# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Sathiyendiran Malaichamy' _publ_contact_author_email 'mvdiran@yahoo.com, msathi@chemistry.du.ac.in' _publ_section_title ; Furans decorated neutral Re(I)-based 2D rectangle and 3D trigonal prism ; _publ_author_name S.Malaichamy # Attachment '- CCDC_Rev-4_778832-33.txt' data_msdu01 _database_code_depnum_ccdc_archive 'CCDC 778832' #TrackingRef '- CCDC_Rev-4_778832-33.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H40 N4 O16 Re4 S4' _chemical_formula_weight 1897.96 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_space_group_name_H-M 'P 1 21/c 1' _symmetry_cell_setting monoclinic 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 12.990(5) _cell_length_b 26.243(5) _cell_length_c 18.903(5) _cell_angle_alpha 90.000 _cell_angle_beta 109.501(5) _cell_angle_gamma 90.000 _cell_volume 6074(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 30004 _cell_measurement_theta_min 2.4093 _cell_measurement_theta_max 29.4393 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 8.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86388 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 113830 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.35 _reflns_number_total 11109 _reflns_number_gt 8062 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis RED (Oxford, 2007)' _computing_cell_refinement 'CrysAlis RED (Oxford, 2007)' _computing_data_reduction 'CrysAlis RED (Oxford, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _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^)+(0.0170P)^2^+0.0000P] 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 11109 _refine_ls_number_parameters 797 _refine_ls_number_restraints 808 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0434 _refine_ls_wR_factor_gt 0.0408 _refine_ls_goodness_of_fit_ref 0.867 _refine_ls_restrained_S_all 0.844 _refine_ls_shift/su_max 0.184 _refine_ls_shift/su_mean 0.005 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 -0.5299(4) 0.55704(19) 0.0507(3) 0.0344(12) Uani 1 1 d U . . H1 H -0.5336 0.5783 0.0106 0.041 Uiso 1 1 calc R . . C2 C -0.4283(4) 0.55878(18) 0.1151(3) 0.0289(12) Uani 1 1 d U . . C3 C -0.4101(4) 0.5283(2) 0.1780(3) 0.0377(13) Uani 1 1 d U . . H3 H -0.4631 0.5052 0.1805 0.045 Uiso 1 1 calc R . . C4 C -0.3133(4) 0.5324(2) 0.2365(3) 0.0386(13) Uani 1 1 d U . . H4 H -0.3023 0.5114 0.2779 0.046 Uiso 1 1 calc R . . C5 C -0.2520(4) 0.59511(18) 0.1764(3) 0.0273(11) Uani 1 1 d U . . H5 H -0.1986 0.6184 0.1754 0.033 Uiso 1 1 calc R . . C6 C -0.3466(4) 0.59260(18) 0.1155(3) 0.0291(12) Uani 1 1 d U . . H6 H -0.3555 0.6138 0.0744 0.035 Uiso 1 1 calc R . . C7 C -0.6164(4) 0.52860(19) 0.0435(3) 0.0331(12) Uani 1 1 d U . . H7 H -0.6131 0.5066 0.0829 0.040 Uiso 1 1 calc R . . C8 C -0.7175(4) 0.52867(19) -0.0213(3) 0.0310(12) Uani 1 1 d U . . C9 C -0.7387(4) 0.5632(2) -0.0795(3) 0.0433(14) Uani 1 1 d U . . H9 H -0.6870 0.5880 -0.0783 0.052 Uiso 1 1 calc R . . C10 C -0.8351(4) 0.5616(2) -0.1393(3) 0.0404(14) Uani 1 1 d U . . H10 H -0.8456 0.5851 -0.1779 0.048 Uiso 1 1 calc R . . C11 C -0.8946(4) 0.49477(19) -0.0866(3) 0.0338(13) Uani 1 1 d U . . H11 H -0.9482 0.4710 -0.0879 0.041 Uiso 1 1 calc R . . C12 C -0.7995(4) 0.49451(19) -0.0261(3) 0.0335(13) Uani 1 1 d U . . H12 H -0.7907 0.4708 0.0121 0.040 Uiso 1 1 calc R . . C13 C -0.0153(4) 0.44874(19) 0.4074(3) 0.0392(13) Uani 1 1 d U . . H13A H 0.0596 0.4604 0.4290 0.047 Uiso 1 1 calc R . . H13B H -0.0553 0.4613 0.4388 0.047 Uiso 1 1 calc R . . C14 C -0.0160(4) 0.3931(2) 0.4090(3) 0.0445(14) Uani 1 1 d U . . C15 C 0.0604(6) 0.3573(2) 0.4305(3) 0.0693(19) Uani 1 1 d U . . H15 H 0.1356 0.3624 0.4473 0.083 Uiso 1 1 calc R . . C16 C 0.0047(6) 0.3093(3) 0.4228(4) 0.087(2) Uani 1 1 d U . . H16 H 0.0364 0.2772 0.4342 0.105 Uiso 1 1 calc R . . C17 C -0.1027(7) 0.3201(3) 0.3957(5) 0.113(3) Uani 1 1 d U . . H17 H -0.1581 0.2959 0.3848 0.136 Uiso 1 1 calc R . . C23 C 0.3729(4) 0.94580(19) 0.1161(3) 0.0376(13) Uani 1 1 d U . . H23 H 0.3078 0.9493 0.0763 0.045 Uiso 1 1 calc R . . C24 C 0.3847(4) 0.90600(19) 0.1640(3) 0.0373(13) Uani 1 1 d U . . H24 H 0.3259 0.8839 0.1565 0.045 Uiso 1 1 calc R . . C25 C 0.5576(4) 0.93118(18) 0.2305(3) 0.0330(12) Uani 1 1 d U . . H25 H 0.6229 0.9260 0.2697 0.040 Uiso 1 1 calc R . . C26 C 0.5498(4) 0.97297(18) 0.1857(3) 0.0307(12) Uani 1 1 d U . . H26 H 0.6077 0.9958 0.1959 0.037 Uiso 1 1 calc R . . C27 C 0.4553(4) 0.98140(18) 0.1247(3) 0.0290(11) Uani 1 1 d U . . C28 C 0.4415(4) 1.02329(19) 0.0732(3) 0.0346(12) Uani 1 1 d U . . H28 H 0.3777 1.0230 0.0319 0.042 Uiso 1 1 calc R . . C29 C 0.5079(4) 1.06211(19) 0.0773(3) 0.0364(13) Uani 1 1 d U . . H29 H 0.5727 1.0626 0.1178 0.044 Uiso 1 1 calc R . . C30 C 0.4896(4) 1.10428(19) 0.0244(3) 0.0359(13) Uani 1 1 d U . . C31 C 0.3885(4) 1.11321(19) -0.0300(3) 0.0344(12) Uani 1 1 d U . . H31 H 0.3298 1.0921 -0.0325 0.041 Uiso 1 1 calc R . . C32 C 0.3743(4) 1.15289(19) -0.0801(3) 0.0343(13) Uani 1 1 d U . . H32 H 0.3054 1.1577 -0.1156 0.041 Uiso 1 1 calc R . . C33 C 0.5526(4) 1.1769(2) -0.0275(3) 0.0416(14) Uani 1 1 d U . . H33 H 0.6098 1.1989 -0.0252 0.050 Uiso 1 1 calc R . . C34 C 0.5725(4) 1.1376(2) 0.0237(3) 0.0446(14) Uani 1 1 d U . . H34 H 0.6423 1.1333 0.0582 0.054 Uiso 1 1 calc R . . C35 C 0.7712(4) 0.7854(2) 0.3321(3) 0.0452(14) Uani 1 1 d U . . H35A H 0.7451 0.7537 0.3463 0.054 Uiso 1 1 calc R . . H35B H 0.8297 0.7773 0.3129 0.054 Uiso 1 1 calc R . . C36 C 0.8153(4) 0.8176(2) 0.3997(3) 0.0431(14) Uani 1 1 d U . . C37 C 0.8176(5) 0.8133(2) 0.4704(3) 0.0591(16) Uani 1 1 d U . . H37 H 0.7863 0.7873 0.4897 0.071 Uiso 1 1 calc R . . C38 C 0.8764(5) 0.8555(3) 0.5107(3) 0.0648(18) Uani 1 1 d U . . H38 H 0.8905 0.8625 0.5613 0.078 Uiso 1 1 calc R . . C39 C 0.9076(5) 0.8833(3) 0.4623(3) 0.0683(19) Uani 1 1 d U . . H39 H 0.9476 0.9133 0.4740 0.082 Uiso 1 1 calc R . . C45 C -0.0921(4) 0.6427(2) 0.3415(3) 0.0404(13) Uani 1 1 d U . . C46 C 0.0555(4) 0.57361(19) 0.4147(3) 0.0351(12) Uani 1 1 d U . . C47 C -0.1585(4) 0.5639(2) 0.4030(3) 0.0384(13) Uani 1 1 d U . . C48 C 0.0814(4) 0.4045(2) 0.2538(3) 0.0357(13) Uani 1 1 d U . . C49 C 0.1561(4) 0.48338(19) 0.1891(3) 0.0328(12) Uani 1 1 d U . . C50 C 0.1810(4) 0.48579(19) 0.3362(3) 0.0305(12) Uani 1 1 d U . . C51 C 0.7105(4) 0.7324(2) 0.1432(3) 0.0374(13) Uani 1 1 d U . . C52 C 0.4985(4) 0.7063(2) 0.0782(3) 0.0439(14) Uani 1 1 d U . . C53 C 0.5989(4) 0.6941(2) 0.2279(3) 0.0414(13) Uani 1 1 d U . . C54 C 0.5310(5) 0.7744(2) 0.3668(3) 0.0481(15) Uani 1 1 d U . . C55 C 0.3626(5) 0.8396(2) 0.3132(3) 0.0461(14) Uani 1 1 d U . . C56 C 0.5702(4) 0.8747(2) 0.3826(3) 0.0373(13) Uani 1 1 d U . . N1 N -0.2335(3) 0.56542(15) 0.2370(2) 0.0280(9) Uani 1 1 d U . . N2 N -0.9139(3) 0.52768(15) -0.1441(2) 0.0285(9) Uani 1 1 d U . . N3 N 0.4763(3) 0.89679(14) 0.2214(2) 0.0305(9) Uani 1 1 d U . . N4 N 0.4553(3) 1.18524(15) -0.0805(2) 0.0336(10) Uani 1 1 d U . . O1 O -0.0974(3) 0.68604(16) 0.3483(3) 0.0741(14) Uani 1 1 d U . . O2 O 0.1392(3) 0.57581(15) 0.46243(19) 0.0481(10) Uani 1 1 d U . . O3 O -0.2062(3) 0.55926(16) 0.4449(2) 0.0575(11) Uani 1 1 d U . . O4 O -0.1192(3) 0.37129(17) 0.3866(3) 0.0824(14) Uani 1 1 d U . . O5 O 0.0939(3) 0.36085(14) 0.2600(2) 0.0550(11) Uani 1 1 d U . . O6 O 0.2162(3) 0.48686(14) 0.15496(19) 0.0464(10) Uani 1 1 d U . . O7 O 0.2532(3) 0.49174(14) 0.39158(19) 0.0431(10) Uani 1 1 d U . . O9 O 0.7917(3) 0.72170(15) 0.1348(2) 0.0584(11) Uani 1 1 d U . . O10 O 0.4529(3) 0.67999(15) 0.0269(2) 0.0601(12) Uani 1 1 d U . . O11 O 0.6116(3) 0.66043(14) 0.2697(2) 0.0577(11) Uani 1 1 d U . . O12 O 0.5523(4) 0.74068(16) 0.4084(3) 0.0765(14) Uani 1 1 d U . . O13 O 0.2781(3) 0.84226(15) 0.3216(3) 0.0701(13) Uani 1 1 d U . . O14 O 0.6096(3) 0.90190(15) 0.4324(2) 0.0551(11) Uani 1 1 d U . . O15 O 0.8718(3) 0.86085(15) 0.3926(2) 0.0573(11) Uani 1 1 d U . . Re1 Re -0.080588(15) 0.570707(8) 0.334738(11) 0.02713(5) Uani 1 1 d U A . Re2 Re 0.061432(15) 0.477100(8) 0.245756(11) 0.02593(5) Uani 1 1 d U . . Re3 Re 0.576083(17) 0.749229(8) 0.158394(12) 0.03369(6) Uani 1 1 d U . . Re4 Re 0.499887(17) 0.831250(8) 0.299692(12) 0.03432(6) Uani 1 1 d U A . S1 S -0.07410(10) 0.47674(5) 0.31402(6) 0.0291(3) Uani 1 1 d U . . S2 S 0.01274(9) 0.56983(5) 0.23823(7) 0.0278(3) Uani 1 1 d U . . S3 S 0.65944(10) 0.81541(5) 0.25721(7) 0.0335(3) Uani 1 1 d U . . S4 S 0.40954(11) 0.77930(5) 0.18435(8) 0.0415(4) Uani 1 1 d U . . C18A C 0.1399(4) 0.60671(19) 0.2734(3) 0.0420(13) Uani 0.834(4) 1 d PDU A 1 H18A H 0.1834 0.5935 0.3222 0.050 Uiso 0.834(4) 1 calc PR A 1 H18B H 0.1814 0.6020 0.2397 0.050 Uiso 0.834(4) 1 calc PR A 1 C19A C 0.1217(5) 0.6611(3) 0.2803(4) 0.0521(18) Uani 0.834(4) 1 d PDU A 1 O8A O 0.1646(5) 0.6812(2) 0.3497(3) 0.102(2) Uani 0.834(4) 1 d PDU A 1 C20A C 0.0683(5) 0.6964(3) 0.2308(4) 0.062(2) Uani 0.834(4) 1 d PDU A 1 H20A H 0.0325 0.6917 0.1796 0.075 Uiso 0.834(4) 1 calc PR A 1 C21A C 0.0770(9) 0.7417(4) 0.2709(7) 0.095(3) Uani 0.834(4) 1 d PDU A 1 H21A H 0.0484 0.7730 0.2503 0.114 Uiso 0.834(4) 1 calc PR A 1 C22A C 0.1332(10) 0.7333(4) 0.3441(7) 0.118(4) Uani 0.834(4) 1 d PDU A 1 H22A H 0.1484 0.7569 0.3830 0.142 Uiso 0.834(4) 1 calc PR A 1 C40A C 0.3467(5) 0.7259(2) 0.2191(4) 0.072(2) Uani 0.834(4) 1 d PU A 1 H40A H 0.4028 0.7089 0.2596 0.086 Uiso 0.834(4) 1 calc PR A 1 H40B H 0.2931 0.7394 0.2395 0.086 Uiso 0.834(4) 1 calc PR A 1 C41A C 0.2943(7) 0.6887(3) 0.1617(5) 0.065(2) Uani 0.834(4) 1 d PU A 1 O16A O 0.2093(5) 0.7075(2) 0.1014(4) 0.092(2) Uani 0.834(4) 1 d PU A 1 C42A C 0.3046(8) 0.6389(3) 0.1536(6) 0.086(3) Uani 0.834(4) 1 d PU A 1 H42A H 0.3557 0.6173 0.1859 0.104 Uiso 0.834(4) 1 calc PR A 1 C43A C 0.2196(10) 0.6252(5) 0.0841(8) 0.115(4) Uani 0.834(4) 1 d PU A 1 H43A H 0.2044 0.5925 0.0646 0.137 Uiso 0.834(4) 1 calc PR A 1 C44A C 0.1661(9) 0.6683(5) 0.0524(7) 0.128(4) Uani 0.834(4) 1 d PU A 1 H44A H 0.1107 0.6707 0.0062 0.153 Uiso 0.834(4) 1 calc PR A 1 C18B C 0.1399(4) 0.60671(19) 0.2734(3) 0.0420(13) Uani 0.166(4) 1 d PDU A 2 H18C H 0.1229 0.6411 0.2849 0.050 Uiso 0.166(4) 1 calc PR A 2 H18D H 0.1868 0.5914 0.3197 0.050 Uiso 0.166(4) 1 calc PR A 2 C19B C 0.1952(17) 0.6089(7) 0.2230(12) 0.040(8) Uiso 0.166(4) 1 d PDU A 2 O8B O 0.3017(17) 0.5925(8) 0.2491(11) 0.069(8) Uiso 0.166(4) 1 d PDU A 2 C20B C 0.173(2) 0.6239(10) 0.1500(13) 0.051(10) Uiso 0.166(4) 1 d PDU A 2 H20B H 0.1064 0.6365 0.1185 0.062 Uiso 0.166(4) 1 calc PR A 2 C21B C 0.266(3) 0.6170(17) 0.1311(17) 0.072(18) Uiso 0.166(4) 1 d PDU A 2 H21B H 0.2736 0.6243 0.0850 0.086 Uiso 0.166(4) 1 calc PR A 2 C22B C 0.344(2) 0.5975(14) 0.1924(18) 0.093(15) Uiso 0.166(4) 1 d PDU A 2 H22B H 0.4153 0.5890 0.1952 0.112 Uiso 0.166(4) 1 calc PR A 2 C40B C 0.3467(5) 0.7259(2) 0.2191(4) 0.072(2) Uani 0.166(4) 1 d PDU A 2 H40C H 0.3221 0.7009 0.1792 0.086 Uiso 0.166(4) 1 calc PR A 2 H40D H 0.4034 0.7099 0.2603 0.086 Uiso 0.166(4) 1 calc PR A 2 C41B C 0.260(3) 0.7368(12) 0.243(3) 0.8(2) Uiso 0.166(4) 1 d PDU A 2 O16B O 0.155(3) 0.7544(17) 0.215(2) 0.23(2) Uiso 0.166(4) 1 d PDU A 2 C42B C 0.278(3) 0.7299(16) 0.318(3) 0.14(2) Uiso 0.166(4) 1 d PDU A 2 H42B H 0.3419 0.7172 0.3523 0.166 Uiso 0.166(4) 1 calc PR A 2 C43B C 0.189(4) 0.7439(17) 0.337(2) 0.115(4) Uani 0.166(4) 1 d PDU A 2 H43B H 0.1837 0.7440 0.3849 0.137 Uiso 0.166(4) 1 calc PR A 2 C44B C 0.109(3) 0.7581(16) 0.271(3) 0.09(2) Uiso 0.166(4) 1 d PDU A 2 H44B H 0.0384 0.7681 0.2654 0.108 Uiso 0.166(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(3) 0.045(3) 0.024(3) 0.000(3) 0.006(2) -0.001(2) C2 0.024(3) 0.034(3) 0.027(3) 0.002(2) 0.006(2) -0.001(2) C3 0.026(3) 0.050(3) 0.032(3) 0.010(3) 0.002(2) -0.010(3) C4 0.028(3) 0.051(4) 0.036(3) 0.013(3) 0.009(2) -0.002(3) C5 0.019(3) 0.033(3) 0.028(3) 0.002(2) 0.004(2) 0.000(2) C6 0.027(3) 0.032(3) 0.025(3) 0.006(2) 0.004(2) 0.006(2) C7 0.033(3) 0.034(3) 0.027(3) 0.006(2) 0.003(2) 0.003(2) C8 0.029(3) 0.036(3) 0.022(3) 0.001(2) 0.001(2) 0.002(2) C9 0.039(3) 0.045(3) 0.036(3) 0.005(3) -0.001(3) -0.021(3) C10 0.041(3) 0.044(3) 0.027(3) 0.009(3) 0.000(3) -0.013(3) C11 0.033(3) 0.043(3) 0.023(3) 0.005(2) 0.006(2) -0.008(2) C12 0.038(3) 0.040(3) 0.018(3) 0.009(2) 0.003(2) -0.006(2) C13 0.040(3) 0.042(3) 0.036(3) 0.006(3) 0.013(3) -0.001(3) C14 0.037(3) 0.049(3) 0.041(3) 0.004(3) 0.003(3) -0.007(3) C15 0.063(4) 0.062(4) 0.063(5) 0.003(4) -0.005(4) 0.024(3) C16 0.083(5) 0.045(4) 0.107(6) 0.010(4) -0.004(5) 0.012(4) C17 0.098(5) 0.048(4) 0.162(9) 0.026(5) 0.002(6) -0.007(4) C23 0.029(3) 0.034(3) 0.040(3) -0.003(3) -0.001(3) 0.004(2) C24 0.027(3) 0.031(3) 0.051(4) -0.002(3) 0.009(3) -0.001(2) C25 0.021(3) 0.036(3) 0.039(3) -0.002(3) 0.006(2) 0.001(2) C26 0.026(3) 0.029(3) 0.035(3) 0.000(2) 0.008(2) -0.005(2) C27 0.033(3) 0.026(3) 0.025(3) -0.003(2) 0.005(2) 0.006(2) C28 0.029(3) 0.042(3) 0.027(3) -0.005(2) 0.003(2) 0.005(3) C29 0.027(3) 0.041(3) 0.035(3) 0.008(3) 0.002(2) 0.011(2) C30 0.034(3) 0.034(3) 0.034(3) -0.001(2) 0.004(3) 0.008(2) C31 0.025(3) 0.035(3) 0.039(3) 0.006(3) 0.005(2) 0.000(2) C32 0.024(3) 0.041(3) 0.034(3) 0.006(3) 0.005(2) 0.006(2) C33 0.032(3) 0.037(3) 0.048(4) -0.001(3) 0.003(3) -0.006(3) C34 0.031(3) 0.044(4) 0.048(4) 0.004(3) -0.001(3) 0.001(3) C35 0.040(3) 0.043(3) 0.051(3) 0.003(3) 0.013(3) 0.007(3) C36 0.041(3) 0.041(3) 0.042(3) 0.010(3) 0.006(3) 0.012(3) C37 0.062(4) 0.072(4) 0.040(3) 0.012(3) 0.013(3) 0.013(3) C38 0.065(5) 0.088(5) 0.030(3) -0.002(3) 0.001(3) 0.023(4) C39 0.078(5) 0.066(5) 0.044(4) -0.008(3) -0.003(4) 0.005(4) C45 0.030(3) 0.046(3) 0.038(3) -0.006(3) 0.001(3) 0.005(3) C46 0.036(3) 0.039(3) 0.031(3) -0.001(3) 0.012(2) -0.001(3) C47 0.022(3) 0.053(4) 0.032(3) -0.002(3) -0.002(2) 0.003(3) C48 0.036(3) 0.042(3) 0.027(3) 0.004(3) 0.009(3) 0.006(3) C49 0.023(3) 0.046(3) 0.022(3) 0.000(3) -0.002(2) 0.001(3) C50 0.027(3) 0.036(3) 0.029(3) 0.001(2) 0.011(2) 0.004(2) C51 0.042(3) 0.039(3) 0.031(3) 0.004(3) 0.012(3) 0.002(3) C52 0.041(3) 0.036(3) 0.050(4) 0.008(3) 0.008(3) 0.001(3) C53 0.048(4) 0.036(3) 0.047(3) 0.000(3) 0.025(3) 0.010(3) C54 0.058(4) 0.043(3) 0.056(4) 0.005(3) 0.035(3) 0.002(3) C55 0.050(3) 0.030(3) 0.064(4) -0.011(3) 0.027(3) -0.002(3) C56 0.041(3) 0.035(3) 0.039(3) 0.011(2) 0.019(3) 0.003(3) N1 0.021(2) 0.034(2) 0.026(2) 0.0026(19) 0.0051(18) -0.0008(19) N2 0.028(2) 0.035(2) 0.018(2) -0.0040(19) 0.0015(18) -0.004(2) N3 0.027(2) 0.027(2) 0.038(2) -0.0016(19) 0.011(2) 0.0010(19) N4 0.027(2) 0.035(3) 0.036(3) -0.001(2) 0.006(2) 0.004(2) O1 0.073(3) 0.040(3) 0.107(4) -0.008(3) 0.027(3) 0.010(2) O2 0.029(2) 0.074(3) 0.032(2) -0.002(2) -0.0018(18) 0.000(2) O3 0.043(2) 0.093(3) 0.044(2) -0.009(2) 0.024(2) -0.009(2) O4 0.053(3) 0.062(3) 0.119(4) 0.011(3) 0.010(3) -0.010(2) O5 0.074(3) 0.037(2) 0.059(3) 0.003(2) 0.029(2) 0.010(2) O6 0.040(2) 0.068(3) 0.033(2) 0.001(2) 0.0140(19) 0.007(2) O7 0.026(2) 0.062(3) 0.031(2) 0.0001(19) -0.0041(17) 0.0036(18) O9 0.050(3) 0.066(3) 0.070(3) 0.005(2) 0.034(2) 0.013(2) O10 0.065(3) 0.045(3) 0.057(3) -0.009(2) 0.003(2) -0.002(2) O11 0.085(3) 0.039(2) 0.059(3) 0.014(2) 0.037(2) 0.012(2) O12 0.105(4) 0.052(3) 0.088(4) 0.031(3) 0.052(3) 0.015(3) O13 0.051(3) 0.063(3) 0.111(4) -0.030(3) 0.046(3) -0.007(2) O14 0.062(3) 0.063(3) 0.038(2) -0.008(2) 0.014(2) 0.002(2) O15 0.065(3) 0.061(3) 0.045(2) -0.001(2) 0.017(2) -0.001(2) Re1 0.02050(11) 0.03380(12) 0.02397(11) 0.00074(10) 0.00329(9) 0.00180(10) Re2 0.02255(11) 0.03122(12) 0.02081(11) 0.00116(10) 0.00295(9) 0.00142(9) Re3 0.03548(13) 0.02696(12) 0.04022(13) 0.00056(11) 0.01476(11) 0.00382(10) Re4 0.03623(13) 0.02772(12) 0.04372(14) 0.00080(11) 0.01960(11) 0.00231(10) S1 0.0268(7) 0.0350(7) 0.0230(7) 0.0041(6) 0.0048(6) -0.0021(6) S2 0.0206(6) 0.0322(7) 0.0277(7) 0.0009(6) 0.0041(6) -0.0029(6) S3 0.0316(7) 0.0323(8) 0.0367(8) 0.0026(6) 0.0117(6) 0.0044(6) S4 0.0352(8) 0.0292(8) 0.0627(10) -0.0075(7) 0.0197(7) -0.0026(6) C18A 0.032(3) 0.046(3) 0.047(4) 0.004(3) 0.012(3) -0.011(3) C19A 0.033(4) 0.048(4) 0.071(5) 0.002(4) 0.012(4) -0.005(3) O8A 0.104(5) 0.077(4) 0.102(4) -0.029(4) 0.002(4) -0.009(4) C20A 0.048(5) 0.052(4) 0.084(5) 0.021(4) 0.019(4) 0.006(4) C21A 0.076(7) 0.048(5) 0.176(10) 0.017(6) 0.064(7) -0.013(5) C22A 0.133(12) 0.065(6) 0.161(9) -0.036(7) 0.055(9) -0.041(7) C40A 0.071(5) 0.049(4) 0.113(6) -0.018(4) 0.055(4) -0.022(3) C41A 0.067(5) 0.042(4) 0.102(6) -0.024(4) 0.051(4) -0.015(4) O16A 0.070(4) 0.073(4) 0.125(5) -0.044(4) 0.021(3) -0.019(3) C42A 0.092(7) 0.042(5) 0.153(9) -0.033(5) 0.079(6) -0.024(4) C43A 0.119(9) 0.090(6) 0.168(12) -0.079(8) 0.092(8) -0.061(6) C44A 0.087(8) 0.118(8) 0.173(10) -0.081(8) 0.036(6) -0.048(7) C18B 0.032(3) 0.046(3) 0.047(4) 0.004(3) 0.012(3) -0.011(3) C40B 0.071(5) 0.049(4) 0.113(6) -0.018(4) 0.055(4) -0.022(3) C43B 0.119(9) 0.090(6) 0.168(12) -0.079(8) 0.092(8) -0.061(6) _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 C7 1.318(6) . ? C1 C2 1.467(6) . ? C1 H1 0.9300 . ? C2 C6 1.382(6) . ? C2 C3 1.386(6) . ? C3 C4 1.374(6) . ? C3 H3 0.9300 . ? C4 N1 1.348(6) . ? C4 H4 0.9300 . ? C5 N1 1.340(5) . ? C5 C6 1.377(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.467(6) . ? C7 H7 0.9300 . ? C8 C12 1.372(6) . ? C8 C9 1.380(6) . ? C9 C10 1.379(7) . ? C9 H9 0.9300 . ? C10 N2 1.337(6) . ? C10 H10 0.9300 . ? C11 N2 1.344(6) . ? C11 C12 1.375(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.461(7) . ? C13 S1 1.827(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.328(7) . ? C14 O4 1.387(6) . ? C15 C16 1.437(9) . ? C15 H15 0.9300 . ? C16 C17 1.346(9) . ? C16 H16 0.9300 . ? C17 O4 1.363(8) . ? C17 H17 0.9300 . ? C23 C24 1.357(7) . ? C23 C27 1.389(6) . ? C23 H23 0.9300 . ? C24 N3 1.339(6) . ? C24 H24 0.9300 . ? C25 N3 1.356(6) . ? C25 C26 1.369(6) . ? C25 H25 0.9300 . ? C26 C27 1.392(6) . ? C26 H26 0.9300 . ? C27 C28 1.439(6) . ? C28 C29 1.321(6) . ? C28 H28 0.9300 . ? C29 C30 1.457(7) . ? C29 H29 0.9300 . ? C30 C31 1.391(6) . ? C30 C34 1.391(7) . ? C31 C32 1.379(6) . ? C31 H31 0.9300 . ? C32 N4 1.354(6) . ? C32 H32 0.9300 . ? C33 N4 1.343(6) . ? C33 C34 1.378(7) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.478(7) . ? C35 S3 1.833(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.331(7) . ? C36 O15 1.382(6) . ? C37 C38 1.415(8) . ? C37 H37 0.9300 . ? C38 C39 1.335(8) . ? C38 H38 0.9300 . ? C39 O15 1.374(7) . ? C39 H39 0.9300 . ? C45 O1 1.150(6) . ? C45 Re1 1.902(6) . ? C46 O2 1.160(5) . ? C46 Re1 1.905(5) . ? C47 O3 1.163(6) . ? C47 Re1 1.896(6) . ? C48 O5 1.158(6) . ? C48 Re2 1.921(6) . ? C49 O6 1.170(5) . ? C49 Re2 1.889(5) . ? C50 O7 1.159(5) . ? C50 Re2 1.901(5) . ? C51 O9 1.152(5) . ? C51 Re3 1.914(6) . ? C52 O10 1.177(6) . ? C52 Re3 1.888(6) . ? C53 O11 1.159(6) . ? C53 Re3 1.910(6) . ? C54 O12 1.155(6) . ? C54 Re4 1.912(6) . ? C55 O13 1.163(6) . ? C55 Re4 1.896(6) . ? C56 O14 1.156(6) . ? C56 Re4 1.906(6) . ? N1 Re1 2.220(4) . ? N2 Re2 2.218(4) 3_465 ? N3 Re4 2.222(4) . ? N4 Re3 2.212(4) 3_675 ? Re1 S1 2.5027(14) . ? Re1 S2 2.5049(13) . ? Re2 N2 2.218(4) 3_465 ? Re2 S1 2.5063(14) . ? Re2 S2 2.5065(13) . ? Re3 N4 2.212(4) 3_675 ? Re3 S4 2.5006(15) . ? Re3 S3 2.5155(14) . ? Re4 S3 2.4948(15) . ? Re4 S4 2.5062(15) . ? S2 C18A 1.837(5) . ? S4 C40A 1.850(6) . ? C18A C19A 1.460(8) . ? C18A H18A 0.9700 . ? C18A H18B 0.9700 . ? C19A C20A 1.335(8) . ? C19A O8A 1.349(8) . ? O8A C22A 1.422(10) . ? C20A C21A 1.394(10) . ? C20A H20A 0.9300 . ? C21A C22A 1.350(11) . ? C21A H21A 0.9300 . ? C22A H22A 0.9300 . ? C40A C41A 1.449(9) . ? C40A H40A 0.9700 . ? C40A H40B 0.9700 . ? C41A C42A 1.327(10) . ? C41A O16A 1.386(10) . ? O16A C44A 1.372(10) . ? C42A C43A 1.451(15) . ? C42A H42A 0.9300 . ? C43A C44A 1.357(16) . ? C43A H43A 0.9300 . ? C44A H44A 0.9300 . ? C19B C20B 1.369(17) . ? C19B O8B 1.374(17) . ? O8B C22B 1.368(18) . ? C20B C21B 1.383(18) . ? C20B H20B 0.9300 . ? C21B C22B 1.361(18) . ? C21B H21B 0.9300 . ? C22B H22B 0.9300 . ? C41B O16B 1.369(19) . ? C41B C42B 1.368(19) . ? O16B C44B 1.378(18) . ? C42B C43B 1.360(18) . ? C42B H42B 0.9300 . ? C43B C44B 1.380(19) . ? C43B H43B 0.9300 . ? C44B H44B 0.9300 . ? 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 C7 C1 C2 127.1(5) . . ? C7 C1 H1 116.4 . . ? C2 C1 H1 116.4 . . ? C6 C2 C3 117.1(4) . . ? C6 C2 C1 120.1(4) . . ? C3 C2 C1 122.8(4) . . ? C4 C3 C2 119.5(5) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? N1 C4 C3 123.5(5) . . ? N1 C4 H4 118.2 . . ? C3 C4 H4 118.2 . . ? N1 C5 C6 122.8(4) . . ? N1 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C5 C6 C2 120.3(4) . . ? C5 C6 H6 119.8 . . ? C2 C6 H6 119.9 . . ? C1 C7 C8 125.5(5) . . ? C1 C7 H7 117.3 . . ? C8 C7 H7 117.3 . . ? C12 C8 C9 115.6(4) . . ? C12 C8 C7 120.9(4) . . ? C9 C8 C7 123.5(5) . . ? C10 C9 C8 121.2(5) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? N2 C10 C9 122.8(5) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N2 C11 C12 123.3(5) . . ? N2 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C8 C12 C11 120.9(4) . . ? C8 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 S1 114.8(4) . . ? C14 C13 H13A 108.6 . . ? S1 C13 H13A 108.6 . . ? C14 C13 H13B 108.6 . . ? S1 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C15 C14 O4 110.4(5) . . ? C15 C14 C13 134.7(6) . . ? O4 C14 C13 114.8(5) . . ? C14 C15 C16 106.8(6) . . ? C14 C15 H15 126.6 . . ? C16 C15 H15 126.6 . . ? C17 C16 C15 106.1(6) . . ? C17 C16 H16 127.0 . . ? C15 C16 H16 127.0 . . ? C16 C17 O4 110.8(7) . . ? C16 C17 H17 124.6 . . ? O4 C17 H17 124.6 . . ? C24 C23 C27 121.9(5) . . ? C24 C23 H23 119.0 . . ? C27 C23 H23 119.0 . . ? N3 C24 C23 123.5(5) . . ? N3 C24 H24 118.3 . . ? C23 C24 H24 118.3 . . ? N3 C25 C26 124.1(5) . . ? N3 C25 H25 117.9 . . ? C26 C25 H25 117.9 . . ? C25 C26 C27 120.2(5) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C23 C27 C26 115.0(4) . . ? C23 C27 C28 121.1(4) . . ? C26 C27 C28 123.9(5) . . ? C29 C28 C27 128.2(5) . . ? C29 C28 H28 115.9 . . ? C27 C28 H28 115.9 . . ? C28 C29 C30 126.3(5) . . ? C28 C29 H29 116.8 . . ? C30 C29 H29 116.8 . . ? C31 C30 C34 115.4(5) . . ? C31 C30 C29 122.2(5) . . ? C34 C30 C29 122.3(5) . . ? C32 C31 C30 120.8(5) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? N4 C32 C31 123.4(4) . . ? N4 C32 H32 118.3 . . ? C31 C32 H32 118.3 . . ? N4 C33 C34 123.6(5) . . ? N4 C33 H33 118.2 . . ? C34 C33 H33 118.2 . . ? C33 C34 C30 120.9(5) . . ? C33 C34 H34 119.6 . . ? C30 C34 H34 119.6 . . ? C36 C35 S3 113.6(4) . . ? C36 C35 H35A 108.8 . . ? S3 C35 H35A 108.8 . . ? C36 C35 H35B 108.8 . . ? S3 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C37 C36 O15 109.4(5) . . ? C37 C36 C35 133.7(6) . . ? O15 C36 C35 116.8(5) . . ? C36 C37 C38 107.6(6) . . ? C36 C37 H37 126.2 . . ? C38 C37 H37 126.2 . . ? C39 C38 C37 106.8(6) . . ? C39 C38 H38 126.6 . . ? C37 C38 H38 126.6 . . ? C38 C39 O15 109.9(6) . . ? C38 C39 H39 125.0 . . ? O15 C39 H39 125.0 . . ? O1 C45 Re1 177.5(5) . . ? O2 C46 Re1 178.7(5) . . ? O3 C47 Re1 179.3(5) . . ? O5 C48 Re2 178.8(4) . . ? O6 C49 Re2 178.8(4) . . ? O7 C50 Re2 178.9(5) . . ? O9 C51 Re3 179.0(5) . . ? O10 C52 Re3 177.5(5) . . ? O11 C53 Re3 179.2(6) . . ? O12 C54 Re4 178.3(6) . . ? O13 C55 Re4 176.7(5) . . ? O14 C56 Re4 177.7(5) . . ? C5 N1 C4 116.7(4) . . ? C5 N1 Re1 122.0(3) . . ? C4 N1 Re1 121.3(3) . . ? C10 N2 C11 116.1(4) . . ? C10 N2 Re2 121.1(3) . 3_465 ? C11 N2 Re2 122.6(3) . 3_465 ? C24 N3 C25 115.3(4) . . ? C24 N3 Re4 124.6(3) . . ? C25 N3 Re4 120.2(3) . . ? C33 N4 C32 115.7(4) . . ? C33 N4 Re3 122.8(3) . 3_675 ? C32 N4 Re3 121.3(3) . 3_675 ? C17 O4 C14 105.9(5) . . ? C39 O15 C36 106.2(5) . . ? C47 Re1 C45 88.6(2) . . ? C47 Re1 C46 91.7(2) . . ? C45 Re1 C46 88.9(2) . . ? C47 Re1 N1 91.58(17) . . ? C45 Re1 N1 92.82(18) . . ? C46 Re1 N1 176.39(17) . . ? C47 Re1 S1 93.88(16) . . ? C45 Re1 S1 175.08(16) . . ? C46 Re1 S1 95.32(15) . . ? N1 Re1 S1 82.86(10) . . ? C47 Re1 S2 173.27(16) . . ? C45 Re1 S2 97.26(17) . . ? C46 Re1 S2 91.80(15) . . ? N1 Re1 S2 84.82(10) . . ? S1 Re1 S2 80.05(4) . . ? C49 Re2 C50 90.46(19) . . ? C49 Re2 C48 92.0(2) . . ? C50 Re2 C48 90.0(2) . . ? C49 Re2 N2 92.94(17) . 3_465 ? C50 Re2 N2 174.78(17) . 3_465 ? C48 Re2 N2 93.84(18) . 3_465 ? C49 Re2 S1 174.12(15) . . ? C50 Re2 S1 92.35(14) . . ? C48 Re2 S1 93.16(15) . . ? N2 Re2 S1 83.91(10) 3_465 . ? C49 Re2 S2 94.76(16) . . ? C50 Re2 S2 92.84(15) . . ? C48 Re2 S2 172.65(15) . . ? N2 Re2 S2 82.94(11) 3_465 . ? S1 Re2 S2 79.95(4) . . ? C52 Re3 C53 91.1(2) . . ? C52 Re3 C51 90.6(2) . . ? C53 Re3 C51 89.4(2) . . ? C52 Re3 N4 89.94(19) . 3_675 ? C53 Re3 N4 177.33(18) . 3_675 ? C51 Re3 N4 93.07(18) . 3_675 ? C52 Re3 S4 94.65(17) . . ? C53 Re3 S4 92.85(15) . . ? C51 Re3 S4 174.24(16) . . ? N4 Re3 S4 84.62(10) 3_675 . ? C52 Re3 S3 172.11(16) . . ? C53 Re3 S3 94.72(16) . . ? C51 Re3 S3 94.75(16) . . ? N4 Re3 S3 84.01(11) 3_675 . ? S4 Re3 S3 79.77(5) . . ? C55 Re4 C56 91.9(2) . . ? C55 Re4 C54 90.1(2) . . ? C56 Re4 C54 89.0(2) . . ? C55 Re4 N3 94.20(19) . . ? C56 Re4 N3 90.37(18) . . ? C54 Re4 N3 175.71(19) . . ? C55 Re4 S3 169.13(17) . . ? C56 Re4 S3 98.22(16) . . ? C54 Re4 S3 93.97(16) . . ? N3 Re4 S3 81.90(10) . . ? C55 Re4 S4 89.54(17) . . ? C56 Re4 S4 175.71(15) . . ? C54 Re4 S4 95.01(18) . . ? N3 Re4 S4 85.49(11) . . ? S3 Re4 S4 80.07(5) . . ? C13 S1 Re1 105.68(17) . . ? C13 S1 Re2 111.07(17) . . ? Re1 S1 Re2 98.22(4) . . ? C18A S2 Re1 109.06(18) . . ? C18A S2 Re2 108.15(17) . . ? Re1 S2 Re2 98.16(4) . . ? C35 S3 Re4 110.59(18) . . ? C35 S3 Re3 108.10(18) . . ? Re4 S3 Re3 98.98(5) . . ? C40A S4 Re3 110.1(2) . . ? C40A S4 Re4 103.7(2) . . ? Re3 S4 Re4 99.08(5) . . ? C19A C18A S2 113.2(4) . . ? C19A C18A H18A 108.9 . . ? S2 C18A H18A 108.9 . . ? C19A C18A H18B 108.9 . . ? S2 C18A H18B 108.9 . . ? H18A C18A H18B 107.7 . . ? C20A C19A O8A 111.2(6) . . ? C20A C19A C18A 132.7(7) . . ? O8A C19A C18A 116.2(6) . . ? C19A O8A C22A 106.7(7) . . ? C19A C20A C21A 106.3(8) . . ? C19A C20A H20A 126.8 . . ? C21A C20A H20A 126.8 . . ? C22A C21A C20A 109.6(9) . . ? C22A C21A H21A 125.2 . . ? C20A C21A H21A 125.2 . . ? C21A C22A O8A 106.1(9) . . ? C21A C22A H22A 127.0 . . ? O8A C22A H22A 126.9 . . ? C41A C40A S4 113.4(5) . . ? C41A C40A H40A 108.9 . . ? S4 C40A H40A 108.9 . . ? C41A C40A H40B 108.9 . . ? S4 C40A H40B 108.9 . . ? H40A C40A H40B 107.7 . . ? C42A C41A O16A 109.8(8) . . ? C42A C41A C40A 135.0(10) . . ? O16A C41A C40A 115.1(7) . . ? C44A O16A C41A 108.8(8) . . ? C41A C42A C43A 105.8(10) . . ? C41A C42A H42A 127.1 . . ? C43A C42A H42A 127.1 . . ? C44A C43A C42A 108.5(10) . . ? C44A C43A H43A 125.8 . . ? C42A C43A H43A 125.8 . . ? C43A C44A O16A 107.0(11) . . ? C43A C44A H44A 126.5 . . ? O16A C44A H44A 126.5 . . ? C20B C19B O8B 107.6(15) . . ? C22B O8B C19B 108.2(16) . . ? C19B C20B C21B 108.1(17) . . ? C19B C20B H20B 125.9 . . ? C21B C20B H20B 125.9 . . ? C22B C21B C20B 107.6(18) . . ? C22B C21B H21B 126.2 . . ? C20B C21B H21B 126.2 . . ? C21B C22B O8B 108.5(18) . . ? C21B C22B H22B 125.8 . . ? O8B C22B H22B 125.7 . . ? O16B C41B C42B 104.2(17) . . ? C44B O16B C41B 110.7(18) . . ? C43B C42B C41B 111.9(19) . . ? C43B C42B H42B 123.8 . . ? C41B C42B H42B 124.3 . . ? C42B C43B C44B 106.3(19) . . ? C42B C43B H43B 127.1 . . ? C44B C43B H43B 126.6 . . ? C43B C44B O16B 106.7(19) . . ? C43B C44B H44B 126.9 . . ? O16B C44B H44B 126.4 . . ? 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 C7 C1 C2 C6 -177.0(5) . . . . ? C7 C1 C2 C3 1.7(8) . . . . ? C6 C2 C3 C4 -0.6(7) . . . . ? C1 C2 C3 C4 -179.3(5) . . . . ? C2 C3 C4 N1 0.7(8) . . . . ? N1 C5 C6 C2 0.6(7) . . . . ? C3 C2 C6 C5 0.0(7) . . . . ? C1 C2 C6 C5 178.7(4) . . . . ? C2 C1 C7 C8 178.7(5) . . . . ? C1 C7 C8 C12 174.5(5) . . . . ? C1 C7 C8 C9 -7.7(8) . . . . ? C12 C8 C9 C10 -2.2(8) . . . . ? C7 C8 C9 C10 179.9(5) . . . . ? C8 C9 C10 N2 1.3(9) . . . . ? C9 C8 C12 C11 1.6(7) . . . . ? C7 C8 C12 C11 179.6(5) . . . . ? N2 C11 C12 C8 -0.1(8) . . . . ? S1 C13 C14 C15 119.1(7) . . . . ? S1 C13 C14 O4 -64.5(6) . . . . ? O4 C14 C15 C16 -0.8(8) . . . . ? C13 C14 C15 C16 175.6(6) . . . . ? C14 C15 C16 C17 0.9(9) . . . . ? C15 C16 C17 O4 -0.7(10) . . . . ? C27 C23 C24 N3 -2.1(8) . . . . ? N3 C25 C26 C27 -2.3(7) . . . . ? C24 C23 C27 C26 0.1(7) . . . . ? C24 C23 C27 C28 179.9(4) . . . . ? C25 C26 C27 C23 1.9(7) . . . . ? C25 C26 C27 C28 -177.8(4) . . . . ? C23 C27 C28 C29 174.1(5) . . . . ? C26 C27 C28 C29 -6.2(8) . . . . ? C27 C28 C29 C30 -178.8(5) . . . . ? C28 C29 C30 C31 12.4(8) . . . . ? C28 C29 C30 C34 -166.0(5) . . . . ? C34 C30 C31 C32 -0.3(7) . . . . ? C29 C30 C31 C32 -178.8(4) . . . . ? C30 C31 C32 N4 0.2(8) . . . . ? N4 C33 C34 C30 -1.7(8) . . . . ? C31 C30 C34 C33 1.0(8) . . . . ? C29 C30 C34 C33 179.5(5) . . . . ? S3 C35 C36 C37 115.1(6) . . . . ? S3 C35 C36 O15 -68.5(6) . . . . ? O15 C36 C37 C38 0.7(6) . . . . ? C35 C36 C37 C38 177.3(6) . . . . ? C36 C37 C38 C39 -0.4(7) . . . . ? C37 C38 C39 O15 -0.1(7) . . . . ? C6 C5 N1 C4 -0.5(7) . . . . ? C6 C5 N1 Re1 -179.6(3) . . . . ? C3 C4 N1 C5 -0.1(7) . . . . ? C3 C4 N1 Re1 178.9(4) . . . . ? C9 C10 N2 C11 0.2(7) . . . . ? C9 C10 N2 Re2 -175.1(4) . . . 3_465 ? C12 C11 N2 C10 -0.8(7) . . . . ? C12 C11 N2 Re2 174.4(4) . . . 3_465 ? C23 C24 N3 C25 1.8(7) . . . . ? C23 C24 N3 Re4 -178.8(4) . . . . ? C26 C25 N3 C24 0.3(7) . . . . ? C26 C25 N3 Re4 -179.1(4) . . . . ? C34 C33 N4 C32 1.5(7) . . . . ? C34 C33 N4 Re3 177.1(4) . . . 3_675 ? C31 C32 N4 C33 -0.8(7) . . . . ? C31 C32 N4 Re3 -176.4(4) . . . 3_675 ? C16 C17 O4 C14 0.3(10) . . . . ? C15 C14 O4 C17 0.4(8) . . . . ? C13 C14 O4 C17 -176.8(6) . . . . ? C38 C39 O15 C36 0.5(7) . . . . ? C37 C36 O15 C39 -0.8(6) . . . . ? C35 C36 O15 C39 -178.0(5) . . . . ? O3 C47 Re1 C45 -177(100) . . . . ? O3 C47 Re1 C46 -88(39) . . . . ? O3 C47 Re1 N1 90(39) . . . . ? O3 C47 Re1 S1 7(39) . . . . ? O3 C47 Re1 S2 33(39) . . . . ? O1 C45 Re1 C47 55(12) . . . . ? O1 C45 Re1 C46 -36(12) . . . . ? O1 C45 Re1 N1 147(12) . . . . ? O1 C45 Re1 S1 176(100) . . . . ? O1 C45 Re1 S2 -128(12) . . . . ? O2 C46 Re1 C47 -159(100) . . . . ? O2 C46 Re1 C45 -70(24) . . . . ? O2 C46 Re1 N1 48(26) . . . . ? O2 C46 Re1 S1 107(24) . . . . ? O2 C46 Re1 S2 27(24) . . . . ? C5 N1 Re1 C47 138.9(4) . . . . ? C4 N1 Re1 C47 -40.1(4) . . . . ? C5 N1 Re1 C45 50.2(4) . . . . ? C4 N1 Re1 C45 -128.8(4) . . . . ? C5 N1 Re1 C46 -68(3) . . . . ? C4 N1 Re1 C46 113(3) . . . . ? C5 N1 Re1 S1 -127.4(3) . . . . ? C4 N1 Re1 S1 53.6(4) . . . . ? C5 N1 Re1 S2 -46.8(3) . . . . ? C4 N1 Re1 S2 134.2(4) . . . . ? O6 C49 Re2 C50 34(25) . . . . ? O6 C49 Re2 C48 -56(26) . . . . ? O6 C49 Re2 N2 -150(25) . . . 3_465 ? O6 C49 Re2 S1 152(24) . . . . ? O6 C49 Re2 S2 127(25) . . . . ? O7 C50 Re2 C49 120(29) . . . . ? O7 C50 Re2 C48 -148(29) . . . . ? O7 C50 Re2 N2 -11(31) . . . 3_465 ? O7 C50 Re2 S1 -55(29) . . . . ? O7 C50 Re2 S2 25(29) . . . . ? O5 C48 Re2 C49 126(22) . . . . ? O5 C48 Re2 C50 36(22) . . . . ? O5 C48 Re2 N2 -141(22) . . . 3_465 ? O5 C48 Re2 S1 -57(22) . . . . ? O5 C48 Re2 S2 -77(22) . . . . ? O10 C52 Re3 C53 -122(11) . . . . ? O10 C52 Re3 C51 -33(11) . . . . ? O10 C52 Re3 N4 60(11) . . . 3_675 ? O10 C52 Re3 S4 145(11) . . . . ? O10 C52 Re3 S3 100(11) . . . . ? O11 C53 Re3 C52 -33(39) . . . . ? O11 C53 Re3 C51 -124(39) . . . . ? O11 C53 Re3 N4 80(39) . . . 3_675 ? O11 C53 Re3 S4 61(39) . . . . ? O11 C53 Re3 S3 141(39) . . . . ? O9 C51 Re3 C52 -92(33) . . . . ? O9 C51 Re3 C53 -1(33) . . . . ? O9 C51 Re3 N4 178(100) . . . 3_675 ? O9 C51 Re3 S4 112(33) . . . . ? O9 C51 Re3 S3 94(33) . . . . ? O13 C55 Re4 C56 -126(9) . . . . ? O13 C55 Re4 C54 -37(9) . . . . ? O13 C55 Re4 N3 144(9) . . . . ? O13 C55 Re4 S3 75(10) . . . . ? O13 C55 Re4 S4 58(9) . . . . ? O14 C56 Re4 C55 -31(12) . . . . ? O14 C56 Re4 C54 -121(12) . . . . ? O14 C56 Re4 N3 63(12) . . . . ? O14 C56 Re4 S3 145(12) . . . . ? O14 C56 Re4 S4 79(12) . . . . ? O12 C54 Re4 C55 -126(18) . . . . ? O12 C54 Re4 C56 -34(18) . . . . ? O12 C54 Re4 N3 48(19) . . . . ? O12 C54 Re4 S3 64(18) . . . . ? O12 C54 Re4 S4 144(18) . . . . ? C24 N3 Re4 C55 -45.6(4) . . . . ? C25 N3 Re4 C55 133.8(4) . . . . ? C24 N3 Re4 C56 -137.6(4) . . . . ? C25 N3 Re4 C56 41.8(4) . . . . ? C24 N3 Re4 C54 140(3) . . . . ? C25 N3 Re4 C54 -40(3) . . . . ? C24 N3 Re4 S3 124.2(4) . . . . ? C25 N3 Re4 S3 -56.4(3) . . . . ? C24 N3 Re4 S4 43.6(4) . . . . ? C25 N3 Re4 S4 -137.0(3) . . . . ? C14 C13 S1 Re1 173.0(4) . . . . ? C14 C13 S1 Re2 -81.5(4) . . . . ? C47 Re1 S1 C13 -53.8(2) . . . . ? C45 Re1 S1 C13 -173.7(19) . . . . ? C46 Re1 S1 C13 38.2(2) . . . . ? N1 Re1 S1 C13 -144.9(2) . . . . ? S2 Re1 S1 C13 129.12(18) . . . . ? C47 Re1 S1 Re2 -168.50(14) . . . . ? C45 Re1 S1 Re2 71.6(19) . . . . ? C46 Re1 S1 Re2 -76.48(15) . . . . ? N1 Re1 S1 Re2 100.38(10) . . . . ? S2 Re1 S1 Re2 14.42(4) . . . . ? C49 Re2 S1 C13 -150.9(14) . . . . ? C50 Re2 S1 C13 -32.3(2) . . . . ? C48 Re2 S1 C13 57.8(2) . . . . ? N2 Re2 S1 C13 151.3(2) 3_465 . . . ? S2 Re2 S1 C13 -124.79(18) . . . . ? C49 Re2 S1 Re1 -40.5(14) . . . . ? C50 Re2 S1 Re1 78.06(15) . . . . ? C48 Re2 S1 Re1 168.18(15) . . . . ? N2 Re2 S1 Re1 -98.30(11) 3_465 . . . ? S2 Re2 S1 Re1 -14.41(4) . . . . ? C47 Re1 S2 C18A -152.6(13) . . . . ? C45 Re1 S2 C18A 57.3(2) . . . . ? C46 Re1 S2 C18A -31.8(2) . . . . ? N1 Re1 S2 C18A 149.5(2) . . . . ? S1 Re1 S2 C18A -126.91(18) . . . . ? C47 Re1 S2 Re2 -40.1(13) . . . . ? C45 Re1 S2 Re2 169.75(15) . . . . ? C46 Re1 S2 Re2 80.67(15) . . . . ? N1 Re1 S2 Re2 -98.05(10) . . . . ? S1 Re1 S2 Re2 -14.42(4) . . . . ? C49 Re2 S2 C18A -55.0(2) . . . . ? C50 Re2 S2 C18A 35.7(2) . . . . ? C48 Re2 S2 C18A 148.3(12) . . . . ? N2 Re2 S2 C18A -147.4(2) 3_465 . . . ? S1 Re2 S2 C18A 127.61(18) . . . . ? C49 Re2 S2 Re1 -168.19(14) . . . . ? C50 Re2 S2 Re1 -77.49(14) . . . . ? C48 Re2 S2 Re1 35.1(12) . . . . ? N2 Re2 S2 Re1 99.43(11) 3_465 . . . ? S1 Re2 S2 Re1 14.40(4) . . . . ? C36 C35 S3 Re4 -63.0(4) . . . . ? C36 C35 S3 Re3 -170.3(4) . . . . ? C55 Re4 S3 C35 -141.4(9) . . . . ? C56 Re4 S3 C35 59.7(2) . . . . ? C54 Re4 S3 C35 -29.9(3) . . . . ? N3 Re4 S3 C35 148.9(2) . . . . ? S4 Re4 S3 C35 -124.26(19) . . . . ? C55 Re4 S3 Re3 -28.2(9) . . . . ? C56 Re4 S3 Re3 173.01(15) . . . . ? C54 Re4 S3 Re3 83.42(18) . . . . ? N3 Re4 S3 Re3 -97.79(11) . . . . ? S4 Re4 S3 Re3 -10.98(4) . . . . ? C52 Re3 S3 C35 171.7(12) . . . . ? C53 Re3 S3 C35 34.2(2) . . . . ? C51 Re3 S3 C35 -55.6(2) . . . . ? N4 Re3 S3 C35 -148.2(2) 3_675 . . . ? S4 Re3 S3 C35 126.24(19) . . . . ? C52 Re3 S3 Re4 56.5(12) . . . . ? C53 Re3 S3 Re4 -81.04(16) . . . . ? C51 Re3 S3 Re4 -170.80(15) . . . . ? N4 Re3 S3 Re4 96.60(11) 3_675 . . . ? S4 Re3 S3 Re4 11.01(4) . . . . ? C52 Re3 S4 C40A 66.4(3) . . . . ? C53 Re3 S4 C40A -25.0(3) . . . . ? C51 Re3 S4 C40A -137.6(15) . . . . ? N4 Re3 S4 C40A 155.9(3) 3_675 . . . ? S3 Re3 S4 C40A -119.3(2) . . . . ? C52 Re3 S4 Re4 174.67(16) . . . . ? C53 Re3 S4 Re4 83.32(17) . . . . ? C51 Re3 S4 Re4 -29.3(15) . . . . ? N4 Re3 S4 Re4 -95.83(11) 3_675 . . . ? S3 Re3 S4 Re4 -10.97(4) . . . . ? C55 Re4 S4 C40A -58.7(3) . . . . ? C56 Re4 S4 C40A -169(2) . . . . ? C54 Re4 S4 C40A 31.3(3) . . . . ? N3 Re4 S4 C40A -153.0(2) . . . . ? S3 Re4 S4 C40A 124.4(2) . . . . ? C55 Re4 S4 Re3 -172.14(17) . . . . ? C56 Re4 S4 Re3 78(2) . . . . ? C54 Re4 S4 Re3 -82.12(17) . . . . ? N3 Re4 S4 Re3 93.60(10) . . . . ? S3 Re4 S4 Re3 11.05(4) . . . . ? Re1 S2 C18A C19A -67.3(5) . . . . ? Re2 S2 C18A C19A -173.1(4) . . . . ? S2 C18A C19A C20A -58.9(8) . . . . ? S2 C18A C19A O8A 120.1(5) . . . . ? C20A C19A O8A C22A 1.7(8) . . . . ? C18A C19A O8A C22A -177.4(7) . . . . ? O8A C19A C20A C21A -0.4(8) . . . . ? C18A C19A C20A C21A 178.6(7) . . . . ? C19A C20A C21A C22A -1.2(11) . . . . ? C20A C21A C22A O8A 2.2(13) . . . . ? C19A O8A C22A C21A -2.4(11) . . . . ? Re3 S4 C40A C41A -71.4(6) . . . . ? Re4 S4 C40A C41A -176.7(5) . . . . ? S4 C40A C41A C42A 122.8(9) . . . . ? S4 C40A C41A O16A -60.9(8) . . . . ? C42A C41A O16A C44A -1.6(10) . . . . ? C40A C41A O16A C44A -178.9(7) . . . . ? O16A C41A C42A C43A -0.7(9) . . . . ? C40A C41A C42A C43A 175.7(8) . . . . ? C41A C42A C43A C44A 2.9(12) . . . . ? C42A C43A C44A O16A -3.8(12) . . . . ? C41A O16A C44A C43A 3.4(12) . . . . ? C20B C19B O8B C22B 0.2(19) . . . . ? O8B C19B C20B C21B 0(2) . . . . ? C19B C20B C21B C22B 0(4) . . . . ? C20B C21B C22B O8B 0(4) . . . . ? C19B O8B C22B C21B 0(4) . . . . ? C42B C41B O16B C44B 0(2) . . . . ? O16B C41B C42B C43B -2(2) . . . . ? C41B C42B C43B C44B 3(4) . . . . ? C42B C43B C44B O16B -3(4) . . . . ? C41B O16B C44B C43B 2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.358 _refine_diff_density_min -1.114 _refine_diff_density_rms 0.111 #===END# data_msdu02 _database_code_depnum_ccdc_archive 'CCDC 778833' #TrackingRef '- CCDC_Rev-4_778832-33.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H54 N12 O24 Re6 S6' _chemical_formula_weight 2924.95 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' 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' _symmetry_space_group_name_H-M 'P 31 2 1' _symmetry_cell_setting hexagonal loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' 'y, x, -z' '-x+y, -x, z+2/3' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 23.2217(3) _cell_length_b 23.2217(3) _cell_length_c 29.1908(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13632.2(4) _cell_formula_units_Z 6 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 20173 _cell_measurement_theta_min 2.4548 _cell_measurement_theta_max 29.3507 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8280 _exptl_absorpt_coefficient_mu 8.178 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.87685 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 151845 _diffrn_reflns_av_R_equivalents 0.1201 _diffrn_reflns_av_sigmaI/netI 0.1247 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 24.71 _reflns_number_total 15483 _reflns_number_gt 9321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis RED (Oxford, 2007)' _computing_cell_refinement 'CrysAlis RED (Oxford, 2007)' _computing_data_reduction 'CrysAlis RED (Oxford, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _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^)+(0.0090P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(6) _refine_ls_number_reflns 15483 _refine_ls_number_parameters 1141 _refine_ls_number_restraints 152 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.0451 _refine_ls_wR_factor_gt 0.0395 _refine_ls_goodness_of_fit_ref 0.814 _refine_ls_restrained_S_all 0.813 _refine_ls_shift/su_max 0.022 _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 1.3288(6) 1.0787(8) 0.0626(6) 0.089(5) Uani 1 1 d . . . C2 C 1.4327(7) 1.1139(6) 0.1181(5) 0.079(5) Uani 1 1 d . . . C3 C 1.4010(7) 1.0165(7) 0.0601(6) 0.077(6) Uani 1 1 d . . . C4 C 1.4573(6) 1.0102(6) 0.1808(5) 0.089(5) Uani 1 1 d . . . H4A H 1.4790 1.0581 0.1779 0.107 Uiso 1 1 calc R . . H4B H 1.4632 1.0001 0.2121 0.107 Uiso 1 1 calc R . . C5 C 1.4894(12) 0.9854(15) 0.1500(9) 0.188(5) Uani 1 1 d . . . C6 C 1.4798(7) 0.9318(7) 0.1424(7) 0.131(8) Uani 1 1 d . . . H6 H 1.4453 0.8931 0.1550 0.158 Uiso 1 1 calc R . . C7 C 1.5679(11) 0.9949(13) 0.1045(9) 0.188(5) Uani 1 1 d . . . H7 H 1.6054 1.0115 0.0859 0.226 Uiso 1 1 calc R . . C8 C 1.5251(10) 0.9332(10) 0.1129(8) 0.153(9) Uani 1 1 d U . . H8 H 1.5255 0.8964 0.1007 0.184 Uiso 1 1 calc R . . C9 C 1.1975(5) 0.9385(6) 0.1020(4) 0.052(4) Uani 1 1 d . . . H9 H 1.1969 0.9782 0.1043 0.063 Uiso 1 1 calc R . . C10 C 1.1369(5) 0.8802(5) 0.1043(4) 0.044(3) Uani 1 1 d . . . H10 H 1.0976 0.8807 0.1092 0.052 Uiso 1 1 calc R . . C11 C 1.1370(5) 0.8217(5) 0.0990(3) 0.025(3) Uani 1 1 d . . . C12 C 1.1965(5) 0.8237(5) 0.0899(3) 0.035(3) Uani 1 1 d . . . H12 H 1.1973 0.7847 0.0840 0.042 Uiso 1 1 calc R . . C13 C 1.2543(5) 0.8839(5) 0.0897(4) 0.050(3) Uani 1 1 d . . . H13 H 1.2940 0.8842 0.0844 0.060 Uiso 1 1 calc R . . C14 C 1.0732(6) 0.7592(6) 0.1029(4) 0.044(3) Uani 1 1 d . . . C15 C 0.9616(5) 0.6995(6) 0.1114(4) 0.027(3) Uani 1 1 d . . . C16 C 0.8968(4) 0.6977(5) 0.1138(4) 0.029(3) Uani 1 1 d . . . C17 C 0.8926(5) 0.7541(5) 0.1043(4) 0.059(4) Uani 1 1 d . . . H17 H 0.9306 0.7944 0.0978 0.070 Uiso 1 1 calc R . . C18 C 0.8309(5) 0.7492(6) 0.1046(4) 0.061(4) Uani 1 1 d . . . H18 H 0.8296 0.7881 0.0997 0.074 Uiso 1 1 calc R . . C19 C 0.7795(5) 0.6404(5) 0.1210(4) 0.043(3) Uani 1 1 d . . . H19 H 0.7409 0.6003 0.1269 0.051 Uiso 1 1 calc R . . C20 C 0.8390(5) 0.6419(5) 0.1227(4) 0.042(3) Uani 1 1 d . . . H20 H 0.8396 0.6032 0.1302 0.050 Uiso 1 1 calc R . . C21 C 1.0214(5) 0.6452(6) 0.1066(4) 0.041(4) Uani 1 1 d . . . C22 C 1.0196(5) 0.5800(5) 0.1065(4) 0.035(2) Uani 1 1 d U . . C23 C 0.9614(5) 0.5222(5) 0.1030(4) 0.037(2) Uani 1 1 d U . . H23 H 0.9213 0.5222 0.1017 0.044 Uiso 1 1 calc R . . C24 C 0.9623(5) 0.4652(5) 0.1016(3) 0.041(3) Uani 1 1 d . . . H24 H 0.9220 0.4258 0.0985 0.049 Uiso 1 1 calc R . . C25 C 1.0757(4) 0.5206(5) 0.1086(3) 0.034(3) Uani 1 1 d . . . H25 H 1.1156 0.5205 0.1116 0.041 Uiso 1 1 calc R . . C26 C 1.0789(5) 0.5803(5) 0.1086(3) 0.037(2) Uani 1 1 d U . . H26 H 1.1194 0.6198 0.1099 0.045 Uiso 1 1 calc R . . C27 C 0.7118(7) 0.7548(6) 0.0522(5) 0.072(4) Uani 1 1 d . . . C28 C 0.5922(6) 0.6834(6) 0.0888(5) 0.067(3) Uani 1 1 d . . . C29 C 0.6572(6) 0.6198(6) 0.0543(5) 0.067(3) Uani 1 1 d . . . C30 C 0.6649(8) 0.8148(7) 0.1566(7) 0.182(10) Uani 1 1 d U . . H30A H 0.6355 0.7981 0.1303 0.218 Uiso 1 1 calc R . . H30B H 0.6381 0.8091 0.1836 0.218 Uiso 1 1 calc R . . C31 C 0.7132(9) 0.8860(8) 0.1501(6) 0.105(6) Uani 1 1 d D . . C32 C 0.7766(11) 0.9273(9) 0.1523(6) 0.165(5) Uani 1 1 d D . . H32 H 0.8100 0.9163 0.1543 0.198 Uiso 1 1 calc R . . C33 C 0.7288(15) 0.9850(12) 0.1481(8) 0.27(2) Uani 1 1 d D . . H33 H 0.7199 1.0194 0.1429 0.330 Uiso 1 1 calc R . . C34 C 0.7861(14) 0.9958(12) 0.1508(6) 0.228(15) Uani 1 1 d DU . . H34 H 0.8256 1.0364 0.1518 0.274 Uiso 1 1 calc R . . C35 C 1.0936(6) 0.4038(6) 0.0633(5) 0.065(4) Uani 1 1 d . . . C36 C 0.9634(8) 0.3303(7) 0.0540(5) 0.079(5) Uani 1 1 d . . . C37 C 1.0212(8) 0.2875(9) 0.1033(5) 0.103(6) Uani 1 1 d . . . C38 C 0.8686(6) 0.2356(6) 0.1476(5) 0.092(5) Uani 1 1 d . . . H38A H 0.8679 0.2259 0.1152 0.110 Uiso 1 1 calc R . . H38B H 0.8881 0.2129 0.1636 0.110 Uiso 1 1 calc R . . C39 C 0.8000(7) 0.2088(8) 0.1634(5) 0.087(5) Uani 1 1 d . . . C40 C 0.7588(6) 0.1443(6) 0.1569(5) 0.052(4) Uani 1 1 d . . . H40 H 0.7705 0.1150 0.1440 0.063 Uiso 1 1 calc R . . C41 C 0.6986(6) 0.1795(9) 0.1879(5) 0.084(5) Uani 1 1 d . . . H41 H 0.6619 0.1802 0.2000 0.100 Uiso 1 1 calc R . . C42 C 0.7006(11) 0.1284(9) 0.1711(6) 0.114(7) Uani 1 1 d . . . H42 H 0.6641 0.0856 0.1696 0.137 Uiso 1 1 calc R . . C43 C 0.7031(6) 0.4511(6) 0.1598(4) 0.061(4) Uani 1 1 d . . . C44 C 0.7619(5) 0.3869(5) 0.1327(4) 0.043(3) Uani 1 1 d . . . C45 C 0.6435(5) 0.3171(5) 0.1694(4) 0.052(3) Uani 1 1 d . . . C46 C 0.6640(7) 0.2314(6) 0.0857(4) 0.068(4) Uani 1 1 d . . . H46A H 0.7108 0.2565 0.0938 0.082 Uiso 1 1 calc R . . H46B H 0.6392 0.2101 0.1133 0.082 Uiso 1 1 calc R . . C47 C 0.6542(7) 0.1810(8) 0.0529(5) 0.071(4) Uani 1 1 d . . . C48 C 0.6955(8) 0.1668(8) 0.0300(6) 0.097(5) Uani 1 1 d . . . H48 H 0.7416 0.1916 0.0311 0.117 Uiso 1 1 calc R . . C49 C 0.5942(11) 0.0900(8) 0.0091(6) 0.126(7) Uani 1 1 d . . . H49 H 0.5581 0.0537 -0.0045 0.151 Uiso 1 1 calc R . . C50 C 0.6584(11) 0.1086(11) 0.0039(6) 0.116(7) Uani 1 1 d . . . H50 H 0.6754 0.0872 -0.0137 0.139 Uiso 1 1 calc R . . C51 C 0.5841(5) 0.4298(5) 0.0873(4) 0.062(4) Uani 1 1 d . . . H51 H 0.6243 0.4691 0.0835 0.075 Uiso 1 1 calc R . . C52 C 0.5262(5) 0.4282(5) 0.0742(4) 0.051(3) Uani 1 1 d . . . H52 H 0.5281 0.4646 0.0595 0.061 Uiso 1 1 calc R . . C53 C 0.4653(5) 0.3721(5) 0.0832(4) 0.039(3) Uani 1 1 d . . . C54 C 0.4671(5) 0.3197(5) 0.1019(4) 0.041(3) Uani 1 1 d . . . H54 H 0.4273 0.2806 0.1076 0.049 Uiso 1 1 calc R . . C55 C 0.5261(5) 0.3229(5) 0.1126(4) 0.056(4) Uani 1 1 d . . . H55 H 0.5254 0.2859 0.1255 0.067 Uiso 1 1 calc R . . C56 C 0.4046(5) 0.3725(6) 0.0713(4) 0.030(3) Uani 1 1 d . . . C57 C 0.3511(6) 0.4263(6) 0.0502(4) 0.049(4) Uani 1 1 d . . . C58 C 0.3499(5) 0.4879(5) 0.0373(4) 0.044(3) Uani 1 1 d . . . C59 C 0.4084(5) 0.5489(5) 0.0406(3) 0.051(3) Uani 1 1 d . . . H59 H 0.4482 0.5508 0.0483 0.061 Uiso 1 1 calc R . . C60 C 0.4067(6) 0.6064(5) 0.0323(4) 0.055(4) Uani 1 1 d . . . H60 H 0.4459 0.6470 0.0353 0.066 Uiso 1 1 calc R . . C61 C 0.2951(5) 0.5447(5) 0.0165(4) 0.048(3) Uani 1 1 d . . . H61 H 0.2560 0.5433 0.0073 0.058 Uiso 1 1 calc R . . C62 C 0.2922(5) 0.4860(5) 0.0252(4) 0.044(3) Uani 1 1 d . . . H62 H 0.2524 0.4459 0.0231 0.053 Uiso 1 1 calc R . . C63 C 0.4085(7) 0.7469(5) 0.0544(4) 0.061(4) Uani 1 1 d . . . C64 C 0.2800(6) 0.6754(6) 0.0442(4) 0.051(4) Uani 1 1 d . . . C65 C 0.3508(6) 0.7780(6) -0.0136(4) 0.063(4) Uani 1 1 d . . . C66 C 0.4966(6) 0.8098(5) -0.0557(5) 0.080(5) Uani 1 1 d . . . H66A H 0.5145 0.8191 -0.0866 0.096 Uiso 1 1 calc R . . H66B H 0.4691 0.8301 -0.0522 0.096 Uiso 1 1 calc R . . C67 C 0.5535(7) 0.8413(7) -0.0220(6) 0.1003(12) Uani 1 1 d U . . C68 C 0.5950(6) 0.8252(7) -0.0116(5) 0.1003(12) Uani 1 1 d U . . H68 H 0.5940 0.7867 -0.0217 0.120 Uiso 1 1 calc R . . C69 C 0.6429(7) 0.8715(6) 0.0169(5) 0.1003(12) Uani 1 1 d U . . H69 H 0.6772 0.8677 0.0304 0.120 Uiso 1 1 calc R . . C70 C 0.6331(7) 0.9205(7) 0.0220(6) 0.1003(12) Uani 1 1 d U . . H70 H 0.6585 0.9591 0.0388 0.120 Uiso 1 1 calc R . . C71 C 0.2911(8) 0.3131(7) 0.0599(6) 0.1003(12) Uani 1 1 d . . . C72 C 0.2277(5) 0.2492(5) 0.0586(4) 0.050(3) Uani 1 1 d . . . C73 C 0.1672(5) 0.2467(5) 0.0574(4) 0.054(4) Uani 1 1 d . . . H73 H 0.1649 0.2855 0.0566 0.065 Uiso 1 1 calc R . . C74 C 0.1109(5) 0.1860(5) 0.0573(4) 0.062(4) Uani 1 1 d . . . H74 H 0.0705 0.1845 0.0534 0.074 Uiso 1 1 calc R . . C75 C 0.1693(5) 0.1301(5) 0.0647(4) 0.063(4) Uani 1 1 d . . . H75 H 0.1701 0.0906 0.0669 0.075 Uiso 1 1 calc R . . C76 C 0.2279(5) 0.1886(5) 0.0637(4) 0.057(4) Uani 1 1 d . . . H76 H 0.2680 0.1889 0.0664 0.069 Uiso 1 1 calc R . . C77 C 0.0484(6) 0.0027(8) 0.1139(6) 0.098(6) Uani 1 1 d U . . C78 C -0.0652(7) -0.0531(7) 0.0658(4) 0.061(4) Uani 1 1 d . . . C79 C -0.0238(7) 0.0669(6) 0.1053(5) 0.068(4) Uani 1 1 d . . . C80 C -0.0983(6) 0.0303(6) -0.0171(4) 0.065(4) Uani 1 1 d . . . H80A H -0.1065 0.0324 -0.0495 0.078 Uiso 1 1 calc R . . H80B H -0.1179 -0.0162 -0.0089 0.078 Uiso 1 1 calc R . . C81 C -0.1321(7) 0.0588(7) 0.0088(4) 0.059(3) Uani 1 1 d . . . C82 C -0.1848(9) 0.0333(8) 0.0318(10) 0.256(16) Uani 1 1 d U . . H82 H -0.2123 -0.0120 0.0369 0.308 Uiso 1 1 calc R . . C83 C -0.1962(10) 0.0834(10) 0.0488(9) 0.196(13) Uani 1 1 d U . . H83 H -0.2276 0.0782 0.0707 0.235 Uiso 1 1 calc R . . C84 C -0.1572(9) 0.1348(9) 0.0297(6) 0.097(6) Uani 1 1 d . . . H84 H -0.1567 0.1750 0.0319 0.117 Uiso 1 1 calc R . . N1 N 1.2573(5) 0.9430(5) 0.0967(3) 0.050(3) Uani 1 1 d . . . N2 N 0.7740(4) 0.6944(5) 0.1111(3) 0.053(3) Uani 1 1 d . . . N3 N 1.0198(4) 0.4613(4) 0.1047(3) 0.034(2) Uani 1 1 d . . . N4 N 0.5842(4) 0.3772(5) 0.1050(3) 0.046(3) Uani 1 1 d . . . N5 N 0.3519(4) 0.6066(4) 0.0203(3) 0.047(3) Uani 1 1 d . . . N6 N 0.1102(4) 0.1276(4) 0.0625(4) 0.058(3) Uani 1 1 d . . . N7 N 1.0169(4) 0.7598(4) 0.1053(3) 0.039(3) Uani 1 1 d . . . N8 N 0.9621(4) 0.6413(4) 0.1111(3) 0.031(2) Uani 1 1 d . . . N9 N 1.0772(4) 0.7033(5) 0.1026(3) 0.030(2) Uani 1 1 d . . . N10 N 0.4071(4) 0.4296(4) 0.0597(3) 0.030(2) Uani 1 1 d . . . N11 N 0.2902(4) 0.3689(5) 0.0474(3) 0.045(3) Uani 1 1 d . . . N12 N 0.3474(5) 0.3131(5) 0.0727(4) 0.055(3) Uani 1 1 d . . . O1 O 1.3145(5) 1.1075(6) 0.0343(4) 0.122(5) Uani 1 1 d U . . O2 O 1.4829(4) 1.1652(4) 0.1267(4) 0.120(4) Uani 1 1 d . . . O3 O 1.4301(5) 1.0067(6) 0.0335(4) 0.108(4) Uani 1 1 d . . . O4 O 1.5448(6) 1.0315(8) 0.1300(6) 0.188(5) Uani 1 1 d . . . O5 O 0.7303(5) 0.7960(4) 0.0239(4) 0.100(4) Uani 1 1 d . . . O6 O 0.5436(4) 0.6809(4) 0.0830(4) 0.100(3) Uani 1 1 d U . . O7 O 0.6426(5) 0.5771(4) 0.0277(3) 0.085(3) Uani 1 1 d . . . O8 O 0.6799(6) 0.9228(6) 0.1528(4) 0.122(5) Uani 1 1 d . . . O9 O 1.1395(4) 0.4271(5) 0.0386(3) 0.092(4) Uani 1 1 d . . . O10 O 0.9286(5) 0.3061(5) 0.0204(3) 0.087(3) Uani 1 1 d . . . O11 O 1.0217(6) 0.2353(6) 0.1047(4) 0.123(5) Uani 1 1 d . . . O12 O 0.7676(7) 0.2363(8) 0.1835(4) 0.181(6) Uani 1 1 d . . . O13 O 0.7192(5) 0.4958(4) 0.1873(3) 0.091(3) Uani 1 1 d . . . O14 O 0.8130(3) 0.3910(4) 0.1401(3) 0.071(3) Uani 1 1 d . . . O15 O 0.6261(4) 0.2778(4) 0.1999(3) 0.073(3) Uani 1 1 d . . . O16 O 0.5925(5) 0.1367(5) 0.0395(4) 0.108(3) Uani 1 1 d . . . O17 O 0.4462(5) 0.7773(5) 0.0838(4) 0.121(4) Uani 1 1 d U . . O18 O 0.2342(5) 0.6572(5) 0.0685(3) 0.097(4) Uani 1 1 d . . . O19 O 0.3510(5) 0.8251(5) -0.0254(4) 0.111(4) Uani 1 1 d . . . O20 O 0.5736(6) 0.9024(6) -0.0044(5) 0.165(5) Uani 1 1 d . . . O21 O 0.0717(5) -0.0132(5) 0.1447(3) 0.087(3) Uani 1 1 d . . . O22 O -0.1143(4) -0.1016(4) 0.0649(3) 0.079(3) Uani 1 1 d . . . O23 O -0.0519(5) 0.0826(5) 0.1293(4) 0.095(4) Uani 1 1 d . . . O24 O -0.1133(5) 0.1234(5) 0.0038(4) 0.121(4) Uani 1 1 d . . . S1 S 1.36783(13) 0.97431(14) 0.16943(12) 0.0504(9) Uani 1 1 d . . . S2 S 0.70777(15) 0.76762(15) 0.16351(14) 0.0738(13) Uani 1 1 d . . . S3 S 0.92155(14) 0.32547(14) 0.15620(12) 0.0511(9) Uani 1 1 d . . . S4 S 0.63812(14) 0.28781(13) 0.06450(10) 0.0447(8) Uani 1 1 d . . . S5 S 0.44590(14) 0.72215(14) -0.04893(11) 0.0535(9) Uani 1 1 d . . . S6 S -0.00898(13) 0.07072(13) -0.00805(11) 0.0484(9) Uani 1 1 d . . . Re1 Re 1.35184(2) 1.03733(2) 0.10601(2) 0.0646(2) Uani 1 1 d . . . Re2 Re 0.67673(2) 0.68706(2) 0.09847(2) 0.06090(19) Uani 1 1 d . . . Re3 Re 1.01839(2) 0.36517(2) 0.10259(2) 0.05077(16) Uani 1 1 d . . . Re4 Re 0.67862(2) 0.37953(2) 0.121811(17) 0.04233(14) Uani 1 1 d . . . Re5 Re 0.35175(3) 0.70005(2) 0.004459(17) 0.05083(15) Uani 1 1 d . . . Re6 Re 0.01733(2) 0.03134(2) 0.064534(19) 0.04705(13) Uani 1 1 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 0.037(9) 0.094(13) 0.138(17) 0.009(11) 0.017(10) 0.033(9) C2 0.076(11) 0.035(8) 0.141(16) 0.027(9) 0.023(10) 0.039(8) C3 0.037(9) 0.072(11) 0.116(17) 0.052(11) 0.004(9) 0.023(8) C4 0.060(10) 0.035(8) 0.148(15) 0.031(9) -0.041(10) 0.004(7) C5 0.105(10) 0.214(14) 0.264(15) -0.032(10) 0.051(9) 0.093(10) C6 0.099(13) 0.043(9) 0.28(2) 0.050(12) 0.114(14) 0.054(9) C7 0.105(10) 0.214(14) 0.264(15) -0.032(10) 0.051(9) 0.093(10) C8 0.103(16) 0.111(16) 0.26(3) -0.004(17) 0.039(16) 0.067(13) C9 0.039(7) 0.041(8) 0.076(11) 0.010(7) -0.009(7) 0.019(7) C10 0.030(7) 0.025(7) 0.061(9) 0.001(6) -0.008(6) 0.003(6) C11 0.022(6) 0.026(7) 0.022(7) 0.008(5) -0.007(5) 0.009(5) C12 0.016(6) 0.021(6) 0.057(9) -0.005(5) -0.001(5) 0.002(5) C13 0.034(8) 0.038(7) 0.077(11) 0.013(7) -0.007(7) 0.017(7) C14 0.052(9) 0.032(8) 0.034(9) 0.006(6) -0.019(7) 0.012(7) C15 0.006(6) 0.037(7) 0.031(8) -0.001(6) 0.000(5) 0.007(6) C16 0.007(6) 0.036(7) 0.042(8) -0.003(6) -0.003(5) 0.009(5) C17 0.033(7) 0.052(8) 0.091(11) 0.027(7) 0.015(7) 0.021(7) C18 0.030(7) 0.041(8) 0.113(12) 0.035(8) 0.025(7) 0.018(7) C19 0.032(7) 0.035(7) 0.071(10) 0.013(6) 0.004(6) 0.024(6) C20 0.020(7) 0.019(6) 0.081(11) 0.002(6) -0.012(6) 0.007(6) C21 0.008(6) 0.073(9) 0.036(9) 0.040(7) 0.009(6) 0.016(7) C22 0.032(4) 0.034(4) 0.050(5) 0.013(4) 0.001(4) 0.024(4) C23 0.029(4) 0.037(5) 0.052(5) 0.009(4) 0.005(4) 0.023(4) C24 0.027(6) 0.028(7) 0.056(9) 0.008(6) 0.003(6) 0.005(5) C25 0.020(6) 0.040(7) 0.041(8) 0.017(6) 0.010(5) 0.014(6) C26 0.031(4) 0.036(4) 0.053(5) 0.012(4) 0.006(4) 0.023(4) C27 0.061(10) 0.052(9) 0.118(15) -0.007(9) -0.023(9) 0.040(9) C28 0.030(5) 0.048(6) 0.107(10) 0.018(6) -0.017(6) 0.009(5) C29 0.030(5) 0.048(6) 0.107(10) 0.018(6) -0.017(6) 0.009(5) C30 0.083(11) 0.059(12) 0.44(3) 0.031(16) -0.020(15) 0.064(11) C31 0.119(14) 0.069(12) 0.164(18) -0.050(11) -0.050(12) 0.075(11) C32 0.145(10) 0.089(8) 0.252(13) -0.031(8) -0.068(10) 0.051(7) C33 0.21(3) 0.059(16) 0.34(4) 0.068(19) -0.10(3) -0.10(2) C34 0.17(3) 0.057(16) 0.34(4) 0.007(16) -0.05(2) -0.028(18) C35 0.037(8) 0.047(9) 0.098(13) 0.005(8) -0.009(8) 0.012(7) C36 0.128(15) 0.054(10) 0.066(12) 0.002(9) 0.043(11) 0.053(10) C37 0.103(14) 0.105(15) 0.107(15) 0.006(12) 0.017(11) 0.055(12) C38 0.056(10) 0.049(9) 0.163(17) -0.001(9) 0.024(9) 0.021(8) C39 0.039(9) 0.072(12) 0.147(17) 0.001(10) 0.019(9) 0.025(9) C40 0.021(7) 0.017(7) 0.096(12) -0.013(7) 0.014(7) -0.008(6) C41 0.025(8) 0.115(14) 0.067(11) 0.045(11) 0.027(7) 0.003(9) C42 0.17(2) 0.066(13) 0.109(17) -0.006(12) -0.005(15) 0.061(15) C43 0.035(8) 0.064(9) 0.084(11) -0.009(8) -0.006(8) 0.025(7) C44 0.034(7) 0.036(7) 0.050(9) 0.006(6) -0.005(6) 0.012(6) C45 0.045(8) 0.043(8) 0.067(9) -0.026(7) -0.002(8) 0.022(7) C46 0.116(12) 0.067(9) 0.051(10) -0.030(8) -0.028(8) 0.068(9) C47 0.055(10) 0.104(14) 0.066(12) 0.006(10) -0.015(9) 0.049(10) C48 0.087(13) 0.099(14) 0.107(16) -0.020(12) 0.001(11) 0.047(11) C49 0.141(19) 0.093(13) 0.119(17) -0.075(11) -0.004(14) 0.040(13) C50 0.130(18) 0.15(2) 0.073(15) -0.016(13) 0.013(14) 0.075(17) C51 0.033(8) 0.021(7) 0.131(13) 0.012(7) 0.004(7) 0.012(6) C52 0.046(8) 0.040(7) 0.079(10) 0.013(6) 0.004(7) 0.031(7) C53 0.018(6) 0.020(7) 0.064(10) -0.004(6) 0.003(6) -0.002(6) C54 0.020(6) 0.026(7) 0.083(10) -0.006(6) -0.003(6) 0.016(5) C55 0.029(7) 0.018(7) 0.120(12) 0.010(7) -0.020(7) 0.011(6) C56 0.012(6) 0.043(8) 0.031(9) 0.001(6) -0.007(6) 0.012(6) C57 0.034(8) 0.056(9) 0.053(10) -0.017(7) 0.006(7) 0.020(8) C58 0.027(7) 0.032(7) 0.067(10) 0.007(6) -0.014(6) 0.010(6) C59 0.038(7) 0.050(8) 0.057(9) 0.013(7) -0.019(6) 0.016(7) C60 0.037(8) 0.030(7) 0.089(11) 0.002(7) -0.021(7) 0.008(6) C61 0.008(6) 0.048(8) 0.066(10) 0.012(7) -0.003(6) -0.004(6) C62 0.035(7) 0.024(7) 0.071(10) 0.005(6) -0.020(6) 0.013(6) C63 0.077(10) 0.018(7) 0.061(10) 0.011(6) 0.008(8) 0.003(7) C64 0.083(10) 0.045(8) 0.033(9) 0.018(7) 0.017(7) 0.038(8) C65 0.065(9) 0.033(8) 0.076(11) 0.006(7) 0.013(8) 0.014(7) C66 0.047(9) 0.056(9) 0.121(13) 0.033(9) 0.019(9) 0.014(7) C67 0.0676(18) 0.0570(18) 0.173(2) -0.0375(19) -0.0472(19) 0.0284(16) C68 0.0676(18) 0.0570(18) 0.173(2) -0.0375(19) -0.0472(19) 0.0284(16) C69 0.0676(18) 0.0570(18) 0.173(2) -0.0375(19) -0.0472(19) 0.0284(16) C70 0.0676(18) 0.0570(18) 0.173(2) -0.0375(19) -0.0472(19) 0.0284(16) C71 0.0676(18) 0.0570(18) 0.173(2) -0.0375(19) -0.0472(19) 0.0284(16) C72 0.025(7) 0.029(7) 0.080(11) -0.011(7) -0.013(7) 0.002(6) C73 0.022(7) 0.043(7) 0.108(12) -0.041(7) -0.028(7) 0.023(6) C74 0.030(7) 0.030(7) 0.125(12) -0.017(7) -0.012(7) 0.014(6) C75 0.022(7) 0.009(6) 0.138(13) 0.004(7) 0.006(7) -0.006(6) C76 0.028(7) 0.034(8) 0.114(12) -0.004(7) -0.009(7) 0.019(6) C77 0.020(8) 0.115(14) 0.137(16) -0.096(13) -0.001(9) 0.018(8) C78 0.080(11) 0.079(11) 0.064(10) -0.001(9) -0.013(8) 0.069(9) C79 0.054(10) 0.041(9) 0.085(13) -0.007(9) -0.037(9) 0.007(7) C80 0.056(9) 0.063(9) 0.071(11) -0.015(8) -0.008(8) 0.027(8) C81 0.054(9) 0.053(9) 0.066(10) 0.003(8) -0.009(8) 0.024(8) C82 0.100(14) 0.035(10) 0.60(4) -0.032(17) 0.21(2) 0.006(10) C83 0.16(2) 0.081(15) 0.35(3) 0.047(18) 0.16(2) 0.057(15) C84 0.103(14) 0.122(17) 0.117(16) -0.027(12) -0.004(12) 0.094(14) N1 0.046(7) 0.062(8) 0.050(8) 0.012(6) -0.002(5) 0.033(6) N2 0.025(6) 0.036(6) 0.090(9) 0.003(6) -0.004(5) 0.010(5) N3 0.019(5) 0.032(6) 0.041(7) 0.014(4) 0.016(5) 0.005(5) N4 0.023(6) 0.044(7) 0.072(8) -0.005(6) -0.001(5) 0.017(5) N5 0.036(6) 0.031(6) 0.060(8) 0.007(5) -0.028(5) 0.007(5) N6 0.032(6) 0.040(6) 0.097(9) -0.028(6) -0.034(6) 0.013(5) N7 0.020(5) 0.046(7) 0.054(8) -0.003(5) -0.011(5) 0.017(5) N8 0.036(6) 0.016(5) 0.041(7) -0.008(5) 0.002(5) 0.014(5) N9 0.024(6) 0.031(6) 0.036(7) -0.009(5) -0.012(5) 0.014(5) N10 0.030(6) 0.014(5) 0.044(7) -0.012(5) -0.015(5) 0.011(4) N11 0.022(6) 0.036(6) 0.076(9) -0.011(6) -0.010(5) 0.012(5) N12 0.029(6) 0.038(6) 0.093(10) -0.016(7) -0.021(6) 0.014(6) O1 0.104(9) 0.165(11) 0.138(11) 0.106(9) 0.049(7) 0.098(8) O2 0.041(6) 0.037(6) 0.244(14) 0.009(7) 0.007(7) -0.008(5) O3 0.074(8) 0.123(10) 0.126(12) 0.023(8) 0.026(7) 0.049(7) O4 0.105(10) 0.214(14) 0.264(15) -0.032(10) 0.051(9) 0.093(10) O5 0.084(8) 0.050(6) 0.152(11) 0.050(6) 0.001(7) 0.023(6) O6 0.043(5) 0.077(6) 0.183(8) -0.009(5) -0.041(5) 0.031(4) O7 0.100(8) 0.060(6) 0.092(9) 0.021(6) -0.016(7) 0.038(6) O8 0.112(10) 0.088(9) 0.184(15) 0.006(8) -0.001(9) 0.064(8) O9 0.048(6) 0.115(9) 0.086(8) -0.015(7) 0.026(5) 0.022(6) O10 0.090(8) 0.075(7) 0.081(9) -0.031(7) 0.008(6) 0.030(6) O11 0.178(12) 0.098(9) 0.148(11) 0.002(8) 0.045(9) 0.111(9) O12 0.135(13) 0.240(18) 0.193(14) 0.024(12) 0.025(10) 0.114(14) O13 0.105(8) 0.057(6) 0.117(9) -0.047(6) -0.047(7) 0.046(6) O14 0.024(4) 0.073(6) 0.117(8) -0.001(5) -0.011(5) 0.025(5) O15 0.099(7) 0.064(6) 0.057(6) 0.011(5) 0.024(6) 0.041(6) O16 0.102(9) 0.094(8) 0.128(10) -0.028(7) -0.011(7) 0.050(7) O17 0.082(6) 0.065(6) 0.143(7) -0.013(5) -0.050(6) -0.019(5) O18 0.082(8) 0.124(10) 0.065(8) 0.005(7) 0.015(6) 0.037(7) O19 0.162(10) 0.050(6) 0.140(11) 0.022(6) 0.025(8) 0.068(7) O20 0.145(10) 0.089(8) 0.252(13) -0.031(8) -0.068(10) 0.051(7) O21 0.075(8) 0.115(9) 0.086(9) -0.006(7) -0.007(6) 0.057(7) O22 0.062(6) 0.040(6) 0.094(8) 0.005(5) -0.003(6) -0.007(5) O23 0.067(8) 0.108(9) 0.114(9) -0.046(7) -0.008(6) 0.047(6) O24 0.106(9) 0.087(8) 0.178(12) 0.033(7) 0.007(8) 0.054(7) S1 0.0231(16) 0.0319(18) 0.089(3) -0.0013(17) -0.0062(17) 0.0085(13) S2 0.033(2) 0.0388(19) 0.157(4) 0.002(2) -0.002(2) 0.0234(17) S3 0.0409(19) 0.0256(17) 0.083(3) -0.0048(17) 0.0066(18) 0.0141(15) S4 0.0424(19) 0.0366(18) 0.060(2) 0.0022(16) -0.0102(15) 0.0236(16) S5 0.0447(19) 0.0247(17) 0.087(3) 0.0060(17) -0.0099(17) 0.0139(15) S6 0.0240(17) 0.0256(17) 0.087(3) -0.0005(17) 0.0040(16) 0.0059(13) Re1 0.0283(3) 0.0347(3) 0.1238(6) 0.0268(3) 0.0037(3) 0.0105(3) Re2 0.0318(3) 0.0442(3) 0.1094(6) 0.0136(3) -0.0080(3) 0.0210(3) Re3 0.0465(3) 0.0356(3) 0.0738(5) -0.0029(3) 0.0144(3) 0.0231(3) Re4 0.0312(3) 0.0308(3) 0.0642(4) -0.0012(3) -0.0091(3) 0.0148(2) Re5 0.0522(3) 0.0354(3) 0.0616(4) 0.0061(3) -0.0065(3) 0.0195(3) Re6 0.0293(3) 0.0309(3) 0.0727(4) -0.0084(3) -0.0070(3) 0.0088(2) _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 O1 1.210(16) . ? C1 Re1 1.823(17) . ? C2 O2 1.205(14) . ? C2 Re1 1.863(15) . ? C3 O3 1.124(16) . ? C3 Re1 1.971(17) . ? C4 C5 1.46(2) . ? C4 S1 1.842(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.17(3) . ? C5 O4 1.33(3) . ? C6 C8 1.346(19) . ? C6 H6 0.9300 . ? C7 C8 1.29(2) . ? C7 O4 1.42(2) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 N1 1.348(12) . ? C9 C10 1.382(12) . ? C9 H9 0.9300 . ? C10 C11 1.367(12) . ? C10 H10 0.9300 . ? C11 C12 1.386(12) . ? C11 C14 1.472(13) . ? C12 C13 1.371(12) . ? C12 H12 0.9300 . ? C13 N1 1.354(12) . ? C13 H13 0.9300 . ? C14 N7 1.317(13) . ? C14 N9 1.347(13) . ? C15 N7 1.357(12) . ? C15 N8 1.359(12) . ? C15 C16 1.486(12) . ? C16 C20 1.346(12) . ? C16 C17 1.389(13) . ? C17 C18 1.379(13) . ? C17 H17 0.9300 . ? C18 N2 1.311(11) . ? C18 H18 0.9300 . ? C19 N2 1.353(12) . ? C19 C20 1.366(12) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 N9 1.328(12) . ? C21 N8 1.340(13) . ? C21 C22 1.493(15) . ? C22 C23 1.351(13) . ? C22 C26 1.375(12) . ? C23 C24 1.336(12) . ? C23 H23 0.9300 . ? C24 N3 1.385(11) . ? C24 H24 0.9300 . ? C25 N3 1.346(10) . ? C25 C26 1.351(12) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 O5 1.171(14) . ? C27 Re2 1.918(15) . ? C28 O6 1.112(12) . ? C28 Re2 1.943(12) . ? C29 O7 1.168(14) . ? C29 Re2 1.897(15) . ? C30 C31 1.474(19) . ? C30 S2 1.822(11) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.30(2) . ? C31 O8 1.412(15) . ? C32 C34 1.49(3) . ? C32 H32 0.9300 . ? C33 C34 1.23(4) . ? C33 O8 1.33(2) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 O9 1.170(13) . ? C35 Re3 1.899(14) . ? C36 O10 1.215(15) . ? C36 Re3 1.806(17) . ? C37 O11 1.219(16) . ? C37 Re3 1.838(18) . ? C38 C39 1.466(16) . ? C38 S3 1.835(12) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.328(16) . ? C39 O12 1.339(15) . ? C40 C42 1.277(19) . ? C40 H40 0.9300 . ? C41 C42 1.307(18) . ? C41 O12 1.486(16) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 O13 1.213(12) . ? C43 Re4 1.836(13) . ? C44 O14 1.161(11) . ? C44 Re4 1.882(11) . ? C45 O15 1.192(11) . ? C45 Re4 1.875(12) . ? C46 C47 1.440(17) . ? C46 S4 1.803(11) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.337(18) . ? C47 O16 1.339(14) . ? C48 C50 1.41(2) . ? C48 H48 0.9300 . ? C49 C50 1.34(2) . ? C49 O16 1.417(15) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 N4 1.329(12) . ? C51 C52 1.378(13) . ? C51 H51 0.9300 . ? C52 C53 1.388(13) . ? C52 H52 0.9300 . ? C53 C54 1.353(13) . ? C53 C56 1.457(13) . ? C54 C55 1.371(12) . ? C54 H54 0.9300 . ? C55 N4 1.326(12) . ? C55 H55 0.9300 . ? C56 N10 1.343(12) . ? C56 N12 1.354(12) . ? C57 N10 1.293(13) . ? C57 N11 1.377(13) . ? C57 C58 1.492(15) . ? C58 C62 1.364(13) . ? C58 C59 1.393(13) . ? C59 C60 1.377(13) . ? C59 H59 0.9300 . ? C60 N5 1.323(12) . ? C60 H60 0.9300 . ? C61 C62 1.354(13) . ? C61 N5 1.388(11) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 O17 1.177(13) . ? C63 Re5 1.899(13) . ? C64 O18 1.167(12) . ? C64 Re5 1.871(13) . ? C65 O19 1.143(12) . ? C65 Re5 1.898(13) . ? C66 C67 1.509(16) . ? C66 S5 1.781(11) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.234(16) . ? C67 O20 1.356(15) . ? C68 C69 1.375(15) . ? C68 H68 0.9300 . ? C69 C70 1.275(16) . ? C69 H69 0.9300 . ? C70 O20 1.449(16) . ? C70 H70 0.9300 . ? C71 N11 1.356(16) . ? C71 N12 1.358(16) . ? C71 C72 1.479(16) . ? C72 C73 1.375(13) . ? C72 C76 1.418(14) . ? C73 C74 1.361(12) . ? C73 H73 0.9300 . ? C74 N6 1.358(12) . ? C74 H74 0.9300 . ? C75 N6 1.346(12) . ? C75 C76 1.360(13) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C77 O21 1.200(18) . ? C77 Re6 1.88(2) . ? C78 O22 1.133(13) . ? C78 Re6 1.939(15) . ? C79 O23 1.137(14) . ? C79 Re6 1.948(16) . ? C80 C81 1.464(15) . ? C80 S6 1.818(11) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 C82 1.255(17) . ? C81 O24 1.345(13) . ? C82 C83 1.41(2) . ? C82 H82 0.9300 . ? C83 C84 1.22(2) . ? C83 H83 0.9300 . ? C84 O24 1.394(15) . ? C84 H84 0.9300 . ? N1 Re1 2.211(9) . ? N2 Re2 2.210(8) . ? N3 Re3 2.217(8) . ? N4 Re4 2.221(8) . ? N5 Re5 2.220(8) . ? N6 Re6 2.198(9) . ? S1 Re1 2.500(3) . ? S1 Re2 2.507(3) 6_765 ? S2 Re2 2.505(4) . ? S2 Re1 2.527(4) 6_765 ? S3 Re3 2.497(3) 6_765 ? S3 Re3 2.507(3) . ? S4 Re5 2.488(3) 3 ? S4 Re4 2.493(3) . ? S5 Re5 2.520(3) . ? S5 Re4 2.523(3) 3 ? S6 Re6 2.501(3) . ? S6 Re6 2.509(3) 3 ? Re1 S2 2.527(4) 6_765 ? Re2 S1 2.507(3) 6_765 ? Re3 S3 2.497(3) 6_765 ? Re4 S5 2.523(3) 3 ? Re5 S4 2.488(3) 3 ? Re6 S6 2.509(3) 3 ? 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 178.5(16) . . ? O2 C2 Re1 176.1(12) . . ? O3 C3 Re1 177.8(15) . . ? C5 C4 S1 113.2(13) . . ? C5 C4 H4A 108.9 . . ? S1 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? S1 C4 H4B 108.9 . . ? H4A C4 H4B 107.8 . . ? C6 C5 O4 111(2) . . ? C6 C5 C4 132(3) . . ? O4 C5 C4 116(2) . . ? C5 C6 C8 111.4(19) . . ? C5 C6 H6 124.3 . . ? C8 C6 H6 124.3 . . ? C8 C7 O4 104.6(19) . . ? C8 C7 H7 127.7 . . ? O4 C7 H7 127.7 . . ? C7 C8 C6 107.8(19) . . ? C7 C8 H8 126.1 . . ? C6 C8 H8 126.1 . . ? N1 C9 C10 125.8(12) . . ? N1 C9 H9 117.1 . . ? C10 C9 H9 117.1 . . ? C11 C10 C9 117.5(11) . . ? C11 C10 H10 121.2 . . ? C9 C10 H10 121.2 . . ? C10 C11 C12 119.0(9) . . ? C10 C11 C14 118.1(10) . . ? C12 C11 C14 122.9(10) . . ? C13 C12 C11 119.1(10) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? N1 C13 C12 124.0(11) . . ? N1 C13 H13 118.0 . . ? C12 C13 H13 118.0 . . ? N7 C14 N9 123.9(10) . . ? N7 C14 C11 120.6(11) . . ? N9 C14 C11 115.5(11) . . ? N7 C15 N8 123.4(9) . . ? N7 C15 C16 117.2(10) . . ? N8 C15 C16 119.1(9) . . ? C20 C16 C17 116.1(9) . . ? C20 C16 C15 123.0(10) . . ? C17 C16 C15 120.8(9) . . ? C18 C17 C16 118.7(10) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? N2 C18 C17 125.6(11) . . ? N2 C18 H18 117.2 . . ? C17 C18 H18 117.2 . . ? N2 C19 C20 123.2(10) . . ? N2 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C16 C20 C19 121.8(10) . . ? C16 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? N9 C21 N8 121.7(11) . . ? N9 C21 C22 123.3(10) . . ? N8 C21 C22 115.1(10) . . ? C23 C22 C26 120.8(10) . . ? C23 C22 C21 121.0(10) . . ? C26 C22 C21 118.3(10) . . ? C24 C23 C22 118.9(10) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 N3 123.8(9) . . ? C23 C24 H24 118.1 . . ? N3 C24 H24 118.1 . . ? N3 C25 C26 125.4(9) . . ? N3 C25 H25 117.3 . . ? C26 C25 H25 117.3 . . ? C25 C26 C22 117.0(10) . . ? C25 C26 H26 121.5 . . ? C22 C26 H26 121.5 . . ? O5 C27 Re2 176.7(12) . . ? O6 C28 Re2 179.4(15) . . ? O7 C29 Re2 177.3(13) . . ? C31 C30 S2 110.6(10) . . ? C31 C30 H30A 109.5 . . ? S2 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? S2 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? C32 C31 O8 108.2(14) . . ? C32 C31 C30 140.2(16) . . ? O8 C31 C30 109.4(14) . . ? C31 C32 C34 107(2) . . ? C31 C32 H32 126.4 . . ? C34 C32 H32 126.4 . . ? C34 C33 O8 118(4) . . ? C34 C33 H33 121.2 . . ? O8 C33 H33 121.2 . . ? C33 C34 C32 103(2) . . ? C33 C34 H34 128.7 . . ? C32 C34 H34 128.7 . . ? O9 C35 Re3 179.1(14) . . ? O10 C36 Re3 177.0(13) . . ? O11 C37 Re3 178.1(15) . . ? C39 C38 S3 114.0(9) . . ? C39 C38 H38A 108.7 . . ? S3 C38 H38A 108.7 . . ? C39 C38 H38B 108.8 . . ? S3 C38 H38B 108.7 . . ? H38A C38 H38B 107.6 . . ? C40 C39 O12 109.9(12) . . ? C40 C39 C38 116.7(14) . . ? O12 C39 C38 133.3(15) . . ? C42 C40 C39 109.9(14) . . ? C42 C40 H40 125.0 . . ? C39 C40 H40 125.0 . . ? C42 C41 O12 105.2(15) . . ? C42 C41 H41 127.4 . . ? O12 C41 H41 127.4 . . ? C40 C42 C41 111.8(18) . . ? C40 C42 H42 124.1 . . ? C41 C42 H42 124.1 . . ? O13 C43 Re4 175.7(11) . . ? O14 C44 Re4 178.9(11) . . ? O15 C45 Re4 174.7(10) . . ? C47 C46 S4 112.9(9) . . ? C47 C46 H46A 109.0 . . ? S4 C46 H46A 109.0 . . ? C47 C46 H46B 109.0 . . ? S4 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C48 C47 O16 106.7(14) . . ? C48 C47 C46 133.8(16) . . ? O16 C47 C46 119.5(14) . . ? C47 C48 C50 109.8(16) . . ? C47 C48 H48 125.1 . . ? C50 C48 H48 125.1 . . ? C50 C49 O16 106.1(16) . . ? C50 C49 H49 127.0 . . ? O16 C49 H49 127.0 . . ? C49 C50 C48 107.2(17) . . ? C49 C50 H50 126.4 . . ? C48 C50 H50 126.4 . . ? N4 C51 C52 122.2(10) . . ? N4 C51 H51 118.9 . . ? C52 C51 H51 118.9 . . ? C51 C52 C53 119.7(10) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C54 C53 C52 116.5(10) . . ? C54 C53 C56 124.5(9) . . ? C52 C53 C56 119.0(10) . . ? C53 C54 C55 121.4(10) . . ? C53 C54 H54 119.3 . . ? C55 C54 H54 119.3 . . ? N4 C55 C54 121.9(10) . . ? N4 C55 H55 119.1 . . ? C54 C55 H55 119.1 . . ? N10 C56 N12 123.2(10) . . ? N10 C56 C53 120.2(10) . . ? N12 C56 C53 116.6(10) . . ? N10 C57 N11 125.8(11) . . ? N10 C57 C58 119.8(11) . . ? N11 C57 C58 114.2(11) . . ? C62 C58 C59 119.5(10) . . ? C62 C58 C57 121.6(10) . . ? C59 C58 C57 118.8(10) . . ? C60 C59 C58 119.3(10) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? N5 C60 C59 122.9(10) . . ? N5 C60 H60 118.5 . . ? C59 C60 H60 118.5 . . ? C62 C61 N5 124.8(10) . . ? C62 C61 H61 117.6 . . ? N5 C61 H61 117.6 . . ? C61 C62 C58 117.6(10) . . ? C61 C62 H62 121.2 . . ? C58 C62 H62 121.2 . . ? O17 C63 Re5 176.7(12) . . ? O18 C64 Re5 177.1(12) . . ? O19 C65 Re5 178.4(13) . . ? C67 C66 S5 113.5(9) . . ? C67 C66 H66A 108.9 . . ? S5 C66 H66A 108.9 . . ? C67 C66 H66B 108.9 . . ? S5 C66 H66B 108.9 . . ? H66A C66 H66B 107.7 . . ? C68 C67 O20 108.1(14) . . ? C68 C67 C66 129.9(14) . . ? O20 C67 C66 121.0(13) . . ? C67 C68 C69 111.3(14) . . ? C67 C68 H68 124.4 . . ? C69 C68 H68 124.4 . . ? C70 C69 C68 109.4(14) . . ? C70 C69 H69 125.3 . . ? C68 C69 H69 125.3 . . ? C69 C70 O20 104.6(13) . . ? C69 C70 H70 127.7 . . ? O20 C70 H70 127.7 . . ? N11 C71 N12 123.1(13) . . ? N11 C71 C72 118.0(13) . . ? N12 C71 C72 118.9(13) . . ? C73 C72 C76 118.1(10) . . ? C73 C72 C71 121.8(12) . . ? C76 C72 C71 119.8(11) . . ? C74 C73 C72 118.4(11) . . ? C74 C73 H73 120.8 . . ? C72 C73 H73 120.8 . . ? N6 C74 C73 124.0(11) . . ? N6 C74 H74 118.0 . . ? C73 C74 H74 118.0 . . ? N6 C75 C76 122.1(11) . . ? N6 C75 H75 118.9 . . ? C76 C75 H75 118.9 . . ? C75 C76 C72 119.7(10) . . ? C75 C76 H76 120.1 . . ? C72 C76 H76 120.1 . . ? O21 C77 Re6 176.4(14) . . ? O22 C78 Re6 177.1(12) . . ? O23 C79 Re6 174.5(14) . . ? C81 C80 S6 115.1(9) . . ? C81 C80 H80A 108.5 . . ? S6 C80 H80A 108.5 . . ? C81 C80 H80B 108.5 . . ? S6 C80 H80B 108.5 . . ? H80A C80 H80B 107.5 . . ? C82 C81 O24 106.2(13) . . ? C82 C81 C80 132.9(14) . . ? O24 C81 C80 120.0(13) . . ? C81 C82 C83 110.0(15) . . ? C81 C82 H82 125.0 . . ? C83 C82 H82 125.0 . . ? C84 C83 C82 107.1(19) . . ? C84 C83 H83 126.5 . . ? C82 C83 H83 126.5 . . ? C83 C84 O24 108.6(17) . . ? C83 C84 H84 125.7 . . ? O24 C84 H84 125.7 . . ? C9 N1 C13 114.3(10) . . ? C9 N1 Re1 122.4(8) . . ? C13 N1 Re1 123.0(8) . . ? C18 N2 C19 114.4(9) . . ? C18 N2 Re2 123.1(8) . . ? C19 N2 Re2 122.0(7) . . ? C25 N3 C24 114.1(8) . . ? C25 N3 Re3 123.6(6) . . ? C24 N3 Re3 122.3(6) . . ? C55 N4 C51 118.1(9) . . ? C55 N4 Re4 120.6(8) . . ? C51 N4 Re4 121.3(7) . . ? C60 N5 C61 115.9(9) . . ? C60 N5 Re5 122.0(7) . . ? C61 N5 Re5 122.1(8) . . ? C75 N6 C74 117.4(9) . . ? C75 N6 Re6 120.3(7) . . ? C74 N6 Re6 122.3(7) . . ? C14 N7 C15 115.4(9) . . ? C21 N8 C15 117.0(9) . . ? C21 N9 C14 118.4(10) . . ? C57 N10 C56 116.7(9) . . ? C71 N11 C57 114.2(11) . . ? C56 N12 C71 116.6(11) . . ? C5 O4 C7 105(2) . . ? C33 O8 C31 103(2) . . ? C39 O12 C41 103.2(14) . . ? C47 O16 C49 110.0(13) . . ? C67 O20 C70 106.5(12) . . ? C81 O24 C84 107.1(12) . . ? C4 S1 Re1 109.5(4) . . ? C4 S1 Re2 105.8(5) . 6_765 ? Re1 S1 Re2 99.33(10) . 6_765 ? C30 S2 Re2 109.0(7) . . ? C30 S2 Re1 106.1(6) . 6_765 ? Re2 S2 Re1 98.66(10) . 6_765 ? C38 S3 Re3 109.6(5) . 6_765 ? C38 S3 Re3 107.5(4) . . ? Re3 S3 Re3 99.30(10) 6_765 . ? C46 S4 Re5 114.1(5) . 3 ? C46 S4 Re4 105.7(4) . . ? Re5 S4 Re4 100.05(10) 3 . ? C66 S5 Re5 108.2(4) . . ? C66 S5 Re4 106.6(4) . 3 ? Re5 S5 Re4 98.39(10) . 3 ? C80 S6 Re6 111.0(4) . . ? C80 S6 Re6 105.1(4) . 3 ? Re6 S6 Re6 98.99(9) . 3 ? C1 Re1 C2 92.9(6) . . ? C1 Re1 C3 90.9(6) . . ? C2 Re1 C3 86.1(6) . . ? C1 Re1 N1 91.7(5) . . ? C2 Re1 N1 175.4(5) . . ? C3 Re1 N1 94.8(5) . . ? C1 Re1 S1 172.3(4) . . ? C2 Re1 S1 92.6(4) . . ? C3 Re1 S1 94.9(4) . . ? N1 Re1 S1 82.8(2) . . ? C1 Re1 S2 93.9(5) . 6_765 ? C2 Re1 S2 93.3(4) . 6_765 ? C3 Re1 S2 175.2(4) . 6_765 ? N1 Re1 S2 85.4(3) . 6_765 ? S1 Re1 S2 80.34(11) . 6_765 ? C29 Re2 C27 91.4(6) . . ? C29 Re2 C28 92.6(5) . . ? C27 Re2 C28 86.6(5) . . ? C29 Re2 N2 89.5(4) . . ? C27 Re2 N2 93.2(5) . . ? C28 Re2 N2 177.9(5) . . ? C29 Re2 S2 172.3(4) . . ? C27 Re2 S2 94.4(4) . . ? C28 Re2 S2 92.8(4) . . ? N2 Re2 S2 85.1(3) . . ? C29 Re2 S1 93.7(4) . 6_765 ? C27 Re2 S1 174.9(4) . 6_765 ? C28 Re2 S1 92.7(4) . 6_765 ? N2 Re2 S1 87.4(3) . 6_765 ? S2 Re2 S1 80.63(11) . 6_765 ? C36 Re3 C37 86.1(6) . . ? C36 Re3 C35 90.8(6) . . ? C37 Re3 C35 89.7(6) . . ? C36 Re3 N3 97.2(5) . . ? C37 Re3 N3 176.7(6) . . ? C35 Re3 N3 89.6(4) . . ? C36 Re3 S3 171.1(5) . 6_765 ? C37 Re3 S3 93.2(5) . 6_765 ? C35 Re3 S3 98.0(4) . 6_765 ? N3 Re3 S3 83.6(2) . 6_765 ? C36 Re3 S3 91.3(4) . . ? C37 Re3 S3 95.6(5) . . ? C35 Re3 S3 174.4(4) . . ? N3 Re3 S3 84.9(2) . . ? S3 Re3 S3 79.93(10) 6_765 . ? C43 Re4 C45 94.0(5) . . ? C43 Re4 C44 88.6(5) . . ? C45 Re4 C44 88.6(5) . . ? C43 Re4 N4 90.6(4) . . ? C45 Re4 N4 95.9(4) . . ? C44 Re4 N4 175.6(4) . . ? C43 Re4 S4 173.0(4) . . ? C45 Re4 S4 90.2(3) . . ? C44 Re4 S4 97.1(3) . . ? N4 Re4 S4 83.4(2) . . ? C43 Re4 S5 96.3(4) . 3 ? C45 Re4 S5 169.6(3) . 3 ? C44 Re4 S5 90.4(3) . 3 ? N4 Re4 S5 85.3(3) . 3 ? S4 Re4 S5 79.68(9) . 3 ? C64 Re5 C65 91.8(5) . . ? C64 Re5 C63 87.5(5) . . ? C65 Re5 C63 90.2(5) . . ? C64 Re5 N5 90.5(4) . . ? C65 Re5 N5 175.8(4) . . ? C63 Re5 N5 93.4(4) . . ? C64 Re5 S4 98.2(4) . 3 ? C65 Re5 S4 92.2(4) . 3 ? C63 Re5 S4 173.8(4) . 3 ? N5 Re5 S4 84.0(2) . 3 ? C64 Re5 S5 174.7(3) . . ? C65 Re5 S5 93.3(4) . . ? C63 Re5 S5 94.3(4) . . ? N5 Re5 S5 84.4(3) . . ? S4 Re5 S5 79.84(9) 3 . ? C77 Re6 C78 89.3(5) . . ? C77 Re6 C79 92.2(5) . . ? C78 Re6 C79 88.3(5) . . ? C77 Re6 N6 91.5(5) . . ? C78 Re6 N6 179.2(4) . . ? C79 Re6 N6 91.5(5) . . ? C77 Re6 S6 171.0(4) . . ? C78 Re6 S6 95.0(3) . . ? C79 Re6 S6 95.8(4) . . ? N6 Re6 S6 84.3(3) . . ? C77 Re6 S6 91.3(4) . 3 ? C78 Re6 S6 93.3(4) . 3 ? C79 Re6 S6 176.1(4) . 3 ? N6 Re6 S6 86.8(3) . 3 ? S6 Re6 S6 80.58(9) . 3 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.377 _refine_diff_density_min -1.298 _refine_diff_density_rms 0.121 #===END#