Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email JPCOLLIN@CHIMIE.U-STRASBG.FR _publ_contact_author_name 'Dr Jean-Paul Collin' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Faculte de chimie Universite Louis Pasteur ILB 4 rue Blaise Pascal Strasbourg France 67000 FRANCE ; _publ_section_title ; Photochemical and thermal synthesis and characterization of polypyridine ruthenium(II) complexes containing different monodentate ligands. ; loop_ _publ_author_name 'Jean-Paul Collin' 'Sylvestre Bonnet' 'Nathalie Gruber' 'Jean-Pierre Sauvage' 'Emma R. Schofield' data_st532 _database_code_depnum_ccdc_archive 'CCDC 218272' #========================================================================== #==== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C31 H25 Cl F6 N7 P Ru' _chemical_formula_structural [Ru(terpy)(phen)(Cl][PF6] _chemical_formula_analytical ? _chemical_formula_sum 'C31 H25 Cl F6 N7 P Ru' _chemical_formula_weight 777.08 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1 #========================================================================== #==== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 8.8775(4) _cell_length_b 12.0354(5) _cell_length_c 15.3203(6) _cell_angle_alpha 80.973(8) _cell_angle_beta 80.067(8) _cell_angle_gamma 85.708(8) _cell_volume 1590.5(1) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 7235 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.62 _exptl_crystal_density_method none _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 0.697 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #========================================================================== #==== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 7235 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 20 sec per frame. Data collection was divided into 5 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.40 Omega = 0.00 Kappa = 0.00 91 frames Set 2 Theta = -3.40 Kappa = -172.00 Phi = 0.00 22 frames Set 3 Theta = -5.50 Kappa = -167.00 Phi = 0.00 20 frames Set 4 Theta = -6.40 Kappa = 112.00 Phi = 0.00 14 frames Set 5 Theta = -6.40 Kappa = -74.00 Phi = 0.00 29 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7235 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7235 _reflns_number_gt 5225 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #========================================================================== #==== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5225 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.062 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_all 0.124 _refine_ls_wR_factor_ref 0.051 _refine_ls_goodness_of_fit_all 1.700 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_shift/su_max 0.005 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.624 _refine_diff_density_min -0.166 #========================================================================== #==== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RU 0.32302(3) 0.06609(2) 0.79408(2) 0.0198(1) Uani ? ? Ru CL 0.38164(9) 0.12318(6) 0.92844(5) 0.0267(3) Uani ? ? Cl N1 0.4288(3) 0.2036(2) 0.7097(2) 0.022(1) Uani ? ? N C1 0.4994(3) 0.2868(2) 0.7315(2) 0.027(2) Uani ? ? C C2 0.5671(4) 0.3734(2) 0.6663(2) 0.031(2) Uani ? ? C C3 0.5621(4) 0.3732(2) 0.5779(2) 0.029(2) Uani ? ? C C4 0.4870(3) 0.2863(2) 0.5528(2) 0.026(1) Uani ? ? C C5 0.4718(4) 0.2786(3) 0.4617(2) 0.035(2) Uani ? ? C C6 0.3996(4) 0.1917(3) 0.4420(2) 0.036(2) Uani ? ? C C7 0.3348(4) 0.1055(3) 0.5112(2) 0.031(2) Uani ? ? C C8 0.2588(4) 0.0123(3) 0.4959(2) 0.038(2) Uani ? ? C C9 0.2061(4) -0.0669(2) 0.5659(2) 0.036(2) Uani ? ? C C10 0.2214(4) -0.0546(2) 0.6529(2) 0.030(2) Uani ? ? C N2 0.2903(3) 0.0334(2) 0.6714(2) 0.023(1) Uani ? ? N C11 0.3468(3) 0.1125(2) 0.6000(2) 0.025(1) Uani ? ? C C12 0.4219(3) 0.2038(2) 0.6210(2) 0.024(1) Uani ? ? C N3 0.5079(3) -0.0500(2) 0.7940(2) 0.023(1) Uani ? ? N C13 0.6567(3) -0.0333(2) 0.7579(2) 0.028(2) Uani ? ? C C14 0.7687(4) -0.1206(3) 0.7593(2) 0.033(2) Uani ? ? C C15 0.7285(4) -0.2275(3) 0.7988(2) 0.037(2) Uani ? ? C C16 0.5782(4) -0.2457(2) 0.8375(2) 0.034(2) Uani ? ? C C17 0.4685(4) -0.1558(2) 0.8345(2) 0.026(1) Uani ? ? C C18 0.3057(3) -0.1661(2) 0.8729(2) 0.023(1) Uani ? ? C C19 0.2350(4) -0.2633(2) 0.9167(2) 0.029(2) Uani ? ? C C20 0.0775(4) -0.2584(2) 0.9468(2) 0.031(2) Uani ? ? C C21 -0.0077(4) -0.1570(2) 0.9343(2) 0.028(1) Uani ? ? C C22 0.0673(3) -0.0610(2) 0.8904(2) 0.022(1) Uani ? ? C N4 0.2216(3) -0.0680(2) 0.8611(2) 0.022(1) Uani ? ? N C23 -0.0017(3) 0.0531(2) 0.8696(2) 0.022(1) Uani ? ? C N5 0.0993(3) 0.1320(2) 0.8232(1) 0.022(1) Uani ? ? N C24 0.0449(3) 0.2392(2) 0.8045(2) 0.026(1) Uani ? ? C C25 -0.1062(4) 0.2723(2) 0.8293(2) 0.031(2) Uani ? ? C C26 -0.2090(4) 0.1940(3) 0.8740(2) 0.032(2) Uani ? ? C C27 -0.1562(3) 0.0822(2) 0.8948(2) 0.027(1) Uani ? ? C P 0.1279(1) -0.41288(6) 0.70599(6) 0.0329(4) Uani ? ? P F1 0.1984(3) -0.5348(2) 0.6998(3) 0.083(2) Uani ? ? F F2 0.0598(3) -0.2897(2) 0.7113(2) 0.078(2) Uani ? ? F F3 0.2825(3) -0.3789(2) 0.7306(2) 0.071(1) Uani ? ? F F4 -0.0271(3) -0.4461(2) 0.6806(2) 0.073(1) Uani ? ? F F5 0.1953(3) -0.3764(3) 0.6029(2) 0.067(2) Uani ? ? F F6 0.0575(3) -0.4460(2) 0.8079(2) 0.074(2) Uani ? ? F C28 0.0228(5) 0.3339(3) 0.5544(3) 0.057(2) Uani ? ? C C29 -0.0425(4) 0.2264(3) 0.5944(2) 0.045(2) Uani ? ? C N6 -0.0938(4) 0.1431(3) 0.6251(2) 0.060(2) Uani ? ? N C30 0.2828(5) -0.5858(3) 0.9532(3) 0.054(2) Uani ? ? C C31 0.4446(4) -0.5649(3) 0.9204(2) 0.044(2) Uani ? ? C N7 0.5689(4) -0.5485(3) 0.8952(2) 0.060(2) Uani ? ? N H1 0.5045 0.2880 0.7928 0.0354 Uiso calc C1 H H2 0.6160 0.4317 0.6842 0.0412 Uiso calc C2 H H3 0.6084 0.4305 0.5338 0.0406 Uiso calc C3 H H4 0.5128 0.3348 0.4147 0.0488 Uiso calc C5 H H5 0.3920 0.1882 0.3814 0.0492 Uiso calc C6 H H6 0.2449 0.0053 0.4369 0.0498 Uiso calc C8 H H7 0.1587 -0.1307 0.5554 0.0464 Uiso calc C9 H H8 0.1819 -0.1101 0.7009 0.0384 Uiso calc C10 H H9 0.6852 0.0403 0.7309 0.0363 Uiso calc C13 H H10 0.8719 -0.1066 0.7333 0.0432 Uiso calc C14 H H11 0.8035 -0.2881 0.7993 0.0486 Uiso calc C15 H H12 0.5495 -0.3187 0.8660 0.0444 Uiso calc C16 H H13 0.2933 -0.3323 0.9260 0.0390 Uiso calc C19 H H14 0.0281 -0.3247 0.9759 0.0407 Uiso calc C20 H H15 -0.1148 -0.1532 0.9553 0.0365 Uiso calc C21 H H16 0.1138 0.2942 0.7730 0.0344 Uiso calc C24 H H17 -0.1397 0.3489 0.8155 0.0407 Uiso calc C25 H H18 -0.3139 0.2156 0.8905 0.0417 Uiso calc C26 H H19 -0.2248 0.0268 0.9257 0.0348 Uiso calc C27 H H20 0.1036 0.3469 0.5843 0.0730 Uiso calc C28 H H21 0.0615 0.3320 0.4928 0.0730 Uiso calc C28 H H22 -0.0543 0.3927 0.5600 0.0730 Uiso calc C28 H H23 0.2677 -0.6640 0.9584 0.0746 Uiso calc C30 H H24 0.2535 -0.5618 1.0102 0.0746 Uiso calc C30 H H25 0.2222 -0.5450 0.9123 0.0746 Uiso calc C30 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RU 0.0199(1) 0.0198(1) 0.0197(1) -0.00262(9) -0.00247(9) -0.00127(9) Ru CL 0.0272(4) 0.0307(3) 0.0227(3) -0.0049(3) -0.0037(3) -0.0034(3) Cl N1 0.020(1) 0.023(1) 0.023(1) 0.0009(9) -0.002(1) -0.0037(9) N C1 0.027(2) 0.026(1) 0.029(2) -0.001(1) -0.004(1) -0.003(1) C C2 0.032(2) 0.024(1) 0.040(2) -0.008(1) -0.006(1) -0.003(1) C C3 0.029(2) 0.027(1) 0.032(2) -0.004(1) 0.001(1) 0.007(1) C C4 0.025(2) 0.030(1) 0.025(2) -0.005(1) -0.001(1) 0.000(1) C C5 0.039(2) 0.045(2) 0.024(2) -0.008(2) 0.000(2) 0.006(1) C C6 0.040(2) 0.047(2) 0.025(2) -0.009(2) -0.004(2) -0.001(1) C C7 0.029(2) 0.039(2) 0.026(2) -0.000(1) -0.005(1) -0.008(1) C C8 0.047(2) 0.044(2) 0.027(2) -0.006(2) -0.012(1) -0.008(1) C C9 0.046(2) 0.030(1) 0.034(2) -0.008(1) -0.007(1) -0.011(1) C C10 0.032(2) 0.030(1) 0.028(2) -0.006(1) -0.007(1) -0.004(1) C N2 0.020(1) 0.025(1) 0.025(1) -0.000(1) -0.002(1) -0.002(1) N C11 0.023(2) 0.028(1) 0.023(1) -0.001(1) -0.003(1) -0.002(1) C C12 0.020(1) 0.028(1) 0.024(2) 0.001(1) 0.000(1) -0.001(1) C N3 0.024(1) 0.025(1) 0.022(1) -0.003(1) -0.003(1) -0.004(1) N C13 0.024(2) 0.038(1) 0.023(1) -0.001(1) -0.004(1) -0.008(1) C C14 0.025(2) 0.043(2) 0.032(2) -0.001(1) -0.003(1) -0.009(1) C C15 0.034(2) 0.036(2) 0.040(2) 0.012(1) -0.006(2) -0.007(1) C C16 0.036(2) 0.028(1) 0.038(2) 0.005(1) -0.009(1) -0.002(1) C C17 0.029(2) 0.027(1) 0.022(1) -0.001(1) -0.004(1) -0.006(1) C C18 0.025(2) 0.023(1) 0.021(1) -0.000(1) -0.005(1) -0.002(1) C C19 0.038(2) 0.020(1) 0.031(2) -0.001(1) -0.005(1) -0.002(1) C C20 0.038(2) 0.026(1) 0.030(2) -0.012(1) -0.002(1) -0.002(1) C C21 0.029(2) 0.030(1) 0.026(2) -0.009(1) -0.003(1) -0.005(1) C C22 0.022(1) 0.028(1) 0.019(1) -0.005(1) -0.004(1) -0.006(1) C N4 0.023(1) 0.022(1) 0.021(1) -0.003(1) -0.004(1) -0.0016(9) N C23 0.021(1) 0.029(1) 0.018(1) -0.006(1) -0.004(1) -0.005(1) C N5 0.024(1) 0.023(1) 0.019(1) 0.000(1) -0.003(1) -0.003(1) N C24 0.027(2) 0.024(1) 0.028(2) -0.001(1) -0.006(1) -0.002(1) C C25 0.031(2) 0.030(1) 0.033(2) 0.004(1) -0.010(1) -0.003(1) C C26 0.026(2) 0.040(2) 0.032(2) 0.004(1) -0.007(1) -0.010(1) C C27 0.021(2) 0.036(1) 0.025(1) -0.004(1) -0.005(1) -0.007(1) C P 0.0341(5) 0.0291(4) 0.0359(5) -0.0042(4) 0.0017(4) -0.0042(4) P F1 0.073(2) 0.035(1) 0.224(4) 0.009(1) 0.018(2) -0.009(2) F F2 0.067(2) 0.038(1) 0.183(3) 0.001(1) 0.043(2) -0.008(2) F F3 0.049(1) 0.122(2) 0.061(1) -0.032(1) -0.002(1) -0.022(1) F F4 0.044(1) 0.128(2) 0.069(1) -0.035(1) 0.001(1) -0.031(1) F F5 0.054(1) 0.148(2) 0.038(1) -0.023(1) 0.005(1) -0.005(1) F F6 0.071(2) 0.152(2) 0.038(1) -0.040(2) 0.003(1) 0.014(2) F C28 0.059(2) 0.053(2) 0.059(2) -0.011(2) -0.018(2) -0.004(2) C C29 0.044(2) 0.055(2) 0.037(2) -0.006(2) -0.010(2) -0.016(2) C N6 0.066(2) 0.064(2) 0.051(2) -0.026(2) -0.003(2) -0.014(2) N C30 0.053(2) 0.035(2) 0.087(3) -0.004(2) -0.018(2) -0.009(2) C C31 0.061(2) 0.027(1) 0.052(2) -0.001(2) -0.017(2) -0.014(1) C N7 0.058(2) 0.054(2) 0.068(2) -0.008(1) -0.005(2) -0.026(1) N # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU CL 2.4180(8) . . ? RU N1 2.105(2) . . ? RU N2 2.051(3) . . ? RU N3 2.074(3) . . ? RU N4 1.961(2) . . ? RU N5 2.084(3) . . ? RU N1 2.105(2) . . ? RU N2 2.051(3) . . ? RU N3 2.074(3) . . ? RU N4 1.961(2) . . ? RU N5 2.084(3) . . ? N1 C1 1.334(4) . . ? N1 C12 1.370(4) . . ? C1 C2 1.417(4) . . ? C2 C3 1.363(5) . . ? C3 C4 1.416(4) . . ? C4 C5 1.442(5) . . ? C4 C12 1.402(4) . . ? C5 C6 1.364(5) . . ? C6 C7 1.437(5) . . ? C7 C8 1.421(5) . . ? C7 C11 1.398(4) . . ? C8 C9 1.360(5) . . ? C9 C10 1.394(5) . . ? C10 N2 1.353(4) . . ? N2 C11 1.382(4) . . ? C11 C12 1.433(4) . . ? N3 C13 1.358(4) . . ? N3 C17 1.368(4) . . ? C13 C14 1.391(5) . . ? C14 C15 1.378(5) . . ? C15 C16 1.382(5) . . ? C16 C17 1.401(4) . . ? C17 C18 1.470(4) . . ? C18 C19 1.389(4) . . ? C18 N4 1.354(4) . . ? C19 C20 1.394(5) . . ? C20 C21 1.391(5) . . ? C21 C22 1.396(4) . . ? C22 N4 1.367(4) . . ? C22 C23 1.471(4) . . ? C23 N5 1.380(4) . . ? C23 C27 1.393(4) . . ? N5 C24 1.349(4) . . ? C24 C25 1.376(5) . . ? C25 C26 1.379(5) . . ? C26 C27 1.397(5) . . ? P F1 1.562(3) . . ? P F2 1.567(3) . . ? P F3 1.582(3) . . ? P F4 1.587(3) . . ? P F5 1.594(3) . . ? P F6 1.579(3) . . ? C28 C29 1.457(6) . . ? C29 N6 1.132(5) . . ? C30 C31 1.465(6) . . ? C31 N7 1.125(5) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CL RU N1 93.51(7) . . . ? CL RU N2 172.82(7) . . . ? CL RU N3 89.41(7) . . . ? CL RU N4 92.56(7) . . . ? CL RU N5 90.01(7) . . . ? N1 RU N2 79.38(9) . . . ? N1 RU N3 99.9(1) . . . ? N1 RU N4 173.90(9) . . . ? N1 RU N5 101.17(9) . . . ? N2 RU N3 90.8(1) . . . ? N2 RU N4 94.5(1) . . . ? N2 RU N5 92.3(1) . . . ? N3 RU N4 79.5(1) . . . ? N3 RU N5 158.9(1) . . . ? N4 RU N5 79.5(1) . . . ? N1 RU N2 79.38(9) . . . ? N1 RU N3 99.9(1) . . . ? N1 RU N4 173.90(9) . . . ? N1 RU N5 101.17(9) . . . ? N2 RU N3 90.8(1) . . . ? N2 RU N4 94.5(1) . . . ? N2 RU N5 92.3(1) . . . ? N3 RU N4 79.5(1) . . . ? N3 RU N5 158.9(1) . . . ? N4 RU N5 79.5(1) . . . ? RU N1 C1 128.8(2) . . . ? RU N1 C12 113.2(2) . . . ? C1 N1 C12 118.0(3) . . . ? N1 C1 C2 122.1(3) . . . ? C1 C2 C3 120.0(3) . . . ? C2 C3 C4 119.1(3) . . . ? C3 C4 C5 124.1(3) . . . ? C3 C4 C12 117.7(3) . . . ? C5 C4 C12 118.3(3) . . . ? C4 C5 C6 121.0(3) . . . ? C5 C6 C7 121.3(3) . . . ? C6 C7 C8 124.5(3) . . . ? C6 C7 C11 118.4(3) . . . ? C8 C7 C11 117.0(3) . . . ? C7 C8 C9 119.9(3) . . . ? C8 C9 C10 120.1(3) . . . ? C9 C10 N2 122.4(3) . . . ? RU N2 C10 128.1(2) . . . ? RU N2 C11 114.6(2) . . . ? C10 N2 C11 117.3(3) . . . ? C7 C11 N2 123.2(3) . . . ? C7 C11 C12 120.5(3) . . . ? N2 C11 C12 116.3(3) . . . ? N1 C12 C4 123.1(3) . . . ? N1 C12 C11 116.4(3) . . . ? C4 C12 C11 120.5(3) . . . ? RU N3 C13 128.1(2) . . . ? RU N3 C17 113.4(2) . . . ? C13 N3 C17 118.5(3) . . . ? N3 C13 C14 122.1(3) . . . ? C13 C14 C15 119.4(3) . . . ? C14 C15 C16 119.4(3) . . . ? C15 C16 C17 119.6(3) . . . ? N3 C17 C16 121.0(3) . . . ? N3 C17 C18 115.0(3) . . . ? C16 C17 C18 124.0(3) . . . ? C17 C18 C19 126.9(3) . . . ? C17 C18 N4 113.3(2) . . . ? C19 C18 N4 119.8(3) . . . ? C18 C19 C20 119.3(3) . . . ? C19 C20 C21 120.5(3) . . . ? C20 C21 C22 118.7(3) . . . ? C21 C22 N4 119.8(3) . . . ? C21 C22 C23 127.2(3) . . . ? N4 C22 C23 113.1(2) . . . ? RU N4 C18 118.8(2) . . . ? RU N4 C22 119.1(2) . . . ? C18 N4 C22 122.0(2) . . . ? C22 C23 N5 114.9(3) . . . ? C22 C23 C27 123.8(3) . . . ? N5 C23 C27 121.3(3) . . . ? RU N5 C23 113.4(2) . . . ? RU N5 C24 128.5(2) . . . ? C23 N5 C24 118.1(3) . . . ? N5 C24 C25 122.7(3) . . . ? C24 C25 C26 119.8(3) . . . ? C25 C26 C27 118.9(3) . . . ? C23 C27 C26 119.2(3) . . . ? F1 P F2 179.0(2) . . . ? F1 P F3 89.6(2) . . . ? F1 P F4 90.7(2) . . . ? F1 P F5 89.7(2) . . . ? F1 P F6 91.9(2) . . . ? F2 P F3 89.7(2) . . . ? F2 P F4 90.0(2) . . . ? F2 P F5 89.6(2) . . . ? F2 P F6 88.8(2) . . . ? F3 P F4 179.5(2) . . . ? F3 P F5 88.7(1) . . . ? F3 P F6 92.0(2) . . . ? F4 P F5 90.9(2) . . . ? F4 P F6 88.4(1) . . . ? F5 P F6 178.3(2) . . . ? C28 C29 N6 179.5(4) . . . ? C30 C31 N7 180(1) . . . ? #===END data_st542 _database_code_depnum_ccdc_archive 'CCDC 218273' _audit_creation_date 10-02-00 # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C33 H28 F12 N8 P2 Ru' _chemical_formula_structural [Ru(terpy)(phen)(CH3CN)][PF6]2 _chemical_formula_analytical ? _chemical_formula_sum 'C33 H28 F12 N8 P2 Ru' _chemical_formula_weight 927.64 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1 #========================================================================== #==== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 8.7526(3) _cell_length_b 11.5332(2) _cell_length_c 36.851(1) _cell_angle_alpha 90 _cell_angle_beta 92.216(5) _cell_angle_gamma 90 _cell_volume 3717.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.66 _exptl_crystal_density_method none _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #========================================================================== #==== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 12879 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 44. mm. Scan angle = 0.8 deg 1 scans of 60 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 9.20 Omega = 0.00 Kappa = 0.00 227 frames Set 2 Theta = -9.20 Kappa = -80.00 Phi = 0.00 47 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12879 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8203 _reflns_number_gt 3803 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #========================================================================== #==== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0025 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3803 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.102 _refine_ls_R_factor_gt 0.041 _refine_ls_wR_factor_all 0.200 _refine_ls_wR_factor_ref 0.050 _refine_ls_goodness_of_fit_all 5.855 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_shift/su_max 0.023 _refine_ls_shift/esd_mean 0.004 _refine_diff_density_max 0.508 _refine_diff_density_min -0.158 #========================================================================== #==== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RU 0.07789(4) 0.10819(3) 0.37551(1) 0.0271(2) Uani ? ? Ru N1 -0.0131(4) 0.2440(3) 0.4056(1) 0.029(2) Uani ? ? N C1 -0.0939(6) 0.3369(4) 0.3943(1) 0.042(3) Uani ? ? C C2 -0.1522(6) 0.4186(4) 0.4188(2) 0.049(3) Uani ? ? C C3 -0.1247(6) 0.4064(4) 0.4551(2) 0.048(3) Uani ? ? C C4 -0.0354(5) 0.3120(4) 0.4687(1) 0.041(3) Uani ? ? C C5 0.0042(6) 0.2916(4) 0.5057(1) 0.049(3) Uani ? ? C C6 0.0888(6) 0.1992(5) 0.5164(1) 0.048(3) Uani ? ? C C7 0.1429(6) 0.1158(4) 0.4912(1) 0.036(3) Uani ? ? C C8 0.2302(6) 0.0172(4) 0.5002(1) 0.045(3) Uani ? ? C C9 0.2736(6) -0.0556(4) 0.4733(1) 0.042(3) Uani ? ? C C10 0.2329(5) -0.0323(4) 0.4371(1) 0.035(3) Uani ? ? C N2 0.1520(4) 0.0616(3) 0.4270(1) 0.028(2) Uani ? ? N C11 0.1068(5) 0.1345(4) 0.4540(1) 0.031(3) Uani ? ? C C12 0.0162(5) 0.2325(4) 0.4425(1) 0.031(3) Uani ? ? C N3 -0.0944(4) -0.0154(3) 0.3785(1) 0.028(2) Uani ? ? N C13 -0.2322(5) -0.0054(4) 0.3930(1) 0.033(3) Uani ? ? C C14 -0.3350(5) -0.0957(4) 0.3949(1) 0.037(3) Uani ? ? C C15 -0.2961(6) -0.2030(4) 0.3811(1) 0.045(3) Uani ? ? C C16 -0.1524(6) -0.2156(4) 0.3660(1) 0.038(3) Uani ? ? C C17 -0.0557(5) -0.1210(4) 0.3643(1) 0.031(3) Uani ? ? C C18 0.0963(5) -0.1260(4) 0.3482(1) 0.030(3) Uani ? ? C C19 0.1645(5) -0.2207(4) 0.3317(1) 0.033(3) Uani ? ? C C20 0.3087(6) -0.2092(4) 0.3188(1) 0.038(3) Uani ? ? C C21 0.3870(5) -0.1039(4) 0.3216(1) 0.035(3) Uani ? ? C C22 0.3168(5) -0.0111(4) 0.3382(1) 0.029(3) Uani ? ? C N4 0.1733(4) -0.0244(3) 0.3513(1) 0.027(2) Uani ? ? N C23 0.3796(5) 0.1071(4) 0.3446(1) 0.030(3) Uani ? ? C N5 0.2867(4) 0.1806(3) 0.3633(1) 0.027(2) Uani ? ? N C24 0.3393(5) 0.2887(4) 0.3699(1) 0.034(3) Uani ? ? C C25 0.4792(6) 0.3279(4) 0.3588(1) 0.040(3) Uani ? ? C C26 0.5699(6) 0.2535(4) 0.3400(1) 0.043(3) Uani ? ? C C27 0.5206(5) 0.1411(4) 0.3329(1) 0.037(3) Uani ? ? C N6 -0.0081(4) 0.1637(3) 0.3262(1) 0.033(2) Uani ? ? N C28 -0.0537(5) 0.1851(4) 0.2978(1) 0.036(3) Uani ? ? C C29 -0.1141(7) 0.2134(5) 0.2611(1) 0.052(4) Uani ? ? C P1 0.2683(2) 0.0432(1) 0.21715(5) 0.059(1) Uani ? ? P F1 0.1516(6) -0.0327(5) 0.1958(1) 0.167(4) Uani ? ? F F2 0.3865(7) 0.1131(4) 0.2391(2) 0.187(5) Uani ? ? F F3 0.1792(5) 0.0228(4) 0.2522(1) 0.139(3) Uani ? ? F F4 0.3546(5) 0.0605(4) 0.1818(1) 0.170(3) Uani ? ? F F5 0.3632(4) -0.0714(3) 0.2261(1) 0.091(3) Uani ? ? F F6 0.1739(5) 0.1557(3) 0.2091(1) 0.122(3) Uani ? ? F P2 0.3049(2) -0.3895(1) 0.41872(4) 0.0493(9) Uani ? ? P F7 0.3007(5) -0.4240(3) 0.37689(9) 0.083(3) Uani ? ? F F8 0.3072(4) -0.3598(3) 0.46099(9) 0.077(2) Uani ? ? F F9 0.2241(4) -0.5097(3) 0.42745(9) 0.071(2) Uani ? ? F F10 0.3834(4) -0.2701(3) 0.4098(1) 0.091(3) Uani ? ? F F11 0.1416(3) -0.3282(3) 0.41353(8) 0.062(2) Uani ? ? F F12 0.4693(3) -0.4510(3) 0.4246(1) 0.071(2) Uani ? ? F C30 0.4351(6) -0.6698(5) 0.4796(2) 0.063(4) Uani ? ? C C31 0.4995(6) -0.7654(4) 0.4594(2) 0.050(3) Uani ? ? C N7 0.5475(6) -0.8400(5) 0.4442(1) 0.074(4) Uani ? ? N C32 0.7399(8) -0.1177(6) 0.2220(2) 0.086(5) Uani ? ? C C33 0.7515(6) -0.0798(5) 0.2593(2) 0.052(4) Uani ? ? C N8 0.7595(5) -0.0481(4) 0.2884(1) 0.065(3) Uani ? ? N H1 -0.1126 0.3482 0.3689 0.0549 Uiso calc C1 H H2 -0.2109 0.4824 0.4098 0.0668 Uiso calc C2 H H3 -0.1653 0.4611 0.4714 0.0638 Uiso calc C3 H H4 -0.0296 0.3443 0.5235 0.0643 Uiso calc C5 H H5 0.1133 0.1891 0.5416 0.0654 Uiso calc C6 H H6 0.2588 0.0013 0.5248 0.0627 Uiso calc C8 H H7 0.3321 -0.1228 0.4793 0.0561 Uiso calc C9 H H8 0.2636 -0.0849 0.4189 0.0461 Uiso calc C10 H H9 -0.2603 0.0677 0.4026 0.0427 Uiso calc C13 H H10 -0.4311 -0.0844 0.4055 0.0498 Uiso calc C14 H H11 -0.3652 -0.2665 0.3818 0.0589 Uiso calc C15 H H12 -0.1216 -0.2888 0.3570 0.0496 Uiso calc C16 H H13 0.1115 -0.2924 0.3293 0.0442 Uiso calc C19 H H14 0.3559 -0.2738 0.3078 0.0503 Uiso calc C20 H H15 0.4862 -0.0960 0.3124 0.0462 Uiso calc C21 H H16 0.2772 0.3405 0.3829 0.0445 Uiso calc C24 H H17 0.5121 0.4048 0.3640 0.0527 Uiso calc C25 H H18 0.6659 0.2789 0.3319 0.0562 Uiso calc C26 H H19 0.5828 0.0886 0.3202 0.0486 Uiso calc C27 H H20 -0.0474 0.1834 0.2437 0.0717 Uiso calc C29 H H21 -0.2126 0.1800 0.2574 0.0717 Uiso calc C29 H H22 -0.1212 0.2952 0.2585 0.0717 Uiso calc C29 H H23 0.4743 -0.5985 0.4710 0.0834 Uiso calc C30 H H24 0.3269 -0.6703 0.4762 0.0834 Uiso calc C30 H H25 0.4620 -0.6782 0.5046 0.0834 Uiso calc C30 H H26 0.7751 -0.1953 0.2204 0.1168 Uiso calc C32 H H27 0.6363 -0.1136 0.2134 0.1168 Uiso calc C32 H H28 0.8007 -0.0689 0.2076 0.1168 Uiso calc C32 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RU 0.0282(2) 0.0297(2) 0.0237(2) 0.0004(2) -0.0000(2) -0.0018(2) Ru N1 0.025(2) 0.024(2) 0.041(3) -0.002(2) 0.005(2) -0.005(2) N C1 0.040(3) 0.036(3) 0.051(4) -0.002(3) 0.001(3) -0.008(3) C C2 0.041(3) 0.039(3) 0.074(4) 0.009(3) -0.000(3) -0.011(3) C C3 0.036(3) 0.046(3) 0.067(4) -0.006(3) 0.017(3) -0.024(3) C C4 0.033(3) 0.043(3) 0.048(3) -0.011(2) 0.013(3) -0.015(3) C C5 0.053(3) 0.057(3) 0.040(3) -0.014(3) 0.020(3) -0.023(3) C C6 0.060(4) 0.063(3) 0.029(3) -0.016(3) 0.009(3) -0.005(3) C C7 0.045(3) 0.046(3) 0.023(3) -0.013(3) 0.007(2) -0.003(3) C C8 0.061(4) 0.056(3) 0.027(3) -0.010(3) -0.002(3) 0.008(3) C C9 0.050(3) 0.048(3) 0.031(3) -0.001(3) -0.008(3) 0.007(3) C C10 0.039(3) 0.034(3) 0.032(3) -0.007(2) -0.001(2) 0.001(2) C N2 0.034(2) 0.030(2) 0.022(2) -0.003(2) 0.002(2) -0.000(2) N C11 0.028(3) 0.037(3) 0.028(3) -0.007(2) 0.007(2) -0.001(2) C C12 0.031(3) 0.035(3) 0.027(3) -0.009(2) 0.008(2) -0.008(2) C N3 0.031(2) 0.037(2) 0.019(2) 0.000(2) -0.001(2) 0.001(2) N C13 0.032(3) 0.036(3) 0.031(3) 0.002(2) 0.001(2) -0.001(2) C C14 0.027(3) 0.051(3) 0.037(3) 0.001(3) 0.005(2) 0.010(3) C C15 0.043(3) 0.050(3) 0.042(3) -0.014(3) -0.006(3) 0.003(3) C C16 0.039(3) 0.041(3) 0.034(3) -0.008(3) 0.001(2) -0.001(3) C C17 0.029(3) 0.033(3) 0.030(3) -0.003(2) -0.005(2) -0.003(2) C C18 0.035(3) 0.035(3) 0.022(3) -0.000(2) -0.003(2) -0.001(2) C C19 0.045(3) 0.027(2) 0.030(3) -0.004(2) -0.003(2) -0.009(2) C C20 0.043(3) 0.039(3) 0.033(3) 0.005(3) -0.002(3) -0.008(3) C C21 0.036(3) 0.044(3) 0.027(3) 0.006(3) 0.004(2) -0.007(3) C C22 0.030(3) 0.039(3) 0.021(3) -0.000(2) -0.001(2) 0.003(2) C N4 0.028(2) 0.030(2) 0.024(2) -0.003(2) -0.002(2) 0.001(2) N C23 0.030(3) 0.031(2) 0.031(3) 0.002(2) 0.000(2) 0.003(2) C N5 0.029(2) 0.031(2) 0.023(2) 0.001(2) -0.001(2) 0.001(2) N C24 0.039(3) 0.031(3) 0.033(3) -0.002(2) 0.001(2) -0.003(2) C C25 0.041(3) 0.033(3) 0.047(3) -0.008(3) -0.005(3) -0.000(3) C C26 0.035(3) 0.050(3) 0.045(3) -0.007(3) 0.003(3) 0.003(3) C C27 0.031(3) 0.042(3) 0.040(3) 0.002(2) 0.006(2) 0.002(2) C N6 0.034(2) 0.033(2) 0.032(2) -0.000(2) 0.001(2) 0.003(2) N C28 0.040(3) 0.038(3) 0.031(3) 0.009(2) 0.003(2) 0.003(2) C C29 0.073(4) 0.061(3) 0.031(3) 0.019(3) -0.002(3) 0.004(3) C P1 0.073(1) 0.0502(9) 0.055(1) 0.0168(9) 0.0117(9) 0.0023(8) P F1 0.168(4) 0.168(4) 0.167(5) -0.038(4) -0.091(4) -0.006(4) F F2 0.206(6) 0.107(4) 0.297(8) -0.041(4) -0.085(5) -0.031(4) F F3 0.199(3) 0.165(3) 0.082(3) 0.126(2) 0.078(2) 0.062(2) F F4 0.236(4) 0.126(3) 0.165(4) 0.084(3) 0.147(3) 0.064(3) F F5 0.100(3) 0.070(2) 0.106(3) 0.036(2) 0.015(2) 0.013(2) F F6 0.197(4) 0.113(2) 0.081(3) 0.106(2) 0.052(3) 0.042(2) F P2 0.0517(9) 0.0455(8) 0.0510(9) 0.0002(8) 0.0192(7) -0.0022(8) P F7 0.160(3) 0.081(2) 0.044(2) 0.049(2) 0.029(2) 0.006(2) F F8 0.055(2) 0.143(3) 0.058(2) 0.020(2) -0.009(2) -0.043(2) F F9 0.066(2) 0.064(2) 0.085(3) -0.013(2) -0.007(2) 0.023(2) F F10 0.080(2) 0.046(2) 0.204(4) -0.006(2) 0.075(2) -0.000(2) F F11 0.061(2) 0.074(2) 0.053(2) 0.017(2) 0.009(2) 0.008(2) F F12 0.049(2) 0.070(2) 0.103(3) 0.014(2) 0.024(2) -0.000(2) F C30 0.056(4) 0.061(4) 0.075(5) 0.003(3) -0.011(3) 0.003(4) C C31 0.044(3) 0.059(3) 0.048(4) 0.003(3) -0.005(3) 0.018(3) C N7 0.072(4) 0.093(3) 0.060(4) 0.021(3) 0.011(3) 0.009(3) N C32 0.097(5) 0.116(5) 0.057(4) 0.010(4) 0.006(4) -0.038(4) C C33 0.039(3) 0.061(4) 0.059(4) -0.004(3) 0.002(3) -0.014(3) C N8 0.065(3) 0.071(3) 0.059(3) 0.003(3) 0.000(3) -0.016(3) N # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU N1 2.093(4) . . ? RU N2 2.054(4) . . ? RU N3 2.081(4) . . ? RU N4 1.973(4) . . ? RU N5 2.075(4) . . ? RU N6 2.041(5) . . ? N1 C1 1.341(6) . . ? N1 C12 1.383(6) . . ? C1 C2 1.414(8) . . ? C2 C3 1.359(8) . . ? C3 C4 1.420(8) . . ? C4 C5 1.416(8) . . ? C4 C12 1.416(7) . . ? C5 C6 1.347(8) . . ? C6 C7 1.431(7) . . ? C7 C8 1.402(7) . . ? C7 C11 1.413(7) . . ? C8 C9 1.365(8) . . ? C9 C10 1.393(7) . . ? C10 N2 1.338(6) . . ? N2 C11 1.371(6) . . ? C11 C12 1.435(7) . . ? N3 C13 1.343(6) . . ? N3 C17 1.373(6) . . ? C13 C14 1.380(7) . . ? C14 C15 1.386(7) . . ? C15 C16 1.402(7) . . ? C16 C17 1.384(7) . . ? C17 C18 1.478(7) . . ? C18 C19 1.397(6) . . ? C18 N4 1.354(5) . . ? C19 C20 1.372(7) . . ? C20 C21 1.397(7) . . ? C21 C22 1.387(7) . . ? C22 N4 1.372(6) . . ? C22 C23 1.486(6) . . ? C23 N5 1.376(6) . . ? C23 C27 1.380(7) . . ? N5 C24 1.348(6) . . ? C24 C25 1.382(7) . . ? C25 C26 1.374(7) . . ? C26 C27 1.388(7) . . ? N6 C28 1.134(6) . . ? C28 C29 1.470(8) . . ? P1 F1 1.539(5) . . ? P1 F2 1.519(6) . . ? P1 F3 1.552(4) . . ? P1 F4 1.544(5) . . ? P1 F5 1.590(4) . . ? P1 F6 1.561(4) . . ? F1 F3 2.180(8) . . ? F1 F4 2.156(8) . . ? F1 F5 2.172(7) . . ? F2 F3 2.162(9) . . ? F2 F5 2.189(6) . . ? F2 F6 2.184(8) . . ? F3 F5 2.195(5) . . ? F4 F6 2.199(6) . . ? P2 F7 1.591(4) . . ? P2 F8 1.594(4) . . ? P2 F9 1.595(3) . . ? P2 F10 1.580(4) . . ? P2 F11 1.600(3) . . ? P2 F12 1.611(4) . . ? C30 C31 1.455(9) . . ? C31 N7 1.117(7) . . ? C32 C33 1.444(9) . . ? C33 N8 1.130(8) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 RU N2 79.6(2) . . . ? N1 RU N3 101.1(2) . . . ? N1 RU N4 174.8(2) . . . ? N1 RU N5 99.8(2) . . . ? N1 RU N6 95.8(2) . . . ? N2 RU N3 88.6(2) . . . ? N2 RU N4 95.2(2) . . . ? N2 RU N5 93.3(2) . . . ? N2 RU N6 175.3(2) . . . ? N3 RU N4 79.2(2) . . . ? N3 RU N5 159.0(2) . . . ? N3 RU N6 91.1(2) . . . ? N4 RU N5 79.7(2) . . . ? N4 RU N6 89.3(2) . . . ? N5 RU N6 88.7(2) . . . ? RU N1 C1 129.8(4) . . . ? RU N1 C12 112.9(3) . . . ? C1 N1 C12 117.3(4) . . . ? N1 C1 C2 122.2(6) . . . ? C1 C2 C3 120.4(6) . . . ? C2 C3 C4 120.0(5) . . . ? C3 C4 C5 125.3(5) . . . ? C3 C4 C12 116.3(6) . . . ? C5 C4 C12 118.4(6) . . . ? C4 C5 C6 121.6(5) . . . ? C5 C6 C7 122.3(6) . . . ? C6 C7 C8 125.7(5) . . . ? C6 C7 C11 117.4(5) . . . ? C8 C7 C11 116.9(5) . . . ? C7 C8 C9 119.5(5) . . . ? C8 C9 C10 120.6(5) . . . ? C9 C10 N2 122.3(5) . . . ? RU N2 C10 127.8(3) . . . ? RU N2 C11 114.8(3) . . . ? C10 N2 C11 117.3(4) . . . ? C7 C11 N2 123.3(5) . . . ? C7 C11 C12 120.4(5) . . . ? N2 C11 C12 116.2(5) . . . ? N1 C12 C4 123.8(5) . . . ? N1 C12 C11 116.4(4) . . . ? C4 C12 C11 119.8(5) . . . ? RU N3 C13 128.7(3) . . . ? RU N3 C17 113.4(3) . . . ? C13 N3 C17 117.8(4) . . . ? N3 C13 C14 123.5(5) . . . ? C13 C14 C15 119.1(5) . . . ? C14 C15 C16 118.4(5) . . . ? C15 C16 C17 119.7(5) . . . ? N3 C17 C16 121.5(5) . . . ? N3 C17 C18 115.2(4) . . . ? C16 C17 C18 123.3(5) . . . ? C17 C18 C19 127.7(5) . . . ? C17 C18 N4 112.7(4) . . . ? C19 C18 N4 119.6(5) . . . ? C18 C19 C20 119.3(5) . . . ? C19 C20 C21 120.9(5) . . . ? C20 C21 C22 118.7(5) . . . ? C21 C22 N4 119.7(4) . . . ? C21 C22 C23 127.7(5) . . . ? N4 C22 C23 112.6(4) . . . ? RU N4 C18 119.4(3) . . . ? RU N4 C22 118.8(3) . . . ? C18 N4 C22 121.8(4) . . . ? C22 C23 N5 115.0(4) . . . ? C22 C23 C27 122.7(5) . . . ? N5 C23 C27 122.3(5) . . . ? RU N5 C23 113.8(3) . . . ? RU N5 C24 129.0(3) . . . ? C23 N5 C24 117.2(4) . . . ? N5 C24 C25 123.3(5) . . . ? C24 C25 C26 118.7(5) . . . ? C25 C26 C27 119.8(5) . . . ? C23 C27 C26 118.8(5) . . . ? RU N6 C28 174.1(5) . . . ? N6 C28 C29 179.5(6) . . . ? F1 P1 F2 177.3(4) . . . ? F1 P1 F3 89.7(4) . . . ? F1 P1 F4 88.8(4) . . . ? F1 P1 F5 87.9(3) . . . ? F1 P1 F6 92.3(3) . . . ? F2 P1 F3 89.5(4) . . . ? F2 P1 F4 92.0(4) . . . ? F2 P1 F5 89.5(3) . . . ? F2 P1 F6 90.3(3) . . . ? F3 P1 F4 178.4(4) . . . ? F3 P1 F5 88.6(2) . . . ? F3 P1 F6 90.3(2) . . . ? F4 P1 F5 90.8(2) . . . ? F4 P1 F6 90.2(2) . . . ? F5 P1 F6 179.0(2) . . . ? P1 F1 F3 45.4(2) . . . ? P1 F1 F4 45.7(2) . . . ? P1 F1 F5 47.0(2) . . . ? F3 F1 F4 91.1(3) . . . ? F3 F1 F5 60.6(2) . . . ? F4 F1 F5 62.1(3) . . . ? P1 F2 F3 45.9(2) . . . ? P1 F2 F5 46.6(2) . . . ? P1 F2 F6 45.6(2) . . . ? F3 F2 F5 60.6(2) . . . ? F3 F2 F6 61.1(3) . . . ? F5 F2 F6 92.2(3) . . . ? P1 F3 F1 44.9(2) . . . ? P1 F3 F2 44.6(3) . . . ? P1 F3 F5 46.4(2) . . . ? F1 F3 F2 89.5(3) . . . ? F1 F3 F5 59.5(2) . . . ? F2 F3 F5 60.3(2) . . . ? P1 F4 F1 45.5(2) . . . ? P1 F4 F6 45.2(2) . . . ? F1 F4 F6 61.7(3) . . . ? P1 F5 F1 45.1(2) . . . ? P1 F5 F2 44.0(2) . . . ? P1 F5 F3 45.0(2) . . . ? F1 F5 F2 89.0(3) . . . ? F1 F5 F3 59.9(3) . . . ? F2 F5 F3 59.1(3) . . . ? P1 F6 F2 44.1(2) . . . ? P1 F6 F4 44.6(2) . . . ? F2 F6 F4 60.4(3) . . . ? F7 P2 F8 177.9(2) . . . ? F7 P2 F9 89.1(2) . . . ? F7 P2 F10 90.6(2) . . . ? F7 P2 F11 90.5(2) . . . ? F7 P2 F12 90.4(2) . . . ? F8 P2 F9 88.8(2) . . . ? F8 P2 F10 91.5(3) . . . ? F8 P2 F11 89.9(2) . . . ? F8 P2 F12 89.2(2) . . . ? F9 P2 F10 179.4(3) . . . ? F9 P2 F11 90.5(2) . . . ? F9 P2 F12 89.5(2) . . . ? F10 P2 F11 89.0(2) . . . ? F10 P2 F12 91.0(2) . . . ? F11 P2 F12 179.2(2) . . . ? C30 C31 N7 178.8(8) . . . ? C32 C33 N8 178.7(8) . . . ? data_Complex_3 _database_code_depnum_ccdc_archive 'CCDC 218274' _audit_creation_date 25-09-03 #========================================================================== #==== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(tpy)(phen)(CN)][PF6] _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H21 F6 N6 O P Ru' _chemical_formula_weight 703.55 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1 #========================================================================== #==== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 8.6848(3) _cell_length_b 10.3229(7) _cell_length_c 16.632(1) _cell_angle_alpha 79.267(5) _cell_angle_beta 77.266(5) _cell_angle_gamma 68.952(5) _cell_volume 1347.9(1) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 6680 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.73 _exptl_crystal_density_method none _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #========================================================================== #==== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 6680 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 40 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.40 Omega = 0.00 Kappa = 0.00 91 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6680 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5280 _reflns_number_gt 4174 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #========================================================================== #==== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4174 _refine_ls_number_parameters 388 _refine_ls_number_restraints 8 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_all 0.078 _refine_ls_wR_factor_ref 0.038 _refine_ls_goodness_of_fit_all 1.102 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.446 _refine_diff_density_min -0.182 #========================================================================== #==== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RU 0.43415(2) 0.42475(2) 0.79479(1) 0.01622(9) Uani ? ? Ru N1 0.5300(2) 0.2609(2) 0.7198(1) 0.017(1) Uani ? ? N C1 0.5247(3) 0.1310(3) 0.7377(2) 0.023(1) Uani ? ? C C2 0.5943(3) 0.0315(3) 0.6818(2) 0.029(1) Uani ? ? C C3 0.6753(3) 0.0651(3) 0.6041(2) 0.029(1) Uani ? ? C C4 0.6832(3) 0.2012(3) 0.5818(2) 0.024(1) Uani ? ? C C5 0.7612(3) 0.2479(3) 0.5022(2) 0.031(1) Uani ? ? C C6 0.7617(3) 0.3810(4) 0.4833(2) 0.030(1) Uani ? ? C C7 0.6840(3) 0.4818(3) 0.5418(2) 0.027(1) Uani ? ? C C8 0.6744(3) 0.6230(3) 0.5250(2) 0.031(1) Uani ? ? C C9 0.5906(3) 0.7112(3) 0.5845(2) 0.029(1) Uani ? ? C C10 0.5198(3) 0.6591(3) 0.6615(2) 0.023(1) Uani ? ? C N2 0.5289(2) 0.5249(2) 0.6815(1) 0.0178(9) Uani ? ? N C11 0.6073(3) 0.4374(3) 0.6215(2) 0.020(1) Uani ? ? C C12 0.6071(3) 0.2962(3) 0.6414(2) 0.020(1) Uani ? ? C N3 0.1930(2) 0.5143(2) 0.7679(1) 0.019(1) Uani ? ? N C13 0.1135(3) 0.4619(3) 0.7277(2) 0.022(1) Uani ? ? C C14 -0.0469(3) 0.5344(3) 0.7111(2) 0.027(1) Uani ? ? C C15 -0.1290(3) 0.6646(3) 0.7375(2) 0.029(1) Uani ? ? C C16 -0.0522(3) 0.7203(3) 0.7805(2) 0.026(1) Uani ? ? C C17 0.1094(3) 0.6425(3) 0.7955(2) 0.020(1) Uani ? ? C C18 0.2014(3) 0.6907(3) 0.8421(2) 0.019(1) Uani ? ? C C19 0.1490(3) 0.8182(3) 0.8736(2) 0.026(1) Uani ? ? C C20 0.2579(3) 0.8460(3) 0.9131(2) 0.030(1) Uani ? ? C C21 0.4143(3) 0.7481(3) 0.9210(2) 0.028(1) Uani ? ? C C22 0.4621(3) 0.6221(3) 0.8890(2) 0.020(1) Uani ? ? C N4 0.3546(2) 0.5952(2) 0.8508(1) 0.018(1) Uani ? ? N C23 0.6233(3) 0.5063(3) 0.8895(2) 0.020(1) Uani ? ? C C24 0.7483(3) 0.5044(3) 0.9305(2) 0.025(1) Uani ? ? C C25 0.8952(3) 0.3917(3) 0.9279(2) 0.028(1) Uani ? ? C C26 0.9154(3) 0.2836(3) 0.8849(2) 0.025(1) Uani ? ? C C27 0.7884(3) 0.2891(3) 0.8448(2) 0.022(1) Uani ? ? C N5 0.6436(2) 0.3986(2) 0.8464(1) 0.018(1) Uani ? ? N C28 0.3606(3) 0.3016(3) 0.8924(2) 0.019(1) Uani ? ? C N6 0.3256(3) 0.2225(3) 0.9466(1) 0.030(1) Uani ? ? N P 0.12150(9) 0.08239(8) 0.65601(5) 0.0267(3) Uani ? ? P F1 -0.0391(2) 0.0546(2) 0.7132(1) 0.054(1) Uani ? ? F F2 0.2266(2) -0.0797(2) 0.6713(1) 0.050(1) Uani ? ? F F3 0.0673(2) 0.0565(2) 0.5762(1) 0.048(1) Uani ? ? F F4 0.2818(2) 0.1100(3) 0.5991(1) 0.070(1) Uani ? ? F F5 0.0144(2) 0.2451(2) 0.6418(1) 0.052(1) Uani ? ? F F6 0.1749(2) 0.1077(2) 0.7367(1) 0.055(1) Uani ? ? F O -0.2889(3) -0.0178(3) 0.9155(2) 0.049(1) Uani ? ? O H01 -0.3900 0.0632 0.9201 0.0732 Uiso ? ? H H02 -0.3065 -0.0847 0.9644 0.0732 Uiso ? ? H H1 0.4706 0.1049 0.7912 0.0310 Uiso calc C1 H H2 0.5858 -0.0593 0.6974 0.0393 Uiso calc C2 H H3 0.7251 -0.0026 0.5660 0.0385 Uiso calc C3 H H4 0.8136 0.1844 0.4619 0.0416 Uiso calc C5 H H5 0.8150 0.4087 0.4300 0.0428 Uiso calc C6 H H6 0.7256 0.6570 0.4728 0.0402 Uiso calc C8 H H7 0.5810 0.8072 0.5733 0.0365 Uiso calc C9 H H8 0.4621 0.7219 0.7018 0.0288 Uiso calc C10 H H9 0.1698 0.3717 0.7100 0.0282 Uiso calc C13 H H10 -0.0993 0.4952 0.6822 0.0338 Uiso calc C14 H H11 -0.2386 0.7163 0.7263 0.0403 Uiso calc C15 H H12 -0.1084 0.8096 0.7993 0.0354 Uiso calc C16 H H13 0.0417 0.8847 0.8684 0.0349 Uiso calc C19 H H14 0.2247 0.9327 0.9347 0.0400 Uiso calc C20 H H15 0.4880 0.7674 0.9480 0.0350 Uiso calc C21 H H16 0.7326 0.5799 0.9600 0.0324 Uiso calc C24 H H17 0.9812 0.3890 0.9556 0.0376 Uiso calc C25 H H18 1.0157 0.2055 0.8826 0.0360 Uiso calc C26 H H19 0.8036 0.2137 0.8153 0.0293 Uiso calc C27 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RU 0.01642(9) 0.01673(9) 0.01554(9) -0.00459(7) -0.00323(7) -0.00303(7) Ru N1 0.0147(9) 0.017(1) 0.020(1) -0.0037(7) -0.0038(7) -0.0039(8) N C1 0.025(1) 0.018(1) 0.028(1) -0.005(1) -0.007(1) -0.002(1) C C2 0.030(1) 0.019(1) 0.043(2) -0.007(1) -0.011(1) -0.006(1) C C3 0.025(1) 0.026(1) 0.037(1) -0.002(1) -0.006(1) -0.016(1) C C4 0.020(1) 0.028(1) 0.026(1) -0.003(1) -0.005(1) -0.010(1) C C5 0.030(1) 0.038(2) 0.026(1) -0.005(1) -0.003(1) -0.017(1) C C6 0.033(1) 0.044(2) 0.019(1) -0.012(1) 0.004(1) -0.006(1) C C7 0.028(1) 0.033(1) 0.021(1) -0.010(1) -0.005(1) -0.004(1) C C8 0.038(1) 0.035(1) 0.022(1) -0.018(1) -0.007(1) 0.006(1) C C9 0.034(1) 0.024(1) 0.029(1) -0.014(1) -0.011(1) 0.005(1) C C10 0.021(1) 0.024(1) 0.024(1) -0.0076(9) -0.0093(9) -0.002(1) C N2 0.0155(9) 0.018(1) 0.020(1) -0.0050(7) -0.0070(7) 0.0001(9) N C11 0.018(1) 0.025(1) 0.019(1) -0.0054(9) -0.0059(9) -0.004(1) C C12 0.016(1) 0.024(1) 0.020(1) -0.0055(9) -0.0051(9) -0.004(1) C N3 0.0189(9) 0.020(1) 0.018(1) -0.0073(8) -0.0031(8) -0.0000(9) N C13 0.027(1) 0.022(1) 0.019(1) -0.0117(9) -0.0023(9) -0.003(1) C C14 0.025(1) 0.031(1) 0.027(1) -0.014(1) -0.0096(9) 0.001(1) C C15 0.021(1) 0.027(1) 0.045(2) -0.004(1) -0.015(1) -0.000(1) C C16 0.023(1) 0.022(1) 0.035(1) -0.003(1) -0.008(1) -0.004(1) C C17 0.020(1) 0.020(1) 0.020(1) -0.0075(9) -0.0039(9) 0.000(1) C C18 0.021(1) 0.019(1) 0.018(1) -0.0054(9) -0.0036(9) -0.003(1) C C19 0.023(1) 0.024(1) 0.030(1) -0.001(1) -0.006(1) -0.007(1) C C20 0.039(1) 0.021(1) 0.033(1) -0.004(1) -0.009(1) -0.013(1) C C21 0.029(1) 0.028(1) 0.027(1) -0.008(1) -0.011(1) -0.008(1) C C22 0.022(1) 0.023(1) 0.016(1) -0.0083(9) -0.0031(9) -0.005(1) C N4 0.0158(9) 0.020(1) 0.018(1) -0.0048(7) -0.0008(7) -0.0047(8) N C23 0.019(1) 0.024(1) 0.017(1) -0.0091(9) -0.0023(9) -0.004(1) C C24 0.023(1) 0.031(1) 0.022(1) -0.008(1) -0.0042(9) -0.007(1) C C25 0.022(1) 0.042(2) 0.025(1) -0.012(1) -0.0072(9) -0.001(1) C C26 0.018(1) 0.031(2) 0.029(1) -0.001(1) -0.007(1) -0.001(1) C C27 0.021(1) 0.022(1) 0.022(1) -0.006(1) -0.000(1) -0.004(1) C N5 0.0156(9) 0.022(1) 0.017(1) -0.0038(8) -0.0010(8) -0.0022(9) N C28 0.015(1) 0.022(1) 0.021(1) -0.0027(9) -0.0050(9) -0.007(1) C N6 0.035(1) 0.035(1) 0.021(1) -0.0155(9) -0.0047(9) 0.004(1) N P 0.0256(3) 0.0243(4) 0.0306(4) -0.0060(3) -0.0041(3) -0.0035(3) P F1 0.0412(9) 0.070(1) 0.054(1) -0.0288(8) 0.0042(8) -0.014(1) F F2 0.073(1) 0.033(1) 0.052(1) 0.016(1) -0.0137(9) -0.007(1) F F3 0.051(1) 0.051(1) 0.0429(9) 0.0023(9) -0.0161(7) -0.0223(8) F F4 0.0435(9) 0.121(2) 0.065(1) -0.043(1) -0.0082(9) 0.030(1) F F5 0.078(1) 0.024(1) 0.075(1) -0.0002(9) -0.0389(8) -0.0100(9) F F6 0.0528(9) 0.059(1) 0.053(1) -0.0153(8) -0.0250(7) -0.0115(9) F O 0.057(1) 0.044(1) 0.048(1) -0.007(1) 0.008(1) 0.015(1) O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU N1 2.104(2) . . ? RU N2 2.121(2) . . ? RU N3 2.076(2) . . ? RU N4 1.973(2) . . ? RU N5 2.090(2) . . ? RU C28 2.004(3) . . ? N1 C1 1.334(4) . . ? N1 C12 1.376(4) . . ? C1 C2 1.394(4) . . ? C2 C3 1.376(4) . . ? C3 C4 1.407(5) . . ? C4 C5 1.431(4) . . ? C4 C12 1.411(4) . . ? C5 C6 1.352(5) . . ? C6 C7 1.437(4) . . ? C7 C8 1.408(5) . . ? C7 C11 1.419(4) . . ? C8 C9 1.371(5) . . ? C9 C10 1.392(4) . . ? C10 N2 1.341(4) . . ? N2 C11 1.367(4) . . ? C11 C12 1.434(4) . . ? N3 C13 1.351(4) . . ? N3 C17 1.370(4) . . ? C13 C14 1.386(4) . . ? C14 C15 1.379(5) . . ? C15 C16 1.388(4) . . ? C16 C17 1.395(4) . . ? C17 C18 1.480(4) . . ? C18 C19 1.391(4) . . ? C18 N4 1.361(4) . . ? C19 C20 1.395(4) . . ? C20 C21 1.388(4) . . ? C21 C22 1.385(4) . . ? C22 N4 1.366(4) . . ? C22 C23 1.479(4) . . ? C23 C24 1.398(4) . . ? C23 N5 1.371(4) . . ? C24 C25 1.382(4) . . ? C25 C26 1.375(5) . . ? C26 C27 1.390(4) . . ? C27 N5 1.355(4) . . ? C28 N6 1.164(4) . . ? P F1 1.592(2) . . ? P F2 1.595(2) . . ? P F3 1.599(2) . . ? P F4 1.587(2) . . ? P F5 1.603(2) . . ? P F6 1.604(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 RU N2 78.66(9) . . . ? N1 RU N3 100.31(9) . . . ? N1 RU N4 171.73(9) . . . ? N1 RU N5 100.97(9) . . . ? N1 RU C28 91.9(1) . . . ? N2 RU N3 90.67(8) . . . ? N2 RU N4 93.08(9) . . . ? N2 RU N5 91.87(8) . . . ? N2 RU C28 170.6(1) . . . ? N3 RU N4 79.35(9) . . . ? N3 RU N5 158.7(1) . . . ? N3 RU C28 91.7(1) . . . ? N4 RU N5 79.35(9) . . . ? N4 RU C28 96.3(1) . . . ? N5 RU C28 89.3(1) . . . ? RU N1 C1 129.2(2) . . . ? RU N1 C12 113.8(2) . . . ? C1 N1 C12 117.0(3) . . . ? N1 C1 C2 123.4(3) . . . ? C1 C2 C3 120.0(3) . . . ? C2 C3 C4 119.0(3) . . . ? C3 C4 C5 123.6(3) . . . ? C3 C4 C12 117.5(3) . . . ? C5 C4 C12 118.9(3) . . . ? C4 C5 C6 121.2(3) . . . ? C5 C6 C7 121.8(3) . . . ? C6 C7 C8 124.6(3) . . . ? C6 C7 C11 118.0(3) . . . ? C8 C7 C11 117.3(3) . . . ? C7 C8 C9 119.5(3) . . . ? C8 C9 C10 119.6(3) . . . ? C9 C10 N2 123.3(3) . . . ? RU N2 C10 129.2(2) . . . ? RU N2 C11 113.5(2) . . . ? C10 N2 C11 117.3(2) . . . ? C7 C11 N2 122.8(3) . . . ? C7 C11 C12 120.1(3) . . . ? N2 C11 C12 117.1(3) . . . ? N1 C12 C4 123.2(3) . . . ? N1 C12 C11 116.8(3) . . . ? C4 C12 C11 120.0(3) . . . ? RU N3 C13 128.1(2) . . . ? RU N3 C17 113.4(2) . . . ? C13 N3 C17 118.5(2) . . . ? N3 C13 C14 122.6(3) . . . ? C13 C14 C15 118.6(3) . . . ? C14 C15 C16 120.3(3) . . . ? C15 C16 C17 118.6(3) . . . ? N3 C17 C16 121.4(3) . . . ? N3 C17 C18 115.5(3) . . . ? C16 C17 C18 123.1(3) . . . ? C17 C18 C19 127.3(3) . . . ? C17 C18 N4 112.3(3) . . . ? C19 C18 N4 120.4(3) . . . ? C18 C19 C20 118.4(3) . . . ? C19 C20 C21 120.6(3) . . . ? C20 C21 C22 119.4(3) . . . ? C21 C22 N4 119.8(3) . . . ? C21 C22 C23 127.7(3) . . . ? N4 C22 C23 112.5(2) . . . ? RU N4 C18 119.1(2) . . . ? RU N4 C22 119.0(2) . . . ? C18 N4 C22 121.4(3) . . . ? C22 C23 C24 123.3(3) . . . ? C22 C23 N5 115.5(2) . . . ? C24 C23 N5 121.2(3) . . . ? C23 C24 C25 119.5(3) . . . ? C24 C25 C26 119.3(3) . . . ? C25 C26 C27 119.7(3) . . . ? C26 C27 N5 122.0(3) . . . ? RU N5 C23 113.3(2) . . . ? RU N5 C27 128.3(2) . . . ? C23 N5 C27 118.4(2) . . . ? RU C28 N6 175.5(3) . . . ? F1 P F2 90.1(1) . . . ? F1 P F3 90.3(1) . . . ? F1 P F4 180.00 . . . ? F1 P F5 89.3(1) . . . ? F1 P F6 89.2(1) . . . ? F2 P F3 90.4(1) . . . ? F2 P F4 89.9(1) . . . ? F2 P F5 179.3(1) . . . ? F2 P F6 89.5(1) . . . ? F3 P F4 89.8(1) . . . ? F3 P F5 90.0(1) . . . ? F3 P F6 179.5(1) . . . ? F4 P F5 90.8(1) . . . ? F4 P F6 90.7(1) . . . ? F5 P F6 90.2(1) . . . ? #===END data_Complex_4 _database_code_depnum_ccdc_archive 'CCDC 218275' _audit_creation_date 26-09-03 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(terpy)(phen)(py)][PF6]2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H30 F12 N6 P2 Ru' _chemical_formula_weight 961.70 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1 #========================================================================== #==== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 15.3374(5) _cell_length_b 19.8829(8) _cell_length_c 12.9446(4) _cell_angle_alpha 90 _cell_angle_beta 105.241(5) _cell_angle_gamma 90 _cell_volume 3808.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 8974 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.68 _exptl_crystal_density_method none _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #========================================================================== #==== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 8974 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.9 deg 1 scans of 50 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.40 Omega = 0.00 Kappa = 0.00 95 frames Set 2 Theta = -6.40 Kappa = 109.00 Phi = 0.00 13 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8974 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8974 _reflns_number_gt 4761 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #========================================================================== #==== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4761 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.103 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_all 0.267 _refine_ls_wR_factor_ref 0.061 _refine_ls_goodness_of_fit_all 1.122 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.734 _refine_diff_density_min -0.168 #========================================================================== #==== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RU 0.28554(2) 0.03759(2) 0.64962(3) 0.0204(2) Uani ? ? Ru N1 0.2315(2) 0.1306(2) 0.6815(3) 0.024(2) Uani ? ? N C1 0.2627(3) 0.1738(2) 0.7618(3) 0.027(2) Uani ? ? C C2 0.2154(3) 0.2316(2) 0.7759(4) 0.039(3) Uani ? ? C C3 0.1334(3) 0.2468(2) 0.7066(4) 0.040(3) Uani ? ? C C4 0.0966(3) 0.2010(2) 0.6205(4) 0.032(2) Uani ? ? C C5 0.0122(3) 0.2118(3) 0.5419(5) 0.045(3) Uani ? ? C C6 -0.0179(3) 0.1672(3) 0.4622(4) 0.039(3) Uani ? ? C C7 0.0307(3) 0.1063(2) 0.4550(4) 0.031(2) Uani ? ? C C8 0.0010(3) 0.0568(3) 0.3758(4) 0.035(3) Uani ? ? C C9 0.0499(3) -0.0013(3) 0.3793(3) 0.032(2) Uani ? ? C C10 0.1287(3) -0.0108(2) 0.4608(3) 0.029(2) Uani ? ? C N2 0.1615(2) 0.0362(2) 0.5364(3) 0.024(2) Uani ? ? N C11 0.1121(2) 0.0947(2) 0.5321(3) 0.024(2) Uani ? ? C C12 0.1479(3) 0.1440(2) 0.6126(3) 0.026(2) Uani ? ? C N3 0.3404(2) 0.0575(2) 0.5213(3) 0.022(2) Uani ? ? N C13 0.3493(3) 0.1176(2) 0.4756(3) 0.029(2) Uani ? ? C C14 0.3860(3) 0.1241(2) 0.3891(4) 0.030(2) Uani ? ? C C15 0.4129(3) 0.0661(3) 0.3451(3) 0.033(2) Uani ? ? C C16 0.4031(3) 0.0045(2) 0.3900(3) 0.029(2) Uani ? ? C C17 0.3679(3) 0.0006(2) 0.4782(3) 0.022(2) Uani ? ? C C18 0.3566(2) -0.0630(2) 0.5316(3) 0.023(2) Uani ? ? C C19 0.3780(3) -0.1275(2) 0.5056(3) 0.029(2) Uani ? ? C C20 0.3607(3) -0.1822(2) 0.5632(4) 0.033(2) Uani ? ? C C21 0.3212(3) -0.1718(2) 0.6482(4) 0.032(2) Uani ? ? C C22 0.3004(2) -0.1065(2) 0.6723(3) 0.025(2) Uani ? ? C N4 0.3193(2) -0.0544(2) 0.6157(3) 0.024(2) Uani ? ? N C23 0.2574(3) -0.0866(2) 0.7572(3) 0.027(2) Uani ? ? C C24 0.2322(3) -0.1311(2) 0.8260(4) 0.029(2) Uani ? ? C C25 0.1919(3) -0.1075(3) 0.9032(3) 0.034(2) Uani ? ? C C26 0.1789(3) -0.0392(3) 0.9106(4) 0.038(3) Uani ? ? C C27 0.2057(3) 0.0037(3) 0.8396(3) 0.031(2) Uani ? ? C N5 0.2435(2) -0.0181(2) 0.7636(3) 0.024(2) Uani ? ? N N6 0.4147(2) 0.0542(2) 0.7548(3) 0.023(2) Uani ? ? N C28 0.4595(3) 0.0096(2) 0.8270(3) 0.026(2) Uani ? ? C C29 0.5471(3) 0.0195(2) 0.8858(4) 0.032(3) Uani ? ? C C30 0.5922(3) 0.0773(3) 0.8722(4) 0.034(3) Uani ? ? C C31 0.5468(3) 0.1246(2) 0.8004(4) 0.031(2) Uani ? ? C C32 0.4590(3) 0.1120(2) 0.7434(3) 0.027(2) Uani ? ? C P1 0.82600(9) 0.16054(7) 0.7483(1) 0.0413(8) Uani ? ? P F1 0.8226(4) 0.1509(4) 0.8632(3) 0.132(4) Uani ? ? F F2 0.8294(2) 0.1677(3) 0.6271(3) 0.102(3) Uani ? ? F F3 0.8744(3) 0.2291(2) 0.7753(5) 0.115(4) Uani ? ? F F4 0.7312(2) 0.1961(2) 0.7189(3) 0.081(2) Uani ? ? F F5 0.7768(3) 0.0924(2) 0.7093(4) 0.086(3) Uani ? ? F F6 0.9224(2) 0.1254(2) 0.7737(3) 0.088(3) Uani ? ? F P2 0.46353(8) 0.30418(7) 0.5680(1) 0.0337(7) Uani ? ? P F7 0.5567(2) 0.3402(2) 0.5704(3) 0.060(2) Uani ? ? F F8 0.4668(2) 0.3346(2) 0.6811(3) 0.081(2) Uani ? ? F F9 0.3704(2) 0.2672(2) 0.5645(3) 0.063(2) Uani ? ? F F10 0.4597(2) 0.2750(2) 0.4516(2) 0.065(2) Uani ? ? F F11 0.5165(2) 0.2381(2) 0.6193(2) 0.063(2) Uani ? ? F F12 0.4088(2) 0.3694(1) 0.5116(3) 0.057(2) Uani ? ? F C33 0.2235(3) 0.3968(3) 0.6177(4) 0.045(3) Uani ? ? C C34 0.1707(4) 0.4373(3) 0.6648(4) 0.047(3) Uani ? ? C C35 0.0788(3) 0.4422(3) 0.6163(4) 0.052(3) Uani ? ? C C36 0.0410(3) 0.4062(3) 0.5235(4) 0.045(3) Uani ? ? C C37 0.0938(3) 0.3670(3) 0.4778(4) 0.042(3) Uani ? ? C C38 0.1858(3) 0.3623(3) 0.5261(4) 0.045(3) Uani ? ? C H1 0.3193 0.1649 0.8112 0.0356 Uiso calc C1 H H2 0.2402 0.2608 0.8344 0.0506 Uiso calc C2 H H3 0.1018 0.2867 0.7153 0.0536 Uiso calc C3 H H4 -0.0226 0.2507 0.5461 0.0629 Uiso calc C5 H H5 -0.0727 0.1763 0.4095 0.0559 Uiso calc C6 H H6 -0.0527 0.0636 0.3201 0.0491 Uiso calc C8 H H7 0.0301 -0.0349 0.3262 0.0428 Uiso calc C9 H H8 0.1606 -0.0520 0.4633 0.0374 Uiso calc C10 H H9 0.3296 0.1570 0.5042 0.0381 Uiso calc C13 H H10 0.3926 0.1671 0.3602 0.0397 Uiso calc C14 H H11 0.4376 0.0689 0.2852 0.0443 Uiso calc C15 H H12 0.4206 -0.0354 0.3604 0.0380 Uiso calc C16 H H13 0.4047 -0.1342 0.4479 0.0374 Uiso calc C19 H H14 0.3754 -0.2264 0.5455 0.0452 Uiso calc C20 H H15 0.3088 -0.2087 0.6886 0.0447 Uiso calc C21 H H16 0.2424 -0.1779 0.8204 0.0395 Uiso calc C24 H H17 0.1737 -0.1379 0.9503 0.0446 Uiso calc C25 H H18 0.1520 -0.0217 0.9632 0.0497 Uiso calc C26 H H19 0.1967 0.0507 0.8453 0.0401 Uiso calc C27 H H20 0.4295 -0.0305 0.8381 0.0352 Uiso calc C28 H H21 0.5766 -0.0135 0.9359 0.0436 Uiso calc C29 H H22 0.6532 0.0843 0.9114 0.0492 Uiso calc C30 H H23 0.5757 0.1654 0.7903 0.0405 Uiso calc C31 H H24 0.4281 0.1450 0.6941 0.0362 Uiso calc C32 H H25 0.2865 0.3932 0.6499 0.0620 Uiso calc C33 H H26 0.1972 0.4612 0.7289 0.0665 Uiso calc C34 H H27 0.0418 0.4702 0.6467 0.0685 Uiso calc C35 H H28 -0.0222 0.4088 0.4916 0.0597 Uiso calc C36 H H29 0.0678 0.3432 0.4134 0.0557 Uiso calc C37 H H30 0.2228 0.3348 0.4949 0.0568 Uiso calc C38 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RU 0.0218(1) 0.0197(2) 0.0197(1) 0.0011(2) 0.0050(1) -0.0019(2) Ru N1 0.026(2) 0.023(2) 0.022(2) 0.003(2) 0.007(1) 0.000(2) N C1 0.030(2) 0.027(2) 0.025(2) 0.001(2) 0.007(2) -0.003(2) C C2 0.045(2) 0.031(3) 0.042(3) 0.001(2) 0.013(2) -0.011(2) C C3 0.046(2) 0.023(3) 0.060(3) 0.013(2) 0.024(2) -0.003(2) C C4 0.036(2) 0.020(2) 0.046(3) -0.000(2) 0.012(2) 0.005(2) C C5 0.035(2) 0.038(3) 0.070(4) 0.014(2) 0.009(2) 0.014(3) C C6 0.035(2) 0.035(3) 0.050(3) 0.008(2) -0.006(2) 0.003(3) C C7 0.028(2) 0.034(3) 0.032(2) -0.000(2) 0.005(2) 0.009(2) C C8 0.026(2) 0.051(3) 0.033(3) -0.003(2) 0.002(2) 0.002(2) C C9 0.030(2) 0.043(3) 0.025(2) -0.008(2) 0.006(2) -0.010(2) C C10 0.029(2) 0.032(2) 0.027(2) -0.007(2) 0.011(2) -0.009(2) C N2 0.024(2) 0.026(2) 0.024(2) -0.004(2) 0.007(1) -0.002(2) N C11 0.022(2) 0.023(2) 0.028(2) -0.002(2) 0.008(2) 0.004(2) C C12 0.026(2) 0.022(2) 0.029(2) 0.001(2) 0.011(2) 0.003(2) C N3 0.022(2) 0.024(2) 0.019(2) 0.003(2) 0.005(1) -0.001(2) N C13 0.031(2) 0.031(3) 0.025(2) 0.003(2) 0.005(2) -0.002(2) C C14 0.031(2) 0.032(3) 0.028(2) -0.004(2) 0.006(2) 0.005(2) C C15 0.031(2) 0.050(3) 0.024(2) 0.001(2) 0.011(2) -0.003(2) C C16 0.028(2) 0.034(3) 0.026(2) 0.011(2) 0.008(2) 0.000(2) C C17 0.019(2) 0.029(3) 0.019(2) 0.002(2) 0.000(2) -0.003(2) C C18 0.019(2) 0.025(2) 0.024(2) 0.006(2) 0.005(2) -0.003(2) C C19 0.025(2) 0.033(3) 0.030(2) -0.001(2) 0.008(2) -0.008(2) C C20 0.036(2) 0.023(2) 0.045(3) 0.007(2) 0.010(2) -0.008(2) C C21 0.036(2) 0.022(2) 0.042(3) -0.003(2) 0.005(2) 0.001(2) C C22 0.026(2) 0.023(2) 0.027(2) -0.003(2) 0.007(2) 0.002(2) C N4 0.023(2) 0.022(2) 0.026(2) 0.004(2) 0.003(1) -0.003(2) N C23 0.026(2) 0.030(3) 0.025(2) -0.001(2) 0.001(2) -0.000(2) C C24 0.030(2) 0.024(3) 0.035(2) -0.003(2) 0.005(2) 0.005(2) C C25 0.037(2) 0.040(3) 0.026(2) -0.007(2) 0.008(2) 0.007(2) C C26 0.030(2) 0.055(3) 0.031(2) -0.005(2) 0.013(2) -0.006(3) C C27 0.029(2) 0.032(3) 0.031(2) -0.006(2) 0.008(2) -0.006(2) C N5 0.022(2) 0.028(2) 0.024(2) 0.001(2) 0.007(1) -0.003(2) N N6 0.028(2) 0.021(2) 0.021(2) 0.001(2) 0.005(1) 0.000(2) N C28 0.032(2) 0.026(2) 0.022(2) 0.000(2) 0.006(2) 0.001(2) C C29 0.032(2) 0.029(3) 0.035(3) 0.006(2) 0.002(2) 0.000(2) C C30 0.025(2) 0.043(3) 0.037(3) 0.003(2) -0.007(2) -0.006(3) C C31 0.033(2) 0.028(3) 0.033(2) -0.006(2) 0.008(2) -0.007(2) C C32 0.036(2) 0.028(2) 0.019(2) 0.003(2) 0.006(2) -0.002(2) C P1 0.0475(7) 0.0355(8) 0.0416(8) 0.0047(7) 0.0013(6) -0.0093(7) P F1 0.175(4) 0.385(9) 0.034(2) 0.076(5) 0.033(2) 0.037(4) F F2 0.075(2) 0.203(5) 0.068(2) -0.007(3) 0.017(2) 0.028(3) F F3 0.081(3) 0.064(3) 0.295(6) -0.000(2) -0.046(3) -0.067(3) F F4 0.056(2) 0.078(2) 0.120(3) 0.026(2) -0.003(2) -0.054(2) F F5 0.107(3) 0.038(2) 0.155(4) -0.012(2) -0.006(3) 0.001(3) F F6 0.069(2) 0.105(3) 0.093(3) 0.041(2) -0.024(2) -0.035(2) F P2 0.0345(6) 0.0279(7) 0.0399(7) 0.0020(6) 0.0091(5) -0.0029(6) P F7 0.043(1) 0.067(2) 0.077(2) -0.015(2) 0.016(1) 0.002(2) F F8 0.110(2) 0.084(3) 0.057(2) -0.005(2) 0.038(2) -0.029(2) F F9 0.044(1) 0.041(2) 0.142(3) -0.007(1) 0.035(2) -0.013(2) F F10 0.093(2) 0.067(2) 0.044(2) -0.003(2) 0.013(2) -0.018(2) F F11 0.067(2) 0.052(2) 0.071(2) 0.026(2) 0.028(1) 0.029(2) F F12 0.061(2) 0.032(2) 0.094(3) 0.009(2) 0.000(2) 0.006(2) F C33 0.038(2) 0.068(4) 0.036(3) 0.005(3) 0.007(2) 0.006(3) C C34 0.070(3) 0.049(3) 0.031(3) 0.001(3) 0.006(2) -0.006(3) C C35 0.058(3) 0.063(4) 0.039(3) 0.017(3) 0.016(2) -0.004(3) C C36 0.035(2) 0.055(4) 0.048(3) 0.003(3) 0.011(2) 0.005(3) C C37 0.049(3) 0.046(3) 0.032(3) -0.002(3) 0.008(2) -0.001(3) C C38 0.043(2) 0.052(3) 0.040(3) 0.017(2) 0.017(2) 0.003(3) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU N1 2.112(4) . . ? RU N2 2.074(4) . . ? RU N3 2.088(4) . . ? RU N4 1.981(4) . . ? RU N5 2.078(4) . . ? RU N6 2.113(4) . . ? N1 C1 1.337(6) . . ? N1 C12 1.382(6) . . ? C1 C2 1.396(7) . . ? C2 C3 1.373(7) . . ? C3 C4 1.435(7) . . ? C4 C5 1.436(7) . . ? C4 C12 1.398(6) . . ? C5 C6 1.345(8) . . ? C6 C7 1.439(7) . . ? C7 C8 1.407(7) . . ? C7 C11 1.398(6) . . ? C8 C9 1.372(7) . . ? C9 C10 1.393(7) . . ? C10 N2 1.351(6) . . ? N2 C11 1.381(6) . . ? C11 C12 1.432(6) . . ? N3 C13 1.356(6) . . ? N3 C17 1.376(6) . . ? C13 C14 1.385(6) . . ? C14 C15 1.396(7) . . ? C15 C16 1.380(7) . . ? C16 C17 1.387(6) . . ? C17 C18 1.473(7) . . ? C18 C19 1.388(6) . . ? C18 N4 1.367(6) . . ? C19 C20 1.383(7) . . ? C20 C21 1.403(7) . . ? C21 C22 1.390(7) . . ? C22 N4 1.344(6) . . ? C22 C23 1.477(6) . . ? C23 C24 1.381(6) . . ? C23 N5 1.385(6) . . ? C24 C25 1.387(7) . . ? C25 C26 1.381(7) . . ? C26 C27 1.392(7) . . ? C27 N5 1.338(6) . . ? N6 C28 1.339(6) . . ? N6 C32 1.365(6) . . ? C28 C29 1.373(6) . . ? C29 C30 1.376(7) . . ? C30 C31 1.376(7) . . ? C31 C32 1.378(6) . . ? P1 F1 1.514(5) . . ? P1 F2 1.590(4) . . ? P1 F3 1.548(5) . . ? P1 F4 1.571(4) . . ? P1 F5 1.568(4) . . ? P1 F6 1.589(4) . . ? F1 F3 2.196(9) . . ? F1 F4 2.210(7) . . ? F1 F6 2.208(7) . . ? F2 F5 2.117(6) . . ? F2 F6 2.218(6) . . ? F3 F6 2.192(6) . . ? F4 F5 2.192(5) . . ? P2 F7 1.591(3) . . ? P2 F8 1.572(4) . . ? P2 F9 1.596(3) . . ? P2 F10 1.602(4) . . ? P2 F11 1.595(3) . . ? P2 F12 1.612(3) . . ? C33 C34 1.390(8) . . ? C33 C38 1.361(8) . . ? C34 C35 1.388(8) . . ? C35 C36 1.388(8) . . ? C36 C37 1.366(7) . . ? C37 C38 1.389(7) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 RU N2 79.4(1) . . . ? N1 RU N3 104.5(1) . . . ? N1 RU N4 172.2(1) . . . ? N1 RU N5 96.7(1) . . . ? N1 RU N6 95.0(1) . . . ? N2 RU N3 85.8(1) . . . ? N2 RU N4 94.3(1) . . . ? N2 RU N5 95.6(1) . . . ? N2 RU N6 170.9(1) . . . ? N3 RU N4 79.4(2) . . . ? N3 RU N5 158.6(1) . . . ? N3 RU N6 88.7(1) . . . ? N4 RU N5 79.2(1) . . . ? N4 RU N6 91.8(1) . . . ? N5 RU N6 92.2(1) . . . ? RU N1 C1 129.5(3) . . . ? RU N1 C12 112.9(3) . . . ? C1 N1 C12 117.4(4) . . . ? N1 C1 C2 122.6(4) . . . ? C1 C2 C3 120.9(5) . . . ? C2 C3 C4 118.3(4) . . . ? C3 C4 C5 123.6(5) . . . ? C3 C4 C12 117.2(5) . . . ? C5 C4 C12 119.2(5) . . . ? C4 C5 C6 120.6(5) . . . ? C5 C6 C7 121.7(5) . . . ? C6 C7 C8 124.2(5) . . . ? C6 C7 C11 118.2(5) . . . ? C8 C7 C11 117.5(5) . . . ? C7 C8 C9 119.7(4) . . . ? C8 C9 C10 119.8(5) . . . ? C9 C10 N2 122.6(5) . . . ? RU N2 C10 128.3(3) . . . ? RU N2 C11 114.1(3) . . . ? C10 N2 C11 117.2(4) . . . ? C7 C11 N2 123.1(4) . . . ? C7 C11 C12 120.4(4) . . . ? N2 C11 C12 116.5(4) . . . ? N1 C12 C4 123.6(4) . . . ? N1 C12 C11 116.8(4) . . . ? C4 C12 C11 119.6(4) . . . ? RU N3 C13 128.5(3) . . . ? RU N3 C17 113.4(3) . . . ? C13 N3 C17 118.1(4) . . . ? N3 C13 C14 122.9(4) . . . ? C13 C14 C15 118.6(5) . . . ? C14 C15 C16 119.0(4) . . . ? C15 C16 C17 120.4(5) . . . ? N3 C17 C16 120.9(4) . . . ? N3 C17 C18 115.4(4) . . . ? C16 C17 C18 123.6(4) . . . ? C17 C18 C19 127.9(4) . . . ? C17 C18 N4 113.1(4) . . . ? C19 C18 N4 119.0(4) . . . ? C18 C19 C20 120.2(4) . . . ? C19 C20 C21 119.4(4) . . . ? C20 C21 C22 119.1(5) . . . ? C21 C22 N4 120.1(4) . . . ? C21 C22 C23 126.2(4) . . . ? N4 C22 C23 113.7(4) . . . ? RU N4 C18 118.7(3) . . . ? RU N4 C22 119.0(3) . . . ? C18 N4 C22 122.2(4) . . . ? C22 C23 C24 124.3(5) . . . ? C22 C23 N5 114.4(4) . . . ? C24 C23 N5 121.2(4) . . . ? C23 C24 C25 120.1(5) . . . ? C24 C25 C26 118.8(5) . . . ? C25 C26 C27 118.9(5) . . . ? C26 C27 N5 123.2(5) . . . ? RU N5 C23 113.6(3) . . . ? RU N5 C27 128.7(3) . . . ? C23 N5 C27 117.7(4) . . . ? RU N6 C28 124.7(3) . . . ? RU N6 C32 118.1(3) . . . ? C28 N6 C32 117.0(4) . . . ? N6 C28 C29 122.7(4) . . . ? C28 C29 C30 120.0(5) . . . ? C29 C30 C31 118.4(4) . . . ? C30 C31 C32 119.1(5) . . . ? N6 C32 C31 122.7(4) . . . ? F1 P1 F2 177.9(4) . . . ? F1 P1 F3 91.6(4) . . . ? F1 P1 F4 91.5(3) . . . ? F1 P1 F5 93.9(4) . . . ? F1 P1 F6 90.7(3) . . . ? F2 P1 F3 90.3(4) . . . ? F2 P1 F4 89.4(2) . . . ? F2 P1 F5 84.2(3) . . . ? F2 P1 F6 88.5(2) . . . ? F3 P1 F4 90.9(2) . . . ? F3 P1 F5 174.4(4) . . . ? F3 P1 F6 88.6(2) . . . ? F4 P1 F5 88.6(2) . . . ? F4 P1 F6 177.8(3) . . . ? F5 P1 F6 91.7(2) . . . ? P1 F1 F3 44.8(3) . . . ? P1 F1 F4 45.3(2) . . . ? P1 F1 F6 46.0(2) . . . ? F3 F1 F4 60.6(2) . . . ? F3 F1 F6 59.7(2) . . . ? F4 F1 F6 91.3(2) . . . ? P1 F2 F5 47.5(2) . . . ? P1 F2 F6 45.8(2) . . . ? F5 F2 F6 63.0(2) . . . ? P1 F3 F1 43.6(2) . . . ? P1 F3 F6 46.5(2) . . . ? F1 F3 F6 60.4(3) . . . ? P1 F4 F1 43.2(2) . . . ? P1 F4 F5 45.7(2) . . . ? F1 F4 F5 61.6(3) . . . ? P1 F5 F2 48.3(2) . . . ? P1 F5 F4 45.8(2) . . . ? F2 F5 F4 62.1(2) . . . ? P1 F6 F1 43.3(2) . . . ? P1 F6 F2 45.8(2) . . . ? P1 F6 F3 44.9(2) . . . ? F1 F6 F2 89.0(2) . . . ? F1 F6 F3 59.9(3) . . . ? F2 F6 F3 60.6(2) . . . ? F7 P2 F8 90.0(2) . . . ? F7 P2 F9 179.1(2) . . . ? F7 P2 F10 89.5(2) . . . ? F7 P2 F11 90.3(2) . . . ? F7 P2 F12 90.3(2) . . . ? F8 P2 F9 90.7(2) . . . ? F8 P2 F10 178.7(2) . . . ? F8 P2 F11 92.3(2) . . . ? F8 P2 F12 89.9(2) . . . ? F9 P2 F10 89.7(2) . . . ? F9 P2 F11 89.2(2) . . . ? F9 P2 F12 90.1(2) . . . ? F10 P2 F11 88.9(2) . . . ? F10 P2 F12 88.8(2) . . . ? F11 P2 F12 177.7(2) . . . ? C34 C33 C38 120.8(5) . . . ? C33 C34 C35 118.8(5) . . . ? C34 C35 C36 119.9(5) . . . ? C35 C36 C37 120.6(5) . . . ? C36 C37 C38 119.5(5) . . . ? C33 C38 C37 120.4(5) . . . ? #===END data_Complex_5 _database_code_depnum_ccdc_archive 'CCDC 218276' _audit_creation_date 26-09-03 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(terpy)(phen)(IQ)][PF6]2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C79 H60 Cl2 F24 N12 P4 Ru2' _chemical_formula_weight 2030.34 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1 #========================================================================== #==== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 14.0923(4) _cell_length_b 21.9960(8) _cell_length_c 25.6543(6) _cell_angle_alpha 90 _cell_angle_beta 99.395(5) _cell_angle_gamma 90 _cell_volume 7845.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 9212 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.72 _exptl_crystal_density_method none _exptl_crystal_F_000 4064 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #========================================================================== #==== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 9212 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.3 deg 1 scans of 50 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 139 frames Set 2 Theta = -6.30 Kappa = 134.00 Phi = 0.00 15 frames Friedel pairs were averaged. Internal R = 0.05 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9212 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9212 _reflns_number_gt 5096 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #========================================================================== #==== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5096 _refine_ls_number_parameters 564 _refine_ls_number_restraints 4 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.113 _refine_ls_R_factor_gt 0.052 _refine_ls_wR_factor_all 0.830 _refine_ls_wR_factor_ref 0.072 _refine_ls_goodness_of_fit_all 1.422 _refine_ls_goodness_of_fit_ref 1.309 _refine_ls_shift/su_max 0.008 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.580 _refine_diff_density_min -0.096 #========================================================================== #==== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RU 0.66428(3) 0.11456(2) 0.15181(1) 0.0243(2) 1.000 Uani ? ? Ru N1 0.5509(3) 0.0510(2) 0.1423(2) 0.027(2) 1.000 Uani ? ? N C1 0.5219(4) 0.0131(2) 0.1773(2) 0.034(3) 1.000 Uani ? ? C C2 0.4445(4) -0.0276(3) 0.1632(2) 0.041(3) 1.000 Uani ? ? C C3 0.3951(4) -0.0284(2) 0.1136(2) 0.037(3) 1.000 Uani ? ? C C4 0.4206(4) 0.0126(2) 0.0761(2) 0.036(3) 1.000 Uani ? ? C C5 0.3711(4) 0.0168(3) 0.0221(2) 0.043(3) 1.000 Uani ? ? C C6 0.3995(4) 0.0563(3) -0.0116(2) 0.045(3) 1.000 Uani ? ? C C7 0.4810(4) 0.0962(2) 0.0034(2) 0.035(3) 1.000 Uani ? ? C C8 0.5144(4) 0.1385(3) -0.0304(2) 0.042(3) 1.000 Uani ? ? C C9 0.5912(4) 0.1735(3) -0.0126(2) 0.044(3) 1.000 Uani ? ? C C10 0.6359(4) 0.1678(2) 0.0401(2) 0.036(3) 1.000 Uani ? ? C N2 0.6066(3) 0.1288(2) 0.0737(1) 0.027(2) 1.000 Uani ? ? N C11 0.5293(4) 0.0926(2) 0.0557(2) 0.031(3) 1.000 Uani ? ? C C12 0.5003(3) 0.0508(2) 0.0922(2) 0.027(2) 1.000 Uani ? ? C N3 0.5881(3) 0.1889(2) 0.1707(1) 0.028(2) 1.000 Uani ? ? N C13 0.4933(4) 0.1925(2) 0.1749(2) 0.034(3) 1.000 Uani ? ? C C14 0.4477(4) 0.2457(3) 0.1816(2) 0.038(3) 1.000 Uani ? ? C C15 0.5000(4) 0.2994(3) 0.1846(2) 0.041(3) 1.000 Uani ? ? C C16 0.5971(4) 0.2975(2) 0.1819(2) 0.035(3) 1.000 Uani ? ? C C17 0.6392(3) 0.2420(2) 0.1739(2) 0.027(3) 1.000 Uani ? ? C C18 0.7408(3) 0.2357(2) 0.1660(2) 0.029(3) 1.000 Uani ? ? C C19 0.8089(4) 0.2808(2) 0.1684(2) 0.036(3) 1.000 Uani ? ? C C20 0.8988(4) 0.2660(3) 0.1579(2) 0.042(3) 1.000 Uani ? ? C C21 0.9193(4) 0.2081(3) 0.1434(2) 0.039(3) 1.000 Uani ? ? C C22 0.8495(3) 0.1632(2) 0.1407(2) 0.028(3) 1.000 Uani ? ? C N4 0.7619(3) 0.1779(2) 0.1533(1) 0.027(2) 1.000 Uani ? ? N C23 0.8557(4) 0.0994(2) 0.1250(2) 0.031(3) 1.000 Uani ? ? C C24 0.9329(4) 0.0749(3) 0.1059(2) 0.039(3) 1.000 Uani ? ? C C25 0.9317(4) 0.0153(3) 0.0897(2) 0.045(3) 1.000 Uani ? ? C C26 0.8523(4) -0.0201(3) 0.0949(2) 0.041(3) 1.000 Uani ? ? C C27 0.7766(4) 0.0064(2) 0.1140(2) 0.034(3) 1.000 Uani ? ? C N5 0.7756(3) 0.0646(2) 0.1286(1) 0.027(2) 1.000 Uani ? ? N N6 0.7165(3) 0.0929(2) 0.2307(2) 0.028(2) 1.000 Uani ? ? N C28 0.7358(4) 0.0327(2) 0.2446(2) 0.034(3) 1.000 Uani ? ? C C29 0.7686(4) 0.0140(2) 0.2950(2) 0.032(3) 1.000 Uani ? ? C C30 0.7862(3) 0.0565(2) 0.3361(2) 0.032(3) 1.000 Uani ? ? C C31 0.8176(4) 0.0401(2) 0.3898(2) 0.038(3) 1.000 Uani ? ? C C32 0.8349(4) 0.0850(3) 0.4273(2) 0.041(3) 1.000 Uani ? ? C C33 0.8212(4) 0.1461(3) 0.4138(2) 0.043(3) 1.000 Uani ? ? C C34 0.7919(4) 0.1628(3) 0.3627(2) 0.038(3) 1.000 Uani ? ? C C35 0.7713(4) 0.1188(2) 0.3228(2) 0.032(3) 1.000 Uani ? ? C C36 0.7368(3) 0.1329(2) 0.2696(2) 0.028(3) 1.000 Uani ? ? C P1 0.6216(1) 0.36243(8) 0.03963(6) 0.0462(9) 1.000 Uani ? ? P F1 0.7059(4) 0.3134(3) 0.0532(2) 0.154(5) 1.000 Uani ? ? F F2 0.6558(5) 0.3888(2) 0.0953(2) 0.109(4) 1.000 Uani ? ? F F3 0.5625(4) 0.3116(2) 0.0617(2) 0.107(3) 1.000 Uani ? ? F F4 0.5982(5) 0.3344(2) -0.0162(2) 0.098(3) 1.000 Uani ? ? F F5 0.5470(4) 0.4099(3) 0.0249(2) 0.172(4) 1.000 Uani ? ? F F6 0.6925(4) 0.4073(2) 0.0173(2) 0.131(4) 1.000 Uani ? ? F P2 0.8137(1) 0.34940(7) 0.31277(6) 0.0381(8) 1.000 Uani ? ? P F7 0.8805(3) 0.3080(2) 0.3551(1) 0.065(2) 1.000 Uani ? ? F F8 0.7337(3) 0.3469(2) 0.3483(1) 0.077(2) 1.000 Uani ? ? F F9 0.7681(3) 0.2901(1) 0.2823(1) 0.056(2) 1.000 Uani ? ? F F10 0.8587(3) 0.4084(2) 0.3440(1) 0.062(2) 1.000 Uani ? ? F F11 0.8977(3) 0.3500(2) 0.2787(1) 0.094(3) 1.000 Uani ? ? F F12 0.7512(4) 0.3897(2) 0.2711(2) 0.085(3) 1.000 Uani ? ? F C37 0.3454(5) 0.2342(3) 0.0188(3) 0.061(4) 1.000 Uani ? ? C C38 0.3081(5) 0.2794(3) 0.0440(2) 0.062(4) 1.000 Uani ? ? C C39 0.2140(4) 0.2954(3) 0.0267(2) 0.054(4) 1.000 Uani ? ? C C40 0.013(1) 0.0136(7) 0.2718(5) 0.07(1) 0.500 Uani ? ? C CL1 -0.0286(3) -0.0399(2) 0.2262(2) 0.104(3) 0.500 Uani ? ? Cl CL2 0.0000 0.0864(1) 0.2500 0.074(2) 0.500 Uani ? ? Cl H1 0.5544 0.0135 0.2128 0.0452 1.000 Uiso calc C1 H H2 0.4271 -0.0546 0.1889 0.0539 1.000 Uiso calc C2 H H3 0.3438 -0.0563 0.1041 0.0504 1.000 Uiso calc C3 H H4 0.3177 -0.0090 0.0106 0.0590 1.000 Uiso calc C5 H H5 0.3650 0.0584 -0.0466 0.0623 1.000 Uiso calc C6 H H6 0.4828 0.1424 -0.0659 0.0588 1.000 Uiso calc C8 H H7 0.6147 0.2017 -0.0355 0.0604 1.000 Uiso calc C9 H H8 0.6897 0.1930 0.0524 0.0465 1.000 Uiso calc C10 H H9 0.4571 0.1559 0.1731 0.0450 1.000 Uiso calc C13 H H10 0.3812 0.2462 0.1841 0.0517 1.000 Uiso calc C14 H H11 0.4693 0.3372 0.1885 0.0529 1.000 Uiso calc C15 H H12 0.6344 0.3337 0.1855 0.0479 1.000 Uiso calc C16 H H13 0.7943 0.3213 0.1773 0.0465 1.000 Uiso calc C19 H H14 0.9473 0.2964 0.1606 0.0545 1.000 Uiso calc C20 H H15 0.9810 0.1987 0.1352 0.0527 1.000 Uiso calc C21 H H16 0.9877 0.0994 0.1038 0.0523 1.000 Uiso calc C24 H H17 0.9840 -0.0013 0.0753 0.0603 1.000 Uiso calc C25 H H18 0.8504 -0.0620 0.0855 0.0544 1.000 Uiso calc C26 H H19 0.7221 -0.0180 0.1169 0.0449 1.000 Uiso calc C27 H H20 0.7796 -0.0280 0.3022 0.0445 1.000 Uiso calc C29 H H21 0.8264 -0.0014 0.3996 0.0496 1.000 Uiso calc C31 H H22 0.8566 0.0743 0.4631 0.0571 1.000 Uiso calc C32 H H23 0.8324 0.1763 0.4405 0.0565 1.000 Uiso calc C33 H H24 0.7852 0.2047 0.3539 0.0500 1.000 Uiso calc C34 H H25 0.7272 0.1747 0.2607 0.0376 1.000 Uiso calc C36 H H26 0.7257 0.0028 0.2175 0.0444 1.000 Uiso calc C28 H H27 0.4098 0.2213 0.0302 0.0804 1.000 Uiso calc C37 H H28 0.3456 0.2997 0.0730 0.0824 1.000 Uiso calc C38 H H29 0.1862 0.3268 0.0447 0.0691 1.000 Uiso calc C39 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RU 0.0213(2) 0.0277(2) 0.0245(2) -0.0014(2) 0.0012(2) -0.0026(2) Ru N1 0.023(2) 0.026(2) 0.034(2) 0.002(2) 0.005(2) -0.003(2) N C1 0.030(3) 0.034(3) 0.039(3) -0.001(2) 0.003(2) -0.005(3) C C2 0.034(3) 0.035(3) 0.059(3) -0.004(3) 0.018(3) -0.000(3) C C3 0.028(3) 0.032(3) 0.056(3) -0.005(2) 0.006(3) -0.013(3) C C4 0.026(3) 0.036(3) 0.048(3) -0.004(2) 0.003(2) -0.009(3) C C5 0.032(3) 0.052(4) 0.049(3) -0.004(3) -0.002(3) -0.017(3) C C6 0.041(3) 0.053(4) 0.043(3) -0.005(3) -0.016(3) -0.013(3) C C7 0.033(3) 0.043(3) 0.030(3) 0.002(3) -0.005(2) -0.004(3) C C8 0.049(3) 0.055(4) 0.027(3) 0.007(3) -0.008(3) -0.002(3) C C9 0.052(3) 0.057(4) 0.030(3) 0.007(3) 0.003(3) 0.008(3) C C10 0.033(3) 0.040(3) 0.034(3) -0.000(3) 0.005(2) 0.002(3) C N2 0.026(2) 0.029(2) 0.027(2) -0.000(2) 0.002(2) -0.002(2) N C11 0.027(3) 0.035(3) 0.030(3) 0.001(2) 0.001(2) -0.004(2) C C12 0.024(2) 0.027(3) 0.031(2) 0.002(2) -0.004(2) -0.010(2) C N3 0.026(2) 0.032(2) 0.025(2) 0.001(2) 0.001(2) -0.002(2) N C13 0.026(3) 0.042(3) 0.036(3) 0.001(2) 0.006(2) -0.004(3) C C14 0.026(3) 0.052(3) 0.041(3) 0.006(3) 0.004(2) -0.002(3) C C15 0.044(3) 0.036(3) 0.043(3) 0.012(3) 0.011(3) -0.003(3) C C16 0.047(3) 0.026(3) 0.037(3) 0.003(3) 0.004(3) 0.000(2) C C17 0.030(3) 0.028(3) 0.023(2) 0.001(2) -0.000(2) -0.001(2) C C18 0.034(3) 0.030(3) 0.023(2) 0.002(2) 0.006(2) 0.002(2) C C19 0.040(3) 0.029(3) 0.039(3) -0.008(2) 0.009(2) -0.008(2) C C20 0.041(3) 0.038(3) 0.045(3) -0.015(3) 0.004(3) -0.002(3) C C21 0.027(3) 0.046(3) 0.050(3) -0.004(3) 0.008(2) -0.001(3) C C22 0.022(2) 0.039(3) 0.027(2) -0.003(2) 0.002(2) 0.003(2) C N4 0.026(2) 0.030(2) 0.024(2) -0.000(2) 0.001(2) -0.001(2) N C23 0.029(3) 0.035(3) 0.030(3) -0.001(2) 0.002(2) 0.001(2) C C24 0.028(3) 0.053(4) 0.041(3) -0.002(3) 0.008(2) -0.005(3) C C25 0.030(3) 0.058(4) 0.052(3) 0.010(3) 0.008(3) -0.005(3) C C26 0.033(3) 0.044(3) 0.049(3) 0.007(3) 0.006(3) -0.012(3) C C27 0.036(3) 0.035(3) 0.032(3) 0.000(3) 0.003(2) -0.006(2) C N5 0.025(2) 0.033(2) 0.024(2) -0.000(2) 0.000(2) -0.005(2) N N6 0.024(2) 0.029(2) 0.032(2) 0.000(2) 0.005(2) -0.001(2) N C28 0.032(3) 0.031(3) 0.040(3) -0.005(2) 0.007(2) -0.005(3) C C29 0.032(3) 0.023(3) 0.044(3) -0.004(2) -0.003(2) 0.003(2) C C30 0.027(3) 0.036(3) 0.033(3) 0.000(2) -0.000(2) 0.007(2) C C31 0.032(3) 0.041(3) 0.042(3) 0.002(3) 0.006(2) 0.009(3) C C32 0.040(3) 0.064(4) 0.028(3) -0.002(3) 0.005(2) 0.002(3) C C33 0.041(3) 0.054(4) 0.035(3) 0.005(3) 0.004(3) -0.013(3) C C34 0.038(3) 0.039(3) 0.037(3) 0.006(3) 0.001(2) -0.001(3) C C35 0.028(2) 0.038(3) 0.030(2) -0.000(2) 0.007(2) -0.000(2) C C36 0.026(2) 0.027(3) 0.033(3) 0.005(2) -0.002(2) -0.003(2) C P1 0.055(1) 0.0427(8) 0.0419(8) -0.0075(8) -0.0009(8) 0.0046(8) P F1 0.129(4) 0.133(4) 0.214(6) 0.042(4) 0.028(4) 0.069(4) F F2 0.338(7) 0.080(3) 0.048(2) -0.089(4) -0.029(4) 0.002(2) F F3 0.161(4) 0.124(3) 0.061(2) -0.082(3) 0.017(2) 0.008(2) F F4 0.290(7) 0.067(3) 0.049(2) -0.047(4) 0.033(3) -0.001(2) F F5 0.190(4) 0.227(5) 0.118(4) 0.159(3) 0.029(4) 0.029(4) F F6 0.147(4) 0.157(4) 0.098(3) -0.086(3) -0.008(3) 0.047(3) F P2 0.0395(8) 0.0339(8) 0.0412(7) -0.0103(7) 0.0051(7) -0.0028(7) P F7 0.060(2) 0.061(2) 0.075(2) 0.008(2) -0.017(2) -0.001(2) F F8 0.055(2) 0.094(3) 0.090(2) -0.020(2) 0.034(2) -0.028(2) F F9 0.072(2) 0.050(2) 0.049(2) -0.025(2) 0.001(2) -0.008(2) F F10 0.066(2) 0.046(2) 0.078(2) -0.021(2) 0.012(2) -0.023(2) F F11 0.088(3) 0.125(3) 0.075(2) -0.044(3) 0.044(2) -0.028(2) F F12 0.124(3) 0.046(2) 0.105(3) -0.014(2) -0.047(3) 0.034(2) F C37 0.053(4) 0.062(4) 0.071(4) 0.021(3) 0.010(3) 0.023(3) C C38 0.067(4) 0.073(5) 0.048(4) -0.003(4) 0.002(3) 0.012(4) C C39 0.055(4) 0.055(4) 0.052(3) 0.011(3) 0.015(3) 0.002(3) C C40 0.09(1) 0.08(1) 0.055(8) 0.005(9) 0.010(9) 0.014(7) C CL1 0.131(4) 0.081(3) 0.105(3) 0.023(3) -0.042(2) -0.032(2) Cl CL2 0.086(2) 0.080(2) 0.059(1) 0.0000 -0.016(1) 0.0000 Cl # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU N1 2.107(4) . . ? RU N2 2.060(4) . . ? RU N3 2.057(4) . . ? RU N4 1.953(4) . . ? RU N5 2.082(4) . . ? RU N6 2.091(4) . . ? N1 C1 1.338(7) . . ? N1 C12 1.363(6) . . ? C1 C2 1.410(8) . . ? C2 C3 1.347(8) . . ? C3 C4 1.408(8) . . ? C4 C5 1.447(8) . . ? C4 C12 1.410(7) . . ? C5 C6 1.332(9) . . ? C6 C7 1.447(8) . . ? C7 C8 1.405(9) . . ? C7 C11 1.404(7) . . ? C8 C9 1.345(8) . . ? C9 C10 1.401(7) . . ? C10 N2 1.330(7) . . ? N2 C11 1.366(7) . . ? C11 C12 1.418(8) . . ? N3 C13 1.359(6) . . ? N3 C17 1.368(7) . . ? C13 C14 1.361(8) . . ? C14 C15 1.388(8) . . ? C15 C16 1.381(8) . . ? C16 C17 1.387(7) . . ? C17 C18 1.486(7) . . ? C18 C19 1.374(7) . . ? C18 N4 1.356(7) . . ? C19 C20 1.377(8) . . ? C20 C21 1.371(8) . . ? C21 C22 1.387(7) . . ? C22 N4 1.366(6) . . ? C22 C23 1.466(8) . . ? C23 C24 1.374(8) . . ? C23 N5 1.380(7) . . ? C24 C25 1.375(9) . . ? C25 C26 1.387(9) . . ? C26 C27 1.374(8) . . ? C27 N5 1.334(7) . . ? N6 C28 1.387(7) . . ? N6 C36 1.327(7) . . ? C28 C29 1.363(7) . . ? C29 C30 1.402(8) . . ? C30 C31 1.421(7) . . ? C30 C35 1.419(7) . . ? C31 C32 1.372(8) . . ? C32 C33 1.391(9) . . ? C33 C34 1.359(8) . . ? C34 C35 1.403(8) . . ? C35 C36 1.409(7) . . ? P1 F1 1.601(6) . . ? P1 F2 1.545(5) . . ? P1 F3 1.555(5) . . ? P1 F4 1.544(5) . . ? P1 F5 1.486(6) . . ? P1 F6 1.577(5) . . ? F1 F2 2.16(1) . . ? F1 F3 2.069(9) . . ? F1 F4 2.191(8) . . ? F2 F6 2.185(8) . . ? F3 F4 2.197(6) . . ? F4 F5 2.153(8) . . ? F4 F6 2.168(7) . . ? F5 F6 2.092(9) . . ? P2 F7 1.599(4) . . ? P2 F8 1.561(4) . . ? P2 F9 1.600(4) . . ? P2 F10 1.601(4) . . ? P2 F11 1.583(4) . . ? P2 F12 1.549(4) . . ? C37 C38 1.34(1) . . ? C37 C39 1.47(1) . 7_555 ? C38 C39 1.375(9) . . ? C40 C40 1.12(3) . 2_555 ? C40 CL1 1.69(2) . . ? C40 CL1 1.20(2) . 2_555 ? C40 CL2 1.70(2) . . ? C40 CL2 1.70(2) . 2_555 ? CL1 CL1 1.347(9) . 2_555 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 RU N2 79.4(2) . . . ? N1 RU N3 98.0(2) . . . ? N1 RU N4 173.5(2) . . . ? N1 RU N5 102.1(2) . . . ? N1 RU N6 95.8(2) . . . ? N2 RU N3 88.3(2) . . . ? N2 RU N4 94.4(2) . . . ? N2 RU N5 89.9(2) . . . ? N2 RU N6 175.0(2) . . . ? N3 RU N4 79.7(2) . . . ? N3 RU N5 159.1(2) . . . ? N3 RU N6 93.9(2) . . . ? N4 RU N5 79.7(2) . . . ? N4 RU N6 90.4(2) . . . ? N5 RU N6 89.7(2) . . . ? RU N1 C1 130.1(3) . . . ? RU N1 C12 112.4(3) . . . ? C1 N1 C12 117.5(4) . . . ? N1 C1 C2 122.1(5) . . . ? C1 C2 C3 120.6(5) . . . ? C2 C3 C4 119.2(5) . . . ? C3 C4 C5 123.9(5) . . . ? C3 C4 C12 117.4(5) . . . ? C5 C4 C12 118.7(5) . . . ? C4 C5 C6 120.8(5) . . . ? C5 C6 C7 122.2(5) . . . ? C6 C7 C8 124.7(5) . . . ? C6 C7 C11 117.4(5) . . . ? C8 C7 C11 117.9(5) . . . ? C7 C8 C9 120.0(5) . . . ? C8 C9 C10 119.2(6) . . . ? C9 C10 N2 123.0(5) . . . ? RU N2 C10 127.8(4) . . . ? RU N2 C11 114.0(3) . . . ? C10 N2 C11 118.2(4) . . . ? C7 C11 N2 121.7(5) . . . ? C7 C11 C12 121.3(5) . . . ? N2 C11 C12 117.0(4) . . . ? N1 C12 C4 123.2(5) . . . ? N1 C12 C11 117.2(4) . . . ? C4 C12 C11 119.6(5) . . . ? RU N3 C13 128.4(4) . . . ? RU N3 C17 113.8(3) . . . ? C13 N3 C17 117.4(5) . . . ? N3 C13 C14 123.4(5) . . . ? C13 C14 C15 118.8(5) . . . ? C14 C15 C16 119.5(5) . . . ? C15 C16 C17 119.1(5) . . . ? N3 C17 C16 121.7(5) . . . ? N3 C17 C18 114.9(5) . . . ? C16 C17 C18 123.3(5) . . . ? C17 C18 C19 127.3(5) . . . ? C17 C18 N4 112.0(5) . . . ? C19 C18 N4 120.6(5) . . . ? C18 C19 C20 118.6(5) . . . ? C19 C20 C21 121.0(5) . . . ? C20 C21 C22 119.6(5) . . . ? C21 C22 N4 118.8(5) . . . ? C21 C22 C23 128.4(5) . . . ? N4 C22 C23 112.8(4) . . . ? RU N4 C18 119.5(4) . . . ? RU N4 C22 119.2(4) . . . ? C18 N4 C22 121.3(5) . . . ? C22 C23 C24 124.1(5) . . . ? C22 C23 N5 115.3(5) . . . ? C24 C23 N5 120.6(5) . . . ? C23 C24 C25 120.8(5) . . . ? C24 C25 C26 118.4(6) . . . ? C25 C26 C27 118.7(6) . . . ? C26 C27 N5 123.5(5) . . . ? RU N5 C23 112.9(4) . . . ? RU N5 C27 129.1(4) . . . ? C23 N5 C27 117.9(5) . . . ? RU N6 C28 119.4(3) . . . ? RU N6 C36 125.1(4) . . . ? C28 N6 C36 115.5(4) . . . ? N6 C28 C29 123.7(5) . . . ? C28 C29 C30 120.2(5) . . . ? C29 C30 C31 123.3(5) . . . ? C29 C30 C35 117.5(5) . . . ? C31 C30 C35 119.2(5) . . . ? C30 C31 C32 119.2(5) . . . ? C31 C32 C33 121.2(5) . . . ? C32 C33 C34 120.6(5) . . . ? C33 C34 C35 120.7(6) . . . ? C30 C35 C34 119.0(5) . . . ? C30 C35 C36 117.4(5) . . . ? C34 C35 C36 123.5(5) . . . ? N6 C36 C35 125.6(5) . . . ? F1 P1 F2 86.8(4) . . . ? F1 P1 F3 81.9(3) . . . ? F1 P1 F4 88.3(4) . . . ? F1 P1 F5 176.4(4) . . . ? F1 P1 F6 90.5(4) . . . ? F2 P1 F3 92.2(3) . . . ? F2 P1 F4 174.2(5) . . . ? F2 P1 F5 94.1(4) . . . ? F2 P1 F6 88.9(3) . . . ? F3 P1 F4 90.3(3) . . . ? F3 P1 F5 101.5(4) . . . ? F3 P1 F6 172.3(4) . . . ? F4 P1 F5 90.5(4) . . . ? F4 P1 F6 88.0(3) . . . ? F5 P1 F6 86.1(4) . . . ? P1 F1 F2 45.5(2) . . . ? P1 F1 F3 48.1(2) . . . ? P1 F1 F4 44.8(2) . . . ? F2 F1 F3 63.7(3) . . . ? F2 F1 F4 90.3(3) . . . ? F3 F1 F4 62.0(3) . . . ? P1 F2 F1 47.7(3) . . . ? P1 F2 F6 46.2(2) . . . ? F1 F2 F6 62.5(3) . . . ? P1 F3 F1 50.0(2) . . . ? P1 F3 F4 44.7(2) . . . ? F1 F3 F4 61.7(3) . . . ? P1 F4 F1 46.9(3) . . . ? P1 F4 F3 45.0(2) . . . ? P1 F4 F5 43.6(2) . . . ? P1 F4 F6 46.6(2) . . . ? F1 F4 F3 56.3(3) . . . ? F1 F4 F5 90.5(3) . . . ? F1 F4 F6 62.3(3) . . . ? F3 F4 F5 65.5(3) . . . ? F3 F4 F6 91.4(3) . . . ? F5 F4 F6 57.9(3) . . . ? P1 F5 F4 45.8(2) . . . ? P1 F5 F6 48.8(3) . . . ? F4 F5 F6 61.4(3) . . . ? P1 F6 F2 45.0(2) . . . ? P1 F6 F4 45.4(2) . . . ? P1 F6 F5 45.1(3) . . . ? F2 F6 F4 90.2(3) . . . ? F2 F6 F5 62.5(3) . . . ? F4 F6 F5 60.7(3) . . . ? F7 P2 F8 89.1(2) . . . ? F7 P2 F9 90.7(2) . . . ? F7 P2 F10 88.9(2) . . . ? F7 P2 F11 88.3(3) . . . ? F7 P2 F12 178.6(3) . . . ? F8 P2 F9 89.2(2) . . . ? F8 P2 F10 90.1(2) . . . ? F8 P2 F11 177.4(3) . . . ? F8 P2 F12 92.3(3) . . . ? F9 P2 F10 179.2(2) . . . ? F9 P2 F11 90.8(2) . . . ? F9 P2 F12 89.5(2) . . . ? F10 P2 F11 89.9(2) . . . ? F10 P2 F12 90.9(2) . . . ? F11 P2 F12 90.3(3) . . . ? C38 C37 C39 119.7(6) . . 7_555 ? C37 C38 C39 117.9(7) . . . ? C37 C39 C38 122.4(6) 7_555 . . ? C40 C40 CL1 44.8(6) 2_555 . . ? C40 C40 CL1 94.0(8) 2_555 . 2_555 ? C40 C40 CL2 70.7(5) 2_555 . . ? CL1 C40 CL1 52.2(8) . . 2_555 ? CL1 C40 CL2 114.9(8) . . . ? CL1 C40 CL2 162(1) 2_555 . . ? C40 CL1 C40 41(1) . . 2_555 ? C40 CL1 CL1 44.5(6) . . 2_555 ? C40 CL1 CL1 83.3(7) 2_555 . 2_555 ? C40 CL2 C40 38(1) . . 2_555 ? #===END data_Complex_6 _database_code_depnum_ccdc_archive 'CCDC 218277' _audit_creation_date 26-09-03 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(terpy)(phen)(DMAP)][PF6]2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H35 F12 N9 P2 Ru' _chemical_formula_weight 1008.76 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1 #========================================================================== #==== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.0753(2) _cell_length_b 11.5163(4) _cell_length_c 20.6798(6) _cell_angle_alpha 76.071(5) _cell_angle_beta 88.935(5) _cell_angle_gamma 89.917(5) _cell_volume 2097.4(1) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 13964 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.60 _exptl_crystal_density_method none _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.545 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #========================================================================== #==== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 13964 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 30 sec per frame. Data collection was divided into 3 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.40 Omega = 0.00 Kappa = 0.00 101 frames Set 2 Theta = -4.80 Kappa = -172.00 Phi = 0.00 23 frames Set 3 Theta = -6.40 Kappa = -171.00 Phi = 0.00 22 frames Friedel pairs were averaged. Internal R = 0.03 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13964 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.52 _reflns_number_total 9540 _reflns_number_gt 6791 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #========================================================================== #==== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6791 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.061 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_all 0.142 _refine_ls_wR_factor_ref 0.049 _refine_ls_goodness_of_fit_all 1.490 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_shift/su_max 0.023 _refine_ls_shift/esd_mean 0.003 _refine_diff_density_max 0.595 _refine_diff_density_min -0.119 #========================================================================== #==== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RU 0.42757(2) 0.47564(2) 0.77805(1) 0.0220(1) 1.000 Uani ? ? Ru N1 0.5126(2) 0.3180(2) 0.8403(1) 0.025(1) 1.000 Uani ? ? N C1 0.5973(3) 0.2318(3) 0.8253(1) 0.031(1) 1.000 Uani ? ? C C2 0.6508(3) 0.1344(3) 0.8735(2) 0.038(2) 1.000 Uani ? ? C C3 0.6155(3) 0.1230(3) 0.9392(2) 0.035(2) 1.000 Uani ? ? C C4 0.5256(3) 0.2106(3) 0.9579(1) 0.030(1) 1.000 Uani ? ? C C5 0.4811(3) 0.2071(3) 1.0255(2) 0.037(2) 1.000 Uani ? ? C C6 0.3979(3) 0.2958(3) 1.0402(1) 0.036(2) 1.000 Uani ? ? C C7 0.3515(3) 0.3967(3) 0.9893(1) 0.031(1) 1.000 Uani ? ? C C8 0.2677(4) 0.4924(3) 1.0010(1) 0.038(2) 1.000 Uani ? ? C C9 0.2331(3) 0.5860(3) 0.9489(2) 0.039(2) 1.000 Uani ? ? C C10 0.2802(3) 0.5854(3) 0.8843(1) 0.031(1) 1.000 Uani ? ? C N2 0.3580(2) 0.4955(2) 0.8702(1) 0.025(1) 1.000 Uani ? ? N C11 0.3943(3) 0.4014(3) 0.9226(1) 0.026(1) 1.000 Uani ? ? C C12 0.4788(3) 0.3072(3) 0.9067(1) 0.026(1) 1.000 Uani ? ? C N3 0.2171(2) 0.4234(2) 0.7586(1) 0.025(1) 1.000 Uani ? ? N C13 0.1538(3) 0.3144(3) 0.7779(1) 0.029(1) 1.000 Uani ? ? C C14 0.0135(3) 0.2904(3) 0.7587(2) 0.037(2) 1.000 Uani ? ? C C15 -0.0645(3) 0.3803(3) 0.7179(2) 0.038(2) 1.000 Uani ? ? C C16 -0.0034(3) 0.4942(3) 0.6975(2) 0.035(2) 1.000 Uani ? ? C C17 0.1368(3) 0.5144(3) 0.7189(1) 0.027(1) 1.000 Uani ? ? C C18 0.2113(3) 0.6322(2) 0.7020(1) 0.027(1) 1.000 Uani ? ? C C19 0.1548(3) 0.7393(3) 0.6653(1) 0.034(2) 1.000 Uani ? ? C C20 0.2419(4) 0.8426(3) 0.6532(2) 0.037(2) 1.000 Uani ? ? C C21 0.3817(4) 0.8373(3) 0.6798(2) 0.034(2) 1.000 Uani ? ? C C22 0.4336(3) 0.7295(3) 0.7172(1) 0.027(1) 1.000 Uani ? ? C N4 0.3488(2) 0.6292(2) 0.7273(1) 0.024(1) 1.000 Uani ? ? N C23 0.5788(3) 0.7064(3) 0.7497(1) 0.030(1) 1.000 Uani ? ? C C24 0.6801(4) 0.7961(3) 0.7505(2) 0.041(2) 1.000 Uani ? ? C C25 0.8143(3) 0.7664(3) 0.7808(2) 0.047(2) 1.000 Uani ? ? C C26 0.8432(3) 0.6477(3) 0.8103(2) 0.041(2) 1.000 Uani ? ? C C27 0.7391(3) 0.5608(3) 0.8092(1) 0.032(1) 1.000 Uani ? ? C N5 0.6057(2) 0.5882(2) 0.7796(1) 0.029(1) 1.000 Uani ? ? N N6 0.4990(2) 0.4350(2) 0.6885(1) 0.027(1) 1.000 Uani ? ? N C28 0.5819(3) 0.5101(3) 0.6418(1) 0.031(1) 1.000 Uani ? ? C C29 0.6403(3) 0.4828(3) 0.5853(1) 0.037(2) 1.000 Uani ? ? C C30 0.6180(3) 0.3687(3) 0.5734(1) 0.038(2) 1.000 Uani ? ? C C31 0.5206(3) 0.2935(3) 0.6194(2) 0.040(2) 1.000 Uani ? ? C C32 0.4673(3) 0.3287(3) 0.6741(1) 0.034(1) 1.000 Uani ? ? C N7 0.6847(3) 0.3337(3) 0.5224(1) 0.054(2) 1.000 Uani ? ? N C33 0.7764(5) 0.4178(4) 0.4732(2) 0.071(2) 1.000 Uani ? ? C C34 0.6674(5) 0.2126(4) 0.5129(2) 0.079(2) 1.000 Uani ? ? C P1 0.2099(1) 0.95495(8) 0.84027(5) 0.0436(5) 1.000 Uani ? ? P F1 0.2224(3) 1.0371(2) 0.7666(1) 0.079(2) 1.000 Uani ? ? F F2 0.3653(2) 0.8958(2) 0.8312(1) 0.059(1) 1.000 Uani ? ? F F3 0.1328(3) 0.8525(2) 0.8141(1) 0.100(2) 1.000 Uani ? ? F F4 0.1999(2) 0.8763(2) 0.9154(1) 0.067(1) 1.000 Uani ? ? F F5 0.0531(2) 1.0138(2) 0.8507(1) 0.071(1) 1.000 Uani ? ? F F6 0.2901(2) 1.0577(2) 0.8671(1) 0.069(1) 1.000 Uani ? ? F P2 0.79189(9) 0.83292(9) 0.54518(4) 0.0406(5) 1.000 Uani ? ? P F7 0.9462(4) 0.8798(4) 0.5393(3) 0.077(3) 0.500 Uani ? ? F F8 0.9574(5) 0.8053(5) 0.5256(2) 0.077(3) 0.500 Uani ? ? F F9 0.8444(7) 0.7295(5) 0.5074(3) 0.109(4) 0.500 Uani ? ? F F10 0.7309(5) 0.7647(4) 0.4984(2) 0.081(3) 0.500 Uani ? ? F F11 0.7730(3) 0.9361(3) 0.4820(1) 0.118(2) 1.000 Uani ? ? F F12 0.8120(2) 0.7269(2) 0.6100(1) 0.072(1) 1.000 Uani ? ? F F13 0.6293(5) 0.7699(5) 0.5485(3) 0.080(3) 0.500 Uani ? ? F F14 0.6377(5) 0.8622(6) 0.5703(3) 0.083(3) 0.500 Uani ? ? F F15 0.7273(7) 0.9215(5) 0.5827(3) 0.111(4) 0.500 Uani ? ? F F16 0.8661(5) 0.9093(4) 0.5950(2) 0.073(3) 0.500 Uani ? ? F C35 1.0176(5) 0.8708(5) 0.3702(2) 0.081(3) 1.000 Uani ? ? C C36 1.1402(4) 0.8952(3) 0.3217(2) 0.054(2) 1.000 Uani ? ? C N8 1.2357(3) 0.9091(3) 0.2844(2) 0.062(2) 1.000 Uani ? ? N C37 0.0676(5) 0.1675(4) 0.9734(2) 0.069(2) 1.000 Uani ? ? C C38 0.0082(4) 0.2819(3) 0.9384(2) 0.054(2) 1.000 Uani ? ? C N9 -0.0372(4) 0.3724(3) 0.9107(2) 0.075(2) 1.000 Uani ? ? N H1 0.6221 0.2371 0.7799 0.0414 1.000 Uiso calc C1 H H2 0.7114 0.0764 0.8605 0.0506 1.000 Uiso calc C2 H H3 0.6510 0.0570 0.9721 0.0485 1.000 Uiso calc C3 H H4 0.5102 0.1417 1.0603 0.0520 1.000 Uiso calc C5 H H5 0.3698 0.2909 1.0853 0.0504 1.000 Uiso calc C6 H H6 0.2350 0.4921 1.0449 0.0513 1.000 Uiso calc C8 H H7 0.1772 0.6513 0.9567 0.0502 1.000 Uiso calc C9 H H8 0.2560 0.6516 0.8489 0.0409 1.000 Uiso calc C10 H H9 0.2074 0.2515 0.8059 0.0385 1.000 Uiso calc C13 H H10 -0.0279 0.2126 0.7736 0.0490 1.000 Uiso calc C14 H H11 -0.1599 0.3648 0.7037 0.0487 1.000 Uiso calc C15 H H12 -0.0564 0.5572 0.6695 0.0456 1.000 Uiso calc C16 H H13 0.0578 0.7426 0.6485 0.0457 1.000 Uiso calc C19 H H14 0.2057 0.9160 0.6270 0.0521 1.000 Uiso calc C20 H H15 0.4413 0.9071 0.6723 0.0473 1.000 Uiso calc C21 H H16 0.6575 0.8772 0.7305 0.0535 1.000 Uiso calc C24 H H17 0.8855 0.8266 0.7812 0.0596 1.000 Uiso calc C25 H H18 0.9347 0.6259 0.8314 0.0530 1.000 Uiso calc C26 H H19 0.7608 0.4797 0.8296 0.0418 1.000 Uiso calc C27 H H20 0.6016 0.5874 0.6483 0.0405 1.000 Uiso calc C28 H H21 0.6958 0.5412 0.5541 0.0483 1.000 Uiso calc C29 H H22 0.4922 0.2182 0.6123 0.0492 1.000 Uiso calc C31 H H23 0.4036 0.2751 0.7040 0.0432 1.000 Uiso calc C32 H H24 0.8146 0.3786 0.4410 0.0930 1.000 Uiso calc C33 H H25 0.7183 0.4841 0.4517 0.0930 1.000 Uiso calc C33 H H26 0.8556 0.4452 0.4951 0.0930 1.000 Uiso calc C33 H H27 0.7224 0.2052 0.4746 0.0941 1.000 Uiso calc C34 H H28 0.7022 0.1563 0.5510 0.0941 1.000 Uiso calc C34 H H29 0.5662 0.1976 0.5071 0.0941 1.000 Uiso calc C34 H H30 0.9802 0.9442 0.3769 0.1059 1.000 Uiso calc C35 H H31 0.9418 0.8294 0.3539 0.1059 1.000 Uiso calc C35 H H32 1.0514 0.8231 0.4113 0.1059 1.000 Uiso calc C35 H H33 -0.0111 0.1137 0.9901 0.0895 1.000 Uiso calc C37 H H34 0.1274 0.1358 0.9436 0.0895 1.000 Uiso calc C37 H H35 0.1253 0.1781 1.0094 0.0895 1.000 Uiso calc C37 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RU 0.0258(1) 0.0197(1) 0.02109(9) 0.00067(8) 0.00262(8) -0.00419(8) Ru N1 0.024(1) 0.025(1) 0.027(1) -0.0002(9) 0.0029(9) -0.0070(9) N C1 0.034(1) 0.027(1) 0.034(1) 0.004(1) 0.005(1) -0.006(1) C C2 0.037(2) 0.028(2) 0.052(2) 0.009(1) 0.001(1) -0.011(1) C C3 0.034(1) 0.028(2) 0.045(2) 0.006(1) -0.007(1) 0.001(1) C C4 0.030(1) 0.029(2) 0.032(1) -0.000(1) -0.004(1) -0.001(1) C C5 0.044(2) 0.039(2) 0.031(2) -0.000(1) -0.006(1) 0.005(1) C C6 0.048(2) 0.043(2) 0.022(1) 0.001(2) 0.001(1) -0.002(1) C C7 0.034(1) 0.036(2) 0.025(1) -0.003(1) 0.000(1) -0.005(1) C C8 0.050(2) 0.046(2) 0.024(1) -0.001(2) 0.008(1) -0.014(1) C C9 0.051(2) 0.035(2) 0.034(1) 0.006(1) 0.007(1) -0.016(1) C C10 0.039(2) 0.025(1) 0.030(1) 0.003(1) 0.005(1) -0.006(1) C N2 0.028(1) 0.023(1) 0.023(1) -0.001(1) 0.0037(9) -0.0061(9) N C11 0.026(1) 0.028(1) 0.025(1) -0.000(1) 0.001(1) -0.006(1) C C12 0.024(1) 0.027(1) 0.029(1) -0.002(1) -0.001(1) -0.006(1) C N3 0.029(1) 0.024(1) 0.022(1) 0.001(1) 0.0043(9) -0.0056(9) N C13 0.034(1) 0.025(1) 0.028(1) -0.003(1) 0.004(1) -0.002(1) C C14 0.039(2) 0.031(2) 0.043(2) -0.008(1) 0.004(1) -0.009(1) C C15 0.031(1) 0.040(2) 0.043(2) -0.002(1) -0.000(1) -0.013(1) C C16 0.033(1) 0.035(2) 0.038(2) 0.004(1) -0.002(1) -0.011(1) C C17 0.027(1) 0.029(1) 0.025(1) 0.002(1) 0.002(1) -0.008(1) C C18 0.033(1) 0.026(1) 0.022(1) 0.004(1) 0.002(1) -0.008(1) C C19 0.044(2) 0.031(2) 0.029(1) 0.004(1) -0.005(1) -0.004(1) C C20 0.058(2) 0.026(2) 0.034(2) 0.005(1) -0.004(1) -0.001(1) C C21 0.054(2) 0.022(1) 0.033(2) -0.005(1) 0.006(1) -0.005(1) C C22 0.038(1) 0.023(1) 0.023(1) -0.004(1) 0.005(1) -0.005(1) C N4 0.029(1) 0.024(1) 0.022(1) 0.001(1) 0.0020(9) -0.0037(9) N C23 0.036(1) 0.030(1) 0.025(1) -0.007(1) 0.008(1) -0.010(1) C C24 0.046(2) 0.038(2) 0.041(2) -0.011(1) 0.007(1) -0.011(1) C C25 0.045(2) 0.049(2) 0.047(2) -0.020(1) 0.007(1) -0.020(1) C C26 0.030(1) 0.055(2) 0.041(2) -0.007(1) 0.004(1) -0.021(1) C C27 0.031(1) 0.039(2) 0.028(1) 0.000(1) 0.004(1) -0.012(1) C N5 0.033(1) 0.030(1) 0.024(1) -0.000(1) 0.002(1) -0.0105(9) N N6 0.028(1) 0.028(1) 0.025(1) -0.000(1) 0.003(1) -0.0061(9) N C28 0.036(1) 0.030(1) 0.027(1) -0.001(1) 0.004(1) -0.006(1) C C29 0.039(2) 0.042(2) 0.029(1) -0.000(1) 0.005(1) -0.008(1) C C30 0.038(2) 0.046(2) 0.032(1) 0.005(1) -0.002(1) -0.017(1) C C31 0.042(2) 0.038(2) 0.039(2) -0.002(1) -0.002(1) -0.020(1) C C32 0.033(1) 0.031(1) 0.038(2) -0.002(1) 0.004(1) -0.012(1) C N7 0.056(2) 0.066(2) 0.043(1) -0.001(1) 0.014(1) -0.031(1) N C33 0.083(3) 0.091(3) 0.046(2) -0.004(2) 0.026(2) -0.030(2) C C34 0.072(3) 0.087(2) 0.078(2) -0.002(2) 0.015(2) -0.058(2) C P1 0.0527(5) 0.0327(4) 0.0480(5) 0.0093(4) -0.0185(4) -0.0095(4) P F1 0.142(2) 0.076(2) 0.046(1) 0.045(1) -0.021(1) -0.001(1) F F2 0.064(1) 0.067(1) 0.049(1) 0.025(1) -0.009(1) -0.017(1) F F3 0.083(1) 0.068(1) 0.175(2) 0.014(1) -0.066(1) -0.061(1) F F4 0.062(1) 0.069(2) 0.069(1) 0.014(1) 0.009(1) 0.019(1) F F5 0.056(1) 0.068(1) 0.094(2) 0.025(1) -0.020(1) -0.015(1) F F6 0.074(1) 0.051(1) 0.085(1) -0.003(1) -0.010(1) -0.032(1) F P2 0.0410(4) 0.0420(5) 0.0388(5) 0.0017(4) 0.0002(4) 0.0017(4) P F7 0.047(2) 0.070(3) 0.140(5) -0.031(2) -0.012(3) 0.028(3) F F8 0.057(2) 0.128(4) 0.063(3) 0.035(3) 0.013(2) 0.010(3) F F9 0.161(5) 0.062(3) 0.129(4) -0.020(3) 0.073(4) -0.038(3) F F10 0.096(3) 0.073(3) 0.077(2) 0.016(2) -0.042(2) -0.043(2) F F11 0.144(2) 0.127(2) 0.090(2) 0.038(2) 0.002(2) 0.066(2) F F12 0.078(1) 0.069(2) 0.069(1) -0.012(1) -0.016(1) 0.026(1) F F13 0.054(2) 0.072(3) 0.132(4) -0.015(2) -0.031(3) 0.033(3) F F14 0.042(2) 0.166(5) 0.082(3) 0.021(3) 0.004(2) -0.037(3) F F15 0.166(5) 0.065(3) 0.128(4) 0.020(3) 0.079(3) -0.022(3) F F16 0.083(3) 0.061(3) 0.077(3) 0.001(2) -0.021(2) -0.035(2) F C35 0.069(3) 0.112(4) 0.069(3) 0.011(3) 0.013(2) -0.034(2) C C36 0.064(2) 0.041(2) 0.059(2) 0.006(2) -0.007(2) -0.022(2) C N8 0.068(2) 0.050(2) 0.071(2) -0.007(2) 0.012(2) -0.025(1) N C37 0.069(2) 0.059(2) 0.081(3) -0.001(2) 0.019(2) -0.021(2) C C38 0.047(2) 0.065(2) 0.052(2) 0.002(2) 0.010(2) -0.028(2) C N9 0.080(2) 0.089(2) 0.059(2) 0.030(2) 0.002(2) -0.026(2) N # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU N1 2.111(2) . . ? RU N2 2.062(2) . . ? RU N3 2.079(2) . . ? RU N4 1.967(2) . . ? RU N5 2.079(3) . . ? RU N6 2.107(2) . . ? N1 C1 1.345(4) . . ? N1 C12 1.377(4) . . ? C1 C2 1.401(4) . . ? C2 C3 1.365(5) . . ? C3 C4 1.416(5) . . ? C4 C5 1.438(5) . . ? C4 C12 1.409(4) . . ? C5 C6 1.358(5) . . ? C6 C7 1.436(4) . . ? C7 C8 1.403(5) . . ? C7 C11 1.414(4) . . ? C8 C9 1.368(5) . . ? C9 C10 1.397(4) . . ? C10 N2 1.339(4) . . ? N2 C11 1.379(4) . . ? C11 C12 1.426(4) . . ? N3 C13 1.348(4) . . ? N3 C17 1.381(4) . . ? C13 C14 1.389(4) . . ? C14 C15 1.373(5) . . ? C15 C16 1.390(5) . . ? C16 C17 1.393(4) . . ? C17 C18 1.478(4) . . ? C18 C19 1.387(4) . . ? C18 N4 1.359(4) . . ? C19 C20 1.398(5) . . ? C20 C21 1.387(5) . . ? C21 C22 1.382(4) . . ? C22 N4 1.361(4) . . ? C22 C23 1.484(4) . . ? C23 C24 1.388(4) . . ? C23 N5 1.376(4) . . ? C24 C25 1.384(5) . . ? C25 C26 1.383(5) . . ? C26 C27 1.382(5) . . ? C27 N5 1.369(4) . . ? N6 C28 1.349(4) . . ? N6 C32 1.361(4) . . ? C28 C29 1.378(4) . . ? C29 C30 1.409(5) . . ? C30 C31 1.418(5) . . ? C30 N7 1.350(4) . . ? C31 C32 1.370(4) . . ? N7 C33 1.471(5) . . ? N7 C34 1.463(5) . . ? P1 F1 1.591(3) . . ? P1 F2 1.593(2) . . ? P1 F3 1.581(3) . . ? P1 F4 1.601(2) . . ? P1 F5 1.608(2) . . ? P1 F6 1.604(2) . . ? P2 F7 1.494(6) . . ? P2 F8 1.600(6) . . ? P2 F9 1.640(6) . . ? P2 F10 1.499(5) . . ? P2 F11 1.553(3) . . ? P2 F12 1.595(2) . . ? P2 F13 1.638(5) . . ? P2 F14 1.548(6) . . ? P2 F15 1.532(7) . . ? P2 F16 1.659(5) . . ? F7 F11 1.998(8) . . ? F7 F16 1.46(1) . . ? F8 F9 1.46(1) . . ? F8 F12 2.183(7) . . ? F9 F10 1.110(9) . . ? F9 F12 2.131(8) . . ? F10 F11 1.958(7) . . ? F10 F13 1.39(1) . . ? F11 F14 2.178(8) . . ? F11 F15 2.083(9) . . ? F12 F13 2.094(6) . . ? F12 F16 2.106(6) . . ? F13 F14 1.25(1) . . ? F14 F15 1.13(1) . . ? F15 F16 1.29(1) . . ? C35 C36 1.465(6) . . ? C36 N8 1.135(5) . . ? C37 C38 1.450(6) . . ? C38 N9 1.143(5) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 RU N2 79.35(9) . . . ? N1 RU N3 102.60(9) . . . ? N1 RU N4 174.7(1) . . . ? N1 RU N5 98.42(9) . . . ? N1 RU N6 94.95(9) . . . ? N2 RU N3 90.78(9) . . . ? N2 RU N4 95.78(9) . . . ? N2 RU N5 90.14(9) . . . ? N2 RU N6 173.73(9) . . . ? N3 RU N4 79.51(9) . . . ? N3 RU N5 158.8(1) . . . ? N3 RU N6 87.88(9) . . . ? N4 RU N5 79.3(1) . . . ? N4 RU N6 90.00(9) . . . ? N5 RU N6 93.33(9) . . . ? RU N1 C1 130.3(2) . . . ? RU N1 C12 112.9(2) . . . ? C1 N1 C12 116.8(2) . . . ? N1 C1 C2 123.2(3) . . . ? C1 C2 C3 119.9(3) . . . ? C2 C3 C4 119.4(3) . . . ? C3 C4 C5 124.0(3) . . . ? C3 C4 C12 117.3(3) . . . ? C5 C4 C12 118.6(3) . . . ? C4 C5 C6 121.1(3) . . . ? C5 C6 C7 121.5(3) . . . ? C6 C7 C8 124.6(3) . . . ? C6 C7 C11 118.1(3) . . . ? C8 C7 C11 117.3(3) . . . ? C7 C8 C9 119.9(3) . . . ? C8 C9 C10 119.8(3) . . . ? C9 C10 N2 122.7(3) . . . ? RU N2 C10 128.0(2) . . . ? RU N2 C11 114.3(2) . . . ? C10 N2 C11 117.6(2) . . . ? C7 C11 N2 122.6(3) . . . ? C7 C11 C12 120.5(3) . . . ? N2 C11 C12 116.8(3) . . . ? N1 C12 C4 123.4(3) . . . ? N1 C12 C11 116.5(3) . . . ? C4 C12 C11 120.1(3) . . . ? RU N3 C13 128.6(2) . . . ? RU N3 C17 113.4(2) . . . ? C13 N3 C17 117.9(3) . . . ? N3 C13 C14 122.7(3) . . . ? C13 C14 C15 119.2(3) . . . ? C14 C15 C16 119.7(3) . . . ? C15 C16 C17 119.0(3) . . . ? N3 C17 C16 121.5(3) . . . ? N3 C17 C18 114.7(3) . . . ? C16 C17 C18 123.8(3) . . . ? C17 C18 C19 127.1(3) . . . ? C17 C18 N4 113.1(2) . . . ? C19 C18 N4 119.8(3) . . . ? C18 C19 C20 119.4(3) . . . ? C19 C20 C21 119.6(3) . . . ? C20 C21 C22 119.5(3) . . . ? C21 C22 N4 120.2(3) . . . ? C21 C22 C23 127.3(3) . . . ? N4 C22 C23 112.5(3) . . . ? RU N4 C18 119.1(2) . . . ? RU N4 C22 119.5(2) . . . ? C18 N4 C22 121.4(3) . . . ? C22 C23 C24 123.1(3) . . . ? C22 C23 N5 114.8(3) . . . ? C24 C23 N5 122.1(3) . . . ? C23 C24 C25 119.4(3) . . . ? C24 C25 C26 119.0(3) . . . ? C25 C26 C27 120.0(3) . . . ? C26 C27 N5 121.9(3) . . . ? RU N5 C23 113.7(2) . . . ? RU N5 C27 128.6(2) . . . ? C23 N5 C27 117.5(3) . . . ? RU N6 C28 123.3(2) . . . ? RU N6 C32 122.1(2) . . . ? C28 N6 C32 114.6(3) . . . ? N6 C28 C29 124.8(3) . . . ? C28 C29 C30 120.4(3) . . . ? C29 C30 C31 114.7(3) . . . ? C29 C30 N7 122.6(3) . . . ? C31 C30 N7 122.7(3) . . . ? C30 C31 C32 120.4(3) . . . ? N6 C32 C31 124.7(3) . . . ? C30 N7 C33 120.6(3) . . . ? C30 N7 C34 122.0(3) . . . ? C33 N7 C34 117.4(3) . . . ? F1 P1 F2 90.7(1) . . . ? F1 P1 F3 91.0(2) . . . ? F1 P1 F4 177.8(2) . . . ? F1 P1 F5 90.2(1) . . . ? F1 P1 F6 89.3(2) . . . ? F2 P1 F3 88.9(1) . . . ? F2 P1 F4 89.5(1) . . . ? F2 P1 F5 179.1(1) . . . ? F2 P1 F6 90.3(1) . . . ? F3 P1 F4 91.2(2) . . . ? F3 P1 F5 91.3(1) . . . ? F3 P1 F6 179.2(1) . . . ? F4 P1 F5 89.7(1) . . . ? F4 P1 F6 88.5(1) . . . ? F5 P1 F6 89.5(1) . . . ? F7 P2 F8 36.4(4) . . . ? F7 P2 F9 89.3(5) . . . ? F7 P2 F10 122.7(5) . . . ? F7 P2 F11 81.9(3) . . . ? F7 P2 F12 97.8(3) . . . ? F7 P2 F13 174.0(5) . . . ? F7 P2 F14 139.8(6) . . . ? F7 P2 F15 96.8(6) . . . ? F7 P2 F16 54.8(4) . . . ? F8 P2 F9 53.5(4) . . . ? F8 P2 F10 91.5(4) . . . ? F8 P2 F11 93.5(3) . . . ? F8 P2 F12 86.2(3) . . . ? F8 P2 F13 137.6(5) . . . ? F8 P2 F14 174.5(4) . . . ? F8 P2 F15 132.3(6) . . . ? F8 P2 F16 86.2(4) . . . ? F9 P2 F10 41.1(3) . . . ? F9 P2 F11 97.5(3) . . . ? F9 P2 F12 82.4(3) . . . ? F9 P2 F13 84.7(5) . . . ? F9 P2 F14 130.8(5) . . . ? F9 P2 F15 173.7(5) . . . ? F9 P2 F16 137.1(5) . . . ? F10 P2 F11 79.8(3) . . . ? F10 P2 F12 100.2(3) . . . ? F10 P2 F13 52.2(4) . . . ? F10 P2 F14 93.7(4) . . . ? F10 P2 F15 134.5(5) . . . ? F10 P2 F16 177.5(4) . . . ? F11 P2 F12 180(1) . . . ? F11 P2 F13 99.5(3) . . . ? F11 P2 F14 89.2(4) . . . ? F11 P2 F15 84.9(3) . . . ? F11 P2 F16 99.3(3) . . . ? F12 P2 F13 80.7(2) . . . ? F12 P2 F14 91.0(4) . . . ? F12 P2 F15 95.2(3) . . . ? F12 P2 F16 80.6(2) . . . ? F13 P2 F14 46.2(4) . . . ? F13 P2 F15 89.2(5) . . . ? F13 P2 F16 130.3(5) . . . ? F14 P2 F15 43.2(4) . . . ? F14 P2 F16 88.6(4) . . . ? F15 P2 F16 47.5(4) . . . ? P2 F7 F11 50.3(2) . . . ? P2 F7 F16 68.4(4) . . . ? F11 F7 F16 88.8(4) . . . ? P2 F8 F9 64.7(4) . . . ? P2 F8 F12 46.8(2) . . . ? F9 F8 F12 68.3(4) . . . ? P2 F9 F8 61.8(4) . . . ? P2 F9 F10 62.6(4) . . . ? P2 F9 F12 47.9(2) . . . ? F8 F9 F10 119.0(7) . . . ? F8 F9 F12 72.2(4) . . . ? F10 F9 F12 88.4(5) . . . ? P2 F10 F9 76.3(5) . . . ? P2 F10 F11 51.3(2) . . . ? P2 F10 F13 69.1(4) . . . ? F9 F10 F11 99.3(6) . . . ? F9 F10 F13 124.2(7) . . . ? F11 F10 F13 91.9(4) . . . ? P2 F11 F7 47.7(2) . . . ? P2 F11 F10 48.9(2) . . . ? P2 F11 F14 45.3(2) . . . ? P2 F11 F15 47.1(2) . . . ? F7 F11 F10 83.2(3) . . . ? F7 F11 F14 86.2(3) . . . ? F7 F11 F15 67.3(4) . . . ? F10 F11 F14 64.8(3) . . . ? F10 F11 F15 87.5(3) . . . ? F14 F11 F15 30.8(3) . . . ? P2 F12 F8 47.0(2) . . . ? P2 F12 F9 49.7(2) . . . ? P2 F12 F13 50.5(2) . . . ? P2 F12 F16 51.0(2) . . . ? F8 F12 F9 39.5(3) . . . ? F8 F12 F13 89.8(3) . . . ? F8 F12 F16 62.6(3) . . . ? F9 F12 F13 63.0(4) . . . ? F9 F12 F16 92.9(3) . . . ? F13 F12 F16 90.8(3) . . . ? P2 F13 F10 58.7(3) . . . ? P2 F13 F12 48.7(2) . . . ? P2 F13 F14 63.1(4) . . . ? F10 F13 F12 83.4(3) . . . ? F10 F13 F14 114.6(6) . . . ? F12 F13 F14 79.8(5) . . . ? P2 F14 F11 45.5(2) . . . ? P2 F14 F13 70.7(4) . . . ? P2 F14 F15 67.6(5) . . . ? F11 F14 F13 86.0(5) . . . ? F11 F14 F15 70.0(6) . . . ? F13 F14 F15 137.7(8) . . . ? P2 F15 F11 47.9(2) . . . ? P2 F15 F14 69.1(6) . . . ? P2 F15 F16 71.4(4) . . . ? F11 F15 F14 79.2(7) . . . ? F11 F15 F16 89.9(4) . . . ? F14 F15 F16 135.1(8) . . . ? P2 F16 F7 56.8(3) . . . ? P2 F16 F12 48.4(2) . . . ? P2 F16 F15 61.1(4) . . . ? F7 F16 F12 79.3(3) . . . ? F7 F16 F15 110.7(6) . . . ? F12 F16 F15 81.9(4) . . . ? C35 C36 N8 177.2(5) . . . ? C37 C38 N9 179.4(5) . . . ? #===END data_Complex_7 _database_code_depnum_ccdc_archive 'CCDC 218278' _audit_creation_date 25-09-03 #========================================================================== #==== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(terpy)(phen)(PTZ)][PF6]2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C88 H74 F24 N12 O2 P4 Ru2 S2' _chemical_formula_weight 2177.78 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1 S ? 0.110 0.124 International_Tables_Vol_IV_Table_2.3.1 #========================================================================== #==== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.2143(3) _cell_length_b 12.4444(5) _cell_length_c 19.6448(8) _cell_angle_alpha 97.540(5) _cell_angle_beta 94.916(5) _cell_angle_gamma 111.387(5) _cell_volume 2280.8(1) _cell_formula_units_Z 1 _cell_measurement_temperature 173 _cell_measurement_reflns_used 13528 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.6 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.59 _exptl_crystal_density_method none _exptl_crystal_F_000 1098 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #========================================================================== #==== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 13528 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 60 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = -6.30 Omega = 0.00 Kappa = 0.00 140 frames Set 2 Theta = -5.20 Kappa = -172.00 Phi = 0.00 27 frames Friedel pairs were averaged. Internal R = 0.07 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13528 _diffrn_reflns_av_R_equivalents 0.070 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.56 _reflns_number_total 10236 _reflns_number_gt 4541 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #========================================================================== #==== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4541 _refine_ls_number_parameters 637 _refine_ls_number_restraints -7 _refine_ls_number_constraints 28 _refine_ls_R_factor_all 0.129 _refine_ls_R_factor_gt 0.076 _refine_ls_wR_factor_all 0.228 _refine_ls_wR_factor_ref 0.092 _refine_ls_goodness_of_fit_all 1.249 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_shift/su_max 0.010 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.908 _refine_diff_density_min -0.238 #========================================================================== #==== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RU 0.51462(9) 0.43932(7) 0.73459(4) 0.0289(3) 1.000 Uani ? ? Ru N1 0.3111(8) 0.3966(7) 0.6797(4) 0.033(4) 1.000 Uani ? ? N C1 0.191(1) 0.3869(9) 0.7029(5) 0.038(5) 1.000 Uani ? ? C C2 0.060(1) 0.351(1) 0.6603(6) 0.047(6) 1.000 Uani ? ? C C3 0.054(1) 0.325(1) 0.5902(6) 0.043(6) 1.000 Uani ? ? C C4 0.179(1) 0.3309(9) 0.5622(5) 0.039(5) 1.000 Uani ? ? C C5 0.184(1) 0.303(1) 0.4905(6) 0.056(7) 1.000 Uani ? ? C C6 0.306(1) 0.311(1) 0.4670(5) 0.053(7) 1.000 Uani ? ? C C7 0.437(1) 0.346(1) 0.5137(6) 0.051(6) 1.000 Uani ? ? C C8 0.569(1) 0.357(1) 0.4935(6) 0.061(7) 1.000 Uani ? ? C C9 0.687(1) 0.393(1) 0.5422(6) 0.058(7) 1.000 Uani ? ? C C10 0.675(1) 0.416(1) 0.6115(6) 0.045(6) 1.000 Uani ? ? C N2 0.5529(8) 0.4062(7) 0.6338(4) 0.033(4) 1.000 Uani ? ? N C11 0.434(1) 0.3717(8) 0.5848(5) 0.037(5) 1.000 Uani ? ? C C12 0.305(1) 0.3675(8) 0.6099(5) 0.034(5) 1.000 Uani ? ? C N3 0.4872(9) 0.2710(7) 0.7485(4) 0.038(4) 1.000 Uani ? ? N C13 0.370(1) 0.174(1) 0.7326(6) 0.050(6) 1.000 Uani ? ? C C14 0.365(1) 0.064(1) 0.7430(7) 0.056(7) 1.000 Uani ? ? C C15 0.489(1) 0.055(1) 0.7706(7) 0.065(7) 1.000 Uani ? ? C C16 0.612(1) 0.156(1) 0.7889(7) 0.062(6) 1.000 Uani ? ? C C17 0.611(1) 0.2622(9) 0.7766(5) 0.042(5) 1.000 Uani ? ? C C18 0.736(1) 0.3739(9) 0.7924(5) 0.039(5) 1.000 Uani ? ? C C19 0.871(1) 0.389(1) 0.8220(6) 0.053(6) 1.000 Uani ? ? C C20 0.976(1) 0.500(1) 0.8307(6) 0.049(6) 1.000 Uani ? ? C C21 0.948(1) 0.594(1) 0.8114(6) 0.044(6) 1.000 Uani ? ? C C22 0.811(1) 0.575(1) 0.7822(5) 0.035(5) 1.000 Uani ? ? C N4 0.7080(8) 0.4655(7) 0.7747(4) 0.035(4) 1.000 Uani ? ? N C23 0.757(1) 0.6574(9) 0.7580(5) 0.035(5) 1.000 Uani ? ? C C24 0.842(1) 0.774(1) 0.7593(6) 0.047(6) 1.000 Uani ? ? C C25 0.781(1) 0.849(1) 0.7352(6) 0.047(6) 1.000 Uani ? ? C C26 0.639(1) 0.805(1) 0.7117(6) 0.048(6) 1.000 Uani ? ? C C27 0.561(1) 0.6884(9) 0.7122(5) 0.033(5) 1.000 Uani ? ? C N5 0.6162(8) 0.6153(7) 0.7336(4) 0.034(4) 1.000 Uani ? ? N S 0.4426(3) 0.4765(2) 0.8441(1) 0.038(1) 1.000 Uani ? ? S C28 0.491(1) 0.6292(9) 0.8701(5) 0.038(5) 1.000 Uani ? ? C C29 0.395(1) 0.678(1) 0.8497(6) 0.051(6) 1.000 Uani ? ? C C30 0.430(1) 0.796(1) 0.8648(6) 0.060(6) 1.000 Uani ? ? C C31 0.566(1) 0.869(1) 0.8996(6) 0.058(7) 1.000 Uani ? ? C C32 0.660(1) 0.820(1) 0.9199(6) 0.051(6) 1.000 Uani ? ? C C33 0.625(1) 0.6993(9) 0.9056(5) 0.043(6) 1.000 Uani ? ? C N6 0.726(1) 0.6531(8) 0.9277(5) 0.053(5) 1.000 Uani ? ? N C34 0.683(1) 0.538(1) 0.9400(6) 0.048(6) 1.000 Uani ? ? C C35 0.775(1) 0.508(1) 0.9825(6) 0.060(7) 1.000 Uani ? ? C C36 0.741(1) 0.396(1) 0.9946(6) 0.069(8) 1.000 Uani ? ? C C37 0.610(1) 0.310(1) 0.9649(6) 0.067(7) 1.000 Uani ? ? C C38 0.515(1) 0.338(1) 0.9237(6) 0.053(7) 1.000 Uani ? ? C C39 0.553(1) 0.451(1) 0.9089(5) 0.041(6) 1.000 Uani ? ? C P1 0.1618(3) 0.7077(3) 0.6481(2) 0.047(2) 1.000 Uani ? ? P F1 0.3201(8) 0.8005(7) 0.6523(5) 0.077(5) 1.000 Uani ? ? F F2 0.0057(8) 0.6172(8) 0.6471(5) 0.088(5) 1.000 Uani ? ? F F3 0.1353(9) 0.697(1) 0.5682(4) 0.117(6) 1.000 Uani ? ? F F4 0.189(1) 0.719(2) 0.7257(5) 0.129(9) 1.000 Uani ? ? F F5 0.1029(9) 0.8069(8) 0.6535(7) 0.118(7) 1.000 Uani ? ? F F6 0.2247(9) 0.6106(7) 0.6344(7) 0.106(7) 1.000 Uani ? ? F P2 0.0431(4) 0.1478(3) 0.8660(2) 0.060(2) 1.000 Uani ? ? P F7 -0.061(1) 0.1389(8) 0.7993(5) 0.129(6) 1.000 Uani ? ? F F8 0.147(2) 0.257(1) 0.8455(7) 0.21(1) 1.000 Uani ? ? F F9 -0.016(1) 0.2262(9) 0.9109(6) 0.191(8) 1.000 Uani ? ? F F10 0.148(1) 0.1581(9) 0.9289(5) 0.152(7) 1.000 Uani ? ? F F11 -0.063(1) 0.037(1) 0.8843(7) 0.143(9) 1.000 Uani ? ? F F12 0.090(1) 0.0600(9) 0.8194(6) 0.153(7) 1.000 Uani ? ? F C40 0.132(2) 0.956(2) 0.410(1) 0.16(3) 0.500 Uani ? ? C C41 0.1364(2) 0.9802(2) 0.4809(1) 0.1618(3) 0.500 Uani ? ? C C42 0.2586(2) 0.9969(2) 0.5246(1) 0.1745(3) 0.500 Uani ? ? C C43 0.3762(2) 0.9900(2) 0.4971(1) 0.1745(3) 0.500 Uani ? ? C C44 0.3707(2) 0.9662(2) 0.4258(1) 0.1746(3) 0.500 Uani ? ? C C45 0.2494(2) 0.9495(2) 0.3821(1) 0.1745(3) 0.500 Uani ? ? C C46 0.0096(2) 0.9397(2) 0.3660(1) 0.1770(3) 0.500 Uani ? ? C C47 0.4984(2) 1.0067(2) 0.5407(1) 0.1808(3) 0.500 Uani ? ? C O3 0.061(4) 0.791(3) 0.955(2) 0.22(3) 0.500 Uani ? ? O C48 0.158(2) 0.884(2) 0.948(1) 0.05(1) 0.500 Uani ? ? C O4 0.170(3) 0.895(3) 0.882(2) 0.15(2) 0.500 Uani ? ? O C49 0.042(4) 0.853(3) 0.924(2) 0.10(2) 0.500 Uani ? ? C H1 0.1926 0.4055 0.7515 0.0544 1.000 Uiso calc C1 H H2 -0.0235 0.3445 0.6800 0.0653 1.000 Uiso calc C2 H H3 -0.0329 0.3033 0.5605 0.0673 1.000 Uiso calc C3 H H4 0.0987 0.2780 0.4584 0.0802 1.000 Uiso calc C5 H H5 0.3060 0.2921 0.4185 0.0801 1.000 Uiso calc C6 H H6 0.5767 0.3382 0.4458 0.0830 1.000 Uiso calc C8 H H7 0.7774 0.4027 0.5286 0.0753 1.000 Uiso calc C9 H H8 0.7576 0.4403 0.6449 0.0597 1.000 Uiso calc C10 H H9 0.2851 0.1798 0.7132 0.0665 1.000 Uiso calc C13 H H10 0.2787 -0.0029 0.7315 0.0849 1.000 Uiso calc C14 H H11 0.4901 -0.0195 0.7771 0.0851 1.000 Uiso calc C15 H H12 0.6975 0.1522 0.8097 0.0748 1.000 Uiso calc C16 H H13 0.8916 0.3254 0.8356 0.0666 1.000 Uiso calc C19 H H14 1.0692 0.5129 0.8507 0.0708 1.000 Uiso calc C20 H H15 1.0219 0.6696 0.8180 0.0659 1.000 Uiso calc C21 H H16 0.9400 0.8038 0.7766 0.0708 1.000 Uiso calc C24 H H17 0.8378 0.9285 0.7352 0.0727 1.000 Uiso calc C25 H H18 0.5941 0.8533 0.6954 0.0655 1.000 Uiso calc C26 H H19 0.4619 0.6587 0.6962 0.0496 1.000 Uiso calc C27 H H20 0.3037 0.6286 0.8250 0.0639 1.000 Uiso calc C29 H H21 0.3627 0.8291 0.8519 0.0755 1.000 Uiso calc C30 H H22 0.5928 0.9514 0.9089 0.0806 1.000 Uiso calc C31 H H23 0.7512 0.8698 0.9443 0.0725 1.000 Uiso calc C32 H H24 0.8640 0.5668 1.0037 0.0814 1.000 Uiso calc C35 H H25 0.8067 0.3763 1.0229 0.0935 1.000 Uiso calc C36 H H26 0.5858 0.2325 0.9732 0.0860 1.000 Uiso calc C37 H H27 0.4242 0.2795 0.9052 0.0754 1.000 Uiso calc C38 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RU 0.0254(3) 0.0343(3) 0.0278(3) 0.0047(3) -0.0025(3) 0.0059(3) Ru N1 0.031(4) 0.036(4) 0.030(4) 0.008(3) -0.002(3) 0.008(3) N C1 0.036(5) 0.041(5) 0.039(5) 0.006(4) -0.004(5) 0.005(4) C C2 0.035(5) 0.057(6) 0.054(6) 0.014(4) -0.007(5) 0.009(5) C C3 0.031(5) 0.043(6) 0.062(7) -0.000(5) -0.018(5) 0.001(5) C C4 0.037(5) 0.039(5) 0.041(5) 0.013(4) -0.014(4) 0.006(4) C C5 0.064(7) 0.070(7) 0.039(6) 0.020(6) -0.019(5) 0.000(5) C C6 0.077(7) 0.080(8) 0.024(5) 0.031(6) -0.004(5) -0.003(5) C C7 0.050(6) 0.061(6) 0.043(6) 0.025(5) -0.002(5) 0.008(5) C C8 0.076(7) 0.088(8) 0.034(6) 0.041(5) 0.009(5) 0.002(6) C C9 0.054(6) 0.072(7) 0.051(6) 0.025(5) 0.011(5) 0.015(6) C C10 0.034(5) 0.057(6) 0.048(6) 0.017(4) 0.012(5) 0.010(5) C N2 0.036(4) 0.044(4) 0.023(4) 0.009(3) 0.001(3) -0.001(3) N C11 0.043(5) 0.036(5) 0.033(5) 0.015(4) 0.001(4) 0.002(4) C C12 0.051(5) 0.024(4) 0.031(5) 0.016(4) -0.012(4) 0.002(4) C N3 0.038(4) 0.034(4) 0.042(4) 0.009(3) 0.004(4) 0.007(4) N C13 0.051(6) 0.047(6) 0.052(6) 0.016(5) 0.003(5) 0.006(5) C C14 0.061(8) 0.042(7) 0.068(8) -0.003(6) -0.008(7) 0.003(6) C C15 0.077(7) 0.046(6) 0.076(8) 0.024(5) 0.018(6) 0.014(6) C C16 0.056(6) 0.061(6) 0.068(7) 0.035(4) 0.008(6) 0.018(5) C C17 0.038(5) 0.046(5) 0.043(5) 0.022(4) 0.002(4) 0.011(4) C C18 0.037(5) 0.049(5) 0.034(5) 0.017(4) 0.006(4) 0.008(4) C C19 0.045(5) 0.069(6) 0.049(6) 0.031(4) 0.001(5) 0.018(5) C C20 0.032(5) 0.071(7) 0.052(6) 0.015(5) -0.007(5) 0.007(6) C C21 0.028(5) 0.068(7) 0.044(6) 0.007(5) 0.004(5) 0.003(5) C C22 0.029(5) 0.063(6) 0.023(5) 0.008(4) 0.001(4) 0.006(4) C N4 0.025(4) 0.052(5) 0.033(4) 0.009(3) -0.002(3) 0.002(4) N C23 0.036(5) 0.036(5) 0.033(5) 0.004(4) 0.002(4) 0.003(4) C C24 0.051(7) 0.048(6) 0.043(6) -0.003(6) -0.000(5) 0.004(5) C C25 0.068(8) 0.031(6) 0.048(6) -0.003(5) 0.005(6) 0.003(5) C C26 0.064(7) 0.044(6) 0.039(5) 0.013(5) 0.012(5) 0.008(5) C C27 0.034(5) 0.036(5) 0.029(5) -0.000(4) -0.002(4) -0.003(4) C N5 0.033(4) 0.040(4) 0.029(4) 0.009(3) 0.004(3) 0.008(3) N S 0.035(1) 0.047(1) 0.034(1) 0.005(1) -0.002(1) 0.004(1) S C28 0.040(5) 0.038(5) 0.035(5) 0.007(4) 0.002(5) 0.003(4) C C29 0.047(5) 0.058(6) 0.048(6) 0.027(4) 0.010(5) 0.008(5) C C30 0.065(7) 0.064(6) 0.052(7) 0.033(5) 0.006(6) 0.010(5) C C31 0.077(8) 0.046(6) 0.056(7) 0.016(6) 0.009(6) 0.005(6) C C32 0.055(7) 0.044(6) 0.055(7) 0.011(5) -0.009(6) -0.001(5) C C33 0.055(6) 0.040(6) 0.036(5) 0.009(5) 0.005(5) 0.004(5) C N6 0.049(5) 0.054(5) 0.057(5) 0.017(4) -0.012(4) 0.006(4) N C34 0.044(6) 0.058(6) 0.043(6) 0.018(5) -0.006(5) 0.002(5) C C35 0.061(7) 0.067(7) 0.054(7) 0.024(5) -0.012(6) 0.004(6) C C36 0.085(8) 0.086(8) 0.045(7) 0.037(6) -0.004(6) 0.008(6) C C37 0.094(8) 0.078(7) 0.041(6) 0.044(6) 0.013(6) 0.026(5) C C38 0.063(7) 0.062(7) 0.039(6) 0.012(6) 0.005(6) 0.011(5) C C39 0.042(6) 0.054(6) 0.031(5) 0.008(5) 0.006(5) 0.011(4) C P1 0.037(1) 0.062(2) 0.046(2) 0.015(1) 0.001(1) 0.012(1) P F1 0.046(4) 0.069(5) 0.144(7) 0.007(4) 0.013(5) 0.005(5) F F2 0.048(4) 0.105(6) 0.135(7) 0.001(4) 0.008(5) 0.049(5) F F3 0.096(5) 0.27(1) 0.063(5) 0.087(5) 0.019(4) 0.027(6) F F4 0.069(6) 0.55(2) 0.057(5) 0.03(1) -0.005(5) 0.100(8) F F5 0.085(5) 0.086(5) 0.23(1) 0.048(4) -0.012(7) -0.025(7) F F6 0.075(5) 0.055(4) 0.29(1) 0.021(4) -0.013(7) 0.039(6) F P2 0.055(2) 0.052(2) 0.075(2) 0.009(1) -0.014(2) 0.007(2) P F7 0.141(6) 0.104(5) 0.146(7) 0.077(4) -0.075(5) -0.037(5) F F8 0.19(1) 0.200(9) 0.22(1) -0.110(9) -0.092(9) 0.143(7) F F9 0.33(1) 0.170(6) 0.125(9) 0.181(5) 0.012(8) 0.010(6) F F10 0.191(8) 0.127(7) 0.146(7) 0.035(6) -0.112(5) 0.019(5) F F11 0.140(9) 0.113(8) 0.18(1) -0.027(8) 0.062(8) 0.021(8) F F12 0.134(6) 0.197(7) 0.137(8) 0.117(4) 0.036(6) 0.046(6) F C40 0.16(2) 0.16(4) 0.16(4) 0.06(3) 0.02(3) 0.03(3) C C41 0.1620(2) 0.16(4) 0.16(4) 0.06(3) 0.02(3) 0.03(3) C C42 0.1746(2) 0.17(4) 0.17(4) 0.07(3) 0.03(4) 0.03(4) C C43 0.1746(2) 0.17(4) 0.17(4) 0.07(3) 0.03(4) 0.03(4) C C44 0.1746(2) 0.17(4) 0.17(4) 0.07(3) 0.03(4) 0.03(3) C C45 0.1746(2) 0.17(4) 0.17(4) 0.07(3) 0.03(4) 0.03(3) C C46 0.1772(2) 0.18(4) 0.18(4) 0.07(3) 0.03(4) 0.03(4) C C47 0.1809(2) 0.18(4) 0.18(5) 0.07(3) 0.03(5) 0.03(4) C O3 0.22(3) 0.22(3) 0.22(4) 0.08(3) 0.03(3) 0.04(3) O C48 0.05(1) 0.05(1) 0.05(1) 0.019(9) 0.01(1) 0.01(1) C O4 0.15(2) 0.15(2) 0.15(2) 0.06(2) 0.02(2) 0.03(2) O C49 0.10(2) 0.10(2) 0.10(2) 0.04(2) 0.01(2) 0.02(2) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU N1 2.104(8) . . ? RU N2 2.069(8) . . ? RU N3 2.068(9) . . ? RU N4 1.956(8) . . ? RU N5 2.056(9) . . ? RU S 2.375(3) . . ? N1 C1 1.32(1) . . ? N1 C12 1.36(1) . . ? C1 C2 1.40(1) . . ? C2 C3 1.36(2) . . ? C3 C4 1.41(2) . . ? C4 C5 1.41(2) . . ? C4 C12 1.42(1) . . ? C5 C6 1.34(2) . . ? C6 C7 1.45(2) . . ? C7 C8 1.40(2) . . ? C7 C11 1.40(2) . . ? C8 C9 1.37(2) . . ? C9 C10 1.38(2) . . ? C10 N2 1.32(1) . . ? N2 C11 1.37(1) . . ? C11 C12 1.43(2) . . ? N3 C13 1.33(1) . . ? N3 C17 1.38(1) . . ? C13 C14 1.39(2) . . ? C14 C15 1.38(2) . . ? C15 C16 1.40(2) . . ? C16 C17 1.38(2) . . ? C17 C18 1.48(2) . . ? C18 C19 1.39(1) . . ? C18 N4 1.35(1) . . ? C19 C20 1.38(2) . . ? C20 C21 1.38(2) . . ? C21 C22 1.39(1) . . ? C22 N4 1.36(1) . . ? C22 C23 1.44(2) . . ? C23 C24 1.39(2) . . ? C23 N5 1.36(1) . . ? C24 C25 1.39(2) . . ? C25 C26 1.37(2) . . ? C26 C27 1.37(2) . . ? C27 N5 1.33(1) . . ? S C28 1.77(1) . . ? S C39 1.77(1) . . ? C28 C29 1.39(2) . . ? C28 C33 1.39(2) . . ? C29 C30 1.37(2) . . ? C30 C31 1.41(2) . . ? C31 C32 1.37(2) . . ? C32 C33 1.40(2) . . ? C33 N6 1.41(2) . . ? N6 C34 1.40(2) . . ? C34 C35 1.39(2) . . ? C34 C39 1.39(2) . . ? C35 C36 1.37(2) . . ? C36 C37 1.39(2) . . ? C37 C38 1.37(2) . . ? C38 C39 1.40(2) . . ? P1 F1 1.595(8) . . ? P1 F2 1.578(9) . . ? P1 F3 1.550(9) . . ? P1 F4 1.50(1) . . ? P1 F5 1.55(1) . . ? P1 F6 1.57(1) . . ? P2 F7 1.58(1) . . ? P2 F8 1.51(1) . . ? P2 F9 1.54(1) . . ? P2 F10 1.53(1) . . ? P2 F11 1.52(1) . . ? P2 F12 1.57(1) . . ? C40 C41 1.39(3) . . ? C40 C45 1.38(3) . . ? C40 C46 1.38(4) . . ? C41 C42 1.3850 . . ? C42 C43 1.3850 . . ? C43 C44 1.3850 . . ? C43 C47 1.3850 . . ? C43 C47 1.5247 . 2_676 ? C44 C45 1.3773 . . ? C44 C47 1.3401 . 2_676 ? C47 C47 1.5920 . 2_676 ? O3 C48 1.25(6) . . ? O3 C49 1.09(5) . . ? C48 O4 1.33(4) . . ? C48 C49 1.14(5) . . ? O4 C49 1.57(6) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 RU N2 79.5(4) . . . ? N1 RU N3 96.5(3) . . . ? N1 RU N4 172.1(4) . . . ? N1 RU N5 103.9(3) . . . ? N1 RU S 93.4(3) . . . ? N2 RU N3 91.6(4) . . . ? N2 RU N4 93.3(4) . . . ? N2 RU N5 88.3(3) . . . ? N2 RU S 172.8(3) . . . ? N3 RU N4 80.1(4) . . . ? N3 RU N5 159.2(3) . . . ? N3 RU S 90.6(3) . . . ? N4 RU N5 79.2(4) . . . ? N4 RU S 93.8(3) . . . ? N5 RU S 92.2(2) . . . ? C1 N1 C12 117.1(9) . . . ? N1 C1 C2 124(1) . . . ? C1 C2 C3 119(1) . . . ? C2 C3 C4 119(1) . . . ? C3 C4 C5 124(1) . . . ? C3 C4 C12 116(1) . . . ? C5 C4 C12 119(1) . . . ? C4 C5 C6 121(1) . . . ? C5 C6 C7 121(1) . . . ? C6 C7 C8 125(1) . . . ? C6 C7 C11 118(1) . . . ? C8 C7 C11 116(1) . . . ? C7 C8 C9 120(1) . . . ? C8 C9 C10 119(1) . . . ? C9 C10 N2 123(1) . . . ? C10 N2 C11 117.6(9) . . . ? C7 C11 N2 122(1) . . . ? C7 C11 C12 120(1) . . . ? N2 C11 C12 116.5(9) . . . ? N1 C12 C4 123(1) . . . ? N1 C12 C11 117.3(9) . . . ? C4 C12 C11 119(1) . . . ? C13 N3 C17 118(1) . . . ? N3 C13 C14 123(1) . . . ? C13 C14 C15 118(1) . . . ? C14 C15 C16 118(1) . . . ? C15 C16 C17 120(1) . . . ? N3 C17 C16 121(1) . . . ? N3 C17 C18 114(1) . . . ? C16 C17 C18 124(1) . . . ? C17 C18 C19 125(1) . . . ? C17 C18 N4 113.4(9) . . . ? C19 C18 N4 120(1) . . . ? C18 C19 C20 117(1) . . . ? C19 C20 C21 122(1) . . . ? C20 C21 C22 118(1) . . . ? C21 C22 N4 119(1) . . . ? C21 C22 C23 128(1) . . . ? N4 C22 C23 112.2(9) . . . ? C18 N4 C22 122.1(9) . . . ? C22 C23 C24 123(1) . . . ? C22 C23 N5 116(1) . . . ? C24 C23 N5 120(1) . . . ? C23 C24 C25 119(1) . . . ? C24 C25 C26 118(1) . . . ? C25 C26 C27 118(1) . . . ? C26 C27 N5 123(1) . . . ? C23 N5 C27 118.5(9) . . . ? C28 S C39 99.5(5) . . . ? S C28 C29 117.9(9) . . . ? S C28 C33 120.9(9) . . . ? C29 C28 C33 121(1) . . . ? C28 C29 C30 120(1) . . . ? C29 C30 C31 119(1) . . . ? C30 C31 C32 119(1) . . . ? C31 C32 C33 121(1) . . . ? C28 C33 C32 117(1) . . . ? C28 C33 N6 122(1) . . . ? C32 C33 N6 119(1) . . . ? C33 N6 C34 120(1) . . . ? N6 C34 C35 118(1) . . . ? N6 C34 C39 122(1) . . . ? C35 C34 C39 118(1) . . . ? C34 C35 C36 121(1) . . . ? C35 C36 C37 119(1) . . . ? C36 C37 C38 120(1) . . . ? C37 C38 C39 119(1) . . . ? S C39 C34 121(1) . . . ? S C39 C38 118.5(9) . . . ? C34 C39 C38 119(1) . . . ? F1 P1 F2 177.8(6) . . . ? F1 P1 F3 91.6(6) . . . ? F1 P1 F4 87.9(6) . . . ? F1 P1 F5 91.2(5) . . . ? F1 P1 F6 86.5(5) . . . ? F2 P1 F3 90.5(6) . . . ? F2 P1 F4 90.0(6) . . . ? F2 P1 F5 88.4(6) . . . ? F2 P1 F6 94.1(6) . . . ? F3 P1 F4 179.5(9) . . . ? F3 P1 F5 87.7(7) . . . ? F3 P1 F6 86.4(7) . . . ? F4 P1 F5 92(1) . . . ? F4 P1 F6 93(1) . . . ? F5 P1 F6 173.6(8) . . . ? F7 P2 F8 86.9(7) . . . ? F7 P2 F9 91.7(7) . . . ? F7 P2 F10 177.9(9) . . . ? F7 P2 F11 91.4(8) . . . ? F7 P2 F12 85.9(6) . . . ? F8 P2 F9 88(1) . . . ? F8 P2 F10 91.3(7) . . . ? F8 P2 F11 178.2(8) . . . ? F8 P2 F12 95(1) . . . ? F9 P2 F10 89.5(8) . . . ? F9 P2 F11 91.9(9) . . . ? F9 P2 F12 175.1(9) . . . ? F10 P2 F11 90.3(8) . . . ? F10 P2 F12 93.0(8) . . . ? F11 P2 F12 84.0(8) . . . ? C41 C40 C45 120(2) . . . ? C41 C40 C46 120(2) . . . ? C45 C40 C46 119(1) . . . ? C40 C41 C42 120(1) . . . ? C41 C42 C43 120.00 . . . ? C42 C43 C44 119.63 . . . ? C42 C43 C47 120.00 . . . ? C42 C43 C47 171.54 . . 2_676 ? C44 C43 C47 120.37 . . . ? C44 C43 C47 54.59 . . 2_676 ? C47 C43 C47 66.14 . . 2_676 ? C43 C44 C45 120.55 . . . ? C43 C44 C47 68.02 . . 2_676 ? C45 C44 C47 169.20 . . 2_676 ? C40 C45 C44 119(1) . . . ? C43 C47 C43 113.86 . . 2_676 ? C43 C47 C44 169.35 . . 2_676 ? C43 C47 C47 61.15 . . 2_676 ? C43 C47 C44 57.39 2_676 . 2_676 ? C43 C47 C47 52.71 2_676 . 2_676 ? C44 C47 C47 109.81 2_676 . 2_676 ? C48 O3 C49 57(4) . . . ? O3 C48 O4 113(3) . . . ? O3 C48 C49 53(3) . . . ? O4 C48 C49 78(3) . . . ? C48 O4 C49 45(2) . . . ? O3 C49 C48 68(4) . . . ? O3 C49 O4 106(6) . . . ? C48 C49 O4 56(3) . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.970 #===END data_Complex_8 _database_code_depnum_ccdc_archive 'CCDC 218279' _audit_creation_date 30-09-03 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(terpy)(phen)(MQT)][PF6]3 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C164 H140 F72 N34 O P12 Ru4' _chemical_formula_weight 4747.02 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1 #========================================================================== #==== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 17.0076(5) _cell_length_b 17.7093(6) _cell_length_c 18.7337(5) _cell_angle_alpha 62.319(5) _cell_angle_beta 85.332(5) _cell_angle_gamma 71.423(5) _cell_volume 4721.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173 _cell_measurement_reflns_used 31400 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.67 _exptl_crystal_density_method none _exptl_crystal_F_000 2374 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #========================================================================== #==== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 31400 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 50 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 91 frames Set 2 Theta = -3.40 Kappa = 174.50 Phi = 0.00 22 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31400 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.49 _reflns_number_total 21458 _reflns_number_gt 10147 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #========================================================================== #==== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 10147 _refine_ls_number_parameters 1279 _refine_ls_number_restraints 0 _refine_ls_number_constraints 18 _refine_ls_R_factor_all 0.164 _refine_ls_R_factor_gt 0.084 _refine_ls_wR_factor_all 0.244 _refine_ls_wR_factor_ref 0.104 _refine_ls_goodness_of_fit_all 1.267 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_shift/su_max 0.048 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 1.370 _refine_diff_density_min -0.976 #========================================================================== #==== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RU1 0.65291(5) 0.21146(5) 0.84940(4) 0.0298(3) 1.000 Uani ? ? Ru N1 0.5359(5) 0.1919(5) 0.8683(5) 0.034(4) 1.000 Uani ? ? N C1 0.5101(7) 0.1284(7) 0.8689(7) 0.052(5) 1.000 Uani ? ? C C2 0.4272(7) 0.1298(7) 0.8761(8) 0.062(6) 1.000 Uani ? ? C C3 0.3686(7) 0.1962(7) 0.8868(7) 0.049(5) 1.000 Uani ? ? C C4 0.3927(6) 0.2647(7) 0.8868(6) 0.044(5) 1.000 Uani ? ? C C5 0.3360(7) 0.3388(8) 0.8978(6) 0.045(6) 1.000 Uani ? ? C C6 0.3620(7) 0.4051(7) 0.8953(6) 0.050(6) 1.000 Uani ? ? C C7 0.4451(7) 0.4048(7) 0.8797(6) 0.039(5) 1.000 Uani ? ? C C8 0.4749(8) 0.4729(7) 0.8717(6) 0.050(6) 1.000 Uani ? ? C C9 0.5546(8) 0.4687(7) 0.8560(7) 0.053(5) 1.000 Uani ? ? C C10 0.6063(7) 0.3965(7) 0.8433(6) 0.043(5) 1.000 Uani ? ? C N2 0.5827(5) 0.3282(5) 0.8515(4) 0.034(3) 1.000 Uani ? ? N C11 0.5015(6) 0.3320(6) 0.8698(5) 0.033(4) 1.000 Uani ? ? C C12 0.4761(6) 0.2614(6) 0.8763(5) 0.032(4) 1.000 Uani ? ? C N3 0.6411(6) 0.2681(5) 0.7244(5) 0.043(4) 1.000 Uani ? ? N C13 0.5835(8) 0.2743(7) 0.6760(6) 0.056(6) 1.000 Uani ? ? C C14 0.582(1) 0.3140(9) 0.5945(8) 0.077(8) 1.000 Uani ? ? C C15 0.643(1) 0.352(1) 0.5566(8) 0.09(1) 1.000 Uani ? ? C C16 0.702(1) 0.347(1) 0.6043(8) 0.076(9) 1.000 Uani ? ? C C17 0.7025(8) 0.3048(8) 0.6883(7) 0.052(6) 1.000 Uani ? ? C C18 0.7652(8) 0.2948(8) 0.7434(7) 0.060(6) 1.000 Uani ? ? C C19 0.8294(9) 0.329(1) 0.723(1) 0.093(9) 1.000 Uani ? ? C C20 0.8820(9) 0.317(1) 0.780(1) 0.095(9) 1.000 Uani ? ? C C21 0.8698(8) 0.2721(8) 0.8612(9) 0.087(6) 1.000 Uani ? ? C C22 0.8027(7) 0.2354(7) 0.8825(7) 0.050(5) 1.000 Uani ? ? C N4 0.7529(5) 0.2476(5) 0.8239(5) 0.041(4) 1.000 Uani ? ? N C23 0.7754(7) 0.1897(7) 0.9632(6) 0.052(5) 1.000 Uani ? ? C C24 0.8154(9) 0.1689(8) 1.0348(7) 0.078(6) 1.000 Uani ? ? C C25 0.783(1) 0.1309(9) 1.1068(7) 0.087(8) 1.000 Uani ? ? C C26 0.709(1) 0.1141(9) 1.1078(7) 0.062(7) 1.000 Uani ? ? C C27 0.6704(9) 0.1348(7) 1.0349(7) 0.049(6) 1.000 Uani ? ? C N5 0.7010(6) 0.1717(5) 0.9640(4) 0.037(4) 1.000 Uani ? ? N N6 0.7185(5) 0.0835(5) 0.8606(4) 0.030(3) 1.000 Uani ? ? N C28 0.7759(6) 0.0703(6) 0.8095(5) 0.035(4) 1.000 Uani ? ? C C29 0.8198(6) -0.0138(6) 0.8171(5) 0.035(4) 1.000 Uani ? ? C C30 0.8045(6) -0.0896(6) 0.8786(5) 0.035(4) 1.000 Uani ? ? C C31 0.7459(7) -0.0763(7) 0.9306(6) 0.039(5) 1.000 Uani ? ? C C32 0.7060(6) 0.0095(7) 0.9203(6) 0.038(5) 1.000 Uani ? ? C C33 0.8486(6) -0.1797(6) 0.8875(5) 0.034(4) 1.000 Uani ? ? C C34 0.8063(7) -0.2403(7) 0.9016(6) 0.040(5) 1.000 Uani ? ? C C35 0.8496(8) -0.3238(7) 0.9067(6) 0.051(6) 1.000 Uani ? ? C N7 0.9320(6) -0.3469(5) 0.8971(5) 0.042(4) 1.000 Uani ? ? N C36 0.9729(8) -0.2900(7) 0.8849(6) 0.042(5) 1.000 Uani ? ? C C37 0.9347(7) -0.2060(7) 0.8786(6) 0.042(5) 1.000 Uani ? ? C C38 0.974(1) -0.4331(8) 0.8946(7) 0.065(7) 1.000 Uani ? ? C RU2 0.63072(5) 0.21828(5) 1.35135(4) 0.0313(3) 1.000 Uani ? ? Ru N8 0.7418(5) 0.2497(5) 1.3124(4) 0.037(4) 1.000 Uani ? ? N C39 0.8112(7) 0.2024(7) 1.2955(6) 0.049(5) 1.000 Uani ? ? C C40 0.8833(8) 0.228(1) 1.2784(8) 0.071(8) 1.000 Uani ? ? C C41 0.8800(8) 0.3064(9) 1.2758(8) 0.073(7) 1.000 Uani ? ? C C42 0.8086(8) 0.3605(8) 1.2898(7) 0.054(6) 1.000 Uani ? ? C C43 0.8005(9) 0.4433(9) 1.2895(9) 0.081(7) 1.000 Uani ? ? C C44 0.7281(9) 0.4932(7) 1.3021(8) 0.067(6) 1.000 Uani ? ? C C45 0.6554(9) 0.4641(7) 1.3203(7) 0.058(6) 1.000 Uani ? ? C C46 0.5789(9) 0.5110(7) 1.3356(7) 0.059(6) 1.000 Uani ? ? C C47 0.5134(9) 0.4783(7) 1.3498(6) 0.049(6) 1.000 Uani ? ? C C48 0.5254(7) 0.3930(7) 1.3541(6) 0.046(5) 1.000 Uani ? ? C N9 0.5981(5) 0.3454(5) 1.3412(4) 0.036(4) 1.000 Uani ? ? N C49 0.6636(7) 0.3803(6) 1.3244(6) 0.040(5) 1.000 Uani ? ? C C50 0.7386(7) 0.3297(7) 1.3084(6) 0.046(5) 1.000 Uani ? ? C N10 0.5672(5) 0.2662(5) 1.2415(4) 0.031(4) 1.000 Uani ? ? N C51 0.5942(7) 0.3012(6) 1.1664(5) 0.039(4) 1.000 Uani ? ? C C52 0.5429(7) 0.3376(6) 1.0967(6) 0.040(5) 1.000 Uani ? ? C C53 0.4621(8) 0.3395(7) 1.1043(6) 0.048(5) 1.000 Uani ? ? C C54 0.4325(7) 0.3018(6) 1.1807(6) 0.046(5) 1.000 Uani ? ? C C55 0.4877(6) 0.2649(6) 1.2491(6) 0.038(4) 1.000 Uani ? ? C C56 0.4630(6) 0.2207(6) 1.3318(6) 0.037(5) 1.000 Uani ? ? C C57 0.3918(7) 0.1985(8) 1.3574(7) 0.058(6) 1.000 Uani ? ? C C58 0.3842(7) 0.1528(8) 1.4385(7) 0.066(6) 1.000 Uani ? ? C C59 0.4467(8) 0.1275(8) 1.4946(7) 0.055(6) 1.000 Uani ? ? C C60 0.5173(7) 0.1512(6) 1.4680(6) 0.039(5) 1.000 Uani ? ? C N11 0.5263(5) 0.1957(5) 1.3873(4) 0.035(3) 1.000 Uani ? ? N C61 0.5911(7) 0.1331(6) 1.5182(6) 0.042(5) 1.000 Uani ? ? C C62 0.5979(8) 0.0879(8) 1.6019(6) 0.051(6) 1.000 Uani ? ? C C63 0.6684(8) 0.0738(8) 1.6432(6) 0.051(6) 1.000 Uani ? ? C C64 0.7314(8) 0.1066(8) 1.6007(6) 0.052(6) 1.000 Uani ? ? C C65 0.7210(7) 0.1512(7) 1.5168(6) 0.048(5) 1.000 Uani ? ? C N12 0.6534(5) 0.1628(5) 1.4759(4) 0.035(4) 1.000 Uani ? ? N N13 0.6787(5) 0.0894(5) 1.3625(4) 0.033(4) 1.000 Uani ? ? N C66 0.7488(6) 0.0283(6) 1.4109(5) 0.035(4) 1.000 Uani ? ? C C67 0.7859(6) -0.0551(7) 1.4178(6) 0.038(5) 1.000 Uani ? ? C C68 0.7509(6) -0.0837(6) 1.3747(5) 0.033(5) 1.000 Uani ? ? C C69 0.6755(6) -0.0259(6) 1.3290(5) 0.035(4) 1.000 Uani ? ? C C70 0.6425(6) 0.0577(6) 1.3245(5) 0.034(4) 1.000 Uani ? ? C C71 0.7906(7) -0.1729(7) 1.3780(6) 0.038(5) 1.000 Uani ? ? C C72 0.7821(9) -0.1855(8) 1.3113(7) 0.056(6) 1.000 Uani ? ? C C73 0.821(1) -0.2676(8) 1.3145(7) 0.070(7) 1.000 Uani ? ? C N14 0.8661(8) -0.3354(6) 1.3797(5) 0.056(5) 1.000 Uani ? ? N C74 0.8751(9) -0.3256(8) 1.4441(7) 0.053(7) 1.000 Uani ? ? C C75 0.8399(8) -0.2460(7) 1.4450(6) 0.047(6) 1.000 Uani ? ? C C76 0.906(1) -0.428(1) 1.3857(9) 0.09(1) 1.000 Uani ? ? C P1 0.5396(2) -0.0852(2) 0.8317(2) 0.049(1) 1.000 Uani ? ? P F1 0.5582(6) -0.0932(5) 0.7512(4) 0.100(4) 1.000 Uani ? ? F F2 0.6057(5) -0.1824(5) 0.8826(5) 0.089(4) 1.000 Uani ? ? F F3 0.6079(5) -0.0385(5) 0.8189(5) 0.101(4) 1.000 Uani ? ? F F4 0.4696(5) -0.1315(4) 0.8441(4) 0.081(4) 1.000 Uani ? ? F F5 0.4730(5) 0.0101(5) 0.7820(5) 0.076(4) 1.000 Uani ? ? F F6 0.5186(6) -0.0759(4) 0.9125(4) 0.073(4) 1.000 Uani ? ? F P2 0.9110(2) -0.3513(2) 1.1365(2) 0.054(1) 1.000 Uani ? ? P F7 0.8860(6) -0.3997(5) 1.0941(4) 0.106(4) 1.000 Uani ? ? F F8 0.9701(7) -0.4438(6) 1.2011(5) 0.124(5) 1.000 Uani ? ? F F9 0.9810(6) -0.3338(9) 1.0783(6) 0.149(7) 1.000 Uani ? ? F F10 0.8464(5) -0.2602(5) 1.0752(4) 0.061(4) 1.000 Uani ? ? F F11 0.9341(5) -0.3018(4) 1.1808(4) 0.083(4) 1.000 Uani ? ? F F12 0.8366(5) -0.3655(5) 1.1947(4) 0.089(4) 1.000 Uani ? ? F P3 0.8493(2) -0.1784(3) 1.6564(2) 0.058(2) 1.000 Uani ? ? P F13 0.8201(6) -0.2266(5) 1.6146(4) 0.085(4) 1.000 Uani ? ? F F14 0.9149(6) -0.2692(8) 1.7151(6) 0.100(7) 1.000 Uani ? ? F F15 0.9131(6) -0.1566(8) 1.5903(5) 0.108(6) 1.000 Uani ? ? F F16 0.8775(8) -0.1309(7) 1.6982(5) 0.152(6) 1.000 Uani ? ? F F17 0.7859(6) -0.2059(8) 1.7226(5) 0.118(6) 1.000 Uani ? ? F F18 0.7818(8) -0.0898(6) 1.6000(5) 0.112(6) 1.000 Uani ? ? F P4 0.7763(2) 0.4249(2) 1.0064(2) 0.058(2) 1.000 Uani ? ? P F19 0.7363(7) 0.3893(6) 0.9635(6) 0.216(6) 1.000 Uani ? ? F F20 0.8235(8) 0.3262(6) 1.0657(7) 0.139(8) 1.000 Uani ? ? F F21 0.8526(8) 0.421(1) 0.9616(8) 0.22(1) 1.000 Uani ? ? F F22 0.8186(7) 0.4586(6) 1.0505(7) 0.164(6) 1.000 Uani ? ? F F23 0.7327(9) 0.5255(8) 0.9510(9) 0.139(9) 1.000 Uani ? ? F F24 0.7042(8) 0.4288(7) 1.0557(8) 0.331(7) 1.000 Uani ? ? F P5 0.3390(4) 0.3862(4) 1.5046(6) 0.201(4) 1.000 Uani ? ? P F25 0.3874(7) 0.4401(7) 1.5181(6) 0.129(7) 1.000 Uani ? ? F F26 0.340(1) 0.326(1) 1.588(1) 0.21(1) 1.000 Uani ? ? F F27 0.290(1) 0.340(1) 1.482(1) 0.25(2) 1.000 Uani ? ? F F28 0.341(1) 0.457(1) 1.395(1) 0.24(2) 1.000 Uani ? ? F F29 0.254(1) 0.462(1) 1.496(1) 0.25(2) 1.000 Uani ? ? F F30 0.4242(7) 0.3202(7) 1.4993(6) 0.121(7) 1.000 Uani ? ? F P6 0.9835(2) -0.0616(3) 1.2747(3) 0.091(3) 1.000 Uani ? ? P F31 0.8981(2) -0.0485(3) 1.2394(3) 0.18(1) 1.000 Uani ? ? F F32 1.0267(2) -0.0820(3) 1.2066(3) 0.26(2) 1.000 Uani ? ? F F33 1.0690(2) -0.0747(3) 1.3100(3) 0.20(1) 1.000 Uani ? ? F F34 0.9404(2) -0.0412(3) 1.3428(3) 0.41(3) 1.000 Uani ? ? F F35 0.9954(2) -0.1630(3) 1.3286(3) 0.39(3) 1.000 Uani ? ? F F36 0.9717(2) 0.0398(3) 1.2209(3) 0.34(3) 1.000 Uani ? ? F C77 0.909(1) -0.082(1) 1.063(2) 0.12(1) 1.000 Uani ? ? C C78 0.8304(9) -0.0852(8) 1.0955(9) 0.069(7) 1.000 Uani ? ? C N15 0.7655(8) -0.0859(7) 1.1150(6) 0.074(6) 1.000 Uani ? ? N C87 0.075(2) 0.642(2) 0.463(1) 0.16(2) 1.000 Uani ? ? C C88 0.082(2) 0.706(2) 0.487(1) 0.15(2) 1.000 Uani ? ? C N20 0.106(2) 0.743(2) 0.509(2) 0.29(3) 1.000 Uani ? ? N C90 0.094(2) 0.462(2) 0.369(2) 0.25(3) 1.000 Uani ? ? C C91 0.140(2) 0.441(2) 0.316(2) 0.22(3) 1.000 Uani ? ? C N21 0.204(2) 0.435(2) 0.268(2) 0.25(2) 1.000 Uani ? ? N O1 0.948(2) 0.044(2) 1.488(2) 0.12(2) 0.500 Uani ? ? O H1 0.5499 0.0795 0.8641 0.0661 1.000 Uiso calc C1 H H2 0.4117 0.0841 0.8736 0.0758 1.000 Uiso calc C2 H H3 0.3127 0.1960 0.8941 0.0654 1.000 Uiso calc C3 H H4 0.2797 0.3411 0.9069 0.0658 1.000 Uiso calc C5 H H5 0.3241 0.4521 0.9040 0.0684 1.000 Uiso calc C6 H H6 0.4387 0.5229 0.8773 0.0708 1.000 Uiso calc C8 H H7 0.5755 0.5135 0.8536 0.0690 1.000 Uiso calc C9 H H8 0.6610 0.3967 0.8281 0.0573 1.000 Uiso calc C10 H H9 0.5407 0.2490 0.7006 0.0767 1.000 Uiso calc C13 H H10 0.5390 0.3160 0.5635 0.1227 1.000 Uiso calc C14 H H11 0.6435 0.3797 0.4993 0.1588 1.000 Uiso calc C15 H H12 0.7444 0.3733 0.5797 0.1238 1.000 Uiso calc C16 H H13 0.8373 0.3627 0.6673 0.1186 1.000 Uiso calc C19 H H14 0.9281 0.3385 0.7652 0.1252 1.000 Uiso calc C20 H H15 0.9050 0.2661 0.9016 0.1097 1.000 Uiso calc C21 H H16 0.8660 0.1814 1.0334 0.0990 1.000 Uiso calc C24 H H17 0.8112 0.1161 1.1557 0.1237 1.000 Uiso calc C25 H H18 0.6849 0.0888 1.1573 0.1021 1.000 Uiso calc C26 H H19 0.6200 0.1219 1.0363 0.0777 1.000 Uiso calc C27 H H20 0.7866 0.1213 0.7664 0.0470 1.000 Uiso calc C28 H H21 0.8603 -0.0198 0.7804 0.0452 1.000 Uiso calc C29 H H22 0.7332 -0.1261 0.9734 0.0548 1.000 Uiso calc C31 H H23 0.6673 0.0165 0.9580 0.0525 1.000 Uiso calc C32 H H24 0.7483 -0.2246 0.9078 0.0558 1.000 Uiso calc C34 H H25 0.8208 -0.3655 0.9172 0.0673 1.000 Uiso calc C35 H H26 1.0312 -0.3082 0.8805 0.0630 1.000 Uiso calc C36 H H27 0.9656 -0.1663 0.8684 0.0565 1.000 Uiso calc C37 H H28 1.0313 -0.4400 0.8876 0.0878 1.000 Uiso calc C38 H H29 0.9682 -0.4817 0.9439 0.0878 1.000 Uiso calc C38 H H30 0.9491 -0.4328 0.8508 0.0878 1.000 Uiso calc C38 H H31 0.8120 0.1487 1.2950 0.0639 1.000 Uiso calc C39 H H32 0.9329 0.1907 1.2689 0.0970 1.000 Uiso calc C40 H H33 0.9283 0.3248 1.2640 0.0965 1.000 Uiso calc C41 H H34 0.8475 0.4637 1.2803 0.1109 1.000 Uiso calc C43 H H35 0.7247 0.5493 1.2990 0.0925 1.000 Uiso calc C44 H H36 0.5723 0.5660 1.3363 0.0855 1.000 Uiso calc C46 H H37 0.4602 0.5123 1.3567 0.0743 1.000 Uiso calc C47 H H38 0.4803 0.3694 1.3665 0.0620 1.000 Uiso calc C48 H H39 0.6504 0.3008 1.1614 0.0494 1.000 Uiso calc C51 H H40 0.5637 0.3606 1.0449 0.0578 1.000 Uiso calc C52 H H41 0.4255 0.3667 1.0572 0.0680 1.000 Uiso calc C53 H H42 0.3767 0.3012 1.1862 0.0585 1.000 Uiso calc C54 H H43 0.3483 0.2147 1.3192 0.0727 1.000 Uiso calc C57 H H44 0.3345 0.1384 1.4562 0.0781 1.000 Uiso calc C58 H H45 0.4415 0.0942 1.5507 0.0718 1.000 Uiso calc C59 H H46 0.5542 0.0669 1.6304 0.0690 1.000 Uiso calc C62 H H47 0.6744 0.0418 1.7006 0.0727 1.000 Uiso calc C63 H H48 0.7801 0.0987 1.6284 0.0703 1.000 Uiso calc C64 H H49 0.7633 0.1742 1.4874 0.0611 1.000 Uiso calc C65 H H50 0.7735 0.0454 1.4423 0.0471 1.000 Uiso calc C66 H H51 0.8356 -0.0935 1.4518 0.0526 1.000 Uiso calc C67 H H52 0.6474 -0.0444 1.3013 0.0464 1.000 Uiso calc C69 H H53 0.5913 0.0960 1.2930 0.0444 1.000 Uiso calc C70 H H54 0.7492 -0.1373 1.2638 0.0834 1.000 Uiso calc C72 H H55 0.8157 -0.2757 1.2687 0.1065 1.000 Uiso calc C73 H H56 0.9072 -0.3758 1.4910 0.0846 1.000 Uiso calc C74 H H57 0.8489 -0.2401 1.4913 0.0693 1.000 Uiso calc C75 H H58 0.8951 -0.4266 1.3359 0.1535 1.000 Uiso calc C76 H H59 0.9644 -0.4468 1.3972 0.1535 1.000 Uiso calc C76 H H60 0.8834 -0.4701 1.4278 0.1535 1.000 Uiso calc C76 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RU1 0.0269(3) 0.0294(3) 0.0335(3) -0.0063(2) -0.0011(3) -0.0165(2) Ru N1 0.023(4) 0.031(3) 0.054(4) -0.003(3) 0.003(3) -0.021(3) N C1 0.031(5) 0.050(4) 0.089(6) -0.010(4) 0.009(5) -0.049(3) C C2 0.046(6) 0.058(5) 0.090(7) -0.026(4) 0.013(5) -0.044(4) C C3 0.031(5) 0.059(5) 0.067(6) -0.015(4) 0.008(5) -0.033(4) C C4 0.030(5) 0.060(5) 0.046(4) -0.007(4) 0.005(4) -0.032(3) C C5 0.038(6) 0.054(6) 0.044(5) 0.002(5) 0.003(5) -0.020(4) C C6 0.043(6) 0.053(5) 0.054(5) 0.007(5) -0.000(5) -0.033(4) C C7 0.049(6) 0.038(5) 0.031(4) 0.006(4) -0.008(4) -0.017(3) C C8 0.078(8) 0.029(4) 0.055(5) -0.001(5) -0.009(5) -0.026(3) C C9 0.075(7) 0.039(4) 0.051(5) -0.020(4) -0.001(5) -0.023(3) C C10 0.053(6) 0.035(4) 0.042(5) -0.013(4) -0.007(4) -0.016(3) C N2 0.040(4) 0.029(3) 0.035(3) -0.007(3) -0.003(3) -0.018(2) N C11 0.036(5) 0.032(4) 0.031(4) 0.003(4) -0.007(4) -0.014(3) C C12 0.034(5) 0.029(4) 0.034(4) -0.002(3) 0.000(4) -0.017(3) C N3 0.057(5) 0.038(4) 0.038(4) -0.003(4) -0.007(4) -0.018(3) N C13 0.070(7) 0.048(5) 0.052(5) 0.010(5) -0.032(5) -0.030(3) C C14 0.14(1) 0.052(6) 0.061(6) 0.024(8) -0.043(7) -0.031(4) C C15 0.20(2) 0.09(1) 0.038(7) 0.00(1) -0.030(9) -0.019(6) C C16 0.14(1) 0.063(8) 0.048(7) -0.020(9) 0.031(8) -0.012(6) C C17 0.064(7) 0.050(5) 0.044(5) -0.014(5) 0.015(5) -0.023(4) C C18 0.060(7) 0.054(6) 0.066(6) -0.020(5) 0.015(6) -0.028(4) C C19 0.079(8) 0.090(8) 0.11(1) -0.052(6) 0.040(8) -0.044(7) C C20 0.069(7) 0.098(8) 0.13(1) -0.056(6) 0.040(8) -0.042(8) C C21 0.045(6) 0.100(6) 0.145(8) -0.029(4) -0.011(5) -0.079(4) C C22 0.033(5) 0.053(5) 0.071(6) -0.010(4) -0.004(4) -0.035(4) C N4 0.034(4) 0.044(3) 0.046(4) -0.014(3) -0.000(3) -0.024(3) N C23 0.054(6) 0.045(5) 0.058(5) 0.007(4) -0.026(4) -0.032(3) C C24 0.083(8) 0.070(6) 0.081(6) 0.006(5) -0.039(5) -0.052(4) C C25 0.13(1) 0.078(7) 0.067(5) 0.030(8) -0.047(6) -0.053(4) C C26 0.12(1) 0.055(6) 0.035(5) 0.010(8) -0.011(7) -0.025(4) C C27 0.084(9) 0.034(5) 0.040(5) 0.008(6) 0.002(6) -0.018(4) C N5 0.050(5) 0.032(3) 0.032(3) -0.002(3) -0.003(3) -0.019(2) N N6 0.030(4) 0.031(3) 0.029(3) -0.005(3) -0.000(3) -0.017(2) N C28 0.034(5) 0.041(4) 0.032(4) -0.011(4) 0.003(4) -0.016(3) C C29 0.028(5) 0.039(4) 0.038(4) -0.004(4) 0.003(4) -0.023(3) C C30 0.030(5) 0.037(4) 0.038(4) -0.004(3) -0.001(4) -0.022(3) C C31 0.049(6) 0.032(4) 0.038(5) -0.006(4) 0.008(4) -0.015(3) C C32 0.034(5) 0.046(5) 0.035(4) -0.004(4) 0.008(4) -0.020(3) C C33 0.037(5) 0.036(4) 0.030(4) 0.000(4) -0.002(4) -0.016(3) C C34 0.045(6) 0.032(4) 0.044(5) 0.000(4) 0.003(5) -0.019(3) C C35 0.061(7) 0.049(5) 0.043(5) -0.015(5) -0.004(5) -0.020(4) C N7 0.068(6) 0.032(4) 0.034(4) 0.002(4) -0.000(4) -0.019(3) N C36 0.050(7) 0.039(5) 0.036(5) 0.007(5) -0.001(5) -0.015(4) C C37 0.044(6) 0.040(4) 0.044(5) -0.003(4) -0.004(4) -0.023(3) C C38 0.09(1) 0.050(5) 0.060(6) -0.005(6) 0.013(6) -0.035(4) C RU2 0.0345(4) 0.0334(3) 0.0267(3) -0.0119(3) 0.0016(3) -0.0143(2) Ru N8 0.048(4) 0.044(4) 0.023(3) -0.025(3) 0.003(3) -0.010(3) N C39 0.045(5) 0.067(5) 0.038(5) -0.027(4) 0.006(4) -0.021(4) C C40 0.067(7) 0.085(8) 0.062(8) -0.043(6) 0.019(6) -0.017(6) C C41 0.064(6) 0.106(7) 0.057(7) -0.062(5) 0.019(6) -0.022(6) C C42 0.077(7) 0.060(6) 0.034(5) -0.041(4) -0.000(5) -0.006(4) C C43 0.110(8) 0.082(7) 0.060(8) -0.071(5) -0.010(6) -0.001(6) C C44 0.115(8) 0.045(5) 0.058(7) -0.047(4) -0.009(6) -0.011(4) C C45 0.112(9) 0.048(5) 0.035(5) -0.036(5) -0.013(5) -0.012(4) C C46 0.11(1) 0.043(5) 0.045(5) -0.018(5) -0.016(6) -0.020(4) C C47 0.083(8) 0.033(5) 0.043(5) 0.003(5) -0.016(5) -0.018(3) C C48 0.066(7) 0.043(5) 0.034(4) -0.017(4) -0.007(4) -0.017(3) C N9 0.052(5) 0.031(3) 0.028(3) -0.010(3) -0.004(3) -0.014(2) N C49 0.070(6) 0.039(4) 0.023(4) -0.027(4) -0.008(4) -0.007(3) C C50 0.068(6) 0.048(5) 0.029(5) -0.030(4) -0.005(4) -0.010(3) C N10 0.038(4) 0.028(3) 0.028(3) -0.003(3) -0.003(3) -0.013(2) N C51 0.057(6) 0.027(4) 0.038(4) -0.016(3) 0.007(4) -0.020(3) C C52 0.063(7) 0.029(4) 0.033(4) -0.006(4) -0.008(5) -0.012(3) C C53 0.073(7) 0.044(5) 0.035(5) -0.007(5) -0.015(5) -0.018(3) C C54 0.047(6) 0.038(4) 0.053(5) -0.006(4) -0.009(4) -0.027(3) C C55 0.040(5) 0.035(4) 0.039(4) -0.007(3) -0.006(4) -0.021(3) C C56 0.038(5) 0.037(4) 0.037(4) -0.003(4) -0.002(4) -0.019(3) C C57 0.041(6) 0.073(5) 0.066(6) -0.017(4) 0.003(5) -0.043(4) C C58 0.048(5) 0.089(6) 0.069(6) -0.042(4) 0.024(5) -0.047(4) C C59 0.059(6) 0.064(6) 0.045(5) -0.028(5) 0.016(5) -0.023(4) C C60 0.047(5) 0.039(4) 0.031(4) -0.017(4) 0.011(4) -0.016(3) C N11 0.031(4) 0.039(3) 0.035(3) -0.015(3) 0.008(3) -0.020(2) N C61 0.058(6) 0.039(4) 0.034(4) -0.017(4) 0.002(4) -0.018(3) C C62 0.071(7) 0.059(5) 0.032(5) -0.028(5) 0.010(5) -0.020(4) C C63 0.068(7) 0.058(6) 0.033(5) -0.017(5) -0.002(5) -0.016(4) C C64 0.053(6) 0.063(6) 0.042(5) -0.010(5) -0.008(5) -0.025(4) C C65 0.050(6) 0.055(5) 0.041(5) -0.017(4) -0.002(4) -0.026(3) C N12 0.036(4) 0.037(3) 0.031(3) -0.008(3) -0.004(3) -0.016(2) N N13 0.031(4) 0.040(4) 0.028(3) -0.011(3) 0.002(3) -0.014(3) N C66 0.029(5) 0.045(4) 0.033(4) -0.009(4) 0.003(4) -0.018(3) C C67 0.031(5) 0.048(5) 0.036(4) -0.004(4) 0.004(4) -0.020(3) C C68 0.039(5) 0.035(4) 0.026(4) -0.002(4) 0.006(4) -0.013(3) C C69 0.043(5) 0.036(4) 0.027(4) -0.016(3) 0.002(4) -0.011(3) C C70 0.038(5) 0.037(4) 0.029(4) -0.009(3) -0.002(4) -0.017(3) C C71 0.048(6) 0.039(5) 0.030(4) -0.006(4) 0.006(4) -0.017(3) C C72 0.087(9) 0.049(6) 0.043(5) 0.006(6) -0.006(6) -0.025(4) C C73 0.12(1) 0.057(6) 0.049(5) 0.016(7) -0.010(7) -0.035(4) C N14 0.088(8) 0.043(5) 0.046(4) 0.019(5) 0.002(5) -0.023(3) N C74 0.079(9) 0.043(6) 0.044(6) 0.008(6) -0.008(6) -0.013(4) C C75 0.065(8) 0.044(5) 0.038(5) 0.001(5) 0.002(5) -0.020(4) C C76 0.19(2) 0.061(7) 0.073(7) 0.02(1) 0.00(1) -0.043(5) C P1 0.056(2) 0.044(1) 0.048(1) -0.014(1) -0.005(1) -0.0252(8) P F1 0.137(6) 0.100(3) 0.073(3) -0.064(3) 0.035(4) -0.065(2) F F2 0.085(5) 0.065(4) 0.127(5) 0.009(3) -0.046(4) -0.052(3) F F3 0.085(4) 0.117(3) 0.105(4) -0.067(3) 0.029(3) -0.072(3) F F4 0.079(4) 0.081(3) 0.083(4) -0.045(3) 0.011(3) -0.044(2) F F5 0.107(6) 0.046(3) 0.089(4) 0.003(4) -0.044(4) -0.026(3) F F6 0.121(6) 0.062(3) 0.052(3) -0.033(3) 0.010(4) -0.030(2) F P2 0.047(2) 0.056(1) 0.058(1) 0.009(1) -0.011(1) -0.0367(9) P F7 0.114(6) 0.088(3) 0.120(4) 0.026(4) -0.051(4) -0.083(2) F F8 0.162(8) 0.091(4) 0.131(5) 0.077(5) -0.100(4) -0.078(3) F F9 0.067(5) 0.32(1) 0.152(6) -0.056(6) 0.050(5) -0.161(5) F F10 0.077(5) 0.049(3) 0.060(4) 0.002(3) -0.011(4) -0.019(3) F F11 0.067(4) 0.086(3) 0.097(4) -0.026(3) -0.003(3) -0.062(2) F F12 0.104(5) 0.094(4) 0.072(4) -0.053(3) 0.020(4) -0.045(3) F P3 0.061(2) 0.089(2) 0.036(1) -0.031(1) -0.003(1) -0.021(1) P F13 0.122(6) 0.083(4) 0.061(4) -0.038(4) -0.004(4) -0.032(3) F F14 0.087(6) 0.149(9) 0.077(5) -0.007(6) -0.031(5) -0.017(5) F F15 0.101(5) 0.215(8) 0.058(5) -0.096(4) 0.025(4) -0.032(5) F F16 0.281(9) 0.173(6) 0.072(4) -0.139(4) -0.030(5) -0.042(3) F F17 0.095(5) 0.264(9) 0.066(4) -0.086(5) 0.027(4) -0.078(4) F F18 0.174(9) 0.089(5) 0.090(5) 0.029(6) -0.049(5) -0.052(3) F P4 0.046(2) 0.061(1) 0.068(1) -0.009(1) 0.009(1) -0.041(1) P F19 0.160(8) 0.195(5) 0.323(6) 0.052(5) -0.138(4) -0.211(3) F F20 0.24(1) 0.065(5) 0.175(8) -0.046(5) -0.107(6) -0.007(5) F F21 0.149(9) 0.29(1) 0.242(8) -0.045(9) 0.127(6) -0.164(7) F F22 0.161(8) 0.122(5) 0.223(7) -0.034(4) -0.062(5) -0.106(3) F F23 0.16(1) 0.081(7) 0.21(1) 0.015(7) -0.082(8) -0.019(7) F F24 0.291(8) 0.266(6) 0.470(8) -0.230(5) 0.324(6) -0.307(5) F P5 0.088(3) 0.214(4) 0.431(7) -0.086(2) 0.097(4) -0.229(3) P F25 0.129(8) 0.128(7) 0.129(7) -0.041(6) 0.010(6) -0.060(5) F F26 0.21(1) 0.21(1) 0.21(1) -0.07(1) 0.02(1) -0.099(9) F F27 0.25(2) 0.25(1) 0.25(2) -0.08(1) 0.02(1) -0.11(1) F F28 0.24(2) 0.24(1) 0.24(1) -0.08(1) 0.02(1) -0.11(1) F F29 0.25(2) 0.25(2) 0.25(2) -0.08(1) 0.02(1) -0.12(1) F F30 0.121(7) 0.121(6) 0.121(6) -0.038(5) 0.010(6) -0.056(4) F P6 0.058(2) 0.129(3) 0.100(3) -0.042(2) 0.010(2) -0.037(2) P F31 0.18(1) 0.18(1) 0.18(1) -0.058(9) 0.01(1) -0.085(7) F F32 0.26(2) 0.26(2) 0.26(2) -0.08(1) 0.02(2) -0.12(1) F F33 0.20(1) 0.20(1) 0.20(1) -0.06(1) 0.02(1) -0.092(8) F F34 0.41(4) 0.41(3) 0.41(3) -0.13(3) 0.03(3) -0.19(2) F F35 0.39(3) 0.39(3) 0.39(3) -0.12(2) 0.03(3) -0.18(2) F F36 0.34(3) 0.34(2) 0.34(2) -0.11(2) 0.03(2) -0.16(2) F C77 0.08(1) 0.086(9) 0.27(2) -0.023(7) -0.01(1) -0.085(9) C C78 0.078(8) 0.043(5) 0.099(8) -0.010(5) -0.032(6) -0.027(5) C N15 0.123(9) 0.058(5) 0.058(5) -0.020(5) -0.030(6) -0.017(4) N C87 0.16(2) 0.16(2) 0.16(2) -0.05(1) 0.01(2) -0.07(1) C C88 0.15(2) 0.15(2) 0.15(2) -0.05(1) 0.01(1) -0.07(1) C N20 0.29(4) 0.29(3) 0.29(3) -0.09(2) 0.02(3) -0.14(2) N C90 0.25(4) 0.25(3) 0.25(3) -0.08(3) 0.02(3) -0.12(2) C C91 0.22(3) 0.22(2) 0.22(3) -0.07(2) 0.02(2) -0.10(2) C N21 0.25(3) 0.25(2) 0.25(2) -0.08(2) 0.02(2) -0.11(2) N O1 0.12(2) 0.12(2) 0.12(2) -0.04(1) 0.01(1) -0.06(1) O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU1 N1 2.101(9) . . ? RU1 N2 2.049(8) . . ? RU1 N3 2.072(8) . . ? RU1 N4 1.951(9) . . ? RU1 N5 2.072(9) . . ? RU1 N6 2.100(8) . . ? N1 C1 1.33(2) . . ? N1 C12 1.39(1) . . ? C1 C2 1.40(2) . . ? C2 C3 1.36(2) . . ? C3 C4 1.40(2) . . ? C4 C5 1.45(2) . . ? C4 C12 1.40(2) . . ? C5 C6 1.36(2) . . ? C6 C7 1.42(2) . . ? C7 C8 1.39(2) . . ? C7 C11 1.42(2) . . ? C8 C9 1.35(2) . . ? C9 C10 1.41(2) . . ? C10 N2 1.33(2) . . ? N2 C11 1.38(1) . . ? C11 C12 1.40(2) . . ? N3 C13 1.33(2) . . ? N3 C17 1.37(2) . . ? C13 C14 1.35(2) . . ? C14 C15 1.38(3) . . ? C15 C16 1.36(3) . . ? C16 C17 1.39(2) . . ? C17 C18 1.46(2) . . ? C18 C19 1.36(2) . . ? C18 N4 1.38(1) . . ? C19 C20 1.35(3) . . ? C20 C21 1.38(2) . . ? C21 C22 1.43(2) . . ? C22 N4 1.34(2) . . ? C22 C23 1.46(1) . . ? C23 C24 1.39(2) . . ? C23 N5 1.40(2) . . ? C24 C25 1.36(2) . . ? C25 C26 1.38(3) . . ? C26 C27 1.40(2) . . ? C27 N5 1.33(1) . . ? N6 C28 1.35(1) . . ? N6 C32 1.34(1) . . ? C28 C29 1.38(1) . . ? C29 C30 1.39(1) . . ? C30 C31 1.38(2) . . ? C30 C33 1.47(1) . . ? C31 C32 1.38(2) . . ? C33 C34 1.39(2) . . ? C33 C37 1.41(2) . . ? C34 C35 1.39(2) . . ? C35 N7 1.35(2) . . ? N7 C36 1.33(2) . . ? N7 C38 1.49(2) . . ? C36 C37 1.37(2) . . ? RU2 N8 2.117(9) . . ? RU2 N9 2.058(9) . . ? RU2 N10 2.069(8) . . ? RU2 N11 1.942(8) . . ? RU2 N12 2.081(8) . . ? RU2 N13 2.078(9) . . ? N8 C39 1.32(1) . . ? N8 C50 1.37(2) . . ? C39 C40 1.40(2) . . ? C40 C41 1.36(3) . . ? C41 C42 1.38(2) . . ? C42 C43 1.43(2) . . ? C42 C50 1.42(2) . . ? C43 C44 1.34(2) . . ? C44 C45 1.44(2) . . ? C45 C46 1.39(2) . . ? C45 C49 1.41(2) . . ? C46 C47 1.37(2) . . ? C47 C48 1.42(2) . . ? C48 N9 1.33(1) . . ? N9 C49 1.39(2) . . ? C49 C50 1.41(2) . . ? N10 C51 1.36(1) . . ? N10 C55 1.35(1) . . ? C51 C52 1.39(2) . . ? C52 C53 1.36(2) . . ? C53 C54 1.40(1) . . ? C54 C55 1.41(2) . . ? C55 C56 1.47(1) . . ? C56 C57 1.37(2) . . ? C56 N11 1.37(1) . . ? C57 C58 1.37(2) . . ? C58 C59 1.37(2) . . ? C59 C60 1.38(2) . . ? C60 N11 1.36(1) . . ? C60 C61 1.49(2) . . ? C61 C62 1.38(1) . . ? C61 N12 1.36(1) . . ? C62 C63 1.37(2) . . ? C63 C64 1.40(2) . . ? C64 C65 1.39(1) . . ? C65 N12 1.34(2) . . ? N13 C66 1.36(1) . . ? N13 C70 1.37(2) . . ? C66 C67 1.36(2) . . ? C67 C68 1.38(2) . . ? C68 C69 1.40(1) . . ? C68 C71 1.48(2) . . ? C69 C70 1.37(2) . . ? C71 C72 1.39(2) . . ? C71 C75 1.39(1) . . ? C72 C73 1.37(2) . . ? C73 N14 1.31(1) . . ? N14 C74 1.32(2) . . ? N14 C76 1.52(2) . . ? C74 C75 1.35(2) . . ? P1 F1 1.576(9) . . ? P1 F2 1.597(7) . . ? P1 F3 1.57(1) . . ? P1 F4 1.59(1) . . ? P1 F5 1.579(7) . . ? P1 F6 1.598(9) . . ? P2 F7 1.57(1) . . ? P2 F8 1.570(8) . . ? P2 F9 1.55(1) . . ? P2 F10 1.576(6) . . ? P2 F11 1.60(1) . . ? P2 F12 1.606(9) . . ? F10 F12 2.186(9) . . ? P3 F13 1.60(1) . . ? P3 F14 1.565(9) . . ? P3 F15 1.57(1) . . ? P3 F16 1.58(2) . . ? P3 F17 1.58(1) . . ? P3 F18 1.552(9) . . ? F13 F18 2.19(1) . . ? F14 F16 2.20(2) . . ? F14 F17 2.15(1) . . ? P4 F19 1.53(2) . . ? P4 F20 1.544(9) . . ? P4 F21 1.49(1) . . ? P4 F22 1.54(2) . . ? P4 F23 1.54(1) . . ? P4 F24 1.48(1) . . ? P5 F25 1.55(2) . . ? P5 F26 1.42(2) . . ? P5 F27 1.53(3) . . ? P5 F28 1.85(2) . . ? P5 F29 1.58(2) . . ? P5 F30 1.57(1) . . ? P6 F31 1.550(5) . . ? P6 F32 1.550(5) . . ? P6 F33 1.550(5) . . ? P6 F34 1.550(5) . . ? P6 F35 1.550(5) . . ? P6 F36 1.550(5) . . ? C77 C78 1.42(3) . . ? C78 N15 1.14(2) . . ? C87 C88 1.44(5) . . ? C88 N20 1.11(6) . . ? C90 C91 1.32(6) . . ? C91 N21 1.37(5) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 RU1 N2 79.5(4) . . . ? N1 RU1 N3 96.3(4) . . . ? N1 RU1 N4 172.0(3) . . . ? N1 RU1 N5 104.0(4) . . . ? N1 RU1 N6 95.9(3) . . . ? N2 RU1 N3 94.0(3) . . . ? N2 RU1 N4 93.5(4) . . . ? N2 RU1 N5 85.9(3) . . . ? N2 RU1 N6 172.9(3) . . . ? N3 RU1 N4 80.2(4) . . . ? N3 RU1 N5 159.3(4) . . . ? N3 RU1 N6 91.8(3) . . . ? N4 RU1 N5 79.2(4) . . . ? N4 RU1 N6 91.5(3) . . . ? N5 RU1 N6 90.1(3) . . . ? RU1 N1 C1 131.0(7) . . . ? RU1 N1 C12 112.4(8) . . . ? C1 N1 C12 116.5(9) . . . ? N1 C1 C2 123(1) . . . ? C1 C2 C3 120(1) . . . ? C2 C3 C4 118(1) . . . ? C3 C4 C5 123(1) . . . ? C3 C4 C12 118(1) . . . ? C5 C4 C12 118(1) . . . ? C4 C5 C6 121(1) . . . ? C5 C6 C7 120(1) . . . ? C6 C7 C8 123(1) . . . ? C6 C7 C11 118(1) . . . ? C8 C7 C11 117(1) . . . ? C7 C8 C9 120(1) . . . ? C8 C9 C10 118(1) . . . ? C9 C10 N2 123(1) . . . ? RU1 N2 C10 128.8(7) . . . ? RU1 N2 C11 114.1(7) . . . ? C10 N2 C11 116.9(9) . . . ? C7 C11 N2 122(1) . . . ? C7 C11 C12 120(1) . . . ? N2 C11 C12 116.8(9) . . . ? N1 C12 C4 122(1) . . . ? N1 C12 C11 116.9(9) . . . ? C4 C12 C11 120(1) . . . ? RU1 N3 C13 129.8(8) . . . ? RU1 N3 C17 113.0(8) . . . ? C13 N3 C17 117.2(9) . . . ? N3 C13 C14 124(1) . . . ? C13 C14 C15 119(1) . . . ? C14 C15 C16 117(1) . . . ? C15 C16 C17 121(1) . . . ? N3 C17 C16 119(1) . . . ? N3 C17 C18 115(1) . . . ? C16 C17 C18 124(1) . . . ? C17 C18 C19 126(1) . . . ? C17 C18 N4 113(1) . . . ? C19 C18 N4 119(1) . . . ? C18 C19 C20 120(1) . . . ? C19 C20 C21 121(1) . . . ? C20 C21 C22 118(1) . . . ? C21 C22 N4 119(1) . . . ? C21 C22 C23 128(1) . . . ? N4 C22 C23 112(1) . . . ? RU1 N4 C18 117.8(9) . . . ? RU1 N4 C22 120.6(7) . . . ? C18 N4 C22 121(1) . . . ? C22 C23 C24 124(1) . . . ? C22 C23 N5 114(1) . . . ? C24 C23 N5 120(1) . . . ? C23 C24 C25 120(1) . . . ? C24 C25 C26 118(1) . . . ? C25 C26 C27 119(1) . . . ? C26 C27 N5 122(1) . . . ? RU1 N5 C23 112.8(6) . . . ? RU1 N5 C27 129(1) . . . ? C23 N5 C27 117(1) . . . ? RU1 N6 C28 122.9(6) . . . ? RU1 N6 C32 121.0(7) . . . ? C28 N6 C32 116.1(8) . . . ? N6 C28 C29 123.1(8) . . . ? C28 C29 C30 119.8(9) . . . ? C29 C30 C31 117.2(9) . . . ? C29 C30 C33 121.3(9) . . . ? C31 C30 C33 121.5(8) . . . ? C30 C31 C32 119.7(9) . . . ? N6 C32 C31 124(1) . . . ? C30 C33 C34 121.1(9) . . . ? C30 C33 C37 120(1) . . . ? C34 C33 C37 118(1) . . . ? C33 C34 C35 119(1) . . . ? C34 C35 N7 121(1) . . . ? C35 N7 C36 119(1) . . . ? C35 N7 C38 119(1) . . . ? C36 N7 C38 121(1) . . . ? N7 C36 C37 122(1) . . . ? C33 C37 C36 118(1) . . . ? N8 RU2 N9 79.5(4) . . . ? N8 RU2 N10 100.8(3) . . . ? N8 RU2 N11 176.8(4) . . . ? N8 RU2 N12 100.1(3) . . . ? N8 RU2 N13 93.9(3) . . . ? N9 RU2 N10 91.9(3) . . . ? N9 RU2 N11 97.3(4) . . . ? N9 RU2 N12 90.0(3) . . . ? N9 RU2 N13 173.0(4) . . . ? N10 RU2 N11 79.4(3) . . . ? N10 RU2 N12 159.0(3) . . . ? N10 RU2 N13 91.8(3) . . . ? N11 RU2 N12 79.6(3) . . . ? N11 RU2 N13 89.3(3) . . . ? N12 RU2 N13 88.7(3) . . . ? RU2 N8 C39 129.5(9) . . . ? RU2 N8 C50 111.8(7) . . . ? C39 N8 C50 118(1) . . . ? N8 C39 C40 123(1) . . . ? C39 C40 C41 117(1) . . . ? C40 C41 C42 121(1) . . . ? C41 C42 C43 125(1) . . . ? C41 C42 C50 117(1) . . . ? C43 C42 C50 117(1) . . . ? C42 C43 C44 121(1) . . . ? C43 C44 C45 121(1) . . . ? C44 C45 C46 125(1) . . . ? C44 C45 C49 116(1) . . . ? C46 C45 C49 117(1) . . . ? C45 C46 C47 120(1) . . . ? C46 C47 C48 119(1) . . . ? C47 C48 N9 121(1) . . . ? RU2 N9 C48 128.0(9) . . . ? RU2 N9 C49 113.5(6) . . . ? C48 N9 C49 118(1) . . . ? C45 C49 N9 122(1) . . . ? C45 C49 C50 120(1) . . . ? N9 C49 C50 116(1) . . . ? N8 C50 C42 121(1) . . . ? N8 C50 C49 117(1) . . . ? C42 C50 C49 120(1) . . . ? RU2 N10 C51 128.2(8) . . . ? RU2 N10 C55 112.7(6) . . . ? C51 N10 C55 119.0(9) . . . ? N10 C51 C52 122(1) . . . ? C51 C52 C53 118(1) . . . ? C52 C53 C54 120(1) . . . ? C53 C54 C55 118(1) . . . ? N10 C55 C54 121.0(9) . . . ? N10 C55 C56 117.0(9) . . . ? C54 C55 C56 121(1) . . . ? C55 C56 C57 129(1) . . . ? C55 C56 N11 110.2(9) . . . ? C57 C56 N11 120.0(9) . . . ? C56 C57 C58 119(1) . . . ? C57 C58 C59 121(1) . . . ? C58 C59 C60 118(1) . . . ? C59 C60 N11 120(1) . . . ? C59 C60 C61 127.4(9) . . . ? N11 C60 C61 111.8(9) . . . ? RU2 N11 C56 120.3(6) . . . ? RU2 N11 C60 119.8(7) . . . ? C56 N11 C60 119.9(9) . . . ? C60 C61 C62 123(1) . . . ? C60 C61 N12 115.2(8) . . . ? C62 C61 N12 121(1) . . . ? C61 C62 C63 119(1) . . . ? C62 C63 C64 119(1) . . . ? C63 C64 C65 118(1) . . . ? C64 C65 N12 122(1) . . . ? RU2 N12 C61 113.2(7) . . . ? RU2 N12 C65 128.0(7) . . . ? C61 N12 C65 118.8(8) . . . ? RU2 N13 C66 121.9(9) . . . ? RU2 N13 C70 123.7(5) . . . ? C66 N13 C70 114.3(9) . . . ? N13 C66 C67 125(1) . . . ? C66 C67 C68 119.4(9) . . . ? C67 C68 C69 117(1) . . . ? C67 C68 C71 121.5(9) . . . ? C69 C68 C71 120(1) . . . ? C68 C69 C70 119(1) . . . ? N13 C70 C69 124.0(8) . . . ? C68 C71 C72 120.4(8) . . . ? C68 C71 C75 122(1) . . . ? C72 C71 C75 117(1) . . . ? C71 C72 C73 119(1) . . . ? C72 C73 N14 121(1) . . . ? C73 N14 C74 120(1) . . . ? C73 N14 C76 121(1) . . . ? C74 N14 C76 117(1) . . . ? N14 C74 C75 121(1) . . . ? C71 C75 C74 119(1) . . . ? F1 P1 F2 90.8(5) . . . ? F1 P1 F3 91.6(5) . . . ? F1 P1 F4 88.4(5) . . . ? F1 P1 F5 89.5(4) . . . ? F1 P1 F6 178.8(5) . . . ? F2 P1 F3 91.4(5) . . . ? F2 P1 F4 89.3(4) . . . ? F2 P1 F5 179.0(5) . . . ? F2 P1 F6 90.3(4) . . . ? F3 P1 F4 179.3(4) . . . ? F3 P1 F5 89.6(5) . . . ? F3 P1 F6 89.0(5) . . . ? F4 P1 F5 89.7(5) . . . ? F4 P1 F6 90.9(5) . . . ? F5 P1 F6 89.5(4) . . . ? F7 P2 F8 90.5(5) . . . ? F7 P2 F9 89.8(7) . . . ? F7 P2 F10 88.8(5) . . . ? F7 P2 F11 178.4(5) . . . ? F7 P2 F12 90.6(6) . . . ? F8 P2 F9 92.8(5) . . . ? F8 P2 F10 175.9(6) . . . ? F8 P2 F11 89.9(5) . . . ? F8 P2 F12 89.2(5) . . . ? F9 P2 F10 91.2(5) . . . ? F9 P2 F11 91.7(7) . . . ? F9 P2 F12 177.9(5) . . . ? F10 P2 F11 90.8(5) . . . ? F10 P2 F12 86.8(4) . . . ? F11 P2 F12 87.8(5) . . . ? F13 P3 F14 91.3(7) . . . ? F13 P3 F15 88.2(7) . . . ? F13 P3 F16 179.5(6) . . . ? F13 P3 F17 88.8(7) . . . ? F13 P3 F18 87.9(6) . . . ? F14 P3 F15 92.0(5) . . . ? F14 P3 F16 88.8(7) . . . ? F14 P3 F17 86.2(5) . . . ? F14 P3 F18 177.9(7) . . . ? F15 P3 F16 92.3(7) . . . ? F15 P3 F17 176.4(8) . . . ? F15 P3 F18 90.0(5) . . . ? F16 P3 F17 90.7(7) . . . ? F16 P3 F18 92.0(6) . . . ? F17 P3 F18 91.8(5) . . . ? F19 P4 F20 87.7(7) . . . ? F19 P4 F21 94.5(9) . . . ? F19 P4 F22 178.5(5) . . . ? F19 P4 F23 96.8(8) . . . ? F19 P4 F24 89.8(8) . . . ? F20 P4 F21 85.0(7) . . . ? F20 P4 F22 90.9(7) . . . ? F20 P4 F23 175(1) . . . ? F20 P4 F24 93.6(6) . . . ? F21 P4 F22 84.7(9) . . . ? F21 P4 F23 94.6(8) . . . ? F21 P4 F24 175(1) . . . ? F22 P4 F23 84.6(8) . . . ? F22 P4 F24 91.0(8) . . . ? F23 P4 F24 86.4(7) . . . ? F25 P5 F26 95(1) . . . ? F25 P5 F27 174.1(9) . . . ? F25 P5 F28 86(1) . . . ? F25 P5 F29 90(1) . . . ? F25 P5 F30 89.4(8) . . . ? F26 P5 F27 89(1) . . . ? F26 P5 F28 175(1) . . . ? F26 P5 F29 98(1) . . . ? F26 P5 F30 90.0(8) . . . ? F27 P5 F28 87(1) . . . ? F27 P5 F29 88(1) . . . ? F27 P5 F30 91(1) . . . ? F28 P5 F29 84.8(9) . . . ? F28 P5 F30 86.6(8) . . . ? F29 P5 F30 171(1) . . . ? F31 P6 F32 90.0(3) . . . ? F31 P6 F33 180.00 . . . ? F31 P6 F34 90.0(2) . . . ? F31 P6 F35 90.0(3) . . . ? F31 P6 F36 90.0(2) . . . ? F32 P6 F33 90.0(2) . . . ? F32 P6 F34 180.00 . . . ? F32 P6 F35 90.0(3) . . . ? F32 P6 F36 90.0(2) . . . ? F33 P6 F34 90.0(3) . . . ? F33 P6 F35 90.0(2) . . . ? F33 P6 F36 90.0(3) . . . ? F34 P6 F35 90.0(2) . . . ? F34 P6 F36 90.0(3) . . . ? F35 P6 F36 180.00 . . . ? C77 C78 N15 174(1) . . . ? C87 C88 N20 164(2) . . . ? C90 C91 N21 158(4) . . . ? #===END data_Complex_10 _database_code_depnum_ccdc_archive 'CCDC 218280' _audit_creation_date 17-10-03 # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(terpy*)(phen)(LU)][PF6]2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C55 H64 F12 N6 O2 P2 Ru' _chemical_formula_weight 1232.16 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1 #========================================================================== #==== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 23.7601(2) _cell_length_b 13.1662(1) _cell_length_c 37.2176(4) _cell_angle_alpha 90 _cell_angle_beta 97.638(5) _cell_angle_gamma 90 _cell_volume 11539.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173 _cell_measurement_reflns_used 15413 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 29.1 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.42 _exptl_crystal_density_method none _exptl_crystal_F_000 5072 _exptl_absorpt_coefficient_mu 0.411 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.952 _exptl_absorpt_correction_T_max 0.984 #========================================================================== #==== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 15413 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 45. mm. Scan angle = 0.6 deg 1 scans of 120 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 10.80 Omega = 0.00 Kappa = 0.00 226 frames Set 2 Theta = -9.90 Kappa = -74.00 Phi = 0.00 89 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15413 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 29.12 _reflns_number_total 15413 _reflns_number_gt 9565 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #========================================================================== #==== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 9565 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.112 _refine_ls_R_factor_gt 0.066 _refine_ls_wR_factor_all 0.221 _refine_ls_wR_factor_ref 0.079 _refine_ls_goodness_of_fit_all 1.296 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_shift/su_max 0.002 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.936 _refine_diff_density_min -0.876 #========================================================================== #==== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RU 0.63760(2) 0.21468(3) 0.61669(1) 0.0258(1) Uani ? ? Ru N2 0.7140(2) 0.2659(3) 0.6036(1) 0.032(2) Uani ? ? N C1 0.7446(2) 0.3455(4) 0.6176(2) 0.042(3) Uani ? ? C C2 0.7948(3) 0.3759(5) 0.6051(2) 0.053(3) Uani ? ? C C3 0.8150(3) 0.3231(5) 0.5781(2) 0.056(4) Uani ? ? C C4 0.7839(2) 0.2402(5) 0.5620(2) 0.046(3) Uani ? ? C C5 0.8011(3) 0.1794(6) 0.5338(2) 0.061(4) Uani ? ? C C6 0.7693(3) 0.1009(5) 0.5194(2) 0.060(3) Uani ? ? C C7 0.7168(2) 0.0754(4) 0.5320(1) 0.044(3) Uani ? ? C C8 0.6823(3) -0.0063(5) 0.5186(2) 0.049(3) Uani ? ? C C9 0.6329(3) -0.0246(4) 0.5326(2) 0.044(3) Uani ? ? C C10 0.6179(2) 0.0377(4) 0.5600(1) 0.036(3) Uani ? ? C N1 0.6488(2) 0.1165(3) 0.5736(1) 0.030(2) Uani ? ? N C11 0.6984(2) 0.1336(4) 0.5597(1) 0.033(2) Uani ? ? C C12 0.7333(2) 0.2158(4) 0.5753(1) 0.035(2) Uani ? ? C N3 0.5991(2) 0.3419(3) 0.5916(1) 0.029(2) Uani ? ? N C13 0.5814(2) 0.3562(4) 0.5562(1) 0.037(3) Uani ? ? C C14 0.5546(3) 0.4441(5) 0.5428(2) 0.046(3) Uani ? ? C C15 0.5456(3) 0.5204(4) 0.5668(2) 0.047(3) Uani ? ? C C16 0.5647(2) 0.5087(4) 0.6033(2) 0.040(3) Uani ? ? C C17 0.5911(2) 0.4190(4) 0.6154(1) 0.030(2) Uani ? ? C C18 0.6120(2) 0.3975(4) 0.6537(1) 0.030(2) Uani ? ? C C19 0.6088(2) 0.4606(4) 0.6833(1) 0.032(2) Uani ? ? C C20 0.6298(2) 0.4280(4) 0.7183(1) 0.031(2) Uani ? ? C C21 0.6549(2) 0.3318(4) 0.7220(1) 0.033(2) Uani ? ? C C22 0.6577(2) 0.2712(4) 0.6918(1) 0.031(2) Uani ? ? C N4 0.6362(2) 0.3049(3) 0.6586(1) 0.028(2) Uani ? ? N C23 0.6821(2) 0.1679(4) 0.6913(1) 0.032(2) Uani ? ? C C24 0.7083(2) 0.1183(4) 0.7217(1) 0.040(3) Uani ? ? C C25 0.7299(2) 0.0219(4) 0.7186(2) 0.042(3) Uani ? ? C C26 0.7257(2) -0.0227(4) 0.6850(2) 0.039(3) Uani ? ? C C27 0.6991(2) 0.0292(4) 0.6553(1) 0.034(2) Uani ? ? C N5 0.6772(2) 0.1231(3) 0.6576(1) 0.030(2) Uani ? ? N C28 0.6249(2) 0.4935(4) 0.7502(1) 0.033(2) Uani ? ? C C29 0.6263(2) 0.5989(4) 0.7468(1) 0.035(2) Uani ? ? C C30 0.6219(2) 0.6619(4) 0.7763(1) 0.036(3) Uani ? ? C C31 0.6149(2) 0.6163(4) 0.8091(1) 0.045(3) Uani ? ? C C32 0.6122(2) 0.5116(4) 0.8135(1) 0.042(3) Uani ? ? C C33 0.6179(2) 0.4507(4) 0.7836(1) 0.038(3) Uani ? ? C C34 0.6241(3) 0.7773(4) 0.7730(2) 0.049(3) Uani ? ? C C35 0.6091(6) 0.8337(7) 0.8030(3) 0.120(7) Uani ? ? C C36 0.6207(8) 0.8166(7) 0.7376(3) 0.105(8) Uani ? ? C C37 0.6917(6) 0.8047(8) 0.7820(5) 0.14(1) Uani ? ? C C38 0.6026(3) 0.4654(5) 0.8501(2) 0.057(3) Uani ? ? C C39 0.5861(4) 0.5395(7) 0.8760(2) 0.097(5) Uani ? ? C C40 0.5477(5) 0.3975(9) 0.8430(3) 0.154(7) Uani ? ? C C41 0.6472(5) 0.399(1) 0.8643(2) 0.225(7) Uani ? ? C N6 0.5554(2) 0.1628(3) 0.6237(1) 0.030(2) Uani ? ? N C42 0.5403(2) 0.1450(4) 0.6566(1) 0.037(3) Uani ? ? C C43 0.4854(2) 0.1212(4) 0.6624(2) 0.044(3) Uani ? ? C C44 0.4451(2) 0.1130(5) 0.6327(2) 0.047(3) Uani ? ? C C45 0.4587(2) 0.1302(4) 0.5980(2) 0.041(3) Uani ? ? C C46 0.5143(2) 0.1558(4) 0.5951(1) 0.036(3) Uani ? ? C C47 0.4722(3) 0.1059(6) 0.7008(2) 0.071(4) Uani ? ? C C48 0.4161(3) 0.1206(6) 0.5648(2) 0.062(4) Uani ? ? C P1 0.76554(7) 0.6363(1) 0.66936(4) 0.0458(8) Uani ? ? P F1 0.7225(2) 0.6655(5) 0.6964(1) 0.098(3) Uani ? ? F F2 0.8081(2) 0.6125(5) 0.6419(1) 0.105(3) Uani ? ? F F3 0.8150(2) 0.6921(4) 0.6953(1) 0.082(3) Uani ? ? F F4 0.7497(2) 0.7389(3) 0.6481(1) 0.079(3) Uani ? ? F F5 0.7164(2) 0.5800(3) 0.6437(1) 0.066(2) Uani ? ? F F6 0.7780(3) 0.5364(4) 0.6913(2) 0.123(4) Uani ? ? F P2 0.52439(6) 0.1896(1) 0.46583(4) 0.0396(7) Uani ? ? P F7 0.5852(2) 0.1651(5) 0.4845(2) 0.116(4) Uani ? ? F F8 0.4639(2) 0.2169(5) 0.4478(2) 0.123(5) Uani ? ? F F9 0.5056(3) 0.1850(9) 0.5021(2) 0.164(5) Uani ? ? F F10 0.5449(3) 0.3019(4) 0.4721(2) 0.120(4) Uani ? ? F F11 0.5435(3) 0.2018(8) 0.4295(2) 0.172(6) Uani ? ? F F12 0.5054(3) 0.0805(4) 0.4578(2) 0.137(5) Uani ? ? F C49 0.7475(5) 0.741(1) 0.5571(3) 0.122(8) Uani ? ? C C50 0.7223(6) 0.6442(9) 0.5550(2) 0.104(8) Uani ? ? C O1 0.6950(3) 0.6112(5) 0.5206(2) 0.108(4) Uani ? ? O C51 0.6423(4) 0.6584(8) 0.5090(3) 0.106(6) Uani ? ? C C52 0.6158(5) 0.6093(9) 0.4734(3) 0.121(8) Uani ? ? C C53 0.4386(3) 0.2232(5) 0.3551(2) 0.054(4) Uani ? ? C O2 0.4563(2) 0.2996(3) 0.3427(1) 0.069(3) Uani ? ? O C54 0.4668(4) 0.1231(6) 0.3536(2) 0.084(5) Uani ? ? C C55 0.3859(4) 0.2233(6) 0.3724(3) 0.080(5) Uani ? ? C H1 0.7315 0.3826 0.6368 0.0553 Uiso calc C1 H H2 0.8149 0.4335 0.6154 0.0701 Uiso calc C2 H H3 0.8498 0.3422 0.5701 0.0750 Uiso calc C3 H H4 0.8358 0.1945 0.5248 0.0775 Uiso calc C5 H H5 0.7820 0.0618 0.5006 0.0756 Uiso calc C6 H H6 0.6931 -0.0484 0.4999 0.0632 Uiso calc C8 H H7 0.6091 -0.0794 0.5238 0.0583 Uiso calc C9 H H8 0.5836 0.0231 0.5696 0.0468 Uiso calc C10 H H9 0.5875 0.3037 0.5396 0.0481 Uiso calc C13 H H10 0.5427 0.4518 0.5176 0.0621 Uiso calc C14 H H11 0.5264 0.5808 0.5583 0.0624 Uiso calc C15 H H12 0.5597 0.5618 0.6199 0.0531 Uiso calc C16 H H13 0.5923 0.5262 0.6797 0.0417 Uiso calc C19 H H14 0.6702 0.3079 0.7454 0.0437 Uiso calc C21 H H15 0.7114 0.1505 0.7447 0.0528 Uiso calc C24 H H16 0.7474 -0.0131 0.7395 0.0561 Uiso calc C25 H H17 0.7410 -0.0885 0.6822 0.0521 Uiso calc C26 H H18 0.6959 -0.0027 0.6323 0.0444 Uiso calc C27 H H19 0.6303 0.6282 0.7239 0.0448 Uiso calc C29 H H20 0.6118 0.6586 0.8294 0.0573 Uiso calc C31 H H21 0.6170 0.3788 0.7859 0.0488 Uiso calc C33 H H22 0.6119 0.9043 0.7982 0.2048 Uiso calc C35 H H23 0.5713 0.8177 0.8065 0.2048 Uiso calc C35 H H24 0.6342 0.8168 0.8242 0.2048 Uiso calc C35 H H25 0.6225 0.8886 0.7385 0.2321 Uiso calc C36 H H26 0.6515 0.7914 0.7263 0.2321 Uiso calc C36 H H27 0.5859 0.7962 0.7239 0.2321 Uiso calc C36 H H28 0.6968 0.8761 0.7805 0.2154 Uiso calc C37 H H29 0.7057 0.7822 0.8057 0.2154 Uiso calc C37 H H30 0.7120 0.7718 0.7649 0.2154 Uiso calc C37 H H31 0.5809 0.5059 0.8979 0.1314 Uiso calc C39 H H32 0.6151 0.5892 0.8808 0.1314 Uiso calc C39 H H33 0.5517 0.5715 0.8661 0.1314 Uiso calc C39 H H34 0.5404 0.3675 0.8651 0.2049 Uiso calc C40 H H35 0.5162 0.4384 0.8335 0.2049 Uiso calc C40 H H36 0.5532 0.3456 0.8260 0.2049 Uiso calc C40 H H37 0.6394 0.3727 0.8868 0.3204 Uiso calc C41 H H38 0.6501 0.3453 0.8477 0.3204 Uiso calc C41 H H39 0.6819 0.4361 0.8678 0.3204 Uiso calc C41 H H40 0.5688 0.1488 0.6770 0.0479 Uiso calc C42 H H41 0.4073 0.0952 0.6357 0.0608 Uiso calc C44 H H42 0.5242 0.1693 0.5716 0.0467 Uiso calc C46 H H43 0.4331 0.0902 0.7003 0.0901 Uiso calc C47 H H44 0.4945 0.0516 0.7119 0.0901 Uiso calc C47 H H45 0.4808 0.1663 0.7144 0.0901 Uiso calc C47 H H46 0.3802 0.1027 0.5716 0.0847 Uiso calc C48 H H47 0.4129 0.1836 0.5522 0.0847 Uiso calc C48 H H48 0.4280 0.0695 0.5494 0.0847 Uiso calc C48 H H49 0.7642 0.7542 0.5813 0.1711 Uiso calc C49 H H50 0.7759 0.7444 0.5414 0.1711 Uiso calc C49 H H51 0.7193 0.7913 0.5499 0.1711 Uiso calc C49 H H52 0.6947 0.6433 0.5713 0.1753 Uiso calc C50 H H53 0.7514 0.5964 0.5627 0.1753 Uiso calc C50 H H54 0.6480 0.7288 0.5053 0.1346 Uiso calc C51 H H55 0.6177 0.6497 0.5269 0.1346 Uiso calc C51 H H56 0.5803 0.6406 0.4654 0.1582 Uiso calc C52 H H57 0.6405 0.6179 0.4556 0.1582 Uiso calc C52 H H58 0.6102 0.5389 0.4772 0.1582 Uiso calc C52 H H59 0.4461 0.0733 0.3649 0.1189 Uiso calc C54 H H60 0.4679 0.1048 0.3290 0.1189 Uiso calc C54 H H61 0.5044 0.1271 0.3659 0.1189 Uiso calc C54 H H62 0.3787 0.1566 0.3805 0.1078 Uiso calc C55 H H63 0.3901 0.2685 0.3925 0.1078 Uiso calc C55 H H64 0.3549 0.2447 0.3553 0.1078 Uiso calc C55 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RU 0.0260(2) 0.0257(1) 0.0258(1) 0.0011(2) 0.0027(1) -0.0019(2) Ru N2 0.031(2) 0.030(2) 0.034(2) -0.000(2) 0.003(2) 0.001(2) N C1 0.039(3) 0.040(3) 0.047(3) -0.005(2) 0.002(2) -0.004(3) C C2 0.043(3) 0.049(3) 0.070(4) -0.016(3) 0.007(3) -0.009(3) C C3 0.037(3) 0.060(4) 0.079(4) -0.009(3) 0.019(3) -0.002(3) C C4 0.037(3) 0.050(3) 0.054(3) 0.000(3) 0.017(2) -0.001(3) C C5 0.047(3) 0.067(4) 0.071(4) -0.002(3) 0.032(3) -0.007(3) C C6 0.053(3) 0.066(4) 0.061(3) 0.005(3) 0.027(3) -0.012(3) C C7 0.043(3) 0.047(3) 0.043(3) 0.005(3) 0.015(2) -0.009(2) C C8 0.056(3) 0.047(3) 0.044(3) 0.004(3) 0.010(3) -0.017(3) C C9 0.052(3) 0.039(3) 0.043(3) -0.002(3) 0.004(3) -0.015(2) C C10 0.033(2) 0.036(3) 0.038(3) -0.000(2) 0.003(2) -0.005(2) C N1 0.029(2) 0.032(2) 0.030(2) 0.004(2) 0.003(2) -0.000(2) N C11 0.033(2) 0.034(2) 0.032(2) 0.005(2) 0.004(2) -0.002(2) C C12 0.031(2) 0.038(2) 0.034(2) 0.002(2) 0.006(2) -0.002(2) C N3 0.029(2) 0.028(2) 0.029(2) 0.001(2) 0.003(2) -0.001(2) N C13 0.039(3) 0.040(3) 0.032(2) 0.001(2) 0.003(2) 0.000(2) C C14 0.058(3) 0.047(3) 0.036(3) 0.006(3) -0.004(3) 0.008(3) C C15 0.056(3) 0.038(3) 0.048(3) 0.010(3) -0.002(3) 0.011(3) C C16 0.045(3) 0.033(3) 0.045(3) 0.004(2) 0.007(2) 0.003(2) C C17 0.025(2) 0.029(2) 0.036(2) 0.002(2) 0.006(2) 0.004(2) C C18 0.027(2) 0.028(2) 0.035(2) -0.001(2) 0.006(2) -0.000(2) C C19 0.031(2) 0.028(2) 0.038(2) 0.000(2) 0.010(2) -0.002(2) C C20 0.030(2) 0.032(2) 0.032(2) -0.004(2) 0.008(2) -0.005(2) C C21 0.039(3) 0.031(2) 0.030(2) -0.003(2) 0.003(2) 0.000(2) C C22 0.032(2) 0.030(2) 0.029(2) 0.005(2) 0.002(2) -0.001(2) C N4 0.029(2) 0.025(2) 0.030(2) -0.000(2) 0.004(2) -0.004(2) N C23 0.038(3) 0.030(2) 0.030(2) 0.000(2) -0.000(2) -0.003(2) C C24 0.047(3) 0.041(3) 0.033(2) 0.005(2) -0.000(2) 0.001(2) C C25 0.047(3) 0.036(3) 0.044(3) 0.008(2) -0.006(2) 0.005(2) C C26 0.038(3) 0.031(2) 0.050(3) 0.007(2) 0.004(2) 0.000(2) C C27 0.035(3) 0.029(2) 0.038(2) 0.004(2) 0.004(2) -0.003(2) C N5 0.031(2) 0.027(2) 0.031(2) 0.003(2) 0.002(2) 0.001(2) N C28 0.030(2) 0.035(2) 0.035(2) -0.003(2) 0.009(2) -0.005(2) C C29 0.037(3) 0.033(2) 0.036(2) 0.000(2) 0.010(2) -0.004(2) C C30 0.039(3) 0.030(2) 0.041(3) -0.001(2) 0.011(2) -0.006(2) C C31 0.049(3) 0.046(3) 0.040(3) 0.005(3) 0.012(2) -0.011(2) C C32 0.043(3) 0.040(3) 0.042(3) 0.002(2) 0.016(2) -0.003(2) C C33 0.040(3) 0.033(2) 0.042(3) -0.005(2) 0.013(2) -0.003(2) C C34 0.087(4) 0.031(3) 0.043(3) 0.009(3) 0.013(3) -0.006(3) C C35 0.32(1) 0.040(4) 0.136(6) -0.006(7) 0.126(6) -0.020(5) C C36 0.43(2) 0.036(4) 0.076(6) -0.030(8) 0.052(9) -0.005(4) C C37 0.15(1) 0.072(6) 0.27(2) -0.032(7) 0.04(1) -0.020(9) C C38 0.077(4) 0.054(4) 0.045(3) 0.012(3) 0.032(2) 0.006(3) C C39 0.168(7) 0.090(6) 0.060(3) 0.025(5) 0.069(3) 0.009(4) C C40 0.243(9) 0.149(8) 0.100(5) -0.104(6) 0.094(5) -0.016(6) C C41 0.249(7) 0.41(1) 0.112(4) 0.258(6) 0.136(4) 0.178(5) C N6 0.030(2) 0.026(2) 0.034(2) 0.002(2) 0.009(2) -0.001(2) N C42 0.043(3) 0.028(2) 0.041(3) -0.001(2) 0.009(2) -0.002(2) C C43 0.046(3) 0.034(3) 0.055(3) -0.004(2) 0.020(2) -0.001(2) C C44 0.035(3) 0.048(3) 0.061(3) -0.003(3) 0.018(2) -0.007(3) C C45 0.029(3) 0.041(3) 0.057(3) 0.003(2) 0.004(2) -0.003(3) C C46 0.036(3) 0.034(3) 0.037(2) 0.003(2) 0.006(2) 0.000(2) C C47 0.074(4) 0.081(5) 0.060(3) -0.015(4) 0.034(3) 0.001(4) C C48 0.042(3) 0.077(5) 0.073(4) 0.003(3) -0.005(3) -0.006(4) C P1 0.0468(8) 0.0543(9) 0.0378(7) -0.0039(7) 0.0094(6) -0.0052(7) P F1 0.082(3) 0.160(5) 0.071(2) -0.014(3) 0.043(2) -0.025(3) F F2 0.059(2) 0.187(5) 0.104(3) 0.003(3) 0.033(2) -0.067(3) F F3 0.073(3) 0.128(4) 0.058(2) -0.034(3) -0.001(2) -0.018(2) F F4 0.091(3) 0.061(2) 0.089(3) -0.014(2) -0.003(3) 0.008(2) F F5 0.068(2) 0.065(2) 0.065(2) -0.018(2) 0.001(2) -0.009(2) F F6 0.173(5) 0.084(3) 0.129(4) -0.002(4) -0.055(4) 0.040(3) F P2 0.0334(7) 0.0426(7) 0.0434(7) 0.0004(6) 0.0035(6) -0.0006(6) P F7 0.050(3) 0.150(4) 0.209(6) 0.010(3) -0.008(3) 0.084(4) F F8 0.057(3) 0.173(6) 0.189(6) 0.025(3) -0.032(3) 0.014(5) F F9 0.122(4) 0.51(1) 0.070(3) -0.133(5) 0.050(2) -0.079(5) F F10 0.166(5) 0.061(3) 0.172(6) -0.014(3) -0.053(4) 0.009(3) F F11 0.157(4) 0.45(1) 0.073(3) -0.150(5) 0.041(3) -0.027(5) F F12 0.182(6) 0.065(3) 0.216(7) -0.026(4) -0.015(6) -0.024(4) F C49 0.14(1) 0.18(1) 0.073(6) 0.003(9) -0.003(6) 0.033(7) C C50 0.24(1) 0.117(8) 0.040(4) -0.007(9) -0.001(6) -0.013(5) C O1 0.141(5) 0.115(5) 0.078(4) 0.027(4) 0.023(4) -0.013(4) O C51 0.101(6) 0.098(7) 0.121(7) 0.019(5) 0.045(5) 0.002(6) C C52 0.111(8) 0.130(9) 0.122(8) -0.014(7) 0.011(7) -0.017(7) C C53 0.089(5) 0.041(3) 0.044(3) 0.004(3) -0.007(3) -0.007(3) C O2 0.115(4) 0.040(2) 0.072(3) 0.003(3) 0.022(3) -0.003(2) O C54 0.152(7) 0.053(4) 0.074(5) 0.028(5) 0.031(5) 0.001(4) C C55 0.069(5) 0.073(5) 0.101(6) -0.003(4) -0.010(5) 0.000(5) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU N2 2.056(4) . . ? RU N1 2.106(4) . . ? RU N3 2.070(4) . . ? RU N4 1.963(4) . . ? RU N5 2.068(4) . . ? RU N6 2.118(4) . . ? N2 C1 1.340(7) . . ? N2 C12 1.370(6) . . ? C1 C2 1.397(8) . . ? C2 C3 1.361(9) . . ? C3 C4 1.405(9) . . ? C4 C5 1.421(9) . . ? C4 C12 1.400(7) . . ? C5 C6 1.35(1) . . ? C6 C7 1.431(8) . . ? C7 C8 1.404(8) . . ? C7 C11 1.400(7) . . ? C8 C9 1.367(8) . . ? C9 C10 1.390(7) . . ? C10 N1 1.331(6) . . ? N1 C11 1.367(6) . . ? C11 C12 1.437(7) . . ? N3 C13 1.344(6) . . ? N3 C17 1.378(6) . . ? C13 C14 1.380(8) . . ? C14 C15 1.380(9) . . ? C15 C16 1.382(8) . . ? C16 C17 1.385(7) . . ? C17 C18 1.472(7) . . ? C18 C19 1.389(7) . . ? C18 N4 1.350(6) . . ? C19 C20 1.401(7) . . ? C20 C21 1.399(7) . . ? C20 C28 1.483(7) . . ? C21 C22 1.390(7) . . ? C22 N4 1.347(6) . . ? C22 C23 1.480(7) . . ? C23 C24 1.382(7) . . ? C23 N5 1.376(6) . . ? C24 C25 1.378(8) . . ? C25 C26 1.376(8) . . ? C26 C27 1.377(7) . . ? C27 N5 1.348(6) . . ? C28 C29 1.394(7) . . ? C28 C33 1.395(7) . . ? C29 C30 1.392(7) . . ? C30 C31 1.388(8) . . ? C30 C34 1.527(8) . . ? C31 C32 1.391(8) . . ? C32 C33 1.395(7) . . ? C32 C38 1.534(8) . . ? C34 C35 1.42(1) . . ? C34 C36 1.41(1) . . ? C34 C37 1.64(2) . . ? C38 C39 1.46(1) . . ? C38 C40 1.58(1) . . ? C38 C41 1.42(1) . . ? N6 C42 1.340(6) . . ? N6 C46 1.349(6) . . ? C42 C43 1.388(8) . . ? C43 C44 1.369(9) . . ? C43 C47 1.517(9) . . ? C44 C45 1.390(8) . . ? C45 C46 1.381(7) . . ? C45 C48 1.495(9) . . ? P1 F1 1.576(4) . . ? P1 F2 1.561(4) . . ? P1 F3 1.596(4) . . ? P1 F4 1.585(5) . . ? P1 F5 1.592(4) . . ? P1 F6 1.556(5) . . ? F1 F6 2.175(9) . . ? F2 F4 2.199(7) . . ? P2 F7 1.551(5) . . ? P2 F8 1.545(5) . . ? P2 F9 1.477(6) . . ? P2 F10 1.564(5) . . ? P2 F11 1.492(6) . . ? P2 F12 1.524(6) . . ? F7 F9 2.097(9) . . ? F7 F10 2.063(8) . . ? F8 F9 2.17(1) . . ? F8 F11 2.10(1) . . ? F8 F12 2.059(9) . . ? F9 F10 2.18(1) . . ? F9 F12 2.15(1) . . ? F10 F11 2.06(1) . . ? F11 F12 2.18(1) . . ? C49 C50 1.41(2) . . ? C50 O1 1.42(1) . . ? O1 C51 1.41(1) . . ? C51 C52 1.53(2) . . ? C53 O2 1.205(8) . . ? C53 C54 1.48(1) . . ? C53 C55 1.48(1) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 RU N1 79.4(2) . . . ? N2 RU N3 88.8(2) . . . ? N2 RU N4 95.7(2) . . . ? N2 RU N5 92.1(2) . . . ? N2 RU N6 173.4(2) . . . ? N1 RU N3 104.3(2) . . . ? N1 RU N4 173.7(2) . . . ? N1 RU N5 96.4(2) . . . ? N1 RU N6 96.2(2) . . . ? N3 RU N4 79.3(2) . . . ? N3 RU N5 159.1(2) . . . ? N3 RU N6 87.6(2) . . . ? N4 RU N5 79.8(2) . . . ? N4 RU N6 89.1(2) . . . ? N5 RU N6 93.3(2) . . . ? RU N2 C1 127.8(4) . . . ? RU N2 C12 114.8(3) . . . ? C1 N2 C12 117.2(5) . . . ? N2 C1 C2 122.5(5) . . . ? C1 C2 C3 120.0(6) . . . ? C2 C3 C4 119.7(6) . . . ? C3 C4 C5 124.5(6) . . . ? C3 C4 C12 117.0(5) . . . ? C5 C4 C12 118.5(6) . . . ? C4 C5 C6 121.6(6) . . . ? C5 C6 C7 121.1(6) . . . ? C6 C7 C8 123.8(5) . . . ? C6 C7 C11 119.0(6) . . . ? C8 C7 C11 117.3(5) . . . ? C7 C8 C9 119.2(5) . . . ? C8 C9 C10 119.5(5) . . . ? C9 C10 N1 123.7(5) . . . ? RU N1 C10 130.4(3) . . . ? RU N1 C11 112.8(3) . . . ? C10 N1 C11 116.5(4) . . . ? C7 C11 N1 123.7(5) . . . ? C7 C11 C12 119.4(5) . . . ? N1 C11 C12 116.9(4) . . . ? N2 C12 C4 123.5(5) . . . ? N2 C12 C11 116.1(4) . . . ? C4 C12 C11 120.4(5) . . . ? RU N3 C13 128.2(3) . . . ? RU N3 C17 113.4(3) . . . ? C13 N3 C17 118.4(4) . . . ? N3 C13 C14 122.7(5) . . . ? C13 C14 C15 118.8(5) . . . ? C14 C15 C16 119.7(5) . . . ? C15 C16 C17 119.4(5) . . . ? N3 C17 C16 121.0(5) . . . ? N3 C17 C18 115.0(4) . . . ? C16 C17 C18 124.1(5) . . . ? C17 C18 C19 127.1(4) . . . ? C17 C18 N4 112.8(4) . . . ? C19 C18 N4 120.1(4) . . . ? C18 C19 C20 120.2(5) . . . ? C19 C20 C21 117.6(4) . . . ? C19 C20 C28 120.7(5) . . . ? C21 C20 C28 121.7(5) . . . ? C20 C21 C22 120.4(5) . . . ? C21 C22 N4 120.1(4) . . . ? C21 C22 C23 126.8(4) . . . ? N4 C22 C23 113.1(4) . . . ? RU N4 C18 119.4(3) . . . ? RU N4 C22 119.0(3) . . . ? C18 N4 C22 121.5(4) . . . ? C22 C23 C24 124.0(5) . . . ? C22 C23 N5 114.8(4) . . . ? C24 C23 N5 121.2(5) . . . ? C23 C24 C25 119.9(5) . . . ? C24 C25 C26 119.1(5) . . . ? C25 C26 C27 119.1(5) . . . ? C26 C27 N5 123.0(5) . . . ? RU N5 C23 113.3(3) . . . ? RU N5 C27 129.1(3) . . . ? C23 N5 C27 117.6(4) . . . ? C20 C28 C29 120.1(5) . . . ? C20 C28 C33 120.5(5) . . . ? C29 C28 C33 119.4(5) . . . ? C28 C29 C30 121.1(5) . . . ? C29 C30 C31 117.8(5) . . . ? C29 C30 C34 121.5(5) . . . ? C31 C30 C34 120.7(5) . . . ? C30 C31 C32 123.1(5) . . . ? C31 C32 C33 117.7(5) . . . ? C31 C32 C38 120.9(5) . . . ? C33 C32 C38 121.4(5) . . . ? C28 C33 C32 121.0(5) . . . ? C30 C34 C35 116.2(6) . . . ? C30 C34 C36 116.2(6) . . . ? C30 C34 C37 104.3(6) . . . ? C35 C34 C36 123.6(8) . . . ? C35 C34 C37 93.8(9) . . . ? C36 C34 C37 92(1) . . . ? C32 C38 C39 113.8(6) . . . ? C32 C38 C40 107.1(6) . . . ? C32 C38 C41 112.5(6) . . . ? C39 C38 C40 101.6(8) . . . ? C39 C38 C41 114(1) . . . ? C40 C38 C41 106(1) . . . ? RU N6 C42 122.1(4) . . . ? RU N6 C46 120.4(3) . . . ? C42 N6 C46 117.1(4) . . . ? N6 C42 C43 123.7(5) . . . ? C42 C43 C44 117.4(5) . . . ? C42 C43 C47 119.6(6) . . . ? C44 C43 C47 122.9(6) . . . ? C43 C44 C45 121.1(5) . . . ? C44 C45 C46 117.0(5) . . . ? C44 C45 C48 122.6(6) . . . ? C46 C45 C48 120.4(6) . . . ? N6 C46 C45 123.6(5) . . . ? F1 P1 F2 177.4(4) . . . ? F1 P1 F3 89.4(3) . . . ? F1 P1 F4 88.8(3) . . . ? F1 P1 F5 90.6(3) . . . ? F1 P1 F6 88.0(4) . . . ? F2 P1 F3 89.9(3) . . . ? F2 P1 F4 88.7(3) . . . ? F2 P1 F5 90.1(3) . . . ? F2 P1 F6 94.5(4) . . . ? F3 P1 F4 90.9(3) . . . ? F3 P1 F5 179.6(3) . . . ? F3 P1 F6 89.9(3) . . . ? F4 P1 F5 89.5(2) . . . ? F4 P1 F6 176.7(4) . . . ? F5 P1 F6 89.7(3) . . . ? P1 F1 F6 45.6(2) . . . ? P1 F2 F4 46.1(2) . . . ? P1 F4 F2 45.2(2) . . . ? P1 F6 F1 46.4(2) . . . ? F7 P2 F8 178.4(4) . . . ? F7 P2 F9 87.6(4) . . . ? F7 P2 F10 83.0(4) . . . ? F7 P2 F11 93.0(5) . . . ? F7 P2 F12 97.2(4) . . . ? F8 P2 F9 91.7(5) . . . ? F8 P2 F10 95.6(4) . . . ? F8 P2 F11 87.6(5) . . . ? F8 P2 F12 84.3(4) . . . ? F9 P2 F10 91.5(5) . . . ? F9 P2 F11 176.2(7) . . . ? F9 P2 F12 91.3(6) . . . ? F10 P2 F11 84.8(5) . . . ? F10 P2 F12 177.1(5) . . . ? F11 P2 F12 92.4(5) . . . ? P2 F7 F9 44.7(3) . . . ? P2 F7 F10 48.8(2) . . . ? F9 F7 F10 63.2(4) . . . ? P2 F8 F9 42.9(3) . . . ? P2 F8 F11 45.1(3) . . . ? P2 F8 F12 47.4(3) . . . ? F9 F8 F11 88.0(3) . . . ? F9 F8 F12 61.0(4) . . . ? F11 F8 F12 63.0(4) . . . ? P2 F9 F7 47.6(3) . . . ? P2 F9 F8 45.4(3) . . . ? P2 F9 F10 45.8(3) . . . ? P2 F9 F12 45.2(3) . . . ? F7 F9 F8 93.0(3) . . . ? F7 F9 F10 57.6(3) . . . ? F7 F9 F12 65.8(4) . . . ? F8 F9 F10 64.0(4) . . . ? F8 F9 F12 57.0(3) . . . ? F10 F9 F12 91.0(3) . . . ? P2 F10 F7 48.3(2) . . . ? P2 F10 F9 42.6(3) . . . ? P2 F10 F11 46.1(3) . . . ? F7 F10 F9 59.2(4) . . . ? F7 F10 F11 64.7(4) . . . ? F9 F10 F11 88.8(4) . . . ? P2 F11 F8 47.2(3) . . . ? P2 F11 F10 49.1(3) . . . ? P2 F11 F12 44.4(3) . . . ? F8 F11 F10 67.2(4) . . . ? F8 F11 F12 57.5(3) . . . ? F10 F11 F12 93.5(3) . . . ? P2 F12 F8 48.3(3) . . . ? P2 F12 F9 43.5(3) . . . ? P2 F12 F11 43.2(3) . . . ? F8 F12 F9 62.1(4) . . . ? F8 F12 F11 59.5(4) . . . ? F9 F12 F11 86.7(4) . . . ? C49 C50 O1 117(1) . . . ? C50 O1 C51 114.9(9) . . . ? O1 C51 C52 109.0(9) . . . ? O2 C53 C54 123.1(8) . . . ? O2 C53 C55 121.5(7) . . . ? C54 C53 C55 115.4(7) . . . ? #===END #===END data_Complex_9 _database_code_depnum_ccdc_archive 'CCDC 218935' _audit_creation_date 26-09-03 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ru(terpy*)(phen)(H2O)][PF6]2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C97 H112 F24 N10 O7 P4 Ru2' _chemical_formula_weight 2312.03 _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 ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1 #========================================================================== #==== # 6. CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 32 2 1' _symmetry_space_group_name_Hall ' P 32 2"' loop_ _symmetry_equiv_pos_as_xyz x,y,z -y,+x-y,2/3+z -x+y,-x,1/3+z +y,+x,-z +x-y,-y,1/3-z -x,-x+y,2/3-z _cell_length_a 13.5432(1) _cell_length_b 13.5432(1) _cell_length_c 50.1170(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 7960.8(1) _cell_formula_units_Z 3 _cell_measurement_temperature 173 _cell_measurement_reflns_used 21140 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 30.0 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_method none _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 0.443 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.8662 _exptl_absorpt_correction_T_max 1.0000 #========================================================================== #==== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 21140 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 67. mm. Scan angle = 0.5 deg 1 scans of 40 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = -9.90 Omega = 0.00 Kappa = 0.00 296 frames Set 2 Theta = 16.20 Kappa = -124.00 Phi = 0.00 185 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21140 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_limit_l_max 70 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.04 _reflns_number_total 13745 _reflns_number_gt 9858 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #========================================================================== #==== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack 0.01(5) _refine_ls_number_reflns 9858 _refine_ls_number_parameters 650 _refine_ls_number_restraints 4 _refine_ls_number_constraints 4 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_R_factor_all 0.096 _refine_ls_R_factor_gt 0.073 _refine_ls_wR_factor_all 0.204 _refine_ls_wR_factor_ref 0.091 _refine_ls_goodness_of_fit_all 1.204 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_shift/su_max 0.006 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.341 _refine_diff_density_min -0.9000 #========================================================================== #==== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RU 0.46969(4) 1.10678(4) 0.59738(1) 0.0323(2) 1.000 Uani ? ? Ru N1 0.5921(4) 1.2028(5) 0.6257(1) 0.034(2) 1.000 Uani ? ? N C1 0.5786(6) 1.2286(6) 0.6507(1) 0.041(3) 1.000 Uani ? ? C C2 0.6724(7) 1.3016(7) 0.6667(2) 0.048(4) 1.000 Uani ? ? C C3 0.7800(7) 1.3428(7) 0.6578(2) 0.046(4) 1.000 Uani ? ? C C4 0.7988(6) 1.3186(6) 0.6312(2) 0.038(3) 1.000 Uani ? ? C C5 0.9079(6) 1.3584(6) 0.6192(2) 0.045(4) 1.000 Uani ? ? C C6 0.9191(6) 1.3366(7) 0.5936(2) 0.042(4) 1.000 Uani ? ? C C7 0.8187(5) 1.2684(6) 0.5769(2) 0.035(3) 1.000 Uani ? ? C C8 0.8226(6) 1.2440(6) 0.5500(2) 0.044(3) 1.000 Uani ? ? C C9 0.7233(6) 1.1805(6) 0.5368(2) 0.044(3) 1.000 Uani ? ? C C10 0.6177(6) 1.1377(5) 0.5493(1) 0.035(3) 1.000 Uani ? ? C N2 0.6120(4) 1.1601(4) 0.5751(1) 0.033(2) 1.000 Uani ? ? N C11 0.7104(5) 1.2246(6) 0.5890(1) 0.033(3) 1.000 Uani ? ? C C12 0.7003(5) 1.2481(5) 0.6160(1) 0.033(3) 1.000 Uani ? ? C N3 0.4598(5) 0.9500(5) 0.6009(1) 0.035(2) 1.000 Uani ? ? N C13 0.5248(6) 0.9214(7) 0.6157(1) 0.039(3) 1.000 Uani ? ? C C14 0.5236(6) 0.8197(6) 0.6128(2) 0.047(3) 1.000 Uani ? ? C C15 0.4514(6) 0.7404(6) 0.5950(2) 0.051(3) 1.000 Uani ? ? C C16 0.3814(6) 0.7663(6) 0.5796(2) 0.038(3) 1.000 Uani ? ? C C17 0.3870(5) 0.8708(5) 0.5826(1) 0.034(3) 1.000 Uani ? ? C C18 0.3225(5) 0.9108(5) 0.5661(1) 0.032(3) 1.000 Uani ? ? C C19 0.2365(5) 0.8452(5) 0.5477(1) 0.028(3) 1.000 Uani ? ? C C20 0.1862(5) 0.8979(6) 0.5334(1) 0.031(3) 1.000 Uani ? ? C C21 0.2268(5) 1.0131(5) 0.5368(1) 0.032(3) 1.000 Uani ? ? C C22 0.3133(5) 1.0726(6) 0.5551(1) 0.031(2) 1.000 Uani ? ? C N4 0.3582(4) 1.0211(4) 0.5692(1) 0.026(2) 1.000 Uani ? ? N C23 0.3687(5) 1.1975(5) 0.5609(1) 0.027(3) 1.000 Uani ? ? C C24 0.3493(6) 1.2742(5) 0.5467(1) 0.042(3) 1.000 Uani ? ? C C25 0.4084(7) 1.3882(6) 0.5528(2) 0.048(3) 1.000 Uani ? ? C C26 0.4881(6) 1.4255(6) 0.5730(2) 0.043(3) 1.000 Uani ? ? C C27 0.5063(6) 1.3470(6) 0.5868(1) 0.036(3) 1.000 Uani ? ? C N5 0.4484(4) 1.2360(4) 0.5811(1) 0.031(2) 1.000 Uani ? ? N C28 0.0880(5) 0.8293(5) 0.5153(1) 0.031(3) 1.000 Uani ? ? C C29 0.0055(5) 0.7183(6) 0.5226(1) 0.035(3) 1.000 Uani ? ? C C30 -0.0907(5) 0.6557(6) 0.5075(1) 0.036(3) 1.000 Uani ? ? C C31 -0.0986(5) 0.7034(5) 0.4838(1) 0.036(3) 1.000 Uani ? ? C C32 -0.0173(5) 0.8131(5) 0.4752(2) 0.034(3) 1.000 Uani ? ? C C33 0.0764(6) 0.8773(5) 0.4915(1) 0.033(3) 1.000 Uani ? ? C C34 -0.1855(6) 0.5372(6) 0.5149(2) 0.041(4) 1.000 Uani ? ? C C35 -0.1756(8) 0.5087(7) 0.5442(2) 0.044(4) 1.000 Uani ? ? C C36 -0.3045(7) 0.5251(8) 0.5103(2) 0.058(5) 1.000 Uani ? ? C C37 -0.1742(8) 0.4500(7) 0.4974(2) 0.047(4) 1.000 Uani ? ? C C38 -0.0352(6) 0.8551(7) 0.4482(2) 0.051(3) 1.000 Uani ? ? C C39 -0.1484(7) 0.8593(8) 0.4501(2) 0.068(4) 1.000 Uani ? ? C C40 -0.0434(7) 0.7783(8) 0.4258(2) 0.054(4) 1.000 Uani ? ? C C41 0.0644(8) 0.9783(7) 0.4416(2) 0.057(4) 1.000 Uani ? ? C O1 0.3364(4) 1.0633(4) 0.6259(1) 0.041(2) 1.000 Uani ? ? O P1 0.3658(2) 1.0712(2) 0.30205(5) 0.046(1) 1.000 Uani ? ? P F1 0.3204(8) 1.1506(8) 0.3115(2) 0.145(7) 1.000 Uani ? ? F F2 0.2811(7) 0.9649(7) 0.3194(2) 0.130(6) 1.000 Uani ? ? F F3 0.296(1) 1.042(1) 0.2775(3) 0.23(1) 1.000 Uani ? ? F F4 0.4604(9) 1.1778(9) 0.2894(2) 0.160(7) 1.000 Uani ? ? F F5 0.432(1) 1.0966(9) 0.3286(2) 0.179(9) 1.000 Uani ? ? F F6 0.4076(7) 0.9868(7) 0.2915(2) 0.120(5) 1.000 Uani ? ? F P2 0.4704(2) 1.1716(2) 0.47377(5) 0.0416(9) 1.000 Uani ? ? P F7 0.538(1) 1.215(1) 0.4997(3) 0.21(1) 1.000 Uani ? ? F F8 0.5393(6) 1.2884(6) 0.4597(2) 0.101(4) 1.000 Uani ? ? F F9 0.4029(6) 1.0526(5) 0.4889(1) 0.091(4) 1.000 Uani ? ? F F10 0.3817(8) 1.1280(9) 0.4507(2) 0.153(7) 1.000 Uani ? ? F F11 0.3958(7) 1.2178(7) 0.4856(2) 0.121(5) 1.000 Uani ? ? F F12 0.527(1) 1.117(1) 0.4562(3) 0.179(9) 1.000 Uani ? ? F C42 0.052(1) 0.869(1) 0.3550(3) 0.111(8) 1.000 Uani ? ? C C43 0.0000 0.793(1) 0.3333 0.080(8) 0.500 Uani ? ? C O2 0.0000 0.705(1) 0.3333 0.133(9) 0.500 Uani ? ? O C44 0.058(1) 0.842(1) 0.6043(3) 0.080(7) 1.000 Uani ? ? C C45 0.1159(8) 0.7812(8) 0.6176(2) 0.050(4) 1.000 Uani ? ? C C46 0.061(1) 0.656(1) 0.6134(3) 0.088(8) 1.000 Uani ? ? C O3 0.2042(5) 0.8329(5) 0.6296(1) 0.057(3) 1.000 Uani ? ? O C47 0.0074(9) 0.677(1) 0.6891(2) 0.091(6) 1.000 Uani ? ? C C48 -0.0249(7) 0.7368(8) 0.7104(2) 0.065(5) 1.000 Uani ? ? C C49 -0.142(1) 0.681(1) 0.7215(3) 0.079(8) 1.000 Uani ? ? C O4 0.0499(5) 0.8344(6) 0.7180(2) 0.065(4) 1.000 Uani ? ? O H1 0.5038 1.1968 0.6578 0.0525 1.000 Uiso calc C1 H H2 0.6597 1.3222 0.6839 0.0624 1.000 Uiso calc C2 H H3 0.8428 1.3876 0.6693 0.0678 1.000 Uiso calc C3 H H4 0.9745 1.4016 0.6296 0.0644 1.000 Uiso calc C5 H H5 0.9931 1.3659 0.5862 0.0617 1.000 Uiso calc C6 H H6 0.8935 1.2715 0.5411 0.0534 1.000 Uiso calc C8 H H7 0.7255 1.1644 0.5184 0.0525 1.000 Uiso calc C9 H H8 0.5496 1.0926 0.5395 0.0436 1.000 Uiso calc C10 H H9 0.5736 0.9738 0.6288 0.0539 1.000 Uiso calc C13 H H10 0.5733 0.8048 0.6232 0.0577 1.000 Uiso calc C14 H H11 0.4489 0.6694 0.5930 0.0606 1.000 Uiso calc C15 H H12 0.3297 0.7122 0.5672 0.0495 1.000 Uiso calc C16 H H13 0.2127 0.7670 0.5450 0.0380 1.000 Uiso calc C19 H H14 0.1960 1.0508 0.5267 0.0409 1.000 Uiso calc C21 H H15 0.2947 1.2476 0.5327 0.0507 1.000 Uiso calc C24 H H16 0.3945 1.4407 0.5432 0.0576 1.000 Uiso calc C25 H H17 0.5303 1.5042 0.5774 0.0555 1.000 Uiso calc C26 H H18 0.5615 1.3732 0.6006 0.0474 1.000 Uiso calc C27 H H19 0.0163 0.6857 0.5383 0.0426 1.000 Uiso calc C29 H H20 -0.1627 0.6594 0.4727 0.0453 1.000 Uiso calc C31 H H21 0.1320 0.9528 0.4866 0.0430 1.000 Uiso calc C33 H H22 -0.2359 0.4342 0.5483 0.0640 1.000 Uiso calc C35 H H23 -0.1045 0.5120 0.5469 0.0640 1.000 Uiso calc C35 H H24 -0.1802 0.5623 0.5556 0.0640 1.000 Uiso calc C35 H H25 -0.3623 0.4503 0.5151 0.0867 1.000 Uiso calc C36 H H26 -0.3115 0.5791 0.5211 0.0867 1.000 Uiso calc C36 H H27 -0.3125 0.5386 0.4921 0.0867 1.000 Uiso calc C36 H H28 -0.2331 0.3752 0.5017 0.0698 1.000 Uiso calc C37 H H29 -0.1803 0.4650 0.4791 0.0698 1.000 Uiso calc C37 H H30 -0.1021 0.4561 0.5004 0.0698 1.000 Uiso calc C37 H H31 -0.0544 0.8071 0.4095 0.0697 1.000 Uiso calc C40 H H32 0.0251 0.7751 0.4249 0.0697 1.000 Uiso calc C40 H H33 -0.1059 0.7039 0.4288 0.0697 1.000 Uiso calc C40 H H34 -0.1619 0.8851 0.4337 0.0788 1.000 Uiso calc C39 H H35 -0.2100 0.7852 0.4539 0.0788 1.000 Uiso calc C39 H H36 -0.1419 0.9101 0.4640 0.0788 1.000 Uiso calc C39 H H37 0.0506 1.0016 0.4248 0.0734 1.000 Uiso calc C41 H H38 0.0684 1.0297 0.4551 0.0734 1.000 Uiso calc C41 H H39 0.1344 0.9782 0.4410 0.0734 1.000 Uiso calc C41 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RU 0.0306(2) 0.0341(2) 0.0323(2) 0.0167(1) -0.0019(2) -0.0034(2) Ru N1 0.034(2) 0.038(2) 0.030(3) 0.020(2) -0.004(2) -0.004(2) N C1 0.055(3) 0.044(3) 0.028(3) 0.029(2) -0.005(3) -0.002(3) C C2 0.068(4) 0.062(4) 0.026(3) 0.042(3) -0.009(3) -0.005(3) C C3 0.047(4) 0.045(4) 0.047(4) 0.010(3) -0.029(3) -0.003(3) C C4 0.038(3) 0.030(3) 0.047(4) 0.017(2) -0.016(3) -0.007(3) C C5 0.038(3) 0.037(3) 0.062(4) 0.010(3) -0.021(3) 0.003(3) C C6 0.028(3) 0.044(3) 0.060(4) 0.010(2) -0.002(3) 0.012(4) C C7 0.027(3) 0.029(3) 0.053(4) 0.013(2) 0.002(3) 0.011(3) C C8 0.043(3) 0.043(3) 0.047(4) 0.028(2) 0.015(3) 0.012(3) C C9 0.050(3) 0.051(3) 0.033(3) 0.035(2) 0.010(3) 0.007(3) C C10 0.044(3) 0.028(2) 0.037(3) 0.023(2) -0.004(3) -0.005(2) C N2 0.030(2) 0.035(2) 0.033(3) 0.020(2) 0.002(2) 0.001(2) N C11 0.028(2) 0.031(2) 0.040(3) 0.017(2) -0.002(2) 0.002(3) C C12 0.034(3) 0.032(3) 0.035(3) 0.018(2) -0.006(2) 0.003(2) C N3 0.034(2) 0.034(2) 0.036(3) 0.020(2) 0.003(2) 0.004(2) N C13 0.039(3) 0.054(4) 0.029(3) 0.022(2) 0.000(3) 0.006(3) C C14 0.047(3) 0.047(3) 0.048(4) 0.029(2) 0.002(3) 0.017(3) C C15 0.063(3) 0.047(3) 0.044(4) 0.038(2) 0.007(3) 0.009(3) C C16 0.042(3) 0.031(3) 0.043(4) 0.020(2) 0.006(3) -0.001(3) C C17 0.030(2) 0.035(3) 0.038(3) 0.020(2) 0.003(2) 0.003(2) C C18 0.028(2) 0.034(2) 0.034(3) 0.018(2) 0.000(3) -0.004(2) C C19 0.026(3) 0.026(3) 0.034(3) 0.011(2) -0.001(2) -0.003(2) C C20 0.030(3) 0.034(3) 0.028(3) 0.016(2) 0.003(2) -0.005(2) C C21 0.030(2) 0.032(3) 0.034(3) 0.017(2) -0.005(2) -0.003(2) C C22 0.030(2) 0.031(2) 0.032(3) 0.019(2) -0.003(2) -0.009(3) C N4 0.019(2) 0.032(2) 0.028(2) 0.014(1) -0.002(2) -0.002(2) N C23 0.022(2) 0.025(2) 0.037(3) 0.010(2) -0.002(2) -0.005(2) C C24 0.047(3) 0.039(3) 0.040(3) 0.028(2) -0.007(3) -0.005(3) C C25 0.049(3) 0.044(3) 0.049(4) 0.031(2) -0.009(3) -0.002(3) C C26 0.049(3) 0.032(3) 0.051(4) 0.024(2) -0.005(3) -0.009(3) C C27 0.035(3) 0.039(3) 0.035(3) 0.018(2) -0.005(3) -0.008(3) C N5 0.032(2) 0.029(2) 0.031(3) 0.017(1) -0.001(2) -0.003(2) N C28 0.031(2) 0.035(3) 0.026(3) 0.019(2) 0.001(2) -0.004(2) C C29 0.036(3) 0.034(2) 0.034(3) 0.022(2) -0.004(2) -0.006(3) C C30 0.036(3) 0.034(3) 0.038(3) 0.018(2) -0.002(3) -0.005(3) C C31 0.035(3) 0.035(3) 0.040(3) 0.021(2) -0.006(3) -0.008(3) C C32 0.030(3) 0.031(3) 0.042(4) 0.018(2) -0.008(3) -0.009(3) C C33 0.034(3) 0.032(3) 0.033(3) 0.016(2) 0.006(3) -0.005(2) C C34 0.033(3) 0.035(3) 0.059(5) 0.014(2) -0.006(3) -0.000(3) C C35 0.050(4) 0.035(4) 0.049(5) 0.011(3) -0.001(4) -0.002(3) C C36 0.036(4) 0.055(4) 0.100(7) 0.016(3) -0.000(4) 0.018(5) C C37 0.060(5) 0.030(3) 0.060(5) 0.013(3) -0.010(4) -0.010(3) C C38 0.050(3) 0.056(3) 0.047(4) 0.037(2) -0.002(3) 0.002(3) C C39 0.062(3) 0.083(4) 0.060(5) 0.054(2) -0.001(4) 0.007(4) C C40 0.063(4) 0.063(4) 0.041(4) 0.036(3) -0.011(4) -0.011(4) C C41 0.077(4) 0.053(4) 0.047(5) 0.038(3) -0.009(4) 0.004(3) C O1 0.033(2) 0.053(3) 0.041(3) 0.026(1) 0.009(2) 0.002(2) O P1 0.0491(9) 0.0436(9) 0.045(1) 0.0241(6) 0.0048(8) 0.0012(8) P F1 0.145(7) 0.145(6) 0.145(8) 0.073(4) 0.000(6) -0.000(6) F F2 0.130(5) 0.130(5) 0.130(7) 0.065(4) 0.000(5) 0.000(5) F F3 0.23(1) 0.23(1) 0.23(1) 0.113(8) -0.00(1) -0.00(1) F F4 0.160(7) 0.160(7) 0.160(9) 0.080(5) 0.000(7) 0.000(7) F F5 0.179(8) 0.179(8) 0.18(1) 0.089(6) -0.000(8) -0.000(8) F F6 0.120(5) 0.120(5) 0.120(6) 0.060(4) 0.000(5) 0.000(5) F P2 0.0381(9) 0.0351(9) 0.054(1) 0.0152(6) -0.0050(8) 0.0006(8) P F7 0.21(1) 0.21(1) 0.21(1) 0.103(7) -0.00(1) 0.00(1) F F8 0.101(4) 0.101(4) 0.101(5) 0.050(3) 0.000(4) 0.000(4) F F9 0.091(4) 0.091(4) 0.091(4) 0.045(3) 0.000(4) 0.000(3) F F10 0.153(7) 0.153(7) 0.153(9) 0.077(5) -0.000(6) -0.000(7) F F11 0.121(5) 0.121(5) 0.121(6) 0.060(3) 0.000(5) 0.000(5) F F12 0.179(8) 0.179(8) 0.18(1) 0.089(6) 0.000(8) 0.000(8) F C42 0.120(8) 0.16(1) 0.071(7) 0.077(6) 0.025(6) -0.008(7) C C43 0.09(1) 0.074(7) 0.081(8) 0.0425 0.053(7) 0.0266 C O2 0.20(1) 0.123(7) 0.097(8) 0.0978 0.065(8) 0.0327 O C44 0.056(6) 0.096(8) 0.095(8) 0.019(5) -0.008(6) 0.025(7) C C45 0.049(4) 0.058(5) 0.046(4) 0.012(4) 0.006(4) 0.001(4) C C46 0.098(9) 0.061(6) 0.11(1) 0.021(6) 0.006(8) -0.010(7) C O3 0.048(3) 0.060(3) 0.066(4) 0.021(2) -0.002(3) 0.010(3) O C47 0.102(6) 0.111(6) 0.067(6) 0.072(4) -0.022(5) -0.030(5) C C48 0.051(4) 0.078(5) 0.068(6) 0.036(3) -0.018(4) 0.003(4) C C49 0.044(6) 0.12(1) 0.089(8) 0.010(6) 0.006(6) -0.009(8) C O4 0.045(3) 0.079(4) 0.078(5) 0.031(2) -0.002(3) 0.002(4) O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU N1 2.072(6) . . ? RU N2 2.024(6) . . ? RU N3 2.066(7) . . ? RU N4 1.966(6) . . ? RU N5 2.077(6) . . ? RU O1 2.142(5) . . ? N1 C1 1.34(1) . . ? N1 C12 1.36(1) . . ? C1 C2 1.41(1) . . ? C2 C3 1.35(1) . . ? C3 C4 1.43(1) . . ? C4 C5 1.43(1) . . ? C4 C12 1.41(1) . . ? C5 C6 1.34(1) . . ? C6 C7 1.46(1) . . ? C7 C8 1.40(1) . . ? C7 C11 1.42(1) . . ? C8 C9 1.35(1) . . ? C9 C10 1.39(1) . . ? C10 N2 1.34(1) . . ? N2 C11 1.365(9) . . ? C11 C12 1.41(1) . . ? N3 C13 1.35(1) . . ? N3 C17 1.38(1) . . ? C13 C14 1.38(1) . . ? C14 C15 1.36(1) . . ? C15 C16 1.39(1) . . ? C16 C17 1.39(1) . . ? C17 C18 1.49(1) . . ? C18 C19 1.40(1) . . ? C18 N4 1.330(9) . . ? C19 C20 1.40(1) . . ? C20 C21 1.38(1) . . ? C20 C28 1.49(1) . . ? C21 C22 1.39(1) . . ? C22 N4 1.334(9) . . ? C22 C23 1.50(1) . . ? C23 C24 1.39(1) . . ? C23 N5 1.379(9) . . ? C24 C25 1.37(1) . . ? C25 C26 1.38(1) . . ? C26 C27 1.39(1) . . ? C27 N5 1.33(1) . . ? C28 C29 1.40(1) . . ? C28 C33 1.41(1) . . ? C29 C30 1.37(1) . . ? C30 C31 1.38(1) . . ? C30 C34 1.52(1) . . ? C31 C32 1.40(1) . . ? C32 C33 1.39(1) . . ? C32 C38 1.53(1) . . ? C34 C35 1.54(1) . . ? C34 C36 1.55(1) . . ? C34 C37 1.54(1) . . ? C38 C39 1.56(1) . . ? C38 C40 1.50(1) . . ? C38 C41 1.57(1) . . ? P1 F1 1.56(1) . . ? P1 F2 1.58(1) . . ? P1 F3 1.48(2) . . ? P1 F4 1.51(1) . . ? P1 F5 1.54(1) . . ? P1 F6 1.60(1) . . ? F1 F3 2.17(2) . . ? F1 F4 2.07(2) . . ? F1 F5 2.15(2) . . ? F2 F5 1.98(2) . . ? F2 F6 2.11(1) . . ? F3 F4 2.15(2) . . ? F3 F6 2.11(2) . . ? F4 F5 2.19(2) . . ? P2 F7 1.53(2) . . ? P2 F8 1.548(8) . . ? P2 F9 1.593(8) . . ? P2 F10 1.55(1) . . ? P2 F11 1.55(1) . . ? P2 F12 1.57(1) . . ? F7 F9 2.11(2) . . ? F7 F11 2.06(2) . . ? F8 F10 2.20(1) . . ? F8 F11 2.13(1) . . ? F9 F12 2.19(2) . . ? F10 F11 2.08(1) . . ? F10 F12 2.06(2) . . ? C42 C43 1.42(2) . . ? C42 C43 1.42(2) . 6_555 ? C43 O2 1.18(2) . . ? C43 O2 1.18(2) . 6_555 ? C44 C45 1.54(2) . . ? C45 C46 1.49(2) . . ? C45 O3 1.20(1) . . ? C47 C48 1.53(2) . . ? C48 C49 1.49(2) . . ? C48 O4 1.26(1) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 RU N2 80.4(2) . . . ? N1 RU N3 102.0(3) . . . ? N1 RU N4 177.2(3) . . . ? N1 RU N5 98.3(3) . . . ? N1 RU O1 90.9(2) . . . ? N2 RU N3 88.5(2) . . . ? N2 RU N4 97.3(2) . . . ? N2 RU N5 89.5(2) . . . ? N2 RU O1 171.3(2) . . . ? N3 RU N4 79.5(2) . . . ? N3 RU N5 159.0(2) . . . ? N3 RU O1 92.8(2) . . . ? N4 RU N5 80.0(2) . . . ? N4 RU O1 91.4(2) . . . ? N5 RU O1 92.4(2) . . . ? RU N1 C1 129.3(6) . . . ? RU N1 C12 112.5(5) . . . ? C1 N1 C12 118.1(7) . . . ? N1 C1 C2 121.6(8) . . . ? C1 C2 C3 120.9(8) . . . ? C2 C3 C4 119.5(7) . . . ? C3 C4 C5 125.3(7) . . . ? C3 C4 C12 116.3(8) . . . ? C5 C4 C12 118.4(8) . . . ? C4 C5 C6 122.0(8) . . . ? C5 C6 C7 120.8(8) . . . ? C6 C7 C8 124.6(8) . . . ? C6 C7 C11 117.5(8) . . . ? C8 C7 C11 118.0(7) . . . ? C7 C8 C9 118.7(8) . . . ? C8 C9 C10 122.1(8) . . . ? C9 C10 N2 120.2(8) . . . ? RU N2 C10 127.3(6) . . . ? RU N2 C11 113.3(5) . . . ? C10 N2 C11 119.4(7) . . . ? C7 C11 N2 121.6(7) . . . ? C7 C11 C12 120.8(7) . . . ? N2 C11 C12 117.5(7) . . . ? N1 C12 C4 123.5(7) . . . ? N1 C12 C11 116.2(7) . . . ? C4 C12 C11 120.3(7) . . . ? RU N3 C13 128.7(6) . . . ? RU N3 C17 113.4(5) . . . ? C13 N3 C17 117.2(7) . . . ? N3 C13 C14 123.1(8) . . . ? C13 C14 C15 120.2(8) . . . ? C14 C15 C16 118.3(8) . . . ? C15 C16 C17 120.0(8) . . . ? N3 C17 C16 121.2(7) . . . ? N3 C17 C18 114.0(7) . . . ? C16 C17 C18 124.8(7) . . . ? C17 C18 C19 126.0(7) . . . ? C17 C18 N4 113.2(7) . . . ? C19 C18 N4 120.7(7) . . . ? C18 C19 C20 118.3(7) . . . ? C19 C20 C21 119.6(7) . . . ? C19 C20 C28 120.1(7) . . . ? C21 C20 C28 120.3(7) . . . ? C20 C21 C22 118.7(7) . . . ? C21 C22 N4 121.4(7) . . . ? C21 C22 C23 125.8(7) . . . ? N4 C22 C23 112.8(6) . . . ? RU N4 C18 119.3(5) . . . ? RU N4 C22 119.2(5) . . . ? C18 N4 C22 121.3(6) . . . ? C22 C23 C24 125.0(7) . . . ? C22 C23 N5 115.0(6) . . . ? C24 C23 N5 119.9(7) . . . ? C23 C24 C25 120.5(7) . . . ? C24 C25 C26 119.0(8) . . . ? C25 C26 C27 119.4(8) . . . ? C26 C27 N5 121.9(7) . . . ? RU N5 C23 112.5(5) . . . ? RU N5 C27 128.0(5) . . . ? C23 N5 C27 119.3(7) . . . ? C20 C28 C29 119.8(7) . . . ? C20 C28 C33 120.0(7) . . . ? C29 C28 C33 120.2(7) . . . ? C28 C29 C30 121.6(7) . . . ? C29 C30 C31 117.1(8) . . . ? C29 C30 C34 124.1(7) . . . ? C31 C30 C34 118.7(7) . . . ? C30 C31 C32 123.7(7) . . . ? C31 C32 C33 118.1(7) . . . ? C31 C32 C38 118.6(7) . . . ? C33 C32 C38 123.4(8) . . . ? C28 C33 C32 119.2(7) . . . ? C30 C34 C35 111.3(7) . . . ? C30 C34 C36 111.2(7) . . . ? C30 C34 C37 108.4(7) . . . ? C35 C34 C36 109.3(8) . . . ? C35 C34 C37 107.3(8) . . . ? C36 C34 C37 109.4(8) . . . ? C32 C38 C39 107.4(7) . . . ? C32 C38 C40 112.0(8) . . . ? C32 C38 C41 111.7(7) . . . ? C39 C38 C40 109.7(8) . . . ? C39 C38 C41 108.1(8) . . . ? C40 C38 C41 107.8(8) . . . ? F1 P1 F2 96.0(6) . . . ? F1 P1 F3 91.0(8) . . . ? F1 P1 F4 84.7(6) . . . ? F1 P1 F5 88.1(7) . . . ? F1 P1 F6 177.4(6) . . . ? F2 P1 F3 98.0(8) . . . ? F2 P1 F4 170.4(6) . . . ? F2 P1 F5 78.7(6) . . . ? F2 P1 F6 83.5(5) . . . ? F3 P1 F4 91.6(8) . . . ? F3 P1 F5 176.4(8) . . . ? F3 P1 F6 86.6(8) . . . ? F4 P1 F5 91.8(7) . . . ? F4 P1 F6 96.3(6) . . . ? F5 P1 F6 94.3(6) . . . ? P1 F1 F3 43.1(6) . . . ? P1 F1 F4 46.7(5) . . . ? P1 F1 F5 45.7(5) . . . ? F3 F1 F4 60.8(6) . . . ? F3 F1 F5 88.8(7) . . . ? F4 F1 F5 62.5(6) . . . ? P1 F2 F5 49.9(5) . . . ? P1 F2 F6 48.6(4) . . . ? F5 F2 F6 68.4(6) . . . ? P1 F3 F1 45.9(6) . . . ? P1 F3 F4 44.7(6) . . . ? P1 F3 F6 49.0(6) . . . ? F1 F3 F4 57.2(6) . . . ? F1 F3 F6 94.9(8) . . . ? F4 F3 F6 65.9(7) . . . ? P1 F4 F1 48.6(5) . . . ? P1 F4 F3 43.6(6) . . . ? P1 F4 F5 44.7(5) . . . ? F1 F4 F3 61.9(7) . . . ? F1 F4 F5 60.7(6) . . . ? F3 F4 F5 88.3(7) . . . ? P1 F5 F1 46.2(5) . . . ? P1 F5 F2 51.5(5) . . . ? P1 F5 F4 43.5(5) . . . ? F1 F5 F2 68.5(6) . . . ? F1 F5 F4 56.8(5) . . . ? F2 F5 F4 95.0(7) . . . ? P1 F6 F2 47.9(4) . . . ? P1 F6 F3 44.4(5) . . . ? F2 F6 F3 66.2(6) . . . ? F7 P2 F8 93.3(7) . . . ? F7 P2 F9 85.0(6) . . . ? F7 P2 F10 168.0(8) . . . ? F7 P2 F11 84.3(7) . . . ? F7 P2 F12 108.8(8) . . . ? F8 P2 F9 178.2(5) . . . ? F8 P2 F10 90.3(6) . . . ? F8 P2 F11 86.8(5) . . . ? F8 P2 F12 92.2(6) . . . ? F9 P2 F10 91.5(5) . . . ? F9 P2 F11 93.8(5) . . . ? F9 P2 F12 87.6(6) . . . ? F10 P2 F11 84.4(6) . . . ? F10 P2 F12 82.5(7) . . . ? F11 P2 F12 166.9(6) . . . ? P2 F7 F9 48.8(5) . . . ? P2 F7 F11 48.3(5) . . . ? F9 F7 F11 66.7(6) . . . ? P2 F8 F10 44.9(4) . . . ? P2 F8 F11 46.6(4) . . . ? F10 F8 F11 57.6(5) . . . ? P2 F9 F7 46.1(5) . . . ? P2 F9 F12 45.7(4) . . . ? F7 F9 F12 71.7(6) . . . ? P2 F10 F8 44.7(4) . . . ? P2 F10 F11 47.7(4) . . . ? P2 F10 F12 49.1(5) . . . ? F8 F10 F11 59.5(5) . . . ? F8 F10 F12 63.5(6) . . . ? F11 F10 F12 96.7(7) . . . ? P2 F11 F7 47.4(5) . . . ? P2 F11 F8 46.6(4) . . . ? P2 F11 F10 47.9(4) . . . ? F7 F11 F8 64.4(6) . . . ? F7 F11 F10 95.2(7) . . . ? F8 F11 F10 63.0(5) . . . ? P2 F12 F9 46.6(4) . . . ? P2 F12 F10 48.4(5) . . . ? F9 F12 F10 64.0(6) . . . ? C42 C43 C42 123(2) . . 6_555 ? C42 C43 O2 118(1) . . . ? C42 C43 O2 118(1) 6_555 . . ? C44 C45 C46 116(1) . . . ? C44 C45 O3 121(1) . . . ? C46 C45 O3 121(1) . . . ? C47 C48 C49 120(1) . . . ? C47 C48 O4 118(1) . . . ? C49 C48 O4 121(1) . . . ?