#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:45:55 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227309 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/59/4035909.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_4035909 loop_ _publ_author_name 'Hewage, Nisansala' 'Daddario, Pedro' 'Lau, Kimberly S. F.' 'Guberman-Pfeffer, Matthew J' 'Gasc\'on, Jos\'e A' 'Zeller, Matthias' 'Lee, Christal O.' 'Khalil, Gamal E.' 'Gouterman, Martin' 'Br\"uckner, Christian' _publ_section_title ; Bacterio- and Isobacteriodilactones by Stepwise or Direct Oxidations of meso-Tetrakis(pentafluorophenyl)porphyrin. ; _journal_issue 1 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 239 _journal_page_last 256 _journal_paper_doi 10.1021/acs.joc.8b02628 _journal_volume 84 _journal_year 2019 _chemical_formula_moiety '2(C54 H20 F20 N6 O4 Os), C6 H14, 5(C H Cl3)' _chemical_formula_sum 'C119 H59 Cl15 F40 N12 O8 Os2' _chemical_formula_weight 3456.93 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 115.910(4) _cell_angle_beta 90.019(5) _cell_angle_gamma 92.124(5) _cell_formula_units_Z 1 _cell_length_a 13.330(4) _cell_length_b 16.128(5) _cell_length_c 16.174(5) _cell_measurement_reflns_used 8564 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.5865 _cell_measurement_theta_min 2.5335 _cell_volume 3125.0(17) _computing_cell_refinement 'SAINT+ 6.45 (Bruker, 2003)' _computing_data_collection 'SMART 5.630 (Bruker, 1997-2002)' _computing_data_reduction 'SAINT+ 6.45' _computing_structure_refinement ; SHELXL-2018/3 (Sheldrick, 2015, 2018), SHELXLE Rev882 (H\"ubschle et al., 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_unetI/netI 0.0909 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 30865 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.281 _diffrn_reflns_theta_min 1.400 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 2.475 _exptl_absorpt_correction_T_max 0.512 _exptl_absorpt_correction_T_min 0.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D. (2015). J. Appl. Cryst. 48 3-10. ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.837 _exptl_crystal_description block _exptl_crystal_F_000 1688 _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.370 _exptl_crystal_size_min 0.290 _refine_diff_density_max 6.777 _refine_diff_density_min -3.784 _refine_diff_density_rms 0.222 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1077 _refine_ls_number_reflns 15345 _refine_ls_number_restraints 671 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.1234 _refine_ls_R_factor_gt 0.0992 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1626P)^2^+30.2913P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2531 _refine_ls_wR_factor_ref 0.2812 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12306 _reflns_number_total 15345 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b02628_si_005.cif _cod_data_source_block 05mz176_0m_new _cod_original_cell_volume 3124.8(16) _cod_database_code 4035909 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.371 _shelx_estimated_absorpt_t_max 0.534 _shelx_res_file ; TITL 05mz176_0m_new in P-1 05mz176_0m_new.res created by SHELXL-2018/3 at 12:39:37 on 11-Apr-2018 CELL 0.71073 13.32960 16.12790 16.17360 115.9100 90.0193 92.1237 ZERR 1.00 0.00400 0.00470 0.00470 0.0044 0.0054 0.0052 LATT 1 SFAC C H N O F CL OS UNIT 119 59 12 8 40 15 2 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.5 SIZE 0.29 0.37 0.50 L.S. 14 BOND $H ACTA CONF FMAP 2 PLAN 120 EADP Os1 Os1B ISOR 0.001 Os1 SIMU 0.01 Os1 > C54B SIMU 0.01 C56 > Cl6B SIMU 0.01 C57 > Cl9 SHEL 99 0.75 DFIX 1.53 C58 C59 C59 C60 C60 C61 C61 C62 C62 C63 DFIX 2.5 C58 C60 C59 C61 C60 C62 C61 C63 DFIX -3.5 C63 C59 SIMU 0.01 C58 > C63 ISOR 0.1 C58 > C63 TWIN -1 0 0 0 0 -1 0 -1 0 WGHT 0.162600 30.291300 BASF 0.20030 FVAR 0.08711 0.51560 C1 1 0.819672 0.497527 0.511965 11.00000 0.03292 0.02810 = 0.04353 0.00775 0.00703 0.00425 C2 1 0.826876 0.573574 0.611332 11.00000 0.03542 0.02446 = 0.03574 0.00199 0.00268 -0.00400 AFIX 13 H2 2 0.892331 0.609230 0.621169 11.00000 -1.20000 AFIX 0 C3 1 0.826280 0.519106 0.667731 11.00000 0.04506 0.02690 = 0.03770 0.00522 -0.00306 0.00003 AFIX 13 H3 2 0.889458 0.533397 0.705640 11.00000 -1.20000 AFIX 0 C4 1 0.823943 0.418888 0.593994 11.00000 0.03577 0.02902 = 0.03646 0.00216 0.00129 -0.00078 C5 1 0.822166 0.345797 0.617344 11.00000 0.05683 0.02733 = 0.02454 0.00618 0.00546 0.00534 C6 1 0.823343 0.251127 0.557954 11.00000 0.05281 0.02747 = 0.03070 0.00356 0.00138 0.00045 C7 1 0.821448 0.177356 0.583804 11.00000 0.07008 0.03223 = 0.03255 0.01070 0.00185 0.00618 AFIX 43 H7 2 0.821602 0.183162 0.644841 11.00000 -1.20000 AFIX 0 C8 1 0.819364 0.096513 0.504890 11.00000 0.08587 0.02131 = 0.03518 0.01088 0.00383 0.00356 AFIX 43 H8 2 0.817558 0.036196 0.501580 11.00000 -1.20000 AFIX 0 C9 1 0.820362 0.118282 0.428976 11.00000 0.05913 0.02354 = 0.03281 0.00285 -0.00042 -0.00221 C10 1 0.818255 0.056918 0.336008 11.00000 0.05616 0.02510 = 0.03646 0.00623 -0.00094 -0.00252 C11 1 0.817849 0.080076 0.261864 11.00000 0.05658 0.02932 = 0.03782 0.00682 -0.00126 -0.00280 C12 1 0.817722 0.012881 0.166483 11.00000 0.09164 0.02805 = 0.03396 0.00301 0.00255 -0.00375 AFIX 43 H12 2 0.816872 -0.052309 0.143913 11.00000 -1.20000 AFIX 0 C13 1 0.819019 0.059816 0.116788 11.00000 0.09952 0.03049 = 0.02891 0.00246 0.00030 -0.00563 AFIX 43 H13 2 0.820593 0.034835 0.051645 11.00000 -1.20000 AFIX 0 C14 1 0.817565 0.157555 0.181377 11.00000 0.05738 0.03009 = 0.03788 -0.00127 0.00190 0.00085 C15 1 0.817247 0.227515 0.154746 11.00000 0.07078 0.03914 = 0.03448 0.01133 0.00868 0.00791 C16 1 0.815659 0.321551 0.212218 11.00000 0.07571 0.03752 = 0.03474 0.00773 0.01739 0.01660 C17 1 0.817799 0.394654 0.188935 11.00000 0.10394 0.04563 = 0.04436 0.01679 0.03125 0.02582 AFIX 43 H17 2 0.821830 0.389445 0.128220 11.00000 -1.20000 AFIX 0 C18 1 0.813158 0.476050 0.267703 11.00000 0.09611 0.03157 = 0.04875 0.01137 0.02132 0.01919 AFIX 43 H18 2 0.810964 0.536265 0.271099 11.00000 -1.20000 AFIX 0 C19 1 0.812281 0.453056 0.342391 11.00000 0.06181 0.02513 = 0.04404 0.01183 0.01678 0.01110 C20 1 0.813774 0.517084 0.437341 11.00000 0.04556 0.02466 = 0.03781 0.00975 0.00954 0.00387 C21 1 0.825211 0.367139 0.717597 11.00000 0.07002 0.02329 = 0.03583 0.00438 0.00896 0.01565 C22 1 0.913548 0.393220 0.768011 11.00000 0.10692 0.02375 = 0.04039 0.00933 -0.01436 -0.00008 C23 1 0.920392 0.405007 0.856314 11.00000 0.13053 0.03525 = 0.03893 0.00196 -0.01270 0.01346 C24 1 0.834673 0.391822 0.898567 11.00000 0.13961 0.04266 = 0.02779 0.01164 -0.00501 0.02056 C25 1 0.745965 0.367775 0.852276 11.00000 0.12810 0.03452 = 0.04647 0.01340 0.03031 0.03105 C26 1 0.741166 0.355739 0.763310 11.00000 0.08359 0.03715 = 0.03786 0.01500 0.00876 0.01961 C27 1 0.813003 -0.043582 0.312923 11.00000 0.07065 0.02856 = 0.02711 0.00705 0.00421 0.01018 C28 1 0.896650 -0.087793 0.320183 11.00000 0.07046 0.02610 = 0.02796 0.00248 0.00143 0.00163 C29 1 0.892759 -0.183125 0.292247 11.00000 0.09822 0.02782 = 0.03409 0.00984 0.00948 0.01580 C30 1 0.804761 -0.232909 0.260373 11.00000 0.10760 0.01738 = 0.04228 0.00464 0.00391 -0.00203 C31 1 0.718717 -0.189982 0.254916 11.00000 0.07852 0.03142 = 0.05168 0.02158 -0.01076 -0.00874 C32 1 0.726596 -0.096659 0.282738 11.00000 0.06645 0.02863 = 0.04356 0.00858 -0.00441 -0.00158 C33 1 0.819679 0.203191 0.053855 11.00000 0.09982 0.03457 = 0.03089 0.01006 0.00804 0.01412 C34 1 0.732832 0.192911 0.006161 11.00000 0.08881 0.04595 = 0.04224 0.00985 0.01113 -0.00030 C35 1 0.732370 0.172062 -0.087906 11.00000 0.10422 0.04581 = 0.04415 0.00517 0.00209 0.00325 C36 1 0.820235 0.158123 -0.133382 11.00000 0.13413 0.03381 = 0.03312 0.00841 0.01563 0.01885 C37 1 0.907229 0.165339 -0.087418 11.00000 0.11815 0.11732 = 0.05557 0.03959 0.02740 0.03113 C38 1 0.908307 0.187900 0.005569 11.00000 0.11999 0.12415 = 0.06299 0.06449 0.03912 0.05155 C39 1 0.802481 0.615534 0.453998 11.00000 0.06201 0.02752 = 0.03743 0.01240 0.01027 0.00738 C40 1 0.882011 0.679403 0.477588 11.00000 0.05999 0.03108 = 0.03106 0.00571 0.00280 0.00345 C41 1 0.869889 0.769223 0.490993 11.00000 0.07102 0.02254 = 0.03601 0.00544 0.00644 0.00130 C42 1 0.776344 0.793904 0.478062 11.00000 0.06600 0.03933 = 0.04312 0.01872 0.01237 0.01229 C43 1 0.695137 0.735232 0.455333 11.00000 0.06765 0.04007 = 0.04417 0.01053 0.01336 0.01527 C44 1 0.711416 0.644430 0.444571 11.00000 0.06546 0.02735 = 0.04974 0.01106 0.01334 0.00110 PART 1 10.5 OS1 7 0.632045 0.607028 0.695629 10.50000 0.03600 0.02213 = 0.02412 0.00287 -0.00207 0.00407 N5 3 0.531370 0.688561 0.665097 10.50000 0.04107 0.02819 = 0.03290 0.00279 0.00097 0.00870 C45 1 0.539929 0.783002 0.711756 10.50000 0.04885 0.03075 = 0.03769 0.00374 0.00009 0.00335 AFIX 43 H45 2 0.587754 0.810436 0.760754 10.50000 -1.20000 AFIX 0 C46 1 0.482370 0.837979 0.690026 10.50000 0.05121 0.03286 = 0.04155 0.00762 -0.00082 0.00425 AFIX 43 H46 2 0.484357 0.902557 0.728179 10.50000 -1.20000 AFIX 0 C47 1 0.420491 0.801023 0.612617 10.50000 0.05083 0.03545 = 0.04242 0.00881 -0.00290 0.00698 AFIX 43 H47 2 0.385460 0.839704 0.592991 10.50000 -1.20000 AFIX 0 C48 1 0.411392 0.707638 0.565529 10.50000 0.04791 0.03573 = 0.04042 0.00491 -0.00344 0.00738 AFIX 43 H48 2 0.366562 0.679934 0.514158 10.50000 -1.20000 AFIX 0 C49 1 0.467797 0.652804 0.592698 10.50000 0.04533 0.03015 = 0.03546 0.00184 -0.00301 0.00852 AFIX 43 H49 2 0.461059 0.587649 0.558746 10.50000 -1.20000 AFIX 0 SAME N5 > C49 N6 3 0.518744 0.562230 0.763699 10.50000 0.05498 0.03947 = 0.04747 0.01622 0.01187 0.00645 C50 1 0.471957 0.622733 0.840949 10.50000 0.05689 0.04327 = 0.04801 0.01685 0.01182 0.00533 AFIX 43 H50 2 0.487374 0.687009 0.863901 10.50000 -1.20000 AFIX 0 C51 1 0.404133 0.592513 0.885144 10.50000 0.06049 0.04539 = 0.04962 0.01984 0.01295 0.00288 AFIX 43 H51 2 0.370728 0.635982 0.936988 10.50000 -1.20000 AFIX 0 C52 1 0.382898 0.499013 0.855666 10.50000 0.06082 0.04394 = 0.05091 0.02117 0.01238 0.00116 AFIX 43 H52 2 0.335008 0.477927 0.886420 10.50000 -1.20000 AFIX 0 C53 1 0.432477 0.437880 0.781319 10.50000 0.06029 0.04350 = 0.05184 0.01715 0.01091 0.00045 AFIX 43 H53 2 0.419886 0.373317 0.759407 10.50000 -1.20000 AFIX 0 C54 1 0.501752 0.471992 0.738320 10.50000 0.05674 0.04120 = 0.05226 0.01466 0.01101 0.00200 AFIX 43 H54 2 0.538656 0.429300 0.688706 10.50000 -1.20000 AFIX 0 PART 2 10.5 SAME Os1 > C54 OS1B 7 0.650980 0.601195 0.702373 10.50000 0.03600 0.02213 = 0.02412 0.00287 -0.00207 0.00407 N5B 3 0.542680 0.678964 0.671989 10.50000 0.04246 0.02999 = 0.03119 0.00078 -0.00347 0.00736 C45B 1 0.508500 0.760990 0.737076 10.50000 0.05024 0.03571 = 0.04090 -0.00054 -0.00095 0.00921 AFIX 43 H45B 2 0.532359 0.782857 0.798675 10.50000 -1.20000 AFIX 0 C46B 1 0.442481 0.812002 0.717482 10.50000 0.05445 0.03976 = 0.04428 0.00121 -0.00148 0.00696 AFIX 43 H46B 2 0.421576 0.868417 0.764876 10.50000 -1.20000 AFIX 0 C47B 1 0.405125 0.782269 0.628392 10.50000 0.05125 0.03669 = 0.04240 0.00718 -0.00256 0.00809 AFIX 43 H47B 2 0.363141 0.819550 0.612391 10.50000 -1.20000 AFIX 0 C48B 1 0.431329 0.697255 0.564901 10.50000 0.04728 0.03446 = 0.03899 0.00575 -0.00501 0.00896 AFIX 43 H48B 2 0.406092 0.673361 0.503540 10.50000 -1.20000 AFIX 0 C49B 1 0.495076 0.645734 0.590314 10.50000 0.04417 0.03095 = 0.03518 0.00154 -0.00180 0.00757 AFIX 43 H49B 2 0.505372 0.583766 0.547511 10.50000 -1.20000 AFIX 0 N6B 3 0.544346 0.572207 0.789002 10.50000 0.05580 0.03974 = 0.04952 0.01581 0.01287 0.00510 C50B 1 0.533779 0.632370 0.880596 10.50000 0.05826 0.04382 = 0.05051 0.01560 0.01401 0.00344 AFIX 43 H50B 2 0.565018 0.692233 0.902371 10.50000 -1.20000 AFIX 0 C51B 1 0.481639 0.611302 0.941286 10.50000 0.06022 0.04771 = 0.05119 0.01539 0.01458 0.00275 AFIX 43 H51B 2 0.475220 0.656467 1.002955 10.50000 -1.20000 AFIX 0 C52B 1 0.437787 0.523962 0.913319 10.50000 0.06246 0.04792 = 0.05362 0.01636 0.01367 0.00029 AFIX 43 H52B 2 0.402991 0.507214 0.955385 10.50000 -1.20000 AFIX 0 C53B 1 0.446228 0.462450 0.822942 10.50000 0.06145 0.04616 = 0.05400 0.01569 0.01186 0.00025 AFIX 43 H53B 2 0.413622 0.403077 0.800287 10.50000 -1.20000 AFIX 0 C54B 1 0.502931 0.487432 0.764359 10.50000 0.05708 0.04255 = 0.05235 0.01440 0.01001 0.00267 AFIX 43 H54B 2 0.512826 0.441812 0.703476 10.50000 -1.20000 AFIX 0 PART 0 N1 3 0.820133 0.411231 0.507859 11.00000 0.04020 0.02835 = 0.04056 0.01241 0.00478 0.00264 N2 3 0.822805 0.213139 0.463998 11.00000 0.05967 0.02480 = 0.02815 0.00629 -0.00284 -0.00162 AFIX 43 H2A 2 0.823856 0.244412 0.430989 11.00000 -1.20000 AFIX 0 N3 3 0.816304 0.167295 0.269492 11.00000 0.05617 0.02845 = 0.03137 0.00518 0.00104 -0.00289 N4 3 0.816558 0.358990 0.308753 11.00000 0.07033 0.02736 = 0.03019 0.00878 0.01094 0.00618 AFIX 43 H4 2 0.819357 0.327758 0.341676 11.00000 -1.20000 AFIX 0 O1 4 0.746828 0.634550 0.631691 11.00000 0.05330 0.02643 = 0.04169 0.01339 0.00603 0.00685 O2 4 0.741112 0.534361 0.724977 11.00000 0.06271 0.02998 = 0.01743 0.00256 0.00318 0.00069 O3 4 0.585727 0.512316 0.605858 11.00000 0.05991 0.02507 = 0.05378 -0.00441 -0.01368 -0.00480 O4 4 0.663682 0.704556 0.801492 11.00000 0.08483 0.02846 = 0.02861 0.00896 -0.00417 -0.00339 F1 5 0.652689 0.328699 0.716754 11.00000 0.07634 0.05332 = 0.06481 0.02590 0.02350 0.01734 F2 5 0.662638 0.357501 0.894095 11.00000 0.16270 0.06092 = 0.05739 0.02420 0.04713 0.03488 F3 5 0.835851 0.406105 0.987161 11.00000 0.22016 0.06438 = 0.02725 0.01886 -0.00310 0.02615 F4 5 1.010426 0.429545 0.901927 11.00000 0.15484 0.05485 = 0.05975 0.01093 -0.05287 -0.00038 F5 5 0.998394 0.405113 0.728007 11.00000 0.07967 0.04057 = 0.05569 0.01422 -0.02232 -0.00187 F6 5 0.984469 -0.042117 0.348486 11.00000 0.07086 0.03786 = 0.05087 0.00227 -0.00183 0.00329 F7 5 0.975186 -0.224065 0.296609 11.00000 0.10004 0.04174 = 0.06963 0.01100 0.00763 0.02640 F8 5 0.799288 -0.324106 0.236310 11.00000 0.12422 0.01893 = 0.05455 0.00814 0.00199 0.00110 F9 5 0.632485 -0.239610 0.224430 11.00000 0.10089 0.03471 = 0.08687 0.01812 -0.02010 -0.02287 F10 5 0.642960 -0.056581 0.272963 11.00000 0.08322 0.04204 = 0.08772 0.02385 -0.02426 -0.01242 F11 5 0.643805 0.204627 0.048838 11.00000 0.07459 0.13610 = 0.04288 0.00407 0.00955 0.00720 F12 5 0.644403 0.165096 -0.130392 11.00000 0.11818 0.15113 = 0.05348 -0.00236 -0.02375 -0.00055 F13 5 0.817988 0.137287 -0.222862 11.00000 0.16868 0.05169 = 0.03337 0.01269 0.00694 0.01643 F14 5 0.990810 0.147719 -0.135660 11.00000 0.12045 0.28459 = 0.06489 0.06873 0.02083 0.02672 F15 5 0.993049 0.189589 0.047072 11.00000 0.10335 0.37319 = 0.07893 0.12338 0.03816 0.07467 F16 5 0.973858 0.655839 0.490784 11.00000 0.05233 0.04071 = 0.04439 0.01319 0.00487 0.00431 F17 5 0.948472 0.829304 0.512899 11.00000 0.07113 0.03496 = 0.05416 0.00595 0.00504 -0.00205 F18 5 0.765220 0.881061 0.490151 11.00000 0.08481 0.03247 = 0.05794 0.01755 0.01210 0.01093 F19 5 0.607336 0.759626 0.446246 11.00000 0.07670 0.07051 = 0.14324 0.07669 0.04475 0.04128 F20 5 0.630277 0.584875 0.422127 11.00000 0.04972 0.05177 = 0.09463 0.03690 0.00854 0.00320 C55 1 1.175025 0.156798 0.239594 11.00000 0.06844 0.04199 = 0.06015 0.01037 0.01766 0.00099 AFIX 13 H55 2 1.215713 0.215459 0.256448 11.00000 -1.20000 AFIX 0 CL1 6 1.054339 0.183611 0.282457 11.00000 0.07501 0.07427 = 0.06285 0.01343 0.01751 0.00674 CL2 6 1.235356 0.089847 0.282087 11.00000 0.12655 0.10254 = 0.07103 0.02091 0.02155 0.04950 CL3 6 1.168751 0.096681 0.121840 11.00000 0.25382 0.27603 = 0.03778 -0.01061 0.00676 0.16842 PART 1 10.5 SAME C55 > Cl3 C56 1 0.809465 0.661177 0.939802 10.50000 0.10995 0.04833 = 0.06986 0.01354 -0.01231 0.00799 AFIX 13 H56 2 0.772199 0.637162 0.879626 10.50000 -1.20000 AFIX 0 CL4 6 0.795024 0.779870 0.995999 10.50000 0.11245 0.03968 = 0.07842 -0.00564 -0.03352 0.01274 CL5 6 0.757736 0.606853 1.001956 10.50000 0.11793 0.06187 = 0.07515 0.01589 0.01920 0.02144 CL6 6 0.934458 0.635370 0.916779 10.50000 0.08289 0.04517 = 0.09224 0.00670 -0.01332 0.00653 PART 2 10.5 SAME C55 > Cl3 C56B 1 0.736385 0.658615 0.957315 10.50000 0.11386 0.04601 = 0.06371 0.01570 -0.01520 0.00512 AFIX 13 H56B 2 0.739958 0.647572 0.891565 10.50000 -1.20000 AFIX 0 CL4B 6 0.706891 0.774235 1.024162 10.50000 0.15673 0.03666 = 0.04687 0.01013 -0.01395 -0.00288 CL5B 6 0.645720 0.583295 0.965771 10.50000 0.10730 0.04213 = 0.05393 0.02435 -0.00469 -0.00328 CL6B 6 0.852568 0.635766 0.990604 10.50000 0.10479 0.06392 = 0.08963 0.02590 -0.03715 -0.00786 PART -1 10.5 SAME C55 > Cl3 C57 1 0.540977 1.005607 1.042332 10.50000 0.16347 0.12756 = 0.10119 0.00475 -0.01728 -0.02468 AFIX 13 H57 2 0.583256 1.059624 1.085906 10.50000 -1.20000 AFIX 0 CL7 6 0.544687 0.921389 1.082337 10.50000 0.16313 0.15121 = 0.12310 0.02208 -0.03916 -0.04909 CL8 6 0.587680 0.976048 0.933764 10.50000 0.17731 0.11015 = 0.08204 -0.02175 0.02558 -0.06688 CL9 6 0.419916 1.043518 1.047407 10.50000 0.14902 0.13675 = 0.11061 0.00538 -0.04388 0.03655 PART -1 10.5 C58 1 0.590053 0.998060 0.618115 10.50000 0.11757 0.16311 = 0.13698 0.04917 0.03311 0.04015 AFIX 33 H58A 2 0.648019 1.041408 0.642598 10.50000 -1.50000 H58B 2 0.539405 1.012309 0.665801 10.50000 -1.50000 H58C 2 0.611567 0.934950 0.598983 10.50000 -1.50000 AFIX 0 C59 1 0.545382 1.006598 0.535940 10.50000 0.10921 0.15177 = 0.14213 0.06315 0.03146 0.03993 AFIX 23 H59A 2 0.596690 0.993020 0.487993 10.50000 -1.20000 H59B 2 0.524396 1.070520 0.554934 10.50000 -1.20000 AFIX 0 C60 1 0.454387 0.939134 0.496623 10.50000 0.10489 0.14728 = 0.14096 0.06828 0.03310 0.03847 AFIX 23 H60A 2 0.453579 0.893212 0.521914 10.50000 -1.20000 H60B 2 0.391646 0.973187 0.514509 10.50000 -1.20000 AFIX 0 C61 1 0.460303 0.890369 0.392667 10.50000 0.10591 0.14715 = 0.14837 0.06535 0.03533 0.03311 AFIX 23 H61A 2 0.529749 0.897398 0.374278 10.50000 -1.20000 H61B 2 0.444494 0.823681 0.371582 10.50000 -1.20000 AFIX 0 C62 1 0.389309 0.927610 0.346406 10.50000 0.10892 0.14888 = 0.14690 0.06757 0.03615 0.02667 AFIX 23 H62A 2 0.323174 0.935134 0.376122 10.50000 -1.20000 H62B 2 0.379953 0.882437 0.281207 10.50000 -1.20000 AFIX 0 C63 1 0.426636 1.020261 0.350814 10.50000 0.10582 0.15797 = 0.15275 0.05655 0.03839 0.03037 AFIX 33 H63A 2 0.377789 1.041510 0.319760 10.50000 -1.50000 H63B 2 0.434628 1.065686 0.415221 10.50000 -1.50000 H63C 2 0.491420 1.012979 0.320286 10.50000 -1.50000 PART 0 AFIX 0 HKLF 4 REM 05mz176_0m_new in P-1 REM wR2 = 0.2812, GooF = S = 1.036, Restrained GooF = 1.026 for all data REM R1 = 0.0992 for 12306 Fo > 4sig(Fo) and 0.1234 for all 15345 data REM 1077 parameters refined using 671 restraints END WGHT 0.1625 30.1024 REM Highest difference peak 6.777, deepest hole -3.784, 1-sigma level 0.222 Q1 1 0.6449 0.5797 0.7399 11.00000 0.05 6.78 Q2 1 0.6374 0.6298 0.6605 11.00000 0.05 6.71 Q3 1 0.5801 0.6085 0.6901 11.00000 0.05 4.62 Q4 1 0.7103 0.6053 0.7129 11.00000 0.05 3.44 Q5 1 0.6542 0.7820 0.5346 11.00000 0.05 3.07 Q6 1 0.6438 0.8031 0.4906 11.00000 0.05 2.85 Q7 1 1.0752 -0.0126 0.1106 11.00000 0.05 2.68 Q8 1 1.0638 0.0108 0.0697 11.00000 0.05 2.14 Q9 1 1.1198 0.0564 0.1290 11.00000 0.05 1.58 Q10 1 0.6154 0.9998 1.0704 11.00000 0.05 1.38 Q11 1 1.0797 0.1804 -0.1029 11.00000 0.05 1.14 Q12 1 0.6815 0.6646 0.6311 11.00000 0.05 1.11 Q13 1 1.2611 0.1359 0.2790 11.00000 0.05 0.96 Q14 1 0.7381 0.6514 0.5900 11.00000 0.05 0.95 Q15 1 0.5970 0.7341 0.4730 11.00000 0.05 0.93 Q16 1 0.6019 0.6664 0.6336 11.00000 0.05 0.92 Q17 1 0.5278 1.0209 0.9146 11.00000 0.05 0.88 Q18 1 0.5317 1.1011 0.5473 11.00000 0.05 0.85 Q19 1 0.6206 0.7824 0.4194 11.00000 0.05 0.84 Q20 1 0.5971 0.5353 0.7607 11.00000 0.05 0.80 Q21 1 0.5350 0.6763 0.4834 11.00000 0.05 0.80 Q22 1 1.0032 0.2300 0.0657 11.00000 0.05 0.79 Q23 1 0.7465 -0.2133 0.2800 11.00000 0.05 0.78 Q24 1 1.0533 0.2148 0.2468 11.00000 0.05 0.78 Q25 1 0.7765 0.5626 0.7081 11.00000 0.05 0.76 Q26 1 0.5121 0.6473 0.6792 11.00000 0.05 0.76 Q27 1 0.8599 0.7779 1.0434 11.00000 0.05 0.75 Q28 1 0.7518 0.5149 0.7591 11.00000 0.05 0.74 Q29 1 1.1240 0.0370 0.1691 11.00000 0.05 0.74 Q30 1 1.1626 0.1508 0.2812 11.00000 0.05 0.74 Q31 1 0.8095 0.7601 1.0440 11.00000 0.05 0.73 Q32 1 0.5006 0.6218 0.7036 11.00000 0.05 0.71 Q33 1 0.6255 0.3920 0.8526 11.00000 0.05 0.70 Q34 1 0.7115 0.5824 0.9652 11.00000 0.05 0.66 Q35 1 0.8184 0.4212 0.8591 11.00000 0.05 0.66 Q36 1 0.8185 0.6665 1.0039 11.00000 0.05 0.66 Q37 1 0.8615 0.6298 0.9414 11.00000 0.05 0.65 Q38 1 1.0016 0.1853 0.2699 11.00000 0.05 0.65 Q39 1 0.9239 0.6715 0.4802 11.00000 0.05 0.63 Q40 1 0.8167 0.2161 0.0031 11.00000 0.05 0.62 Q41 1 1.0568 0.1620 0.3308 11.00000 0.05 0.61 Q42 1 0.6575 0.5581 0.9992 11.00000 0.05 0.61 Q43 1 0.7005 0.1887 0.0510 11.00000 0.05 0.61 Q44 1 1.0404 0.0701 0.0895 11.00000 0.05 0.61 Q45 1 0.8449 0.7815 0.4645 11.00000 0.05 0.60 Q46 1 0.6271 0.7765 1.0402 11.00000 0.05 0.59 Q47 1 1.0277 0.1450 0.1306 11.00000 0.05 0.58 Q48 1 0.8958 0.0867 0.3020 11.00000 0.05 0.58 Q49 1 0.9584 0.4184 0.9083 11.00000 0.05 0.56 Q50 1 0.6470 -0.0247 0.2345 11.00000 0.05 0.56 Q51 1 0.8877 0.5504 0.6710 11.00000 0.05 0.56 Q52 1 0.9566 -0.0130 -0.1831 11.00000 0.05 0.56 Q53 1 0.9842 0.3822 0.7768 11.00000 0.05 0.56 Q54 1 0.4258 0.6769 0.6004 11.00000 0.05 0.55 Q55 1 0.7541 0.3913 0.9632 11.00000 0.05 0.55 Q56 1 0.5274 0.9711 0.5057 11.00000 0.05 0.54 Q57 1 0.7744 0.9162 0.4516 11.00000 0.05 0.53 Q58 1 1.2825 0.0616 0.2770 11.00000 0.05 0.53 Q59 1 0.6123 0.6045 0.9573 11.00000 0.05 0.53 Q60 1 0.9187 0.4022 0.7270 11.00000 0.05 0.52 Q61 1 0.9456 0.6034 0.9536 11.00000 0.05 0.52 Q62 1 0.7583 0.9498 0.4731 11.00000 0.05 0.52 Q63 1 0.4284 0.9024 0.3439 11.00000 0.05 0.52 Q64 1 0.5003 0.7997 0.7176 11.00000 0.05 0.52 Q65 1 0.8075 0.7867 0.5071 11.00000 0.05 0.51 Q66 1 0.7024 0.1644 -0.1260 11.00000 0.05 0.51 Q67 1 0.6422 -0.0519 0.3241 11.00000 0.05 0.51 Q68 1 0.9751 0.6771 0.4539 11.00000 0.05 0.51 Q69 1 0.7020 1.0255 0.6721 11.00000 0.05 0.50 Q70 1 0.9907 0.4560 0.8604 11.00000 0.05 0.50 Q71 1 0.6346 -0.2611 0.2690 11.00000 0.05 0.50 Q72 1 0.3391 0.3859 0.6764 11.00000 0.05 0.50 Q73 1 0.5218 0.5361 0.6693 11.00000 0.05 0.49 Q74 1 1.0534 0.0014 0.3452 11.00000 0.05 0.48 Q75 1 0.9987 -0.0046 0.3126 11.00000 0.05 0.48 Q76 1 0.3174 0.7864 0.6618 11.00000 0.05 0.48 Q77 1 0.6756 0.3703 0.8220 11.00000 0.05 0.48 Q78 1 0.8831 0.6806 0.9085 11.00000 0.05 0.48 Q79 1 1.1642 0.1864 0.2103 11.00000 0.05 0.48 Q80 1 0.6827 0.6783 0.4759 11.00000 0.05 0.48 Q81 1 0.9472 0.2008 -0.1454 11.00000 0.05 0.47 Q82 1 1.2568 0.1844 0.2292 11.00000 0.05 0.47 Q83 1 0.9750 0.0960 0.0521 11.00000 0.05 0.47 Q84 1 0.7005 -0.0234 0.2794 11.00000 0.05 0.47 Q85 1 0.8189 0.0634 0.3032 11.00000 0.05 0.47 Q86 1 0.8363 0.2043 -0.1031 11.00000 0.05 0.47 Q87 1 0.8876 0.2251 0.4724 11.00000 0.05 0.47 Q88 1 0.8403 0.3600 1.0170 11.00000 0.05 0.47 Q89 1 0.6629 0.6959 0.8467 11.00000 0.05 0.47 Q90 1 0.9241 0.2275 -0.1115 11.00000 0.05 0.47 Q91 1 0.8938 0.3542 0.9886 11.00000 0.05 0.47 Q92 1 0.7764 0.1726 -0.1039 11.00000 0.05 0.47 Q93 1 0.8850 -0.0001 0.3196 11.00000 0.05 0.47 Q94 1 0.8724 0.0720 0.3371 11.00000 0.05 0.46 Q95 1 1.1182 0.2370 -0.1053 11.00000 0.05 0.46 Q96 1 0.7542 0.6334 0.4678 11.00000 0.05 0.46 Q97 1 0.8613 0.9021 0.4854 11.00000 0.05 0.46 Q98 1 0.8225 0.5534 0.6485 11.00000 0.05 0.46 Q99 1 0.7267 0.0858 0.4780 11.00000 0.05 0.46 Q100 1 0.8863 0.0670 0.1388 11.00000 0.05 0.45 Q101 1 0.4817 0.6789 0.5659 11.00000 0.05 0.45 Q102 1 0.8847 0.4150 0.5180 11.00000 0.05 0.45 Q103 1 1.0025 0.8007 0.5018 11.00000 0.05 0.45 Q104 1 0.4141 1.0837 1.0100 11.00000 0.05 0.45 Q105 1 1.0583 0.3924 0.9282 11.00000 0.05 0.45 Q106 1 0.8442 0.6634 1.1143 11.00000 0.05 0.45 Q107 1 0.9143 -0.1189 0.2873 11.00000 0.05 0.45 Q108 1 0.7612 0.3801 0.8716 11.00000 0.05 0.45 Q109 1 1.0557 -0.1777 0.3194 11.00000 0.05 0.45 Q110 1 0.8366 0.5878 1.0275 11.00000 0.05 0.44 Q111 1 0.4164 0.6096 0.8382 11.00000 0.05 0.44 Q112 1 1.1230 0.0849 0.2764 11.00000 0.05 0.44 Q113 1 0.7784 0.3659 0.9786 11.00000 0.05 0.44 Q114 1 0.4628 1.1164 0.5384 11.00000 0.05 0.44 Q115 1 1.0888 0.4163 0.7161 11.00000 0.05 0.44 Q116 1 1.1468 0.0202 0.2225 11.00000 0.05 0.44 Q117 1 0.8823 0.0046 0.1779 11.00000 0.05 0.43 Q118 1 0.8839 0.2068 0.2757 11.00000 0.05 0.43 Q119 1 0.8636 0.8425 1.0790 11.00000 0.05 0.43 Q120 1 0.6040 -0.2065 0.2049 11.00000 0.05 0.43 ; _shelx_res_checksum 11008 _shelx_hkl_file ; 1 0 0 1.30 0.13 -1 0 0 1.07 0.12 2 0 0 259.19 22.67 -2 0 0 278.62 22.82 -2 0 0 281.81 22.75 3 0 0 88.41 7.10 -3 0 0 85.84 7.09 -3 0 0 80.85 7.10 4 0 0 60.82 5.64 -4 0 0 70.32 5.63 -4 0 0 70.57 5.64 5 0 0 549.97 44.27 -5 0 0 546.26 44.32 -5 0 0 507.68 44.26 6 0 0 269.80 22.83 6 0 0 269.74 22.83 -6 0 0 266.97 22.81 -6 0 0 293.44 22.86 7 0 0 94.76 7.77 -7 0 0 91.30 7.77 -7 0 0 90.94 7.73 8 0 0 0.69 0.64 -8 0 0 2.11 0.55 -8 0 0 0.95 0.48 9 0 0 6.25 1.01 -9 0 0 8.12 0.97 -9 0 0 9.85 1.07 10 0 0 14.85 1.47 -10 0 0 13.70 1.40 -10 0 0 12.61 1.49 11 0 0 85.41 7.31 -11 0 0 83.92 7.28 -11 0 0 88.91 7.38 12 0 0 -0.90 0.85 13 0 0 15.43 1.61 -13 0 0 14.76 1.54 14 0 0 0.92 0.96 -14 0 0 0.69 0.78 15 0 0 2.45 0.90 16 0 0 -0.12 0.99 17 0 0 8.98 1.21 18 0 0 2.68 0.88 18 0 -1 1.97 1.00 17 0 -1 2.03 1.07 16 0 -1 4.12 0.91 -15 0 1 5.71 0.98 15 0 -1 6.79 1.05 -14 0 1 -0.04 0.80 14 0 -1 0.37 0.85 -13 0 1 0.91 0.84 13 0 -1 2.11 0.93 -12 0 1 1.34 0.86 12 0 -1 2.10 0.75 -11 0 1 28.20 2.64 11 0 -1 30.35 2.68 -10 0 1 7.50 1.01 10 0 -1 8.92 1.05 -9 0 1 80.53 7.12 -9 0 1 90.28 7.16 9 0 -1 82.41 7.14 -8 0 1 27.83 2.68 -8 0 1 30.41 2.67 8 0 -1 32.86 2.71 -7 0 1 2.68 0.50 -7 0 1 0.75 0.55 7 0 -1 1.64 0.55 -6 0 1 8.37 0.85 -6 0 1 8.53 0.85 6 0 -1 6.49 0.85 -5 0 1 52.48 4.91 -5 0 1 66.55 4.93 5 0 -1 56.24 4.93 -4 0 1 177.54 16.69 -4 0 1 208.29 16.68 4 0 -1 216.44 16.69 -3 0 1 65.82 5.45 3 0 -1 64.47 5.45 -2 0 1 98.41 7.92 2 0 -1 91.65 7.91 -1 0 1 159.92 13.42 1 0 -1 161.54 13.40 0 0 1 35.88 3.03 1 0 1 48.35 4.16 -1 0 -1 51.01 4.17 2 0 1 180.96 14.54 -2 0 -1 179.34 14.69 -2 0 -1 164.91 14.55 3 0 1 57.90 4.07 -3 0 -1 37.28 4.04 -3 0 -1 49.50 4.04 4 0 1 67.45 5.69 -4 0 -1 67.34 5.70 -4 0 -1 68.47 5.66 5 0 1 4.66 0.78 -5 0 -1 8.51 0.79 -5 0 -1 7.99 0.72 6 0 1 50.42 4.11 -6 0 -1 43.29 4.10 -6 0 -1 50.47 4.07 7 0 1 45.70 3.64 -7 0 -1 41.95 3.58 -7 0 -1 38.39 3.64 8 0 1 26.23 2.56 -8 0 -1 26.79 2.50 -8 0 -1 33.29 2.61 9 0 1 39.70 3.28 -9 0 -1 33.29 3.18 -9 0 -1 37.88 3.29 10 0 1 4.69 0.86 -10 0 -1 3.73 0.87 -10 0 -1 3.58 0.73 11 0 1 12.84 1.32 -11 0 -1 8.15 1.36 -11 0 -1 8.92 1.18 12 0 1 0.40 0.99 -12 0 -1 0.15 0.85 -12 0 -1 -0.66 0.78 13 0 1 14.97 1.55 -13 0 -1 12.40 1.44 14 0 1 2.04 1.02 16 0 1 2.17 1.11 17 0 1 2.56 0.88 18 0 1 0.48 0.97 18 0 -2 0.59 0.99 17 0 -2 2.05 0.81 -16 0 2 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65.71 5.47 1 0 -3 65.07 5.47 0 0 3 132.25 10.98 0 0 3 131.30 10.98 0 0 -3 131.49 10.96 1 0 3 118.97 10.82 -1 0 -3 140.93 10.83 2 0 3 176.77 15.42 -2 0 -3 194.66 15.45 3 0 3 110.58 9.22 4 0 3 34.28 2.70 -4 0 -3 28.15 2.71 5 0 3 3.65 0.50 -5 0 -3 1.56 0.49 6 0 3 19.65 1.86 -6 0 -3 22.13 1.91 -6 0 -3 20.19 1.80 7 0 3 21.96 2.26 -7 0 -3 24.87 2.20 -7 0 -3 29.18 2.33 8 0 3 22.46 1.78 -8 0 -3 16.24 1.78 -8 0 -3 16.83 1.66 9 0 3 32.54 2.83 -9 0 -3 33.02 2.90 -9 0 -3 29.38 2.75 10 0 3 10.62 1.35 -10 0 -3 14.70 1.47 -10 0 -3 12.68 1.27 11 0 3 8.16 1.18 -11 0 -3 11.97 1.32 -11 0 -3 8.32 1.05 12 0 3 6.94 0.99 -12 0 -3 3.63 1.01 13 0 3 7.36 1.13 -13 0 -3 7.74 1.14 14 0 3 4.62 0.94 15 0 3 1.56 1.07 16 0 3 1.74 0.83 17 0 3 0.95 0.98 18 0 3 1.50 1.03 -18 0 4 -0.32 0.79 18 0 -4 0.54 0.85 -17 0 4 1.73 0.95 17 0 -4 2.37 0.78 -16 0 4 2.59 0.87 16 0 -4 3.41 0.79 -15 0 4 0.10 0.88 15 0 -4 0.64 0.81 -14 0 4 1.64 0.79 14 0 -4 1.72 0.76 -13 0 4 16.91 1.73 13 0 -4 16.33 1.71 -12 0 4 0.57 0.86 12 0 -4 1.70 0.71 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8 0.77 0.50 -6 21 -8 -0.70 1.16 6 -21 8 -0.09 0.49 -5 21 -8 0.98 1.22 5 -21 8 0.74 0.58 -4 21 -8 1.99 1.42 4 -21 8 2.48 0.63 -3 21 -8 1.59 1.34 3 -21 8 1.18 0.56 -2 21 -8 2.42 1.39 2 -21 8 1.98 0.61 -1 21 -8 3.45 1.36 1 -21 8 5.06 0.81 0 21 -8 4.76 1.37 0 -21 8 3.43 0.75 1 21 -8 3.37 1.29 -1 -21 8 0.48 0.62 2 21 -8 1.90 1.42 -2 -21 8 1.37 0.60 3 21 -8 3.67 1.35 -3 -21 8 4.78 0.80 4 21 -8 1.51 1.34 -4 -21 8 0.39 0.61 5 21 -8 0.91 1.33 -5 -21 8 0.45 0.62 6 21 -8 4.59 1.36 -6 -21 8 4.12 0.79 7 21 -8 2.25 1.17 -7 -21 8 1.50 0.54 -8 21 -7 0.03 1.01 8 -21 7 -0.15 0.41 -7 21 -7 -0.43 1.15 7 -21 7 0.07 0.45 -6 21 -7 -0.19 1.20 6 -21 7 0.60 0.52 -5 21 -7 2.68 1.28 5 -21 7 4.20 0.69 -4 21 -7 1.07 1.30 4 -21 7 0.89 0.61 -3 21 -7 5.63 1.41 3 -21 7 4.70 0.78 -2 21 -7 2.84 1.28 2 -21 7 4.00 0.74 -1 21 -7 1.93 1.34 1 -21 7 1.66 0.63 0 21 -7 2.56 1.22 0 -21 7 1.29 0.70 1 21 -7 2.64 1.20 -1 -21 7 1.85 0.61 2 21 -7 0.67 1.18 -2 -21 7 1.21 0.67 3 21 -7 1.23 1.36 -3 -21 7 0.24 0.62 4 21 -7 0.80 1.31 -4 -21 7 0.62 0.66 5 21 -7 2.27 1.39 -5 -21 7 2.70 0.71 6 21 -7 1.73 1.33 -6 -21 7 2.40 0.69 7 21 -7 -0.16 1.13 8 -21 6 0.82 0.37 -7 21 -6 0.98 1.16 7 -21 6 1.11 0.44 -6 21 -6 -0.43 1.11 6 -21 6 0.15 0.50 -5 21 -6 -0.45 1.19 5 -21 6 0.48 0.55 -4 21 -6 7.24 1.42 4 -21 6 6.29 0.88 -3 21 -6 3.26 1.23 3 -21 6 2.84 0.68 -2 21 -6 -0.61 1.09 2 -21 6 -0.18 0.58 -1 21 -6 1.65 1.27 1 -21 6 1.56 0.62 0 21 -6 6.97 1.40 0 -21 6 6.10 0.91 1 21 -6 2.60 1.21 -1 -21 6 2.45 0.66 2 21 -6 1.99 1.28 -2 -21 6 1.06 0.67 3 21 -6 2.31 1.19 -3 -21 6 2.30 0.68 4 21 -6 3.15 1.29 -4 -21 6 2.94 0.75 5 21 -6 0.33 1.22 -5 -21 6 -0.13 0.69 6 21 -6 1.55 1.31 -6 -21 6 1.64 0.66 -7 21 -5 -0.12 1.03 7 -21 5 -0.30 0.40 -6 21 -5 -0.65 1.05 6 -21 5 0.06 0.49 -5 21 -5 3.73 1.22 5 -21 5 3.14 0.64 -4 21 -5 1.41 1.15 4 -21 5 1.28 0.54 -3 21 -5 -0.17 1.13 3 -21 5 -0.12 0.57 -2 21 -5 3.73 1.18 2 -21 5 4.12 0.76 -1 21 -5 5.80 1.27 1 -21 5 4.40 0.79 0 21 -5 1.41 1.25 0 -21 5 0.16 0.58 1 21 -5 -0.43 1.09 -1 -21 5 0.31 0.62 2 21 -5 5.47 1.30 -2 -21 5 5.38 0.90 3 21 -5 2.31 1.14 -3 -21 5 1.53 0.69 4 21 -5 -0.42 1.05 -4 -21 5 -0.24 0.64 5 21 -5 1.73 1.34 -5 -21 5 2.57 0.74 6 21 -5 3.81 1.24 -6 -21 5 3.58 0.77 -6 21 -4 0.89 1.11 6 -21 4 1.95 0.51 -5 21 -4 1.30 1.10 5 -21 4 1.18 0.50 -4 21 -4 0.43 1.07 4 -21 4 0.68 0.59 -3 21 -4 2.39 1.09 3 -21 4 3.83 0.69 -2 21 -4 5.32 1.24 2 -21 4 3.40 0.73 -1 21 -4 1.59 1.13 1 -21 4 0.69 0.62 0 21 -4 2.10 1.10 0 -21 4 2.51 0.67 1 21 -4 5.83 1.29 -1 -21 4 5.32 0.90 2 21 -4 2.87 1.14 -2 -21 4 2.03 0.73 3 21 -4 0.12 1.08 -3 -21 4 1.08 0.76 4 21 -4 0.97 1.11 -4 -21 4 1.94 0.70 5 21 -4 0.56 1.10 -5 -21 4 1.99 0.69 -6 21 -3 0.84 0.97 6 -21 3 0.52 0.42 -5 21 -3 2.98 1.05 5 -21 3 3.21 0.62 -4 21 -3 2.16 1.06 4 -21 3 3.03 0.63 -3 21 -3 2.39 1.03 3 -21 3 0.84 0.61 -2 21 -3 0.76 1.05 2 -21 3 0.69 0.59 -1 21 -3 1.32 1.09 1 -21 3 0.93 0.64 0 21 -3 1.91 1.15 0 -21 3 1.97 0.65 1 21 -3 4.14 1.11 -1 -21 3 1.74 0.71 2 21 -3 1.00 1.12 -2 -21 3 1.43 0.77 3 21 -3 3.61 1.18 -3 -21 3 4.46 0.87 4 21 -3 2.81 1.09 -4 -21 3 1.67 0.72 -5 21 -2 2.86 0.96 5 -21 2 4.29 0.65 -4 21 -2 1.73 0.91 4 -21 2 1.25 0.51 -3 21 -2 2.71 1.03 3 -21 2 2.39 0.59 -2 21 -2 3.61 1.07 2 -21 2 3.99 0.72 -1 21 -2 2.04 0.99 1 -21 2 1.84 0.62 0 21 -2 3.28 1.05 0 -21 2 2.60 0.71 1 21 -2 2.90 1.05 -1 -21 2 3.59 0.79 2 21 -2 4.95 1.18 -2 -21 2 5.41 0.93 3 21 -2 1.28 1.04 -3 -21 2 0.73 0.72 3 -21 1 2.85 0.60 -2 21 -1 0.25 0.90 2 -21 1 0.87 0.57 -1 21 -1 3.14 0.94 1 -21 1 2.29 0.64 0 21 -1 6.34 1.21 0 -21 1 8.20 1.06 1 21 -1 2.49 0.92 -1 -21 1 1.74 0.68 3 -22 15 2.52 0.53 -2 22 -15 2.78 1.17 2 -22 15 1.21 0.46 -1 22 -15 0.48 1.32 1 -22 15 0.24 0.46 0 22 -15 1.59 1.30 0 -22 15 0.45 0.48 1 22 -15 3.54 1.27 -1 -22 15 1.64 0.49 2 22 -15 5.22 1.33 -2 -22 15 3.39 0.59 4 -22 14 1.40 0.49 -3 22 -14 3.96 1.29 3 -22 14 3.79 0.64 -2 22 -14 2.55 1.23 2 -22 14 0.39 0.51 -1 22 -14 2.01 1.38 1 -22 14 2.83 0.58 0 22 -14 3.41 1.36 0 -22 14 1.21 0.50 1 22 -14 3.77 1.36 -1 -22 14 1.94 0.54 2 22 -14 3.45 1.29 -2 -22 14 0.30 0.50 3 22 -14 5.92 1.43 -3 -22 14 4.89 0.72 5 -22 13 1.85 0.51 -4 22 -13 1.13 1.31 4 -22 13 1.67 0.50 -3 22 -13 0.49 1.23 3 -22 13 0.32 0.52 -2 22 -13 2.82 1.34 2 -22 13 3.61 0.65 -1 22 -13 6.77 1.51 1 -22 13 3.63 0.68 0 22 -13 2.98 1.39 0 -22 13 0.03 0.53 1 22 -13 1.70 1.43 -1 -22 13 1.44 0.54 2 22 -13 7.39 1.57 -2 -22 13 6.52 0.89 3 22 -13 6.31 1.43 -3 -22 13 2.17 0.58 4 22 -13 1.61 1.28 -4 -22 13 -0.32 0.42 6 -22 12 1.23 0.47 -5 22 -12 -0.74 1.22 5 -22 12 0.82 0.53 -4 22 -12 0.24 1.22 4 -22 12 0.28 0.51 -3 22 -12 0.18 1.36 3 -22 12 1.26 0.60 -2 22 -12 4.80 1.45 2 -22 12 4.34 0.72 -1 22 -12 4.80 1.47 0 22 -12 3.47 1.49 0 -22 12 2.86 0.64 1 22 -12 2.48 1.48 -1 -22 12 1.35 0.64 2 22 -12 3.61 1.39 -2 -22 12 1.41 0.55 3 22 -12 2.96 1.34 -3 -22 12 0.45 0.56 4 22 -12 5.48 1.46 -4 -22 12 5.84 0.80 -6 22 -11 -0.85 1.14 6 -22 11 0.95 0.44 -5 22 -11 3.19 1.26 5 -22 11 2.97 0.61 -4 22 -11 2.69 1.35 4 -22 11 3.07 0.62 -3 22 -11 -0.34 1.39 3 -22 11 0.78 0.57 -2 22 -11 1.64 1.38 2 -22 11 1.19 0.54 -1 22 -11 3.86 1.41 1 -22 11 2.60 0.64 0 22 -11 3.91 1.40 0 -22 11 2.60 0.64 1 22 -11 3.50 1.44 -1 -22 11 0.94 0.61 2 22 -11 2.07 1.42 -2 -22 11 1.60 0.58 3 22 -11 1.61 1.39 -3 -22 11 1.02 0.63 4 22 -11 2.22 1.38 -4 -22 11 2.37 0.61 5 22 -11 0.63 1.17 -6 22 -10 -0.03 1.17 6 -22 10 1.03 0.47 -5 22 -10 1.32 1.37 5 -22 10 1.58 0.53 -4 22 -10 0.01 1.34 4 -22 10 0.66 0.57 -3 22 -10 6.63 1.52 3 -22 10 6.52 0.89 -2 22 -10 4.37 1.41 2 -22 10 2.79 0.66 -1 22 -10 0.16 1.28 1 -22 10 0.20 0.56 0 22 -10 0.56 1.34 0 -22 10 0.87 0.61 1 22 -10 6.50 1.48 -1 -22 10 5.70 0.87 2 22 -10 5.95 1.51 -2 -22 10 4.56 0.80 3 22 -10 2.73 1.33 -3 -22 10 -0.06 0.58 4 22 -10 1.26 1.36 -4 -22 10 0.58 0.60 5 22 -10 2.02 1.30 -5 -22 10 2.20 0.57 -6 22 -9 0.06 1.18 6 -22 9 0.00 0.46 -5 22 -9 -0.60 1.19 5 -22 9 -0.27 0.50 -4 22 -9 1.37 1.43 4 -22 9 1.97 0.57 -3 22 -9 6.16 1.50 3 -22 9 5.01 0.80 -2 22 -9 1.55 1.40 2 -22 9 0.45 0.60 -1 22 -9 3.78 1.37 1 -22 9 3.80 0.73 0 22 -9 3.87 1.39 0 -22 9 3.60 0.71 1 22 -9 1.92 1.39 -1 -22 9 1.36 0.57 2 22 -9 0.66 1.38 -2 -22 9 0.12 0.60 3 22 -9 3.32 1.29 -3 -22 9 2.76 0.69 4 22 -9 2.74 1.31 -4 -22 9 1.91 0.59 5 22 -9 0.03 1.14 -6 22 -8 -0.95 1.07 6 -22 8 -0.05 0.47 -5 22 -8 0.42 1.22 5 -22 8 1.18 0.58 -4 22 -8 1.47 1.35 4 -22 8 1.25 0.55 -3 22 -8 0.47 1.27 3 -22 8 -0.01 0.55 -2 22 -8 2.29 1.40 2 -22 8 3.94 0.72 -1 22 -8 6.06 1.47 1 -22 8 4.94 0.83 0 22 -8 2.79 1.24 0 -22 8 0.68 0.64 1 22 -8 1.11 1.25 -1 -22 8 1.54 0.62 2 22 -8 2.74 1.27 -2 -22 8 3.12 0.69 3 22 -8 2.23 1.43 -3 -22 8 1.21 0.57 4 22 -8 0.50 1.20 -4 -22 8 -0.21 0.52 6 -22 7 1.54 0.48 -5 22 -7 0.17 1.15 5 -22 7 0.40 0.52 -4 22 -7 1.59 1.27 4 -22 7 1.77 0.57 -3 22 -7 0.21 1.25 3 -22 7 0.31 0.57 -2 22 -7 1.59 1.31 2 -22 7 1.41 0.59 -1 22 -7 1.22 1.25 1 -22 7 0.21 0.62 0 22 -7 1.29 1.24 0 -22 7 1.34 0.69 1 22 -7 1.09 1.23 -1 -22 7 2.04 0.63 2 22 -7 1.11 1.25 -2 -22 7 0.75 0.64 3 22 -7 -0.40 1.12 -3 -22 7 0.01 0.57 4 22 -7 2.13 1.32 -4 -22 7 2.46 0.63 -5 22 -6 1.68 1.18 5 -22 6 1.93 0.54 -4 22 -6 3.18 1.17 4 -22 6 3.90 0.67 -3 22 -6 0.80 1.21 3 -22 6 0.19 0.59 -2 22 -6 1.12 1.21 2 -22 6 0.66 0.62 -1 22 -6 4.92 1.31 1 -22 6 5.80 0.87 0 22 -6 6.34 1.40 0 -22 6 6.03 0.90 1 22 -6 3.45 1.24 -1 -22 6 1.92 0.65 2 22 -6 2.33 1.16 -2 -22 6 1.71 0.63 3 22 -6 0.44 1.09 -3 -22 6 0.52 0.63 4 22 -6 0.27 1.03 -4 22 -5 0.70 1.13 4 -22 5 1.64 0.54 -3 22 -5 5.27 1.21 3 -22 5 4.93 0.80 -2 22 -5 5.28 1.28 2 -22 5 5.13 0.83 -1 22 -5 0.82 1.11 1 -22 5 0.19 0.58 0 22 -5 0.04 1.10 0 -22 5 0.96 0.66 1 22 -5 6.49 1.33 -1 -22 5 5.01 0.86 2 22 -5 4.77 1.22 -2 -22 5 4.30 0.82 3 22 -5 0.36 1.02 -3 -22 5 -0.05 0.57 -3 22 -4 4.79 1.14 3 -22 4 4.48 0.74 -2 22 -4 1.04 1.05 2 -22 4 0.70 0.60 -1 22 -4 5.65 1.21 1 -22 4 5.03 0.84 0 22 -4 2.79 1.06 0 -22 4 2.33 0.66 1 22 -4 0.92 1.04 -1 -22 4 0.59 0.64 2 22 -4 0.04 0.99 -1 23 -12 2.11 1.33 -2 23 -11 0.03 1.23 -1 23 -11 0.11 1.30 1 -23 11 0.33 0.54 0 23 -11 1.66 1.34 0 -23 11 0.90 0.55 1 23 -11 0.71 1.22 -2 23 -10 2.81 1.32 2 -23 10 2.63 0.61 -1 23 -10 3.60 1.32 1 -23 10 1.46 0.55 0 23 -10 3.33 1.32 0 -23 10 4.02 0.68 1 23 -10 1.90 1.35 -2 23 -9 1.70 1.33 2 -23 9 1.36 0.55 -1 23 -9 4.91 1.31 1 -23 9 4.07 0.72 0 23 -9 1.73 1.33 0 -23 9 1.32 0.55 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 80099 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8197(9) 0.4975(8) 0.5120(9) 0.038(3) Uani 1 1 d . . . . . C2 C 0.8269(9) 0.5736(8) 0.6113(9) 0.036(2) Uani 1 1 d . . . . . H2 H 0.892331 0.609230 0.621169 0.043 Uiso 1 1 calc R U . . . C3 C 0.8263(10) 0.5191(8) 0.6677(9) 0.040(3) Uani 1 1 d . . . . . H3 H 0.889458 0.533397 0.705640 0.048 Uiso 1 1 calc R U . . . C4 C 0.8239(9) 0.4189(9) 0.5940(9) 0.038(3) Uani 1 1 d . . . . . C5 C 0.8222(11) 0.3458(8) 0.6173(8) 0.038(3) Uani 1 1 d . . . . . C6 C 0.8233(11) 0.2511(9) 0.5580(9) 0.040(3) Uani 1 1 d . . . . . C7 C 0.8214(12) 0.1774(9) 0.5838(9) 0.046(3) Uani 1 1 d . . . . . H7 H 0.821602 0.183162 0.644841 0.055 Uiso 1 1 calc R U . . . C8 C 0.8194(13) 0.0965(9) 0.5049(9) 0.048(3) Uani 1 1 d . . . . . H8 H 0.817558 0.036196 0.501580 0.058 Uiso 1 1 calc R U . . . C9 C 0.8204(11) 0.1183(8) 0.4290(9) 0.042(3) Uani 1 1 d . . . . . C10 C 0.8183(11) 0.0569(9) 0.3360(9) 0.042(3) Uani 1 1 d . . . . . C11 C 0.8178(11) 0.0801(9) 0.2619(10) 0.044(3) Uani 1 1 d . . . . . C12 C 0.8177(15) 0.0129(10) 0.1665(10) 0.055(4) Uani 1 1 d . . . . . H12 H 0.816872 -0.052309 0.143913 0.066 Uiso 1 1 calc R U . . . C13 C 0.8190(15) 0.0598(10) 0.1168(10) 0.057(4) Uani 1 1 d . . . . . H13 H 0.820593 0.034835 0.051645 0.068 Uiso 1 1 calc R U . . . C14 C 0.8176(12) 0.1576(9) 0.1814(10) 0.048(3) Uani 1 1 d . . . . . C15 C 0.8172(13) 0.2275(10) 0.1547(10) 0.050(3) Uani 1 1 d . . . . . C16 C 0.8157(13) 0.3216(10) 0.2122(10) 0.052(4) Uani 1 1 d . . . . . C17 C 0.8178(17) 0.3947(12) 0.1889(12) 0.065(5) Uani 1 1 d . . . . . H17 H 0.821830 0.389445 0.128220 0.078 Uiso 1 1 calc R U . . . C18 C 0.8132(16) 0.4760(11) 0.2677(12) 0.061(4) Uani 1 1 d . . . . . H18 H 0.810964 0.536265 0.271099 0.073 Uiso 1 1 calc R U . . . C19 C 0.8123(11) 0.4531(8) 0.3424(10) 0.045(3) Uani 1 1 d . . . . . C20 C 0.8138(10) 0.5171(8) 0.4373(9) 0.037(3) Uani 1 1 d . . . . . C21 C 0.8252(12) 0.3671(9) 0.7176(10) 0.046(3) Uani 1 1 d . . . . . C22 C 0.9135(17) 0.3932(10) 0.7680(11) 0.059(5) Uani 1 1 d . . . . . C23 C 0.920(2) 0.4050(12) 0.8563(12) 0.073(6) Uani 1 1 d . . . . . C24 C 0.835(2) 0.3918(12) 0.8986(11) 0.071(6) Uani 1 1 d . . . . . C25 C 0.7460(19) 0.3678(11) 0.8523(12) 0.070(6) Uani 1 1 d . . . . . C26 C 0.7412(15) 0.3557(10) 0.7633(11) 0.053(4) Uani 1 1 d . . . . . C27 C 0.8130(12) -0.0436(9) 0.3129(9) 0.044(3) Uani 1 1 d . . . . . C28 C 0.8966(12) -0.0878(9) 0.3202(9) 0.045(3) Uani 1 1 d . . . . . C29 C 0.8928(15) -0.1831(10) 0.2922(10) 0.054(4) Uani 1 1 d . . . . . C30 C 0.8048(16) -0.2329(9) 0.2604(11) 0.059(4) Uani 1 1 d . . . . . C31 C 0.7187(14) -0.1900(10) 0.2549(12) 0.053(4) Uani 1 1 d . . . . . C32 C 0.7266(13) -0.0967(10) 0.2827(10) 0.049(3) Uani 1 1 d . . . . . C33 C 0.8197(16) 0.2032(10) 0.0539(10) 0.056(4) Uani 1 1 d . . . . . C34 C 0.7328(16) 0.1929(12) 0.0062(12) 0.062(4) Uani 1 1 d . . . . . C35 C 0.7324(18) 0.1721(13) -0.0879(13) 0.070(5) Uani 1 1 d . . . . . C36 C 0.8202(19) 0.1581(11) -0.1334(11) 0.069(6) Uani 1 1 d . . . . . C37 C 0.907(2) 0.165(2) -0.0874(16) 0.096(8) Uani 1 1 d . . . . . C38 C 0.908(2) 0.188(2) 0.0056(16) 0.093(8) Uani 1 1 d . . . . . C39 C 0.8025(12) 0.6155(9) 0.4540(9) 0.043(3) Uani 1 1 d . . . . . C40 C 0.8820(12) 0.6794(9) 0.4776(9) 0.044(3) Uani 1 1 d . . . . . C41 C 0.8699(12) 0.7692(9) 0.4910(9) 0.046(3) Uani 1 1 d . . . . . C42 C 0.7763(13) 0.7939(10) 0.4781(10) 0.049(3) Uani 1 1 d . . . . . C43 C 0.6951(13) 0.7352(11) 0.4553(11) 0.053(4) Uani 1 1 d . . . . . C44 C 0.7114(13) 0.6444(9) 0.4446(11) 0.050(3) Uani 1 1 d . . . . . Os1 Os 0.6320(2) 0.6070(3) 0.6956(3) 0.0300(4) Uani 0.5 1 d D U P A 1 N5 N 0.531(2) 0.6886(13) 0.6651(16) 0.038(3) Uani 0.5 1 d D U P A 1 C45 C 0.540(2) 0.7830(14) 0.7118(17) 0.043(3) Uani 0.5 1 d D U P A 1 H45 H 0.587754 0.810436 0.760754 0.052 Uiso 0.5 1 calc R U P A 1 C46 C 0.482(2) 0.8380(15) 0.6900(18) 0.045(3) Uani 0.5 1 d D U P A 1 H46 H 0.484357 0.902557 0.728179 0.054 Uiso 0.5 1 calc R U P A 1 C47 C 0.420(2) 0.8010(16) 0.6126(18) 0.046(4) Uani 0.5 1 d D U P A 1 H47 H 0.385460 0.839704 0.592991 0.055 Uiso 0.5 1 calc R U P A 1 C48 C 0.411(3) 0.7076(18) 0.566(2) 0.045(3) Uani 0.5 1 d D U P A 1 H48 H 0.366562 0.679934 0.514158 0.055 Uiso 0.5 1 calc R U P A 1 C49 C 0.468(2) 0.6528(16) 0.5927(17) 0.041(3) Uani 0.5 1 d D U P A 1 H49 H 0.461059 0.587649 0.558746 0.050 Uiso 0.5 1 calc R U P A 1 N6 N 0.5187(18) 0.5622(15) 0.7637(16) 0.048(4) Uani 0.5 1 d D U P A 1 C50 C 0.472(2) 0.6227(16) 0.8409(18) 0.050(4) Uani 0.5 1 d D U P A 1 H50 H 0.487374 0.687009 0.863901 0.061 Uiso 0.5 1 calc R U P A 1 C51 C 0.404(2) 0.5925(16) 0.8851(19) 0.052(3) Uani 0.5 1 d D U P A 1 H51 H 0.370728 0.635982 0.936988 0.063 Uiso 0.5 1 calc R U P A 1 C52 C 0.383(2) 0.4990(16) 0.856(2) 0.052(4) Uani 0.5 1 d D U P A 1 H52 H 0.335008 0.477927 0.886420 0.062 Uiso 0.5 1 calc R U P A 1 C53 C 0.432(2) 0.4379(16) 0.781(2) 0.053(4) Uani 0.5 1 d D U P A 1 H53 H 0.419886 0.373317 0.759407 0.064 Uiso 0.5 1 calc R U P A 1 C54 C 0.502(3) 0.4720(15) 0.738(2) 0.052(4) Uani 0.5 1 d D U P A 1 H54 H 0.538656 0.429300 0.688706 0.063 Uiso 0.5 1 calc R U P A 1 Os1B Os 0.6510(2) 0.6012(3) 0.7024(3) 0.0300(4) Uani 0.5 1 d D U P A 2 N5B N 0.543(2) 0.6790(14) 0.6720(15) 0.039(3) Uani 0.5 1 d D U P A 2 C45B C 0.508(2) 0.7610(17) 0.7371(17) 0.048(4) Uani 0.5 1 d D U P A 2 H45B H 0.532359 0.782857 0.798675 0.058 Uiso 0.5 1 calc R U P A 2 C46B C 0.442(2) 0.8120(18) 0.7175(17) 0.052(4) Uani 0.5 1 d D U P A 2 H46B H 0.421576 0.868417 0.764876 0.063 Uiso 0.5 1 calc R U P A 2 C47B C 0.405(2) 0.7823(18) 0.6284(17) 0.047(4) Uani 0.5 1 d D U P A 2 H47B H 0.363141 0.819550 0.612391 0.056 Uiso 0.5 1 calc R U P A 2 C48B C 0.431(3) 0.6973(19) 0.5649(18) 0.044(3) Uani 0.5 1 d D U P A 2 H48B H 0.406092 0.673361 0.503540 0.053 Uiso 0.5 1 calc R U P A 2 C49B C 0.495(2) 0.6457(17) 0.5903(16) 0.041(3) Uani 0.5 1 d D U P A 2 H49B H 0.505372 0.583766 0.547511 0.050 Uiso 0.5 1 calc R U P A 2 N6B N 0.544(2) 0.5722(15) 0.7890(15) 0.050(4) Uani 0.5 1 d D U P A 2 C50B C 0.534(2) 0.6324(17) 0.8806(16) 0.053(4) Uani 0.5 1 d D U P A 2 H50B H 0.565018 0.692233 0.902371 0.063 Uiso 0.5 1 calc R U P A 2 C51B C 0.482(2) 0.6113(17) 0.9413(17) 0.055(4) Uani 0.5 1 d D U P A 2 H51B H 0.475220 0.656467 1.002955 0.066 Uiso 0.5 1 calc R U P A 2 C52B C 0.438(3) 0.5240(18) 0.9133(18) 0.057(4) Uani 0.5 1 d D U P A 2 H52B H 0.402991 0.507214 0.955385 0.068 Uiso 0.5 1 calc R U P A 2 C53B C 0.446(3) 0.4625(18) 0.8229(19) 0.056(4) Uani 0.5 1 d D U P A 2 H53B H 0.413622 0.403077 0.800287 0.067 Uiso 0.5 1 calc R U P A 2 C54B C 0.503(3) 0.4874(17) 0.7644(19) 0.053(4) Uani 0.5 1 d D U P A 2 H54B H 0.512826 0.441812 0.703476 0.064 Uiso 0.5 1 calc R U P A 2 N1 N 0.8201(7) 0.4112(7) 0.5079(7) 0.037(2) Uani 1 1 d . . . . . N2 N 0.8228(9) 0.2131(7) 0.4640(7) 0.040(2) Uani 1 1 d . . . . . H2A H 0.823856 0.244412 0.430989 0.047 Uiso 1 1 calc R U . . . N3 N 0.8163(9) 0.1673(7) 0.2695(7) 0.042(2) Uani 1 1 d . . . . . N4 N 0.8166(10) 0.3590(7) 0.3088(8) 0.044(3) Uani 1 1 d . . . . . H4 H 0.819357 0.327758 0.341676 0.053 Uiso 1 1 calc R U . . . O1 O 0.7468(7) 0.6345(6) 0.6317(7) 0.041(2) Uani 1 1 d . . . . . O2 O 0.7411(8) 0.5344(6) 0.7250(5) 0.040(2) Uani 1 1 d . . . . . O3 O 0.5857(8) 0.5123(6) 0.6059(8) 0.054(2) Uani 1 1 d . . . . . O4 O 0.6637(8) 0.7046(6) 0.8015(6) 0.049(2) Uani 1 1 d . . . . . F1 F 0.6527(8) 0.3287(7) 0.7168(8) 0.064(3) Uani 1 1 d . . . . . F2 F 0.6626(13) 0.3575(9) 0.8941(8) 0.093(4) Uani 1 1 d . . . . . F3 F 0.8359(15) 0.4061(9) 0.9872(7) 0.104(5) Uani 1 1 d . . . . . F4 F 1.0104(13) 0.4295(8) 0.9019(9) 0.095(5) Uani 1 1 d . . . . . F5 F 0.9984(8) 0.4051(6) 0.7280(7) 0.061(2) Uani 1 1 d . . . . . F6 F 0.9845(8) -0.0421(6) 0.3485(7) 0.059(2) Uani 1 1 d . . . . . F7 F 0.9752(10) -0.2241(7) 0.2966(8) 0.075(3) Uani 1 1 d . . . . . F8 F 0.7993(10) -0.3241(6) 0.2363(7) 0.069(3) Uani 1 1 d . . . . . F9 F 0.6325(10) -0.2396(7) 0.2244(9) 0.078(3) Uani 1 1 d . . . . . F10 F 0.6430(9) -0.0566(7) 0.2730(9) 0.073(3) Uani 1 1 d . . . . . F11 F 0.6438(10) 0.2046(12) 0.0488(8) 0.097(5) Uani 1 1 d . . . . . F12 F 0.6444(13) 0.1651(14) -0.1304(10) 0.125(6) Uani 1 1 d . . . . . F13 F 0.8180(13) 0.1373(8) -0.2229(7) 0.086(4) Uani 1 1 d . . . . . F14 F 0.9908(15) 0.148(2) -0.1357(11) 0.159(10) Uani 1 1 d . . . . . F15 F 0.9930(14) 0.190(2) 0.0471(12) 0.175(12) Uani 1 1 d . . . . . F16 F 0.9739(7) 0.6558(6) 0.4908(6) 0.0477(18) Uani 1 1 d . . . . . F17 F 0.9485(8) 0.8293(6) 0.5129(7) 0.058(2) Uani 1 1 d . . . . . F18 F 0.7652(8) 0.8811(6) 0.4902(7) 0.059(2) Uani 1 1 d . . . . . F19 F 0.6073(9) 0.7596(8) 0.4462(11) 0.085(4) Uani 1 1 d . . . . . F20 F 0.6303(7) 0.5849(7) 0.4221(8) 0.064(3) Uani 1 1 d . . . . . C55 C 1.1750(12) 0.1568(10) 0.2396(12) 0.061(4) Uani 1 1 d D . . . . H55 H 1.215713 0.215459 0.256448 0.073 Uiso 1 1 calc R U . . . Cl1 Cl 1.0543(4) 0.1836(4) 0.2825(4) 0.0766(12) Uani 1 1 d D . . . . Cl2 Cl 1.2354(6) 0.0898(5) 0.2821(4) 0.105(2) Uani 1 1 d D . . . . Cl3 Cl 1.1688(11) 0.0967(11) 0.1218(4) 0.213(8) Uani 1 1 d D . . . . C56 C 0.809(2) 0.6612(15) 0.940(2) 0.080(5) Uani 0.5 1 d D U P B 1 H56 H 0.772199 0.637162 0.879626 0.096 Uiso 0.5 1 calc R U P B 1 Cl4 Cl 0.7950(10) 0.7799(6) 0.9960(8) 0.088(3) Uani 0.5 1 d D U P B 1 Cl5 Cl 0.7577(11) 0.6069(8) 1.0020(9) 0.090(3) Uani 0.5 1 d D U P B 1 Cl6 Cl 0.9345(8) 0.6354(6) 0.9168(8) 0.082(3) Uani 0.5 1 d D U P B 1 C56B C 0.7364(19) 0.6586(14) 0.957(2) 0.077(5) Uani 0.5 1 d D U P C 2 H56B H 0.739958 0.647572 0.891565 0.093 Uiso 0.5 1 calc R U P C 2 Cl4B Cl 0.7069(11) 0.7742(6) 1.0242(6) 0.083(3) Uani 0.5 1 d D U P C 2 Cl5B Cl 0.6457(8) 0.5833(6) 0.9658(6) 0.067(2) Uani 0.5 1 d D U P C 2 Cl6B Cl 0.8526(9) 0.6358(8) 0.9906(9) 0.089(3) Uani 0.5 1 d D U P C 2 C57 C 0.541(3) 1.006(3) 1.042(2) 0.148(10) Uani 0.5 1 d D U P D -1 H57 H 0.583256 1.059624 1.085906 0.177 Uiso 0.5 1 calc R U P D -1 Cl7 Cl 0.5447(18) 0.9214(16) 1.0823(15) 0.161(8) Uani 0.5 1 d D U P D -1 Cl8 Cl 0.588(2) 0.9760(18) 0.9338(16) 0.148(9) Uani 0.5 1 d D U P D -1 Cl9 Cl 0.420(2) 1.044(2) 1.047(2) 0.149(10) Uani 0.5 1 d D U P D -1 C58 C 0.590(5) 0.998(6) 0.618(4) 0.144(17) Uani 0.5 1 d D U P E -1 H58A H 0.648019 1.041408 0.642598 0.216 Uiso 0.5 1 calc R U P E -1 H58B H 0.539405 1.012309 0.665801 0.216 Uiso 0.5 1 calc R U P E -1 H58C H 0.611567 0.934950 0.598983 0.216 Uiso 0.5 1 calc R U P E -1 C59 C 0.545(5) 1.007(4) 0.536(3) 0.134(13) Uani 0.5 1 d D U P E -1 H59A H 0.596690 0.993020 0.487993 0.161 Uiso 0.5 1 calc R U P E -1 H59B H 0.524396 1.070520 0.554934 0.161 Uiso 0.5 1 calc R U P E -1 C60 C 0.454(4) 0.939(4) 0.497(3) 0.128(12) Uani 0.5 1 d D U P E -1 H60A H 0.453579 0.893212 0.521914 0.154 Uiso 0.5 1 calc R U P E -1 H60B H 0.391646 0.973187 0.514509 0.154 Uiso 0.5 1 calc R U P E -1 C61 C 0.460(4) 0.890(3) 0.393(3) 0.133(12) Uani 0.5 1 d D U P E -1 H61A H 0.529749 0.897398 0.374278 0.159 Uiso 0.5 1 calc R U P E -1 H61B H 0.444494 0.823681 0.371582 0.159 Uiso 0.5 1 calc R U P E -1 C62 C 0.389(4) 0.928(4) 0.346(4) 0.133(13) Uani 0.5 1 d D U P E -1 H62A H 0.323174 0.935134 0.376122 0.160 Uiso 0.5 1 calc R U P E -1 H62B H 0.379953 0.882437 0.281207 0.160 Uiso 0.5 1 calc R U P E -1 C63 C 0.427(5) 1.020(4) 0.351(4) 0.142(17) Uani 0.5 1 d D U P E -1 H63A H 0.377789 1.041510 0.319760 0.213 Uiso 0.5 1 calc R U P E -1 H63B H 0.434628 1.065686 0.415221 0.213 Uiso 0.5 1 calc R U P E -1 H63C H 0.491420 1.012979 0.320286 0.213 Uiso 0.5 1 calc R U P E -1 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 C1 0.033(6) 0.028(5) 0.044(7) 0.008(5) 0.007(5) 0.004(4) C2 0.035(6) 0.024(5) 0.036(6) 0.002(4) 0.003(5) -0.004(4) C3 0.045(7) 0.027(5) 0.038(6) 0.005(5) -0.003(5) 0.000(5) C4 0.036(6) 0.029(5) 0.036(6) 0.002(5) 0.001(5) -0.001(4) C5 0.057(8) 0.027(5) 0.025(5) 0.006(4) 0.005(5) 0.005(5) C6 0.053(7) 0.027(6) 0.031(6) 0.004(5) 0.001(5) 0.000(5) C7 0.070(9) 0.032(6) 0.033(6) 0.011(5) 0.002(6) 0.006(6) C8 0.086(11) 0.021(5) 0.035(6) 0.011(5) 0.004(6) 0.004(6) C9 0.059(8) 0.024(5) 0.033(6) 0.003(5) 0.000(5) -0.002(5) C10 0.056(8) 0.025(5) 0.036(6) 0.006(5) -0.001(5) -0.003(5) C11 0.057(8) 0.029(6) 0.038(7) 0.007(5) -0.001(6) -0.003(5) C12 0.092(12) 0.028(6) 0.034(7) 0.003(5) 0.003(7) -0.004(7) C13 0.100(13) 0.030(6) 0.029(6) 0.002(5) 0.000(7) -0.006(7) C14 0.057(8) 0.030(6) 0.038(7) -0.001(5) 0.002(6) 0.001(5) C15 0.071(9) 0.039(7) 0.034(6) 0.011(6) 0.009(6) 0.008(6) C16 0.076(10) 0.038(7) 0.035(7) 0.008(5) 0.017(6) 0.017(6) C17 0.104(14) 0.046(8) 0.044(8) 0.017(7) 0.031(9) 0.026(9) C18 0.096(13) 0.032(7) 0.049(8) 0.011(6) 0.021(8) 0.019(7) C19 0.062(8) 0.025(5) 0.044(7) 0.012(5) 0.017(6) 0.011(5) C20 0.046(6) 0.025(5) 0.038(6) 0.010(5) 0.010(5) 0.004(4) C21 0.070(9) 0.023(5) 0.036(7) 0.004(5) 0.009(6) 0.016(6) C22 0.107(15) 0.024(6) 0.040(8) 0.009(6) -0.014(8) 0.000(7) C23 0.131(18) 0.035(8) 0.039(8) 0.002(6) -0.013(10) 0.013(9) C24 0.140(19) 0.043(8) 0.028(7) 0.012(6) -0.005(9) 0.021(10) C25 0.128(18) 0.035(7) 0.046(9) 0.013(7) 0.030(10) 0.031(9) C26 0.084(12) 0.037(7) 0.038(7) 0.015(6) 0.009(7) 0.020(7) C27 0.071(9) 0.029(6) 0.027(6) 0.007(5) 0.004(6) 0.010(6) C28 0.070(9) 0.026(6) 0.028(6) 0.002(5) 0.001(5) 0.002(6) C29 0.098(13) 0.028(6) 0.034(7) 0.010(5) 0.009(7) 0.016(7) C30 0.108(14) 0.017(5) 0.042(8) 0.005(5) 0.004(8) -0.002(7) C31 0.079(11) 0.031(6) 0.052(8) 0.022(6) -0.011(7) -0.009(7) C32 0.066(9) 0.029(6) 0.044(7) 0.009(6) -0.004(6) -0.002(6) C33 0.100(13) 0.035(7) 0.031(7) 0.010(6) 0.008(7) 0.014(7) C34 0.089(13) 0.046(8) 0.042(8) 0.010(7) 0.011(8) 0.000(8) C35 0.104(15) 0.046(9) 0.044(9) 0.005(7) 0.002(9) 0.003(9) C36 0.134(18) 0.034(7) 0.033(7) 0.008(6) 0.016(9) 0.019(9) C37 0.12(2) 0.12(2) 0.056(12) 0.040(13) 0.027(13) 0.031(16) C38 0.120(19) 0.12(2) 0.063(12) 0.064(14) 0.039(13) 0.052(16) C39 0.062(8) 0.028(6) 0.037(6) 0.012(5) 0.010(6) 0.007(5) C40 0.060(8) 0.031(6) 0.031(6) 0.006(5) 0.003(5) 0.003(6) C41 0.071(9) 0.023(5) 0.036(6) 0.005(5) 0.006(6) 0.001(5) C42 0.066(9) 0.039(7) 0.043(7) 0.019(6) 0.012(6) 0.012(6) C43 0.068(10) 0.040(7) 0.044(8) 0.011(6) 0.013(7) 0.015(7) C44 0.065(9) 0.027(6) 0.050(8) 0.011(6) 0.013(7) 0.001(6) Os1 0.0360(10) 0.0221(4) 0.0241(5) 0.0029(3) -0.0021(6) 0.0041(6) N5 0.041(6) 0.028(5) 0.033(5) 0.003(4) 0.001(5) 0.009(5) C45 0.049(6) 0.031(6) 0.038(6) 0.004(5) 0.000(5) 0.003(5) C46 0.051(7) 0.033(6) 0.042(6) 0.008(5) -0.001(5) 0.004(5) C47 0.051(7) 0.035(6) 0.042(6) 0.009(5) -0.003(5) 0.007(5) C48 0.048(7) 0.036(6) 0.040(5) 0.005(5) -0.003(5) 0.007(5) C49 0.045(7) 0.030(5) 0.035(5) 0.002(4) -0.003(5) 0.009(5) N6 0.055(7) 0.039(6) 0.047(7) 0.016(6) 0.012(6) 0.006(5) C50 0.057(7) 0.043(6) 0.048(7) 0.017(6) 0.012(6) 0.005(6) C51 0.060(6) 0.045(6) 0.050(7) 0.020(6) 0.013(6) 0.003(5) C52 0.061(7) 0.044(7) 0.051(7) 0.021(6) 0.012(6) 0.001(6) C53 0.060(7) 0.043(6) 0.052(7) 0.017(6) 0.011(6) 0.000(6) C54 0.057(6) 0.041(6) 0.052(8) 0.015(6) 0.011(6) 0.002(5) Os1B 0.0360(10) 0.0221(4) 0.0241(5) 0.0029(3) -0.0021(6) 0.0041(6) N5B 0.042(5) 0.030(5) 0.031(5) 0.001(4) -0.003(4) 0.007(4) C45B 0.050(6) 0.036(6) 0.041(6) -0.001(5) -0.001(5) 0.009(5) C46B 0.054(6) 0.040(6) 0.044(6) 0.001(5) -0.001(5) 0.007(5) C47B 0.051(7) 0.037(6) 0.042(6) 0.007(5) -0.003(5) 0.008(5) C48B 0.047(7) 0.034(6) 0.039(5) 0.006(5) -0.005(5) 0.009(5) C49B 0.044(7) 0.031(5) 0.035(5) 0.002(5) -0.002(5) 0.008(5) N6B 0.056(7) 0.040(6) 0.050(7) 0.016(6) 0.013(6) 0.005(5) C50B 0.058(7) 0.044(6) 0.051(7) 0.016(6) 0.014(6) 0.003(6) C51B 0.060(7) 0.048(7) 0.051(7) 0.015(6) 0.015(6) 0.003(6) C52B 0.062(7) 0.048(6) 0.054(7) 0.016(6) 0.014(6) 0.000(6) C53B 0.061(6) 0.046(6) 0.054(7) 0.016(6) 0.012(6) 0.000(5) C54B 0.057(6) 0.043(6) 0.052(8) 0.014(6) 0.010(6) 0.003(5) N1 0.040(5) 0.028(5) 0.041(6) 0.012(4) 0.005(4) 0.003(4) N2 0.060(7) 0.025(5) 0.028(5) 0.006(4) -0.003(4) -0.002(4) N3 0.056(6) 0.028(5) 0.031(5) 0.005(4) 0.001(4) -0.003(4) N4 0.070(8) 0.027(5) 0.030(5) 0.009(4) 0.011(5) 0.006(5) O1 0.053(5) 0.026(4) 0.042(5) 0.013(4) 0.006(4) 0.007(4) O2 0.063(6) 0.030(4) 0.017(3) 0.003(3) 0.003(3) 0.001(4) O3 0.060(6) 0.025(4) 0.054(6) -0.004(4) -0.014(5) -0.005(4) O4 0.085(7) 0.028(4) 0.029(4) 0.009(3) -0.004(4) -0.003(4) F1 0.076(7) 0.053(5) 0.065(6) 0.026(5) 0.024(5) 0.017(5) F2 0.163(13) 0.061(7) 0.057(7) 0.024(6) 0.047(8) 0.035(8) F3 0.220(17) 0.064(7) 0.027(5) 0.019(5) -0.003(7) 0.026(9) F4 0.155(13) 0.055(6) 0.060(7) 0.011(5) -0.053(8) 0.000(7) F5 0.080(7) 0.041(5) 0.056(5) 0.014(4) -0.022(5) -0.002(4) F6 0.071(6) 0.038(4) 0.051(5) 0.002(4) -0.002(4) 0.003(4) F7 0.100(8) 0.042(5) 0.070(7) 0.011(5) 0.008(6) 0.026(5) F8 0.124(9) 0.019(4) 0.055(5) 0.008(4) 0.002(5) 0.001(4) F9 0.101(8) 0.035(5) 0.087(8) 0.018(5) -0.020(6) -0.023(5) F10 0.083(7) 0.042(5) 0.088(8) 0.024(5) -0.024(6) -0.012(5) F11 0.075(7) 0.136(12) 0.043(6) 0.004(6) 0.010(5) 0.007(8) F12 0.118(12) 0.151(16) 0.053(7) -0.002(8) -0.024(8) -0.001(11) F13 0.169(13) 0.052(6) 0.033(5) 0.013(4) 0.007(6) 0.016(7) F14 0.120(13) 0.28(3) 0.065(9) 0.069(14) 0.021(9) 0.027(16) F15 0.103(12) 0.37(4) 0.079(10) 0.123(18) 0.038(9) 0.075(17) F16 0.052(5) 0.041(4) 0.044(4) 0.013(4) 0.005(3) 0.004(3) F17 0.071(6) 0.035(4) 0.054(5) 0.006(4) 0.005(4) -0.002(4) F18 0.085(7) 0.032(4) 0.058(5) 0.018(4) 0.012(5) 0.011(4) F19 0.077(7) 0.071(7) 0.143(12) 0.077(8) 0.045(7) 0.041(6) F20 0.050(5) 0.052(5) 0.095(8) 0.037(5) 0.009(5) 0.003(4) C55 0.068(10) 0.042(8) 0.060(10) 0.010(7) 0.018(8) 0.001(7) Cl1 0.075(3) 0.074(3) 0.063(3) 0.013(2) 0.018(2) 0.007(2) Cl2 0.127(5) 0.103(5) 0.071(3) 0.021(3) 0.022(3) 0.050(4) Cl3 0.254(13) 0.276(15) 0.038(3) -0.011(5) 0.007(5) 0.168(12) C56 0.110(9) 0.048(7) 0.070(8) 0.014(7) -0.012(8) 0.008(8) Cl4 0.112(7) 0.040(4) 0.078(6) -0.006(4) -0.034(6) 0.013(5) Cl5 0.118(7) 0.062(5) 0.075(6) 0.016(4) 0.019(5) 0.021(5) Cl6 0.083(6) 0.045(4) 0.092(7) 0.007(4) -0.013(5) 0.007(4) C56B 0.114(8) 0.046(7) 0.064(7) 0.016(7) -0.015(8) 0.005(8) Cl4B 0.157(9) 0.037(4) 0.047(4) 0.010(3) -0.014(5) -0.003(5) Cl5B 0.107(6) 0.042(4) 0.054(4) 0.024(3) -0.005(4) -0.003(4) Cl6B 0.105(7) 0.064(5) 0.090(6) 0.026(5) -0.037(5) -0.008(5) C57 0.163(14) 0.128(15) 0.101(14) 0.005(13) -0.017(13) -0.025(14) Cl7 0.163(14) 0.151(15) 0.123(13) 0.022(11) -0.039(11) -0.049(12) Cl8 0.177(15) 0.110(12) 0.082(11) -0.022(9) 0.026(10) -0.067(11) Cl9 0.149(15) 0.137(17) 0.111(14) 0.005(11) -0.044(13) 0.037(13) C58 0.12(3) 0.16(3) 0.14(3) 0.05(3) 0.03(2) 0.04(3) C59 0.11(2) 0.15(3) 0.14(3) 0.06(2) 0.031(19) 0.04(2) C60 0.105(19) 0.15(3) 0.14(3) 0.07(2) 0.033(18) 0.038(19) C61 0.106(19) 0.15(3) 0.15(3) 0.07(2) 0.035(18) 0.033(19) C62 0.11(2) 0.15(3) 0.15(3) 0.07(2) 0.036(19) 0.03(2) C63 0.11(2) 0.16(3) 0.15(3) 0.06(3) 0.04(2) 0.03(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Os Os -1.2165 7.6030 '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 N1 C1 C20 125.4(12) N1 C1 C2 112.3(11) C20 C1 C2 122.3(11) O1 C2 C3 113.4(11) O1 C2 C1 111.9(11) C3 C2 C1 102.9(10) O1 C2 H2 109.5 C3 C2 H2 109.5 C1 C2 H2 109.5 O2 C3 C2 113.4(11) O2 C3 C4 110.2(10) C2 C3 C4 102.9(11) O2 C3 H3 110.1 C2 C3 H3 110.1 C4 C3 H3 110.1 N1 C4 C5 125.4(11) N1 C4 C3 113.2(11) C5 C4 C3 121.4(12) C4 C5 C6 127.8(12) C4 C5 C21 118.3(11) C6 C5 C21 113.8(11) N2 C6 C5 125.8(12) N2 C6 C7 107.5(11) C5 C6 C7 126.7(12) C8 C7 C6 107.7(12) C8 C7 H7 126.2 C6 C7 H7 126.2 C7 C8 C9 108.2(11) C7 C8 H8 125.9 C9 C8 H8 125.9 N2 C9 C10 125.5(13) N2 C9 C8 107.1(11) C10 C9 C8 127.4(12) C9 C10 C11 126.4(12) C9 C10 C27 116.8(12) C11 C10 C27 116.8(11) N3 C11 C10 125.1(12) N3 C11 C12 111.1(12) C10 C11 C12 123.8(12) C13 C12 C11 106.7(13) C13 C12 H12 126.7 C11 C12 H12 126.7 C12 C13 C14 106.8(13) C12 C13 H13 126.6 C14 C13 H13 126.6 N3 C14 C15 126.3(12) N3 C14 C13 110.1(13) C15 C14 C13 123.6(14) C14 C15 C16 126.6(14) C14 C15 C33 118.7(13) C16 C15 C33 114.7(13) C17 C16 C15 128.8(14) C17 C16 N4 107.4(13) C15 C16 N4 123.7(14) C18 C17 C16 109.2(15) C18 C17 H17 125.4 C16 C17 H17 125.4 C17 C18 C19 107.0(13) C17 C18 H18 126.5 C19 C18 H18 126.5 N4 C19 C18 108.6(12) N4 C19 C20 125.5(12) C18 C19 C20 125.8(12) C1 C20 C19 127.4(11) C1 C20 C39 118.7(11) C19 C20 C39 113.9(11) C22 C21 C26 116.0(15) C22 C21 C5 121.4(15) C26 C21 C5 122.5(15) F5 C22 C23 117.9(19) F5 C22 C21 119.3(14) C23 C22 C21 123(2) C22 C23 F4 120(2) C22 C23 C24 119(2) F4 C23 C24 121.1(17) F3 C24 C25 118(2) F3 C24 C23 122(2) C25 C24 C23 120.2(16) F2 C25 C24 120.1(18) F2 C25 C26 120(2) C24 C25 C26 120(2) F1 C26 C25 119.0(18) F1 C26 C21 118.6(14) C25 C26 C21 122.4(19) C32 C27 C28 116.4(13) C32 C27 C10 122.4(14) C28 C27 C10 121.2(14) F6 C28 C27 120.9(12) F6 C28 C29 118.2(15) C27 C28 C29 120.8(15) F7 C29 C30 120.6(14) F7 C29 C28 119.3(17) C30 C29 C28 120.1(16) F8 C30 C29 120.6(17) F8 C30 C31 118.9(16) C29 C30 C31 120.5(13) F9 C31 C32 123.0(16) F9 C31 C30 119.8(13) C32 C31 C30 117.2(15) F10 C32 C27 118.5(13) F10 C32 C31 116.3(14) C27 C32 C31 125.0(16) C34 C33 C38 117.5(17) C34 C33 C15 120.0(17) C38 C33 C15 122.5(19) F11 C34 C33 120.3(16) F11 C34 C35 118.1(19) C33 C34 C35 121.6(19) F12 C35 C36 121.7(19) F12 C35 C34 119(2) C36 C35 C34 120(2) F13 C36 C37 122(2) F13 C36 C35 119(2) C37 C36 C35 119.4(18) F14 C37 C36 117(2) F14 C37 C38 122(3) C36 C37 C38 121(2) F15 C38 C37 120(2) F15 C38 C33 119.6(18) C37 C38 C33 121(3) C44 C39 C40 117.0(13) C44 C39 C20 119.8(13) C40 C39 C20 123.2(13) F16 C40 C39 119.9(13) F16 C40 C41 118.0(13) C39 C40 C41 122.1(14) F17 C41 C42 120.9(13) F17 C41 C40 120.7(14) C42 C41 C40 118.3(14) F18 C42 C43 119.1(15) F18 C42 C41 118.1(14) C43 C42 C41 122.8(14) F19 C43 C42 122.5(15) F19 C43 C44 121.0(16) C42 C43 C44 116.5(15) C39 C44 F20 119.7(13) C39 C44 C43 123.2(15) F20 C44 C43 117.1(15) O3 Os1 O4 170.2(6) O3 Os1 O1 97.4(5) O4 Os1 O1 92.3(5) O3 Os1 O2 92.7(5) O4 Os1 O2 89.0(4) O1 Os1 O2 81.2(4) O3 Os1 N5 90.1(7) O4 Os1 N5 88.9(7) O1 Os1 N5 94.4(9) O2 Os1 N5 175.0(9) O3 Os1 N6 80.2(8) O4 Os1 N6 90.1(7) O1 Os1 N6 172.5(7) O2 Os1 N6 91.8(8) N5 Os1 N6 92.7(9) C49 N5 C45 117.1(16) C49 N5 Os1 122.4(13) C45 N5 Os1 119.8(14) C46 C45 N5 121.9(18) C46 C45 H45 119.0 N5 C45 H45 119.0 C45 C46 C47 120.5(18) C45 C46 H46 119.7 C47 C46 H46 119.7 C48 C47 C46 117.9(19) C48 C47 H47 121.0 C46 C47 H47 121.0 C47 C48 C49 119.8(18) C47 C48 H48 120.1 C49 C48 H48 120.1 N5 C49 C48 122.3(17) N5 C49 H49 118.8 C48 C49 H49 118.8 C54 N6 C50 117.5(16) C54 N6 Os1 119.6(14) C50 N6 Os1 122.3(14) C51 C50 N6 121.2(19) C51 C50 H50 119.4 N6 C50 H50 119.4 C50 C51 C52 120.9(19) C50 C51 H51 119.6 C52 C51 H51 119.6 C53 C52 C51 118.4(18) C53 C52 H52 120.8 C51 C52 H52 120.8 C52 C53 C54 118.7(19) C52 C53 H53 120.6 C54 C53 H53 120.6 N6 C54 C53 123.0(19) N6 C54 H54 118.5 C53 C54 H54 118.5 O4 Os1B O2 100.9(5) O4 Os1B O3 155.8(5) O2 Os1B O3 99.9(5) O4 Os1B O1 95.9(5) O2 Os1B O1 91.0(4) O3 Os1B O1 96.0(5) O4 Os1B N5B 80.4(7) O2 Os1B N5B 178.7(7) O3 Os1B N5B 78.9(7) O1 Os1B N5B 88.6(10) O4 Os1B N6B 80.5(7) O2 Os1B N6B 89.9(9) O3 Os1B N6B 87.2(8) O1 Os1B N6B 176.4(7) N5B Os1B N6B 90.6(9) C49B N5B C45B 115.0(16) C49B N5B Os1B 121.7(13) C45B N5B Os1B 122.9(14) C46B C45B N5B 123.1(18) C46B C45B H45B 118.4 N5B C45B H45B 118.4 C45B C46B C47B 120.4(18) C45B C46B H46B 119.8 C47B C46B H46B 119.8 C48B C47B C46B 117.2(19) C48B C47B H47B 121.4 C46B C47B H47B 121.4 C47B C48B C49B 119.8(18) C47B C48B H48B 120.1 C49B C48B H48B 120.1 N5B C49B C48B 123.3(17) N5B C49B H49B 118.3 C48B C49B H49B 118.3 C54B N6B C50B 114.6(16) C54B N6B Os1B 121.9(14) C50B N6B Os1B 121.7(14) C51B C50B N6B 124.1(19) C51B C50B H50B 118.0 N6B C50B H50B 118.0 C50B C51B C52B 119.9(19) C50B C51B H51B 120.0 C52B C51B H51B 120.0 C53B C52B C51B 117.7(19) C53B C52B H52B 121.1 C51B C52B H52B 121.1 C52B C53B C54B 120(2) C52B C53B H53B 120.2 C54B C53B H53B 120.2 N6B C54B C53B 123.8(19) N6B C54B H54B 118.1 C53B C54B H54B 118.1 C4 N1 C1 108.7(10) C6 N2 C9 109.5(11) C6 N2 H2A 125.2 C9 N2 H2A 125.2 C11 N3 C14 105.2(10) C19 N4 C16 107.7(12) C19 N4 H4 126.2 C16 N4 H4 126.2 C2 O1 Os1B 107.5(7) C2 O1 Os1 115.1(7) C3 O2 Os1B 112.0(8) C3 O2 Os1 112.6(8) Cl3 C55 Cl2 107.8(9) Cl3 C55 Cl1 109.7(10) Cl2 C55 Cl1 112.7(10) Cl3 C55 H55 108.9 Cl2 C55 H55 108.9 Cl1 C55 H55 108.9 Cl5 C56 Cl6 111.1(15) Cl5 C56 Cl4 111.1(15) Cl6 C56 Cl4 111.4(15) Cl5 C56 H56 107.7 Cl6 C56 H56 107.7 Cl4 C56 H56 107.7 Cl5B C56B Cl6B 109.2(14) Cl5B C56B Cl4B 111.5(15) Cl6B C56B Cl4B 110.9(15) Cl5B C56B H56B 108.4 Cl6B C56B H56B 108.4 Cl4B C56B H56B 108.4 Cl8 C57 Cl9 109.4(18) Cl8 C57 Cl7 116(2) Cl9 C57 Cl7 111(2) Cl8 C57 H57 106.7 Cl9 C57 H57 106.7 Cl7 C57 H57 106.7 C59 C58 H58A 109.5 C59 C58 H58B 109.5 H58A C58 H58B 109.5 C59 C58 H58C 109.5 H58A C58 H58C 109.5 H58B C58 H58C 109.5 C58 C59 C60 110(2) C58 C59 H59A 109.6 C60 C59 H59A 109.6 C58 C59 H59B 109.6 C60 C59 H59B 109.6 H59A C59 H59B 108.1 C61 C60 C59 109.5(19) C61 C60 H60A 109.8 C59 C60 H60A 109.8 C61 C60 H60B 109.8 C59 C60 H60B 109.8 H60A C60 H60B 108.2 C62 C61 C60 112(2) C62 C61 H61A 109.1 C60 C61 H61A 109.1 C62 C61 H61B 109.1 C60 C61 H61B 109.1 H61A C61 H61B 107.9 C61 C62 C63 113(2) C61 C62 H62A 109.1 C63 C62 H62A 109.1 C61 C62 H62B 109.1 C63 C62 H62B 109.1 H62A C62 H62B 107.8 C62 C63 H63A 109.5 C62 C63 H63B 109.5 H63A C63 H63B 109.5 C62 C63 H63C 109.5 H63A C63 H63C 109.5 H63B C63 H63C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.364(16) C1 C20 1.377(19) C1 C2 1.538(17) C2 O1 1.417(15) C2 C3 1.518(17) C2 H2 1.0000 C3 O2 1.424(16) C3 C4 1.532(16) C3 H3 1.0000 C4 N1 1.345(18) C4 C5 1.386(18) C5 C6 1.405(16) C5 C21 1.503(18) C6 N2 1.368(16) C6 C7 1.423(19) C7 C8 1.368(18) C7 H7 0.9500 C8 C9 1.417(19) C8 H8 0.9500 C9 N2 1.379(15) C9 C10 1.392(17) C10 C11 1.40(2) C10 C27 1.495(18) C11 N3 1.358(17) C11 C12 1.447(19) C12 C13 1.32(2) C12 H12 0.9500 C13 C14 1.463(18) C13 H13 0.9500 C14 N3 1.364(19) C14 C15 1.37(2) C15 C16 1.391(19) C15 C33 1.50(2) C16 C17 1.38(2) C16 N4 1.406(18) C17 C18 1.38(2) C17 H17 0.9500 C18 C19 1.41(2) C18 H18 0.9500 C19 N4 1.373(16) C19 C20 1.427(18) C20 C39 1.503(17) C21 C22 1.38(3) C21 C26 1.39(2) C22 F5 1.35(2) C22 C23 1.36(2) C23 F4 1.36(3) C23 C24 1.39(3) C24 F3 1.348(18) C24 C25 1.35(3) C25 F2 1.34(3) C25 C26 1.37(2) C26 F1 1.35(2) C27 C32 1.36(2) C27 C28 1.38(2) C28 F6 1.328(19) C28 C29 1.399(19) C29 F7 1.32(2) C29 C30 1.36(3) C30 F8 1.346(15) C30 C31 1.38(3) C31 F9 1.34(2) C31 C32 1.369(19) C32 F10 1.35(2) C33 C34 1.36(3) C33 C38 1.39(3) C34 F11 1.35(2) C34 C35 1.41(3) C35 F12 1.33(3) C35 C36 1.36(3) C36 F13 1.335(19) C36 C37 1.35(4) C37 F14 1.33(3) C37 C38 1.38(3) C38 F15 1.31(3) C39 C44 1.35(2) C39 C40 1.38(2) C40 F16 1.339(18) C40 C41 1.384(19) C41 F17 1.336(18) C41 C42 1.37(2) C42 F18 1.346(16) C42 C43 1.35(2) C43 F19 1.28(2) C43 C44 1.42(2) C44 F20 1.357(18) Os1 O3 1.677(10) Os1 O4 1.783(10) Os1 O1 1.990(10) Os1 O2 2.080(10) Os1 N5 2.115(15) Os1 N6 2.152(15) N5 C49 1.340(18) N5 C45 1.373(19) C45 C46 1.35(2) C45 H45 0.9500 C46 C47 1.38(2) C46 H46 0.9500 C47 C48 1.36(2) C47 H47 0.9500 C48 C49 1.39(2) C48 H48 0.9500 C49 H49 0.9500 N6 C54 1.338(19) N6 C50 1.37(2) C50 C51 1.36(2) C50 H50 0.9500 C51 C52 1.39(2) C51 H51 0.9500 C52 C53 1.37(2) C52 H52 0.9500 C53 C54 1.39(2) C53 H53 0.9500 C54 H54 0.9500 Os1B O4 1.738(9) Os1B O2 1.783(10) Os1B O3 1.789(10) Os1B O1 1.928(10) Os1B N5B 2.138(15) Os1B N6B 2.174(15) N5B C49B 1.338(18) N5B C45B 1.376(19) C45B C46B 1.35(2) C45B H45B 0.9500 C46B C47B 1.39(2) C46B H46B 0.9500 C47B C48B 1.36(2) C47B H47B 0.9500 C48B C49B 1.39(2) C48B H48B 0.9500 C49B H49B 0.9500 N6B C54B 1.342(19) N6B C50B 1.38(2) C50B C51B 1.36(2) C50B H50B 0.9500 C51B C52B 1.38(2) C51B H51B 0.9500 C52B C53B 1.37(2) C52B H52B 0.9500 C53B C54B 1.39(2) C53B H53B 0.9500 C54B H54B 0.9500 N2 H2A 0.8800 N4 H4 0.8800 C55 Cl3 1.719(17) C55 Cl2 1.731(18) C55 Cl1 1.745(15) C55 H55 1.0000 C56 Cl5 1.73(2) C56 Cl6 1.73(2) C56 Cl4 1.74(2) C56 H56 1.0000 C56B Cl5B 1.73(2) C56B Cl6B 1.74(2) C56B Cl4B 1.76(2) C56B H56B 1.0000 C57 Cl8 1.73(2) C57 Cl9 1.74(2) C57 Cl7 1.74(2) C57 H57 1.0000 C58 C59 1.52(2) C58 H58A 0.9800 C58 H58B 0.9800 C58 H58C 0.9800 C59 C60 1.54(2) C59 H59A 0.9900 C59 H59B 0.9900 C60 C61 1.52(2) C60 H60A 0.9900 C60 H60B 0.9900 C61 C62 1.50(2) C61 H61A 0.9900 C61 H61B 0.9900 C62 C63 1.53(2) C62 H62A 0.9900 C62 H62B 0.9900 C63 H63A 0.9800 C63 H63B 0.9800 C63 H63C 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 C1 C2 O1 -124.9(11) C20 C1 C2 O1 55.2(15) N1 C1 C2 C3 -2.9(14) C20 C1 C2 C3 177.3(12) O1 C2 C3 O2 4.7(16) C1 C2 C3 O2 -116.3(11) O1 C2 C3 C4 123.6(11) C1 C2 C3 C4 2.6(13) O2 C3 C4 N1 119.3(12) C2 C3 C4 N1 -1.9(15) O2 C3 C4 C5 -58.4(16) C2 C3 C4 C5 -179.6(12) N1 C4 C5 C6 5(2) C3 C4 C5 C6 -177.7(14) N1 C4 C5 C21 -178.9(13) C3 C4 C5 C21 -2(2) C4 C5 C6 N2 -3(2) C21 C5 C6 N2 -178.9(14) C4 C5 C6 C7 -180.0(15) C21 C5 C6 C7 4(2) N2 C6 C7 C8 -0.3(18) C5 C6 C7 C8 177.5(15) C6 C7 C8 C9 0(2) C7 C8 C9 N2 -0.2(19) C7 C8 C9 C10 -179.5(16) N2 C9 C10 C11 0(3) C8 C9 C10 C11 179.0(16) N2 C9 C10 C27 -178.4(14) C8 C9 C10 C27 1(2) C9 C10 C11 N3 -2(3) C27 C10 C11 N3 176.0(14) C9 C10 C11 C12 178.7(16) C27 C10 C11 C12 -3(2) N3 C11 C12 C13 2(2) C10 C11 C12 C13 -179.0(17) C11 C12 C13 C14 -1(2) C12 C13 C14 N3 1(2) C12 C13 C14 C15 -179.3(18) N3 C14 C15 C16 0(3) C13 C14 C15 C16 179.8(17) N3 C14 C15 C33 179.5(16) C13 C14 C15 C33 -1(3) C14 C15 C16 C17 178.2(19) C33 C15 C16 C17 -1(3) C14 C15 C16 N4 2(3) C33 C15 C16 N4 -177.9(16) C15 C16 C17 C18 178.9(19) N4 C16 C17 C18 -4(2) C16 C17 C18 C19 2(2) C17 C18 C19 N4 0(2) C17 C18 C19 C20 176.1(16) N1 C1 C20 C19 -4(2) C2 C1 C20 C19 176.3(13) N1 C1 C20 C39 173.2(12) C2 C1 C20 C39 -6.9(18) N4 C19 C20 C1 0(2) C18 C19 C20 C1 -175.3(16) N4 C19 C20 C39 -176.9(14) C18 C19 C20 C39 8(2) C4 C5 C21 C22 -78.6(17) C6 C5 C21 C22 98.1(16) C4 C5 C21 C26 106.0(16) C6 C5 C21 C26 -77.4(17) C26 C21 C22 F5 179.6(12) C5 C21 C22 F5 4(2) C26 C21 C22 C23 2(2) C5 C21 C22 C23 -174.0(14) F5 C22 C23 F4 1(2) C21 C22 C23 F4 179.0(14) F5 C22 C23 C24 -179.0(14) C21 C22 C23 C24 -1(2) C22 C23 C24 F3 -177.3(15) F4 C23 C24 F3 3(3) C22 C23 C24 C25 0(3) F4 C23 C24 C25 179.8(15) F3 C24 C25 F2 -1(2) C23 C24 C25 F2 -178.2(15) F3 C24 C25 C26 177.8(14) C23 C24 C25 C26 1(2) F2 C25 C26 F1 -3(2) C24 C25 C26 F1 177.8(14) F2 C25 C26 C21 178.9(13) C24 C25 C26 C21 0(2) C22 C21 C26 F1 -178.9(12) C5 C21 C26 F1 -3(2) C22 C21 C26 C25 -1(2) C5 C21 C26 C25 174.4(13) C9 C10 C27 C32 103.7(17) C11 C10 C27 C32 -74.7(19) C9 C10 C27 C28 -77.1(18) C11 C10 C27 C28 104.5(16) C32 C27 C28 F6 179.6(13) C10 C27 C28 F6 0(2) C32 C27 C28 C29 4(2) C10 C27 C28 C29 -175.4(13) F6 C28 C29 F7 1(2) C27 C28 C29 F7 177.3(13) F6 C28 C29 C30 -178.2(14) C27 C28 C29 C30 -2(2) F7 C29 C30 F8 3(2) C28 C29 C30 F8 -177.7(14) F7 C29 C30 C31 -179.3(15) C28 C29 C30 C31 0(2) F8 C30 C31 F9 -1(2) C29 C30 C31 F9 -179.2(16) F8 C30 C31 C32 178.0(15) C29 C30 C31 C32 0(2) C28 C27 C32 F10 -178.8(13) C10 C27 C32 F10 0(2) C28 C27 C32 C31 -4(2) C10 C27 C32 C31 175.5(15) F9 C31 C32 F10 -4(2) C30 C31 C32 F10 177.1(15) F9 C31 C32 C27 -179.0(16) C30 C31 C32 C27 2(3) C14 C15 C33 C34 94(2) C16 C15 C33 C34 -86(2) C14 C15 C33 C38 -84(2) C16 C15 C33 C38 96(2) C38 C33 C34 F11 178(2) C15 C33 C34 F11 0(3) C38 C33 C34 C35 -3(3) C15 C33 C34 C35 178.7(16) F11 C34 C35 F12 0(3) C33 C34 C35 F12 -178.3(19) F11 C34 C35 C36 -178.8(17) C33 C34 C35 C36 3(3) F12 C35 C36 F13 0(3) C34 C35 C36 F13 179.2(16) F12 C35 C36 C37 -180(2) C34 C35 C36 C37 -1(3) F13 C36 C37 F14 -2(4) C35 C36 C37 F14 178(2) F13 C36 C37 C38 179(2) C35 C36 C37 C38 -1(4) F14 C37 C38 F15 -2(5) C36 C37 C38 F15 176(3) F14 C37 C38 C33 -178(3) C36 C37 C38 C33 0(4) C34 C33 C38 F15 -174(3) C15 C33 C38 F15 4(4) C34 C33 C38 C37 2(4) C15 C33 C38 C37 180(2) C1 C20 C39 C44 -100.8(16) C19 C20 C39 C44 76.3(17) C1 C20 C39 C40 80.2(17) C19 C20 C39 C40 -102.6(16) C44 C39 C40 F16 177.9(13) C20 C39 C40 F16 -3(2) C44 C39 C40 C41 0(2) C20 C39 C40 C41 178.9(13) F16 C40 C41 F17 2.6(19) C39 C40 C41 F17 -179.3(13) F16 C40 C41 C42 -179.7(12) C39 C40 C41 C42 -2(2) F17 C41 C42 F18 -2(2) C40 C41 C42 F18 -179.2(12) F17 C41 C42 C43 179.6(14) C40 C41 C42 C43 2(2) F18 C42 C43 F19 -1(2) C41 C42 C43 F19 177.7(15) F18 C42 C43 C44 -179.3(13) C41 C42 C43 C44 0(2) C40 C39 C44 F20 -179.5(13) C20 C39 C44 F20 1(2) C40 C39 C44 C43 2(2) C20 C39 C44 C43 -177.3(13) F19 C43 C44 C39 -179.6(15) C42 C43 C44 C39 -1(2) F19 C43 C44 F20 2(2) C42 C43 C44 F20 179.7(14) C49 N5 C45 C46 4(5) Os1 N5 C45 C46 175(2) N5 C45 C46 C47 -8(5) C45 C46 C47 C48 7(5) C46 C47 C48 C49 -4(6) C45 N5 C49 C48 -1(5) Os1 N5 C49 C48 -171(3) C47 C48 C49 N5 1(5) C54 N6 C50 C51 -6(5) Os1 N6 C50 C51 -177(3) N6 C50 C51 C52 3(6) C50 C51 C52 C53 0(6) C51 C52 C53 C54 0(6) C50 N6 C54 C53 6(6) Os1 N6 C54 C53 178(3) C52 C53 C54 N6 -3(6) C49B N5B C45B C46B -9(5) Os1B N5B C45B C46B 178(3) N5B C45B C46B C47B 0(6) C45B C46B C47B C48B 5(6) C46B C47B C48B C49B -2(6) C45B N5B C49B C48B 13(5) Os1B N5B C49B C48B -174(3) C47B C48B C49B N5B -8(6) C54B N6B C50B C51B -3(5) Os1B N6B C50B C51B -168(3) N6B C50B C51B C52B 2(6) C50B C51B C52B C53B -2(6) C51B C52B C53B C54B 4(6) C50B N6B C54B C53B 5(6) Os1B N6B C54B C53B 170(3) C52B C53B C54B N6B -6(6) C5 C4 N1 C1 177.7(13) C3 C4 N1 C1 0.1(14) C20 C1 N1 C4 -178.4(13) C2 C1 N1 C4 1.8(13) C5 C6 N2 C9 -177.7(14) C7 C6 N2 C9 0.2(16) C10 C9 N2 C6 179.4(14) C8 C9 N2 C6 0.0(17) C10 C11 N3 C14 179.4(15) C12 C11 N3 C14 -1.4(17) C15 C14 N3 C11 -179.6(17) C13 C14 N3 C11 0.5(17) C18 C19 N4 C16 -2.6(19) C20 C19 N4 C16 -178.6(14) C17 C16 N4 C19 4.0(19) C15 C16 N4 C19 -178.7(16) C3 C2 O1 Os1B -13.7(12) C1 C2 O1 Os1B 102.1(10) C3 C2 O1 Os1 -18.7(13) C1 C2 O1 Os1 97.1(10) C2 C3 O2 Os1B 7.9(13) C4 C3 O2 Os1B -106.7(10) C2 C3 O2 Os1 10.6(13) C4 C3 O2 Os1 -104.1(10) O4 Os1B O2 C3 -109.4(8) O3 Os1B O2 C3 83.1(9) O1 Os1B O2 C3 -13.2(8) N6B Os1B O2 C3 170.3(9) C58 C59 C60 C61 -135(5) C59 C60 C61 C62 -104(4) C60 C61 C62 C63 76(5)