Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Lappin, A.' 'Maiti, Rabindranath' 'Shang, Maoyu' _publ_contact_author_name 'Dr A Lappin' _publ_contact_author_address ; Department of Chemistry & Biochemistry University of Notre Dame 251 Nieuwland Science Hall Notre Dame IN 46556-5670 UNITED STATES OF AMERICA ; _publ_section_title ; The chemistry of ruthenium complexes of 1,2-dicyanoethylene dithiolate (mnt2-). Synthesis and characterization of [RuIV/III(mnt)3]2-/3- and the derivatives trans-[RuIII(mnt)2(PPh3)2]-, trans-[RuIII(mnt)2(py)2]- and trans-[RuIV(mnt)2(Br)2]2- ; data_la1806 _database_code_CSD 174146 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Et4N)2Ru[S2C2(CN)2]2Br2 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C8 H20 N 1+), (C8 Br2 N4 Ru S4 2-)' _chemical_formula_sum 'C24 H40 Br2 N6 Ru S4' _chemical_formula_weight 801.75 _publ_requested_journal 'test' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2017(6) _cell_length_b 9.4615(8) _cell_length_c 12.5828(12) _cell_angle_alpha 75.457(7) _cell_angle_beta 88.446(7) _cell_angle_gamma 81.798(7) _cell_volume 821.38(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description plate-like _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 3.188 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4260 _exptl_absorpt_correction_T_max 0.6240 _exptl_absorpt_process_details ; Absorption correction was based on psi-scan data of 6 reflecations (North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2891 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2891 _reflns_number_gt 2510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-ARGUS (Enraf-Nonius, 1994)' _computing_cell_refinement 'CAD4-ARGUS (Enraf-Nonius, 1994)' _computing_data_reduction ; Chi90s (Boyle, 1997), Xcad4 (Harms, 1996), SHELXTL-v5 (Siemens, 1994) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXTL-v5 (Siemens, 1994)' _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^)+(0.0343P)^2^+0.3862P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2891 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0657 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.5000 0.5000 0.5000 0.03728(10) Uani 1 2 d S . . Br Br 0.55425(5) 0.24091(3) 0.46364(2) 0.05552(11) Uani 1 1 d . . . S1 S 0.65891(10) 0.40745(8) 0.66287(5) 0.04253(17) Uani 1 1 d . . . S2 S 0.22990(10) 0.44168(9) 0.58965(6) 0.04593(18) Uani 1 1 d . . . C1 C 0.4900(4) 0.3442(3) 0.7524(2) 0.0387(6) Uani 1 1 d . . . C2 C 0.5433(4) 0.2743(3) 0.8648(2) 0.0461(7) Uani 1 1 d . . . N1 N 0.5839(4) 0.2174(3) 0.9534(2) 0.0649(8) Uani 1 1 d . . . C3 C 0.3050(4) 0.3575(3) 0.7204(2) 0.0401(6) Uani 1 1 d . . . C4 C 0.1703(4) 0.3002(4) 0.7989(2) 0.0501(7) Uani 1 1 d . . . N2 N 0.0649(4) 0.2531(4) 0.8627(2) 0.0790(10) Uani 1 1 d . . . N3 N 0.9041(3) 0.8265(2) 0.78117(17) 0.0393(5) Uani 1 1 d . . . C5 C 0.7571(4) 0.9248(4) 0.8272(3) 0.0546(8) Uani 1 1 d . . . H5A H 0.8071 1.0142 0.8287 0.066 Uiso 1 1 calc R . . H5B H 0.7321 0.8749 0.9024 0.066 Uiso 1 1 calc R . . C6 C 0.5737(5) 0.9668(4) 0.7634(3) 0.0655(9) Uani 1 1 d . . . H6A H 0.5907 1.0361 0.6948 0.098 Uiso 1 1 calc R . . H6B H 0.4796 1.0107 0.8053 0.098 Uiso 1 1 calc R . . H6C H 0.5347 0.8802 0.7495 0.098 Uiso 1 1 calc R . . C7 C 0.8330(4) 0.6842(3) 0.7789(3) 0.0515(7) Uani 1 1 d . . . H7A H 0.9304 0.6233 0.7492 0.062 Uiso 1 1 calc R . . H7B H 0.7258 0.7073 0.7294 0.062 Uiso 1 1 calc R . . C8 C 0.7759(5) 0.5956(4) 0.8898(3) 0.0616(9) Uani 1 1 d . . . H8A H 0.7501 0.5013 0.8834 0.092 Uiso 1 1 calc R . . H8B H 0.6655 0.6477 0.9143 0.092 Uiso 1 1 calc R . . H8C H 0.8760 0.5818 0.9418 0.092 Uiso 1 1 calc R . . C9 C 0.9510(5) 0.8984(4) 0.6639(2) 0.0571(8) Uani 1 1 d . . . H9A H 0.8380 0.9166 0.6194 0.069 Uiso 1 1 calc R . . H9B H 1.0410 0.8295 0.6368 0.069 Uiso 1 1 calc R . . C10 C 1.0309(6) 1.0429(4) 0.6473(3) 0.0715(10) Uani 1 1 d . . . H10A H 1.0363 1.0886 0.5702 0.107 Uiso 1 1 calc R . . H10B H 1.1549 1.0237 0.6785 0.107 Uiso 1 1 calc R . . H10C H 0.9518 1.1076 0.6828 0.107 Uiso 1 1 calc R . . C11 C 1.0748(4) 0.7950(4) 0.8564(2) 0.0518(7) Uani 1 1 d . . . H11A H 1.1252 0.8864 0.8503 0.062 Uiso 1 1 calc R . . H11B H 1.0348 0.7612 0.9316 0.062 Uiso 1 1 calc R . . C12 C 1.2297(4) 0.6815(4) 0.8325(3) 0.0606(9) Uani 1 1 d . . . H12A H 1.1891 0.5860 0.8518 0.091 Uiso 1 1 calc R . . H12B H 1.3394 0.6796 0.8749 0.091 Uiso 1 1 calc R . . H12C H 1.2589 0.7069 0.7558 0.091 Uiso 1 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 Ru 0.04106(18) 0.04514(19) 0.02415(15) -0.00697(12) 0.00019(12) -0.00418(13) Br 0.0727(2) 0.0503(2) 0.04418(18) -0.01574(14) 0.00041(15) -0.00335(16) S1 0.0438(4) 0.0529(4) 0.0293(3) -0.0076(3) -0.0019(3) -0.0059(3) S2 0.0429(4) 0.0596(5) 0.0320(3) -0.0062(3) -0.0007(3) -0.0056(3) C1 0.0503(16) 0.0388(15) 0.0273(12) -0.0095(11) -0.0003(11) -0.0044(12) C2 0.0521(17) 0.0527(17) 0.0349(16) -0.0125(13) 0.0031(13) -0.0099(14) N1 0.0770(19) 0.079(2) 0.0336(14) -0.0032(13) -0.0071(13) -0.0119(15) C3 0.0489(16) 0.0420(15) 0.0293(13) -0.0097(11) 0.0044(11) -0.0055(12) C4 0.0493(17) 0.063(2) 0.0362(15) -0.0102(14) -0.0001(13) -0.0060(15) N2 0.0658(19) 0.117(3) 0.0509(17) -0.0080(17) 0.0132(15) -0.0269(19) N3 0.0456(12) 0.0419(13) 0.0327(11) -0.0136(9) -0.0024(9) -0.0054(10) C5 0.0601(19) 0.0531(19) 0.0560(19) -0.0244(15) 0.0082(15) -0.0077(15) C6 0.0554(19) 0.050(2) 0.088(3) -0.0157(18) -0.0046(18) 0.0015(15) C7 0.0560(18) 0.0489(17) 0.0536(18) -0.0190(14) -0.0089(14) -0.0072(14) C8 0.059(2) 0.057(2) 0.065(2) -0.0047(16) -0.0004(16) -0.0145(16) C9 0.069(2) 0.068(2) 0.0328(15) -0.0106(14) 0.0023(14) -0.0093(17) C10 0.090(3) 0.065(2) 0.057(2) -0.0037(17) 0.0104(19) -0.023(2) C11 0.0559(18) 0.064(2) 0.0394(16) -0.0167(14) -0.0037(13) -0.0152(15) C12 0.0468(17) 0.080(2) 0.0558(19) -0.0220(17) -0.0023(15) -0.0012(16) _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 S1 2.2840(7) 2_666 ? Ru S1 2.2840(7) . ? Ru S2 2.2881(7) . ? Ru S2 2.2881(7) 2_666 ? Ru Br 2.5790(4) . ? Ru Br 2.5790(4) 2_666 ? S1 C1 1.704(3) . ? S2 C3 1.704(3) . ? C1 C3 1.382(4) . ? C1 C2 1.439(4) . ? C2 N1 1.136(4) . ? C3 C4 1.428(4) . ? C4 N2 1.141(4) . ? N3 C5 1.509(4) . ? N3 C9 1.513(3) . ? N3 C7 1.514(4) . ? N3 C11 1.521(4) . ? C5 C6 1.515(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.515(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.522(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.514(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 S1 Ru S1 180.0 2_666 . ? S1 Ru S2 91.28(3) 2_666 . ? S1 Ru S2 88.72(3) . . ? S1 Ru S2 88.72(3) 2_666 2_666 ? S1 Ru S2 91.28(3) . 2_666 ? S2 Ru S2 180.0 . 2_666 ? S1 Ru Br 90.52(2) 2_666 . ? S1 Ru Br 89.48(2) . . ? S2 Ru Br 88.73(2) . . ? S2 Ru Br 91.27(2) 2_666 . ? S1 Ru Br 89.48(2) 2_666 2_666 ? S1 Ru Br 90.52(2) . 2_666 ? S2 Ru Br 91.27(2) . 2_666 ? S2 Ru Br 88.73(2) 2_666 2_666 ? Br Ru Br 180.0 . 2_666 ? C1 S1 Ru 103.49(9) . . ? C3 S2 Ru 103.34(10) . . ? C3 C1 C2 119.4(2) . . ? C3 C1 S1 122.1(2) . . ? C2 C1 S1 118.5(2) . . ? N1 C2 C1 179.0(3) . . ? C1 C3 C4 119.5(2) . . ? C1 C3 S2 122.2(2) . . ? C4 C3 S2 118.2(2) . . ? N2 C4 C3 178.9(4) . . ? C5 N3 C9 111.4(2) . . ? C5 N3 C7 110.5(2) . . ? C9 N3 C7 106.4(2) . . ? C5 N3 C11 106.5(2) . . ? C9 N3 C11 111.6(2) . . ? C7 N3 C11 110.4(2) . . ? N3 C5 C6 114.3(3) . . ? N3 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? N3 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 114.6(2) . . ? N3 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N3 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 115.4(3) . . ? N3 C9 H9A 108.4 . . ? C10 C9 H9A 108.4 . . ? N3 C9 H9B 108.4 . . ? C10 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 N3 114.6(2) . . ? C12 C11 H11A 108.6 . . ? N3 C11 H11A 108.6 . . ? C12 C11 H11B 108.6 . . ? N3 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.430 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.054 data_la9802 _database_code_CSD 174147 _audit_creation_method SHELXL _chemical_name_systematic ; (Et4N)[Ru(dithiolate)2(PPh3)2] ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H50 N5 P2 Ru S4' _chemical_formula_weight 1036.22 _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' 'N' 'N' 0.0061 0.0033 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 17.188(2) _cell_length_b 12.8718(11) _cell_length_c 22.896(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.873(8) _cell_angle_gamma 90.00 _cell_volume 4957.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description block-shaped _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method ? _exptl_crystal_F_000 2140 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8472 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w/2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8986 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 24.97 _reflns_number_total 8684 _reflns_number_observed 5936 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius, 1985)' _computing_cell_refinement 'CAD4 (Enraf-Nonius, 1985)' _computing_data_reduction ; Chi90s (Boyle, 1996) Xcad4 (Harms, 1996) SHELXTL-V5 (Siemens, 1994) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXTL-V5 (Siemens, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0376P)^2^+3.5728P] 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 'idealized with riding models' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8684 _refine_ls_number_parameters 655 _refine_ls_number_restraints 196 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_obs 0.0354 _refine_ls_wR_factor_all 0.0937 _refine_ls_wR_factor_obs 0.0806 _refine_ls_goodness_of_fit_all 0.984 _refine_ls_goodness_of_fit_obs 1.042 _refine_ls_restrained_S_all 0.977 _refine_ls_restrained_S_obs 1.031 _refine_ls_shift/esd_max 0.035 _refine_ls_shift/esd_mean 0.001 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 0.5000 0.5000 0.5000 0.03025(9) Uani 1 d S . S1 S 0.36706(4) 0.47735(6) 0.50789(3) 0.0368(2) Uani 1 d . . S2 S 0.55048(5) 0.44814(6) 0.59810(3) 0.0412(2) Uani 1 d . . C1 C 0.3142(2) 0.4907(2) 0.43544(14) 0.0415(8) Uani 1 d . . C2 C 0.2307(2) 0.4690(3) 0.4238(2) 0.0532(9) Uani 1 d . . N1 N 0.1638(2) 0.4524(3) 0.4133(2) 0.0795(11) Uani 1 d . . C3 C 0.6499(2) 0.4782(2) 0.60967(14) 0.0422(8) Uani 1 d . . C4 C 0.6953(2) 0.4661(3) 0.6692(2) 0.0544(9) Uani 1 d . . N2 N 0.7300(2) 0.4576(3) 0.71744(15) 0.0868(12) Uani 1 d . . P1 P 0.49290(5) 0.67726(6) 0.53797(3) 0.0346(2) Uani 1 d . . C5 C 0.5881(2) 0.7390(2) 0.56999(13) 0.0372(7) Uani 1 d . . C6 C 0.6414(2) 0.7626(2) 0.53306(15) 0.0461(8) Uani 1 d . . H6 H 0.6282(2) 0.7474(2) 0.49251(15) 0.055 Uiso 1 calc R . C7 C 0.7133(2) 0.8082(3) 0.5570(2) 0.0564(9) Uani 1 d . . H7 H 0.7485(2) 0.8236(3) 0.5324(2) 0.068 Uiso 1 calc R . C8 C 0.7340(2) 0.8314(3) 0.6171(2) 0.0626(10) Uani 1 d . . H8 H 0.7825(2) 0.8628(3) 0.6327(2) 0.075 Uiso 1 calc R . C9 C 0.6826(2) 0.8079(3) 0.6533(2) 0.0610(10) Uani 1 d . . H9 H 0.6964(2) 0.8237(3) 0.6937(2) 0.073 Uiso 1 calc R . C10 C 0.6105(2) 0.7611(3) 0.63073(15) 0.0482(8) Uani 1 d . . H10 H 0.5767(2) 0.7441(3) 0.65620(15) 0.058 Uiso 1 calc R . C11 C 0.4376(2) 0.6998(3) 0.59757(14) 0.0413(7) Uani 1 d . . C12 C 0.4193(2) 0.6213(3) 0.63334(15) 0.0549(9) Uani 1 d . . H12 H 0.4333(2) 0.5533(3) 0.62649(15) 0.066 Uiso 1 calc R . C13 C 0.3602(3) 0.7424(4) 0.6899(2) 0.0820(14) Uani 1 d . . H13 H 0.3348(3) 0.7570(4) 0.7211(2) 0.098 Uiso 1 calc R . C14 C 0.3803(2) 0.6423(4) 0.6796(2) 0.0717(12) Uani 1 d . . H14 H 0.3679(2) 0.5886(4) 0.7033(2) 0.086 Uiso 1 calc R . C15 C 0.3777(2) 0.8220(4) 0.6542(2) 0.0712(12) Uani 1 d . . H15 H 0.3636(2) 0.8899(4) 0.6612(2) 0.085 Uiso 1 calc R . C16 C 0.4156(2) 0.8008(3) 0.6087(2) 0.0537(9) Uani 1 d . . H16 H 0.4270(2) 0.8548(3) 0.5848(2) 0.064 Uiso 1 calc R . C17 C 0.4417(2) 0.7722(2) 0.48289(14) 0.0420(7) Uani 1 d . . C18 C 0.4760(2) 0.8595(3) 0.4644(2) 0.0586(10) Uani 1 d . . H18 H 0.5300(2) 0.8718(3) 0.4780(2) 0.070 Uiso 1 calc R . C19 C 0.4304(3) 0.9294(3) 0.4256(2) 0.0816(14) Uani 1 d . . H19 H 0.4540(3) 0.9884(3) 0.4133(2) 0.098 Uiso 1 calc R . C20 C 0.3505(3) 0.9117(3) 0.4052(2) 0.0847(14) Uani 1 d . . H20 H 0.3199(3) 0.9585(3) 0.3792(2) 0.102 Uiso 1 calc R . C21 C 0.3163(3) 0.8252(3) 0.4234(2) 0.0728(12) Uani 1 d . . H21 H 0.2622(3) 0.8133(3) 0.4099(2) 0.087 Uiso 1 calc R . C22 C 0.3609(2) 0.7556(3) 0.4615(2) 0.0538(9) Uani 1 d . . H22 H 0.3369(2) 0.6966(3) 0.4733(2) 0.065 Uiso 1 calc R . Ru2 Ru 0.0000 1.0000 0.5000 0.02926(9) Uani 1 d S . S3 S -0.13165(4) 0.96385(6) 0.50547(3) 0.0362(2) Uani 1 d . . S4 S 0.05185(5) 0.93479(6) 0.59515(3) 0.0398(2) Uani 1 d . . C23 C -0.1840(2) 0.9806(2) 0.43310(14) 0.0398(7) Uani 1 d . . C24 C -0.2654(2) 0.9494(3) 0.4195(2) 0.0526(9) Uani 1 d . . N3 N -0.3307(2) 0.9246(3) 0.4084(2) 0.0804(11) Uani 1 d . . C25 C 0.1495(2) 0.9758(2) 0.60962(13) 0.0392(7) Uani 1 d . . C26 C 0.1929(2) 0.9608(3) 0.6692(2) 0.0533(9) Uani 1 d . . N4 N 0.2255(2) 0.9493(3) 0.71780(15) 0.0799(11) Uani 1 d . . P2 P 0.01546(5) 0.83175(6) 0.45339(3) 0.0345(2) Uani 1 d . . C27 C -0.0776(2) 0.7629(2) 0.42374(13) 0.0377(7) Uani 1 d . . C28 C -0.1250(2) 0.7304(2) 0.46280(15) 0.0446(8) Uani 1 d . . H28 H -0.1082(2) 0.7421(2) 0.50354(15) 0.054 Uiso 1 calc R . C29 C -0.1965(2) 0.6811(3) 0.4418(2) 0.0520(9) Uani 1 d . . H29 H -0.2274(2) 0.6591(3) 0.4684(2) 0.062 Uiso 1 calc R . C30 C -0.2220(2) 0.6645(3) 0.3818(2) 0.0624(10) Uani 1 d . . H30 H -0.2705(2) 0.6320(3) 0.3675(2) 0.075 Uiso 1 calc R . C31 C -0.1765(2) 0.6957(3) 0.3433(2) 0.0702(12) Uani 1 d . . H31 H -0.1938(2) 0.6833(3) 0.3027(2) 0.084 Uiso 1 calc R . C32 C -0.1044(2) 0.7459(3) 0.3633(2) 0.0548(9) Uani 1 d . . H32 H -0.0743(2) 0.7679(3) 0.3362(2) 0.066 Uiso 1 calc R . C33 C 0.0677(2) 0.8280(3) 0.39033(14) 0.0437(8) Uani 1 d . . C34 C 0.0846(2) 0.9160(3) 0.36130(15) 0.0525(9) Uani 1 d . . H34 H 0.0696(2) 0.9806(3) 0.37354(15) 0.063 Uiso 1 calc R . C35 C 0.1237(2) 0.9103(4) 0.3140(2) 0.0665(11) Uani 1 d . . H35 H 0.1350(2) 0.9706(4) 0.2950(2) 0.080 Uiso 1 calc R . C36 C 0.1455(2) 0.8161(4) 0.2958(2) 0.0742(13) Uani 1 d . . H36 H 0.1707(2) 0.8119(4) 0.2637(2) 0.089 Uiso 1 calc R . C37 C 0.1305(2) 0.7269(4) 0.3248(2) 0.0763(13) Uani 1 d . . H37 H 0.1469(2) 0.6629(4) 0.3128(2) 0.092 Uiso 1 calc R . C38 C 0.0910(2) 0.7325(3) 0.3716(2) 0.0597(10) Uani 1 d . . H38 H 0.0801(2) 0.6720(3) 0.3907(2) 0.072 Uiso 1 calc R . C39 C 0.0760(2) 0.7367(2) 0.50240(14) 0.0420(8) Uani 1 d . . C40 C 0.0486(2) 0.6442(3) 0.5214(2) 0.0568(9) Uani 1 d . . H40 H -0.0051(2) 0.6277(3) 0.5106(2) 0.068 Uiso 1 calc R . C41 C 0.1005(3) 0.5758(3) 0.5562(2) 0.0737(12) Uani 1 d . . H41 H 0.0815(3) 0.5134(3) 0.5682(2) 0.088 Uiso 1 calc R . C42 C 0.1801(3) 0.5994(3) 0.5732(2) 0.0716(12) Uani 1 d . . H42 H 0.2148(3) 0.5532(3) 0.5967(2) 0.086 Uiso 1 calc R . C43 C 0.2074(2) 0.6904(3) 0.5555(2) 0.0654(11) Uani 1 d . . H43 H 0.2610(2) 0.7066(3) 0.5671(2) 0.078 Uiso 1 calc R . C44 C 0.1565(2) 0.7596(3) 0.5204(2) 0.0535(9) Uani 1 d . . H44 H 0.1763(2) 0.8219(3) 0.5088(2) 0.064 Uiso 1 calc R . N5 N 0.4878(2) 0.1809(3) 0.7552(2) 0.0704(9) Uani 1 d DU . C45 C 0.4363(4) 0.1875(5) 0.8004(3) 0.104(2) Uani 0.798(5) d PDU 1 H45A H 0.4455(4) 0.2542(5) 0.8204(3) 0.124 Uiso 0.798(5) calc PR 1 H45B H 0.4531(4) 0.1341(5) 0.8302(3) 0.124 Uiso 0.798(5) calc PR 1 C46 C 0.3467(9) 0.1756(10) 0.7762(8) 0.138(5) Uani 0.798(5) d PDU 1 H46A H 0.3191(9) 0.1811(10) 0.8085(8) 0.207 Uiso 0.798(5) calc PR 1 H46B H 0.3362(9) 0.1089(10) 0.7575(8) 0.207 Uiso 0.798(5) calc PR 1 H46C H 0.3286(9) 0.2293(10) 0.7475(8) 0.207 Uiso 0.798(5) calc PR 1 C47 C 0.4826(4) 0.0733(5) 0.7265(3) 0.115(3) Uani 0.798(5) d PDU 1 H47A H 0.5140(4) 0.0731(5) 0.6958(3) 0.138 Uiso 0.798(5) calc PR 1 H47B H 0.4278(4) 0.0600(5) 0.7072(3) 0.138 Uiso 0.798(5) calc PR 1 C48 C 0.5114(11) -0.0151(11) 0.7705(11) 0.217(13) Uani 0.798(5) d PDU 1 H48A H 0.5064(11) -0.0801(11) 0.7495(11) 0.325 Uiso 0.798(5) calc PR 1 H48B H 0.4798(11) -0.0167(11) 0.8006(11) 0.325 Uiso 0.798(5) calc PR 1 H48C H 0.5661(11) -0.0037(11) 0.7891(11) 0.325 Uiso 0.798(5) calc PR 1 C49 C 0.5715(4) 0.2026(6) 0.7872(3) 0.113(3) Uani 0.798(5) d PDU 1 H49A H 0.5840(4) 0.1580(6) 0.8220(3) 0.136 Uiso 0.798(5) calc PR 1 H49B H 0.5747(4) 0.2740(6) 0.8010(3) 0.136 Uiso 0.798(5) calc PR 1 C50 C 0.6331(7) 0.1858(13) 0.7495(6) 0.164(6) Uani 0.798(5) d PDU 1 H50A H 0.6849(7) 0.2011(13) 0.7727(6) 0.246 Uiso 0.798(5) calc PR 1 H50B H 0.6220(7) 0.2308(13) 0.7153(6) 0.246 Uiso 0.798(5) calc PR 1 H50C H 0.6314(7) 0.1148(13) 0.7364(6) 0.246 Uiso 0.798(5) calc PR 1 C51 C 0.4586(4) 0.2534(5) 0.7038(3) 0.087(2) Uani 0.798(5) d PDU 1 H51A H 0.4064(4) 0.2308(5) 0.6830(3) 0.105 Uiso 0.798(5) calc PR 1 H51B H 0.4941(4) 0.2490(5) 0.6760(3) 0.105 Uiso 0.798(5) calc PR 1 C52 C 0.4535(6) 0.3662(7) 0.7229(6) 0.127(4) Uani 0.798(5) d PDU 1 H52A H 0.4346(6) 0.4085(7) 0.6883(6) 0.191 Uiso 0.798(5) calc PR 1 H52B H 0.5052(6) 0.3897(7) 0.7427(6) 0.191 Uiso 0.798(5) calc PR 1 H52C H 0.4174(6) 0.3715(7) 0.7497(6) 0.191 Uiso 0.798(5) calc PR 1 C45A C 0.4030(11) 0.1682(18) 0.7234(11) 0.098(8) Uani 0.202(5) d PDU 2 H45C H 0.4005(11) 0.1191(18) 0.6909(11) 0.118 Uiso 0.202(5) calc PR 2 H45D H 0.3829(11) 0.2343(18) 0.7063(11) 0.118 Uiso 0.202(5) calc PR 2 C46A C 0.3502(38) 0.1296(40) 0.7650(28) 0.129(18) Uani 0.202(5) d PDU 2 H46D H 0.2966(38) 0.1226(40) 0.7431(28) 0.194 Uiso 0.202(5) calc PR 2 H46E H 0.3518(38) 0.1787(40) 0.7968(28) 0.194 Uiso 0.202(5) calc PR 2 H46F H 0.3692(38) 0.0635(40) 0.7814(28) 0.194 Uiso 0.202(5) calc PR 2 C47A C 0.5106(15) 0.1059(16) 0.8045(10) 0.110(9) Uani 0.202(5) d PDU 2 H47C H 0.4862(15) 0.1254(16) 0.8375(10) 0.132 Uiso 0.202(5) calc PR 2 H47D H 0.5679(15) 0.1068(16) 0.8185(10) 0.132 Uiso 0.202(5) calc PR 2 C48A C 0.4834(38) -0.0044(28) 0.7829(35) 0.119(15) Uani 0.202(5) d PDU 2 H48D H 0.4984(38) -0.0528(28) 0.8151(35) 0.178 Uiso 0.202(5) calc PR 2 H48E H 0.5081(38) -0.0238(28) 0.7505(35) 0.178 Uiso 0.202(5) calc PR 2 H48F H 0.4267(38) -0.0052(28) 0.7695(35) 0.178 Uiso 0.202(5) calc PR 2 C49A C 0.5408(13) 0.1792(21) 0.7105(9) 0.112(9) Uani 0.202(5) d PDU 2 H49C H 0.5135(13) 0.2155(21) 0.6750(9) 0.134 Uiso 0.202(5) calc PR 2 H49D H 0.5468(13) 0.1074(21) 0.6992(9) 0.134 Uiso 0.202(5) calc PR 2 C50A C 0.6251(21) 0.2267(43) 0.7292(18) 0.104(13) Uani 0.202(5) d PDU 2 H50D H 0.6526(21) 0.2200(43) 0.6970(18) 0.157 Uiso 0.202(5) calc PR 2 H50E H 0.6540(21) 0.1906(43) 0.7636(18) 0.157 Uiso 0.202(5) calc PR 2 H50F H 0.6208(21) 0.2988(43) 0.7387(18) 0.157 Uiso 0.202(5) calc PR 2 C51A C 0.4991(14) 0.2909(13) 0.7862(8) 0.083(7) Uani 0.202(5) d PDU 2 H51C H 0.4581(14) 0.3003(13) 0.8092(8) 0.100 Uiso 0.202(5) calc PR 2 H51D H 0.5501(14) 0.2921(13) 0.8139(8) 0.100 Uiso 0.202(5) calc PR 2 C52A C 0.4958(22) 0.3816(29) 0.7429(19) 0.103(12) Uani 0.202(5) d PDU 2 H52D H 0.5032(22) 0.4456(29) 0.7649(19) 0.154 Uiso 0.202(5) calc PR 2 H52E H 0.4450(22) 0.3824(29) 0.7160(19) 0.154 Uiso 0.202(5) calc PR 2 H52F H 0.5370(22) 0.3740(29) 0.7207(19) 0.154 Uiso 0.202(5) calc PR 2 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 0.0292(2) 0.0333(2) 0.0292(2) 0.00240(14) 0.00832(15) 0.00063(14) S1 0.0308(4) 0.0447(5) 0.0361(4) 0.0018(3) 0.0096(3) -0.0011(3) S2 0.0409(5) 0.0495(5) 0.0350(4) 0.0077(4) 0.0120(4) 0.0069(4) C1 0.037(2) 0.046(2) 0.042(2) -0.0028(15) 0.007(2) 0.0034(15) C2 0.045(2) 0.063(2) 0.048(2) -0.001(2) -0.001(2) -0.001(2) N1 0.040(2) 0.114(3) 0.079(2) -0.001(2) -0.001(2) -0.008(2) C3 0.044(2) 0.044(2) 0.038(2) -0.0020(14) 0.006(2) 0.0101(15) C4 0.049(2) 0.072(2) 0.040(2) -0.002(2) 0.005(2) 0.018(2) N2 0.083(3) 0.126(3) 0.045(2) 0.000(2) -0.003(2) 0.039(2) P1 0.0340(4) 0.0345(4) 0.0357(4) -0.0010(3) 0.0083(3) -0.0001(3) C5 0.035(2) 0.033(2) 0.040(2) 0.0008(13) 0.0020(14) -0.0023(13) C6 0.049(2) 0.041(2) 0.049(2) 0.001(2) 0.013(2) -0.007(2) C7 0.048(2) 0.049(2) 0.075(3) 0.003(2) 0.020(2) -0.012(2) C8 0.045(2) 0.055(2) 0.081(3) 0.004(2) -0.003(2) -0.013(2) C9 0.057(2) 0.065(2) 0.053(2) 0.000(2) -0.007(2) -0.008(2) C10 0.044(2) 0.052(2) 0.046(2) 0.003(2) 0.004(2) -0.003(2) C11 0.033(2) 0.051(2) 0.040(2) -0.0106(15) 0.0079(14) 0.0021(14) C12 0.054(2) 0.066(2) 0.050(2) 0.004(2) 0.023(2) 0.020(2) C13 0.077(3) 0.119(4) 0.057(2) -0.017(3) 0.030(2) 0.032(3) C14 0.073(3) 0.094(3) 0.055(2) 0.011(2) 0.031(2) 0.026(2) C15 0.066(3) 0.082(3) 0.066(3) -0.030(2) 0.016(2) 0.016(2) C16 0.046(2) 0.054(2) 0.061(2) -0.016(2) 0.011(2) 0.002(2) C17 0.048(2) 0.032(2) 0.043(2) 0.0009(14) 0.004(2) 0.0030(14) C18 0.066(3) 0.043(2) 0.061(2) 0.011(2) 0.000(2) -0.004(2) C19 0.103(4) 0.045(2) 0.086(3) 0.022(2) -0.005(3) -0.009(2) C20 0.103(4) 0.053(3) 0.082(3) 0.016(2) -0.020(3) 0.014(3) C21 0.062(3) 0.061(3) 0.083(3) 0.002(2) -0.016(2) 0.012(2) C22 0.050(2) 0.047(2) 0.059(2) 0.003(2) -0.002(2) 0.006(2) Ru2 0.0294(2) 0.0312(2) 0.0277(2) 0.00090(14) 0.00704(14) -0.00028(14) S3 0.0319(4) 0.0414(4) 0.0358(4) 0.0017(3) 0.0084(3) -0.0031(3) S4 0.0406(5) 0.0455(5) 0.0343(4) 0.0068(3) 0.0098(4) 0.0032(4) C23 0.035(2) 0.039(2) 0.043(2) -0.0008(14) 0.0028(15) 0.0037(14) C24 0.040(2) 0.063(2) 0.051(2) 0.008(2) 0.001(2) 0.000(2) N3 0.046(2) 0.105(3) 0.082(3) 0.019(2) -0.005(2) -0.015(2) C25 0.038(2) 0.043(2) 0.035(2) -0.0005(14) 0.0019(14) 0.0046(14) C26 0.050(2) 0.064(2) 0.044(2) 0.004(2) 0.006(2) 0.011(2) N4 0.075(3) 0.107(3) 0.049(2) 0.010(2) -0.006(2) 0.015(2) P2 0.0339(4) 0.0344(4) 0.0352(4) -0.0029(3) 0.0072(3) 0.0003(3) C27 0.035(2) 0.035(2) 0.042(2) -0.0037(14) 0.0060(14) 0.0001(13) C28 0.047(2) 0.037(2) 0.050(2) 0.0004(15) 0.012(2) -0.0014(15) C29 0.047(2) 0.044(2) 0.067(2) 0.010(2) 0.017(2) -0.005(2) C30 0.049(2) 0.058(2) 0.074(3) 0.005(2) -0.003(2) -0.015(2) C31 0.060(3) 0.090(3) 0.053(2) 0.001(2) -0.008(2) -0.022(2) C32 0.051(2) 0.065(2) 0.046(2) 0.002(2) 0.004(2) -0.011(2) C33 0.035(2) 0.056(2) 0.040(2) -0.012(2) 0.0102(14) -0.004(2) C34 0.054(2) 0.061(2) 0.047(2) -0.002(2) 0.020(2) 0.006(2) C35 0.065(3) 0.087(3) 0.055(2) -0.002(2) 0.031(2) -0.003(2) C36 0.065(3) 0.113(4) 0.053(2) -0.027(3) 0.030(2) -0.007(3) C37 0.063(3) 0.084(3) 0.088(3) -0.047(3) 0.028(2) -0.003(2) C38 0.053(2) 0.061(2) 0.071(3) -0.021(2) 0.024(2) -0.005(2) C39 0.042(2) 0.033(2) 0.048(2) -0.0056(14) 0.003(2) 0.0058(14) C40 0.056(2) 0.040(2) 0.067(2) 0.002(2) -0.006(2) -0.003(2) C41 0.082(3) 0.041(2) 0.086(3) 0.010(2) -0.011(3) 0.000(2) C42 0.069(3) 0.049(2) 0.084(3) 0.007(2) -0.014(2) 0.013(2) C43 0.049(2) 0.056(2) 0.082(3) -0.007(2) -0.009(2) 0.008(2) C44 0.046(2) 0.043(2) 0.067(2) -0.004(2) 0.002(2) 0.004(2) N5 0.073(2) 0.063(2) 0.067(2) -0.011(2) -0.007(2) 0.003(2) C45 0.135(7) 0.090(5) 0.090(5) 0.020(4) 0.031(5) -0.012(5) C46 0.100(7) 0.125(11) 0.197(13) 0.017(9) 0.051(8) -0.007(7) C47 0.118(6) 0.070(4) 0.122(5) -0.031(4) -0.054(4) 0.013(4) C48 0.236(24) 0.077(8) 0.271(20) -0.001(9) -0.102(19) 0.043(9) C49 0.080(5) 0.111(6) 0.131(6) -0.033(5) -0.022(4) -0.015(4) C50 0.088(7) 0.235(17) 0.168(13) -0.019(11) 0.019(8) 0.007(9) C51 0.099(5) 0.089(4) 0.080(4) 0.013(3) 0.034(4) 0.018(4) C52 0.150(11) 0.073(6) 0.185(12) 0.046(7) 0.095(8) 0.017(6) C45A 0.088(16) 0.074(15) 0.110(17) -0.019(14) -0.031(14) 0.001(13) C46A 0.134(34) 0.119(36) 0.128(28) 0.003(28) 0.011(24) -0.030(28) C47A 0.096(18) 0.098(18) 0.116(18) 0.021(16) -0.024(15) 0.014(15) C48A 0.114(26) 0.046(17) 0.163(32) 0.010(19) -0.050(24) 0.038(17) C49A 0.116(19) 0.136(20) 0.078(15) -0.038(15) 0.008(15) 0.027(17) C50A 0.076(20) 0.167(33) 0.072(17) 0.060(19) 0.018(15) 0.005(20) C51A 0.117(17) 0.085(15) 0.064(12) -0.027(11) 0.057(12) -0.023(13) C52A 0.109(27) 0.093(21) 0.109(23) -0.017(18) 0.030(20) -0.033(21) _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 S2 2.3327(8) 3_666 ? Ru1 S2 2.3327(8) . ? Ru1 S1 2.3471(8) . ? Ru1 S1 2.3471(8) 3_666 ? Ru1 P1 2.4537(8) . ? Ru1 P1 2.4537(8) 3_666 ? S1 C1 1.728(3) . ? S2 C3 1.719(3) . ? C1 C3 1.367(4) 3_666 ? C1 C2 1.432(5) . ? C2 N1 1.145(4) . ? C3 C1 1.367(4) 3_666 ? C3 C4 1.432(4) . ? C4 N2 1.148(4) . ? P1 C5 1.831(3) . ? P1 C11 1.840(3) . ? P1 C17 1.844(3) . ? C5 C10 1.394(4) . ? C5 C6 1.401(4) . ? C6 C7 1.378(5) . ? C7 C8 1.380(5) . ? C8 C9 1.363(5) . ? C9 C10 1.379(5) . ? C11 C12 1.377(5) . ? C11 C16 1.392(5) . ? C12 C14 1.391(5) . ? C13 C14 1.367(6) . ? C13 C15 1.381(6) . ? C15 C16 1.366(5) . ? C17 C18 1.375(5) . ? C17 C22 1.391(5) . ? C18 C19 1.388(5) . ? C19 C20 1.376(6) . ? C20 C21 1.365(6) . ? C21 C22 1.370(5) . ? Ru2 S4 2.3338(8) 3_576 ? Ru2 S4 2.3338(8) . ? Ru2 S3 2.3387(8) . ? Ru2 S3 2.3387(8) 3_576 ? Ru2 P2 2.4528(8) 3_576 ? Ru2 P2 2.4528(8) . ? S3 C23 1.729(3) . ? S4 C25 1.725(3) . ? C23 C25 1.365(4) 3_576 ? C23 C24 1.427(5) . ? C24 N3 1.145(4) . ? C25 C23 1.365(4) 3_576 ? C25 C26 1.427(4) . ? C26 N4 1.147(4) . ? P2 C27 1.832(3) . ? P2 C39 1.832(3) . ? P2 C33 1.851(3) . ? C27 C32 1.383(4) . ? C27 C28 1.393(4) . ? C28 C29 1.379(4) . ? C29 C30 1.371(5) . ? C30 C31 1.354(5) . ? C31 C32 1.389(5) . ? C33 C34 1.375(5) . ? C33 C38 1.387(5) . ? C34 C35 1.389(4) . ? C35 C36 1.360(6) . ? C36 C37 1.376(6) . ? C37 C38 1.385(5) . ? C39 C40 1.383(5) . ? C39 C44 1.392(4) . ? C40 C41 1.383(5) . ? C41 C42 1.376(6) . ? C42 C43 1.355(5) . ? C43 C44 1.384(5) . ? N5 C47A 1.48(2) . ? N5 C45 1.496(7) . ? N5 C45A 1.50(2) . ? N5 C49 1.500(6) . ? N5 C49A 1.50(2) . ? N5 C51 1.504(6) . ? N5 C47 1.528(6) . ? N5 C51A 1.578(15) . ? C45 C46 1.53(2) . ? C47 C48 1.53(2) . ? C49 C50 1.513(14) . ? C51 C52 1.524(11) . ? C45A C46A 1.53(3) . ? C47A C48A 1.54(3) . ? C49A C50A 1.55(3) . ? C51A C52A 1.53(3) . ? 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 S2 Ru1 S2 180.0 3_666 . ? S2 Ru1 S1 86.24(3) 3_666 . ? S2 Ru1 S1 93.76(3) . . ? S2 Ru1 S1 93.76(3) 3_666 3_666 ? S2 Ru1 S1 86.24(3) . 3_666 ? S1 Ru1 S1 180.0 . 3_666 ? S2 Ru1 P1 92.25(3) 3_666 . ? S2 Ru1 P1 87.75(3) . . ? S1 Ru1 P1 88.17(3) . . ? S1 Ru1 P1 91.83(3) 3_666 . ? S2 Ru1 P1 87.75(3) 3_666 3_666 ? S2 Ru1 P1 92.25(3) . 3_666 ? S1 Ru1 P1 91.83(3) . 3_666 ? S1 Ru1 P1 88.17(3) 3_666 3_666 ? P1 Ru1 P1 180.0 . 3_666 ? C1 S1 Ru1 104.00(11) . . ? C3 S2 Ru1 104.18(11) . . ? C3 C1 C2 120.4(3) 3_666 . ? C3 C1 S1 121.6(3) 3_666 . ? C2 C1 S1 118.0(3) . . ? N1 C2 C1 178.6(4) . . ? C1 C3 C4 120.6(3) 3_666 . ? C1 C3 S2 122.6(3) 3_666 . ? C4 C3 S2 116.8(3) . . ? N2 C4 C3 178.1(4) . . ? C5 P1 C11 100.97(14) . . ? C5 P1 C17 104.33(14) . . ? C11 P1 C17 98.98(15) . . ? C5 P1 Ru1 116.10(10) . . ? C11 P1 Ru1 118.71(11) . . ? C17 P1 Ru1 115.18(10) . . ? C10 C5 C6 118.5(3) . . ? C10 C5 P1 121.9(2) . . ? C6 C5 P1 119.6(2) . . ? C7 C6 C5 119.8(3) . . ? C6 C7 C8 121.0(3) . . ? C9 C8 C7 119.4(3) . . ? C8 C9 C10 121.0(4) . . ? C9 C10 C5 120.3(3) . . ? C12 C11 C16 118.2(3) . . ? C12 C11 P1 122.8(2) . . ? C16 C11 P1 119.0(3) . . ? C11 C12 C14 121.0(4) . . ? C14 C13 C15 120.2(4) . . ? C13 C14 C12 119.5(4) . . ? C16 C15 C13 119.9(4) . . ? C15 C16 C11 121.1(4) . . ? C18 C17 C22 118.5(3) . . ? C18 C17 P1 125.3(3) . . ? C22 C17 P1 116.1(2) . . ? C17 C18 C19 120.4(4) . . ? C20 C19 C18 120.2(4) . . ? C21 C20 C19 119.6(4) . . ? C20 C21 C22 120.6(4) . . ? C21 C22 C17 120.7(4) . . ? S4 Ru2 S4 180.0 3_576 . ? S4 Ru2 S3 86.20(3) 3_576 . ? S4 Ru2 S3 93.80(3) . . ? S4 Ru2 S3 93.80(3) 3_576 3_576 ? S4 Ru2 S3 86.20(3) . 3_576 ? S3 Ru2 S3 180.0 . 3_576 ? S4 Ru2 P2 91.94(3) 3_576 3_576 ? S4 Ru2 P2 88.06(3) . 3_576 ? S3 Ru2 P2 87.69(3) . 3_576 ? S3 Ru2 P2 92.31(3) 3_576 3_576 ? S4 Ru2 P2 88.06(3) 3_576 . ? S4 Ru2 P2 91.94(3) . . ? S3 Ru2 P2 92.31(3) . . ? S3 Ru2 P2 87.69(3) 3_576 . ? P2 Ru2 P2 180.0 3_576 . ? C23 S3 Ru2 104.03(11) . . ? C25 S4 Ru2 103.82(11) . . ? C25 C23 C24 120.7(3) 3_576 . ? C25 C23 S3 121.4(2) 3_576 . ? C24 C23 S3 117.9(3) . . ? N3 C24 C23 179.7(4) . . ? C23 C25 C26 121.4(3) 3_576 . ? C23 C25 S4 122.5(2) 3_576 . ? C26 C25 S4 116.1(2) . . ? N4 C26 C25 177.7(4) . . ? C27 P2 C39 104.26(14) . . ? C27 P2 C33 103.00(14) . . ? C39 P2 C33 98.93(15) . . ? C27 P2 Ru2 115.07(10) . . ? C39 P2 Ru2 114.94(10) . . ? C33 P2 Ru2 118.41(11) . . ? C32 C27 C28 118.4(3) . . ? C32 C27 P2 122.2(2) . . ? C28 C27 P2 119.3(2) . . ? C29 C28 C27 120.8(3) . . ? C30 C29 C28 119.9(3) . . ? C31 C30 C29 119.9(4) . . ? C30 C31 C32 121.2(4) . . ? C27 C32 C31 119.7(3) . . ? C34 C33 C38 118.5(3) . . ? C34 C33 P2 122.7(2) . . ? C38 C33 P2 118.7(3) . . ? C33 C34 C35 121.2(4) . . ? C36 C35 C34 119.6(4) . . ? C35 C36 C37 120.4(3) . . ? C36 C37 C38 120.0(4) . . ? C33 C38 C37 120.2(4) . . ? C40 C39 C44 118.1(3) . . ? C40 C39 P2 125.5(3) . . ? C44 C39 P2 116.4(3) . . ? C39 C40 C41 120.5(4) . . ? C42 C41 C40 120.6(4) . . ? C43 C42 C41 119.4(4) . . ? C42 C43 C44 121.0(4) . . ? C43 C44 C39 120.4(3) . . ? C47A N5 C45A 112.3(13) . . ? C45 N5 C49 107.2(5) . . ? C47A N5 C49A 114.1(13) . . ? C45A N5 C49A 109.5(12) . . ? C45 N5 C51 110.8(4) . . ? C49 N5 C51 113.5(5) . . ? C45 N5 C47 111.0(5) . . ? C49 N5 C47 110.1(4) . . ? C51 N5 C47 104.2(4) . . ? C47A N5 C51A 104.7(11) . . ? C45A N5 C51A 109.6(12) . . ? C49A N5 C51A 106.5(11) . . ? N5 C45 C46 116.0(7) . . ? N5 C47 C48 114.0(9) . . ? N5 C49 C50 114.1(7) . . ? N5 C51 C52 113.4(6) . . ? N5 C45A C46A 112.0(32) . . ? N5 C47A C48A 109.9(29) . . ? N5 C49A C50A 118.0(23) . . ? C52A C51A N5 114.2(20) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Ru1 S1 C1 9.57(11) 3_666 . . . ? S2 Ru1 S1 C1 -170.43(11) . . . . ? S1 Ru1 S1 C1 0.0(1000) 3_666 . . . ? P1 Ru1 S1 C1 101.95(11) . . . . ? P1 Ru1 S1 C1 -78.05(11) 3_666 . . . ? S2 Ru1 S2 C3 15.5(1000) 3_666 . . . ? S1 Ru1 S2 C3 -170.07(11) . . . . ? S1 Ru1 S2 C3 9.93(11) 3_666 . . . ? P1 Ru1 S2 C3 -82.05(11) . . . . ? P1 Ru1 S2 C3 97.95(11) 3_666 . . . ? Ru1 S1 C1 C3 -7.7(3) . . . 3_666 ? Ru1 S1 C1 C2 172.9(2) . . . . ? C3 C1 C2 N1 -6.8(189) 3_666 . . . ? S1 C1 C2 N1 172.6(1000) . . . . ? Ru1 S2 C3 C1 -9.1(3) . . . 3_666 ? Ru1 S2 C3 C4 172.8(2) . . . . ? C1 C3 C4 N2 139.4(145) 3_666 . . . ? S2 C3 C4 N2 -42.5(147) . . . . ? S2 Ru1 P1 C5 -114.27(11) 3_666 . . . ? S2 Ru1 P1 C5 65.73(11) . . . . ? S1 Ru1 P1 C5 159.57(11) . . . . ? S1 Ru1 P1 C5 -20.43(11) 3_666 . . . ? P1 Ru1 P1 C5 -59.7(1000) 3_666 . . . ? S2 Ru1 P1 C11 125.07(12) 3_666 . . . ? S2 Ru1 P1 C11 -54.93(12) . . . . ? S1 Ru1 P1 C11 38.90(12) . . . . ? S1 Ru1 P1 C11 -141.10(12) 3_666 . . . ? P1 Ru1 P1 C11 179.7(1000) 3_666 . . . ? S2 Ru1 P1 C17 8.06(12) 3_666 . . . ? S2 Ru1 P1 C17 -171.94(12) . . . . ? S1 Ru1 P1 C17 -78.11(12) . . . . ? S1 Ru1 P1 C17 101.89(12) 3_666 . . . ? P1 Ru1 P1 C17 62.7(1000) 3_666 . . . ? C11 P1 C5 C10 17.7(3) . . . . ? C17 P1 C5 C10 120.0(3) . . . . ? Ru1 P1 C5 C10 -112.1(3) . . . . ? C11 P1 C5 C6 -164.1(3) . . . . ? C17 P1 C5 C6 -61.7(3) . . . . ? Ru1 P1 C5 C6 66.1(3) . . . . ? C10 C5 C6 C7 -1.2(5) . . . . ? P1 C5 C6 C7 -179.5(3) . . . . ? C5 C6 C7 C8 -0.1(5) . . . . ? C6 C7 C8 C9 0.6(6) . . . . ? C7 C8 C9 C10 0.2(6) . . . . ? C8 C9 C10 C5 -1.5(6) . . . . ? C6 C5 C10 C9 1.9(5) . . . . ? P1 C5 C10 C9 -179.8(3) . . . . ? C5 P1 C11 C12 -109.2(3) . . . . ? C17 P1 C11 C12 144.2(3) . . . . ? Ru1 P1 C11 C12 18.9(3) . . . . ? C5 P1 C11 C16 68.3(3) . . . . ? C17 P1 C11 C16 -38.3(3) . . . . ? Ru1 P1 C11 C16 -163.6(2) . . . . ? C16 C11 C12 C14 -0.3(5) . . . . ? P1 C11 C12 C14 177.3(3) . . . . ? C15 C13 C14 C12 0.9(7) . . . . ? C11 C12 C14 C13 -0.5(6) . . . . ? C14 C13 C15 C16 -0.5(7) . . . . ? C13 C15 C16 C11 -0.3(6) . . . . ? C12 C11 C16 C15 0.6(5) . . . . ? P1 C11 C16 C15 -177.0(3) . . . . ? C5 P1 C17 C18 10.2(3) . . . . ? C11 P1 C17 C18 114.0(3) . . . . ? Ru1 P1 C17 C18 -118.2(3) . . . . ? C5 P1 C17 C22 -165.9(3) . . . . ? C11 P1 C17 C22 -62.1(3) . . . . ? Ru1 P1 C17 C22 65.6(3) . . . . ? C22 C17 C18 C19 0.4(6) . . . . ? P1 C17 C18 C19 -175.7(3) . . . . ? C17 C18 C19 C20 -0.1(7) . . . . ? C18 C19 C20 C21 0.1(7) . . . . ? C19 C20 C21 C22 -0.3(7) . . . . ? C20 C21 C22 C17 0.6(6) . . . . ? C18 C17 C22 C21 -0.6(5) . . . . ? P1 C17 C22 C21 175.8(3) . . . . ? S4 Ru2 S3 C23 11.96(11) 3_576 . . . ? S4 Ru2 S3 C23 -168.04(11) . . . . ? S3 Ru2 S3 C23 -100.5(1000) 3_576 . . . ? P2 Ru2 S3 C23 104.06(11) 3_576 . . . ? P2 Ru2 S3 C23 -75.94(11) . . . . ? S4 Ru2 S4 C25 -158.7(1000) 3_576 . . . ? S3 Ru2 S4 C25 -168.23(11) . . . . ? S3 Ru2 S4 C25 11.77(11) 3_576 . . . ? P2 Ru2 S4 C25 -80.68(11) 3_576 . . . ? P2 Ru2 S4 C25 99.32(11) . . . . ? Ru2 S3 C23 C25 -10.4(3) . . . 3_576 ? Ru2 S3 C23 C24 171.0(2) . . . . ? C25 C23 C24 N3 1.6(859) 3_576 . . . ? S3 C23 C24 N3 -179.9(1000) . . . . ? Ru2 S4 C25 C23 -9.9(3) . . . 3_576 ? Ru2 S4 C25 C26 170.4(2) . . . . ? C23 C25 C26 N4 149.8(107) 3_576 . . . ? S4 C25 C26 N4 -30.5(109) . . . . ? S4 Ru2 P2 C27 -71.04(11) 3_576 . . . ? S4 Ru2 P2 C27 108.96(11) . . . . ? S3 Ru2 P2 C27 15.08(11) . . . . ? S3 Ru2 P2 C27 -164.92(11) 3_576 . . . ? P2 Ru2 P2 C27 -74.7(742) 3_576 . . . ? S4 Ru2 P2 C39 167.81(12) 3_576 . . . ? S4 Ru2 P2 C39 -12.19(12) . . . . ? S3 Ru2 P2 C39 -106.08(12) . . . . ? S3 Ru2 P2 C39 73.92(12) 3_576 . . . ? P2 Ru2 P2 C39 164.1(744) 3_576 . . . ? S4 Ru2 P2 C33 51.32(12) 3_576 . . . ? S4 Ru2 P2 C33 -128.68(12) . . . . ? S3 Ru2 P2 C33 137.44(12) . . . . ? S3 Ru2 P2 C33 -42.56(12) 3_576 . . . ? P2 Ru2 P2 C33 47.6(744) 3_576 . . . ? C39 P2 C27 C32 -119.7(3) . . . . ? C33 P2 C27 C32 -16.8(3) . . . . ? Ru2 P2 C27 C32 113.5(3) . . . . ? C39 P2 C27 C28 63.2(3) . . . . ? C33 P2 C27 C28 166.1(3) . . . . ? Ru2 P2 C27 C28 -63.6(3) . . . . ? C32 C27 C28 C29 0.9(5) . . . . ? P2 C27 C28 C29 178.1(3) . . . . ? C27 C28 C29 C30 -0.7(5) . . . . ? C28 C29 C30 C31 0.7(6) . . . . ? C29 C30 C31 C32 -0.9(7) . . . . ? C28 C27 C32 C31 -1.1(5) . . . . ? P2 C27 C32 C31 -178.2(3) . . . . ? C30 C31 C32 C27 1.1(6) . . . . ? C27 P2 C33 C34 115.5(3) . . . . ? C39 P2 C33 C34 -137.5(3) . . . . ? Ru2 P2 C33 C34 -12.7(3) . . . . ? C27 P2 C33 C38 -64.7(3) . . . . ? C39 P2 C33 C38 42.3(3) . . . . ? Ru2 P2 C33 C38 167.0(2) . . . . ? C38 C33 C34 C35 0.4(5) . . . . ? P2 C33 C34 C35 -179.9(3) . . . . ? C33 C34 C35 C36 0.3(6) . . . . ? C34 C35 C36 C37 -1.4(6) . . . . ? C35 C36 C37 C38 1.8(7) . . . . ? C34 C33 C38 C37 0.1(5) . . . . ? P2 C33 C38 C37 -179.7(3) . . . . ? C36 C37 C38 C33 -1.1(6) . . . . ? C27 P2 C39 C40 -12.5(3) . . . . ? C33 P2 C39 C40 -118.4(3) . . . . ? Ru2 P2 C39 C40 114.4(3) . . . . ? C27 P2 C39 C44 165.8(3) . . . . ? C33 P2 C39 C44 59.8(3) . . . . ? Ru2 P2 C39 C44 -67.3(3) . . . . ? C44 C39 C40 C41 -1.3(5) . . . . ? P2 C39 C40 C41 176.9(3) . . . . ? C39 C40 C41 C42 0.9(6) . . . . ? C40 C41 C42 C43 0.0(7) . . . . ? C41 C42 C43 C44 -0.3(7) . . . . ? C42 C43 C44 C39 -0.2(6) . . . . ? C40 C39 C44 C43 1.0(5) . . . . ? P2 C39 C44 C43 -177.4(3) . . . . ? C47A N5 C45 C46 -124.6(13) . . . . ? C45A N5 C45 C46 0.3(12) . . . . ? C49 N5 C45 C46 175.8(7) . . . . ? C49A N5 C45 C46 119.8(218) . . . . ? C51 N5 C45 C46 51.4(9) . . . . ? C47 N5 C45 C46 -63.9(8) . . . . ? C51A N5 C45 C46 119.4(12) . . . . ? C47A N5 C47 C48 -5.1(16) . . . . ? C45 N5 C47 C48 -61.9(12) . . . . ? C45A N5 C47 C48 -124.7(15) . . . . ? C49 N5 C47 C48 56.7(12) . . . . ? C49A N5 C47 C48 117.9(15) . . . . ? C51 N5 C47 C48 178.7(11) . . . . ? C51A N5 C47 C48 58.7(123) . . . . ? C47A N5 C49 C50 115.5(14) . . . . ? C45 N5 C49 C50 172.7(8) . . . . ? C45A N5 C49 C50 -110.9(138) . . . . ? C49A N5 C49 C50 -9.6(14) . . . . ? C51 N5 C49 C50 -64.5(9) . . . . ? C47 N5 C49 C50 51.9(10) . . . . ? C51A N5 C49 C50 -128.0(12) . . . . ? C47A N5 C51 C52 116.3(148) . . . . ? C45 N5 C51 C52 56.7(8) . . . . ? C45A N5 C51 C52 112.4(12) . . . . ? C49 N5 C51 C52 -64.0(7) . . . . ? C49A N5 C51 C52 -120.7(12) . . . . ? C47 N5 C51 C52 176.2(7) . . . . ? C51A N5 C51 C52 -7.1(10) . . . . ? C47A N5 C45A C46A 31.2(30) . . . . ? C45 N5 C45A C46A -23.5(25) . . . . ? C49 N5 C45A C46A -101.3(140) . . . . ? C49A N5 C45A C46A 158.9(27) . . . . ? C51 N5 C45A C46A -149.1(28) . . . . ? C47 N5 C45A C46A 95.6(27) . . . . ? C51A N5 C45A C46A -84.7(27) . . . . ? C45 N5 C47A C48A 105.0(34) . . . . ? C45A N5 C47A C48A 47.7(37) . . . . ? C49 N5 C47A C48A -135.8(35) . . . . ? C49A N5 C47A C48A -77.6(36) . . . . ? C51 N5 C47A C48A 43.9(163) . . . . ? C47 N5 C47A C48A -17.0(32) . . . . ? C51A N5 C47A C48A 166.4(33) . . . . ? C47A N5 C49A C50A -73.3(30) . . . . ? C45 N5 C49A C50A 41.3(233) . . . . ? C45A N5 C49A C50A 159.9(26) . . . . ? C49 N5 C49A C50A -15.4(25) . . . . ? C51 N5 C49A C50A 110.6(28) . . . . ? C47 N5 C49A C50A -135.1(28) . . . . ? C51A N5 C49A C50A 41.6(30) . . . . ? C47A N5 C51A C52A 167.9(23) . . . . ? C45 N5 C51A C52A -133.3(24) . . . . ? C45A N5 C51A C52A -71.5(25) . . . . ? C49 N5 C51A C52A 107.1(23) . . . . ? C49A N5 C51A C52A 46.8(26) . . . . ? C51 N5 C51A C52A -15.8(21) . . . . ? C47 N5 C51A C52A 105.0(122) . . . . ? _refine_diff_density_max 0.441 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.059 data_La0904 _database_code_CSD 174148 _audit_creation_method SHELXL _chemical_name_systematic ; (Et4N){Ru[S2C2(CN)2]2(py)2} ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H30 N7 Ru S4' _chemical_formula_weight 669.88 _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' 'N' 'N' 0.0061 0.0033 '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.268(5) _cell_length_b 14.078(3) _cell_length_c 15.039(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.82(2) _cell_angle_gamma 90.00 _cell_volume 3073.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description block-shaped _exptl_crystal_colour black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method ? _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 0.810 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9307 _exptl_absorpt_correction_T_max 0.9949 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w/2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2814 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2709 _reflns_number_observed 2384 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4-ARGUS (Enraf-Nonius, 1994)' _computing_cell_refinement 'CAD4-ARGUS (Enraf-Nonius, 1994)' _computing_data_reduction ; chi90s (Boyle, 1996), xcad4 (Harms, 1996), SHELXTL-v5 (Siemens, 1994) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1996)' _computing_publication_material 'SHELXTL-v5 (Siemens, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0542P)^2^+5.9272P] 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 'idealized riding models' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2709 _refine_ls_number_parameters 183 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_obs 0.0348 _refine_ls_wR_factor_all 0.1029 _refine_ls_wR_factor_obs 0.0980 _refine_ls_goodness_of_fit_all 1.068 _refine_ls_goodness_of_fit_obs 1.089 _refine_ls_restrained_S_all 1.081 _refine_ls_restrained_S_obs 1.103 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.2500 0.7500 0.0000 0.03858(15) Uani 1 d S . S1 S 0.21774(6) 0.58953(7) 0.00108(7) 0.0481(2) Uani 1 d . . S2 S 0.40536(6) 0.71171(7) 0.06724(7) 0.0461(2) Uani 1 d . . C1 C 0.3254(2) 0.5376(2) 0.0441(2) 0.0450(8) Uani 1 d . . C2 C 0.3279(3) 0.4361(3) 0.0420(3) 0.0519(9) Uani 1 d . . N1 N 0.3285(3) 0.3555(3) 0.0383(3) 0.0764(11) Uani 1 d . . C3 C 0.4045(2) 0.5891(2) 0.0739(2) 0.0448(8) Uani 1 d . . C4 C 0.4915(3) 0.5414(3) 0.1124(3) 0.0547(9) Uani 1 d . . N2 N 0.5614(3) 0.5050(3) 0.1443(4) 0.0857(13) Uani 1 d . . N3 N 0.2629(2) 0.7653(2) 0.1466(2) 0.0467(7) Uani 1 d . . C5 C 0.2256(3) 0.8385(3) 0.1721(3) 0.0551(9) Uani 1 d . . H5 H 0.1920(3) 0.8830(3) 0.1236(3) 0.066 Uiso 1 calc R . C6 C 0.2348(3) 0.8510(3) 0.2669(3) 0.0714(12) Uani 1 d . . H6 H 0.2083(3) 0.9035(3) 0.2815(3) 0.086 Uiso 1 calc R . C7 C 0.2831(3) 0.7861(4) 0.3395(3) 0.0775(14) Uani 1 d . . H7 H 0.2902(3) 0.7936(4) 0.4040(3) 0.093 Uiso 1 calc R . C8 C 0.3204(3) 0.7103(4) 0.3145(3) 0.0707(12) Uani 1 d . . H8 H 0.3528(3) 0.6644(4) 0.3620(3) 0.085 Uiso 1 calc R . C9 C 0.3101(3) 0.7018(3) 0.2194(3) 0.0564(9) Uani 1 d . . H9 H 0.3367(3) 0.6499(3) 0.2040(3) 0.068 Uiso 1 calc R . N4 N 0.5000 0.8995(3) 0.7500 0.0691(13) Uani 1 d SDU . C11 C 0.5747(5) 0.9618(7) 0.7469(10) 0.066(4) Uiso 0.336(11) d PDU 1 H11A H 0.6091(5) 0.9244(7) 0.7209(10) 0.079 Uiso 0.336(11) calc PR 1 H11B H 0.6169(5) 0.9795(7) 0.8147(10) 0.079 Uiso 0.336(11) calc PR 1 C12 C 0.5416(15) 1.0534(12) 0.6843(16) 0.133(9) Uiso 0.336(11) d PDU 1 H12A H 0.5120(15) 1.0374(12) 0.6148(16) 0.200 Uiso 0.336(11) calc PR 1 H12B H 0.5934(15) 1.0939(12) 0.6980(16) 0.200 Uiso 0.336(11) calc PR 1 H12C H 0.4987(15) 1.0860(12) 0.7012(16) 0.200 Uiso 0.336(11) calc PR 1 C13 C 0.5412(9) 0.8398(8) 0.8415(4) 0.107(6) Uiso 0.336(11) d PDU 1 H13A H 0.5604(9) 0.8800(8) 0.9000(4) 0.128 Uiso 0.336(11) calc PR 1 H13B H 0.5952(9) 0.8074(8) 0.8451(4) 0.128 Uiso 0.336(11) calc PR 1 C14 C 0.4713(17) 0.7666(15) 0.8407(22) 0.149(11) Uiso 0.336(11) d PDU 1 H14A H 0.4973(17) 0.7317(15) 0.9021(22) 0.224 Uiso 0.336(11) calc PR 1 H14B H 0.4563(17) 0.7236(15) 0.7860(22) 0.224 Uiso 0.336(11) calc PR 1 H14C H 0.4165(17) 0.7986(15) 0.8334(22) 0.224 Uiso 0.336(11) calc PR 1 C15 C 0.5597(7) 0.9825(7) 0.7692(9) 0.070(4) Uiso 0.332(5) d PDU 2 H15A H 0.5890(7) 0.9817(7) 0.7256(9) 0.084 Uiso 0.332(5) calc PR 2 H15B H 0.6074(7) 0.9817(7) 0.8377(9) 0.084 Uiso 0.332(5) calc PR 2 C16 C 0.5000 1.0724(12) 0.7500 0.218(11) Uiso 0.664(11) d SPDU 2 H16A H 0.5360 1.1274(12) 0.7529 0.327 Uiso 0.332(5) calc PR 2 H16B H 0.4786 1.0774(12) 0.7998 0.327 Uiso 0.332(5) calc PR 2 H16C H 0.4481 1.0684(12) 0.6853 0.327 Uiso 0.332(5) calc PR 2 C17 C 0.5494(9) 0.8118(7) 0.7968(10) 0.103(5) Uiso 0.332(5) d PDU . H17A H 0.5620(9) 0.8124(7) 0.8663(10) 0.123 Uiso 0.332(5) calc PR . H17B H 0.6083(9) 0.8124(7) 0.7950(10) 0.123 Uiso 0.332(5) calc PR . C18 C 0.5000 0.7182(12) 0.7500 0.202(10) Uiso 0.664(11) d SPDU . H18A H 0.4470 0.7110(12) 0.7618 0.304 Uiso 0.332(5) calc PR . H18B H 0.5413 0.6659(12) 0.7795 0.304 Uiso 0.332(5) calc PR . H18C H 0.4808 0.7193(12) 0.6796 0.304 Uiso 0.332(5) calc PR . C19 C 0.4199(8) 0.9178(13) 0.7730(11) 0.133(8) Uiso 0.332(5) d PDU 3 H19A H 0.3879(8) 0.8583(13) 0.7674(11) 0.160 Uiso 0.332(5) calc PR 3 H19B H 0.3772(8) 0.9606(13) 0.7230(11) 0.160 Uiso 0.332(5) calc PR 3 C20 C 0.4465(19) 0.9601(20) 0.8761(14) 0.161(10) Uiso 0.332(5) d PDU 3 H20A H 0.3921(19) 0.9682(20) 0.8851(14) 0.241 Uiso 0.332(5) calc PR 3 H20B H 0.4756(19) 1.0206(20) 0.8814(14) 0.241 Uiso 0.332(5) calc PR 3 H20C H 0.4883(19) 0.9180(20) 0.9263(14) 0.241 Uiso 0.332(5) calc PR 3 C21 C 0.4497(7) 0.8803(9) 0.6342(5) 0.060(3) Uiso 0.332(5) d PDU 3 H21A H 0.4024(7) 0.8328(9) 0.6207(5) 0.072 Uiso 0.332(5) calc PR 3 H21B H 0.4192(7) 0.9383(9) 0.6008(5) 0.072 Uiso 0.332(5) calc PR 3 C22 C 0.5117(13) 0.8470(15) 0.5890(15) 0.112(6) Uiso 0.332(5) d PDU 3 H22A H 0.4807(13) 0.8561(15) 0.5182(15) 0.167 Uiso 0.332(5) calc PR 3 H22B H 0.5256(13) 0.7808(15) 0.6036(15) 0.167 Uiso 0.332(5) calc PR 3 H22C H 0.5678(13) 0.8830(15) 0.6169(15) 0.167 Uiso 0.332(5) calc PR 3 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 0.0357(2) 0.0430(2) 0.0368(2) -0.00137(15) 0.0161(2) 0.00118(14) S1 0.0425(5) 0.0489(5) 0.0532(5) -0.0041(4) 0.0217(4) -0.0047(4) S2 0.0372(4) 0.0449(5) 0.0534(5) -0.0015(4) 0.0180(4) -0.0004(3) C1 0.049(2) 0.047(2) 0.041(2) -0.0021(15) 0.022(2) -0.0013(15) C2 0.061(2) 0.051(2) 0.052(2) 0.000(2) 0.033(2) -0.002(2) N1 0.108(3) 0.051(2) 0.092(3) -0.004(2) 0.065(3) -0.007(2) C3 0.044(2) 0.046(2) 0.044(2) 0.0022(14) 0.020(2) 0.0037(15) C4 0.050(2) 0.046(2) 0.064(2) 0.002(2) 0.023(2) 0.005(2) N2 0.055(2) 0.064(2) 0.122(4) 0.010(2) 0.026(2) 0.015(2) N3 0.045(2) 0.055(2) 0.042(2) 0.0000(13) 0.0204(13) 0.0057(13) C5 0.055(2) 0.064(2) 0.047(2) 0.006(2) 0.024(2) 0.017(2) C6 0.079(3) 0.087(3) 0.052(2) 0.002(2) 0.034(2) 0.031(2) C7 0.086(3) 0.107(4) 0.044(2) 0.011(2) 0.033(2) 0.040(3) C8 0.077(3) 0.090(3) 0.050(2) 0.020(2) 0.034(2) 0.035(3) C9 0.062(2) 0.062(2) 0.047(2) 0.007(2) 0.026(2) 0.017(2) N4 0.057(3) 0.066(3) 0.076(3) 0.000 0.023(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N3 2.130(3) . ? Ru N3 2.130(3) 7_565 ? Ru S1 2.3209(10) 7_565 ? Ru S1 2.3209(10) . ? Ru S2 2.3227(11) . ? Ru S2 2.3227(11) 7_565 ? S1 C1 1.732(4) . ? S2 C3 1.730(4) . ? C1 C3 1.364(5) . ? C1 C2 1.430(5) . ? C2 N1 1.136(5) . ? C3 C4 1.431(5) . ? C4 N2 1.137(5) . ? N3 C5 1.337(4) . ? N3 C9 1.352(5) . ? C5 C6 1.375(6) . ? C5 H5 0.93 . ? C6 C7 1.367(6) . ? C6 H6 0.93 . ? C7 C8 1.363(6) . ? C7 H7 0.93 . ? C8 C9 1.368(5) . ? C8 H8 0.93 . ? C9 H9 0.93 . ? N4 C15 1.462(7) . ? N4 C15 1.462(7) 2_656 ? N4 C17 1.468(7) 2_656 ? N4 C17 1.468(7) . ? N4 C13 1.490(6) 2_656 ? N4 C13 1.490(6) . ? N4 C19 1.512(7) 2_656 ? N4 C19 1.512(7) . ? N4 C11 1.516(6) . ? N4 C11 1.516(6) 2_656 ? N4 C21 1.578(7) . ? N4 C21 1.578(7) 2_656 ? C11 C12 1.543(10) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C13 C14 1.531(10) . ? C13 H13A 0.97 . ? C13 H13B 0.97 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 C16 1.542(9) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? C17 C18 1.539(10) . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C18 H18A 0.96 . ? C18 H18B 0.96 . ? C18 H18C 0.96 . ? C19 C20 1.530(10) . ? C19 H19A 0.97 . ? C19 H19B 0.97 . ? C20 H20A 0.96 . ? C20 H20B 0.96 . ? C20 H20C 0.96 . ? C21 C22 1.521(9) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 H22A 0.96 . ? C22 H22B 0.96 . ? C22 H22C 0.96 . ? 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 N3 Ru N3 180.0 . 7_565 ? N3 Ru S1 89.54(8) . 7_565 ? N3 Ru S1 90.46(8) 7_565 7_565 ? N3 Ru S1 90.46(8) . . ? N3 Ru S1 89.54(8) 7_565 . ? S1 Ru S1 180.0 7_565 . ? N3 Ru S2 89.61(9) . . ? N3 Ru S2 90.39(8) 7_565 . ? S1 Ru S2 91.37(3) 7_565 . ? S1 Ru S2 88.63(3) . . ? N3 Ru S2 90.39(9) . 7_565 ? N3 Ru S2 89.61(8) 7_565 7_565 ? S1 Ru S2 88.63(3) 7_565 7_565 ? S1 Ru S2 91.37(3) . 7_565 ? S2 Ru S2 180.0 . 7_565 ? C1 S1 Ru 102.70(12) . . ? C3 S2 Ru 102.80(12) . . ? C3 C1 C2 120.4(3) . . ? C3 C1 S1 122.9(3) . . ? C2 C1 S1 116.6(3) . . ? N1 C2 C1 178.5(5) . . ? C1 C3 C4 119.9(3) . . ? C1 C3 S2 122.8(3) . . ? C4 C3 S2 117.3(3) . . ? N2 C4 C3 178.7(4) . . ? C5 N3 C9 116.3(3) . . ? C5 N3 Ru 122.0(2) . . ? C9 N3 Ru 121.7(2) . . ? N3 C5 C6 123.0(4) . . ? N3 C5 H5 118.5(2) . . ? C6 C5 H5 118.5(2) . . ? C7 C6 C5 119.8(4) . . ? C7 C6 H6 120.1(3) . . ? C5 C6 H6 120.1(2) . . ? C8 C7 C6 118.1(4) . . ? C8 C7 H7 121.0(2) . . ? C6 C7 H7 121.0(3) . . ? C7 C8 C9 119.8(4) . . ? C7 C8 H8 120.1(3) . . ? C9 C8 H8 120.1(3) . . ? N3 C9 C8 123.1(4) . . ? N3 C9 H9 118.5(2) . . ? C8 C9 H9 118.5(3) . . ? C15 N4 C17 113.9(6) 2_656 2_656 ? C15 N4 C17 113.9(6) . . ? C13 N4 C13 111.3(8) 2_656 . ? C17 N4 C19 112.0(7) 2_656 2_656 ? C17 N4 C19 112.0(7) . . ? C13 N4 C11 109.3(4) 2_656 . ? C13 N4 C11 108.8(4) . . ? C13 N4 C11 108.8(4) 2_656 2_656 ? C13 N4 C11 109.3(4) . 2_656 ? C11 N4 C11 109.3(7) . 2_656 ? C17 N4 C21 106.5(6) . . ? C19 N4 C21 102.1(6) . . ? C17 N4 C21 106.5(6) 2_656 2_656 ? C19 N4 C21 102.1(6) 2_656 2_656 ? N4 C11 C12 116.0(10) . . ? N4 C11 H11A 108.3(4) . . ? C12 C11 H11A 108.3(9) . . ? N4 C11 H11B 108.3(5) . . ? C12 C11 H11B 108.3(10) . . ? H11A C11 H11B 107.4 . . ? C11 C12 H12A 109.5(10) . . ? C11 C12 H12B 109.5(9) . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5(9) . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C14 110.4(13) . . ? N4 C13 H13A 109.6(4) . . ? C14 C13 H13A 109.6(11) . . ? N4 C13 H13B 109.6(5) . . ? C14 C13 H13B 109.6(11) . . ? H13A C13 H13B 108.1 . . ? C13 C14 H14A 109.5(11) . . ? C13 C14 H14B 109.5(11) . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5(11) . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N4 C15 C16 108.2(10) . . ? N4 C15 H15A 110.1(5) . . ? C16 C15 H15A 110.1(5) . . ? N4 C15 H15B 110.1(5) . . ? C16 C15 H15B 110.1(5) . . ? H15A C15 H15B 108.4 . . ? C15 C16 H16A 109.5(5) . . ? C15 C16 H16B 109.5(5) . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5(5) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 C18 116.2(10) . . ? N4 C17 H17A 108.2(6) . . ? C18 C17 H17A 108.2(6) . . ? N4 C17 H17B 108.2(6) . . ? C18 C17 H17B 108.2(6) . . ? H17A C17 H17B 107.4 . . ? C17 C18 H18A 109.5(6) . . ? C17 C18 H18B 109.5(6) . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5(6) . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 C20 114.8(14) . . ? N4 C19 H19A 108.6(7) . . ? C20 C19 H19A 108.6(13) . . ? N4 C19 H19B 108.6(7) . . ? C20 C19 H19B 108.6(13) . . ? H19A C19 H19B 107.5 . . ? C19 C20 H20A 109.5(11) . . ? C19 C20 H20B 109.5(13) . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5(13) . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N4 115.3(10) . . ? C22 C21 H21A 108.4(9) . . ? N4 C21 H21A 108.4(4) . . ? C22 C21 H21B 108.4(9) . . ? N4 C21 H21B 108.4(5) . . ? H21A C21 H21B 107.5 . . ? C21 C22 H22A 109.5(9) . . ? C21 C22 H22B 109.5(9) . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5(9) . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _refine_diff_density_max 0.647 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.070