# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wen-Ren Li' _publ_contact_author_email ch01@ncu.edu.tw loop_ _publ_author_name 'Wen-Ren Li' 'Chaochin Su' data_100730lts _database_code_depnum_ccdc_archive 'CCDC 789379' #TrackingRef 'web_deposit_cif_file_0_Wei-ChunChang_1281924352.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H25 F2 N7 O4 Ru S2' _chemical_formula_weight 774.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'C 1 c 1' _symmetry_space_group_name_hall 'C -2yc' 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' _cell_length_a 15.827(2) _cell_length_b 17.404(3) _cell_length_c 15.344(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.473(3) _cell_angle_gamma 90.00 _cell_volume 3984.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9951 _cell_measurement_theta_min 2.5486 _cell_measurement_theta_max 26.3953 _exptl_crystal_description Needle _exptl_crystal_colour Black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5985 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 26959 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.46 _reflns_number_total 7550 _reflns_number_gt 6257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.34A (Bruker AXS, 2006)' _computing_data_reduction 'SAINT V7.34A (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material SHELXTL _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^)+(0.0433P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 7550 _refine_ls_number_parameters 436 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.511183(18) 0.468725(17) 0.745045(19) 0.01603(8) Uani 1 1 d . . . S1 S 0.35074(9) 0.26521(8) 0.83786(10) 0.0374(3) Uani 1 1 d . . . S2 S 0.62174(12) 0.24828(8) 0.62868(11) 0.0497(4) Uani 1 1 d . . . N1 N 0.4454(3) 0.3864(3) 0.7920(3) 0.0198(11) Uani 1 1 d . . . N2 N 0.5778(3) 0.3813(3) 0.7058(3) 0.0183(10) Uani 1 1 d . . . N3 N 0.4472(3) 0.5554(3) 0.7910(3) 0.0214(11) Uani 1 1 d . . . N4 N 0.5735(3) 0.5495(2) 0.9181(3) 0.0245(9) Uani 1 1 d . . . N5 N 0.6790(2) 0.4681(2) 0.9304(2) 0.0225(8) Uani 1 1 d . . . N6 N 0.5612(3) 0.5507(3) 0.6795(3) 0.0177(10) Uani 1 1 d . . . N7 N 0.4146(3) 0.4656(2) 0.6114(3) 0.0188(10) Uani 1 1 d . . . O1 O 0.6903(2) 0.7757(2) 0.5552(2) 0.0412(9) Uani 1 1 d . . . O2 O 0.5865(2) 0.72188(17) 0.4330(2) 0.0309(7) Uani 1 1 d . . . O3 O 0.1515(2) 0.44988(19) 0.3176(3) 0.0306(8) Uani 1 1 d . . . O4 O 0.23548(19) 0.54562(17) 0.2929(2) 0.0288(7) Uani 1 1 d . . . C1 C 0.4043(3) 0.3352(3) 0.8083(4) 0.0210(12) Uani 1 1 d . . . C2 C 0.5952(3) 0.3267(3) 0.6760(4) 0.0227(12) Uani 1 1 d . . . C3 C 0.3676(3) 0.5884(3) 0.7434(4) 0.0317(13) Uani 1 1 d . . . H3 H 0.3337 0.5683 0.6845 0.038 Uiso 1 1 calc R . . C4 C 0.3338(3) 0.6512(3) 0.7785(5) 0.0452(16) Uani 1 1 d . . . H4 H 0.2773 0.6723 0.7436 0.054 Uiso 1 1 calc R . . C5 C 0.3814(4) 0.6824(3) 0.8623(5) 0.0471(17) Uani 1 1 d . . . C6 C 0.4624(3) 0.6493(3) 0.9113(4) 0.0393(14) Uani 1 1 d . . . H6 H 0.4974 0.6691 0.9699 0.047 Uiso 1 1 calc R . . C7 C 0.4922(3) 0.5865(3) 0.8738(4) 0.0242(11) Uani 1 1 d . . . C8 C 0.5987(3) 0.4902(3) 0.8712(4) 0.0207(11) Uani 1 1 d . . . C9 C 0.6389(3) 0.5646(3) 1.0025(4) 0.0372(13) Uani 1 1 d . . . H9 H 0.6371 0.6032 1.0456 0.045 Uiso 1 1 calc R . . C10 C 0.7041(3) 0.5147(3) 1.0112(4) 0.0354(13) Uani 1 1 d . . . H10 H 0.7581 0.5106 1.0623 0.042 Uiso 1 1 calc R . . C11 C 0.7378(3) 0.4107(3) 0.9119(3) 0.0265(10) Uani 1 1 d . . . H11A H 0.7024 0.3781 0.8595 0.032 Uiso 1 1 calc R . . H11B H 0.7617 0.3772 0.9668 0.032 Uiso 1 1 calc R . . C12 C 0.8150(3) 0.4454(2) 0.8890(3) 0.0244(10) Uani 1 1 d . . . C13 C 0.8918(3) 0.4680(3) 0.9583(4) 0.0450(13) Uani 1 1 d . . . H13 H 0.8978 0.4596 1.0213 0.054 Uiso 1 1 calc R . . C14 C 0.9600(4) 0.5029(4) 0.9354(4) 0.0537(16) Uani 1 1 d . . . C15 C 0.9563(3) 0.5145(3) 0.8463(4) 0.0430(14) Uani 1 1 d . . . H15 H 1.0046 0.5366 0.8311 0.052 Uiso 1 1 calc R . . C16 C 0.8784(4) 0.4922(4) 0.7805(4) 0.0453(14) Uani 1 1 d . . . C17 C 0.8082(3) 0.4582(3) 0.7981(4) 0.0380(13) Uani 1 1 d . . . H17 H 0.7559 0.4437 0.7490 0.046 Uiso 1 1 calc R . . C18 C 0.3472(4) 0.7524(3) 0.8979(6) 0.071(2) Uani 1 1 d . . . H18A H 0.2947 0.7729 0.8492 0.107 Uiso 1 1 calc R . . H18B H 0.3943 0.7916 0.9159 0.107 Uiso 1 1 calc R . . H18C H 0.3302 0.7383 0.9517 0.107 Uiso 1 1 calc R . . C19 C 0.6350(3) 0.5924(3) 0.7150(3) 0.0213(11) Uani 1 1 d . . . H19 H 0.6719 0.5821 0.7768 0.026 Uiso 1 1 calc R . . C20 C 0.6618(3) 0.6503(3) 0.6672(3) 0.0264(11) Uani 1 1 d . . . H20 H 0.7139 0.6800 0.6966 0.032 Uiso 1 1 calc R . . C21 C 0.6103(3) 0.6635(3) 0.5755(3) 0.0204(9) Uani 1 1 d . . . C22 C 0.5340(3) 0.6205(3) 0.5368(3) 0.0199(9) Uani 1 1 d . . . H22 H 0.4979 0.6291 0.4744 0.024 Uiso 1 1 calc R . . C23 C 0.5094(3) 0.5648(3) 0.5883(3) 0.0183(10) Uani 1 1 d . . . C24 C 0.4281(3) 0.5184(2) 0.5519(3) 0.0190(11) Uani 1 1 d . . . C25 C 0.3654(3) 0.5277(2) 0.4641(3) 0.0178(9) Uani 1 1 d . . . H25 H 0.3745 0.5655 0.4234 0.021 Uiso 1 1 calc R . . C26 C 0.2886(3) 0.4810(2) 0.4357(3) 0.0201(9) Uani 1 1 d . . . C27 C 0.2774(3) 0.4263(3) 0.4962(3) 0.0258(10) Uani 1 1 d . . . H27 H 0.2264 0.3936 0.4790 0.031 Uiso 1 1 calc R . . C28 C 0.3427(3) 0.4204(3) 0.5832(3) 0.0276(11) Uani 1 1 d . . . H28 H 0.3357 0.3821 0.6244 0.033 Uiso 1 1 calc R . . C29 C 0.6347(3) 0.7272(2) 0.5220(3) 0.0208(9) Uani 1 1 d . . . C30 C 0.5945(3) 0.7840(3) 0.3732(3) 0.0353(12) Uani 1 1 d . . . H30A H 0.5841 0.8332 0.3989 0.053 Uiso 1 1 calc R . . H30B H 0.5501 0.7770 0.3115 0.053 Uiso 1 1 calc R . . H30C H 0.6548 0.7836 0.3687 0.053 Uiso 1 1 calc R . . C31 C 0.2172(3) 0.4890(2) 0.3426(3) 0.0232(10) Uani 1 1 d . . . C32 C 0.1688(3) 0.5576(3) 0.2036(4) 0.0395(13) Uani 1 1 d U . . H32A H 0.1679 0.5135 0.1637 0.059 Uiso 1 1 calc R . . H32B H 0.1832 0.6043 0.1757 0.059 Uiso 1 1 calc R . . H32C H 0.1098 0.5634 0.2107 0.059 Uiso 1 1 calc R . . F1 F 1.0359(2) 0.5248(3) 1.0033(3) 0.1002(19) Uani 1 1 d . . . F2 F 0.8741(2) 0.5037(3) 0.6917(2) 0.0917(16) Uani 1 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 0.01718(13) 0.01769(14) 0.00906(14) 0.0015(2) -0.00117(10) -0.00101(19) S1 0.0413(7) 0.0350(7) 0.0283(8) 0.0055(6) 0.0014(6) -0.0163(6) S2 0.0820(11) 0.0347(8) 0.0287(8) -0.0003(6) 0.0137(8) 0.0278(8) N1 0.022(2) 0.021(3) 0.012(2) -0.0020(19) -0.0012(18) 0.0056(19) N2 0.021(2) 0.023(3) 0.010(2) -0.0022(19) 0.0044(18) 0.0002(18) N3 0.015(2) 0.018(2) 0.030(3) -0.0028(19) 0.0051(18) -0.0009(17) N4 0.026(2) 0.028(2) 0.017(2) -0.0086(18) 0.0037(18) 0.0005(18) N5 0.0209(17) 0.029(2) 0.0136(19) -0.0045(17) 0.0005(15) 0.0017(16) N6 0.021(2) 0.020(2) 0.011(2) 0.0016(17) 0.0024(17) 0.0010(16) N7 0.020(2) 0.023(2) 0.009(2) 0.0065(16) -0.0015(17) -0.0059(16) O1 0.050(2) 0.044(2) 0.0183(19) 0.0073(16) -0.0043(16) -0.0312(17) O2 0.0441(18) 0.0263(17) 0.0126(17) 0.0047(13) -0.0035(14) -0.0151(14) O3 0.0247(17) 0.041(2) 0.020(2) 0.0033(15) -0.0003(14) -0.0098(14) O4 0.0267(15) 0.0380(19) 0.0126(17) 0.0075(13) -0.0058(13) -0.0059(13) C1 0.019(2) 0.028(3) 0.013(3) -0.004(2) 0.0010(19) 0.002(2) C2 0.029(3) 0.027(3) 0.009(3) 0.001(2) 0.002(2) -0.003(2) C3 0.025(2) 0.031(3) 0.032(4) 0.018(2) 0.001(2) 0.007(2) C4 0.023(3) 0.025(3) 0.082(5) 0.011(3) 0.011(3) 0.010(2) C5 0.043(3) 0.026(3) 0.079(5) -0.012(3) 0.029(3) -0.001(3) C6 0.034(3) 0.035(3) 0.053(4) -0.018(3) 0.020(3) -0.013(2) C7 0.018(2) 0.023(3) 0.028(3) -0.003(2) 0.004(2) 0.0016(19) C8 0.016(2) 0.020(2) 0.023(3) 0.005(2) 0.002(2) 0.0034(19) C9 0.036(3) 0.045(3) 0.020(3) -0.018(3) -0.005(2) -0.002(3) C10 0.027(3) 0.049(4) 0.021(3) -0.018(2) -0.003(2) 0.002(2) C11 0.025(2) 0.024(2) 0.024(3) 0.005(2) -0.001(2) 0.0023(19) C12 0.024(2) 0.024(2) 0.019(3) -0.0005(18) -0.0010(18) 0.0058(17) C13 0.028(2) 0.081(4) 0.021(3) -0.001(3) 0.002(2) -0.009(3) C14 0.036(3) 0.093(4) 0.027(4) -0.019(3) 0.005(3) -0.020(3) C15 0.030(3) 0.062(4) 0.036(3) -0.005(3) 0.010(2) -0.013(2) C16 0.035(3) 0.074(4) 0.022(3) 0.006(3) 0.003(2) -0.008(3) C17 0.024(2) 0.058(4) 0.030(3) -0.002(3) 0.006(2) -0.007(2) C18 0.052(4) 0.042(4) 0.125(7) -0.018(4) 0.035(4) 0.007(3) C19 0.020(2) 0.032(3) 0.006(2) 0.0018(19) -0.0033(19) -0.005(2) C20 0.016(2) 0.037(3) 0.017(3) -0.003(2) -0.0068(19) -0.010(2) C21 0.023(2) 0.025(2) 0.011(2) -0.0029(18) 0.0023(18) -0.0012(19) C22 0.021(2) 0.027(2) 0.006(2) 0.0034(18) -0.0025(17) -0.0007(18) C23 0.012(2) 0.021(2) 0.016(3) -0.0034(19) -0.0045(18) -0.0016(17) C24 0.015(2) 0.017(2) 0.021(3) 0.0044(19) 0.0011(19) -0.0023(17) C25 0.020(2) 0.018(2) 0.012(2) 0.0017(18) 0.0008(18) -0.0032(18) C26 0.019(2) 0.016(2) 0.021(2) 0.0017(18) 0.0003(18) -0.0062(16) C27 0.024(2) 0.032(3) 0.014(2) 0.0032(19) -0.0037(18) -0.0076(19) C28 0.024(2) 0.034(3) 0.017(3) 0.007(2) -0.0042(19) -0.010(2) C29 0.022(2) 0.022(2) 0.014(2) 0.0003(18) 0.0017(18) -0.0021(18) C30 0.044(3) 0.035(3) 0.020(3) 0.005(2) 0.000(2) -0.016(2) C31 0.019(2) 0.028(3) 0.018(2) 0.0021(18) -0.0006(18) -0.0056(17) C32 0.031(3) 0.056(3) 0.018(3) 0.019(2) -0.011(2) 0.003(2) F1 0.049(2) 0.210(6) 0.033(2) -0.033(3) 0.0020(19) -0.059(3) F2 0.050(2) 0.193(5) 0.022(2) 0.013(3) -0.0009(16) -0.055(3) _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 C8 2.004(5) . ? Ru1 N1 2.039(5) . ? Ru1 N6 2.051(5) . ? Ru1 N2 2.053(5) . ? Ru1 N3 2.068(5) . ? Ru1 N7 2.111(4) . ? S1 C1 1.633(6) . ? S2 C2 1.665(6) . ? N1 C1 1.177(6) . ? N2 C2 1.127(6) . ? N3 C7 1.346(7) . ? N3 C3 1.355(6) . ? N4 C9 1.387(6) . ? N4 C8 1.391(7) . ? N4 C7 1.396(6) . ? N5 C8 1.348(6) . ? N5 C10 1.423(6) . ? N5 C11 1.457(5) . ? N6 C19 1.328(6) . ? N6 C23 1.387(6) . ? N7 C28 1.331(6) . ? N7 C24 1.361(6) . ? O1 C29 1.204(5) . ? O2 C29 1.327(5) . ? O2 C30 1.451(5) . ? O3 C31 1.193(5) . ? O4 C31 1.336(5) . ? O4 C32 1.439(5) . ? C3 C4 1.401(8) . ? C3 H3 0.9500 . ? C4 C5 1.369(9) . ? C4 H4 0.9500 . ? C5 C6 1.379(8) . ? C5 C18 1.507(8) . ? C6 C7 1.388(7) . ? C6 H6 0.9500 . ? C9 C10 1.321(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.506(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.378(6) . ? C12 C17 1.381(7) . ? C13 C14 1.382(8) . ? C13 H13 0.9500 . ? C14 F1 1.356(7) . ? C14 C15 1.364(8) . ? C15 C16 1.364(7) . ? C15 H15 0.9500 . ? C16 F2 1.356(7) . ? C16 C17 1.363(7) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.393(7) . ? C19 H19 0.9500 . ? C20 C21 1.390(6) . ? C20 H20 0.9500 . ? C21 C22 1.376(6) . ? C21 C29 1.504(6) . ? C22 C23 1.386(6) . ? C22 H22 0.9500 . ? C23 C24 1.462(6) . ? C24 C25 1.391(7) . ? C25 C26 1.405(6) . ? C25 H25 0.9500 . ? C26 C27 1.383(6) . ? C26 C31 1.504(6) . ? C27 C28 1.392(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? 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 C8 Ru1 N1 93.43(19) . . ? C8 Ru1 N6 95.1(2) . . ? N1 Ru1 N6 171.29(17) . . ? C8 Ru1 N2 99.44(18) . . ? N1 Ru1 N2 87.44(11) . . ? N6 Ru1 N2 92.98(19) . . ? C8 Ru1 N3 78.1(2) . . ? N1 Ru1 N3 91.54(19) . . ? N6 Ru1 N3 88.41(12) . . ? N2 Ru1 N3 177.3(2) . . ? C8 Ru1 N7 170.62(19) . . ? N1 Ru1 N7 92.02(16) . . ? N6 Ru1 N7 79.30(16) . . ? N2 Ru1 N7 88.43(16) . . ? N3 Ru1 N7 94.09(17) . . ? C1 N1 Ru1 171.8(4) . . ? C2 N2 Ru1 164.3(4) . . ? C7 N3 C3 116.3(5) . . ? C7 N3 Ru1 116.7(3) . . ? C3 N3 Ru1 126.8(4) . . ? C9 N4 C8 111.7(4) . . ? C9 N4 C7 130.3(4) . . ? C8 N4 C7 117.9(4) . . ? C8 N5 C10 110.6(4) . . ? C8 N5 C11 125.7(4) . . ? C10 N5 C11 123.4(3) . . ? C19 N6 C23 117.4(4) . . ? C19 N6 Ru1 127.6(4) . . ? C23 N6 Ru1 115.0(3) . . ? C28 N7 C24 119.3(4) . . ? C28 N7 Ru1 126.5(3) . . ? C24 N7 Ru1 114.1(3) . . ? C29 O2 C30 117.2(3) . . ? C31 O4 C32 114.9(3) . . ? N1 C1 S1 176.4(5) . . ? N2 C2 S2 177.7(5) . . ? N3 C3 C4 121.9(5) . . ? N3 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C5 C4 C3 120.7(5) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 117.8(5) . . ? C4 C5 C18 120.7(6) . . ? C6 C5 C18 121.5(6) . . ? C5 C6 C7 119.1(5) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? N3 C7 C6 124.2(5) . . ? N3 C7 N4 112.7(4) . . ? C6 C7 N4 123.1(5) . . ? N5 C8 N4 103.4(4) . . ? N5 C8 Ru1 142.3(4) . . ? N4 C8 Ru1 114.4(3) . . ? C10 C9 N4 106.6(5) . . ? C10 C9 H9 126.7 . . ? N4 C9 H9 126.7 . . ? C9 C10 N5 107.7(4) . . ? C9 C10 H10 126.1 . . ? N5 C10 H10 126.1 . . ? N5 C11 C12 113.0(3) . . ? N5 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N5 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C17 119.0(4) . . ? C13 C12 C11 120.7(4) . . ? C17 C12 C11 120.3(4) . . ? C12 C13 C14 119.4(5) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? F1 C14 C15 117.3(5) . . ? F1 C14 C13 119.6(6) . . ? C15 C14 C13 123.0(5) . . ? C16 C15 C14 115.2(5) . . ? C16 C15 H15 122.4 . . ? C14 C15 H15 122.4 . . ? F2 C16 C17 119.5(5) . . ? F2 C16 C15 115.6(5) . . ? C17 C16 C15 124.9(5) . . ? C16 C17 C12 118.4(5) . . ? C16 C17 H17 120.8 . . ? C12 C17 H17 120.8 . . ? C5 C18 H18A 109.5 . . ? C5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C19 C20 124.1(4) . . ? N6 C19 H19 118.0 . . ? C20 C19 H19 118.0 . . ? C21 C20 C19 118.3(4) . . ? C21 C20 H20 120.9 . . ? C19 C20 H20 120.9 . . ? C22 C21 C20 118.7(4) . . ? C22 C21 C29 120.8(4) . . ? C20 C21 C29 120.3(4) . . ? C21 C22 C23 120.5(4) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 N6 120.9(4) . . ? C22 C23 C24 123.2(4) . . ? N6 C23 C24 115.9(4) . . ? N7 C24 C25 120.4(4) . . ? N7 C24 C23 115.6(4) . . ? C25 C24 C23 123.9(4) . . ? C24 C25 C26 119.8(4) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 118.8(4) . . ? C27 C26 C31 118.5(4) . . ? C25 C26 C31 122.7(4) . . ? C26 C27 C28 118.3(4) . . ? C26 C27 H27 120.9 . . ? C28 C27 H27 120.9 . . ? N7 C28 C27 123.3(4) . . ? N7 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? O1 C29 O2 125.0(4) . . ? O1 C29 C21 124.7(4) . . ? O2 C29 C21 110.3(3) . . ? O2 C30 H30A 109.5 . . ? O2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O3 C31 O4 124.7(4) . . ? O3 C31 C26 123.4(4) . . ? O4 C31 C26 111.9(3) . . ? O4 C32 H32A 109.5 . . ? O4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.685 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.079 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.162 0.250 -0.097 444.5 75.3 2 0.662 0.750 -0.097 444.5 75.3 3 0.426 0.834 0.141 59.1 2.7 4 0.926 0.334 0.141 59.1 2.7 5 0.426 0.166 0.641 59.1 2.6 6 0.926 0.666 0.641 59.1 2.6 _platon_squeeze_details ; ;