Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email TANISJKA@HOTMAIL.COM _publ_contact_author_name 'Mr Lars Preuss Nielsen' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_section_references ; Altomare,A., Cascarano,G., Giacovazzo,C., Guagliardi,A., Moliterni,.A,G,G., Burla,M.C., Polidori,G., Camalli,M. & Spagna,R. (1997). SIR97. University of Bari, Italy. Becker,P.J. & Coppens, P. (1974). Acta Cryst. A30, 129-153. Burnett,M.N. & Johnson,C.K. (1996). ORTEP-III. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. Busing,W.R., Martin,K.O. & Levy,H.A. (1962). ORFLS. Report ORNL-TM-305. Oak Ridge National Laboratory, Tennessee, USA. Hazell,A. (1995). KRYSTAL, An integrated system of crystallographic programs. Aarhus University, Denmark. Pawley,G.S. Adv. Struct. Res. Diffr. Methods. (1971) 4 1-64. Siemens (1995) SMART, SAINT and XPREP Area-Detector Control and Integration Software. Siemens Analytical X-ray Instruments Inc. Madison, Wisconsin, USA. ; loop_ _publ_author_name L.P.Nielsen A.Hazell R.G.Hazell C.J.McKenzie data_rucu-3b' _database_code_CSD 200507 # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common (Cu2Ru(tpbd)2(bipy)2(BF4)2)(BF4)2(PF6)2 _chemical_formula_sum 'C80 H74 B4 Cu2 F28 N16 O P2 Ru' _chemical_formula_weight 2140.88 #=================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _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 14.122(2) _cell_length_b 21.427(3) _cell_length_c 30.472(5) _cell_angle_alpha 90.000 _cell_angle_beta 93.110(4) _cell_angle_gamma 90.000 _cell_volume 9207(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 29.8 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4312 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.612 _exptl_absorpt_correction_T_max 0.836 _exptl_absorpt_process_details 'XPREP, 1995' #=================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation scans with narrow frames' _diffrn_standards_decay_% 0 _diffrn_reflns_number 36703 _diffrn_reflns_av_R_equivalents 0.079 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.9 _diffrn_reflns_theta_max 29.8 _diffrn_reflns_reduction_process 36703 _reflns_number_total 13183 _reflns_number_gt 7282 _reflns_threshold_expression I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Altomare et al., 1997 ), KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #=================================== # 8. REFINEMENT DATA _refine_special_details ; In the latest refinement cycles the BF4 groups were constrained ( Pawley, 1971) to regular tetrahedral geometry. The supposed water molcule is found on a 2-axis and surrounded by the highest peaks (too close to be meaningfull). The water hydrogen atoms are included in the direction towards F13 as indicated by a short distance. The deepest holes in the difference map are found at least 1.25\%A from the nearest atom in the region of the water molecule and BF4 groups. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w= 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^- |F|}^2^ ; _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7282 _refine_ls_number_parameters 588 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_gt 0.140 _refine_ls_wR_factor_ref 0.142 _refine_ls_goodness_of_fit_ref 1.62 _refine_ls_shift/su_max 0.0017 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_max 1.68(8) _refine_diff_density_min -2.38(8) #========================================== # 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_thermal_displace_type Ru 0.0000 0.31032(6) 0.25000 0.0383(8) Uij Cu 0.2227(1) 0.55615(7) 0.06881(5) 0.0512(10) Uij N1 -0.0402(6) 0.3743(4) 0.1965(3) 0.040(5) Uij N2 0.2731(7) 0.5121(4) 0.1378(3) 0.050(6) Uij C1 0.0365(9) 0.4127(6) 0.1800(4) 0.047(7) Uij C2 0.0432(8) 0.4759(6) 0.1873(4) 0.047(7) Uij C3 0.1220(9) 0.5070(5) 0.1744(4) 0.049(7) Uij C4 0.1943(7) 0.4774(6) 0.1532(4) 0.044(7) Uij C5 0.1804(8) 0.4142(6) 0.1434(4) 0.051(8) Uij C6 0.1035(9) 0.3818(6) 0.1573(4) 0.049(7) Uij N11 -0.0123(7) 0.2482(4) 0.1981(4) 0.048(6) Uij C12 0.0239(10) 0.1912(7) 0.1971(5) 0.067(9) Uij C13 0.0279(11) 0.1546(7) 0.1607(6) 0.076(11) Uij C14 -0.0049(10) 0.1776(7) 0.1211(6) 0.074(11) Uij C15 -0.0457(11) 0.2372(7) 0.1204(5) 0.068(10) Uij C16 -0.0454(8) 0.2715(6) 0.1596(5) 0.050(8) Uij C17 -0.0846(8) 0.3348(6) 0.1600(4) 0.047(7) Uij N21 -0.1480(6) 0.3178(4) 0.2551(3) 0.041(6) Uij C22 -0.2062(8) 0.2793(5) 0.2757(4) 0.047(7) Uij C23 -0.2995(8) 0.2930(7) 0.2809(5) 0.061(9) Uij C24 -0.3389(8) 0.3473(8) 0.2637(6) 0.079(11) Uij C25 -0.2808(8) 0.3862(7) 0.2411(5) 0.065(9) Uij C26 -0.1843(7) 0.3714(6) 0.2378(4) 0.045(7) Uij C27 -0.1209(8) 0.4123(5) 0.2148(4) 0.043(7) Uij N31 0.3656(7) 0.5461(5) 0.0638(4) 0.051(6) Uij C32 0.4126(10) 0.5753(6) 0.0335(5) 0.060(9) Uij C33 0.5110(12) 0.5697(8) 0.0312(6) 0.075(11) Uij C34 0.5589(10) 0.5329(8) 0.0610(6) 0.076(11) Uij C35 0.5093(10) 0.5049(7) 0.0933(5) 0.065(9) Uij C36 0.4127(9) 0.5116(7) 0.0940(5) 0.056(8) Uij C37 0.3563(10) 0.4768(7) 0.1262(5) 0.068(10) Uij N41 0.2410(7) 0.6347(5) 0.1034(4) 0.049(6) Uij C42 0.2146(11) 0.6918(7) 0.0881(5) 0.070(10) Uij C43 0.1986(10) 0.7420(6) 0.1147(6) 0.065(10) Uij C44 0.2091(10) 0.7328(7) 0.1588(6) 0.065(10) Uij C45 0.2413(10) 0.6760(6) 0.1757(5) 0.058(9) Uij C46 0.2562(8) 0.6285(6) 0.1474(5) 0.051(8) Uij C47 0.2954(10) 0.5687(6) 0.1643(4) 0.060(9) Uij N51 0.0804(7) 0.5585(5) 0.0753(4) 0.051(6) Uij C52 0.0313(9) 0.6014(7) 0.0955(5) 0.060(9) Uij C53 -0.0642(11) 0.5941(7) 0.1044(6) 0.074(10) Uij C54 -0.1050(9) 0.5378(8) 0.0928(5) 0.072(10) Uij C55 -0.0571(10) 0.4922(7) 0.0723(5) 0.063(9) Uij C56 0.0371(8) 0.5032(6) 0.0636(4) 0.049(8) Uij N61 0.1887(8) 0.4751(5) 0.0391(3) 0.055(7) Uij C66 0.0974(9) 0.4575(6) 0.0417(4) 0.050(8) Uij C62 0.2473(10) 0.4359(7) 0.0198(5) 0.068(10) Uij C63 0.2175(12) 0.3794(8) 0.0027(6) 0.083(12) Uij C64 0.1268(13) 0.3625(7) 0.0049(6) 0.080(12) Uij C65 0.0642(12) 0.4013(7) 0.0247(5) 0.073(10) Uij P1 0.4221(7) 0.2964(4) 0.0879(4) 0.162(8) Uij F1 0.3425(16) 0.3196(10) 0.1092(9) 0.279(25) Uij F2 0.3582(22) 0.2607(16) 0.0555(15) 0.463(48) Uij F3 0.4426(29) 0.2450(11) 0.1217(12) 0.372(43) Uij F4 0.4966(17) 0.2619(15) 0.0667(10) 0.315(31) Uij F5 0.4947(24) 0.3331(11) 0.1170(12) 0.371(38) Uij F6 0.4189(19) 0.3543(9) 0.0614(7) 0.252(24) Uij F11 0.7581(19) 0.1333(7) 0.2937(10) 0.378(39) Uij B1 0.7656(9) 0.0721(7) 0.2943(4) 0.180(35) Uij F12 0.6880(11) 0.0472(8) 0.2759(6) 0.252(19) Uij F13 0.8390(13) 0.0551(17) 0.2724(7) 0.409(52) Uij F14 0.7772(12) 0.0527(10) 0.3352(5) 0.286(27) Uij F21 0.1458(7) 0.6617(6) -0.0552(4) 0.183(13) Uij B2 0.2216(5) 0.6345(3) -0.0369(2) 0.086(15) Uij F22 0.1984(6) 0.6039(5) -0.0016(3) 0.118(8) Uij F23 0.2567(9) 0.5952(6) -0.0650(4) 0.239(20) Uij F24 0.2856(6) 0.6771(4) -0.0258(3) 0.126(9) Uij O 0.000 -0.002(6) 0.250 0.66(17) Uij H -0.054 0.018 0.257 0.80 Uiso H2 -0.006 0.498 0.201 0.06 Uiso H3 0.127 0.551 0.180 0.06 Uiso H5 0.225 0.393 0.127 0.06 Uiso H6 0.097 0.338 0.151 0.06 Uiso H12 0.049 0.174 0.224 0.08 Uiso H13 0.053 0.114 0.163 0.09 Uiso H14 0.000 0.154 0.095 0.09 Uiso H15 -0.073 0.254 0.094 0.08 Uiso H17a -0.074 0.354 0.133 0.06 Uiso H17b -0.151 0.332 0.164 0.06 Uiso H22 -0.182 0.241 0.287 0.06 Uiso H23 -0.337 0.265 0.296 0.07 Uiso H24 -0.403 0.358 0.267 0.10 Uiso H25 -0.306 0.423 0.228 0.08 Uiso H27a -0.156 0.433 0.191 0.05 Uiso H27b -0.095 0.443 0.235 0.05 Uiso H32 0.378 0.601 0.012 0.07 Uiso H33 0.544 0.591 0.009 0.09 Uiso H34 0.625 0.527 0.060 0.09 Uiso H35 0.542 0.481 0.115 0.08 Uiso H37a 0.336 0.438 0.114 0.08 Uiso H37b 0.395 0.469 0.152 0.08 Uiso H42 0.207 0.698 0.057 0.08 Uiso H43 0.181 0.782 0.103 0.08 Uiso H44 0.194 0.766 0.178 0.08 Uiso H45 0.253 0.670 0.207 0.07 Uiso H47a 0.362 0.573 0.167 0.07 Uiso H47b 0.272 0.562 0.193 0.07 Uiso H52 0.062 0.639 0.104 0.07 Uiso H53 -0.099 0.626 0.118 0.09 Uiso H54 -0.169 0.531 0.099 0.09 Uiso H55 -0.087 0.454 0.064 0.08 Uiso H62 0.312 0.448 0.018 0.08 Uiso H63 0.261 0.353 -0.011 0.10 Uiso H64 0.106 0.324 -0.007 0.10 Uiso H65 0.000 0.390 0.027 0.09 Uiso 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 Ru 0.0348(7) 0.0311(7) 0.0487(9) 0.0000 -0.0004(6) 0.0000 Cu 0.0468(9) 0.0522(10) 0.0545(11) -0.0132(7) 0.0009(7) -0.0005(8) N1 0.037(5) 0.037(5) 0.048(6) -0.001(4) 0.010(4) 0.002(4) N2 0.051(6) 0.039(6) 0.061(7) -0.004(5) 0.013(5) 0.003(5) C1 0.055(7) 0.045(7) 0.042(7) -0.004(6) 0.001(6) 0.003(6) C2 0.042(6) 0.043(7) 0.057(8) 0.001(5) 0.009(6) 0.010(6) C3 0.055(7) 0.036(7) 0.057(8) -0.005(6) 0.005(6) 0.002(6) C4 0.032(6) 0.046(7) 0.055(8) -0.007(5) 0.002(5) 0.011(6) C5 0.046(7) 0.052(8) 0.055(8) 0.000(6) 0.002(6) 0.003(6) C6 0.064(8) 0.041(7) 0.041(7) -0.007(6) 0.000(6) 0.007(6) N11 0.043(6) 0.036(6) 0.066(8) -0.007(4) 0.003(5) -0.005(5) C12 0.061(8) 0.059(9) 0.081(11) -0.001(7) 0.000(7) -0.023(9) C13 0.073(10) 0.050(9) 0.103(14) -0.008(7) -0.009(10) -0.030(9) C14 0.056(9) 0.068(11) 0.098(13) -0.012(7) -0.003(8) -0.043(9) C15 0.080(10) 0.057(9) 0.066(10) -0.010(8) -0.005(8) -0.010(8) C16 0.046(7) 0.043(7) 0.062(9) -0.006(6) 0.004(6) -0.010(7) C17 0.042(6) 0.050(7) 0.048(8) -0.007(5) -0.008(6) 0.002(6) N21 0.035(5) 0.032(5) 0.055(7) 0.006(4) -0.008(5) 0.002(5) C22 0.038(6) 0.037(6) 0.067(9) 0.001(5) 0.001(6) 0.006(6) C23 0.018(5) 0.067(9) 0.097(11) -0.007(6) 0.009(6) 0.008(8) C24 0.012(5) 0.107(13) 0.119(14) 0.014(7) 0.002(7) 0.007(11) C25 0.027(6) 0.068(9) 0.098(12) 0.011(6) -0.003(7) -0.002(8) C26 0.030(6) 0.047(7) 0.057(8) 0.001(5) -0.002(5) -0.001(6) C27 0.035(6) 0.039(6) 0.053(8) -0.001(5) -0.003(5) 0.006(6) N31 0.049(6) 0.053(6) 0.051(7) -0.019(5) 0.011(5) 0.000(5) C32 0.067(9) 0.059(9) 0.056(9) -0.019(7) 0.007(7) -0.009(7) C33 0.081(11) 0.072(11) 0.075(11) -0.014(9) 0.037(9) -0.009(9) C34 0.057(9) 0.063(10) 0.109(14) -0.012(8) 0.024(9) -0.016(10) C35 0.050(8) 0.077(10) 0.069(10) -0.008(7) 0.010(7) -0.008(8) C36 0.052(8) 0.062(9) 0.055(9) -0.017(7) 0.009(7) -0.007(7) C37 0.059(8) 0.062(9) 0.085(11) 0.008(7) 0.010(8) 0.001(8) N41 0.038(5) 0.053(6) 0.056(7) -0.010(5) 0.008(5) 0.003(5) C42 0.090(11) 0.058(9) 0.060(9) -0.024(8) -0.015(8) 0.012(8) C43 0.055(8) 0.046(8) 0.097(13) -0.002(6) 0.025(8) 0.011(8) C44 0.058(8) 0.051(9) 0.085(12) -0.018(7) 0.006(8) -0.013(8) C45 0.065(8) 0.046(8) 0.064(9) -0.016(6) 0.004(7) -0.005(7) C46 0.041(7) 0.051(8) 0.061(9) -0.017(6) 0.001(6) 0.001(7) C47 0.072(9) 0.050(8) 0.057(9) -0.020(7) -0.008(7) 0.002(7) N51 0.043(6) 0.041(6) 0.068(8) -0.017(5) -0.005(5) 0.006(5) C52 0.034(7) 0.061(9) 0.082(11) -0.011(6) -0.004(7) -0.002(8) C53 0.062(9) 0.062(10) 0.096(12) -0.004(8) -0.007(8) -0.010(9) C54 0.041(7) 0.090(12) 0.085(11) -0.008(8) 0.009(7) 0.013(9) C55 0.049(8) 0.070(10) 0.070(10) -0.019(7) -0.006(7) 0.002(8) C56 0.047(7) 0.050(8) 0.050(8) -0.003(6) -0.001(6) 0.011(6) N61 0.061(7) 0.052(7) 0.051(7) -0.021(6) -0.003(5) -0.002(5) C66 0.056(7) 0.045(7) 0.047(8) -0.012(6) -0.007(6) 0.006(6) C62 0.053(8) 0.070(10) 0.082(11) -0.015(7) 0.003(8) -0.020(9) C63 0.070(10) 0.077(11) 0.101(13) -0.007(9) -0.001(9) -0.030(10) C64 0.094(12) 0.063(10) 0.082(12) -0.013(9) -0.004(10) -0.023(9) C65 0.095(12) 0.054(9) 0.070(10) -0.023(8) 0.005(9) -0.004(8) P1 0.172(8) 0.109(6) 0.206(9) 0.040(6) 0.033(8) 0.009(7) F1 0.246(22) 0.227(21) 0.383(31) 0.101(18) 0.194(23) -0.020(21) F2 0.341(35) 0.341(36) 0.675(66) 0.184(28) -0.265(40) -0.366(45) F3 0.567(59) 0.159(20) 0.401(41) 0.159(28) 0.117(42) 0.072(25) F4 0.213(21) 0.384(36) 0.344(32) 0.180(23) -0.035(22) -0.148(29) F5 0.439(43) 0.160(19) 0.482(46) -0.001(22) -0.283(39) -0.064(24) F6 0.392(32) 0.163(17) 0.203(19) 0.002(18) 0.036(20) 0.089(15) F11 0.384(36) 0.117(14) 0.601(55) -0.122(19) -0.270(39) 0.089(23) B1 0.136(26) 0.265(47) 0.141(29) -0.146(31) 0.011(22) -0.103(31) F12 0.263(20) 0.230(18) 0.249(19) -0.182(17) -0.121(16) 0.085(15) F13 0.269(32) 0.719(79) 0.242(29) -0.120(41) 0.052(23) -0.112(39) F14 0.205(18) 0.493(39) 0.156(16) -0.123(22) -0.018(14) 0.134(21) F21 0.151(12) 0.180(13) 0.207(15) -0.063(10) -0.089(11) 0.116(12) B2 0.074(13) 0.093(16) 0.088(16) -0.021(12) -0.019(12) 0.014(13) F22 0.112(8) 0.151(10) 0.087(7) -0.057(7) -0.027(6) 0.063(7) F23 0.183(16) 0.293(23) 0.245(20) -0.083(16) 0.066(14) -0.165(18) F24 0.135(9) 0.119(9) 0.120(9) -0.066(7) -0.047(7) 0.039(7) O 0.38(9) 0.83(21) 0.79(19) 0.00 0.15(10) 0.00 #================================= # 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 Ru N11 2.067(10) . . Ru N11 2.067(10) . 2_555 Ru N21 2.111(9) . . Ru N21 2.111(9) . 2_555 Ru N1 2.183(9) . . Ru N1 2.183(9) . 2_555 Cu N41 1.996(10) . . Cu N61 2.005(10) . . Cu N51 2.031(10) . . Cu N31 2.043(10) . . Cu N2 2.377(10) . . Cu F22 2.385(7) . . N1 C1 1.469(14) . . N1 C17 1.507(14) . . N1 C27 1.531(14) . . N2 C4 1.438(14) . . N2 C37 1.456(16) . . N2 C47 1.483(16) . . C1 C6 1.371(17) . . C1 C2 1.375(16) . . C2 C3 1.373(16) . . C3 C4 1.392(16) . . C4 C5 1.398(16) . . C5 C6 1.375(16) . . N11 C12 1.325(16) . . N11 C16 1.334(16) . . C12 C13 1.362(20) . . C13 C14 1.361(22) . . C14 C15 1.402(20) . . C15 C16 1.402(18) . . C16 C17 1.465(17) . . N21 C22 1.344(14) . . N21 C26 1.353(14) . . C22 C23 1.367(15) . . C23 C24 1.380(20) . . C24 C25 1.380(20) . . C25 C26 1.408(15) . . C26 C27 1.458(16) . . N31 C32 1.325(16) . . N31 C36 1.329(16) . . C32 C33 1.401(20) . . C33 C34 1.356(22) . . C34 C35 1.375(21) . . C35 C36 1.374(18) . . C36 C37 1.497(19) . . N41 C46 1.351(15) . . N41 C42 1.355(17) . . C42 C43 1.371(20) . . C43 C44 1.358(20) . . C44 C45 1.390(19) . . C45 C46 1.359(18) . . C46 C47 1.477(18) . . N51 C52 1.324(16) . . N51 C56 1.372(15) . . C52 C53 1.399(18) . . C53 C54 1.375(20) . . C54 C55 1.360(21) . . C55 C56 1.390(17) . . C56 C66 1.481(18) . . N61 C62 1.336(17) . . N61 C66 1.349(15) . . C66 C65 1.383(18) . . C62 C63 1.376(20) . . C63 C64 1.336(21) . . C64 C65 1.377(22) . . P1 F1 1.419(16) . . P1 F4 1.466(21) . . P1 F6 1.479(17) . . P1 F2 1.509(23) . . P1 F3 1.526(27) . . P1 F5 1.536(21) . . F11 B1 1.316(5) . . B1 F12 1.316(5) . . B1 F13 1.316(4) . . B1 F14 1.316(4) . . F21 B2 1.316(5) . . B2 F22 1.316(5) . . B2 F23 1.316(4) . . B2 F24 1.316(4) . . C2 H2 0.95 . . C3 H3 0.95 . . C5 H5 0.95 . . C6 H6 0.95 . . C12 H12 0.95 . . C13 H13 0.95 . . C14 H14 0.95 . . C15 H15 0.95 . . C17 H17a 0.95 . . C17 H17b 0.95 . . C22 H22 0.95 . . C23 H23 0.95 . . C24 H24 0.95 . . C25 H25 0.95 . . C27 H27a 0.95 . . C27 H27b 0.95 . . C32 H32 0.95 . . C33 H33 0.95 . . C34 H34 0.95 . . C35 H35 0.95 . . C37 H37a 0.95 . . C37 H37b 0.95 . . C42 H42 0.95 . . C43 H43 0.95 . . C44 H44 0.95 . . C45 H45 0.95 . . C47 H47a 0.95 . . C47 H47b 0.95 . . C52 H52 0.95 . . C53 H53 0.95 . . C54 H54 0.95 . . C55 H55 0.94 . . C62 H62 0.95 . . C63 H63 0.95 . . C64 H64 0.95 . . C65 H65 0.95 . . O H 0.91 . . 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 N11 Ru N11 99.9(6) . . 2_555 N11 Ru N21 93.7(4) . . . N11 Ru N21 92.0(4) . . 2_555 N1 Ru N11 79.9(4) . . . N1 Ru N11 169.8(3) 2_555 . . N11 Ru N21 92.0(4) 2_555 . . N11 Ru N21 93.7(4) 2_555 . 2_555 N1 Ru N11 169.8(3) . . 2_555 N1 Ru N11 79.9(4) 2_555 . 2_555 N21 Ru N21 171.2(5) . . 2_555 N1 Ru N21 77.8(3) . . . N1 Ru N21 96.6(3) 2_555 . . N1 Ru N21 96.6(3) . . 2_555 N1 Ru N21 77.8(3) 2_555 . 2_555 N1 Ru N1 102.1(5) . . 2_555 N41 Cu N61 172.0(4) . . . N41 Cu N51 91.6(4) . . . N31 Cu N41 91.6(4) . . . N2 Cu N41 81.0(4) . . . N41 Cu F22 97.0(4) . . . N51 Cu N61 81.4(4) . . . N31 Cu N61 95.1(4) . . . N2 Cu N61 96.2(4) . . . N61 Cu F22 87.0(4) . . . N31 Cu N51 175.2(4) . . . N2 Cu N51 100.0(4) . . . N51 Cu F22 88.9(4) . . . N2 Cu N31 77.0(4) . . . N31 Cu F22 94.2(4) . . . N2 Cu F22 170.8(3) . . . C1 N1 C17 110.4(9) . . . C1 N1 C27 113.9(9) . . . Ru N1 C1 116.1(7) . . . C17 N1 C27 106.2(8) . . . Ru N1 C17 106.1(7) . . . Ru N1 C27 103.3(6) . . . C4 N2 C37 117.3(10) . . . C4 N2 C47 113.0(10) . . . Cu N2 C4 107.1(7) . . . C37 N2 C47 114.0(10) . . . Cu N2 C37 101.5(8) . . . Cu N2 C47 101.6(7) . . . C2 C1 C6 120.9(11) . . . N1 C1 C6 116.4(10) . . . N1 C1 C2 122.7(11) . . . C1 C2 C3 118.8(11) . . . C2 C3 C4 122.5(11) . . . C3 C4 C5 116.3(10) . . . N2 C4 C3 121.1(11) . . . N2 C4 C5 122.2(11) . . . C4 C5 C6 121.8(12) . . . C1 C6 C5 119.4(11) . . . C12 N11 C16 116.2(12) . . . Ru N11 C12 126.5(9) . . . Ru N11 C16 116.2(8) . . . N11 C12 C13 125.6(15) . . . C12 C13 C14 119.1(15) . . . C13 C14 C15 117.6(14) . . . C14 C15 C16 118.8(14) . . . N11 C16 C15 122.5(12) . . . N11 C16 C17 116.9(11) . . . C15 C16 C17 120.5(13) . . . N1 C17 C16 112.6(10) . . . C22 N21 C26 118.4(9) . . . Ru N21 C22 128.4(7) . . . Ru N21 C26 113.0(7) . . . N21 C22 C23 122.6(11) . . . C22 C23 C24 120.6(12) . . . C23 C24 C25 117.4(11) . . . C24 C25 C26 120.3(12) . . . N21 C26 C25 120.6(11) . . . N21 C26 C27 118.0(10) . . . C25 C26 C27 121.4(11) . . . N1 C27 C26 110.2(9) . . . C32 N31 C36 119.7(12) . . . Cu N31 C32 122.4(10) . . . Cu N31 C36 117.8(8) . . . N31 C32 C33 122.0(14) . . . C32 C33 C34 118.5(14) . . . C33 C34 C35 118.6(14) . . . C34 C35 C36 120.7(15) . . . N31 C36 C35 120.5(13) . . . N31 C36 C37 117.9(12) . . . C35 C36 C37 121.4(14) . . . N2 C37 C36 111.3(12) . . . C42 N41 C46 117.1(12) . . . Cu N41 C42 123.7(9) . . . Cu N41 C46 116.7(8) . . . N41 C42 C43 123.8(13) . . . C42 C43 C44 117.2(13) . . . C43 C44 C45 120.7(14) . . . C44 C45 C46 118.5(13) . . . N41 C46 C45 122.4(13) . . . N41 C46 C47 117.9(12) . . . C45 C46 C47 119.6(13) . . . N2 C47 C46 117.1(11) . . . C52 N51 C56 118.9(11) . . . Cu N51 C52 127.5(8) . . . Cu N51 C56 112.5(9) . . . N51 C52 C53 123.1(12) . . . C52 C53 C54 116.4(14) . . . C53 C54 C55 122.5(13) . . . C54 C55 C56 118.0(13) . . . N51 C56 C55 121.0(12) . . . N51 C56 C66 115.4(11) . . . C55 C56 C66 123.6(12) . . . C66 N61 C62 117.8(11) . . . Cu N61 C62 127.1(9) . . . Cu N61 C66 115.0(9) . . . N61 C66 C65 121.9(13) . . . C56 C66 N61 114.6(11) . . . C56 C66 C65 123.5(12) . . . N61 C62 C63 122.4(13) . . . C62 C63 C64 119.5(15) . . . C63 C64 C65 120.0(15) . . . C66 C65 C64 118.4(14) . . . F1 P1 F4 170.1(19) . . . F1 P1 F6 87.4(13) . . . F1 P1 F2 91.0(19) . . . F1 P1 F3 94.0(18) . . . F1 P1 F5 94.4(18) . . . F4 P1 F6 100.6(19) . . . F2 P1 F4 82.7(16) . . . F3 P1 F4 79.6(16) . . . F4 P1 F5 92.3(18) . . . F2 P1 F6 93.9(21) . . . F3 P1 F6 166.7(20) . . . F5 P1 F6 83.4(15) . . . F2 P1 F3 99.3(22) . . . F2 P1 F5 173.9(26) . . . F3 P1 F5 83.2(20) . . . F11 B1 F12 109.47 . . . F11 B1 F13 109.47 . . . F11 B1 F14 109.47 . . . F12 B1 F13 109.47 . . . F12 B1 F14 109.47 . . . F13 B1 F14 109.47 . . . F21 B2 F22 109.47 . . . F21 B2 F23 109.47 . . . F21 B2 F24 109.47 . . . F22 B2 F23 109.47 . . . F22 B2 F24 109.47 . . . F23 B2 F24 109.47 . . . C3 C2 H2 120 . . . C1 C2 H2 120 . . . C2 C3 H3 119 . . . C4 C3 H3 119 . . . C6 C5 H5 119 . . . C4 C5 H5 119 . . . C1 C6 H6 120 . . . C5 C6 H6 120 . . . N11 C12 H12 117 . . . C13 C12 H12 117 . . . C14 C13 H13 120 . . . C12 C13 H13 121 . . . C13 C14 H14 121 . . . C15 C14 H14 121 . . . C14 C15 H15 121 . . . C16 C15 H15 121 . . . H17a C17 H17b 109 . . . C16 C17 H17a 109 . . . N1 C17 H17a 109 . . . C16 C17 H17b 109 . . . N1 C17 H17b 109 . . . N21 C22 H22 119 . . . C23 C22 H22 119 . . . C22 C23 H23 120 . . . C24 C23 H23 120 . . . C23 C24 H24 121 . . . C25 C24 H24 121 . . . C24 C25 H25 120 . . . C26 C25 H25 120 . . . H27a C27 H27b 109 . . . C26 C27 H27a 109 . . . N1 C27 H27a 109 . . . C26 C27 H27b 109 . . . N1 C27 H27b 109 . . . N31 C32 H32 119 . . . C33 C32 H32 119 . . . C34 C33 H33 121 . . . C32 C33 H33 121 . . . C33 C34 H34 121 . . . C35 C34 H34 121 . . . C34 C35 H35 120 . . . C36 C35 H35 120 . . . H37a C37 H37b 109 . . . N2 C37 H37a 109 . . . C36 C37 H37a 109 . . . N2 C37 H37b 109 . . . C36 C37 H37b 109 . . . N41 C42 H42 118 . . . C43 C42 H42 118 . . . C44 C43 H43 121 . . . C42 C43 H43 121 . . . C43 C44 H44 120 . . . C45 C44 H44 120 . . . C46 C45 H45 121 . . . C44 C45 H45 121 . . . H47a C47 H47b 109 . . . C46 C47 H47a 108 . . . N2 C47 H47a 108 . . . C46 C47 H47b 108 . . . N2 C47 H47b 108 . . . N51 C52 H52 118 . . . C53 C52 H52 118 . . . C54 C53 H53 122 . . . C52 C53 H53 122 . . . C55 C54 H54 119 . . . C53 C54 H54 119 . . . C54 C55 H55 121 . . . C56 C55 H55 121 . . . N61 C62 H62 119 . . . C63 C62 H62 119 . . . C64 C63 H63 120 . . . C62 C63 H63 120 . . . C63 C64 H64 120 . . . C65 C64 H64 120 . . . C64 C65 H65 121 . . . C66 C65 H65 121 . . . H O H 123 . . 2_555 data_rucu-3a' _database_code_CSD 200508 _chemical_name_systematic ; ? ; _chemical_name_common ; (Cu2Ru(tpbd)2(H2O)4)(BF4)4(PF6)2,8H2O ; _chemical_formula_sum 'C60 H80 B4 Cu2 F28 N12 O12 P2 Ru' _chemical_formula_weight 2026.81 #=================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _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 30.059(6) _cell_length_b 17.996(4) _cell_length_c 20.338(4) _cell_angle_alpha 90.000 _cell_angle_beta 132.337(4) _cell_angle_gamma 90.000 _cell_volume 8132(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 19.5 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4096 _exptl_absorpt_coefficient_mu 0.868 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'XPREP, 1995' _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.90 #=================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation scans with narrow frames' _diffrn_reflns_number 55898 _diffrn_reflns_av_R_equivalents 0.132 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.3 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_reduction_process 55898 _reflns_number_total 9297 _reflns_number_gt 5037 _reflns_threshold_expression I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Altomare et al., 1997 ), KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #=================================== # 8. REFINEMENT DATA _refine_special_details ;Atomic displacement parameters for most atoms were kept isotropic. They cover disorder over different comformations, but no extra information could be gained from constrained refinement of two conformers obtained by splitting the worst afflicted atoms into two. The deepest holes as well as the biggest peak are found close to O3, a supposed water molecule on a position x,-y,z relative to the Cu-atom. Other peaks are found close to Cu, and most of the disorder concerns the ligands around copper. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w= 1/{8.0+[\s~cs~(F^2^)+1.10F^2^]^1/2^- |F|}^2^ ; _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5037 _refine_ls_number_parameters 348 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.21 _refine_ls_wR_factor_ref 0.28 _refine_ls_goodness_of_fit_ref 2.22 _refine_ls_shift/su_max 0.0011 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_max 1.5(2) _refine_diff_density_min -1.9(2) #========================================== # 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_thermal_displace_type Ru 0.0000 0.0170(2) 0.2500 0.019(3) Uij Cu 0.1573(2) 0.3148(2) 0.1400(3) 0.050(5) Uij P1 0.3282(5) 0.3980(7) 0.3145(7) 0.071(13) Uij F1 0.3760(12) 0.343(1) 0.388(1) 0.091(29) Uij F2 0.2804(9) 0.338(1) 0.263(2) 0.091(27) Uij F3 0.2769(10) 0.459(1) 0.236(1) 0.077(26) Uij F4 0.3766(9) 0.461(1) 0.357(1) 0.089(25) Uij F5 0.3497(11) 0.374(2) 0.260(2) 0.100(34) Uij F6 0.3082(10) 0.416(1) 0.366(1) 0.074(28) Uij F7 0.1354(20) -0.284(3) 0.014(2) 0.219(68) Uij F8 0.1473(14) -0.399(2) -0.024(3) 0.190(71) Uij F9 0.1025(15) -0.310(2) -0.115(2) 0.122(49) Uij F10 0.1896(13) -0.300(1) -0.024(2) 0.110(46) Uij F11 0.1723(23) -0.327(3) 0.384(2) 0.313(74) Uij F12 0.0713(17) -0.290(3) 0.303(2) 0.208(64) Uij F13 0.1245(24) -0.226(3) 0.336(2) 0.233(75) Uij F14 0.1013(14) -0.311(2) 0.243(1) 0.130(37) Uij O1 0.1670(10) 0.380(1) 0.072(1) 0.057(27) Uij O2 0.0562(9) 0.318(1) 0.023(1) 0.051(24) Uij N1 -0.0241(10) 0.094(1) 0.147(1) 0.031(5) Uiso N2 0.1771(11) 0.246(1) 0.243(2) 0.044(7) Uiso N11 -0.0057(9) -0.059(1) 0.168(1) 0.022(5) Uiso N21 -0.0922(10) 0.026(1) 0.170(1) 0.034(6) Uiso N31 0.1757(11) 0.221(1) 0.109(2) 0.041(6) Uiso N41 0.1520(15) 0.385(2) 0.199(2) 0.074(10) Uiso C1 0.025(2) 0.135(2) 0.170(2) 0.057(10) Uiso C2 0.026(2) 0.214(2) 0.170(2) 0.051(9) Uiso C3 0.080(2) 0.253(2) 0.200(2) 0.055(9) Uiso C4 0.127(1) 0.211(2) 0.215(2) 0.030(6) Uiso C5 0.117(1) 0.138(2) 0.198(2) 0.038(7) Uiso C6 0.069(1) 0.098(2) 0.178(2) 0.038(7) Uiso C12 0.010(1) -0.127(2) 0.183(2) 0.036(7) Uiso C13 0.009(1) -0.175(2) 0.124(2) 0.045(8) Uiso C14 -0.018(2) -0.146(2) 0.040(2) 0.055(9) Uiso C15 -0.039(1) -0.074(2) 0.020(2) 0.039(7) Uiso C16 -0.034(1) -0.029(2) 0.082(2) 0.038(7) Uiso C17 -0.055(1) 0.043(2) 0.066(2) 0.028(6) Uiso C22 -0.134(1) -0.021(2) 0.161(2) 0.048(8) Uiso C23 -0.183(1) 0.002(2) 0.119(2) 0.045(8) Uiso C24 -0.214(1) 0.061(2) 0.073(2) 0.043(8) Uiso C25 -0.172(1) 0.114(1) 0.082(2) 0.025(6) Uiso C26 -0.115(1) 0.090(2) 0.124(2) 0.035(7) Uiso C27 -0.071(1) 0.140(2) 0.131(2) 0.049(8) Uiso C32 0.158(2) 0.203(2) 0.031(2) 0.056(9) Uiso C33 0.172(2) 0.141(2) 0.018(3) 0.069(11) Uiso C34 0.201(2) 0.089(2) 0.077(2) 0.056(9) Uiso C35 0.223(2) 0.105(2) 0.159(2) 0.060(10) Uiso C36 0.207(1) 0.169(2) 0.175(2) 0.039(7) Uiso C37 0.226(1) 0.199(2) 0.261(2) 0.049(9) Uiso C42 0.134(2) 0.465(3) 0.171(3) 0.107(17) Uiso C43 0.138(2) 0.522(3) 0.224(4) 0.115(18) Uiso C44 0.152(2) 0.494(2) 0.306(2) 0.063(10) Uiso C45 0.174(2) 0.423(2) 0.333(2) 0.056(9) Uiso C46 0.175(2) 0.375(2) 0.287(2) 0.052(9) Uiso C47 0.202(4) 0.295(4) 0.318(4) 0.243(44) Uiso B1 0.147(2) -0.324(3) -0.029(3) 0.051(10) Uiso B2 0.125(3) -0.298(4) 0.319(4) 0.076(15) Uiso O3 0.353(1) 0.182(1) 0.336(2) 0.062(7) Uiso O4 0.244(2) -0.338(2) 0.560(2) 0.139(66) Uij O5 0.045(2) -0.398(2) 0.391(3) 0.168(94) Uij O6 0.025(2) -0.442(5) -0.169(4) 0.37(11) Uij H2 -0.008 0.242 0.150 0.06 Uiso H3 0.084 0.305 0.210 0.07 Uiso H5 0.145 0.111 0.199 0.05 Uiso H6 0.067 0.046 0.171 0.05 Uiso H12 0.025 -0.148 0.237 0.04 Uiso H13 0.024 -0.224 0.141 0.05 Uiso H14 -0.021 -0.176 -0.001 0.07 Uiso H15 -0.056 -0.053 -0.036 0.05 Uiso H17a -0.050 0.065 0.029 0.03 Uiso H17b -0.096 0.041 0.036 0.03 Uiso H22 -0.123 -0.068 0.187 0.06 Uiso H23 -0.207 -0.032 0.120 0.05 Uiso H24 -0.256 0.068 0.039 0.05 Uiso H25 -0.185 0.163 0.059 0.03 Uiso H27a -0.092 0.166 0.076 0.06 Uiso H27b -0.053 0.174 0.178 0.06 Uiso H32 0.133 0.238 -0.017 0.07 Uiso H33 0.161 0.133 -0.038 0.08 Uiso H34 0.207 0.041 0.063 0.07 Uiso H35 0.249 0.071 0.207 0.07 Uiso H37a 0.234 0.158 0.298 0.06 Uiso H37b 0.261 0.229 0.291 0.06 Uiso H42 0.119 0.479 0.114 0.13 Uiso H43 0.132 0.573 0.209 0.14 Uiso H44 0.146 0.524 0.338 0.08 Uiso H45 0.191 0.408 0.391 0.07 Uiso H47a 0.244 0.298 0.354 0.29 Uiso H47b 0.194 0.275 0.352 0.29 Uiso 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 Ru 0.017(1) 0.028(2) 0.013(1) 0.000 0.010(1) 0.000 Cu 0.049(3) 0.052(3) 0.044(2) -0.005(2) 0.030(2) -0.004(2) P1 0.079(8) 0.070(8) 0.059(7) -0.016(7) 0.045(6) -0.003(6) F1 0.114(20) 0.085(18) 0.040(12) 0.014(15) 0.039(13) 0.015(12) F2 0.043(12) 0.103(20) 0.080(15) -0.026(13) 0.022(12) -0.054(14) F3 0.093(17) 0.074(16) 0.038(11) 0.007(13) 0.034(12) 0.012(11) F4 0.053(13) 0.110(20) 0.057(13) -0.036(13) 0.018(11) 0.011(13) F5 0.092(18) 0.167(27) 0.084(16) -0.033(18) 0.076(16) -0.002(17) F6 0.107(18) 0.080(16) 0.049(12) -0.028(14) 0.058(13) -0.024(11) F7 0.292(48) 0.290(49) 0.084(20) 0.236(43) 0.130(28) 0.102(26) F8 0.102(23) 0.105(24) 0.346(54) 0.013(19) 0.143(32) 0.119(30) F9 0.161(30) 0.080(20) 0.132(25) 0.012(19) 0.101(24) -0.028(18) F10 0.132(25) 0.066(17) 0.157(26) 0.036(16) 0.107(23) 0.049(17) F11 0.289(54) 0.273(55) 0.073(21) 0.230(48) -0.002(28) -0.038(27) F12 0.114(29) 0.363(70) 0.122(28) 0.012(37) 0.069(25) 0.092(38) F13 0.278(57) 0.218(50) 0.057(19) -0.102(43) 0.054(28) 0.013(25) F14 0.146(26) 0.119(23) 0.040(13) 0.067(20) 0.028(15) -0.002(14) O1 0.049(14) 0.061(17) 0.059(14) 0.023(12) 0.035(13) 0.030(13) O2 0.042(13) 0.045(14) 0.055(14) -0.010(11) 0.029(12) -0.005(11) O4 0.234(45) 0.130(32) 0.106(26) 0.069(30) 0.136(32) 0.009(23) O5 0.302(61) 0.154(38) 0.191(42) 0.004(39) 0.224(48) 0.011(33) O6 0.134(43) 0.55(15) 0.218(55) 0.025(57) 0.032(40) -0.295(74) #================================= # 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 Ru N1 2.176(23) . . Ru N11 2.064(21) . . Ru N21 2.068(22) . . Cu N2 2.148(26) . . Cu N31 2.005(26) . . Cu N41 1.818(34) . . Cu O1 1.970(23) . . Cu O2 2.271(21) . . Cu F2 2.767(20) . . N1 C1 1.421(41) . . N1 C27 1.470(39) . . N1 C17 1.535(33) . . N2 C4 1.355(36) . . N2 C47 1.461(26) . . N2 C37 1.510(41) . . N11 C12 1.286(35) . . N11 C16 1.435(33) . . N21 C26 1.346(36) . . N21 C22 1.419(39) . . N31 C32 1.312(40) . . N31 C36 1.370(37) . . N41 C46 1.429(44) . . N41 C42 1.51(6) . . C1 C6 1.391(45) . . C1 C2 1.431(49) . . C2 C3 1.476(47) . . C3 C4 1.432(43) . . C4 C5 1.340(40) . . C5 C6 1.403(40) . . C12 C13 1.441(41) . . C13 C14 1.409(43) . . C14 C15 1.385(45) . . C15 C16 1.418(39) . . C16 C17 1.380(39) . . C22 C23 1.157(40) . . C23 C24 1.302(41) . . C24 C25 1.475(40) . . C25 C26 1.375(37) . . C26 C27 1.524(43) . . C32 C33 1.29(5) . . C33 C34 1.294(49) . . C34 C35 1.368(47) . . C35 C36 1.347(45) . . C36 C37 1.546(43) . . C42 C43 1.44(7) . . C43 C44 1.50(6) . . C44 C45 1.380(49) . . C45 C46 1.281(45) . . C46 C47 1.568(35) . . P1 F2 1.522(23) . . P1 F1 1.544(24) . . P1 F6 1.561(23) . . P1 F4 1.570(23) . . P1 F5 1.678(25) . . P1 F3 1.679(23) . . B1 F7 1.328(48) . . B1 F8 1.35(5) . . B1 F9 1.328(48) . . B1 F10 1.304(48) . . B2 F11 1.22(6) . . B2 F12 1.43(6) . . B2 F13 1.34(7) . . B2 F14 1.23(6) . . C2 H2 0.95 . . C3 H3 0.95 . . C5 H5 0.95 . . C6 H6 0.95 . . C12 H12 0.95 . . C13 H13 0.95 . . C14 H14 0.95 . . C15 H15 0.95 . . C17 H17a 0.95 . . C17 H17b 0.95 . . C22 H22 0.95 . . C23 H23 0.95 . . C24 H24 0.95 . . C25 H25 0.95 . . C27 H27b 0.95 . . C27 H27a 0.95 . . C32 H32 0.95 . . C33 H33 0.95 . . C34 H34 0.95 . . C35 H35 0.95 . . C37 H37a 0.95 . . C37 H37b 0.95 . . C42 H42 0.95 . . C43 H43 0.95 . . C44 H44 0.95 . . C45 H45 0.95 . . C47 H47a 0.95 . . C47 H47b 0.95 . . 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 N1 Ru N11 81.5(8) . . . N1 Ru N21 77.9(9) . . . N1 Ru N1 101.4(12) . . 4_555 N1 Ru N11 169.2(8) . . 4_555 N1 Ru N21 96.5(9) . . 4_555 N11 Ru N21 94.2(8) . . . N11 Ru N11 97.6(12) . . 4_555 N11 Ru N21 91.5(8) . . 4_555 N21 Ru N21 171.4(14) . . 4_555 N2 Cu N31 82.7(10) . . . N2 Cu N41 81.2(13) . . . O1 Cu N2 161.9(10) . . . O2 Cu N2 109.4(9) . . . F2 Cu N2 83.3(9) . . . N31 Cu N41 163.2(13) . . . O1 Cu N31 94.3(10) . . . O2 Cu N31 98.5(9) . . . F2 Cu N31 85.6(9) . . . O1 Cu N41 99.6(13) . . . O2 Cu N41 91.4(12) . . . F2 Cu N41 87.8(12) . . . O1 Cu O2 88.7(9) . . . F2 Cu O1 78.7(9) . . . F2 Cu O2 167.0(8) . . . C1 N1 C27 114.1(26) . . . C1 N1 C17 113.5(23) . . . Ru N1 C1 114.6(20) . . . C17 N1 C27 107.4(22) . . . Ru N1 C27 103.1(17) . . . Ru N1 C17 103.1(15) . . . C4 N2 C47 111.5(21) . . . C4 N2 C37 117.9(26) . . . Cu N2 C4 111.0(19) . . . C37 N2 C47 110.7(20) . . . Cu N2 C47 106.1(14) . . . Cu N2 C37 98.2(18) . . . C12 N11 C16 117.0(23) . . . Ru N11 C12 129.4(19) . . . Ru N11 C16 113.6(17) . . . C22 N21 C26 114.5(25) . . . Ru N21 C26 113.7(19) . . . Ru N21 C22 131.5(20) . . . C32 N31 C36 117.2(28) . . . Cu N31 C32 127.4(24) . . . Cu N31 C36 115.2(20) . . . C42 N41 C46 109.6(34) . . . Cu N41 C46 124.0(27) . . . Cu N41 C42 125.6(30) . . . N1 C1 C6 119.6(31) . . . C2 C1 C6 116.6(33) . . . N1 C1 C2 122.9(32) . . . C1 C2 C3 119.4(32) . . . C2 C3 C4 119.2(31) . . . C2 C3 C4 119.2(31) . . . N2 C4 C5 123.4(28) . . . C3 C4 C5 116.9(28) . . . N2 C4 C3 119.7(28) . . . C4 C5 C6 124.9(29) . . . C1 C6 C5 121.0(30) . . . N11 C12 C13 126.1(27) . . . C12 C13 C14 116.8(30) . . . C13 C14 C15 119.0(32) . . . C14 C15 C16 120.7(29) . . . C15 C16 C17 124.2(27) . . . N11 C16 C17 115.7(25) . . . N11 C16 C15 120.1(26) . . . N1 C17 C16 117.2(23) . . . N21 C22 C23 117.2(34) . . . C22 C23 C24 139(4) . . . C23 C24 C25 107.2(27) . . . C24 C25 C26 118.1(26) . . . N21 C26 C25 123.2(26) . . . N21 C26 C27 115.5(26) . . . C25 C26 C27 121.1(27) . . . N1 C27 C26 109.6(26) . . . N31 C32 C33 122(4) . . . C32 C33 C34 124(4) . . . C33 C34 C35 116(4) . . . C34 C35 C36 121(4) . . . N31 C36 C35 118.9(29) . . . C35 C36 C37 130.0(30) . . . N31 C36 C37 110.6(26) . . . N2 C37 C36 112.0(25) . . . N41 C42 C43 124(5) . . . C42 C43 C44 115(5) . . . C43 C44 C45 117(4) . . . C44 C45 C46 124(4) . . . N41 C46 C45 128(4) . . . C45 C46 C47 124.8(30) . . . N41 C46 C47 107.4(27) . . . N2 C47 C46 111.9(16) . . . F1 P1 F2 92.5(15) . . . F2 P1 F6 90.5(14) . . . F2 P1 F4 172.7(15) . . . F2 P1 F5 87.7(14) . . . F2 P1 F3 88.6(14) . . . F1 P1 F6 90.3(14) . . . F1 P1 F4 90.8(14) . . . F1 P1 F5 87.8(15) . . . F1 P1 F3 178.6(14) . . . F4 P1 F6 96.1(14) . . . F5 P1 F6 177.3(16) . . . F3 P1 F6 88.8(13) . . . F4 P1 F5 85.9(14) . . . F3 P1 F4 88.1(13) . . . F3 P1 F5 93.1(13) . . . F9 B1 F10 95(4) . . . F7 B1 F10 117(5) . . . F8 B1 F10 111(4) . . . F7 B1 F9 108(4) . . . F8 B1 F9 103(4) . . . F7 B1 F8 119(5) . . . F11 B2 F14 123(6) . . . F11 B2 F13 111(6) . . . F11 B2 F12 127(6) . . . F13 B2 F14 114(5) . . . F12 B2 F14 97(5) . . . F12 B2 F13 76(4) . . . C1 C2 H2 120 . . . C3 C2 H2 120 . . . C4 C3 H3 120 . . . C2 C3 H3 120 . . . C4 C5 H5 118 . . . C6 C5 H5 118 . . . C1 C6 H6 119 . . . C5 C6 H6 119 . . . N11 C12 H12 118 . . . C13 C12 H12 118 . . . C14 C13 H13 122 . . . C12 C13 H13 122 . . . C15 C14 H14 121 . . . C13 C14 H14 120 . . . C14 C15 H15 120 . . . C16 C15 H15 120 . . . H17a C17 H17b 110 . . . C16 C17 H17a 108 . . . N1 C17 H17a 108 . . . C16 C17 H17b 108 . . . N1 C17 H17b 108 . . . C23 C22 H22 121 . . . N21 C22 H22 121 . . . C22 C23 H23 110 . . . C24 C23 H23 110 . . . C23 C24 H24 126 . . . C25 C24 H24 126 . . . C26 C25 H25 121 . . . C24 C25 H25 121 . . . H27a C27 H27b 110 . . . N1 C27 H27b 109 . . . C26 C27 H27b 109 . . . N1 C27 H27a 109 . . . C26 C27 H27a 109 . . . C33 C32 H32 119 . . . N31 C32 H32 119 . . . C34 C33 H33 118 . . . C32 C33 H33 118 . . . C33 C34 H34 122 . . . C35 C34 H34 122 . . . C36 C35 H35 120 . . . C34 C35 H35 120 . . . H37a C37 H37b 110 . . . N2 C37 H37a 109 . . . C36 C37 H37a 109 . . . N2 C37 H37b 109 . . . C36 C37 H37b 109 . . . C43 C42 H42 118 . . . N41 C42 H42 118 . . . C42 C43 H43 123 . . . C44 C43 H43 123 . . . C45 C44 H44 121 . . . C43 C44 H44 121 . . . C46 C45 H45 118 . . . C44 C45 H45 118 . . . H47a C47 H47b 109 . . . N2 C47 H47a 109 . . . C46 C47 H47a 109 . . . N2 C47 H47b 109 . . . C46 C47 H47b 109 . . . #============================================================================== data_1 _database_code_CSD 200509 #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common (Ru(1,4-tppb)2)(PF6)2 _chemical_formula_sum 'C60 H56 F12 N12 P2 Ru' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety 'C60 H56 N12 Ru, 2(F6 P)' _chemical_formula_weight 1336.18 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d d ' _symmetry_space_group_name_Hall '-F 2uv 2vw' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 3/4-x,3/4-y,+z 3/4-x,+y,3/4-z +x,3/4-y,3/4-z -x,-y,-z 1/4+x,1/4+y,-z 1/4+x,-y,1/4+z -x,1/4+y,1/4+z +x,1/2+y,1/2+z 3/4-x,1/4-y,1/2+z 3/4-x,1/2+y,1/4-z +x,1/4-y,1/4-z -x,1/2-y,1/2-z 1/4+x,3/4+y,1/2-z 1/4+x,1/2-y,3/4+z -x,3/4+y,3/4+z 1/2+x,+y,1/2+z 1/4-x,3/4-y,1/2+z 1/4-x,+y,1/4-z 1/2+x,3/4-y,1/4-z 1/2-x,-y,1/2-z 3/4+x,1/4+y,1/2-z 3/4+x,-y,3/4+z 1/2-x,1/4+y,3/4+z 1/2+x,1/2+y,+z 1/4-x,1/4-y,+z 1/4-x,1/2+y,3/4-z 1/2+x,1/4-y,3/4-z 1/2-x,1/2-y,-z 3/4+x,3/4+y,-z 3/4+x,1/2-y,1/4+z 1/2-x,3/4+y,1/4+z _cell_length_a 25.578(1) _cell_length_b 27.030(1) _cell_length_c 35.028(2) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 24217(2) _cell_formula_units_Z 16 _cell_measurement_temperature 120 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 27.8 _exptl_crystal_description octahedron _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10912 _exptl_absorpt_coefficient_mu 0.399 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick,1996)' _exptl_absorpt_correction_T_min 0.636 _exptl_absorpt_correction_T_max 0.940 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames ' _diffrn_standards_decay_% 0 _diffrn_reflns_number 67793 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 27.8 _diffrn_reflns_reduction_process 67793 _reflns_number_total 6779 _reflns_number_gt 4565 _reflns_threshold_expression I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Altomare et al., 1997) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; 1/{[\s~cs~(F^2^)+B +(1 +A)F^2^]^1/2^-|F|}^2^ where A = 0.03, B = 3.0 ; _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4565 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.054 _refine_ls_wR_factor_ref 0.058 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_shift/su_max 0.0019 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_max 0.98(4) _refine_diff_density_min -0.62(4) #========================================== # 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_thermal_displace_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag Ru 0.87500 0.09938(2) 0.37500 0.0298(3) Uij 1. 16 d N11 0.9328(2) 0.1485(2) 0.3912(1) 0.042(2) Uij 1. 32 d C12 0.9391(3) 0.1951(2) 0.3776(2) 0.057(4) Uij 1. 32 d C13 0.9805(3) 0.2248(2) 0.3866(2) 0.079(6) Uij 1. 32 d C14 1.0180(3) 0.2068(3) 0.4112(3) 0.084(6) Uij 1. 32 d C15 1.0131(3) 0.1589(3) 0.4247(2) 0.066(5) Uij 1. 32 d C16 0.9706(2) 0.1309(2) 0.4141(1) 0.043(3) Uij 1. 32 d C17 0.9640(2) 0.0794(2) 0.4279(1) 0.040(3) Uij 1. 32 d N21 0.8462(2) 0.0931(2) 0.4306(1) 0.037(2) Uij 1. 32 d C22 0.8155(2) 0.1248(2) 0.4498(1) 0.047(3) Uij 1. 32 d C23 0.7954(3) 0.1138(2) 0.4855(2) 0.059(4) Uij 1. 32 d C24 0.8060(3) 0.0693(3) 0.5018(2) 0.056(4) Uij 1. 32 d C25 0.8383(2) 0.0365(2) 0.4829(2) 0.045(3) Uij 1. 32 d C26 0.8584(2) 0.0498(2) 0.4476(1) 0.036(3) Uij 1. 32 d C27 0.8958(2) 0.0173(2) 0.4265(1) 0.037(3) Uij 1. 32 d N31 1.1738(2) -0.0050(2) 0.2493(2) 0.071(4) Uij 1. 32 d C32 1.1836(3) 0.0250(3) 0.2196(3) 0.089(6) Uij 1. 32 d C33 1.1452(5) 0.0480(4) 0.1985(3) 0.100(7) Uij 1. 32 d C34 1.0943(4) 0.0393(4) 0.2079(3) 0.099(7) Uij 1. 32 d C35 1.0829(3) 0.0087(3) 0.2382(2) 0.073(5) Uij 1. 32 d C36 1.1233(3) -0.0122(2) 0.2582(2) 0.052(3) Uij 1. 32 d C37 1.1157(2) -0.0440(2) 0.2928(2) 0.055(4) Uij 1. 32 d N41 1.0428(2) -0.1905(2) 0.2720(1) 0.049(3) Uij 1. 32 d C42 1.0554(3) -0.2357(2) 0.2833(2) 0.055(4) Uij 1. 32 d C43 1.0839(3) -0.2457(2) 0.3158(2) 0.059(4) Uij 1. 32 d C44 1.1002(3) -0.2066(3) 0.3379(2) 0.061(4) Uij 1. 32 d C45 1.0869(2) -0.1593(2) 0.3268(2) 0.053(4) Uij 1. 32 d C46 1.0588(2) -0.1525(2) 0.2940(2) 0.045(3) Uij 1. 32 d C47 1.0432(2) -0.1020(2) 0.2793(2) 0.052(4) Uij 1. 32 d N1 0.9305(2) 0.0482(1) 0.4016(1) 0.033(2) Uij 1. 32 d N2 1.0625(2) -0.0599(2) 0.3007(1) 0.049(3) Uij 1. 32 d C1 0.9643(2) 0.0186(2) 0.3764(2) 0.034(3) Uij 1. 32 d C2 0.9585(2) -0.0321(2) 0.3713(2) 0.038(3) Uij 1. 32 d C3 0.9905(2) -0.0580(2) 0.3459(2) 0.042(3) Uij 1. 32 d C4 1.0303(2) -0.0340(2) 0.3257(1) 0.040(3) Uij 1. 32 d C5 1.0367(2) 0.0168(2) 0.3321(2) 0.042(3) Uij 1. 32 d C6 1.0044(2) 0.0420(2) 0.3565(2) 0.039(3) Uij 1. 32 d P1 0.87500 -0.12500 0.26800(8) 0.059(1) Uij 1. 16 d P2 1.23786(9) -0.12500 0.37500 0.052(1) Uij 1. 16 d F11 0.9079(4) -0.1516(3) 0.2946(3) 0.274(11) Uij 1. 32 d F12 0.9127(2) -0.0805(2) 0.2675(2) 0.158(6) Uij 1. 32 d F13 0.9058(4) -0.1508(3) 0.2390(3) 0.268(11) Uij 1. 32 d F21 1.2361(3) -0.1599(3) 0.3404(2) 0.179(6) Uij 1. 32 d F22 1.2783(5) -0.1556(3) 0.3867(4) 0.358(15) Uij 1. 32 d F23 1.2018(5) -0.0931(3) 0.3597(4) 0.356(15) Uij 1. 32 d H12 0.9133 0.2079 0.3608 0.069 Uiso 1. 32 c H13 0.9834 0.2571 0.3762 0.095 Uiso 1. 32 c H14 1.0467 0.2269 0.4187 0.101 Uiso 1. 32 c H15 1.0390 0.1454 0.4412 0.079 Uiso 1. 32 c H17a 0.9481 0.0802 0.4524 0.048 Uiso 1. 32 c H17b 0.9976 0.0645 0.4298 0.048 Uiso 1. 32 c H22 0.8073 0.1558 0.4385 0.057 Uiso 1. 32 c H23 0.7743 0.1373 0.4986 0.070 Uiso 1. 32 c H24 0.7914 0.0609 0.5259 0.068 Uiso 1. 32 c H25 0.8465 0.0053 0.4939 0.054 Uiso 1. 32 c H27a 0.8767 -0.0053 0.4111 0.044 Uiso 1. 32 c H27b 0.9166 -0.0005 0.4443 0.044 Uiso 1. 32 c H32 1.2190 0.0306 0.2128 0.107 Uiso 1. 32 c H33 1.1539 0.0694 0.1780 0.120 Uiso 1. 32 c H34 1.0669 0.0542 0.1937 0.119 Uiso 1. 32 c H35 1.0477 0.0020 0.2450 0.087 Uiso 1. 32 c H37a 1.1277 -0.0260 0.3143 0.066 Uiso 1. 32 c H37b 1.1364 -0.0729 0.2896 0.066 Uiso 1. 32 c H42 1.0441 -0.2628 0.2681 0.066 Uiso 1. 32 c H43 1.0920 -0.2787 0.3227 0.071 Uiso 1. 32 c H44 1.1203 -0.2121 0.3603 0.073 Uiso 1. 32 c H45 1.0971 -0.1317 0.3418 0.064 Uiso 1. 32 c H47a 1.0061 -0.1004 0.2793 0.063 Uiso 1. 32 c H47b 1.0557 -0.0990 0.2539 0.063 Uiso 1. 32 c H2 0.9325 -0.0494 0.3853 0.046 Uiso 1. 32 c H3 0.9852 -0.0924 0.3423 0.051 Uiso 1. 32 c H5 1.0638 0.0340 0.3192 0.050 Uiso 1. 32 c H6 1.0096 0.0765 0.3600 0.046 Uiso 1. 32 c 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 Ru 0.0357(3) 0.0247(3) 0.0290(3) 0.0000 -0.0015(3) 0.0000 N11 0.049(3) 0.033(2) 0.044(2) -0.003(2) -0.001(2) -0.004(2) C12 0.074(4) 0.033(3) 0.065(4) -0.008(3) -0.003(4) 0.002(3) C13 0.089(6) 0.043(4) 0.106(7) -0.026(4) -0.004(5) -0.002(4) C14 0.071(5) 0.067(5) 0.114(7) -0.036(4) -0.007(5) -0.018(5) C15 0.053(4) 0.070(5) 0.074(5) -0.014(4) -0.012(3) -0.012(4) C16 0.042(3) 0.045(3) 0.041(3) -0.004(3) -0.001(2) -0.011(3) C17 0.037(3) 0.053(3) 0.032(3) 0.000(3) -0.004(2) -0.006(2) N21 0.040(2) 0.035(2) 0.035(2) 0.000(2) 0.000(2) -0.006(2) C22 0.052(3) 0.043(3) 0.046(3) 0.010(3) 0.003(3) -0.011(3) C23 0.064(4) 0.063(5) 0.048(4) 0.008(3) 0.016(3) -0.023(3) C24 0.058(4) 0.076(5) 0.034(3) -0.004(4) 0.013(3) -0.004(3) C25 0.045(3) 0.057(4) 0.034(3) -0.002(3) 0.005(3) 0.003(3) C26 0.039(3) 0.036(3) 0.033(3) -0.001(2) -0.001(2) -0.001(2) C27 0.039(3) 0.036(3) 0.034(3) 0.002(2) 0.004(2) 0.006(2) N31 0.057(4) 0.079(4) 0.078(4) -0.004(3) 0.019(3) -0.001(3) C32 0.081(6) 0.088(6) 0.098(7) -0.020(5) 0.031(5) 0.003(5) C33 0.125(9) 0.096(7) 0.079(6) -0.012(6) 0.029(6) 0.020(5) C34 0.116(8) 0.106(7) 0.075(6) 0.000(6) -0.007(6) 0.027(5) C35 0.063(5) 0.092(6) 0.064(5) 0.004(4) 0.003(4) 0.016(4) C36 0.051(3) 0.057(4) 0.050(3) 0.004(4) 0.010(3) -0.006(3) C37 0.047(4) 0.062(4) 0.056(4) 0.009(3) 0.012(3) -0.001(3) N41 0.052(3) 0.051(3) 0.044(3) -0.001(2) 0.002(2) -0.005(2) C42 0.054(4) 0.054(4) 0.058(4) -0.009(3) 0.005(3) -0.003(3) C43 0.055(4) 0.059(4) 0.063(4) -0.005(3) 0.003(3) 0.012(3) C44 0.061(4) 0.071(5) 0.050(4) -0.003(4) -0.002(3) 0.011(3) C45 0.058(4) 0.060(4) 0.042(3) -0.003(3) 0.001(3) -0.006(3) C46 0.043(3) 0.054(4) 0.038(3) 0.004(3) 0.007(3) -0.005(3) C47 0.053(4) 0.056(4) 0.048(3) 0.012(3) 0.004(3) -0.009(3) N1 0.035(2) 0.033(2) 0.031(2) 0.001(2) 0.002(2) 0.000(2) N2 0.045(3) 0.048(3) 0.054(3) 0.006(2) 0.012(2) -0.011(2) C1 0.034(3) 0.036(3) 0.031(2) 0.004(2) -0.001(3) 0.002(3) C2 0.033(3) 0.037(3) 0.044(3) 0.003(2) 0.005(3) 0.004(3) C3 0.043(3) 0.036(3) 0.047(3) 0.002(3) 0.007(3) -0.002(3) C4 0.042(3) 0.042(3) 0.038(3) 0.007(3) 0.001(2) 0.001(2) C5 0.039(3) 0.046(3) 0.040(3) -0.004(3) 0.007(3) 0.002(3) C6 0.041(3) 0.033(3) 0.042(3) 0.001(2) 0.004(3) 0.000(2) P1 0.049(1) 0.037(1) 0.090(2) 0.004(1) 0.000 0.000 P2 0.057(1) 0.045(1) 0.053(1) 0.000 0.000 -0.001(1) F11 0.344(13) 0.127(6) 0.352(12) -0.056(6) -0.238(11) 0.118(7) F12 0.077(3) 0.057(3) 0.340(9) -0.021(3) -0.029(5) 0.014(4) F13 0.316(12) 0.121(6) 0.366(13) -0.035(6) 0.238(11) -0.073(7) F21 0.244(8) 0.177(6) 0.116(5) 0.066(6) -0.039(5) -0.097(5) F22 0.410(15) 0.192(8) 0.473(18) 0.118(9) -0.378(16) -0.066(11) F23 0.445(16) 0.248(10) 0.375(16) 0.242(11) -0.310(15) -0.142(11) #================================= # 10. MOLECULAR GEOMETRY # 3_655 1.750000 -1 0 0 0.000000 0 1 0 0.750000 0 0 -1 # 2_645 1.750000 -1 0 0 -0.250000 0 -1 0 0.000000 0 0 1 # 4_545 0.000000 1 0 0 -0.250000 0 -1 0 0.750000 0 0 -1 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 N11 2.066(4) . . yes Ru N11 2.066(4) . 3_655 yes Ru N21 2.088(4) . . yes Ru N21 2.088(4) . 3_655 yes Ru N1 2.191(4) . . yes Ru N1 2.191(4) . 3_655 yes N11 C16 1.345(6) . . no N11 C12 1.358(6) . . no C12 C13 1.365(8) . . no C13 C14 1.378(10) . . no C14 C15 1.386(9) . . no C15 C16 1.375(7) . . no C16 C17 1.484(7) . . no C17 N1 1.515(6) . . no N21 C22 1.345(6) . . no N21 C26 1.350(6) . . no C22 C23 1.387(7) . . no C23 C24 1.357(8) . . no C24 C25 1.381(7) . . no C25 C26 1.387(7) . . no C26 C27 1.493(6) . . no C27 N1 1.497(6) . . no N31 C32 1.340(9) . . no N31 C36 1.345(7) . . no C32 C33 1.378(11) . . no C33 C34 1.363(11) . . no C34 C35 1.376(9) . . no C35 C36 1.370(8) . . no C36 C37 1.497(7) . . no C37 N2 1.453(7) . . no N41 C42 1.325(7) . . no N41 C46 1.346(7) . . no C42 C43 1.377(8) . . no C43 C44 1.374(8) . . no C44 C45 1.379(8) . . no C45 C46 1.368(7) . . no C46 C47 1.513(7) . . no C47 N2 1.448(7) . . no N1 C1 1.472(6) . . no N2 C4 1.391(6) . . no C1 C2 1.391(6) . . no C1 C6 1.393(6) . . no C2 C3 1.395(7) . . no C3 C4 1.400(7) . . no C4 C5 1.400(7) . . no C5 C6 1.371(7) . . no P1 F11 1.448(6) . . no P1 F11 1.448(6) . 2_645 no P1 F12 1.541(4) . . no P1 F12 1.541(4) . 2_645 no P1 F13 1.463(6) . . no P1 F13 1.463(6) . 2_645 no P2 F21 1.536(4) . . no P2 F21 1.536(4) . 4_545 no P2 F22 1.388(7) . . no P2 F22 1.388(7) . 4_545 no P2 F23 1.371(6) . . no P2 F23 1.371(6) . 4_545 no C12 H12 0.950 . . no C13 H13 0.950 . . no C14 H14 0.950 . . no C15 H15 0.950 . . no C17 H17a 0.950 . . no C17 H17b 0.950 . . no C22 H22 0.950 . . no C23 H23 0.950 . . no C24 H24 0.950 . . no C25 H25 0.950 . . no C27 H27a 0.950 . . no C27 H27b 0.950 . . no C32 H32 0.950 . . no C33 H33 0.950 . . no C34 H34 0.950 . . no C35 H35 0.950 . . no C37 H37a 0.950 . . no C37 H37b 0.950 . . no C42 H42 0.950 . . no C43 H43 0.950 . . no C44 H44 0.950 . . no C45 H45 0.950 . . no C47 H47a 0.950 . . no C47 H47b 0.950 . . no C2 H2 0.950 . . no C3 H3 0.950 . . no C5 H5 0.950 . . no C6 H6 0.950 . . no 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 N11 Ru N11 100.0(2) . . 3_655 yes N11 Ru N21 92.8(2) . . . yes N11 Ru N21 93.3(2) . . 3_655 yes N11 Ru N1 80.0(2) . . . yes N11 Ru N1 170.5(2) . . 3_655 yes N11 Ru N21 93.3(2) 3_655 . . yes N11 Ru N21 92.8(2) 3_655 . 3_655 yes N11 Ru N1 170.5(1) 3_655 . . yes N11 Ru N1 80.0(2) 3_655 . 3_655 yes N21 Ru N21 170.6(2) . . 3_655 yes N21 Ru N1 77.2(1) . . . yes N21 Ru N1 96.7(1) . . 3_655 yes N21 Ru N1 96.7(1) 3_655 . . yes N21 Ru N1 77.2(1) 3_655 . 3_655 yes N1 Ru N1 101.6(2) . . 3_655 yes Ru N11 C12 125.9(4) . . . yes Ru N11 C16 116.9(3) . . . yes Ru N21 C22 128.3(3) . . . yes Ru N21 C26 113.7(3) . . . yes Ru N1 C1 117.9(3) . . . yes Ru N1 C17 105.9(3) . . . yes Ru N1 C27 102.5(3) . . . yes C12 N11 C16 116.8(5) . . . no N11 C12 C13 123.8(6) . . . no C12 C13 C14 118.6(6) . . . no C13 C14 C15 118.7(6) . . . no C14 C15 C16 119.5(6) . . . no N11 C16 C15 122.5(5) . . . no N11 C16 C17 116.3(4) . . . no C15 C16 C17 121.2(5) . . . no C16 C17 N1 113.0(4) . . . no C22 N21 C26 117.9(4) . . . no N21 C22 C23 122.1(5) . . . no C22 C23 C24 119.7(5) . . . no C23 C24 C25 119.2(5) . . . no C24 C25 C26 118.8(5) . . . no N21 C26 C25 122.2(5) . . . no N21 C26 C27 116.0(4) . . . no C25 C26 C27 121.8(4) . . . no C26 C27 N1 109.9(4) . . . no C32 N31 C36 116.6(6) . . . no N31 C32 C33 123.7(7) . . . no C32 C33 C34 118.4(8) . . . no C33 C34 C35 119.4(8) . . . no C34 C35 C36 118.9(7) . . . no N31 C36 C35 123.1(6) . . . no N31 C36 C37 113.3(5) . . . no C35 C36 C37 123.6(6) . . . no C36 C37 N2 116.5(5) . . . no C42 N41 C46 117.3(5) . . . no N41 C42 C43 123.7(6) . . . no C42 C43 C44 118.5(6) . . . no C43 C44 C45 118.5(6) . . . no C44 C45 C46 119.5(6) . . . no N41 C46 C45 122.5(5) . . . no N41 C46 C47 114.4(5) . . . no C45 C46 C47 123.1(5) . . . no C46 C47 N2 116.3(5) . . . no C27 N1 C1 113.2(3) . . . no C17 N1 C1 109.5(4) . . . no C17 N1 C27 107.1(3) . . . no C47 N2 C4 121.3(4) . . . no C37 N2 C4 121.7(4) . . . no C37 N2 C47 116.9(4) . . . no C2 C1 C6 117.4(4) . . . no N1 C1 C2 123.4(4) . . . no N1 C1 C6 119.1(4) . . . no C1 C2 C3 120.9(4) . . . no C2 C3 C4 121.2(5) . . . no N2 C4 C3 121.1(5) . . . no N2 C4 C5 121.7(5) . . . no C3 C4 C5 117.2(4) . . . no C4 C5 C6 121.2(4) . . . no C1 C6 C5 122.1(4) . . . no F11 P1 F11 99.7(11) . . 2_645 no F11 P1 F13 84.1(5) . . . no F11 P1 F13 176.1(9) . . 2_645 no F11 P1 F12 91.7(4) . . . no F11 P1 F12 89.0(4) . . 2_645 no F11 P1 F13 176.1(9) 2_645 . . no F11 P1 F13 84.1(5) 2_645 . 2_645 no F11 P1 F12 89.0(4) 2_645 . . no F11 P1 F12 91.7(4) 2_645 . 2_645 no F13 P1 F13 92.0(10) . . 2_645 no F12 P1 F13 91.5(4) . . . no F12 P1 F13 87.6(4) 2_645 . . no F12 P1 F13 87.6(4) . . 2_645 no F12 P1 F13 91.5(4) 2_645 . 2_645 no F12 P1 F12 178.8(6) . . 2_645 no F23 P2 F23 95.4(13) . . 4_545 no F22 P2 F23 172.9(11) . . . no F22 P2 F23 90.7(7) 4_545 . . no F21 P2 F23 93.3(4) . . . no F21 P2 F23 84.4(5) 4_545 . . no F22 P2 F23 90.7(7) . . 4_545 no F22 P2 F23 172.9(11) 4_545 . 4_545 no F21 P2 F23 84.4(5) . . 4_545 no F21 P2 F23 93.3(4) 4_545 . 4_545 no F22 P2 F22 83.5(12) . . 4_545 no F21 P2 F22 83.7(5) . . . no F21 P2 F22 98.9(5) 4_545 . . no F21 P2 F22 98.9(5) . . 4_545 no F21 P2 F22 83.7(5) 4_545 . 4_545 no F21 P2 F21 176.6(6) . . 4_545 no N11 C12 H12 118.1 . . . no C13 C12 H12 118.1 . . . no C12 C13 H13 120.7 . . . no C14 C13 H13 120.7 . . . no C13 C14 H14 120.6 . . . no C15 C14 H14 120.6 . . . no C16 C15 H15 120.2 . . . no C14 C15 H15 120.2 . . . no H17a C17 H17b 109.5 . . . no C16 C17 H17a 108.6 . . . no N1 C17 H17a 108.6 . . . no C16 C17 H17b 108.6 . . . no N1 C17 H17b 108.6 . . . no N21 C22 H22 119.0 . . . no C23 C22 H22 119.0 . . . no C24 C23 H23 120.2 . . . no C22 C23 H23 120.2 . . . no C23 C24 H24 120.4 . . . no C25 C24 H24 120.4 . . . no C24 C25 H25 120.6 . . . no C26 C25 H25 120.6 . . . no H27a C27 H27b 109.5 . . . no C26 C27 H27a 109.4 . . . no N1 C27 H27a 109.4 . . . no C26 C27 H27b 109.4 . . . no N1 C27 H27b 109.4 . . . no N31 C32 H32 118.2 . . . no C33 C32 H32 118.2 . . . no C34 C33 H33 120.8 . . . no C32 C33 H33 120.8 . . . no C33 C34 H34 120.3 . . . no C35 C34 H34 120.3 . . . no C36 C35 H35 120.5 . . . no C34 C35 H35 120.5 . . . no H37a C37 H37b 109.5 . . . no N2 C37 H37a 107.7 . . . no C36 C37 H37a 107.7 . . . no N2 C37 H37b 107.7 . . . no C36 C37 H37b 107.7 . . . no N41 C42 H42 118.1 . . . no C43 C42 H42 118.1 . . . no C44 C43 H43 120.7 . . . no C42 C43 H43 120.7 . . . no C43 C44 H44 120.8 . . . no C45 C44 H44 120.8 . . . no C46 C45 H45 120.3 . . . no C44 C45 H45 120.3 . . . no H47a C47 H47b 109.5 . . . no N2 C47 H47a 107.7 . . . no C46 C47 H47a 107.7 . . . no N2 C47 H47b 107.7 . . . no C46 C47 H47b 107.7 . . . no C1 C2 H2 119.5 . . . no C3 C2 H2 119.5 . . . no C2 C3 H3 119.4 . . . no C4 C3 H3 119.4 . . . no C6 C5 H5 119.4 . . . no C4 C5 H5 119.4 . . . no C5 C6 H6 119.0 . . . no C1 C6 H6 119.0 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 N1 N1 N2 117.5(1) . . 3_655 3_655 no