# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1609 data_global # Chelating versus bridging behaviour and NMR fluxionality of dppf # in the nido clusters (M3Se2(CO)7(dppf) (M=Fe or Ru, dppf=Fe(eta5- # C5H4PPh2)2. Crystal structure of the chelated ruthenium derivative. # # by Daniele Cauzzi, Claudia Graiff, Chiara Massera, # Giovanni Predieri, Antonio Tiripicchio, # Domenico Acquotti # # Submitted to Dalton Transactions # #--------------------------------- # Person for contact _publ_contact_author ; Prof. Giovanni Predieri Dipartimento di Chimica Generale ed Inorganica , Chimica Analitica , Chimica Fisica , University of Parma, Centro di studio per la Strutturistica diffrattometrica del CNR Viale delle Scienze, I-43100 Parma, Italy ; _publ_contact_author_email PREDIERI@IPRUNIV.CCE.UNIPR.IT #-------------------------------------- # Publication details loop_ _publ_author_name 'Cauzzi, D.' 'Graiff, C.' 'Massera, C.' 'Predieri, G.' 'Tiripicchio, A.' 'Acquotti, D.' _journal_name_full 'Journal of the Chemical Society, Dalton Transactions' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '1999' #-------------------------------------- #Data for compound (2) data_g13f _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C41H28O7P2FeRu3Se2 .CH2Cl2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H30 Cl2 Fe O7 P2 Ru3 Se2' _chemical_formula_weight 1296.52 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 '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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.201(2) _cell_length_b 12.020(3) _cell_length_c 21.405(5) _cell_angle_alpha 79.77(2) _cell_angle_beta 84.24(3) _cell_angle_gamma 72.31(2) _cell_volume 2216.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11.06 _cell_measurement_theta_max 14.84 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method ? _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 3.206 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8196 _exptl_absorpt_correction_T_max 1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Philips PW 1100' _diffrn_measurement_method '\q/2\q scans' _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10683 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1656 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10683 _reflns_number_observed 4549 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+( 0.0944P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10679 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_obs 0.0425 _refine_ls_wR_factor_all 0.1449 _refine_ls_wR_factor_obs 0.1012 _refine_ls_goodness_of_fit_all 0.561 _refine_ls_goodness_of_fit_obs 0.680 _refine_ls_restrained_S_all 0.619 _refine_ls_restrained_S_obs 0.680 _refine_ls_shift/esd_max 0.174 _refine_ls_shift/esd_mean 0.006 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.26961(6) 0.05725(5) 0.76576(2) 0.02912(13) Uani 1 d . . Ru2 Ru 0.05896(7) 0.29397(5) 0.76150(3) 0.0386(2) Uani 1 d . . Ru3 Ru 0.24836(7) 0.33012(5) 0.84308(3) 0.0440(2) Uani 1 d . . Se1 Se 0.34758(8) 0.24299(6) 0.74356(3) 0.0362(2) Uani 1 d . . Se2 Se 0.14959(8) 0.15235(6) 0.86133(3) 0.0391(2) Uani 1 d . . Fe1 Fe 0.70107(10) -0.15182(9) 0.68932(5) 0.0359(2) Uani 1 d . . P1 P 0.4565(2) -0.0923(2) 0.82023(8) 0.0321(4) Uani 1 d . . P2 P 0.3451(2) 0.0254(2) 0.65975(8) 0.0310(4) Uani 1 d . . O1 O 0.0505(6) -0.0882(5) 0.7829(3) 0.062(2) Uani 1 d . . O2 O 0.0213(11) 0.4377(8) 0.9431(4) 0.134(4) Uani 1 d . . O3 O 0.2726(9) 0.5726(6) 0.7825(3) 0.092(2) Uani 1 d . . O4 O 0.5136(9) 0.2745(6) 0.9285(4) 0.099(2) Uani 1 d . . O5 O 0.0530(7) 0.4856(5) 0.6470(3) 0.070(2) Uani 1 d . . O6 O -0.1385(7) 0.1690(6) 0.7115(3) 0.078(2) Uani 1 d . . O7 O -0.2116(8) 0.4316(6) 0.8369(3) 0.101(3) Uani 1 d . . C1 C 0.1405(8) -0.0387(6) 0.7770(3) 0.042(2) Uani 1 d . . C2 C 0.1062(13) 0.3968(9) 0.9061(5) 0.083(3) Uani 1 d . . C3 C 0.2678(10) 0.4809(8) 0.8052(4) 0.058(2) Uani 1 d . . C4 C 0.4191(11) 0.2890(7) 0.8952(4) 0.059(2) Uani 1 d . . C5 C 0.0510(8) 0.4139(7) 0.6893(4) 0.049(2) Uani 1 d . . C6 C -0.0548(10) 0.2085(7) 0.7284(4) 0.054(2) Uani 1 d . . C7 C -0.1091(10) 0.3837(7) 0.8083(4) 0.060(2) Uani 1 d . . C8 C 0.6123(7) -0.1895(6) 0.7782(3) 0.035(2) Uani 1 d . . C9 C 0.7724(8) -0.2059(6) 0.7810(3) 0.044(2) Uani 1 d . . H9 H 0.8158(8) -0.1665(6) 0.8041(3) 0.044(10) Uiso 1 calc R . C10 C 0.8542(8) -0.2918(7) 0.7426(4) 0.051(2) Uani 1 d . . H10 H 0.9598(8) -0.3176(7) 0.7361(4) 0.044(10) Uiso 1 calc R . C11 C 0.7473(8) -0.3319(6) 0.7160(4) 0.049(2) Uani 1 d . . H11 H 0.7700(8) -0.3880(6) 0.6888(4) 0.044(10) Uiso 1 calc R . C12 C 0.5974(8) -0.2695(6) 0.7390(3) 0.042(2) Uani 1 d . . H12 H 0.5059(8) -0.2795(6) 0.7297(3) 0.044(10) Uiso 1 calc R . C13 C 0.5477(7) -0.0180(6) 0.6390(3) 0.0309(15) Uani 1 d . . C14 C 0.6593(7) 0.0249(6) 0.6621(3) 0.039(2) Uani 1 d . . H14 H 0.6403(7) 0.0808(6) 0.6892(3) 0.059(12) Uiso 1 calc R . C15 C 0.8034(8) -0.0344(7) 0.6355(3) 0.047(2) Uani 1 d . . H15 H 0.8950(8) -0.0215(7) 0.6420(3) 0.059(12) Uiso 1 calc R . C16 C 0.7896(8) -0.1138(7) 0.5988(3) 0.050(2) Uani 1 d . . H16 H 0.8689(8) -0.1654(7) 0.5784(3) 0.059(12) Uiso 1 calc R . C17 C 0.6279(7) -0.1017(6) 0.5980(3) 0.040(2) Uani 1 d . . H17 H 0.5841(7) -0.1411(6) 0.5750(3) 0.059(12) Uiso 1 calc R . C18 C 0.3884(8) -0.2027(6) 0.8757(3) 0.040(2) Uani 1 d . . C19 C 0.4734(10) -0.3215(7) 0.8857(4) 0.053(2) Uani 1 d . . H19 H 0.5662(10) -0.3464(7) 0.8631(4) 0.073(12) Uiso 1 calc R . C20 C 0.4218(11) -0.4012(7) 0.9281(4) 0.062(2) Uani 1 d . . H20 H 0.4812(11) -0.4798(7) 0.9345(4) 0.073(12) Uiso 1 calc R . C21 C 0.2869(11) -0.3693(8) 0.9611(4) 0.070(3) Uani 1 d . . H21 H 0.2528(11) -0.4257(8) 0.9891(4) 0.073(12) Uiso 1 calc R . C22 C 0.1998(11) -0.2523(8) 0.9529(5) 0.081(3) Uani 1 d . . H22 H 0.1077(11) -0.2288(8) 0.9762(5) 0.073(12) Uiso 1 calc R . C23 C 0.2505(9) -0.1708(7) 0.9101(4) 0.058(2) Uani 1 d . . H23 H 0.1907(9) -0.0923(7) 0.9041(4) 0.073(12) Uiso 1 calc R . C24 C 0.2839(7) -0.0815(6) 0.6246(3) 0.036(2) Uani 1 d . . C25 C 0.2538(8) -0.1778(6) 0.6619(4) 0.041(2) Uani 1 d . . H25 H 0.2589(8) -0.1865(6) 0.7058(4) 0.050(10) Uiso 1 calc R . C26 C 0.2159(8) -0.2629(7) 0.6361(4) 0.047(2) Uani 1 d . . H26 H 0.1974(8) -0.3284(7) 0.6620(4) 0.050(10) Uiso 1 calc R . C27 C 0.2066(10) -0.2479(8) 0.5713(4) 0.062(2) Uani 1 d . . H27 H 0.1813(10) -0.3038(8) 0.5530(4) 0.050(10) Uiso 1 calc R . C28 C 0.2341(10) -0.1517(8) 0.5335(4) 0.060(2) Uani 1 d . . H28 H 0.2274(10) -0.1426(8) 0.4897(4) 0.050(10) Uiso 1 calc R . C29 C 0.2718(8) -0.0675(6) 0.5596(3) 0.043(2) Uani 1 d . . H29 H 0.2890(8) -0.0017(6) 0.5335(3) 0.050(10) Uiso 1 calc R . C30 C 0.2788(8) 0.1575(6) 0.6005(3) 0.038(2) Uani 1 d . . C31 C 0.1240(8) 0.1998(7) 0.5864(4) 0.050(2) Uani 1 d . . H31 H 0.0554(8) 0.1617(7) 0.6079(4) 0.093(15) Uiso 1 calc R . C32 C 0.0719(11) 0.2993(8) 0.5398(4) 0.066(3) Uani 1 d . . H32 H -0.0306(11) 0.3268(8) 0.5305(4) 0.093(15) Uiso 1 calc R . C33 C 0.1751(12) 0.3563(7) 0.5079(4) 0.070(3) Uani 1 d . . H33 H 0.1409(12) 0.4229(7) 0.4776(4) 0.093(15) Uiso 1 calc R . C34 C 0.3218(12) 0.3162(8) 0.5206(4) 0.078(3) Uani 1 d . . H34 H 0.3893(12) 0.3545(8) 0.4981(4) 0.093(15) Uiso 1 calc R . C35 C 0.3779(9) 0.2178(6) 0.5669(4) 0.050(2) Uani 1 d . . H35 H 0.4811(9) 0.1925(6) 0.5753(4) 0.093(15) Uiso 1 calc R . C36 C 0.5700(8) -0.0437(6) 0.8699(3) 0.039(2) Uani 1 d . . C37 C 0.6440(9) 0.0379(7) 0.8440(4) 0.054(2) Uani 1 d . . H37 H 0.6225(9) 0.0786(7) 0.8033(4) 0.071(12) Uiso 1 calc R . C38 C 0.7497(9) 0.0611(7) 0.8772(4) 0.059(2) Uani 1 d . . H38 H 0.8013(9) 0.1148(7) 0.8578(4) 0.071(12) Uiso 1 calc R . C39 C 0.7797(11) 0.0065(8) 0.9379(4) 0.069(3) Uani 1 d . . H39 H 0.8534(11) 0.0201(8) 0.9599(4) 0.071(12) Uiso 1 calc R . C40 C 0.6975(12) -0.0694(10) 0.9657(4) 0.088(3) Uani 1 d . . H40 H 0.7097(12) -0.1027(10) 1.0082(4) 0.071(12) Uiso 1 calc R . C41 C 0.5969(11) -0.0967(8) 0.9313(4) 0.070(3) Uani 1 d . . H41 H 0.5470(11) -0.1518(8) 0.9502(4) 0.071(12) Uiso 1 calc R . C1S C 0.5134(18) 0.4370(17) 0.6229(7) 0.170(7) Uani 1 d . . Cl1 Cl 0.6574(6) 0.3846(5) 0.5706(3) 0.204(2) Uani 1 d . . Cl2 Cl 0.5812(6) 0.4642(6) 0.6859(4) 0.255(3) Uani 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 0.0269(3) 0.0304(3) 0.0305(3) -0.0033(2) -0.0026(2) -0.0094(2) Ru2 0.0380(3) 0.0344(3) 0.0410(3) -0.0069(3) -0.0021(3) -0.0064(3) Ru3 0.0566(4) 0.0423(4) 0.0394(4) -0.0109(3) -0.0003(3) -0.0219(3) Se1 0.0396(4) 0.0362(4) 0.0358(4) -0.0047(3) 0.0001(3) -0.0165(3) Se2 0.0458(4) 0.0399(4) 0.0337(4) -0.0063(3) 0.0032(3) -0.0169(3) Fe1 0.0267(5) 0.0391(6) 0.0379(6) -0.0029(4) -0.0018(4) -0.0054(4) P1 0.0303(9) 0.0335(9) 0.0318(10) 0.0012(7) -0.0023(7) -0.0115(8) P2 0.0253(9) 0.0386(10) 0.0296(9) -0.0030(8) -0.0033(7) -0.0109(8) O1 0.044(3) 0.073(4) 0.084(4) -0.019(3) 0.009(3) -0.037(3) O2 0.155(8) 0.162(8) 0.116(7) -0.100(7) 0.055(6) -0.067(7) O3 0.133(6) 0.060(4) 0.091(5) 0.008(4) -0.025(5) -0.044(4) O4 0.122(6) 0.081(5) 0.102(6) -0.022(4) -0.053(5) -0.021(4) O5 0.085(5) 0.059(4) 0.054(4) 0.010(3) -0.008(3) -0.010(3) O6 0.057(4) 0.085(5) 0.108(5) -0.020(4) -0.025(4) -0.035(4) O7 0.087(5) 0.086(5) 0.099(6) -0.026(4) 0.042(4) 0.010(4) C1 0.031(4) 0.050(5) 0.046(5) -0.010(4) 0.003(3) -0.011(3) C2 0.108(9) 0.070(7) 0.085(8) -0.044(6) 0.038(7) -0.042(6) C3 0.073(6) 0.058(6) 0.046(5) -0.010(4) -0.008(4) -0.023(5) C4 0.081(6) 0.053(5) 0.052(5) -0.013(4) -0.020(5) -0.024(5) C5 0.044(5) 0.040(4) 0.055(5) -0.004(4) -0.010(4) 0.000(4) C6 0.064(6) 0.044(5) 0.050(5) -0.001(4) -0.010(4) -0.012(4) C7 0.055(5) 0.052(5) 0.064(6) -0.012(4) 0.006(5) -0.003(4) C8 0.033(4) 0.032(4) 0.040(4) 0.002(3) -0.008(3) -0.011(3) C9 0.037(4) 0.050(5) 0.039(4) 0.005(4) -0.004(3) -0.012(4) C10 0.032(4) 0.054(5) 0.053(5) 0.006(4) 0.001(4) 0.001(4) C11 0.040(4) 0.034(4) 0.062(5) -0.006(4) -0.005(4) 0.004(3) C12 0.041(4) 0.034(4) 0.045(4) 0.003(3) -0.001(3) -0.009(3) C13 0.025(3) 0.037(4) 0.030(4) -0.001(3) -0.003(3) -0.009(3) C14 0.034(4) 0.036(4) 0.048(4) -0.003(3) 0.000(3) -0.015(3) C15 0.034(4) 0.058(5) 0.046(5) 0.007(4) -0.002(3) -0.020(4) C16 0.037(4) 0.060(5) 0.041(4) -0.001(4) 0.007(3) -0.004(4) C17 0.030(4) 0.055(5) 0.033(4) -0.005(3) -0.009(3) -0.007(3) C18 0.035(4) 0.040(4) 0.041(4) 0.005(3) -0.008(3) -0.012(3) C19 0.066(5) 0.044(5) 0.045(5) 0.002(4) 0.008(4) -0.018(4) C20 0.088(7) 0.041(5) 0.052(5) 0.007(4) -0.003(5) -0.018(5) C21 0.071(6) 0.066(6) 0.075(7) 0.023(5) -0.004(5) -0.040(5) C22 0.074(7) 0.068(7) 0.091(8) 0.010(6) 0.034(6) -0.030(5) C23 0.058(5) 0.046(5) 0.061(6) 0.005(4) 0.013(4) -0.015(4) C24 0.034(4) 0.041(4) 0.036(4) -0.006(3) -0.004(3) -0.014(3) C25 0.040(4) 0.040(4) 0.042(4) -0.007(3) 0.005(3) -0.013(3) C26 0.045(4) 0.041(4) 0.058(5) -0.006(4) 0.001(4) -0.019(4) C27 0.065(6) 0.066(6) 0.068(6) -0.028(5) -0.008(5) -0.023(5) C28 0.079(6) 0.064(6) 0.044(5) -0.018(4) -0.010(4) -0.022(5) C29 0.041(4) 0.046(4) 0.042(4) 0.001(4) -0.006(3) -0.014(4) C30 0.049(4) 0.035(4) 0.029(4) -0.005(3) -0.005(3) -0.010(3) C31 0.042(4) 0.054(5) 0.050(5) -0.011(4) -0.013(4) -0.003(4) C32 0.069(6) 0.059(6) 0.056(6) -0.006(5) -0.027(5) 0.009(5) C33 0.085(7) 0.041(5) 0.065(6) 0.008(4) -0.028(6) 0.006(5) C34 0.094(8) 0.062(6) 0.061(6) 0.016(5) 0.010(6) -0.014(6) C35 0.047(5) 0.040(4) 0.055(5) 0.008(4) -0.013(4) -0.008(4) C36 0.036(4) 0.049(4) 0.036(4) -0.009(3) -0.006(3) -0.015(3) C37 0.062(5) 0.071(6) 0.041(5) -0.012(4) -0.007(4) -0.035(5) C38 0.055(5) 0.067(6) 0.064(6) -0.002(5) -0.015(4) -0.032(5) C39 0.073(6) 0.084(7) 0.063(6) -0.021(5) -0.027(5) -0.028(6) C40 0.112(9) 0.127(9) 0.039(5) 0.004(6) -0.033(6) -0.054(8) C41 0.099(7) 0.082(7) 0.039(5) 0.004(5) -0.016(5) -0.044(6) C1S 0.173(15) 0.298(22) 0.111(11) -0.104(13) 0.050(10) -0.150(16) Cl1 0.179(5) 0.199(5) 0.237(6) -0.060(4) 0.101(4) -0.076(4) Cl2 0.168(5) 0.266(7) 0.403(10) -0.197(7) 0.040(6) -0.105(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.865(7) . ? Ru1 P1 2.308(2) . ? Ru1 P2 2.368(2) . ? Ru1 Se1 2.5006(10) . ? Ru1 Se2 2.5141(11) . ? Ru1 Ru2 2.9073(11) . ? Ru2 C7 1.901(8) . ? Ru2 C5 1.908(8) . ? Ru2 C6 1.927(9) . ? Ru2 Se2 2.5223(12) . ? Ru2 Se1 2.5426(11) . ? Ru2 Ru3 2.7597(11) . ? Ru3 C2 1.888(10) . ? Ru3 C3 1.902(9) . ? Ru3 C4 1.908(9) . ? Ru3 Se1 2.5078(11) . ? Ru3 Se2 2.5212(11) . ? Fe1 C13 2.012(6) . ? Fe1 C8 2.025(7) . ? Fe1 C12 2.030(7) . ? Fe1 C9 2.061(7) . ? Fe1 C14 2.027(7) . ? Fe1 C17 2.059(7) . ? Fe1 C16 2.054(7) . ? Fe1 C15 2.054(7) . ? Fe1 C11 2.060(7) . ? Fe1 C10 2.078(7) . ? P1 C8 1.823(7) . ? P1 C18 1.833(7) . ? P1 C36 1.837(7) . ? P2 C30 1.831(7) . ? P2 C24 1.845(7) . ? P2 C13 1.809(6) . ? O1 C1 1.143(8) . ? O2 C2 1.123(10) . ? O3 C3 1.135(9) . ? O4 C4 1.132(9) . ? O5 C5 1.136(9) . ? O6 C6 1.135(9) . ? O7 C7 1.130(9) . ? C8 C9 1.431(9) . ? C8 C12 1.428(9) . ? C9 C10 1.418(10) . ? C10 C11 1.423(10) . ? C11 C12 1.440(9) . ? C13 C14 1.441(9) . ? C13 C17 1.436(9) . ? C14 C15 1.416(9) . ? C15 C16 1.381(10) . ? C16 C17 1.452(9) . ? C18 C23 1.384(10) . ? C18 C19 1.393(10) . ? C19 C20 1.360(10) . ? C20 C21 1.348(11) . ? C21 C22 1.381(12) . ? C22 C23 1.375(10) . ? C24 C25 1.371(9) . ? C24 C29 1.383(9) . ? C25 C26 1.389(9) . ? C26 C27 1.375(10) . ? C27 C28 1.364(11) . ? C28 C29 1.382(10) . ? C30 C35 1.400(10) . ? C30 C31 1.404(9) . ? C31 C32 1.406(11) . ? C32 C33 1.391(12) . ? C33 C34 1.327(12) . ? C34 C35 1.401(11) . ? C36 C37 1.367(10) . ? C36 C41 1.367(10) . ? C37 C38 1.380(10) . ? C38 C39 1.361(11) . ? C39 C40 1.377(12) . ? C40 C41 1.384(12) . ? C1S Cl2 1.662(14) . ? C1S Cl1 1.688(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 P1 90.7(2) . . ? C1 Ru1 P2 93.9(2) . . ? P1 Ru1 P2 100.62(7) . . ? C1 Ru1 Se1 158.3(2) . . ? P1 Ru1 Se1 109.68(5) . . ? P2 Ru1 Se1 89.56(5) . . ? C1 Ru1 Se2 92.2(2) . . ? P1 Ru1 Se2 95.55(6) . . ? P2 Ru1 Se2 162.63(5) . . ? Se1 Ru1 Se2 78.97(3) . . ? C1 Ru1 Ru2 103.3(2) . . ? P1 Ru1 Ru2 147.09(5) . . ? P2 Ru1 Ru2 107.83(5) . . ? Se1 Ru1 Ru2 55.48(3) . . ? Se2 Ru1 Ru2 54.88(3) . . ? C7 Ru2 C5 96.1(3) . . ? C7 Ru2 C6 95.8(4) . . ? C5 Ru2 C6 97.4(3) . . ? C7 Ru2 Se2 90.7(3) . . ? C5 Ru2 Se2 160.8(2) . . ? C6 Ru2 Se2 99.7(2) . . ? C7 Ru2 Se1 142.8(3) . . ? C5 Ru2 Se1 85.8(2) . . ? C6 Ru2 Se1 120.9(2) . . ? Se2 Ru2 Se1 78.04(4) . . ? C7 Ru2 Ru3 87.8(3) . . ? C5 Ru2 Ru3 105.4(2) . . ? C6 Ru2 Ru3 156.3(2) . . ? Se2 Ru2 Ru3 56.81(3) . . ? Se1 Ru2 Ru3 56.27(3) . . ? C7 Ru2 Ru1 141.2(3) . . ? C5 Ru2 Ru1 122.4(2) . . ? C6 Ru2 Ru1 76.3(2) . . ? Se2 Ru2 Ru1 54.61(3) . . ? Se1 Ru2 Ru1 54.12(3) . . ? Ru3 Ru2 Ru1 86.21(3) . . ? C2 Ru3 C3 91.7(4) . . ? C2 Ru3 C4 94.1(4) . . ? C3 Ru3 C4 95.7(4) . . ? C2 Ru3 Se1 158.9(3) . . ? C3 Ru3 Se1 92.5(2) . . ? C4 Ru3 Se1 106.0(3) . . ? C2 Ru3 Se2 90.0(3) . . ? C3 Ru3 Se2 158.2(2) . . ? C4 Ru3 Se2 105.9(2) . . ? Se1 Ru3 Se2 78.70(3) . . ? C2 Ru3 Ru2 101.5(3) . . ? C3 Ru3 Ru2 101.6(2) . . ? C4 Ru3 Ru2 156.3(2) . . ? Se1 Ru3 Ru2 57.48(3) . . ? Se2 Ru3 Ru2 56.85(3) . . ? Ru1 Se1 Ru3 101.34(4) . . ? Ru1 Se1 Ru2 70.40(3) . . ? Ru3 Se1 Ru2 66.24(4) . . ? Ru1 Se2 Ru2 70.51(3) . . ? Ru1 Se2 Ru3 100.60(4) . . ? Ru2 Se2 Ru3 66.35(3) . . ? C13 Fe1 C8 109.8(3) . . ? C13 Fe1 C12 110.1(3) . . ? C8 Fe1 C12 41.2(3) . . ? C13 Fe1 C9 139.4(3) . . ? C8 Fe1 C9 41.0(3) . . ? C12 Fe1 C9 68.3(3) . . ? C13 Fe1 C14 41.8(2) . . ? C8 Fe1 C14 111.3(3) . . ? C12 Fe1 C14 139.8(3) . . ? C9 Fe1 C14 112.3(3) . . ? C13 Fe1 C17 41.3(2) . . ? C8 Fe1 C17 138.2(3) . . ? C12 Fe1 C17 110.3(3) . . ? C9 Fe1 C17 178.5(3) . . ? C14 Fe1 C17 69.1(3) . . ? C13 Fe1 C16 69.9(3) . . ? C8 Fe1 C16 179.5(3) . . ? C12 Fe1 C16 138.4(3) . . ? C9 Fe1 C16 139.4(3) . . ? C14 Fe1 C16 68.8(3) . . ? C17 Fe1 C16 41.3(3) . . ? C13 Fe1 C15 68.7(3) . . ? C8 Fe1 C15 141.1(3) . . ? C12 Fe1 C15 177.5(3) . . ? C9 Fe1 C15 114.1(3) . . ? C14 Fe1 C15 40.6(3) . . ? C17 Fe1 C15 67.3(3) . . ? C16 Fe1 C15 39.3(3) . . ? C13 Fe1 C11 138.6(3) . . ? C8 Fe1 C11 69.6(3) . . ? C12 Fe1 C11 41.2(3) . . ? C9 Fe1 C11 68.0(3) . . ? C14 Fe1 C11 178.9(3) . . ? C17 Fe1 C11 110.6(3) . . ? C16 Fe1 C11 110.3(3) . . ? C15 Fe1 C11 138.3(3) . . ? C13 Fe1 C10 178.3(3) . . ? C8 Fe1 C10 68.8(3) . . ? C12 Fe1 C10 68.2(3) . . ? C9 Fe1 C10 40.1(3) . . ? C14 Fe1 C10 139.4(3) . . ? C17 Fe1 C10 139.2(3) . . ? C16 Fe1 C10 111.5(3) . . ? C15 Fe1 C10 113.0(3) . . ? C11 Fe1 C10 40.2(3) . . ? C8 P1 C18 99.9(3) . . ? C8 P1 C36 98.8(3) . . ? C18 P1 C36 103.2(3) . . ? C8 P1 Ru1 121.2(2) . . ? C18 P1 Ru1 115.5(2) . . ? C36 P1 Ru1 115.2(2) . . ? C30 P2 C24 99.9(3) . . ? C30 P2 C13 100.9(3) . . ? C24 P2 C13 100.9(3) . . ? C30 P2 Ru1 113.8(2) . . ? C24 P2 Ru1 121.0(2) . . ? C13 P2 Ru1 117.2(2) . . ? O1 C1 Ru1 173.7(7) . . ? O2 C2 Ru3 179.2(11) . . ? O3 C3 Ru3 177.0(8) . . ? O4 C4 Ru3 173.3(8) . . ? O5 C5 Ru2 176.7(7) . . ? O6 C6 Ru2 170.9(7) . . ? O7 C7 Ru2 176.2(8) . . ? C9 C8 C12 106.8(6) . . ? C9 C8 P1 127.1(5) . . ? C12 C8 P1 126.0(5) . . ? C9 C8 Fe1 70.8(4) . . ? C12 C8 Fe1 69.6(4) . . ? P1 C8 Fe1 127.2(3) . . ? C8 C9 C10 108.9(7) . . ? C8 C9 Fe1 68.2(4) . . ? C10 C9 Fe1 70.6(4) . . ? C11 C10 C9 108.4(6) . . ? C11 C10 Fe1 69.2(4) . . ? C9 C10 Fe1 69.3(4) . . ? C10 C11 C12 107.1(7) . . ? C10 C11 Fe1 70.6(4) . . ? C12 C11 Fe1 68.3(4) . . ? C8 C12 C11 108.8(6) . . ? C8 C12 Fe1 69.2(4) . . ? C11 C12 Fe1 70.5(4) . . ? C14 C13 C17 107.4(6) . . ? C14 C13 P2 125.5(5) . . ? C17 C13 P2 127.1(5) . . ? C14 C13 Fe1 69.7(4) . . ? C17 C13 Fe1 71.1(4) . . ? P2 C13 Fe1 123.8(3) . . ? C13 C14 C15 106.8(6) . . ? C13 C14 Fe1 68.5(4) . . ? C15 C14 Fe1 70.7(4) . . ? C16 C15 C14 111.0(6) . . ? C16 C15 Fe1 70.4(4) . . ? C14 C15 Fe1 68.7(4) . . ? C15 C16 C17 107.1(7) . . ? C15 C16 Fe1 70.3(4) . . ? C17 C16 Fe1 69.5(4) . . ? C13 C17 C16 107.6(6) . . ? C13 C17 Fe1 67.6(4) . . ? C16 C17 Fe1 69.2(4) . . ? C23 C18 C19 117.2(7) . . ? C23 C18 P1 121.0(5) . . ? C19 C18 P1 121.7(6) . . ? C20 C19 C18 120.5(8) . . ? C19 C20 C21 121.8(8) . . ? C20 C21 C22 119.5(8) . . ? C23 C22 C21 119.3(9) . . ? C18 C23 C22 121.6(8) . . ? C25 C24 C29 118.7(6) . . ? C25 C24 P2 120.8(5) . . ? C29 C24 P2 120.4(5) . . ? C24 C25 C26 121.8(7) . . ? C27 C26 C25 118.4(7) . . ? C26 C27 C28 120.5(8) . . ? C29 C28 C27 120.6(8) . . ? C28 C29 C24 119.9(7) . . ? C35 C30 C31 117.7(7) . . ? C35 C30 P2 122.4(5) . . ? C31 C30 P2 119.8(6) . . ? C30 C31 C32 120.6(8) . . ? C33 C32 C31 119.4(8) . . ? C34 C33 C32 120.4(8) . . ? C33 C34 C35 121.8(9) . . ? C30 C35 C34 120.1(8) . . ? C37 C36 C41 117.9(7) . . ? C37 C36 P1 120.4(5) . . ? C41 C36 P1 121.3(6) . . ? C36 C37 C38 121.4(7) . . ? C39 C38 C37 121.0(8) . . ? C40 C39 C38 117.8(8) . . ? C39 C40 C41 120.9(8) . . ? C36 C41 C40 120.8(9) . . ? Cl2 C1S Cl1 110.5(9) . . ? _refine_diff_density_max 1.365 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.129 #===END #Data for compound (3) data_gra5h _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C33H24O7P2Ru3Se2' _chemical_formula_sum 'C33 H24 O7 P2 Ru3 Se2' _chemical_formula_weight 1055.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ru' 'Ru' -1.2594 0.8363 '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' 'P' 'P' 0.1023 0.0942 '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' '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P21/c' 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 13.550(5) _cell_length_b 10.891(4) _cell_length_c 24.876(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.31(2) _cell_angle_gamma 90.00 _cell_volume 3587(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11.13 _cell_measurement_theta_max 16.76 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 3.411 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9026 _exptl_absorpt_correction_T_max 1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW 1100' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8840 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.1637 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 28.02 _reflns_number_total 8658 _reflns_number_gt 3277 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0947P)^2^+4.6451P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8658 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2953 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.2664 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.195 _refine_ls_shift/su_max 0.250 _refine_ls_shift/su_mean 0.014 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 0.71903(9) 0.15246(11) 0.74045(5) 0.0439(4) Uani 1 d . . . Ru2 Ru 0.60021(9) -0.00550(12) 0.66229(5) 0.0477(4) Uani 1 d . . . Ru3 Ru 0.68661(9) 0.12530(12) 0.58724(5) 0.0459(4) Uani 1 d . . . Se1 Se 0.60042(11) 0.22623(14) 0.65524(6) 0.0465(4) Uani 1 d . . . Se2 Se 0.78844(11) 0.02995(14) 0.67227(6) 0.0471(4) Uani 1 d . . . P1 P 0.8336(3) 0.3100(4) 0.75083(15) 0.0416(9) Uani 1 d . . . P2 P 0.7904(3) 0.2899(4) 0.57976(16) 0.0456(10) Uani 1 d . . . O1 O 0.8494(11) -0.0072(11) 0.8267(5) 0.086(4) Uani 1 d . . . O2 O 0.5968(10) 0.2549(12) 0.8184(5) 0.084(4) Uani 1 d . . . O3 O 0.5528(8) -0.0775(11) 0.7722(5) 0.072(3) Uani 1 d . . . O4 O 0.6297(10) -0.2640(13) 0.6236(6) 0.088(4) Uani 1 d . . . O5 O 0.3818(11) 0.0033(15) 0.6001(7) 0.119(6) Uani 1 d . . . O6 O 0.5155(11) 0.1872(15) 0.4933(5) 0.106(5) Uani 1 d . . . O7 O 0.7562(12) -0.0633(15) 0.5155(6) 0.112(6) Uani 1 d . . . C1 C 0.7985(13) 0.0583(14) 0.7970(6) 0.053(4) Uani 1 d . . . C2 C 0.6413(12) 0.2197(15) 0.7882(7) 0.057(4) Uani 1 d . . . C3 C 0.5751(11) -0.0439(15) 0.7317(7) 0.052(4) Uani 1 d . . . C4 C 0.6175(12) -0.1680(19) 0.6398(8) 0.068(5) Uani 1 d . . . C5 C 0.4632(14) 0.0009(18) 0.6236(7) 0.073(5) Uani 1 d . . . C6 C 0.5809(13) 0.1645(17) 0.5289(7) 0.065(5) Uani 1 d . . . C7 C 0.7321(13) 0.0093(17) 0.5424(6) 0.062(5) Uani 1 d . . . C8 C 0.8902(11) 0.3350(14) 0.6896(6) 0.049(4) Uani 1 d . . . H8A H 0.9481 0.3890 0.7001 0.06(2) Uiso 1 calc R . . H8B H 0.9145 0.2570 0.6789 0.06(2) Uiso 1 calc R . . C9 C 0.8201(12) 0.3887(14) 0.6416(5) 0.053(4) Uani 1 d . . . H9A H 0.8491 0.4648 0.6317 0.06(2) Uiso 1 calc R . . H9B H 0.7574 0.4091 0.6524 0.06(2) Uiso 1 calc R . . C10 C 0.7922(11) 0.4625(13) 0.7654(6) 0.043(4) Uani 1 d . . . C11 C 0.6922(12) 0.4979(16) 0.7511(7) 0.067(5) Uani 1 d . . . H11 H 0.6437 0.4416 0.7344 0.068(11) Uiso 1 calc R . . C12 C 0.6628(13) 0.6165(16) 0.7615(8) 0.074(5) Uani 1 d . . . H12 H 0.5958 0.6407 0.7501 0.068(11) Uiso 1 calc R . . C13 C 0.7328(13) 0.6966(15) 0.7885(7) 0.065(5) Uani 1 d . . . H13 H 0.7127 0.7747 0.7968 0.068(11) Uiso 1 calc R . . C14 C 0.8330(12) 0.6643(15) 0.8039(7) 0.059(4) Uani 1 d . . . H14 H 0.8808 0.7196 0.8223 0.068(11) Uiso 1 calc R . . C15 C 0.8613(12) 0.5460(14) 0.7910(5) 0.048(4) Uani 1 d . . . H15 H 0.9291 0.5238 0.8003 0.068(11) Uiso 1 calc R . . C16 C 0.9389(11) 0.2820(13) 0.8089(6) 0.046(4) Uani 1 d . . . C17 C 0.9197(13) 0.2927(17) 0.8612(7) 0.072(5) Uani 1 d . . . H17 H 0.8564 0.3182 0.8657 0.068(11) Uiso 1 calc R . . C18 C 0.9951(16) 0.2651(18) 0.9071(7) 0.079(6) Uani 1 d . . . H18 H 0.9817 0.2720 0.9421 0.068(11) Uiso 1 calc R . . C19 C 1.0890(15) 0.2278(17) 0.9012(7) 0.073(5) Uani 1 d . . . H19 H 1.1394 0.2084 0.9317 0.068(11) Uiso 1 calc R . . C20 C 1.1061(12) 0.2200(15) 0.8491(8) 0.067(5) Uani 1 d . . . H20 H 1.1698 0.1962 0.8447 0.068(11) Uiso 1 calc R . . C21 C 1.0325(11) 0.2463(15) 0.8023(7) 0.061(5) Uani 1 d . . . H21 H 1.0465 0.2397 0.7674 0.068(11) Uiso 1 calc R . . C22 C 0.9162(12) 0.2663(16) 0.5670(6) 0.051(4) Uani 1 d . . . C23 C 0.9752(12) 0.3643(17) 0.5583(7) 0.064(5) Uani 1 d . . . H23 H 0.9486 0.4432 0.5574 0.068(11) Uiso 1 calc R . . C24 C 1.0721(12) 0.3489(19) 0.5510(7) 0.070(5) Uani 1 d . . . H24 H 1.1100 0.4172 0.5456 0.068(11) Uiso 1 calc R . . C25 C 1.1132(14) 0.234(2) 0.5514(7) 0.075(6) Uani 1 d . . . H25 H 1.1786 0.2235 0.5462 0.068(11) Uiso 1 calc R . . C26 C 1.0563(13) 0.1359(18) 0.5598(7) 0.072(5) Uani 1 d . . . H26 H 1.0837 0.0575 0.5605 0.068(11) Uiso 1 calc R . . C27 C 0.9585(12) 0.1497(15) 0.5674(6) 0.056(4) Uani 1 d . . . H27 H 0.9211 0.0809 0.5728 0.068(11) Uiso 1 calc R . . C28 C 0.7326(11) 0.3973(15) 0.5251(6) 0.049(4) Uani 1 d . . . C29 C 0.6835(17) 0.5019(19) 0.5360(8) 0.103(8) Uani 1 d . . . H29 H 0.6804 0.5227 0.5718 0.068(11) Uiso 1 calc R . . C30 C 0.639(2) 0.575(2) 0.4924(10) 0.137(11) Uani 1 d . . . H30 H 0.6096 0.6481 0.5000 0.068(11) Uiso 1 calc R . . C31 C 0.6364(18) 0.547(2) 0.4417(10) 0.109(8) Uani 1 d . . . H31 H 0.6004 0.5964 0.4136 0.068(11) Uiso 1 calc R . . C32 C 0.6858(18) 0.447(2) 0.4295(8) 0.099(7) Uani 1 d . . . H32 H 0.6872 0.4279 0.3932 0.068(11) Uiso 1 calc R . . C33 C 0.7335(16) 0.3750(19) 0.4716(8) 0.089(7) Uani 1 d . . . H33 H 0.7686 0.3066 0.4633 0.068(11) Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0428(7) 0.0450(8) 0.0444(7) -0.0004(6) 0.0104(6) 0.0010(6) Ru2 0.0411(7) 0.0476(8) 0.0537(8) -0.0028(6) 0.0087(6) -0.0017(6) Ru3 0.0451(7) 0.0482(8) 0.0442(7) -0.0040(6) 0.0090(6) 0.0043(6) Se1 0.0438(9) 0.0471(9) 0.0485(9) -0.0015(7) 0.0096(7) 0.0088(7) Se2 0.0412(9) 0.0455(9) 0.0538(10) -0.0032(7) 0.0087(7) 0.0048(7) P1 0.038(2) 0.045(2) 0.042(2) -0.0007(18) 0.0096(17) -0.0001(18) P2 0.048(2) 0.047(2) 0.045(2) 0.0012(19) 0.0151(19) 0.004(2) O1 0.105(11) 0.060(8) 0.082(9) 0.008(7) -0.003(8) 0.010(8) O2 0.102(10) 0.101(11) 0.059(8) -0.001(7) 0.039(7) 0.034(8) O3 0.056(7) 0.081(9) 0.085(9) 0.018(7) 0.030(7) -0.009(6) O4 0.079(9) 0.076(9) 0.108(11) -0.040(8) 0.014(8) -0.004(8) O5 0.065(9) 0.121(13) 0.147(14) 0.016(11) -0.032(10) -0.009(9) O6 0.104(11) 0.130(13) 0.065(9) -0.013(9) -0.021(8) 0.045(10) O7 0.123(13) 0.121(13) 0.087(10) -0.033(10) 0.012(9) 0.048(11) C1 0.074(12) 0.035(9) 0.051(10) 0.005(8) 0.014(9) 0.000(9) C2 0.052(10) 0.054(11) 0.063(11) -0.009(9) 0.008(9) 0.005(8) C3 0.041(9) 0.055(10) 0.061(11) 0.003(9) 0.012(8) 0.001(8) C4 0.043(10) 0.081(14) 0.079(13) -0.027(11) 0.012(9) 0.000(10) C5 0.061(12) 0.097(15) 0.055(11) 0.001(11) 0.002(9) -0.004(12) C6 0.060(11) 0.086(14) 0.047(10) 0.004(10) 0.008(9) 0.025(10) C7 0.072(12) 0.071(12) 0.042(10) -0.004(9) 0.015(9) 0.007(10) C8 0.048(9) 0.050(10) 0.048(9) -0.006(8) 0.011(8) -0.002(8) C9 0.075(11) 0.051(10) 0.039(9) 0.004(8) 0.027(8) -0.002(9) C10 0.049(9) 0.042(9) 0.040(8) 0.001(7) 0.016(7) 0.003(7) C11 0.047(10) 0.062(12) 0.085(13) -0.005(10) 0.000(9) -0.001(9) C12 0.050(11) 0.055(11) 0.114(16) -0.016(11) 0.013(11) 0.014(9) C13 0.069(12) 0.040(10) 0.087(13) 0.004(9) 0.018(10) 0.011(9) C14 0.053(10) 0.055(11) 0.068(11) 0.013(9) 0.013(9) -0.007(9) C15 0.071(11) 0.049(10) 0.024(7) 0.006(7) 0.011(7) 0.008(9) C16 0.043(9) 0.043(9) 0.052(9) -0.015(7) 0.013(7) -0.008(7) C17 0.064(12) 0.072(13) 0.079(13) 0.011(11) 0.011(10) 0.032(10) C18 0.105(16) 0.094(15) 0.030(9) -0.013(9) -0.002(10) 0.020(13) C19 0.076(14) 0.071(13) 0.055(12) 0.018(10) -0.020(10) 0.005(11) C20 0.044(10) 0.049(11) 0.105(16) -0.006(11) 0.008(11) -0.001(8) C21 0.042(9) 0.060(11) 0.079(12) 0.005(9) 0.006(9) 0.004(8) C22 0.060(10) 0.066(11) 0.032(8) -0.011(8) 0.022(7) -0.008(9) C23 0.061(11) 0.071(13) 0.065(11) -0.019(9) 0.025(9) 0.000(10) C24 0.049(10) 0.089(15) 0.079(13) 0.002(11) 0.032(10) -0.003(10) C25 0.056(12) 0.103(17) 0.069(13) -0.014(12) 0.020(10) 0.011(12) C26 0.061(12) 0.077(14) 0.084(14) 0.004(11) 0.029(11) 0.013(11) C27 0.062(11) 0.057(11) 0.055(10) -0.005(8) 0.027(9) 0.004(9) C28 0.045(9) 0.068(11) 0.033(8) 0.006(8) 0.010(7) 0.007(8) C29 0.15(2) 0.097(17) 0.058(12) 0.017(12) 0.015(13) 0.066(16) C30 0.18(3) 0.12(2) 0.094(18) 0.018(18) -0.007(19) 0.09(2) C31 0.111(19) 0.11(2) 0.089(18) 0.034(16) -0.020(15) 0.032(16) C32 0.13(2) 0.113(19) 0.048(12) 0.031(13) 0.002(12) 0.021(16) C33 0.112(17) 0.086(15) 0.080(15) 0.013(12) 0.045(13) 0.020(13) _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 C1 1.883(17) . ? Ru1 C2 1.894(18) . ? Ru1 P1 2.291(4) . ? Ru1 Se2 2.494(2) . ? Ru1 Se1 2.504(2) . ? Ru1 Ru2 2.8280(19) . ? Ru2 C3 1.876(17) . ? Ru2 C4 1.89(2) . ? Ru2 C5 1.901(19) . ? Ru2 Se1 2.530(2) . ? Ru2 Se2 2.539(2) . ? Ru2 Ru3 2.7960(18) . ? Ru3 C6 1.859(17) . ? Ru3 C7 1.874(18) . ? Ru3 P2 2.310(4) . ? Ru3 Se2 2.492(2) . ? Ru3 Se1 2.5053(19) . ? P1 C10 1.814(15) . ? P1 C16 1.827(15) . ? P1 C8 1.865(14) . ? P2 C22 1.817(15) . ? P2 C28 1.838(15) . ? P2 C9 1.849(15) . ? O1 C1 1.146(17) . ? O2 C2 1.126(18) . ? O3 C3 1.172(17) . ? O4 C4 1.145(19) . ? O5 C5 1.133(19) . ? O6 C6 1.137(18) . ? O7 C7 1.130(18) . ? C8 C9 1.481(19) . ? C10 C15 1.36(2) . ? C10 C11 1.38(2) . ? C11 C12 1.39(2) . ? C12 C13 1.36(2) . ? C13 C14 1.38(2) . ? C14 C15 1.40(2) . ? C16 C21 1.369(19) . ? C16 C17 1.39(2) . ? C17 C18 1.39(2) . ? C18 C19 1.37(2) . ? C19 C20 1.37(2) . ? C20 C21 1.39(2) . ? C22 C27 1.39(2) . ? C22 C23 1.38(2) . ? C23 C24 1.37(2) . ? C24 C25 1.37(2) . ? C25 C26 1.36(2) . ? C26 C27 1.39(2) . ? C28 C33 1.36(2) . ? C28 C29 1.37(2) . ? C29 C30 1.37(3) . ? C30 C31 1.29(3) . ? C31 C32 1.35(3) . ? C32 C33 1.36(2) . ? 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 Ru1 C2 92.7(7) . . ? C1 Ru1 P1 93.3(5) . . ? C2 Ru1 P1 95.4(5) . . ? C1 Ru1 Se2 88.8(5) . . ? C2 Ru1 Se2 166.8(5) . . ? P1 Ru1 Se2 97.62(11) . . ? C1 Ru1 Se1 165.7(5) . . ? C2 Ru1 Se1 93.7(5) . . ? P1 Ru1 Se1 98.76(11) . . ? Se2 Ru1 Se1 82.12(6) . . ? C1 Ru1 Ru2 109.5(5) . . ? C2 Ru1 Ru2 110.8(5) . . ? P1 Ru1 Ru2 143.69(11) . . ? Se2 Ru1 Ru2 56.57(5) . . ? Se1 Ru1 Ru2 56.26(5) . . ? C3 Ru2 C4 97.0(8) . . ? C3 Ru2 C5 97.1(7) . . ? C4 Ru2 C5 93.1(8) . . ? C3 Ru2 Se1 106.8(5) . . ? C4 Ru2 Se1 156.0(6) . . ? C5 Ru2 Se1 86.8(6) . . ? C3 Ru2 Se2 108.6(5) . . ? C4 Ru2 Se2 89.2(5) . . ? C5 Ru2 Se2 153.7(5) . . ? Se1 Ru2 Se2 80.74(6) . . ? C3 Ru2 Ru3 155.7(5) . . ? C4 Ru2 Ru3 100.6(6) . . ? C5 Ru2 Ru3 98.4(6) . . ? Se1 Ru2 Ru3 55.85(5) . . ? Se2 Ru2 Ru3 55.45(5) . . ? C3 Ru2 Ru1 72.0(5) . . ? C4 Ru2 Ru1 133.3(5) . . ? C5 Ru2 Ru1 132.6(6) . . ? Se1 Ru2 Ru1 55.38(5) . . ? Se2 Ru2 Ru1 55.07(5) . . ? Ru3 Ru2 Ru1 83.75(5) . . ? C6 Ru3 C7 89.2(7) . . ? C6 Ru3 P2 98.0(6) . . ? C7 Ru3 P2 101.1(6) . . ? C6 Ru3 Se2 162.5(6) . . ? C7 Ru3 Se2 91.8(5) . . ? P2 Ru3 Se2 98.93(12) . . ? C6 Ru3 Se1 91.9(5) . . ? C7 Ru3 Se1 163.2(5) . . ? P2 Ru3 Se1 95.35(11) . . ? Se2 Ru3 Se1 82.13(6) . . ? C6 Ru3 Ru2 106.0(6) . . ? C7 Ru3 Ru2 106.9(5) . . ? P2 Ru3 Ru2 142.92(11) . . ? Se2 Ru3 Ru2 57.03(5) . . ? Se1 Ru3 Ru2 56.69(6) . . ? Ru1 Se1 Ru3 97.09(7) . . ? Ru1 Se1 Ru2 68.36(6) . . ? Ru3 Se1 Ru2 67.46(6) . . ? Ru3 Se2 Ru1 97.67(7) . . ? Ru3 Se2 Ru2 67.51(6) . . ? Ru1 Se2 Ru2 68.36(6) . . ? C10 P1 C16 102.6(7) . . ? C10 P1 C8 103.2(7) . . ? C16 P1 C8 106.3(7) . . ? C10 P1 Ru1 118.5(5) . . ? C16 P1 Ru1 111.1(5) . . ? C8 P1 Ru1 113.9(5) . . ? C22 P2 C28 103.2(7) . . ? C22 P2 C9 100.5(7) . . ? C28 P2 C9 103.1(7) . . ? C22 P2 Ru3 120.9(6) . . ? C28 P2 Ru3 112.5(5) . . ? C9 P2 Ru3 114.4(5) . . ? O1 C1 Ru1 172.1(15) . . ? O2 C2 Ru1 176.5(16) . . ? O3 C3 Ru2 172.9(14) . . ? O4 C4 Ru2 176.1(18) . . ? O5 C5 Ru2 178.9(19) . . ? O6 C6 Ru3 179.1(19) . . ? O7 C7 Ru3 177.3(18) . . ? C9 C8 P1 114.3(10) . . ? C8 C9 P2 115.5(11) . . ? C15 C10 C11 118.2(14) . . ? C15 C10 P1 119.6(11) . . ? C11 C10 P1 122.2(12) . . ? C10 C11 C12 121.0(16) . . ? C13 C12 C11 119.4(16) . . ? C12 C13 C14 121.2(16) . . ? C13 C14 C15 118.3(16) . . ? C10 C15 C14 121.8(15) . . ? C21 C16 C17 120.1(15) . . ? C21 C16 P1 122.7(12) . . ? C17 C16 P1 117.2(12) . . ? C16 C17 C18 119.9(16) . . ? C19 C18 C17 120.8(16) . . ? C18 C19 C20 117.8(15) . . ? C21 C20 C19 123.0(17) . . ? C16 C21 C20 118.3(17) . . ? C27 C22 C23 117.1(15) . . ? C27 C22 P2 121.8(12) . . ? C23 C22 P2 121.0(13) . . ? C24 C23 C22 121.9(17) . . ? C23 C24 C25 120.7(18) . . ? C26 C25 C24 118.4(17) . . ? C25 C26 C27 121.7(18) . . ? C22 C27 C26 120.1(16) . . ? C33 C28 C29 116.6(16) . . ? C33 C28 P2 121.4(14) . . ? C29 C28 P2 122.0(12) . . ? C30 C29 C28 118.2(19) . . ? C31 C30 C29 124(2) . . ? C30 C31 C32 120(2) . . ? C33 C32 C31 118(2) . . ? C28 C33 C32 123(2) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 1.419 _refine_diff_density_min -1.245 _refine_diff_density_rms 0.226