#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:31:31 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242513 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132547.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_4132547 loop_ _publ_author_name 'Shao, Xinxin' 'Li, Kangnan' 'Malcolmson, Steven J.' _publ_section_title ; Enantioselective Synthesis of anti-1,2-Diamines by Cu-Catalyzed Reductive Couplings of Azadienes with Aldimines and Ketimines. ; _journal_issue 23 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7083 _journal_page_last 7087 _journal_paper_doi 10.1021/jacs.8b04750 _journal_volume 140 _journal_year 2018 _chemical_absolute_configuration ad _chemical_formula_moiety 'C34 H30 Br N2 O P' _chemical_formula_sum 'C34 H30 Br N2 O P' _chemical_formula_weight 593.48 _chemical_name_common Shaoxx-2-214 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.4874(2) _cell_length_b 19.8805(3) _cell_length_c 20.6103(3) _cell_measurement_reflns_used 447 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 22.8405 _cell_measurement_theta_min 2.4305 _cell_volume 5936.11(15) _computing_cell_refinement 'APEX3 v2017.3-0 (Bruker AXS)' _computing_data_collection 'Bruker Instrument Service v2013.12.0.0' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 833)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker-Nonius X8 Kappa APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 57674 _diffrn_reflns_theta_full 27.13 _diffrn_reflns_theta_max 27.13 _diffrn_reflns_theta_min 1.98 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.468 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2448 _exptl_crystal_size_max 0.299 _exptl_crystal_size_mid 0.212 _exptl_crystal_size_min 0.148 _refine_diff_density_max 0.419 _refine_diff_density_min -0.397 _refine_ls_abs_structure_details ; Flack x determined using 4876 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.0062(17) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 711 _refine_ls_number_reflns 13136 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0280 _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^)+(0.0280P)^2^+1.0534P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.0589 _reflns_number_gt 11800 _reflns_number_total 13136 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04750_si_001.cif _cod_data_source_block rds750 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_database_code 4132547 _shelx_res_file ; TITL rds750_0m in P2(1)2(1)2(1) rds750_0m.res created by SHELXL-2016/6 at 13:40:20 on 23-Feb-2018 CELL 0.71073 14.4874 19.8805 20.6103 90 90 90 ZERR 8 0.0002 0.0003 0.0003 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Br N O P UNIT 272 240 8 16 8 8 LIST 4 L.S. 10 PLAN 10 SIZE 0.148 0.212 0.299 TEMP -173.16 BOND $h conf htab EQIV $1 -x+1, y-1/2, -z+1/2 HTAB N1 O2_$1 HTAB N3 O1 acta fmap 2 OMIT 0 1 1 OMIT 1 0 1 WGHT 0.028000 1.053370 FVAR 0.07538 BR1 3 0.929390 0.430692 0.054447 11.00000 0.01623 0.02508 = 0.04428 -0.00618 0.00885 -0.00298 P1 6 0.555766 0.438674 0.250251 11.00000 0.01597 0.00985 = 0.01356 -0.00058 -0.00144 0.00091 O1 5 0.546569 0.504586 0.217032 11.00000 0.02584 0.01033 = 0.01958 0.00004 -0.00076 0.00109 N1 4 0.514756 0.377651 0.205139 11.00000 0.01974 0.00947 = 0.01055 0.00252 -0.00189 -0.00058 H1 2 0.504412 0.341120 0.220628 11.00000 -1.20000 N2 4 0.481658 0.322553 0.034980 11.00000 0.01543 0.01473 = 0.01152 0.00089 -0.00234 0.00044 C1 1 0.524688 0.378818 0.134257 11.00000 0.01419 0.01010 = 0.01211 0.00084 -0.00118 0.00112 AFIX 13 H1A 2 0.487206 0.417315 0.117493 11.00000 -1.20000 AFIX 0 C2 1 0.483990 0.313926 0.105804 11.00000 0.01477 0.01193 = 0.01308 0.00066 -0.00142 0.00167 AFIX 13 H2 2 0.523293 0.274448 0.117671 11.00000 -1.20000 AFIX 0 C3 1 0.385092 0.302396 0.127351 11.00000 0.01584 0.01605 = 0.01591 0.00145 -0.00100 -0.00106 AFIX 137 H3A 2 0.347142 0.341030 0.114679 11.00000 -1.50000 H3B 2 0.383209 0.297108 0.174607 11.00000 -1.50000 H3C 2 0.361053 0.261605 0.106683 11.00000 -1.50000 AFIX 0 C4 1 0.623409 0.389365 0.112153 11.00000 0.01511 0.01206 = 0.01248 -0.00268 -0.00069 0.00080 C5 1 0.645905 0.442760 0.071708 11.00000 0.01652 0.01641 = 0.02345 0.00262 0.00132 0.00422 AFIX 43 H5 2 0.598516 0.471848 0.056616 11.00000 -1.20000 AFIX 0 C6 1 0.736676 0.454306 0.052967 11.00000 0.02053 0.01672 = 0.03108 0.00556 0.00591 -0.00156 AFIX 43 H6 2 0.751660 0.490444 0.024708 11.00000 -1.20000 AFIX 0 C7 1 0.804474 0.412107 0.076330 11.00000 0.01133 0.01924 = 0.02530 -0.00646 0.00455 -0.00274 C8 1 0.784603 0.357788 0.115454 11.00000 0.01587 0.01989 = 0.02077 -0.00140 -0.00215 0.00477 AFIX 43 H8 2 0.832206 0.328718 0.130240 11.00000 -1.20000 AFIX 0 C9 1 0.693721 0.346692 0.132619 11.00000 0.01917 0.01403 = 0.01855 0.00204 -0.00082 0.00038 AFIX 43 H9 2 0.678877 0.309042 0.159016 11.00000 -1.20000 AFIX 0 C10 1 0.673905 0.421287 0.271940 11.00000 0.01583 0.02069 = 0.01564 -0.00414 -0.00169 0.00145 C11 1 0.741327 0.470660 0.265792 11.00000 0.02298 0.02520 = 0.03115 -0.00831 0.00188 -0.00399 AFIX 43 H11 2 0.725085 0.514595 0.251712 11.00000 -1.20000 AFIX 0 C12 1 0.832734 0.455343 0.280382 11.00000 0.02001 0.04753 = 0.05453 -0.01422 0.00044 -0.01027 AFIX 43 H12 2 0.878840 0.489112 0.276749 11.00000 -1.20000 AFIX 0 C13 1 0.856700 0.391487 0.300061 11.00000 0.01753 0.05562 = 0.05129 -0.01915 -0.01359 0.00744 AFIX 43 H13 2 0.919386 0.381391 0.309451 11.00000 -1.20000 AFIX 0 C14 1 0.790450 0.342061 0.306252 11.00000 0.02994 0.03886 = 0.03177 -0.00449 -0.01086 0.01338 AFIX 43 H14 2 0.807425 0.298156 0.319986 11.00000 -1.20000 AFIX 0 C15 1 0.699545 0.356621 0.292437 11.00000 0.02484 0.02415 = 0.02206 0.00037 -0.00658 0.00374 AFIX 43 H15 2 0.653893 0.322621 0.296823 11.00000 -1.20000 AFIX 0 C16 1 0.490524 0.432635 0.324848 11.00000 0.02165 0.00888 = 0.01735 -0.00111 -0.00078 0.00024 C17 1 0.531339 0.429325 0.385778 11.00000 0.02589 0.02129 = 0.01797 -0.00091 -0.00338 -0.00086 AFIX 43 H17 2 0.596685 0.427748 0.389313 11.00000 -1.20000 AFIX 0 C18 1 0.477432 0.428295 0.441709 11.00000 0.04125 0.02134 = 0.01513 -0.00287 -0.00197 -0.00395 AFIX 43 H18 2 0.505816 0.425545 0.483176 11.00000 -1.20000 AFIX 0 C19 1 0.382589 0.431291 0.436562 11.00000 0.03749 0.01798 = 0.01951 -0.00567 0.00967 -0.00392 AFIX 43 H19 2 0.345571 0.430813 0.474606 11.00000 -1.20000 AFIX 0 C20 1 0.341345 0.434975 0.376374 11.00000 0.02251 0.02762 = 0.02808 -0.00564 0.00673 0.00221 AFIX 43 H20 2 0.275995 0.436959 0.373085 11.00000 -1.20000 AFIX 0 C21 1 0.394915 0.435795 0.320644 11.00000 0.02419 0.02374 = 0.01770 -0.00510 -0.00184 0.00168 AFIX 43 H21 2 0.366073 0.438534 0.279332 11.00000 -1.20000 AFIX 0 C22 1 0.528533 0.284787 -0.002895 11.00000 0.01130 0.01049 = 0.01244 0.00103 -0.00015 -0.00300 C23 1 0.593822 0.229766 0.016717 11.00000 0.01474 0.01626 = 0.00985 -0.00351 -0.00187 0.00193 C24 1 0.561393 0.170355 0.044258 11.00000 0.01945 0.01644 = 0.01504 -0.00272 -0.00102 0.00137 AFIX 43 H24 2 0.497255 0.165114 0.052412 11.00000 -1.20000 AFIX 0 C25 1 0.621660 0.118898 0.059858 11.00000 0.03362 0.01820 = 0.01417 -0.00060 0.00012 0.00354 AFIX 43 H25 2 0.598733 0.078172 0.077792 11.00000 -1.20000 AFIX 0 C26 1 0.715139 0.126730 0.049362 11.00000 0.03282 0.03111 = 0.01325 -0.00402 -0.00463 0.01849 AFIX 43 H26 2 0.756564 0.091439 0.060222 11.00000 -1.20000 AFIX 0 C27 1 0.748590 0.185984 0.023016 11.00000 0.01457 0.03708 = 0.01529 -0.00393 -0.00034 0.00764 AFIX 43 H27 2 0.813050 0.191775 0.016659 11.00000 -1.20000 AFIX 0 C28 1 0.687739 0.236882 0.005924 11.00000 0.01658 0.02183 = 0.01428 -0.00159 0.00035 0.00016 AFIX 43 H28 2 0.710649 0.276953 -0.013344 11.00000 -1.20000 AFIX 0 C29 1 0.513833 0.294033 -0.074249 11.00000 0.00900 0.01747 = 0.01361 0.00135 0.00137 -0.00002 C30 1 0.517338 0.238956 -0.115530 11.00000 0.01668 0.01705 = 0.01850 0.00193 -0.00180 -0.00107 AFIX 43 H30 2 0.536556 0.196503 -0.099243 11.00000 -1.20000 AFIX 0 C31 1 0.492949 0.245306 -0.180629 11.00000 0.01898 0.02583 = 0.01588 -0.00263 -0.00240 -0.00187 AFIX 43 H31 2 0.493813 0.206964 -0.208131 11.00000 -1.20000 AFIX 0 C32 1 0.467615 0.306945 -0.205199 11.00000 0.01568 0.03377 = 0.01474 0.00535 -0.00238 0.00224 AFIX 43 H32 2 0.450851 0.311331 -0.249560 11.00000 -1.20000 AFIX 0 C33 1 0.466757 0.362576 -0.164699 11.00000 0.02482 0.02308 = 0.02010 0.00572 0.00061 0.00790 AFIX 43 H33 2 0.450944 0.405417 -0.181827 11.00000 -1.20000 AFIX 0 C34 1 0.488687 0.356481 -0.099503 11.00000 0.02007 0.01811 = 0.01844 0.00006 0.00093 0.00526 AFIX 43 H34 2 0.486589 0.394824 -0.072034 11.00000 -1.20000 AFIX 0 BR2 3 0.422729 0.539185 -0.102105 11.00000 0.03210 0.03149 = 0.01261 -0.00279 0.00021 0.00513 P2 6 0.540107 0.688617 0.210275 11.00000 0.01354 0.01109 = 0.01496 -0.00227 -0.00087 -0.00004 O2 5 0.503982 0.756930 0.224799 11.00000 0.02029 0.01371 = 0.02240 -0.00555 -0.00251 0.00146 N3 4 0.458758 0.631419 0.211484 11.00000 0.01269 0.01075 = 0.01741 -0.00076 -0.00144 0.00216 H3 2 0.475670 0.592882 0.214234 11.00000 -1.20000 N4 4 0.205600 0.631952 0.185008 11.00000 0.01265 0.01996 = 0.01366 -0.00352 -0.00022 0.00312 C35 1 0.371339 0.643094 0.177654 11.00000 0.01204 0.01276 = 0.01503 -0.00196 -0.00193 0.00263 AFIX 13 H35 2 0.361444 0.692819 0.175373 11.00000 -1.20000 AFIX 0 C36 1 0.291833 0.613009 0.217185 11.00000 0.01429 0.02229 = 0.01387 -0.00056 -0.00090 -0.00083 AFIX 13 H36 2 0.297657 0.562925 0.219032 11.00000 -1.20000 AFIX 0 C37 1 0.288452 0.642071 0.285472 11.00000 0.01841 0.05306 = 0.01550 -0.00599 -0.00161 0.00021 AFIX 137 H37A 2 0.279636 0.690882 0.283071 11.00000 -1.50000 H37B 2 0.346529 0.632235 0.307930 11.00000 -1.50000 H37C 2 0.237015 0.621807 0.309380 11.00000 -1.50000 AFIX 0 C38 1 0.373651 0.616608 0.108838 11.00000 0.00938 0.01492 = 0.01571 -0.00122 -0.00156 -0.00090 C39 1 0.365217 0.659859 0.056126 11.00000 0.02235 0.01316 = 0.02089 0.00124 -0.00220 0.00285 AFIX 43 H39 2 0.351982 0.706046 0.063424 11.00000 -1.20000 AFIX 0 C40 1 0.375810 0.636679 -0.006949 11.00000 0.02608 0.02127 = 0.01482 0.00685 -0.00124 0.00119 AFIX 43 H40 2 0.369368 0.666358 -0.042790 11.00000 -1.20000 AFIX 0 C41 1 0.395831 0.569821 -0.016397 11.00000 0.01489 0.02325 = 0.01061 -0.00329 -0.00085 0.00068 C42 1 0.401007 0.524745 0.034199 11.00000 0.01930 0.01491 = 0.01754 -0.00245 -0.00297 0.00289 AFIX 43 H42 2 0.412188 0.478371 0.026334 11.00000 -1.20000 AFIX 0 C43 1 0.389517 0.548621 0.096904 11.00000 0.02070 0.01426 = 0.01460 0.00348 -0.00196 0.00151 AFIX 43 H43 2 0.392516 0.518100 0.132307 11.00000 -1.20000 AFIX 0 C44 1 0.595107 0.689374 0.131411 11.00000 0.01203 0.01746 = 0.01657 -0.00193 -0.00065 -0.00001 C45 1 0.614510 0.750267 0.101601 11.00000 0.02538 0.01748 = 0.02258 0.00005 0.00121 0.00003 AFIX 43 H45 2 0.602960 0.791201 0.123954 11.00000 -1.20000 AFIX 0 C46 1 0.650840 0.751742 0.039064 11.00000 0.03569 0.02324 = 0.02413 0.00839 0.00257 -0.00061 AFIX 43 H46 2 0.665243 0.793548 0.019166 11.00000 -1.20000 AFIX 0 C47 1 0.665991 0.691915 0.005809 11.00000 0.02687 0.03175 = 0.01821 0.00551 0.00253 0.00532 AFIX 43 H47 2 0.689522 0.692742 -0.037208 11.00000 -1.20000 AFIX 0 C48 1 0.646600 0.630961 0.035705 11.00000 0.02289 0.02176 = 0.02170 -0.00440 0.00283 0.00543 AFIX 43 H48 2 0.656955 0.590069 0.012994 11.00000 -1.20000 AFIX 0 C49 1 0.612260 0.629327 0.098417 11.00000 0.01479 0.01661 = 0.02317 0.00302 -0.00003 0.00013 AFIX 43 H49 2 0.600402 0.587419 0.118936 11.00000 -1.20000 AFIX 0 C50 1 0.624049 0.657814 0.267521 11.00000 0.01627 0.01137 = 0.01578 -0.00467 -0.00247 0.00014 C51 1 0.716919 0.673454 0.260349 11.00000 0.01680 0.01912 = 0.02443 0.00157 -0.00169 -0.00128 AFIX 43 H51 2 0.737185 0.696400 0.222510 11.00000 -1.20000 AFIX 0 C52 1 0.780376 0.655968 0.307767 11.00000 0.01435 0.02640 = 0.03818 -0.00226 -0.00379 -0.00072 AFIX 43 H52 2 0.843620 0.667464 0.302735 11.00000 -1.20000 AFIX 0 C53 1 0.751160 0.621680 0.362483 11.00000 0.02418 0.02476 = 0.02843 -0.00463 -0.01185 0.00260 AFIX 43 H53 2 0.794668 0.609397 0.394871 11.00000 -1.20000 AFIX 0 C54 1 0.659122 0.605166 0.370364 11.00000 0.02352 0.02297 = 0.01993 -0.00237 -0.00380 0.00305 AFIX 43 H54 2 0.639481 0.581489 0.407946 11.00000 -1.20000 AFIX 0 C55 1 0.595572 0.623334 0.323128 11.00000 0.01502 0.01911 = 0.01796 -0.00273 -0.00072 0.00026 AFIX 43 H55 2 0.532266 0.612258 0.328627 11.00000 -1.20000 AFIX 0 C56 1 0.146125 0.588281 0.167874 11.00000 0.01391 0.02137 = 0.01052 -0.00357 0.00339 0.00005 C57 1 0.154874 0.513702 0.174618 11.00000 0.00880 0.02208 = 0.01472 -0.00189 0.00127 0.00022 C58 1 0.161376 0.481867 0.234859 11.00000 0.02383 0.02425 = 0.01185 -0.00332 -0.00035 -0.00127 AFIX 43 H58 2 0.159553 0.508028 0.273409 11.00000 -1.20000 AFIX 0 C59 1 0.170435 0.412740 0.239115 11.00000 0.02250 0.02583 = 0.01732 0.00358 -0.00056 -0.00257 AFIX 43 H59 2 0.173201 0.391643 0.280426 11.00000 -1.20000 AFIX 0 C60 1 0.175458 0.374406 0.183431 11.00000 0.01775 0.01725 = 0.02529 -0.00119 -0.00092 0.00067 AFIX 43 H60 2 0.183481 0.327080 0.186402 11.00000 -1.20000 AFIX 0 C61 1 0.168780 0.405020 0.122984 11.00000 0.01941 0.02397 = 0.01716 -0.00605 0.00067 -0.00036 AFIX 43 H61 2 0.171594 0.378641 0.084602 11.00000 -1.20000 AFIX 0 C62 1 0.158004 0.474152 0.118894 11.00000 0.01649 0.02303 = 0.01319 -0.00098 -0.00025 -0.00064 AFIX 43 H62 2 0.152680 0.494844 0.077515 11.00000 -1.20000 AFIX 0 C63 1 0.058493 0.614070 0.138394 11.00000 0.01507 0.02285 = 0.01501 -0.00800 0.00033 0.00338 C64 1 -0.023990 0.580239 0.146318 11.00000 0.01696 0.02498 = 0.02716 -0.00902 -0.00166 -0.00013 AFIX 43 H64 2 -0.024697 0.537723 0.167352 11.00000 -1.20000 AFIX 0 C65 1 -0.105977 0.607973 0.123726 11.00000 0.01462 0.04243 = 0.04576 -0.01466 -0.00694 0.00220 AFIX 43 H65 2 -0.162677 0.584932 0.130221 11.00000 -1.20000 AFIX 0 C66 1 -0.104950 0.668544 0.092095 11.00000 0.02177 0.04066 = 0.04781 -0.00782 -0.01499 0.01457 AFIX 43 H66 2 -0.161062 0.687437 0.076708 11.00000 -1.20000 AFIX 0 C67 1 -0.022058 0.702608 0.082358 11.00000 0.03355 0.03235 = 0.04209 0.00396 -0.01352 0.01004 AFIX 43 H67 2 -0.021280 0.744166 0.059611 11.00000 -1.20000 AFIX 0 C68 1 0.058822 0.675522 0.105997 11.00000 0.02107 0.02690 = 0.02421 -0.00017 -0.00519 0.00023 AFIX 43 H68 2 0.115316 0.699008 0.100127 11.00000 -1.20000 AFIX 0 HKLF 4 REM rds750_0m in P2(1)2(1)2(1) REM R1 = 0.0280 for 11800 Fo > 4sig(Fo) and 0.0353 for all 13136 data REM 711 parameters refined using 0 restraints END WGHT 0.0280 1.0533 REM Instructions for potential hydrogen bonds HTAB N1 O2_$1 HTAB N3 O1 HTAB C35 O2 REM Highest difference peak 0.419, deepest hole -0.397, 1-sigma level 0.048 Q1 1 0.9353 0.4367 0.0946 11.00000 0.05 0.42 Q2 1 0.4222 0.5800 -0.1037 11.00000 0.05 0.30 Q3 1 0.5670 0.6848 0.1678 11.00000 0.05 0.27 Q4 1 0.5203 0.4385 0.2884 11.00000 0.05 0.26 Q5 1 0.4949 0.6552 0.1977 11.00000 0.05 0.25 Q6 1 0.4980 0.3443 0.1275 11.00000 0.05 0.25 Q7 1 0.4172 0.5540 -0.0565 11.00000 0.05 0.24 Q8 1 0.6169 0.4370 0.2700 11.00000 0.05 0.24 Q9 1 0.5864 0.6735 0.2437 11.00000 0.05 0.23 Q10 1 0.1015 0.5990 0.1457 11.00000 0.05 0.23 ; _shelx_res_checksum 29145 _shelx_hkl_file ; 1 0 0 0.00 0.03 -1 0 0 0.03 0.04 2 0 0 585.30 12.00 -2 0 0 592.25 11.98 -2 0 0 579.80 11.96 3 0 0 -0.16 0.16 -3 0 0 0.02 0.14 -3 0 0 -0.01 0.13 -4 0 0 35.72 0.89 -4 0 0 37.62 0.92 4 0 0 36.44 0.93 -5 0 0 -0.25 0.21 -5 0 0 0.33 0.17 5 0 0 0.09 0.21 -6 0 0 2.71 0.28 -6 0 0 4.17 0.35 6 0 0 2.68 0.32 -7 0 0 0.09 0.21 7 0 0 -0.27 0.27 -7 0 0 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0 3.56 0.56 11 1 0 4.31 0.59 12 -1 0 5.57 0.63 12 1 0 6.37 0.70 13 1 0 8.39 0.79 13 -1 0 9.06 0.79 14 -1 0 0.06 0.57 14 1 0 0.42 0.60 15 1 0 6.32 0.87 15 -1 0 4.89 0.83 16 1 0 0.10 0.63 16 -1 0 -0.35 0.61 17 1 0 1.14 0.81 17 -1 0 0.39 0.79 18 1 0 3.63 0.88 18 -1 0 0.50 0.83 -1 2 0 17.76 0.40 -1 -2 0 17.25 0.43 -1 -2 0 17.48 0.45 1 -2 0 17.05 0.40 1 -2 0 17.44 0.38 1 2 0 17.92 0.43 1 -2 0 17.71 0.42 -1 2 0 17.98 0.42 -2 2 0 4.38 0.18 -2 -2 0 4.36 0.24 -2 2 0 4.54 0.14 2 -2 0 4.13 0.19 -2 2 0 4.10 0.19 2 2 0 4.47 0.26 2 -2 0 3.93 0.19 -2 2 0 4.30 0.17 3 2 0 585.08 12.31 -3 2 0 595.43 12.27 3 -2 0 598.40 12.23 -3 2 0 593.85 12.05 -3 -2 0 600.94 12.12 3 -2 0 622.55 12.01 4 -2 0 235.19 4.85 -4 2 0 237.18 4.83 -4 -2 0 241.58 4.91 -4 2 0 236.86 4.84 4 -2 0 236.64 4.83 4 2 0 241.34 4.91 5 2 0 225.29 4.68 -5 2 0 221.74 4.58 -5 -2 0 224.22 4.67 5 -2 0 219.52 4.62 5 -2 0 220.45 4.58 -5 2 0 231.89 4.61 6 2 0 182.30 4.02 6 -2 0 186.42 3.98 6 -2 0 184.78 3.92 -6 2 0 191.66 3.96 -6 2 0 191.74 3.93 -6 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0.50 2 -7 0 13.82 0.38 -2 -7 0 14.24 0.60 2 -7 0 13.27 0.49 3 -7 0 70.53 1.52 3 7 0 69.22 1.65 3 -7 0 69.80 1.59 3 -7 0 70.33 1.66 -3 7 0 72.19 1.59 -3 -7 0 73.57 1.69 -3 -7 0 75.71 1.76 -3 7 0 73.13 1.62 -4 7 0 23.70 0.72 4 -7 0 23.35 0.72 4 -7 0 22.75 0.63 -4 7 0 22.83 0.63 4 7 0 22.51 0.76 -4 7 0 22.72 0.67 4 -7 0 22.19 0.61 5 -7 0 53.40 1.22 -5 7 0 53.93 1.22 5 -7 0 52.28 1.25 5 -7 0 55.52 1.33 -5 7 0 54.18 1.32 5 7 0 50.88 1.39 6 -7 0 24.84 0.77 6 -7 0 24.31 0.73 -6 7 0 23.20 0.65 6 7 0 24.78 0.88 -6 7 0 24.31 0.77 7 -7 0 79.76 1.86 7 7 0 78.92 1.98 -7 7 0 78.28 1.85 7 -7 0 77.02 1.84 -7 7 0 77.65 1.71 8 -7 0 34.09 1.05 -8 7 0 34.81 0.82 8 7 0 36.35 1.21 -8 7 0 36.06 0.89 8 -7 0 33.22 1.02 -8 7 0 34.94 1.02 -9 7 0 0.50 0.17 -9 7 0 0.94 0.29 -9 7 0 0.42 0.19 9 -7 0 0.25 0.27 9 7 0 0.65 0.40 9 -7 0 1.26 0.34 10 -7 0 43.73 1.35 -10 7 0 43.85 1.11 10 7 0 42.98 1.49 10 -7 0 45.09 1.26 -10 7 0 43.41 1.07 11 -7 0 39.71 1.18 11 -7 0 40.54 1.31 -11 7 0 37.54 1.02 -11 7 0 36.22 1.02 11 7 0 40.28 1.47 12 -7 0 36.77 1.19 12 7 0 36.37 1.48 12 -7 0 35.70 1.31 13 7 0 21.49 1.25 13 -7 0 18.79 1.05 14 7 0 0.10 0.66 14 -7 0 0.87 0.57 15 7 0 -0.45 0.70 15 -7 0 0.70 0.61 16 7 0 7.10 1.00 16 -7 0 5.96 0.84 17 -7 0 4.49 0.86 17 7 0 5.07 0.95 -17 -7 0 5.51 0.94 0 8 0 78.70 1.64 0 -8 0 81.07 1.73 0 -8 0 82.26 1.84 0 8 0 77.24 1.83 0 -8 0 81.61 1.73 0 -8 0 78.32 1.86 -1 -8 0 106.01 2.38 1 -8 0 102.12 2.17 1 8 0 103.62 2.19 1 -8 0 102.15 2.34 -1 -8 0 105.98 2.25 1 8 0 105.67 2.35 -1 8 0 100.83 2.29 1 -8 0 106.32 2.32 -1 -8 0 103.65 2.35 1 8 0 104.79 2.19 1 -8 0 107.34 2.30 2 -8 0 170.51 3.50 2 -8 0 172.55 3.63 -2 -8 0 170.68 3.71 -2 -8 0 167.18 3.74 2 8 0 167.78 3.59 2 -8 0 177.41 3.69 -2 8 0 173.60 3.63 -2 8 0 176.46 3.64 -2 -8 0 178.51 3.64 -3 8 0 4.20 0.31 -3 8 0 4.08 0.29 -3 -8 0 4.15 0.40 3 -8 0 4.26 0.25 3 -8 0 4.18 0.30 3 -8 0 4.09 0.37 3 8 0 3.38 0.31 4 -8 0 0.15 0.15 4 -8 0 0.10 0.18 4 8 0 0.25 0.25 4 -8 0 0.43 0.23 -4 8 0 0.18 0.23 -4 8 0 0.25 0.20 -4 8 0 0.38 0.18 5 -8 0 39.62 1.09 -5 8 0 40.38 1.08 -5 8 0 41.84 0.98 5 -8 0 39.99 0.99 5 -8 0 39.50 0.98 5 8 0 37.58 1.13 -6 8 0 105.73 2.34 6 -8 0 104.20 2.27 6 -8 0 103.32 2.35 -6 8 0 103.39 2.21 6 8 0 98.84 2.43 7 8 0 0.57 0.36 7 -8 0 0.91 0.25 7 -8 0 0.83 0.29 -7 8 0 0.95 0.27 -7 8 0 0.66 0.18 -8 8 0 92.25 2.00 8 -8 0 90.68 2.16 -8 8 0 91.99 2.16 8 -8 0 93.22 2.17 8 8 0 92.46 2.32 9 8 0 2.66 0.52 -9 8 0 3.04 0.26 9 -8 0 2.53 0.39 9 -8 0 2.85 0.38 -10 8 0 28.45 0.79 10 8 0 28.89 1.17 -10 8 0 28.47 0.73 10 -8 0 27.95 0.98 10 -8 0 27.47 1.03 11 -8 0 0.08 0.38 11 -8 0 0.62 0.35 11 8 0 -0.15 0.50 12 8 0 12.38 0.95 12 -8 0 12.97 0.74 12 -8 0 12.78 0.84 13 8 0 0.86 0.63 13 -8 0 1.40 0.52 14 8 0 1.58 0.65 14 -8 0 2.65 0.61 15 8 0 -1.07 0.66 15 -8 0 -0.07 0.59 16 -8 0 0.92 0.68 16 8 0 1.60 0.81 -16 -8 0 1.53 0.80 -17 -8 0 1.04 0.83 17 -8 0 0.56 0.71 17 8 0 1.68 0.90 0 -9 0 -0.51 0.22 0 9 0 -0.66 0.23 0 -9 0 -0.04 0.24 0 9 0 0.11 0.09 0 -9 0 0.16 0.17 -1 9 0 35.72 0.97 1 -9 0 35.53 1.04 -1 -9 0 35.07 1.01 1 9 0 34.54 0.85 1 9 0 35.35 1.04 -1 -9 0 35.58 0.93 1 -9 0 34.67 1.00 1 9 0 35.82 0.85 1 -9 0 35.59 0.85 -1 -9 0 35.78 1.05 1 -9 0 36.62 0.97 -2 9 0 212.79 4.42 -2 -9 0 214.31 4.42 2 -9 0 209.95 4.42 2 9 0 216.89 4.36 -2 -9 0 207.17 4.54 2 9 0 209.36 4.51 2 9 0 210.65 4.36 2 -9 0 209.40 4.29 2 -9 0 206.05 4.48 2 -9 0 217.62 4.43 -3 9 0 14.76 0.55 3 -9 0 12.71 0.60 3 9 0 14.67 0.55 -3 -9 0 14.24 0.69 3 -9 0 13.93 0.54 -3 9 0 14.33 0.54 3 -9 0 13.41 0.43 -4 9 0 82.28 1.82 -4 9 0 80.52 1.84 4 -9 0 81.92 1.82 4 -9 0 81.03 1.75 4 -9 0 81.23 1.92 4 9 0 78.24 1.90 5 -9 0 -0.32 0.24 5 -9 0 -0.06 0.18 -5 9 0 -0.02 0.17 5 9 0 -0.17 0.25 -5 9 0 -0.13 0.23 -5 9 0 0.09 0.21 5 -9 0 0.19 0.18 6 -9 0 21.04 0.63 6 -9 0 22.21 0.69 -6 9 0 21.44 0.77 -6 9 0 21.56 0.64 6 9 0 20.89 0.84 6 -9 0 20.98 0.76 -7 9 0 13.85 0.61 -7 9 0 13.04 0.47 7 -9 0 12.90 0.61 7 -9 0 12.49 0.56 7 9 0 12.33 0.69 8 9 0 15.48 0.80 8 -9 0 15.50 0.67 -8 9 0 16.25 0.53 8 -9 0 15.88 0.68 9 -9 0 17.69 0.77 9 -9 0 18.27 0.78 9 9 0 17.13 0.89 -9 9 0 17.12 0.56 10 -9 0 12.44 0.68 10 9 0 11.29 0.83 10 -9 0 9.82 0.69 -10 9 0 11.10 0.45 11 -9 0 10.78 0.78 11 9 0 9.80 0.81 11 -9 0 11.68 0.70 12 -9 0 7.25 0.68 12 9 0 8.41 0.84 12 -9 0 6.90 0.59 13 9 0 23.99 1.36 13 -9 0 25.31 1.19 13 -9 0 24.13 1.00 14 -9 0 0.40 0.52 14 9 0 0.11 0.66 15 -9 0 1.17 0.64 15 9 0 1.29 0.76 -16 -9 0 6.59 0.94 16 9 0 7.31 1.03 16 -9 0 6.16 0.88 17 9 0 2.50 0.93 -17 -9 0 2.64 0.84 17 -9 0 0.75 0.72 0 10 0 98.28 2.29 0 -10 0 99.95 2.33 0 -10 0 101.34 2.30 1 -10 0 40.83 1.09 1 10 0 38.98 0.92 1 -10 0 38.98 1.14 -1 -10 0 38.95 1.01 1 10 0 37.92 1.11 1 -10 0 38.83 0.95 -1 10 0 37.60 1.08 1 10 0 40.46 0.92 1 -10 0 39.20 1.11 -1 -10 0 38.25 1.15 -2 -10 0 2.14 0.37 -2 10 0 1.88 0.29 2 -10 0 1.87 0.33 2 10 0 1.92 0.23 2 -10 0 2.27 0.21 2 10 0 1.56 0.22 2 -10 0 1.67 0.28 2 -10 0 1.73 0.30 3 10 0 32.25 0.91 3 -10 0 31.73 0.80 3 -10 0 31.22 0.97 -3 10 0 32.01 0.93 -3 -10 0 33.11 1.09 3 -10 0 33.24 0.93 -4 10 0 2.99 0.30 4 -10 0 2.80 0.36 4 -10 0 2.53 0.29 4 10 0 2.33 0.33 -4 -10 0 1.83 0.40 4 -10 0 2.35 0.13 -4 10 0 2.06 0.29 4 -10 0 2.29 0.22 5 10 0 2.94 0.38 5 -10 0 3.30 0.27 5 -10 0 2.96 0.28 -5 10 0 3.13 0.29 5 -10 0 3.11 0.38 -5 10 0 3.00 0.32 -6 10 0 52.39 1.34 6 -10 0 53.80 1.27 -6 10 0 54.26 1.27 6 -10 0 53.01 1.29 6 10 0 50.64 1.44 6 -10 0 52.52 1.41 7 -10 0 23.79 0.80 -7 10 0 25.33 0.72 -7 10 0 26.59 0.83 7 -10 0 23.95 0.87 7 10 0 25.53 0.99 -8 10 0 6.27 0.35 8 -10 0 5.18 0.43 8 10 0 5.54 0.55 8 -10 0 5.15 0.47 9 -10 0 3.51 0.43 -9 10 0 4.10 0.29 9 -10 0 3.17 0.42 9 10 0 3.35 0.52 10 -10 0 9.90 0.67 10 10 0 10.42 0.79 10 -10 0 11.40 0.71 11 -10 0 1.87 0.44 11 10 0 1.78 0.59 11 -10 0 1.69 0.42 12 -10 0 4.50 0.52 12 10 0 3.72 0.67 12 -10 0 4.50 0.59 13 -10 0 0.64 0.51 13 -10 0 2.39 0.46 13 10 0 2.44 0.71 14 -10 0 41.30 1.58 14 10 0 42.93 1.80 15 10 0 6.54 0.97 -15 -10 0 6.88 1.03 15 -10 0 6.38 0.80 16 10 0 8.75 1.11 16 -10 0 8.86 1.07 -16 -10 0 9.43 1.07 17 10 0 0.86 0.89 -17 -10 0 1.82 0.92 0 -11 0 -0.18 0.28 0 11 0 0.14 0.28 1 -11 0 14.12 0.66 1 -11 0 13.28 0.48 1 11 0 13.83 0.68 1 11 0 12.71 0.42 1 11 0 13.77 0.43 1 -11 0 14.08 0.65 -1 -11 0 12.98 0.66 1 -11 0 13.09 0.68 -1 11 0 13.95 0.63 2 -11 0 38.83 1.10 2 11 0 39.36 0.98 -2 11 0 39.76 1.10 2 -11 0 39.73 1.09 2 -11 0 38.10 0.95 2 -11 0 38.44 1.18 2 11 0 38.22 0.98 -2 -11 0 39.33 1.22 3 11 0 76.85 1.82 3 -11 0 77.49 1.87 -3 -11 0 82.57 2.06 -3 11 0 79.65 1.88 3 -11 0 77.64 1.93 3 -11 0 80.86 1.73 3 11 0 78.21 1.82 -4 11 0 21.90 0.76 4 -11 0 22.36 0.64 4 11 0 23.25 0.78 4 -11 0 23.00 0.84 -4 -11 0 20.47 0.92 4 -11 0 22.82 0.53 4 -11 0 22.93 0.75 5 -11 0 12.50 0.49 5 11 0 12.85 0.65 -5 11 0 13.03 0.53 -5 11 0 12.24 0.57 5 -11 0 12.65 0.65 -5 -11 0 13.49 0.85 5 -11 0 12.83 0.53 6 11 0 0.50 0.32 6 -11 0 0.18 0.29 6 -11 0 -0.02 0.21 6 -11 0 0.37 0.21 -6 11 0 0.20 0.25 -6 11 0 0.18 0.21 7 11 0 -0.07 0.31 -7 11 0 0.26 0.26 7 -11 0 0.18 0.24 7 -11 0 0.11 0.32 7 -11 0 -0.12 0.20 -7 11 0 0.26 0.20 -8 11 0 14.28 0.52 8 -11 0 13.76 0.64 8 11 0 13.40 0.83 -8 11 0 14.28 0.64 8 -11 0 14.17 0.71 9 11 0 24.25 1.06 -9 11 0 24.10 0.70 9 -11 0 26.03 0.94 9 -11 0 23.19 0.89 10 -11 0 3.16 0.45 10 11 0 2.33 0.54 10 -11 0 2.80 0.46 11 -11 0 1.08 0.43 11 -11 0 1.79 0.44 11 11 0 1.15 0.58 12 -11 0 0.76 0.42 12 -11 0 0.48 0.44 12 11 0 1.43 0.63 13 -11 0 2.00 0.55 -13 -11 0 1.99 0.73 13 11 0 1.83 0.70 13 -11 0 1.62 0.49 14 -11 0 11.67 0.92 -14 -11 0 9.37 1.11 14 11 0 11.98 1.06 -15 -11 0 0.06 0.72 15 11 0 -1.18 0.69 -16 -11 0 19.38 1.45 16 11 0 21.82 1.52 0 -12 0 8.87 0.62 0 12 0 10.04 0.61 -1 -12 0 3.94 0.47 1 12 0 3.55 0.24 1 -12 0 3.54 0.42 -1 12 0 2.93 0.37 1 -12 0 2.83 0.42 1 12 0 2.92 0.21 1 12 0 2.48 0.38 1 -12 0 3.28 0.29 2 12 0 0.05 0.17 2 -12 0 -0.17 0.25 -2 -12 0 -0.13 0.37 2 -12 0 0.39 0.30 2 12 0 -0.09 0.18 2 -12 0 -0.09 0.17 -2 12 0 -0.02 0.26 -3 12 0 1.28 0.31 -3 -12 0 1.77 0.42 3 12 0 1.19 0.26 3 12 0 1.12 0.24 3 -12 0 1.45 0.31 3 -12 0 1.39 0.21 3 -12 0 1.76 0.36 4 12 0 1.07 0.30 -4 12 0 0.93 0.30 -4 -12 0 1.45 0.41 4 -12 0 1.62 0.35 4 -12 0 1.12 0.28 4 -12 0 1.07 0.21 4 -12 0 1.63 0.15 5 12 0 36.98 1.12 5 -12 0 37.22 1.03 -5 12 0 35.68 1.06 5 -12 0 36.24 1.15 5 -12 0 36.88 0.96 -5 -12 0 35.28 1.29 6 -12 0 29.37 1.02 6 12 0 27.54 1.02 6 -12 0 29.77 0.85 -6 12 0 29.81 0.93 6 -12 0 29.06 0.87 -6 -12 0 29.05 1.18 7 -12 0 6.04 0.42 7 -12 0 4.38 0.48 -7 -12 0 5.85 0.71 7 -12 0 5.58 0.38 -7 12 0 5.37 0.44 -7 12 0 5.47 0.40 7 12 0 4.95 0.53 8 -12 0 0.38 0.29 -8 -12 0 0.87 0.50 8 -12 0 1.27 0.37 8 12 0 1.29 0.45 -8 12 0 0.28 0.22 -8 12 0 0.19 0.29 9 -12 0 7.50 0.54 -9 12 0 8.30 0.55 9 -12 0 8.02 0.62 9 12 0 6.57 0.69 10 -12 0 1.05 0.38 10 12 0 1.26 0.57 -10 12 0 1.10 0.36 10 -12 0 0.73 0.39 11 -12 0 2.93 0.50 -11 -12 0 1.75 0.67 11 -12 0 2.77 0.48 11 12 0 2.80 0.67 12 -12 0 0.90 0.45 -12 -12 0 0.85 0.65 12 12 0 0.18 0.61 12 -12 0 0.41 0.45 13 12 0 5.77 0.81 -13 -12 0 8.34 1.05 13 -12 0 6.05 0.70 14 12 0 1.55 0.77 -14 -12 0 1.59 0.75 -15 -12 0 10.58 1.14 15 12 0 12.28 1.16 -16 -12 0 2.09 0.98 16 12 0 3.03 0.87 0 13 0 0.15 0.30 0 -13 0 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0.33 0.17 -2 -15 0 1.04 0.48 2 -15 0 0.16 0.35 2 -15 0 -0.13 0.23 2 15 0 -0.07 0.15 -2 15 0 0.17 0.33 -3 15 0 140.29 3.16 3 15 0 135.57 2.96 3 15 0 137.37 2.96 3 -15 0 136.18 3.17 3 -15 0 138.61 2.97 -3 -15 0 136.98 3.38 3 -15 0 137.50 3.27 4 15 0 5.97 0.43 4 -15 0 6.27 0.52 4 -15 0 5.58 0.38 -4 15 0 5.60 0.51 4 -15 0 5.51 0.57 4 15 0 5.77 0.45 -4 -15 0 6.01 0.73 4 -15 0 5.65 0.32 5 15 0 81.06 2.00 5 -15 0 80.55 2.00 5 -15 0 80.17 1.87 5 -15 0 82.60 2.14 -5 -15 0 80.15 2.34 -5 15 0 80.95 2.02 6 -15 0 -0.32 0.40 -6 -15 0 0.64 0.54 6 -15 0 0.24 0.26 6 15 0 0.27 0.36 -6 15 0 -0.04 0.32 6 -15 0 -0.03 0.29 7 -15 0 15.78 0.68 7 -15 0 16.16 0.69 -7 15 0 15.59 0.74 -7 -15 0 17.14 1.15 7 15 0 15.71 0.85 7 -15 0 18.08 0.91 -8 15 0 13.74 0.70 8 -15 0 14.02 0.85 8 -15 0 13.78 0.62 8 15 0 14.01 0.87 8 -15 0 11.97 0.65 -8 -15 0 12.10 1.01 -9 -15 0 25.15 1.34 9 15 0 26.88 1.19 9 -15 0 25.89 1.08 -9 15 0 23.64 0.93 -10 -15 0 3.56 0.85 10 -15 0 2.99 0.56 10 15 0 4.23 0.66 -11 -15 0 53.51 2.05 11 -15 0 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0.94 1 3 -25 7.49 0.89 1 -3 25 8.82 1.22 -1 3 25 5.99 0.99 1 3 25 6.85 1.03 -1 3 -25 6.89 0.96 -1 -3 25 7.47 0.93 -1 -3 25 5.69 1.10 1 -3 -25 7.84 0.87 2 -3 25 0.23 0.66 -2 3 25 1.25 0.90 2 3 -25 0.61 0.69 2 -3 25 1.05 0.76 2 -3 25 -1.00 0.78 -2 3 -25 0.60 0.78 -2 -3 25 0.95 0.68 2 3 25 0.83 0.91 -2 -3 25 1.77 0.87 3 3 -25 5.54 0.87 -3 3 25 6.73 1.11 3 -3 25 7.31 1.08 3 -3 25 6.96 0.99 3 -3 25 4.88 0.91 3 3 25 6.04 0.89 -3 -3 25 5.96 1.07 3 3 25 6.25 1.16 4 3 -25 3.60 0.74 -4 3 25 0.98 0.88 4 -3 25 1.96 0.93 4 -3 25 3.37 0.96 4 -3 25 1.99 0.80 4 3 25 1.79 1.00 4 3 25 4.48 0.85 -4 -3 25 3.69 0.95 5 -3 25 11.57 1.29 5 -3 25 11.09 1.32 -5 3 25 8.67 1.16 5 -3 25 10.60 1.25 5 3 -25 10.61 0.99 5 3 25 13.04 1.16 -5 -3 25 11.97 1.27 5 3 25 13.68 1.34 0 4 -25 7.86 1.03 0 -4 25 8.95 1.16 0 -4 25 8.26 1.01 0 4 25 7.70 1.08 1 -4 25 5.67 0.95 -1 4 25 7.53 1.05 1 4 -25 7.62 0.99 1 -4 25 5.65 1.05 -1 -4 25 7.76 0.97 -1 4 -25 7.04 1.00 -1 -4 25 6.57 1.08 1 4 25 7.66 1.14 2 -4 25 14.93 1.33 2 -4 25 11.96 1.22 2 -4 25 16.92 1.29 -2 4 25 17.14 1.42 2 4 -25 14.76 1.17 -2 -4 25 12.64 1.10 -2 4 -25 10.93 1.15 2 4 25 14.62 1.39 -2 -4 25 13.35 1.36 3 -4 25 11.52 1.28 3 -4 25 10.35 1.12 -3 4 25 12.87 1.29 3 -4 25 10.98 1.20 3 4 -25 12.30 1.12 3 4 25 10.70 1.02 -3 -4 25 12.51 1.27 3 4 25 11.18 1.22 4 -4 25 3.84 1.00 4 -4 25 6.84 1.15 -4 4 25 5.60 0.96 4 4 -25 5.38 0.85 4 -4 25 5.29 1.04 -4 -4 25 4.12 0.98 4 4 25 5.59 0.87 4 4 25 5.10 1.01 5 4 -25 12.26 1.07 5 -4 25 9.80 1.17 -5 4 25 12.90 1.31 5 -4 25 9.66 1.27 5 -4 25 12.22 1.28 -5 -4 25 19.52 1.56 5 4 25 15.07 1.38 -5 -4 25 14.38 1.32 5 4 25 13.86 1.17 0 -5 25 11.64 1.24 0 5 -25 13.95 1.22 0 5 25 11.90 1.23 0 -5 25 10.64 1.13 1 -5 25 1.46 0.98 1 5 -25 2.57 0.82 1 -5 25 2.67 0.86 -1 5 25 2.98 0.89 1 5 25 3.44 1.00 -1 5 -25 3.84 0.89 -1 -5 25 3.48 1.07 -1 -5 25 3.15 0.82 2 -5 25 1.54 0.84 2 -5 25 1.70 0.87 2 -5 25 1.68 0.83 2 5 -25 1.27 0.77 -2 5 25 0.31 0.73 -2 5 -25 2.10 0.77 -2 -5 25 2.08 0.74 -2 -5 25 0.91 0.87 2 5 25 -0.29 0.79 -3 5 25 9.84 1.12 3 -5 25 7.20 1.18 3 -5 25 8.45 1.14 3 5 -25 7.87 0.95 3 -5 25 9.38 1.11 3 5 25 7.20 1.11 -3 -5 25 8.29 1.17 -3 -5 25 8.76 1.24 -3 5 -25 7.79 1.08 4 5 -25 3.04 0.79 4 -5 25 1.24 0.88 -4 5 25 3.03 0.96 4 -5 25 1.49 0.90 4 -5 25 0.93 0.83 4 5 25 1.50 0.99 -4 -5 25 3.18 0.95 -4 -5 25 1.97 1.01 4 5 25 1.97 0.76 0 -6 25 -0.72 0.71 0 6 25 2.47 0.93 0 -6 25 1.21 0.91 0 6 -25 1.42 0.82 -1 6 25 2.80 0.88 1 -6 25 3.45 0.89 1 -6 25 3.72 0.97 1 6 -25 3.59 0.81 -1 -6 25 4.17 0.85 -1 -6 25 3.53 0.96 1 6 25 2.69 0.99 -1 6 -25 2.35 0.87 2 6 -25 1.21 0.70 2 -6 25 0.19 0.78 2 -6 25 2.41 0.82 -2 6 25 0.98 0.88 2 -6 25 0.77 0.99 -2 -6 25 0.47 0.72 -2 -6 25 3.02 0.89 2 6 25 0.62 0.81 -2 -6 25 2.54 1.00 -2 6 -25 1.76 0.79 3 6 -25 13.41 1.12 3 -6 25 11.53 1.26 3 -6 25 11.88 1.28 3 -6 25 10.60 1.21 -3 6 25 11.22 1.24 -3 -6 25 15.52 1.18 3 6 25 15.45 1.45 -3 6 -25 14.53 1.27 -3 -6 25 15.82 1.38 -3 -6 25 13.78 1.34 4 -6 25 0.58 0.79 -4 6 25 0.97 0.77 4 -6 25 1.58 0.97 4 -6 25 0.26 0.82 4 6 -25 -0.25 0.69 4 6 25 0.11 0.69 -4 6 -25 0.09 0.84 4 6 25 1.50 0.95 -4 -6 25 -0.90 0.81 0 7 25 16.27 1.42 0 7 -25 13.31 1.26 0 -7 25 14.80 1.39 0 -7 25 13.39 1.25 -1 7 25 2.92 0.98 1 -7 25 2.80 0.90 1 -7 25 1.71 0.89 1 7 -25 1.92 0.84 -1 -7 25 0.57 0.93 -1 7 -25 2.79 0.88 1 7 25 1.70 0.84 -1 -7 25 3.03 0.84 -1 -7 25 2.16 0.94 -2 7 25 4.49 0.91 2 7 -25 4.35 0.93 2 -7 25 6.30 1.14 2 -7 25 4.57 1.06 2 -7 25 5.15 0.94 -2 -7 25 3.96 1.08 -2 7 -25 5.62 1.02 2 7 25 5.14 0.99 -2 -7 25 4.45 0.88 -2 -7 25 5.80 1.04 -3 7 25 3.96 0.96 3 -7 25 2.97 1.00 3 -7 25 4.12 1.05 3 7 -25 3.44 0.88 3 -7 25 2.28 0.89 -3 -7 25 4.03 0.99 -3 7 -25 2.08 0.89 -3 -7 25 4.97 0.86 -3 -7 25 4.10 0.96 3 7 25 3.59 1.04 0 8 -25 0.00 0.78 0 8 25 -0.30 0.75 0 -8 25 0.39 0.71 0 -8 25 -1.07 0.80 0 -8 25 -1.16 0.80 -1 8 25 2.12 0.91 1 -8 25 2.38 0.94 1 8 -25 2.31 0.90 1 -8 25 2.14 0.90 -1 -8 25 1.72 0.92 -1 8 -25 2.08 0.81 -1 -8 25 2.50 1.00 1 8 25 2.90 0.89 -1 -8 25 3.82 0.83 0 0 -26 41.19 1.76 0 0 26 39.68 1.98 -1 0 26 -0.94 0.84 -1 0 -26 0.38 0.71 1 0 26 -0.87 0.89 1 0 -26 1.18 0.69 -2 0 26 16.82 1.44 2 0 -26 17.90 1.22 2 0 26 20.65 1.59 3 0 26 1.05 0.82 3 0 26 0.72 0.95 -3 0 26 1.91 0.90 0 1 26 3.01 0.92 0 -1 26 4.61 0.87 0 1 -26 2.06 0.77 0 -1 -26 5.31 0.86 0 -1 26 4.84 1.09 1 -1 26 2.16 0.80 1 1 -26 2.47 0.74 -1 1 26 3.43 1.04 1 -1 26 3.15 1.04 -1 -1 26 0.77 0.86 1 -1 -26 0.84 0.68 1 1 26 0.69 0.92 -1 1 -26 1.66 0.73 -1 -1 26 1.95 0.83 2 -1 26 2.95 1.03 -2 1 26 2.72 1.02 2 1 -26 3.70 0.76 2 -1 26 1.47 0.83 2 1 26 2.87 1.02 -2 -1 26 2.82 0.94 3 -1 26 0.93 0.85 3 -1 26 0.75 0.85 3 1 -26 -0.37 1.00 3 -1 26 0.77 0.97 -3 1 26 0.49 0.92 3 1 26 1.83 0.82 3 1 26 1.42 0.98 -3 -1 26 -0.73 0.79 0 -2 26 10.83 1.09 0 2 26 9.90 1.28 0 2 -26 9.00 1.04 0 -2 -26 9.00 0.97 0 -2 26 7.80 1.13 1 -2 26 2.59 0.83 1 2 -26 3.49 0.84 1 -2 26 4.25 1.08 -1 2 26 2.61 0.92 1 2 26 3.31 0.96 -1 2 -26 4.49 0.85 -1 -2 26 6.61 1.09 -1 -2 26 4.78 0.85 2 -2 26 4.00 1.07 2 -2 26 5.09 0.97 -2 2 26 6.91 1.08 2 2 -26 5.52 0.88 -2 2 -26 6.11 0.93 -2 -2 26 6.20 1.08 2 2 26 7.34 1.13 3 -2 26 5.81 1.03 -3 2 26 4.29 0.98 3 2 -26 5.01 0.83 3 -2 26 5.87 1.05 3 -2 26 5.00 1.05 -3 -2 26 7.71 1.13 3 2 26 6.69 1.21 3 2 26 6.66 0.99 0 -3 26 10.98 1.14 0 3 26 12.52 1.31 0 3 -26 12.60 1.15 0 -3 26 12.44 1.31 1 -3 26 3.48 0.98 -1 3 26 4.06 0.97 1 -3 26 1.56 0.83 1 3 -26 4.24 0.80 -1 -3 26 6.54 1.19 -1 3 -26 4.22 0.84 -1 -3 26 4.13 0.84 1 3 26 4.31 1.09 -2 3 26 0.96 0.91 2 -3 26 0.76 0.70 2 3 -26 1.23 0.74 2 -3 26 1.53 0.89 2 3 26 0.12 0.81 -2 -3 26 0.79 0.88 -2 3 -26 1.57 0.74 0 -4 26 1.40 0.99 0 4 -26 2.42 0.77 0 -4 26 3.16 0.85 0 4 26 2.76 0.94 1 -4 26 1.88 0.92 1 4 -26 0.38 0.75 -1 4 26 0.70 0.92 1 -4 26 2.77 0.87 -1 -4 26 3.51 0.99 -1 4 -26 1.84 0.83 1 4 26 3.76 0.96 -1 -4 26 2.21 0.76 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 7079 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_posn _atom_site_occupancy Br Br1 0.92939(2) 0.43069(2) 0.05445(2) 0.02853(8) Uani d . . 1 P P1 0.55577(5) 0.43867(3) 0.25025(3) 0.01313(14) Uani d . . 1 O O1 0.54657(14) 0.50459(9) 0.21703(9) 0.0186(4) Uani d . . 1 N N1 0.51476(16) 0.37765(11) 0.20514(11) 0.0132(5) Uani d . . 1 H H1 0.504(2) 0.3411(16) 0.2206(14) 0.016 Uiso d U . 1 N N2 0.48166(16) 0.32255(11) 0.03498(10) 0.0139(5) Uani d . . 1 C C1 0.52469(19) 0.37882(13) 0.13426(12) 0.0121(5) Uani d . . 1 H H1A 0.487206 0.417315 0.117493 0.015 Uiso calc U R 1 C C2 0.48399(18) 0.31393(13) 0.10580(13) 0.0133(5) Uani d . . 1 H H2 0.523293 0.274448 0.117671 0.016 Uiso calc U R 1 C C3 0.38509(19) 0.30240(14) 0.12735(13) 0.0159(6) Uani d . . 1 H H3A 0.347142 0.34103 0.114679 0.024 Uiso calc U R 1 H H3B 0.383209 0.297108 0.174607 0.024 Uiso calc U R 1 H H3C 0.361053 0.261605 0.106683 0.024 Uiso calc U R 1 C C4 0.62341(19) 0.38936(13) 0.11215(12) 0.0132(6) Uani d . . 1 C C5 0.6459(2) 0.44276(13) 0.07171(14) 0.0188(6) Uani d . . 1 H H5 0.598516 0.471848 0.056616 0.023 Uiso calc U R 1 C C6 0.7367(2) 0.45431(14) 0.05297(15) 0.0228(6) Uani d . . 1 H H6 0.75166 0.490444 0.024708 0.027 Uiso calc U R 1 C C7 0.8045(2) 0.41211(14) 0.07633(14) 0.0186(6) Uani d . . 1 C C8 0.7846(2) 0.35779(14) 0.11545(13) 0.0188(6) Uani d . . 1 H H8 0.832206 0.328718 0.13024 0.023 Uiso calc U R 1 C C9 0.6937(2) 0.34669(13) 0.13262(13) 0.0173(6) Uani d . . 1 H H9 0.678877 0.309042 0.159016 0.021 Uiso calc U R 1 C C10 0.6739(2) 0.42129(14) 0.27194(13) 0.0174(6) Uani d . . 1 C C11 0.7413(2) 0.47066(16) 0.26579(15) 0.0264(7) Uani d . . 1 H H11 0.725085 0.514595 0.251712 0.032 Uiso calc U R 1 C C12 0.8327(2) 0.4553(2) 0.28038(19) 0.0407(9) Uani d . . 1 H H12 0.87884 0.489112 0.276749 0.049 Uiso calc U R 1 C C13 0.8567(2) 0.3915(2) 0.30006(19) 0.0415(10) Uani d . . 1 H H13 0.919386 0.381391 0.309451 0.05 Uiso calc U R 1 C C14 0.7904(2) 0.34206(18) 0.30625(16) 0.0335(8) Uani d . . 1 H H14 0.807425 0.298156 0.319986 0.04 Uiso calc U R 1 C C15 0.6995(2) 0.35662(15) 0.29244(14) 0.0237(7) Uani d . . 1 H H15 0.653893 0.322621 0.296823 0.028 Uiso calc U R 1 C C16 0.4905(2) 0.43264(13) 0.32485(13) 0.0160(6) Uani d . . 1 C C17 0.5313(2) 0.42932(14) 0.38578(13) 0.0217(6) Uani d . . 1 H H17 0.596685 0.427748 0.389313 0.026 Uiso calc U R 1 C C18 0.4774(2) 0.42830(15) 0.44171(14) 0.0259(7) Uani d . . 1 H H18 0.505816 0.425545 0.483176 0.031 Uiso calc U R 1 C C19 0.3826(2) 0.43129(15) 0.43656(14) 0.0250(7) Uani d . . 1 H H19 0.345571 0.430813 0.474606 0.03 Uiso calc U R 1 C C20 0.3413(2) 0.43498(16) 0.37637(15) 0.0261(7) Uani d . . 1 H H20 0.275995 0.436959 0.373085 0.031 Uiso calc U R 1 C C21 0.3949(2) 0.43580(15) 0.32064(14) 0.0219(6) Uani d . . 1 H H21 0.366073 0.438534 0.279332 0.026 Uiso calc U R 1 C C22 0.52853(19) 0.28479(12) -0.00290(12) 0.0114(5) Uani d . . 1 C C23 0.59382(19) 0.22977(13) 0.01672(12) 0.0136(6) Uani d . . 1 C C24 0.5614(2) 0.17036(12) 0.04426(12) 0.0170(6) Uani d . . 1 H H24 0.497255 0.165114 0.052412 0.02 Uiso calc U R 1 C C25 0.6217(2) 0.11890(14) 0.05986(13) 0.0220(7) Uani d . . 1 H H25 0.598733 0.078172 0.077792 0.026 Uiso calc U R 1 C C26 0.7151(2) 0.12673(15) 0.04936(14) 0.0257(7) Uani d . . 1 H H26 0.756564 0.091439 0.060222 0.031 Uiso calc U R 1 C C27 0.7486(2) 0.18598(16) 0.02302(13) 0.0223(7) Uani d . . 1 H H27 0.81305 0.191775 0.016659 0.027 Uiso calc U R 1 C C28 0.6877(2) 0.23688(14) 0.00592(13) 0.0176(6) Uani d . . 1 H H28 0.710649 0.276953 -0.013344 0.021 Uiso calc U R 1 C C29 0.51383(19) 0.29403(13) -0.07425(13) 0.0134(6) Uani d . . 1 C C30 0.5173(2) 0.23896(14) -0.11553(13) 0.0174(6) Uani d . . 1 H H30 0.536556 0.196503 -0.099243 0.021 Uiso calc U R 1 C C31 0.4929(2) 0.24531(15) -0.18063(13) 0.0202(6) Uani d . . 1 H H31 0.493813 0.206964 -0.208131 0.024 Uiso calc U R 1 C C32 0.4676(2) 0.30694(15) -0.20520(14) 0.0214(6) Uani d . . 1 H H32 0.450851 0.311331 -0.24956 0.026 Uiso calc U R 1 C C33 0.4668(2) 0.36258(15) -0.16470(14) 0.0227(7) Uani d . . 1 H H33 0.450944 0.405417 -0.181827 0.027 Uiso calc U R 1 C C34 0.4887(2) 0.35648(14) -0.09950(14) 0.0189(6) Uani d . . 1 H H34 0.486589 0.394824 -0.072034 0.023 Uiso calc U R 1 Br Br2 0.42273(2) 0.53918(2) -0.10211(2) 0.02540(8) Uani d . . 1 P P2 0.54011(5) 0.68862(3) 0.21028(3) 0.01320(15) Uani d . . 1 O O2 0.50398(14) 0.75693(9) 0.22480(9) 0.0188(4) Uani d . . 1 N N3 0.45876(16) 0.63142(11) 0.21148(11) 0.0136(5) Uani d . . 1 H H3 0.476(2) 0.5929(16) 0.2142(14) 0.016 Uiso d U . 1 N N4 0.20560(16) 0.63195(11) 0.18501(10) 0.0154(5) Uani d . . 1 C C35 0.37134(19) 0.64309(13) 0.17765(13) 0.0133(6) Uani d . . 1 H H35 0.361444 0.692819 0.175373 0.016 Uiso calc U R 1 C C36 0.29183(19) 0.61301(14) 0.21719(13) 0.0168(6) Uani d . . 1 H H36 0.297657 0.562925 0.219032 0.02 Uiso calc U R 1 C C37 0.2885(2) 0.64207(18) 0.28547(14) 0.0290(8) Uani d . . 1 H H37A 0.279636 0.690882 0.283071 0.043 Uiso calc U R 1 H H37B 0.346529 0.632235 0.30793 0.043 Uiso calc U R 1 H H37C 0.237015 0.621807 0.30938 0.043 Uiso calc U R 1 C C38 0.37365(18) 0.61661(13) 0.10884(13) 0.0133(5) Uani d . . 1 C C39 0.3652(2) 0.65986(13) 0.05613(14) 0.0188(6) Uani d . . 1 H H39 0.351982 0.706046 0.063424 0.023 Uiso calc U R 1 C C40 0.3758(2) 0.63668(14) -0.00695(13) 0.0207(6) Uani d . . 1 H H40 0.369368 0.666358 -0.04279 0.025 Uiso calc U R 1 C C41 0.39583(19) 0.56982(15) -0.01640(12) 0.0162(6) Uani d . . 1 C C42 0.40101(19) 0.52475(13) 0.03420(13) 0.0173(6) Uani d . . 1 H H42 0.412188 0.478371 0.026334 0.021 Uiso calc U R 1 C C43 0.38952(19) 0.54862(13) 0.09690(13) 0.0165(6) Uani d . . 1 H H43 0.392516 0.5181 0.132307 0.02 Uiso calc U R 1 C C44 0.59511(19) 0.68937(13) 0.13141(13) 0.0154(6) Uani d . . 1 C C45 0.6145(2) 0.75027(14) 0.10160(14) 0.0218(6) Uani d . . 1 H H45 0.60296 0.791201 0.123954 0.026 Uiso calc U R 1 C C46 0.6508(2) 0.75174(15) 0.03906(15) 0.0277(7) Uani d . . 1 H H46 0.665243 0.793548 0.019166 0.033 Uiso calc U R 1 C C47 0.6660(2) 0.69191(16) 0.00581(15) 0.0256(7) Uani d . . 1 H H47 0.689522 0.692742 -0.037208 0.031 Uiso calc U R 1 C C48 0.6466(2) 0.63096(15) 0.03571(14) 0.0221(7) Uani d . . 1 H H48 0.656955 0.590069 0.012994 0.027 Uiso calc U R 1 C C49 0.61226(19) 0.62933(14) 0.09842(14) 0.0182(6) Uani d . . 1 H H49 0.600402 0.587419 0.118936 0.022 Uiso calc U R 1 C C50 0.62405(19) 0.65781(13) 0.26752(13) 0.0145(6) Uani d . . 1 C C51 0.7169(2) 0.67345(14) 0.26035(14) 0.0201(6) Uani d . . 1 H H51 0.737185 0.6964 0.22251 0.024 Uiso calc U R 1 C C52 0.7804(2) 0.65597(15) 0.30777(16) 0.0263(7) Uani d . . 1 H H52 0.84362 0.667464 0.302735 0.032 Uiso calc U R 1 C C53 0.7512(2) 0.62168(15) 0.36248(15) 0.0258(7) Uani d . . 1 H H53 0.794668 0.609397 0.394871 0.031 Uiso calc U R 1 C C54 0.6591(2) 0.60517(15) 0.37036(15) 0.0221(7) Uani d . . 1 H H54 0.639481 0.581489 0.407946 0.027 Uiso calc U R 1 C C55 0.5956(2) 0.62333(13) 0.32313(13) 0.0174(6) Uani d . . 1 H H55 0.532266 0.612258 0.328627 0.021 Uiso calc U R 1 C C56 0.14613(19) 0.58828(14) 0.16787(13) 0.0153(6) Uani d . . 1 C C57 0.15487(19) 0.51370(14) 0.17462(13) 0.0152(6) Uani d . . 1 C C58 0.1614(2) 0.48187(15) 0.23486(13) 0.0200(6) Uani d . . 1 H H58 0.159553 0.508028 0.273409 0.024 Uiso calc U R 1 C C59 0.1704(2) 0.41274(15) 0.23911(14) 0.0219(7) Uani d . . 1 H H59 0.173201 0.391643 0.280426 0.026 Uiso calc U R 1 C C60 0.1755(2) 0.37441(15) 0.18343(14) 0.0201(6) Uani d . . 1 H H60 0.183481 0.32708 0.186402 0.024 Uiso calc U R 1 C C61 0.1688(2) 0.40502(14) 0.12298(14) 0.0202(6) Uani d . . 1 H H61 0.171594 0.378641 0.084602 0.024 Uiso calc U R 1 C C62 0.1580(2) 0.47415(14) 0.11889(13) 0.0176(6) Uani d . . 1 H H62 0.15268 0.494844 0.077515 0.021 Uiso calc U R 1 C C63 0.05849(19) 0.61407(14) 0.13839(12) 0.0176(6) Uani d . . 1 C C64 -0.0240(2) 0.58024(15) 0.14632(15) 0.0230(7) Uani d . . 1 H H64 -0.024697 0.537723 0.167352 0.028 Uiso calc U R 1 C C65 -0.1060(2) 0.60797(18) 0.12373(17) 0.0343(8) Uani d . . 1 H H65 -0.162677 0.584932 0.130221 0.041 Uiso calc U R 1 C C66 -0.1050(2) 0.66854(18) 0.09210(18) 0.0367(9) Uani d . . 1 H H66 -0.161062 0.687437 0.076708 0.044 Uiso calc U R 1 C C67 -0.0221(3) 0.70261(18) 0.08236(18) 0.0360(9) Uani d . . 1 H H67 -0.02128 0.744166 0.059611 0.043 Uiso calc U R 1 C C68 0.0588(2) 0.67552(14) 0.10600(14) 0.0241(6) Uani d . . 1 H H68 0.115316 0.699008 0.100127 0.029 Uiso calc U R 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.01623(15) 0.02508(15) 0.04428(18) -0.00298(13) 0.00885(15) -0.00618(14) P1 0.0160(4) 0.0099(3) 0.0136(3) 0.0009(3) -0.0014(3) -0.0006(3) O1 0.0258(12) 0.0103(9) 0.0196(10) 0.0011(8) -0.0008(8) 0.0000(8) N1 0.0197(14) 0.0095(10) 0.0105(11) -0.0006(10) -0.0019(9) 0.0025(9) N2 0.0154(13) 0.0147(11) 0.0115(11) 0.0004(9) -0.0023(9) 0.0009(9) C1 0.0142(15) 0.0101(12) 0.0121(13) 0.0011(10) -0.0012(11) 0.0008(10) C2 0.0148(15) 0.0119(12) 0.0131(12) 0.0017(11) -0.0014(11) 0.0007(11) C3 0.0158(15) 0.0161(14) 0.0159(13) -0.0011(11) -0.0010(11) 0.0014(11) C4 0.0151(15) 0.0121(13) 0.0125(13) 0.0008(11) -0.0007(11) -0.0027(10) C5 0.0165(15) 0.0164(14) 0.0235(15) 0.0042(11) 0.0013(12) 0.0026(11) C6 0.0205(16) 0.0167(14) 0.0311(16) -0.0016(12) 0.0059(13) 0.0056(13) C7 0.0113(15) 0.0192(14) 0.0253(15) -0.0027(11) 0.0046(12) -0.0065(12) C8 0.0159(16) 0.0199(14) 0.0208(15) 0.0048(12) -0.0021(12) -0.0014(12) C9 0.0192(16) 0.0140(13) 0.0185(14) 0.0004(12) -0.0008(12) 0.0020(11) C10 0.0158(15) 0.0207(15) 0.0156(14) 0.0015(12) -0.0017(11) -0.0041(11) C11 0.0230(18) 0.0252(16) 0.0311(17) -0.0040(13) 0.0019(13) -0.0083(14) C12 0.0200(19) 0.048(2) 0.055(2) -0.0103(17) 0.0004(17) -0.0142(19) C13 0.0175(19) 0.056(2) 0.051(2) 0.0074(17) -0.0136(16) -0.019(2) C14 0.030(2) 0.039(2) 0.0318(19) 0.0134(16) -0.0109(15) -0.0045(15) C15 0.0248(18) 0.0242(15) 0.0221(15) 0.0037(13) -0.0066(13) 0.0004(13) C16 0.0216(16) 0.0089(12) 0.0174(14) 0.0002(12) -0.0008(11) -0.0011(11) C17 0.0259(16) 0.0213(14) 0.0180(15) -0.0009(13) -0.0034(12) -0.0009(12) C18 0.041(2) 0.0213(14) 0.0151(14) -0.0039(15) -0.0020(14) -0.0029(13) C19 0.037(2) 0.0180(14) 0.0195(15) -0.0039(14) 0.0097(14) -0.0057(13) C20 0.0225(17) 0.0276(16) 0.0281(16) 0.0022(14) 0.0067(13) -0.0056(14) C21 0.0242(17) 0.0237(15) 0.0177(14) 0.0017(13) -0.0018(12) -0.0051(12) C22 0.0113(14) 0.0105(12) 0.0124(12) -0.0030(10) -0.0001(10) 0.0010(10) C23 0.0147(16) 0.0163(13) 0.0099(12) 0.0019(11) -0.0019(11) -0.0035(10) C24 0.0195(16) 0.0164(13) 0.0150(13) 0.0014(12) -0.0010(12) -0.0027(10) C25 0.0336(19) 0.0182(14) 0.0142(13) 0.0035(13) 0.0001(13) -0.0006(12) C26 0.0328(19) 0.0311(17) 0.0133(14) 0.0185(14) -0.0046(13) -0.0040(13) C27 0.0146(16) 0.0371(18) 0.0153(14) 0.0076(13) -0.0003(12) -0.0039(13) C28 0.0166(16) 0.0218(15) 0.0143(13) 0.0002(12) 0.0003(12) -0.0016(12) C29 0.0090(14) 0.0175(13) 0.0136(13) 0.0000(11) 0.0014(10) 0.0014(11) C30 0.0167(16) 0.0171(13) 0.0185(15) -0.0011(11) -0.0018(11) 0.0019(11) C31 0.0190(17) 0.0258(15) 0.0159(14) -0.0019(13) -0.0024(12) -0.0026(12) C32 0.0157(15) 0.0338(17) 0.0147(13) 0.0022(13) -0.0024(12) 0.0053(13) C33 0.0248(17) 0.0231(15) 0.0201(15) 0.0079(13) 0.0006(13) 0.0057(12) C34 0.0201(16) 0.0181(14) 0.0184(14) 0.0053(12) 0.0009(13) 0.0001(12) Br2 0.03210(18) 0.03149(15) 0.01261(12) 0.00513(14) 0.00021(13) -0.00279(12) P2 0.0135(4) 0.0111(3) 0.0150(3) 0.0000(3) -0.0009(3) -0.0023(3) O2 0.0203(12) 0.0137(9) 0.0224(11) 0.0015(8) -0.0025(9) -0.0056(8) N3 0.0127(12) 0.0108(11) 0.0174(11) 0.0022(9) -0.0014(9) -0.0008(9) N4 0.0127(13) 0.0200(12) 0.0137(11) 0.0031(10) -0.0002(9) -0.0035(9) C35 0.0120(14) 0.0128(13) 0.0150(13) 0.0026(11) -0.0019(11) -0.0020(11) C36 0.0143(15) 0.0223(14) 0.0139(13) -0.0008(12) -0.0009(11) -0.0006(11) C37 0.0184(17) 0.053(2) 0.0155(15) 0.0002(15) -0.0016(13) -0.0060(15) C38 0.0094(14) 0.0149(13) 0.0157(13) -0.0009(11) -0.0016(11) -0.0012(11) C39 0.0224(16) 0.0132(13) 0.0209(14) 0.0029(11) -0.0022(13) 0.0012(12) C40 0.0261(17) 0.0213(15) 0.0148(14) 0.0012(13) -0.0012(12) 0.0068(12) C41 0.0149(14) 0.0232(14) 0.0106(12) 0.0007(12) -0.0009(10) -0.0033(11) C42 0.0193(16) 0.0149(13) 0.0175(13) 0.0029(11) -0.0030(11) -0.0024(11) C43 0.0207(15) 0.0143(13) 0.0146(13) 0.0015(11) -0.0020(12) 0.0035(11) C44 0.0120(15) 0.0175(13) 0.0166(12) 0.0000(11) -0.0007(11) -0.0019(11) C45 0.0254(17) 0.0175(14) 0.0226(14) 0.0000(12) 0.0012(13) 0.0001(12) C46 0.036(2) 0.0232(16) 0.0241(16) -0.0006(14) 0.0026(14) 0.0084(13) C47 0.0269(18) 0.0318(17) 0.0182(15) 0.0053(14) 0.0025(13) 0.0055(13) C48 0.0229(17) 0.0218(15) 0.0217(15) 0.0054(13) 0.0028(12) -0.0044(12) C49 0.0148(15) 0.0166(14) 0.0232(14) 0.0001(11) 0.0000(12) 0.0030(12) C50 0.0163(15) 0.0114(13) 0.0158(14) 0.0001(11) -0.0025(11) -0.0047(10) C51 0.0168(16) 0.0191(14) 0.0244(15) -0.0013(12) -0.0017(12) 0.0016(12) C52 0.0143(17) 0.0264(16) 0.0382(19) -0.0007(13) -0.0038(14) -0.0023(14) C53 0.0242(18) 0.0248(16) 0.0284(17) 0.0026(13) -0.0119(14) -0.0046(13) C54 0.0235(17) 0.0230(15) 0.0199(14) 0.0031(13) -0.0038(13) -0.0024(12) C55 0.0150(16) 0.0191(14) 0.0180(13) 0.0003(11) -0.0007(11) -0.0027(11) C56 0.0139(15) 0.0214(15) 0.0105(13) 0.0001(11) 0.0034(11) -0.0036(11) C57 0.0088(14) 0.0221(14) 0.0147(13) 0.0002(11) 0.0013(11) -0.0019(11) C58 0.0238(17) 0.0243(15) 0.0119(13) -0.0013(13) -0.0003(12) -0.0033(11) C59 0.0225(17) 0.0258(16) 0.0173(14) -0.0026(13) -0.0006(12) 0.0036(12) C60 0.0178(16) 0.0173(14) 0.0253(15) 0.0007(12) -0.0009(12) -0.0012(12) C61 0.0194(16) 0.0240(15) 0.0172(14) -0.0004(12) 0.0007(12) -0.0061(12) C62 0.0165(16) 0.0230(15) 0.0132(13) -0.0006(12) -0.0003(11) -0.0010(11) C63 0.0151(16) 0.0228(14) 0.0150(13) 0.0034(12) 0.0003(11) -0.0080(11) C64 0.0170(16) 0.0250(16) 0.0272(16) -0.0001(13) -0.0017(13) -0.0090(13) C65 0.0146(17) 0.042(2) 0.046(2) 0.0022(15) -0.0069(15) -0.0147(17) C66 0.0218(19) 0.041(2) 0.048(2) 0.0146(15) -0.0150(16) -0.0078(17) C67 0.034(2) 0.0323(18) 0.042(2) 0.0100(16) -0.0135(16) 0.0040(15) C68 0.0211(17) 0.0269(15) 0.0242(14) 0.0002(13) -0.0052(14) -0.0002(13) 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' Br Br -0.2901 2.4595 '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' P P 0.1023 0.0942 '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 O1 P1 N1 111.04(11) O1 P1 C10 111.65(13) N1 P1 C10 110.05(12) O1 P1 C16 113.81(12) N1 P1 C16 104.09(12) C10 P1 C16 105.82(13) C1 N1 P1 121.13(18) C1 N1 H1 115.(2) P1 N1 H1 121.(2) C22 N2 C2 121.7(2) N1 C1 C4 113.2(2) N1 C1 C2 109.2(2) C4 C1 C2 111.3(2) N1 C1 H1A 107.6 C4 C1 H1A 107.6 C2 C1 H1A 107.6 N2 C2 C3 106.6(2) N2 C2 C1 106.9(2) C3 C2 C1 112.2(2) N2 C2 H2 110.3 C3 C2 H2 110.3 C1 C2 H2 110.3 C2 C3 H3A 109.5 C2 C3 H3B 109.5 H3A C3 H3B 109.5 C2 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 C5 C4 C9 118.4(3) C5 C4 C1 120.5(2) C9 C4 C1 121.0(2) C4 C5 C6 121.0(3) C4 C5 H5 119.5 C6 C5 H5 119.5 C7 C6 C5 118.5(3) C7 C6 H6 120.8 C5 C6 H6 120.8 C8 C7 C6 122.2(3) C8 C7 Br1 119.3(2) C6 C7 Br1 118.5(2) C7 C8 C9 118.3(3) C7 C8 H8 120.8 C9 C8 H8 120.8 C8 C9 C4 121.5(3) C8 C9 H9 119.2 C4 C9 H9 119.2 C11 C10 C15 119.2(3) C11 C10 P1 120.6(2) C15 C10 P1 120.1(2) C10 C11 C12 119.6(3) C10 C11 H11 120.2 C12 C11 H11 120.2 C13 C12 C11 120.3(3) C13 C12 H12 119.8 C11 C12 H12 119.8 C12 C13 C14 120.6(3) C12 C13 H13 119.7 C14 C13 H13 119.7 C15 C14 C13 119.7(3) C15 C14 H14 120.1 C13 C14 H14 120.1 C14 C15 C10 120.5(3) C14 C15 H15 119.7 C10 C15 H15 119.7 C21 C16 C17 118.9(3) C21 C16 P1 117.7(2) C17 C16 P1 123.3(2) C16 C17 C18 120.7(3) C16 C17 H17 119.7 C18 C17 H17 119.7 C19 C18 C17 119.6(3) C19 C18 H18 120.2 C17 C18 H18 120.2 C20 C19 C18 120.2(3) C20 C19 H19 119.9 C18 C19 H19 119.9 C19 C20 C21 120.2(3) C19 C20 H20 119.9 C21 C20 H20 119.9 C20 C21 C16 120.4(3) C20 C21 H21 119.8 C16 C21 H21 119.8 N2 C22 C29 116.9(2) N2 C22 C23 126.7(2) C29 C22 C23 116.3(2) C28 C23 C24 118.9(3) C28 C23 C22 120.1(2) C24 C23 C22 121.0(2) C25 C24 C23 120.6(3) C25 C24 H24 119.7 C23 C24 H24 119.7 C26 C25 C24 120.0(3) C26 C25 H25 120.0 C24 C25 H25 120.0 C25 C26 C27 120.1(3) C25 C26 H26 120.0 C27 C26 H26 120.0 C26 C27 C28 119.8(3) C26 C27 H27 120.1 C28 C27 H27 120.1 C23 C28 C27 120.6(3) C23 C28 H28 119.7 C27 C28 H28 119.7 C30 C29 C34 118.9(2) C30 C29 C22 120.0(2) C34 C29 C22 120.9(2) C29 C30 C31 120.6(3) C29 C30 H30 119.7 C31 C30 H30 119.7 C32 C31 C30 120.2(3) C32 C31 H31 119.9 C30 C31 H31 119.9 C31 C32 C33 119.4(3) C31 C32 H32 120.3 C33 C32 H32 120.3 C32 C33 C34 120.8(3) C32 C33 H33 119.6 C34 C33 H33 119.6 C33 C34 C29 120.0(3) C33 C34 H34 120.0 C29 C34 H34 120.0 O2 P2 N3 112.21(12) O2 P2 C50 114.61(12) N3 P2 C50 103.87(12) O2 P2 C44 109.17(12) N3 P2 C44 109.64(12) C50 P2 C44 107.08(13) C35 N3 P2 120.34(18) C35 N3 H3 117.(2) P2 N3 H3 116.(2) C56 N4 C36 121.9(2) N3 C35 C38 111.8(2) N3 C35 C36 109.6(2) C38 C35 C36 112.3(2) N3 C35 H35 107.6 C38 C35 H35 107.6 C36 C35 H35 107.6 N4 C36 C37 107.1(2) N4 C36 C35 107.5(2) C37 C36 C35 111.6(2) N4 C36 H36 110.2 C37 C36 H36 110.2 C35 C36 H36 110.2 C36 C37 H37A 109.5 C36 C37 H37B 109.5 H37A C37 H37B 109.5 C36 C37 H37C 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 C39 C38 C43 118.5(2) C39 C38 C35 121.0(2) C43 C38 C35 120.5(2) C40 C39 C38 121.1(2) C40 C39 H39 119.4 C38 C39 H39 119.4 C41 C40 C39 118.5(3) C41 C40 H40 120.7 C39 C40 H40 120.7 C40 C41 C42 122.2(2) C40 C41 Br2 118.9(2) C42 C41 Br2 118.8(2) C41 C42 C43 118.5(2) C41 C42 H42 120.8 C43 C42 H42 120.8 C42 C43 C38 121.1(2) C42 C43 H43 119.5 C38 C43 H43 119.5 C45 C44 C49 119.6(3) C45 C44 P2 119.6(2) C49 C44 P2 120.6(2) C44 C45 C46 120.3(3) C44 C45 H45 119.8 C46 C45 H45 119.8 C47 C46 C45 119.9(3) C47 C46 H46 120.1 C45 C46 H46 120.1 C48 C47 C46 119.7(3) C48 C47 H47 120.1 C46 C47 H47 120.1 C49 C48 C47 120.5(3) C49 C48 H48 119.8 C47 C48 H48 119.8 C48 C49 C44 119.9(3) C48 C49 H49 120.1 C44 C49 H49 120.1 C51 C50 C55 118.9(3) C51 C50 P2 120.5(2) C55 C50 P2 120.3(2) C52 C51 C50 120.8(3) C52 C51 H51 119.6 C50 C51 H51 119.6 C53 C52 C51 119.7(3) C53 C52 H52 120.2 C51 C52 H52 120.2 C54 C53 C52 120.5(3) C54 C53 H53 119.8 C52 C53 H53 119.7 C53 C54 C55 119.7(3) C53 C54 H54 120.1 C55 C54 H54 120.1 C54 C55 C50 120.5(3) C54 C55 H55 119.8 C50 C55 H55 119.8 N4 C56 C57 126.4(3) N4 C56 C63 116.9(2) C57 C56 C63 116.7(2) C62 C57 C58 118.4(3) C62 C57 C56 119.1(2) C58 C57 C56 122.5(2) C59 C58 C57 120.9(3) C59 C58 H58 119.6 C57 C58 H58 119.6 C60 C59 C58 120.1(3) C60 C59 H59 120.0 C58 C59 H59 120.0 C59 C60 C61 120.0(3) C59 C60 H60 120.0 C61 C60 H60 120.0 C62 C61 C60 119.8(3) C62 C61 H61 120.1 C60 C61 H61 120.1 C61 C62 C57 120.9(3) C61 C62 H62 119.6 C57 C62 H62 119.6 C64 C63 C68 119.1(3) C64 C63 C56 121.2(3) C68 C63 C56 119.5(3) C63 C64 C65 120.4(3) C63 C64 H64 119.8 C65 C64 H64 119.8 C66 C65 C64 119.9(3) C66 C65 H65 120.0 C64 C65 H65 120.0 C65 C66 C67 120.4(3) C65 C66 H66 119.8 C67 C66 H66 119.8 C68 C67 C66 119.5(3) C68 C67 H67 120.3 C66 C67 H67 120.3 C67 C68 C63 120.6(3) C67 C68 H68 119.7 C63 C68 H68 119.7 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C7 1.901(3) P1 O1 1.4844(19) P1 N1 1.640(2) P1 C10 1.802(3) P1 C16 1.809(3) N1 C1 1.468(3) N1 H1 0.81(3) N2 C22 1.278(3) N2 C2 1.470(3) C1 C4 1.516(4) C1 C2 1.535(4) C1 H1A 1.0 C2 C3 1.517(4) C2 H2 1.0 C3 H3A 0.98 C3 H3B 0.98 C3 H3C 0.98 C4 C5 1.388(4) C4 C9 1.391(4) C5 C6 1.390(4) C5 H5 0.95 C6 C7 1.379(4) C6 H6 0.95 C7 C8 1.378(4) C8 C9 1.381(4) C8 H8 0.95 C9 H9 0.95 C10 C11 1.391(4) C10 C15 1.403(4) C11 C12 1.392(5) C11 H11 0.95 C12 C13 1.377(5) C12 H12 0.95 C13 C14 1.379(5) C13 H13 0.95 C14 C15 1.378(4) C14 H14 0.95 C15 H15 0.95 C16 C21 1.389(4) C16 C17 1.390(4) C17 C18 1.393(4) C17 H17 0.95 C18 C19 1.379(4) C18 H18 0.95 C19 C20 1.379(4) C19 H19 0.95 C20 C21 1.386(4) C20 H20 0.95 C21 H21 0.95 C22 C29 1.497(4) C22 C23 1.502(4) C23 C28 1.386(4) C23 C24 1.392(4) C24 C25 1.383(4) C24 H24 0.95 C25 C26 1.380(4) C25 H25 0.95 C26 C27 1.385(4) C26 H26 0.95 C27 C28 1.387(4) C27 H27 0.95 C28 H28 0.95 C29 C30 1.388(4) C29 C34 1.395(4) C30 C31 1.393(4) C30 H30 0.95 C31 C32 1.376(4) C31 H31 0.95 C32 C33 1.386(4) C32 H32 0.95 C33 C34 1.386(4) C33 H33 0.95 C34 H34 0.95 Br2 C41 1.909(3) P2 O2 1.486(2) P2 N3 1.638(2) P2 C50 1.802(3) P2 C44 1.810(3) N3 C35 1.464(3) N3 H3 0.81(3) N4 C56 1.273(3) N4 C36 1.464(4) C35 C38 1.513(4) C35 C36 1.532(4) C35 H35 1.0 C36 C37 1.522(4) C36 H36 1.0 C37 H37A 0.98 C37 H37B 0.98 C37 H37C 0.98 C38 C39 1.391(4) C38 C43 1.393(4) C39 C40 1.388(4) C39 H39 0.95 C40 C41 1.374(4) C40 H40 0.95 C41 C42 1.377(4) C42 C43 1.387(4) C42 H42 0.95 C43 H43 0.95 C44 C45 1.386(4) C44 C49 1.396(4) C45 C46 1.393(4) C45 H45 0.95 C46 C47 1.390(4) C46 H46 0.95 C47 C48 1.388(4) C47 H47 0.95 C48 C49 1.385(4) C48 H48 0.95 C49 H49 0.95 C50 C51 1.389(4) C50 C55 1.398(4) C51 C52 1.386(4) C51 H51 0.95 C52 C53 1.384(4) C52 H52 0.95 C53 C54 1.383(4) C53 H53 0.95 C54 C55 1.388(4) C54 H54 0.95 C55 H55 0.95 C56 C57 1.495(4) C56 C63 1.498(4) C57 C62 1.393(4) C57 C58 1.397(4) C58 C59 1.383(4) C58 H58 0.95 C59 C60 1.380(4) C59 H59 0.95 C60 C61 1.390(4) C60 H60 0.95 C61 C62 1.386(4) C61 H61 0.95 C62 H62 0.95 C63 C64 1.381(4) C63 C68 1.392(4) C64 C65 1.390(4) C64 H64 0.95 C65 C66 1.369(5) C65 H65 0.95 C66 C67 1.393(5) C66 H66 0.95 C67 C68 1.379(4) C67 H67 0.95 C68 H68 0.95 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1 O2 3_645 0.81(3) 2.02(3) 2.814(3) 168.(3) N3 H3 O1 . 0.81(3) 2.03(3) 2.827(3) 167.(3) 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 O1 P1 N1 C1 35.6(2) C10 P1 N1 C1 -88.5(2) C16 P1 N1 C1 158.4(2) P1 N1 C1 C4 52.6(3) P1 N1 C1 C2 177.31(18) C22 N2 C2 C3 -122.8(3) C22 N2 C2 C1 117.1(3) N1 C1 C2 N2 170.8(2) C4 C1 C2 N2 -63.4(3) N1 C1 C2 C3 54.3(3) C4 C1 C2 C3 180.0(2) N1 C1 C4 C5 -123.1(3) C2 C1 C4 C5 113.4(3) N1 C1 C4 C9 55.8(3) C2 C1 C4 C9 -67.7(3) C9 C4 C5 C6 -1.2(4) C1 C4 C5 C6 177.7(3) C4 C5 C6 C7 -1.1(4) C5 C6 C7 C8 2.4(4) C5 C6 C7 Br1 -176.7(2) C6 C7 C8 C9 -1.4(4) Br1 C7 C8 C9 177.7(2) C7 C8 C9 C4 -1.0(4) C5 C4 C9 C8 2.3(4) C1 C4 C9 C8 -176.7(2) O1 P1 C10 C11 9.1(3) N1 P1 C10 C11 132.9(2) C16 P1 C10 C11 -115.2(2) O1 P1 C10 C15 -167.9(2) N1 P1 C10 C15 -44.1(3) C16 P1 C10 C15 67.7(3) C15 C10 C11 C12 -0.4(4) P1 C10 C11 C12 -177.5(3) C10 C11 C12 C13 0.8(5) C11 C12 C13 C14 -0.7(6) C12 C13 C14 C15 0.2(6) C13 C14 C15 C10 0.2(5) C11 C10 C15 C14 -0.1(4) P1 C10 C15 C14 177.0(2) O1 P1 C16 C21 64.7(3) N1 P1 C16 C21 -56.3(3) C10 P1 C16 C21 -172.3(2) O1 P1 C16 C17 -111.1(2) N1 P1 C16 C17 127.9(2) C10 P1 C16 C17 11.9(3) C21 C16 C17 C18 0.8(4) P1 C16 C17 C18 176.6(2) C16 C17 C18 C19 -0.7(5) C17 C18 C19 C20 0.3(5) C18 C19 C20 C21 -0.1(5) C19 C20 C21 C16 0.3(5) C17 C16 C21 C20 -0.6(5) P1 C16 C21 C20 -176.6(2) C2 N2 C22 C29 174.4(2) C2 N2 C22 C23 -2.6(4) N2 C22 C23 C28 -112.0(3) C29 C22 C23 C28 71.0(3) N2 C22 C23 C24 69.7(4) C29 C22 C23 C24 -107.3(3) C28 C23 C24 C25 -0.8(4) C22 C23 C24 C25 177.5(2) C23 C24 C25 C26 1.3(4) C24 C25 C26 C27 -0.2(4) C25 C26 C27 C28 -1.4(4) C24 C23 C28 C27 -0.8(4) C22 C23 C28 C27 -179.1(2) C26 C27 C28 C23 1.9(4) N2 C22 C29 C30 -144.8(3) C23 C22 C29 C30 32.5(4) N2 C22 C29 C34 29.6(4) C23 C22 C29 C34 -153.1(3) C34 C29 C30 C31 -2.3(4) C22 C29 C30 C31 172.2(3) C29 C30 C31 C32 1.9(4) C30 C31 C32 C33 0.1(5) C31 C32 C33 C34 -1.7(5) C32 C33 C34 C29 1.3(5) C30 C29 C34 C33 0.7(4) C22 C29 C34 C33 -173.8(3) O2 P2 N3 C35 47.0(2) C50 P2 N3 C35 171.39(19) C44 P2 N3 C35 -74.4(2) P2 N3 C35 C38 91.7(2) P2 N3 C35 C36 -143.15(19) C56 N4 C36 C37 -114.6(3) C56 N4 C36 C35 125.4(3) N3 C35 C36 N4 174.2(2) C38 C35 C36 N4 -60.8(3) N3 C35 C36 C37 57.1(3) C38 C35 C36 C37 -177.9(2) N3 C35 C38 C39 -116.4(3) C36 C35 C38 C39 119.9(3) N3 C35 C38 C43 59.9(3) C36 C35 C38 C43 -63.7(3) C43 C38 C39 C40 -2.5(4) C35 C38 C39 C40 174.0(3) C38 C39 C40 C41 -0.6(4) C39 C40 C41 C42 3.4(4) C39 C40 C41 Br2 -173.8(2) C40 C41 C42 C43 -2.9(4) Br2 C41 C42 C43 174.3(2) C41 C42 C43 C38 -0.4(4) C39 C38 C43 C42 3.0(4) C35 C38 C43 C42 -173.5(3) O2 P2 C44 C45 13.1(3) N3 P2 C44 C45 136.4(2) C50 P2 C44 C45 -111.5(2) O2 P2 C44 C49 -162.4(2) N3 P2 C44 C49 -39.1(3) C50 P2 C44 C49 73.0(3) C49 C44 C45 C46 0.1(4) P2 C44 C45 C46 -175.5(2) C44 C45 C46 C47 1.3(5) C45 C46 C47 C48 -1.4(5) C46 C47 C48 C49 0.0(5) C47 C48 C49 C44 1.4(4) C45 C44 C49 C48 -1.4(4) P2 C44 C49 C48 174.1(2) O2 P2 C50 C51 -86.1(2) N3 P2 C50 C51 151.1(2) C44 P2 C50 C51 35.2(2) O2 P2 C50 C55 87.7(2) N3 P2 C50 C55 -35.0(2) C44 P2 C50 C55 -151.0(2) C55 C50 C51 C52 -0.8(4) P2 C50 C51 C52 173.1(2) C50 C51 C52 C53 0.9(4) C51 C52 C53 C54 -0.4(5) C52 C53 C54 C55 -0.2(4) C53 C54 C55 C50 0.4(4) C51 C50 C55 C54 0.1(4) P2 C50 C55 C54 -173.8(2) C36 N4 C56 C57 -2.6(4) C36 N4 C56 C63 177.0(2) N4 C56 C57 C62 -115.5(3) C63 C56 C57 C62 64.8(3) N4 C56 C57 C58 63.5(4) C63 C56 C57 C58 -116.1(3) C62 C57 C58 C59 -0.2(4) C56 C57 C58 C59 -179.3(3) C57 C58 C59 C60 1.6(5) C58 C59 C60 C61 -1.8(5) C59 C60 C61 C62 0.6(5) C60 C61 C62 C57 0.8(5) C58 C57 C62 C61 -1.0(4) C56 C57 C62 C61 178.1(3) N4 C56 C63 C64 -148.5(3) C57 C56 C63 C64 31.1(4) N4 C56 C63 C68 27.2(4) C57 C56 C63 C68 -153.1(3) C68 C63 C64 C65 -1.6(4) C56 C63 C64 C65 174.1(3) C63 C64 C65 C66 1.5(5) C64 C65 C66 C67 0.0(5) C65 C66 C67 C68 -1.3(5) C66 C67 C68 C63 1.1(5) C64 C63 C68 C67 0.3(4) C56 C63 C68 C67 -175.5(3)