#------------------------------------------------------------------------------ #$Date: 2017-04-19 05:59:00 +0300 (Wed, 19 Apr 2017) $ #$Revision: 195532 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042717.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_7042717 loop_ _publ_author_name 'Figueroa, Joshua S.' 'Agnew, Douglas W.' 'Moore, Curtis E.' 'Rheingold, Arnold L.' _publ_section_title ; Comparison of Nucleophilic- and Radical-Based Routes to the Formation of Manganese-Main Group Element Single Bonds ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT01102D _journal_year 2017 _chemical_formula_moiety 'C65 H74 F2 Mn N2 O3 Sb, 2(C5 H5 N)' _chemical_formula_sum 'C75 H84 F2 Mn N4 O3 Sb' _chemical_formula_weight 1304.15 _chemical_name_common Mn(SbF2)(CO)3(CNArDipp2)2_2(pyr) _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2016-10-27 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227) ; _audit_update_record ; 2017-03-20 deposited with the CCDC. 2017-04-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.8090(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.9656(4) _cell_length_b 17.3952(4) _cell_length_c 25.1885(6) _cell_measurement_reflns_used 9853 _cell_measurement_temperature 100 _cell_measurement_theta_max 25.908 _cell_measurement_theta_min 2.217 _cell_volume 6847.4(3) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'APEX2 v2013.6-2 (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SIR2004 (Burla et al., 2007)' _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX-II CCD' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker APEX II Ultra' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_unetI/netI 0.0355 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 55310 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.120 _diffrn_reflns_theta_min 1.303 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker TXS' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.6909 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1079 before and 0.0442 after correction. The Ratio of minimum to maximum transmission is 0.9270. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour 'clear orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.265 _exptl_crystal_description block _exptl_crystal_F_000 2720 _exptl_crystal_recrystallization_method 'Grown from saturated pyridine solution at -40C' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.672 _refine_diff_density_min -1.205 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 838 _refine_ls_number_reflns 13552 _refine_ls_number_restraints 72 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0445 _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^)+(0.0678P)^2^+10.8995P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1213 _refine_ls_wR_factor_ref 0.1308 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10944 _reflns_number_total 13552 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt01102d2.cif _cod_data_source_block jfig1141 _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7042717 _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. ; _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. Uiso/Uaniso restraints and constraints Uanis(F2A) = Uanis(F1) = Uanis(F1A) = Uanis(F2) Uanis(C16A) = Uanis(C16) = Uanis(C15) = Uanis(C15A) 3. Rigid body (RIGU) restrains C14S, N3S, C11S, C13S, C15S, C12S with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C7S, C8S, C9S, C10S, N2S, C6S with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(F1A)=Sof(F2A)=1-FVAR(1) Sof(F2)=Sof(F1)=FVAR(1) Sof(H14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)= Sof(H16E)=Sof(H16F)=1-FVAR(2) Sof(H14)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C15)=Sof(H15A)=Sof(H15B)= Sof(H15C)=FVAR(2) Sof(C7S)=Sof(H7S)=Sof(C8S)=Sof(H8S)=Sof(C9S)=Sof(H9S)=Sof(C10S)=Sof(H10S)= Sof(N2S)=Sof(C6S)=Sof(H6S)=1-FVAR(3) Sof(N3S)=Sof(C11S)=Sof(H11S)=Sof(C13S)=Sof(H13S)=Sof(C12S)=Sof(H12S)= Sof(C15S)=Sof(H15S)=Sof(C14S)=Sof(H14S)=FVAR(3) 5.a Ternary CH refined with riding coordinates: C33(H33), C26(H26), C44(H44), C51(H51), C21(H21), C63(H63), C56(H56), C14(H14), C14(H14A) 5.b Aromatic/amide H refined with riding coordinates: C39(H39), C40(H40), C10(H10), C9(H9), C38(H38), C8(H8), C61(H61), C59(H59), C30(H30), C29(H29), C60(H60), C31(H31), C17(H17), C18(H18), C47(H47), C49(H49), C19(H19), C5S(H5S), C48(H48), C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C11S(H11S), C13S(H13S), C12S(H12S), C15S(H15S), C14S(H14S), C7S(H7S), C8S(H8S), C9S(H9S), C10S(H10S), C6S(H6S) 5.c Fitted hexagon refined as free rotating group: C7S(C8S,C9S,C10S,N2S,C6S) 5.d Idealised Me refined as rotating group: C64(H64A,H64B,H64C), C53(H53A,H53B,H53C), C46(H46A,H46B,H46C), C65(H65A,H65B, H65C), C52(H52A,H52B,H52C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C28(H28A, H28B,H28C), C45(H45A,H45B,H45C), C58(H58A,H58B,H58C), C35(H35A,H35B,H35C), C57(H57A,H57B,H57C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C16(H16A,H16B, H16C), C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F) ; _shelx_res_file ; jfig1141_p21c_a.res created by SHELXL-2014/7 TITL JFig1141_P21c_a.res in P2(1)/c REM Old TITL JFig1141_P21c in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.136, Rweak 0.006, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C77 N3 O4 Mn Sb CELL 0.71073 15.9656 17.3952 25.1885 90 101.809 90 ZERR 4 0.0004 0.0004 0.0006 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F Mn N O Sb UNIT 300 336 8 4 16 12 4 RIGU C14S N3S C11S C13S C15S C12S RIGU C7S C8S C9S C10S N2S C6S EADP F2A F1 F1A F2 EADP C16A C16 C15 C15A L.S. 10 PLAN 20 TEMP -173.15 BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 OMIT 0 1 1 OMIT 0 0 2 REM REM REM WGHT 0.067800 10.899500 FVAR 0.17612 0.21485 0.64237 0.87711 SB1 7 0.229464 0.280318 0.415814 11.00000 0.03016 0.03194 = 0.02921 0.00856 0.01044 0.00946 MN1 4 0.280540 0.341084 0.333122 11.00000 0.01192 0.00827 = 0.02026 -0.00088 0.00336 0.00404 N1 5 0.394930 0.200204 0.333847 11.00000 0.01119 0.00953 = 0.01337 -0.00035 0.00269 0.00127 N2 5 0.158104 0.473429 0.341620 11.00000 0.01147 0.00811 = 0.01369 -0.00200 -0.00049 0.00086 PART 1 F1A 3 0.139823 0.353598 0.423586 -21.00000 0.04976 0.03280 = 0.05227 0.00004 0.02711 -0.00113 PART 0 O1 6 0.136854 0.258519 0.262710 11.00000 0.03249 0.03192 = 0.05419 -0.01672 -0.01367 0.00996 C6 1 0.451151 0.138478 0.333906 11.00000 0.00766 0.00808 = 0.01282 -0.00143 -0.00105 0.00122 O2 6 0.416306 0.417922 0.414904 11.00000 0.02788 0.03385 = 0.08308 -0.02603 -0.02062 0.00663 C7 1 0.455791 0.082763 0.374639 11.00000 0.00853 0.00844 = 0.01128 -0.00226 -0.00102 -0.00151 C36 1 0.101945 0.534728 0.342929 11.00000 0.01061 0.00675 = 0.01488 0.00075 0.00415 0.00070 C11 1 0.499846 0.135048 0.293730 11.00000 0.01158 0.00701 = 0.01244 -0.00197 0.00014 -0.00264 O3 6 0.340722 0.406253 0.240344 11.00000 0.07671 0.04157 = 0.08415 0.02853 0.05365 0.02917 N1S 5 0.833513 0.191939 0.534741 11.00000 0.03307 0.02730 = 0.02773 -0.00624 0.00173 -0.00167 C5 1 0.351248 0.253235 0.333993 11.00000 0.01174 0.01167 = 0.01322 0.00091 0.00179 -0.00281 C24 1 0.399679 0.086862 0.415411 11.00000 0.01192 0.00671 = 0.01185 0.00165 0.00081 0.00139 C32 1 0.430734 0.121278 0.466014 11.00000 0.01752 0.00947 = 0.01451 0.00200 0.00156 0.00081 C41 1 0.123774 0.590087 0.383978 11.00000 0.01266 0.00815 = 0.01164 -0.00059 0.00294 -0.00095 C4 1 0.204780 0.423626 0.338304 11.00000 0.01080 0.01209 = 0.01321 -0.00021 -0.00043 -0.00298 C33 1 0.518721 0.158696 0.479135 11.00000 0.01851 0.01462 = 0.01417 -0.00019 0.00066 -0.00518 AFIX 13 H33 2 0.544285 0.154270 0.446186 11.00000 -1.20000 AFIX 0 C39 1 -0.003206 0.659742 0.341997 11.00000 0.01880 0.01072 = 0.02080 -0.00194 -0.00075 0.00719 AFIX 43 H39 2 -0.039665 0.702996 0.341570 11.00000 -1.20000 AFIX 0 C62 1 -0.033020 0.412364 0.266432 11.00000 0.01370 0.00955 = 0.01641 0.00045 -0.00138 0.00380 C40 1 0.069876 0.652894 0.382644 11.00000 0.01947 0.00897 = 0.01393 -0.00385 0.00267 0.00141 AFIX 43 H40 2 0.082975 0.691556 0.409711 11.00000 -1.20000 AFIX 0 C10 1 0.556310 0.073570 0.295543 11.00000 0.01657 0.01317 = 0.01604 -0.00044 0.00625 0.00170 AFIX 43 H10 2 0.589734 0.068963 0.268536 11.00000 -1.20000 AFIX 0 C25 1 0.317199 0.055221 0.402639 11.00000 0.01194 0.01206 = 0.01685 0.00344 -0.00067 -0.00053 C9 1 0.564167 0.018798 0.336625 11.00000 0.01809 0.01096 = 0.02193 0.00343 0.00405 0.00673 AFIX 43 H9 2 0.604020 -0.022066 0.337961 11.00000 -1.20000 AFIX 0 C42 1 0.206301 0.582847 0.424654 11.00000 0.01249 0.00649 = 0.01476 -0.00358 -0.00114 0.00106 C12 1 0.490636 0.194992 0.249903 11.00000 0.01230 0.00957 = 0.01406 0.00076 0.00499 0.00200 PART 1 F2A 3 0.144577 0.211551 0.379391 -21.00000 0.04976 0.03280 = 0.05227 0.00004 0.02711 -0.00113 PART 0 C13 1 0.432902 0.182989 0.200797 11.00000 0.02133 0.01345 = 0.01693 0.00146 0.00121 -0.00228 C43 1 0.282676 0.605653 0.409099 11.00000 0.01591 0.00853 = 0.02076 -0.00785 0.00294 -0.00181 C38 1 -0.023298 0.603905 0.302062 11.00000 0.01211 0.01530 = 0.01848 -0.00175 -0.00324 0.00400 AFIX 43 H38 2 -0.073382 0.609510 0.274544 11.00000 -1.20000 AFIX 0 C37 1 0.028820 0.539778 0.301696 11.00000 0.01293 0.00931 = 0.01362 -0.00105 0.00117 0.00042 C8 1 0.514454 0.023417 0.375463 11.00000 0.01863 0.00994 = 0.01217 0.00174 -0.00044 0.00257 AFIX 43 H8 2 0.520440 -0.014502 0.403127 11.00000 -1.20000 AFIX 0 C26 1 0.282130 0.020133 0.347196 11.00000 0.01311 0.02159 = 0.01655 0.00093 -0.00174 -0.00556 AFIX 13 H26 2 0.321339 0.035104 0.322660 11.00000 -1.20000 AFIX 0 C44 1 0.281382 0.641827 0.354049 11.00000 0.02123 0.01633 = 0.02294 -0.00524 0.01038 -0.00577 AFIX 13 H44 2 0.226825 0.625958 0.329356 11.00000 -1.20000 AFIX 0 C61 1 -0.054131 0.360085 0.223724 11.00000 0.02237 0.00950 = 0.02268 -0.00175 -0.00106 -0.00066 AFIX 43 H61 2 -0.083728 0.314155 0.228784 11.00000 -1.20000 AFIX 0 C20 1 0.540258 0.262037 0.258779 11.00000 0.01822 0.01385 = 0.01533 -0.00043 0.00585 -0.00106 C59 1 0.011821 0.440049 0.166634 11.00000 0.02675 0.01783 = 0.01699 -0.00427 0.00518 0.00079 AFIX 43 H59 2 0.027918 0.448538 0.132829 11.00000 -1.20000 AFIX 0 C30 1 0.298060 0.088277 0.492627 11.00000 0.02318 0.02866 = 0.02149 0.00264 0.01257 0.00082 AFIX 43 H30 2 0.263636 0.088109 0.519247 11.00000 -1.20000 AFIX 0 C51 1 0.125813 0.531462 0.495188 11.00000 0.02100 0.02576 = 0.01613 0.00502 0.00161 -0.00329 AFIX 13 H51 2 0.081500 0.518463 0.462243 11.00000 -1.20000 AFIX 0 C29 1 0.267740 0.056054 0.442316 11.00000 0.01300 0.02615 = 0.02553 0.00290 0.00187 -0.00337 AFIX 43 H29 2 0.212126 0.034018 0.434549 11.00000 -1.20000 AFIX 0 C54 1 0.009844 0.480513 0.257595 11.00000 0.01167 0.01069 = 0.01564 -0.00298 -0.00103 0.00363 C60 1 -0.032524 0.374224 0.174025 11.00000 0.02448 0.01253 = 0.01999 -0.00749 -0.00260 0.00368 AFIX 43 H60 2 -0.048257 0.338604 0.145113 11.00000 -1.20000 AFIX 0 C50 1 0.207593 0.553505 0.476774 11.00000 0.01805 0.01183 = 0.01827 0.00026 -0.00081 -0.00277 C31 1 0.378736 0.120805 0.504133 11.00000 0.02478 0.02053 = 0.01214 -0.00023 0.00485 0.00014 AFIX 43 H31 2 0.399099 0.143282 0.538742 11.00000 -1.20000 AFIX 0 C21 1 0.602710 0.276638 0.311879 11.00000 0.02283 0.01888 = 0.01749 -0.00125 0.00165 -0.00955 AFIX 13 H21 2 0.590661 0.238123 0.338825 11.00000 -1.20000 AFIX 0 C55 1 0.033459 0.494338 0.207817 11.00000 0.02061 0.01476 = 0.01990 -0.00578 0.00393 -0.00114 C17 1 0.427583 0.238277 0.160110 11.00000 0.02727 0.02022 = 0.01624 0.00432 -0.00112 0.00065 AFIX 43 H17 2 0.388948 0.230751 0.126447 11.00000 -1.20000 AFIX 0 C18 1 0.477351 0.303535 0.167907 11.00000 0.03131 0.01608 = 0.01838 0.00752 0.00668 0.00132 AFIX 43 H18 2 0.473420 0.340322 0.139628 11.00000 -1.20000 AFIX 0 C47 1 0.359827 0.598020 0.446748 11.00000 0.01305 0.01745 = 0.03331 -0.00890 0.00246 -0.00292 AFIX 43 H47 2 0.411801 0.612777 0.436793 11.00000 -1.20000 AFIX 0 C63 1 -0.059651 0.397378 0.319918 11.00000 0.02346 0.01099 = 0.01689 0.00120 -0.00024 0.00170 AFIX 13 H63 2 -0.017348 0.423752 0.348975 11.00000 -1.20000 AFIX 0 PART 1 N3S 5 0.109989 0.095265 0.556533 41.00000 0.05053 0.03410 = 0.03739 0.00460 0.02328 0.00150 PART 0 C49 1 0.286591 0.547840 0.512762 11.00000 0.02934 0.01957 = 0.01843 0.00387 -0.00773 -0.00115 AFIX 43 H49 2 0.288718 0.528607 0.548313 11.00000 -1.20000 AFIX 0 C19 1 0.532862 0.315404 0.216785 11.00000 0.02564 0.01203 = 0.02373 0.00092 0.00840 -0.00467 AFIX 43 H19 2 0.566704 0.360757 0.221970 11.00000 -1.20000 AFIX 0 C1 1 0.189969 0.289169 0.289305 11.00000 0.02377 0.01312 = 0.03431 -0.00121 0.00249 0.01072 C5S 1 0.773342 0.232013 0.501456 11.00000 0.03017 0.02094 = 0.02839 -0.00580 0.00790 -0.00324 AFIX 43 H5S 2 0.758743 0.281322 0.513010 11.00000 -1.20000 AFIX 0 C48 1 0.361793 0.569670 0.497680 11.00000 0.01662 0.02367 = 0.03146 -0.00280 -0.01077 0.00130 AFIX 43 H48 2 0.414822 0.564967 0.522710 11.00000 -1.20000 AFIX 0 C1S 1 0.851848 0.122880 0.517190 11.00000 0.03407 0.03135 = 0.03375 0.00389 0.00878 0.00512 AFIX 43 H1S 2 0.894083 0.093020 0.540293 11.00000 -1.20000 AFIX 0 C56 1 0.085421 0.564969 0.198497 11.00000 0.04634 0.02329 = 0.02387 -0.00982 0.01660 -0.01425 AFIX 13 H56 2 0.083689 0.602397 0.228387 11.00000 -1.20000 AFIX 0 C64 1 -0.147826 0.433508 0.319128 11.00000 0.03199 0.02299 = 0.02879 0.00431 0.01318 0.00863 AFIX 137 H64A 2 -0.144267 0.489350 0.314938 11.00000 -1.50000 H64B 2 -0.165656 0.421840 0.353235 11.00000 -1.50000 H64C 2 -0.189735 0.412355 0.288707 11.00000 -1.50000 AFIX 0 C14 1 0.374432 0.112594 0.191455 11.00000 0.04366 0.02673 = 0.02229 0.00929 -0.01558 -0.01863 PART 1 AFIX 13 H14 2 0.392400 0.076377 0.222530 31.00000 -1.20000 AFIX 13 PART 0 PART 2 H14A 2 0.396838 0.077898 0.222799 -31.00000 -1.20000 AFIX 0 PART 0 C53 1 0.093286 0.600544 0.523190 11.00000 0.03072 0.02996 = 0.02723 0.00650 0.00998 0.00218 AFIX 137 H53A 2 0.136903 0.615817 0.554735 11.00000 -1.50000 H53B 2 0.040621 0.586274 0.535039 11.00000 -1.50000 H53C 2 0.081587 0.643600 0.497654 11.00000 -1.50000 AFIX 0 C46 1 0.280677 0.729759 0.358290 11.00000 0.05041 0.01823 = 0.02938 -0.00028 0.01402 -0.00026 AFIX 137 H46A 2 0.230737 0.746131 0.372449 11.00000 -1.50000 H46B 2 0.277813 0.752249 0.322291 11.00000 -1.50000 H46C 2 0.333030 0.747090 0.382841 11.00000 -1.50000 AFIX 0 C3 1 0.319007 0.382950 0.274041 11.00000 0.03208 0.01602 = 0.05948 -0.00013 0.02273 0.01512 C65 1 -0.060034 0.312122 0.334803 11.00000 0.03018 0.01503 = 0.02839 0.00510 0.00715 0.00135 AFIX 137 H65A 2 -0.105554 0.285718 0.309312 11.00000 -1.50000 H65B 2 -0.070157 0.306823 0.371712 11.00000 -1.50000 H65C 2 -0.004638 0.289216 0.332921 11.00000 -1.50000 AFIX 0 C2 1 0.364312 0.388673 0.384079 11.00000 0.01823 0.01397 = 0.05519 -0.00740 0.00279 0.00821 C52 1 0.136938 0.461569 0.533099 11.00000 0.03803 0.02507 = 0.02566 0.00609 0.00591 -0.00802 AFIX 137 H52A 2 0.163330 0.419427 0.516557 11.00000 -1.50000 H52B 2 0.080873 0.445173 0.539077 11.00000 -1.50000 H52C 2 0.173721 0.475445 0.567889 11.00000 -1.50000 AFIX 0 C2S 1 0.813851 0.091993 0.468012 11.00000 0.04897 0.01990 = 0.04106 -0.00754 0.02575 -0.00730 AFIX 43 H2S 2 0.829931 0.042608 0.457458 11.00000 -1.20000 AFIX 0 C27 1 0.193400 0.050040 0.322214 11.00000 0.03449 0.02730 = 0.03530 -0.00902 -0.01931 0.00992 AFIX 137 H27A 2 0.153225 0.035183 0.345059 11.00000 -1.50000 H27B 2 0.174662 0.028023 0.285910 11.00000 -1.50000 H27C 2 0.195083 0.106203 0.319560 11.00000 -1.50000 AFIX 0 C34 1 0.578107 0.117681 0.525298 11.00000 0.02168 0.04344 = 0.03321 0.01961 -0.00473 -0.00657 AFIX 137 H34A 2 0.556394 0.123620 0.558751 11.00000 -1.50000 H34B 2 0.635536 0.140034 0.530324 11.00000 -1.50000 H34C 2 0.580693 0.062934 0.516594 11.00000 -1.50000 AFIX 0 C28 1 0.280703 -0.067630 0.349803 11.00000 0.04425 0.01998 = 0.02629 -0.00536 -0.01056 0.00854 AFIX 137 H28A 2 0.339034 -0.086844 0.362656 11.00000 -1.50000 H28B 2 0.257598 -0.088344 0.313585 11.00000 -1.50000 H28C 2 0.244563 -0.083974 0.374840 11.00000 -1.50000 AFIX 0 C3S 1 0.751614 0.134440 0.434184 11.00000 0.04459 0.04079 = 0.02217 -0.01319 0.00944 -0.01498 AFIX 43 H3S 2 0.723568 0.114813 0.399953 11.00000 -1.20000 AFIX 0 C4S 1 0.731236 0.206340 0.451527 11.00000 0.02793 0.03525 = 0.02603 0.00034 0.00664 -0.00165 AFIX 43 H4S 2 0.688991 0.237269 0.429336 11.00000 -1.20000 AFIX 0 C45 1 0.355104 0.615546 0.328138 11.00000 0.04275 0.02875 = 0.04379 -0.00128 0.02863 0.00062 AFIX 137 H45A 2 0.409361 0.634260 0.349790 11.00000 -1.50000 H45B 2 0.347172 0.636265 0.291266 11.00000 -1.50000 H45C 2 0.356063 0.559259 0.326741 11.00000 -1.50000 AFIX 0 C58 1 0.049213 0.604509 0.145084 11.00000 0.04197 0.01866 = 0.04976 0.00618 0.01690 0.00156 AFIX 137 H58A 2 0.052518 0.569616 0.115036 11.00000 -1.50000 H58B 2 0.082379 0.651077 0.141899 11.00000 -1.50000 H58C 2 -0.010659 0.618389 0.143795 11.00000 -1.50000 AFIX 0 C35 1 0.512540 0.243910 0.491704 11.00000 0.03349 0.01655 = 0.08883 -0.00868 0.00221 -0.00835 AFIX 137 H35A 2 0.475575 0.269580 0.460957 11.00000 -1.50000 H35B 2 0.569759 0.266911 0.498047 11.00000 -1.50000 H35C 2 0.488310 0.250066 0.524193 11.00000 -1.50000 AFIX 0 C57 1 0.179034 0.542427 0.201331 11.00000 0.03265 0.05677 = 0.04448 0.01522 0.00184 -0.02239 AFIX 137 H57A 2 0.201245 0.516160 0.235752 11.00000 -1.50000 H57B 2 0.212996 0.588751 0.198932 11.00000 -1.50000 H57C 2 0.182720 0.507956 0.171120 11.00000 -1.50000 AFIX 0 C23 1 0.694400 0.264385 0.305289 11.00000 0.02425 0.05617 = 0.03223 -0.00014 -0.00196 -0.00403 AFIX 137 H23A 2 0.701394 0.211280 0.293953 11.00000 -1.50000 H23B 2 0.733699 0.274200 0.339938 11.00000 -1.50000 H23C 2 0.707160 0.299785 0.277731 11.00000 -1.50000 AFIX 0 C22 1 0.591879 0.356536 0.334606 11.00000 0.05712 0.03591 = 0.03737 -0.01837 -0.00676 0.00246 AFIX 137 H22A 2 0.605975 0.395580 0.309785 11.00000 -1.50000 H22B 2 0.630215 0.362002 0.370137 11.00000 -1.50000 H22C 2 0.532494 0.363325 0.338490 11.00000 -1.50000 AFIX 0 PART 1 C11S 1 0.070109 0.109163 0.506330 41.00000 0.04280 0.02486 = 0.04466 -0.00218 0.01959 -0.00216 AFIX 43 H11S 2 0.049449 0.066393 0.484009 41.00000 -1.20000 AFIX 0 C13S 1 0.084862 0.243222 0.515537 41.00000 0.04355 0.02721 = 0.05917 -0.00111 0.02495 -0.00199 AFIX 43 H13S 2 0.075908 0.293912 0.501487 41.00000 -1.20000 AFIX 0 C16 1 0.372282 0.070638 0.141314 31.00000 0.03618 0.02632 = 0.06733 -0.01829 0.01127 -0.01592 AFIX 137 H16A 2 0.347275 0.103246 0.110395 31.00000 -1.50000 H16B 2 0.337487 0.024169 0.141022 31.00000 -1.50000 H16C 2 0.430635 0.056200 0.138705 31.00000 -1.50000 AFIX 0 C12S 1 0.056270 0.181558 0.483921 41.00000 0.04014 0.03754 = 0.04673 0.00786 0.00823 -0.00108 AFIX 43 H12S 2 0.027456 0.188125 0.447285 41.00000 -1.20000 AFIX 0 C15S 1 0.138365 0.156537 0.587043 41.00000 0.06968 0.05431 = 0.03210 -0.00227 0.02473 -0.00933 AFIX 43 H15S 2 0.167777 0.148674 0.623416 41.00000 -1.20000 AFIX 0 C14S 1 0.126382 0.231315 0.567461 41.00000 0.06246 0.04000 = 0.05071 -0.01409 0.03089 -0.01301 AFIX 43 H14S 2 0.147078 0.273632 0.590234 41.00000 -1.20000 AFIX 0 C15 1 0.278708 0.144102 0.192766 31.00000 0.03618 0.02632 = 0.06733 -0.01829 0.01127 -0.01592 AFIX 137 H15A 2 0.280680 0.175164 0.225457 31.00000 -1.50000 H15B 2 0.240081 0.100392 0.193067 31.00000 -1.50000 H15C 2 0.257820 0.175689 0.160562 31.00000 -1.50000 AFIX 0 PART 0 PART 2 F2 3 0.286020 0.331698 0.476347 21.00000 0.04976 0.03280 = 0.05227 0.00004 0.02711 -0.00113 F1 3 0.122517 0.331157 0.414202 21.00000 0.04976 0.03280 = 0.05227 0.00004 0.02711 -0.00113 AFIX 66 C7S 1 0.170028 0.249083 0.566302 -41.00000 0.07013 0.03801 = 0.06001 0.01778 0.04201 0.00964 AFIX 43 H7S 2 0.193311 0.299518 0.570118 -41.00000 -1.20000 AFIX 65 C8S 1 0.198561 0.194003 0.605849 -41.00000 0.06437 0.03983 = 0.05945 0.02064 0.03879 0.00258 AFIX 43 H8S 2 0.241345 0.206793 0.636694 -41.00000 -1.20000 AFIX 65 C9S 1 0.164493 0.120209 0.600266 -41.00000 0.05683 0.03564 = 0.06345 0.01930 0.04248 0.00838 AFIX 43 H9S 2 0.183994 0.082564 0.627295 -41.00000 -1.20000 AFIX 65 C10S 1 0.101893 0.101495 0.555136 -41.00000 0.05842 0.04039 = 0.06183 0.01850 0.04326 0.00579 AFIX 43 H10S 2 0.078610 0.051060 0.551320 -41.00000 -1.20000 AFIX 65 N2S 5 0.073359 0.156575 0.515588 -41.00000 0.06321 0.04387 = 0.06375 0.01847 0.04555 0.00857 C6S 1 0.107426 0.230369 0.521171 -41.00000 0.06098 0.04061 = 0.05635 0.01771 0.04719 0.01030 AFIX 43 H6S 2 0.087925 0.268013 0.494142 -41.00000 -1.20000 AFIX 0 C15A 1 0.291211 0.119072 0.190972 -31.00000 0.03618 0.02632 = 0.06733 -0.01829 0.01127 -0.01592 AFIX 137 H15D 2 0.283353 0.143359 0.224718 -31.00000 -1.50000 H15E 2 0.264965 0.067907 0.187818 -31.00000 -1.50000 H15F 2 0.264042 0.150717 0.160026 -31.00000 -1.50000 AFIX 0 C16A 1 0.397761 0.068752 0.138931 -31.00000 0.03618 0.02632 = 0.06733 -0.01829 0.01127 -0.01592 AFIX 137 H16D 2 0.393344 0.105154 0.108790 -31.00000 -1.50000 H16E 2 0.357673 0.026200 0.128115 -31.00000 -1.50000 H16F 2 0.456252 0.048621 0.148399 -31.00000 -1.50000 AFIX 0 HKLF 4 REM JFig1141_P21c_a.res in P2(1)/c REM R1 = 0.0445 for 10944 Fo > 4sig(Fo) and 0.0585 for all 13552 data REM 838 parameters refined using 72 restraints END WGHT 0.0678 10.8985 REM Highest difference peak 0.672, deepest hole -1.205, 1-sigma level 0.088 Q1 1 0.1897 0.2636 0.3783 11.00000 0.05 0.67 Q2 1 0.2769 0.2912 0.4625 11.00000 0.05 0.65 Q3 1 0.2358 0.2945 0.3726 11.00000 0.05 0.65 Q4 1 0.2834 0.3409 0.3582 11.00000 0.05 0.58 Q5 1 0.2595 0.3158 0.3385 11.00000 0.05 0.58 Q6 1 0.1787 0.2927 0.2528 11.00000 0.05 0.55 Q7 1 0.2918 0.3228 0.3274 11.00000 0.05 0.51 Q8 1 0.2795 0.1390 0.1634 11.00000 0.05 0.51 Q9 1 0.3157 0.4053 0.2611 11.00000 0.05 0.50 Q10 1 0.2699 0.3418 0.3138 11.00000 0.05 0.49 Q11 1 0.4625 0.1116 0.3564 11.00000 0.05 0.49 Q12 1 0.1894 0.2540 0.4401 11.00000 0.05 0.49 Q13 1 0.4707 0.1311 0.3100 11.00000 0.05 0.49 Q14 1 0.5481 0.0394 0.3118 11.00000 0.05 0.46 Q15 1 0.1185 0.5663 0.3628 11.00000 0.05 0.46 Q16 1 0.1730 0.5416 0.4835 11.00000 0.05 0.45 Q17 1 0.1626 0.5909 0.3999 11.00000 0.05 0.45 Q18 1 0.4254 0.0855 0.3973 11.00000 0.05 0.45 Q19 1 0.0361 0.4646 0.1925 11.00000 0.05 0.45 Q20 1 0.4989 0.1675 0.2703 11.00000 0.05 0.45 ; _shelx_res_checksum 32700 _shelx_shelxl_version_number 2014/7 _olex2_submission_original_sample_id JFig1141 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Sb1 Sb 0.22946(2) 0.28032(2) 0.41581(2) 0.02982(9) Uani 1 1 d . . . . . Mn1 Mn 0.28054(3) 0.34108(2) 0.33312(2) 0.01347(11) Uani 1 1 d . . . . . N1 N 0.39493(14) 0.20020(13) 0.33385(9) 0.0113(5) Uani 1 1 d . . . . . N2 N 0.15810(14) 0.47343(13) 0.34162(9) 0.0115(5) Uani 1 1 d . . . . . F1A F 0.1398(2) 0.35360(19) 0.42359(15) 0.0426(6) Uani 0.785(4) 1 d . . P A 1 O1 O 0.13685(17) 0.25852(15) 0.26271(12) 0.0427(7) Uani 1 1 d . . . . . C6 C 0.45115(16) 0.13848(15) 0.33391(10) 0.0100(5) Uani 1 1 d . . . . . O2 O 0.41631(17) 0.41792(16) 0.41490(14) 0.0528(8) Uani 1 1 d . . . . . C7 C 0.45579(16) 0.08276(15) 0.37464(10) 0.0099(5) Uani 1 1 d . . . . . C36 C 0.10194(16) 0.53473(15) 0.34293(11) 0.0105(5) Uani 1 1 d . . . . . C11 C 0.49985(17) 0.13505(15) 0.29373(10) 0.0107(5) Uani 1 1 d . . . . . O3 O 0.3407(2) 0.40625(18) 0.24034(15) 0.0622(10) Uani 1 1 d . . . . . N1S N 0.83351(19) 0.19194(17) 0.53474(11) 0.0300(6) Uani 1 1 d . . . . . C5 C 0.35125(17) 0.25323(16) 0.33399(11) 0.0123(5) Uani 1 1 d . . . . . C24 C 0.39968(17) 0.08686(15) 0.41541(10) 0.0104(5) Uani 1 1 d . . . . . C32 C 0.43073(18) 0.12128(15) 0.46601(11) 0.0141(6) Uani 1 1 d . . . . . C41 C 0.12377(17) 0.59009(15) 0.38398(10) 0.0108(5) Uani 1 1 d . . . . . C4 C 0.20478(17) 0.42363(16) 0.33830(11) 0.0124(5) Uani 1 1 d . . . . . C33 C 0.51872(18) 0.15870(16) 0.47914(11) 0.0162(6) Uani 1 1 d . . . . . H33 H 0.5443 0.1543 0.4462 0.019 Uiso 1 1 calc R . . . . C39 C -0.00321(19) 0.65974(16) 0.34200(12) 0.0175(6) Uani 1 1 d . . . . . H39 H -0.0397 0.7030 0.3416 0.021 Uiso 1 1 calc R . . . . C62 C -0.03302(17) 0.41236(16) 0.26643(11) 0.0139(6) Uani 1 1 d . . . . . C40 C 0.06988(18) 0.65289(16) 0.38264(11) 0.0142(6) Uani 1 1 d . . . . . H40 H 0.0830 0.6916 0.4097 0.017 Uiso 1 1 calc R . . . . C10 C 0.55631(18) 0.07357(16) 0.29554(11) 0.0148(6) Uani 1 1 d . . . . . H10 H 0.5897 0.0690 0.2685 0.018 Uiso 1 1 calc R . . . . C25 C 0.31720(17) 0.05522(16) 0.40264(11) 0.0141(6) Uani 1 1 d . . . . . C9 C 0.56417(19) 0.01880(16) 0.33663(12) 0.0170(6) Uani 1 1 d . . . . . H9 H 0.6040 -0.0221 0.3380 0.020 Uiso 1 1 calc R . . . . C42 C 0.20630(17) 0.58285(15) 0.42465(11) 0.0118(5) Uani 1 1 d . . . . . C12 C 0.49064(17) 0.19499(15) 0.24990(11) 0.0117(5) Uani 1 1 d . . . . . F2A F 0.14458(19) 0.21155(15) 0.37939(12) 0.0426(6) Uani 0.785(4) 1 d . . P A 1 C13 C 0.43290(19) 0.18299(17) 0.20080(11) 0.0176(6) Uani 1 1 d . . . . . C43 C 0.28268(18) 0.60565(16) 0.40910(12) 0.0152(6) Uani 1 1 d . . . . . C38 C -0.02330(18) 0.60390(16) 0.30206(11) 0.0162(6) Uani 1 1 d . . . . . H38 H -0.0734 0.6095 0.2745 0.019 Uiso 1 1 calc R . . . . C37 C 0.02882(17) 0.53978(15) 0.30170(11) 0.0122(5) Uani 1 1 d . . . . . C8 C 0.51445(18) 0.02342(16) 0.37546(11) 0.0141(6) Uani 1 1 d . . . . . H8 H 0.5204 -0.0145 0.4031 0.017 Uiso 1 1 calc R . . . . C26 C 0.28213(18) 0.02013(17) 0.34720(11) 0.0178(6) Uani 1 1 d . . . . . H26 H 0.3213 0.0351 0.3227 0.021 Uiso 1 1 calc R . . . . C44 C 0.2814(2) 0.64183(17) 0.35405(12) 0.0193(6) Uani 1 1 d . . . . . H44 H 0.2268 0.6260 0.3294 0.023 Uiso 1 1 calc R . . . . C61 C -0.05413(19) 0.36008(17) 0.22372(12) 0.0190(6) Uani 1 1 d . . . . . H61 H -0.0837 0.3142 0.2288 0.023 Uiso 1 1 calc R . . . . C20 C 0.54026(18) 0.26204(16) 0.25878(11) 0.0155(6) Uani 1 1 d . . . . . C59 C 0.0118(2) 0.44005(17) 0.16663(12) 0.0204(6) Uani 1 1 d . . . . . H59 H 0.0279 0.4485 0.1328 0.025 Uiso 1 1 calc R . . . . C30 C 0.2981(2) 0.08828(19) 0.49263(12) 0.0233(7) Uani 1 1 d . . . . . H30 H 0.2636 0.0881 0.5192 0.028 Uiso 1 1 calc R . . . . C51 C 0.1258(2) 0.53146(18) 0.49519(12) 0.0213(6) Uani 1 1 d . . . . . H51 H 0.0815 0.5185 0.4622 0.026 Uiso 1 1 calc R . . . . C29 C 0.26774(19) 0.05605(19) 0.44232(12) 0.0219(6) Uani 1 1 d . . . . . H29 H 0.2121 0.0340 0.4345 0.026 Uiso 1 1 calc R . . . . C54 C 0.00984(17) 0.48051(16) 0.25760(11) 0.0132(5) Uani 1 1 d . . . . . C60 C -0.0325(2) 0.37422(17) 0.17403(12) 0.0200(6) Uani 1 1 d . . . . . H60 H -0.0483 0.3386 0.1451 0.024 Uiso 1 1 calc R . . . . C50 C 0.20759(18) 0.55351(16) 0.47677(12) 0.0167(6) Uani 1 1 d . . . . . C31 C 0.37874(19) 0.12080(17) 0.50413(11) 0.0190(6) Uani 1 1 d . . . . . H31 H 0.3991 0.1433 0.5387 0.023 Uiso 1 1 calc R . . . . C21 C 0.6027(2) 0.27664(17) 0.31188(12) 0.0201(6) Uani 1 1 d . . . . . H21 H 0.5907 0.2381 0.3388 0.024 Uiso 1 1 calc R . . . . C55 C 0.03346(19) 0.49434(17) 0.20782(12) 0.0185(6) Uani 1 1 d . . . . . C17 C 0.4276(2) 0.23828(18) 0.16011(12) 0.0220(7) Uani 1 1 d . . . . . H17 H 0.3889 0.2308 0.1264 0.026 Uiso 1 1 calc R . . . . C18 C 0.4774(2) 0.30354(18) 0.16791(12) 0.0217(6) Uani 1 1 d . . . . . H18 H 0.4734 0.3403 0.1396 0.026 Uiso 1 1 calc R . . . . C47 C 0.35983(19) 0.59802(17) 0.44675(13) 0.0216(6) Uani 1 1 d . . . . . H47 H 0.4118 0.6128 0.4368 0.026 Uiso 1 1 calc R . . . . C63 C -0.05965(19) 0.39738(16) 0.31992(12) 0.0177(6) Uani 1 1 d . . . . . H63 H -0.0173 0.4238 0.3490 0.021 Uiso 1 1 calc R . . . . N3S N 0.1100(4) 0.0953(3) 0.55653(18) 0.0386(17) Uani 0.877(8) 1 d . U P B 1 C49 C 0.2866(2) 0.54784(18) 0.51276(13) 0.0242(7) Uani 1 1 d . . . . . H49 H 0.2887 0.5286 0.5483 0.029 Uiso 1 1 calc R . . . . C19 C 0.5329(2) 0.31540(17) 0.21678(12) 0.0200(6) Uani 1 1 d . . . . . H19 H 0.5667 0.3608 0.2220 0.024 Uiso 1 1 calc R . . . . C1 C 0.1900(2) 0.28917(18) 0.28930(14) 0.0242(7) Uani 1 1 d . . . . . C5S C 0.7733(2) 0.23201(19) 0.50146(13) 0.0262(7) Uani 1 1 d . . . . . H5S H 0.7587 0.2813 0.5130 0.031 Uiso 1 1 calc R . . . . C48 C 0.3618(2) 0.56967(19) 0.49768(14) 0.0262(7) Uani 1 1 d . . . . . H48 H 0.4148 0.5650 0.5227 0.031 Uiso 1 1 calc R . . . . C1S C 0.8518(2) 0.1229(2) 0.51719(15) 0.0328(8) Uani 1 1 d . . . . . H1S H 0.8941 0.0930 0.5403 0.039 Uiso 1 1 calc R . . . . C56 C 0.0854(2) 0.56497(19) 0.19850(13) 0.0298(8) Uani 1 1 d . . . . . H56 H 0.0837 0.6024 0.2284 0.036 Uiso 1 1 calc R . . . . C64 C -0.1478(2) 0.43351(19) 0.31913(14) 0.0269(7) Uani 1 1 d . . . . . H64A H -0.1443 0.4894 0.3149 0.040 Uiso 1 1 calc GR . . . . H64B H -0.1657 0.4218 0.3532 0.040 Uiso 1 1 calc GR . . . . H64C H -0.1897 0.4124 0.2887 0.040 Uiso 1 1 calc GR . . . . C14 C 0.3744(2) 0.1126(2) 0.19145(13) 0.0341(9) Uani 1 1 d . . . . . H14 H 0.3924 0.0764 0.2225 0.041 Uiso 0.64(3) 1 calc R . P C 1 H14A H 0.3968 0.0779 0.2228 0.041 Uiso 0.36(3) 1 calc R . P C 2 C53 C 0.0933(2) 0.6005(2) 0.52319(14) 0.0287(7) Uani 1 1 d . . . . . H53A H 0.1369 0.6158 0.5547 0.043 Uiso 1 1 calc GR . . . . H53B H 0.0406 0.5863 0.5350 0.043 Uiso 1 1 calc GR . . . . H53C H 0.0816 0.6436 0.4977 0.043 Uiso 1 1 calc GR . . . . C46 C 0.2807(3) 0.72976(19) 0.35829(14) 0.0318(8) Uani 1 1 d . . . . . H46A H 0.2307 0.7461 0.3724 0.048 Uiso 1 1 calc GR . . . . H46B H 0.2778 0.7522 0.3223 0.048 Uiso 1 1 calc GR . . . . H46C H 0.3330 0.7471 0.3828 0.048 Uiso 1 1 calc GR . . . . C3 C 0.3190(2) 0.38295(19) 0.27404(17) 0.0340(9) Uani 1 1 d . . . . . C65 C -0.0600(2) 0.31212(18) 0.33480(13) 0.0244(7) Uani 1 1 d . . . . . H65A H -0.1056 0.2857 0.3093 0.037 Uiso 1 1 calc GR . . . . H65B H -0.0702 0.3068 0.3717 0.037 Uiso 1 1 calc GR . . . . H65C H -0.0046 0.2892 0.3329 0.037 Uiso 1 1 calc GR . . . . C2 C 0.3643(2) 0.38867(18) 0.38408(16) 0.0298(8) Uani 1 1 d . . . . . C52 C 0.1369(2) 0.4616(2) 0.53310(14) 0.0297(8) Uani 1 1 d . . . . . H52A H 0.1633 0.4194 0.5166 0.045 Uiso 1 1 calc GR . . . . H52B H 0.0809 0.4452 0.5391 0.045 Uiso 1 1 calc GR . . . . H52C H 0.1737 0.4754 0.5679 0.045 Uiso 1 1 calc GR . . . . C2S C 0.8139(3) 0.0920(2) 0.46801(15) 0.0343(9) Uani 1 1 d . . . . . H2S H 0.8299 0.0426 0.4575 0.041 Uiso 1 1 calc R . . . . C27 C 0.1934(2) 0.0500(2) 0.32221(15) 0.0361(9) Uani 1 1 d . . . . . H27A H 0.1532 0.0352 0.3451 0.054 Uiso 1 1 calc GR . . . . H27B H 0.1747 0.0280 0.2859 0.054 Uiso 1 1 calc GR . . . . H27C H 0.1951 0.1062 0.3196 0.054 Uiso 1 1 calc GR . . . . C34 C 0.5781(2) 0.1177(2) 0.52530(14) 0.0342(9) Uani 1 1 d . . . . . H34A H 0.5564 0.1236 0.5588 0.051 Uiso 1 1 calc GR . . . . H34B H 0.6355 0.1400 0.5303 0.051 Uiso 1 1 calc GR . . . . H34C H 0.5807 0.0629 0.5166 0.051 Uiso 1 1 calc GR . . . . C28 C 0.2807(2) -0.06763(19) 0.34980(14) 0.0327(8) Uani 1 1 d . . . . . H28A H 0.3390 -0.0868 0.3627 0.049 Uiso 1 1 calc GR . . . . H28B H 0.2576 -0.0883 0.3136 0.049 Uiso 1 1 calc GR . . . . H28C H 0.2446 -0.0840 0.3748 0.049 Uiso 1 1 calc GR . . . . C3S C 0.7516(3) 0.1344(2) 0.43418(14) 0.0355(9) Uani 1 1 d . . . . . H3S H 0.7236 0.1148 0.4000 0.043 Uiso 1 1 calc R . . . . C4S C 0.7312(2) 0.2063(2) 0.45153(14) 0.0296(8) Uani 1 1 d . . . . . H4S H 0.6890 0.2373 0.4293 0.035 Uiso 1 1 calc R . . . . C45 C 0.3551(2) 0.6155(2) 0.32814(16) 0.0356(9) Uani 1 1 d . . . . . H45A H 0.4094 0.6343 0.3498 0.053 Uiso 1 1 calc GR . . . . H45B H 0.3472 0.6363 0.2913 0.053 Uiso 1 1 calc GR . . . . H45C H 0.3561 0.5593 0.3267 0.053 Uiso 1 1 calc GR . . . . C58 C 0.0492(3) 0.6045(2) 0.14508(16) 0.0357(8) Uani 1 1 d . . . . . H58A H 0.0525 0.5696 0.1150 0.054 Uiso 1 1 calc GR . . . . H58B H 0.0824 0.6511 0.1419 0.054 Uiso 1 1 calc GR . . . . H58C H -0.0107 0.6184 0.1438 0.054 Uiso 1 1 calc GR . . . . C35 C 0.5125(3) 0.2439(2) 0.4917(2) 0.0478(11) Uani 1 1 d . . . . . H35A H 0.4756 0.2696 0.4610 0.072 Uiso 1 1 calc GR . . . . H35B H 0.5698 0.2669 0.4980 0.072 Uiso 1 1 calc GR . . . . H35C H 0.4883 0.2501 0.5242 0.072 Uiso 1 1 calc GR . . . . C57 C 0.1790(2) 0.5424(3) 0.20133(17) 0.0455(11) Uani 1 1 d . . . . . H57A H 0.2012 0.5162 0.2358 0.068 Uiso 1 1 calc GR . . . . H57B H 0.2130 0.5888 0.1989 0.068 Uiso 1 1 calc GR . . . . H57C H 0.1827 0.5080 0.1711 0.068 Uiso 1 1 calc GR . . . . C23 C 0.6944(2) 0.2644(3) 0.30529(15) 0.0386(9) Uani 1 1 d . . . . . H23A H 0.7014 0.2113 0.2940 0.058 Uiso 1 1 calc GR . . . . H23B H 0.7337 0.2742 0.3399 0.058 Uiso 1 1 calc GR . . . . H23C H 0.7072 0.2998 0.2777 0.058 Uiso 1 1 calc GR . . . . C22 C 0.5919(3) 0.3565(2) 0.33461(16) 0.0458(10) Uani 1 1 d . . . . . H22A H 0.6060 0.3956 0.3098 0.069 Uiso 1 1 calc GR . . . . H22B H 0.6302 0.3620 0.3701 0.069 Uiso 1 1 calc GR . . . . H22C H 0.5325 0.3633 0.3385 0.069 Uiso 1 1 calc GR . . . . C11S C 0.0701(3) 0.1092(3) 0.50633(19) 0.0359(11) Uani 0.877(8) 1 d . U P B 1 H11S H 0.0494 0.0664 0.4840 0.043 Uiso 0.877(8) 1 calc R . P B 1 C13S C 0.0849(4) 0.2432(3) 0.5155(2) 0.0412(13) Uani 0.877(8) 1 d . U P B 1 H13S H 0.0759 0.2939 0.5015 0.049 Uiso 0.877(8) 1 calc R . P B 1 C16 C 0.3723(9) 0.0706(8) 0.1413(4) 0.0432(15) Uani 0.64(3) 1 d . . P C 1 H16A H 0.3473 0.1032 0.1104 0.065 Uiso 0.64(3) 1 calc GR . P C 1 H16B H 0.3375 0.0242 0.1410 0.065 Uiso 0.64(3) 1 calc GR . P C 1 H16C H 0.4306 0.0562 0.1387 0.065 Uiso 0.64(3) 1 calc GR . P C 1 C12S C 0.0563(3) 0.1816(3) 0.4839(2) 0.0416(12) Uani 0.877(8) 1 d . U P B 1 H12S H 0.0275 0.1881 0.4473 0.050 Uiso 0.877(8) 1 calc R . P B 1 C15S C 0.1384(4) 0.1565(3) 0.5870(2) 0.0500(14) Uani 0.877(8) 1 d . U P B 1 H15S H 0.1678 0.1487 0.6234 0.060 Uiso 0.877(8) 1 calc R . P B 1 C14S C 0.1264(4) 0.2313(3) 0.5675(2) 0.0483(14) Uani 0.877(8) 1 d . U P B 1 H14S H 0.1471 0.2736 0.5902 0.058 Uiso 0.877(8) 1 calc R . P B 1 C15 C 0.2787(8) 0.1441(7) 0.1928(4) 0.0432(15) Uani 0.64(3) 1 d . . P C 1 H15A H 0.2807 0.1752 0.2255 0.065 Uiso 0.64(3) 1 calc GR . P C 1 H15B H 0.2401 0.1004 0.1931 0.065 Uiso 0.64(3) 1 calc GR . P C 1 H15C H 0.2578 0.1757 0.1606 0.065 Uiso 0.64(3) 1 calc GR . P C 1 F2 F 0.2860(7) 0.3317(6) 0.4763(4) 0.0426(6) Uani 0.215(4) 1 d . . P A 2 F1 F 0.1225(9) 0.3312(7) 0.4142(6) 0.0426(6) Uani 0.215(4) 1 d . . P A 2 C7S C 0.170(2) 0.2491(11) 0.5663(11) 0.052(9) Uani 0.123(8) 1 d . U P B 2 H7S H 0.1933 0.2995 0.5701 0.062 Uiso 0.123(8) 1 calc R . P B 2 C8S C 0.1986(17) 0.1940(14) 0.6058(9) 0.051(9) Uani 0.123(8) 1 d G U P B 2 H8S H 0.2413 0.2068 0.6367 0.061 Uiso 0.123(8) 1 calc R . P B 2 C9S C 0.1645(18) 0.1202(13) 0.6003(11) 0.048(8) Uani 0.123(8) 1 d G U P B 2 H9S H 0.1840 0.0826 0.6273 0.057 Uiso 0.123(8) 1 calc R . P B 2 C10S C 0.1019(19) 0.1015(14) 0.5551(13) 0.049(15) Uani 0.123(8) 1 d G U P B 2 H10S H 0.0786 0.0511 0.5513 0.059 Uiso 0.123(8) 1 calc R . P B 2 N2S N 0.0734(16) 0.1566(18) 0.5156(11) 0.052(8) Uani 0.123(8) 1 d G U P B 2 C6S C 0.1074(19) 0.2304(16) 0.5212(10) 0.048(10) Uani 0.123(8) 1 d G U P B 2 H6S H 0.0879 0.2680 0.4941 0.057 Uiso 0.123(8) 1 calc R . P B 2 C15A C 0.2912(13) 0.1191(13) 0.1910(7) 0.0432(15) Uani 0.36(3) 1 d . . P C 2 H15D H 0.2834 0.1434 0.2247 0.065 Uiso 0.36(3) 1 calc GR . P C 2 H15E H 0.2650 0.0679 0.1878 0.065 Uiso 0.36(3) 1 calc GR . P C 2 H15F H 0.2640 0.1507 0.1600 0.065 Uiso 0.36(3) 1 calc GR . P C 2 C16A C 0.3978(13) 0.0688(15) 0.1389(9) 0.0432(15) Uani 0.36(3) 1 d . . P C 2 H16D H 0.3933 0.1052 0.1088 0.065 Uiso 0.36(3) 1 calc GR . P C 2 H16E H 0.3577 0.0262 0.1281 0.065 Uiso 0.36(3) 1 calc GR . P C 2 H16F H 0.4563 0.0486 0.1484 0.065 Uiso 0.36(3) 1 calc GR . P C 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 Sb1 0.03016(14) 0.03194(15) 0.02921(14) 0.00856(10) 0.01044(10) 0.00946(10) Mn1 0.0119(2) 0.0083(2) 0.0203(2) -0.00088(16) 0.00336(17) 0.00404(16) N1 0.0112(11) 0.0095(11) 0.0134(11) -0.0004(9) 0.0027(9) 0.0013(9) N2 0.0115(11) 0.0081(11) 0.0137(11) -0.0020(9) -0.0005(9) 0.0009(9) F1A 0.0498(13) 0.0328(13) 0.0523(13) 0.0000(10) 0.0271(11) -0.0011(10) O1 0.0325(14) 0.0319(15) 0.0542(17) -0.0167(13) -0.0137(13) 0.0100(12) C6 0.0077(12) 0.0081(13) 0.0128(12) -0.0014(10) -0.0010(10) 0.0012(10) O2 0.0279(14) 0.0338(16) 0.083(2) -0.0260(15) -0.0206(15) 0.0066(12) C7 0.0085(12) 0.0084(13) 0.0113(12) -0.0023(10) -0.0010(10) -0.0015(10) C36 0.0106(12) 0.0067(13) 0.0149(13) 0.0007(10) 0.0041(10) 0.0007(10) C11 0.0116(13) 0.0070(13) 0.0124(12) -0.0020(10) 0.0001(10) -0.0026(10) O3 0.077(2) 0.0416(18) 0.084(2) 0.0285(17) 0.054(2) 0.0292(16) N1S 0.0331(16) 0.0273(16) 0.0277(15) -0.0062(12) 0.0017(12) -0.0017(13) C5 0.0117(13) 0.0117(14) 0.0132(13) 0.0009(10) 0.0018(10) -0.0028(11) C24 0.0119(13) 0.0067(12) 0.0118(12) 0.0016(10) 0.0008(10) 0.0014(10) C32 0.0175(14) 0.0095(13) 0.0145(13) 0.0020(11) 0.0016(11) 0.0008(11) C41 0.0127(13) 0.0081(13) 0.0116(12) -0.0006(10) 0.0029(10) -0.0010(10) C4 0.0108(13) 0.0121(14) 0.0132(13) -0.0002(10) -0.0004(10) -0.0030(11) C33 0.0185(14) 0.0146(14) 0.0142(13) -0.0002(11) 0.0007(11) -0.0052(11) C39 0.0188(15) 0.0107(14) 0.0208(15) -0.0019(11) -0.0008(12) 0.0072(11) C62 0.0137(13) 0.0096(13) 0.0164(13) 0.0004(11) -0.0014(11) 0.0038(11) C40 0.0195(14) 0.0090(13) 0.0139(13) -0.0039(10) 0.0027(11) 0.0014(11) C10 0.0166(14) 0.0132(14) 0.0160(13) -0.0004(11) 0.0062(11) 0.0017(11) C25 0.0119(13) 0.0121(14) 0.0169(14) 0.0034(11) -0.0007(11) -0.0005(11) C9 0.0181(14) 0.0110(14) 0.0219(15) 0.0034(11) 0.0041(12) 0.0067(11) C42 0.0125(13) 0.0065(13) 0.0148(13) -0.0036(10) -0.0011(11) 0.0011(10) C12 0.0123(13) 0.0096(13) 0.0141(13) 0.0008(10) 0.0050(10) 0.0020(10) F2A 0.0498(13) 0.0328(13) 0.0523(13) 0.0000(10) 0.0271(11) -0.0011(10) C13 0.0213(15) 0.0134(14) 0.0169(14) 0.0015(11) 0.0012(12) -0.0023(12) C43 0.0159(14) 0.0085(13) 0.0208(14) -0.0078(11) 0.0029(11) -0.0018(11) C38 0.0121(13) 0.0153(14) 0.0185(14) -0.0017(11) -0.0032(11) 0.0040(11) C37 0.0129(13) 0.0093(13) 0.0136(13) -0.0011(10) 0.0012(11) 0.0004(10) C8 0.0186(14) 0.0099(13) 0.0122(13) 0.0017(10) -0.0004(11) 0.0026(11) C26 0.0131(14) 0.0216(16) 0.0166(14) 0.0009(12) -0.0017(11) -0.0056(12) C44 0.0212(15) 0.0163(15) 0.0229(15) -0.0052(12) 0.0104(12) -0.0058(12) C61 0.0224(15) 0.0095(14) 0.0227(15) -0.0018(11) -0.0011(12) -0.0007(12) C20 0.0182(14) 0.0138(14) 0.0153(14) -0.0004(11) 0.0059(11) -0.0011(11) C59 0.0267(16) 0.0178(15) 0.0170(14) -0.0043(12) 0.0052(12) 0.0008(13) C30 0.0232(16) 0.0287(18) 0.0215(15) 0.0026(13) 0.0126(13) 0.0008(13) C51 0.0210(15) 0.0258(17) 0.0161(14) 0.0050(12) 0.0016(12) -0.0033(13) C29 0.0130(14) 0.0261(17) 0.0255(16) 0.0029(13) 0.0019(12) -0.0034(12) C54 0.0117(13) 0.0107(13) 0.0156(13) -0.0030(11) -0.0010(11) 0.0036(11) C60 0.0245(16) 0.0125(14) 0.0200(15) -0.0075(12) -0.0026(12) 0.0037(12) C50 0.0180(14) 0.0118(14) 0.0183(14) 0.0003(11) -0.0008(12) -0.0028(11) C31 0.0248(16) 0.0205(16) 0.0121(13) -0.0002(11) 0.0048(12) 0.0001(13) C21 0.0228(15) 0.0189(16) 0.0175(14) -0.0013(12) 0.0017(12) -0.0095(12) C55 0.0206(15) 0.0148(15) 0.0199(14) -0.0058(12) 0.0039(12) -0.0011(12) C17 0.0273(16) 0.0202(16) 0.0162(14) 0.0043(12) -0.0011(13) 0.0007(13) C18 0.0313(17) 0.0161(15) 0.0184(15) 0.0075(12) 0.0067(13) 0.0013(13) C47 0.0131(14) 0.0175(15) 0.0333(17) -0.0089(13) 0.0025(13) -0.0029(12) C63 0.0235(15) 0.0110(14) 0.0169(14) 0.0012(11) -0.0002(12) 0.0017(12) N3S 0.051(3) 0.034(2) 0.037(2) 0.0046(17) 0.023(2) 0.001(2) C49 0.0293(17) 0.0196(16) 0.0184(15) 0.0039(12) -0.0077(13) -0.0011(13) C19 0.0256(16) 0.0120(14) 0.0237(15) 0.0009(12) 0.0084(13) -0.0047(12) C1 0.0238(17) 0.0131(15) 0.0343(18) -0.0012(13) 0.0025(14) 0.0107(13) C5S 0.0302(18) 0.0209(17) 0.0284(17) -0.0058(13) 0.0079(14) -0.0032(14) C48 0.0166(15) 0.0237(17) 0.0315(17) -0.0028(14) -0.0108(13) 0.0013(13) C1S 0.0341(19) 0.031(2) 0.0337(19) 0.0039(15) 0.0088(16) 0.0051(16) C56 0.046(2) 0.0233(17) 0.0239(16) -0.0098(14) 0.0166(15) -0.0143(16) C64 0.0320(18) 0.0230(17) 0.0288(17) 0.0043(14) 0.0132(14) 0.0086(14) C14 0.044(2) 0.0267(19) 0.0223(16) 0.0093(14) -0.0156(15) -0.0186(16) C53 0.0307(18) 0.0300(19) 0.0272(17) 0.0065(14) 0.0100(14) 0.0022(15) C46 0.050(2) 0.0182(17) 0.0294(18) -0.0003(14) 0.0140(16) -0.0003(16) C3 0.0321(19) 0.0160(17) 0.059(2) -0.0001(17) 0.0227(18) 0.0151(15) C65 0.0302(17) 0.0150(16) 0.0284(17) 0.0051(13) 0.0072(14) 0.0013(13) C2 0.0182(16) 0.0140(16) 0.055(2) -0.0074(15) 0.0028(16) 0.0082(13) C52 0.038(2) 0.0251(18) 0.0257(17) 0.0061(14) 0.0059(15) -0.0080(15) C2S 0.049(2) 0.0199(17) 0.041(2) -0.0075(15) 0.0257(18) -0.0073(16) C27 0.034(2) 0.0273(19) 0.0353(19) -0.0090(15) -0.0193(16) 0.0099(16) C34 0.0217(17) 0.043(2) 0.0332(19) 0.0196(16) -0.0047(14) -0.0066(16) C28 0.044(2) 0.0200(17) 0.0263(17) -0.0054(14) -0.0106(15) 0.0085(15) C3S 0.045(2) 0.041(2) 0.0222(17) -0.0132(16) 0.0094(16) -0.0150(18) C4S 0.0279(18) 0.035(2) 0.0260(17) 0.0003(14) 0.0066(14) -0.0016(15) C45 0.043(2) 0.0287(19) 0.044(2) -0.0013(16) 0.0286(18) 0.0006(16) C58 0.042(2) 0.0187(17) 0.050(2) 0.0062(16) 0.0169(18) 0.0016(16) C35 0.033(2) 0.0166(18) 0.089(3) -0.009(2) 0.002(2) -0.0084(16) C57 0.033(2) 0.057(3) 0.044(2) 0.015(2) 0.0018(17) -0.022(2) C23 0.0242(18) 0.056(3) 0.0322(19) -0.0001(18) -0.0020(15) -0.0040(17) C22 0.057(3) 0.036(2) 0.037(2) -0.0184(18) -0.0068(19) 0.002(2) C11S 0.043(2) 0.025(2) 0.045(2) -0.0022(18) 0.0196(19) -0.0022(19) C13S 0.044(3) 0.027(2) 0.059(3) -0.001(2) 0.025(2) -0.002(2) C16 0.036(4) 0.026(2) 0.067(2) -0.018(2) 0.011(2) -0.016(4) C12S 0.040(3) 0.038(2) 0.047(3) 0.008(2) 0.008(2) -0.001(2) C15S 0.070(4) 0.054(3) 0.032(2) -0.002(2) 0.025(2) -0.009(3) C14S 0.062(3) 0.040(3) 0.051(3) -0.014(2) 0.031(2) -0.013(2) C15 0.036(4) 0.026(2) 0.067(2) -0.018(2) 0.011(2) -0.016(4) F2 0.0498(13) 0.0328(13) 0.0523(13) 0.0000(10) 0.0271(11) -0.0011(10) F1 0.0498(13) 0.0328(13) 0.0523(13) 0.0000(10) 0.0271(11) -0.0011(10) C7S 0.070(18) 0.038(12) 0.060(14) 0.018(10) 0.042(13) 0.010(11) C8S 0.064(16) 0.040(12) 0.059(14) 0.021(10) 0.039(12) 0.003(11) C9S 0.057(16) 0.036(12) 0.063(16) 0.019(10) 0.042(12) 0.008(11) C10S 0.06(2) 0.040(14) 0.062(19) 0.019(12) 0.043(16) 0.006(13) N2S 0.063(15) 0.044(13) 0.064(15) 0.018(11) 0.046(12) 0.009(11) C6S 0.06(2) 0.041(13) 0.056(15) 0.018(11) 0.047(12) 0.010(11) C15A 0.036(4) 0.026(2) 0.067(2) -0.018(2) 0.011(2) -0.016(4) C16A 0.036(4) 0.026(2) 0.067(2) -0.018(2) 0.011(2) -0.016(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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' Sb Sb -0.5866 1.5461 '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 F1A Sb1 Mn1 99.81(10) F2A Sb1 Mn1 100.27(8) F2A Sb1 F1A 89.68(13) F2 Sb1 Mn1 106.5(3) F2 Sb1 F1 94.4(5) F1 Sb1 Mn1 102.6(4) C5 Mn1 Sb1 86.96(8) C5 Mn1 C4 173.72(11) C4 Mn1 Sb1 86.79(8) C1 Mn1 Sb1 86.85(11) C1 Mn1 C5 90.25(12) C1 Mn1 C4 88.81(12) C1 Mn1 C3 93.37(16) C3 Mn1 Sb1 178.74(10) C3 Mn1 C5 91.80(12) C3 Mn1 C4 94.46(12) C2 Mn1 Sb1 85.82(12) C2 Mn1 C5 90.48(12) C2 Mn1 C4 89.67(12) C2 Mn1 C1 172.59(16) C2 Mn1 C3 93.98(17) C5 N1 C6 177.2(3) C4 N2 C36 177.1(3) N1 C6 C7 118.0(2) C11 C6 N1 118.9(2) C11 C6 C7 123.1(2) C6 C7 C24 121.3(2) C8 C7 C6 117.3(2) C8 C7 C24 121.4(2) N2 C36 C41 118.5(2) C37 C36 N2 118.2(2) C37 C36 C41 123.2(2) C6 C11 C12 121.1(2) C10 C11 C6 117.5(2) C10 C11 C12 121.4(2) C1S N1S C5S 116.2(3) N1 C5 Mn1 178.9(2) C32 C24 C7 119.6(2) C25 C24 C7 119.3(2) C25 C24 C32 121.1(2) C24 C32 C33 121.2(2) C31 C32 C24 118.3(3) C31 C32 C33 120.5(3) C36 C41 C42 119.8(2) C40 C41 C36 117.6(2) C40 C41 C42 122.5(2) N2 C4 Mn1 179.4(3) C32 C33 H33 107.6 C32 C33 C35 111.4(3) C34 C33 C32 111.7(2) C34 C33 H33 107.6 C34 C33 C35 110.8(3) C35 C33 H33 107.6 C40 C39 H39 119.7 C38 C39 H39 119.7 C38 C39 C40 120.5(3) C61 C62 C54 118.3(3) C61 C62 C63 120.4(3) C54 C62 C63 121.2(2) C41 C40 C39 120.5(3) C41 C40 H40 119.7 C39 C40 H40 119.7 C11 C10 H10 119.7 C9 C10 C11 120.6(3) C9 C10 H10 119.7 C24 C25 C26 121.3(2) C29 C25 C24 118.3(3) C29 C25 C26 120.4(2) C10 C9 H9 119.7 C8 C9 C10 120.6(3) C8 C9 H9 119.7 C43 C42 C41 118.3(2) C50 C42 C41 120.8(2) C50 C42 C43 120.9(3) C13 C12 C11 119.6(2) C13 C12 C20 120.9(3) C20 C12 C11 119.5(2) C12 C13 C14 121.8(3) C17 C13 C12 118.5(3) C17 C13 C14 119.7(3) C42 C43 C44 121.2(3) C47 C43 C42 118.4(3) C47 C43 C44 120.3(3) C39 C38 H38 119.5 C39 C38 C37 121.0(3) C37 C38 H38 119.5 C36 C37 C54 121.2(2) C38 C37 C36 117.0(2) C38 C37 C54 121.7(2) C7 C8 H8 119.5 C9 C8 C7 121.0(2) C9 C8 H8 119.5 C25 C26 H26 107.7 C25 C26 C28 111.5(2) C27 C26 C25 112.3(3) C27 C26 H26 107.7 C27 C26 C28 109.8(3) C28 C26 H26 107.7 C43 C44 H44 107.5 C43 C44 C46 110.4(2) C43 C44 C45 113.5(3) C46 C44 H44 107.5 C45 C44 H44 107.5 C45 C44 C46 110.2(3) C62 C61 H61 119.5 C60 C61 C62 121.0(3) C60 C61 H61 119.5 C12 C20 C21 121.9(2) C19 C20 C12 118.4(3) C19 C20 C21 119.7(3) C60 C59 H59 119.4 C60 C59 C55 121.2(3) C55 C59 H59 119.4 C29 C30 H30 120.1 C29 C30 C31 119.7(3) C31 C30 H30 120.1 C50 C51 H51 108.0 C50 C51 C53 109.5(3) C50 C51 C52 113.1(3) C53 C51 H51 108.0 C52 C51 H51 108.0 C52 C51 C53 109.9(3) C25 C29 H29 119.4 C30 C29 C25 121.2(3) C30 C29 H29 119.4 C62 C54 C37 119.5(2) C55 C54 C62 120.9(3) C55 C54 C37 119.6(2) C61 C60 H60 120.0 C59 C60 C61 119.9(3) C59 C60 H60 120.0 C42 C50 C51 121.8(3) C49 C50 C42 118.1(3) C49 C50 C51 120.1(3) C32 C31 H31 119.3 C30 C31 C32 121.3(3) C30 C31 H31 119.3 C20 C21 H21 107.6 C20 C21 C23 110.7(3) C20 C21 C22 112.2(3) C23 C21 H21 107.6 C23 C21 C22 110.7(3) C22 C21 H21 107.6 C59 C55 C54 118.6(3) C59 C55 C56 119.4(3) C54 C55 C56 122.0(3) C13 C17 H17 119.4 C18 C17 C13 121.1(3) C18 C17 H17 119.4 C17 C18 H18 120.1 C17 C18 C19 119.9(3) C19 C18 H18 120.1 C43 C47 H47 119.4 C48 C47 C43 121.2(3) C48 C47 H47 119.4 C62 C63 H63 107.5 C62 C63 C64 109.9(2) C62 C63 C65 113.6(2) C64 C63 H63 107.5 C65 C63 H63 107.5 C65 C63 C64 110.5(3) C11S N3S C15S 116.5(5) C50 C49 H49 119.3 C48 C49 C50 121.4(3) C48 C49 H49 119.3 C20 C19 H19 119.4 C18 C19 C20 121.2(3) C18 C19 H19 119.4 O1 C1 Mn1 179.0(3) N1S C5S H5S 118.0 N1S C5S C4S 124.0(3) C4S C5S H5S 118.0 C47 C48 C49 120.1(3) C47 C48 H48 120.0 C49 C48 H48 120.0 N1S C1S H1S 117.8 N1S C1S C2S 124.4(3) C2S C1S H1S 117.8 C55 C56 H56 108.0 C55 C56 C57 110.0(3) C58 C56 C55 112.4(3) C58 C56 H56 108.0 C58 C56 C57 110.4(3) C57 C56 H56 108.0 C63 C64 H64A 109.5 C63 C64 H64B 109.5 C63 C64 H64C 109.5 H64A C64 H64B 109.5 H64A C64 H64C 109.5 H64B C64 H64C 109.5 C13 C14 H14 108.4 C13 C14 H14A 104.7 C13 C14 C15 105.8(4) C13 C14 C16A 105.4(8) C16 C14 C13 116.2(5) C16 C14 H14 108.4 C16 C14 C15 109.3(6) C15 C14 H14 108.4 C15A C14 C13 120.7(10) C15A C14 H14A 104.7 C15A C14 C16A 115.1(9) C16A C14 H14A 104.7 C51 C53 H53A 109.5 C51 C53 H53B 109.5 C51 C53 H53C 109.5 H53A C53 H53B 109.5 H53A C53 H53C 109.5 H53B C53 H53C 109.5 C44 C46 H46A 109.5 C44 C46 H46B 109.5 C44 C46 H46C 109.5 H46A C46 H46B 109.5 H46A C46 H46C 109.5 H46B C46 H46C 109.5 O3 C3 Mn1 179.5(4) C63 C65 H65A 109.5 C63 C65 H65B 109.5 C63 C65 H65C 109.5 H65A C65 H65B 109.5 H65A C65 H65C 109.5 H65B C65 H65C 109.5 O2 C2 Mn1 179.2(4) C51 C52 H52A 109.5 C51 C52 H52B 109.5 C51 C52 H52C 109.5 H52A C52 H52B 109.5 H52A C52 H52C 109.5 H52B C52 H52C 109.5 C1S C2S H2S 120.8 C1S C2S C3S 118.4(3) C3S C2S H2S 120.8 C26 C27 H27A 109.5 C26 C27 H27B 109.5 C26 C27 H27C 109.5 H27A C27 H27B 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C33 C34 H34A 109.5 C33 C34 H34B 109.5 C33 C34 H34C 109.5 H34A C34 H34B 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 C26 C28 H28A 109.5 C26 C28 H28B 109.5 C26 C28 H28C 109.5 H28A C28 H28B 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C2S C3S H3S 120.9 C2S C3S C4S 118.2(3) C4S C3S H3S 120.9 C5S C4S C3S 118.7(3) C5S C4S H4S 120.7 C3S C4S H4S 120.7 C44 C45 H45A 109.5 C44 C45 H45B 109.5 C44 C45 H45C 109.5 H45A C45 H45B 109.5 H45A C45 H45C 109.5 H45B C45 H45C 109.5 C56 C58 H58A 109.5 C56 C58 H58B 109.5 C56 C58 H58C 109.5 H58A C58 H58B 109.5 H58A C58 H58C 109.5 H58B C58 H58C 109.5 C33 C35 H35A 109.5 C33 C35 H35B 109.5 C33 C35 H35C 109.5 H35A C35 H35B 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 C56 C57 H57A 109.5 C56 C57 H57B 109.5 C56 C57 H57C 109.5 H57A C57 H57B 109.5 H57A C57 H57C 109.5 H57B C57 H57C 109.5 C21 C23 H23A 109.5 C21 C23 H23B 109.5 C21 C23 H23C 109.5 H23A C23 H23B 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C21 C22 H22A 109.5 C21 C22 H22B 109.5 C21 C22 H22C 109.5 H22A C22 H22B 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 N3S C11S H11S 117.8 N3S C11S C12S 124.5(5) C12S C11S H11S 117.8 C12S C13S H13S 120.5 C14S C13S H13S 120.5 C14S C13S C12S 119.0(6) C14 C16 H16A 109.5 C14 C16 H16B 109.5 C14 C16 H16C 109.5 H16A C16 H16B 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C11S C12S H12S 120.8 C13S C12S C11S 118.3(5) C13S C12S H12S 120.8 N3S C15S H15S 118.8 N3S C15S C14S 122.4(5) C14S C15S H15S 118.8 C13S C14S C15S 119.3(5) C13S C14S H14S 120.3 C15S C14S H14S 120.3 C14 C15 H15A 109.5 C14 C15 H15B 109.5 C14 C15 H15C 109.5 H15A C15 H15B 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C8S C7S H7S 120.0 C8S C7S C6S 120.0 C6S C7S H7S 120.0 C7S C8S H8S 120.0 C9S C8S C7S 120.0 C9S C8S H8S 120.0 C8S C9S H9S 120.0 C8S C9S C10S 120.0 C10S C9S H9S 120.0 C9S C10S H10S 120.0 C9S C10S N2S 120.0 N2S C10S H10S 120.0 C6S N2S C10S 120.0 C7S C6S H6S 120.0 N2S C6S C7S 120.0 N2S C6S H6S 120.0 C14 C15A H15D 109.5 C14 C15A H15E 109.5 C14 C15A H15F 109.5 H15D C15A H15E 109.5 H15D C15A H15F 109.5 H15E C15A H15F 109.5 C14 C16A H16D 109.5 C14 C16A H16E 109.5 C14 C16A H16F 109.5 H16D C16A H16E 109.5 H16D C16A H16F 109.5 H16E C16A H16F 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Sb1 Mn1 2.6107(5) Sb1 F1A 1.956(4) Sb1 F2A 1.897(3) Sb1 F2 1.837(11) Sb1 F1 1.916(15) Mn1 C5 1.897(3) Mn1 C4 1.899(3) Mn1 C1 1.863(4) Mn1 C3 1.870(4) Mn1 C2 1.849(4) N1 C6 1.399(3) N1 C5 1.157(4) N2 C36 1.398(3) N2 C4 1.157(4) O1 C1 1.104(4) C6 C7 1.402(4) C6 C11 1.398(4) O2 C2 1.134(4) C7 C24 1.496(4) C7 C8 1.391(4) C36 C41 1.404(4) C36 C37 1.398(4) C11 C10 1.393(4) C11 C12 1.504(4) O3 C3 1.061(4) N1S C5S 1.335(5) N1S C1S 1.333(5) C24 C32 1.404(4) C24 C25 1.403(4) C32 C33 1.522(4) C32 C31 1.392(4) C41 C40 1.387(4) C41 C42 1.500(4) C33 H33 1.0000 C33 C34 1.519(4) C33 C35 1.523(5) C39 H39 0.9500 C39 C40 1.391(4) C39 C38 1.388(4) C62 C61 1.396(4) C62 C54 1.409(4) C62 C63 1.516(4) C40 H40 0.9500 C10 H10 0.9500 C10 C9 1.393(4) C25 C26 1.522(4) C25 C29 1.395(4) C9 H9 0.9500 C9 C8 1.382(4) C42 C43 1.412(4) C42 C50 1.405(4) C12 C13 1.399(4) C12 C20 1.402(4) C13 C17 1.395(4) C13 C14 1.529(4) C43 C44 1.519(4) C43 C47 1.399(4) C38 H38 0.9500 C38 C37 1.393(4) C37 C54 1.500(4) C8 H8 0.9500 C26 H26 1.0000 C26 C27 1.519(4) C26 C28 1.528(4) C44 H44 1.0000 C44 C46 1.534(4) C44 C45 1.528(4) C61 H61 0.9500 C61 C60 1.387(4) C20 C21 1.517(4) C20 C19 1.394(4) C59 H59 0.9500 C59 C60 1.379(4) C59 C55 1.393(4) C30 H30 0.9500 C30 C29 1.380(4) C30 C31 1.382(4) C51 H51 1.0000 C51 C50 1.521(4) C51 C53 1.537(5) C51 C52 1.534(4) C29 H29 0.9500 C54 C55 1.402(4) C60 H60 0.9500 C50 C49 1.398(4) C31 H31 0.9500 C21 H21 1.0000 C21 C23 1.522(5) C21 C22 1.526(5) C55 C56 1.527(4) C17 H17 0.9500 C17 C18 1.376(4) C18 H18 0.9500 C18 C19 1.377(4) C47 H47 0.9500 C47 C48 1.369(5) C63 H63 1.0000 C63 C64 1.538(4) C63 C65 1.530(4) N3S C11S 1.317(6) N3S C15S 1.338(7) C49 H49 0.9500 C49 C48 1.384(5) C19 H19 0.9500 C5S H5S 0.9500 C5S C4S 1.374(5) C48 H48 0.9500 C1S H1S 0.9500 C1S C2S 1.372(5) C56 H56 1.0000 C56 C58 1.516(5) C56 C57 1.533(5) C64 H64A 0.9800 C64 H64B 0.9800 C64 H64C 0.9800 C14 H14 1.0000 C14 H14A 1.0000 C14 C16 1.453(12) C14 C15 1.630(15) C14 C15A 1.33(2) C14 C16A 1.63(2) C53 H53A 0.9800 C53 H53B 0.9800 C53 H53C 0.9800 C46 H46A 0.9800 C46 H46B 0.9800 C46 H46C 0.9800 C65 H65A 0.9800 C65 H65B 0.9800 C65 H65C 0.9800 C52 H52A 0.9800 C52 H52B 0.9800 C52 H52C 0.9800 C2S H2S 0.9500 C2S C3S 1.383(6) C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C3S H3S 0.9500 C3S C4S 1.385(5) C4S H4S 0.9500 C45 H45A 0.9800 C45 H45B 0.9800 C45 H45C 0.9800 C58 H58A 0.9800 C58 H58B 0.9800 C58 H58C 0.9800 C35 H35A 0.9800 C35 H35B 0.9800 C35 H35C 0.9800 C57 H57A 0.9800 C57 H57B 0.9800 C57 H57C 0.9800 C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C11S H11S 0.9500 C11S C12S 1.379(7) C13S H13S 0.9500 C13S C12S 1.358(7) C13S C14S 1.356(8) C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 C12S H12S 0.9500 C15S H15S 0.9500 C15S C14S 1.390(8) C14S H14S 0.9500 C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C7S H7S 0.9500 C7S C8S 1.3900 C7S C6S 1.3900 C8S H8S 0.9500 C8S C9S 1.3900 C9S H9S 0.9500 C9S C10S 1.3900 C10S H10S 0.9500 C10S N2S 1.3900 N2S C6S 1.3900 C6S H6S 0.9500 C15A H15D 0.9800 C15A H15E 0.9800 C15A H15F 0.9800 C16A H16D 0.9800 C16A H16E 0.9800 C16A H16F 0.9800 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 N1 C6 C7 C24 2.7(4) N1 C6 C7 C8 -177.5(2) N1 C6 C11 C10 178.9(2) N1 C6 C11 C12 -1.9(4) N2 C36 C41 C40 176.1(2) N2 C36 C41 C42 0.7(4) N2 C36 C37 C38 -176.1(2) N2 C36 C37 C54 1.0(4) C6 C7 C24 C32 -95.3(3) C6 C7 C24 C25 85.6(3) C6 C7 C8 C9 -1.8(4) C6 C11 C10 C9 -1.0(4) C6 C11 C12 C13 -92.2(3) C6 C11 C12 C20 88.0(3) C7 C6 C11 C10 -1.1(4) C7 C6 C11 C12 178.1(2) C7 C24 C32 C33 3.5(4) C7 C24 C32 C31 -176.8(3) C7 C24 C25 C26 -2.9(4) C7 C24 C25 C29 176.6(3) C36 C41 C40 C39 0.4(4) C36 C41 C42 C43 78.7(3) C36 C41 C42 C50 -100.7(3) C36 C37 C54 C62 84.9(3) C36 C37 C54 C55 -96.4(3) C11 C6 C7 C24 -177.3(2) C11 C6 C7 C8 2.5(4) C11 C10 C9 C8 1.7(4) C11 C12 C13 C17 -177.9(3) C11 C12 C13 C14 3.8(4) C11 C12 C20 C21 -0.8(4) C11 C12 C20 C19 177.6(3) N1S C5S C4S C3S 0.2(5) N1S C1S C2S C3S -0.7(5) C24 C7 C8 C9 178.0(3) C24 C32 C33 C34 -116.3(3) C24 C32 C33 C35 119.2(3) C24 C32 C31 C30 -0.8(4) C24 C25 C26 C27 -130.7(3) C24 C25 C26 C28 105.5(3) C24 C25 C29 C30 1.1(4) C32 C24 C25 C26 178.0(3) C32 C24 C25 C29 -2.5(4) C41 C36 C37 C38 0.7(4) C41 C36 C37 C54 177.8(2) C41 C42 C43 C44 4.2(4) C41 C42 C43 C47 -179.2(2) C41 C42 C50 C51 -2.9(4) C41 C42 C50 C49 179.7(3) C33 C32 C31 C30 178.9(3) C39 C38 C37 C36 -0.4(4) C39 C38 C37 C54 -177.6(3) C62 C61 C60 C59 1.2(4) C62 C54 C55 C59 1.5(4) C62 C54 C55 C56 -175.6(3) C40 C41 C42 C43 -96.5(3) C40 C41 C42 C50 84.0(3) C40 C39 C38 C37 0.1(5) C10 C11 C12 C13 87.1(3) C10 C11 C12 C20 -92.7(3) C10 C9 C8 C7 -0.2(4) C25 C24 C32 C33 -177.4(3) C25 C24 C32 C31 2.3(4) C42 C41 C40 C39 175.7(3) C42 C43 C44 C46 94.4(3) C42 C43 C44 C45 -141.3(3) C42 C43 C47 C48 -0.4(4) C42 C50 C49 C48 -0.6(5) C12 C11 C10 C9 179.7(3) C12 C13 C17 C18 -0.4(5) C12 C13 C14 C16 -131.5(7) C12 C13 C14 C15 107.0(5) C12 C13 C14 C15A 106.1(10) C12 C13 C14 C16A -121.4(9) C12 C20 C21 C23 104.9(3) C12 C20 C21 C22 -130.8(3) C12 C20 C19 C18 1.0(4) C13 C12 C20 C21 179.4(3) C13 C12 C20 C19 -2.1(4) C13 C17 C18 C19 -0.7(5) C43 C42 C50 C51 177.6(3) C43 C42 C50 C49 0.2(4) C43 C47 C48 C49 0.1(5) C38 C39 C40 C41 -0.1(4) C38 C37 C54 C62 -98.1(3) C38 C37 C54 C55 80.6(4) C37 C36 C41 C40 -0.7(4) C37 C36 C41 C42 -176.1(2) C37 C54 C55 C59 -177.2(3) C37 C54 C55 C56 5.7(4) C8 C7 C24 C32 84.9(3) C8 C7 C24 C25 -94.2(3) C26 C25 C29 C30 -179.3(3) C44 C43 C47 C48 176.2(3) C61 C62 C54 C37 176.5(2) C61 C62 C54 C55 -2.2(4) C61 C62 C63 C64 -90.6(3) C61 C62 C63 C65 33.8(4) C20 C12 C13 C17 1.9(4) C20 C12 C13 C14 -176.4(3) C59 C55 C56 C58 48.7(4) C59 C55 C56 C57 -74.7(4) C51 C50 C49 C48 -178.0(3) C29 C25 C26 C27 49.8(4) C29 C25 C26 C28 -74.0(4) C29 C30 C31 C32 -0.5(5) C54 C62 C61 C60 0.9(4) C54 C62 C63 C64 86.5(3) C54 C62 C63 C65 -149.2(3) C54 C55 C56 C58 -134.1(3) C54 C55 C56 C57 102.4(3) C60 C59 C55 C54 0.6(5) C60 C59 C55 C56 177.8(3) C50 C42 C43 C44 -176.3(2) C50 C42 C43 C47 0.3(4) C50 C49 C48 C47 0.5(5) C31 C32 C33 C34 64.0(4) C31 C32 C33 C35 -60.4(4) C31 C30 C29 C25 0.3(5) C21 C20 C19 C18 179.4(3) C55 C59 C60 C61 -1.9(5) C17 C13 C14 C16 50.3(8) C17 C13 C14 C15 -71.2(5) C17 C13 C14 C15A -72.2(10) C17 C13 C14 C16A 60.3(9) C17 C18 C19 C20 0.5(5) C47 C43 C44 C46 -82.2(3) C47 C43 C44 C45 42.1(4) C63 C62 C61 C60 178.0(3) C63 C62 C54 C37 -0.6(4) C63 C62 C54 C55 -179.3(3) N3S C11S C12S C13S -0.5(8) N3S C15S C14S C13S -0.3(9) C19 C20 C21 C23 -73.5(4) C19 C20 C21 C22 50.8(4) C5S N1S C1S C2S 0.6(5) C1S N1S C5S C4S -0.3(5) C1S C2S C3S C4S 0.5(5) C14 C13 C17 C18 177.9(3) C53 C51 C50 C42 -91.9(3) C53 C51 C50 C49 85.4(3) C52 C51 C50 C42 145.1(3) C52 C51 C50 C49 -37.6(4) C2S C3S C4S C5S -0.3(5) C11S N3S C15S C14S 0.4(8) C12S C13S C14S C15S -0.2(9) C15S N3S C11S C12S 0.0(8) C14S C13S C12S C11S 0.6(9) C7S C8S C9S C10S 0.0 C8S C7S C6S N2S 0.0 C8S C9S C10S N2S 0.0 C9S C10S N2S C6S 0.0 C10S N2S C6S C7S 0.0 C6S C7S C8S C9S 0.0