# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C127 H96 N12 O20 Re4 S6' _chemical_formula_sum 'C127 H96 N12 O20 Re4 S6' _chemical_formula_weight 3047.32 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 28.6866(15) _cell_length_b 18.3837(9) _cell_length_c 25.0892(14) _cell_angle_alpha 90.00 _cell_angle_beta 111.660(6) _cell_angle_gamma 90.00 _cell_volume 12296.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6554 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 28.46 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5992 _exptl_absorpt_coefficient_mu 4.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3631 _exptl_absorpt_correction_T_max 0.5258 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur Sapphire3' _diffrn_measurement_method 'w scan' _diffrn_detector_area_resol_mean 15.9853 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 180182 _diffrn_reflns_av_R_equivalents 0.1379 _diffrn_reflns_av_unetI/netI 0.1040 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 26.37 _reflns_number_total 25113 _reflns_number_gt 15657 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_data_reduction 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+31.3274P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25113 _refine_ls_number_parameters 1494 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1214 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1862 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.078 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3300(5) 0.1806(7) 0.2903(5) 0.052(3) Uani 1 1 d . . . C2 C 0.3263(4) 0.0456(7) 0.3235(5) 0.047(3) Uani 1 1 d . . . C3 C 0.3832(4) 0.1404(6) 0.3935(5) 0.048(3) Uani 1 1 d . . . C4 C 0.5905(5) 0.0520(8) 0.0831(5) 0.056(3) Uani 1 1 d . . . C5 C 0.6446(5) 0.1469(8) 0.1552(5) 0.061(4) Uani 1 1 d . . . C6 C 0.5603(5) 0.1863(8) 0.0759(6) 0.060(4) Uani 1 1 d . . . C7 C 0.4128(4) 0.0780(5) 0.2182(4) 0.034(2) Uani 1 1 d . . . C8 C 0.4002(4) 0.0385(5) 0.1641(4) 0.031(2) Uani 1 1 d . . . C9 C 0.3558(4) -0.0009(6) 0.1429(5) 0.046(3) Uani 1 1 d . . . H9 H 0.3348 -0.0026 0.1636 0.055 Uiso 1 1 calc R . . C10 C 0.3428(4) -0.0367(6) 0.0924(5) 0.050(3) Uani 1 1 d . . . H10 H 0.3123 -0.0609 0.0778 0.060 Uiso 1 1 calc R . . C11 C 0.3750(4) -0.0375(7) 0.0622(5) 0.051(3) Uani 1 1 d . . . H11 H 0.3669 -0.0644 0.0286 0.061 Uiso 1 1 calc R . . C12 C 0.4187(4) 0.0019(7) 0.0826(5) 0.051(3) Uani 1 1 d . . . H12 H 0.4399 0.0026 0.0621 0.061 Uiso 1 1 calc R . . C13 C 0.4316(4) 0.0408(5) 0.1336(4) 0.034(2) Uani 1 1 d . . . C14 C 0.4774(4) 0.0823(6) 0.1540(4) 0.036(2) Uani 1 1 d . . . C15 C 0.4902(4) 0.1245(6) 0.2063(4) 0.034(2) Uani 1 1 d . . . C16 C 0.5325(4) 0.1692(5) 0.2244(5) 0.036(3) Uani 1 1 d . . . C17 C 0.5428(4) 0.2133(6) 0.2759(5) 0.042(3) Uani 1 1 d . . . C18 C 0.5860(4) 0.2572(6) 0.2957(5) 0.051(3) Uani 1 1 d . . . H18 H 0.6075 0.2585 0.2756 0.062 Uiso 1 1 calc R . . C19 C 0.5967(5) 0.2982(7) 0.3449(6) 0.069(4) Uani 1 1 d . . . H19 H 0.6238 0.3299 0.3564 0.083 Uiso 1 1 calc R . . C20 C 0.5667(6) 0.2918(7) 0.3772(6) 0.068(4) Uani 1 1 d . . . H20 H 0.5749 0.3169 0.4117 0.082 Uiso 1 1 calc R . . C21 C 0.5251(5) 0.2488(6) 0.3583(6) 0.057(3) Uani 1 1 d . . . H21 H 0.5048 0.2460 0.3798 0.068 Uiso 1 1 calc R . . C22 C 0.5121(4) 0.2091(6) 0.3079(5) 0.040(3) Uani 1 1 d . . . C23 C 0.4676(4) 0.1639(5) 0.2882(5) 0.037(3) Uani 1 1 d . . . C24 C 0.4569(4) 0.1216(5) 0.2380(4) 0.032(2) Uani 1 1 d . . . C25 C 0.4342(4) -0.0489(6) 0.3412(5) 0.041(3) Uani 1 1 d . . . C26 C 0.5092(4) -0.0366(6) 0.4096(5) 0.045(3) Uani 1 1 d . . . C27 C 0.5563(4) -0.0464(7) 0.4536(5) 0.057(3) Uani 1 1 d . . . H27 H 0.5732 -0.0905 0.4595 0.069 Uiso 1 1 calc R . . C28 C 0.5754(5) 0.0121(7) 0.4869(6) 0.067(4) Uani 1 1 d . . . H28 H 0.6062 0.0075 0.5169 0.081 Uiso 1 1 calc R . . C29 C 0.5509(5) 0.0797(8) 0.4782(6) 0.074(4) Uani 1 1 d . . . H29 H 0.5657 0.1187 0.5020 0.089 Uiso 1 1 calc R . . C30 C 0.5051(5) 0.0885(6) 0.4347(6) 0.056(3) Uani 1 1 d . . . H30 H 0.4890 0.1334 0.4280 0.067 Uiso 1 1 calc R . . C31 C 0.3607(5) -0.1479(8) 0.3297(7) 0.092(5) Uani 1 1 d . . . H31A H 0.3880 -0.1603 0.3644 0.137 Uiso 1 1 calc R . . H31B H 0.3475 -0.1912 0.3080 0.137 Uiso 1 1 calc R . . H31C H 0.3348 -0.1245 0.3390 0.137 Uiso 1 1 calc R . . C32 C 0.4874(4) -0.1618(6) 0.3642(5) 0.047(3) Uani 1 1 d . . . H32A H 0.4612 -0.1793 0.3296 0.056 Uiso 1 1 calc R . . H32B H 0.4844 -0.1884 0.3961 0.056 Uiso 1 1 calc R . . C33 C 0.5376(4) -0.1811(6) 0.3606(5) 0.038(3) Uani 1 1 d . . . C34 C 0.5711(4) -0.2272(5) 0.4018(4) 0.037(3) Uani 1 1 d . . . C35 C 0.6148(4) -0.2479(6) 0.3944(4) 0.038(3) Uani 1 1 d . . . C36 C 0.6265(4) -0.2221(5) 0.3478(5) 0.040(3) Uani 1 1 d . . . C37 C 0.5923(4) -0.1771(5) 0.3070(4) 0.037(3) Uani 1 1 d . . . C38 C 0.5484(4) -0.1551(6) 0.3138(5) 0.044(3) Uani 1 1 d . . . C39 C 0.5595(4) -0.2561(6) 0.4514(5) 0.049(3) Uani 1 1 d . . . H39A H 0.5406 -0.3004 0.4402 0.074 Uiso 1 1 calc R . . H39B H 0.5402 -0.2209 0.4626 0.074 Uiso 1 1 calc R . . H39C H 0.5902 -0.2656 0.4830 0.074 Uiso 1 1 calc R . . C40 C 0.6756(4) -0.2433(8) 0.3439(5) 0.065(4) Uani 1 1 d . . . H40A H 0.6828 -0.2117 0.3174 0.097 Uiso 1 1 calc R . . H40B H 0.6737 -0.2927 0.3308 0.097 Uiso 1 1 calc R . . H40C H 0.7018 -0.2392 0.3811 0.097 Uiso 1 1 calc R . . C41 C 0.5098(4) -0.1075(7) 0.2681(5) 0.052(3) Uani 1 1 d . . . H41A H 0.5203 -0.0576 0.2737 0.078 Uiso 1 1 calc R . . H41B H 0.4777 -0.1122 0.2715 0.078 Uiso 1 1 calc R . . H41C H 0.5073 -0.1231 0.2306 0.078 Uiso 1 1 calc R . . C42 C 0.6478(4) -0.3056(6) 0.4327(5) 0.051(3) Uani 1 1 d . . . H42A H 0.6267 -0.3390 0.4434 0.061 Uiso 1 1 calc R . . H42B H 0.6634 -0.3329 0.4105 0.061 Uiso 1 1 calc R . . C43 C 0.7177(5) -0.3346(9) 0.5236(5) 0.131(10) Uani 1 1 d D . . C44 C 0.7196(5) -0.4047(6) 0.5245(5) 0.044(3) Uiso 1 1 d D . . H44 H 0.6966 -0.4259 0.4916 0.052 Uiso 1 1 calc R . . C45 C 0.7473(7) -0.4534(9) 0.5623(8) 0.127(8) Uani 1 1 d D . . H45 H 0.7440 -0.5037 0.5593 0.153 Uiso 1 1 calc R . . C46 C 0.7803(6) -0.4168(8) 0.6048(7) 0.090(6) Uani 1 1 d D . . H46 H 0.8034 -0.4445 0.6335 0.108 Uiso 1 1 calc R . . C47 C 0.7844(6) -0.3442(9) 0.6115(7) 0.107(6) Uani 1 1 d D . . H47 H 0.8088 -0.3236 0.6435 0.129 Uiso 1 1 calc R . . C48 C 0.7507(6) -0.3003(9) 0.5686(6) 0.091(5) Uani 1 1 d D . . C49 C 0.7066(6) -0.2151(9) 0.5088(6) 0.078(5) Uani 1 1 d . . . C50 C 0.7262(8) -0.0771(9) 0.5380(9) 0.133(8) Uani 1 1 d . . . H50A H 0.7286 -0.0972 0.5742 0.200 Uiso 1 1 calc R . . H50B H 0.7123 -0.0290 0.5341 0.200 Uiso 1 1 calc R . . H50C H 0.7590 -0.0748 0.5362 0.200 Uiso 1 1 calc R . . C51 C 0.6017(4) -0.1584(6) 0.2527(5) 0.046(3) Uani 1 1 d . . . H51A H 0.6319 -0.1829 0.2534 0.055 Uiso 1 1 calc R . . H51B H 0.5739 -0.1761 0.2196 0.055 Uiso 1 1 calc R . . C52 C 0.5871(4) -0.0397(6) 0.1963(4) 0.041(3) Uani 1 1 d . . . C53 C 0.6341(4) -0.0287(6) 0.2882(5) 0.047(3) Uani 1 1 d . . . C54 C 0.6622(5) -0.0356(8) 0.3459(5) 0.070(4) Uani 1 1 d . . . H54 H 0.6657 -0.0799 0.3649 0.084 Uiso 1 1 calc R . . C55 C 0.6843(6) 0.0246(9) 0.3728(6) 0.091(6) Uani 1 1 d . . . H55 H 0.7046 0.0214 0.4114 0.110 Uiso 1 1 calc R . . C56 C 0.6783(6) 0.0925(8) 0.3461(6) 0.079(5) Uani 1 1 d . . . H56 H 0.6943 0.1329 0.3674 0.095 Uiso 1 1 calc R . . C57 C 0.6502(5) 0.1006(7) 0.2908(5) 0.060(4) Uani 1 1 d . . . H57 H 0.6454 0.1458 0.2730 0.072 Uiso 1 1 calc R . . C58 C 0.6282(4) 0.0375(6) 0.2607(4) 0.041(3) Uani 1 1 d . . . C59 C 0.5886(6) -0.1444(8) 0.1154(6) 0.087(5) Uani 1 1 d . . . H59A H 0.6154 -0.1184 0.1096 0.130 Uiso 1 1 calc R . . H59B H 0.5698 -0.1706 0.0811 0.130 Uiso 1 1 calc R . . H59C H 0.6023 -0.1780 0.1466 0.130 Uiso 1 1 calc R . . C60 C 0.8756(6) 0.0577(7) 0.0239(5) 0.060(4) Uani 1 1 d . . . C61 C 0.9599(5) 0.0009(7) 0.0377(5) 0.050(3) Uani 1 1 d . . . C62 C 0.9478(5) 0.1399(7) 0.0122(5) 0.056(3) Uani 1 1 d . . . C63 C 1.1401(5) 0.0205(7) 0.4660(5) 0.050(3) Uani 1 1 d . . . C64 C 1.1399(5) 0.1611(7) 0.4877(5) 0.052(3) Uani 1 1 d . . . C65 C 1.0707(5) 0.0756(7) 0.4984(5) 0.052(3) Uani 1 1 d . . . C66 C 0.9492(4) -0.0141(5) 0.2355(4) 0.034(2) Uani 1 1 d . . . C67 C 0.9069(4) -0.0570(6) 0.2115(5) 0.050(3) Uani 1 1 d . . . H67 H 0.8902 -0.0588 0.1719 0.060 Uiso 1 1 calc R . . C68 C 0.8896(5) -0.0974(7) 0.2476(6) 0.068(4) Uani 1 1 d . . . H68 H 0.8610 -0.1258 0.2314 0.081 Uiso 1 1 calc R . . C69 C 0.9134(5) -0.0968(7) 0.3062(6) 0.060(4) Uani 1 1 d . . . H69 H 0.9013 -0.1242 0.3295 0.072 Uiso 1 1 calc R . . C70 C 0.9563(4) -0.0536(6) 0.3298(5) 0.041(3) Uani 1 1 d . . . H70 H 0.9729 -0.0522 0.3694 0.049 Uiso 1 1 calc R . . C71 C 0.9743(4) -0.0135(5) 0.2958(4) 0.033(2) Uani 1 1 d . . . C72 C 1.0189(4) 0.0312(5) 0.3220(4) 0.030(2) Uani 1 1 d . . . C73 C 1.0371(4) 0.0723(5) 0.2862(4) 0.033(2) Uani 1 1 d . . . C74 C 1.1042(4) 0.1473(6) 0.2731(5) 0.037(3) Uani 1 1 d . . . C75 C 1.1512(4) 0.1835(7) 0.2973(5) 0.053(3) Uani 1 1 d . . . H75 H 1.1682 0.1840 0.3368 0.064 Uiso 1 1 calc R . . C76 C 1.1715(4) 0.2175(6) 0.2622(6) 0.056(3) Uani 1 1 d . . . H76 H 1.2025 0.2405 0.2777 0.067 Uiso 1 1 calc R . . C77 C 1.0835(4) 0.1113(5) 0.3111(4) 0.032(2) Uani 1 1 d . . . C78 C 1.1453(5) 0.2174(7) 0.2033(6) 0.056(3) Uani 1 1 d . . . H78 H 1.1590 0.2413 0.1798 0.067 Uiso 1 1 calc R . . C79 C 1.1009(4) 0.1836(6) 0.1792(5) 0.043(3) Uani 1 1 d . . . H79 H 1.0844 0.1840 0.1396 0.051 Uiso 1 1 calc R . . C80 C 1.0792(4) 0.1476(5) 0.2144(5) 0.035(2) Uani 1 1 d . . . C81 C 1.0312(4) 0.1099(5) 0.1865(5) 0.034(2) Uani 1 1 d . . . C82 C 1.0119(4) 0.0717(5) 0.2241(4) 0.031(2) Uani 1 1 d . . . C83 C 0.9277(4) 0.2456(6) 0.1123(4) 0.033(2) Uani 1 1 d . . . C84 C 0.8624(4) 0.2425(7) 0.1384(5) 0.045(3) Uani 1 1 d . . . C85 C 0.8214(5) 0.2597(7) 0.1515(6) 0.061(4) Uani 1 1 d . . . H85 H 0.8134 0.3071 0.1578 0.074 Uiso 1 1 calc R . . C86 C 0.7926(6) 0.1994(9) 0.1544(7) 0.084(5) Uani 1 1 d . . . H86 H 0.7634 0.2077 0.1615 0.101 Uiso 1 1 calc R . . C87 C 0.8051(5) 0.1277(8) 0.1473(7) 0.076(4) Uani 1 1 d . . . H87 H 0.7858 0.0897 0.1525 0.091 Uiso 1 1 calc R . . C88 C 0.8459(5) 0.1133(8) 0.1325(6) 0.067(4) Uani 1 1 d . . . H88 H 0.8541 0.0660 0.1262 0.081 Uiso 1 1 calc R . . C088 C 0.4834(4) 0.0294(6) 0.4013(4) 0.040(3) Uani 1 1 d . . . C89 C 0.8744(4) 0.1730(6) 0.1273(5) 0.039(3) Uani 1 1 d . . . C90 C 0.9462(5) 0.3353(7) 0.0349(6) 0.072(4) Uani 1 1 d . . . H90A H 0.9265 0.3054 0.0033 0.108 Uiso 1 1 calc R . . H90B H 0.9706 0.3616 0.0247 0.108 Uiso 1 1 calc R . . H90C H 0.9248 0.3690 0.0442 0.108 Uiso 1 1 calc R . . C91 C 0.9033(4) 0.3672(5) 0.1427(5) 0.039(3) Uani 1 1 d . . . H91A H 0.8763 0.3930 0.1135 0.046 Uiso 1 1 calc R . . H91B H 0.9346 0.3835 0.1403 0.046 Uiso 1 1 calc R . . C92 C 0.9029(4) 0.3874(5) 0.2009(4) 0.029(2) Uani 1 1 d . . . C93 C 0.9432(4) 0.3633(5) 0.2508(5) 0.034(2) Uani 1 1 d . . . C94 C 0.9444(4) 0.3853(5) 0.3035(4) 0.031(2) Uani 1 1 d . . . C95 C 0.9083(4) 0.4316(5) 0.3100(4) 0.033(2) Uani 1 1 d . . . C96 C 0.8688(4) 0.4524(5) 0.2608(5) 0.034(2) Uani 1 1 d . . . C97 C 0.8657(4) 0.4326(5) 0.2058(4) 0.031(2) Uani 1 1 d . . . C98 C 0.9833(4) 0.3141(6) 0.2455(5) 0.042(3) Uani 1 1 d . . . H98A H 1.0140 0.3217 0.2777 0.063 Uiso 1 1 calc R . . H98B H 0.9884 0.3250 0.2106 0.063 Uiso 1 1 calc R . . H98C H 0.9730 0.2643 0.2449 0.063 Uiso 1 1 calc R . . C99 C 0.9116(5) 0.4587(6) 0.3684(5) 0.051(3) Uani 1 1 d . . . H99A H 0.8866 0.4954 0.3636 0.077 Uiso 1 1 calc R . . H99B H 0.9443 0.4789 0.3884 0.077 Uiso 1 1 calc R . . H99C H 0.9061 0.4189 0.3901 0.077 Uiso 1 1 calc R . . C100 C 0.8231(5) 0.4581(6) 0.1540(5) 0.055(3) Uani 1 1 d . . . H10A H 0.8321 0.5030 0.1407 0.082 Uiso 1 1 calc R . . H10B H 0.7941 0.4657 0.1637 0.082 Uiso 1 1 calc R . . H10C H 0.8157 0.4221 0.1243 0.082 Uiso 1 1 calc R . . C101 C 0.9898(4) 0.3635(5) 0.3570(5) 0.040(3) Uani 1 1 d . . . H10D H 1.0200 0.3808 0.3524 0.048 Uiso 1 1 calc R . . H10E H 0.9872 0.3880 0.3900 0.048 Uiso 1 1 calc R . . C102 C 1.0393(4) 0.2479(6) 0.3881(4) 0.037(3) Uani 1 1 d . . . C103 C 0.9591(4) 0.2376(6) 0.3717(5) 0.039(3) Uani 1 1 d . . . C104 C 0.9067(4) 0.2447(6) 0.3565(5) 0.045(3) Uani 1 1 d . . . H104 H 0.8899 0.2877 0.3414 0.054 Uiso 1 1 calc R . . C105 C 0.8820(5) 0.1852(7) 0.3653(6) 0.066(4) Uani 1 1 d . . . H105 H 0.8477 0.1884 0.3571 0.079 Uiso 1 1 calc R . . C106 C 0.9065(5) 0.1201(6) 0.3859(6) 0.054(3) Uani 1 1 d . . . H106 H 0.8882 0.0808 0.3912 0.065 Uiso 1 1 calc R . . C107 C 0.9560(4) 0.1125(6) 0.3983(5) 0.048(3) Uani 1 1 d . . . H107 H 0.9719 0.0685 0.4119 0.058 Uiso 1 1 calc R . . C108 C 0.9827(4) 0.1714(6) 0.3905(4) 0.039(3) Uani 1 1 d . . . C109 C 1.1110(5) 0.3494(7) 0.4462(6) 0.082(5) Uani 1 1 d . . . H10F H 1.0880 0.3894 0.4339 0.123 Uiso 1 1 calc R . . H10G H 1.1447 0.3667 0.4550 0.123 Uiso 1 1 calc R . . H10H H 1.1084 0.3275 0.4797 0.123 Uiso 1 1 calc R . . C110 C 0.8280(4) 0.5021(6) 0.2678(5) 0.045(3) Uani 1 1 d . . . H11A H 0.8439 0.5456 0.2884 0.054 Uiso 1 1 calc R . . H11B H 0.8053 0.5170 0.2300 0.054 Uiso 1 1 calc R . . C111 C 0.7818(5) 0.5032(6) 0.3358(5) 0.051(3) Uani 1 1 d . . . C112 C 0.7540(4) 0.3958(7) 0.3295(6) 0.052(3) Uani 1 1 d . . . C113 C 0.7314(5) 0.3316(8) 0.3358(6) 0.070(4) Uani 1 1 d . . . H113 H 0.7124 0.3294 0.3589 0.084 Uiso 1 1 calc R . . C114 C 0.7377(5) 0.2710(8) 0.3069(6) 0.070(4) Uani 1 1 d . . . H114 H 0.7221 0.2279 0.3102 0.085 Uiso 1 1 calc R . . C115 C 0.7667(5) 0.2719(7) 0.2729(6) 0.062(4) Uani 1 1 d . . . H115 H 0.7713 0.2295 0.2552 0.075 Uiso 1 1 calc R . . C116 C 0.7882(5) 0.3356(6) 0.2658(6) 0.058(3) Uani 1 1 d . . . H116 H 0.8072 0.3374 0.2428 0.070 Uiso 1 1 calc R . . C117 C 0.7814(4) 0.3972(6) 0.2934(5) 0.041(3) Uani 1 1 d . . . C118 C 0.7709(7) 0.6016(8) 0.4059(7) 0.092(5) Uani 1 1 d . . . H11C H 0.7382 0.5798 0.3940 0.138 Uiso 1 1 calc R . . H11D H 0.7687 0.6519 0.4148 0.138 Uiso 1 1 calc R . . H11E H 0.7932 0.5768 0.4392 0.138 Uiso 1 1 calc R . . C126 C 0.9666(4) 0.0297(5) 0.1991(4) 0.033(2) Uani 1 1 d . . . O1 O 0.3005(4) 0.2246(6) 0.2749(5) 0.095(4) Uani 1 1 d . . . O2 O 0.2934(3) 0.0117(5) 0.3254(4) 0.075(3) Uani 1 1 d . . . O3 O 0.3846(4) 0.1638(6) 0.4367(4) 0.077(3) Uani 1 1 d . . . O4 O 0.5995(4) 0.0163(6) 0.0505(4) 0.090(3) Uani 1 1 d . . . O5 O 0.6844(3) 0.1683(6) 0.1668(5) 0.094(4) Uani 1 1 d . . . O6 O 0.5536(4) 0.2250(6) 0.0389(4) 0.092(4) Uani 1 1 d . . . O7 O 0.3808(3) 0.0705(4) 0.2427(3) 0.0435(19) Uani 1 1 d . . . O8 O 0.4413(3) 0.1673(4) 0.3199(3) 0.0422(18) Uani 1 1 d . . . O9 O 0.5040(3) 0.0792(4) 0.1229(3) 0.0405(18) Uani 1 1 d . . . O10 O 0.5637(3) 0.1777(4) 0.1990(3) 0.0464(19) Uani 1 1 d . . . O11 O 1.0381(3) 0.0283(4) 0.3761(3) 0.0386(17) Uani 1 1 d . . . O12 O 1.1087(3) 0.1183(4) 0.3644(3) 0.0422(18) Uani 1 1 d . . . O13 O 0.9406(3) 0.0257(4) 0.1460(3) 0.0418(18) Uani 1 1 d . . . O14 O 1.0121(3) 0.1124(4) 0.1331(3) 0.0406(18) Uani 1 1 d . . . O15 O 0.8356(4) 0.0423(6) -0.0061(5) 0.104(4) Uani 1 1 d . . . O16 O 0.9519(4) 0.1724(5) -0.0248(4) 0.084(3) Uani 1 1 d . . . O17 O 0.9658(4) -0.0483(5) 0.0135(4) 0.064(3) Uani 1 1 d . . . O18 O 1.1695(4) -0.0227(5) 0.4869(4) 0.086(3) Uani 1 1 d . . . O19 O 1.1701(4) 0.1980(5) 0.5190(4) 0.093(4) Uani 1 1 d . . . O20 O 1.0582(4) 0.0634(6) 0.5368(4) 0.086(3) Uani 1 1 d . . . S1 S 0.38236(11) -0.08764(17) 0.28812(14) 0.0527(8) Uani 1 1 d . . . S2 S 0.54816(13) -0.08113(18) 0.13184(13) 0.0560(9) Uani 1 1 d . . . S3 S 0.68482(19) -0.1358(2) 0.47864(19) 0.0925(14) Uani 1 1 d . . . S4 S 0.97780(11) 0.27866(16) 0.09605(13) 0.0457(7) Uani 1 1 d . . . S5 S 1.09639(11) 0.28395(16) 0.39044(14) 0.0517(8) Uani 1 1 d . . . S6 S 0.79372(17) 0.59446(19) 0.3507(2) 0.0791(12) Uani 1 1 d . . . Re1 Re 0.379552(16) 0.10598(2) 0.321793(19) 0.03725(13) Uani 1 1 d . . . Re2 Re 0.577534(17) 0.11424(3) 0.13607(2) 0.04118(13) Uani 1 1 d . . . Re3 Re 0.941740(18) 0.08313(2) 0.073033(18) 0.03898(13) Uani 1 1 d . . . Re4 Re 1.091705(17) 0.09556(2) 0.437348(19) 0.03940(13) Uani 1 1 d . . . N1 N 0.4368(3) 0.0205(5) 0.3568(4) 0.039(2) Uani 1 1 d . . . N2 N 0.4775(3) -0.0851(4) 0.3712(4) 0.040(2) Uani 1 1 d . . . N3 N 0.5981(3) 0.0299(5) 0.2031(4) 0.039(2) Uani 1 1 d . . . N4 N 0.6073(3) -0.0789(5) 0.2467(4) 0.043(2) Uani 1 1 d . . . N5 N 0.6878(4) -0.2798(6) 0.4855(4) 0.059(3) Uani 1 1 d D . . N6 N 0.7447(5) -0.2253(9) 0.5604(5) 0.097(5) Uani 1 1 d D . . N7 N 0.9150(3) 0.1753(4) 0.1103(4) 0.037(2) Uani 1 1 d . . . N8 N 0.8976(3) 0.2894(4) 0.1301(3) 0.034(2) Uani 1 1 d . . . N9 N 1.0337(3) 0.1799(4) 0.4012(4) 0.035(2) Uani 1 1 d . . . N10 N 0.9948(3) 0.2856(4) 0.3686(4) 0.038(2) Uani 1 1 d . . . N11 N 0.7990(3) 0.4683(5) 0.2979(4) 0.040(2) Uani 1 1 d . . . N12 N 0.7541(4) 0.4616(6) 0.3551(4) 0.055(3) Uani 1 1 d . . . C5A C 0.7558(7) 0.8812(10) 0.2740(8) 0.099(5) Uiso 1 1 d D . . C6A C 0.7297(9) 0.9042(12) 0.2183(9) 0.135(8) Uiso 1 1 d D . . C3A C 0.7752(9) 1.0101(12) 0.3048(10) 0.136(8) Uiso 1 1 d D . . C4A C 0.7777(9) 0.9354(12) 0.3157(10) 0.137(8) Uiso 1 1 d D . . C1A C 0.7236(9) 0.9812(13) 0.1990(10) 0.145(8) Uiso 1 1 d D . . C2A C 0.7496(10) 1.0271(13) 0.2458(11) 0.161(9) Uiso 1 1 d D . . C7A C 0.8034(10) 0.9189(14) 0.3744(11) 0.167(10) Uiso 1 1 d D . . 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 0.059(8) 0.068(9) 0.047(8) 0.006(7) 0.039(7) 0.002(7) C2 0.041(7) 0.058(8) 0.046(7) -0.010(6) 0.020(6) -0.006(6) C3 0.041(7) 0.050(7) 0.055(8) -0.007(6) 0.020(6) -0.004(6) C4 0.047(8) 0.083(10) 0.038(7) 0.008(7) 0.017(6) -0.016(7) C5 0.052(8) 0.087(10) 0.044(8) 0.006(7) 0.018(6) 0.008(8) C6 0.049(8) 0.091(10) 0.049(8) -0.003(8) 0.028(7) -0.002(7) C7 0.030(6) 0.036(6) 0.038(6) 0.001(5) 0.015(5) -0.001(5) C8 0.032(6) 0.036(6) 0.028(6) 0.005(4) 0.014(5) -0.001(5) C9 0.031(6) 0.071(8) 0.036(6) -0.005(6) 0.014(5) -0.017(6) C10 0.045(7) 0.066(8) 0.035(7) -0.011(6) 0.011(6) -0.019(6) C11 0.032(6) 0.084(9) 0.043(7) -0.018(6) 0.020(5) -0.011(6) C12 0.046(7) 0.075(9) 0.043(7) 0.004(6) 0.030(6) -0.009(6) C13 0.030(6) 0.039(6) 0.033(6) 0.006(5) 0.013(5) 0.000(5) C14 0.026(5) 0.045(6) 0.040(6) 0.011(5) 0.018(5) 0.007(5) C15 0.028(6) 0.043(6) 0.032(6) 0.003(5) 0.011(5) 0.002(5) C16 0.030(6) 0.032(6) 0.042(7) 0.012(5) 0.010(5) 0.001(5) C17 0.034(6) 0.045(7) 0.054(7) -0.002(6) 0.025(5) -0.012(5) C18 0.039(7) 0.060(8) 0.059(8) -0.006(7) 0.023(6) -0.010(6) C19 0.064(9) 0.067(9) 0.081(11) -0.019(8) 0.032(8) -0.029(7) C20 0.092(11) 0.057(9) 0.062(9) -0.013(7) 0.036(8) -0.013(8) C21 0.058(8) 0.041(7) 0.081(10) -0.024(7) 0.036(7) -0.020(6) C22 0.033(6) 0.038(6) 0.049(7) 0.000(5) 0.016(5) -0.008(5) C23 0.036(6) 0.028(6) 0.055(7) 0.008(5) 0.026(6) 0.003(5) C24 0.038(6) 0.030(5) 0.027(5) 0.001(4) 0.010(5) -0.001(5) C25 0.038(6) 0.033(6) 0.048(7) 0.007(5) 0.010(5) 0.006(5) C26 0.043(7) 0.040(7) 0.053(8) 0.002(6) 0.018(6) 0.002(5) C27 0.041(7) 0.067(9) 0.056(8) -0.008(7) 0.008(6) 0.005(6) C28 0.063(9) 0.062(9) 0.059(9) -0.007(7) 0.003(7) 0.007(7) C29 0.070(10) 0.077(10) 0.061(9) -0.027(8) 0.008(8) -0.012(8) C30 0.045(7) 0.045(7) 0.073(9) -0.021(7) 0.016(7) -0.001(6) C31 0.060(10) 0.077(11) 0.121(14) 0.013(10) 0.013(9) -0.021(8) C32 0.053(7) 0.038(6) 0.051(7) -0.008(5) 0.021(6) -0.010(5) C33 0.035(6) 0.039(6) 0.039(6) -0.004(5) 0.010(5) -0.002(5) C34 0.036(6) 0.032(6) 0.031(6) -0.004(5) -0.002(5) 0.000(5) C35 0.046(7) 0.037(6) 0.024(6) 0.003(5) 0.005(5) -0.001(5) C36 0.040(6) 0.028(6) 0.047(7) -0.002(5) 0.008(5) 0.008(5) C37 0.038(6) 0.036(6) 0.035(6) -0.006(5) 0.011(5) -0.001(5) C38 0.050(7) 0.030(6) 0.043(7) -0.004(5) 0.007(6) -0.007(5) C39 0.051(7) 0.056(7) 0.033(6) 0.006(6) 0.008(6) -0.002(6) C40 0.054(8) 0.088(10) 0.055(8) 0.021(7) 0.024(7) 0.035(7) C41 0.039(7) 0.063(8) 0.049(8) 0.015(6) 0.010(6) 0.013(6) C42 0.056(8) 0.046(7) 0.033(6) 0.005(5) -0.004(6) 0.013(6) C43 0.041(9) 0.32(3) 0.023(8) -0.038(14) -0.001(7) -0.011(14) C45 0.126(17) 0.091(14) 0.128(18) 0.015(13) 0.004(14) 0.000(13) C46 0.062(10) 0.070(11) 0.091(13) -0.004(9) -0.027(9) 0.007(8) C47 0.085(13) 0.129(17) 0.069(12) 0.021(11) -0.018(10) -0.001(12) C48 0.072(11) 0.120(15) 0.072(12) 0.000(11) 0.018(9) -0.015(11) C49 0.099(12) 0.090(11) 0.048(9) -0.019(8) 0.028(9) -0.050(10) C50 0.17(2) 0.091(13) 0.15(2) -0.034(13) 0.082(17) -0.070(14) C51 0.044(7) 0.051(7) 0.035(7) 0.011(5) 0.008(5) 0.011(6) C52 0.038(6) 0.058(8) 0.030(6) 0.009(5) 0.017(5) 0.012(6) C53 0.051(7) 0.052(7) 0.040(7) -0.001(6) 0.019(6) -0.013(6) C54 0.082(10) 0.073(10) 0.039(8) 0.011(7) 0.003(7) -0.023(8) C55 0.113(13) 0.098(12) 0.036(8) 0.008(8) -0.004(8) -0.047(11) C56 0.098(12) 0.063(9) 0.053(9) -0.001(7) 0.001(8) -0.031(8) C57 0.069(9) 0.061(8) 0.045(8) -0.002(6) 0.017(7) -0.016(7) C58 0.046(7) 0.055(7) 0.024(6) 0.003(5) 0.017(5) 0.000(6) C59 0.137(15) 0.078(10) 0.062(10) -0.017(8) 0.056(10) 0.023(10) C60 0.070(10) 0.067(9) 0.036(7) -0.005(6) 0.010(7) 0.013(8) C61 0.066(8) 0.052(8) 0.033(7) 0.004(6) 0.020(6) -0.023(7) C62 0.073(9) 0.044(7) 0.039(7) -0.008(6) 0.006(7) 0.015(7) C63 0.052(8) 0.059(8) 0.037(7) -0.003(6) 0.012(6) 0.004(6) C64 0.052(8) 0.056(8) 0.042(7) 0.002(6) 0.012(6) 0.007(6) C65 0.057(8) 0.059(8) 0.037(7) 0.011(6) 0.013(6) 0.013(6) C66 0.034(6) 0.033(6) 0.038(6) -0.003(5) 0.017(5) -0.009(5) C67 0.055(8) 0.056(7) 0.037(7) -0.009(6) 0.015(6) -0.024(6) C68 0.064(9) 0.075(9) 0.065(9) 0.006(7) 0.025(7) -0.046(7) C69 0.064(9) 0.069(9) 0.056(9) 0.014(7) 0.032(7) -0.025(7) C70 0.049(7) 0.039(6) 0.038(6) 0.002(5) 0.019(5) -0.005(5) C71 0.042(6) 0.021(5) 0.043(6) 0.001(4) 0.025(5) -0.004(4) C72 0.032(6) 0.030(5) 0.029(6) -0.004(4) 0.011(5) 0.006(4) C73 0.043(6) 0.025(5) 0.035(6) -0.003(4) 0.019(5) 0.002(5) C74 0.025(5) 0.039(6) 0.050(7) -0.001(5) 0.017(5) -0.006(5) C75 0.042(7) 0.061(8) 0.052(8) -0.004(6) 0.012(6) -0.010(6) C76 0.036(7) 0.056(8) 0.075(10) -0.011(7) 0.021(7) -0.025(6) C77 0.028(5) 0.031(6) 0.037(6) -0.010(5) 0.012(5) 0.001(4) C78 0.048(8) 0.057(8) 0.076(10) -0.002(7) 0.039(7) -0.011(6) C79 0.041(7) 0.039(6) 0.051(7) 0.012(5) 0.022(6) 0.003(5) C80 0.026(5) 0.039(6) 0.045(7) -0.008(5) 0.017(5) 0.001(5) C81 0.034(6) 0.030(6) 0.048(7) -0.001(5) 0.026(5) 0.006(5) C82 0.038(6) 0.022(5) 0.038(6) -0.001(4) 0.020(5) -0.002(4) C83 0.039(6) 0.041(6) 0.029(6) -0.006(5) 0.022(5) 0.002(5) C84 0.033(6) 0.070(8) 0.042(7) -0.015(6) 0.028(5) -0.004(6) C85 0.054(8) 0.062(8) 0.076(10) -0.024(7) 0.033(7) -0.017(7) C86 0.071(10) 0.097(12) 0.116(13) -0.042(10) 0.073(10) -0.029(9) C87 0.066(10) 0.084(11) 0.097(12) -0.024(9) 0.052(9) -0.024(8) C88 0.057(9) 0.078(10) 0.071(10) -0.018(8) 0.028(8) -0.025(7) C088 0.035(6) 0.045(7) 0.036(6) 0.001(5) 0.010(5) -0.004(5) C89 0.046(7) 0.035(6) 0.044(7) -0.016(5) 0.025(6) -0.009(5) C90 0.090(11) 0.077(10) 0.066(10) 0.019(8) 0.049(8) -0.001(8) C91 0.034(6) 0.040(6) 0.052(7) 0.001(5) 0.028(5) 0.002(5) C92 0.028(5) 0.029(5) 0.033(6) 0.004(4) 0.014(5) -0.001(4) C93 0.030(6) 0.028(5) 0.048(7) -0.005(5) 0.020(5) 0.001(4) C94 0.032(6) 0.025(5) 0.036(6) 0.002(4) 0.014(5) 0.002(4) C95 0.041(6) 0.025(5) 0.038(6) 0.004(5) 0.018(5) 0.000(5) C96 0.035(6) 0.027(5) 0.050(7) -0.002(5) 0.029(5) -0.006(5) C97 0.028(5) 0.026(5) 0.038(6) 0.008(4) 0.012(5) -0.004(4) C98 0.038(6) 0.042(6) 0.050(7) -0.004(5) 0.019(5) 0.005(5) C99 0.059(8) 0.053(7) 0.042(7) -0.004(6) 0.019(6) 0.013(6) C100 0.066(9) 0.051(7) 0.046(7) 0.007(6) 0.020(7) 0.006(6) C101 0.048(7) 0.030(6) 0.045(7) -0.002(5) 0.021(6) 0.001(5) C102 0.037(6) 0.031(6) 0.039(6) -0.003(5) 0.011(5) 0.000(5) C103 0.033(6) 0.043(7) 0.040(7) 0.001(5) 0.014(5) 0.006(5) C104 0.045(7) 0.040(7) 0.053(8) 0.005(5) 0.023(6) 0.015(6) C105 0.049(8) 0.069(9) 0.092(11) -0.001(8) 0.040(8) -0.013(7) C106 0.056(8) 0.036(7) 0.082(10) 0.019(6) 0.038(7) -0.004(6) C107 0.046(7) 0.048(7) 0.049(7) 0.010(6) 0.016(6) 0.011(6) C108 0.041(7) 0.045(7) 0.025(6) -0.004(5) 0.007(5) 0.002(5) C109 0.059(9) 0.067(9) 0.093(12) -0.032(8) -0.004(8) -0.003(8) C110 0.054(7) 0.040(6) 0.050(7) 0.010(5) 0.029(6) 0.010(6) C111 0.053(8) 0.048(7) 0.062(8) 0.008(6) 0.033(7) 0.024(6) C112 0.042(7) 0.058(8) 0.067(9) 0.005(7) 0.033(6) -0.001(6) C113 0.053(8) 0.089(11) 0.081(11) -0.009(9) 0.040(8) -0.024(8) C114 0.059(9) 0.067(10) 0.083(11) 0.006(8) 0.022(8) -0.028(7) C115 0.068(9) 0.051(8) 0.072(10) -0.004(7) 0.029(8) -0.011(7) C116 0.068(9) 0.047(8) 0.066(9) -0.010(7) 0.032(7) -0.010(7) C117 0.037(6) 0.049(7) 0.038(6) 0.001(5) 0.016(5) 0.003(5) C118 0.110(14) 0.092(12) 0.082(12) -0.008(9) 0.045(10) 0.033(10) C126 0.035(6) 0.035(6) 0.030(6) -0.007(5) 0.013(5) -0.006(5) O1 0.086(8) 0.087(8) 0.127(10) 0.029(7) 0.057(7) 0.038(7) O2 0.052(6) 0.091(7) 0.096(8) -0.012(6) 0.043(6) -0.021(5) O3 0.081(7) 0.103(8) 0.052(6) -0.022(6) 0.030(5) 0.004(6) O4 0.126(9) 0.107(8) 0.065(7) -0.017(6) 0.066(7) 0.003(7) O5 0.036(5) 0.146(10) 0.108(9) 0.014(7) 0.035(6) -0.020(6) O6 0.101(8) 0.118(9) 0.068(7) 0.062(7) 0.045(6) 0.019(7) O7 0.039(4) 0.057(5) 0.045(5) -0.011(4) 0.028(4) -0.012(4) O8 0.043(4) 0.043(4) 0.051(5) -0.014(4) 0.029(4) -0.010(4) O9 0.034(4) 0.058(5) 0.035(4) 0.003(4) 0.019(3) -0.006(4) O10 0.041(4) 0.057(5) 0.049(5) 0.005(4) 0.026(4) -0.009(4) O11 0.046(4) 0.037(4) 0.034(4) 0.004(3) 0.016(4) -0.001(3) O12 0.040(4) 0.045(4) 0.044(5) -0.003(4) 0.018(4) -0.004(3) O13 0.046(5) 0.046(4) 0.030(4) -0.004(3) 0.009(4) -0.019(4) O14 0.048(5) 0.044(4) 0.028(4) 0.003(3) 0.013(4) -0.004(4) O15 0.073(8) 0.121(10) 0.083(8) -0.023(7) -0.011(6) -0.006(7) O16 0.168(11) 0.055(6) 0.043(6) 0.008(5) 0.055(6) 0.012(6) O17 0.098(7) 0.046(5) 0.055(6) -0.017(4) 0.036(5) -0.007(5) O18 0.092(8) 0.068(6) 0.076(7) 0.007(5) 0.007(6) 0.048(6) O19 0.098(8) 0.083(7) 0.058(6) -0.007(6) -0.020(6) -0.021(6) O20 0.098(8) 0.114(8) 0.060(7) 0.024(6) 0.047(6) 0.029(7) S1 0.0418(17) 0.0497(18) 0.060(2) -0.0075(16) 0.0107(15) -0.0029(14) S2 0.064(2) 0.061(2) 0.0354(17) -0.0026(15) 0.0095(15) -0.0031(17) S3 0.118(4) 0.072(3) 0.083(3) -0.003(2) 0.032(3) -0.016(3) S4 0.0499(18) 0.0469(17) 0.0536(19) -0.0029(14) 0.0345(15) -0.0039(14) S5 0.0389(17) 0.0414(17) 0.070(2) 0.0013(15) 0.0141(15) -0.0023(13) S6 0.100(3) 0.055(2) 0.112(3) -0.011(2) 0.073(3) 0.004(2) Re1 0.0329(2) 0.0444(3) 0.0407(3) -0.0011(2) 0.0208(2) 0.0001(2) Re2 0.0353(3) 0.0551(3) 0.0396(3) 0.0077(2) 0.0214(2) -0.0027(2) Re3 0.0504(3) 0.0378(3) 0.0298(2) -0.00402(19) 0.0161(2) 0.0004(2) Re4 0.0431(3) 0.0387(3) 0.0307(2) 0.00165(19) 0.0069(2) 0.0064(2) N1 0.033(5) 0.040(5) 0.040(5) 0.003(4) 0.007(4) 0.000(4) N2 0.045(6) 0.033(5) 0.037(5) -0.002(4) 0.008(4) -0.006(4) N3 0.038(5) 0.048(6) 0.036(5) 0.002(4) 0.019(4) -0.007(4) N4 0.045(6) 0.044(6) 0.040(6) -0.005(5) 0.014(5) -0.007(4) N5 0.046(6) 0.076(8) 0.041(6) 0.013(6) -0.002(5) 0.000(6) N6 0.079(9) 0.143(13) 0.060(9) -0.040(9) 0.016(7) -0.060(10) N7 0.043(5) 0.036(5) 0.032(5) -0.005(4) 0.016(4) 0.003(4) N8 0.034(5) 0.042(5) 0.034(5) -0.010(4) 0.021(4) -0.014(4) N9 0.037(5) 0.027(5) 0.038(5) -0.001(4) 0.011(4) 0.003(4) N10 0.034(5) 0.036(5) 0.035(5) -0.001(4) 0.005(4) 0.001(4) N11 0.032(5) 0.041(5) 0.049(6) 0.001(4) 0.016(4) 0.001(4) N12 0.057(7) 0.062(7) 0.062(7) -0.004(6) 0.039(6) 0.006(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.131(14) . ? C1 Re1 1.923(14) . ? C2 O2 1.146(13) . ? C2 Re1 1.901(12) . ? C3 O3 1.153(13) . ? C3 Re1 1.873(13) . ? C4 O4 1.149(15) . ? C4 Re2 1.892(15) . ? C5 O5 1.140(14) . ? C5 Re2 1.900(14) . ? C6 O6 1.128(14) . ? C6 Re2 1.932(15) . ? C7 O7 1.287(11) . ? C7 C24 1.424(14) . ? C7 C8 1.462(14) . ? C8 C13 1.380(13) . ? C8 C9 1.388(13) . ? C9 C10 1.351(15) . ? C9 H9 0.9300 . ? C10 C11 1.393(15) . ? C10 H10 0.9300 . ? C11 C12 1.372(15) . ? C11 H11 0.9300 . ? C12 C13 1.390(15) . ? C12 H12 0.9300 . ? C13 C14 1.441(14) . ? C14 O9 1.278(11) . ? C14 C15 1.448(14) . ? C15 C16 1.393(14) . ? C15 C24 1.455(14) . ? C16 O10 1.285(12) . ? C16 C17 1.462(15) . ? C17 C22 1.395(14) . ? C17 C18 1.406(14) . ? C18 C19 1.381(17) . ? C18 H18 0.9300 . ? C19 C20 1.388(18) . ? C19 H19 0.9300 . ? C20 C21 1.363(17) . ? C20 H20 0.9300 . ? C21 C22 1.385(15) . ? C21 H21 0.9300 . ? C22 C23 1.450(14) . ? C23 O8 1.284(12) . ? C23 C24 1.413(14) . ? C25 N1 1.329(13) . ? C25 N2 1.365(13) . ? C25 S1 1.741(11) . ? C26 N2 1.379(13) . ? C26 C088 1.395(14) . ? C26 C27 1.406(15) . ? C27 C28 1.346(17) . ? C27 H27 0.9300 . ? C28 C29 1.405(18) . ? C28 H28 0.9300 . ? C29 C30 1.372(17) . ? C29 H29 0.9300 . ? C30 C088 1.373(14) . ? C30 H30 0.9300 . ? C31 S1 1.783(15) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N2 1.462(13) . ? C32 C33 1.517(15) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.406(14) . ? C33 C38 1.404(15) . ? C34 C35 1.388(15) . ? C34 C39 1.498(15) . ? C35 C36 1.413(15) . ? C35 C42 1.508(14) . ? C36 C37 1.398(14) . ? C36 C40 1.499(15) . ? C37 C38 1.393(15) . ? C37 C51 1.522(15) . ? C38 C41 1.538(14) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N5 1.475(14) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.289(15) . ? C43 C48 1.333(14) . ? C43 N5 1.434(14) . ? C44 C45 1.332(14) . ? C44 H44 0.9300 . ? C45 C46 1.318(15) . ? C45 H45 0.9300 . ? C46 C47 1.346(15) . ? C46 H46 0.9300 . ? C47 C48 1.405(15) . ? C47 H47 0.9300 . ? C48 N6 1.395(14) . ? C49 N5 1.347(16) . ? C49 N6 1.365(18) . ? C49 S3 1.654(17) . ? C50 S3 1.868(18) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 N4 1.484(13) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 N3 1.315(13) . ? C52 N4 1.382(13) . ? C52 S2 1.763(11) . ? C53 C54 1.378(16) . ? C53 C58 1.379(15) . ? C53 N4 1.393(13) . ? C54 C55 1.330(18) . ? C54 H54 0.9300 . ? C55 C56 1.397(18) . ? C55 H55 0.9300 . ? C56 C57 1.331(17) . ? C56 H56 0.9300 . ? C57 C58 1.399(15) . ? C57 H57 0.9300 . ? C58 N3 1.391(13) . ? C59 S2 1.796(14) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 O15 1.151(15) . ? C60 Re3 1.899(14) . ? C61 O17 1.137(13) . ? C61 Re3 1.918(14) . ? C62 O16 1.146(15) . ? C62 Re3 1.908(15) . ? C63 O18 1.137(13) . ? C63 Re4 1.901(13) . ? C64 O19 1.149(13) . ? C64 Re4 1.917(13) . ? C65 O20 1.166(14) . ? C65 Re4 1.878(13) . ? C66 C67 1.384(14) . ? C66 C71 1.415(14) . ? C66 C126 1.439(14) . ? C67 C68 1.395(16) . ? C67 H67 0.9300 . ? C68 C69 1.375(17) . ? C68 H68 0.9300 . ? C69 C70 1.399(15) . ? C69 H69 0.9300 . ? C70 C71 1.365(14) . ? C70 H70 0.9300 . ? C71 C72 1.457(13) . ? C72 O11 1.263(11) . ? C72 C73 1.413(14) . ? C73 C77 1.435(14) . ? C73 C82 1.457(14) . ? C74 C80 1.380(14) . ? C74 C75 1.421(14) . ? C74 C77 1.456(14) . ? C75 C76 1.373(16) . ? C75 H75 0.9300 . ? C76 C78 1.388(17) . ? C76 H76 0.9300 . ? C77 O12 1.270(12) . ? C78 C79 1.345(15) . ? C78 H78 0.9300 . ? C79 C80 1.419(14) . ? C79 H79 0.9300 . ? C80 C81 1.468(14) . ? C81 O14 1.247(12) . ? C81 C82 1.438(14) . ? C82 C126 1.441(13) . ? C83 N7 1.338(12) . ? C83 N8 1.371(12) . ? C83 S4 1.742(10) . ? C84 C85 1.368(15) . ? C84 C89 1.379(15) . ? C84 N8 1.402(13) . ? C85 C86 1.400(17) . ? C85 H85 0.9300 . ? C86 C87 1.394(19) . ? C86 H86 0.9300 . ? C87 C88 1.377(18) . ? C87 H87 0.9300 . ? C88 C89 1.403(16) . ? C88 H88 0.9300 . ? C088 N1 1.401(12) . ? C89 N7 1.379(13) . ? C90 S4 1.797(13) . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 N8 1.460(12) . ? C91 C92 1.511(14) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 C97 1.392(13) . ? C92 C93 1.424(13) . ? C93 C94 1.372(14) . ? C93 C98 1.507(13) . ? C94 C95 1.395(13) . ? C94 C101 1.537(14) . ? C95 C96 1.386(14) . ? C95 C99 1.517(14) . ? C96 C97 1.400(14) . ? C96 C110 1.544(14) . ? C97 C100 1.494(14) . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? C99 H99A 0.9600 . ? C99 H99B 0.9600 . ? C99 H99C 0.9600 . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? C101 N10 1.458(12) . ? C101 H10D 0.9700 . ? C101 H10E 0.9700 . ? C102 N9 1.318(12) . ? C102 N10 1.373(12) . ? C102 S5 1.748(11) . ? C103 N10 1.375(13) . ? C103 C108 1.388(14) . ? C103 C104 1.413(14) . ? C104 C105 1.365(16) . ? C104 H104 0.9300 . ? C105 C106 1.387(16) . ? C105 H105 0.9300 . ? C106 C107 1.344(16) . ? C106 H106 0.9300 . ? C107 C108 1.382(15) . ? C107 H107 0.9300 . ? C108 N9 1.397(13) . ? C109 S5 1.773(13) . ? C109 H10F 0.9600 . ? C109 H10G 0.9600 . ? C109 H10H 0.9600 . ? C110 N11 1.455(13) . ? C110 H11A 0.9700 . ? C110 H11B 0.9700 . ? C111 N12 1.318(15) . ? C111 N11 1.380(14) . ? C111 S6 1.726(12) . ? C112 N12 1.370(15) . ? C112 C113 1.383(17) . ? C112 C117 1.402(15) . ? C113 C114 1.378(19) . ? C113 H113 0.9300 . ? C114 C115 1.393(19) . ? C114 H114 0.9300 . ? C115 C116 1.366(16) . ? C115 H115 0.9300 . ? C116 C117 1.378(15) . ? C116 H116 0.9300 . ? C117 N11 1.391(13) . ? C118 S6 1.741(15) . ? C118 H11C 0.9600 . ? C118 H11D 0.9600 . ? C118 H11E 0.9600 . ? C126 O13 1.267(11) . ? O7 Re1 2.102(7) . ? O8 Re1 2.115(7) . ? O9 Re2 2.112(7) . ? O10 Re2 2.116(8) . ? O11 Re4 2.123(7) . ? O12 Re4 2.104(7) . ? O13 Re3 2.123(7) . ? O14 Re3 2.094(7) . ? Re1 N1 2.207(8) . ? Re2 N3 2.201(9) . ? Re3 N7 2.207(8) . ? Re4 N9 2.208(8) . ? C5A C6A 1.386(16) . ? C5A C4A 1.41(3) . ? C6A C1A 1.49(3) . ? C3A C4A 1.396(16) . ? C3A C2A 1.42(3) . ? C4A C7A 1.416(17) . ? C1A C2A 1.412(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Re1 175.7(11) . . ? O2 C2 Re1 177.0(11) . . ? O3 C3 Re1 177.5(12) . . ? O4 C4 Re2 177.5(12) . . ? O5 C5 Re2 178.2(14) . . ? O6 C6 Re2 173.0(12) . . ? O7 C7 C24 126.2(9) . . ? O7 C7 C8 114.6(9) . . ? C24 C7 C8 119.2(9) . . ? C13 C8 C9 119.7(10) . . ? C13 C8 C7 120.8(9) . . ? C9 C8 C7 119.5(9) . . ? C10 C9 C8 120.7(10) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.4(11) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 119.2(11) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C13 120.7(10) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C8 C13 C12 119.2(9) . . ? C8 C13 C14 120.9(9) . . ? C12 C13 C14 119.9(10) . . ? O9 C14 C13 115.5(10) . . ? O9 C14 C15 124.4(9) . . ? C13 C14 C15 120.0(9) . . ? C16 C15 C14 120.8(10) . . ? C16 C15 C24 120.7(9) . . ? C14 C15 C24 118.5(9) . . ? O10 C16 C15 126.2(10) . . ? O10 C16 C17 114.8(9) . . ? C15 C16 C17 119.0(10) . . ? C22 C17 C18 119.3(10) . . ? C22 C17 C16 120.8(9) . . ? C18 C17 C16 119.7(10) . . ? C19 C18 C17 120.2(12) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.8(12) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 119.8(13) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 121.9(12) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C21 C22 C17 118.8(10) . . ? C21 C22 C23 121.2(10) . . ? C17 C22 C23 119.9(10) . . ? O8 C23 C24 126.5(10) . . ? O8 C23 C22 114.0(10) . . ? C24 C23 C22 119.6(10) . . ? C23 C24 C7 119.7(9) . . ? C23 C24 C15 119.8(9) . . ? C7 C24 C15 120.5(9) . . ? N1 C25 N2 111.5(9) . . ? N1 C25 S1 123.8(8) . . ? N2 C25 S1 124.7(8) . . ? N2 C26 C088 106.4(9) . . ? N2 C26 C27 131.3(11) . . ? C088 C26 C27 122.0(11) . . ? C28 C27 C26 116.0(12) . . ? C28 C27 H27 122.0 . . ? C26 C27 H27 122.0 . . ? C27 C28 C29 123.0(13) . . ? C27 C28 H28 118.5 . . ? C29 C28 H28 118.5 . . ? C30 C29 C28 120.3(12) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C088 118.5(12) . . ? C29 C30 H30 120.8 . . ? C088 C30 H30 120.8 . . ? S1 C31 H31A 109.5 . . ? S1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N2 C32 C33 117.5(9) . . ? N2 C32 H32A 107.9 . . ? C33 C32 H32A 107.9 . . ? N2 C32 H32B 107.9 . . ? C33 C32 H32B 107.9 . . ? H32A C32 H32B 107.2 . . ? C34 C33 C38 121.3(10) . . ? C34 C33 C32 120.2(10) . . ? C38 C33 C32 118.5(10) . . ? C35 C34 C33 118.2(10) . . ? C35 C34 C39 120.2(9) . . ? C33 C34 C39 121.6(10) . . ? C34 C35 C36 121.5(10) . . ? C34 C35 C42 119.6(10) . . ? C36 C35 C42 118.5(10) . . ? C37 C36 C35 119.1(10) . . ? C37 C36 C40 122.0(11) . . ? C35 C36 C40 118.9(10) . . ? C38 C37 C36 120.3(10) . . ? C38 C37 C51 120.8(10) . . ? C36 C37 C51 118.7(10) . . ? C37 C38 C33 119.5(10) . . ? C37 C38 C41 120.6(11) . . ? C33 C38 C41 119.7(11) . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N5 C42 C35 116.4(9) . . ? N5 C42 H42A 108.2 . . ? C35 C42 H42A 108.2 . . ? N5 C42 H42B 108.2 . . ? C35 C42 H42B 108.2 . . ? H42A C42 H42B 107.3 . . ? C44 C43 C48 116.5(14) . . ? C44 C43 N5 136.4(13) . . ? C48 C43 N5 107.1(14) . . ? C43 C44 C45 133.9(14) . . ? C43 C44 H44 113.1 . . ? C45 C44 H44 113.1 . . ? C46 C45 C44 107.2(15) . . ? C46 C45 H45 126.4 . . ? C44 C45 H45 126.4 . . ? C45 C46 C47 127.6(15) . . ? C45 C46 H46 116.2 . . ? C47 C46 H46 116.2 . . ? C46 C47 C48 118.1(15) . . ? C46 C47 H47 121.0 . . ? C48 C47 H47 121.0 . . ? C43 C48 N6 109.4(13) . . ? C43 C48 C47 116.7(15) . . ? N6 C48 C47 133.8(15) . . ? N5 C49 N6 109.9(14) . . ? N5 C49 S3 123.9(11) . . ? N6 C49 S3 126.2(12) . . ? S3 C50 H50A 109.5 . . ? S3 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? S3 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N4 C51 C37 112.0(9) . . ? N4 C51 H51A 109.2 . . ? C37 C51 H51A 109.2 . . ? N4 C51 H51B 109.2 . . ? C37 C51 H51B 109.2 . . ? H51A C51 H51B 107.9 . . ? N3 C52 N4 113.0(10) . . ? N3 C52 S2 125.4(8) . . ? N4 C52 S2 121.5(9) . . ? C54 C53 C58 121.5(11) . . ? C54 C53 N4 132.3(11) . . ? C58 C53 N4 106.2(10) . . ? C55 C54 C53 116.2(13) . . ? C55 C54 H54 121.9 . . ? C53 C54 H54 121.9 . . ? C54 C55 C56 123.3(13) . . ? C54 C55 H55 118.3 . . ? C56 C55 H55 118.3 . . ? C57 C56 C55 121.3(13) . . ? C57 C56 H56 119.4 . . ? C55 C56 H56 119.4 . . ? C56 C57 C58 116.6(12) . . ? C56 C57 H57 121.7 . . ? C58 C57 H57 121.7 . . ? C53 C58 N3 110.2(10) . . ? C53 C58 C57 121.0(10) . . ? N3 C58 C57 128.8(10) . . ? S2 C59 H59A 109.5 . . ? S2 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? S2 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O15 C60 Re3 179.7(15) . . ? O17 C61 Re3 173.3(12) . . ? O16 C62 Re3 178.2(11) . . ? O18 C63 Re4 175.1(11) . . ? O19 C64 Re4 177.2(11) . . ? O20 C65 Re4 179.2(13) . . ? C67 C66 C71 119.3(9) . . ? C67 C66 C126 119.8(10) . . ? C71 C66 C126 120.9(9) . . ? C66 C67 C68 118.9(11) . . ? C66 C67 H67 120.5 . . ? C68 C67 H67 120.5 . . ? C69 C68 C67 122.4(11) . . ? C69 C68 H68 118.8 . . ? C67 C68 H68 118.8 . . ? C68 C69 C70 118.0(11) . . ? C68 C69 H69 121.0 . . ? C70 C69 H69 121.0 . . ? C71 C70 C69 121.2(11) . . ? C71 C70 H70 119.4 . . ? C69 C70 H70 119.4 . . ? C70 C71 C66 120.2(9) . . ? C70 C71 C72 119.6(10) . . ? C66 C71 C72 120.2(9) . . ? O11 C72 C73 126.0(9) . . ? O11 C72 C71 115.0(9) . . ? C73 C72 C71 119.0(9) . . ? C72 C73 C77 119.5(9) . . ? C72 C73 C82 121.4(9) . . ? C77 C73 C82 118.9(9) . . ? C80 C74 C75 119.5(10) . . ? C80 C74 C77 121.5(9) . . ? C75 C74 C77 119.0(10) . . ? C76 C75 C74 120.0(11) . . ? C76 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C75 C76 C78 119.3(11) . . ? C75 C76 H76 120.3 . . ? C78 C76 H76 120.3 . . ? O12 C77 C73 125.8(10) . . ? O12 C77 C74 115.5(9) . . ? C73 C77 C74 118.7(9) . . ? C79 C78 C76 122.1(11) . . ? C79 C78 H78 119.0 . . ? C76 C78 H78 119.0 . . ? C78 C79 C80 119.8(11) . . ? C78 C79 H79 120.1 . . ? C80 C79 H79 120.1 . . ? C74 C80 C79 119.4(9) . . ? C74 C80 C81 122.3(10) . . ? C79 C80 C81 118.3(10) . . ? O14 C81 C82 126.8(10) . . ? O14 C81 C80 117.2(9) . . ? C82 C81 C80 116.0(10) . . ? C81 C82 C126 118.7(9) . . ? C81 C82 C73 122.6(9) . . ? C126 C82 C73 118.7(9) . . ? N7 C83 N8 112.6(9) . . ? N7 C83 S4 124.5(8) . . ? N8 C83 S4 122.9(8) . . ? C85 C84 C89 124.3(11) . . ? C85 C84 N8 128.6(11) . . ? C89 C84 N8 107.0(9) . . ? C84 C85 C86 113.9(12) . . ? C84 C85 H85 123.0 . . ? C86 C85 H85 123.0 . . ? C87 C86 C85 123.8(13) . . ? C87 C86 H86 118.1 . . ? C85 C86 H86 118.1 . . ? C88 C87 C86 120.1(14) . . ? C88 C87 H87 120.0 . . ? C86 C87 H87 120.0 . . ? C87 C88 C89 117.2(13) . . ? C87 C88 H88 121.4 . . ? C89 C88 H88 121.4 . . ? C30 C088 C26 120.1(10) . . ? C30 C088 N1 131.5(10) . . ? C26 C088 N1 108.4(9) . . ? C84 C89 N7 109.6(9) . . ? C84 C89 C88 120.5(11) . . ? N7 C89 C88 129.9(11) . . ? S4 C90 H90A 109.5 . . ? S4 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? S4 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? N8 C91 C92 114.2(8) . . ? N8 C91 H91A 108.7 . . ? C92 C91 H91A 108.7 . . ? N8 C91 H91B 108.7 . . ? C92 C91 H91B 108.7 . . ? H91A C91 H91B 107.6 . . ? C97 C92 C93 120.5(9) . . ? C97 C92 C91 120.7(9) . . ? C93 C92 C91 118.7(9) . . ? C94 C93 C92 118.7(9) . . ? C94 C93 C98 120.8(9) . . ? C92 C93 C98 120.5(9) . . ? C93 C94 C95 122.4(9) . . ? C93 C94 C101 118.5(9) . . ? C95 C94 C101 118.9(9) . . ? C96 C95 C94 117.7(9) . . ? C96 C95 C99 120.5(9) . . ? C94 C95 C99 121.8(9) . . ? C95 C96 C97 122.6(9) . . ? C95 C96 C110 117.9(9) . . ? C97 C96 C110 119.5(9) . . ? C92 C97 C96 118.1(9) . . ? C92 C97 C100 121.3(10) . . ? C96 C97 C100 120.6(10) . . ? C93 C98 H98A 109.5 . . ? C93 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C93 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C95 C99 H99A 109.5 . . ? C95 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C95 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C97 C100 H10A 109.5 . . ? C97 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C97 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? N10 C101 C94 114.8(8) . . ? N10 C101 H10D 108.6 . . ? C94 C101 H10D 108.6 . . ? N10 C101 H10E 108.6 . . ? C94 C101 H10E 108.6 . . ? H10D C101 H10E 107.5 . . ? N9 C102 N10 112.7(9) . . ? N9 C102 S5 123.3(8) . . ? N10 C102 S5 123.9(8) . . ? N10 C103 C108 107.6(9) . . ? N10 C103 C104 131.7(10) . . ? C108 C103 C104 120.6(10) . . ? C105 C104 C103 116.5(11) . . ? C105 C104 H104 121.8 . . ? C103 C104 H104 121.8 . . ? C104 C105 C106 122.1(12) . . ? C104 C105 H105 118.9 . . ? C106 C105 H105 118.9 . . ? C107 C106 C105 121.4(11) . . ? C107 C106 H106 119.3 . . ? C105 C106 H106 119.3 . . ? C106 C107 C108 118.6(11) . . ? C106 C107 H107 120.7 . . ? C108 C107 H107 120.7 . . ? C107 C108 C103 120.6(10) . . ? C107 C108 N9 131.0(10) . . ? C103 C108 N9 108.2(9) . . ? S5 C109 H10F 109.5 . . ? S5 C109 H10G 109.5 . . ? H10F C109 H10G 109.5 . . ? S5 C109 H10H 109.5 . . ? H10F C109 H10H 109.5 . . ? H10G C109 H10H 109.5 . . ? N11 C110 C96 114.1(8) . . ? N11 C110 H11A 108.7 . . ? C96 C110 H11A 108.7 . . ? N11 C110 H11B 108.7 . . ? C96 C110 H11B 108.7 . . ? H11A C110 H11B 107.6 . . ? N12 C111 N11 113.7(10) . . ? N12 C111 S6 125.7(9) . . ? N11 C111 S6 120.5(9) . . ? N12 C112 C113 128.3(12) . . ? N12 C112 C117 112.5(11) . . ? C113 C112 C117 119.2(12) . . ? C114 C113 C112 118.0(13) . . ? C114 C113 H113 121.0 . . ? C112 C113 H113 121.0 . . ? C113 C114 C115 122.6(13) . . ? C113 C114 H114 118.7 . . ? C115 C114 H114 118.7 . . ? C116 C115 C114 119.2(13) . . ? C116 C115 H115 120.4 . . ? C114 C115 H115 120.4 . . ? C115 C116 C117 119.1(13) . . ? C115 C116 H116 120.5 . . ? C117 C116 H116 120.5 . . ? C116 C117 N11 134.3(11) . . ? C116 C117 C112 121.8(11) . . ? N11 C117 C112 103.8(10) . . ? S6 C118 H11C 109.5 . . ? S6 C118 H11D 109.5 . . ? H11C C118 H11D 109.5 . . ? S6 C118 H11E 109.5 . . ? H11C C118 H11E 109.5 . . ? H11D C118 H11E 109.5 . . ? O13 C126 C66 115.3(9) . . ? O13 C126 C82 125.1(9) . . ? C66 C126 C82 119.6(9) . . ? C7 O7 Re1 133.0(7) . . ? C23 O8 Re1 132.5(7) . . ? C14 O9 Re2 132.7(7) . . ? C16 O10 Re2 131.2(7) . . ? C72 O11 Re4 131.7(6) . . ? C77 O12 Re4 132.1(7) . . ? C126 O13 Re3 133.4(6) . . ? C81 O14 Re3 133.5(7) . . ? C25 S1 C31 101.0(6) . . ? C52 S2 C59 104.2(6) . . ? C49 S3 C50 97.1(8) . . ? C83 S4 C90 101.7(6) . . ? C102 S5 C109 103.3(6) . . ? C111 S6 C118 98.2(7) . . ? C3 Re1 C2 86.4(5) . . ? C3 Re1 C1 85.7(5) . . ? C2 Re1 C1 87.1(5) . . ? C3 Re1 O7 175.7(4) . . ? C2 Re1 O7 97.7(4) . . ? C1 Re1 O7 95.8(4) . . ? C3 Re1 O8 95.2(4) . . ? C2 Re1 O8 176.5(4) . . ? C1 Re1 O8 96.2(4) . . ? O7 Re1 O8 80.7(3) . . ? C3 Re1 N1 95.1(4) . . ? C2 Re1 N1 93.5(4) . . ? C1 Re1 N1 179.1(4) . . ? O7 Re1 N1 83.4(3) . . ? O8 Re1 N1 83.3(3) . . ? C4 Re2 C5 85.7(5) . . ? C4 Re2 C6 85.7(5) . . ? C5 Re2 C6 85.6(5) . . ? C4 Re2 O9 98.7(4) . . ? C5 Re2 O9 174.7(4) . . ? C6 Re2 O9 97.7(4) . . ? C4 Re2 O10 176.2(4) . . ? C5 Re2 O10 95.1(4) . . ? C6 Re2 O10 98.1(4) . . ? O9 Re2 O10 80.4(3) . . ? C4 Re2 N3 92.5(4) . . ? C5 Re2 N3 93.9(4) . . ? C6 Re2 N3 178.2(5) . . ? O9 Re2 N3 82.9(3) . . ? O10 Re2 N3 83.7(3) . . ? C60 Re3 C62 88.8(6) . . ? C60 Re3 C61 83.2(5) . . ? C62 Re3 C61 86.6(5) . . ? C60 Re3 O14 174.8(4) . . ? C62 Re3 O14 95.0(4) . . ? C61 Re3 O14 100.5(4) . . ? C60 Re3 O13 96.2(4) . . ? C62 Re3 O13 174.7(4) . . ? C61 Re3 O13 95.7(4) . . ? O14 Re3 O13 79.9(3) . . ? C60 Re3 N7 92.5(4) . . ? C62 Re3 N7 93.9(4) . . ? C61 Re3 N7 175.7(4) . . ? O14 Re3 N7 83.7(3) . . ? O13 Re3 N7 84.2(3) . . ? C65 Re4 C63 87.7(5) . . ? C65 Re4 C64 87.4(5) . . ? C63 Re4 C64 87.6(5) . . ? C65 Re4 O12 175.1(4) . . ? C63 Re4 O12 95.8(4) . . ? C64 Re4 O12 96.1(4) . . ? C65 Re4 O11 96.5(4) . . ? C63 Re4 O11 94.8(4) . . ? C64 Re4 O11 175.5(4) . . ? O12 Re4 O11 79.9(3) . . ? C65 Re4 N9 93.0(4) . . ? C63 Re4 N9 177.7(4) . . ? C64 Re4 N9 94.6(4) . . ? O12 Re4 N9 83.4(3) . . ? O11 Re4 N9 83.0(3) . . ? C25 N1 C088 106.2(9) . . ? C25 N1 Re1 127.9(7) . . ? C088 N1 Re1 125.9(7) . . ? C25 N2 C26 107.5(9) . . ? C25 N2 C32 125.6(9) . . ? C26 N2 C32 126.9(9) . . ? C52 N3 C58 105.1(9) . . ? C52 N3 Re2 127.1(7) . . ? C58 N3 Re2 127.7(7) . . ? C52 N4 C53 105.5(9) . . ? C52 N4 C51 125.6(9) . . ? C53 N4 C51 128.9(9) . . ? C49 N5 C43 106.7(11) . . ? C49 N5 C42 136.6(11) . . ? C43 N5 C42 116.7(10) . . ? C49 N6 C48 106.7(12) . . ? C83 N7 C89 105.6(8) . . ? C83 N7 Re3 128.6(7) . . ? C89 N7 Re3 124.9(7) . . ? C83 N8 C84 105.1(8) . . ? C83 N8 C91 127.8(8) . . ? C84 N8 C91 126.9(8) . . ? C102 N9 C108 105.8(8) . . ? C102 N9 Re4 128.8(7) . . ? C108 N9 Re4 125.3(7) . . ? C102 N10 C103 105.7(8) . . ? C102 N10 C101 125.2(9) . . ? C103 N10 C101 128.3(9) . . ? C111 N11 C117 106.3(9) . . ? C111 N11 C110 125.4(10) . . ? C117 N11 C110 128.3(9) . . ? C111 N12 C112 103.7(10) . . ? C6A C5A C4A 117.3(19) . . ? C5A C6A C1A 125(2) . . ? C4A C3A C2A 113(2) . . ? C3A C4A C5A 125(2) . . ? C3A C4A C7A 113(2) . . ? C5A C4A C7A 122(2) . . ? C2A C1A C6A 110(2) . . ? C1A C2A C3A 130(2) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 C7 C8 C13 -179.0(9) . . . . ? C24 C7 C8 C13 2.8(14) . . . . ? O7 C7 C8 C9 1.8(14) . . . . ? C24 C7 C8 C9 -176.4(10) . . . . ? C13 C8 C9 C10 -0.4(17) . . . . ? C7 C8 C9 C10 178.8(11) . . . . ? C8 C9 C10 C11 3.1(18) . . . . ? C9 C10 C11 C12 -3.6(19) . . . . ? C10 C11 C12 C13 1.6(19) . . . . ? C9 C8 C13 C12 -1.6(15) . . . . ? C7 C8 C13 C12 179.2(10) . . . . ? C9 C8 C13 C14 178.9(10) . . . . ? C7 C8 C13 C14 -0.3(15) . . . . ? C11 C12 C13 C8 1.0(17) . . . . ? C11 C12 C13 C14 -179.5(11) . . . . ? C8 C13 C14 O9 178.7(9) . . . . ? C12 C13 C14 O9 -0.9(15) . . . . ? C8 C13 C14 C15 -2.2(15) . . . . ? C12 C13 C14 C15 178.3(10) . . . . ? O9 C14 C15 C16 3.9(16) . . . . ? C13 C14 C15 C16 -175.1(9) . . . . ? O9 C14 C15 C24 -178.8(9) . . . . ? C13 C14 C15 C24 2.1(14) . . . . ? C14 C15 C16 O10 -0.6(16) . . . . ? C24 C15 C16 O10 -177.8(9) . . . . ? C14 C15 C16 C17 177.2(9) . . . . ? C24 C15 C16 C17 0.0(14) . . . . ? O10 C16 C17 C22 -179.5(10) . . . . ? C15 C16 C17 C22 2.4(15) . . . . ? O10 C16 C17 C18 -3.7(15) . . . . ? C15 C16 C17 C18 178.2(10) . . . . ? C22 C17 C18 C19 -3.0(18) . . . . ? C16 C17 C18 C19 -178.9(12) . . . . ? C17 C18 C19 C20 5(2) . . . . ? C18 C19 C20 C21 -4(2) . . . . ? C19 C20 C21 C22 2(2) . . . . ? C20 C21 C22 C17 0.2(18) . . . . ? C20 C21 C22 C23 -179.6(11) . . . . ? C18 C17 C22 C21 0.5(17) . . . . ? C16 C17 C22 C21 176.3(11) . . . . ? C18 C17 C22 C23 -179.7(10) . . . . ? C16 C17 C22 C23 -3.9(16) . . . . ? C21 C22 C23 O8 3.0(15) . . . . ? C17 C22 C23 O8 -176.8(10) . . . . ? C21 C22 C23 C24 -177.2(10) . . . . ? C17 C22 C23 C24 3.0(15) . . . . ? O8 C23 C24 C7 0.6(16) . . . . ? C22 C23 C24 C7 -179.2(9) . . . . ? O8 C23 C24 C15 179.1(10) . . . . ? C22 C23 C24 C15 -0.7(14) . . . . ? O7 C7 C24 C23 -2.3(16) . . . . ? C8 C7 C24 C23 175.7(9) . . . . ? O7 C7 C24 C15 179.2(10) . . . . ? C8 C7 C24 C15 -2.8(14) . . . . ? C16 C15 C24 C23 -0.8(14) . . . . ? C14 C15 C24 C23 -178.1(9) . . . . ? C16 C15 C24 C7 177.6(9) . . . . ? C14 C15 C24 C7 0.4(14) . . . . ? N2 C26 C27 C28 -174.4(13) . . . . ? C088 C26 C27 C28 -1.0(19) . . . . ? C26 C27 C28 C29 -1(2) . . . . ? C27 C28 C29 C30 1(2) . . . . ? C28 C29 C30 C088 2(2) . . . . ? N2 C32 C33 C34 118.9(11) . . . . ? N2 C32 C33 C38 -64.4(13) . . . . ? C38 C33 C34 C35 -1.5(15) . . . . ? C32 C33 C34 C35 175.0(9) . . . . ? C38 C33 C34 C39 -179.0(10) . . . . ? C32 C33 C34 C39 -2.5(15) . . . . ? C33 C34 C35 C36 1.9(15) . . . . ? C39 C34 C35 C36 179.4(10) . . . . ? C33 C34 C35 C42 -171.2(9) . . . . ? C39 C34 C35 C42 6.3(15) . . . . ? C34 C35 C36 C37 -2.8(16) . . . . ? C42 C35 C36 C37 170.4(9) . . . . ? C34 C35 C36 C40 176.7(10) . . . . ? C42 C35 C36 C40 -10.1(15) . . . . ? C35 C36 C37 C38 3.2(15) . . . . ? C40 C36 C37 C38 -176.2(10) . . . . ? C35 C36 C37 C51 -171.4(9) . . . . ? C40 C36 C37 C51 9.2(16) . . . . ? C36 C37 C38 C33 -2.9(15) . . . . ? C51 C37 C38 C33 171.6(9) . . . . ? C36 C37 C38 C41 -178.1(10) . . . . ? C51 C37 C38 C41 -3.6(15) . . . . ? C34 C33 C38 C37 2.0(16) . . . . ? C32 C33 C38 C37 -174.6(9) . . . . ? C34 C33 C38 C41 177.3(10) . . . . ? C32 C33 C38 C41 0.7(15) . . . . ? C34 C35 C42 N5 -90.9(13) . . . . ? C36 C35 C42 N5 95.8(13) . . . . ? C48 C43 C44 C45 2(3) . . . . ? N5 C43 C44 C45 -177.1(19) . . . . ? C43 C44 C45 C46 -4(3) . . . . ? C44 C45 C46 C47 3(3) . . . . ? C45 C46 C47 C48 -1(4) . . . . ? C44 C43 C48 N6 178.4(15) . . . . ? N5 C43 C48 N6 -2.2(19) . . . . ? C44 C43 C48 C47 1(3) . . . . ? N5 C43 C48 C47 -179.5(15) . . . . ? C46 C47 C48 C43 -2(3) . . . . ? C46 C47 C48 N6 -178(2) . . . . ? C38 C37 C51 N4 65.7(13) . . . . ? C36 C37 C51 N4 -119.8(10) . . . . ? C58 C53 C54 C55 -2(2) . . . . ? N4 C53 C54 C55 178.2(14) . . . . ? C53 C54 C55 C56 3(3) . . . . ? C54 C55 C56 C57 -1(3) . . . . ? C55 C56 C57 C58 -2(2) . . . . ? C54 C53 C58 N3 -179.8(11) . . . . ? N4 C53 C58 N3 0.4(13) . . . . ? C54 C53 C58 C57 -0.9(19) . . . . ? N4 C53 C58 C57 179.2(11) . . . . ? C56 C57 C58 C53 3(2) . . . . ? C56 C57 C58 N3 -178.9(13) . . . . ? C71 C66 C67 C68 1.2(17) . . . . ? C126 C66 C67 C68 -178.1(11) . . . . ? C66 C67 C68 C69 -1(2) . . . . ? C67 C68 C69 C70 0(2) . . . . ? C68 C69 C70 C71 -0.3(19) . . . . ? C69 C70 C71 C66 0.9(16) . . . . ? C69 C70 C71 C72 179.6(10) . . . . ? C67 C66 C71 C70 -1.3(16) . . . . ? C126 C66 C71 C70 177.9(10) . . . . ? C67 C66 C71 C72 179.9(10) . . . . ? C126 C66 C71 C72 -0.8(15) . . . . ? C70 C71 C72 O11 0.7(14) . . . . ? C66 C71 C72 O11 179.4(9) . . . . ? C70 C71 C72 C73 179.9(9) . . . . ? C66 C71 C72 C73 -1.4(14) . . . . ? O11 C72 C73 C77 4.7(15) . . . . ? C71 C72 C73 C77 -174.4(9) . . . . ? O11 C72 C73 C82 180.0(9) . . . . ? C71 C72 C73 C82 0.9(14) . . . . ? C80 C74 C75 C76 -0.7(17) . . . . ? C77 C74 C75 C76 179.8(11) . . . . ? C74 C75 C76 C78 1.1(19) . . . . ? C72 C73 C77 O12 -6.8(15) . . . . ? C82 C73 C77 O12 177.8(9) . . . . ? C72 C73 C77 C74 173.9(9) . . . . ? C82 C73 C77 C74 -1.5(13) . . . . ? C80 C74 C77 O12 -176.2(9) . . . . ? C75 C74 C77 O12 3.2(14) . . . . ? C80 C74 C77 C73 3.2(15) . . . . ? C75 C74 C77 C73 -177.4(10) . . . . ? C75 C76 C78 C79 -1(2) . . . . ? C76 C78 C79 C80 0.8(18) . . . . ? C75 C74 C80 C79 0.3(15) . . . . ? C77 C74 C80 C79 179.8(9) . . . . ? C75 C74 C80 C81 178.5(10) . . . . ? C77 C74 C80 C81 -2.0(15) . . . . ? C78 C79 C80 C74 -0.3(16) . . . . ? C78 C79 C80 C81 -178.6(10) . . . . ? C74 C80 C81 O14 -178.7(9) . . . . ? C79 C80 C81 O14 -0.5(14) . . . . ? C74 C80 C81 C82 -0.7(14) . . . . ? C79 C80 C81 C82 177.5(9) . . . . ? O14 C81 C82 C126 1.8(15) . . . . ? C80 C81 C82 C126 -175.9(9) . . . . ? O14 C81 C82 C73 -179.9(9) . . . . ? C80 C81 C82 C73 2.4(13) . . . . ? C72 C73 C82 C81 -176.6(9) . . . . ? C77 C73 C82 C81 -1.2(14) . . . . ? C72 C73 C82 C126 1.7(14) . . . . ? C77 C73 C82 C126 177.1(9) . . . . ? C89 C84 C85 C86 1.7(19) . . . . ? N8 C84 C85 C86 177.4(12) . . . . ? C84 C85 C86 C87 3(2) . . . . ? C85 C86 C87 C88 -5(3) . . . . ? C86 C87 C88 C89 2(2) . . . . ? C29 C30 C088 C26 -3.9(19) . . . . ? C29 C30 C088 N1 176.1(13) . . . . ? N2 C26 C088 C30 178.4(11) . . . . ? C27 C26 C088 C30 3.6(19) . . . . ? N2 C26 C088 N1 -1.6(13) . . . . ? C27 C26 C088 N1 -176.4(11) . . . . ? C85 C84 C89 N7 174.2(11) . . . . ? N8 C84 C89 N7 -2.2(13) . . . . ? C85 C84 C89 C88 -4.1(19) . . . . ? N8 C84 C89 C88 179.5(10) . . . . ? C87 C88 C89 C84 1.9(19) . . . . ? C87 C88 C89 N7 -176.0(13) . . . . ? N8 C91 C92 C97 -117.8(10) . . . . ? N8 C91 C92 C93 66.3(12) . . . . ? C97 C92 C93 C94 0.2(14) . . . . ? C91 C92 C93 C94 176.2(9) . . . . ? C97 C92 C93 C98 179.7(9) . . . . ? C91 C92 C93 C98 -4.4(14) . . . . ? C92 C93 C94 C95 -1.5(15) . . . . ? C98 C93 C94 C95 179.1(9) . . . . ? C92 C93 C94 C101 -175.9(9) . . . . ? C98 C93 C94 C101 4.7(14) . . . . ? C93 C94 C95 C96 3.4(15) . . . . ? C101 C94 C95 C96 177.8(9) . . . . ? C93 C94 C95 C99 -176.7(10) . . . . ? C101 C94 C95 C99 -2.3(14) . . . . ? C94 C95 C96 C97 -4.2(14) . . . . ? C99 C95 C96 C97 175.8(9) . . . . ? C94 C95 C96 C110 178.5(9) . . . . ? C99 C95 C96 C110 -1.5(14) . . . . ? C93 C92 C97 C96 -1.0(14) . . . . ? C91 C92 C97 C96 -176.8(9) . . . . ? C93 C92 C97 C100 -179.7(9) . . . . ? C91 C92 C97 C100 4.5(14) . . . . ? C95 C96 C97 C92 3.0(14) . . . . ? C110 C96 C97 C92 -179.7(9) . . . . ? C95 C96 C97 C100 -178.3(9) . . . . ? C110 C96 C97 C100 -1.0(14) . . . . ? C93 C94 C101 N10 -65.5(13) . . . . ? C95 C94 C101 N10 119.9(10) . . . . ? N10 C103 C104 C105 180.0(12) . . . . ? C108 C103 C104 C105 4.4(17) . . . . ? C103 C104 C105 C106 -2.4(19) . . . . ? C104 C105 C106 C107 0(2) . . . . ? C105 C106 C107 C108 0(2) . . . . ? C106 C107 C108 C103 1.8(17) . . . . ? C106 C107 C108 N9 177.8(11) . . . . ? N10 C103 C108 C107 179.2(10) . . . . ? C104 C103 C108 C107 -4.2(16) . . . . ? N10 C103 C108 N9 2.4(12) . . . . ? C104 C103 C108 N9 178.9(9) . . . . ? C95 C96 C110 N11 -65.5(13) . . . . ? C97 C96 C110 N11 117.1(10) . . . . ? N12 C112 C113 C114 -178.0(13) . . . . ? C117 C112 C113 C114 1(2) . . . . ? C112 C113 C114 C115 1(2) . . . . ? C113 C114 C115 C116 -3(2) . . . . ? C114 C115 C116 C117 1(2) . . . . ? C115 C116 C117 N11 176.7(12) . . . . ? C115 C116 C117 C112 1.6(19) . . . . ? N12 C112 C117 C116 176.5(11) . . . . ? C113 C112 C117 C116 -2.9(19) . . . . ? N12 C112 C117 N11 0.2(13) . . . . ? C113 C112 C117 N11 -179.2(11) . . . . ? C67 C66 C126 O13 0.5(15) . . . . ? C71 C66 C126 O13 -178.7(9) . . . . ? C67 C66 C126 C82 -177.3(10) . . . . ? C71 C66 C126 C82 3.4(15) . . . . ? C81 C82 C126 O13 -3.1(15) . . . . ? C73 C82 C126 O13 178.5(9) . . . . ? C81 C82 C126 C66 174.5(9) . . . . ? C73 C82 C126 C66 -3.9(14) . . . . ? C24 C7 O7 Re1 -6.8(16) . . . . ? C8 C7 O7 Re1 175.2(6) . . . . ? C24 C23 O8 Re1 10.1(16) . . . . ? C22 C23 O8 Re1 -170.2(7) . . . . ? C13 C14 O9 Re2 -169.6(6) . . . . ? C15 C14 O9 Re2 11.2(15) . . . . ? C15 C16 O10 Re2 -17.6(15) . . . . ? C17 C16 O10 Re2 164.4(7) . . . . ? C73 C72 O11 Re4 15.9(15) . . . . ? C71 C72 O11 Re4 -165.0(6) . . . . ? C73 C77 O12 Re4 -11.9(15) . . . . ? C74 C77 O12 Re4 167.5(7) . . . . ? C66 C126 O13 Re3 172.5(7) . . . . ? C82 C126 O13 Re3 -9.8(16) . . . . ? C82 C81 O14 Re3 12.7(15) . . . . ? C80 C81 O14 Re3 -169.6(6) . . . . ? N1 C25 S1 C31 -112.4(11) . . . . ? N2 C25 S1 C31 68.9(12) . . . . ? N3 C52 S2 C59 118.2(11) . . . . ? N4 C52 S2 C59 -65.4(11) . . . . ? N5 C49 S3 C50 176.2(14) . . . . ? N6 C49 S3 C50 -2.3(16) . . . . ? N7 C83 S4 C90 117.1(10) . . . . ? N8 C83 S4 C90 -64.6(10) . . . . ? N9 C102 S5 C109 -114.4(10) . . . . ? N10 C102 S5 C109 70.4(10) . . . . ? N12 C111 S6 C118 11.9(13) . . . . ? N11 C111 S6 C118 -172.6(10) . . . . ? O3 C3 Re1 C2 -102(27) . . . . ? O3 C3 Re1 C1 -14(27) . . . . ? O3 C3 Re1 O7 97(27) . . . . ? O3 C3 Re1 O8 81(27) . . . . ? O3 C3 Re1 N1 165(27) . . . . ? O2 C2 Re1 C3 44(23) . . . . ? O2 C2 Re1 C1 -42(23) . . . . ? O2 C2 Re1 O7 -137(23) . . . . ? O2 C2 Re1 O8 161(18) . . . . ? O2 C2 Re1 N1 139(23) . . . . ? O1 C1 Re1 C3 -21(17) . . . . ? O1 C1 Re1 C2 65(17) . . . . ? O1 C1 Re1 O7 163(17) . . . . ? O1 C1 Re1 O8 -116(17) . . . . ? O1 C1 Re1 N1 -169(31) . . . . ? C7 O7 Re1 C3 -4(6) . . . . ? C7 O7 Re1 C2 -165.7(10) . . . . ? C7 O7 Re1 C1 106.5(10) . . . . ? C7 O7 Re1 O8 11.2(9) . . . . ? C7 O7 Re1 N1 -73.1(9) . . . . ? C23 O8 Re1 C3 166.1(10) . . . . ? C23 O8 Re1 C2 49(7) . . . . ? C23 O8 Re1 C1 -107.7(10) . . . . ? C23 O8 Re1 O7 -12.8(9) . . . . ? C23 O8 Re1 N1 71.6(9) . . . . ? O4 C4 Re2 C5 -37(31) . . . . ? O4 C4 Re2 C6 49(31) . . . . ? O4 C4 Re2 O9 146(31) . . . . ? O4 C4 Re2 O10 -139(27) . . . . ? O4 C4 Re2 N3 -131(31) . . . . ? O5 C5 Re2 C4 141(38) . . . . ? O5 C5 Re2 C6 55(38) . . . . ? O5 C5 Re2 O9 -74(40) . . . . ? O5 C5 Re2 O10 -43(38) . . . . ? O5 C5 Re2 N3 -127(38) . . . . ? O6 C6 Re2 C4 -30(11) . . . . ? O6 C6 Re2 C5 56(11) . . . . ? O6 C6 Re2 O9 -128(11) . . . . ? O6 C6 Re2 O10 151(11) . . . . ? O6 C6 Re2 N3 -20(23) . . . . ? C14 O9 Re2 C4 157.3(10) . . . . ? C14 O9 Re2 C5 13(5) . . . . ? C14 O9 Re2 C6 -115.9(10) . . . . ? C14 O9 Re2 O10 -19.0(9) . . . . ? C14 O9 Re2 N3 65.8(9) . . . . ? C16 O10 Re2 C4 -54(6) . . . . ? C16 O10 Re2 C5 -155.3(9) . . . . ? C16 O10 Re2 C6 118.4(9) . . . . ? C16 O10 Re2 O9 21.9(9) . . . . ? C16 O10 Re2 N3 -61.9(9) . . . . ? O15 C60 Re3 C62 34(100) . . . . ? O15 C60 Re3 C61 -53(100) . . . . ? O15 C60 Re3 O14 171(100) . . . . ? O15 C60 Re3 O13 -148(100) . . . . ? O15 C60 Re3 N7 128(100) . . . . ? O16 C62 Re3 C60 -92(45) . . . . ? O16 C62 Re3 C61 -9(45) . . . . ? O16 C62 Re3 O14 91(45) . . . . ? O16 C62 Re3 O13 107(43) . . . . ? O16 C62 Re3 N7 175(100) . . . . ? O17 C61 Re3 C60 4(9) . . . . ? O17 C61 Re3 C62 -85(9) . . . . ? O17 C61 Re3 O14 -180(100) . . . . ? O17 C61 Re3 O13 99(9) . . . . ? O17 C61 Re3 N7 12(13) . . . . ? C81 O14 Re3 C60 24(5) . . . . ? C81 O14 Re3 C62 161.5(9) . . . . ? C81 O14 Re3 C61 -111.0(9) . . . . ? C81 O14 Re3 O13 -17.0(9) . . . . ? C81 O14 Re3 N7 68.2(9) . . . . ? C126 O13 Re3 C60 -160.9(10) . . . . ? C126 O13 Re3 C62 -1(5) . . . . ? C126 O13 Re3 C61 115.3(10) . . . . ? C126 O13 Re3 O14 15.7(9) . . . . ? C126 O13 Re3 N7 -69.0(10) . . . . ? O20 C65 Re4 C63 59(86) . . . . ? O20 C65 Re4 C64 -28(86) . . . . ? O20 C65 Re4 O12 -165(100) . . . . ? O20 C65 Re4 O11 154(86) . . . . ? O20 C65 Re4 N9 -123(86) . . . . ? O18 C63 Re4 C65 -39(14) . . . . ? O18 C63 Re4 C64 49(14) . . . . ? O18 C63 Re4 O12 145(14) . . . . ? O18 C63 Re4 O11 -135(14) . . . . ? O18 C63 Re4 N9 -146(11) . . . . ? O19 C64 Re4 C65 79(26) . . . . ? O19 C64 Re4 C63 -9(26) . . . . ? O19 C64 Re4 O12 -105(26) . . . . ? O19 C64 Re4 O11 -131(23) . . . . ? O19 C64 Re4 N9 172(100) . . . . ? C77 O12 Re4 C65 -21(5) . . . . ? C77 O12 Re4 C63 114.8(9) . . . . ? C77 O12 Re4 C64 -157.0(9) . . . . ? C77 O12 Re4 O11 20.9(8) . . . . ? C77 O12 Re4 N9 -63.1(9) . . . . ? C72 O11 Re4 C65 153.7(9) . . . . ? C72 O11 Re4 C63 -118.1(9) . . . . ? C72 O11 Re4 C64 4(6) . . . . ? C72 O11 Re4 O12 -23.0(8) . . . . ? C72 O11 Re4 N9 61.5(9) . . . . ? N2 C25 N1 C088 -2.9(13) . . . . ? S1 C25 N1 C088 178.3(8) . . . . ? N2 C25 N1 Re1 178.0(7) . . . . ? S1 C25 N1 Re1 -0.9(15) . . . . ? C30 C088 N1 C25 -177.3(13) . . . . ? C26 C088 N1 C25 2.7(12) . . . . ? C30 C088 N1 Re1 1.9(18) . . . . ? C26 C088 N1 Re1 -178.1(7) . . . . ? C3 Re1 N1 C25 132.5(10) . . . . ? C2 Re1 N1 C25 45.8(10) . . . . ? C1 Re1 N1 C25 -80(30) . . . . ? O7 Re1 N1 C25 -51.5(9) . . . . ? O8 Re1 N1 C25 -132.9(10) . . . . ? C3 Re1 N1 C088 -46.5(9) . . . . ? C2 Re1 N1 C088 -133.2(9) . . . . ? C1 Re1 N1 C088 101(30) . . . . ? O7 Re1 N1 C088 129.5(9) . . . . ? O8 Re1 N1 C088 48.2(8) . . . . ? N1 C25 N2 C26 2.0(13) . . . . ? S1 C25 N2 C26 -179.2(9) . . . . ? N1 C25 N2 C32 -179.4(10) . . . . ? S1 C25 N2 C32 -0.6(16) . . . . ? C088 C26 N2 C25 -0.2(13) . . . . ? C27 C26 N2 C25 174.0(13) . . . . ? C088 C26 N2 C32 -178.8(10) . . . . ? C27 C26 N2 C32 -5(2) . . . . ? C33 C32 N2 C25 134.2(11) . . . . ? C33 C32 N2 C26 -47.4(16) . . . . ? N4 C52 N3 C58 1.4(12) . . . . ? S2 C52 N3 C58 178.1(8) . . . . ? N4 C52 N3 Re2 177.5(7) . . . . ? S2 C52 N3 Re2 -5.7(14) . . . . ? C53 C58 N3 C52 -1.1(12) . . . . ? C57 C58 N3 C52 -179.8(12) . . . . ? C53 C58 N3 Re2 -177.2(7) . . . . ? C57 C58 N3 Re2 4.1(17) . . . . ? C4 Re2 N3 C52 -40.5(9) . . . . ? C5 Re2 N3 C52 -126.3(9) . . . . ? C6 Re2 N3 C52 -50(15) . . . . ? O9 Re2 N3 C52 57.9(9) . . . . ? O10 Re2 N3 C52 138.9(9) . . . . ? C4 Re2 N3 C58 134.8(9) . . . . ? C5 Re2 N3 C58 48.9(10) . . . . ? C6 Re2 N3 C58 125(15) . . . . ? O9 Re2 N3 C58 -126.8(9) . . . . ? O10 Re2 N3 C58 -45.8(9) . . . . ? N3 C52 N4 C53 -1.2(12) . . . . ? S2 C52 N4 C53 -178.0(8) . . . . ? N3 C52 N4 C51 -179.7(10) . . . . ? S2 C52 N4 C51 3.5(15) . . . . ? C54 C53 N4 C52 -179.4(14) . . . . ? C58 C53 N4 C52 0.4(12) . . . . ? C54 C53 N4 C51 -1(2) . . . . ? C58 C53 N4 C51 178.8(10) . . . . ? C37 C51 N4 C52 -138.5(10) . . . . ? C37 C51 N4 C53 43.4(15) . . . . ? N6 C49 N5 C43 -3.1(17) . . . . ? S3 C49 N5 C43 178.2(12) . . . . ? N6 C49 N5 C42 179.8(14) . . . . ? S3 C49 N5 C42 1(2) . . . . ? C44 C43 N5 C49 -177.6(19) . . . . ? C48 C43 N5 C49 3.3(17) . . . . ? C44 C43 N5 C42 0(3) . . . . ? C48 C43 N5 C42 -179.0(13) . . . . ? C35 C42 N5 C49 -6(2) . . . . ? C35 C42 N5 C43 176.9(12) . . . . ? N5 C49 N6 C48 1.8(18) . . . . ? S3 C49 N6 C48 -179.6(13) . . . . ? C43 C48 N6 C49 0(2) . . . . ? C47 C48 N6 C49 177(2) . . . . ? N8 C83 N7 C89 0.3(12) . . . . ? S4 C83 N7 C89 178.8(8) . . . . ? N8 C83 N7 Re3 169.8(6) . . . . ? S4 C83 N7 Re3 -11.7(13) . . . . ? C84 C89 N7 C83 1.2(12) . . . . ? C88 C89 N7 C83 179.3(12) . . . . ? C84 C89 N7 Re3 -168.8(7) . . . . ? C88 C89 N7 Re3 9.3(17) . . . . ? C60 Re3 N7 C83 -123.3(9) . . . . ? C62 Re3 N7 C83 -34.3(9) . . . . ? C61 Re3 N7 C83 -131(5) . . . . ? O14 Re3 N7 C83 60.3(9) . . . . ? O13 Re3 N7 C83 140.7(9) . . . . ? C60 Re3 N7 C89 44.4(9) . . . . ? C62 Re3 N7 C89 133.3(9) . . . . ? C61 Re3 N7 C89 37(5) . . . . ? O14 Re3 N7 C89 -132.0(8) . . . . ? O13 Re3 N7 C89 -51.6(8) . . . . ? N7 C83 N8 C84 -1.6(11) . . . . ? S4 C83 N8 C84 179.9(8) . . . . ? N7 C83 N8 C91 173.5(9) . . . . ? S4 C83 N8 C91 -5.0(15) . . . . ? C85 C84 N8 C83 -174.0(12) . . . . ? C89 C84 N8 C83 2.2(12) . . . . ? C85 C84 N8 C91 10.9(18) . . . . ? C89 C84 N8 C91 -172.9(10) . . . . ? C92 C91 N8 C83 -127.4(10) . . . . ? C92 C91 N8 C84 46.7(14) . . . . ? N10 C102 N9 C108 -0.5(12) . . . . ? S5 C102 N9 C108 -176.2(8) . . . . ? N10 C102 N9 Re4 -177.5(6) . . . . ? S5 C102 N9 Re4 6.9(14) . . . . ? C107 C108 N9 C102 -177.6(12) . . . . ? C103 C108 N9 C102 -1.1(11) . . . . ? C107 C108 N9 Re4 -0.5(16) . . . . ? C103 C108 N9 Re4 175.9(7) . . . . ? C65 Re4 N9 C102 126.4(10) . . . . ? C63 Re4 N9 C102 -127(11) . . . . ? C64 Re4 N9 C102 38.7(10) . . . . ? O12 Re4 N9 C102 -56.9(9) . . . . ? O11 Re4 N9 C102 -137.5(9) . . . . ? C65 Re4 N9 C108 -50.0(9) . . . . ? C63 Re4 N9 C108 57(12) . . . . ? C64 Re4 N9 C108 -137.7(8) . . . . ? O12 Re4 N9 C108 126.7(8) . . . . ? O11 Re4 N9 C108 46.1(8) . . . . ? N9 C102 N10 C103 2.0(12) . . . . ? S5 C102 N10 C103 177.6(8) . . . . ? N9 C102 N10 C101 172.8(9) . . . . ? S5 C102 N10 C101 -11.6(15) . . . . ? C108 C103 N10 C102 -2.6(11) . . . . ? C104 C103 N10 C102 -178.6(12) . . . . ? C108 C103 N10 C101 -173.0(9) . . . . ? C104 C103 N10 C101 11.0(19) . . . . ? C94 C101 N10 C102 140.9(10) . . . . ? C94 C101 N10 C103 -50.4(14) . . . . ? N12 C111 N11 C117 -1.3(13) . . . . ? S6 C111 N11 C117 -177.3(8) . . . . ? N12 C111 N11 C110 176.6(10) . . . . ? S6 C111 N11 C110 0.5(15) . . . . ? C116 C117 N11 C111 -175.1(13) . . . . ? C112 C117 N11 C111 0.6(12) . . . . ? C116 C117 N11 C110 7(2) . . . . ? C112 C117 N11 C110 -177.1(10) . . . . ? C96 C110 N11 C111 143.0(10) . . . . ? C96 C110 N11 C117 -39.7(15) . . . . ? N11 C111 N12 C112 1.3(14) . . . . ? S6 C111 N12 C112 177.1(10) . . . . ? C113 C112 N12 C111 178.4(14) . . . . ? C117 C112 N12 C111 -0.9(14) . . . . ? C4A C5A C6A C1A 1(4) . . . . ? C2A C3A C4A C5A -2(4) . . . . ? C2A C3A C4A C7A 180(2) . . . . ? C6A C5A C4A C3A 0(4) . . . . ? C6A C5A C4A C7A 177(2) . . . . ? C5A C6A C1A C2A 2(4) . . . . ? C6A C1A C2A C3A -5(4) . . . . ? C4A C3A C2A C1A 6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.992 _refine_diff_density_min -1.089 _refine_diff_density_rms 0.182 _iucr_instructions_refinement_details ; TITL RK5-94- in P2(1)/c CELL 0.71073 28.6866 18.3837 25.0892 90.000 111.660 90.000 ZERR 4.00 0.0015 0.0009 0.0014 0.000 0.006 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O S RE N UNIT 508 384 80 24 16 48 MERG 2 DFIX 1.390 0.020 C2A C1A C6A C5A C4A C3A DFIX 1.430 0.020 C4A C7A DFIX 1.390 0.020 C43 C44 DFIX 1.390 0.020 C44 C45 DFIX 1.390 0.020 C45 C46 DFIX 1.390 0.020 C46 C47 DFIX 1.390 0.020 C47 C48 DFIX 1.390 0.020 C43 C48 DFIX 1.390 0.020 C43 N5 DFIX 1.390 0.020 C48 N6 FMAP 2 PLAN 20 SIZE 0.18 0.24 0.31 ACTA BOND $H CONF shel 0.8 30 L.S. 12 TEMP 20.00 WGHT 0.078900 31.327400 FVAR 0.39798 C1 1 0.330037 0.180621 0.290274 11.00000 0.05860 0.06800 = 0.04743 0.00590 0.03912 0.00170 C2 1 0.326334 0.045557 0.323490 11.00000 0.04082 0.05816 = 0.04583 -0.00958 0.02036 -0.00557 C3 1 0.383247 0.140377 0.393500 11.00000 0.04117 0.05030 = 0.05454 -0.00747 0.02034 -0.00360 C4 1 0.590538 0.052040 0.083070 11.00000 0.04696 0.08293 = 0.03838 0.00786 0.01665 -0.01559 C5 1 0.644580 0.146877 0.155177 11.00000 0.05197 0.08718 = 0.04386 0.00629 0.01827 0.00813 C6 1 0.560262 0.186349 0.075884 11.00000 0.04923 0.09145 = 0.04889 -0.00276 0.02801 -0.00153 C7 1 0.412790 0.077965 0.218169 11.00000 0.03034 0.03601 = 0.03786 0.00071 0.01507 -0.00091 C8 1 0.400189 0.038534 0.164071 11.00000 0.03189 0.03578 = 0.02764 0.00500 0.01445 -0.00123 C9 1 0.355826 -0.000859 0.142860 11.00000 0.03132 0.07132 = 0.03562 -0.00536 0.01409 -0.01734 AFIX 43 H9 2 0.334833 -0.002606 0.163576 11.00000 -1.20000 AFIX 0 C10 1 0.342839 -0.036679 0.092439 11.00000 0.04504 0.06564 = 0.03523 -0.01078 0.01070 -0.01904 AFIX 43 H10 2 0.312270 -0.060935 0.077821 11.00000 -1.20000 AFIX 0 C11 1 0.374960 -0.037502 0.062212 11.00000 0.03208 0.08383 = 0.04278 -0.01825 0.01966 -0.01093 AFIX 43 H11 2 0.366896 -0.064407 0.028611 11.00000 -1.20000 AFIX 0 C12 1 0.418652 0.001875 0.082622 11.00000 0.04587 0.07483 = 0.04279 0.00419 0.02952 -0.00910 AFIX 43 H12 2 0.439859 0.002551 0.062145 11.00000 -1.20000 AFIX 0 C13 1 0.431557 0.040762 0.133562 11.00000 0.03037 0.03948 = 0.03273 0.00565 0.01295 0.00043 C14 1 0.477395 0.082258 0.154043 11.00000 0.02606 0.04531 = 0.04044 0.01068 0.01823 0.00737 C15 1 0.490247 0.124452 0.206266 11.00000 0.02837 0.04292 = 0.03163 0.00328 0.01088 0.00231 C16 1 0.532451 0.169159 0.224387 11.00000 0.03036 0.03241 = 0.04185 0.01151 0.00959 0.00120 C17 1 0.542806 0.213346 0.275918 11.00000 0.03429 0.04516 = 0.05432 -0.00249 0.02511 -0.01165 C18 1 0.586022 0.257163 0.295691 11.00000 0.03918 0.06022 = 0.05890 -0.00648 0.02264 -0.01007 AFIX 43 H18 2 0.607500 0.258534 0.275564 11.00000 -1.20000 AFIX 0 C19 1 0.596669 0.298165 0.344907 11.00000 0.06352 0.06725 = 0.08097 -0.01924 0.03219 -0.02905 AFIX 43 H19 2 0.623840 0.329889 0.356353 11.00000 -1.20000 AFIX 0 C20 1 0.566672 0.291848 0.377209 11.00000 0.09231 0.05719 = 0.06216 -0.01324 0.03573 -0.01260 AFIX 43 H20 2 0.574933 0.316917 0.411672 11.00000 -1.20000 AFIX 0 C21 1 0.525056 0.248787 0.358285 11.00000 0.05762 0.04054 = 0.08070 -0.02363 0.03627 -0.01976 AFIX 43 H21 2 0.504753 0.245976 0.379789 11.00000 -1.20000 AFIX 0 C22 1 0.512141 0.209096 0.307943 11.00000 0.03282 0.03768 = 0.04880 -0.00034 0.01553 -0.00826 C23 1 0.467601 0.163882 0.288223 11.00000 0.03624 0.02796 = 0.05483 0.00826 0.02586 0.00305 C24 1 0.456874 0.121645 0.238033 11.00000 0.03798 0.02963 = 0.02652 0.00067 0.00983 -0.00068 C25 1 0.434216 -0.048885 0.341185 11.00000 0.03771 0.03276 = 0.04752 0.00692 0.00988 0.00597 C26 1 0.509191 -0.036581 0.409558 11.00000 0.04284 0.04013 = 0.05324 0.00193 0.01820 0.00238 C27 1 0.556291 -0.046358 0.453646 11.00000 0.04052 0.06695 = 0.05646 -0.00815 0.00792 0.00491 AFIX 43 H27 2 0.573228 -0.090548 0.459506 11.00000 -1.20000 AFIX 0 C28 1 0.575380 0.012109 0.486853 11.00000 0.06340 0.06178 = 0.05929 -0.00669 0.00277 0.00659 AFIX 43 H28 2 0.606195 0.007536 0.516903 11.00000 -1.20000 AFIX 0 C29 1 0.550857 0.079728 0.478169 11.00000 0.07042 0.07664 = 0.06117 -0.02725 0.00839 -0.01196 AFIX 43 H29 2 0.565732 0.118735 0.501974 11.00000 -1.20000 AFIX 0 C30 1 0.505053 0.088463 0.434714 11.00000 0.04526 0.04453 = 0.07255 -0.02062 0.01611 -0.00114 AFIX 43 H30 2 0.489042 0.133407 0.428044 11.00000 -1.20000 AFIX 0 C31 1 0.360672 -0.147876 0.329680 11.00000 0.05971 0.07659 = 0.12092 0.01286 0.01305 -0.02090 AFIX 137 H31A 2 0.388033 -0.160348 0.364361 11.00000 -1.50000 H31B 2 0.347545 -0.191243 0.308022 11.00000 -1.50000 H31C 2 0.334760 -0.124464 0.339033 11.00000 -1.50000 AFIX 0 C32 1 0.487387 -0.161808 0.364182 11.00000 0.05286 0.03771 = 0.05077 -0.00801 0.02103 -0.00962 AFIX 23 H32A 2 0.461193 -0.179342 0.329570 11.00000 -1.20000 H32B 2 0.484351 -0.188434 0.396123 11.00000 -1.20000 AFIX 0 C33 1 0.537581 -0.181074 0.360591 11.00000 0.03465 0.03865 = 0.03874 -0.00422 0.01043 -0.00238 C34 1 0.571054 -0.227175 0.401823 11.00000 0.03601 0.03217 = 0.03092 -0.00352 -0.00154 0.00007 C35 1 0.614772 -0.247921 0.394356 11.00000 0.04644 0.03715 = 0.02362 0.00259 0.00474 -0.00124 C36 1 0.626517 -0.222105 0.347760 11.00000 0.04001 0.02783 = 0.04679 -0.00155 0.00848 0.00810 C37 1 0.592277 -0.177100 0.306951 11.00000 0.03754 0.03562 = 0.03546 -0.00598 0.01089 -0.00070 C38 1 0.548366 -0.155079 0.313776 11.00000 0.05038 0.03042 = 0.04266 -0.00416 0.00706 -0.00676 C39 1 0.559453 -0.256119 0.451384 11.00000 0.05125 0.05612 = 0.03349 0.00592 0.00799 -0.00191 AFIX 137 H39A 2 0.540583 -0.300381 0.440238 11.00000 -1.50000 H39B 2 0.540153 -0.220874 0.462642 11.00000 -1.50000 H39C 2 0.590192 -0.265645 0.483021 11.00000 -1.50000 AFIX 0 C40 1 0.675617 -0.243318 0.343907 11.00000 0.05418 0.08838 = 0.05518 0.02129 0.02432 0.03537 AFIX 137 H40A 2 0.682772 -0.211723 0.317425 11.00000 -1.50000 H40B 2 0.673747 -0.292671 0.330770 11.00000 -1.50000 H40C 2 0.701785 -0.239150 0.381056 11.00000 -1.50000 AFIX 0 C41 1 0.509777 -0.107516 0.268116 11.00000 0.03863 0.06327 = 0.04929 0.01521 0.00993 0.01273 AFIX 137 H41A 2 0.520305 -0.057603 0.273713 11.00000 -1.50000 H41B 2 0.477657 -0.112209 0.271509 11.00000 -1.50000 H41C 2 0.507287 -0.123054 0.230631 11.00000 -1.50000 AFIX 0 C42 1 0.647841 -0.305577 0.432678 11.00000 0.05562 0.04624 = 0.03283 0.00495 -0.00388 0.01295 AFIX 23 H42A 2 0.626675 -0.339032 0.443441 11.00000 -1.20000 H42B 2 0.663353 -0.332872 0.410536 11.00000 -1.20000 AFIX 0 C43 1 0.717724 -0.334633 0.523581 11.00000 0.04061 0.32045 = 0.02257 -0.03830 -0.00055 -0.01131 C44 1 0.719595 -0.404722 0.524499 11.00000 0.04373 AFIX 43 H44 2 0.696617 -0.425918 0.491637 11.00000 -1.20000 AFIX 0 C45 1 0.747312 -0.453363 0.562324 11.00000 0.12591 0.09140 = 0.12777 0.01530 0.00436 0.00006 AFIX 43 H45 2 0.744007 -0.503675 0.559316 11.00000 -1.20000 AFIX 0 C46 1 0.780291 -0.416838 0.604801 11.00000 0.06188 0.07043 = 0.09088 -0.00417 -0.02657 0.00710 AFIX 43 H46 2 0.803439 -0.444490 0.633501 11.00000 -1.20000 AFIX 0 C47 1 0.784361 -0.344160 0.611472 11.00000 0.08531 0.12850 = 0.06862 0.02069 -0.01786 -0.00121 AFIX 43 H47 2 0.808773 -0.323572 0.643534 11.00000 -1.20000 AFIX 0 C48 1 0.750654 -0.300311 0.568587 11.00000 0.07239 0.11967 = 0.07245 -0.00021 0.01791 -0.01539 C49 1 0.706573 -0.215076 0.508762 11.00000 0.09883 0.08967 = 0.04804 -0.01941 0.02846 -0.05012 C50 1 0.726190 -0.077069 0.537993 11.00000 0.17498 0.09124 = 0.15295 -0.03441 0.08246 -0.06995 AFIX 137 H50A 2 0.728558 -0.097228 0.574200 11.00000 -1.50000 H50B 2 0.712266 -0.028987 0.534095 11.00000 -1.50000 H50C 2 0.759009 -0.074786 0.536192 11.00000 -1.50000 AFIX 0 C51 1 0.601668 -0.158413 0.252656 11.00000 0.04395 0.05133 = 0.03541 0.01059 0.00761 0.01138 AFIX 23 H51A 2 0.631874 -0.182877 0.253441 11.00000 -1.20000 H51B 2 0.573897 -0.176103 0.219586 11.00000 -1.20000 AFIX 0 C52 1 0.587107 -0.039739 0.196310 11.00000 0.03797 0.05803 = 0.03014 0.00899 0.01730 0.01169 C53 1 0.634077 -0.028711 0.288220 11.00000 0.05134 0.05222 = 0.03995 -0.00058 0.01863 -0.01344 C54 1 0.662245 -0.035621 0.345882 11.00000 0.08174 0.07261 = 0.03923 0.01080 0.00309 -0.02264 AFIX 43 H54 2 0.665667 -0.079911 0.364866 11.00000 -1.20000 AFIX 0 C55 1 0.684250 0.024639 0.372826 11.00000 0.11321 0.09820 = 0.03615 0.00765 -0.00393 -0.04652 AFIX 43 H55 2 0.704632 0.021434 0.411417 11.00000 -1.20000 AFIX 0 C56 1 0.678307 0.092535 0.346106 11.00000 0.09803 0.06322 = 0.05290 -0.00120 0.00089 -0.03057 AFIX 43 H56 2 0.694298 0.132888 0.367380 11.00000 -1.20000 AFIX 0 C57 1 0.650197 0.100592 0.290778 11.00000 0.06909 0.06112 = 0.04549 -0.00193 0.01669 -0.01627 AFIX 43 H57 2 0.645406 0.145845 0.272990 11.00000 -1.20000 AFIX 0 C58 1 0.628228 0.037546 0.260747 11.00000 0.04550 0.05547 = 0.02424 0.00313 0.01667 -0.00046 C59 1 0.588642 -0.144406 0.115354 11.00000 0.13678 0.07807 = 0.06193 -0.01696 0.05611 0.02315 AFIX 137 H59A 2 0.615439 -0.118399 0.109631 11.00000 -1.50000 H59B 2 0.569792 -0.170631 0.081063 11.00000 -1.50000 H59C 2 0.602328 -0.177999 0.146559 11.00000 -1.50000 AFIX 0 C60 1 0.875648 0.057730 0.023893 11.00000 0.07035 0.06662 = 0.03559 -0.00498 0.01037 0.01319 C61 1 0.959852 0.000905 0.037710 11.00000 0.06578 0.05151 = 0.03310 0.00426 0.02026 -0.02294 C62 1 0.947754 0.139888 0.012207 11.00000 0.07255 0.04399 = 0.03919 -0.00838 0.00589 0.01526 C63 1 1.140113 0.020471 0.465956 11.00000 0.05192 0.05863 = 0.03654 -0.00328 0.01185 0.00435 C64 1 1.139923 0.161121 0.487739 11.00000 0.05221 0.05583 = 0.04240 0.00201 0.01239 0.00696 C65 1 1.070676 0.075622 0.498419 11.00000 0.05718 0.05898 = 0.03739 0.01135 0.01346 0.01274 C66 1 0.949170 -0.014116 0.235514 11.00000 0.03418 0.03270 = 0.03782 -0.00343 0.01747 -0.00887 C67 1 0.906877 -0.056985 0.211486 11.00000 0.05544 0.05635 = 0.03685 -0.00857 0.01548 -0.02404 AFIX 43 H67 2 0.890222 -0.058827 0.171916 11.00000 -1.20000 AFIX 0 C68 1 0.889642 -0.097374 0.247572 11.00000 0.06393 0.07545 = 0.06474 0.00584 0.02521 -0.04554 AFIX 43 H68 2 0.861032 -0.125758 0.231357 11.00000 -1.20000 AFIX 0 C69 1 0.913399 -0.096754 0.306219 11.00000 0.06363 0.06922 = 0.05598 0.01353 0.03188 -0.02513 AFIX 43 H69 2 0.901321 -0.124199 0.329493 11.00000 -1.20000 AFIX 0 C70 1 0.956292 -0.053588 0.329831 11.00000 0.04899 0.03883 = 0.03755 0.00214 0.01933 -0.00541 AFIX 43 H70 2 0.972857 -0.052193 0.369427 11.00000 -1.20000 AFIX 0 C71 1 0.974291 -0.013460 0.295814 11.00000 0.04200 0.02063 = 0.04341 0.00083 0.02547 -0.00370 C72 1 1.018903 0.031233 0.321990 11.00000 0.03241 0.02992 = 0.02867 -0.00401 0.01072 0.00579 C73 1 1.037139 0.072344 0.286239 11.00000 0.04264 0.02460 = 0.03495 -0.00274 0.01947 0.00229 C74 1 1.104243 0.147331 0.273093 11.00000 0.02472 0.03893 = 0.04968 -0.00099 0.01673 -0.00571 C75 1 1.151201 0.183456 0.297252 11.00000 0.04171 0.06130 = 0.05169 -0.00419 0.01245 -0.00953 AFIX 43 H75 2 1.168162 0.184006 0.336799 11.00000 -1.20000 AFIX 0 C76 1 1.171507 0.217546 0.262163 11.00000 0.03620 0.05642 = 0.07543 -0.01107 0.02128 -0.02540 AFIX 43 H76 2 1.202496 0.240530 0.277688 11.00000 -1.20000 AFIX 0 C77 1 1.083497 0.111329 0.311102 11.00000 0.02839 0.03114 = 0.03670 -0.01043 0.01195 0.00120 C78 1 1.145328 0.217362 0.203301 11.00000 0.04760 0.05724 = 0.07612 -0.00213 0.03870 -0.01140 AFIX 43 H78 2 1.158974 0.241306 0.179803 11.00000 -1.20000 AFIX 0 C79 1 1.100852 0.183648 0.179182 11.00000 0.04117 0.03949 = 0.05139 0.01163 0.02224 0.00321 AFIX 43 H79 2 1.084370 0.183974 0.139558 11.00000 -1.20000 AFIX 0 C80 1 1.079156 0.147581 0.214382 11.00000 0.02586 0.03889 = 0.04501 -0.00839 0.01690 0.00147 C81 1 1.031152 0.109908 0.186538 11.00000 0.03395 0.02966 = 0.04790 -0.00105 0.02588 0.00586 C82 1 1.011914 0.071742 0.224058 11.00000 0.03825 0.02150 = 0.03789 -0.00063 0.02019 -0.00160 C83 1 0.927708 0.245561 0.112323 11.00000 0.03857 0.04101 = 0.02884 -0.00606 0.02249 0.00199 C84 1 0.862389 0.242500 0.138408 11.00000 0.03337 0.07033 = 0.04227 -0.01482 0.02845 -0.00389 C85 1 0.821419 0.259684 0.151465 11.00000 0.05406 0.06235 = 0.07582 -0.02445 0.03343 -0.01652 AFIX 43 H85 2 0.813435 0.307106 0.157824 11.00000 -1.20000 AFIX 0 C86 1 0.792599 0.199413 0.154388 11.00000 0.07097 0.09687 = 0.11618 -0.04179 0.07264 -0.02875 AFIX 43 H86 2 0.763441 0.207681 0.161504 11.00000 -1.20000 AFIX 0 C87 1 0.805077 0.127741 0.147250 11.00000 0.06576 0.08405 = 0.09665 -0.02369 0.05159 -0.02427 AFIX 43 H87 2 0.785839 0.089661 0.152456 11.00000 -1.20000 AFIX 0 C88 1 0.845867 0.113282 0.132497 11.00000 0.05704 0.07754 = 0.07092 -0.01847 0.02807 -0.02541 AFIX 43 H88 2 0.854140 0.065979 0.126223 11.00000 -1.20000 AFIX 0 C088 1 0.483412 0.029362 0.401323 11.00000 0.03468 0.04507 = 0.03600 0.00071 0.00974 -0.00381 C89 1 0.874419 0.172953 0.127331 11.00000 0.04614 0.03507 = 0.04437 -0.01574 0.02522 -0.00901 C90 1 0.946238 0.335263 0.034946 11.00000 0.08978 0.07714 = 0.06646 0.01870 0.04862 -0.00083 AFIX 137 H90A 2 0.926457 0.305431 0.003265 11.00000 -1.50000 H90B 2 0.970597 0.361639 0.024719 11.00000 -1.50000 H90C 2 0.924796 0.368962 0.044206 11.00000 -1.50000 AFIX 0 C91 1 0.903302 0.367188 0.142682 11.00000 0.03396 0.03997 = 0.05213 0.00097 0.02778 0.00236 AFIX 23 H91A 2 0.876320 0.392968 0.113523 11.00000 -1.20000 H91B 2 0.934645 0.383454 0.140309 11.00000 -1.20000 AFIX 0 C92 1 0.902944 0.387402 0.200914 11.00000 0.02833 0.02910 = 0.03289 0.00442 0.01403 -0.00064 C93 1 0.943190 0.363300 0.250767 11.00000 0.03010 0.02804 = 0.04765 -0.00517 0.02020 0.00136 C94 1 0.944418 0.385274 0.303528 11.00000 0.03179 0.02503 = 0.03640 0.00200 0.01385 0.00223 C95 1 0.908321 0.431581 0.309963 11.00000 0.04073 0.02480 = 0.03787 0.00354 0.01811 0.00031 C96 1 0.868770 0.452383 0.260812 11.00000 0.03542 0.02746 = 0.05008 -0.00187 0.02876 -0.00646 C97 1 0.865743 0.432566 0.205765 11.00000 0.02752 0.02564 = 0.03832 0.00814 0.01161 -0.00358 C98 1 0.983296 0.314128 0.245524 11.00000 0.03788 0.04167 = 0.04994 -0.00392 0.01949 0.00492 AFIX 137 H98A 2 1.014019 0.321731 0.277651 11.00000 -1.50000 H98B 2 0.988405 0.324978 0.210647 11.00000 -1.50000 H98C 2 0.973019 0.264341 0.244932 11.00000 -1.50000 AFIX 0 C99 1 0.911647 0.458704 0.368377 11.00000 0.05914 0.05288 = 0.04188 -0.00435 0.01872 0.01335 AFIX 137 H99A 2 0.886647 0.495446 0.363619 11.00000 -1.50000 H99B 2 0.944330 0.478911 0.388386 11.00000 -1.50000 H99C 2 0.906068 0.418915 0.390084 11.00000 -1.50000 AFIX 0 C100 1 0.823076 0.458107 0.154010 11.00000 0.06574 0.05117 = 0.04584 0.00730 0.01962 0.00643 AFIX 137 H10A 2 0.832059 0.502973 0.140706 11.00000 -1.50000 H10B 2 0.794068 0.465661 0.163750 11.00000 -1.50000 H10C 2 0.815682 0.422100 0.124314 11.00000 -1.50000 AFIX 0 C101 1 0.989755 0.363504 0.356977 11.00000 0.04812 0.03021 = 0.04480 -0.00153 0.02066 0.00149 AFIX 23 H10D 2 1.020026 0.380774 0.352437 11.00000 -1.20000 H10E 2 0.987206 0.388035 0.390023 11.00000 -1.20000 AFIX 0 C102 1 1.039272 0.247937 0.388108 11.00000 0.03708 0.03133 = 0.03930 -0.00272 0.01069 0.00043 C103 1 0.959081 0.237634 0.371664 11.00000 0.03255 0.04328 = 0.04045 0.00068 0.01394 0.00597 C104 1 0.906706 0.244747 0.356507 11.00000 0.04506 0.03991 = 0.05320 0.00478 0.02276 0.01498 AFIX 43 H104 2 0.889946 0.287729 0.341377 11.00000 -1.20000 AFIX 0 C105 1 0.882031 0.185189 0.365251 11.00000 0.04854 0.06912 = 0.09214 -0.00123 0.04033 -0.01304 AFIX 43 H105 2 0.847735 0.188364 0.357131 11.00000 -1.20000 AFIX 0 C106 1 0.906459 0.120089 0.385856 11.00000 0.05567 0.03615 = 0.08162 0.01910 0.03787 -0.00375 AFIX 43 H106 2 0.888188 0.080840 0.391182 11.00000 -1.20000 AFIX 0 C107 1 0.955957 0.112485 0.398295 11.00000 0.04617 0.04765 = 0.04948 0.00979 0.01647 0.01081 AFIX 43 H107 2 0.971908 0.068481 0.411889 11.00000 -1.20000 AFIX 0 C108 1 0.982668 0.171413 0.390469 11.00000 0.04107 0.04510 = 0.02486 -0.00354 0.00674 0.00191 C109 1 1.111048 0.349389 0.446157 11.00000 0.05855 0.06730 = 0.09250 -0.03173 -0.00449 -0.00309 AFIX 137 H10F 2 1.088037 0.389410 0.433949 11.00000 -1.50000 H10G 2 1.144651 0.366695 0.455030 11.00000 -1.50000 H10H 2 1.108393 0.327489 0.479658 11.00000 -1.50000 AFIX 0 C110 1 0.827993 0.502100 0.267767 11.00000 0.05376 0.04046 = 0.04960 0.01004 0.02948 0.00966 AFIX 23 H11A 2 0.843917 0.545562 0.288426 11.00000 -1.20000 H11B 2 0.805280 0.517018 0.230027 11.00000 -1.20000 AFIX 0 C111 1 0.781791 0.503170 0.335818 11.00000 0.05276 0.04767 = 0.06201 0.00838 0.03345 0.02372 C112 1 0.753982 0.395761 0.329537 11.00000 0.04217 0.05832 = 0.06657 0.00471 0.03324 -0.00093 C113 1 0.731355 0.331607 0.335813 11.00000 0.05268 0.08864 = 0.08059 -0.00889 0.03982 -0.02369 AFIX 43 H113 2 0.712402 0.329407 0.358891 11.00000 -1.20000 AFIX 0 C114 1 0.737722 0.271049 0.306865 11.00000 0.05871 0.06665 = 0.08272 0.00575 0.02211 -0.02795 AFIX 43 H114 2 0.722067 0.227907 0.310153 11.00000 -1.20000 AFIX 0 C115 1 0.766678 0.271861 0.272861 11.00000 0.06751 0.05053 = 0.07202 -0.00446 0.02916 -0.01094 AFIX 43 H115 2 0.771304 0.229502 0.255152 11.00000 -1.20000 AFIX 0 C116 1 0.788190 0.335615 0.265846 11.00000 0.06820 0.04749 = 0.06592 -0.00986 0.03243 -0.00967 AFIX 43 H116 2 0.807180 0.337425 0.242795 11.00000 -1.20000 AFIX 0 C117 1 0.781360 0.397210 0.293402 11.00000 0.03742 0.04932 = 0.03775 0.00123 0.01590 0.00325 C118 1 0.770893 0.601558 0.405861 11.00000 0.10988 0.09221 = 0.08193 -0.00843 0.04525 0.03330 AFIX 137 H11C 2 0.738201 0.579829 0.393995 11.00000 -1.50000 H11D 2 0.768710 0.651927 0.414768 11.00000 -1.50000 H11E 2 0.793182 0.576829 0.439243 11.00000 -1.50000 AFIX 0 C126 1 0.966650 0.029685 0.199111 11.00000 0.03545 0.03502 = 0.02986 -0.00665 0.01263 -0.00563 O1 3 0.300480 0.224553 0.274866 11.00000 0.08596 0.08696 = 0.12720 0.02937 0.05737 0.03783 O2 3 0.293416 0.011683 0.325351 11.00000 0.05249 0.09106 = 0.09565 -0.01221 0.04319 -0.02058 O3 3 0.384595 0.163807 0.436693 11.00000 0.08146 0.10281 = 0.05187 -0.02219 0.03040 0.00447 O4 3 0.599458 0.016276 0.050505 11.00000 0.12611 0.10681 = 0.06474 -0.01721 0.06610 0.00271 O5 3 0.684420 0.168287 0.166768 11.00000 0.03560 0.14621 = 0.10801 0.01430 0.03488 -0.01977 O6 3 0.553584 0.225019 0.038880 11.00000 0.10072 0.11847 = 0.06794 0.06154 0.04500 0.01918 O7 3 0.380821 0.070463 0.242713 11.00000 0.03928 0.05662 = 0.04542 -0.01065 0.02817 -0.01228 O8 3 0.441275 0.167341 0.319883 11.00000 0.04296 0.04321 = 0.05089 -0.01367 0.02947 -0.00997 O9 3 0.503999 0.079235 0.122932 11.00000 0.03377 0.05809 = 0.03541 0.00259 0.01946 -0.00567 O10 3 0.563664 0.177712 0.199016 11.00000 0.04081 0.05668 = 0.04938 0.00508 0.02576 -0.00886 O11 3 1.038148 0.028316 0.376069 11.00000 0.04632 0.03718 = 0.03363 0.00369 0.01634 -0.00094 O12 3 1.108737 0.118328 0.364388 11.00000 0.04012 0.04501 = 0.04362 -0.00337 0.01789 -0.00385 O13 3 0.940634 0.025677 0.145962 11.00000 0.04565 0.04578 = 0.02984 -0.00413 0.00923 -0.01929 O14 3 1.012051 0.112425 0.133131 11.00000 0.04828 0.04401 = 0.02842 0.00306 0.01300 -0.00370 O15 3 0.835644 0.042335 -0.006102 11.00000 0.07322 0.12055 = 0.08346 -0.02303 -0.01085 -0.00565 O16 3 0.951895 0.172408 -0.024759 11.00000 0.16815 0.05497 = 0.04263 0.00778 0.05520 0.01182 O17 3 0.965766 -0.048315 0.013505 11.00000 0.09766 0.04641 = 0.05451 -0.01657 0.03618 -0.00676 O18 3 1.169533 -0.022724 0.486927 11.00000 0.09250 0.06834 = 0.07618 0.00744 0.00696 0.04811 O19 3 1.170053 0.197976 0.518976 11.00000 0.09751 0.08253 = 0.05764 -0.00716 -0.01959 -0.02079 O20 3 1.058213 0.063437 0.536808 11.00000 0.09823 0.11366 = 0.05991 0.02404 0.04692 0.02913 S1 4 0.382361 -0.087641 0.288115 11.00000 0.04182 0.04973 = 0.05964 -0.00746 0.01072 -0.00294 S2 4 0.548158 -0.081132 0.131838 11.00000 0.06399 0.06118 = 0.03536 -0.00255 0.00950 -0.00311 S3 4 0.684819 -0.135839 0.478640 11.00000 0.11814 0.07242 = 0.08270 -0.00342 0.03226 -0.01559 S4 4 0.977798 0.278662 0.096049 11.00000 0.04991 0.04689 = 0.05360 -0.00293 0.03452 -0.00385 S5 4 1.096386 0.283952 0.390438 11.00000 0.03891 0.04141 = 0.06956 0.00126 0.01405 -0.00229 S6 4 0.793723 0.594463 0.350682 11.00000 0.10017 0.05451 = 0.11157 -0.01060 0.07281 0.00448 RE1 5 0.379552 0.105975 0.321793 11.00000 0.03287 0.04435 = 0.04068 -0.00114 0.02077 0.00005 RE2 5 0.577534 0.114238 0.136073 11.00000 0.03528 0.05513 = 0.03964 0.00768 0.02144 -0.00274 RE3 5 0.941740 0.083131 0.073033 11.00000 0.05041 0.03784 = 0.02982 -0.00402 0.01612 0.00036 RE4 5 1.091705 0.095560 0.437348 11.00000 0.04307 0.03866 = 0.03069 0.00165 0.00686 0.00642 N1 6 0.436764 0.020512 0.356795 11.00000 0.03277 0.03981 = 0.04003 0.00289 0.00728 -0.00028 N2 6 0.477539 -0.085088 0.371157 11.00000 0.04486 0.03277 = 0.03660 -0.00223 0.00786 -0.00567 N3 6 0.598118 0.029928 0.203088 11.00000 0.03768 0.04809 = 0.03604 0.00244 0.01943 -0.00712 N4 6 0.607283 -0.078944 0.246657 11.00000 0.04462 0.04393 = 0.03978 -0.00497 0.01397 -0.00721 N5 6 0.687824 -0.279843 0.485537 11.00000 0.04616 0.07635 = 0.04067 0.01296 -0.00158 -0.00040 N6 6 0.744672 -0.225306 0.560377 11.00000 0.07889 0.14315 = 0.06017 -0.03974 0.01635 -0.06018 N7 6 0.914952 0.175346 0.110321 11.00000 0.04306 0.03644 = 0.03229 -0.00539 0.01610 0.00253 N8 6 0.897609 0.289445 0.130091 11.00000 0.03359 0.04172 = 0.03417 -0.00984 0.02128 -0.01364 N9 6 1.033744 0.179882 0.401240 11.00000 0.03677 0.02742 = 0.03763 -0.00147 0.01119 0.00330 N10 6 0.994800 0.285610 0.368645 11.00000 0.03417 0.03641 = 0.03491 -0.00054 0.00454 0.00147 N11 6 0.798954 0.468317 0.297910 11.00000 0.03153 0.04062 = 0.04900 0.00142 0.01586 0.00073 N12 6 0.754067 0.461580 0.355143 11.00000 0.05745 0.06212 = 0.06156 -0.00367 0.03922 0.00562 C5A 1 0.755812 0.881168 0.273985 11.00000 0.09860 C6A 1 0.729699 0.904170 0.218261 11.00000 0.13522 C3A 1 0.775198 1.010058 0.304778 11.00000 0.13582 C4A 1 0.777709 0.935447 0.315747 11.00000 0.13664 C1A 1 0.723628 0.981196 0.199048 11.00000 0.14516 C2A 1 0.749608 1.027051 0.245762 11.00000 0.16088 C7A 1 0.803449 0.918890 0.374443 11.00000 0.16745 HKLF 4 REM RK5-94- in P2(1)/c REM R1 = 0.0671 for 15657 Fo > 4sig(Fo) and 0.1214 for all 25113 data REM 1494 parameters refined using 12 restraints END WGHT 0.0733 44.4392 REM Highest difference peak 2.992, deepest hole -1.089, 1-sigma level 0.182 Q1 1 0.7490 0.1664 0.4998 11.00000 0.05 2.99 Q2 1 0.2611 -0.2052 0.0008 11.00000 0.05 2.44 Q3 1 0.7976 0.2607 0.4776 11.00000 0.05 1.96 Q4 1 1.2062 -0.1966 0.5206 11.00000 0.05 1.87 Q5 1 0.7624 0.2258 0.4898 11.00000 0.05 1.65 Q6 1 0.7180 0.1909 0.5027 11.00000 0.05 1.59 Q7 1 0.2986 -0.2136 -0.0151 11.00000 0.05 1.55 Q8 1 0.6939 0.1708 0.5172 11.00000 0.05 1.55 Q9 1 0.6732 0.2113 0.5208 11.00000 0.05 1.38 Q10 1 0.7067 -0.3918 0.5431 11.00000 0.05 1.31 Q11 1 1.0944 0.1435 0.4366 11.00000 0.05 1.18 Q12 1 0.6833 -0.0596 0.4921 11.00000 0.05 1.16 Q13 1 0.7375 -0.3819 0.5325 11.00000 0.05 1.13 Q14 1 1.0903 0.0364 0.4367 11.00000 0.05 0.96 Q15 1 0.9430 0.1379 0.0700 11.00000 0.05 0.95 Q16 1 0.5812 0.1769 0.1376 11.00000 0.05 0.95 Q17 1 0.9430 0.0268 0.0774 11.00000 0.05 0.91 Q18 1 0.7435 -0.1226 0.5799 11.00000 0.05 0.91 Q19 1 0.7176 -0.4260 0.5057 11.00000 0.05 0.85 Q20 1 0.9097 0.0828 0.0424 11.00000 0.05 0.84 ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.720 0.210 0.486 265 87 ' ' 2 0.893 0.113 0.261 27 7 ' ' 3 0.481 0.080 0.001 11 2 ' ' 4 0.720 0.290 -0.014 264 88 ' ' 5 0.072 0.261 0.048 32 9 ' ' 6 0.072 0.239 0.548 32 9 ' ' 7 0.893 0.387 0.761 27 8 ' ' 8 0.481 0.420 0.501 11 4 ' ' 9 0.280 0.710 0.014 265 87 ' ' 10 0.107 0.613 0.239 27 7 ' ' 11 0.519 0.580 0.499 11 3 ' ' 12 0.279 0.790 0.514 264 89 ' ' 13 0.928 0.739 0.952 32 10 ' ' 14 0.928 0.761 0.452 32 10 ' ' 15 0.107 0.887 0.739 27 7 ' ' 16 0.519 0.920 -0.001 11 4 ' ' _platon_squeeze_details ; The solvent accessible cavity is that of the solvent toluene molecules (estimated volume 258 \%A^3^) for which no reasonable model could be developed. Therefore, the observed structure amplitudes were modified by PLATON (Spek, 1990) to eliminate the diffuse electron density in the cavity. One of the two solvent molecules appeared in the final difference Fourier map and has been modeled using SHELXL restrains. Two solvent molecules are included in the scheme, formula, FW, density, etc., and one solvent molecule is included in the refined model. ; _database_code_depnum_ccdc_archive 'CCDC 935808' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H40 N10 O6 Re2 S3' _chemical_formula_sum 'C52 H40 N10 O6 Re2 S3' _chemical_formula_weight 1369.52 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1042(4) _cell_length_b 13.4573(4) _cell_length_c 14.6018(5) _cell_angle_alpha 91.058(3) _cell_angle_beta 93.181(3) _cell_angle_gamma 101.095(3) _cell_volume 2521.85(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8854 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 28.00 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 4.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.26 _exptl_absorpt_correction_T_max 0.30 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur Sapphire3 CCD Diffractometer' _diffrn_measurement_method 'w scan' _diffrn_detector_area_resol_mean 15.9853 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39562 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_unetI/netI 0.0351 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 28.00 _reflns_number_total 12108 _reflns_number_gt 10181 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_data_reduction 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+1.4340P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12108 _refine_ls_number_parameters 664 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.496123(9) 0.153558(9) 0.138610(10) 0.03070(4) Uani 1 1 d . . . Re2 Re 0.238228(9) 0.366854(9) -0.078369(9) 0.02770(4) Uani 1 1 d . . . S1 S 0.48181(7) 0.29490(7) 0.35216(7) 0.0418(2) Uani 1 1 d . . . S2 S 0.21482(6) 0.55345(6) 0.10348(6) 0.03309(18) Uani 1 1 d . . . S3 S -0.24945(9) 0.28724(9) 0.67927(8) 0.0611(3) Uani 1 1 d . . . O1 O 0.2338(3) 0.5848(2) -0.1324(2) 0.0675(9) Uani 1 1 d . . . O2 O 0.0664(2) 0.3061(3) -0.2295(2) 0.0750(10) Uani 1 1 d . . . O3 O 0.3950(3) 0.3491(3) -0.2216(3) 0.0894(12) Uani 1 1 d . . . O4 O 0.6911(2) 0.2166(2) 0.2669(2) 0.0623(8) Uani 1 1 d . . . O5 O 0.5229(2) -0.0658(2) 0.1586(2) 0.0635(9) Uani 1 1 d . . . O6 O 0.6491(2) 0.1905(2) -0.0128(2) 0.0638(8) Uani 1 1 d . . . N1 N 0.2529(2) 0.21109(18) -0.04313(19) 0.0300(6) Uani 1 1 d . . . N2 N 0.3575(2) 0.12624(19) 0.0391(2) 0.0317(6) Uani 1 1 d . . . N3 N 0.35970(19) 0.39403(18) 0.03861(19) 0.0297(6) Uani 1 1 d . . . N4 N 0.45906(19) 0.30826(19) 0.12631(19) 0.0301(6) Uani 1 1 d . . . N5 N 0.13349(19) 0.36304(18) 0.03466(19) 0.0278(6) Uani 1 1 d . . . N6 N 0.06384(19) 0.40240(19) 0.16354(18) 0.0287(6) Uani 1 1 d . . . N7 N 0.3781(2) 0.1363(2) 0.2428(2) 0.0318(6) Uani 1 1 d . . . N8 N 0.2855(2) 0.1810(2) 0.35468(19) 0.0329(6) Uani 1 1 d . . . N9 N -0.1691(2) 0.2130(2) 0.5328(2) 0.0418(7) Uani 1 1 d . . . N10 N -0.3205(3) 0.1181(3) 0.5723(3) 0.0553(9) Uani 1 1 d . . . C1 C 0.2375(3) 0.5043(3) -0.1081(2) 0.0400(8) Uani 1 1 d . . . C2 C 0.1311(3) 0.3283(3) -0.1712(3) 0.0430(9) Uani 1 1 d . . . C3 C 0.3362(3) 0.3589(3) -0.1678(3) 0.0461(9) Uani 1 1 d . . . C4 C 0.6156(3) 0.1931(3) 0.2204(3) 0.0412(9) Uani 1 1 d . . . C5 C 0.5118(3) 0.0161(3) 0.1488(3) 0.0418(9) Uani 1 1 d . . . C6 C 0.5908(3) 0.1758(3) 0.0434(3) 0.0420(9) Uani 1 1 d . . . C7 C 0.2338(3) 0.1120(2) -0.0745(3) 0.0360(8) Uani 1 1 d . . . H7 H 0.1858 0.0844 -0.1219 0.043 Uiso 1 1 calc R . . C8 C 0.2969(2) 0.0607(2) -0.0248(2) 0.0356(8) Uani 1 1 d . . . H8 H 0.2987 -0.0077 -0.0327 0.043 Uiso 1 1 calc R . . C9 C 0.3267(2) 0.2130(2) 0.0235(2) 0.0302(7) Uani 1 1 d . . . C10 C 0.3792(2) 0.3053(2) 0.0654(2) 0.0301(7) Uani 1 1 d . . . C11 C 0.4340(2) 0.4628(2) 0.0897(2) 0.0336(8) Uani 1 1 d . . . H11 H 0.4418 0.5329 0.0885 0.040 Uiso 1 1 calc R . . C12 C 0.4945(2) 0.4106(2) 0.1425(3) 0.0350(8) Uani 1 1 d . . . H12 H 0.5503 0.4396 0.1827 0.042 Uiso 1 1 calc R . . C13 C 0.1336(2) 0.4336(2) 0.0993(2) 0.0261(6) Uani 1 1 d . . . C14 C 0.0569(2) 0.2811(2) 0.0574(2) 0.0278(7) Uani 1 1 d . . . C15 C 0.0192(2) 0.1888(2) 0.0110(3) 0.0362(8) Uani 1 1 d . . . H15 H 0.0483 0.1710 -0.0421 0.043 Uiso 1 1 calc R . . C16 C -0.0627(3) 0.1255(3) 0.0468(3) 0.0427(9) Uani 1 1 d . . . H16 H -0.0897 0.0635 0.0171 0.051 Uiso 1 1 calc R . . C17 C -0.1067(3) 0.1512(3) 0.1264(3) 0.0449(9) Uani 1 1 d . . . H17 H -0.1622 0.1060 0.1483 0.054 Uiso 1 1 calc R . . C18 C -0.0706(3) 0.2412(3) 0.1733(2) 0.0379(8) Uani 1 1 d . . . H18 H -0.0999 0.2584 0.2265 0.046 Uiso 1 1 calc R . . C19 C 0.0123(2) 0.3052(2) 0.1368(2) 0.0281(7) Uani 1 1 d . . . C20 C 0.0529(3) 0.4547(2) 0.2502(2) 0.0333(7) Uani 1 1 d . . . H20A H -0.0147 0.4743 0.2485 0.040 Uiso 1 1 calc R . . H20B H 0.1058 0.5161 0.2569 0.040 Uiso 1 1 calc R . . C21 C 0.0632(2) 0.3888(2) 0.3338(2) 0.0297(7) Uani 1 1 d . . . C22 C 0.1542(2) 0.3491(2) 0.3476(2) 0.0302(7) Uani 1 1 d . . . C23 C 0.2446(2) 0.3804(3) 0.2880(2) 0.0377(8) Uani 1 1 d . . . H23A H 0.3087 0.3811 0.3234 0.057 Uiso 1 1 calc R . . H23B H 0.2438 0.4469 0.2657 0.057 Uiso 1 1 calc R . . H23C H 0.2389 0.3332 0.2371 0.057 Uiso 1 1 calc R . . C24 C 0.1610(2) 0.2822(2) 0.4190(2) 0.0332(7) Uani 1 1 d . . . C25 C 0.2589(3) 0.2378(3) 0.4339(2) 0.0362(8) Uani 1 1 d . . . H25A H 0.3171 0.2927 0.4505 0.043 Uiso 1 1 calc R . . H25B H 0.2501 0.1931 0.4855 0.043 Uiso 1 1 calc R . . C26 C 0.3775(2) 0.1994(2) 0.3130(2) 0.0317(7) Uani 1 1 d . . . C27 C 0.2823(2) 0.0693(2) 0.2413(2) 0.0323(7) Uani 1 1 d . . . C28 C 0.2444(3) -0.0168(3) 0.1869(3) 0.0400(8) Uani 1 1 d . . . H28 H 0.2833 -0.0371 0.1412 0.048 Uiso 1 1 calc R . . C29 C 0.1471(3) -0.0711(3) 0.2032(3) 0.0462(9) Uani 1 1 d . . . H29 H 0.1203 -0.1295 0.1680 0.055 Uiso 1 1 calc R . . C30 C 0.0884(3) -0.0409(3) 0.2704(3) 0.0493(10) Uani 1 1 d . . . H30 H 0.0223 -0.0786 0.2782 0.059 Uiso 1 1 calc R . . C31 C 0.1252(3) 0.0435(3) 0.3262(3) 0.0432(9) Uani 1 1 d . . . H31 H 0.0860 0.0633 0.3719 0.052 Uiso 1 1 calc R . . C32 C 0.2241(2) 0.0975(2) 0.3104(2) 0.0330(7) Uani 1 1 d . . . C33 C -0.0155(3) 0.3704(3) 0.3961(2) 0.0347(8) Uani 1 1 d . . . C34 C -0.1136(3) 0.4141(3) 0.3825(3) 0.0535(11) Uani 1 1 d . . . H34A H -0.1347 0.4116 0.3183 0.080 Uiso 1 1 calc R . . H34B H -0.0999 0.4832 0.4050 0.080 Uiso 1 1 calc R . . H34C H -0.1682 0.3752 0.4155 0.080 Uiso 1 1 calc R . . C35 C -0.0030(3) 0.3098(3) 0.4707(2) 0.0365(8) Uani 1 1 d . . . C36 C 0.0823(3) 0.2616(3) 0.4801(2) 0.0379(8) Uani 1 1 d . . . C37 C 0.0867(3) 0.1869(3) 0.5565(3) 0.0611(12) Uani 1 1 d . . . H37A H 0.1198 0.1335 0.5358 0.092 Uiso 1 1 calc R . . H37B H 0.0173 0.1587 0.5726 0.092 Uiso 1 1 calc R . . H37C H 0.1259 0.2213 0.6092 0.092 Uiso 1 1 calc R . . C38 C -0.0804(3) 0.2983(3) 0.5444(3) 0.0478(10) Uani 1 1 d . . . H38A H -0.0432 0.2917 0.6026 0.057 Uiso 1 1 calc R . . H38B H -0.1075 0.3603 0.5484 0.057 Uiso 1 1 calc R . . C39 C -0.2491(3) 0.1992(3) 0.5917(3) 0.0461(9) Uani 1 1 d . . . C40 C -0.1917(3) 0.1320(3) 0.4697(3) 0.0457(9) Uani 1 1 d . . . C41 C -0.1415(3) 0.1042(3) 0.3937(3) 0.0467(10) Uani 1 1 d . . . H41 H -0.0776 0.1409 0.3778 0.056 Uiso 1 1 calc R . . C42 C -0.1927(4) 0.0188(3) 0.3433(3) 0.0632(12) Uani 1 1 d . . . H42 H -0.1629 -0.0021 0.2918 0.076 Uiso 1 1 calc R . . C43 C -0.2881(4) -0.0364(4) 0.3687(4) 0.0747(15) Uani 1 1 d . . . H43 H -0.3204 -0.0931 0.3334 0.090 Uiso 1 1 calc R . . C44 C -0.3347(4) -0.0091(3) 0.4437(4) 0.0716(14) Uani 1 1 d . . . H44 H -0.3984 -0.0464 0.4595 0.086 Uiso 1 1 calc R . . C45 C -0.2858(3) 0.0750(3) 0.4959(3) 0.0505(10) Uani 1 1 d . . . C46 C 0.5378(3) 0.2272(3) 0.4410(3) 0.0672(13) Uani 1 1 d . . . H46A H 0.6068 0.2631 0.4592 0.101 Uiso 1 1 calc R . . H46B H 0.5411 0.1606 0.4182 0.101 Uiso 1 1 calc R . . H46C H 0.4954 0.2219 0.4929 0.101 Uiso 1 1 calc R . . C47 C 0.1214(3) 0.6310(3) 0.0732(3) 0.0575(12) Uani 1 1 d . . . H47A H 0.1573 0.6975 0.0591 0.086 Uiso 1 1 calc R . . H47B H 0.0786 0.6356 0.1237 0.086 Uiso 1 1 calc R . . H47C H 0.0785 0.6012 0.0206 0.086 Uiso 1 1 calc R . . C48 C -0.3717(4) 0.2319(4) 0.7273(4) 0.0807(16) Uani 1 1 d . . . H48A H -0.3973 0.2834 0.7603 0.121 Uiso 1 1 calc R . . H48B H -0.3606 0.1795 0.7682 0.121 Uiso 1 1 calc R . . H48C H -0.4217 0.2036 0.6786 0.121 Uiso 1 1 calc R . . C49 C 0.4159(7) 0.4751(6) 0.5462(6) 0.118(3) Uani 1 1 d D . . C50 C 0.3250(10) 0.4563(11) 0.5885(11) 0.276(8) Uani 1 1 d D . . C51 C 0.5063(8) 0.4467(5) 0.5790(5) 0.102(2) Uani 1 1 d D . . C52 C 0.4048(8) 0.5299(6) 0.4648(6) 0.122(3) Uani 1 1 d D . . 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 Re1 0.02321(7) 0.02918(7) 0.04113(9) 0.00305(6) 0.00465(6) 0.00765(5) Re2 0.02794(7) 0.02877(7) 0.02550(7) 0.00297(5) 0.00279(5) 0.00276(5) S1 0.0333(4) 0.0426(5) 0.0473(6) -0.0022(4) -0.0063(4) 0.0049(4) S2 0.0331(4) 0.0250(4) 0.0403(5) 0.0024(3) 0.0024(4) 0.0031(3) S3 0.0590(7) 0.0740(7) 0.0524(7) 0.0023(6) 0.0249(5) 0.0117(6) O1 0.094(2) 0.0452(17) 0.069(2) 0.0255(15) 0.0118(18) 0.0238(16) O2 0.068(2) 0.110(3) 0.0417(19) -0.0131(18) -0.0219(17) 0.0112(19) O3 0.094(3) 0.090(3) 0.083(3) -0.010(2) 0.062(2) 0.001(2) O4 0.0326(14) 0.081(2) 0.071(2) 0.0045(17) -0.0110(15) 0.0096(14) O5 0.0659(19) 0.0393(16) 0.093(3) 0.0161(15) 0.0248(17) 0.0221(14) O6 0.0558(18) 0.070(2) 0.067(2) 0.0084(16) 0.0312(16) 0.0073(15) N1 0.0314(14) 0.0238(13) 0.0339(16) -0.0023(11) 0.0006(12) 0.0041(11) N2 0.0268(13) 0.0275(14) 0.0408(17) -0.0027(12) 0.0020(12) 0.0053(11) N3 0.0275(13) 0.0245(13) 0.0359(16) 0.0019(11) -0.0012(12) 0.0026(11) N4 0.0247(13) 0.0276(14) 0.0378(17) 0.0009(12) 0.0002(12) 0.0048(11) N5 0.0247(13) 0.0263(13) 0.0320(16) 0.0035(11) 0.0023(11) 0.0035(10) N6 0.0282(13) 0.0297(14) 0.0289(15) 0.0001(11) 0.0019(11) 0.0071(11) N7 0.0262(13) 0.0308(14) 0.0387(17) 0.0008(12) 0.0025(12) 0.0061(11) N8 0.0331(14) 0.0345(15) 0.0322(16) 0.0020(12) 0.0043(12) 0.0086(12) N9 0.0401(16) 0.0506(18) 0.0363(18) 0.0070(14) 0.0117(14) 0.0093(14) N10 0.050(2) 0.055(2) 0.060(2) 0.0169(18) 0.0075(18) 0.0065(17) C1 0.044(2) 0.046(2) 0.031(2) 0.0068(16) 0.0036(16) 0.0106(17) C2 0.045(2) 0.050(2) 0.034(2) 0.0001(17) 0.0026(18) 0.0085(17) C3 0.049(2) 0.041(2) 0.045(2) 0.0011(17) 0.0142(19) -0.0019(17) C4 0.0316(18) 0.042(2) 0.053(2) 0.0079(17) 0.0065(17) 0.0109(16) C5 0.0309(17) 0.042(2) 0.055(3) 0.0077(18) 0.0139(17) 0.0109(16) C6 0.0356(19) 0.039(2) 0.053(3) 0.0038(17) 0.0091(18) 0.0078(16) C7 0.0340(17) 0.0296(17) 0.041(2) -0.0075(15) 0.0006(16) -0.0012(14) C8 0.0337(17) 0.0278(17) 0.044(2) -0.0071(15) 0.0044(16) 0.0026(14) C9 0.0258(15) 0.0261(16) 0.038(2) 0.0016(14) 0.0031(14) 0.0029(13) C10 0.0246(15) 0.0275(16) 0.037(2) -0.0006(14) 0.0012(14) 0.0023(13) C11 0.0302(16) 0.0241(16) 0.043(2) -0.0016(14) 0.0005(15) -0.0021(13) C12 0.0270(16) 0.0308(17) 0.045(2) -0.0004(15) -0.0003(15) 0.0004(13) C13 0.0249(15) 0.0274(15) 0.0267(17) 0.0039(13) -0.0007(13) 0.0069(12) C14 0.0221(14) 0.0307(16) 0.0298(18) 0.0048(13) -0.0011(13) 0.0038(12) C15 0.0333(17) 0.0339(18) 0.039(2) -0.0034(15) 0.0030(15) 0.0013(14) C16 0.041(2) 0.0336(19) 0.048(2) -0.0030(16) 0.0017(18) -0.0066(15) C17 0.0369(19) 0.042(2) 0.049(2) 0.0054(17) 0.0095(17) -0.0113(16) C18 0.0329(17) 0.045(2) 0.034(2) 0.0038(16) 0.0086(15) 0.0005(15) C19 0.0237(15) 0.0298(16) 0.0298(18) 0.0035(13) -0.0029(13) 0.0037(12) C20 0.0347(17) 0.0369(18) 0.0307(19) -0.0010(14) 0.0053(15) 0.0120(14) C21 0.0318(16) 0.0315(17) 0.0249(17) -0.0045(13) 0.0006(14) 0.0051(13) C22 0.0299(16) 0.0363(17) 0.0241(17) -0.0022(13) 0.0031(13) 0.0056(14) C23 0.0297(17) 0.051(2) 0.035(2) 0.0112(16) 0.0045(15) 0.0113(15) C24 0.0338(17) 0.0407(19) 0.0257(18) -0.0016(14) 0.0017(14) 0.0088(15) C25 0.0402(19) 0.045(2) 0.0261(18) -0.0014(15) 0.0016(15) 0.0145(16) C26 0.0295(16) 0.0321(17) 0.0344(19) 0.0030(14) 0.0023(14) 0.0080(14) C27 0.0301(16) 0.0311(17) 0.036(2) 0.0053(14) 0.0012(15) 0.0057(13) C28 0.041(2) 0.0344(19) 0.042(2) -0.0011(16) 0.0063(17) 0.0019(15) C29 0.048(2) 0.040(2) 0.043(2) -0.0007(17) 0.0013(18) -0.0080(17) C30 0.0358(19) 0.053(2) 0.053(3) 0.0076(19) 0.0092(18) -0.0096(17) C31 0.0365(19) 0.048(2) 0.043(2) 0.0061(17) 0.0093(17) 0.0013(16) C32 0.0293(16) 0.0359(18) 0.034(2) 0.0059(14) 0.0026(14) 0.0070(14) C33 0.0319(17) 0.0403(19) 0.0321(19) -0.0062(15) 0.0056(15) 0.0071(14) C34 0.041(2) 0.068(3) 0.057(3) 0.006(2) 0.019(2) 0.023(2) C35 0.0374(18) 0.046(2) 0.0247(18) -0.0059(15) 0.0067(15) 0.0047(16) C36 0.0414(19) 0.049(2) 0.0233(18) 0.0032(15) 0.0056(15) 0.0086(16) C37 0.060(3) 0.088(3) 0.042(3) 0.028(2) 0.015(2) 0.025(2) C38 0.044(2) 0.069(3) 0.031(2) -0.0029(18) 0.0136(17) 0.0091(19) C39 0.041(2) 0.061(2) 0.040(2) 0.0151(19) 0.0126(17) 0.0152(19) C40 0.048(2) 0.048(2) 0.043(2) 0.0082(18) -0.0013(18) 0.0148(18) C41 0.057(2) 0.048(2) 0.037(2) 0.0012(18) 0.0005(19) 0.0161(19) C42 0.083(3) 0.058(3) 0.053(3) -0.001(2) -0.003(3) 0.026(3) C43 0.093(4) 0.050(3) 0.077(4) -0.004(3) -0.016(3) 0.011(3) C44 0.074(3) 0.049(3) 0.088(4) 0.012(3) 0.000(3) 0.004(2) C45 0.051(2) 0.048(2) 0.054(3) 0.011(2) -0.002(2) 0.0130(19) C46 0.058(3) 0.074(3) 0.066(3) 0.011(2) -0.022(2) 0.012(2) C47 0.055(2) 0.039(2) 0.083(3) 0.017(2) 0.003(2) 0.0181(19) C48 0.065(3) 0.109(4) 0.074(4) 0.019(3) 0.041(3) 0.020(3) C49 0.137(7) 0.080(5) 0.127(8) -0.055(5) 0.005(6) 0.002(5) C50 0.221(14) 0.284(16) 0.32(2) -0.144(15) 0.001(13) 0.071(12) C51 0.135(6) 0.074(4) 0.096(6) -0.015(4) -0.021(5) 0.025(4) C52 0.199(10) 0.073(4) 0.089(6) -0.023(4) -0.021(6) 0.028(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C4 1.900(4) . ? Re1 C6 1.905(4) . ? Re1 C5 1.907(4) . ? Re1 N7 2.213(3) . ? Re1 N2 2.231(3) . ? Re1 N4 2.235(2) . ? Re2 C2 1.887(4) . ? Re2 C3 1.897(4) . ? Re2 C1 1.910(4) . ? Re2 N5 2.200(3) . ? Re2 N1 2.209(2) . ? Re2 N3 2.244(3) . ? S1 C26 1.748(3) . ? S1 C46 1.801(4) . ? S2 C13 1.751(3) . ? S2 C47 1.798(4) . ? S3 C39 1.728(4) . ? S3 C48 1.815(4) . ? O1 C1 1.155(4) . ? O2 C2 1.160(4) . ? O3 C3 1.153(5) . ? O4 C4 1.156(4) . ? O5 C5 1.150(4) . ? O6 C6 1.145(4) . ? N1 C9 1.329(4) . ? N1 C7 1.374(4) . ? N2 C9 1.326(4) . ? N2 C8 1.378(4) . ? N3 C10 1.329(4) . ? N3 C11 1.381(4) . ? N4 C10 1.329(4) . ? N4 C12 1.378(4) . ? N5 C13 1.326(4) . ? N5 C14 1.399(4) . ? N6 C13 1.362(4) . ? N6 C19 1.389(4) . ? N6 C20 1.464(4) . ? N7 C26 1.320(4) . ? N7 C27 1.397(4) . ? N8 C26 1.363(4) . ? N8 C32 1.377(4) . ? N8 C25 1.470(4) . ? N9 C39 1.379(5) . ? N9 C40 1.391(5) . ? N9 C38 1.468(5) . ? N10 C39 1.309(5) . ? N10 C45 1.386(5) . ? C7 C8 1.363(5) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.410(4) . ? C11 C12 1.372(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C14 C19 1.387(5) . ? C14 C15 1.393(4) . ? C15 C16 1.371(5) . ? C15 H15 0.9300 . ? C16 C17 1.392(5) . ? C16 H16 0.9300 . ? C17 C18 1.368(5) . ? C17 H17 0.9300 . ? C18 C19 1.389(4) . ? C18 H18 0.9300 . ? C20 C21 1.538(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C33 1.402(4) . ? C21 C22 1.404(4) . ? C22 C24 1.400(4) . ? C22 C23 1.507(4) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C36 1.393(5) . ? C24 C25 1.522(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C27 C28 1.385(5) . ? C27 C32 1.387(5) . ? C28 C29 1.377(5) . ? C28 H28 0.9300 . ? C29 C30 1.383(5) . ? C29 H29 0.9300 . ? C30 C31 1.377(5) . ? C30 H30 0.9300 . ? C31 C32 1.393(4) . ? C31 H31 0.9300 . ? C33 C35 1.393(5) . ? C33 C34 1.518(5) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.398(5) . ? C35 C38 1.509(5) . ? C36 C37 1.521(5) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C40 C45 1.398(5) . ? C40 C41 1.402(5) . ? C41 C42 1.388(5) . ? C41 H41 0.9300 . ? C42 C43 1.398(7) . ? C42 H42 0.9300 . ? C43 C44 1.362(7) . ? C43 H43 0.9300 . ? C44 C45 1.381(6) . ? C44 H44 0.9300 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.355(12) . ? C49 C51 1.377(9) . ? C49 C52 1.426(9) . ? C51 C52 1.347(11) 2_666 ? C52 C51 1.347(11) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Re1 C6 85.72(16) . . ? C4 Re1 C5 88.98(15) . . ? C6 Re1 C5 91.88(15) . . ? C4 Re1 N7 97.38(13) . . ? C6 Re1 N7 174.99(12) . . ? C5 Re1 N7 92.11(13) . . ? C4 Re1 N2 173.32(12) . . ? C6 Re1 N2 92.61(14) . . ? C5 Re1 N2 97.55(13) . . ? N7 Re1 N2 83.86(10) . . ? C4 Re1 N4 95.96(12) . . ? C6 Re1 N4 92.28(13) . . ? C5 Re1 N4 173.76(12) . . ? N7 Re1 N4 83.50(10) . . ? N2 Re1 N4 77.62(9) . . ? C2 Re2 C3 88.36(17) . . ? C2 Re2 C1 87.62(15) . . ? C3 Re2 C1 90.43(16) . . ? C2 Re2 N5 95.47(13) . . ? C3 Re2 N5 173.10(14) . . ? C1 Re2 N5 95.46(13) . . ? C2 Re2 N1 95.79(13) . . ? C3 Re2 N1 86.57(14) . . ? C1 Re2 N1 175.39(12) . . ? N5 Re2 N1 87.33(10) . . ? C2 Re2 N3 173.12(13) . . ? C3 Re2 N3 93.73(14) . . ? C1 Re2 N3 98.91(12) . . ? N5 Re2 N3 81.81(10) . . ? N1 Re2 N3 77.81(9) . . ? C26 S1 C46 98.96(18) . . ? C13 S2 C47 100.29(16) . . ? C39 S3 C48 99.2(2) . . ? C9 N1 C7 103.0(3) . . ? C9 N1 Re2 110.36(19) . . ? C7 N1 Re2 144.4(2) . . ? C9 N2 C8 102.7(3) . . ? C9 N2 Re1 109.5(2) . . ? C8 N2 Re1 146.8(2) . . ? C10 N3 C11 102.8(3) . . ? C10 N3 Re2 108.85(19) . . ? C11 N3 Re2 147.6(2) . . ? C10 N4 C12 102.9(3) . . ? C10 N4 Re1 109.7(2) . . ? C12 N4 Re1 145.9(2) . . ? C13 N5 C14 105.2(3) . . ? C13 N5 Re2 128.1(2) . . ? C14 N5 Re2 126.5(2) . . ? C13 N6 C19 106.9(3) . . ? C13 N6 C20 127.2(3) . . ? C19 N6 C20 125.6(3) . . ? C26 N7 C27 105.3(3) . . ? C26 N7 Re1 125.5(2) . . ? C27 N7 Re1 128.5(2) . . ? C26 N8 C32 107.0(3) . . ? C26 N8 C25 126.1(3) . . ? C32 N8 C25 126.8(3) . . ? C39 N9 C40 106.2(3) . . ? C39 N9 C38 122.1(3) . . ? C40 N9 C38 131.7(3) . . ? C39 N10 C45 104.0(3) . . ? O1 C1 Re2 175.0(3) . . ? O2 C2 Re2 178.5(4) . . ? O3 C3 Re2 176.7(4) . . ? O4 C4 Re1 176.9(4) . . ? O5 C5 Re1 177.1(4) . . ? O6 C6 Re1 178.7(4) . . ? C8 C7 N1 108.8(3) . . ? C8 C7 H7 125.6 . . ? N1 C7 H7 125.6 . . ? C7 C8 N2 109.1(3) . . ? C7 C8 H8 125.4 . . ? N2 C8 H8 125.4 . . ? N2 C9 N1 116.4(3) . . ? N2 C9 C10 122.0(3) . . ? N1 C9 C10 121.0(3) . . ? N4 C10 N3 116.6(3) . . ? N4 C10 C9 121.1(3) . . ? N3 C10 C9 121.9(3) . . ? C12 C11 N3 108.8(3) . . ? C12 C11 H11 125.6 . . ? N3 C11 H11 125.6 . . ? C11 C12 N4 108.9(3) . . ? C11 C12 H12 125.6 . . ? N4 C12 H12 125.6 . . ? N5 C13 N6 112.5(3) . . ? N5 C13 S2 124.4(2) . . ? N6 C13 S2 123.1(2) . . ? C19 C14 C15 120.1(3) . . ? C19 C14 N5 109.5(3) . . ? C15 C14 N5 130.3(3) . . ? C16 C15 C14 117.2(3) . . ? C16 C15 H15 121.4 . . ? C14 C15 H15 121.4 . . ? C15 C16 C17 121.9(3) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C18 C17 C16 121.9(3) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C17 C18 C19 116.0(3) . . ? C17 C18 H18 122.0 . . ? C19 C18 H18 122.0 . . ? C14 C19 C18 122.9(3) . . ? C14 C19 N6 105.9(3) . . ? C18 C19 N6 131.1(3) . . ? N6 C20 C21 112.5(3) . . ? N6 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? N6 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C33 C21 C22 120.6(3) . . ? C33 C21 C20 120.8(3) . . ? C22 C21 C20 118.5(3) . . ? C24 C22 C21 119.1(3) . . ? C24 C22 C23 120.4(3) . . ? C21 C22 C23 120.4(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C36 C24 C22 120.5(3) . . ? C36 C24 C25 119.8(3) . . ? C22 C24 C25 119.6(3) . . ? N8 C25 C24 115.1(3) . . ? N8 C25 H25A 108.5 . . ? C24 C25 H25A 108.5 . . ? N8 C25 H25B 108.5 . . ? C24 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? N7 C26 N8 112.3(3) . . ? N7 C26 S1 125.3(3) . . ? N8 C26 S1 122.4(3) . . ? C28 C27 C32 120.5(3) . . ? C28 C27 N7 130.2(3) . . ? C32 C27 N7 109.2(3) . . ? C29 C28 C27 117.5(4) . . ? C29 C28 H28 121.2 . . ? C27 C28 H28 121.2 . . ? C28 C29 C30 121.7(4) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C31 C30 C29 121.7(3) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C32 116.4(4) . . ? C30 C31 H31 121.8 . . ? C32 C31 H31 121.8 . . ? N8 C32 C27 106.1(3) . . ? N8 C32 C31 131.8(3) . . ? C27 C32 C31 122.1(3) . . ? C35 C33 C21 118.8(3) . . ? C35 C33 C34 120.2(3) . . ? C21 C33 C34 121.0(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 C36 121.0(3) . . ? C33 C35 C38 119.9(3) . . ? C36 C35 C38 119.0(3) . . ? C24 C36 C35 119.4(3) . . ? C24 C36 C37 121.3(3) . . ? C35 C36 C37 119.3(3) . . ? 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 . . ? N9 C38 C35 116.8(3) . . ? N9 C38 H38A 108.1 . . ? C35 C38 H38A 108.1 . . ? N9 C38 H38B 108.1 . . ? C35 C38 H38B 108.1 . . ? H38A C38 H38B 107.3 . . ? N10 C39 N9 113.9(4) . . ? N10 C39 S3 126.3(3) . . ? N9 C39 S3 119.7(3) . . ? N9 C40 C45 104.5(4) . . ? N9 C40 C41 133.4(4) . . ? C45 C40 C41 122.1(4) . . ? C42 C41 C40 116.2(4) . . ? C42 C41 H41 121.9 . . ? C40 C41 H41 121.9 . . ? C41 C42 C43 121.3(5) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C44 C43 C42 121.7(5) . . ? C44 C43 H43 119.2 . . ? C42 C43 H43 119.2 . . ? C43 C44 C45 118.7(5) . . ? C43 C44 H44 120.6 . . ? C45 C44 H44 120.6 . . ? C44 C45 N10 128.5(4) . . ? C44 C45 C40 119.9(5) . . ? N10 C45 C40 111.5(4) . . ? S1 C46 H46A 109.5 . . ? S1 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? S1 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? S2 C47 H47A 109.5 . . ? S2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? S2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? S3 C48 H48A 109.5 . . ? S3 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? S3 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C51 124.3(12) . . ? C50 C49 C52 110.4(12) . . ? C51 C49 C52 125.3(9) . . ? C52 C51 C49 121.6(8) 2_666 . ? C51 C52 C49 113.1(8) 2_666 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Re2 N1 C9 179.7(2) . . . . ? C3 Re2 N1 C9 91.7(2) . . . . ? C1 Re2 N1 C9 42.1(17) . . . . ? N5 Re2 N1 C9 -85.1(2) . . . . ? N3 Re2 N1 C9 -2.9(2) . . . . ? C2 Re2 N1 C7 21.3(4) . . . . ? C3 Re2 N1 C7 -66.7(4) . . . . ? C1 Re2 N1 C7 -116.2(16) . . . . ? N5 Re2 N1 C7 116.5(4) . . . . ? N3 Re2 N1 C7 -161.3(4) . . . . ? C4 Re1 N2 C9 -15.5(12) . . . . ? C6 Re1 N2 C9 -90.9(2) . . . . ? C5 Re1 N2 C9 176.9(2) . . . . ? N7 Re1 N2 C9 85.6(2) . . . . ? N4 Re1 N2 C9 0.9(2) . . . . ? C4 Re1 N2 C8 149.6(11) . . . . ? C6 Re1 N2 C8 74.3(4) . . . . ? C5 Re1 N2 C8 -18.0(4) . . . . ? N7 Re1 N2 C8 -109.3(4) . . . . ? N4 Re1 N2 C8 166.0(4) . . . . ? C2 Re2 N3 C10 23.8(12) . . . . ? C3 Re2 N3 C10 -83.7(2) . . . . ? C1 Re2 N3 C10 -174.7(2) . . . . ? N5 Re2 N3 C10 91.0(2) . . . . ? N1 Re2 N3 C10 2.0(2) . . . . ? C2 Re2 N3 C11 -168.8(10) . . . . ? C3 Re2 N3 C11 83.7(4) . . . . ? C1 Re2 N3 C11 -7.3(4) . . . . ? N5 Re2 N3 C11 -101.6(4) . . . . ? N1 Re2 N3 C11 169.4(4) . . . . ? C4 Re1 N4 C10 175.6(2) . . . . ? C6 Re1 N4 C10 89.7(2) . . . . ? C5 Re1 N4 C10 -42.1(13) . . . . ? N7 Re1 N4 C10 -87.6(2) . . . . ? N2 Re1 N4 C10 -2.5(2) . . . . ? C4 Re1 N4 C12 13.5(4) . . . . ? C6 Re1 N4 C12 -72.4(4) . . . . ? C5 Re1 N4 C12 155.8(12) . . . . ? N7 Re1 N4 C12 110.3(4) . . . . ? N2 Re1 N4 C12 -164.6(4) . . . . ? C2 Re2 N5 C13 -130.2(3) . . . . ? C3 Re2 N5 C13 106.3(11) . . . . ? C1 Re2 N5 C13 -42.1(3) . . . . ? N1 Re2 N5 C13 134.2(3) . . . . ? N3 Re2 N5 C13 56.2(2) . . . . ? C2 Re2 N5 C14 55.0(3) . . . . ? C3 Re2 N5 C14 -68.4(11) . . . . ? C1 Re2 N5 C14 143.2(2) . . . . ? N1 Re2 N5 C14 -40.5(2) . . . . ? N3 Re2 N5 C14 -118.6(2) . . . . ? C4 Re1 N7 C26 43.1(3) . . . . ? C6 Re1 N7 C26 -84.8(15) . . . . ? C5 Re1 N7 C26 132.4(3) . . . . ? N2 Re1 N7 C26 -130.3(3) . . . . ? N4 Re1 N7 C26 -52.1(3) . . . . ? C4 Re1 N7 C27 -148.4(3) . . . . ? C6 Re1 N7 C27 83.7(15) . . . . ? C5 Re1 N7 C27 -59.1(3) . . . . ? N2 Re1 N7 C27 38.3(3) . . . . ? N4 Re1 N7 C27 116.4(3) . . . . ? C2 Re2 C1 O1 -23(4) . . . . ? C3 Re2 C1 O1 65(4) . . . . ? N5 Re2 C1 O1 -118(4) . . . . ? N1 Re2 C1 O1 115(4) . . . . ? N3 Re2 C1 O1 159(4) . . . . ? C3 Re2 C2 O2 -46(15) . . . . ? C1 Re2 C2 O2 44(15) . . . . ? N5 Re2 C2 O2 140(15) . . . . ? N1 Re2 C2 O2 -133(15) . . . . ? N3 Re2 C2 O2 -154(15) . . . . ? C2 Re2 C3 O3 -81(7) . . . . ? C1 Re2 C3 O3 -169(7) . . . . ? N5 Re2 C3 O3 42(8) . . . . ? N1 Re2 C3 O3 14(7) . . . . ? N3 Re2 C3 O3 92(7) . . . . ? C6 Re1 C4 O4 -15(6) . . . . ? C5 Re1 C4 O4 77(6) . . . . ? N7 Re1 C4 O4 169(6) . . . . ? N2 Re1 C4 O4 -91(6) . . . . ? N4 Re1 C4 O4 -107(6) . . . . ? C4 Re1 C5 O5 32(6) . . . . ? C6 Re1 C5 O5 117(6) . . . . ? N7 Re1 C5 O5 -66(6) . . . . ? N2 Re1 C5 O5 -150(6) . . . . ? N4 Re1 C5 O5 -111(6) . . . . ? C4 Re1 C6 O6 -25(16) . . . . ? C5 Re1 C6 O6 -114(16) . . . . ? N7 Re1 C6 O6 104(16) . . . . ? N2 Re1 C6 O6 149(16) . . . . ? N4 Re1 C6 O6 71(16) . . . . ? C9 N1 C7 C8 0.1(4) . . . . ? Re2 N1 C7 C8 159.4(3) . . . . ? N1 C7 C8 N2 -0.1(4) . . . . ? C9 N2 C8 C7 0.0(4) . . . . ? Re1 N2 C8 C7 -165.6(3) . . . . ? C8 N2 C9 N1 0.1(4) . . . . ? Re1 N2 C9 N1 171.8(2) . . . . ? C8 N2 C9 C10 -170.8(3) . . . . ? Re1 N2 C9 C10 0.9(4) . . . . ? C7 N1 C9 N2 -0.1(4) . . . . ? Re2 N1 C9 N2 -167.4(2) . . . . ? C7 N1 C9 C10 170.9(3) . . . . ? Re2 N1 C9 C10 3.6(4) . . . . ? C12 N4 C10 N3 1.3(4) . . . . ? Re1 N4 C10 N3 -168.5(2) . . . . ? C12 N4 C10 C9 173.8(3) . . . . ? Re1 N4 C10 C9 3.9(4) . . . . ? C11 N3 C10 N4 -1.6(4) . . . . ? Re2 N3 C10 N4 171.5(2) . . . . ? C11 N3 C10 C9 -174.0(3) . . . . ? Re2 N3 C10 C9 -0.8(4) . . . . ? N2 C9 C10 N4 -3.5(5) . . . . ? N1 C9 C10 N4 -174.0(3) . . . . ? N2 C9 C10 N3 168.5(3) . . . . ? N1 C9 C10 N3 -2.0(5) . . . . ? C10 N3 C11 C12 1.2(4) . . . . ? Re2 N3 C11 C12 -166.6(3) . . . . ? N3 C11 C12 N4 -0.5(4) . . . . ? C10 N4 C12 C11 -0.4(4) . . . . ? Re1 N4 C12 C11 162.3(3) . . . . ? C14 N5 C13 N6 1.3(3) . . . . ? Re2 N5 C13 N6 -174.35(18) . . . . ? C14 N5 C13 S2 -179.3(2) . . . . ? Re2 N5 C13 S2 5.0(4) . . . . ? C19 N6 C13 N5 -1.9(3) . . . . ? C20 N6 C13 N5 171.2(3) . . . . ? C19 N6 C13 S2 178.7(2) . . . . ? C20 N6 C13 S2 -8.2(4) . . . . ? C47 S2 C13 N5 108.3(3) . . . . ? C47 S2 C13 N6 -72.4(3) . . . . ? C13 N5 C14 C19 -0.1(3) . . . . ? Re2 N5 C14 C19 175.60(19) . . . . ? C13 N5 C14 C15 176.0(3) . . . . ? Re2 N5 C14 C15 -8.3(5) . . . . ? C19 C14 C15 C16 0.6(5) . . . . ? N5 C14 C15 C16 -175.2(3) . . . . ? C14 C15 C16 C17 -0.3(5) . . . . ? C15 C16 C17 C18 0.0(6) . . . . ? C16 C17 C18 C19 0.1(5) . . . . ? C15 C14 C19 C18 -0.6(5) . . . . ? N5 C14 C19 C18 176.0(3) . . . . ? C15 C14 C19 N6 -177.6(3) . . . . ? N5 C14 C19 N6 -1.0(3) . . . . ? C17 C18 C19 C14 0.3(5) . . . . ? C17 C18 C19 N6 176.4(3) . . . . ? C13 N6 C19 C14 1.7(3) . . . . ? C20 N6 C19 C14 -171.6(3) . . . . ? C13 N6 C19 C18 -174.9(3) . . . . ? C20 N6 C19 C18 11.8(5) . . . . ? C13 N6 C20 C21 -123.2(3) . . . . ? C19 N6 C20 C21 48.7(4) . . . . ? N6 C20 C21 C33 -124.8(3) . . . . ? N6 C20 C21 C22 56.6(4) . . . . ? C33 C21 C22 C24 6.6(5) . . . . ? C20 C21 C22 C24 -174.8(3) . . . . ? C33 C21 C22 C23 -171.7(3) . . . . ? C20 C21 C22 C23 6.9(4) . . . . ? C21 C22 C24 C36 -5.2(5) . . . . ? C23 C22 C24 C36 173.2(3) . . . . ? C21 C22 C24 C25 179.3(3) . . . . ? C23 C22 C24 C25 -2.4(5) . . . . ? C26 N8 C25 C24 123.8(3) . . . . ? C32 N8 C25 C24 -58.4(4) . . . . ? C36 C24 C25 N8 126.6(3) . . . . ? C22 C24 C25 N8 -57.9(4) . . . . ? C27 N7 C26 N8 -3.0(4) . . . . ? Re1 N7 C26 N8 167.7(2) . . . . ? C27 N7 C26 S1 175.6(2) . . . . ? Re1 N7 C26 S1 -13.7(4) . . . . ? C32 N8 C26 N7 2.6(4) . . . . ? C25 N8 C26 N7 -179.4(3) . . . . ? C32 N8 C26 S1 -176.1(2) . . . . ? C25 N8 C26 S1 2.0(5) . . . . ? C46 S1 C26 N7 -95.1(3) . . . . ? C46 S1 C26 N8 83.4(3) . . . . ? C26 N7 C27 C28 -174.4(3) . . . . ? Re1 N7 C27 C28 15.3(5) . . . . ? C26 N7 C27 C32 2.3(4) . . . . ? Re1 N7 C27 C32 -168.0(2) . . . . ? C32 C27 C28 C29 1.2(5) . . . . ? N7 C27 C28 C29 177.6(3) . . . . ? C27 C28 C29 C30 0.6(6) . . . . ? C28 C29 C30 C31 -1.7(6) . . . . ? C29 C30 C31 C32 0.8(6) . . . . ? C26 N8 C32 C27 -0.9(3) . . . . ? C25 N8 C32 C27 -179.0(3) . . . . ? C26 N8 C32 C31 177.2(4) . . . . ? C25 N8 C32 C31 -0.9(6) . . . . ? C28 C27 C32 N8 176.2(3) . . . . ? N7 C27 C32 N8 -0.9(4) . . . . ? C28 C27 C32 C31 -2.1(5) . . . . ? N7 C27 C32 C31 -179.2(3) . . . . ? C30 C31 C32 N8 -176.8(3) . . . . ? C30 C31 C32 C27 1.1(5) . . . . ? C22 C21 C33 C35 -1.7(5) . . . . ? C20 C21 C33 C35 179.7(3) . . . . ? C22 C21 C33 C34 179.2(3) . . . . ? C20 C21 C33 C34 0.6(5) . . . . ? C21 C33 C35 C36 -4.8(5) . . . . ? C34 C33 C35 C36 174.4(3) . . . . ? C21 C33 C35 C38 173.1(3) . . . . ? C34 C33 C35 C38 -7.7(5) . . . . ? C22 C24 C36 C35 -1.2(5) . . . . ? C25 C24 C36 C35 174.3(3) . . . . ? C22 C24 C36 C37 178.2(3) . . . . ? C25 C24 C36 C37 -6.3(5) . . . . ? C33 C35 C36 C24 6.2(5) . . . . ? C38 C35 C36 C24 -171.7(3) . . . . ? C33 C35 C36 C37 -173.2(3) . . . . ? C38 C35 C36 C37 8.9(5) . . . . ? C39 N9 C38 C35 -174.8(3) . . . . ? C40 N9 C38 C35 7.4(6) . . . . ? C33 C35 C38 N9 91.8(4) . . . . ? C36 C35 C38 N9 -90.3(4) . . . . ? C45 N10 C39 N9 0.2(4) . . . . ? C45 N10 C39 S3 178.5(3) . . . . ? C40 N9 C39 N10 -0.3(4) . . . . ? C38 N9 C39 N10 -178.6(3) . . . . ? C40 N9 C39 S3 -178.7(3) . . . . ? C38 N9 C39 S3 2.9(5) . . . . ? C48 S3 C39 N10 -0.4(4) . . . . ? C48 S3 C39 N9 177.8(3) . . . . ? C39 N9 C40 C45 0.2(4) . . . . ? C38 N9 C40 C45 178.3(4) . . . . ? C39 N9 C40 C41 179.4(4) . . . . ? C38 N9 C40 C41 -2.5(7) . . . . ? N9 C40 C41 C42 -176.5(4) . . . . ? C45 C40 C41 C42 2.6(5) . . . . ? C40 C41 C42 C43 -0.9(6) . . . . ? C41 C42 C43 C44 -0.2(7) . . . . ? C42 C43 C44 C45 -0.3(7) . . . . ? C43 C44 C45 N10 177.4(4) . . . . ? C43 C44 C45 C40 2.0(7) . . . . ? C39 N10 C45 C44 -175.8(4) . . . . ? C39 N10 C45 C40 -0.1(4) . . . . ? N9 C40 C45 C44 176.1(4) . . . . ? C41 C40 C45 C44 -3.2(6) . . . . ? N9 C40 C45 N10 -0.1(4) . . . . ? C41 C40 C45 N10 -179.4(3) . . . . ? C50 C49 C51 C52 -178.1(9) . . . 2_666 ? C52 C49 C51 C52 0.5(12) . . . 2_666 ? C50 C49 C52 C51 178.3(8) . . . 2_666 ? C51 C49 C52 C51 -0.5(11) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.818 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.096 _iucr_refine_instructions_details ; TITL RK5-98 in P1 New: P-1 CELL 0.71073 13.1042 13.4573 14.6018 91.058 93.181 101.095 ZERR 2 0.0004 0.0004 0.0005 0.003 0.003 0.003 LATT 1 SFAC C H N O Re S UNIT 104 80 20 12 4 6 L.S. 40 FMAP 2 PLAN -20 ACTA 50.0 SADI C49 C51 C49 C52 rem delu 0.02 c49 c50 rem simu 0.004 c49 c50 merg 2 BOND $H dfix c50 c49 1.5 CONF WGHT 0.022500 1.434000 FVAR 2.22461 RE1 5 0.496123 0.153558 0.138610 11.00000 0.02321 0.02918 = 0.04113 0.00305 0.00465 0.00765 RE2 5 0.238228 0.366854 -0.078369 11.00000 0.02794 0.02877 = 0.02550 0.00297 0.00279 0.00276 S1 6 0.481814 0.294899 0.352162 11.00000 0.03330 0.04263 = 0.04726 -0.00220 -0.00628 0.00488 S2 6 0.214820 0.553448 0.103482 11.00000 0.03307 0.02497 = 0.04032 0.00238 0.00244 0.00312 S3 6 -0.249450 0.287237 0.679266 11.00000 0.05895 0.07399 = 0.05241 0.00233 0.02492 0.01169 O1 4 0.233832 0.584795 -0.132436 11.00000 0.09443 0.04520 = 0.06855 0.02553 0.01181 0.02379 O2 4 0.066380 0.306065 -0.229530 11.00000 0.06750 0.11007 = 0.04173 -0.01307 -0.02194 0.01121 O3 4 0.394953 0.349106 -0.221618 11.00000 0.09372 0.09044 = 0.08331 -0.01000 0.06203 0.00092 O4 4 0.691090 0.216573 0.266870 11.00000 0.03259 0.08121 = 0.07088 0.00448 -0.01100 0.00963 O5 4 0.522916 -0.065772 0.158645 11.00000 0.06594 0.03932 = 0.09298 0.01612 0.02484 0.02215 O6 4 0.649063 0.190451 -0.012823 11.00000 0.05576 0.06992 = 0.06706 0.00841 0.03119 0.00728 N1 3 0.252927 0.211092 -0.043129 11.00000 0.03144 0.02379 = 0.03391 -0.00232 0.00064 0.00408 N2 3 0.357477 0.126242 0.039124 11.00000 0.02675 0.02748 = 0.04085 -0.00273 0.00204 0.00529 N3 3 0.359698 0.394026 0.038612 11.00000 0.02751 0.02452 = 0.03586 0.00195 -0.00120 0.00260 N4 3 0.459060 0.308264 0.126310 11.00000 0.02469 0.02762 = 0.03784 0.00086 0.00021 0.00482 N5 3 0.133488 0.363041 0.034665 11.00000 0.02468 0.02634 = 0.03198 0.00348 0.00231 0.00350 N6 3 0.063843 0.402395 0.163538 11.00000 0.02820 0.02966 = 0.02892 0.00007 0.00194 0.00714 N7 3 0.378072 0.136322 0.242809 11.00000 0.02617 0.03081 = 0.03874 0.00084 0.00255 0.00606 N8 3 0.285481 0.180996 0.354683 11.00000 0.03307 0.03450 = 0.03216 0.00196 0.00428 0.00857 N9 3 -0.169053 0.213021 0.532840 11.00000 0.04009 0.05063 = 0.03633 0.00700 0.01173 0.00933 N10 3 -0.320490 0.118133 0.572279 11.00000 0.05030 0.05485 = 0.06038 0.01694 0.00746 0.00652 C1 1 0.237476 0.504321 -0.108145 11.00000 0.04414 0.04576 = 0.03111 0.00677 0.00358 0.01061 C2 1 0.131079 0.328287 -0.171240 11.00000 0.04517 0.04973 = 0.03376 0.00008 0.00261 0.00850 C3 1 0.336227 0.358863 -0.167798 11.00000 0.04918 0.04085 = 0.04528 0.00108 0.01419 -0.00185 C4 1 0.615627 0.193105 0.220405 11.00000 0.03157 0.04167 = 0.05254 0.00787 0.00654 0.01091 C5 1 0.511792 0.016128 0.148810 11.00000 0.03093 0.04215 = 0.05531 0.00775 0.01394 0.01091 C6 1 0.590834 0.175818 0.043360 11.00000 0.03565 0.03863 = 0.05289 0.00378 0.00912 0.00779 C7 1 0.233821 0.112001 -0.074491 11.00000 0.03398 0.02960 = 0.04090 -0.00747 0.00061 -0.00123 AFIX 43 H7 2 0.185762 0.084448 -0.121864 11.00000 -1.20000 AFIX 0 C8 1 0.296856 0.060696 -0.024787 11.00000 0.03366 0.02780 = 0.04394 -0.00707 0.00442 0.00258 AFIX 43 H8 2 0.298658 -0.007657 -0.032745 11.00000 -1.20000 AFIX 0 C9 1 0.326671 0.212984 0.023537 11.00000 0.02585 0.02610 = 0.03800 0.00156 0.00305 0.00292 C10 1 0.379222 0.305335 0.065448 11.00000 0.02462 0.02754 = 0.03699 -0.00064 0.00122 0.00231 C11 1 0.434024 0.462772 0.089717 11.00000 0.03020 0.02407 = 0.04343 -0.00156 0.00050 -0.00209 AFIX 43 H11 2 0.441789 0.532890 0.088519 11.00000 -1.20000 AFIX 0 C12 1 0.494490 0.410594 0.142520 11.00000 0.02697 0.03075 = 0.04489 -0.00035 -0.00031 0.00042 AFIX 43 H12 2 0.550283 0.439567 0.182694 11.00000 -1.20000 AFIX 0 C13 1 0.133629 0.433589 0.099305 11.00000 0.02493 0.02738 = 0.02668 0.00387 -0.00070 0.00691 C14 1 0.056866 0.281135 0.057359 11.00000 0.02212 0.03067 = 0.02983 0.00477 -0.00114 0.00379 C15 1 0.019166 0.188827 0.010968 11.00000 0.03330 0.03387 = 0.03919 -0.00344 0.00299 0.00125 AFIX 43 H15 2 0.048334 0.170962 -0.042065 11.00000 -1.20000 AFIX 0 C16 1 -0.062720 0.125467 0.046794 11.00000 0.04098 0.03361 = 0.04784 -0.00295 0.00166 -0.00661 AFIX 43 H16 2 -0.089695 0.063487 0.017092 11.00000 -1.20000 AFIX 0 C17 1 -0.106678 0.151233 0.126383 11.00000 0.03692 0.04199 = 0.04915 0.00538 0.00947 -0.01134 AFIX 43 H17 2 -0.162188 0.105970 0.148284 11.00000 -1.20000 AFIX 0 C18 1 -0.070595 0.241173 0.173287 11.00000 0.03286 0.04493 = 0.03407 0.00380 0.00856 0.00050 AFIX 43 H18 2 -0.099863 0.258421 0.226479 11.00000 -1.20000 AFIX 0 C19 1 0.012350 0.305226 0.136770 11.00000 0.02372 0.02979 = 0.02984 0.00348 -0.00293 0.00366 C20 1 0.052854 0.454728 0.250210 11.00000 0.03467 0.03685 = 0.03071 -0.00095 0.00527 0.01199 AFIX 23 H20A 2 -0.014699 0.474278 0.248504 11.00000 -1.20000 H20B 2 0.105786 0.516054 0.256863 11.00000 -1.20000 AFIX 0 C21 1 0.063173 0.388772 0.333822 11.00000 0.03183 0.03152 = 0.02487 -0.00446 0.00059 0.00514 C22 1 0.154247 0.349120 0.347620 11.00000 0.02986 0.03633 = 0.02414 -0.00223 0.00306 0.00561 C23 1 0.244610 0.380427 0.288035 11.00000 0.02967 0.05068 = 0.03483 0.01123 0.00455 0.01129 AFIX 137 H23A 2 0.308743 0.381119 0.323395 11.00000 -1.50000 H23B 2 0.243753 0.446923 0.265690 11.00000 -1.50000 H23C 2 0.238880 0.333175 0.237077 11.00000 -1.50000 AFIX 0 C24 1 0.161044 0.282208 0.419004 11.00000 0.03381 0.04065 = 0.02573 -0.00161 0.00174 0.00876 C25 1 0.258904 0.237823 0.433945 11.00000 0.04017 0.04458 = 0.02613 -0.00137 0.00157 0.01446 AFIX 23 H25A 2 0.317093 0.292661 0.450508 11.00000 -1.20000 H25B 2 0.250075 0.193144 0.485486 11.00000 -1.20000 AFIX 0 C26 1 0.377495 0.199428 0.313000 11.00000 0.02952 0.03214 = 0.03438 0.00298 0.00227 0.00801 C27 1 0.282281 0.069263 0.241311 11.00000 0.03007 0.03115 = 0.03558 0.00528 0.00117 0.00572 C28 1 0.244430 -0.016793 0.186934 11.00000 0.04129 0.03444 = 0.04248 -0.00107 0.00635 0.00191 AFIX 43 H28 2 0.283258 -0.037148 0.141178 11.00000 -1.20000 AFIX 0 C29 1 0.147149 -0.071073 0.203172 11.00000 0.04836 0.04015 = 0.04316 -0.00072 0.00125 -0.00801 AFIX 43 H29 2 0.120292 -0.129520 0.167990 11.00000 -1.20000 AFIX 0 C30 1 0.088371 -0.040930 0.270426 11.00000 0.03581 0.05282 = 0.05291 0.00763 0.00923 -0.00964 AFIX 43 H30 2 0.022260 -0.078638 0.278225 11.00000 -1.20000 AFIX 0 C31 1 0.125163 0.043467 0.326161 11.00000 0.03651 0.04805 = 0.04327 0.00611 0.00928 0.00128 AFIX 43 H31 2 0.086023 0.063336 0.371904 11.00000 -1.20000 AFIX 0 C32 1 0.224112 0.097472 0.310369 11.00000 0.02934 0.03592 = 0.03434 0.00593 0.00260 0.00695 C33 1 -0.015502 0.370376 0.396135 11.00000 0.03192 0.04031 = 0.03205 -0.00622 0.00555 0.00712 C34 1 -0.113575 0.414128 0.382490 11.00000 0.04147 0.06835 = 0.05744 0.00584 0.01866 0.02260 AFIX 137 H34A 2 -0.134695 0.411638 0.318341 11.00000 -1.50000 H34B 2 -0.099884 0.483179 0.404987 11.00000 -1.50000 H34C 2 -0.168156 0.375232 0.415514 11.00000 -1.50000 AFIX 0 C35 1 -0.003032 0.309797 0.470662 11.00000 0.03743 0.04629 = 0.02470 -0.00590 0.00666 0.00471 C36 1 0.082296 0.261596 0.480111 11.00000 0.04140 0.04937 = 0.02335 0.00316 0.00559 0.00856 C37 1 0.086704 0.186853 0.556468 11.00000 0.06023 0.08782 = 0.04189 0.02778 0.01539 0.02470 AFIX 137 H37A 2 0.119778 0.133451 0.535815 11.00000 -1.50000 H37B 2 0.017255 0.158691 0.572590 11.00000 -1.50000 H37C 2 0.125861 0.221254 0.609179 11.00000 -1.50000 AFIX 0 C38 1 -0.080362 0.298309 0.544399 11.00000 0.04448 0.06856 = 0.03070 -0.00290 0.01359 0.00911 AFIX 23 H38A 2 -0.043180 0.291667 0.602587 11.00000 -1.20000 H38B 2 -0.107476 0.360327 0.548439 11.00000 -1.20000 AFIX 0 C39 1 -0.249068 0.199195 0.591661 11.00000 0.04146 0.06056 = 0.04002 0.01509 0.01255 0.01523 C40 1 -0.191728 0.132039 0.469689 11.00000 0.04840 0.04820 = 0.04252 0.00819 -0.00125 0.01483 C41 1 -0.141548 0.104209 0.393657 11.00000 0.05679 0.04813 = 0.03716 0.00123 0.00048 0.01610 AFIX 43 H41 2 -0.077643 0.140880 0.377826 11.00000 -1.20000 AFIX 0 C42 1 -0.192668 0.018812 0.343348 11.00000 0.08309 0.05823 = 0.05256 -0.00101 -0.00258 0.02634 AFIX 43 H42 2 -0.162909 -0.002101 0.291797 11.00000 -1.20000 AFIX 0 C43 1 -0.288062 -0.036364 0.368711 11.00000 0.09318 0.04987 = 0.07744 -0.00383 -0.01639 0.01128 AFIX 43 H43 2 -0.320450 -0.093111 0.333449 11.00000 -1.20000 AFIX 0 C44 1 -0.334747 -0.009111 0.443744 11.00000 0.07371 0.04916 = 0.08846 0.01244 -0.00026 0.00359 AFIX 43 H44 2 -0.398385 -0.046404 0.459523 11.00000 -1.20000 AFIX 0 C45 1 -0.285778 0.074958 0.495942 11.00000 0.05133 0.04754 = 0.05380 0.01131 -0.00229 0.01301 C46 1 0.537838 0.227247 0.440968 11.00000 0.05768 0.07436 = 0.06643 0.01144 -0.02222 0.01181 AFIX 137 H46A 2 0.606805 0.263140 0.459217 11.00000 -1.50000 H46B 2 0.541145 0.160647 0.418159 11.00000 -1.50000 H46C 2 0.495423 0.221898 0.492860 11.00000 -1.50000 AFIX 0 C47 1 0.121418 0.630985 0.073176 11.00000 0.05518 0.03862 = 0.08264 0.01698 0.00322 0.01811 AFIX 137 H47A 2 0.157328 0.697546 0.059062 11.00000 -1.50000 H47B 2 0.078578 0.635599 0.123729 11.00000 -1.50000 H47C 2 0.078464 0.601220 0.020551 11.00000 -1.50000 AFIX 0 C48 1 -0.371661 0.231940 0.727264 11.00000 0.06494 0.10913 = 0.07388 0.01900 0.04133 0.01964 AFIX 137 H48A 2 -0.397330 0.283407 0.760350 11.00000 -1.50000 H48B 2 -0.360628 0.179522 0.768232 11.00000 -1.50000 H48C 2 -0.421659 0.203646 0.678595 11.00000 -1.50000 AFIX 0 C49 1 0.415926 0.475121 0.546234 11.00000 0.13702 0.08022 = 0.12660 -0.05491 0.00484 0.00207 C50 1 0.325034 0.456306 0.588494 11.00000 0.22144 0.28428 = 0.32444 -0.14360 0.00099 0.07097 C51 1 0.506342 0.446683 0.578977 11.00000 0.13545 0.07365 = 0.09625 -0.01538 -0.02058 0.02501 C52 1 0.404762 0.529933 0.464807 11.00000 0.19881 0.07343 = 0.08933 -0.02350 -0.02055 0.02804 HKLF 4 REM RK5-98 in P1 New: P-1 REM R1 = 0.0267 for 10181 Fo > 4sig(Fo) and 0.0365 for all 12108 data REM 664 parameters refined using 2 restraints END WGHT 0.0223 1.4788 REM Highest difference peak 0.818, deepest hole -0.698, 1-sigma level 0.096 Q1 1 0.2040 0.4128 -0.0892 11.00000 0.05 0.82 Q2 1 0.5357 0.1980 0.1900 11.00000 0.05 0.77 Q3 1 0.4836 0.1641 0.1928 11.00000 0.05 0.76 Q4 1 0.1777 0.3195 -0.0951 11.00000 0.05 0.66 Q5 1 0.4613 0.1870 0.1023 11.00000 0.05 0.59 Q6 1 0.5455 0.2166 0.1480 11.00000 0.05 0.59 Q7 1 0.2488 0.2946 -0.0761 11.00000 0.05 0.57 Q8 1 0.5420 0.0968 0.1616 11.00000 0.05 0.56 Q9 1 0.4841 0.2366 0.1309 11.00000 0.05 0.54 Q10 1 0.0331 0.4201 0.2969 11.00000 0.05 0.52 Q11 1 0.5868 0.1756 0.1161 11.00000 0.05 0.52 Q12 1 0.2709 0.3291 -0.1341 11.00000 0.05 0.50 Q13 1 0.1954 0.3258 -0.1459 11.00000 0.05 0.48 Q14 1 0.4790 0.0747 0.1572 11.00000 0.05 0.47 Q15 1 0.5121 0.1795 0.0724 11.00000 0.05 0.44 Q16 1 0.3204 0.3648 -0.0752 11.00000 0.05 0.44 Q17 1 0.5139 0.0818 0.1542 11.00000 0.05 0.44 Q18 1 0.4580 0.1161 0.0722 11.00000 0.05 0.43 Q19 1 0.2994 0.3389 -0.0561 11.00000 0.05 0.42 Q20 1 0.2798 0.0218 0.2348 11.00000 0.05 0.41 _restraints_details The solvent molecule is placed across inversion centre which is at the centre of the six-membered ring and hence it appears that the methyl group is not half occupied. The solvent molecule toluene is highly disordered which is quite usual for those placed across symmetry positions in the lattice. SHELXL restraints were used to provide reasonable model for the solvent toluene. ; _database_code_depnum_ccdc_archive 'CCDC 935809' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_update_record ; 2013-06-01 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H38 N6 O12 Re2 S3' _chemical_formula_sum 'C57 H38 N6 O12 Re2 S3' _chemical_formula_weight 1467.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0180 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.346(3) _cell_length_b 13.6127(9) _cell_length_c 18.1764(16) _cell_angle_alpha 90.00 _cell_angle_beta 110.725(12) _cell_angle_gamma 90.00 _cell_volume 5402.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 12234 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 28.28 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2863 _exptl_absorpt_coefficient_mu 4.663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.28 _exptl_absorpt_correction_T_max 0.56 _exptl_absorpt_process_details '(CrysAlis RED; Oxford Diffraction, 2007)' _exptl_special_details ? _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur Sapphire3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9853 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 59145 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_unetI/netI 0.0865 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 28.28 _reflns_number_total 13288 _reflns_number_gt 8954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_data_reduction 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+40.0122P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13288 _refine_ls_number_parameters 718 _refine_ls_number_restraints 131 _refine_ls_R_factor_all 0.1563 _refine_ls_R_factor_gt 0.1023 _refine_ls_wR_factor_ref 0.2268 _refine_ls_wR_factor_gt 0.2030 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0587(8) 0.8478(11) 0.2995(8) 0.067(4) Uani 1 1 d . . . C2 C -0.0849(6) 0.7907(11) 0.4241(8) 0.056(3) Uani 1 1 d . . . C3 C -0.0949(7) 0.6673(12) 0.3079(8) 0.067(4) Uani 1 1 d . . . C4 C 0.0596(6) 0.5847(9) 0.4425(6) 0.042(3) Uani 1 1 d . . . C5 C 0.0959(5) 0.5179(9) 0.4926(7) 0.044(3) Uani 1 1 d . . . C6 C 0.1446(6) 0.4795(9) 0.4742(7) 0.048(3) Uani 1 1 d . . . C7 C 0.1560(6) 0.5120(9) 0.4005(7) 0.051(3) Uani 1 1 d . . . C8 C 0.1198(6) 0.5841(9) 0.3533(7) 0.047(3) Uani 1 1 d . . . C9 C 0.0725(5) 0.6197(8) 0.3715(6) 0.040(3) Uani 1 1 d . . . C10 C 0.2287(10) 0.2622(12) 0.4363(11) 0.092(6) Uani 1 1 d . . . C11 C 0.3052(8) 0.3116(12) 0.5736(12) 0.085(5) Uani 1 1 d . . . C12 C 0.3254(8) 0.3667(13) 0.4492(10) 0.080(5) Uani 1 1 d . . . C13 C 0.0986(6) 0.8663(8) 0.4211(7) 0.042(3) Uani 1 1 d . . . C14 C 0.1020(7) 0.8703(8) 0.3468(7) 0.053(3) Uani 1 1 d . . . H14 H 0.0721 0.8417 0.3038 0.064 Uiso 1 1 calc R . . C15 C 0.1493(8) 0.9162(10) 0.3392(8) 0.062(4) Uani 1 1 d . . . H15 H 0.1517 0.9198 0.2893 0.075 Uiso 1 1 calc R . . C16 C 0.1946(8) 0.9584(11) 0.3999(9) 0.072(4) Uani 1 1 d . . . H16 H 0.2273 0.9882 0.3907 0.087 Uiso 1 1 calc R . . C17 C 0.1931(7) 0.9581(10) 0.4774(8) 0.060(4) Uani 1 1 d . . . H17 H 0.2231 0.9878 0.5198 0.072 Uiso 1 1 calc R . . C18 C 0.1433(6) 0.9097(8) 0.4845(7) 0.043(3) Uani 1 1 d . . . C19 C 0.0697(5) 0.8481(8) 0.5219(6) 0.036(2) Uani 1 1 d . . . C20 C 0.0341(6) 0.8321(8) 0.5720(6) 0.050(2) Uani 1 1 d DU . . C21 C 0.0209(6) 0.7377(10) 0.6016(6) 0.054(2) Uani 1 1 d DU . . H21 H 0.0365 0.6761 0.5970 0.064 Uiso 1 1 calc R . . C22 C -0.0221(7) 0.7628(12) 0.6395(8) 0.076(3) Uani 1 1 d DU . . H22 H -0.0383 0.7147 0.6629 0.091 Uiso 1 1 calc R . . C23 C -0.0386(7) 0.8606(12) 0.6401(8) 0.084(3) Uani 1 1 d DU . . H23 H -0.0656 0.8848 0.6630 0.101 Uiso 1 1 calc R . . C24 C 0.2993(6) 0.6126(8) 0.5004(7) 0.046(3) Uani 1 1 d . . . C25 C 0.2938(7) 0.6294(10) 0.4226(8) 0.064(4) Uani 1 1 d . . . H25 H 0.2808 0.5801 0.3849 0.077 Uiso 1 1 calc R . . C26 C 0.3083(8) 0.7200(11) 0.4041(9) 0.073(5) Uani 1 1 d . . . H26 H 0.3053 0.7327 0.3526 0.088 Uiso 1 1 calc R . . C27 C 0.3272(8) 0.7943(11) 0.4591(8) 0.068(4) Uani 1 1 d . . . H27 H 0.3364 0.8555 0.4433 0.081 Uiso 1 1 calc R . . C28 C 0.3328(7) 0.7815(9) 0.5343(8) 0.061(4) Uani 1 1 d . . . H28 H 0.3455 0.8321 0.5709 0.073 Uiso 1 1 calc R . . C29 C 0.3187(6) 0.6894(9) 0.5549(7) 0.047(3) Uani 1 1 d . . . C30 C 0.3038(6) 0.5562(9) 0.6143(7) 0.045(3) Uani 1 1 d . . . C31 C 0.3034(6) 0.4867(9) 0.6792(7) 0.060(3) Uani 1 1 d DU . . C32 C 0.2465(8) 0.4454(13) 0.6905(10) 0.100 Uiso 1 1 d DU . . H32 H 0.2054 0.4548 0.6608 0.120 Uiso 1 1 calc R . . C33 C 0.2754(8) 0.3859(12) 0.7624(9) 0.086(4) Uani 1 1 d DU . . H33 H 0.2518 0.3495 0.7844 0.103 Uiso 1 1 calc R . . C34 C 0.3386(8) 0.3865(13) 0.7955(10) 0.096(5) Uani 1 1 d DU . . H34 H 0.3606 0.3525 0.8412 0.116 Uiso 1 1 calc R . . C35 C 0.3363(6) 0.7015(9) 0.7021(7) 0.051(3) Uani 1 1 d . . . H35A H 0.3806 0.7048 0.7253 0.061 Uiso 1 1 calc R . . H35B H 0.3219 0.6628 0.7369 0.061 Uiso 1 1 calc R . . C36 C 0.3112(6) 0.8028(8) 0.6973(6) 0.040(3) Uani 1 1 d . . . C37 C 0.2473(6) 0.8199(8) 0.6665(6) 0.041(3) Uani 1 1 d . . . C38 C 0.2041(6) 0.7330(9) 0.6413(8) 0.056(3) Uani 1 1 d . . . H38A H 0.2231 0.6762 0.6712 0.084 Uiso 1 1 calc R . . H38B H 0.1950 0.7204 0.5863 0.084 Uiso 1 1 calc R . . H38C H 0.1669 0.7476 0.6502 0.084 Uiso 1 1 calc R . . C39 C 0.2256(5) 0.9147(8) 0.6619(6) 0.040(3) Uani 1 1 d . . . C40 C 0.1562(6) 0.9329(10) 0.6289(7) 0.052(3) Uani 1 1 d . . . H40A H 0.1380 0.9013 0.6632 0.063 Uiso 1 1 calc R . . H40B H 0.1489 1.0030 0.6302 0.063 Uiso 1 1 calc R . . C41 C 0.2405(8) 1.1007(11) 0.6923(13) 0.108(8) Uani 1 1 d . . . H41A H 0.2099 1.1004 0.7163 0.162 Uiso 1 1 calc R . . H41B H 0.2228 1.1243 0.6392 0.162 Uiso 1 1 calc R . . H41C H 0.2736 1.1428 0.7216 0.162 Uiso 1 1 calc R . . C42 C 0.2653(6) 0.9930(9) 0.6917(7) 0.048(3) Uani 1 1 d . . . C43 C 0.3279(6) 0.9777(9) 0.7237(7) 0.045(3) Uani 1 1 d . . . C44 C 0.3510(6) 0.8820(9) 0.7277(7) 0.051(3) Uani 1 1 d . . . C45 C 0.4192(6) 0.8648(11) 0.7675(10) 0.070(4) Uani 1 1 d . . . H45A H 0.4261 0.7999 0.7894 0.106 Uiso 1 1 calc R . . H45B H 0.4358 0.9122 0.8087 0.106 Uiso 1 1 calc R . . H45C H 0.4390 0.8715 0.7296 0.106 Uiso 1 1 calc R . . C46 C 0.3721(6) 1.0625(10) 0.7573(8) 0.057(3) Uani 1 1 d . . . H46A H 0.3483 1.1225 0.7506 0.068 Uiso 1 1 calc R . . H46B H 0.3919 1.0519 0.8134 0.068 Uiso 1 1 calc R . . C47 C 0.4150(7) 1.0742(10) 0.6469(9) 0.064(4) Uani 1 1 d . . . C48 C 0.3666(8) 1.0579(12) 0.5765(10) 0.075(4) Uani 1 1 d . . . H48 H 0.3273 1.0457 0.5761 0.090 Uiso 1 1 calc R . . C49 C 0.3779(10) 1.0601(13) 0.5104(11) 0.089(5) Uani 1 1 d . . . H49 H 0.3459 1.0498 0.4630 0.107 Uiso 1 1 calc R . . C50 C 0.4372(12) 1.0776(17) 0.5095(13) 0.109(7) Uani 1 1 d . . . H50 H 0.4435 1.0798 0.4619 0.131 Uiso 1 1 calc R . . C51 C 0.4851(10) 1.0913(17) 0.5781(14) 0.110(7) Uani 1 1 d . . . H51 H 0.5244 1.1006 0.5776 0.132 Uiso 1 1 calc R . . C52 C 0.4749(8) 1.0912(14) 0.6478(12) 0.084(5) Uani 1 1 d . . . C53 C 0.4793(7) 1.1024(11) 0.7676(11) 0.072(4) Uani 1 1 d . . . C54 C 0.5026(7) 1.1155(12) 0.8524(11) 0.104(4) Uani 1 1 d DU . . C55 C 0.4917(7) 1.2051(15) 0.8946(9) 0.103(4) Uani 1 1 d DU . . H55 H 0.4717 1.2635 0.8743 0.124 Uiso 1 1 calc R . . C56 C 0.5217(10) 1.174(2) 0.9771(11) 0.135(5) Uani 1 1 d DU . . H56 H 0.5192 1.2124 1.0181 0.162 Uiso 1 1 calc R . . C57 C 0.5549(11) 1.0830(19) 0.9929(12) 0.144(5) Uani 1 1 d DU . . H57 H 0.5757 1.0576 1.0427 0.173 Uiso 1 1 calc R . . N1 N 0.0540(4) 0.8263(7) 0.4473(5) 0.040(2) Uani 1 1 d . . . N2 N 0.2895(5) 0.5288(7) 0.5388(5) 0.045(2) Uani 1 1 d . . . N3 N 0.3193(5) 0.6505(7) 0.6253(6) 0.048(2) Uani 1 1 d . . . N4 N 0.1246(5) 0.8970(7) 0.5475(5) 0.042(2) Uani 1 1 d . . . N5 N 0.4191(6) 1.0778(8) 0.7241(7) 0.058(3) Uani 1 1 d . . . N6 N 0.5138(7) 1.1092(12) 0.7234(9) 0.092(5) Uani 1 1 d . . . O1 O 0.0126(4) 0.6258(6) 0.4518(5) 0.049(2) Uani 1 1 d . . . O2 O 0.0354(4) 0.6820(6) 0.3283(4) 0.046(2) Uani 1 1 d . . . O3 O -0.0758(7) 0.9082(9) 0.2539(7) 0.103(4) Uani 1 1 d . . . O4 O -0.1179(5) 0.8129(10) 0.4526(6) 0.083(3) Uani 1 1 d . . . O5 O -0.1338(6) 0.6215(10) 0.2661(7) 0.096(4) Uani 1 1 d . . . O6 O 0.1311(5) 0.6169(7) 0.2890(5) 0.070(3) Uani 1 1 d . . . H6 H 0.1057 0.6589 0.2665 0.105 Uiso 1 1 calc R . . O7 O 0.0872(5) 0.4912(8) 0.5605(5) 0.070(3) Uani 1 1 d . . . H7 H 0.1128 0.4501 0.5838 0.104 Uiso 1 1 calc R . . O8 O 0.1807(4) 0.4163(6) 0.5156(5) 0.052(2) Uani 1 1 d . . . O9 O 0.2021(4) 0.4710(7) 0.3910(5) 0.055(2) Uani 1 1 d . . . O10 O 0.3624(8) 0.3564(12) 0.4241(9) 0.133(6) Uani 1 1 d . . . O11 O 0.3335(8) 0.2636(10) 0.6292(8) 0.120(6) Uani 1 1 d . . . O12 O 0.2078(9) 0.1905(10) 0.4062(10) 0.156(7) Uani 1 1 d . . . Re1 Re -0.02907(2) 0.74548(4) 0.37403(3) 0.04509(16) Uani 1 1 d . . . Re2 Re 0.25990(3) 0.38386(4) 0.48531(3) 0.05659(19) Uani 1 1 d . . . S1 S -0.0030(2) 0.9278(4) 0.5938(3) 0.0806(12) Uani 1 1 d DU . . S2 S 0.3701(3) 0.4525(5) 0.7465(4) 0.121(2) Uani 1 1 d DU . . S3 S 0.5504(4) 1.0291(7) 0.9075(5) 0.157(3) Uani 1 1 d DU . . 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 0.088(12) 0.057(8) 0.042(7) 0.009(6) 0.008(8) 0.012(8) C2 0.044(8) 0.075(9) 0.045(7) -0.007(6) 0.011(6) 0.016(7) C3 0.064(10) 0.083(11) 0.049(8) -0.012(7) 0.012(8) -0.019(8) C4 0.043(7) 0.049(7) 0.030(5) -0.005(5) 0.006(5) 0.002(6) C5 0.039(7) 0.057(7) 0.038(6) 0.009(5) 0.014(5) 0.009(6) C6 0.058(8) 0.037(6) 0.038(6) -0.002(5) 0.004(6) -0.004(6) C7 0.056(9) 0.052(7) 0.039(6) -0.022(6) 0.010(6) -0.016(6) C8 0.063(9) 0.043(6) 0.037(6) -0.002(5) 0.020(6) -0.002(6) C9 0.038(7) 0.045(6) 0.034(6) -0.011(5) 0.007(5) -0.011(5) C10 0.133(17) 0.052(9) 0.094(13) -0.028(9) 0.045(13) -0.001(10) C11 0.085(13) 0.062(10) 0.112(14) -0.012(10) 0.041(11) 0.028(9) C12 0.088(13) 0.084(11) 0.088(12) 0.003(9) 0.057(11) 0.024(9) C13 0.053(8) 0.030(6) 0.044(6) 0.002(5) 0.020(6) 0.001(5) C14 0.083(10) 0.038(6) 0.044(7) 0.000(5) 0.030(7) -0.008(6) C15 0.087(12) 0.062(8) 0.051(8) 0.008(7) 0.040(8) -0.005(8) C16 0.080(12) 0.070(10) 0.078(11) 0.022(8) 0.041(10) -0.014(9) C17 0.063(10) 0.058(8) 0.060(8) -0.007(7) 0.024(7) -0.013(7) C18 0.050(8) 0.032(6) 0.052(7) 0.003(5) 0.024(6) 0.006(5) C19 0.036(6) 0.043(6) 0.025(5) -0.002(4) 0.004(5) 0.011(5) C20 0.043(6) 0.074(5) 0.029(5) -0.005(5) 0.007(4) 0.000(5) C21 0.045(6) 0.089(4) 0.024(5) 0.004(5) 0.009(4) -0.004(5) C22 0.065(8) 0.129(6) 0.039(6) 0.003(7) 0.025(6) -0.003(7) C23 0.069(8) 0.135(8) 0.056(7) -0.025(7) 0.030(6) 0.000(7) C24 0.052(8) 0.040(6) 0.049(7) 0.005(5) 0.021(6) 0.007(6) C25 0.094(12) 0.052(8) 0.051(8) 0.004(6) 0.032(8) 0.000(8) C26 0.111(14) 0.069(9) 0.054(8) 0.016(7) 0.048(9) 0.006(9) C27 0.103(13) 0.055(8) 0.057(8) 0.010(7) 0.043(9) 0.004(8) C28 0.091(11) 0.042(7) 0.058(8) 0.004(6) 0.038(8) -0.004(7) C29 0.056(8) 0.046(7) 0.041(6) -0.003(5) 0.020(6) -0.001(6) C30 0.039(7) 0.054(7) 0.046(7) 0.004(6) 0.022(6) 0.008(6) C31 0.091(7) 0.046(7) 0.057(6) 0.000(5) 0.043(5) 0.009(6) C33 0.117(8) 0.081(10) 0.068(9) 0.038(8) 0.042(9) 0.027(9) C34 0.118(8) 0.101(12) 0.061(9) 0.024(7) 0.022(8) 0.020(10) C35 0.053(8) 0.050(7) 0.042(7) 0.003(6) 0.008(6) 0.000(6) C36 0.047(7) 0.047(6) 0.022(5) -0.003(5) 0.007(5) 0.000(5) C37 0.047(7) 0.047(7) 0.029(5) -0.003(5) 0.011(5) -0.009(6) C38 0.050(8) 0.052(8) 0.059(8) 0.000(6) 0.009(7) -0.001(6) C39 0.043(7) 0.046(6) 0.030(5) -0.004(5) 0.014(5) 0.001(5) C40 0.050(8) 0.058(8) 0.042(7) -0.017(6) 0.007(6) -0.003(6) C41 0.048(10) 0.062(10) 0.17(2) -0.017(11) -0.016(11) 0.025(8) C42 0.043(8) 0.053(7) 0.048(7) -0.007(6) 0.015(6) 0.007(6) C43 0.047(8) 0.046(7) 0.039(6) -0.010(5) 0.011(6) -0.004(6) C44 0.057(8) 0.055(8) 0.035(6) 0.005(6) 0.008(6) -0.006(6) C45 0.031(8) 0.076(10) 0.088(11) 0.003(8) 0.002(7) 0.003(7) C46 0.042(8) 0.063(8) 0.065(8) -0.011(7) 0.017(7) -0.007(6) C47 0.055(10) 0.052(8) 0.074(10) 0.008(7) 0.012(8) -0.001(7) C48 0.062(11) 0.078(11) 0.079(11) -0.006(9) 0.019(9) -0.009(8) C49 0.112(16) 0.085(12) 0.082(12) -0.001(10) 0.048(12) -0.012(11) C50 0.122(19) 0.134(18) 0.083(14) 0.006(13) 0.052(15) -0.009(15) C51 0.074(14) 0.15(2) 0.110(17) 0.009(15) 0.035(14) 0.007(13) C52 0.067(12) 0.095(13) 0.098(14) -0.007(10) 0.039(11) -0.003(9) C53 0.049(9) 0.064(9) 0.102(13) -0.017(9) 0.024(9) -0.008(7) C54 0.052(8) 0.151(10) 0.103(7) -0.046(6) 0.021(7) -0.030(7) C55 0.046(8) 0.191(10) 0.061(7) -0.062(7) 0.006(7) -0.026(7) C56 0.091(12) 0.215(14) 0.081(7) -0.029(8) 0.007(9) -0.034(10) C57 0.098(12) 0.200(14) 0.117(7) -0.004(8) 0.018(9) -0.045(10) N1 0.039(6) 0.040(5) 0.032(5) 0.000(4) 0.003(4) 0.008(4) N2 0.051(7) 0.043(5) 0.040(5) 0.002(4) 0.015(5) 0.001(5) N3 0.057(7) 0.039(5) 0.049(6) -0.006(4) 0.020(5) 0.005(5) N4 0.048(6) 0.043(5) 0.033(5) -0.001(4) 0.012(5) 0.001(5) N5 0.061(8) 0.049(6) 0.063(7) -0.004(5) 0.020(6) -0.007(6) N6 0.060(9) 0.136(14) 0.085(10) -0.024(9) 0.030(8) -0.011(9) O1 0.054(6) 0.057(5) 0.040(4) 0.009(4) 0.020(4) 0.002(4) O2 0.050(5) 0.050(5) 0.033(4) 0.005(4) 0.008(4) 0.002(4) O3 0.153(13) 0.079(8) 0.063(7) 0.023(6) 0.021(8) 0.039(8) O4 0.050(6) 0.133(10) 0.063(6) 0.002(7) 0.017(5) 0.031(6) O5 0.075(8) 0.134(11) 0.072(7) -0.032(7) 0.015(7) -0.040(8) O6 0.104(8) 0.072(6) 0.045(5) 0.002(5) 0.040(6) 0.009(6) O7 0.070(7) 0.093(7) 0.053(5) 0.036(5) 0.030(5) 0.017(6) O8 0.054(6) 0.044(5) 0.058(5) 0.005(4) 0.021(5) 0.009(4) O9 0.058(6) 0.062(6) 0.045(5) -0.011(4) 0.019(4) 0.005(5) O10 0.147(14) 0.161(14) 0.125(12) 0.028(10) 0.093(11) 0.066(11) O11 0.168(15) 0.090(9) 0.104(10) 0.030(8) 0.051(10) 0.079(10) O12 0.25(2) 0.055(8) 0.169(15) -0.047(9) 0.080(15) -0.030(10) Re1 0.0440(3) 0.0519(3) 0.0325(2) 0.0002(2) 0.0050(2) 0.0022(2) Re2 0.0714(4) 0.0394(3) 0.0628(3) -0.0063(2) 0.0285(3) 0.0120(3) S1 0.074(3) 0.099(3) 0.076(3) -0.019(2) 0.036(2) 0.009(2) S2 0.110(4) 0.131(5) 0.110(4) 0.038(4) 0.023(3) -0.002(4) S3 0.132(6) 0.184(7) 0.139(5) -0.007(5) 0.026(5) -0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O3 1.135(16) . ? C1 Re1 1.895(14) . ? C2 O4 1.111(15) . ? C2 Re1 1.935(14) . ? C3 O5 1.140(16) . ? C3 Re1 1.906(15) . ? C4 O1 1.294(14) . ? C4 C5 1.353(16) . ? C4 C9 1.503(16) . ? C5 O7 1.369(13) . ? C5 C6 1.394(17) . ? C6 O8 1.251(14) . ? C6 C7 1.520(17) . ? C7 O9 1.278(15) . ? C7 C8 1.379(18) . ? C8 C9 1.350(17) . ? C8 O6 1.361(14) . ? C9 O2 1.268(14) . ? C10 O12 1.141(19) . ? C10 Re2 1.899(16) . ? C11 O11 1.19(2) . ? C11 Re2 1.86(2) . ? C12 O10 1.120(18) . ? C12 Re2 1.879(16) . ? C13 C14 1.382(16) . ? C13 C18 1.383(17) . ? C13 N1 1.400(15) . ? C14 C15 1.317(19) . ? C14 H14 0.9300 . ? C15 C16 1.36(2) . ? C15 H15 0.9300 . ? C16 C17 1.422(19) . ? C16 H16 0.9300 . ? C17 C18 1.382(18) . ? C17 H17 0.9300 . ? C18 N4 1.372(14) . ? C19 N1 1.307(13) . ? C19 N4 1.372(15) . ? C19 C20 1.450(15) . ? C20 C21 1.468(14) . ? C20 S1 1.688(11) . ? C21 C22 1.446(14) . ? C21 H21 0.9300 . ? C22 C23 1.388(15) . ? C22 H22 0.9300 . ? C23 S1 1.651(13) . ? C23 H23 0.9300 . ? C24 C25 1.392(17) . ? C24 N2 1.398(14) . ? C24 C29 1.401(16) . ? C25 C26 1.353(19) . ? C25 H25 0.9300 . ? C26 C27 1.38(2) . ? C26 H26 0.9300 . ? C27 C28 1.339(18) . ? C27 H27 0.9300 . ? C28 C29 1.381(17) . ? C28 H28 0.9300 . ? C29 N3 1.381(15) . ? C30 N3 1.329(15) . ? C30 N2 1.344(14) . ? C30 C31 1.515(16) . ? C31 C32 1.522(16) . ? C31 S2 1.669(13) . ? C32 C33 1.480(15) . ? C32 H32 0.9300 . ? C33 C34 1.383(16) . ? C33 H33 0.9300 . ? C34 S2 1.615(14) . ? C34 H34 0.9300 . ? C35 N3 1.482(15) . ? C35 C36 1.490(17) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C44 1.403(17) . ? C36 C37 1.414(17) . ? C37 C39 1.378(16) . ? C37 C38 1.517(17) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C42 1.391(17) . ? C39 C40 1.535(17) . ? C40 N4 1.483(14) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.577(18) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.385(17) . ? C43 C44 1.402(17) . ? C43 C46 1.525(17) . ? C44 C45 1.517(18) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 N5 1.443(16) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 N5 1.374(18) . ? C47 C48 1.39(2) . ? C47 C52 1.41(2) . ? C48 C49 1.32(2) . ? C48 H48 0.9300 . ? C49 C50 1.41(3) . ? C49 H49 0.9300 . ? C50 C51 1.36(3) . ? C50 H50 0.9300 . ? C51 C52 1.37(3) . ? C51 H51 0.9300 . ? C52 N6 1.37(2) . ? C53 N6 1.33(2) . ? C53 N5 1.386(18) . ? C53 C54 1.45(2) . ? C54 C55 1.508(16) . ? C54 S3 1.685(15) . ? C55 C56 1.476(16) . ? C55 H55 0.9300 . ? C56 C57 1.433(18) . ? C56 H56 0.9300 . ? C57 S3 1.686(16) . ? C57 H57 0.9300 . ? N1 Re1 2.218(9) . ? N2 Re2 2.201(10) . ? O1 Re1 2.151(8) . ? O2 Re1 2.142(8) . ? O6 H6 0.8200 . ? O7 H7 0.8200 . ? O8 Re2 2.154(8) . ? O9 Re2 2.129(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 C1 Re1 178.6(15) . . ? O4 C2 Re1 177.2(14) . . ? O5 C3 Re1 177.6(14) . . ? O1 C4 C5 124.2(11) . . ? O1 C4 C9 114.3(10) . . ? C5 C4 C9 121.5(11) . . ? C4 C5 O7 121.8(11) . . ? C4 C5 C6 117.4(11) . . ? O7 C5 C6 120.7(11) . . ? O8 C6 C5 123.0(11) . . ? O8 C6 C7 116.0(12) . . ? C5 C6 C7 120.9(11) . . ? O9 C7 C8 125.9(12) . . ? O9 C7 C6 114.3(12) . . ? C8 C7 C6 119.8(12) . . ? C9 C8 O6 121.1(12) . . ? C9 C8 C7 118.5(11) . . ? O6 C8 C7 120.5(12) . . ? O2 C9 C8 121.8(11) . . ? O2 C9 C4 116.3(10) . . ? C8 C9 C4 121.8(11) . . ? O12 C10 Re2 178(2) . . ? O11 C11 Re2 178.5(18) . . ? O10 C12 Re2 176.6(18) . . ? C14 C13 C18 120.7(11) . . ? C14 C13 N1 130.9(12) . . ? C18 C13 N1 108.3(10) . . ? C15 C14 C13 117.5(13) . . ? C15 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? C14 C15 C16 123.8(13) . . ? C14 C15 H15 118.1 . . ? C16 C15 H15 118.1 . . ? C15 C16 C17 121.2(13) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 114.3(13) . . ? C18 C17 H17 122.9 . . ? C16 C17 H17 122.9 . . ? N4 C18 C17 131.6(12) . . ? N4 C18 C13 105.8(10) . . ? C17 C18 C13 122.5(11) . . ? N1 C19 N4 110.3(10) . . ? N1 C19 C20 127.3(11) . . ? N4 C19 C20 122.3(9) . . ? C19 C20 C21 127.1(10) . . ? C19 C20 S1 119.2(9) . . ? C21 C20 S1 113.4(9) . . ? C22 C21 C20 103.9(12) . . ? C22 C21 H21 128.1 . . ? C20 C21 H21 128.1 . . ? C23 C22 C21 118.1(13) . . ? C23 C22 H22 120.9 . . ? C21 C22 H22 120.9 . . ? C22 C23 S1 109.7(11) . . ? C22 C23 H23 125.1 . . ? S1 C23 H23 125.1 . . ? C25 C24 N2 132.0(12) . . ? C25 C24 C29 119.1(11) . . ? N2 C24 C29 108.9(10) . . ? C26 C25 C24 117.4(13) . . ? C26 C25 H25 121.3 . . ? C24 C25 H25 121.3 . . ? C25 C26 C27 122.2(13) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C28 C27 C26 122.4(14) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C29 116.6(13) . . ? C27 C28 H28 121.7 . . ? C29 C28 H28 121.7 . . ? N3 C29 C28 132.4(11) . . ? N3 C29 C24 105.3(10) . . ? C28 C29 C24 122.3(11) . . ? N3 C30 N2 112.2(10) . . ? N3 C30 C31 124.1(11) . . ? N2 C30 C31 123.6(11) . . ? C30 C31 C32 125.6(11) . . ? C30 C31 S2 118.9(10) . . ? C32 C31 S2 115.5(10) . . ? C33 C32 C31 100.1(13) . . ? C33 C32 H32 130.0 . . ? C31 C32 H32 130.0 . . ? C34 C33 C32 117.6(15) . . ? C34 C33 H33 121.2 . . ? C32 C33 H33 121.2 . . ? C33 C34 S2 112.7(12) . . ? C33 C34 H34 123.6 . . ? S2 C34 H34 123.6 . . ? N3 C35 C36 114.2(9) . . ? N3 C35 H35A 108.7 . . ? C36 C35 H35A 108.7 . . ? N3 C35 H35B 108.7 . . ? C36 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C44 C36 C37 119.2(11) . . ? C44 C36 C35 119.7(11) . . ? C37 C36 C35 121.0(11) . . ? C39 C37 C36 119.5(11) . . ? C39 C37 C38 121.3(11) . . ? C36 C37 C38 119.1(11) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 C42 120.9(11) . . ? C37 C39 C40 119.4(11) . . ? C42 C39 C40 119.6(10) . . ? N4 C40 C39 114.8(10) . . ? N4 C40 H40A 108.6 . . ? C39 C40 H40A 108.6 . . ? N4 C40 H40B 108.6 . . ? C39 C40 H40B 108.6 . . ? H40A C40 H40B 107.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C39 120.5(11) . . ? C43 C42 C41 118.2(12) . . ? C39 C42 C41 121.3(12) . . ? C42 C43 C44 119.4(11) . . ? C42 C43 C46 121.2(11) . . ? C44 C43 C46 119.3(12) . . ? C43 C44 C36 120.3(12) . . ? C43 C44 C45 119.2(12) . . ? C36 C44 C45 120.5(12) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N5 C46 C43 116.6(11) . . ? N5 C46 H46A 108.1 . . ? C43 C46 H46A 108.1 . . ? N5 C46 H46B 108.1 . . ? C43 C46 H46B 108.1 . . ? H46A C46 H46B 107.3 . . ? N5 C47 C48 133.2(15) . . ? N5 C47 C52 105.8(14) . . ? C48 C47 C52 121.0(16) . . ? C49 C48 C47 118.3(17) . . ? C49 C48 H48 120.9 . . ? C47 C48 H48 120.9 . . ? C48 C49 C50 122(2) . . ? C48 C49 H49 119.1 . . ? C50 C49 H49 119.1 . . ? C51 C50 C49 120.4(19) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C52 119(2) . . ? C50 C51 H51 120.3 . . ? C52 C51 H51 120.3 . . ? C51 C52 N6 130.9(18) . . ? C51 C52 C47 119.1(19) . . ? N6 C52 C47 110.0(16) . . ? N6 C53 N5 112.5(15) . . ? N6 C53 C54 123.6(15) . . ? N5 C53 C54 123.9(15) . . ? C53 C54 C55 124.8(14) . . ? C53 C54 S3 117.7(12) . . ? C55 C54 S3 117.2(14) . . ? C56 C55 C54 100.3(18) . . ? C56 C55 H55 129.8 . . ? C54 C55 H55 129.8 . . ? C57 C56 C55 119(2) . . ? C57 C56 H56 120.6 . . ? C55 C56 H56 120.6 . . ? C56 C57 S3 109.8(19) . . ? C56 C57 H57 125.1 . . ? S3 C57 H57 125.1 . . ? C19 N1 C13 107.2(10) . . ? C19 N1 Re1 126.9(8) . . ? C13 N1 Re1 125.9(7) . . ? C30 N2 C24 105.0(10) . . ? C30 N2 Re2 128.7(8) . . ? C24 N2 Re2 126.3(7) . . ? C30 N3 C29 108.5(10) . . ? C30 N3 C35 124.3(10) . . ? C29 N3 C35 127.2(10) . . ? C18 N4 C19 108.2(9) . . ? C18 N4 C40 126.7(11) . . ? C19 N4 C40 125.0(9) . . ? C47 N5 C53 106.3(13) . . ? C47 N5 C46 129.3(12) . . ? C53 N5 C46 124.3(12) . . ? C53 N6 C52 105.3(14) . . ? C4 O1 Re1 116.7(7) . . ? C9 O2 Re1 116.7(7) . . ? C8 O6 H6 109.5 . . ? C5 O7 H7 109.5 . . ? C6 O8 Re2 116.3(8) . . ? C7 O9 Re2 117.3(8) . . ? C1 Re1 C3 87.2(7) . . ? C1 Re1 C2 88.1(6) . . ? C3 Re1 C2 87.0(6) . . ? C1 Re1 O2 98.5(5) . . ? C3 Re1 O2 92.9(5) . . ? C2 Re1 O2 173.4(5) . . ? C1 Re1 O1 172.9(5) . . ? C3 Re1 O1 93.9(5) . . ? C2 Re1 O1 98.9(5) . . ? O2 Re1 O1 74.5(3) . . ? C1 Re1 N1 94.9(5) . . ? C3 Re1 N1 174.0(5) . . ? C2 Re1 N1 98.7(5) . . ? O2 Re1 N1 81.3(3) . . ? O1 Re1 N1 83.4(3) . . ? C11 Re2 C12 87.2(7) . . ? C11 Re2 C10 87.1(8) . . ? C12 Re2 C10 87.3(8) . . ? C11 Re2 O9 174.0(5) . . ? C12 Re2 O9 98.7(6) . . ? C10 Re2 O9 94.5(7) . . ? C11 Re2 O8 99.5(6) . . ? C12 Re2 O8 173.1(6) . . ? C10 Re2 O8 94.4(7) . . ? O9 Re2 O8 74.6(3) . . ? C11 Re2 N2 95.7(6) . . ? C12 Re2 N2 95.7(6) . . ? C10 Re2 N2 176.0(7) . . ? O9 Re2 N2 82.4(3) . . ? O8 Re2 N2 82.4(3) . . ? C23 S1 C20 94.9(7) . . ? C34 S2 C31 94.1(8) . . ? C54 S3 C57 93.2(12) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C4 C5 O7 -3(2) . . . . ? C9 C4 C5 O7 174.9(11) . . . . ? O1 C4 C5 C6 179.4(11) . . . . ? C9 C4 C5 C6 -2.7(18) . . . . ? C4 C5 C6 O8 -179.0(12) . . . . ? O7 C5 C6 O8 3.4(19) . . . . ? C4 C5 C6 C7 0.1(18) . . . . ? O7 C5 C6 C7 -177.5(11) . . . . ? O8 C6 C7 O9 -0.9(15) . . . . ? C5 C6 C7 O9 179.9(11) . . . . ? O8 C6 C7 C8 -177.4(11) . . . . ? C5 C6 C7 C8 3.4(17) . . . . ? O9 C7 C8 C9 179.9(11) . . . . ? C6 C7 C8 C9 -4.0(17) . . . . ? O9 C7 C8 O6 1.1(19) . . . . ? C6 C7 C8 O6 177.2(10) . . . . ? O6 C8 C9 O2 2.8(18) . . . . ? C7 C8 C9 O2 -175.9(11) . . . . ? O6 C8 C9 C4 -179.7(10) . . . . ? C7 C8 C9 C4 1.5(17) . . . . ? O1 C4 C9 O2 -2.3(15) . . . . ? C5 C4 C9 O2 179.6(11) . . . . ? O1 C4 C9 C8 -179.9(11) . . . . ? C5 C4 C9 C8 2.1(17) . . . . ? C18 C13 C14 C15 0.4(19) . . . . ? N1 C13 C14 C15 177.8(12) . . . . ? C13 C14 C15 C16 1(2) . . . . ? C14 C15 C16 C17 -2(3) . . . . ? C15 C16 C17 C18 2(2) . . . . ? C16 C17 C18 N4 -177.0(13) . . . . ? C16 C17 C18 C13 -0.6(19) . . . . ? C14 C13 C18 N4 176.8(11) . . . . ? N1 C13 C18 N4 -1.1(12) . . . . ? C14 C13 C18 C17 -0.4(18) . . . . ? N1 C13 C18 C17 -178.3(11) . . . . ? N1 C19 C20 C21 71.4(17) . . . . ? N4 C19 C20 C21 -113.7(13) . . . . ? N1 C19 C20 S1 -102.1(13) . . . . ? N4 C19 C20 S1 72.9(13) . . . . ? C19 C20 C21 C22 -172.9(12) . . . . ? S1 C20 C21 C22 0.9(12) . . . . ? C20 C21 C22 C23 -0.8(17) . . . . ? C21 C22 C23 S1 0.4(19) . . . . ? N2 C24 C25 C26 -178.5(14) . . . . ? C29 C24 C25 C26 0(2) . . . . ? C24 C25 C26 C27 -1(3) . . . . ? C25 C26 C27 C28 0(3) . . . . ? C26 C27 C28 C29 0(2) . . . . ? C27 C28 C29 N3 179.8(15) . . . . ? C27 C28 C29 C24 0(2) . . . . ? C25 C24 C29 N3 179.9(12) . . . . ? N2 C24 C29 N3 -0.9(14) . . . . ? C25 C24 C29 C28 0(2) . . . . ? N2 C24 C29 C28 179.1(12) . . . . ? N3 C30 C31 C32 108.5(17) . . . . ? N2 C30 C31 C32 -72.8(18) . . . . ? N3 C30 C31 S2 -70.1(15) . . . . ? N2 C30 C31 S2 108.6(13) . . . . ? C30 C31 C32 C33 -179.0(13) . . . . ? S2 C31 C32 C33 -0.3(17) . . . . ? C31 C32 C33 C34 1(2) . . . . ? C32 C33 C34 S2 -1(2) . . . . ? N3 C35 C36 C44 -124.4(12) . . . . ? N3 C35 C36 C37 59.3(15) . . . . ? C44 C36 C37 C39 4.5(16) . . . . ? C35 C36 C37 C39 -179.1(10) . . . . ? C44 C36 C37 C38 -173.9(11) . . . . ? C35 C36 C37 C38 2.4(16) . . . . ? C36 C37 C39 C42 -4.1(16) . . . . ? C38 C37 C39 C42 174.2(11) . . . . ? C36 C37 C39 C40 -179.7(10) . . . . ? C38 C37 C39 C40 -1.3(16) . . . . ? C37 C39 C40 N4 -58.7(15) . . . . ? C42 C39 C40 N4 125.7(12) . . . . ? C37 C39 C42 C43 2.7(17) . . . . ? C40 C39 C42 C43 178.3(11) . . . . ? C37 C39 C42 C41 -175.5(14) . . . . ? C40 C39 C42 C41 0.0(19) . . . . ? C39 C42 C43 C44 -1.6(18) . . . . ? C41 C42 C43 C44 176.7(14) . . . . ? C39 C42 C43 C46 -179.3(11) . . . . ? C41 C42 C43 C46 -1(2) . . . . ? C42 C43 C44 C36 2.1(18) . . . . ? C46 C43 C44 C36 179.8(11) . . . . ? C42 C43 C44 C45 -176.1(12) . . . . ? C46 C43 C44 C45 1.7(18) . . . . ? C37 C36 C44 C43 -3.5(17) . . . . ? C35 C36 C44 C43 -179.9(10) . . . . ? C37 C36 C44 C45 174.6(11) . . . . ? C35 C36 C44 C45 -1.8(17) . . . . ? C42 C43 C46 N5 -123.1(13) . . . . ? C44 C43 C46 N5 59.2(17) . . . . ? N5 C47 C48 C49 179.4(16) . . . . ? C52 C47 C48 C49 -1(2) . . . . ? C47 C48 C49 C50 1(3) . . . . ? C48 C49 C50 C51 1(3) . . . . ? C49 C50 C51 C52 -2(4) . . . . ? C50 C51 C52 N6 -175(2) . . . . ? C50 C51 C52 C47 2(3) . . . . ? N5 C47 C52 C51 179.6(17) . . . . ? C48 C47 C52 C51 0(3) . . . . ? N5 C47 C52 N6 -2.8(19) . . . . ? C48 C47 C52 N6 177.5(15) . . . . ? N6 C53 C54 C55 105(2) . . . . ? N5 C53 C54 C55 -77(2) . . . . ? N6 C53 C54 S3 -69(2) . . . . ? N5 C53 C54 S3 108.6(16) . . . . ? C53 C54 C55 C56 176.1(17) . . . . ? S3 C54 C55 C56 -9.4(19) . . . . ? C54 C55 C56 C57 6(3) . . . . ? C55 C56 C57 S3 -1(3) . . . . ? N4 C19 N1 C13 -3.0(12) . . . . ? C20 C19 N1 C13 172.4(11) . . . . ? N4 C19 N1 Re1 178.9(7) . . . . ? C20 C19 N1 Re1 -5.6(16) . . . . ? C14 C13 N1 C19 -175.1(12) . . . . ? C18 C13 N1 C19 2.6(12) . . . . ? C14 C13 N1 Re1 3.0(17) . . . . ? C18 C13 N1 Re1 -179.3(7) . . . . ? N3 C30 N2 C24 2.4(14) . . . . ? C31 C30 N2 C24 -176.5(11) . . . . ? N3 C30 N2 Re2 -179.4(8) . . . . ? C31 C30 N2 Re2 1.7(17) . . . . ? C25 C24 N2 C30 178.2(15) . . . . ? C29 C24 N2 C30 -0.8(14) . . . . ? C25 C24 N2 Re2 0(2) . . . . ? C29 C24 N2 Re2 -179.1(8) . . . . ? N2 C30 N3 C29 -3.1(14) . . . . ? C31 C30 N3 C29 175.8(11) . . . . ? N2 C30 N3 C35 179.0(11) . . . . ? C31 C30 N3 C35 -2.1(19) . . . . ? C28 C29 N3 C30 -177.7(15) . . . . ? C24 C29 N3 C30 2.4(14) . . . . ? C28 C29 N3 C35 0(2) . . . . ? C24 C29 N3 C35 -179.8(12) . . . . ? C36 C35 N3 C30 -139.6(12) . . . . ? C36 C35 N3 C29 42.9(18) . . . . ? C17 C18 N4 C19 176.2(13) . . . . ? C13 C18 N4 C19 -0.7(12) . . . . ? C17 C18 N4 C40 -1(2) . . . . ? C13 C18 N4 C40 -178.3(11) . . . . ? N1 C19 N4 C18 2.4(12) . . . . ? C20 C19 N4 C18 -173.4(10) . . . . ? N1 C19 N4 C40 -180.0(10) . . . . ? C20 C19 N4 C40 4.3(17) . . . . ? C39 C40 N4 C18 -45.8(16) . . . . ? C39 C40 N4 C19 137.0(11) . . . . ? C48 C47 N5 C53 -176.8(16) . . . . ? C52 C47 N5 C53 3.6(16) . . . . ? C48 C47 N5 C46 2(3) . . . . ? C52 C47 N5 C46 -177.9(14) . . . . ? N6 C53 N5 C47 -3.4(17) . . . . ? C54 C53 N5 C47 178.8(14) . . . . ? N6 C53 N5 C46 178.0(13) . . . . ? C54 C53 N5 C46 0(2) . . . . ? C43 C46 N5 C47 42(2) . . . . ? C43 C46 N5 C53 -139.8(13) . . . . ? N5 C53 N6 C52 1.6(19) . . . . ? C54 C53 N6 C52 179.4(16) . . . . ? C51 C52 N6 C53 178(2) . . . . ? C47 C52 N6 C53 1(2) . . . . ? C5 C4 O1 Re1 170.7(10) . . . . ? C9 C4 O1 Re1 -7.3(12) . . . . ? C8 C9 O2 Re1 -171.7(9) . . . . ? C4 C9 O2 Re1 10.8(12) . . . . ? C5 C6 O8 Re2 -171.2(9) . . . . ? C7 C6 O8 Re2 9.7(13) . . . . ? C8 C7 O9 Re2 167.8(9) . . . . ? C6 C7 O9 Re2 -8.5(13) . . . . ? O3 C1 Re1 C3 -81(72) . . . . ? O3 C1 Re1 C2 -168(72) . . . . ? O3 C1 Re1 O2 11(72) . . . . ? O3 C1 Re1 O1 17(75) . . . . ? O3 C1 Re1 N1 93(72) . . . . ? O5 C3 Re1 C1 47(40) . . . . ? O5 C3 Re1 C2 135(40) . . . . ? O5 C3 Re1 O2 -51(40) . . . . ? O5 C3 Re1 O1 -126(40) . . . . ? O5 C3 Re1 N1 -63(42) . . . . ? O4 C2 Re1 C1 125(25) . . . . ? O4 C2 Re1 C3 38(25) . . . . ? O4 C2 Re1 O2 -51(27) . . . . ? O4 C2 Re1 O1 -55(25) . . . . ? O4 C2 Re1 N1 -140(25) . . . . ? C9 O2 Re1 C1 168.3(9) . . . . ? C9 O2 Re1 C3 -104.1(9) . . . . ? C9 O2 Re1 C2 -16(4) . . . . ? C9 O2 Re1 O1 -10.9(7) . . . . ? C9 O2 Re1 N1 74.6(8) . . . . ? C4 O1 Re1 C1 3(4) . . . . ? C4 O1 Re1 C3 101.5(9) . . . . ? C4 O1 Re1 C2 -171.0(9) . . . . ? C4 O1 Re1 O2 9.6(8) . . . . ? C4 O1 Re1 N1 -73.2(8) . . . . ? C19 N1 Re1 C1 121.8(10) . . . . ? C13 N1 Re1 C1 -55.9(10) . . . . ? C19 N1 Re1 C3 -128(5) . . . . ? C13 N1 Re1 C3 54(5) . . . . ? C19 N1 Re1 C2 33.0(10) . . . . ? C13 N1 Re1 C2 -144.7(9) . . . . ? C19 N1 Re1 O2 -140.3(9) . . . . ? C13 N1 Re1 O2 42.0(8) . . . . ? C19 N1 Re1 O1 -65.1(9) . . . . ? C13 N1 Re1 O1 117.2(9) . . . . ? O11 C11 Re2 C12 -91(65) . . . . ? O11 C11 Re2 C10 -4(65) . . . . ? O11 C11 Re2 O9 103(63) . . . . ? O11 C11 Re2 O8 90(65) . . . . ? O11 C11 Re2 N2 174(100) . . . . ? O10 C12 Re2 C11 147(29) . . . . ? O10 C12 Re2 C10 60(29) . . . . ? O10 C12 Re2 O9 -34(29) . . . . ? O10 C12 Re2 O8 -44(32) . . . . ? O10 C12 Re2 N2 -117(29) . . . . ? O12 C10 Re2 C11 128(43) . . . . ? O12 C10 Re2 C12 -144(43) . . . . ? O12 C10 Re2 O9 -46(43) . . . . ? O12 C10 Re2 O8 29(43) . . . . ? O12 C10 Re2 N2 -7(51) . . . . ? C7 O9 Re2 C11 -3(6) . . . . ? C7 O9 Re2 C12 -168.6(10) . . . . ? C7 O9 Re2 C10 103.5(10) . . . . ? C7 O9 Re2 O8 10.1(8) . . . . ? C7 O9 Re2 N2 -74.0(8) . . . . ? C6 O8 Re2 C11 168.1(10) . . . . ? C6 O8 Re2 C12 0(5) . . . . ? C6 O8 Re2 C10 -104.1(10) . . . . ? C6 O8 Re2 O9 -10.6(8) . . . . ? C6 O8 Re2 N2 73.5(8) . . . . ? C30 N2 Re2 C11 -32.4(12) . . . . ? C24 N2 Re2 C11 145.5(11) . . . . ? C30 N2 Re2 C12 -120.1(11) . . . . ? C24 N2 Re2 C12 57.8(11) . . . . ? C30 N2 Re2 C10 103(9) . . . . ? C24 N2 Re2 C10 -79(9) . . . . ? C30 N2 Re2 O9 141.9(11) . . . . ? C24 N2 Re2 O9 -40.2(10) . . . . ? C30 N2 Re2 O8 66.5(10) . . . . ? C24 N2 Re2 O8 -115.6(10) . . . . ? C22 C23 S1 C20 0.1(13) . . . . ? C19 C20 S1 C23 173.7(10) . . . . ? C21 C20 S1 C23 -0.6(11) . . . . ? C33 C34 S2 C31 0.9(16) . . . . ? C30 C31 S2 C34 178.5(11) . . . . ? C32 C31 S2 C34 -0.3(14) . . . . ? C53 C54 S3 C57 -176.6(16) . . . . ? C55 C54 S3 C57 8.6(17) . . . . ? C56 C57 S3 C54 -4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 4.856 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.190 _iucr_refine_instructions_details ; TITL rk5 83 in P2(1)/c CELL 0.71073 23.3463 13.6127 18.1764 90.000 110.725 90.000 ZERR 4.00 0.0026 0.0009 0.0016 0.000 0.012 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C 2.31000 20.84392 1.02000 10.20751 1.58860 0.56870 = 0.86500 51.65125 0.21560 0.003 0.002 11.500 0.770 12.011 SFAC H 0.49300 10.51091 0.32291 26.12573 0.14019 3.14236 = 0.04081 57.79977 0.00304 0.000 0.000 0.620 0.320 1.008 SFAC N 12.21261 0.00570 3.13220 9.89331 2.01250 28.99754 = 1.16630 0.58260 -11.52901 0.006 0.003 19.600 0.700 14.007 SFAC O 3.04850 13.27711 2.28680 5.70111 1.54630 0.32390 = 0.86700 32.90894 0.25080 0.011 0.006 32.500 0.660 15.999 SFAC RE 28.76213 1.67191 15.71892 9.09228 14.55641 0.35050 = 5.44174 52.08615 10.47201 -1.018 7.231 30100.000 1.370 186.207 SFAC S 6.90531 1.46790 5.20341 22.21512 1.43790 0.25360 = 1.58630 56.17207 0.86690 0.125 0.123 532.000 1.040 32.066 UNIT 228 152 24 48 8 12 MERG 2 FMAP 2 PLAN 25 ACTA 50.0 CONF simu 0.02 c54 c55 c56 c57 s3 delu 0.004 c54 c55 c56 c57 s3 simu 0.02 c20 c21 c22 c23 s1 delu 0.004 c20 c21 c22 c23 s1 simu 0.04 c34 c33 c32 c31 s2 delu 0.004 c34 c33 c32 c31 s2 dfix 1.67 s3 c54 s3 c57 s1 c20 s1 c23 s2 c34 s2 c31 dfix 1.46 c23 c22 c22 c21 c21 c20 dfix 1.46 c31 c32 c32 c33 c33 c34 dfix 1.46 c57 c56 c56 c55 c55 c54 BOND $H L.S. 10 WGHT 0.082100 40.012196 FVAR 0.62699 C1 1 -0.058675 0.847818 0.299469 11.00000 0.08849 0.05730 = 0.04163 0.00870 0.00782 0.01171 C2 1 -0.084879 0.790671 0.424138 11.00000 0.04352 0.07487 = 0.04532 -0.00717 0.01097 0.01610 C3 1 -0.094908 0.667296 0.307886 11.00000 0.06420 0.08261 = 0.04903 -0.01231 0.01232 -0.01868 C4 1 0.059559 0.584665 0.442487 11.00000 0.04257 0.04853 = 0.03032 -0.00538 0.00563 0.00223 C5 1 0.095930 0.517873 0.492592 11.00000 0.03886 0.05671 = 0.03797 0.00873 0.01389 0.00868 C6 1 0.144567 0.479456 0.474164 11.00000 0.05767 0.03734 = 0.03847 -0.00155 0.00359 -0.00415 C7 1 0.155964 0.511968 0.400535 11.00000 0.05569 0.05197 = 0.03937 -0.02217 0.00981 -0.01613 C8 1 0.119812 0.584110 0.353318 11.00000 0.06254 0.04311 = 0.03663 -0.00197 0.01994 -0.00246 C9 1 0.072542 0.619737 0.371540 11.00000 0.03814 0.04530 = 0.03354 -0.01088 0.00732 -0.01054 C10 1 0.228683 0.262218 0.436285 11.00000 0.13275 0.05245 = 0.09433 -0.02831 0.04548 -0.00070 C11 1 0.305197 0.311563 0.573632 11.00000 0.08504 0.06181 = 0.11178 -0.01205 0.04084 0.02751 C12 1 0.325357 0.366671 0.449224 11.00000 0.08784 0.08402 = 0.08833 0.00333 0.05695 0.02366 C13 1 0.098625 0.866301 0.421130 11.00000 0.05323 0.02993 = 0.04419 0.00189 0.01978 0.00066 C14 1 0.102038 0.870346 0.346823 11.00000 0.08330 0.03795 = 0.04443 0.00018 0.02970 -0.00844 AFIX 43 H14 2 0.072078 0.841750 0.303814 11.00000 -1.20000 AFIX 0 C15 1 0.149281 0.916186 0.339172 11.00000 0.08729 0.06151 = 0.05082 0.00827 0.04018 -0.00513 AFIX 43 H15 2 0.151735 0.919836 0.289280 11.00000 -1.20000 AFIX 0 C16 1 0.194630 0.958443 0.399949 11.00000 0.07978 0.07017 = 0.07797 0.02209 0.04118 -0.01440 AFIX 43 H16 2 0.227302 0.988195 0.390699 11.00000 -1.20000 AFIX 0 C17 1 0.193100 0.958056 0.477441 11.00000 0.06320 0.05794 = 0.06008 -0.00694 0.02444 -0.01261 AFIX 43 H17 2 0.223075 0.987846 0.519761 11.00000 -1.20000 AFIX 0 C18 1 0.143286 0.909653 0.484538 11.00000 0.05039 0.03235 = 0.05236 0.00340 0.02437 0.00630 C19 1 0.069667 0.848134 0.521885 11.00000 0.03585 0.04300 = 0.02475 -0.00157 0.00443 0.01071 C20 1 0.034112 0.832092 0.572040 11.00000 0.04342 0.07414 = 0.02894 -0.00456 0.00714 0.00043 C21 1 0.020880 0.737657 0.601618 11.00000 0.04495 0.08898 = 0.02440 0.00404 0.00887 -0.00447 AFIX 43 H21 2 0.036519 0.676057 0.597036 11.00000 -1.20000 AFIX 0 C22 1 -0.022133 0.762751 0.639531 11.00000 0.06467 0.12935 = 0.03929 0.00284 0.02543 -0.00326 AFIX 43 H22 2 -0.038306 0.714667 0.662898 11.00000 -1.20000 AFIX 0 C23 1 -0.038610 0.860637 0.640070 11.00000 0.06851 0.13518 = 0.05553 -0.02457 0.02971 -0.00031 AFIX 43 H23 2 -0.065609 0.884754 0.663008 11.00000 -1.20000 AFIX 0 C24 1 0.299260 0.612627 0.500368 11.00000 0.05151 0.04021 = 0.04855 0.00497 0.02126 0.00723 C25 1 0.293827 0.629378 0.422606 11.00000 0.09354 0.05178 = 0.05115 0.00442 0.03173 -0.00032 AFIX 43 H25 2 0.280781 0.580146 0.384852 11.00000 -1.20000 AFIX 0 C26 1 0.308263 0.720043 0.404106 11.00000 0.11114 0.06908 = 0.05413 0.01575 0.04793 0.00646 AFIX 43 H26 2 0.305348 0.732724 0.352627 11.00000 -1.20000 AFIX 0 C27 1 0.327176 0.794347 0.459107 11.00000 0.10338 0.05452 = 0.05663 0.01046 0.04258 0.00420 AFIX 43 H27 2 0.336373 0.855497 0.443327 11.00000 -1.20000 AFIX 0 C28 1 0.332752 0.781537 0.534347 11.00000 0.09127 0.04179 = 0.05799 0.00364 0.03777 -0.00385 AFIX 43 H28 2 0.345459 0.832124 0.570938 11.00000 -1.20000 AFIX 0 C29 1 0.318682 0.689403 0.554893 11.00000 0.05604 0.04627 = 0.04095 -0.00256 0.01977 -0.00135 C30 1 0.303831 0.556212 0.614251 11.00000 0.03943 0.05371 = 0.04628 0.00443 0.02168 0.00840 C31 1 0.303450 0.486704 0.679202 11.00000 0.09062 0.04644 = 0.05713 0.00017 0.04275 0.00883 C32 1 0.246549 0.445390 0.690518 11.00000 10.09994 AFIX 43 H32 2 0.205379 0.454811 0.660761 11.00000 -1.20000 AFIX 0 C33 1 0.275390 0.385949 0.762365 11.00000 0.11669 0.08078 = 0.06760 0.03789 0.04191 0.02677 AFIX 43 H33 2 0.251833 0.349527 0.784414 11.00000 -1.20000 AFIX 0 C34 1 0.338616 0.386514 0.795529 11.00000 0.11812 0.10144 = 0.06120 0.02357 0.02153 0.02005 AFIX 43 H34 2 0.360632 0.352532 0.841182 11.00000 -1.20000 AFIX 0 C35 1 0.336322 0.701491 0.702100 11.00000 0.05283 0.05014 = 0.04242 0.00288 0.00765 -0.00028 AFIX 23 H35A 2 0.380624 0.704751 0.725332 11.00000 -1.20000 H35B 2 0.321940 0.662813 0.736919 11.00000 -1.20000 AFIX 0 C36 1 0.311164 0.802817 0.697272 11.00000 0.04664 0.04668 = 0.02238 -0.00279 0.00728 0.00008 C37 1 0.247327 0.819922 0.666548 11.00000 0.04728 0.04669 = 0.02853 -0.00319 0.01135 -0.00862 C38 1 0.204095 0.733048 0.641259 11.00000 0.04983 0.05161 = 0.05938 0.00013 0.00943 -0.00110 AFIX 137 H38A 2 0.223052 0.676158 0.671220 11.00000 -1.50000 H38B 2 0.195008 0.720415 0.586327 11.00000 -1.50000 H38C 2 0.166860 0.747582 0.650222 11.00000 -1.50000 AFIX 0 C39 1 0.225555 0.914705 0.661930 11.00000 0.04300 0.04602 = 0.03047 -0.00446 0.01377 0.00093 C40 1 0.156183 0.932925 0.628908 11.00000 0.04956 0.05817 = 0.04223 -0.01695 0.00711 -0.00332 AFIX 23 H40A 2 0.137990 0.901305 0.663177 11.00000 -1.20000 H40B 2 0.148933 1.002964 0.630157 11.00000 -1.20000 AFIX 0 C41 1 0.240464 1.100662 0.692253 11.00000 0.04831 0.06159 = 0.17047 -0.01713 -0.01556 0.02451 AFIX 137 H41A 2 0.209863 1.100367 0.716265 11.00000 -1.50000 H41B 2 0.222790 1.124309 0.639219 11.00000 -1.50000 H41C 2 0.273634 1.142833 0.721622 11.00000 -1.50000 AFIX 0 C42 1 0.265276 0.993040 0.691684 11.00000 0.04294 0.05331 = 0.04807 -0.00677 0.01516 0.00727 C43 1 0.327907 0.977734 0.723657 11.00000 0.04685 0.04590 = 0.03936 -0.00957 0.01113 -0.00368 C44 1 0.350977 0.882018 0.727682 11.00000 0.05688 0.05532 = 0.03531 0.00492 0.00783 -0.00629 C45 1 0.419245 0.864840 0.767517 11.00000 0.03129 0.07627 = 0.08805 0.00302 0.00197 0.00344 AFIX 137 H45A 2 0.426128 0.799869 0.789448 11.00000 -1.50000 H45B 2 0.435788 0.912242 0.808716 11.00000 -1.50000 H45C 2 0.439010 0.871541 0.729592 11.00000 -1.50000 AFIX 0 C46 1 0.372080 1.062546 0.757338 11.00000 0.04163 0.06263 = 0.06492 -0.01124 0.01702 -0.00738 AFIX 23 H46A 2 0.348328 1.122522 0.750566 11.00000 -1.20000 H46B 2 0.391861 1.051863 0.813437 11.00000 -1.20000 AFIX 0 C47 1 0.415024 1.074232 0.646874 11.00000 0.05549 0.05205 = 0.07448 0.00827 0.01176 -0.00105 C48 1 0.366601 1.057858 0.576453 11.00000 0.06186 0.07816 = 0.07906 -0.00556 0.01906 -0.00914 AFIX 43 H48 2 0.327299 1.045681 0.576069 11.00000 -1.20000 AFIX 0 C49 1 0.377949 1.060074 0.510373 11.00000 0.11202 0.08502 = 0.08186 -0.00072 0.04770 -0.01195 AFIX 43 H49 2 0.345930 1.049770 0.462974 11.00000 -1.20000 AFIX 0 C50 1 0.437165 1.077597 0.509516 11.00000 0.12230 0.13431 = 0.08341 0.00605 0.05188 -0.00940 AFIX 43 H50 2 0.443546 1.079844 0.461857 11.00000 -1.20000 AFIX 0 C51 1 0.485101 1.091260 0.578062 11.00000 0.07450 0.14662 = 0.10998 0.00866 0.03533 0.00740 AFIX 43 H51 2 0.524425 1.100583 0.577568 11.00000 -1.20000 AFIX 0 C52 1 0.474901 1.091154 0.647750 11.00000 0.06691 0.09458 = 0.09820 -0.00671 0.03931 -0.00313 C53 1 0.479270 1.102371 0.767552 11.00000 0.04935 0.06366 = 0.10189 -0.01660 0.02356 -0.00810 C54 1 0.502616 1.115539 0.852434 11.00000 0.05220 0.15150 = 0.10342 -0.04554 0.02144 -0.02975 C55 1 0.491710 1.205060 0.894570 11.00000 0.04648 0.19127 = 0.06098 -0.06206 0.00639 -0.02582 AFIX 43 H55 2 0.471701 1.263481 0.874259 11.00000 -1.20000 AFIX 0 C56 1 0.521733 1.173855 0.977124 11.00000 0.09060 0.21547 = 0.08072 -0.02870 0.00661 -0.03405 AFIX 43 H56 2 0.519179 1.212395 1.018098 11.00000 -1.20000 AFIX 0 C57 1 0.554888 1.083023 0.992897 11.00000 0.09846 0.20037 = 0.11674 -0.00403 0.01780 -0.04518 AFIX 43 H57 2 0.575747 1.057625 1.042729 11.00000 -1.20000 AFIX 0 N1 3 0.054034 0.826282 0.447344 11.00000 0.03857 0.04030 = 0.03220 0.00034 0.00260 0.00755 N2 3 0.289523 0.528845 0.538836 11.00000 0.05127 0.04259 = 0.03981 0.00174 0.01529 0.00122 N3 3 0.319296 0.650469 0.625307 11.00000 0.05726 0.03938 = 0.04861 -0.00642 0.01981 0.00484 N4 3 0.124613 0.896985 0.547500 11.00000 0.04778 0.04303 = 0.03281 -0.00130 0.01219 0.00084 N5 3 0.419140 1.077805 0.724141 11.00000 0.06138 0.04898 = 0.06262 -0.00440 0.02008 -0.00721 N6 3 0.513802 1.109226 0.723354 11.00000 0.05991 0.13601 = 0.08471 -0.02427 0.02954 -0.01070 O1 4 0.012585 0.625773 0.451750 11.00000 0.05367 0.05661 = 0.03993 0.00909 0.01961 0.00163 O2 4 0.035363 0.681980 0.328257 11.00000 0.04990 0.05010 = 0.03262 0.00466 0.00850 0.00154 O3 4 -0.075800 0.908240 0.253865 11.00000 0.15284 0.07905 = 0.06278 0.02320 0.02081 0.03917 O4 4 -0.117854 0.812935 0.452614 11.00000 0.05044 0.13327 = 0.06305 0.00191 0.01699 0.03055 O5 4 -0.133787 0.621542 0.266142 11.00000 0.07463 0.13409 = 0.07191 -0.03186 0.01536 -0.03956 O6 4 0.131069 0.616947 0.289026 11.00000 0.10407 0.07180 = 0.04484 0.00217 0.04037 0.00915 AFIX 83 H6 2 0.105750 0.658938 0.266512 11.00000 -1.50000 AFIX 0 O7 4 0.087171 0.491216 0.560464 11.00000 0.07047 0.09276 = 0.05259 0.03611 0.03036 0.01680 AFIX 83 H7 2 0.112806 0.450068 0.583826 11.00000 -1.50000 AFIX 0 O8 4 0.180652 0.416329 0.515564 11.00000 0.05448 0.04392 = 0.05812 0.00485 0.02134 0.00888 O9 4 0.202067 0.470974 0.390957 11.00000 0.05813 0.06242 = 0.04454 -0.01147 0.01880 0.00450 O10 4 0.362356 0.356388 0.424102 11.00000 0.14745 0.16150 = 0.12513 0.02789 0.09302 0.06615 O11 4 0.333493 0.263572 0.629159 11.00000 0.16818 0.09041 = 0.10352 0.03043 0.05131 0.07936 O12 4 0.207847 0.190463 0.406153 11.00000 0.24754 0.05534 = 0.16946 -0.04664 0.07978 -0.03048 RE1 5 -0.029070 0.745483 0.374026 11.00000 0.04395 0.05191 = 0.03253 0.00024 0.00503 0.00216 RE2 5 0.259897 0.383858 0.485312 11.00000 0.07140 0.03941 = 0.06277 -0.00634 0.02846 0.01198 S1 6 -0.003035 0.927793 0.593837 11.00000 0.07441 0.09907 = 0.07558 -0.01933 0.03565 0.00889 S2 6 0.370104 0.452529 0.746454 11.00000 0.11012 0.13145 = 0.11006 0.03758 0.02346 -0.00213 S3 6 0.550395 1.029118 0.907513 11.00000 0.13204 0.18356 = 0.13867 -0.00662 0.02585 -0.00585 HKLF 4 REM rk5 83 in P2(1)/c REM R1 = 0.1023 for 8954 Fo > 4sig(Fo) and 0.1563 for all 13288 data REM 718 parameters refined using 131 restraints END WGHT 0.0812 40.7977 REM Highest difference peak 4.856, deepest hole -1.215, 1-sigma level 0.190 Q1 1 0.0077 0.7228 0.3728 11.00000 0.05 2.70 Q2 1 0.0004 0.7903 0.3683 11.00000 0.05 2.47 Q3 1 -0.0188 0.7516 0.3293 11.00000 0.05 1.80 Q4 1 0.2371 0.3378 0.4683 11.00000 0.05 1.65 Q5 1 0.2529 0.3849 0.5290 11.00000 0.05 1.60 Q6 1 0.2269 0.4240 0.4824 11.00000 0.05 1.51 Q7 1 0.3020 0.3688 0.4887 11.00000 0.05 1.43 Q8 1 0.2876 0.3778 0.5317 11.00000 0.05 1.40 Q9 1 -0.0354 0.7424 0.4215 11.00000 0.05 1.30 Q10 1 0.2693 0.3841 0.4370 11.00000 0.05 1.20 Q11 1 -0.0710 0.7812 0.3807 11.00000 0.05 1.20 Q12 1 -0.0615 0.7136 0.3283 11.00000 0.05 1.01 Q13 1 -0.0705 0.6938 0.3702 11.00000 0.05 0.98 Q14 1 0.2473 1.0464 0.6968 11.00000 0.05 0.82 Q15 1 -0.0609 0.7816 0.3295 11.00000 0.05 0.80 Q16 1 -0.0218 0.8114 0.6618 11.00000 0.05 0.76 Q17 1 0.4698 1.1666 0.8938 11.00000 0.05 0.76 Q18 1 0.1878 0.9493 0.4413 11.00000 0.05 0.74 Q19 1 0.2687 0.6411 0.4896 11.00000 0.05 0.63 Q20 1 0.2582 0.1467 0.4604 11.00000 0.05 0.59 Q21 1 0.2488 1.0866 0.4965 11.00000 0.05 0.59 Q22 1 0.1816 0.5309 0.4354 11.00000 0.05 0.59 Q23 1 0.3371 0.4107 0.7899 11.00000 0.05 0.58 Q24 1 0.3010 1.1175 0.4990 11.00000 0.05 0.57 Q25 1 0.5206 1.1031 0.9297 11.00000 0.05 0.57 ; _database_code_depnum_ccdc_archive 'CCDC 935810' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H38 N6 O12 Re2 S3' _chemical_formula_sum 'C48 H38 N6 O12 Re2 S3' _chemical_formula_weight 1359.42 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8639(2) _cell_length_b 21.2643(4) _cell_length_c 21.5350(4) _cell_angle_alpha 107.672(2) _cell_angle_beta 90.2800(10) _cell_angle_gamma 100.230(2) _cell_volume 5512.64(17) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 20613 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 27.96 _exptl_crystal_description prism _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 4.563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.34 _exptl_absorpt_correction_T_max 0.64 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur Sapphire3' _diffrn_measurement_method 'w scan' _diffrn_detector_area_resol_mean 15.9853 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 85834 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_unetI/netI 0.0530 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.96 _reflns_number_total 26285 _reflns_number_gt 18702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_data_reduction 'CrysAlis PRO (Oxford Diffraction, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+14.5548P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26285 _refine_ls_number_parameters 1291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1723 _refine_ls_wR_factor_gt 0.1580 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re3 Re -0.21306(2) 0.722500(19) 0.081350(15) 0.04130(10) Uani 1 1 d . . . Re4 Re 0.30966(3) 0.62706(2) -0.102165(16) 0.05363(12) Uani 1 1 d . . . S1 S 0.28440(19) 0.51732(13) -0.00092(11) 0.0559(6) Uani 1 1 d . . . S2 S -0.16282(16) 0.60645(12) 0.16800(11) 0.0463(5) Uani 1 1 d . . . S6 S 0.4274(3) 0.8411(2) 0.35110(19) 0.0997(11) Uani 1 1 d . . . O12 O -0.2825(6) 0.8533(4) 0.1565(4) 0.077(2) Uani 1 1 d . . . O13 O -0.3998(5) 0.6457(4) 0.1315(3) 0.0596(17) Uani 1 1 d . . . O14 O -0.1450(4) 0.6375(3) 0.0287(3) 0.0473(14) Uani 1 1 d . . . O15 O -0.0785(4) 0.7629(3) 0.0380(3) 0.0484(14) Uani 1 1 d . . . O16 O 0.2250(4) 0.7076(3) -0.0675(3) 0.0555(16) Uani 1 1 d . . . O17 O 0.1589(4) 0.5821(3) -0.0782(3) 0.0560(16) Uani 1 1 d . . . O18 O 0.1112(5) 0.8075(3) -0.0133(3) 0.0593(17) Uani 1 1 d . . . H18 H 0.0693 0.8309 0.0052 0.089 Uiso 1 1 d R . . O19 O -0.0368(5) 0.5360(4) -0.0349(4) 0.072(2) Uani 1 1 d . . . H19 H 0.0047 0.5132 -0.0548 0.108 Uiso 1 1 d R . . O20 O 0.5046(6) 0.7165(5) -0.1334(4) 0.093(3) Uani 1 1 d . . . O21 O 0.4250(7) 0.5088(5) -0.1458(4) 0.097(3) Uani 1 1 d . . . O22 O -0.3772(7) 0.7062(6) -0.0265(4) 0.121(4) Uani 1 1 d . . . O24 O 0.2477(8) 0.5972(8) -0.2456(4) 0.161(6) Uani 1 1 d . . . N5 N -0.0915(5) 0.7310(3) 0.1578(3) 0.0399(15) Uani 1 1 d . . . N6 N 0.0031(5) 0.7075(3) 0.2314(3) 0.0371(14) Uani 1 1 d . . . N7 N 0.3456(5) 0.6458(4) 0.0031(3) 0.0507(18) Uani 1 1 d . . . N8 N 0.3586(5) 0.6339(4) 0.1010(3) 0.0417(15) Uani 1 1 d . . . N9 N 0.3849(5) 0.7751(4) 0.4397(3) 0.0475(17) Uani 1 1 d . . . N12 N 0.3863(8) 0.8859(5) 0.4764(6) 0.090(3) Uani 1 1 d . . . C34 C -0.3119(7) 0.7143(7) 0.0129(5) 0.071(3) Uani 1 1 d . . . C35 C -0.2558(7) 0.8039(5) 0.1283(5) 0.051(2) Uani 1 1 d . . . C36 C -0.3283(7) 0.6753(5) 0.1153(4) 0.047(2) Uani 1 1 d . . . C37 C 0.2673(9) 0.6081(8) -0.1924(6) 0.090(4) Uani 1 1 d . . . C38 C 0.3813(8) 0.5528(7) -0.1286(5) 0.073(3) Uani 1 1 d . . . C39 C 0.4349(8) 0.6814(7) -0.1198(5) 0.067(3) Uani 1 1 d . . . C40 C 0.1367(6) 0.6946(5) -0.0433(4) 0.045(2) Uani 1 1 d . . . C41 C 0.0989(6) 0.6220(5) -0.0499(4) 0.050(2) Uani 1 1 d . . . C42 C 0.0022(6) 0.6010(5) -0.0258(4) 0.049(2) Uani 1 1 d . . . C43 C -0.0540(6) 0.6512(5) 0.0058(4) 0.046(2) Uani 1 1 d . . . C44 C -0.0169(6) 0.7225(4) 0.0101(4) 0.0430(19) Uani 1 1 d . . . C45 C 0.0753(6) 0.7426(5) -0.0152(4) 0.0434(19) Uani 1 1 d . . . C46 C -0.0077(5) 0.7852(4) 0.1844(4) 0.0378(17) Uani 1 1 d . . . C47 C 0.0200(7) 0.8455(4) 0.1708(4) 0.048(2) Uani 1 1 d . . . H47 H -0.0197 0.8561 0.1404 0.057 Uiso 1 1 calc R . . C48 C 0.1100(8) 0.8896(5) 0.2047(5) 0.061(3) Uani 1 1 d . . . H48 H 0.1312 0.9305 0.1970 0.073 Uiso 1 1 calc R . . C49 C 0.1686(8) 0.8733(5) 0.2501(5) 0.059(2) Uani 1 1 d . . . H49 H 0.2285 0.9037 0.2716 0.071 Uiso 1 1 calc R . . C50 C 0.1407(6) 0.8130(5) 0.2643(4) 0.050(2) Uani 1 1 d . . . H50 H 0.1801 0.8023 0.2947 0.060 Uiso 1 1 calc R . . C51 C 0.0504(6) 0.7700(4) 0.2303(4) 0.0397(17) Uani 1 1 d . . . C52 C -0.0825(6) 0.6869(4) 0.1870(4) 0.0383(17) Uani 1 1 d . . . C53 C -0.2254(8) 0.6116(6) 0.2443(5) 0.065(3) Uani 1 1 d . . . H53A H -0.2630 0.5679 0.2428 0.097 Uiso 1 1 calc R . . H53B H -0.2740 0.6421 0.2506 0.097 Uiso 1 1 calc R . . H53C H -0.1722 0.6276 0.2798 0.097 Uiso 1 1 calc R . . C54 C 0.3354(6) 0.6035(4) 0.0360(4) 0.0428(19) Uani 1 1 d . . . C55 C 0.3725(10) 0.4731(6) 0.0285(6) 0.084(4) Uani 1 1 d . . . H55A H 0.3368 0.4522 0.0582 0.126 Uiso 1 1 calc R . . H55B H 0.4346 0.5044 0.0505 0.126 Uiso 1 1 calc R . . H55C H 0.3927 0.4393 -0.0078 0.126 Uiso 1 1 calc R . . C56 C 0.3874(6) 0.7008(4) 0.1104(4) 0.0421(19) Uani 1 1 d . . . C57 C 0.4205(8) 0.7553(6) 0.1655(5) 0.068(3) Uani 1 1 d . . . H57 H 0.4289 0.7496 0.2063 0.081 Uiso 1 1 calc R . . C58 C 0.4402(11) 0.8176(6) 0.1576(6) 0.084(4) Uani 1 1 d . . . H58 H 0.4616 0.8552 0.1939 0.100 Uiso 1 1 calc R . . C59 C 0.3527(6) 0.5987(4) 0.1525(4) 0.0396(18) Uani 1 1 d . . . H59A H 0.3098 0.5541 0.1346 0.048 Uiso 1 1 calc R . . H59B H 0.4233 0.5934 0.1632 0.048 Uiso 1 1 calc R . . C60 C 0.3067(6) 0.6352(4) 0.2141(3) 0.0349(16) Uani 1 1 d . . . C61 C 0.1996(5) 0.6398(4) 0.2127(3) 0.0337(16) Uani 1 1 d . . . C62 C 0.1338(7) 0.6132(5) 0.1489(4) 0.054(2) Uani 1 1 d . . . H62A H 0.1587 0.5751 0.1209 0.081 Uiso 1 1 calc R . . H62B H 0.1396 0.6477 0.1282 0.081 Uiso 1 1 calc R . . H62C H 0.0611 0.6000 0.1570 0.081 Uiso 1 1 calc R . . C63 C 0.1544(5) 0.6674(4) 0.2711(4) 0.0339(16) Uani 1 1 d . . . C64 C 0.2154(6) 0.6909(4) 0.3314(4) 0.0336(15) Uani 1 1 d . . . C65 C 0.1666(7) 0.7196(5) 0.3943(4) 0.050(2) Uani 1 1 d . . . H65A H 0.1846 0.7677 0.4075 0.075 Uiso 1 1 calc R . . H65B H 0.1929 0.7036 0.4274 0.075 Uiso 1 1 calc R . . H65C H 0.0911 0.7057 0.3883 0.075 Uiso 1 1 calc R . . C66 C 0.3230(6) 0.6861(4) 0.3321(3) 0.0337(16) Uani 1 1 d . . . C67 C 0.3872(7) 0.7070(5) 0.3964(4) 0.049(2) Uani 1 1 d . . . H67A H 0.3616 0.6753 0.4196 0.059 Uiso 1 1 calc R . . H67B H 0.4601 0.7038 0.3874 0.059 Uiso 1 1 calc R . . C69 C 0.3694(6) 0.6570(4) 0.2737(4) 0.0384(17) Uani 1 1 d . . . C70 C 0.4853(6) 0.6502(6) 0.2754(4) 0.059(3) Uani 1 1 d . . . H70A H 0.4901 0.6063 0.2772 0.088 Uiso 1 1 calc R . . H70B H 0.5226 0.6836 0.3132 0.088 Uiso 1 1 calc R . . H70C H 0.5163 0.6565 0.2367 0.088 Uiso 1 1 calc R . . C71 C 0.0370(6) 0.6678(5) 0.2705(4) 0.0415(18) Uani 1 1 d . . . H71A H -0.0012 0.6218 0.2534 0.050 Uiso 1 1 calc R . . H71B H 0.0178 0.6857 0.3151 0.050 Uiso 1 1 calc R . . C72 C 0.3776(7) 0.7090(5) 0.0492(4) 0.048(2) Uani 1 1 d . . . C76 C 0.3611(7) 0.7896(5) 0.5043(5) 0.055(2) Uani 1 1 d . . . C86 C 0.4001(7) 0.8331(5) 0.4246(5) 0.061(3) Uani 1 1 d . . . C88 C 0.3987(9) 0.7722(6) 0.0420(5) 0.072(3) Uani 1 1 d . . . H88 H 0.3928 0.7784 0.0012 0.086 Uiso 1 1 calc R . . C96 C 0.3379(6) 0.7453(5) 0.5456(3) 0.045(2) Uani 1 1 d . . . H96 H 0.3412 0.6999 0.5317 0.054 Uiso 1 1 calc R . . C97 C 0.3102(11) 0.7795(8) 0.6085(6) 0.091(4) Uani 1 1 d . . . H97 H 0.2932 0.7551 0.6375 0.109 Uiso 1 1 calc R . . C98 C 0.3330(10) 0.8870(8) 0.5908(7) 0.096(5) Uani 1 1 d . . . H98 H 0.3323 0.9327 0.6069 0.115 Uiso 1 1 calc R . . C99 C 0.4289(11) 0.8259(6) 0.0977(6) 0.083(4) Uani 1 1 d . . . H99 H 0.4421 0.8692 0.0944 0.100 Uiso 1 1 calc R . . C101 C 0.3607(9) 0.8577(6) 0.5268(5) 0.064(3) Uani 1 1 d . . . C103 C 0.3069(11) 0.8454(10) 0.6290(7) 0.104(5) Uani 1 1 d . . . H103 H 0.2860 0.8640 0.6708 0.124 Uiso 1 1 calc R . . C104 C 0.4325(11) 0.9261(9) 0.3651(11) 0.151(9) Uani 1 1 d . . . H10D H 0.4455 0.9494 0.4110 0.227 Uiso 1 1 calc R . . H10E H 0.3662 0.9332 0.3503 0.227 Uiso 1 1 calc R . . H10F H 0.4884 0.9431 0.3418 0.227 Uiso 1 1 calc R . . Re1 Re 0.21009(3) 0.171359(15) 0.606102(15) 0.03800(9) Uani 1 1 d . . . Re2 Re 0.28695(3) 0.489333(17) 0.469521(18) 0.04675(10) Uani 1 1 d . . . S3 S -0.05914(17) 0.13488(11) 0.52975(11) 0.0484(5) Uani 1 1 d . . . S4 S 0.00705(19) 0.41461(13) 0.42595(13) 0.0587(6) Uani 1 1 d . . . S5 S -0.1971(2) -0.07937(15) 0.02668(13) 0.0651(7) Uani 1 1 d . . . O1 O 0.3932(7) 0.6083(4) 0.5849(4) 0.084(2) Uani 1 1 d . . . O2 O 0.4461(7) 0.5439(4) 0.3862(4) 0.089(3) Uani 1 1 d . . . O3 O 0.3711(4) 0.4161(3) 0.4860(3) 0.0503(15) Uani 1 1 d . . . O4 O 0.1872(4) 0.4426(3) 0.5295(3) 0.0463(13) Uani 1 1 d . . . O5 O 0.3252(4) 0.2336(3) 0.5673(3) 0.0420(13) Uani 1 1 d . . . O6 O 0.1399(4) 0.2568(3) 0.6064(3) 0.0387(12) Uani 1 1 d . . . O7 O 0.3100(7) 0.2293(4) 0.7452(4) 0.090(3) Uani 1 1 d . . . O8 O 0.0339(6) 0.0881(4) 0.6572(4) 0.078(2) Uani 1 1 d . . . O9 O 0.3207(7) 0.0549(4) 0.5967(5) 0.102(3) Uani 1 1 d . . . O10 O 0.0611(5) 0.3673(3) 0.5956(3) 0.0611(18) Uani 1 1 d . . . H10 H 0.0508 0.4014 0.5882 0.092 Uiso 1 1 d R . . O11 O 0.4500(4) 0.3069(3) 0.4986(3) 0.0552(16) Uani 1 1 d . . . H11 H 0.4762 0.3341 0.4803 0.083 Uiso 1 1 d R . . O23 O 0.1445(7) 0.5801(4) 0.4429(4) 0.087(2) Uani 1 1 d . . . N1 N 0.2071(5) 0.4010(4) 0.3918(3) 0.0461(16) Uani 1 1 d . . . N2 N 0.0831(6) 0.3217(4) 0.3258(3) 0.0490(17) Uani 1 1 d . . . N3 N 0.1481(5) 0.1319(3) 0.5038(3) 0.0347(13) Uani 1 1 d . . . N4 N 0.0379(5) 0.0956(3) 0.4146(3) 0.0400(15) Uani 1 1 d . . . N10 N -0.0389(6) 0.0080(4) 0.1063(3) 0.0505(18) Uani 1 1 d . . . N11 N 0.0168(6) -0.0774(4) 0.0348(4) 0.0552(19) Uani 1 1 d . . . C1 C 0.1970(9) 0.5460(5) 0.4521(5) 0.062(3) Uani 1 1 d . . . C2 C 0.3856(8) 0.5230(5) 0.4158(5) 0.059(2) Uani 1 1 d . . . C3 C 0.3561(8) 0.5622(6) 0.5413(6) 0.063(3) Uani 1 1 d . . . C4 C 0.2724(8) 0.2089(5) 0.6934(4) 0.055(2) Uani 1 1 d . . . C5 C 0.2818(8) 0.0993(5) 0.5988(5) 0.061(3) Uani 1 1 d . . . C6 C 0.0974(8) 0.1200(5) 0.6382(4) 0.051(2) Uani 1 1 d . . . C7 C 0.1904(6) 0.2970(4) 0.5786(4) 0.0355(16) Uani 1 1 d . . . C8 C 0.2967(6) 0.2827(4) 0.5548(4) 0.0361(16) Uani 1 1 d . . . C9 C 0.3567(6) 0.3215(4) 0.5217(4) 0.0398(17) Uani 1 1 d . . . C10 C 0.3201(6) 0.3761(4) 0.5144(4) 0.0392(17) Uani 1 1 d . . . C11 C 0.2159(6) 0.3923(4) 0.5395(4) 0.0408(18) Uani 1 1 d . . . C12 C 0.1559(6) 0.3525(4) 0.5718(4) 0.0408(18) Uani 1 1 d . . . C13 C 0.0460(6) 0.1187(4) 0.4813(4) 0.0372(16) Uani 1 1 d . . . C14 C 0.1380(6) 0.0901(4) 0.3940(4) 0.0443(19) Uani 1 1 d . . . C16 C -0.0621(6) 0.0786(4) 0.3745(4) 0.046(2) Uani 1 1 d . . . H16A H -0.1178 0.0929 0.4025 0.056 Uiso 1 1 calc R . . H16B H -0.0803 0.0302 0.3554 0.056 Uiso 1 1 calc R . . C17 C -0.0579(6) 0.1108(4) 0.3198(4) 0.0432(19) Uani 1 1 d . . . C18 C -0.0842(6) 0.0684(4) 0.2548(4) 0.047(2) Uani 1 1 d . . . C19 C -0.0336(6) 0.1807(4) 0.3330(4) 0.0408(18) Uani 1 1 d . . . C20 C -0.0114(8) 0.2260(5) 0.4031(4) 0.054(2) Uani 1 1 d . . . H20A H -0.0397 0.2660 0.4083 0.081 Uiso 1 1 calc R . . H20B H 0.0636 0.2379 0.4133 0.081 Uiso 1 1 calc R . . H20C H -0.0442 0.2028 0.4319 0.081 Uiso 1 1 calc R . . C21 C -0.0376(6) 0.2082(4) 0.2828(4) 0.0446(19) Uani 1 1 d . . . C22 C -0.0618(7) 0.1666(6) 0.2176(4) 0.058(2) Uani 1 1 d . . . C23 C -0.0853(7) 0.0974(5) 0.2043(4) 0.052(2) Uani 1 1 d . . . C24 C -0.1166(9) 0.0508(6) 0.1356(5) 0.075(3) Uani 1 1 d . . . H24A H -0.1838 0.0218 0.1361 0.090 Uiso 1 1 calc R . . H24B H -0.1273 0.0777 0.1078 0.090 Uiso 1 1 calc R . . C25 C -0.0254(7) 0.2837(5) 0.2989(5) 0.053(2) Uani 1 1 d . . . H25A H -0.0425 0.2940 0.2596 0.064 Uiso 1 1 calc R . . H25B H -0.0762 0.2991 0.3305 0.064 Uiso 1 1 calc R . . C26 C 0.1801(7) 0.3067(5) 0.3034(4) 0.049(2) Uani 1 1 d . . . C27 C 0.2050(9) 0.2572(6) 0.2507(5) 0.070(3) Uani 1 1 d . . . H27 H 0.1527 0.2253 0.2225 0.084 Uiso 1 1 calc R . . C28 C 0.3109(9) 0.2571(6) 0.2415(6) 0.080(3) Uani 1 1 d . . . H28 H 0.3310 0.2252 0.2058 0.096 Uiso 1 1 calc R . . C29 C 0.3892(9) 0.3048(6) 0.2858(6) 0.080(3) Uani 1 1 d . . . H29 H 0.4599 0.3015 0.2801 0.095 Uiso 1 1 calc R . . C30 C 0.3650(8) 0.3569(5) 0.3376(5) 0.061(3) Uani 1 1 d . . . H30 H 0.4169 0.3895 0.3654 0.074 Uiso 1 1 calc R . . C31 C 0.2553(7) 0.3566(5) 0.3450(4) 0.050(2) Uani 1 1 d . . . C32 C 0.1043(7) 0.3780(4) 0.3778(4) 0.0445(19) Uani 1 1 d . . . C33 C -0.0694(11) 0.4398(7) 0.3704(7) 0.098(4) Uani 1 1 d . . . H33A H -0.0241 0.4710 0.3537 0.148 Uiso 1 1 calc R . . H33B H -0.1244 0.4607 0.3931 0.148 Uiso 1 1 calc R . . H33C H -0.1004 0.4010 0.3349 0.148 Uiso 1 1 calc R . . C73 C 0.2068(6) 0.1136(4) 0.4492(4) 0.0426(18) Uani 1 1 d . . . C74 C 0.1755(8) 0.0677(5) 0.3305(4) 0.062(3) Uani 1 1 d . . . H74 H 0.1297 0.0525 0.2932 0.075 Uiso 1 1 calc R . . C75 C 0.3151(7) 0.1151(5) 0.4454(5) 0.055(2) Uani 1 1 d . . . H75 H 0.3607 0.1299 0.4827 0.066 Uiso 1 1 calc R . . C78 C 0.0706(7) 0.0200(5) 0.1190(4) 0.052(2) Uani 1 1 d . . . C79 C -0.0638(7) -0.0497(5) 0.0563(4) 0.049(2) Uani 1 1 d . . . C82 C -0.1864(10) -0.1510(6) -0.0403(5) 0.079(3) Uani 1 1 d . . . H82A H -0.1329 -0.1387 -0.0676 0.118 Uiso 1 1 calc R . . H82B H -0.2531 -0.1679 -0.0653 0.118 Uiso 1 1 calc R . . H82C H -0.1676 -0.1852 -0.0243 0.118 Uiso 1 1 calc R . . C83 C 0.2444(9) 0.0626(6) 0.1596(6) 0.072(3) Uani 1 1 d . . . H83 H 0.2940 0.0966 0.1879 0.087 Uiso 1 1 calc R . . C84 C 0.2816(8) 0.0696(6) 0.3267(5) 0.070(3) Uani 1 1 d . . . H84 H 0.3090 0.0550 0.2860 0.084 Uiso 1 1 calc R . . C89 C -0.1281(8) 0.0509(6) 0.5201(6) 0.075(3) Uani 1 1 d . . . H89A H -0.1308 0.0243 0.4751 0.113 Uiso 1 1 calc R . . H89B H -0.1988 0.0521 0.5338 0.113 Uiso 1 1 calc R . . H89C H -0.0916 0.0313 0.5463 0.113 Uiso 1 1 calc R . . C90 C -0.1166(9) -0.0077(5) 0.2394(5) 0.068(3) Uani 1 1 d . . . H90A H -0.1332 -0.0280 0.1933 0.101 Uiso 1 1 calc R . . H90B H -0.1777 -0.0178 0.2626 0.101 Uiso 1 1 calc R . . H90C H -0.0593 -0.0253 0.2525 0.101 Uiso 1 1 calc R . . C91 C 0.2796(9) 0.0080(7) 0.1153(6) 0.079(3) Uani 1 1 d . . . H91 H 0.3513 0.0060 0.1151 0.095 Uiso 1 1 calc R . . C92 C 0.2088(9) -0.0418(6) 0.0728(6) 0.073(3) Uani 1 1 d . . . H92 H 0.2303 -0.0792 0.0445 0.088 Uiso 1 1 calc R . . C93 C 0.1031(8) -0.0350(5) 0.0732(5) 0.057(2) Uani 1 1 d . . . C94 C 0.1419(8) 0.0673(5) 0.1626(5) 0.061(2) Uani 1 1 d . . . H94 H 0.1203 0.1025 0.1941 0.073 Uiso 1 1 calc R . . C95 C 0.3516(8) 0.0937(6) 0.3841(5) 0.074(3) Uani 1 1 d . . . H95 H 0.4238 0.0950 0.3798 0.089 Uiso 1 1 calc R . . C100 C -0.0588(12) 0.1991(7) 0.1621(5) 0.092(4) Uani 1 1 d . . . H10A H -0.0594 0.1652 0.1208 0.138 Uiso 1 1 calc R . . H10B H 0.0045 0.2326 0.1682 0.138 Uiso 1 1 calc R . . H10C H -0.1195 0.2198 0.1630 0.138 Uiso 1 1 calc R . . 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 Re3 0.02641(15) 0.0645(2) 0.03773(17) 0.02124(16) 0.00117(12) 0.01137(14) Re4 0.03465(18) 0.0946(3) 0.03252(17) 0.01742(18) 0.00601(13) 0.01840(18) S1 0.0519(13) 0.0608(15) 0.0436(12) 0.0046(11) -0.0003(10) 0.0015(11) S2 0.0358(10) 0.0518(13) 0.0491(12) 0.0173(10) -0.0021(9) 0.0000(9) S6 0.104(3) 0.098(3) 0.100(3) 0.051(2) -0.002(2) -0.007(2) O12 0.074(5) 0.063(5) 0.104(6) 0.036(4) 0.017(4) 0.025(4) O13 0.033(3) 0.077(5) 0.065(4) 0.019(4) 0.013(3) 0.007(3) O14 0.028(3) 0.071(4) 0.042(3) 0.018(3) 0.006(2) 0.005(3) O15 0.040(3) 0.063(4) 0.047(3) 0.021(3) 0.006(3) 0.016(3) O16 0.036(3) 0.082(5) 0.056(4) 0.032(3) 0.015(3) 0.013(3) O17 0.034(3) 0.078(5) 0.051(4) 0.008(3) 0.013(3) 0.021(3) O18 0.053(4) 0.067(4) 0.063(4) 0.027(3) 0.023(3) 0.012(3) O19 0.055(4) 0.061(5) 0.096(6) 0.018(4) 0.013(4) 0.015(3) O20 0.054(4) 0.163(9) 0.091(6) 0.081(6) 0.024(4) 0.021(5) O21 0.071(5) 0.111(7) 0.092(6) -0.005(5) 0.015(4) 0.040(5) O22 0.080(6) 0.213(12) 0.081(6) 0.055(7) -0.032(5) 0.038(7) O24 0.109(8) 0.323(19) 0.046(5) 0.057(8) -0.015(5) 0.028(10) N5 0.032(3) 0.049(4) 0.044(4) 0.021(3) -0.001(3) 0.009(3) N6 0.027(3) 0.046(4) 0.042(3) 0.018(3) -0.004(3) 0.007(3) N7 0.043(4) 0.072(5) 0.033(4) 0.013(4) 0.003(3) 0.005(4) N8 0.035(3) 0.052(4) 0.034(3) 0.012(3) 0.000(3) 0.000(3) N9 0.047(4) 0.049(4) 0.042(4) 0.011(3) -0.011(3) 0.005(3) N12 0.084(7) 0.060(6) 0.105(8) 0.003(6) -0.031(6) 0.005(5) C34 0.044(5) 0.128(10) 0.048(5) 0.033(6) -0.002(4) 0.026(6) C35 0.045(5) 0.061(6) 0.059(5) 0.035(5) 0.000(4) 0.014(4) C36 0.034(4) 0.063(6) 0.049(5) 0.020(4) 0.000(4) 0.016(4) C37 0.054(6) 0.156(13) 0.054(7) 0.026(8) -0.006(5) 0.013(7) C38 0.052(6) 0.109(10) 0.045(6) 0.003(6) 0.002(4) 0.022(6) C39 0.050(6) 0.123(10) 0.042(5) 0.036(6) 0.009(4) 0.032(6) C40 0.035(4) 0.070(6) 0.036(4) 0.026(4) 0.000(3) 0.007(4) C41 0.036(4) 0.074(6) 0.043(5) 0.021(4) -0.005(4) 0.012(4) C42 0.029(4) 0.064(6) 0.051(5) 0.013(4) 0.001(3) 0.009(4) C43 0.032(4) 0.061(6) 0.041(4) 0.016(4) -0.007(3) 0.000(4) C44 0.041(4) 0.056(5) 0.033(4) 0.017(4) 0.002(3) 0.008(4) C45 0.034(4) 0.064(6) 0.036(4) 0.021(4) 0.006(3) 0.011(4) C46 0.026(3) 0.049(5) 0.041(4) 0.017(4) 0.005(3) 0.007(3) C47 0.046(5) 0.050(5) 0.053(5) 0.024(4) -0.008(4) 0.010(4) C48 0.062(6) 0.053(6) 0.070(6) 0.028(5) -0.003(5) -0.001(5) C49 0.052(5) 0.046(5) 0.075(7) 0.020(5) -0.014(5) -0.004(4) C50 0.038(4) 0.054(5) 0.058(5) 0.023(4) -0.012(4) 0.000(4) C51 0.031(4) 0.047(5) 0.043(4) 0.015(4) -0.001(3) 0.011(3) C52 0.028(4) 0.046(5) 0.040(4) 0.014(4) 0.002(3) 0.003(3) C53 0.055(6) 0.075(7) 0.063(6) 0.027(5) 0.009(5) 0.000(5) C54 0.034(4) 0.057(5) 0.032(4) 0.009(4) 0.002(3) 0.003(4) C55 0.078(8) 0.087(9) 0.084(8) 0.013(7) -0.004(6) 0.034(7) C56 0.029(4) 0.052(5) 0.039(4) 0.011(4) 0.001(3) -0.001(3) C57 0.074(7) 0.070(7) 0.048(6) 0.016(5) 0.006(5) -0.010(6) C58 0.117(10) 0.063(7) 0.059(7) 0.012(6) 0.007(7) -0.001(7) C59 0.033(4) 0.052(5) 0.037(4) 0.019(4) 0.003(3) 0.006(3) C60 0.031(4) 0.042(4) 0.032(4) 0.016(3) 0.001(3) -0.001(3) C61 0.032(4) 0.042(4) 0.030(4) 0.018(3) -0.002(3) 0.002(3) C62 0.038(4) 0.080(7) 0.035(4) 0.006(4) -0.003(3) 0.007(4) C63 0.024(3) 0.042(4) 0.040(4) 0.020(3) -0.002(3) 0.004(3) C64 0.034(4) 0.034(4) 0.036(4) 0.015(3) 0.005(3) 0.007(3) C65 0.041(4) 0.065(6) 0.041(5) 0.009(4) 0.000(4) 0.015(4) C66 0.032(4) 0.040(4) 0.030(4) 0.015(3) -0.002(3) 0.004(3) C67 0.044(5) 0.064(6) 0.041(4) 0.013(4) -0.007(4) 0.021(4) C69 0.027(4) 0.048(5) 0.041(4) 0.016(4) -0.002(3) 0.006(3) C70 0.030(4) 0.097(8) 0.044(5) 0.012(5) 0.002(3) 0.013(5) C71 0.027(4) 0.059(5) 0.043(4) 0.025(4) 0.002(3) 0.006(3) C72 0.041(4) 0.061(6) 0.044(5) 0.023(4) 0.005(4) 0.003(4) C76 0.046(5) 0.060(6) 0.054(5) 0.005(5) -0.016(4) 0.016(4) C86 0.047(5) 0.052(6) 0.072(7) 0.013(5) -0.020(5) -0.010(4) C88 0.082(7) 0.082(8) 0.053(6) 0.032(6) 0.003(5) 0.000(6) C96 0.053(5) 0.071(6) 0.017(3) 0.012(4) 0.011(3) 0.032(4) C97 0.093(9) 0.103(11) 0.078(9) 0.025(8) 0.014(7) 0.029(8) C98 0.063(7) 0.099(10) 0.103(11) -0.013(9) -0.009(7) 0.036(7) C99 0.126(11) 0.054(7) 0.068(7) 0.031(6) -0.009(7) -0.009(7) C101 0.071(7) 0.063(7) 0.049(6) 0.003(5) -0.013(5) 0.012(5) C103 0.088(10) 0.143(16) 0.080(9) 0.026(10) 0.018(7) 0.037(10) C104 0.058(8) 0.172(17) 0.28(3) 0.171(19) -0.003(11) -0.002(9) Re1 0.04974(19) 0.03168(17) 0.03515(17) 0.01524(13) -0.00104(13) 0.00574(13) Re2 0.0530(2) 0.03719(19) 0.0566(2) 0.02699(16) 0.00745(16) 0.00339(15) S3 0.0460(11) 0.0474(12) 0.0539(13) 0.0155(10) 0.0135(9) 0.0142(10) S4 0.0528(13) 0.0548(14) 0.0697(16) 0.0166(12) 0.0083(11) 0.0180(11) S5 0.0590(15) 0.0723(18) 0.0569(15) 0.0099(13) -0.0063(11) 0.0118(13) O1 0.088(6) 0.067(5) 0.084(6) 0.012(4) -0.011(5) 0.001(4) O2 0.097(6) 0.086(6) 0.098(6) 0.059(5) 0.033(5) -0.006(5) O3 0.047(3) 0.056(4) 0.061(4) 0.037(3) 0.014(3) 0.009(3) O4 0.048(3) 0.041(3) 0.060(4) 0.028(3) 0.009(3) 0.011(3) O5 0.041(3) 0.039(3) 0.049(3) 0.020(3) -0.002(2) 0.005(2) O6 0.049(3) 0.032(3) 0.041(3) 0.017(2) 0.013(2) 0.011(2) O7 0.118(7) 0.088(6) 0.050(4) 0.021(4) -0.025(4) -0.018(5) O8 0.084(5) 0.073(5) 0.089(5) 0.054(4) 0.020(4) -0.004(4) O9 0.092(6) 0.064(5) 0.152(9) 0.024(5) -0.037(6) 0.034(5) O10 0.057(4) 0.058(4) 0.089(5) 0.043(4) 0.035(3) 0.028(3) O11 0.039(3) 0.071(4) 0.071(4) 0.040(3) 0.014(3) 0.018(3) O23 0.101(6) 0.071(5) 0.117(7) 0.060(5) 0.004(5) 0.032(5) N1 0.045(4) 0.046(4) 0.054(4) 0.025(3) 0.009(3) 0.008(3) N2 0.056(4) 0.046(4) 0.047(4) 0.018(3) 0.004(3) 0.007(3) N3 0.036(3) 0.036(3) 0.034(3) 0.009(3) 0.003(3) 0.015(3) N4 0.039(3) 0.042(4) 0.039(4) 0.012(3) -0.003(3) 0.010(3) N10 0.054(4) 0.053(5) 0.044(4) 0.011(3) -0.004(3) 0.018(4) N11 0.048(4) 0.056(5) 0.063(5) 0.020(4) 0.007(4) 0.011(4) C1 0.078(7) 0.040(5) 0.076(7) 0.036(5) 0.005(5) 0.002(5) C2 0.067(6) 0.054(6) 0.063(6) 0.032(5) 0.011(5) 0.003(5) C3 0.065(6) 0.056(6) 0.071(7) 0.026(6) 0.011(5) 0.009(5) C4 0.079(7) 0.049(5) 0.041(5) 0.022(4) -0.003(4) 0.008(5) C5 0.063(6) 0.050(6) 0.071(6) 0.021(5) -0.011(5) 0.012(5) C6 0.071(6) 0.047(5) 0.044(5) 0.024(4) 0.007(4) 0.013(5) C7 0.041(4) 0.031(4) 0.036(4) 0.014(3) 0.002(3) 0.003(3) C8 0.045(4) 0.031(4) 0.035(4) 0.014(3) 0.001(3) 0.009(3) C9 0.034(4) 0.042(5) 0.047(4) 0.018(4) 0.005(3) 0.010(3) C10 0.034(4) 0.035(4) 0.051(5) 0.023(4) 0.006(3) -0.002(3) C11 0.047(4) 0.040(4) 0.043(4) 0.021(4) 0.006(3) 0.013(4) C12 0.040(4) 0.036(4) 0.052(5) 0.021(4) 0.013(3) 0.008(3) C13 0.038(4) 0.036(4) 0.038(4) 0.011(3) 0.004(3) 0.012(3) C14 0.044(4) 0.046(5) 0.043(5) 0.010(4) 0.005(4) 0.015(4) C16 0.038(4) 0.045(5) 0.050(5) 0.010(4) -0.011(4) 0.001(4) C17 0.029(4) 0.050(5) 0.046(5) 0.010(4) -0.010(3) 0.004(3) C18 0.035(4) 0.049(5) 0.048(5) 0.005(4) -0.009(4) 0.000(4) C19 0.034(4) 0.046(5) 0.037(4) 0.005(4) -0.002(3) 0.006(3) C20 0.062(6) 0.049(5) 0.047(5) 0.013(4) -0.006(4) 0.002(4) C21 0.035(4) 0.051(5) 0.049(5) 0.018(4) -0.001(3) 0.006(4) C22 0.051(5) 0.084(8) 0.043(5) 0.023(5) -0.004(4) 0.017(5) C23 0.046(5) 0.063(6) 0.042(5) 0.003(4) -0.012(4) 0.019(4) C24 0.086(8) 0.073(7) 0.055(6) -0.005(5) -0.029(5) 0.032(6) C25 0.051(5) 0.057(6) 0.053(5) 0.019(4) -0.002(4) 0.012(4) C26 0.050(5) 0.052(5) 0.047(5) 0.019(4) 0.010(4) 0.011(4) C27 0.063(6) 0.072(7) 0.067(7) 0.017(6) 0.015(5) 0.001(5) C28 0.072(7) 0.083(8) 0.080(8) 0.019(7) 0.035(6) 0.016(6) C29 0.054(6) 0.083(8) 0.102(9) 0.031(7) 0.032(6) 0.008(6) C30 0.058(6) 0.060(6) 0.067(6) 0.021(5) 0.016(5) 0.009(5) C31 0.057(5) 0.046(5) 0.053(5) 0.023(4) 0.016(4) 0.013(4) C32 0.048(5) 0.040(5) 0.052(5) 0.021(4) 0.009(4) 0.013(4) C33 0.093(9) 0.089(9) 0.125(11) 0.030(8) -0.003(8) 0.053(8) C73 0.036(4) 0.048(5) 0.048(5) 0.016(4) 0.005(3) 0.014(4) C74 0.065(6) 0.076(7) 0.040(5) 0.001(5) -0.007(4) 0.030(5) C75 0.038(4) 0.069(6) 0.054(5) 0.009(5) -0.006(4) 0.016(4) C78 0.057(5) 0.059(6) 0.050(5) 0.027(5) 0.006(4) 0.019(5) C79 0.059(5) 0.051(5) 0.045(5) 0.023(4) 0.004(4) 0.015(4) C82 0.099(9) 0.063(7) 0.060(6) -0.002(5) -0.019(6) 0.016(6) C83 0.074(7) 0.075(8) 0.075(7) 0.036(6) -0.017(6) 0.009(6) C84 0.066(6) 0.105(9) 0.043(5) 0.012(5) 0.016(5) 0.044(6) C89 0.059(6) 0.068(7) 0.099(9) 0.036(7) 0.017(6) -0.005(5) C90 0.084(7) 0.054(6) 0.053(6) 0.006(5) -0.003(5) 0.003(5) C91 0.056(6) 0.107(10) 0.092(9) 0.057(8) 0.006(6) 0.013(7) C92 0.063(7) 0.084(8) 0.078(8) 0.027(6) 0.022(6) 0.018(6) C93 0.064(6) 0.052(6) 0.064(6) 0.033(5) 0.011(5) 0.007(5) C94 0.065(6) 0.061(6) 0.059(6) 0.021(5) -0.004(5) 0.018(5) C95 0.039(5) 0.108(9) 0.061(6) 0.005(6) 0.007(4) 0.017(5) C100 0.125(11) 0.109(10) 0.045(6) 0.026(6) -0.010(6) 0.021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re3 C34 1.889(9) . ? Re3 C35 1.898(10) . ? Re3 C36 1.915(9) . ? Re3 O15 2.140(6) . ? Re3 O14 2.156(6) . ? Re3 N5 2.210(6) . ? Re4 C38 1.908(13) . ? Re4 C39 1.919(12) . ? Re4 C37 1.916(11) . ? Re4 O16 2.138(7) . ? Re4 O17 2.143(6) . ? Re4 N7 2.211(7) . ? S1 C54 1.761(9) . ? S1 C55 1.818(12) . ? S2 C52 1.762(8) . ? S2 C53 1.814(10) . ? S6 C86 1.674(12) . ? S6 C104 1.730(17) . ? O12 C35 1.154(11) . ? O13 C36 1.139(10) . ? O14 C43 1.292(9) . ? O15 C44 1.287(10) . ? O16 C40 1.273(9) . ? O17 C41 1.269(10) . ? O18 C45 1.363(11) . ? O18 H18 0.8200 . ? O19 C42 1.336(11) . ? O19 H19 0.8200 . ? O20 C39 1.160(13) . ? O21 C38 1.144(14) . ? O22 C34 1.143(11) . ? O24 C37 1.117(12) . ? N5 C52 1.296(10) . ? N5 C46 1.405(10) . ? N6 C52 1.372(9) . ? N6 C51 1.366(10) . ? N6 C71 1.475(10) . ? N7 C54 1.294(11) . ? N7 C72 1.397(12) . ? N8 C56 1.356(11) . ? N8 C54 1.359(10) . ? N8 C59 1.510(10) . ? N9 C86 1.352(12) . ? N9 C76 1.379(12) . ? N9 C67 1.469(11) . ? N12 C86 1.359(14) . ? N12 C101 1.407(15) . ? C40 C45 1.395(12) . ? C40 C41 1.497(13) . ? C41 C42 1.401(12) . ? C42 C43 1.403(12) . ? C43 C44 1.481(12) . ? C44 C45 1.363(11) . ? C46 C51 1.385(10) . ? C46 C47 1.386(11) . ? C47 C48 1.394(13) . ? C47 H47 0.9300 . ? C48 C49 1.389(13) . ? C48 H48 0.9300 . ? C49 C50 1.393(12) . ? C49 H49 0.9300 . ? C50 C51 1.390(11) . ? C50 H50 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 C57 1.385(13) . ? C56 C72 1.388(11) . ? C57 C58 1.367(15) . ? C57 H57 0.9300 . ? C58 C99 1.365(15) . ? C58 H58 0.9300 . ? C59 C60 1.503(10) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.399(10) . ? C60 C69 1.418(10) . ? C61 C63 1.395(10) . ? C61 C62 1.506(10) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 C64 1.417(10) . ? C63 C71 1.512(10) . ? C64 C66 1.406(10) . ? C64 C65 1.498(11) . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 C69 1.408(11) . ? C66 C67 1.512(10) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C69 C70 1.525(10) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 C88 1.380(14) . ? C76 C101 1.381(14) . ? C76 C96 1.476(13) . ? C88 C99 1.379(15) . ? C88 H88 0.9300 . ? C96 C97 1.411(15) . ? C96 H96 0.9300 . ? C97 C103 1.34(2) . ? C97 H97 0.9300 . ? C98 C103 1.38(2) . ? C98 C101 1.406(17) . ? C98 H98 0.9300 . ? C99 H99 0.9300 . ? C103 H103 0.9300 . ? C104 H10D 0.9600 . ? C104 H10E 0.9600 . ? C104 H10F 0.9600 . ? Re1 C5 1.893(10) . ? Re1 C6 1.918(9) . ? Re1 C4 1.913(9) . ? Re1 O5 2.152(5) . ? Re1 O6 2.166(5) . ? Re1 N3 2.195(6) . ? Re2 C3 1.903(12) . ? Re2 C2 1.911(9) . ? Re2 C1 1.922(11) . ? Re2 O4 2.156(5) . ? Re2 O3 2.157(6) . ? Re2 N1 2.185(7) . ? S3 C13 1.732(8) . ? S3 C89 1.798(10) . ? S4 C32 1.765(9) . ? S4 C33 1.802(12) . ? S5 C79 1.763(10) . ? S5 C82 1.779(11) . ? O1 C3 1.158(12) . ? O2 C2 1.125(11) . ? O3 C10 1.284(9) . ? O4 C11 1.266(9) . ? O5 C8 1.265(9) . ? O6 C7 1.277(8) . ? O7 C4 1.138(10) . ? O8 C6 1.128(11) . ? O9 C5 1.134(11) . ? O10 C12 1.376(9) . ? O10 H10 0.8199 . ? O11 C9 1.353(9) . ? O11 H11 0.8199 . ? O23 C1 1.131(12) . ? N1 C32 1.325(11) . ? N1 C31 1.388(11) . ? N2 C32 1.352(11) . ? N2 C26 1.395(11) . ? N2 C25 1.498(11) . ? N3 C13 1.349(9) . ? N3 C73 1.392(10) . ? N4 C13 1.365(10) . ? N4 C14 1.377(10) . ? N4 C16 1.472(9) . ? N10 C79 1.349(11) . ? N10 C78 1.396(11) . ? N10 C24 1.485(12) . ? N11 C79 1.302(11) . ? N11 C93 1.382(12) . ? C7 C12 1.378(11) . ? C7 C8 1.512(11) . ? C8 C9 1.385(10) . ? C9 C10 1.379(11) . ? C10 C11 1.505(11) . ? C11 C12 1.389(11) . ? C14 C73 1.386(11) . ? C14 C74 1.423(12) . ? C16 C17 1.529(12) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C19 1.402(12) . ? C17 C18 1.417(11) . ? C18 C23 1.405(13) . ? C18 C90 1.528(13) . ? C19 C21 1.381(12) . ? C19 C20 1.517(11) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.412(12) . ? C21 C25 1.515(12) . ? C22 C23 1.389(14) . ? C22 C100 1.549(14) . ? C23 C24 1.514(12) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.378(13) . ? C26 C31 1.384(13) . ? C27 C28 1.378(15) . ? C27 H27 0.9300 . ? C28 C29 1.412(16) . ? C28 H28 0.9300 . ? C29 C30 1.395(15) . ? C29 H29 0.9300 . ? C30 C31 1.420(13) . ? C30 H30 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C73 C75 1.391(11) . ? C74 C84 1.362(14) . ? C74 H74 0.9300 . ? C75 C95 1.375(13) . ? C75 H75 0.9300 . ? C78 C94 1.351(13) . ? C78 C93 1.412(13) . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 C94 1.340(15) . ? C83 C91 1.408(17) . ? C83 H83 0.9300 . ? C84 C95 1.428(14) . ? C84 H84 0.9300 . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 C92 1.360(16) . ? C91 H91 0.9300 . ? C92 C93 1.393(14) . ? C92 H92 0.9300 . ? C94 H94 0.9300 . ? C95 H95 0.9300 . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C34 Re3 C35 88.2(5) . . ? C34 Re3 C36 85.4(4) . . ? C35 Re3 C36 88.3(4) . . ? C34 Re3 O15 95.5(4) . . ? C35 Re3 O15 99.1(3) . . ? C36 Re3 O15 172.6(3) . . ? C34 Re3 O14 95.3(4) . . ? C35 Re3 O14 172.8(3) . . ? C36 Re3 O14 98.2(3) . . ? O15 Re3 O14 74.4(2) . . ? C34 Re3 N5 177.2(3) . . ? C35 Re3 N5 93.7(3) . . ? C36 Re3 N5 96.8(3) . . ? O15 Re3 N5 82.2(2) . . ? O14 Re3 N5 82.5(2) . . ? C38 Re4 C39 87.4(5) . . ? C38 Re4 C37 87.4(5) . . ? C39 Re4 C37 85.8(5) . . ? C38 Re4 O16 176.2(4) . . ? C39 Re4 O16 95.6(4) . . ? C37 Re4 O16 95.1(5) . . ? C38 Re4 O17 102.5(4) . . ? C39 Re4 O17 170.0(4) . . ? C37 Re4 O17 94.3(4) . . ? O16 Re4 O17 74.5(2) . . ? C38 Re4 N7 93.9(4) . . ? C39 Re4 N7 98.6(3) . . ? C37 Re4 N7 175.5(4) . . ? O16 Re4 N7 83.3(3) . . ? O17 Re4 N7 81.2(2) . . ? C54 S1 C55 105.7(5) . . ? C52 S2 C53 101.2(4) . . ? C86 S6 C104 101.8(8) . . ? C43 O14 Re3 116.1(6) . . ? C44 O15 Re3 117.2(5) . . ? C40 O16 Re4 117.2(6) . . ? C41 O17 Re4 116.5(6) . . ? C45 O18 H18 109.5 . . ? C42 O19 H19 109.5 . . ? C52 N5 C46 106.1(6) . . ? C52 N5 Re3 127.2(5) . . ? C46 N5 Re3 126.8(5) . . ? C52 N6 C51 106.7(6) . . ? C52 N6 C71 125.4(7) . . ? C51 N6 C71 127.8(6) . . ? C54 N7 C72 105.5(7) . . ? C54 N7 Re4 129.1(6) . . ? C72 N7 Re4 125.3(6) . . ? C56 N8 C54 107.3(7) . . ? C56 N8 C59 127.2(6) . . ? C54 N8 C59 125.5(7) . . ? C86 N9 C76 107.7(8) . . ? C86 N9 C67 128.1(8) . . ? C76 N9 C67 124.1(8) . . ? C86 N12 C101 104.5(9) . . ? O22 C34 Re3 174.6(11) . . ? O12 C35 Re3 179.5(9) . . ? O13 C36 Re3 175.6(8) . . ? O24 C37 Re4 176.6(11) . . ? O21 C38 Re4 178.3(11) . . ? O20 C39 Re4 173.9(9) . . ? O16 C40 C45 124.0(9) . . ? O16 C40 C41 114.9(8) . . ? C45 C40 C41 121.0(7) . . ? O17 C41 C42 123.3(9) . . ? O17 C41 C40 116.1(8) . . ? C42 C41 C40 120.6(8) . . ? O19 C42 C41 121.8(8) . . ? O19 C42 C43 121.4(8) . . ? C41 C42 C43 116.7(9) . . ? O14 C43 C42 122.1(8) . . ? O14 C43 C44 115.9(8) . . ? C42 C43 C44 121.9(8) . . ? O15 C44 C45 123.3(8) . . ? O15 C44 C43 115.4(7) . . ? C45 C44 C43 121.2(8) . . ? O18 C45 C44 123.0(8) . . ? O18 C45 C40 118.6(7) . . ? C44 C45 C40 118.4(8) . . ? C51 C46 C47 121.6(7) . . ? C51 C46 N5 108.2(7) . . ? C47 C46 N5 130.2(7) . . ? C46 C47 C48 116.9(8) . . ? C46 C47 H47 121.5 . . ? C48 C47 H47 121.5 . . ? C49 C48 C47 121.1(9) . . ? C49 C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? C48 C49 C50 122.3(8) . . ? C48 C49 H49 118.8 . . ? C50 C49 H49 118.8 . . ? C51 C50 C49 115.8(8) . . ? C51 C50 H50 122.1 . . ? C49 C50 H50 122.1 . . ? N6 C51 C46 106.7(7) . . ? N6 C51 C50 130.9(7) . . ? C46 C51 C50 122.3(8) . . ? N5 C52 N6 112.3(7) . . ? N5 C52 S2 124.8(6) . . ? N6 C52 S2 122.7(6) . . ? S2 C53 H53A 109.5 . . ? S2 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? S2 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N7 C54 N8 112.6(8) . . ? N7 C54 S1 121.9(6) . . ? N8 C54 S1 125.3(7) . . ? S1 C55 H55A 109.5 . . ? S1 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? S1 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N8 C56 C57 132.7(8) . . ? N8 C56 C72 106.0(7) . . ? C57 C56 C72 121.3(9) . . ? C58 C57 C56 117.4(10) . . ? C58 C57 H57 121.3 . . ? C56 C57 H57 121.3 . . ? C57 C58 C99 121.4(11) . . ? C57 C58 H58 119.3 . . ? C99 C58 H58 119.3 . . ? C60 C59 N8 113.6(7) . . ? C60 C59 H59A 108.9 . . ? N8 C59 H59A 108.9 . . ? C60 C59 H59B 108.9 . . ? N8 C59 H59B 108.9 . . ? H59A C59 H59B 107.7 . . ? C61 C60 C69 121.3(7) . . ? C61 C60 C59 119.2(6) . . ? C69 C60 C59 119.0(7) . . ? C63 C61 C60 119.2(6) . . ? C63 C61 C62 120.7(7) . . ? C60 C61 C62 120.1(7) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 C64 120.9(6) . . ? C61 C63 C71 119.4(6) . . ? C64 C63 C71 119.5(7) . . ? C66 C64 C63 119.3(6) . . ? C66 C64 C65 119.6(7) . . ? C63 C64 C65 121.1(6) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C69 C66 C64 120.5(6) . . ? C69 C66 C67 119.5(6) . . ? C64 C66 C67 119.8(7) . . ? N9 C67 C66 115.7(7) . . ? N9 C67 H67A 108.4 . . ? C66 C67 H67A 108.4 . . ? N9 C67 H67B 108.4 . . ? C66 C67 H67B 108.4 . . ? H67A C67 H67B 107.4 . . ? C66 C69 C60 118.7(6) . . ? C66 C69 C70 120.0(7) . . ? C60 C69 C70 121.2(7) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N6 C71 C63 113.8(6) . . ? N6 C71 H71A 108.8 . . ? C63 C71 H71A 108.8 . . ? N6 C71 H71B 108.8 . . ? C63 C71 H71B 108.8 . . ? H71A C71 H71B 107.7 . . ? C88 C72 C56 120.6(9) . . ? C88 C72 N7 130.8(8) . . ? C56 C72 N7 108.6(8) . . ? N9 C76 C101 106.7(9) . . ? N9 C76 C96 130.4(8) . . ? C101 C76 C96 122.8(9) . . ? N9 C86 N12 111.7(10) . . ? N9 C86 S6 125.7(8) . . ? N12 C86 S6 122.5(9) . . ? C99 C88 C72 117.1(9) . . ? C99 C88 H88 121.4 . . ? C72 C88 H88 121.4 . . ? C97 C96 C76 112.6(10) . . ? C97 C96 H96 123.7 . . ? C76 C96 H96 123.7 . . ? C103 C97 C96 123.7(14) . . ? C103 C97 H97 118.1 . . ? C96 C97 H97 118.1 . . ? C103 C98 C101 117.6(14) . . ? C103 C98 H98 121.2 . . ? C101 C98 H98 121.2 . . ? C88 C99 C58 122.2(11) . . ? C88 C99 H99 118.9 . . ? C58 C99 H99 118.9 . . ? C76 C101 N12 109.3(9) . . ? C76 C101 C98 119.9(12) . . ? N12 C101 C98 130.7(12) . . ? C97 C103 C98 123.2(14) . . ? C97 C103 H103 118.4 . . ? C98 C103 H103 118.4 . . ? S6 C104 H10D 109.5 . . ? S6 C104 H10E 109.5 . . ? H10D C104 H10E 109.5 . . ? S6 C104 H10F 109.5 . . ? H10D C104 H10F 109.5 . . ? H10E C104 H10F 109.5 . . ? C5 Re1 C6 85.6(4) . . ? C5 Re1 C4 86.7(4) . . ? C6 Re1 C4 88.6(4) . . ? C5 Re1 O5 99.4(4) . . ? C6 Re1 O5 174.5(3) . . ? C4 Re1 O5 94.0(3) . . ? C5 Re1 O6 173.4(4) . . ? C6 Re1 O6 100.5(3) . . ? C4 Re1 O6 95.8(3) . . ? O5 Re1 O6 74.4(2) . . ? C5 Re1 N3 93.3(3) . . ? C6 Re1 N3 95.3(3) . . ? C4 Re1 N3 176.1(3) . . ? O5 Re1 N3 82.1(2) . . ? O6 Re1 N3 83.8(2) . . ? C3 Re2 C2 87.0(4) . . ? C3 Re2 C1 89.9(5) . . ? C2 Re2 C1 86.8(4) . . ? C3 Re2 O4 94.4(3) . . ? C2 Re2 O4 173.2(3) . . ? C1 Re2 O4 99.8(3) . . ? C3 Re2 O3 95.6(4) . . ? C2 Re2 O3 97.8(3) . . ? C1 Re2 O3 173.0(3) . . ? O4 Re2 O3 75.5(2) . . ? C3 Re2 N1 175.8(4) . . ? C2 Re2 N1 96.2(4) . . ? C1 Re2 N1 93.1(4) . . ? O4 Re2 N1 82.2(2) . . ? O3 Re2 N1 81.2(3) . . ? C13 S3 C89 100.8(5) . . ? C32 S4 C33 104.1(5) . . ? C79 S5 C82 101.3(5) . . ? C10 O3 Re2 115.5(5) . . ? C11 O4 Re2 115.4(5) . . ? C8 O5 Re1 117.3(5) . . ? C7 O6 Re1 116.1(5) . . ? C12 O10 H10 109.5 . . ? C9 O11 H11 109.5 . . ? C32 N1 C31 104.6(7) . . ? C32 N1 Re2 128.9(6) . . ? C31 N1 Re2 126.5(6) . . ? C32 N2 C26 107.1(7) . . ? C32 N2 C25 125.2(7) . . ? C26 N2 C25 127.7(7) . . ? C13 N3 C73 106.4(6) . . ? C13 N3 Re1 127.1(5) . . ? C73 N3 Re1 126.5(5) . . ? C13 N4 C14 107.4(6) . . ? C13 N4 C16 124.5(7) . . ? C14 N4 C16 128.1(7) . . ? C79 N10 C78 106.8(7) . . ? C79 N10 C24 123.7(8) . . ? C78 N10 C24 129.2(8) . . ? C79 N11 C93 104.8(8) . . ? O23 C1 Re2 178.8(11) . . ? O2 C2 Re2 177.4(10) . . ? O1 C3 Re2 176.1(10) . . ? O7 C4 Re1 177.8(9) . . ? O9 C5 Re1 176.0(11) . . ? O8 C6 Re1 177.1(9) . . ? O6 C7 C12 124.2(7) . . ? O6 C7 C8 116.0(6) . . ? C12 C7 C8 119.8(6) . . ? O5 C8 C9 123.8(7) . . ? O5 C8 C7 115.2(6) . . ? C9 C8 C7 121.0(7) . . ? O11 C9 C10 121.0(7) . . ? O11 C9 C8 120.6(7) . . ? C10 C9 C8 118.4(7) . . ? O3 C10 C9 123.1(7) . . ? O3 C10 C11 115.6(7) . . ? C9 C10 C11 121.3(7) . . ? O4 C11 C12 123.1(7) . . ? O4 C11 C10 117.2(7) . . ? C12 C11 C10 119.7(7) . . ? O10 C12 C7 120.1(7) . . ? O10 C12 C11 120.2(7) . . ? C7 C12 C11 119.7(7) . . ? N3 C13 N4 110.5(6) . . ? N3 C13 S3 124.7(6) . . ? N4 C13 S3 124.6(6) . . ? N4 C14 C73 107.1(7) . . ? N4 C14 C74 131.7(8) . . ? C73 C14 C74 121.2(8) . . ? N4 C16 C17 113.7(7) . . ? N4 C16 H16A 108.8 . . ? C17 C16 H16A 108.8 . . ? N4 C16 H16B 108.8 . . ? C17 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C19 C17 C18 120.0(8) . . ? C19 C17 C16 121.6(7) . . ? C18 C17 C16 118.4(8) . . ? C23 C18 C17 119.1(8) . . ? C23 C18 C90 119.7(8) . . ? C17 C18 C90 121.1(8) . . ? C21 C19 C17 119.9(7) . . ? C21 C19 C20 120.1(8) . . ? C17 C19 C20 119.8(8) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 C22 120.8(8) . . ? C19 C21 C25 119.2(8) . . ? C22 C21 C25 119.7(8) . . ? C23 C22 C21 119.4(8) . . ? C23 C22 C100 121.2(9) . . ? C21 C22 C100 119.4(10) . . ? C22 C23 C18 120.7(8) . . ? C22 C23 C24 121.4(9) . . ? C18 C23 C24 117.8(9) . . ? N10 C24 C23 115.0(8) . . ? N10 C24 H24A 108.5 . . ? C23 C24 H24A 108.5 . . ? N10 C24 H24B 108.5 . . ? C23 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? N2 C25 C21 114.1(7) . . ? N2 C25 H25A 108.7 . . ? C21 C25 H25A 108.7 . . ? N2 C25 H25B 108.7 . . ? C21 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C27 C26 C31 123.4(9) . . ? C27 C26 N2 131.7(9) . . ? C31 C26 N2 104.8(8) . . ? C28 C27 C26 117.0(10) . . ? C28 C27 H27 121.5 . . ? C26 C27 H27 121.5 . . ? C27 C28 C29 120.7(11) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 122.7(10) . . ? C30 C29 H29 118.7 . . ? C28 C29 H29 118.7 . . ? C29 C30 C31 115.3(10) . . ? C29 C30 H30 122.4 . . ? C31 C30 H30 122.4 . . ? C26 C31 N1 110.6(8) . . ? C26 C31 C30 120.8(9) . . ? N1 C31 C30 128.6(9) . . ? N1 C32 N2 112.9(7) . . ? N1 C32 S4 122.8(7) . . ? N2 C32 S4 124.3(7) . . ? S4 C33 H33A 109.5 . . ? S4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? S4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C14 C73 C75 121.8(8) . . ? C14 C73 N3 108.5(7) . . ? C75 C73 N3 129.7(8) . . ? C84 C74 C14 116.9(8) . . ? C84 C74 H74 121.5 . . ? C14 C74 H74 121.5 . . ? C95 C75 C73 117.0(8) . . ? C95 C75 H75 121.5 . . ? C73 C75 H75 121.5 . . ? C94 C78 N10 135.7(9) . . ? C94 C78 C93 120.4(9) . . ? N10 C78 C93 103.9(8) . . ? N11 C79 N10 114.2(8) . . ? N11 C79 S5 126.9(7) . . ? N10 C79 S5 118.9(7) . . ? S5 C82 H82A 109.5 . . ? S5 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? S5 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C94 C83 C91 122.3(11) . . ? C94 C83 H83 118.9 . . ? C91 C83 H83 118.9 . . ? C74 C84 C95 121.2(9) . . ? C74 C84 H84 119.4 . . ? C95 C84 H84 119.4 . . ? S3 C89 H89A 109.5 . . ? S3 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? S3 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C18 C90 H90A 109.5 . . ? C18 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C18 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C92 C91 C83 120.0(11) . . ? C92 C91 H91 120.0 . . ? C83 C91 H91 120.0 . . ? C91 C92 C93 117.7(11) . . ? C91 C92 H92 121.1 . . ? C93 C92 H92 121.1 . . ? N11 C93 C92 129.1(10) . . ? N11 C93 C78 110.2(9) . . ? C92 C93 C78 120.6(10) . . ? C83 C94 C78 118.9(10) . . ? C83 C94 H94 120.6 . . ? C78 C94 H94 120.6 . . ? C75 C95 C84 121.8(9) . . ? C75 C95 H95 119.1 . . ? C84 C95 H95 119.1 . . ? C22 C100 H10A 109.5 . . ? C22 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C22 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C34 Re3 O14 C43 103.2(6) . . . . ? C35 Re3 O14 C43 -16(3) . . . . ? C36 Re3 O14 C43 -170.7(6) . . . . ? O15 Re3 O14 C43 9.0(5) . . . . ? N5 Re3 O14 C43 -74.9(5) . . . . ? C34 Re3 O15 C44 -102.1(7) . . . . ? C35 Re3 O15 C44 168.9(6) . . . . ? C36 Re3 O15 C44 -6(2) . . . . ? O14 Re3 O15 C44 -8.0(5) . . . . ? N5 Re3 O15 C44 76.4(6) . . . . ? C38 Re4 O16 C40 -32(5) . . . . ? C39 Re4 O16 C40 -173.1(6) . . . . ? C37 Re4 O16 C40 100.7(7) . . . . ? O17 Re4 O16 C40 7.6(6) . . . . ? N7 Re4 O16 C40 -75.1(6) . . . . ? C38 Re4 O17 C41 170.2(6) . . . . ? C39 Re4 O17 C41 -11(2) . . . . ? C37 Re4 O17 C41 -101.5(7) . . . . ? O16 Re4 O17 C41 -7.3(6) . . . . ? N7 Re4 O17 C41 78.2(6) . . . . ? C34 Re3 N5 C52 -103(9) . . . . ? C35 Re3 N5 C52 125.1(7) . . . . ? C36 Re3 N5 C52 36.3(7) . . . . ? O15 Re3 N5 C52 -136.3(7) . . . . ? O14 Re3 N5 C52 -61.1(7) . . . . ? C34 Re3 N5 C46 76(9) . . . . ? C35 Re3 N5 C46 -55.5(7) . . . . ? C36 Re3 N5 C46 -144.2(6) . . . . ? O15 Re3 N5 C46 43.2(6) . . . . ? O14 Re3 N5 C46 118.4(6) . . . . ? C38 Re4 N7 C54 -47.6(8) . . . . ? C39 Re4 N7 C54 -135.5(8) . . . . ? C37 Re4 N7 C54 59(7) . . . . ? O16 Re4 N7 C54 129.8(7) . . . . ? O17 Re4 N7 C54 54.5(7) . . . . ? C38 Re4 N7 C72 137.7(7) . . . . ? C39 Re4 N7 C72 49.7(7) . . . . ? C37 Re4 N7 C72 -115(7) . . . . ? O16 Re4 N7 C72 -45.0(7) . . . . ? O17 Re4 N7 C72 -120.2(7) . . . . ? C35 Re3 C34 O22 -96(13) . . . . ? C36 Re3 C34 O22 -7(13) . . . . ? O15 Re3 C34 O22 165(13) . . . . ? O14 Re3 C34 O22 90(13) . . . . ? N5 Re3 C34 O22 132(10) . . . . ? C34 Re3 C35 O12 10(100) . . . . ? C36 Re3 C35 O12 -76(100) . . . . ? O15 Re3 C35 O12 105(100) . . . . ? O14 Re3 C35 O12 129(100) . . . . ? N5 Re3 C35 O12 -172(100) . . . . ? C34 Re3 C36 O13 22(10) . . . . ? C35 Re3 C36 O13 110(10) . . . . ? O15 Re3 C36 O13 -75(11) . . . . ? O14 Re3 C36 O13 -73(10) . . . . ? N5 Re3 C36 O13 -156(10) . . . . ? C38 Re4 C37 O24 -54(27) . . . . ? C39 Re4 C37 O24 34(27) . . . . ? O16 Re4 C37 O24 129(27) . . . . ? O17 Re4 C37 O24 -156(27) . . . . ? N7 Re4 C37 O24 -161(22) . . . . ? C39 Re4 C38 O21 -45(36) . . . . ? C37 Re4 C38 O21 41(36) . . . . ? O16 Re4 C38 O21 173(32) . . . . ? O17 Re4 C38 O21 134(36) . . . . ? N7 Re4 C38 O21 -144(36) . . . . ? C38 Re4 C39 O20 133(10) . . . . ? C37 Re4 C39 O20 46(10) . . . . ? O16 Re4 C39 O20 -49(10) . . . . ? O17 Re4 C39 O20 -45(11) . . . . ? N7 Re4 C39 O20 -133(10) . . . . ? Re4 O16 C40 C45 176.0(6) . . . . ? Re4 O16 C40 C41 -6.9(9) . . . . ? Re4 O17 C41 C42 -174.0(6) . . . . ? Re4 O17 C41 C40 6.3(9) . . . . ? O16 C40 C41 O17 0.4(11) . . . . ? C45 C40 C41 O17 177.5(7) . . . . ? O16 C40 C41 C42 -179.3(7) . . . . ? C45 C40 C41 C42 -2.1(12) . . . . ? O17 C41 C42 O19 -4.3(13) . . . . ? C40 C41 C42 O19 175.4(8) . . . . ? O17 C41 C42 C43 178.5(8) . . . . ? C40 C41 C42 C43 -1.9(12) . . . . ? Re3 O14 C43 C42 175.9(6) . . . . ? Re3 O14 C43 C44 -8.9(8) . . . . ? O19 C42 C43 O14 1.3(13) . . . . ? C41 C42 C43 O14 178.6(7) . . . . ? O19 C42 C43 C44 -173.6(8) . . . . ? C41 C42 C43 C44 3.7(12) . . . . ? Re3 O15 C44 C45 -175.1(6) . . . . ? Re3 O15 C44 C43 6.2(9) . . . . ? O14 C43 C44 O15 1.9(10) . . . . ? C42 C43 C44 O15 177.1(7) . . . . ? O14 C43 C44 C45 -176.8(7) . . . . ? C42 C43 C44 C45 -1.7(12) . . . . ? O15 C44 C45 O18 0.1(13) . . . . ? C43 C44 C45 O18 178.8(7) . . . . ? O15 C44 C45 C40 178.9(7) . . . . ? C43 C44 C45 C40 -2.4(11) . . . . ? O16 C40 C45 O18 0.0(12) . . . . ? C41 C40 C45 O18 -176.9(7) . . . . ? O16 C40 C45 C44 -178.8(7) . . . . ? C41 C40 C45 C44 4.3(11) . . . . ? C52 N5 C46 C51 0.2(9) . . . . ? Re3 N5 C46 C51 -179.4(5) . . . . ? C52 N5 C46 C47 180.0(9) . . . . ? Re3 N5 C46 C47 0.4(12) . . . . ? C51 C46 C47 C48 1.0(13) . . . . ? N5 C46 C47 C48 -178.8(8) . . . . ? C46 C47 C48 C49 -0.1(15) . . . . ? C47 C48 C49 C50 -0.5(17) . . . . ? C48 C49 C50 C51 0.0(15) . . . . ? C52 N6 C51 C46 -0.7(8) . . . . ? C71 N6 C51 C46 177.7(7) . . . . ? C52 N6 C51 C50 -178.4(9) . . . . ? C71 N6 C51 C50 0.0(14) . . . . ? C47 C46 C51 N6 -179.5(7) . . . . ? N5 C46 C51 N6 0.3(9) . . . . ? C47 C46 C51 C50 -1.5(13) . . . . ? N5 C46 C51 C50 178.3(8) . . . . ? C49 C50 C51 N6 178.4(9) . . . . ? C49 C50 C51 C46 0.9(13) . . . . ? C46 N5 C52 N6 -0.6(9) . . . . ? Re3 N5 C52 N6 178.9(5) . . . . ? C46 N5 C52 S2 -175.5(6) . . . . ? Re3 N5 C52 S2 4.0(10) . . . . ? C51 N6 C52 N5 0.9(9) . . . . ? C71 N6 C52 N5 -177.6(7) . . . . ? C51 N6 C52 S2 175.9(6) . . . . ? C71 N6 C52 S2 -2.6(11) . . . . ? C53 S2 C52 N5 -117.9(8) . . . . ? C53 S2 C52 N6 67.7(7) . . . . ? C72 N7 C54 N8 -0.2(9) . . . . ? Re4 N7 C54 N8 -175.8(5) . . . . ? C72 N7 C54 S1 174.2(6) . . . . ? Re4 N7 C54 S1 -1.4(11) . . . . ? C56 N8 C54 N7 -0.9(9) . . . . ? C59 N8 C54 N7 178.9(7) . . . . ? C56 N8 C54 S1 -175.0(6) . . . . ? C59 N8 C54 S1 4.8(11) . . . . ? C55 S1 C54 N7 134.2(8) . . . . ? C55 S1 C54 N8 -52.2(9) . . . . ? C54 N8 C56 C57 -178.8(10) . . . . ? C59 N8 C56 C57 1.4(14) . . . . ? C54 N8 C56 C72 1.6(9) . . . . ? C59 N8 C56 C72 -178.3(7) . . . . ? N8 C56 C57 C58 -177.7(10) . . . . ? C72 C56 C57 C58 1.8(15) . . . . ? C56 C57 C58 C99 -0.8(19) . . . . ? C56 N8 C59 C60 41.0(10) . . . . ? C54 N8 C59 C60 -138.8(7) . . . . ? N8 C59 C60 C61 68.2(9) . . . . ? N8 C59 C60 C69 -119.5(8) . . . . ? C69 C60 C61 C63 1.2(11) . . . . ? C59 C60 C61 C63 173.3(7) . . . . ? C69 C60 C61 C62 -177.1(8) . . . . ? C59 C60 C61 C62 -5.0(11) . . . . ? C60 C61 C63 C64 0.1(11) . . . . ? C62 C61 C63 C64 178.4(8) . . . . ? C60 C61 C63 C71 -175.5(7) . . . . ? C62 C61 C63 C71 2.8(11) . . . . ? C61 C63 C64 C66 -0.1(11) . . . . ? C71 C63 C64 C66 175.5(7) . . . . ? C61 C63 C64 C65 -178.9(8) . . . . ? C71 C63 C64 C65 -3.3(11) . . . . ? C63 C64 C66 C69 -1.2(11) . . . . ? C65 C64 C66 C69 177.6(8) . . . . ? C63 C64 C66 C67 -176.3(7) . . . . ? C65 C64 C66 C67 2.6(11) . . . . ? C86 N9 C67 C66 -48.5(12) . . . . ? C76 N9 C67 C66 128.3(8) . . . . ? C69 C66 C67 N9 131.3(8) . . . . ? C64 C66 C67 N9 -53.6(11) . . . . ? C64 C66 C69 C60 2.5(11) . . . . ? C67 C66 C69 C60 177.5(7) . . . . ? C64 C66 C69 C70 -178.3(8) . . . . ? C67 C66 C69 C70 -3.2(12) . . . . ? C61 C60 C69 C66 -2.5(12) . . . . ? C59 C60 C69 C66 -174.6(7) . . . . ? C61 C60 C69 C70 178.3(8) . . . . ? C59 C60 C69 C70 6.2(12) . . . . ? C52 N6 C71 C63 133.5(8) . . . . ? C51 N6 C71 C63 -44.7(11) . . . . ? C61 C63 C71 N6 -62.5(10) . . . . ? C64 C63 C71 N6 121.8(8) . . . . ? N8 C56 C72 C88 178.4(9) . . . . ? C57 C56 C72 C88 -1.3(14) . . . . ? N8 C56 C72 N7 -1.7(9) . . . . ? C57 C56 C72 N7 178.6(8) . . . . ? C54 N7 C72 C88 -178.9(10) . . . . ? Re4 N7 C72 C88 -3.1(14) . . . . ? C54 N7 C72 C56 1.2(9) . . . . ? Re4 N7 C72 C56 177.0(5) . . . . ? C86 N9 C76 C101 1.1(10) . . . . ? C67 N9 C76 C101 -176.2(8) . . . . ? C86 N9 C76 C96 -179.8(9) . . . . ? C67 N9 C76 C96 2.9(14) . . . . ? C76 N9 C86 N12 -0.6(10) . . . . ? C67 N9 C86 N12 176.5(8) . . . . ? C76 N9 C86 S6 -178.1(7) . . . . ? C67 N9 C86 S6 -0.9(13) . . . . ? C101 N12 C86 N9 -0.1(11) . . . . ? C101 N12 C86 S6 177.5(7) . . . . ? C104 S6 C86 N9 178.1(9) . . . . ? C104 S6 C86 N12 0.9(10) . . . . ? C56 C72 C88 C99 -0.3(16) . . . . ? N7 C72 C88 C99 179.8(11) . . . . ? N9 C76 C96 C97 -175.9(9) . . . . ? C101 C76 C96 C97 3.1(13) . . . . ? C76 C96 C97 C103 -1.0(17) . . . . ? C72 C88 C99 C58 1(2) . . . . ? C57 C58 C99 C88 -1(2) . . . . ? N9 C76 C101 N12 -1.1(11) . . . . ? C96 C76 C101 N12 179.6(8) . . . . ? N9 C76 C101 C98 176.6(9) . . . . ? C96 C76 C101 C98 -2.7(15) . . . . ? C86 N12 C101 C76 0.8(12) . . . . ? C86 N12 C101 C98 -176.6(11) . . . . ? C103 C98 C101 C76 -0.1(17) . . . . ? C103 C98 C101 N12 177.1(12) . . . . ? C96 C97 C103 C98 -2(2) . . . . ? C101 C98 C103 C97 2(2) . . . . ? C3 Re2 O3 C10 101.2(6) . . . . ? C2 Re2 O3 C10 -171.1(6) . . . . ? C1 Re2 O3 C10 -40(3) . . . . ? O4 Re2 O3 C10 8.1(6) . . . . ? N1 Re2 O3 C10 -76.0(6) . . . . ? C3 Re2 O4 C11 -102.0(6) . . . . ? C2 Re2 O4 C11 -1(3) . . . . ? C1 Re2 O4 C11 167.3(6) . . . . ? O3 Re2 O4 C11 -7.4(6) . . . . ? N1 Re2 O4 C11 75.5(6) . . . . ? C5 Re1 O5 C8 169.0(6) . . . . ? C6 Re1 O5 C8 14(3) . . . . ? C4 Re1 O5 C8 -103.8(6) . . . . ? O6 Re1 O5 C8 -8.8(5) . . . . ? N3 Re1 O5 C8 76.9(5) . . . . ? C5 Re1 O6 C7 -12(3) . . . . ? C6 Re1 O6 C7 -170.5(6) . . . . ? C4 Re1 O6 C7 99.8(6) . . . . ? O5 Re1 O6 C7 7.3(5) . . . . ? N3 Re1 O6 C7 -76.3(5) . . . . ? C3 Re2 N1 C32 88(5) . . . . ? C2 Re2 N1 C32 -133.2(8) . . . . ? C1 Re2 N1 C32 -46.1(8) . . . . ? O4 Re2 N1 C32 53.4(7) . . . . ? O3 Re2 N1 C32 129.8(7) . . . . ? C3 Re2 N1 C31 -93(5) . . . . ? C2 Re2 N1 C31 45.9(7) . . . . ? C1 Re2 N1 C31 133.0(7) . . . . ? O4 Re2 N1 C31 -127.5(7) . . . . ? O3 Re2 N1 C31 -51.1(7) . . . . ? C5 Re1 N3 C13 125.0(7) . . . . ? C6 Re1 N3 C13 39.1(7) . . . . ? C4 Re1 N3 C13 -146(5) . . . . ? O5 Re1 N3 C13 -136.0(6) . . . . ? O6 Re1 N3 C13 -60.9(6) . . . . ? C5 Re1 N3 C73 -52.8(7) . . . . ? C6 Re1 N3 C73 -138.7(7) . . . . ? C4 Re1 N3 C73 36(5) . . . . ? O5 Re1 N3 C73 46.2(6) . . . . ? O6 Re1 N3 C73 121.3(6) . . . . ? C3 Re2 C1 O23 -17(47) . . . . ? C2 Re2 C1 O23 -104(47) . . . . ? O4 Re2 C1 O23 77(47) . . . . ? O3 Re2 C1 O23 124(45) . . . . ? N1 Re2 C1 O23 160(46) . . . . ? C3 Re2 C2 O2 25(22) . . . . ? C1 Re2 C2 O2 115(22) . . . . ? O4 Re2 C2 O2 -77(23) . . . . ? O3 Re2 C2 O2 -71(22) . . . . ? N1 Re2 C2 O2 -153(22) . . . . ? C2 Re2 C3 O1 106(14) . . . . ? C1 Re2 C3 O1 19(14) . . . . ? O4 Re2 C3 O1 -81(14) . . . . ? O3 Re2 C3 O1 -157(14) . . . . ? N1 Re2 C3 O1 -116(13) . . . . ? C5 Re1 C4 O7 -19(26) . . . . ? C6 Re1 C4 O7 67(26) . . . . ? O5 Re1 C4 O7 -118(26) . . . . ? O6 Re1 C4 O7 167(26) . . . . ? N3 Re1 C4 O7 -108(24) . . . . ? C6 Re1 C5 O9 -16(14) . . . . ? C4 Re1 C5 O9 73(14) . . . . ? O5 Re1 C5 O9 167(14) . . . . ? O6 Re1 C5 O9 -174(12) . . . . ? N3 Re1 C5 O9 -111(14) . . . . ? C5 Re1 C6 O8 11(18) . . . . ? C4 Re1 C6 O8 -75(18) . . . . ? O5 Re1 C6 O8 167(16) . . . . ? O6 Re1 C6 O8 -171(18) . . . . ? N3 Re1 C6 O8 104(18) . . . . ? Re1 O6 C7 C12 177.4(6) . . . . ? Re1 O6 C7 C8 -5.3(8) . . . . ? Re1 O5 C8 C9 -171.0(6) . . . . ? Re1 O5 C8 C7 9.0(8) . . . . ? O6 C7 C8 O5 -2.4(10) . . . . ? C12 C7 C8 O5 175.1(7) . . . . ? O6 C7 C8 C9 177.5(7) . . . . ? C12 C7 C8 C9 -5.0(11) . . . . ? O5 C8 C9 O11 2.3(12) . . . . ? C7 C8 C9 O11 -177.7(7) . . . . ? O5 C8 C9 C10 -176.2(7) . . . . ? C7 C8 C9 C10 3.9(11) . . . . ? Re2 O3 C10 C9 172.1(6) . . . . ? Re2 O3 C10 C11 -7.7(9) . . . . ? O11 C9 C10 O3 -0.3(13) . . . . ? C8 C9 C10 O3 178.2(8) . . . . ? O11 C9 C10 C11 179.5(7) . . . . ? C8 C9 C10 C11 -2.0(12) . . . . ? Re2 O4 C11 C12 -173.9(6) . . . . ? Re2 O4 C11 C10 5.9(9) . . . . ? O3 C10 C11 O4 1.2(11) . . . . ? C9 C10 C11 O4 -178.5(8) . . . . ? O3 C10 C11 C12 -179.0(8) . . . . ? C9 C10 C11 C12 1.2(12) . . . . ? O6 C7 C12 O10 -0.3(13) . . . . ? C8 C7 C12 O10 -177.5(7) . . . . ? O6 C7 C12 C11 -178.7(7) . . . . ? C8 C7 C12 C11 4.1(12) . . . . ? O4 C11 C12 O10 -1.0(13) . . . . ? C10 C11 C12 O10 179.3(7) . . . . ? O4 C11 C12 C7 177.4(8) . . . . ? C10 C11 C12 C7 -2.3(12) . . . . ? C73 N3 C13 N4 -2.7(9) . . . . ? Re1 N3 C13 N4 179.1(5) . . . . ? C73 N3 C13 S3 -178.0(6) . . . . ? Re1 N3 C13 S3 3.9(10) . . . . ? C14 N4 C13 N3 3.6(9) . . . . ? C16 N4 C13 N3 -177.9(7) . . . . ? C14 N4 C13 S3 178.9(6) . . . . ? C16 N4 C13 S3 -2.6(11) . . . . ? C89 S3 C13 N3 -113.0(8) . . . . ? C89 S3 C13 N4 72.4(8) . . . . ? C13 N4 C14 C73 -3.0(9) . . . . ? C16 N4 C14 C73 178.6(8) . . . . ? C13 N4 C14 C74 178.7(10) . . . . ? C16 N4 C14 C74 0.2(16) . . . . ? C13 N4 C16 C17 130.1(8) . . . . ? C14 N4 C16 C17 -51.8(11) . . . . ? N4 C16 C17 C19 -58.8(10) . . . . ? N4 C16 C17 C18 124.2(8) . . . . ? C19 C17 C18 C23 0.1(12) . . . . ? C16 C17 C18 C23 177.2(7) . . . . ? C19 C17 C18 C90 -176.7(8) . . . . ? C16 C17 C18 C90 0.3(12) . . . . ? C18 C17 C19 C21 1.4(12) . . . . ? C16 C17 C19 C21 -175.6(7) . . . . ? C18 C17 C19 C20 176.7(8) . . . . ? C16 C17 C19 C20 -0.3(11) . . . . ? C17 C19 C21 C22 -2.5(12) . . . . ? C20 C19 C21 C22 -177.8(8) . . . . ? C17 C19 C21 C25 172.0(7) . . . . ? C20 C19 C21 C25 -3.3(12) . . . . ? C19 C21 C22 C23 2.1(13) . . . . ? C25 C21 C22 C23 -172.3(8) . . . . ? C19 C21 C22 C100 -176.3(9) . . . . ? C25 C21 C22 C100 9.2(13) . . . . ? C21 C22 C23 C18 -0.6(13) . . . . ? C100 C22 C23 C18 177.8(10) . . . . ? C21 C22 C23 C24 177.2(9) . . . . ? C100 C22 C23 C24 -4.4(15) . . . . ? C17 C18 C23 C22 -0.5(13) . . . . ? C90 C18 C23 C22 176.4(9) . . . . ? C17 C18 C23 C24 -178.3(8) . . . . ? C90 C18 C23 C24 -1.4(13) . . . . ? C79 N10 C24 C23 158.6(9) . . . . ? C78 N10 C24 C23 -27.6(16) . . . . ? C22 C23 C24 N10 112.8(11) . . . . ? C18 C23 C24 N10 -69.4(13) . . . . ? C32 N2 C25 C21 -135.2(8) . . . . ? C26 N2 C25 C21 44.3(12) . . . . ? C19 C21 C25 N2 68.5(10) . . . . ? C22 C21 C25 N2 -116.9(9) . . . . ? C32 N2 C26 C27 -176.8(10) . . . . ? C25 N2 C26 C27 3.5(16) . . . . ? C32 N2 C26 C31 0.2(9) . . . . ? C25 N2 C26 C31 -179.4(8) . . . . ? C31 C26 C27 C28 2.4(16) . . . . ? N2 C26 C27 C28 178.9(10) . . . . ? C26 C27 C28 C29 1.8(18) . . . . ? C27 C28 C29 C30 -5(2) . . . . ? C28 C29 C30 C31 3.1(17) . . . . ? C27 C26 C31 N1 177.4(9) . . . . ? N2 C26 C31 N1 0.1(10) . . . . ? C27 C26 C31 C30 -3.8(15) . . . . ? N2 C26 C31 C30 178.8(8) . . . . ? C32 N1 C31 C26 -0.4(10) . . . . ? Re2 N1 C31 C26 -179.6(6) . . . . ? C32 N1 C31 C30 -179.0(9) . . . . ? Re2 N1 C31 C30 1.8(13) . . . . ? C29 C30 C31 C26 1.0(14) . . . . ? C29 C30 C31 N1 179.4(9) . . . . ? C31 N1 C32 N2 0.5(9) . . . . ? Re2 N1 C32 N2 179.7(5) . . . . ? C31 N1 C32 S4 176.7(6) . . . . ? Re2 N1 C32 S4 -4.1(11) . . . . ? C26 N2 C32 N1 -0.5(10) . . . . ? C25 N2 C32 N1 179.2(7) . . . . ? C26 N2 C32 S4 -176.6(6) . . . . ? C25 N2 C32 S4 3.1(12) . . . . ? C33 S4 C32 N1 120.4(8) . . . . ? C33 S4 C32 N2 -63.8(9) . . . . ? N4 C14 C73 C75 -179.9(8) . . . . ? C74 C14 C73 C75 -1.4(14) . . . . ? N4 C14 C73 N3 1.4(9) . . . . ? C74 C14 C73 N3 179.9(8) . . . . ? C13 N3 C73 C14 0.8(9) . . . . ? Re1 N3 C73 C14 178.9(5) . . . . ? C13 N3 C73 C75 -177.8(9) . . . . ? Re1 N3 C73 C75 0.4(13) . . . . ? N4 C14 C74 C84 179.0(10) . . . . ? C73 C14 C74 C84 0.9(15) . . . . ? C14 C73 C75 C95 1.5(15) . . . . ? N3 C73 C75 C95 180.0(10) . . . . ? C79 N10 C78 C94 -178.2(11) . . . . ? C24 N10 C78 C94 7.1(18) . . . . ? C79 N10 C78 C93 -0.6(9) . . . . ? C24 N10 C78 C93 -175.3(9) . . . . ? C93 N11 C79 N10 -0.1(10) . . . . ? C93 N11 C79 S5 179.4(7) . . . . ? C78 N10 C79 N11 0.5(10) . . . . ? C24 N10 C79 N11 175.5(9) . . . . ? C78 N10 C79 S5 -179.0(6) . . . . ? C24 N10 C79 S5 -4.0(12) . . . . ? C82 S5 C79 N11 -3.2(10) . . . . ? C82 S5 C79 N10 176.3(8) . . . . ? C14 C74 C84 C95 -0.6(17) . . . . ? C94 C83 C91 C92 1.1(18) . . . . ? C83 C91 C92 C93 2.7(17) . . . . ? C79 N11 C93 C92 177.4(10) . . . . ? C79 N11 C93 C78 -0.3(10) . . . . ? C91 C92 C93 N11 179.0(10) . . . . ? C91 C92 C93 C78 -3.6(15) . . . . ? C94 C78 C93 N11 178.6(9) . . . . ? N10 C78 C93 N11 0.6(10) . . . . ? C94 C78 C93 C92 0.7(14) . . . . ? N10 C78 C93 C92 -177.3(9) . . . . ? C91 C83 C94 C78 -4.0(16) . . . . ? N10 C78 C94 C83 -179.6(10) . . . . ? C93 C78 C94 C83 3.1(15) . . . . ? C73 C75 C95 C84 -1.3(18) . . . . ? C74 C84 C95 C75 1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.264 _refine_diff_density_min -1.398 _refine_diff_density_rms 0.197 _iucr_refine_instructions_details ; TITL RK5-79- in P-1 New: P-1 CELL 0.71073 12.8639 21.2643 21.5350 107.672 90.280 100.230 ZERR 4 0.0002 0.0004 0.0004 0.002 0.001 0.002 LATT 1 SFAC C H N O Re S UNIT 192 152 24 48 8 12 FMAP 2 MERG 2 PLAN -20 ACTA omit 0 -3 4 omit -1 1 3 omit 0 0 3 omit 0 -1 4 omit 0 -2 4 omit 0 -4 4 omit 0 -4 6 omit 0 -3 2 omit 0 -5 5 omit -2 0 1 omit -1 -2 2 omit 0 -4 3 omit -1 -4 2 omit 0 2 2 omit -2 -1 1 omit 4 0 1 omit 1 -5 3 omit -3 -2 2 omit -1 -6 4 ACTA 50.0 L.S. 20 BOND $H CONF WGHT 0.090300 14.554800 FVAR 5.06901 RE3 5 -0.213064 0.722500 0.081350 11.00000 0.02641 0.06454 = 0.03773 0.02124 0.00117 0.01137 RE4 5 0.309659 0.627059 -0.102165 11.00000 0.03465 0.09464 = 0.03252 0.01742 0.00601 0.01840 S1 6 0.284403 0.517322 -0.000921 11.00000 0.05189 0.06080 = 0.04363 0.00461 -0.00033 0.00154 S2 6 -0.162823 0.606449 0.168001 11.00000 0.03584 0.05178 = 0.04911 0.01735 -0.00208 -0.00003 S6 6 0.427427 0.841069 0.351104 11.00000 0.10435 0.09827 = 0.10045 0.05146 -0.00235 -0.00678 O12 4 -0.282486 0.853275 0.156487 11.00000 0.07439 0.06341 = 0.10353 0.03589 0.01712 0.02499 O13 4 -0.399822 0.645707 0.131529 11.00000 0.03312 0.07719 = 0.06503 0.01913 0.01271 0.00653 O14 4 -0.144977 0.637499 0.028705 11.00000 0.02815 0.07113 = 0.04162 0.01808 0.00582 0.00514 O15 4 -0.078506 0.762882 0.038002 11.00000 0.04031 0.06347 = 0.04679 0.02129 0.00628 0.01634 O16 4 0.225008 0.707607 -0.067525 11.00000 0.03614 0.08215 = 0.05629 0.03192 0.01531 0.01279 O17 4 0.158869 0.582142 -0.078232 11.00000 0.03414 0.07844 = 0.05132 0.00764 0.01270 0.02146 O18 4 0.111215 0.807474 -0.013263 11.00000 0.05330 0.06698 = 0.06253 0.02667 0.02326 0.01162 AFIX 3 H18 2 0.069345 0.830864 0.005167 11.00000 -1.50000 AFIX 0 O19 4 -0.036780 0.536033 -0.034922 11.00000 0.05535 0.06073 = 0.09627 0.01751 0.01295 0.01465 AFIX 3 H19 2 0.004710 0.513183 -0.054812 11.00000 -1.50000 AFIX 0 O20 4 0.504604 0.716475 -0.133391 11.00000 0.05414 0.16343 = 0.09113 0.08105 0.02448 0.02080 O21 4 0.424999 0.508793 -0.145830 11.00000 0.07113 0.11148 = 0.09247 -0.00505 0.01485 0.04021 O22 4 -0.377191 0.706188 -0.026479 11.00000 0.07995 0.21317 = 0.08060 0.05501 -0.03155 0.03816 O24 4 0.247710 0.597176 -0.245645 11.00000 0.10896 0.32290 = 0.04564 0.05709 -0.01548 0.02785 N5 3 -0.091515 0.730970 0.157837 11.00000 0.03186 0.04917 = 0.04410 0.02132 -0.00107 0.00928 N6 3 0.003070 0.707502 0.231352 11.00000 0.02652 0.04599 = 0.04153 0.01778 -0.00371 0.00679 N7 3 0.345606 0.645790 0.003117 11.00000 0.04301 0.07175 = 0.03288 0.01319 0.00347 0.00487 N8 3 0.358649 0.633919 0.101043 11.00000 0.03463 0.05247 = 0.03370 0.01187 -0.00036 -0.00037 N9 3 0.384950 0.775061 0.439687 11.00000 0.04740 0.04909 = 0.04226 0.01097 -0.01061 0.00544 N12 3 0.386337 0.885885 0.476352 11.00000 0.08442 0.06039 = 0.10486 0.00273 -0.03088 0.00464 C34 1 -0.311880 0.714335 0.012904 11.00000 0.04389 0.12795 = 0.04845 0.03287 -0.00174 0.02617 C35 1 -0.255833 0.803884 0.128291 11.00000 0.04512 0.06092 = 0.05858 0.03454 -0.00021 0.01387 C36 1 -0.328264 0.675317 0.115313 11.00000 0.03426 0.06272 = 0.04921 0.02044 -0.00025 0.01617 C37 1 0.267350 0.608078 -0.192394 11.00000 0.05426 0.15551 = 0.05439 0.02589 -0.00593 0.01259 C38 1 0.381270 0.552800 -0.128648 11.00000 0.05198 0.10941 = 0.04529 0.00342 0.00156 0.02156 C39 1 0.434877 0.681370 -0.119805 11.00000 0.04986 0.12320 = 0.04224 0.03615 0.00851 0.03216 C40 1 0.136721 0.694633 -0.043314 11.00000 0.03483 0.06992 = 0.03577 0.02559 -0.00004 0.00686 C41 1 0.098899 0.622018 -0.049872 11.00000 0.03615 0.07357 = 0.04328 0.02089 -0.00459 0.01204 C42 1 0.002231 0.600958 -0.025836 11.00000 0.02903 0.06418 = 0.05111 0.01275 0.00145 0.00872 C43 1 -0.054044 0.651214 0.005818 11.00000 0.03157 0.06106 = 0.04112 0.01555 -0.00725 -0.00032 C44 1 -0.016948 0.722524 0.010141 11.00000 0.04072 0.05647 = 0.03330 0.01668 0.00193 0.00824 C45 1 0.075340 0.742572 -0.015209 11.00000 0.03423 0.06387 = 0.03641 0.02064 0.00575 0.01087 C46 1 -0.007691 0.785242 0.184372 11.00000 0.02589 0.04891 = 0.04064 0.01689 0.00507 0.00699 C47 1 0.019962 0.845503 0.170779 11.00000 0.04591 0.05013 = 0.05320 0.02384 -0.00797 0.01026 AFIX 43 H47 2 -0.019690 0.856066 0.140412 11.00000 -1.20000 AFIX 0 C48 1 0.109992 0.889552 0.204749 11.00000 0.06189 0.05264 = 0.07023 0.02838 -0.00324 -0.00112 AFIX 43 H48 2 0.131170 0.930483 0.196952 11.00000 -1.20000 AFIX 0 C49 1 0.168555 0.873275 0.250052 11.00000 0.05210 0.04603 = 0.07545 0.02038 -0.01435 -0.00449 AFIX 43 H49 2 0.228481 0.903664 0.271620 11.00000 -1.20000 AFIX 0 C50 1 0.140684 0.813037 0.264315 11.00000 0.03828 0.05432 = 0.05784 0.02289 -0.01205 0.00023 AFIX 43 H50 2 0.180063 0.802317 0.294695 11.00000 -1.20000 AFIX 0 C51 1 0.050378 0.769959 0.230322 11.00000 0.03137 0.04675 = 0.04333 0.01528 -0.00132 0.01133 C52 1 -0.082532 0.686879 0.186972 11.00000 0.02792 0.04570 = 0.04021 0.01414 0.00225 0.00259 C53 1 -0.225365 0.611619 0.244279 11.00000 0.05472 0.07531 = 0.06291 0.02712 0.00932 0.00031 AFIX 137 H53A 2 -0.263004 0.567908 0.242818 11.00000 -1.50000 H53B 2 -0.273962 0.642132 0.250611 11.00000 -1.50000 H53C 2 -0.172218 0.627551 0.279765 11.00000 -1.50000 AFIX 0 C54 1 0.335363 0.603472 0.035986 11.00000 0.03365 0.05702 = 0.03215 0.00897 0.00183 0.00295 C55 1 0.372502 0.473063 0.028465 11.00000 0.07772 0.08700 = 0.08422 0.01318 -0.00356 0.03373 AFIX 137 H55A 2 0.336809 0.452191 0.058221 11.00000 -1.50000 H55B 2 0.434573 0.504353 0.050523 11.00000 -1.50000 H55C 2 0.392653 0.439271 -0.007830 11.00000 -1.50000 AFIX 0 C56 1 0.387410 0.700811 0.110354 11.00000 0.02900 0.05218 = 0.03948 0.01086 0.00066 -0.00070 C57 1 0.420470 0.755275 0.165504 11.00000 0.07408 0.06971 = 0.04845 0.01581 0.00564 -0.01038 AFIX 43 H57 2 0.428942 0.749645 0.206282 11.00000 -1.20000 AFIX 0 C58 1 0.440165 0.817644 0.157648 11.00000 0.11732 0.06310 = 0.05882 0.01239 0.00718 -0.00080 AFIX 43 H58 2 0.461650 0.855219 0.193896 11.00000 -1.20000 AFIX 0 C59 1 0.352657 0.598658 0.152477 11.00000 0.03268 0.05237 = 0.03669 0.01936 0.00275 0.00553 AFIX 23 H59A 2 0.309817 0.554096 0.134571 11.00000 -1.20000 H59B 2 0.423299 0.593399 0.163159 11.00000 -1.20000 AFIX 0 C60 1 0.306684 0.635246 0.214079 11.00000 0.03122 0.04155 = 0.03203 0.01552 0.00086 -0.00054 C61 1 0.199611 0.639782 0.212669 11.00000 0.03218 0.04185 = 0.02998 0.01811 -0.00234 0.00208 C62 1 0.133753 0.613230 0.148920 11.00000 0.03811 0.07977 = 0.03496 0.00554 -0.00274 0.00697 AFIX 137 H62A 2 0.158663 0.575068 0.120943 11.00000 -1.50000 H62B 2 0.139553 0.647670 0.128156 11.00000 -1.50000 H62C 2 0.061074 0.600030 0.157036 11.00000 -1.50000 AFIX 0 C63 1 0.154399 0.667442 0.271073 11.00000 0.02419 0.04157 = 0.04046 0.02049 -0.00228 0.00384 C64 1 0.215418 0.690942 0.331374 11.00000 0.03378 0.03415 = 0.03606 0.01498 0.00538 0.00742 C65 1 0.166634 0.719584 0.394298 11.00000 0.04083 0.06522 = 0.04112 0.00867 0.00015 0.01488 AFIX 137 H65A 2 0.184608 0.767747 0.407533 11.00000 -1.50000 H65B 2 0.192932 0.703629 0.427362 11.00000 -1.50000 H65C 2 0.091098 0.705732 0.388325 11.00000 -1.50000 AFIX 0 C66 1 0.322953 0.686074 0.332060 11.00000 0.03213 0.04049 = 0.03012 0.01478 -0.00207 0.00430 C67 1 0.387152 0.707017 0.396444 11.00000 0.04433 0.06370 = 0.04057 0.01263 -0.00749 0.02050 AFIX 23 H67A 2 0.361583 0.675255 0.419623 11.00000 -1.20000 H67B 2 0.460150 0.703752 0.387450 11.00000 -1.20000 AFIX 0 C69 1 0.369356 0.657014 0.273716 11.00000 0.02739 0.04784 = 0.04083 0.01597 -0.00208 0.00558 C70 1 0.485340 0.650249 0.275367 11.00000 0.02980 0.09737 = 0.04379 0.01211 0.00241 0.01350 AFIX 137 H70A 2 0.490113 0.606311 0.277244 11.00000 -1.50000 H70B 2 0.522610 0.683638 0.313191 11.00000 -1.50000 H70C 2 0.516290 0.656538 0.236703 11.00000 -1.50000 AFIX 0 C71 1 0.036959 0.667769 0.270520 11.00000 0.02704 0.05925 = 0.04341 0.02468 0.00196 0.00596 AFIX 23 H71A 2 -0.001222 0.621820 0.253405 11.00000 -1.20000 H71B 2 0.017804 0.685704 0.315091 11.00000 -1.20000 AFIX 0 C72 1 0.377602 0.709012 0.049176 11.00000 0.04114 0.06103 = 0.04415 0.02305 0.00546 0.00294 C76 1 0.361122 0.789622 0.504305 11.00000 0.04589 0.05972 = 0.05403 0.00470 -0.01616 0.01575 C86 1 0.400141 0.833119 0.424560 11.00000 0.04726 0.05203 = 0.07229 0.01304 -0.02029 -0.01038 C88 1 0.398712 0.772235 0.041952 11.00000 0.08172 0.08163 = 0.05297 0.03199 0.00258 -0.00022 AFIX 43 H88 2 0.392804 0.778393 0.001221 11.00000 -1.20000 AFIX 0 C96 1 0.337883 0.745336 0.545616 11.00000 0.05323 0.07135 = 0.01733 0.01197 0.01140 0.03203 AFIX 43 H96 2 0.341152 0.699872 0.531694 11.00000 -1.20000 AFIX 0 C97 1 0.310174 0.779532 0.608522 11.00000 0.09292 0.10263 = 0.07789 0.02453 0.01359 0.02890 AFIX 43 H97 2 0.293237 0.755091 0.637496 11.00000 -1.20000 AFIX 0 C98 1 0.332995 0.886971 0.590800 11.00000 0.06261 0.09917 = 0.10309 -0.01294 -0.00878 0.03599 AFIX 43 H98 2 0.332319 0.932721 0.606866 11.00000 -1.20000 AFIX 0 C99 1 0.428946 0.825905 0.097702 11.00000 0.12576 0.05413 = 0.06801 0.03116 -0.00943 -0.00850 AFIX 43 H99 2 0.442128 0.869158 0.094353 11.00000 -1.20000 AFIX 0 C101 1 0.360654 0.857669 0.526817 11.00000 0.07081 0.06261 = 0.04942 0.00333 -0.01340 0.01219 C103 1 0.306866 0.845429 0.628954 11.00000 0.08802 0.14348 = 0.07973 0.02566 0.01814 0.03747 AFIX 43 H103 2 0.285961 0.863950 0.670827 11.00000 -1.20000 AFIX 0 C104 1 0.432460 0.926135 0.365093 11.00000 0.05792 0.17229 = 0.28336 0.17085 -0.00263 -0.00186 AFIX 137 H10D 2 0.445536 0.949358 0.410990 11.00000 -1.50000 H10E 2 0.366220 0.933157 0.350281 11.00000 -1.50000 H10F 2 0.488418 0.943083 0.341770 11.00000 -1.50000 AFIX 0 RE1 5 0.210089 0.171359 0.606102 11.00000 0.04974 0.03168 = 0.03515 0.01524 -0.00104 0.00574 RE2 5 0.286954 0.489333 0.469521 11.00000 0.05302 0.03719 = 0.05662 0.02699 0.00745 0.00339 S3 6 -0.059144 0.134877 0.529753 11.00000 0.04602 0.04736 = 0.05391 0.01546 0.01349 0.01420 S4 6 0.007054 0.414612 0.425948 11.00000 0.05282 0.05484 = 0.06966 0.01655 0.00828 0.01800 S5 6 -0.197128 -0.079369 0.026677 11.00000 0.05897 0.07227 = 0.05687 0.00994 -0.00635 0.01179 O1 4 0.393159 0.608283 0.584897 11.00000 0.08788 0.06723 = 0.08411 0.01153 -0.01069 0.00106 O2 4 0.446150 0.543931 0.386222 11.00000 0.09663 0.08596 = 0.09779 0.05878 0.03287 -0.00623 O3 4 0.371098 0.416086 0.485976 11.00000 0.04669 0.05600 = 0.06094 0.03713 0.01371 0.00851 O4 4 0.187185 0.442574 0.529506 11.00000 0.04794 0.04068 = 0.05952 0.02782 0.00891 0.01054 O5 4 0.325167 0.233606 0.567297 11.00000 0.04117 0.03945 = 0.04887 0.02022 -0.00184 0.00520 O6 4 0.139905 0.256806 0.606370 11.00000 0.04863 0.03247 = 0.04060 0.01748 0.01319 0.01071 O7 4 0.309999 0.229297 0.745232 11.00000 0.11782 0.08849 = 0.04964 0.02056 -0.02503 -0.01810 O8 4 0.033896 0.088060 0.657231 11.00000 0.08442 0.07314 = 0.08870 0.05380 0.01952 -0.00357 O9 4 0.320699 0.054871 0.596719 11.00000 0.09210 0.06350 = 0.15216 0.02396 -0.03691 0.03391 O10 4 0.061128 0.367320 0.595585 11.00000 0.05712 0.05830 = 0.08852 0.04260 0.03458 0.02804 AFIX 3 H10 2 0.050768 0.401380 0.588165 11.00000 -1.50000 AFIX 0 O11 4 0.450010 0.306853 0.498551 11.00000 0.03891 0.07129 = 0.07114 0.04046 0.01447 0.01807 AFIX 3 H11 2 0.476220 0.334063 0.480331 11.00000 -1.50000 AFIX 0 O23 4 0.144548 0.580058 0.442894 11.00000 0.10086 0.07061 = 0.11726 0.06009 0.00437 0.03245 N1 3 0.207113 0.400979 0.391830 11.00000 0.04536 0.04561 = 0.05422 0.02548 0.00900 0.00848 N2 3 0.083072 0.321721 0.325806 11.00000 0.05571 0.04596 = 0.04658 0.01787 0.00427 0.00666 N3 3 0.148145 0.131922 0.503759 11.00000 0.03613 0.03622 = 0.03386 0.00925 0.00311 0.01534 N4 3 0.037874 0.095587 0.414649 11.00000 0.03887 0.04236 = 0.03896 0.01164 -0.00319 0.01016 N10 3 -0.038922 0.007964 0.106341 11.00000 0.05416 0.05335 = 0.04381 0.01066 -0.00365 0.01764 N11 3 0.016812 -0.077391 0.034803 11.00000 0.04791 0.05625 = 0.06323 0.02034 0.00680 0.01087 C1 1 0.197018 0.545956 0.452078 11.00000 0.07757 0.03974 = 0.07628 0.03592 0.00493 0.00240 C2 1 0.385572 0.523008 0.415827 11.00000 0.06723 0.05368 = 0.06336 0.03210 0.01131 0.00265 C3 1 0.356062 0.562188 0.541260 11.00000 0.06539 0.05639 = 0.07114 0.02557 0.01079 0.00856 C4 1 0.272355 0.208927 0.693366 11.00000 0.07920 0.04863 = 0.04085 0.02241 -0.00317 0.00763 C5 1 0.281839 0.099284 0.598803 11.00000 0.06264 0.05037 = 0.07078 0.02086 -0.01104 0.01218 C6 1 0.097373 0.119978 0.638178 11.00000 0.07056 0.04663 = 0.04439 0.02425 0.00651 0.01306 C7 1 0.190448 0.297015 0.578560 11.00000 0.04053 0.03146 = 0.03564 0.01447 0.00163 0.00256 C8 1 0.296733 0.282664 0.554781 11.00000 0.04512 0.03113 = 0.03532 0.01398 0.00139 0.00913 C9 1 0.356674 0.321464 0.521701 11.00000 0.03434 0.04231 = 0.04658 0.01798 0.00546 0.00991 C10 1 0.320080 0.376109 0.514373 11.00000 0.03429 0.03522 = 0.05138 0.02271 0.00556 -0.00182 C11 1 0.215883 0.392332 0.539491 11.00000 0.04708 0.04031 = 0.04262 0.02104 0.00642 0.01349 C12 1 0.155905 0.352476 0.571815 11.00000 0.04004 0.03576 = 0.05179 0.02051 0.01255 0.00774 C13 1 0.045981 0.118657 0.481272 11.00000 0.03833 0.03644 = 0.03816 0.01091 0.00427 0.01151 C14 1 0.137967 0.090142 0.393971 11.00000 0.04438 0.04611 = 0.04264 0.01034 0.00513 0.01470 C16 1 -0.062093 0.078584 0.374516 11.00000 0.03816 0.04515 = 0.05015 0.01042 -0.01071 0.00116 AFIX 23 H16A 2 -0.117827 0.092875 0.402542 11.00000 -1.20000 H16B 2 -0.080325 0.030155 0.355393 11.00000 -1.20000 AFIX 0 C17 1 -0.057877 0.110799 0.319817 11.00000 0.02868 0.05011 = 0.04620 0.01019 -0.00953 0.00393 C18 1 -0.084176 0.068363 0.254801 11.00000 0.03500 0.04873 = 0.04835 0.00524 -0.00921 0.00026 C19 1 -0.033620 0.180683 0.333030 11.00000 0.03420 0.04584 = 0.03673 0.00528 -0.00239 0.00621 C20 1 -0.011437 0.226005 0.403060 11.00000 0.06236 0.04891 = 0.04652 0.01294 -0.00563 0.00194 AFIX 137 H20A 2 -0.039711 0.266032 0.408289 11.00000 -1.50000 H20B 2 0.063600 0.237851 0.413293 11.00000 -1.50000 H20C 2 -0.044159 0.202819 0.431926 11.00000 -1.50000 AFIX 0 C21 1 -0.037575 0.208190 0.282839 11.00000 0.03515 0.05084 = 0.04868 0.01822 -0.00124 0.00554 C22 1 -0.061777 0.166638 0.217631 11.00000 0.05090 0.08409 = 0.04317 0.02312 -0.00384 0.01692 C23 1 -0.085255 0.097355 0.204291 11.00000 0.04631 0.06341 = 0.04205 0.00329 -0.01226 0.01947 C24 1 -0.116601 0.050784 0.135626 11.00000 0.08574 0.07344 = 0.05527 -0.00501 -0.02934 0.03221 AFIX 23 H24A 2 -0.183771 0.021834 0.136128 11.00000 -1.20000 H24B 2 -0.127306 0.077682 0.107786 11.00000 -1.20000 AFIX 0 C25 1 -0.025439 0.283699 0.298916 11.00000 0.05138 0.05711 = 0.05333 0.01897 -0.00166 0.01232 AFIX 23 H25A 2 -0.042519 0.294016 0.259611 11.00000 -1.20000 H25B 2 -0.076162 0.299129 0.330500 11.00000 -1.20000 AFIX 0 C26 1 0.180061 0.306720 0.303358 11.00000 0.04991 0.05185 = 0.04736 0.01937 0.01018 0.01051 C27 1 0.204972 0.257182 0.250656 11.00000 0.06282 0.07194 = 0.06665 0.01679 0.01522 0.00144 AFIX 43 H27 2 0.152659 0.225250 0.222524 11.00000 -1.20000 AFIX 0 C28 1 0.310901 0.257078 0.241503 11.00000 0.07213 0.08313 = 0.08000 0.01892 0.03490 0.01568 AFIX 43 H28 2 0.331017 0.225220 0.205806 11.00000 -1.20000 AFIX 0 C29 1 0.389240 0.304840 0.285759 11.00000 0.05429 0.08268 = 0.10171 0.03094 0.03158 0.00779 AFIX 43 H29 2 0.459883 0.301460 0.280078 11.00000 -1.20000 AFIX 0 C30 1 0.364963 0.356878 0.337646 11.00000 0.05754 0.05988 = 0.06690 0.02133 0.01640 0.00882 AFIX 43 H30 2 0.416948 0.389456 0.365427 11.00000 -1.20000 AFIX 0 C31 1 0.255280 0.356593 0.345047 11.00000 0.05662 0.04554 = 0.05313 0.02317 0.01630 0.01271 C32 1 0.104315 0.377969 0.377844 11.00000 0.04780 0.03974 = 0.05209 0.02050 0.00906 0.01310 C33 1 -0.069378 0.439777 0.370422 11.00000 0.09317 0.08948 = 0.12467 0.03030 -0.00285 0.05312 AFIX 137 H33A 2 -0.024085 0.471032 0.353662 11.00000 -1.50000 H33B 2 -0.124405 0.460746 0.393095 11.00000 -1.50000 H33C 2 -0.100365 0.400961 0.334925 11.00000 -1.50000 AFIX 0 C73 1 0.206791 0.113629 0.449200 11.00000 0.03574 0.04762 = 0.04767 0.01552 0.00501 0.01449 C74 1 0.175532 0.067728 0.330455 11.00000 0.06505 0.07604 = 0.04044 0.00053 -0.00742 0.02952 AFIX 43 H74 2 0.129731 0.052477 0.293221 11.00000 -1.20000 AFIX 0 C75 1 0.315089 0.115126 0.445392 11.00000 0.03808 0.06850 = 0.05356 0.00923 -0.00585 0.01550 AFIX 43 H75 2 0.360739 0.129939 0.482677 11.00000 -1.20000 AFIX 0 C78 1 0.070557 0.020038 0.118965 11.00000 0.05729 0.05881 = 0.05005 0.02655 0.00591 0.01940 C79 1 -0.063825 -0.049684 0.056337 11.00000 0.05891 0.05131 = 0.04544 0.02305 0.00431 0.01486 C82 1 -0.186430 -0.151036 -0.040311 11.00000 0.09928 0.06269 = 0.05969 -0.00190 -0.01917 0.01648 AFIX 137 H82A 2 -0.132887 -0.138652 -0.067566 11.00000 -1.50000 H82B 2 -0.253074 -0.167905 -0.065262 11.00000 -1.50000 H82C 2 -0.167555 -0.185228 -0.024257 11.00000 -1.50000 AFIX 0 C83 1 0.244431 0.062617 0.159647 11.00000 0.07355 0.07514 = 0.07483 0.03581 -0.01742 0.00862 AFIX 43 H83 2 0.294039 0.096631 0.187855 11.00000 -1.20000 AFIX 0 C84 1 0.281644 0.069630 0.326679 11.00000 0.06650 0.10473 = 0.04251 0.01175 0.01590 0.04449 AFIX 43 H84 2 0.309046 0.054971 0.286006 11.00000 -1.20000 AFIX 0 C89 1 -0.128116 0.050875 0.520125 11.00000 0.05933 0.06846 = 0.09946 0.03639 0.01666 -0.00462 AFIX 137 H89A 2 -0.130775 0.024298 0.475077 11.00000 -1.50000 H89B 2 -0.198822 0.052149 0.533825 11.00000 -1.50000 H89C 2 -0.091585 0.031317 0.546330 11.00000 -1.50000 AFIX 0 C90 1 -0.116612 -0.007734 0.239367 11.00000 0.08429 0.05447 = 0.05309 0.00626 -0.00331 0.00314 AFIX 137 H90A 2 -0.133222 -0.027979 0.193287 11.00000 -1.50000 H90B 2 -0.177654 -0.017765 0.262602 11.00000 -1.50000 H90C 2 -0.059336 -0.025264 0.252516 11.00000 -1.50000 AFIX 0 C91 1 0.279624 0.007980 0.115322 11.00000 0.05615 0.10679 = 0.09155 0.05662 0.00582 0.01285 AFIX 43 H91 2 0.351258 0.005970 0.115108 11.00000 -1.20000 AFIX 0 C92 1 0.208820 -0.041839 0.072834 11.00000 0.06252 0.08393 = 0.07764 0.02748 0.02216 0.01849 AFIX 43 H92 2 0.230260 -0.079201 0.044488 11.00000 -1.20000 AFIX 0 C93 1 0.103057 -0.035004 0.073215 11.00000 0.06368 0.05162 = 0.06432 0.03306 0.01091 0.00704 C94 1 0.141919 0.067288 0.162579 11.00000 0.06519 0.06092 = 0.05933 0.02104 -0.00366 0.01759 AFIX 43 H94 2 0.120280 0.102451 0.194096 11.00000 -1.20000 AFIX 0 C95 1 0.351598 0.093730 0.384054 11.00000 0.03857 0.10816 = 0.06112 0.00451 0.00682 0.01699 AFIX 43 H95 2 0.423783 0.094980 0.379800 11.00000 -1.20000 AFIX 0 C100 1 -0.058787 0.199136 0.162126 11.00000 0.12462 0.10864 = 0.04458 0.02624 -0.00994 0.02143 AFIX 137 H10A 2 -0.059445 0.165179 0.120782 11.00000 -1.50000 H10B 2 0.004479 0.232562 0.168227 11.00000 -1.50000 H10C 2 -0.119544 0.219804 0.162975 11.00000 -1.50000 HKLF 4 REM RK5-79- in P-1 New: P-1 REM R1 = 0.0607 for 18702 Fo > 4sig(Fo) and 0.0923 for all 26285 data REM 1291 parameters refined using 0 restraints END WGHT 0.0926 13.4624 REM Highest difference peak 3.264, deepest hole -1.398, 1-sigma level 0.197 Q1 1 0.3037 0.6719 -0.0902 11.00000 0.05 3.26 Q2 1 0.2136 0.4883 0.2507 11.00000 0.05 2.99 Q3 1 0.5970 0.0253 0.1195 11.00000 0.05 2.59 Q4 1 0.1060 0.3890 0.1736 11.00000 0.05 2.37 Q5 1 0.2783 0.4518 0.2217 11.00000 0.05 2.18 Q6 1 0.1122 0.4511 0.2126 11.00000 0.05 2.14 Q7 1 -0.2441 0.7491 0.1081 11.00000 0.05 2.03 Q8 1 -0.2359 0.6819 0.0571 11.00000 0.05 1.93 Q9 1 0.2022 0.3761 0.1670 11.00000 0.05 1.89 Q10 1 0.5467 0.1124 0.2151 11.00000 0.05 1.83 Q11 1 0.5726 0.0475 0.1857 11.00000 0.05 1.79 Q12 1 0.2391 0.1537 0.5830 11.00000 0.05 1.77 Q13 1 0.1668 0.1533 0.6022 11.00000 0.05 1.66 Q14 1 0.1798 0.1421 0.5902 11.00000 0.05 1.62 Q15 1 0.0453 0.4725 0.2321 11.00000 0.05 1.51 Q16 1 0.2121 0.2000 0.6288 11.00000 0.05 1.48 Q17 1 0.2946 0.4011 0.1839 11.00000 0.05 1.42 Q18 1 0.5887 0.0913 0.1155 11.00000 0.05 1.40 Q19 1 0.6178 0.0663 0.0899 11.00000 0.05 1.30 Q20 1 0.3341 0.4784 0.4762 11.00000 0.05 1.28 ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.194 0.766 0.117 11 1 ' ' 2 0.288 0.226 0.380 17 2 ' ' 3 0.391 0.519 0.690 33 4 ' ' 4 0.350 0.694 0.704 7 1 ' ' 5 0.383 0.092 0.731 9 1 ' ' 6 0.435 0.135 0.013 15 1 ' ' 7 0.473 0.211 0.345 13 2 ' ' 8 0.538 0.787 0.651 14 2 ' ' 9 0.609 0.481 0.310 33 4 ' ' 10 0.565 0.864 0.987 16 1 ' ' 11 0.616 0.907 0.268 9 1 ' ' 12 0.650 0.306 0.296 7 1 ' ' 13 0.727 0.775 0.619 16 2 ' ' 14 0.806 0.234 0.883 11 1 ' ' _platon_squeeze_details ; The solvent accessible cavity is that of the solvent toluene molecules (estimated volume 189 \%A^3^) for which no reasonable model could be developed. Therefore, the observed structure amplitudes were modified by PLATON (Spek, 1990) to eliminate the diffuse electron density in the cavity. The solvent is included only in the scheme and not in the formula, FW, density, etc., and is also not included in the refined model. ; _database_code_depnum_ccdc_archive 'CCDC 935811'