#------------------------------------------------------------------------------ #$Date: 2017-04-19 05:59:00 +0300 (Wed, 19 Apr 2017) $ #$Revision: 195532 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042718.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_7042718 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 H74.57 F1.57 Mn N2 O3, 0.43(F), C2 H5 O0.47' _chemical_formula_sum 'C67 H79.57 F2 Mn N2 O3.47' _chemical_formula_weight 1061.27 _chemical_name_common Mn(FHF)(CO)3(CNArDipp2) _chemical_name_systematic ; ? ; _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 mixed _atom_sites_solution_primary direct _audit_creation_date 2017-03-19 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.03.14 svn.r3398 for OlexSys, GUI svn.r5328) ; _audit_update_record ; 2017-03-20 deposited with the CCDC. 2017-04-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 114.1020(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.1678(5) _cell_length_b 16.5149(4) _cell_length_c 20.6165(5) _cell_measurement_reflns_used 3483 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 68.11 _cell_measurement_theta_min 3.78 _cell_volume 5957.3(3) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2016)' _computing_data_collection 'APEX3 v2016.9-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution '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 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 46752 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 67.500 _diffrn_reflns_theta_max 68.284 _diffrn_reflns_theta_min 2.525 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker MicroStar FR-592' _exptl_absorpt_coefficient_mu 2.221 _exptl_absorpt_correction_T_max 0.5210 _exptl_absorpt_correction_T_min 0.4202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.183 _exptl_crystal_description block _exptl_crystal_F_000 2265 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.631 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.053 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 749 _refine_ls_number_reflns 10877 _refine_ls_number_restraints 654 _refine_ls_restrained_S_all 1.009 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0462 _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^)+(0.0702P)^2^+3.8567P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1251 _refine_ls_wR_factor_ref 0.1307 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9629 _reflns_number_total 10877 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt01102d2.cif _cod_data_source_block jfigcu128 _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 7042718 _shelx_shelxl_version_number 2016/6 _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(C6) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C1S2) = Uanis(C1S) Uanis(C2S2) = Uanis(C2S) 3. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(C1S)=Sof(H1SC)=Sof(H1SD)=Sof(C2S)=Sof(H2SD)=Sof(H2SE)=Sof(H2SF)=1-FVAR(1) Sof(C1S2)=Sof(H1SA)=Sof(H1SB)=Sof(C2S2)=Sof(H2SA)=Sof(H2SB)=Sof(H2SC)=FVAR(1) Sof(F4)=Sof(H4)=Sof(F2)=Sof(O4)=Sof(C5)=1-FVAR(2) Sof(F1)=Sof(F3)=Sof(O3)=Sof(C6)=FVAR(2) 5.a Ternary CH refined with riding coordinates: C19(H19), C22(H22), C27(H27), C34(H34), C45(H45), C52(H52), C57(H57), C64(H64) 5.b Secondary CH2 refined with riding coordinates: C1S2(H1SA,H1SB), C1S(H1SC,H1SD) 5.c Aromatic/amide H refined with riding coordinates: C9(H9), C10(H10), C11(H11), C15(H15), C16(H16), C17(H17), C30(H30), C31(H31), C32(H32), C39(H39), C40(H40), C41(H41), C48(H48), C49(H49), C51(H51), C60(H60), C61(H61), C62(H62) 5.d Idealised Me refined as rotating group: C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B, H24C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C36(H36A, H36B,H36C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C65(H65A,H65B, H65C), C66(H66A,H66B,H66C), C2S2(H2SA,H2SB,H2SC), C2S(H2SD,H2SE,H2SF) ; _shelx_res_file ; TITL JFigCu128_0m_a.res in P2(1)/c jfigcu128_0m_a.res created by SHELXL-2016/6 at 18:09:12 on 19-Mar-2017 REM Old TITL JFigCu128_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.174, Rweak 0.010, Alpha 0.051, Orientation as input REM Formula found by SHELXT: C132 N13 H66b Mn2 CELL 1.54178 19.1678 16.5149 20.6165 90 114.102 90 ZERR 4 0.0005 0.0004 0.0005 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F Mn N O UNIT 268 318.27 8 4 8 13.86 RIGU ISOR C6 O3 EADP C1S2 C1S EADP C2S2 C2S L.S. 10 PLAN 10 TEMP -173.15 BOND $H MORE -1 List 4 CONF fmap 2 acta 135 REM REM REM WGHT 0.070200 3.856700 FVAR 0.29473 0.54599 0.43169 MN01 4 0.736728 0.555590 0.260619 11.00000 0.02260 0.01948 = 0.02497 -0.00434 0.01090 0.00375 PART 1 F4 3 0.539809 0.520538 0.131281 -31.00000 0.04653 0.04445 = 0.07189 0.00304 0.00067 -0.00506 H4 2 0.600434 0.499876 0.175923 -31.00000 0.01337 F2 3 0.647897 0.485028 0.226728 -31.00000 0.04364 0.05189 = 0.05635 -0.02004 0.03253 0.01052 PART 0 PART 2 F1 3 0.828606 0.627760 0.293524 31.00000 0.07087 0.04411 = 0.13300 -0.03523 0.07320 -0.01151 F3 3 0.934644 0.660298 0.391946 31.00000 0.04957 0.08678 = 0.07116 -0.01103 0.03345 -0.01655 PART 0 O1 6 0.680974 0.634249 0.116797 11.00000 0.09694 0.06330 = 0.04356 0.01970 0.03948 0.03381 O2 6 0.791546 0.480231 0.406179 11.00000 0.11019 0.08548 = 0.03593 0.01772 0.02888 0.05673 PART 1 O4 6 0.879046 0.651997 0.319585 -31.00000 0.01899 0.05389 = 0.13770 -0.06152 0.01837 -0.01201 PART 0 PART 2 O3 6 0.602131 0.450410 0.205383 31.00000 0.06056 0.11065 = 0.16251 -0.10587 0.07487 -0.05064 PART 0 N1 5 0.822431 0.427607 0.212213 11.00000 0.01907 0.01916 = 0.02490 -0.00146 0.00841 0.00311 N2 5 0.650380 0.681076 0.311062 11.00000 0.02034 0.01348 = 0.01643 -0.00003 0.00806 0.00194 C1 1 0.790310 0.475488 0.230429 11.00000 0.01956 0.02440 = 0.02388 -0.00237 0.00644 -0.00009 C2 1 0.681955 0.634595 0.291177 11.00000 0.02102 0.01946 = 0.01787 0.00077 0.00664 0.00183 C3 1 0.701932 0.604758 0.171060 11.00000 0.04916 0.03430 = 0.03974 0.00127 0.02646 0.01518 C4 1 0.770920 0.508317 0.350733 11.00000 0.05675 0.04643 = 0.03171 -0.00192 0.01639 0.02668 C7 1 0.861333 0.370322 0.189450 11.00000 0.02172 0.01554 = 0.03100 -0.00089 0.01435 0.00280 C8 1 0.937043 0.352175 0.234265 11.00000 0.02355 0.02255 = 0.03314 -0.00022 0.01170 0.00407 C9 1 0.974315 0.294697 0.210147 11.00000 0.02415 0.03076 = 0.04334 -0.00289 0.01356 0.00866 AFIX 43 H9 2 1.025982 0.281179 0.238891 11.00000 -1.20000 AFIX 0 C10 1 0.937098 0.257061 0.144921 11.00000 0.03118 0.02771 = 0.04936 -0.00899 0.02088 0.00647 AFIX 43 H10 2 0.963467 0.218140 0.129428 11.00000 -1.20000 AFIX 0 C11 1 0.861568 0.275784 0.102026 11.00000 0.02882 0.02265 = 0.03701 -0.00890 0.01653 -0.00096 AFIX 43 H11 2 0.836745 0.249374 0.057502 11.00000 -1.20000 AFIX 0 C12 1 0.821655 0.332915 0.123496 11.00000 0.02290 0.01691 = 0.03153 -0.00038 0.01464 -0.00092 C13 1 0.739795 0.354459 0.080493 11.00000 0.02404 0.01826 = 0.02805 -0.00846 0.00984 0.00101 C14 1 0.683092 0.317624 0.097424 11.00000 0.02552 0.02852 = 0.03389 -0.01388 0.01353 -0.00250 C15 1 0.607356 0.341099 0.058946 11.00000 0.02335 0.05508 = 0.04361 -0.02225 0.01230 -0.00194 AFIX 43 H15 2 0.568135 0.316627 0.069177 11.00000 -1.20000 AFIX 0 C16 1 0.588287 0.398933 0.006508 11.00000 0.03060 0.06453 = 0.03984 -0.01622 0.00128 0.01560 AFIX 43 H16 2 0.536397 0.414424 -0.018675 11.00000 -1.20000 AFIX 0 C17 1 0.644467 0.434496 -0.009570 11.00000 0.04815 0.03790 = 0.03305 -0.00353 0.00237 0.01637 AFIX 43 H17 2 0.630679 0.473965 -0.046218 11.00000 -1.20000 AFIX 0 C18 1 0.721256 0.413385 0.027178 11.00000 0.03817 0.02148 = 0.03033 -0.00661 0.00980 0.00359 C19 1 0.781769 0.451739 0.007341 11.00000 0.05562 0.02680 = 0.03781 0.00251 0.01863 -0.00379 AFIX 13 H19 2 0.832428 0.440482 0.047142 11.00000 -1.20000 AFIX 0 C20 1 0.782447 0.411637 -0.059033 11.00000 0.08902 0.06096 = 0.05826 -0.00936 0.04252 -0.01483 AFIX 137 H20A 2 0.788729 0.353015 -0.051552 11.00000 -1.50000 H20B 2 0.824945 0.433297 -0.068542 11.00000 -1.50000 H20C 2 0.734103 0.422828 -0.099655 11.00000 -1.50000 AFIX 0 C21 1 0.773995 0.543068 -0.000857 11.00000 0.11114 0.02896 = 0.10225 0.00543 0.05146 -0.00337 AFIX 137 H21A 2 0.727625 0.556360 -0.042907 11.00000 -1.50000 H21B 2 0.818677 0.565234 -0.006394 11.00000 -1.50000 H21C 2 0.770664 0.566561 0.041438 11.00000 -1.50000 AFIX 0 C22 1 0.703421 0.252449 0.153463 11.00000 0.03432 0.03636 = 0.04388 -0.00472 0.02212 -0.00903 AFIX 13 H22 2 0.756064 0.264477 0.189693 11.00000 -1.20000 AFIX 0 C23 1 0.706490 0.169966 0.120971 11.00000 0.05744 0.03142 = 0.07459 -0.00041 0.03969 -0.00728 AFIX 137 H23A 2 0.655851 0.156622 0.084472 11.00000 -1.50000 H23B 2 0.722045 0.128485 0.158200 11.00000 -1.50000 H23C 2 0.743541 0.171948 0.099425 11.00000 -1.50000 AFIX 0 C24 1 0.650456 0.249743 0.192489 11.00000 0.05522 0.07341 = 0.06055 -0.00992 0.03984 -0.01874 AFIX 137 H24A 2 0.647271 0.303787 0.210723 11.00000 -1.50000 H24B 2 0.670842 0.211466 0.232167 11.00000 -1.50000 H24C 2 0.599374 0.232246 0.159540 11.00000 -1.50000 AFIX 0 C25 1 0.973822 0.392012 0.305286 11.00000 0.01964 0.03148 = 0.03172 -0.00161 0.00754 0.01032 C26 1 0.962673 0.357627 0.362762 11.00000 0.02627 0.04888 = 0.03501 0.00096 0.01278 0.01126 C27 1 0.917144 0.279769 0.355109 11.00000 0.03517 0.05959 = 0.04298 0.00593 0.01878 -0.00021 AFIX 13 H27 2 0.905095 0.258154 0.306394 11.00000 -1.20000 AFIX 0 C28 1 0.841093 0.293591 0.360616 11.00000 0.03979 0.06085 = 0.07670 0.02029 0.02791 0.00666 AFIX 137 H28A 2 0.850565 0.313823 0.408170 11.00000 -1.50000 H28B 2 0.812891 0.242407 0.352267 11.00000 -1.50000 H28C 2 0.810946 0.333428 0.324950 11.00000 -1.50000 AFIX 0 C29 1 0.962732 0.215188 0.407351 11.00000 0.04042 0.04919 = 0.08144 0.00097 0.01758 0.00726 AFIX 137 H29A 2 1.011501 0.206862 0.403462 11.00000 -1.50000 H29B 2 0.933757 0.164406 0.396652 11.00000 -1.50000 H29C 2 0.972444 0.232497 0.455753 11.00000 -1.50000 AFIX 0 C30 1 0.995075 0.396529 0.428210 11.00000 0.04067 0.06140 = 0.03793 -0.00272 0.01903 0.00946 AFIX 43 H30 2 0.988555 0.374328 0.467883 11.00000 -1.20000 AFIX 0 C31 1 1.036558 0.466930 0.436283 11.00000 0.03972 0.06412 = 0.03291 -0.01346 0.00882 0.01563 AFIX 43 H31 2 1.058216 0.492704 0.481374 11.00000 -1.20000 AFIX 0 C32 1 1.046877 0.500282 0.379348 11.00000 0.03454 0.03483 = 0.04268 -0.00999 0.00697 0.00844 AFIX 43 H32 2 1.075357 0.548951 0.385783 11.00000 -1.20000 AFIX 0 C33 1 1.016187 0.463678 0.312676 11.00000 0.02661 0.02860 = 0.03502 -0.00376 0.00652 0.01193 C34 1 1.027141 0.501083 0.249952 11.00000 0.04267 0.02627 = 0.03854 -0.00237 0.00783 -0.00131 AFIX 13 H34 2 1.019809 0.456984 0.214517 11.00000 -1.20000 AFIX 0 C35 1 1.106778 0.536712 0.269259 11.00000 0.03501 0.06329 = 0.05608 0.00258 0.01985 0.00901 AFIX 137 H35A 2 1.113480 0.584501 0.299402 11.00000 -1.50000 H35B 2 1.112353 0.552327 0.225760 11.00000 -1.50000 H35C 2 1.145538 0.496139 0.294985 11.00000 -1.50000 AFIX 0 C36 1 0.967918 0.565656 0.213587 11.00000 0.03179 0.06492 = 0.10471 0.04982 0.01487 0.00172 AFIX 137 H36A 2 0.916860 0.541260 0.194437 11.00000 -1.50000 H36B 2 0.977881 0.589722 0.174751 11.00000 -1.50000 H36C 2 0.970682 0.607776 0.248037 11.00000 -1.50000 AFIX 0 C37 1 0.617336 0.739973 0.338666 11.00000 0.01610 0.01288 = 0.01624 -0.00217 0.00843 -0.00003 C38 1 0.622098 0.729665 0.407893 11.00000 0.01450 0.01241 = 0.01712 0.00038 0.00612 -0.00179 C39 1 0.592306 0.791347 0.435060 11.00000 0.02049 0.01563 = 0.01543 -0.00109 0.00900 -0.00280 AFIX 43 H39 2 0.595373 0.786997 0.482098 11.00000 -1.20000 AFIX 0 C40 1 0.558247 0.859000 0.394735 11.00000 0.02098 0.01306 = 0.02103 -0.00196 0.01142 0.00043 AFIX 43 H40 2 0.538803 0.900684 0.414483 11.00000 -1.20000 AFIX 0 C41 1 0.552439 0.866075 0.325510 11.00000 0.02089 0.01325 = 0.01953 0.00212 0.00839 0.00229 AFIX 43 H41 2 0.528045 0.912205 0.298103 11.00000 -1.20000 AFIX 0 C42 1 0.581738 0.806764 0.295713 11.00000 0.01767 0.01504 = 0.01674 0.00030 0.00821 -0.00050 C43 1 0.656778 0.655376 0.450692 11.00000 0.02201 0.01432 = 0.01543 0.00138 0.01014 0.00260 C44 1 0.731484 0.659506 0.504624 11.00000 0.02288 0.01915 = 0.01986 0.00268 0.01045 0.00310 C45 1 0.779198 0.735905 0.517206 11.00000 0.01956 0.02145 = 0.02561 0.00334 0.00468 0.00073 AFIX 13 H45 2 0.743298 0.783002 0.502531 11.00000 -1.20000 AFIX 0 C46 1 0.823138 0.735089 0.469457 11.00000 0.03099 0.04021 = 0.02923 0.00315 0.01084 -0.01040 AFIX 137 H46A 2 0.857906 0.688578 0.481804 11.00000 -1.50000 H46B 2 0.852679 0.785231 0.476468 11.00000 -1.50000 H46C 2 0.786884 0.730938 0.419611 11.00000 -1.50000 AFIX 0 C47 1 0.833565 0.748423 0.594834 11.00000 0.02992 0.03647 = 0.02940 -0.00301 0.00611 -0.00355 AFIX 137 H47A 2 0.804828 0.745512 0.624658 11.00000 -1.50000 H47B 2 0.857929 0.801659 0.600415 11.00000 -1.50000 H47C 2 0.872859 0.706140 0.609289 11.00000 -1.50000 AFIX 0 C48 1 0.762059 0.589988 0.544520 11.00000 0.02481 0.02579 = 0.02568 0.00773 0.00860 0.00746 AFIX 43 H48 2 0.812496 0.591394 0.580694 11.00000 -1.20000 AFIX 0 C49 1 0.720392 0.519169 0.532419 11.00000 0.03644 0.02039 = 0.03136 0.01100 0.01393 0.00956 AFIX 43 H49 2 0.742229 0.472564 0.560360 11.00000 -1.20000 AFIX 0 C50 1 0.614010 0.583625 0.437881 11.00000 0.02588 0.01559 = 0.01986 0.00031 0.01124 0.00101 C51 1 0.647117 0.515757 0.479889 11.00000 0.03687 0.01459 = 0.03151 0.00356 0.01695 0.00057 AFIX 43 H51 2 0.618839 0.466794 0.472162 11.00000 -1.20000 AFIX 0 C52 1 0.533409 0.576884 0.379980 11.00000 0.02949 0.01392 = 0.02180 -0.00142 0.00851 -0.00532 AFIX 13 H52 2 0.518887 0.630740 0.356037 11.00000 -1.20000 AFIX 0 C53 1 0.529500 0.514163 0.323864 11.00000 0.04215 0.02573 = 0.02745 -0.00696 0.01542 -0.00752 AFIX 137 H53A 2 0.567429 0.527476 0.304954 11.00000 -1.50000 H53B 2 0.478295 0.514639 0.285163 11.00000 -1.50000 H53C 2 0.540273 0.460244 0.345573 11.00000 -1.50000 AFIX 0 C54 1 0.474757 0.554578 0.409998 11.00000 0.02936 0.03965 = 0.02724 -0.00741 0.01099 -0.00662 AFIX 137 H54A 2 0.487089 0.501170 0.432559 11.00000 -1.50000 H54B 2 0.423537 0.553260 0.371345 11.00000 -1.50000 H54C 2 0.476157 0.595046 0.445275 11.00000 -1.50000 AFIX 0 C55 1 0.574808 0.812748 0.220849 11.00000 0.02832 0.01386 = 0.01845 0.00413 0.01269 0.00756 C56 1 0.505905 0.790365 0.164446 11.00000 0.03448 0.01646 = 0.01970 -0.00044 0.00987 0.00663 C57 1 0.438396 0.758845 0.178134 11.00000 0.03074 0.03095 = 0.02397 -0.00656 0.00674 -0.00258 AFIX 13 H57 2 0.441150 0.783642 0.223369 11.00000 -1.20000 AFIX 0 C58 1 0.444507 0.667593 0.188182 11.00000 0.04649 0.03605 = 0.03012 0.00336 0.01278 -0.00389 AFIX 137 H58A 2 0.442492 0.641855 0.144620 11.00000 -1.50000 H58B 2 0.401959 0.647967 0.198644 11.00000 -1.50000 H58C 2 0.493014 0.654093 0.227762 11.00000 -1.50000 AFIX 0 C59 1 0.360886 0.781440 0.118941 11.00000 0.03564 0.04288 = 0.05853 0.00887 0.00424 -0.00030 AFIX 137 H59A 2 0.358958 0.840005 0.110728 11.00000 -1.50000 H59B 2 0.319813 0.765812 0.133143 11.00000 -1.50000 H59C 2 0.354388 0.752932 0.075150 11.00000 -1.50000 AFIX 0 C60 1 0.501076 0.795539 0.095481 11.00000 0.05286 0.02514 = 0.01787 -0.00086 0.01087 0.01107 AFIX 43 H60 2 0.455068 0.780244 0.056833 11.00000 -1.20000 AFIX 0 C61 1 0.562131 0.822563 0.082354 11.00000 0.07002 0.02675 = 0.02262 0.00803 0.02717 0.02012 AFIX 43 H61 2 0.557930 0.825321 0.034870 11.00000 -1.20000 AFIX 0 C62 1 0.629026 0.845543 0.137443 11.00000 0.05337 0.03062 = 0.03789 0.01408 0.03471 0.01497 AFIX 43 H62 2 0.670407 0.864739 0.127590 11.00000 -1.20000 AFIX 0 C63 1 0.636886 0.841006 0.207749 11.00000 0.03493 0.02387 = 0.02926 0.00870 0.02047 0.00745 C64 1 0.710242 0.869508 0.267023 11.00000 0.02987 0.04821 = 0.04145 0.01038 0.02092 -0.00256 AFIX 13 H64 2 0.709637 0.851625 0.313131 11.00000 -1.20000 AFIX 0 C65 1 0.781209 0.833148 0.261658 11.00000 0.03695 0.05096 = 0.10015 0.01233 0.03196 0.00684 AFIX 137 H65A 2 0.775741 0.774173 0.257086 11.00000 -1.50000 H65B 2 0.826611 0.846634 0.304551 11.00000 -1.50000 H65C 2 0.786680 0.855372 0.219906 11.00000 -1.50000 AFIX 0 C66 1 0.714512 0.961606 0.267657 11.00000 0.03718 0.05352 = 0.07023 -0.01536 0.01916 -0.00308 AFIX 137 H66A 2 0.714561 0.980657 0.222658 11.00000 -1.50000 H66B 2 0.761532 0.979325 0.307089 11.00000 -1.50000 H66C 2 0.670189 0.984098 0.273633 11.00000 -1.50000 AFIX 0 PART 1 C5 1 0.821633 0.618338 0.292430 -31.00000 0.01335 0.04124 = 0.04503 -0.02765 -0.00275 0.00311 PART 0 PART 2 C6 1 0.650639 0.480469 0.233346 31.00000 0.03968 0.01499 = 0.03845 0.00963 0.01375 -0.00563 PART 0 O1S 6 1.000000 1.000000 0.500000 0.46596 0.12793 0.08980 = 0.07816 -0.02600 0.05237 -0.03476 PART 1 C1S2 1 1.009657 0.956617 0.452325 21.00000 0.06379 0.07948 = 0.05958 0.00076 0.02827 -0.00166 AFIX 23 H1SA 2 1.055078 0.921753 0.475898 21.00000 -1.20000 H1SB 2 1.020413 0.993048 0.419383 21.00000 -1.20000 AFIX 0 C2S2 1 0.945237 0.905920 0.411469 21.00000 0.05463 0.07720 = 0.07783 -0.00277 0.03089 0.00863 AFIX 137 H2SA 2 0.957129 0.874524 0.376930 21.00000 -1.50000 H2SB 2 0.900338 0.939924 0.386319 21.00000 -1.50000 H2SC 2 0.934529 0.868912 0.443432 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C1S 1 0.957831 0.939415 0.464473 -21.00000 0.06379 0.07948 = 0.05958 0.00076 0.02827 -0.00166 AFIX 23 H1SC 2 0.909860 0.962181 0.428487 -21.00000 -1.20000 H1SD 2 0.943845 0.907255 0.497910 -21.00000 -1.20000 AFIX 0 C2S 1 0.989521 0.882119 0.427051 -21.00000 0.05463 0.07720 = 0.07783 -0.00277 0.03089 0.00863 AFIX 137 H2SD 2 0.949251 0.844849 0.397612 -21.00000 -1.50000 H2SE 2 1.031645 0.851183 0.462214 -21.00000 -1.50000 H2SF 2 1.008408 0.912826 0.396838 -21.00000 -1.50000 AFIX 0 HKLF 4 REM JFigCu128_0m_a.res in P2(1)/c REM R1 = 0.0462 for 9629 Fo > 4sig(Fo) and 0.0529 for all 10877 data REM 749 parameters refined using 654 restraints END WGHT 0.0702 3.8567 REM Highest difference peak 0.631, deepest hole -0.448, 1-sigma level 0.053 Q1 1 1.0374 1.0221 0.4814 11.00000 0.05 0.63 Q2 1 0.7501 0.4627 -0.0707 11.00000 0.05 0.38 Q3 1 0.6284 0.6020 0.1098 11.00000 0.05 0.38 Q4 1 0.9681 0.9860 0.4464 11.00000 0.05 0.37 Q5 1 0.5767 0.8068 0.2601 11.00000 0.05 0.36 Q6 1 0.7336 0.4523 0.3723 11.00000 0.05 0.34 Q7 1 0.7238 0.5034 0.2867 11.00000 0.05 0.34 Q8 1 1.0871 0.4864 0.2524 11.00000 0.05 0.33 Q9 1 0.9102 0.6748 0.3375 11.00000 0.05 0.33 Q10 1 0.7104 0.6213 0.2388 11.00000 0.05 0.33 ; _shelx_res_checksum 87331 _olex2_submission_original_sample_id JFigCu128 _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 Mn01 Mn 0.73673(2) 0.55559(2) 0.26062(2) 0.02196(10) Uani 1 1 d . U . . . F4 F 0.53981(16) 0.52054(17) 0.13128(17) 0.0620(10) Uani 0.568(4) 1 d . U . A 1 H4 H 0.600(3) 0.500(3) 0.176(2) 0.013(10) Uiso 0.568(4) 1 d . . . A 1 F2 F 0.6479(6) 0.4850(5) 0.2267(5) 0.0467(19) Uani 0.568(4) 1 d . U . A 1 F1 F 0.8286(7) 0.6278(7) 0.2935(6) 0.072(3) Uani 0.432(4) 1 d . U . A 2 F3 F 0.9346(2) 0.6603(3) 0.3919(2) 0.0663(14) Uani 0.432(4) 1 d . U . A 2 O1 O 0.68097(14) 0.63425(13) 0.11680(11) 0.0644(6) Uani 1 1 d . U . . . O2 O 0.79155(15) 0.48023(16) 0.40618(11) 0.0775(8) Uani 1 1 d . U . . . O4 O 0.8790(2) 0.6520(3) 0.3196(3) 0.0746(16) Uani 0.568(4) 1 d . U . A 1 O3 O 0.6021(4) 0.4504(5) 0.2054(5) 0.102(4) Uani 0.432(4) 1 d . U . A 2 N1 N 0.82243(9) 0.42761(10) 0.21221(9) 0.0212(3) Uani 1 1 d . U . . . N2 N 0.65038(8) 0.68108(9) 0.31106(8) 0.0166(3) Uani 1 1 d . U . . . C1 C 0.79031(10) 0.47549(12) 0.23043(10) 0.0234(4) Uani 1 1 d . U . . . C2 C 0.68196(10) 0.63460(11) 0.29118(10) 0.0199(4) Uani 1 1 d . U . . . C3 C 0.70193(14) 0.60476(15) 0.17106(13) 0.0383(5) Uani 1 1 d . U . . . C4 C 0.77092(16) 0.50832(16) 0.35073(13) 0.0455(6) Uani 1 1 d . U . . . C7 C 0.86133(10) 0.37032(11) 0.18945(11) 0.0216(4) Uani 1 1 d . U . . . C8 C 0.93704(11) 0.35217(12) 0.23427(11) 0.0264(4) Uani 1 1 d . U . . . C9 C 0.97431(12) 0.29470(14) 0.21015(12) 0.0328(5) Uani 1 1 d . U . . . H9 H 1.025982 0.281179 0.238891 0.039 Uiso 1 1 calc R . . . . C10 C 0.93710(12) 0.25706(14) 0.14492(13) 0.0346(5) Uani 1 1 d . U . . . H10 H 0.963467 0.218140 0.129428 0.042 Uiso 1 1 calc R . . . . C11 C 0.86157(12) 0.27578(12) 0.10203(12) 0.0285(4) Uani 1 1 d . U . . . H11 H 0.836745 0.249374 0.057502 0.034 Uiso 1 1 calc R . . . . C12 C 0.82165(11) 0.33292(11) 0.12350(11) 0.0226(4) Uani 1 1 d . U . . . C13 C 0.73980(11) 0.35446(12) 0.08049(11) 0.0237(4) Uani 1 1 d . U . . . C14 C 0.68309(11) 0.31762(13) 0.09742(11) 0.0288(4) Uani 1 1 d . U . . . C15 C 0.60736(12) 0.34110(16) 0.05895(13) 0.0411(6) Uani 1 1 d . U . . . H15 H 0.568135 0.316627 0.069177 0.049 Uiso 1 1 calc R . . . . C16 C 0.58829(14) 0.39893(18) 0.00651(14) 0.0493(7) Uani 1 1 d . U . . . H16 H 0.536397 0.414424 -0.018675 0.059 Uiso 1 1 calc R . . . . C17 C 0.64447(15) 0.43450(16) -0.00957(13) 0.0443(6) Uani 1 1 d . U . . . H17 H 0.630679 0.473965 -0.046218 0.053 Uiso 1 1 calc R . . . . C18 C 0.72126(13) 0.41338(13) 0.02718(12) 0.0314(5) Uani 1 1 d . U . . . C19 C 0.78177(16) 0.45174(14) 0.00734(14) 0.0402(6) Uani 1 1 d . U . . . H19 H 0.832428 0.440482 0.047142 0.048 Uiso 1 1 calc R . . . . C20 C 0.7824(2) 0.4116(2) -0.05903(18) 0.0653(9) Uani 1 1 d . U . . . H20A H 0.788729 0.353015 -0.051552 0.098 Uiso 1 1 calc GR . . . . H20B H 0.824945 0.433297 -0.068542 0.098 Uiso 1 1 calc GR . . . . H20C H 0.734103 0.422828 -0.099655 0.098 Uiso 1 1 calc GR . . . . C21 C 0.7740(3) 0.54307(18) -0.0009(2) 0.0782(11) Uani 1 1 d . U . . . H21A H 0.727625 0.556360 -0.042907 0.117 Uiso 1 1 calc GR . . . . H21B H 0.818677 0.565234 -0.006394 0.117 Uiso 1 1 calc GR . . . . H21C H 0.770664 0.566561 0.041438 0.117 Uiso 1 1 calc GR . . . . C22 C 0.70342(13) 0.25245(14) 0.15346(13) 0.0362(5) Uani 1 1 d . U . . . H22 H 0.756064 0.264477 0.189693 0.043 Uiso 1 1 calc R . . . . C23 C 0.70649(17) 0.16997(15) 0.12097(17) 0.0503(7) Uani 1 1 d . U . . . H23A H 0.655851 0.156622 0.084472 0.075 Uiso 1 1 calc GR . . . . H23B H 0.722045 0.128485 0.158200 0.075 Uiso 1 1 calc GR . . . . H23C H 0.743541 0.171948 0.099425 0.075 Uiso 1 1 calc GR . . . . C24 C 0.65046(17) 0.2497(2) 0.19249(17) 0.0578(8) Uani 1 1 d . U . . . H24A H 0.647271 0.303787 0.210723 0.087 Uiso 1 1 calc GR . . . . H24B H 0.670842 0.211466 0.232167 0.087 Uiso 1 1 calc GR . . . . H24C H 0.599374 0.232246 0.159540 0.087 Uiso 1 1 calc GR . . . . C25 C 0.97382(11) 0.39201(13) 0.30529(11) 0.0286(4) Uani 1 1 d . U . . . C26 C 0.96267(12) 0.35763(16) 0.36276(12) 0.0366(5) Uani 1 1 d . U . . . C27 C 0.91714(14) 0.27977(18) 0.35511(14) 0.0450(6) Uani 1 1 d . U . . . H27 H 0.905095 0.258154 0.306394 0.054 Uiso 1 1 calc R . . . . C28 C 0.84109(15) 0.2936(2) 0.36062(18) 0.0578(8) Uani 1 1 d . U . . . H28A H 0.850565 0.313823 0.408170 0.087 Uiso 1 1 calc GR . . . . H28B H 0.812891 0.242407 0.352267 0.087 Uiso 1 1 calc GR . . . . H28C H 0.810946 0.333428 0.324950 0.087 Uiso 1 1 calc GR . . . . C29 C 0.96273(16) 0.21519(19) 0.40735(19) 0.0594(8) Uani 1 1 d . U . . . H29A H 1.011501 0.206862 0.403462 0.089 Uiso 1 1 calc GR . . . . H29B H 0.933757 0.164406 0.396652 0.089 Uiso 1 1 calc GR . . . . H29C H 0.972444 0.232497 0.455753 0.089 Uiso 1 1 calc GR . . . . C30 C 0.99507(14) 0.39653(18) 0.42821(14) 0.0457(6) Uani 1 1 d . U . . . H30 H 0.988555 0.374328 0.467883 0.055 Uiso 1 1 calc R . . . . C31 C 1.03656(14) 0.46693(19) 0.43628(14) 0.0475(6) Uani 1 1 d . U . . . H31 H 1.058216 0.492704 0.481374 0.057 Uiso 1 1 calc R . . . . C32 C 1.04688(13) 0.50028(15) 0.37935(13) 0.0402(5) Uani 1 1 d . U . . . H32 H 1.075357 0.548951 0.385783 0.048 Uiso 1 1 calc R . . . . C33 C 1.01619(12) 0.46368(14) 0.31268(12) 0.0321(5) Uani 1 1 d . U . . . C34 C 1.02714(14) 0.50108(14) 0.24995(13) 0.0387(5) Uani 1 1 d . U . . . H34 H 1.019809 0.456984 0.214517 0.046 Uiso 1 1 calc R . . . . C35 C 1.10678(14) 0.53671(19) 0.26926(16) 0.0511(7) Uani 1 1 d . U . . . H35A H 1.113480 0.584501 0.299402 0.077 Uiso 1 1 calc GR . . . . H35B H 1.112353 0.552327 0.225760 0.077 Uiso 1 1 calc GR . . . . H35C H 1.145538 0.496139 0.294985 0.077 Uiso 1 1 calc GR . . . . C36 C 0.96792(16) 0.5657(2) 0.2136(2) 0.0714(11) Uani 1 1 d . U . . . H36A H 0.916860 0.541260 0.194437 0.107 Uiso 1 1 calc GR . . . . H36B H 0.977881 0.589722 0.174751 0.107 Uiso 1 1 calc GR . . . . H36C H 0.970682 0.607776 0.248037 0.107 Uiso 1 1 calc GR . . . . C37 C 0.61734(9) 0.73997(10) 0.33867(9) 0.0145(3) Uani 1 1 d . U . . . C38 C 0.62210(9) 0.72966(10) 0.40789(9) 0.0148(3) Uani 1 1 d . U . . . C39 C 0.59231(10) 0.79135(11) 0.43506(9) 0.0166(3) Uani 1 1 d . U . . . H39 H 0.595373 0.786997 0.482098 0.020 Uiso 1 1 calc R . . . . C40 C 0.55825(10) 0.85900(11) 0.39474(9) 0.0174(4) Uani 1 1 d . U . . . H40 H 0.538803 0.900684 0.414483 0.021 Uiso 1 1 calc R . . . . C41 C 0.55244(10) 0.86608(11) 0.32551(9) 0.0178(4) Uani 1 1 d . U . . . H41 H 0.528045 0.912205 0.298103 0.021 Uiso 1 1 calc R . . . . C42 C 0.58174(10) 0.80676(11) 0.29571(9) 0.0161(3) Uani 1 1 d . U . . . C43 C 0.65678(10) 0.65538(11) 0.45069(9) 0.0164(3) Uani 1 1 d . U . . . C44 C 0.73148(10) 0.65951(11) 0.50462(10) 0.0201(4) Uani 1 1 d . U . . . C45 C 0.77920(10) 0.73590(12) 0.51721(10) 0.0237(4) Uani 1 1 d . U . . . H45 H 0.743298 0.783002 0.502531 0.028 Uiso 1 1 calc R . . . . C46 C 0.82314(12) 0.73509(15) 0.46946(12) 0.0340(5) Uani 1 1 d . U . . . H46A H 0.857906 0.688578 0.481804 0.051 Uiso 1 1 calc GR . . . . H46B H 0.852679 0.785231 0.476468 0.051 Uiso 1 1 calc GR . . . . H46C H 0.786884 0.730938 0.419611 0.051 Uiso 1 1 calc GR . . . . C47 C 0.83357(12) 0.74842(14) 0.59483(12) 0.0339(5) Uani 1 1 d . U . . . H47A H 0.804828 0.745512 0.624658 0.051 Uiso 1 1 calc GR . . . . H47B H 0.857929 0.801659 0.600415 0.051 Uiso 1 1 calc GR . . . . H47C H 0.872859 0.706140 0.609289 0.051 Uiso 1 1 calc GR . . . . C48 C 0.76206(11) 0.58999(12) 0.54452(11) 0.0260(4) Uani 1 1 d . U . . . H48 H 0.812496 0.591394 0.580694 0.031 Uiso 1 1 calc R . . . . C49 C 0.72039(12) 0.51917(12) 0.53242(11) 0.0294(4) Uani 1 1 d . U . . . H49 H 0.742229 0.472564 0.560360 0.035 Uiso 1 1 calc R . . . . C50 C 0.61401(10) 0.58363(11) 0.43788(10) 0.0198(4) Uani 1 1 d . U . . . C51 C 0.64712(12) 0.51576(12) 0.47989(11) 0.0267(4) Uani 1 1 d . U . . . H51 H 0.618839 0.466794 0.472162 0.032 Uiso 1 1 calc R . . . . C52 C 0.53341(11) 0.57688(11) 0.37998(10) 0.0224(4) Uani 1 1 d . U . . . H52 H 0.518887 0.630740 0.356037 0.027 Uiso 1 1 calc R . . . . C53 C 0.52950(13) 0.51416(13) 0.32386(11) 0.0314(5) Uani 1 1 d . U . . . H53A H 0.567429 0.527476 0.304954 0.047 Uiso 1 1 calc GR . . . . H53B H 0.478295 0.514639 0.285163 0.047 Uiso 1 1 calc GR . . . . H53C H 0.540273 0.460244 0.345573 0.047 Uiso 1 1 calc GR . . . . C54 C 0.47476(12) 0.55458(14) 0.41000(12) 0.0323(5) Uani 1 1 d . U . . . H54A H 0.487089 0.501170 0.432559 0.048 Uiso 1 1 calc GR . . . . H54B H 0.423537 0.553260 0.371345 0.048 Uiso 1 1 calc GR . . . . H54C H 0.476157 0.595046 0.445275 0.048 Uiso 1 1 calc GR . . . . C55 C 0.57481(11) 0.81275(11) 0.22085(10) 0.0192(4) Uani 1 1 d . U . . . C56 C 0.50591(11) 0.79037(12) 0.16445(10) 0.0239(4) Uani 1 1 d . U . . . C57 C 0.43840(12) 0.75884(13) 0.17813(11) 0.0300(4) Uani 1 1 d . U . . . H57 H 0.441150 0.783642 0.223369 0.036 Uiso 1 1 calc R . . . . C58 C 0.44451(14) 0.66759(15) 0.18818(12) 0.0385(5) Uani 1 1 d . U . . . H58A H 0.442492 0.641855 0.144620 0.058 Uiso 1 1 calc GR . . . . H58B H 0.401959 0.647967 0.198644 0.058 Uiso 1 1 calc GR . . . . H58C H 0.493014 0.654093 0.227762 0.058 Uiso 1 1 calc GR . . . . C59 C 0.36089(14) 0.78144(17) 0.11894(16) 0.0506(7) Uani 1 1 d . U . . . H59A H 0.358958 0.840005 0.110728 0.076 Uiso 1 1 calc GR . . . . H59B H 0.319813 0.765812 0.133143 0.076 Uiso 1 1 calc GR . . . . H59C H 0.354388 0.752932 0.075150 0.076 Uiso 1 1 calc GR . . . . C60 C 0.50108(14) 0.79554(13) 0.09548(11) 0.0331(5) Uani 1 1 d . U . . . H60 H 0.455068 0.780244 0.056833 0.040 Uiso 1 1 calc R . . . . C61 C 0.56213(15) 0.82256(13) 0.08235(12) 0.0371(5) Uani 1 1 d . U . . . H61 H 0.557930 0.825321 0.034870 0.045 Uiso 1 1 calc R . . . . C62 C 0.62903(14) 0.84554(14) 0.13744(12) 0.0354(5) Uani 1 1 d . U . . . H62 H 0.670407 0.864739 0.127590 0.042 Uiso 1 1 calc R . . . . C63 C 0.63689(12) 0.84101(12) 0.20775(11) 0.0269(4) Uani 1 1 d . U . . . C64 C 0.71024(12) 0.86951(16) 0.26702(13) 0.0378(5) Uani 1 1 d . U . . . H64 H 0.709637 0.851625 0.313131 0.045 Uiso 1 1 calc R . . . . C65 C 0.78121(16) 0.83315(19) 0.2617(2) 0.0614(8) Uani 1 1 d . U . . . H65A H 0.775741 0.774173 0.257086 0.092 Uiso 1 1 calc GR . . . . H65B H 0.826611 0.846634 0.304551 0.092 Uiso 1 1 calc GR . . . . H65C H 0.786680 0.855372 0.219906 0.092 Uiso 1 1 calc GR . . . . C66 C 0.71451(16) 0.96161(18) 0.26766(18) 0.0545(7) Uani 1 1 d . U . . . H66A H 0.714561 0.980657 0.222658 0.082 Uiso 1 1 calc GR . . . . H66B H 0.761532 0.979325 0.307089 0.082 Uiso 1 1 calc GR . . . . H66C H 0.670189 0.984098 0.273633 0.082 Uiso 1 1 calc GR . . . . C5 C 0.8216(5) 0.6183(8) 0.2924(5) 0.038(2) Uani 0.568(4) 1 d . U . A 1 C6 C 0.6506(13) 0.4805(9) 0.2333(11) 0.032(3) Uani 0.432(4) 1 d . U . A 2 O1S O 1.000000 1.000000 0.500000 0.095(2) Uani 0.932(13) 2 d S TU P . . C1S2 C 1.0097(4) 0.9566(4) 0.4523(3) 0.0666(12) Uani 0.546(4) 1 d . U . B 1 H1SA H 1.055078 0.921753 0.475898 0.080 Uiso 0.546(4) 1 calc R . . B 1 H1SB H 1.020413 0.993048 0.419383 0.080 Uiso 0.546(4) 1 calc R . . B 1 C2S2 C 0.9452(4) 0.9059(4) 0.4115(4) 0.0686(13) Uani 0.546(4) 1 d . U . B 1 H2SA H 0.957129 0.874524 0.376930 0.103 Uiso 0.546(4) 1 calc GR . . B 1 H2SB H 0.900338 0.939924 0.386319 0.103 Uiso 0.546(4) 1 calc GR . . B 1 H2SC H 0.934529 0.868912 0.443432 0.103 Uiso 0.546(4) 1 calc GR . . B 1 C1S C 0.9578(4) 0.9394(5) 0.4645(4) 0.0666(12) Uani 0.454(4) 1 d . U . B 2 H1SC H 0.909860 0.962181 0.428487 0.080 Uiso 0.454(4) 1 calc R . . B 2 H1SD H 0.943845 0.907255 0.497910 0.080 Uiso 0.454(4) 1 calc R . . B 2 C2S C 0.9895(5) 0.8821(5) 0.4271(5) 0.0686(13) Uani 0.454(4) 1 d . U . B 2 H2SD H 0.949251 0.844849 0.397612 0.103 Uiso 0.454(4) 1 calc GR . . B 2 H2SE H 1.031645 0.851183 0.462214 0.103 Uiso 0.454(4) 1 calc GR . . B 2 H2SF H 1.008408 0.912826 0.396838 0.103 Uiso 0.454(4) 1 calc GR . . 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 Mn01 0.02260(17) 0.01948(17) 0.02497(18) -0.00434(12) 0.01090(13) 0.00375(12) F4 0.0465(16) 0.0445(17) 0.072(2) 0.0030(14) 0.0007(14) -0.0051(12) F2 0.044(3) 0.052(4) 0.056(4) -0.020(3) 0.033(3) 0.011(3) F1 0.071(5) 0.044(4) 0.133(7) -0.035(4) 0.073(4) -0.012(3) F3 0.050(2) 0.087(3) 0.071(3) -0.011(2) 0.033(2) -0.017(2) O1 0.0969(16) 0.0633(13) 0.0436(11) 0.0197(10) 0.0395(11) 0.0338(12) O2 0.1102(19) 0.0855(17) 0.0359(11) 0.0177(11) 0.0289(11) 0.0567(15) O4 0.0190(17) 0.054(2) 0.138(4) -0.062(2) 0.018(2) -0.0120(16) O3 0.061(3) 0.111(6) 0.163(7) -0.106(6) 0.075(4) -0.051(4) N1 0.0191(7) 0.0192(8) 0.0249(8) -0.0015(7) 0.0084(6) 0.0031(6) N2 0.0203(7) 0.0135(7) 0.0164(7) 0.0000(6) 0.0081(6) 0.0019(6) C1 0.0196(9) 0.0244(10) 0.0239(10) -0.0024(8) 0.0064(7) -0.0001(8) C2 0.0210(8) 0.0195(9) 0.0179(9) 0.0008(7) 0.0066(7) 0.0018(7) C3 0.0492(13) 0.0343(12) 0.0397(13) 0.0013(10) 0.0265(11) 0.0152(10) C4 0.0568(15) 0.0464(15) 0.0317(13) -0.0019(11) 0.0164(11) 0.0267(12) C7 0.0217(9) 0.0155(9) 0.0310(10) -0.0009(8) 0.0143(8) 0.0028(7) C8 0.0235(9) 0.0226(10) 0.0331(11) -0.0002(8) 0.0117(8) 0.0041(8) C9 0.0241(10) 0.0308(11) 0.0433(13) -0.0029(10) 0.0136(9) 0.0087(9) C10 0.0312(11) 0.0277(11) 0.0494(14) -0.0090(10) 0.0209(10) 0.0065(9) C11 0.0288(10) 0.0227(10) 0.0370(12) -0.0089(9) 0.0165(9) -0.0010(8) C12 0.0229(9) 0.0169(9) 0.0315(10) -0.0004(8) 0.0146(8) -0.0009(7) C13 0.0240(9) 0.0183(9) 0.0280(10) -0.0085(8) 0.0098(8) 0.0010(7) C14 0.0255(10) 0.0285(11) 0.0339(11) -0.0139(9) 0.0135(8) -0.0025(8) C15 0.0233(10) 0.0551(15) 0.0436(14) -0.0223(12) 0.0123(10) -0.0019(10) C16 0.0306(12) 0.0645(18) 0.0398(14) -0.0162(12) 0.0013(10) 0.0156(12) C17 0.0482(14) 0.0379(13) 0.0330(13) -0.0035(10) 0.0024(10) 0.0164(11) C18 0.0382(11) 0.0215(10) 0.0303(11) -0.0066(8) 0.0098(9) 0.0036(9) C19 0.0556(15) 0.0268(12) 0.0378(13) 0.0025(10) 0.0186(11) -0.0038(10) C20 0.089(2) 0.061(2) 0.0583(19) -0.0094(16) 0.0425(18) -0.0148(17) C21 0.111(3) 0.0290(15) 0.102(3) 0.0054(16) 0.051(2) -0.0034(17) C22 0.0343(11) 0.0364(12) 0.0439(13) -0.0047(10) 0.0221(10) -0.0090(10) C23 0.0574(16) 0.0314(13) 0.0746(19) -0.0004(13) 0.0397(15) -0.0073(12) C24 0.0552(16) 0.073(2) 0.0605(18) -0.0099(15) 0.0398(15) -0.0187(15) C25 0.0196(9) 0.0315(11) 0.0317(11) -0.0016(9) 0.0075(8) 0.0103(8) C26 0.0263(10) 0.0489(14) 0.0350(12) 0.0010(10) 0.0128(9) 0.0113(10) C27 0.0352(12) 0.0596(17) 0.0430(14) 0.0059(12) 0.0188(11) -0.0002(11) C28 0.0398(14) 0.0608(18) 0.077(2) 0.0203(16) 0.0279(14) 0.0067(13) C29 0.0404(14) 0.0492(17) 0.081(2) 0.0010(15) 0.0176(14) 0.0073(12) C30 0.0407(13) 0.0614(17) 0.0379(13) -0.0027(12) 0.0190(11) 0.0095(12) C31 0.0397(13) 0.0641(17) 0.0329(13) -0.0135(12) 0.0088(10) 0.0156(12) C32 0.0345(12) 0.0348(12) 0.0427(13) -0.0100(10) 0.0070(10) 0.0084(10) C33 0.0266(10) 0.0286(11) 0.0350(12) -0.0038(9) 0.0065(9) 0.0119(8) C34 0.0427(12) 0.0263(11) 0.0385(13) -0.0024(10) 0.0078(10) -0.0013(10) C35 0.0350(13) 0.0633(18) 0.0561(17) 0.0026(14) 0.0198(12) 0.0090(12) C36 0.0318(13) 0.065(2) 0.105(3) 0.0498(19) 0.0149(15) 0.0017(13) C37 0.0161(8) 0.0129(8) 0.0162(8) -0.0022(6) 0.0084(7) 0.0000(6) C38 0.0145(7) 0.0124(8) 0.0171(8) 0.0004(7) 0.0061(6) -0.0018(6) C39 0.0205(8) 0.0156(8) 0.0154(8) -0.0011(7) 0.0090(7) -0.0028(7) C40 0.0210(8) 0.0131(8) 0.0210(9) -0.0020(7) 0.0114(7) 0.0004(7) C41 0.0209(8) 0.0133(8) 0.0195(9) 0.0021(7) 0.0084(7) 0.0023(7) C42 0.0177(8) 0.0150(8) 0.0167(8) 0.0003(7) 0.0082(7) -0.0005(7) C43 0.0220(8) 0.0143(8) 0.0154(8) 0.0014(7) 0.0101(7) 0.0026(7) C44 0.0229(9) 0.0192(9) 0.0199(9) 0.0027(7) 0.0105(7) 0.0031(7) C45 0.0196(9) 0.0214(10) 0.0256(10) 0.0033(8) 0.0047(7) 0.0007(7) C46 0.0310(11) 0.0402(13) 0.0292(11) 0.0032(10) 0.0108(9) -0.0104(9) C47 0.0299(11) 0.0365(12) 0.0294(11) -0.0030(9) 0.0061(9) -0.0035(9) C48 0.0248(9) 0.0258(10) 0.0257(10) 0.0077(8) 0.0086(8) 0.0075(8) C49 0.0364(11) 0.0204(10) 0.0314(11) 0.0110(8) 0.0139(9) 0.0096(8) C50 0.0259(9) 0.0156(9) 0.0199(9) 0.0003(7) 0.0112(7) 0.0010(7) C51 0.0369(11) 0.0146(9) 0.0315(11) 0.0036(8) 0.0169(9) 0.0006(8) C52 0.0295(10) 0.0139(9) 0.0218(9) -0.0014(7) 0.0085(8) -0.0053(7) C53 0.0422(12) 0.0257(11) 0.0274(11) -0.0070(9) 0.0154(9) -0.0075(9) C54 0.0294(10) 0.0397(13) 0.0272(11) -0.0074(9) 0.0110(9) -0.0066(9) C55 0.0283(9) 0.0139(9) 0.0184(9) 0.0041(7) 0.0127(7) 0.0076(7) C56 0.0345(10) 0.0165(9) 0.0197(9) -0.0004(7) 0.0099(8) 0.0066(8) C57 0.0307(10) 0.0309(11) 0.0240(10) -0.0066(9) 0.0067(8) -0.0026(9) C58 0.0465(13) 0.0361(13) 0.0301(12) 0.0034(10) 0.0128(10) -0.0039(10) C59 0.0356(13) 0.0429(15) 0.0585(17) 0.0089(13) 0.0042(12) -0.0003(11) C60 0.0529(13) 0.0251(11) 0.0179(10) -0.0009(8) 0.0109(9) 0.0111(10) C61 0.0700(15) 0.0267(11) 0.0226(10) 0.0080(9) 0.0272(11) 0.0201(11) C62 0.0534(13) 0.0306(12) 0.0379(12) 0.0141(10) 0.0347(11) 0.0150(10) C63 0.0349(10) 0.0239(10) 0.0293(10) 0.0087(8) 0.0205(9) 0.0075(8) C64 0.0299(11) 0.0482(14) 0.0415(13) 0.0104(11) 0.0209(10) -0.0026(10) C65 0.0369(13) 0.0510(17) 0.100(2) 0.0123(17) 0.0320(15) 0.0068(12) C66 0.0372(13) 0.0535(16) 0.070(2) -0.0154(15) 0.0192(13) -0.0031(12) C5 0.013(3) 0.041(4) 0.045(4) -0.028(3) -0.003(2) 0.003(3) C6 0.040(5) 0.015(4) 0.038(5) 0.010(4) 0.014(4) -0.006(4) O1S 0.128(4) 0.090(3) 0.078(3) -0.026(2) 0.052(3) -0.035(3) C1S2 0.064(3) 0.079(3) 0.060(3) 0.001(2) 0.028(2) -0.002(2) C2S2 0.055(3) 0.077(4) 0.078(3) -0.003(3) 0.031(3) 0.009(3) C1S 0.064(3) 0.079(3) 0.060(3) 0.001(2) 0.028(2) -0.002(2) C2S 0.055(3) 0.077(4) 0.078(3) -0.003(3) 0.031(3) 0.009(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 Mn01 F2 88.7(2) . . C1 Mn01 F1 90.4(3) . . C1 Mn01 C2 179.06(8) . . C1 Mn01 C6 88.3(6) . . C2 Mn01 F2 90.5(2) . . C2 Mn01 F1 90.4(3) . . C2 Mn01 C6 90.9(6) . . C3 Mn01 F2 89.9(3) . . C3 Mn01 F1 89.2(4) . . C3 Mn01 C1 90.08(9) . . C3 Mn01 C2 90.37(9) . . C3 Mn01 C6 94.2(6) . . C4 Mn01 F2 90.4(3) . . C4 Mn01 F1 90.5(4) . . C4 Mn01 C1 91.00(9) . . C4 Mn01 C2 88.55(9) . . C4 Mn01 C3 178.88(10) . . C4 Mn01 C6 86.2(6) . . C5 Mn01 F2 178.0(4) . . C5 Mn01 C1 89.5(4) . . C5 Mn01 C2 91.3(4) . . C5 Mn01 C3 90.8(4) . . C5 Mn01 C4 88.9(4) . . C6 Mn01 F1 176.4(6) . . Mn01 F2 H4 118(3) . . C1 N1 C7 179.2(2) . . C2 N2 C37 175.69(18) . . N1 C1 Mn01 179.84(19) . . N2 C2 Mn01 178.33(17) . . O1 C3 Mn01 179.7(2) . . O2 C4 Mn01 179.1(2) . . N1 C7 C12 118.11(16) . . C8 C7 N1 118.35(17) . . C8 C7 C12 123.52(17) . . C7 C8 C25 120.03(17) . . C9 C8 C7 117.03(19) . . C9 C8 C25 122.91(18) . . C8 C9 H9 119.5 . . C10 C9 C8 121.01(19) . . C10 C9 H9 119.5 . . C9 C10 H10 119.7 . . C9 C10 C11 120.52(19) . . C11 C10 H10 119.7 . . C10 C11 H11 119.6 . . C10 C11 C12 120.8(2) . . C12 C11 H11 119.6 . . C7 C12 C13 119.50(16) . . C11 C12 C7 117.07(18) . . C11 C12 C13 123.43(18) . . C14 C13 C12 118.63(18) . . C18 C13 C12 119.92(18) . . C18 C13 C14 121.36(19) . . C13 C14 C22 120.91(18) . . C15 C14 C13 117.9(2) . . C15 C14 C22 121.1(2) . . C14 C15 H15 119.3 . . C16 C15 C14 121.4(2) . . C16 C15 H15 119.3 . . C15 C16 H16 120.0 . . C15 C16 C17 120.1(2) . . C17 C16 H16 120.0 . . C16 C17 H17 119.5 . . C16 C17 C18 121.1(2) . . C18 C17 H17 119.5 . . C13 C18 C19 121.6(2) . . C17 C18 C13 118.2(2) . . C17 C18 C19 120.1(2) . . C18 C19 H19 107.1 . . C18 C19 C20 110.4(2) . . C18 C19 C21 113.2(3) . . C20 C19 H19 107.1 . . C21 C19 H19 107.1 . . C21 C19 C20 111.6(3) . . C19 C20 H20A 109.5 . . C19 C20 H20B 109.5 . . C19 C20 H20C 109.5 . . H20A C20 H20B 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . C19 C21 H21A 109.5 . . C19 C21 H21B 109.5 . . C19 C21 H21C 109.5 . . H21A C21 H21B 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . C14 C22 H22 107.2 . . C14 C22 C23 110.1(2) . . C14 C22 C24 113.8(2) . . C23 C22 H22 107.2 . . C23 C22 C24 110.9(2) . . C24 C22 H22 107.2 . . C22 C23 H23A 109.5 . . C22 C23 H23B 109.5 . . C22 C23 H23C 109.5 . . H23A C23 H23B 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . C22 C24 H24A 109.5 . . C22 C24 H24B 109.5 . . C22 C24 H24C 109.5 . . H24A C24 H24B 109.5 . . H24A C24 H24C 109.5 . . H24B C24 H24C 109.5 . . C26 C25 C8 118.3(2) . . C26 C25 C33 121.8(2) . . C33 C25 C8 119.79(19) . . C25 C26 C27 122.0(2) . . C30 C26 C25 118.0(2) . . C30 C26 C27 120.0(2) . . C26 C27 H27 107.0 . . C28 C27 C26 113.0(2) . . C28 C27 H27 107.0 . . C29 C27 C26 112.4(2) . . C29 C27 H27 107.0 . . C29 C27 C28 110.1(2) . . C27 C28 H28A 109.5 . . C27 C28 H28B 109.5 . . C27 C28 H28C 109.5 . . H28A C28 H28B 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . C27 C29 H29A 109.5 . . C27 C29 H29B 109.5 . . C27 C29 H29C 109.5 . . H29A C29 H29B 109.5 . . H29A C29 H29C 109.5 . . H29B C29 H29C 109.5 . . C26 C30 H30 119.6 . . C31 C30 C26 120.9(2) . . C31 C30 H30 119.6 . . C30 C31 H31 119.7 . . C30 C31 C32 120.6(2) . . C32 C31 H31 119.7 . . C31 C32 H32 119.5 . . C31 C32 C33 121.1(2) . . C33 C32 H32 119.5 . . C25 C33 C34 121.5(2) . . C32 C33 C25 117.6(2) . . C32 C33 C34 120.8(2) . . C33 C34 H34 107.3 . . C33 C34 C35 113.8(2) . . C35 C34 H34 107.3 . . C36 C34 C33 111.8(2) . . C36 C34 H34 107.3 . . C36 C34 C35 108.9(2) . . C34 C35 H35A 109.5 . . C34 C35 H35B 109.5 . . C34 C35 H35C 109.5 . . H35A C35 H35B 109.5 . . H35A C35 H35C 109.5 . . H35B C35 H35C 109.5 . . C34 C36 H36A 109.5 . . C34 C36 H36B 109.5 . . C34 C36 H36C 109.5 . . H36A C36 H36B 109.5 . . H36A C36 H36C 109.5 . . H36B C36 H36C 109.5 . . N2 C37 C38 118.44(15) . . N2 C37 C42 118.20(15) . . C38 C37 C42 123.35(15) . . C37 C38 C43 121.82(15) . . C39 C38 C37 116.97(16) . . C39 C38 C43 121.21(15) . . C38 C39 H39 119.4 . . C40 C39 C38 121.22(16) . . C40 C39 H39 119.4 . . C39 C40 H40 119.9 . . C39 C40 C41 120.26(16) . . C41 C40 H40 119.9 . . C40 C41 H41 119.4 . . C40 C41 C42 121.11(16) . . C42 C41 H41 119.4 . . C37 C42 C55 121.16(15) . . C41 C42 C37 117.03(16) . . C41 C42 C55 121.80(16) . . C44 C43 C38 119.19(16) . . C50 C43 C38 119.72(15) . . C50 C43 C44 121.06(16) . . C43 C44 C45 121.45(16) . . C48 C44 C43 118.15(17) . . C48 C44 C45 120.33(17) . . C44 C45 H45 107.6 . . C44 C45 C46 109.48(17) . . C44 C45 C47 113.44(17) . . C46 C45 H45 107.6 . . C47 C45 H45 107.6 . . C47 C45 C46 110.81(17) . . C45 C46 H46A 109.5 . . C45 C46 H46B 109.5 . . C45 C46 H46C 109.5 . . H46A C46 H46B 109.5 . . H46A C46 H46C 109.5 . . H46B C46 H46C 109.5 . . C45 C47 H47A 109.5 . . C45 C47 H47B 109.5 . . C45 C47 H47C 109.5 . . H47A C47 H47B 109.5 . . H47A C47 H47C 109.5 . . H47B C47 H47C 109.5 . . C44 C48 H48 119.4 . . C49 C48 C44 121.21(18) . . C49 C48 H48 119.4 . . C48 C49 H49 119.9 . . C48 C49 C51 120.30(18) . . C51 C49 H49 119.9 . . C43 C50 C52 122.49(16) . . C51 C50 C43 118.50(17) . . C51 C50 C52 119.01(17) . . C49 C51 C50 120.76(19) . . C49 C51 H51 119.6 . . C50 C51 H51 119.6 . . C50 C52 H52 108.1 . . C50 C52 C53 111.26(16) . . C50 C52 C54 112.19(16) . . C53 C52 H52 108.1 . . C53 C52 C54 108.94(16) . . C54 C52 H52 108.1 . . C52 C53 H53A 109.5 . . C52 C53 H53B 109.5 . . C52 C53 H53C 109.5 . . H53A C53 H53B 109.5 . . H53A C53 H53C 109.5 . . H53B C53 H53C 109.5 . . C52 C54 H54A 109.5 . . C52 C54 H54B 109.5 . . C52 C54 H54C 109.5 . . H54A C54 H54B 109.5 . . H54A C54 H54C 109.5 . . H54B C54 H54C 109.5 . . C56 C55 C42 119.53(16) . . C63 C55 C42 119.67(17) . . C63 C55 C56 120.80(17) . . C55 C56 C57 121.21(17) . . C60 C56 C55 118.52(19) . . C60 C56 C57 120.24(19) . . C56 C57 H57 107.9 . . C56 C57 C59 112.90(19) . . C58 C57 C56 109.88(18) . . C58 C57 H57 107.9 . . C58 C57 C59 110.20(19) . . C59 C57 H57 107.9 . . C57 C58 H58A 109.5 . . C57 C58 H58B 109.5 . . C57 C58 H58C 109.5 . . H58A C58 H58B 109.5 . . H58A C58 H58C 109.5 . . H58B C58 H58C 109.5 . . C57 C59 H59A 109.5 . . C57 C59 H59B 109.5 . . C57 C59 H59C 109.5 . . H59A C59 H59B 109.5 . . H59A C59 H59C 109.5 . . H59B C59 H59C 109.5 . . C56 C60 H60 119.5 . . C61 C60 C56 120.9(2) . . C61 C60 H60 119.5 . . C60 C61 H61 119.8 . . C62 C61 C60 120.50(19) . . C62 C61 H61 119.8 . . C61 C62 H62 119.6 . . C61 C62 C63 120.8(2) . . C63 C62 H62 119.6 . . C55 C63 C64 121.97(18) . . C62 C63 C55 118.5(2) . . C62 C63 C64 119.50(19) . . C63 C64 H64 108.0 . . C63 C64 C65 112.3(2) . . C63 C64 C66 110.3(2) . . C65 C64 H64 108.0 . . C66 C64 H64 108.0 . . C66 C64 C65 110.2(2) . . C64 C65 H65A 109.5 . . C64 C65 H65B 109.5 . . C64 C65 H65C 109.5 . . H65A C65 H65B 109.5 . . H65A C65 H65C 109.5 . . H65B C65 H65C 109.5 . . C64 C66 H66A 109.5 . . C64 C66 H66B 109.5 . . C64 C66 H66C 109.5 . . H66A C66 H66B 109.5 . . H66A C66 H66C 109.5 . . H66B C66 H66C 109.5 . . O4 C5 Mn01 171.7(10) . . O3 C6 Mn01 162.8(16) . . C1S2 O1S C1S2 180.0(5) . 3_776 C1S2 O1S C1S 127.2(4) . 3_776 C1S2 O1S C1S 52.8(4) 3_776 3_776 C1S O1S C1S 180.0(7) 3_776 . O1S C1S2 H1SA 108.7 . . O1S C1S2 H1SB 108.7 . . O1S C1S2 C2S2 114.3(5) . . H1SA C1S2 H1SB 107.6 . . C2S2 C1S2 H1SA 108.7 . . C2S2 C1S2 H1SB 108.7 . . C1S2 C2S2 H2SA 109.5 . . C1S2 C2S2 H2SB 109.5 . . C1S2 C2S2 H2SC 109.5 . . H2SA C2S2 H2SB 109.5 . . H2SA C2S2 H2SC 109.5 . . H2SB C2S2 H2SC 109.5 . . O1S C1S H1SC 107.6 . . O1S C1S H1SD 107.6 . . O1S C1S C2S 119.0(6) . . H1SC C1S H1SD 107.0 . . C2S C1S H1SC 107.6 . . C2S C1S H1SD 107.6 . . C1S C2S H2SD 109.5 . . C1S C2S H2SE 109.5 . . C1S C2S H2SF 109.5 . . H2SD C2S H2SE 109.5 . . H2SD C2S H2SF 109.5 . . H2SE C2S H2SF 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mn01 F2 1.943(11) . Mn01 F1 2.002(12) . Mn01 C1 1.927(2) . Mn01 C2 1.9343(19) . Mn01 C3 1.873(2) . Mn01 C4 1.870(3) . Mn01 C5 1.811(12) . Mn01 C6 1.955(19) . F4 H4 1.20(5) . F2 H4 1.10(5) . O1 C3 1.133(3) . O2 C4 1.144(3) . O4 C5 1.153(13) . O3 C6 1.00(3) . N1 C1 1.155(3) . N1 C7 1.399(2) . N2 C2 1.152(2) . N2 C37 1.402(2) . C7 C8 1.398(3) . C7 C12 1.402(3) . C8 C9 1.396(3) . C8 C25 1.494(3) . C9 H9 0.9500 . C9 C10 1.386(3) . C10 H10 0.9500 . C10 C11 1.389(3) . C11 H11 0.9500 . C11 C12 1.396(3) . C12 C13 1.496(3) . C13 C14 1.408(3) . C13 C18 1.401(3) . C14 C15 1.395(3) . C14 C22 1.509(3) . C15 H15 0.9500 . C15 C16 1.375(4) . C16 H16 0.9500 . C16 C17 1.381(4) . C17 H17 0.9500 . C17 C18 1.397(3) . C18 C19 1.517(3) . C19 H19 1.0000 . C19 C20 1.525(4) . C19 C21 1.518(4) . C20 H20A 0.9800 . C20 H20B 0.9800 . C20 H20C 0.9800 . C21 H21A 0.9800 . C21 H21B 0.9800 . C21 H21C 0.9800 . C22 H22 1.0000 . C22 C23 1.530(3) . C22 C24 1.532(3) . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . C24 H24A 0.9800 . C24 H24B 0.9800 . C24 H24C 0.9800 . C25 C26 1.407(3) . C25 C33 1.408(3) . C26 C27 1.526(4) . C26 C30 1.391(4) . C27 H27 1.0000 . C27 C28 1.525(3) . C27 C29 1.514(4) . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C29 H29A 0.9800 . C29 H29B 0.9800 . C29 H29C 0.9800 . C30 H30 0.9500 . C30 C31 1.380(4) . C31 H31 0.9500 . C31 C32 1.382(4) . C32 H32 0.9500 . C32 C33 1.393(3) . C33 C34 1.523(3) . C34 H34 1.0000 . C34 C35 1.529(4) . C34 C36 1.514(4) . C35 H35A 0.9800 . C35 H35B 0.9800 . C35 H35C 0.9800 . C36 H36A 0.9800 . C36 H36B 0.9800 . C36 H36C 0.9800 . C37 C38 1.403(2) . C37 C42 1.405(2) . C38 C39 1.392(2) . C38 C43 1.499(2) . C39 H39 0.9500 . C39 C40 1.387(3) . C40 H40 0.9500 . C40 C41 1.390(3) . C41 H41 0.9500 . C41 C42 1.391(2) . C42 C55 1.497(2) . C43 C44 1.411(3) . C43 C50 1.403(3) . C44 C45 1.517(3) . C44 C48 1.394(3) . C45 H45 1.0000 . C45 C46 1.535(3) . C45 C47 1.526(3) . C46 H46A 0.9800 . C46 H46B 0.9800 . C46 H46C 0.9800 . C47 H47A 0.9800 . C47 H47B 0.9800 . C47 H47C 0.9800 . C48 H48 0.9500 . C48 C49 1.380(3) . C49 H49 0.9500 . C49 C51 1.381(3) . C50 C51 1.400(3) . C50 C52 1.522(3) . C51 H51 0.9500 . C52 H52 1.0000 . C52 C53 1.532(3) . C52 C54 1.533(3) . C53 H53A 0.9800 . C53 H53B 0.9800 . C53 H53C 0.9800 . C54 H54A 0.9800 . C54 H54B 0.9800 . C54 H54C 0.9800 . C55 C56 1.407(3) . C55 C63 1.403(3) . C56 C57 1.524(3) . C56 C60 1.389(3) . C57 H57 1.0000 . C57 C58 1.519(3) . C57 C59 1.535(3) . C58 H58A 0.9800 . C58 H58B 0.9800 . C58 H58C 0.9800 . C59 H59A 0.9800 . C59 H59B 0.9800 . C59 H59C 0.9800 . C60 H60 0.9500 . C60 C61 1.379(4) . C61 H61 0.9500 . C61 C62 1.374(4) . C62 H62 0.9500 . C62 C63 1.397(3) . C63 C64 1.513(3) . C64 H64 1.0000 . C64 C65 1.532(3) . C64 C66 1.523(4) . C65 H65A 0.9800 . C65 H65B 0.9800 . C65 H65C 0.9800 . C66 H66A 0.9800 . C66 H66B 0.9800 . C66 H66C 0.9800 . O1S C1S2 1.289(7) . O1S C1S2 1.289(7) 3_776 O1S C1S 1.307(8) 3_776 O1S C1S 1.307(8) . C1S2 H1SA 0.9900 . C1S2 H1SB 0.9900 . C1S2 C2S2 1.444(9) . C2S2 H2SA 0.9800 . C2S2 H2SB 0.9800 . C2S2 H2SC 0.9800 . C1S H1SC 0.9900 . C1S H1SD 0.9900 . C1S C2S 1.497(11) . C2S H2SD 0.9800 . C2S H2SE 0.9800 . C2S H2SF 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 C7 C8 C9 179.90(18) N1 C7 C8 C25 1.6(3) N1 C7 C12 C11 -179.79(17) N1 C7 C12 C13 -0.7(3) N2 C37 C38 C39 176.67(15) N2 C37 C38 C43 -4.0(2) N2 C37 C42 C41 -177.20(15) N2 C37 C42 C55 3.7(2) C7 C8 C9 C10 -0.7(3) C7 C8 C25 C26 84.9(2) C7 C8 C25 C33 -93.0(2) C7 C12 C13 C14 -81.1(2) C7 C12 C13 C18 95.5(2) C8 C7 C12 C11 -1.2(3) C8 C7 C12 C13 177.88(18) C8 C9 C10 C11 -0.1(4) C8 C25 C26 C27 2.4(3) C8 C25 C26 C30 -177.98(19) C8 C25 C33 C32 177.54(18) C8 C25 C33 C34 -1.4(3) C9 C8 C25 C26 -93.4(2) C9 C8 C25 C33 88.7(3) C9 C10 C11 C12 0.2(3) C10 C11 C12 C7 0.4(3) C10 C11 C12 C13 -178.6(2) C11 C12 C13 C14 97.9(2) C11 C12 C13 C18 -85.4(2) C12 C7 C8 C9 1.3(3) C12 C7 C8 C25 -177.01(19) C12 C13 C14 C15 177.14(18) C12 C13 C14 C22 -5.2(3) C12 C13 C18 C17 -177.08(19) C12 C13 C18 C19 5.1(3) C13 C14 C15 C16 -0.6(3) C13 C14 C22 C23 -84.9(2) C13 C14 C22 C24 150.0(2) C13 C18 C19 C20 99.2(3) C13 C18 C19 C21 -134.9(3) C14 C13 C18 C17 -0.5(3) C14 C13 C18 C19 -178.38(19) C14 C15 C16 C17 0.7(4) C15 C14 C22 C23 92.7(2) C15 C14 C22 C24 -32.5(3) C15 C16 C17 C18 -0.7(4) C16 C17 C18 C13 0.6(3) C16 C17 C18 C19 178.5(2) C17 C18 C19 C20 -78.6(3) C17 C18 C19 C21 47.2(3) C18 C13 C14 C15 0.5(3) C18 C13 C14 C22 178.18(19) C22 C14 C15 C16 -178.2(2) C25 C8 C9 C10 177.6(2) C25 C26 C27 C28 -110.6(3) C25 C26 C27 C29 124.1(3) C25 C26 C30 C31 0.3(3) C25 C33 C34 C35 -141.5(2) C25 C33 C34 C36 94.5(3) C26 C25 C33 C32 -0.3(3) C26 C25 C33 C34 -179.22(19) C26 C30 C31 C32 -0.1(4) C27 C26 C30 C31 179.9(2) C30 C26 C27 C28 69.9(3) C30 C26 C27 C29 -55.5(3) C30 C31 C32 C33 -0.4(4) C31 C32 C33 C25 0.5(3) C31 C32 C33 C34 179.5(2) C32 C33 C34 C35 39.6(3) C32 C33 C34 C36 -84.4(3) C33 C25 C26 C27 -179.70(19) C33 C25 C26 C30 -0.1(3) C37 C38 C39 C40 1.2(2) C37 C38 C43 C44 102.6(2) C37 C38 C43 C50 -79.0(2) C37 C42 C55 C56 98.5(2) C37 C42 C55 C63 -81.8(2) C38 C37 C42 C41 2.2(3) C38 C37 C42 C55 -176.91(16) C38 C39 C40 C41 0.7(3) C38 C43 C44 C45 -3.8(2) C38 C43 C44 C48 178.95(16) C38 C43 C50 C51 -178.37(16) C38 C43 C50 C52 1.9(3) C39 C38 C43 C44 -78.1(2) C39 C38 C43 C50 100.3(2) C39 C40 C41 C42 -1.3(3) C40 C41 C42 C37 -0.1(3) C40 C41 C42 C55 178.95(16) C41 C42 C55 C56 -80.5(2) C41 C42 C55 C63 99.1(2) C42 C37 C38 C39 -2.7(2) C42 C37 C38 C43 176.61(16) C42 C55 C56 C57 -0.9(3) C42 C55 C56 C60 -179.28(17) C42 C55 C63 C62 179.64(17) C42 C55 C63 C64 -2.8(3) C43 C38 C39 C40 -178.12(16) C43 C44 C45 C46 -87.6(2) C43 C44 C45 C47 148.06(18) C43 C44 C48 C49 -0.7(3) C43 C50 C51 C49 -0.4(3) C43 C50 C52 C53 117.51(19) C43 C50 C52 C54 -120.16(19) C44 C43 C50 C51 0.0(3) C44 C43 C50 C52 -179.75(16) C44 C48 C49 C51 0.3(3) C45 C44 C48 C49 -178.02(18) C48 C44 C45 C46 89.6(2) C48 C44 C45 C47 -34.8(3) C48 C49 C51 C50 0.3(3) C50 C43 C44 C45 177.85(17) C50 C43 C44 C48 0.6(3) C51 C50 C52 C53 -62.2(2) C51 C50 C52 C54 60.1(2) C52 C50 C51 C49 179.29(18) C55 C56 C57 C58 -88.4(2) C55 C56 C57 C59 148.1(2) C55 C56 C60 C61 -0.5(3) C55 C63 C64 C65 132.5(2) C55 C63 C64 C66 -104.1(2) C56 C55 C63 C62 -0.7(3) C56 C55 C63 C64 176.84(19) C56 C60 C61 C62 -0.5(3) C57 C56 C60 C61 -178.84(19) C60 C56 C57 C58 89.9(2) C60 C56 C57 C59 -33.6(3) C60 C61 C62 C63 0.8(3) C61 C62 C63 C55 -0.3(3) C61 C62 C63 C64 -177.9(2) C62 C63 C64 C65 -49.9(3) C62 C63 C64 C66 73.4(3) C63 C55 C56 C57 179.41(18) C63 C55 C56 C60 1.1(3)