# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Kuang-Lieh Lu' _publ_contact_author_email LU@CHEM.SINICA.EDU.TW _publ_section_title ; Rhenium-based molecular rectangles with large inner cavity and high shape selectivity toward benzene molecule ; loop_ _publ_author_name 'Kuang-Lieh Lu.' 'Rong-Tang Liao.' 'Hsiu-Mei Lin.' 'Yen-Hsiang Liu.' ; T.Rajendran ; 'M Sathiyendiran' 'P Thanasekaran' 'Chen-Chuan Tsai.' ; Tien-Wen Tseng ; 'Woei-Chyuan Yang.' # Attachment '1a-mesitylene_ic9448-revised.cif' data_ic9448 _database_code_depnum_ccdc_archive 'CCDC 678660' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H28 Cl4 N4 O20 Re4' _chemical_formula_weight 1927.39 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' O O 0.0106 0.0060 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0200(2) _cell_length_b 18.4422(5) _cell_length_c 14.9444(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.0179(11) _cell_angle_gamma 90.00 _cell_volume 2946.75(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 8.448 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.367 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18829 _diffrn_reflns_av_R_equivalents 0.0909 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6751 _reflns_number_gt 4466 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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. In order to refine the dis ordered mesitylene molecule, the following distances were restrained: C26- C29 = C24-C28 = C24-C28' = 1.54 and C23-C27 = 2.65. ; _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^)+(0.0638P)^2^+16.6144P] 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 0.00153(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6751 _refine_ls_number_parameters 373 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 0.14782(4) 0.59837(3) 0.07205(3) 0.04179(18) Uani 1 1 d . . . Re2 Re 0.65767(4) 0.27333(3) 0.15669(4) 0.0494(2) Uani 1 1 d . . . Cl1 Cl 0.1975(3) 0.3293(2) 0.1510(3) 0.0704(10) Uani 1 1 d . . . Cl2 Cl 0.6219(3) 0.55091(19) 0.1120(2) 0.0549(8) Uani 1 1 d . . . O1 O -0.1302(7) 0.6083(5) 0.0695(6) 0.053(2) Uani 1 1 d . . . O2 O 0.1405(10) 0.7632(5) 0.0447(8) 0.070(3) Uani 1 1 d . . . O3 O 0.0806(7) 0.5731(5) -0.1365(7) 0.056(2) Uani 1 1 d . . . O4 O 0.5818(10) 0.2396(7) -0.0521(8) 0.087(3) Uani 1 1 d . . . O5 O 0.9366(9) 0.2533(6) 0.1724(8) 0.071(3) Uani 1 1 d . . . O6 O 0.6528(10) 0.1095(6) 0.1916(9) 0.085(3) Uani 1 1 d . . . O7 O 0.3444(7) 0.5776(4) 0.0887(6) 0.0436(19) Uani 1 1 d . . . O8 O 0.1731(6) 0.4858(4) 0.1049(5) 0.0421(18) Uani 1 1 d . . . O9 O 0.6399(7) 0.3889(5) 0.1372(6) 0.048(2) Uani 1 1 d . . . O10 O 0.4667(7) 0.2981(4) 0.1539(5) 0.0448(19) Uani 1 1 d . . . N1 N 0.1976(9) 0.6082(5) 0.2202(7) 0.044(2) Uani 1 1 d . . . N2 N 0.3093(9) 0.6951(6) 0.6972(7) 0.051(3) Uani 1 1 d . . . C1 C -0.0250(11) 0.6046(7) 0.0686(8) 0.044(3) Uani 1 1 d . . . C2 C 0.1441(11) 0.7001(8) 0.0545(9) 0.050(3) Uani 1 1 d . . . C3 C 0.1077(9) 0.5820(7) -0.0577(9) 0.041(3) Uani 1 1 d . . . C4 C 0.6167(11) 0.2535(8) 0.0276(10) 0.052(3) Uani 1 1 d . . . C5 C 0.8290(12) 0.2615(8) 0.1653(9) 0.055(3) Uani 1 1 d . . . C6 C 0.6547(12) 0.1734(10) 0.1804(9) 0.062(4) Uani 1 1 d . . . C7 C 0.3820(10) 0.5136(7) 0.1042(8) 0.039(3) Uani 1 1 d . . . C8 C 0.2811(10) 0.4589(7) 0.1132(8) 0.041(3) Uani 1 1 d . . . C9 C 0.3124(11) 0.3864(7) 0.1356(8) 0.043(3) Uani 1 1 d . . . C10 C 0.4317(10) 0.3638(6) 0.1383(7) 0.035(2) Uani 1 1 d . . . C11 C 0.5320(10) 0.4171(7) 0.1286(7) 0.041(3) Uani 1 1 d . . . C12 C 0.5038(9) 0.4896(6) 0.1160(7) 0.037(2) Uani 1 1 d . . . C13 C 0.3031(11) 0.6443(7) 0.2679(9) 0.050(3) Uani 1 1 d . . . H13A H 0.3599 0.6623 0.2345 0.060 Uiso 1 1 calc R . . C14 C 0.3297(11) 0.6557(7) 0.3613(9) 0.053(3) Uani 1 1 d . . . H14A H 0.4059 0.6784 0.3917 0.064 Uiso 1 1 calc R . . C15 C 0.2469(11) 0.6344(7) 0.4105(8) 0.048(3) Uani 1 1 d . A . C16 C 0.1458(13) 0.5939(8) 0.3656(9) 0.061(4) Uani 1 1 d . . . H16A H 0.0899 0.5740 0.3985 0.073 Uiso 1 1 calc R . . C17 C 0.1273(14) 0.5830(8) 0.2750(9) 0.058(4) Uani 1 1 d . . . H17A H 0.0569 0.5544 0.2464 0.069 Uiso 1 1 calc R . . C18 C 0.361(2) 0.7307(15) 0.6460(16) 0.053(6) Uiso 0.59(3) 1 d P A 1 H18A H 0.4116 0.7714 0.6692 0.064 Uiso 0.59(3) 1 calc PR A 1 C19 C 0.343(3) 0.7093(16) 0.5528(17) 0.059(7) Uiso 0.59(3) 1 d P A 1 H19A H 0.3854 0.7362 0.5153 0.071 Uiso 0.59(3) 1 calc PR A 1 C18' C 0.402(4) 0.699(2) 0.647(2) 0.056(9) Uiso 0.41(3) 1 d P A 2 H18B H 0.4809 0.7184 0.6786 0.067 Uiso 0.41(3) 1 calc PR A 2 C19' C 0.390(3) 0.6776(18) 0.560(2) 0.047(8) Uiso 0.41(3) 1 d P A 2 H19B H 0.4578 0.6788 0.5314 0.056 Uiso 0.41(3) 1 calc PR A 2 C20 C 0.2704(11) 0.6531(7) 0.5130(8) 0.050(3) Uani 1 1 d . . . C21 C 0.202(2) 0.6199(13) 0.5724(15) 0.047(6) Uiso 0.59(3) 1 d P A 1 H21A H 0.1382 0.5854 0.5481 0.057 Uiso 0.59(3) 1 calc PR A 1 C22 C 0.228(2) 0.6380(14) 0.6654(15) 0.046(6) Uiso 0.59(3) 1 d P A 1 H22A H 0.1903 0.6118 0.7065 0.055 Uiso 0.59(3) 1 calc PR A 1 C21' C 0.169(6) 0.658(3) 0.545(4) 0.081(18) Uiso 0.41(3) 1 d P A 2 H21B H 0.0860 0.6504 0.5097 0.097 Uiso 0.41(3) 1 calc PR A 2 C22' C 0.203(4) 0.674(3) 0.639(3) 0.077(13) Uiso 0.41(3) 1 d P A 2 H22B H 0.1351 0.6700 0.6674 0.093 Uiso 0.41(3) 1 calc PR A 2 C23 C 0.542(3) 0.522(2) 0.513(3) 0.094(11) Uiso 0.50 1 d PD . . H23A H 0.6094 0.5551 0.5374 0.113 Uiso 0.50 1 d P . . C24 C 0.534(2) 0.5110(12) 0.4316(14) 0.104(6) Uiso 1 1 d D . . C25 C 0.408(3) 0.4744(19) 0.372(2) 0.077(9) Uiso 0.50 1 d P . . H25A H 0.3847 0.4714 0.3040 0.093 Uiso 0.50 1 d P . . C26 C 0.317(3) 0.4424(19) 0.407(2) 0.080(9) Uiso 0.50 1 d PD . . C27 C 0.334(3) 0.4503(18) 0.511(2) 0.082(9) Uiso 0.50 1 d PD . . H27A H 0.2723 0.4346 0.5405 0.098 Uiso 0.50 1 d P . . C28 C 0.606(4) 0.541(2) 0.364(3) 0.102(12) Uiso 0.50 1 d PD . 1 H28A H 0.6764 0.5591 0.3855 0.154 Uiso 0.50 1 d P B 1 H28B H 0.6169 0.4956 0.3195 0.154 Uiso 0.50 1 d P C 1 H28C H 0.5481 0.5705 0.3138 0.154 Uiso 0.50 1 d P D 1 C28' C 0.529(5) 0.508(3) 0.3281(17) 0.136(18) Uiso 0.50 1 d PD . 2 H28D H 0.5997 0.5276 0.3143 0.204 Uiso 0.50 1 d P E 2 H28E H 0.5185 0.4572 0.3074 0.204 Uiso 0.50 1 d P F 2 H28F H 0.4536 0.5334 0.2938 0.204 Uiso 0.50 1 d P G 2 C29 C 0.190(3) 0.408(2) 0.359(3) 0.122(16) Uiso 0.50 1 d PD . . H29A H 0.1894 0.4042 0.2929 0.183 Uiso 0.50 1 d P . . H29B H 0.1869 0.3599 0.3819 0.183 Uiso 0.50 1 d P . . H29C H 0.1249 0.4368 0.3665 0.183 Uiso 0.50 1 d P . . 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 0.0301(3) 0.0456(3) 0.0524(3) -0.0013(2) 0.0154(2) -0.0014(2) Re2 0.0352(3) 0.0582(4) 0.0559(3) -0.0034(3) 0.0136(2) 0.0077(2) Cl1 0.0465(18) 0.053(2) 0.118(3) 0.011(2) 0.033(2) -0.0024(16) Cl2 0.0346(15) 0.071(2) 0.0621(19) -0.0057(17) 0.0173(14) -0.0116(15) O1 0.029(4) 0.068(6) 0.064(6) 0.004(5) 0.015(4) 0.002(4) O2 0.072(7) 0.046(6) 0.106(8) 0.006(5) 0.047(6) 0.005(5) O3 0.031(4) 0.071(6) 0.071(6) 0.003(5) 0.020(4) 0.004(4) O4 0.062(7) 0.123(10) 0.072(8) -0.019(7) 0.007(6) 0.004(7) O5 0.040(5) 0.079(7) 0.100(8) 0.000(6) 0.025(5) 0.012(5) O6 0.063(7) 0.067(7) 0.121(10) 0.011(7) 0.014(6) 0.012(6) O7 0.032(4) 0.045(5) 0.057(5) -0.004(4) 0.017(4) -0.004(4) O8 0.023(4) 0.045(5) 0.058(5) -0.006(4) 0.009(3) -0.002(3) O9 0.029(4) 0.061(5) 0.057(5) -0.003(4) 0.018(4) 0.004(4) O10 0.037(4) 0.048(5) 0.050(5) -0.003(4) 0.013(4) 0.004(4) N1 0.041(5) 0.046(6) 0.051(6) -0.006(5) 0.022(5) -0.003(5) N2 0.035(5) 0.058(7) 0.056(6) -0.001(5) 0.006(5) 0.005(5) C1 0.042(7) 0.049(7) 0.044(6) 0.001(6) 0.017(5) -0.012(6) C2 0.037(7) 0.062(9) 0.054(8) -0.007(7) 0.015(6) -0.003(6) C3 0.020(5) 0.055(7) 0.045(7) 0.011(6) 0.003(5) 0.004(5) C4 0.034(6) 0.068(9) 0.056(8) -0.001(7) 0.015(6) 0.013(6) C5 0.042(7) 0.062(9) 0.061(8) 0.002(7) 0.013(6) 0.014(6) C6 0.036(7) 0.093(12) 0.054(8) -0.006(8) 0.008(6) -0.011(8) C7 0.028(6) 0.047(7) 0.044(6) -0.003(6) 0.011(5) -0.007(5) C8 0.028(6) 0.059(8) 0.041(6) -0.006(6) 0.017(5) -0.006(5) C9 0.035(6) 0.050(7) 0.046(7) 0.002(6) 0.011(5) -0.004(5) C10 0.032(6) 0.045(7) 0.026(5) -0.001(5) 0.007(4) 0.007(5) C11 0.039(6) 0.056(7) 0.029(5) -0.011(5) 0.012(5) -0.002(5) C12 0.028(5) 0.043(6) 0.042(6) -0.002(5) 0.010(5) -0.005(5) C13 0.038(6) 0.059(8) 0.057(8) -0.009(6) 0.017(6) -0.007(6) C14 0.044(7) 0.052(8) 0.065(9) -0.015(7) 0.019(6) -0.019(6) C15 0.047(7) 0.056(8) 0.045(7) -0.010(6) 0.018(6) -0.007(6) C16 0.051(8) 0.083(11) 0.049(8) 0.000(7) 0.011(6) -0.012(7) C17 0.063(9) 0.071(9) 0.042(7) 0.007(7) 0.018(6) -0.020(7) C20 0.033(6) 0.067(9) 0.048(7) -0.008(6) 0.010(5) 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 C2 1.894(15) . ? Re1 C1 1.896(12) . ? Re1 C3 1.906(13) . ? Re1 O8 2.135(8) . ? Re1 O7 2.154(7) . ? Re1 N1 2.156(10) . ? Re2 C5 1.874(13) . ? Re2 C6 1.878(18) . ? Re2 C4 1.908(14) . ? Re2 O10 2.144(8) . ? Re2 O9 2.153(9) . ? Re2 N2 2.203(10) 3_666 ? Cl1 C9 1.704(12) . ? Cl2 C12 1.736(11) . ? O1 C1 1.164(14) . ? O2 C2 1.171(16) . ? O3 C3 1.153(14) . ? O4 C4 1.187(16) . ? O5 C5 1.174(15) . ? O6 C6 1.192(19) . ? O7 C7 1.254(14) . ? O8 C8 1.268(13) . ? O9 C11 1.276(13) . ? O10 C10 1.275(13) . ? N1 C17 1.339(15) . ? N1 C13 1.379(15) . ? N2 C18 1.25(3) . ? N2 C22' 1.34(4) . ? N2 C22 1.39(2) . ? N2 C18' 1.41(4) . ? N2 Re2 2.203(10) 3_666 ? C7 C12 1.384(15) . ? C7 C8 1.531(15) . ? C8 C9 1.402(17) . ? C9 C10 1.370(15) . ? C10 C11 1.512(16) . ? C11 C12 1.374(16) . ? C13 C14 1.371(17) . ? C14 C15 1.361(16) . ? C15 C16 1.373(17) . ? C15 C20 1.529(17) . ? C16 C17 1.335(18) . ? C18 C19 1.42(3) . ? C19 C20 1.36(3) . ? C18' C19' 1.34(4) . ? C19' C20 1.41(3) . ? C20 C21' 1.32(6) . ? C20 C21 1.44(3) . ? C21 C22 1.39(3) . ? C21' C22' 1.39(6) . ? C23 C24 1.22(4) . ? C23 C23 1.23(5) 3_666 ? C23 C24 1.45(4) 3_666 ? C23 C27 1.58(5) 3_666 ? C23 C25 1.67(5) 3_666 ? C23 C26 1.83(4) 3_666 ? C24 C23 1.45(4) 3_666 ? C24 C28 1.536(10) . ? C24 C28' 1.537(10) . ? C24 C25 1.60(4) . ? C24 C27 1.66(3) 3_666 ? C25 C26 1.38(4) . ? C25 C23 1.67(5) 3_666 ? C25 C28' 1.74(6) . ? C26 C27 1.53(4) . ? C26 C29 1.545(10) . ? C26 C23 1.83(4) 3_666 ? C27 C23 1.58(5) 3_666 ? C27 C24 1.66(3) 3_666 ? C27 C28 1.83(5) 3_666 ? C28 C27 1.83(5) 3_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C1 87.1(5) . . ? C2 Re1 C3 91.4(5) . . ? C1 Re1 C3 89.9(5) . . ? C2 Re1 O8 172.8(4) . . ? C1 Re1 O8 98.0(4) . . ? C3 Re1 O8 93.7(4) . . ? C2 Re1 O7 100.3(4) . . ? C1 Re1 O7 171.6(4) . . ? C3 Re1 O7 93.9(4) . . ? O8 Re1 O7 74.3(3) . . ? C2 Re1 N1 92.9(5) . . ? C1 Re1 N1 91.6(4) . . ? C3 Re1 N1 175.5(4) . . ? O8 Re1 N1 81.9(3) . . ? O7 Re1 N1 84.1(3) . . ? C5 Re2 C6 86.3(6) . . ? C5 Re2 C4 92.0(5) . . ? C6 Re2 C4 89.5(6) . . ? C5 Re2 O10 173.8(5) . . ? C6 Re2 O10 98.7(5) . . ? C4 Re2 O10 91.8(4) . . ? C5 Re2 O9 100.5(5) . . ? C6 Re2 O9 172.4(5) . . ? C4 Re2 O9 93.5(5) . . ? O10 Re2 O9 74.3(3) . . ? C5 Re2 N2 92.3(5) . 3_666 ? C6 Re2 N2 94.5(5) . 3_666 ? C4 Re2 N2 174.3(4) . 3_666 ? O10 Re2 N2 83.6(3) . 3_666 ? O9 Re2 N2 82.0(4) . 3_666 ? C7 O7 Re1 117.8(7) . . ? C8 O8 Re1 118.0(7) . . ? C11 O9 Re2 118.1(8) . . ? C10 O10 Re2 117.3(7) . . ? C17 N1 C13 113.1(11) . . ? C17 N1 Re1 123.9(9) . . ? C13 N1 Re1 123.0(8) . . ? C18 N2 C22' 102(2) . . ? C18 N2 C22 122.8(17) . . ? C22' N2 C22 33.7(19) . . ? C18 N2 C18' 31.6(15) . . ? C22' N2 C18' 108(2) . . ? C22 N2 C18' 110.5(19) . . ? C18 N2 Re2 118.6(13) . 3_666 ? C22' N2 Re2 129(2) . 3_666 ? C22 N2 Re2 118.5(11) . 3_666 ? C18' N2 Re2 123.0(16) . 3_666 ? O1 C1 Re1 177.8(10) . . ? O2 C2 Re1 178.8(11) . . ? O3 C3 Re1 178.1(10) . . ? O4 C4 Re2 174.6(11) . . ? O5 C5 Re2 178.6(13) . . ? O6 C6 Re2 177.2(13) . . ? O7 C7 C12 126.3(10) . . ? O7 C7 C8 115.0(10) . . ? C12 C7 C8 118.7(11) . . ? O8 C8 C9 124.6(10) . . ? O8 C8 C7 114.7(11) . . ? C9 C8 C7 120.5(10) . . ? C10 C9 C8 118.4(10) . . ? C10 C9 Cl1 123.2(10) . . ? C8 C9 Cl1 118.3(9) . . ? O10 C10 C9 122.6(11) . . ? O10 C10 C11 116.1(9) . . ? C9 C10 C11 121.2(10) . . ? O9 C11 C12 125.9(11) . . ? O9 C11 C10 114.1(10) . . ? C12 C11 C10 119.9(10) . . ? C11 C12 C7 120.6(10) . . ? C11 C12 Cl2 119.4(8) . . ? C7 C12 Cl2 119.9(9) . . ? C14 C13 N1 123.1(11) . . ? C15 C14 C13 120.0(11) . . ? C14 C15 C16 117.6(11) . . ? C14 C15 C20 120.2(11) . . ? C16 C15 C20 122.2(11) . . ? C17 C16 C15 119.0(13) . . ? C16 C17 N1 126.8(13) . . ? N2 C18 C19 119(2) . . ? C20 C19 C18 125(2) . . ? C19' C18' N2 126(3) . . ? C18' C19' C20 116(3) . . ? C21' C20 C19 105(3) . . ? C21' C20 C19' 125(3) . . ? C19 C20 C19' 32.2(14) . . ? C21' C20 C21 35(3) . . ? C19 C20 C21 113.5(17) . . ? C19' C20 C21 113.4(18) . . ? C21' C20 C15 115(3) . . ? C19 C20 C15 123.4(15) . . ? C19' C20 C15 118.9(16) . . ? C21 C20 C15 122.4(13) . . ? C22 C21 C20 120.3(19) . . ? C21 C22 N2 119(2) . . ? C20 C21' C22' 110(5) . . ? N2 C22' C21' 134(4) . . ? C24 C23 C23 72(4) . 3_666 ? C24 C23 C24 126(2) . 3_666 ? C23 C23 C24 54(3) 3_666 3_666 ? C24 C23 C27 71(2) . 3_666 ? C23 C23 C27 140(5) 3_666 3_666 ? C24 C23 C27 157(3) 3_666 3_666 ? C24 C23 C25 164(4) . 3_666 ? C23 C23 C25 113(4) 3_666 3_666 ? C24 C23 C25 61(2) 3_666 3_666 ? C27 C23 C25 98(2) 3_666 3_666 ? C24 C23 C26 124(3) . 3_666 ? C23 C23 C26 155(5) 3_666 3_666 ? C24 C23 C26 107(3) 3_666 3_666 ? C27 C23 C26 52.8(19) 3_666 3_666 ? C25 C23 C26 46.0(17) 3_666 3_666 ? C23 C24 C23 54(2) . 3_666 ? C23 C24 C28 133(3) . . ? C23 C24 C28 173(3) 3_666 . ? C23 C24 C28' 172(3) . . ? C23 C24 C28' 133(3) 3_666 . ? C28 C24 C28' 41(2) . . ? C23 C24 C25 119(2) . . ? C23 C24 C25 66(2) 3_666 . ? C28 C24 C25 107(2) . . ? C28' C24 C25 67(3) . . ? C23 C24 C27 64(2) . 3_666 ? C23 C24 C27 117(2) 3_666 3_666 ? C28 C24 C27 70(2) . 3_666 ? C28' C24 C27 110(3) . 3_666 ? C25 C24 C27 177(2) . 3_666 ? C26 C25 C24 125(3) . . ? C26 C25 C23 73(2) . 3_666 ? C24 C25 C23 52.3(15) . 3_666 ? C26 C25 C28' 175(4) . . ? C24 C25 C28' 54.6(15) . . ? C23 C25 C28' 106(2) 3_666 . ? C25 C26 C27 116(3) . . ? C25 C26 C29 132(3) . . ? C27 C26 C29 112(3) . . ? C25 C26 C23 61(2) . 3_666 ? C27 C26 C23 55(2) . 3_666 ? C29 C26 C23 167(3) . 3_666 ? C26 C27 C23 72(2) . 3_666 ? C26 C27 C24 116(2) . 3_666 ? C23 C27 C24 44.2(16) 3_666 3_666 ? C26 C27 C28 166(2) . 3_666 ? C23 C27 C28 95(2) 3_666 3_666 ? C24 C27 C28 51.9(12) 3_666 3_666 ? C24 C28 C27 58.2(16) . 3_666 ? C24 C28' C25 58.3(19) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.127 _refine_diff_density_min -1.595 _refine_diff_density_rms 0.304 # Attachment '2a-2benzene_i7252revised.cif' data_i7252 _database_code_depnum_ccdc_archive 'CCDC 678661' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H36 N4 O20 Re4' _chemical_formula_weight 1925.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x, -y, -z' '-x+1/2, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x-1/2, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x, -y+1/2, z-1/2' _cell_length_a 12.277(3) _cell_length_b 19.785(4) _cell_length_c 26.044(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6326(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 7.707 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25744 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2944 _reflns_number_gt 1865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2944 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _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 0.0000 1.08136(3) 0.214606(19) 0.0357(2) Uani 1 2 d S . . Re2 Re 0.0000 0.66786(3) 0.51941(2) 0.0366(2) Uani 1 2 d S . . O1 O 0.1124(4) 1.1302(3) 0.2617(2) 0.0316(15) Uani 1 1 d . . . O2 O 0.1140(5) 0.7164(3) 0.5671(2) 0.0367(17) Uani 1 1 d . . . O3 O 0.0000 1.1889(6) 0.1308(4) 0.056(3) Uani 1 2 d S . . O4 O -0.1704(6) 1.0031(4) 0.1543(2) 0.057(2) Uani 1 1 d . . . O5 O 0.0000 0.5305(6) 0.5714(4) 0.064(4) Uani 1 2 d S . . O6 O -0.1746(6) 0.6099(4) 0.4483(3) 0.056(2) Uani 1 1 d . . . N1 N 0.0000 1.0102(6) 0.2806(4) 0.037(3) Uani 1 2 d S . . N2 N 0.0000 0.7682(5) 0.4797(3) 0.029(3) Uani 1 2 d S . . C1 C 0.0898(8) 0.9903(6) 0.3016(4) 0.055(3) Uani 1 1 d . . . H1 H 0.1551 1.0055 0.2878 0.065 Uiso 1 1 calc R . . C2 C 0.0938(8) 0.9480(6) 0.3430(4) 0.058(3) Uani 1 1 d . . . H2 H 0.1610 0.9349 0.3561 0.069 Uiso 1 1 calc R . . C3 C 0.0000 0.9246(7) 0.3656(5) 0.033(3) Uani 1 2 d S . . C4 C 0.0939(8) 0.7949(5) 0.4632(3) 0.037(2) Uani 1 1 d . . . H4 H 0.1595 0.7779 0.4755 0.044 Uiso 1 1 calc R . . C5 C 0.0947(8) 0.8471(5) 0.4283(3) 0.041(3) Uani 1 1 d . . . H5 H 0.1616 0.8646 0.4181 0.049 Uiso 1 1 calc R . . C6 C 0.0000 0.8751(7) 0.4073(5) 0.033(3) Uani 1 2 d S . . C7 C 0.1002(6) 1.1655(5) 0.3025(3) 0.032(2) Uani 1 1 d . . . C8 C 0.2008(8) 1.1846(5) 0.3268(3) 0.038(2) Uani 1 1 d . . . H8 H 0.2667 1.1710 0.3124 0.045 Uiso 1 1 calc R . . C9 C 0.2008(7) 1.2212(5) 0.3692(3) 0.042(3) Uani 1 1 d . . . H9 H 0.2670 1.2327 0.3843 0.051 Uiso 1 1 calc R . . C10 C 0.1016(7) 1.2439(5) 0.3929(3) 0.038(3) Uani 1 1 d . . . C11 C 0.0000 1.2241(7) 0.3714(4) 0.030(3) Uani 1 2 d S . . C12 C 0.0000 1.1834(7) 0.3248(5) 0.034(3) Uani 1 2 d S . . C13 C 0.0000 1.1478(8) 0.1622(5) 0.039(4) Uani 1 2 d S . . C14 C -0.1059(8) 1.0334(6) 0.1782(4) 0.046(3) Uani 1 1 d . . . C15 C 0.0000 0.5896(12) 0.5530(6) 0.071(6) Uani 1 2 d S . . C16 C -0.1070(9) 0.6317(5) 0.4756(4) 0.045(3) Uani 1 1 d . . . C17 C 0.0541(10) 0.9579(6) 0.5336(4) 0.076(4) Uani 1 1 d . . . H17 H 0.0920 0.9299 0.5559 0.091 Uiso 1 1 calc R . . C18 C 0.1105(16) 1.0000 0.5000 0.080(6) Uani 1 2 d S . . H18 H 0.1862 1.0000 0.5000 0.096 Uiso 1 2 calc SR . . C21 C 1.0000 0.8696(14) 0.1949(10) 0.041(7) Uiso 0.50 2 d SP . . C22 C 0.916(3) 0.8433(19) 0.2290(14) 0.024(9) Uiso 0.25 1 d P . . C23 C 0.9457(13) 0.8040(8) 0.2726(6) 0.027(4) Uiso 0.50 1 d P . . C24 C 0.863(3) 0.8176(17) 0.2447(13) 0.026(9) Uiso 0.25 1 d P . . C25 C 1.103(3) 0.8553(18) 0.2042(14) 0.025(9) Uiso 0.25 1 d P . . 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 0.0221(3) 0.0625(5) 0.0225(3) -0.0051(3) 0.000 0.000 Re2 0.0349(4) 0.0497(4) 0.0254(3) -0.0028(3) 0.000 0.000 O1 0.016(4) 0.060(5) 0.019(3) -0.003(3) 0.003(3) -0.003(3) O2 0.024(4) 0.057(5) 0.029(4) -0.007(3) -0.002(3) 0.003(3) O3 0.050(7) 0.087(9) 0.029(6) -0.005(6) 0.000 0.000 O4 0.034(5) 0.095(6) 0.043(4) -0.023(4) 0.002(3) -0.009(4) O5 0.072(9) 0.067(9) 0.054(7) -0.001(6) 0.000 0.000 O6 0.049(5) 0.068(6) 0.051(5) -0.005(4) -0.011(4) -0.010(4) N1 0.020(7) 0.041(8) 0.050(7) -0.010(6) 0.000 0.000 N2 0.033(7) 0.036(7) 0.018(5) -0.007(5) 0.000 0.000 C1 0.023(6) 0.080(9) 0.061(7) 0.032(7) 0.017(5) 0.012(6) C2 0.013(6) 0.083(9) 0.077(8) 0.024(7) 0.002(5) 0.004(5) C3 0.022(8) 0.044(10) 0.034(8) -0.002(7) 0.000 0.000 C4 0.027(6) 0.043(7) 0.040(6) -0.004(5) -0.004(5) 0.001(5) C5 0.033(6) 0.046(7) 0.044(6) -0.004(5) 0.004(5) -0.006(5) C6 0.015(7) 0.043(9) 0.041(8) -0.007(7) 0.000 0.000 C7 0.008(5) 0.065(7) 0.025(5) 0.003(5) -0.005(4) 0.006(5) C8 0.032(6) 0.058(7) 0.022(5) -0.010(5) 0.003(5) 0.003(5) C9 0.015(6) 0.075(8) 0.037(6) -0.004(5) -0.001(5) -0.003(5) C10 0.043(7) 0.051(7) 0.021(5) -0.004(5) -0.004(4) -0.002(5) C11 0.019(8) 0.055(10) 0.017(7) -0.001(6) 0.000 0.000 C12 0.023(8) 0.054(10) 0.025(7) -0.010(7) 0.000 0.000 C13 0.028(9) 0.068(12) 0.021(8) 0.009(7) 0.000 0.000 C14 0.032(7) 0.077(9) 0.028(5) -0.010(6) 0.008(5) -0.008(6) C15 0.023(9) 0.15(2) 0.043(10) -0.055(12) 0.000 0.000 C16 0.051(8) 0.045(7) 0.039(6) 0.010(5) 0.007(5) 0.007(6) C17 0.085(11) 0.076(10) 0.065(8) -0.027(7) -0.003(7) 0.003(7) C18 0.072(14) 0.069(15) 0.099(15) -0.049(13) 0.000 0.000 _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 C14 1.867(11) . ? Re1 C14 1.867(11) 11 ? Re1 C13 1.894(14) . ? Re1 O1 2.083(6) . ? Re1 O1 2.083(6) 11 ? Re1 N1 2.222(11) . ? Re2 C15 1.78(2) . ? Re2 C16 1.882(12) . ? Re2 C16 1.882(12) 11 ? Re2 O2 2.103(6) . ? Re2 O2 2.103(6) 11 ? Re2 N2 2.239(10) . ? O1 C7 1.282(10) . ? O2 C10 1.314(9) 3_576 ? O3 C13 1.155(15) . ? O4 C14 1.173(10) . ? O5 C15 1.26(2) . ? O6 C16 1.174(11) . ? N1 C1 1.292(11) . ? N1 C1 1.292(11) 11 ? N2 C4 1.338(10) 11 ? N2 C4 1.338(10) . ? C1 C2 1.364(13) . ? C2 C3 1.374(12) . ? C3 C2 1.374(12) 11 ? C3 C6 1.461(18) . ? C4 C5 1.377(12) . ? C5 C6 1.399(11) . ? C6 C5 1.399(11) 11 ? C7 C12 1.405(10) . ? C7 C8 1.439(12) . ? C8 C9 1.322(11) . ? C9 C10 1.437(12) . ? C10 O2 1.314(9) 3_576 ? C10 C11 1.422(10) . ? C11 C10 1.422(10) 11 ? C11 C12 1.456(17) . ? C12 C7 1.405(10) 11 ? C17 C17 1.33(3) 11 ? C17 C18 1.392(14) . ? C18 C17 1.392(14) 3_576 ? C21 C25 1.32(4) . ? C21 C25 1.32(4) 11_755 ? C21 C22 1.46(4) . ? C21 C22 1.46(4) 11_755 ? C22 C25 0.73(4) 11_755 ? C22 C24 0.92(4) . ? C22 C23 1.42(4) . ? C23 C24 1.28(4) . ? C23 C23 1.33(3) 11_755 ? C24 C25 1.36(5) 11_755 ? C25 C22 0.73(4) 11_755 ? C25 C24 1.36(5) 11_755 ? 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 C14 Re1 C14 88.3(6) . 11 ? C14 Re1 C13 89.2(4) . . ? C14 Re1 C13 89.2(4) 11 . ? C14 Re1 O1 174.4(3) . . ? C14 Re1 O1 94.2(3) 11 . ? C13 Re1 O1 95.8(4) . . ? C14 Re1 O1 94.2(3) . 11 ? C14 Re1 O1 174.4(3) 11 11 ? C13 Re1 O1 95.8(4) . 11 ? O1 Re1 O1 83.0(3) . 11 ? C14 Re1 N1 94.1(4) . . ? C14 Re1 N1 94.1(4) 11 . ? C13 Re1 N1 175.4(5) . . ? O1 Re1 N1 80.7(3) . . ? O1 Re1 N1 80.7(3) 11 . ? C15 Re2 C16 88.1(4) . . ? C15 Re2 C16 88.1(4) . 11 ? C16 Re2 C16 88.5(6) . 11 ? C15 Re2 O2 96.1(4) . . ? C16 Re2 O2 175.2(4) . . ? C16 Re2 O2 93.9(3) 11 . ? C15 Re2 O2 96.1(4) . 11 ? C16 Re2 O2 93.9(3) . 11 ? C16 Re2 O2 175.2(4) 11 11 ? O2 Re2 O2 83.4(3) . 11 ? C15 Re2 N2 178.0(5) . . ? C16 Re2 N2 93.3(3) . . ? C16 Re2 N2 93.3(3) 11 . ? O2 Re2 N2 82.4(2) . . ? O2 Re2 N2 82.4(2) 11 . ? C7 O1 Re1 131.6(5) . . ? C10 O2 Re2 131.6(5) 3_576 . ? C1 N1 C1 117.1(13) . 11 ? C1 N1 Re1 121.4(6) . . ? C1 N1 Re1 121.4(6) 11 . ? C4 N2 C4 119.0(12) 11 . ? C4 N2 Re2 119.8(6) 11 . ? C4 N2 Re2 119.8(6) . . ? N1 C1 C2 123.5(10) . . ? C1 C2 C3 121.0(10) . . ? C2 C3 C2 113.9(13) 11 . ? C2 C3 C6 123.0(7) 11 . ? C2 C3 C6 123.0(7) . . ? N2 C4 C5 120.9(9) . . ? C4 C5 C6 123.3(10) . . ? C5 C6 C5 112.4(13) 11 . ? C5 C6 C3 123.7(6) 11 . ? C5 C6 C3 123.7(6) . . ? O1 C7 C12 125.7(8) . . ? O1 C7 C8 114.0(7) . . ? C12 C7 C8 120.3(8) . . ? C9 C8 C7 120.7(9) . . ? C8 C9 C10 122.0(9) . . ? O2 C10 C11 125.4(9) 3_576 . ? O2 C10 C9 115.3(8) 3_576 . ? C11 C10 C9 119.3(8) . . ? C10 C11 C10 122.6(12) 11 . ? C10 C11 C12 118.7(6) 11 . ? C10 C11 C12 118.7(6) . . ? C7 C12 C7 122.1(11) 11 . ? C7 C12 C11 118.9(6) 11 . ? C7 C12 C11 118.9(6) . . ? O3 C13 Re1 179.1(13) . . ? O4 C14 Re1 178.1(8) . . ? O5 C15 Re2 172.7(13) . . ? O6 C16 Re2 179.1(10) . . ? C17 C17 C18 119.9(10) 11 . ? C17 C18 C17 120(2) 3_576 . ? C25 C21 C25 147(4) . 11_755 ? C25 C21 C22 120(3) . . ? C25 C21 C22 29.8(18) 11_755 . ? C25 C21 C22 29.8(18) . 11_755 ? C25 C21 C22 120(3) 11_755 11_755 ? C22 C21 C22 90(3) . 11_755 ? C25 C22 C24 110(6) 11_755 . ? C25 C22 C23 166(6) 11_755 . ? C24 C22 C23 62(3) . . ? C25 C22 C21 65(5) 11_755 . ? C24 C22 C21 165(5) . . ? C23 C22 C21 120(3) . . ? C24 C23 C23 142.7(18) . 11_755 ? C24 C23 C22 39.3(19) . . ? C23 C23 C22 104.9(17) 11_755 . ? C22 C24 C23 79(4) . . ? C22 C24 C25 30(3) . 11_755 ? C23 C24 C25 108(3) . 11_755 ? C22 C25 C21 86(5) 11_755 . ? C22 C25 C24 39(4) 11_755 11_755 ? C21 C25 C24 124(4) . 11_755 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 4.229 _refine_diff_density_min -2.287 _refine_diff_density_rms 0.175