#------------------------------------------------------------------------------ #$Date: 2014-12-21 17:20:32 +0200 (Sun, 21 Dec 2014) $ #$Revision: 128920 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/12/31/4123114.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4123114 loop_ _publ_author_name 'Hamilton, Clifton R.' 'Gau, Michael R.' 'Baglia, Regina A.' 'McWilliams, Sean F.' 'Zdilla, Michael J.' _publ_section_title ; Mechanistic Elucidation of the Stepwise Formation of a Tetranuclear Manganese Pinned Butterfly Cluster via N-N Bond Cleavage, Hydrogen Atom Transfer, and Cluster Rearrangement. ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 141218154447008 _journal_paper_doi 10.1021/ja508244x _journal_year 2014 _chemical_formula_moiety '[C70 H66 Mn4 N12],[NC5H5],[NC5H5]' _chemical_formula_sum 'C80 H76 Mn4 N14' _chemical_formula_weight 1453.30 _chemical_melting_point ? _chemical_name_common 'Methylmarked Red House' _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens constr _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 92.7590(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.7510(10) _cell_length_b 24.8219(16) _cell_length_c 19.4882(14) _cell_measurement_reflns_used 9773 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 26.98 _cell_measurement_theta_min 2.586 _cell_volume 7127.3(8) _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_collection 'COSMO (Bruker-AXS)' _computing_data_reduction 'SADABS (Bruker-AXS)' _computing_molecular_graphics XP _computing_publication_material 'APEX2 Report Generator (Bruker-AXS)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Kappa APEX II DUO' _diffrn_measurement_method 'Omega Scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_unetI/netI 0.0331 _diffrn_reflns_laue_measured_fraction_full 1.000 _diffrn_reflns_laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 56118 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.129 _diffrn_reflns_theta_min 1.329 _diffrn_source 'fine-focused sealed tube' _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6848 _exptl_absorpt_process_details ; 56898 Corrected reflections written to file mo_497_0m.hkl Estimated minimum and maximum transmission: 0.6848 0.7455 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.2000 Lambda/2 correction factor = 0.0015 ; _exptl_crystal_colour Needle _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Red _exptl_crystal_F_000 3016 _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.240 _refine_diff_density_max 0.990 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.068 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 891 _refine_ls_number_reflns 15592 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0429 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+7.1710P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1071 _refine_ls_wR_factor_ref 0.1204 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11749 _reflns_number_total 15592 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file ja508244x_si_002.cif _[local]_cod_data_source_block 2Tol _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value 'not determined' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius ; _cod_database_code 4123114 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.715 _shelx_estimated_absorpt_t_max 0.841 _shelxl_version_number 2013-3 _shelx_res_file ; TITL solveFINAL in P2(1)/n CELL 0.71073 14.7510 24.8219 19.4882 90.000 92.759 90.000 ZERR 4.00 0.0010 0.0016 0.0014 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N Mn UNIT 320 304 56 16 L.S. 4 BOND FMAP 2 PLAN 20 SIZE 0.240 0.300 0.480 TEMP -100.150 ACTA CONF WGHT 0.055200 7.171000 FVAR 0.07533 MN1 4 0.117494 0.120572 0.862125 11.00000 0.02282 0.02627 = 0.02380 0.00464 -0.00002 -0.00239 MN2 4 0.279016 0.150763 0.784025 11.00000 0.02238 0.03027 = 0.02596 -0.00066 0.00171 -0.00118 MN3 4 0.032669 0.224059 0.781524 11.00000 0.02195 0.02405 = 0.02596 0.00179 -0.00069 -0.00095 MN4 4 0.255408 0.270450 0.845996 11.00000 0.02179 0.02568 = 0.02605 0.00428 -0.00115 -0.00075 N1 3 0.002919 0.170905 0.865287 11.00000 0.02254 0.03190 = 0.02761 0.00032 0.00015 -0.00131 N2 3 0.146514 0.122634 0.753960 11.00000 0.02687 0.02411 = 0.02217 0.00218 -0.00097 -0.00059 N3 3 0.124140 0.177318 0.729741 11.00000 0.03063 0.02200 = 0.02569 0.00238 0.00257 -0.00122 N4 3 0.064177 0.301406 0.810007 11.00000 0.02097 0.02301 = 0.02660 0.00225 0.00176 -0.00150 N5 3 0.330120 0.228997 0.770144 11.00000 0.02156 0.03485 = 0.02793 0.00411 0.00071 -0.00009 N6 3 0.246490 0.152138 0.893753 11.00000 0.02680 0.02243 = 0.02391 0.00091 -0.00310 0.00040 N7 3 0.221264 0.207522 0.909983 11.00000 0.02782 0.02406 = 0.02599 0.00267 -0.00034 0.00045 N8 3 0.157162 0.316551 0.798459 11.00000 0.01957 0.02513 = 0.02797 0.00352 -0.00014 -0.00080 N10 3 0.098648 0.041675 0.908335 11.00000 0.02972 0.02621 = 0.02751 0.00435 0.00574 -0.00075 N20 3 0.382788 0.100143 0.736386 11.00000 0.03576 0.03530 = 0.03265 -0.00067 0.00364 0.00357 N30 3 -0.090298 0.232017 0.712588 11.00000 0.02836 0.03246 = 0.03260 0.00126 -0.00324 0.00003 N40 3 0.359896 0.315189 0.912041 11.00000 0.03249 0.03179 = 0.03380 0.00208 -0.00484 -0.00491 C11 1 -0.084801 0.147763 0.866815 11.00000 0.02476 0.02853 = 0.02770 0.00761 0.00007 0.00129 C12 1 -0.147564 0.164559 0.914025 11.00000 0.03377 0.03613 = 0.03428 0.00308 0.00418 0.00399 AFIX 43 H12A 2 -0.130712 0.191386 0.946989 11.00000 -1.20000 AFIX 0 C13 1 -0.234194 0.142511 0.913312 11.00000 0.03038 0.04440 = 0.05410 0.00863 0.01376 0.00564 AFIX 43 H13A 2 -0.275201 0.154244 0.946341 11.00000 -1.20000 AFIX 0 C14 1 -0.262169 0.103924 0.865724 11.00000 0.02868 0.03728 = 0.07295 0.01273 0.00423 -0.00002 C15 1 -0.199459 0.086131 0.820083 11.00000 0.03475 0.03261 = 0.05203 0.00271 -0.00552 -0.00486 AFIX 43 H15A 2 -0.216433 0.058979 0.787596 11.00000 -1.20000 AFIX 0 C16 1 -0.112241 0.107291 0.820999 11.00000 0.03075 0.03170 = 0.03331 0.00143 0.00118 -0.00026 AFIX 43 H16A 2 -0.070393 0.093828 0.789641 11.00000 -1.20000 AFIX 0 C17 1 -0.358179 0.081310 0.864123 11.00000 0.03218 0.05865 = 0.13325 0.00253 0.01405 -0.01013 AFIX 33 H17A 2 -0.392322 0.098611 0.899985 11.00000 -1.50000 H17B 2 -0.355725 0.042363 0.872246 11.00000 -1.50000 H17C 2 -0.388296 0.088398 0.819107 11.00000 -1.50000 AFIX 0 C21 1 0.102105 0.081077 0.717012 11.00000 0.02518 0.02864 = 0.02599 -0.00114 0.00293 -0.00247 C22 1 0.035772 0.089994 0.664615 11.00000 0.03347 0.03064 = 0.03578 0.00004 -0.00476 -0.00050 AFIX 43 H22A 2 0.022204 0.125791 0.650257 11.00000 -1.20000 AFIX 0 C23 1 -0.010390 0.047368 0.633385 11.00000 0.04653 0.04712 = 0.05286 -0.00629 -0.01579 -0.01042 AFIX 43 H23A 2 -0.055596 0.054289 0.598115 11.00000 -1.20000 AFIX 0 C24 1 0.008305 -0.004876 0.652726 11.00000 0.07217 0.03981 = 0.06813 -0.00980 -0.01694 -0.01965 AFIX 43 H24A 2 -0.024867 -0.033874 0.631942 11.00000 -1.20000 AFIX 0 C25 1 0.075912 -0.014761 0.702759 11.00000 0.07574 0.02395 = 0.05639 -0.00426 -0.00358 -0.00350 AFIX 43 H25A 2 0.089934 -0.050825 0.715678 11.00000 -1.20000 AFIX 0 C26 1 0.123409 0.027337 0.734243 11.00000 0.04581 0.03003 = 0.03350 0.00158 -0.00097 0.00226 AFIX 43 H26A 2 0.170707 0.019888 0.767708 11.00000 -1.20000 AFIX 0 C31 1 0.163175 0.191564 0.668526 11.00000 0.02647 0.03011 = 0.02283 0.00088 -0.00243 -0.00501 C32 1 0.218068 0.158142 0.630550 11.00000 0.03244 0.03839 = 0.02633 0.00172 0.00072 -0.00017 AFIX 43 H32A 2 0.226210 0.121513 0.643571 11.00000 -1.20000 AFIX 0 C33 1 0.261048 0.178118 0.573639 11.00000 0.04358 0.05534 = 0.03261 0.00111 0.01100 0.00119 AFIX 43 H33A 2 0.300297 0.155230 0.549654 11.00000 -1.20000 AFIX 0 C34 1 0.247817 0.230091 0.551609 11.00000 0.06976 0.06221 = 0.03097 0.01016 0.01971 -0.01392 AFIX 43 H34A 2 0.276988 0.243211 0.512538 11.00000 -1.20000 AFIX 0 C35 1 0.190753 0.263234 0.587681 11.00000 0.06846 0.03875 = 0.03635 0.01232 0.00144 -0.00925 AFIX 43 H35A 2 0.180622 0.299263 0.572759 11.00000 -1.20000 AFIX 0 C36 1 0.148910 0.244725 0.644417 11.00000 0.04545 0.03127 = 0.02654 0.00133 0.00133 -0.00470 AFIX 43 H36A 2 0.109723 0.268003 0.667879 11.00000 -1.20000 AFIX 0 C41 1 0.019593 0.335335 0.852486 11.00000 0.02442 0.02820 = 0.02121 0.00582 -0.00006 0.00136 C42 1 0.056674 0.382640 0.882145 11.00000 0.03843 0.02856 = 0.03418 0.00184 0.00485 -0.00077 AFIX 43 H42A 2 0.115716 0.393755 0.870759 11.00000 -1.20000 AFIX 0 C43 1 0.009059 0.413304 0.927504 11.00000 0.05772 0.03271 = 0.04056 -0.00347 0.00487 0.00438 AFIX 43 H43A 2 0.036929 0.444374 0.947658 11.00000 -1.20000 AFIX 0 C44 1 -0.077838 0.399867 0.944163 11.00000 0.05068 0.05072 = 0.03830 -0.00098 0.00909 0.01807 AFIX 43 H44A 2 -0.110345 0.421406 0.974911 11.00000 -1.20000 AFIX 0 C45 1 -0.116117 0.354161 0.914783 11.00000 0.03137 0.06172 = 0.03218 0.00574 0.00573 0.00835 AFIX 43 H45A 2 -0.176076 0.344419 0.925538 11.00000 -1.20000 AFIX 0 C46 1 -0.069840 0.322041 0.870096 11.00000 0.02523 0.03914 = 0.02763 0.00359 -0.00052 0.00221 AFIX 43 H46A 2 -0.098317 0.290758 0.851028 11.00000 -1.20000 AFIX 0 C51 1 0.423789 0.239501 0.780687 11.00000 0.02232 0.03052 = 0.03290 -0.00142 0.00339 0.00037 C52 1 0.471734 0.216932 0.837397 11.00000 0.02671 0.03803 = 0.03707 0.00640 0.00157 -0.00324 AFIX 43 H52A 2 0.441069 0.193682 0.867294 11.00000 -1.20000 AFIX 0 C53 1 0.562435 0.227750 0.850718 11.00000 0.02843 0.04885 = 0.04213 0.00799 -0.00227 0.00151 AFIX 43 H53A 2 0.592654 0.212322 0.890137 11.00000 -1.20000 AFIX 0 C54 1 0.610693 0.260567 0.808069 11.00000 0.02756 0.05866 = 0.05000 0.00455 0.00414 -0.00654 C55 1 0.563962 0.282658 0.751748 11.00000 0.03453 0.06146 = 0.04229 0.01031 0.00721 -0.01252 AFIX 43 H55A 2 0.595445 0.305204 0.721507 11.00000 -1.20000 AFIX 0 C56 1 0.472320 0.272807 0.738167 11.00000 0.03262 0.04577 = 0.03287 0.00699 0.00568 -0.00052 AFIX 43 H56A 2 0.442171 0.289028 0.699255 11.00000 -1.20000 AFIX 0 C57 1 0.709737 0.271649 0.823944 11.00000 0.03305 0.09511 = 0.06996 0.01758 -0.00106 -0.01417 AFIX 33 H57A 2 0.729834 0.252281 0.865779 11.00000 -1.50000 H57B 2 0.718854 0.310415 0.830855 11.00000 -1.50000 H57C 2 0.745056 0.259471 0.785543 11.00000 -1.50000 AFIX 0 C61 1 0.319565 0.130364 0.933645 11.00000 0.02587 0.03066 = 0.02541 0.00575 0.00275 -0.00112 C62 1 0.351660 0.079387 0.915633 11.00000 0.03842 0.02995 = 0.03139 0.00140 0.00142 0.00467 AFIX 43 H62A 2 0.320639 0.059646 0.879947 11.00000 -1.20000 AFIX 0 C63 1 0.427394 0.057504 0.948840 11.00000 0.04701 0.04184 = 0.04846 0.00378 0.00500 0.01730 AFIX 43 H63A 2 0.448712 0.023181 0.935282 11.00000 -1.20000 AFIX 0 C64 1 0.472761 0.085003 1.001759 11.00000 0.04231 0.06093 = 0.04332 0.01201 -0.00533 0.01922 AFIX 43 H64A 2 0.525442 0.069950 1.024229 11.00000 -1.20000 AFIX 0 C65 1 0.441166 0.133804 1.021280 11.00000 0.03561 0.05280 = 0.03383 0.00226 -0.00957 0.00060 AFIX 43 H65A 2 0.471904 0.152546 1.057986 11.00000 -1.20000 AFIX 0 C66 1 0.364413 0.156984 0.988485 11.00000 0.03316 0.03648 = 0.02968 -0.00055 -0.00334 0.00117 AFIX 43 H66A 2 0.342763 0.190833 1.003495 11.00000 -1.20000 AFIX 0 C71 1 0.163745 0.213070 0.963047 11.00000 0.02336 0.02895 = 0.02100 0.00037 -0.00544 -0.00187 C72 1 0.123151 0.264233 0.971337 11.00000 0.03202 0.03101 = 0.02360 0.00204 -0.00386 0.00043 AFIX 43 H72A 2 0.143670 0.293701 0.945122 11.00000 -1.20000 AFIX 0 C73 1 0.055021 0.272833 1.016008 11.00000 0.03394 0.04131 = 0.02876 -0.00055 -0.00497 0.00635 AFIX 43 H73A 2 0.027650 0.307375 1.018548 11.00000 -1.20000 AFIX 0 C74 1 0.026198 0.231310 1.057289 11.00000 0.02943 0.05470 = 0.02915 -0.00287 0.00324 -0.00165 AFIX 43 H74A 2 -0.022067 0.236666 1.087126 11.00000 -1.20000 AFIX 0 C75 1 0.069288 0.181868 1.054082 11.00000 0.04073 0.04238 = 0.02690 0.00418 0.00002 -0.01373 AFIX 43 H75A 2 0.051994 0.153747 1.083824 11.00000 -1.20000 AFIX 0 C76 1 0.137361 0.172229 1.008397 11.00000 0.03454 0.02780 = 0.02590 0.00103 -0.00182 -0.00628 AFIX 43 H76A 2 0.166135 0.138004 1.007783 11.00000 -1.20000 AFIX 0 C81 1 0.167661 0.354623 0.748932 11.00000 0.02773 0.02255 = 0.02352 0.00001 0.00083 -0.00355 C82 1 0.257139 0.367045 0.728979 11.00000 0.03110 0.03426 = 0.03692 0.00610 -0.00061 -0.00686 AFIX 43 H82A 2 0.307688 0.350025 0.751934 11.00000 -1.20000 AFIX 0 C83 1 0.271569 0.403314 0.676970 11.00000 0.04093 0.04383 = 0.04194 0.00594 0.01111 -0.01366 AFIX 43 H83A 2 0.331775 0.410021 0.663951 11.00000 -1.20000 AFIX 0 C84 1 0.200174 0.430103 0.643403 11.00000 0.05521 0.03781 = 0.03943 0.01555 0.00867 -0.00832 AFIX 43 H84A 2 0.210608 0.454996 0.607606 11.00000 -1.20000 AFIX 0 C85 1 0.113530 0.419718 0.663274 11.00000 0.05039 0.03910 = 0.03668 0.01506 -0.00083 0.00414 AFIX 43 H85A 2 0.064040 0.438253 0.641000 11.00000 -1.20000 AFIX 0 C86 1 0.096219 0.383073 0.714754 11.00000 0.03297 0.02906 = 0.03039 0.00646 0.00265 -0.00156 AFIX 43 H86A 2 0.035519 0.377090 0.727109 11.00000 -1.20000 AFIX 0 C102 1 0.031710 0.008163 0.887216 11.00000 0.03081 0.03417 = 0.03915 0.00507 -0.00085 -0.00215 AFIX 43 H10A 2 -0.007598 0.018878 0.849634 11.00000 -1.20000 AFIX 0 C103 1 0.017200 -0.041092 0.917426 11.00000 0.03403 0.03102 = 0.04836 0.00119 0.00399 -0.00572 AFIX 43 H10B 2 -0.031725 -0.063402 0.901477 11.00000 -1.20000 AFIX 0 C104 1 0.074585 -0.057350 0.970897 11.00000 0.04682 0.02911 = 0.04090 0.00850 0.01252 0.00095 AFIX 43 H10C 2 0.066839 -0.091480 0.991881 11.00000 -1.20000 AFIX 0 C105 1 0.143391 -0.023619 0.993690 11.00000 0.04583 0.03719 = 0.03344 0.00832 0.00121 0.00360 AFIX 43 H10D 2 0.183690 -0.033986 1.030846 11.00000 -1.20000 AFIX 0 C106 1 0.153136 0.025357 0.961984 11.00000 0.03468 0.03153 = 0.03020 0.00031 0.00239 -0.00240 AFIX 43 H10E 2 0.200256 0.048739 0.978540 11.00000 -1.20000 AFIX 0 C202 1 0.385169 0.046858 0.737501 11.00000 0.05781 0.03871 = 0.05065 -0.00118 0.01793 0.00017 AFIX 43 H20A 2 0.343790 0.028507 0.765170 11.00000 -1.20000 AFIX 0 C203 1 0.444003 0.016572 0.700968 11.00000 0.08619 0.03784 = 0.07016 -0.00485 0.02701 0.01161 AFIX 43 H20B 2 0.442905 -0.021639 0.703557 11.00000 -1.20000 AFIX 0 C204 1 0.503961 0.042003 0.660969 11.00000 0.06512 0.05469 = 0.07515 -0.01402 0.02939 0.01693 AFIX 43 H20C 2 0.545321 0.021805 0.635333 11.00000 -1.20000 AFIX 0 C205 1 0.503723 0.097444 0.658250 11.00000 0.06221 0.05606 = 0.06889 -0.00579 0.03560 -0.00282 AFIX 43 H20D 2 0.544696 0.116313 0.630775 11.00000 -1.20000 AFIX 0 C206 1 0.442257 0.124859 0.696578 11.00000 0.04929 0.03913 = 0.05358 -0.00336 0.02016 -0.00052 AFIX 43 H20E 2 0.441924 0.163104 0.694759 11.00000 -1.20000 AFIX 0 C302 1 -0.118316 0.281010 0.692927 11.00000 0.04009 0.03323 = 0.04219 0.00184 -0.00601 -0.00140 AFIX 43 H30A 2 -0.082297 0.311307 0.706308 11.00000 -1.20000 AFIX 0 C303 1 -0.197572 0.289314 0.653924 11.00000 0.04844 0.04025 = 0.04789 0.00531 -0.01190 0.00842 AFIX 43 H30B 2 -0.215129 0.324684 0.640225 11.00000 -1.20000 AFIX 0 C304 1 -0.250973 0.245791 0.635057 11.00000 0.03532 0.05884 = 0.04396 0.00016 -0.01234 0.00611 AFIX 43 H30C 2 -0.306487 0.250740 0.609056 11.00000 -1.20000 AFIX 0 C305 1 -0.222883 0.195534 0.654288 11.00000 0.04095 0.04898 = 0.05138 -0.00075 -0.01261 -0.00951 AFIX 43 H30D 2 -0.258394 0.164815 0.641832 11.00000 -1.20000 AFIX 0 C306 1 -0.142019 0.189963 0.692153 11.00000 0.03938 0.03424 = 0.04793 0.00373 -0.00784 -0.00141 AFIX 43 H30E 2 -0.121992 0.154713 0.704341 11.00000 -1.20000 AFIX 0 C402 1 0.368066 0.300545 0.977733 11.00000 0.04393 0.04554 = 0.03828 0.00001 -0.00352 -0.01375 AFIX 43 H40A 2 0.318241 0.282846 0.997110 11.00000 -1.20000 AFIX 0 C403 1 0.445053 0.309676 1.019286 11.00000 0.05908 0.06541 = 0.03997 0.00140 -0.01286 -0.01489 AFIX 43 H40B 2 0.447794 0.297951 1.065744 11.00000 -1.20000 AFIX 0 C404 1 0.516830 0.335579 0.993112 11.00000 0.04919 0.07080 = 0.04846 -0.00131 -0.01215 -0.01749 AFIX 43 H40C 2 0.570570 0.342034 1.020720 11.00000 -1.20000 AFIX 0 C405 1 0.509940 0.352216 0.925852 11.00000 0.04093 0.04851 = 0.06209 0.00278 -0.00290 -0.01688 AFIX 43 H40D 2 0.558371 0.371109 0.906250 11.00000 -1.20000 AFIX 0 C406 1 0.431083 0.340925 0.887186 11.00000 0.04362 0.03909 = 0.04224 0.00419 -0.00448 -0.00939 AFIX 43 H40E 2 0.427225 0.352027 0.840486 11.00000 -1.20000 AFIX 0 N1S 3 0.805229 0.933880 0.850080 11.00000 0.06039 0.06120 = 0.07500 0.01063 -0.01970 -0.01085 C4S 1 0.718292 0.938318 0.862022 11.00000 0.06657 0.05139 = 0.05823 -0.00067 -0.00618 -0.00985 AFIX 43 H4SA 2 0.701609 0.944029 0.907936 11.00000 -1.20000 AFIX 0 C3S 1 0.650853 0.935071 0.811223 11.00000 0.04990 0.05423 = 0.07201 -0.00877 -0.00720 -0.00722 AFIX 43 H3SA 2 0.589198 0.938700 0.822472 11.00000 -1.20000 AFIX 0 C2S 1 0.671484 0.926778 0.745586 11.00000 0.06955 0.05860 = 0.05851 -0.00680 -0.02133 -0.00090 AFIX 43 H2SA 2 0.625528 0.923747 0.709938 11.00000 -1.20000 AFIX 0 C5S 1 0.825540 0.926822 0.786132 11.00000 0.05151 0.07979 = 0.10301 0.00230 0.00625 -0.00026 AFIX 43 H5SA 2 0.887767 0.924248 0.776061 11.00000 -1.20000 AFIX 0 C12S 1 0.244929 0.990411 0.423600 11.00000 0.09011 0.13506 = 0.10341 0.06995 -0.02541 -0.04085 AFIX 43 H12B 2 0.254772 1.002697 0.378395 11.00000 -1.20000 AFIX 0 C1S 1 0.761179 0.922911 0.732405 11.00000 0.09580 0.09876 = 0.05411 -0.00639 0.01099 0.00171 AFIX 43 H1SA 2 0.779272 0.917582 0.686770 11.00000 -1.20000 AFIX 0 C11S 1 0.198889 1.004490 0.536630 11.00000 0.08200 0.08999 = 0.17253 -0.00831 0.02496 0.00946 AFIX 43 H11A 2 0.177775 1.025147 0.573666 11.00000 -1.20000 AFIX 0 N7S 3 0.226998 0.951752 0.545362 11.00000 0.11267 0.14082 = 0.12920 0.01110 -0.00115 0.00694 C9S 1 0.203435 1.027704 0.465050 11.00000 0.06590 0.06605 = 0.27269 0.04182 -0.03823 -0.02332 AFIX 43 H90A 2 0.181522 1.062114 0.450800 11.00000 -1.20000 AFIX 0 C8S 1 0.272049 0.942365 0.436130 11.00000 0.08325 0.14159 = 0.09616 0.04358 0.00312 -0.02437 AFIX 43 H8SA 2 0.300227 0.921628 0.402159 11.00000 -1.20000 AFIX 0 C10S 1 0.260795 0.924289 0.492141 11.00000 0.09045 0.14007 = 0.10917 -0.00294 -0.00919 0.00380 AFIX 43 H10F 2 0.276907 0.887658 0.499878 11.00000 -1.20000 AFIX 0 H1A 2 0.009085 0.193546 0.900717 11.00000 0.02649 H5A 2 0.306573 0.242013 0.733135 11.00000 0.04301 HKLF 4 REM solveFINAL in P2(1)/n REM R1 = 0.0429 for 11749 Fo > 4sig(Fo) and 0.0650 for all 15592 data REM 891 parameters refined using 0 restraints END WGHT 0.0552 7.1718 REM Highest difference peak 0.990, deepest hole -0.451, 1-sigma level 0.068 Q1 1 0.1809 1.0460 0.5046 11.00000 0.05 0.99 Q2 1 0.1998 1.0360 0.4336 11.00000 0.05 0.77 Q3 1 0.2094 1.0096 0.4574 11.00000 0.05 0.73 Q4 1 0.4809 0.3710 0.9888 11.00000 0.05 0.48 Q5 1 0.3027 0.9610 0.4817 11.00000 0.05 0.40 Q6 1 0.2766 0.9342 0.4227 11.00000 0.05 0.38 Q7 1 0.2061 0.9913 0.5287 11.00000 0.05 0.36 Q8 1 0.2789 0.9924 0.5539 11.00000 0.05 0.36 Q9 1 0.3451 0.3338 0.9414 11.00000 0.05 0.35 Q10 1 0.7239 0.3048 0.7872 11.00000 0.05 0.35 Q11 1 0.2437 0.2499 0.5773 11.00000 0.05 0.34 Q12 1 0.4261 0.0791 0.9809 11.00000 0.05 0.33 Q13 1 0.1151 0.4041 0.6995 11.00000 0.05 0.33 Q14 1 0.0851 0.0829 0.6833 11.00000 0.05 0.33 Q15 1 0.4589 0.3850 0.9450 11.00000 0.05 0.33 Q16 1 0.5187 0.0716 0.6806 11.00000 0.05 0.32 Q17 1 -0.3606 0.0472 0.8190 11.00000 0.05 0.32 Q18 1 0.1188 0.0536 0.7199 11.00000 0.05 0.31 Q19 1 -0.0188 0.3267 0.8641 11.00000 0.05 0.31 Q20 1 0.2783 0.2147 0.5760 11.00000 0.05 0.31 ; _shelx_res_checksum 33052 _shelx_hkl_file ; -2 0 0 62.49 1.07 2 0 0 62.38 1.07 -3 0 0 -0.16 0.13 3 0 0 0.04 0.14 4 0 0 106.95 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5 -24 8.91 0.78 3 -5 24 2.99 0.56 -3 -5 -24 2.42 0.57 -3 5 -24 2.10 0.55 3 5 24 2.58 0.62 4 -6 -24 1.02 0.54 -4 6 24 1.13 0.61 4 6 -24 1.41 0.56 3 -6 -24 2.61 0.54 3 6 -24 4.57 0.63 -3 6 24 3.34 0.66 2 -6 -24 0.36 0.47 -2 6 24 -0.02 0.54 2 6 -24 -0.06 0.48 1 -6 -24 0.75 0.51 -1 6 24 0.92 0.57 1 6 -24 1.02 0.52 0 -6 -24 1.33 0.49 0 6 24 0.90 0.58 0 6 -24 0.81 0.51 -1 -6 -24 0.34 0.47 -1 6 -24 -0.28 0.48 1 6 24 0.62 0.56 -2 -6 -24 3.94 0.58 -2 6 -24 3.61 0.59 2 6 24 4.51 0.69 3 -7 -24 0.29 0.50 -3 7 24 -0.16 0.54 3 7 -24 0.18 0.49 2 -7 -24 4.14 0.60 2 7 -24 3.48 0.58 -2 7 24 3.21 0.66 1 -7 -24 -0.43 0.45 -1 7 24 -0.71 0.57 1 7 -24 0.34 0.51 0 -7 -24 0.35 0.49 0 7 24 -0.32 0.58 0 7 -24 0.32 0.51 -1 -7 -24 -0.93 0.47 -1 7 -24 0.37 0.49 1 7 24 -0.46 0.59 2 -8 -24 2.03 0.55 -2 8 24 1.42 0.59 2 8 -24 2.19 0.57 1 -8 -24 4.92 0.68 1 8 -24 4.69 0.71 -1 8 24 4.54 0.67 0 -8 -24 0.37 0.50 0 8 -24 0.25 0.49 0 8 24 0.09 0.56 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 97380 loop_ _space_group_symop_operation_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' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Mn1 Mn 0.11749(2) 0.12057(2) 0.86213(2) 0.02434(9) Uani 1 1 d . . Mn2 Mn 0.27902(2) 0.15076(2) 0.78403(2) 0.02619(10) Uani 1 1 d . . Mn3 Mn 0.03267(2) 0.22406(2) 0.78152(2) 0.02405(9) Uani 1 1 d . . Mn4 Mn 0.25541(2) 0.27045(2) 0.84600(2) 0.02458(9) Uani 1 1 d . . N1 N 0.00292(13) 0.17091(9) 0.86529(12) 0.0274(5) Uani 1 1 d . . N2 N 0.14651(13) 0.12263(8) 0.75396(10) 0.0244(4) Uani 1 1 d . . N3 N 0.12414(14) 0.17732(8) 0.72974(11) 0.0261(4) Uani 1 1 d . . N4 N 0.06418(13) 0.30141(8) 0.81001(10) 0.0235(4) Uani 1 1 d . . N5 N 0.33012(14) 0.22900(9) 0.77014(12) 0.0281(5) Uani 1 1 d . . N6 N 0.24649(13) 0.15214(8) 0.89375(10) 0.0245(4) Uani 1 1 d . . N7 N 0.22126(14) 0.20752(9) 0.90998(11) 0.0260(4) Uani 1 1 d . . N8 N 0.15716(13) 0.31655(8) 0.79846(11) 0.0243(4) Uani 1 1 d . . N10 N 0.09865(14) 0.04167(9) 0.90833(11) 0.0277(5) Uani 1 1 d . . N20 N 0.38279(15) 0.10014(10) 0.73639(12) 0.0345(5) Uani 1 1 d . . N30 N -0.09030(14) 0.23202(9) 0.71259(12) 0.0313(5) Uani 1 1 d . . N40 N 0.35990(15) 0.31519(9) 0.91204(12) 0.0329(5) Uani 1 1 d . . C11 C -0.08480(16) 0.14776(11) 0.86682(13) 0.0270(5) Uani 1 1 d . . C12 C -0.14756(18) 0.16456(12) 0.91403(15) 0.0346(6) Uani 1 1 d . . H12A H -0.1307 0.1914 0.9470 0.042 Uiso 1 1 calc R U C13 C -0.23419(19) 0.14251(13) 0.91331(17) 0.0426(7) Uani 1 1 d . . H13A H -0.2752 0.1542 0.9463 0.051 Uiso 1 1 calc R U C14 C -0.26217(19) 0.10392(13) 0.86572(19) 0.0462(8) Uani 1 1 d . . C15 C -0.19946(19) 0.08613(12) 0.82008(17) 0.0400(7) Uani 1 1 d . . H15A H -0.2164 0.0590 0.7876 0.048 Uiso 1 1 calc R U C16 C -0.11224(18) 0.10729(11) 0.82100(14) 0.0319(6) Uani 1 1 d . . H16A H -0.0704 0.0938 0.7896 0.038 Uiso 1 1 calc R U C17 C -0.3582(2) 0.08131(17) 0.8641(3) 0.0744(13) Uani 1 1 d . . H17A H -0.3923 0.0986 0.9000 0.112 Uiso 1 1 calc R U H17B H -0.3557 0.0424 0.8722 0.112 Uiso 1 1 calc R U H17C H -0.3883 0.0884 0.8191 0.112 Uiso 1 1 calc R U C21 C 0.10210(16) 0.08108(10) 0.71701(13) 0.0265(5) Uani 1 1 d . . C22 C 0.03577(18) 0.08999(12) 0.66462(14) 0.0335(6) Uani 1 1 d . . H22A H 0.0222 0.1258 0.6503 0.040 Uiso 1 1 calc R U C23 C -0.0104(2) 0.04737(14) 0.63338(18) 0.0494(8) Uani 1 1 d . . H23A H -0.0556 0.0543 0.5981 0.059 Uiso 1 1 calc R U C24 C 0.0083(3) -0.00488(15) 0.6527(2) 0.0607(10) Uani 1 1 d . . H24A H -0.0249 -0.0339 0.6319 0.073 Uiso 1 1 calc R U C25 C 0.0759(3) -0.01476(13) 0.70276(18) 0.0522(8) Uani 1 1 d . . H25A H 0.0899 -0.0508 0.7157 0.063 Uiso 1 1 calc R U C26 C 0.1234(2) 0.02734(11) 0.73424(15) 0.0365(6) Uani 1 1 d . . H26A H 0.1707 0.0199 0.7677 0.044 Uiso 1 1 calc R U C31 C 0.16318(16) 0.19156(11) 0.66853(13) 0.0266(5) Uani 1 1 d . . C32 C 0.21807(18) 0.15814(12) 0.63055(13) 0.0324(6) Uani 1 1 d . . H32A H 0.2262 0.1215 0.6436 0.039 Uiso 1 1 calc R U C33 C 0.2610(2) 0.17812(14) 0.57364(15) 0.0436(7) Uani 1 1 d . . H33A H 0.3003 0.1552 0.5497 0.052 Uiso 1 1 calc R U C34 C 0.2478(3) 0.23009(15) 0.55161(16) 0.0538(9) Uani 1 1 d . . H34A H 0.2770 0.2432 0.5125 0.065 Uiso 1 1 calc R U C35 C 0.1908(2) 0.26323(14) 0.58768(16) 0.0479(8) Uani 1 1 d . . H35A H 0.1806 0.2993 0.5728 0.057 Uiso 1 1 calc R U C36 C 0.1489(2) 0.24473(12) 0.64442(14) 0.0344(6) Uani 1 1 d . . H36A H 0.1097 0.2680 0.6679 0.041 Uiso 1 1 calc R U C41 C 0.01959(16) 0.33534(10) 0.85249(12) 0.0246(5) Uani 1 1 d . . C42 C 0.05667(19) 0.38264(11) 0.88215(14) 0.0336(6) Uani 1 1 d . . H42A H 0.1157 0.3938 0.8708 0.040 Uiso 1 1 calc R U C43 C 0.0091(2) 0.41330(13) 0.92750(16) 0.0436(7) Uani 1 1 d . . H43A H 0.0369 0.4444 0.9477 0.052 Uiso 1 1 calc R U C44 C -0.0778(2) 0.39987(14) 0.94416(16) 0.0463(8) Uani 1 1 d . . H44A H -0.1103 0.4214 0.9749 0.056 Uiso 1 1 calc R U C45 C -0.11612(19) 0.35416(14) 0.91478(15) 0.0416(7) Uani 1 1 d . . H45A H -0.1761 0.3444 0.9255 0.050 Uiso 1 1 calc R U C46 C -0.06984(17) 0.32204(12) 0.87010(13) 0.0307(6) Uani 1 1 d . . H46A H -0.0983 0.2908 0.8510 0.037 Uiso 1 1 calc R U C51 C 0.42379(16) 0.23950(11) 0.78069(14) 0.0285(5) Uani 1 1 d . . C52 C 0.47173(17) 0.21693(12) 0.83740(15) 0.0339(6) Uani 1 1 d . . H52A H 0.4411 0.1937 0.8673 0.041 Uiso 1 1 calc R U C53 C 0.56244(18) 0.22775(13) 0.85072(16) 0.0399(7) Uani 1 1 d . . H53A H 0.5927 0.2123 0.8901 0.048 Uiso 1 1 calc R U C54 C 0.61069(19) 0.26057(14) 0.80807(17) 0.0453(8) Uani 1 1 d . . C55 C 0.5640(2) 0.28266(14) 0.75175(16) 0.0459(8) Uani 1 1 d . . H55A H 0.5954 0.3052 0.7215 0.055 Uiso 1 1 calc R U C56 C 0.47232(18) 0.27281(12) 0.73817(15) 0.0370(6) Uani 1 1 d . . H56A H 0.4422 0.2890 0.6993 0.044 Uiso 1 1 calc R U C57 C 0.7097(2) 0.27165(18) 0.8239(2) 0.0662(11) Uani 1 1 d . . H57A H 0.7298 0.2523 0.8658 0.099 Uiso 1 1 calc R U H57B H 0.7189 0.3104 0.8309 0.099 Uiso 1 1 calc R U H57C H 0.7451 0.2595 0.7855 0.099 Uiso 1 1 calc R U C61 C 0.31956(16) 0.13036(11) 0.93364(13) 0.0273(5) Uani 1 1 d . . C62 C 0.35166(18) 0.07939(11) 0.91563(14) 0.0333(6) Uani 1 1 d . . H62A H 0.3206 0.0596 0.8799 0.040 Uiso 1 1 calc R U C63 C 0.4274(2) 0.05750(14) 0.94884(17) 0.0457(8) Uani 1 1 d . . H63A H 0.4487 0.0232 0.9353 0.055 Uiso 1 1 calc R U C64 C 0.4728(2) 0.08500(15) 1.00176(17) 0.0491(8) Uani 1 1 d . . H64A H 0.5254 0.0699 1.0242 0.059 Uiso 1 1 calc R U C65 C 0.44117(19) 0.13380(13) 1.02128(15) 0.0411(7) Uani 1 1 d . . H65A H 0.4719 0.1525 1.0580 0.049 Uiso 1 1 calc R U C66 C 0.36441(18) 0.15698(12) 0.98849(14) 0.0333(6) Uani 1 1 d . . H66A H 0.3428 0.1908 1.0035 0.040 Uiso 1 1 calc R U C71 C 0.16375(16) 0.21307(10) 0.96305(12) 0.0246(5) Uani 1 1 d . . C72 C 0.12315(17) 0.26423(11) 0.97134(13) 0.0290(5) Uani 1 1 d . . H72A H 0.1437 0.2937 0.9451 0.035 Uiso 1 1 calc R U C73 C 0.05502(18) 0.27283(12) 1.01601(14) 0.0349(6) Uani 1 1 d . . H73A H 0.0276 0.3074 1.0185 0.042 Uiso 1 1 calc R U C74 C 0.02620(18) 0.23131(13) 1.05729(14) 0.0377(7) Uani 1 1 d . . H74A H -0.0221 0.2367 1.0871 0.045 Uiso 1 1 calc R U C75 C 0.06929(19) 0.18187(12) 1.05408(14) 0.0367(6) Uani 1 1 d . . H75A H 0.0520 0.1537 1.0838 0.044 Uiso 1 1 calc R U C76 C 0.13736(18) 0.17223(11) 1.00840(13) 0.0295(6) Uani 1 1 d . . H76A H 0.1661 0.1380 1.0078 0.035 Uiso 1 1 calc R U C81 C 0.16766(16) 0.35462(10) 0.74893(12) 0.0246(5) Uani 1 1 d . . C82 C 0.25714(18) 0.36704(11) 0.72898(15) 0.0342(6) Uani 1 1 d . . H82A H 0.3077 0.3500 0.7519 0.041 Uiso 1 1 calc R U C83 C 0.2716(2) 0.40331(13) 0.67697(16) 0.0419(7) Uani 1 1 d . . H83A H 0.3318 0.4100 0.6640 0.050 Uiso 1 1 calc R U C84 C 0.2002(2) 0.43010(13) 0.64340(16) 0.0439(7) Uani 1 1 d . . H84A H 0.2106 0.4550 0.6076 0.053 Uiso 1 1 calc R U C85 C 0.1135(2) 0.41972(13) 0.66327(15) 0.0421(7) Uani 1 1 d . . H85A H 0.0640 0.4383 0.6410 0.051 Uiso 1 1 calc R U C86 C 0.09622(18) 0.38307(11) 0.71475(14) 0.0308(6) Uani 1 1 d . . H86A H 0.0355 0.3771 0.7271 0.037 Uiso 1 1 calc R U C102 C 0.03171(18) 0.00816(12) 0.88722(15) 0.0348(6) Uani 1 1 d . . H10A H -0.0076 0.0189 0.8496 0.042 Uiso 1 1 calc R U C103 C 0.01720(19) -0.04109(12) 0.91743(16) 0.0377(6) Uani 1 1 d . . H10B H -0.0317 -0.0634 0.9015 0.045 Uiso 1 1 calc R U C104 C 0.0746(2) -0.05735(12) 0.97090(15) 0.0386(7) Uani 1 1 d . . H10C H 0.0668 -0.0915 0.9919 0.046 Uiso 1 1 calc R U C105 C 0.1434(2) -0.02362(12) 0.99369(15) 0.0388(7) Uani 1 1 d . . H10D H 0.1837 -0.0340 1.0308 0.047 Uiso 1 1 calc R U C106 C 0.15314(18) 0.02536(11) 0.96198(14) 0.0321(6) Uani 1 1 d . . H10E H 0.2003 0.0487 0.9785 0.039 Uiso 1 1 calc R U C202 C 0.3852(2) 0.04686(13) 0.73750(18) 0.0486(8) Uani 1 1 d . . H20A H 0.3438 0.0285 0.7652 0.058 Uiso 1 1 calc R U C203 C 0.4440(3) 0.01657(15) 0.7010(2) 0.0640(11) Uani 1 1 d . . H20B H 0.4429 -0.0216 0.7036 0.077 Uiso 1 1 calc R U C204 C 0.5040(3) 0.04200(16) 0.6610(2) 0.0642(11) Uani 1 1 d . . H20C H 0.5453 0.0218 0.6353 0.077 Uiso 1 1 calc R U C205 C 0.5037(3) 0.09744(16) 0.6582(2) 0.0613(10) Uani 1 1 d . . H20D H 0.5447 0.1163 0.6308 0.074 Uiso 1 1 calc R U C206 C 0.4423(2) 0.12486(14) 0.69658(18) 0.0468(8) Uani 1 1 d . . H20E H 0.4419 0.1631 0.6948 0.056 Uiso 1 1 calc R U C302 C -0.1183(2) 0.28101(12) 0.69293(15) 0.0388(7) Uani 1 1 d . . H30A H -0.0823 0.3113 0.7063 0.047 Uiso 1 1 calc R U C303 C -0.1976(2) 0.28931(13) 0.65392(17) 0.0460(8) Uani 1 1 d . . H30B H -0.2151 0.3247 0.6402 0.055 Uiso 1 1 calc R U C304 C -0.2510(2) 0.24579(14) 0.63506(16) 0.0465(8) Uani 1 1 d . . H30C H -0.3065 0.2507 0.6091 0.056 Uiso 1 1 calc R U C305 C -0.2229(2) 0.19553(14) 0.65429(17) 0.0476(8) Uani 1 1 d . . H30D H -0.2584 0.1648 0.6418 0.057 Uiso 1 1 calc R U C306 C -0.1420(2) 0.18996(12) 0.69215(16) 0.0408(7) Uani 1 1 d . . H30E H -0.1220 0.1547 0.7043 0.049 Uiso 1 1 calc R U C402 C 0.3681(2) 0.30054(13) 0.97773(16) 0.0428(7) Uani 1 1 d . . H40A H 0.3182 0.2828 0.9971 0.051 Uiso 1 1 calc R U C403 C 0.4451(2) 0.30968(15) 1.01929(18) 0.0553(9) Uani 1 1 d . . H40B H 0.4478 0.2980 1.0657 0.066 Uiso 1 1 calc R U C404 C 0.5168(2) 0.33558(16) 0.99311(18) 0.0566(9) Uani 1 1 d . . H40C H 0.5706 0.3420 1.0207 0.068 Uiso 1 1 calc R U C405 C 0.5099(2) 0.35222(14) 0.92585(19) 0.0507(8) Uani 1 1 d . . H40D H 0.5584 0.3711 0.9063 0.061 Uiso 1 1 calc R U C406 C 0.4311(2) 0.34093(12) 0.88719(17) 0.0419(7) Uani 1 1 d . . H40E H 0.4272 0.3520 0.8405 0.050 Uiso 1 1 calc R U N1S N 0.8052(2) 0.93388(14) 0.85008(19) 0.0663(9) Uani 1 1 d . . C4S C 0.7183(3) 0.93832(15) 0.8620(2) 0.0590(9) Uani 1 1 d . . H4SA H 0.7016 0.9440 0.9079 0.071 Uiso 1 1 calc R U C3S C 0.6509(2) 0.93507(15) 0.8112(2) 0.0590(9) Uani 1 1 d . . H3SA H 0.5892 0.9387 0.8225 0.071 Uiso 1 1 calc R U C2S C 0.6715(3) 0.92678(16) 0.7456(2) 0.0630(10) Uani 1 1 d . . H2SA H 0.6255 0.9237 0.7099 0.076 Uiso 1 1 calc R U C5S C 0.8255(3) 0.92682(19) 0.7861(3) 0.0780(13) Uani 1 1 d . . H5SA H 0.8878 0.9242 0.7761 0.094 Uiso 1 1 calc R U C12S C 0.2449(4) 0.9904(3) 0.4236(3) 0.110(2) Uani 1 1 d . . H12B H 0.2548 1.0027 0.3784 0.133 Uiso 1 1 calc R U C1S C 0.7612(4) 0.9229(2) 0.7324(2) 0.0827(14) Uani 1 1 d . . H1SA H 0.7793 0.9176 0.6868 0.099 Uiso 1 1 calc R U C11S C 0.1989(4) 1.0045(3) 0.5366(4) 0.114(2) Uani 1 1 d . . H11A H 0.1778 1.0251 0.5737 0.137 Uiso 1 1 calc R U N7S N 0.2270(4) 0.9518(3) 0.5454(3) 0.1278(18) Uani 1 1 d . . C9S C 0.2034(4) 1.0277(2) 0.4651(5) 0.136(3) Uani 1 1 d . . H90A H 0.1815 1.0621 0.4508 0.164 Uiso 1 1 calc R U C8S C 0.2720(4) 0.9424(3) 0.4361(3) 0.107(2) Uani 1 1 d . . H8SA H 0.3002 0.9216 0.4022 0.128 Uiso 1 1 calc R U C10S C 0.2608(4) 0.9243(3) 0.4921(4) 0.114(2) Uani 1 1 d . . H10F H 0.2769 0.8877 0.4999 0.136 Uiso 1 1 calc R U H1A H 0.0091(18) 0.1935(12) 0.9007(15) 0.026(7) Uiso 1 1 d . . H5A H 0.307(2) 0.2420(13) 0.7331(17) 0.043(9) Uiso 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.02282(17) 0.0263(2) 0.02380(19) 0.00464(15) -0.00002(14) -0.00239(14) Mn2 0.02238(17) 0.0303(2) 0.0260(2) -0.00066(16) 0.00171(14) -0.00118(15) Mn3 0.02195(17) 0.0240(2) 0.02596(19) 0.00179(15) -0.00069(14) -0.00095(14) Mn4 0.02179(17) 0.0257(2) 0.02605(19) 0.00428(16) -0.00115(14) -0.00075(14) N1 0.0225(10) 0.0319(12) 0.0276(11) 0.0003(10) 0.0001(8) -0.0013(9) N2 0.0269(10) 0.0241(11) 0.0222(10) 0.0022(8) -0.0010(8) -0.0006(8) N3 0.0306(10) 0.0220(11) 0.0257(11) 0.0024(9) 0.0026(8) -0.0012(8) N4 0.0210(9) 0.0230(11) 0.0266(11) 0.0023(9) 0.0018(8) -0.0015(8) N5 0.0216(10) 0.0349(13) 0.0279(11) 0.0041(10) 0.0007(8) -0.0001(9) N6 0.0268(10) 0.0224(11) 0.0239(10) 0.0009(8) -0.0031(8) 0.0004(8) N7 0.0278(10) 0.0241(11) 0.0260(11) 0.0027(9) -0.0003(8) 0.0004(8) N8 0.0196(9) 0.0251(11) 0.0280(11) 0.0035(9) -0.0001(8) -0.0008(8) N10 0.0297(10) 0.0262(12) 0.0275(11) 0.0043(9) 0.0057(9) -0.0008(9) N20 0.0358(12) 0.0353(14) 0.0326(12) -0.0007(10) 0.0036(10) 0.0036(10) N30 0.0284(11) 0.0325(13) 0.0326(12) 0.0013(10) -0.0032(9) 0.0000(9) N40 0.0325(11) 0.0318(13) 0.0338(12) 0.0021(10) -0.0048(9) -0.0049(9) C11 0.0248(11) 0.0285(14) 0.0277(13) 0.0076(11) 0.0001(10) 0.0013(10) C12 0.0338(14) 0.0361(16) 0.0343(15) 0.0031(12) 0.0042(11) 0.0040(11) C13 0.0304(14) 0.0444(18) 0.0541(19) 0.0086(15) 0.0138(13) 0.0056(12) C14 0.0287(14) 0.0373(18) 0.073(2) 0.0127(16) 0.0042(14) 0.0000(12) C15 0.0348(14) 0.0326(16) 0.0520(18) 0.0027(14) -0.0055(13) -0.0049(12) C16 0.0307(13) 0.0317(15) 0.0333(14) 0.0014(12) 0.0012(11) -0.0003(11) C17 0.0322(17) 0.059(3) 0.133(4) 0.003(2) 0.014(2) -0.0101(16) C21 0.0252(11) 0.0286(14) 0.0260(12) -0.0011(10) 0.0029(10) -0.0025(10) C22 0.0335(13) 0.0306(15) 0.0358(15) 0.0000(12) -0.0048(11) -0.0005(11) C23 0.0465(17) 0.047(2) 0.053(2) -0.0063(16) -0.0158(15) -0.0104(15) C24 0.072(2) 0.040(2) 0.068(2) -0.0098(18) -0.0169(19) -0.0196(17) C25 0.076(2) 0.0239(16) 0.056(2) -0.0043(14) -0.0036(18) -0.0035(15) C26 0.0458(16) 0.0300(15) 0.0335(15) 0.0016(12) -0.0010(12) 0.0023(12) C31 0.0265(12) 0.0301(14) 0.0228(12) 0.0009(10) -0.0024(9) -0.0050(10) C32 0.0324(13) 0.0384(16) 0.0263(13) 0.0017(12) 0.0007(11) -0.0002(11) C33 0.0436(16) 0.055(2) 0.0326(15) 0.0011(14) 0.0110(13) 0.0012(14) C34 0.070(2) 0.062(2) 0.0310(16) 0.0102(16) 0.0197(15) -0.0139(18) C35 0.068(2) 0.0388(18) 0.0364(16) 0.0123(14) 0.0014(15) -0.0093(15) C36 0.0454(15) 0.0313(15) 0.0265(13) 0.0013(11) 0.0013(12) -0.0047(12) C41 0.0244(11) 0.0282(14) 0.0212(12) 0.0058(10) -0.0001(9) 0.0014(10) C42 0.0384(14) 0.0286(15) 0.0342(14) 0.0018(12) 0.0048(11) -0.0008(11) C43 0.0577(19) 0.0327(16) 0.0406(17) -0.0035(13) 0.0049(14) 0.0044(14) C44 0.0507(18) 0.051(2) 0.0383(17) -0.0010(15) 0.0091(14) 0.0181(15) C45 0.0314(14) 0.062(2) 0.0322(15) 0.0057(14) 0.0057(12) 0.0083(13) C46 0.0252(12) 0.0391(16) 0.0276(13) 0.0036(12) -0.0005(10) 0.0022(11) C51 0.0223(11) 0.0305(14) 0.0329(14) -0.0014(11) 0.0034(10) 0.0004(10) C52 0.0267(12) 0.0380(16) 0.0371(15) 0.0064(12) 0.0016(11) -0.0032(11) C53 0.0284(13) 0.0489(18) 0.0421(16) 0.0080(14) -0.0023(12) 0.0015(12) C54 0.0276(14) 0.059(2) 0.0500(18) 0.0045(16) 0.0041(13) -0.0065(13) C55 0.0345(15) 0.061(2) 0.0423(17) 0.0103(15) 0.0072(13) -0.0125(14) C56 0.0326(13) 0.0458(18) 0.0329(15) 0.0070(13) 0.0057(11) -0.0005(12) C57 0.0331(16) 0.095(3) 0.070(3) 0.018(2) -0.0011(16) -0.0142(18) C61 0.0259(12) 0.0307(14) 0.0254(12) 0.0057(11) 0.0027(10) -0.0011(10) C62 0.0384(14) 0.0300(15) 0.0314(14) 0.0014(12) 0.0014(11) 0.0047(11) C63 0.0470(17) 0.0418(19) 0.0485(19) 0.0038(15) 0.0050(14) 0.0173(14) C64 0.0423(16) 0.061(2) 0.0433(18) 0.0120(16) -0.0053(14) 0.0192(15) C65 0.0356(15) 0.053(2) 0.0338(15) 0.0023(14) -0.0096(12) 0.0006(13) C66 0.0332(13) 0.0365(16) 0.0297(14) -0.0006(12) -0.0033(11) 0.0012(11) C71 0.0234(11) 0.0290(14) 0.0210(12) 0.0004(10) -0.0054(9) -0.0019(9) C72 0.0320(13) 0.0310(14) 0.0236(12) 0.0020(11) -0.0039(10) 0.0004(11) C73 0.0339(14) 0.0413(17) 0.0288(14) -0.0006(12) -0.0050(11) 0.0063(12) C74 0.0294(13) 0.055(2) 0.0291(14) -0.0029(13) 0.0032(11) -0.0016(12) C75 0.0407(15) 0.0424(17) 0.0269(14) 0.0042(12) 0.0000(11) -0.0137(13) C76 0.0345(13) 0.0278(14) 0.0259(13) 0.0010(11) -0.0018(10) -0.0063(11) C81 0.0277(12) 0.0226(13) 0.0235(12) 0.0000(10) 0.0008(9) -0.0036(9) C82 0.0311(13) 0.0343(16) 0.0369(15) 0.0061(12) -0.0006(11) -0.0069(11) C83 0.0409(15) 0.0438(18) 0.0419(17) 0.0059(14) 0.0111(13) -0.0137(13) C84 0.0552(18) 0.0378(17) 0.0394(17) 0.0155(14) 0.0087(14) -0.0083(14) C85 0.0504(17) 0.0391(17) 0.0367(16) 0.0151(13) -0.0008(13) 0.0041(13) C86 0.0330(13) 0.0291(14) 0.0304(14) 0.0065(11) 0.0027(11) -0.0016(11) C102 0.0308(13) 0.0342(16) 0.0392(15) 0.0051(12) -0.0009(11) -0.0022(11) C103 0.0340(14) 0.0310(16) 0.0484(17) 0.0012(13) 0.0040(12) -0.0057(11) C104 0.0468(16) 0.0291(15) 0.0409(16) 0.0085(13) 0.0125(13) 0.0010(12) C105 0.0458(16) 0.0372(17) 0.0334(15) 0.0083(13) 0.0012(12) 0.0036(13) C106 0.0347(13) 0.0315(15) 0.0302(14) 0.0003(11) 0.0024(11) -0.0024(11) C202 0.0578(19) 0.0387(18) 0.0507(19) -0.0012(15) 0.0179(16) 0.0002(15) C203 0.086(3) 0.038(2) 0.070(3) -0.0048(18) 0.027(2) 0.0116(18) C204 0.065(2) 0.055(2) 0.075(3) -0.014(2) 0.029(2) 0.0169(18) C205 0.062(2) 0.056(2) 0.069(2) -0.0058(19) 0.0356(19) -0.0028(18) C206 0.0493(18) 0.0391(18) 0.054(2) -0.0034(15) 0.0202(15) -0.0005(14) C302 0.0401(15) 0.0332(16) 0.0422(16) 0.0018(13) -0.0060(13) -0.0014(12) C303 0.0484(17) 0.0403(18) 0.0479(18) 0.0053(14) -0.0119(14) 0.0084(14) C304 0.0353(15) 0.059(2) 0.0440(18) 0.0002(16) -0.0123(13) 0.0061(14) C305 0.0410(16) 0.049(2) 0.0514(19) -0.0007(15) -0.0126(14) -0.0095(14) C306 0.0394(15) 0.0342(16) 0.0479(18) 0.0037(13) -0.0078(13) -0.0014(12) C402 0.0439(16) 0.0455(18) 0.0383(16) 0.0000(14) -0.0035(13) -0.0137(14) C403 0.059(2) 0.065(2) 0.0400(18) 0.0014(17) -0.0129(15) -0.0149(18) C404 0.0492(19) 0.071(3) 0.048(2) -0.0013(18) -0.0121(15) -0.0175(17) C405 0.0409(16) 0.049(2) 0.062(2) 0.0028(17) -0.0029(15) -0.0169(14) C406 0.0436(16) 0.0391(17) 0.0422(17) 0.0042(14) -0.0045(13) -0.0094(13) N1S 0.060(2) 0.061(2) 0.075(2) 0.0106(18) -0.0197(17) -0.0109(16) C4S 0.067(2) 0.051(2) 0.058(2) -0.0007(18) -0.0062(18) -0.0098(18) C3S 0.0499(19) 0.054(2) 0.072(3) -0.0088(19) -0.0072(18) -0.0072(16) C2S 0.070(2) 0.059(2) 0.059(2) -0.0068(19) -0.0213(19) -0.0009(19) C5S 0.052(2) 0.080(3) 0.103(4) 0.002(3) 0.006(2) 0.000(2) C12S 0.090(4) 0.135(6) 0.103(4) 0.070(4) -0.025(3) -0.041(4) C1S 0.096(4) 0.099(4) 0.054(2) -0.006(2) 0.011(2) 0.002(3) C11S 0.082(4) 0.090(4) 0.173(7) -0.008(4) 0.025(4) 0.009(3) N7S 0.113(4) 0.141(5) 0.129(5) 0.011(4) -0.001(4) 0.007(4) C9S 0.066(3) 0.066(4) 0.273(11) 0.042(5) -0.038(5) -0.023(3) C8S 0.083(4) 0.142(6) 0.096(4) 0.044(4) 0.003(3) -0.024(4) C10S 0.090(4) 0.140(6) 0.109(5) -0.003(5) -0.009(4) 0.004(4) 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 Mn1 N6 118.84(9) N1 Mn1 N2 102.15(8) N6 Mn1 N2 93.29(8) N1 Mn1 N10 113.75(8) N6 Mn1 N10 110.02(8) N2 Mn1 N10 117.22(8) N1 Mn1 Mn2 121.86(6) N6 Mn1 Mn2 47.82(6) N2 Mn1 Mn2 45.53(5) N10 Mn1 Mn2 123.88(6) N1 Mn1 Mn3 41.39(6) N6 Mn1 Mn3 99.70(6) N2 Mn1 Mn3 66.37(6) N10 Mn1 Mn3 149.46(6) Mn2 Mn1 Mn3 81.514(14) N5 Mn2 N2 126.60(8) N5 Mn2 N6 101.86(8) N2 Mn2 N6 91.84(8) N5 Mn2 N20 102.13(9) N2 Mn2 N20 109.98(9) N6 Mn2 N20 126.79(8) N5 Mn2 N3 91.57(8) N2 Mn2 N3 35.06(7) N6 Mn2 N3 99.48(7) N20 Mn2 N3 126.41(8) N5 Mn2 Mn1 126.64(6) N2 Mn2 Mn1 46.66(6) N6 Mn2 Mn1 45.24(5) N20 Mn2 Mn1 130.94(7) N3 Mn2 Mn1 63.67(5) N5 Mn2 Mn4 41.05(6) N2 Mn2 Mn4 106.86(6) N6 Mn2 Mn4 65.97(5) N20 Mn2 Mn4 139.99(6) N3 Mn2 Mn4 78.90(5) Mn1 Mn2 Mn4 86.400(14) N4 Mn3 N3 120.76(8) N4 Mn3 N1 114.83(9) N3 Mn3 N1 100.74(8) N4 Mn3 N30 104.46(8) N3 Mn3 N30 106.70(8) N1 Mn3 N30 108.83(8) N4 Mn3 Mn1 122.45(6) N3 Mn3 Mn1 63.05(6) N1 Mn3 Mn1 40.11(6) N30 Mn3 Mn1 130.75(6) N8 Mn4 N7 120.58(8) N8 Mn4 N5 109.50(9) N7 Mn4 N5 101.55(9) N8 Mn4 N40 115.83(9) N7 Mn4 N40 101.94(8) N5 Mn4 N40 105.65(8) N8 Mn4 Mn2 115.73(6) N7 Mn4 Mn2 64.31(6) N5 Mn4 Mn2 40.06(6) N40 Mn4 Mn2 125.70(6) C11 N1 Mn1 119.68(17) C11 N1 Mn3 118.83(16) Mn1 N1 Mn3 98.50(9) C21 N2 N3 114.99(19) C21 N2 Mn2 141.43(17) N3 N2 Mn2 88.54(13) C21 N2 Mn1 111.84(15) N3 N2 Mn1 106.37(14) Mn2 N2 Mn1 87.82(7) C31 N3 N2 114.4(2) C31 N3 Mn3 125.33(17) N2 N3 Mn3 120.06(14) C31 N3 Mn2 91.25(14) N2 N3 Mn2 56.40(10) Mn3 N3 Mn2 122.08(9) C41 N4 N8 114.79(19) C41 N4 Mn3 129.12(16) N8 N4 Mn3 113.92(14) C51 N5 Mn2 120.38(17) C51 N5 Mn4 110.02(17) Mn2 N5 Mn4 98.90(9) C61 N6 N7 115.97(19) C61 N6 Mn1 132.18(17) N7 N6 Mn1 100.14(13) C61 N6 Mn2 109.39(15) N7 N6 Mn2 107.01(13) Mn1 N6 Mn2 86.95(7) C71 N7 N6 115.4(2) C71 N7 Mn4 123.54(17) N6 N7 Mn4 120.38(15) C81 N8 N4 115.44(18) C81 N8 Mn4 127.51(16) N4 N8 Mn4 116.22(14) C102 N10 C106 117.0(2) C102 N10 Mn1 122.52(18) C106 N10 Mn1 120.45(18) C202 N20 C206 116.6(3) C202 N20 Mn2 125.3(2) C206 N20 Mn2 117.7(2) C302 N30 C306 117.4(2) C302 N30 Mn3 119.27(18) C306 N30 Mn3 123.25(19) C402 N40 C406 116.2(2) C402 N40 Mn4 116.28(18) C406 N40 Mn4 123.7(2) C16 C11 C12 117.1(2) C16 C11 N1 121.1(2) C12 C11 N1 121.8(2) C13 C12 C11 120.9(3) C14 C13 C12 121.6(3) C13 C14 C15 117.7(3) C13 C14 C17 121.1(3) C15 C14 C17 121.2(3) C14 C15 C16 121.2(3) C15 C16 C11 121.5(3) C22 C21 N2 123.5(2) C22 C21 C26 117.7(2) N2 C21 C26 118.8(2) C23 C22 C21 120.9(3) C24 C23 C22 120.9(3) C23 C24 C25 119.3(3) C24 C25 C26 120.7(3) C25 C26 C21 120.5(3) N3 C31 C32 125.2(2) N3 C31 C36 117.4(2) C32 C31 C36 117.4(2) C33 C32 C31 120.5(3) C34 C33 C32 121.4(3) C33 C34 C35 118.6(3) C36 C35 C34 121.1(3) C35 C36 C31 121.0(3) N4 C41 C42 124.9(2) N4 C41 C46 118.8(2) C42 C41 C46 116.3(2) C43 C42 C41 121.5(3) C44 C43 C42 121.6(3) C43 C44 C45 117.9(3) C44 C45 C46 122.0(3) C45 C46 C41 120.7(3) C56 C51 C52 116.9(2) C56 C51 N5 123.4(2) C52 C51 N5 119.7(2) C53 C52 C51 121.3(3) C52 C53 C54 121.6(3) C55 C54 C53 117.3(3) C55 C54 C57 122.2(3) C53 C54 C57 120.4(3) C54 C55 C56 121.8(3) C55 C56 C51 121.0(3) C66 C61 C62 117.8(2) C66 C61 N6 124.3(2) C62 C61 N6 117.9(2) C63 C62 C61 121.0(3) C62 C63 C64 120.6(3) C65 C64 C63 119.3(3) C64 C65 C66 121.4(3) C61 C66 C65 119.9(3) N7 C71 C76 126.7(2) N7 C71 C72 117.1(2) C76 C71 C72 116.2(2) C73 C72 C71 122.4(3) C72 C73 C74 120.3(3) C75 C74 C73 118.6(3) C74 C75 C76 121.8(3) C75 C76 C71 120.3(3) N8 C81 C86 125.0(2) N8 C81 C82 118.7(2) C86 C81 C82 116.3(2) C83 C82 C81 121.2(3) C82 C83 C84 121.3(3) C85 C84 C83 118.2(3) C84 C85 C86 122.1(3) C85 C86 C81 120.7(2) N10 C102 C103 123.1(3) C104 C103 C102 118.9(3) C103 C104 C105 119.1(3) C104 C105 C106 119.1(3) N10 C106 C105 122.8(3) N20 C202 C203 123.8(3) C204 C203 C202 119.2(3) C203 C204 C205 119.0(3) C204 C205 C206 118.2(3) N20 C206 C205 123.4(3) N30 C302 C303 122.5(3) C304 C303 C302 119.3(3) C305 C304 C303 118.9(3) C304 C305 C306 118.9(3) N30 C306 C305 123.1(3) N40 C402 C403 123.6(3) C404 C403 C402 119.4(3) C403 C404 C405 118.5(3) C404 C405 C406 118.7(3) N40 C406 C405 123.6(3) C5S N1S C4S 116.7(4) N1S C4S C3S 123.0(4) C2S C3S C4S 120.4(4) C3S C2S C1S 117.1(4) N1S C5S C1S 123.4(4) C8S C12S C9S 130.8(7) C2S C1S C5S 119.3(4) N7S C11S C9S 116.6(6) C10S N7S C11S 120.1(7) C12S C9S C11S 108.8(5) C10S C8S C12S 117.9(8) C8S C10S N7S 125.5(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Mn1 N1 2.105(2) Mn1 N6 2.122(2) Mn1 N2 2.172(2) Mn1 N10 2.179(2) Mn1 Mn2 2.9840(5) Mn1 Mn3 3.2315(5) Mn2 N5 2.105(2) Mn2 N2 2.131(2) Mn2 N6 2.214(2) Mn2 N20 2.218(2) Mn2 N3 2.557(2) Mn2 Mn4 3.2321(6) Mn3 N4 2.046(2) Mn3 N3 2.078(2) Mn3 N1 2.160(2) Mn3 N30 2.213(2) Mn4 N8 2.034(2) Mn4 N7 2.076(2) Mn4 N5 2.148(2) Mn4 N40 2.253(2) N1 C11 1.417(3) N2 C21 1.402(3) N2 N3 1.469(3) N3 C31 1.395(3) N4 C41 1.371(3) N4 N8 1.450(3) N5 C51 1.411(3) N6 C61 1.406(3) N6 N7 1.463(3) N7 C71 1.376(3) N8 C81 1.365(3) N10 C102 1.341(3) N10 C106 1.350(3) N20 C202 1.323(4) N20 C206 1.347(4) N30 C302 1.335(4) N30 C306 1.342(4) N40 C402 1.331(4) N40 C406 1.340(4) C11 C16 1.391(4) C11 C12 1.400(4) C12 C13 1.390(4) C13 C14 1.382(5) C14 C15 1.386(5) C14 C17 1.522(4) C15 C16 1.389(4) C21 C22 1.397(4) C21 C26 1.407(4) C22 C23 1.383(4) C23 C24 1.375(5) C24 C25 1.383(5) C25 C26 1.385(4) C31 C32 1.396(4) C31 C36 1.413(4) C32 C33 1.395(4) C33 C34 1.371(5) C34 C35 1.392(5) C35 C36 1.371(4) C41 C42 1.408(4) C41 C46 1.418(3) C42 C43 1.383(4) C43 C44 1.378(5) C44 C45 1.379(5) C45 C46 1.385(4) C51 C56 1.393(4) C51 C52 1.400(4) C52 C53 1.377(4) C53 C54 1.385(4) C54 C55 1.381(4) C54 C57 1.504(4) C55 C56 1.387(4) C61 C66 1.396(4) C61 C62 1.402(4) C62 C63 1.376(4) C63 C64 1.382(5) C64 C65 1.359(5) C65 C66 1.397(4) C71 C76 1.412(4) C71 C72 1.417(4) C72 C73 1.378(4) C73 C74 1.387(4) C74 C75 1.385(4) C75 C76 1.394(4) C81 C86 1.409(4) C81 C82 1.428(3) C82 C83 1.380(4) C83 C84 1.383(4) C84 C85 1.378(4) C85 C86 1.387(4) C102 C103 1.378(4) C103 C104 1.371(4) C104 C105 1.373(4) C105 C106 1.374(4) C202 C203 1.373(5) C203 C204 1.362(5) C204 C205 1.377(5) C205 C206 1.381(4) C302 C303 1.379(4) C303 C304 1.377(5) C304 C305 1.361(5) C305 C306 1.379(4) C402 C403 1.381(4) C403 C404 1.359(5) C404 C405 1.373(5) C405 C406 1.384(4) N1S C5S 1.307(6) N1S C4S 1.319(5) C4S C3S 1.372(5) C3S C2S 1.345(5) C2S C1S 1.363(6) C5S C1S 1.383(7) C12S C8S 1.278(9) C12S C9S 1.390(10) C11S N7S 1.381(8) C11S C9S 1.514(10) N7S C10S 1.356(8) C8S C10S 1.199(8) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C21 N2 N3 C31 -74.2(3) Mn2 N2 N3 C31 74.17(18) Mn1 N2 N3 C31 161.46(16) C21 N2 N3 Mn3 101.1(2) Mn2 N2 N3 Mn3 -110.63(13) Mn1 N2 N3 Mn3 -23.33(18) C21 N2 N3 Mn2 -148.3(2) Mn1 N2 N3 Mn2 87.29(9) C61 N6 N7 C71 -84.3(2) Mn1 N6 N7 C71 63.47(19) Mn2 N6 N7 C71 153.37(16) C61 N6 N7 Mn4 104.8(2) Mn1 N6 N7 Mn4 -107.44(13) Mn2 N6 N7 Mn4 -17.55(18) C41 N4 N8 C81 -82.7(3) Mn3 N4 N8 C81 112.5(2) C41 N4 N8 Mn4 106.9(2) Mn3 N4 N8 Mn4 -57.89(18) Mn1 N1 C11 C16 -48.4(3) Mn3 N1 C11 C16 72.2(3) Mn1 N1 C11 C12 131.8(2) Mn3 N1 C11 C12 -107.6(3) C16 C11 C12 C13 -1.8(4) N1 C11 C12 C13 178.0(3) C11 C12 C13 C14 -0.9(5) C12 C13 C14 C15 2.6(5) C12 C13 C14 C17 -178.1(3) C13 C14 C15 C16 -1.6(5) C17 C14 C15 C16 179.2(3) C14 C15 C16 C11 -1.1(4) C12 C11 C16 C15 2.8(4) N1 C11 C16 C15 -177.0(2) N3 N2 C21 C22 -5.1(3) Mn2 N2 C21 C22 -127.7(3) Mn1 N2 C21 C22 116.4(2) N3 N2 C21 C26 176.5(2) Mn2 N2 C21 C26 53.8(4) Mn1 N2 C21 C26 -62.1(3) N2 C21 C22 C23 -175.2(3) C26 C21 C22 C23 3.2(4) C21 C22 C23 C24 -0.5(5) C22 C23 C24 C25 -1.8(6) C23 C24 C25 C26 1.2(6) C24 C25 C26 C21 1.6(5) C22 C21 C26 C25 -3.7(4) N2 C21 C26 C25 174.8(3) N2 N3 C31 C32 1.1(3) Mn3 N3 C31 C32 -173.81(19) Mn2 N3 C31 C32 54.4(2) N2 N3 C31 C36 -176.3(2) Mn3 N3 C31 C36 8.8(3) Mn2 N3 C31 C36 -123.0(2) N3 C31 C32 C33 -173.6(3) C36 C31 C32 C33 3.8(4) C31 C32 C33 C34 -2.8(5) C32 C33 C34 C35 0.6(5) C33 C34 C35 C36 0.5(5) C34 C35 C36 C31 0.7(5) N3 C31 C36 C35 174.8(3) C32 C31 C36 C35 -2.8(4) N8 N4 C41 C42 2.1(3) Mn3 N4 C41 C42 164.1(2) N8 N4 C41 C46 -176.3(2) Mn3 N4 C41 C46 -14.2(3) N4 C41 C42 C43 -176.5(3) C46 C41 C42 C43 1.9(4) C41 C42 C43 C44 -2.0(5) C42 C43 C44 C45 0.8(5) C43 C44 C45 C46 0.3(5) C44 C45 C46 C41 -0.3(4) N4 C41 C46 C45 177.7(2) C42 C41 C46 C45 -0.8(4) Mn2 N5 C51 C56 138.9(2) Mn4 N5 C51 C56 -107.2(3) Mn2 N5 C51 C52 -42.8(3) Mn4 N5 C51 C52 71.1(3) C56 C51 C52 C53 0.7(4) N5 C51 C52 C53 -177.7(3) C51 C52 C53 C54 -1.2(5) C52 C53 C54 C55 0.7(5) C52 C53 C54 C57 -180.0(3) C53 C54 C55 C56 0.3(5) C57 C54 C55 C56 -179.0(3) C54 C55 C56 C51 -0.8(5) C52 C51 C56 C55 0.3(4) N5 C51 C56 C55 178.6(3) N7 N6 C61 C66 3.6(3) Mn1 N6 C61 C66 -131.3(2) Mn2 N6 C61 C66 124.6(2) N7 N6 C61 C62 -174.0(2) Mn1 N6 C61 C62 51.1(3) Mn2 N6 C61 C62 -52.9(3) C66 C61 C62 C63 -3.0(4) N6 C61 C62 C63 174.7(3) C61 C62 C63 C64 1.2(5) C62 C63 C64 C65 0.7(5) C63 C64 C65 C66 -0.7(5) C62 C61 C66 C65 3.0(4) N6 C61 C66 C65 -174.6(3) C64 C65 C66 C61 -1.2(5) N6 N7 C71 C76 9.2(3) Mn4 N7 C71 C76 179.84(18) N6 N7 C71 C72 -167.5(2) Mn4 N7 C71 C72 3.1(3) N7 C71 C72 C73 170.6(2) C76 C71 C72 C73 -6.4(4) C71 C72 C73 C74 2.9(4) C72 C73 C74 C75 2.0(4) C73 C74 C75 C76 -3.1(4) C74 C75 C76 C71 -0.7(4) N7 C71 C76 C75 -171.5(2) C72 C71 C76 C75 5.3(3) N4 N8 C81 C86 6.8(4) Mn4 N8 C81 C86 175.9(2) N4 N8 C81 C82 -172.8(2) Mn4 N8 C81 C82 -3.7(3) N8 C81 C82 C83 176.9(3) C86 C81 C82 C83 -2.7(4) C81 C82 C83 C84 1.7(5) C82 C83 C84 C85 0.1(5) C83 C84 C85 C86 -0.8(5) C84 C85 C86 C81 -0.2(5) N8 C81 C86 C85 -177.7(3) C82 C81 C86 C85 1.9(4) C106 N10 C102 C103 -0.2(4) Mn1 N10 C102 C103 -177.8(2) N10 C102 C103 C104 -1.2(4) C102 C103 C104 C105 1.4(4) C103 C104 C105 C106 -0.4(4) C102 N10 C106 C105 1.3(4) Mn1 N10 C106 C105 179.0(2) C104 C105 C106 N10 -1.1(4) C206 N20 C202 C203 0.1(5) Mn2 N20 C202 C203 172.2(3) N20 C202 C203 C204 0.0(6) C202 C203 C204 C205 -0.1(7) C203 C204 C205 C206 0.1(7) C202 N20 C206 C205 -0.1(5) Mn2 N20 C206 C205 -172.9(3) C204 C205 C206 N20 0.1(6) C306 N30 C302 C303 0.8(4) Mn3 N30 C302 C303 -175.5(2) N30 C302 C303 C304 0.9(5) C302 C303 C304 C305 -1.4(5) C303 C304 C305 C306 0.2(5) C302 N30 C306 C305 -2.2(5) Mn3 N30 C306 C305 174.0(3) C304 C305 C306 N30 1.7(5) C406 N40 C402 C403 -1.2(5) Mn4 N40 C402 C403 157.8(3) N40 C402 C403 C404 0.9(6) C402 C403 C404 C405 0.4(6) C403 C404 C405 C406 -1.3(6) C402 N40 C406 C405 0.2(5) Mn4 N40 C406 C405 -157.0(3) C404 C405 C406 N40 1.0(5) C5S N1S C4S C3S 1.0(6) N1S C4S C3S C2S 0.3(6) C4S C3S C2S C1S -1.2(6) C4S N1S C5S C1S -1.3(7) C3S C2S C1S C5S 0.9(7) N1S C5S C1S C2S 0.3(8) C9S C11S N7S C10S 3.1(9) C8S C12S C9S C11S 4.4(9) N7S C11S C9S C12S -5.8(7) C9S C12S C8S C10S 0.7(10) C12S C8S C10S N7S -4.7(10) C11S N7S C10S C8S 2.6(10)