#------------------------------------------------------------------------------ #$Date: 2019-02-22 01:09:21 +0200 (Fri, 22 Feb 2019) $ #$Revision: 213770 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/30/7123039.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_7123039 loop_ _publ_author_name 'Sarbajna, Abir' 'Patil, Pradnya H.' 'Dinh, Minh Hoan' 'Gladkovskaya, Olga' 'Fayzullin, Robert R.' 'Lapointe, S\'ebastien' 'Khaskin, Eugene' 'Khusnutdinova, Julia R.' _publ_section_title ; Facile and reversible double dearomatization of pyridines in non-phosphine MnI complexes with N,S-donor pyridinophane ligand ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC00424F _journal_year 2019 _chemical_formula_moiety 'C28 H12 D24 K Mn N2 O5 S2' _chemical_formula_sum 'C28 H12 D24 K Mn N2 O5 S2' _chemical_formula_weight 662.89 _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 mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2018-12-30 deposited with the CCDC. 2019-02-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.431(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.3544(2) _cell_length_b 16.4310(4) _cell_length_c 19.2887(5) _cell_measurement_reflns_used 13914 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 29.1650 _cell_measurement_theta_min 2.3750 _cell_volume 2955.85(12) _computing_cell_refinement 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_molecular_graphics ; WinGX (Farrugia, 2012); Olex2 (Dolomanov et al., 2009); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009) ; _computing_publication_material 'enCIFer (Allen, 2004)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)' _diffrn_ambient_temperature 93(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'XtaLAB Pro: Kappa dual offset/far' _diffrn_measurement_method '\w scans' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 52162 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.000 _diffrn_reflns_theta_min 2.352 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015). Numerical absorption correction based on gaussian integration over a multifaceted crystal model. Empirical absorption correction using spherical harmonics, frame scaling and detector area scaling, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.490 _exptl_crystal_description plate _exptl_crystal_F_000 1336 _exptl_crystal_recrystallization_method 'vapor diffusion of pentane into a THF-d8 solution at -30 \%C' _exptl_crystal_size_max 0.409 _exptl_crystal_size_mid 0.123 _exptl_crystal_size_min 0.061 _refine_diff_density_max 1.404 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.075 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 416 _refine_ls_number_reflns 6427 _refine_ls_number_restraints 211 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0460 _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^)+(0.0384P)^2^+5.3215P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1076 _refine_ls_wR_factor_ref 0.1123 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5519 _reflns_number_total 6427 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc00424f2.cif _cod_data_source_block jk330 _cod_original_cell_volume 2955.84(13) _cod_database_code 7123039 _shelx_shelxl_version_number 2018/3 _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 0.744 _shelx_estimated_absorpt_t_max 0.955 _shelx_res_file ; TITL jk330 in P2(1)/n shelx.res created by SHELXL-2018/3 at 20:07:13 on 29-Dec-2018 CELL 0.71073 9.354373 16.430997 19.288678 90.0000 94.4309 90.0000 ZERR 4.00 0.000204 0.000379 0.000538 0.0000 0.0023 0.0000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H D N O S K MN UNIT 112 48 96 8 20 8 4 4 MERG 2 OMIT -2.00 54.00 OMIT 2 2 2 OMIT 2 0 4 SIMU 0.02 O4 > C57 SADI C11 H11 C27 H27 EQIV $1 x+1, y, z BIND MN1 K1_$1 MORE -1 FMAP 2 PLAN 20 SIZE 0.061 0.123 0.409 ACTA BOND $H CONF LIST 4 L.S. 20 TEMP -180.15 WGHT 0.038400 5.321500 FVAR 0.26764 0.78473 0.64618 MN1 8 0.594916 0.281702 0.258780 11.00000 0.01397 0.02275 = 0.01800 -0.00279 -0.00151 0.00252 S1 6 0.577651 0.419637 0.251591 11.00000 0.03078 0.02406 = 0.02462 0.00201 -0.00025 0.00907 S2 6 0.678713 0.152399 0.278684 11.00000 0.02242 0.01946 = 0.02866 -0.00330 -0.00206 -0.00344 O1 5 0.321112 0.248787 0.318968 11.00000 0.02070 0.05434 = 0.04784 -0.00498 0.00718 -0.00404 O2 5 0.437252 0.259858 0.122247 11.00000 0.05002 0.08669 = 0.02982 -0.01883 -0.01747 0.01730 N2 4 0.790074 0.299969 0.219902 11.00000 0.02037 0.02360 = 0.02034 -0.00257 0.00276 0.00093 N1 4 0.698876 0.304077 0.353979 11.00000 0.01350 0.02160 = 0.01706 -0.00161 -0.00001 0.00062 C1 1 0.430451 0.263439 0.295399 11.00000 0.01934 0.03380 = 0.02781 -0.00570 -0.00228 -0.00014 C2 1 0.503147 0.266764 0.175514 11.00000 0.02533 0.04093 = 0.02712 -0.00788 -0.00200 0.00784 C11 1 0.675247 0.445572 0.328724 11.00000 0.02996 0.02110 = 0.02969 -0.00321 0.00056 -0.00042 H11 2 0.685499 0.499172 0.339795 11.00000 0.03110 C12 1 0.725749 0.384007 0.373101 11.00000 0.01604 0.02336 = 0.02251 -0.00258 0.00353 -0.00083 C13 1 0.803711 0.399177 0.438960 11.00000 0.02279 0.02972 = 0.02515 -0.00828 0.00104 -0.00461 AFIX 43 H13 2 0.827172 0.453452 0.452467 11.00000 -1.20000 AFIX 0 C14 1 0.844228 0.336382 0.482163 11.00000 0.01948 0.04151 = 0.02173 -0.00643 -0.00265 0.00137 AFIX 43 H14 2 0.894791 0.347118 0.525823 11.00000 -1.20000 AFIX 0 C15 1 0.811491 0.255550 0.462397 11.00000 0.01968 0.03320 = 0.02000 0.00390 0.00114 0.00572 AFIX 43 H15 2 0.838746 0.211254 0.492197 11.00000 -1.20000 AFIX 0 C16 1 0.738433 0.242746 0.398247 11.00000 0.01521 0.02344 = 0.02132 -0.00039 0.00305 0.00063 C17 1 0.695315 0.159197 0.373405 11.00000 0.03172 0.02404 = 0.02777 0.00127 0.00150 0.00313 AFIX 23 H17A 2 0.602396 0.144762 0.391478 11.00000 -1.20000 H17B 2 0.767717 0.119376 0.392184 11.00000 -1.20000 AFIX 0 C21 1 0.700506 0.432367 0.183714 11.00000 0.04384 0.03219 = 0.03087 0.00762 0.01333 0.00425 AFIX 23 H21A 2 0.648037 0.423958 0.137710 11.00000 -1.20000 H21B 2 0.738595 0.488607 0.185229 11.00000 -1.20000 AFIX 0 C22 1 0.823337 0.372927 0.192576 11.00000 0.03483 0.02777 = 0.02911 0.00119 0.01157 -0.00106 C23 1 0.956349 0.390902 0.171368 11.00000 0.04360 0.03487 = 0.04281 0.00278 0.01598 -0.00631 AFIX 43 H23 2 0.976786 0.442909 0.153017 11.00000 -1.20000 AFIX 0 C24 1 1.061316 0.329593 0.177767 11.00000 0.02795 0.05001 = 0.04085 -0.00156 0.01211 -0.00949 AFIX 43 H24 2 1.154771 0.340398 0.163974 11.00000 -1.20000 AFIX 0 C25 1 1.031006 0.255238 0.203360 11.00000 0.02181 0.04217 = 0.03467 -0.00523 0.00349 0.00428 AFIX 43 H25 2 1.102583 0.214103 0.206324 11.00000 -1.20000 AFIX 0 C26 1 0.890492 0.238153 0.226164 11.00000 0.02034 0.02913 = 0.02393 -0.00275 0.00086 0.00362 C27 1 0.854413 0.165896 0.255326 11.00000 0.02427 0.02548 = 0.03671 -0.00300 0.00398 0.00697 H27 2 0.907382 0.119612 0.256635 11.00000 0.04660 K1 7 0.064210 0.284833 0.370232 11.00000 0.01662 0.03185 = 0.03215 -0.00241 0.00208 -0.00285 O3 5 0.233908 0.292140 0.490720 11.00000 0.03723 0.03744 = 0.05785 -0.01807 -0.01795 0.00541 C31 1 0.234669 0.356730 0.540314 11.00000 0.02718 0.04314 = 0.05383 -0.01606 0.00650 -0.00400 AFIX 23 D31A 3 0.192517 0.338278 0.583140 11.00000 -1.20000 D31B 3 0.178420 0.403608 0.520887 11.00000 -1.20000 AFIX 0 C32 1 0.391290 0.380681 0.556215 11.00000 0.02825 0.04532 = 0.04740 -0.01408 -0.00211 -0.00396 AFIX 23 D32A 3 0.408128 0.437390 0.541536 11.00000 -1.20000 D32B 3 0.419822 0.375494 0.606523 11.00000 -1.20000 AFIX 0 C33 1 0.473622 0.321045 0.514316 11.00000 0.03265 0.06443 = 0.04456 -0.00745 0.00703 0.00801 AFIX 23 D33A 3 0.497822 0.345189 0.469677 11.00000 -1.20000 D33B 3 0.562785 0.302748 0.540738 11.00000 -1.20000 AFIX 0 C34 1 0.369652 0.253173 0.502972 11.00000 0.04824 0.05072 = 0.04557 -0.01412 -0.01000 0.01659 AFIX 23 D34A 3 0.391896 0.219935 0.462370 11.00000 -1.20000 D34B 3 0.371139 0.217644 0.544474 11.00000 -1.20000 AFIX 0 SAME O4 C41 C45 > C47 O4 5 0.136196 0.444876 0.373003 11.00000 0.02665 0.04057 = 0.07216 0.02167 0.00636 -0.00498 C41 1 0.054170 0.508614 0.340609 11.00000 0.02330 0.03874 = 0.07184 0.01322 0.00423 -0.00304 PART 1 AFIX 23 D41A 3 0.026286 0.548992 0.375193 21.00000 -1.20000 D41B 3 -0.033358 0.487306 0.314663 21.00000 -1.20000 AFIX 23 PART 2 D41C 3 -0.015194 0.529778 0.372425 -21.00000 -1.20000 D41D 3 0.000187 0.488511 0.297846 -21.00000 -1.20000 AFIX 0 PART 1 C42 1 0.158064 0.546493 0.290564 21.00000 0.02879 0.04268 = 0.05258 0.02029 0.00080 -0.00251 AFIX 23 D42A 3 0.168479 0.511846 0.249267 21.00000 -1.20000 D42B 3 0.128200 0.601960 0.275543 21.00000 -1.20000 AFIX 0 C43 1 0.295129 0.547434 0.339940 21.00000 0.02210 0.03200 = 0.04281 -0.00847 0.00602 -0.00447 AFIX 23 D43A 3 0.381755 0.547730 0.313523 21.00000 -1.20000 D43B 3 0.297343 0.595668 0.370762 21.00000 -1.20000 AFIX 0 C44 1 0.286237 0.471431 0.380472 21.00000 0.02468 0.05088 = 0.04794 0.01632 -0.00527 -0.00846 AFIX 23 D44A 3 0.349149 0.429190 0.362478 21.00000 -1.20000 D44B 3 0.316871 0.481356 0.430029 21.00000 -1.20000 AFIX 0 PART 2 C45 1 0.155506 0.574109 0.323158 -21.00000 0.02728 0.03058 = 0.04556 0.00157 0.01422 0.00571 AFIX 23 D45A 3 0.159891 0.617586 0.358793 -21.00000 -1.20000 D45B 3 0.126456 0.598348 0.277229 -21.00000 -1.20000 AFIX 0 C46 1 0.297691 0.531281 0.322090 -21.00000 0.03149 0.05159 = 0.05573 0.01176 0.01710 0.00455 AFIX 23 D46A 3 0.334681 0.535624 0.275510 -21.00000 -1.20000 D46B 3 0.368770 0.555636 0.356734 -21.00000 -1.20000 AFIX 0 C47 1 0.271659 0.446262 0.339152 -21.00000 0.02283 0.03652 = 0.06719 -0.00030 0.00366 0.00263 AFIX 23 D47A 3 0.350973 0.424825 0.370936 -21.00000 -1.20000 D47B 3 0.263833 0.412601 0.296459 -21.00000 -1.20000 AFIX 0 PART 0 SAME O5 C51 C55 > C57 O5 5 0.107835 0.126289 0.413900 11.00000 0.05867 0.03808 = 0.04590 -0.00171 -0.00740 0.00882 C51 1 0.112174 0.100443 0.483610 11.00000 0.06112 0.03609 = 0.05486 0.00674 0.02206 0.00967 PART 1 AFIX 23 D51A 3 0.017837 0.078675 0.494561 31.00000 -1.20000 D51B 3 0.138137 0.146202 0.515524 31.00000 -1.20000 AFIX 23 PART 2 D51C 3 0.026045 0.068034 0.492122 -31.00000 -1.20000 D51D 3 0.118148 0.147574 0.515679 -31.00000 -1.20000 AFIX 0 PART 1 C52 1 0.226646 0.033849 0.490551 31.00000 0.07731 0.03618 = 0.04916 0.00497 -0.00315 0.01929 AFIX 23 D52A 3 0.322291 0.057286 0.503984 31.00000 -1.20000 D52B 3 0.203604 -0.007007 0.525728 31.00000 -1.20000 AFIX 0 C53 1 0.222626 -0.003243 0.420073 31.00000 0.04864 0.03375 = 0.05625 -0.00811 0.01486 0.00533 AFIX 23 D53A 3 0.150061 -0.047089 0.414488 31.00000 -1.20000 D53B 3 0.317461 -0.025207 0.410149 31.00000 -1.20000 AFIX 0 C54 1 0.181286 0.069120 0.374340 31.00000 0.07833 0.03863 = 0.04352 -0.01220 0.00001 -0.01407 AFIX 23 D54A 3 0.268230 0.094438 0.357550 31.00000 -1.20000 D54B 3 0.118556 0.051335 0.333457 31.00000 -1.20000 AFIX 0 PART 2 C55 1 0.248097 0.048194 0.493125 -31.00000 0.07290 0.03332 = 0.05712 -0.00549 0.00952 0.01254 AFIX 23 D55A 3 0.327872 0.078491 0.518032 -31.00000 -1.20000 D55B 3 0.230548 -0.002567 0.518783 -31.00000 -1.20000 AFIX 0 C56 1 0.278489 0.030920 0.420457 -31.00000 0.06879 0.04695 = 0.06780 -0.00983 0.01431 0.01221 AFIX 23 D56A 3 0.295647 -0.027951 0.413992 -31.00000 -1.20000 D56B 3 0.364135 0.061381 0.407979 -31.00000 -1.20000 AFIX 0 C57 1 0.146056 0.058393 0.375907 -31.00000 0.08076 0.03120 = 0.05374 -0.01625 -0.00604 -0.00951 AFIX 23 D57A 3 0.169098 0.073337 0.328313 -31.00000 -1.20000 D57B 3 0.070037 0.016342 0.373374 -31.00000 -1.20000 PART 0 AFIX 0 HKLF 4 REM jk330 in P2(1)/n REM wR2 = 0.1123, GooF = S = 1.076, Restrained GooF = 1.067 for all data REM R1 = 0.0460 for 5519 Fo > 4sig(Fo) and 0.0561 for all 6427 data REM 416 parameters refined using 211 restraints END WGHT 0.0384 5.3216 REM Highest difference peak 1.404, deepest hole -0.574, 1-sigma level 0.075 Q1 1 0.6550 0.4362 0.2363 11.00000 0.05 1.40 Q2 1 0.3907 0.4177 0.5212 11.00000 0.05 0.63 Q3 1 0.7868 0.1442 0.2276 11.00000 0.05 0.59 Q4 1 0.3185 0.3084 0.3097 11.00000 0.05 0.52 Q5 1 0.2966 0.2921 0.4589 11.00000 0.05 0.52 Q6 1 0.8048 0.4352 0.2139 11.00000 0.05 0.50 Q7 1 0.5936 0.2963 0.2126 11.00000 0.05 0.50 Q8 1 0.4127 0.2880 0.4668 11.00000 0.05 0.49 Q9 1 0.1157 0.4407 0.3287 11.00000 0.05 0.46 Q10 1 0.6028 0.1731 0.2892 11.00000 0.05 0.46 Q11 1 0.0628 0.2984 0.3254 11.00000 0.05 0.46 Q12 1 0.6617 0.1594 0.3301 11.00000 0.05 0.45 Q13 1 0.2362 0.3958 0.5054 11.00000 0.05 0.43 Q14 1 0.7414 0.2022 0.3727 11.00000 0.05 0.41 Q15 1 0.0714 0.2446 0.3521 11.00000 0.05 0.37 Q16 1 1.0260 0.3717 0.2024 11.00000 0.05 0.37 Q17 1 0.6014 0.2843 0.3129 11.00000 0.05 0.37 Q18 1 0.2270 0.2731 0.5480 11.00000 0.05 0.36 Q19 1 0.6011 0.3270 0.2843 11.00000 0.05 0.35 Q20 1 0.4661 0.2746 0.5481 11.00000 0.05 0.35 ; _shelx_res_checksum 74106 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.59492(4) 0.28170(2) 0.25878(2) 0.01838(11) Uani 1 1 d . . . . . S1 S 0.57765(7) 0.41964(4) 0.25159(3) 0.02661(16) Uani 1 1 d . . . . . S2 S 0.67871(7) 0.15240(4) 0.27868(3) 0.02372(15) Uani 1 1 d . . . . . O1 O 0.3211(2) 0.24879(15) 0.31897(12) 0.0407(5) Uani 1 1 d . . . . . O2 O 0.4373(3) 0.25986(19) 0.12225(12) 0.0566(7) Uani 1 1 d . . . . . N2 N 0.7901(2) 0.29997(13) 0.21990(11) 0.0214(4) Uani 1 1 d . . . . . N1 N 0.6989(2) 0.30408(12) 0.35398(10) 0.0174(4) Uani 1 1 d . . . . . C1 C 0.4305(3) 0.26344(17) 0.29540(14) 0.0272(6) Uani 1 1 d . . . . . C2 C 0.5031(3) 0.26676(19) 0.17551(15) 0.0313(6) Uani 1 1 d . . . . . C11 C 0.6752(3) 0.44557(17) 0.32872(15) 0.0270(6) Uani 1 1 d D . . . . H11 H 0.685(3) 0.4992(17) 0.3398(17) 0.031(8) Uiso 1 1 d D . . . . C12 C 0.7257(3) 0.38401(16) 0.37310(13) 0.0205(5) Uani 1 1 d . . . . . C13 C 0.8037(3) 0.39918(17) 0.43896(14) 0.0259(6) Uani 1 1 d . . . . . H13 H 0.827172 0.453452 0.452467 0.031 Uiso 1 1 calc R U . . . C14 C 0.8442(3) 0.33638(18) 0.48216(14) 0.0278(6) Uani 1 1 d . . . . . H14 H 0.894791 0.347118 0.525823 0.033 Uiso 1 1 calc R U . . . C15 C 0.8115(3) 0.25555(17) 0.46240(13) 0.0243(5) Uani 1 1 d . . . . . H15 H 0.838746 0.211254 0.492197 0.029 Uiso 1 1 calc R U . . . C16 C 0.7384(3) 0.24275(15) 0.39825(13) 0.0199(5) Uani 1 1 d . . . . . C17 C 0.6953(3) 0.15920(16) 0.37341(14) 0.0279(6) Uani 1 1 d . . . . . H17A H 0.602396 0.144762 0.391478 0.033 Uiso 1 1 calc R U . . . H17B H 0.767717 0.119376 0.392184 0.033 Uiso 1 1 calc R U . . . C21 C 0.7005(3) 0.43237(19) 0.18371(16) 0.0351(7) Uani 1 1 d . . . . . H21A H 0.648037 0.423958 0.137710 0.042 Uiso 1 1 calc R U . . . H21B H 0.738595 0.488607 0.185229 0.042 Uiso 1 1 calc R U . . . C22 C 0.8233(3) 0.37293(17) 0.19258(15) 0.0301(6) Uani 1 1 d . . . . . C23 C 0.9563(4) 0.3909(2) 0.17137(17) 0.0398(7) Uani 1 1 d . . . . . H23 H 0.976786 0.442909 0.153017 0.048 Uiso 1 1 calc R U . . . C24 C 1.0613(3) 0.3296(2) 0.17777(17) 0.0391(7) Uani 1 1 d . . . . . H24 H 1.154771 0.340398 0.163974 0.047 Uiso 1 1 calc R U . . . C25 C 1.0310(3) 0.2552(2) 0.20336(15) 0.0328(6) Uani 1 1 d . . . . . H25 H 1.102583 0.214103 0.206324 0.039 Uiso 1 1 calc R U . . . C26 C 0.8905(3) 0.23815(17) 0.22616(14) 0.0245(5) Uani 1 1 d . . . . . C27 C 0.8544(3) 0.16590(17) 0.25533(15) 0.0287(6) Uani 1 1 d D . . . . H27 H 0.907(4) 0.1196(19) 0.2566(19) 0.047(10) Uiso 1 1 d D . . . . K1 K 0.06421(6) 0.28483(4) 0.37023(3) 0.02686(14) Uani 1 1 d . . . . . O3 O 0.2339(2) 0.29214(14) 0.49072(13) 0.0453(6) Uani 1 1 d . . . . . C31 C 0.2347(3) 0.3567(2) 0.54031(19) 0.0412(8) Uani 1 1 d . . . . . D31A D 0.192517 0.338278 0.583140 0.049 Uiso 1 1 calc R U . . . D31B D 0.178420 0.403608 0.520887 0.049 Uiso 1 1 calc R U . . . C32 C 0.3913(3) 0.3807(2) 0.55621(18) 0.0406(7) Uani 1 1 d . . . . . D32A D 0.408128 0.437390 0.541536 0.049 Uiso 1 1 calc R U . . . D32B D 0.419822 0.375494 0.606523 0.049 Uiso 1 1 calc R U . . . C33 C 0.4736(4) 0.3210(2) 0.51432(19) 0.0470(8) Uani 1 1 d . . . . . D33A D 0.497822 0.345189 0.469677 0.056 Uiso 1 1 calc R U . . . D33B D 0.562785 0.302748 0.540738 0.056 Uiso 1 1 calc R U . . . C34 C 0.3697(4) 0.2532(2) 0.5030(2) 0.0489(9) Uani 1 1 d . . . . . D34A D 0.391896 0.219935 0.462370 0.059 Uiso 1 1 calc R U . . . D34B D 0.371139 0.217644 0.544474 0.059 Uiso 1 1 calc R U . . . O4 O 0.1362(2) 0.44488(14) 0.37300(14) 0.0463(6) Uani 1 1 d D U . . . C41 C 0.0542(3) 0.5086(2) 0.3406(2) 0.0446(8) Uani 1 1 d D U . . . D41A D 0.026286 0.548992 0.375193 0.054 Uiso 0.785(9) 1 calc R U P A 1 D41B D -0.033358 0.487306 0.314663 0.054 Uiso 0.785(9) 1 calc R U P A 1 D41C D -0.015194 0.529778 0.372425 0.054 Uiso 0.215(9) 1 calc R U P A 2 D41D D 0.000187 0.488511 0.297846 0.054 Uiso 0.215(9) 1 calc R U P A 2 C42 C 0.1581(5) 0.5465(4) 0.2906(3) 0.0415(13) Uani 0.785(9) 1 d D U P A 1 D42A D 0.168479 0.511846 0.249267 0.050 Uiso 0.785(9) 1 calc R U P A 1 D42B D 0.128200 0.601960 0.275543 0.050 Uiso 0.785(9) 1 calc R U P A 1 C43 C 0.2951(5) 0.5474(3) 0.3399(3) 0.0321(12) Uani 0.785(9) 1 d D U P A 1 D43A D 0.381755 0.547730 0.313523 0.039 Uiso 0.785(9) 1 calc R U P A 1 D43B D 0.297343 0.595668 0.370762 0.039 Uiso 0.785(9) 1 calc R U P A 1 C44 C 0.2862(4) 0.4714(3) 0.3805(3) 0.0416(13) Uani 0.785(9) 1 d D U P A 1 D44A D 0.349149 0.429190 0.362478 0.050 Uiso 0.785(9) 1 calc R U P A 1 D44B D 0.316871 0.481356 0.430029 0.050 Uiso 0.785(9) 1 calc R U P A 1 C45 C 0.1555(14) 0.5741(8) 0.3232(11) 0.034(3) Uani 0.215(9) 1 d D U P A 2 D45A D 0.159891 0.617586 0.358793 0.041 Uiso 0.215(9) 1 calc R U P A 2 D45B D 0.126456 0.598348 0.277229 0.041 Uiso 0.215(9) 1 calc R U P A 2 C46 C 0.2977(19) 0.5313(11) 0.3221(15) 0.046(4) Uani 0.215(9) 1 d D U P A 2 D46A D 0.334681 0.535624 0.275510 0.055 Uiso 0.215(9) 1 calc R U P A 2 D46B D 0.368770 0.555636 0.356734 0.055 Uiso 0.215(9) 1 calc R U P A 2 C47 C 0.2717(15) 0.4463(9) 0.3392(12) 0.042(4) Uani 0.215(9) 1 d D U P A 2 D47A D 0.350973 0.424825 0.370936 0.051 Uiso 0.215(9) 1 calc R U P A 2 D47B D 0.263833 0.412601 0.296459 0.051 Uiso 0.215(9) 1 calc R U P A 2 O5 O 0.1078(3) 0.12629(14) 0.41390(13) 0.0481(6) Uani 1 1 d D U . . . C51 C 0.1122(4) 0.1004(2) 0.4836(2) 0.0498(9) Uani 1 1 d D U . . . D51A D 0.017837 0.078675 0.494561 0.060 Uiso 0.646(16) 1 calc R U P B 1 D51B D 0.138137 0.146202 0.515524 0.060 Uiso 0.646(16) 1 calc R U P B 1 D51C D 0.026045 0.068034 0.492122 0.060 Uiso 0.354(16) 1 calc R U P B 2 D51D D 0.118148 0.147574 0.515679 0.060 Uiso 0.354(16) 1 calc R U P B 2 C52 C 0.2266(15) 0.0338(8) 0.4906(5) 0.055(3) Uani 0.646(16) 1 d D U P B 1 D52A D 0.322291 0.057286 0.503984 0.066 Uiso 0.646(16) 1 calc R U P B 1 D52B D 0.203604 -0.007007 0.525728 0.066 Uiso 0.646(16) 1 calc R U P B 1 C53 C 0.2226(9) -0.0032(4) 0.4201(3) 0.0457(18) Uani 0.646(16) 1 d D U P B 1 D53A D 0.150061 -0.047089 0.414488 0.055 Uiso 0.646(16) 1 calc R U P B 1 D53B D 0.317461 -0.025207 0.410149 0.055 Uiso 0.646(16) 1 calc R U P B 1 C54 C 0.1813(13) 0.0691(6) 0.3743(5) 0.054(3) Uani 0.646(16) 1 d D U P B 1 D54A D 0.268230 0.094438 0.357550 0.064 Uiso 0.646(16) 1 calc R U P B 1 D54B D 0.118556 0.051335 0.333457 0.064 Uiso 0.646(16) 1 calc R U P B 1 C55 C 0.248(3) 0.0482(17) 0.4931(8) 0.054(5) Uani 0.354(16) 1 d D U P B 2 D55A D 0.327872 0.078491 0.518032 0.065 Uiso 0.354(16) 1 calc R U P B 2 D55B D 0.230548 -0.002567 0.518783 0.065 Uiso 0.354(16) 1 calc R U P B 2 C56 C 0.2785(18) 0.0309(11) 0.4205(7) 0.061(3) Uani 0.354(16) 1 d D U P B 2 D56A D 0.295647 -0.027951 0.413992 0.073 Uiso 0.354(16) 1 calc R U P B 2 D56B D 0.364135 0.061381 0.407979 0.073 Uiso 0.354(16) 1 calc R U P B 2 C57 C 0.146(2) 0.0584(12) 0.3759(9) 0.056(4) Uani 0.354(16) 1 d D U P B 2 D57A D 0.169098 0.073337 0.328313 0.067 Uiso 0.354(16) 1 calc R U P B 2 D57B D 0.070037 0.016342 0.373374 0.067 Uiso 0.354(16) 1 calc R U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01397(18) 0.0227(2) 0.01800(19) -0.00279(14) -0.00151(13) 0.00252(14) S1 0.0308(4) 0.0241(3) 0.0246(3) 0.0020(3) -0.0002(3) 0.0091(3) S2 0.0224(3) 0.0195(3) 0.0287(3) -0.0033(2) -0.0021(2) -0.0034(2) O1 0.0207(10) 0.0543(14) 0.0478(13) -0.0050(11) 0.0072(9) -0.0040(9) O2 0.0500(15) 0.087(2) 0.0298(12) -0.0188(13) -0.0175(11) 0.0173(14) N2 0.0204(10) 0.0236(11) 0.0203(10) -0.0026(8) 0.0028(8) 0.0009(8) N1 0.0135(9) 0.0216(10) 0.0171(10) -0.0016(8) 0.0000(7) 0.0006(8) C1 0.0193(13) 0.0338(15) 0.0278(14) -0.0057(11) -0.0023(10) -0.0001(11) C2 0.0253(14) 0.0409(16) 0.0271(14) -0.0079(12) -0.0020(11) 0.0078(12) C11 0.0300(14) 0.0211(13) 0.0297(14) -0.0032(11) 0.0006(11) -0.0004(11) C12 0.0160(11) 0.0234(12) 0.0225(12) -0.0026(10) 0.0035(9) -0.0008(10) C13 0.0228(13) 0.0297(14) 0.0251(13) -0.0083(11) 0.0010(10) -0.0046(11) C14 0.0195(12) 0.0415(16) 0.0217(13) -0.0064(11) -0.0027(10) 0.0014(11) C15 0.0197(12) 0.0332(14) 0.0200(12) 0.0039(11) 0.0011(10) 0.0057(11) C16 0.0152(11) 0.0234(12) 0.0213(12) -0.0004(10) 0.0030(9) 0.0006(9) C17 0.0317(14) 0.0240(13) 0.0278(14) 0.0013(11) 0.0015(11) 0.0031(11) C21 0.0438(17) 0.0322(15) 0.0309(15) 0.0076(12) 0.0133(13) 0.0042(13) C22 0.0348(15) 0.0278(14) 0.0291(14) 0.0012(11) 0.0116(12) -0.0011(12) C23 0.0436(18) 0.0349(16) 0.0428(18) 0.0028(14) 0.0160(14) -0.0063(14) C24 0.0279(15) 0.0500(19) 0.0408(17) -0.0016(14) 0.0121(13) -0.0095(14) C25 0.0218(13) 0.0422(17) 0.0347(15) -0.0052(13) 0.0035(11) 0.0043(12) C26 0.0203(12) 0.0291(14) 0.0239(13) -0.0028(10) 0.0009(10) 0.0036(10) C27 0.0243(13) 0.0255(14) 0.0367(15) -0.0030(11) 0.0040(11) 0.0070(11) K1 0.0166(3) 0.0319(3) 0.0321(3) -0.0024(2) 0.0021(2) -0.0029(2) O3 0.0372(12) 0.0374(12) 0.0578(15) -0.0181(11) -0.0180(11) 0.0054(10) C31 0.0272(15) 0.0431(18) 0.054(2) -0.0161(15) 0.0065(14) -0.0040(13) C32 0.0282(15) 0.0453(18) 0.0474(19) -0.0141(15) -0.0021(13) -0.0040(14) C33 0.0327(17) 0.064(2) 0.0446(19) -0.0074(17) 0.0070(14) 0.0080(16) C34 0.048(2) 0.051(2) 0.0456(19) -0.0141(16) -0.0100(16) 0.0166(17) O4 0.0267(11) 0.0406(13) 0.0722(17) 0.0217(12) 0.0064(11) -0.0050(9) C41 0.0233(14) 0.0387(17) 0.072(2) 0.0132(16) 0.0042(15) -0.0030(13) C42 0.029(2) 0.043(3) 0.053(3) 0.020(2) 0.001(2) -0.0025(19) C43 0.022(2) 0.032(2) 0.043(3) -0.0085(19) 0.0060(18) -0.0045(16) C44 0.025(2) 0.051(3) 0.048(3) 0.016(2) -0.0053(18) -0.0085(18) C45 0.027(6) 0.031(7) 0.046(8) 0.002(6) 0.014(6) 0.006(5) C46 0.031(7) 0.052(8) 0.056(8) 0.012(7) 0.017(7) 0.005(6) C47 0.023(6) 0.037(7) 0.067(8) 0.000(7) 0.004(6) 0.003(5) O5 0.0587(15) 0.0381(13) 0.0459(14) -0.0017(10) -0.0074(12) 0.0088(11) C51 0.061(2) 0.0361(18) 0.055(2) 0.0067(16) 0.0221(18) 0.0097(16) C52 0.077(6) 0.036(5) 0.049(4) 0.005(3) -0.003(4) 0.019(5) C53 0.049(4) 0.034(3) 0.056(3) -0.008(3) 0.015(3) 0.005(3) C54 0.078(6) 0.039(4) 0.044(4) -0.012(3) 0.000(3) -0.014(4) C55 0.073(8) 0.033(8) 0.057(7) -0.005(5) 0.010(6) 0.013(7) C56 0.069(7) 0.047(7) 0.068(6) -0.010(5) 0.014(6) 0.012(6) C57 0.081(9) 0.031(6) 0.054(7) -0.016(5) -0.006(6) -0.010(7) 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' D D 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 C1 Mn1 C2 87.89(13) . . C1 Mn1 N1 92.29(10) . . C2 Mn1 N1 177.56(12) . . C1 Mn1 N2 177.44(11) . . C2 Mn1 N2 94.09(11) . . N1 Mn1 N2 85.81(8) . . C1 Mn1 S1 97.68(10) . . C2 Mn1 S1 93.17(10) . . N1 Mn1 S1 84.39(6) . . N2 Mn1 S1 83.85(6) . . C1 Mn1 S2 94.18(10) . . C2 Mn1 S2 99.13(10) . . N1 Mn1 S2 83.29(6) . . N2 Mn1 S2 83.91(6) . . S1 Mn1 S2 163.21(3) . . C1 Mn1 K1 128.70(9) . 1_655 C2 Mn1 K1 140.99(9) . 1_655 N1 Mn1 K1 39.67(6) . 1_655 N2 Mn1 K1 48.98(6) . 1_655 S1 Mn1 K1 94.34(2) . 1_655 S2 Mn1 K1 68.915(19) . 1_655 C11 S1 C21 105.58(15) . . C11 S1 Mn1 99.32(10) . . C21 S1 Mn1 96.46(10) . . C27 S2 C17 103.93(14) . . C27 S2 Mn1 98.94(10) . . C17 S2 Mn1 96.47(9) . . C1 O1 K1 155.6(2) . . C22 N2 C26 120.6(2) . . C22 N2 Mn1 120.65(18) . . C26 N2 Mn1 118.63(17) . . C16 N1 C12 120.3(2) . . C16 N1 Mn1 121.38(16) . . C12 N1 Mn1 118.35(16) . . C16 N1 K1 69.58(13) . 1_655 C12 N1 K1 84.47(13) . 1_655 Mn1 N1 K1 117.92(8) . 1_655 O1 C1 Mn1 177.9(3) . . O2 C2 Mn1 176.2(3) . . C12 C11 S1 118.8(2) . . C12 C11 H11 123(2) . . S1 C11 H11 119(2) . . N1 C12 C11 118.9(2) . . N1 C12 C13 118.1(2) . . C11 C12 C13 123.1(2) . . C14 C13 C12 120.5(2) . . C14 C13 K1 69.41(16) . 1_655 C12 C13 K1 83.70(15) . 1_655 C14 C13 H13 119.7 . . C12 C13 H13 119.7 . . K1 C13 H13 117.7 1_655 . C13 C14 C15 120.3(2) . . C13 C14 K1 87.19(17) . 1_655 C15 C14 K1 72.93(15) . 1_655 C13 C14 H14 119.9 . . C15 C14 H14 119.9 . . K1 C14 H14 110.1 1_655 . C16 C15 C14 117.9(2) . . C16 C15 K1 81.76(15) . 1_655 C14 C15 K1 81.35(16) . 1_655 C16 C15 H15 121.1 . . C14 C15 H15 121.1 . . K1 C15 H15 106.5 1_655 . N1 C16 C15 122.9(2) . . N1 C16 C17 115.2(2) . . C15 C16 C17 121.8(2) . . N1 C16 K1 87.15(14) . 1_655 C15 C16 K1 73.02(14) . 1_655 C17 C16 K1 112.26(16) . 1_655 C16 C17 S2 112.09(19) . . C16 C17 H17A 109.2 . . S2 C17 H17A 109.2 . . C16 C17 H17B 109.2 . . S2 C17 H17B 109.2 . . H17A C17 H17B 107.9 . . C22 C21 S1 111.2(2) . . C22 C21 H21A 109.4 . . S1 C21 H21A 109.4 . . C22 C21 H21B 109.4 . . S1 C21 H21B 109.4 . . H21A C21 H21B 108.0 . . N2 C22 C23 123.2(3) . . N2 C22 C21 114.9(2) . . C23 C22 C21 121.8(3) . . C22 C23 C24 117.6(3) . . C22 C23 H23 121.2 . . C24 C23 H23 121.2 . . C25 C24 C23 120.9(3) . . C25 C24 H24 119.6 . . C23 C24 H24 119.6 . . C24 C25 C26 120.4(3) . . C24 C25 K1 102.7(2) . 1_655 C26 C25 K1 75.34(16) . 1_655 C24 C25 H25 119.8 . . C26 C25 H25 119.8 . . K1 C25 H25 91.9 1_655 . C27 C26 N2 119.1(2) . . C27 C26 C25 123.6(3) . . N2 C26 C25 117.3(2) . . C27 C26 K1 88.61(17) . 1_655 N2 C26 K1 101.28(15) . 1_655 C25 C26 K1 78.76(16) . 1_655 C26 C27 S2 118.8(2) . . C26 C27 K1 68.06(16) . 1_655 S2 C27 K1 113.88(12) . 1_655 C26 C27 H27 126(2) . . S2 C27 H27 114(2) . . K1 C27 H27 100(2) 1_655 . O3 K1 O4 79.19(7) . . O3 K1 O1 81.20(7) . . O4 K1 O1 89.62(7) . . O3 K1 O5 73.58(7) . . O4 K1 O5 151.45(8) . . O1 K1 O5 78.02(8) . . O3 K1 C15 86.41(8) . 1_455 O4 K1 C15 109.74(8) . 1_455 O1 K1 C15 154.64(8) . 1_455 O5 K1 C15 77.29(8) . 1_455 O3 K1 C26 167.90(7) . 1_455 O4 K1 C26 110.96(8) . 1_455 O1 K1 C26 92.04(7) . 1_455 O5 K1 C26 95.28(7) . 1_455 C15 K1 C26 95.86(7) 1_455 1_455 O3 K1 C14 77.01(7) . 1_455 O4 K1 C14 84.38(8) . 1_455 O1 K1 C14 158.11(7) . 1_455 O5 K1 C14 97.54(8) . 1_455 C15 K1 C14 25.72(7) 1_455 1_455 C26 K1 C14 109.77(7) 1_455 1_455 O3 K1 C16 111.43(8) . 1_455 O4 K1 C16 116.27(7) . 1_455 O1 K1 C16 152.44(7) . 1_455 O5 K1 C16 82.25(7) . 1_455 C15 K1 C16 25.22(6) 1_455 1_455 C26 K1 C16 70.72(7) 1_455 1_455 C14 K1 C16 43.74(7) 1_455 1_455 O3 K1 C25 149.37(8) . 1_455 O4 K1 C25 99.74(8) . 1_455 O1 K1 C25 68.18(7) . 1_455 O5 K1 C25 99.32(8) . 1_455 C15 K1 C25 121.74(7) 1_455 1_455 C26 K1 C25 25.89(7) 1_455 1_455 C14 K1 C25 133.58(7) 1_455 1_455 C16 K1 C25 96.62(7) 1_455 1_455 O3 K1 C47 79.1(4) . . O4 K1 C47 25.2(2) . . O1 K1 C47 64.6(2) . . O5 K1 C47 136.4(2) . . C15 K1 C47 134.4(3) 1_455 . C26 K1 C47 107.2(4) 1_455 . C14 K1 C47 108.7(3) 1_455 . C16 K1 C47 140.1(2) 1_455 . C25 K1 C47 87.4(4) 1_455 . O3 K1 N1 126.03(7) . 1_455 O4 K1 N1 99.02(6) . 1_455 O1 K1 N1 152.44(6) . 1_455 O5 K1 N1 103.79(7) . 1_455 C15 K1 N1 42.88(6) 1_455 1_455 C26 K1 N1 60.42(6) 1_455 1_455 C14 K1 N1 49.43(6) 1_455 1_455 C16 K1 N1 23.27(6) 1_455 1_455 C25 K1 N1 84.53(6) 1_455 1_455 O3 K1 C13 91.77(7) . 1_455 O4 K1 C13 69.12(7) . 1_455 O1 K1 C13 158.57(7) . 1_455 O5 K1 C13 119.53(8) . 1_455 C15 K1 C13 42.85(7) 1_455 1_455 C26 K1 C13 97.98(6) 1_455 1_455 C14 K1 C13 23.40(7) 1_455 1_455 C16 K1 C13 48.70(6) 1_455 1_455 C25 K1 C13 116.72(7) 1_455 1_455 N1 K1 C13 41.35(5) 1_455 1_455 C34 O3 C31 105.3(2) . . C34 O3 K1 125.2(2) . . C31 O3 K1 125.36(19) . . O3 C31 C32 106.3(2) . . O3 C31 D31A 110.5 . . C32 C31 D31A 110.5 . . O3 C31 D31B 110.5 . . C32 C31 D31B 110.5 . . D31A C31 D31B 108.7 . . C33 C32 C31 104.2(3) . . C33 C32 D32A 110.9 . . C31 C32 D32A 110.9 . . C33 C32 D32B 110.9 . . C31 C32 D32B 110.9 . . D32A C32 D32B 108.9 . . C34 C33 C32 102.1(3) . . C34 C33 D33A 111.3 . . C32 C33 D33A 111.3 . . C34 C33 D33B 111.3 . . C32 C33 D33B 111.3 . . D33A C33 D33B 109.2 . . O3 C34 C33 104.6(3) . . O3 C34 D34A 110.8 . . C33 C34 D34A 110.8 . . O3 C34 D34B 110.8 . . C33 C34 D34B 110.8 . . D34A C34 D34B 108.9 . . C41 O4 C44 107.8(3) . . C41 O4 C47 104.4(7) . . C41 O4 K1 125.68(19) . . C44 O4 K1 121.6(2) . . C47 O4 K1 103.1(6) . . O4 C41 C45 107.6(6) . . O4 C41 C42 103.1(3) . . O4 C41 D41A 111.1 . . C42 C41 D41A 111.1 . . O4 C41 D41B 111.1 . . C42 C41 D41B 111.1 . . D41A C41 D41B 109.1 . . O4 C41 D41C 110.2 . . C45 C41 D41C 110.2 . . O4 C41 D41D 110.2 . . C45 C41 D41D 110.2 . . D41C C41 D41D 108.5 . . C43 C42 C41 98.7(4) . . C43 C42 D42A 112.0 . . C41 C42 D42A 112.0 . . C43 C42 D42B 112.0 . . C41 C42 D42B 112.0 . . D42A C42 D42B 109.7 . . C44 C43 C42 103.9(4) . . C44 C43 D43A 111.0 . . C42 C43 D43A 111.0 . . C44 C43 D43B 111.0 . . C42 C43 D43B 111.0 . . D43A C43 D43B 109.0 . . O4 C44 C43 107.0(3) . . O4 C44 D44A 110.3 . . C43 C44 D44A 110.3 . . O4 C44 D44B 110.3 . . C43 C44 D44B 110.3 . . D44A C44 D44B 108.6 . . C41 C45 C46 104.1(10) . . C41 C45 D45A 110.9 . . C46 C45 D45A 110.9 . . C41 C45 D45B 110.9 . . C46 C45 D45B 110.9 . . D45A C45 D45B 109.0 . . C47 C46 C45 106.3(12) . . C47 C46 D46A 110.5 . . C45 C46 D46A 110.5 . . C47 C46 D46B 110.5 . . C45 C46 D46B 110.5 . . D46A C46 D46B 108.7 . . C46 C47 O4 106.2(11) . . C46 C47 K1 154.5(10) . . O4 C47 K1 51.7(5) . . C46 C47 D47A 110.5 . . O4 C47 D47A 110.5 . . K1 C47 D47A 91.4 . . C46 C47 D47B 110.5 . . O4 C47 D47B 110.5 . . K1 C47 D47B 72.6 . . D47A C47 D47B 108.7 . . C57 O5 C51 105.7(9) . . C51 O5 C54 109.5(4) . . C57 O5 K1 129.2(9) . . C51 O5 K1 124.7(2) . . C54 O5 K1 121.8(5) . . O5 C51 C52 105.5(4) . . O5 C51 C55 104.2(8) . . O5 C51 D51A 110.6 . . C52 C51 D51A 110.6 . . O5 C51 D51B 110.6 . . C52 C51 D51B 110.6 . . D51A C51 D51B 108.8 . . O5 C51 D51C 110.9 . . C55 C51 D51C 110.9 . . O5 C51 D51D 110.9 . . C55 C51 D51D 110.9 . . D51C C51 D51D 108.9 . . C53 C52 C51 104.2(5) . . C53 C52 D52A 110.9 . . C51 C52 D52A 110.9 . . C53 C52 D52B 110.9 . . C51 C52 D52B 110.9 . . D52A C52 D52B 108.9 . . C52 C53 C54 101.4(6) . . C52 C53 D53A 111.5 . . C54 C53 D53A 111.5 . . C52 C53 D53B 111.5 . . C54 C53 D53B 111.5 . . D53A C53 D53B 109.3 . . O5 C54 C53 108.6(6) . . O5 C54 D54A 110.0 . . C53 C54 D54A 110.0 . . O5 C54 D54B 110.0 . . C53 C54 D54B 110.0 . . D54A C54 D54B 108.4 . . C56 C55 C51 102.3(10) . . C56 C55 D55A 111.3 . . C51 C55 D55A 111.3 . . C56 C55 D55B 111.3 . . C51 C55 D55B 111.3 . . D55A C55 D55B 109.2 . . C55 C56 C57 105.7(12) . . C55 C56 D56A 110.6 . . C57 C56 D56A 110.6 . . C55 C56 D56B 110.6 . . C57 C56 D56B 110.6 . . D56A C56 D56B 108.7 . . O5 C57 C56 99.8(10) . . O5 C57 D57A 111.8 . . C56 C57 D57A 111.8 . . O5 C57 D57B 111.8 . . C56 C57 D57B 111.8 . . D57A C57 D57B 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mn1 C1 1.767(3) . Mn1 C2 1.779(3) . Mn1 N1 2.044(2) . Mn1 N2 2.049(2) . Mn1 S1 2.2756(8) . Mn1 S2 2.2867(7) . Mn1 K1 4.7368(7) 1_655 S1 C11 1.737(3) . S1 C21 1.820(3) . S2 C27 1.752(3) . S2 C17 1.825(3) . O1 C1 1.176(3) . O1 K1 2.733(2) . O2 C2 1.162(4) . N2 C22 1.355(4) . N2 C26 1.382(3) . N1 C16 1.354(3) . N1 C12 1.382(3) . N1 K1 3.422(2) 1_655 C11 C12 1.384(4) . C11 H11 0.91(3) . C12 C13 1.437(4) . C13 C14 1.362(4) . C13 K1 3.424(3) 1_655 C13 H13 0.9500 . C14 C15 1.409(4) . C14 K1 3.209(3) 1_655 C14 H14 0.9500 . C15 C16 1.383(4) . C15 K1 3.103(3) 1_655 C15 H15 0.9500 . C16 C17 1.499(4) . C16 K1 3.211(2) 1_655 C17 H17A 0.9900 . C17 H17B 0.9900 . C21 C22 1.508(4) . C21 H21A 0.9900 . C21 H21B 0.9900 . C22 C23 1.372(4) . C23 C24 1.405(5) . C23 H23 0.9500 . C24 C25 1.356(5) . C24 H24 0.9500 . C25 C26 1.445(4) . C25 K1 3.246(3) 1_655 C25 H25 0.9500 . C26 C27 1.367(4) . C26 K1 3.202(3) 1_655 C27 K1 3.451(3) 1_655 C27 H27 0.91(3) . K1 O3 2.714(2) . K1 O4 2.714(2) . K1 O5 2.758(2) . K1 C47 3.368(14) . O3 C34 1.425(4) . O3 C31 1.428(4) . C31 C32 1.525(4) . C31 D31A 0.9900 . C31 D31B 0.9900 . C32 C33 1.517(5) . C32 D32A 0.9900 . C32 D32B 0.9900 . C33 C34 1.485(5) . C33 D33A 0.9900 . C33 D33B 0.9900 . C34 D34A 0.9900 . C34 D34B 0.9900 . O4 C41 1.415(4) . O4 C44 1.466(4) . O4 C47 1.470(12) . C41 C45 1.490(12) . C41 C42 1.552(5) . C41 D41A 0.9900 . C41 D41B 0.9900 . C41 D41C 0.9900 . C41 D41D 0.9900 . C42 C43 1.537(6) . C42 D42A 0.9900 . C42 D42B 0.9900 . C43 C44 1.479(6) . C43 D43A 0.9900 . C43 D43B 0.9900 . C44 D44A 0.9900 . C44 D44B 0.9900 . C45 C46 1.506(16) . C45 D45A 0.9900 . C45 D45B 0.9900 . C46 C47 1.460(16) . C46 D46A 0.9900 . C46 D46B 0.9900 . C47 D47A 0.9900 . C47 D47B 0.9900 . O5 C57 1.396(13) . O5 C51 1.408(4) . O5 C54 1.420(8) . C51 C52 1.530(8) . C51 C55 1.533(14) . C51 D51A 0.9900 . C51 D51B 0.9900 . C51 D51C 0.9900 . C51 D51D 0.9900 . C52 C53 1.488(10) . C52 D52A 0.9900 . C52 D52B 0.9900 . C53 C54 1.513(10) . C53 D53A 0.9900 . C53 D53B 0.9900 . C54 D54A 0.9900 . C54 D54B 0.9900 . C55 C56 1.479(15) . C55 D55A 0.9900 . C55 D55B 0.9900 . C56 C57 1.521(15) . C56 D56A 0.9900 . C56 D56B 0.9900 . C57 D57A 0.9900 . C57 D57B 0.9900 . 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 C21 S1 C11 C12 -103.4(2) . . Mn1 S1 C11 C12 -3.9(2) . . C16 N1 C12 C11 -175.6(2) . . Mn1 N1 C12 C11 3.1(3) . . K1 N1 C12 C11 122.0(2) 1_655 . C16 N1 C12 C13 3.6(3) . . Mn1 N1 C12 C13 -177.66(17) . . K1 N1 C12 C13 -58.8(2) 1_655 . S1 C11 C12 N1 1.1(3) . . S1 C11 C12 C13 -178.1(2) . . N1 C12 C13 C14 -2.7(4) . . C11 C12 C13 C14 176.5(3) . . N1 C12 C13 K1 58.9(2) . 1_655 C11 C12 C13 K1 -121.9(2) . 1_655 C12 C13 C14 C15 0.7(4) . . K1 C13 C14 C15 -68.3(2) 1_655 . C12 C13 C14 K1 69.1(2) . 1_655 C13 C14 C15 C16 0.3(4) . . K1 C14 C15 C16 -75.8(2) 1_655 . C13 C14 C15 K1 76.2(2) . 1_655 C12 N1 C16 C15 -2.7(4) . . Mn1 N1 C16 C15 178.61(18) . . K1 N1 C16 C15 67.6(2) 1_655 . C12 N1 C16 C17 176.3(2) . . Mn1 N1 C16 C17 -2.3(3) . . K1 N1 C16 C17 -113.3(2) 1_655 . C12 N1 C16 K1 -70.3(2) . 1_655 Mn1 N1 C16 K1 110.98(13) . 1_655 C14 C15 C16 N1 0.7(4) . . K1 C15 C16 N1 -75.0(2) 1_655 . C14 C15 C16 C17 -178.3(2) . . K1 C15 C16 C17 106.1(2) 1_655 . C14 C15 C16 K1 75.6(2) . 1_655 N1 C16 C17 S2 27.4(3) . . C15 C16 C17 S2 -153.6(2) . . K1 C16 C17 S2 -70.28(19) 1_655 . C27 S2 C17 C16 66.5(2) . . Mn1 S2 C17 C16 -34.44(19) . . C11 S1 C21 C22 64.9(3) . . Mn1 S1 C21 C22 -36.7(2) . . C26 N2 C22 C23 -1.6(4) . . Mn1 N2 C22 C23 174.2(2) . . C26 N2 C22 C21 175.5(2) . . Mn1 N2 C22 C21 -8.7(3) . . S1 C21 C22 N2 32.8(3) . . S1 C21 C22 C23 -150.1(3) . . N2 C22 C23 C24 0.9(5) . . C21 C22 C23 C24 -176.0(3) . . C22 C23 C24 C25 0.7(5) . . C23 C24 C25 C26 -1.5(5) . . C23 C24 C25 K1 -81.7(3) . 1_655 C22 N2 C26 C27 178.6(3) . . Mn1 N2 C26 C27 2.7(3) . . C22 N2 C26 C25 0.8(4) . . Mn1 N2 C26 C25 -175.10(19) . . C22 N2 C26 K1 83.9(2) . 1_655 Mn1 N2 C26 K1 -92.03(15) . 1_655 C24 C25 C26 C27 -177.0(3) . . K1 C25 C26 C27 -80.7(3) 1_655 . C24 C25 C26 N2 0.7(4) . . K1 C25 C26 N2 97.0(2) 1_655 . C24 C25 C26 K1 -96.3(3) . 1_655 N2 C26 C27 S2 3.9(4) . . C25 C26 C27 S2 -178.4(2) . . K1 C26 C27 S2 106.05(19) 1_655 . N2 C26 C27 K1 -102.2(2) . 1_655 C25 C26 C27 K1 75.5(3) . 1_655 C17 S2 C27 C26 -106.3(2) . . Mn1 S2 C27 C26 -7.2(2) . . C17 S2 C27 K1 -29.13(15) . 1_655 Mn1 S2 C27 K1 69.88(11) . 1_655 C34 O3 C31 C32 27.4(4) . . K1 O3 C31 C32 -130.7(2) . . O3 C31 C32 C33 -2.9(4) . . C31 C32 C33 C34 -21.3(4) . . C31 O3 C34 C33 -42.1(4) . . K1 O3 C34 C33 116.1(2) . . C32 C33 C34 O3 38.8(4) . . C47 O4 C41 C45 -33.3(14) . . K1 O4 C41 C45 -151.5(9) . . C44 O4 C41 C42 34.0(5) . . K1 O4 C41 C42 -121.2(3) . . O4 C41 C42 C43 -43.5(5) . . C41 C42 C43 C44 36.9(5) . . C41 O4 C44 C43 -10.0(5) . . K1 O4 C44 C43 146.4(3) . . C42 C43 C44 O4 -18.5(6) . . O4 C41 C45 C46 21(2) . . C41 C45 C46 C47 -1(2) . . C45 C46 C47 O4 -19(2) . . C45 C46 C47 K1 8(5) . . C41 O4 C47 C46 32.6(17) . . K1 O4 C47 C46 165.3(15) . . C41 O4 C47 K1 -132.7(5) . . C54 O5 C51 C52 14.3(10) . . K1 O5 C51 C52 -143.4(7) . . C57 O5 C51 C55 41.9(17) . . K1 O5 C51 C55 -131.4(13) . . O5 C51 C52 C53 -29.7(11) . . C51 C52 C53 C54 31.8(12) . . C51 O5 C54 C53 6.3(11) . . K1 O5 C54 C53 164.8(6) . . C52 C53 C54 O5 -24.4(12) . . O5 C51 C55 C56 -17(2) . . C51 C55 C56 C57 -11(2) . . C51 O5 C57 C56 -47.8(18) . . K1 O5 C57 C56 125.2(12) . . C55 C56 C57 O5 35(2) . .