# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Nikolay Naumov' _publ_contact_author_email NAUMOV@CHE.NSK.SU _publ_section_title ; Unusual H-bonding in novel cyanocluster polymeric hydrates [(H){Ln(H2O)4}{Re6S8(CN)6}]*2H2O, Ln= Yb, Lu ; loop_ _publ_author_name 'Nikolay Naumov' 'Vladimir E Fedorov' 'Eugeny O Golenkov' 'Nikolay K Moroz' 'Maria S Tarasenko' # Attachment 't40-6_revised.cif' data_t40-6_fin _database_code_depnum_ccdc_archive 'CCDC 686681' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H13 N6 O6 Re6 S8 Yb' _chemical_formula_weight 1811.94 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.2849(16) _cell_length_b 12.5696(16) _cell_length_c 12.4395(12) _cell_angle_alpha 90.00 _cell_angle_beta 121.840(3) _cell_angle_gamma 90.00 _cell_volume 2694.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 2435 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 29.46 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3148 _exptl_absorpt_coefficient_mu 30.929 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1910 _exptl_absorpt_correction_T_max 0.2584 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 Nonius X8Apex CCD area-detector' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 25 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9579 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3334 _reflns_number_gt 2667 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXTL (Bruker, 2004)' _computing_structure_refinement 'SHELXTL (Bruker, 2004)' _computing_molecular_graphics 'SHELXTL (Bruker, 2004)' _computing_publication_material 'SHELXTL (Bruker, 2004)' _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^)+(0.0001P)^2^+237.9536P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 3334 _refine_ls_number_parameters 182 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.19582(3) 0.12437(5) 0.93857(6) 0.01899(16) Uani 1 1 d . . . Re2 Re 0.19788(3) 0.27703(5) 1.08122(6) 0.01775(15) Uani 1 1 d . . . Re3 Re 0.17411(3) 0.32006(5) 0.85845(5) 0.01856(15) Uani 1 1 d . . . Yb1 Yb 0.0056(3) -0.23157(10) 0.7730(2) 0.0232(6) Uani 0.50 1 d P . . S1 S 0.2221(2) 0.0941(3) 1.1488(4) 0.0245(8) Uani 1 1 d . . . S2 S 0.1816(2) 0.4570(3) 1.0021(4) 0.0260(9) Uani 1 1 d . . . S3 S 0.1785(2) 0.1731(3) 0.7382(3) 0.0232(8) Uani 1 1 d . . . S4 S 0.0822(2) 0.2246(3) 0.8887(4) 0.0242(8) Uani 1 1 d . . . N1 N 0.0878(9) -0.0877(12) 0.8169(15) 0.040(4) Uani 1 1 d . . . N2 N 0.0952(9) 0.2960(14) 1.2116(15) 0.042(4) Uani 1 1 d . . . N3 N 0.0454(8) 0.4397(13) 0.6013(13) 0.037(4) Uani 1 1 d . . . C1 C 0.1275(9) -0.0142(13) 0.8626(15) 0.025(3) Uani 1 1 d . . . C2 C 0.1346(9) 0.2996(14) 1.1725(15) 0.027(4) Uani 1 1 d . . . C3 C 0.0912(9) 0.3973(13) 0.6920(15) 0.024(3) Uani 1 1 d . . . O1 O 0.0121(16) -0.4152(18) 0.786(2) 0.039(7) Uani 0.50 1 d PU . . O2 O 0.0101(15) -0.153(3) 0.945(2) 0.048(8) Uani 0.50 1 d P . . O4 O -0.0766(15) -0.279(3) 0.563(2) 0.057(10) Uani 0.50 1 d P . . O3 O 0.1266(18) -0.278(2) 0.962(2) 0.041(6) Uani 0.50 1 d PU . . O1W O 0.240(3) -0.274(4) 1.019(5) 0.102(15) Uani 0.50 1 d PU . . O2W O -0.010(5) -0.048(13) 0.989(9) 0.25(9) Uani 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 0.0188(3) 0.0167(3) 0.0185(3) 0.0005(2) 0.0078(2) -0.0014(2) Re2 0.0176(3) 0.0200(3) 0.0164(3) 0.0021(2) 0.0095(2) 0.0019(2) Re3 0.0170(3) 0.0190(3) 0.0159(3) 0.0033(2) 0.0061(2) 0.0023(2) Yb1 0.0234(13) 0.0217(6) 0.0281(19) -0.0023(6) 0.0160(18) -0.0013(7) S1 0.028(2) 0.022(2) 0.027(2) 0.0088(16) 0.0167(17) 0.0018(16) S2 0.029(2) 0.018(2) 0.029(2) 0.0039(17) 0.0144(17) 0.0065(16) S3 0.0263(19) 0.023(2) 0.0171(18) 0.0007(16) 0.0092(16) -0.0009(16) S4 0.0148(17) 0.029(2) 0.0242(19) 0.0007(17) 0.0073(15) -0.0016(16) N1 0.050(10) 0.027(8) 0.041(9) -0.012(7) 0.023(8) -0.008(7) N2 0.043(9) 0.057(12) 0.047(10) -0.003(8) 0.038(8) 0.013(8) N3 0.034(8) 0.049(10) 0.018(7) 0.007(7) 0.006(6) 0.013(7) C1 0.028(8) 0.019(8) 0.027(8) 0.001(7) 0.014(7) 0.001(7) C2 0.018(7) 0.037(11) 0.021(8) 0.000(7) 0.006(6) 0.001(7) C3 0.033(9) 0.023(9) 0.021(8) -0.007(7) 0.017(7) -0.007(7) O1 0.037(10) 0.030(9) 0.050(12) 0.000(7) 0.024(9) -0.005(8) O2 0.031(14) 0.10(3) 0.019(12) -0.011(14) 0.018(11) 0.004(14) O4 0.018(13) 0.10(3) 0.030(14) -0.021(15) 0.000(11) 0.027(15) O3 0.052(10) 0.037(10) 0.032(9) 0.019(7) 0.021(8) 0.007(8) O1W 0.097(17) 0.101(17) 0.102(17) 0.001(10) 0.048(11) 0.001(10) O2W 0.10(5) 0.6(3) 0.11(5) 0.06(10) 0.06(4) -0.10(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 2.113(16) . ? Re1 S4 2.403(4) . ? Re1 S3 2.405(4) . ? Re1 S1 2.408(4) . ? Re1 S2 2.417(4) 7_557 ? Re1 Re2 2.5990(9) . ? Re1 Re3 2.6027(9) . ? Re1 Re3 2.6069(8) 7_557 ? Re1 Re2 2.6088(8) 7_557 ? Re2 C2 2.133(17) . ? Re2 S4 2.398(4) . ? Re2 S3 2.405(4) 7_557 ? Re2 S1 2.408(4) . ? Re2 S2 2.419(4) . ? Re2 Re3 2.5960(8) 7_557 ? Re2 Re3 2.6066(9) . ? Re2 Re1 2.6088(9) 7_557 ? Re3 C3 2.093(16) . ? Re3 S3 2.407(4) . ? Re3 S4 2.408(4) . ? Re3 S1 2.410(4) 7_557 ? Re3 S2 2.428(4) . ? Re3 Re2 2.5960(8) 7_557 ? Re3 Re1 2.6069(8) 7_557 ? Yb1 Yb1 0.491(4) 2_556 ? Yb1 O4 1.87(3) 2_556 ? Yb1 N2 2.300(16) 5_557 ? Yb1 O2 2.31(2) . ? Yb1 O1 2.31(2) . ? Yb1 O4 2.32(3) . ? Yb1 N1 2.321(16) . ? Yb1 O1 2.39(2) 2_556 ? Yb1 O3 2.41(3) . ? Yb1 N1 2.424(15) 2_556 ? Yb1 N2 2.450(16) 6 ? Yb1 O2 2.74(2) 2_556 ? S1 Re3 2.410(4) 7_557 ? S2 Re1 2.417(4) 7_557 ? S3 Re2 2.405(4) 7_557 ? N1 C1 1.16(2) . ? N1 Yb1 2.424(15) 2_556 ? N2 C2 1.14(2) . ? N2 Yb1 2.300(16) 5_557 ? N2 Yb1 2.450(16) 6_556 ? N3 C3 1.15(2) . ? O1 O1 0.77(4) 2_556 ? O1 Yb1 2.39(2) 2_556 ? O2 O2W 1.57(17) . ? O2 Yb1 2.74(2) 2_556 ? O4 O3 0.89(3) 2_556 ? O4 Yb1 1.87(3) 2_556 ? O3 O4 0.89(3) 2_556 ? O3 Yb1 2.79(3) 2_556 ? O1W O1W 0.98(8) 7_547 ? O2W O2W 1.2(3) 5_557 ? 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 90.2(4) . . ? C1 Re1 S3 92.5(5) . . ? S4 Re1 S3 90.17(14) . . ? C1 Re1 S1 94.2(5) . . ? S4 Re1 S1 89.76(14) . . ? S3 Re1 S1 173.34(14) . . ? C1 Re1 S2 96.6(4) . 7_557 ? S4 Re1 S2 173.26(14) . 7_557 ? S3 Re1 S2 89.35(14) . 7_557 ? S1 Re1 S2 89.94(14) . 7_557 ? C1 Re1 Re2 133.2(4) . . ? S4 Re1 Re2 57.12(10) . . ? S3 Re1 Re2 117.40(10) . . ? S1 Re1 Re2 57.35(10) . . ? S2 Re1 Re2 117.43(10) 7_557 . ? C1 Re1 Re3 132.0(4) . . ? S4 Re1 Re3 57.34(10) . . ? S3 Re1 Re3 57.30(10) . . ? S1 Re1 Re3 117.46(10) . . ? S2 Re1 Re3 117.13(10) 7_557 . ? Re2 Re1 Re3 60.15(2) . . ? C1 Re1 Re3 138.1(4) . 7_557 ? S4 Re1 Re3 116.90(10) . 7_557 ? S3 Re1 Re3 117.09(10) . 7_557 ? S1 Re1 Re3 57.28(10) . 7_557 ? S2 Re1 Re3 57.65(10) 7_557 7_557 ? Re2 Re1 Re3 59.82(2) . 7_557 ? Re3 Re1 Re3 89.89(3) . 7_557 ? C1 Re1 Re2 136.8(5) . 7_557 ? S4 Re1 Re2 117.04(10) . 7_557 ? S3 Re1 Re2 57.15(9) . 7_557 ? S1 Re1 Re2 117.22(10) . 7_557 ? S2 Re1 Re2 57.40(10) 7_557 7_557 ? Re2 Re1 Re2 89.85(3) . 7_557 ? Re3 Re1 Re2 59.75(2) . 7_557 ? Re3 Re1 Re2 59.97(2) 7_557 7_557 ? C2 Re2 S4 91.2(4) . . ? C2 Re2 S3 95.3(4) . 7_557 ? S4 Re2 S3 173.48(14) . 7_557 ? C2 Re2 S1 90.6(5) . . ? S4 Re2 S1 89.88(14) . . ? S3 Re2 S1 90.16(14) 7_557 . ? C2 Re2 S2 95.8(5) . . ? S4 Re2 S2 89.94(14) . . ? S3 Re2 S2 89.30(14) 7_557 . ? S1 Re2 S2 173.63(14) . . ? C2 Re2 Re3 134.4(4) . 7_557 ? S4 Re2 Re3 117.53(10) . 7_557 ? S3 Re2 Re3 57.40(10) 7_557 7_557 ? S1 Re2 Re3 57.43(10) . 7_557 ? S2 Re2 Re3 117.29(10) . 7_557 ? C2 Re2 Re1 131.6(5) . . ? S4 Re2 Re1 57.33(10) . . ? S3 Re2 Re1 117.60(10) 7_557 . ? S1 Re2 Re1 57.33(10) . . ? S2 Re2 Re1 117.58(11) . . ? Re3 Re2 Re1 60.24(2) 7_557 . ? C2 Re2 Re3 135.4(4) . . ? S4 Re2 Re3 57.34(10) . . ? S3 Re2 Re3 117.11(10) 7_557 . ? S1 Re2 Re3 117.29(10) . . ? S2 Re2 Re3 57.62(10) . . ? Re3 Re2 Re3 90.04(3) 7_557 . ? Re1 Re2 Re3 60.00(2) . . ? C2 Re2 Re1 138.2(5) . 7_557 ? S4 Re2 Re1 117.29(10) . 7_557 ? S3 Re2 Re1 57.16(10) 7_557 7_557 ? S1 Re2 Re1 117.40(10) . 7_557 ? S2 Re2 Re1 57.30(10) . 7_557 ? Re3 Re2 Re1 60.01(2) 7_557 7_557 ? Re1 Re2 Re1 90.15(3) . 7_557 ? Re3 Re2 Re1 59.98(2) . 7_557 ? C3 Re3 S3 90.9(4) . . ? C3 Re3 S4 95.8(4) . . ? S3 Re3 S4 90.00(14) . . ? C3 Re3 S1 91.0(4) . 7_557 ? S3 Re3 S1 90.06(14) . 7_557 ? S4 Re3 S1 173.19(13) . 7_557 ? C3 Re3 S2 96.0(4) . . ? S3 Re3 S2 173.12(13) . . ? S4 Re3 S2 89.50(14) . . ? S1 Re3 S2 89.63(14) 7_557 . ? C3 Re3 Re2 131.5(4) . 7_557 ? S3 Re3 Re2 57.30(9) . 7_557 ? S4 Re3 Re2 117.35(10) . 7_557 ? S1 Re3 Re2 57.37(10) 7_557 7_557 ? S2 Re3 Re2 117.14(10) . 7_557 ? C3 Re3 Re1 134.6(4) . . ? S3 Re3 Re1 57.22(10) . . ? S4 Re3 Re1 57.16(10) . . ? S1 Re3 Re1 117.57(10) 7_557 . ? S2 Re3 Re1 117.13(10) . . ? Re2 Re3 Re1 60.24(2) 7_557 . ? C3 Re3 Re2 138.5(4) . . ? S3 Re3 Re2 117.03(10) . . ? S4 Re3 Re2 56.96(10) . . ? S1 Re3 Re2 117.22(10) 7_557 . ? S2 Re3 Re2 57.31(10) . . ? Re2 Re3 Re2 89.96(3) 7_557 . ? Re1 Re3 Re2 59.85(2) . . ? C3 Re3 Re1 135.1(4) . 7_557 ? S3 Re3 Re1 117.20(9) . 7_557 ? S4 Re3 Re1 116.98(10) . 7_557 ? S1 Re3 Re1 57.20(10) 7_557 7_557 ? S2 Re3 Re1 57.24(10) . 7_557 ? Re2 Re3 Re1 59.94(2) 7_557 7_557 ? Re1 Re3 Re1 90.11(3) . 7_557 ? Re2 Re3 Re1 60.05(2) . 7_557 ? Yb1 Yb1 O4 152.8(15) 2_556 2_556 ? Yb1 Yb1 N2 102.1(12) 2_556 5_557 ? O4 Yb1 N2 90.2(9) 2_556 5_557 ? Yb1 Yb1 O2 147.6(11) 2_556 . ? O4 Yb1 O2 59.4(14) 2_556 . ? N2 Yb1 O2 71.1(9) 5_557 . ? Yb1 Yb1 O1 93.3(6) 2_556 . ? O4 Yb1 O1 67.9(12) 2_556 . ? N2 Yb1 O1 70.2(9) 5_557 . ? O2 Yb1 O1 112.7(11) . . ? Yb1 Yb1 O4 21.6(12) 2_556 . ? O4 Yb1 O4 146(2) 2_556 . ? N2 Yb1 O4 82.1(9) 5_557 . ? O2 Yb1 O4 143.8(9) . . ? O1 Yb1 O4 78.8(10) . . ? Yb1 Yb1 N1 96.3(9) 2_556 . ? O4 Yb1 N1 86.9(10) 2_556 . ? N2 Yb1 N1 144.5(6) 5_557 . ? O2 Yb1 N1 77.1(9) . . ? O1 Yb1 N1 139.0(8) . . ? O4 Yb1 N1 117.7(10) . . ? Yb1 Yb1 O1 74.9(6) 2_556 2_556 ? O4 Yb1 O1 86.3(12) 2_556 2_556 ? N2 Yb1 O1 72.0(9) 5_557 2_556 ? O2 Yb1 O1 128.5(11) . 2_556 ? O1 Yb1 O1 18.7(11) . 2_556 ? O4 Yb1 O1 60.2(10) . 2_556 ? N1 Yb1 O1 142.8(9) . 2_556 ? Yb1 Yb1 O3 138.1(14) 2_556 . ? O4 Yb1 O3 19.4(10) 2_556 . ? N2 Yb1 O3 109.1(8) 5_557 . ? O2 Yb1 O3 71.2(10) . . ? O1 Yb1 O3 72.5(9) . . ? O4 Yb1 O3 142.7(9) . . ? N1 Yb1 O3 73.9(8) . . ? O1 Yb1 O3 88.7(9) 2_556 . ? Yb1 Yb1 N1 72.1(8) 2_556 2_556 ? O4 Yb1 N1 134.8(12) 2_556 2_556 ? N2 Yb1 N1 77.8(6) 5_557 2_556 ? O2 Yb1 N1 75.5(8) . 2_556 ? O1 Yb1 N1 141.1(8) . 2_556 ? O4 Yb1 N1 75.4(8) . 2_556 ? N1 Yb1 N1 79.4(8) . 2_556 ? O1 Yb1 N1 128.6(7) 2_556 2_556 ? O3 Yb1 N1 141.0(8) . 2_556 ? Yb1 Yb1 N2 66.6(12) 2_556 6 ? O4 Yb1 N2 88.1(11) 2_556 6 ? N2 Yb1 N2 138.4(8) 5_557 6 ? O2 Yb1 N2 139.0(8) . 6 ? O1 Yb1 N2 70.7(9) . 6 ? O4 Yb1 N2 76.9(8) . 6 ? N1 Yb1 N2 76.9(6) . 6 ? O1 Yb1 N2 66.4(8) 2_556 6 ? O3 Yb1 N2 71.4(8) . 6 ? N1 Yb1 N2 129.1(6) 2_556 6 ? Yb1 Yb1 O2 26.9(9) 2_556 2_556 ? O4 Yb1 O2 144.7(10) 2_556 2_556 ? N2 Yb1 O2 124.3(7) 5_557 2_556 ? O2 Yb1 O2 133.6(16) . 2_556 ? O1 Yb1 O2 113.7(10) . 2_556 ? O4 Yb1 O2 48.4(11) . 2_556 ? N1 Yb1 O2 69.4(8) . 2_556 ? O1 Yb1 O2 97.0(10) 2_556 2_556 ? O3 Yb1 O2 125.3(9) . 2_556 ? N1 Yb1 O2 67.7(8) 2_556 2_556 ? N2 Yb1 O2 61.9(8) 6 2_556 ? Re1 S1 Re2 65.32(10) . . ? Re1 S1 Re3 65.52(10) . 7_557 ? Re2 S1 Re3 65.20(10) . 7_557 ? Re1 S2 Re2 65.30(10) 7_557 . ? Re1 S2 Re3 65.12(10) 7_557 . ? Re2 S2 Re3 65.07(10) . . ? Re2 S3 Re1 65.69(10) 7_557 . ? Re2 S3 Re3 65.30(10) 7_557 . ? Re1 S3 Re3 65.48(10) . . ? Re2 S4 Re1 65.55(10) . . ? Re2 S4 Re3 65.70(10) . . ? Re1 S4 Re3 65.50(10) . . ? C1 N1 Yb1 164.6(15) . . ? C1 N1 Yb1 173.3(15) . 2_556 ? Yb1 N1 Yb1 11.62(13) . 2_556 ? C2 N2 Yb1 155.3(16) . 5_557 ? C2 N2 Yb1 162.3(16) . 6_556 ? Yb1 N2 Yb1 11.31(14) 5_557 6_556 ? N1 C1 Re1 177.2(16) . . ? N2 C2 Re2 168.5(16) . . ? N3 C3 Re3 179.4(15) . . ? O1 O1 Yb1 86.5(6) 2_556 . ? O1 O1 Yb1 74.8(6) 2_556 2_556 ? Yb1 O1 Yb1 11.84(15) . 2_556 ? O2W O2 Yb1 142(4) . . ? O2W O2 Yb1 137(4) . 2_556 ? Yb1 O2 Yb1 5.52(18) . 2_556 ? O3 O4 Yb1 117(3) 2_556 2_556 ? O3 O4 Yb1 113(3) 2_556 . ? Yb1 O4 Yb1 5.6(3) 2_556 . ? O4 O3 Yb1 44(2) 2_556 . ? O4 O3 Yb1 50(2) 2_556 2_556 ? Yb1 O3 Yb1 6.8(2) . 2_556 ? O2W O2W O2 142(10) 5_557 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.429 _refine_diff_density_min -2.309 _refine_diff_density_rms 0.420 # Attachment 'tm24_revised.cif' data_tm24_2_fin _database_code_depnum_ccdc_archive 'CCDC 686682' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H13 Lu N6 O6 Re6 S8' _chemical_formula_weight 1813.87 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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.2069(16) _cell_length_b 12.5260(16) _cell_length_c 12.4548(12) _cell_angle_alpha 90.00 _cell_angle_beta 121.784(3) _cell_angle_gamma 90.00 _cell_volume 2679.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 3314 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 28.33 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 31.294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1886 _exptl_absorpt_correction_T_max 0.3675 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 Nonius X8Apex CCD area-detector' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 25 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8143 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.30 _reflns_number_total 3145 _reflns_number_gt 2908 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXTL (Bruker, 2004)' _computing_structure_refinement 'SHELXTL (Bruker, 2004)' _computing_molecular_graphics 'SHELXTL (Bruker, 2004)' _computing_publication_material 'SHELXTL (Bruker, 2004)' _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^+1183.3381P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 3145 _refine_ls_number_parameters 182 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0780 _refine_ls_wR_factor_ref 0.1789 _refine_ls_wR_factor_gt 0.1774 _refine_ls_goodness_of_fit_ref 1.376 _refine_ls_restrained_S_all 1.366 _refine_ls_shift/su_max 0.009 _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 0.19525(6) 0.12429(9) 0.93835(10) 0.0122(3) Uani 1 1 d . . . Re2 Re 0.19810(6) 0.27712(9) 1.08177(10) 0.0107(3) Uani 1 1 d . . . Re3 Re 0.17383(6) 0.32058(9) 0.85918(10) 0.0118(3) Uani 1 1 d . . . Lu1 Lu 0.0075(2) -0.23383(19) 0.7773(2) 0.0146(7) Uani 0.50 1 d P . . S1 S 0.2222(4) 0.0933(6) 1.1476(6) 0.0144(13) Uani 1 1 d . . . S2 S 0.1826(4) 0.4573(6) 1.0039(7) 0.0184(14) Uani 1 1 d . . . S3 S 0.1780(4) 0.1733(6) 0.7399(6) 0.0161(13) Uani 1 1 d . . . S4 S 0.0819(4) 0.2250(6) 0.8901(7) 0.0160(13) Uani 1 1 d . . . N1 N 0.0853(18) -0.088(3) 0.814(3) 0.037(7) Uani 1 1 d . . . N2 N 0.0953(17) 0.296(3) 1.213(3) 0.031(7) Uani 1 1 d U . . N3 N 0.0453(15) 0.440(3) 0.603(3) 0.029(6) Uani 1 1 d . . . C1 C 0.1267(17) -0.016(2) 0.861(3) 0.016(6) Uani 1 1 d . . . C2 C 0.1360(16) 0.300(2) 1.173(3) 0.018(6) Uani 1 1 d U . . C3 C 0.0912(17) 0.398(2) 0.694(3) 0.018(6) Uani 1 1 d . . . O1 O 0.014(3) -0.415(4) 0.795(4) 0.025(10) Uani 0.50 1 d PU . . O2 O 0.009(4) -0.151(5) 0.951(6) 0.051(15) Uani 0.50 1 d PU . . O4 O -0.073(3) -0.271(4) 0.566(4) 0.026(10) Uani 0.50 1 d PU . . O3 O 0.133(2) -0.269(3) 0.967(3) 0.010(7) Uani 0.50 1 d PU . . O1W O 0.236(5) -0.281(6) 1.024(8) 0.07(2) Uani 0.50 1 d PU . . O2W O 0.002(5) -0.041(6) 1.007(8) 0.07(2) Uani 0.50 1 d PU . . 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 0.0096(5) 0.0139(5) 0.0122(5) 0.0006(4) 0.0052(4) -0.0008(4) Re2 0.0081(5) 0.0160(5) 0.0100(5) 0.0018(4) 0.0060(4) 0.0013(4) Re3 0.0082(5) 0.0153(5) 0.0106(5) 0.0025(4) 0.0040(4) 0.0013(4) Lu1 0.0136(17) 0.0160(10) 0.017(2) 0.0003(8) 0.010(2) 0.0001(10) S1 0.016(3) 0.016(3) 0.015(3) 0.006(3) 0.011(3) 0.001(2) S2 0.016(3) 0.014(3) 0.026(4) 0.005(3) 0.013(3) 0.005(3) S3 0.017(3) 0.019(3) 0.012(3) 0.001(3) 0.007(3) 0.000(3) S4 0.007(3) 0.019(3) 0.019(3) 0.004(3) 0.005(3) -0.002(2) N1 0.031(16) 0.032(17) 0.036(17) -0.016(14) 0.010(14) -0.009(13) N2 0.031(12) 0.040(14) 0.035(13) -0.010(11) 0.025(11) 0.008(10) N3 0.014(12) 0.047(18) 0.014(13) -0.002(12) -0.001(10) -0.007(12) C1 0.019(13) 0.023(15) 0.009(12) 0.005(11) 0.009(11) -0.002(11) C2 0.012(11) 0.024(12) 0.011(11) -0.006(10) 0.001(9) -0.004(9) C3 0.022(14) 0.018(14) 0.022(15) -0.007(11) 0.017(13) -0.003(11) O1 0.027(17) 0.022(16) 0.029(17) -0.006(13) 0.018(14) -0.003(13) O2 0.051(17) 0.056(18) 0.052(18) 0.001(10) 0.031(12) 0.000(10) O4 0.026(12) 0.022(13) 0.023(12) -0.004(9) 0.009(9) 0.006(9) O3 0.014(10) 0.007(10) 0.005(10) 0.002(8) 0.002(8) 0.005(8) O1W 0.07(2) 0.07(2) 0.07(2) -0.004(10) 0.034(14) 0.004(10) O2W 0.07(2) 0.07(2) 0.07(2) 0.001(10) 0.037(14) -0.001(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 2.12(3) . ? Re1 S3 2.388(7) . ? Re1 S1 2.397(7) . ? Re1 S4 2.397(7) . ? Re1 S2 2.406(7) 7_557 ? Re1 Re2 2.5981(15) . ? Re1 Re3 2.5991(16) . ? Re1 Re2 2.6078(14) 7_557 ? Re1 Re3 2.6089(15) 7_557 ? Re2 C2 2.10(3) . ? Re2 S3 2.393(7) 7_557 ? Re2 S4 2.394(7) . ? Re2 S1 2.407(7) . ? Re2 S2 2.411(7) . ? Re2 Re3 2.5943(14) 7_557 ? Re2 Re3 2.6058(15) . ? Re2 Re1 2.6078(14) 7_557 ? Re3 C3 2.08(3) . ? Re3 S3 2.398(7) . ? Re3 S1 2.402(7) 7_557 ? Re3 S4 2.405(7) . ? Re3 S2 2.425(8) . ? Re3 Re2 2.5943(14) 7_557 ? Re3 Re1 2.6089(15) 7_557 ? Lu1 Lu1 0.581(4) 2_556 ? Lu1 O4 1.75(5) 2_556 ? Lu1 N2 2.28(3) 5_557 ? Lu1 O1 2.28(4) . ? Lu1 N1 2.30(3) . ? Lu1 O4 2.30(5) . ? Lu1 O2 2.39(6) . ? Lu1 O1 2.39(4) 2_556 ? Lu1 N2 2.43(3) 6 ? Lu1 N1 2.43(3) 2_556 ? Lu1 O3 2.43(4) . ? Lu1 O2 2.88(6) 2_556 ? S1 Re3 2.402(7) 7_557 ? S2 Re1 2.406(7) 7_557 ? S3 Re2 2.393(7) 7_557 ? N1 C1 1.16(4) . ? N1 Lu1 2.43(3) 2_556 ? N2 C2 1.17(4) . ? N2 Lu1 2.28(3) 5_557 ? N2 Lu1 2.43(3) 6_556 ? N3 C3 1.15(4) . ? O1 O1 0.95(8) 2_556 ? O1 Lu1 2.39(4) 2_556 ? O2 O2W 1.58(10) . ? O2 Lu1 2.88(6) 2_556 ? O4 O3 1.06(6) 2_556 ? O4 Lu1 1.75(5) 2_556 ? O3 O4 1.06(6) 2_556 ? O3 O1W 1.81(8) . ? O1W O1W 1.28(15) 7_547 ? O2W O2W 1.04(14) 5_557 ? 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 92.1(7) . . ? C1 Re1 S1 94.7(7) . . ? S3 Re1 S1 173.2(2) . . ? C1 Re1 S4 90.7(8) . . ? S3 Re1 S4 90.3(2) . . ? S1 Re1 S4 89.9(2) . . ? C1 Re1 S2 96.1(8) . 7_557 ? S3 Re1 S2 89.2(3) . 7_557 ? S1 Re1 S2 89.8(2) . 7_557 ? S4 Re1 S2 173.2(3) . 7_557 ? C1 Re1 Re2 133.9(7) . . ? S3 Re1 Re2 117.42(18) . . ? S1 Re1 Re2 57.45(17) . . ? S4 Re1 Re2 57.11(18) . . ? S2 Re1 Re2 117.39(19) 7_557 . ? C1 Re1 Re3 132.0(8) . . ? S3 Re1 Re3 57.29(18) . . ? S1 Re1 Re3 117.58(18) . . ? S4 Re1 Re3 57.38(17) . . ? S2 Re1 Re3 117.07(18) 7_557 . ? Re2 Re1 Re3 60.18(4) . . ? C1 Re1 Re2 136.1(7) . 7_557 ? S3 Re1 Re2 57.05(17) . 7_557 ? S1 Re1 Re2 117.07(17) . 7_557 ? S4 Re1 Re2 117.09(17) . 7_557 ? S2 Re1 Re2 57.32(17) 7_557 7_557 ? Re2 Re1 Re2 89.83(5) . 7_557 ? Re3 Re1 Re2 59.77(4) . 7_557 ? C1 Re1 Re3 138.1(8) . 7_557 ? S3 Re1 Re3 116.96(18) . 7_557 ? S1 Re1 Re3 57.16(17) . 7_557 ? S4 Re1 Re3 116.84(18) . 7_557 ? S2 Re1 Re3 57.67(19) 7_557 7_557 ? Re2 Re1 Re3 59.77(4) . 7_557 ? Re3 Re1 Re3 89.87(5) . 7_557 ? Re2 Re1 Re3 59.94(4) 7_557 7_557 ? C2 Re2 S3 95.4(8) . 7_557 ? C2 Re2 S4 91.4(8) . . ? S3 Re2 S4 173.2(2) 7_557 . ? C2 Re2 S1 90.9(9) . . ? S3 Re2 S1 90.4(2) 7_557 . ? S4 Re2 S1 89.7(2) . . ? C2 Re2 S2 95.9(9) . . ? S3 Re2 S2 88.9(3) 7_557 . ? S4 Re2 S2 90.2(3) . . ? S1 Re2 S2 173.2(2) . . ? C2 Re2 Re3 134.3(8) . 7_557 ? S3 Re2 Re3 57.30(17) 7_557 7_557 ? S4 Re2 Re3 117.49(18) . 7_557 ? S1 Re2 Re3 57.26(16) . 7_557 ? S2 Re2 Re3 117.05(17) . 7_557 ? C2 Re2 Re1 131.6(8) . . ? S3 Re2 Re1 117.56(18) 7_557 . ? S4 Re2 Re1 57.20(18) . . ? S1 Re2 Re1 57.06(17) . . ? S2 Re2 Re1 117.54(19) . . ? Re3 Re2 Re1 60.32(4) 7_557 . ? C2 Re2 Re3 135.5(8) . . ? S3 Re2 Re3 116.86(17) 7_557 . ? S4 Re2 Re3 57.31(17) . . ? S1 Re2 Re3 116.95(17) . . ? S2 Re2 Re3 57.65(19) . . ? Re3 Re2 Re3 90.05(4) 7_557 . ? Re1 Re2 Re3 59.93(4) . . ? C2 Re2 Re1 138.2(8) . 7_557 ? S3 Re2 Re1 56.84(17) 7_557 7_557 ? S4 Re2 Re1 117.33(17) . 7_557 ? S1 Re2 Re1 117.16(16) . 7_557 ? S2 Re2 Re1 57.12(17) . 7_557 ? Re3 Re2 Re1 59.95(4) 7_557 7_557 ? Re1 Re2 Re1 90.17(5) . 7_557 ? Re3 Re2 Re1 60.05(4) . 7_557 ? C3 Re3 S3 91.0(8) . . ? C3 Re3 S1 91.0(8) . 7_557 ? S3 Re3 S1 90.4(2) . 7_557 ? C3 Re3 S4 96.0(8) . . ? S3 Re3 S4 89.9(3) . . ? S1 Re3 S4 173.0(2) 7_557 . ? C3 Re3 S2 96.4(8) . . ? S3 Re3 S2 172.6(2) . . ? S1 Re3 S2 89.2(2) 7_557 . ? S4 Re3 S2 89.6(3) . . ? C3 Re3 Re2 131.3(7) . 7_557 ? S3 Re3 Re2 57.14(17) . 7_557 ? S1 Re3 Re2 57.44(17) 7_557 7_557 ? S4 Re3 Re2 117.30(17) . 7_557 ? S2 Re3 Re2 116.83(17) . 7_557 ? C3 Re3 Re1 134.5(8) . . ? S3 Re3 Re1 56.91(17) . . ? S1 Re3 Re1 117.67(17) 7_557 . ? S4 Re3 Re1 57.08(17) . . ? S2 Re3 Re1 116.99(18) . . ? Re2 Re3 Re1 60.28(4) 7_557 . ? C3 Re3 Re2 138.7(7) . . ? S3 Re3 Re2 116.75(17) . . ? S1 Re3 Re2 116.95(17) 7_557 . ? S4 Re3 Re2 56.92(18) . . ? S2 Re3 Re2 57.14(18) . . ? Re2 Re3 Re2 89.95(4) 7_557 . ? Re1 Re3 Re2 59.89(4) . . ? C3 Re3 Re1 135.1(8) . 7_557 ? S3 Re3 Re1 116.99(17) . 7_557 ? S1 Re3 Re1 56.97(17) 7_557 7_557 ? S4 Re3 Re1 116.90(18) . 7_557 ? S2 Re3 Re1 56.96(17) . 7_557 ? Re2 Re3 Re1 59.91(4) 7_557 7_557 ? Re1 Re3 Re1 90.13(5) . 7_557 ? Re2 Re3 Re1 60.01(4) . 7_557 ? Lu1 Lu1 O4 158.5(17) 2_556 2_556 ? Lu1 Lu1 N2 97.8(11) 2_556 5_557 ? O4 Lu1 N2 91.3(17) 2_556 5_557 ? Lu1 Lu1 O1 94.6(11) 2_556 . ? O4 Lu1 O1 70.1(19) 2_556 . ? N2 Lu1 O1 70.3(14) 5_557 . ? Lu1 Lu1 N1 96.4(10) 2_556 . ? O4 Lu1 N1 87.4(17) 2_556 . ? N2 Lu1 N1 144.0(11) 5_557 . ? O1 Lu1 N1 141.0(14) . . ? Lu1 Lu1 O4 16.2(14) 2_556 . ? O4 Lu1 O4 153(3) 2_556 . ? N2 Lu1 O4 83.2(14) 5_557 . ? O1 Lu1 O4 83.1(16) . . ? N1 Lu1 O4 112.4(15) . . ? Lu1 Lu1 O2 144.4(17) 2_556 . ? O4 Lu1 O2 57(2) 2_556 . ? N2 Lu1 O2 71.2(17) 5_557 . ? O1 Lu1 O2 111.9(19) . . ? N1 Lu1 O2 78.1(18) . . ? O4 Lu1 O2 142.4(19) . . ? Lu1 Lu1 O1 71.4(10) 2_556 2_556 ? O4 Lu1 O1 92.9(18) 2_556 2_556 ? N2 Lu1 O1 73.0(13) 5_557 2_556 ? O1 Lu1 O1 23(2) . 2_556 ? N1 Lu1 O1 142.9(14) . 2_556 ? O4 Lu1 O1 60.1(15) . 2_556 ? O2 Lu1 O1 131.8(19) . 2_556 ? Lu1 Lu1 N2 68.5(10) 2_556 6 ? O4 Lu1 N2 91.9(18) 2_556 6 ? N2 Lu1 N2 138.9(14) 5_557 6 ? O1 Lu1 N2 72.4(13) . 6 ? N1 Lu1 N2 77.1(11) . 6 ? O4 Lu1 N2 75.8(14) . 6 ? O2 Lu1 N2 140.9(17) . 6 ? O1 Lu1 N2 65.9(13) 2_556 6 ? Lu1 Lu1 N1 69.9(10) 2_556 2_556 ? O4 Lu1 N1 131.4(18) 2_556 2_556 ? N2 Lu1 N1 77.3(11) 5_557 2_556 ? O1 Lu1 N1 141.8(14) . 2_556 ? N1 Lu1 N1 76.8(16) . 2_556 ? O4 Lu1 N1 73.2(14) . 2_556 ? O2 Lu1 N1 74.6(18) . 2_556 ? O1 Lu1 N1 126.6(13) 2_556 2_556 ? N2 Lu1 N1 127.3(11) 6 2_556 ? Lu1 Lu1 O3 140.5(12) 2_556 . ? O4 Lu1 O3 22.8(17) 2_556 . ? N2 Lu1 O3 113.6(12) 5_557 . ? O1 Lu1 O3 75.3(14) . . ? N1 Lu1 O3 72.5(12) . . ? O4 Lu1 O3 145.4(14) . . ? O2 Lu1 O3 71.9(18) . . ? O1 Lu1 O3 94.6(13) 2_556 . ? N2 Lu1 O3 72.0(11) 6 . ? N1 Lu1 O3 138.2(12) 2_556 . ? Lu1 Lu1 O2 28.9(14) 2_556 2_556 ? O4 Lu1 O2 146(2) 2_556 2_556 ? N2 Lu1 O2 122.7(15) 5_557 2_556 ? O1 Lu1 O2 115.2(17) . 2_556 ? N1 Lu1 O2 67.6(16) . 2_556 ? O4 Lu1 O2 45.1(18) . 2_556 ? O2 Lu1 O2 133(3) . 2_556 ? O1 Lu1 O2 93.8(17) 2_556 2_556 ? N2 Lu1 O2 60.9(15) 6 2_556 ? N1 Lu1 O2 66.9(15) 2_556 2_556 ? O3 Lu1 O2 123.1(15) . 2_556 ? Re1 S1 Re3 65.87(17) . 7_557 ? Re1 S1 Re2 65.49(17) . . ? Re3 S1 Re2 65.30(17) 7_557 . ? Re1 S2 Re2 65.55(18) 7_557 . ? Re1 S2 Re3 65.37(18) 7_557 . ? Re2 S2 Re3 65.21(19) . . ? Re1 S3 Re2 66.11(18) . 7_557 ? Re1 S3 Re3 65.79(18) . . ? Re2 S3 Re3 65.57(19) 7_557 . ? Re2 S4 Re1 65.68(17) . . ? Re2 S4 Re3 65.78(17) . . ? Re1 S4 Re3 65.55(17) . . ? C1 N1 Lu1 163(3) . . ? C1 N1 Lu1 175(3) . 2_556 ? Lu1 N1 Lu1 13.8(2) . 2_556 ? C2 N2 Lu1 155(3) . 5_557 ? C2 N2 Lu1 163(3) . 6_556 ? Lu1 N2 Lu1 13.7(2) 5_557 6_556 ? N1 C1 Re1 176(3) . . ? N2 C2 Re2 168(3) . . ? N3 C3 Re3 180(3) . . ? O1 O1 Lu1 85.4(10) 2_556 . ? O1 O1 Lu1 71.4(10) 2_556 2_556 ? Lu1 O1 Lu1 14.0(3) . 2_556 ? O2W O2 Lu1 145(5) . . ? O2W O2 Lu1 139(5) . 2_556 ? Lu1 O2 Lu1 6.8(3) . 2_556 ? O3 O4 Lu1 118(4) 2_556 2_556 ? O3 O4 Lu1 114(4) 2_556 . ? Lu1 O4 Lu1 5.3(4) 2_556 . ? O4 O3 O1W 175(5) 2_556 . ? O4 O3 Lu1 40(3) 2_556 . ? O1W O3 Lu1 142(3) . . ? O1W O1W O3 118(9) 7_547 . ? O2W O2W O2 144(10) 5_557 . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 3.697 _refine_diff_density_min -4.562 _refine_diff_density_rms 0.667