# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_FeC60Me5CpAc _ccdc_journal_depnumber ? # #------------------------------------------------------------------------- _audit_creation_date 2004-10-01T17:28:31-00:00 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; FeC60Me5C5H4COMe ; _chemical_formula_moiety 'C72.50 H22 Fe1 O1 S1' _chemical_formula_sum 'C72.50 H22 Fe O S' _chemical_formula_weight 996.81 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7620(5) _cell_length_b 16.7030(6) _cell_length_c 20.5620(9) _cell_angle_alpha 90 _cell_angle_beta 95.519(3) _cell_angle_gamma 90 _cell_volume 4020.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7597 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.67 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_unetI/netI 0.0425 _diffrn_reflns_number 7597 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.67 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 7597 _reflns_number_gt 5742 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1266P)^2^+0.4145P] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0060(8) _refine_ls_number_reflns 7597 _refine_ls_number_parameters 683 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1848 _refine_ls_wR_factor_gt 0.166 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.624 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.081 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' 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 Fe Fe 0.53686(4) 0.31343(2) 0.92364(2) 0.03590(17) Uani 1 1 d . . . O O 0.6159(4) 0.3349(2) 1.11215(15) 0.0937(12) Uani 1 1 d . . . S S 0.07969(16) 0.55645(11) 0.96701(11) 0.1142(6) Uani 1 1 d . . . C1 C 0.4217(2) 0.22188(17) 0.94238(13) 0.0325(6) Uani 1 1 d . . . C2 C 0.3618(3) 0.29546(17) 0.92886(14) 0.0327(6) Uani 1 1 d . . . C3 C 0.3838(3) 0.32083(16) 0.86482(14) 0.0317(6) Uani 1 1 d . . . C4 C 0.4559(3) 0.26296(16) 0.83883(14) 0.0326(6) Uani 1 1 d . . . C5 C 0.4801(2) 0.20196(17) 0.88678(14) 0.0331(6) Uani 1 1 d . . . C6 C 0.3906(3) 0.16197(18) 0.99315(15) 0.0369(7) Uani 1 1 d . . . C7 C 0.2623(3) 0.32308(17) 0.96367(15) 0.0367(7) Uani 1 1 d . . . C8 C 0.3088(3) 0.37923(16) 0.82407(14) 0.0355(6) Uani 1 1 d . . . C9 C 0.4676(3) 0.25269(17) 0.76683(14) 0.0357(6) Uani 1 1 d . . . C10 C 0.5184(3) 0.11829(17) 0.87117(15) 0.0359(6) Uani 1 1 d . . . C11 C 0.2642(3) 0.17584(19) 1.00185(14) 0.0388(7) Uani 1 1 d . . . C12 C 0.2072(3) 0.24657(18) 0.98974(14) 0.0383(7) Uani 1 1 d . . . C13 C 0.1684(3) 0.34818(17) 0.90992(15) 0.0370(7) Uani 1 1 d . . . C14 C 0.1898(3) 0.37273(17) 0.84838(16) 0.0376(7) Uani 1 1 d . . . C15 C 0.2866(3) 0.34025(17) 0.75597(14) 0.0368(7) Uani 1 1 d . . . C16 C 0.3562(3) 0.28486(18) 0.73088(14) 0.0369(7) Uani 1 1 d . . . C17 C 0.4537(3) 0.16221(18) 0.75277(15) 0.0367(7) Uani 1 1 d . . . C18 C 0.4764(3) 0.10327(17) 0.79897(15) 0.0374(7) Uani 1 1 d . . . C19 C 0.4407(3) 0.06073(17) 0.90525(15) 0.0370(7) Uani 1 1 d . . . C20 C 0.3845(3) 0.07985(17) 0.95873(15) 0.0379(7) Uani 1 1 d . . . C21 C 0.2027(3) 0.10095(19) 0.99365(15) 0.0413(7) Uani 1 1 d . . . C22 C 0.0873(3) 0.24523(19) 0.96803(15) 0.0410(7) Uani 1 1 d . . . C23 C 0.0639(3) 0.30785(18) 0.91888(16) 0.0404(7) Uani 1 1 d . . . C24 C 0.1060(3) 0.35760(17) 0.79407(16) 0.0408(7) Uani 1 1 d . . . C25 C 0.1651(3) 0.33719(18) 0.73775(15) 0.0398(7) Uani 1 1 d . . . C26 C 0.3065(3) 0.22424(19) 0.68657(14) 0.0392(7) Uani 1 1 d . . . C27 C 0.3668(3) 0.14956(19) 0.70027(14) 0.0388(7) Uani 1 1 d . . . C28 C 0.4116(3) 0.02977(17) 0.79340(16) 0.0394(7) Uani 1 1 d . . . C29 C 0.3898(3) 0.00392(16) 0.85803(16) 0.0400(7) Uani 1 1 d . . . C30 C 0.2764(3) 0.04237(18) 0.96712(15) 0.0403(7) Uani 1 1 d . . . C31 C 0.0851(3) 0.0993(2) 0.97574(16) 0.0443(8) Uani 1 1 d . . . C32 C 0.0259(3) 0.1735(2) 0.96262(17) 0.0429(7) Uani 1 1 d . . . C33 C -0.0203(3) 0.2958(2) 0.86737(18) 0.0446(8) Uani 1 1 d . . . C34 C 0.0014(3) 0.32142(19) 0.80260(18) 0.0443(8) Uani 1 1 d . . . C35 C 0.1167(3) 0.2820(2) 0.69176(15) 0.0440(7) Uani 1 1 d . . . C36 C 0.1901(3) 0.2235(2) 0.66571(15) 0.0443(8) Uani 1 1 d . . . C37 C 0.3079(3) 0.0773(2) 0.69256(15) 0.0439(8) Uani 1 1 d . . . C38 C 0.3306(3) 0.01566(18) 0.74060(16) 0.0419(7) Uani 1 1 d . . . C39 C 0.2883(3) -0.03562(17) 0.86749(17) 0.0427(7) Uani 1 1 d . . . C40 C 0.2299(3) -0.01535(18) 0.92413(17) 0.0446(8) Uani 1 1 d . . . C41 C 0.0371(3) 0.0405(2) 0.92971(16) 0.0447(8) Uani 1 1 d . . . C42 C -0.0601(3) 0.1611(2) 0.90736(18) 0.0460(8) Uani 1 1 d . . . C43 C -0.0820(3) 0.2206(2) 0.86111(18) 0.0457(8) Uani 1 1 d . . . C44 C -0.0477(3) 0.2630(2) 0.75619(17) 0.0468(8) Uani 1 1 d . . . C45 C 0.0092(3) 0.2438(2) 0.70163(17) 0.0468(8) Uani 1 1 d . . . C46 C 0.1289(3) 0.1486(2) 0.65950(15) 0.0456(8) Uani 1 1 d . . . C47 C 0.1856(3) 0.0770(2) 0.67209(15) 0.0444(8) Uani 1 1 d . . . C48 C 0.2241(3) -0.02411(18) 0.75054(17) 0.0439(8) Uani 1 1 d . . . C49 C 0.2025(3) -0.04919(18) 0.81243(17) 0.0429(7) Uani 1 1 d . . . C50 C 0.1081(3) -0.01638(18) 0.90426(17) 0.0446(8) Uani 1 1 d . . . C51 C -0.0529(3) 0.0781(2) 0.88770(17) 0.0448(8) Uani 1 1 d . . . C52 C -0.0991(3) 0.2000(2) 0.79207(18) 0.0471(8) Uani 1 1 d . . . C53 C 0.0167(3) 0.1608(2) 0.68123(16) 0.0466(8) Uani 1 1 d . . . C54 C 0.1340(3) 0.01393(19) 0.70790(16) 0.0444(8) Uani 1 1 d . . . C55 C 0.0907(3) -0.03730(18) 0.83507(17) 0.0454(8) Uani 1 1 d . . . C56 C -0.0691(3) 0.0585(2) 0.82129(18) 0.0460(8) Uani 1 1 d . . . C57 C -0.0931(3) 0.1205(2) 0.77227(18) 0.0479(8) Uani 1 1 d . . . C58 C -0.0339(3) 0.1005(2) 0.71625(17) 0.0468(8) Uani 1 1 d . . . C59 C 0.0265(3) 0.02584(19) 0.72998(17) 0.0453(8) Uani 1 1 d . . . C60 C 0.0048(3) -0.00030(19) 0.79488(18) 0.0461(8) Uani 1 1 d . . . C61 C 0.4668(3) 0.1619(2) 1.05781(16) 0.0514(9) Uani 1 1 d . . . H61A H 0.4399 0.1223 1.0865 0.077 Uiso 1 1 calc R . . H61B H 0.4644 0.2137 1.0778 0.077 Uiso 1 1 calc R . . H61C H 0.5439 0.1497 1.0497 0.077 Uiso 1 1 calc R . . C62 C 0.2906(3) 0.38679(19) 1.01616(16) 0.0463(8) Uani 1 1 d . . . H62A H 0.2225 0.4009 1.0358 0.07 Uiso 1 1 calc R . . H62B H 0.3207 0.4334 0.9966 0.07 Uiso 1 1 calc R . . H62C H 0.3464 0.366 1.049 0.07 Uiso 1 1 calc R . . C63 C 0.3505(3) 0.46622(17) 0.82064(18) 0.0478(8) Uani 1 1 d . . . H63A H 0.2957 0.497 0.7936 0.072 Uiso 1 1 calc R . . H63B H 0.4226 0.4673 0.8024 0.072 Uiso 1 1 calc R . . H63C H 0.3594 0.4887 0.8638 0.072 Uiso 1 1 calc R . . C64 C 0.5758(3) 0.2890(2) 0.74184(17) 0.0483(8) Uani 1 1 d . . . H64A H 0.5751 0.2793 0.6958 0.072 Uiso 1 1 calc R . . H64B H 0.6423 0.2646 0.7643 0.072 Uiso 1 1 calc R . . H64C H 0.5774 0.3456 0.7498 0.072 Uiso 1 1 calc R . . C65 C 0.6463(3) 0.1010(2) 0.8870(2) 0.0522(9) Uani 1 1 d . . . H65A H 0.662 0.0467 0.8755 0.078 Uiso 1 1 calc R . . H65B H 0.6669 0.1087 0.9329 0.078 Uiso 1 1 calc R . . H65C H 0.6899 0.1368 0.8626 0.078 Uiso 1 1 calc R . . C66 C 0.6549(3) 0.33724(19) 1.00262(16) 0.0421(7) Uani 1 1 d . . . C67 C 0.5893(3) 0.40714(19) 0.98353(19) 0.0486(8) Uani 1 1 d . . . H67 H 0.5422 0.4351 1.0094 0.058 Uiso 1 1 calc R . . C68 C 0.6084(4) 0.4262(2) 0.9188(2) 0.0600(10) Uani 1 1 d . . . H68 H 0.5776 0.4696 0.8948 0.072 Uiso 1 1 calc R . . C69 C 0.6824(4) 0.3679(3) 0.89658(18) 0.0641(12) Uani 1 1 d . . . H69 H 0.7077 0.3661 0.8551 0.077 Uiso 1 1 calc R . . C70 C 0.7119(3) 0.3129(2) 0.94733(18) 0.0505(9) Uani 1 1 d . . . H70 H 0.7597 0.2688 0.9453 0.061 Uiso 1 1 calc R . . C71 C 0.6693(4) 0.3062(2) 1.07021(19) 0.0606(11) Uani 1 1 d . . . C72 C 0.7595(4) 0.2418(3) 1.0844(3) 0.0949(19) Uani 1 1 d . . . H72A H 0.7621 0.2262 1.1294 0.142 Uiso 1 1 calc R . . H72B H 0.8327 0.2624 1.0756 0.142 Uiso 1 1 calc R . . H72C H 0.7409 0.1962 1.0571 0.142 Uiso 1 1 calc R . . C101 C 0 0.5 1 0.0683(16) Uani 1 2 d S . . 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 Fe 0.0354(3) 0.0366(3) 0.0355(3) 0.00051(17) 0.00256(18) -0.00506(17) O 0.151(4) 0.088(2) 0.0435(17) -0.0035(16) 0.018(2) -0.023(2) S 0.0979(12) 0.0929(10) 0.1521(16) 0.0234(10) 0.0145(11) 0.0004(9) C1 0.0332(16) 0.0343(14) 0.0300(14) 0.0044(12) 0.0032(11) -0.0032(11) C2 0.0368(16) 0.0315(13) 0.0301(14) -0.0035(11) 0.0049(11) -0.0030(11) C3 0.0345(16) 0.0281(13) 0.0328(14) 0.0005(11) 0.0043(12) 0.0005(11) C4 0.0349(16) 0.0319(14) 0.0314(14) 0.0008(11) 0.0056(12) -0.0016(11) C5 0.0294(15) 0.0339(14) 0.0362(15) 0.0011(12) 0.0041(11) -0.0005(11) C6 0.0371(17) 0.0388(15) 0.0348(15) 0.0083(12) 0.0029(12) -0.0047(12) C7 0.0391(17) 0.0375(15) 0.0346(15) -0.0039(12) 0.0092(12) -0.0018(12) C8 0.0408(17) 0.0283(13) 0.0369(15) 0.0013(12) 0.0018(12) 0.0001(12) C9 0.0379(17) 0.0378(15) 0.0327(14) 0.0003(12) 0.0094(12) -0.0046(12) C10 0.0331(16) 0.0328(14) 0.0422(16) 0.0006(12) 0.0052(12) 0.0026(12) C11 0.0428(18) 0.0469(17) 0.0273(14) 0.0030(12) 0.0062(12) -0.0059(13) C12 0.0429(18) 0.0420(16) 0.0317(15) -0.0043(12) 0.0120(13) -0.0060(13) C13 0.0369(17) 0.0312(14) 0.0437(16) -0.0079(13) 0.0078(13) 0.0027(12) C14 0.0392(17) 0.0282(13) 0.0455(17) -0.0018(12) 0.0038(13) 0.0030(12) C15 0.0446(18) 0.0310(14) 0.0349(15) 0.0077(12) 0.0044(13) -0.0006(12) C16 0.0430(18) 0.0386(15) 0.0295(14) 0.0038(12) 0.0052(12) -0.0048(13) C17 0.0372(17) 0.0376(15) 0.0372(15) -0.0057(13) 0.0134(12) -0.0011(12) C18 0.0321(16) 0.0357(14) 0.0454(17) -0.0070(13) 0.0092(13) 0.0038(12) C19 0.0321(16) 0.0312(14) 0.0472(17) 0.0074(13) 0.0014(13) 0.0015(11) C20 0.0399(17) 0.0337(15) 0.0393(16) 0.0087(13) -0.0003(13) 0.0017(12) C21 0.0457(19) 0.0448(17) 0.0346(15) 0.0076(13) 0.0096(13) -0.0084(14) C22 0.0357(17) 0.0485(17) 0.0411(16) -0.0090(14) 0.0154(13) -0.0008(13) C23 0.0359(17) 0.0399(16) 0.0473(18) -0.0076(13) 0.0136(14) 0.0058(12) C24 0.0424(18) 0.0284(14) 0.0510(18) 0.0059(13) 0.0004(14) 0.0091(12) C25 0.0456(19) 0.0355(15) 0.0367(16) 0.0085(13) -0.0050(13) 0.0036(13) C26 0.0453(19) 0.0462(17) 0.0269(14) -0.0012(12) 0.0079(12) -0.0061(13) C27 0.0437(18) 0.0423(16) 0.0318(15) -0.0058(13) 0.0113(12) -0.0035(13) C28 0.0354(17) 0.0310(14) 0.0528(18) -0.0066(13) 0.0097(14) 0.0060(12) C29 0.0414(18) 0.0229(13) 0.0559(19) 0.0011(13) 0.0049(14) 0.0067(12) C30 0.0449(18) 0.0355(15) 0.0406(16) 0.0150(13) 0.0048(13) -0.0036(13) C31 0.0430(19) 0.0507(18) 0.0414(17) 0.0031(14) 0.0153(14) -0.0114(14) C32 0.0371(17) 0.0489(17) 0.0450(18) -0.0053(14) 0.0159(14) -0.0045(14) C33 0.0341(17) 0.0422(16) 0.058(2) -0.0042(15) 0.0061(14) 0.0099(13) C34 0.0346(17) 0.0422(16) 0.055(2) -0.0005(15) -0.0013(14) 0.0109(13) C35 0.048(2) 0.0449(17) 0.0366(16) 0.0081(14) -0.0060(14) 0.0030(14) C36 0.055(2) 0.0483(18) 0.0289(14) 0.0012(13) -0.0001(13) -0.0039(15) C37 0.0472(19) 0.0476(18) 0.0379(16) -0.0154(14) 0.0090(14) -0.0022(14) C38 0.0453(19) 0.0344(15) 0.0472(18) -0.0112(14) 0.0108(14) 0.0037(13) C39 0.0471(19) 0.0239(13) 0.0570(19) 0.0034(13) 0.0042(15) 0.0013(12) C40 0.050(2) 0.0311(14) 0.0528(19) 0.0103(14) 0.0054(15) -0.0052(13) C41 0.0407(18) 0.0446(17) 0.0503(19) 0.0033(14) 0.0128(15) -0.0130(13) C42 0.0308(17) 0.0543(19) 0.055(2) -0.0068(16) 0.0131(14) -0.0046(14) C43 0.0289(17) 0.0493(18) 0.060(2) -0.0057(16) 0.0084(14) 0.0017(13) C44 0.0355(18) 0.0492(18) 0.0532(19) -0.0002(15) -0.0090(15) 0.0087(14) C45 0.0419(19) 0.0493(18) 0.0462(18) 0.0018(15) -0.0105(15) 0.0017(14) C46 0.049(2) 0.0532(19) 0.0338(16) -0.0070(14) -0.0015(13) -0.0057(15) C47 0.049(2) 0.0503(18) 0.0341(15) -0.0138(14) 0.0031(14) -0.0054(15) C48 0.049(2) 0.0296(14) 0.0538(19) -0.0115(14) 0.0071(15) -0.0054(13) C49 0.0454(19) 0.0275(14) 0.0560(19) -0.0054(13) 0.0058(15) -0.0047(12) C50 0.0440(19) 0.0327(15) 0.058(2) 0.0061(14) 0.0100(15) -0.0102(13) C51 0.0363(17) 0.0444(17) 0.0550(19) -0.0034(15) 0.0112(14) -0.0099(13) C52 0.0279(16) 0.0521(19) 0.060(2) -0.0009(16) -0.0025(14) 0.0012(14) C53 0.0420(19) 0.0541(19) 0.0410(17) -0.0061(15) -0.0102(14) -0.0033(15) C54 0.050(2) 0.0380(16) 0.0443(18) -0.0153(14) 0.0021(14) -0.0087(14) C55 0.046(2) 0.0327(15) 0.057(2) -0.0045(14) 0.0037(15) -0.0128(13) C56 0.0318(17) 0.0447(17) 0.061(2) -0.0080(15) 0.0046(14) -0.0109(13) C57 0.0305(17) 0.0535(19) 0.059(2) -0.0078(16) -0.0015(14) -0.0065(14) C58 0.0384(18) 0.0511(18) 0.0487(19) -0.0091(15) -0.0067(14) -0.0069(14) C59 0.0447(19) 0.0409(16) 0.0490(18) -0.0099(14) -0.0016(14) -0.0085(14) C60 0.0388(18) 0.0416(17) 0.058(2) -0.0072(15) 0.0075(15) -0.0137(14) C61 0.054(2) 0.060(2) 0.0385(17) 0.0101(16) -0.0055(15) -0.0074(16) C62 0.053(2) 0.0459(17) 0.0410(17) -0.0124(14) 0.0118(15) -0.0048(15) C63 0.056(2) 0.0297(15) 0.058(2) 0.0048(14) 0.0030(16) -0.0030(14) C64 0.049(2) 0.0546(19) 0.0440(18) -0.0005(15) 0.0162(15) -0.0134(16) C65 0.0333(18) 0.0505(19) 0.072(2) 0.0034(17) 0.0014(16) 0.0038(14) C66 0.0435(19) 0.0396(16) 0.0423(17) -0.0010(14) 0.0000(14) -0.0060(13) C67 0.045(2) 0.0384(16) 0.061(2) -0.0056(15) 0.0003(16) -0.0041(14) C68 0.063(3) 0.052(2) 0.061(2) 0.0127(18) -0.0146(19) -0.0224(18) C69 0.061(3) 0.089(3) 0.0431(19) -0.0028(19) 0.0089(17) -0.037(2) C70 0.0357(18) 0.059(2) 0.057(2) -0.0130(16) 0.0037(15) -0.0041(15) C71 0.074(3) 0.057(2) 0.047(2) 0.0067(17) -0.0135(19) -0.0243(19) C72 0.075(3) 0.089(3) 0.110(4) 0.048(3) -0.046(3) -0.019(3) C101 0.070(4) 0.061(3) 0.071(4) -0.012(3) -0.014(3) 0.017(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Fe C67 2.049(3) . ? Fe C69 2.062(4) . ? Fe C70 2.070(4) . ? Fe C68 2.069(4) . ? Fe C66 2.071(3) . ? Fe C3 2.074(3) . ? Fe C4 2.083(3) . ? Fe C2 2.094(3) . ? Fe C5 2.095(3) . ? Fe C1 2.103(3) . ? O C71 1.213(5) . ? S C101 1.5330(18) . ? C1 C5 1.428(4) . ? C1 C2 1.431(4) . ? C1 C6 1.516(4) . ? C2 C3 1.430(4) . ? C2 C7 1.502(4) . ? C3 C4 1.424(4) . ? C3 C8 1.513(4) . ? C4 C5 1.427(4) . ? C4 C9 1.510(4) . ? C5 C10 1.512(4) . ? C6 C61 1.530(4) . ? C6 C11 1.532(4) . ? C6 C20 1.542(4) . ? C7 C62 1.529(4) . ? C7 C13 1.543(4) . ? C7 C12 1.552(4) . ? C8 C14 1.536(4) . ? C8 C63 1.537(4) . ? C8 C15 1.544(4) . ? C9 C16 1.538(4) . ? C9 C64 1.541(4) . ? C9 C17 1.544(4) . ? C10 C65 1.535(4) . ? C10 C18 1.540(4) . ? C10 C19 1.541(4) . ? C11 C12 1.369(4) . ? C11 C21 1.446(4) . ? C12 C22 1.438(5) . ? C13 C14 1.376(4) . ? C13 C23 1.429(4) . ? C14 C24 1.439(5) . ? C15 C16 1.369(4) . ? C15 C25 1.442(5) . ? C16 C26 1.448(4) . ? C17 C18 1.376(4) . ? C17 C27 1.429(5) . ? C18 C28 1.444(4) . ? C19 C20 1.374(4) . ? C19 C29 1.446(4) . ? C20 C30 1.443(4) . ? C21 C31 1.398(5) . ? C21 C30 1.448(5) . ? C22 C32 1.397(4) . ? C22 C23 1.462(5) . ? C23 C33 1.394(5) . ? C24 C34 1.397(5) . ? C24 C25 1.448(5) . ? C25 C35 1.402(5) . ? C26 C36 1.395(5) . ? C26 C27 1.449(5) . ? C27 C37 1.392(4) . ? C28 C38 1.394(5) . ? C28 C29 1.444(5) . ? C29 C39 1.394(5) . ? C30 C40 1.384(5) . ? C31 C32 1.435(5) . ? C31 C41 1.440(5) . ? C32 C42 1.462(5) . ? C33 C34 1.445(5) . ? C33 C43 1.449(5) . ? C34 C44 1.445(5) . ? C35 C36 1.440(5) . ? C35 C45 1.449(5) . ? C36 C46 1.443(5) . ? C37 C38 1.435(5) . ? C37 C47 1.459(5) . ? C38 C48 1.450(5) . ? C39 C40 1.448(5) . ? C39 C49 1.460(5) . ? C40 C50 1.451(5) . ? C41 C50 1.400(5) . ? C41 C51 1.444(5) . ? C42 C43 1.383(5) . ? C42 C51 1.448(5) . ? C43 C52 1.456(5) . ? C44 C45 1.398(5) . ? C44 C52 1.451(5) . ? C45 C53 1.453(5) . ? C46 C47 1.381(5) . ? C46 C53 1.447(5) . ? C47 C54 1.452(5) . ? C48 C49 1.386(5) . ? C48 C54 1.455(5) . ? C49 C55 1.451(5) . ? C50 C55 1.460(5) . ? C51 C56 1.400(5) . ? C52 C57 1.392(5) . ? C53 C58 1.404(5) . ? C54 C59 1.398(5) . ? C55 C60 1.387(5) . ? C56 C60 1.451(5) . ? C56 C57 1.454(5) . ? C57 C58 1.442(5) . ? C58 C59 1.449(5) . ? C59 C60 1.450(5) . ? C66 C70 1.433(5) . ? C66 C67 1.433(5) . ? C66 C71 1.478(5) . ? C67 C68 1.408(5) . ? C68 C69 1.411(6) . ? C69 C70 1.408(6) . ? C71 C72 1.519(7) . ? C101 S 1.5330(18) 3_567 ? 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 C67 Fe C69 67.39(16) . . ? C67 Fe C70 68.09(14) . . ? C69 Fe C70 39.85(16) . . ? C67 Fe C68 39.98(15) . . ? C69 Fe C68 39.94(17) . . ? C70 Fe C68 67.37(16) . . ? C67 Fe C66 40.71(13) . . ? C69 Fe C66 67.39(14) . . ? C70 Fe C66 40.51(13) . . ? C68 Fe C66 67.56(14) . . ? C67 Fe C3 119.92(13) . . ? C69 Fe C3 120.87(14) . . ? C70 Fe C3 157.77(14) . . ? C68 Fe C3 104.57(13) . . ? C66 Fe C3 157.62(13) . . ? C67 Fe C4 154.01(13) . . ? C69 Fe C4 106.10(13) . . ? C70 Fe C4 124.04(13) . . ? C68 Fe C4 118.88(13) . . ? C66 Fe C4 162.22(13) . . ? C3 Fe C4 40.05(11) . . ? C67 Fe C2 108.60(13) . . ? C69 Fe C2 157.40(16) . . ? C70 Fe C2 161.50(14) . . ? C68 Fe C2 122.64(15) . . ? C66 Fe C2 125.14(12) . . ? C3 Fe C2 40.14(11) . . ? C4 Fe C2 67.18(11) . . ? C67 Fe C5 164.38(13) . . ? C69 Fe C5 122.59(15) . . ? C70 Fe C5 110.90(13) . . ? C68 Fe C5 155.27(15) . . ? C66 Fe C5 128.37(12) . . ? C3 Fe C5 67.25(11) . . ? C4 Fe C5 39.95(11) . . ? C2 Fe C5 67.07(11) . . ? C67 Fe C1 127.38(13) . . ? C69 Fe C1 159.47(16) . . ? C70 Fe C1 126.69(13) . . ? C68 Fe C1 160.54(16) . . ? C66 Fe C1 113.01(12) . . ? C3 Fe C1 67.17(11) . . ? C4 Fe C1 66.95(11) . . ? C2 Fe C1 39.87(11) . . ? C5 Fe C1 39.78(11) . . ? C5 C1 C2 108.1(2) . . ? C5 C1 C6 124.3(3) . . ? C2 C1 C6 123.6(3) . . ? C5 C1 Fe 69.83(16) . . ? C2 C1 Fe 69.73(16) . . ? C6 C1 Fe 144.0(2) . . ? C3 C2 C1 107.7(2) . . ? C3 C2 C7 124.5(3) . . ? C1 C2 C7 124.3(2) . . ? C3 C2 Fe 69.18(17) . . ? C1 C2 Fe 70.40(17) . . ? C7 C2 Fe 142.7(2) . . ? C4 C3 C2 108.1(2) . . ? C4 C3 C8 124.5(3) . . ? C2 C3 C8 123.6(3) . . ? C4 C3 Fe 70.33(17) . . ? C2 C3 Fe 70.68(17) . . ? C8 C3 Fe 142.0(2) . . ? C3 C4 C5 108.2(2) . . ? C3 C4 C9 124.0(3) . . ? C5 C4 C9 124.4(3) . . ? C3 C4 Fe 69.62(16) . . ? C5 C4 Fe 70.48(16) . . ? C9 C4 Fe 142.1(2) . . ? C4 C5 C1 107.9(2) . . ? C4 C5 C10 123.8(3) . . ? C1 C5 C10 124.1(3) . . ? C4 C5 Fe 69.57(16) . . ? C1 C5 Fe 70.39(16) . . ? C10 C5 Fe 143.8(2) . . ? C1 C6 C61 116.0(3) . . ? C1 C6 C11 106.4(2) . . ? C61 C6 C11 113.1(3) . . ? C1 C6 C20 105.9(2) . . ? C61 C6 C20 113.3(3) . . ? C11 C6 C20 100.7(2) . . ? C2 C7 C62 115.0(3) . . ? C2 C7 C13 106.2(2) . . ? C62 C7 C13 114.1(3) . . ? C2 C7 C12 106.4(2) . . ? C62 C7 C12 113.5(3) . . ? C13 C7 C12 100.2(2) . . ? C3 C8 C14 106.0(2) . . ? C3 C8 C63 117.6(3) . . ? C14 C8 C63 112.8(2) . . ? C3 C8 C15 105.6(2) . . ? C14 C8 C15 100.7(2) . . ? C63 C8 C15 112.6(2) . . ? C4 C9 C16 106.1(2) . . ? C4 C9 C64 116.0(3) . . ? C16 C9 C64 113.2(3) . . ? C4 C9 C17 106.1(2) . . ? C16 C9 C17 100.5(2) . . ? C64 C9 C17 113.5(3) . . ? C5 C10 C65 115.8(3) . . ? C5 C10 C18 106.3(2) . . ? C65 C10 C18 113.0(3) . . ? C5 C10 C19 106.1(2) . . ? C65 C10 C19 113.5(3) . . ? C18 C10 C19 100.8(2) . . ? C12 C11 C21 119.7(3) . . ? C12 C11 C6 124.9(3) . . ? C21 C11 C6 109.6(3) . . ? C11 C12 C22 119.4(3) . . ? C11 C12 C7 124.1(3) . . ? C22 C12 C7 109.6(3) . . ? C14 C13 C23 119.6(3) . . ? C14 C13 C7 123.9(3) . . ? C23 C13 C7 110.2(3) . . ? C13 C14 C24 119.3(3) . . ? C13 C14 C8 125.0(3) . . ? C24 C14 C8 109.7(3) . . ? C16 C15 C25 119.5(3) . . ? C16 C15 C8 124.8(3) . . ? C25 C15 C8 109.2(3) . . ? C15 C16 C26 119.3(3) . . ? C15 C16 C9 124.6(3) . . ? C26 C16 C9 109.4(3) . . ? C18 C17 C27 119.5(3) . . ? C18 C17 C9 124.1(3) . . ? C27 C17 C9 109.9(3) . . ? C17 C18 C28 119.2(3) . . ? C17 C18 C10 124.9(3) . . ? C28 C18 C10 109.5(3) . . ? C20 C19 C29 119.3(3) . . ? C20 C19 C10 124.8(3) . . ? C29 C19 C10 109.3(3) . . ? C19 C20 C30 119.5(3) . . ? C19 C20 C6 124.7(3) . . ? C30 C20 C6 109.5(3) . . ? C31 C21 C11 121.3(3) . . ? C31 C21 C30 120.0(3) . . ? C11 C21 C30 108.6(3) . . ? C32 C22 C12 121.4(3) . . ? C32 C22 C23 119.8(3) . . ? C12 C22 C23 108.5(3) . . ? C33 C23 C13 121.8(3) . . ? C33 C23 C22 119.6(3) . . ? C13 C23 C22 108.6(3) . . ? C34 C24 C14 121.6(3) . . ? C34 C24 C25 119.7(3) . . ? C14 C24 C25 108.4(3) . . ? C35 C25 C15 121.8(3) . . ? C35 C25 C24 119.9(3) . . ? C15 C25 C24 108.9(3) . . ? C36 C26 C16 121.7(3) . . ? C36 C26 C27 120.0(3) . . ? C16 C26 C27 108.6(3) . . ? C37 C27 C17 121.7(3) . . ? C37 C27 C26 119.6(3) . . ? C17 C27 C26 108.7(3) . . ? C38 C28 C18 121.4(3) . . ? C38 C28 C29 119.9(3) . . ? C18 C28 C29 108.7(3) . . ? C39 C29 C28 120.0(3) . . ? C39 C29 C19 121.5(3) . . ? C28 C29 C19 108.8(3) . . ? C40 C30 C20 121.6(3) . . ? C40 C30 C21 119.8(3) . . ? C20 C30 C21 108.5(3) . . ? C21 C31 C32 118.8(3) . . ? C21 C31 C41 120.2(3) . . ? C32 C31 C41 108.2(3) . . ? C22 C32 C31 119.3(3) . . ? C22 C32 C42 119.8(3) . . ? C31 C32 C42 108.1(3) . . ? C23 C33 C34 118.8(3) . . ? C23 C33 C43 120.4(3) . . ? C34 C33 C43 107.8(3) . . ? C24 C34 C44 120.6(3) . . ? C24 C34 C33 118.7(3) . . ? C44 C34 C33 108.3(3) . . ? C25 C35 C36 118.6(3) . . ? C25 C35 C45 119.9(3) . . ? C36 C35 C45 108.4(3) . . ? C26 C36 C35 119.0(3) . . ? C26 C36 C46 120.1(3) . . ? C35 C36 C46 108.0(3) . . ? C27 C37 C38 119.1(3) . . ? C27 C37 C47 120.1(3) . . ? C38 C37 C47 108.0(3) . . ? C28 C38 C37 118.9(3) . . ? C28 C38 C48 120.2(3) . . ? C37 C38 C48 108.7(3) . . ? C29 C39 C40 118.7(3) . . ? C29 C39 C49 120.2(3) . . ? C40 C39 C49 108.3(3) . . ? C30 C40 C39 119.2(3) . . ? C30 C40 C50 120.4(3) . . ? C39 C40 C50 107.6(3) . . ? C50 C41 C31 119.9(3) . . ? C50 C41 C51 120.1(3) . . ? C31 C41 C51 108.4(3) . . ? C43 C42 C51 120.5(3) . . ? C43 C42 C32 120.1(3) . . ? C51 C42 C32 107.3(3) . . ? C42 C43 C33 120.2(3) . . ? C42 C43 C52 120.0(3) . . ? C33 C43 C52 108.2(3) . . ? C45 C44 C34 119.6(3) . . ? C45 C44 C52 119.7(3) . . ? C34 C44 C52 108.3(3) . . ? C44 C45 C35 120.2(3) . . ? C44 C45 C53 119.9(3) . . ? C35 C45 C53 107.5(3) . . ? C47 C46 C36 120.4(3) . . ? C47 C46 C53 120.2(3) . . ? C36 C46 C53 108.1(3) . . ? C46 C47 C54 120.3(3) . . ? C46 C47 C37 119.8(3) . . ? C54 C47 C37 107.8(3) . . ? C49 C48 C38 120.3(3) . . ? C49 C48 C54 119.9(3) . . ? C38 C48 C54 107.7(3) . . ? C48 C49 C55 120.3(3) . . ? C48 C49 C39 119.4(3) . . ? C55 C49 C39 108.1(3) . . ? C41 C50 C40 119.7(3) . . ? C41 C50 C55 119.6(3) . . ? C40 C50 C55 108.6(3) . . ? C56 C51 C41 120.3(3) . . ? C56 C51 C42 119.4(3) . . ? C41 C51 C42 108.0(3) . . ? C57 C52 C44 120.6(3) . . ? C57 C52 C43 120.3(3) . . ? C44 C52 C43 107.4(3) . . ? C58 C53 C46 120.1(3) . . ? C58 C53 C45 119.7(3) . . ? C46 C53 C45 107.9(3) . . ? C59 C54 C47 119.8(3) . . ? C59 C54 C48 119.7(3) . . ? C47 C54 C48 107.8(3) . . ? C60 C55 C49 120.0(3) . . ? C60 C55 C50 120.0(3) . . ? C49 C55 C50 107.4(3) . . ? C51 C56 C60 119.6(3) . . ? C51 C56 C57 120.5(3) . . ? C60 C56 C57 107.8(3) . . ? C52 C57 C58 119.8(3) . . ? C52 C57 C56 119.2(3) . . ? C58 C57 C56 108.2(3) . . ? C53 C58 C57 120.3(3) . . ? C53 C58 C59 119.6(3) . . ? C57 C58 C59 108.0(3) . . ? C54 C59 C58 120.0(3) . . ? C54 C59 C60 120.0(3) . . ? C58 C59 C60 108.2(3) . . ? C55 C60 C59 120.0(3) . . ? C55 C60 C56 120.4(3) . . ? C59 C60 C56 107.8(3) . . ? C70 C66 C67 107.1(3) . . ? C70 C66 C71 128.8(4) . . ? C67 C66 C71 123.6(3) . . ? C70 C66 Fe 69.70(19) . . ? C67 C66 Fe 68.84(19) . . ? C71 C66 Fe 132.7(2) . . ? C68 C67 C66 108.2(3) . . ? C68 C67 Fe 70.8(2) . . ? C66 C67 Fe 70.45(19) . . ? C67 C68 C69 108.0(3) . . ? C67 C68 Fe 69.25(19) . . ? C69 C68 Fe 69.7(2) . . ? C70 C69 C68 109.0(3) . . ? C70 C69 Fe 70.4(2) . . ? C68 C69 Fe 70.3(2) . . ? C69 C70 C66 107.6(3) . . ? C69 C70 Fe 69.8(2) . . ? C66 C70 Fe 69.8(2) . . ? O C71 C66 120.6(4) . . ? O C71 C72 122.9(4) . . ? C66 C71 C72 116.4(4) . . ? S C101 S 180.00(11) 3_567 . ? #===END _database_code_depnum_ccdc_archive 'CCDC 950092' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_RuC60Me5AcCp _audit_creation_date 2004-10-01T15:57:13-00:00 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; RuC60Me5C5H4COMe ; _chemical_formula_moiety 'C72 H22 O1 Ru1' _chemical_formula_structural 'C72 H22 O1 RU1' _chemical_formula_sum 'C72.50 H22 O Ru S' _chemical_formula_weight 1042.03 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7120(4) _cell_length_b 16.7440(4) _cell_length_c 20.5640(8) _cell_angle_alpha 90 _cell_angle_beta 94.978(2) _cell_angle_gamma 90 _cell_volume 4017.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7639 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 25.73 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2100 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.503 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_number 7639 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.73 _diffrn_reflns_theta_full 25.73 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 7639 _reflns_number_gt 6066 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.2000P)^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_number_reflns 7639 _refine_ls_number_parameters 682 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.2902 _refine_ls_wR_factor_gt 0.2503 _refine_ls_goodness_of_fit_ref 1.32 _refine_ls_restrained_S_all 1.32 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 8.436 _refine_diff_density_min -2.33 _refine_diff_density_rms 0.208 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ru Ru 0.45891(3) 0.31523(2) 0.073614(18) 0.0248(2) Uani 1 1 d . . . O O 0.3779(4) 0.3342(3) -0.1173(2) 0.0523(12) Uani 1 1 d . . . S S 0.92310(17) 0.55199(11) 0.04049(10) 0.0609(5) Uani 1 1 d . . . C1 C 0.5840(4) 0.2192(3) 0.0577(2) 0.0243(10) Uani 1 1 d . . . C2 C 0.6440(4) 0.2912(3) 0.0714(2) 0.0246(10) Uani 1 1 d . . . C3 C 0.6209(4) 0.3187(2) 0.1352(3) 0.0231(10) Uani 1 1 d . . . C4 C 0.5472(4) 0.2610(3) 0.1613(2) 0.0239(9) Uani 1 1 d . . . C5 C 0.5241(4) 0.2000(3) 0.1134(3) 0.0265(10) Uani 1 1 d . . . C6 C 0.6152(4) 0.1591(3) 0.0070(2) 0.0275(10) Uani 1 1 d . . . C7 C 0.7439(5) 0.3194(3) 0.0368(3) 0.0278(11) Uani 1 1 d . . . C8 C 0.6940(4) 0.3773(2) 0.1759(2) 0.0249(10) Uani 1 1 d . . . C9 C 0.5315(4) 0.2507(3) 0.2330(2) 0.0280(10) Uani 1 1 d . . . C10 C 0.4841(4) 0.1160(3) 0.1290(2) 0.0260(10) Uani 1 1 d . . . C11 C 0.7433(5) 0.1726(3) -0.0015(2) 0.0266(10) Uani 1 1 d . . . C12 C 0.8004(4) 0.2447(3) 0.0108(2) 0.0271(10) Uani 1 1 d . . . C13 C 0.8383(4) 0.3464(3) 0.0907(2) 0.0259(10) Uani 1 1 d . . . C14 C 0.8154(4) 0.3696(3) 0.1522(2) 0.0276(10) Uani 1 1 d . . . C15 C 0.7147(4) 0.3383(3) 0.2445(2) 0.0264(10) Uani 1 1 d . . . C16 C 0.6441(4) 0.2837(3) 0.2699(2) 0.0279(10) Uani 1 1 d . . . C17 C 0.5460(4) 0.1609(3) 0.2477(2) 0.0266(10) Uani 1 1 d . . . C18 C 0.5242(4) 0.1020(3) 0.2021(2) 0.0270(10) Uani 1 1 d . . . C19 C 0.5629(4) 0.0582(3) 0.0947(2) 0.0280(10) Uani 1 1 d . . . C20 C 0.6209(4) 0.0772(3) 0.0420(2) 0.0277(10) Uani 1 1 d . . . C21 C 0.8049(4) 0.0978(3) 0.0072(2) 0.0284(10) Uani 1 1 d . . . C22 C 0.9203(4) 0.2426(3) 0.0328(2) 0.0306(11) Uani 1 1 d . . . C23 C 0.9439(4) 0.3052(3) 0.0818(3) 0.0296(12) Uani 1 1 d . . . C24 C 0.8985(4) 0.3556(3) 0.2066(2) 0.0285(10) Uani 1 1 d . . . C25 C 0.8374(4) 0.3361(3) 0.2622(2) 0.0296(10) Uani 1 1 d . . . C26 C 0.6936(4) 0.2239(3) 0.3142(2) 0.0276(10) Uani 1 1 d . . . C27 C 0.6320(4) 0.1488(3) 0.2996(2) 0.0309(11) Uani 1 1 d . . . C28 C 0.5901(4) 0.0286(3) 0.2077(2) 0.0261(10) Uani 1 1 d . . . C29 C 0.6129(4) 0.0020(2) 0.1426(3) 0.0288(11) Uani 1 1 d . . . C30 C 0.7299(4) 0.0401(3) 0.0342(2) 0.0305(11) Uani 1 1 d . . . C31 C 0.9222(4) 0.0953(3) 0.0258(2) 0.0321(11) Uani 1 1 d . . . C32 C 0.9827(4) 0.1713(3) 0.0390(2) 0.0284(10) Uani 1 1 d . . . C33 C 1.0261(4) 0.2936(3) 0.1329(3) 0.0296(11) Uani 1 1 d . . . C34 C 1.0024(5) 0.3196(3) 0.1982(3) 0.0329(12) Uani 1 1 d . . . C35 C 0.8830(5) 0.2803(3) 0.3088(2) 0.0331(11) Uani 1 1 d . . . C36 C 0.8090(4) 0.2231(3) 0.3350(2) 0.0288(10) Uani 1 1 d . . . C37 C 0.6910(4) 0.0761(3) 0.3080(3) 0.0318(11) Uani 1 1 d . . . C38 C 0.6698(4) 0.0143(3) 0.2606(2) 0.0291(10) Uani 1 1 d . . . C39 C 0.7160(4) -0.0373(3) 0.1336(2) 0.0287(10) Uani 1 1 d . . . C40 C 0.7750(5) -0.0177(3) 0.0774(3) 0.0339(12) Uani 1 1 d . . . C41 C 0.9692(4) 0.0375(3) 0.0715(2) 0.0303(12) Uani 1 1 d . . . C42 C 1.0663(4) 0.1581(3) 0.0938(2) 0.0313(11) Uani 1 1 d . . . C43 C 1.0890(4) 0.2184(3) 0.1397(3) 0.0303(11) Uani 1 1 d . . . C44 C 1.0507(4) 0.2617(3) 0.2453(3) 0.0331(11) Uani 1 1 d . . . C45 C 0.9915(4) 0.2421(3) 0.2991(3) 0.0329(11) Uani 1 1 d . . . C46 C 0.8706(5) 0.1467(3) 0.3412(2) 0.0306(11) Uani 1 1 d . . . C47 C 0.8137(4) 0.0757(3) 0.3288(2) 0.0271(10) Uani 1 1 d . . . C48 C 0.7774(4) -0.0251(3) 0.2511(2) 0.0308(11) Uani 1 1 d . . . C49 C 0.8006(4) -0.0504(3) 0.1893(2) 0.0286(10) Uani 1 1 d . . . C50 C 0.8973(4) -0.0186(3) 0.0974(3) 0.0308(11) Uani 1 1 d . . . C51 C 1.0582(4) 0.0757(3) 0.1148(3) 0.0311(11) Uani 1 1 d . . . C52 C 1.1040(4) 0.1980(3) 0.2093(3) 0.0306(11) Uani 1 1 d . . . C53 C 0.9844(4) 0.1601(3) 0.3195(3) 0.0308(11) Uani 1 1 d . . . C54 C 0.8665(5) 0.0136(3) 0.2935(2) 0.0294(11) Uani 1 1 d . . . C55 C 0.9126(5) -0.0388(3) 0.1663(3) 0.0321(11) Uani 1 1 d . . . C56 C 1.0724(5) 0.0562(3) 0.1801(3) 0.0333(11) Uani 1 1 d . . . C57 C 1.0976(4) 0.1183(3) 0.2293(3) 0.0346(12) Uani 1 1 d . . . C58 C 1.0356(4) 0.0990(3) 0.2850(2) 0.0309(11) Uani 1 1 d . . . C59 C 0.9758(4) 0.0240(3) 0.2718(2) 0.0301(10) Uani 1 1 d . . . C60 C 0.9991(4) -0.0018(3) 0.2066(3) 0.0338(12) Uani 1 1 d . . . C61 C 0.5378(5) 0.1592(3) -0.0575(3) 0.0352(12) Uani 1 1 d . . . H61A H 0.5649 0.1187 -0.087 0.053 Uiso 1 1 calc R . . H61B H 0.5405 0.2119 -0.078 0.053 Uiso 1 1 calc R . . H61C H 0.4588 0.1471 -0.0486 0.053 Uiso 1 1 calc R . . C62 C 0.7146(4) 0.3839(3) -0.0158(2) 0.0308(11) Uani 1 1 d . . . H62A H 0.7842 0.3989 -0.0361 0.046 Uiso 1 1 calc R . . H62B H 0.683 0.431 0.0045 0.046 Uiso 1 1 calc R . . H62C H 0.6579 0.3627 -0.0492 0.046 Uiso 1 1 calc R . . C63 C 0.6500(5) 0.4641(3) 0.1767(3) 0.0345(11) Uani 1 1 d . . . H63A H 0.7036 0.4967 0.2046 0.052 Uiso 1 1 calc R . . H63B H 0.5744 0.4651 0.1938 0.052 Uiso 1 1 calc R . . H63C H 0.6438 0.4856 0.1322 0.052 Uiso 1 1 calc R . . C64 C 0.4233(4) 0.2885(3) 0.2566(3) 0.0313(11) Uani 1 1 d . . . H64A H 0.4213 0.2786 0.3035 0.047 Uiso 1 1 calc R . . H64B H 0.3554 0.2648 0.2329 0.047 Uiso 1 1 calc R . . H64C H 0.4241 0.3461 0.2486 0.047 Uiso 1 1 calc R . . C65 C 0.3556(4) 0.0997(3) 0.1130(3) 0.0336(11) Uani 1 1 d . . . H65A H 0.3386 0.0443 0.1242 0.05 Uiso 1 1 calc R . . H65B H 0.3352 0.1084 0.0663 0.05 Uiso 1 1 calc R . . H65C H 0.311 0.136 0.1384 0.05 Uiso 1 1 calc R . . C66 C 0.3339(4) 0.3435(3) -0.0089(2) 0.0310(11) Uani 1 1 d . . . C67 C 0.4005(4) 0.4135(3) 0.0096(2) 0.0303(11) Uani 1 1 d . . . H67 H 0.4493 0.4415 -0.017 0.036 Uiso 1 1 calc R . . C68 C 0.3801(5) 0.4331(3) 0.0747(3) 0.0347(12) Uani 1 1 d . . . H68 H 0.413 0.4768 0.0992 0.042 Uiso 1 1 calc R . . C69 C 0.3013(5) 0.3760(3) 0.0973(3) 0.0376(12) Uani 1 1 d . . . H69 H 0.2724 0.3759 0.1391 0.045 Uiso 1 1 calc R . . C70 C 0.2735(5) 0.3190(3) 0.0461(3) 0.0306(12) Uani 1 1 d . . . H70 H 0.2247 0.2739 0.048 0.037 Uiso 1 1 calc R . . C71 C 0.3244(5) 0.3080(3) -0.0748(3) 0.0363(13) Uani 1 1 d . . . C72 C 0.2412(6) 0.2395(3) -0.0862(3) 0.0489(15) Uani 1 1 d . . . H72A H 0.2416 0.2207 -0.1314 0.073 Uiso 1 1 calc R . . H72B H 0.1639 0.2575 -0.0785 0.073 Uiso 1 1 calc R . . H72C H 0.264 0.1957 -0.0562 0.073 Uiso 1 1 calc R . . C101 C 1 0.5 0 0.044(2) Uani 1 2 d S . . 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 Ru 0.0262(3) 0.0232(3) 0.0251(3) 0.00047(12) 0.0024(2) 0.00211(12) O 0.081(4) 0.050(2) 0.027(2) -0.0005(18) 0.008(2) 0.005(2) S 0.0558(11) 0.0564(10) 0.0701(12) -0.0155(9) 0.0030(9) 0.0020(8) C1 0.027(2) 0.020(2) 0.026(2) 0.0009(18) 0.0035(18) 0.0051(17) C2 0.026(2) 0.020(2) 0.027(2) 0.0026(19) 0.0007(18) 0.0033(18) C3 0.020(2) 0.024(2) 0.025(3) -0.0021(17) 0.0014(19) 0.0030(16) C4 0.025(2) 0.024(2) 0.022(2) 0.0031(17) 0.0020(18) 0.0014(17) C5 0.023(2) 0.020(2) 0.036(3) 0.001(2) 0.003(2) 0.0068(18) C6 0.035(3) 0.022(2) 0.026(2) -0.001(2) 0.006(2) 0.0008(19) C7 0.026(3) 0.032(3) 0.025(3) 0.0005(18) 0.003(2) 0.0019(18) C8 0.038(3) 0.018(2) 0.019(2) -0.0009(17) 0.0035(19) 0.0023(18) C9 0.027(2) 0.031(2) 0.026(2) -0.002(2) 0.0032(19) 0.0030(19) C10 0.027(2) 0.022(2) 0.030(2) 0.0027(18) 0.0047(19) -0.0029(18) C11 0.033(3) 0.029(2) 0.018(2) 0.0002(18) 0.0029(19) 0.006(2) C12 0.035(3) 0.030(2) 0.017(2) 0.0010(18) 0.0055(19) 0.001(2) C13 0.027(2) 0.021(2) 0.031(2) 0.0048(19) 0.0067(19) -0.0041(18) C14 0.032(3) 0.020(2) 0.031(3) -0.0034(18) 0.002(2) -0.0041(18) C15 0.035(3) 0.019(2) 0.026(2) -0.0053(19) 0.005(2) -0.0026(19) C16 0.027(3) 0.033(3) 0.025(2) -0.002(2) 0.0040(19) 0.003(2) C17 0.028(3) 0.024(2) 0.029(2) 0.005(2) 0.013(2) -0.0036(19) C18 0.021(2) 0.024(2) 0.036(3) 0.008(2) 0.0056(19) -0.0006(18) C19 0.026(2) 0.022(2) 0.036(3) -0.0054(19) 0.002(2) 0.0019(18) C20 0.033(3) 0.017(2) 0.032(3) -0.0059(18) 0.001(2) 0.0012(18) C21 0.032(3) 0.030(2) 0.024(2) -0.0058(19) 0.006(2) 0.004(2) C22 0.029(3) 0.032(3) 0.033(3) 0.007(2) 0.012(2) 0.002(2) C23 0.024(3) 0.032(3) 0.034(3) 0.002(2) 0.007(2) -0.0047(19) C24 0.031(3) 0.021(2) 0.034(3) -0.0011(19) 0.002(2) -0.0102(18) C25 0.035(3) 0.028(2) 0.026(2) -0.006(2) 0.000(2) 0.002(2) C26 0.035(3) 0.027(2) 0.022(2) 0.0022(18) 0.009(2) 0.002(2) C27 0.031(3) 0.035(3) 0.028(3) -0.007(2) 0.008(2) -0.001(2) C28 0.031(3) 0.021(2) 0.028(2) 0.0012(18) 0.0091(19) 0.0011(18) C29 0.038(3) 0.0129(19) 0.037(3) -0.0033(19) 0.010(2) -0.0077(18) C30 0.034(3) 0.029(2) 0.029(3) -0.007(2) 0.006(2) 0.001(2) C31 0.030(3) 0.040(3) 0.028(3) -0.010(2) 0.009(2) 0.002(2) C32 0.027(3) 0.033(2) 0.026(3) 0.002(2) 0.009(2) 0.0024(19) C33 0.027(3) 0.023(2) 0.039(3) 0.004(2) 0.002(2) -0.003(2) C34 0.030(3) 0.023(3) 0.045(3) 0.001(2) -0.004(2) -0.0025(18) C35 0.036(3) 0.033(3) 0.029(3) -0.003(2) -0.002(2) -0.001(2) C36 0.041(3) 0.026(2) 0.019(2) 0.0004(18) 0.001(2) 0.001(2) C37 0.034(3) 0.029(3) 0.034(3) 0.009(2) 0.007(2) -0.003(2) C38 0.029(3) 0.027(2) 0.033(3) 0.004(2) 0.009(2) 0.0006(19) C39 0.033(3) 0.020(2) 0.034(3) -0.0019(19) 0.004(2) -0.0013(18) C40 0.041(3) 0.022(2) 0.039(3) -0.007(2) 0.004(2) 0.007(2) C41 0.034(3) 0.030(3) 0.028(3) -0.0031(18) 0.010(2) 0.0065(19) C42 0.025(3) 0.038(3) 0.033(3) 0.003(2) 0.011(2) 0.001(2) C43 0.020(2) 0.033(3) 0.039(3) 0.001(2) 0.008(2) -0.0036(19) C44 0.027(3) 0.034(3) 0.037(3) 0.004(2) -0.002(2) -0.006(2) C45 0.029(3) 0.031(3) 0.036(3) 0.004(2) -0.007(2) -0.005(2) C46 0.038(3) 0.032(3) 0.022(2) 0.0030(19) 0.002(2) 0.004(2) C47 0.029(3) 0.029(2) 0.024(2) 0.0136(19) 0.0052(19) 0.0049(19) C48 0.036(3) 0.022(2) 0.034(3) 0.0088(19) 0.003(2) 0.0029(19) C49 0.031(3) 0.014(2) 0.041(3) 0.0004(19) 0.010(2) -0.0003(17) C50 0.022(2) 0.028(2) 0.042(3) -0.006(2) 0.002(2) 0.0077(19) C51 0.023(2) 0.032(3) 0.038(3) -0.009(2) 0.003(2) 0.0039(19) C52 0.023(3) 0.033(2) 0.035(3) 0.007(2) -0.004(2) -0.001(2) C53 0.027(3) 0.031(2) 0.032(3) 0.005(2) -0.006(2) -0.001(2) C54 0.037(3) 0.026(2) 0.025(2) 0.0041(19) 0.002(2) 0.001(2) C55 0.040(3) 0.022(2) 0.034(3) 0.002(2) 0.000(2) 0.011(2) C56 0.033(3) 0.025(2) 0.041(3) 0.003(2) 0.000(2) 0.009(2) C57 0.025(3) 0.038(3) 0.040(3) -0.001(2) -0.001(2) 0.000(2) C58 0.026(3) 0.035(3) 0.031(3) 0.004(2) -0.002(2) -0.004(2) C59 0.031(3) 0.027(2) 0.031(3) 0.003(2) -0.004(2) 0.002(2) C60 0.026(3) 0.031(2) 0.045(3) 0.005(2) 0.003(2) 0.009(2) C61 0.046(3) 0.034(3) 0.025(2) 0.001(2) -0.004(2) 0.002(2) C62 0.036(3) 0.029(2) 0.027(3) 0.0035(19) 0.002(2) 0.001(2) C63 0.039(3) 0.022(2) 0.042(3) -0.005(2) 0.005(2) -0.002(2) C64 0.032(3) 0.029(3) 0.033(3) -0.002(2) 0.004(2) 0.009(2) C65 0.027(3) 0.029(2) 0.044(3) 0.000(2) -0.003(2) -0.002(2) C66 0.028(3) 0.033(3) 0.031(3) 0.003(2) 0.001(2) 0.006(2) C67 0.026(3) 0.032(2) 0.032(3) 0.000(2) -0.003(2) 0.0039(19) C68 0.041(3) 0.026(2) 0.037(3) -0.006(2) -0.002(2) 0.006(2) C69 0.033(3) 0.046(3) 0.034(3) 0.002(2) 0.006(2) 0.017(2) C70 0.023(3) 0.034(3) 0.035(3) 0.0027(19) 0.003(2) 0.0031(18) C71 0.043(3) 0.034(3) 0.031(3) 0.001(2) -0.001(2) 0.016(2) C72 0.054(4) 0.040(3) 0.049(4) -0.012(3) -0.015(3) 0.001(3) C101 0.043(5) 0.029(4) 0.057(5) 0.001(4) -0.010(4) -0.001(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ru C67 2.180(5) . ? Ru C68 2.181(5) . ? Ru C3 2.188(5) . ? Ru C66 2.195(5) . ? Ru C4 2.196(5) . ? Ru C70 2.197(5) . ? Ru C69 2.199(5) . ? Ru C5 2.206(5) . ? Ru C2 2.209(5) . ? Ru C1 2.219(4) . ? O C71 1.202(7) . ? S C101 1.5468(18) . ? C1 C2 1.412(6) . ? C1 C5 1.431(7) . ? C1 C6 1.516(6) . ? C2 C3 1.438(7) . ? C2 C7 1.498(7) . ? C3 C4 1.431(6) . ? C3 C8 1.508(6) . ? C4 C5 1.427(7) . ? C4 C9 1.513(6) . ? C5 C10 1.526(6) . ? C6 C61 1.542(7) . ? C6 C11 1.542(7) . ? C6 C20 1.547(6) . ? C7 C12 1.532(7) . ? C7 C62 1.547(7) . ? C7 C13 1.563(7) . ? C8 C63 1.542(6) . ? C8 C14 1.548(7) . ? C8 C15 1.553(6) . ? C9 C64 1.532(6) . ? C9 C17 1.540(6) . ? C9 C16 1.564(7) . ? C10 C65 1.537(7) . ? C10 C19 1.548(6) . ? C10 C18 1.553(7) . ? C11 C12 1.392(7) . ? C11 C21 1.448(7) . ? C12 C22 1.438(7) . ? C13 C14 1.373(7) . ? C13 C23 1.441(7) . ? C14 C24 1.437(7) . ? C15 C16 1.367(7) . ? C15 C25 1.452(7) . ? C16 C26 1.441(7) . ? C17 C18 1.370(7) . ? C17 C27 1.417(7) . ? C18 C28 1.451(6) . ? C19 C20 1.365(7) . ? C19 C29 1.449(7) . ? C20 C30 1.441(7) . ? C21 C31 1.395(7) . ? C21 C30 1.449(7) . ? C22 C32 1.400(7) . ? C22 C23 1.464(7) . ? C23 C33 1.377(7) . ? C24 C34 1.381(7) . ? C24 C25 1.438(7) . ? C25 C35 1.409(7) . ? C26 C36 1.382(7) . ? C26 C27 1.469(7) . ? C27 C37 1.402(7) . ? C28 C38 1.391(7) . ? C28 C29 1.457(6) . ? C29 C39 1.402(7) . ? C30 C40 1.387(7) . ? C31 C41 1.426(7) . ? C31 C32 1.470(7) . ? C32 C42 1.444(7) . ? C33 C43 1.459(7) . ? C33 C34 1.462(8) . ? C34 C44 1.450(7) . ? C35 C36 1.429(7) . ? C35 C45 1.452(7) . ? C36 C46 1.468(7) . ? C37 C38 1.428(7) . ? C37 C47 1.463(7) . ? C38 C48 1.451(7) . ? C39 C40 1.436(7) . ? C39 C49 1.464(7) . ? C40 C50 1.456(7) . ? C41 C50 1.397(7) . ? C41 C51 1.459(7) . ? C42 C43 1.392(7) . ? C42 C51 1.450(7) . ? C43 C52 1.467(7) . ? C44 C45 1.395(7) . ? C44 C52 1.469(8) . ? C45 C53 1.441(7) . ? C46 C47 1.376(7) . ? C46 C53 1.459(7) . ? C47 C54 1.438(7) . ? C48 C49 1.388(7) . ? C48 C54 1.454(7) . ? C49 C55 1.447(7) . ? C50 C55 1.452(7) . ? C51 C56 1.378(7) . ? C52 C57 1.400(7) . ? C53 C58 1.407(8) . ? C54 C59 1.403(7) . ? C55 C60 1.397(8) . ? C56 C60 1.435(7) . ? C56 C57 1.463(7) . ? C57 C58 1.446(7) . ? C58 C59 1.453(7) . ? C59 C60 1.457(7) . ? C66 C67 1.440(7) . ? C66 C70 1.445(7) . ? C66 C71 1.475(7) . ? C67 C68 1.420(7) . ? C68 C69 1.433(8) . ? C69 C70 1.438(8) . ? C71 C72 1.511(8) . ? C101 S 1.5468(19) 3_765 ? 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 C67 Ru C68 38.00(18) . . ? C67 Ru C3 122.69(18) . . ? C68 Ru C3 108.43(18) . . ? C67 Ru C66 38.44(18) . . ? C68 Ru C66 63.79(19) . . ? C3 Ru C66 158.17(19) . . ? C67 Ru C4 155.35(17) . . ? C68 Ru C4 122.38(18) . . ? C3 Ru C4 38.10(17) . . ? C66 Ru C4 163.59(19) . . ? C67 Ru C70 64.60(18) . . ? C68 Ru C70 64.31(19) . . ? C3 Ru C70 159.4(2) . . ? C66 Ru C70 38.42(19) . . ? C4 Ru C70 127.46(19) . . ? C67 Ru C69 63.8(2) . . ? C68 Ru C69 38.2(2) . . ? C3 Ru C69 124.15(19) . . ? C66 Ru C69 63.59(19) . . ? C4 Ru C69 110.74(19) . . ? C70 Ru C69 38.2(2) . . ? C67 Ru C5 164.71(19) . . ? C68 Ru C5 157.1(2) . . ? C3 Ru C5 63.50(17) . . ? C66 Ru C5 131.45(19) . . ? C4 Ru C5 37.84(18) . . ? C70 Ru C5 115.06(18) . . ? C69 Ru C5 126.4(2) . . ? C67 Ru C2 112.47(18) . . ? C68 Ru C2 125.61(19) . . ? C3 Ru C2 38.18(17) . . ? C66 Ru C2 127.82(18) . . ? C4 Ru C2 63.15(17) . . ? C70 Ru C2 161.8(2) . . ? C69 Ru C2 158.9(2) . . ? C5 Ru C2 62.59(17) . . ? C67 Ru C1 129.41(18) . . ? C68 Ru C1 160.64(19) . . ? C3 Ru C1 63.54(17) . . ? C66 Ru C1 116.55(18) . . ? C4 Ru C1 63.33(17) . . ? C70 Ru C1 129.31(18) . . ? C69 Ru C1 161.05(19) . . ? C5 Ru C1 37.74(17) . . ? C2 Ru C1 37.18(16) . . ? C2 C1 C5 107.6(4) . . ? C2 C1 C6 124.0(4) . . ? C5 C1 C6 124.4(4) . . ? C2 C1 Ru 71.0(3) . . ? C5 C1 Ru 70.7(3) . . ? C6 C1 Ru 141.7(3) . . ? C1 C2 C3 109.0(4) . . ? C1 C2 C7 124.8(4) . . ? C3 C2 C7 123.3(4) . . ? C1 C2 Ru 71.8(3) . . ? C3 C2 Ru 70.1(3) . . ? C7 C2 Ru 139.6(3) . . ? C4 C3 C2 107.0(4) . . ? C4 C3 C8 124.3(4) . . ? C2 C3 C8 124.9(4) . . ? C4 C3 Ru 71.2(3) . . ? C2 C3 Ru 71.7(3) . . ? C8 C3 Ru 139.6(3) . . ? C5 C4 C3 108.0(4) . . ? C5 C4 C9 124.0(4) . . ? C3 C4 C9 124.9(4) . . ? C5 C4 Ru 71.5(3) . . ? C3 C4 Ru 70.7(3) . . ? C9 C4 Ru 139.4(3) . . ? C4 C5 C1 108.4(4) . . ? C4 C5 C10 124.0(4) . . ? C1 C5 C10 123.7(4) . . ? C4 C5 Ru 70.7(3) . . ? C1 C5 Ru 71.6(3) . . ? C10 C5 Ru 141.4(3) . . ? C1 C6 C61 115.6(4) . . ? C1 C6 C11 106.0(4) . . ? C61 C6 C11 114.0(4) . . ? C1 C6 C20 105.8(4) . . ? C61 C6 C20 113.6(4) . . ? C11 C6 C20 100.4(4) . . ? C2 C7 C12 106.7(4) . . ? C2 C7 C62 114.6(4) . . ? C12 C7 C62 113.8(4) . . ? C2 C7 C13 106.7(4) . . ? C12 C7 C13 100.5(4) . . ? C62 C7 C13 113.2(4) . . ? C3 C8 C63 116.4(4) . . ? C3 C8 C14 105.3(4) . . ? C63 C8 C14 113.5(4) . . ? C3 C8 C15 105.5(4) . . ? C63 C8 C15 114.4(4) . . ? C14 C8 C15 100.1(4) . . ? C4 C9 C64 115.8(4) . . ? C4 C9 C17 106.4(4) . . ? C64 C9 C17 114.9(4) . . ? C4 C9 C16 105.3(4) . . ? C64 C9 C16 112.7(4) . . ? C17 C9 C16 100.2(4) . . ? C5 C10 C65 115.6(4) . . ? C5 C10 C19 105.9(4) . . ? C65 C10 C19 113.8(4) . . ? C5 C10 C18 105.6(4) . . ? C65 C10 C18 112.8(4) . . ? C19 C10 C18 101.8(4) . . ? C12 C11 C21 120.1(5) . . ? C12 C11 C6 124.3(4) . . ? C21 C11 C6 109.7(4) . . ? C11 C12 C22 118.5(4) . . ? C11 C12 C7 123.8(5) . . ? C22 C12 C7 110.5(4) . . ? C14 C13 C23 119.5(5) . . ? C14 C13 C7 123.5(4) . . ? C23 C13 C7 109.5(4) . . ? C13 C14 C24 119.8(4) . . ? C13 C14 C8 125.0(4) . . ? C24 C14 C8 110.3(4) . . ? C16 C15 C25 120.3(4) . . ? C16 C15 C8 125.2(4) . . ? C25 C15 C8 108.2(4) . . ? C15 C16 C26 118.9(4) . . ? C15 C16 C9 124.3(4) . . ? C26 C16 C9 109.7(4) . . ? C18 C17 C27 119.4(4) . . ? C18 C17 C9 123.8(4) . . ? C27 C17 C9 110.2(4) . . ? C17 C18 C28 119.2(4) . . ? C17 C18 C10 125.3(4) . . ? C28 C18 C10 108.6(4) . . ? C20 C19 C29 119.4(4) . . ? C20 C19 C10 125.0(4) . . ? C29 C19 C10 108.5(4) . . ? C19 C20 C30 119.6(4) . . ? C19 C20 C6 124.8(4) . . ? C30 C20 C6 109.5(4) . . ? C31 C21 C11 121.9(5) . . ? C31 C21 C30 119.3(5) . . ? C11 C21 C30 108.2(4) . . ? C32 C22 C12 122.5(5) . . ? C32 C22 C23 118.8(5) . . ? C12 C22 C23 108.6(4) . . ? C33 C23 C13 121.4(5) . . ? C33 C23 C22 120.1(5) . . ? C13 C23 C22 108.5(4) . . ? C34 C24 C14 121.2(5) . . ? C34 C24 C25 120.3(5) . . ? C14 C24 C25 107.8(4) . . ? C35 C25 C24 120.3(5) . . ? C35 C25 C15 119.7(5) . . ? C24 C25 C15 110.1(4) . . ? C36 C26 C16 122.2(4) . . ? C36 C26 C27 120.3(4) . . ? C16 C26 C27 107.6(4) . . ? C37 C27 C17 121.8(5) . . ? C37 C27 C26 119.3(5) . . ? C17 C27 C26 109.7(4) . . ? C38 C28 C18 121.6(4) . . ? C38 C28 C29 120.1(4) . . ? C18 C28 C29 108.9(4) . . ? C39 C29 C19 121.1(4) . . ? C39 C29 C28 119.5(5) . . ? C19 C29 C28 109.3(4) . . ? C40 C30 C20 121.4(5) . . ? C40 C30 C21 120.1(5) . . ? C20 C30 C21 109.1(4) . . ? C21 C31 C41 121.1(5) . . ? C21 C31 C32 118.2(5) . . ? C41 C31 C32 108.2(5) . . ? C22 C32 C42 121.0(5) . . ? C22 C32 C31 118.8(5) . . ? C42 C32 C31 107.2(4) . . ? C23 C33 C43 120.6(5) . . ? C23 C33 C34 118.9(5) . . ? C43 C33 C34 107.7(4) . . ? C24 C34 C44 120.3(5) . . ? C24 C34 C33 119.0(5) . . ? C44 C34 C33 108.7(4) . . ? C25 C35 C36 119.7(5) . . ? C25 C35 C45 119.0(5) . . ? C36 C35 C45 108.8(4) . . ? C26 C36 C35 119.0(4) . . ? C26 C36 C46 119.8(4) . . ? C35 C36 C46 107.9(5) . . ? C27 C37 C38 119.4(5) . . ? C27 C37 C47 120.1(4) . . ? C38 C37 C47 107.7(4) . . ? C28 C38 C37 118.3(4) . . ? C28 C38 C48 120.3(4) . . ? C37 C38 C48 108.7(4) . . ? C29 C39 C40 118.6(4) . . ? C29 C39 C49 120.0(4) . . ? C40 C39 C49 109.0(4) . . ? C30 C40 C39 119.5(5) . . ? C30 C40 C50 119.9(5) . . ? C39 C40 C50 107.4(4) . . ? C50 C41 C31 119.8(5) . . ? C50 C41 C51 119.0(4) . . ? C31 C41 C51 108.6(5) . . ? C43 C42 C32 119.6(5) . . ? C43 C42 C51 120.1(5) . . ? C32 C42 C51 108.6(5) . . ? C42 C43 C33 119.8(5) . . ? C42 C43 C52 119.4(5) . . ? C33 C43 C52 108.1(4) . . ? C45 C44 C34 119.6(5) . . ? C45 C44 C52 119.4(5) . . ? C34 C44 C52 107.9(5) . . ? C44 C45 C53 120.0(5) . . ? C44 C45 C35 120.4(4) . . ? C53 C45 C35 107.9(5) . . ? C47 C46 C53 121.1(4) . . ? C47 C46 C36 120.6(5) . . ? C53 C46 C36 107.1(4) . . ? C46 C47 C54 119.7(4) . . ? C46 C47 C37 119.8(4) . . ? C54 C47 C37 108.1(4) . . ? C49 C48 C38 120.2(5) . . ? C49 C48 C54 119.9(5) . . ? C38 C48 C54 107.7(4) . . ? C48 C49 C55 120.9(5) . . ? C48 C49 C39 119.8(4) . . ? C55 C49 C39 107.2(4) . . ? C41 C50 C55 120.1(5) . . ? C41 C50 C40 119.7(5) . . ? C55 C50 C40 108.3(4) . . ? C56 C51 C42 120.6(4) . . ? C56 C51 C41 120.6(5) . . ? C42 C51 C41 107.3(5) . . ? C57 C52 C43 120.3(5) . . ? C57 C52 C44 120.5(5) . . ? C43 C52 C44 107.6(4) . . ? C58 C53 C45 120.5(5) . . ? C58 C53 C46 118.9(5) . . ? C45 C53 C46 108.2(4) . . ? C59 C54 C47 121.0(5) . . ? C59 C54 C48 119.5(5) . . ? C47 C54 C48 107.9(5) . . ? C60 C55 C49 119.8(5) . . ? C60 C55 C50 119.8(5) . . ? C49 C55 C50 108.2(4) . . ? C51 C56 C60 120.3(5) . . ? C51 C56 C57 120.4(5) . . ? C60 C56 C57 108.0(5) . . ? C52 C57 C58 119.3(5) . . ? C52 C57 C56 119.1(5) . . ? C58 C57 C56 107.7(5) . . ? C53 C58 C57 120.2(5) . . ? C53 C58 C59 120.1(5) . . ? C57 C58 C59 108.2(4) . . ? C54 C59 C58 119.1(5) . . ? C54 C59 C60 120.4(5) . . ? C58 C59 C60 107.6(4) . . ? C55 C60 C56 120.1(5) . . ? C55 C60 C59 119.5(5) . . ? C56 C60 C59 108.4(4) . . ? C67 C66 C70 108.3(5) . . ? C67 C66 C71 124.6(5) . . ? C70 C66 C71 127.0(5) . . ? C67 C66 Ru 70.2(3) . . ? C70 C66 Ru 70.9(3) . . ? C71 C66 Ru 128.0(4) . . ? C68 C67 C66 107.9(5) . . ? C68 C67 Ru 71.0(3) . . ? C66 C67 Ru 71.4(3) . . ? C67 C68 C69 108.5(4) . . ? C67 C68 Ru 71.0(3) . . ? C69 C68 Ru 71.6(3) . . ? C68 C69 C70 108.5(5) . . ? C68 C69 Ru 70.2(3) . . ? C70 C69 Ru 70.8(3) . . ? C69 C70 C66 106.9(5) . . ? C69 C70 Ru 71.0(3) . . ? C66 C70 Ru 70.7(3) . . ? O C71 C66 121.2(6) . . ? O C71 C72 122.3(6) . . ? C66 C71 C72 116.4(5) . . ? S C101 S 180.00(12) 3_765 . ? #===END _database_code_depnum_ccdc_archive 'CCDC 950176'