# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1245 data_shelxl97 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[RuSe~6~C~16~H~36~][CF~3~SO~3~]~2~' _chemical_formula_sum 'C18 H36 F6 O6 Ru S2 Se6' _chemical_formula_weight 1101.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8436(5) _cell_length_b 11.6692(15) _cell_length_c 8.7056(8) _cell_angle_alpha 107.369(9) _cell_angle_beta 91.648(7) _cell_angle_gamma 106.530(7) _cell_volume 815.62(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.6 _cell_measurement_theta_max 19.5 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 7.368 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_T_max 1.000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.9% _diffrn_reflns_number 3079 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2875 _reflns_number_gt 2263 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _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 w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+2.2211P] 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 2875 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.0000 0.0000 0.5000 0.03238(18) Uani 1 d S . . Se1 Se 0.09550(7) 0.19489(6) 0.42426(7) 0.04209(19) Uani 1 d . . . Se2 Se 0.03635(8) 0.12823(6) 0.78893(7) 0.0451(2) Uani 1 d . . . Se3 Se -0.27277(7) 0.01666(6) 0.48365(8) 0.04126(19) Uani 1 d . . . S1 S -0.3575(4) 0.3297(3) 0.1715(3) 0.0920(9) Uani 1 d . . . F1 F -0.5583(11) 0.3250(10) -0.0481(10) 0.170(4) Uani 1 d . . . F2 F -0.5840(13) 0.4251(13) 0.2004(15) 0.204(5) Uani 1 d . . . F3 F -0.6399(15) 0.2276(14) 0.1253(14) 0.300(10) Uani 1 d . . . O1 O -0.3535(11) 0.3417(11) 0.3334(10) 0.138(4) Uani 1 d . . . O2 O -0.2623(14) 0.4557(11) 0.1551(15) 0.196(6) Uani 1 d . . . O3 O -0.3267(19) 0.2351(12) 0.0558(16) 0.210(7) Uani 1 d . . . C1 C 0.3064(8) 0.2937(7) 0.5414(11) 0.065(2) Uani 1 d . . . H1A H 0.3803 0.2478 0.5062 0.080 Uiso 1 calc . . . H1B H 0.3025 0.3093 0.6557 0.080 Uiso 1 calc . . . H1C H 0.3400 0.3726 0.5200 0.080 Uiso 1 calc . . . C2 C -0.0206(8) 0.3132(6) 0.5289(9) 0.0474(15) Uani 1 d . . . H2A H 0.0559 0.3970 0.5666 0.080 Uiso 1 calc . . . H2B H -0.0955 0.3129 0.4449 0.080 Uiso 1 calc . . . C3 C -0.1111(8) 0.2959(6) 0.6680(9) 0.0487(16) Uani 1 d . . . C4 C -0.1584(10) 0.4183(7) 0.7383(10) 0.064(2) Uani 1 d . . . H4A H -0.2177 0.4122 0.8277 0.080 Uiso 1 calc . . . H4B H -0.2224 0.4286 0.6556 0.080 Uiso 1 calc . . . H4C H -0.0641 0.4897 0.7751 0.080 Uiso 1 calc . . . C5 C -0.0133(9) 0.2854(6) 0.8069(8) 0.0507(16) Uani 1 d . . . H5A H -0.0680 0.3037 0.9020 0.080 Uiso 1 calc . . . H5B H 0.0871 0.3524 0.8293 0.080 Uiso 1 calc . . . C6 C -0.1424(11) 0.0513(8) 0.8899(10) 0.066(2) Uani 1 d . . . H6A H -0.1381 -0.0298 0.8904 0.080 Uiso 1 calc . . . H6B H -0.2404 0.0415 0.8295 0.080 Uiso 1 calc . . . H6C H -0.1366 0.1045 0.9993 0.080 Uiso 1 calc . . . C7 C -0.2699(8) 0.1880(7) 0.6118(8) 0.0479(15) Uani 1 d . . . H7A H -0.3380 0.2140 0.5487 0.080 Uiso 1 calc . . . H7B H -0.3195 0.1818 0.7081 0.080 Uiso 1 calc . . . C8 C -0.3330(9) 0.0245(8) 0.2697(9) 0.0598(19) Uani 1 d . . . H8A H -0.3393 -0.0538 0.1883 0.080 Uiso 1 calc . . . H8B H -0.2547 0.0923 0.2486 0.080 Uiso 1 calc . . . H8C H -0.4346 0.0388 0.2672 0.080 Uiso 1 calc . . . C9 C -0.5434(16) 0.3412(12) 0.1102(16) 0.103(3) Uiso 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 Ru1 0.0243(3) 0.0379(4) 0.0318(3) 0.0058(3) 0.0069(2) 0.0100(3) Se1 0.0393(3) 0.0430(4) 0.0420(4) 0.0108(3) 0.0134(3) 0.0117(3) Se2 0.0446(4) 0.0532(4) 0.0340(3) 0.0035(3) 0.0041(3) 0.0207(3) Se3 0.0263(3) 0.0486(4) 0.0482(4) 0.0129(3) 0.0079(2) 0.0129(3) S1 0.106(2) 0.127(2) 0.0758(16) 0.0316(15) 0.0256(14) 0.0859(19) F1 0.140(7) 0.236(10) 0.106(6) 0.075(7) -0.032(5) -0.001(7) F2 0.169(9) 0.268(13) 0.237(11) 0.068(10) 0.046(8) 0.176(10) F3 0.223(12) 0.307(16) 0.161(9) 0.023(10) 0.037(8) -0.181(12) O1 0.124(7) 0.229(11) 0.098(6) 0.064(7) 0.011(5) 0.100(8) O2 0.155(10) 0.138(8) 0.194(11) 0.025(8) 0.047(8) -0.080(8) O3 0.337(18) 0.201(11) 0.213(12) 0.105(10) 0.199(13) 0.211(13) C1 0.034(4) 0.059(4) 0.088(6) 0.012(4) 0.004(4) 0.007(3) C2 0.040(3) 0.045(4) 0.057(4) 0.010(3) 0.008(3) 0.018(3) C3 0.047(4) 0.046(4) 0.054(4) 0.008(3) 0.013(3) 0.023(3) C4 0.069(5) 0.058(4) 0.073(5) 0.012(4) 0.020(4) 0.036(4) C5 0.056(4) 0.041(3) 0.047(4) 0.001(3) 0.011(3) 0.016(3) C6 0.086(6) 0.076(5) 0.056(4) 0.028(4) 0.038(4) 0.046(5) C7 0.036(3) 0.054(4) 0.053(4) 0.009(3) 0.012(3) 0.019(3) C8 0.054(4) 0.072(5) 0.055(4) 0.019(4) 0.000(3) 0.025(4) _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 Ru1 Se2 2.4701(7) 2_556 ? Ru1 Se2 2.4701(7) . ? Ru1 Se3 2.4781(6) 2_556 ? Ru1 Se3 2.4781(6) . ? Ru1 Se1 2.4808(7) . ? Ru1 Se1 2.4808(7) 2_556 ? Se1 C1 1.953(7) . ? Se1 C2 1.975(6) . ? Se2 C6 1.955(8) . ? Se2 C5 1.968(7) . ? Se3 C8 1.958(7) . ? Se3 C7 1.970(7) . ? S1 O3 1.353(9) . ? S1 O1 1.373(8) . ? S1 O2 1.522(10) . ? S1 C9 1.767(14) . ? F1 C9 1.332(14) . ? F2 C9 1.208(15) . ? F3 C9 1.403(16) . ? C2 C3 1.502(10) . ? C3 C5 1.522(10) . ? C3 C7 1.544(9) . ? C3 C4 1.556(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se2 Ru1 Se2 180.0 2_556 . ? Se2 Ru1 Se3 87.56(2) 2_556 2_556 ? Se2 Ru1 Se3 92.44(2) . 2_556 ? Se2 Ru1 Se3 92.44(2) 2_556 . ? Se2 Ru1 Se3 87.56(2) . . ? Se3 Ru1 Se3 180.0 2_556 . ? Se2 Ru1 Se1 89.81(2) 2_556 . ? Se2 Ru1 Se1 90.19(2) . . ? Se3 Ru1 Se1 90.99(2) 2_556 . ? Se3 Ru1 Se1 89.02(2) . . ? Se2 Ru1 Se1 90.19(2) 2_556 2_556 ? Se2 Ru1 Se1 89.82(2) . 2_556 ? Se3 Ru1 Se1 89.01(2) 2_556 2_556 ? Se3 Ru1 Se1 90.98(2) . 2_556 ? Se1 Ru1 Se1 180.0 . 2_556 ? C1 Se1 C2 98.1(3) . . ? C1 Se1 Ru1 109.1(3) . . ? C2 Se1 Ru1 109.3(2) . . ? C6 Se2 C5 97.8(3) . . ? C6 Se2 Ru1 108.1(3) . . ? C5 Se2 Ru1 109.2(2) . . ? C8 Se3 C7 97.5(3) . . ? C8 Se3 Ru1 109.8(2) . . ? C7 Se3 Ru1 109.59(19) . . ? O3 S1 O1 125.1(7) . . ? O3 S1 O2 109.3(8) . . ? O1 S1 O2 108.4(7) . . ? O3 S1 C9 108.7(9) . . ? O1 S1 C9 106.6(6) . . ? O2 S1 C9 94.5(7) . . ? C3 C2 Se1 120.7(5) . . ? C2 C3 C5 114.1(6) . . ? C2 C3 C7 112.3(6) . . ? C5 C3 C7 112.3(6) . . ? C2 C3 C4 105.8(6) . . ? C5 C3 C4 106.1(6) . . ? C7 C3 C4 105.3(6) . . ? C3 C5 Se2 120.7(4) . . ? C3 C7 Se3 120.3(4) . . ? F2 C9 F1 118.4(13) . . ? F2 C9 F3 106.9(14) . . ? F1 C9 F3 105.0(11) . . ? F2 C9 S1 115.8(11) . . ? F1 C9 S1 109.9(10) . . ? F3 C9 S1 98.0(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.241 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.131