# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef 'publiEL11.cif' # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication in Chemical Communications ; _publ_contact_author ; Alain Igau ; _publ_contact_author_address ; Laboratoire de Chimie de Coordination 205 Route de Narbonne 31077 Toulouse Cedex 04 ; _publ_contact_author_email alain.igau@lcc-toulouse.fr #============================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ;Can a functionalized phosphine ligand promote room temperature luminescence of the [Ru(bpy)(tpy)]2+ core ? ; loop_ _publ_author_name _publ_author_address 'Emilie Lebon' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; "St\'ephanie Bastin" ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; 'Pierre Sutra' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; 'Laure Vendier' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; "R\'emi E. Piau" ; Laboratoire de Chimie et Physique Quantiques UMR 5626, IRSAMC CNRS et Universit\'e de Toulouse France ; 'Isabelle M. Dixon' ; Laboratoire de Chimie et Physique Quantiques UMR 5626, IRSAMC CNRS et Universit\'e de Toulouse France ; ; M.Boggio-Pasqua ; ; Laboratoire de Chimie et Physique Quantiques UMR 5626, IRSAMC CNRS et Universit\'e de Toulouse France ; 'Fabienne Alary' ; Laboratoire de Chimie et Physique Quantiques UMR 5626, IRSAMC CNRS et Universit\'e de Toulouse France ; 'Jean-Louis Heully' ; Laboratoire de Chimie et Physique Quantiques UMR 5626, IRSAMC CNRS et Universit\'e de Toulouse France ; 'Alain Igau' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; 'Alberto Juris' ; Dipartimento di Chimica "G. Ciamician" Universit\`a di Bologna via Selmi 2 40126 Bologna, Italy ; #============================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. and Camalli, M. (1994)., SIR92 program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of Crystal Structures. University of Gottingen, Germany. MULTI SCAN - c.f. r.h. blessing, acta cryst. (1995), a51, 33-38 WINGX - 1.63 Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-Ray Diffraction Data. Farrugia, L. J. Appl. Crystallogr., 1999, 32, 837. ORTEP3 for Windows, Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565. SQUEEZE - Sluis, P. v.d. and Spek, A. L. (1990) Acta Cryst. A46, 194-201. ; _publ_contact_author_name 'Alain Igau' #----------------------------------------------------------------------------# data_EL11 _database_code_depnum_ccdc_archive 'CCDC 836293' #TrackingRef 'publiEL11.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C38 H48 N7 P Ru, 2(F6 P)' _chemical_formula_sum 'C38 H48 F12 N7 P3 Ru' _chemical_formula_weight 1024.81 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.0299(8) _cell_length_b 17.0758(12) _cell_length_c 21.0409(12) _cell_angle_alpha 90 _cell_angle_beta 104.414(5) _cell_angle_gamma 90 _cell_volume 4534.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5690 _cell_measurement_theta_min 2.9927 _cell_measurement_theta_max 32.2079 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description stick _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.703 _exptl_absorpt_correction_T_max 0.918 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.1055 _diffrn_reflns_av_unetI/netI 0.1538 _diffrn_reflns_number 44527 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.1 _diffrn_reflns_theta_max 32.27 _diffrn_reflns_theta_full 32.27 _diffrn_measured_fraction_theta_full 0.931 _diffrn_measured_fraction_theta_max 0.931 _reflns_number_total 15022 _reflns_number_gt 7694 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 15022 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.112 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.334 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.123 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7419(3) 0.06250(18) 0.31164(17) 0.0244(7) Uani 1 1 d . . . H1 H 0.7375 0.0885 0.3508 0.029 Uiso 1 1 calc R . . C2 C 0.8486(3) -0.0110(2) 0.25192(18) 0.0358(9) Uani 1 1 d . . . H2 H 0.7816 -0.0045 0.2168 0.043 Uiso 1 1 calc R . . C3 C 0.9373(4) 0.0269(3) 0.2276(3) 0.0644(14) Uani 1 1 d . . . H3A H 0.9205 0.0822 0.2177 0.097 Uiso 1 1 calc R . . H3B H 0.9447 0.0001 0.1878 0.097 Uiso 1 1 calc R . . H3C H 1.0039 0.0229 0.2616 0.097 Uiso 1 1 calc R . . C4 C 0.8666(3) -0.0977(2) 0.2634(2) 0.0469(11) Uani 1 1 d . . . H4A H 0.9345 -0.1063 0.2953 0.07 Uiso 1 1 calc R . . H4B H 0.8675 -0.1235 0.2219 0.07 Uiso 1 1 calc R . . H4C H 0.8093 -0.1198 0.2804 0.07 Uiso 1 1 calc R . . C5 C 0.9205(3) 0.0266(2) 0.37153(19) 0.0360(9) Uani 1 1 d . . . H5 H 0.9828 0.0013 0.3602 0.043 Uiso 1 1 calc R . . C6 C 0.8897(4) -0.0249(2) 0.4231(2) 0.0537(12) Uani 1 1 d . . . H6A H 0.8364 0.0022 0.4407 0.081 Uiso 1 1 calc R . . H6B H 0.9526 -0.0354 0.4588 0.081 Uiso 1 1 calc R . . H6C H 0.8604 -0.0744 0.403 0.081 Uiso 1 1 calc R . . C7 C 0.9552(3) 0.1079(2) 0.3972(2) 0.0415(10) Uani 1 1 d . . . H7A H 0.9766 0.138 0.363 0.062 Uiso 1 1 calc R . . H7B H 1.0152 0.1037 0.4358 0.062 Uiso 1 1 calc R . . H7C H 0.8962 0.1345 0.4093 0.062 Uiso 1 1 calc R . . C8 C 0.5325(3) 0.18148(18) 0.20099(16) 0.0246(7) Uani 1 1 d . . . H8 H 0.4658 0.2113 0.1992 0.03 Uiso 1 1 calc R . . C9 C 0.5259(3) 0.15095(19) 0.13214(16) 0.0299(8) Uani 1 1 d . . . H9A H 0.5104 0.1945 0.1008 0.045 Uiso 1 1 calc R . . H9B H 0.4695 0.1117 0.1205 0.045 Uiso 1 1 calc R . . H9C H 0.5937 0.127 0.1308 0.045 Uiso 1 1 calc R . . C10 C 0.6238(3) 0.23944(19) 0.21880(19) 0.0351(9) Uani 1 1 d . . . H10A H 0.6912 0.2113 0.2252 0.053 Uiso 1 1 calc R . . H10B H 0.6215 0.2668 0.2594 0.053 Uiso 1 1 calc R . . H10C H 0.6175 0.2776 0.1833 0.053 Uiso 1 1 calc R . . C11 C 0.5620(3) 0.16422(18) 0.33939(16) 0.0249(7) Uani 1 1 d . . . H11 H 0.6303 0.1929 0.3438 0.03 Uiso 1 1 calc R . . C12 C 0.4763(3) 0.2269(2) 0.33368(19) 0.0360(9) Uani 1 1 d . . . H12A H 0.4068 0.2016 0.3268 0.054 Uiso 1 1 calc R . . H12B H 0.4766 0.2613 0.2965 0.054 Uiso 1 1 calc R . . H12C H 0.4904 0.2578 0.3741 0.054 Uiso 1 1 calc R . . C13 C 0.5738(3) 0.1176(2) 0.40252(16) 0.0347(9) Uani 1 1 d . . . H13A H 0.616 0.1477 0.4395 0.052 Uiso 1 1 calc R . . H13B H 0.6095 0.0678 0.3989 0.052 Uiso 1 1 calc R . . H13C H 0.5036 0.1071 0.4097 0.052 Uiso 1 1 calc R . . C21 C 0.2137(3) -0.09791(18) 0.24339(18) 0.0276(8) Uani 1 1 d . . . H21 H 0.2193 -0.0781 0.2863 0.033 Uiso 1 1 calc R . . C22 C 0.1320(3) -0.14774(19) 0.21658(19) 0.0330(9) Uani 1 1 d . . . H22 H 0.0827 -0.1622 0.241 0.04 Uiso 1 1 calc R . . C23 C 0.1215(3) -0.1768(2) 0.1546(2) 0.0365(9) Uani 1 1 d . . . H23 H 0.0642 -0.2105 0.1351 0.044 Uiso 1 1 calc R . . C24 C 0.1955(3) -0.15614(19) 0.12107(19) 0.0330(9) Uani 1 1 d . . . H24 H 0.1908 -0.1763 0.0784 0.04 Uiso 1 1 calc R . . C25 C 0.2782(3) -0.10505(18) 0.15028(16) 0.0238(7) Uani 1 1 d . . . C26 C 0.3651(3) -0.08493(18) 0.12116(16) 0.0252(7) Uani 1 1 d . . . C27 C 0.3735(3) -0.1159(2) 0.06125(17) 0.0348(9) Uani 1 1 d . . . H27 H 0.317 -0.1457 0.035 0.042 Uiso 1 1 calc R . . C28 C 0.4633(3) -0.1032(2) 0.04068(19) 0.0402(10) Uani 1 1 d . . . H28 H 0.4687 -0.1224 -0.0007 0.048 Uiso 1 1 calc R . . C29 C 0.5463(3) -0.0623(2) 0.08034(18) 0.0349(9) Uani 1 1 d . . . H29 H 0.6112 -0.0558 0.0681 0.042 Uiso 1 1 calc R . . C30 C 0.5327(3) -0.03124(18) 0.13815(17) 0.0264(8) Uani 1 1 d . . . H30 H 0.5895 -0.0024 0.1652 0.032 Uiso 1 1 calc R . . C31 C 0.5837(3) -0.10874(17) 0.30496(18) 0.0273(8) Uani 1 1 d . . . H31 H 0.6047 -0.1078 0.2648 0.033 Uiso 1 1 calc R . . C32 C 0.6384(3) -0.15514(19) 0.3557(2) 0.0359(9) Uani 1 1 d . . . H32 H 0.6965 -0.1855 0.35 0.043 Uiso 1 1 calc R . . C33 C 0.6101(3) -0.1581(2) 0.4143(2) 0.0403(10) Uani 1 1 d . . . H33 H 0.6479 -0.1902 0.4491 0.048 Uiso 1 1 calc R . . C34 C 0.5262(3) -0.11371(19) 0.42127(18) 0.0335(9) Uani 1 1 d . . . H34 H 0.504 -0.1154 0.461 0.04 Uiso 1 1 calc R . . C35 C 0.4738(3) -0.06610(18) 0.36993(16) 0.0243(7) Uani 1 1 d . . . C36 C 0.3875(3) -0.01257(18) 0.37439(16) 0.0230(7) Uani 1 1 d . . . C37 C 0.3420(3) -0.00388(19) 0.42649(17) 0.0303(8) Uani 1 1 d . . . H37 H 0.3652 -0.0351 0.4647 0.036 Uiso 1 1 calc R . . C38 C 0.2624(3) 0.0505(2) 0.42262(18) 0.0357(9) Uani 1 1 d . . . H38 H 0.2325 0.0583 0.459 0.043 Uiso 1 1 calc R . . C39 C 0.2264(3) 0.09346(19) 0.36624(17) 0.0291(8) Uani 1 1 d . . . H39 H 0.1703 0.13 0.363 0.035 Uiso 1 1 calc R . . C40 C 0.2725(3) 0.08300(17) 0.31434(16) 0.0225(7) Uani 1 1 d . . . C41 C 0.2387(2) 0.11850(17) 0.24913(16) 0.0203(7) Uani 1 1 d . . . C42 C 0.1584(3) 0.17315(19) 0.23240(18) 0.0295(8) Uani 1 1 d . . . H42 H 0.1258 0.1925 0.2649 0.035 Uiso 1 1 calc R . . C43 C 0.1256(3) 0.1994(2) 0.16944(19) 0.0331(9) Uani 1 1 d . . . H43 H 0.0696 0.2364 0.1576 0.04 Uiso 1 1 calc R . . C44 C 0.1749(3) 0.1716(2) 0.12318(18) 0.0318(8) Uani 1 1 d . . . H44 H 0.1532 0.1889 0.079 0.038 Uiso 1 1 calc R . . C45 C 0.2565(3) 0.11788(18) 0.14197(16) 0.0240(7) Uani 1 1 d . . . H45 H 0.2901 0.0987 0.1099 0.029 Uiso 1 1 calc R . . N1 N 0.2863(2) -0.07603(14) 0.21138(13) 0.0209(6) Uani 1 1 d . . . N2 N 0.4429(2) -0.03969(14) 0.15816(13) 0.0205(6) Uani 1 1 d . . . N3 N 0.3538(2) 0.03280(14) 0.31977(13) 0.0197(6) Uani 1 1 d . . . N4 N 0.5010(2) -0.06465(14) 0.31119(13) 0.0213(6) Uani 1 1 d . . . N5 N 0.28977(19) 0.09208(14) 0.20377(13) 0.0194(6) Uani 1 1 d . . . N6 N 0.6583(2) 0.06210(15) 0.26360(13) 0.0224(6) Uani 1 1 d . . . N7 N 0.8342(2) 0.02919(16) 0.31063(14) 0.0280(7) Uani 1 1 d . . . F1 F 0.12275(16) 0.27048(12) 0.36911(10) 0.0417(5) Uani 1 1 d . . . F2 F 0.28296(18) 0.33982(14) 0.49866(12) 0.0570(7) Uani 1 1 d . . . F3 F 0.1935(2) 0.22579(14) 0.47104(12) 0.0608(7) Uani 1 1 d . . . F4 F 0.2085(2) 0.38524(14) 0.39709(13) 0.0715(8) Uani 1 1 d . . . F5 F 0.29901(19) 0.27207(18) 0.41080(14) 0.0786(9) Uani 1 1 d . . . F6 F 0.10410(19) 0.33830(15) 0.45784(13) 0.0609(7) Uani 1 1 d . . . F7 F 0.8605(3) 0.2503(2) 0.6280(2) 0.1372(17) Uani 1 1 d . . . F8 F 0.8105(3) 0.12186(19) 0.52059(17) 0.0966(11) Uani 1 1 d . . . F9 F 0.9486(2) 0.1974(2) 0.56189(18) 0.1072(13) Uani 1 1 d . . . F10 F 0.7196(2) 0.17978(17) 0.58250(17) 0.0855(10) Uani 1 1 d . . . F11 F 0.8736(3) 0.1240(3) 0.6245(2) 0.1367(15) Uani 1 1 d . . . F12 F 0.7942(3) 0.2498(3) 0.5186(3) 0.191(3) Uani 1 1 d . . . P1 P 0.54263(6) 0.10383(5) 0.26392(4) 0.01888(18) Uani 1 1 d . . . P2 P 0.20283(8) 0.30574(6) 0.43423(5) 0.0353(2) Uani 1 1 d . . . P3 P 0.83282(9) 0.19133(7) 0.57097(6) 0.0456(3) Uani 1 1 d . . . Ru1 Ru 0.40771(2) 0.009020(13) 0.242966(13) 0.01753(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0221(17) 0.0267(18) 0.0243(19) -0.0009(13) 0.0057(14) -0.0023(14) C2 0.0246(19) 0.060(3) 0.024(2) -0.0065(17) 0.0085(15) 0.0072(18) C3 0.058(3) 0.084(3) 0.060(3) 0.005(3) 0.034(3) 0.004(3) C4 0.040(2) 0.057(3) 0.045(3) -0.013(2) 0.012(2) 0.007(2) C5 0.0205(18) 0.049(2) 0.033(2) -0.0010(17) -0.0023(16) 0.0026(16) C6 0.054(3) 0.056(3) 0.037(3) 0.010(2) -0.014(2) -0.003(2) C7 0.027(2) 0.051(2) 0.041(3) -0.0054(19) -0.0015(18) -0.0037(18) C8 0.0256(18) 0.0232(17) 0.0243(19) 0.0024(13) 0.0049(15) 0.0027(14) C9 0.041(2) 0.0270(18) 0.0231(19) 0.0042(14) 0.0107(17) 0.0004(16) C10 0.038(2) 0.0299(19) 0.039(2) 0.0043(16) 0.0109(18) -0.0082(16) C11 0.0248(18) 0.0269(17) 0.0230(19) -0.0080(13) 0.0058(14) -0.0060(14) C12 0.032(2) 0.038(2) 0.039(2) -0.0161(17) 0.0126(18) -0.0012(17) C13 0.039(2) 0.051(2) 0.0150(18) -0.0094(15) 0.0083(16) -0.0164(18) C21 0.0204(17) 0.0284(18) 0.036(2) -0.0014(15) 0.0112(16) 0.0000(14) C22 0.0192(18) 0.031(2) 0.049(3) -0.0012(17) 0.0087(17) -0.0043(15) C23 0.0238(19) 0.032(2) 0.049(3) -0.0070(17) -0.0001(18) -0.0051(16) C24 0.032(2) 0.034(2) 0.029(2) -0.0058(15) 0.0001(17) -0.0051(16) C25 0.0226(17) 0.0230(17) 0.0239(19) 0.0011(13) 0.0020(14) 0.0010(13) C26 0.0282(18) 0.0223(17) 0.0220(18) -0.0018(13) 0.0002(15) -0.0001(14) C27 0.040(2) 0.041(2) 0.022(2) -0.0076(15) 0.0056(17) -0.0052(17) C28 0.056(3) 0.043(2) 0.026(2) -0.0071(17) 0.018(2) 0.001(2) C29 0.038(2) 0.039(2) 0.032(2) -0.0022(16) 0.0184(18) 0.0061(17) C30 0.0299(19) 0.0255(17) 0.0253(19) -0.0035(14) 0.0098(15) 0.0017(14) C31 0.0230(18) 0.0201(17) 0.036(2) -0.0024(14) 0.0028(15) -0.0004(14) C32 0.0245(19) 0.0234(19) 0.053(3) 0.0022(17) -0.0031(18) 0.0049(15) C33 0.037(2) 0.030(2) 0.041(3) 0.0124(17) -0.0129(19) 0.0004(17) C34 0.039(2) 0.0312(19) 0.024(2) 0.0074(15) -0.0040(17) -0.0024(16) C35 0.0236(17) 0.0225(17) 0.0227(19) 0.0013(13) -0.0021(14) -0.0033(13) C36 0.0252(17) 0.0243(16) 0.0187(17) 0.0014(13) 0.0038(13) -0.0052(14) C37 0.037(2) 0.036(2) 0.0171(17) 0.0015(14) 0.0056(15) -0.0052(16) C38 0.044(2) 0.041(2) 0.028(2) -0.0064(16) 0.0200(19) -0.0062(18) C39 0.033(2) 0.0316(19) 0.027(2) -0.0015(15) 0.0157(16) 0.0028(15) C40 0.0226(17) 0.0215(16) 0.0242(18) -0.0033(13) 0.0075(14) -0.0013(13) C41 0.0162(15) 0.0208(16) 0.0226(18) -0.0008(13) 0.0024(13) -0.0011(12) C42 0.0257(18) 0.0300(19) 0.034(2) -0.0007(15) 0.0092(16) 0.0066(15) C43 0.0216(18) 0.033(2) 0.041(2) 0.0040(16) 0.0012(17) 0.0092(15) C44 0.0275(19) 0.036(2) 0.026(2) 0.0079(15) -0.0026(16) 0.0024(16) C45 0.0241(17) 0.0292(18) 0.0191(18) 0.0017(13) 0.0058(14) -0.0001(14) N1 0.0165(13) 0.0196(13) 0.0241(16) 0.0017(11) 0.0001(11) 0.0024(11) N2 0.0220(14) 0.0207(13) 0.0196(15) -0.0027(11) 0.0068(12) 0.0002(11) N3 0.0186(14) 0.0248(14) 0.0156(14) -0.0030(10) 0.0041(11) -0.0034(11) N4 0.0174(13) 0.0206(14) 0.0242(15) 0.0006(11) 0.0021(11) -0.0026(11) N5 0.0136(12) 0.0221(14) 0.0196(14) 0.0013(11) -0.0016(11) -0.0012(10) N6 0.0148(13) 0.0309(15) 0.0203(15) -0.0005(11) 0.0022(11) 0.0001(11) N7 0.0148(14) 0.0422(17) 0.0243(16) 0.0000(13) -0.0001(12) 0.0023(12) F1 0.0369(13) 0.0557(14) 0.0302(13) -0.0060(10) 0.0042(10) -0.0017(11) F2 0.0425(14) 0.0825(18) 0.0390(15) -0.0113(12) -0.0031(12) -0.0069(13) F3 0.0603(17) 0.0600(16) 0.0534(17) 0.0179(13) -0.0024(14) -0.0006(13) F4 0.099(2) 0.0553(16) 0.0521(18) 0.0082(13) 0.0034(16) -0.0180(15) F5 0.0305(14) 0.133(2) 0.079(2) -0.0387(18) 0.0255(14) -0.0005(15) F6 0.0432(15) 0.0851(18) 0.0528(17) -0.0194(13) 0.0090(13) 0.0178(13) F7 0.110(3) 0.166(3) 0.156(4) -0.105(3) 0.072(3) -0.072(3) F8 0.090(2) 0.113(2) 0.100(3) -0.052(2) 0.050(2) -0.042(2) F9 0.0507(19) 0.162(3) 0.114(3) -0.060(2) 0.030(2) -0.040(2) F10 0.0517(17) 0.089(2) 0.128(3) -0.0357(19) 0.0459(19) -0.0180(15) F11 0.132(4) 0.176(4) 0.093(3) 0.055(3) 0.011(3) 0.046(3) F12 0.137(4) 0.189(4) 0.245(6) 0.185(4) 0.043(4) 0.045(3) P1 0.0180(4) 0.0213(4) 0.0170(4) -0.0019(3) 0.0037(3) -0.0011(3) P2 0.0299(5) 0.0445(6) 0.0301(6) -0.0019(4) 0.0049(4) 0.0035(4) P3 0.0335(6) 0.0606(7) 0.0397(7) -0.0035(5) 0.0037(5) -0.0098(5) Ru1 0.01547(12) 0.02060(14) 0.01588(13) -0.00064(10) 0.00272(9) 0.00089(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N6 1.288(4) . ? C1 N7 1.335(4) . ? C1 H1 0.95 . ? C2 N7 1.465(4) . ? C2 C4 1.509(5) . ? C2 C3 1.521(6) . ? C2 H2 1 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 N7 1.480(4) . ? C5 C7 1.517(5) . ? C5 C6 1.527(6) . ? C5 H5 1 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C10 1.521(4) . ? C8 C9 1.522(4) . ? C8 P1 1.855(3) . ? C8 H8 1 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C13 1.524(5) . ? C11 C12 1.530(4) . ? C11 P1 1.857(3) . ? C11 H11 1 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C21 N1 1.343(4) . ? C21 C22 1.370(4) . ? C21 H21 0.95 . ? C22 C23 1.371(5) . ? C22 H22 0.95 . ? C23 C24 1.375(5) . ? C23 H23 0.95 . ? C24 C25 1.403(4) . ? C24 H24 0.95 . ? C25 N1 1.357(4) . ? C25 C26 1.457(5) . ? C26 N2 1.356(4) . ? C26 C27 1.397(5) . ? C27 C28 1.361(5) . ? C27 H27 0.95 . ? C28 C29 1.380(5) . ? C28 H28 0.95 . ? C29 C30 1.378(5) . ? C29 H29 0.95 . ? C30 N2 1.346(4) . ? C30 H30 0.95 . ? C31 N4 1.347(4) . ? C31 C32 1.377(5) . ? C31 H31 0.95 . ? C32 C33 1.373(5) . ? C32 H32 0.95 . ? C33 C34 1.368(5) . ? C33 H33 0.95 . ? C34 C35 1.388(4) . ? C34 H34 0.95 . ? C35 N4 1.368(4) . ? C35 C36 1.470(4) . ? C36 N3 1.365(4) . ? C36 C37 1.378(5) . ? C37 C38 1.379(5) . ? C37 H37 0.95 . ? C38 C39 1.374(5) . ? C38 H38 0.95 . ? C39 C40 1.383(4) . ? C39 H39 0.95 . ? C40 N3 1.346(4) . ? C40 C41 1.464(4) . ? C41 N5 1.369(4) . ? C41 C42 1.381(4) . ? C42 C43 1.363(5) . ? C42 H42 0.95 . ? C43 C44 1.377(5) . ? C43 H43 0.95 . ? C44 C45 1.385(4) . ? C44 H44 0.95 . ? C45 N5 1.339(4) . ? C45 H45 0.95 . ? N1 Ru1 2.129(3) . ? N2 Ru1 2.120(3) . ? N3 Ru1 1.958(3) . ? N4 Ru1 2.062(3) . ? N5 Ru1 2.103(2) . ? N6 P1 1.669(3) . ? F1 P2 1.618(2) . ? F2 P2 1.601(2) . ? F3 P2 1.589(2) . ? F4 P2 1.577(3) . ? F5 P2 1.566(3) . ? F6 P2 1.590(2) . ? F7 P3 1.539(3) . ? F8 P3 1.569(3) . ? F9 P3 1.570(3) . ? F10 P3 1.566(3) . ? F11 P3 1.605(4) . ? F12 P3 1.479(3) . ? P1 Ru1 2.3496(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 C1 N7 125.0(3) . . ? N6 C1 H1 117.5 . . ? N7 C1 H1 117.5 . . ? N7 C2 C4 111.8(3) . . ? N7 C2 C3 110.6(3) . . ? C4 C2 C3 111.8(3) . . ? N7 C2 H2 107.5 . . ? C4 C2 H2 107.5 . . ? C3 C2 H2 107.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N7 C5 C7 112.1(3) . . ? N7 C5 C6 110.8(3) . . ? C7 C5 C6 112.4(4) . . ? N7 C5 H5 107.1 . . ? C7 C5 H5 107.1 . . ? C6 C5 H5 107.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C9 108.2(3) . . ? C10 C8 P1 112.2(2) . . ? C9 C8 P1 114.3(2) . . ? C10 C8 H8 107.3 . . ? C9 C8 H8 107.3 . . ? P1 C8 H8 107.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 110.3(3) . . ? C13 C11 P1 114.7(2) . . ? C12 C11 P1 112.3(2) . . ? C13 C11 H11 106.3 . . ? C12 C11 H11 106.3 . . ? P1 C11 H11 106.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C21 C22 122.5(3) . . ? N1 C21 H21 118.7 . . ? C22 C21 H21 118.7 . . ? C21 C22 C23 120.0(4) . . ? C21 C22 H22 120 . . ? C23 C22 H22 120 . . ? C22 C23 C24 118.5(3) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C23 C24 C25 119.7(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? N1 C25 C24 120.8(3) . . ? N1 C25 C26 115.3(3) . . ? C24 C25 C26 123.7(3) . . ? N2 C26 C27 121.3(3) . . ? N2 C26 C25 116.2(3) . . ? C27 C26 C25 122.3(3) . . ? C28 C27 C26 119.6(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 119.6(3) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 118.3(4) . . ? C30 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? N2 C30 C29 123.2(3) . . ? N2 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? N4 C31 C32 121.2(4) . . ? N4 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? C33 C32 C31 121.0(4) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C34 C33 C32 118.5(3) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C33 C34 C35 119.5(4) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? N4 C35 C34 121.7(3) . . ? N4 C35 C36 114.9(3) . . ? C34 C35 C36 123.4(3) . . ? N3 C36 C37 119.8(3) . . ? N3 C36 C35 113.0(3) . . ? C37 C36 C35 127.2(3) . . ? C36 C37 C38 119.4(3) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 120.1(3) . . ? C39 C38 H38 120 . . ? C37 C38 H38 120 . . ? C38 C39 C40 119.4(3) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? N3 C40 C39 120.2(3) . . ? N3 C40 C41 113.0(3) . . ? C39 C40 C41 126.7(3) . . ? N5 C41 C42 120.9(3) . . ? N5 C41 C40 115.6(3) . . ? C42 C41 C40 123.4(3) . . ? C43 C42 C41 120.3(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 119.0(3) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.5 . . ? C43 C44 C45 119.1(3) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? N5 C45 C44 122.4(3) . . ? N5 C45 H45 118.8 . . ? C44 C45 H45 118.8 . . ? C21 N1 C25 118.4(3) . . ? C21 N1 Ru1 126.5(2) . . ? C25 N1 Ru1 114.9(2) . . ? C30 N2 C26 117.7(3) . . ? C30 N2 Ru1 127.5(2) . . ? C26 N2 Ru1 114.8(2) . . ? C40 N3 C36 121.0(3) . . ? C40 N3 Ru1 119.9(2) . . ? C36 N3 Ru1 118.1(2) . . ? C31 N4 C35 118.1(3) . . ? C31 N4 Ru1 128.3(2) . . ? C35 N4 Ru1 113.5(2) . . ? C45 N5 C41 118.2(3) . . ? C45 N5 Ru1 129.2(2) . . ? C41 N5 Ru1 112.5(2) . . ? C1 N6 P1 125.6(2) . . ? C1 N7 C2 121.2(3) . . ? C1 N7 C5 119.5(3) . . ? C2 N7 C5 119.1(3) . . ? N6 P1 C8 101.89(15) . . ? N6 P1 C11 108.05(14) . . ? C8 P1 C11 100.59(14) . . ? N6 P1 Ru1 109.84(9) . . ? C8 P1 Ru1 116.21(11) . . ? C11 P1 Ru1 118.63(11) . . ? F5 P2 F4 91.14(18) . . ? F5 P2 F3 90.13(16) . . ? F4 P2 F3 178.37(16) . . ? F5 P2 F6 178.88(16) . . ? F4 P2 F6 89.74(16) . . ? F3 P2 F6 88.97(15) . . ? F5 P2 F2 89.76(14) . . ? F4 P2 F2 90.32(14) . . ? F3 P2 F2 90.71(14) . . ? F6 P2 F2 90.92(13) . . ? F5 P2 F1 89.69(13) . . ? F4 P2 F1 90.05(13) . . ? F3 P2 F1 88.94(13) . . ? F6 P2 F1 89.62(12) . . ? F2 P2 F1 179.35(14) . . ? F12 P3 F7 96.3(3) . . ? F12 P3 F10 92.4(2) . . ? F7 P3 F10 90.48(19) . . ? F12 P3 F8 92.0(3) . . ? F7 P3 F8 171.7(3) . . ? F10 P3 F8 89.21(16) . . ? F12 P3 F9 91.3(2) . . ? F7 P3 F9 90.33(18) . . ? F10 P3 F9 176.1(2) . . ? F8 P3 F9 89.43(17) . . ? F12 P3 F11 176.6(3) . . ? F7 P3 F11 87.1(3) . . ? F10 P3 F11 87.8(2) . . ? F8 P3 F11 84.6(2) . . ? F9 P3 F11 88.4(2) . . ? N3 Ru1 N4 79.77(11) . . ? N3 Ru1 N5 78.86(10) . . ? N4 Ru1 N5 158.61(11) . . ? N3 Ru1 N2 166.72(10) . . ? N4 Ru1 N2 97.64(10) . . ? N5 Ru1 N2 102.99(10) . . ? N3 Ru1 N1 90.45(10) . . ? N4 Ru1 N1 93.71(9) . . ? N5 Ru1 N1 85.64(9) . . ? N2 Ru1 N1 76.66(10) . . ? N3 Ru1 P1 96.17(8) . . ? N4 Ru1 P1 90.33(7) . . ? N5 Ru1 P1 92.78(7) . . ? N2 Ru1 P1 96.87(7) . . ? N1 Ru1 P1 172.77(8) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'publiEL16bBisN.cif' data_el16b _database_code_depnum_ccdc_archive 'CCDC 836294' #TrackingRef 'publiEL16bBisN.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C44 H44 N7 P Ru, 2(F6 P)' _chemical_formula_sum 'C44 H44 F12 N7 P3 Ru' _chemical_formula_weight 1092.84 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.2051(17) _cell_length_b 14.2527(8) _cell_length_c 23.982(2) _cell_angle_alpha 90 _cell_angle_beta 99.011(12) _cell_angle_gamma 90 _cell_volume 5808.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.025 _exptl_crystal_density_diffrn 1.25 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.931 _exptl_absorpt_correction_T_max 0.987 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 4 _diffrn_standards_decay_% 0.1 _diffrn_reflns_av_R_equivalents 0.082 _diffrn_reflns_av_unetI/netI 0.1099 _diffrn_reflns_number 44287 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 11025 _reflns_number_gt 5275 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0844P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11025 _refine_ls_number_parameters 609 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 0.817 _refine_ls_restrained_S_all 0.818 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.61 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.086 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1655(3) 0.2985(4) 0.7305(3) 0.0597(14) Uani 1 1 d . . . H1 H 1.1569 0.3292 0.6949 0.072 Uiso 1 1 calc R . . C14 C 1.0196(3) 0.3709(4) 0.6601(2) 0.0554(13) Uani 1 1 d . . . C19 C 1.0098(3) 0.4657(4) 0.6716(3) 0.0610(14) Uani 1 1 d . . . H19 H 0.9947 0.4839 0.7065 0.073 Uiso 1 1 calc R . . C18 C 1.0220(4) 0.5339(4) 0.6325(3) 0.0793(18) Uani 1 1 d . . . H18 H 1.0158 0.5983 0.6409 0.095 Uiso 1 1 calc R . . C17 C 1.0428(5) 0.5083(5) 0.5818(3) 0.100(2) Uani 1 1 d . . . H17 H 1.0496 0.555 0.5547 0.12 Uiso 1 1 calc R . . C16 C 1.0538(5) 0.4147(5) 0.5699(3) 0.095(2) Uani 1 1 d . . . H16 H 1.0703 0.3973 0.5353 0.114 Uiso 1 1 calc R . . C15 C 1.0409(3) 0.3467(4) 0.6082(2) 0.0689(16) Uani 1 1 d . . . H15 H 1.0465 0.2824 0.5991 0.083 Uiso 1 1 calc R . . C8 C 0.9949(3) 0.1751(3) 0.6768(2) 0.0513(13) Uani 1 1 d . . . C13 C 0.9332(3) 0.1670(4) 0.6323(2) 0.0594(14) Uani 1 1 d . . . H13 H 0.9053 0.2216 0.6181 0.071 Uiso 1 1 calc R . . C12 C 0.9117(4) 0.0804(5) 0.6084(3) 0.088(2) Uani 1 1 d . . . H12 H 0.871 0.0759 0.5769 0.105 Uiso 1 1 calc R . . C11 C 0.9510(6) -0.0007(5) 0.6316(4) 0.103(3) Uani 1 1 d . . . H11 H 0.9347 -0.0609 0.6173 0.124 Uiso 1 1 calc R . . C10 C 1.0112(5) 0.0075(5) 0.6736(4) 0.100(3) Uani 1 1 d . . . H10 H 1.0391 -0.047 0.6879 0.12 Uiso 1 1 calc R . . C9 C 1.0335(3) 0.0934(4) 0.6967(3) 0.0689(16) Uani 1 1 d . . . H9 H 1.0764 0.097 0.7268 0.083 Uiso 1 1 calc R . . C45 C 0.8374(3) 0.4686(4) 0.7062(2) 0.0590(14) Uani 1 1 d . . . H45 H 0.8729 0.5108 0.7277 0.071 Uiso 1 1 calc R . . C44 C 0.7827(3) 0.5041(4) 0.6638(3) 0.0699(16) Uani 1 1 d . . . H44 H 0.7816 0.5694 0.6557 0.084 Uiso 1 1 calc R . . C43 C 0.7294(3) 0.4449(5) 0.6329(3) 0.0767(18) Uani 1 1 d . . . H43 H 0.6909 0.4684 0.6035 0.092 Uiso 1 1 calc R . . C42 C 0.7332(3) 0.3496(5) 0.6456(2) 0.0664(15) Uani 1 1 d . . . H42 H 0.6966 0.3074 0.6251 0.08 Uiso 1 1 calc R . . C41 C 0.7896(3) 0.3165(4) 0.6879(2) 0.0497(12) Uani 1 1 d . . . C40 C 0.7983(3) 0.2179(4) 0.7032(2) 0.0501(13) Uani 1 1 d . . . C39 C 0.7507(3) 0.1426(4) 0.6805(2) 0.0603(14) Uani 1 1 d . . . H39 H 0.7057 0.1537 0.6529 0.072 Uiso 1 1 calc R . . C38 C 0.7695(4) 0.0541(4) 0.6984(3) 0.0683(16) Uani 1 1 d . . . H38 H 0.7383 0.0029 0.6824 0.082 Uiso 1 1 calc R . . C37 C 0.8335(3) 0.0377(4) 0.7397(3) 0.0636(15) Uani 1 1 d . . . H37 H 0.8467 -0.0243 0.7522 0.076 Uiso 1 1 calc R . . C36 C 0.8780(3) 0.1130(3) 0.7624(2) 0.0501(12) Uani 1 1 d . . . C35 C 0.9466(3) 0.1090(3) 0.8085(2) 0.0525(12) Uani 1 1 d . . . C34 C 0.9768(4) 0.0273(4) 0.8342(3) 0.0698(16) Uani 1 1 d . . . H34 H 0.953 -0.0314 0.8233 0.084 Uiso 1 1 calc R . . C33 C 1.0412(4) 0.0314(5) 0.8755(3) 0.0825(19) Uani 1 1 d . . . H33 H 1.0626 -0.0243 0.8935 0.099 Uiso 1 1 calc R . . C32 C 1.0747(4) 0.1169(5) 0.8909(3) 0.0790(18) Uani 1 1 d . . . H32 H 1.1197 0.1207 0.9193 0.095 Uiso 1 1 calc R . . C31 C 1.0427(3) 0.1967(4) 0.8649(2) 0.0642(14) Uani 1 1 d . . . H31 H 1.0658 0.2556 0.8762 0.077 Uiso 1 1 calc R . . C21 C 0.7811(3) 0.2887(4) 0.8400(2) 0.0586(14) Uani 1 1 d . . . H21 H 0.7629 0.2439 0.8116 0.07 Uiso 1 1 calc R . . C22 C 0.7342(3) 0.3082(5) 0.8810(2) 0.0689(15) Uani 1 1 d . . . H22 H 0.6854 0.2771 0.8808 0.083 Uiso 1 1 calc R . . C23 C 0.7605(4) 0.3729(5) 0.9211(3) 0.0801(19) Uani 1 1 d . . . H23 H 0.73 0.3869 0.9498 0.096 Uiso 1 1 calc R . . C24 C 0.8316(4) 0.4188(5) 0.9205(2) 0.0761(18) Uani 1 1 d . . . H24 H 0.8498 0.4645 0.9483 0.091 Uiso 1 1 calc R . . C25 C 0.8756(3) 0.3967(4) 0.8784(2) 0.0609(15) Uani 1 1 d . . . C26 C 0.9494(3) 0.4420(4) 0.8725(2) 0.0602(14) Uani 1 1 d . . . C27 C 0.9840(4) 0.5129(5) 0.9098(3) 0.083(2) Uani 1 1 d . . . H27 H 0.9583 0.5346 0.9396 0.1 Uiso 1 1 calc R . . C28 C 1.0551(5) 0.5494(5) 0.9021(4) 0.100(3) Uani 1 1 d . . . H28 H 1.0796 0.5959 0.9272 0.12 Uiso 1 1 calc R . . C29 C 1.0905(4) 0.5196(4) 0.8590(3) 0.082(2) Uani 1 1 d . . . H29 H 1.1399 0.5446 0.8535 0.098 Uiso 1 1 calc R . . C30 C 1.0539(3) 0.4529(4) 0.8235(3) 0.0698(16) Uani 1 1 d . . . H30 H 1.0796 0.4325 0.7934 0.084 Uiso 1 1 calc R . . N6 N 1.1052(2) 0.2718(4) 0.7492(2) 0.0677(13) Uani 1 1 d . . . N5 N 0.8428(2) 0.3761(3) 0.71861(17) 0.0485(10) Uani 1 1 d . . . N3 N 0.8606(2) 0.2006(3) 0.74350(16) 0.0434(9) Uani 1 1 d . . . N4 N 0.9797(2) 0.1946(3) 0.82411(17) 0.0500(9) Uani 1 1 d . . . N1 N 0.8507(2) 0.3304(3) 0.83890(16) 0.0481(10) Uani 1 1 d . . . N2 N 0.9842(2) 0.4142(3) 0.82815(18) 0.0540(11) Uani 1 1 d . . . F1 F 0.8880(3) 0.6803(3) 0.7124(3) 0.148(2) Uani 1 1 d . . . F2 F 1.0059(3) 0.7963(4) 0.7957(3) 0.172(3) Uani 1 1 d . . . F3 F 0.9729(4) 0.7910(4) 0.7053(3) 0.189(3) Uani 1 1 d . . . F4 F 1.0135(3) 0.6641(3) 0.7519(2) 0.1309(17) Uani 1 1 d . . . F5 F 0.8805(2) 0.8105(3) 0.7580(3) 0.146(2) Uani 1 1 d . . . F6 F 0.9229(3) 0.6791(6) 0.8033(3) 0.192(3) Uani 1 1 d . . . F7 F 1.1676(6) 0.2228(5) 1.0076(3) 0.230(4) Uani 1 1 d . . . F8 F 1.2160(5) 0.4332(6) 0.9851(3) 0.196(3) Uani 1 1 d . . . F9 F 1.1887(4) 0.3034(6) 0.9339(3) 0.209(4) Uani 1 1 d . . . F10 F 1.1818(9) 0.3526(5) 1.0558(3) 0.334(8) Uani 1 1 d . . . F11 F 1.1042(5) 0.3542(6) 0.9787(3) 0.211(3) Uani 1 1 d . . . F12 F 1.2770(6) 0.3019(7) 1.0117(7) 0.425(11) Uani 1 1 d . . . P1 P 1.01397(7) 0.28448(9) 0.71562(6) 0.0484(3) Uani 1 1 d . . . P2 P 0.94738(9) 0.73754(11) 0.75498(9) 0.0726(5) Uani 1 1 d . . . P3 P 1.1947(2) 0.3280(2) 0.99494(11) 0.1622(15) Uani 1 1 d . . . Ru1 Ru 0.92475(2) 0.30573(3) 0.777980(17) 0.04392(13) Uani 1 1 d . . . C2 C 1.3049(4) 0.3191(7) 0.7233(4) 0.110(3) Uani 1 1 d D . . H2 H 1.3559 0.2982 0.7457 0.132 Uiso 1 1 calc R A 1 C4A C 1.3058(10) 0.2935(12) 0.6637(5) 0.137(4) Uani 0.58 1 d PD B 1 H4A1 H 1.2611 0.3231 0.6398 0.206 Uiso 0.58 1 calc PR B 1 H4A2 H 1.3019 0.2252 0.6596 0.206 Uiso 0.58 1 calc PR B 1 H4A3 H 1.355 0.3153 0.6523 0.206 Uiso 0.58 1 calc PR B 1 C3A C 1.3043(12) 0.4213(8) 0.7229(7) 0.137(4) Uani 0.58 1 d PD B 1 H3A1 H 1.3539 0.4445 0.7129 0.206 Uiso 0.58 1 calc PR B 1 H3A2 H 1.2984 0.4445 0.7605 0.206 Uiso 0.58 1 calc PR B 1 H3A3 H 1.2603 0.4437 0.6952 0.206 Uiso 0.58 1 calc PR B 1 C4B C 1.2967(15) 0.2429(12) 0.6811(8) 0.137(4) Uani 0.42 1 d PD B 2 H4B1 H 1.2519 0.2561 0.6516 0.206 Uiso 0.42 1 calc PR B 2 H4B2 H 1.2879 0.1833 0.6995 0.206 Uiso 0.42 1 calc PR B 2 H4B3 H 1.3449 0.2386 0.6642 0.206 Uiso 0.42 1 calc PR B 2 C3B C 1.3090(17) 0.4072(10) 0.6950(10) 0.137(4) Uani 0.42 1 d PD B 2 H3B1 H 1.2963 0.4582 0.7195 0.206 Uiso 0.42 1 calc PR B 2 H3B2 H 1.2713 0.4073 0.6599 0.206 Uiso 0.42 1 calc PR B 2 H3B3 H 1.3623 0.4163 0.6863 0.206 Uiso 0.42 1 calc PR B 2 N7 N 1.2398(2) 0.2888(3) 0.7545(2) 0.0715(14) Uani 1 1 d . B . C5A C 1.2585(10) 0.2079(15) 0.7975(9) 0.143(4) Uani 0.46 1 d PD B 1 H5A H 1.2095 0.1874 0.8116 0.172 Uiso 0.46 1 calc PR B 1 C6A C 1.3177(10) 0.2388(17) 0.8449(7) 0.143(4) Uani 0.46 1 d PD B 1 H6A1 H 1.3316 0.1863 0.8709 0.215 Uiso 0.46 1 calc PR B 1 H6A2 H 1.2962 0.2903 0.8649 0.215 Uiso 0.46 1 calc PR B 1 H6A3 H 1.3648 0.2606 0.8305 0.215 Uiso 0.46 1 calc PR B 1 C7A C 1.2959(10) 0.1281(14) 0.7746(8) 0.143(4) Uani 0.46 1 d PD B 1 H7A1 H 1.3502 0.1445 0.7707 0.215 Uiso 0.46 1 calc PR B 1 H7A2 H 1.2666 0.1118 0.7374 0.215 Uiso 0.46 1 calc PR B 1 H7A3 H 1.2962 0.0744 0.8001 0.215 Uiso 0.46 1 calc PR B 1 C5B C 1.2570(9) 0.2720(11) 0.8143(8) 0.143(4) Uani 0.54 1 d PD B 2 H5B H 1.2055 0.2778 0.8283 0.172 Uiso 0.54 1 calc PR B 2 C6B C 1.3087(8) 0.3419(12) 0.8458(7) 0.143(4) Uani 0.54 1 d PD B 2 H6B1 H 1.3627 0.3178 0.8527 0.215 Uiso 0.54 1 calc PR B 2 H6B2 H 1.2908 0.3546 0.8819 0.215 Uiso 0.54 1 calc PR B 2 H6B3 H 1.3071 0.4 0.8238 0.215 Uiso 0.54 1 calc PR B 2 C7B C 1.2871(9) 0.1797(11) 0.8320(9) 0.143(4) Uani 0.54 1 d PD B 2 H7B1 H 1.2535 0.1315 0.8116 0.215 Uiso 0.54 1 calc PR B 2 H7B2 H 1.2872 0.1724 0.8727 0.215 Uiso 0.54 1 calc PR B 2 H7B3 H 1.3409 0.1731 0.8239 0.215 Uiso 0.54 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(3) 0.053(3) 0.081(4) -0.004(3) 0.006(3) 0.002(3) C14 0.050(3) 0.051(3) 0.066(4) 0.004(3) 0.008(3) -0.012(2) C19 0.055(3) 0.055(3) 0.072(4) 0.008(3) 0.008(3) -0.004(3) C18 0.090(5) 0.060(4) 0.085(5) 0.008(4) 0.005(4) -0.012(3) C17 0.135(7) 0.083(5) 0.077(5) 0.024(4) 0.002(5) -0.031(5) C16 0.126(6) 0.086(5) 0.074(5) 0.006(4) 0.021(4) -0.021(4) C15 0.085(4) 0.065(3) 0.059(4) 0.001(3) 0.018(3) -0.014(3) C8 0.047(3) 0.049(3) 0.063(3) -0.003(3) 0.022(2) 0.000(2) C13 0.060(3) 0.065(4) 0.059(3) -0.013(3) 0.023(3) -0.008(3) C12 0.080(4) 0.095(5) 0.098(5) -0.038(4) 0.044(4) -0.029(4) C11 0.110(6) 0.073(5) 0.143(8) -0.050(5) 0.070(6) -0.015(5) C10 0.089(5) 0.059(4) 0.168(9) -0.007(5) 0.070(6) 0.007(4) C9 0.061(3) 0.057(4) 0.095(5) 0.000(3) 0.032(3) 0.010(3) C45 0.055(3) 0.057(3) 0.066(4) 0.007(3) 0.012(3) 0.010(3) C44 0.069(4) 0.068(4) 0.071(4) 0.016(3) 0.006(3) 0.018(3) C43 0.057(4) 0.105(5) 0.065(4) 0.014(4) 0.003(3) 0.020(4) C42 0.048(3) 0.087(4) 0.063(4) -0.006(3) 0.004(3) 0.003(3) C41 0.039(2) 0.065(3) 0.046(3) -0.002(3) 0.009(2) 0.004(2) C40 0.039(3) 0.063(3) 0.052(3) -0.010(3) 0.018(2) 0.001(2) C39 0.046(3) 0.075(4) 0.060(4) -0.015(3) 0.009(3) -0.017(3) C38 0.071(4) 0.069(4) 0.066(4) -0.018(3) 0.013(3) -0.029(3) C37 0.075(4) 0.050(3) 0.071(4) -0.011(3) 0.028(3) -0.017(3) C36 0.048(3) 0.052(3) 0.054(3) -0.006(3) 0.018(2) -0.001(2) C35 0.059(3) 0.046(3) 0.055(3) 0.000(3) 0.015(3) 0.001(2) C34 0.088(4) 0.049(3) 0.073(4) 0.004(3) 0.015(4) 0.003(3) C33 0.094(5) 0.060(4) 0.090(5) 0.017(4) 0.002(4) 0.022(4) C32 0.076(4) 0.078(4) 0.075(4) 0.010(4) -0.011(3) 0.017(3) C31 0.061(3) 0.064(3) 0.062(3) -0.002(3) -0.007(3) 0.002(3) C21 0.063(3) 0.058(3) 0.056(3) -0.002(3) 0.013(3) 0.004(3) C22 0.064(3) 0.080(4) 0.066(4) -0.005(4) 0.022(3) 0.012(3) C23 0.084(5) 0.094(5) 0.065(4) 0.003(4) 0.020(3) 0.031(4) C24 0.090(5) 0.084(4) 0.053(4) -0.012(3) 0.008(3) 0.026(4) C25 0.065(3) 0.056(3) 0.055(3) -0.003(3) -0.012(3) 0.022(3) C26 0.061(3) 0.048(3) 0.065(4) -0.008(3) -0.012(3) 0.008(3) C27 0.091(5) 0.078(4) 0.074(5) -0.025(4) -0.008(4) 0.008(4) C28 0.101(6) 0.074(5) 0.109(6) -0.031(4) -0.031(5) -0.009(4) C29 0.076(4) 0.063(4) 0.099(5) -0.013(4) -0.012(4) -0.019(3) C30 0.060(3) 0.057(3) 0.088(4) -0.006(3) -0.004(3) -0.011(3) N6 0.037(2) 0.098(4) 0.068(3) 0.023(3) 0.006(2) -0.005(2) N5 0.041(2) 0.054(3) 0.051(3) -0.003(2) 0.0064(19) 0.0034(19) N3 0.0381(19) 0.044(2) 0.050(2) 0.000(2) 0.0108(17) -0.0010(18) N4 0.051(2) 0.046(2) 0.052(2) -0.001(2) 0.0040(19) 0.003(2) N1 0.051(2) 0.045(2) 0.046(2) -0.0040(19) -0.0002(19) 0.0088(18) N2 0.057(3) 0.044(2) 0.057(3) -0.009(2) -0.004(2) 0.003(2) F1 0.136(4) 0.091(3) 0.193(5) -0.030(3) -0.051(4) 0.006(3) F2 0.086(3) 0.157(5) 0.259(7) -0.110(5) -0.013(4) -0.008(3) F3 0.183(6) 0.172(6) 0.230(7) 0.096(5) 0.089(5) -0.005(4) F4 0.111(3) 0.102(3) 0.180(5) -0.015(3) 0.022(3) 0.045(3) F5 0.085(3) 0.113(3) 0.234(6) -0.052(4) 0.008(3) 0.033(3) F6 0.115(4) 0.284(8) 0.183(6) 0.127(6) 0.044(4) -0.002(4) F7 0.382(12) 0.135(5) 0.140(5) -0.031(4) -0.059(6) 0.102(6) F8 0.240(8) 0.193(7) 0.154(6) -0.064(5) 0.027(5) 0.008(6) F9 0.166(5) 0.326(10) 0.135(5) -0.129(6) 0.018(4) -0.053(6) F10 0.73(2) 0.164(6) 0.083(4) -0.031(4) -0.025(8) 0.138(10) F11 0.223(7) 0.229(7) 0.195(7) 0.075(6) 0.079(6) 0.110(6) F12 0.259(10) 0.247(10) 0.66(2) -0.205(13) -0.280(14) 0.135(9) P1 0.0377(6) 0.0514(8) 0.0549(8) 0.0020(6) 0.0041(6) -0.0016(5) P2 0.0567(9) 0.0504(8) 0.1133(14) -0.0013(9) 0.0214(9) -0.0028(7) P3 0.242(4) 0.137(3) 0.0838(17) -0.0578(17) -0.0487(19) 0.074(2) Ru1 0.0410(2) 0.0408(2) 0.0485(2) -0.0036(2) 0.00253(15) -0.00114(19) C2 0.052(4) 0.142(7) 0.134(7) 0.009(6) 0.011(4) -0.007(5) C4A 0.096(5) 0.208(11) 0.118(10) 0.033(8) 0.048(7) -0.033(7) C3A 0.096(5) 0.208(11) 0.118(10) 0.033(8) 0.048(7) -0.033(7) C4B 0.096(5) 0.208(11) 0.118(10) 0.033(8) 0.048(7) -0.033(7) C3B 0.096(5) 0.208(11) 0.118(10) 0.033(8) 0.048(7) -0.033(7) N7 0.032(2) 0.091(4) 0.090(4) 0.002(3) 0.005(2) -0.002(2) C5A 0.063(4) 0.216(13) 0.140(7) 0.069(9) -0.015(4) -0.011(6) C6A 0.063(4) 0.216(13) 0.140(7) 0.069(9) -0.015(4) -0.011(6) C7A 0.063(4) 0.216(13) 0.140(7) 0.069(9) -0.015(4) -0.011(6) C5B 0.063(4) 0.216(13) 0.140(7) 0.069(9) -0.015(4) -0.011(6) C6B 0.063(4) 0.216(13) 0.140(7) 0.069(9) -0.015(4) -0.011(6) C7B 0.063(4) 0.216(13) 0.140(7) 0.069(9) -0.015(4) -0.011(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N6 1.252(6) . ? C1 N7 1.325(6) . ? C1 H1 0.95 . ? C14 C19 1.395(7) . ? C14 C15 1.396(8) . ? C14 P1 1.827(5) . ? C19 C18 1.389(8) . ? C19 H19 0.95 . ? C18 C17 1.370(10) . ? C18 H18 0.95 . ? C17 C16 1.385(10) . ? C17 H17 0.95 . ? C16 C15 1.377(8) . ? C16 H16 0.95 . ? C15 H15 0.95 . ? C8 C13 1.385(7) . ? C8 C9 1.388(7) . ? C8 P1 1.820(5) . ? C13 C12 1.386(8) . ? C13 H13 0.95 . ? C12 C11 1.409(11) . ? C12 H12 0.95 . ? C11 C10 1.333(11) . ? C11 H11 0.95 . ? C10 C9 1.373(9) . ? C10 H10 0.95 . ? C9 H9 0.95 . ? C45 N5 1.353(6) . ? C45 C44 1.369(7) . ? C45 H45 0.95 . ? C44 C43 1.375(9) . ? C44 H44 0.95 . ? C43 C42 1.392(9) . ? C43 H43 0.95 . ? C42 C41 1.373(7) . ? C42 H42 0.95 . ? C41 N5 1.375(6) . ? C41 C40 1.453(7) . ? C40 N3 1.350(6) . ? C40 C39 1.406(7) . ? C39 C38 1.355(8) . ? C39 H39 0.95 . ? C38 C37 1.381(8) . ? C38 H38 0.95 . ? C37 C36 1.380(7) . ? C37 H37 0.95 . ? C36 N3 1.346(6) . ? C36 C35 1.486(7) . ? C35 N4 1.374(6) . ? C35 C34 1.381(7) . ? C34 C33 1.367(9) . ? C34 H34 0.95 . ? C33 C32 1.373(9) . ? C33 H33 0.95 . ? C32 C31 1.371(8) . ? C32 H32 0.95 . ? C31 N4 1.341(6) . ? C31 H31 0.95 . ? C21 N1 1.341(6) . ? C21 C22 1.392(7) . ? C21 H21 0.95 . ? C22 C23 1.359(9) . ? C22 H22 0.95 . ? C23 C24 1.390(9) . ? C23 H23 0.95 . ? C24 C25 1.390(8) . ? C24 H24 0.95 . ? C25 N1 1.359(6) . ? C25 C26 1.450(8) . ? C26 N2 1.358(7) . ? C26 C27 1.417(8) . ? C27 C28 1.367(10) . ? C27 H27 0.95 . ? C28 C29 1.348(10) . ? C28 H28 0.95 . ? C29 C30 1.362(8) . ? C29 H29 0.95 . ? C30 N2 1.342(7) . ? C30 H30 0.95 . ? N6 P1 1.658(4) . ? N5 Ru1 2.095(4) . ? N3 Ru1 1.965(4) . ? N4 Ru1 2.074(4) . ? N1 Ru1 2.113(4) . ? N2 Ru1 2.121(4) . ? F1 P2 1.558(5) . ? F2 P2 1.537(5) . ? F3 P2 1.536(6) . ? F4 P2 1.556(4) . ? F5 P2 1.561(4) . ? F6 P2 1.539(5) . ? F7 P3 1.613(9) . ? F8 P3 1.570(9) . ? F9 P3 1.493(6) . ? F10 P3 1.551(8) . ? F11 P3 1.589(8) . ? F12 P3 1.459(8) . ? P1 Ru1 2.3247(14) . ? C2 C3B 1.434(9) . ? C2 C3A 1.456(9) . ? C2 C4B 1.476(9) . ? C2 C4A 1.477(9) . ? C2 N7 1.504(9) . ? C2 H2 1 . ? C4A H4A1 0.98 . ? C4A H4A2 0.98 . ? C4A H4A3 0.98 . ? C3A H3A1 0.98 . ? C3A H3A2 0.98 . ? C3A H3A3 0.98 . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 0.98 . ? C3B H3B1 0.98 . ? C3B H3B2 0.98 . ? C3B H3B3 0.98 . ? N7 C5B 1.438(18) . ? N7 C5A 1.55(2) . ? C5A C7A 1.457(10) . ? C5A C6A 1.470(9) . ? C5A H5A 1 . ? C6A H6A1 0.98 . ? C6A H6A2 0.98 . ? C6A H6A3 0.98 . ? C7A H7A1 0.98 . ? C7A H7A2 0.98 . ? C7A H7A3 0.98 . ? C5B C7B 1.453(9) . ? C5B C6B 1.463(9) . ? C5B H5B 1 . ? C6B H6B1 0.98 . ? C6B H6B2 0.98 . ? C6B H6B3 0.98 . ? C7B H7B1 0.98 . ? C7B H7B2 0.98 . ? C7B H7B3 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 C1 N7 127.6(6) . . ? N6 C1 H1 116.2 . . ? N7 C1 H1 116.2 . . ? C19 C14 C15 118.2(5) . . ? C19 C14 P1 119.2(4) . . ? C15 C14 P1 122.4(4) . . ? C18 C19 C14 120.6(6) . . ? C18 C19 H19 119.7 . . ? C14 C19 H19 119.7 . . ? C17 C18 C19 120.1(6) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C17 C16 120.2(6) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C15 C16 C17 119.9(7) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C15 C14 121.0(6) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C13 C8 C9 117.6(5) . . ? C13 C8 P1 121.3(4) . . ? C9 C8 P1 120.3(4) . . ? C8 C13 C12 121.0(6) . . ? C8 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C12 C11 119.1(7) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C10 C11 C12 119.6(7) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C10 C9 121.2(7) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C9 C8 121.4(7) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? N5 C45 C44 122.7(5) . . ? N5 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? C45 C44 C43 119.7(6) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C43 C42 118.5(5) . . ? C44 C43 H43 120.8 . . ? C42 C43 H43 120.8 . . ? C41 C42 C43 120.1(6) . . ? C41 C42 H42 120 . . ? C43 C42 H42 120 . . ? C42 C41 N5 121.2(5) . . ? C42 C41 C40 123.4(5) . . ? N5 C41 C40 115.4(4) . . ? N3 C40 C39 119.1(5) . . ? N3 C40 C41 113.3(4) . . ? C39 C40 C41 127.6(5) . . ? C38 C39 C40 119.5(5) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C39 C38 C37 120.6(5) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C36 C37 C38 118.8(5) . . ? C36 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? N3 C36 C37 120.5(5) . . ? N3 C36 C35 113.3(4) . . ? C37 C36 C35 126.2(5) . . ? N4 C35 C34 121.0(5) . . ? N4 C35 C36 114.6(4) . . ? C34 C35 C36 124.4(5) . . ? C33 C34 C35 119.6(6) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C33 C32 119.4(6) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C31 C32 C33 119.5(6) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? N4 C31 C32 122.3(6) . . ? N4 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? N1 C21 C22 122.9(5) . . ? N1 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C23 C22 C21 118.1(6) . . ? C23 C22 H22 121 . . ? C21 C22 H22 121 . . ? C22 C23 C24 120.5(6) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 118.8(6) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? N1 C25 C24 121.0(6) . . ? N1 C25 C26 115.3(5) . . ? C24 C25 C26 123.6(6) . . ? N2 C26 C27 120.6(6) . . ? N2 C26 C25 116.5(5) . . ? C27 C26 C25 123.0(6) . . ? C28 C27 C26 118.9(7) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C29 C28 C27 120.3(7) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 118.6(7) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? N2 C30 C29 124.5(6) . . ? N2 C30 H30 117.8 . . ? C29 C30 H30 117.8 . . ? C1 N6 P1 124.5(4) . . ? C45 N5 C41 117.8(4) . . ? C45 N5 Ru1 129.2(4) . . ? C41 N5 Ru1 112.9(3) . . ? C36 N3 C40 121.4(4) . . ? C36 N3 Ru1 119.0(3) . . ? C40 N3 Ru1 119.5(3) . . ? C31 N4 C35 118.2(4) . . ? C31 N4 Ru1 128.4(4) . . ? C35 N4 Ru1 113.4(3) . . ? C21 N1 C25 118.7(5) . . ? C21 N1 Ru1 125.3(3) . . ? C25 N1 Ru1 116.0(4) . . ? C30 N2 C26 117.0(5) . . ? C30 N2 Ru1 127.7(4) . . ? C26 N2 Ru1 115.1(3) . . ? N6 P1 C8 103.7(2) . . ? N6 P1 C14 105.8(2) . . ? C8 P1 C14 103.3(2) . . ? N6 P1 Ru1 111.84(18) . . ? C8 P1 Ru1 110.88(16) . . ? C14 P1 Ru1 119.77(18) . . ? F3 P2 F2 89.1(4) . . ? F3 P2 F6 177.0(4) . . ? F2 P2 F6 92.6(4) . . ? F3 P2 F4 89.8(3) . . ? F2 P2 F4 89.2(3) . . ? F6 P2 F4 87.7(3) . . ? F3 P2 F1 89.3(4) . . ? F2 P2 F1 178.3(4) . . ? F6 P2 F1 89.0(4) . . ? F4 P2 F1 91.4(3) . . ? F3 P2 F5 90.4(4) . . ? F2 P2 F5 91.2(3) . . ? F6 P2 F5 92.0(4) . . ? F4 P2 F5 179.5(3) . . ? F1 P2 F5 88.1(3) . . ? F12 P3 F9 97.2(7) . . ? F12 P3 F10 94.2(8) . . ? F9 P3 F10 168.0(7) . . ? F12 P3 F8 92.6(7) . . ? F9 P3 F8 93.4(5) . . ? F10 P3 F8 89.8(4) . . ? F12 P3 F11 177.8(8) . . ? F9 P3 F11 84.3(4) . . ? F10 P3 F11 84.2(6) . . ? F8 P3 F11 88.9(4) . . ? F12 P3 F7 90.4(6) . . ? F9 P3 F7 89.3(4) . . ? F10 P3 F7 86.9(5) . . ? F8 P3 F7 175.7(5) . . ? F11 P3 F7 87.9(5) . . ? N3 Ru1 N4 79.71(15) . . ? N3 Ru1 N5 78.76(16) . . ? N4 Ru1 N5 158.45(16) . . ? N3 Ru1 N1 93.31(15) . . ? N4 Ru1 N1 91.85(15) . . ? N5 Ru1 N1 88.62(15) . . ? N3 Ru1 N2 169.65(17) . . ? N4 Ru1 N2 96.61(15) . . ? N5 Ru1 N2 104.47(16) . . ? N1 Ru1 N2 77.06(16) . . ? N3 Ru1 P1 90.80(11) . . ? N4 Ru1 P1 87.23(11) . . ? N5 Ru1 P1 93.83(11) . . ? N1 Ru1 P1 175.56(11) . . ? N2 Ru1 P1 98.72(13) . . ? C3B C2 C3A 28.7(10) . . ? C3B C2 C4B 109.0(11) . . ? C3A C2 C4B 137.1(13) . . ? C3B C2 C4A 75.5(11) . . ? C3A C2 C4A 104.0(9) . . ? C4B C2 C4A 33.9(9) . . ? C3B C2 N7 125.6(12) . . ? C3A C2 N7 106.6(8) . . ? C4B C2 N7 97.5(9) . . ? C4A C2 N7 122.1(8) . . ? C3B C2 H2 114.3 . . ? C3A C2 H2 107.8 . . ? C4B C2 H2 97.5 . . ? C4A C2 H2 107.8 . . ? N7 C2 H2 107.8 . . ? C2 C4A H4A1 109.5 . . ? C2 C4A H4A2 109.5 . . ? C2 C4A H4A3 109.5 . . ? C2 C3A H3A1 109.5 . . ? C2 C3A H3A2 109.5 . . ? C2 C3A H3A3 109.5 . . ? C2 C4B H4B1 109.5 . . ? C2 C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C2 C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C2 C3B H3B1 109.5 . . ? C2 C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C2 C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C1 N7 C5B 118.9(8) . . ? C1 N7 C2 119.9(5) . . ? C5B N7 C2 119.4(8) . . ? C1 N7 C5A 116.9(8) . . ? C5B N7 C5A 38.9(10) . . ? C2 N7 C5A 116.9(9) . . ? C7A C5A C6A 103.4(12) . . ? C7A C5A N7 112.8(18) . . ? C6A C5A N7 109.8(16) . . ? C7A C5A H5A 110.2 . . ? C6A C5A H5A 110.2 . . ? N7 C5A H5A 110.2 . . ? N7 C5B C7B 116.8(16) . . ? N7 C5B C6B 114.5(13) . . ? C7B C5B C6B 107.7(11) . . ? N7 C5B H5B 105.6 . . ? C7B C5B H5B 105.6 . . ? C6B C5B H5B 105.6 . . ? C5B C6B H6B1 109.5 . . ? C5B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C5B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C5B C7B H7B1 109.5 . . ? C5B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C5B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF