Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_paper _publ_contact_author ; Dr Patrick Batail Laboratoire Chimie Inorganique, Mat\'eriaux et Interfaces, FRE 2447 CNRS-Universit\'e d'Angers, Bat. K, 2, Boulevard Lavoisier, Angers, France ; _publ_contact_author_email patrick.batail@univ-angers.fr _publ_contact_author_fax '33 2 41 73 50 11' _publ_contact_author_phone '33 2 41 73 52 64' _publ_requested_journal 'Journal of Chemical Society Chemical Communication' _publ_requested_category FM loop_ _publ_author_name _publ_author_address 'Baudron, Stephane A.' ; Laboratoire Chimie Inorganique, Mat\'eriaux et Interfaces, FRE 2447 CNRS-Universit\'e d'Angers, Bat. K, 2, Boulevard Lavoisier, Angers, France ; 'Deluzet, Andr\'e' ; Laboratoire Chimie Inorganique, Mat\'eriaux et Interfaces, FRE 2447 CNRS-Universit\'e d'Angers, Bat. K, 2, Boulevard Lavoisier, Angers, France ; 'Boubekeur, Kamal' ; Laboratoire Chimie Inorganique, Mat\'eriaux et Interfaces, FRE 2447 CNRS-Universit\'e d'Angers, Bat. K, 2, Boulevard Lavoisier, Angers, France ; 'Batail, Patrick' ; Laboratoire Chimie Inorganique, Mat\'eriaux et Interfaces, FRE 2447 CNRS-Universit\'e d'Angers, Bat. K, 2, Boulevard Lavoisier, Angers, France ; _publ_section_title ; Jahn-Teller core distortion and isomerism in crystals of the open-shell 23-electron chalcogenide rhenium cluster series, {[Re6Q8]3+(X-)6}3- (Q == S, Se ; X == Cl, CN), ; #################### Material relevant to compound 1 at 150K ############ data_test3 _database_code_CSD 186991 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris (tetrabutylammonium)(octa-\m~eq~3-sulfido-hexachloro-octahedro- rhenate(IV)pentarhenate(III)) ; _chemical_name_common '(TBA)3[Re6S8Cl6]' _chemical_formula_moiety '(N(C4H9)4)3 [Re6S8Cl6]' _chemical_formula_sum 'C48 H108 Cl6 N3 Re6 S8' _chemical_formula_weight 2313.75 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.422(3) _cell_length_b 17.341(4) _cell_length_c 18.197(4) _cell_angle_alpha 96.07(3) _cell_angle_beta 106.44(3) _cell_angle_gamma 103.89(3) _cell_volume 3585.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2194 _exptl_absorpt_coefficient_mu 10.576 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0629 _exptl_absorpt_correction_T_max 0.7324 _exptl_absorpt_process_details 'FACEIT (Stoe IPDS)' _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_radiation_detector 'area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'Oscillation, \D\f==1.2%' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13792 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.82 _reflns_number_total 13792 _reflns_number_gt 10165 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS)' _computing_cell_refinement 'SELECT (Stoe IPDS)' _computing_data_reduction 'INTEGRATE (Stoe IPDS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0873P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13792 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_restrained_S_all 0.889 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1A Re -0.05936(3) 0.583922(18) 0.469820(18) 0.01478(9) Uani 1 1 d . . . Re2A Re -0.14357(3) 0.426679(18) 0.446522(18) 0.01509(9) Uani 1 1 d . . . Re3A Re 0.04464(3) 0.490077(18) 0.412641(17) 0.01444(9) Uani 1 1 d . . . S1A S -0.1465(2) 0.49954(13) 0.34176(11) 0.0200(4) Uani 1 1 d . . . S2A S -0.2275(2) 0.51957(13) 0.50408(12) 0.0187(4) Uani 1 1 d . . . S3A S 0.0354(2) 0.65448(12) 0.60224(12) 0.0194(5) Uani 1 1 d . . . S4A S 0.1188(2) 0.63620(11) 0.44113(12) 0.0183(4) Uani 1 1 d . . . Cl1A Cl -0.1357(2) 0.69586(13) 0.43056(13) 0.0252(5) Uani 1 1 d . . . Cl3A Cl 0.1063(2) 0.47898(12) 0.29916(12) 0.0238(5) Uani 1 1 d . . . Cl2A Cl -0.3338(2) 0.33219(13) 0.37689(13) 0.0252(5) Uani 1 1 d . . . Re1B Re -0.06056(3) 0.087071(18) -0.004835(18) 0.01404(9) Uani 1 1 d . . . Re2B Re 0.12503(3) 0.059414(18) 0.084772(17) 0.01400(9) Uani 1 1 d . . . Re3B Re -0.08199(3) -0.036047(18) 0.065642(18) 0.01403(9) Uani 1 1 d . . . S1B S -0.0956(2) 0.05805(12) -0.14341(11) 0.0179(4) Uani 1 1 d . . . S2B S -0.24697(19) -0.00775(12) -0.02179(12) 0.0176(4) Uani 1 1 d . . . S3B S 0.1350(2) 0.16879(12) 0.01424(12) 0.0196(4) Uani 1 1 d . . . S4B S -0.0161(2) 0.10274(13) 0.13455(12) 0.0193(4) Uani 1 1 d . . . Cl1B Cl -0.1422(2) 0.20081(13) -0.01560(13) 0.0251(5) Uani 1 1 d . . . Cl2B Cl 0.2906(2) 0.13282(13) 0.19712(12) 0.0244(5) Uani 1 1 d . . . Cl3B Cl -0.1874(2) -0.08372(14) 0.15295(12) 0.0252(5) Uani 1 1 d . . . N1C N 0.6745(7) 0.1736(4) 0.1786(4) 0.0212(16) Uani 1 1 d . . . C1C C 0.7600(9) 0.2247(5) 0.1471(5) 0.025(2) Uani 1 1 d . . . H1C1 H 0.7251 0.2176 0.0911 0.030 Uiso 1 1 calc R . . H1C2 H 0.8289 0.2053 0.1568 0.030 Uiso 1 1 calc R . . C2C C 0.7989(10) 0.3158(6) 0.1820(5) 0.030(2) Uani 1 1 d . . . H2C1 H 0.7309 0.3333 0.1836 0.036 Uiso 1 1 calc R . . H2C2 H 0.8511 0.3252 0.2351 0.036 Uiso 1 1 calc R . . C3C C 0.8616(10) 0.3656(6) 0.1334(6) 0.033(2) Uani 1 1 d . . . H3C1 H 0.9031 0.4195 0.1635 0.040 Uiso 1 1 calc R . . H3C2 H 0.9190 0.3407 0.1226 0.040 Uiso 1 1 calc R . . C4C C 0.7771(10) 0.3719(6) 0.0563(6) 0.035(2) Uani 1 1 d . . . H4C1 H 0.8202 0.4030 0.0279 0.053 Uiso 1 1 calc R . . H4C2 H 0.7215 0.3980 0.0666 0.053 Uiso 1 1 calc R . . H4C3 H 0.7366 0.3187 0.0259 0.053 Uiso 1 1 calc R . . C5C C 0.5691(8) 0.2065(5) 0.1738(5) 0.0223(19) Uani 1 1 d . . . H5C1 H 0.5130 0.1688 0.1901 0.027 Uiso 1 1 calc R . . H5C2 H 0.5954 0.2572 0.2105 0.027 Uiso 1 1 calc R . . C6C C 0.5070(9) 0.2206(6) 0.0935(5) 0.030(2) Uani 1 1 d . . . H6C1 H 0.5633 0.2349 0.0661 0.036 Uiso 1 1 calc R . . H6C2 H 0.4486 0.1709 0.0637 0.036 Uiso 1 1 calc R . . C7C C 0.4471(11) 0.2883(6) 0.0983(6) 0.038(3) Uani 1 1 d . . . H7C1 H 0.5022 0.3352 0.1353 0.046 Uiso 1 1 calc R . . H7C2 H 0.3815 0.2701 0.1172 0.046 Uiso 1 1 calc R . . C8C C 0.4041(11) 0.3119(8) 0.0198(7) 0.048(3) Uani 1 1 d . . . H8C1 H 0.3676 0.3542 0.0250 0.072 Uiso 1 1 calc R . . H8C2 H 0.3483 0.2658 -0.0167 0.072 Uiso 1 1 calc R . . H8C3 H 0.4691 0.3307 0.0013 0.072 Uiso 1 1 calc R . . C9C C 0.6334(8) 0.0885(5) 0.1280(5) 0.0209(19) Uani 1 1 d . . . H9C1 H 0.5846 0.0908 0.0767 0.025 Uiso 1 1 calc R . . H9C2 H 0.7017 0.0744 0.1217 0.025 Uiso 1 1 calc R . . C10C C 0.5660(10) 0.0213(5) 0.1580(5) 0.028(2) Uani 1 1 d . . . H10A H 0.5014 0.0363 0.1697 0.034 Uiso 1 1 calc R . . H10B H 0.6168 0.0122 0.2057 0.034 Uiso 1 1 calc R . . C11C C 0.5186(9) -0.0571(5) 0.0953(5) 0.025(2) Uani 1 1 d . . . H11A H 0.4593 -0.0499 0.0508 0.030 Uiso 1 1 calc R . . H11B H 0.5819 -0.0664 0.0776 0.030 Uiso 1 1 calc R . . C12C C 0.4662(12) -0.1307(6) 0.1256(7) 0.045(3) Uani 1 1 d . . . H12A H 0.4384 -0.1776 0.0850 0.067 Uiso 1 1 calc R . . H12B H 0.4022 -0.1223 0.1419 0.067 Uiso 1 1 calc R . . H12C H 0.5249 -0.1386 0.1691 0.067 Uiso 1 1 calc R . . C13C C 0.7291(8) 0.1710(5) 0.2639(5) 0.0206(19) Uani 1 1 d . . . H13A H 0.7517 0.2252 0.2940 0.025 Uiso 1 1 calc R . . H13B H 0.6703 0.1373 0.2814 0.025 Uiso 1 1 calc R . . C14C C 0.8351(8) 0.1389(5) 0.2808(5) 0.0222(19) Uani 1 1 d . . . H14A H 0.9017 0.1795 0.2775 0.027 Uiso 1 1 calc R . . H14B H 0.8198 0.0912 0.2422 0.027 Uiso 1 1 calc R . . C15C C 0.8634(10) 0.1176(6) 0.3625(5) 0.031(2) Uani 1 1 d . . . H15A H 0.8776 0.1653 0.4009 0.038 Uiso 1 1 calc R . . H15B H 0.7967 0.0769 0.3655 0.038 Uiso 1 1 calc R . . C16C C 0.9699(12) 0.0860(8) 0.3816(7) 0.052(3) Uani 1 1 d . . . H16A H 0.9852 0.0733 0.4330 0.078 Uiso 1 1 calc R . . H16B H 1.0364 0.1265 0.3796 0.078 Uiso 1 1 calc R . . H16C H 0.9555 0.0382 0.3443 0.078 Uiso 1 1 calc R . . N1D N -0.0347(7) 0.6889(4) 0.1910(4) 0.0197(16) Uani 1 1 d . . . C1D C -0.0674(8) 0.6853(5) 0.1039(5) 0.0206(19) Uani 1 1 d . . . H1D1 H 0.0008 0.7153 0.0925 0.025 Uiso 1 1 calc R . . H1D2 H -0.1271 0.7131 0.0888 0.025 Uiso 1 1 calc R . . C2D C -0.1123(9) 0.6015(5) 0.0528(5) 0.024(2) Uani 1 1 d . . . H2D1 H -0.0600 0.5695 0.0724 0.029 Uiso 1 1 calc R . . H2D2 H -0.1891 0.5746 0.0550 0.029 Uiso 1 1 calc R . . C3D C -0.1201(11) 0.6070(6) -0.0308(5) 0.034(2) Uani 1 1 d . . . H3D1 H -0.0431 0.6345 -0.0323 0.041 Uiso 1 1 calc R . . H3D2 H -0.1718 0.6397 -0.0495 0.041 Uiso 1 1 calc R . . C4D C -0.1646(13) 0.5252(6) -0.0856(6) 0.047(3) Uani 1 1 d . . . H4D1 H -0.1674 0.5331 -0.1374 0.071 Uiso 1 1 calc R . . H4D2 H -0.2416 0.4981 -0.0855 0.071 Uiso 1 1 calc R . . H4D3 H -0.1128 0.4929 -0.0683 0.071 Uiso 1 1 calc R . . C5D C -0.0001(8) 0.7791(5) 0.2288(5) 0.0217(19) Uani 1 1 d . . . H5D1 H 0.0566 0.8093 0.2075 0.026 Uiso 1 1 calc R . . H5D2 H -0.0690 0.7983 0.2139 0.026 Uiso 1 1 calc R . . C6D C 0.0504(10) 0.7979(6) 0.3158(5) 0.032(2) Uani 1 1 d . . . H6D1 H 0.1261 0.7873 0.3315 0.038 Uiso 1 1 calc R . . H6D2 H -0.0006 0.7632 0.3380 0.038 Uiso 1 1 calc R . . C7D C 0.0643(10) 0.8875(6) 0.3468(6) 0.035(2) Uani 1 1 d . . . H7D1 H 0.1108 0.9217 0.3215 0.042 Uiso 1 1 calc R . . H7D2 H -0.0122 0.8968 0.3336 0.042 Uiso 1 1 calc R . . C8D C 0.1221(14) 0.9101(7) 0.4335(6) 0.058(4) Uani 1 1 d . . . H8D1 H 0.1288 0.9659 0.4505 0.087 Uiso 1 1 calc R . . H8D2 H 0.1986 0.9021 0.4467 0.087 Uiso 1 1 calc R . . H8D3 H 0.0757 0.8769 0.4588 0.087 Uiso 1 1 calc R . . C9D C -0.1349(9) 0.6402(5) 0.2130(5) 0.024(2) Uani 1 1 d . . . H9D1 H -0.1099 0.6437 0.2691 0.029 Uiso 1 1 calc R . . H9D2 H -0.1528 0.5839 0.1892 0.029 Uiso 1 1 calc R . . C10D C -0.2472(10) 0.6666(7) 0.1889(7) 0.040(3) Uani 1 1 d . . . H10C H -0.2322 0.7215 0.2156 0.048 Uiso 1 1 calc R . . H10D H -0.2711 0.6661 0.1332 0.048 Uiso 1 1 calc R . . C11D C -0.3451(10) 0.6110(7) 0.2087(7) 0.039(3) Uani 1 1 d . . . H11C H -0.4091 0.6352 0.2026 0.047 Uiso 1 1 calc R . . H11D H -0.3169 0.6060 0.2629 0.047 Uiso 1 1 calc R . . C12D C -0.3911(11) 0.5267(8) 0.1577(8) 0.053(3) Uani 1 1 d . . . H12D H -0.4529 0.4943 0.1727 0.079 Uiso 1 1 calc R . . H12E H -0.3287 0.5017 0.1645 0.079 Uiso 1 1 calc R . . H12F H -0.4205 0.5310 0.1040 0.079 Uiso 1 1 calc R . . C13D C 0.0667(8) 0.6536(5) 0.2199(5) 0.0197(18) Uani 1 1 d . . . H13C H 0.0878 0.6600 0.2763 0.024 Uiso 1 1 calc R . . H13D H 0.0402 0.5960 0.1988 0.024 Uiso 1 1 calc R . . C14D C 0.1753(8) 0.6902(6) 0.1994(5) 0.025(2) Uani 1 1 d . . . H14C H 0.1948 0.7487 0.2112 0.030 Uiso 1 1 calc R . . H14D H 0.1608 0.6738 0.1440 0.030 Uiso 1 1 calc R . . C15D C 0.2772(9) 0.6622(6) 0.2460(6) 0.028(2) Uani 1 1 d . . . H15C H 0.2541 0.6036 0.2381 0.034 Uiso 1 1 calc R . . H15D H 0.2956 0.6829 0.3011 0.034 Uiso 1 1 calc R . . C16D C 0.3861(10) 0.6911(7) 0.2216(7) 0.041(3) Uani 1 1 d . . . H16D H 0.4481 0.6722 0.2518 0.062 Uiso 1 1 calc R . . H16E H 0.4103 0.7491 0.2306 0.062 Uiso 1 1 calc R . . H16F H 0.3684 0.6702 0.1673 0.062 Uiso 1 1 calc R . . N1E N 0.3806(7) 0.2219(5) 0.4669(4) 0.0250(17) Uani 1 1 d . . . C1E C 0.2798(9) 0.2395(6) 0.4077(5) 0.030(2) Uani 1 1 d . . . H1E1 H 0.2257 0.1880 0.3783 0.035 Uiso 1 1 calc R . . H1E2 H 0.2389 0.2653 0.4363 0.035 Uiso 1 1 calc R . . C2E C 0.3071(10) 0.2909(6) 0.3503(5) 0.031(2) Uani 1 1 d . . . H2E1 H 0.3575 0.2712 0.3257 0.037 Uiso 1 1 calc R . . H2E2 H 0.3471 0.3464 0.3768 0.037 Uiso 1 1 calc R . . C3E C 0.1907(9) 0.2867(6) 0.2886(5) 0.028(2) Uani 1 1 d . . . H3E1 H 0.1450 0.2305 0.2704 0.034 Uiso 1 1 calc R . . H3E2 H 0.1468 0.3144 0.3130 0.034 Uiso 1 1 calc R . . C4E C 0.2051(9) 0.3234(6) 0.2194(5) 0.031(2) Uani 1 1 d . . . H4E1 H 0.1294 0.3185 0.1833 0.046 Uiso 1 1 calc R . . H4E2 H 0.2470 0.2957 0.1942 0.046 Uiso 1 1 calc R . . H4E3 H 0.2481 0.3796 0.2366 0.046 Uiso 1 1 calc R . . C5E C 0.4772(10) 0.3011(6) 0.5112(6) 0.033(2) Uani 1 1 d . . . H5E1 H 0.5436 0.2873 0.5440 0.040 Uiso 1 1 calc R . . H5E2 H 0.5031 0.3296 0.4734 0.040 Uiso 1 1 calc R . . C6E C 0.4391(9) 0.3578(6) 0.5618(6) 0.032(2) Uani 1 1 d . . . H6E1 H 0.4206 0.3321 0.6033 0.039 Uiso 1 1 calc R . . H6E2 H 0.3691 0.3690 0.5305 0.039 Uiso 1 1 calc R . . C7E C 0.5382(9) 0.4384(6) 0.5977(6) 0.038(3) Uani 1 1 d . . . H7E1 H 0.6112 0.4267 0.6222 0.045 Uiso 1 1 calc R . . H7E2 H 0.5485 0.4680 0.5567 0.045 Uiso 1 1 calc R . . C8E C 0.5081(13) 0.4898(7) 0.6578(7) 0.054(3) Uani 1 1 d . . . H8E1 H 0.5702 0.5391 0.6797 0.081 Uiso 1 1 calc R . . H8E2 H 0.4982 0.4605 0.6984 0.081 Uiso 1 1 calc R . . H8E3 H 0.4367 0.5023 0.6331 0.081 Uiso 1 1 calc R . . C9E C 0.4426(10) 0.1709(7) 0.4271(6) 0.037(3) Uani 1 1 d . . . H9E1 H 0.4671 0.1987 0.3884 0.045 Uiso 1 1 calc R . . H9E2 H 0.5126 0.1680 0.4661 0.045 Uiso 1 1 calc R . . C10E C 0.3676(10) 0.0845(7) 0.3871(6) 0.037(3) Uani 1 1 d . . . H10E H 0.2996 0.0862 0.3455 0.044 Uiso 1 1 calc R . . H10F H 0.3406 0.0561 0.4246 0.044 Uiso 1 1 calc R . . C11E C 0.4419(11) 0.0396(7) 0.3533(7) 0.043(3) Uani 1 1 d . . . H11E H 0.4683 0.0680 0.3157 0.052 Uiso 1 1 calc R . . H11F H 0.5103 0.0387 0.3950 0.052 Uiso 1 1 calc R . . C12E C 0.3691(12) -0.0480(8) 0.3134(7) 0.058(4) Uani 1 1 d . . . H12G H 0.4165 -0.0752 0.2932 0.087 Uiso 1 1 calc R . . H12H H 0.3023 -0.0471 0.2714 0.087 Uiso 1 1 calc R . . H12I H 0.3433 -0.0762 0.3507 0.087 Uiso 1 1 calc R . . C13E C 0.3285(9) 0.1790(6) 0.5221(5) 0.027(2) Uani 1 1 d . . . H13E H 0.2644 0.1326 0.4913 0.032 Uiso 1 1 calc R . . H13F H 0.2953 0.2152 0.5470 0.032 Uiso 1 1 calc R . . C14E C 0.4095(9) 0.1499(6) 0.5858(5) 0.027(2) Uani 1 1 d . . . H14E H 0.4697 0.1960 0.6210 0.033 Uiso 1 1 calc R . . H14F H 0.4475 0.1159 0.5627 0.033 Uiso 1 1 calc R . . C15E C 0.3399(12) 0.1023(7) 0.6311(7) 0.043(3) Uani 1 1 d . . . H15E H 0.3916 0.0803 0.6682 0.051 Uiso 1 1 calc R . . H15F H 0.2791 0.0572 0.5951 0.051 Uiso 1 1 calc R . . C16E C 0.2832(11) 0.1520(9) 0.6752(7) 0.052(3) Uani 1 1 d . . . H16G H 0.2403 0.1180 0.7018 0.078 Uiso 1 1 calc R . . H16H H 0.2308 0.1734 0.6389 0.078 Uiso 1 1 calc R . . H16I H 0.3429 0.1957 0.7125 0.078 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 Re1A 0.0186(2) 0.01070(15) 0.01805(16) 0.00563(12) 0.00707(14) 0.00688(14) Re2A 0.0177(2) 0.01103(15) 0.01768(16) 0.00387(12) 0.00621(14) 0.00494(14) Re3A 0.0185(2) 0.01024(15) 0.01702(16) 0.00449(12) 0.00709(14) 0.00594(13) S1A 0.0241(14) 0.0199(10) 0.0182(9) 0.0075(8) 0.0049(9) 0.0108(9) S2A 0.0162(13) 0.0191(10) 0.0225(10) 0.0063(8) 0.0063(9) 0.0066(9) S3A 0.0281(14) 0.0106(9) 0.0208(10) 0.0030(8) 0.0094(9) 0.0055(9) S4A 0.0262(14) 0.0087(9) 0.0233(10) 0.0060(8) 0.0113(9) 0.0054(9) Cl1A 0.0320(14) 0.0200(10) 0.0362(11) 0.0154(9) 0.0174(11) 0.0180(10) Cl3A 0.0339(14) 0.0210(10) 0.0240(10) 0.0084(8) 0.0159(10) 0.0118(10) Cl2A 0.0146(13) 0.0224(11) 0.0314(11) -0.0034(8) 0.0058(9) -0.0024(9) Re1B 0.0148(2) 0.01141(15) 0.01927(16) 0.00625(12) 0.00697(14) 0.00650(13) Re2B 0.0137(2) 0.01224(16) 0.01772(16) 0.00536(12) 0.00542(14) 0.00506(13) Re3B 0.0141(2) 0.01308(16) 0.01814(16) 0.00678(12) 0.00687(14) 0.00602(13) S1B 0.0168(13) 0.0186(10) 0.0196(9) 0.0082(8) 0.0056(9) 0.0057(9) S2B 0.0140(12) 0.0188(10) 0.0233(10) 0.0079(8) 0.0072(9) 0.0073(9) S3B 0.0202(13) 0.0142(10) 0.0264(10) 0.0088(8) 0.0089(10) 0.0049(9) S4B 0.0209(13) 0.0179(10) 0.0222(10) 0.0030(8) 0.0085(9) 0.0094(9) Cl1B 0.0304(14) 0.0196(10) 0.0357(11) 0.0130(9) 0.0161(10) 0.0164(10) Cl2B 0.0205(13) 0.0247(11) 0.0241(10) 0.0046(8) 0.0024(9) 0.0048(9) Cl3B 0.0246(13) 0.0308(11) 0.0296(10) 0.0180(9) 0.0156(10) 0.0112(10) N1C 0.026(5) 0.018(4) 0.024(4) 0.007(3) 0.011(3) 0.011(3) C1C 0.026(6) 0.024(5) 0.027(4) 0.006(4) 0.012(4) 0.007(4) C2C 0.041(7) 0.026(5) 0.028(5) 0.007(4) 0.015(5) 0.013(5) C3C 0.036(7) 0.025(5) 0.034(5) 0.002(4) 0.010(5) 0.001(5) C4C 0.051(8) 0.023(5) 0.037(5) 0.012(4) 0.015(5) 0.015(5) C5C 0.022(6) 0.023(5) 0.026(4) 0.008(4) 0.011(4) 0.009(4) C6C 0.029(6) 0.033(5) 0.030(5) 0.011(4) 0.007(4) 0.011(5) C7C 0.041(8) 0.022(5) 0.051(6) 0.013(4) 0.008(5) 0.013(5) C8C 0.033(8) 0.050(7) 0.063(7) 0.035(6) 0.006(6) 0.020(6) C9C 0.015(5) 0.023(5) 0.018(4) 0.000(3) 0.002(4) 0.000(4) C10C 0.045(7) 0.023(5) 0.017(4) 0.002(3) 0.012(4) 0.009(5) C11C 0.021(6) 0.024(5) 0.024(4) -0.003(4) 0.002(4) 0.002(4) C12C 0.064(9) 0.023(5) 0.046(6) 0.009(5) 0.018(6) 0.008(5) C13C 0.026(6) 0.019(4) 0.021(4) 0.003(3) 0.012(4) 0.007(4) C14C 0.018(5) 0.021(4) 0.029(4) 0.006(4) 0.008(4) 0.005(4) C15C 0.037(7) 0.027(5) 0.033(5) 0.012(4) 0.010(5) 0.013(5) C16C 0.052(9) 0.065(8) 0.050(7) 0.026(6) 0.014(6) 0.037(7) N1D 0.025(5) 0.016(3) 0.026(4) 0.013(3) 0.012(3) 0.012(3) C1D 0.023(6) 0.019(4) 0.020(4) 0.011(3) 0.004(4) 0.006(4) C2D 0.031(6) 0.017(4) 0.027(4) 0.006(3) 0.009(4) 0.010(4) C3D 0.052(8) 0.021(5) 0.027(5) 0.002(4) 0.013(5) 0.009(5) C4D 0.094(11) 0.022(5) 0.027(5) 0.006(4) 0.016(6) 0.021(6) C5D 0.024(6) 0.006(4) 0.036(5) 0.007(3) 0.009(4) 0.005(4) C6D 0.046(7) 0.022(5) 0.033(5) 0.013(4) 0.016(5) 0.013(5) C7D 0.042(7) 0.022(5) 0.038(5) 0.003(4) 0.013(5) 0.008(5) C8D 0.093(12) 0.031(6) 0.038(6) -0.003(5) 0.014(7) 0.006(7) C9D 0.038(6) 0.017(4) 0.028(4) 0.011(3) 0.017(4) 0.014(4) C10D 0.042(8) 0.042(6) 0.057(7) 0.025(5) 0.029(6) 0.032(6) C11D 0.028(7) 0.040(6) 0.057(7) 0.015(5) 0.023(6) 0.010(5) C12D 0.025(8) 0.052(8) 0.069(8) -0.005(6) 0.017(6) -0.007(6) C13D 0.019(5) 0.013(4) 0.025(4) 0.007(3) 0.004(4) 0.004(4) C14D 0.021(6) 0.023(5) 0.033(5) 0.010(4) 0.010(4) 0.007(4) C15D 0.017(6) 0.026(5) 0.037(5) 0.002(4) 0.003(4) 0.005(4) C16D 0.020(7) 0.043(6) 0.056(7) 0.012(5) 0.007(5) 0.006(5) N1E 0.014(5) 0.035(4) 0.029(4) 0.013(3) 0.012(4) 0.005(4) C1E 0.032(7) 0.034(5) 0.032(5) 0.013(4) 0.012(5) 0.022(5) C2E 0.051(8) 0.024(5) 0.021(4) 0.008(4) 0.013(5) 0.015(5) C3E 0.033(6) 0.027(5) 0.028(5) 0.009(4) 0.009(4) 0.014(4) C4E 0.028(7) 0.031(5) 0.028(5) 0.005(4) 0.000(4) 0.007(5) C5E 0.035(7) 0.040(6) 0.035(5) 0.017(4) 0.016(5) 0.020(5) C6E 0.021(6) 0.033(6) 0.045(6) 0.014(4) 0.008(5) 0.011(5) C7E 0.009(6) 0.040(6) 0.048(6) 0.016(5) -0.003(5) -0.014(4) C8E 0.064(10) 0.034(6) 0.052(7) 0.007(5) 0.004(7) 0.011(6) C9E 0.045(8) 0.047(6) 0.038(5) 0.021(5) 0.024(5) 0.028(6) C10E 0.038(7) 0.053(7) 0.033(5) 0.014(5) 0.017(5) 0.030(6) C11E 0.038(8) 0.058(8) 0.042(6) 0.009(5) 0.013(6) 0.029(6) C12E 0.051(10) 0.067(9) 0.053(7) -0.011(6) 0.000(6) 0.041(8) C13E 0.019(6) 0.034(5) 0.027(4) 0.010(4) 0.006(4) 0.005(4) C14E 0.019(6) 0.034(5) 0.030(5) 0.010(4) 0.006(4) 0.009(4) C15E 0.058(9) 0.037(6) 0.045(6) 0.024(5) 0.020(6) 0.025(6) C16E 0.044(8) 0.082(10) 0.055(7) 0.043(7) 0.032(7) 0.031(7) _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 Re1A S2A 2.400(2) . ? Re1A S3A 2.402(2) . ? Re1A S4A 2.405(2) . ? Re1A S1A 2.415(2) . ? Re1A Cl1A 2.443(2) . ? Re1A Re3A 2.5935(8) 2_566 ? Re1A Re3A 2.6100(8) . ? Re1A Re2A 2.6106(10) 2_566 ? Re1A Re2A 2.6161(9) . ? Re2A S1A 2.393(2) . ? Re2A S4A 2.396(2) 2_566 ? Re2A S2A 2.418(2) . ? Re2A Cl2A 2.425(3) . ? Re2A S3A 2.428(2) 2_566 ? Re2A Re3A 2.5970(12) 2_566 ? Re2A Re3A 2.6039(9) . ? Re2A Re1A 2.6106(10) 2_566 ? Re3A Cl3A 2.4022(19) . ? Re3A S2A 2.402(2) 2_566 ? Re3A S1A 2.414(2) . ? Re3A S3A 2.419(2) 2_566 ? Re3A S4A 2.423(2) . ? Re3A Re1A 2.5935(8) 2_566 ? Re3A Re2A 2.5970(12) 2_566 ? S2A Re3A 2.402(2) 2_566 ? S3A Re3A 2.419(2) 2_566 ? S3A Re2A 2.428(2) 2_566 ? S4A Re2A 2.396(2) 2_566 ? Re1B S3B 2.408(2) . ? Re1B S4B 2.409(2) . ? Re1B S1B 2.410(2) . ? Re1B S2B 2.413(2) . ? Re1B Cl1B 2.426(2) . ? Re1B Re2B 2.6023(10) . ? Re1B Re3B 2.6025(8) . ? Re1B Re2B 2.6061(11) 2 ? Re1B Re3B 2.6071(8) 2 ? Re2B S1B 2.397(2) 2 ? Re2B S3B 2.398(2) . ? Re2B S2B 2.414(2) 2 ? Re2B Cl2B 2.417(3) . ? Re2B S4B 2.418(2) . ? Re2B Re3B 2.6028(8) 2 ? Re2B Re1B 2.6061(11) 2 ? Re2B Re3B 2.6081(11) . ? Re3B S1B 2.401(2) 2 ? Re3B S2B 2.403(2) . ? Re3B Cl3B 2.420(2) . ? Re3B S3B 2.422(2) 2 ? Re3B S4B 2.423(2) . ? Re3B Re2B 2.6028(8) 2 ? Re3B Re1B 2.6071(8) 2 ? S1B Re2B 2.397(2) 2 ? S1B Re3B 2.401(2) 2 ? S2B Re2B 2.414(2) 2 ? S3B Re3B 2.422(2) 2 ? N1C C1C 1.498(11) . ? N1C C13C 1.517(11) . ? N1C C5C 1.534(11) . ? N1C C9C 1.540(11) . ? C1C C2C 1.544(12) . ? C1C H1C1 0.9700 . ? C1C H1C2 0.9700 . ? C2C C3C 1.537(13) . ? C2C H2C1 0.9700 . ? C2C H2C2 0.9700 . ? C3C C4C 1.528(14) . ? C3C H3C1 0.9700 . ? C3C H3C2 0.9700 . ? C4C H4C1 0.9600 . ? C4C H4C2 0.9600 . ? C4C H4C3 0.9600 . ? C5C C6C 1.523(12) . ? C5C H5C1 0.9700 . ? C5C H5C2 0.9700 . ? C6C C7C 1.539(14) . ? C6C H6C1 0.9700 . ? C6C H6C2 0.9700 . ? C7C C8C 1.514(14) . ? C7C H7C1 0.9700 . ? C7C H7C2 0.9700 . ? C8C H8C1 0.9600 . ? C8C H8C2 0.9600 . ? C8C H8C3 0.9600 . ? C9C C10C 1.510(12) . ? C9C H9C1 0.9700 . ? C9C H9C2 0.9700 . ? C10C C11C 1.551(12) . ? C10C H10A 0.9700 . ? C10C H10B 0.9700 . ? C11C C12C 1.521(13) . ? C11C H11A 0.9700 . ? C11C H11B 0.9700 . ? C12C H12A 0.9600 . ? C12C H12B 0.9600 . ? C12C H12C 0.9600 . ? C13C C14C 1.515(12) . ? C13C H13A 0.9700 . ? C13C H13B 0.9700 . ? C14C C15C 1.535(12) . ? C14C H14A 0.9700 . ? C14C H14B 0.9700 . ? C15C C16C 1.516(15) . ? C15C H15A 0.9700 . ? C15C H15B 0.9700 . ? C16C H16A 0.9600 . ? C16C H16B 0.9600 . ? C16C H16C 0.9600 . ? N1D C1D 1.512(10) . ? N1D C9D 1.507(11) . ? N1D C13D 1.516(11) . ? N1D C5D 1.546(10) . ? C1D C2D 1.523(12) . ? C1D H1D1 0.9700 . ? C1D H1D2 0.9700 . ? C2D C3D 1.511(12) . ? C2D H2D1 0.9700 . ? C2D H2D2 0.9700 . ? C3D C4D 1.525(13) . ? C3D H3D1 0.9700 . ? C3D H3D2 0.9700 . ? C4D H4D1 0.9600 . ? C4D H4D2 0.9600 . ? C4D H4D3 0.9600 . ? C5D C6D 1.495(13) . ? C5D H5D1 0.9700 . ? C5D H5D2 0.9700 . ? C6D C7D 1.546(13) . ? C6D H6D1 0.9700 . ? C6D H6D2 0.9700 . ? C7D C8D 1.501(15) . ? C7D H7D1 0.9700 . ? C7D H7D2 0.9700 . ? C8D H8D1 0.9600 . ? C8D H8D2 0.9600 . ? C8D H8D3 0.9600 . ? C9D C10D 1.534(14) . ? C9D H9D1 0.9700 . ? C9D H9D2 0.9700 . ? C10D C11D 1.515(14) . ? C10D H10C 0.9700 . ? C10D H10D 0.9700 . ? C11D C12D 1.529(16) . ? C11D H11C 0.9700 . ? C11D H11D 0.9700 . ? C12D H12D 0.9600 . ? C12D H12E 0.9600 . ? C12D H12F 0.9600 . ? C13D C14D 1.513(12) . ? C13D H13C 0.9700 . ? C13D H13D 0.9700 . ? C14D C15D 1.527(13) . ? C14D H14C 0.9700 . ? C14D H14D 0.9700 . ? C15D C16D 1.530(14) . ? C15D H15C 0.9700 . ? C15D H15D 0.9700 . ? C16D H16D 0.9600 . ? C16D H16E 0.9600 . ? C16D H16F 0.9600 . ? N1E C13E 1.508(11) . ? N1E C1E 1.520(12) . ? N1E C9E 1.551(12) . ? N1E C5E 1.551(14) . ? C1E C2E 1.501(12) . ? C1E H1E1 0.9700 . ? C1E H1E2 0.9700 . ? C2E C3E 1.540(14) . ? C2E H2E1 0.9700 . ? C2E H2E2 0.9700 . ? C3E C4E 1.506(12) . ? C3E H3E1 0.9700 . ? C3E H3E2 0.9700 . ? C4E H4E1 0.9600 . ? C4E H4E2 0.9600 . ? C4E H4E3 0.9600 . ? C5E C6E 1.523(13) . ? C5E H5E1 0.9700 . ? C5E H5E2 0.9700 . ? C6E C7E 1.556(14) . ? C6E H6E1 0.9700 . ? C6E H6E2 0.9700 . ? C7E C8E 1.523(16) . ? C7E H7E1 0.9700 . ? C7E H7E2 0.9700 . ? C8E H8E1 0.9600 . ? C8E H8E2 0.9600 . ? C8E H8E3 0.9600 . ? C9E C10E 1.535(16) . ? C9E H9E1 0.9700 . ? C9E H9E2 0.9700 . ? C10E C11E 1.550(13) . ? C10E H10E 0.9700 . ? C10E H10F 0.9700 . ? C11E C12E 1.545(18) . ? C11E H11E 0.9700 . ? C11E H11F 0.9700 . ? C12E H12G 0.9600 . ? C12E H12H 0.9600 . ? C12E H12I 0.9600 . ? C13E C14E 1.524(13) . ? C13E H13E 0.9700 . ? C13E H13F 0.9700 . ? C14E C15E 1.520(13) . ? C14E H14E 0.9700 . ? C14E H14F 0.9700 . ? C15E C16E 1.532(16) . ? C15E H15E 0.9700 . ? C15E H15F 0.9700 . ? C16E H16G 0.9600 . ? C16E H16H 0.9600 . ? C16E H16I 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 S2A Re1A S3A 89.72(8) . . ? S2A Re1A S4A 173.27(7) . . ? S3A Re1A S4A 89.50(8) . . ? S2A Re1A S1A 89.49(8) . . ? S3A Re1A S1A 173.14(7) . . ? S4A Re1A S1A 90.49(8) . . ? S2A Re1A Cl1A 93.71(8) . . ? S3A Re1A Cl1A 92.44(8) . . ? S4A Re1A Cl1A 93.00(7) . . ? S1A Re1A Cl1A 94.42(8) . . ? S2A Re1A Re3A 57.35(6) . 2_566 ? S3A Re1A Re3A 57.78(5) . 2_566 ? S4A Re1A Re3A 116.90(6) . 2_566 ? S1A Re1A Re3A 116.38(5) . 2_566 ? Cl1A Re1A Re3A 135.18(5) . 2_566 ? S2A Re1A Re3A 117.16(5) . . ? S3A Re1A Re3A 117.38(6) . . ? S4A Re1A Re3A 57.60(5) . . ? S1A Re1A Re3A 57.25(6) . . ? Cl1A Re1A Re3A 135.39(5) . . ? Re3A Re1A Re3A 89.43(2) 2_566 . ? S2A Re1A Re2A 117.37(6) . 2_566 ? S3A Re1A Re2A 57.76(6) . 2_566 ? S4A Re1A Re2A 56.88(5) . 2_566 ? S1A Re1A Re2A 116.87(6) . 2_566 ? Cl1A Re1A Re2A 134.34(7) . 2_566 ? Re3A Re1A Re2A 60.04(3) 2_566 2_566 ? Re3A Re1A Re2A 59.66(3) . 2_566 ? S2A Re1A Re2A 57.44(5) . . ? S3A Re1A Re2A 117.56(6) . . ? S4A Re1A Re2A 117.32(5) . . ? S1A Re1A Re2A 56.62(6) . . ? Cl1A Re1A Re2A 135.71(6) . . ? Re3A Re1A Re2A 59.80(3) 2_566 . ? Re3A Re1A Re2A 59.77(2) . . ? Re2A Re1A Re2A 89.94(4) 2_566 . ? S1A Re2A S4A 173.50(8) . 2_566 ? S1A Re2A S2A 89.61(7) . . ? S4A Re2A S2A 90.42(7) 2_566 . ? S1A Re2A Cl2A 93.12(8) . . ? S4A Re2A Cl2A 93.37(8) 2_566 . ? S2A Re2A Cl2A 92.68(8) . . ? S1A Re2A S3A 90.04(7) . 2_566 ? S4A Re2A S3A 89.11(7) 2_566 2_566 ? S2A Re2A S3A 172.74(8) . 2_566 ? Cl2A Re2A S3A 94.58(8) . 2_566 ? S1A Re2A Re3A 117.08(6) . 2_566 ? S4A Re2A Re3A 57.89(5) 2_566 2_566 ? S2A Re2A Re3A 57.11(6) . 2_566 ? Cl2A Re2A Re3A 134.59(6) . 2_566 ? S3A Re2A Re3A 116.91(6) 2_566 2_566 ? S1A Re2A Re3A 57.59(6) . . ? S4A Re2A Re3A 116.85(6) 2_566 . ? S2A Re2A Re3A 116.74(6) . . ? Cl2A Re2A Re3A 135.91(5) . . ? S3A Re2A Re3A 57.35(5) 2_566 . ? Re3A Re2A Re3A 89.49(4) 2_566 . ? S1A Re2A Re1A 117.22(6) . 2_566 ? S4A Re2A Re1A 57.24(6) 2_566 2_566 ? S2A Re2A Re1A 117.23(6) . 2_566 ? Cl2A Re2A Re1A 135.77(6) . 2_566 ? S3A Re2A Re1A 56.80(6) 2_566 2_566 ? Re3A Re2A Re1A 60.16(3) 2_566 2_566 ? Re3A Re2A Re1A 59.65(2) . 2_566 ? S1A Re2A Re1A 57.45(6) . . ? S4A Re2A Re1A 117.51(6) 2_566 . ? S2A Re2A Re1A 56.79(5) . . ? Cl2A Re2A Re1A 134.17(6) . . ? S3A Re2A Re1A 117.31(6) 2_566 . ? Re3A Re2A Re1A 59.67(3) 2_566 . ? Re3A Re2A Re1A 60.00(3) . . ? Re1A Re2A Re1A 90.06(4) 2_566 . ? Cl3A Re3A S2A 92.26(8) . 2_566 ? Cl3A Re3A S1A 94.21(8) . . ? S2A Re3A S1A 173.51(7) 2_566 . ? Cl3A Re3A S3A 93.75(7) . 2_566 ? S2A Re3A S3A 89.26(8) 2_566 2_566 ? S1A Re3A S3A 89.74(8) . 2_566 ? Cl3A Re3A S4A 92.81(7) . . ? S2A Re3A S4A 90.15(8) 2_566 . ? S1A Re3A S4A 90.11(8) . . ? S3A Re3A S4A 173.43(6) 2_566 . ? Cl3A Re3A Re1A 134.65(5) . 2_566 ? S2A Re3A Re1A 57.28(5) 2_566 2_566 ? S1A Re3A Re1A 117.09(6) . 2_566 ? S3A Re3A Re1A 57.13(6) 2_566 2_566 ? S4A Re3A Re1A 117.37(6) . 2_566 ? Cl3A Re3A Re2A 133.66(6) . 2_566 ? S2A Re3A Re2A 57.69(6) 2_566 2_566 ? S1A Re3A Re2A 117.44(6) . 2_566 ? S3A Re3A Re2A 117.63(6) 2_566 2_566 ? S4A Re3A Re2A 56.89(6) . 2_566 ? Re1A Re3A Re2A 60.53(2) 2_566 2_566 ? Cl3A Re3A Re2A 135.83(7) . . ? S2A Re3A Re2A 117.55(5) 2_566 . ? S1A Re3A Re2A 56.81(5) . . ? S3A Re3A Re2A 57.66(6) 2_566 . ? S4A Re3A Re2A 117.15(6) . . ? Re1A Re3A Re2A 60.30(3) 2_566 . ? Re2A Re3A Re2A 90.51(4) 2_566 . ? Cl3A Re3A Re1A 134.76(5) . . ? S2A Re3A Re1A 117.83(5) 2_566 . ? S1A Re3A Re1A 57.31(5) . . ? S3A Re3A Re1A 117.85(6) 2_566 . ? S4A Re3A Re1A 56.95(5) . . ? Re1A Re3A Re1A 90.57(2) 2_566 . ? Re2A Re3A Re1A 60.18(3) 2_566 . ? Re2A Re3A Re1A 60.23(2) . . ? Re2A S1A Re3A 65.61(6) . . ? Re2A S1A Re1A 65.93(5) . . ? Re3A S1A Re1A 65.43(6) . . ? Re1A S2A Re3A 65.37(6) . 2_566 ? Re1A S2A Re2A 65.77(6) . . ? Re3A S2A Re2A 65.20(6) 2_566 . ? Re1A S3A Re3A 65.09(6) . 2_566 ? Re1A S3A Re2A 65.44(5) . 2_566 ? Re3A S3A Re2A 64.99(5) 2_566 2_566 ? Re2A S4A Re1A 65.88(6) 2_566 . ? Re2A S4A Re3A 65.23(6) 2_566 . ? Re1A S4A Re3A 65.45(6) . . ? S3B Re1B S4B 89.28(8) . . ? S3B Re1B S1B 90.30(8) . . ? S4B Re1B S1B 173.25(7) . . ? S3B Re1B S2B 173.37(7) . . ? S4B Re1B S2B 89.79(8) . . ? S1B Re1B S2B 89.84(8) . . ? S3B Re1B Cl1B 93.45(8) . . ? S4B Re1B Cl1B 94.73(8) . . ? S1B Re1B Cl1B 92.02(8) . . ? S2B Re1B Cl1B 93.17(8) . . ? S3B Re1B Re2B 57.05(5) . . ? S4B Re1B Re2B 57.54(6) . . ? S1B Re1B Re2B 116.93(6) . . ? S2B Re1B Re2B 117.22(6) . . ? Cl1B Re1B Re2B 136.32(7) . . ? S3B Re1B Re3B 117.17(6) . . ? S4B Re1B Re3B 57.67(6) . . ? S1B Re1B Re3B 116.85(6) . . ? S2B Re1B Re3B 57.11(5) . . ? Cl1B Re1B Re3B 136.02(5) . . ? Re2B Re1B Re3B 60.15(3) . . ? S3B Re1B Re2B 117.59(6) . 2 ? S4B Re1B Re2B 117.59(6) . 2 ? S1B Re1B Re2B 56.93(6) . 2 ? S2B Re1B Re2B 57.35(5) . 2 ? Cl1B Re1B Re2B 133.63(6) . 2 ? Re2B Re1B Re2B 90.03(4) . 2 ? Re3B Re1B Re2B 59.96(2) . 2 ? S3B Re1B Re3B 57.60(5) . 2 ? S4B Re1B Re3B 117.46(6) . 2 ? S1B Re1B Re3B 57.03(6) . 2 ? S2B Re1B Re3B 117.34(5) . 2 ? Cl1B Re1B Re3B 133.89(5) . 2 ? Re2B Re1B Re3B 59.95(2) . 2 ? Re3B Re1B Re3B 90.05(3) . 2 ? Re2B Re1B Re3B 60.04(3) 2 2 ? S1B Re2B S3B 173.55(8) 2 . ? S1B Re2B S2B 90.12(7) 2 2 ? S3B Re2B S2B 90.05(7) . 2 ? S1B Re2B Cl2B 91.57(8) 2 . ? S3B Re2B Cl2B 94.86(8) . . ? S2B Re2B Cl2B 92.47(8) 2 . ? S1B Re2B S4B 89.81(7) 2 . ? S3B Re2B S4B 89.28(7) . . ? S2B Re2B S4B 173.33(8) 2 . ? Cl2B Re2B S4B 94.20(8) . . ? S1B Re2B Re1B 117.05(6) 2 . ? S3B Re2B Re1B 57.38(6) . . ? S2B Re2B Re1B 117.17(5) 2 . ? Cl2B Re2B Re1B 136.96(6) . . ? S4B Re2B Re1B 57.20(5) . . ? S1B Re2B Re3B 117.31(6) 2 2 ? S3B Re2B Re3B 57.77(6) . 2 ? S2B Re2B Re3B 57.09(5) 2 2 ? Cl2B Re2B Re3B 135.53(6) . 2 ? S4B Re2B Re3B 117.29(6) . 2 ? Re1B Re2B Re3B 60.12(3) . 2 ? S1B Re2B Re1B 57.40(5) 2 2 ? S3B Re2B Re1B 117.67(5) . 2 ? S2B Re2B Re1B 57.30(6) 2 2 ? Cl2B Re2B Re1B 133.06(6) . 2 ? S4B Re2B Re1B 117.45(6) . 2 ? Re1B Re2B Re1B 89.97(4) . 2 ? Re3B Re2B Re1B 59.95(3) 2 2 ? S1B Re2B Re3B 57.15(6) 2 . ? S3B Re2B Re3B 117.29(6) . . ? S2B Re2B Re3B 117.25(6) 2 . ? Cl2B Re2B Re3B 134.37(6) . . ? S4B Re2B Re3B 57.49(6) . . ? Re1B Re2B Re3B 59.93(3) . . ? Re3B Re2B Re3B 90.03(4) 2 . ? Re1B Re2B Re3B 60.00(3) 2 . ? S1B Re3B S2B 173.30(6) 2 . ? S1B Re3B Cl3B 92.83(7) 2 . ? S2B Re3B Cl3B 93.86(8) . . ? S1B Re3B S3B 90.15(8) 2 2 ? S2B Re3B S3B 89.74(8) . 2 ? Cl3B Re3B S3B 93.73(8) . 2 ? S1B Re3B S4B 89.58(8) 2 . ? S2B Re3B S4B 89.69(8) . . ? Cl3B Re3B S4B 93.41(8) . . ? S3B Re3B S4B 172.86(7) 2 . ? S1B Re3B Re1B 116.88(6) 2 . ? S2B Re3B Re1B 57.47(6) . . ? Cl3B Re3B Re1B 135.50(6) . . ? S3B Re3B Re1B 116.92(5) 2 . ? S4B Re3B Re1B 57.14(5) . . ? S1B Re3B Re2B 117.23(5) 2 2 ? S2B Re3B Re2B 57.50(5) . 2 ? Cl3B Re3B Re2B 135.48(6) . 2 ? S3B Re3B Re2B 56.88(5) 2 2 ? S4B Re3B Re2B 117.20(6) . 2 ? Re1B Re3B Re2B 60.09(3) . 2 ? S1B Re3B Re1B 57.34(5) 2 2 ? S2B Re3B Re1B 117.40(5) . 2 ? Cl3B Re3B Re1B 134.55(5) . 2 ? S3B Re3B Re1B 57.06(6) 2 2 ? S4B Re3B Re1B 117.22(6) . 2 ? Re1B Re3B Re1B 89.95(3) . 2 ? Re2B Re3B Re1B 59.93(3) 2 2 ? S1B Re3B Re2B 56.99(5) 2 . ? S2B Re3B Re2B 117.36(6) . . ? Cl3B Re3B Re2B 134.54(6) . . ? S3B Re3B Re2B 116.97(6) 2 . ? S4B Re3B Re2B 57.30(6) . . ? Re1B Re3B Re2B 59.92(3) . . ? Re2B Re3B Re2B 89.97(4) 2 . ? Re1B Re3B Re2B 59.96(2) 2 . ? Re2B S1B Re3B 65.86(6) 2 2 ? Re2B S1B Re1B 65.67(6) 2 . ? Re3B S1B Re1B 65.63(6) 2 . ? Re3B S2B Re1B 65.42(6) . . ? Re3B S2B Re2B 65.41(6) . 2 ? Re1B S2B Re2B 65.36(6) . 2 ? Re2B S3B Re1B 65.57(6) . . ? Re2B S3B Re3B 65.35(5) . 2 ? Re1B S3B Re3B 65.34(6) . 2 ? Re1B S4B Re2B 65.26(5) . . ? Re1B S4B Re3B 65.19(6) . . ? Re2B S4B Re3B 65.21(6) . . ? C1C N1C C13C 111.9(7) . . ? C1C N1C C5C 111.6(6) . . ? C13C N1C C5C 106.5(6) . . ? C1C N1C C9C 106.3(6) . . ? C13C N1C C9C 111.0(6) . . ? C5C N1C C9C 109.8(7) . . ? N1C C1C C2C 114.7(7) . . ? N1C C1C H1C1 108.6 . . ? C2C C1C H1C1 108.6 . . ? N1C C1C H1C2 108.6 . . ? C2C C1C H1C2 108.6 . . ? H1C1 C1C H1C2 107.6 . . ? C3C C2C C1C 111.1(7) . . ? C3C C2C H2C1 109.4 . . ? C1C C2C H2C1 109.4 . . ? C3C C2C H2C2 109.4 . . ? C1C C2C H2C2 109.4 . . ? H2C1 C2C H2C2 108.0 . . ? C4C C3C C2C 112.5(9) . . ? C4C C3C H3C1 109.1 . . ? C2C C3C H3C1 109.1 . . ? C4C C3C H3C2 109.1 . . ? C2C C3C H3C2 109.1 . . ? H3C1 C3C H3C2 107.8 . . ? C3C C4C H4C1 109.5 . . ? C3C C4C H4C2 109.5 . . ? H4C1 C4C H4C2 109.5 . . ? C3C C4C H4C3 109.5 . . ? H4C1 C4C H4C3 109.5 . . ? H4C2 C4C H4C3 109.5 . . ? C6C C5C N1C 115.1(7) . . ? C6C C5C H5C1 108.5 . . ? N1C C5C H5C1 108.5 . . ? C6C C5C H5C2 108.5 . . ? N1C C5C H5C2 108.5 . . ? H5C1 C5C H5C2 107.5 . . ? C7C C6C C5C 112.2(8) . . ? C7C C6C H6C1 109.2 . . ? C5C C6C H6C1 109.2 . . ? C7C C6C H6C2 109.2 . . ? C5C C6C H6C2 109.2 . . ? H6C1 C6C H6C2 107.9 . . ? C6C C7C C8C 111.7(9) . . ? C6C C7C H7C1 109.3 . . ? C8C C7C H7C1 109.3 . . ? C6C C7C H7C2 109.3 . . ? C8C C7C H7C2 109.3 . . ? H7C1 C7C H7C2 107.9 . . ? C7C C8C H8C1 109.5 . . ? C7C C8C H8C2 109.5 . . ? H8C1 C8C H8C2 109.5 . . ? C7C C8C H8C3 109.5 . . ? H8C1 C8C H8C3 109.5 . . ? H8C2 C8C H8C3 109.5 . . ? C10C C9C N1C 116.4(6) . . ? C10C C9C H9C1 108.2 . . ? N1C C9C H9C1 108.2 . . ? C10C C9C H9C2 108.2 . . ? N1C C9C H9C2 108.2 . . ? H9C1 C9C H9C2 107.3 . . ? C9C C10C C11C 109.3(7) . . ? C9C C10C H10A 109.8 . . ? C11C C10C H10A 109.8 . . ? C9C C10C H10B 109.8 . . ? C11C C10C H10B 109.8 . . ? H10A C10C H10B 108.3 . . ? C12C C11C C10C 112.5(8) . . ? C12C C11C H11A 109.1 . . ? C10C C11C H11A 109.1 . . ? C12C C11C H11B 109.1 . . ? C10C C11C H11B 109.1 . . ? H11A C11C H11B 107.8 . . ? C11C C12C H12A 109.5 . . ? C11C C12C H12B 109.5 . . ? H12A C12C H12B 109.5 . . ? C11C C12C H12C 109.5 . . ? H12A C12C H12C 109.5 . . ? H12B C12C H12C 109.5 . . ? C14C C13C N1C 114.6(6) . . ? C14C C13C H13A 108.6 . . ? N1C C13C H13A 108.6 . . ? C14C C13C H13B 108.6 . . ? N1C C13C H13B 108.6 . . ? H13A C13C H13B 107.6 . . ? C13C C14C C15C 110.3(7) . . ? C13C C14C H14A 109.6 . . ? C15C C14C H14A 109.6 . . ? C13C C14C H14B 109.6 . . ? C15C C14C H14B 109.6 . . ? H14A C14C H14B 108.1 . . ? C16C C15C C14C 111.6(8) . . ? C16C C15C H15A 109.3 . . ? C14C C15C H15A 109.3 . . ? C16C C15C H15B 109.3 . . ? C14C C15C H15B 109.3 . . ? H15A C15C H15B 108.0 . . ? C15C C16C H16A 109.5 . . ? C15C C16C H16B 109.5 . . ? H16A C16C H16B 109.5 . . ? C15C C16C H16C 109.5 . . ? H16A C16C H16C 109.5 . . ? H16B C16C H16C 109.5 . . ? C1D N1D C9D 111.3(7) . . ? C1D N1D C13D 111.1(6) . . ? C9D N1D C13D 106.6(6) . . ? C1D N1D C5D 106.5(6) . . ? C9D N1D C5D 111.0(6) . . ? C13D N1D C5D 110.4(7) . . ? N1D C1D C2D 116.6(6) . . ? N1D C1D H1D1 108.1 . . ? C2D C1D H1D1 108.1 . . ? N1D C1D H1D2 108.1 . . ? C2D C1D H1D2 108.1 . . ? H1D1 C1D H1D2 107.3 . . ? C3D C2D C1D 110.8(7) . . ? C3D C2D H2D1 109.5 . . ? C1D C2D H2D1 109.5 . . ? C3D C2D H2D2 109.5 . . ? C1D C2D H2D2 109.5 . . ? H2D1 C2D H2D2 108.1 . . ? C2D C3D C4D 113.8(8) . . ? C2D C3D H3D1 108.8 . . ? C4D C3D H3D1 108.8 . . ? C2D C3D H3D2 108.8 . . ? C4D C3D H3D2 108.8 . . ? H3D1 C3D H3D2 107.7 . . ? C3D C4D H4D1 109.5 . . ? C3D C4D H4D2 109.5 . . ? H4D1 C4D H4D2 109.5 . . ? C3D C4D H4D3 109.5 . . ? H4D1 C4D H4D3 109.5 . . ? H4D2 C4D H4D3 109.5 . . ? C6D C5D N1D 115.6(7) . . ? C6D C5D H5D1 108.4 . . ? N1D C5D H5D1 108.4 . . ? C6D C5D H5D2 108.4 . . ? N1D C5D H5D2 108.4 . . ? H5D1 C5D H5D2 107.4 . . ? C5D C6D C7D 110.3(7) . . ? C5D C6D H6D1 109.6 . . ? C7D C6D H6D1 109.6 . . ? C5D C6D H6D2 109.6 . . ? C7D C6D H6D2 109.6 . . ? H6D1 C6D H6D2 108.1 . . ? C8D C7D C6D 111.9(9) . . ? C8D C7D H7D1 109.2 . . ? C6D C7D H7D1 109.2 . . ? C8D C7D H7D2 109.2 . . ? C6D C7D H7D2 109.2 . . ? H7D1 C7D H7D2 107.9 . . ? C7D C8D H8D1 109.5 . . ? C7D C8D H8D2 109.5 . . ? H8D1 C8D H8D2 109.5 . . ? C7D C8D H8D3 109.5 . . ? H8D1 C8D H8D3 109.5 . . ? H8D2 C8D H8D3 109.5 . . ? N1D C9D C10D 114.9(7) . . ? N1D C9D H9D1 108.5 . . ? C10D C9D H9D1 108.5 . . ? N1D C9D H9D2 108.5 . . ? C10D C9D H9D2 108.5 . . ? H9D1 C9D H9D2 107.5 . . ? C11D C10D C9D 111.1(8) . . ? C11D C10D H10C 109.4 . . ? C9D C10D H10C 109.4 . . ? C11D C10D H10D 109.4 . . ? C9D C10D H10D 109.4 . . ? H10C C10D H10D 108.0 . . ? C10D C11D C12D 113.2(9) . . ? C10D C11D H11C 108.9 . . ? C12D C11D H11C 108.9 . . ? C10D C11D H11D 108.9 . . ? C12D C11D H11D 108.9 . . ? H11C C11D H11D 107.7 . . ? C11D C12D H12D 109.5 . . ? C11D C12D H12E 109.5 . . ? H12D C12D H12E 109.5 . . ? C11D C12D H12F 109.5 . . ? H12D C12D H12F 109.5 . . ? H12E C12D H12F 109.5 . . ? C14D C13D N1D 115.6(7) . . ? C14D C13D H13C 108.4 . . ? N1D C13D H13C 108.4 . . ? C14D C13D H13D 108.4 . . ? N1D C13D H13D 108.4 . . ? H13C C13D H13D 107.4 . . ? C13D C14D C15D 109.8(7) . . ? C13D C14D H14C 109.7 . . ? C15D C14D H14C 109.7 . . ? C13D C14D H14D 109.7 . . ? C15D C14D H14D 109.7 . . ? H14C C14D H14D 108.2 . . ? C14D C15D C16D 111.8(8) . . ? C14D C15D H15C 109.3 . . ? C16D C15D H15C 109.3 . . ? C14D C15D H15D 109.3 . . ? C16D C15D H15D 109.3 . . ? H15C C15D H15D 107.9 . . ? C15D C16D H16D 109.5 . . ? C15D C16D H16E 109.5 . . ? H16D C16D H16E 109.5 . . ? C15D C16D H16F 109.5 . . ? H16D C16D H16F 109.5 . . ? H16E C16D H16F 109.5 . . ? C13E N1E C1E 106.0(7) . . ? C13E N1E C9E 112.2(7) . . ? C1E N1E C9E 111.8(7) . . ? C13E N1E C5E 110.9(7) . . ? C1E N1E C5E 111.0(7) . . ? C9E N1E C5E 105.0(7) . . ? C2E C1E N1E 118.4(8) . . ? C2E C1E H1E1 107.7 . . ? N1E C1E H1E1 107.7 . . ? C2E C1E H1E2 107.7 . . ? N1E C1E H1E2 107.7 . . ? H1E1 C1E H1E2 107.1 . . ? C1E C2E C3E 107.9(9) . . ? C1E C2E H2E1 110.1 . . ? C3E C2E H2E1 110.1 . . ? C1E C2E H2E2 110.1 . . ? C3E C2E H2E2 110.1 . . ? H2E1 C2E H2E2 108.4 . . ? C4E C3E C2E 113.9(8) . . ? C4E C3E H3E1 108.8 . . ? C2E C3E H3E1 108.8 . . ? C4E C3E H3E2 108.8 . . ? C2E C3E H3E2 108.8 . . ? H3E1 C3E H3E2 107.7 . . ? C3E C4E H4E1 109.5 . . ? C3E C4E H4E2 109.5 . . ? H4E1 C4E H4E2 109.5 . . ? C3E C4E H4E3 109.5 . . ? H4E1 C4E H4E3 109.5 . . ? H4E2 C4E H4E3 109.5 . . ? C6E C5E N1E 114.4(8) . . ? C6E C5E H5E1 108.7 . . ? N1E C5E H5E1 108.7 . . ? C6E C5E H5E2 108.7 . . ? N1E C5E H5E2 108.7 . . ? H5E1 C5E H5E2 107.6 . . ? C5E C6E C7E 110.3(9) . . ? C5E C6E H6E1 109.6 . . ? C7E C6E H6E1 109.6 . . ? C5E C6E H6E2 109.6 . . ? C7E C6E H6E2 109.6 . . ? H6E1 C6E H6E2 108.1 . . ? C8E C7E C6E 110.4(9) . . ? C8E C7E H7E1 109.6 . . ? C6E C7E H7E1 109.6 . . ? C8E C7E H7E2 109.6 . . ? C6E C7E H7E2 109.6 . . ? H7E1 C7E H7E2 108.1 . . ? C7E C8E H8E1 109.5 . . ? C7E C8E H8E2 109.5 . . ? H8E1 C8E H8E2 109.5 . . ? C7E C8E H8E3 109.5 . . ? H8E1 C8E H8E3 109.5 . . ? H8E2 C8E H8E3 109.5 . . ? C10E C9E N1E 114.7(8) . . ? C10E C9E H9E1 108.6 . . ? N1E C9E H9E1 108.6 . . ? C10E C9E H9E2 108.6 . . ? N1E C9E H9E2 108.6 . . ? H9E1 C9E H9E2 107.6 . . ? C9E C10E C11E 109.2(9) . . ? C9E C10E H10E 109.8 . . ? C11E C10E H10E 109.8 . . ? C9E C10E H10F 109.8 . . ? C11E C10E H10F 109.8 . . ? H10E C10E H10F 108.3 . . ? C12E C11E C10E 110.5(10) . . ? C12E C11E H11E 109.6 . . ? C10E C11E H11E 109.6 . . ? C12E C11E H11F 109.6 . . ? C10E C11E H11F 109.6 . . ? H11E C11E H11F 108.1 . . ? C11E C12E H12G 109.5 . . ? C11E C12E H12H 109.5 . . ? H12G C12E H12H 109.5 . . ? C11E C12E H12I 109.5 . . ? H12G C12E H12I 109.5 . . ? H12H C12E H12I 109.5 . . ? N1E C13E C14E 117.5(8) . . ? N1E C13E H13E 107.9 . . ? C14E C13E H13E 107.9 . . ? N1E C13E H13F 107.9 . . ? C14E C13E H13F 107.9 . . ? H13E C13E H13F 107.2 . . ? C13E C14E C15E 110.0(9) . . ? C13E C14E H14E 109.7 . . ? C15E C14E H14E 109.7 . . ? C13E C14E H14F 109.7 . . ? C15E C14E H14F 109.7 . . ? H14E C14E H14F 108.2 . . ? C14E C15E C16E 114.2(9) . . ? C14E C15E H15E 108.7 . . ? C16E C15E H15E 108.7 . . ? C14E C15E H15F 108.7 . . ? C16E C15E H15F 108.7 . . ? H15E C15E H15F 107.6 . . ? C15E C16E H16G 109.5 . . ? C15E C16E H16H 109.5 . . ? H16G C16E H16H 109.5 . . ? C15E C16E H16I 109.5 . . ? H16G C16E H16I 109.5 . . ? H16H C16E H16I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.82 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.312 _refine_diff_density_min -3.743 _refine_diff_density_rms 0.342 #################### Material relevant to compound 1 at 100K ############ data_rad100o _database_code_CSD 186992 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(tetrabutylammonium) octa-\m-eq-3-sulfido-hexachloro-octahedro- rhenate(IV)pentarhenate(III)' ; _chemical_name_common '(TBA)3 (Re6S8Cl6)' _chemical_formula_moiety '3(C16 H36 N), (Cl6 Re6 S8)' _chemical_formula_sum 'C48 H108 Cl6 N3 Re6 S8' _chemical_formula_weight 2313.75 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3773(12) _cell_length_b 17.1805(18) _cell_length_c 18.1666(18) _cell_angle_alpha 96.632(12) _cell_angle_beta 106.425(11) _cell_angle_gamma 103.608(12) _cell_volume 3532.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2194 _exptl_absorpt_coefficient_mu 10.736 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0257 _exptl_absorpt_correction_T_max 0.2574 _exptl_absorpt_process_details 'FACEIT (Stoe IPDS)' _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_radiation_detector 'area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'Rotation, \D\f==1.3%' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13710 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.91 _reflns_number_total 13710 _reflns_number_gt 11105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS)' _computing_cell_refinement 'SELECT (Stoe IPDS)' _computing_data_reduction 'INTEGRATE (Stoe IPDS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0351P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12790 _refine_ls_number_parameters 652 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1A Re 0.144627(16) 0.073452(13) 0.053206(12) 0.01244(5) Uani 1 1 d . . . Re2A Re 0.059099(16) -0.084501(13) 0.029694(13) 0.01236(5) Uani 1 1 d . . . Re3A Re -0.042833(16) 0.010467(13) 0.087998(12) 0.01223(5) Uani 1 1 d . . . S1A S 0.14937(11) 0.00054(9) 0.15823(8) 0.0166(3) Uani 1 1 d . . . S2A S 0.22718(11) -0.02040(9) -0.00540(8) 0.0162(3) Uani 1 1 d . . . S3A S 0.03784(11) 0.15543(8) 0.10278(8) 0.0153(3) Uani 1 1 d . . . S4A S 0.11907(11) 0.13655(8) -0.05907(8) 0.0151(3) Uani 1 1 d . . . Cl2A Cl 0.13454(11) -0.19705(8) 0.06842(8) 0.0193(3) Uani 1 1 d . . . Cl1A Cl 0.33622(10) 0.16828(9) 0.12247(8) 0.0197(3) Uani 1 1 d . . . Cl3A Cl -0.10211(11) 0.02241(8) 0.20277(8) 0.0191(3) Uani 1 1 d . . . Re1B Re 0.124229(16) -0.439657(13) -0.414414(12) 0.01147(5) Uani 1 1 d . . . Re2B Re -0.061565(16) -0.413338(13) -0.505475(12) 0.01146(5) Uani 1 1 d . . . Re3B Re 0.082919(16) -0.463482(13) -0.565181(12) 0.01148(5) Uani 1 1 d . . . S1B S 0.09525(10) -0.55694(9) -0.35556(8) 0.0149(3) Uani 1 1 d . . . S2B S 0.24853(10) -0.49053(8) -0.47644(8) 0.0147(3) Uani 1 1 d . . . S3B S -0.01843(10) -0.39705(8) -0.36550(8) 0.0152(3) Uani 1 1 d . . . S4B S 0.13441(10) -0.33032(8) -0.48524(8) 0.0152(3) Uani 1 1 d . . . Cl2B Cl -0.14474(11) -0.30006(8) -0.51700(9) 0.0193(3) Uani 1 1 d . . . Cl1B Cl 0.28909(10) -0.36509(8) -0.30090(8) 0.0183(3) Uani 1 1 d . . . Cl3B Cl 0.18981(10) -0.41483(9) -0.65163(8) 0.0202(3) Uani 1 1 d . . . N1C N 0.0337(4) 0.8107(3) 0.3088(3) 0.0163(10) Uani 1 1 d . . . C1C C 0.1352(4) 0.8593(4) 0.2862(3) 0.0168(11) Uani 1 1 d . . . H1C1 H 0.1102 0.8546 0.2299 0.020 Uiso 1 1 calc R . . H1C2 H 0.1531 0.9164 0.3096 0.020 Uiso 1 1 calc R . . C2C C 0.2458(5) 0.8328(4) 0.3109(4) 0.0281(15) Uani 1 1 d . . . H2C1 H 0.2310 0.7773 0.2840 0.034 Uiso 1 1 calc R . . H2C2 H 0.2690 0.8337 0.3667 0.034 Uiso 1 1 calc R . . C3C C 0.3459(5) 0.8898(4) 0.2915(4) 0.0250(13) Uani 1 1 d . . . H3C1 H 0.4106 0.8656 0.2981 0.030 Uiso 1 1 calc R . . H3C2 H 0.3183 0.8942 0.2370 0.030 Uiso 1 1 calc R . . C4C C 0.3906(5) 0.9746(5) 0.3420(5) 0.0376(17) Uani 1 1 d . . . H4C1 H 0.3306 1.0022 0.3298 0.056 Uiso 1 1 calc R . . H4C2 H 0.4590 1.0049 0.3320 0.056 Uiso 1 1 calc R . . H4C3 H 0.4104 0.9705 0.3961 0.056 Uiso 1 1 calc R . . C5C C -0.0010(5) 0.7208(3) 0.2712(3) 0.0180(12) Uani 1 1 d . . . H5C1 H 0.0679 0.7012 0.2861 0.022 Uiso 1 1 calc R . . H5C2 H -0.0579 0.6908 0.2925 0.022 Uiso 1 1 calc R . . C6C C -0.0524(5) 0.7012(4) 0.1829(4) 0.0224(12) Uani 1 1 d . . . H6C1 H -0.0022 0.7366 0.1607 0.027 Uiso 1 1 calc R . . H6C2 H -0.1291 0.7108 0.1672 0.027 Uiso 1 1 calc R . . C7C C -0.0638(5) 0.6122(4) 0.1522(4) 0.0274(14) Uani 1 1 d . . . H7C1 H 0.0136 0.6037 0.1663 0.033 Uiso 1 1 calc R . . H7C2 H -0.1103 0.5774 0.1771 0.033 Uiso 1 1 calc R . . C8C C -0.1201(7) 0.5881(5) 0.0649(5) 0.0450(19) Uani 1 1 d . . . H8C1 H -0.1998 0.5908 0.0511 0.067 Uiso 1 1 calc R . . H8C2 H -0.1192 0.5334 0.0476 0.067 Uiso 1 1 calc R . . H8C3 H -0.0774 0.6248 0.0401 0.067 Uiso 1 1 calc R . . C9C C 0.0666(5) 0.8152(4) 0.3959(3) 0.0179(12) Uani 1 1 d . . . H9C1 H -0.0018 0.7852 0.4073 0.022 Uiso 1 1 calc R . . H9C2 H 0.1266 0.7873 0.4111 0.022 Uiso 1 1 calc R . . C10C C 0.1110(5) 0.8995(4) 0.4469(4) 0.0210(12) Uani 1 1 d . . . H10A H 0.0591 0.9320 0.4268 0.025 Uiso 1 1 calc R . . H10B H 0.1885 0.9262 0.4456 0.025 Uiso 1 1 calc R . . C11C C 0.1166(5) 0.8942(4) 0.5311(4) 0.0247(13) Uani 1 1 d . . . H11A H 0.0385 0.8679 0.5317 0.030 Uiso 1 1 calc R . . H11B H 0.1666 0.8600 0.5499 0.030 Uiso 1 1 calc R . . C12C C 0.1624(7) 0.9753(5) 0.5859(4) 0.0388(17) Uani 1 1 d . . . H12A H 0.2440 0.9979 0.5923 0.058 Uiso 1 1 calc R . . H12B H 0.1535 0.9684 0.6357 0.058 Uiso 1 1 calc R . . H12C H 0.1191 1.0117 0.5647 0.058 Uiso 1 1 calc R . . C13C C -0.0671(4) 0.8471(4) 0.2797(3) 0.0180(12) Uani 1 1 d . . . H13A H -0.0873 0.8413 0.2233 0.022 Uiso 1 1 calc R . . H13B H -0.0406 0.9051 0.3019 0.022 Uiso 1 1 calc R . . C14C C -0.1775(4) 0.8093(4) 0.2990(4) 0.0196(12) Uani 1 1 d . . . H14A H -0.1642 0.8257 0.3545 0.024 Uiso 1 1 calc R . . H14B H -0.1964 0.7502 0.2867 0.024 Uiso 1 1 calc R . . C15C C -0.2799(4) 0.8374(4) 0.2516(4) 0.0205(12) Uani 1 1 d . . . H15A H -0.2981 0.8158 0.1964 0.025 Uiso 1 1 calc R . . H15B H -0.2567 0.8966 0.2593 0.025 Uiso 1 1 calc R . . C16C C -0.3894(5) 0.8094(4) 0.2753(4) 0.0317(15) Uani 1 1 d . . . H16A H -0.4126 0.7509 0.2679 0.048 Uiso 1 1 calc R . . H16B H -0.4518 0.8271 0.2436 0.048 Uiso 1 1 calc R . . H16C H -0.3727 0.8325 0.3294 0.048 Uiso 1 1 calc R . . N1D N 0.3298(4) 0.3279(3) 0.3223(3) 0.0151(9) Uani 1 1 d . . . C1D C 0.2730(4) 0.3290(3) 0.2369(3) 0.0169(11) Uani 1 1 d . . . H1D1 H 0.2495 0.2737 0.2071 0.020 Uiso 1 1 calc R . . H1D2 H 0.3313 0.3618 0.2184 0.020 Uiso 1 1 calc R . . C2D C 0.1670(4) 0.3618(4) 0.2199(3) 0.0179(12) Uani 1 1 d . . . H2D1 H 0.1824 0.4100 0.2590 0.021 Uiso 1 1 calc R . . H2D2 H 0.0999 0.3211 0.2226 0.021 Uiso 1 1 calc R . . C3D C 0.1392(5) 0.3836(4) 0.1387(4) 0.0233(13) Uani 1 1 d . . . H3D1 H 0.2067 0.4241 0.1360 0.028 Uiso 1 1 calc R . . H3D2 H 0.1240 0.3353 0.0996 0.028 Uiso 1 1 calc R . . C4D C 0.0335(6) 0.4169(5) 0.1205(5) 0.0398(18) Uani 1 1 d . . . H4D1 H -0.0345 0.3755 0.1195 0.060 Uiso 1 1 calc R . . H4D2 H 0.0207 0.4326 0.0704 0.060 Uiso 1 1 calc R . . H4D3 H 0.0474 0.4636 0.1600 0.060 Uiso 1 1 calc R . . C5D C 0.2434(4) 0.2751(4) 0.3540(4) 0.0188(12) Uani 1 1 d . . . H5D1 H 0.1743 0.2947 0.3449 0.023 Uiso 1 1 calc R . . H5D2 H 0.2789 0.2824 0.4102 0.023 Uiso 1 1 calc R . . C6D C 0.2043(5) 0.1837(4) 0.3191(4) 0.0212(12) Uani 1 1 d . . . H6D1 H 0.2720 0.1659 0.3161 0.025 Uiso 1 1 calc R . . H6D2 H 0.1502 0.1738 0.2663 0.025 Uiso 1 1 calc R . . C7D C 0.1446(5) 0.1344(4) 0.3687(4) 0.0269(14) Uani 1 1 d . . . H7D1 H 0.0859 0.1589 0.3790 0.032 Uiso 1 1 calc R . . H7D2 H 0.1043 0.0794 0.3390 0.032 Uiso 1 1 calc R . . C8D C 0.2290(6) 0.1298(4) 0.4464(4) 0.0288(14) Uani 1 1 d . . . H8D1 H 0.2853 0.1033 0.4368 0.043 Uiso 1 1 calc R . . H8D2 H 0.1858 0.0991 0.4750 0.043 Uiso 1 1 calc R . . H8D3 H 0.2690 0.1839 0.4764 0.043 Uiso 1 1 calc R . . C9D C 0.3701(5) 0.4132(4) 0.3729(3) 0.0193(12) Uani 1 1 d . . . H9D1 H 0.4205 0.4115 0.4240 0.023 Uiso 1 1 calc R . . H9D2 H 0.3016 0.4269 0.3801 0.023 Uiso 1 1 calc R . . C10D C 0.4356(5) 0.4816(4) 0.3417(4) 0.0206(12) Uani 1 1 d . . . H10C H 0.4995 0.4666 0.3284 0.025 Uiso 1 1 calc R . . H10D H 0.3828 0.4907 0.2948 0.025 Uiso 1 1 calc R . . C11D C 0.4837(5) 0.5591(4) 0.4043(3) 0.0196(12) Uani 1 1 d . . . H11C H 0.4218 0.5678 0.4244 0.024 Uiso 1 1 calc R . . H11D H 0.5460 0.5524 0.4474 0.024 Uiso 1 1 calc R . . C12D C 0.5310(5) 0.6333(4) 0.3730(4) 0.0300(14) Uani 1 1 d . . . H12D H 0.5907 0.6243 0.3517 0.045 Uiso 1 1 calc R . . H12E H 0.5639 0.6803 0.4148 0.045 Uiso 1 1 calc R . . H12F H 0.4684 0.6424 0.3328 0.045 Uiso 1 1 calc R . . C13D C 0.4351(4) 0.2946(4) 0.3268(3) 0.0179(12) Uani 1 1 d . . . H13C H 0.4918 0.3329 0.3113 0.022 Uiso 1 1 calc R . . H13D H 0.4090 0.2436 0.2894 0.022 Uiso 1 1 calc R . . C14D C 0.4963(5) 0.2798(4) 0.4071(4) 0.0217(13) Uani 1 1 d . . . H14C H 0.4395 0.2655 0.4343 0.026 Uiso 1 1 calc R . . H14D H 0.5555 0.3295 0.4377 0.026 Uiso 1 1 calc R . . C15D C 0.5544(5) 0.2109(4) 0.4001(4) 0.0259(14) Uani 1 1 d . . . H15C H 0.4980 0.1637 0.3629 0.031 Uiso 1 1 calc R . . H15D H 0.6195 0.2286 0.3804 0.031 Uiso 1 1 calc R . . C16D C 0.5992(6) 0.1867(5) 0.4786(4) 0.0387(18) Uani 1 1 d . . . H16D H 0.6549 0.2333 0.5156 0.058 Uiso 1 1 calc R . . H16E H 0.6364 0.1443 0.4726 0.058 Uiso 1 1 calc R . . H16F H 0.5345 0.1672 0.4973 0.058 Uiso 1 1 calc R . . N1E N 0.6207(4) 0.2786(3) 0.0336(3) 0.0206(11) Uani 1 1 d . . . C1E C 0.7220(5) 0.2615(4) 0.0926(4) 0.0221(13) Uani 1 1 d . . . H1E1 H 0.7750 0.3135 0.1232 0.027 Uiso 1 1 calc R . . H1E2 H 0.7645 0.2367 0.0638 0.027 Uiso 1 1 calc R . . C2E C 0.6952(5) 0.2078(4) 0.1490(4) 0.0207(12) Uani 1 1 d . . . H2E1 H 0.6571 0.1518 0.1214 0.025 Uiso 1 1 calc R . . H2E2 H 0.6428 0.2262 0.1733 0.025 Uiso 1 1 calc R . . C3E C 0.8106(5) 0.2128(4) 0.2115(4) 0.0230(13) Uani 1 1 d . . . H3E1 H 0.8566 0.1866 0.1871 0.028 Uiso 1 1 calc R . . H3E2 H 0.8545 0.2698 0.2310 0.028 Uiso 1 1 calc R . . C4E C 0.7972(6) 0.1743(4) 0.2796(4) 0.0292(14) Uani 1 1 d . . . H4E1 H 0.7496 0.1985 0.3033 0.044 Uiso 1 1 calc R . . H4E2 H 0.8731 0.1831 0.3174 0.044 Uiso 1 1 calc R . . H4E3 H 0.7602 0.1168 0.2618 0.044 Uiso 1 1 calc R . . C5E C 0.6740(5) 0.3227(4) -0.0208(3) 0.0194(12) Uani 1 1 d . . . H5E1 H 0.7089 0.2868 -0.0455 0.023 Uiso 1 1 calc R . . H5E2 H 0.7371 0.3701 0.0107 0.023 Uiso 1 1 calc R . . C6E C 0.5917(5) 0.3511(4) -0.0849(4) 0.0237(13) Uani 1 1 d . . . H6E1 H 0.5316 0.3042 -0.1200 0.028 Uiso 1 1 calc R . . H6E2 H 0.5533 0.3855 -0.0617 0.028 Uiso 1 1 calc R . . C7E C 0.6614(5) 0.3988(4) -0.1307(4) 0.0258(13) Uani 1 1 d . . . H7E1 H 0.6096 0.4211 -0.1677 0.031 Uiso 1 1 calc R . . H7E2 H 0.7230 0.4443 -0.0945 0.031 Uiso 1 1 calc R . . C8E C 0.7165(5) 0.3477(5) -0.1750(4) 0.0314(16) Uani 1 1 d . . . H8E1 H 0.7735 0.3296 -0.1384 0.047 Uiso 1 1 calc R . . H8E2 H 0.7541 0.3801 -0.2052 0.047 Uiso 1 1 calc R . . H8E3 H 0.6566 0.3012 -0.2093 0.047 Uiso 1 1 calc R . . C9E C 0.5620(5) 0.3306(4) 0.0744(4) 0.0247(14) Uani 1 1 d . . . H9E1 H 0.4902 0.3324 0.0362 0.030 Uiso 1 1 calc R . . H9E2 H 0.5400 0.3036 0.1141 0.030 Uiso 1 1 calc R . . C10E C 0.6348(5) 0.4178(4) 0.1127(4) 0.0246(13) Uani 1 1 d . . . H10E H 0.6590 0.4456 0.0741 0.030 Uiso 1 1 calc R . . H10F H 0.7048 0.4172 0.1534 0.030 Uiso 1 1 calc R . . C11E C 0.5637(6) 0.4639(5) 0.1484(4) 0.0322(16) Uani 1 1 d . . . H11E H 0.4934 0.4639 0.1076 0.039 Uiso 1 1 calc R . . H11F H 0.5395 0.4357 0.1868 0.039 Uiso 1 1 calc R . . C12E C 0.6322(6) 0.5499(5) 0.1865(4) 0.044(2) Uani 1 1 d . . . H12G H 0.7027 0.5503 0.2262 0.066 Uiso 1 1 calc R . . H12H H 0.5858 0.5758 0.2098 0.066 Uiso 1 1 calc R . . H12I H 0.6522 0.5790 0.1479 0.066 Uiso 1 1 calc R . . C13E C 0.5249(5) 0.1998(4) -0.0108(4) 0.0248(13) Uani 1 1 d . . . H13E H 0.4991 0.1711 0.0268 0.030 Uiso 1 1 calc R . . H13F H 0.4582 0.2141 -0.0432 0.030 Uiso 1 1 calc R . . C14E C 0.5616(5) 0.1425(4) -0.0623(4) 0.0239(13) Uani 1 1 d . . . H14E H 0.6329 0.1321 -0.0317 0.029 Uiso 1 1 calc R . . H14F H 0.5780 0.1680 -0.1043 0.029 Uiso 1 1 calc R . . C15E C 0.4653(5) 0.0617(4) -0.0968(4) 0.0309(15) Uani 1 1 d . . . H15E H 0.4580 0.0320 -0.0554 0.037 Uiso 1 1 calc R . . H15F H 0.3909 0.0727 -0.1199 0.037 Uiso 1 1 calc R . . C16E C 0.4922(6) 0.0097(4) -0.1585(5) 0.0375(17) Uani 1 1 d . . . H16G H 0.4983 0.0386 -0.2000 0.056 Uiso 1 1 calc R . . H16H H 0.4304 -0.0404 -0.1791 0.056 Uiso 1 1 calc R . . H16I H 0.5652 -0.0021 -0.1356 0.056 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 Re1A 0.01408(10) 0.01238(11) 0.01259(12) 0.00442(8) 0.00586(8) 0.00406(8) Re2A 0.01459(10) 0.01228(11) 0.01289(12) 0.00535(8) 0.00634(8) 0.00505(8) Re3A 0.01517(10) 0.01198(11) 0.01215(12) 0.00475(8) 0.00665(8) 0.00481(8) S1A 0.0186(6) 0.0200(7) 0.0132(7) 0.0072(5) 0.0049(5) 0.0076(5) S2A 0.0166(6) 0.0170(7) 0.0191(8) 0.0059(5) 0.0089(5) 0.0076(5) S3A 0.0189(6) 0.0133(7) 0.0153(7) 0.0041(5) 0.0077(5) 0.0044(5) S4A 0.0182(6) 0.0144(7) 0.0154(7) 0.0067(5) 0.0086(5) 0.0037(5) Cl2A 0.0247(6) 0.0174(7) 0.0244(8) 0.0110(6) 0.0130(5) 0.0125(5) Cl1A 0.0159(6) 0.0197(7) 0.0204(8) 0.0003(5) 0.0060(5) 0.0009(5) Cl3A 0.0276(6) 0.0184(7) 0.0172(8) 0.0075(5) 0.0136(5) 0.0080(5) Re1B 0.01121(9) 0.01283(11) 0.01193(12) 0.00471(8) 0.00490(7) 0.00370(8) Re2B 0.01141(9) 0.01251(11) 0.01275(12) 0.00504(8) 0.00553(7) 0.00438(8) Re3B 0.01133(9) 0.01362(11) 0.01208(12) 0.00562(8) 0.00576(7) 0.00439(8) S1B 0.0151(6) 0.0191(7) 0.0134(7) 0.0080(5) 0.0059(5) 0.0065(5) S2B 0.0129(5) 0.0183(7) 0.0168(8) 0.0075(5) 0.0075(5) 0.0066(5) S3B 0.0163(6) 0.0181(7) 0.0132(7) 0.0023(5) 0.0072(5) 0.0057(5) S4B 0.0156(6) 0.0154(7) 0.0155(7) 0.0060(5) 0.0057(5) 0.0041(5) Cl2B 0.0205(6) 0.0175(7) 0.0259(8) 0.0091(6) 0.0109(5) 0.0100(5) Cl1B 0.0154(5) 0.0199(7) 0.0158(7) 0.0024(5) 0.0022(5) 0.0022(5) Cl3B 0.0175(6) 0.0277(8) 0.0213(8) 0.0129(6) 0.0118(5) 0.0070(5) N1C 0.022(2) 0.019(3) 0.013(3) 0.0082(19) 0.0087(18) 0.008(2) C1C 0.020(2) 0.018(3) 0.016(3) 0.010(2) 0.010(2) 0.002(2) C2C 0.025(3) 0.027(4) 0.042(4) 0.017(3) 0.018(3) 0.013(3) C3C 0.020(3) 0.027(3) 0.030(4) 0.006(3) 0.012(2) 0.004(2) C4C 0.023(3) 0.035(4) 0.049(5) 0.000(3) 0.014(3) -0.001(3) C5C 0.021(3) 0.014(3) 0.021(3) 0.008(2) 0.009(2) 0.004(2) C6C 0.028(3) 0.021(3) 0.020(3) 0.006(2) 0.010(2) 0.007(2) C7C 0.033(3) 0.023(3) 0.025(4) 0.003(3) 0.011(3) 0.004(3) C8C 0.066(5) 0.033(4) 0.030(5) -0.004(3) 0.017(4) 0.004(4) C9C 0.021(3) 0.022(3) 0.016(3) 0.011(2) 0.010(2) 0.008(2) C10C 0.024(3) 0.019(3) 0.021(3) 0.008(2) 0.007(2) 0.006(2) C11C 0.032(3) 0.021(3) 0.020(4) 0.006(3) 0.010(2) 0.003(3) C12C 0.069(5) 0.033(4) 0.019(4) 0.009(3) 0.015(3) 0.019(4) C13C 0.021(3) 0.022(3) 0.016(3) 0.011(2) 0.006(2) 0.011(2) C14C 0.018(2) 0.018(3) 0.024(3) 0.009(2) 0.008(2) 0.005(2) C15C 0.015(2) 0.020(3) 0.023(3) 0.005(2) 0.004(2) 0.001(2) C16C 0.021(3) 0.037(4) 0.042(4) 0.013(3) 0.012(3) 0.011(3) N1D 0.017(2) 0.016(2) 0.015(3) 0.0041(19) 0.0084(18) 0.0051(19) C1D 0.020(3) 0.016(3) 0.014(3) 0.003(2) 0.006(2) 0.003(2) C2D 0.018(2) 0.025(3) 0.012(3) 0.005(2) 0.007(2) 0.007(2) C3D 0.025(3) 0.023(3) 0.028(4) 0.013(3) 0.013(2) 0.007(2) C4D 0.031(3) 0.061(5) 0.037(5) 0.025(4) 0.010(3) 0.023(4) C5D 0.017(2) 0.018(3) 0.021(3) 0.005(2) 0.008(2) 0.003(2) C6D 0.021(3) 0.019(3) 0.019(3) 0.002(2) 0.005(2) -0.001(2) C7D 0.032(3) 0.019(3) 0.027(4) 0.006(3) 0.011(3) 0.000(3) C8D 0.042(3) 0.021(3) 0.029(4) 0.011(3) 0.016(3) 0.011(3) C9D 0.021(3) 0.021(3) 0.016(3) 0.002(2) 0.005(2) 0.006(2) C10D 0.021(3) 0.022(3) 0.018(3) 0.004(2) 0.005(2) 0.006(2) C11D 0.019(3) 0.022(3) 0.016(3) 0.001(2) 0.002(2) 0.008(2) C12D 0.027(3) 0.021(3) 0.032(4) 0.002(3) 0.004(3) -0.004(3) C13D 0.019(2) 0.019(3) 0.020(3) 0.006(2) 0.011(2) 0.007(2) C14D 0.016(2) 0.024(3) 0.023(4) 0.006(3) 0.004(2) 0.004(2) C15D 0.022(3) 0.024(3) 0.035(4) 0.014(3) 0.010(3) 0.009(3) C16D 0.030(3) 0.047(5) 0.038(5) 0.023(4) 0.002(3) 0.014(3) N1E 0.022(2) 0.026(3) 0.019(3) 0.010(2) 0.0113(19) 0.009(2) C1E 0.023(3) 0.029(3) 0.020(3) 0.012(3) 0.008(2) 0.012(3) C2E 0.028(3) 0.022(3) 0.019(3) 0.008(2) 0.014(2) 0.009(2) C3E 0.028(3) 0.029(3) 0.017(3) 0.008(3) 0.007(2) 0.017(3) C4E 0.038(3) 0.034(4) 0.024(4) 0.013(3) 0.013(3) 0.017(3) C5E 0.023(3) 0.025(3) 0.017(3) 0.009(2) 0.012(2) 0.010(2) C6E 0.030(3) 0.030(4) 0.022(4) 0.013(3) 0.015(2) 0.017(3) C7E 0.027(3) 0.027(3) 0.023(4) 0.011(3) 0.006(2) 0.007(3) C8E 0.029(3) 0.045(4) 0.037(4) 0.026(3) 0.022(3) 0.017(3) C9E 0.026(3) 0.032(4) 0.029(4) 0.015(3) 0.018(3) 0.016(3) C10E 0.031(3) 0.033(4) 0.020(4) 0.009(3) 0.015(2) 0.018(3) C11E 0.038(3) 0.050(5) 0.022(4) 0.010(3) 0.015(3) 0.030(3) C12E 0.037(4) 0.059(5) 0.032(4) -0.010(4) -0.001(3) 0.029(4) C13E 0.022(3) 0.029(4) 0.028(4) 0.014(3) 0.008(2) 0.011(3) C14E 0.020(3) 0.023(3) 0.030(4) 0.008(3) 0.011(2) 0.004(2) C15E 0.023(3) 0.034(4) 0.033(4) 0.017(3) 0.006(3) 0.002(3) C16E 0.039(4) 0.016(3) 0.043(5) 0.006(3) 0.003(3) -0.006(3) _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 Re1A S1A 2.3949(14) . ? Re1A S4A 2.3964(13) . ? Re1A S2A 2.4024(13) . ? Re1A S3A 2.4079(13) . ? Re1A Cl1A 2.4254(14) . ? Re1A Re3A 2.5903(5) 2 ? Re1A Re3A 2.6000(4) . ? Re1A Re2A 2.6062(5) . ? Re1A Re2A 2.6089(4) 2 ? Re2A S3A 2.3912(15) 2 ? Re2A S1A 2.4091(15) . ? Re2A S4A 2.4073(12) 2 ? Re2A S2A 2.4044(13) . ? Re2A Cl2A 2.4286(12) . ? Re2A Re3A 2.5886(4) . ? Re2A Re3A 2.5952(4) 2 ? Re2A Re1A 2.6089(4) 2 ? Re3A Cl3A 2.4010(13) . ? Re3A S2A 2.4069(13) 2 ? Re3A S3A 2.4074(14) . ? Re3A S1A 2.4167(12) . ? Re3A S4A 2.4162(14) 2 ? Re3A Re1A 2.5903(5) 2 ? Re3A Re2A 2.5952(4) 2 ? S2A Re3A 2.4069(13) 2 ? S3A Re2A 2.3912(15) 2 ? S4A Re2A 2.4073(12) 2 ? S4A Re3A 2.4162(14) 2 ? Re1B S1B 2.3888(13) . ? Re1B S4B 2.3955(13) . ? Re1B S2B 2.4055(12) . ? Re1B S3B 2.4060(12) . ? Re1B Cl1B 2.4161(14) . ? Re1B Re2B 2.5863(5) 2_544 ? Re1B Re2B 2.5962(4) . ? Re1B Re3B 2.6041(4) . ? Re1B Re3B 2.6063(5) 2_544 ? Re2B S1B 2.4113(14) 2_544 ? Re2B S4B 2.4082(13) . ? Re2B Cl2B 2.4097(12) . ? Re2B S2B 2.4160(13) 2_544 ? Re2B S3B 2.4140(14) . ? Re2B Re1B 2.5863(5) 2_544 ? Re2B Re3B 2.5928(4) . ? Re2B Re3B 2.5985(4) 2_544 ? Re3B S1B 2.3968(12) 2_544 ? Re3B S4B 2.4026(15) . ? Re3B S2B 2.4019(12) . ? Re3B S3B 2.4082(15) 2_544 ? Re3B Cl3B 2.4235(13) . ? Re3B Re2B 2.5985(4) 2_544 ? Re3B Re1B 2.6063(5) 2_544 ? S1B Re3B 2.3968(12) 2_544 ? S1B Re2B 2.4113(14) 2_544 ? S2B Re2B 2.4160(13) 2_544 ? S3B Re3B 2.4082(15) 2_544 ? N1C C9C 1.507(8) . ? N1C C13C 1.516(6) . ? N1C C5C 1.522(7) . ? N1C C1C 1.523(6) . ? C1C C2C 1.509(7) . ? C1C H1C1 0.9700 . ? C1C H1C2 0.9700 . ? C2C C3C 1.541(8) . ? C2C H2C1 0.9700 . ? C2C H2C2 0.9700 . ? C3C C4C 1.516(10) . ? C3C H3C1 0.9700 . ? C3C H3C2 0.9700 . ? C4C H4C1 0.9600 . ? C4C H4C2 0.9600 . ? C4C H4C3 0.9600 . ? C5C C6C 1.512(9) . ? C5C H5C1 0.9700 . ? C5C H5C2 0.9700 . ? C6C C7C 1.524(9) . ? C6C H6C1 0.9700 . ? C6C H6C2 0.9700 . ? C7C C8C 1.504(10) . ? C7C H7C1 0.9700 . ? C7C H7C2 0.9700 . ? C8C H8C1 0.9600 . ? C8C H8C2 0.9600 . ? C8C H8C3 0.9600 . ? C9C C10C 1.512(8) . ? C9C H9C1 0.9700 . ? C9C H9C2 0.9700 . ? C10C C11C 1.525(9) . ? C10C H10A 0.9700 . ? C10C H10B 0.9700 . ? C11C C12C 1.498(10) . ? C11C H11A 0.9700 . ? C11C H11B 0.9700 . ? C12C H12A 0.9600 . ? C12C H12B 0.9600 . ? C12C H12C 0.9600 . ? C13C C14C 1.523(7) . ? C13C H13A 0.9700 . ? C13C H13B 0.9700 . ? C14C C15C 1.533(7) . ? C14C H14A 0.9700 . ? C14C H14B 0.9700 . ? C15C C16C 1.524(8) . ? C15C H15A 0.9700 . ? C15C H15B 0.9700 . ? C16C H16A 0.9600 . ? C16C H16B 0.9600 . ? C16C H16C 0.9600 . ? N1D C1D 1.516(7) . ? N1D C5D 1.521(7) . ? N1D C9D 1.526(7) . ? N1D C13D 1.527(6) . ? C1D C2D 1.515(7) . ? C1D H1D1 0.9700 . ? C1D H1D2 0.9700 . ? C2D C3D 1.529(8) . ? C2D H2D1 0.9700 . ? C2D H2D2 0.9700 . ? C3D C4D 1.516(8) . ? C3D H3D1 0.9700 . ? C3D H3D2 0.9700 . ? C4D H4D1 0.9600 . ? C4D H4D2 0.9600 . ? C4D H4D3 0.9600 . ? C5D C6D 1.530(8) . ? C5D H5D1 0.9700 . ? C5D H5D2 0.9700 . ? C6D C7D 1.528(8) . ? C6D H6D1 0.9700 . ? C6D H6D2 0.9700 . ? C7D C8D 1.525(9) . ? C7D H7D1 0.9700 . ? C7D H7D2 0.9700 . ? C8D H8D1 0.9600 . ? C8D H8D2 0.9600 . ? C8D H8D3 0.9600 . ? C9D C10D 1.524(8) . ? C9D H9D1 0.9700 . ? C9D H9D2 0.9700 . ? C10D C11D 1.522(8) . ? C10D H10C 0.9700 . ? C10D H10D 0.9700 . ? C11D C12D 1.515(9) . ? C11D H11C 0.9700 . ? C11D H11D 0.9700 . ? C12D H12D 0.9600 . ? C12D H12E 0.9600 . ? C12D H12F 0.9600 . ? C13D C14D 1.523(8) . ? C13D H13C 0.9700 . ? C13D H13D 0.9700 . ? C14D C15D 1.534(8) . ? C14D H14C 0.9700 . ? C14D H14D 0.9700 . ? C15D C16D 1.521(9) . ? C15D H15C 0.9700 . ? C15D H15D 0.9700 . ? C16D H16D 0.9600 . ? C16D H16E 0.9600 . ? C16D H16F 0.9600 . ? N1E C5E 1.514(7) . ? N1E C1E 1.516(7) . ? N1E C9E 1.527(7) . ? N1E C13E 1.530(8) . ? C1E C2E 1.508(8) . ? C1E H1E1 0.9700 . ? C1E H1E2 0.9700 . ? C2E C3E 1.529(8) . ? C2E H2E1 0.9700 . ? C2E H2E2 0.9700 . ? C3E C4E 1.500(8) . ? C3E H3E1 0.9700 . ? C3E H3E2 0.9700 . ? C4E H4E1 0.9600 . ? C4E H4E2 0.9600 . ? C4E H4E3 0.9600 . ? C5E C6E 1.526(7) . ? C5E H5E1 0.9700 . ? C5E H5E2 0.9700 . ? C6E C7E 1.530(8) . ? C6E H6E1 0.9700 . ? C6E H6E2 0.9700 . ? C7E C8E 1.520(9) . ? C7E H7E1 0.9700 . ? C7E H7E2 0.9700 . ? C8E H8E1 0.9600 . ? C8E H8E2 0.9600 . ? C8E H8E3 0.9600 . ? C9E C10E 1.519(9) . ? C9E H9E1 0.9700 . ? C9E H9E2 0.9700 . ? C10E C11E 1.534(8) . ? C10E H10E 0.9700 . ? C10E H10F 0.9700 . ? C11E C12E 1.491(11) . ? C11E H11E 0.9700 . ? C11E H11F 0.9700 . ? C12E H12G 0.9600 . ? C12E H12H 0.9600 . ? C12E H12I 0.9600 . ? C13E C14E 1.512(9) . ? C13E H13E 0.9700 . ? C13E H13F 0.9700 . ? C14E C15E 1.530(9) . ? C14E H14E 0.9700 . ? C14E H14F 0.9700 . ? C15E C16E 1.511(10) . ? C15E H15E 0.9700 . ? C15E H15F 0.9700 . ? C16E H16G 0.9600 . ? C16E H16H 0.9600 . ? C16E H16I 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 S1A Re1A S4A 173.79(5) . . ? S1A Re1A S2A 89.61(5) . . ? S4A Re1A S2A 90.33(5) . . ? S1A Re1A S3A 90.14(5) . . ? S4A Re1A S3A 89.13(5) . . ? S2A Re1A S3A 172.69(5) . . ? S1A Re1A Cl1A 92.98(5) . . ? S4A Re1A Cl1A 93.23(5) . . ? S2A Re1A Cl1A 92.47(5) . . ? S3A Re1A Cl1A 94.85(5) . . ? S1A Re1A Re3A 117.29(4) . 2 ? S4A Re1A Re3A 57.81(4) . 2 ? S2A Re1A Re3A 57.50(3) . 2 ? S3A Re1A Re3A 116.44(3) . 2 ? Cl1A Re1A Re3A 134.67(4) . 2 ? S1A Re1A Re3A 57.70(3) . . ? S4A Re1A Re3A 117.04(3) . . ? S2A Re1A Re3A 116.79(3) . . ? S3A Re1A Re3A 57.31(3) . . ? Cl1A Re1A Re3A 136.01(4) . . ? Re3A Re1A Re3A 89.309(16) 2 . ? S1A Re1A Re2A 57.41(4) . . ? S4A Re1A Re2A 117.69(4) . . ? S2A Re1A Re2A 57.21(3) . . ? S3A Re1A Re2A 116.90(3) . . ? Cl1A Re1A Re2A 134.26(3) . . ? Re3A Re1A Re2A 59.922(15) 2 . ? Re3A Re1A Re2A 59.633(13) . . ? S1A Re1A Re2A 117.44(3) . 2 ? S4A Re1A Re2A 57.31(3) . 2 ? S2A Re1A Re2A 117.18(4) . 2 ? S3A Re1A Re2A 56.76(3) . 2 ? Cl1A Re1A Re2A 135.88(3) . 2 ? Re3A Re1A Re2A 59.720(13) 2 2 ? Re3A Re1A Re2A 59.765(11) . 2 ? Re2A Re1A Re2A 89.858(17) . 2 ? S3A Re2A S1A 173.22(4) 2 . ? S3A Re2A S4A 89.27(5) 2 2 ? S1A Re2A S4A 90.92(5) . 2 ? S3A Re2A S2A 89.81(5) 2 . ? S1A Re2A S2A 89.22(5) . . ? S4A Re2A S2A 173.30(4) 2 . ? S3A Re2A Cl2A 92.96(5) 2 . ? S1A Re2A Cl2A 93.80(5) . . ? S4A Re2A Cl2A 92.66(4) 2 . ? S2A Re2A Cl2A 94.01(4) . . ? S3A Re2A Re3A 117.12(3) 2 . ? S1A Re2A Re3A 57.70(3) . . ? S4A Re2A Re3A 57.71(3) 2 . ? S2A Re2A Re3A 117.15(3) . . ? Cl2A Re2A Re3A 134.99(3) . . ? S3A Re2A Re3A 57.56(3) 2 2 ? S1A Re2A Re3A 116.58(3) . 2 ? S4A Re2A Re3A 116.82(3) 2 2 ? S2A Re2A Re3A 57.40(3) . 2 ? Cl2A Re2A Re3A 135.55(3) . 2 ? Re3A Re2A Re3A 89.451(13) . 2 ? S3A Re2A Re1A 117.27(4) 2 . ? S1A Re2A Re1A 56.89(3) . . ? S4A Re2A Re1A 117.73(3) 2 . ? S2A Re2A Re1A 57.13(3) . . ? Cl2A Re2A Re1A 135.59(3) . . ? Re3A Re2A Re1A 60.065(11) . . ? Re3A Re2A Re1A 59.735(14) 2 . ? S3A Re2A Re1A 57.38(3) 2 2 ? S1A Re2A Re1A 117.44(3) . 2 ? S4A Re2A Re1A 56.90(3) 2 2 ? S2A Re2A Re1A 117.32(3) . 2 ? Cl2A Re2A Re1A 134.27(4) . 2 ? Re3A Re2A Re1A 59.783(13) . 2 ? Re3A Re2A Re1A 59.948(12) 2 2 ? Re1A Re2A Re1A 90.142(17) . 2 ? Cl3A Re3A S2A 92.49(5) . 2 ? Cl3A Re3A S3A 94.16(5) . . ? S2A Re3A S3A 89.37(5) 2 . ? Cl3A Re3A S1A 93.87(5) . . ? S2A Re3A S1A 173.61(5) 2 . ? S3A Re3A S1A 89.64(5) . . ? Cl3A Re3A S4A 92.41(5) . 2 ? S2A Re3A S4A 89.75(5) 2 2 ? S3A Re3A S4A 173.40(5) . 2 ? S1A Re3A S4A 90.52(5) . 2 ? Cl3A Re3A Re2A 134.51(3) . . ? S2A Re3A Re2A 117.78(4) 2 . ? S3A Re3A Re2A 117.58(3) . . ? S1A Re3A Re2A 57.42(4) . . ? S4A Re3A Re2A 57.38(3) 2 . ? Cl3A Re3A Re1A 133.60(4) . 2 ? S2A Re3A Re1A 57.33(4) 2 2 ? S3A Re3A Re1A 117.28(4) . 2 ? S1A Re3A Re1A 117.86(4) . 2 ? S4A Re3A Re1A 57.07(3) 2 2 ? Re2A Re3A Re1A 60.497(12) . 2 ? Cl3A Re3A Re2A 134.93(3) . 2 ? S2A Re3A Re2A 57.31(3) 2 2 ? S3A Re3A Re2A 56.96(4) . 2 ? S1A Re3A Re2A 117.15(3) . 2 ? S4A Re3A Re2A 117.37(4) 2 2 ? Re2A Re3A Re2A 90.549(13) . 2 ? Re1A Re3A Re2A 60.343(12) 2 2 ? Cl3A Re3A Re1A 135.71(4) . . ? S2A Re3A Re1A 117.57(3) 2 . ? S3A Re3A Re1A 57.33(3) . . ? S1A Re3A Re1A 56.89(3) . . ? S4A Re3A Re1A 117.63(3) 2 . ? Re2A Re3A Re1A 60.302(12) . . ? Re1A Re3A Re1A 90.691(16) 2 . ? Re2A Re3A Re1A 60.287(12) 2 . ? Re1A S1A Re2A 65.71(4) . . ? Re1A S1A Re3A 65.41(3) . . ? Re2A S1A Re3A 64.88(4) . . ? Re1A S2A Re3A 65.18(3) . 2 ? Re1A S2A Re2A 65.66(3) . . ? Re3A S2A Re2A 65.28(3) 2 . ? Re2A S3A Re3A 65.48(4) 2 . ? Re2A S3A Re1A 65.86(4) 2 . ? Re3A S3A Re1A 65.36(4) . . ? Re1A S4A Re2A 65.79(3) . 2 ? Re1A S4A Re3A 65.12(4) . 2 ? Re2A S4A Re3A 64.91(3) 2 2 ? S1B Re1B S4B 173.68(5) . . ? S1B Re1B S2B 90.73(4) . . ? S4B Re1B S2B 89.38(4) . . ? S1B Re1B S3B 89.27(4) . . ? S4B Re1B S3B 89.90(4) . . ? S2B Re1B S3B 173.48(5) . . ? S1B Re1B Cl1B 91.18(5) . . ? S4B Re1B Cl1B 95.13(5) . . ? S2B Re1B Cl1B 92.17(5) . . ? S3B Re1B Cl1B 94.35(5) . . ? S1B Re1B Re2B 57.82(4) . 2_544 ? S4B Re1B Re2B 117.30(4) . 2_544 ? S2B Re1B Re2B 57.76(3) . 2_544 ? S3B Re1B Re2B 117.13(4) . 2_544 ? Cl1B Re1B Re2B 133.03(3) . 2_544 ? S1B Re1B Re2B 117.05(3) . . ? S4B Re1B Re2B 57.52(3) . . ? S2B Re1B Re2B 116.92(3) . . ? S3B Re1B Re2B 57.56(3) . . ? Cl1B Re1B Re2B 137.39(3) . . ? Re2B Re1B Re2B 89.577(17) 2_544 . ? S1B Re1B Re3B 117.86(4) . . ? S4B Re1B Re3B 57.26(4) . . ? S2B Re1B Re3B 57.14(3) . . ? S3B Re1B Re3B 117.35(3) . . ? Cl1B Re1B Re3B 135.45(3) . . ? Re2B Re1B Re3B 60.082(14) 2_544 . ? Re2B Re1B Re3B 59.814(12) . . ? S1B Re1B Re3B 57.15(3) . 2_544 ? S4B Re1B Re3B 117.43(3) . 2_544 ? S2B Re1B Re3B 117.62(4) . 2_544 ? S3B Re1B Re3B 57.26(3) . 2_544 ? Cl1B Re1B Re3B 134.28(3) . 2_544 ? Re2B Re1B Re3B 59.910(14) 2_544 2_544 ? Re2B Re1B Re3B 59.930(12) . 2_544 ? Re3B Re1B Re3B 90.193(17) . 2_544 ? S1B Re2B S4B 90.24(5) 2_544 . ? S1B Re2B Cl2B 91.71(5) 2_544 . ? S4B Re2B Cl2B 93.57(4) . . ? S1B Re2B S2B 89.94(5) 2_544 2_544 ? S4B Re2B S2B 173.45(4) . 2_544 ? Cl2B Re2B S2B 92.97(4) . 2_544 ? S1B Re2B S3B 173.29(4) 2_544 . ? S4B Re2B S3B 89.41(5) . . ? Cl2B Re2B S3B 95.00(5) . . ? S2B Re2B S3B 89.65(5) 2_544 . ? S1B Re2B Re1B 56.98(3) 2_544 2_544 ? S4B Re2B Re1B 117.66(4) . 2_544 ? Cl2B Re2B Re1B 133.28(4) . 2_544 ? S2B Re2B Re1B 57.36(3) 2_544 2_544 ? S3B Re2B Re1B 117.55(4) . 2_544 ? S1B Re2B Re3B 57.10(3) 2_544 . ? S4B Re2B Re3B 57.28(3) . . ? Cl2B Re2B Re3B 133.56(3) . . ? S2B Re2B Re3B 117.75(3) 2_544 . ? S3B Re2B Re3B 117.48(3) . . ? Re1B Re2B Re3B 60.427(12) 2_544 . ? S1B Re2B Re1B 117.29(3) 2_544 . ? S4B Re2B Re1B 57.05(3) . . ? Cl2B Re2B Re1B 136.28(4) . . ? S2B Re2B Re1B 117.30(3) 2_544 . ? S3B Re2B Re1B 57.26(3) . . ? Re1B Re2B Re1B 90.423(17) 2_544 . ? Re3B Re2B Re1B 60.245(11) . . ? S1B Re2B Re3B 117.24(4) 2_544 2_544 ? S4B Re2B Re3B 117.25(3) . 2_544 ? Cl2B Re2B Re3B 135.80(3) . 2_544 ? S2B Re2B Re3B 57.10(3) 2_544 2_544 ? S3B Re2B Re3B 57.28(3) . 2_544 ? Re1B Re2B Re3B 60.297(11) 2_544 2_544 ? Re3B Re2B Re3B 90.616(13) . 2_544 ? Re1B Re2B Re3B 60.229(13) . 2_544 ? S1B Re3B S4B 90.72(5) 2_544 . ? S1B Re3B S2B 173.32(4) 2_544 . ? S4B Re3B S2B 89.30(5) . . ? S1B Re3B S3B 89.03(5) 2_544 2_544 ? S4B Re3B S3B 172.89(4) . 2_544 ? S2B Re3B S3B 90.12(5) . 2_544 ? S1B Re3B Cl3B 92.73(4) 2_544 . ? S4B Re3B Cl3B 93.43(5) . . ? S2B Re3B Cl3B 93.94(4) . . ? S3B Re3B Cl3B 93.68(5) 2_544 . ? S1B Re3B Re2B 57.64(3) 2_544 . ? S4B Re3B Re2B 57.49(3) . . ? S2B Re3B Re2B 117.17(3) . . ? S3B Re3B Re2B 116.81(3) 2_544 . ? Cl3B Re3B Re2B 134.63(3) . . ? S1B Re3B Re2B 116.67(3) 2_544 2_544 ? S4B Re3B Re2B 116.58(3) . 2_544 ? S2B Re3B Re2B 57.62(3) . 2_544 ? S3B Re3B Re2B 57.50(3) 2_544 2_544 ? Cl3B Re3B Re2B 135.99(3) . 2_544 ? Re2B Re3B Re2B 89.384(13) . 2_544 ? S1B Re3B Re1B 117.52(3) 2_544 . ? S4B Re3B Re1B 57.00(3) . . ? S2B Re3B Re1B 57.27(3) . . ? S3B Re3B Re1B 117.09(4) 2_544 . ? Cl3B Re3B Re1B 135.46(4) . . ? Re2B Re3B Re1B 59.941(12) . . ? Re2B Re3B Re1B 59.620(13) 2_544 . ? S1B Re3B Re1B 56.85(3) 2_544 2_544 ? S4B Re3B Re1B 117.11(3) . 2_544 ? S2B Re3B Re1B 117.43(3) . 2_544 ? S3B Re3B Re1B 57.18(3) 2_544 2_544 ? Cl3B Re3B Re1B 134.72(4) . 2_544 ? Re2B Re3B Re1B 59.663(12) . 2_544 ? Re2B Re3B Re1B 59.841(12) 2_544 2_544 ? Re1B Re3B Re1B 89.807(17) . 2_544 ? Re1B S1B Re3B 66.00(3) . 2_544 ? Re1B S1B Re2B 65.20(4) . 2_544 ? Re3B S1B Re2B 65.27(4) 2_544 2_544 ? Re1B S2B Re3B 65.60(3) . . ? Re1B S2B Re2B 64.88(3) . 2_544 ? Re3B S2B Re2B 65.28(3) . 2_544 ? Re1B S3B Re3B 65.56(4) . 2_544 ? Re1B S3B Re2B 65.18(4) . . ? Re3B S3B Re2B 65.21(4) 2_544 . ? Re1B S4B Re3B 65.74(4) . . ? Re1B S4B Re2B 65.43(4) . . ? Re3B S4B Re2B 65.23(4) . . ? C9C N1C C13C 111.2(4) . . ? C9C N1C C5C 106.7(4) . . ? C13C N1C C5C 110.6(4) . . ? C9C N1C C1C 111.5(4) . . ? C13C N1C C1C 106.2(4) . . ? C5C N1C C1C 110.8(4) . . ? C2C C1C N1C 114.6(4) . . ? C2C C1C H1C1 108.6 . . ? N1C C1C H1C1 108.6 . . ? C2C C1C H1C2 108.6 . . ? N1C C1C H1C2 108.6 . . ? H1C1 C1C H1C2 107.6 . . ? C1C C2C C3C 110.7(5) . . ? C1C C2C H2C1 109.5 . . ? C3C C2C H2C1 109.5 . . ? C1C C2C H2C2 109.5 . . ? C3C C2C H2C2 109.5 . . ? H2C1 C2C H2C2 108.1 . . ? C4C C3C C2C 113.3(6) . . ? C4C C3C H3C1 108.9 . . ? C2C C3C H3C1 108.9 . . ? C4C C3C H3C2 108.9 . . ? C2C C3C H3C2 108.9 . . ? H3C1 C3C H3C2 107.7 . . ? C3C C4C H4C1 109.5 . . ? C3C C4C H4C2 109.5 . . ? H4C1 C4C H4C2 109.5 . . ? C3C C4C H4C3 109.5 . . ? H4C1 C4C H4C3 109.5 . . ? H4C2 C4C H4C3 109.5 . . ? C6C C5C N1C 115.6(5) . . ? C6C C5C H5C1 108.4 . . ? N1C C5C H5C1 108.4 . . ? C6C C5C H5C2 108.4 . . ? N1C C5C H5C2 108.4 . . ? H5C1 C5C H5C2 107.4 . . ? C5C C6C C7C 110.1(5) . . ? C5C C6C H6C1 109.6 . . ? C7C C6C H6C1 109.6 . . ? C5C C6C H6C2 109.6 . . ? C7C C6C H6C2 109.6 . . ? H6C1 C6C H6C2 108.2 . . ? C8C C7C C6C 112.3(6) . . ? C8C C7C H7C1 109.1 . . ? C6C C7C H7C1 109.1 . . ? C8C C7C H7C2 109.1 . . ? C6C C7C H7C2 109.1 . . ? H7C1 C7C H7C2 107.9 . . ? C7C C8C H8C1 109.5 . . ? C7C C8C H8C2 109.5 . . ? H8C1 C8C H8C2 109.5 . . ? C7C C8C H8C3 109.5 . . ? H8C1 C8C H8C3 109.5 . . ? H8C2 C8C H8C3 109.5 . . ? C10C C9C N1C 116.8(5) . . ? C10C C9C H9C1 108.1 . . ? N1C C9C H9C1 108.1 . . ? C10C C9C H9C2 108.1 . . ? N1C C9C H9C2 108.1 . . ? H9C1 C9C H9C2 107.3 . . ? C9C C10C C11C 110.5(5) . . ? C9C C10C H10A 109.6 . . ? C11C C10C H10A 109.6 . . ? C9C C10C H10B 109.6 . . ? C11C C10C H10B 109.6 . . ? H10A C10C H10B 108.1 . . ? C12C C11C C10C 113.8(5) . . ? C12C C11C H11A 108.8 . . ? C10C C11C H11A 108.8 . . ? C12C C11C H11B 108.8 . . ? C10C C11C H11B 108.8 . . ? H11A C11C H11B 107.7 . . ? C11C C12C H12A 109.5 . . ? C11C C12C H12B 109.5 . . ? H12A C12C H12B 109.5 . . ? C11C C12C H12C 109.5 . . ? H12A C12C H12C 109.5 . . ? H12B C12C H12C 109.5 . . ? N1C C13C C14C 115.0(4) . . ? N1C C13C H13A 108.5 . . ? C14C C13C H13A 108.5 . . ? N1C C13C H13B 108.5 . . ? C14C C13C H13B 108.5 . . ? H13A C13C H13B 107.5 . . ? C13C C14C C15C 109.7(4) . . ? C13C C14C H14A 109.7 . . ? C15C C14C H14A 109.7 . . ? C13C C14C H14B 109.7 . . ? C15C C14C H14B 109.7 . . ? H14A C14C H14B 108.2 . . ? C14C C15C C16C 112.0(5) . . ? C14C C15C H15A 109.2 . . ? C16C C15C H15A 109.2 . . ? C14C C15C H15B 109.2 . . ? C16C C15C H15B 109.2 . . ? H15A C15C H15B 107.9 . . ? C15C C16C H16A 109.5 . . ? C15C C16C H16B 109.5 . . ? H16A C16C H16B 109.5 . . ? C15C C16C H16C 109.5 . . ? H16A C16C H16C 109.5 . . ? H16B C16C H16C 109.5 . . ? C1D N1D C5D 110.9(4) . . ? C1D N1D C9D 111.5(4) . . ? C5D N1D C9D 106.6(4) . . ? C1D N1D C13D 106.8(4) . . ? C5D N1D C13D 111.1(4) . . ? C9D N1D C13D 110.0(4) . . ? N1D C1D C2D 115.1(4) . . ? N1D C1D H1D1 108.5 . . ? C2D C1D H1D1 108.5 . . ? N1D C1D H1D2 108.5 . . ? C2D C1D H1D2 108.5 . . ? H1D1 C1D H1D2 107.5 . . ? C1D C2D C3D 110.5(4) . . ? C1D C2D H2D1 109.5 . . ? C3D C2D H2D1 109.6 . . ? C1D C2D H2D2 109.6 . . ? C3D C2D H2D2 109.5 . . ? H2D1 C2D H2D2 108.1 . . ? C4D C3D C2D 111.4(5) . . ? C4D C3D H3D1 109.3 . . ? C2D C3D H3D1 109.3 . . ? C4D C3D H3D2 109.3 . . ? C2D C3D H3D2 109.3 . . ? H3D1 C3D H3D2 108.0 . . ? C3D C4D H4D1 109.5 . . ? C3D C4D H4D2 109.5 . . ? H4D1 C4D H4D2 109.5 . . ? C3D C4D H4D3 109.5 . . ? H4D1 C4D H4D3 109.5 . . ? H4D2 C4D H4D3 109.5 . . ? N1D C5D C6D 115.5(5) . . ? N1D C5D H5D1 108.4 . . ? C6D C5D H5D1 108.4 . . ? N1D C5D H5D2 108.4 . . ? C6D C5D H5D2 108.4 . . ? H5D1 C5D H5D2 107.5 . . ? C5D C6D C7D 110.9(5) . . ? C5D C6D H6D1 109.5 . . ? C7D C6D H6D1 109.5 . . ? C5D C6D H6D2 109.5 . . ? C7D C6D H6D2 109.5 . . ? H6D1 C6D H6D2 108.0 . . ? C8D C7D C6D 113.8(5) . . ? C8D C7D H7D1 108.8 . . ? C6D C7D H7D1 108.8 . . ? C8D C7D H7D2 108.8 . . ? C6D C7D H7D2 108.8 . . ? H7D1 C7D H7D2 107.7 . . ? C7D C8D H8D1 109.5 . . ? C7D C8D H8D2 109.5 . . ? H8D1 C8D H8D2 109.5 . . ? C7D C8D H8D3 109.5 . . ? H8D1 C8D H8D3 109.5 . . ? H8D2 C8D H8D3 109.5 . . ? N1D C9D C10D 116.3(5) . . ? N1D C9D H9D1 108.2 . . ? C10D C9D H9D1 108.2 . . ? N1D C9D H9D2 108.2 . . ? C10D C9D H9D2 108.2 . . ? H9D1 C9D H9D2 107.4 . . ? C11D C10D C9D 109.0(5) . . ? C11D C10D H10C 109.9 . . ? C9D C10D H10C 109.9 . . ? C11D C10D H10D 109.9 . . ? C9D C10D H10D 109.9 . . ? H10C C10D H10D 108.3 . . ? C12D C11D C10D 112.1(5) . . ? C12D C11D H11C 109.2 . . ? C10D C11D H11C 109.2 . . ? C12D C11D H11D 109.2 . . ? C10D C11D H11D 109.2 . . ? H11C C11D H11D 107.9 . . ? C11D C12D H12D 109.5 . . ? C11D C12D H12E 109.5 . . ? H12D C12D H12E 109.5 . . ? C11D C12D H12F 109.5 . . ? H12D C12D H12F 109.5 . . ? H12E C12D H12F 109.5 . . ? N1D C13D C14D 114.8(4) . . ? N1D C13D H13C 108.6 . . ? C14D C13D H13C 108.6 . . ? N1D C13D H13D 108.6 . . ? C14D C13D H13D 108.6 . . ? H13C C13D H13D 107.5 . . ? C13D C14D C15D 111.1(5) . . ? C13D C14D H14C 109.4 . . ? C15D C14D H14C 109.4 . . ? C13D C14D H14D 109.4 . . ? C15D C14D H14D 109.4 . . ? H14C C14D H14D 108.0 . . ? C16D C15D C14D 111.4(6) . . ? C16D C15D H15C 109.4 . . ? C14D C15D H15C 109.4 . . ? C16D C15D H15D 109.4 . . ? C14D C15D H15D 109.4 . . ? H15C C15D H15D 108.0 . . ? C15D C16D H16D 109.5 . . ? C15D C16D H16E 109.5 . . ? H16D C16D H16E 109.5 . . ? C15D C16D H16F 109.5 . . ? H16D C16D H16F 109.5 . . ? H16E C16D H16F 109.5 . . ? C5E N1E C1E 105.4(4) . . ? C5E N1E C9E 111.5(4) . . ? C1E N1E C9E 110.9(5) . . ? C5E N1E C13E 111.6(5) . . ? C1E N1E C13E 111.5(4) . . ? C9E N1E C13E 106.1(4) . . ? N1E C1E C2E 118.4(5) . . ? N1E C1E H1E1 107.7 . . ? C2E C1E H1E1 107.7 . . ? N1E C1E H1E2 107.7 . . ? C2E C1E H1E2 107.7 . . ? H1E1 C1E H1E2 107.1 . . ? C1E C2E C3E 108.4(5) . . ? C1E C2E H2E1 110.0 . . ? C3E C2E H2E1 110.0 . . ? C1E C2E H2E2 110.0 . . ? C3E C2E H2E2 110.0 . . ? H2E1 C2E H2E2 108.4 . . ? C4E C3E C2E 114.9(5) . . ? C4E C3E H3E1 108.6 . . ? C2E C3E H3E1 108.6 . . ? C4E C3E H3E2 108.6 . . ? C2E C3E H3E2 108.6 . . ? H3E1 C3E H3E2 107.5 . . ? C3E C4E H4E1 109.5 . . ? C3E C4E H4E2 109.5 . . ? H4E1 C4E H4E2 109.5 . . ? C3E C4E H4E3 109.5 . . ? H4E1 C4E H4E3 109.5 . . ? H4E2 C4E H4E3 109.5 . . ? N1E C5E C6E 116.9(4) . . ? N1E C5E H5E1 108.1 . . ? C6E C5E H5E1 108.1 . . ? N1E C5E H5E2 108.1 . . ? C6E C5E H5E2 108.1 . . ? H5E1 C5E H5E2 107.3 . . ? C7E C6E C5E 109.8(4) . . ? C7E C6E H6E1 109.7 . . ? C5E C6E H6E1 109.7 . . ? C7E C6E H6E2 109.7 . . ? C5E C6E H6E2 109.7 . . ? H6E1 C6E H6E2 108.2 . . ? C8E C7E C6E 113.7(5) . . ? C8E C7E H7E1 108.8 . . ? C6E C7E H7E1 108.8 . . ? C8E C7E H7E2 108.8 . . ? C6E C7E H7E2 108.8 . . ? H7E1 C7E H7E2 107.7 . . ? C7E C8E H8E1 109.5 . . ? C7E C8E H8E2 109.5 . . ? H8E1 C8E H8E2 109.5 . . ? C7E C8E H8E3 109.5 . . ? H8E1 C8E H8E3 109.5 . . ? H8E2 C8E H8E3 109.5 . . ? C10E C9E N1E 116.1(4) . . ? C10E C9E H9E1 108.3 . . ? N1E C9E H9E1 108.3 . . ? C10E C9E H9E2 108.3 . . ? N1E C9E H9E2 108.3 . . ? H9E1 C9E H9E2 107.4 . . ? C9E C10E C11E 110.6(5) . . ? C9E C10E H10E 109.5 . . ? C11E C10E H10E 109.5 . . ? C9E C10E H10F 109.5 . . ? C11E C10E H10F 109.5 . . ? H10E C10E H10F 108.1 . . ? C12E C11E C10E 112.2(5) . . ? C12E C11E H11E 109.2 . . ? C10E C11E H11E 109.2 . . ? C12E C11E H11F 109.2 . . ? C10E C11E H11F 109.2 . . ? H11E C11E H11F 107.9 . . ? C11E C12E H12G 109.5 . . ? C11E C12E H12H 109.5 . . ? H12G C12E H12H 109.5 . . ? C11E C12E H12I 109.5 . . ? H12G C12E H12I 109.5 . . ? H12H C12E H12I 109.5 . . ? C14E C13E N1E 114.8(4) . . ? C14E C13E H13E 108.6 . . ? N1E C13E H13E 108.6 . . ? C14E C13E H13F 108.6 . . ? N1E C13E H13F 108.6 . . ? H13E C13E H13F 107.5 . . ? C13E C14E C15E 111.0(5) . . ? C13E C14E H14E 109.4 . . ? C15E C14E H14E 109.4 . . ? C13E C14E H14F 109.4 . . ? C15E C14E H14F 109.4 . . ? H14E C14E H14F 108.0 . . ? C16E C15E C14E 111.4(5) . . ? C16E C15E H15E 109.4 . . ? C14E C15E H15E 109.4 . . ? C16E C15E H15F 109.4 . . ? C14E C15E H15F 109.4 . . ? H15E C15E H15F 108.0 . . ? C15E C16E H16G 109.5 . . ? C15E C16E H16H 109.5 . . ? H16G C16E H16H 109.5 . . ? C15E C16E H16I 109.5 . . ? H16G C16E H16I 109.5 . . ? H16H C16E H16I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.91 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.336 _refine_diff_density_min -2.166 _refine_diff_density_rms 0.268 #################### Material relevant to compound 2 at 293K ############ data_sb83e_abmerge _database_code_CSD 186993 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(PPh4)3 Re6S8(CN)6' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H60 N6 P3 Re6 S8' _chemical_formula_weight 2547.91 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' 'P' 'P' 0.1023 0.0942 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8727(11) _cell_length_b 15.2511(13) _cell_length_c 19.8989(18) _cell_angle_alpha 92.353(11) _cell_angle_beta 108.276(10) _cell_angle_gamma 100.193(9) _cell_volume 3913.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.2310 _exptl_crystal_size_mid 0.0770 _exptl_crystal_size_min 0.0578 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2386 _exptl_absorpt_coefficient_mu 9.564 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4146 _exptl_absorpt_correction_T_max 0.5981 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _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 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, Phi. incr. == 1.1' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41925 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.1403 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.79 _reflns_number_total 15502 _reflns_number_gt 8599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE, [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15502 _refine_ls_number_parameters 910 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0420 _refine_ls_wR_factor_gt 0.0352 _refine_ls_goodness_of_fit_ref 0.639 _refine_ls_restrained_S_all 0.639 _refine_ls_shift/su_max 0.004 _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 0.87562(3) 0.01538(2) 0.008254(14) 0.02524(8) Uani 1 1 d . . . Re2 Re 1.04211(3) 0.122163(19) 0.005164(14) 0.02531(8) Uani 1 1 d . . . Re3 Re 1.05487(2) 0.00470(2) 0.098015(14) 0.02509(8) Uani 1 1 d . . . S1 S 0.79513(16) -0.10267(12) -0.08819(9) 0.0327(5) Uani 1 1 d . . . S2 S 0.97596(16) 0.13223(13) 0.10267(9) 0.0325(5) Uani 1 1 d . . . S3 S 0.87238(16) 0.12217(12) -0.07812(9) 0.0322(5) Uani 1 1 d . . . S4 S 0.89641(16) -0.09486(12) 0.09264(9) 0.0326(5) Uani 1 1 d . . . C3 C 1.1136(6) 0.0073(5) 0.2126(4) 0.034(2) Uani 1 1 d . . . C1 C 0.7334(7) 0.0343(5) 0.0239(4) 0.031(2) Uani 1 1 d . . . C2 C 1.0879(6) 0.2637(6) 0.0074(4) 0.035(2) Uani 1 1 d . . . N2 N 1.1156(6) 0.3352(5) 0.0099(3) 0.055(2) Uani 1 1 d . . . N1 N 0.6708(7) 0.0500(5) 0.0379(4) 0.061(2) Uani 1 1 d . . . N3 N 1.1337(6) 0.0049(5) 0.2687(4) 0.068(2) Uani 1 1 d . . . Re4 Re 0.35972(2) 0.46576(2) 0.486144(14) 0.02614(8) Uani 1 1 d . . . Re5 Re 0.48246(3) 0.43523(2) 0.415690(14) 0.02604(8) Uani 1 1 d . . . Re6 Re 0.47593(3) 0.59891(2) 0.452514(14) 0.02645(8) Uani 1 1 d . . . S5 S 0.40863(16) 0.43616(13) 0.60860(9) 0.0342(5) Uani 1 1 d . . . S6 S 0.36484(16) 0.61999(13) 0.52128(9) 0.0337(5) Uani 1 1 d . . . S7 S 0.33115(16) 0.49929(13) 0.36580(9) 0.0344(5) Uani 1 1 d . . . S8 S 0.37660(16) 0.31670(12) 0.45350(9) 0.0336(5) Uani 1 1 d . . . C4 C 0.1967(8) 0.4283(5) 0.4708(4) 0.039(2) Uani 1 1 d . . . C5 C 0.4659(6) 0.3624(5) 0.3186(4) 0.034(2) Uani 1 1 d . . . C6 C 0.4499(6) 0.7147(5) 0.3938(4) 0.0285(18) Uani 1 1 d . . . N6 N 0.4324(6) 0.7653(5) 0.3632(4) 0.065(2) Uani 1 1 d . . . N4 N 0.1163(7) 0.4093(6) 0.4614(4) 0.068(3) Uani 1 1 d . . . N5 N 0.4595(6) 0.3232(5) 0.2691(4) 0.057(2) Uani 1 1 d . . . P1 P 0.96040(17) 0.43966(13) 0.18811(10) 0.0338(5) Uani 1 1 d . . . C7 C 1.0511(6) 0.3687(4) 0.2196(3) 0.0315(19) Uani 1 1 d . . . C8 C 1.1135(7) 0.3546(5) 0.1801(4) 0.040(2) Uani 1 1 d . . . H8 H 1.1077 0.3825 0.1387 0.048 Uiso 1 1 calc R . . C9 C 1.1850(7) 0.2996(5) 0.2009(4) 0.046(2) Uani 1 1 d . . . H9 H 1.2267 0.2904 0.1737 0.055 Uiso 1 1 calc R . . C10 C 1.1933(7) 0.2594(5) 0.2611(5) 0.056(3) Uani 1 1 d . . . H10 H 1.2413 0.2226 0.2752 0.067 Uiso 1 1 calc R . . C11 C 1.1327(8) 0.2717(6) 0.3015(4) 0.065(3) Uani 1 1 d . . . H11 H 1.1397 0.2435 0.3429 0.078 Uiso 1 1 calc R . . C12 C 1.0605(7) 0.3261(5) 0.2811(4) 0.052(3) Uani 1 1 d . . . H12 H 1.0186 0.3341 0.3084 0.063 Uiso 1 1 calc R . . C13 C 0.8935(6) 0.4021(5) 0.0960(4) 0.0320(19) Uani 1 1 d . . . C14 C 0.8414(7) 0.3135(5) 0.0780(4) 0.043(2) Uani 1 1 d . . . H14 H 0.8384 0.2762 0.1134 0.052 Uiso 1 1 calc R . . C15 C 0.7933(7) 0.2809(6) 0.0063(4) 0.046(2) Uani 1 1 d . . . H15 H 0.7584 0.2216 -0.0062 0.056 Uiso 1 1 calc R . . C16 C 0.7977(7) 0.3358(7) -0.0447(4) 0.054(3) Uani 1 1 d . . . H16 H 0.7657 0.3136 -0.0923 0.065 Uiso 1 1 calc R . . C17 C 0.8480(8) 0.4228(7) -0.0279(4) 0.063(3) Uani 1 1 d . . . H17 H 0.8508 0.4595 -0.0637 0.075 Uiso 1 1 calc R . . C18 C 0.8951(6) 0.4565(5) 0.0429(4) 0.047(2) Uani 1 1 d . . . H18 H 0.9280 0.5163 0.0546 0.056 Uiso 1 1 calc R . . C19 C 1.0293(7) 0.5532(5) 0.1979(3) 0.034(2) Uani 1 1 d . . . C20 C 0.9728(7) 0.6217(6) 0.1798(4) 0.053(3) Uani 1 1 d . . . H20 H 0.9008 0.6074 0.1630 0.064 Uiso 1 1 calc R . . C21 C 1.0220(10) 0.7085(6) 0.1865(4) 0.062(3) Uani 1 1 d . . . H21 H 0.9841 0.7533 0.1736 0.075 Uiso 1 1 calc R . . C22 C 1.1279(9) 0.7295(6) 0.2124(4) 0.060(3) Uani 1 1 d . . . H22 H 1.1613 0.7891 0.2173 0.072 Uiso 1 1 calc R . . C23 C 1.1860(8) 0.6655(6) 0.2313(4) 0.055(3) Uani 1 1 d . . . H23 H 1.2580 0.6807 0.2490 0.066 Uiso 1 1 calc R . . C24 C 1.1346(7) 0.5766(5) 0.2233(4) 0.042(2) Uani 1 1 d . . . H24 H 1.1732 0.5322 0.2357 0.051 Uiso 1 1 calc R . . C25 C 0.8713(7) 0.4345(5) 0.2372(4) 0.038(2) Uani 1 1 d . . . C26 C 0.9091(8) 0.4573(6) 0.3094(5) 0.062(3) Uani 1 1 d . . . H26 H 0.9802 0.4750 0.3318 0.074 Uiso 1 1 calc R . . C27 C 0.8428(11) 0.4543(7) 0.3495(5) 0.076(3) Uani 1 1 d . . . H27 H 0.8685 0.4702 0.3984 0.091 Uiso 1 1 calc R . . C28 C 0.7396(11) 0.4276(7) 0.3151(7) 0.089(4) Uani 1 1 d . . . H28 H 0.6949 0.4238 0.3417 0.106 Uiso 1 1 calc R . . C29 C 0.6987(9) 0.4061(7) 0.2438(6) 0.088(4) Uani 1 1 d . . . H29 H 0.6275 0.3888 0.2217 0.106 Uiso 1 1 calc R . . C30 C 0.7666(9) 0.4107(6) 0.2049(5) 0.070(3) Uani 1 1 d . . . H30 H 0.7401 0.3973 0.1558 0.084 Uiso 1 1 calc R . . P2 P 0.55878(19) 0.75937(14) 0.13822(10) 0.0408(6) Uani 1 1 d . . . C31 C 0.5667(7) 0.7634(5) 0.0499(4) 0.035(2) Uani 1 1 d . . . C32 C 0.4826(7) 0.7808(5) -0.0042(4) 0.054(3) Uani 1 1 d . . . H32 H 0.4283 0.7995 0.0065 0.065 Uiso 1 1 calc R . . C33 C 0.4806(8) 0.7698(6) -0.0741(4) 0.059(3) Uani 1 1 d . . . H33 H 0.4235 0.7793 -0.1107 0.070 Uiso 1 1 calc R . . C34 C 0.5615(9) 0.7454(6) -0.0899(4) 0.057(3) Uani 1 1 d . . . H34 H 0.5605 0.7391 -0.1368 0.068 Uiso 1 1 calc R . . C35 C 0.6442(8) 0.7302(5) -0.0356(5) 0.054(2) Uani 1 1 d . . . H35 H 0.6997 0.7138 -0.0462 0.065 Uiso 1 1 calc R . . C36 C 0.6471(7) 0.7388(5) 0.0343(4) 0.042(2) Uani 1 1 d . . . H36 H 0.7038 0.7279 0.0705 0.050 Uiso 1 1 calc R . . C37 C 0.6850(7) 0.7679(6) 0.2009(4) 0.046(2) Uani 1 1 d . . . C38 C 0.7552(8) 0.8471(7) 0.2158(4) 0.059(3) Uani 1 1 d . . . H38 H 0.7339 0.8967 0.1945 0.071 Uiso 1 1 calc R . . C40 C 0.8852(9) 0.7840(9) 0.2939(5) 0.081(4) Uani 1 1 d . . . H40 H 0.9512 0.7899 0.3268 0.097 Uiso 1 1 calc R . . C39 C 0.8561(9) 0.8575(7) 0.2608(5) 0.070(3) Uani 1 1 d . . . H39 H 0.9026 0.9118 0.2684 0.083 Uiso 1 1 calc R . . C41 C 0.8191(11) 0.7036(8) 0.2793(6) 0.086(4) Uani 1 1 d . . . H41 H 0.8411 0.6544 0.3009 0.104 Uiso 1 1 calc R . . C42 C 0.7192(8) 0.6940(7) 0.2324(5) 0.072(3) Uani 1 1 d . . . H42 H 0.6748 0.6382 0.2220 0.086 Uiso 1 1 calc R . . C43 C 0.4831(7) 0.6518(5) 0.1406(4) 0.041(2) Uani 1 1 d . . . C44 C 0.4434(7) 0.5909(6) 0.0811(4) 0.057(3) Uani 1 1 d . . . H44 H 0.4546 0.6063 0.0391 0.069 Uiso 1 1 calc R . . C46 C 0.3735(9) 0.4848(7) 0.1445(6) 0.080(3) Uani 1 1 d . . . H46 H 0.3353 0.4286 0.1455 0.096 Uiso 1 1 calc R . . C45 C 0.3870(9) 0.5072(6) 0.0828(5) 0.078(3) Uani 1 1 d . . . H45 H 0.3588 0.4670 0.0420 0.094 Uiso 1 1 calc R . . C47 C 0.4135(8) 0.5409(7) 0.2045(5) 0.069(3) Uani 1 1 d . . . H47 H 0.4045 0.5227 0.2466 0.083 Uiso 1 1 calc R . . C48 C 0.4672(8) 0.6247(6) 0.2037(4) 0.061(3) Uani 1 1 d . . . H48 H 0.4935 0.6641 0.2451 0.073 Uiso 1 1 calc R . . C49 C 0.5007(7) 0.8476(5) 0.1578(4) 0.043(2) Uani 1 1 d . . . C50 C 0.5107(8) 0.9271(6) 0.1254(4) 0.063(3) Uani 1 1 d . . . H50 H 0.5486 0.9344 0.0942 0.075 Uiso 1 1 calc R . . C51 C 0.4627(9) 0.9958(7) 0.1405(5) 0.079(4) Uani 1 1 d . . . H51 H 0.4665 1.0478 0.1179 0.094 Uiso 1 1 calc R . . C52 C 0.4102(9) 0.9860(8) 0.1889(6) 0.079(3) Uani 1 1 d . . . H52 H 0.3830 1.0333 0.2012 0.094 Uiso 1 1 calc R . . C53 C 0.3978(9) 0.9104(8) 0.2179(6) 0.078(3) Uani 1 1 d . . . H53 H 0.3576 0.9032 0.2477 0.094 Uiso 1 1 calc R . . C54 C 0.4443(8) 0.8420(7) 0.2042(5) 0.067(3) Uani 1 1 d . . . H54 H 0.4375 0.7904 0.2271 0.080 Uiso 1 1 calc R . . P3 P 0.26246(18) 0.91471(14) 0.57698(10) 0.0383(6) Uani 1 1 d . . . C55 C 0.3973(6) 0.9274(5) 0.5958(4) 0.037(2) Uani 1 1 d . . . C56 C 0.4446(8) 0.8558(6) 0.6155(4) 0.055(3) Uani 1 1 d . . . H56 H 0.4049 0.8013 0.6188 0.066 Uiso 1 1 calc R . . C57 C 0.5503(9) 0.8639(7) 0.6306(5) 0.069(3) Uani 1 1 d . . . H57 H 0.5809 0.8152 0.6448 0.083 Uiso 1 1 calc R . . C58 C 0.6101(8) 0.9423(8) 0.6248(5) 0.067(3) Uani 1 1 d . . . H58 H 0.6809 0.9471 0.6340 0.081 Uiso 1 1 calc R . . C59 C 0.5640(9) 1.0147(7) 0.6050(5) 0.070(3) Uani 1 1 d . . . H59 H 0.6044 1.0690 0.6020 0.084 Uiso 1 1 calc R . . C60 C 0.4579(8) 1.0072(6) 0.5897(4) 0.053(2) Uani 1 1 d . . . H60 H 0.4274 1.0559 0.5752 0.064 Uiso 1 1 calc R . . C61 C 0.2293(7) 0.9032(5) 0.6568(4) 0.040(2) Uani 1 1 d . . . C62 C 0.1302(8) 0.9085(6) 0.6554(4) 0.067(3) Uani 1 1 d . . . H62 H 0.0817 0.9170 0.6130 0.081 Uiso 1 1 calc R . . C63 C 0.1030(8) 0.9012(6) 0.7155(5) 0.063(3) Uani 1 1 d . . . H63 H 0.0360 0.9045 0.7138 0.075 Uiso 1 1 calc R . . C64 C 0.1723(10) 0.8892(7) 0.7769(5) 0.078(3) Uani 1 1 d . . . H64 H 0.1526 0.8812 0.8172 0.093 Uiso 1 1 calc R . . C65 C 0.2696(11) 0.8887(8) 0.7802(5) 0.101(4) Uani 1 1 d . . . H65 H 0.3183 0.8850 0.8239 0.121 Uiso 1 1 calc R . . C66 C 0.3010(8) 0.8935(7) 0.7198(5) 0.074(3) Uani 1 1 d . . . H66 H 0.3683 0.8901 0.7225 0.089 Uiso 1 1 calc R . . C67 C 0.2193(7) 1.0130(5) 0.5409(4) 0.042(2) Uani 1 1 d . . . C68 C 0.1752(7) 1.0148(6) 0.4676(4) 0.054(3) Uani 1 1 d . . . H68 H 0.1628 0.9636 0.4367 0.065 Uiso 1 1 calc R . . C69 C 0.1504(8) 1.0927(7) 0.4414(5) 0.072(3) Uani 1 1 d . . . H69 H 0.1213 1.0946 0.3927 0.087 Uiso 1 1 calc R . . C70 C 0.1689(9) 1.1674(7) 0.4877(6) 0.080(4) Uani 1 1 d . . . H70 H 0.1501 1.2195 0.4697 0.096 Uiso 1 1 calc R . . C71 C 0.2139(10) 1.1678(7) 0.5592(6) 0.091(4) Uani 1 1 d . . . H71 H 0.2261 1.2191 0.5900 0.109 Uiso 1 1 calc R . . C72 C 0.2411(9) 1.0886(7) 0.5848(5) 0.080(4) Uani 1 1 d . . . H72 H 0.2750 1.0881 0.6331 0.097 Uiso 1 1 calc R . . C73 C 0.1996(7) 0.8176(5) 0.5145(4) 0.036(2) Uani 1 1 d . . . C74 C 0.2378(7) 0.8031(6) 0.4580(4) 0.048(2) Uani 1 1 d . . . H74 H 0.2944 0.8431 0.4542 0.058 Uiso 1 1 calc R . . C75 C 0.1912(9) 0.7295(7) 0.4081(4) 0.069(3) Uani 1 1 d . . . H75 H 0.2166 0.7204 0.3709 0.083 Uiso 1 1 calc R . . C76 C 0.1092(9) 0.6707(8) 0.4130(5) 0.079(3) Uani 1 1 d . . . H76 H 0.0768 0.6226 0.3783 0.094 Uiso 1 1 calc R . . C77 C 0.0736(9) 0.6821(7) 0.4690(6) 0.087(3) Uani 1 1 d . . . H77 H 0.0200 0.6392 0.4737 0.104 Uiso 1 1 calc R . . C78 C 0.1160(8) 0.7562(7) 0.5186(5) 0.064(3) Uani 1 1 d . . . H78 H 0.0884 0.7648 0.5548 0.077 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 Re1 0.0261(2) 0.02717(18) 0.02619(15) 0.00622(13) 0.01196(14) 0.00796(15) Re2 0.0289(2) 0.02307(17) 0.02613(16) 0.00575(13) 0.01103(14) 0.00625(15) Re3 0.0283(2) 0.02661(18) 0.02254(15) 0.00531(13) 0.01004(14) 0.00719(15) S1 0.0293(14) 0.0315(12) 0.0344(10) 0.0041(9) 0.0076(9) 0.0037(10) S2 0.0376(14) 0.0316(11) 0.0321(10) 0.0011(8) 0.0152(9) 0.0099(10) S3 0.0351(14) 0.0316(11) 0.0322(10) 0.0106(9) 0.0094(9) 0.0140(10) S4 0.0374(14) 0.0341(12) 0.0321(10) 0.0116(9) 0.0191(9) 0.0060(10) C3 0.036(6) 0.037(5) 0.036(4) 0.002(4) 0.019(4) 0.010(4) C1 0.041(7) 0.035(5) 0.021(4) 0.003(3) 0.014(4) 0.008(4) C2 0.041(6) 0.036(5) 0.033(4) 0.012(4) 0.014(4) 0.016(5) N2 0.070(6) 0.040(5) 0.054(4) 0.016(4) 0.019(4) 0.010(4) N1 0.057(7) 0.073(6) 0.051(5) 0.014(4) 0.017(4) 0.011(5) N3 0.079(7) 0.083(6) 0.040(4) 0.004(4) 0.013(4) 0.024(5) Re4 0.0261(2) 0.02933(18) 0.02726(16) 0.00701(13) 0.01303(14) 0.00766(15) Re5 0.0295(2) 0.02819(18) 0.02443(15) 0.00536(13) 0.01284(14) 0.00818(15) Re6 0.0306(2) 0.02651(18) 0.02699(16) 0.00939(13) 0.01326(14) 0.00936(15) S5 0.0376(15) 0.0405(12) 0.0322(10) 0.0124(9) 0.0211(9) 0.0082(10) S6 0.0355(14) 0.0350(12) 0.0378(11) 0.0073(9) 0.0166(9) 0.0168(10) S7 0.0346(14) 0.0405(12) 0.0288(10) 0.0099(9) 0.0090(9) 0.0106(10) S8 0.0362(14) 0.0290(11) 0.0368(11) 0.0039(9) 0.0150(9) 0.0039(10) C4 0.044(7) 0.039(5) 0.038(5) 0.011(4) 0.020(5) 0.006(5) C5 0.026(5) 0.037(5) 0.041(5) 0.013(4) 0.015(4) 0.000(4) C6 0.022(5) 0.028(5) 0.039(4) 0.008(4) 0.013(4) 0.008(4) N6 0.083(7) 0.030(5) 0.085(6) 0.019(4) 0.031(5) 0.010(4) N4 0.054(7) 0.093(7) 0.066(5) 0.015(5) 0.033(5) 0.015(6) N5 0.065(6) 0.054(5) 0.056(5) 0.003(4) 0.030(4) 0.004(4) P1 0.0372(15) 0.0323(12) 0.0359(11) 0.0074(9) 0.0155(10) 0.0101(11) C7 0.037(6) 0.027(4) 0.025(4) 0.003(3) 0.005(4) 0.003(4) C8 0.053(7) 0.033(5) 0.037(4) 0.002(4) 0.018(4) 0.012(4) C9 0.041(6) 0.035(5) 0.059(6) 0.003(4) 0.010(4) 0.011(4) C10 0.045(7) 0.034(5) 0.077(7) 0.002(5) -0.001(5) 0.017(5) C11 0.080(9) 0.065(7) 0.048(6) 0.038(5) 0.009(5) 0.024(6) C12 0.073(8) 0.053(6) 0.039(5) 0.012(4) 0.023(5) 0.022(5) C13 0.030(6) 0.032(5) 0.037(4) 0.010(4) 0.012(4) 0.010(4) C14 0.048(7) 0.048(6) 0.043(5) 0.012(4) 0.022(4) 0.018(5) C15 0.049(7) 0.040(5) 0.061(6) 0.002(5) 0.028(5) 0.017(5) C16 0.047(7) 0.064(7) 0.045(5) -0.006(5) 0.010(5) 0.005(5) C17 0.072(8) 0.079(8) 0.037(5) 0.016(5) 0.021(5) 0.007(6) C18 0.041(6) 0.044(5) 0.046(5) 0.007(4) 0.005(4) 0.001(4) C19 0.036(6) 0.038(5) 0.028(4) 0.010(3) 0.008(4) 0.006(4) C20 0.059(7) 0.045(6) 0.052(5) 0.008(4) 0.008(5) 0.018(5) C21 0.103(10) 0.030(6) 0.061(6) 0.013(5) 0.030(6) 0.027(6) C22 0.092(9) 0.041(6) 0.032(5) 0.001(4) 0.012(5) -0.008(6) C23 0.062(8) 0.051(6) 0.042(5) 0.000(4) 0.013(5) -0.010(6) C24 0.053(7) 0.035(5) 0.036(4) 0.006(4) 0.010(4) 0.009(5) C25 0.033(6) 0.032(5) 0.052(5) 0.001(4) 0.018(4) 0.008(4) C26 0.060(8) 0.063(7) 0.065(6) -0.013(5) 0.036(5) -0.004(5) C27 0.104(11) 0.081(8) 0.054(6) -0.010(5) 0.046(7) 0.014(8) C28 0.096(12) 0.079(9) 0.118(11) -0.011(7) 0.077(9) 0.016(8) C29 0.045(8) 0.109(10) 0.111(9) -0.029(7) 0.043(7) -0.006(7) C30 0.064(9) 0.087(8) 0.067(6) -0.014(5) 0.038(6) 0.011(6) P2 0.0475(17) 0.0426(14) 0.0375(12) 0.0106(10) 0.0204(11) 0.0090(12) C31 0.047(6) 0.026(4) 0.039(4) 0.009(4) 0.024(4) 0.006(4) C32 0.054(7) 0.059(6) 0.064(6) 0.024(5) 0.032(5) 0.022(5) C33 0.056(8) 0.069(7) 0.043(5) 0.008(5) 0.008(5) 0.007(6) C34 0.080(9) 0.057(6) 0.045(5) 0.011(5) 0.040(6) 0.006(6) C35 0.056(7) 0.046(6) 0.070(6) 0.009(5) 0.036(5) 0.007(5) C36 0.047(7) 0.034(5) 0.046(5) 0.012(4) 0.020(4) 0.002(4) C37 0.056(7) 0.048(6) 0.041(5) -0.001(4) 0.029(4) 0.008(5) C38 0.057(8) 0.071(7) 0.051(6) -0.004(5) 0.019(5) 0.018(6) C40 0.059(9) 0.108(10) 0.065(7) -0.010(7) 0.001(6) 0.027(8) C39 0.065(9) 0.081(8) 0.055(6) -0.013(6) 0.019(6) 0.003(7) C41 0.089(11) 0.075(9) 0.093(8) 0.020(7) 0.008(7) 0.049(8) C42 0.065(9) 0.063(7) 0.081(7) 0.024(6) 0.010(6) 0.018(6) C43 0.051(7) 0.033(5) 0.042(5) 0.010(4) 0.018(4) 0.011(4) C44 0.082(8) 0.054(6) 0.046(5) 0.007(5) 0.035(5) 0.015(6) C46 0.105(11) 0.054(7) 0.090(8) 0.045(6) 0.046(7) 0.004(6) C45 0.107(10) 0.033(6) 0.083(7) 0.011(5) 0.030(7) -0.012(6) C47 0.091(10) 0.072(8) 0.057(6) 0.035(6) 0.039(6) 0.017(7) C48 0.086(9) 0.064(7) 0.047(5) 0.025(5) 0.040(5) 0.017(6) C49 0.048(7) 0.040(5) 0.039(5) 0.005(4) 0.013(4) 0.005(4) C50 0.090(9) 0.046(6) 0.056(6) 0.014(5) 0.028(5) 0.014(6) C51 0.108(11) 0.048(7) 0.073(7) 0.013(6) 0.009(7) 0.034(7) C52 0.070(9) 0.076(9) 0.087(8) -0.017(7) 0.017(7) 0.029(7) C53 0.075(9) 0.073(8) 0.098(8) -0.005(7) 0.044(7) 0.017(7) C54 0.078(9) 0.060(7) 0.080(7) 0.020(5) 0.045(6) 0.024(6) P3 0.0429(16) 0.0425(14) 0.0360(11) 0.0067(10) 0.0204(10) 0.0107(12) C55 0.037(6) 0.040(5) 0.038(4) -0.004(4) 0.017(4) 0.006(4) C56 0.055(8) 0.035(5) 0.083(7) 0.003(5) 0.036(5) 0.007(5) C57 0.043(8) 0.060(7) 0.110(8) -0.004(6) 0.032(6) 0.013(6) C58 0.046(8) 0.094(9) 0.068(6) 0.004(6) 0.025(5) 0.017(7) C59 0.056(9) 0.068(8) 0.081(7) -0.003(6) 0.030(6) -0.012(6) C60 0.060(8) 0.047(6) 0.054(5) 0.017(4) 0.024(5) 0.004(5) C61 0.041(6) 0.050(5) 0.029(4) 0.000(4) 0.016(4) 0.002(5) C62 0.063(9) 0.107(8) 0.044(5) 0.014(5) 0.030(5) 0.023(7) C63 0.062(8) 0.091(8) 0.048(6) 0.009(5) 0.035(5) 0.019(6) C64 0.063(9) 0.122(10) 0.062(7) 0.014(6) 0.046(6) 0.003(7) C65 0.114(13) 0.161(12) 0.033(6) 0.033(6) 0.023(7) 0.035(10) C66 0.067(9) 0.114(9) 0.058(6) 0.028(6) 0.028(6) 0.042(7) C67 0.056(7) 0.041(5) 0.041(5) 0.002(4) 0.032(4) 0.007(5) C68 0.056(7) 0.053(6) 0.051(5) 0.004(5) 0.013(5) 0.012(5) C69 0.089(9) 0.080(8) 0.063(6) 0.034(6) 0.031(6) 0.038(7) C70 0.109(11) 0.070(8) 0.108(9) 0.049(7) 0.076(8) 0.056(7) C71 0.180(14) 0.048(7) 0.085(8) 0.016(6) 0.088(8) 0.041(8) C72 0.145(12) 0.060(7) 0.053(6) 0.008(5) 0.040(6) 0.048(7) C73 0.040(6) 0.038(5) 0.036(4) 0.011(4) 0.013(4) 0.015(4) C74 0.044(7) 0.056(6) 0.043(5) 0.003(4) 0.017(4) 0.002(5) C75 0.073(9) 0.093(9) 0.036(5) -0.011(5) 0.015(5) 0.015(7) C76 0.064(9) 0.090(9) 0.065(7) -0.037(6) 0.008(6) 0.004(7) C77 0.071(9) 0.073(8) 0.104(9) -0.021(7) 0.034(7) -0.021(6) C78 0.058(8) 0.071(7) 0.065(6) -0.004(5) 0.034(5) -0.006(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 Re1 C1 2.156(9) . ? Re1 S3 2.4116(18) . ? Re1 S4 2.4143(17) . ? Re1 S1 2.4150(19) . ? Re1 S2 2.419(2) . ? Re1 Re2 2.5993(5) . ? Re1 Re2 2.6013(5) 2_755 ? Re1 Re3 2.6042(5) . ? Re1 Re3 2.6125(5) 2_755 ? Re2 C2 2.135(8) . ? Re2 S2 2.4025(19) . ? Re2 S4 2.4059(18) 2_755 ? Re2 S3 2.4173(19) . ? Re2 S1 2.4197(19) 2_755 ? Re2 Re1 2.6013(5) 2_755 ? Re2 Re3 2.6056(6) 2_755 ? Re2 Re3 2.6141(5) . ? Re3 C3 2.164(7) . ? Re3 S1 2.404(2) 2_755 ? Re3 S2 2.4067(19) . ? Re3 S3 2.4079(19) 2_755 ? Re3 S4 2.410(2) . ? Re3 Re2 2.6056(6) 2_755 ? Re3 Re1 2.6125(5) 2_755 ? S1 Re3 2.404(2) 2_755 ? S1 Re2 2.4196(19) 2_755 ? S3 Re3 2.4080(19) 2_755 ? S4 Re2 2.4059(18) 2_755 ? C3 N3 1.066(7) . ? C1 N1 1.053(9) . ? C2 N2 1.083(8) . ? Re4 C4 2.152(10) . ? Re4 S7 2.3939(17) . ? Re4 S5 2.4007(17) . ? Re4 S6 2.4086(19) . ? Re4 S8 2.4099(19) . ? Re4 Re5 2.6067(6) 2_666 ? Re4 Re6 2.6077(5) . ? Re4 Re5 2.6089(5) . ? Re4 Re6 2.6097(5) 2_666 ? Re5 C5 2.116(8) . ? Re5 S6 2.4128(19) 2_666 ? Re5 S7 2.418(2) . ? Re5 S5 2.419(2) 2_666 ? Re5 S8 2.420(2) . ? Re5 Re6 2.5978(5) . ? Re5 Re6 2.5983(4) 2_666 ? Re5 Re4 2.6066(6) 2_666 ? Re6 C6 2.178(7) . ? Re6 S5 2.408(2) 2_666 ? Re6 S8 2.410(2) 2_666 ? Re6 S6 2.411(2) . ? Re6 S7 2.419(2) . ? Re6 Re5 2.5984(4) 2_666 ? Re6 Re4 2.6098(5) 2_666 ? S5 Re6 2.4084(19) 2_666 ? S5 Re5 2.419(2) 2_666 ? S6 Re5 2.4128(19) 2_666 ? S8 Re6 2.410(2) 2_666 ? C4 N4 1.055(10) . ? C5 N5 1.100(8) . ? C6 N6 1.019(7) . ? P1 C7 1.787(7) . ? P1 C13 1.791(7) . ? P1 C25 1.793(8) . ? P1 C19 1.795(8) . ? C7 C8 1.375(10) . ? C7 C12 1.389(9) . ? C8 C9 1.388(10) . ? C9 C10 1.350(10) . ? C10 C11 1.363(12) . ? C11 C12 1.387(11) . ? C13 C18 1.372(9) . ? C13 C14 1.388(10) . ? C14 C15 1.399(10) . ? C15 C16 1.351(10) . ? C16 C17 1.360(11) . ? C17 C18 1.387(10) . ? C19 C24 1.362(10) . ? C19 C20 1.407(10) . ? C20 C21 1.358(11) . ? C21 C22 1.368(12) . ? C22 C23 1.366(11) . ? C23 C24 1.392(11) . ? C25 C30 1.365(12) . ? C25 C26 1.371(10) . ? C26 C27 1.391(13) . ? C27 C28 1.357(14) . ? C28 C29 1.353(13) . ? C29 C30 1.389(13) . ? P2 C49 1.774(8) . ? P2 C37 1.782(9) . ? P2 C43 1.795(8) . ? P2 C31 1.798(7) . ? C31 C36 1.356(10) . ? C31 C32 1.390(10) . ? C32 C33 1.386(10) . ? C33 C34 1.362(12) . ? C34 C35 1.369(11) . ? C35 C36 1.380(10) . ? C37 C38 1.368(12) . ? C37 C42 1.396(10) . ? C38 C39 1.382(12) . ? C40 C41 1.355(14) . ? C40 C39 1.381(13) . ? C41 C42 1.385(13) . ? C43 C44 1.373(9) . ? C43 C48 1.407(10) . ? C44 C45 1.382(12) . ? C46 C47 1.340(12) . ? C46 C45 1.347(12) . ? C47 C48 1.365(12) . ? C49 C54 1.382(12) . ? C49 C50 1.402(10) . ? C50 C51 1.406(12) . ? C51 C52 1.375(14) . ? C52 C53 1.319(13) . ? C53 C54 1.379(12) . ? P3 C55 1.761(8) . ? P3 C73 1.793(8) . ? P3 C61 1.794(7) . ? P3 C67 1.805(8) . ? C55 C56 1.380(10) . ? C55 C60 1.385(11) . ? C56 C57 1.383(12) . ? C57 C58 1.360(13) . ? C58 C59 1.383(12) . ? C59 C60 1.388(12) . ? C61 C66 1.366(10) . ? C61 C62 1.382(12) . ? C62 C63 1.366(11) . ? C63 C64 1.340(12) . ? C64 C65 1.332(14) . ? C65 C66 1.400(13) . ? C67 C72 1.345(10) . ? C67 C68 1.397(9) . ? C68 C69 1.372(11) . ? C69 C70 1.369(12) . ? C70 C71 1.362(13) . ? C71 C72 1.398(11) . ? C73 C78 1.382(11) . ? C73 C74 1.410(10) . ? C74 C75 1.382(11) . ? C75 C76 1.350(13) . ? C76 C77 1.370(13) . ? C77 C78 1.381(12) . ? 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 C1 Re1 S3 95.12(19) . . ? C1 Re1 S4 91.34(19) . . ? S3 Re1 S4 173.54(7) . . ? C1 Re1 S1 95.7(2) . . ? S3 Re1 S1 89.05(6) . . ? S4 Re1 S1 90.05(6) . . ? C1 Re1 S2 91.3(2) . . ? S3 Re1 S2 89.99(6) . . ? S4 Re1 S2 90.13(6) . . ? S1 Re1 S2 173.02(7) . . ? C1 Re1 Re2 134.6(2) . . ? S3 Re1 Re2 57.54(5) . . ? S4 Re1 Re2 117.51(5) . . ? S1 Re1 Re2 116.93(5) . . ? S2 Re1 Re2 57.08(5) . . ? C1 Re1 Re2 135.1(2) . 2_755 ? S3 Re1 Re2 117.26(5) . 2_755 ? S4 Re1 Re2 57.18(5) . 2_755 ? S1 Re1 Re2 57.53(5) . 2_755 ? S2 Re1 Re2 117.13(5) . 2_755 ? Re2 Re1 Re2 90.063(15) . 2_755 ? C1 Re1 Re3 131.73(18) . . ? S3 Re1 Re3 117.82(5) . . ? S4 Re1 Re3 57.24(5) . . ? S1 Re1 Re3 117.56(5) . . ? S2 Re1 Re3 57.12(5) . . ? Re2 Re1 Re3 60.313(14) . . ? Re2 Re1 Re3 60.071(15) 2_755 . ? C1 Re1 Re3 137.85(18) . 2_755 ? S3 Re1 Re3 57.11(5) . 2_755 ? S4 Re1 Re3 117.34(5) . 2_755 ? S1 Re1 Re3 56.97(5) . 2_755 ? S2 Re1 Re3 117.03(5) . 2_755 ? Re2 Re1 Re3 59.991(15) . 2_755 ? Re2 Re1 Re3 60.180(13) 2_755 2_755 ? Re3 Re1 Re3 90.418(16) . 2_755 ? C2 Re2 S2 94.2(2) . . ? C2 Re2 S4 91.9(2) . 2_755 ? S2 Re2 S4 173.83(7) . 2_755 ? C2 Re2 S3 91.8(2) . . ? S2 Re2 S3 90.24(7) . . ? S4 Re2 S3 89.79(7) 2_755 . ? C2 Re2 S1 95.2(2) . 2_755 ? S2 Re2 S1 89.08(6) . 2_755 ? S4 Re2 S1 90.14(6) 2_755 2_755 ? S3 Re2 S1 173.00(7) . 2_755 ? C2 Re2 Re1 134.6(2) . . ? S2 Re2 Re1 57.68(5) . . ? S4 Re2 Re1 117.53(5) 2_755 . ? S3 Re2 Re1 57.33(5) . . ? S1 Re2 Re1 116.80(5) 2_755 . ? C2 Re2 Re1 135.4(2) . 2_755 ? S2 Re2 Re1 117.25(5) . 2_755 ? S4 Re2 Re1 57.50(4) 2_755 2_755 ? S3 Re2 Re1 117.11(5) . 2_755 ? S1 Re2 Re1 57.36(5) 2_755 2_755 ? Re1 Re2 Re1 89.935(15) . 2_755 ? C2 Re2 Re3 132.80(18) . 2_755 ? S2 Re2 Re3 117.90(5) . 2_755 ? S4 Re2 Re3 57.32(5) 2_755 2_755 ? S3 Re2 Re3 57.15(5) . 2_755 ? S1 Re2 Re3 117.34(5) 2_755 2_755 ? Re1 Re2 Re3 60.256(14) . 2_755 ? Re1 Re2 Re3 60.019(14) 2_755 2_755 ? C2 Re2 Re3 136.85(18) . . ? S2 Re2 Re3 57.15(4) . . ? S4 Re2 Re3 117.59(5) 2_755 . ? S3 Re2 Re3 117.23(5) . . ? S1 Re2 Re3 56.90(5) 2_755 . ? Re1 Re2 Re3 59.936(14) . . ? Re1 Re2 Re3 60.123(13) 2_755 . ? Re3 Re2 Re3 90.353(15) 2_755 . ? C3 Re3 S1 95.5(2) . 2_755 ? C3 Re3 S2 93.29(19) . . ? S1 Re3 S2 89.35(7) 2_755 . ? C3 Re3 S3 93.58(19) . 2_755 ? S1 Re3 S3 89.39(7) 2_755 2_755 ? S2 Re3 S3 173.11(6) . 2_755 ? C3 Re3 S4 91.3(2) . . ? S1 Re3 S4 173.18(6) 2_755 . ? S2 Re3 S4 90.52(7) . . ? S3 Re3 S4 89.92(7) 2_755 . ? C3 Re3 Re1 133.5(2) . . ? S1 Re3 Re1 117.19(4) 2_755 . ? S2 Re3 Re1 57.56(5) . . ? S3 Re3 Re1 117.35(5) 2_755 . ? S4 Re3 Re1 57.41(4) . . ? C3 Re3 Re2 133.7(2) . 2_755 ? S1 Re3 Re2 117.10(5) 2_755 2_755 ? S2 Re3 Re2 117.41(5) . 2_755 ? S3 Re3 Re2 57.49(5) 2_755 2_755 ? S4 Re3 Re2 57.17(4) . 2_755 ? Re1 Re3 Re2 59.910(14) . 2_755 ? C3 Re3 Re1 136.9(2) . 2_755 ? S1 Re3 Re1 57.37(5) 2_755 2_755 ? S2 Re3 Re1 116.67(5) . 2_755 ? S3 Re3 Re1 57.24(4) 2_755 2_755 ? S4 Re3 Re1 116.88(5) . 2_755 ? Re1 Re3 Re1 89.581(15) . 2_755 ? Re2 Re3 Re1 59.751(14) 2_755 2_755 ? C3 Re3 Re2 136.6(2) . . ? S1 Re3 Re2 57.48(4) 2_755 . ? S2 Re3 Re2 57.00(4) . . ? S3 Re3 Re2 116.91(4) 2_755 . ? S4 Re3 Re2 117.11(4) . . ? Re1 Re3 Re2 59.751(14) . . ? Re2 Re3 Re2 89.646(15) 2_755 . ? Re1 Re3 Re2 59.696(12) 2_755 . ? Re3 S1 Re1 65.66(5) 2_755 . ? Re3 S1 Re2 65.63(5) 2_755 2_755 ? Re1 S1 Re2 65.10(5) . 2_755 ? Re2 S2 Re3 65.85(5) . . ? Re2 S2 Re1 65.25(5) . . ? Re3 S2 Re1 65.32(5) . . ? Re3 S3 Re1 65.65(5) 2_755 . ? Re3 S3 Re2 65.36(5) 2_755 . ? Re1 S3 Re2 65.13(4) . . ? Re2 S4 Re3 65.51(5) 2_755 . ? Re2 S4 Re1 65.32(4) 2_755 . ? Re3 S4 Re1 65.34(5) . . ? N3 C3 Re3 173.4(8) . . ? N1 C1 Re1 171.8(9) . . ? N2 C2 Re2 176.8(8) . . ? C4 Re4 S7 93.2(2) . . ? C4 Re4 S5 93.2(2) . . ? S7 Re4 S5 173.61(7) . . ? C4 Re4 S6 92.4(2) . . ? S7 Re4 S6 89.85(6) . . ? S5 Re4 S6 90.12(6) . . ? C4 Re4 S8 94.4(2) . . ? S7 Re4 S8 89.95(6) . . ? S5 Re4 S8 89.32(6) . . ? S6 Re4 S8 173.12(7) . . ? C4 Re4 Re5 134.4(2) . 2_666 ? S7 Re4 Re5 117.40(5) . 2_666 ? S5 Re4 Re5 57.59(5) . 2_666 ? S6 Re4 Re5 57.35(5) . 2_666 ? S8 Re4 Re5 116.93(5) . 2_666 ? C4 Re4 Re6 134.5(2) . . ? S7 Re4 Re6 57.65(5) . . ? S5 Re4 Re6 117.32(5) . . ? S6 Re4 Re6 57.29(5) . . ? S8 Re4 Re6 117.18(5) . . ? Re5 Re4 Re6 59.777(14) 2_666 . ? C4 Re4 Re5 136.1(2) . . ? S7 Re4 Re5 57.61(5) . . ? S5 Re4 Re5 116.97(5) . . ? S6 Re4 Re5 116.98(5) . . ? S8 Re4 Re5 57.49(5) . . ? Re5 Re4 Re5 89.533(15) 2_666 . ? Re6 Re4 Re5 59.735(14) . . ? C4 Re4 Re6 135.9(2) . 2_666 ? S7 Re4 Re6 117.30(5) . 2_666 ? S5 Re4 Re6 57.28(5) . 2_666 ? S6 Re4 Re6 117.04(5) . 2_666 ? S8 Re4 Re6 57.23(5) . 2_666 ? Re5 Re4 Re6 59.735(14) 2_666 2_666 ? Re6 Re4 Re6 89.575(16) . 2_666 ? Re5 Re4 Re6 59.722(13) . 2_666 ? C5 Re5 S6 92.6(2) . 2_666 ? C5 Re5 S7 94.1(2) . . ? S6 Re5 S7 173.29(6) 2_666 . ? C5 Re5 S5 92.3(2) . 2_666 ? S6 Re5 S5 89.60(7) 2_666 2_666 ? S7 Re5 S5 90.55(7) . 2_666 ? C5 Re5 S8 94.6(2) . . ? S6 Re5 S8 89.89(7) 2_666 . ? S7 Re5 S8 89.16(7) . . ? S5 Re5 S8 173.09(6) 2_666 . ? C5 Re5 Re6 134.54(19) . . ? S6 Re5 Re6 117.35(5) 2_666 . ? S7 Re5 Re6 57.53(5) . . ? S5 Re5 Re6 57.25(5) 2_666 . ? S8 Re5 Re6 117.19(5) . . ? C5 Re5 Re6 135.38(19) . 2_666 ? S6 Re5 Re6 57.38(5) 2_666 2_666 ? S7 Re5 Re6 116.85(4) . 2_666 ? S5 Re5 Re6 117.01(5) 2_666 2_666 ? S8 Re5 Re6 57.28(5) . 2_666 ? Re6 Re5 Re6 90.042(17) . 2_666 ? C5 Re5 Re4 133.4(2) . 2_666 ? S6 Re5 Re4 57.20(5) 2_666 2_666 ? S7 Re5 Re4 117.67(5) . 2_666 ? S5 Re5 Re4 56.92(4) 2_666 2_666 ? S8 Re5 Re4 117.38(5) . 2_666 ? Re6 Re5 Re4 60.191(15) . 2_666 ? Re6 Re5 Re4 60.132(15) 2_666 2_666 ? C5 Re5 Re4 136.1(2) . . ? S6 Re5 Re4 117.50(5) 2_666 . ? S7 Re5 Re4 56.73(4) . . ? S5 Re5 Re4 117.32(5) 2_666 . ? S8 Re5 Re4 57.12(5) . . ? Re6 Re5 Re4 60.110(14) . . ? Re6 Re5 Re4 60.155(13) 2_666 . ? Re4 Re5 Re4 90.467(16) 2_666 . ? C6 Re6 S5 91.35(19) . 2_666 ? C6 Re6 S8 93.50(19) . 2_666 ? S5 Re6 S8 89.13(7) 2_666 2_666 ? C6 Re6 S6 95.11(19) . . ? S5 Re6 S6 173.53(6) 2_666 . ? S8 Re6 S6 90.16(7) 2_666 . ? C6 Re6 S7 93.16(19) . . ? S5 Re6 S7 90.77(7) 2_666 . ? S8 Re6 S7 173.34(6) 2_666 . ? S6 Re6 S7 89.20(7) . . ? C6 Re6 Re5 133.41(18) . . ? S5 Re6 Re5 57.63(5) 2_666 . ? S8 Re6 Re5 117.25(5) 2_666 . ? S6 Re6 Re5 117.31(5) . . ? S7 Re6 Re5 57.49(5) . . ? C6 Re6 Re5 136.61(18) . 2_666 ? S5 Re6 Re5 117.08(4) 2_666 2_666 ? S8 Re6 Re5 57.63(5) 2_666 2_666 ? S6 Re6 Re5 57.44(4) . 2_666 ? S7 Re6 Re5 116.79(5) . 2_666 ? Re5 Re6 Re5 89.956(16) . 2_666 ? C6 Re6 Re4 135.8(2) . . ? S5 Re6 Re4 117.75(5) 2_666 . ? S8 Re6 Re4 117.69(5) 2_666 . ? S6 Re6 Re4 57.20(5) . . ? S7 Re6 Re4 56.73(4) . . ? Re5 Re6 Re4 60.155(14) . . ? Re5 Re6 Re4 60.092(16) 2_666 . ? C6 Re6 Re4 133.7(2) . 2_666 ? S5 Re6 Re4 56.99(4) 2_666 2_666 ? S8 Re6 Re4 57.21(5) 2_666 2_666 ? S6 Re6 Re4 117.53(4) . 2_666 ? S7 Re6 Re4 117.51(5) . 2_666 ? Re5 Re6 Re4 60.072(15) . 2_666 ? Re5 Re6 Re4 60.121(14) 2_666 2_666 ? Re4 Re6 Re4 90.424(15) . 2_666 ? Re4 S5 Re6 65.73(5) . 2_666 ? Re4 S5 Re5 65.48(5) . 2_666 ? Re6 S5 Re5 65.12(5) 2_666 2_666 ? Re4 S6 Re6 65.51(5) . . ? Re4 S6 Re5 65.46(5) . 2_666 ? Re6 S6 Re5 65.19(5) . 2_666 ? Re4 S7 Re5 65.67(5) . . ? Re4 S7 Re6 65.61(5) . . ? Re5 S7 Re6 64.98(5) . . ? Re4 S8 Re6 65.56(5) . 2_666 ? Re4 S8 Re5 65.39(5) . . ? Re6 S8 Re5 65.08(5) 2_666 . ? N4 C4 Re4 178.1(8) . . ? N5 C5 Re5 177.9(7) . . ? N6 C6 Re6 175.1(8) . . ? C7 P1 C13 106.5(3) . . ? C7 P1 C25 111.5(3) . . ? C13 P1 C25 110.9(4) . . ? C7 P1 C19 109.2(4) . . ? C13 P1 C19 110.3(3) . . ? C25 P1 C19 108.5(4) . . ? C8 C7 C12 118.6(7) . . ? C8 C7 P1 118.0(5) . . ? C12 C7 P1 123.4(6) . . ? C7 C8 C9 121.2(7) . . ? C10 C9 C8 119.1(8) . . ? C9 C10 C11 121.3(8) . . ? C10 C11 C12 120.1(8) . . ? C11 C12 C7 119.6(8) . . ? C18 C13 C14 119.2(7) . . ? C18 C13 P1 122.5(6) . . ? C14 C13 P1 118.3(5) . . ? C13 C14 C15 119.6(7) . . ? C16 C15 C14 119.8(8) . . ? C15 C16 C17 121.4(8) . . ? C16 C17 C18 119.6(8) . . ? C13 C18 C17 120.5(8) . . ? C24 C19 C20 118.1(8) . . ? C24 C19 P1 122.8(6) . . ? C20 C19 P1 119.1(7) . . ? C21 C20 C19 120.9(9) . . ? C20 C21 C22 119.4(9) . . ? C23 C22 C21 121.9(9) . . ? C22 C23 C24 118.2(9) . . ? C19 C24 C23 121.6(8) . . ? C30 C25 C26 118.6(8) . . ? C30 C25 P1 122.3(7) . . ? C26 C25 P1 119.1(7) . . ? C25 C26 C27 121.1(10) . . ? C28 C27 C26 117.9(10) . . ? C29 C28 C27 123.1(11) . . ? C28 C29 C30 117.8(10) . . ? C25 C30 C29 121.5(9) . . ? C49 P2 C37 110.7(4) . . ? C49 P2 C43 111.4(4) . . ? C37 P2 C43 108.0(4) . . ? C49 P2 C31 109.6(3) . . ? C37 P2 C31 109.8(4) . . ? C43 P2 C31 107.2(4) . . ? C36 C31 C32 120.2(7) . . ? C36 C31 P2 120.5(6) . . ? C32 C31 P2 118.7(7) . . ? C33 C32 C31 119.2(8) . . ? C34 C33 C32 120.7(8) . . ? C33 C34 C35 119.0(8) . . ? C34 C35 C36 121.5(9) . . ? C31 C36 C35 119.4(8) . . ? C38 C37 C42 117.3(9) . . ? C38 C37 P2 120.2(7) . . ? C42 C37 P2 122.3(8) . . ? C37 C38 C39 123.5(10) . . ? C41 C40 C39 121.1(10) . . ? C40 C39 C38 117.4(10) . . ? C40 C41 C42 120.5(10) . . ? C41 C42 C37 120.1(10) . . ? C44 C43 C48 117.6(8) . . ? C44 C43 P2 120.6(6) . . ? C48 C43 P2 121.8(7) . . ? C43 C44 C45 121.1(8) . . ? C47 C46 C45 122.2(10) . . ? C46 C45 C44 119.0(9) . . ? C46 C47 C48 119.9(8) . . ? C47 C48 C43 120.3(9) . . ? C54 C49 C50 117.1(8) . . ? C54 C49 P2 122.8(7) . . ? C50 C49 P2 120.1(7) . . ? C49 C50 C51 119.4(9) . . ? C52 C51 C50 119.9(10) . . ? C53 C52 C51 121.0(10) . . ? C52 C53 C54 120.2(11) . . ? C53 C54 C49 122.2(9) . . ? C55 P3 C73 108.5(4) . . ? C55 P3 C61 110.6(4) . . ? C73 P3 C61 110.4(4) . . ? C55 P3 C67 110.3(4) . . ? C73 P3 C67 110.4(3) . . ? C61 P3 C67 106.7(4) . . ? C56 C55 C60 118.3(9) . . ? C56 C55 P3 119.9(7) . . ? C60 C55 P3 121.8(7) . . ? C55 C56 C57 121.0(9) . . ? C58 C57 C56 120.8(10) . . ? C57 C58 C59 119.0(11) . . ? C58 C59 C60 120.7(10) . . ? C55 C60 C59 120.2(9) . . ? C66 C61 C62 119.2(8) . . ? C66 C61 P3 121.6(7) . . ? C62 C61 P3 119.2(6) . . ? C63 C62 C61 120.6(9) . . ? C64 C63 C62 120.3(10) . . ? C65 C64 C63 119.8(9) . . ? C64 C65 C66 122.1(10) . . ? C61 C66 C65 117.8(10) . . ? C72 C67 C68 119.6(8) . . ? C72 C67 P3 119.0(6) . . ? C68 C67 P3 121.0(6) . . ? C69 C68 C67 119.7(8) . . ? C70 C69 C68 119.3(9) . . ? C71 C70 C69 122.1(9) . . ? C70 C71 C72 117.8(9) . . ? C67 C72 C71 121.4(9) . . ? C78 C73 C74 118.2(8) . . ? C78 C73 P3 123.7(6) . . ? C74 C73 P3 118.0(7) . . ? C75 C74 C73 120.1(9) . . ? C76 C75 C74 120.7(9) . . ? C75 C76 C77 120.0(10) . . ? C76 C77 C78 121.0(11) . . ? C77 C78 C73 119.9(9) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 26.79 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.707 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.162 #################### Material relevant to compound 2 at 250K ############ data_sb250k _database_code_CSD 186994 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H60 N6 P3 Re6 S8' _chemical_formula_weight 2547.91 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' 'P' 'P' 0.1023 0.0942 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8680(16) _cell_length_b 15.1960(16) _cell_length_c 19.842(2) _cell_angle_alpha 92.538(13) _cell_angle_beta 108.475(13) _cell_angle_gamma 100.220(13) _cell_volume 3880.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2310 _exptl_crystal_size_mid 0.1924 _exptl_crystal_size_min 0.1887 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2386 _exptl_absorpt_coefficient_mu 9.645 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1592 _exptl_absorpt_correction_T_max 0.2744 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, Phi. incr. == 1.2' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39108 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.95 _reflns_number_total 14093 _reflns_number_gt 10113 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0388P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14093 _refine_ls_number_parameters 910 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _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 0.87533(3) 0.01531(2) 0.007926(19) 0.02073(9) Uani 1 1 d . . . Re2 Re 1.04222(3) 0.12251(2) 0.005071(19) 0.02079(9) Uani 1 1 d . . . Re3 Re 1.05524(3) 0.00538(2) 0.098468(19) 0.02076(9) Uani 1 1 d . . . S1 S 0.79452(18) -0.10394(16) -0.08908(13) 0.0277(5) Uani 1 1 d . . . S2 S 0.97643(19) 0.13277(16) 0.10256(13) 0.0271(5) Uani 1 1 d . . . S3 S 0.87187(18) 0.12119(16) -0.07889(12) 0.0260(5) Uani 1 1 d . . . S4 S 0.89632(18) -0.09410(16) 0.09235(12) 0.0264(5) Uani 1 1 d . . . C3 C 1.1128(8) 0.0069(7) 0.2126(6) 0.034(2) Uani 1 1 d . . . C1 C 0.7374(8) 0.0361(7) 0.0252(5) 0.030(2) Uani 1 1 d . . . C2 C 1.0881(7) 0.2636(7) 0.0086(5) 0.028(2) Uani 1 1 d . . . N2 N 1.1159(8) 0.3389(6) 0.0101(5) 0.050(3) Uani 1 1 d . . . N1 N 0.6666(7) 0.0498(7) 0.0367(5) 0.047(3) Uani 1 1 d . . . N3 N 1.1359(8) 0.0059(8) 0.2711(5) 0.055(3) Uani 1 1 d . . . Re4 Re 0.35914(3) 0.46497(2) 0.485794(19) 0.02149(9) Uani 1 1 d . . . Re5 Re 0.48227(3) 0.43533(2) 0.415365(19) 0.02144(9) Uani 1 1 d . . . Re6 Re 0.47560(3) 0.59923(2) 0.452750(19) 0.02184(9) Uani 1 1 d . . . S5 S 0.40881(19) 0.43507(16) 0.60817(13) 0.0280(5) Uani 1 1 d . . . S6 S 0.36482(19) 0.61959(17) 0.52173(13) 0.0296(6) Uani 1 1 d . . . S7 S 0.33059(19) 0.49874(17) 0.36510(13) 0.0281(5) Uani 1 1 d . . . S8 S 0.37655(19) 0.31606(16) 0.45251(13) 0.0285(5) Uani 1 1 d . . . C4 C 0.1982(9) 0.4269(7) 0.4687(5) 0.035(3) Uani 1 1 d . . . C5 C 0.4656(8) 0.3611(7) 0.3178(6) 0.034(2) Uani 1 1 d . . . C6 C 0.4474(7) 0.7118(7) 0.3951(5) 0.030(2) Uani 1 1 d . . . N6 N 0.4311(9) 0.7674(7) 0.3622(6) 0.058(3) Uani 1 1 d . . . N4 N 0.1109(8) 0.4065(8) 0.4587(5) 0.056(3) Uani 1 1 d . . . N5 N 0.4593(8) 0.3240(6) 0.2663(5) 0.044(2) Uani 1 1 d . . . P1 P 0.9594(2) 0.43879(17) 0.18760(14) 0.0285(6) Uani 1 1 d . . . C7 C 1.0506(7) 0.3676(6) 0.2201(5) 0.027(2) Uani 1 1 d . . . C8 C 1.1150(8) 0.3548(7) 0.1802(6) 0.035(3) Uani 1 1 d . . . H8 H 1.1103 0.3838 0.1394 0.042 Uiso 1 1 calc R . . C9 C 1.1847(8) 0.3000(7) 0.2011(6) 0.041(3) Uani 1 1 d . . . H9 H 1.2252 0.2900 0.1732 0.049 Uiso 1 1 calc R . . C10 C 1.1953(9) 0.2599(7) 0.2620(7) 0.044(3) Uani 1 1 d . . . H10 H 1.2451 0.2248 0.2768 0.053 Uiso 1 1 calc R . . C11 C 1.1328(9) 0.2710(8) 0.3019(6) 0.048(3) Uani 1 1 d . . . H11 H 1.1383 0.2414 0.3425 0.058 Uiso 1 1 calc R . . C12 C 1.0622(9) 0.3257(7) 0.2818(6) 0.039(3) Uani 1 1 d . . . H12 H 1.0218 0.3348 0.3100 0.047 Uiso 1 1 calc R . . C13 C 0.8914(8) 0.4013(6) 0.0954(5) 0.030(2) Uani 1 1 d . . . C14 C 0.8397(8) 0.3112(7) 0.0768(5) 0.031(2) Uani 1 1 d . . . H14 H 0.8385 0.2736 0.1124 0.037 Uiso 1 1 calc R . . C15 C 0.7904(8) 0.2783(7) 0.0059(6) 0.042(3) Uani 1 1 d . . . H15 H 0.7540 0.2191 -0.0066 0.051 Uiso 1 1 calc R . . C16 C 0.7961(9) 0.3349(8) -0.0468(6) 0.045(3) Uani 1 1 d . . . H16 H 0.7645 0.3128 -0.0947 0.054 Uiso 1 1 calc R . . C17 C 0.8470(10) 0.4219(9) -0.0288(6) 0.051(3) Uani 1 1 d . . . H17 H 0.8487 0.4586 -0.0648 0.061 Uiso 1 1 calc R . . C18 C 0.8961(8) 0.4570(7) 0.0415(6) 0.039(3) Uani 1 1 d . . . H18 H 0.9317 0.5165 0.0530 0.047 Uiso 1 1 calc R . . C19 C 1.0278(8) 0.5537(6) 0.1972(5) 0.028(2) Uani 1 1 d . . . C20 C 0.9694(10) 0.6205(7) 0.1797(6) 0.046(3) Uani 1 1 d . . . H20 H 0.8972 0.6064 0.1634 0.055 Uiso 1 1 calc R . . C21 C 1.0229(12) 0.7084(9) 0.1875(7) 0.054(3) Uani 1 1 d . . . H21 H 0.9854 0.7537 0.1755 0.065 Uiso 1 1 calc R . . C22 C 1.1260(11) 0.7305(8) 0.2116(6) 0.051(3) Uani 1 1 d . . . H22 H 1.1591 0.7903 0.2156 0.061 Uiso 1 1 calc R . . C23 C 1.1838(10) 0.6653(8) 0.2305(6) 0.047(3) Uani 1 1 d . . . H23 H 1.2558 0.6816 0.2483 0.056 Uiso 1 1 calc R . . C24 C 1.1360(9) 0.5756(7) 0.2236(5) 0.034(2) Uani 1 1 d . . . H24 H 1.1750 0.5314 0.2362 0.041 Uiso 1 1 calc R . . C25 C 0.8694(9) 0.4329(7) 0.2367(6) 0.038(3) Uani 1 1 d . . . C26 C 0.9097(10) 0.4547(8) 0.3107(6) 0.046(3) Uani 1 1 d . . . H26 H 0.9810 0.4708 0.3339 0.055 Uiso 1 1 calc R . . C27 C 0.8411(12) 0.4520(9) 0.3490(8) 0.062(4) Uani 1 1 d . . . H27 H 0.8668 0.4667 0.3983 0.075 Uiso 1 1 calc R . . C28 C 0.7385(13) 0.4284(10) 0.3158(9) 0.075(5) Uani 1 1 d . . . H28 H 0.6944 0.4250 0.3429 0.090 Uiso 1 1 calc R . . C29 C 0.6962(11) 0.4090(11) 0.2425(9) 0.080(5) Uani 1 1 d . . . H29 H 0.6246 0.3953 0.2201 0.096 Uiso 1 1 calc R . . C30 C 0.7641(9) 0.4105(9) 0.2024(7) 0.053(3) Uani 1 1 d . . . H30 H 0.7378 0.3963 0.1531 0.064 Uiso 1 1 calc R . . P2 P 0.5594(2) 0.75998(18) 0.13867(14) 0.0327(6) Uani 1 1 d . . . C31 C 0.5661(8) 0.7637(7) 0.0503(6) 0.036(3) Uani 1 1 d . . . C32 C 0.4819(9) 0.7805(8) -0.0037(6) 0.040(3) Uani 1 1 d . . . H32 H 0.4277 0.7989 0.0073 0.048 Uiso 1 1 calc R . . C33 C 0.4783(9) 0.7697(8) -0.0746(6) 0.044(3) Uani 1 1 d . . . H33 H 0.4212 0.7796 -0.1112 0.052 Uiso 1 1 calc R . . C34 C 0.5603(10) 0.7442(8) -0.0901(6) 0.045(3) Uani 1 1 d . . . H34 H 0.5581 0.7368 -0.1373 0.054 Uiso 1 1 calc R . . C35 C 0.6434(10) 0.7299(8) -0.0373(6) 0.046(3) Uani 1 1 d . . . H35 H 0.6984 0.7136 -0.0487 0.055 Uiso 1 1 calc R . . C36 C 0.6487(8) 0.7390(7) 0.0341(6) 0.038(3) Uani 1 1 d . . . H36 H 0.7063 0.7288 0.0701 0.045 Uiso 1 1 calc R . . C37 C 0.6877(8) 0.7692(7) 0.2016(5) 0.035(3) Uani 1 1 d . . . C38 C 0.7586(9) 0.8516(8) 0.2170(6) 0.047(3) Uani 1 1 d . . . H38 H 0.7380 0.9022 0.1969 0.057 Uiso 1 1 calc R . . C40 C 0.8902(11) 0.7852(11) 0.2941(7) 0.064(4) Uani 1 1 d . . . H40 H 0.9578 0.7906 0.3249 0.077 Uiso 1 1 calc R . . C39 C 0.8584(10) 0.8575(10) 0.2618(7) 0.058(3) Uani 1 1 d . . . H39 H 0.9054 0.9120 0.2704 0.069 Uiso 1 1 calc R . . C41 C 0.8195(12) 0.7025(12) 0.2800(7) 0.070(4) Uani 1 1 d . . . H41 H 0.8407 0.6530 0.3018 0.084 Uiso 1 1 calc R . . C42 C 0.7182(11) 0.6937(9) 0.2339(7) 0.058(4) Uani 1 1 d . . . H42 H 0.6717 0.6389 0.2246 0.070 Uiso 1 1 calc R . . C43 C 0.4824(8) 0.6515(7) 0.1403(6) 0.037(3) Uani 1 1 d . . . C44 C 0.4403(10) 0.5926(8) 0.0794(6) 0.048(3) Uani 1 1 d . . . H44 H 0.4487 0.6099 0.0369 0.058 Uiso 1 1 calc R . . C46 C 0.3696(12) 0.4831(9) 0.1424(8) 0.064(4) Uani 1 1 d . . . H46 H 0.3297 0.4271 0.1426 0.077 Uiso 1 1 calc R . . C45 C 0.3851(12) 0.5072(8) 0.0804(8) 0.068(4) Uani 1 1 d . . . H45 H 0.3589 0.4667 0.0393 0.081 Uiso 1 1 calc R . . C47 C 0.4117(11) 0.5398(9) 0.2033(8) 0.059(4) Uani 1 1 d . . . H47 H 0.4024 0.5213 0.2452 0.071 Uiso 1 1 calc R . . C48 C 0.4681(10) 0.6245(8) 0.2044(6) 0.050(3) Uani 1 1 d . . . H48 H 0.4964 0.6632 0.2465 0.060 Uiso 1 1 calc R . . C49 C 0.4998(8) 0.8499(7) 0.1574(6) 0.034(2) Uani 1 1 d . . . C50 C 0.5093(10) 0.9274(7) 0.1253(6) 0.047(3) Uani 1 1 d . . . H50 H 0.5476 0.9344 0.0943 0.056 Uiso 1 1 calc R . . C51 C 0.4611(11) 0.9958(8) 0.1397(7) 0.058(4) Uani 1 1 d . . . H51 H 0.4637 1.0472 0.1159 0.069 Uiso 1 1 calc R . . C52 C 0.4099(11) 0.9877(10) 0.1885(7) 0.063(4) Uani 1 1 d . . . H52 H 0.3813 1.0349 0.1998 0.075 Uiso 1 1 calc R . . C53 C 0.4007(11) 0.9111(10) 0.2207(8) 0.065(4) Uani 1 1 d . . . H53 H 0.3642 0.9055 0.2528 0.078 Uiso 1 1 calc R . . C54 C 0.4452(10) 0.8418(8) 0.2060(7) 0.055(3) Uani 1 1 d . . . H54 H 0.4390 0.7896 0.2283 0.066 Uiso 1 1 calc R . . P3 P 0.2606(2) 0.91331(18) 0.57663(14) 0.0315(6) Uani 1 1 d . . . C55 C 0.3970(8) 0.9254(7) 0.5957(5) 0.033(2) Uani 1 1 d . . . C56 C 0.4431(9) 0.8533(7) 0.6166(6) 0.043(3) Uani 1 1 d . . . H56 H 0.4036 0.7986 0.6203 0.052 Uiso 1 1 calc R . . C57 C 0.5506(9) 0.8641(8) 0.6321(7) 0.048(3) Uani 1 1 d . . . H57 H 0.5820 0.8160 0.6472 0.058 Uiso 1 1 calc R . . C58 C 0.6103(10) 0.9416(9) 0.6260(7) 0.055(3) Uani 1 1 d . . . H58 H 0.6813 0.9466 0.6354 0.065 Uiso 1 1 calc R . . C59 C 0.5632(10) 1.0135(9) 0.6054(8) 0.062(4) Uani 1 1 d . . . H59 H 0.6037 1.0675 0.6015 0.074 Uiso 1 1 calc R . . C60 C 0.4586(9) 1.0074(7) 0.5905(6) 0.043(3) Uani 1 1 d . . . H60 H 0.4286 1.0568 0.5771 0.051 Uiso 1 1 calc R . . C61 C 0.2277(8) 0.9019(7) 0.6569(5) 0.034(2) Uani 1 1 d . . . C62 C 0.1261(9) 0.9067(8) 0.6541(6) 0.048(3) Uani 1 1 d . . . H62 H 0.0766 0.9135 0.6113 0.057 Uiso 1 1 calc R . . C63 C 0.1012(9) 0.9013(9) 0.7162(6) 0.051(3) Uani 1 1 d . . . H63 H 0.0342 0.9038 0.7152 0.061 Uiso 1 1 calc R . . C64 C 0.1739(10) 0.8923(9) 0.7785(6) 0.056(3) Uani 1 1 d . . . H64 H 0.1552 0.8863 0.8194 0.067 Uiso 1 1 calc R . . C65 C 0.2751(11) 0.8919(11) 0.7826(7) 0.071(5) Uani 1 1 d . . . H65 H 0.3256 0.8905 0.8263 0.085 Uiso 1 1 calc R . . C66 C 0.2999(10) 0.8938(9) 0.7206(6) 0.055(4) Uani 1 1 d . . . H66 H 0.3666 0.8895 0.7221 0.065 Uiso 1 1 calc R . . C67 C 0.2197(8) 1.0123(7) 0.5398(5) 0.034(2) Uani 1 1 d . . . C68 C 0.1764(8) 1.0141(8) 0.4675(6) 0.039(3) Uani 1 1 d . . . H68 H 0.1640 0.9626 0.4364 0.047 Uiso 1 1 calc R . . C69 C 0.1513(10) 1.0924(9) 0.4412(6) 0.052(3) Uani 1 1 d . . . H69 H 0.1214 1.0937 0.3922 0.063 Uiso 1 1 calc R . . C70 C 0.1703(10) 1.1688(9) 0.4871(7) 0.056(4) Uani 1 1 d . . . H70 H 0.1538 1.2217 0.4691 0.067 Uiso 1 1 calc R . . C71 C 0.2129(13) 1.1672(9) 0.5587(8) 0.074(5) Uani 1 1 d . . . H71 H 0.2249 1.2189 0.5894 0.089 Uiso 1 1 calc R . . C72 C 0.2389(12) 1.0890(9) 0.5863(7) 0.064(4) Uani 1 1 d . . . H72 H 0.2687 1.0882 0.6353 0.077 Uiso 1 1 calc R . . C73 C 0.1985(8) 0.8161(7) 0.5138(5) 0.030(2) Uani 1 1 d . . . C74 C 0.2354(9) 0.8020(8) 0.4583(6) 0.043(3) Uani 1 1 d . . . H74 H 0.2923 0.8427 0.4556 0.052 Uiso 1 1 calc R . . C75 C 0.1915(10) 0.7308(9) 0.4077(6) 0.051(3) Uani 1 1 d . . . H75 H 0.2182 0.7228 0.3708 0.061 Uiso 1 1 calc R . . C76 C 0.1064(10) 0.6697(9) 0.4112(7) 0.057(3) Uani 1 1 d . . . H76 H 0.0748 0.6214 0.3760 0.069 Uiso 1 1 calc R . . C77 C 0.0689(11) 0.6808(10) 0.4665(8) 0.071(4) Uani 1 1 d . . . H77 H 0.0127 0.6393 0.4694 0.085 Uiso 1 1 calc R . . C78 C 0.1144(9) 0.7529(8) 0.5174(7) 0.050(3) Uani 1 1 d . . . H78 H 0.0890 0.7599 0.5550 0.060 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 Re1 0.02119(19) 0.02337(19) 0.02004(19) 0.00431(16) 0.01050(16) 0.00336(15) Re2 0.0227(2) 0.02074(18) 0.02020(19) 0.00423(15) 0.00990(17) 0.00203(16) Re3 0.02268(19) 0.02336(19) 0.01764(18) 0.00387(15) 0.00920(16) 0.00310(16) S1 0.0249(12) 0.0271(13) 0.0284(13) 0.0029(11) 0.0081(11) -0.0004(11) S2 0.0319(13) 0.0294(13) 0.0235(12) -0.0011(11) 0.0149(11) 0.0052(11) S3 0.0260(12) 0.0291(13) 0.0227(12) 0.0073(11) 0.0061(11) 0.0078(11) S4 0.0290(13) 0.0295(13) 0.0222(12) 0.0067(11) 0.0124(11) 0.0016(11) C3 0.027(6) 0.032(6) 0.044(7) -0.003(5) 0.016(5) 0.002(5) C1 0.032(6) 0.037(6) 0.019(5) 0.007(5) 0.006(5) 0.009(5) C2 0.025(5) 0.029(6) 0.019(5) 0.002(4) -0.001(4) -0.005(4) N2 0.073(7) 0.033(6) 0.043(6) 0.009(5) 0.023(6) 0.004(5) N1 0.034(5) 0.071(7) 0.038(6) 0.010(5) 0.015(5) 0.012(5) N3 0.061(7) 0.085(8) 0.011(5) 0.002(5) 0.004(5) 0.010(6) Re4 0.02175(19) 0.0259(2) 0.01953(19) 0.00466(16) 0.01108(17) 0.00325(16) Re5 0.0239(2) 0.02507(19) 0.01803(19) 0.00368(16) 0.01129(17) 0.00349(16) Re6 0.0251(2) 0.02403(19) 0.01996(19) 0.00677(16) 0.01167(17) 0.00503(16) S5 0.0318(13) 0.0323(13) 0.0248(13) 0.0066(11) 0.0177(12) 0.0032(11) S6 0.0337(14) 0.0327(13) 0.0303(13) 0.0049(11) 0.0178(12) 0.0128(12) S7 0.0257(12) 0.0369(14) 0.0191(12) 0.0066(11) 0.0050(11) 0.0037(11) S8 0.0304(13) 0.0248(12) 0.0302(13) 0.0028(11) 0.0132(12) -0.0008(11) C4 0.043(7) 0.044(6) 0.026(6) 0.010(5) 0.022(5) 0.013(5) C5 0.042(6) 0.031(5) 0.036(6) 0.002(5) 0.026(6) 0.000(5) C6 0.026(5) 0.038(6) 0.028(5) 0.011(5) 0.010(5) 0.010(5) N6 0.067(7) 0.052(7) 0.055(7) 0.022(6) 0.017(6) 0.013(6) N4 0.030(6) 0.092(9) 0.041(6) 0.002(6) 0.013(5) 0.000(6) N5 0.055(6) 0.051(6) 0.029(5) -0.002(5) 0.026(5) 0.002(5) P1 0.0314(14) 0.0290(14) 0.0289(14) 0.0069(12) 0.0149(12) 0.0054(12) C7 0.034(6) 0.024(5) 0.022(5) 0.004(4) 0.012(5) 0.001(4) C8 0.038(6) 0.035(6) 0.041(6) 0.015(5) 0.021(6) 0.013(5) C9 0.028(6) 0.042(6) 0.054(7) -0.002(6) 0.013(6) 0.011(5) C10 0.033(6) 0.033(6) 0.056(8) 0.009(6) -0.001(6) 0.008(5) C11 0.052(7) 0.047(7) 0.036(7) 0.021(6) 0.000(6) 0.008(6) C12 0.044(7) 0.041(6) 0.028(6) 0.010(5) 0.010(5) -0.001(5) C13 0.035(6) 0.030(5) 0.033(6) 0.009(5) 0.020(5) 0.009(5) C14 0.037(6) 0.031(6) 0.023(5) 0.004(5) 0.011(5) 0.006(5) C15 0.040(7) 0.030(6) 0.063(8) 0.002(6) 0.028(7) 0.004(5) C16 0.051(7) 0.052(8) 0.034(6) 0.002(6) 0.019(6) 0.009(6) C17 0.059(8) 0.064(9) 0.028(6) 0.016(6) 0.011(6) 0.010(7) C18 0.042(7) 0.034(6) 0.036(6) 0.004(5) 0.008(6) 0.000(5) C19 0.034(6) 0.029(5) 0.026(5) 0.006(4) 0.016(5) 0.005(5) C20 0.055(8) 0.033(6) 0.051(8) 0.011(6) 0.019(7) 0.012(6) C21 0.083(10) 0.045(7) 0.043(7) 0.017(6) 0.021(8) 0.030(8) C22 0.077(10) 0.039(7) 0.030(7) 0.002(6) 0.018(7) -0.005(7) C23 0.056(8) 0.052(7) 0.031(6) 0.007(6) 0.022(6) -0.004(6) C24 0.049(7) 0.031(6) 0.023(5) 0.006(5) 0.014(5) 0.004(5) C25 0.044(7) 0.044(6) 0.034(6) 0.007(5) 0.022(6) 0.013(6) C26 0.052(7) 0.056(7) 0.036(7) 0.010(6) 0.026(6) 0.007(6) C27 0.075(10) 0.064(9) 0.054(9) -0.009(7) 0.039(9) 0.004(8) C28 0.078(11) 0.082(11) 0.088(12) -0.006(9) 0.063(11) 0.010(9) C29 0.042(8) 0.116(13) 0.086(12) -0.021(11) 0.039(9) 0.000(9) C30 0.041(7) 0.072(9) 0.047(7) -0.008(7) 0.016(7) 0.013(7) P2 0.0384(15) 0.0351(15) 0.0283(14) 0.0075(12) 0.0168(13) 0.0053(13) C31 0.041(6) 0.034(6) 0.042(6) 0.016(5) 0.029(6) -0.001(5) C32 0.037(6) 0.049(7) 0.038(6) 0.008(6) 0.013(6) 0.013(6) C33 0.051(7) 0.050(7) 0.028(6) 0.011(6) 0.013(6) 0.005(6) C34 0.064(8) 0.047(7) 0.030(6) 0.005(6) 0.026(7) 0.002(6) C35 0.051(7) 0.046(7) 0.045(7) -0.004(6) 0.030(7) -0.004(6) C36 0.036(6) 0.039(6) 0.044(7) 0.009(5) 0.024(6) 0.003(5) C37 0.037(6) 0.048(7) 0.026(6) 0.005(5) 0.016(5) 0.009(5) C38 0.046(8) 0.052(8) 0.047(7) 0.005(6) 0.019(7) 0.013(6) C40 0.040(8) 0.098(12) 0.050(8) -0.007(9) 0.010(7) 0.014(9) C39 0.047(8) 0.067(9) 0.057(9) 0.001(8) 0.018(7) 0.002(7) C41 0.064(10) 0.093(12) 0.049(8) 0.007(9) -0.002(8) 0.041(10) C42 0.059(9) 0.052(8) 0.057(9) 0.005(7) 0.007(7) 0.017(7) C43 0.046(7) 0.037(6) 0.035(6) 0.011(5) 0.025(6) 0.007(5) C44 0.069(9) 0.042(7) 0.039(7) 0.016(6) 0.027(7) 0.004(6) C46 0.086(10) 0.035(7) 0.076(11) 0.016(7) 0.040(9) -0.007(7) C45 0.108(12) 0.037(7) 0.052(9) 0.006(7) 0.031(9) -0.009(8) C47 0.074(9) 0.054(8) 0.064(9) 0.026(8) 0.045(8) 0.005(7) C48 0.076(9) 0.055(8) 0.029(6) 0.011(6) 0.033(7) 0.010(7) C49 0.036(6) 0.034(6) 0.029(6) 0.001(5) 0.009(5) 0.003(5) C50 0.065(8) 0.039(7) 0.040(7) 0.010(6) 0.019(7) 0.015(6) C51 0.087(10) 0.039(7) 0.046(8) 0.015(6) 0.014(8) 0.022(7) C52 0.058(9) 0.061(9) 0.055(9) -0.010(8) -0.009(7) 0.030(8) C53 0.057(9) 0.071(10) 0.068(10) -0.014(8) 0.029(8) 0.008(8) C54 0.062(8) 0.052(8) 0.067(9) 0.011(7) 0.047(8) 0.006(7) P3 0.0350(15) 0.0369(15) 0.0262(14) 0.0044(12) 0.0164(13) 0.0048(13) C55 0.036(6) 0.038(6) 0.030(6) -0.001(5) 0.019(5) 0.005(5) C56 0.042(7) 0.031(6) 0.056(8) -0.005(6) 0.021(6) 0.001(5) C57 0.032(6) 0.051(7) 0.065(9) 0.001(7) 0.020(6) 0.011(6) C58 0.052(8) 0.068(9) 0.054(8) -0.005(7) 0.038(7) 0.004(7) C59 0.046(8) 0.061(9) 0.078(10) 0.011(8) 0.029(8) -0.010(7) C60 0.048(7) 0.036(6) 0.049(7) 0.008(6) 0.028(6) -0.002(5) C61 0.035(6) 0.045(6) 0.028(6) 0.008(5) 0.017(5) 0.007(5) C62 0.039(7) 0.076(9) 0.033(6) 0.007(6) 0.021(6) 0.008(6) C63 0.042(7) 0.075(9) 0.044(7) 0.001(7) 0.029(6) 0.002(6) C64 0.068(9) 0.075(9) 0.031(7) 0.009(7) 0.030(7) 0.007(8) C65 0.069(10) 0.122(13) 0.037(7) 0.030(9) 0.026(7) 0.037(10) C66 0.045(7) 0.089(10) 0.041(7) 0.022(7) 0.021(6) 0.026(7) C67 0.038(6) 0.037(6) 0.031(6) 0.004(5) 0.017(5) 0.008(5) C68 0.036(6) 0.049(7) 0.030(6) 0.003(5) 0.009(5) 0.008(6) C69 0.063(8) 0.060(8) 0.034(7) 0.016(7) 0.009(7) 0.022(7) C70 0.070(9) 0.059(8) 0.058(9) 0.033(7) 0.036(8) 0.028(7) C71 0.122(14) 0.048(8) 0.073(11) 0.010(8) 0.059(11) 0.022(9) C72 0.109(12) 0.057(8) 0.044(8) 0.014(7) 0.040(9) 0.034(9) C73 0.033(6) 0.036(6) 0.025(5) 0.006(5) 0.013(5) 0.009(5) C74 0.043(7) 0.047(7) 0.038(7) -0.005(6) 0.020(6) -0.005(6) C75 0.056(8) 0.060(8) 0.034(7) -0.013(6) 0.013(6) 0.012(7) C76 0.048(8) 0.058(8) 0.049(8) -0.016(7) 0.005(7) -0.006(7) C77 0.064(9) 0.065(9) 0.076(11) -0.009(9) 0.034(9) -0.022(8) C78 0.051(7) 0.057(8) 0.045(7) 0.002(6) 0.031(7) -0.005(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 Re1 C1 2.120(9) . ? Re1 S4 2.401(2) . ? Re1 S3 2.404(2) . ? Re1 S2 2.413(3) . ? Re1 S1 2.418(3) . ? Re1 Re2 2.5979(5) 2_755 ? Re1 Re2 2.6013(6) . ? Re1 Re3 2.6062(7) . ? Re1 Re3 2.6113(5) 2_755 ? Re2 C2 2.117(10) . ? Re2 S2 2.396(2) . ? Re2 S4 2.398(2) 2_755 ? Re2 S3 2.417(2) . ? Re2 S1 2.421(2) 2_755 ? Re2 Re1 2.5979(5) 2_755 ? Re2 Re3 2.6036(7) 2_755 ? Re2 Re3 2.6132(6) . ? Re3 C3 2.147(11) . ? Re3 S2 2.396(2) . ? Re3 S3 2.397(2) 2_755 ? Re3 S1 2.404(2) 2_755 ? Re3 S4 2.406(2) . ? Re3 Re2 2.6036(7) 2_755 ? Re3 Re1 2.6114(5) 2_755 ? S1 Re3 2.404(2) 2_755 ? S1 Re2 2.421(2) 2_755 ? S3 Re3 2.397(2) 2_755 ? S4 Re2 2.398(2) 2_755 ? C3 N3 1.103(13) . ? C1 N1 1.127(11) . ? C2 N2 1.137(13) . ? Re4 C4 2.116(11) . ? Re4 S5 2.393(2) . ? Re4 S7 2.395(2) . ? Re4 S8 2.404(2) . ? Re4 S6 2.405(2) . ? Re4 Re5 2.6076(8) 2_666 ? Re4 Re5 2.6079(5) . ? Re4 Re6 2.6113(6) 2_666 ? Re4 Re6 2.6117(6) . ? Re5 C5 2.122(10) . ? Re5 S6 2.407(2) 2_666 ? Re5 S7 2.413(2) . ? Re5 S8 2.416(2) . ? Re5 S5 2.419(2) 2_666 ? Re5 Re6 2.5930(6) . ? Re5 Re6 2.5936(6) 2_666 ? Re5 Re4 2.6076(8) 2_666 ? Re6 C6 2.126(10) . ? Re6 S5 2.402(2) 2_666 ? Re6 S6 2.407(2) . ? Re6 S8 2.409(3) 2_666 ? Re6 S7 2.420(3) . ? Re6 Re5 2.5935(6) 2_666 ? Re6 Re4 2.6114(6) 2_666 ? S5 Re6 2.402(2) 2_666 ? S5 Re5 2.419(2) 2_666 ? S6 Re5 2.407(2) 2_666 ? S8 Re6 2.409(3) 2_666 ? C4 N4 1.145(13) . ? C5 N5 1.116(12) . ? C6 N6 1.101(12) . ? P1 C13 1.785(11) . ? P1 C7 1.793(9) . ? P1 C19 1.804(10) . ? P1 C25 1.804(9) . ? C7 C12 1.383(13) . ? C7 C8 1.399(12) . ? C8 C9 1.365(13) . ? C9 C10 1.356(16) . ? C10 C11 1.371(16) . ? C11 C12 1.372(14) . ? C13 C14 1.402(14) . ? C13 C18 1.403(13) . ? C14 C15 1.380(15) . ? C15 C16 1.395(15) . ? C16 C17 1.356(17) . ? C17 C18 1.379(16) . ? C19 C24 1.395(15) . ? C19 C20 1.398(13) . ? C20 C21 1.384(17) . ? C21 C22 1.329(18) . ? C22 C23 1.374(16) . ? C23 C24 1.385(15) . ? C25 C30 1.373(16) . ? C25 C26 1.395(15) . ? C26 C27 1.391(15) . ? C27 C28 1.34(2) . ? C28 C29 1.38(2) . ? C29 C30 1.410(16) . ? P2 C31 1.788(10) . ? P2 C37 1.798(11) . ? P2 C49 1.799(10) . ? P2 C43 1.805(11) . ? C31 C32 1.383(15) . ? C31 C36 1.390(13) . ? C32 C33 1.394(14) . ? C33 C34 1.379(14) . ? C34 C35 1.348(16) . ? C35 C36 1.395(15) . ? C37 C38 1.402(16) . ? C37 C42 1.405(15) . ? C38 C39 1.372(17) . ? C40 C39 1.366(18) . ? C40 C41 1.41(2) . ? C41 C42 1.391(19) . ? C43 C44 1.369(16) . ? C43 C48 1.415(13) . ? C44 C45 1.389(17) . ? C46 C47 1.351(19) . ? C46 C45 1.368(17) . ? C47 C48 1.378(17) . ? C49 C50 1.370(14) . ? C49 C54 1.399(14) . ? C50 C51 1.397(15) . ? C51 C52 1.369(18) . ? C52 C53 1.356(19) . ? C53 C54 1.376(16) . ? P3 C55 1.782(10) . ? P3 C73 1.784(11) . ? P3 C61 1.797(9) . ? P3 C67 1.805(10) . ? C55 C56 1.379(14) . ? C55 C60 1.408(15) . ? C56 C57 1.401(15) . ? C57 C58 1.348(17) . ? C58 C59 1.382(17) . ? C59 C60 1.371(16) . ? C61 C66 1.368(15) . ? C61 C62 1.408(14) . ? C62 C63 1.383(14) . ? C63 C64 1.356(17) . ? C64 C65 1.382(17) . ? C65 C66 1.379(15) . ? C67 C68 1.372(14) . ? C67 C72 1.385(16) . ? C68 C69 1.377(14) . ? C69 C70 1.376(18) . ? C70 C71 1.356(19) . ? C71 C72 1.388(17) . ? C73 C74 1.376(13) . ? C73 C78 1.396(15) . ? C74 C75 1.354(16) . ? C75 C76 1.389(18) . ? C76 C77 1.370(17) . ? C77 C78 1.369(18) . ? 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 C1 Re1 S4 91.2(2) . . ? C1 Re1 S3 95.4(2) . . ? S4 Re1 S3 173.42(7) . . ? C1 Re1 S2 90.2(3) . . ? S4 Re1 S2 90.04(8) . . ? S3 Re1 S2 90.19(8) . . ? C1 Re1 S1 97.1(3) . . ? S4 Re1 S1 90.10(8) . . ? S3 Re1 S1 88.85(8) . . ? S2 Re1 S1 172.76(7) . . ? C1 Re1 Re2 135.9(3) . 2_755 ? S4 Re1 Re2 57.17(5) . 2_755 ? S3 Re1 Re2 117.10(5) . 2_755 ? S2 Re1 Re2 116.85(6) . 2_755 ? S1 Re1 Re2 57.58(6) . 2_755 ? C1 Re1 Re2 133.8(3) . . ? S4 Re1 Re2 117.45(6) . . ? S3 Re1 Re2 57.59(6) . . ? S2 Re1 Re2 56.94(5) . . ? S1 Re1 Re2 116.86(6) . . ? Re2 Re1 Re2 89.982(18) 2_755 . ? C1 Re1 Re3 130.7(3) . . ? S4 Re1 Re3 57.26(6) . . ? S3 Re1 Re3 117.79(6) . . ? S2 Re1 Re3 56.87(6) . . ? S1 Re1 Re3 117.57(6) . . ? Re2 Re1 Re3 60.038(19) 2_755 . ? Re2 Re1 Re3 60.241(18) . . ? C1 Re1 Re3 138.9(3) . 2_755 ? S4 Re1 Re3 117.36(5) . 2_755 ? S3 Re1 Re3 56.91(5) . 2_755 ? S2 Re1 Re3 116.82(5) . 2_755 ? S1 Re1 Re3 56.96(5) . 2_755 ? Re2 Re1 Re3 60.216(16) 2_755 2_755 ? Re2 Re1 Re3 59.930(19) . 2_755 ? Re3 Re1 Re3 90.386(18) . 2_755 ? C2 Re2 S2 93.8(3) . . ? C2 Re2 S4 92.7(3) . 2_755 ? S2 Re2 S4 173.50(8) . 2_755 ? C2 Re2 S3 92.4(3) . . ? S2 Re2 S3 90.28(8) . . ? S4 Re2 S3 89.93(8) 2_755 . ? C2 Re2 S1 94.7(3) . 2_755 ? S2 Re2 S1 88.88(8) . 2_755 ? S4 Re2 S1 90.10(8) 2_755 2_755 ? S3 Re2 S1 172.87(8) . 2_755 ? C2 Re2 Re1 135.5(2) . 2_755 ? S2 Re2 Re1 117.08(6) . 2_755 ? S4 Re2 Re1 57.28(5) 2_755 2_755 ? S3 Re2 Re1 116.97(6) . 2_755 ? S1 Re2 Re1 57.48(6) 2_755 2_755 ? C2 Re2 Re1 134.5(2) . . ? S2 Re2 Re1 57.58(6) . . ? S4 Re2 Re1 117.51(6) 2_755 . ? S3 Re2 Re1 57.10(6) . . ? S1 Re2 Re1 116.85(6) 2_755 . ? Re1 Re2 Re1 90.018(18) 2_755 . ? C2 Re2 Re3 133.5(3) . 2_755 ? S2 Re2 Re3 117.76(7) . 2_755 ? S4 Re2 Re3 57.34(6) 2_755 2_755 ? S3 Re2 Re3 56.88(6) . 2_755 ? S1 Re2 Re3 117.57(6) 2_755 2_755 ? Re1 Re2 Re3 60.139(17) 2_755 2_755 ? Re1 Re2 Re3 60.226(18) . 2_755 ? C2 Re2 Re3 136.1(3) . . ? S2 Re2 Re3 56.96(6) . . ? S4 Re2 Re3 117.40(6) 2_755 . ? S3 Re2 Re3 117.03(6) . . ? S1 Re2 Re3 56.91(6) 2_755 . ? Re1 Re2 Re3 60.147(15) 2_755 . ? Re1 Re2 Re3 59.973(18) . . ? Re3 Re2 Re3 90.402(19) 2_755 . ? C3 Re3 S2 93.8(2) . . ? C3 Re3 S3 93.1(2) . 2_755 ? S2 Re3 S3 172.98(8) . 2_755 ? C3 Re3 S1 96.0(3) . 2_755 ? S2 Re3 S1 89.26(8) . 2_755 ? S3 Re3 S1 89.34(8) 2_755 2_755 ? C3 Re3 S4 90.9(3) . . ? S2 Re3 S4 90.33(8) . . ? S3 Re3 S4 90.23(8) 2_755 . ? S1 Re3 S4 173.06(8) 2_755 . ? C3 Re3 Re2 133.0(3) . 2_755 ? S2 Re3 Re2 117.26(7) . 2_755 ? S3 Re3 Re2 57.64(6) 2_755 2_755 ? S1 Re3 Re2 117.28(6) 2_755 2_755 ? S4 Re3 Re2 57.04(6) . 2_755 ? C3 Re3 Re1 133.3(2) . . ? S2 Re3 Re1 57.50(6) . . ? S3 Re3 Re1 117.41(6) 2_755 . ? S1 Re3 Re1 117.27(6) 2_755 . ? S4 Re3 Re1 57.07(6) . . ? Re2 Re3 Re1 59.822(19) 2_755 . ? C3 Re3 Re1 137.0(2) . 2_755 ? S2 Re3 Re1 116.56(6) . 2_755 ? S3 Re3 Re1 57.18(5) 2_755 2_755 ? S1 Re3 Re1 57.47(6) 2_755 2_755 ? S4 Re3 Re1 116.83(6) . 2_755 ? Re2 Re3 Re1 59.842(17) 2_755 2_755 ? Re1 Re3 Re1 89.614(18) . 2_755 ? C3 Re3 Re2 137.4(3) . . ? S2 Re3 Re2 56.95(5) . . ? S3 Re3 Re2 116.79(6) 2_755 . ? S1 Re3 Re2 57.51(6) 2_755 . ? S4 Re3 Re2 116.81(6) . . ? Re2 Re3 Re2 89.595(19) 2_755 . ? Re1 Re3 Re2 59.786(17) . . ? Re1 Re3 Re2 59.635(15) 2_755 . ? Re3 S1 Re1 65.56(7) 2_755 . ? Re3 S1 Re2 65.58(6) 2_755 2_755 ? Re1 S1 Re2 64.94(7) . 2_755 ? Re2 S2 Re3 66.09(5) . . ? Re2 S2 Re1 65.49(6) . . ? Re3 S2 Re1 65.62(6) . . ? Re3 S3 Re1 65.91(6) 2_755 . ? Re3 S3 Re2 65.48(6) 2_755 . ? Re1 S3 Re2 65.31(6) . . ? Re2 S4 Re1 65.55(6) 2_755 . ? Re2 S4 Re3 65.63(6) 2_755 . ? Re1 S4 Re3 65.66(6) . . ? N3 C3 Re3 175.4(10) . . ? N1 C1 Re1 177.1(10) . . ? N2 C2 Re2 177.6(9) . . ? C4 Re4 S5 94.1(3) . . ? C4 Re4 S7 92.6(3) . . ? S5 Re4 S7 173.32(8) . . ? C4 Re4 S8 94.2(3) . . ? S5 Re4 S8 89.25(8) . . ? S7 Re4 S8 89.81(8) . . ? C4 Re4 S6 93.1(3) . . ? S5 Re4 S6 90.17(8) . . ? S7 Re4 S6 89.93(8) . . ? S8 Re4 S6 172.77(8) . . ? C4 Re4 Re5 135.4(3) . 2_666 ? S5 Re4 Re5 57.67(6) . 2_666 ? S7 Re4 Re5 117.18(7) . 2_666 ? S8 Re4 Re5 116.77(7) . 2_666 ? S6 Re4 Re5 57.22(6) . 2_666 ? C4 Re4 Re5 135.4(3) . . ? S5 Re4 Re5 116.75(5) . . ? S7 Re4 Re5 57.49(5) . . ? S8 Re4 Re5 57.47(5) . . ? S6 Re4 Re5 116.69(6) . . ? Re5 Re4 Re5 89.201(19) 2_666 . ? C4 Re4 Re6 136.2(3) . 2_666 ? S5 Re4 Re6 57.18(5) . 2_666 ? S7 Re4 Re6 117.05(6) . 2_666 ? S8 Re4 Re6 57.23(6) . 2_666 ? S6 Re4 Re6 116.76(7) . 2_666 ? Re5 Re4 Re6 59.584(17) 2_666 2_666 ? Re5 Re4 Re6 59.594(15) . 2_666 ? C4 Re4 Re6 134.4(3) . . ? S5 Re4 Re6 117.21(7) . . ? S7 Re4 Re6 57.63(7) . . ? S8 Re4 Re6 117.01(6) . . ? S6 Re4 Re6 57.16(5) . . ? Re5 Re4 Re6 59.592(18) 2_666 . ? Re5 Re4 Re6 59.575(15) . . ? Re6 Re4 Re6 89.369(19) 2_666 . ? C5 Re5 S6 92.1(3) . 2_666 ? C5 Re5 S7 94.3(3) . . ? S6 Re5 S7 173.55(8) 2_666 . ? C5 Re5 S8 94.2(3) . . ? S6 Re5 S8 90.00(8) 2_666 . ? S7 Re5 S8 89.09(8) . . ? C5 Re5 S5 92.7(3) . 2_666 ? S6 Re5 S5 89.51(8) 2_666 2_666 ? S7 Re5 S5 90.63(8) . 2_666 ? S8 Re5 S5 173.06(8) . 2_666 ? C5 Re5 Re6 135.0(3) . . ? S6 Re5 Re6 117.39(7) 2_666 . ? S7 Re5 Re6 57.69(7) . . ? S8 Re5 Re6 117.26(6) . . ? S5 Re5 Re6 57.16(5) 2_666 . ? C5 Re5 Re6 134.8(3) . 2_666 ? S6 Re5 Re6 57.40(5) 2_666 2_666 ? S7 Re5 Re6 117.06(6) . 2_666 ? S8 Re5 Re6 57.34(6) . 2_666 ? S5 Re5 Re6 116.94(6) 2_666 2_666 ? Re6 Re5 Re6 90.17(2) . 2_666 ? C5 Re5 Re4 133.2(3) . 2_666 ? S6 Re5 Re4 57.16(6) 2_666 2_666 ? S7 Re5 Re4 117.93(7) . 2_666 ? S8 Re5 Re4 117.59(7) . 2_666 ? S5 Re5 Re4 56.71(6) 2_666 2_666 ? Re6 Re5 Re4 60.281(19) . 2_666 ? Re6 Re5 Re4 60.282(18) 2_666 2_666 ? C5 Re5 Re4 136.0(3) . . ? S6 Re5 Re4 117.64(6) 2_666 . ? S7 Re5 Re4 56.82(5) . . ? S8 Re5 Re4 57.01(5) . . ? S5 Re5 Re4 117.40(5) 2_666 . ? Re6 Re5 Re4 60.286(17) . . ? Re6 Re5 Re4 60.268(16) 2_666 . ? Re4 Re5 Re4 90.799(19) 2_666 . ? C6 Re6 S5 91.8(2) . 2_666 ? C6 Re6 S6 94.8(2) . . ? S5 Re6 S6 173.42(8) 2_666 . ? C6 Re6 S8 94.3(3) . 2_666 ? S5 Re6 S8 88.91(8) 2_666 2_666 ? S6 Re6 S8 90.18(8) . 2_666 ? C6 Re6 S7 92.5(3) . . ? S5 Re6 S7 90.85(8) 2_666 . ? S6 Re6 S7 89.28(9) . . ? S8 Re6 S7 173.22(8) 2_666 . ? C6 Re6 Re5 133.3(3) . . ? S5 Re6 Re5 57.77(6) 2_666 . ? S6 Re6 Re5 117.19(6) . . ? S8 Re6 Re5 117.15(6) 2_666 . ? S7 Re6 Re5 57.42(6) . . ? C6 Re6 Re5 136.9(3) . 2_666 ? S5 Re6 Re5 116.94(6) 2_666 2_666 ? S6 Re6 Re5 57.40(6) . 2_666 ? S8 Re6 Re5 57.62(6) 2_666 2_666 ? S7 Re6 Re5 116.77(6) . 2_666 ? Re5 Re6 Re5 89.83(2) . 2_666 ? C6 Re6 Re4 134.4(3) . 2_666 ? S5 Re6 Re4 56.83(6) 2_666 2_666 ? S6 Re6 Re4 117.51(6) . 2_666 ? S8 Re6 Re4 57.05(6) 2_666 2_666 ? S7 Re6 Re4 117.51(6) . 2_666 ? Re5 Re6 Re4 60.14(2) . 2_666 ? Re5 Re6 Re4 60.137(17) 2_666 2_666 ? C6 Re6 Re4 134.9(3) . . ? S5 Re6 Re4 117.87(6) 2_666 . ? S6 Re6 Re4 57.10(6) . . ? S8 Re6 Re4 117.72(6) 2_666 . ? S7 Re6 Re4 56.68(6) . . ? Re5 Re6 Re4 60.139(15) . . ? Re5 Re6 Re4 60.13(2) 2_666 . ? Re4 Re6 Re4 90.631(19) 2_666 . ? Re4 S5 Re6 65.99(6) . 2_666 ? Re4 S5 Re5 65.63(6) . 2_666 ? Re6 S5 Re5 65.07(6) 2_666 2_666 ? Re4 S6 Re6 65.74(6) . . ? Re4 S6 Re5 65.62(6) . 2_666 ? Re6 S6 Re5 65.20(6) . 2_666 ? Re4 S7 Re5 65.70(6) . . ? Re4 S7 Re6 65.69(7) . . ? Re5 S7 Re6 64.89(6) . . ? Re4 S8 Re6 65.73(7) . 2_666 ? Re4 S8 Re5 65.51(6) . . ? Re6 S8 Re5 65.03(7) 2_666 . ? N4 C4 Re4 179.2(9) . . ? N5 C5 Re5 177.9(10) . . ? N6 C6 Re6 176.5(10) . . ? C13 P1 C7 107.4(4) . . ? C13 P1 C19 109.9(4) . . ? C7 P1 C19 109.6(5) . . ? C13 P1 C25 110.2(5) . . ? C7 P1 C25 111.0(4) . . ? C19 P1 C25 108.7(5) . . ? C12 C7 C8 118.1(9) . . ? C12 C7 P1 124.6(7) . . ? C8 C7 P1 117.3(7) . . ? C9 C8 C7 120.3(9) . . ? C10 C9 C8 120.6(10) . . ? C9 C10 C11 120.2(9) . . ? C10 C11 C12 120.1(10) . . ? C11 C12 C7 120.6(10) . . ? C14 C13 C18 119.7(10) . . ? C14 C13 P1 118.2(7) . . ? C18 C13 P1 121.8(8) . . ? C15 C14 C13 120.1(9) . . ? C14 C15 C16 119.1(10) . . ? C17 C16 C15 120.7(11) . . ? C16 C17 C18 121.6(11) . . ? C17 C18 C13 118.7(11) . . ? C24 C19 C20 120.9(10) . . ? C24 C19 P1 121.0(7) . . ? C20 C19 P1 118.1(8) . . ? C21 C20 C19 117.5(12) . . ? C22 C21 C20 122.5(11) . . ? C21 C22 C23 120.2(12) . . ? C22 C23 C24 120.8(12) . . ? C23 C24 C19 118.1(10) . . ? C30 C25 C26 120.7(10) . . ? C30 C25 P1 121.2(9) . . ? C26 C25 P1 118.1(9) . . ? C27 C26 C25 118.7(12) . . ? C28 C27 C26 120.8(13) . . ? C27 C28 C29 121.9(12) . . ? C28 C29 C30 118.4(13) . . ? C25 C30 C29 119.5(12) . . ? C31 P2 C37 109.6(5) . . ? C31 P2 C49 108.7(5) . . ? C37 P2 C49 111.5(5) . . ? C31 P2 C43 106.8(5) . . ? C37 P2 C43 108.9(5) . . ? C49 P2 C43 111.3(5) . . ? C32 C31 C36 120.0(9) . . ? C32 C31 P2 119.0(7) . . ? C36 C31 P2 120.5(8) . . ? C31 C32 C33 120.0(9) . . ? C34 C33 C32 119.4(10) . . ? C35 C34 C33 120.6(10) . . ? C34 C35 C36 121.3(10) . . ? C31 C36 C35 118.6(11) . . ? C38 C37 C42 119.8(11) . . ? C38 C37 P2 119.9(8) . . ? C42 C37 P2 120.3(9) . . ? C39 C38 C37 120.0(11) . . ? C39 C40 C41 119.2(12) . . ? C40 C39 C38 121.5(13) . . ? C42 C41 C40 120.9(13) . . ? C41 C42 C37 118.7(14) . . ? C44 C43 C48 119.0(10) . . ? C44 C43 P2 119.9(7) . . ? C48 C43 P2 121.1(9) . . ? C43 C44 C45 120.7(11) . . ? C47 C46 C45 120.7(12) . . ? C46 C45 C44 119.5(13) . . ? C46 C47 C48 121.2(11) . . ? C47 C48 C43 118.8(12) . . ? C50 C49 C54 119.5(10) . . ? C50 C49 P2 120.3(8) . . ? C54 C49 P2 120.2(8) . . ? C49 C50 C51 119.4(11) . . ? C52 C51 C50 120.3(11) . . ? C53 C52 C51 120.4(11) . . ? C52 C53 C54 120.3(12) . . ? C53 C54 C49 120.0(12) . . ? C55 P3 C73 107.6(5) . . ? C55 P3 C61 110.6(5) . . ? C73 P3 C61 110.7(5) . . ? C55 P3 C67 109.5(5) . . ? C73 P3 C67 110.6(5) . . ? C61 P3 C67 107.8(4) . . ? C56 C55 C60 119.6(10) . . ? C56 C55 P3 119.3(8) . . ? C60 C55 P3 121.1(8) . . ? C55 C56 C57 118.6(11) . . ? C58 C57 C56 122.6(11) . . ? C57 C58 C59 118.2(12) . . ? C60 C59 C58 121.9(12) . . ? C59 C60 C55 119.1(11) . . ? C66 C61 C62 119.8(9) . . ? C66 C61 P3 121.8(8) . . ? C62 C61 P3 118.3(8) . . ? C63 C62 C61 118.7(11) . . ? C64 C63 C62 120.4(11) . . ? C63 C64 C65 121.4(10) . . ? C66 C65 C64 118.7(12) . . ? C61 C66 C65 120.9(11) . . ? C68 C67 C72 120.3(10) . . ? C68 C67 P3 121.4(8) . . ? C72 C67 P3 118.2(8) . . ? C67 C68 C69 119.7(11) . . ? C70 C69 C68 120.2(11) . . ? C71 C70 C69 120.2(11) . . ? C70 C71 C72 120.5(13) . . ? C67 C72 C71 119.0(12) . . ? C74 C73 C78 117.7(10) . . ? C74 C73 P3 118.4(8) . . ? C78 C73 P3 124.0(8) . . ? C75 C74 C73 122.1(11) . . ? C74 C75 C76 119.4(11) . . ? C77 C76 C75 120.0(13) . . ? C78 C77 C76 119.9(12) . . ? C77 C78 C73 120.9(10) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 2.731 _refine_diff_density_min -2.622 _refine_diff_density_rms 0.240 #################### Material relevant to compound 2 at 200K ############ data_sb200k _database_code_CSD 186995 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(PPh4)3 (Re6Se8(CN)6)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H60 N6 P3 Re6 S8' _chemical_formula_weight 2547.91 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' 'P' 'P' 0.1023 0.0942 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8428(17) _cell_length_b 15.1586(17) _cell_length_c 19.825(2) _cell_angle_alpha 92.627(14) _cell_angle_beta 108.619(13) _cell_angle_gamma 100.289(14) _cell_volume 3855.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7997 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2310 _exptl_crystal_size_mid 0.1924 _exptl_crystal_size_min 0.1733 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2386 _exptl_absorpt_coefficient_mu 9.708 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1545 _exptl_absorpt_correction_T_max 0.2875 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, Phi. incr. == 1.2' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39707 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.92 _reflns_number_total 13976 _reflns_number_gt 10337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE, [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0429P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000177(19) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13976 _refine_ls_number_parameters 911 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _refine_ls_shift/su_max 0.001 _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 0.87496(3) 0.01515(2) 0.007660(19) 0.01609(9) Uani 1 1 d . . . Re2 Re 1.04229(3) 0.12285(2) 0.005076(19) 0.01610(9) Uani 1 1 d . . . Re3 Re 1.05552(3) 0.00577(2) 0.098701(19) 0.01626(9) Uani 1 1 d . . . S1 S 0.79424(19) -0.10444(16) -0.08954(13) 0.0229(5) Uani 1 1 d . . . S2 S 0.97645(19) 0.13342(16) 0.10251(12) 0.0214(5) Uani 1 1 d . . . S3 S 0.87121(18) 0.12086(16) -0.07949(12) 0.0202(5) Uani 1 1 d . . . S4 S 0.89619(18) -0.09410(16) 0.09235(12) 0.0206(5) Uani 1 1 d . . . C3 C 1.1121(7) 0.0073(6) 0.2129(6) 0.024(2) Uani 1 1 d . . . C1 C 0.7359(8) 0.0357(7) 0.0244(5) 0.024(2) Uani 1 1 d . . . C2 C 1.0881(8) 0.2648(7) 0.0074(5) 0.026(2) Uani 1 1 d . . . N2 N 1.1153(8) 0.3401(6) 0.0100(5) 0.039(2) Uani 1 1 d . . . N1 N 0.6654(7) 0.0487(7) 0.0369(5) 0.037(2) Uani 1 1 d . . . N3 N 1.1348(8) 0.0059(7) 0.2721(5) 0.044(3) Uani 1 1 d . . . Re4 Re 0.35858(3) 0.46445(2) 0.485540(19) 0.01666(9) Uani 1 1 d . . . Re5 Re 0.48208(3) 0.43536(2) 0.415174(18) 0.01661(9) Uani 1 1 d . . . Re6 Re 0.47535(3) 0.59952(2) 0.452914(19) 0.01694(9) Uani 1 1 d . . . S5 S 0.40872(19) 0.43438(16) 0.60795(12) 0.0219(5) Uani 1 1 d . . . S6 S 0.36414(19) 0.61923(17) 0.52185(13) 0.0239(5) Uani 1 1 d . . . S7 S 0.32986(19) 0.49861(17) 0.36490(12) 0.0227(5) Uani 1 1 d . . . S8 S 0.37602(19) 0.31547(16) 0.45178(13) 0.0228(5) Uani 1 1 d . . . C4 C 0.1962(8) 0.4260(7) 0.4689(5) 0.028(2) Uani 1 1 d . . . C5 C 0.4646(8) 0.3610(7) 0.3169(5) 0.026(2) Uani 1 1 d . . . C6 C 0.4470(8) 0.7129(7) 0.3947(5) 0.025(2) Uani 1 1 d . . . N6 N 0.4298(8) 0.7693(7) 0.3624(6) 0.048(3) Uani 1 1 d . . . N4 N 0.1099(7) 0.4049(7) 0.4580(5) 0.041(2) Uani 1 1 d . . . N5 N 0.4572(7) 0.3233(6) 0.2650(5) 0.036(2) Uani 1 1 d . . . P1 P 0.9586(2) 0.43802(17) 0.18742(13) 0.0222(5) Uani 1 1 d . . . C7 C 1.0512(8) 0.3671(6) 0.2193(5) 0.022(2) Uani 1 1 d . . . C8 C 1.1145(8) 0.3540(7) 0.1798(5) 0.026(2) Uani 1 1 d . . . H8 H 1.1082 0.3818 0.1381 0.031 Uiso 1 1 calc R . . C9 C 1.1859(8) 0.3011(7) 0.2008(6) 0.030(2) Uani 1 1 d . . . H9 H 1.2283 0.2936 0.1738 0.036 Uiso 1 1 calc R . . C10 C 1.1960(8) 0.2587(7) 0.2617(6) 0.033(3) Uani 1 1 d . . . H10 H 1.2454 0.2230 0.2761 0.040 Uiso 1 1 calc R . . C11 C 1.1315(8) 0.2696(8) 0.3016(5) 0.035(3) Uani 1 1 d . . . H11 H 1.1370 0.2396 0.3421 0.042 Uiso 1 1 calc R . . C12 C 1.0601(8) 0.3237(7) 0.2822(5) 0.030(2) Uani 1 1 d . . . H12 H 1.0183 0.3318 0.3096 0.036 Uiso 1 1 calc R . . C13 C 0.8904(7) 0.4008(7) 0.0950(5) 0.024(2) Uani 1 1 d . . . C14 C 0.8375(8) 0.3098(7) 0.0757(5) 0.027(2) Uani 1 1 d . . . H14 H 0.8352 0.2718 0.1109 0.032 Uiso 1 1 calc R . . C15 C 0.7892(8) 0.2774(7) 0.0039(6) 0.036(3) Uani 1 1 d . . . H15 H 0.7528 0.2180 -0.0092 0.043 Uiso 1 1 calc R . . C16 C 0.7953(8) 0.3335(8) -0.0476(5) 0.033(3) Uani 1 1 d . . . H16 H 0.7637 0.3112 -0.0957 0.039 Uiso 1 1 calc R . . C17 C 0.8467(9) 0.4211(8) -0.0300(6) 0.040(3) Uani 1 1 d . . . H17 H 0.8496 0.4576 -0.0660 0.048 Uiso 1 1 calc R . . C18 C 0.8952(8) 0.4569(7) 0.0415(6) 0.032(2) Uani 1 1 d . . . H18 H 0.9300 0.5168 0.0535 0.038 Uiso 1 1 calc R . . C19 C 1.0271(8) 0.5531(7) 0.1973(5) 0.026(2) Uani 1 1 d . . . C20 C 0.9694(10) 0.6203(7) 0.1797(6) 0.037(3) Uani 1 1 d . . . H20 H 0.8970 0.6057 0.1630 0.045 Uiso 1 1 calc R . . C21 C 1.0215(11) 0.7091(8) 0.1874(6) 0.043(3) Uani 1 1 d . . . H21 H 0.9835 0.7543 0.1756 0.051 Uiso 1 1 calc R . . C22 C 1.1277(10) 0.7314(8) 0.2121(6) 0.040(3) Uani 1 1 d . . . H22 H 1.1611 0.7914 0.2166 0.048 Uiso 1 1 calc R . . C23 C 1.1858(10) 0.6661(8) 0.2304(6) 0.038(3) Uani 1 1 d . . . H23 H 1.2582 0.6816 0.2479 0.046 Uiso 1 1 calc R . . C24 C 1.1343(9) 0.5761(7) 0.2222(5) 0.029(2) Uani 1 1 d . . . H24 H 1.1728 0.5312 0.2337 0.035 Uiso 1 1 calc R . . C25 C 0.8688(8) 0.4325(7) 0.2360(6) 0.031(2) Uani 1 1 d . . . C26 C 0.9080(9) 0.4531(8) 0.3115(6) 0.036(3) Uani 1 1 d . . . H26 H 0.9794 0.4686 0.3355 0.043 Uiso 1 1 calc R . . C27 C 0.8392(11) 0.4499(9) 0.3488(7) 0.051(3) Uani 1 1 d . . . H27 H 0.8646 0.4629 0.3984 0.061 Uiso 1 1 calc R . . C28 C 0.7359(11) 0.4283(10) 0.3146(8) 0.058(4) Uani 1 1 d . . . H28 H 0.6912 0.4264 0.3412 0.069 Uiso 1 1 calc R . . C29 C 0.6944(10) 0.4089(10) 0.2414(8) 0.059(4) Uani 1 1 d . . . H29 H 0.6227 0.3952 0.2183 0.070 Uiso 1 1 calc R . . C30 C 0.7631(9) 0.4105(8) 0.2032(7) 0.043(3) Uani 1 1 d . . . H30 H 0.7364 0.3961 0.1537 0.052 Uiso 1 1 calc R . . P2 P 0.5596(2) 0.76010(18) 0.13931(14) 0.0254(6) Uani 1 1 d . . . C31 C 0.5664(8) 0.7649(7) 0.0504(5) 0.028(2) Uani 1 1 d . . . C32 C 0.4812(8) 0.7809(8) -0.0039(6) 0.033(3) Uani 1 1 d . . . H32 H 0.4267 0.7990 0.0070 0.040 Uiso 1 1 calc R . . C33 C 0.4777(9) 0.7697(8) -0.0746(6) 0.037(3) Uani 1 1 d . . . H33 H 0.4206 0.7798 -0.1113 0.045 Uiso 1 1 calc R . . C34 C 0.5604(9) 0.7432(7) -0.0901(5) 0.033(3) Uani 1 1 d . . . H34 H 0.5581 0.7349 -0.1374 0.040 Uiso 1 1 calc R . . C35 C 0.6445(9) 0.7295(7) -0.0361(6) 0.033(3) Uani 1 1 d . . . H35 H 0.7000 0.7137 -0.0472 0.040 Uiso 1 1 calc R . . C36 C 0.6495(8) 0.7385(7) 0.0352(6) 0.029(2) Uani 1 1 d . . . H36 H 0.7063 0.7273 0.0715 0.035 Uiso 1 1 calc R . . C37 C 0.6876(9) 0.7683(7) 0.2023(5) 0.031(2) Uani 1 1 d . . . C38 C 0.7583(9) 0.8512(8) 0.2167(6) 0.037(3) Uani 1 1 d . . . H38 H 0.7378 0.9013 0.1955 0.044 Uiso 1 1 calc R . . C40 C 0.8913(10) 0.7846(10) 0.2940(7) 0.054(4) Uani 1 1 d . . . H40 H 0.9599 0.7897 0.3236 0.065 Uiso 1 1 calc R . . C39 C 0.8598(10) 0.8577(9) 0.2630(6) 0.045(3) Uani 1 1 d . . . H39 H 0.9066 0.9127 0.2730 0.054 Uiso 1 1 calc R . . C41 C 0.8219(11) 0.7028(11) 0.2816(7) 0.057(4) Uani 1 1 d . . . H41 H 0.8430 0.6540 0.3048 0.069 Uiso 1 1 calc R . . C42 C 0.7188(9) 0.6932(8) 0.2337(6) 0.042(3) Uani 1 1 d . . . H42 H 0.6728 0.6377 0.2234 0.051 Uiso 1 1 calc R . . C43 C 0.4817(8) 0.6515(7) 0.1401(5) 0.027(2) Uani 1 1 d . . . C44 C 0.4411(10) 0.5924(8) 0.0790(6) 0.040(3) Uani 1 1 d . . . H44 H 0.4529 0.6093 0.0374 0.048 Uiso 1 1 calc R . . C46 C 0.3683(11) 0.4813(9) 0.1406(8) 0.054(4) Uani 1 1 d . . . H46 H 0.3295 0.4245 0.1407 0.065 Uiso 1 1 calc R . . C45 C 0.3820(11) 0.5068(8) 0.0780(7) 0.050(3) Uani 1 1 d . . . H45 H 0.3527 0.4679 0.0358 0.060 Uiso 1 1 calc R . . C47 C 0.4109(11) 0.5386(8) 0.2028(7) 0.051(4) Uani 1 1 d . . . H47 H 0.4011 0.5200 0.2446 0.061 Uiso 1 1 calc R . . C48 C 0.4688(10) 0.6245(8) 0.2043(6) 0.039(3) Uani 1 1 d . . . H48 H 0.4981 0.6630 0.2467 0.047 Uiso 1 1 calc R . . C49 C 0.5000(8) 0.8500(6) 0.1585(5) 0.025(2) Uani 1 1 d . . . C50 C 0.5090(10) 0.9282(8) 0.1268(6) 0.040(3) Uani 1 1 d . . . H50 H 0.5474 0.9357 0.0958 0.048 Uiso 1 1 calc R . . C51 C 0.4603(10) 0.9966(8) 0.1411(6) 0.046(3) Uani 1 1 d . . . H51 H 0.4629 1.0483 0.1177 0.055 Uiso 1 1 calc R . . C52 C 0.4089(10) 0.9874(9) 0.1893(6) 0.048(3) Uani 1 1 d . . . H52 H 0.3799 1.0343 0.2009 0.057 Uiso 1 1 calc R . . C53 C 0.3998(10) 0.9096(9) 0.2208(7) 0.050(3) Uani 1 1 d . . . H53 H 0.3615 0.9029 0.2518 0.060 Uiso 1 1 calc R . . C54 C 0.4463(9) 0.8410(8) 0.2075(7) 0.042(3) Uani 1 1 d . . . H54 H 0.4421 0.7893 0.2308 0.050 Uiso 1 1 calc R . . P3 P 0.2599(2) 0.91265(18) 0.57692(13) 0.0242(6) Uani 1 1 d . . . C55 C 0.3971(8) 0.9251(7) 0.5964(5) 0.025(2) Uani 1 1 d . . . C56 C 0.4436(8) 0.8532(7) 0.6173(6) 0.031(2) Uani 1 1 d . . . H56 H 0.4035 0.7988 0.6213 0.037 Uiso 1 1 calc R . . C57 C 0.5494(9) 0.8616(8) 0.6324(7) 0.040(3) Uani 1 1 d . . . H57 H 0.5803 0.8130 0.6475 0.048 Uiso 1 1 calc R . . C58 C 0.6106(9) 0.9416(8) 0.6254(6) 0.042(3) Uani 1 1 d . . . H58 H 0.6817 0.9470 0.6347 0.051 Uiso 1 1 calc R . . C59 C 0.5620(10) 1.0131(9) 0.6041(7) 0.048(3) Uani 1 1 d . . . H59 H 0.6019 1.0673 0.5995 0.058 Uiso 1 1 calc R . . C60 C 0.4579(9) 1.0066(8) 0.5899(6) 0.036(3) Uani 1 1 d . . . H60 H 0.4274 1.0557 0.5760 0.044 Uiso 1 1 calc R . . C61 C 0.2272(8) 0.9019(7) 0.6570(5) 0.024(2) Uani 1 1 d . . . C62 C 0.1257(9) 0.9057(8) 0.6539(6) 0.037(3) Uani 1 1 d . . . H62 H 0.0760 0.9114 0.6107 0.045 Uiso 1 1 calc R . . C63 C 0.0998(10) 0.9009(9) 0.7156(6) 0.042(3) Uani 1 1 d . . . H63 H 0.0323 0.9027 0.7138 0.051 Uiso 1 1 calc R . . C64 C 0.1732(10) 0.8936(8) 0.7793(6) 0.042(3) Uani 1 1 d . . . H64 H 0.1547 0.8892 0.8204 0.051 Uiso 1 1 calc R . . C65 C 0.2746(10) 0.8927(9) 0.7832(7) 0.049(3) Uani 1 1 d . . . H65 H 0.3250 0.8905 0.8270 0.058 Uiso 1 1 calc R . . C66 C 0.3004(9) 0.8951(8) 0.7212(6) 0.037(3) Uani 1 1 d . . . H66 H 0.3677 0.8920 0.7231 0.045 Uiso 1 1 calc R . . C67 C 0.2192(8) 1.0119(7) 0.5404(5) 0.029(2) Uani 1 1 d . . . C68 C 0.1773(8) 1.0145(7) 0.4676(6) 0.031(2) Uani 1 1 d . . . H68 H 0.1661 0.9632 0.4362 0.037 Uiso 1 1 calc R . . C69 C 0.1518(9) 1.0927(8) 0.4412(6) 0.040(3) Uani 1 1 d . . . H69 H 0.1233 1.0941 0.3921 0.048 Uiso 1 1 calc R . . C70 C 0.1682(10) 1.1686(8) 0.4869(7) 0.045(3) Uani 1 1 d . . . H70 H 0.1491 1.2208 0.4689 0.054 Uiso 1 1 calc R . . C71 C 0.2130(13) 1.1673(9) 0.5595(7) 0.062(4) Uani 1 1 d . . . H71 H 0.2266 1.2194 0.5906 0.074 Uiso 1 1 calc R . . C72 C 0.2376(12) 1.0885(8) 0.5861(6) 0.052(4) Uani 1 1 d . . . H72 H 0.2668 1.0874 0.6353 0.062 Uiso 1 1 calc R . . C73 C 0.1983(8) 0.8153(7) 0.5138(5) 0.026(2) Uani 1 1 d . . . C74 C 0.2364(8) 0.8022(7) 0.4584(6) 0.032(3) Uani 1 1 d . . . H74 H 0.2933 0.8430 0.4557 0.039 Uiso 1 1 calc R . . C75 C 0.1906(9) 0.7293(8) 0.4077(6) 0.039(3) Uani 1 1 d . . . H75 H 0.2173 0.7209 0.3709 0.047 Uiso 1 1 calc R . . C76 C 0.1057(10) 0.6684(9) 0.4104(7) 0.046(3) Uani 1 1 d . . . H76 H 0.0738 0.6199 0.3751 0.055 Uiso 1 1 calc R . . C77 C 0.0691(11) 0.6805(9) 0.4659(7) 0.054(4) Uani 1 1 d . . . H77 H 0.0132 0.6384 0.4687 0.065 Uiso 1 1 calc R . . C78 C 0.1120(9) 0.7520(8) 0.5167(6) 0.039(3) Uani 1 1 d . . . H78 H 0.0847 0.7594 0.5533 0.046 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 Re1 0.01714(19) 0.01800(19) 0.01495(18) 0.00427(15) 0.00828(16) 0.00217(15) Re2 0.01840(19) 0.01587(18) 0.01493(18) 0.00407(15) 0.00778(16) 0.00104(15) Re3 0.01827(19) 0.01802(19) 0.01337(18) 0.00388(15) 0.00722(16) 0.00173(15) S1 0.0214(12) 0.0227(13) 0.0225(13) 0.0042(11) 0.0069(11) -0.0004(11) S2 0.0245(13) 0.0239(12) 0.0185(12) 0.0009(10) 0.0116(11) 0.0043(11) S3 0.0211(12) 0.0219(12) 0.0174(12) 0.0076(10) 0.0053(10) 0.0049(10) S4 0.0230(12) 0.0220(12) 0.0182(12) 0.0061(10) 0.0105(11) 0.0005(10) C3 0.020(5) 0.024(5) 0.034(6) 0.005(5) 0.018(5) 0.001(4) C1 0.032(6) 0.025(5) 0.020(5) 0.009(4) 0.011(5) 0.012(5) C2 0.028(6) 0.030(6) 0.015(5) 0.006(5) 0.004(5) -0.001(5) N2 0.056(7) 0.027(5) 0.036(6) 0.011(5) 0.018(5) 0.007(5) N1 0.029(5) 0.058(7) 0.027(5) 0.006(5) 0.013(5) 0.009(5) N3 0.047(6) 0.070(8) 0.013(5) 0.010(5) 0.007(5) 0.013(6) Re4 0.01732(19) 0.02030(19) 0.01426(18) 0.00447(15) 0.00846(16) 0.00212(16) Re5 0.0189(2) 0.01958(19) 0.01310(18) 0.00361(15) 0.00854(16) 0.00190(16) Re6 0.0200(2) 0.01871(19) 0.01453(18) 0.00588(15) 0.00881(16) 0.00327(16) S5 0.0252(13) 0.0258(13) 0.0176(12) 0.0060(10) 0.0128(11) 0.0011(11) S6 0.0285(14) 0.0261(13) 0.0228(12) 0.0043(11) 0.0134(11) 0.0107(11) S7 0.0221(12) 0.0311(14) 0.0133(11) 0.0052(11) 0.0049(10) 0.0025(11) S8 0.0251(13) 0.0197(12) 0.0242(13) 0.0040(11) 0.0117(11) -0.0007(10) C4 0.035(6) 0.035(6) 0.020(5) 0.008(5) 0.018(5) 0.006(5) C5 0.037(6) 0.020(5) 0.028(6) 0.004(5) 0.019(5) 0.007(5) C6 0.022(5) 0.033(6) 0.023(5) 0.005(5) 0.007(5) 0.010(5) N6 0.055(7) 0.038(6) 0.048(7) 0.019(5) 0.013(6) 0.006(5) N4 0.022(5) 0.065(7) 0.035(6) 0.005(5) 0.012(5) -0.001(5) N5 0.045(6) 0.042(6) 0.024(5) 0.003(5) 0.018(5) 0.002(5) P1 0.0249(13) 0.0227(13) 0.0223(13) 0.0070(11) 0.0123(12) 0.0036(11) C7 0.027(5) 0.019(5) 0.021(5) 0.006(4) 0.008(5) 0.004(4) C8 0.026(6) 0.027(6) 0.025(5) 0.005(5) 0.011(5) 0.003(5) C9 0.023(5) 0.024(5) 0.044(7) 0.003(5) 0.016(5) 0.001(5) C10 0.023(6) 0.027(6) 0.044(7) 0.009(5) 0.002(5) 0.006(5) C11 0.035(6) 0.035(6) 0.014(5) 0.006(5) -0.014(5) -0.003(5) C12 0.037(6) 0.033(6) 0.023(5) 0.014(5) 0.013(5) 0.007(5) C13 0.023(5) 0.033(6) 0.022(5) 0.011(5) 0.016(5) 0.008(5) C14 0.028(6) 0.027(6) 0.023(5) 0.012(5) 0.008(5) -0.001(5) C15 0.030(6) 0.028(6) 0.051(7) -0.001(6) 0.017(6) 0.006(5) C16 0.029(6) 0.049(7) 0.015(5) -0.002(5) 0.006(5) 0.000(6) C17 0.046(7) 0.049(8) 0.022(6) 0.016(6) 0.006(6) 0.007(6) C18 0.037(6) 0.027(6) 0.030(6) 0.008(5) 0.011(5) 0.001(5) C19 0.034(6) 0.025(5) 0.022(5) 0.006(5) 0.015(5) 0.004(5) C20 0.050(7) 0.027(6) 0.039(7) 0.013(5) 0.016(6) 0.013(6) C21 0.069(9) 0.029(6) 0.038(7) 0.016(6) 0.018(7) 0.024(7) C22 0.061(8) 0.031(6) 0.020(6) 0.003(5) 0.011(6) -0.005(6) C23 0.043(7) 0.043(7) 0.018(6) -0.003(5) 0.005(5) -0.010(6) C24 0.036(6) 0.026(6) 0.023(6) 0.003(5) 0.011(5) 0.001(5) C25 0.027(6) 0.033(6) 0.035(6) 0.005(5) 0.014(5) 0.004(5) C26 0.042(7) 0.041(7) 0.025(6) -0.002(5) 0.012(6) 0.009(6) C27 0.067(10) 0.054(8) 0.043(8) 0.003(7) 0.032(8) 0.013(8) C28 0.055(9) 0.062(9) 0.064(10) -0.008(8) 0.040(9) 0.002(8) C29 0.029(7) 0.081(10) 0.068(10) -0.010(8) 0.032(7) -0.005(7) C30 0.037(7) 0.057(8) 0.042(7) 0.005(6) 0.024(6) 0.007(6) P2 0.0300(15) 0.0269(14) 0.0207(13) 0.0063(12) 0.0111(12) 0.0035(12) C31 0.031(6) 0.026(5) 0.030(6) 0.012(5) 0.016(5) 0.001(5) C32 0.029(6) 0.044(7) 0.033(6) 0.014(5) 0.018(5) 0.011(5) C33 0.044(7) 0.040(7) 0.025(6) 0.012(5) 0.008(6) 0.005(6) C34 0.044(7) 0.039(6) 0.019(5) 0.004(5) 0.018(5) -0.003(6) C35 0.046(7) 0.029(6) 0.034(6) 0.001(5) 0.029(6) 0.000(5) C36 0.032(6) 0.024(5) 0.038(6) 0.010(5) 0.024(5) 0.000(5) C37 0.040(7) 0.034(6) 0.023(6) 0.005(5) 0.016(5) 0.006(5) C38 0.036(7) 0.045(7) 0.030(6) 0.007(6) 0.011(6) 0.010(6) C40 0.036(8) 0.072(10) 0.057(9) 0.005(8) 0.014(7) 0.021(8) C39 0.044(8) 0.051(8) 0.038(7) -0.004(6) 0.018(7) -0.001(6) C41 0.058(9) 0.068(10) 0.043(8) 0.010(8) -0.001(7) 0.037(9) C42 0.042(7) 0.039(7) 0.048(8) 0.011(6) 0.015(6) 0.014(6) C43 0.037(6) 0.025(5) 0.023(5) 0.007(5) 0.016(5) 0.005(5) C44 0.058(8) 0.033(6) 0.033(6) 0.010(6) 0.022(6) 0.006(6) C46 0.066(9) 0.028(7) 0.065(10) 0.014(7) 0.024(8) -0.003(7) C45 0.081(10) 0.024(6) 0.039(7) 0.003(6) 0.025(8) -0.014(6) C47 0.069(9) 0.042(8) 0.055(9) 0.025(7) 0.038(8) 0.008(7) C48 0.059(8) 0.042(7) 0.024(6) 0.012(5) 0.023(6) 0.007(6) C49 0.031(6) 0.018(5) 0.019(5) 0.001(4) 0.005(5) -0.005(4) C50 0.053(8) 0.041(7) 0.028(6) 0.010(6) 0.013(6) 0.012(6) C51 0.070(9) 0.028(7) 0.035(7) 0.008(6) 0.007(7) 0.019(7) C52 0.045(8) 0.052(8) 0.036(7) -0.012(6) -0.008(6) 0.028(7) C53 0.048(8) 0.052(8) 0.057(9) -0.002(7) 0.028(7) 0.008(7) C54 0.054(8) 0.036(7) 0.050(8) 0.009(6) 0.040(7) 0.003(6) P3 0.0273(14) 0.0288(14) 0.0189(13) 0.0047(11) 0.0120(12) 0.0037(12) C55 0.027(6) 0.028(6) 0.025(5) 0.004(5) 0.019(5) 0.000(5) C56 0.028(6) 0.026(6) 0.038(6) 0.006(5) 0.014(5) -0.002(5) C57 0.037(7) 0.036(7) 0.049(7) 0.000(6) 0.016(6) 0.010(6) C58 0.031(7) 0.055(8) 0.040(7) -0.010(6) 0.021(6) -0.004(6) C59 0.041(7) 0.045(8) 0.053(8) 0.003(7) 0.021(7) -0.014(6) C60 0.040(7) 0.038(7) 0.038(7) 0.013(6) 0.024(6) 0.003(6) C61 0.027(5) 0.029(6) 0.020(5) 0.007(5) 0.012(5) 0.005(5) C62 0.036(6) 0.049(7) 0.030(6) 0.010(6) 0.017(6) 0.006(6) C63 0.042(7) 0.063(8) 0.029(6) 0.006(6) 0.026(6) 0.005(6) C64 0.057(8) 0.056(8) 0.024(6) 0.011(6) 0.027(6) 0.010(7) C65 0.054(8) 0.066(9) 0.034(7) 0.026(7) 0.021(7) 0.016(7) C66 0.033(6) 0.053(8) 0.034(6) 0.015(6) 0.020(6) 0.012(6) C67 0.034(6) 0.032(6) 0.026(6) 0.002(5) 0.018(5) 0.007(5) C68 0.032(6) 0.035(6) 0.025(6) 0.008(5) 0.006(5) 0.007(5) C69 0.048(7) 0.044(7) 0.036(7) 0.017(6) 0.017(6) 0.019(6) C70 0.053(8) 0.040(7) 0.060(8) 0.029(7) 0.036(7) 0.020(6) C71 0.114(13) 0.039(8) 0.040(8) 0.006(7) 0.034(9) 0.021(9) C72 0.099(11) 0.042(7) 0.030(7) 0.012(6) 0.036(8) 0.027(8) C73 0.026(5) 0.028(6) 0.025(5) 0.007(5) 0.012(5) 0.002(5) C74 0.028(6) 0.041(7) 0.027(6) 0.000(5) 0.015(5) -0.004(5) C75 0.048(7) 0.046(7) 0.025(6) -0.002(6) 0.012(6) 0.013(6) C76 0.041(7) 0.044(8) 0.042(8) -0.010(6) 0.011(7) -0.008(6) C77 0.049(8) 0.053(9) 0.057(9) -0.001(7) 0.025(8) -0.014(7) C78 0.040(7) 0.047(7) 0.030(6) -0.001(6) 0.021(6) -0.004(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 Re1 C1 2.127(9) . ? Re1 S4 2.400(2) . ? Re1 S3 2.405(2) . ? Re1 S2 2.414(3) . ? Re1 S1 2.414(3) . ? Re1 Re2 2.5970(6) 2_755 ? Re1 Re2 2.6011(7) . ? Re1 Re3 2.6067(7) . ? Re1 Re3 2.6108(5) 2_755 ? Re1 Re1 3.6760(8) 2_755 ? Re2 C2 2.126(11) . ? Re2 S2 2.395(2) . ? Re2 S4 2.398(2) 2_755 ? Re2 S1 2.419(2) 2_755 ? Re2 S3 2.420(2) . ? Re2 Re1 2.5970(6) 2_755 ? Re2 Re3 2.6035(8) 2_755 ? Re2 Re3 2.6134(6) . ? Re2 Re2 3.6751(9) 2_755 ? Re3 C3 2.143(10) . ? Re3 S3 2.394(2) 2_755 ? Re3 S2 2.397(2) . ? Re3 S1 2.398(2) 2_755 ? Re3 S4 2.405(2) . ? Re3 Re2 2.6035(8) 2_755 ? Re3 Re1 2.6108(5) 2_755 ? Re3 Re3 3.7026(9) 2_755 ? S1 Re3 2.398(2) 2_755 ? S1 Re2 2.419(2) 2_755 ? S3 Re3 2.394(2) 2_755 ? S4 Re2 2.398(2) 2_755 ? C3 N3 1.116(12) . ? C1 N1 1.128(11) . ? C2 N2 1.129(13) . ? Re4 C4 2.131(11) . ? Re4 S5 2.391(2) . ? Re4 S7 2.393(2) . ? Re4 S8 2.401(2) . ? Re4 S6 2.403(2) . ? Re4 Re5 2.6075(5) . ? Re4 Re5 2.6083(8) 2_666 ? Re4 Re6 2.6129(6) 2_666 ? Re4 Re6 2.6135(6) . ? Re4 Re4 3.7179(9) 2_666 ? Re5 C5 2.127(10) . ? Re5 S6 2.409(2) 2_666 ? Re5 S7 2.413(2) . ? Re5 S8 2.415(2) . ? Re5 S5 2.419(2) 2_666 ? Re5 Re6 2.5918(6) . ? Re5 Re6 2.5923(6) 2_666 ? Re5 Re4 2.6083(8) 2_666 ? Re5 Re5 3.6582(9) 2_666 ? Re6 C6 2.138(10) . ? Re6 S5 2.402(2) 2_666 ? Re6 S6 2.408(2) . ? Re6 S8 2.411(3) 2_666 ? Re6 S7 2.419(3) . ? Re6 Re5 2.5923(6) 2_666 ? Re6 Re4 2.6129(6) 2_666 ? Re6 Re6 3.6733(8) 2_666 ? S5 Re6 2.402(2) 2_666 ? S5 Re5 2.419(2) 2_666 ? S6 Re5 2.409(2) 2_666 ? S8 Re6 2.411(3) 2_666 ? C4 N4 1.127(13) . ? C5 N5 1.120(12) . ? C6 N6 1.106(12) . ? P1 C13 1.783(10) . ? P1 C25 1.793(9) . ? P1 C7 1.798(9) . ? P1 C19 1.800(11) . ? C7 C8 1.381(12) . ? C7 C12 1.418(12) . ? C8 C9 1.358(13) . ? C9 C10 1.373(14) . ? C10 C11 1.394(15) . ? C11 C12 1.368(14) . ? C13 C18 1.399(13) . ? C13 C14 1.414(14) . ? C14 C15 1.387(15) . ? C15 C16 1.373(15) . ? C16 C17 1.361(16) . ? C17 C18 1.395(16) . ? C19 C24 1.378(15) . ? C19 C20 1.393(13) . ? C20 C21 1.387(17) . ? C21 C22 1.365(17) . ? C22 C23 1.374(16) . ? C23 C24 1.399(15) . ? C25 C30 1.369(16) . ? C25 C26 1.418(15) . ? C26 C27 1.377(15) . ? C27 C28 1.34(2) . ? C28 C29 1.375(19) . ? C29 C30 1.391(14) . ? P2 C37 1.791(12) . ? P2 C49 1.799(9) . ? P2 C31 1.800(10) . ? P2 C43 1.804(11) . ? C31 C32 1.387(15) . ? C31 C36 1.395(12) . ? C32 C33 1.387(14) . ? C33 C34 1.394(14) . ? C34 C35 1.362(15) . ? C35 C36 1.393(14) . ? C37 C42 1.393(14) . ? C37 C38 1.403(16) . ? C38 C39 1.394(16) . ? C40 C39 1.364(17) . ? C40 C41 1.38(2) . ? C41 C42 1.417(18) . ? C43 C44 1.368(15) . ? C43 C48 1.410(13) . ? C44 C45 1.400(16) . ? C46 C47 1.370(19) . ? C46 C45 1.376(16) . ? C47 C48 1.395(17) . ? C49 C50 1.372(14) . ? C49 C54 1.397(13) . ? C50 C51 1.399(15) . ? C51 C52 1.360(17) . ? C52 C53 1.363(18) . ? C53 C54 1.374(15) . ? P3 C73 1.780(11) . ? P3 C55 1.787(10) . ? P3 C61 1.792(9) . ? P3 C67 1.802(10) . ? C55 C56 1.376(13) . ? C55 C60 1.401(14) . ? C56 C57 1.380(15) . ? C57 C58 1.389(16) . ? C58 C59 1.389(16) . ? C59 C60 1.362(16) . ? C61 C66 1.372(14) . ? C61 C62 1.398(14) . ? C62 C63 1.381(13) . ? C63 C64 1.369(16) . ? C64 C65 1.384(16) . ? C65 C66 1.385(14) . ? C67 C72 1.373(15) . ? C67 C68 1.379(14) . ? C68 C69 1.376(14) . ? C69 C70 1.369(17) . ? C70 C71 1.376(18) . ? C71 C72 1.382(16) . ? C73 C74 1.382(13) . ? C73 C78 1.410(15) . ? C74 C75 1.370(16) . ? C75 C76 1.377(17) . ? C76 C77 1.367(16) . ? C77 C78 1.353(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 C1 Re1 S4 91.2(2) . . ? C1 Re1 S3 95.3(2) . . ? S4 Re1 S3 173.44(7) . . ? C1 Re1 S2 90.4(3) . . ? S4 Re1 S2 90.02(8) . . ? S3 Re1 S2 90.24(8) . . ? C1 Re1 S1 97.0(3) . . ? S4 Re1 S1 90.24(8) . . ? S3 Re1 S1 88.66(8) . . ? S2 Re1 S1 172.65(7) . . ? C1 Re1 Re2 135.9(3) . 2_755 ? S4 Re1 Re2 57.20(5) . 2_755 ? S3 Re1 Re2 117.07(5) . 2_755 ? S2 Re1 Re2 116.85(5) . 2_755 ? S1 Re1 Re2 57.58(6) . 2_755 ? C1 Re1 Re2 133.9(3) . . ? S4 Re1 Re2 117.43(6) . . ? S3 Re1 Re2 57.65(6) . . ? S2 Re1 Re2 56.90(5) . . ? S1 Re1 Re2 116.75(6) . . ? Re2 Re1 Re2 89.986(19) 2_755 . ? C1 Re1 Re3 130.8(3) . . ? S4 Re1 Re3 57.24(6) . . ? S3 Re1 Re3 117.85(6) . . ? S2 Re1 Re3 56.87(5) . . ? S1 Re1 Re3 117.57(6) . . ? Re2 Re1 Re3 60.04(2) 2_755 . ? Re2 Re1 Re3 60.242(18) . . ? C1 Re1 Re3 138.7(3) . 2_755 ? S4 Re1 Re3 117.41(5) . 2_755 ? S3 Re1 Re3 56.85(5) . 2_755 ? S2 Re1 Re3 116.80(5) . 2_755 ? S1 Re1 Re3 56.84(5) . 2_755 ? Re2 Re1 Re3 60.242(16) 2_755 2_755 ? Re2 Re1 Re3 59.936(18) . 2_755 ? Re3 Re1 Re3 90.413(19) . 2_755 ? C1 Re1 Re1 175.9(3) . 2_755 ? S4 Re1 Re1 86.74(5) . 2_755 ? S3 Re1 Re1 86.73(5) . 2_755 ? S2 Re1 Re1 86.14(5) . 2_755 ? S1 Re1 Re1 86.55(6) . 2_755 ? Re2 Re1 Re1 45.039(15) 2_755 2_755 ? Re2 Re1 Re1 44.948(13) . 2_755 ? Re3 Re1 Re1 45.252(13) . 2_755 ? Re3 Re1 Re1 45.161(14) 2_755 2_755 ? C2 Re2 S2 94.3(2) . . ? C2 Re2 S4 92.2(2) . 2_755 ? S2 Re2 S4 173.51(8) . 2_755 ? C2 Re2 S1 95.2(3) . 2_755 ? S2 Re2 S1 88.80(8) . 2_755 ? S4 Re2 S1 90.18(8) 2_755 2_755 ? C2 Re2 S3 92.1(3) . . ? S2 Re2 S3 90.34(8) . . ? S4 Re2 S3 89.86(8) 2_755 . ? S1 Re2 S3 172.70(8) 2_755 . ? C2 Re2 Re1 135.3(3) . 2_755 ? S2 Re2 Re1 117.10(6) . 2_755 ? S4 Re2 Re1 57.28(5) 2_755 2_755 ? S1 Re2 Re1 57.42(6) 2_755 2_755 ? S3 Re2 Re1 116.91(6) . 2_755 ? C2 Re2 Re1 134.6(3) . . ? S2 Re2 Re1 57.61(6) . . ? S4 Re2 Re1 117.47(6) 2_755 . ? S1 Re2 Re1 116.71(6) 2_755 . ? S3 Re2 Re1 57.09(5) . . ? Re1 Re2 Re1 90.014(18) 2_755 . ? C2 Re2 Re3 132.9(3) . 2_755 ? S2 Re2 Re3 117.79(7) . 2_755 ? S4 Re2 Re3 57.30(6) 2_755 2_755 ? S1 Re2 Re3 117.53(6) 2_755 2_755 ? S3 Re2 Re3 56.79(6) . 2_755 ? Re1 Re2 Re3 60.165(18) 2_755 2_755 ? Re1 Re2 Re3 60.217(18) . 2_755 ? C2 Re2 Re3 136.7(3) . . ? S2 Re2 Re3 56.98(5) . . ? S4 Re2 Re3 117.39(5) 2_755 . ? S1 Re2 Re3 56.75(6) 2_755 . ? S3 Re2 Re3 117.03(6) . . ? Re1 Re2 Re3 60.141(15) 2_755 . ? Re1 Re2 Re3 59.986(17) . . ? Re3 Re2 Re3 90.427(19) 2_755 . ? C2 Re2 Re2 178.1(3) . 2_755 ? S2 Re2 Re2 86.72(6) . 2_755 ? S4 Re2 Re2 86.82(6) 2_755 2_755 ? S1 Re2 Re2 86.42(6) 2_755 2_755 ? S3 Re2 Re2 86.29(6) . 2_755 ? Re1 Re2 Re2 45.052(13) 2_755 2_755 ? Re1 Re2 Re2 44.961(14) . 2_755 ? Re3 Re2 Re2 45.324(15) 2_755 2_755 ? Re3 Re2 Re2 45.103(15) . 2_755 ? C3 Re3 S3 93.2(2) . 2_755 ? C3 Re3 S2 93.7(2) . . ? S3 Re3 S2 173.02(8) 2_755 . ? C3 Re3 S1 96.5(3) . 2_755 ? S3 Re3 S1 89.29(8) 2_755 2_755 ? S2 Re3 S1 89.25(8) . 2_755 ? C3 Re3 S4 90.5(3) . . ? S3 Re3 S4 90.30(8) 2_755 . ? S2 Re3 S4 90.33(8) . . ? S1 Re3 S4 173.06(8) 2_755 . ? C3 Re3 Re2 132.7(3) . 2_755 ? S3 Re3 Re2 57.73(6) 2_755 2_755 ? S2 Re3 Re2 117.24(6) . 2_755 ? S1 Re3 Re2 117.27(6) 2_755 2_755 ? S4 Re3 Re2 57.05(6) . 2_755 ? C3 Re3 Re1 132.9(2) . . ? S3 Re3 Re1 117.47(6) 2_755 . ? S2 Re3 Re1 57.51(6) . . ? S1 Re3 Re1 117.27(6) 2_755 . ? S4 Re3 Re1 57.06(5) . . ? Re2 Re3 Re1 59.794(19) 2_755 . ? C3 Re3 Re1 137.4(2) . 2_755 ? S3 Re3 Re1 57.23(5) 2_755 2_755 ? S2 Re3 Re1 116.51(5) . 2_755 ? S1 Re3 Re1 57.45(6) 2_755 2_755 ? S4 Re3 Re1 116.85(6) . 2_755 ? Re2 Re3 Re1 59.846(17) 2_755 2_755 ? Re1 Re3 Re1 89.587(19) . 2_755 ? C3 Re3 Re2 137.6(3) . . ? S3 Re3 Re2 116.82(5) 2_755 . ? S2 Re3 Re2 56.91(5) . . ? S1 Re3 Re2 57.53(6) 2_755 . ? S4 Re3 Re2 116.79(6) . . ? Re2 Re3 Re2 89.573(19) 2_755 . ? Re1 Re3 Re2 59.772(18) . . ? Re1 Re3 Re2 59.616(15) 2_755 . ? C3 Re3 Re3 176.8(3) . 2_755 ? S3 Re3 Re3 86.74(6) 2_755 2_755 ? S2 Re3 Re3 86.36(6) . 2_755 ? S1 Re3 Re3 86.75(6) 2_755 2_755 ? S4 Re3 Re3 86.31(6) . 2_755 ? Re2 Re3 Re3 44.895(15) 2_755 2_755 ? Re1 Re3 Re3 44.838(14) . 2_755 ? Re1 Re3 Re3 44.749(13) 2_755 2_755 ? Re2 Re3 Re3 44.678(15) . 2_755 ? Re3 S1 Re1 65.71(7) 2_755 . ? Re3 S1 Re2 65.71(6) 2_755 2_755 ? Re1 S1 Re2 65.00(7) . 2_755 ? Re2 S2 Re3 66.10(5) . . ? Re2 S2 Re1 65.48(6) . . ? Re3 S2 Re1 65.61(6) . . ? Re3 S3 Re1 65.92(6) 2_755 . ? Re3 S3 Re2 65.47(6) 2_755 . ? Re1 S3 Re2 65.25(6) . . ? Re2 S4 Re1 65.53(5) 2_755 . ? Re2 S4 Re3 65.64(6) 2_755 . ? Re1 S4 Re3 65.70(6) . . ? N3 C3 Re3 175.3(9) . . ? N1 C1 Re1 176.2(9) . . ? N2 C2 Re2 177.9(10) . . ? C4 Re4 S5 93.7(3) . . ? C4 Re4 S7 93.0(3) . . ? S5 Re4 S7 173.24(8) . . ? C4 Re4 S8 94.4(3) . . ? S5 Re4 S8 89.30(8) . . ? S7 Re4 S8 89.79(8) . . ? C4 Re4 S6 92.8(3) . . ? S5 Re4 S6 90.19(8) . . ? S7 Re4 S6 89.88(8) . . ? S8 Re4 S6 172.80(8) . . ? C4 Re4 Re5 135.9(3) . . ? S5 Re4 Re5 116.68(5) . . ? S7 Re4 Re5 57.50(5) . . ? S8 Re4 Re5 57.48(5) . . ? S6 Re4 Re5 116.66(6) . . ? C4 Re4 Re5 135.0(3) . 2_666 ? S5 Re4 Re5 57.69(6) . 2_666 ? S7 Re4 Re5 117.07(7) . 2_666 ? S8 Re4 Re5 116.77(6) . 2_666 ? S6 Re4 Re5 57.28(6) . 2_666 ? Re5 Re4 Re5 89.073(19) . 2_666 ? C4 Re4 Re6 136.2(3) . 2_666 ? S5 Re4 Re6 57.16(5) . 2_666 ? S7 Re4 Re6 117.02(6) . 2_666 ? S8 Re4 Re6 57.29(6) . 2_666 ? S6 Re4 Re6 116.76(7) . 2_666 ? Re5 Re4 Re6 59.546(15) . 2_666 ? Re5 Re4 Re6 59.524(17) 2_666 2_666 ? C4 Re4 Re6 134.5(3) . . ? S5 Re4 Re6 117.17(6) . . ? S7 Re4 Re6 57.58(7) . . ? S8 Re4 Re6 116.97(5) . . ? S6 Re4 Re6 57.18(5) . . ? Re5 Re4 Re6 59.527(16) . . ? Re5 Re4 Re6 59.528(18) 2_666 . ? Re6 Re4 Re6 89.308(19) 2_666 . ? C4 Re4 Re4 179.1(3) . 2_666 ? S5 Re4 Re4 86.55(6) . 2_666 ? S7 Re4 Re4 86.70(6) . 2_666 ? S8 Re4 Re4 86.50(6) . 2_666 ? S6 Re4 Re4 86.30(6) . 2_666 ? Re5 Re4 Re4 44.545(15) . 2_666 ? Re5 Re4 Re4 44.527(15) 2_666 2_666 ? Re6 Re4 Re4 44.660(13) 2_666 2_666 ? Re6 Re4 Re4 44.648(15) . 2_666 ? C5 Re5 S6 92.4(3) . 2_666 ? C5 Re5 S7 94.1(3) . . ? S6 Re5 S7 173.55(8) 2_666 . ? C5 Re5 S8 94.1(3) . . ? S6 Re5 S8 90.18(8) 2_666 . ? S7 Re5 S8 89.00(8) . . ? C5 Re5 S5 92.8(3) . 2_666 ? S6 Re5 S5 89.38(8) 2_666 2_666 ? S7 Re5 S5 90.66(8) . 2_666 ? S8 Re5 S5 173.11(8) . 2_666 ? C5 Re5 Re6 134.9(2) . . ? S6 Re5 Re6 117.36(7) 2_666 . ? S7 Re5 Re6 57.68(7) . . ? S8 Re5 Re6 117.27(5) . . ? S5 Re5 Re6 57.16(5) 2_666 . ? C5 Re5 Re6 134.9(2) . 2_666 ? S6 Re5 Re6 57.42(5) 2_666 2_666 ? S7 Re5 Re6 117.08(5) . 2_666 ? S8 Re5 Re6 57.43(6) . 2_666 ? S5 Re5 Re6 116.93(6) 2_666 2_666 ? Re6 Re5 Re6 90.24(2) . 2_666 ? C5 Re5 Re4 135.7(3) . . ? S6 Re5 Re4 117.72(5) 2_666 . ? S7 Re5 Re4 56.78(5) . . ? S8 Re5 Re4 56.96(5) . . ? S5 Re5 Re4 117.47(5) 2_666 . ? Re6 Re5 Re4 60.351(17) . . ? Re6 Re5 Re4 60.331(16) 2_666 . ? C5 Re5 Re4 133.4(3) . 2_666 ? S6 Re5 Re4 57.07(6) 2_666 2_666 ? S7 Re5 Re4 117.96(7) . 2_666 ? S8 Re5 Re4 117.73(6) . 2_666 ? S5 Re5 Re4 56.65(6) 2_666 2_666 ? Re6 Re5 Re4 60.326(19) . 2_666 ? Re6 Re5 Re4 60.335(18) 2_666 2_666 ? Re4 Re5 Re4 90.927(19) . 2_666 ? C5 Re5 Re5 178.8(3) . 2_666 ? S6 Re5 Re5 86.79(6) 2_666 2_666 ? S7 Re5 Re5 86.78(6) . 2_666 ? S8 Re5 Re5 86.74(6) . 2_666 ? S5 Re5 Re5 86.37(6) 2_666 2_666 ? Re6 Re5 Re5 45.123(15) . 2_666 ? Re6 Re5 Re5 45.113(13) 2_666 2_666 ? Re4 Re5 Re5 45.473(14) . 2_666 ? Re4 Re5 Re5 45.454(15) 2_666 2_666 ? C6 Re6 S5 91.6(2) . 2_666 ? C6 Re6 S6 95.0(2) . . ? S5 Re6 S6 173.36(8) 2_666 . ? C6 Re6 S8 94.5(3) . 2_666 ? S5 Re6 S8 88.82(8) 2_666 2_666 ? S6 Re6 S8 90.30(8) . 2_666 ? C6 Re6 S7 92.4(3) . . ? S5 Re6 S7 90.93(8) 2_666 . ? S6 Re6 S7 89.15(8) . . ? S8 Re6 S7 173.13(8) 2_666 . ? C6 Re6 Re5 133.1(3) . . ? S5 Re6 Re5 57.81(6) 2_666 . ? S6 Re6 Re5 117.08(6) . . ? S8 Re6 Re5 117.04(6) 2_666 . ? S7 Re6 Re5 57.44(6) . . ? C6 Re6 Re5 137.2(3) . 2_666 ? S5 Re6 Re5 116.86(6) 2_666 2_666 ? S6 Re6 Re5 57.46(6) . 2_666 ? S8 Re6 Re5 57.59(5) 2_666 2_666 ? S7 Re6 Re5 116.72(6) . 2_666 ? Re5 Re6 Re5 89.76(2) . 2_666 ? C6 Re6 Re4 134.2(3) . 2_666 ? S5 Re6 Re4 56.77(6) 2_666 2_666 ? S6 Re6 Re4 117.55(6) . 2_666 ? S8 Re6 Re4 56.93(5) 2_666 2_666 ? S7 Re6 Re4 117.55(6) . 2_666 ? Re5 Re6 Re4 60.15(2) . 2_666 ? Re5 Re6 Re4 60.123(17) 2_666 2_666 ? C6 Re6 Re4 135.0(3) . . ? S5 Re6 Re4 117.88(6) 2_666 . ? S6 Re6 Re4 57.01(6) . . ? S8 Re6 Re4 117.69(6) 2_666 . ? S7 Re6 Re4 56.63(5) . . ? Re5 Re6 Re4 60.121(16) . . ? Re5 Re6 Re4 60.137(19) 2_666 . ? Re4 Re6 Re4 90.692(19) 2_666 . ? C6 Re6 Re6 177.9(2) . 2_666 ? S5 Re6 Re6 86.73(6) 2_666 2_666 ? S6 Re6 Re6 86.65(6) . 2_666 ? S8 Re6 Re6 86.71(6) 2_666 2_666 ? S7 Re6 Re6 86.42(6) . 2_666 ? Re5 Re6 Re6 44.887(13) . 2_666 ? Re5 Re6 Re6 44.877(14) 2_666 2_666 ? Re4 Re6 Re6 45.352(15) 2_666 2_666 ? Re4 Re6 Re6 45.340(14) . 2_666 ? Re4 S5 Re6 66.07(5) . 2_666 ? Re4 S5 Re5 65.67(6) . 2_666 ? Re6 S5 Re5 65.04(5) 2_666 2_666 ? Re4 S6 Re6 65.81(6) . . ? Re4 S6 Re5 65.65(6) . 2_666 ? Re6 S6 Re5 65.12(6) . 2_666 ? Re4 S7 Re5 65.72(6) . . ? Re4 S7 Re6 65.79(6) . . ? Re5 S7 Re6 64.88(6) . . ? Re4 S8 Re6 65.78(7) . 2_666 ? Re4 S8 Re5 65.56(6) . . ? Re6 S8 Re5 64.98(7) 2_666 . ? N4 C4 Re4 178.0(9) . . ? N5 C5 Re5 178.4(10) . . ? N6 C6 Re6 177.3(11) . . ? C13 P1 C25 110.1(5) . . ? C13 P1 C7 107.2(4) . . ? C25 P1 C7 112.0(4) . . ? C13 P1 C19 109.7(5) . . ? C25 P1 C19 108.5(5) . . ? C7 P1 C19 109.2(5) . . ? C8 C7 C12 119.4(8) . . ? C8 C7 P1 118.0(7) . . ? C12 C7 P1 122.6(7) . . ? C9 C8 C7 120.9(9) . . ? C8 C9 C10 120.6(9) . . ? C9 C10 C11 119.4(9) . . ? C12 C11 C10 121.2(9) . . ? C11 C12 C7 118.5(9) . . ? C18 C13 C14 119.7(9) . . ? C18 C13 P1 121.8(8) . . ? C14 C13 P1 118.3(7) . . ? C15 C14 C13 119.7(9) . . ? C16 C15 C14 119.6(10) . . ? C17 C16 C15 121.5(10) . . ? C16 C17 C18 120.8(10) . . ? C17 C18 C13 118.7(10) . . ? C24 C19 C20 119.7(10) . . ? C24 C19 P1 121.7(7) . . ? C20 C19 P1 118.6(8) . . ? C21 C20 C19 119.0(11) . . ? C22 C21 C20 121.0(10) . . ? C21 C22 C23 120.8(11) . . ? C22 C23 C24 118.8(11) . . ? C19 C24 C23 120.7(10) . . ? C30 C25 C26 118.1(9) . . ? C30 C25 P1 122.7(9) . . ? C26 C25 P1 119.1(8) . . ? C27 C26 C25 119.2(11) . . ? C28 C27 C26 120.9(12) . . ? C27 C28 C29 121.9(11) . . ? C28 C29 C30 117.8(12) . . ? C25 C30 C29 122.0(12) . . ? C37 P2 C49 111.8(5) . . ? C37 P2 C31 109.7(5) . . ? C49 P2 C31 108.5(4) . . ? C37 P2 C43 108.7(5) . . ? C49 P2 C43 111.0(4) . . ? C31 P2 C43 107.0(5) . . ? C32 C31 C36 121.0(9) . . ? C32 C31 P2 118.9(7) . . ? C36 C31 P2 119.2(8) . . ? C33 C32 C31 119.7(9) . . ? C32 C33 C34 119.5(10) . . ? C35 C34 C33 120.1(9) . . ? C34 C35 C36 121.7(9) . . ? C35 C36 C31 117.9(10) . . ? C42 C37 C38 120.2(10) . . ? C42 C37 P2 121.1(9) . . ? C38 C37 P2 118.6(8) . . ? C39 C38 C37 119.4(11) . . ? C39 C40 C41 120.4(12) . . ? C40 C39 C38 121.0(13) . . ? C40 C41 C42 120.1(12) . . ? C37 C42 C41 118.9(12) . . ? C44 C43 C48 119.7(10) . . ? C44 C43 P2 119.6(7) . . ? C48 C43 P2 120.5(9) . . ? C43 C44 C45 121.2(10) . . ? C47 C46 C45 120.8(12) . . ? C46 C45 C44 118.8(12) . . ? C46 C47 C48 121.0(11) . . ? C47 C48 C43 118.4(11) . . ? C50 C49 C54 119.7(9) . . ? C50 C49 P2 120.6(7) . . ? C54 C49 P2 119.7(7) . . ? C49 C50 C51 119.8(10) . . ? C52 C51 C50 119.9(11) . . ? C51 C52 C53 120.2(10) . . ? C52 C53 C54 121.2(11) . . ? C53 C54 C49 119.0(11) . . ? C73 P3 C55 107.4(5) . . ? C73 P3 C61 111.2(5) . . ? C55 P3 C61 110.6(5) . . ? C73 P3 C67 110.8(5) . . ? C55 P3 C67 109.4(5) . . ? C61 P3 C67 107.4(4) . . ? C56 C55 C60 119.6(9) . . ? C56 C55 P3 119.5(8) . . ? C60 C55 P3 120.9(8) . . ? C55 C56 C57 120.2(10) . . ? C56 C57 C58 120.9(10) . . ? C59 C58 C57 117.8(11) . . ? C60 C59 C58 122.1(11) . . ? C59 C60 C55 119.3(10) . . ? C66 C61 C62 120.0(9) . . ? C66 C61 P3 121.6(7) . . ? C62 C61 P3 118.4(8) . . ? C63 C62 C61 119.3(11) . . ? C64 C63 C62 120.3(10) . . ? C63 C64 C65 120.6(9) . . ? C64 C65 C66 119.3(11) . . ? C61 C66 C65 120.4(10) . . ? C72 C67 C68 119.5(10) . . ? C72 C67 P3 118.9(8) . . ? C68 C67 P3 121.5(8) . . ? C69 C68 C67 120.1(10) . . ? C70 C69 C68 120.4(11) . . ? C69 C70 C71 119.9(11) . . ? C70 C71 C72 119.8(12) . . ? C67 C72 C71 120.3(11) . . ? C74 C73 C78 118.5(10) . . ? C74 C73 P3 117.9(8) . . ? C78 C73 P3 123.6(7) . . ? C75 C74 C73 120.3(10) . . ? C74 C75 C76 120.8(10) . . ? C77 C76 C75 118.9(12) . . ? C78 C77 C76 121.8(12) . . ? C77 C78 C73 119.7(10) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 3.178 _refine_diff_density_min -3.011 _refine_diff_density_rms 0.274 #################### Material relevant to compound 2 at 150K ############ data_sb150k_fac _database_code_CSD 186996 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(PPh4)3 (Re6S8(CN)6)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H60 N6 P3 Re6 S8' _chemical_formula_weight 2547.91 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' 'P' 'P' 0.1023 0.0942 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8186(16) _cell_length_b 15.1117(16) _cell_length_c 19.803(2) _cell_angle_alpha 92.685(13) _cell_angle_beta 108.774(13) _cell_angle_gamma 100.383(13) _cell_volume 3826.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2310 _exptl_crystal_size_mid 0.1924 _exptl_crystal_size_min 0.1924 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2386 _exptl_absorpt_coefficient_mu 9.780 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1524 _exptl_absorpt_correction_T_max 0.2598 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, Phi. incr. == 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38630 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.92 _reflns_number_total 13904 _reflns_number_gt 10748 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE, [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0385P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00035(2) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13904 _refine_ls_number_parameters 896 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _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 0.87467(3) 0.01500(2) 0.007426(17) 0.01225(8) Uani 1 1 d . . . Re2 Re 1.04236(3) 0.12316(2) 0.005131(17) 0.01230(8) Uani 1 1 d . . . Re3 Re 1.05578(3) 0.00613(2) 0.099041(17) 0.01219(8) Uani 1 1 d . . . S1 S 0.79316(17) -0.10559(14) -0.09017(11) 0.0173(4) Uani 1 1 d . . . S2 S 0.97653(17) 0.13420(14) 0.10255(11) 0.0167(4) Uani 1 1 d . . . S3 S 0.87079(17) 0.12065(14) -0.07985(11) 0.0164(4) Uani 1 1 d . . . S4 S 0.89647(17) -0.09399(14) 0.09268(11) 0.0164(4) Uani 1 1 d . . . C3 C 1.1125(7) 0.0080(6) 0.2135(5) 0.0186(19) Uani 1 1 d . . . C1 C 0.7361(7) 0.0358(6) 0.0239(4) 0.0149(17) Uani 1 1 d . . . C2 C 1.0880(8) 0.2656(6) 0.0076(5) 0.024(2) Uani 1 1 d . . . N2 N 1.1174(7) 0.3414(5) 0.0112(4) 0.0282(19) Uani 1 1 d . . . N1 N 0.6666(7) 0.0495(6) 0.0377(4) 0.030(2) Uani 1 1 d . . . N3 N 1.1335(7) 0.0062(6) 0.2725(4) 0.034(2) Uani 1 1 d . . . Re4 Re 0.35802(3) 0.46392(2) 0.485342(17) 0.01261(8) Uani 1 1 d . . . Re5 Re 0.48195(3) 0.43551(2) 0.415025(17) 0.01265(8) Uani 1 1 d . . . Re6 Re 0.47506(3) 0.59979(2) 0.453091(17) 0.01290(8) Uani 1 1 d . . . S5 S 0.40846(17) 0.43376(14) 0.60778(11) 0.0169(4) Uani 1 1 d . . . S6 S 0.36337(17) 0.61896(14) 0.52187(11) 0.0178(5) Uani 1 1 d . . . S7 S 0.32894(17) 0.49857(15) 0.36476(11) 0.0173(4) Uani 1 1 d . . . S8 S 0.37523(17) 0.31469(14) 0.45115(11) 0.0170(4) Uani 1 1 d . . . C4 C 0.1958(8) 0.4246(6) 0.4685(5) 0.023(2) Uani 1 1 d . . . C5 C 0.4648(7) 0.3618(6) 0.3165(5) 0.0186(19) Uani 1 1 d . . . C6 C 0.4444(6) 0.7121(6) 0.3947(5) 0.0184(19) Uani 1 1 d . . . N6 N 0.4264(7) 0.7690(6) 0.3616(5) 0.034(2) Uani 1 1 d . . . N4 N 0.1085(6) 0.4036(6) 0.4571(4) 0.0285(18) Uani 1 1 d . . . N5 N 0.4567(6) 0.3231(5) 0.2643(4) 0.0272(19) Uani 1 1 d . . . P1 P 0.95786(18) 0.43745(15) 0.18753(12) 0.0165(5) Uani 1 1 d . . . C7 C 1.0501(7) 0.3664(6) 0.2199(5) 0.0180(19) Uani 1 1 d . . . C8 C 1.1133(7) 0.3541(6) 0.1792(5) 0.0201(19) Uani 1 1 d . . . H8 H 1.1054 0.3812 0.1371 0.024 Uiso 1 1 calc R . . C9 C 1.1877(7) 0.3017(6) 0.2014(5) 0.0215(19) Uani 1 1 d . . . H9 H 1.2324 0.2964 0.1756 0.026 Uiso 1 1 calc R . . C10 C 1.1956(7) 0.2575(6) 0.2612(5) 0.0229(19) Uiso 1 1 d . . . H10 H 1.2431 0.2198 0.2747 0.028 Uiso 1 1 calc R . . C11 C 1.1328(8) 0.2692(6) 0.3011(5) 0.026(2) Uani 1 1 d . . . H11 H 1.1399 0.2402 0.3423 0.031 Uiso 1 1 calc R . . C12 C 1.0602(8) 0.3225(6) 0.2818(5) 0.024(2) Uani 1 1 d . . . H12 H 1.0183 0.3294 0.3094 0.029 Uiso 1 1 calc R . . C13 C 0.8889(7) 0.3993(6) 0.0939(5) 0.0186(19) Uani 1 1 d . . . C14 C 0.8358(8) 0.3091(6) 0.0751(5) 0.025(2) Uani 1 1 d . . . H14 H 0.8322 0.2716 0.1105 0.030 Uiso 1 1 calc R . . C15 C 0.7892(8) 0.2764(6) 0.0044(5) 0.026(2) Uani 1 1 d . . . H15 H 0.7528 0.2167 -0.0086 0.031 Uiso 1 1 calc R . . C16 C 0.7962(8) 0.3331(7) -0.0485(5) 0.029(2) Uani 1 1 d . . . H16 H 0.7659 0.3101 -0.0967 0.034 Uiso 1 1 calc R . . C17 C 0.8457(8) 0.4194(7) -0.0308(5) 0.033(3) Uani 1 1 d . . . H17 H 0.8473 0.4563 -0.0669 0.040 Uiso 1 1 calc R . . C18 C 0.8954(7) 0.4556(6) 0.0409(5) 0.0214(19) Uani 1 1 d . . . H18 H 0.9317 0.5154 0.0530 0.026 Uiso 1 1 calc R . . C19 C 1.0284(7) 0.5536(6) 0.1985(5) 0.0177(18) Uani 1 1 d . . . C20 C 0.9704(8) 0.6209(6) 0.1809(6) 0.029(2) Uani 1 1 d . . . H20 H 0.8978 0.6055 0.1651 0.035 Uiso 1 1 calc R . . C21 C 1.0197(10) 0.7096(7) 0.1869(5) 0.035(3) Uani 1 1 d . . . H21 H 0.9807 0.7539 0.1736 0.042 Uiso 1 1 calc R . . C22 C 1.1276(8) 0.7331(7) 0.2127(5) 0.029(2) Uiso 1 1 d . . . H22 H 1.1616 0.7933 0.2186 0.035 Uiso 1 1 calc R . . C23 C 1.1838(9) 0.6661(7) 0.2294(5) 0.032(2) Uani 1 1 d . . . H23 H 1.2564 0.6814 0.2458 0.038 Uiso 1 1 calc R . . C24 C 1.1344(8) 0.5759(6) 0.2223(5) 0.026(2) Uani 1 1 d . . . H24 H 1.1734 0.5313 0.2338 0.031 Uiso 1 1 calc R . . C25 C 0.8678(7) 0.4320(6) 0.2366(5) 0.024(2) Uani 1 1 d . . . C26 C 0.9076(9) 0.4513(6) 0.3105(5) 0.030(2) Uani 1 1 d . . . H26 H 0.9794 0.4665 0.3342 0.036 Uiso 1 1 calc R . . C27 C 0.8394(9) 0.4476(8) 0.3487(6) 0.039(3) Uani 1 1 d . . . H27 H 0.8660 0.4590 0.3984 0.047 Uiso 1 1 calc R . . C28 C 0.7350(11) 0.4278(8) 0.3152(7) 0.052(4) Uani 1 1 d . . . H28 H 0.6902 0.4271 0.3417 0.062 Uiso 1 1 calc R . . C29 C 0.6947(9) 0.4083(8) 0.2411(7) 0.043(3) Uani 1 1 d . . . H29 H 0.6228 0.3941 0.2179 0.052 Uiso 1 1 calc R . . C30 C 0.7608(7) 0.4100(7) 0.2016(6) 0.031(2) Uani 1 1 d . . . H30 H 0.7338 0.3964 0.1519 0.037 Uiso 1 1 calc R . . P2 P 0.55988(18) 0.76054(15) 0.13989(12) 0.0178(5) Uani 1 1 d . . . C31 C 0.5653(7) 0.7640(6) 0.0504(5) 0.023(2) Uani 1 1 d . . . C32 C 0.4833(8) 0.7824(6) -0.0033(5) 0.024(2) Uani 1 1 d . . . H32 H 0.4306 0.8034 0.0082 0.029 Uiso 1 1 calc R . . C33 C 0.4767(8) 0.7704(7) -0.0749(5) 0.030(2) Uani 1 1 d . . . H33 H 0.4187 0.7794 -0.1116 0.036 Uiso 1 1 calc R . . C34 C 0.5617(9) 0.7437(6) -0.0897(5) 0.033(3) Uani 1 1 d . . . H34 H 0.5606 0.7367 -0.1368 0.040 Uiso 1 1 calc R . . C35 C 0.6443(8) 0.7285(6) -0.0359(5) 0.026(2) Uani 1 1 d . . . H35 H 0.6987 0.7105 -0.0471 0.032 Uiso 1 1 calc R . . C36 C 0.6506(8) 0.7392(6) 0.0362(5) 0.026(2) Uani 1 1 d . . . H36 H 0.7086 0.7301 0.0729 0.031 Uiso 1 1 calc R . . C37 C 0.6892(7) 0.7693(6) 0.2037(5) 0.021(2) Uani 1 1 d . . . C38 C 0.7598(8) 0.8515(7) 0.2180(6) 0.032(3) Uani 1 1 d . . . H38 H 0.7390 0.9021 0.1975 0.038 Uiso 1 1 calc R . . C40 C 0.8907(9) 0.7832(8) 0.2943(6) 0.040(3) Uani 1 1 d . . . H40 H 0.9594 0.7887 0.3244 0.048 Uiso 1 1 calc R . . C39 C 0.8598(8) 0.8574(7) 0.2624(5) 0.032(2) Uani 1 1 d . . . H39 H 0.9078 0.9119 0.2712 0.039 Uiso 1 1 calc R . . C41 C 0.8234(10) 0.7027(9) 0.2829(7) 0.047(3) Uani 1 1 d . . . H41 H 0.8444 0.6539 0.3062 0.056 Uiso 1 1 calc R . . C42 C 0.7218(8) 0.6944(7) 0.2355(5) 0.030(2) Uani 1 1 d . . . H42 H 0.6756 0.6386 0.2249 0.036 Uiso 1 1 calc R . . C43 C 0.4824(7) 0.6513(6) 0.1402(4) 0.0182(19) Uani 1 1 d . . . C44 C 0.4378(9) 0.5917(6) 0.0777(5) 0.031(2) Uani 1 1 d . . . H44 H 0.4460 0.6092 0.0352 0.037 Uiso 1 1 calc R . . C46 C 0.3671(8) 0.4815(7) 0.1403(6) 0.037(3) Uani 1 1 d . . . H46 H 0.3269 0.4248 0.1395 0.045 Uiso 1 1 calc R . . C45 C 0.3818(9) 0.5075(7) 0.0783(6) 0.037(3) Uani 1 1 d . . . H45 H 0.3535 0.4677 0.0364 0.044 Uiso 1 1 calc R . . C47 C 0.4113(9) 0.5386(7) 0.2040(6) 0.039(3) Uani 1 1 d . . . H47 H 0.4023 0.5200 0.2461 0.046 Uiso 1 1 calc R . . C48 C 0.4683(8) 0.6227(6) 0.2040(5) 0.026(2) Uani 1 1 d . . . H48 H 0.4981 0.6615 0.2465 0.031 Uiso 1 1 calc R . . C49 C 0.5023(7) 0.8513(6) 0.1602(5) 0.0186(18) Uani 1 1 d . . . C50 C 0.5073(7) 0.9287(6) 0.1271(5) 0.024(2) Uani 1 1 d . . . H50 H 0.5434 0.9355 0.0947 0.028 Uiso 1 1 calc R . . C51 C 0.4597(8) 0.9967(6) 0.1412(5) 0.028(2) Uani 1 1 d . . . H51 H 0.4630 1.0484 0.1177 0.034 Uiso 1 1 calc R . . C52 C 0.4073(8) 0.9886(7) 0.1898(6) 0.038(3) Uani 1 1 d . . . H52 H 0.3761 1.0348 0.1999 0.045 Uiso 1 1 calc R . . C53 C 0.4018(8) 0.9099(7) 0.2237(6) 0.035(2) Uani 1 1 d . . . H53 H 0.3668 0.9036 0.2568 0.042 Uiso 1 1 calc R . . C54 C 0.4475(8) 0.8424(7) 0.2087(6) 0.034(3) Uani 1 1 d . . . H54 H 0.4422 0.7897 0.2309 0.041 Uiso 1 1 calc R . . P3 P 0.25950(18) 0.91181(15) 0.57690(12) 0.0178(5) Uani 1 1 d . . . C55 C 0.3992(7) 0.9256(6) 0.5974(5) 0.0182(18) Uani 1 1 d . . . C56 C 0.4432(7) 0.8522(6) 0.6186(5) 0.0206(19) Uani 1 1 d . . . H56 H 0.4023 0.7983 0.6231 0.025 Uiso 1 1 calc R . . C57 C 0.5493(9) 0.8602(7) 0.6333(6) 0.035(2) Uani 1 1 d . . . H57 H 0.5805 0.8118 0.6487 0.042 Uiso 1 1 calc R . . C58 C 0.6095(8) 0.9401(6) 0.6250(5) 0.026(2) Uiso 1 1 d . . . H58 H 0.6806 0.9448 0.6339 0.031 Uiso 1 1 calc R . . C59 C 0.5643(8) 1.0119(7) 0.6037(6) 0.035(2) Uani 1 1 d . . . H59 H 0.6053 1.0657 0.5990 0.042 Uiso 1 1 calc R . . C60 C 0.4572(8) 1.0055(6) 0.5888(5) 0.029(2) Uani 1 1 d . . . H60 H 0.4261 1.0540 0.5735 0.035 Uiso 1 1 calc R . . C61 C 0.2250(7) 0.9012(6) 0.6573(5) 0.0182(18) Uani 1 1 d . . . C62 C 0.1247(8) 0.9045(7) 0.6542(5) 0.032(3) Uani 1 1 d . . . H62 H 0.0743 0.9091 0.6108 0.039 Uiso 1 1 calc R . . C63 C 0.1000(8) 0.9010(7) 0.7172(5) 0.031(2) Uani 1 1 d . . . H63 H 0.0325 0.9030 0.7158 0.038 Uiso 1 1 calc R . . C64 C 0.1738(9) 0.8946(8) 0.7806(6) 0.040(3) Uani 1 1 d . . . H64 H 0.1560 0.8911 0.8220 0.048 Uiso 1 1 calc R . . C65 C 0.2756(8) 0.8934(7) 0.7840(5) 0.034(2) Uani 1 1 d . . . H65 H 0.3261 0.8908 0.8279 0.041 Uiso 1 1 calc R . . C66 C 0.3020(8) 0.8959(7) 0.7223(5) 0.027(2) Uani 1 1 d . . . H66 H 0.3697 0.8942 0.7240 0.032 Uiso 1 1 calc R . . C67 C 0.2196(7) 1.0115(6) 0.5409(5) 0.0214(19) Uani 1 1 d . . . C68 C 0.1757(7) 1.0132(6) 0.4661(5) 0.0216(19) Uani 1 1 d . . . H68 H 0.1635 0.9615 0.4347 0.026 Uiso 1 1 calc R . . C69 C 0.1514(8) 1.0919(6) 0.4402(5) 0.026(2) Uani 1 1 d . . . H69 H 0.1214 1.0936 0.3911 0.032 Uiso 1 1 calc R . . C70 C 0.1721(8) 1.1707(7) 0.4887(5) 0.030(2) Uani 1 1 d . . . H70 H 0.1584 1.2248 0.4712 0.036 Uiso 1 1 calc R . . C71 C 0.2113(11) 1.1674(7) 0.5592(6) 0.048(3) Uani 1 1 d . . . H71 H 0.2220 1.2188 0.5906 0.057 Uiso 1 1 calc R . . C72 C 0.2362(10) 1.0883(7) 0.5867(5) 0.041(3) Uani 1 1 d . . . H72 H 0.2641 1.0873 0.6361 0.049 Uiso 1 1 calc R . . C73 C 0.1973(7) 0.8139(6) 0.5138(4) 0.0171(18) Uani 1 1 d . . . C74 C 0.2382(7) 0.8010(6) 0.4588(5) 0.022(2) Uani 1 1 d . . . H74 H 0.2967 0.8410 0.4571 0.027 Uiso 1 1 calc R . . C75 C 0.1898(8) 0.7271(7) 0.4069(5) 0.028(2) Uani 1 1 d . . . H75 H 0.2156 0.7186 0.3696 0.034 Uiso 1 1 calc R . . C76 C 0.1051(9) 0.6670(7) 0.4097(6) 0.037(3) Uani 1 1 d . . . H76 H 0.0728 0.6181 0.3744 0.045 Uiso 1 1 calc R . . C77 C 0.0683(9) 0.6796(7) 0.4650(6) 0.042(3) Uani 1 1 d . . . H77 H 0.0120 0.6373 0.4677 0.050 Uiso 1 1 calc R . . C78 C 0.1107(8) 0.7508(7) 0.5155(6) 0.032(2) Uani 1 1 d . . . H78 H 0.0825 0.7583 0.5517 0.038 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 Re1 0.01335(17) 0.01334(16) 0.01106(16) 0.00325(13) 0.00591(14) 0.00140(13) Re2 0.01448(18) 0.01168(15) 0.01126(16) 0.00319(13) 0.00576(15) 0.00081(13) Re3 0.01365(17) 0.01317(16) 0.00991(16) 0.00284(13) 0.00499(14) 0.00086(13) S1 0.0180(11) 0.0162(10) 0.0163(11) 0.0028(9) 0.0056(10) 0.0003(9) S2 0.0202(12) 0.0174(10) 0.0136(10) -0.0003(9) 0.0076(10) 0.0033(9) S3 0.0194(11) 0.0159(10) 0.0157(10) 0.0073(9) 0.0068(10) 0.0052(9) S4 0.0192(11) 0.0178(10) 0.0141(10) 0.0064(9) 0.0082(10) 0.0024(9) C3 0.012(4) 0.018(4) 0.025(5) 0.003(4) 0.008(4) -0.002(4) C1 0.012(4) 0.020(4) 0.006(4) -0.003(4) -0.004(4) 0.001(4) C2 0.036(6) 0.022(5) 0.022(5) 0.010(4) 0.018(5) 0.013(4) N2 0.042(5) 0.017(4) 0.026(5) 0.009(4) 0.013(4) 0.003(4) N1 0.033(5) 0.046(5) 0.017(4) 0.011(4) 0.013(4) 0.010(4) N3 0.035(5) 0.049(6) 0.016(4) 0.003(4) 0.008(4) 0.009(5) Re4 0.01359(17) 0.01469(16) 0.01067(16) 0.00337(13) 0.00617(15) 0.00133(14) Re5 0.01470(18) 0.01448(16) 0.00994(16) 0.00285(13) 0.00632(15) 0.00149(14) Re6 0.01525(18) 0.01379(16) 0.01132(16) 0.00455(13) 0.00665(15) 0.00234(14) S5 0.0201(11) 0.0193(10) 0.0127(10) 0.0047(9) 0.0088(10) 0.0008(9) S6 0.0206(12) 0.0203(11) 0.0166(11) 0.0043(9) 0.0093(10) 0.0080(9) S7 0.0141(11) 0.0235(11) 0.0111(10) 0.0036(9) 0.0010(9) 0.0018(9) S8 0.0182(11) 0.0146(10) 0.0173(11) 0.0019(9) 0.0076(10) -0.0018(9) C4 0.031(6) 0.028(5) 0.015(5) 0.007(4) 0.013(5) 0.011(5) C5 0.028(5) 0.017(4) 0.016(5) 0.002(4) 0.016(4) 0.001(4) C6 0.005(4) 0.026(5) 0.019(5) 0.000(4) -0.001(4) 0.004(4) N6 0.034(5) 0.025(4) 0.042(5) 0.011(4) 0.013(5) 0.004(4) N4 0.009(4) 0.042(5) 0.021(4) -0.003(4) -0.006(4) -0.009(4) N5 0.031(5) 0.030(4) 0.027(5) 0.005(4) 0.020(4) 0.001(4) P1 0.0159(12) 0.0180(11) 0.0155(11) 0.0038(9) 0.0062(10) 0.0009(9) C7 0.025(5) 0.014(4) 0.018(4) 0.006(4) 0.010(4) 0.006(4) C8 0.024(5) 0.018(4) 0.024(5) 0.009(4) 0.013(4) 0.005(4) C9 0.013(5) 0.021(5) 0.027(5) 0.000(4) 0.003(4) 0.002(4) C11 0.031(6) 0.020(5) 0.014(5) 0.009(4) -0.005(4) -0.004(4) C12 0.031(6) 0.020(5) 0.021(5) 0.007(4) 0.010(5) 0.003(4) C13 0.022(5) 0.021(4) 0.017(4) 0.007(4) 0.010(4) 0.007(4) C14 0.040(6) 0.021(5) 0.028(5) 0.014(4) 0.026(5) 0.013(4) C15 0.028(5) 0.023(5) 0.031(5) -0.001(4) 0.016(5) 0.004(4) C16 0.035(6) 0.034(6) 0.021(5) 0.003(4) 0.015(5) 0.009(5) C17 0.042(7) 0.039(6) 0.028(5) 0.025(5) 0.020(5) 0.013(5) C18 0.024(5) 0.019(4) 0.019(5) 0.008(4) 0.006(4) 0.001(4) C19 0.022(5) 0.017(4) 0.018(4) 0.006(4) 0.011(4) 0.003(4) C20 0.034(6) 0.023(5) 0.038(6) 0.014(5) 0.018(5) 0.013(5) C21 0.063(8) 0.024(5) 0.028(6) 0.014(5) 0.020(6) 0.021(5) C23 0.032(6) 0.035(6) 0.020(5) 0.000(5) 0.009(5) -0.013(5) C24 0.046(7) 0.024(5) 0.021(5) 0.013(4) 0.022(5) 0.017(5) C25 0.028(5) 0.027(5) 0.026(5) 0.005(4) 0.018(5) 0.008(4) C26 0.043(6) 0.026(5) 0.030(6) 0.004(4) 0.024(5) 0.009(5) C27 0.046(7) 0.043(6) 0.036(6) 0.001(5) 0.023(6) 0.009(6) C28 0.063(9) 0.050(7) 0.065(9) 0.011(7) 0.051(8) 0.016(7) C29 0.029(6) 0.054(7) 0.044(7) -0.007(6) 0.016(6) -0.004(6) C30 0.012(5) 0.044(6) 0.028(6) -0.014(5) 0.002(5) -0.003(5) P2 0.0201(12) 0.0191(11) 0.0140(11) 0.0045(9) 0.0067(10) 0.0009(10) C31 0.030(5) 0.021(4) 0.031(5) 0.018(4) 0.022(5) 0.009(4) C32 0.032(6) 0.025(5) 0.024(5) 0.009(4) 0.016(5) 0.016(4) C33 0.032(6) 0.032(5) 0.025(5) 0.010(5) 0.010(5) 0.002(5) C34 0.061(8) 0.026(5) 0.028(6) 0.015(5) 0.032(6) 0.014(5) C35 0.036(6) 0.023(5) 0.025(5) 0.000(4) 0.019(5) -0.001(4) C36 0.029(5) 0.019(5) 0.032(5) 0.007(4) 0.017(5) -0.002(4) C37 0.022(5) 0.023(5) 0.020(5) 0.003(4) 0.012(4) 0.003(4) C38 0.043(7) 0.033(5) 0.034(6) 0.009(5) 0.028(6) 0.015(5) C40 0.034(7) 0.060(8) 0.030(6) 0.006(6) 0.009(6) 0.021(6) C39 0.021(5) 0.038(6) 0.025(5) -0.009(5) -0.002(5) -0.004(5) C41 0.055(8) 0.050(8) 0.044(7) 0.018(6) 0.015(7) 0.032(7) C42 0.023(5) 0.033(6) 0.027(5) 0.004(5) 0.000(5) 0.003(5) C43 0.021(5) 0.023(5) 0.011(4) 0.007(4) 0.006(4) 0.004(4) C44 0.048(7) 0.022(5) 0.026(5) 0.007(4) 0.017(5) 0.006(5) C46 0.032(6) 0.029(6) 0.039(7) 0.007(5) 0.008(6) -0.015(5) C45 0.054(7) 0.022(5) 0.023(5) -0.001(4) 0.007(6) -0.013(5) C47 0.046(7) 0.032(6) 0.044(7) 0.009(5) 0.025(6) 0.003(5) C48 0.040(6) 0.027(5) 0.012(4) 0.006(4) 0.014(5) 0.000(5) C49 0.012(4) 0.020(4) 0.012(4) -0.004(4) -0.008(4) -0.004(4) C50 0.017(5) 0.027(5) 0.014(5) -0.005(4) -0.008(4) -0.004(4) C51 0.034(6) 0.023(5) 0.014(5) -0.004(4) -0.005(5) -0.003(5) C52 0.027(6) 0.036(6) 0.032(6) -0.016(5) -0.015(5) 0.011(5) C53 0.030(6) 0.040(6) 0.035(6) -0.001(5) 0.018(5) -0.002(5) C54 0.041(7) 0.034(6) 0.036(6) 0.010(5) 0.026(6) 0.005(5) P3 0.0184(12) 0.0209(11) 0.0133(11) 0.0016(9) 0.0064(10) 0.0000(10) C55 0.018(5) 0.019(4) 0.015(4) -0.005(4) 0.006(4) -0.003(4) C56 0.010(4) 0.023(5) 0.018(5) -0.004(4) -0.002(4) -0.009(4) C57 0.037(6) 0.032(6) 0.039(6) 0.003(5) 0.016(6) 0.012(5) C59 0.022(5) 0.040(6) 0.031(6) -0.003(5) 0.007(5) -0.019(5) C60 0.040(6) 0.022(5) 0.028(5) 0.007(4) 0.016(5) 0.003(5) C61 0.017(5) 0.019(4) 0.015(4) 0.001(4) 0.005(4) -0.004(4) C62 0.040(6) 0.047(6) 0.025(5) 0.009(5) 0.023(5) 0.020(5) C63 0.031(6) 0.041(6) 0.026(5) 0.001(5) 0.018(5) 0.001(5) C64 0.057(8) 0.055(7) 0.032(6) 0.024(6) 0.038(6) 0.024(6) C65 0.034(6) 0.049(7) 0.014(5) 0.009(5) 0.004(5) 0.005(5) C66 0.028(6) 0.039(6) 0.018(5) 0.006(4) 0.013(5) 0.011(5) C67 0.016(5) 0.028(5) 0.019(5) 0.004(4) 0.005(4) 0.001(4) C68 0.016(5) 0.019(4) 0.022(5) -0.001(4) 0.002(4) -0.005(4) C69 0.024(5) 0.028(5) 0.020(5) 0.002(4) 0.003(5) -0.002(4) C70 0.042(6) 0.029(5) 0.026(5) 0.016(5) 0.019(5) 0.006(5) C71 0.094(11) 0.026(6) 0.045(7) 0.006(5) 0.047(8) 0.024(7) C72 0.086(10) 0.034(6) 0.021(5) 0.011(5) 0.033(6) 0.031(6) C73 0.013(4) 0.019(4) 0.010(4) -0.002(4) -0.002(4) -0.007(4) C74 0.015(5) 0.027(5) 0.017(5) -0.002(4) 0.003(4) -0.009(4) C75 0.031(6) 0.041(6) 0.008(4) -0.002(4) 0.004(4) 0.003(5) C76 0.045(7) 0.031(6) 0.036(6) -0.003(5) 0.016(6) 0.004(5) C77 0.044(7) 0.034(6) 0.050(7) -0.002(6) 0.028(7) -0.006(5) C78 0.038(6) 0.031(5) 0.038(6) 0.009(5) 0.030(6) 0.003(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 Re1 C1 2.117(8) . ? Re1 S4 2.4013(19) . ? Re1 S3 2.4018(19) . ? Re1 S2 2.416(2) . ? Re1 S1 2.419(2) . ? Re1 Re2 2.5949(5) 2_755 ? Re1 Re2 2.5987(6) . ? Re1 Re3 2.6066(6) . ? Re1 Re3 2.6121(5) 2_755 ? Re1 Re1 3.6742(7) 2_755 ? Re2 C2 2.125(9) . ? Re2 S2 2.3940(19) . ? Re2 S4 2.4020(19) 2_755 ? Re2 S3 2.418(2) . ? Re2 S1 2.422(2) 2_755 ? Re2 Re1 2.5949(5) 2_755 ? Re2 Re3 2.6036(7) 2_755 ? Re2 Re3 2.6125(5) . ? Re2 Re2 3.6706(8) 2_755 ? Re3 C3 2.144(9) . ? Re3 S3 2.3928(19) 2_755 ? Re3 S2 2.398(2) . ? Re3 S4 2.399(2) . ? Re3 S1 2.403(2) 2_755 ? Re3 Re2 2.6036(7) 2_755 ? Re3 Re1 2.6121(5) 2_755 ? Re3 Re3 3.7061(8) 2_755 ? S1 Re3 2.404(2) 2_755 ? S1 Re2 2.422(2) 2_755 ? S3 Re3 2.3928(19) 2_755 ? S4 Re2 2.4020(19) 2_755 ? C3 N3 1.113(12) . ? C1 N1 1.130(10) . ? C2 N2 1.135(12) . ? Re4 C4 2.124(10) . ? Re4 S5 2.388(2) . ? Re4 S7 2.390(2) . ? Re4 S8 2.399(2) . ? Re4 S6 2.401(2) . ? Re4 Re5 2.6061(7) 2_666 ? Re4 Re5 2.6077(5) . ? Re4 Re6 2.6134(6) . ? Re4 Re6 2.6142(6) 2_666 ? Re4 Re4 3.7222(8) 2_666 ? Re5 C5 2.123(8) . ? Re5 S6 2.412(2) 2_666 ? Re5 S7 2.414(2) . ? Re5 S5 2.418(2) 2_666 ? Re5 S8 2.419(2) . ? Re5 Re6 2.5877(5) . ? Re5 Re6 2.5894(5) 2_666 ? Re5 Re4 2.6061(7) 2_666 ? Re5 Re5 3.6509(8) 2_666 ? Re6 C6 2.127(9) . ? Re6 S5 2.4055(19) 2_666 ? Re6 S6 2.4080(19) . ? Re6 S8 2.414(2) 2_666 ? Re6 S7 2.416(2) . ? Re6 Re5 2.5894(5) 2_666 ? Re6 Re4 2.6142(6) 2_666 ? Re6 Re6 3.6706(8) 2_666 ? S5 Re6 2.4056(19) 2_666 ? S5 Re5 2.418(2) 2_666 ? S6 Re5 2.412(2) 2_666 ? S8 Re6 2.414(2) 2_666 ? C4 N4 1.134(12) . ? C5 N5 1.126(11) . ? C6 N6 1.121(11) . ? P1 C7 1.794(8) . ? P1 C13 1.800(9) . ? P1 C25 1.803(8) . ? P1 C19 1.814(9) . ? C7 C8 1.395(11) . ? C7 C12 1.400(11) . ? C8 C9 1.382(12) . ? C9 C10 1.371(12) . ? C10 C11 1.375(12) . ? C11 C12 1.369(13) . ? C13 C18 1.396(11) . ? C13 C14 1.397(13) . ? C14 C15 1.363(14) . ? C15 C16 1.400(13) . ? C16 C17 1.331(15) . ? C17 C18 1.398(14) . ? C19 C24 1.358(14) . ? C19 C20 1.394(12) . ? C20 C21 1.371(14) . ? C21 C22 1.382(15) . ? C22 C23 1.374(14) . ? C23 C24 1.388(14) . ? C25 C26 1.383(14) . ? C25 C30 1.386(13) . ? C26 C27 1.380(13) . ? C27 C28 1.349(18) . ? C28 C29 1.388(18) . ? C29 C30 1.378(13) . ? P2 C49 1.795(8) . ? P2 C43 1.800(9) . ? P2 C31 1.800(9) . ? P2 C37 1.804(10) . ? C31 C32 1.363(13) . ? C31 C36 1.404(12) . ? C32 C33 1.393(13) . ? C33 C34 1.416(13) . ? C34 C35 1.351(15) . ? C35 C36 1.401(13) . ? C37 C38 1.388(14) . ? C37 C42 1.396(12) . ? C38 C39 1.363(15) . ? C40 C41 1.352(17) . ? C40 C39 1.379(14) . ? C41 C42 1.394(16) . ? C43 C44 1.387(13) . ? C43 C48 1.416(11) . ? C44 C45 1.368(14) . ? C46 C45 1.370(14) . ? C46 C47 1.386(16) . ? C47 C48 1.369(14) . ? C49 C50 1.369(12) . ? C49 C54 1.398(12) . ? C50 C51 1.379(13) . ? C51 C52 1.376(14) . ? C52 C53 1.395(15) . ? C53 C54 1.363(13) . ? P3 C73 1.779(9) . ? P3 C67 1.796(9) . ? P3 C61 1.808(8) . ? P3 C55 1.810(9) . ? C55 C60 1.374(13) . ? C55 C56 1.378(12) . ? C56 C57 1.381(13) . ? C57 C58 1.385(14) . ? C58 C59 1.364(14) . ? C59 C60 1.397(14) . ? C61 C62 1.378(13) . ? C61 C66 1.398(13) . ? C62 C63 1.397(12) . ? C63 C64 1.359(15) . ? C64 C65 1.391(14) . ? C65 C66 1.384(12) . ? C67 C72 1.376(13) . ? C67 C68 1.412(12) . ? C68 C69 1.372(12) . ? C69 C70 1.419(14) . ? C70 C71 1.333(15) . ? C71 C72 1.390(14) . ? C73 C78 1.400(13) . ? C73 C74 1.401(11) . ? C74 C75 1.389(14) . ? C75 C76 1.365(15) . ? C76 C77 1.367(14) . ? C77 C78 1.340(15) . ? 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 C1 Re1 S4 91.4(2) . . ? C1 Re1 S3 95.2(2) . . ? S4 Re1 S3 173.41(7) . . ? C1 Re1 S2 90.2(2) . . ? S4 Re1 S2 89.87(7) . . ? S3 Re1 S2 90.22(7) . . ? C1 Re1 S1 97.0(2) . . ? S4 Re1 S1 90.42(7) . . ? S3 Re1 S1 88.67(7) . . ? S2 Re1 S1 172.77(7) . . ? C1 Re1 Re2 136.1(2) . 2_755 ? S4 Re1 Re2 57.31(5) . 2_755 ? S3 Re1 Re2 117.03(5) . 2_755 ? S2 Re1 Re2 116.89(5) . 2_755 ? S1 Re1 Re2 57.65(5) . 2_755 ? C1 Re1 Re2 133.7(2) . . ? S4 Re1 Re2 117.27(6) . . ? S3 Re1 Re2 57.68(6) . . ? S2 Re1 Re2 56.89(5) . . ? S1 Re1 Re2 116.84(5) . . ? Re2 Re1 Re2 89.945(17) 2_755 . ? C1 Re1 Re3 130.7(2) . . ? S4 Re1 Re3 57.07(5) . . ? S3 Re1 Re3 117.89(6) . . ? S2 Re1 Re3 56.88(5) . . ? S1 Re1 Re3 117.67(5) . . ? Re2 Re1 Re3 60.073(18) 2_755 . ? Re2 Re1 Re3 60.251(16) . . ? C1 Re1 Re3 138.7(2) . 2_755 ? S4 Re1 Re3 117.51(5) . 2_755 ? S3 Re1 Re3 56.82(5) . 2_755 ? S2 Re1 Re3 116.81(5) . 2_755 ? S1 Re1 Re3 56.91(5) . 2_755 ? Re2 Re1 Re3 60.229(15) 2_755 2_755 ? Re2 Re1 Re3 59.955(17) . 2_755 ? Re3 Re1 Re3 90.495(17) . 2_755 ? C1 Re1 Re1 175.9(2) . 2_755 ? S4 Re1 Re1 86.71(5) . 2_755 ? S3 Re1 Re1 86.72(5) . 2_755 ? S2 Re1 Re1 86.16(5) . 2_755 ? S1 Re1 Re1 86.64(5) . 2_755 ? Re2 Re1 Re1 45.014(13) 2_755 2_755 ? Re2 Re1 Re1 44.930(12) . 2_755 ? Re3 Re1 Re1 45.308(12) . 2_755 ? Re3 Re1 Re1 45.187(14) 2_755 2_755 ? C2 Re2 S2 94.0(2) . . ? C2 Re2 S4 92.4(2) . 2_755 ? S2 Re2 S4 173.57(7) . 2_755 ? C2 Re2 S3 92.1(3) . . ? S2 Re2 S3 90.35(7) . . ? S4 Re2 S3 89.69(7) 2_755 . ? C2 Re2 S1 95.1(3) . 2_755 ? S2 Re2 S1 88.83(7) . 2_755 ? S4 Re2 S1 90.33(7) 2_755 2_755 ? S3 Re2 S1 172.85(7) . 2_755 ? C2 Re2 Re1 135.4(2) . 2_755 ? S2 Re2 Re1 117.22(5) . 2_755 ? S4 Re2 Re1 57.29(5) 2_755 2_755 ? S3 Re2 Re1 116.90(5) . 2_755 ? S1 Re2 Re1 57.54(5) 2_755 2_755 ? C2 Re2 Re1 134.4(2) . . ? S2 Re2 Re1 57.70(6) . . ? S4 Re2 Re1 117.33(6) 2_755 . ? S3 Re2 Re1 57.07(5) . . ? S1 Re2 Re1 116.87(5) 2_755 . ? Re1 Re2 Re1 90.055(17) 2_755 . ? C2 Re2 Re3 132.8(3) . 2_755 ? S2 Re2 Re3 117.94(6) . 2_755 ? S4 Re2 Re3 57.10(6) 2_755 2_755 ? S3 Re2 Re3 56.77(5) . 2_755 ? S1 Re2 Re3 117.68(5) 2_755 2_755 ? Re1 Re2 Re3 60.187(16) 2_755 2_755 ? Re1 Re2 Re3 60.277(17) . 2_755 ? C2 Re2 Re3 136.6(3) . . ? S2 Re2 Re3 57.03(5) . . ? S4 Re2 Re3 117.46(5) 2_755 . ? S3 Re2 Re3 117.05(5) . . ? S1 Re2 Re3 56.87(5) 2_755 . ? Re1 Re2 Re3 60.211(14) 2_755 . ? Re1 Re2 Re3 60.025(16) . . ? Re3 Re2 Re3 90.551(18) 2_755 . ? C2 Re2 Re2 178.1(3) . 2_755 ? S2 Re2 Re2 86.85(5) . 2_755 ? S4 Re2 Re2 86.73(5) 2_755 2_755 ? S3 Re2 Re2 86.27(5) . 2_755 ? S1 Re2 Re2 86.59(5) 2_755 2_755 ? Re1 Re2 Re2 45.070(11) 2_755 2_755 ? Re1 Re2 Re2 44.986(13) . 2_755 ? Re3 Re2 Re2 45.374(14) 2_755 2_755 ? Re3 Re2 Re2 45.177(13) . 2_755 ? C3 Re3 S3 93.3(2) . 2_755 ? C3 Re3 S2 93.8(2) . . ? S3 Re3 S2 172.89(7) 2_755 . ? C3 Re3 S4 90.3(2) . . ? S3 Re3 S4 90.37(7) 2_755 . ? S2 Re3 S4 90.35(7) . . ? C3 Re3 S1 96.5(2) . 2_755 ? S3 Re3 S1 89.26(7) 2_755 2_755 ? S2 Re3 S1 89.19(7) . 2_755 ? S4 Re3 S1 173.20(7) . 2_755 ? C3 Re3 Re2 132.8(2) . 2_755 ? S3 Re3 Re2 57.71(6) 2_755 2_755 ? S2 Re3 Re2 117.22(6) . 2_755 ? S4 Re3 Re2 57.21(5) . 2_755 ? S1 Re3 Re2 117.24(5) 2_755 2_755 ? C3 Re3 Re1 132.9(2) . . ? S3 Re3 Re1 117.39(6) 2_755 . ? S2 Re3 Re1 57.55(6) . . ? S4 Re3 Re1 57.15(5) . . ? S1 Re3 Re1 117.27(5) 2_755 . ? Re2 Re3 Re1 59.740(17) 2_755 . ? C3 Re3 Re1 137.5(2) . 2_755 ? S3 Re3 Re1 57.16(5) 2_755 2_755 ? S2 Re3 Re1 116.43(5) . 2_755 ? S4 Re3 Re1 116.93(5) . 2_755 ? S1 Re3 Re1 57.50(5) 2_755 2_755 ? Re2 Re3 Re1 59.767(16) 2_755 2_755 ? Re1 Re3 Re1 89.505(17) . 2_755 ? C3 Re3 Re2 137.7(2) . . ? S3 Re3 Re2 116.69(5) 2_755 . ? S2 Re3 Re2 56.89(5) . . ? S4 Re3 Re2 116.83(5) . . ? S1 Re3 Re2 57.57(5) 2_755 . ? Re2 Re3 Re2 89.449(18) 2_755 . ? Re1 Re3 Re2 59.724(17) . . ? Re1 Re3 Re2 59.559(14) 2_755 . ? C3 Re3 Re3 176.8(2) . 2_755 ? S3 Re3 Re3 86.64(5) 2_755 2_755 ? S2 Re3 Re3 86.34(5) . 2_755 ? S4 Re3 Re3 86.43(5) . 2_755 ? S1 Re3 Re3 86.77(5) 2_755 2_755 ? Re2 Re3 Re3 44.821(14) 2_755 2_755 ? Re1 Re3 Re3 44.812(13) . 2_755 ? Re1 Re3 Re3 44.693(12) 2_755 2_755 ? Re2 Re3 Re3 44.628(14) . 2_755 ? Re3 S1 Re1 65.58(6) 2_755 . ? Re3 S1 Re2 65.55(6) 2_755 2_755 ? Re1 S1 Re2 64.81(6) . 2_755 ? Re2 S2 Re3 66.08(5) . . ? Re2 S2 Re1 65.40(5) . . ? Re3 S2 Re1 65.57(5) . . ? Re3 S3 Re1 66.02(5) 2_755 . ? Re3 S3 Re2 65.53(5) 2_755 . ? Re1 S3 Re2 65.25(5) . . ? Re3 S4 Re1 65.78(5) . . ? Re3 S4 Re2 65.68(5) . 2_755 ? Re1 S4 Re2 65.40(5) . 2_755 ? N3 C3 Re3 174.2(8) . . ? N1 C1 Re1 174.9(8) . . ? N2 C2 Re2 176.5(10) . . ? C4 Re4 S5 93.7(2) . . ? C4 Re4 S7 93.0(2) . . ? S5 Re4 S7 173.27(7) . . ? C4 Re4 S8 94.2(2) . . ? S5 Re4 S8 89.38(7) . . ? S7 Re4 S8 89.86(7) . . ? C4 Re4 S6 92.9(2) . . ? S5 Re4 S6 90.21(7) . . ? S7 Re4 S6 89.73(7) . . ? S8 Re4 S6 172.94(7) . . ? C4 Re4 Re5 135.2(2) . 2_666 ? S5 Re4 Re5 57.71(6) . 2_666 ? S7 Re4 Re5 116.99(6) . 2_666 ? S8 Re4 Re5 116.78(6) . 2_666 ? S6 Re4 Re5 57.43(6) . 2_666 ? C4 Re4 Re5 135.9(2) . . ? S5 Re4 Re5 116.70(5) . . ? S7 Re4 Re5 57.58(5) . . ? S8 Re4 Re5 57.60(5) . . ? S6 Re4 Re5 116.59(5) . . ? Re5 Re4 Re5 88.892(18) 2_666 . ? C4 Re4 Re6 134.7(2) . . ? S5 Re4 Re6 117.15(6) . . ? S7 Re4 Re6 57.55(6) . . ? S8 Re4 Re6 116.99(5) . . ? S6 Re4 Re6 57.21(5) . . ? Re5 Re4 Re6 59.484(18) 2_666 . ? Re5 Re4 Re6 59.422(15) . . ? C4 Re4 Re6 136.1(2) . 2_666 ? S5 Re4 Re6 57.27(5) . 2_666 ? S7 Re4 Re6 117.00(5) . 2_666 ? S8 Re4 Re6 57.38(6) . 2_666 ? S6 Re4 Re6 116.82(6) . 2_666 ? Re5 Re4 Re6 59.432(16) 2_666 2_666 ? Re5 Re4 Re6 59.454(14) . 2_666 ? Re6 Re4 Re6 89.200(18) . 2_666 ? C4 Re4 Re4 179.2(2) . 2_666 ? S5 Re4 Re4 86.60(5) . 2_666 ? S7 Re4 Re4 86.68(5) . 2_666 ? S8 Re4 Re4 86.56(5) . 2_666 ? S6 Re4 Re4 86.37(5) . 2_666 ? Re5 Re4 Re4 44.463(14) 2_666 2_666 ? Re5 Re4 Re4 44.429(13) . 2_666 ? Re6 Re4 Re4 44.608(13) . 2_666 ? Re6 Re4 Re4 44.592(12) 2_666 2_666 ? C5 Re5 S6 92.3(2) . 2_666 ? C5 Re5 S7 94.1(2) . . ? S6 Re5 S7 173.54(7) 2_666 . ? C5 Re5 S5 92.4(2) . 2_666 ? S6 Re5 S5 89.23(7) 2_666 2_666 ? S7 Re5 S5 90.86(7) . 2_666 ? C5 Re5 S8 94.3(2) . . ? S6 Re5 S8 90.34(7) 2_666 . ? S7 Re5 S8 88.81(7) . . ? S5 Re5 S8 173.25(7) 2_666 . ? C5 Re5 Re6 134.6(2) . . ? S6 Re5 Re6 117.39(6) 2_666 . ? S7 Re5 Re6 57.65(6) . . ? S5 Re5 Re6 57.33(5) 2_666 . ? S8 Re5 Re6 117.22(5) . . ? C5 Re5 Re6 135.0(2) . 2_666 ? S6 Re5 Re6 57.43(5) 2_666 2_666 ? S7 Re5 Re6 117.05(5) . 2_666 ? S5 Re5 Re6 116.97(6) 2_666 2_666 ? S8 Re5 Re6 57.51(6) . 2_666 ? Re6 Re5 Re6 90.308(19) . 2_666 ? C5 Re5 Re4 133.0(2) . 2_666 ? S6 Re5 Re4 57.00(6) 2_666 2_666 ? S7 Re5 Re4 118.04(6) . 2_666 ? S5 Re5 Re4 56.61(5) 2_666 2_666 ? S8 Re5 Re4 117.88(6) . 2_666 ? Re6 Re5 Re4 60.439(17) . 2_666 ? Re6 Re5 Re4 60.399(17) 2_666 2_666 ? C5 Re5 Re4 135.8(2) . . ? S6 Re5 Re4 117.80(5) 2_666 . ? S7 Re5 Re4 56.68(5) . . ? S5 Re5 Re4 117.68(5) 2_666 . ? S8 Re5 Re4 56.86(5) . . ? Re6 Re5 Re4 60.399(16) . . ? Re6 Re5 Re4 60.398(15) 2_666 . ? Re4 Re5 Re4 91.108(18) 2_666 . ? C5 Re5 Re5 178.6(2) . 2_666 ? S6 Re5 Re5 86.81(5) 2_666 2_666 ? S7 Re5 Re5 86.75(5) . 2_666 ? S5 Re5 Re5 86.50(5) 2_666 2_666 ? S8 Re5 Re5 86.75(5) . 2_666 ? Re6 Re5 Re5 45.172(13) . 2_666 ? Re6 Re5 Re5 45.136(12) 2_666 2_666 ? Re4 Re5 Re5 45.572(14) 2_666 2_666 ? Re4 Re5 Re5 45.536(13) . 2_666 ? C6 Re6 S5 92.0(2) . 2_666 ? C6 Re6 S6 94.6(2) . . ? S5 Re6 S6 173.35(7) 2_666 . ? C6 Re6 S8 95.2(3) . 2_666 ? S5 Re6 S8 88.61(7) 2_666 2_666 ? S6 Re6 S8 90.57(7) . 2_666 ? C6 Re6 S7 91.7(3) . . ? S5 Re6 S7 91.10(7) 2_666 . ? S6 Re6 S7 88.94(7) . . ? S8 Re6 S7 173.15(7) 2_666 . ? C6 Re6 Re5 132.9(2) . . ? S5 Re6 Re5 57.78(5) 2_666 . ? S6 Re6 Re5 117.08(5) . . ? S8 Re6 Re5 116.91(5) 2_666 . ? S7 Re6 Re5 57.57(5) . . ? C6 Re6 Re5 137.5(2) . 2_666 ? S5 Re6 Re5 116.74(5) 2_666 2_666 ? S6 Re6 Re5 57.59(5) . 2_666 ? S8 Re6 Re5 57.70(5) 2_666 2_666 ? S7 Re6 Re5 116.66(5) . 2_666 ? Re5 Re6 Re5 89.692(19) . 2_666 ? C6 Re6 Re4 134.2(2) . . ? S5 Re6 Re4 117.91(5) 2_666 . ? S6 Re6 Re4 56.94(5) . . ? S8 Re6 Re4 117.78(5) 2_666 . ? S7 Re6 Re4 56.58(5) . . ? Re5 Re6 Re4 60.179(14) . . ? Re5 Re6 Re4 60.117(18) 2_666 . ? C6 Re6 Re4 134.9(2) . 2_666 ? S5 Re6 Re4 56.63(5) 2_666 2_666 ? S6 Re6 Re4 117.71(5) . 2_666 ? S8 Re6 Re4 56.82(5) 2_666 2_666 ? S7 Re6 Re4 117.66(5) . 2_666 ? Re5 Re6 Re4 60.128(18) . 2_666 ? Re5 Re6 Re4 60.148(16) 2_666 2_666 ? Re4 Re6 Re4 90.800(18) . 2_666 ? C6 Re6 Re6 177.7(2) . 2_666 ? S5 Re6 Re6 86.65(5) 2_666 2_666 ? S6 Re6 Re6 86.72(5) . 2_666 ? S8 Re6 Re6 86.68(5) 2_666 2_666 ? S7 Re6 Re6 86.47(5) . 2_666 ? Re5 Re6 Re6 44.864(12) . 2_666 ? Re5 Re6 Re6 44.828(13) 2_666 2_666 ? Re4 Re6 Re6 45.408(13) . 2_666 ? Re4 Re6 Re6 45.391(13) 2_666 2_666 ? Re4 S5 Re6 66.10(5) . 2_666 ? Re4 S5 Re5 65.68(5) . 2_666 ? Re6 S5 Re5 64.89(5) 2_666 2_666 ? Re4 S6 Re6 65.84(5) . . ? Re4 S6 Re5 65.57(5) . 2_666 ? Re6 S6 Re5 64.98(5) . 2_666 ? Re4 S7 Re5 65.74(5) . . ? Re4 S7 Re6 65.87(6) . . ? Re5 S7 Re6 64.78(6) . . ? Re4 S8 Re6 65.80(6) . 2_666 ? Re4 S8 Re5 65.54(5) . . ? Re6 S8 Re5 64.79(6) 2_666 . ? N4 C4 Re4 177.7(8) . . ? N5 C5 Re5 179.3(9) . . ? N6 C6 Re6 177.3(9) . . ? C7 P1 C13 107.2(4) . . ? C7 P1 C25 111.5(4) . . ? C13 P1 C25 110.5(4) . . ? C7 P1 C19 108.8(4) . . ? C13 P1 C19 110.3(4) . . ? C25 P1 C19 108.4(4) . . ? C8 C7 C12 119.3(7) . . ? C8 C7 P1 116.7(6) . . ? C12 C7 P1 124.0(6) . . ? C9 C8 C7 120.1(8) . . ? C10 C9 C8 120.1(8) . . ? C9 C10 C11 119.7(8) . . ? C12 C11 C10 121.8(8) . . ? C11 C12 C7 119.0(8) . . ? C18 C13 C14 120.4(8) . . ? C18 C13 P1 121.2(7) . . ? C14 C13 P1 118.2(6) . . ? C15 C14 C13 119.5(8) . . ? C14 C15 C16 119.8(9) . . ? C17 C16 C15 120.9(9) . . ? C16 C17 C18 121.3(8) . . ? C13 C18 C17 118.0(9) . . ? C24 C19 C20 120.0(9) . . ? C24 C19 P1 122.0(6) . . ? C20 C19 P1 118.0(7) . . ? C21 C20 C19 120.4(10) . . ? C20 C21 C22 119.9(9) . . ? C23 C22 C21 119.1(10) . . ? C22 C23 C24 121.3(10) . . ? C19 C24 C23 119.3(9) . . ? C26 C25 C30 120.2(8) . . ? C26 C25 P1 118.6(8) . . ? C30 C25 P1 121.2(7) . . ? C27 C26 C25 119.1(10) . . ? C28 C27 C26 121.4(11) . . ? C27 C28 C29 119.6(10) . . ? C30 C29 C28 120.4(11) . . ? C29 C30 C25 119.3(9) . . ? C49 P2 C43 112.0(4) . . ? C49 P2 C31 109.2(4) . . ? C43 P2 C31 106.0(4) . . ? C49 P2 C37 110.7(4) . . ? C43 P2 C37 108.6(4) . . ? C31 P2 C37 110.2(4) . . ? C32 C31 C36 121.2(8) . . ? C32 C31 P2 119.9(6) . . ? C36 C31 P2 118.6(7) . . ? C31 C32 C33 121.3(8) . . ? C32 C33 C34 117.5(9) . . ? C35 C34 C33 120.6(8) . . ? C34 C35 C36 122.1(9) . . ? C35 C36 C31 117.1(9) . . ? C38 C37 C42 119.4(9) . . ? C38 C37 P2 118.8(7) . . ? C42 C37 P2 121.6(7) . . ? C39 C38 C37 119.3(9) . . ? C41 C40 C39 121.4(10) . . ? C38 C39 C40 120.8(10) . . ? C40 C41 C42 118.7(10) . . ? C41 C42 C37 120.3(10) . . ? C44 C43 C48 118.4(8) . . ? C44 C43 P2 120.3(6) . . ? C48 C43 P2 121.3(7) . . ? C45 C44 C43 120.5(9) . . ? C45 C46 C47 120.9(9) . . ? C44 C45 C46 120.5(10) . . ? C48 C47 C46 119.0(9) . . ? C47 C48 C43 120.8(9) . . ? C50 C49 C54 118.6(8) . . ? C50 C49 P2 121.3(7) . . ? C54 C49 P2 120.0(7) . . ? C49 C50 C51 121.0(9) . . ? C52 C51 C50 120.5(9) . . ? C51 C52 C53 118.9(9) . . ? C54 C53 C52 120.3(9) . . ? C53 C54 C49 120.8(9) . . ? C73 P3 C67 111.2(4) . . ? C73 P3 C61 110.8(4) . . ? C67 P3 C61 106.9(4) . . ? C73 P3 C55 108.1(4) . . ? C67 P3 C55 108.8(4) . . ? C61 P3 C55 111.0(4) . . ? C60 C55 C56 122.0(8) . . ? C60 C55 P3 120.4(7) . . ? C56 C55 P3 117.5(6) . . ? C55 C56 C57 118.8(8) . . ? C56 C57 C58 120.3(9) . . ? C59 C58 C57 120.0(9) . . ? C58 C59 C60 120.8(9) . . ? C55 C60 C59 118.1(9) . . ? C62 C61 C66 121.1(8) . . ? C62 C61 P3 119.2(7) . . ? C66 C61 P3 119.6(6) . . ? C61 C62 C63 118.9(10) . . ? C64 C63 C62 120.6(9) . . ? C63 C64 C65 120.5(8) . . ? C66 C65 C64 120.1(10) . . ? C65 C66 C61 118.8(9) . . ? C72 C67 C68 119.6(8) . . ? C72 C67 P3 119.5(7) . . ? C68 C67 P3 120.8(7) . . ? C69 C68 C67 119.4(8) . . ? C68 C69 C70 119.7(9) . . ? C71 C70 C69 120.1(9) . . ? C70 C71 C72 121.1(10) . . ? C67 C72 C71 120.0(9) . . ? C78 C73 C74 118.8(8) . . ? C78 C73 P3 124.4(7) . . ? C74 C73 P3 116.8(6) . . ? C75 C74 C73 118.8(8) . . ? C76 C75 C74 121.0(8) . . ? C75 C76 C77 119.2(11) . . ? C78 C77 C76 122.1(10) . . ? C77 C78 C73 120.1(8) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 2.519 _refine_diff_density_min -2.717 _refine_diff_density_rms 0.247 #################### Material relevant to compound 3 at 293K ############ data_p280_abm _database_code_CSD 186997 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(PPh4)3 (Re6Se8(CN)6) (CH3CN) (H2O)3' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H69 N7 O3 P3 Re6 Se8' _chemical_formula_weight 3018.21 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6233(9) _cell_length_b 14.2701(9) _cell_length_c 26.1709(18) _cell_angle_alpha 74.555(8) _cell_angle_beta 89.578(8) _cell_angle_gamma 62.626(7) _cell_volume 4315.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description platelet _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.4620 _exptl_crystal_size_mid 0.3850 _exptl_crystal_size_min 0.1386 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2778 _exptl_absorpt_coefficient_mu 11.860 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0512 _exptl_absorpt_correction_T_max 0.2485 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_special_details ; 'The hydrogen atoms on the water molecules were not found on the Fourier map' ; _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 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, Phi. incr. == 0.9' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41983 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.88 _reflns_number_total 15591 _reflns_number_gt 10805 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0156P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15591 _refine_ls_number_parameters 947 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0506 _refine_ls_wR_factor_gt 0.0459 _refine_ls_goodness_of_fit_ref 0.828 _refine_ls_restrained_S_all 0.828 _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 0.97835(2) 0.07827(2) 0.049288(8) 0.03181(6) Uani 1 1 d . . . Re2 Re 1.15215(2) -0.08318(2) 0.026652(9) 0.03144(6) Uani 1 1 d . . . Re3 Re 0.97241(2) -0.10328(2) 0.048938(9) 0.03218(6) Uani 1 1 d . . . Se1 Se 0.80855(6) 0.05548(6) 0.06915(2) 0.04195(16) Uani 1 1 d . . . Se2 Se 0.85983(6) 0.25279(5) -0.02508(2) 0.03988(16) Uani 1 1 d . . . Se3 Se 1.09717(6) -0.10332(6) 0.11961(2) 0.04006(16) Uani 1 1 d . . . Se4 Se 1.15088(6) 0.09475(6) 0.02576(2) 0.04010(16) Uani 1 1 d . . . C1 C 0.9494(6) 0.1709(6) 0.1038(2) 0.0452(18) Uani 1 1 d . . . C2 C 1.3248(6) -0.1800(5) 0.0568(2) 0.0393(15) Uani 1 1 d . . . C3 C 0.9407(6) -0.2211(6) 0.1035(2) 0.0489(18) Uani 1 1 d . . . N1 N 0.9332(6) 0.2236(5) 0.1323(2) 0.0642(19) Uani 1 1 d . . . N2 N 1.4169(5) -0.2346(5) 0.0732(2) 0.0542(16) Uani 1 1 d . . . N3 N 0.9249(7) -0.2873(6) 0.1326(2) 0.076(2) Uani 1 1 d . . . Re4 Re 0.96227(2) 0.06897(2) 0.426542(9) 0.03235(6) Uani 1 1 d . . . Re5 Re 1.14737(2) -0.08200(2) 0.490210(9) 0.03324(6) Uani 1 1 d . . . Re6 Re 0.96916(2) -0.11013(2) 0.492153(9) 0.03394(6) Uani 1 1 d . . . Se5 Se 0.79409(5) 0.03947(6) 0.43126(2) 0.04252(16) Uani 1 1 d . . . Se6 Se 1.07584(6) -0.11823(5) 0.41281(2) 0.04164(16) Uani 1 1 d . . . Se7 Se 1.13522(6) 0.09214(6) 0.42799(2) 0.04254(16) Uani 1 1 d . . . Se8 Se 0.85270(6) 0.24939(5) 0.44699(2) 0.04383(17) Uani 1 1 d . . . C4 C 0.9122(5) 0.1518(5) 0.3434(3) 0.0413(16) Uani 1 1 d . . . C5 C 1.3147(6) -0.1725(6) 0.4800(3) 0.054(2) Uani 1 1 d . . . C6 C 0.9367(6) -0.2379(6) 0.4865(3) 0.0498(18) Uani 1 1 d . . . N4 N 0.8821(5) 0.1995(5) 0.2994(2) 0.0566(17) Uani 1 1 d . . . N5 N 1.4074(6) -0.2194(7) 0.4753(3) 0.082(2) Uani 1 1 d . . . N6 N 0.9164(7) -0.3069(6) 0.4852(3) 0.081(2) Uani 1 1 d . . . P1 P 0.49744(15) 0.86505(15) 0.31978(6) 0.0418(4) Uani 1 1 d . . . C101 C 0.5345(6) 0.7241(5) 0.3514(2) 0.0429(17) Uani 1 1 d . . . C102 C 0.6462(6) 0.6424(6) 0.3634(3) 0.062(2) Uani 1 1 d . . . H102 H 0.7021 0.6610 0.3534 0.074 Uiso 1 1 calc R . . C103 C 0.6737(8) 0.5353(7) 0.3899(3) 0.073(3) Uani 1 1 d . . . H103 H 0.7479 0.4807 0.3970 0.088 Uiso 1 1 calc R . . C104 C 0.5914(8) 0.5090(7) 0.4058(3) 0.072(3) Uani 1 1 d . . . H104 H 0.6098 0.4366 0.4244 0.087 Uiso 1 1 calc R . . C105 C 0.4827(8) 0.5885(7) 0.3944(3) 0.073(3) Uani 1 1 d . . . H105 H 0.4275 0.5690 0.4046 0.088 Uiso 1 1 calc R . . C106 C 0.4532(6) 0.6945(7) 0.3688(3) 0.058(2) Uani 1 1 d . . . H106 H 0.3786 0.7479 0.3627 0.070 Uiso 1 1 calc R . . C107 C 0.3570(6) 0.9353(6) 0.2880(3) 0.0479(18) Uani 1 1 d . . . C108 C 0.3370(6) 0.9451(7) 0.2343(3) 0.0533(19) Uani 1 1 d . . . H108 H 0.3965 0.9168 0.2154 0.064 Uiso 1 1 calc R . . C109 C 0.2288(7) 0.9967(8) 0.2091(3) 0.073(3) Uani 1 1 d . . . H109 H 0.2154 1.0065 0.1728 0.087 Uiso 1 1 calc R . . C110 C 0.1424(8) 1.0330(9) 0.2374(4) 0.091(3) Uani 1 1 d . . . H110 H 0.0696 1.0654 0.2206 0.109 Uiso 1 1 calc R . . C111 C 0.1614(7) 1.0221(8) 0.2911(4) 0.087(3) Uani 1 1 d . . . H111 H 0.1014 1.0486 0.3100 0.104 Uiso 1 1 calc R . . C112 C 0.2668(7) 0.9731(7) 0.3162(3) 0.067(2) Uani 1 1 d . . . H112 H 0.2790 0.9647 0.3524 0.080 Uiso 1 1 calc R . . C113 C 0.5115(7) 0.9285(7) 0.3683(3) 0.0522(19) Uani 1 1 d . . . C114 C 0.5900(7) 0.8681(8) 0.4121(3) 0.064(2) Uani 1 1 d . . . H114 H 0.6338 0.7923 0.4184 0.076 Uiso 1 1 calc R . . C115 C 0.6048(9) 0.9193(11) 0.4473(3) 0.086(3) Uani 1 1 d . . . H115 H 0.6597 0.8777 0.4768 0.103 Uiso 1 1 calc R . . C116 C 0.5413(12) 1.0274(14) 0.4393(5) 0.107(4) Uani 1 1 d . . . H116 H 0.5522 1.0607 0.4633 0.128 Uiso 1 1 calc R . . C117 C 0.4616(12) 1.0887(10) 0.3969(5) 0.113(4) Uani 1 1 d . . . H117 H 0.4178 1.1642 0.3914 0.135 Uiso 1 1 calc R . . C118 C 0.4446(10) 1.0392(9) 0.3614(4) 0.100(4) Uani 1 1 d . . . H118 H 0.3878 1.0811 0.3327 0.120 Uiso 1 1 calc R . . C119 C 0.5860(6) 0.8746(7) 0.2700(3) 0.0518(19) Uani 1 1 d . . . C120 C 0.6049(7) 0.9656(7) 0.2563(3) 0.064(2) Uani 1 1 d . . . H120 H 0.5743 1.0187 0.2743 0.077 Uiso 1 1 calc R . . C121 C 0.6689(8) 0.9775(10) 0.2161(3) 0.084(3) Uani 1 1 d . . . H121 H 0.6813 1.0384 0.2070 0.101 Uiso 1 1 calc R . . C122 C 0.7130(8) 0.9000(11) 0.1904(3) 0.089(4) Uani 1 1 d . . . H122 H 0.7569 0.9077 0.1639 0.106 Uiso 1 1 calc R . . C123 C 0.6953(8) 0.8110(9) 0.2021(3) 0.085(3) Uani 1 1 d . . . H123 H 0.7260 0.7590 0.1836 0.102 Uiso 1 1 calc R . . C124 C 0.6303(6) 0.7982(7) 0.2423(3) 0.066(2) Uani 1 1 d . . . H124 H 0.6172 0.7378 0.2503 0.079 Uiso 1 1 calc R . . P2 P 1.64371(15) -0.28907(15) -0.08428(7) 0.0415(4) Uani 1 1 d . . . C201 C 1.5690(5) -0.1492(5) -0.0833(2) 0.0370(15) Uani 1 1 d . . . C202 C 1.6024(6) -0.0730(6) -0.1090(3) 0.0489(18) Uani 1 1 d . . . H202 H 1.6614 -0.0940 -0.1290 0.059 Uiso 1 1 calc R . . C203 C 1.5504(7) 0.0332(6) -0.1057(3) 0.060(2) Uani 1 1 d . . . H203 H 1.5739 0.0837 -0.1231 0.072 Uiso 1 1 calc R . . C204 C 1.4630(7) 0.0633(7) -0.0763(3) 0.059(2) Uani 1 1 d . . . H204 H 1.4270 0.1350 -0.0739 0.071 Uiso 1 1 calc R . . C205 C 1.4284(6) -0.0106(7) -0.0506(3) 0.058(2) Uani 1 1 d . . . H205 H 1.3684 0.0115 -0.0313 0.069 Uiso 1 1 calc R . . C206 C 1.4816(6) -0.1174(7) -0.0531(3) 0.0518(19) Uani 1 1 d . . . H206 H 1.4592 -0.1681 -0.0346 0.062 Uiso 1 1 calc R . . C207 C 1.5479(6) -0.3431(6) -0.0858(2) 0.0451(17) Uani 1 1 d . . . C208 C 1.5817(7) -0.4543(6) -0.0635(3) 0.058(2) Uani 1 1 d . . . H208 H 1.6537 -0.5015 -0.0457 0.070 Uiso 1 1 calc R . . C209 C 1.5096(9) -0.4958(8) -0.0673(3) 0.079(3) Uani 1 1 d . . . H209 H 1.5307 -0.5700 -0.0515 0.094 Uiso 1 1 calc R . . C210 C 1.4057(9) -0.4236(9) -0.0953(4) 0.082(3) Uani 1 1 d . . . H210 H 1.3579 -0.4516 -0.0998 0.099 Uiso 1 1 calc R . . C211 C 1.3686(8) -0.3142(9) -0.1169(4) 0.092(3) Uani 1 1 d . . . H211 H 1.2954 -0.2675 -0.1332 0.111 Uiso 1 1 calc R . . C212 C 1.4416(7) -0.2737(8) -0.1140(3) 0.070(3) Uani 1 1 d . . . H212 H 1.4199 -0.1996 -0.1309 0.084 Uiso 1 1 calc R . . C213 C 1.7146(6) -0.2950(6) -0.1421(3) 0.0494(18) Uani 1 1 d . . . C214 C 1.6653(7) -0.2908(7) -0.1891(3) 0.059(2) Uani 1 1 d . . . H214 H 1.5961 -0.2886 -0.1906 0.071 Uiso 1 1 calc R . . C215 C 1.7186(10) -0.2897(8) -0.2337(3) 0.078(3) Uani 1 1 d . . . H215 H 1.6854 -0.2879 -0.2651 0.094 Uiso 1 1 calc R . . C216 C 1.8182(10) -0.2913(8) -0.2327(4) 0.085(3) Uani 1 1 d . . . H216 H 1.8541 -0.2921 -0.2631 0.102 Uiso 1 1 calc R . . C217 C 1.8658(8) -0.2916(8) -0.1872(4) 0.083(3) Uani 1 1 d . . . H217 H 1.9333 -0.2899 -0.1871 0.100 Uiso 1 1 calc R . . C218 C 1.8165(7) -0.2945(7) -0.1418(3) 0.067(2) Uani 1 1 d . . . H218 H 1.8507 -0.2960 -0.1108 0.080 Uiso 1 1 calc R . . C219 C 1.7446(6) -0.3715(6) -0.0254(2) 0.0497(19) Uani 1 1 d . . . C220 C 1.8306(6) -0.4743(7) -0.0226(3) 0.062(2) Uani 1 1 d . . . H220 H 1.8415 -0.4996 -0.0525 0.075 Uiso 1 1 calc R . . C221 C 1.9011(7) -0.5400(7) 0.0251(4) 0.078(3) Uani 1 1 d . . . H221 H 1.9583 -0.6103 0.0276 0.094 Uiso 1 1 calc R . . C222 C 1.8860(9) -0.5007(10) 0.0682(4) 0.091(3) Uani 1 1 d . . . H222 H 1.9329 -0.5452 0.1002 0.109 Uiso 1 1 calc R . . C223 C 1.8042(9) -0.3983(10) 0.0654(3) 0.097(4) Uani 1 1 d . . . H223 H 1.7970 -0.3725 0.0950 0.116 Uiso 1 1 calc R . . C224 C 1.7314(7) -0.3321(8) 0.0190(3) 0.074(3) Uani 1 1 d . . . H224 H 1.6744 -0.2621 0.0173 0.089 Uiso 1 1 calc R . . P3 P 1.11380(15) -0.39367(15) 0.31047(6) 0.0401(4) Uani 1 1 d . . . C301 C 1.0113(6) -0.2560(6) 0.3068(2) 0.0413(16) Uani 1 1 d . . . C302 C 1.0129(6) -0.1626(6) 0.2730(3) 0.0531(19) Uani 1 1 d . . . H302 H 1.0672 -0.1702 0.2503 0.064 Uiso 1 1 calc R . . C303 C 0.9337(7) -0.0598(6) 0.2736(3) 0.062(2) Uani 1 1 d . . . H303 H 0.9344 0.0024 0.2510 0.075 Uiso 1 1 calc R . . C304 C 0.8541(7) -0.0468(7) 0.3066(3) 0.058(2) Uani 1 1 d . . . H304 H 0.8012 0.0237 0.3067 0.070 Uiso 1 1 calc R . . C305 C 0.8521(6) -0.1364(7) 0.3394(3) 0.054(2) Uani 1 1 d . . . H305 H 0.7983 -0.1272 0.3625 0.065 Uiso 1 1 calc R . . C306 C 0.9279(6) -0.2404(6) 0.3393(3) 0.0466(18) Uani 1 1 d . . . H306 H 0.9234 -0.3011 0.3611 0.056 Uiso 1 1 calc R . . C307 C 1.2018(6) -0.3921(6) 0.2594(3) 0.0482(18) Uani 1 1 d . . . C308 C 1.1910(7) -0.4216(7) 0.2137(3) 0.064(2) Uani 1 1 d . . . H308 H 1.1380 -0.4438 0.2095 0.077 Uiso 1 1 calc R . . C309 C 1.2584(9) -0.4177(8) 0.1756(3) 0.079(3) Uani 1 1 d . . . H309 H 1.2502 -0.4371 0.1452 0.094 Uiso 1 1 calc R . . C310 C 1.3374(10) -0.3863(8) 0.1804(4) 0.089(3) Uani 1 1 d . . . H310 H 1.3825 -0.3843 0.1537 0.107 Uiso 1 1 calc R . . C311 C 1.3498(8) -0.3575(8) 0.2252(4) 0.086(3) Uani 1 1 d . . . H311 H 1.4043 -0.3371 0.2292 0.103 Uiso 1 1 calc R . . C312 C 1.2815(7) -0.3591(8) 0.2640(3) 0.070(2) Uani 1 1 d . . . H312 H 1.2889 -0.3377 0.2937 0.084 Uiso 1 1 calc R . . C313 C 1.2036(6) -0.4602(6) 0.3728(2) 0.0416(16) Uani 1 1 d . . . C314 C 1.1757(6) -0.4191(6) 0.4162(3) 0.054(2) Uani 1 1 d . . . H314 H 1.1119 -0.3524 0.4129 0.065 Uiso 1 1 calc R . . C315 C 1.2445(7) -0.4792(8) 0.4645(3) 0.071(3) Uani 1 1 d . . . H315 H 1.2247 -0.4541 0.4943 0.085 Uiso 1 1 calc R . . C316 C 1.3411(7) -0.5748(7) 0.4693(3) 0.064(2) Uani 1 1 d . . . H316 H 1.3877 -0.6120 0.5018 0.077 Uiso 1 1 calc R . . C317 C 1.3693(7) -0.6155(7) 0.4272(3) 0.067(2) Uani 1 1 d . . . H317 H 1.4338 -0.6818 0.4308 0.080 Uiso 1 1 calc R . . C318 C 1.3009(6) -0.5572(7) 0.3786(3) 0.060(2) Uani 1 1 d . . . H318 H 1.3210 -0.5840 0.3493 0.072 Uiso 1 1 calc R . . C319 C 1.0420(6) -0.4693(5) 0.3051(2) 0.0406(16) Uani 1 1 d . . . C320 C 1.0555(6) -0.5592(6) 0.3454(3) 0.0523(19) Uani 1 1 d . . . H320 H 1.1076 -0.5859 0.3754 0.063 Uiso 1 1 calc R . . C321 C 0.9929(7) -0.6110(7) 0.3422(3) 0.067(2) Uani 1 1 d . . . H321 H 1.0031 -0.6727 0.3698 0.080 Uiso 1 1 calc R . . C322 C 0.9148(8) -0.5706(7) 0.2978(3) 0.070(2) Uani 1 1 d . . . H322 H 0.8713 -0.6044 0.2956 0.084 Uiso 1 1 calc R . . C323 C 0.9018(7) -0.4813(7) 0.2575(3) 0.070(2) Uani 1 1 d . . . H323 H 0.8510 -0.4559 0.2271 0.084 Uiso 1 1 calc R . . C324 C 0.9618(3) -0.4291(3) 0.26086(12) 0.058(2) Uani 1 1 d . . . H324 H 0.9497 -0.3662 0.2337 0.070 Uiso 1 1 calc R . . C7 C 0.5766(3) 0.2824(3) 0.28705(12) 0.156(6) Uani 1 1 d R . . N7 N 0.5561(3) 0.2263(3) 0.28015(12) 0.334(15) Uani 1 1 d R . . C8 C 0.6029(3) 0.3830(3) 0.29105(12) 0.196(8) Uani 1 1 d R . . H8A H 0.6331 0.4051 0.2596 0.293 Uiso 1 1 calc R . . H8B H 0.6558 0.3571 0.3221 0.293 Uiso 1 1 calc R . . H8C H 0.5350 0.4449 0.2937 0.293 Uiso 1 1 calc R . . O1 O 0.8075(3) 0.3707(3) 0.19535(12) 0.0827(19) Uani 1 1 d R . . O2 O 0.9024(3) 0.5437(3) 0.43525(12) 0.112(3) Uani 1 1 d R . . O3 O 0.6175(3) 0.6126(3) 0.17245(12) 0.131(3) Uani 1 1 d 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 Re1 0.03450(14) 0.03299(14) 0.02769(11) -0.00958(10) 0.00403(10) -0.01552(12) Re2 0.03110(14) 0.03236(14) 0.02959(11) -0.00785(10) 0.00313(10) -0.01473(11) Re3 0.03557(15) 0.03374(14) 0.02764(11) -0.00622(10) 0.00476(10) -0.01834(12) Se1 0.0378(4) 0.0509(4) 0.0382(3) -0.0157(3) 0.0137(3) -0.0207(3) Se2 0.0429(4) 0.0302(4) 0.0411(3) -0.0093(3) 0.0008(3) -0.0136(3) Se3 0.0470(4) 0.0430(4) 0.0264(3) -0.0059(3) -0.0003(3) -0.0205(3) Se4 0.0403(4) 0.0416(4) 0.0432(3) -0.0112(3) 0.0019(3) -0.0241(3) C1 0.045(4) 0.038(4) 0.039(3) -0.016(3) -0.001(3) -0.007(3) C2 0.038(4) 0.034(4) 0.046(3) -0.014(3) 0.007(3) -0.016(3) C3 0.058(5) 0.055(5) 0.037(3) -0.007(3) 0.006(3) -0.033(4) N1 0.070(5) 0.063(5) 0.058(4) -0.033(3) 0.004(3) -0.022(4) N2 0.037(4) 0.043(4) 0.073(4) -0.007(3) -0.003(3) -0.016(3) N3 0.099(6) 0.083(6) 0.052(4) 0.007(4) 0.002(4) -0.063(5) Re4 0.03103(14) 0.02531(13) 0.03224(11) -0.00438(10) 0.00207(10) -0.00867(11) Re5 0.02860(14) 0.02690(14) 0.03519(12) -0.00647(10) 0.00320(10) -0.00728(11) Re6 0.03544(15) 0.02550(13) 0.03690(12) -0.00707(10) 0.00339(11) -0.01237(12) Se5 0.0343(4) 0.0446(4) 0.0441(3) -0.0105(3) -0.0011(3) -0.0163(3) Se6 0.0449(4) 0.0352(4) 0.0395(3) -0.0147(3) 0.0064(3) -0.0127(3) Se7 0.0414(4) 0.0404(4) 0.0441(3) -0.0063(3) 0.0108(3) -0.0214(3) Se8 0.0437(4) 0.0238(3) 0.0462(3) -0.0031(3) 0.0021(3) -0.0053(3) C4 0.033(4) 0.035(4) 0.047(4) -0.009(3) 0.005(3) -0.011(3) C5 0.042(5) 0.050(5) 0.051(4) -0.017(3) 0.005(4) -0.006(4) C6 0.069(5) 0.030(4) 0.053(4) -0.011(3) 0.012(4) -0.025(4) N4 0.060(4) 0.055(4) 0.038(3) -0.003(3) 0.001(3) -0.019(3) N5 0.048(5) 0.088(6) 0.080(5) -0.027(4) 0.007(4) -0.006(4) N6 0.107(6) 0.050(5) 0.105(5) -0.026(4) 0.021(5) -0.052(5) P1 0.0362(10) 0.0406(10) 0.0407(8) -0.0055(8) 0.0029(8) -0.0152(8) C101 0.048(4) 0.037(4) 0.038(3) -0.006(3) 0.003(3) -0.019(3) C102 0.043(5) 0.043(5) 0.072(5) 0.004(4) 0.000(4) -0.009(4) C103 0.059(6) 0.051(6) 0.076(5) -0.008(4) -0.002(5) -0.005(5) C104 0.078(7) 0.035(5) 0.080(6) 0.003(4) 0.000(5) -0.016(5) C105 0.083(7) 0.055(6) 0.084(6) 0.000(5) 0.002(5) -0.045(6) C106 0.042(5) 0.047(5) 0.075(5) -0.006(4) -0.002(4) -0.019(4) C107 0.045(5) 0.044(4) 0.047(4) -0.001(3) 0.005(3) -0.021(4) C108 0.041(4) 0.072(6) 0.054(4) -0.019(4) 0.014(3) -0.032(4) C109 0.054(6) 0.108(8) 0.053(4) 0.007(5) -0.010(4) -0.052(5) C110 0.045(6) 0.100(8) 0.094(7) 0.031(6) -0.017(5) -0.038(6) C111 0.035(5) 0.090(8) 0.081(6) 0.009(5) 0.015(5) -0.004(5) C112 0.046(5) 0.071(6) 0.057(4) -0.009(4) 0.011(4) -0.011(4) C113 0.059(5) 0.057(5) 0.043(4) -0.006(3) 0.007(3) -0.034(4) C114 0.061(5) 0.079(6) 0.062(4) -0.019(4) 0.009(4) -0.043(5) C115 0.093(8) 0.141(11) 0.056(5) -0.033(6) 0.010(5) -0.080(8) C116 0.139(12) 0.174(14) 0.089(8) -0.076(9) 0.049(8) -0.121(11) C117 0.164(12) 0.090(9) 0.118(9) -0.063(8) 0.034(9) -0.071(9) C118 0.132(10) 0.066(7) 0.090(7) -0.026(6) -0.002(6) -0.035(7) C119 0.042(5) 0.055(5) 0.046(4) -0.002(3) -0.003(3) -0.020(4) C120 0.064(6) 0.077(6) 0.054(4) -0.004(4) -0.005(4) -0.044(5) C121 0.070(7) 0.123(10) 0.056(5) 0.017(6) -0.012(5) -0.066(7) C122 0.059(7) 0.124(10) 0.044(5) 0.022(5) 0.007(4) -0.038(7) C123 0.068(7) 0.091(8) 0.051(5) 0.002(5) 0.019(4) -0.015(6) C124 0.049(5) 0.068(6) 0.053(4) -0.002(4) 0.006(4) -0.013(4) P2 0.0362(10) 0.0392(10) 0.0444(9) -0.0075(8) 0.0015(8) -0.0165(8) C201 0.031(4) 0.042(4) 0.038(3) -0.012(3) 0.005(3) -0.017(3) C202 0.050(5) 0.051(5) 0.043(3) -0.012(3) 0.008(3) -0.024(4) C203 0.094(7) 0.049(5) 0.049(4) -0.013(4) 0.011(4) -0.044(5) C204 0.067(6) 0.047(5) 0.058(4) -0.021(4) 0.006(4) -0.020(4) C205 0.045(5) 0.075(6) 0.061(4) -0.038(4) 0.020(4) -0.026(4) C206 0.051(5) 0.057(5) 0.057(4) -0.018(4) 0.011(4) -0.033(4) C207 0.046(4) 0.046(4) 0.048(4) -0.017(3) 0.005(3) -0.023(4) C208 0.072(6) 0.046(5) 0.064(4) -0.016(4) 0.010(4) -0.034(4) C209 0.100(8) 0.077(7) 0.081(6) -0.024(5) 0.015(6) -0.060(6) C210 0.087(7) 0.100(8) 0.095(7) -0.042(6) 0.010(6) -0.067(7) C211 0.068(7) 0.089(8) 0.126(8) -0.034(7) -0.017(6) -0.040(6) C212 0.057(5) 0.070(6) 0.083(5) -0.016(5) -0.011(5) -0.032(5) C213 0.048(5) 0.046(4) 0.053(4) -0.015(3) 0.001(3) -0.020(4) C214 0.061(5) 0.063(5) 0.057(4) -0.021(4) 0.010(4) -0.031(4) C215 0.105(9) 0.074(7) 0.058(5) -0.025(5) 0.010(5) -0.042(6) C216 0.094(8) 0.067(7) 0.075(6) -0.021(5) 0.036(6) -0.024(6) C217 0.067(7) 0.090(8) 0.077(6) -0.016(5) 0.017(5) -0.029(6) C218 0.057(6) 0.074(6) 0.057(5) -0.009(4) 0.002(4) -0.026(5) C219 0.057(5) 0.049(5) 0.042(3) -0.002(3) -0.004(3) -0.031(4) C220 0.050(5) 0.045(5) 0.079(5) -0.008(4) -0.003(4) -0.017(4) C221 0.067(6) 0.047(5) 0.091(6) 0.011(5) -0.019(5) -0.020(5) C222 0.074(7) 0.107(9) 0.072(6) 0.016(6) -0.021(5) -0.050(7) C223 0.095(8) 0.104(9) 0.053(5) -0.007(5) -0.027(5) -0.025(7) C224 0.056(5) 0.081(7) 0.066(5) -0.026(5) -0.007(4) -0.014(5) P3 0.0461(11) 0.0386(10) 0.0339(8) -0.0055(7) 0.0013(7) -0.0214(9) C301 0.042(4) 0.047(4) 0.041(3) -0.014(3) 0.004(3) -0.026(3) C302 0.054(5) 0.050(5) 0.055(4) -0.008(4) 0.001(4) -0.028(4) C303 0.069(6) 0.035(4) 0.076(5) -0.005(4) -0.007(5) -0.024(4) C304 0.048(5) 0.047(5) 0.072(5) -0.026(4) -0.008(4) -0.011(4) C305 0.051(5) 0.066(6) 0.045(4) -0.021(4) 0.000(3) -0.026(4) C306 0.040(4) 0.053(5) 0.046(4) -0.018(3) 0.005(3) -0.019(4) C307 0.047(5) 0.043(4) 0.048(4) -0.008(3) 0.012(3) -0.019(4) C308 0.072(6) 0.068(6) 0.054(4) -0.018(4) 0.021(4) -0.035(5) C309 0.101(8) 0.068(6) 0.060(5) -0.020(4) 0.025(5) -0.034(6) C310 0.097(9) 0.064(7) 0.064(6) 0.002(5) 0.042(5) -0.016(6) C311 0.060(6) 0.082(7) 0.117(8) -0.015(6) 0.040(6) -0.044(6) C312 0.062(6) 0.092(7) 0.066(5) -0.020(5) 0.012(4) -0.047(5) C313 0.040(4) 0.048(4) 0.037(3) -0.011(3) 0.005(3) -0.021(3) C314 0.049(5) 0.057(5) 0.049(4) -0.019(4) 0.012(3) -0.017(4) C315 0.066(6) 0.086(7) 0.041(4) -0.016(4) -0.008(4) -0.021(5) C316 0.058(5) 0.069(6) 0.049(4) -0.001(4) -0.016(4) -0.026(5) C317 0.057(5) 0.056(5) 0.074(5) -0.014(4) -0.014(4) -0.018(4) C318 0.043(5) 0.063(5) 0.064(4) -0.025(4) 0.001(4) -0.014(4) C319 0.054(4) 0.035(4) 0.035(3) -0.006(3) 0.009(3) -0.025(3) C320 0.051(5) 0.049(5) 0.050(4) -0.004(3) 0.006(3) -0.024(4) C321 0.072(6) 0.046(5) 0.079(5) -0.004(4) 0.017(5) -0.033(5) C322 0.082(7) 0.059(6) 0.093(6) -0.025(5) 0.022(5) -0.052(5) C323 0.071(6) 0.074(6) 0.078(5) -0.020(5) -0.006(5) -0.046(5) C324 0.066(5) 0.050(5) 0.053(4) 0.000(3) -0.009(4) -0.033(4) C7 0.126(13) 0.184(17) 0.126(11) 0.003(11) -0.016(9) -0.074(13) N7 0.37(3) 0.38(3) 0.33(2) -0.01(2) -0.11(2) -0.29(3) C8 0.103(12) 0.182(18) 0.30(2) -0.131(17) 0.048(14) -0.038(12) O1 0.108(5) 0.072(4) 0.060(3) -0.024(3) 0.003(3) -0.033(4) O2 0.155(7) 0.128(7) 0.097(5) -0.045(5) 0.024(5) -0.097(6) O3 0.125(7) 0.167(9) 0.135(6) -0.077(6) 0.024(5) -0.079(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 Re1 C1 2.111(6) . ? Re1 Se1 2.5122(8) . ? Re1 Se2 2.5227(8) . ? Re1 Se3 2.5236(8) . ? Re1 Se4 2.5236(8) . ? Re1 Re3 2.6252(4) 2_755 ? Re1 Re3 2.6313(4) . ? Re1 Re2 2.6372(4) . ? Re1 Re2 2.6418(4) 2_755 ? Re1 Re1 3.7187(5) 2_755 ? Re2 C2 2.127(7) . ? Re2 Se2 2.5105(7) 2_755 ? Re2 Se3 2.5220(7) . ? Re2 Se4 2.5249(7) . ? Re2 Se1 2.5250(7) 2_755 ? Re2 Re3 2.6371(4) . ? Re2 Re3 2.6394(5) 2_755 ? Re2 Re1 2.6418(4) 2_755 ? Re2 Re2 3.7469(6) 2_755 ? Re3 C3 2.105(8) . ? Re3 Se3 2.5207(6) . ? Re3 Se1 2.5230(8) . ? Re3 Se2 2.5238(8) 2_755 ? Re3 Se4 2.5280(6) 2_755 ? Re3 Re1 2.6252(4) 2_755 ? Re3 Re2 2.6394(5) 2_755 ? Re3 Re3 3.7151(6) 2_755 ? Se1 Re2 2.5250(7) 2_755 ? Se2 Re2 2.5105(7) 2_755 ? Se2 Re3 2.5238(8) 2_755 ? Se4 Re3 2.5280(6) 2_755 ? C1 N1 1.146(8) . ? C2 N2 1.138(8) . ? C3 N3 1.149(9) . ? Re4 C4 2.122(6) . ? Re4 Se5 2.5095(8) . ? Re4 Se8 2.5161(8) . ? Re4 Se6 2.5222(7) . ? Re4 Se7 2.5271(8) . ? Re4 Re5 2.6315(4) 2_756 ? Re4 Re5 2.6326(5) . ? Re4 Re6 2.6332(4) . ? Re4 Re6 2.6353(4) 2_756 ? Re4 Re4 3.7258(6) 2_756 ? Re5 C5 2.098(8) . ? Re5 Se8 2.5135(8) 2_756 ? Re5 Se7 2.5149(8) . ? Re5 Se5 2.5224(7) 2_756 ? Re5 Se6 2.5238(6) . ? Re5 Re6 2.6289(4) 2_756 ? Re5 Re4 2.6315(4) 2_756 ? Re5 Re6 2.6347(4) . ? Re5 Re5 3.7188(6) 2_756 ? Re6 C6 2.104(7) . ? Re6 Se8 2.5123(8) 2_756 ? Re6 Se5 2.5194(8) . ? Re6 Se7 2.5223(8) 2_756 ? Re6 Se6 2.5231(8) . ? Re6 Re5 2.6289(4) 2_756 ? Re6 Re4 2.6353(4) 2_756 ? Re6 Re6 3.7251(5) 2_756 ? Se5 Re5 2.5224(7) 2_756 ? Se7 Re6 2.5223(8) 2_756 ? Se8 Re6 2.5123(8) 2_756 ? Se8 Re5 2.5135(8) 2_756 ? C4 N4 1.137(7) . ? C5 N5 1.150(9) . ? C6 N6 1.148(9) . ? P1 C107 1.781(7) . ? P1 C101 1.781(7) . ? P1 C119 1.790(8) . ? P1 C113 1.801(7) . ? C101 C106 1.390(10) . ? C101 C102 1.398(10) . ? C102 C103 1.367(11) . ? C103 C104 1.366(12) . ? C104 C105 1.360(12) . ? C105 C106 1.343(10) . ? C107 C112 1.390(10) . ? C107 C108 1.392(9) . ? C108 C109 1.380(10) . ? C109 C110 1.355(13) . ? C110 C111 1.385(12) . ? C111 C112 1.352(11) . ? C113 C114 1.357(9) . ? C113 C118 1.373(12) . ? C114 C115 1.388(11) . ? C115 C116 1.333(15) . ? C116 C117 1.343(15) . ? C117 C118 1.387(12) . ? C119 C124 1.374(11) . ? C119 C120 1.392(11) . ? C120 C121 1.388(12) . ? C121 C122 1.347(14) . ? C122 C123 1.356(14) . ? C123 C124 1.398(12) . ? P2 C201 1.783(7) . ? P2 C213 1.789(8) . ? P2 C219 1.796(6) . ? P2 C207 1.801(7) . ? C201 C202 1.379(9) . ? C201 C206 1.389(9) . ? C202 C203 1.373(10) . ? C203 C204 1.373(11) . ? C204 C205 1.365(11) . ? C205 C206 1.375(10) . ? C207 C208 1.382(10) . ? C207 C212 1.388(10) . ? C208 C209 1.375(11) . ? C209 C210 1.369(13) . ? C210 C211 1.348(13) . ? C211 C212 1.373(12) . ? C213 C214 1.380(9) . ? C213 C218 1.393(11) . ? C214 C215 1.369(12) . ? C215 C216 1.347(13) . ? C216 C217 1.358(12) . ? C217 C218 1.361(12) . ? C219 C220 1.375(10) . ? C219 C224 1.399(10) . ? C220 C221 1.387(10) . ? C221 C222 1.363(13) . ? C222 C223 1.352(14) . ? C223 C224 1.376(10) . ? P3 C301 1.788(7) . ? P3 C313 1.788(6) . ? P3 C319 1.788(7) . ? P3 C307 1.792(7) . ? C301 C306 1.385(9) . ? C301 C302 1.400(10) . ? C302 C303 1.369(11) . ? C303 C304 1.357(11) . ? C304 C305 1.349(11) . ? C305 C306 1.364(10) . ? C307 C312 1.385(10) . ? C307 C308 1.397(9) . ? C308 C309 1.359(12) . ? C309 C310 1.361(14) . ? C310 C311 1.377(13) . ? C311 C312 1.375(12) . ? C313 C318 1.378(10) . ? C313 C314 1.386(9) . ? C314 C315 1.383(9) . ? C315 C316 1.366(11) . ? C316 C317 1.354(11) . ? C317 C318 1.386(9) . ? C319 C320 1.363(9) . ? C319 C324 1.397(6) . ? C320 C321 1.375(10) . ? C321 C322 1.384(10) . ? C322 C323 1.359(11) . ? C323 C324 1.353(8) . ? C7 N7 1.0173 . ? C7 C8 1.6595 . ? 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 C1 Re1 Se1 91.0(2) . . ? C1 Re1 Se2 90.36(17) . . ? Se1 Re1 Se2 89.58(3) . . ? C1 Re1 Se3 93.31(17) . . ? Se1 Re1 Se3 89.77(3) . . ? Se2 Re1 Se3 176.29(2) . . ? C1 Re1 Se4 92.3(2) . . ? Se1 Re1 Se4 176.77(2) . . ? Se2 Re1 Se4 90.46(3) . . ? Se3 Re1 Se4 89.99(3) . . ? C1 Re1 Re3 134.3(2) . 2_755 ? Se1 Re1 Re3 118.681(18) . 2_755 ? Se2 Re1 Re3 58.675(19) . 2_755 ? Se3 Re1 Re3 118.65(2) . 2_755 ? Se4 Re1 Re3 58.772(17) . 2_755 ? C1 Re1 Re3 135.7(2) . . ? Se1 Re1 Re3 58.694(19) . . ? Se2 Re1 Re3 118.177(18) . . ? Se3 Re1 Re3 58.505(17) . . ? Se4 Re1 Re3 118.59(2) . . ? Re3 Re1 Re3 89.945(13) 2_755 . ? C1 Re1 Re2 136.29(18) . . ? Se1 Re1 Re2 118.76(2) . . ? Se2 Re1 Re2 118.87(2) . . ? Se3 Re1 Re2 58.458(19) . . ? Se4 Re1 Re2 58.534(18) . . ? Re3 Re1 Re2 60.206(14) 2_755 . ? Re3 Re1 Re2 60.071(11) . . ? C1 Re1 Re2 133.27(18) . 2_755 ? Se1 Re1 Re2 58.604(16) . 2_755 ? Se2 Re1 Re2 58.116(18) . 2_755 ? Se3 Re1 Re2 118.57(2) . 2_755 ? Se4 Re1 Re2 118.852(18) . 2_755 ? Re3 Re1 Re2 60.089(10) 2_755 2_755 ? Re3 Re1 Re2 60.071(12) . 2_755 ? Re2 Re1 Re2 90.432(13) . 2_755 ? C1 Re1 Re1 178.33(17) . 2_755 ? Se1 Re1 Re1 88.346(18) . 2_755 ? Se2 Re1 Re1 88.115(17) . 2_755 ? Se3 Re1 Re1 88.210(18) . 2_755 ? Se4 Re1 Re1 88.432(18) . 2_755 ? Re3 Re1 Re1 45.039(9) 2_755 2_755 ? Re3 Re1 Re1 44.906(9) . 2_755 ? Re2 Re1 Re1 45.266(10) . 2_755 ? Re2 Re1 Re1 45.166(9) 2_755 2_755 ? C2 Re2 Se2 90.87(17) . 2_755 ? C2 Re2 Se3 92.10(17) . . ? Se2 Re2 Se3 89.95(2) 2_755 . ? C2 Re2 Se4 92.88(17) . . ? Se2 Re2 Se4 176.26(2) 2_755 . ? Se3 Re2 Se4 89.99(2) . . ? C2 Re2 Se1 92.29(17) . 2_755 ? Se2 Re2 Se1 89.56(2) 2_755 2_755 ? Se3 Re2 Se1 175.60(2) . 2_755 ? Se4 Re2 Se1 90.20(3) . 2_755 ? C2 Re2 Re3 134.57(18) . . ? Se2 Re2 Re3 58.658(19) 2_755 . ? Se3 Re2 Re3 58.447(18) . . ? Se4 Re2 Re3 118.32(2) . . ? Se1 Re2 Re3 117.765(19) 2_755 . ? C2 Re2 Re1 135.88(16) . . ? Se2 Re2 Re1 118.50(2) 2_755 . ? Se3 Re2 Re1 58.52(2) . . ? Se4 Re2 Re1 58.483(19) . . ? Se1 Re2 Re1 118.09(2) 2_755 . ? Re3 Re2 Re1 59.854(11) . . ? C2 Re2 Re3 135.91(18) . 2_755 ? Se2 Re2 Re3 118.324(18) 2_755 2_755 ? Se3 Re2 Re3 118.17(2) . 2_755 ? Se4 Re2 Re3 58.566(16) . 2_755 ? Se1 Re2 Re3 58.438(19) 2_755 2_755 ? Re3 Re2 Re3 89.512(14) . 2_755 ? Re1 Re2 Re3 59.672(12) . 2_755 ? C2 Re2 Re1 134.55(16) . 2_755 ? Se2 Re2 Re1 58.566(17) 2_755 2_755 ? Se3 Re2 Re1 118.077(19) . 2_755 ? Se4 Re2 Re1 118.321(19) . 2_755 ? Se1 Re2 Re1 58.133(18) 2_755 2_755 ? Re3 Re2 Re1 59.643(10) . 2_755 ? Re1 Re2 Re1 89.568(13) . 2_755 ? Re3 Re2 Re1 59.767(11) 2_755 2_755 ? C2 Re2 Re2 179.04(17) . 2_755 ? Se2 Re2 Re2 88.174(19) 2_755 2_755 ? Se3 Re2 Re2 87.95(2) . 2_755 ? Se4 Re2 Re2 88.083(19) . 2_755 ? Se1 Re2 Re2 87.66(2) 2_755 2_755 ? Re3 Re2 Re2 44.781(9) . 2_755 ? Re1 Re2 Re2 44.833(9) . 2_755 ? Re3 Re2 Re2 44.731(10) 2_755 2_755 ? Re1 Re2 Re2 44.734(10) 2_755 2_755 ? C3 Re3 Se3 92.40(17) . . ? C3 Re3 Se1 92.3(2) . . ? Se3 Re3 Se1 89.59(2) . . ? C3 Re3 Se2 91.5(2) . 2_755 ? Se3 Re3 Se2 89.68(2) . 2_755 ? Se1 Re3 Se2 176.13(3) . 2_755 ? C3 Re3 Se4 90.92(17) . 2_755 ? Se3 Re3 Se4 176.67(3) . 2_755 ? Se1 Re3 Se4 90.18(2) . 2_755 ? Se2 Re3 Se4 90.33(2) 2_755 2_755 ? C3 Re3 Re1 134.11(18) . 2_755 ? Se3 Re3 Re1 118.75(2) . 2_755 ? Se1 Re3 Re1 118.61(2) . 2_755 ? Se2 Re3 Re1 58.634(19) 2_755 2_755 ? Se4 Re3 Re1 58.606(19) 2_755 2_755 ? C3 Re3 Re1 135.83(19) . . ? Se3 Re3 Re1 58.610(19) . . ? Se1 Re3 Re1 58.295(19) . . ? Se2 Re3 Re1 118.23(2) 2_755 . ? Se4 Re3 Re1 118.60(2) 2_755 . ? Re1 Re3 Re1 90.055(13) 2_755 . ? C3 Re3 Re2 135.0(2) . . ? Se3 Re3 Re2 58.493(18) . . ? Se1 Re3 Re2 118.37(2) . . ? Se2 Re3 Re2 58.166(18) 2_755 . ? Se4 Re3 Re2 118.87(2) 2_755 . ? Re1 Re3 Re2 60.268(11) 2_755 . ? Re1 Re3 Re2 60.076(12) . . ? C3 Re3 Re2 134.52(19) . 2_755 ? Se3 Re3 Re2 118.77(2) . 2_755 ? Se1 Re3 Re2 58.512(18) . 2_755 ? Se2 Re3 Re2 118.74(2) 2_755 2_755 ? Se4 Re3 Re2 58.453(19) 2_755 2_755 ? Re1 Re3 Re2 60.122(12) 2_755 2_755 ? Re1 Re3 Re2 60.162(11) . 2_755 ? Re2 Re3 Re2 90.488(14) . 2_755 ? C3 Re3 Re3 179.17(17) . 2_755 ? Se3 Re3 Re3 88.335(19) . 2_755 ? Se1 Re3 Re3 88.06(2) . 2_755 ? Se2 Re3 Re3 88.12(2) 2_755 2_755 ? Se4 Re3 Re3 88.337(19) 2_755 2_755 ? Re1 Re3 Re3 45.094(9) 2_755 2_755 ? Re1 Re3 Re3 44.961(9) . 2_755 ? Re2 Re3 Re3 45.269(11) . 2_755 ? Re2 Re3 Re3 45.218(10) 2_755 2_755 ? Re1 Se1 Re3 63.011(19) . . ? Re1 Se1 Re2 63.263(19) . 2_755 ? Re3 Se1 Re2 63.05(2) . 2_755 ? Re2 Se2 Re1 63.318(19) 2_755 . ? Re2 Se2 Re3 63.176(19) 2_755 2_755 ? Re1 Se2 Re3 62.691(19) . 2_755 ? Re3 Se3 Re2 63.061(16) . . ? Re3 Se3 Re1 62.885(17) . . ? Re2 Se3 Re1 63.025(18) . . ? Re1 Se4 Re2 62.983(19) . . ? Re1 Se4 Re3 62.622(17) . 2_755 ? Re2 Se4 Re3 62.980(18) . 2_755 ? N1 C1 Re1 178.1(6) . . ? N2 C2 Re2 178.0(6) . . ? N3 C3 Re3 178.4(8) . . ? C4 Re4 Se5 89.96(18) . . ? C4 Re4 Se8 90.25(18) . . ? Se5 Re4 Se8 90.06(3) . . ? C4 Re4 Se6 93.65(18) . . ? Se5 Re4 Se6 89.91(3) . . ? Se8 Re4 Se6 176.09(2) . . ? C4 Re4 Se7 93.64(18) . . ? Se5 Re4 Se7 176.40(2) . . ? Se8 Re4 Se7 90.01(3) . . ? Se6 Re4 Se7 89.77(3) . . ? C4 Re4 Re5 132.58(18) . 2_756 ? Se5 Re4 Re5 58.709(18) . 2_756 ? Se8 Re4 Re5 58.40(2) . 2_756 ? Se6 Re4 Re5 118.46(2) . 2_756 ? Se7 Re4 Re5 118.467(19) . 2_756 ? C4 Re4 Re5 137.53(18) . . ? Se5 Re4 Re5 118.64(2) . . ? Se8 Re4 Re5 118.182(19) . . ? Se6 Re4 Re5 58.582(17) . . ? Se7 Re4 Re5 58.298(18) . . ? Re5 Re4 Re5 89.893(13) 2_756 . ? C4 Re4 Re6 135.05(18) . . ? Se5 Re4 Re6 58.609(19) . . ? Se8 Re4 Re6 118.30(2) . . ? Se6 Re4 Re6 58.556(19) . . ? Se7 Re4 Re6 118.33(2) . . ? Re5 Re4 Re6 59.913(12) 2_756 . ? Re5 Re4 Re6 60.044(12) . . ? C4 Re4 Re6 134.85(18) . 2_756 ? Se5 Re4 Re6 118.73(2) . 2_756 ? Se8 Re4 Re6 58.323(18) . 2_756 ? Se6 Re4 Re6 118.445(19) . 2_756 ? Se7 Re4 Re6 58.450(18) . 2_756 ? Re5 Re4 Re6 60.033(10) 2_756 2_756 ? Re5 Re4 Re6 59.874(11) . 2_756 ? Re6 Re4 Re6 89.989(13) . 2_756 ? C4 Re4 Re4 177.53(18) . 2_756 ? Se5 Re4 Re4 88.388(19) . 2_756 ? Se8 Re4 Re4 87.917(19) . 2_756 ? Se6 Re4 Re4 88.18(2) . 2_756 ? Se7 Re4 Re4 88.014(18) . 2_756 ? Re5 Re4 Re4 44.959(9) 2_756 2_756 ? Re5 Re4 Re4 44.934(11) . 2_756 ? Re6 Re4 Re4 45.017(9) . 2_756 ? Re6 Re4 Re4 44.973(8) 2_756 2_756 ? C5 Re5 Se8 92.5(2) . 2_756 ? C5 Re5 Se7 91.0(2) . . ? Se8 Re5 Se7 176.53(3) 2_756 . ? C5 Re5 Se5 90.76(18) . 2_756 ? Se8 Re5 Se5 89.83(2) 2_756 2_756 ? Se7 Re5 Se5 90.18(2) . 2_756 ? C5 Re5 Se6 92.97(18) . . ? Se8 Re5 Se6 89.75(2) 2_756 . ? Se7 Re5 Se6 90.01(2) . . ? Se5 Re5 Se6 176.27(3) 2_756 . ? C5 Re5 Re6 133.7(2) . 2_756 ? Se8 Re5 Re6 118.56(2) 2_756 2_756 ? Se7 Re5 Re6 58.677(19) . 2_756 ? Se5 Re5 Re6 58.517(19) 2_756 2_756 ? Se6 Re5 Re6 118.63(2) . 2_756 ? C5 Re5 Re4 134.48(18) . 2_756 ? Se8 Re5 Re4 58.503(19) 2_756 2_756 ? Se7 Re5 Re4 118.75(2) . 2_756 ? Se5 Re5 Re4 58.230(19) 2_756 2_756 ? Se6 Re5 Re4 118.56(2) . 2_756 ? Re6 Re5 Re4 60.077(12) 2_756 2_756 ? C5 Re5 Re4 135.38(18) . . ? Se8 Re5 Re4 118.34(2) 2_756 . ? Se7 Re5 Re4 58.752(19) . . ? Se5 Re5 Re4 118.61(2) 2_756 . ? Se6 Re5 Re4 58.522(18) . . ? Re6 Re5 Re4 60.113(11) 2_756 . ? Re4 Re5 Re4 90.107(13) 2_756 . ? C5 Re5 Re6 136.2(2) . . ? Se8 Re5 Re6 58.36(2) 2_756 . ? Se7 Re5 Re6 118.73(2) . . ? Se5 Re5 Re6 118.28(2) 2_756 . ? Se6 Re5 Re6 58.518(19) . . ? Re6 Re5 Re6 90.096(13) 2_756 . ? Re4 Re5 Re6 60.055(11) 2_756 . ? Re4 Re5 Re6 59.990(11) . . ? C5 Re5 Re5 178.7(2) . 2_756 ? Se8 Re5 Re5 88.07(2) 2_756 2_756 ? Se7 Re5 Re5 88.46(2) . 2_756 ? Se5 Re5 Re5 88.08(2) 2_756 2_756 ? Se6 Re5 Re5 88.21(2) . 2_756 ? Re6 Re5 Re5 45.111(9) 2_756 2_756 ? Re4 Re5 Re5 45.066(11) 2_756 2_756 ? Re4 Re5 Re5 45.041(9) . 2_756 ? Re6 Re5 Re5 44.985(9) . 2_756 ? C6 Re6 Se8 90.19(19) . 2_756 ? C6 Re6 Se5 93.68(19) . . ? Se8 Re6 Se5 176.11(3) 2_756 . ? C6 Re6 Se7 90.4(2) . 2_756 ? Se8 Re6 Se7 90.21(2) 2_756 2_756 ? Se5 Re6 Se7 90.08(3) . 2_756 ? C6 Re6 Se6 93.3(2) . . ? Se8 Re6 Se6 89.79(3) 2_756 . ? Se5 Re6 Se6 89.66(2) . . ? Se7 Re6 Se6 176.32(3) 2_756 . ? C6 Re6 Re5 135.2(2) . 2_756 ? Se8 Re6 Re5 118.46(2) 2_756 2_756 ? Se5 Re6 Re5 58.627(18) . 2_756 ? Se7 Re6 Re5 58.40(2) 2_756 2_756 ? Se6 Re6 Re5 118.52(2) . 2_756 ? C6 Re6 Re4 137.23(18) . . ? Se8 Re6 Re4 118.36(2) 2_756 . ? Se5 Re6 Re4 58.24(2) . . ? Se7 Re6 Re4 118.41(2) 2_756 . ? Se6 Re6 Re4 58.522(19) . . ? Re5 Re6 Re4 60.010(12) 2_756 . ? C6 Re6 Re5 134.8(2) . . ? Se8 Re6 Re5 58.40(2) 2_756 . ? Se5 Re6 Re5 118.20(2) . . ? Se7 Re6 Re5 118.526(19) 2_756 . ? Se6 Re6 Re5 58.544(18) . . ? Re5 Re6 Re5 89.904(13) 2_756 . ? Re4 Re6 Re5 59.966(13) . . ? C6 Re6 Re4 132.76(18) . 2_756 ? Se8 Re6 Re4 58.465(18) 2_756 2_756 ? Se5 Re6 Re4 118.62(2) . 2_756 ? Se7 Re6 Re4 58.631(18) 2_756 2_756 ? Se6 Re6 Re4 118.45(2) . 2_756 ? Re5 Re6 Re4 60.013(12) 2_756 2_756 ? Re4 Re6 Re4 90.011(13) . 2_756 ? Re5 Re6 Re4 59.912(11) . 2_756 ? C6 Re6 Re6 177.73(18) . 2_756 ? Se8 Re6 Re6 88.04(2) 2_756 2_756 ? Se5 Re6 Re6 88.10(2) . 2_756 ? Se7 Re6 Re6 88.167(19) 2_756 2_756 ? Se6 Re6 Re6 88.16(2) . 2_756 ? Re5 Re6 Re6 45.015(9) 2_756 2_756 ? Re4 Re6 Re6 45.027(9) . 2_756 ? Re5 Re6 Re6 44.889(9) . 2_756 ? Re4 Re6 Re6 44.983(9) 2_756 2_756 ? Re4 Se5 Re6 63.150(18) . . ? Re4 Se5 Re5 63.061(18) . 2_756 ? Re6 Se5 Re5 62.855(17) . 2_756 ? Re4 Se6 Re6 62.922(19) . . ? Re4 Se6 Re5 62.896(19) . . ? Re6 Se6 Re5 62.938(17) . . ? Re5 Se7 Re6 62.919(19) . 2_756 ? Re5 Se7 Re4 62.95(2) . . ? Re6 Se7 Re4 62.92(2) 2_756 . ? Re6 Se8 Re5 63.234(19) 2_756 2_756 ? Re6 Se8 Re4 63.212(19) 2_756 . ? Re5 Se8 Re4 63.094(19) 2_756 . ? N4 C4 Re4 177.3(6) . . ? N5 C5 Re5 177.2(7) . . ? N6 C6 Re6 177.1(7) . . ? C107 P1 C101 108.7(3) . . ? C107 P1 C119 108.7(3) . . ? C101 P1 C119 110.1(4) . . ? C107 P1 C113 110.1(4) . . ? C101 P1 C113 110.3(3) . . ? C119 P1 C113 108.9(4) . . ? C106 C101 C102 118.5(7) . . ? C106 C101 P1 120.4(6) . . ? C102 C101 P1 120.9(6) . . ? C103 C102 C101 120.3(8) . . ? C104 C103 C102 119.6(8) . . ? C105 C104 C103 120.2(8) . . ? C106 C105 C104 121.5(9) . . ? C105 C106 C101 119.8(8) . . ? C112 C107 C108 118.9(6) . . ? C112 C107 P1 122.0(5) . . ? C108 C107 P1 118.9(6) . . ? C109 C108 C107 120.0(8) . . ? C110 C109 C108 119.8(7) . . ? C109 C110 C111 120.6(7) . . ? C112 C111 C110 120.3(9) . . ? C111 C112 C107 120.3(8) . . ? C114 C113 C118 118.6(8) . . ? C114 C113 P1 120.6(7) . . ? C118 C113 P1 120.8(6) . . ? C113 C114 C115 120.0(9) . . ? C116 C115 C114 120.7(10) . . ? C115 C116 C117 120.4(10) . . ? C116 C117 C118 119.9(11) . . ? C113 C118 C117 120.2(10) . . ? C124 C119 C120 118.7(8) . . ? C124 C119 P1 121.8(7) . . ? C120 C119 P1 119.3(7) . . ? C121 C120 C119 120.4(9) . . ? C122 C121 C120 119.4(10) . . ? C121 C122 C123 121.9(10) . . ? C122 C123 C124 119.4(10) . . ? C119 C124 C123 120.1(10) . . ? C201 P2 C213 109.4(3) . . ? C201 P2 C219 110.1(3) . . ? C213 P2 C219 109.0(3) . . ? C201 P2 C207 109.6(3) . . ? C213 P2 C207 109.9(3) . . ? C219 P2 C207 108.9(3) . . ? C202 C201 C206 118.9(7) . . ? C202 C201 P2 120.7(5) . . ? C206 C201 P2 120.3(6) . . ? C203 C202 C201 121.4(8) . . ? C204 C203 C202 118.8(8) . . ? C205 C204 C203 120.9(8) . . ? C204 C205 C206 120.4(8) . . ? C205 C206 C201 119.6(7) . . ? C208 C207 C212 119.5(7) . . ? C208 C207 P2 121.0(5) . . ? C212 C207 P2 119.3(6) . . ? C209 C208 C207 120.5(8) . . ? C210 C209 C208 117.4(9) . . ? C211 C210 C209 124.0(8) . . ? C210 C211 C212 118.2(9) . . ? C211 C212 C207 120.1(9) . . ? C214 C213 C218 118.6(7) . . ? C214 C213 P2 120.8(6) . . ? C218 C213 P2 120.4(5) . . ? C215 C214 C213 119.9(8) . . ? C216 C215 C214 121.1(8) . . ? C215 C216 C217 119.7(9) . . ? C216 C217 C218 121.1(9) . . ? C217 C218 C213 119.7(8) . . ? C220 C219 C224 119.9(7) . . ? C220 C219 P2 121.2(5) . . ? C224 C219 P2 118.8(6) . . ? C219 C220 C221 119.7(8) . . ? C222 C221 C220 119.5(9) . . ? C223 C222 C221 121.3(8) . . ? C222 C223 C224 120.5(9) . . ? C223 C224 C219 119.0(9) . . ? C301 P3 C313 111.2(3) . . ? C301 P3 C319 107.8(3) . . ? C313 P3 C319 108.7(3) . . ? C301 P3 C307 110.5(3) . . ? C313 P3 C307 106.3(3) . . ? C319 P3 C307 112.4(3) . . ? C306 C301 C302 118.2(7) . . ? C306 C301 P3 119.1(5) . . ? C302 C301 P3 122.6(6) . . ? C303 C302 C301 119.3(8) . . ? C304 C303 C302 121.2(8) . . ? C305 C304 C303 119.8(8) . . ? C304 C305 C306 120.9(8) . . ? C305 C306 C301 120.4(8) . . ? C312 C307 C308 118.3(7) . . ? C312 C307 P3 120.1(6) . . ? C308 C307 P3 121.6(6) . . ? C309 C308 C307 119.7(8) . . ? C308 C309 C310 122.0(9) . . ? C309 C310 C311 119.2(9) . . ? C312 C311 C310 119.9(9) . . ? C311 C312 C307 120.8(8) . . ? C318 C313 C314 119.2(6) . . ? C318 C313 P3 119.2(5) . . ? C314 C313 P3 121.6(6) . . ? C315 C314 C313 118.7(7) . . ? C316 C315 C314 121.3(7) . . ? C317 C316 C315 120.4(7) . . ? C316 C317 C318 119.2(8) . . ? C313 C318 C317 121.2(7) . . ? C320 C319 C324 118.9(6) . . ? C320 C319 P3 121.7(5) . . ? C324 C319 P3 119.1(4) . . ? C319 C320 C321 120.7(7) . . ? C320 C321 C322 119.5(7) . . ? C323 C322 C321 119.8(7) . . ? C324 C323 C322 120.8(7) . . ? C323 C324 C319 120.2(5) . . ? N7 C7 C8 173.3 . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.88 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.176 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.133 #################### Material relevant to compound 3 at 150K ############ data_sb280150_abmerge _database_code_CSD 186998 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(PPh4)3 (RE6Se8(CN)6) CH3CN (H2O)3' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H69 N7 O3 P3 Re6 Se8' _chemical_formula_weight 3018.21 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4983(9) _cell_length_b 14.1705(10) _cell_length_c 25.9583(19) _cell_angle_alpha 74.976(8) _cell_angle_beta 89.776(8) _cell_angle_gamma 62.578(8) _cell_volume 4217.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7995 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description platelet _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.4620 _exptl_crystal_size_mid 0.3850 _exptl_crystal_size_min 0.1386 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2778 _exptl_absorpt_coefficient_mu 12.134 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0531 _exptl_absorpt_correction_T_max 0.2469 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_special_details ; 'The hydrogen atoms on the water molecules were not found on the Fourier map' ; _diffrn_ambient_temperature 150(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 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, PHi. incr. == 0.9' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41780 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.88 _reflns_number_total 15278 _reflns_number_gt 11832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0230P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000068(10) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 15278 _refine_ls_number_parameters 948 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max 0.003 _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 0.977946(19) 0.079559(18) 0.049541(8) 0.01432(5) Uani 1 1 d . . . Re2 Re 1.154209(19) -0.084055(18) 0.027127(8) 0.01431(5) Uani 1 1 d . . . Re3 Re 0.971818(19) -0.102929(18) 0.049015(8) 0.01442(5) Uani 1 1 d . . . Se1 Se 0.80601(5) 0.05783(5) 0.06915(2) 0.01877(12) Uani 1 1 d . . . Se2 Se 0.85840(5) 0.25436(5) -0.02535(2) 0.01819(12) Uani 1 1 d . . . Se3 Se 1.09785(5) -0.10291(5) 0.12051(2) 0.01833(12) Uani 1 1 d . . . Se4 Se 1.15293(5) 0.09489(5) 0.02641(2) 0.01801(12) Uani 1 1 d . . . C1 C 0.9500(5) 0.1739(5) 0.1043(2) 0.0218(13) Uani 1 1 d . . . C2 C 1.3276(5) -0.1809(5) 0.0575(2) 0.0192(13) Uani 1 1 d . . . C3 C 0.9407(5) -0.2219(5) 0.1032(2) 0.0231(14) Uani 1 1 d . . . N1 N 0.9322(5) 0.2299(5) 0.1322(2) 0.0311(13) Uani 1 1 d . . . N2 N 1.4215(4) -0.2369(4) 0.0745(2) 0.0241(12) Uani 1 1 d . . . N3 N 0.9221(5) -0.2868(5) 0.1323(2) 0.0356(14) Uani 1 1 d . . . Re4 Re 0.959712(19) 0.070045(18) 0.426066(8) 0.01534(6) Uani 1 1 d . . . Re5 Re 1.147936(19) -0.081655(18) 0.489123(8) 0.01555(6) Uani 1 1 d . . . Re6 Re 0.968632(19) -0.110882(18) 0.491911(9) 0.01609(6) Uani 1 1 d . . . Se5 Se 0.79066(5) 0.03963(5) 0.43163(2) 0.02007(13) Uani 1 1 d . . . Se6 Se 1.07380(5) -0.11805(5) 0.41128(2) 0.01985(13) Uani 1 1 d . . . Se7 Se 1.13397(5) 0.09403(5) 0.42674(2) 0.02042(13) Uani 1 1 d . . . Se8 Se 0.84997(5) 0.25075(5) 0.44791(2) 0.02144(13) Uani 1 1 d . . . C4 C 0.9056(5) 0.1539(5) 0.3433(2) 0.0207(13) Uani 1 1 d . . . C5 C 1.3158(5) -0.1706(5) 0.4779(2) 0.0236(14) Uani 1 1 d . . . C6 C 0.9330(5) -0.2385(5) 0.4864(2) 0.0245(14) Uani 1 1 d . . . N4 N 0.8723(5) 0.2034(4) 0.2983(2) 0.0269(12) Uani 1 1 d . . . N5 N 1.4103(5) -0.2175(5) 0.4727(2) 0.0390(15) Uani 1 1 d . . . N6 N 0.9132(6) -0.3090(5) 0.4854(3) 0.0450(16) Uani 1 1 d . . . P1 P 0.49482(13) 0.86788(13) 0.31940(6) 0.0191(3) Uani 1 1 d . . . C101 C 0.5326(5) 0.7258(5) 0.3515(2) 0.0210(13) Uani 1 1 d . . . C102 C 0.6454(5) 0.6441(6) 0.3636(2) 0.0282(15) Uani 1 1 d . . . H102 H 0.7016 0.6627 0.3531 0.034 Uiso 1 1 calc R . . C103 C 0.6736(6) 0.5363(6) 0.3909(3) 0.0338(16) Uani 1 1 d . . . H103 H 0.7488 0.4819 0.3990 0.041 Uiso 1 1 calc R . . C104 C 0.5896(6) 0.5088(6) 0.4065(3) 0.0355(17) Uani 1 1 d . . . H104 H 0.6086 0.4357 0.4247 0.043 Uiso 1 1 calc R . . C105 C 0.4784(6) 0.5889(6) 0.3950(3) 0.0308(15) Uani 1 1 d . . . H105 H 0.4223 0.5703 0.4059 0.037 Uiso 1 1 calc R . . C106 C 0.4509(6) 0.6956(6) 0.3677(2) 0.0274(15) Uani 1 1 d . . . H106 H 0.3755 0.7493 0.3597 0.033 Uiso 1 1 calc R . . C107 C 0.3526(5) 0.9382(5) 0.2867(2) 0.0219(13) Uani 1 1 d . . . C108 C 0.3332(6) 0.9492(6) 0.2322(2) 0.0258(14) Uani 1 1 d . . . H108 H 0.3930 0.9236 0.2126 0.031 Uiso 1 1 calc R . . C109 C 0.2236(6) 0.9989(7) 0.2080(3) 0.0373(18) Uani 1 1 d . . . H109 H 0.2103 1.0058 0.1717 0.045 Uiso 1 1 calc R . . C110 C 0.1349(6) 1.0378(7) 0.2351(3) 0.042(2) Uani 1 1 d . . . H110 H 0.0617 1.0730 0.2175 0.050 Uiso 1 1 calc R . . C111 C 0.1541(6) 1.0248(7) 0.2896(3) 0.044(2) Uani 1 1 d . . . H111 H 0.0932 1.0501 0.3086 0.053 Uiso 1 1 calc R . . C112 C 0.2607(6) 0.9754(6) 0.3156(3) 0.0312(16) Uani 1 1 d . . . H112 H 0.2727 0.9664 0.3523 0.037 Uiso 1 1 calc R . . C113 C 0.5075(6) 0.9332(5) 0.3685(2) 0.0249(14) Uani 1 1 d . . . C114 C 0.5892(5) 0.8721(6) 0.4126(2) 0.0278(15) Uani 1 1 d . . . H114 H 0.6343 0.7961 0.4186 0.033 Uiso 1 1 calc R . . C115 C 0.6042(7) 0.9242(8) 0.4481(3) 0.0418(19) Uani 1 1 d . . . H115 H 0.6600 0.8835 0.4777 0.050 Uiso 1 1 calc R . . C116 C 0.5359(8) 1.0364(8) 0.4393(3) 0.048(2) Uani 1 1 d . . . H116 H 0.5464 1.0713 0.4629 0.058 Uiso 1 1 calc R . . C117 C 0.4538(8) 1.0966(7) 0.3966(3) 0.052(2) Uani 1 1 d . . . H117 H 0.4075 1.1721 0.3915 0.062 Uiso 1 1 calc R . . C118 C 0.4382(7) 1.0456(6) 0.3601(3) 0.0422(19) Uani 1 1 d . . . H118 H 0.3821 1.0868 0.3307 0.051 Uiso 1 1 calc R . . C119 C 0.5850(5) 0.8768(5) 0.2692(2) 0.0230(13) Uani 1 1 d . . . C120 C 0.6032(6) 0.9686(6) 0.2561(3) 0.0308(15) Uani 1 1 d . . . H120 H 0.5722 1.0228 0.2739 0.037 Uiso 1 1 calc R . . C121 C 0.6682(6) 0.9773(7) 0.2160(3) 0.042(2) Uani 1 1 d . . . H121 H 0.6808 1.0384 0.2070 0.050 Uiso 1 1 calc R . . C122 C 0.7147(6) 0.8992(7) 0.1892(3) 0.0371(18) Uani 1 1 d . . . H122 H 0.7595 0.9064 0.1627 0.045 Uiso 1 1 calc R . . C123 C 0.6945(6) 0.8099(7) 0.2019(3) 0.0383(18) Uani 1 1 d . . . H123 H 0.7251 0.7571 0.1833 0.046 Uiso 1 1 calc R . . C124 C 0.6294(5) 0.7967(6) 0.2418(2) 0.0297(15) Uani 1 1 d . . . H124 H 0.6158 0.7362 0.2501 0.036 Uiso 1 1 calc R . . P2 P 1.64486(13) -0.28983(13) -0.08492(6) 0.0191(3) Uani 1 1 d . . . C201 C 1.5682(5) -0.1482(5) -0.0833(2) 0.0187(12) Uani 1 1 d . . . C202 C 1.6025(5) -0.0725(5) -0.1099(2) 0.0221(13) Uani 1 1 d . . . H202 H 1.6614 -0.0941 -0.1304 0.027 Uiso 1 1 calc R . . C203 C 1.5493(6) 0.0358(5) -0.1064(2) 0.0270(15) Uani 1 1 d . . . H203 H 1.5735 0.0862 -0.1237 0.032 Uiso 1 1 calc R . . C204 C 1.4602(6) 0.0677(5) -0.0768(2) 0.0271(15) Uani 1 1 d . . . H204 H 1.4233 0.1403 -0.0747 0.032 Uiso 1 1 calc R . . C205 C 1.4254(5) -0.0087(5) -0.0501(2) 0.0261(14) Uani 1 1 d . . . H205 H 1.3651 0.0134 -0.0304 0.031 Uiso 1 1 calc R . . C206 C 1.4799(5) -0.1170(6) -0.0527(2) 0.0265(14) Uani 1 1 d . . . H206 H 1.4579 -0.1684 -0.0342 0.032 Uiso 1 1 calc R . . C207 C 1.5485(5) -0.3437(5) -0.0876(2) 0.0215(13) Uani 1 1 d . . . C208 C 1.5824(6) -0.4556(6) -0.0623(2) 0.0293(15) Uani 1 1 d . . . H208 H 1.6539 -0.5017 -0.0429 0.035 Uiso 1 1 calc R . . C209 C 1.5094(7) -0.4978(6) -0.0661(3) 0.0369(17) Uani 1 1 d . . . H209 H 1.5319 -0.5725 -0.0497 0.044 Uiso 1 1 calc R . . C210 C 1.4023(6) -0.4276(7) -0.0946(3) 0.0387(18) Uani 1 1 d . . . H210 H 1.3537 -0.4560 -0.0983 0.046 Uiso 1 1 calc R . . C211 C 1.3681(7) -0.3181(7) -0.1170(3) 0.045(2) Uani 1 1 d . . . H211 H 1.2948 -0.2715 -0.1344 0.054 Uiso 1 1 calc R . . C212 C 1.4397(6) -0.2747(6) -0.1147(3) 0.0332(16) Uani 1 1 d . . . H212 H 1.4157 -0.1997 -0.1311 0.040 Uiso 1 1 calc R . . C213 C 1.7166(5) -0.2961(5) -0.1436(2) 0.0208(13) Uani 1 1 d . . . C214 C 1.6646(6) -0.2923(5) -0.1907(2) 0.0279(15) Uani 1 1 d . . . H214 H 1.5950 -0.2908 -0.1913 0.034 Uiso 1 1 calc R . . C215 C 1.7168(6) -0.2908(6) -0.2368(2) 0.0328(16) Uani 1 1 d . . . H215 H 1.6829 -0.2898 -0.2683 0.039 Uiso 1 1 calc R . . C216 C 1.8187(7) -0.2908(6) -0.2360(3) 0.0397(18) Uani 1 1 d . . . H216 H 1.8529 -0.2890 -0.2672 0.048 Uiso 1 1 calc R . . C217 C 1.8709(6) -0.2934(6) -0.1896(3) 0.0353(17) Uani 1 1 d . . . H217 H 1.9401 -0.2941 -0.1893 0.042 Uiso 1 1 calc R . . C218 C 1.8182(5) -0.2951(6) -0.1434(3) 0.0299(15) Uani 1 1 d . . . H218 H 1.8519 -0.2955 -0.1121 0.036 Uiso 1 1 calc R . . C219 C 1.7459(5) -0.3708(5) -0.0257(2) 0.0206(13) Uani 1 1 d . . . C220 C 1.8343(6) -0.4749(6) -0.0233(3) 0.0292(15) Uani 1 1 d . . . H220 H 1.8461 -0.4993 -0.0539 0.035 Uiso 1 1 calc R . . C221 C 1.9046(6) -0.5422(6) 0.0245(3) 0.0316(16) Uani 1 1 d . . . H221 H 1.9619 -0.6130 0.0267 0.038 Uiso 1 1 calc R . . C222 C 1.8889(6) -0.5028(6) 0.0697(3) 0.0383(18) Uani 1 1 d . . . H222 H 1.9369 -0.5473 0.1017 0.046 Uiso 1 1 calc R . . C223 C 1.8036(7) -0.3994(7) 0.0673(3) 0.045(2) Uani 1 1 d . . . H223 H 1.7940 -0.3738 0.0975 0.055 Uiso 1 1 calc R . . C224 C 1.7320(6) -0.3333(6) 0.0198(3) 0.0375(18) Uani 1 1 d . . . H224 H 1.6739 -0.2632 0.0182 0.045 Uiso 1 1 calc R . . P3 P 1.11357(13) -0.39291(13) 0.31010(6) 0.0185(3) Uani 1 1 d . . . C301 C 1.0090(5) -0.2543(5) 0.3073(2) 0.0195(13) Uani 1 1 d . . . C302 C 1.0123(6) -0.1620(5) 0.2733(2) 0.0247(14) Uani 1 1 d . . . H302 H 1.0674 -0.1705 0.2506 0.030 Uiso 1 1 calc R . . C303 C 0.9306(6) -0.0563(5) 0.2743(3) 0.0298(15) Uani 1 1 d . . . H303 H 0.9311 0.0066 0.2522 0.036 Uiso 1 1 calc R . . C304 C 0.8491(5) -0.0453(5) 0.3082(2) 0.0264(15) Uani 1 1 d . . . H304 H 0.7953 0.0252 0.3087 0.032 Uiso 1 1 calc R . . C305 C 0.8464(5) -0.1357(5) 0.3404(3) 0.0274(15) Uani 1 1 d . . . H305 H 0.7911 -0.1265 0.3630 0.033 Uiso 1 1 calc R . . C306 C 0.9250(5) -0.2420(5) 0.3403(2) 0.0243(14) Uani 1 1 d . . . H306 H 0.9217 -0.3038 0.3618 0.029 Uiso 1 1 calc R . . C307 C 1.2003(5) -0.3915(5) 0.2579(2) 0.0237(14) Uani 1 1 d . . . C308 C 1.1903(6) -0.4219(5) 0.2116(2) 0.0268(14) Uani 1 1 d . . . H308 H 1.1363 -0.4432 0.2065 0.032 Uiso 1 1 calc R . . C309 C 1.2610(7) -0.4197(6) 0.1741(3) 0.0398(18) Uani 1 1 d . . . H309 H 1.2547 -0.4409 0.1438 0.048 Uiso 1 1 calc R . . C310 C 1.3410(6) -0.3874(6) 0.1794(3) 0.0374(17) Uani 1 1 d . . . H310 H 1.3890 -0.3881 0.1535 0.045 Uiso 1 1 calc R . . C311 C 1.3491(7) -0.3534(7) 0.2245(3) 0.0426(19) Uani 1 1 d . . . H311 H 1.4013 -0.3292 0.2282 0.051 Uiso 1 1 calc R . . C312 C 1.2799(5) -0.3557(6) 0.2633(3) 0.0306(16) Uani 1 1 d . . . H312 H 1.2859 -0.3334 0.2933 0.037 Uiso 1 1 calc R . . C313 C 1.2059(5) -0.4605(5) 0.3733(2) 0.0210(13) Uani 1 1 d . . . C314 C 1.1740(5) -0.4220(5) 0.4180(2) 0.0261(14) Uani 1 1 d . . . H314 H 1.1074 -0.3570 0.4152 0.031 Uiso 1 1 calc R . . C315 C 1.2434(6) -0.4826(6) 0.4668(3) 0.0350(17) Uani 1 1 d . . . H315 H 1.2222 -0.4584 0.4971 0.042 Uiso 1 1 calc R . . C316 C 1.3429(6) -0.5776(6) 0.4712(3) 0.0313(16) Uani 1 1 d . . . H316 H 1.3899 -0.6160 0.5038 0.038 Uiso 1 1 calc R . . C317 C 1.3728(6) -0.6159(5) 0.4266(3) 0.0294(15) Uani 1 1 d . . . H317 H 1.4392 -0.6812 0.4296 0.035 Uiso 1 1 calc R . . C318 C 1.3047(5) -0.5578(5) 0.3774(3) 0.0266(14) Uani 1 1 d . . . H318 H 1.3250 -0.5837 0.3475 0.032 Uiso 1 1 calc R . . C319 C 1.0402(5) -0.4694(5) 0.3050(2) 0.0190(12) Uani 1 1 d . . . C320 C 1.0553(5) -0.5605(5) 0.3463(3) 0.0268(14) Uani 1 1 d . . . H320 H 1.1094 -0.5878 0.3759 0.032 Uiso 1 1 calc R . . C321 C 0.9907(6) -0.6111(5) 0.3438(3) 0.0327(16) Uani 1 1 d . . . H321 H 0.9996 -0.6715 0.3720 0.039 Uiso 1 1 calc R . . C322 C 0.9112(6) -0.5715(6) 0.2985(3) 0.0351(17) Uani 1 1 d . . . H322 H 0.8681 -0.6064 0.2963 0.042 Uiso 1 1 calc R . . C323 C 0.8968(6) -0.4812(6) 0.2574(3) 0.0354(17) Uani 1 1 d . . . H323 H 0.8454 -0.4563 0.2269 0.043 Uiso 1 1 calc R . . C324 C 0.9585(2) -0.4267(2) 0.26079(10) 0.0284(15) Uani 1 1 d . . . H324 H 0.9455 -0.3627 0.2340 0.034 Uiso 1 1 calc R . . N7 N 0.5605(2) 0.2282(2) 0.27608(10) 0.117(5) Uani 1 1 d R . . C7 C 0.5795(2) 0.2967(2) 0.28388(10) 0.075(3) Uani 1 1 d R . . C8 C 0.6004(2) 0.3886(2) 0.29388(10) 0.099(5) Uani 1 1 d R . . H8A H 0.5374 0.4598 0.2764 0.149 Uiso 1 1 calc R . . H8B H 0.6675 0.3845 0.2796 0.149 Uiso 1 1 calc R . . H8C H 0.6092 0.3791 0.3319 0.149 Uiso 1 1 calc R . . O1 O 0.8042(2) 0.3731(2) 0.19527(10) 0.0407(13) Uani 1 1 d R . . O2 O 0.8991(2) 0.5461(2) 0.43517(10) 0.0663(19) Uani 1 1 d R . . O3 O 0.6142(2) 0.6150(2) 0.17237(10) 0.0596(17) Uani 1 1 d 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 Re1 0.01455(12) 0.01541(12) 0.01346(10) -0.00453(9) 0.00247(9) -0.00733(9) Re2 0.01350(12) 0.01492(11) 0.01454(10) -0.00395(9) 0.00201(9) -0.00693(9) Re3 0.01499(12) 0.01555(12) 0.01334(10) -0.00325(8) 0.00265(9) -0.00826(9) Se1 0.0169(3) 0.0220(3) 0.0184(3) -0.0069(2) 0.0067(2) -0.0096(3) Se2 0.0181(3) 0.0140(3) 0.0205(3) -0.0048(2) 0.0013(2) -0.0062(2) Se3 0.0203(3) 0.0201(3) 0.0138(2) -0.0036(2) 0.0012(2) -0.0096(3) Se4 0.0175(3) 0.0193(3) 0.0201(3) -0.0057(2) 0.0017(2) -0.0110(2) C1 0.022(3) 0.018(3) 0.016(3) 0.000(2) -0.001(2) -0.005(3) C2 0.020(3) 0.018(3) 0.023(3) -0.008(2) 0.005(3) -0.010(3) C3 0.029(4) 0.019(3) 0.025(3) -0.001(3) 0.001(3) -0.017(3) N1 0.030(3) 0.027(3) 0.030(3) -0.011(3) 0.000(2) -0.007(3) N2 0.019(3) 0.024(3) 0.031(3) -0.008(2) 0.004(2) -0.011(2) N3 0.043(4) 0.043(4) 0.033(3) -0.011(3) 0.007(3) -0.030(3) Re4 0.01417(12) 0.01265(11) 0.01563(10) -0.00249(9) 0.00176(9) -0.00432(9) Re5 0.01330(12) 0.01301(11) 0.01663(10) -0.00323(9) 0.00215(9) -0.00381(9) Re6 0.01604(12) 0.01258(11) 0.01822(11) -0.00393(9) 0.00272(9) -0.00594(10) Se5 0.0158(3) 0.0221(3) 0.0210(3) -0.0057(2) 0.0004(2) -0.0082(3) Se6 0.0205(3) 0.0176(3) 0.0189(3) -0.0075(2) 0.0036(2) -0.0060(3) Se7 0.0196(3) 0.0192(3) 0.0220(3) -0.0032(2) 0.0057(2) -0.0102(3) Se8 0.0214(3) 0.0116(3) 0.0233(3) -0.0015(2) 0.0023(2) -0.0033(2) C4 0.018(3) 0.016(3) 0.022(3) -0.004(2) 0.003(3) -0.005(3) C5 0.017(3) 0.030(4) 0.019(3) -0.009(3) 0.005(3) -0.007(3) C6 0.023(3) 0.021(3) 0.028(3) -0.005(3) 0.007(3) -0.010(3) N4 0.026(3) 0.024(3) 0.024(3) -0.002(2) 0.001(2) -0.009(2) N5 0.035(4) 0.040(4) 0.031(3) -0.008(3) 0.003(3) -0.010(3) N6 0.053(4) 0.034(4) 0.056(4) -0.016(3) 0.014(3) -0.026(3) P1 0.0192(8) 0.0186(8) 0.0170(7) -0.0027(6) 0.0015(6) -0.0082(7) C101 0.016(3) 0.023(3) 0.018(3) -0.005(2) 0.003(2) -0.005(3) C102 0.020(3) 0.032(4) 0.028(3) -0.008(3) 0.004(3) -0.010(3) C103 0.034(4) 0.023(4) 0.031(3) -0.001(3) -0.003(3) -0.007(3) C104 0.047(5) 0.020(3) 0.039(4) -0.005(3) 0.006(3) -0.017(3) C105 0.027(4) 0.028(4) 0.040(4) -0.006(3) 0.010(3) -0.017(3) C106 0.027(4) 0.031(4) 0.029(3) -0.012(3) 0.005(3) -0.015(3) C107 0.023(3) 0.017(3) 0.020(3) 0.000(2) 0.001(3) -0.008(3) C108 0.024(4) 0.037(4) 0.017(3) -0.003(3) 0.006(3) -0.017(3) C109 0.037(5) 0.052(5) 0.028(3) 0.005(3) -0.006(3) -0.034(4) C110 0.013(4) 0.049(5) 0.040(4) 0.020(4) -0.011(3) -0.014(3) C111 0.011(4) 0.047(5) 0.044(4) 0.006(4) 0.011(3) 0.001(3) C112 0.026(4) 0.027(4) 0.029(3) -0.006(3) 0.010(3) -0.005(3) C113 0.039(4) 0.027(3) 0.019(3) -0.006(3) 0.009(3) -0.023(3) C114 0.022(4) 0.037(4) 0.023(3) -0.009(3) 0.004(3) -0.014(3) C115 0.040(5) 0.069(6) 0.038(4) -0.023(4) 0.014(4) -0.040(4) C116 0.067(6) 0.073(6) 0.048(5) -0.039(5) 0.035(4) -0.057(5) C117 0.075(6) 0.042(5) 0.047(5) -0.020(4) 0.006(4) -0.032(5) C118 0.057(5) 0.027(4) 0.036(4) -0.008(3) 0.000(4) -0.015(4) C119 0.013(3) 0.029(4) 0.023(3) 0.000(3) 0.001(2) -0.010(3) C120 0.024(4) 0.038(4) 0.031(3) -0.005(3) 0.003(3) -0.018(3) C121 0.038(5) 0.057(5) 0.033(4) 0.009(4) -0.006(3) -0.036(4) C122 0.018(4) 0.058(5) 0.024(3) 0.002(3) 0.010(3) -0.016(4) C123 0.017(4) 0.043(5) 0.034(4) -0.005(3) 0.005(3) 0.000(3) C124 0.020(4) 0.031(4) 0.029(3) -0.002(3) 0.003(3) -0.008(3) P2 0.0174(8) 0.0185(8) 0.0204(7) -0.0038(6) 0.0001(6) -0.0085(7) C201 0.009(3) 0.020(3) 0.023(3) -0.008(2) 0.005(2) -0.002(2) C202 0.029(4) 0.028(3) 0.017(3) -0.009(3) 0.009(3) -0.019(3) C203 0.036(4) 0.025(3) 0.025(3) -0.004(3) 0.008(3) -0.020(3) C204 0.035(4) 0.023(3) 0.021(3) -0.010(3) -0.001(3) -0.011(3) C205 0.017(3) 0.032(4) 0.030(3) -0.013(3) 0.005(3) -0.010(3) C206 0.026(4) 0.031(4) 0.026(3) -0.005(3) 0.001(3) -0.018(3) C207 0.017(3) 0.026(3) 0.023(3) -0.012(3) 0.008(3) -0.009(3) C208 0.031(4) 0.032(4) 0.025(3) -0.007(3) 0.004(3) -0.016(3) C209 0.053(5) 0.030(4) 0.041(4) -0.015(3) 0.013(4) -0.028(4) C210 0.038(4) 0.052(5) 0.047(4) -0.031(4) 0.009(4) -0.030(4) C211 0.036(4) 0.044(5) 0.062(5) -0.017(4) -0.004(4) -0.024(4) C212 0.023(4) 0.027(4) 0.049(4) -0.012(3) 0.002(3) -0.010(3) C213 0.029(4) 0.009(3) 0.020(3) 0.000(2) 0.000(3) -0.007(3) C214 0.029(4) 0.026(4) 0.030(3) -0.004(3) 0.001(3) -0.016(3) C215 0.048(5) 0.033(4) 0.022(3) -0.014(3) 0.011(3) -0.021(4) C216 0.050(5) 0.032(4) 0.036(4) -0.013(3) 0.020(4) -0.017(4) C217 0.018(4) 0.047(5) 0.032(4) -0.008(3) 0.012(3) -0.010(3) C218 0.020(4) 0.032(4) 0.032(3) -0.002(3) 0.000(3) -0.011(3) C219 0.020(3) 0.024(3) 0.019(3) -0.005(2) 0.003(2) -0.013(3) C220 0.029(4) 0.029(4) 0.030(3) -0.007(3) 0.000(3) -0.016(3) C221 0.020(4) 0.020(3) 0.043(4) 0.005(3) -0.007(3) -0.007(3) C222 0.036(4) 0.045(5) 0.030(4) 0.001(3) -0.006(3) -0.023(4) C223 0.045(5) 0.051(5) 0.028(4) -0.008(3) -0.009(3) -0.014(4) C224 0.036(4) 0.035(4) 0.031(4) -0.009(3) -0.008(3) -0.008(3) P3 0.0209(8) 0.0191(8) 0.0154(7) -0.0036(6) 0.0021(6) -0.0103(7) C301 0.018(3) 0.025(3) 0.015(3) -0.002(2) 0.002(2) -0.012(3) C302 0.026(4) 0.026(4) 0.025(3) -0.008(3) 0.008(3) -0.015(3) C303 0.028(4) 0.022(3) 0.037(4) -0.003(3) -0.003(3) -0.012(3) C304 0.024(4) 0.023(3) 0.030(3) -0.012(3) -0.001(3) -0.007(3) C305 0.021(3) 0.029(4) 0.030(3) -0.012(3) -0.001(3) -0.008(3) C306 0.024(3) 0.025(3) 0.020(3) -0.006(3) -0.003(3) -0.009(3) C307 0.017(3) 0.020(3) 0.021(3) 0.006(2) -0.002(3) -0.005(3) C308 0.034(4) 0.027(4) 0.019(3) -0.005(3) 0.005(3) -0.015(3) C309 0.050(5) 0.036(4) 0.025(3) -0.002(3) 0.011(3) -0.017(4) C310 0.033(4) 0.035(4) 0.035(4) -0.004(3) 0.027(3) -0.012(3) C311 0.037(5) 0.043(5) 0.049(4) -0.005(4) 0.007(4) -0.025(4) C312 0.020(4) 0.043(4) 0.032(3) -0.008(3) 0.005(3) -0.019(3) C313 0.026(3) 0.020(3) 0.019(3) -0.005(2) 0.002(3) -0.013(3) C314 0.023(4) 0.023(3) 0.028(3) -0.011(3) 0.003(3) -0.007(3) C315 0.035(4) 0.037(4) 0.021(3) -0.006(3) -0.003(3) -0.009(3) C316 0.031(4) 0.034(4) 0.029(3) -0.008(3) -0.002(3) -0.016(3) C317 0.029(4) 0.020(3) 0.037(4) -0.005(3) -0.003(3) -0.012(3) C318 0.021(3) 0.031(4) 0.028(3) -0.012(3) 0.002(3) -0.010(3) C319 0.022(3) 0.017(3) 0.019(3) -0.004(2) 0.005(2) -0.010(3) C320 0.024(4) 0.025(3) 0.030(3) -0.008(3) 0.004(3) -0.010(3) C321 0.040(4) 0.020(3) 0.036(4) 0.002(3) 0.012(3) -0.019(3) C322 0.027(4) 0.027(4) 0.059(5) -0.018(3) 0.009(3) -0.016(3) C323 0.040(4) 0.041(4) 0.035(4) -0.006(3) -0.004(3) -0.030(4) C324 0.034(4) 0.026(4) 0.024(3) -0.001(3) 0.000(3) -0.017(3) N7 0.123(9) 0.124(10) 0.113(8) 0.004(7) -0.053(7) -0.086(8) C7 0.052(6) 0.094(9) 0.076(7) -0.015(6) -0.012(5) -0.036(6) C8 0.044(6) 0.097(10) 0.166(13) -0.073(10) 0.016(8) -0.024(6) O1 0.052(3) 0.035(3) 0.029(2) -0.011(2) 0.000(2) -0.015(3) O2 0.090(5) 0.086(5) 0.053(3) -0.022(3) 0.013(3) -0.066(4) O3 0.052(4) 0.058(4) 0.071(4) -0.032(3) 0.007(3) -0.022(3) _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 Re1 C1 2.114(6) . ? Re1 Se1 2.5116(7) . ? Re1 Se2 2.5229(7) . ? Re1 Se4 2.5260(7) . ? Re1 Se3 2.5294(7) . ? Re1 Re3 2.6208(4) 2_755 ? Re1 Re3 2.6286(4) . ? Re1 Re2 2.6424(4) . ? Re1 Re2 2.6466(4) 2_755 ? Re1 Re1 3.7164(5) 2_755 ? Re2 C2 2.116(6) . ? Re2 Se2 2.5082(6) 2_755 ? Re2 Se3 2.5226(6) . ? Re2 Se1 2.5227(6) 2_755 ? Re2 Se4 2.5231(6) . ? Re2 Re3 2.6405(4) . ? Re2 Re3 2.6421(5) 2_755 ? Re2 Re1 2.6466(4) 2_755 ? Re2 Re2 3.7632(6) 2_755 ? Re3 C3 2.101(6) . ? Re3 Se3 2.5227(6) . ? Re3 Se2 2.5253(7) 2_755 ? Re3 Se1 2.5266(7) . ? Re3 Se4 2.5329(6) 2_755 ? Re3 Re1 2.6208(4) 2_755 ? Re3 Re2 2.6421(5) 2_755 ? Re3 Re3 3.7073(6) 2_755 ? Se1 Re2 2.5227(6) 2_755 ? Se2 Re2 2.5082(6) 2_755 ? Se2 Re3 2.5253(7) 2_755 ? Se4 Re3 2.5329(6) 2_755 ? C1 N1 1.154(7) . ? C2 N2 1.152(7) . ? C3 N3 1.153(8) . ? Re4 C4 2.109(6) . ? Re4 Se5 2.5070(7) . ? Re4 Se8 2.5150(7) . ? Re4 Se6 2.5236(7) . ? Re4 Se7 2.5275(7) . ? Re4 Re5 2.6321(4) 2_756 ? Re4 Re5 2.6331(5) . ? Re4 Re6 2.6371(4) . ? Re4 Re6 2.6409(3) 2_756 ? Re4 Re4 3.7350(6) 2_756 ? Re5 C5 2.088(6) . ? Re5 Se8 2.5143(7) 2_756 ? Re5 Se7 2.5171(7) . ? Re5 Se5 2.5251(6) 2_756 ? Re5 Se6 2.5264(6) . ? Re5 Re6 2.6264(4) 2_756 ? Re5 Re4 2.6321(4) 2_756 ? Re5 Re6 2.6346(4) . ? Re5 Re5 3.7110(6) 2_756 ? Re6 C6 2.111(6) . ? Re6 Se8 2.5138(7) 2_756 ? Re6 Se5 2.5196(7) . ? Re6 Se6 2.5220(7) . ? Re6 Se7 2.5236(7) 2_756 ? Re6 Re5 2.6264(4) 2_756 ? Re6 Re4 2.6409(3) 2_756 ? Re6 Re6 3.7292(5) 2_756 ? Se5 Re5 2.5251(6) 2_756 ? Se7 Re6 2.5236(7) 2_756 ? Se8 Re6 2.5138(7) 2_756 ? Se8 Re5 2.5143(7) 2_756 ? C4 N4 1.161(7) . ? C5 N5 1.163(8) . ? C6 N6 1.154(8) . ? P1 C101 1.788(6) . ? P1 C107 1.792(6) . ? P1 C119 1.801(7) . ? P1 C113 1.809(6) . ? C101 C106 1.384(9) . ? C101 C102 1.396(8) . ? C102 C103 1.374(9) . ? C103 C104 1.386(10) . ? C104 C105 1.374(10) . ? C105 C106 1.362(9) . ? C107 C108 1.395(8) . ? C107 C112 1.407(9) . ? C108 C109 1.377(9) . ? C109 C110 1.350(11) . ? C110 C111 1.386(10) . ? C111 C112 1.361(9) . ? C113 C114 1.376(8) . ? C113 C118 1.381(10) . ? C114 C115 1.388(9) . ? C115 C116 1.375(12) . ? C116 C117 1.354(12) . ? C117 C118 1.400(9) . ? C119 C120 1.391(9) . ? C119 C124 1.393(9) . ? C120 C121 1.375(10) . ? C121 C122 1.364(11) . ? C122 C123 1.374(11) . ? C123 C124 1.388(10) . ? P2 C219 1.789(6) . ? P2 C207 1.795(6) . ? P2 C201 1.798(6) . ? P2 C213 1.801(6) . ? C201 C202 1.382(9) . ? C201 C206 1.392(9) . ? C202 C203 1.392(9) . ? C203 C204 1.383(9) . ? C204 C205 1.396(9) . ? C205 C206 1.384(9) . ? C207 C212 1.391(9) . ? C207 C208 1.397(9) . ? C208 C209 1.382(10) . ? C209 C210 1.390(10) . ? C210 C211 1.354(11) . ? C211 C212 1.373(10) . ? C213 C218 1.379(9) . ? C213 C214 1.390(8) . ? C214 C215 1.387(9) . ? C215 C216 1.376(11) . ? C216 C217 1.381(9) . ? C217 C218 1.394(9) . ? C219 C220 1.391(9) . ? C219 C224 1.396(8) . ? C220 C221 1.384(8) . ? C221 C222 1.400(10) . ? C222 C223 1.370(11) . ? C223 C224 1.381(9) . ? P3 C307 1.790(7) . ? P3 C301 1.796(6) . ? P3 C319 1.799(6) . ? P3 C313 1.807(6) . ? C301 C306 1.392(9) . ? C301 C302 1.395(9) . ? C302 C303 1.400(9) . ? C303 C304 1.384(10) . ? C304 C305 1.352(9) . ? C305 C306 1.387(9) . ? C307 C312 1.403(9) . ? C307 C308 1.405(8) . ? C308 C309 1.365(10) . ? C309 C310 1.372(11) . ? C310 C311 1.398(10) . ? C311 C312 1.376(10) . ? C313 C318 1.387(9) . ? C313 C314 1.391(8) . ? C314 C315 1.388(8) . ? C315 C316 1.374(10) . ? C316 C317 1.385(9) . ? C317 C318 1.385(8) . ? C319 C320 1.377(9) . ? C319 C324 1.392(6) . ? C320 C321 1.370(9) . ? C321 C322 1.400(9) . ? C322 C323 1.371(10) . ? C323 C324 1.389(7) . ? N7 C7 1.1750 . ? C7 C8 1.5353 . ? 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 C1 Re1 Se1 91.51(18) . . ? C1 Re1 Se2 90.36(15) . . ? Se1 Re1 Se2 89.36(2) . . ? C1 Re1 Se4 91.61(18) . . ? Se1 Re1 Se4 176.87(2) . . ? Se2 Re1 Se4 90.74(2) . . ? C1 Re1 Se3 93.34(15) . . ? Se1 Re1 Se3 89.91(2) . . ? Se2 Re1 Se3 176.247(19) . . ? Se4 Re1 Se3 89.79(2) . . ? C1 Re1 Re3 133.98(17) . 2_755 ? Se1 Re1 Re3 118.646(16) . 2_755 ? Se2 Re1 Re3 58.769(17) . 2_755 ? Se4 Re1 Re3 58.926(15) . 2_755 ? Se3 Re1 Re3 118.577(19) . 2_755 ? C1 Re1 Re3 136.14(17) . . ? Se1 Re1 Re3 58.831(17) . . ? Se2 Re1 Re3 118.093(16) . . ? Se4 Re1 Re3 118.502(18) . . ? Se3 Re1 Re3 58.523(15) . . ? Re3 Re1 Re3 89.859(12) 2_755 . ? C1 Re1 Re2 135.72(16) . . ? Se1 Re1 Re2 118.953(18) . . ? Se2 Re1 Re2 119.017(19) . . ? Se4 Re1 Re2 58.390(16) . . ? Se3 Re1 Re2 58.337(17) . . ? Re3 Re1 Re2 60.262(13) 2_755 . ? Re3 Re1 Re2 60.125(10) . . ? C1 Re1 Re2 133.55(16) . 2_755 ? Se1 Re1 Re2 58.489(15) . 2_755 ? Se2 Re1 Re2 57.992(16) . 2_755 ? Se4 Re1 Re2 119.088(16) . 2_755 ? Se3 Re1 Re2 118.631(18) . 2_755 ? Re3 Re1 Re2 60.169(10) 2_755 2_755 ? Re3 Re1 Re2 60.112(12) . 2_755 ? Re2 Re1 Re2 90.716(13) . 2_755 ? C1 Re1 Re1 178.49(16) . 2_755 ? Se1 Re1 Re1 88.395(16) . 2_755 ? Se2 Re1 Re1 88.134(16) . 2_755 ? Se4 Re1 Re1 88.484(16) . 2_755 ? Se3 Re1 Re1 88.166(17) . 2_755 ? Re3 Re1 Re1 45.014(8) 2_755 2_755 ? Re3 Re1 Re1 44.845(8) . 2_755 ? Re2 Re1 Re1 45.404(9) . 2_755 ? Re2 Re1 Re1 45.313(9) 2_755 2_755 ? C2 Re2 Se2 91.00(15) . 2_755 ? C2 Re2 Se3 92.24(16) . . ? Se2 Re2 Se3 89.87(2) 2_755 . ? C2 Re2 Se1 92.33(16) . 2_755 ? Se2 Re2 Se1 89.44(2) 2_755 2_755 ? Se3 Re2 Se1 175.39(2) . 2_755 ? C2 Re2 Se4 92.87(15) . . ? Se2 Re2 Se4 176.12(2) 2_755 . ? Se3 Re2 Se4 90.01(2) . . ? Se1 Re2 Se4 90.37(2) 2_755 . ? C2 Re2 Re3 134.83(17) . . ? Se2 Re2 Re3 58.675(17) 2_755 . ? Se3 Re2 Re3 58.444(16) . . ? Se1 Re2 Re3 117.498(17) 2_755 . ? Se4 Re2 Re3 118.161(19) . . ? C2 Re2 Re3 136.02(17) . 2_755 ? Se2 Re2 Re3 118.127(17) 2_755 2_755 ? Se3 Re2 Re3 118.033(18) . 2_755 ? Se1 Re2 Re3 58.521(17) 2_755 2_755 ? Se4 Re2 Re3 58.676(15) . 2_755 ? Re3 Re2 Re3 89.143(13) . 2_755 ? C2 Re2 Re1 136.05(14) . . ? Se2 Re2 Re1 118.340(19) 2_755 . ? Se3 Re2 Re1 58.590(18) . . ? Se1 Re2 Re1 117.96(2) 2_755 . ? Se4 Re2 Re1 58.496(16) . . ? Re3 Re2 Re1 59.678(10) . . ? Re3 Re2 Re1 59.464(12) 2_755 . ? C2 Re2 Re1 134.66(14) . 2_755 ? Se2 Re2 Re1 58.531(16) 2_755 2_755 ? Se3 Re2 Re1 117.864(17) . 2_755 ? Se1 Re2 Re1 58.079(16) 2_755 2_755 ? Se4 Re2 Re1 118.269(18) . 2_755 ? Re3 Re2 Re1 59.431(10) . 2_755 ? Re3 Re2 Re1 59.607(11) 2_755 2_755 ? Re1 Re2 Re1 89.284(13) . 2_755 ? C2 Re2 Re2 179.06(15) . 2_755 ? Se2 Re2 Re2 88.063(18) 2_755 2_755 ? Se3 Re2 Re2 87.865(18) . 2_755 ? Se1 Re2 Re2 87.555(18) 2_755 2_755 ? Se4 Re2 Re2 88.060(18) . 2_755 ? Re3 Re2 Re2 44.588(9) . 2_755 ? Re3 Re2 Re2 44.555(10) 2_755 2_755 ? Re1 Re2 Re2 44.686(9) . 2_755 ? Re1 Re2 Re2 44.597(9) 2_755 2_755 ? C3 Re3 Se3 92.48(15) . . ? C3 Re3 Se2 90.80(18) . 2_755 ? Se3 Re3 Se2 89.49(2) . 2_755 ? C3 Re3 Se1 93.01(18) . . ? Se3 Re3 Se1 89.72(2) . . ? Se2 Re3 Se1 176.14(2) 2_755 . ? C3 Re3 Se4 90.67(15) . 2_755 ? Se3 Re3 Se4 176.84(2) . 2_755 ? Se2 Re3 Se4 90.53(2) 2_755 2_755 ? Se1 Re3 Se4 90.06(2) . 2_755 ? C3 Re3 Re1 133.43(16) . 2_755 ? Se3 Re3 Re1 118.827(18) . 2_755 ? Se2 Re3 Re1 58.679(18) 2_755 2_755 ? Se1 Re3 Re1 118.627(19) . 2_755 ? Se4 Re3 Re1 58.668(16) 2_755 2_755 ? C3 Re3 Re1 136.43(16) . . ? Se3 Re3 Re1 58.774(17) . . ? Se2 Re3 Re1 118.229(18) 2_755 . ? Se1 Re3 Re1 58.272(16) . . ? Se4 Re3 Re1 118.583(19) 2_755 . ? Re1 Re3 Re1 90.141(12) 2_755 . ? C3 Re3 Re2 134.47(17) . . ? Se3 Re3 Re2 58.440(16) . . ? Se2 Re3 Re2 58.045(16) 2_755 . ? Se1 Re3 Re2 118.467(18) . . ? Se4 Re3 Re2 119.060(18) 2_755 . ? Re1 Re3 Re2 60.399(11) 2_755 . ? Re1 Re3 Re2 60.197(11) . . ? C3 Re3 Re2 134.64(17) . 2_755 ? Se3 Re3 Re2 119.052(18) . 2_755 ? Se2 Re3 Re2 118.939(18) 2_755 2_755 ? Se1 Re3 Re2 58.378(17) . 2_755 ? Se4 Re3 Re2 58.315(17) 2_755 2_755 ? Re1 Re3 Re2 60.275(12) 2_755 2_755 ? Re1 Re3 Re2 60.282(10) . 2_755 ? Re2 Re3 Re2 90.857(13) . 2_755 ? C3 Re3 Re3 178.58(16) . 2_755 ? Se3 Re3 Re3 88.469(18) . 2_755 ? Se2 Re3 Re3 88.160(19) 2_755 2_755 ? Se1 Re3 Re3 88.041(18) . 2_755 ? Se4 Re3 Re3 88.374(18) 2_755 2_755 ? Re1 Re3 Re3 45.156(8) 2_755 2_755 ? Re1 Re3 Re3 44.985(8) . 2_755 ? Re2 Re3 Re3 45.446(10) . 2_755 ? Re2 Re3 Re3 45.411(9) 2_755 2_755 ? Re1 Se1 Re2 63.432(17) . 2_755 ? Re1 Se1 Re3 62.897(17) . . ? Re2 Se1 Re3 63.102(18) 2_755 . ? Re2 Se2 Re1 63.476(17) 2_755 . ? Re2 Se2 Re3 63.280(16) 2_755 2_755 ? Re1 Se2 Re3 62.552(17) . 2_755 ? Re2 Se3 Re3 63.116(15) . . ? Re2 Se3 Re1 63.073(17) . . ? Re3 Se3 Re1 62.703(16) . . ? Re2 Se4 Re1 63.115(17) . . ? Re2 Se4 Re3 63.009(17) . 2_755 ? Re1 Se4 Re3 62.405(16) . 2_755 ? N1 C1 Re1 176.8(5) . . ? N2 C2 Re2 177.6(5) . . ? N3 C3 Re3 178.8(5) . . ? C4 Re4 Se5 89.52(17) . . ? C4 Re4 Se8 90.05(16) . . ? Se5 Re4 Se8 90.11(2) . . ? C4 Re4 Se6 94.03(16) . . ? Se5 Re4 Se6 89.80(2) . . ? Se8 Re4 Se6 175.91(2) . . ? C4 Re4 Se7 94.12(17) . . ? Se5 Re4 Se7 176.36(2) . . ? Se8 Re4 Se7 89.96(2) . . ? Se6 Re4 Se7 89.87(2) . . ? C4 Re4 Re5 132.21(17) . 2_756 ? Se5 Re4 Re5 58.800(16) . 2_756 ? Se8 Re4 Re5 58.431(18) . 2_756 ? Se6 Re4 Re5 118.241(19) . 2_756 ? Se7 Re4 Re5 118.339(17) . 2_756 ? C4 Re4 Re5 138.16(17) . . ? Se5 Re4 Re5 118.567(18) . . ? Se8 Re4 Re5 118.018(17) . . ? Se6 Re4 Re5 58.625(16) . . ? Se7 Re4 Re5 58.343(16) . . ? Re5 Re4 Re5 89.630(13) 2_756 . ? C4 Re4 Re6 134.94(16) . . ? Se5 Re4 Re6 58.591(18) . . ? Se8 Re4 Re6 118.212(19) . . ? Se6 Re4 Re6 58.461(17) . . ? Se7 Re4 Re6 118.321(19) . . ? Re5 Re4 Re6 59.795(11) 2_756 . ? Re5 Re4 Re6 59.986(12) . . ? C4 Re4 Re6 134.99(16) . 2_756 ? Se5 Re4 Re6 118.743(17) . 2_756 ? Se8 Re4 Re6 58.299(17) . 2_756 ? Se6 Re4 Re6 118.349(18) . 2_756 ? Se7 Re4 Re6 58.405(16) . 2_756 ? Re5 Re4 Re6 59.952(10) 2_756 2_756 ? Re5 Re4 Re6 59.735(11) . 2_756 ? Re6 Re4 Re6 89.910(12) . 2_756 ? C4 Re4 Re4 177.03(17) . 2_756 ? Se5 Re4 Re4 88.399(18) . 2_756 ? Se8 Re4 Re4 87.835(18) . 2_756 ? Se6 Re4 Re4 88.076(18) . 2_756 ? Se7 Re4 Re4 87.967(17) . 2_756 ? Re5 Re4 Re4 44.826(9) 2_756 2_756 ? Re5 Re4 Re4 44.804(10) . 2_756 ? Re6 Re4 Re4 44.996(9) . 2_756 ? Re6 Re4 Re4 44.914(8) 2_756 2_756 ? C5 Re5 Se8 92.71(18) . 2_756 ? C5 Re5 Se7 90.63(18) . . ? Se8 Re5 Se7 176.66(2) 2_756 . ? C5 Re5 Se5 90.34(15) . 2_756 ? Se8 Re5 Se5 89.71(2) 2_756 2_756 ? Se7 Re5 Se5 90.32(2) . 2_756 ? C5 Re5 Se6 93.30(15) . . ? Se8 Re5 Se6 89.71(2) 2_756 . ? Se7 Re5 Se6 90.05(2) . . ? Se5 Re5 Se6 176.34(2) 2_756 . ? C5 Re5 Re6 133.09(18) . 2_756 ? Se8 Re5 Re6 118.639(19) 2_756 2_756 ? Se7 Re5 Re6 58.719(17) . 2_756 ? Se5 Re5 Re6 58.523(18) 2_756 2_756 ? Se6 Re5 Re6 118.790(19) . 2_756 ? C5 Re5 Re4 134.27(16) . 2_756 ? Se8 Re5 Re4 58.455(17) 2_756 2_756 ? Se7 Re5 Re4 118.908(18) . 2_756 ? Se5 Re5 Re4 58.126(17) 2_756 2_756 ? Se6 Re5 Re4 118.646(18) . 2_756 ? Re6 Re5 Re4 60.198(12) 2_756 2_756 ? C5 Re5 Re4 135.31(16) . . ? Se8 Re5 Re4 118.465(19) 2_756 . ? Se7 Re5 Re4 58.729(17) . . ? Se5 Re5 Re4 118.782(18) 2_756 . ? Se6 Re5 Re4 58.521(16) . . ? Re6 Re5 Re4 60.280(11) 2_756 . ? Re4 Re5 Re4 90.370(13) 2_756 . ? C5 Re5 Re6 136.63(18) . . ? Se8 Re5 Re6 58.391(18) 2_756 . ? Se7 Re5 Re6 118.803(19) . . ? Se5 Re5 Re6 118.307(19) 2_756 . ? Se6 Re5 Re6 58.463(17) . . ? Re6 Re5 Re6 90.280(12) 2_756 . ? Re4 Re5 Re6 60.190(10) 2_756 . ? Re4 Re5 Re6 60.083(11) . . ? C5 Re5 Re5 178.24(17) . 2_756 ? Se8 Re5 Re5 88.12(2) 2_756 2_756 ? Se7 Re5 Re5 88.542(19) . 2_756 ? Se5 Re5 Re5 88.114(18) 2_756 2_756 ? Se6 Re5 Re5 88.253(18) . 2_756 ? Re6 Re5 Re5 45.229(9) 2_756 2_756 ? Re4 Re5 Re5 45.196(10) 2_756 2_756 ? Re4 Re5 Re5 45.174(9) . 2_756 ? Re6 Re5 Re5 45.051(8) . 2_756 ? C6 Re6 Se8 90.85(17) . 2_756 ? C6 Re6 Se5 93.15(17) . . ? Se8 Re6 Se5 175.99(2) 2_756 . ? C6 Re6 Se6 94.02(17) . . ? Se8 Re6 Se6 89.82(2) 2_756 . ? Se5 Re6 Se6 89.55(2) . . ? C6 Re6 Se7 89.65(17) . 2_756 ? Se8 Re6 Se7 90.08(2) 2_756 2_756 ? Se5 Re6 Se7 90.30(2) . 2_756 ? Se6 Re6 Se7 176.33(2) . 2_756 ? C6 Re6 Re5 134.30(18) . 2_756 ? Se8 Re6 Re5 118.312(18) 2_756 2_756 ? Se5 Re6 Re5 58.728(16) . 2_756 ? Se6 Re6 Re5 118.510(19) . 2_756 ? Se7 Re6 Re5 58.476(17) 2_756 2_756 ? C6 Re6 Re5 135.88(18) . . ? Se8 Re6 Re5 58.412(18) 2_756 . ? Se5 Re6 Re5 118.043(19) . . ? Se6 Re6 Re5 58.623(16) . . ? Se7 Re6 Re5 118.390(17) 2_756 . ? Re5 Re6 Re5 89.720(12) 2_756 . ? C6 Re6 Re4 137.33(16) . . ? Se8 Re6 Re4 118.33(2) 2_756 . ? Se5 Re6 Re4 58.122(18) . . ? Se6 Re6 Re4 58.518(17) . . ? Se7 Re6 Re4 118.476(18) 2_756 . ? Re5 Re6 Re4 60.007(11) 2_756 . ? Re5 Re6 Re4 59.931(12) . . ? C6 Re6 Re4 132.57(16) . 2_756 ? Se8 Re6 Re4 58.344(16) 2_756 2_756 ? Se5 Re6 Re4 118.693(18) . 2_756 ? Se6 Re6 Re4 118.475(17) . 2_756 ? Se7 Re6 Re4 58.550(15) 2_756 2_756 ? Re5 Re6 Re4 59.985(12) 2_756 2_756 ? Re5 Re6 Re4 59.858(10) . 2_756 ? Re4 Re6 Re4 90.090(12) . 2_756 ? C6 Re6 Re6 177.48(17) . 2_756 ? Se8 Re6 Re6 87.935(18) 2_756 2_756 ? Se5 Re6 Re6 88.082(18) . 2_756 ? Se6 Re6 Re6 88.185(17) . 2_756 ? Se7 Re6 Re6 88.148(17) 2_756 2_756 ? Re5 Re6 Re6 44.948(8) 2_756 2_756 ? Re5 Re6 Re6 44.772(9) . 2_756 ? Re4 Re6 Re6 45.086(8) . 2_756 ? Re4 Re6 Re6 45.004(9) 2_756 2_756 ? Re4 Se5 Re6 63.287(17) . . ? Re4 Se5 Re5 63.074(16) . 2_756 ? Re6 Se5 Re5 62.749(16) . 2_756 ? Re6 Se6 Re4 63.021(18) . . ? Re6 Se6 Re5 62.914(15) . . ? Re4 Se6 Re5 62.854(17) . . ? Re5 Se7 Re6 62.805(18) . 2_756 ? Re5 Se7 Re4 62.927(19) . . ? Re6 Se7 Re4 63.045(18) 2_756 . ? Re6 Se8 Re5 63.198(18) 2_756 2_756 ? Re6 Se8 Re4 63.357(17) 2_756 . ? Re5 Se8 Re4 63.114(17) 2_756 . ? N4 C4 Re4 177.3(5) . . ? N5 C5 Re5 177.2(6) . . ? N6 C6 Re6 177.5(6) . . ? C101 P1 C107 108.7(3) . . ? C101 P1 C119 110.2(3) . . ? C107 P1 C119 108.3(3) . . ? C101 P1 C113 110.3(3) . . ? C107 P1 C113 110.1(3) . . ? C119 P1 C113 109.3(3) . . ? C106 C101 C102 118.6(6) . . ? C106 C101 P1 120.6(5) . . ? C102 C101 P1 120.8(5) . . ? C103 C102 C101 120.2(7) . . ? C102 C103 C104 119.8(7) . . ? C105 C104 C103 120.4(6) . . ? C106 C105 C104 119.6(7) . . ? C105 C106 C101 121.5(6) . . ? C108 C107 C112 119.5(6) . . ? C108 C107 P1 119.1(5) . . ? C112 C107 P1 121.2(4) . . ? C109 C108 C107 118.6(7) . . ? C110 C109 C108 122.3(6) . . ? C109 C110 C111 119.2(6) . . ? C112 C111 C110 121.1(7) . . ? C111 C112 C107 119.3(6) . . ? C114 C113 C118 120.4(6) . . ? C114 C113 P1 120.0(5) . . ? C118 C113 P1 119.5(5) . . ? C113 C114 C115 119.8(7) . . ? C116 C115 C114 119.6(7) . . ? C117 C116 C115 120.9(7) . . ? C116 C117 C118 120.3(8) . . ? C113 C118 C117 119.0(7) . . ? C120 C119 C124 121.1(7) . . ? C120 C119 P1 118.5(5) . . ? C124 C119 P1 120.3(5) . . ? C121 C120 C119 118.2(7) . . ? C122 C121 C120 122.2(7) . . ? C121 C122 C123 118.9(7) . . ? C122 C123 C124 121.6(7) . . ? C123 C124 C119 118.0(7) . . ? C219 P2 C207 109.8(3) . . ? C219 P2 C201 109.3(3) . . ? C207 P2 C201 109.4(3) . . ? C219 P2 C213 109.4(3) . . ? C207 P2 C213 109.2(3) . . ? C201 P2 C213 109.7(3) . . ? C202 C201 C206 120.5(6) . . ? C202 C201 P2 119.3(5) . . ? C206 C201 P2 120.1(5) . . ? C201 C202 C203 120.5(6) . . ? C204 C203 C202 119.3(6) . . ? C203 C204 C205 120.2(6) . . ? C206 C205 C204 120.5(6) . . ? C205 C206 C201 119.1(6) . . ? C212 C207 C208 119.5(6) . . ? C212 C207 P2 120.5(5) . . ? C208 C207 P2 120.0(5) . . ? C209 C208 C207 119.9(6) . . ? C208 C209 C210 119.4(7) . . ? C211 C210 C209 120.4(6) . . ? C210 C211 C212 121.2(7) . . ? C211 C212 C207 119.5(7) . . ? C218 C213 C214 119.8(6) . . ? C218 C213 P2 120.3(4) . . ? C214 C213 P2 119.6(5) . . ? C215 C214 C213 119.8(6) . . ? C216 C215 C214 119.9(6) . . ? C215 C216 C217 120.9(7) . . ? C216 C217 C218 119.0(6) . . ? C213 C218 C217 120.6(6) . . ? C220 C219 C224 119.4(6) . . ? C220 C219 P2 120.4(4) . . ? C224 C219 P2 120.0(5) . . ? C221 C220 C219 120.0(6) . . ? C220 C221 C222 119.5(6) . . ? C223 C222 C221 120.8(6) . . ? C222 C223 C224 119.6(7) . . ? C223 C224 C219 120.6(7) . . ? C307 P3 C301 111.0(3) . . ? C307 P3 C319 112.1(3) . . ? C301 P3 C319 107.2(3) . . ? C307 P3 C313 106.9(3) . . ? C301 P3 C313 111.1(3) . . ? C319 P3 C313 108.5(3) . . ? C306 C301 C302 121.0(6) . . ? C306 C301 P3 117.9(5) . . ? C302 C301 P3 121.0(5) . . ? C301 C302 C303 118.3(6) . . ? C304 C303 C302 120.0(6) . . ? C305 C304 C303 120.9(6) . . ? C304 C305 C306 120.9(7) . . ? C305 C306 C301 118.8(6) . . ? C312 C307 C308 119.0(6) . . ? C312 C307 P3 118.1(5) . . ? C308 C307 P3 123.0(5) . . ? C309 C308 C307 119.0(6) . . ? C308 C309 C310 122.7(7) . . ? C309 C310 C311 118.6(7) . . ? C312 C311 C310 120.1(7) . . ? C311 C312 C307 120.5(6) . . ? C318 C313 C314 120.8(5) . . ? C318 C313 P3 117.9(4) . . ? C314 C313 P3 121.0(5) . . ? C315 C314 C313 118.7(6) . . ? C316 C315 C314 121.1(6) . . ? C315 C316 C317 119.5(6) . . ? C316 C317 C318 120.7(6) . . ? C317 C318 C313 119.1(6) . . ? C320 C319 C324 120.6(5) . . ? C320 C319 P3 121.2(4) . . ? C324 C319 P3 117.8(4) . . ? C321 C320 C319 120.2(6) . . ? C320 C321 C322 119.7(6) . . ? C323 C322 C321 120.0(6) . . ? C322 C323 C324 120.5(5) . . ? C323 C324 C319 118.9(4) . . ? N7 C7 C8 178.2 . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.88 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.985 _refine_diff_density_min -1.321 _refine_diff_density_rms 0.192 #################### Material relevant to compound 4 at 293K ############ data_rt _database_code_CSD 186999 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(PPh4)4 (Re6S8(CN)6) (CH3CN)2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H86 N8 P4 Re6 S8' _chemical_formula_weight 2969.39 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' 'P' 'P' 0.1023 0.0942 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5444(15) _cell_length_b 13.0670(14) _cell_length_c 16.8159(19) _cell_angle_alpha 109.480(13) _cell_angle_beta 95.962(14) _cell_angle_gamma 101.912(14) _cell_volume 2497.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.5370 _exptl_crystal_size_mid 0.4236 _exptl_crystal_size_min 0.0770 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 7.524 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0479 _exptl_absorpt_correction_T_max 0.5597 _exptl_absorpt_process_details 'FACEIT STOE-IPDS' _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 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, Phi. incr. == 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24655 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0814 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.94 _reflns_number_total 9056 _reflns_number_gt 6222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE, [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0105P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00037(3) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9056 _refine_ls_number_parameters 597 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0544 _refine_ls_wR_factor_gt 0.0514 _refine_ls_goodness_of_fit_ref 0.801 _refine_ls_restrained_S_all 0.801 _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 0.38186(3) 0.06378(2) 0.013788(15) 0.02306(8) Uani 1 1 d . . . Re2 Re 0.46354(3) -0.06597(2) 0.078475(15) 0.02320(8) Uani 1 1 d . . . Re3 Re 0.58957(3) 0.12475(2) 0.087891(15) 0.02286(8) Uani 1 1 d . . . S1 S 0.27546(16) -0.11701(14) 0.00385(10) 0.0300(4) Uani 1 1 d . . . S2 S 0.34188(17) 0.00392(14) -0.14030(9) 0.0297(4) Uani 1 1 d . . . S3 S 0.50809(18) 0.23455(14) 0.02196(10) 0.0319(4) Uani 1 1 d . . . S4 S 0.43959(17) 0.11189(14) 0.16553(9) 0.0310(4) Uani 1 1 d . . . C1 C 0.2459(7) 0.1429(5) 0.0278(4) 0.0339(19) Uani 1 1 d . . . C2 C 0.4233(6) -0.1419(6) 0.1718(4) 0.0303(17) Uani 1 1 d . . . C3 C 0.6926(7) 0.2728(6) 0.1906(4) 0.0351(19) Uani 1 1 d . . . N1 N 0.1800(6) 0.1857(5) 0.0367(4) 0.0459(18) Uani 1 1 d . . . N2 N 0.4090(7) -0.1763(6) 0.2208(4) 0.057(2) Uani 1 1 d . . . N3 N 0.7433(6) 0.3471(6) 0.2439(4) 0.0479(19) Uani 1 1 d . . . P1 P 0.00884(17) -0.27537(15) 0.20767(10) 0.0309(4) Uani 1 1 d . . . C4 C -0.1400(6) -0.3191(6) 0.1815(4) 0.0320(17) Uani 1 1 d . . . C5 C -0.2010(7) -0.2556(6) 0.1516(4) 0.0377(19) Uani 1 1 d . . . H5 H -0.1647 -0.1872 0.1495 0.045 Uiso 1 1 calc R . . C6 C -0.3148(7) -0.2952(7) 0.1255(5) 0.045(2) Uani 1 1 d . . . H6 H -0.3554 -0.2544 0.1048 0.054 Uiso 1 1 calc R . . C7 C -0.3678(8) -0.3969(8) 0.1306(4) 0.051(2) Uani 1 1 d . . . H7 H -0.4444 -0.4240 0.1134 0.061 Uiso 1 1 calc R . . C8 C -0.3086(7) -0.4567(7) 0.1606(5) 0.046(2) Uani 1 1 d . . . H8 H -0.3454 -0.5247 0.1631 0.056 Uiso 1 1 calc R . . C9 C -0.1951(7) -0.4191(6) 0.1874(4) 0.0355(18) Uani 1 1 d . . . H9 H -0.1561 -0.4602 0.2091 0.043 Uiso 1 1 calc R . . C10 C 0.0542(7) -0.2714(6) 0.3143(4) 0.0313(17) Uani 1 1 d . . . C11 C -0.0170(7) -0.2644(6) 0.3724(4) 0.0402(19) Uani 1 1 d . . . H11 H -0.0907 -0.2655 0.3569 0.048 Uiso 1 1 calc R . . C12 C 0.0259(8) -0.2558(6) 0.4553(4) 0.044(2) Uani 1 1 d . . . H12 H -0.0208 -0.2508 0.4951 0.053 Uiso 1 1 calc R . . C13 C 0.1319(8) -0.2542(6) 0.4795(4) 0.043(2) Uani 1 1 d . . . H13 H 0.1577 -0.2480 0.5352 0.052 Uiso 1 1 calc R . . C14 C 0.2032(8) -0.2621(8) 0.4203(5) 0.056(3) Uani 1 1 d . . . H14 H 0.2768 -0.2606 0.4363 0.067 Uiso 1 1 calc R . . C15 C 0.1628(8) -0.2721(7) 0.3375(5) 0.052(2) Uani 1 1 d . . . H15 H 0.2091 -0.2794 0.2973 0.063 Uiso 1 1 calc R . . C16 C 0.0606(7) -0.1404(6) 0.2047(4) 0.0353(19) Uani 1 1 d . . . C17 C 0.1379(8) -0.0566(7) 0.2729(5) 0.052(2) Uani 1 1 d . . . H17 H 0.1564 -0.0686 0.3234 0.062 Uiso 1 1 calc R . . C18 C 0.1862(9) 0.0422(7) 0.2659(5) 0.060(3) Uani 1 1 d . . . H18 H 0.2381 0.0967 0.3118 0.071 Uiso 1 1 calc R . . C19 C 0.1603(9) 0.0637(7) 0.1925(5) 0.056(3) Uani 1 1 d . . . H19 H 0.1937 0.1321 0.1890 0.067 Uiso 1 1 calc R . . C20 C 0.0836(8) -0.0182(7) 0.1237(5) 0.048(2) Uani 1 1 d . . . H20 H 0.0647 -0.0047 0.0738 0.058 Uiso 1 1 calc R . . C21 C 0.0365(7) -0.1175(6) 0.1295(4) 0.041(2) Uani 1 1 d . . . H21 H -0.0133 -0.1725 0.0825 0.049 Uiso 1 1 calc R . . C22 C 0.0711(7) -0.3709(6) 0.1358(4) 0.0333(18) Uani 1 1 d . . . C23 C 0.1537(7) -0.3323(7) 0.0970(4) 0.043(2) Uani 1 1 d . . . H23 H 0.1734 -0.2565 0.1047 0.051 Uiso 1 1 calc R . . C24 C 0.2078(8) -0.4043(8) 0.0467(5) 0.054(3) Uani 1 1 d . . . H24 H 0.2624 -0.3773 0.0199 0.064 Uiso 1 1 calc R . . C25 C 0.1808(8) -0.5152(8) 0.0366(4) 0.050(3) Uani 1 1 d . . . H25 H 0.2183 -0.5636 0.0041 0.060 Uiso 1 1 calc R . . C26 C 0.0999(9) -0.5546(7) 0.0736(5) 0.059(3) Uani 1 1 d . . . H26 H 0.0811 -0.6307 0.0650 0.071 Uiso 1 1 calc R . . C27 C 0.0437(8) -0.4852(6) 0.1241(5) 0.050(2) Uani 1 1 d . . . H27 H -0.0111 -0.5138 0.1499 0.060 Uiso 1 1 calc R . . P2 P 0.39904(17) 0.30839(15) 0.55747(11) 0.0310(4) Uani 1 1 d . . . C28 C 0.4789(7) 0.2418(6) 0.4831(4) 0.0337(18) Uani 1 1 d . . . C29 C 0.5569(7) 0.3082(6) 0.4556(4) 0.041(2) Uani 1 1 d . . . H29 H 0.5704 0.3860 0.4784 0.049 Uiso 1 1 calc R . . C30 C 0.6137(8) 0.2583(8) 0.3946(5) 0.051(2) Uani 1 1 d . . . H30 H 0.6656 0.3027 0.3760 0.061 Uiso 1 1 calc R . . C31 C 0.5949(8) 0.1453(8) 0.3612(5) 0.053(3) Uani 1 1 d . . . H31 H 0.6328 0.1123 0.3191 0.063 Uiso 1 1 calc R . . C32 C 0.5203(9) 0.0796(8) 0.3892(5) 0.060(3) Uani 1 1 d . . . H32 H 0.5100 0.0021 0.3672 0.072 Uiso 1 1 calc R . . C33 C 0.4602(7) 0.1254(6) 0.4490(5) 0.048(2) Uani 1 1 d . . . H33 H 0.4081 0.0797 0.4664 0.057 Uiso 1 1 calc R . . C34 C 0.3088(7) 0.1997(6) 0.5821(4) 0.0373(19) Uani 1 1 d . . . C35 C 0.3315(8) 0.1788(6) 0.6561(4) 0.049(2) Uani 1 1 d . . . H35 H 0.3929 0.2241 0.6982 0.059 Uiso 1 1 calc R . . C36 C 0.2613(10) 0.0889(8) 0.6673(6) 0.062(3) Uani 1 1 d . . . H36 H 0.2750 0.0749 0.7175 0.075 Uiso 1 1 calc R . . C37 C 0.1722(9) 0.0214(7) 0.6042(6) 0.060(3) Uani 1 1 d . . . H37 H 0.1262 -0.0388 0.6119 0.072 Uiso 1 1 calc R . . C38 C 0.1497(8) 0.0415(7) 0.5294(6) 0.058(3) Uani 1 1 d . . . H38 H 0.0894 -0.0053 0.4868 0.070 Uiso 1 1 calc R . . C39 C 0.2167(7) 0.1309(6) 0.5183(4) 0.045(2) Uani 1 1 d . . . H39 H 0.2011 0.1457 0.4685 0.054 Uiso 1 1 calc R . . C40 C 0.4926(6) 0.4081(6) 0.6517(4) 0.0325(17) Uani 1 1 d . . . C41 C 0.4846(7) 0.5186(5) 0.6882(4) 0.0387(19) Uani 1 1 d . . . H41 H 0.4315 0.5440 0.6627 0.046 Uiso 1 1 calc R . . C42 C 0.5574(8) 0.5895(6) 0.7634(5) 0.053(3) Uani 1 1 d . . . H42 H 0.5546 0.6640 0.7868 0.064 Uiso 1 1 calc R . . C43 C 0.6328(8) 0.5534(7) 0.8038(5) 0.051(2) Uani 1 1 d . . . H43 H 0.6789 0.6020 0.8553 0.062 Uiso 1 1 calc R . . C44 C 0.6406(8) 0.4445(7) 0.7682(5) 0.054(3) Uani 1 1 d . . . H44 H 0.6934 0.4201 0.7950 0.065 Uiso 1 1 calc R . . C45 C 0.5711(7) 0.3722(6) 0.6936(4) 0.042(2) Uani 1 1 d . . . H45 H 0.5761 0.2984 0.6706 0.050 Uiso 1 1 calc R . . C46 C 0.3137(6) 0.3723(6) 0.5086(4) 0.0356(18) Uani 1 1 d . . . C47 C 0.3073(7) 0.3633(7) 0.4238(5) 0.047(2) Uani 1 1 d . . . H47 H 0.3531 0.3265 0.3912 0.056 Uiso 1 1 calc R . . C48 C 0.2346(9) 0.4075(8) 0.3866(6) 0.066(3) Uani 1 1 d . . . H48 H 0.2307 0.3988 0.3291 0.079 Uiso 1 1 calc R . . C49 C 0.1695(9) 0.4628(8) 0.4327(8) 0.075(3) Uani 1 1 d . . . H49 H 0.1219 0.4936 0.4072 0.090 Uiso 1 1 calc R . . C50 C 0.1721(9) 0.4750(8) 0.5193(7) 0.062(3) Uani 1 1 d . . . H50 H 0.1264 0.5128 0.5512 0.074 Uiso 1 1 calc R . . C51 C 0.2444(7) 0.4294(7) 0.5556(5) 0.044(2) Uani 1 1 d . . . H51 H 0.2471 0.4368 0.6128 0.053 Uiso 1 1 calc R . . N4 N 0.9643(12) 0.1923(12) 0.3294(7) 0.143(6) Uani 1 1 d . . . C52 C 0.9591(10) 0.1965(11) 0.2649(7) 0.089(4) Uani 1 1 d . . . C53 C 0.9542(11) 0.2092(13) 0.1803(7) 0.108(5) Uani 1 1 d . . . H53A H 0.9896 0.2853 0.1883 0.161 Uiso 1 1 calc R . . H53B H 0.8782 0.1908 0.1528 0.161 Uiso 1 1 calc R . . H53C H 0.9917 0.1595 0.1450 0.161 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 Re1 0.02641(18) 0.02226(14) 0.02366(12) 0.01103(11) 0.00367(11) 0.00903(12) Re2 0.02839(18) 0.02189(14) 0.02252(12) 0.01189(11) 0.00369(11) 0.00740(12) Re3 0.02672(18) 0.02058(14) 0.02226(12) 0.00957(11) 0.00220(11) 0.00644(12) S1 0.0311(12) 0.0293(9) 0.0315(8) 0.0140(7) 0.0064(8) 0.0068(8) S2 0.0364(12) 0.0288(9) 0.0262(8) 0.0131(7) -0.0002(7) 0.0109(8) S3 0.0440(13) 0.0237(9) 0.0327(8) 0.0148(7) 0.0044(8) 0.0119(8) S4 0.0420(13) 0.0297(9) 0.0245(8) 0.0112(7) 0.0073(8) 0.0130(9) C1 0.056(6) 0.014(3) 0.026(3) 0.007(3) 0.003(3) 0.000(4) C2 0.027(4) 0.031(4) 0.033(3) 0.011(3) 0.002(3) 0.008(3) C3 0.053(6) 0.034(4) 0.035(4) 0.023(3) 0.014(4) 0.027(4) N1 0.049(5) 0.044(4) 0.054(4) 0.027(3) 0.011(3) 0.017(4) N2 0.071(6) 0.042(4) 0.051(4) 0.022(4) -0.001(4) -0.002(4) N3 0.052(5) 0.044(4) 0.039(3) 0.012(3) 0.000(3) 0.005(4) P1 0.0299(12) 0.0332(10) 0.0308(8) 0.0139(8) 0.0037(8) 0.0082(9) C4 0.034(5) 0.033(4) 0.037(3) 0.020(3) 0.008(3) 0.012(3) C5 0.039(5) 0.043(4) 0.042(4) 0.026(4) 0.008(4) 0.015(4) C6 0.038(6) 0.052(5) 0.056(4) 0.027(4) 0.013(4) 0.023(4) C7 0.037(6) 0.074(6) 0.034(4) 0.015(4) 0.003(4) 0.009(5) C8 0.034(5) 0.046(5) 0.055(4) 0.017(4) 0.008(4) 0.005(4) C9 0.040(5) 0.035(4) 0.040(4) 0.024(3) 0.009(3) 0.011(4) C10 0.036(5) 0.034(4) 0.029(3) 0.015(3) 0.007(3) 0.014(3) C11 0.033(5) 0.047(5) 0.038(4) 0.018(4) -0.003(3) 0.004(4) C12 0.054(6) 0.044(4) 0.034(4) 0.014(3) 0.015(4) 0.010(4) C13 0.059(7) 0.050(5) 0.034(4) 0.027(4) 0.003(4) 0.025(5) C14 0.054(7) 0.080(6) 0.042(4) 0.028(4) -0.002(4) 0.033(5) C15 0.048(6) 0.073(6) 0.043(4) 0.024(4) 0.009(4) 0.025(5) C16 0.043(5) 0.029(4) 0.033(3) 0.011(3) 0.006(3) 0.007(4) C17 0.071(7) 0.047(5) 0.042(4) 0.027(4) 0.004(4) 0.012(5) C18 0.077(8) 0.040(5) 0.053(5) 0.022(4) 0.000(5) -0.005(5) C19 0.076(8) 0.045(5) 0.058(5) 0.030(4) 0.028(5) 0.014(5) C20 0.063(7) 0.044(5) 0.042(4) 0.024(4) 0.012(4) 0.010(5) C21 0.042(5) 0.040(4) 0.041(4) 0.018(4) 0.004(4) 0.006(4) C22 0.036(5) 0.037(4) 0.025(3) 0.010(3) 0.001(3) 0.010(4) C23 0.039(5) 0.046(5) 0.046(4) 0.017(4) 0.013(4) 0.013(4) C24 0.048(6) 0.071(6) 0.040(4) 0.010(4) 0.017(4) 0.024(5) C25 0.050(6) 0.064(6) 0.025(3) -0.005(4) 0.003(4) 0.027(5) C26 0.068(8) 0.039(5) 0.050(5) -0.003(4) -0.010(5) 0.012(5) C27 0.045(6) 0.040(4) 0.057(5) 0.010(4) 0.009(4) 0.008(4) P2 0.0330(12) 0.0272(9) 0.0320(8) 0.0113(8) 0.0048(8) 0.0060(9) C28 0.032(5) 0.039(4) 0.031(3) 0.016(3) 0.004(3) 0.008(4) C29 0.046(6) 0.036(4) 0.042(4) 0.015(4) 0.010(4) 0.011(4) C30 0.053(6) 0.071(6) 0.047(4) 0.037(4) 0.011(4) 0.026(5) C31 0.067(7) 0.063(6) 0.036(4) 0.012(4) 0.019(4) 0.041(5) C32 0.066(7) 0.047(5) 0.048(4) -0.001(4) 0.005(5) 0.006(5) C33 0.047(6) 0.035(4) 0.043(4) -0.002(4) 0.006(4) 0.001(4) C34 0.041(5) 0.033(4) 0.038(4) 0.011(3) 0.016(4) 0.010(4) C35 0.077(7) 0.037(4) 0.032(4) 0.011(4) 0.009(4) 0.017(5) C36 0.098(9) 0.052(5) 0.062(5) 0.042(5) 0.036(6) 0.026(6) C37 0.071(8) 0.039(5) 0.074(6) 0.025(5) 0.039(6) -0.001(5) C38 0.037(6) 0.043(5) 0.081(6) 0.020(5) 0.004(5) -0.008(4) C39 0.044(6) 0.045(5) 0.034(4) 0.010(4) -0.001(4) -0.001(4) C40 0.029(5) 0.032(4) 0.035(3) 0.011(3) 0.008(3) 0.006(3) C41 0.043(5) 0.025(4) 0.047(4) 0.012(3) 0.005(4) 0.009(4) C42 0.074(8) 0.030(4) 0.047(4) 0.003(4) 0.012(5) 0.013(4) C43 0.053(6) 0.046(5) 0.038(4) 0.004(4) -0.003(4) 0.001(4) C44 0.045(6) 0.060(5) 0.046(4) 0.007(4) -0.011(4) 0.021(5) C45 0.046(6) 0.033(4) 0.040(4) 0.006(3) 0.002(4) 0.012(4) C46 0.024(5) 0.036(4) 0.046(4) 0.020(3) 0.001(3) 0.000(3) C47 0.041(6) 0.042(4) 0.056(5) 0.026(4) -0.006(4) 0.002(4) C48 0.064(8) 0.057(6) 0.079(6) 0.047(5) -0.021(5) -0.001(5) C49 0.047(7) 0.061(6) 0.131(9) 0.056(7) -0.006(6) 0.019(5) C50 0.048(7) 0.055(5) 0.099(7) 0.044(6) 0.018(5) 0.019(5) C51 0.031(5) 0.056(5) 0.054(4) 0.026(4) 0.011(4) 0.014(4) N4 0.172(15) 0.170(12) 0.074(6) 0.052(8) 0.033(8) -0.001(10) C52 0.066(9) 0.119(10) 0.077(7) 0.037(7) 0.015(6) 0.012(7) C53 0.084(11) 0.180(14) 0.107(9) 0.084(9) 0.034(8) 0.076(10) _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 Re1 C1 2.164(9) . ? Re1 S1 2.4040(19) . ? Re1 S4 2.4060(17) . ? Re1 S2 2.4070(16) . ? Re1 S3 2.408(2) . ? Re1 Re3 2.6045(6) . ? Re1 Re2 2.6079(5) 2_655 ? Re1 Re3 2.6083(5) 2_655 ? Re1 Re2 2.6121(5) . ? Re1 Re1 3.6863(7) 2_655 ? Re2 C2 2.167(8) . ? Re2 S4 2.3968(16) . ? Re2 S1 2.401(2) . ? Re2 S2 2.406(2) 2_655 ? Re2 S3 2.4081(15) 2_655 ? Re2 Re3 2.6064(6) . ? Re2 Re1 2.6079(5) 2_655 ? Re2 Re3 2.6132(5) 2_655 ? Re2 Re2 3.6959(7) 2_655 ? Re3 C3 2.161(8) . ? Re3 S3 2.4006(19) . ? Re3 S1 2.4013(18) 2_655 ? Re3 S2 2.4022(18) 2_655 ? Re3 S4 2.4081(19) . ? Re3 Re1 2.6083(5) 2_655 ? Re3 Re2 2.6132(5) 2_655 ? Re3 Re3 3.6857(10) 2_655 ? S1 Re3 2.4013(18) 2_655 ? S2 Re3 2.4022(18) 2_655 ? S2 Re2 2.406(2) 2_655 ? S3 Re2 2.4081(15) 2_655 ? C1 N1 1.086(9) . ? C2 N2 1.077(9) . ? C3 N3 1.094(9) . ? P1 C16 1.769(8) . ? P1 C22 1.795(6) . ? P1 C4 1.797(8) . ? P1 C10 1.805(7) . ? C4 C9 1.386(10) . ? C4 C5 1.409(10) . ? C5 C6 1.383(11) . ? C6 C7 1.392(12) . ? C7 C8 1.357(11) . ? C8 C9 1.378(11) . ? C10 C15 1.381(11) . ? C10 C11 1.384(10) . ? C11 C12 1.400(10) . ? C12 C13 1.344(11) . ? C13 C14 1.398(11) . ? C14 C15 1.383(11) . ? C16 C17 1.395(11) . ? C16 C21 1.411(10) . ? C17 C18 1.357(12) . ? C18 C19 1.376(12) . ? C19 C20 1.388(12) . ? C20 C21 1.350(11) . ? C22 C23 1.378(11) . ? C22 C27 1.402(11) . ? C23 C24 1.384(9) . ? C24 C25 1.366(13) . ? C25 C26 1.346(13) . ? C26 C27 1.383(11) . ? P2 C46 1.779(8) . ? P2 C40 1.787(7) . ? P2 C28 1.794(7) . ? P2 C34 1.815(8) . ? C28 C29 1.391(11) . ? C28 C33 1.393(10) . ? C29 C30 1.372(10) . ? C30 C31 1.352(12) . ? C31 C32 1.366(13) . ? C32 C33 1.371(11) . ? C34 C35 1.375(10) . ? C34 C39 1.402(11) . ? C35 C36 1.395(12) . ? C36 C37 1.369(14) . ? C37 C38 1.381(13) . ? C38 C39 1.370(12) . ? C40 C41 1.397(9) . ? C40 C45 1.399(10) . ? C41 C42 1.385(11) . ? C42 C43 1.358(12) . ? C43 C44 1.376(11) . ? C44 C45 1.367(10) . ? C46 C47 1.382(11) . ? C46 C51 1.399(10) . ? C47 C48 1.378(12) . ? C48 C49 1.339(13) . ? C49 C50 1.407(14) . ? C50 C51 1.378(12) . ? N4 C52 1.099(14) . ? C52 C53 1.484(16) . ? 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 C1 Re1 S1 95.60(19) . . ? C1 Re1 S4 94.56(17) . . ? S1 Re1 S4 89.40(6) . . ? C1 Re1 S2 92.45(17) . . ? S1 Re1 S2 89.63(6) . . ? S4 Re1 S2 172.99(6) . . ? C1 Re1 S3 91.64(19) . . ? S1 Re1 S3 172.75(6) . . ? S4 Re1 S3 89.97(7) . . ? S2 Re1 S3 90.12(6) . . ? C1 Re1 Re3 134.32(17) . . ? S1 Re1 Re3 116.91(5) . . ? S4 Re1 Re3 57.29(5) . . ? S2 Re1 Re3 117.31(5) . . ? S3 Re1 Re3 57.07(5) . . ? C1 Re1 Re2 132.82(19) . 2_655 ? S1 Re1 Re2 116.99(4) . 2_655 ? S4 Re1 Re2 117.41(5) . 2_655 ? S2 Re1 Re2 57.18(5) . 2_655 ? S3 Re1 Re2 57.22(4) . 2_655 ? Re3 Re1 Re2 60.178(14) . 2_655 ? C1 Re1 Re3 135.61(17) . 2_655 ? S1 Re1 Re3 57.07(4) . 2_655 ? S4 Re1 Re3 116.93(5) . 2_655 ? S2 Re1 Re3 57.07(4) . 2_655 ? S3 Re1 Re3 117.12(4) . 2_655 ? Re3 Re1 Re3 89.99(2) . 2_655 ? Re2 Re1 Re3 59.957(16) 2_655 2_655 ? C1 Re1 Re2 137.03(19) . . ? S1 Re1 Re2 57.00(5) . . ? S4 Re1 Re2 56.88(4) . . ? S2 Re1 Re2 117.11(4) . . ? S3 Re1 Re2 116.99(5) . . ? Re3 Re1 Re2 59.952(16) . . ? Re2 Re1 Re2 90.149(16) 2_655 . ? Re3 Re1 Re2 60.075(14) 2_655 . ? C1 Re1 Re1 177.85(19) . 2_655 ? S1 Re1 Re1 86.28(5) . 2_655 ? S4 Re1 Re1 86.48(5) . 2_655 ? S2 Re1 Re1 86.53(5) . 2_655 ? S3 Re1 Re1 86.47(5) . 2_655 ? Re3 Re1 Re1 45.038(12) . 2_655 ? Re2 Re1 Re1 45.121(11) 2_655 2_655 ? Re3 Re1 Re1 44.953(16) 2_655 2_655 ? Re2 Re1 Re1 45.028(12) . 2_655 ? C2 Re2 S4 93.12(17) . . ? C2 Re2 S1 94.6(2) . . ? S4 Re2 S1 89.70(7) . . ? C2 Re2 S2 92.7(2) . 2_655 ? S4 Re2 S2 89.88(7) . 2_655 ? S1 Re2 S2 172.72(6) . 2_655 ? C2 Re2 S3 93.89(17) . 2_655 ? S4 Re2 S3 172.99(6) . 2_655 ? S1 Re2 S3 89.40(6) . 2_655 ? S2 Re2 S3 90.13(7) 2_655 2_655 ? C2 Re2 Re3 134.21(17) . . ? S4 Re2 Re3 57.36(5) . . ? S1 Re2 Re3 116.96(5) . . ? S2 Re2 Re3 57.10(5) 2_655 . ? S3 Re2 Re3 117.18(5) 2_655 . ? C2 Re2 Re1 134.57(18) . 2_655 ? S4 Re2 Re1 117.34(5) . 2_655 ? S1 Re2 Re1 116.85(4) . 2_655 ? S2 Re2 Re1 57.20(4) 2_655 2_655 ? S3 Re2 Re1 57.20(5) 2_655 2_655 ? Re3 Re2 Re1 60.030(16) . 2_655 ? C2 Re2 Re1 135.57(18) . . ? S4 Re2 Re1 57.22(4) . . ? S1 Re2 Re1 57.13(5) . . ? S2 Re2 Re1 116.94(5) 2_655 . ? S3 Re2 Re1 116.80(5) 2_655 . ? Re3 Re2 Re1 59.878(15) . . ? Re1 Re2 Re1 89.851(16) 2_655 . ? C2 Re2 Re3 135.95(17) . 2_655 ? S4 Re2 Re3 117.08(5) . 2_655 ? S1 Re2 Re3 57.04(4) . 2_655 ? S2 Re2 Re3 117.00(4) 2_655 2_655 ? S3 Re2 Re3 56.94(5) 2_655 2_655 ? Re3 Re2 Re3 89.84(2) . 2_655 ? Re1 Re2 Re3 59.846(16) 2_655 2_655 ? Re1 Re2 Re3 59.891(14) . 2_655 ? C2 Re2 Re2 179.08(19) . 2_655 ? S4 Re2 Re2 86.65(5) . 2_655 ? S1 Re2 Re2 86.28(5) . 2_655 ? S2 Re2 Re2 86.44(5) 2_655 2_655 ? S3 Re2 Re2 86.36(5) 2_655 2_655 ? Re3 Re2 Re2 44.995(13) . 2_655 ? Re1 Re2 Re2 44.971(12) 2_655 2_655 ? Re1 Re2 Re2 44.880(11) . 2_655 ? Re3 Re2 Re2 44.847(13) 2_655 2_655 ? C3 Re3 S3 92.35(19) . . ? C3 Re3 S1 94.0(2) . 2_655 ? S3 Re3 S1 89.56(7) . 2_655 ? C3 Re3 S2 94.28(19) . 2_655 ? S3 Re3 S2 173.36(6) . 2_655 ? S1 Re3 S2 89.81(6) 2_655 2_655 ? C3 Re3 S4 93.2(2) . . ? S3 Re3 S4 90.09(7) . . ? S1 Re3 S4 172.79(6) 2_655 . ? S2 Re3 S4 89.71(6) 2_655 . ? C3 Re3 Re1 134.00(19) . . ? S3 Re3 Re1 57.33(5) . . ? S1 Re3 Re1 116.95(5) 2_655 . ? S2 Re3 Re1 117.38(5) 2_655 . ? S4 Re3 Re1 57.21(5) . . ? C3 Re3 Re2 135.25(19) . . ? S3 Re3 Re2 117.47(5) . . ? S1 Re3 Re2 117.15(5) 2_655 . ? S2 Re3 Re2 57.25(5) 2_655 . ? S4 Re3 Re2 56.94(4) . . ? Re1 Re3 Re2 60.169(16) . . ? C3 Re3 Re1 135.99(19) . 2_655 ? S3 Re3 Re1 117.22(4) . 2_655 ? S1 Re3 Re1 57.17(4) 2_655 2_655 ? S2 Re3 Re1 57.24(4) 2_655 2_655 ? S4 Re3 Re1 116.91(5) . 2_655 ? Re1 Re3 Re1 90.01(2) . 2_655 ? Re2 Re3 Re1 60.013(14) . 2_655 ? C3 Re3 Re2 134.58(19) . 2_655 ? S3 Re3 Re2 57.22(4) . 2_655 ? S1 Re3 Re2 57.02(5) 2_655 2_655 ? S2 Re3 Re2 117.24(4) 2_655 2_655 ? S4 Re3 Re2 117.14(5) . 2_655 ? Re1 Re3 Re2 59.976(17) . 2_655 ? Re2 Re3 Re2 90.16(2) . 2_655 ? Re1 Re3 Re2 60.034(15) 2_655 2_655 ? C3 Re3 Re3 178.97(19) . 2_655 ? S3 Re3 Re3 86.69(5) . 2_655 ? S1 Re3 Re3 86.37(4) 2_655 2_655 ? S2 Re3 Re3 86.68(4) 2_655 2_655 ? S4 Re3 Re3 86.42(4) . 2_655 ? Re1 Re3 Re3 45.047(15) . 2_655 ? Re2 Re3 Re3 45.153(13) . 2_655 ? Re1 Re3 Re3 44.962(13) 2_655 2_655 ? Re2 Re3 Re3 45.004(13) 2_655 2_655 ? Re2 S1 Re3 65.94(5) . 2_655 ? Re2 S1 Re1 65.87(5) . . ? Re3 S1 Re1 65.75(5) 2_655 . ? Re3 S2 Re2 65.65(5) 2_655 2_655 ? Re3 S2 Re1 65.69(5) 2_655 . ? Re2 S2 Re1 65.62(5) 2_655 . ? Re3 S3 Re1 65.59(5) . . ? Re3 S3 Re2 65.84(5) . 2_655 ? Re1 S3 Re2 65.58(5) . 2_655 ? Re2 S4 Re1 65.89(4) . . ? Re2 S4 Re3 65.70(4) . . ? Re1 S4 Re3 65.50(4) . . ? N1 C1 Re1 177.7(7) . . ? N2 C2 Re2 176.0(7) . . ? N3 C3 Re3 178.3(7) . . ? C16 P1 C22 107.9(4) . . ? C16 P1 C4 111.6(4) . . ? C22 P1 C4 112.1(3) . . ? C16 P1 C10 108.6(3) . . ? C22 P1 C10 107.2(3) . . ? C4 P1 C10 109.3(3) . . ? C9 C4 C5 119.7(8) . . ? C9 C4 P1 119.4(6) . . ? C5 C4 P1 120.8(6) . . ? C6 C5 C4 119.9(8) . . ? C5 C6 C7 119.2(8) . . ? C8 C7 C6 120.4(9) . . ? C7 C8 C9 121.6(9) . . ? C8 C9 C4 119.1(8) . . ? C15 C10 C11 120.7(7) . . ? C15 C10 P1 118.4(5) . . ? C11 C10 P1 120.9(6) . . ? C10 C11 C12 117.6(8) . . ? C13 C12 C11 122.6(7) . . ? C12 C13 C14 119.5(7) . . ? C15 C14 C13 119.2(9) . . ? C10 C15 C14 120.4(8) . . ? C17 C16 C21 117.1(7) . . ? C17 C16 P1 121.1(6) . . ? C21 C16 P1 121.3(5) . . ? C18 C17 C16 120.5(8) . . ? C17 C18 C19 121.6(9) . . ? C18 C19 C20 119.1(8) . . ? C21 C20 C19 119.7(8) . . ? C20 C21 C16 122.0(7) . . ? C23 C22 C27 118.5(7) . . ? C23 C22 P1 120.8(6) . . ? C27 C22 P1 120.4(6) . . ? C22 C23 C24 121.1(8) . . ? C25 C24 C23 119.7(8) . . ? C26 C25 C24 120.0(7) . . ? C25 C26 C27 122.0(9) . . ? C26 C27 C22 118.8(8) . . ? C46 P2 C40 112.0(3) . . ? C46 P2 C28 109.8(3) . . ? C40 P2 C28 108.3(3) . . ? C46 P2 C34 107.8(4) . . ? C40 P2 C34 111.1(3) . . ? C28 P2 C34 107.6(3) . . ? C29 C28 C33 119.5(6) . . ? C29 C28 P2 118.8(5) . . ? C33 C28 P2 121.6(6) . . ? C30 C29 C28 119.7(7) . . ? C31 C30 C29 120.6(9) . . ? C30 C31 C32 120.1(7) . . ? C31 C32 C33 121.4(8) . . ? C32 C33 C28 118.6(8) . . ? C35 C34 C39 120.4(8) . . ? C35 C34 P2 123.0(7) . . ? C39 C34 P2 116.4(6) . . ? C34 C35 C36 119.2(9) . . ? C37 C36 C35 120.0(8) . . ? C36 C37 C38 120.9(8) . . ? C39 C38 C37 119.7(9) . . ? C38 C39 C34 119.7(8) . . ? C41 C40 C45 118.9(6) . . ? C41 C40 P2 122.1(6) . . ? C45 C40 P2 118.8(5) . . ? C42 C41 C40 118.6(8) . . ? C43 C42 C41 121.9(7) . . ? C42 C43 C44 119.7(7) . . ? C45 C44 C43 120.3(8) . . ? C44 C45 C40 120.6(7) . . ? C47 C46 C51 117.4(8) . . ? C47 C46 P2 123.2(6) . . ? C51 C46 P2 119.3(6) . . ? C48 C47 C46 121.5(8) . . ? C49 C48 C47 120.4(9) . . ? C48 C49 C50 120.9(10) . . ? C51 C50 C49 118.2(8) . . ? C50 C51 C46 121.6(8) . . ? N4 C52 C53 176.7(17) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.469 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.135 #################### Material relevant to compound 4 at 250K ############ data_s8250k _database_code_CSD 187000 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(PPh4)4 (Re6S8(CN)6) (CH3CN)2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H86 N8 P4 Re6 S8' _chemical_formula_weight 2969.39 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' 'P' 'P' 0.1023 0.0942 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4955(17) _cell_length_b 13.0836(17) _cell_length_c 16.758(2) _cell_angle_alpha 109.432(15) _cell_angle_beta 95.958(16) _cell_angle_gamma 101.837(16) _cell_volume 2484.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.5390 _exptl_crystal_size_mid 0.4236 _exptl_crystal_size_min 0.0770 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.985 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 7.564 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0465 _exptl_absorpt_correction_T_max 0.5627 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(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 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, Phi. incr. == 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25526 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.93 _reflns_number_total 9004 _reflns_number_gt 6379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE, [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0099P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00026(3) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9004 _refine_ls_number_parameters 597 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0503 _refine_ls_goodness_of_fit_ref 0.850 _refine_ls_restrained_S_all 0.850 _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 0.38170(2) 0.06421(2) 0.014204(15) 0.01927(8) Uani 1 1 d . . . Re2 Re 0.46352(2) -0.06593(2) 0.078695(15) 0.01933(7) Uani 1 1 d . . . Re3 Re 0.59021(2) 0.12472(2) 0.087894(15) 0.01909(7) Uani 1 1 d . . . S1 S 0.27465(15) -0.11652(13) 0.00458(10) 0.0261(4) Uani 1 1 d . . . S2 S 0.34081(16) 0.00409(14) -0.13995(10) 0.0257(4) Uani 1 1 d . . . S3 S 0.50854(16) 0.23476(13) 0.02190(10) 0.0273(4) Uani 1 1 d . . . S4 S 0.43988(16) 0.11214(13) 0.16619(9) 0.0257(4) Uani 1 1 d . . . C1 C 0.2445(6) 0.1449(5) 0.0295(4) 0.0229(15) Uani 1 1 d . . . C2 C 0.4254(6) -0.1396(5) 0.1722(4) 0.0230(15) Uani 1 1 d . . . C3 C 0.6940(7) 0.2731(6) 0.1916(4) 0.0311(17) Uani 1 1 d . . . N1 N 0.1792(6) 0.1866(5) 0.0378(4) 0.0390(16) Uani 1 1 d . . . N2 N 0.4075(6) -0.1747(5) 0.2207(4) 0.0459(19) Uani 1 1 d . . . N3 N 0.7450(6) 0.3486(5) 0.2439(4) 0.0414(17) Uani 1 1 d . . . P1 P 0.00862(16) -0.27429(14) 0.20804(10) 0.0246(4) Uani 1 1 d . . . C4 C -0.1407(6) -0.3187(5) 0.1815(4) 0.0241(16) Uani 1 1 d . . . C5 C -0.2020(6) -0.2556(6) 0.1524(4) 0.0308(17) Uani 1 1 d . . . H5 H -0.1661 -0.1864 0.1516 0.037 Uiso 1 1 calc R . . C6 C -0.3163(6) -0.2961(6) 0.1247(4) 0.0343(18) Uani 1 1 d . . . H6 H -0.3568 -0.2561 0.1026 0.041 Uiso 1 1 calc R . . C7 C -0.3691(7) -0.3960(7) 0.1303(5) 0.041(2) Uani 1 1 d . . . H7 H -0.4459 -0.4226 0.1126 0.050 Uiso 1 1 calc R . . C8 C -0.3108(7) -0.4574(6) 0.1615(4) 0.039(2) Uani 1 1 d . . . H8 H -0.3479 -0.5247 0.1651 0.047 Uiso 1 1 calc R . . C9 C -0.1972(6) -0.4184(6) 0.1874(4) 0.0316(17) Uani 1 1 d . . . H9 H -0.1577 -0.4593 0.2092 0.038 Uiso 1 1 calc R . . C10 C 0.0532(6) -0.2717(5) 0.3138(4) 0.0257(16) Uani 1 1 d . . . C11 C -0.0162(7) -0.2627(6) 0.3739(4) 0.0339(18) Uani 1 1 d . . . H11 H -0.0895 -0.2610 0.3591 0.041 Uiso 1 1 calc R . . C12 C 0.0238(7) -0.2563(6) 0.4557(4) 0.0368(19) Uani 1 1 d . . . H12 H -0.0237 -0.2528 0.4952 0.044 Uiso 1 1 calc R . . C13 C 0.1314(7) -0.2551(6) 0.4795(4) 0.040(2) Uani 1 1 d . . . H13 H 0.1568 -0.2500 0.5352 0.048 Uiso 1 1 calc R . . C14 C 0.2031(7) -0.2611(8) 0.4222(5) 0.051(2) Uani 1 1 d . . . H14 H 0.2771 -0.2587 0.4393 0.061 Uiso 1 1 calc R . . C15 C 0.1637(7) -0.2710(7) 0.3376(4) 0.044(2) Uani 1 1 d . . . H15 H 0.2109 -0.2770 0.2978 0.053 Uiso 1 1 calc R . . C16 C 0.0619(6) -0.1371(6) 0.2053(4) 0.0277(16) Uani 1 1 d . . . C17 C 0.1394(7) -0.0556(6) 0.2741(4) 0.039(2) Uani 1 1 d . . . H17 H 0.1579 -0.0690 0.3243 0.047 Uiso 1 1 calc R . . C18 C 0.1892(8) 0.0459(7) 0.2679(5) 0.051(2) Uani 1 1 d . . . H18 H 0.2412 0.1005 0.3138 0.061 Uiso 1 1 calc R . . C19 C 0.1616(8) 0.0654(7) 0.1942(5) 0.049(2) Uani 1 1 d . . . H19 H 0.1947 0.1337 0.1903 0.059 Uiso 1 1 calc R . . C20 C 0.0847(7) -0.0156(6) 0.1251(5) 0.0371(19) Uani 1 1 d . . . H20 H 0.0663 -0.0011 0.0754 0.044 Uiso 1 1 calc R . . C21 C 0.0352(6) -0.1174(6) 0.1295(4) 0.0332(18) Uani 1 1 d . . . H21 H -0.0152 -0.1722 0.0827 0.040 Uiso 1 1 calc R . . C22 C 0.0724(6) -0.3697(6) 0.1356(4) 0.0254(16) Uani 1 1 d . . . C23 C 0.1549(6) -0.3304(6) 0.0969(4) 0.0340(18) Uani 1 1 d . . . H23 H 0.1749 -0.2546 0.1053 0.041 Uiso 1 1 calc R . . C24 C 0.2083(7) -0.4023(7) 0.0460(4) 0.042(2) Uani 1 1 d . . . H24 H 0.2630 -0.3748 0.0194 0.051 Uiso 1 1 calc R . . C25 C 0.1812(7) -0.5142(7) 0.0341(4) 0.041(2) Uani 1 1 d . . . H25 H 0.2179 -0.5624 0.0001 0.049 Uiso 1 1 calc R . . C26 C 0.0985(7) -0.5548(6) 0.0734(5) 0.043(2) Uani 1 1 d . . . H26 H 0.0798 -0.6305 0.0653 0.051 Uiso 1 1 calc R . . C27 C 0.0438(7) -0.4842(6) 0.1241(4) 0.040(2) Uani 1 1 d . . . H27 H -0.0113 -0.5119 0.1504 0.048 Uiso 1 1 calc R . . P2 P 0.39894(16) 0.30822(14) 0.55755(10) 0.0245(4) Uani 1 1 d . . . C28 C 0.4786(6) 0.2429(5) 0.4833(4) 0.0232(15) Uani 1 1 d . . . C29 C 0.5574(6) 0.3083(6) 0.4554(4) 0.0335(18) Uani 1 1 d . . . H29 H 0.5707 0.3860 0.4785 0.040 Uiso 1 1 calc R . . C30 C 0.6161(7) 0.2602(7) 0.3943(4) 0.042(2) Uani 1 1 d . . . H30 H 0.6673 0.3048 0.3753 0.051 Uiso 1 1 calc R . . C31 C 0.5983(8) 0.1462(7) 0.3620(4) 0.046(2) Uani 1 1 d . . . H31 H 0.6390 0.1139 0.3215 0.055 Uiso 1 1 calc R . . C32 C 0.5212(8) 0.0780(7) 0.3881(5) 0.049(2) Uani 1 1 d . . . H32 H 0.5081 0.0005 0.3645 0.059 Uiso 1 1 calc R . . C33 C 0.4644(7) 0.1276(6) 0.4496(5) 0.040(2) Uani 1 1 d . . . H33 H 0.4148 0.0824 0.4694 0.048 Uiso 1 1 calc R . . C34 C 0.3088(7) 0.2004(5) 0.5809(4) 0.0326(18) Uani 1 1 d . . . C35 C 0.3304(7) 0.1803(6) 0.6561(4) 0.0351(19) Uani 1 1 d . . . H35 H 0.3909 0.2271 0.6989 0.042 Uiso 1 1 calc R . . C36 C 0.2625(8) 0.0908(7) 0.6681(5) 0.049(2) Uani 1 1 d . . . H36 H 0.2769 0.0767 0.7185 0.058 Uiso 1 1 calc R . . C37 C 0.1716(8) 0.0217(7) 0.6028(6) 0.054(3) Uani 1 1 d . . . H37 H 0.1247 -0.0377 0.6108 0.065 Uiso 1 1 calc R . . C38 C 0.1505(7) 0.0398(7) 0.5284(5) 0.048(2) Uani 1 1 d . . . H38 H 0.0914 -0.0087 0.4851 0.057 Uiso 1 1 calc R . . C39 C 0.2169(7) 0.1302(6) 0.5168(5) 0.0390(19) Uani 1 1 d . . . H39 H 0.2007 0.1444 0.4667 0.047 Uiso 1 1 calc R . . C40 C 0.4937(6) 0.4096(5) 0.6537(4) 0.0254(16) Uani 1 1 d . . . C41 C 0.4843(6) 0.5192(5) 0.6888(4) 0.0295(17) Uani 1 1 d . . . H41 H 0.4309 0.5440 0.6627 0.035 Uiso 1 1 calc R . . C42 C 0.5587(7) 0.5909(6) 0.7652(4) 0.042(2) Uani 1 1 d . . . H42 H 0.5557 0.6651 0.7894 0.050 Uiso 1 1 calc R . . C43 C 0.6351(7) 0.5535(6) 0.8043(4) 0.045(2) Uani 1 1 d . . . H43 H 0.6832 0.6018 0.8552 0.055 Uiso 1 1 calc R . . C44 C 0.6411(7) 0.4438(6) 0.7683(4) 0.041(2) Uani 1 1 d . . . H44 H 0.6927 0.4181 0.7954 0.049 Uiso 1 1 calc R . . C45 C 0.5709(6) 0.3722(5) 0.6924(4) 0.0328(18) Uani 1 1 d . . . H45 H 0.5762 0.2988 0.6678 0.039 Uiso 1 1 calc R . . C46 C 0.3134(6) 0.3737(5) 0.5089(4) 0.0272(16) Uani 1 1 d . . . C47 C 0.3085(7) 0.3632(6) 0.4237(4) 0.0380(19) Uani 1 1 d . . . H47 H 0.3550 0.3263 0.3918 0.046 Uiso 1 1 calc R . . C48 C 0.2351(8) 0.4069(7) 0.3852(5) 0.055(3) Uani 1 1 d . . . H48 H 0.2320 0.3991 0.3278 0.066 Uiso 1 1 calc R . . C49 C 0.1676(8) 0.4614(7) 0.4323(7) 0.057(3) Uani 1 1 d . . . H49 H 0.1172 0.4895 0.4063 0.068 Uiso 1 1 calc R . . C50 C 0.1729(8) 0.4756(7) 0.5185(6) 0.053(2) Uani 1 1 d . . . H50 H 0.1287 0.5158 0.5507 0.064 Uiso 1 1 calc R . . C51 C 0.2438(7) 0.4301(6) 0.5562(5) 0.040(2) Uani 1 1 d . . . H51 H 0.2453 0.4369 0.6134 0.048 Uiso 1 1 calc R . . N4 N 0.9604(11) 0.1888(11) 0.3268(6) 0.119(5) Uani 1 1 d . . . C52 C 0.9585(9) 0.2003(9) 0.2639(7) 0.068(3) Uani 1 1 d . . . C53 C 0.9546(11) 0.2128(11) 0.1807(6) 0.092(4) Uani 1 1 d . . . H53A H 0.9244 0.2750 0.1819 0.138 Uiso 1 1 calc R . . H53B H 0.9084 0.1455 0.1368 0.138 Uiso 1 1 calc R . . H53C H 1.0285 0.2261 0.1685 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 Re1 0.02253(17) 0.01847(13) 0.01963(12) 0.00895(10) 0.00369(10) 0.00798(11) Re2 0.02421(17) 0.01796(13) 0.01870(12) 0.00980(10) 0.00363(10) 0.00647(11) Re3 0.02288(17) 0.01695(13) 0.01847(12) 0.00778(10) 0.00241(10) 0.00572(11) S1 0.0271(11) 0.0248(8) 0.0271(8) 0.0106(7) 0.0053(7) 0.0062(8) S2 0.0300(11) 0.0259(8) 0.0230(7) 0.0103(7) 0.0010(7) 0.0104(8) S3 0.0366(11) 0.0193(8) 0.0265(8) 0.0079(7) 0.0031(7) 0.0099(8) S4 0.0345(11) 0.0225(8) 0.0209(7) 0.0068(7) 0.0067(7) 0.0101(7) C1 0.031(4) 0.015(3) 0.021(3) 0.004(3) 0.002(3) 0.006(3) C2 0.027(4) 0.022(3) 0.022(3) 0.014(3) 0.001(3) 0.002(3) C3 0.037(5) 0.030(4) 0.034(4) 0.016(3) 0.011(3) 0.016(4) N1 0.042(5) 0.037(3) 0.041(3) 0.016(3) 0.004(3) 0.012(3) N2 0.050(5) 0.027(3) 0.049(4) 0.009(3) -0.009(3) 0.001(3) N3 0.039(4) 0.041(4) 0.037(3) 0.010(3) 0.000(3) 0.006(3) P1 0.0246(11) 0.0265(9) 0.0234(8) 0.0101(7) 0.0034(7) 0.0071(8) C4 0.034(4) 0.024(3) 0.016(3) 0.007(3) 0.001(3) 0.011(3) C5 0.034(5) 0.033(4) 0.029(3) 0.014(3) 0.006(3) 0.013(3) C6 0.029(5) 0.048(4) 0.047(4) 0.037(4) 0.015(3) 0.019(4) C7 0.018(4) 0.057(5) 0.043(4) 0.012(4) 0.001(3) 0.009(4) C8 0.035(5) 0.033(4) 0.039(4) 0.008(4) 0.007(4) -0.002(4) C9 0.035(5) 0.033(4) 0.038(4) 0.027(3) 0.010(3) 0.008(3) C10 0.030(4) 0.022(3) 0.028(3) 0.010(3) 0.002(3) 0.009(3) C11 0.029(5) 0.039(4) 0.034(4) 0.015(3) 0.003(3) 0.009(3) C12 0.038(5) 0.051(5) 0.021(3) 0.015(3) 0.006(3) 0.006(4) C13 0.051(6) 0.049(5) 0.029(3) 0.025(4) 0.001(4) 0.013(4) C14 0.035(5) 0.080(6) 0.041(4) 0.021(4) -0.001(4) 0.028(5) C15 0.043(6) 0.056(5) 0.035(4) 0.010(4) 0.005(4) 0.026(4) C16 0.022(4) 0.037(4) 0.029(3) 0.016(3) 0.008(3) 0.007(3) C17 0.060(6) 0.036(4) 0.018(3) 0.015(3) -0.004(3) 0.004(4) C18 0.068(7) 0.040(4) 0.034(4) 0.012(4) 0.000(4) 0.000(4) C19 0.049(6) 0.045(5) 0.064(5) 0.029(4) 0.021(4) 0.012(4) C20 0.038(5) 0.042(4) 0.042(4) 0.025(4) 0.014(4) 0.011(4) C21 0.028(4) 0.040(4) 0.023(3) 0.005(3) -0.006(3) 0.007(3) C22 0.022(4) 0.034(4) 0.020(3) 0.009(3) -0.001(3) 0.008(3) C23 0.026(4) 0.041(4) 0.032(3) 0.010(3) 0.006(3) 0.006(3) C24 0.027(5) 0.061(5) 0.032(4) 0.010(4) 0.001(3) 0.010(4) C25 0.038(5) 0.053(5) 0.023(3) 0.001(4) -0.007(3) 0.021(4) C26 0.042(6) 0.028(4) 0.048(4) 0.005(4) -0.004(4) 0.006(4) C27 0.042(5) 0.038(4) 0.037(4) 0.013(4) 0.004(4) 0.011(4) P2 0.0251(11) 0.0215(8) 0.0261(8) 0.0092(7) 0.0033(7) 0.0041(7) C28 0.024(4) 0.025(3) 0.020(3) 0.013(3) -0.003(3) 0.000(3) C29 0.030(5) 0.033(4) 0.035(4) 0.010(3) 0.004(3) 0.008(3) C30 0.038(5) 0.067(5) 0.027(3) 0.019(4) 0.009(3) 0.020(4) C31 0.060(7) 0.055(5) 0.029(4) 0.010(4) 0.013(4) 0.035(5) C32 0.056(6) 0.040(4) 0.037(4) -0.005(4) 0.005(4) 0.014(4) C33 0.031(5) 0.024(4) 0.056(4) 0.007(4) 0.005(4) 0.002(3) C34 0.035(5) 0.025(3) 0.036(4) 0.008(3) 0.010(3) 0.008(3) C35 0.051(6) 0.025(4) 0.032(3) 0.014(3) 0.008(3) 0.009(4) C36 0.070(7) 0.044(5) 0.039(4) 0.017(4) 0.019(4) 0.021(5) C37 0.063(7) 0.040(4) 0.065(5) 0.020(5) 0.037(5) 0.008(5) C38 0.041(6) 0.045(5) 0.053(5) 0.015(4) 0.012(4) 0.006(4) C39 0.032(5) 0.045(4) 0.040(4) 0.017(4) 0.006(3) 0.006(4) C40 0.023(4) 0.025(3) 0.026(3) 0.007(3) 0.004(3) 0.006(3) C41 0.034(5) 0.020(3) 0.038(4) 0.016(3) 0.001(3) 0.007(3) C42 0.063(6) 0.019(3) 0.036(4) -0.003(3) 0.017(4) 0.012(4) C43 0.054(6) 0.037(4) 0.029(4) -0.004(3) -0.005(4) 0.007(4) C44 0.028(5) 0.042(4) 0.038(4) 0.001(4) -0.010(3) 0.010(4) C45 0.035(5) 0.019(3) 0.037(4) 0.003(3) 0.005(3) 0.006(3) C46 0.011(4) 0.024(3) 0.037(4) 0.007(3) 0.000(3) -0.006(3) C47 0.040(5) 0.032(4) 0.041(4) 0.017(3) 0.002(4) 0.003(4) C48 0.051(6) 0.056(5) 0.052(5) 0.029(5) -0.018(4) 0.000(5) C49 0.030(5) 0.054(5) 0.093(7) 0.048(5) -0.013(5) 0.002(4) C50 0.036(6) 0.044(5) 0.092(7) 0.037(5) 0.012(5) 0.016(4) C51 0.024(5) 0.035(4) 0.064(5) 0.023(4) 0.010(4) 0.002(3) N4 0.144(12) 0.145(10) 0.069(6) 0.053(7) 0.035(7) 0.011(9) C52 0.047(7) 0.078(7) 0.069(6) 0.025(6) 0.007(5) -0.003(5) C53 0.088(10) 0.139(11) 0.079(7) 0.057(8) 0.028(7) 0.054(9) _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 Re1 C1 2.184(7) . ? Re1 S2 2.4005(16) . ? Re1 S4 2.4032(16) . ? Re1 S1 2.4105(18) . ? Re1 S3 2.4131(19) . ? Re1 Re3 2.6030(7) . ? Re1 Re2 2.6068(6) 2_655 ? Re1 Re2 2.6119(5) . ? Re1 Re3 2.6129(6) 2_655 ? Re1 Re1 3.6863(8) 2_655 ? Re2 C2 2.141(7) . ? Re2 S1 2.3988(19) . ? Re2 S4 2.4010(15) . ? Re2 S2 2.4085(19) 2_655 ? Re2 S3 2.4090(15) 2_655 ? Re2 Re1 2.6068(6) 2_655 ? Re2 Re3 2.6089(6) 2_655 ? Re2 Re3 2.6125(6) . ? Re2 Re2 3.6941(7) 2_655 ? Re3 C3 2.173(7) . ? Re3 S2 2.4005(18) 2_655 ? Re3 S3 2.4011(19) . ? Re3 S1 2.4024(18) 2_655 ? Re3 S4 2.4095(19) . ? Re3 Re2 2.6089(6) 2_655 ? Re3 Re1 2.6129(6) 2_655 ? Re3 Re3 3.6901(11) 2_655 ? S1 Re3 2.4025(18) 2_655 ? S2 Re3 2.4005(18) 2_655 ? S2 Re2 2.4085(19) 2_655 ? S3 Re2 2.4090(15) 2_655 ? C1 N1 1.067(9) . ? C2 N2 1.078(9) . ? C3 N3 1.096(8) . ? P1 C10 1.789(7) . ? P1 C4 1.796(7) . ? P1 C16 1.799(7) . ? P1 C22 1.807(6) . ? C4 C9 1.390(10) . ? C4 C5 1.398(9) . ? C5 C6 1.387(10) . ? C6 C7 1.376(11) . ? C7 C8 1.374(11) . ? C8 C9 1.375(10) . ? C10 C11 1.387(10) . ? C10 C15 1.395(10) . ? C11 C12 1.378(10) . ? C12 C13 1.358(11) . ? C13 C14 1.374(12) . ? C14 C15 1.407(10) . ? C16 C17 1.390(9) . ? C16 C21 1.399(10) . ? C17 C18 1.389(11) . ? C18 C19 1.367(11) . ? C19 C20 1.386(11) . ? C20 C21 1.378(10) . ? C22 C23 1.375(10) . ? C22 C27 1.409(10) . ? C23 C24 1.378(10) . ? C24 C25 1.375(12) . ? C25 C26 1.390(12) . ? C26 C27 1.378(10) . ? P2 C28 1.780(7) . ? P2 C46 1.789(8) . ? P2 C34 1.794(8) . ? P2 C40 1.816(6) . ? C28 C33 1.389(9) . ? C28 C29 1.392(10) . ? C29 C30 1.378(10) . ? C30 C31 1.367(11) . ? C31 C32 1.382(12) . ? C32 C33 1.372(10) . ? C34 C35 1.384(10) . ? C34 C39 1.404(10) . ? C35 C36 1.384(11) . ? C36 C37 1.403(12) . ? C37 C38 1.354(12) . ? C38 C39 1.381(11) . ? C40 C45 1.366(10) . ? C40 C41 1.392(9) . ? C41 C42 1.407(10) . ? C42 C43 1.362(11) . ? C43 C44 1.381(10) . ? C44 C45 1.379(9) . ? C46 C47 1.382(10) . ? C46 C51 1.395(10) . ? C47 C48 1.387(12) . ? C48 C49 1.361(13) . ? C49 C50 1.387(13) . ? C50 C51 1.374(12) . ? N4 C52 1.112(13) . ? C52 C53 1.454(15) . ? 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 C1 Re1 S2 92.78(16) . . ? C1 Re1 S4 94.18(16) . . ? S2 Re1 S4 173.02(6) . . ? C1 Re1 S1 95.67(18) . . ? S2 Re1 S1 89.46(6) . . ? S4 Re1 S1 89.39(6) . . ? C1 Re1 S3 91.55(18) . . ? S2 Re1 S3 90.25(6) . . ? S4 Re1 S3 90.03(6) . . ? S1 Re1 S3 172.78(6) . . ? C1 Re1 Re3 134.01(15) . . ? S2 Re1 Re3 117.37(5) . . ? S4 Re1 Re3 57.38(5) . . ? S1 Re1 Re3 116.98(5) . . ? S3 Re1 Re3 57.05(5) . . ? C1 Re1 Re2 133.02(18) . 2_655 ? S2 Re1 Re2 57.32(5) . 2_655 ? S4 Re1 Re2 117.42(5) . 2_655 ? S1 Re1 Re2 117.00(4) . 2_655 ? S3 Re1 Re2 57.20(4) . 2_655 ? Re3 Re1 Re2 60.102(15) . 2_655 ? C1 Re1 Re2 136.84(18) . . ? S2 Re1 Re2 116.91(4) . . ? S4 Re1 Re2 57.03(4) . . ? S1 Re1 Re2 56.89(5) . . ? S3 Re1 Re2 117.13(5) . . ? Re3 Re1 Re2 60.128(17) . . ? Re2 Re1 Re2 90.121(17) 2_655 . ? C1 Re1 Re3 135.87(15) . 2_655 ? S2 Re1 Re3 57.03(4) . 2_655 ? S4 Re1 Re3 116.90(4) . 2_655 ? S1 Re1 Re3 56.97(4) . 2_655 ? S3 Re1 Re3 117.22(4) . 2_655 ? Re3 Re1 Re3 90.06(2) . 2_655 ? Re2 Re1 Re3 60.067(17) 2_655 2_655 ? Re2 Re1 Re3 59.911(15) . 2_655 ? C1 Re1 Re1 177.98(18) . 2_655 ? S2 Re1 Re1 86.50(5) . 2_655 ? S4 Re1 Re1 86.56(5) . 2_655 ? S1 Re1 Re1 86.21(5) . 2_655 ? S3 Re1 Re1 86.57(5) . 2_655 ? Re3 Re1 Re1 45.139(13) . 2_655 ? Re2 Re1 Re1 45.117(12) 2_655 2_655 ? Re2 Re1 Re1 45.004(12) . 2_655 ? Re3 Re1 Re1 44.920(16) 2_655 2_655 ? C2 Re2 S1 94.99(19) . . ? C2 Re2 S4 92.91(17) . . ? S1 Re2 S4 89.72(6) . . ? C2 Re2 S2 92.37(19) . 2_655 ? S1 Re2 S2 172.65(6) . 2_655 ? S4 Re2 S2 89.83(6) . 2_655 ? C2 Re2 S3 93.96(17) . 2_655 ? S1 Re2 S3 89.42(6) . 2_655 ? S4 Re2 S3 173.13(6) . 2_655 ? S2 Re2 S3 90.15(6) 2_655 2_655 ? C2 Re2 Re1 134.35(19) . 2_655 ? S1 Re2 Re1 116.99(4) . 2_655 ? S4 Re2 Re1 117.30(5) . 2_655 ? S2 Re2 Re1 57.03(4) 2_655 2_655 ? S3 Re2 Re1 57.35(5) 2_655 2_655 ? C2 Re2 Re3 136.41(16) . 2_655 ? S1 Re2 Re3 57.15(4) . 2_655 ? S4 Re2 Re3 117.14(5) . 2_655 ? S2 Re2 Re3 116.85(5) 2_655 2_655 ? S3 Re2 Re3 57.01(5) 2_655 2_655 ? Re1 Re2 Re3 59.877(17) 2_655 2_655 ? C2 Re2 Re1 135.74(19) . . ? S1 Re2 Re1 57.32(5) . . ? S4 Re2 Re1 57.11(4) . . ? S2 Re2 Re1 116.67(5) 2_655 . ? S3 Re2 Re1 117.04(5) 2_655 . ? Re1 Re2 Re1 89.879(17) 2_655 . ? Re3 Re2 Re1 60.064(15) 2_655 . ? C2 Re2 Re3 133.64(16) . . ? S1 Re2 Re3 117.04(5) . . ? S4 Re2 Re3 57.26(5) . . ? S2 Re2 Re3 56.95(5) 2_655 . ? S3 Re2 Re3 117.38(5) 2_655 . ? Re1 Re2 Re3 60.083(16) 2_655 . ? Re3 Re2 Re3 89.94(2) 2_655 . ? Re1 Re2 Re3 59.766(16) . . ? C2 Re2 Re2 178.44(17) . 2_655 ? S1 Re2 Re2 86.47(5) . 2_655 ? S4 Re2 Re2 86.54(5) . 2_655 ? S2 Re2 Re2 86.17(5) 2_655 2_655 ? S3 Re2 Re2 86.60(5) 2_655 2_655 ? Re1 Re2 Re2 44.996(12) 2_655 2_655 ? Re3 Re2 Re2 45.009(14) 2_655 2_655 ? Re1 Re2 Re2 44.884(11) . 2_655 ? Re3 Re2 Re2 44.930(14) . 2_655 ? C3 Re3 S2 94.3(2) . 2_655 ? C3 Re3 S3 92.3(2) . . ? S2 Re3 S3 173.32(5) 2_655 . ? C3 Re3 S1 94.3(2) . 2_655 ? S2 Re3 S1 89.65(6) 2_655 2_655 ? S3 Re3 S1 89.53(6) . 2_655 ? C3 Re3 S4 93.0(2) . . ? S2 Re3 S4 89.81(6) 2_655 . ? S3 Re3 S4 90.17(7) . . ? S1 Re3 S4 172.74(5) 2_655 . ? C3 Re3 Re1 133.88(19) . . ? S2 Re3 Re1 117.30(5) 2_655 . ? S3 Re3 Re1 57.49(5) . . ? S1 Re3 Re1 117.00(4) 2_655 . ? S4 Re3 Re1 57.14(4) . . ? C3 Re3 Re2 134.9(2) . 2_655 ? S2 Re3 Re2 117.02(4) 2_655 2_655 ? S3 Re3 Re2 57.30(4) . 2_655 ? S1 Re3 Re2 57.02(4) 2_655 2_655 ? S4 Re3 Re2 117.11(4) . 2_655 ? Re1 Re3 Re2 60.021(19) . 2_655 ? C3 Re3 Re2 135.1(2) . . ? S2 Re3 Re2 57.24(5) 2_655 . ? S3 Re3 Re2 117.56(5) . . ? S1 Re3 Re2 117.07(4) 2_655 . ? S4 Re3 Re2 56.95(4) . . ? Re1 Re3 Re2 60.105(17) . . ? Re2 Re3 Re2 90.06(2) 2_655 . ? C3 Re3 Re1 136.18(19) . 2_655 ? S2 Re3 Re1 57.03(4) 2_655 2_655 ? S3 Re3 Re1 117.29(4) . 2_655 ? S1 Re3 Re1 57.27(4) 2_655 2_655 ? S4 Re3 Re1 116.76(4) . 2_655 ? Re1 Re3 Re1 89.94(2) . 2_655 ? Re2 Re3 Re1 60.025(16) 2_655 2_655 ? Re2 Re3 Re1 59.850(16) . 2_655 ? C3 Re3 Re3 178.96(19) . 2_655 ? S2 Re3 Re3 86.45(4) 2_655 2_655 ? S3 Re3 Re3 86.88(4) . 2_655 ? S1 Re3 Re3 86.41(4) 2_655 2_655 ? S4 Re3 Re3 86.33(4) . 2_655 ? Re1 Re3 Re3 45.079(16) . 2_655 ? Re2 Re3 Re3 45.070(15) 2_655 2_655 ? Re2 Re3 Re3 44.991(14) . 2_655 ? Re1 Re3 Re3 44.861(13) 2_655 2_655 ? Re2 S1 Re3 65.83(5) . 2_655 ? Re2 S1 Re1 65.79(5) . . ? Re3 S1 Re1 65.76(5) 2_655 . ? Re1 S2 Re3 65.95(5) . 2_655 ? Re1 S2 Re2 65.65(5) . 2_655 ? Re3 S2 Re2 65.81(5) 2_655 2_655 ? Re3 S3 Re2 65.69(4) . 2_655 ? Re3 S3 Re1 65.46(5) . . ? Re2 S3 Re1 65.45(4) 2_655 . ? Re2 S4 Re1 65.87(4) . . ? Re2 S4 Re3 65.79(4) . . ? Re1 S4 Re3 65.48(4) . . ? N1 C1 Re1 178.4(7) . . ? N2 C2 Re2 178.5(6) . . ? N3 C3 Re3 178.9(7) . . ? C10 P1 C4 109.1(3) . . ? C10 P1 C16 108.8(3) . . ? C4 P1 C16 112.2(3) . . ? C10 P1 C22 106.9(3) . . ? C4 P1 C22 112.1(3) . . ? C16 P1 C22 107.6(3) . . ? C9 C4 C5 118.7(7) . . ? C9 C4 P1 120.4(5) . . ? C5 C4 P1 120.9(5) . . ? C6 C5 C4 120.2(7) . . ? C7 C6 C5 119.2(7) . . ? C8 C7 C6 121.5(7) . . ? C7 C8 C9 119.2(7) . . ? C8 C9 C4 121.0(7) . . ? C11 C10 C15 119.6(7) . . ? C11 C10 P1 122.1(6) . . ? C15 C10 P1 118.1(6) . . ? C12 C11 C10 119.8(7) . . ? C13 C12 C11 121.1(7) . . ? C12 C13 C14 120.7(7) . . ? C13 C14 C15 119.4(8) . . ? C10 C15 C14 119.4(7) . . ? C17 C16 C21 120.0(7) . . ? C17 C16 P1 120.1(5) . . ? C21 C16 P1 119.4(5) . . ? C18 C17 C16 119.9(7) . . ? C19 C18 C17 119.9(7) . . ? C18 C19 C20 120.6(8) . . ? C21 C20 C19 120.6(7) . . ? C20 C21 C16 119.1(6) . . ? C23 C22 C27 119.4(6) . . ? C23 C22 P1 120.7(5) . . ? C27 C22 P1 119.6(6) . . ? C22 C23 C24 120.7(7) . . ? C25 C24 C23 120.5(8) . . ? C24 C25 C26 119.3(7) . . ? C27 C26 C25 120.9(8) . . ? C26 C27 C22 119.1(8) . . ? C28 P2 C46 109.8(3) . . ? C28 P2 C34 107.7(3) . . ? C46 P2 C34 107.8(3) . . ? C28 P2 C40 108.6(3) . . ? C46 P2 C40 111.3(3) . . ? C34 P2 C40 111.6(3) . . ? C33 C28 C29 117.4(7) . . ? C33 C28 P2 122.9(6) . . ? C29 C28 P2 119.6(5) . . ? C30 C29 C28 121.2(7) . . ? C31 C30 C29 119.4(9) . . ? C30 C31 C32 121.3(7) . . ? C33 C32 C31 118.4(7) . . ? C32 C33 C28 122.1(8) . . ? C35 C34 C39 119.7(7) . . ? C35 C34 P2 122.7(6) . . ? C39 C34 P2 117.5(6) . . ? C34 C35 C36 120.3(7) . . ? C35 C36 C37 118.7(8) . . ? C38 C37 C36 121.5(8) . . ? C37 C38 C39 120.0(8) . . ? C38 C39 C34 119.8(8) . . ? C45 C40 C41 121.5(6) . . ? C45 C40 P2 117.1(5) . . ? C41 C40 P2 121.3(5) . . ? C40 C41 C42 117.4(7) . . ? C43 C42 C41 121.1(6) . . ? C42 C43 C44 119.8(6) . . ? C45 C44 C43 120.4(8) . . ? C40 C45 C44 119.7(6) . . ? C47 C46 C51 118.9(7) . . ? C47 C46 P2 121.7(6) . . ? C51 C46 P2 119.2(6) . . ? C46 C47 C48 120.8(8) . . ? C49 C48 C47 119.5(8) . . ? C48 C49 C50 120.8(8) . . ? C51 C50 C49 119.8(8) . . ? C50 C51 C46 120.1(8) . . ? N4 C52 C53 178.8(14) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.700 _refine_diff_density_min -1.370 _refine_diff_density_rms 0.186 #################### Material relevant to compound 4 at 200K ############ data_s8200k _database_code_CSD 187001 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(PPh4)4 (Re6S8(CN)6) (CH3CN)2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H86 N8 P4 Re6 S8' _chemical_formula_weight 2969.39 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' 'P' 'P' 0.1023 0.0942 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4400(16) _cell_length_b 13.0657(16) _cell_length_c 16.729(2) _cell_angle_alpha 109.471(14) _cell_angle_beta 95.916(15) _cell_angle_gamma 101.857(15) _cell_volume 2465.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.5390 _exptl_crystal_size_mid 0.3850 _exptl_crystal_size_min 0.0760 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 7.623 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0581 _exptl_absorpt_correction_T_max 0.5634 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, Phi. incr. == 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25335 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.94 _reflns_number_total 8946 _reflns_number_gt 6440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE, [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0158P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00022(4) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8946 _refine_ls_number_parameters 597 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.001 _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 0.38137(2) 0.06455(2) 0.014597(15) 0.01534(8) Uani 1 1 d . . . Re2 Re 0.46354(2) -0.06599(2) 0.078912(15) 0.01539(7) Uani 1 1 d . . . Re3 Re 0.59089(2) 0.12481(2) 0.087956(15) 0.01507(7) Uani 1 1 d . . . S1 S 0.27385(15) -0.11618(14) 0.00493(10) 0.0213(4) Uani 1 1 d . . . S2 S 0.34004(16) 0.00462(14) -0.13975(10) 0.0216(4) Uani 1 1 d . . . S3 S 0.50886(17) 0.23494(13) 0.02222(10) 0.0227(4) Uani 1 1 d . . . S4 S 0.44047(16) 0.11230(14) 0.16671(10) 0.0216(4) Uani 1 1 d . . . C1 C 0.2454(6) 0.1447(5) 0.0296(4) 0.0188(15) Uani 1 1 d . . . C2 C 0.4267(6) -0.1391(6) 0.1720(4) 0.0179(15) Uani 1 1 d . . . C3 C 0.6960(6) 0.2729(5) 0.1902(4) 0.0215(16) Uani 1 1 d . . . N1 N 0.1785(6) 0.1870(5) 0.0380(4) 0.0322(16) Uani 1 1 d . . . N2 N 0.4070(6) -0.1746(5) 0.2216(5) 0.0399(19) Uani 1 1 d . . . N3 N 0.7457(5) 0.3481(5) 0.2442(4) 0.0298(16) Uani 1 1 d . . . P1 P 0.00882(16) -0.27334(14) 0.20824(10) 0.0197(4) Uani 1 1 d . . . C4 C -0.1421(6) -0.3182(5) 0.1817(4) 0.0178(15) Uani 1 1 d . . . C5 C -0.2028(6) -0.2564(6) 0.1524(4) 0.0220(16) Uani 1 1 d . . . H5 H -0.1663 -0.1873 0.1514 0.026 Uiso 1 1 calc R . . C6 C -0.3178(7) -0.2960(6) 0.1243(4) 0.0261(17) Uani 1 1 d . . . H6 H -0.3579 -0.2554 0.1024 0.031 Uiso 1 1 calc R . . C7 C -0.3721(6) -0.3970(7) 0.1295(4) 0.032(2) Uani 1 1 d . . . H7 H -0.4492 -0.4240 0.1113 0.039 Uiso 1 1 calc R . . C8 C -0.3118(7) -0.4580(7) 0.1619(5) 0.035(2) Uani 1 1 d . . . H8 H -0.3486 -0.5251 0.1662 0.042 Uiso 1 1 calc R . . C9 C -0.1975(6) -0.4186(6) 0.1876(4) 0.0226(16) Uani 1 1 d . . . H9 H -0.1570 -0.4594 0.2089 0.027 Uiso 1 1 calc R . . C10 C 0.0536(6) -0.2711(5) 0.3141(4) 0.0195(15) Uani 1 1 d . . . C11 C -0.0156(6) -0.2626(6) 0.3745(4) 0.0276(18) Uani 1 1 d . . . H11 H -0.0893 -0.2613 0.3593 0.033 Uiso 1 1 calc R . . C12 C 0.0232(7) -0.2560(6) 0.4571(4) 0.033(2) Uani 1 1 d . . . H12 H -0.0247 -0.2519 0.4966 0.040 Uiso 1 1 calc R . . C13 C 0.1318(7) -0.2553(6) 0.4805(4) 0.0309(18) Uani 1 1 d . . . H13 H 0.1577 -0.2509 0.5360 0.037 Uiso 1 1 calc R . . C14 C 0.2032(7) -0.2612(7) 0.4221(5) 0.039(2) Uani 1 1 d . . . H14 H 0.2772 -0.2602 0.4387 0.047 Uiso 1 1 calc R . . C15 C 0.1650(7) -0.2688(6) 0.3384(4) 0.0316(19) Uani 1 1 d . . . H15 H 0.2133 -0.2722 0.2992 0.038 Uiso 1 1 calc R . . C16 C 0.0612(6) -0.1366(5) 0.2060(4) 0.0199(15) Uani 1 1 d . . . C17 C 0.1394(7) -0.0542(6) 0.2744(4) 0.0302(19) Uani 1 1 d . . . H17 H 0.1584 -0.0671 0.3248 0.036 Uiso 1 1 calc R . . C18 C 0.1882(7) 0.0451(6) 0.2678(5) 0.037(2) Uani 1 1 d . . . H18 H 0.2407 0.0991 0.3140 0.044 Uiso 1 1 calc R . . C19 C 0.1621(7) 0.0678(6) 0.1953(5) 0.038(2) Uani 1 1 d . . . H19 H 0.1961 0.1365 0.1924 0.046 Uiso 1 1 calc R . . C20 C 0.0838(7) -0.0133(6) 0.1256(4) 0.0292(18) Uani 1 1 d . . . H20 H 0.0652 0.0017 0.0761 0.035 Uiso 1 1 calc R . . C21 C 0.0337(6) -0.1162(6) 0.1297(4) 0.0267(17) Uani 1 1 d . . . H21 H -0.0173 -0.1709 0.0829 0.032 Uiso 1 1 calc R . . C22 C 0.0724(6) -0.3691(5) 0.1354(4) 0.0208(15) Uani 1 1 d . . . C23 C 0.1556(6) -0.3281(7) 0.0969(4) 0.0289(18) Uani 1 1 d . . . H23 H 0.1754 -0.2521 0.1055 0.035 Uiso 1 1 calc R . . C24 C 0.2095(7) -0.4009(7) 0.0453(4) 0.0333(19) Uani 1 1 d . . . H24 H 0.2645 -0.3736 0.0186 0.040 Uiso 1 1 calc R . . C25 C 0.1817(7) -0.5140(6) 0.0335(4) 0.0281(18) Uani 1 1 d . . . H25 H 0.2177 -0.5627 -0.0011 0.034 Uiso 1 1 calc R . . C26 C 0.1005(7) -0.5532(6) 0.0732(5) 0.035(2) Uani 1 1 d . . . H26 H 0.0832 -0.6287 0.0663 0.042 Uiso 1 1 calc R . . C27 C 0.0439(7) -0.4837(6) 0.1232(4) 0.0277(18) Uani 1 1 d . . . H27 H -0.0123 -0.5122 0.1484 0.033 Uiso 1 1 calc R . . P2 P 0.39906(16) 0.30857(14) 0.55746(10) 0.0196(4) Uani 1 1 d . . . C28 C 0.4790(6) 0.2424(5) 0.4828(3) 0.0156(14) Uani 1 1 d . . . C29 C 0.5570(7) 0.3086(6) 0.4549(5) 0.0304(19) Uani 1 1 d . . . H29 H 0.5694 0.3863 0.4776 0.037 Uiso 1 1 calc R . . C30 C 0.6169(7) 0.2601(7) 0.3931(4) 0.034(2) Uani 1 1 d . . . H30 H 0.6685 0.3048 0.3742 0.041 Uiso 1 1 calc R . . C31 C 0.5988(7) 0.1454(7) 0.3607(4) 0.034(2) Uani 1 1 d . . . H31 H 0.6379 0.1123 0.3190 0.041 Uiso 1 1 calc R . . C32 C 0.5230(8) 0.0784(6) 0.3892(5) 0.041(2) Uani 1 1 d . . . H32 H 0.5123 0.0009 0.3673 0.050 Uiso 1 1 calc R . . C33 C 0.4636(6) 0.1259(6) 0.4495(5) 0.0307(19) Uani 1 1 d . . . H33 H 0.4127 0.0805 0.4684 0.037 Uiso 1 1 calc R . . C34 C 0.3076(6) 0.2011(6) 0.5810(4) 0.0277(18) Uani 1 1 d . . . C35 C 0.3292(7) 0.1801(5) 0.6557(4) 0.0249(17) Uani 1 1 d . . . H35 H 0.3903 0.2261 0.6986 0.030 Uiso 1 1 calc R . . C36 C 0.2601(8) 0.0907(6) 0.6668(5) 0.038(2) Uani 1 1 d . . . H36 H 0.2739 0.0770 0.7175 0.046 Uiso 1 1 calc R . . C37 C 0.1700(7) 0.0210(6) 0.6022(5) 0.039(2) Uani 1 1 d . . . H37 H 0.1232 -0.0390 0.6099 0.047 Uiso 1 1 calc R . . C38 C 0.1500(7) 0.0401(6) 0.5280(5) 0.038(2) Uani 1 1 d . . . H38 H 0.0907 -0.0083 0.4844 0.046 Uiso 1 1 calc R . . C39 C 0.2168(6) 0.1308(6) 0.5161(5) 0.0322(19) Uani 1 1 d . . . H39 H 0.2015 0.1448 0.4657 0.039 Uiso 1 1 calc R . . C40 C 0.4930(6) 0.4101(5) 0.6532(4) 0.0171(14) Uani 1 1 d . . . C41 C 0.4859(7) 0.5200(6) 0.6899(4) 0.0269(17) Uani 1 1 d . . . H41 H 0.4319 0.5451 0.6644 0.032 Uiso 1 1 calc R . . C42 C 0.5598(7) 0.5922(6) 0.7647(4) 0.0316(19) Uani 1 1 d . . . H42 H 0.5580 0.6670 0.7878 0.038 Uiso 1 1 calc R . . C43 C 0.6354(7) 0.5541(6) 0.8048(4) 0.032(2) Uani 1 1 d . . . H43 H 0.6825 0.6025 0.8562 0.038 Uiso 1 1 calc R . . C44 C 0.6426(7) 0.4440(6) 0.7695(5) 0.035(2) Uani 1 1 d . . . H44 H 0.6943 0.4186 0.7969 0.043 Uiso 1 1 calc R . . C45 C 0.5716(7) 0.3720(5) 0.6926(4) 0.0245(17) Uani 1 1 d . . . H45 H 0.5769 0.2986 0.6677 0.029 Uiso 1 1 calc R . . C46 C 0.3127(6) 0.3743(5) 0.5090(4) 0.0217(16) Uani 1 1 d . . . C47 C 0.3086(7) 0.3645(6) 0.4224(4) 0.0264(17) Uani 1 1 d . . . H47 H 0.3550 0.3272 0.3901 0.032 Uiso 1 1 calc R . . C48 C 0.2361(8) 0.4099(7) 0.3849(5) 0.041(2) Uani 1 1 d . . . H48 H 0.2343 0.4037 0.3277 0.049 Uiso 1 1 calc R . . C49 C 0.1663(8) 0.4643(7) 0.4321(7) 0.049(2) Uani 1 1 d . . . H49 H 0.1157 0.4924 0.4061 0.059 Uiso 1 1 calc R . . C50 C 0.1716(7) 0.4772(7) 0.5177(6) 0.041(2) Uani 1 1 d . . . H50 H 0.1265 0.5167 0.5498 0.049 Uiso 1 1 calc R . . C51 C 0.2439(7) 0.4318(6) 0.5568(5) 0.0296(18) Uani 1 1 d . . . H51 H 0.2462 0.4398 0.6144 0.035 Uiso 1 1 calc R . . N4 N 0.9600(10) 0.1918(9) 0.3276(6) 0.090(4) Uani 1 1 d . . . C52 C 0.9592(9) 0.2007(9) 0.2638(6) 0.057(3) Uani 1 1 d . . . C53 C 0.9558(10) 0.2130(11) 0.1804(6) 0.076(4) Uani 1 1 d . . . H53A H 0.9284 0.2771 0.1821 0.114 Uiso 1 1 calc R . . H53B H 0.9072 0.1468 0.1367 0.114 Uiso 1 1 calc R . . H53C H 1.0298 0.2232 0.1673 0.114 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 Re1 0.01866(17) 0.01444(13) 0.01503(12) 0.00670(10) 0.00301(10) 0.00657(11) Re2 0.01998(17) 0.01418(13) 0.01420(12) 0.00739(10) 0.00290(10) 0.00545(11) Re3 0.01876(17) 0.01335(13) 0.01415(12) 0.00609(10) 0.00226(10) 0.00492(11) S1 0.0216(11) 0.0213(8) 0.0221(8) 0.0085(7) 0.0050(7) 0.0063(7) S2 0.0264(11) 0.0212(8) 0.0185(7) 0.0079(7) 0.0008(7) 0.0090(7) S3 0.0315(11) 0.0159(8) 0.0216(7) 0.0063(7) 0.0031(7) 0.0099(8) S4 0.0297(11) 0.0202(8) 0.0162(7) 0.0048(7) 0.0067(7) 0.0108(8) C1 0.027(4) 0.011(3) 0.017(3) 0.002(3) 0.003(3) 0.006(3) C2 0.021(4) 0.024(4) 0.014(3) 0.016(3) 0.005(3) 0.003(3) C3 0.025(4) 0.020(3) 0.024(3) 0.009(3) 0.009(3) 0.012(3) N1 0.033(4) 0.031(3) 0.031(3) 0.011(3) 0.003(3) 0.006(3) N2 0.034(4) 0.024(3) 0.047(4) 0.001(3) -0.007(3) 0.004(3) N3 0.028(4) 0.026(3) 0.025(3) -0.001(3) 0.000(3) 0.005(3) P1 0.0195(10) 0.0204(8) 0.0188(8) 0.0070(7) 0.0012(7) 0.0053(7) C4 0.023(4) 0.019(3) 0.012(3) 0.005(3) 0.004(3) 0.007(3) C5 0.029(5) 0.023(3) 0.022(3) 0.015(3) 0.007(3) 0.010(3) C6 0.029(5) 0.034(4) 0.029(3) 0.024(3) 0.010(3) 0.013(3) C7 0.012(4) 0.046(5) 0.030(4) 0.005(4) 0.000(3) 0.006(4) C8 0.022(5) 0.038(4) 0.038(4) 0.009(4) 0.004(3) 0.001(4) C9 0.029(5) 0.024(3) 0.025(3) 0.021(3) 0.006(3) 0.005(3) C10 0.020(4) 0.017(3) 0.022(3) 0.009(3) 0.001(3) 0.005(3) C11 0.018(4) 0.030(4) 0.029(3) 0.004(3) 0.001(3) 0.006(3) C12 0.041(5) 0.034(4) 0.020(3) 0.007(3) 0.006(3) 0.005(4) C13 0.033(5) 0.039(4) 0.026(3) 0.019(3) 0.003(3) 0.009(4) C14 0.033(5) 0.054(5) 0.032(4) 0.013(4) 0.002(4) 0.023(4) C15 0.027(5) 0.038(4) 0.029(4) 0.008(3) 0.007(3) 0.012(4) C16 0.024(4) 0.021(3) 0.023(3) 0.017(3) 0.009(3) 0.007(3) C17 0.047(6) 0.025(4) 0.017(3) 0.018(3) -0.005(3) -0.005(3) C18 0.042(6) 0.029(4) 0.034(4) 0.015(4) -0.002(4) -0.006(4) C19 0.041(6) 0.022(4) 0.050(5) 0.017(4) 0.006(4) 0.001(4) C20 0.034(5) 0.040(4) 0.032(4) 0.031(4) 0.014(3) 0.015(4) C21 0.021(4) 0.028(4) 0.020(3) 0.001(3) -0.002(3) 0.001(3) C22 0.022(4) 0.023(3) 0.019(3) 0.011(3) 0.000(3) 0.005(3) C23 0.025(4) 0.040(4) 0.016(3) 0.002(3) -0.001(3) 0.011(4) C24 0.027(5) 0.045(5) 0.028(4) 0.012(4) 0.007(3) 0.009(4) C25 0.028(5) 0.037(4) 0.014(3) 0.000(3) -0.004(3) 0.016(4) C26 0.040(5) 0.021(4) 0.036(4) 0.000(3) -0.002(4) 0.013(4) C27 0.036(5) 0.024(4) 0.026(3) 0.014(3) 0.007(3) 0.003(3) P2 0.0208(11) 0.0173(8) 0.0211(8) 0.0077(7) 0.0039(7) 0.0041(7) C28 0.021(4) 0.017(3) 0.009(3) 0.010(2) -0.003(2) 0.001(3) C29 0.028(5) 0.027(4) 0.037(4) 0.011(3) 0.002(3) 0.013(3) C30 0.027(5) 0.058(5) 0.018(3) 0.010(3) 0.005(3) 0.019(4) C31 0.046(6) 0.044(5) 0.019(3) 0.011(3) 0.013(3) 0.024(4) C32 0.052(6) 0.026(4) 0.032(4) -0.008(4) 0.000(4) 0.015(4) C33 0.020(4) 0.019(3) 0.045(4) 0.006(3) 0.003(3) 0.000(3) C34 0.028(5) 0.025(4) 0.030(4) 0.006(3) 0.010(3) 0.011(3) C35 0.036(5) 0.019(3) 0.026(3) 0.017(3) 0.006(3) 0.004(3) C36 0.063(7) 0.030(4) 0.032(4) 0.014(4) 0.019(4) 0.023(4) C37 0.046(6) 0.026(4) 0.038(4) 0.007(4) 0.022(4) -0.003(4) C38 0.021(4) 0.032(4) 0.046(4) 0.001(4) 0.009(4) -0.006(3) C39 0.023(5) 0.033(4) 0.031(4) 0.005(3) 0.002(3) -0.001(3) C40 0.020(4) 0.011(3) 0.019(3) 0.006(3) 0.007(3) 0.001(3) C41 0.029(5) 0.026(4) 0.033(4) 0.017(3) 0.008(3) 0.012(3) C42 0.056(6) 0.019(3) 0.026(3) 0.013(3) 0.013(4) 0.011(4) C43 0.050(6) 0.025(4) 0.014(3) 0.009(3) 0.003(3) -0.004(4) C44 0.028(5) 0.028(4) 0.038(4) -0.001(3) -0.007(3) 0.009(3) C45 0.042(5) 0.015(3) 0.018(3) 0.006(3) 0.011(3) 0.007(3) C46 0.011(4) 0.017(3) 0.030(3) 0.006(3) -0.001(3) -0.006(3) C47 0.036(5) 0.023(3) 0.030(3) 0.025(3) 0.005(3) 0.004(3) C48 0.043(6) 0.041(5) 0.040(4) 0.027(4) -0.009(4) -0.001(4) C49 0.023(5) 0.048(5) 0.085(7) 0.041(5) -0.007(5) 0.005(4) C50 0.032(5) 0.038(4) 0.071(6) 0.040(5) 0.012(4) 0.010(4) C51 0.030(5) 0.027(4) 0.042(4) 0.028(4) 0.012(3) 0.001(3) N4 0.122(11) 0.101(8) 0.063(6) 0.057(6) 0.032(6) 0.008(7) C52 0.044(7) 0.068(7) 0.061(6) 0.028(6) 0.017(5) 0.007(5) C53 0.073(9) 0.128(10) 0.067(6) 0.061(7) 0.033(6) 0.057(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 Re1 C1 2.159(7) . ? Re1 S2 2.3995(16) . ? Re1 S4 2.4028(17) . ? Re1 S1 2.4071(19) . ? Re1 S3 2.410(2) . ? Re1 Re3 2.6024(6) . ? Re1 Re2 2.6070(6) 2_655 ? Re1 Re2 2.6124(5) . ? Re1 Re3 2.6128(6) 2_655 ? Re1 Re1 3.6863(7) 2_655 ? Re2 C2 2.123(7) . ? Re2 S4 2.3973(16) . ? Re2 S1 2.3982(19) . ? Re2 S2 2.406(2) 2_655 ? Re2 S3 2.4073(16) 2_655 ? Re2 Re1 2.6070(6) 2_655 ? Re2 Re3 2.6093(5) 2_655 ? Re2 Re3 2.6122(6) . ? Re2 Re2 3.6951(7) 2_655 ? Re3 C3 2.161(6) . ? Re3 S3 2.3976(19) . ? Re3 S1 2.3997(18) 2_655 ? Re3 S2 2.4019(19) 2_655 ? Re3 S4 2.4064(19) . ? Re3 Re2 2.6093(5) 2_655 ? Re3 Re1 2.6128(6) 2_655 ? Re3 Re3 3.6892(11) 2_655 ? S1 Re3 2.3997(18) 2_655 ? S2 Re3 2.4018(18) 2_655 ? S2 Re2 2.406(2) 2_655 ? S3 Re2 2.4072(16) 2_655 ? C1 N1 1.086(9) . ? C2 N2 1.103(9) . ? C3 N3 1.099(8) . ? P1 C16 1.786(7) . ? P1 C10 1.790(7) . ? P1 C22 1.807(7) . ? P1 C4 1.808(7) . ? C4 C5 1.379(9) . ? C4 C9 1.390(10) . ? C5 C6 1.390(10) . ? C6 C7 1.388(11) . ? C7 C8 1.394(11) . ? C8 C9 1.378(10) . ? C10 C11 1.385(10) . ? C10 C15 1.394(10) . ? C11 C12 1.384(10) . ? C12 C13 1.364(11) . ? C13 C14 1.381(11) . ? C14 C15 1.397(11) . ? C16 C17 1.390(9) . ? C16 C21 1.411(10) . ? C17 C18 1.360(11) . ? C18 C19 1.364(11) . ? C19 C20 1.396(10) . ? C20 C21 1.389(10) . ? C22 C23 1.383(10) . ? C22 C27 1.404(10) . ? C23 C24 1.391(10) . ? C24 C25 1.387(11) . ? C25 C26 1.369(12) . ? C26 C27 1.377(10) . ? P2 C28 1.786(7) . ? P2 C46 1.792(8) . ? P2 C34 1.797(8) . ? P2 C40 1.803(6) . ? C28 C29 1.387(11) . ? C28 C33 1.398(9) . ? C29 C30 1.393(10) . ? C30 C31 1.372(11) . ? C31 C32 1.384(12) . ? C32 C33 1.369(11) . ? C34 C35 1.378(10) . ? C34 C39 1.398(10) . ? C35 C36 1.379(11) . ? C36 C37 1.388(12) . ? C37 C38 1.354(12) . ? C38 C39 1.386(11) . ? C40 C45 1.387(10) . ? C40 C41 1.387(9) . ? C41 C42 1.387(10) . ? C42 C43 1.366(11) . ? C43 C44 1.386(10) . ? C44 C45 1.392(9) . ? C46 C51 1.392(10) . ? C46 C47 1.407(9) . ? C47 C48 1.383(11) . ? C48 C49 1.380(13) . ? C49 C50 1.378(13) . ? C50 C51 1.395(11) . ? N4 C52 1.110(12) . ? C52 C53 1.455(14) . ? 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 C1 Re1 S2 92.56(17) . . ? C1 Re1 S4 94.50(17) . . ? S2 Re1 S4 172.93(6) . . ? C1 Re1 S1 95.77(19) . . ? S2 Re1 S1 89.50(6) . . ? S4 Re1 S1 89.41(6) . . ? C1 Re1 S3 91.51(19) . . ? S2 Re1 S3 90.20(6) . . ? S4 Re1 S3 90.01(6) . . ? S1 Re1 S3 172.72(6) . . ? C1 Re1 Re3 134.11(16) . . ? S2 Re1 Re3 117.33(5) . . ? S4 Re1 Re3 57.31(5) . . ? S1 Re1 Re3 116.98(5) . . ? S3 Re1 Re3 57.00(5) . . ? C1 Re1 Re2 132.80(19) . 2_655 ? S2 Re1 Re2 57.26(5) . 2_655 ? S4 Re1 Re2 117.37(5) . 2_655 ? S1 Re1 Re2 116.96(4) . 2_655 ? S3 Re1 Re2 57.19(4) . 2_655 ? Re3 Re1 Re2 60.116(14) . 2_655 ? C1 Re1 Re2 137.05(19) . . ? S2 Re1 Re2 116.96(5) . . ? S4 Re1 Re2 56.93(4) . . ? S1 Re1 Re2 56.90(5) . . ? S3 Re1 Re2 117.08(5) . . ? Re3 Re1 Re2 60.120(16) . . ? Re2 Re1 Re2 90.138(16) 2_655 . ? C1 Re1 Re3 135.77(15) . 2_655 ? S2 Re1 Re3 57.07(4) . 2_655 ? S4 Re1 Re3 116.81(5) . 2_655 ? S1 Re1 Re3 56.94(4) . 2_655 ? S3 Re1 Re3 117.19(4) . 2_655 ? Re3 Re1 Re3 90.05(2) . 2_655 ? Re2 Re1 Re3 60.058(17) 2_655 2_655 ? Re2 Re1 Re3 59.916(14) . 2_655 ? C1 Re1 Re1 177.81(19) . 2_655 ? S2 Re1 Re1 86.49(5) . 2_655 ? S4 Re1 Re1 86.46(5) . 2_655 ? S1 Re1 Re1 86.19(5) . 2_655 ? S3 Re1 Re1 86.53(5) . 2_655 ? Re3 Re1 Re1 45.136(12) . 2_655 ? Re2 Re1 Re1 45.129(12) 2_655 2_655 ? Re2 Re1 Re1 45.009(12) . 2_655 ? Re3 Re1 Re1 44.909(16) 2_655 2_655 ? C2 Re2 S4 93.03(18) . . ? C2 Re2 S1 95.38(19) . . ? S4 Re2 S1 89.75(6) . . ? C2 Re2 S2 92.06(19) . 2_655 ? S4 Re2 S2 89.84(6) . 2_655 ? S1 Re2 S2 172.57(6) . 2_655 ? C2 Re2 S3 93.95(18) . 2_655 ? S4 Re2 S3 173.02(6) . 2_655 ? S1 Re2 S3 89.41(6) . 2_655 ? S2 Re2 S3 90.10(6) 2_655 2_655 ? C2 Re2 Re1 134.08(19) . 2_655 ? S4 Re2 Re1 117.26(5) . 2_655 ? S1 Re2 Re1 116.90(4) . 2_655 ? S2 Re2 Re1 57.03(4) 2_655 2_655 ? S3 Re2 Re1 57.28(5) 2_655 2_655 ? C2 Re2 Re3 136.54(17) . 2_655 ? S4 Re2 Re3 117.14(5) . 2_655 ? S1 Re2 Re3 57.08(4) . 2_655 ? S2 Re2 Re3 116.83(5) 2_655 2_655 ? S3 Re2 Re3 56.93(5) 2_655 2_655 ? Re1 Re2 Re3 59.855(16) 2_655 2_655 ? C2 Re2 Re3 133.54(17) . . ? S4 Re2 Re3 57.23(5) . . ? S1 Re2 Re3 116.94(5) . . ? S2 Re2 Re3 57.02(5) 2_655 . ? S3 Re2 Re3 117.30(5) 2_655 . ? Re1 Re2 Re3 60.081(16) 2_655 . ? Re3 Re2 Re3 89.91(2) 2_655 . ? C2 Re2 Re1 136.02(19) . . ? S4 Re2 Re1 57.13(4) . . ? S1 Re2 Re1 57.23(5) . . ? S2 Re2 Re1 116.72(5) 2_655 . ? S3 Re2 Re1 116.94(5) 2_655 . ? Re1 Re2 Re1 89.862(16) 2_655 . ? Re3 Re2 Re1 60.048(15) 2_655 . ? Re3 Re2 Re1 59.750(16) . . ? C2 Re2 Re2 178.21(18) . 2_655 ? S4 Re2 Re2 86.53(5) . 2_655 ? S1 Re2 Re2 86.36(5) . 2_655 ? S2 Re2 Re2 86.21(5) 2_655 2_655 ? S3 Re2 Re2 86.50(5) 2_655 2_655 ? Re1 Re2 Re2 44.991(12) 2_655 2_655 ? Re3 Re2 Re2 44.985(13) 2_655 2_655 ? Re3 Re2 Re2 44.922(14) . 2_655 ? Re1 Re2 Re2 44.872(11) . 2_655 ? C3 Re3 S3 92.17(19) . . ? C3 Re3 S1 93.72(19) . 2_655 ? S3 Re3 S1 89.61(6) . 2_655 ? C3 Re3 S2 94.59(19) . 2_655 ? S3 Re3 S2 173.23(5) . 2_655 ? S1 Re3 S2 89.61(6) 2_655 2_655 ? C3 Re3 S4 93.58(19) . . ? S3 Re3 S4 90.21(7) . . ? S1 Re3 S4 172.70(5) 2_655 . ? S2 Re3 S4 89.71(6) 2_655 . ? C3 Re3 Re1 134.14(18) . . ? S3 Re3 Re1 57.45(5) . . ? S1 Re3 Re1 117.01(5) 2_655 . ? S2 Re3 Re1 117.24(5) 2_655 . ? S4 Re3 Re1 57.17(4) . . ? C3 Re3 Re2 134.29(19) . 2_655 ? S3 Re3 Re2 57.29(4) . 2_655 ? S1 Re3 Re2 57.03(4) 2_655 2_655 ? S2 Re3 Re2 116.99(4) 2_655 2_655 ? S4 Re3 Re2 117.14(5) . 2_655 ? Re1 Re3 Re2 60.029(18) . 2_655 ? C3 Re3 Re2 135.61(19) . . ? S3 Re3 Re2 117.53(5) . . ? S1 Re3 Re2 117.03(4) 2_655 . ? S2 Re3 Re2 57.16(5) 2_655 . ? S4 Re3 Re2 56.89(4) . . ? Re1 Re3 Re2 60.130(17) . . ? Re2 Re3 Re2 90.09(2) 2_655 . ? C3 Re3 Re1 135.89(18) . 2_655 ? S3 Re3 Re1 117.29(4) . 2_655 ? S1 Re3 Re1 57.21(4) 2_655 2_655 ? S2 Re3 Re1 56.99(4) 2_655 2_655 ? S4 Re3 Re1 116.71(4) . 2_655 ? Re1 Re3 Re1 89.95(2) . 2_655 ? Re2 Re3 Re1 60.035(16) 2_655 2_655 ? Re2 Re3 Re1 59.861(15) . 2_655 ? C3 Re3 Re3 179.01(19) . 2_655 ? S3 Re3 Re3 86.85(4) . 2_655 ? S1 Re3 Re3 86.38(4) 2_655 2_655 ? S2 Re3 Re3 86.39(4) 2_655 2_655 ? S4 Re3 Re3 86.33(4) . 2_655 ? Re1 Re3 Re3 45.091(16) . 2_655 ? Re2 Re3 Re3 45.078(14) 2_655 2_655 ? Re2 Re3 Re3 45.015(14) . 2_655 ? Re1 Re3 Re3 44.864(13) 2_655 2_655 ? Re2 S1 Re3 65.89(5) . 2_655 ? Re2 S1 Re1 65.87(5) . . ? Re3 S1 Re1 65.85(5) 2_655 . ? Re1 S2 Re3 65.94(5) . 2_655 ? Re1 S2 Re2 65.71(5) . 2_655 ? Re3 S2 Re2 65.82(5) 2_655 2_655 ? Re3 S3 Re2 65.78(4) . 2_655 ? Re3 S3 Re1 65.55(5) . . ? Re2 S3 Re1 65.53(4) 2_655 . ? Re2 S4 Re1 65.95(4) . . ? Re2 S4 Re3 65.88(4) . . ? Re1 S4 Re3 65.52(4) . . ? N1 C1 Re1 178.6(7) . . ? N2 C2 Re2 178.2(6) . . ? N3 C3 Re3 176.9(7) . . ? C16 P1 C10 108.8(3) . . ? C16 P1 C22 108.1(3) . . ? C10 P1 C22 106.9(3) . . ? C16 P1 C4 112.0(3) . . ? C10 P1 C4 109.0(3) . . ? C22 P1 C4 111.9(3) . . ? C5 C4 C9 119.5(7) . . ? C5 C4 P1 120.8(5) . . ? C9 C4 P1 119.6(5) . . ? C4 C5 C6 120.8(7) . . ? C7 C6 C5 119.1(7) . . ? C6 C7 C8 120.4(7) . . ? C9 C8 C7 119.6(8) . . ? C8 C9 C4 120.5(7) . . ? C11 C10 C15 119.1(6) . . ? C11 C10 P1 122.4(6) . . ? C15 C10 P1 118.2(5) . . ? C12 C11 C10 121.0(7) . . ? C13 C12 C11 119.9(7) . . ? C12 C13 C14 120.3(7) . . ? C13 C14 C15 120.4(8) . . ? C10 C15 C14 119.3(7) . . ? C17 C16 C21 119.3(6) . . ? C17 C16 P1 120.8(5) . . ? C21 C16 P1 119.4(5) . . ? C18 C17 C16 120.2(7) . . ? C17 C18 C19 121.8(7) . . ? C18 C19 C20 119.3(7) . . ? C21 C20 C19 120.3(7) . . ? C20 C21 C16 119.0(6) . . ? C23 C22 C27 119.8(6) . . ? C23 C22 P1 119.9(5) . . ? C27 C22 P1 120.1(6) . . ? C22 C23 C24 119.8(7) . . ? C25 C24 C23 120.3(8) . . ? C26 C25 C24 119.3(7) . . ? C25 C26 C27 121.7(7) . . ? C26 C27 C22 119.0(7) . . ? C28 P2 C46 110.1(3) . . ? C28 P2 C34 107.9(3) . . ? C46 P2 C34 107.2(3) . . ? C28 P2 C40 109.0(3) . . ? C46 P2 C40 110.9(3) . . ? C34 P2 C40 111.7(3) . . ? C29 C28 C33 118.8(6) . . ? C29 C28 P2 118.8(5) . . ? C33 C28 P2 122.3(6) . . ? C28 C29 C30 120.8(7) . . ? C31 C30 C29 119.1(8) . . ? C30 C31 C32 120.8(7) . . ? C33 C32 C31 120.2(7) . . ? C32 C33 C28 120.3(8) . . ? C35 C34 C39 120.0(7) . . ? C35 C34 P2 122.8(6) . . ? C39 C34 P2 116.9(6) . . ? C34 C35 C36 119.8(7) . . ? C35 C36 C37 120.1(7) . . ? C38 C37 C36 120.2(8) . . ? C37 C38 C39 120.8(7) . . ? C38 C39 C34 119.1(8) . . ? C45 C40 C41 120.1(6) . . ? C45 C40 P2 116.7(4) . . ? C41 C40 P2 123.1(6) . . ? C40 C41 C42 119.5(7) . . ? C43 C42 C41 120.4(6) . . ? C42 C43 C44 120.6(6) . . ? C43 C44 C45 119.4(8) . . ? C40 C45 C44 119.9(6) . . ? C51 C46 C47 119.1(7) . . ? C51 C46 P2 119.4(5) . . ? C47 C46 P2 121.4(5) . . ? C48 C47 C46 120.4(7) . . ? C49 C48 C47 120.1(8) . . ? C50 C49 C48 120.1(8) . . ? C49 C50 C51 120.7(8) . . ? C46 C51 C50 119.6(7) . . ? N4 C52 C53 178.8(13) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 1.754 _refine_diff_density_min -1.395 _refine_diff_density_rms 0.204 #################### Material relevant to compound 4 at 150K ############ data_4moins_abmerge _database_code_CSD 187002 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(PPh4)4 Re6S8(CN)6 (CH3CN)2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H86 N8 P4 Re6 S8' _chemical_formula_weight 2969.39 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' 'P' 'P' 0.1023 0.0942 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4120(18) _cell_length_b 13.0464(16) _cell_length_c 16.699(2) _cell_angle_alpha 109.451(14) _cell_angle_beta 95.717(16) _cell_angle_gamma 102.070(16) _cell_volume 2451.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.5390 _exptl_crystal_size_mid 0.4236 _exptl_crystal_size_min 0.0770 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 7.667 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0464 _exptl_absorpt_correction_T_max 0.5597 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, Phi. incr. == 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24095 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.87 _reflns_number_total 8855 _reflns_number_gt 6557 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE, [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0094P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00061(4) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8855 _refine_ls_number_parameters 592 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0514 _refine_ls_wR_factor_gt 0.0480 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.004 _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 0.38110(2) 0.064785(19) 0.014901(13) 0.01041(6) Uani 1 1 d . . . Re2 Re 0.46358(2) -0.065979(19) 0.079087(13) 0.01049(6) Uani 1 1 d . . . Re3 Re 0.59147(2) 0.124868(18) 0.088008(13) 0.01033(6) Uani 1 1 d . . . S1 S 0.27310(13) -0.11581(12) 0.00549(9) 0.0152(3) Uani 1 1 d . . . S2 S 0.33912(13) 0.00454(12) -0.13984(9) 0.0147(3) Uani 1 1 d . . . S3 S 0.50939(13) 0.23544(12) 0.02248(9) 0.0152(3) Uani 1 1 d . . . S4 S 0.44104(13) 0.11289(12) 0.16730(8) 0.0148(3) Uani 1 1 d . . . C1 C 0.2432(5) 0.1455(5) 0.0296(3) 0.0178(14) Uani 1 1 d . . . C2 C 0.4257(5) -0.1422(5) 0.1736(3) 0.0116(12) Uani 1 1 d . . . C3 C 0.6957(5) 0.2732(5) 0.1909(4) 0.0182(13) Uiso 1 1 d . . . N1 N 0.1770(5) 0.1893(4) 0.0390(3) 0.0207(12) Uani 1 1 d . . . N2 N 0.4077(5) -0.1757(5) 0.2238(3) 0.0283(14) Uani 1 1 d . . . N3 N 0.7476(4) 0.3492(4) 0.2438(3) 0.0225(12) Uani 1 1 d . . . P1 P 0.00857(13) -0.27272(13) 0.20888(9) 0.0133(3) Uani 1 1 d . . . C4 C -0.1420(5) -0.3176(5) 0.1822(3) 0.0168(14) Uani 1 1 d . . . C5 C -0.2043(5) -0.2551(5) 0.1519(3) 0.0165(13) Uani 1 1 d . . . H5 H -0.1687 -0.1861 0.1498 0.020 Uiso 1 1 calc R . . C6 C -0.3177(5) -0.2971(5) 0.1254(4) 0.0189(14) Uani 1 1 d . . . H6 H -0.3588 -0.2569 0.1038 0.023 Uiso 1 1 calc R . . C7 C -0.3722(5) -0.3978(6) 0.1302(4) 0.0234(15) Uani 1 1 d . . . H7 H -0.4495 -0.4247 0.1120 0.028 Uiso 1 1 calc R . . C8 C -0.3134(5) -0.4584(5) 0.1616(4) 0.0190(14) Uani 1 1 d . . . H8 H -0.3509 -0.5260 0.1650 0.023 Uiso 1 1 calc R . . C9 C -0.1979(5) -0.4191(5) 0.1883(3) 0.0140(12) Uani 1 1 d . . . H9 H -0.1580 -0.4599 0.2101 0.017 Uiso 1 1 calc R . . C10 C 0.0537(5) -0.2703(5) 0.3148(3) 0.0145(13) Uani 1 1 d . . . C11 C -0.0164(5) -0.2614(5) 0.3755(4) 0.0161(13) Uani 1 1 d . . . H11 H -0.0898 -0.2588 0.3607 0.019 Uiso 1 1 calc R . . C12 C 0.0216(5) -0.2566(5) 0.4564(4) 0.0206(14) Uani 1 1 d . . . H12 H -0.0272 -0.2546 0.4953 0.025 Uiso 1 1 calc R . . C13 C 0.1316(6) -0.2548(5) 0.4813(4) 0.0214(14) Uani 1 1 d . . . H13 H 0.1573 -0.2494 0.5372 0.026 Uiso 1 1 calc R . . C14 C 0.2037(6) -0.2610(6) 0.4224(4) 0.0261(16) Uani 1 1 d . . . H14 H 0.2779 -0.2601 0.4387 0.031 Uiso 1 1 calc R . . C15 C 0.1655(5) -0.2684(6) 0.3395(4) 0.0231(15) Uani 1 1 d . . . H15 H 0.2139 -0.2720 0.3002 0.028 Uiso 1 1 calc R . . C16 C 0.0628(5) -0.1348(5) 0.2062(4) 0.0156(13) Uani 1 1 d . . . C17 C 0.1403(5) -0.0540(5) 0.2764(4) 0.0220(14) Uani 1 1 d . . . H17 H 0.1579 -0.0674 0.3268 0.026 Uiso 1 1 calc R . . C18 C 0.1909(6) 0.0479(6) 0.2687(4) 0.0263(15) Uani 1 1 d . . . H18 H 0.2442 0.1025 0.3142 0.032 Uiso 1 1 calc R . . C19 C 0.1630(6) 0.0681(5) 0.1947(4) 0.0250(15) Uani 1 1 d . . . H19 H 0.1973 0.1362 0.1904 0.030 Uiso 1 1 calc R . . C20 C 0.0841(5) -0.0121(5) 0.1266(4) 0.0214(14) Uani 1 1 d . . . H20 H 0.0637 0.0034 0.0776 0.026 Uiso 1 1 calc R . . C21 C 0.0351(5) -0.1152(5) 0.1306(4) 0.0187(13) Uani 1 1 d . . . H21 H -0.0155 -0.1705 0.0836 0.022 Uiso 1 1 calc R . . C22 C 0.0731(5) -0.3687(5) 0.1358(3) 0.0145(13) Uani 1 1 d . . . C23 C 0.1554(5) -0.3265(5) 0.0966(4) 0.0193(14) Uani 1 1 d . . . H23 H 0.1740 -0.2506 0.1041 0.023 Uiso 1 1 calc R . . C24 C 0.2100(6) -0.3999(6) 0.0455(4) 0.0245(15) Uani 1 1 d . . . H24 H 0.2659 -0.3722 0.0192 0.029 Uiso 1 1 calc R . . C25 C 0.1826(6) -0.5119(6) 0.0332(4) 0.0227(15) Uani 1 1 d . . . H25 H 0.2199 -0.5597 -0.0010 0.027 Uiso 1 1 calc R . . C26 C 0.0994(6) -0.5542(5) 0.0718(4) 0.0237(15) Uani 1 1 d . . . H26 H 0.0809 -0.6302 0.0639 0.028 Uiso 1 1 calc R . . C27 C 0.0440(6) -0.4829(5) 0.1221(4) 0.0214(15) Uani 1 1 d . . . H27 H -0.0131 -0.5114 0.1471 0.026 Uiso 1 1 calc R . . P2 P 0.39906(13) 0.30917(12) 0.55759(9) 0.0134(3) Uani 1 1 d . . . C28 C 0.4798(5) 0.2424(5) 0.4821(3) 0.0150(13) Uani 1 1 d . . . C29 C 0.5589(5) 0.3092(5) 0.4542(4) 0.0158(13) Uani 1 1 d . . . H29 H 0.5723 0.3872 0.4769 0.019 Uiso 1 1 calc R . . C30 C 0.6170(5) 0.2589(6) 0.3927(4) 0.0217(15) Uani 1 1 d . . . H30 H 0.6683 0.3030 0.3727 0.026 Uiso 1 1 calc R . . C31 C 0.5997(6) 0.1443(6) 0.3610(4) 0.0263(17) Uani 1 1 d . . . H31 H 0.6393 0.1114 0.3195 0.032 Uiso 1 1 calc R . . C32 C 0.5246(6) 0.0773(6) 0.3898(4) 0.0277(16) Uani 1 1 d . . . H32 H 0.5150 -0.0002 0.3693 0.033 Uiso 1 1 calc R . . C33 C 0.4631(6) 0.1271(5) 0.4499(4) 0.0220(15) Uani 1 1 d . . . H33 H 0.4105 0.0824 0.4685 0.026 Uiso 1 1 calc R . . C34 C 0.3068(5) 0.2006(5) 0.5799(4) 0.0177(14) Uani 1 1 d . . . C35 C 0.3279(5) 0.1793(5) 0.6560(4) 0.0207(14) Uani 1 1 d . . . H35 H 0.3885 0.2261 0.6993 0.025 Uiso 1 1 calc R . . C36 C 0.2597(6) 0.0897(5) 0.6669(4) 0.0273(16) Uani 1 1 d . . . H36 H 0.2736 0.0760 0.7176 0.033 Uiso 1 1 calc R . . C37 C 0.1703(6) 0.0198(6) 0.6026(4) 0.0271(16) Uani 1 1 d . . . H37 H 0.1237 -0.0409 0.6100 0.033 Uiso 1 1 calc R . . C38 C 0.1504(6) 0.0405(6) 0.5267(4) 0.0283(16) Uani 1 1 d . . . H38 H 0.0914 -0.0078 0.4826 0.034 Uiso 1 1 calc R . . C39 C 0.2164(5) 0.1306(5) 0.5166(4) 0.0200(14) Uani 1 1 d . . . H39 H 0.2006 0.1453 0.4665 0.024 Uiso 1 1 calc R . . C40 C 0.4921(5) 0.4085(5) 0.6532(3) 0.0140(13) Uani 1 1 d . . . C41 C 0.4860(5) 0.5200(5) 0.6895(4) 0.0190(14) Uani 1 1 d . . . H41 H 0.4330 0.5456 0.6635 0.023 Uiso 1 1 calc R . . C42 C 0.5601(6) 0.5922(5) 0.7649(4) 0.0211(15) Uani 1 1 d . . . H42 H 0.5577 0.6668 0.7886 0.025 Uiso 1 1 calc R . . C43 C 0.6373(5) 0.5539(5) 0.8051(4) 0.0220(15) Uani 1 1 d . . . H43 H 0.6851 0.6022 0.8564 0.026 Uiso 1 1 calc R . . C44 C 0.6434(6) 0.4438(6) 0.7690(4) 0.0265(16) Uani 1 1 d . . . H44 H 0.6956 0.4182 0.7959 0.032 Uiso 1 1 calc R . . C45 C 0.5717(6) 0.3712(5) 0.6928(4) 0.0231(15) Uani 1 1 d . . . H45 H 0.5770 0.2976 0.6681 0.028 Uiso 1 1 calc R . . C46 C 0.3122(5) 0.3741(5) 0.5081(4) 0.0182(13) Uani 1 1 d . . . C47 C 0.3087(5) 0.3646(5) 0.4228(4) 0.0185(13) Uani 1 1 d . . . H47 H 0.3552 0.3275 0.3905 0.022 Uiso 1 1 calc R . . C48 C 0.2362(6) 0.4100(6) 0.3858(5) 0.0345(18) Uani 1 1 d . . . H48 H 0.2338 0.4028 0.3283 0.041 Uiso 1 1 calc R . . C49 C 0.1678(6) 0.4656(6) 0.4326(5) 0.0358(18) Uani 1 1 d . . . H49 H 0.1185 0.4951 0.4067 0.043 Uiso 1 1 calc R . . C50 C 0.1717(6) 0.4780(6) 0.5181(5) 0.0320(17) Uani 1 1 d . . . H50 H 0.1263 0.5173 0.5500 0.038 Uiso 1 1 calc R . . C51 C 0.2437(5) 0.4318(5) 0.5574(4) 0.0222(15) Uani 1 1 d . . . H51 H 0.2460 0.4392 0.6149 0.027 Uiso 1 1 calc R . . N4 N 0.9614(7) 0.1937(7) 0.3273(5) 0.064(2) Uani 1 1 d . . . C52 C 0.9597(7) 0.2024(8) 0.2624(5) 0.048(2) Uani 1 1 d . . . C53 C 0.9564(8) 0.2124(9) 0.1788(6) 0.061(3) Uani 1 1 d . . . H53A H 0.9078 0.1453 0.1357 0.091 Uiso 1 1 calc R . . H53B H 1.0306 0.2226 0.1656 0.091 Uiso 1 1 calc R . . H53C H 0.9287 0.2760 0.1795 0.091 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 Re1 0.01259(13) 0.01047(12) 0.01061(10) 0.00530(9) 0.00252(9) 0.00548(9) Re2 0.01367(13) 0.01003(12) 0.01013(10) 0.00583(9) 0.00237(9) 0.00437(9) Re3 0.01302(13) 0.00931(12) 0.01017(11) 0.00472(9) 0.00193(9) 0.00417(9) S1 0.0162(8) 0.0141(7) 0.0159(6) 0.0068(6) 0.0033(6) 0.0028(6) S2 0.0191(8) 0.0142(7) 0.0129(6) 0.0061(6) 0.0018(6) 0.0074(6) S3 0.0232(9) 0.0105(7) 0.0152(6) 0.0070(6) 0.0028(6) 0.0074(6) S4 0.0218(9) 0.0139(7) 0.0111(6) 0.0053(6) 0.0048(6) 0.0079(6) C1 0.028(4) 0.007(3) 0.011(3) 0.002(2) 0.005(3) -0.008(3) C2 0.008(3) 0.013(3) 0.006(2) -0.004(2) -0.001(2) 0.001(2) N1 0.024(3) 0.021(3) 0.021(3) 0.010(2) 0.009(2) 0.008(2) N2 0.031(4) 0.022(3) 0.025(3) 0.006(3) -0.002(3) 0.000(3) N3 0.019(3) 0.025(3) 0.025(3) 0.013(2) 0.004(2) 0.003(2) P1 0.0132(8) 0.0152(8) 0.0123(7) 0.0057(6) 0.0011(6) 0.0044(6) C4 0.016(3) 0.026(3) 0.008(2) 0.001(2) 0.001(2) 0.014(3) C5 0.020(3) 0.019(3) 0.012(3) 0.005(2) 0.006(2) 0.010(3) C6 0.016(3) 0.024(3) 0.028(3) 0.018(3) 0.008(3) 0.013(3) C7 0.006(3) 0.035(4) 0.027(3) 0.007(3) 0.002(3) 0.006(3) C8 0.025(4) 0.014(3) 0.019(3) 0.009(3) 0.005(3) 0.001(3) C9 0.018(3) 0.014(3) 0.017(3) 0.012(2) 0.006(2) 0.007(3) C10 0.017(3) 0.016(3) 0.011(3) 0.005(2) 0.002(2) 0.007(2) C11 0.010(3) 0.018(3) 0.021(3) 0.011(3) -0.003(2) 0.002(2) C12 0.024(4) 0.023(3) 0.016(3) 0.009(3) 0.008(3) 0.002(3) C13 0.030(4) 0.024(3) 0.013(3) 0.010(3) 0.000(3) 0.009(3) C14 0.021(4) 0.039(4) 0.024(3) 0.016(3) -0.001(3) 0.016(3) C15 0.013(3) 0.032(4) 0.024(3) 0.008(3) 0.000(3) 0.011(3) C16 0.011(3) 0.016(3) 0.019(3) 0.005(3) 0.006(2) 0.003(2) C17 0.024(4) 0.023(3) 0.016(3) 0.007(3) 0.001(3) 0.001(3) C18 0.024(4) 0.023(4) 0.022(3) 0.004(3) -0.002(3) -0.004(3) C19 0.025(4) 0.019(3) 0.031(3) 0.010(3) 0.010(3) 0.003(3) C20 0.016(3) 0.027(4) 0.022(3) 0.009(3) 0.004(3) 0.008(3) C21 0.017(3) 0.020(3) 0.020(3) 0.007(3) 0.002(2) 0.006(3) C22 0.011(3) 0.019(3) 0.011(2) 0.005(2) -0.001(2) 0.001(2) C23 0.016(3) 0.021(3) 0.017(3) 0.006(3) 0.002(3) -0.001(3) C24 0.020(4) 0.028(4) 0.025(3) 0.010(3) 0.009(3) 0.005(3) C25 0.026(4) 0.028(4) 0.011(3) 0.001(3) 0.002(3) 0.011(3) C26 0.025(4) 0.015(3) 0.024(3) 0.002(3) -0.006(3) 0.005(3) C27 0.026(4) 0.021(3) 0.019(3) 0.007(3) 0.003(3) 0.010(3) P2 0.0131(8) 0.0123(7) 0.0141(7) 0.0049(6) 0.0018(6) 0.0022(6) C28 0.012(3) 0.022(3) 0.009(2) 0.002(2) 0.000(2) 0.008(3) C29 0.008(3) 0.016(3) 0.024(3) 0.010(3) 0.001(2) 0.002(2) C30 0.015(3) 0.039(4) 0.015(3) 0.014(3) 0.006(2) 0.006(3) C31 0.031(4) 0.041(4) 0.008(3) 0.005(3) 0.003(3) 0.018(3) C32 0.036(4) 0.017(3) 0.022(3) -0.003(3) 0.002(3) 0.006(3) C33 0.023(4) 0.013(3) 0.026(3) 0.006(3) -0.001(3) 0.001(3) C34 0.017(3) 0.016(3) 0.023(3) 0.008(3) 0.009(3) 0.006(3) C35 0.018(3) 0.018(3) 0.025(3) 0.006(3) 0.007(3) 0.003(3) C36 0.040(5) 0.016(3) 0.031(3) 0.012(3) 0.012(3) 0.009(3) C37 0.025(4) 0.023(4) 0.035(4) 0.010(3) 0.019(3) 0.003(3) C38 0.021(4) 0.030(4) 0.027(3) 0.004(3) 0.005(3) 0.001(3) C39 0.021(4) 0.019(3) 0.023(3) 0.009(3) 0.006(3) 0.006(3) C40 0.017(3) 0.011(3) 0.012(3) 0.003(2) 0.005(2) -0.001(2) C41 0.024(4) 0.014(3) 0.023(3) 0.010(3) 0.003(3) 0.007(3) C42 0.030(4) 0.010(3) 0.020(3) 0.000(3) 0.009(3) 0.005(3) C43 0.021(4) 0.023(4) 0.017(3) 0.004(3) 0.000(3) 0.004(3) C44 0.020(4) 0.030(4) 0.024(3) 0.003(3) -0.002(3) 0.007(3) C45 0.033(4) 0.014(3) 0.019(3) -0.003(3) 0.002(3) 0.012(3) C46 0.021(4) 0.008(3) 0.022(3) 0.007(3) -0.002(3) -0.002(3) C47 0.013(3) 0.020(3) 0.022(3) 0.011(3) 0.001(2) -0.003(3) C48 0.032(4) 0.043(5) 0.036(4) 0.026(4) 0.004(3) 0.008(4) C49 0.019(4) 0.042(5) 0.061(5) 0.039(4) 0.001(3) 0.008(3) C50 0.019(4) 0.030(4) 0.056(5) 0.025(4) 0.008(3) 0.008(3) C51 0.023(4) 0.014(3) 0.030(3) 0.010(3) 0.007(3) 0.001(3) N4 0.075(6) 0.075(6) 0.041(4) 0.024(4) 0.027(4) 0.005(5) C52 0.039(5) 0.053(5) 0.048(5) 0.017(4) 0.015(4) 0.004(4) C53 0.051(6) 0.098(8) 0.071(6) 0.059(6) 0.029(5) 0.044(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 Re1 C1 2.183(7) . ? Re1 S1 2.4007(16) . ? Re1 S2 2.4029(14) . ? Re1 S4 2.4059(14) . ? Re1 S3 2.4079(17) . ? Re1 Re2 2.6052(5) 2_655 ? Re1 Re3 2.6066(6) . ? Re1 Re3 2.6131(5) 2_655 ? Re1 Re2 2.6148(5) . ? Re1 Re1 3.6928(7) 2_655 ? Re2 C2 2.167(6) . ? Re2 S4 2.3999(14) . ? Re2 S1 2.4018(17) . ? Re2 S3 2.4090(13) 2_655 ? Re2 S2 2.4106(17) 2_655 ? Re2 Re1 2.6052(5) 2_655 ? Re2 Re3 2.6066(6) . ? Re2 Re3 2.6108(5) 2_655 ? Re2 Re2 3.6894(7) 2_655 ? Re3 C3 2.161(6) . ? Re3 S3 2.4000(15) . ? Re3 S1 2.4001(14) 2_655 ? Re3 S4 2.4025(15) . ? Re3 S2 2.4029(16) 2_655 ? Re3 Re2 2.6108(5) 2_655 ? Re3 Re1 2.6131(5) 2_655 ? Re3 Re3 3.6891(11) 2_655 ? S1 Re3 2.4001(14) 2_655 ? S2 Re3 2.4031(16) 2_655 ? S2 Re2 2.4107(17) 2_655 ? S3 Re2 2.4090(13) 2_655 ? C1 N1 1.090(8) . ? C2 N2 1.088(8) . ? C3 N3 1.102(8) . ? P1 C10 1.790(6) . ? P1 C4 1.799(6) . ? P1 C16 1.802(6) . ? P1 C22 1.816(5) . ? C4 C9 1.403(9) . ? C4 C5 1.407(8) . ? C5 C6 1.367(9) . ? C6 C7 1.379(9) . ? C7 C8 1.368(9) . ? C8 C9 1.390(8) . ? C10 C11 1.391(7) . ? C10 C15 1.399(8) . ? C11 C12 1.363(8) . ? C12 C13 1.380(9) . ? C13 C14 1.389(8) . ? C14 C15 1.383(9) . ? C16 C17 1.392(8) . ? C16 C21 1.394(8) . ? C17 C18 1.400(9) . ? C18 C19 1.374(9) . ? C19 C20 1.379(9) . ? C20 C21 1.382(9) . ? C22 C23 1.383(8) . ? C22 C27 1.391(9) . ? C23 C24 1.395(8) . ? C24 C25 1.369(9) . ? C25 C26 1.384(9) . ? C26 C27 1.381(8) . ? P2 C40 1.787(6) . ? P2 C34 1.793(6) . ? P2 C46 1.799(7) . ? P2 C28 1.800(5) . ? C28 C33 1.379(8) . ? C28 C29 1.394(8) . ? C29 C30 1.380(7) . ? C30 C31 1.370(9) . ? C31 C32 1.376(10) . ? C32 C33 1.393(8) . ? C34 C39 1.380(9) . ? C34 C35 1.400(9) . ? C35 C36 1.369(9) . ? C36 C37 1.379(10) . ? C37 C38 1.391(10) . ? C38 C39 1.356(9) . ? C40 C45 1.391(9) . ? C40 C41 1.399(8) . ? C41 C42 1.391(9) . ? C42 C43 1.383(9) . ? C43 C44 1.382(9) . ? C44 C45 1.388(9) . ? C46 C47 1.383(8) . ? C46 C51 1.399(8) . ? C47 C48 1.378(10) . ? C48 C49 1.368(9) . ? C49 C50 1.377(10) . ? C50 C51 1.402(10) . ? N4 C52 1.126(11) . ? C52 C53 1.442(12) . ? 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 C1 Re1 S1 95.70(16) . . ? C1 Re1 S2 92.13(15) . . ? S1 Re1 S2 89.43(6) . . ? C1 Re1 S4 94.97(15) . . ? S1 Re1 S4 89.53(6) . . ? S2 Re1 S4 172.90(5) . . ? C1 Re1 S3 91.61(16) . . ? S1 Re1 S3 172.70(5) . . ? S2 Re1 S3 90.37(5) . . ? S4 Re1 S3 89.78(6) . . ? C1 Re1 Re2 132.66(15) . 2_655 ? S1 Re1 Re2 116.90(4) . 2_655 ? S2 Re1 Re2 57.38(4) . 2_655 ? S4 Re1 Re2 117.18(4) . 2_655 ? S3 Re1 Re2 57.28(3) . 2_655 ? C1 Re1 Re3 134.48(15) . . ? S1 Re1 Re3 116.89(4) . . ? S2 Re1 Re3 117.45(4) . . ? S4 Re1 Re3 57.11(4) . . ? S3 Re1 Re3 57.02(4) . . ? Re2 Re1 Re3 60.123(14) 2_655 . ? C1 Re1 Re3 135.49(15) . 2_655 ? S1 Re1 Re3 57.01(3) . 2_655 ? S2 Re1 Re3 57.07(4) . 2_655 ? S4 Re1 Re3 116.81(4) . 2_655 ? S3 Re1 Re3 117.16(4) . 2_655 ? Re2 Re1 Re3 59.935(17) 2_655 2_655 ? Re3 Re1 Re3 89.94(2) . 2_655 ? C1 Re1 Re2 137.39(15) . . ? S1 Re1 Re2 57.03(4) . . ? S2 Re1 Re2 116.96(4) . . ? S4 Re1 Re2 56.93(4) . . ? S3 Re1 Re2 116.88(4) . . ? Re2 Re1 Re2 89.948(15) 2_655 . ? Re3 Re1 Re2 59.896(15) . . ? Re3 Re1 Re2 59.919(14) 2_655 . ? C1 Re1 Re1 177.70(15) . 2_655 ? S1 Re1 Re1 86.21(4) . 2_655 ? S2 Re1 Re1 86.60(4) . 2_655 ? S4 Re1 Re1 86.32(4) . 2_655 ? S3 Re1 Re1 86.49(4) . 2_655 ? Re2 Re1 Re1 45.079(11) 2_655 2_655 ? Re3 Re1 Re1 45.042(12) . 2_655 ? Re3 Re1 Re1 44.900(16) 2_655 2_655 ? Re2 Re1 Re1 44.869(11) . 2_655 ? C2 Re2 S4 93.51(13) . . ? C2 Re2 S1 95.39(15) . . ? S4 Re2 S1 89.64(5) . . ? C2 Re2 S3 93.47(13) . 2_655 ? S4 Re2 S3 173.02(5) . 2_655 ? S1 Re2 S3 89.49(5) . 2_655 ? C2 Re2 S2 92.00(15) . 2_655 ? S4 Re2 S2 89.81(5) . 2_655 ? S1 Re2 S2 172.62(5) . 2_655 ? S3 Re2 S2 90.16(5) 2_655 2_655 ? C2 Re2 Re1 133.70(14) . 2_655 ? S4 Re2 Re1 117.32(4) . 2_655 ? S1 Re2 Re1 116.96(4) . 2_655 ? S3 Re2 Re1 57.24(4) 2_655 2_655 ? S2 Re2 Re1 57.09(3) 2_655 2_655 ? C2 Re2 Re3 133.84(14) . . ? S4 Re2 Re3 57.18(4) . . ? S1 Re2 Re3 116.85(4) . . ? S3 Re2 Re3 117.36(4) 2_655 . ? S2 Re2 Re3 57.07(4) 2_655 . ? Re1 Re2 Re3 60.183(15) 2_655 . ? C2 Re2 Re3 136.14(14) . 2_655 ? S4 Re2 Re3 117.12(4) . 2_655 ? S1 Re2 Re3 57.03(4) . 2_655 ? S3 Re2 Re3 56.95(4) 2_655 2_655 ? S2 Re2 Re3 117.00(4) 2_655 2_655 ? Re1 Re2 Re3 59.965(16) 2_655 2_655 ? Re3 Re2 Re3 89.99(2) . 2_655 ? C2 Re2 Re1 136.23(14) . . ? S4 Re2 Re1 57.15(4) . . ? S1 Re2 Re1 56.99(4) . . ? S3 Re2 Re1 116.93(4) 2_655 . ? S2 Re2 Re1 116.92(4) 2_655 . ? Re1 Re2 Re1 90.052(15) 2_655 . ? Re3 Re2 Re1 59.897(15) . . ? Re3 Re2 Re1 60.009(14) 2_655 . ? C2 Re2 Re2 178.40(14) . 2_655 ? S4 Re2 Re2 86.54(4) . 2_655 ? S1 Re2 Re2 86.22(4) . 2_655 ? S3 Re2 Re2 86.49(4) 2_655 2_655 ? S2 Re2 Re2 86.40(4) 2_655 2_655 ? Re1 Re2 Re2 45.131(11) 2_655 2_655 ? Re3 Re2 Re2 45.043(14) . 2_655 ? Re3 Re2 Re2 44.952(14) 2_655 2_655 ? Re1 Re2 Re2 44.921(11) . 2_655 ? C3 Re3 S3 92.11(17) . . ? C3 Re3 S1 94.40(15) . 2_655 ? S3 Re3 S1 89.75(5) . 2_655 ? C3 Re3 S4 92.87(15) . . ? S3 Re3 S4 90.05(5) . . ? S1 Re3 S4 172.73(5) 2_655 . ? C3 Re3 S2 94.50(17) . 2_655 ? S3 Re3 S2 173.39(5) . 2_655 ? S1 Re3 S2 89.44(5) 2_655 2_655 ? S4 Re3 S2 89.93(5) . 2_655 ? C3 Re3 Re2 135.26(16) . . ? S3 Re3 Re2 117.48(4) . . ? S1 Re3 Re2 116.87(4) 2_655 . ? S4 Re3 Re2 57.08(4) . . ? S2 Re3 Re2 57.36(4) 2_655 . ? C3 Re3 Re1 133.63(16) . . ? S3 Re3 Re1 57.32(4) . . ? S1 Re3 Re1 116.96(4) 2_655 . ? S4 Re3 Re1 57.24(4) . . ? S2 Re3 Re1 117.52(4) 2_655 . ? Re2 Re3 Re1 60.208(17) . . ? C3 Re3 Re2 134.70(17) . 2_655 ? S3 Re3 Re2 57.29(3) . 2_655 ? S1 Re3 Re2 57.09(4) 2_655 2_655 ? S4 Re3 Re2 117.09(4) . 2_655 ? S2 Re3 Re2 117.10(3) 2_655 2_655 ? Re2 Re3 Re2 90.01(2) . 2_655 ? Re1 Re3 Re2 59.911(18) . 2_655 ? C3 Re3 Re1 136.31(16) . 2_655 ? S3 Re3 Re1 117.33(3) . 2_655 ? S1 Re3 Re1 57.03(4) 2_655 2_655 ? S4 Re3 Re1 116.92(4) . 2_655 ? S2 Re3 Re1 57.06(3) 2_655 2_655 ? Re2 Re3 Re1 59.882(15) . 2_655 ? Re1 Re3 Re1 90.06(2) . 2_655 ? Re2 Re3 Re1 60.072(15) 2_655 2_655 ? C3 Re3 Re3 178.69(16) . 2_655 ? S3 Re3 Re3 86.77(4) . 2_655 ? S1 Re3 Re3 86.27(4) 2_655 2_655 ? S4 Re3 Re3 86.46(4) . 2_655 ? S2 Re3 Re3 86.63(4) 2_655 2_655 ? Re2 Re3 Re3 45.048(14) . 2_655 ? Re1 Re3 Re3 45.100(16) . 2_655 ? Re2 Re3 Re3 44.957(14) 2_655 2_655 ? Re1 Re3 Re3 44.957(13) 2_655 2_655 ? Re3 S1 Re1 65.95(4) 2_655 . ? Re3 S1 Re2 65.87(4) 2_655 . ? Re1 S1 Re2 65.98(4) . . ? Re1 S2 Re3 65.87(4) . 2_655 ? Re1 S2 Re2 65.53(4) . 2_655 ? Re3 S2 Re2 65.57(4) 2_655 2_655 ? Re3 S3 Re1 65.66(4) . . ? Re3 S3 Re2 65.76(4) . 2_655 ? Re1 S3 Re2 65.48(4) . 2_655 ? Re2 S4 Re3 65.74(4) . . ? Re2 S4 Re1 65.93(4) . . ? Re3 S4 Re1 65.65(4) . . ? N1 C1 Re1 177.4(6) . . ? N2 C2 Re2 176.8(5) . . ? N3 C3 Re3 179.0(5) . . ? C10 P1 C4 109.4(3) . . ? C10 P1 C16 108.7(3) . . ? C4 P1 C16 112.2(3) . . ? C10 P1 C22 106.7(3) . . ? C4 P1 C22 112.0(3) . . ? C16 P1 C22 107.6(3) . . ? C9 C4 C5 119.4(6) . . ? C9 C4 P1 119.3(4) . . ? C5 C4 P1 121.2(5) . . ? C6 C5 C4 119.3(6) . . ? C5 C6 C7 121.1(6) . . ? C8 C7 C6 120.4(6) . . ? C7 C8 C9 120.2(6) . . ? C8 C9 C4 119.6(5) . . ? C11 C10 C15 119.0(5) . . ? C11 C10 P1 121.9(5) . . ? C15 C10 P1 118.8(4) . . ? C12 C11 C10 120.4(6) . . ? C11 C12 C13 120.9(5) . . ? C12 C13 C14 119.5(6) . . ? C15 C14 C13 120.1(6) . . ? C14 C15 C10 119.9(5) . . ? C17 C16 C21 121.5(6) . . ? C17 C16 P1 119.1(5) . . ? C21 C16 P1 119.1(5) . . ? C16 C17 C18 118.0(6) . . ? C19 C18 C17 120.8(6) . . ? C18 C19 C20 120.3(6) . . ? C19 C20 C21 120.6(6) . . ? C20 C21 C16 118.8(6) . . ? C23 C22 C27 120.1(5) . . ? C23 C22 P1 119.3(5) . . ? C27 C22 P1 120.5(4) . . ? C22 C23 C24 118.8(6) . . ? C25 C24 C23 121.1(6) . . ? C24 C25 C26 120.0(5) . . ? C27 C26 C25 119.6(6) . . ? C26 C27 C22 120.4(6) . . ? C40 P2 C34 111.6(3) . . ? C40 P2 C46 112.1(3) . . ? C34 P2 C46 106.9(3) . . ? C40 P2 C28 109.1(3) . . ? C34 P2 C28 107.3(3) . . ? C46 P2 C28 109.6(3) . . ? C33 C28 C29 119.7(5) . . ? C33 C28 P2 121.5(5) . . ? C29 C28 P2 118.8(4) . . ? C30 C29 C28 119.5(6) . . ? C31 C30 C29 120.3(6) . . ? C30 C31 C32 120.9(5) . . ? C31 C32 C33 119.1(6) . . ? C28 C33 C32 120.3(6) . . ? C39 C34 C35 119.2(6) . . ? C39 C34 P2 118.2(5) . . ? C35 C34 P2 122.5(5) . . ? C36 C35 C34 120.1(6) . . ? C35 C36 C37 120.0(7) . . ? C36 C37 C38 119.7(7) . . ? C39 C38 C37 120.4(6) . . ? C38 C39 C34 120.6(6) . . ? C45 C40 C41 119.8(5) . . ? C45 C40 P2 117.7(4) . . ? C41 C40 P2 122.4(5) . . ? C42 C41 C40 119.2(6) . . ? C43 C42 C41 120.7(5) . . ? C44 C43 C42 119.9(6) . . ? C43 C44 C45 120.2(6) . . ? C44 C45 C40 120.1(5) . . ? C47 C46 C51 120.1(6) . . ? C47 C46 P2 121.7(4) . . ? C51 C46 P2 118.1(5) . . ? C48 C47 C46 120.0(6) . . ? C49 C48 C47 120.8(6) . . ? C48 C49 C50 120.0(7) . . ? C49 C50 C51 120.5(6) . . ? C46 C51 C50 118.5(6) . . ? N4 C52 C53 179.3(12) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.87 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 1.235 _refine_diff_density_min -1.274 _refine_diff_density_rms 0.204 #################### Material relevant to compound 5 at 293K ############ data_cluster_abmerge _database_code_CSD 187003 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(PPh4)4 (Re6Se8(CN)6) (CH3CN)2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H86 N8 P4 Re6 Se8' _chemical_formula_weight 3344.59 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6001(13) _cell_length_b 13.1402(12) _cell_length_c 16.9448(18) _cell_angle_alpha 109.720(11) _cell_angle_beta 96.004(13) _cell_angle_gamma 101.447(12) _cell_volume 2543.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.6930 _exptl_crystal_size_mid 0.4259 _exptl_crystal_size_min 0.1924 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 10.087 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0251 _exptl_absorpt_correction_T_max 0.1759 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _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 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, Phi. incr. == 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25005 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.84 _reflns_number_total 9183 _reflns_number_gt 6003 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0363P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00091(5) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9183 _refine_ls_number_parameters 597 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _refine_ls_shift/su_max 0.001 _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 0.11970(3) 0.93621(2) 0.485089(19) 0.02403(9) Uani 1 1 d . . . Re2 Re 0.03563(3) 1.06814(2) 0.422406(19) 0.02401(9) Uani 1 1 d . . . Re3 Re -0.08926(3) 0.87508(2) 0.410794(19) 0.02376(9) Uani 1 1 d . . . Se1 Se 0.23394(7) 1.12376(7) 0.49712(5) 0.03055(19) Uani 1 1 d . . . Se2 Se 0.06412(7) 0.88650(6) 0.32683(5) 0.02898(19) Uani 1 1 d . . . Se3 Se -0.00626(7) 0.75451(6) 0.47447(5) 0.02984(19) Uani 1 1 d . . . Se4 Se 0.16694(7) 0.99418(7) 0.64482(5) 0.02964(19) Uani 1 1 d . . . C1 C 0.2529(7) 0.8588(7) 0.4693(6) 0.035(2) Uani 1 1 d . . . C2 C 0.0713(7) 1.1413(6) 0.3308(5) 0.0292(18) Uani 1 1 d . . . C3 C -0.1900(8) 0.7308(7) 0.3075(5) 0.035(2) Uani 1 1 d . . . N1 N 0.3221(7) 0.8136(7) 0.4589(6) 0.050(2) Uani 1 1 d . . . N2 N 0.0901(7) 1.1778(6) 0.2801(5) 0.052(2) Uani 1 1 d . . . N3 N -0.2403(7) 0.6548(6) 0.2524(5) 0.049(2) Uani 1 1 d . . . P1 P -0.10163(19) 0.30549(18) 0.05462(14) 0.0323(5) Uani 1 1 d . . . C4 C -0.0199(7) 0.2411(7) -0.0184(5) 0.035(2) Uani 1 1 d . . . C5 C 0.0582(8) 0.3072(9) -0.0431(6) 0.046(2) Uani 1 1 d . . . H5 H 0.0700 0.3844 -0.0195 0.055 Uiso 1 1 calc R . . C6 C 0.1194(8) 0.2604(9) -0.1025(6) 0.050(3) Uani 1 1 d . . . H6 H 0.1732 0.3046 -0.1189 0.060 Uiso 1 1 calc R . . C7 C 0.0973(9) 0.1456(11) -0.1363(6) 0.060(3) Uani 1 1 d . . . H7 H 0.1347 0.1119 -0.1783 0.072 Uiso 1 1 calc R . . C8 C 0.0241(10) 0.0813(9) -0.1108(7) 0.062(3) Uani 1 1 d . . . H8 H 0.0139 0.0043 -0.1335 0.075 Uiso 1 1 calc R . . C9 C -0.0366(9) 0.1264(8) -0.0517(6) 0.049(2) Uani 1 1 d . . . H9 H -0.0878 0.0808 -0.0345 0.058 Uiso 1 1 calc R . . C10 C -0.0106(7) 0.4045(6) 0.1501(5) 0.033(2) Uani 1 1 d . . . C11 C 0.0662(8) 0.3672(8) 0.1893(6) 0.047(2) Uani 1 1 d . . . H11 H 0.0724 0.2942 0.1650 0.056 Uiso 1 1 calc R . . C12 C 0.1342(9) 0.4394(8) 0.2654(7) 0.058(3) Uani 1 1 d . . . H12 H 0.1845 0.4139 0.2932 0.069 Uiso 1 1 calc R . . C13 C 0.1281(9) 0.5489(8) 0.3002(7) 0.057(3) Uani 1 1 d . . . H13 H 0.1755 0.5973 0.3506 0.069 Uiso 1 1 calc R . . C14 C 0.0533(9) 0.5859(7) 0.2611(6) 0.052(3) Uani 1 1 d . . . H14 H 0.0492 0.6596 0.2851 0.062 Uiso 1 1 calc R . . C15 C -0.0184(8) 0.5142(7) 0.1848(6) 0.042(2) Uani 1 1 d . . . H15 H -0.0700 0.5396 0.1582 0.051 Uiso 1 1 calc R . . C16 C -0.1862(7) 0.3698(7) 0.0043(6) 0.041(2) Uani 1 1 d . . . C17 C -0.1878(8) 0.3606(8) -0.0794(7) 0.051(3) Uani 1 1 d . . . H17 H -0.1408 0.3241 -0.1105 0.062 Uiso 1 1 calc R . . C20 C -0.3268(9) 0.4699(10) 0.0129(11) 0.080(4) Uani 1 1 d . . . H20 H -0.3740 0.5070 0.0433 0.095 Uiso 1 1 calc R . . C18 C -0.2593(10) 0.4056(10) -0.1173(9) 0.072(4) Uani 1 1 d . . . H18 H -0.2605 0.3992 -0.1738 0.086 Uiso 1 1 calc R . . C19 C -0.3278(11) 0.4591(11) -0.0716(11) 0.085(5) Uani 1 1 d . . . H19 H -0.3759 0.4889 -0.0974 0.102 Uiso 1 1 calc R . . C21 C -0.2574(8) 0.4267(9) 0.0513(8) 0.058(3) Uani 1 1 d . . . H21 H -0.2565 0.4343 0.1080 0.069 Uiso 1 1 calc R . . C22 C -0.1925(7) 0.1977(7) 0.0759(6) 0.034(2) Uani 1 1 d . . . C23 C -0.1734(9) 0.1793(8) 0.1508(6) 0.049(3) Uani 1 1 d . . . H23 H -0.1138 0.2252 0.1936 0.058 Uiso 1 1 calc R . . C24 C -0.2444(10) 0.0909(8) 0.1617(7) 0.056(3) Uani 1 1 d . . . H24 H -0.2334 0.0784 0.2125 0.067 Uiso 1 1 calc R . . C25 C -0.3308(10) 0.0225(9) 0.0968(8) 0.063(3) Uani 1 1 d . . . H25 H -0.3764 -0.0381 0.1031 0.075 Uiso 1 1 calc R . . C26 C -0.3504(9) 0.0425(8) 0.0233(7) 0.060(3) Uani 1 1 d . . . H26 H -0.4097 -0.0038 -0.0196 0.071 Uiso 1 1 calc R . . C27 C -0.2829(8) 0.1306(8) 0.0124(7) 0.049(3) Uani 1 1 d . . . H27 H -0.2975 0.1453 -0.0370 0.058 Uiso 1 1 calc R . . P2 P 0.49212(18) 1.27891(18) 0.29330(14) 0.0315(5) Uani 1 1 d . . . C28 C 0.6404(7) 1.3222(6) 0.3185(5) 0.0297(18) Uani 1 1 d . . . C29 C 0.7021(7) 1.2607(7) 0.3466(5) 0.036(2) Uani 1 1 d . . . H29 H 0.6671 1.1936 0.3504 0.043 Uiso 1 1 calc R . . C30 C 0.8160(8) 1.2988(8) 0.3692(6) 0.046(2) Uani 1 1 d . . . H30 H 0.8571 1.2564 0.3870 0.055 Uiso 1 1 calc R . . C31 C 0.8685(8) 1.3992(8) 0.3653(6) 0.047(2) Uani 1 1 d . . . H31 H 0.9445 1.4259 0.3825 0.057 Uiso 1 1 calc R . . C32 C 0.8080(8) 1.4595(8) 0.3359(6) 0.047(2) Uani 1 1 d . . . H32 H 0.8436 1.5264 0.3323 0.056 Uiso 1 1 calc R . . C33 C 0.6945(7) 1.4219(7) 0.3117(6) 0.041(2) Uani 1 1 d . . . H33 H 0.6544 1.4628 0.2910 0.049 Uiso 1 1 calc R . . C34 C 0.4305(7) 1.3752(7) 0.3645(5) 0.036(2) Uani 1 1 d . . . C35 C 0.3467(8) 1.3357(9) 0.4013(7) 0.052(3) Uani 1 1 d . . . H35 H 0.3271 1.2602 0.3930 0.062 Uiso 1 1 calc R . . C36 C 0.2912(9) 1.4083(10) 0.4509(7) 0.059(3) Uani 1 1 d . . . H36 H 0.2364 1.3815 0.4768 0.071 Uiso 1 1 calc R . . C37 C 0.3171(9) 1.5176(10) 0.4612(6) 0.061(3) Uani 1 1 d . . . H37 H 0.2779 1.5654 0.4919 0.073 Uiso 1 1 calc R . . C38 C 0.4024(10) 1.5580(9) 0.4257(7) 0.063(3) Uani 1 1 d . . . H38 H 0.4219 1.6337 0.4348 0.076 Uiso 1 1 calc R . . C39 C 0.4584(8) 1.4884(8) 0.3775(7) 0.052(3) Uani 1 1 d . . . H39 H 0.5149 1.5166 0.3536 0.063 Uiso 1 1 calc R . . C40 C 0.4470(7) 1.2737(7) 0.1875(5) 0.034(2) Uani 1 1 d . . . C41 C 0.3393(8) 1.2740(9) 0.1637(6) 0.051(3) Uani 1 1 d . . . H41 H 0.2928 1.2810 0.2033 0.061 Uiso 1 1 calc R . . C42 C 0.2996(10) 1.2640(10) 0.0815(7) 0.067(3) Uani 1 1 d . . . H42 H 0.2264 1.2629 0.0654 0.081 Uiso 1 1 calc R . . C43 C 0.3690(9) 1.2558(8) 0.0239(6) 0.051(3) Uani 1 1 d . . . H43 H 0.3434 1.2505 -0.0312 0.061 Uiso 1 1 calc R . . C44 C 0.4764(8) 1.2554(8) 0.0473(6) 0.050(3) Uani 1 1 d . . . H44 H 0.5234 1.2499 0.0081 0.060 Uiso 1 1 calc R . . C45 C 0.5147(7) 1.2631(7) 0.1291(5) 0.040(2) Uani 1 1 d . . . H45 H 0.5871 1.2611 0.1443 0.048 Uiso 1 1 calc R . . C46 C 0.4411(7) 1.1429(7) 0.2965(5) 0.0323(19) Uani 1 1 d . . . C47 C 0.3677(8) 1.0612(8) 0.2301(7) 0.051(3) Uani 1 1 d . . . H47 H 0.3492 1.0724 0.1796 0.061 Uiso 1 1 calc R . . C48 C 0.3204(9) 0.9611(9) 0.2378(7) 0.062(3) Uani 1 1 d . . . H48 H 0.2678 0.9065 0.1933 0.074 Uiso 1 1 calc R . . C49 C 0.3507(9) 0.9427(8) 0.3102(7) 0.052(3) Uani 1 1 d . . . H49 H 0.3199 0.8745 0.3140 0.063 Uiso 1 1 calc R . . C50 C 0.4259(9) 1.0230(8) 0.3776(7) 0.052(3) Uani 1 1 d . . . H50 H 0.4474 1.0090 0.4264 0.062 Uiso 1 1 calc R . . C51 C 0.4691(8) 1.1251(8) 0.3721(6) 0.043(2) Uani 1 1 d . . . H51 H 0.5168 1.1820 0.4186 0.052 Uiso 1 1 calc R . . C53 C 0.4596(12) 1.2033(14) 0.7726(10) 0.094(5) Uani 1 1 d . . . C52 C 0.4583(11) 1.2214(15) 0.6926(10) 0.117(6) Uani 1 1 d . . . H52A H 0.4021 1.2589 0.6853 0.176 Uiso 1 1 calc R . . H52B H 0.4433 1.1509 0.6461 0.176 Uiso 1 1 calc R . . H52C H 0.5287 1.2665 0.6933 0.176 Uiso 1 1 calc R . . N4 N 0.4632(14) 1.1894(13) 0.8331(9) 0.139(6) 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 Re1 0.02906(19) 0.02021(16) 0.02382(17) 0.00852(13) 0.00358(15) 0.00830(14) Re2 0.03127(19) 0.01927(16) 0.02239(17) 0.00923(13) 0.00339(14) 0.00635(14) Re3 0.02965(19) 0.01845(16) 0.02230(17) 0.00722(13) 0.00225(14) 0.00587(14) Se1 0.0317(5) 0.0279(4) 0.0320(4) 0.0123(4) 0.0069(4) 0.0044(4) Se2 0.0378(5) 0.0251(4) 0.0247(4) 0.0076(3) 0.0079(4) 0.0111(4) Se3 0.0406(5) 0.0189(4) 0.0301(4) 0.0097(3) 0.0027(4) 0.0084(4) Se4 0.0368(5) 0.0271(4) 0.0262(4) 0.0112(3) 0.0007(4) 0.0106(4) C1 0.037(5) 0.033(5) 0.039(5) 0.017(4) 0.010(4) 0.012(4) C2 0.035(5) 0.022(4) 0.029(4) 0.008(4) 0.003(4) 0.006(4) C3 0.047(5) 0.030(5) 0.034(5) 0.019(4) 0.007(4) 0.007(4) N1 0.055(5) 0.044(5) 0.056(5) 0.016(4) 0.018(5) 0.027(5) N2 0.073(6) 0.038(4) 0.043(5) 0.020(4) 0.003(4) -0.001(4) N3 0.054(5) 0.031(4) 0.037(4) -0.007(4) -0.009(4) -0.002(4) P1 0.0336(12) 0.0273(11) 0.0337(11) 0.0103(10) 0.0049(10) 0.0050(10) C4 0.040(5) 0.035(5) 0.031(4) 0.011(4) 0.005(4) 0.012(4) C5 0.047(6) 0.054(6) 0.039(5) 0.020(5) 0.007(5) 0.015(5) C6 0.046(6) 0.067(7) 0.036(5) 0.019(5) 0.001(5) 0.017(6) C7 0.058(7) 0.099(9) 0.028(5) 0.016(6) 0.015(5) 0.042(7) C8 0.066(8) 0.050(6) 0.055(7) -0.002(5) 0.005(6) 0.024(6) C9 0.052(6) 0.039(5) 0.048(6) 0.007(5) 0.012(5) 0.010(5) C10 0.040(5) 0.023(4) 0.028(4) 0.004(3) 0.004(4) 0.001(4) C11 0.050(6) 0.034(5) 0.044(5) 0.001(4) -0.005(5) 0.015(5) C12 0.061(7) 0.047(6) 0.053(6) 0.005(5) -0.006(6) 0.021(6) C13 0.061(7) 0.036(5) 0.054(6) -0.001(5) 0.002(6) 0.001(5) C14 0.070(7) 0.023(5) 0.050(6) -0.002(4) 0.010(6) 0.008(5) C15 0.048(6) 0.031(5) 0.049(6) 0.015(4) 0.007(5) 0.012(4) C16 0.027(5) 0.031(5) 0.056(6) 0.017(4) -0.005(5) -0.005(4) C17 0.045(6) 0.044(6) 0.064(7) 0.027(5) -0.007(5) 0.004(5) C20 0.035(6) 0.059(8) 0.153(15) 0.048(9) 0.015(8) 0.016(6) C18 0.066(8) 0.070(8) 0.080(9) 0.043(8) -0.011(7) 0.002(7) C19 0.057(8) 0.076(9) 0.140(14) 0.072(10) -0.009(9) 0.012(7) C21 0.041(6) 0.052(6) 0.086(8) 0.036(6) 0.009(6) 0.007(5) C22 0.037(5) 0.024(4) 0.040(5) 0.011(4) 0.011(4) 0.004(4) C23 0.062(7) 0.038(5) 0.042(5) 0.012(4) 0.009(5) 0.007(5) C24 0.089(9) 0.043(6) 0.045(6) 0.024(5) 0.021(6) 0.017(6) C25 0.083(9) 0.038(6) 0.069(8) 0.021(6) 0.036(7) 0.006(6) C26 0.047(6) 0.037(6) 0.074(8) 0.005(5) 0.015(6) -0.009(5) C27 0.044(6) 0.043(5) 0.053(6) 0.015(5) 0.012(5) 0.000(5) P2 0.0306(12) 0.0309(11) 0.0317(11) 0.0107(10) 0.0031(10) 0.0077(10) C28 0.036(5) 0.027(4) 0.026(4) 0.009(3) 0.008(4) 0.008(4) C29 0.030(5) 0.044(5) 0.033(5) 0.012(4) 0.001(4) 0.012(4) C30 0.042(6) 0.045(6) 0.052(6) 0.022(5) -0.003(5) 0.016(5) C31 0.028(5) 0.057(6) 0.042(5) 0.002(5) 0.000(4) 0.008(5) C32 0.048(6) 0.033(5) 0.055(6) 0.014(5) 0.012(5) 0.001(5) C33 0.032(5) 0.040(5) 0.053(6) 0.021(5) 0.001(5) 0.010(4) C34 0.039(5) 0.037(5) 0.028(4) 0.008(4) 0.001(4) 0.014(4) C35 0.052(6) 0.058(7) 0.053(6) 0.024(5) 0.023(6) 0.020(6) C36 0.047(6) 0.067(8) 0.059(7) 0.014(6) 0.018(6) 0.016(6) C37 0.061(7) 0.085(9) 0.033(5) 0.003(6) 0.006(5) 0.046(7) C38 0.072(8) 0.039(6) 0.061(7) -0.003(5) -0.002(7) 0.019(6) C39 0.046(6) 0.038(5) 0.064(7) 0.011(5) 0.012(6) 0.005(5) C40 0.037(5) 0.032(4) 0.035(5) 0.014(4) 0.003(4) 0.014(4) C41 0.042(6) 0.079(8) 0.041(5) 0.027(6) 0.005(5) 0.025(6) C42 0.065(8) 0.096(9) 0.047(6) 0.026(7) 0.004(6) 0.037(7) C43 0.064(7) 0.053(6) 0.035(5) 0.017(5) -0.006(5) 0.017(6) C44 0.048(6) 0.058(6) 0.040(5) 0.016(5) 0.011(5) 0.005(5) C45 0.031(5) 0.048(5) 0.035(5) 0.013(4) 0.004(4) 0.003(4) C46 0.030(4) 0.028(4) 0.036(5) 0.010(4) 0.006(4) 0.003(4) C47 0.054(6) 0.046(6) 0.051(6) 0.022(5) 0.011(5) -0.003(5) C48 0.062(7) 0.046(6) 0.066(7) 0.020(6) 0.007(6) -0.003(6) C49 0.059(7) 0.043(6) 0.063(7) 0.029(5) 0.016(6) 0.010(5) C50 0.060(7) 0.056(6) 0.055(6) 0.033(6) 0.023(6) 0.018(6) C51 0.044(5) 0.042(5) 0.040(5) 0.015(4) 0.010(5) 0.001(5) C53 0.078(10) 0.112(12) 0.081(10) 0.032(10) 0.025(9) 0.002(9) C52 0.057(9) 0.20(2) 0.115(13) 0.078(14) 0.016(9) 0.053(11) N4 0.185(17) 0.132(13) 0.087(10) 0.039(10) 0.047(11) 0.001(11) _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 Re1 C1 2.124(9) . ? Re1 Se4 2.5202(9) . ? Re1 Se2 2.5203(9) . ? Re1 Se1 2.5256(9) . ? Re1 Se3 2.5294(9) . ? Re1 Re3 2.6358(6) . ? Re1 Re2 2.6361(5) 2_576 ? Re1 Re3 2.6411(6) 2_576 ? Re1 Re2 2.6443(5) . ? Re1 Re1 3.7310(8) 2_576 ? Re2 C2 2.126(7) . ? Re2 Se2 2.5103(10) . ? Re2 Se3 2.5199(10) 2_576 ? Re2 Se1 2.5238(10) . ? Re2 Se4 2.5329(10) 2_576 ? Re2 Re1 2.6361(6) 2_576 ? Re2 Re3 2.6391(5) . ? Re2 Re3 2.6418(5) 2_576 ? Re2 Re2 3.7366(7) 2_576 ? Re3 C3 2.147(9) . ? Re3 Se3 2.5185(9) . ? Re3 Se1 2.5195(10) 2_576 ? Re3 Se4 2.5227(9) 2_576 ? Re3 Se2 2.5271(10) . ? Re3 Re1 2.6411(6) 2_576 ? Re3 Re2 2.6418(5) 2_576 ? Re3 Re3 3.7317(10) 2_576 ? Se1 Re3 2.5196(10) 2_576 ? Se3 Re2 2.5200(10) 2_576 ? Se4 Re3 2.5227(8) 2_576 ? Se4 Re2 2.5329(10) 2_576 ? C1 N1 1.145(11) . ? C2 N2 1.140(9) . ? C3 N3 1.125(10) . ? P1 C4 1.793(9) . ? P1 C10 1.796(8) . ? P1 C16 1.797(9) . ? P1 C22 1.798(8) . ? C4 C5 1.375(11) . ? C4 C9 1.382(12) . ? C5 C6 1.387(14) . ? C6 C7 1.378(15) . ? C7 C8 1.331(14) . ? C8 C9 1.369(15) . ? C10 C11 1.376(12) . ? C10 C15 1.389(12) . ? C11 C12 1.384(13) . ? C12 C13 1.381(14) . ? C13 C14 1.354(14) . ? C14 C15 1.403(13) . ? C16 C17 1.381(13) . ? C16 C21 1.419(14) . ? C17 C18 1.386(14) . ? C20 C21 1.356(15) . ? C20 C19 1.390(19) . ? C18 C19 1.361(18) . ? C22 C23 1.375(12) . ? C22 C27 1.393(12) . ? C23 C24 1.396(12) . ? C24 C25 1.378(15) . ? C25 C26 1.366(15) . ? C26 C27 1.371(12) . ? P2 C34 1.793(9) . ? P2 C46 1.796(8) . ? P2 C40 1.797(8) . ? P2 C28 1.802(9) . ? C28 C29 1.384(11) . ? C28 C33 1.398(10) . ? C29 C30 1.388(12) . ? C30 C31 1.379(12) . ? C31 C32 1.372(13) . ? C32 C33 1.384(13) . ? C34 C35 1.383(12) . ? C34 C39 1.392(12) . ? C35 C36 1.397(15) . ? C36 C37 1.355(15) . ? C37 C38 1.387(15) . ? C38 C39 1.369(15) . ? C40 C45 1.365(12) . ? C40 C41 1.375(12) . ? C41 C42 1.384(13) . ? C42 C43 1.369(15) . ? C43 C44 1.371(14) . ? C44 C45 1.382(12) . ? C46 C47 1.359(12) . ? C46 C51 1.401(11) . ? C47 C48 1.386(12) . ? C48 C49 1.359(14) . ? C49 C50 1.371(14) . ? C50 C51 1.382(12) . ? C53 N4 1.098(17) . ? C53 C52 1.453(18) . ? 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 C1 Re1 Se4 91.0(2) . . ? C1 Re1 Se2 92.6(2) . . ? Se4 Re1 Se2 176.28(3) . . ? C1 Re1 Se1 94.1(2) . . ? Se4 Re1 Se1 89.52(3) . . ? Se2 Re1 Se1 89.48(3) . . ? C1 Re1 Se3 90.0(2) . . ? Se4 Re1 Se3 90.37(3) . . ? Se2 Re1 Se3 90.38(3) . . ? Se1 Re1 Se3 175.92(3) . . ? C1 Re1 Re3 134.0(2) . . ? Se4 Re1 Re3 118.92(3) . . ? Se2 Re1 Re3 58.64(3) . . ? Se1 Re1 Re3 118.35(3) . . ? Se3 Re1 Re3 58.32(2) . . ? C1 Re1 Re2 133.0(2) . 2_576 ? Se4 Re1 Re2 58.79(3) . 2_576 ? Se2 Re1 Re2 118.77(3) . 2_576 ? Se1 Re1 Re2 118.32(3) . 2_576 ? Se3 Re1 Re2 58.35(2) . 2_576 ? Re3 Re1 Re2 60.146(14) . 2_576 ? C1 Re1 Re3 136.0(2) . 2_576 ? Se4 Re1 Re3 58.46(2) . 2_576 ? Se2 Re1 Re3 118.08(2) . 2_576 ? Se1 Re1 Re3 58.32(2) . 2_576 ? Se3 Re1 Re3 118.35(3) . 2_576 ? Re3 Re1 Re3 90.01(2) . 2_576 ? Re2 Re1 Re3 60.013(16) 2_576 2_576 ? C1 Re1 Re2 136.9(2) . . ? Se4 Re1 Re2 118.44(3) . . ? Se2 Re1 Re2 58.10(2) . . ? Se1 Re1 Re2 58.39(2) . . ? Se3 Re1 Re2 118.28(3) . . ? Re3 Re1 Re2 59.976(14) . . ? Re2 Re1 Re2 90.086(15) 2_576 . ? Re3 Re1 Re2 59.977(14) 2_576 . ? C1 Re1 Re1 177.9(2) . 2_576 ? Se4 Re1 Re1 88.36(3) . 2_576 ? Se2 Re1 Re1 88.03(3) . 2_576 ? Se1 Re1 Re1 87.92(3) . 2_576 ? Se3 Re1 Re1 88.00(3) . 2_576 ? Re3 Re1 Re1 45.063(12) . 2_576 ? Re2 Re1 Re1 45.132(11) 2_576 2_576 ? Re3 Re1 Re1 44.948(14) 2_576 2_576 ? Re2 Re1 Re1 44.954(11) . 2_576 ? C2 Re2 Se2 90.7(2) . . ? C2 Re2 Se3 92.8(2) . 2_576 ? Se2 Re2 Se3 176.43(3) . 2_576 ? C2 Re2 Se1 93.9(2) . . ? Se2 Re2 Se1 89.74(3) . . ? Se3 Re2 Se1 89.51(3) 2_576 . ? C2 Re2 Se4 90.3(2) . 2_576 ? Se2 Re2 Se4 90.20(3) . 2_576 ? Se3 Re2 Se4 90.30(3) 2_576 2_576 ? Se1 Re2 Se4 175.83(3) . 2_576 ? C2 Re2 Re1 134.4(2) . 2_576 ? Se2 Re2 Re1 118.79(2) . 2_576 ? Se3 Re2 Re1 58.70(2) 2_576 2_576 ? Se1 Re2 Re1 118.24(3) . 2_576 ? Se4 Re2 Re1 58.32(2) 2_576 2_576 ? C2 Re2 Re3 133.0(2) . . ? Se2 Re2 Re3 58.72(2) . . ? Se3 Re2 Re3 118.77(3) 2_576 . ? Se1 Re2 Re3 118.29(2) . . ? Se4 Re2 Re3 58.34(2) 2_576 . ? Re1 Re2 Re3 60.088(15) 2_576 . ? C2 Re2 Re3 137.1(2) . 2_576 ? Se2 Re2 Re3 118.42(2) . 2_576 ? Se3 Re2 Re3 58.35(2) 2_576 2_576 ? Se1 Re2 Re3 58.33(2) . 2_576 ? Se4 Re2 Re3 118.22(3) 2_576 2_576 ? Re1 Re2 Re3 59.922(15) 2_576 2_576 ? Re3 Re2 Re3 89.925(19) . 2_576 ? C2 Re2 Re1 135.6(2) . . ? Se2 Re2 Re1 58.47(2) . . ? Se3 Re2 Re1 118.30(2) 2_576 . ? Se1 Re2 Re1 58.45(2) . . ? Se4 Re2 Re1 118.18(2) 2_576 . ? Re1 Re2 Re1 89.914(16) 2_576 . ? Re3 Re2 Re1 59.853(14) . . ? Re3 Re2 Re1 59.952(14) 2_576 . ? C2 Re2 Re2 177.9(2) . 2_576 ? Se2 Re2 Re2 88.26(2) . 2_576 ? Se3 Re2 Re2 88.22(2) 2_576 2_576 ? Se1 Re2 Re2 87.91(2) . 2_576 ? Se4 Re2 Re2 87.92(2) 2_576 2_576 ? Re1 Re2 Re2 45.046(11) 2_576 2_576 ? Re3 Re2 Re2 44.992(13) . 2_576 ? Re3 Re2 Re2 44.934(12) 2_576 2_576 ? Re1 Re2 Re2 44.868(11) . 2_576 ? C3 Re3 Se3 91.4(2) . . ? C3 Re3 Se1 92.6(2) . 2_576 ? Se3 Re3 Se1 89.64(3) . 2_576 ? C3 Re3 Se4 92.0(2) . 2_576 ? Se3 Re3 Se4 176.53(3) . 2_576 ? Se1 Re3 Se4 89.59(3) 2_576 2_576 ? C3 Re3 Se2 91.5(2) . . ? Se3 Re3 Se2 90.48(3) . . ? Se1 Re3 Se2 175.90(3) 2_576 . ? Se4 Re3 Se2 90.05(3) 2_576 . ? C3 Re3 Re1 134.2(3) . . ? Se3 Re3 Re1 58.72(2) . . ? Se1 Re3 Re1 118.41(3) 2_576 . ? Se4 Re3 Re1 118.88(2) 2_576 . ? Se2 Re3 Re1 58.39(2) . . ? C3 Re3 Re2 134.63(19) . . ? Se3 Re3 Re2 118.88(3) . . ? Se1 Re3 Re2 118.43(3) 2_576 . ? Se4 Re3 Re2 58.72(2) 2_576 . ? Se2 Re3 Re2 58.10(2) . . ? Re1 Re3 Re2 60.171(15) . . ? C3 Re3 Re1 135.8(3) . 2_576 ? Se3 Re3 Re1 118.47(3) . 2_576 ? Se1 Re3 Re1 58.54(2) 2_576 2_576 ? Se4 Re3 Re1 58.37(2) 2_576 2_576 ? Se2 Re3 Re1 117.98(2) . 2_576 ? Re1 Re3 Re1 89.99(2) . 2_576 ? Re2 Re3 Re1 59.899(15) . 2_576 ? C3 Re3 Re2 135.28(19) . 2_576 ? Se3 Re3 Re2 58.40(2) . 2_576 ? Se1 Re3 Re2 58.49(2) 2_576 2_576 ? Se4 Re3 Re2 118.44(3) 2_576 2_576 ? Se2 Re3 Re2 118.30(3) . 2_576 ? Re1 Re3 Re2 59.932(18) . 2_576 ? Re2 Re3 Re2 90.07(2) . 2_576 ? Re1 Re3 Re2 60.071(15) 2_576 2_576 ? C3 Re3 Re3 179.2(3) . 2_576 ? Se3 Re3 Re3 88.32(2) . 2_576 ? Se1 Re3 Re3 88.09(3) 2_576 2_576 ? Se4 Re3 Re3 88.28(2) 2_576 2_576 ? Se2 Re3 Re3 87.82(3) . 2_576 ? Re1 Re3 Re3 45.052(15) . 2_576 ? Re2 Re3 Re3 45.066(13) . 2_576 ? Re1 Re3 Re3 44.937(12) 2_576 2_576 ? Re2 Re3 Re3 45.008(13) 2_576 2_576 ? Re3 Se1 Re2 63.18(2) 2_576 . ? Re3 Se1 Re1 63.13(2) 2_576 . ? Re2 Se1 Re1 63.16(2) . . ? Re2 Se2 Re1 63.42(2) . . ? Re2 Se2 Re3 63.19(3) . . ? Re1 Se2 Re3 62.96(2) . . ? Re3 Se3 Re2 63.25(2) . 2_576 ? Re3 Se3 Re1 62.95(2) . . ? Re2 Se3 Re1 62.94(2) 2_576 . ? Re1 Se4 Re3 63.17(2) . 2_576 ? Re1 Se4 Re2 62.89(3) . 2_576 ? Re3 Se4 Re2 62.94(2) 2_576 2_576 ? N1 C1 Re1 177.6(9) . . ? N2 C2 Re2 178.2(7) . . ? N3 C3 Re3 178.1(9) . . ? C4 P1 C10 108.4(4) . . ? C4 P1 C16 109.0(4) . . ? C10 P1 C16 112.3(4) . . ? C4 P1 C22 108.1(4) . . ? C10 P1 C22 111.6(4) . . ? C16 P1 C22 107.4(4) . . ? C5 C4 C9 119.9(9) . . ? C5 C4 P1 119.1(7) . . ? C9 C4 P1 121.0(7) . . ? C4 C5 C6 120.9(10) . . ? C7 C6 C5 117.1(10) . . ? C8 C7 C6 122.1(11) . . ? C7 C8 C9 121.4(11) . . ? C8 C9 C4 118.5(9) . . ? C11 C10 C15 120.7(8) . . ? C11 C10 P1 117.5(7) . . ? C15 C10 P1 121.8(7) . . ? C10 C11 C12 119.3(9) . . ? C13 C12 C11 120.6(10) . . ? C14 C13 C12 120.0(10) . . ? C13 C14 C15 120.8(9) . . ? C10 C15 C14 118.6(9) . . ? C17 C16 C21 119.4(9) . . ? C17 C16 P1 122.0(8) . . ? C21 C16 P1 118.4(7) . . ? C16 C17 C18 120.1(12) . . ? C21 C20 C19 120.3(13) . . ? C19 C18 C17 119.7(12) . . ? C18 C19 C20 121.0(11) . . ? C20 C21 C16 119.4(12) . . ? C23 C22 C27 120.4(8) . . ? C23 C22 P1 122.2(7) . . ? C27 C22 P1 117.4(7) . . ? C22 C23 C24 119.3(9) . . ? C25 C24 C23 119.5(9) . . ? C26 C25 C24 120.8(9) . . ? C25 C26 C27 120.3(10) . . ? C26 C27 C22 119.5(9) . . ? C34 P2 C46 108.5(4) . . ? C34 P2 C40 107.3(4) . . ? C46 P2 C40 108.3(4) . . ? C34 P2 C28 112.0(4) . . ? C46 P2 C28 111.7(4) . . ? C40 P2 C28 108.9(4) . . ? C29 C28 C33 119.2(8) . . ? C29 C28 P2 121.5(6) . . ? C33 C28 P2 119.3(6) . . ? C28 C29 C30 120.2(8) . . ? C31 C30 C29 120.3(8) . . ? C32 C31 C30 119.7(8) . . ? C31 C32 C33 120.8(8) . . ? C32 C33 C28 119.8(8) . . ? C35 C34 C39 118.9(10) . . ? C35 C34 P2 119.7(7) . . ? C39 C34 P2 121.1(7) . . ? C34 C35 C36 120.4(10) . . ? C37 C36 C35 120.0(10) . . ? C36 C37 C38 119.6(11) . . ? C39 C38 C37 121.1(10) . . ? C38 C39 C34 119.7(10) . . ? C45 C40 C41 119.3(8) . . ? C45 C40 P2 121.7(7) . . ? C41 C40 P2 118.8(7) . . ? C40 C41 C42 120.7(10) . . ? C43 C42 C41 119.4(10) . . ? C42 C43 C44 120.1(9) . . ? C43 C44 C45 120.1(9) . . ? C40 C45 C44 120.4(9) . . ? C47 C46 C51 119.7(8) . . ? C47 C46 P2 121.1(7) . . ? C51 C46 P2 118.9(6) . . ? C46 C47 C48 119.9(9) . . ? C49 C48 C47 120.2(10) . . ? C48 C49 C50 121.1(9) . . ? C49 C50 C51 119.0(9) . . ? C50 C51 C46 119.9(9) . . ? N4 C53 C52 178(2) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.84 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 2.216 _refine_diff_density_min -2.710 _refine_diff_density_rms 0.199 #################### Material relevant to compound 5 at 90K ############ data_sb8p3 _database_code_CSD 187004 _publ_requested_journal 'Chemical Communication' _publ_requested_category FM _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(PPh4)4 Re6Se8(CN)6 (CH3CN)2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H86 N8 P4 Re6 Se8' _chemical_formula_weight 3344.59 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3276(15) _cell_length_b 13.0743(17) _cell_length_c 16.880(2) _cell_angle_alpha 110.045(15) _cell_angle_beta 95.871(16) _cell_angle_gamma 101.625(15) _cell_volume 2459.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description block _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.5968 _exptl_crystal_size_mid 0.3466 _exptl_crystal_size_min 0.1732 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 10.430 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0188 _exptl_absorpt_correction_T_max 0.2148 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'STOE-IPDS'' _diffrn_measurement_method 'Oscillation, Phi. incr. == 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24295 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.95 _reflns_number_total 8931 _reflns_number_gt 6591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE, [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0240P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00097(4) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8931 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _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 0.122148(19) 0.935929(16) 0.483037(14) 0.00840(6) Uani 1 1 d . . . Re2 Re 0.034586(19) 1.069167(16) 0.422489(14) 0.00844(6) Uani 1 1 d . . . Re3 Re -0.092234(19) 0.874282(16) 0.410056(14) 0.00841(6) Uani 1 1 d . . . Se1 Se 0.23846(5) 1.12508(4) 0.49606(4) 0.01077(12) Uani 1 1 d . . . Se2 Se 0.06248(5) 0.88689(4) 0.32446(4) 0.01011(12) Uani 1 1 d . . . Se3 Se -0.00585(5) 0.75251(4) 0.47148(4) 0.01048(12) Uani 1 1 d . . . Se4 Se 0.17338(5) 0.99388(4) 0.64318(4) 0.01012(12) Uani 1 1 d . . . C1 C 0.2578(5) 0.8575(4) 0.4656(4) 0.0106(12) Uani 1 1 d . . . C2 C 0.0690(5) 1.1426(4) 0.3306(4) 0.0140(12) Uani 1 1 d . . . C3 C -0.1943(5) 0.7298(5) 0.3085(4) 0.0127(12) Uani 1 1 d . . . N1 N 0.3276(4) 0.8127(4) 0.4558(3) 0.0170(11) Uani 1 1 d . . . N2 N 0.0865(5) 1.1799(4) 0.2792(3) 0.0184(12) Uani 1 1 d . . . N3 N -0.2477(5) 0.6506(4) 0.2515(3) 0.0174(11) Uani 1 1 d . . . P1 P -0.10134(13) 0.30834(11) 0.05551(10) 0.0113(3) Uani 1 1 d . . . C4 C -0.0195(5) 0.2420(4) -0.0192(4) 0.0132(12) Uani 1 1 d . . . C5 C 0.0603(5) 0.3081(5) -0.0460(4) 0.0156(13) Uani 1 1 d . . . H5 H 0.0727 0.3859 -0.0236 0.019 Uiso 1 1 calc R . . C6 C 0.1209(5) 0.2586(5) -0.1056(4) 0.0161(13) Uani 1 1 d . . . H6 H 0.1735 0.3030 -0.1238 0.019 Uiso 1 1 calc R . . C7 C 0.1036(5) 0.1419(5) -0.1386(4) 0.0190(14) Uani 1 1 d . . . H7 H 0.1434 0.1084 -0.1798 0.023 Uiso 1 1 calc R . . C8 C 0.0271(6) 0.0761(5) -0.1101(4) 0.0199(14) Uani 1 1 d . . . H8 H 0.0175 -0.0015 -0.1307 0.024 Uiso 1 1 calc R . . C9 C -0.0350(5) 0.1252(5) -0.0511(4) 0.0163(13) Uani 1 1 d . . . H9 H -0.0872 0.0806 -0.0327 0.020 Uiso 1 1 calc R . . C10 C -0.0069(5) 0.4075(4) 0.1506(4) 0.0150(13) Uani 1 1 d . . . C11 C 0.0714(5) 0.3684(5) 0.1908(4) 0.0165(13) Uani 1 1 d . . . H11 H 0.0744 0.2937 0.1667 0.020 Uiso 1 1 calc R . . C12 C 0.1447(6) 0.4401(5) 0.2664(4) 0.0202(14) Uani 1 1 d . . . H12 H 0.1958 0.4130 0.2931 0.024 Uiso 1 1 calc R . . C13 C 0.1421(5) 0.5524(5) 0.3023(4) 0.0144(12) Uani 1 1 d . . . H13 H 0.1926 0.6012 0.3520 0.017 Uiso 1 1 calc R . . C14 C 0.0629(5) 0.5908(5) 0.2630(4) 0.0159(12) Uiso 1 1 d . . . H14 H 0.0597 0.6653 0.2876 0.019 Uiso 1 1 calc R . . C15 C -0.0109(5) 0.5201(4) 0.1879(4) 0.0142(12) Uani 1 1 d . . . H15 H -0.0630 0.5472 0.1623 0.017 Uiso 1 1 calc R . . C16 C -0.1896(5) 0.3748(4) 0.0084(4) 0.0132(12) Uani 1 1 d . . . C17 C -0.1922(5) 0.3637(5) -0.0774(4) 0.0154(12) Uiso 1 1 d . . . H17 H -0.1453 0.3258 -0.1093 0.019 Uiso 1 1 calc R . . C18 C -0.2660(5) 0.4103(5) -0.1149(4) 0.0205(14) Uani 1 1 d . . . H18 H -0.2695 0.4029 -0.1720 0.025 Uiso 1 1 calc R . . C19 C -0.3332(6) 0.4673(5) -0.0657(5) 0.0245(15) Uani 1 1 d . . . H19 H -0.3826 0.4981 -0.0902 0.029 Uiso 1 1 calc R . . C20 C -0.3287(5) 0.4798(5) 0.0187(4) 0.0197(14) Uani 1 1 d . . . H20 H -0.3742 0.5193 0.0510 0.024 Uiso 1 1 calc R . . C21 C -0.2568(5) 0.4337(5) 0.0555(4) 0.0186(13) Uani 1 1 d . . . H21 H -0.2538 0.4425 0.1129 0.022 Uiso 1 1 calc R . . C22 C -0.1950(5) 0.2008(4) 0.0774(4) 0.0128(12) Uani 1 1 d . . . C23 C -0.1744(5) 0.1814(5) 0.1529(4) 0.0145(12) Uani 1 1 d . . . H23 H -0.1145 0.2288 0.1966 0.017 Uiso 1 1 calc R . . C24 C -0.2435(6) 0.0918(5) 0.1621(4) 0.0209(14) Uani 1 1 d . . . H24 H -0.2301 0.0785 0.2125 0.025 Uiso 1 1 calc R . . C25 C -0.3326(6) 0.0209(5) 0.0978(4) 0.0197(14) Uani 1 1 d . . . H25 H -0.3789 -0.0393 0.1054 0.024 Uiso 1 1 calc R . . C26 C -0.3540(5) 0.0385(5) 0.0217(4) 0.0198(13) Uani 1 1 d . . . H26 H -0.4139 -0.0096 -0.0217 0.024 Uiso 1 1 calc R . . C27 C -0.2842(5) 0.1292(5) 0.0117(4) 0.0133(12) Uani 1 1 d . . . H27 H -0.2971 0.1421 -0.0389 0.016 Uiso 1 1 calc R . . P2 P 0.49360(13) 1.27567(11) 0.29160(10) 0.0106(3) Uani 1 1 d . . . C28 C 0.6444(5) 1.3214(4) 0.3172(4) 0.0134(12) Uani 1 1 d . . . C29 C 0.7104(5) 1.2609(4) 0.3465(4) 0.0132(12) Uani 1 1 d . . . H29 H 0.6760 1.1928 0.3499 0.016 Uiso 1 1 calc R . . C30 C 0.8263(5) 1.3019(5) 0.3701(4) 0.0163(12) Uiso 1 1 d . . . H30 H 0.8694 1.2613 0.3892 0.020 Uiso 1 1 calc R . . C31 C 0.8781(5) 1.4036(5) 0.3655(4) 0.0180(13) Uani 1 1 d . . . H31 H 0.9556 1.4324 0.3833 0.022 Uiso 1 1 calc R . . C32 C 0.8138(5) 1.4630(4) 0.3341(4) 0.0154(13) Uani 1 1 d . . . H32 H 0.8490 1.5300 0.3294 0.019 Uiso 1 1 calc R . . C33 C 0.6990(5) 1.4226(4) 0.3102(4) 0.0127(11) Uiso 1 1 d . . . H33 H 0.6568 1.4624 0.2891 0.015 Uiso 1 1 calc R . . C34 C 0.4290(5) 1.3712(4) 0.3644(4) 0.0110(11) Uiso 1 1 d . . . C35 C 0.3425(5) 1.3284(5) 0.3989(4) 0.0135(12) Uani 1 1 d . . . H35 H 0.3225 1.2517 0.3882 0.016 Uiso 1 1 calc R . . C36 C 0.2838(6) 1.4003(5) 0.4504(4) 0.0209(14) Uani 1 1 d . . . H36 H 0.2254 1.3719 0.4738 0.025 Uiso 1 1 calc R . . C37 C 0.3159(5) 1.5149(5) 0.4652(4) 0.0162(12) Uiso 1 1 d . . . H37 H 0.2782 1.5635 0.4987 0.019 Uiso 1 1 calc R . . C38 C 0.4022(5) 1.5565(5) 0.4309(4) 0.0194(14) Uani 1 1 d . . . H38 H 0.4224 1.6332 0.4415 0.023 Uiso 1 1 calc R . . C39 C 0.4600(5) 1.4864(5) 0.3805(4) 0.0136(12) Uani 1 1 d . . . H39 H 0.5187 1.5156 0.3577 0.016 Uiso 1 1 calc R . . C40 C 0.4474(5) 1.2710(4) 0.1861(4) 0.0126(12) Uani 1 1 d . . . C41 C 0.3344(5) 1.2685(5) 0.1615(4) 0.0178(13) Uani 1 1 d . . . H41 H 0.2860 1.2730 0.2007 0.021 Uiso 1 1 calc R . . C42 C 0.2952(5) 1.2594(5) 0.0797(4) 0.0154(13) Uani 1 1 d . . . H42 H 0.2199 1.2563 0.0633 0.018 Uiso 1 1 calc R . . C43 C 0.3681(5) 1.2547(5) 0.0208(4) 0.0185(14) Uani 1 1 d . . . H43 H 0.3416 1.2499 -0.0343 0.022 Uiso 1 1 calc R . . C44 C 0.4803(5) 1.2572(4) 0.0449(4) 0.0126(12) Uani 1 1 d . . . H44 H 0.5292 1.2544 0.0061 0.015 Uiso 1 1 calc R . . C45 C 0.5188(5) 1.2639(4) 0.1271(4) 0.0120(12) Uani 1 1 d . . . H45 H 0.5932 1.2637 0.1428 0.014 Uiso 1 1 calc R . . C46 C 0.4429(5) 1.1385(4) 0.2942(4) 0.0119(12) Uani 1 1 d . . . C47 C 0.3641(5) 1.0560(5) 0.2265(4) 0.0176(13) Uani 1 1 d . . . H47 H 0.3435 1.0691 0.1770 0.021 Uiso 1 1 calc R . . C48 C 0.3161(5) 0.9548(5) 0.2320(4) 0.0175(13) Uani 1 1 d . . . H48 H 0.2622 0.9003 0.1867 0.021 Uiso 1 1 calc R . . C49 C 0.3482(5) 0.9338(5) 0.3051(4) 0.0188(13) Uiso 1 1 d . . . H49 H 0.3166 0.8649 0.3084 0.023 Uiso 1 1 calc R . . C50 C 0.4270(5) 1.0155(5) 0.3729(4) 0.0173(13) Uani 1 1 d . . . H50 H 0.4486 1.0010 0.4216 0.021 Uiso 1 1 calc R . . C51 C 0.4740(5) 1.1184(5) 0.3690(4) 0.0144(12) Uani 1 1 d . . . H51 H 0.5256 1.1738 0.4153 0.017 Uiso 1 1 calc R . . C53 C 0.4628(5) 1.2114(5) 0.7723(5) 0.0239(15) Uani 1 1 d . . . C52 C 0.4649(7) 1.2321(7) 0.6925(5) 0.0387(19) Uani 1 1 d . . . H52A H 0.4166 1.1687 0.6458 0.058 Uiso 1 1 calc R . . H52B H 0.5406 1.2431 0.6817 0.058 Uiso 1 1 calc R . . H52C H 0.4391 1.2982 0.6977 0.058 Uiso 1 1 calc R . . N4 N 0.4606(6) 1.1948(5) 0.8342(4) 0.0382(16) 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 Re1 0.00970(14) 0.00872(11) 0.00738(12) 0.00314(9) 0.00163(9) 0.00337(9) Re2 0.01043(14) 0.00842(11) 0.00709(12) 0.00332(9) 0.00178(9) 0.00289(9) Re3 0.01010(14) 0.00818(11) 0.00721(12) 0.00299(9) 0.00142(9) 0.00273(9) Se1 0.0111(3) 0.0111(3) 0.0101(3) 0.0043(2) 0.0020(2) 0.0023(2) Se2 0.0119(3) 0.0106(3) 0.0084(3) 0.0032(2) 0.0026(2) 0.0042(2) Se3 0.0135(3) 0.0087(2) 0.0097(3) 0.0036(2) 0.0017(2) 0.0037(2) Se4 0.0114(3) 0.0109(3) 0.0089(3) 0.0041(2) 0.0011(2) 0.0042(2) C1 0.017(4) 0.011(3) 0.006(3) 0.004(2) 0.007(2) 0.006(2) C2 0.013(4) 0.012(3) 0.014(3) 0.000(2) 0.002(2) 0.007(2) C3 0.014(3) 0.016(3) 0.018(3) 0.013(3) 0.008(3) 0.009(2) N1 0.015(3) 0.017(2) 0.021(3) 0.009(2) 0.004(2) 0.005(2) N2 0.024(3) 0.014(2) 0.017(3) 0.009(2) -0.001(2) 0.001(2) N3 0.023(3) 0.016(3) 0.013(3) 0.005(2) 0.000(2) 0.008(2) P1 0.0122(9) 0.0109(7) 0.0104(8) 0.0037(6) 0.0017(6) 0.0030(6) C4 0.011(3) 0.014(3) 0.014(3) 0.006(2) -0.005(2) 0.002(2) C5 0.019(4) 0.012(3) 0.012(3) 0.002(2) -0.005(2) 0.003(2) C6 0.009(4) 0.032(3) 0.017(3) 0.017(3) 0.006(2) 0.011(3) C7 0.021(4) 0.024(3) 0.012(3) 0.006(3) -0.002(3) 0.010(3) C8 0.024(4) 0.013(3) 0.016(3) 0.002(3) -0.007(3) 0.002(2) C9 0.015(4) 0.016(3) 0.018(3) 0.004(2) 0.006(3) 0.006(2) C10 0.020(4) 0.009(3) 0.010(3) 0.000(2) 0.004(2) -0.002(2) C11 0.027(4) 0.014(3) 0.008(3) 0.001(2) 0.005(3) 0.008(3) C12 0.027(4) 0.017(3) 0.014(3) 0.004(3) -0.005(3) 0.008(3) C13 0.014(4) 0.017(3) 0.010(3) 0.002(2) 0.003(2) 0.003(2) C15 0.013(4) 0.016(3) 0.016(3) 0.006(2) 0.005(2) 0.005(2) C16 0.015(3) 0.012(3) 0.014(3) 0.008(2) -0.001(2) 0.001(2) C18 0.016(4) 0.023(3) 0.022(4) 0.011(3) 0.001(3) 0.001(3) C19 0.020(4) 0.021(3) 0.033(4) 0.014(3) -0.007(3) 0.004(3) C20 0.012(4) 0.014(3) 0.030(4) 0.005(3) 0.004(3) 0.003(2) C21 0.016(4) 0.018(3) 0.022(4) 0.010(3) 0.003(3) 0.002(2) C22 0.013(3) 0.011(3) 0.015(3) 0.003(2) 0.007(2) 0.004(2) C23 0.019(4) 0.015(3) 0.011(3) 0.003(2) 0.007(2) 0.007(2) C24 0.031(4) 0.017(3) 0.018(3) 0.007(3) 0.005(3) 0.011(3) C25 0.025(4) 0.013(3) 0.025(4) 0.007(3) 0.019(3) 0.007(3) C26 0.009(4) 0.022(3) 0.022(4) 0.002(3) 0.004(3) 0.000(2) C27 0.010(3) 0.023(3) 0.008(3) 0.006(2) 0.005(2) 0.004(2) P2 0.0101(8) 0.0123(7) 0.0106(7) 0.0048(6) 0.0035(6) 0.0039(6) C28 0.012(3) 0.013(3) 0.010(3) 0.000(2) -0.004(2) 0.002(2) C29 0.022(4) 0.010(3) 0.008(3) 0.003(2) -0.001(2) 0.008(2) C31 0.005(3) 0.024(3) 0.017(3) 0.000(3) 0.003(2) 0.000(2) C32 0.024(4) 0.008(3) 0.010(3) 0.003(2) -0.003(2) -0.002(2) C35 0.015(4) 0.016(3) 0.011(3) 0.006(2) 0.001(2) 0.004(2) C36 0.018(4) 0.029(3) 0.014(3) 0.006(3) 0.007(3) 0.007(3) C38 0.023(4) 0.014(3) 0.016(3) 0.000(2) -0.005(3) 0.006(3) C39 0.008(3) 0.018(3) 0.016(3) 0.007(2) 0.006(2) 0.003(2) C40 0.015(3) 0.008(3) 0.013(3) 0.001(2) 0.002(2) 0.006(2) C41 0.018(4) 0.022(3) 0.016(3) 0.007(3) 0.008(3) 0.011(3) C42 0.010(4) 0.030(3) 0.012(3) 0.011(3) 0.003(2) 0.011(3) C43 0.029(4) 0.016(3) 0.012(3) 0.008(2) -0.001(3) 0.006(3) C44 0.015(4) 0.017(3) 0.007(3) 0.006(2) 0.005(2) 0.005(2) C45 0.012(3) 0.012(3) 0.011(3) 0.004(2) 0.001(2) 0.002(2) C46 0.019(4) 0.006(2) 0.010(3) 0.002(2) 0.004(2) 0.003(2) C47 0.028(4) 0.016(3) 0.010(3) 0.010(2) 0.000(3) 0.003(3) C48 0.010(4) 0.018(3) 0.018(3) 0.003(3) -0.001(3) -0.004(2) C50 0.026(4) 0.019(3) 0.014(3) 0.013(3) 0.005(3) 0.012(3) C51 0.007(3) 0.020(3) 0.015(3) 0.005(3) 0.001(2) 0.004(2) C53 0.006(4) 0.032(4) 0.028(4) 0.004(3) 0.007(3) 0.003(3) C52 0.037(5) 0.062(5) 0.029(4) 0.024(4) 0.011(4) 0.023(4) N4 0.050(5) 0.044(4) 0.020(4) 0.017(3) 0.007(3) 0.002(3) _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 Re1 C1 2.126(5) . ? Re1 Se4 2.5168(8) . ? Re1 Se2 2.5195(8) . ? Re1 Se1 2.5207(7) . ? Re1 Se3 2.5239(8) . ? Re1 Re2 2.6329(5) 2_576 ? Re1 Re3 2.6356(6) . ? Re1 Re3 2.6429(6) 2_576 ? Re1 Re2 2.6452(4) . ? Re1 Re1 3.7327(7) 2_576 ? Re2 C2 2.120(6) . ? Re2 Se2 2.5058(7) . ? Re2 Se3 2.5233(8) 2_576 ? Re2 Se1 2.5282(8) . ? Re2 Se4 2.5341(8) 2_576 ? Re2 Re1 2.6329(5) 2_576 ? Re2 Re3 2.6347(5) . ? Re2 Re3 2.6432(6) 2_576 ? Re2 Re2 3.7317(6) 2_576 ? Re3 C3 2.114(6) . ? Re3 Se3 2.5166(6) . ? Re3 Se1 2.5184(7) 2_576 ? Re3 Se4 2.5203(6) 2_576 ? Re3 Se2 2.5205(7) . ? Re3 Re1 2.6429(6) 2_576 ? Re3 Re2 2.6432(6) 2_576 ? Re3 Re3 3.7323(11) 2_576 ? Se1 Re3 2.5184(7) 2_576 ? Se3 Re2 2.5232(8) 2_576 ? Se4 Re3 2.5203(6) 2_576 ? Se4 Re2 2.5340(8) 2_576 ? C1 N1 1.130(7) . ? C2 N2 1.151(7) . ? C3 N3 1.160(8) . ? P1 C10 1.788(6) . ? P1 C4 1.795(6) . ? P1 C22 1.798(6) . ? P1 C16 1.803(5) . ? C4 C5 1.392(8) . ? C4 C9 1.398(7) . ? C5 C6 1.374(8) . ? C6 C7 1.394(8) . ? C7 C8 1.382(9) . ? C8 C9 1.381(9) . ? C10 C11 1.399(8) . ? C10 C15 1.402(7) . ? C11 C12 1.388(9) . ? C12 C13 1.392(8) . ? C13 C14 1.393(8) . ? C14 C15 1.382(9) . ? C16 C21 1.373(8) . ? C16 C17 1.402(8) . ? C17 C18 1.403(8) . ? C18 C19 1.377(9) . ? C19 C20 1.371(10) . ? C20 C21 1.376(8) . ? C22 C23 1.391(8) . ? C22 C27 1.393(8) . ? C23 C24 1.369(8) . ? C24 C25 1.379(9) . ? C25 C26 1.389(9) . ? C26 C27 1.391(8) . ? P2 C40 1.789(6) . ? P2 C28 1.792(6) . ? P2 C46 1.793(5) . ? P2 C34 1.803(6) . ? C28 C29 1.406(7) . ? C28 C33 1.408(8) . ? C29 C30 1.384(9) . ? C30 C31 1.386(8) . ? C31 C32 1.398(8) . ? C32 C33 1.371(9) . ? C34 C35 1.378(8) . ? C34 C39 1.398(7) . ? C35 C36 1.417(8) . ? C36 C37 1.396(8) . ? C37 C38 1.368(9) . ? C38 C39 1.388(8) . ? C40 C45 1.387(8) . ? C40 C41 1.403(8) . ? C41 C42 1.372(8) . ? C42 C43 1.401(9) . ? C43 C44 1.392(8) . ? C44 C45 1.386(8) . ? C46 C47 1.385(8) . ? C46 C51 1.407(8) . ? C47 C48 1.375(8) . ? C48 C49 1.389(9) . ? C49 C50 1.383(9) . ? C50 C51 1.379(8) . ? C53 N4 1.140(9) . ? C53 C52 1.464(10) . ? 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 C1 Re1 Se4 90.60(15) . . ? C1 Re1 Se2 93.13(15) . . ? Se4 Re1 Se2 176.164(18) . . ? C1 Re1 Se1 94.37(15) . . ? Se4 Re1 Se1 89.27(3) . . ? Se2 Re1 Se1 89.55(3) . . ? C1 Re1 Se3 89.62(15) . . ? Se4 Re1 Se3 90.66(3) . . ? Se2 Re1 Se3 90.26(3) . . ? Se1 Re1 Se3 176.01(2) . . ? C1 Re1 Re2 132.55(14) . 2_576 ? Se4 Re1 Re2 58.90(2) . 2_576 ? Se2 Re1 Re2 118.69(2) . 2_576 ? Se1 Re1 Re2 118.23(2) . 2_576 ? Se3 Re1 Re2 58.54(2) . 2_576 ? C1 Re1 Re3 133.95(16) . . ? Se4 Re1 Re3 119.11(2) . . ? Se2 Re1 Re3 58.49(2) . . ? Se1 Re1 Re3 118.39(2) . . ? Se3 Re1 Re3 58.34(2) . . ? Re2 Re1 Re3 60.224(14) 2_576 . ? C1 Re1 Re3 135.96(16) . 2_576 ? Se4 Re1 Re3 58.418(18) . 2_576 ? Se2 Re1 Re3 117.961(19) . 2_576 ? Se1 Re1 Re3 58.324(19) . 2_576 ? Se3 Re1 Re3 118.44(2) . 2_576 ? Re2 Re1 Re3 59.918(16) 2_576 2_576 ? Re3 Re1 Re3 89.99(2) . 2_576 ? C1 Re1 Re2 137.45(14) . . ? Se4 Re1 Re2 118.39(2) . . ? Se2 Re1 Re2 57.988(18) . . ? Se1 Re1 Re2 58.543(18) . . ? Se3 Re1 Re2 118.18(2) . . ? Re2 Re1 Re2 89.984(14) 2_576 . ? Re3 Re1 Re2 59.856(14) . . ? Re3 Re1 Re2 59.978(14) 2_576 . ? C1 Re1 Re1 177.50(14) . 2_576 ? Se4 Re1 Re1 88.43(2) . 2_576 ? Se2 Re1 Re1 87.88(2) . 2_576 ? Se1 Re1 Re1 87.930(19) . 2_576 ? Se3 Re1 Re1 88.084(19) . 2_576 ? Re2 Re1 Re1 45.125(10) 2_576 2_576 ? Re3 Re1 Re1 45.076(12) . 2_576 ? Re3 Re1 Re1 44.918(15) 2_576 2_576 ? Re2 Re1 Re1 44.859(10) . 2_576 ? C2 Re2 Se2 90.37(14) . . ? C2 Re2 Se3 93.23(14) . 2_576 ? Se2 Re2 Se3 176.356(19) . 2_576 ? C2 Re2 Se1 94.08(16) . . ? Se2 Re2 Se1 89.69(3) . . ? Se3 Re2 Se1 89.53(3) 2_576 . ? C2 Re2 Se4 90.28(16) . 2_576 ? Se2 Re2 Se4 90.22(3) . 2_576 ? Se3 Re2 Se4 90.28(3) 2_576 2_576 ? Se1 Re2 Se4 175.646(19) . 2_576 ? C2 Re2 Re1 134.50(15) . 2_576 ? Se2 Re2 Re1 118.88(2) . 2_576 ? Se3 Re2 Re1 58.57(2) 2_576 2_576 ? Se1 Re2 Re1 118.16(2) . 2_576 ? Se4 Re2 Re1 58.263(18) 2_576 2_576 ? C2 Re2 Re3 132.68(16) . . ? Se2 Re2 Re3 58.659(19) . . ? Se3 Re2 Re3 118.78(2) 2_576 . ? Se1 Re2 Re3 118.15(2) . . ? Se4 Re2 Re3 58.329(18) 2_576 . ? Re1 Re2 Re3 60.230(15) 2_576 . ? C2 Re2 Re3 137.30(16) . 2_576 ? Se2 Re2 Re3 118.45(2) . 2_576 ? Se3 Re2 Re3 58.246(19) 2_576 2_576 ? Se1 Re2 Re3 58.24(2) . 2_576 ? Se4 Re2 Re3 118.18(2) 2_576 2_576 ? Re1 Re2 Re3 59.939(15) 2_576 2_576 ? Re3 Re2 Re3 90.01(2) . 2_576 ? C2 Re2 Re1 135.40(15) . . ? Se2 Re2 Re1 58.491(18) . . ? Se3 Re2 Re1 118.208(19) 2_576 . ? Se1 Re2 Re1 58.268(18) . . ? Se4 Re2 Re1 118.202(19) 2_576 . ? Re1 Re2 Re1 90.016(14) 2_576 . ? Re3 Re2 Re1 59.892(14) . . ? Re3 Re2 Re1 59.969(15) 2_576 . ? C2 Re2 Re2 177.76(16) . 2_576 ? Se2 Re2 Re2 88.296(19) . 2_576 ? Se3 Re2 Re2 88.117(19) 2_576 2_576 ? Se1 Re2 Re2 87.72(2) . 2_576 ? Se4 Re2 Re2 87.93(2) 2_576 2_576 ? Re1 Re2 Re2 45.141(11) 2_576 2_576 ? Re3 Re2 Re2 45.098(14) . 2_576 ? Re3 Re2 Re2 44.913(13) 2_576 2_576 ? Re1 Re2 Re2 44.875(10) . 2_576 ? C3 Re3 Se3 90.55(13) . . ? C3 Re3 Se1 92.46(16) . 2_576 ? Se3 Re3 Se1 89.90(2) . 2_576 ? C3 Re3 Se4 92.82(13) . 2_576 ? Se3 Re3 Se4 176.56(2) . 2_576 ? Se1 Re3 Se4 89.25(2) 2_576 2_576 ? C3 Re3 Se2 91.70(16) . . ? Se3 Re3 Se2 90.41(2) . . ? Se1 Re3 Se2 175.83(2) 2_576 . ? Se4 Re3 Se2 90.20(2) 2_576 . ? C3 Re3 Re2 135.39(14) . . ? Se3 Re3 Re2 118.85(2) . . ? Se1 Re3 Re2 118.25(2) 2_576 . ? Se4 Re3 Re2 58.838(19) 2_576 . ? Se2 Re3 Re2 58.116(18) . . ? C3 Re3 Re1 133.78(15) . . ? Se3 Re3 Re1 58.610(19) . . ? Se1 Re3 Re1 118.42(2) 2_576 . ? Se4 Re3 Re1 119.07(2) 2_576 . ? Se2 Re3 Re1 58.451(18) . . ? Re2 Re3 Re1 60.252(16) . . ? C3 Re3 Re1 136.21(15) . 2_576 ? Se3 Re3 Re1 118.54(2) . 2_576 ? Se1 Re3 Re1 58.410(19) 2_576 2_576 ? Se4 Re3 Re1 58.289(18) 2_576 2_576 ? Se2 Re3 Re1 117.96(2) . 2_576 ? Re2 Re3 Re1 59.852(16) . 2_576 ? Re1 Re3 Re1 90.01(2) . 2_576 ? C3 Re3 Re2 134.60(14) . 2_576 ? Se3 Re3 Re2 58.491(19) . 2_576 ? Se1 Re3 Re2 58.60(2) 2_576 2_576 ? Se4 Re3 Re2 118.34(2) 2_576 2_576 ? Se2 Re3 Re2 118.26(2) . 2_576 ? Re2 Re3 Re2 89.99(2) . 2_576 ? Re1 Re3 Re2 59.837(18) . 2_576 ? Re1 Re3 Re2 60.053(14) 2_576 2_576 ? C3 Re3 Re3 178.77(14) . 2_576 ? Se3 Re3 Re3 88.31(2) . 2_576 ? Se1 Re3 Re3 88.00(2) 2_576 2_576 ? Se4 Re3 Re3 88.33(2) 2_576 2_576 ? Se2 Re3 Re3 87.85(2) . 2_576 ? Re2 Re3 Re3 45.087(13) . 2_576 ? Re1 Re3 Re3 45.082(15) . 2_576 ? Re1 Re3 Re3 44.924(12) 2_576 2_576 ? Re2 Re3 Re3 44.902(14) 2_576 2_576 ? Re3 Se1 Re1 63.27(2) 2_576 . ? Re3 Se1 Re2 63.168(19) 2_576 . ? Re1 Se1 Re2 63.19(2) . . ? Re2 Se2 Re1 63.52(2) . . ? Re2 Se2 Re3 63.22(2) . . ? Re1 Se2 Re3 63.06(2) . . ? Re3 Se3 Re2 63.264(18) . 2_576 ? Re3 Se3 Re1 63.052(18) . . ? Re2 Se3 Re1 62.887(19) 2_576 . ? Re1 Se4 Re3 63.294(19) . 2_576 ? Re1 Se4 Re2 62.84(2) . 2_576 ? Re3 Se4 Re2 62.833(19) 2_576 2_576 ? N1 C1 Re1 177.8(5) . . ? N2 C2 Re2 178.3(5) . . ? N3 C3 Re3 178.0(5) . . ? C10 P1 C4 108.4(3) . . ? C10 P1 C22 111.7(3) . . ? C4 P1 C22 108.2(3) . . ? C10 P1 C16 111.6(3) . . ? C4 P1 C16 110.5(3) . . ? C22 P1 C16 106.3(3) . . ? C5 C4 C9 119.5(5) . . ? C5 C4 P1 119.3(4) . . ? C9 C4 P1 121.2(4) . . ? C6 C5 C4 120.2(5) . . ? C5 C6 C7 120.1(6) . . ? C8 C7 C6 120.0(6) . . ? C9 C8 C7 120.2(5) . . ? C8 C9 C4 120.0(6) . . ? C11 C10 C15 119.1(5) . . ? C11 C10 P1 117.6(4) . . ? C15 C10 P1 123.2(4) . . ? C12 C11 C10 120.5(5) . . ? C11 C12 C13 120.2(5) . . ? C12 C13 C14 119.2(6) . . ? C15 C14 C13 121.2(5) . . ? C14 C15 C10 119.7(5) . . ? C21 C16 C17 119.8(5) . . ? C21 C16 P1 120.2(4) . . ? C17 C16 P1 120.0(4) . . ? C16 C17 C18 119.5(6) . . ? C19 C18 C17 118.9(6) . . ? C20 C19 C18 121.4(5) . . ? C19 C20 C21 119.9(6) . . ? C16 C21 C20 120.5(6) . . ? C23 C22 C27 120.4(5) . . ? C23 C22 P1 122.3(5) . . ? C27 C22 P1 117.1(4) . . ? C24 C23 C22 119.2(6) . . ? C23 C24 C25 121.0(6) . . ? C24 C25 C26 120.7(6) . . ? C25 C26 C27 118.9(6) . . ? C26 C27 C22 120.0(5) . . ? C40 P2 C28 108.8(3) . . ? C40 P2 C46 108.7(3) . . ? C28 P2 C46 111.8(3) . . ? C40 P2 C34 107.4(2) . . ? C28 P2 C34 112.0(3) . . ? C46 P2 C34 108.0(3) . . ? C29 C28 C33 118.6(6) . . ? C29 C28 P2 122.1(4) . . ? C33 C28 P2 119.3(4) . . ? C30 C29 C28 120.5(5) . . ? C29 C30 C31 120.0(5) . . ? C30 C31 C32 120.0(6) . . ? C33 C32 C31 120.2(5) . . ? C32 C33 C28 120.6(5) . . ? C35 C34 C39 120.1(5) . . ? C35 C34 P2 119.2(4) . . ? C39 C34 P2 120.5(4) . . ? C34 C35 C36 120.4(5) . . ? C37 C36 C35 118.4(6) . . ? C38 C37 C36 120.7(6) . . ? C37 C38 C39 121.1(5) . . ? C38 C39 C34 119.3(6) . . ? C45 C40 C41 119.5(5) . . ? C45 C40 P2 121.7(4) . . ? C41 C40 P2 118.7(5) . . ? C42 C41 C40 120.1(6) . . ? C41 C42 C43 120.3(5) . . ? C44 C43 C42 119.9(5) . . ? C45 C44 C43 119.5(5) . . ? C44 C45 C40 120.8(5) . . ? C47 C46 C51 119.6(5) . . ? C47 C46 P2 120.2(4) . . ? C51 C46 P2 119.8(4) . . ? C48 C47 C46 120.5(5) . . ? C47 C48 C49 120.0(6) . . ? C50 C49 C48 120.0(5) . . ? C51 C50 C49 120.6(5) . . ? C50 C51 C46 119.3(6) . . ? N4 C53 C52 179.6(9) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 1.457 _refine_diff_density_min -1.360 _refine_diff_density_rms 0.216 ######################################################################### #======END