#------------------------------------------------------------------------------ #$Date: 2020-02-05 05:10:02 +0200 (Wed, 05 Feb 2020) $ #$Revision: 247882 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557246.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_1557246 loop_ _publ_author_name 'Peralta, Ricardo' 'Huxley, Michael' 'Young, Rosemary' 'Linder-Patton, Oliver Michael' 'Evans, Jack D.' 'Doonan, Christian J.' 'Sumby, Christopher J.' _publ_section_title ; MOF Matrix Isolation: Cooperative Conformational Mobility Enables Reliable Single Crystal Transformations ; _journal_name_full 'Faraday Discussions' _journal_paper_doi 10.1039/D0FD00012D _journal_year 2020 _chemical_formula_moiety 'C75 H66 Mn3 N12 O12, 3.75(C8 H10)' _chemical_formula_sum 'C105 H103.5 Mn3 N12 O12' _chemical_formula_weight 1890.31 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-01-15 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-01-15 deposited with the CCDC. 2020-02-04 downloaded from the CCDC. ; _cell_angle_alpha 93.98(3) _cell_angle_beta 97.43(3) _cell_angle_gamma 92.02(3) _cell_formula_units_Z 2 _cell_length_a 12.276(3) _cell_length_b 12.869(3) _cell_length_c 31.586(6) _cell_measurement_reflns_used 50428 _cell_measurement_temperature 100(2) _cell_volume 4931(2) _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.15 _diffrn_measured_fraction_theta_full 0.864 _diffrn_measured_fraction_theta_max 0.658 _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Phi Scan' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.71076 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_unetI/netI 0.0870 _diffrn_reflns_Laue_measured_fraction_full 0.864 _diffrn_reflns_Laue_measured_fraction_max 0.658 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 50428 _diffrn_reflns_point_group_measured_fraction_full 0.864 _diffrn_reflns_point_group_measured_fraction_max 0.658 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.099 _diffrn_reflns_theta_min 0.652 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_T_max 29.099 _exptl_absorpt_correction_T_min 0.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'XDS (Kabsch, 1993)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.273 _exptl_crystal_description plate _exptl_crystal_F_000 1977 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.06 _refine_diff_density_max 2.062 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.197 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.663 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1210 _refine_ls_number_reflns 17416 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.663 _refine_ls_R_factor_all 0.1959 _refine_ls_R_factor_gt 0.1480 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4430 _refine_ls_wR_factor_ref 0.4652 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10440 _reflns_number_total 17416 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; test.res created by SHELXL-2014/7 TITL test_a.res in P-1 REM Old TITL Test in P-1 REM SHELXT solution in P-1: R1 0.228, Rweak 0.050, Alpha 0.207 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C107 N11 O13 Mn3 REM test_a.res in P-1 REM wR2 = 0.5024, GooF = S = 2.875, Restrained GooF = 2.875 for all data REM 503 parameters refined using 0 restraints REM Highest difference peak 3.290, deepest hole -1.721, 1-sigma level 0.264 REM 1210 parameters refined using 1 restraints REM Highest difference peak 2.208, deepest hole -1.059, 1-sigma level 0.207 CELL 0.71076 12.276 12.869 31.586 93.979 97.435 92.024 ZERR 2 0.0025 0.0026 0.0063 0.03 0.03 0.03 LATT 1 SFAC C H N O Mn UNIT 210 207 24 24 6 FLAT C101 C102 C103 C107 L.S. 20 PLAN 20 SIZE 0.6 0.26 0.06 TEMP -173 GRID BOND CONF fmap 2 ACTA50 ACTA 50 MERG 2 REM REM REM WGHT 0.200000 FVAR 0.31290 MN1 5 0.000000 0.000000 0.000000 10.50000 0.03339 0.03171 = 0.04402 0.00244 0.00747 0.00898 C1A 1 0.591749 -0.349119 0.266664 11.00000 0.04760 0.03715 = 0.04836 0.00459 0.00883 0.01209 AFIX 23 H1AA 2 0.629619 -0.279410 0.272452 11.00000 -1.20000 H1AB 2 0.648618 -0.401734 0.269701 11.00000 -1.20000 AFIX 0 C1B 1 0.203312 0.772306 -0.165278 11.00000 0.03534 0.04400 = 0.04438 0.00382 0.00333 0.00167 AFIX 23 H1BA 2 0.148323 0.826738 -0.167861 11.00000 -1.20000 H1BB 2 0.207060 0.739285 -0.194280 11.00000 -1.20000 AFIX 0 C1 1 0.310599 0.836211 0.669535 11.00000 0.04562 0.03095 = 0.03967 -0.00264 0.00824 0.00727 AFIX 23 H1A 2 0.256863 0.890989 0.672448 11.00000 -1.20000 H1B 2 0.333918 0.812446 0.698329 11.00000 -1.20000 AFIX 0 MN2 5 0.173430 -0.095198 -0.074281 11.00000 0.03278 0.03318 = 0.04369 0.00138 0.00667 0.00676 MN3 5 0.000000 0.000000 0.500000 10.50000 0.03213 0.03049 = 0.04297 -0.00039 0.00410 0.00764 MN4 5 0.215650 -0.064634 0.578565 11.00000 0.03383 0.03097 = 0.04365 0.00087 0.00477 0.00713 C97 1 0.290707 -0.580027 0.020891 11.00000 0.08529 0.08464 = 0.06444 -0.00815 -0.00411 0.01449 AFIX 137 H97A 2 0.280872 -0.553858 0.049973 11.00000 -1.50000 H97B 2 0.289157 -0.656408 0.019072 11.00000 -1.50000 H97C 2 0.231226 -0.556615 0.000476 11.00000 -1.50000 AFIX 0 N11A 3 0.518618 -0.362791 0.298703 11.00000 0.05130 0.03195 = 0.04416 -0.00242 0.00700 0.01032 N11B 3 0.169431 0.696099 -0.138801 11.00000 0.04385 0.03524 = 0.04230 0.00261 0.00639 0.00302 N11C 3 0.258263 0.748518 0.641414 11.00000 0.03149 0.03616 = 0.04464 -0.00061 0.00289 0.00186 N12A 3 0.474799 -0.458989 0.301975 11.00000 0.04763 0.04848 = 0.04807 0.00451 0.00730 0.01805 N12B 3 0.139784 0.731207 -0.099444 11.00000 0.04227 0.04237 = 0.04374 -0.00298 0.01018 0.00434 N12C 3 0.207251 0.767978 0.602864 11.00000 0.04327 0.04164 = 0.03736 0.00458 0.00351 0.00973 C13A 1 0.408920 -0.445652 0.333185 11.00000 0.02968 0.05147 = 0.05967 -0.00412 0.00822 0.01206 C13B 1 0.122048 0.647066 -0.079456 11.00000 0.03999 0.02731 = 0.04752 0.00208 0.00658 0.00117 C13 1 0.172787 0.677849 0.582689 11.00000 0.04100 0.02934 = 0.05470 -0.00306 0.00761 0.00274 C14A 1 0.418340 -0.340293 0.350661 11.00000 0.04702 0.04075 = 0.04605 0.00173 0.00842 0.01542 C14B 1 0.145779 0.554956 -0.104545 11.00000 0.03299 0.03448 = 0.04924 0.00433 0.00387 0.00419 C14 1 0.208009 0.596760 0.609275 11.00000 0.04926 0.02623 = 0.04883 -0.00114 0.00597 0.00838 C15A 1 0.488035 -0.288124 0.327579 11.00000 0.05197 0.05317 = 0.03505 -0.00409 0.00392 0.01848 C15B 1 0.170950 0.589301 -0.142040 11.00000 0.03461 0.04985 = 0.04710 -0.00527 0.00392 -0.00136 C15 1 0.258687 0.645277 0.646534 11.00000 0.03925 0.03112 = 0.04384 0.00466 0.00599 -0.00044 C16A 1 0.345623 -0.534281 0.345920 11.00000 0.08309 0.06483 = 0.06845 0.00258 0.03167 0.01443 AFIX 137 H16A 2 0.333169 -0.588383 0.322189 11.00000 -1.50000 H16B 2 0.274711 -0.511037 0.353181 11.00000 -1.50000 H16C 2 0.386668 -0.562679 0.370906 11.00000 -1.50000 AFIX 0 C16B 1 0.087655 0.655375 -0.036122 11.00000 0.06079 0.03590 = 0.05065 0.00311 0.01499 0.01192 AFIX 137 H16D 2 0.147050 0.689983 -0.015735 11.00000 -1.50000 H16E 2 0.071491 0.585440 -0.027435 11.00000 -1.50000 H16F 2 0.021679 0.696196 -0.036537 11.00000 -1.50000 AFIX 0 C16 1 0.113408 0.670458 0.538638 11.00000 0.06569 0.03355 = 0.05375 0.00320 -0.00234 0.00404 AFIX 137 H16G 2 0.043098 0.704241 0.538618 11.00000 -1.50000 H16H 2 0.099838 0.596935 0.528375 11.00000 -1.50000 H16I 2 0.157971 0.705304 0.519753 11.00000 -1.50000 AFIX 0 C17A 1 0.528975 -0.178456 0.333380 11.00000 0.06077 0.04643 = 0.04873 -0.00599 0.01006 0.00791 AFIX 137 H17A 2 0.489966 -0.139026 0.311127 11.00000 -1.50000 H17B 2 0.607930 -0.174712 0.331244 11.00000 -1.50000 H17C 2 0.516276 -0.148641 0.361629 11.00000 -1.50000 AFIX 0 C17B 1 0.193569 0.530901 -0.181903 11.00000 0.04664 0.03031 = 0.04927 0.00024 0.00934 0.00398 AFIX 137 H17D 2 0.151776 0.559512 -0.206675 11.00000 -1.50000 H17E 2 0.171538 0.457173 -0.181178 11.00000 -1.50000 H17F 2 0.272335 0.537445 -0.184189 11.00000 -1.50000 AFIX 0 C17 1 0.303538 0.601513 0.688331 11.00000 0.04733 0.03530 = 0.04838 0.00254 0.00182 0.00088 AFIX 137 H17G 2 0.384058 0.603719 0.691270 11.00000 -1.50000 H17H 2 0.275806 0.529191 0.688428 11.00000 -1.50000 H17I 2 0.279730 0.643348 0.712303 11.00000 -1.50000 AFIX 0 N21A 3 0.538156 -0.358318 0.223154 11.00000 0.04512 0.04042 = 0.04793 -0.00279 0.00804 0.02147 N21B 3 0.310123 0.820268 -0.147969 11.00000 0.03670 0.03094 = 0.04797 -0.00279 0.00514 0.00027 N21C 3 0.405739 0.879594 0.652641 11.00000 0.03776 0.03785 = 0.04265 -0.00266 0.00527 0.00478 N22A 3 0.549621 -0.447702 0.198286 11.00000 0.04083 0.04064 = 0.04864 -0.00489 0.00821 0.00879 N22B 3 0.314627 0.883897 -0.111771 11.00000 0.04052 0.03769 = 0.04366 0.00004 0.00971 0.00786 N22C 3 0.382110 0.931818 0.615969 11.00000 0.03306 0.03248 = 0.04577 0.00322 0.00338 0.00707 C23A 1 0.500658 -0.429049 0.159907 11.00000 0.03821 0.05341 = 0.03959 0.00319 0.00348 0.00369 C23B 1 0.419444 0.907975 -0.099024 11.00000 0.04063 0.03922 = 0.04067 0.00135 0.00763 0.00261 C23 1 0.475481 0.949535 0.602411 11.00000 0.02706 0.03986 = 0.05459 -0.00168 0.00555 0.00638 C24A 1 0.455026 -0.329443 0.159342 11.00000 0.03507 0.05424 = 0.04275 0.00988 0.00470 0.00170 C24B 1 0.485895 0.859386 -0.127707 11.00000 0.04195 0.03883 = 0.04337 0.00186 0.00693 0.01035 C24 1 0.565245 0.909101 0.629633 11.00000 0.02853 0.03374 = 0.04431 0.00099 0.00349 0.00943 C25A 1 0.481276 -0.286550 0.200747 11.00000 0.05155 0.03019 = 0.05023 0.00008 0.01328 0.01456 C25B 1 0.411585 0.802335 -0.158664 11.00000 0.03759 0.03208 = 0.05019 0.00073 0.01120 0.01103 C25 1 0.513250 0.864199 0.661083 11.00000 0.04978 0.03272 = 0.04190 0.00037 0.00299 0.00522 C26A 1 0.493272 -0.510851 0.124482 11.00000 0.04998 0.05172 = 0.04409 0.00238 0.00984 0.01774 AFIX 137 H26A 2 0.544147 -0.492408 0.104428 11.00000 -1.50000 H26B 2 0.417993 -0.516993 0.109513 11.00000 -1.50000 H26C 2 0.512765 -0.577548 0.135950 11.00000 -1.50000 AFIX 0 C26B 1 0.457657 0.979520 -0.060383 11.00000 0.04933 0.04459 = 0.05303 -0.01018 0.00728 0.00348 AFIX 137 H26D 2 0.396189 1.020084 -0.052597 11.00000 -1.50000 H26E 2 0.516786 1.026952 -0.066606 11.00000 -1.50000 H26F 2 0.485114 0.938553 -0.036546 11.00000 -1.50000 AFIX 0 C26 1 0.484969 1.007990 0.563740 11.00000 0.03825 0.05504 = 0.05411 0.01107 0.00201 0.01282 AFIX 137 H26G 2 0.477049 0.958964 0.538255 11.00000 -1.50000 H26H 2 0.557072 1.044938 0.566878 11.00000 -1.50000 H26I 2 0.427012 1.058434 0.560706 11.00000 -1.50000 AFIX 0 C27A 1 0.458494 -0.182644 0.220371 11.00000 0.06833 0.03138 = 0.05248 -0.00056 0.00301 0.01594 AFIX 137 H27A 2 0.436363 -0.136326 0.197739 11.00000 -1.50000 H27B 2 0.524966 -0.152902 0.238265 11.00000 -1.50000 H27C 2 0.399122 -0.190155 0.238053 11.00000 -1.50000 AFIX 0 C27B 1 0.433904 0.736499 -0.197180 11.00000 0.04108 0.04745 = 0.04772 -0.00835 0.00836 0.01092 AFIX 137 H27D 2 0.412793 0.663551 -0.194061 11.00000 -1.50000 H27E 2 0.512442 0.742545 -0.199924 11.00000 -1.50000 H27F 2 0.391113 0.760219 -0.222817 11.00000 -1.50000 AFIX 0 C27 1 0.562593 0.809654 0.699204 11.00000 0.03178 0.05233 = 0.05059 0.00478 -0.00097 0.01032 AFIX 137 H27G 2 0.554285 0.851767 0.725560 11.00000 -1.50000 H27H 2 0.640864 0.800348 0.697565 11.00000 -1.50000 H27I 2 0.524738 0.741351 0.699293 11.00000 -1.50000 AFIX 0 C31A 1 0.361781 -0.291929 0.385882 11.00000 0.03901 0.04680 = 0.04830 -0.00020 0.01167 0.00565 C31B 1 0.142256 0.445930 -0.093082 11.00000 0.05208 0.01937 = 0.04526 -0.00100 0.00507 0.01087 C31C 1 0.194974 0.480856 0.597494 11.00000 0.05086 0.01837 = 0.05147 0.00361 0.00883 0.01011 C32A 1 0.272983 -0.236165 0.375933 11.00000 0.05963 0.08128 = 0.04742 -0.01176 0.00021 0.03792 AFIX 43 H32A 2 0.244889 -0.231563 0.346684 11.00000 -1.20000 AFIX 0 C32B 1 0.058223 0.405266 -0.071749 11.00000 0.05027 0.03523 = 0.04716 -0.00250 0.01257 0.01121 AFIX 43 H32B 2 -0.000123 0.448110 -0.065681 11.00000 -1.20000 AFIX 0 C32C 1 0.287957 0.422154 0.605954 11.00000 0.03653 0.04330 = 0.04952 -0.00426 0.00283 0.00013 AFIX 43 H32C 2 0.354875 0.453807 0.620399 11.00000 -1.20000 AFIX 0 C33A 1 0.220487 -0.184314 0.407849 11.00000 0.04897 0.07424 = 0.05061 0.00782 0.00789 0.03572 AFIX 43 H33A 2 0.156159 -0.147175 0.400311 11.00000 -1.20000 AFIX 0 C33B 1 0.058934 0.305163 -0.059573 11.00000 0.03607 0.03047 = 0.04881 -0.00153 0.01282 0.00291 AFIX 43 H33B 2 0.001352 0.278320 -0.045485 11.00000 -1.20000 AFIX 0 C33C 1 0.280452 0.316543 0.592792 11.00000 0.04975 0.02641 = 0.05641 -0.00005 0.00300 0.00810 AFIX 43 H33C 2 0.342393 0.275225 0.598845 11.00000 -1.20000 AFIX 0 C34A 1 0.262937 -0.188114 0.449413 11.00000 0.04939 0.03760 = 0.04979 0.00131 0.01272 0.00484 C34B 1 0.147183 0.242192 -0.068361 11.00000 0.02933 0.03524 = 0.04610 -0.00121 0.00549 0.01219 C34C 1 0.183840 0.271090 0.571005 11.00000 0.04766 0.03007 = 0.04156 -0.00155 0.00709 0.00211 C35A 1 0.352973 -0.247372 0.459668 11.00000 0.06077 0.04238 = 0.03728 0.00306 0.00815 0.01006 AFIX 43 H35A 2 0.381584 -0.252172 0.488852 11.00000 -1.20000 AFIX 0 C35B 1 0.228310 0.280575 -0.090411 11.00000 0.04666 0.02534 = 0.05502 0.00496 0.01388 0.00759 AFIX 43 H35B 2 0.285018 0.236942 -0.097610 11.00000 -1.20000 AFIX 0 C35C 1 0.092550 0.329405 0.563029 11.00000 0.03913 0.03124 = 0.05171 -0.00077 0.00335 -0.00326 AFIX 43 H35C 2 0.025896 0.297943 0.548268 11.00000 -1.20000 AFIX 0 C36A 1 0.402074 -0.299976 0.427774 11.00000 0.03649 0.04855 = 0.05288 0.00483 0.00925 0.00349 AFIX 43 H36A 2 0.463349 -0.341310 0.435089 11.00000 -1.20000 AFIX 0 C36B 1 0.227160 0.383051 -0.102107 11.00000 0.04547 0.04400 = 0.04634 0.00130 0.01070 0.00047 AFIX 43 H36B 2 0.284581 0.409898 -0.116278 11.00000 -1.20000 AFIX 0 C36C 1 0.098749 0.435781 0.576890 11.00000 0.04596 0.02918 = 0.06100 0.00862 0.00920 0.00737 AFIX 43 H36C 2 0.035807 0.476323 0.571894 11.00000 -1.20000 AFIX 0 C37A 1 0.212430 -0.128813 0.485005 11.00000 0.04253 0.03778 = 0.04126 -0.00082 0.01249 0.01078 C37B 1 0.145822 0.132313 -0.054781 11.00000 0.03188 0.03656 = 0.04959 -0.00051 0.00550 0.00528 C37C 1 0.176069 0.157052 0.556728 11.00000 0.03991 0.03376 = 0.04582 0.00700 0.01186 0.00483 O38A 4 0.121187 -0.089111 0.473697 11.00000 0.03930 0.04585 = 0.04894 -0.00182 0.01241 0.01268 O38B 4 0.100197 0.114582 -0.023265 11.00000 0.06103 0.02974 = 0.04877 0.00372 0.00952 0.00776 O38C 4 0.111256 0.126866 0.524863 11.00000 0.05051 0.04618 = 0.04322 0.00247 0.00041 0.00072 O39A 4 0.262981 -0.123965 0.521796 11.00000 0.04784 0.04251 = 0.04368 -0.00248 0.00853 0.01429 O39B 4 0.200027 0.066669 -0.075099 11.00000 0.05227 0.04170 = 0.05332 0.00664 0.01623 0.01133 O39C 4 0.239766 0.097424 0.578925 11.00000 0.04959 0.03022 = 0.05327 0.00092 0.00657 0.00915 C41A 1 0.397506 -0.281124 0.123074 11.00000 0.04885 0.03775 = 0.04574 0.00030 0.00071 0.01016 C41B 1 0.607963 0.867289 -0.122795 11.00000 0.03403 0.04014 = 0.04978 -0.00325 0.00697 0.00074 C41C 1 0.680523 0.911841 0.623553 11.00000 0.03688 0.04095 = 0.04795 0.00620 0.00799 0.00941 C42A 1 0.432850 -0.277784 0.084091 11.00000 0.05269 0.03992 = 0.04778 0.00630 0.00430 0.01095 AFIX 43 H42A 2 0.498778 -0.311000 0.079679 11.00000 -1.20000 AFIX 0 C42B 1 0.664851 0.902957 -0.154617 11.00000 0.04022 0.04712 = 0.03757 0.00113 0.00556 0.00696 AFIX 43 H42B 2 0.625964 0.921744 -0.180769 11.00000 -1.20000 AFIX 0 C42C 1 0.710136 0.879332 0.583505 11.00000 0.03500 0.05062 = 0.04928 -0.00219 0.00405 0.00290 AFIX 43 H42C 2 0.655077 0.851595 0.561278 11.00000 -1.20000 AFIX 0 C43A 1 0.378835 -0.229347 0.050958 11.00000 0.03071 0.06419 = 0.04027 -0.00185 0.00365 0.01195 AFIX 43 H43A 2 0.406718 -0.230149 0.024253 11.00000 -1.20000 AFIX 0 C43B 1 0.780589 0.911027 -0.147789 11.00000 0.04161 0.05091 = 0.03686 0.00208 0.00837 -0.00198 AFIX 43 H43B 2 0.820270 0.930015 -0.170191 11.00000 -1.20000 AFIX 0 C43C 1 0.819239 0.887157 0.575862 11.00000 0.03677 0.05024 = 0.04578 -0.00022 0.00912 0.00891 AFIX 43 H43C 2 0.838602 0.863001 0.548841 11.00000 -1.20000 AFIX 0 C44A 1 0.282578 -0.178701 0.056481 11.00000 0.02664 0.04858 = 0.04547 0.00002 -0.00122 0.00940 C44B 1 0.836253 0.891404 -0.108651 11.00000 0.03635 0.02454 = 0.05157 -0.00126 0.00623 0.00962 C44C 1 0.899263 0.930141 0.607675 11.00000 0.04080 0.02745 = 0.04829 0.00730 0.00496 0.00122 C45A 1 0.243364 -0.182176 0.095131 11.00000 0.04866 0.05803 = 0.04210 0.00178 0.00877 0.01124 AFIX 43 H45A 2 0.177230 -0.148907 0.099173 11.00000 -1.20000 AFIX 0 C45B 1 0.775133 0.855126 -0.076600 11.00000 0.05279 0.04740 = 0.03805 -0.00011 0.00227 0.01737 AFIX 43 H45B 2 0.812845 0.838936 -0.049833 11.00000 -1.20000 AFIX 0 C45C 1 0.872839 0.961839 0.647762 11.00000 0.04408 0.04273 = 0.04201 0.00279 0.00135 0.00501 AFIX 43 H45C 2 0.928763 0.988369 0.669890 11.00000 -1.20000 AFIX 0 C46A 1 0.297358 -0.232675 0.128295 11.00000 0.04766 0.06158 = 0.03870 -0.00139 0.00769 0.00451 AFIX 43 H46A 2 0.267662 -0.235049 0.154550 11.00000 -1.20000 AFIX 0 C46B 1 0.664822 0.843656 -0.083917 11.00000 0.03835 0.03706 = 0.05207 -0.00371 0.01124 -0.00506 AFIX 43 H46B 2 0.625419 0.819190 -0.062328 11.00000 -1.20000 AFIX 0 C46C 1 0.762997 0.954494 0.655448 11.00000 0.03964 0.04545 = 0.04597 0.00352 0.01029 0.00912 AFIX 43 H46C 2 0.744311 0.978698 0.682572 11.00000 -1.20000 AFIX 0 C47A 1 0.220369 -0.125311 0.020007 11.00000 0.03458 0.03670 = 0.04557 0.00146 0.00083 0.00272 C47B 1 0.958317 0.904126 -0.099469 11.00000 0.04363 0.01733 = 0.05114 0.00317 0.01086 0.00713 C47C 1 1.017329 0.939484 0.599166 11.00000 0.05187 0.02225 = 0.04776 0.00317 0.00640 -0.00212 O48A 4 0.256098 -0.131260 -0.015306 11.00000 0.04224 0.04379 = 0.04376 0.00619 0.00273 -0.00064 O48B 4 1.014779 0.917475 -0.129098 11.00000 0.03625 0.04845 = 0.04904 0.00184 0.00913 0.01512 O48C 4 1.036475 0.923383 0.560649 11.00000 0.04609 0.02898 = 0.04255 0.00343 0.00625 0.00412 O49A 4 0.134561 -0.081718 0.028324 11.00000 0.03820 0.04308 = 0.05445 0.00259 0.00242 0.01350 O49B 4 1.004461 0.903575 -0.060439 11.00000 0.04378 0.03145 = 0.04415 -0.00099 0.00809 0.01047 O49C 4 1.091386 0.961281 0.629195 11.00000 0.03464 0.03973 = 0.05137 -0.00303 0.00815 0.01033 C61 1 1.145404 1.203280 0.711082 11.00000 0.04909 0.04557 = 0.05977 -0.00261 0.00337 -0.00537 C62 1 1.206913 1.111125 0.708609 11.00000 0.07602 0.05473 = 0.04606 -0.00924 0.00510 -0.02127 AFIX 43 H62 2 1.211216 1.073812 0.681894 11.00000 -1.20000 AFIX 0 C63 1 1.258193 1.079162 0.745128 11.00000 0.05212 0.03837 = 0.06253 -0.00559 0.01299 0.00757 AFIX 43 H63 2 1.297001 1.016886 0.742806 11.00000 -1.20000 AFIX 0 C64 1 1.260811 1.126650 0.785631 11.00000 0.03651 0.05266 = 0.06338 0.00748 0.00698 0.00367 C65 1 1.198343 1.217930 0.787461 11.00000 0.04834 0.05155 = 0.05292 -0.00204 0.01079 0.00642 AFIX 43 H65 2 1.195016 1.255867 0.814124 11.00000 -1.20000 AFIX 0 C66 1 1.142925 1.250700 0.750369 11.00000 0.05721 0.05521 = 0.05589 0.00116 0.00988 0.00291 AFIX 43 H66 2 1.100233 1.310508 0.752589 11.00000 -1.20000 AFIX 0 C67 1 1.082029 1.237982 0.670830 11.00000 0.06576 0.06235 = 0.05630 0.00525 0.00525 0.00306 AFIX 137 H67A 2 1.003109 1.232881 0.672956 11.00000 -1.50000 H67B 2 1.097675 1.193230 0.646153 11.00000 -1.50000 H67C 2 1.104069 1.310415 0.667191 11.00000 -1.50000 AFIX 0 C68 1 1.318005 1.089991 0.825661 11.00000 0.06457 0.05818 = 0.06139 0.00996 0.01709 0.00878 AFIX 137 H68A 2 1.355945 1.026344 0.819004 11.00000 -1.50000 H68B 2 1.264185 1.075256 0.845070 11.00000 -1.50000 H68C 2 1.371756 1.144102 0.839415 11.00000 -1.50000 AFIX 0 C71 1 -0.002669 0.834499 -0.252324 11.00000 0.02887 0.08603 = 0.05813 0.00705 0.00509 0.01112 C72 1 -0.038319 0.757047 -0.229312 11.00000 0.06270 0.07041 = 0.05616 0.00995 0.01882 0.01471 AFIX 43 H72 2 -0.062235 0.773839 -0.202338 11.00000 -1.20000 AFIX 0 C73 1 -0.039579 0.653601 -0.245397 11.00000 0.06664 0.05724 = 0.07294 0.01305 0.00907 0.00331 AFIX 43 H73 2 -0.064347 0.601029 -0.228759 11.00000 -1.20000 AFIX 0 C74 1 -0.006931 0.624063 -0.283938 11.00000 0.04252 0.05552 = 0.09221 0.01230 0.00756 0.00497 C75 1 0.029444 0.704508 -0.307563 11.00000 0.05224 0.07371 = 0.07504 0.01782 0.02542 0.02111 AFIX 43 H75 2 0.052523 0.688153 -0.334722 11.00000 -1.20000 AFIX 0 C76 1 0.031516 0.805901 -0.291430 11.00000 0.07708 0.05507 = 0.05951 0.01120 0.01575 0.01109 AFIX 43 H76 2 0.057387 0.858844 -0.307642 11.00000 -1.20000 AFIX 0 C77 1 -0.002945 0.948202 -0.236782 11.00000 0.06221 0.07853 = 0.06224 0.00732 0.00691 0.00049 AFIX 137 H77A 2 -0.077570 0.973030 -0.242609 11.00000 -1.50000 H77B 2 0.046913 0.989001 -0.251749 11.00000 -1.50000 H77C 2 0.021642 0.956318 -0.205909 11.00000 -1.50000 AFIX 0 C78 1 -0.007084 0.515783 -0.301100 11.00000 0.08252 0.06748 = 0.11719 0.01191 0.03343 0.01516 AFIX 137 H78A 2 0.067902 0.491172 -0.296779 11.00000 -1.50000 H78B 2 -0.034210 0.510938 -0.331779 11.00000 -1.50000 H78C 2 -0.055047 0.472537 -0.286266 11.00000 -1.50000 AFIX 0 C81 1 0.202171 -0.509138 0.183072 11.00000 0.07093 0.11028 = 0.06194 -0.01230 0.01540 -0.02208 C82 1 0.115480 -0.449415 0.166795 11.00000 0.05937 0.09578 = 0.07221 0.02025 -0.00428 -0.02264 AFIX 43 H82 2 0.069208 -0.476275 0.141689 11.00000 -1.20000 AFIX 0 C83 1 0.093811 -0.353047 0.185489 11.00000 0.05502 0.08424 = 0.07272 0.02164 -0.00473 -0.01131 AFIX 43 H83 2 0.034979 -0.314676 0.172862 11.00000 -1.20000 AFIX 0 C84 1 0.158560 -0.312704 0.222827 11.00000 0.04257 0.07308 = 0.08113 0.01573 0.00991 -0.00287 C85 1 0.247174 -0.369185 0.239658 11.00000 0.04751 0.06220 = 0.06223 0.00414 0.00031 -0.00613 AFIX 43 H85 2 0.293148 -0.342176 0.264815 11.00000 -1.20000 AFIX 0 C86 1 0.268463 -0.465556 0.219550 11.00000 0.05699 0.06682 = 0.06832 0.00597 0.00157 -0.00237 AFIX 43 H86 2 0.329889 -0.502181 0.231145 11.00000 -1.20000 AFIX 0 C87 1 0.223547 -0.607330 0.160497 11.00000 0.08380 0.09504 = 0.08844 -0.01943 0.02232 -0.01612 AFIX 137 H87A 2 0.287148 -0.638335 0.176063 11.00000 -1.50000 H87B 2 0.238916 -0.594511 0.131579 11.00000 -1.50000 H87C 2 0.158963 -0.655222 0.158657 11.00000 -1.50000 AFIX 0 C88 1 0.144055 -0.207554 0.242780 11.00000 0.05111 0.06664 = 0.14297 0.01209 0.01911 0.02650 AFIX 137 H88A 2 0.148375 -0.210498 0.273870 11.00000 -1.50000 H88B 2 0.072085 -0.183214 0.231429 11.00000 -1.50000 H88C 2 0.202094 -0.159281 0.236262 11.00000 -1.50000 AFIX 0 C96 1 0.405784 -0.449617 -0.011588 11.00000 0.04601 0.08965 = 0.05944 -0.01977 0.00201 0.01689 AFIX 43 H96 2 0.339760 -0.415801 -0.020030 11.00000 -1.20000 AFIX 0 C91 1 0.400168 -0.538632 0.010316 11.00000 0.05147 0.06614 = 0.05044 -0.00794 0.00434 0.00130 C92 1 0.497141 -0.591775 0.021609 11.00000 0.08110 0.08127 = 0.05419 -0.02276 -0.00087 0.01683 AFIX 43 H92 2 0.495188 -0.654462 0.035757 11.00000 -1.20000 AFIX 0 C103 1 0.594702 -0.443583 0.515529 10.50000 0.04403 AFIX 43 H103 2 0.661857 -0.405951 0.525996 10.50000 -1.20000 AFIX 0 C102 1 0.588980 -0.519348 0.482707 10.50000 0.03650 AFIX 43 H102 2 0.654109 -0.531798 0.470215 10.50000 -1.20000 AFIX 0 C101 1 0.500049 -0.576189 0.467175 10.50000 0.03969 C107 1 0.532551 -0.654851 0.430431 10.50000 0.04878 AFIX 137 H10A 2 0.555971 -0.615514 0.407453 10.50000 -1.50000 H10B 2 0.468825 -0.701037 0.418965 10.50000 -1.50000 H10C 2 0.592938 -0.696599 0.442175 10.50000 -1.50000 AFIX 0 HKLF 4 REM test_a.res in P-1 REM R1 = 0.1480 for 10440 Fo > 4sig(Fo) and 0.1959 for all 17416 data REM 1210 parameters refined using 1 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 2.062, deepest hole -1.032, 1-sigma level 0.197 Q1 1 0.0111 0.0040 0.0332 11.00000 0.05 2.06 Q2 1 0.1597 -0.0965 -0.1072 11.00000 0.05 2.00 Q3 1 0.1808 -0.0961 -0.0422 11.00000 0.05 1.91 Q4 1 0.2300 -0.0660 0.6101 11.00000 0.05 1.72 Q5 1 0.6080 -0.4784 0.4962 11.00000 0.05 1.61 Q6 1 0.5517 -0.5542 0.4721 11.00000 0.05 1.56 Q7 1 0.5622 -0.4250 0.5289 11.00000 0.05 1.55 Q8 1 0.7254 -0.4249 0.5216 11.00000 0.05 1.53 Q9 1 -0.0125 -0.0031 0.4671 11.00000 0.05 1.52 Q10 1 0.2038 -0.0723 0.5462 11.00000 0.05 1.50 Q11 1 0.2338 0.9416 0.6423 11.00000 0.05 0.91 Q12 1 0.8852 0.7552 0.5686 11.00000 0.05 0.82 Q13 1 0.4621 -0.5855 0.4271 11.00000 0.05 0.78 Q14 1 0.5380 -0.5403 0.5336 11.00000 0.05 0.74 Q15 1 0.9828 0.8996 -0.1563 11.00000 0.05 0.73 Q16 1 0.3203 1.1192 -0.0210 11.00000 0.05 0.72 Q17 1 0.6727 0.8605 -0.0494 11.00000 0.05 0.72 Q18 1 0.8231 0.7455 -0.0779 11.00000 0.05 0.71 Q19 1 0.5273 -0.5601 0.5235 11.00000 0.05 0.69 Q20 1 1.0919 0.9533 0.6625 11.00000 0.05 0.69 REM The information below was added by Olex2. REM REM R1 = 0.1480 for 10440 Fo > 4sig(Fo) and 0.1959 for all 50428 data REM n/a parameters refined using n/a restraints REM Highest difference peak 2.06, deepest hole -1.03 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1959 REM R1_gt = 0.1480 REM wR_ref = 0.4652 REM GOOF = 1.663 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 50428 REM Reflections_gt = 10440 REM Parameters = n/a REM Hole = -1.03 REM Peak = 2.06 REM Flack = n/a ; _cod_data_source_file d0fd00012d2.cif _cod_data_source_block MnMOF-1(p-xylene) _cod_original_cell_volume 4931.1(18) _cod_original_formula_sum 'C105 H103.50 Mn3 N12 O12' _cod_database_code 1557246 _shelx_shelxl_version_number 2014/7 _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_max 0.974 _shelx_estimated_absorpt_t_min 0.776 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained planarity C101, C102, C103, C107 with sigma of 0.1 3. Others Fixed Sof: C103(0.5) H103(0.5) C102(0.5) H102(0.5) C101(0.5) C107(0.5) H10A(0.5) H10B(0.5) H10C(0.5) 4.a Secondary CH2 refined with riding coordinates: C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1(H1A,H1B) 4.b Aromatic/amide H refined with riding coordinates: C32A(H32A), C32B(H32B), C32C(H32C), C33A(H33A), C33B(H33B), C33C(H33C), C35A(H35A), C35B(H35B), C35C(H35C), C36A(H36A), C36B(H36B), C36C(H36C), C42A(H42A), C42B(H42B), C42C(H42C), C43A(H43A), C43B(H43B), C43C(H43C), C45A(H45A), C45B(H45B), C45C(H45C), C46A(H46A), C46B(H46B), C46C(H46C), C62(H62), C63(H63), C65(H65), C66(H66), C72(H72), C73(H73), C75(H75), C76(H76), C82(H82), C83(H83), C85(H85), C86(H86), C96(H96), C92(H92), C103(H103), C102(H102) 4.c Idealised Me refined as rotating group: C97(H97A,H97B,H97C), C16A(H16A,H16B,H16C), C16B(H16D,H16E,H16F), C16(H16G, H16H,H16I), C17A(H17A,H17B,H17C), C17B(H17D,H17E,H17F), C17(H17G,H17H,H17I), C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F), C26(H26G,H26H,H26I), C27A(H27A, H27B,H27C), C27B(H27D,H27E,H27F), C27(H27G,H27H,H27I), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C87(H87A,H87B, H87C), C88(H88A,H88B,H88C), C107(H10A,H10B,H10C) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 _atom_site_refinement_flags_occupancy Mn1 Mn 0.0000 0.0000 0.0000 0.0360(5) Uani 1 2 d S T P C1A C 0.5917(9) -0.3491(9) 0.2667(3) 0.044(2) Uani 1 1 d . . . H1AA H 0.6296 -0.2794 0.2725 0.053 Uiso 1 1 calc R . . H1AB H 0.6486 -0.4017 0.2697 0.053 Uiso 1 1 calc R . . C1B C 0.2033(9) 0.7723(9) -0.1653(3) 0.041(2) Uani 1 1 d . . . H1BA H 0.1483 0.8267 -0.1679 0.050 Uiso 1 1 calc R . . H1BB H 0.2071 0.7393 -0.1943 0.050 Uiso 1 1 calc R . . C1 C 0.3106(9) 0.8362(8) 0.6695(3) 0.039(2) Uani 1 1 d . . . H1A H 0.2569 0.8910 0.6724 0.046 Uiso 1 1 calc R . . H1B H 0.3339 0.8124 0.6983 0.046 Uiso 1 1 calc R . . Mn2 Mn 0.17343(13) -0.09520(12) -0.07428(5) 0.0364(4) Uani 1 1 d . . . Mn3 Mn 0.0000 0.0000 0.5000 0.0353(5) Uani 1 2 d S T P Mn4 Mn 0.21565(13) -0.06463(12) 0.57857(5) 0.0361(4) Uani 1 1 d . . . C97 C 0.2907(14) -0.5800(14) 0.0209(5) 0.080(5) Uani 1 1 d . . . H97A H 0.2809 -0.5539 0.0500 0.120 Uiso 1 1 calc GR . . H97B H 0.2892 -0.6564 0.0191 0.120 Uiso 1 1 calc GR . . H97C H 0.2312 -0.5566 0.0005 0.120 Uiso 1 1 calc GR . . N11A N 0.5186(8) -0.3628(7) 0.2987(3) 0.042(2) Uani 1 1 d . . . N11B N 0.1694(8) 0.6961(7) -0.1388(3) 0.040(2) Uani 1 1 d . . . N11C N 0.2583(7) 0.7485(7) 0.6414(3) 0.0378(19) Uani 1 1 d . . . N12A N 0.4748(8) -0.4590(8) 0.3020(3) 0.048(2) Uani 1 1 d . . . N12B N 0.1398(8) 0.7312(7) -0.0994(3) 0.043(2) Uani 1 1 d . . . N12C N 0.2073(8) 0.7680(7) 0.6029(2) 0.041(2) Uani 1 1 d . . . C13A C 0.4089(9) -0.4457(10) 0.3332(4) 0.047(3) Uani 1 1 d . . . C13B C 0.1220(9) 0.6471(8) -0.0795(3) 0.038(2) Uani 1 1 d . . . C13 C 0.1728(9) 0.6778(8) 0.5827(3) 0.042(2) Uani 1 1 d . . . C14A C 0.4183(10) -0.3403(9) 0.3507(3) 0.044(3) Uani 1 1 d . . . C14B C 0.1458(9) 0.5550(8) -0.1045(3) 0.039(2) Uani 1 1 d . . . C14 C 0.2080(10) 0.5968(8) 0.6093(3) 0.042(2) Uani 1 1 d . . . C15A C 0.4880(10) -0.2881(10) 0.3276(3) 0.047(3) Uani 1 1 d . . . C15B C 0.1710(9) 0.5893(9) -0.1420(3) 0.044(3) Uani 1 1 d . . . C15 C 0.2587(9) 0.6453(8) 0.6465(3) 0.038(2) Uani 1 1 d . . . C16A C 0.3456(14) -0.5343(12) 0.3459(4) 0.070(4) Uani 1 1 d . . . H16A H 0.3332 -0.5884 0.3222 0.105 Uiso 1 1 calc GR . . H16B H 0.2747 -0.5110 0.3532 0.105 Uiso 1 1 calc GR . . H16C H 0.3867 -0.5627 0.3709 0.105 Uiso 1 1 calc GR . . C16B C 0.0877(11) 0.6554(9) -0.0361(3) 0.048(3) Uani 1 1 d . . . H16D H 0.1470 0.6900 -0.0157 0.072 Uiso 1 1 calc GR . . H16E H 0.0715 0.5854 -0.0274 0.072 Uiso 1 1 calc GR . . H16F H 0.0217 0.6962 -0.0365 0.072 Uiso 1 1 calc GR . . C16 C 0.1134(11) 0.6705(9) 0.5386(3) 0.052(3) Uani 1 1 d . . . H16G H 0.0431 0.7042 0.5386 0.078 Uiso 1 1 calc GR . . H16H H 0.0998 0.5969 0.5284 0.078 Uiso 1 1 calc GR . . H16I H 0.1580 0.7053 0.5198 0.078 Uiso 1 1 calc GR . . C17A C 0.5290(11) -0.1785(10) 0.3334(4) 0.052(3) Uani 1 1 d . . . H17A H 0.4900 -0.1390 0.3111 0.078 Uiso 1 1 calc GR . . H17B H 0.6079 -0.1747 0.3312 0.078 Uiso 1 1 calc GR . . H17C H 0.5163 -0.1486 0.3616 0.078 Uiso 1 1 calc GR . . C17B C 0.1936(10) 0.5309(8) -0.1819(3) 0.042(2) Uani 1 1 d . . . H17D H 0.1518 0.5595 -0.2067 0.063 Uiso 1 1 calc GR . . H17E H 0.1715 0.4572 -0.1812 0.063 Uiso 1 1 calc GR . . H17F H 0.2723 0.5374 -0.1842 0.063 Uiso 1 1 calc GR . . C17 C 0.3035(10) 0.6015(9) 0.6883(3) 0.044(2) Uani 1 1 d . . . H17G H 0.3841 0.6037 0.6913 0.066 Uiso 1 1 calc GR . . H17H H 0.2758 0.5292 0.6884 0.066 Uiso 1 1 calc GR . . H17I H 0.2797 0.6433 0.7123 0.066 Uiso 1 1 calc GR . . N21A N 0.5382(8) -0.3583(7) 0.2232(3) 0.044(2) Uani 1 1 d . . . N21B N 0.3101(7) 0.8203(7) -0.1480(3) 0.0389(19) Uani 1 1 d . . . N21C N 0.4057(7) 0.8796(7) 0.6526(3) 0.040(2) Uani 1 1 d . . . N22A N 0.5496(8) -0.4477(7) 0.1983(3) 0.043(2) Uani 1 1 d . . . N22B N 0.3146(7) 0.8839(7) -0.1118(3) 0.040(2) Uani 1 1 d . . . N22C N 0.3821(7) 0.9318(7) 0.6160(3) 0.0371(19) Uani 1 1 d . . . C23A C 0.5007(9) -0.4290(9) 0.1599(3) 0.044(3) Uani 1 1 d . . . C23B C 0.4194(9) 0.9080(9) -0.0990(3) 0.040(2) Uani 1 1 d . . . C23 C 0.4755(9) 0.9495(9) 0.6024(3) 0.041(2) Uani 1 1 d . . . C24A C 0.4550(9) -0.3294(9) 0.1593(3) 0.044(3) Uani 1 1 d . . . C24B C 0.4859(9) 0.8594(9) -0.1277(3) 0.041(2) Uani 1 1 d . . . C24 C 0.5652(8) 0.9091(8) 0.6296(3) 0.036(2) Uani 1 1 d . . . C25A C 0.4813(10) -0.2865(8) 0.2007(3) 0.043(2) Uani 1 1 d . . . C25B C 0.4116(9) 0.8023(8) -0.1587(3) 0.039(2) Uani 1 1 d . . . C25 C 0.5133(10) 0.8642(8) 0.6611(3) 0.042(2) Uani 1 1 d . . . C26A C 0.4933(10) -0.5109(10) 0.1245(3) 0.048(3) Uani 1 1 d . . . H26A H 0.5441 -0.4924 0.1044 0.072 Uiso 1 1 calc GR . . H26B H 0.4180 -0.5170 0.1095 0.072 Uiso 1 1 calc GR . . H26C H 0.5128 -0.5775 0.1360 0.072 Uiso 1 1 calc GR . . C26B C 0.4577(10) 0.9795(10) -0.0604(3) 0.050(3) Uani 1 1 d . . . H26D H 0.3962 1.0201 -0.0526 0.074 Uiso 1 1 calc GR . . H26E H 0.5168 1.0270 -0.0666 0.074 Uiso 1 1 calc GR . . H26F H 0.4851 0.9386 -0.0365 0.074 Uiso 1 1 calc GR . . C26 C 0.4850(10) 1.0080(10) 0.5637(3) 0.049(3) Uani 1 1 d . . . H26G H 0.4770 0.9590 0.5383 0.073 Uiso 1 1 calc GR . . H26H H 0.5571 1.0449 0.5669 0.073 Uiso 1 1 calc GR . . H26I H 0.4270 1.0584 0.5607 0.073 Uiso 1 1 calc GR . . C27A C 0.4585(11) -0.1826(9) 0.2204(4) 0.051(3) Uani 1 1 d . . . H27A H 0.4364 -0.1363 0.1977 0.077 Uiso 1 1 calc GR . . H27B H 0.5250 -0.1529 0.2383 0.077 Uiso 1 1 calc GR . . H27C H 0.3991 -0.1902 0.2381 0.077 Uiso 1 1 calc GR . . C27B C 0.4339(9) 0.7365(9) -0.1972(3) 0.046(3) Uani 1 1 d . . . H27D H 0.4128 0.6636 -0.1941 0.068 Uiso 1 1 calc GR . . H27E H 0.5124 0.7425 -0.1999 0.068 Uiso 1 1 calc GR . . H27F H 0.3911 0.7602 -0.2228 0.068 Uiso 1 1 calc GR . . C27 C 0.5626(9) 0.8097(10) 0.6992(3) 0.045(3) Uani 1 1 d . . . H27G H 0.5543 0.8518 0.7256 0.068 Uiso 1 1 calc GR . . H27H H 0.6409 0.8003 0.6976 0.068 Uiso 1 1 calc GR . . H27I H 0.5247 0.7414 0.6993 0.068 Uiso 1 1 calc GR . . C31A C 0.3618(9) -0.2919(9) 0.3859(3) 0.044(3) Uani 1 1 d . . . C31B C 0.1423(9) 0.4459(8) -0.0931(3) 0.039(2) Uani 1 1 d . . . C31C C 0.1950(9) 0.4809(8) 0.5975(3) 0.040(2) Uani 1 1 d . . . C32A C 0.2730(11) -0.2362(12) 0.3759(4) 0.063(4) Uani 1 1 d . . . H32A H 0.2449 -0.2316 0.3467 0.076 Uiso 1 1 calc R . . C32B C 0.0582(10) 0.4053(9) -0.0717(3) 0.044(2) Uani 1 1 d . . . H32B H -0.0001 0.4481 -0.0657 0.052 Uiso 1 1 calc R . . C32C C 0.2880(9) 0.4222(9) 0.6060(3) 0.044(2) Uani 1 1 d . . . H32C H 0.3549 0.4538 0.6204 0.053 Uiso 1 1 calc R . . C33A C 0.2205(10) -0.1843(11) 0.4078(4) 0.057(3) Uani 1 1 d . . . H33A H 0.1562 -0.1472 0.4003 0.068 Uiso 1 1 calc R . . C33B C 0.0589(9) 0.3052(8) -0.0596(3) 0.038(2) Uani 1 1 d . . . H33B H 0.0014 0.2783 -0.0455 0.046 Uiso 1 1 calc R . . C33C C 0.2805(10) 0.3165(8) 0.5928(3) 0.045(3) Uani 1 1 d . . . H33C H 0.3424 0.2752 0.5988 0.053 Uiso 1 1 calc R . . C34A C 0.2629(10) -0.1881(9) 0.4494(3) 0.045(3) Uani 1 1 d . . . C34B C 0.1472(8) 0.2422(8) -0.0684(3) 0.037(2) Uani 1 1 d . . . C34C C 0.1838(9) 0.2711(8) 0.5710(3) 0.040(2) Uani 1 1 d . . . C35A C 0.3530(10) -0.2474(9) 0.4597(3) 0.046(3) Uani 1 1 d . . . H35A H 0.3816 -0.2522 0.4889 0.056 Uiso 1 1 calc R . . C35B C 0.2283(9) 0.2806(8) -0.0904(3) 0.041(2) Uani 1 1 d . . . H35B H 0.2850 0.2369 -0.0976 0.050 Uiso 1 1 calc R . . C35C C 0.0925(9) 0.3294(8) 0.5630(3) 0.041(2) Uani 1 1 d . . . H35C H 0.0259 0.2979 0.5483 0.049 Uiso 1 1 calc R . . C36A C 0.4021(9) -0.3000(9) 0.4278(3) 0.046(3) Uani 1 1 d . . . H36A H 0.4633 -0.3413 0.4351 0.055 Uiso 1 1 calc R . . C36B C 0.2272(10) 0.3831(9) -0.1021(3) 0.045(3) Uani 1 1 d . . . H36B H 0.2846 0.4099 -0.1163 0.054 Uiso 1 1 calc R . . C36C C 0.0987(10) 0.4358(8) 0.5769(3) 0.045(2) Uani 1 1 d . . . H36C H 0.0358 0.4763 0.5719 0.054 Uiso 1 1 calc R . . C37A C 0.2124(9) -0.1288(9) 0.4850(3) 0.040(2) Uani 1 1 d . . . C37B C 0.1458(9) 0.1323(8) -0.0548(3) 0.039(2) Uani 1 1 d . . . C37C C 0.1761(9) 0.1571(8) 0.5567(3) 0.039(2) Uani 1 1 d . . . O38A O 0.1212(6) -0.0891(6) 0.4737(2) 0.0441(17) Uani 1 1 d . . . O38B O 0.1002(7) 0.1146(6) -0.0233(2) 0.0461(18) Uani 1 1 d . . . O38C O 0.1113(7) 0.1269(6) 0.5249(2) 0.0472(18) Uani 1 1 d . . . O39A O 0.2630(6) -0.1240(6) 0.5218(2) 0.0444(18) Uani 1 1 d . . . O39B O 0.2000(7) 0.0667(6) -0.0751(2) 0.0479(18) Uani 1 1 d . . . O39C O 0.2398(6) 0.0974(6) 0.5789(2) 0.0443(17) Uani 1 1 d . . . C41A C 0.3975(10) -0.2811(9) 0.1231(3) 0.045(3) Uani 1 1 d . . . C41B C 0.6080(9) 0.8673(9) -0.1228(3) 0.042(2) Uani 1 1 d . . . C41C C 0.6805(9) 0.9118(9) 0.6236(3) 0.041(2) Uani 1 1 d . . . C42A C 0.4329(10) -0.2778(9) 0.0841(3) 0.047(3) Uani 1 1 d . . . H42A H 0.4988 -0.3110 0.0797 0.056 Uiso 1 1 calc R . . C42B C 0.6649(9) 0.9030(9) -0.1546(3) 0.042(2) Uani 1 1 d . . . H42B H 0.6260 0.9217 -0.1808 0.050 Uiso 1 1 calc R . . C42C C 0.7101(9) 0.8793(9) 0.5835(3) 0.045(3) Uani 1 1 d . . . H42C H 0.6551 0.8516 0.5613 0.054 Uiso 1 1 calc R . . C43A C 0.3788(9) -0.2293(10) 0.0510(3) 0.045(3) Uani 1 1 d . . . H43A H 0.4067 -0.2301 0.0243 0.054 Uiso 1 1 calc R . . C43B C 0.7806(9) 0.9110(9) -0.1478(3) 0.043(2) Uani 1 1 d . . . H43B H 0.8203 0.9300 -0.1702 0.052 Uiso 1 1 calc R . . C43C C 0.8192(9) 0.8872(9) 0.5759(3) 0.044(3) Uani 1 1 d . . . H43C H 0.8386 0.8630 0.5488 0.053 Uiso 1 1 calc R . . C44A C 0.2826(8) -0.1787(9) 0.0565(3) 0.041(2) Uani 1 1 d . . . C44B C 0.8363(9) 0.8914(8) -0.1087(3) 0.037(2) Uani 1 1 d . . . C44C C 0.8993(9) 0.9301(8) 0.6077(3) 0.039(2) Uani 1 1 d . . . C45A C 0.2434(10) -0.1822(10) 0.0951(3) 0.049(3) Uani 1 1 d . . . H45A H 0.1772 -0.1489 0.0992 0.059 Uiso 1 1 calc R . . C45B C 0.7751(10) 0.8551(9) -0.0766(3) 0.046(3) Uani 1 1 d . . . H45B H 0.8128 0.8389 -0.0498 0.055 Uiso 1 1 calc R . . C45C C 0.8728(9) 0.9618(9) 0.6478(3) 0.043(2) Uani 1 1 d . . . H45C H 0.9288 0.9884 0.6699 0.052 Uiso 1 1 calc R . . C46A C 0.2974(10) -0.2327(10) 0.1283(3) 0.049(3) Uani 1 1 d . . . H46A H 0.2677 -0.2350 0.1545 0.059 Uiso 1 1 calc R . . C46B C 0.6648(9) 0.8437(9) -0.0839(3) 0.043(2) Uani 1 1 d . . . H46B H 0.6254 0.8192 -0.0623 0.051 Uiso 1 1 calc R . . C46C C 0.7630(9) 0.9545(9) 0.6554(3) 0.043(2) Uani 1 1 d . . . H46C H 0.7443 0.9787 0.6826 0.052 Uiso 1 1 calc R . . C47A C 0.2204(9) -0.1253(8) 0.0200(3) 0.039(2) Uani 1 1 d . . . C47B C 0.9583(9) 0.9041(7) -0.0995(3) 0.037(2) Uani 1 1 d . . . C47C C 1.0173(10) 0.9395(8) 0.5992(3) 0.041(2) Uani 1 1 d . . . O48A O 0.2561(6) -0.1313(6) -0.0153(2) 0.0434(17) Uani 1 1 d . . . O48B O 1.0148(6) 0.9175(6) -0.1291(2) 0.0440(17) Uani 1 1 d . . . O48C O 1.0365(6) 0.9234(5) 0.5606(2) 0.0391(16) Uani 1 1 d . . . O49A O 0.1346(6) -0.0817(6) 0.0283(2) 0.0453(18) Uani 1 1 d . . . O49B O 1.0045(6) 0.9036(6) -0.0604(2) 0.0396(16) Uani 1 1 d . . . O49C O 1.0914(6) 0.9613(6) 0.6292(2) 0.0418(17) Uani 1 1 d . . . C61 C 1.1454(11) 1.2033(10) 0.7111(4) 0.052(3) Uani 1 1 d . . . C62 C 1.2069(12) 1.1111(11) 0.7086(4) 0.060(4) Uani 1 1 d . . . H62 H 1.2112 1.0738 0.6819 0.072 Uiso 1 1 calc R . . C63 C 1.2582(11) 1.0792(10) 0.7451(4) 0.051(3) Uani 1 1 d . . . H63 H 1.2970 1.0169 0.7428 0.061 Uiso 1 1 calc R . . C64 C 1.2608(10) 1.1267(10) 0.7856(4) 0.051(3) Uani 1 1 d . . . C65 C 1.1983(10) 1.2179(10) 0.7875(4) 0.051(3) Uani 1 1 d . . . H65 H 1.1950 1.2559 0.8141 0.061 Uiso 1 1 calc R . . C66 C 1.1429(11) 1.2507(11) 0.7504(4) 0.056(3) Uani 1 1 d . . . H66 H 1.1002 1.3105 0.7526 0.067 Uiso 1 1 calc R . . C67 C 1.0820(12) 1.2380(12) 0.6708(4) 0.062(3) Uani 1 1 d . . . H67A H 1.0031 1.2329 0.6730 0.093 Uiso 1 1 calc GR . . H67B H 1.0977 1.1932 0.6462 0.093 Uiso 1 1 calc GR . . H67C H 1.1041 1.3104 0.6672 0.093 Uiso 1 1 calc GR . . C68 C 1.3180(12) 1.0900(11) 0.8257(4) 0.060(3) Uani 1 1 d . . . H68A H 1.3559 1.0263 0.8190 0.090 Uiso 1 1 calc GR . . H68B H 1.2642 1.0753 0.8451 0.090 Uiso 1 1 calc GR . . H68C H 1.3718 1.1441 0.8394 0.090 Uiso 1 1 calc GR . . C71 C -0.0027(10) 0.8345(12) -0.2523(4) 0.057(3) Uani 1 1 d . . . C72 C -0.0383(12) 0.7570(12) -0.2293(4) 0.062(3) Uani 1 1 d . . . H72 H -0.0622 0.7738 -0.2023 0.074 Uiso 1 1 calc R . . C73 C -0.0396(13) 0.6536(12) -0.2454(4) 0.065(4) Uani 1 1 d . . . H73 H -0.0643 0.6010 -0.2288 0.078 Uiso 1 1 calc R . . C74 C -0.0069(11) 0.6241(11) -0.2839(5) 0.063(3) Uani 1 1 d . . . C75 C 0.0294(12) 0.7045(12) -0.3076(4) 0.064(4) Uani 1 1 d . . . H75 H 0.0525 0.6882 -0.3347 0.077 Uiso 1 1 calc R . . C76 C 0.0315(13) 0.8059(11) -0.2914(4) 0.063(3) Uani 1 1 d . . . H76 H 0.0574 0.8588 -0.3076 0.075 Uiso 1 1 calc R . . C77 C -0.0029(13) 0.9482(12) -0.2368(4) 0.068(4) Uani 1 1 d . . . H77A H -0.0776 0.9730 -0.2426 0.102 Uiso 1 1 calc GR . . H77B H 0.0469 0.9890 -0.2517 0.102 Uiso 1 1 calc GR . . H77C H 0.0216 0.9563 -0.2059 0.102 Uiso 1 1 calc GR . . C78 C -0.0071(15) 0.5158(13) -0.3011(6) 0.087(5) Uani 1 1 d . . . H78A H 0.0679 0.4912 -0.2968 0.130 Uiso 1 1 calc GR . . H78B H -0.0342 0.5109 -0.3318 0.130 Uiso 1 1 calc GR . . H78C H -0.0550 0.4725 -0.2863 0.130 Uiso 1 1 calc GR . . C81 C 0.2022(14) -0.5091(16) 0.1831(5) 0.082(5) Uani 1 1 d . . . C82 C 0.1155(14) -0.4494(15) 0.1668(5) 0.077(5) Uani 1 1 d . . . H82 H 0.0692 -0.4763 0.1417 0.092 Uiso 1 1 calc R . . C83 C 0.0938(13) -0.3530(14) 0.1855(5) 0.071(4) Uani 1 1 d . . . H83 H 0.0350 -0.3147 0.1729 0.086 Uiso 1 1 calc R . . C84 C 0.1586(12) -0.3127(12) 0.2228(5) 0.065(4) Uani 1 1 d . . . C85 C 0.2472(11) -0.3692(11) 0.2397(4) 0.058(3) Uani 1 1 d . . . H85 H 0.2931 -0.3422 0.2648 0.070 Uiso 1 1 calc R . . C86 C 0.2685(12) -0.4656(12) 0.2195(4) 0.065(4) Uani 1 1 d . . . H86 H 0.3299 -0.5022 0.2311 0.078 Uiso 1 1 calc R . . C87 C 0.2235(16) -0.6073(15) 0.1605(5) 0.090(5) Uani 1 1 d . . . H87A H 0.2871 -0.6383 0.1761 0.135 Uiso 1 1 calc GR . . H87B H 0.2389 -0.5945 0.1316 0.135 Uiso 1 1 calc GR . . H87C H 0.1590 -0.6552 0.1587 0.135 Uiso 1 1 calc GR . . C88 C 0.1441(13) -0.2076(13) 0.2428(6) 0.086(5) Uani 1 1 d . . . H88A H 0.1484 -0.2105 0.2739 0.128 Uiso 1 1 calc GR . . H88B H 0.0721 -0.1832 0.2314 0.128 Uiso 1 1 calc GR . . H88C H 0.2021 -0.1593 0.2363 0.128 Uiso 1 1 calc GR . . C96 C 0.4058(12) -0.4496(13) -0.0116(4) 0.066(4) Uani 1 1 d . . . H96 H 0.3398 -0.4158 -0.0200 0.080 Uiso 1 1 calc R . . C91 C 0.4002(11) -0.5386(12) 0.0103(4) 0.057(3) Uani 1 1 d . . . C92 C 0.4971(14) -0.5918(14) 0.0216(4) 0.074(4) Uani 1 1 d . . . H92 H 0.4952 -0.6545 0.0358 0.089 Uiso 1 1 calc R . . C103 C 0.5947(19) -0.4436(17) 0.5155(6) 0.044(5) Uiso 0.5 1 d . . . H103 H 0.6619 -0.4060 0.5260 0.053 Uiso 0.5 1 calc R . . C102 C 0.5890(17) -0.5193(15) 0.4827(6) 0.037(4) Uiso 0.5 1 d . . . H102 H 0.6541 -0.5318 0.4702 0.044 Uiso 0.5 1 calc R . . C101 C 0.5000(18) -0.5762(17) 0.4672(6) 0.040(4) Uiso 0.5 1 d . . . C107 C 0.533(2) -0.6549(19) 0.4304(7) 0.049(5) Uiso 0.5 1 d . . . H10A H 0.5560 -0.6155 0.4075 0.073 Uiso 0.5 1 calc GR . . H10B H 0.4688 -0.7010 0.4190 0.073 Uiso 0.5 1 calc GR . . H10C H 0.5929 -0.6966 0.4422 0.073 Uiso 0.5 1 calc GR . . 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 0.0334(13) 0.0317(12) 0.0440(11) 0.0024(8) 0.0075(8) 0.0090(9) C1A 0.048(7) 0.037(6) 0.048(6) 0.005(4) 0.009(4) 0.012(5) C1B 0.035(6) 0.044(6) 0.044(5) 0.004(4) 0.003(4) 0.002(5) C1 0.046(7) 0.031(6) 0.040(5) -0.003(4) 0.008(4) 0.007(4) Mn2 0.0328(9) 0.0332(9) 0.0437(8) 0.0014(6) 0.0067(6) 0.0068(6) Mn3 0.0321(12) 0.0305(12) 0.0430(11) -0.0004(8) 0.0041(8) 0.0076(9) Mn4 0.0338(9) 0.0310(9) 0.0437(8) 0.0009(6) 0.0048(6) 0.0071(6) C97 0.085(12) 0.085(12) 0.064(8) -0.008(7) -0.004(7) 0.014(9) N11A 0.051(6) 0.032(5) 0.044(5) -0.002(3) 0.007(4) 0.010(4) N11B 0.044(6) 0.035(5) 0.042(4) 0.003(3) 0.006(3) 0.003(4) N11C 0.031(5) 0.036(5) 0.045(5) -0.001(3) 0.003(3) 0.002(4) N12A 0.048(6) 0.048(6) 0.048(5) 0.005(4) 0.007(4) 0.018(5) N12B 0.042(6) 0.042(5) 0.044(5) -0.003(4) 0.010(4) 0.004(4) N12C 0.043(6) 0.042(5) 0.037(4) 0.005(3) 0.004(3) 0.010(4) C13A 0.030(6) 0.051(7) 0.060(6) -0.004(5) 0.008(4) 0.012(5) C13B 0.040(6) 0.027(5) 0.048(5) 0.002(4) 0.007(4) 0.001(4) C13 0.041(7) 0.029(6) 0.055(6) -0.003(4) 0.008(4) 0.003(5) C14A 0.047(7) 0.041(6) 0.046(6) 0.002(4) 0.008(4) 0.015(5) C14B 0.033(6) 0.034(6) 0.049(6) 0.004(4) 0.004(4) 0.004(4) C14 0.049(7) 0.026(6) 0.049(6) -0.001(4) 0.006(4) 0.008(5) C15A 0.052(7) 0.053(7) 0.035(5) -0.004(4) 0.004(4) 0.018(6) C15B 0.035(7) 0.050(7) 0.047(6) -0.005(5) 0.004(4) -0.001(5) C15 0.039(6) 0.031(6) 0.044(5) 0.005(4) 0.006(4) 0.000(4) C16A 0.083(11) 0.065(10) 0.068(8) 0.003(7) 0.032(7) 0.014(8) C16B 0.061(8) 0.036(6) 0.051(6) 0.003(4) 0.015(5) 0.012(5) C16 0.066(9) 0.034(6) 0.054(6) 0.003(5) -0.002(5) 0.004(5) C17A 0.061(8) 0.046(7) 0.049(6) -0.006(5) 0.010(5) 0.008(6) C17B 0.047(7) 0.030(6) 0.049(6) 0.000(4) 0.009(4) 0.004(5) C17 0.047(7) 0.035(6) 0.048(6) 0.003(4) 0.002(4) 0.001(5) N21A 0.045(6) 0.040(5) 0.048(5) -0.003(4) 0.008(4) 0.021(4) N21B 0.037(5) 0.031(5) 0.048(5) -0.003(3) 0.005(3) 0.000(4) N21C 0.038(5) 0.038(5) 0.043(4) -0.003(3) 0.005(3) 0.005(4) N22A 0.041(6) 0.041(5) 0.049(5) -0.005(4) 0.008(4) 0.009(4) N22B 0.041(6) 0.038(5) 0.044(5) 0.000(4) 0.010(3) 0.008(4) N22C 0.033(5) 0.032(5) 0.046(5) 0.003(3) 0.003(3) 0.007(4) C23A 0.038(7) 0.053(7) 0.040(5) 0.003(4) 0.003(4) 0.004(5) C23B 0.041(7) 0.039(6) 0.041(5) 0.001(4) 0.008(4) 0.003(5) C23 0.027(6) 0.040(6) 0.055(6) -0.002(4) 0.006(4) 0.006(4) C24A 0.035(6) 0.054(7) 0.043(6) 0.010(5) 0.005(4) 0.002(5) C24B 0.042(7) 0.039(6) 0.043(5) 0.002(4) 0.007(4) 0.010(5) C24 0.029(6) 0.034(6) 0.044(5) 0.001(4) 0.003(4) 0.009(4) C25A 0.052(7) 0.030(6) 0.050(6) 0.000(4) 0.013(4) 0.015(5) C25B 0.038(6) 0.032(6) 0.050(6) 0.001(4) 0.011(4) 0.011(4) C25 0.050(7) 0.033(6) 0.042(5) 0.000(4) 0.003(4) 0.005(5) C26A 0.050(7) 0.052(7) 0.044(6) 0.002(5) 0.010(4) 0.018(5) C26B 0.049(8) 0.045(7) 0.053(6) -0.010(5) 0.007(5) 0.003(5) C26 0.038(7) 0.055(8) 0.054(6) 0.011(5) 0.002(4) 0.013(5) C27A 0.068(8) 0.031(6) 0.052(6) -0.001(5) 0.003(5) 0.016(5) C27B 0.041(7) 0.047(7) 0.048(6) -0.008(5) 0.008(4) 0.011(5) C27 0.032(6) 0.052(7) 0.051(6) 0.005(5) -0.001(4) 0.010(5) C31A 0.039(7) 0.047(7) 0.048(6) 0.000(5) 0.012(4) 0.006(5) C31B 0.052(7) 0.019(5) 0.045(5) -0.001(4) 0.005(4) 0.011(4) C31C 0.051(7) 0.018(5) 0.051(6) 0.004(4) 0.009(4) 0.010(4) C32A 0.060(8) 0.081(10) 0.047(6) -0.012(6) 0.000(5) 0.038(7) C32B 0.050(7) 0.035(6) 0.047(6) -0.002(4) 0.013(4) 0.011(5) C32C 0.037(7) 0.043(7) 0.050(6) -0.004(4) 0.003(4) 0.000(5) C33A 0.049(8) 0.074(9) 0.051(6) 0.008(6) 0.008(5) 0.036(7) C33B 0.036(6) 0.030(6) 0.049(5) -0.002(4) 0.013(4) 0.003(4) C33C 0.050(7) 0.026(6) 0.056(6) 0.000(4) 0.003(5) 0.008(5) C34A 0.049(7) 0.038(6) 0.050(6) 0.001(4) 0.013(5) 0.005(5) C34B 0.029(6) 0.035(6) 0.046(5) -0.001(4) 0.005(4) 0.012(4) C34C 0.048(7) 0.030(6) 0.042(5) -0.002(4) 0.007(4) 0.002(5) C35A 0.061(8) 0.042(7) 0.037(5) 0.003(4) 0.008(4) 0.010(5) C35B 0.047(7) 0.025(5) 0.055(6) 0.005(4) 0.014(5) 0.008(5) C35C 0.039(7) 0.031(6) 0.052(6) -0.001(4) 0.003(4) -0.003(4) C36A 0.036(7) 0.049(7) 0.053(6) 0.005(5) 0.009(4) 0.003(5) C36B 0.045(7) 0.044(7) 0.046(6) 0.001(4) 0.011(4) 0.000(5) C36C 0.046(7) 0.029(6) 0.061(6) 0.009(4) 0.009(5) 0.007(5) C37A 0.043(7) 0.038(6) 0.041(5) -0.001(4) 0.012(4) 0.011(5) C37B 0.032(6) 0.037(6) 0.050(6) -0.001(4) 0.006(4) 0.005(4) C37C 0.040(6) 0.034(6) 0.046(6) 0.007(4) 0.012(4) 0.005(5) O38A 0.039(5) 0.046(5) 0.049(4) -0.002(3) 0.012(3) 0.013(4) O38B 0.061(5) 0.030(4) 0.049(4) 0.004(3) 0.010(3) 0.008(3) O38C 0.051(5) 0.046(5) 0.043(4) 0.002(3) 0.000(3) 0.001(4) O39A 0.048(5) 0.043(5) 0.044(4) -0.002(3) 0.009(3) 0.014(3) O39B 0.052(5) 0.042(5) 0.053(4) 0.007(3) 0.016(3) 0.011(4) O39C 0.050(5) 0.030(4) 0.053(4) 0.001(3) 0.007(3) 0.009(3) C41A 0.049(7) 0.038(6) 0.046(6) 0.000(4) 0.001(4) 0.010(5) C41B 0.034(6) 0.040(6) 0.050(6) -0.003(4) 0.007(4) 0.001(5) C41C 0.037(6) 0.041(6) 0.048(6) 0.006(4) 0.008(4) 0.009(5) C42A 0.053(8) 0.040(7) 0.048(6) 0.006(5) 0.004(5) 0.011(5) C42B 0.040(7) 0.047(7) 0.038(5) 0.001(4) 0.006(4) 0.007(5) C42C 0.035(7) 0.051(7) 0.049(6) -0.002(5) 0.004(4) 0.003(5) C43A 0.031(6) 0.064(8) 0.040(5) -0.002(5) 0.004(4) 0.012(5) C43B 0.042(7) 0.051(7) 0.037(5) 0.002(4) 0.008(4) -0.002(5) C43C 0.037(7) 0.050(7) 0.046(6) 0.000(5) 0.009(4) 0.009(5) C44A 0.027(6) 0.049(7) 0.045(5) 0.000(4) -0.001(4) 0.009(5) C44B 0.036(6) 0.025(5) 0.052(6) -0.001(4) 0.006(4) 0.010(4) C44C 0.041(6) 0.027(5) 0.048(6) 0.007(4) 0.005(4) 0.001(4) C45A 0.049(7) 0.058(8) 0.042(6) 0.002(5) 0.009(4) 0.011(6) C45B 0.053(8) 0.047(7) 0.038(5) 0.000(4) 0.002(4) 0.017(5) C45C 0.044(7) 0.043(6) 0.042(5) 0.003(4) 0.001(4) 0.005(5) C46A 0.048(7) 0.062(8) 0.039(5) -0.001(5) 0.008(4) 0.005(6) C46B 0.038(7) 0.037(6) 0.052(6) -0.004(4) 0.011(4) -0.005(5) C46C 0.040(7) 0.045(7) 0.046(6) 0.004(4) 0.010(4) 0.009(5) C47A 0.035(6) 0.037(6) 0.046(6) 0.001(4) 0.001(4) 0.003(4) C47B 0.044(7) 0.017(5) 0.051(6) 0.003(4) 0.011(4) 0.007(4) C47C 0.052(7) 0.022(5) 0.048(6) 0.003(4) 0.006(5) -0.002(5) O48A 0.042(5) 0.044(5) 0.044(4) 0.006(3) 0.003(3) -0.001(3) O48B 0.036(4) 0.048(5) 0.049(4) 0.002(3) 0.009(3) 0.015(3) O48C 0.046(5) 0.029(4) 0.043(4) 0.003(3) 0.006(3) 0.004(3) O49A 0.038(5) 0.043(5) 0.054(4) 0.003(3) 0.002(3) 0.013(3) O49B 0.044(5) 0.031(4) 0.044(4) -0.001(3) 0.008(3) 0.010(3) O49C 0.035(4) 0.040(4) 0.051(4) -0.003(3) 0.008(3) 0.010(3) C61 0.049(8) 0.046(7) 0.060(7) -0.003(5) 0.003(5) -0.005(6) C62 0.076(10) 0.055(8) 0.046(6) -0.009(5) 0.005(6) -0.021(7) C63 0.052(8) 0.038(7) 0.063(7) -0.006(5) 0.013(5) 0.008(5) C64 0.037(7) 0.053(8) 0.063(7) 0.007(5) 0.007(5) 0.004(5) C65 0.048(8) 0.052(8) 0.053(6) -0.002(5) 0.011(5) 0.006(6) C66 0.057(9) 0.055(8) 0.056(7) 0.001(5) 0.010(5) 0.003(6) C67 0.066(9) 0.062(9) 0.056(7) 0.005(6) 0.005(6) 0.003(7) C68 0.065(9) 0.058(9) 0.061(7) 0.010(6) 0.017(6) 0.009(7) C71 0.029(7) 0.086(10) 0.058(7) 0.007(6) 0.005(5) 0.011(6) C72 0.063(9) 0.070(10) 0.056(7) 0.010(6) 0.019(6) 0.015(7) C73 0.067(10) 0.057(9) 0.073(9) 0.013(6) 0.009(6) 0.003(7) C74 0.043(8) 0.056(9) 0.092(10) 0.012(7) 0.008(6) 0.005(6) C75 0.052(9) 0.074(10) 0.075(8) 0.018(7) 0.025(6) 0.021(7) C76 0.077(10) 0.055(9) 0.060(7) 0.011(6) 0.016(6) 0.011(7) C77 0.062(10) 0.079(11) 0.062(8) 0.007(7) 0.007(6) 0.000(7) C78 0.083(13) 0.067(11) 0.117(13) 0.012(9) 0.033(9) 0.015(9) C81 0.071(12) 0.110(14) 0.062(8) -0.012(8) 0.015(7) -0.022(10) C82 0.059(11) 0.096(13) 0.072(9) 0.020(8) -0.004(7) -0.023(9) C83 0.055(10) 0.084(12) 0.073(9) 0.022(8) -0.005(6) -0.011(8) C84 0.043(8) 0.073(10) 0.081(9) 0.016(7) 0.010(6) -0.003(7) C85 0.048(8) 0.062(9) 0.062(7) 0.004(6) 0.000(5) -0.006(6) C86 0.057(9) 0.067(10) 0.068(8) 0.006(7) 0.002(6) -0.002(7) C87 0.084(13) 0.095(14) 0.088(11) -0.019(9) 0.022(9) -0.016(10) C88 0.051(10) 0.067(11) 0.143(15) 0.012(9) 0.019(8) 0.026(8) C96 0.046(8) 0.090(11) 0.059(7) -0.020(7) 0.002(5) 0.017(7) C91 0.051(8) 0.066(9) 0.050(7) -0.008(6) 0.004(5) 0.001(6) C92 0.081(12) 0.081(11) 0.054(7) -0.023(7) -0.001(7) 0.017(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O38B Mn1 O38B 180.0(3) 2 . O38B Mn1 O49A 94.4(3) . . O38B Mn1 O49A 85.6(3) 2 . O38B Mn1 O49A 85.6(3) . 2 O38B Mn1 O49A 94.4(3) 2 2 O38B Mn1 O49B 91.6(3) . 2_665 O38B Mn1 O49B 91.6(3) 2 1_445 O38B Mn1 O49B 88.4(3) . 1_445 O38B Mn1 O49B 88.4(3) 2 2_665 O49A Mn1 O49A 180.0 2 . O49A Mn1 O49B 88.8(3) 2 2_665 O49A Mn1 O49B 91.2(3) 2 1_445 O49A Mn1 O49B 91.2(3) . 2_665 O49A Mn1 O49B 88.8(3) . 1_445 O49B Mn1 O49B 180.0(5) 2_665 1_445 N21A C1A N11A 114.6(10) . . N11B C1B N21B 111.4(9) . . N21C C1 N11C 111.1(8) . . N12B Mn2 O48B 78.7(3) 1_545 1_445 N22B Mn2 N12B 80.3(3) 1_545 1_545 N22B Mn2 O48B 104.0(3) 1_545 1_445 O39B Mn2 N12B 159.5(3) . 1_545 O39B Mn2 N22B 88.3(3) . 1_545 O39B Mn2 O48B 87.7(3) . 1_445 O39B Mn2 O49B 98.3(3) . 1_445 O48A Mn2 N12B 93.8(3) . 1_545 O48A Mn2 N22B 96.7(3) . 1_545 O48A Mn2 O39B 104.5(3) . . O48A Mn2 O48B 156.3(3) . 1_445 O48A Mn2 O49B 100.9(3) . 1_445 O49B Mn2 N12B 87.1(3) 1_445 1_545 O49B Mn2 N22B 158.9(3) 1_445 1_545 O49B Mn2 O48B 56.6(2) 1_445 1_445 O38A Mn3 O38A 180.0(3) . 2_556 O38A Mn3 O38C 94.7(3) . . O38A Mn3 O38C 94.7(3) 2_556 2_556 O38A Mn3 O38C 85.3(3) . 2_556 O38A Mn3 O38C 85.3(3) 2_556 . O38A Mn3 O48C 90.6(3) . 2_666 O38A Mn3 O48C 89.4(3) . 1_445 O38A Mn3 O48C 90.6(3) 2_556 1_445 O38A Mn3 O48C 89.4(3) 2_556 2_666 O38C Mn3 O38C 180.0 2_556 . O38C Mn3 O48C 90.2(3) . 1_445 O38C Mn3 O48C 89.8(3) 2_556 1_445 O38C Mn3 O48C 89.8(3) . 2_666 O38C Mn3 O48C 90.2(3) 2_556 2_666 O48C Mn3 O48C 180.0 2_666 1_445 N12C Mn4 C47C 82.5(3) 1_545 1_445 N12C Mn4 O49C 80.2(3) 1_545 1_445 N22C Mn4 N12C 79.6(3) 1_545 1_545 N22C Mn4 C47C 133.9(3) 1_545 1_445 N22C Mn4 O49C 106.3(3) 1_545 1_445 O39A Mn4 N12C 90.7(3) . 1_545 O39A Mn4 N22C 95.0(3) . 1_545 O39A Mn4 O39C 105.4(3) . . O39A Mn4 C47C 127.5(3) . 1_445 O39A Mn4 O48C 99.1(3) . 1_445 O39A Mn4 O49C 154.7(3) . 1_445 O39C Mn4 N12C 160.6(3) . 1_545 O39C Mn4 N22C 88.1(3) . 1_545 O39C Mn4 C47C 95.7(3) . 1_445 O39C Mn4 O48C 98.9(3) . 1_445 O39C Mn4 O49C 89.1(3) . 1_445 O48C Mn4 N12C 89.0(3) 1_445 1_545 O48C Mn4 N22C 161.9(3) 1_445 1_545 O48C Mn4 C47C 29.2(3) 1_445 1_445 O48C Mn4 O49C 57.5(2) 1_445 1_445 O49C Mn4 C47C 28.3(3) 1_445 1_445 N12A N11A C1A 118.5(8) . . N12A N11A C15A 113.9(9) . . C15A N11A C1A 127.6(10) . . N12B N11B C1B 117.4(9) . . C15B N11B C1B 132.0(9) . . C15B N11B N12B 110.2(8) . . N12C N11C C1 118.3(9) . . N12C N11C C15 111.5(8) . . C15 N11C C1 130.0(8) . . N11A N12A C13A 104.4(9) . . N11B N12B Mn2 120.2(6) . 1_565 C13B N12B Mn2 131.4(7) . 1_565 C13B N12B N11B 105.9(8) . . N11C N12C Mn4 120.8(7) . 1_565 C13 N12C Mn4 131.0(7) . 1_565 C13 N12C N11C 107.3(9) . . N12A C13A C14A 110.1(11) . . N12A C13A C16A 120.6(11) . . C14A C13A C16A 129.2(10) . . N12B C13B C14B 110.6(9) . . N12B C13B C16B 120.7(9) . . C14B C13B C16B 128.6(9) . . N12C C13 C14 108.6(9) . . N12C C13 C16 121.7(10) . . C14 C13 C16 129.6(9) . . C13A C14A C31A 128.0(11) . . C15A C14A C13A 106.4(9) . . C15A C14A C31A 125.5(11) . . C13B C14B C31B 128.2(9) . . C15B C14B C13B 105.3(9) . . C15B C14B C31B 126.5(10) . . C13 C14 C31C 126.7(9) . . C15 C14 C13 106.0(9) . . C15 C14 C31C 127.2(10) . . N11A C15A C14A 105.0(10) . . N11A C15A C17A 125.8(11) . . C14A C15A C17A 129.0(10) . . N11B C15B C17B 121.5(10) . . C14B C15B N11B 107.7(9) . . C14B C15B C17B 130.8(11) . . N11C C15 C14 106.5(9) . . N11C C15 C17 122.7(9) . . C14 C15 C17 130.7(10) . . N22A N21A C1A 118.4(8) . . C25A N21A C1A 129.2(9) . . C25A N21A N22A 112.1(8) . . N22B N21B C1B 116.8(8) . . N22B N21B C25B 112.0(8) . . C25B N21B C1B 130.6(9) . . N22C N21C C1 115.2(8) . . C25 N21C C1 132.1(9) . . C25 N21C N22C 111.5(8) . . C23A N22A N21A 104.2(9) . . N21B N22B Mn2 123.9(7) . 1_565 C23B N22B Mn2 127.8(7) . 1_565 C23B N22B N21B 106.5(8) . . N21C N22C Mn4 124.6(6) . 1_565 C23 N22C Mn4 126.9(7) . 1_565 C23 N22C N21C 105.8(8) . . N22A C23A C24A 112.5(9) . . N22A C23A C26A 119.7(10) . . C24A C23A C26A 127.7(10) . . N22B C23B C24B 110.5(9) . . N22B C23B C26B 122.5(10) . . C24B C23B C26B 127.0(11) . . N22C C23 C24 111.8(10) . . N22C C23 C26 122.1(10) . . C24 C23 C26 126.1(10) . . C23A C24A C41A 128.2(10) . . C25A C24A C23A 104.2(9) . . C25A C24A C41A 127.5(11) . . C23B C24B C41B 125.3(10) . . C25B C24B C23B 104.9(10) . . C25B C24B C41B 129.8(9) . . C23 C24 C41C 127.0(9) . . C25 C24 C23 103.3(9) . . C25 C24 C41C 129.7(9) . . N21A C25A C24A 107.0(9) . . N21A C25A C27A 122.6(9) . . C24A C25A C27A 130.4(10) . . N21B C25B C24B 106.2(8) . . N21B C25B C27B 124.8(9) . . C24B C25B C27B 129.0(10) . . N21C C25 C24 107.6(9) . . N21C C25 C27 123.1(10) . . C24 C25 C27 129.3(10) . . C32A C31A C14A 119.3(10) . . C32A C31A C36A 119.7(10) . . C36A C31A C14A 120.9(10) . . C32B C31B C14B 122.1(9) . . C36B C31B C14B 118.6(10) . . C36B C31B C32B 119.3(10) . . C32C C31C C14 117.3(10) . . C36C C31C C14 121.6(10) . . C36C C31C C32C 120.9(10) . . C31A C32A C33A 121.5(11) . . C33B C32B C31B 121.3(10) . . C33C C32C C31C 118.6(10) . . C34A C33A C32A 119.1(11) . . C32B C33B C34B 118.9(10) . . C34C C33C C32C 120.6(11) . . C33A C34A C35A 119.3(10) . . C33A C34A C37A 121.0(10) . . C35A C34A C37A 119.6(10) . . C33B C34B C37B 117.8(9) . . C35B C34B C33B 120.1(10) . . C35B C34B C37B 122.0(9) . . C33C C34C C37C 120.5(10) . . C35C C34C C33C 120.3(10) . . C35C C34C C37C 119.2(10) . . C34A C35A C36A 120.7(10) . . C34B C35B C36B 120.2(10) . . C34C C35C C36C 119.5(10) . . C31A C36A C35A 119.6(11) . . C31B C36B C35B 120.1(10) . . C31C C36C C35C 120.0(10) . . O38A C37A C34A 115.7(9) . . O39A C37A C34A 118.1(10) . . O39A C37A O38A 126.2(9) . . O38B C37B C34B 117.9(9) . . O38B C37B O39B 125.3(10) . . O39B C37B C34B 116.6(9) . . O38C C37C C34C 118.6(10) . . O38C C37C O39C 124.6(10) . . O39C C37C C34C 116.8(9) . . C37A O38A Mn3 140.4(6) . . C37B O38B Mn1 141.4(7) . . C37C O38C Mn3 141.6(7) . . C37A O39A Mn4 129.6(7) . . C37B O39B Mn2 122.5(7) . . C37C O39C Mn4 124.7(7) . . C42A C41A C24A 124.8(11) . . C42A C41A C46A 116.7(10) . . C46A C41A C24A 118.4(10) . . C42B C41B C24B 122.0(10) . . C42B C41B C46B 120.2(10) . . C46B C41B C24B 117.8(9) . . C42C C41C C24 119.5(10) . . C46C C41C C24 121.9(9) . . C46C C41C C42C 118.4(10) . . C41A C42A C43A 123.6(11) . . C41B C42B C43B 119.5(10) . . C43C C42C C41C 120.9(10) . . C42A C43A C44A 119.7(10) . . C44B C43B C42B 120.0(9) . . C44C C43C C42C 119.9(10) . . C43A C44A C47A 120.7(9) . . C45A C44A C43A 118.2(10) . . C45A C44A C47A 121.0(10) . . C43B C44B C45B 118.8(10) . . C43B C44B C47B 121.6(9) . . C45B C44B C47B 119.5(9) . . C43C C44C C45C 120.6(10) . . C43C C44C C47C 119.7(9) . . C45C C44C C47C 119.6(9) . . C44A C45A C46A 121.8(11) . . C46B C45B C44B 120.7(10) . . C44C C45C C46C 119.5(10) . . C45A C46A C41A 119.8(10) . . C45B C46B C41B 120.6(10) . . C41C C46C C45C 120.7(9) . . O48A C47A C44A 117.9(9) . . O48A C47A O49A 126.3(10) . . O49A C47A C44A 115.7(9) . . O48B C47B C44B 120.4(9) . . O48B C47B O49B 120.7(10) . . O49B C47B C44B 118.9(9) . . C44C C47C Mn4 173.2(7) . 1_665 O48C C47C Mn4 57.4(5) . 1_665 O48C C47C C44C 117.7(9) . . O49C C47C Mn4 65.1(6) . 1_665 O49C C47C C44C 119.9(9) . . O49C C47C O48C 122.4(11) . . C47A O48A Mn2 127.0(7) . . C47B O48B Mn2 85.2(6) . 1_665 Mn4 O48C Mn3 107.1(3) 1_665 1_665 C47C O48C Mn3 136.7(7) . 1_665 C47C O48C Mn4 93.3(6) . 1_665 C47A O49A Mn1 142.3(7) . . Mn2 O49B Mn1 108.2(3) 1_665 1_665 C47B O49B Mn1 136.1(6) . 1_665 C47B O49B Mn2 96.9(6) . 1_665 C47C O49C Mn4 86.6(6) . 1_665 C62 C61 C67 119.1(11) . . C66 C61 C62 117.0(12) . . C66 C61 C67 123.8(13) . . C63 C62 C61 117.9(11) . . C62 C63 C64 127.1(13) . . C63 C64 C65 114.1(11) . . C63 C64 C68 126.3(12) . . C65 C64 C68 119.6(11) . . C66 C65 C64 119.6(11) . . C61 C66 C65 124.2(13) . . C72 C71 C76 117.8(14) . . C72 C71 C77 121.9(12) . . C76 C71 C77 120.3(13) . . C71 C72 C73 119.9(12) . . C74 C73 C72 123.1(13) . . C73 C74 C75 116.6(14) . . C73 C74 C78 123.7(14) . . C75 C74 C78 119.7(14) . . C76 C75 C74 120.1(13) . . C75 C76 C71 122.5(13) . . C82 C81 C87 120.2(15) . . C86 C81 C82 116.1(17) . . C86 C81 C87 123.5(18) . . C83 C82 C81 123.2(14) . . C82 C83 C84 119.7(15) . . C83 C84 C85 118.7(15) . . C83 C84 C88 122.3(15) . . C85 C84 C88 118.7(13) . . C84 C85 C86 120.3(12) . . C81 C86 C85 121.9(15) . . C92 C96 C91 122.6(14) 2_645 . C96 C91 C97 120.2(13) . . C96 C91 C92 119.2(14) . . C92 C91 C97 120.6(15) . . C96 C92 C91 118.1(16) 2_645 . C102 C103 C101 118(2) . 2_646 C101 C102 C103 125(2) . . C103 C101 C107 135(2) 2_646 . C102 C101 C103 118(2) . 2_646 C102 C101 C107 107.1(18) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mn1 O38B 2.117(8) 2 Mn1 O38B 2.117(8) . Mn1 O49A 2.123(7) 2 Mn1 O49A 2.123(7) . Mn1 O49B 2.211(6) 1_445 Mn1 O49B 2.211(6) 2_665 C1A N11A 1.452(14) . C1A N21A 1.440(13) . C1B N11B 1.417(14) . C1B N21B 1.452(14) . C1 N11C 1.462(13) . C1 N21C 1.455(14) . Mn2 N12B 2.323(9) 1_545 Mn2 N22B 2.236(9) 1_545 Mn2 O39B 2.100(8) . Mn2 O48A 2.093(7) . Mn2 O48B 2.451(7) 1_445 Mn2 O49B 2.174(7) 1_445 Mn3 O38A 2.128(7) . Mn3 O38A 2.128(7) 2_556 Mn3 O38C 2.129(8) 2_556 Mn3 O38C 2.129(8) . Mn3 O48C 2.217(7) 2_666 Mn3 O48C 2.217(7) 1_445 Mn4 N12C 2.340(9) 1_545 Mn4 N22C 2.228(9) 1_545 Mn4 O39A 2.061(7) . Mn4 O39C 2.095(8) . Mn4 C47C 2.601(12) 1_445 Mn4 O48C 2.196(8) 1_445 Mn4 O49C 2.364(7) 1_445 C97 C91 1.51(2) . N11A N12A 1.348(14) . N11A C15A 1.374(13) . N11B N12B 1.390(11) . N11B C15B 1.372(15) . N11C N12C 1.339(11) . N11C C15 1.350(14) . N12A C13A 1.359(14) . N12B Mn2 2.323(9) 1_565 N12B C13B 1.316(14) . N12C Mn4 2.340(9) 1_565 N12C C13 1.313(14) . C13A C14A 1.423(16) . C13A C16A 1.466(19) . C13B C14B 1.439(14) . C13B C16B 1.482(14) . C13 C14 1.429(15) . C13 C16 1.480(15) . C14A C15A 1.380(17) . C14A C31A 1.497(14) . C14B C15B 1.361(15) . C14B C31B 1.474(15) . C14 C15 1.358(14) . C14 C31C 1.510(14) . C15A C17A 1.472(18) . C15B C17B 1.484(14) . C15 C17 1.517(14) . N21A N22A 1.369(12) . N21A C25A 1.360(14) . N21B N22B 1.353(11) . N21B C25B 1.355(13) . N21C N22C 1.383(12) . N21C C25 1.337(14) . N22A C23A 1.323(13) . N22B Mn2 2.236(9) 1_565 N22B C23B 1.317(14) . N22C Mn4 2.228(8) 1_565 N22C C23 1.293(14) . C23A C24A 1.417(17) . C23A C26A 1.474(15) . C23B C24B 1.423(14) . C23B C26B 1.491(15) . C23 C24 1.443(14) . C23 C26 1.493(16) . C24A C25A 1.377(15) . C24A C41A 1.455(15) . C24B C25B 1.396(15) . C24B C41B 1.486(16) . C24 C25 1.395(15) . C24 C41C 1.452(15) . C25A C27A 1.485(15) . C25B C27B 1.494(13) . C25 C27 1.506(15) . C31A C32A 1.342(17) . C31A C36A 1.364(15) . C31B C32B 1.408(15) . C31B C36B 1.388(15) . C31C C32C 1.398(16) . C31C C36C 1.362(16) . C32A C33A 1.408(16) . C32B C33B 1.370(15) . C32C C33C 1.390(15) . C33A C34A 1.353(16) . C33B C34B 1.420(14) . C33C C34C 1.381(16) . C34A C35A 1.382(17) . C34A C37A 1.525(14) . C34B C35B 1.383(15) . C34B C37B 1.506(15) . C34C C35C 1.377(16) . C34C C37C 1.501(15) . C35A C36A 1.388(15) . C35B C36B 1.394(16) . C35C C36C 1.404(15) . C37A O38A 1.267(13) . C37A O39A 1.241(12) . C37B O38B 1.234(12) . C37B O39B 1.282(12) . C37C O38C 1.230(13) . C37C O39C 1.291(13) . C41A C42A 1.360(15) . C41A C46A 1.421(17) . C41B C42B 1.390(15) . C41B C46B 1.390(15) . C41C C42C 1.401(14) . C41C C46C 1.400(16) . C42A C43A 1.365(15) . C42B C43B 1.408(16) . C42C C43C 1.393(16) . C43A C44A 1.394(15) . C43B C44B 1.377(15) . C43C C44C 1.382(15) . C44A C45A 1.372(15) . C44A C47A 1.517(14) . C44B C45B 1.429(16) . C44B C47B 1.490(15) . C44C C45C 1.385(14) . C44C C47C 1.510(16) . C45A C46A 1.380(16) . C45B C46B 1.345(16) . C45C C46C 1.402(16) . C47A O48A 1.249(12) . C47A O49A 1.259(13) . C47B O48B 1.252(12) . C47B O49B 1.289(12) . C47C Mn4 2.602(12) 1_665 C47C O48C 1.273(12) . C47C O49C 1.236(13) . O48B Mn2 2.451(7) 1_665 O48C Mn3 2.217(7) 1_665 O48C Mn4 2.196(8) 1_665 O49B Mn1 2.211(6) 1_665 O49B Mn2 2.174(7) 1_665 O49C Mn4 2.364(7) 1_665 C61 C62 1.43(2) . C61 C66 1.349(17) . C61 C67 1.506(18) . C62 C63 1.339(18) . C63 C64 1.375(16) . C64 C65 1.427(18) . C64 C68 1.480(18) . C65 C66 1.377(18) . C71 C72 1.37(2) . C71 C76 1.385(17) . C71 C77 1.51(2) . C72 C73 1.39(2) . C73 C74 1.36(2) . C74 C75 1.41(2) . C74 C78 1.46(2) . C75 C76 1.37(2) . C81 C82 1.40(3) . C81 C86 1.39(2) . C81 C87 1.46(2) . C82 C83 1.39(2) . C83 C84 1.39(2) . C84 C85 1.40(2) . C84 C88 1.48(2) . C85 C86 1.40(2) . C96 C91 1.38(2) . C96 C92 1.37(2) 2_645 C91 C92 1.41(2) . C92 C96 1.37(2) 2_645 C103 C102 1.37(3) . C103 C101 1.37(3) 2_646 C102 C101 1.31(3) . C101 C103 1.37(3) 2_646 C101 C107 1.59(3) . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 C1A N11A N12A C13A -178.2(9) . . C1A N11A C15A C14A -179.9(10) . . C1A N11A C15A C17A -3.6(18) . . C1A N21A N22A C23A -174.5(10) . . C1A N21A C25A C24A 174.5(11) . . C1A N21A C25A C27A -4.4(19) . . C1B N11B N12B Mn2 -10.0(12) . 1_565 C1B N11B N12B C13B -174.2(9) . . C1B N11B C15B C14B 170.2(11) . . C1B N11B C15B C17B -11.7(18) . . C1B N21B N22B Mn2 6.8(12) . 1_565 C1B N21B N22B C23B 172.4(9) . . C1B N21B C25B C24B -171.6(10) . . C1B N21B C25B C27B 10.2(18) . . C1 N11C N12C Mn4 5.6(12) . 1_565 C1 N11C N12C C13 176.3(9) . . C1 N11C C15 C14 -173.5(10) . . C1 N11C C15 C17 9.7(17) . . C1 N21C N22C Mn4 -7.8(11) . 1_565 C1 N21C N22C C23 -170.2(8) . . C1 N21C C25 C24 168.0(10) . . C1 N21C C25 C27 -13.4(17) . . Mn2 N12B C13B C14B -158.5(7) 1_565 . Mn2 N12B C13B C16B 18.8(16) 1_565 . Mn2 N22B C23B C24B 165.2(7) 1_565 . Mn2 N22B C23B C26B -16.6(16) 1_565 . Mn4 N12C C13 C14 166.9(7) 1_565 . Mn4 N12C C13 C16 -10.0(17) 1_565 . Mn4 N22C C23 C24 -161.5(7) 1_565 . Mn4 N22C C23 C26 20.1(15) 1_565 . Mn4 C47C O48C Mn3 -119.4(9) 1_665 1_665 C97 C91 C92 C96 -179.5(11) . 2_645 N11A C1A N21A N22A -104.5(11) . . N11A C1A N21A C25A 80.6(15) . . N11A N12A C13A C14A -3.4(12) . . N11A N12A C13A C16A 179.7(11) . . N11B C1B N21B N22B -70.0(12) . . N11B C1B N21B C25B 100.2(12) . . N11B N12B C13B C14B 3.2(12) . . N11B N12B C13B C16B -179.5(10) . . N11C C1 N21C N22C 69.7(11) . . N11C C1 N21C C25 -96.8(12) . . N11C N12C C13 C14 -2.5(12) . . N11C N12C C13 C16 -179.4(10) . . N12A N11A C15A C14A -0.8(12) . . N12A N11A C15A C17A 175.5(11) . . N12A C13A C14A C15A 3.0(13) . . N12A C13A C14A C31A -179.2(11) . . N12B N11B C15B C14B -1.8(12) . . N12B N11B C15B C17B 176.3(9) . . N12B C13B C14B C15B -4.3(12) . . N12B C13B C14B C31B 176.6(11) . . N12C N11C C15 C14 1.4(12) . . N12C N11C C15 C17 -175.4(9) . . N12C C13 C14 C15 3.4(13) . . N12C C13 C14 C31C -174.5(11) . . C13A C14A C15A N11A -1.3(12) . . C13A C14A C15A C17A -177.5(12) . . C13A C14A C31A C32A -100.2(16) . . C13A C14A C31A C36A 82.7(16) . . C13B C14B C15B N11B 3.6(12) . . C13B C14B C15B C17B -174.3(11) . . C13B C14B C31B C32B 40.8(16) . . C13B C14B C31B C36B -136.4(11) . . C13 C14 C15 N11C -2.9(12) . . C13 C14 C15 C17 173.6(11) . . C13 C14 C31C C32C 131.2(12) . . C13 C14 C31C C36C -44.6(17) . . C14A C31A C32A C33A -176.4(13) . . C14A C31A C36A C35A 174.9(11) . . C14B C31B C32B C33B -176.9(10) . . C14B C31B C36B C35B 177.9(10) . . C14 C31C C32C C33C -175.6(10) . . C14 C31C C36C C35C 174.3(10) . . C15A N11A N12A C13A 2.6(12) . . C15A C14A C31A C32A 77.2(17) . . C15A C14A C31A C36A -99.9(14) . . C15B N11B N12B Mn2 163.3(7) . 1_565 C15B N11B N12B C13B -0.9(12) . . C15B C14B C31B C32B -138.0(12) . . C15B C14B C31B C36B 44.7(16) . . C15 N11C N12C Mn4 -170.0(7) . 1_565 C15 N11C N12C C13 0.7(12) . . C15 C14 C31C C32C -46.4(17) . . C15 C14 C31C C36C 137.9(12) . . C16A C13A C14A C15A 179.6(13) . . C16A C13A C14A C31A -3(2) . . C16B C13B C14B C15B 178.6(11) . . C16B C13B C14B C31B -0.4(18) . . C16 C13 C14 C15 179.9(12) . . C16 C13 C14 C31C 2(2) . . N21A C1A N11A N12A 70.9(12) . . N21A C1A N11A C15A -110.0(12) . . N21A N22A C23A C24A -1.3(12) . . N21A N22A C23A C26A -177.9(10) . . N21B C1B N11B N12B 70.7(12) . . N21B C1B N11B C15B -100.8(13) . . N21B N22B C23B C24B 0.3(12) . . N21B N22B C23B C26B 178.5(10) . . N21C C1 N11C N12C -68.4(12) . . N21C C1 N11C C15 106.3(12) . . N21C N22C C23 C24 0.2(11) . . N21C N22C C23 C26 -178.1(10) . . N22A N21A C25A C24A -0.7(13) . . N22A N21A C25A C27A -179.5(10) . . N22A C23A C24A C25A 0.9(13) . . N22A C23A C24A C41A 178.6(11) . . N22B N21B C25B C24B -0.9(12) . . N22B N21B C25B C27B -179.2(10) . . N22B C23B C24B C25B -0.9(13) . . N22B C23B C24B C41B -178.5(10) . . N22C N21C C25 C24 1.2(11) . . N22C N21C C25 C27 179.7(9) . . N22C C23 C24 C25 0.4(12) . . N22C C23 C24 C41C 177.9(10) . . C23A C24A C25A N21A -0.1(13) . . C23A C24A C25A C27A 178.6(12) . . C23A C24A C41A C42A -47.2(19) . . C23A C24A C41A C46A 133.3(12) . . C23B C24B C25B N21B 1.1(12) . . C23B C24B C25B C27B 179.2(11) . . C23B C24B C41B C42B -123.9(12) . . C23B C24B C41B C46B 52.3(16) . . C23 C24 C25 N21C -0.9(11) . . C23 C24 C25 C27 -179.4(11) . . C23 C24 C41C C42C -48.8(16) . . C23 C24 C41C C46C 125.6(12) . . C24A C41A C42A C43A -178.1(12) . . C24A C41A C46A C45A 177.1(11) . . C24B C41B C42B C43B 178.6(10) . . C24B C41B C46B C45B -176.1(10) . . C24 C41C C42C C43C 175.9(11) . . C24 C41C C46C C45C -176.1(10) . . C25A N21A N22A C23A 1.2(12) . . C25A C24A C41A C42A 129.9(13) . . C25A C24A C41A C46A -49.5(18) . . C25B N21B N22B Mn2 -165.3(7) . 1_565 C25B N21B N22B C23B 0.4(12) . . C25B C24B C41B C42B 59.1(17) . . C25B C24B C41B C46B -124.7(13) . . C25 N21C N22C Mn4 161.4(7) . 1_565 C25 N21C N22C C23 -0.9(11) . . C25 C24 C41C C42C 128.1(12) . . C25 C24 C41C C46C -57.5(17) . . C26A C23A C24A C25A 177.2(11) . . C26A C23A C24A C41A -5(2) . . C26B C23B C24B C25B -178.9(11) . . C26B C23B C24B C41B 3.4(18) . . C26 C23 C24 C25 178.7(11) . . C26 C23 C24 C41C -3.8(18) . . C31A C14A C15A N11A -179.2(10) . . C31A C14A C15A C17A 4.6(19) . . C31A C32A C33A C34A 2(2) . . C31B C14B C15B N11B -177.4(10) . . C31B C14B C15B C17B 4.7(19) . . C31B C32B C33B C34B 0.7(16) . . C31C C14 C15 N11C 175.1(11) . . C31C C14 C15 C17 -8(2) . . C31C C32C C33C C34C 1.4(16) . . C32A C31A C36A C35A -2.2(19) . . C32A C33A C34A C35A -4(2) . . C32A C33A C34A C37A 176.9(13) . . C32B C31B C36B C35B 0.5(16) . . C32B C33B C34B C35B -2.6(15) . . C32B C33B C34B C37B -179.8(9) . . C32C C31C C36C C35C -1.3(16) . . C32C C33C C34C C35C -1.8(16) . . C32C C33C C34C C37C 179.8(10) . . C33A C34A C35A C36A 2.1(19) . . C33A C34A C37A O38A 9.5(17) . . C33A C34A C37A O39A -170.7(12) . . C33B C34B C35B C36B 3.5(16) . . C33B C34B C37B O38B -29.2(14) . . C33B C34B C37B O39B 156.1(10) . . C33C C34C C35C C36C 0.6(16) . . C33C C34C C37C O38C -151.9(10) . . C33C C34C C37C O39C 27.4(14) . . C34A C35A C36A C31A 0.8(18) . . C34A C37A O38A Mn3 179.8(8) . . C34A C37A O39A Mn4 -173.4(7) . . C34B C35B C36B C31B -2.4(16) . . C34B C37B O38B Mn1 141.7(9) . . C34B C37B O39B Mn2 -161.9(7) . . C34C C35C C36C C31C 1.0(16) . . C34C C37C O38C Mn3 -142.6(9) . . C34C C37C O39C Mn4 160.8(7) . . C35A C34A C37A O38A -170.0(11) . . C35A C34A C37A O39A 9.8(17) . . C35B C34B C37B O38B 153.7(10) . . C35B C34B C37B O39B -21.0(15) . . C35C C34C C37C O38C 29.7(15) . . C35C C34C C37C O39C -151.0(10) . . C36A C31A C32A C33A 1(2) . . C36B C31B C32B C33B 0.3(16) . . C36C C31C C32C C33C 0.2(16) . . C37A C34A C35A C36A -178.4(11) . . C37B C34B C35B C36B -179.5(9) . . C37C C34C C35C C36C 179.0(9) . . O38A C37A O39A Mn4 6.4(17) . . O38B C37B O39B Mn2 23.9(15) . . O38C C37C O39C Mn4 -19.9(15) . . O39A C37A O38A Mn3 0(2) . . O39B C37B O38B Mn1 -44.1(19) . . O39C C37C O38C Mn3 38.2(18) . . C41A C24A C25A N21A -177.8(11) . . C41A C24A C25A C27A 1(2) . . C41A C42A C43A C44A 0.8(19) . . C41B C24B C25B N21B 178.6(11) . . C41B C24B C25B C27B -3(2) . . C41B C42B C43B C44B -5.0(16) . . C41C C24 C25 N21C -178.3(10) . . C41C C24 C25 C27 3.2(19) . . C41C C42C C43C C44C -1.8(18) . . C42A C41A C46A C45A -2.3(18) . . C42A C43A C44A C45A -2.0(18) . . C42A C43A C44A C47A -179.3(11) . . C42B C41B C46B C45B 0.1(17) . . C42B C43B C44B C45B 4.8(16) . . C42B C43B C44B C47B -177.0(9) . . C42C C41C C46C C45C -1.7(17) . . C42C C43C C44C C45C 2.6(17) . . C42C C43C C44C C47C -179.4(10) . . C43A C44A C45A C46A 1.0(19) . . C43A C44A C47A O48A 2.3(16) . . C43A C44A C47A O49A -179.9(10) . . C43B C44B C45B C46B -2.2(16) . . C43B C44B C47B O48B -11.1(15) . . C43B C44B C47B O49B 167.4(9) . . C43C C44C C45C C46C -2.9(16) . . C43C C44C C47C O48C 11.5(14) . . C43C C44C C47C O49C -167.9(10) . . C44A C45A C46A C41A 1.2(19) . . C44A C47A O48A Mn2 165.9(7) . . C44A C47A O49A Mn1 -176.4(8) . . C44B C45B C46B C41B -0.3(17) . . C44B C47B O48B Mn2 -174.1(8) . 1_665 C44B C47B O49B Mn1 -61.6(12) . 1_665 C44B C47B O49B Mn2 173.1(7) . 1_665 C44C C45C C46C C41C 2.4(17) . . C44C C47C O48C Mn3 66.2(12) . 1_665 C44C C47C O48C Mn4 -174.4(8) . 1_665 C44C C47C O49C Mn4 174.8(9) . 1_665 C45A C44A C47A O48A -174.9(11) . . C45A C44A C47A O49A 2.8(16) . . C45B C44B C47B O48B 167.1(10) . . C45B C44B C47B O49B -14.4(14) . . C45C C44C C47C O48C -170.5(9) . . C45C C44C C47C O49C 10.1(15) . . C46A C41A C42A C43A 1.4(18) . . C46B C41B C42B C43B 2.5(16) . . C46C C41C C42C C43C 1.3(17) . . C47A C44A C45A C46A 178.3(11) . . C47B C44B C45B C46B 179.5(10) . . C47C C44C C45C C46C 179.1(10) . . O48A C47A O49A Mn1 1(2) . . O48B C47B O49B Mn1 116.8(10) . 1_665 O48B C47B O49B Mn2 -8.5(10) . 1_665 O48C C47C O49C Mn4 -4.7(10) . 1_665 O49A C47A O48A Mn2 -11.6(16) . . O49B C47B O48B Mn2 7.5(9) . 1_665 O49C C47C O48C Mn3 -114.4(11) . 1_665 O49C C47C O48C Mn4 5.0(10) . 1_665 C61 C62 C63 C64 -2(2) . . C62 C61 C66 C65 2(2) . . C62 C63 C64 C65 2(2) . . C62 C63 C64 C68 180.0(14) . . C63 C64 C65 C66 -0.3(18) . . C64 C65 C66 C61 -2(2) . . C66 C61 C62 C63 -0.6(19) . . C67 C61 C62 C63 -176.8(13) . . C67 C61 C66 C65 178.3(13) . . C68 C64 C65 C66 -178.4(12) . . C71 C72 C73 C74 0(2) . . C72 C71 C76 C75 1(2) . . C72 C73 C74 C75 0(2) . . C72 C73 C74 C78 179.6(15) . . C73 C74 C75 C76 1(2) . . C74 C75 C76 C71 -1(2) . . C76 C71 C72 C73 0(2) . . C77 C71 C72 C73 178.2(13) . . C77 C71 C76 C75 -177.5(13) . . C78 C74 C75 C76 -179.0(15) . . C81 C82 C83 C84 -1(2) . . C82 C81 C86 C85 2(2) . . C82 C83 C84 C85 3(2) . . C82 C83 C84 C88 176.1(14) . . C83 C84 C85 C86 -1(2) . . C84 C85 C86 C81 -1(2) . . C86 C81 C82 C83 -1(2) . . C87 C81 C82 C83 -176.8(15) . . C87 C81 C86 C85 178.0(15) . . C88 C84 C85 C86 -175.0(14) . . C96 C91 C92 C96 2.3(19) . 2_645 C92 C96 C91 C97 179.3(11) 2_645 . C92 C96 C91 C92 -2(2) 2_645 . C103 C102 C101 C103 2(3) . 2_646 C103 C102 C101 C107 -178.8(16) . . C101 C103 C102 C101 -2(3) 2_646 .