91.36(4) yes O5 2_665 Mn3 . Mn2 . 77.02(4) yes Mn1 . Mn3 . Mn2 . 60.003(12) yes O5 2_665 Mn3 . O4 . 86.18(7) yes Mn1 . Mn3 . O4 . 30.43(5) yes Mn2 . Mn3 . O4 . 29.85(5) yes O5 2_665 Mn3 . O25 . 103.69(8) yes Mn1 . Mn3 . O25 . 61.41(6) yes Mn2 . Mn3 . O25 . 121.41(6) yes O4 . Mn3 . O25 . 91.74(8) yes O5 2_665 Mn3 . O27 . 89.91(8) yes Mn1 . Mn3 . O27 . 151.51(6) yes Mn2 . Mn3 . O27 . 147.25(6) yes O4 . Mn3 . O27 . 175.80(8) yes O25 . Mn3 . O27 . 90.67(8) yes O5 2_665 Mn3 . N35 . 78.26(7) yes Mn1 . Mn3 . N35 . 119.77(6) yes Mn2 . Mn3 . N35 . 59.84(6) yes O4 . Mn3 . N35 . 89.37(8) yes O25 . Mn3 . N35 . 177.81(9) yes O5 2_665 Mn3 . O44 . 162.25(7) yes Mn1 . Mn3 . O44 . 95.01(6) yes Mn2 . Mn3 . O44 . 91.87(5) yes O4 . Mn3 . O44 . 90.95(8) yes O25 . Mn3 . O44 . 93.89(9) yes O27 . Mn3 . N35 . 88.33(9) yes O27 . Mn3 . O44 . 92.31(8) yes N35 . Mn3 . O44 . 84.20(8) yes Mn3 . O4 . Mn1 . 119.08(9) yes Mn3 . O4 . Mn2 . 120.06(9) yes Mn1 . O4 . Mn2 . 120.03(9) yes Mn3 2_665 O5 . Mn2 . 116.81(8) yes Mn3 2_665 O5 . C6 . 112.86(15) yes Mn2 . O5 . C6 . 118.62(16) yes O5 . C6 . C7 . 118.8(2) yes O5 . C6 . C11 . 122.1(2) yes C7 . C6 . C11 . 119.1(2) yes C6 . C7 . C8 . 120.7(3) yes C6 . C7 . H71 . 118.8 no C8 . C7 . H71 . 120.5 no C7 . C8 . C9 . 121.2(3) yes C7 . C8 . H81 . 118.4 no C9 . C8 . H81 . 120.4 no C8 . C9 . C10 . 118.5(3) yes C8 . C9 . H91 . 121.4 no C10 . C9 . H91 . 120.1 no C9 . C10 . C11 . 121.6(3) yes C9 . C10 . H101 . 119.6 no C11 . C10 . H101 . 118.8 no C6 . C11 . C10 . 118.9(2) yes C6 . C11 . C12 . 122.2(2) yes C10 . C11 . C12 . 118.9(3) yes C11 . C12 . N13 . 119.1(2) yes C11 . C12 . C15 . 120.6(2) yes N13 . C12 . C15 . 120.3(2) yes Mn2 . N13 . C12 . 126.34(19) yes Mn2 . N13 . O14 . 116.25(15) yes C12 . N13 . O14 . 116.6(2) yes N13 . O14 . Mn1 . 115.76(14) yes C12 . C15 . H151 . 109.1 no C12 . C15 . H152 . 108.9 no H151 . C15 . H152 . 110.2 no C12 . C15 . H153 . 110.9 no H151 . C15 . H153 . 109.3 no H152 . C15 . H153 . 108.4 no Mn1 . O16 . C17 . 125.91(17) yes O16 . C17 . C18 . 117.6(3) yes O16 . C17 . C22 . 123.4(2) yes C18 . C17 . C22 . 118.9(3) yes C17 . C18 . C19 . 120.7(3) yes C17 . C18 . H181 . 119.2 no C19 . C18 . H181 . 120.1 no C18 . C19 . C20 . 120.9(3) yes C18 . C19 . H191 . 118.7 no C20 . C19 . H191 . 120.3 no C19 . C20 . C21 . 119.0(3) yes C19 . C20 . H201 . 122.2 no C21 . C20 . H201 . 118.9 no C20 . C21 . C22 . 122.6(3) yes C20 . C21 . H211 . 118.7 no C22 . C21 . H211 . 118.7 no C17 . C22 . C21 . 117.8(3) yes C17 . C22 . C23 . 122.6(2) yes C21 . C22 . C23 . 119.5(2) yes C22 . C23 . N24 . 120.0(2) yes C22 . C23 . C26 . 120.1(2) yes N24 . C23 . C26 . 119.8(3) yes Mn1 . N24 . C23 . 128.49(19) yes Mn1 . N24 . O25 . 115.25(15) yes C23 . N24 . O25 . 116.0(2) yes N24 . O25 . Mn3 . 117.60(14) yes C23 . C26 . H263 . 110.1 no C23 . C26 . H262 . 108.8 no H263 . C26 . H262 . 108.3 no C23 . C26 . H261 . 111.3 no H263 . C26 . H261 . 108.9 no H262 . C26 . H261 . 109.4 no Mn3 . O27 . C28 . 124.42(18) yes O27 . C28 . C29 . 116.9(3) yes O27 . C28 . C33 . 123.9(2) yes C29 . C28 . C33 . 119.2(3) yes C28 . C29 . C30 . 120.8(3) yes C28 . C29 . H291 . 119.6 no C30 . C29 . H291 . 119.6 no C29 . C30 . C31 . 120.4(3) yes C29 . C30 . H301 . 119.9 no C31 . C30 . H301 . 119.7 no C30 . C31 . C32 . 119.9(3) yes C30 . C31 . H311 . 120.0 no C32 . C31 . H311 . 120.1 no C31 . C32 . C33 . 121.7(3) yes C31 . C32 . H321 . 118.6 no C33 . C32 . H321 . 119.6 no C28 . C33 . C32 . 118.0(3) yes C28 . C33 . C34 . 122.7(2) yes C32 . C33 . C34 . 119.1(3) yes C33 . C34 . N35 . 118.9(2) yes C33 . C34 . C37 . 121.7(2) yes N35 . C34 . C37 . 119.4(2) yes Mn3 . N35 . C34 . 127.94(18) yes Mn3 . N35 . O36 . 114.69(14) yes C34 . N35 . O36 . 117.3(2) yes N35 . O36 . Mn2 2_665 108.20(13) yes N35 . O36 . Mn2 . 115.20(13) yes Mn2 2_665 O36 . Mn2 . 94.72(7) yes C34 . C37 . H371 . 110.1 no C34 . C37 . H372 . 111.8 no H371 . C37 . H372 . 106.2 no C34 . C37 . H373 . 112.7 no H371 . C37 . H373 . 107.5 no H372 . C37 . H373 . 108.2 no Mn1 . O38 . C39 . 115.96(18) yes Mn1 . O38 . H381 . 109.1 no C39 . O38 . H381 . 111.3 no O38 . C39 . C40 . 111.1(3) yes O38 . C39 . H392 . 111.5 no C40 . C39 . H392 . 105.0 no O38 . C39 . H391 . 111.0 no C40 . C39 . H391 . 110.6 no H392 . C39 . H391 . 107.4 no C39 . C40 . H402 . 108.2 no C39 . C40 . H401 . 109.3 no H402 . C40 . H401 . 110.7 no C39 . C40 . H403 . 108.5 no H402 . C40 . H403 . 110.2 no H401 . C40 . H403 . 110.0 no Mn1 . O41 . C42 . 132.3(2) yes Mn1 . O41 . H411 . 114.0 no C42 . O41 . H411 . 112.5 no O41 . C42 . C43 . 111.4(3) yes O41 . C42 . H421 . 113.4 no C43 . C42 . H421 . 105.0 no O41 . C42 . H422 . 108.0 no C43 . C42 . H422 . 108.3 no H421 . C42 . H422 . 110.8 no C42 . C43 . H431 . 106.3 no C42 . C43 . H432 . 110.6 no H431 . C43 . H432 . 109.0 no C42 . C43 . H433 . 111.6 no H431 . C43 . H433 . 110.5 no H432 . C43 . H433 . 108.8 no Mn3 . O44 . C45 . 130.6(2) yes Mn3 . O44 . H441 . 107.5 no C45 . O44 . H441 . 107.5 no O44 . C45 . C46 . 109.9(3) yes O44 . C45 . H451 . 109.5 no C46 . C45 . H451 . 110.8 no O44 . C45 . H452 . 111.7 no C46 . C45 . H452 . 102.0 no H451 . C45 . H452 . 112.7 no C45 . C46 . H462 . 109.1 no C45 . C46 . H463 . 110.8 no H462 . C46 . H463 . 110.4 no C45 . C46 . H461 . 105.3 no H462 . C46 . H461 . 109.7 no H463 . C46 . H461 . 111.5 no # Attachment '3.cif' data_EB7211 _database_code_depnum_ccdc_archive 'CCDC 693563' _cell_length_a 10.8003(3) _cell_length_b 12.6691(3) _cell_length_c 14.5319(4) _cell_angle_alpha 109.5870(10) _cell_angle_beta 95.737(2) _cell_angle_gamma 110.0270(10) _cell_volume 1707.47(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C62 H82 Mn6 N6 O22 # Dc = 1.55 Fooo = 822.00 Mu = 11.55 M = 796.46 # Found Formula = C62 H82 Mn6 N6 O22 # Dc = 1.55 FOOO = 822.00 Mu = 11.55 M = 796.46 _chemical_formula_sum 'C62 H82 Mn6 N6 O22' _chemical_formula_moiety 'C60 H74 Mn6 N6 O20, 2(C H4 O)' _chemical_compound_source 'Kevin Mason, KM97' _chemical_formula_weight 1592.93 _cell_measurement_reflns_used 7810 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.52 _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 1.155 # Sheldrick geometric approximatio 0.78 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.89 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _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 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 25005 _reflns_number_total 9590 _diffrn_reflns_av_R_equivalents 0.040 # Number of reflections with Friedels Law is 9590 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10477 _diffrn_reflns_theta_min 2.069 _diffrn_reflns_theta_max 30.563 _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 27.812 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.62 _refine_diff_density_max 0.97 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 9590 _refine_ls_number_restraints 0 _refine_ls_number_parameters 433 _oxford_refine_ls_R_factor_ref 0.0603 _refine_ls_wR_factor_ref 0.1065 _refine_ls_goodness_of_fit_ref 0.9378 _refine_ls_shift/su_max 0.000868 # The values computed from all data _oxford_reflns_number_all 9590 _refine_ls_R_factor_all 0.0603 _refine_ls_wR_factor_all 0.1065 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6938 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_gt 0.0951 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Mn1 Mn 0.13000(4) 0.57282(3) 0.59299(3) 0.0164 1.0000 Uani . . . . . . . Mn2 Mn 0.29810(4) 0.84476(3) 0.64816(3) 0.0155 1.0000 Uani . . . . . . . Mn3 Mn 0.08900(4) 0.67672(3) 0.42628(3) 0.0170 1.0000 Uani . . . . . . . O3 O 0.13958(17) 0.71262(15) 0.56634(12) 0.0166 1.0000 Uani . . . . . . . O5 O 0.06336(16) 0.49000(15) 0.42069(12) 0.0168 1.0000 Uani . . . . . . . O7 O -0.10563(17) 0.58606(16) 0.41037(13) 0.0203 1.0000 Uani . . . . . . . O9 O 0.05949(19) 0.64158(17) 0.28964(13) 0.0252 1.0000 Uani . . . . . . . O15 O 0.06278(18) 0.85346(16) 0.47005(13) 0.0224 1.0000 Uani . . . . . . . O17 O 0.21061(18) 0.95329(15) 0.66245(12) 0.0185 1.0000 Uani . . . . . . . O22 O 0.18409(18) 0.69361(16) 0.74834(13) 0.0218 1.0000 Uani . . . . . . . O29 O 0.35424(17) 0.86164(15) 0.53057(12) 0.0190 1.0000 Uani . . . . . . . O30 O 0.45399(17) 0.97530(15) 0.73286(13) 0.0198 1.0000 Uani . . . . . . . O35 O 0.31579(18) 0.61234(15) 0.59517(14) 0.0222 1.0000 Uani . . . . . . . O42 O 0.2918(4) 0.6048(3) 0.8770(3) 0.0923 1.0000 Uani . . . . . . . N21 N 0.2233(2) 0.81032(19) 0.76004(15) 0.0177 1.0000 Uani . . . . . . . N34 N 0.3971(2) 0.73474(17) 0.64305(15) 0.0180 1.0000 Uani . . . . . . . N42 N 0.2862(2) 0.76617(18) 0.43937(15) 0.0176 1.0000 Uani . . . . . . . C6 C 0.1274(3) 0.4163(2) 0.3680(2) 0.0237 1.0000 Uani . . . . . . . C10 C 0.1391(3) 0.6073(2) 0.23339(19) 0.0241 1.0000 Uani . . . . . . . C11 C 0.0787(3) 0.5199(2) 0.1339(2) 0.0307 1.0000 Uani . . . . . . . C12 C 0.1571(3) 0.4858(3) 0.0707(2) 0.0348 1.0000 Uani . . . . . . . C13 C 0.2977(3) 0.5371(3) 0.1034(2) 0.0346 1.0000 Uani . . . . . . . C14 C 0.3599(3) 0.6218(2) 0.1999(2) 0.0260 1.0000 Uani . . . . . . . C16 C 0.1003(3) 0.9233(3) 0.4101(2) 0.0313 1.0000 Uani . . . . . . . C18 C 0.2272(2) 1.0384(2) 0.75294(18) 0.0181 1.0000 Uani . . . . . . . C19 C 0.2311(3) 1.0129(2) 0.84121(19) 0.0222 1.0000 Uani . . . . . . . C20 C 0.2075(3) 0.8902(2) 0.83655(18) 0.0205 1.0000 Uani . . . . . . . C23 C 0.1502(3) 0.8507(3) 0.9164(2) 0.0270 1.0000 Uani . . . . . . . C24 C 0.0041(3) 0.8373(3) 0.9101(2) 0.0327 1.0000 Uani . . . . . . . C25 C 0.2456(3) 1.1064(3) 0.9315(2) 0.0270 1.0000 Uani . . . . . . . C26 C 0.2555(3) 1.2206(2) 0.9373(2) 0.0307 1.0000 Uani . . . . . . . C27 C 0.2493(3) 1.2427(2) 0.8504(2) 0.0284 1.0000 Uani . . . . . . . C28 C 0.2340(3) 1.1522(2) 0.7589(2) 0.0235 1.0000 Uani . . . . . . . C31 C 0.5816(2) 0.9876(2) 0.75397(18) 0.0187 1.0000 Uani . . . . . . . C32 C 0.6221(2) 0.8888(2) 0.72540(17) 0.0180 1.0000 Uani . . . . . . . C33 C 0.5263(2) 0.7613(2) 0.67141(18) 0.0189 1.0000 Uani . . . . . . . C36 C 0.5747(3) 0.6597(2) 0.6507(2) 0.0253 1.0000 Uani . . . . . . . C37 C 0.5897(3) 0.6256(3) 0.7402(3) 0.0360 1.0000 Uani . . . . . . . C38 C 0.7628(3) 0.9161(2) 0.7523(2) 0.0246 1.0000 Uani . . . . . . . C39 C 0.8582(3) 1.0341(3) 0.8059(2) 0.0270 1.0000 Uani . . . . . . . C40 C 0.8155(3) 1.1300(2) 0.8346(2) 0.0269 1.0000 Uani . . . . . . . C41 C 0.6801(3) 1.1069(2) 0.80974(18) 0.0224 1.0000 Uani . . . . . . . C43 C 0.4011(5) 0.7098(5) 0.9429(4) 0.0826 1.0000 Uani . . . . . . . C45 C 0.5014(3) 0.8344(2) 0.39289(18) 0.0227 1.0000 Uani . . . . . . . C49 C -0.2056(3) 0.6184(3) 0.3721(3) 0.0553 1.0000 Uani . . . . . . . C50 C 0.2832(3) 0.6594(2) 0.26771(18) 0.0195 1.0000 Uani . . . . . . . C52 C 0.5860(3) 0.7809(3) 0.4380(2) 0.0361 1.0000 Uani . . . . . . . C53 C 0.3529(3) 0.7546(2) 0.36875(18) 0.0189 1.0000 Uani . . . . . . . H61 H 0.0972 0.3393 0.3729 0.0381 1.0000 Uiso R . . . . . . H62 H 0.2236 0.4549 0.3948 0.0385 1.0000 Uiso R . . . . . . H63 H 0.1115 0.4044 0.2996 0.0368 1.0000 Uiso R . . . . . . H111 H -0.0152 0.4844 0.1110 0.0340 1.0000 Uiso R . . . . . . H121 H 0.1154 0.4287 0.0051 0.0428 1.0000 Uiso R . . . . . . H131 H 0.3509 0.5162 0.0608 0.0434 1.0000 Uiso R . . . . . . H141 H 0.4530 0.6553 0.2224 0.0304 1.0000 Uiso R . . . . . . H151 H 0.1007 0.8940 0.5305 0.0360 1.0000 Uiso R . . . . . . H161 H 0.0527 0.8723 0.3416 0.0498 1.0000 Uiso R . . . . . . H162 H 0.1963 0.9514 0.4158 0.0498 1.0000 Uiso R . . . . . . H163 H 0.0755 0.9920 0.4319 0.0498 1.0000 Uiso R . . . . . . H231 H 0.2057 0.9098 0.9813 0.0360 1.0000 Uiso R . . . . . . H232 H 0.1560 0.7742 0.9090 0.0359 1.0000 Uiso R . . . . . . H241 H -0.0283 0.8124 0.9607 0.0484 1.0000 Uiso R . . . . . . H242 H -0.0061 0.9120 0.9183 0.0485 1.0000 Uiso R . . . . . . H243 H -0.0561 0.7778 0.8475 0.0473 1.0000 Uiso R . . . . . . H251 H 0.2519 1.0933 0.9909 0.0330 1.0000 Uiso R . . . . . . H261 H 0.2702 1.2828 0.9996 0.0338 1.0000 Uiso R . . . . . . H271 H 0.2557 1.3183 0.8527 0.0327 1.0000 Uiso R . . . . . . H281 H 0.2293 1.1665 0.7007 0.0297 1.0000 Uiso R . . . . . . H361 H 0.5110 0.5906 0.5940 0.0303 1.0000 Uiso R . . . . . . H362 H 0.6631 0.6861 0.6346 0.0316 1.0000 Uiso R . . . . . . H371 H 0.6531 0.6943 0.7980 0.0622 1.0000 Uiso R . . . . . . H372 H 0.5027 0.5989 0.7554 0.0620 1.0000 Uiso R . . . . . . H373 H 0.6223 0.5620 0.7266 0.0628 1.0000 Uiso R . . . . . . H381 H 0.7926 0.8533 0.7349 0.0291 1.0000 Uiso R . . . . . . H391 H 0.9488 1.0480 0.8231 0.0315 1.0000 Uiso R . . . . . . H401 H 0.8767 1.2081 0.8688 0.0257 1.0000 Uiso R . . . . . . H411 H 0.6499 1.1691 0.8293 0.0259 1.0000 Uiso R . . . . . . H421 H 0.2678 0.6303 0.8348 0.1469 1.0000 Uiso R . . . . . . H431 H 0.3716 0.7549 0.9969 0.1310 1.0000 Uiso R . . . . . . H432 H 0.4682 0.6890 0.9722 0.1315 1.0000 Uiso R . . . . . . H433 H 0.4391 0.7592 0.9062 0.1306 1.0000 Uiso R . . . . . . H451 H 0.5164 0.9136 0.4415 0.0268 1.0000 Uiso R . . . . . . H452 H 0.5254 0.8416 0.3320 0.0254 1.0000 Uiso R . . . . . . H491 H -0.2941 0.5558 0.3630 0.0766 1.0000 Uiso R . . . . . . H492 H -0.1937 0.6185 0.3087 0.0744 1.0000 Uiso R . . . . . . H493 H -0.1924 0.6935 0.4231 0.0748 1.0000 Uiso R . . . . . . H521 H 0.5731 0.7016 0.3919 0.0551 1.0000 Uiso R . . . . . . H522 H 0.5599 0.7736 0.4968 0.0547 1.0000 Uiso R . . . . . . H523 H 0.6791 0.8341 0.4560 0.0549 1.0000 Uiso 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 0.01672(18) 0.01563(17) 0.01963(18) 0.00827(14) 0.00591(14) 0.00802(14) Mn2 0.01649(17) 0.01527(17) 0.01655(17) 0.00626(13) 0.00617(13) 0.00782(14) Mn3 0.01777(18) 0.01700(17) 0.01769(17) 0.00819(14) 0.00605(14) 0.00697(14) O3 0.0186(8) 0.0186(8) 0.0162(8) 0.0081(6) 0.0051(6) 0.0103(7) O5 0.0167(8) 0.0162(8) 0.0204(8) 0.0064(6) 0.0092(7) 0.0094(7) O7 0.0198(9) 0.0211(8) 0.0272(9) 0.0136(7) 0.0071(7) 0.0122(7) O9 0.0246(9) 0.0286(10) 0.0196(9) 0.0097(8) 0.0052(7) 0.0074(8) O15 0.0281(10) 0.0250(9) 0.0200(8) 0.0120(7) 0.0095(7) 0.0133(8) O17 0.0241(9) 0.0208(8) 0.0148(8) 0.0059(7) 0.0067(7) 0.0143(7) O22 0.0273(10) 0.0191(8) 0.0197(8) 0.0087(7) 0.0043(7) 0.0095(7) O29 0.0193(8) 0.0160(8) 0.0165(8) 0.0036(6) 0.0057(7) 0.0034(7) O30 0.0201(8) 0.0178(8) 0.0205(8) 0.0064(7) 0.0069(7) 0.0072(7) O35 0.0202(9) 0.0126(8) 0.0326(10) 0.0065(7) 0.0090(7) 0.0071(7) O42 0.084(3) 0.119(3) 0.092(3) 0.072(3) 0.002(2) 0.036(2) N21 0.0194(10) 0.0206(10) 0.0162(9) 0.0089(8) 0.0056(8) 0.0096(8) N34 0.0193(10) 0.0125(9) 0.0202(10) 0.0042(7) 0.0048(8) 0.0063(8) N42 0.0203(10) 0.0161(9) 0.0173(9) 0.0075(8) 0.0076(8) 0.0066(8) C6 0.0252(13) 0.0251(13) 0.0263(13) 0.0094(10) 0.0137(11) 0.0152(11) C10 0.0341(15) 0.0237(12) 0.0184(11) 0.0129(10) 0.0077(11) 0.0114(11) C11 0.0401(16) 0.0236(13) 0.0206(12) 0.0072(11) 0.0024(12) 0.0066(12) C12 0.052(2) 0.0323(15) 0.0204(13) 0.0076(12) 0.0081(13) 0.0201(15) C13 0.054(2) 0.0315(15) 0.0236(13) 0.0085(12) 0.0152(13) 0.0234(15) C14 0.0326(14) 0.0235(13) 0.0244(13) 0.0087(10) 0.0089(11) 0.0143(11) C16 0.0338(15) 0.0276(14) 0.0382(16) 0.0199(13) 0.0084(13) 0.0123(12) C18 0.0177(11) 0.0216(11) 0.0187(11) 0.0071(9) 0.0087(9) 0.0117(9) C19 0.0211(12) 0.0266(13) 0.0216(12) 0.0091(10) 0.0070(10) 0.0127(10) C20 0.0260(13) 0.0265(12) 0.0161(11) 0.0112(10) 0.0096(9) 0.0147(10) C23 0.0336(15) 0.0340(14) 0.0227(12) 0.0167(11) 0.0116(11) 0.0174(12) C24 0.0306(15) 0.0358(16) 0.0300(14) 0.0132(12) 0.0129(12) 0.0094(13) C25 0.0342(15) 0.0291(14) 0.0197(12) 0.0074(10) 0.0128(11) 0.0154(12) C26 0.0359(16) 0.0215(13) 0.0260(14) -0.0006(11) 0.0109(12) 0.0103(12) C27 0.0318(15) 0.0150(11) 0.0348(15) 0.0038(11) 0.0134(12) 0.0096(11) C28 0.0255(13) 0.0256(13) 0.0270(13) 0.0123(11) 0.0152(11) 0.0148(11) C31 0.0190(11) 0.0203(11) 0.0171(11) 0.0088(9) 0.0024(9) 0.0073(9) C32 0.0164(11) 0.0191(11) 0.0176(11) 0.0073(9) 0.0062(9) 0.0055(9) C33 0.0199(12) 0.0192(11) 0.0214(11) 0.0100(9) 0.0097(9) 0.0090(9) C36 0.0180(12) 0.0219(12) 0.0374(15) 0.0100(11) 0.0058(11) 0.0116(10) C37 0.0307(15) 0.0423(17) 0.053(2) 0.0315(16) 0.0159(14) 0.0219(14) C38 0.0164(12) 0.0294(13) 0.0285(13) 0.0115(11) 0.0036(10) 0.0102(10) C39 0.0180(12) 0.0332(15) 0.0260(13) 0.0128(11) 0.0018(10) 0.0058(11) C40 0.0222(13) 0.0205(12) 0.0242(13) 0.0069(10) -0.0055(10) -0.0023(10) C41 0.0243(13) 0.0231(12) 0.0178(11) 0.0090(10) 0.0005(10) 0.0076(10) C43 0.062(3) 0.134(5) 0.060(3) 0.042(3) 0.014(2) 0.045(3) C45 0.0244(13) 0.0204(12) 0.0213(12) 0.0061(9) 0.0165(10) 0.0057(10) C49 0.0191(14) 0.0371(18) 0.115(4) 0.047(2) -0.0055(18) 0.0063(13) C50 0.0276(13) 0.0185(11) 0.0176(11) 0.0098(9) 0.0105(10) 0.0112(10) C52 0.0324(16) 0.0450(18) 0.0332(16) 0.0167(14) 0.0119(13) 0.0158(14) C53 0.0233(12) 0.0170(11) 0.0220(11) 0.0106(9) 0.0104(9) 0.0104(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.13664(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mn1 . Mn3 2_566 3.1336(5) yes Mn1 . O5 2_566 1.9252(17) yes Mn1 . O7 2_566 1.9214(17) yes Mn1 . Mn1 2_566 3.1913(7) yes Mn1 . Mn2 . 3.0630(5) yes Mn1 . Mn3 . 3.1813(5) yes Mn1 . O3 . 1.9079(16) yes Mn1 . O5 . 2.2911(17) yes Mn1 . O22 . 2.1418(18) yes Mn1 . O35 . 1.8886(18) yes Mn2 . Mn3 . 3.2677(5) yes Mn2 . O3 . 1.8555(17) yes Mn2 . O17 . 1.8879(17) yes Mn2 . O29 . 1.9227(17) yes Mn2 . O30 . 1.8435(17) yes Mn2 . N21 . 1.996(2) yes Mn2 . N34 . 2.015(2) yes Mn3 . O3 . 1.9065(16) yes Mn3 . O5 . 2.2577(17) yes Mn3 . O7 . 1.9653(18) yes Mn3 . O9 . 1.8509(18) yes Mn3 . O15 . 2.2392(18) yes Mn3 . N42 . 1.994(2) yes O5 . C6 . 1.416(3) yes O7 . C49 . 1.406(3) yes O9 . C10 . 1.324(3) yes O15 . C16 . 1.432(3) yes O15 . H151 . 0.828 no O17 . C18 . 1.340(3) yes O22 . N21 . 1.335(3) yes O29 . N42 . 1.372(2) yes O30 . C31 . 1.324(3) yes O35 . N34 . 1.372(2) yes O42 . C43 . 1.388(6) yes O42 . H421 . 0.840 no N21 . C20 . 1.300(3) yes N34 . C33 . 1.303(3) yes N42 . C53 . 1.309(3) yes C6 . H61 . 0.946 no C6 . H62 . 0.956 no C6 . H63 . 0.942 no C10 . C11 . 1.409(4) yes C10 . C50 . 1.424(4) yes C11 . C12 . 1.374(4) yes C11 . H111 . 0.928 no C12 . C13 . 1.388(4) yes C12 . H121 . 0.929 no C13 . C14 . 1.371(4) yes C13 . H131 . 0.921 no C14 . C50 . 1.415(3) yes C14 . H141 . 0.920 no C16 . H161 . 0.955 no C16 . H162 . 0.959 no C16 . H163 . 0.959 no C18 . C19 . 1.424(3) yes C18 . C28 . 1.390(3) yes C19 . C20 . 1.463(4) yes C19 . C25 . 1.392(3) yes C20 . C23 . 1.516(3) yes C23 . C24 . 1.518(4) yes C23 . H231 . 0.957 no C23 . H232 . 0.962 no C24 . H241 . 0.945 no C24 . H242 . 0.959 no C24 . H243 . 0.951 no C25 . C26 . 1.386(4) yes C25 . H251 . 0.932 no C26 . C27 . 1.383(4) yes C26 . H261 . 0.934 no C27 . C28 . 1.384(3) yes C27 . H271 . 0.925 no C28 . H281 . 0.922 no C31 . C32 . 1.412(3) yes C31 . C41 . 1.407(3) yes C32 . C33 . 1.462(3) yes C32 . C38 . 1.418(3) yes C33 . C36 . 1.501(3) yes C36 . C37 . 1.513(4) yes C36 . H361 . 0.954 no C36 . H362 . 0.978 no C37 . H371 . 0.959 no C37 . H372 . 0.959 no C37 . H373 . 0.956 no C38 . C39 . 1.381(4) yes C38 . H381 . 0.925 no C39 . C40 . 1.395(4) yes C39 . H391 . 0.924 no C40 . C41 . 1.373(4) yes C40 . H401 . 0.904 no C41 . H411 . 0.924 no C43 . H431 . 0.958 no C43 . H432 . 0.960 no C43 . H433 . 0.968 no C45 . C52 . 1.526(4) yes C45 . C53 . 1.502(3) yes C45 . H451 . 0.961 no C45 . H452 . 0.970 no C49 . H491 . 0.972 no C49 . H492 . 0.943 no C49 . H493 . 0.943 no C50 . C53 . 1.465(3) yes C52 . H521 . 0.955 no C52 . H522 . 0.950 no C52 . H523 . 0.948 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Mn3 2_566 Mn1 . O5 2_566 45.69(5) yes Mn3 2_566 Mn1 . O7 2_566 36.75(5) yes O5 2_566 Mn1 . O7 2_566 82.43(7) yes Mn3 2_566 Mn1 . Mn1 2_566 60.386(13) yes O5 2_566 Mn1 . Mn1 2_566 45.31(5) yes O7 2_566 Mn1 . Mn1 2_566 84.91(5) yes Mn3 2_566 Mn1 . Mn2 . 164.313(16) yes O5 2_566 Mn1 . Mn2 . 121.56(5) yes O7 2_566 Mn1 . Mn2 . 153.40(5) yes Mn1 2_566 Mn1 . Mn2 . 119.600(18) yes Mn3 2_566 Mn1 . Mn3 . 119.295(13) yes O5 2_566 Mn1 . Mn3 . 89.00(5) yes O7 2_566 Mn1 . Mn3 . 134.45(6) yes Mn1 2_566 Mn1 . Mn3 . 58.908(13) yes Mn2 . Mn1 . Mn3 . 63.075(12) yes Mn3 2_566 Mn1 . O3 . 139.14(5) yes O5 2_566 Mn1 . O3 . 94.96(7) yes O7 2_566 Mn1 . O3 . 167.90(7) yes Mn1 2_566 Mn1 . O3 . 84.90(5) yes Mn2 . Mn1 . O3 . 34.96(5) yes Mn3 2_566 Mn1 . O5 . 84.19(4) yes O5 2_566 Mn1 . O5 . 81.99(7) yes O7 2_566 Mn1 . O5 . 89.26(7) yes Mn1 2_566 Mn1 . O5 . 36.68(4) yes Mn2 . Mn1 . O5 . 104.37(4) yes Mn3 2_566 Mn1 . O22 . 106.39(5) yes O5 2_566 Mn1 . O22 . 96.21(7) yes O7 2_566 Mn1 . O22 . 106.85(7) yes Mn1 2_566 Mn1 . O22 . 138.89(5) yes Mn2 . Mn1 . O22 . 62.52(5) yes Mn3 2_566 Mn1 . O35 . 127.66(5) yes O5 2_566 Mn1 . O35 . 172.16(7) yes O7 2_566 Mn1 . O35 . 91.09(7) yes Mn1 2_566 Mn1 . O35 . 129.95(6) yes Mn2 . Mn1 . O35 . 65.74(5) yes Mn3 . Mn1 . O3 . 33.47(5) yes Mn3 . Mn1 . O5 . 45.19(4) yes O3 . Mn1 . O5 . 78.66(6) yes Mn3 . Mn1 . O22 . 118.55(5) yes O3 . Mn1 . O22 . 85.15(7) yes O5 . Mn1 . O22 . 163.47(6) yes Mn3 . Mn1 . O35 . 92.43(6) yes O3 . Mn1 . O35 . 90.46(7) yes O5 . Mn1 . O35 . 93.56(7) yes O22 . Mn1 . O35 . 89.88(7) yes Mn1 . Mn2 . Mn3 . 60.231(11) yes Mn1 . Mn2 . O3 . 36.10(5) yes Mn3 . Mn2 . O3 . 30.15(5) yes Mn1 . Mn2 . O17 . 119.83(6) yes Mn3 . Mn2 . O17 . 87.32(5) yes O3 . Mn2 . O17 . 91.29(7) yes Mn1 . Mn2 . O29 . 107.76(5) yes Mn3 . Mn2 . O29 . 60.29(5) yes O3 . Mn2 . O29 . 89.76(7) yes O17 . Mn2 . O29 . 93.97(7) yes Mn1 . Mn2 . O30 . 142.88(6) yes Mn3 . Mn2 . O30 . 151.59(6) yes O3 . Mn2 . O30 . 178.24(8) yes O17 . Mn2 . O30 . 88.69(8) yes O29 . Mn2 . O30 . 91.99(7) yes Mn1 . Mn2 . N21 . 66.55(6) yes Mn3 . Mn2 . N21 . 113.68(6) yes O3 . Mn2 . N21 . 84.07(8) yes O17 . Mn2 . N21 . 87.08(8) yes O29 . Mn2 . N21 . 173.77(8) yes Mn1 . Mn2 . N34 . 61.69(6) yes Mn3 . Mn2 . N34 . 96.44(6) yes O3 . Mn2 . N34 . 91.47(8) yes O17 . Mn2 . N34 . 176.11(8) yes O29 . Mn2 . N34 . 88.77(8) yes O30 . Mn2 . N21 . 94.17(8) yes O30 . Mn2 . N34 . 88.47(8) yes N21 . Mn2 . N34 . 90.49(8) yes Mn1 2_566 Mn3 . Mn1 . 60.705(13) yes Mn1 2_566 Mn3 . Mn2 . 115.218(14) yes Mn1 . Mn3 . Mn2 . 56.694(11) yes Mn1 2_566 Mn3 . O3 . 86.58(5) yes Mn1 . Mn3 . O3 . 33.50(5) yes Mn2 . Mn3 . O3 . 29.26(5) yes Mn1 2_566 Mn3 . O5 . 37.60(4) yes Mn1 . Mn3 . O5 . 46.06(4) yes Mn2 . Mn3 . O5 . 99.12(4) yes O3 . Mn3 . O5 . 79.55(6) yes Mn1 2_566 Mn3 . O7 . 35.80(5) yes Mn1 . Mn3 . O7 . 84.52(5) yes Mn2 . Mn3 . O7 . 121.76(5) yes O3 . Mn3 . O7 . 95.20(7) yes O5 . Mn3 . O7 . 73.40(6) yes Mn1 2_566 Mn3 . O9 . 96.07(6) yes Mn1 . Mn3 . O9 . 144.46(6) yes Mn2 . Mn3 . O9 . 146.51(6) yes O3 . Mn3 . O9 . 173.37(8) yes O5 . Mn3 . O9 . 98.84(7) yes Mn1 2_566 Mn3 . O15 . 125.28(5) yes Mn1 . Mn3 . O15 . 119.40(5) yes Mn2 . Mn3 . O15 . 76.35(5) yes O3 . Mn3 . O15 . 87.56(7) yes O5 . Mn3 . O15 . 158.59(6) yes Mn1 2_566 Mn3 . N42 . 143.71(6) yes Mn1 . Mn3 . N42 . 95.98(6) yes Mn2 . Mn3 . N42 . 59.41(6) yes O3 . Mn3 . N42 . 85.83(8) yes O5 . Mn3 . N42 . 106.11(7) yes O7 . Mn3 . O9 . 90.46(8) yes O7 . Mn3 . O15 . 91.01(7) yes O9 . Mn3 . O15 . 95.80(8) yes O7 . Mn3 . N42 . 178.73(8) yes O9 . Mn3 . N42 . 88.46(8) yes O15 . Mn3 . N42 . 89.77(7) yes Mn1 . O3 . Mn3 . 113.03(8) yes Mn1 . O3 . Mn2 . 108.95(8) yes Mn3 . O3 . Mn2 . 120.59(9) yes Mn3 . O5 . Mn1 . 88.75(6) yes Mn3 . O5 . Mn1 2_566 96.71(7) yes Mn1 . O5 . Mn1 2_566 98.01(7) yes Mn3 . O5 . C6 . 126.54(14) yes Mn1 . O5 . C6 . 117.16(15) yes Mn1 2_566 O5 . C6 . 121.92(15) yes Mn3 . O7 . Mn1 2_566 107.45(8) yes Mn3 . O7 . C49 . 122.22(17) yes Mn1 2_566 O7 . C49 . 126.53(17) yes Mn3 . O9 . C10 . 123.70(17) yes Mn3 . O15 . C16 . 117.95(16) yes Mn3 . O15 . H151 . 107.5 no C16 . O15 . H151 . 112.4 no Mn2 . O17 . C18 . 120.69(15) yes Mn1 . O22 . N21 . 111.86(13) yes Mn2 . O29 . N42 . 117.62(13) yes Mn2 . O30 . C31 . 131.86(16) yes Mn1 . O35 . N34 . 114.39(13) yes C43 . O42 . H421 . 100.3 no O22 . N21 . Mn2 . 113.77(14) yes O22 . N21 . C20 . 121.2(2) yes Mn2 . N21 . C20 . 124.96(17) yes O35 . N34 . Mn2 . 114.04(14) yes O35 . N34 . C33 . 115.38(19) yes Mn2 . N34 . C33 . 130.38(17) yes O29 . N42 . Mn3 . 114.72(14) yes O29 . N42 . C53 . 116.8(2) yes Mn3 . N42 . C53 . 127.92(17) yes O5 . C6 . H61 . 111.8 no O5 . C6 . H62 . 110.8 no H61 . C6 . H62 . 107.1 no O5 . C6 . H63 . 110.5 no H61 . C6 . H63 . 109.3 no H62 . C6 . H63 . 107.1 no O9 . C10 . C11 . 118.4(3) yes O9 . C10 . C50 . 122.7(2) yes C11 . C10 . C50 . 118.8(3) yes C10 . C11 . C12 . 120.8(3) yes C10 . C11 . H111 . 119.6 no C12 . C11 . H111 . 119.6 no C11 . C12 . C13 . 120.7(3) yes C11 . C12 . H121 . 119.5 no C13 . C12 . H121 . 119.8 no C12 . C13 . C14 . 120.1(3) yes C12 . C13 . H131 . 121.1 no C14 . C13 . H131 . 118.8 no C13 . C14 . C50 . 121.1(3) yes C13 . C14 . H141 . 120.6 no C50 . C14 . H141 . 118.3 no O15 . C16 . H161 . 108.5 no O15 . C16 . H162 . 109.8 no H161 . C16 . H162 . 109.8 no O15 . C16 . H163 . 110.0 no H161 . C16 . H163 . 109.0 no H162 . C16 . H163 . 109.8 no O17 . C18 . C19 . 121.6(2) yes O17 . C18 . C28 . 118.5(2) yes C19 . C18 . C28 . 119.8(2) yes C18 . C19 . C20 . 121.7(2) yes C18 . C19 . C25 . 117.4(2) yes C20 . C19 . C25 . 120.6(2) yes C19 . C20 . N21 . 120.9(2) yes C19 . C20 . C23 . 119.8(2) yes N21 . C20 . C23 . 119.0(2) yes C20 . C23 . C24 . 112.4(2) yes C20 . C23 . H231 . 108.7 no C24 . C23 . H231 . 109.6 no C20 . C23 . H232 . 108.9 no C24 . C23 . H232 . 109.8 no H231 . C23 . H232 . 107.2 no C23 . C24 . H241 . 110.1 no C23 . C24 . H242 . 112.7 no H241 . C24 . H242 . 107.9 no C23 . C24 . H243 . 113.1 no H241 . C24 . H243 . 106.7 no H242 . C24 . H243 . 106.0 no C19 . C25 . C26 . 122.4(3) yes C19 . C25 . H251 . 119.4 no C26 . C25 . H251 . 118.2 no C25 . C26 . C27 . 119.1(2) yes C25 . C26 . H261 . 120.4 no C27 . C26 . H261 . 120.4 no C26 . C27 . C28 . 120.4(3) yes C26 . C27 . H271 . 120.4 no C28 . C27 . H271 . 119.2 no C18 . C28 . C27 . 120.7(2) yes C18 . C28 . H281 . 118.7 no C27 . C28 . H281 . 120.6 no O30 . C31 . C32 . 123.9(2) yes O30 . C31 . C41 . 116.7(2) yes C32 . C31 . C41 . 119.4(2) yes C31 . C32 . C33 . 123.2(2) yes C31 . C32 . C38 . 117.6(2) yes C33 . C32 . C38 . 119.2(2) yes C32 . C33 . N34 . 120.1(2) yes C32 . C33 . C36 . 120.5(2) yes N34 . C33 . C36 . 119.3(2) yes C33 . C36 . C37 . 112.1(2) yes C33 . C36 . H361 . 108.2 no C37 . C36 . H361 . 110.0 no C33 . C36 . H362 . 108.9 no C37 . C36 . H362 . 108.5 no H361 . C36 . H362 . 109.1 no C36 . C37 . H371 . 111.0 no C36 . C37 . H372 . 108.4 no H371 . C37 . H372 . 109.0 no C36 . C37 . H373 . 111.4 no H371 . C37 . H373 . 107.3 no H372 . C37 . H373 . 109.7 no C32 . C38 . C39 . 122.2(2) yes C32 . C38 . H381 . 119.7 no C39 . C38 . H381 . 118.1 no C38 . C39 . C40 . 119.2(2) yes C38 . C39 . H391 . 119.6 no C40 . C39 . H391 . 121.1 no C39 . C40 . C41 . 120.1(2) yes C39 . C40 . H401 . 120.5 no C41 . C40 . H401 . 119.3 no C31 . C41 . C40 . 121.5(2) yes C31 . C41 . H411 . 117.2 no C40 . C41 . H411 . 121.3 no O42 . C43 . H431 . 110.0 no O42 . C43 . H432 . 110.4 no H431 . C43 . H432 . 107.3 no O42 . C43 . H433 . 108.5 no H431 . C43 . H433 . 109.9 no H432 . C43 . H433 . 110.7 no C52 . C45 . C53 . 110.0(2) yes C52 . C45 . H451 . 109.1 no C53 . C45 . H451 . 107.7 no C52 . C45 . H452 . 110.9 no C53 . C45 . H452 . 109.3 no H451 . C45 . H452 . 109.7 no O7 . C49 . H491 . 108.1 no O7 . C49 . H492 . 107.2 no H491 . C49 . H492 . 108.9 no O7 . C49 . H493 . 103.9 no H491 . C49 . H493 . 110.9 no H492 . C49 . H493 . 117.3 no C10 . C50 . C14 . 118.5(2) yes C10 . C50 . C53 . 121.6(2) yes C14 . C50 . C53 . 119.8(2) yes C45 . C52 . H521 . 111.6 no C45 . C52 . H522 . 109.5 no H521 . C52 . H522 . 108.0 no C45 . C52 . H523 . 109.3 no H521 . C52 . H523 . 109.6 no H522 . C52 . H523 . 108.7 no C45 . C53 . C50 . 120.5(2) yes C45 . C53 . N42 . 120.0(2) yes C50 . C53 . N42 . 119.4(2) yes