#------------------------------------------------------------------------------ #$Date: 2017-04-19 05:59:00 +0300 (Wed, 19 Apr 2017) $ #$Revision: 195532 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042716.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_7042716 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 Bi Cl2 Mn N2 O3, C4 H8 O, C4 H7 O' _chemical_formula_sum 'C73 H89 Bi Cl2 Mn N2 O5' _chemical_formula_weight 1409.28 _chemical_name_common Mn(BiCl2)(CO)3(CNArDipp2)2 _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 geom _atom_sites_solution_primary direct _audit_creation_date 2016-05-19 _audit_creation_method ; Olex2 1.2 (compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155) ; _audit_update_record ; 2017-03-20 deposited with the CCDC. 2017-04-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 105.3620(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.0881(10) _cell_length_b 16.5315(9) _cell_length_c 24.8358(14) _cell_measurement_reflns_used 7709 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 25.370 _cell_measurement_theta_min 2.353 _cell_volume 6765.2(7) _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 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SIR2004 (Burla et al., 2007)' _diffrn_ambient_temperature 273.15 _diffrn_detector 'Bruker APEX-II CCD' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _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 0.0500 _diffrn_reflns_av_unetI/netI 0.0528 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 40804 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.450 _diffrn_reflns_theta_min 1.236 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker TXS' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.913 _exptl_absorpt_correction_T_max 0.0186 _exptl_absorpt_correction_T_min 0.0056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0832 before and 0.0511 after correction. The Ratio of minimum to maximum transmission is 0.3011. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour 'clear light red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.384 _exptl_crystal_description block _exptl_crystal_F_000 2892 _exptl_crystal_recrystallization_method 'grown from saturated THF solution at -40C' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.586 _refine_diff_density_min -1.590 _refine_diff_density_rms 0.164 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 773 _refine_ls_number_reflns 12473 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0612 _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^)+(0.1098P)^2^+15.7200P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1749 _refine_ls_wR_factor_ref 0.1873 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9740 _reflns_number_total 12473 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt01102d2.cif _cod_data_source_block jfig947_new_a _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 7042716 _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.a Ternary CH refined with riding coordinates: C60(H60), C30(H30), C63(H63), C33(H33), C51(H51), C18(H18), C21(H21), C48(H48) 2.b Secondary CH2 refined with riding coordinates: C1S(H1SA,H1SB), C4S(H4SA,H4SB), C3S(H3SA,H3SB), C6S(H6SA,H6SB), C5S(H5SA, H5SB), C7S(H7SA,H7SB), C2S(H2SA,H2SB) 2.c Aromatic/amide H refined with riding coordinates: C56(H56), C10(H10), C39(H39), C28(H28), C46(H46), C58(H58), C38(H38), C27(H27), C44(H44), C9(H9), C26(H26), C8(H8), C45(H45), C40(H40), C57(H57), C14(H14), C16(H16), C15(H15), C8S(H8S) 2.d Idealised Me refined as rotating group: C61(H61A,H61B,H61C), C31(H31A,H31B,H31C), C62(H62A,H62B,H62C), C53(H53A,H53B, H53C), C65(H65A,H65B,H65C), C32(H32A,H32B,H32C), C23(H23A,H23B,H23C), C52(H52A, H52B,H52C), C35(H35A,H35B,H35C), C64(H64A,H64B,H64C), C34(H34A,H34B,H34C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C50(H50A,H50B, H50C), C49(H49A,H49B,H49C) ; _shelx_res_file ; jfig947_new_a.res created by SHELXL-2014/7 TITL JFig947_new_a.res in P2(1)/c REM Old TITL JFig947_new in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.116, Rweak 0.007, Alpha 0.043, Orientation as input REM Formula found by SHELXT: C70 N5 O5 Cl2 Mn Bi CELL 0.71073 17.0881 16.5315 24.8358 90 105.362 90 ZERR 4 0.001 0.0009 0.0014 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Bi Cl Mn N O UNIT 292 356 4 8 4 8 20 L.S. 10 PLAN 20 TEMP 0 BOND $H LIST 6 MORE -1 CONF fmap 2 acta OMIT -3 0 4 OMIT 0 1 1 OMIT 1 3 2 OMIT -2 0 4 OMIT 0 6 4 REM REM REM WGHT 0.109800 15.720000 FVAR 0.14179 BI1 3 0.229123 0.735793 0.416921 11.00000 0.03812 0.04408 = 0.04206 -0.00207 0.01272 -0.00281 MN1 5 0.277371 0.665717 0.333311 11.00000 0.02487 0.02702 = 0.02613 0.00011 0.00667 -0.00559 CL1 4 0.283393 0.875646 0.413726 11.00000 0.06756 0.04177 = 0.05034 0.00033 0.02083 0.00032 CL2 4 0.335706 0.694243 0.502494 11.00000 0.05875 0.04920 = 0.04118 -0.00044 0.00859 -0.00388 N2 6 0.135639 0.551228 0.328807 11.00000 0.02547 0.02434 = 0.01900 0.00010 0.00476 0.00060 O1S 7 0.114706 0.867175 0.570015 11.00000 0.04783 0.04433 = 0.03572 -0.00523 0.00839 -0.00328 O2 7 0.319541 0.576237 0.241345 11.00000 0.04458 0.05486 = 0.04319 -0.00999 0.01651 -0.00921 O1 7 0.389102 0.560659 0.418211 11.00000 0.03455 0.04759 = 0.03981 0.00540 0.00507 -0.00361 N1 6 0.409667 0.793257 0.341021 11.00000 0.02216 0.02465 = 0.02600 -0.00086 0.00699 -0.00122 O3 7 0.173076 0.774059 0.258046 11.00000 0.03643 0.07569 = 0.04531 0.01649 0.00246 -0.01508 C42 1 0.390425 0.907858 0.252458 11.00000 0.02440 0.02496 = 0.02631 0.00469 0.00378 -0.00006 C54 1 0.550842 0.775224 0.430327 11.00000 0.01988 0.02410 = 0.02946 0.00202 0.00408 -0.00032 C6 1 0.075511 0.494204 0.329522 11.00000 0.02160 0.02185 = 0.02498 0.00362 0.00422 -0.00105 C7 1 0.033372 0.501572 0.371113 11.00000 0.02796 0.02213 = 0.02207 0.00349 0.00570 0.00334 C5 1 0.189064 0.594634 0.330468 11.00000 0.03109 0.02196 = 0.01982 0.00255 0.00713 0.00609 C43 1 0.322788 0.955450 0.255904 11.00000 0.02785 0.02951 = 0.02555 0.00125 0.00593 -0.00078 C11 1 0.060415 0.431788 0.290983 11.00000 0.02416 0.02340 = 0.02292 0.00317 0.00409 0.00217 C41 1 0.464085 0.905938 0.301220 11.00000 0.02823 0.02512 = 0.02278 -0.00077 0.00504 -0.00094 C24 1 0.052461 0.571618 0.412244 11.00000 0.02675 0.02531 = 0.02579 -0.00261 0.01101 -0.00592 C29 1 0.011189 0.644471 0.398629 11.00000 0.02588 0.02540 = 0.02941 0.00168 0.00809 -0.00256 C12 1 0.105167 0.424899 0.247651 11.00000 0.02800 0.02214 = 0.02941 -0.00446 0.00906 -0.00683 C59 1 0.543634 0.793518 0.483833 11.00000 0.02613 0.03026 = 0.03003 0.00338 0.00497 -0.00032 C37 1 0.543913 0.841156 0.387829 11.00000 0.02443 0.02641 = 0.02521 -0.00144 0.00860 0.00029 C55 1 0.565821 0.695406 0.415624 11.00000 0.01934 0.03181 = 0.03365 0.00221 0.00250 0.00085 C1 1 0.361072 0.744861 0.339434 11.00000 0.02973 0.03031 = 0.02349 0.00149 0.00835 0.00346 C56 1 0.570757 0.634510 0.455730 11.00000 0.02688 0.02652 = 0.03836 0.00571 0.00105 0.00241 AFIX 43 H56 2 0.578968 0.581185 0.446612 11.00000 -1.20000 AFIX 0 C60 1 0.529453 0.879626 0.502063 11.00000 0.03884 0.03143 = 0.03353 0.00478 0.01412 -0.00036 AFIX 13 H60 2 0.507188 0.911831 0.468352 11.00000 -1.20000 AFIX 0 C36 1 0.473075 0.848002 0.343955 11.00000 0.02785 0.01837 = 0.03004 -0.00034 0.01265 -0.00139 C10 1 -0.000060 0.376393 0.294288 11.00000 0.03279 0.02614 = 0.03359 -0.00907 0.01063 -0.00745 AFIX 43 H10 2 -0.013254 0.334904 0.268158 11.00000 -1.20000 AFIX 0 C25 1 0.109284 0.559447 0.463881 11.00000 0.02499 0.02836 = 0.01877 0.00112 0.00873 -0.00349 C39 1 0.600367 0.950660 0.346889 11.00000 0.02961 0.03366 = 0.03465 -0.00395 0.00830 -0.00796 AFIX 43 H39 2 0.643073 0.986177 0.348309 11.00000 -1.20000 AFIX 0 C47 1 0.390636 0.864482 0.204826 11.00000 0.03201 0.03341 = 0.02739 0.00051 0.00601 0.00149 O2S 7 0.789380 0.831629 0.477282 11.00000 0.05804 0.07700 = 0.06565 0.01860 -0.00168 -0.00434 C28 1 0.025323 0.705453 0.438668 11.00000 0.03230 0.02799 = 0.03935 -0.00370 0.01319 0.00181 AFIX 43 H28 2 -0.002445 0.754223 0.430620 11.00000 -1.20000 AFIX 0 C30 1 -0.047682 0.658588 0.341646 11.00000 0.02964 0.02810 = 0.03129 0.00130 0.00565 0.00218 AFIX 13 H30 2 -0.047822 0.610016 0.318999 11.00000 -1.20000 AFIX 0 C46 1 0.321781 0.868577 0.158915 11.00000 0.03987 0.04623 = 0.02358 -0.00841 0.00559 -0.00371 AFIX 43 H46 2 0.321512 0.840384 0.126462 11.00000 -1.20000 AFIX 0 C58 1 0.550339 0.729600 0.522438 11.00000 0.03202 0.03922 = 0.02928 0.00618 0.00774 -0.00166 AFIX 43 H58 2 0.545597 0.740307 0.558200 11.00000 -1.20000 AFIX 0 C38 1 0.607750 0.892917 0.388023 11.00000 0.02901 0.02907 = 0.02170 0.00116 0.00476 -0.00559 AFIX 43 H38 2 0.655939 0.888698 0.416097 11.00000 -1.20000 AFIX 0 C13 1 0.073619 0.459966 0.194255 11.00000 0.03133 0.03377 = 0.03215 0.00616 0.00977 0.00087 C63 1 0.579994 0.676304 0.359137 11.00000 0.02999 0.02694 = 0.03414 0.00060 0.00889 0.00107 AFIX 13 H63 2 0.550857 0.716746 0.332409 11.00000 -1.20000 AFIX 0 C27 1 0.079923 0.694659 0.490139 11.00000 0.04135 0.02978 = 0.03105 -0.00765 0.01728 -0.00703 AFIX 43 H27 2 0.088637 0.735935 0.516504 11.00000 -1.20000 AFIX 0 C33 1 0.153703 0.479783 0.478538 11.00000 0.03076 0.02809 = 0.02580 0.00165 0.00438 0.00169 AFIX 13 H33 2 0.140502 0.446054 0.444886 11.00000 -1.20000 AFIX 0 C44 1 0.255762 0.956715 0.209202 11.00000 0.02966 0.03962 = 0.03351 0.00509 0.00541 0.00830 AFIX 43 H44 2 0.210498 0.987271 0.210261 11.00000 -1.20000 AFIX 0 C17 1 0.179329 0.382258 0.259891 11.00000 0.03257 0.01984 = 0.03022 -0.00578 0.00651 -0.00126 C9 1 -0.040535 0.381842 0.335334 11.00000 0.03171 0.03339 = 0.03804 -0.00333 0.01406 -0.01294 AFIX 43 H9 2 -0.079447 0.343430 0.337293 11.00000 -1.20000 AFIX 0 C4 1 0.303758 0.610918 0.276249 11.00000 0.03220 0.03219 = 0.03306 0.00393 0.01014 -0.00729 C26 1 0.121631 0.622514 0.502486 11.00000 0.03374 0.03643 = 0.02039 0.00086 0.01020 -0.00364 AFIX 43 H26 2 0.158607 0.615901 0.537171 11.00000 -1.20000 AFIX 0 C8 1 -0.023164 0.444888 0.373893 11.00000 0.03166 0.02867 = 0.02727 0.00109 0.01191 -0.00115 AFIX 43 H8 2 -0.050349 0.448250 0.401678 11.00000 -1.20000 AFIX 0 C45 1 0.255332 0.913070 0.160989 11.00000 0.03494 0.05292 = 0.02753 -0.00115 -0.00006 0.00493 AFIX 43 H45 2 0.209997 0.914303 0.130435 11.00000 -1.20000 AFIX 0 C40 1 0.530243 0.956609 0.303421 11.00000 0.02932 0.02830 = 0.02921 0.00353 0.00865 -0.00300 AFIX 43 H40 2 0.527273 0.994774 0.275440 11.00000 -1.20000 AFIX 0 C57 1 0.563707 0.652243 0.507876 11.00000 0.02890 0.03714 = 0.03595 0.00953 0.00029 -0.00504 AFIX 43 H57 2 0.568083 0.610942 0.533932 11.00000 -1.20000 AFIX 0 C51 1 0.323384 1.005189 0.306319 11.00000 0.03461 0.03593 = 0.02969 0.00213 0.01181 0.00204 AFIX 13 H51 2 0.354419 0.975825 0.339381 11.00000 -1.20000 AFIX 0 C14 1 0.117876 0.451311 0.154388 11.00000 0.04554 0.04098 = 0.02799 0.00507 0.01690 0.00366 AFIX 43 H14 2 0.098469 0.475091 0.119452 11.00000 -1.20000 AFIX 0 C61 1 0.470415 0.884049 0.537959 11.00000 0.04977 0.03798 = 0.04451 -0.00102 0.01659 0.00299 AFIX 137 H61A 2 0.420630 0.857706 0.519104 11.00000 -1.50000 H61B 2 0.459706 0.939670 0.544549 11.00000 -1.50000 H61C 2 0.493492 0.857575 0.572974 11.00000 -1.50000 AFIX 0 C2 1 0.346537 0.602422 0.387629 11.00000 0.02208 0.03843 = 0.04135 0.00218 0.01100 -0.00715 C16 1 0.219821 0.374489 0.219194 11.00000 0.03117 0.03007 = 0.04243 -0.00181 0.01151 0.00284 AFIX 43 H16 2 0.268550 0.346152 0.226977 11.00000 -1.20000 AFIX 0 C31 1 -0.020007 0.730849 0.311459 11.00000 0.03964 0.04332 = 0.03906 0.01523 0.01213 -0.00077 AFIX 137 H31A 2 -0.022390 0.779744 0.331819 11.00000 -1.50000 H31B 2 -0.055161 0.735589 0.274389 11.00000 -1.50000 H31C 2 0.034676 0.721987 0.309466 11.00000 -1.50000 AFIX 0 C62 1 0.611117 0.917637 0.533721 11.00000 0.05379 0.03584 = 0.03744 -0.00604 0.01117 -0.00930 AFIX 137 H62A 2 0.635204 0.885768 0.566196 11.00000 -1.50000 H62B 2 0.602074 0.971662 0.544915 11.00000 -1.50000 H62C 2 0.646900 0.919138 0.509755 11.00000 -1.50000 AFIX 0 C53 1 0.365889 1.086729 0.303795 11.00000 0.05446 0.02904 = 0.03644 -0.00356 0.01598 0.00082 AFIX 137 H53A 2 0.418408 1.077243 0.297872 11.00000 -1.50000 H53B 2 0.371941 1.115222 0.338338 11.00000 -1.50000 H53C 2 0.333809 1.118539 0.273600 11.00000 -1.50000 AFIX 0 C3 1 0.208310 0.737357 0.284592 11.00000 0.03677 0.04027 = 0.06522 -0.00942 0.02533 -0.01733 C18 1 0.214557 0.343786 0.316784 11.00000 0.03853 0.04541 = 0.02571 0.00016 0.00405 0.01136 AFIX 13 H18 2 0.170534 0.341966 0.335265 11.00000 -1.20000 AFIX 0 C1S 1 0.123980 0.912640 0.524469 11.00000 0.07179 0.03879 = 0.04569 -0.01203 0.01416 -0.00302 AFIX 23 H1SA 2 0.087364 0.958583 0.517968 11.00000 -1.20000 H1SB 2 0.112185 0.879659 0.490979 11.00000 -1.20000 AFIX 0 C21 1 -0.004945 0.508565 0.180888 11.00000 0.03571 0.06722 = 0.02844 0.00695 0.01103 0.01180 AFIX 13 H21 2 -0.033852 0.494756 0.208856 11.00000 -1.20000 AFIX 0 C65 1 0.548517 0.592895 0.337249 11.00000 0.04290 0.04107 = 0.05268 -0.01608 0.01976 -0.00727 AFIX 137 H65A 2 0.581453 0.551903 0.359748 11.00000 -1.50000 H65B 2 0.550956 0.587347 0.299250 11.00000 -1.50000 H65C 2 0.493350 0.586991 0.338985 11.00000 -1.50000 AFIX 0 C15 1 0.188685 0.408798 0.165793 11.00000 0.03798 0.04315 = 0.03551 -0.00463 0.02321 -0.00727 AFIX 43 H15 2 0.216370 0.402427 0.138485 11.00000 -1.20000 AFIX 0 C32 1 -0.135451 0.672683 0.346084 11.00000 0.03561 0.05484 = 0.03877 0.01690 0.00603 0.00047 AFIX 137 H32A 2 -0.153295 0.626135 0.362680 11.00000 -1.50000 H32B 2 -0.170839 0.681275 0.309465 11.00000 -1.50000 H32C 2 -0.136569 0.719369 0.368857 11.00000 -1.50000 AFIX 0 C23 1 -0.060639 0.486820 0.123095 11.00000 0.03836 0.08443 = 0.03655 -0.00006 0.00604 0.00894 AFIX 137 H23A 2 -0.035018 0.502464 0.094648 11.00000 -1.50000 H23B 2 -0.111345 0.514890 0.117499 11.00000 -1.50000 H23C 2 -0.070275 0.429549 0.121109 11.00000 -1.50000 AFIX 0 C48 1 0.462398 0.812778 0.200735 11.00000 0.03575 0.05065 = 0.03586 -0.00669 0.00494 0.01095 AFIX 13 H48 2 0.503343 0.815400 0.236765 11.00000 -1.20000 AFIX 0 C52 1 0.238624 1.022179 0.313544 11.00000 0.04150 0.05014 = 0.03808 -0.00137 0.01659 0.00509 AFIX 137 H52A 2 0.210730 1.059385 0.285259 11.00000 -1.50000 H52B 2 0.243449 1.045272 0.349745 11.00000 -1.50000 H52C 2 0.208576 0.972526 0.310157 11.00000 -1.50000 AFIX 0 C35 1 0.125122 0.435198 0.523287 11.00000 0.05724 0.03026 = 0.05341 0.01022 0.03152 0.00563 AFIX 137 H35A 2 0.141575 0.464553 0.557801 11.00000 -1.50000 H35B 2 0.148678 0.382095 0.528280 11.00000 -1.50000 H35C 2 0.067040 0.430751 0.512080 11.00000 -1.50000 AFIX 0 C4S 1 0.194449 0.850049 0.606013 11.00000 0.07380 0.05355 = 0.05232 -0.01123 -0.00188 0.00167 AFIX 23 H4SA 2 0.199316 0.793024 0.615513 11.00000 -1.20000 H4SB 2 0.203726 0.881132 0.640253 11.00000 -1.20000 AFIX 0 C3S 1 0.253945 0.872698 0.575094 11.00000 0.05371 0.05610 = 0.08956 -0.02495 0.00926 0.00070 AFIX 23 H3SA 2 0.264183 0.828093 0.552511 11.00000 -1.20000 H3SB 2 0.304838 0.889965 0.600282 11.00000 -1.20000 AFIX 0 C64 1 0.671302 0.683387 0.362247 11.00000 0.03168 0.06676 = 0.04104 -0.00482 0.01667 -0.00402 AFIX 137 H64A 2 0.691723 0.734069 0.379104 11.00000 -1.50000 H64B 2 0.678569 0.680708 0.325261 11.00000 -1.50000 H64C 2 0.700311 0.639785 0.384308 11.00000 -1.50000 AFIX 0 C34 1 0.245894 0.491365 0.496179 11.00000 0.03723 0.04645 = 0.08148 0.01678 0.01674 0.00867 AFIX 137 H34A 2 0.262193 0.522317 0.468284 11.00000 -1.50000 H34B 2 0.272047 0.439488 0.500112 11.00000 -1.50000 H34C 2 0.261240 0.519550 0.531202 11.00000 -1.50000 AFIX 0 C6S 1 0.844270 0.762285 0.561787 11.00000 0.05446 0.07884 = 0.04252 0.00364 0.01707 0.00377 AFIX 23 H6SA 2 0.852145 0.707165 0.575550 11.00000 -1.20000 H6SB 2 0.839913 0.797893 0.591900 11.00000 -1.20000 AFIX 0 C20 1 0.243033 0.258922 0.314852 11.00000 0.07487 0.03613 = 0.04053 0.00136 0.01029 0.00326 AFIX 137 H20A 2 0.200838 0.227415 0.290712 11.00000 -1.50000 H20B 2 0.256337 0.236269 0.351757 11.00000 -1.50000 H20C 2 0.290274 0.258399 0.300843 11.00000 -1.50000 AFIX 0 C5S 1 0.772102 0.769047 0.513088 11.00000 0.04252 0.05001 = 0.08184 -0.00261 0.01506 -0.00442 AFIX 23 H5SA 2 0.761999 0.718011 0.493180 11.00000 -1.20000 H5SB 2 0.724477 0.783128 0.525364 11.00000 -1.20000 AFIX 0 C22 1 0.012012 0.598658 0.185090 11.00000 0.07464 0.06459 = 0.03846 -0.00167 0.00226 0.03842 AFIX 137 H22A 2 0.048954 0.610646 0.220629 11.00000 -1.50000 H22B 2 -0.037847 0.627525 0.181535 11.00000 -1.50000 H22C 2 0.035672 0.614868 0.155768 11.00000 -1.50000 AFIX 0 C7S 1 0.911989 0.788679 0.536652 11.00000 0.03658 0.07079 = 0.05677 -0.01544 0.01215 -0.00946 AFIX 23 H7SA 2 0.956064 0.813645 0.564539 11.00000 -1.20000 H7SB 2 0.933036 0.743273 0.520069 11.00000 -1.20000 AFIX 0 C2S 1 0.212327 0.941383 0.539308 11.00000 0.06433 0.05242 = 0.07213 -0.01232 0.03338 -0.00724 AFIX 23 H2SA 2 0.231842 0.947722 0.506260 11.00000 -1.20000 H2SB 2 0.219186 0.991921 0.559874 11.00000 -1.20000 AFIX 0 C8S 1 0.871241 0.848074 0.493496 11.00000 0.06627 0.07006 = 0.06877 0.02724 0.01912 -0.00481 AFIX 43 H8S 2 0.896901 0.889724 0.479632 11.00000 -1.20000 AFIX 0 C19 1 0.280486 0.393419 0.353156 11.00000 0.08565 0.04040 = 0.07301 -0.00960 -0.04084 0.01305 AFIX 137 H19A 2 0.321842 0.403256 0.334266 11.00000 -1.50000 H19B 2 0.303522 0.364925 0.387368 11.00000 -1.50000 H19C 2 0.258581 0.444061 0.361272 11.00000 -1.50000 AFIX 0 C50 1 0.500568 0.847655 0.155721 11.00000 0.06279 0.11581 = 0.08051 0.00440 0.03961 0.03225 AFIX 137 H50A 2 0.462378 0.843410 0.119706 11.00000 -1.50000 H50B 2 0.548714 0.817731 0.155719 11.00000 -1.50000 H50C 2 0.514296 0.903464 0.163810 11.00000 -1.50000 AFIX 0 C49 1 0.439698 0.725876 0.188845 11.00000 0.06633 0.05362 = 0.15863 -0.02703 0.02651 0.01884 AFIX 137 H49A 2 0.422622 0.703337 0.219506 11.00000 -1.50000 H49B 2 0.485786 0.696405 0.184043 11.00000 -1.50000 H49C 2 0.396130 0.722155 0.155361 11.00000 -1.50000 AFIX 0 HKLF 4 REM JFig947_new_a.res in P2(1)/c REM R1 = 0.0612 for 9740 Fo > 4sig(Fo) and 0.0778 for all 12473 data REM 773 parameters refined using 0 restraints END WGHT 0.1104 15.4720 REM Highest difference peak 1.586, deepest hole -1.590, 1-sigma level 0.164 Q1 1 0.2980 0.6780 0.3368 11.00000 0.05 1.54 Q2 1 0.2632 0.6855 0.3371 11.00000 0.05 1.53 Q3 1 0.2466 0.7355 0.3802 11.00000 0.05 1.46 Q4 1 0.2886 0.7434 0.4237 11.00000 0.05 1.22 Q5 1 0.1867 0.7807 0.4026 11.00000 0.05 1.15 Q6 1 0.2112 0.7940 0.4124 11.00000 0.05 1.13 Q7 1 0.1708 0.7516 0.4090 11.00000 0.05 1.11 Q8 1 0.2764 0.7439 0.4473 11.00000 0.05 1.10 Q9 1 0.3690 0.6327 0.4216 11.00000 0.05 1.02 Q10 1 0.1905 0.7404 0.2505 11.00000 0.05 0.90 Q11 1 0.3585 0.9262 0.2558 11.00000 0.05 0.81 Q12 1 0.1505 0.7789 0.2369 11.00000 0.05 0.80 Q13 1 0.2466 0.6783 0.4376 11.00000 0.05 0.79 Q14 1 0.2355 0.6759 0.3995 11.00000 0.05 0.79 Q15 1 0.0564 0.4958 0.3485 11.00000 0.05 0.73 Q16 1 0.2967 0.9479 0.2318 11.00000 0.05 0.73 Q17 1 0.4758 0.8731 0.3195 11.00000 0.05 0.69 Q18 1 0.2091 0.4023 0.1882 11.00000 0.05 0.69 Q19 1 0.4799 0.8383 0.1782 11.00000 0.05 0.68 Q20 1 0.4370 0.8089 0.3445 11.00000 0.05 0.67 ; _shelx_res_checksum 26628 _shelx_shelxl_version_number 2014/7 _olex2_submission_original_sample_id JFig947 _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 Bi1 Bi 0.22912(2) 0.73579(2) 0.41692(2) 0.04102(13) Uani 1 1 d . Mn1 Mn 0.27737(5) 0.66572(6) 0.33331(4) 0.0260(2) Uani 1 1 d . Cl1 Cl 0.28339(14) 0.87565(13) 0.41373(9) 0.0522(5) Uani 1 1 d . Cl2 Cl 0.33571(13) 0.69424(13) 0.50249(8) 0.0506(5) Uani 1 1 d . N2 N 0.1356(3) 0.5512(3) 0.3288(2) 0.0232(11) Uani 1 1 d . O1S O 0.1147(3) 0.8672(3) 0.5700(2) 0.0431(12) Uani 1 1 d . O2 O 0.3195(3) 0.5762(4) 0.2413(2) 0.0466(13) Uani 1 1 d . O1 O 0.3891(3) 0.5607(3) 0.4182(2) 0.0416(12) Uani 1 1 d . N1 N 0.4097(3) 0.7933(3) 0.3410(2) 0.0242(11) Uani 1 1 d . O3 O 0.1731(4) 0.7741(4) 0.2580(3) 0.0541(16) Uani 1 1 d . C42 C 0.3904(4) 0.9079(4) 0.2525(3) 0.0258(13) Uani 1 1 d . C54 C 0.5508(4) 0.7752(4) 0.4303(3) 0.0249(13) Uani 1 1 d . C6 C 0.0755(3) 0.4942(4) 0.3295(3) 0.0232(13) Uani 1 1 d . C7 C 0.0334(4) 0.5016(4) 0.3711(3) 0.0242(13) Uani 1 1 d . C5 C 0.1891(4) 0.5946(4) 0.3305(2) 0.0242(13) Uani 1 1 d . C43 C 0.3228(4) 0.9554(4) 0.2559(3) 0.0279(14) Uani 1 1 d . C11 C 0.0604(4) 0.4318(4) 0.2910(3) 0.0239(13) Uani 1 1 d . C41 C 0.4641(4) 0.9059(4) 0.3012(3) 0.0257(13) Uani 1 1 d . C24 C 0.0525(4) 0.5716(4) 0.4122(3) 0.0252(13) Uani 1 1 d . C29 C 0.0112(4) 0.6445(4) 0.3986(3) 0.0268(13) Uani 1 1 d . C12 C 0.1052(4) 0.4249(4) 0.2477(3) 0.0262(13) Uani 1 1 d . C59 C 0.5436(4) 0.7935(4) 0.4838(3) 0.0293(14) Uani 1 1 d . C37 C 0.5439(4) 0.8412(4) 0.3878(3) 0.0250(13) Uani 1 1 d . C55 C 0.5658(4) 0.6954(4) 0.4156(3) 0.0291(14) Uani 1 1 d . C1 C 0.3611(4) 0.7449(4) 0.3394(3) 0.0276(14) Uani 1 1 d . C56 C 0.5708(4) 0.6345(4) 0.4557(3) 0.0320(15) Uani 1 1 d . H56 H 0.5790 0.5812 0.4466 0.038 Uiso 1 1 calc R C60 C 0.5295(4) 0.8796(4) 0.5021(3) 0.0337(15) Uani 1 1 d . H60 H 0.5072 0.9118 0.4684 0.040 Uiso 1 1 calc R C36 C 0.4731(4) 0.8480(4) 0.3440(3) 0.0245(13) Uani 1 1 d . C10 C -0.0001(4) 0.3764(4) 0.2943(3) 0.0305(14) Uani 1 1 d . H10 H -0.0133 0.3349 0.2682 0.037 Uiso 1 1 calc R C25 C 0.1093(4) 0.5594(4) 0.4639(2) 0.0235(13) Uani 1 1 d . C39 C 0.6004(4) 0.9507(4) 0.3469(3) 0.0327(15) Uani 1 1 d . H39 H 0.6431 0.9862 0.3483 0.039 Uiso 1 1 calc R C47 C 0.3906(4) 0.8645(4) 0.2048(3) 0.0313(14) Uani 1 1 d . O2S O 0.7894(4) 0.8316(4) 0.4773(3) 0.0703(19) Uani 1 1 d . C28 C 0.0253(4) 0.7055(4) 0.4387(3) 0.0325(15) Uani 1 1 d . H28 H -0.0024 0.7542 0.4306 0.039 Uiso 1 1 calc R C30 C -0.0477(4) 0.6586(4) 0.3416(3) 0.0301(14) Uani 1 1 d . H30 H -0.0478 0.6100 0.3190 0.036 Uiso 1 1 calc R C46 C 0.3218(4) 0.8686(5) 0.1589(3) 0.0371(16) Uani 1 1 d . H46 H 0.3215 0.8404 0.1265 0.045 Uiso 1 1 calc R C58 C 0.5503(4) 0.7296(4) 0.5224(3) 0.0336(15) Uani 1 1 d . H58 H 0.5456 0.7403 0.5582 0.040 Uiso 1 1 calc R C38 C 0.6078(4) 0.8929(4) 0.3880(3) 0.0270(13) Uani 1 1 d . H38 H 0.6559 0.8887 0.4161 0.032 Uiso 1 1 calc R C13 C 0.0736(4) 0.4600(4) 0.1943(3) 0.0322(15) Uani 1 1 d . C63 C 0.5800(4) 0.6763(4) 0.3591(3) 0.0303(14) Uani 1 1 d . H63 H 0.5509 0.7167 0.3324 0.036 Uiso 1 1 calc R C27 C 0.0799(4) 0.6947(4) 0.4901(3) 0.0326(15) Uani 1 1 d . H27 H 0.0886 0.7359 0.5165 0.039 Uiso 1 1 calc R C33 C 0.1537(4) 0.4798(4) 0.4785(3) 0.0288(14) Uani 1 1 d . H33 H 0.1405 0.4461 0.4449 0.035 Uiso 1 1 calc R C44 C 0.2558(4) 0.9567(4) 0.2092(3) 0.0348(16) Uani 1 1 d . H44 H 0.2105 0.9873 0.2103 0.042 Uiso 1 1 calc R C17 C 0.1793(4) 0.3823(4) 0.2599(3) 0.0279(14) Uani 1 1 d . C9 C -0.0405(4) 0.3818(4) 0.3353(3) 0.0335(15) Uani 1 1 d . H9 H -0.0794 0.3434 0.3373 0.040 Uiso 1 1 calc R C4 C 0.3038(4) 0.6109(4) 0.2762(3) 0.0322(15) Uani 1 1 d . C26 C 0.1216(4) 0.6225(4) 0.5025(3) 0.0296(14) Uani 1 1 d . H26 H 0.1586 0.6159 0.5372 0.036 Uiso 1 1 calc R C8 C -0.0232(4) 0.4449(4) 0.3739(3) 0.0284(14) Uani 1 1 d . H8 H -0.0503 0.4483 0.4017 0.034 Uiso 1 1 calc R C45 C 0.2553(4) 0.9131(5) 0.1610(3) 0.0400(17) Uani 1 1 d . H45 H 0.2100 0.9143 0.1304 0.048 Uiso 1 1 calc R C40 C 0.5302(4) 0.9566(4) 0.3034(3) 0.0288(14) Uani 1 1 d . H40 H 0.5273 0.9948 0.2754 0.035 Uiso 1 1 calc R C57 C 0.5637(4) 0.6522(4) 0.5079(3) 0.0356(16) Uani 1 1 d . H57 H 0.5681 0.6109 0.5339 0.043 Uiso 1 1 calc R C51 C 0.3234(4) 1.0052(4) 0.3063(3) 0.0328(15) Uani 1 1 d . H51 H 0.3544 0.9758 0.3394 0.039 Uiso 1 1 calc R C14 C 0.1179(4) 0.4513(5) 0.1544(3) 0.0368(16) Uani 1 1 d . H14 H 0.0985 0.4751 0.1195 0.044 Uiso 1 1 calc R C61 C 0.4704(5) 0.8840(5) 0.5380(3) 0.0433(18) Uani 1 1 d . H61A H 0.4206 0.8577 0.5191 0.065 Uiso 1 1 calc GR H61B H 0.4597 0.9397 0.5445 0.065 Uiso 1 1 calc GR H61C H 0.4935 0.8576 0.5730 0.065 Uiso 1 1 calc GR C2 C 0.3465(4) 0.6024(4) 0.3876(3) 0.0335(15) Uani 1 1 d . C16 C 0.2198(4) 0.3745(4) 0.2192(3) 0.0342(15) Uani 1 1 d . H16 H 0.2686 0.3462 0.2270 0.041 Uiso 1 1 calc R C31 C -0.0200(5) 0.7308(5) 0.3115(3) 0.0403(17) Uani 1 1 d . H31A H -0.0224 0.7797 0.3318 0.061 Uiso 1 1 calc GR H31B H -0.0552 0.7356 0.2744 0.061 Uiso 1 1 calc GR H31C H 0.0347 0.7220 0.3095 0.061 Uiso 1 1 calc GR C62 C 0.6111(5) 0.9176(5) 0.5337(3) 0.0425(18) Uani 1 1 d . H62A H 0.6352 0.8858 0.5662 0.064 Uiso 1 1 calc GR H62B H 0.6021 0.9717 0.5449 0.064 Uiso 1 1 calc GR H62C H 0.6469 0.9191 0.5098 0.064 Uiso 1 1 calc GR C53 C 0.3659(5) 1.0867(4) 0.3038(3) 0.0392(17) Uani 1 1 d . H53A H 0.4184 1.0772 0.2979 0.059 Uiso 1 1 calc GR H53B H 0.3719 1.1152 0.3383 0.059 Uiso 1 1 calc GR H53C H 0.3338 1.1185 0.2736 0.059 Uiso 1 1 calc GR C3 C 0.2083(5) 0.7374(5) 0.2846(4) 0.045(2) Uani 1 1 d . C18 C 0.2146(4) 0.3438(5) 0.3168(3) 0.0374(16) Uani 1 1 d . H18 H 0.1705 0.3420 0.3353 0.045 Uiso 1 1 calc R C1S C 0.1240(6) 0.9126(5) 0.5245(4) 0.052(2) Uani 1 1 d . H1SA H 0.0874 0.9586 0.5180 0.063 Uiso 1 1 calc R H1SB H 0.1122 0.8797 0.4910 0.063 Uiso 1 1 calc R C21 C -0.0049(4) 0.5086(5) 0.1809(3) 0.0433(19) Uani 1 1 d . H21 H -0.0339 0.4948 0.2089 0.052 Uiso 1 1 calc R C65 C 0.5485(5) 0.5929(5) 0.3372(3) 0.0442(18) Uani 1 1 d . H65A H 0.5815 0.5519 0.3597 0.066 Uiso 1 1 calc GR H65B H 0.5510 0.5873 0.2993 0.066 Uiso 1 1 calc GR H65C H 0.4934 0.5870 0.3390 0.066 Uiso 1 1 calc GR C15 C 0.1887(4) 0.4088(5) 0.1658(3) 0.0363(16) Uani 1 1 d . H15 H 0.2164 0.4024 0.1385 0.044 Uiso 1 1 calc R C32 C -0.1355(4) 0.6727(5) 0.3461(3) 0.0438(19) Uani 1 1 d . H32A H -0.1533 0.6261 0.3627 0.066 Uiso 1 1 calc GR H32B H -0.1708 0.6813 0.3095 0.066 Uiso 1 1 calc GR H32C H -0.1366 0.7194 0.3689 0.066 Uiso 1 1 calc GR C23 C -0.0606(5) 0.4868(6) 0.1231(3) 0.054(2) Uani 1 1 d . H23A H -0.0350 0.5025 0.0946 0.081 Uiso 1 1 calc GR H23B H -0.1113 0.5149 0.1175 0.081 Uiso 1 1 calc GR H23C H -0.0703 0.4295 0.1211 0.081 Uiso 1 1 calc GR C48 C 0.4624(4) 0.8128(5) 0.2007(3) 0.0416(18) Uani 1 1 d . H48 H 0.5033 0.8154 0.2368 0.050 Uiso 1 1 calc R C52 C 0.2386(5) 1.0222(5) 0.3135(3) 0.0421(18) Uani 1 1 d . H52A H 0.2107 1.0594 0.2853 0.063 Uiso 1 1 calc GR H52B H 0.2434 1.0453 0.3497 0.063 Uiso 1 1 calc GR H52C H 0.2086 0.9725 0.3102 0.063 Uiso 1 1 calc GR C35 C 0.1251(5) 0.4352(5) 0.5233(3) 0.0438(18) Uani 1 1 d . H35A H 0.1416 0.4646 0.5578 0.066 Uiso 1 1 calc GR H35B H 0.1487 0.3821 0.5283 0.066 Uiso 1 1 calc GR H35C H 0.0670 0.4308 0.5121 0.066 Uiso 1 1 calc GR C4S C 0.1944(6) 0.8500(6) 0.6060(4) 0.063(3) Uani 1 1 d . H4SA H 0.1993 0.7930 0.6155 0.076 Uiso 1 1 calc R H4SB H 0.2037 0.8811 0.6403 0.076 Uiso 1 1 calc R C3S C 0.2539(6) 0.8727(6) 0.5751(5) 0.068(3) Uani 1 1 d . H3SA H 0.2642 0.8281 0.5525 0.082 Uiso 1 1 calc R H3SB H 0.3048 0.8900 0.6003 0.082 Uiso 1 1 calc R C64 C 0.6713(4) 0.6834(6) 0.3622(3) 0.0452(19) Uani 1 1 d . H64A H 0.6917 0.7341 0.3791 0.068 Uiso 1 1 calc GR H64B H 0.6786 0.6807 0.3253 0.068 Uiso 1 1 calc GR H64C H 0.7003 0.6398 0.3843 0.068 Uiso 1 1 calc GR C34 C 0.2459(5) 0.4914(5) 0.4962(4) 0.055(2) Uani 1 1 d . H34A H 0.2622 0.5223 0.4683 0.082 Uiso 1 1 calc GR H34B H 0.2720 0.4395 0.5001 0.082 Uiso 1 1 calc GR H34C H 0.2612 0.5196 0.5312 0.082 Uiso 1 1 calc GR C6S C 0.8443(6) 0.7623(6) 0.5618(4) 0.058(2) Uani 1 1 d . H6SA H 0.8521 0.7072 0.5755 0.069 Uiso 1 1 calc R H6SB H 0.8399 0.7979 0.5919 0.069 Uiso 1 1 calc R C20 C 0.2430(6) 0.2589(5) 0.3149(4) 0.051(2) Uani 1 1 d . H20A H 0.2008 0.2274 0.2907 0.077 Uiso 1 1 calc GR H20B H 0.2563 0.2363 0.3518 0.077 Uiso 1 1 calc GR H20C H 0.2903 0.2584 0.3008 0.077 Uiso 1 1 calc GR C5S C 0.7721(5) 0.7690(6) 0.5131(5) 0.058(2) Uani 1 1 d . H5SA H 0.7620 0.7180 0.4932 0.070 Uiso 1 1 calc R H5SB H 0.7245 0.7831 0.5254 0.070 Uiso 1 1 calc R C22 C 0.0120(6) 0.5987(6) 0.1851(4) 0.062(3) Uani 1 1 d . H22A H 0.0490 0.6106 0.2206 0.092 Uiso 1 1 calc GR H22B H -0.0378 0.6275 0.1815 0.092 Uiso 1 1 calc GR H22C H 0.0357 0.6149 0.1558 0.092 Uiso 1 1 calc GR C7S C 0.9120(5) 0.7887(6) 0.5367(4) 0.055(2) Uani 1 1 d . H7SA H 0.9561 0.8136 0.5645 0.066 Uiso 1 1 calc R H7SB H 0.9330 0.7433 0.5201 0.066 Uiso 1 1 calc R C2S C 0.2123(6) 0.9414(6) 0.5393(4) 0.060(2) Uani 1 1 d . H2SA H 0.2318 0.9477 0.5063 0.072 Uiso 1 1 calc R H2SB H 0.2192 0.9919 0.5599 0.072 Uiso 1 1 calc R C8S C 0.8712(6) 0.8481(7) 0.4935(4) 0.068(3) Uani 1 1 d . H8S H 0.8969 0.8897 0.4796 0.082 Uiso 1 1 calc R C19 C 0.2805(7) 0.3934(6) 0.3532(4) 0.078(4) Uani 1 1 d . H19A H 0.3218 0.4033 0.3343 0.117 Uiso 1 1 calc GR H19B H 0.3035 0.3649 0.3874 0.117 Uiso 1 1 calc GR H19C H 0.2586 0.4441 0.3613 0.117 Uiso 1 1 calc GR C50 C 0.5006(6) 0.8477(8) 0.1557(5) 0.082(4) Uani 1 1 d . H50A H 0.4624 0.8434 0.1197 0.124 Uiso 1 1 calc GR H50B H 0.5487 0.8177 0.1557 0.124 Uiso 1 1 calc GR H50C H 0.5143 0.9035 0.1638 0.124 Uiso 1 1 calc GR C49 C 0.4397(7) 0.7259(6) 0.1888(7) 0.093(4) Uani 1 1 d . H49A H 0.4226 0.7033 0.2195 0.140 Uiso 1 1 calc GR H49B H 0.4858 0.6964 0.1840 0.140 Uiso 1 1 calc GR H49C H 0.3961 0.7222 0.1554 0.140 Uiso 1 1 calc GR loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi1 0.03812(18) 0.0441(2) 0.0421(2) -0.00207(13) 0.01272(13) -0.00281(12) Mn1 0.0249(5) 0.0270(5) 0.0261(5) 0.0001(4) 0.0067(4) -0.0056(4) Cl1 0.0676(13) 0.0418(11) 0.0503(12) 0.0003(9) 0.0208(10) 0.0003(9) Cl2 0.0588(12) 0.0492(12) 0.0412(10) -0.0004(9) 0.0086(9) -0.0039(9) N2 0.025(3) 0.024(3) 0.019(2) 0.000(2) 0.005(2) 0.001(2) O1S 0.048(3) 0.044(3) 0.036(3) -0.005(2) 0.008(2) -0.003(2) O2 0.045(3) 0.055(3) 0.043(3) -0.010(3) 0.017(3) -0.009(3) O1 0.035(3) 0.048(3) 0.040(3) 0.005(3) 0.005(2) -0.004(2) N1 0.022(2) 0.025(3) 0.026(3) -0.001(2) 0.007(2) -0.001(2) O3 0.036(3) 0.076(5) 0.045(3) 0.016(3) 0.002(3) -0.015(3) C42 0.024(3) 0.025(3) 0.026(3) 0.005(3) 0.004(2) 0.000(2) C54 0.020(3) 0.024(3) 0.029(3) 0.002(3) 0.004(2) 0.000(2) C6 0.022(3) 0.022(3) 0.025(3) 0.004(2) 0.004(2) -0.001(2) C7 0.028(3) 0.022(3) 0.022(3) 0.003(2) 0.006(2) 0.003(2) C5 0.031(3) 0.022(3) 0.020(3) 0.003(2) 0.007(2) 0.006(3) C43 0.028(3) 0.030(3) 0.026(3) 0.001(3) 0.006(3) -0.001(3) C11 0.024(3) 0.023(3) 0.023(3) 0.003(3) 0.004(2) 0.002(2) C41 0.028(3) 0.025(3) 0.023(3) -0.001(3) 0.005(3) -0.001(2) C24 0.027(3) 0.025(3) 0.026(3) -0.003(3) 0.011(3) -0.006(2) C29 0.026(3) 0.025(3) 0.029(3) 0.002(3) 0.008(3) -0.003(2) C12 0.028(3) 0.022(3) 0.029(3) -0.004(3) 0.009(3) -0.007(2) C59 0.026(3) 0.030(3) 0.030(3) 0.003(3) 0.005(3) 0.000(3) C37 0.024(3) 0.026(3) 0.025(3) -0.001(3) 0.009(2) 0.000(2) C55 0.019(3) 0.032(4) 0.034(4) 0.002(3) 0.003(3) 0.001(3) C1 0.030(3) 0.030(4) 0.023(3) 0.001(3) 0.008(3) 0.003(3) C56 0.027(3) 0.027(3) 0.038(4) 0.006(3) 0.001(3) 0.002(3) C60 0.039(4) 0.031(4) 0.034(4) 0.005(3) 0.014(3) 0.000(3) C36 0.028(3) 0.018(3) 0.030(3) 0.000(3) 0.013(3) -0.001(2) C10 0.033(3) 0.026(3) 0.034(4) -0.009(3) 0.011(3) -0.007(3) C25 0.025(3) 0.028(3) 0.019(3) 0.001(3) 0.009(2) -0.003(2) C39 0.030(3) 0.034(4) 0.035(4) -0.004(3) 0.008(3) -0.008(3) C47 0.032(3) 0.033(4) 0.027(3) 0.001(3) 0.006(3) 0.001(3) O2S 0.058(4) 0.077(5) 0.066(4) 0.019(4) -0.002(3) -0.004(3) C28 0.032(3) 0.028(3) 0.039(4) -0.004(3) 0.013(3) 0.002(3) C30 0.030(3) 0.028(3) 0.031(3) 0.001(3) 0.006(3) 0.002(3) C46 0.040(4) 0.046(4) 0.024(3) -0.008(3) 0.006(3) -0.004(3) C58 0.032(3) 0.039(4) 0.029(4) 0.006(3) 0.008(3) -0.002(3) C38 0.029(3) 0.029(3) 0.022(3) 0.001(3) 0.005(2) -0.006(3) C13 0.031(3) 0.034(4) 0.032(4) 0.006(3) 0.010(3) 0.001(3) C63 0.030(3) 0.027(3) 0.034(4) 0.001(3) 0.009(3) 0.001(3) C27 0.041(4) 0.030(4) 0.031(4) -0.008(3) 0.017(3) -0.007(3) C33 0.031(3) 0.028(3) 0.026(3) 0.002(3) 0.004(3) 0.002(3) C44 0.030(3) 0.040(4) 0.034(4) 0.005(3) 0.005(3) 0.008(3) C17 0.033(3) 0.020(3) 0.030(3) -0.006(3) 0.007(3) -0.001(2) C9 0.032(3) 0.033(4) 0.038(4) -0.003(3) 0.014(3) -0.013(3) C4 0.032(3) 0.032(4) 0.033(4) 0.004(3) 0.010(3) -0.007(3) C26 0.034(3) 0.036(4) 0.020(3) 0.001(3) 0.010(3) -0.004(3) C8 0.032(3) 0.029(3) 0.027(3) 0.001(3) 0.012(3) -0.001(3) C45 0.035(4) 0.053(5) 0.028(4) -0.001(3) 0.000(3) 0.005(3) C40 0.029(3) 0.028(3) 0.029(3) 0.004(3) 0.009(3) -0.003(3) C57 0.029(3) 0.037(4) 0.036(4) 0.010(3) 0.000(3) -0.005(3) C51 0.035(4) 0.036(4) 0.030(3) 0.002(3) 0.012(3) 0.002(3) C14 0.046(4) 0.041(4) 0.028(3) 0.005(3) 0.017(3) 0.004(3) C61 0.050(4) 0.038(4) 0.045(4) -0.001(3) 0.017(4) 0.003(3) C2 0.022(3) 0.038(4) 0.041(4) 0.002(3) 0.011(3) -0.007(3) C16 0.031(3) 0.030(4) 0.042(4) -0.002(3) 0.012(3) 0.003(3) C31 0.040(4) 0.043(4) 0.039(4) 0.015(3) 0.012(3) -0.001(3) C62 0.054(5) 0.036(4) 0.037(4) -0.006(3) 0.011(3) -0.009(3) C53 0.054(4) 0.029(4) 0.036(4) -0.004(3) 0.016(3) 0.001(3) C3 0.037(4) 0.040(5) 0.065(6) -0.009(4) 0.025(4) -0.017(4) C18 0.039(4) 0.045(4) 0.026(3) 0.000(3) 0.004(3) 0.011(3) C1S 0.072(6) 0.039(5) 0.046(5) -0.012(4) 0.014(4) -0.003(4) C21 0.036(4) 0.067(6) 0.028(4) 0.007(4) 0.011(3) 0.012(4) C65 0.043(4) 0.041(4) 0.053(5) -0.016(4) 0.020(4) -0.007(3) C15 0.038(4) 0.043(4) 0.036(4) -0.005(3) 0.023(3) -0.007(3) C32 0.036(4) 0.055(5) 0.039(4) 0.017(4) 0.006(3) 0.000(3) C23 0.038(4) 0.084(7) 0.037(4) 0.000(4) 0.006(3) 0.009(4) C48 0.036(4) 0.051(5) 0.036(4) -0.007(3) 0.005(3) 0.011(3) C52 0.041(4) 0.050(5) 0.038(4) -0.001(4) 0.017(3) 0.005(3) C35 0.057(5) 0.030(4) 0.053(5) 0.010(4) 0.032(4) 0.006(3) C4S 0.074(6) 0.054(6) 0.052(5) -0.011(4) -0.002(5) 0.002(5) C3S 0.054(5) 0.056(6) 0.090(8) -0.025(5) 0.009(5) 0.001(4) C64 0.032(4) 0.067(6) 0.041(4) -0.005(4) 0.017(3) -0.004(3) C34 0.037(4) 0.046(5) 0.081(6) 0.017(5) 0.017(4) 0.009(4) C6S 0.054(5) 0.079(7) 0.043(5) 0.004(4) 0.017(4) 0.004(4) C20 0.075(6) 0.036(4) 0.041(5) 0.001(3) 0.010(4) 0.003(4) C5S 0.043(5) 0.050(5) 0.082(7) -0.003(5) 0.015(5) -0.004(4) C22 0.075(6) 0.065(6) 0.038(5) -0.002(4) 0.002(4) 0.038(5) C7S 0.037(4) 0.071(6) 0.057(5) -0.015(5) 0.012(4) -0.009(4) C2S 0.064(6) 0.052(5) 0.072(6) -0.012(5) 0.033(5) -0.007(4) C8S 0.066(6) 0.070(7) 0.069(6) 0.027(5) 0.019(5) -0.005(5) C19 0.086(7) 0.040(5) 0.073(7) -0.010(5) -0.041(6) 0.013(5) C50 0.063(6) 0.116(10) 0.081(7) 0.004(7) 0.040(6) 0.032(6) C49 0.066(7) 0.054(7) 0.159(13) -0.027(7) 0.027(8) 0.019(5) 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' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle Cl1 Bi1 Mn1 100.46(5) Cl1 Bi1 Cl2 95.06(7) Cl2 Bi1 Mn1 103.56(6) C5 Mn1 Bi1 83.81(18) C5 Mn1 C1 174.5(3) C1 Mn1 Bi1 91.1(2) C4 Mn1 Bi1 175.0(2) C4 Mn1 C5 91.2(3) C4 Mn1 C1 93.9(3) C4 Mn1 C2 92.5(3) C4 Mn1 C3 93.1(3) C2 Mn1 Bi1 87.0(2) C2 Mn1 C5 91.4(3) C2 Mn1 C1 90.5(3) C2 Mn1 C3 174.0(4) C3 Mn1 Bi1 87.5(3) C3 Mn1 C5 90.5(3) C3 Mn1 C1 87.1(3) C5 N2 C6 175.3(6) C1S O1S C4S 108.3(7) C1 N1 C36 176.0(6) C43 C42 C41 119.1(6) C47 C42 C43 121.7(6) C47 C42 C41 119.2(6) C59 C54 C37 120.0(6) C59 C54 C55 121.0(6) C55 C54 C37 118.9(6) N2 C6 C7 118.0(5) C11 C6 N2 119.8(6) C11 C6 C7 122.2(6) C6 C7 C24 119.8(5) C8 C7 C6 119.0(6) C8 C7 C24 121.3(6) N2 C5 Mn1 179.7(7) C42 C43 C51 122.0(6) C44 C43 C42 117.4(6) C44 C43 C51 120.6(6) C6 C11 C12 121.5(6) C6 C11 C10 116.9(6) C10 C11 C12 121.6(6) C36 C41 C42 121.6(6) C40 C41 C42 121.1(6) C40 C41 C36 116.9(6) C29 C24 C7 119.4(5) C29 C24 C25 122.0(6) C25 C24 C7 118.6(5) C24 C29 C30 121.8(6) C28 C29 C24 118.2(6) C28 C29 C30 120.0(6) C13 C12 C11 120.5(6) C17 C12 C11 119.3(6) C17 C12 C13 120.2(6) C54 C59 C60 122.8(6) C54 C59 C58 118.1(6) C58 C59 C60 119.1(6) C36 C37 C54 119.8(5) C38 C37 C54 122.1(5) C38 C37 C36 118.0(6) C54 C55 C63 121.2(6) C56 C55 C54 117.9(6) C56 C55 C63 120.8(6) N1 C1 Mn1 177.3(6) C55 C56 H56 119.5 C57 C56 C55 121.1(7) C57 C56 H56 119.5 C59 C60 H60 108.0 C59 C60 C62 109.7(6) C61 C60 C59 113.6(6) C61 C60 H60 108.0 C61 C60 C62 109.5(6) C62 C60 H60 108.0 N1 C36 C41 118.2(5) N1 C36 C37 119.0(5) C37 C36 C41 122.7(6) C11 C10 H10 119.2 C9 C10 C11 121.6(6) C9 C10 H10 119.2 C24 C25 C33 121.7(6) C26 C25 C24 117.6(6) C26 C25 C33 120.6(5) C38 C39 H39 119.5 C38 C39 C40 121.1(6) C40 C39 H39 119.5 C42 C47 C46 118.5(6) C42 C47 C48 122.2(6) C46 C47 C48 119.3(6) C8S O2S C5S 108.6(7) C29 C28 H28 119.5 C27 C28 C29 121.0(6) C27 C28 H28 119.5 C29 C30 H30 108.0 C29 C30 C31 110.9(6) C29 C30 C32 111.8(6) C31 C30 H30 108.0 C31 C30 C32 110.1(6) C32 C30 H30 108.0 C47 C46 H46 119.3 C45 C46 C47 121.4(7) C45 C46 H46 119.3 C59 C58 H58 119.6 C57 C58 C59 120.7(7) C57 C58 H58 119.6 C37 C38 H38 119.8 C39 C38 C37 120.5(6) C39 C38 H38 119.8 C12 C13 C21 121.0(6) C14 C13 C12 118.4(6) C14 C13 C21 120.6(6) C55 C63 H63 107.9 C55 C63 C65 112.9(6) C55 C63 C64 110.1(5) C65 C63 H63 107.9 C65 C63 C64 110.0(6) C64 C63 H63 107.9 C28 C27 H27 120.0 C28 C27 C26 120.0(6) C26 C27 H27 120.0 C25 C33 H33 107.6 C25 C33 C35 111.1(6) C25 C33 C34 111.8(6) C35 C33 H33 107.6 C35 C33 C34 110.9(6) C34 C33 H33 107.6 C43 C44 H44 119.3 C45 C44 C43 121.4(6) C45 C44 H44 119.3 C12 C17 C18 121.4(6) C16 C17 C12 119.1(6) C16 C17 C18 119.5(6) C10 C9 H9 120.0 C10 C9 C8 120.0(6) C8 C9 H9 120.0 O2 C4 Mn1 179.0(6) C25 C26 H26 119.4 C27 C26 C25 121.2(6) C27 C26 H26 119.4 C7 C8 C9 120.3(6) C7 C8 H8 119.8 C9 C8 H8 119.8 C46 C45 C44 119.7(6) C46 C45 H45 120.2 C44 C45 H45 120.2 C41 C40 H40 119.6 C39 C40 C41 120.7(6) C39 C40 H40 119.6 C56 C57 C58 121.1(7) C56 C57 H57 119.5 C58 C57 H57 119.5 C43 C51 H51 108.1 C43 C51 C53 110.2(6) C43 C51 C52 113.7(6) C53 C51 H51 108.1 C52 C51 H51 108.1 C52 C51 C53 108.4(6) C13 C14 H14 119.3 C15 C14 C13 121.4(7) C15 C14 H14 119.3 C60 C61 H61A 109.5 C60 C61 H61B 109.5 C60 C61 H61C 109.5 H61A C61 H61B 109.5 H61A C61 H61C 109.5 H61B C61 H61C 109.5 O1 C2 Mn1 175.8(7) C17 C16 H16 119.5 C17 C16 C15 121.1(6) C15 C16 H16 119.5 C30 C31 H31A 109.5 C30 C31 H31B 109.5 C30 C31 H31C 109.5 H31A C31 H31B 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 C60 C62 H62A 109.5 C60 C62 H62B 109.5 C60 C62 H62C 109.5 H62A C62 H62B 109.5 H62A C62 H62C 109.5 H62B C62 H62C 109.5 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 O3 C3 Mn1 177.9(9) C17 C18 H18 106.5 C20 C18 C17 114.6(6) C20 C18 H18 106.5 C19 C18 C17 112.5(7) C19 C18 H18 106.5 C19 C18 C20 109.7(7) O1S C1S H1SA 110.4 O1S C1S H1SB 110.4 O1S C1S C2S 106.7(7) H1SA C1S H1SB 108.6 C2S C1S H1SA 110.4 C2S C1S H1SB 110.4 C13 C21 H21 107.6 C13 C21 C23 111.8(7) C23 C21 H21 107.6 C22 C21 C13 111.2(7) C22 C21 H21 107.6 C22 C21 C23 110.7(7) 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 C14 C15 C16 119.7(6) C14 C15 H15 120.1 C16 C15 H15 120.1 C30 C32 H32A 109.5 C30 C32 H32B 109.5 C30 C32 H32C 109.5 H32A C32 H32B 109.5 H32A C32 H32C 109.5 H32B C32 H32C 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 C47 C48 H48 107.9 C47 C48 C50 109.9(7) C50 C48 H48 107.9 C49 C48 C47 112.4(7) C49 C48 H48 107.9 C49 C48 C50 110.6(9) 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 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 O1S C4S H4SA 110.3 O1S C4S H4SB 110.3 O1S C4S C3S 107.2(8) H4SA C4S H4SB 108.5 C3S C4S H4SA 110.3 C3S C4S H4SB 110.3 C4S C3S H3SA 111.3 C4S C3S H3SB 111.3 C4S C3S C2S 102.5(8) H3SA C3S H3SB 109.2 C2S C3S H3SA 111.3 C2S C3S H3SB 111.3 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 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 H6SA C6S H6SB 109.3 C5S C6S H6SA 111.4 C5S C6S H6SB 111.4 C5S C6S C7S 101.7(8) C7S C6S H6SA 111.4 C7S C6S H6SB 111.4 C18 C20 H20A 109.5 C18 C20 H20B 109.5 C18 C20 H20C 109.5 H20A C20 H20B 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 O2S C5S C6S 107.1(7) O2S C5S H5SA 110.3 O2S C5S H5SB 110.3 C6S C5S H5SA 110.3 C6S C5S H5SB 110.3 H5SA C5S H5SB 108.5 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 C6S C7S H7SA 111.2 C6S C7S H7SB 111.2 H7SA C7S H7SB 109.1 C8S C7S C6S 103.0(8) C8S C7S H7SA 111.2 C8S C7S H7SB 111.2 C1S C2S H2SA 111.6 C1S C2S H2SB 111.6 C3S C2S C1S 101.0(8) C3S C2S H2SA 111.6 C3S C2S H2SB 111.6 H2SA C2S H2SB 109.4 O2S C8S C7S 109.1(8) O2S C8S H8S 125.5 C7S C8S H8S 125.5 C18 C19 H19A 109.5 C18 C19 H19B 109.5 C18 C19 H19C 109.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C48 C50 H50A 109.5 C48 C50 H50B 109.5 C48 C50 H50C 109.5 H50A C50 H50B 109.5 H50A C50 H50C 109.5 H50B C50 H50C 109.5 C48 C49 H49A 109.5 C48 C49 H49B 109.5 C48 C49 H49C 109.5 H49A C49 H49B 109.5 H49A C49 H49C 109.5 H49B C49 H49C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Bi1 Mn1 2.6909(10) Bi1 Cl1 2.500(2) Bi1 Cl2 2.501(2) Mn1 C5 1.899(7) Mn1 C1 1.915(7) Mn1 C4 1.836(8) Mn1 C2 1.862(7) Mn1 C3 1.872(11) N2 C6 1.398(8) N2 C5 1.153(8) O1S C1S 1.402(10) O1S C4S 1.446(10) O2 C4 1.130(9) O1 C2 1.136(8) N1 C1 1.146(8) N1 C36 1.399(8) O3 C3 0.977(10) C42 C43 1.419(9) C42 C41 1.498(8) C42 C47 1.384(9) C54 C59 1.400(10) C54 C37 1.500(9) C54 C55 1.410(9) C6 C7 1.412(9) C6 C11 1.384(9) C7 C24 1.521(9) C7 C8 1.361(9) C43 C44 1.398(9) C43 C51 1.496(9) C11 C12 1.481(9) C11 C10 1.399(9) C41 C36 1.407(9) C41 C40 1.396(9) C24 C29 1.391(9) C24 C25 1.403(8) C29 C28 1.391(9) C29 C30 1.522(9) C12 C13 1.417(9) C12 C17 1.411(9) C59 C60 1.532(10) C59 C58 1.411(10) C37 C36 1.402(9) C37 C38 1.385(9) C55 C56 1.403(9) C55 C63 1.519(10) C56 H56 0.9300 C56 C57 1.364(10) C60 H60 0.9800 C60 C61 1.515(10) C60 C62 1.542(10) C10 H10 0.9300 C10 C9 1.378(10) C25 C33 1.515(9) C25 C26 1.394(9) C39 H39 0.9300 C39 C38 1.379(9) C39 C40 1.388(9) C47 C46 1.407(9) C47 C48 1.520(10) O2S C5S 1.445(12) O2S C8S 1.376(12) C28 H28 0.9300 C28 C27 1.380(10) C30 H30 0.9800 C30 C31 1.549(10) C30 C32 1.550(10) C46 H46 0.9300 C46 C45 1.365(10) C58 H58 0.9300 C58 C57 1.365(10) C38 H38 0.9300 C13 C14 1.403(10) C13 C21 1.524(10) C63 H63 0.9800 C63 C65 1.527(10) C63 C64 1.546(9) C27 H27 0.9300 C27 C26 1.382(10) C33 H33 0.9800 C33 C35 1.518(10) C33 C34 1.531(10) C44 H44 0.9300 C44 C45 1.396(10) C17 C16 1.374(10) C17 C18 1.521(9) C9 H9 0.9300 C9 C8 1.393(9) C26 H26 0.9300 C8 H8 0.9300 C45 H45 0.9300 C40 H40 0.9300 C57 H57 0.9300 C51 H51 0.9800 C51 C53 1.540(10) C51 C52 1.532(10) C14 H14 0.9300 C14 C15 1.363(10) C61 H61A 0.9600 C61 H61B 0.9600 C61 H61C 0.9600 C16 H16 0.9300 C16 C15 1.411(10) C31 H31A 0.9600 C31 H31B 0.9600 C31 H31C 0.9600 C62 H62A 0.9600 C62 H62B 0.9600 C62 H62C 0.9600 C53 H53A 0.9600 C53 H53B 0.9600 C53 H53C 0.9600 C18 H18 0.9800 C18 C20 1.490(11) C18 C19 1.490(11) C1S H1SA 0.9700 C1S H1SB 0.9700 C1S C2S 1.532(13) C21 H21 0.9800 C21 C23 1.540(10) C21 C22 1.516(13) C65 H65A 0.9600 C65 H65B 0.9600 C65 H65C 0.9600 C15 H15 0.9300 C32 H32A 0.9600 C32 H32B 0.9600 C32 H32C 0.9600 C23 H23A 0.9600 C23 H23B 0.9600 C23 H23C 0.9600 C48 H48 0.9800 C48 C50 1.547(14) C48 C49 1.497(14) C52 H52A 0.9600 C52 H52B 0.9600 C52 H52C 0.9600 C35 H35A 0.9600 C35 H35B 0.9600 C35 H35C 0.9600 C4S H4SA 0.9700 C4S H4SB 0.9700 C4S C3S 1.476(15) C3S H3SA 0.9700 C3S H3SB 0.9700 C3S C2S 1.500(14) C64 H64A 0.9600 C64 H64B 0.9600 C64 H64C 0.9600 C34 H34A 0.9600 C34 H34B 0.9600 C34 H34C 0.9600 C6S H6SA 0.9700 C6S H6SB 0.9700 C6S C5S 1.485(13) C6S C7S 1.517(13) C20 H20A 0.9600 C20 H20B 0.9600 C20 H20C 0.9600 C5S H5SA 0.9700 C5S H5SB 0.9700 C22 H22A 0.9600 C22 H22B 0.9600 C22 H22C 0.9600 C7S H7SA 0.9700 C7S H7SB 0.9700 C7S C8S 1.484(13) C2S H2SA 0.9700 C2S H2SB 0.9700 C8S H8S 0.9300 C19 H19A 0.9600 C19 H19B 0.9600 C19 H19C 0.9600 C50 H50A 0.9600 C50 H50B 0.9600 C50 H50C 0.9600 C49 H49A 0.9600 C49 H49B 0.9600 C49 H49C 0.9600 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 N2 C6 C7 C24 1.8(8) N2 C6 C7 C8 -177.5(5) N2 C6 C11 C12 -1.6(9) N2 C6 C11 C10 179.5(5) O1S C1S C2S C3S 31.5(9) O1S C4S C3S C2S 31.0(9) C42 C43 C44 C45 -0.1(10) C42 C43 C51 C53 82.7(8) C42 C43 C51 C52 -155.4(6) C42 C41 C36 N1 -2.3(9) C42 C41 C36 C37 175.2(6) C42 C41 C40 C39 -175.6(6) C42 C47 C46 C45 -1.0(11) C42 C47 C48 C50 -115.3(8) C42 C47 C48 C49 121.0(9) C54 C59 C60 C61 140.2(7) C54 C59 C60 C62 -96.8(7) C54 C59 C58 C57 0.2(10) C54 C37 C36 N1 0.6(9) C54 C37 C36 C41 -176.9(6) C54 C37 C38 C39 177.2(6) C54 C55 C56 C57 -1.9(9) C54 C55 C63 C65 -147.5(6) C54 C55 C63 C64 89.1(7) C6 C7 C24 C29 88.3(7) C6 C7 C24 C25 -94.2(7) C6 C7 C8 C9 -1.7(9) C6 C11 C12 C13 -92.5(7) C6 C11 C12 C17 88.1(8) C6 C11 C10 C9 -2.5(10) C7 C6 C11 C12 -180.0(6) C7 C6 C11 C10 1.1(9) C7 C24 C29 C28 175.2(6) C7 C24 C29 C30 -5.2(9) C7 C24 C25 C33 2.2(9) C7 C24 C25 C26 -175.6(6) C43 C42 C41 C36 90.4(8) C43 C42 C41 C40 -95.9(8) C43 C42 C47 C46 0.3(10) C43 C42 C47 C48 -179.5(7) C43 C44 C45 C46 -0.5(12) C11 C6 C7 C24 -179.9(5) C11 C6 C7 C8 0.9(9) C11 C12 C13 C14 -179.5(6) C11 C12 C13 C21 2.7(10) C11 C12 C17 C16 178.6(6) C11 C12 C17 C18 -0.5(9) C11 C10 C9 C8 1.8(11) C41 C42 C43 C44 179.0(6) C41 C42 C43 C51 1.3(9) C41 C42 C47 C46 -178.4(6) C41 C42 C47 C48 1.8(10) C24 C7 C8 C9 179.1(6) C24 C29 C28 C27 1.2(10) C24 C29 C30 C31 -120.0(7) C24 C29 C30 C32 116.7(7) C24 C25 C33 C35 -109.9(7) C24 C25 C33 C34 125.5(7) C24 C25 C26 C27 -0.6(9) C29 C24 C25 C33 179.7(6) C29 C24 C25 C26 2.0(9) C29 C28 C27 C26 0.1(10) C12 C11 C10 C9 178.6(6) C12 C13 C14 C15 1.5(11) C12 C13 C21 C23 -136.1(7) C12 C13 C21 C22 99.6(8) C12 C17 C16 C15 0.4(10) C12 C17 C18 C20 133.0(7) C12 C17 C18 C19 -100.8(9) C59 C54 C37 C36 -105.2(7) C59 C54 C37 C38 79.4(8) C59 C54 C55 C56 1.9(9) C59 C54 C55 C63 -175.3(6) C59 C58 C57 C56 -0.2(10) C37 C54 C59 C60 -0.6(9) C37 C54 C59 C58 179.8(6) C37 C54 C55 C56 -179.0(5) C37 C54 C55 C63 3.7(8) C55 C54 C59 C60 178.5(6) C55 C54 C59 C58 -1.1(9) C55 C54 C37 C36 75.7(8) C55 C54 C37 C38 -99.7(7) C55 C56 C57 C58 1.1(10) C56 C55 C63 C65 35.3(8) C56 C55 C63 C64 -88.1(8) C60 C59 C58 C57 -179.4(6) C36 C41 C40 C39 -1.7(10) C36 C37 C38 C39 1.7(10) C10 C11 C12 C13 86.3(8) C10 C11 C12 C17 -93.0(7) C10 C9 C8 C7 0.4(10) C25 C24 C29 C28 -2.3(9) C25 C24 C29 C30 177.3(6) C47 C42 C43 C44 0.2(10) C47 C42 C43 C51 -177.4(6) C47 C42 C41 C36 -90.9(8) C47 C42 C41 C40 82.8(8) C47 C46 C45 C44 1.1(12) C28 C29 C30 C31 59.6(8) C28 C29 C30 C32 -63.6(8) C28 C27 C26 C25 -0.5(10) C30 C29 C28 C27 -178.4(6) C46 C47 C48 C50 64.9(10) C46 C47 C48 C49 -58.8(11) C58 C59 C60 C61 -40.2(9) C58 C59 C60 C62 82.7(7) C38 C37 C36 N1 176.2(6) C38 C37 C36 C41 -1.2(9) C38 C39 C40 C41 2.2(11) C13 C12 C17 C16 -0.8(9) C13 C12 C17 C18 -179.8(6) C13 C14 C15 C16 -1.8(11) C63 C55 C56 C57 175.4(6) C33 C25 C26 C27 -178.3(6) C44 C43 C51 C53 -94.9(8) C44 C43 C51 C52 27.0(9) C17 C12 C13 C14 -0.1(10) C17 C12 C13 C21 -178.0(6) C17 C16 C15 C14 0.9(11) C26 C25 C33 C35 67.7(8) C26 C25 C33 C34 -56.9(9) C8 C7 C24 C29 -92.5(8) C8 C7 C24 C25 85.1(8) C40 C41 C36 N1 -176.2(6) C40 C41 C36 C37 1.2(9) C40 C39 C38 C37 -2.2(10) C51 C43 C44 C45 177.6(7) C14 C13 C21 C23 46.1(10) C14 C13 C21 C22 -78.2(9) C16 C17 C18 C20 -46.1(10) C16 C17 C18 C19 80.1(9) C18 C17 C16 C15 179.5(6) C1S O1S C4S C3S -11.2(9) C21 C13 C14 C15 179.3(7) C48 C47 C46 C45 178.8(7) C4S O1S C1S C2S -13.1(9) C4S C3S C2S C1S -37.0(9) C6S C7S C8S O2S -24.7(11) C5S O2S C8S C7S 6.9(12) C5S C6S C7S C8S 31.6(10) C7S C6S C5S O2S -28.7(10) C8S O2S C5S C6S 14.4(11)