# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Catherine E Housecroft' 'Edwin Constable' 'Egbert Figgemeier' 'Swarna Latha Kokatam' 'Elaine A. Medlycott' 'Markus Neuburger' 'Silvia Schaffner' 'Jennifer A Zampese' _publ_contact_author_name 'Catherine E Housecroft' _publ_contact_author_email CATHERINE.HOUSECROFT@UNIBAS.CH _publ_section_title ; Wiring terpyridine: approaches to alkynylthienyl 2,2':6',2"-terpyridines ; # Attachment 'Ligand_02.cif' data_em2_173k _database_code_depnum_ccdc_archive 'CCDC 694383' _audit_creation_date 06-12-18 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '12181351 em2_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.05460(10) _cell_length_b 8.78370(10) _cell_length_c 18.2893(2) _cell_angle_alpha 90 _cell_angle_beta 97.1365(8) _cell_angle_gamma 90 _cell_volume 1602.74(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C19 H12 Br1 N3 S1 # Dc = 1.63 Fooo = 792.00 Mu = 27.00 M = 394.29 # Found Formula = C19 H12 Br1 N3 S1 # Dc = 1.63 FOOO = 792.00 Mu = 27.00 M = 394.29 _chemical_formula_sum 'C19 H12 Br1 N3 S1' _chemical_formula_moiety 'C19 H12 Br N3 S' _chemical_compound_source ? _chemical_formula_weight 394.29 _cell_measurement_reflns_used 7055 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_min 0.11 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 2.700 # Sheldrick geometric approximatio 0.65 0.74 # No experimental values of Tmin/max available _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.74 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 13984 _reflns_number_total 3823 _diffrn_reflns_av_R_equivalents 0.026 # Number of reflections with Friedels Law is 3823 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3825 _diffrn_reflns_theta_min 2.204 _diffrn_reflns_theta_max 27.882 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.882 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.30 _refine_diff_density_max 0.31 _refine_ls_number_reflns 2947 _refine_ls_number_restraints 0 _refine_ls_number_parameters 217 #_refine_ls_R_factor_ref 0.0217 _refine_ls_wR_factor_ref 0.0239 _refine_ls_goodness_of_fit_ref 1.0852 #_reflns_number_all 3798 _refine_ls_R_factor_all 0.0301 _refine_ls_wR_factor_all 0.0313 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 2947 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_gt 0.0239 _refine_ls_shift/su_max 0.000710 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.325 0.132 0.130 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Br1 Br 0.221684(17) 0.586211(19) 0.434744(10) 0.0359 1.0000 Uani . . . . . . S1 S 0.38990(4) 0.15188(5) 0.51635(2) 0.0331 1.0000 Uani . . . . . . N1 N -0.21969(13) 0.09336(16) 0.63925(8) 0.0309 1.0000 Uani . . . . . . N2 N 0.03836(13) -0.19176(15) 0.64167(7) 0.0273 1.0000 Uani . . . . . . N3 N 0.35940(14) -0.36919(17) 0.64026(8) 0.0356 1.0000 Uani . . . . . . C1 C -0.34305(16) 0.1072(2) 0.65874(10) 0.0345 1.0000 Uani . . . . . . C2 C -0.41051(17) -0.0084(2) 0.68925(10) 0.0369 1.0000 Uani . . . . . . C3 C -0.34663(18) -0.1467(2) 0.70238(10) 0.0396 1.0000 Uani . . . . . . C4 C -0.21919(17) -0.1644(2) 0.68230(10) 0.0345 1.0000 Uani . . . . . . C5 C -0.15924(15) -0.04239(18) 0.65053(8) 0.0275 1.0000 Uani . . . . . . C6 C -0.02309(15) -0.05707(18) 0.62702(8) 0.0270 1.0000 Uani . . . . . . C7 C 0.03519(16) 0.06161(18) 0.59249(9) 0.0288 1.0000 Uani . . . . . . C8 C 0.16258(15) 0.04240(18) 0.57102(8) 0.0270 1.0000 Uani . . . . . . C9 C 0.22700(15) -0.09726(19) 0.58695(9) 0.0290 1.0000 Uani . . . . . . C10 C 0.16196(15) -0.20943(18) 0.62271(8) 0.0274 1.0000 Uani . . . . . . C11 C 0.22711(16) -0.35840(18) 0.64418(8) 0.0283 1.0000 Uani . . . . . . C12 C 0.15256(17) -0.47697(19) 0.66909(9) 0.0331 1.0000 Uani . . . . . . C13 C 0.21680(19) -0.6105(2) 0.69248(10) 0.0374 1.0000 Uani . . . . . . C14 C 0.35309(19) -0.6228(2) 0.68968(9) 0.0367 1.0000 Uani . . . . . . C15 C 0.41874(18) -0.5010(2) 0.66297(10) 0.0397 1.0000 Uani . . . . . . C16 C 0.22515(15) 0.16524(18) 0.53323(8) 0.0271 1.0000 Uani . . . . . . C17 C 0.17096(15) 0.30214(18) 0.50822(9) 0.0284 1.0000 Uani . . . . . . C18 C 0.26400(16) 0.39261(18) 0.47636(9) 0.0282 1.0000 Uani . . . . . . C19 C 0.38682(16) 0.32811(19) 0.47650(9) 0.0328 1.0000 Uani . . . . . . H11 H -0.3837 0.2069 0.6499 0.0425 1.0000 Uiso R . . . . . H21 H -0.4989 0.0073 0.7026 0.0446 1.0000 Uiso R . . . . . H31 H -0.3884 -0.2293 0.7251 0.0492 1.0000 Uiso R . . . . . H41 H -0.1728 -0.2605 0.6887 0.0421 1.0000 Uiso R . . . . . H71 H -0.0126 0.1551 0.5841 0.0352 1.0000 Uiso R . . . . . H91 H 0.3159 -0.1166 0.5728 0.0342 1.0000 Uiso R . . . . . H121 H 0.0570 -0.4661 0.6711 0.0405 1.0000 Uiso R . . . . . H131 H 0.1687 -0.6973 0.7116 0.0456 1.0000 Uiso R . . . . . H141 H 0.4006 -0.7141 0.7071 0.0447 1.0000 Uiso R . . . . . H151 H 0.5139 -0.5108 0.6592 0.0485 1.0000 Uiso R . . . . . H171 H 0.0812 0.3340 0.5116 0.0348 1.0000 Uiso R . . . . . H191 H 0.4623 0.3696 0.4562 0.0408 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.03307(9) 0.03011(9) 0.04555(10) 0.00928(7) 0.00885(6) 0.00721(7) S1 0.02554(18) 0.0309(2) 0.0443(2) 0.00538(17) 0.00958(16) 0.00943(15) N1 0.0266(6) 0.0296(7) 0.0374(7) 0.0008(6) 0.0076(5) 0.0054(5) N2 0.0242(6) 0.0277(6) 0.0300(6) -0.0008(5) 0.0032(5) 0.0054(5) N3 0.0288(7) 0.0338(7) 0.0453(8) 0.0084(6) 0.0094(6) 0.0101(6) C1 0.0287(8) 0.0338(9) 0.0419(9) -0.0001(7) 0.0080(7) 0.0069(7) C2 0.0274(8) 0.0437(10) 0.0413(9) 0.0018(8) 0.0109(7) 0.0045(7) C3 0.0337(9) 0.0404(10) 0.0463(10) 0.0086(8) 0.0118(7) 0.0015(7) C4 0.0301(8) 0.0315(8) 0.0426(9) 0.0062(7) 0.0079(7) 0.0063(7) C5 0.0241(7) 0.0299(8) 0.0282(7) -0.0006(6) 0.0023(6) 0.0038(6) C6 0.0240(7) 0.0284(8) 0.0284(7) -0.0002(6) 0.0022(6) 0.0036(6) C7 0.0252(7) 0.0268(7) 0.0345(8) 0.0015(6) 0.0046(6) 0.0067(6) C8 0.0260(7) 0.0279(7) 0.0272(7) -0.0010(6) 0.0033(6) 0.0052(6) C9 0.0251(7) 0.0300(8) 0.0323(7) 0.0009(6) 0.0052(6) 0.0063(6) C10 0.0252(7) 0.0280(8) 0.0289(7) -0.0013(6) 0.0023(6) 0.0066(6) C11 0.0290(7) 0.0282(8) 0.0281(7) -0.0011(6) 0.0055(6) 0.0070(6) C12 0.0327(8) 0.0303(8) 0.0372(8) 0.0019(7) 0.0080(7) 0.0054(7) C13 0.0436(9) 0.0309(8) 0.0387(9) 0.0055(7) 0.0095(7) 0.0059(7) C14 0.0450(9) 0.0323(9) 0.0328(8) 0.0045(7) 0.0054(7) 0.0166(7) C15 0.0336(8) 0.0399(10) 0.0466(10) 0.0089(8) 0.0089(7) 0.0153(8) C16 0.0240(7) 0.0281(8) 0.0297(7) -0.0007(6) 0.0048(6) 0.0055(6) C17 0.0253(7) 0.0290(8) 0.0314(8) 0.0005(6) 0.0051(6) 0.0060(6) C18 0.0277(7) 0.0260(7) 0.0311(7) 0.0027(6) 0.0045(6) 0.0048(6) C19 0.0278(7) 0.0315(8) 0.0403(9) 0.0042(7) 0.0085(6) 0.0046(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3830(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 . C18 . 1.8899(15) yes S1 . C16 . 1.7264(15) yes S1 . C19 . 1.7096(17) yes N1 . C1 . 1.338(2) yes N1 . C5 . 1.343(2) yes N2 . C6 . 1.346(2) yes N2 . C10 . 1.3401(19) yes N3 . C11 . 1.344(2) yes N3 . C15 . 1.344(2) yes C1 . C2 . 1.377(3) yes C1 . H11 . 0.972 no C2 . C3 . 1.381(3) yes C2 . H21 . 0.960 no C3 . C4 . 1.385(2) yes C3 . H31 . 0.959 no C4 . C5 . 1.392(2) yes C4 . H41 . 0.964 no C5 . C6 . 1.491(2) yes C6 . C7 . 1.386(2) yes C7 . C8 . 1.396(2) yes C7 . H71 . 0.954 no C8 . C9 . 1.401(2) yes C8 . C16 . 1.465(2) yes C9 . C10 . 1.390(2) yes C9 . H91 . 0.976 no C10 . C11 . 1.494(2) yes C11 . C12 . 1.392(2) yes C12 . C13 . 1.381(2) yes C12 . H121 . 0.971 no C13 . C14 . 1.382(3) yes C13 . H131 . 0.990 no C14 . C15 . 1.378(3) yes C14 . H141 . 0.967 no C15 . H151 . 0.972 no C16 . C17 . 1.375(2) yes C17 . C18 . 1.408(2) yes C17 . H171 . 0.954 no C18 . C19 . 1.358(2) yes C19 . H191 . 0.958 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C16 . S1 . C19 . 92.74(8) yes C1 . N1 . C5 . 117.17(14) yes C6 . N2 . C10 . 117.89(14) yes C11 . N3 . C15 . 116.64(15) yes N1 . C1 . C2 . 124.11(16) yes N1 . C1 . H11 . 115.0 no C2 . C1 . H11 . 120.9 no C1 . C2 . C3 . 118.48(15) yes C1 . C2 . H21 . 121.0 no C3 . C2 . H21 . 120.5 no C2 . C3 . C4 . 118.59(17) yes C2 . C3 . H31 . 121.4 no C4 . C3 . H31 . 120.0 no C3 . C4 . C5 . 119.15(16) yes C3 . C4 . H41 . 121.1 no C5 . C4 . H41 . 119.7 no C4 . C5 . N1 . 122.47(15) yes C4 . C5 . C6 . 120.98(14) yes N1 . C5 . C6 . 116.55(14) yes C5 . C6 . N2 . 115.71(14) yes C5 . C6 . C7 . 121.46(14) yes N2 . C6 . C7 . 122.83(14) yes C6 . C7 . C8 . 119.47(14) yes C6 . C7 . H71 . 119.2 no C8 . C7 . H71 . 121.4 no C7 . C8 . C9 . 117.66(14) yes C7 . C8 . C16 . 120.43(14) yes C9 . C8 . C16 . 121.91(14) yes C8 . C9 . C10 . 119.09(14) yes C8 . C9 . H91 . 120.8 no C10 . C9 . H91 . 120.1 no C9 . C10 . N2 . 123.04(14) yes C9 . C10 . C11 . 121.86(14) yes N2 . C10 . C11 . 115.08(14) yes C10 . C11 . N3 . 116.89(15) yes C10 . C11 . C12 . 120.32(14) yes N3 . C11 . C12 . 122.76(15) yes C11 . C12 . C13 . 119.11(16) yes C11 . C12 . H121 . 120.9 no C13 . C12 . H121 . 119.9 no C12 . C13 . C14 . 118.87(17) yes C12 . C13 . H131 . 122.2 no C14 . C13 . H131 . 118.9 no C13 . C14 . C15 . 118.25(16) yes C13 . C14 . H141 . 120.3 no C15 . C14 . H141 . 121.4 no C14 . C15 . N3 . 124.35(16) yes C14 . C15 . H151 . 118.4 no N3 . C15 . H151 . 117.3 no C8 . C16 . S1 . 120.81(11) yes C8 . C16 . C17 . 128.72(14) yes S1 . C16 . C17 . 110.45(12) yes C16 . C17 . C18 . 112.04(14) yes C16 . C17 . H171 . 125.0 no C18 . C17 . H171 . 122.9 no Br1 . C18 . C17 . 123.14(11) yes Br1 . C18 . C19 . 122.36(12) yes C17 . C18 . C19 . 114.49(14) yes S1 . C19 . C18 . 110.29(12) yes S1 . C19 . H191 . 122.5 no C18 . C19 . H191 . 127.2 no # Attachment 'Ligand_04.cif' data_sk-6r _database_code_depnum_ccdc_archive 'CCDC 694384' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H21 N3 S Si' _chemical_formula_sum 'C24 H21 N3 S Si' _chemical_formula_weight 411.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc 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 17.057(3) _cell_length_b 5.4900(11) _cell_length_c 23.658(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.28(3) _cell_angle_gamma 90.00 _cell_volume 2156.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.221 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25695 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3767 _reflns_number_gt 3565 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.8340P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3767 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0963 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.02793(11) 0.1920(4) -0.14845(9) 0.0560(5) Uani 1 1 d . . . H1A H -0.0818 0.2158 -0.1465 0.067 Uiso 1 1 calc R . . C2 C -0.01108(11) 0.0033(3) -0.18205(8) 0.0528(5) Uani 1 1 d . . . H2A H -0.0524 -0.0980 -0.2025 0.063 Uiso 1 1 calc R . . C3 C 0.06707(11) -0.0333(3) -0.18488(8) 0.0491(4) Uani 1 1 d . . . H3A H 0.0806 -0.1609 -0.2074 0.059 Uiso 1 1 calc R . . C4 C 0.12594(10) 0.1198(3) -0.15429(7) 0.0418(4) Uani 1 1 d . . . H4A H 0.1801 0.0982 -0.1558 0.050 Uiso 1 1 calc R . . C5 C 0.10422(9) 0.3052(3) -0.12150(6) 0.0337(3) Uani 1 1 d . . . C6 C 0.16610(9) 0.4741(3) -0.08754(6) 0.0317(3) Uani 1 1 d . . . C7 C 0.14587(9) 0.6525(3) -0.05202(6) 0.0341(3) Uani 1 1 d . . . H7A H 0.0925 0.6676 -0.0481 0.041 Uiso 1 1 calc R . . C8 C 0.20525(9) 0.8095(3) -0.02219(6) 0.0324(3) Uani 1 1 d . . . C9 C 0.28316(9) 0.7769(3) -0.02989(6) 0.0334(3) Uani 1 1 d . . . H9A H 0.3249 0.8806 -0.0110 0.040 Uiso 1 1 calc R . . C10 C 0.29898(9) 0.5916(3) -0.06538(6) 0.0313(3) Uani 1 1 d . . . C11 C 0.38221(9) 0.5498(3) -0.07275(6) 0.0321(3) Uani 1 1 d . . . C12 C 0.40195(9) 0.3398(3) -0.09859(7) 0.0380(4) Uani 1 1 d . . . H12A H 0.3631 0.2181 -0.1113 0.046 Uiso 1 1 calc R . . C13 C 0.47976(10) 0.3120(3) -0.10536(8) 0.0453(4) Uani 1 1 d . . . H13A H 0.4946 0.1713 -0.1230 0.054 Uiso 1 1 calc R . . C14 C 0.53527(10) 0.4929(3) -0.08598(7) 0.0459(4) Uani 1 1 d . . . H14A H 0.5884 0.4798 -0.0906 0.055 Uiso 1 1 calc R . . C15 C 0.51089(10) 0.6933(3) -0.05963(7) 0.0434(4) Uani 1 1 d . . . H15A H 0.5493 0.8143 -0.0454 0.052 Uiso 1 1 calc R . . C16 C 0.18755(9) 1.0003(3) 0.01619(6) 0.0338(3) Uani 1 1 d . . . C17 C 0.11654(10) 1.0637(4) 0.02866(8) 0.0543(5) Uani 1 1 d . . . H17A H 0.0676 0.9857 0.0121 0.065 Uiso 1 1 calc R . . C18 C 0.12274(11) 1.2576(4) 0.06871(8) 0.0533(5) Uani 1 1 d . . . H18A H 0.0786 1.3221 0.0813 0.064 Uiso 1 1 calc R . . C19 C 0.19928(10) 1.3405(3) 0.08703(6) 0.0360(3) Uani 1 1 d . . . C20 C 0.23159(10) 1.5219(3) 0.12874(6) 0.0378(3) Uani 1 1 d . . . C21 C 0.26368(10) 1.6643(3) 0.16549(7) 0.0417(4) Uani 1 1 d . . . C22 C 0.23689(11) 2.0424(4) 0.24960(8) 0.0512(4) Uani 1 1 d . . . H22A H 0.1961 1.9390 0.2598 0.077 Uiso 1 1 calc R . . H22B H 0.2121 2.1476 0.2175 0.077 Uiso 1 1 calc R . . H22C H 0.2619 2.1412 0.2828 0.077 Uiso 1 1 calc R . . C23 C 0.35942(16) 1.6405(4) 0.28773(9) 0.0752(7) Uani 1 1 d . . . H23A H 0.3174 1.5431 0.2981 0.113 Uiso 1 1 calc R . . H23B H 0.3871 1.7338 0.3212 0.113 Uiso 1 1 calc R . . H23C H 0.3976 1.5343 0.2751 0.113 Uiso 1 1 calc R . . C24 C 0.39428(12) 2.0340(4) 0.20791(9) 0.0626(5) Uani 1 1 d . . . H24A H 0.3706 2.1442 0.1766 0.094 Uiso 1 1 calc R . . H24B H 0.4321 1.9266 0.1953 0.094 Uiso 1 1 calc R . . H24C H 0.4223 2.1272 0.2413 0.094 Uiso 1 1 calc R . . N1 N 0.02760(8) 0.3434(3) -0.11840(7) 0.0464(4) Uani 1 1 d . . . N2 N 0.24156(7) 0.4408(2) -0.09410(5) 0.0323(3) Uani 1 1 d . . . N3 N 0.43594(8) 0.7267(2) -0.05294(6) 0.0377(3) Uani 1 1 d . . . S1 S 0.26354(2) 1.18182(7) 0.054198(17) 0.03806(13) Uani 1 1 d . . . Si1 Si 0.31404(3) 1.85105(8) 0.228006(18) 0.03718(14) 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 0.0345(9) 0.0586(11) 0.0704(13) -0.0193(10) 0.0029(8) -0.0114(8) C2 0.0451(10) 0.0466(10) 0.0583(11) -0.0130(8) -0.0058(8) -0.0151(8) C3 0.0530(10) 0.0426(9) 0.0472(10) -0.0154(8) 0.0020(8) -0.0085(8) C4 0.0404(8) 0.0427(9) 0.0406(9) -0.0090(7) 0.0057(7) -0.0088(7) C5 0.0369(8) 0.0336(8) 0.0283(7) -0.0002(6) 0.0027(6) -0.0079(6) C6 0.0348(7) 0.0333(7) 0.0252(7) 0.0001(6) 0.0031(6) -0.0078(6) C7 0.0337(7) 0.0377(8) 0.0295(7) -0.0031(6) 0.0044(6) -0.0066(6) C8 0.0377(8) 0.0330(8) 0.0246(7) -0.0011(6) 0.0036(6) -0.0065(6) C9 0.0355(7) 0.0339(8) 0.0290(7) -0.0038(6) 0.0034(6) -0.0098(6) C10 0.0349(7) 0.0325(7) 0.0248(7) 0.0013(6) 0.0036(5) -0.0077(6) C11 0.0360(7) 0.0342(8) 0.0244(6) 0.0031(6) 0.0038(6) -0.0060(6) C12 0.0396(8) 0.0375(8) 0.0353(8) -0.0028(6) 0.0055(6) -0.0069(6) C13 0.0460(9) 0.0462(10) 0.0445(9) -0.0019(7) 0.0119(7) 0.0027(8) C14 0.0351(8) 0.0541(10) 0.0482(9) 0.0071(8) 0.0088(7) -0.0009(7) C15 0.0348(8) 0.0458(9) 0.0469(9) 0.0048(7) 0.0037(7) -0.0103(7) C16 0.0366(8) 0.0353(8) 0.0273(7) -0.0044(6) 0.0031(6) -0.0082(6) C17 0.0354(8) 0.0645(12) 0.0620(11) -0.0309(10) 0.0091(8) -0.0124(8) C18 0.0411(9) 0.0629(11) 0.0577(11) -0.0283(10) 0.0151(8) -0.0084(9) C19 0.0438(8) 0.0357(8) 0.0276(7) -0.0039(6) 0.0063(6) -0.0044(6) C20 0.0457(8) 0.0361(8) 0.0301(7) -0.0029(6) 0.0056(6) -0.0025(7) C21 0.0517(10) 0.0374(9) 0.0332(8) -0.0058(7) 0.0036(7) -0.0013(7) C22 0.0484(10) 0.0576(11) 0.0480(10) -0.0140(9) 0.0121(8) -0.0035(8) C23 0.1162(19) 0.0445(11) 0.0459(11) -0.0068(9) -0.0206(12) 0.0110(11) C24 0.0515(10) 0.0776(14) 0.0598(12) -0.0217(11) 0.0151(9) -0.0131(10) N1 0.0364(7) 0.0488(8) 0.0514(8) -0.0150(7) 0.0049(6) -0.0093(6) N2 0.0364(7) 0.0333(6) 0.0261(6) -0.0012(5) 0.0048(5) -0.0079(5) N3 0.0361(7) 0.0374(7) 0.0374(7) 0.0004(6) 0.0038(5) -0.0083(6) S1 0.0359(2) 0.0398(2) 0.0368(2) -0.01261(16) 0.00492(16) -0.00910(16) Si1 0.0459(3) 0.0322(2) 0.0298(2) -0.00761(16) 0.00112(18) -0.00054(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.336(2) . ? C1 C2 1.376(3) . ? C1 H1A 0.9400 . ? C2 C3 1.365(3) . ? C2 H2A 0.9400 . ? C3 C4 1.380(2) . ? C3 H3A 0.9400 . ? C4 C5 1.381(2) . ? C4 H4A 0.9400 . ? C5 N1 1.342(2) . ? C5 C6 1.493(2) . ? C6 N2 1.3438(19) . ? C6 C7 1.385(2) . ? C7 C8 1.392(2) . ? C7 H7A 0.9400 . ? C8 C9 1.394(2) . ? C8 C16 1.463(2) . ? C9 C10 1.385(2) . ? C9 H9A 0.9400 . ? C10 N2 1.3420(18) . ? C10 C11 1.487(2) . ? C11 N3 1.3437(19) . ? C11 C12 1.383(2) . ? C12 C13 1.381(2) . ? C12 H12A 0.9400 . ? C13 C14 1.376(2) . ? C13 H13A 0.9400 . ? C14 C15 1.375(3) . ? C14 H14A 0.9400 . ? C15 N3 1.336(2) . ? C15 H15A 0.9400 . ? C16 C17 1.356(2) . ? C16 S1 1.7163(15) . ? C17 C18 1.413(2) . ? C17 H17A 0.9400 . ? C18 C19 1.356(2) . ? C18 H18A 0.9400 . ? C19 C20 1.421(2) . ? C19 S1 1.7189(16) . ? C20 C21 1.203(2) . ? C21 Si1 1.8421(17) . ? C22 Si1 1.8455(18) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 Si1 1.852(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 Si1 1.846(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? 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 N1 C1 C2 124.01(17) . . ? N1 C1 H1A 118.0 . . ? C2 C1 H1A 118.0 . . ? C3 C2 C1 118.37(16) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 119.08(17) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C3 C4 C5 119.12(16) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? N1 C5 C4 122.42(14) . . ? N1 C5 C6 116.78(14) . . ? C4 C5 C6 120.80(14) . . ? N2 C6 C7 123.03(13) . . ? N2 C6 C5 115.53(13) . . ? C7 C6 C5 121.44(13) . . ? C6 C7 C8 119.45(14) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C7 C8 C9 117.32(14) . . ? C7 C8 C16 121.88(14) . . ? C9 C8 C16 120.80(13) . . ? C10 C9 C8 119.87(13) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? N2 C10 C9 122.62(13) . . ? N2 C10 C11 116.79(13) . . ? C9 C10 C11 120.58(13) . . ? N3 C11 C12 122.77(14) . . ? N3 C11 C10 116.13(13) . . ? C12 C11 C10 121.10(13) . . ? C13 C12 C11 118.78(15) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? C14 C13 C12 119.19(16) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C15 C14 C13 118.15(15) . . ? C15 C14 H14A 120.9 . . ? C13 C14 H14A 120.9 . . ? N3 C15 C14 124.11(15) . . ? N3 C15 H15A 117.9 . . ? C14 C15 H15A 117.9 . . ? C17 C16 C8 129.86(14) . . ? C17 C16 S1 109.99(12) . . ? C8 C16 S1 120.15(11) . . ? C16 C17 C18 113.96(15) . . ? C16 C17 H17A 123.0 . . ? C18 C17 H17A 123.0 . . ? C19 C18 C17 112.66(16) . . ? C19 C18 H18A 123.7 . . ? C17 C18 H18A 123.7 . . ? C18 C19 C20 130.41(16) . . ? C18 C19 S1 110.65(12) . . ? C20 C19 S1 118.88(12) . . ? C21 C20 C19 175.17(18) . . ? C20 C21 Si1 173.04(15) . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C1 N1 C5 117.01(15) . . ? C10 N2 C6 117.69(13) . . ? C15 N3 C11 116.97(14) . . ? C16 S1 C19 92.73(7) . . ? C21 Si1 C22 107.97(8) . . ? C21 Si1 C24 109.43(9) . . ? C22 Si1 C24 112.32(10) . . ? C21 Si1 C23 107.53(9) . . ? C22 Si1 C23 110.11(11) . . ? C24 Si1 C23 109.36(12) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.209 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.036 # Attachment '[Ru_1_2][PF6]2_MeNO2.cif' data_em96_173k _database_code_depnum_ccdc_archive 'CCDC 694385' _audit_creation_date 07-06-11 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '6111128 em96_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 42.2425(5) _cell_length_b 9.13940(10) _cell_length_c 27.5009(3) _cell_angle_alpha 90 _cell_angle_beta 118.1874(7) _cell_angle_gamma 90 _cell_volume 9358.17(19) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 c 1 ' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z x,-y,z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C38 H24 Br2 F12 N6 O5 P2 Ru1 S2 # Dc = 1.79 Fooo = 5136.00 Mu = 22.97 M = 2519.16 # Found Formula = C40 H30 Br2 F12 N8 O4 P2 Ru1 S2 # Dc = 1.85 FOOO = 5136.00 Mu = 23.00 M = 2603.33 _chemical_formula_sum 'C40 H30 Br2 F12 N8 O4 P2 Ru1 S2' _chemical_formula_moiety 'C38 H24 Br2 N6 Ru S2, 2(F6 P), 2(C H3 N O2)' _chemical_compound_source ? _chemical_formula_weight 1301.66 _cell_measurement_reflns_used 23896 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.42 _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 2.300 # Sheldrick geometric approximatio 0.59 0.83 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.83 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 74588 _reflns_number_total 21976 _diffrn_reflns_av_R_equivalents 0.108 # Number of reflections with Friedels Law is 72273 # Number of reflections without Friedels Law is 21976 # Theoretical number of reflections is about 11302 _diffrn_reflns_theta_min 3.004 _diffrn_reflns_theta_max 28.004 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.004 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _reflns_limit_h_min -55 _reflns_limit_h_max 55 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min -36 _reflns_limit_l_max 36 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -2.11 _refine_diff_density_max 2.08 _refine_ls_number_reflns 19131 _refine_ls_number_restraints 2002 _refine_ls_number_parameters 1316 #_refine_ls_R_factor_ref 0.0439 _refine_ls_wR_factor_ref 0.0480 _refine_ls_goodness_of_fit_ref 1.0693 #_reflns_number_all 21787 _refine_ls_R_factor_all 0.0534 _refine_ls_wR_factor_all 0.0570 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 19131 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_gt 0.0480 _refine_ls_shift/su_max 0.004978 _refine_ls_abs_structure_Flack 0.195(5) _refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 14.1 -13.9 14.6 -3.78 2.11 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ru1 Ru 0.388300(16) 0.53641(3) 0.15613(2) 0.0168 1.0000 Uani . . . . . . Ru2 Ru 0.133009(16) 0.40105(3) 0.15137(2) 0.0164 1.0000 Uani . . . . . . N1 N 0.39564(10) 0.7391(4) 0.12835(15) 0.0206 1.0000 Uani . . . . . . N2 N 0.44100(9) 0.5499(4) 0.19420(15) 0.0187 1.0000 Uani . . . . . . N3 N 0.40222(9) 0.3384(4) 0.19750(14) 0.0188 1.0000 Uani . . . . . . N4 N 0.37801(10) 0.4347(4) 0.08291(15) 0.0210 1.0000 Uani . . . . . . N5 N 0.33565(9) 0.5288(4) 0.11880(15) 0.0176 1.0000 Uani . . . . . . N6 N 0.37726(10) 0.6360(4) 0.21420(15) 0.0216 1.0000 Uani . . . . . . N7 N 0.23152(12) 0.9024(5) 0.18811(19) 0.0357 1.0000 Uani . . . . . . N8 N 0.51292(14) 0.8364(6) 0.3395(3) 0.0547 1.0000 Uani . . . . . . N9 N 0.45705(13) 0.6963(5) 0.44672(18) 0.0396 1.0000 Uani . . . . . . N10 N 0.7350(2) 0.8141(8) 0.3956(3) 0.0559 0.7000 Uani D U . . . . N11 N 0.7752(6) 0.813(2) 0.4367(8) 0.0657 0.3000 Uani D U . . . . N51 N 0.13878(9) 0.5022(4) 0.22200(14) 0.0194 1.0000 Uani . . . . . . N52 N 0.18548(9) 0.4261(4) 0.19218(14) 0.0181 1.0000 Uani . . . . . . N53 N 0.14814(9) 0.3037(4) 0.09749(14) 0.0200 1.0000 Uani . . . . . . N54 N 0.11621(9) 0.5940(4) 0.10649(14) 0.0195 1.0000 Uani . . . . . . N55 N 0.08083(9) 0.3709(4) 0.11118(14) 0.0182 1.0000 Uani . . . . . . N56 N 0.12879(9) 0.2000(4) 0.18278(15) 0.0199 1.0000 Uani . . . . . . C1 C 0.37031(11) 0.8292(5) 0.09308(18) 0.0245 1.0000 Uani . . . . . . C2 C 0.37889(14) 0.9604(5) 0.0767(2) 0.0332 1.0000 Uani . . . . . . C3 C 0.41424(15) 0.9991(6) 0.0975(3) 0.0388 1.0000 Uani . . . . . . C4 C 0.44068(13) 0.9074(5) 0.1344(2) 0.0295 1.0000 Uani . . . . . . C5 C 0.43074(11) 0.7764(4) 0.14931(17) 0.0204 1.0000 Uani . . . . . . C6 C 0.45729(11) 0.6708(4) 0.18757(18) 0.0217 1.0000 Uani . . . . . . C7 C 0.49392(11) 0.6843(5) 0.21497(19) 0.0235 1.0000 Uani . . . . . . C8 C 0.51497(11) 0.5755(5) 0.25175(18) 0.0225 1.0000 Uani . . . . . . C9 C 0.49787(11) 0.4525(5) 0.25804(18) 0.0228 1.0000 Uani . . . . . . C10 C 0.46110(11) 0.4407(4) 0.22878(17) 0.0207 1.0000 Uani . . . . . . C11 C 0.43837(11) 0.3166(4) 0.22821(16) 0.0200 1.0000 Uani . . . . . . C12 C 0.45232(13) 0.1862(5) 0.25571(19) 0.0280 1.0000 Uani . . . . . . C13 C 0.42890(14) 0.0737(5) 0.2515(2) 0.0328 1.0000 Uani . . . . . . C14 C 0.39238(14) 0.0956(5) 0.2201(2) 0.0340 1.0000 Uani . . . . . . C15 C 0.38007(12) 0.2290(5) 0.19387(18) 0.0248 1.0000 Uani . . . . . . C16 C 0.40212(11) 0.3855(4) 0.06784(18) 0.0227 1.0000 Uani . . . . . . C17 C 0.39161(13) 0.3168(5) 0.0175(2) 0.0275 1.0000 Uani . . . . . . C18 C 0.35605(14) 0.2963(5) -0.0179(2) 0.0301 1.0000 Uani . . . . . . C19 C 0.33076(12) 0.3463(5) -0.00306(18) 0.0267 1.0000 Uani . . . . . . C20 C 0.34229(11) 0.4152(4) 0.04762(17) 0.0206 1.0000 Uani . . . . . . C21 C 0.31749(11) 0.4722(4) 0.06717(17) 0.0210 1.0000 Uani . . . . . . C22 C 0.28065(12) 0.4730(5) 0.03884(18) 0.0233 1.0000 Uani . . . . . . C23 C 0.26101(12) 0.5367(5) 0.06270(19) 0.0243 1.0000 Uani . . . . . . C24 C 0.28019(11) 0.5949(5) 0.11654(18) 0.0226 1.0000 Uani . . . . . . C25 C 0.31721(11) 0.5894(5) 0.14306(17) 0.0218 1.0000 Uani . . . . . . C26 C 0.34182(11) 0.6484(5) 0.19857(17) 0.0214 1.0000 Uani . . . . . . C27 C 0.32983(13) 0.7142(5) 0.2324(2) 0.0292 1.0000 Uani . . . . . . C28 C 0.35497(14) 0.7708(6) 0.2832(2) 0.0331 1.0000 Uani . . . . . . C29 C 0.39069(14) 0.7599(6) 0.29747(19) 0.0325 1.0000 Uani . . . . . . C30 C 0.40127(12) 0.6901(5) 0.26387(19) 0.0283 1.0000 Uani . . . . . . C31 C 0.55404(12) 0.5944(6) 0.2837(2) 0.0287 1.0000 Uani . . . . . . S1 S 0.58080(4) 0.46607(16) 0.32975(6) 0.0332 0.8500 Uani . . . . . . C32 C 0.57607(9) 0.7160(4) 0.28310(16) 0.0371 0.8500 Uani . . . . . . C33 C 0.61189(14) 0.6972(7) 0.3222(3) 0.0461 1.0000 Uani . . . . . . C34 C 0.61809(13) 0.5689(7) 0.3491(2) 0.0399 1.0000 Uani . . . . . . C35 C 0.22194(12) 0.5440(5) 0.03322(19) 0.0253 1.0000 Uani . . . . . . C36 C 0.19941(13) 0.6221(7) 0.0468(2) 0.0436 1.0000 Uani . . . . . . C37 C 0.16254(15) 0.6012(8) 0.0092(3) 0.0496 1.0000 Uani . . . . . . C38 C 0.15761(12) 0.5116(7) -0.0325(2) 0.0358 1.0000 Uani . . . . . . C39 C 0.26374(16) 0.9920(6) 0.2215(2) 0.0417 1.0000 Uani . . . . . . C40 C 0.53998(19) 0.7866(9) 0.3931(3) 0.0608 1.0000 Uani . . . . . . C41 C 0.4749(3) 0.5666(10) 0.4772(5) 0.0894 1.0000 Uani . . . . . . C42 C 0.7487(2) 0.7141(7) 0.4421(3) 0.0569 1.0000 Uani . U . . . . C51 C 0.11205(11) 0.5373(5) 0.23417(18) 0.0231 1.0000 Uani . . . . . . C52 C 0.11916(12) 0.6027(5) 0.28312(19) 0.0265 1.0000 Uani . . . . . . C53 C 0.15411(12) 0.6367(5) 0.32100(19) 0.0260 1.0000 Uani . . . . . . C54 C 0.18155(12) 0.6012(5) 0.30924(18) 0.0261 1.0000 Uani . . . . . . C55 C 0.17353(11) 0.5329(4) 0.25949(18) 0.0208 1.0000 Uani . . . . . . C56 C 0.20064(11) 0.4859(4) 0.24339(17) 0.0204 1.0000 Uani . . . . . . C57 C 0.23738(11) 0.4911(5) 0.27517(17) 0.0225 1.0000 Uani . . . . . . C58 C 0.25942(10) 0.4359(5) 0.25361(18) 0.0214 1.0000 Uani . . . . . . C59 C 0.24309(11) 0.3778(5) 0.20045(18) 0.0215 1.0000 Uani . . . . . . C60 C 0.20590(11) 0.3713(4) 0.17065(17) 0.0213 1.0000 Uani . . . . . . C61 C 0.18423(11) 0.3022(4) 0.11630(17) 0.0209 1.0000 Uani . . . . . . C62 C 0.19917(13) 0.2352(5) 0.08647(19) 0.0291 1.0000 Uani . . . . . . C63 C 0.17682(14) 0.1647(6) 0.0374(2) 0.0360 1.0000 Uani . . . . . . C64 C 0.14023(13) 0.1695(6) 0.01817(19) 0.0317 1.0000 Uani . . . . . . C65 C 0.12693(11) 0.2390(5) 0.04906(18) 0.0259 1.0000 Uani . . . . . . C66 C 0.13672(12) 0.7109(5) 0.11080(19) 0.0262 1.0000 Uani . . . . . . C67 C 0.12230(14) 0.8354(5) 0.0793(2) 0.0340 1.0000 Uani . . . . . . C68 C 0.08646(14) 0.8394(6) 0.0427(2) 0.0364 1.0000 Uani . . . . . . C69 C 0.06471(12) 0.7204(5) 0.0382(2) 0.0300 1.0000 Uani . . . . . . C70 C 0.08060(11) 0.5989(5) 0.07191(17) 0.0214 1.0000 Uani . . . . . . C71 C 0.05922(11) 0.4730(4) 0.07393(16) 0.0185 1.0000 Uani . . . . . . C72 C 0.02275(11) 0.4538(5) 0.04595(17) 0.0227 1.0000 Uani . . . . . . C73 C 0.00694(11) 0.3301(5) 0.05648(18) 0.0227 1.0000 Uani . . . . . . C74 C 0.02960(11) 0.2266(5) 0.09477(18) 0.0235 1.0000 Uani . . . . . . C75 C 0.06643(11) 0.2495(4) 0.12145(16) 0.0196 1.0000 Uani . . . . . . C76 C 0.09428(11) 0.1523(5) 0.16242(17) 0.0226 1.0000 Uani . . . . . . C77 C 0.08652(13) 0.0230(5) 0.1806(2) 0.0313 1.0000 Uani . . . . . . C78 C 0.11436(15) -0.0590(5) 0.2195(3) 0.0412 1.0000 Uani . . . . . . C79 C 0.14908(14) -0.0134(5) 0.2400(2) 0.0361 1.0000 Uani . . . . . . C80 C 0.15529(12) 0.1194(5) 0.22010(19) 0.0269 1.0000 Uani . . . . . . C81 C 0.29871(11) 0.4367(5) 0.28867(18) 0.0231 1.0000 Uani . . . . . . C82 C 0.31823(12) 0.5045(6) 0.3383(2) 0.0290 1.0000 Uani . . . . . . C83 C 0.35561(12) 0.4796(6) 0.3618(2) 0.0337 1.0000 Uani . . . . . . C84 C 0.36390(11) 0.3945(5) 0.3295(2) 0.0282 1.0000 Uani . . . . . . C85 C -0.03194(11) 0.3088(5) 0.02917(18) 0.0244 1.0000 Uani . U . . . . C86 C -0.05165(13) 0.2017(5) 0.0381(2) 0.0317 1.0000 Uani . U . . . . C87 C -0.08912(13) 0.2171(6) 0.0036(2) 0.0370 1.0000 Uani . U . . . . C88 C -0.09722(11) 0.3326(6) -0.0301(2) 0.0346 1.0000 Uani . U . . . . S2 S 0.19751(3) 0.44816(16) -0.02696(5) 0.0339 1.0000 Uani . . . . . . S51 S 0.32661(3) 0.33990(13) 0.27013(5) 0.0277 1.0000 Uani . . . . . . S52 S -0.05989(3) 0.42806(14) -0.02172(6) 0.0351 1.0000 Uani . U . . . . C101 C 0.58080(4) 0.46607(16) 0.32975(6) 0.0332 0.1500 Uani . . . . . . S101 S 0.57607(9) 0.7160(4) 0.28310(16) 0.0371 0.1500 Uani . . . . . . Br1 Br 0.66309(2) 0.50179(9) 0.40251(4) 0.0481 0.8500 Uani . . . . . . Br2 Br 0.113693(19) 0.44859(8) -0.08884(3) 0.0490 1.0000 Uani . . . . . . Br10 Br 0.66116(9) 0.7428(4) 0.3505(2) 0.0509 0.1500 Uani . . . . . . Br51 Br 0.409930(19) 0.33619(7) 0.34378(3) 0.0414 1.0000 Uani . . . . . . Br52 Br -0.142665(19) 0.40120(7) -0.08030(3) 0.0511 1.0000 Uani . U . . . . O1 O 0.23646(12) 0.7726(4) 0.18211(19) 0.0456 1.0000 Uani . . . . . . O2 O 0.20244(12) 0.9608(5) 0.1679(2) 0.0539 1.0000 Uani . . . . . . O3 O 0.48273(14) 0.7918(7) 0.3213(3) 0.0828 1.0000 Uani . . . . . . O4 O 0.5225(2) 0.9220(6) 0.3144(3) 0.0760 1.0000 Uani . . . . . . O5 O 0.42487(13) 0.7147(6) 0.4308(2) 0.0578 1.0000 Uani . . . . . . O6 O 0.47531(13) 0.7899(6) 0.4393(2) 0.0612 1.0000 Uani . . . . . . O7 O 0.7067(2) 0.7888(9) 0.3560(3) 0.0790 0.7000 Uani D U . . . . O8 O 0.7529(3) 0.9214(11) 0.4017(4) 0.0794 0.7000 Uani D U . . . . O9 O 0.8066(6) 0.795(2) 0.4703(9) 0.0878 0.3000 Uani D U . . . . O10 O 0.7700(9) 0.917(2) 0.4067(11) 0.0893 0.3000 Uani D U . . . . P1 P 0.26203(4) 0.89329(14) 0.35718(6) 0.0325 1.0000 Uani D U . . . . P2 P 0.28346(3) 0.04374(14) 0.08866(6) 0.0296 1.0000 Uani D U . . . . P3 P 0.50899(3) 0.23058(13) 0.14333(5) 0.0279 1.0000 Uani D U . . . . P4 P 0.52458(4) 0.2685(2) 0.41718(6) 0.0455 1.0000 Uani D U . . . . F1 F 0.25839(11) 1.0578(3) 0.33679(17) 0.0597 1.0000 Uani D U . . . . F2 F 0.26616(9) 0.7261(3) 0.37748(12) 0.0437 1.0000 Uani D U . . . . F3 F 0.23660(8) 0.8401(3) 0.29507(11) 0.0402 1.0000 Uani D U . . . . F4 F 0.28768(9) 0.9429(4) 0.41921(13) 0.0482 1.0000 Uani D U . . . . F5 F 0.22781(8) 0.9105(4) 0.36629(14) 0.0484 1.0000 Uani D U . . . . F6 F 0.29642(8) 0.8714(4) 0.34774(14) 0.0492 1.0000 Uani D U . . . . F11 F 0.25282(9) 0.1219(4) 0.03580(14) 0.0524 1.0000 Uani D U . . . . F12 F 0.31388(9) -0.0336(4) 0.14250(13) 0.0489 1.0000 Uani D U . . . . F13 F 0.28403(9) 0.1800(3) 0.12611(14) 0.0445 1.0000 Uani D U . . . . F14 F 0.28322(10) -0.0925(4) 0.05244(14) 0.0523 1.0000 Uani D U . . . . F15 F 0.25307(8) -0.0330(4) 0.09938(14) 0.0457 1.0000 Uani D U . . . . F16 F 0.31366(8) 0.1219(4) 0.07880(15) 0.0459 1.0000 Uani D U . . . . F21 F 0.51944(8) 0.0617(3) 0.15693(15) 0.0440 1.0000 Uani D U . . . . F22 F 0.49828(9) 0.4005(3) 0.12947(14) 0.0428 1.0000 Uani D U . . . . F23 F 0.47929(9) 0.1880(4) 0.08229(12) 0.0486 1.0000 Uani D U . . . . F24 F 0.53864(8) 0.2753(3) 0.20394(12) 0.0421 1.0000 Uani D U . . . . F25 F 0.47977(8) 0.2149(3) 0.16408(13) 0.0385 1.0000 Uani D U . . . . F26 F 0.53798(9) 0.2473(4) 0.12212(15) 0.0485 1.0000 Uani D U . . . . F31 F 0.49858(11) 0.3929(5) 0.37845(18) 0.0803 1.0000 Uani D U . . . . F32 F 0.55065(9) 0.1427(4) 0.45535(13) 0.0525 1.0000 Uani D U . . . . F33 F 0.51594(17) 0.3114(7) 0.4648(2) 0.1195 1.0000 Uani D U . . . . F34 F 0.53463(12) 0.2270(5) 0.36977(14) 0.0653 1.0000 Uani D U . . . . F35 F 0.55717(12) 0.3823(5) 0.43976(19) 0.0897 1.0000 Uani D U . . . . F36 F 0.49274(12) 0.1538(6) 0.3924(2) 0.1244 1.0000 Uani D U . . . . H11 H 0.3462 0.8027 0.0793 0.0274 1.0000 Uiso R . . . . . H21 H 0.3608 1.0206 0.0522 0.0391 1.0000 Uiso R . . . . . H31 H 0.4201 1.0861 0.0873 0.0441 1.0000 Uiso R . . . . . H41 H 0.4644 0.9326 0.1480 0.0330 1.0000 Uiso R . . . . . H71 H 0.5049 0.7653 0.2088 0.0283 1.0000 Uiso R . . . . . H91 H 0.5118 0.3792 0.2823 0.0261 1.0000 Uiso R . . . . . H121 H 0.4770 0.1746 0.2767 0.0310 1.0000 Uiso R . . . . . H131 H 0.4378 -0.0146 0.2694 0.0372 1.0000 Uiso R . . . . . H141 H 0.3762 0.0222 0.2172 0.0374 1.0000 Uiso R . . . . . H151 H 0.3551 0.2445 0.1720 0.0300 1.0000 Uiso R . . . . . H161 H 0.4262 0.3976 0.0922 0.0244 1.0000 Uiso R . . . . . H171 H 0.4088 0.2857 0.0077 0.0363 1.0000 Uiso R . . . . . H181 H 0.3484 0.2481 -0.0509 0.0367 1.0000 Uiso R . . . . . H191 H 0.3063 0.3356 -0.0267 0.0304 1.0000 Uiso R . . . . . H221 H 0.2689 0.4316 0.0042 0.0245 1.0000 Uiso R . . . . . H241 H 0.2679 0.6355 0.1336 0.0284 1.0000 Uiso R . . . . . H271 H 0.3053 0.7209 0.2210 0.0355 1.0000 Uiso R . . . . . H281 H 0.3483 0.8140 0.3073 0.0390 1.0000 Uiso R . . . . . H291 H 0.4076 0.7994 0.3298 0.0344 1.0000 Uiso R . . . . . H301 H 0.4254 0.6803 0.2752 0.0290 1.0000 Uiso R . . . . . H321 H 0.5670 0.7990 0.2589 0.0411 1.0000 Uiso . . . . . . H331 H 0.6303 0.7679 0.3291 0.0529 1.0000 Uiso R . . . . . H361 H 0.2073 0.6818 0.0777 0.0502 1.0000 Uiso R . . . . . H371 H 0.1438 0.6440 0.0128 0.0567 1.0000 Uiso R . . . . . H391 H 0.2579 1.0712 0.2388 0.0512 1.0000 Uiso R . . . . . H392 H 0.2732 1.0305 0.1988 0.0512 1.0000 Uiso R . . . . . H393 H 0.2820 0.9352 0.2498 0.0512 1.0000 Uiso R . . . . . H401 H 0.5635 0.7913 0.3948 0.0711 1.0000 Uiso R . . . . . H402 H 0.5398 0.8500 0.4203 0.0711 1.0000 Uiso R . . . . . H403 H 0.5354 0.6882 0.4000 0.0711 1.0000 Uiso R . . . . . H411 H 0.4903 0.5280 0.4633 0.1030 1.0000 Uiso R . . . . . H412 H 0.4893 0.5914 0.5158 0.1030 1.0000 Uiso R . . . . . H413 H 0.4574 0.4947 0.4735 0.1030 1.0000 Uiso R . . . . . H421 H 0.7713 0.7495 0.4704 0.0741 0.7000 Uiso R . . . . . H422 H 0.7520 0.6191 0.4302 0.0741 0.7000 Uiso R . . . . . H423 H 0.7319 0.7075 0.4563 0.0741 0.7000 Uiso R . . . . . H424 H 0.7250 0.7409 0.4146 0.0741 0.3000 Uiso R . . . . . H425 H 0.7536 0.6151 0.4360 0.0741 0.3000 Uiso R . . . . . H426 H 0.7504 0.7223 0.4780 0.0741 0.3000 Uiso R . . . . . H511 H 0.0883 0.5169 0.2084 0.0261 1.0000 Uiso R . . . . . H521 H 0.1008 0.6240 0.2910 0.0322 1.0000 Uiso R . . . . . H531 H 0.1588 0.6832 0.3534 0.0338 1.0000 Uiso R . . . . . H541 H 0.2053 0.6222 0.3342 0.0296 1.0000 Uiso R . . . . . H571 H 0.2478 0.5302 0.3106 0.0236 1.0000 Uiso R . . . . . H591 H 0.2575 0.3445 0.1853 0.0253 1.0000 Uiso R . . . . . H621 H 0.2237 0.2361 0.0997 0.0333 1.0000 Uiso R . . . . . H631 H 0.1860 0.1174 0.0174 0.0421 1.0000 Uiso R . . . . . H641 H 0.1247 0.1269 -0.0153 0.0352 1.0000 Uiso R . . . . . H651 H 0.1025 0.2416 0.0369 0.0282 1.0000 Uiso R . . . . . H661 H 0.1615 0.7058 0.1363 0.0300 1.0000 Uiso R . . . . . H671 H 0.1371 0.9156 0.0825 0.0413 1.0000 Uiso R . . . . . H681 H 0.0766 0.9221 0.0211 0.0449 1.0000 Uiso R . . . . . H691 H 0.0402 0.7204 0.0131 0.0335 1.0000 Uiso R . . . . . H721 H 0.0083 0.5215 0.0195 0.0247 1.0000 Uiso R . . . . . H741 H 0.0195 0.1433 0.1016 0.0269 1.0000 Uiso R . . . . . H771 H 0.0626 -0.0071 0.1669 0.0347 1.0000 Uiso R . . . . . H781 H 0.1098 -0.1455 0.2325 0.0434 1.0000 Uiso R . . . . . H791 H 0.1679 -0.0667 0.2664 0.0384 1.0000 Uiso R . . . . . H801 H 0.1785 0.1509 0.2331 0.0303 1.0000 Uiso R . . . . . H821 H 0.3081 0.5610 0.3556 0.0338 1.0000 Uiso R . . . . . H831 H 0.3732 0.5163 0.3953 0.0345 1.0000 Uiso R . . . . . H861 H -0.0414 0.1280 0.0640 0.0354 1.0000 Uiso R . . . . . H871 H -0.1063 0.1559 0.0044 0.0412 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01554(12) 0.01497(14) 0.01877(13) 0.00157(11) 0.00708(10) -0.00126(11) Ru2 0.01346(12) 0.01522(14) 0.01816(13) 0.00178(12) 0.00545(10) 0.00012(11) N1 0.0274(17) 0.0151(15) 0.0223(16) 0.0018(13) 0.0142(13) 0.0011(13) N2 0.0160(15) 0.0153(15) 0.0204(16) -0.0009(12) 0.0051(12) -0.0031(12) N3 0.0195(15) 0.0169(16) 0.0188(16) 0.0000(12) 0.0080(13) -0.0035(12) N4 0.0239(16) 0.0156(15) 0.0255(17) 0.0052(13) 0.0133(14) 0.0020(12) N5 0.0185(15) 0.0138(15) 0.0200(16) 0.0033(12) 0.0085(13) 0.0005(12) N6 0.0286(17) 0.0161(16) 0.0205(16) -0.0002(12) 0.0120(14) -0.0042(13) N7 0.042(2) 0.031(2) 0.041(2) 0.0030(18) 0.0246(19) -0.0014(18) N8 0.043(3) 0.048(3) 0.066(3) -0.025(3) 0.020(2) 0.006(2) N9 0.042(2) 0.044(2) 0.033(2) -0.0118(18) 0.0178(18) -0.014(2) N10 0.082(4) 0.039(3) 0.047(3) -0.004(3) 0.031(3) 0.008(3) N11 0.107(5) 0.050(6) 0.063(6) -0.019(5) 0.059(5) -0.011(5) N51 0.0205(15) 0.0175(15) 0.0220(17) 0.0049(13) 0.0115(13) 0.0015(12) N52 0.0160(14) 0.0158(15) 0.0216(16) 0.0008(12) 0.0082(13) -0.0023(12) N53 0.0204(15) 0.0195(17) 0.0192(15) 0.0012(12) 0.0086(13) 0.0009(12) N54 0.0196(15) 0.0165(15) 0.0221(16) 0.0057(13) 0.0097(13) -0.0002(12) N55 0.0173(15) 0.0159(15) 0.0205(16) 0.0002(12) 0.0083(13) 0.0017(12) N56 0.0201(15) 0.0143(15) 0.0229(16) 0.0028(13) 0.0083(13) -0.0035(12) C1 0.0219(18) 0.0196(19) 0.030(2) 0.0080(16) 0.0106(16) 0.0022(15) C2 0.038(2) 0.019(2) 0.045(3) 0.0126(19) 0.021(2) 0.0107(18) C3 0.038(2) 0.025(2) 0.057(3) 0.010(2) 0.025(2) -0.0020(19) C4 0.028(2) 0.018(2) 0.041(2) 0.0074(18) 0.0149(18) -0.0035(16) C5 0.0228(17) 0.0144(17) 0.0259(19) -0.0008(15) 0.0130(15) -0.0023(14) C6 0.0262(19) 0.0144(17) 0.028(2) 0.0014(15) 0.0155(16) -0.0014(15) C7 0.0223(18) 0.0194(19) 0.030(2) -0.0020(16) 0.0135(16) -0.0058(15) C8 0.0231(18) 0.022(2) 0.0225(19) -0.0033(15) 0.0108(16) -0.0010(15) C9 0.0205(18) 0.0224(19) 0.0238(19) -0.0021(15) 0.0092(15) -0.0023(15) C10 0.0230(18) 0.0166(18) 0.0198(18) 0.0009(14) 0.0077(15) 0.0024(14) C11 0.0228(17) 0.0191(18) 0.0160(17) 0.0018(14) 0.0075(14) -0.0002(14) C12 0.028(2) 0.023(2) 0.028(2) 0.0051(17) 0.0094(17) 0.0011(16) C13 0.039(2) 0.019(2) 0.034(2) 0.0088(17) 0.0121(19) -0.0004(18) C14 0.041(2) 0.019(2) 0.038(2) 0.0062(18) 0.015(2) -0.0093(19) C15 0.0232(19) 0.023(2) 0.027(2) 0.0083(16) 0.0104(16) -0.0009(16) C16 0.0198(17) 0.0191(18) 0.027(2) 0.0053(15) 0.0093(15) 0.0030(14) C17 0.039(2) 0.0192(18) 0.034(2) 0.0071(17) 0.0248(19) 0.0060(17) C18 0.040(2) 0.025(2) 0.027(2) -0.0010(17) 0.0175(19) 0.0037(18) C19 0.0240(19) 0.027(2) 0.025(2) -0.0025(16) 0.0080(16) 0.0011(16) C20 0.0235(18) 0.0170(18) 0.0207(18) 0.0034(14) 0.0098(15) 0.0008(14) C21 0.0260(19) 0.0155(18) 0.0234(19) -0.0011(15) 0.0132(16) -0.0006(14) C22 0.0231(19) 0.023(2) 0.0193(19) 0.0006(15) 0.0064(15) -0.0010(15) C23 0.0219(19) 0.021(2) 0.030(2) 0.0031(16) 0.0125(17) -0.0030(15) C24 0.0242(18) 0.0207(19) 0.0253(19) -0.0023(16) 0.0138(15) 0.0001(15) C25 0.0258(18) 0.0202(19) 0.0236(19) 0.0015(15) 0.0152(16) 0.0008(15) C26 0.0236(18) 0.0180(18) 0.0232(19) 0.0028(15) 0.0115(15) 0.0009(14) C27 0.031(2) 0.028(2) 0.034(2) -0.0002(18) 0.0192(18) -0.0030(18) C28 0.037(2) 0.032(2) 0.030(2) -0.0050(19) 0.0160(19) 0.0015(19) C29 0.038(2) 0.031(2) 0.020(2) -0.0045(17) 0.0062(18) -0.0060(19) C30 0.0246(19) 0.029(2) 0.024(2) 0.0013(17) 0.0052(16) -0.0076(17) C31 0.0207(18) 0.033(2) 0.031(2) -0.0032(19) 0.0111(17) -0.0024(17) S1 0.0197(5) 0.0331(7) 0.0384(7) 0.0094(6) 0.0070(5) -0.0020(5) C32 0.0288(15) 0.0266(15) 0.0478(19) 0.0069(14) 0.0113(14) -0.0020(12) C33 0.026(2) 0.061(3) 0.053(3) -0.006(3) 0.019(2) -0.019(2) C34 0.020(2) 0.057(3) 0.032(2) -0.001(2) 0.0034(18) 0.004(2) C35 0.0201(18) 0.028(2) 0.026(2) 0.0002(17) 0.0097(16) 0.0010(16) C36 0.024(2) 0.063(4) 0.038(3) -0.020(2) 0.0091(19) 0.005(2) C37 0.028(2) 0.073(4) 0.043(3) -0.012(3) 0.013(2) 0.013(3) C38 0.0129(18) 0.060(3) 0.027(2) 0.000(2) 0.0031(17) 0.0033(19) C39 0.046(3) 0.039(3) 0.044(3) -0.002(2) 0.023(2) -0.005(2) C40 0.052(3) 0.078(4) 0.049(3) -0.001(3) 0.021(3) -0.012(3) C41 0.100(5) 0.052(4) 0.095(5) 0.020(4) 0.029(5) -0.001(4) C42 0.085(4) 0.039(3) 0.051(3) -0.001(2) 0.036(3) 0.000(3) C51 0.0215(18) 0.0189(19) 0.029(2) 0.0033(15) 0.0118(16) 0.0033(14) C52 0.030(2) 0.024(2) 0.031(2) 0.0055(17) 0.0188(18) 0.0060(16) C53 0.033(2) 0.025(2) 0.024(2) -0.0024(16) 0.0169(17) -0.0010(16) C54 0.0278(19) 0.023(2) 0.024(2) 0.0007(16) 0.0099(16) 0.0006(16) C55 0.0242(18) 0.0157(18) 0.027(2) 0.0017(15) 0.0157(16) -0.0001(14) C56 0.0211(18) 0.0191(18) 0.0230(19) -0.0011(15) 0.0120(15) -0.0013(14) C57 0.0192(17) 0.023(2) 0.0185(18) -0.0031(14) 0.0037(14) -0.0029(14) C58 0.0135(16) 0.0170(18) 0.028(2) 0.0012(15) 0.0055(15) -0.0025(13) C59 0.0187(17) 0.024(2) 0.0259(19) 0.0008(15) 0.0138(15) 0.0017(14) C60 0.0251(19) 0.0163(18) 0.0220(19) 0.0019(14) 0.0105(15) -0.0007(14) C61 0.0205(17) 0.0199(19) 0.0201(18) 0.0009(14) 0.0076(14) 0.0015(14) C62 0.028(2) 0.031(2) 0.028(2) 0.0023(17) 0.0122(17) 0.0040(17) C63 0.037(2) 0.044(3) 0.027(2) -0.009(2) 0.0145(19) 0.001(2) C64 0.032(2) 0.035(2) 0.023(2) -0.0081(18) 0.0089(17) -0.0032(19) C65 0.0195(18) 0.028(2) 0.025(2) -0.0005(17) 0.0063(16) -0.0026(16) C66 0.0238(19) 0.023(2) 0.030(2) 0.0090(17) 0.0112(16) -0.0027(16) C67 0.039(2) 0.021(2) 0.043(3) 0.0086(19) 0.020(2) -0.0025(18) C68 0.038(2) 0.029(2) 0.045(3) 0.021(2) 0.022(2) 0.005(2) C69 0.026(2) 0.025(2) 0.034(2) 0.0149(18) 0.0099(17) 0.0050(17) C70 0.0250(18) 0.0185(18) 0.0204(18) 0.0041(15) 0.0104(15) 0.0046(15) C71 0.0214(17) 0.0187(18) 0.0150(16) 0.0002(14) 0.0083(14) -0.0017(14) C72 0.0239(18) 0.0229(19) 0.0173(17) 0.0015(15) 0.0064(15) 0.0053(15) C73 0.0192(17) 0.0216(19) 0.0257(19) -0.0070(16) 0.0094(15) -0.0023(15) C74 0.0210(18) 0.0192(18) 0.028(2) 0.0015(16) 0.0102(16) 0.0000(15) C75 0.0215(17) 0.0159(18) 0.0190(18) -0.0004(14) 0.0076(15) -0.0007(14) C76 0.0221(18) 0.0203(19) 0.0209(18) 0.0031(15) 0.0066(15) 0.0019(15) C77 0.025(2) 0.019(2) 0.042(3) 0.0046(18) 0.0092(19) -0.0067(16) C78 0.038(2) 0.018(2) 0.055(3) 0.018(2) 0.012(2) -0.0003(18) C79 0.033(2) 0.026(2) 0.040(3) 0.017(2) 0.010(2) 0.0077(18) C80 0.0205(18) 0.023(2) 0.033(2) 0.0064(17) 0.0094(17) 0.0043(16) C81 0.0162(17) 0.023(2) 0.028(2) 0.0005(16) 0.0085(15) 0.0012(14) C82 0.0219(19) 0.035(2) 0.029(2) -0.0047(18) 0.0108(17) 0.0011(17) C83 0.0199(19) 0.046(3) 0.027(2) -0.008(2) 0.0048(16) -0.0030(18) C84 0.0115(16) 0.036(2) 0.033(2) 0.0031(18) 0.0064(16) 0.0014(16) C85 0.0189(17) 0.0242(19) 0.0264(19) -0.0026(15) 0.0075(14) 0.0015(14) C86 0.0252(18) 0.029(2) 0.037(2) 0.0018(18) 0.0120(17) -0.0024(16) C87 0.0234(19) 0.035(2) 0.048(3) -0.0023(19) 0.0132(18) -0.0051(17) C88 0.0127(15) 0.031(2) 0.046(2) -0.0067(17) 0.0016(16) 0.0018(15) S2 0.0177(5) 0.0513(7) 0.0292(6) -0.0083(5) 0.0084(4) -0.0020(5) S51 0.0181(4) 0.0319(6) 0.0294(5) -0.0031(4) 0.0082(4) 0.0024(4) S52 0.0192(5) 0.0303(6) 0.0420(6) 0.0060(5) 0.0030(4) 0.0006(4) C101 0.0197(5) 0.0331(7) 0.0384(7) 0.0094(6) 0.0070(5) -0.0020(5) S101 0.0288(15) 0.0266(15) 0.0478(19) 0.0069(14) 0.0113(14) -0.0020(12) Br1 0.0208(3) 0.0595(4) 0.0481(4) 0.0105(3) 0.0033(2) 0.0000(3) Br2 0.0189(2) 0.0904(5) 0.0315(3) -0.0077(3) 0.00668(19) -0.0033(2) Br10 0.0265(15) 0.0392(19) 0.076(3) 0.0048(18) 0.0150(16) -0.0065(13) Br51 0.0195(2) 0.0589(3) 0.0408(3) 0.0002(2) 0.01024(19) 0.0087(2) Br52 0.0191(2) 0.0444(3) 0.0658(4) -0.0080(3) 0.0004(2) 0.0077(2) O1 0.057(2) 0.0301(19) 0.057(2) -0.0112(17) 0.033(2) -0.0054(17) O2 0.041(2) 0.054(3) 0.061(3) 0.011(2) 0.0198(19) 0.0063(19) O3 0.040(2) 0.088(4) 0.092(4) -0.033(3) 0.007(2) -0.002(3) O4 0.111(4) 0.051(3) 0.072(3) 0.001(2) 0.048(3) 0.013(3) O5 0.050(2) 0.076(3) 0.052(2) -0.019(2) 0.028(2) -0.018(2) O6 0.051(2) 0.056(3) 0.076(3) 0.000(2) 0.030(2) -0.014(2) O7 0.099(4) 0.053(4) 0.055(4) 0.011(3) 0.012(3) 0.017(4) O8 0.104(5) 0.067(5) 0.068(4) 0.017(4) 0.041(5) -0.014(4) O9 0.109(6) 0.066(7) 0.087(7) -0.021(6) 0.045(6) -0.009(7) O10 0.140(6) 0.066(7) 0.081(7) 0.001(6) 0.067(7) -0.010(8) P1 0.0294(6) 0.0289(6) 0.0382(6) -0.0061(5) 0.0150(5) -0.0031(5) P2 0.0284(5) 0.0281(6) 0.0335(6) -0.0002(5) 0.0154(5) 0.0021(5) P3 0.0253(5) 0.0237(5) 0.0387(6) -0.0106(5) 0.0185(5) -0.0068(4) P4 0.0361(7) 0.0685(10) 0.0332(7) 0.0166(7) 0.0176(6) 0.0127(7) F1 0.078(2) 0.0291(16) 0.072(2) 0.0044(16) 0.035(2) -0.0033(16) F2 0.0499(17) 0.0314(15) 0.0378(16) -0.0021(12) 0.0109(14) -0.0018(13) F3 0.0369(15) 0.0424(16) 0.0332(15) -0.0017(12) 0.0099(12) -0.0042(13) F4 0.0430(17) 0.0514(19) 0.0444(17) -0.0191(15) 0.0159(14) -0.0115(14) F5 0.0376(16) 0.057(2) 0.0538(19) -0.0103(16) 0.0241(15) 0.0000(15) F6 0.0359(16) 0.060(2) 0.0540(19) -0.0116(16) 0.0234(15) -0.0057(14) F11 0.0430(17) 0.060(2) 0.0479(18) 0.0164(15) 0.0165(15) 0.0144(15) F12 0.0441(17) 0.0461(18) 0.0455(18) 0.0083(15) 0.0122(14) 0.0059(15) F13 0.0427(16) 0.0410(18) 0.0562(19) -0.0170(14) 0.0285(15) -0.0029(14) F14 0.0548(19) 0.0468(18) 0.0536(19) -0.0217(16) 0.0241(16) 0.0013(16) F15 0.0426(16) 0.0439(17) 0.0548(19) -0.0058(15) 0.0265(15) -0.0142(14) F16 0.0423(16) 0.0459(17) 0.062(2) 0.0059(15) 0.0353(16) 0.0006(14) F21 0.0416(16) 0.0237(13) 0.069(2) -0.0075(13) 0.0283(16) -0.0009(12) F22 0.0475(17) 0.0243(14) 0.0551(19) 0.0002(13) 0.0231(15) -0.0015(12) F23 0.0478(18) 0.0501(19) 0.0434(17) -0.0158(15) 0.0178(14) -0.0125(15) F24 0.0353(15) 0.0411(16) 0.0434(16) -0.0127(13) 0.0133(13) -0.0069(13) F25 0.0349(14) 0.0347(15) 0.0591(18) -0.0110(13) 0.0330(14) -0.0086(12) F26 0.0480(17) 0.0460(18) 0.072(2) -0.0217(16) 0.0450(17) -0.0176(15) F31 0.064(2) 0.103(3) 0.073(3) 0.045(2) 0.032(2) 0.041(2) F32 0.0523(19) 0.056(2) 0.0386(17) 0.0073(15) 0.0127(15) 0.0081(16) F33 0.170(4) 0.140(4) 0.092(3) 0.048(3) 0.097(3) 0.084(4) F34 0.082(3) 0.072(2) 0.0419(19) 0.0014(18) 0.0289(18) 0.009(2) F35 0.085(3) 0.061(3) 0.069(3) 0.004(2) -0.008(2) -0.010(2) F36 0.052(2) 0.149(4) 0.127(4) 0.070(3) 0.005(3) -0.030(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4387(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . N1 . 2.082(3) yes Ru1 . N2 . 1.966(3) yes Ru1 . N3 . 2.070(3) yes Ru1 . N4 . 2.069(4) yes Ru1 . N5 . 1.962(3) yes Ru1 . N6 . 2.074(4) yes Ru2 . N51 . 2.059(4) yes Ru2 . N52 . 1.968(3) yes Ru2 . N53 . 2.071(3) yes Ru2 . N54 . 2.076(3) yes Ru2 . N55 . 1.963(3) yes Ru2 . N56 . 2.073(3) yes N1 . C1 . 1.335(5) yes N1 . C5 . 1.356(5) yes N2 . C6 . 1.359(5) yes N2 . C10 . 1.363(5) yes N3 . C11 . 1.366(5) yes N3 . C15 . 1.340(5) yes N4 . C16 . 1.345(5) yes N4 . C20 . 1.366(5) yes N5 . C21 . 1.358(5) yes N5 . C25 . 1.360(5) yes N6 . C26 . 1.353(5) yes N6 . C30 . 1.353(6) yes N7 . C39 . 1.479(7) yes N7 . O1 . 1.229(6) yes N7 . O2 . 1.207(6) yes N8 . C40 . 1.449(9) yes N8 . O3 . 1.200(8) yes N8 . O4 . 1.231(9) yes N9 . C41 . 1.442(10) yes N9 . O5 . 1.227(7) yes N9 . O6 . 1.231(7) yes N10 . C42 . 1.451(10) yes N10 . O7 . 1.200(7) yes N10 . O8 . 1.200(8) yes N11 . C42 . 1.50(2) yes N11 . O9 . 1.219(9) yes N11 . O10 . 1.207(9) yes N51 . C51 . 1.359(5) yes N51 . C55 . 1.366(5) yes N52 . C56 . 1.357(5) yes N52 . C60 . 1.352(5) yes N53 . C61 . 1.359(5) yes N53 . C65 . 1.341(6) yes N54 . C66 . 1.345(5) yes N54 . C70 . 1.348(5) yes N55 . C71 . 1.368(5) yes N55 . C75 . 1.358(5) yes N56 . C76 . 1.363(5) yes N56 . C80 . 1.328(5) yes C1 . C2 . 1.388(6) yes C1 . H11 . 0.934 no C2 . C3 . 1.369(7) yes C2 . H21 . 0.924 no C3 . C4 . 1.381(7) yes C3 . H31 . 0.915 no C4 . C5 . 1.393(6) yes C4 . H41 . 0.917 no C5 . C6 . 1.477(6) yes C6 . C7 . 1.369(6) yes C7 . C8 . 1.397(6) yes C7 . H71 . 0.930 no C8 . C9 . 1.391(6) yes C8 . C31 . 1.468(6) yes C9 . C10 . 1.375(6) yes C9 . H91 . 0.932 no C10 . C11 . 1.481(6) yes C11 . C12 . 1.385(6) yes C12 . C13 . 1.393(7) yes C12 . H121 . 0.927 no C13 . C14 . 1.381(7) yes C13 . H131 . 0.928 no C14 . C15 . 1.387(6) yes C14 . H141 . 0.933 no C15 . H151 . 0.947 no C16 . C17 . 1.387(7) yes C16 . H161 . 0.924 no C17 . C18 . 1.363(7) yes C17 . H171 . 0.934 no C18 . C19 . 1.389(6) yes C18 . H181 . 0.919 no C19 . C20 . 1.391(6) yes C19 . H191 . 0.928 no C20 . C21 . 1.480(6) yes C21 . C22 . 1.372(6) yes C22 . C23 . 1.404(6) yes C22 . H221 . 0.922 no C23 . C24 . 1.414(6) yes C23 . C35 . 1.457(6) yes C24 . C25 . 1.379(6) yes C24 . H241 . 0.926 no C25 . C26 . 1.484(6) yes C26 . C27 . 1.389(6) yes C27 . C28 . 1.394(7) yes C27 . H271 . 0.932 no C28 . C29 . 1.371(7) yes C28 . H281 . 0.925 no C29 . C30 . 1.361(7) yes C29 . H291 . 0.911 no C30 . H301 . 0.921 no C31 . S1 . 1.704(5) yes C31 . C32 . 1.455(6) yes S1 . C34 . 1.690(6) yes C32 . C33 . 1.392(7) yes C32 . H321 . 0.963 no C33 . C34 . 1.344(9) yes C33 . Br10 . 1.892(6) yes C33 . H331 . 0.960 no C34 . Br1 . 1.873(5) yes C35 . C36 . 1.375(7) yes C35 . S2 . 1.720(5) yes C36 . C37 . 1.418(7) yes C36 . H361 . 0.928 no C37 . C38 . 1.342(8) yes C37 . H371 . 0.930 no C38 . S2 . 1.720(5) yes C38 . Br2 . 1.860(5) yes C39 . H391 . 0.959 no C39 . H392 . 0.956 no C39 . H393 . 0.950 no C40 . H401 . 0.973 no C40 . H402 . 0.947 no C40 . H403 . 0.957 no C41 . H411 . 0.964 no C41 . H412 . 0.970 no C41 . H413 . 0.959 no C42 . H421 . 0.960 no C42 . H422 . 0.960 no C42 . H423 . 0.960 no C42 . H424 . 0.960 no C42 . H425 . 0.960 no C42 . H426 . 0.960 no C51 . C52 . 1.370(6) yes C51 . H511 . 0.933 no C52 . C53 . 1.381(6) yes C52 . H521 . 0.917 no C53 . C54 . 1.381(6) yes C53 . H531 . 0.920 no C54 . C55 . 1.392(6) yes C54 . H541 . 0.931 no C55 . C56 . 1.474(6) yes C56 . C57 . 1.376(6) yes C57 . C58 . 1.412(6) yes C57 . H571 . 0.930 no C58 . C59 . 1.394(6) yes C58 . C81 . 1.474(5) yes C59 . C60 . 1.388(6) yes C59 . H591 . 0.936 no C60 . C61 . 1.476(6) yes C61 . C62 . 1.391(6) yes C62 . C63 . 1.388(7) yes C62 . H621 . 0.922 no C63 . C64 . 1.378(7) yes C63 . H631 . 0.916 no C64 . C65 . 1.375(7) yes C64 . H641 . 0.927 no C65 . H651 . 0.921 no C66 . C67 . 1.385(6) yes C66 . H661 . 0.945 no C67 . C68 . 1.366(7) yes C67 . H671 . 0.940 no C68 . C69 . 1.391(7) yes C68 . H681 . 0.929 no C69 . C70 . 1.399(6) yes C69 . H691 . 0.933 no C70 . C71 . 1.480(6) yes C71 . C72 . 1.370(6) yes C72 . C73 . 1.411(6) yes C72 . H721 . 0.929 no C73 . C74 . 1.403(6) yes C73 . C85 . 1.461(6) yes C74 . C75 . 1.387(6) yes C74 . H741 . 0.935 no C75 . C76 . 1.480(5) yes C76 . C77 . 1.381(6) yes C77 . C78 . 1.379(7) yes C77 . H771 . 0.936 no C78 . C79 . 1.364(8) yes C78 . H781 . 0.925 no C79 . C80 . 1.407(7) yes C79 . H791 . 0.922 no C80 . H801 . 0.917 no C81 . C82 . 1.366(6) yes C81 . S51 . 1.732(4) yes C82 . C83 . 1.414(6) yes C82 . H821 . 0.931 no C83 . C84 . 1.345(7) yes C83 . H831 . 0.932 no C84 . S51 . 1.722(5) yes C84 . Br51 . 1.870(4) yes C85 . C86 . 1.380(6) yes C85 . S52 . 1.726(4) yes C86 . C87 . 1.417(7) yes C86 . H861 . 0.926 no C87 . C88 . 1.338(8) yes C87 . H871 . 0.927 no C88 . S52 . 1.720(5) yes C88 . Br52 . 1.865(4) yes P1 . F1 . 1.586(3) yes P1 . F2 . 1.608(3) yes P1 . F3 . 1.604(3) yes P1 . F4 . 1.595(3) yes P1 . F5 . 1.587(3) yes P1 . F6 . 1.604(3) yes P2 . F11 . 1.588(3) yes P2 . F12 . 1.596(3) yes P2 . F13 . 1.608(3) yes P2 . F14 . 1.592(3) yes P2 . F15 . 1.607(3) yes P2 . F16 . 1.593(3) yes P3 . F21 . 1.601(3) yes P3 . F22 . 1.612(3) yes P3 . F23 . 1.598(3) yes P3 . F24 . 1.594(3) yes P3 . F25 . 1.592(3) yes P3 . F26 . 1.593(3) yes P4 . F31 . 1.590(4) yes P4 . F32 . 1.595(3) yes P4 . F33 . 1.567(4) yes P4 . F34 . 1.596(4) yes P4 . F35 . 1.599(4) yes P4 . F36 . 1.583(4) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 79.19(14) yes N1 . Ru1 . N3 . 157.94(13) yes N2 . Ru1 . N3 . 78.79(14) yes N1 . Ru1 . N4 . 92.42(14) yes N2 . Ru1 . N4 . 102.18(14) yes N3 . Ru1 . N4 . 90.94(13) yes N1 . Ru1 . N5 . 99.67(14) yes N2 . Ru1 . N5 . 178.34(14) yes N3 . Ru1 . N5 . 102.37(13) yes N4 . Ru1 . N5 . 79.04(14) yes N1 . Ru1 . N6 . 91.07(13) yes N2 . Ru1 . N6 . 99.92(15) yes N3 . Ru1 . N6 . 93.97(14) yes N4 . Ru1 . N6 . 157.89(14) yes N5 . Ru1 . N6 . 78.85(15) yes N51 . Ru2 . N52 . 79.06(14) yes N51 . Ru2 . N53 . 158.22(13) yes N52 . Ru2 . N53 . 79.22(14) yes N51 . Ru2 . N54 . 91.96(14) yes N52 . Ru2 . N54 . 102.53(14) yes N53 . Ru2 . N54 . 94.24(14) yes N51 . Ru2 . N55 . 101.27(14) yes N52 . Ru2 . N55 . 178.57(15) yes N53 . Ru2 . N55 . 100.41(14) yes N54 . Ru2 . N55 . 78.87(14) yes N51 . Ru2 . N56 . 90.01(14) yes N52 . Ru2 . N56 . 99.25(14) yes N53 . Ru2 . N56 . 91.94(14) yes N54 . Ru2 . N56 . 158.11(13) yes N55 . Ru2 . N56 . 79.37(14) yes Ru1 . N1 . C1 . 127.4(3) yes Ru1 . N1 . C5 . 112.9(3) yes C1 . N1 . C5 . 119.6(4) yes Ru1 . N2 . C6 . 119.8(3) yes Ru1 . N2 . C10 . 120.1(3) yes C6 . N2 . C10 . 120.0(4) yes Ru1 . N3 . C11 . 114.3(3) yes Ru1 . N3 . C15 . 127.2(3) yes C11 . N3 . C15 . 118.3(4) yes Ru1 . N4 . C16 . 127.5(3) yes Ru1 . N4 . C20 . 113.8(3) yes C16 . N4 . C20 . 118.7(4) yes Ru1 . N5 . C21 . 120.1(3) yes Ru1 . N5 . C25 . 120.0(3) yes C21 . N5 . C25 . 119.8(4) yes Ru1 . N6 . C26 . 114.2(3) yes Ru1 . N6 . C30 . 127.2(3) yes C26 . N6 . C30 . 118.6(4) yes C39 . N7 . O1 . 116.9(5) yes C39 . N7 . O2 . 118.6(5) yes O1 . N7 . O2 . 124.4(5) yes C40 . N8 . O3 . 119.3(7) yes C40 . N8 . O4 . 117.4(6) yes O3 . N8 . O4 . 123.3(7) yes C41 . N9 . O5 . 120.5(6) yes C41 . N9 . O6 . 118.1(6) yes O5 . N9 . O6 . 121.4(6) yes C42 . N10 . O7 . 119.3(8) yes C42 . N10 . O8 . 115.4(8) yes O7 . N10 . O8 . 125.2(9) yes C42 . N11 . O9 . 116.0(18) yes C42 . N11 . O10 . 130(2) yes O9 . N11 . O10 . 114(3) yes Ru2 . N51 . C51 . 126.6(3) yes Ru2 . N51 . C55 . 114.2(3) yes C51 . N51 . C55 . 119.2(4) yes Ru2 . N52 . C56 . 119.4(3) yes Ru2 . N52 . C60 . 119.1(3) yes C56 . N52 . C60 . 121.2(4) yes Ru2 . N53 . C61 . 113.7(3) yes Ru2 . N53 . C65 . 127.8(3) yes C61 . N53 . C65 . 118.5(4) yes Ru2 . N54 . C66 . 126.7(3) yes Ru2 . N54 . C70 . 113.7(3) yes C66 . N54 . C70 . 119.6(4) yes Ru2 . N55 . C71 . 120.0(3) yes Ru2 . N55 . C75 . 119.5(3) yes C71 . N55 . C75 . 120.5(3) yes Ru2 . N56 . C76 . 113.5(3) yes Ru2 . N56 . C80 . 127.3(3) yes C76 . N56 . C80 . 119.2(4) yes N1 . C1 . C2 . 121.7(4) yes N1 . C1 . H11 . 118.7 no C2 . C1 . H11 . 119.5 no C1 . C2 . C3 . 119.2(4) yes C1 . C2 . H21 . 119.9 no C3 . C2 . H21 . 120.9 no C2 . C3 . C4 . 119.6(5) yes C2 . C3 . H31 . 119.6 no C4 . C3 . H31 . 120.8 no C3 . C4 . C5 . 119.1(4) yes C3 . C4 . H41 . 119.7 no C5 . C4 . H41 . 121.3 no C4 . C5 . N1 . 120.8(4) yes C4 . C5 . C6 . 122.5(4) yes N1 . C5 . C6 . 116.7(3) yes C5 . C6 . N2 . 111.4(4) yes C5 . C6 . C7 . 127.8(4) yes N2 . C6 . C7 . 120.8(4) yes C6 . C7 . C8 . 120.1(4) yes C6 . C7 . H71 . 120.1 no C8 . C7 . H71 . 119.9 no C7 . C8 . C9 . 118.4(4) yes C7 . C8 . C31 . 120.0(4) yes C9 . C8 . C31 . 121.6(4) yes C8 . C9 . C10 . 120.0(4) yes C8 . C9 . H91 . 118.7 no C10 . C9 . H91 . 121.2 no C9 . C10 . N2 . 120.7(4) yes C9 . C10 . C11 . 127.9(4) yes N2 . C10 . C11 . 111.5(3) yes C10 . C11 . N3 . 115.2(3) yes C10 . C11 . C12 . 123.1(4) yes N3 . C11 . C12 . 121.7(4) yes C11 . C12 . C13 . 119.1(4) yes C11 . C12 . H121 . 120.1 no C13 . C12 . H121 . 120.8 no C12 . C13 . C14 . 119.0(4) yes C12 . C13 . H131 . 120.2 no C14 . C13 . H131 . 120.8 no C13 . C14 . C15 . 119.1(4) yes C13 . C14 . H141 . 120.4 no C15 . C14 . H141 . 120.5 no C14 . C15 . N3 . 122.7(4) yes C14 . C15 . H151 . 119.6 no N3 . C15 . H151 . 117.8 no N4 . C16 . C17 . 121.8(4) yes N4 . C16 . H161 . 118.1 no C17 . C16 . H161 . 120.1 no C16 . C17 . C18 . 120.0(4) yes C16 . C17 . H171 . 120.2 no C18 . C17 . H171 . 119.8 no C17 . C18 . C19 . 119.1(4) yes C17 . C18 . H181 . 121.7 no C19 . C18 . H181 . 119.2 no C18 . C19 . C20 . 119.3(4) yes C18 . C19 . H191 . 121.0 no C20 . C19 . H191 . 119.7 no C19 . C20 . N4 . 121.2(4) yes C19 . C20 . C21 . 123.4(4) yes N4 . C20 . C21 . 115.5(4) yes C20 . C21 . N5 . 111.5(4) yes C20 . C21 . C22 . 127.1(4) yes N5 . C21 . C22 . 121.4(4) yes C21 . C22 . C23 . 119.9(4) yes C21 . C22 . H221 . 119.8 no C23 . C22 . H221 . 120.2 no C22 . C23 . C24 . 118.2(4) yes C22 . C23 . C35 . 121.5(4) yes C24 . C23 . C35 . 120.3(4) yes C23 . C24 . C25 . 119.1(4) yes C23 . C24 . H241 . 120.0 no C25 . C24 . H241 . 120.9 no C24 . C25 . N5 . 121.6(4) yes C24 . C25 . C26 . 126.8(4) yes N5 . C25 . C26 . 111.5(4) yes C25 . C26 . N6 . 115.4(4) yes C25 . C26 . C27 . 123.1(4) yes N6 . C26 . C27 . 121.5(4) yes C26 . C27 . C28 . 119.0(4) yes C26 . C27 . H271 . 120.2 no C28 . C27 . H271 . 120.8 no C27 . C28 . C29 . 118.3(4) yes C27 . C28 . H281 . 122.1 no C29 . C28 . H281 . 119.5 no C28 . C29 . C30 . 120.6(4) yes C28 . C29 . H291 . 120.0 no C30 . C29 . H291 . 119.4 no C29 . C30 . N6 . 121.8(4) yes C29 . C30 . H301 . 119.0 no N6 . C30 . H301 . 119.2 no C8 . C31 . S1 . 121.8(4) yes C8 . C31 . C32 . 128.8(4) yes S1 . C31 . C32 . 109.3(3) yes C31 . S1 . C34 . 92.5(3) yes C31 . C32 . C33 . 111.4(4) yes C31 . C32 . H321 . 124.2 no C33 . C32 . H321 . 124.4 no C32 . C33 . C34 . 113.0(4) yes C32 . C33 . Br10 . 150.9(5) yes C34 . C33 . Br10 . 94.3(4) yes C32 . C33 . H331 . 123.6 no C34 . C33 . H331 . 123.3 no S1 . C34 . C33 . 113.7(4) yes S1 . C34 . Br1 . 121.0(4) yes C33 . C34 . Br1 . 125.4(4) yes C23 . C35 . C36 . 128.3(4) yes C23 . C35 . S2 . 121.3(3) yes C36 . C35 . S2 . 110.4(3) yes C35 . C36 . C37 . 113.3(5) yes C35 . C36 . H361 . 123.8 no C37 . C36 . H361 . 123.0 no C36 . C37 . C38 . 112.3(5) yes C36 . C37 . H371 . 124.3 no C38 . C37 . H371 . 123.4 no C37 . C38 . S2 . 112.3(4) yes C37 . C38 . Br2 . 126.3(4) yes S2 . C38 . Br2 . 121.3(3) yes N7 . C39 . H391 . 110.4 no N7 . C39 . H392 . 110.2 no H391 . C39 . H392 . 109.3 no N7 . C39 . H393 . 111.1 no H391 . C39 . H393 . 107.9 no H392 . C39 . H393 . 107.9 no N8 . C40 . H401 . 109.2 no N8 . C40 . H402 . 108.3 no H401 . C40 . H402 . 108.9 no N8 . C40 . H403 . 111.2 no H401 . C40 . H403 . 109.2 no H402 . C40 . H403 . 110.0 no N9 . C41 . H411 . 109.7 no N9 . C41 . H412 . 109.3 no H411 . C41 . H412 . 109.2 no N9 . C41 . H413 . 109.6 no H411 . C41 . H413 . 109.8 no H412 . C41 . H413 . 109.2 no N10 . C42 . H421 . 109.5 no N10 . C42 . H422 . 109.3 no H421 . C42 . H422 . 109.5 no N10 . C42 . H423 . 109.6 no H421 . C42 . H423 . 109.5 no H422 . C42 . H423 . 109.5 no N11 . C42 . H424 . 108.6 no N11 . C42 . H425 . 108.8 no N11 . C42 . H426 . 111.0 no H424 . C42 . H425 . 109.5 no H424 . C42 . H426 . 109.5 no H425 . C42 . H426 . 109.5 no N51 . C51 . C52 . 121.5(4) yes N51 . C51 . H511 . 119.1 no C52 . C51 . H511 . 119.4 no C51 . C52 . C53 . 119.9(4) yes C51 . C52 . H521 . 120.4 no C53 . C52 . H521 . 119.7 no C52 . C53 . C54 . 119.1(4) yes C52 . C53 . H531 . 119.8 no C54 . C53 . H531 . 121.1 no C53 . C54 . C55 . 119.6(4) yes C53 . C54 . H541 . 120.7 no C55 . C54 . H541 . 119.7 no C54 . C55 . N51 . 120.6(4) yes C54 . C55 . C56 . 124.3(4) yes N51 . C55 . C56 . 115.1(4) yes C55 . C56 . N52 . 112.1(4) yes C55 . C56 . C57 . 127.1(4) yes N52 . C56 . C57 . 120.7(4) yes C56 . C57 . C58 . 119.4(4) yes C56 . C57 . H571 . 120.8 no C58 . C57 . H571 . 119.8 no C57 . C58 . C59 . 118.6(4) yes C57 . C58 . C81 . 119.0(4) yes C59 . C58 . C81 . 122.3(4) yes C58 . C59 . C60 . 119.8(4) yes C58 . C59 . H591 . 119.1 no C60 . C59 . H591 . 121.1 no C59 . C60 . N52 . 120.3(4) yes C59 . C60 . C61 . 127.1(4) yes N52 . C60 . C61 . 112.5(4) yes C60 . C61 . N53 . 115.4(4) yes C60 . C61 . C62 . 123.2(4) yes N53 . C61 . C62 . 121.3(4) yes C61 . C62 . C63 . 119.3(4) yes C61 . C62 . H621 . 120.2 no C63 . C62 . H621 . 120.6 no C62 . C63 . C64 . 118.8(5) yes C62 . C63 . H631 . 121.1 no C64 . C63 . H631 . 120.1 no C63 . C64 . C65 . 119.3(4) yes C63 . C64 . H641 . 120.5 no C65 . C64 . H641 . 120.2 no C64 . C65 . N53 . 122.7(4) yes C64 . C65 . H651 . 120.0 no N53 . C65 . H651 . 117.3 no N54 . C66 . C67 . 121.5(4) yes N54 . C66 . H661 . 117.8 no C67 . C66 . H661 . 120.7 no C66 . C67 . C68 . 119.3(4) yes C66 . C67 . H671 . 120.3 no C68 . C67 . H671 . 120.3 no C67 . C68 . C69 . 120.0(4) yes C67 . C68 . H681 . 119.9 no C69 . C68 . H681 . 120.1 no C68 . C69 . C70 . 118.1(4) yes C68 . C69 . H691 . 121.4 no C70 . C69 . H691 . 120.5 no C69 . C70 . N54 . 121.3(4) yes C69 . C70 . C71 . 122.2(4) yes N54 . C70 . C71 . 116.4(3) yes C70 . C71 . N55 . 110.8(3) yes C70 . C71 . C72 . 128.5(4) yes N55 . C71 . C72 . 120.6(4) yes C71 . C72 . C73 . 120.2(4) yes C71 . C72 . H721 . 120.1 no C73 . C72 . H721 . 119.7 no C72 . C73 . C74 . 118.2(4) yes C72 . C73 . C85 . 121.8(4) yes C74 . C73 . C85 . 119.9(4) yes C73 . C74 . C75 . 119.5(4) yes C73 . C74 . H741 . 119.0 no C75 . C74 . H741 . 121.5 no C74 . C75 . N55 . 120.9(4) yes C74 . C75 . C76 . 127.0(4) yes N55 . C75 . C76 . 112.1(3) yes C75 . C76 . N56 . 115.6(4) yes C75 . C76 . C77 . 123.3(4) yes N56 . C76 . C77 . 121.1(4) yes C76 . C77 . C78 . 119.0(4) yes C76 . C77 . H771 . 120.1 no C78 . C77 . H771 . 120.9 no C77 . C78 . C79 . 120.7(4) yes C77 . C78 . H781 . 120.5 no C79 . C78 . H781 . 118.7 no C78 . C79 . C80 . 117.7(4) yes C78 . C79 . H791 . 121.5 no C80 . C79 . H791 . 120.8 no C79 . C80 . N56 . 122.4(4) yes C79 . C80 . H801 . 118.7 no N56 . C80 . H801 . 118.9 no C58 . C81 . C82 . 128.2(4) yes C58 . C81 . S51 . 121.2(3) yes C82 . C81 . S51 . 110.7(3) yes C81 . C82 . C83 . 113.6(4) yes C81 . C82 . H821 . 123.9 no C83 . C82 . H821 . 122.6 no C82 . C83 . C84 . 112.0(4) yes C82 . C83 . H831 . 126.1 no C84 . C83 . H831 . 121.8 no C83 . C84 . S51 . 112.7(3) yes C83 . C84 . Br51 . 126.5(4) yes S51 . C84 . Br51 . 120.8(3) yes C73 . C85 . C86 . 129.0(4) yes C73 . C85 . S52 . 120.3(3) yes C86 . C85 . S52 . 110.7(3) yes C85 . C86 . C87 . 112.8(4) yes C85 . C86 . H861 . 123.4 no C87 . C86 . H861 . 123.8 no C86 . C87 . C88 . 112.4(4) yes C86 . C87 . H871 . 124.4 no C88 . C87 . H871 . 123.1 no C87 . C88 . S52 . 112.9(3) yes C87 . C88 . Br52 . 127.9(4) yes S52 . C88 . Br52 . 119.1(3) yes C38 . S2 . C35 . 91.7(2) yes C81 . S51 . C84 . 91.0(2) yes C85 . S52 . C88 . 91.2(2) yes F1 . P1 . F2 . 179.1(2) yes F1 . P1 . F3 . 90.36(19) yes F2 . P1 . F3 . 89.43(16) yes F1 . P1 . F4 . 90.7(2) yes F2 . P1 . F4 . 89.49(18) yes F3 . P1 . F4 . 178.81(19) yes F1 . P1 . F5 . 91.1(2) yes F2 . P1 . F5 . 89.83(19) yes F3 . P1 . F5 . 89.80(17) yes F4 . P1 . F5 . 90.70(18) yes F1 . P1 . F6 . 90.3(2) yes F2 . P1 . F6 . 88.84(19) yes F3 . P1 . F6 . 89.54(17) yes F4 . P1 . F6 . 89.93(18) yes F5 . P1 . F6 . 178.5(2) yes F11 . P2 . F12 . 178.8(2) yes F11 . P2 . F13 . 89.83(19) yes F12 . P2 . F13 . 89.25(19) yes F11 . P2 . F14 . 91.0(2) yes F12 . P2 . F14 . 89.90(19) yes F13 . P2 . F14 . 179.1(2) yes F11 . P2 . F15 . 89.32(18) yes F12 . P2 . F15 . 89.97(18) yes F13 . P2 . F15 . 89.55(17) yes F14 . P2 . F15 . 90.24(18) yes F11 . P2 . F16 . 90.82(19) yes F12 . P2 . F16 . 89.87(18) yes F13 . P2 . F16 . 89.48(17) yes F14 . P2 . F16 . 90.73(19) yes F15 . P2 . F16 . 179.03(19) yes F21 . P3 . F22 . 179.75(18) yes F21 . P3 . F23 . 90.22(18) yes F22 . P3 . F23 . 89.58(18) yes F21 . P3 . F24 . 90.52(18) yes F22 . P3 . F24 . 89.68(17) yes F23 . P3 . F24 . 179.19(19) yes F21 . P3 . F25 . 90.24(17) yes F22 . P3 . F25 . 89.61(17) yes F23 . P3 . F25 . 89.87(17) yes F24 . P3 . F25 . 90.43(17) yes F21 . P3 . F26 . 90.20(18) yes F22 . P3 . F26 . 89.96(18) yes F23 . P3 . F26 . 89.81(18) yes F24 . P3 . F26 . 89.88(17) yes F25 . P3 . F26 . 179.5(2) yes F31 . P4 . F32 . 179.3(2) yes F31 . P4 . F33 . 91.2(2) yes F32 . P4 . F33 . 89.5(2) yes F31 . P4 . F34 . 89.4(2) yes F32 . P4 . F34 . 89.9(2) yes F33 . P4 . F34 . 178.2(3) yes F31 . P4 . F35 . 89.4(2) yes F32 . P4 . F35 . 90.8(2) yes F33 . P4 . F35 . 90.6(3) yes F34 . P4 . F35 . 87.7(3) yes F31 . P4 . F36 . 90.4(2) yes F32 . P4 . F36 . 89.3(2) yes F33 . P4 . F36 . 92.3(3) yes F34 . P4 . F36 . 89.5(3) yes F35 . P4 . F36 . 177.2(3) yes # Attachment '[Ru_1__tpy_][BPh4]2.cif' data_em94_173k _database_code_depnum_ccdc_archive 'CCDC 694386' _audit_creation_date 07-06-06 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '6021808 em94_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 16.8777(2) _cell_length_b 20.6620(2) _cell_length_c 20.1043(2) _cell_angle_alpha 90 _cell_angle_beta 90.4207(6) _cell_angle_gamma 90 _cell_volume 7010.72(13) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_space_group_name_Hall '-P 2yab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z x+1/2,-y+1/2,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C68 H46 B2 Br2 N12 O0.50 Ru2 S2 # Dc = 1.41 Fooo = 2922.40 Mu = 16.79 M = 1486.90 # Found Formula = C84.60 H66.90 B2 Br1 N7.30 Ru1 S1 # Dc = 1.35 FOOO = 2922.40 Mu = 8.75 M = 1420.47 _chemical_formula_sum 'C84.60 H66.90 B2 Br1 N7.30 Ru1 S1' _chemical_formula_moiety 'C34 H23 Br N6 Ru S, 2(C24 H20 B), 1.3(C2 H3 N)' _chemical_compound_source ? _chemical_formula_weight 1420.47 _cell_measurement_reflns_used 29780 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_max 0.47 _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2922.400 _exptl_absorpt_coefficient_mu 0.875 # Sheldrick geometric approximatio 0.69 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.97 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 60911 _reflns_number_total 16769 _diffrn_reflns_av_R_equivalents 0.043 # Number of reflections with Friedels Law is 16769 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 16794 _diffrn_reflns_theta_min 1.013 _diffrn_reflns_theta_max 27.927 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.927 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -22 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.71 _refine_diff_density_max 0.98 _refine_ls_number_reflns 10792 _refine_ls_number_restraints 1424 _refine_ls_number_parameters 946 #_refine_ls_R_factor_ref 0.0353 _refine_ls_wR_factor_ref 0.0407 _refine_ls_goodness_of_fit_ref 1.0119 #_reflns_number_all 16602 _refine_ls_R_factor_all 0.0589 _refine_ls_wR_factor_all 0.0491 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 10792 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_gt 0.0407 _refine_ls_shift/su_max 0.002911 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.23 0.757 0.927 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ru1 Ru 0.785220(9) 0.510113(7) 0.717677(8) 0.0261 1.0000 Uani . . . . . . N1 N 0.87494(10) 0.48787(8) 0.65156(8) 0.0300 1.0000 Uani . . . . . . N2 N 0.77712(11) 0.41443(8) 0.71366(9) 0.0334 1.0000 Uani . . . . . . N3 N 0.69277(10) 0.49351(9) 0.78265(8) 0.0350 1.0000 Uani . . . . . . N4 N 0.87504(10) 0.52426(8) 0.78799(8) 0.0301 1.0000 Uani . . . . . . N5 N 0.78750(9) 0.60557(8) 0.72440(8) 0.0269 1.0000 Uani . . . . . . N6 N 0.69923(9) 0.53515(8) 0.64837(8) 0.0283 1.0000 Uani . . . . . . C1 C 0.92723(13) 0.52912(11) 0.62456(11) 0.0356 1.0000 Uani . . . . . . C2 C 0.99170(14) 0.50808(13) 0.58809(12) 0.0448 1.0000 Uani . . . . . . C3 C 1.00286(15) 0.44245(13) 0.57835(12) 0.0472 1.0000 Uani . . . . . . C4 C 0.94940(15) 0.40001(12) 0.60498(12) 0.0439 1.0000 Uani . . . . . . C5 C 0.88576(13) 0.42308(10) 0.64162(10) 0.0345 1.0000 Uani . . . . . . C6 C 0.82726(14) 0.38120(10) 0.67428(11) 0.0379 1.0000 Uani . . . . . . C7 C 0.82082(17) 0.31446(11) 0.66897(14) 0.0512 1.0000 Uani . . . . . . C8 C 0.7622(2) 0.28337(12) 0.70513(15) 0.0593 1.0000 Uani . . . . . . C9 C 0.71159(18) 0.31759(12) 0.74542(14) 0.0549 1.0000 Uani . . . . . . C10 C 0.72010(14) 0.38464(11) 0.74923(11) 0.0407 1.0000 Uani . . . . . . C11 C 0.67223(13) 0.42974(12) 0.78809(11) 0.0408 1.0000 Uani . . . . . . C12 C 0.60962(16) 0.41044(16) 0.82810(16) 0.0595 1.0000 Uani . . . . . . C13 C 0.56784(17) 0.4568(2) 0.86271(18) 0.0720 1.0000 Uani . . . . . . C14 C 0.58696(16) 0.52084(18) 0.85645(15) 0.0620 1.0000 Uani . . . . . . C15 C 0.64989(14) 0.53806(14) 0.81547(12) 0.0447 1.0000 Uani . . . . . . C16 C 0.92400(13) 0.47926(10) 0.81366(11) 0.0367 1.0000 Uani . . . . . . C17 C 0.98861(14) 0.49526(12) 0.85340(12) 0.0440 1.0000 Uani . . . . . . C18 C 1.00338(14) 0.55947(13) 0.86768(12) 0.0448 1.0000 Uani . . . . . . C19 C 0.95325(13) 0.60658(11) 0.84237(11) 0.0373 1.0000 Uani . . . . . . C20 C 0.88979(11) 0.58775(10) 0.80226(10) 0.0298 1.0000 Uani . . . . . . C21 C 0.83549(11) 0.63413(9) 0.76984(10) 0.0284 1.0000 Uani . . . . . . C22 C 0.82993(12) 0.69981(10) 0.78254(10) 0.0326 1.0000 Uani . . . . . . C23 C 0.77478(12) 0.73701(9) 0.74704(11) 0.0328 1.0000 Uani . . . . . . C24 C 0.72737(12) 0.70666(10) 0.69893(11) 0.0325 1.0000 Uani . . . . . . C25 C 0.73407(11) 0.64057(9) 0.68895(10) 0.0283 1.0000 Uani . . . . . . C26 C 0.68426(11) 0.60018(9) 0.64512(10) 0.0293 1.0000 Uani . . . . . . C27 C 0.62488(12) 0.62469(10) 0.60438(11) 0.0358 1.0000 Uani . . . . . . C28 C 0.57933(13) 0.58257(12) 0.56646(12) 0.0413 1.0000 Uani . . . . . . C29 C 0.59384(14) 0.51696(11) 0.57049(12) 0.0417 1.0000 Uani . . . . . . C30 C 0.65452(13) 0.49508(10) 0.61153(11) 0.0357 1.0000 Uani . . . . . . B1 B 0.39907(12) 0.73678(10) 0.50432(10) 0.0253 1.0000 Uani . . . . . . B2 B 0.90744(14) 0.73615(11) 1.03285(12) 0.0317 1.0000 Uani . . . . . . C31 C 0.44104(11) 0.75373(9) 0.57632(9) 0.0272 1.0000 Uani . . . . . . C32 C 0.49037(12) 0.80751(10) 0.58391(11) 0.0347 1.0000 Uani . . . . . . C33 C 0.53078(13) 0.82166(11) 0.64276(12) 0.0416 1.0000 Uani . . . . . . C34 C 0.52185(14) 0.78226(13) 0.69749(11) 0.0435 1.0000 Uani . . . . . . C35 C 0.47266(15) 0.72905(13) 0.69248(12) 0.0468 1.0000 Uani . . . . . . C36 C 0.43284(13) 0.71550(11) 0.63326(11) 0.0373 1.0000 Uani . . . . . . C37 C 0.46517(11) 0.70468(8) 0.45404(9) 0.0259 1.0000 Uani . . . . . . C38 C 0.54718(11) 0.71045(9) 0.46210(10) 0.0298 1.0000 Uani . . . . . . C39 C 0.60141(12) 0.68093(10) 0.41964(12) 0.0363 1.0000 Uani . . . . . . C40 C 0.57520(14) 0.64560(11) 0.36600(12) 0.0419 1.0000 Uani . . . . . . C41 C 0.49409(14) 0.63934(12) 0.35499(12) 0.0421 1.0000 Uani . . . . . . C42 C 0.44107(12) 0.66820(10) 0.39833(11) 0.0341 1.0000 Uani . . . . . . C43 C 0.32776(11) 0.68359(9) 0.51474(9) 0.0275 1.0000 Uani . . . . . . C44 C 0.34578(12) 0.61871(10) 0.52813(12) 0.0355 1.0000 Uani . . . . . . C45 C 0.28889(13) 0.57139(10) 0.53695(13) 0.0399 1.0000 Uani . . . . . . C46 C 0.21009(13) 0.58697(11) 0.53178(12) 0.0410 1.0000 Uani . . . . . . C47 C 0.18914(12) 0.64994(11) 0.51863(12) 0.0406 1.0000 Uani . . . . . . C48 C 0.24714(12) 0.69746(10) 0.51095(11) 0.0344 1.0000 Uani . . . . . . C49 C 0.36180(10) 0.80287(8) 0.47134(10) 0.0260 1.0000 Uani . . . . . . C50 C 0.35698(12) 0.81347(9) 0.40254(10) 0.0304 1.0000 Uani . . . . . . C51 C 0.31932(13) 0.86744(10) 0.37513(11) 0.0341 1.0000 Uani . . . . . . C52 C 0.28595(13) 0.91385(10) 0.41582(11) 0.0351 1.0000 Uani . . . . . . C53 C 0.28984(12) 0.90525(10) 0.48415(11) 0.0338 1.0000 Uani . . . . . . C54 C 0.32651(12) 0.85080(9) 0.51091(10) 0.0307 1.0000 Uani . . . . . . C55 C 0.86169(12) 0.67257(10) 1.00287(10) 0.0326 1.0000 Uani . . . . . . C56 C 0.89125(14) 0.60939(11) 1.01065(11) 0.0395 1.0000 Uani . . . . . . C57 C 0.85410(16) 0.55577(11) 0.98250(12) 0.0455 1.0000 Uani . . . . . . C58 C 0.78659(15) 0.56342(11) 0.94395(12) 0.0442 1.0000 Uani . . . . . . C59 C 0.75680(15) 0.62496(12) 0.93425(12) 0.0433 1.0000 Uani . . . . . . C60 C 0.79399(13) 0.67797(11) 0.96321(11) 0.0370 1.0000 Uani . . . . . . C61 C 0.84178(12) 0.79473(10) 1.04212(10) 0.0329 1.0000 Uani . . . . . . C62 C 0.77523(13) 0.78225(11) 1.08123(11) 0.0372 1.0000 Uani . . . . . . C63 C 0.71556(14) 0.82700(12) 1.09232(12) 0.0414 1.0000 Uani . . . . . . C64 C 0.71989(15) 0.88738(12) 1.06357(13) 0.0470 1.0000 Uani . . . . . . C65 C 0.78539(16) 0.90235(11) 1.02518(13) 0.0479 1.0000 Uani . . . . . . C66 C 0.84559(15) 0.85696(11) 1.01588(12) 0.0406 1.0000 Uani . . . . . . C67 C 0.94348(13) 0.72407(10) 1.10813(11) 0.0359 1.0000 Uani . . . . . . C68 C 1.00167(15) 0.76589(13) 1.13396(12) 0.0458 1.0000 Uani . . . . . . C69 C 1.02803(17) 0.76305(17) 1.19975(14) 0.0584 1.0000 Uani . . . . . . C70 C 0.99777(18) 0.71735(17) 1.24209(13) 0.0611 1.0000 Uani . . . . . . C71 C 0.94156(19) 0.67468(16) 1.21874(13) 0.0594 1.0000 Uani . . . . . . C72 C 0.91479(15) 0.67830(12) 1.15278(12) 0.0444 1.0000 Uani . . . . . . C73 C 0.97834(12) 0.74873(10) 0.97909(10) 0.0328 1.0000 Uani . . . . . . C74 C 1.05116(13) 0.71702(11) 0.98600(12) 0.0389 1.0000 Uani . . . . . . C75 C 1.11009(14) 0.71982(13) 0.93819(13) 0.0455 1.0000 Uani . . . . . . C76 C 1.09917(15) 0.75571(13) 0.88097(12) 0.0475 1.0000 Uani . . . . . . C77 C 1.02795(16) 0.78813(12) 0.87227(11) 0.0467 1.0000 Uani . . . . . . C78 C 0.96879(14) 0.78372(11) 0.91963(11) 0.0392 1.0000 Uani . . . . . . Br1 Br 0.67786(3) 0.997808(18) 0.74525(3) 0.0724 0.7000 Uani D U . . . . Br2 Br 0.71972(7) 0.98464(5) 0.85851(7) 0.0746 0.3000 Uani D U . . . . C79 C 0.7647(4) 0.8044(2) 0.7679(2) 0.0288 0.7000 Uani D U . . . . C81 C 0.7469(3) 0.89888(17) 0.8298(2) 0.0466 0.7000 Uani D U . . . . C82 C 0.7203(3) 0.91710(16) 0.7697(2) 0.0412 0.7000 Uani D U . . . . C85 C 0.7585(10) 0.8097(5) 0.7484(4) 0.0326 0.3000 Uani D U . . . . C87 C 0.7187(7) 0.9180(4) 0.7360(5) 0.0519 0.3000 Uani D U . . . . C88 C 0.7346(7) 0.9138(4) 0.8019(5) 0.0497 0.3000 Uani D U . . . . S1 S 0.72638(5) 0.85735(3) 0.70896(4) 0.0406 0.7000 Uani D U . . . . S2 S 0.77019(9) 0.83910(7) 0.82801(7) 0.0491 0.3000 Uani D U . . . . C86 C 0.72638(5) 0.85735(3) 0.70896(4) 0.0406 0.3000 Uani D U . . . . C80 C 0.77019(9) 0.83910(7) 0.82801(7) 0.0491 0.7000 Uani D U . . . . N90 N 0.6767(5) 0.6139(4) 0.0903(4) 0.1783 0.8000 Uani . U . . . . C91 C 0.6269(9) 0.5694(8) 0.0617(9) 0.1814 0.5000 Uani . U . . . . C92 C 0.5774(9) 0.5369(8) 0.0249(8) 0.1863 0.5000 Uani . U . . . . C93 C 0.6084(6) 0.5513(5) 0.2280(6) 0.1025 0.5000 Uani . U . . . . C94 C 0.5910(5) 0.5045(4) 0.2543(5) 0.0880 0.5000 Uani . U . . . . N94 N 0.5684(5) 0.4518(5) 0.2810(6) 0.1341 0.5000 Uani . U . . . . C95 C 0.6835(13) 0.6150(10) 0.1598(13) 0.1486 0.3000 Uani . U . . . . C96 C 0.6903(12) 0.6287(9) 0.2143(11) 0.1403 0.3000 Uani . U . . . . H11 H 0.9197 0.5748 0.6308 0.0427 1.0000 Uiso R . . . . . H21 H 1.0282 0.5388 0.5698 0.0537 1.0000 Uiso R . . . . . H31 H 1.0473 0.4269 0.5534 0.0567 1.0000 Uiso R . . . . . H41 H 0.9559 0.3543 0.5983 0.0527 1.0000 Uiso R . . . . . H71 H 0.8560 0.2903 0.6410 0.0612 1.0000 Uiso R . . . . . H81 H 0.7568 0.2372 0.7019 0.0709 1.0000 Uiso R . . . . . H91 H 0.6713 0.2958 0.7704 0.0658 1.0000 Uiso R . . . . . H121 H 0.5957 0.3655 0.8316 0.0714 1.0000 Uiso R . . . . . H131 H 0.5252 0.4441 0.8912 0.0864 1.0000 Uiso R . . . . . H141 H 0.5576 0.5533 0.8798 0.0746 1.0000 Uiso R . . . . . H151 H 0.6630 0.5830 0.8105 0.0537 1.0000 Uiso R . . . . . H161 H 0.9139 0.4345 0.8042 0.0440 1.0000 Uiso R . . . . . H171 H 1.0227 0.4620 0.8708 0.0528 1.0000 Uiso R . . . . . H181 H 1.0480 0.5714 0.8949 0.0537 1.0000 Uiso R . . . . . H191 H 0.9621 0.6515 0.8523 0.0446 1.0000 Uiso R . . . . . H221 H 0.8636 0.7196 0.8154 0.0391 1.0000 Uiso R . . . . . H241 H 0.6904 0.7315 0.6730 0.0389 1.0000 Uiso R . . . . . H271 H 0.6154 0.6705 0.6024 0.0430 1.0000 Uiso R . . . . . H281 H 0.5382 0.5988 0.5378 0.0495 1.0000 Uiso R . . . . . H291 H 0.5624 0.4869 0.5452 0.0499 1.0000 Uiso R . . . . . H301 H 0.6649 0.4494 0.6136 0.0427 1.0000 Uiso R . . . . . H321 H 0.4967 0.8361 0.5467 0.0417 1.0000 Uiso R . . . . . H331 H 0.5648 0.8588 0.6452 0.0498 1.0000 Uiso R . . . . . H341 H 0.5493 0.7916 0.7383 0.0521 1.0000 Uiso R . . . . . H351 H 0.4659 0.7011 0.7302 0.0562 1.0000 Uiso R . . . . . H361 H 0.3984 0.6785 0.6314 0.0448 1.0000 Uiso R . . . . . H381 H 0.5672 0.7359 0.4985 0.0357 1.0000 Uiso R . . . . . H391 H 0.6572 0.6854 0.4280 0.0435 1.0000 Uiso R . . . . . H401 H 0.6123 0.6255 0.3365 0.0504 1.0000 Uiso R . . . . . H411 H 0.4748 0.6151 0.3175 0.0505 1.0000 Uiso R . . . . . H421 H 0.3854 0.6630 0.3899 0.0409 1.0000 Uiso R . . . . . H441 H 0.4005 0.6064 0.5314 0.0426 1.0000 Uiso R . . . . . H451 H 0.3045 0.5277 0.5467 0.0479 1.0000 Uiso R . . . . . H461 H 0.1702 0.5543 0.5373 0.0492 1.0000 Uiso R . . . . . H471 H 0.1342 0.6614 0.5147 0.0487 1.0000 Uiso R . . . . . H481 H 0.2308 0.7413 0.5028 0.0412 1.0000 Uiso R . . . . . H501 H 0.3805 0.7824 0.3732 0.0365 1.0000 Uiso R . . . . . H511 H 0.3165 0.8724 0.3277 0.0409 1.0000 Uiso R . . . . . H521 H 0.2606 0.9513 0.3971 0.0421 1.0000 Uiso R . . . . . H531 H 0.2671 0.9370 0.5131 0.0406 1.0000 Uiso R . . . . . H541 H 0.3278 0.8457 0.5584 0.0369 1.0000 Uiso R . . . . . H561 H 0.9388 0.6030 1.0363 0.0474 1.0000 Uiso R . . . . . H571 H 0.8754 0.5133 0.9899 0.0546 1.0000 Uiso R . . . . . H581 H 0.7609 0.5266 0.9243 0.0531 1.0000 Uiso R . . . . . H591 H 0.7102 0.6311 0.9073 0.0519 1.0000 Uiso R . . . . . H601 H 0.7721 0.7202 0.9556 0.0444 1.0000 Uiso R . . . . . H621 H 0.7707 0.7404 1.1015 0.0445 1.0000 Uiso R . . . . . H631 H 0.6714 0.8159 1.1199 0.0496 1.0000 Uiso R . . . . . H641 H 0.6784 0.9185 1.0700 0.0564 1.0000 Uiso R . . . . . H651 H 0.7894 0.9443 1.0049 0.0575 1.0000 Uiso R . . . . . H661 H 0.8912 0.8691 0.9905 0.0487 1.0000 Uiso R . . . . . H681 H 1.0242 0.7978 1.1050 0.0550 1.0000 Uiso R . . . . . H691 H 1.0674 0.7931 1.2154 0.0700 1.0000 Uiso R . . . . . H701 H 1.0156 0.7152 1.2875 0.0734 1.0000 Uiso R . . . . . H711 H 0.9206 0.6422 1.2479 0.0712 1.0000 Uiso R . . . . . H721 H 0.8752 0.6482 1.1378 0.0533 1.0000 Uiso R . . . . . H741 H 1.0609 0.6922 1.0256 0.0467 1.0000 Uiso R . . . . . H751 H 1.1588 0.6966 0.9450 0.0546 1.0000 Uiso R . . . . . H761 H 1.1399 0.7582 0.8480 0.0570 1.0000 Uiso R . . . . . H771 H 1.0195 0.8139 0.8331 0.0561 1.0000 Uiso R . . . . . H781 H 0.9194 0.8054 0.9114 0.0470 1.0000 Uiso R . . . . . H801 H 0.7910 0.8187 0.8673 0.0589 0.7000 Uiso . . . . . . H811 H 0.7486 0.9261 0.8685 0.0560 0.7000 Uiso R . . . . . H861 H 0.7099 0.8486 0.6641 0.0486 0.3000 Uiso . . . . . . H871 H 0.7120 0.9568 0.7104 0.0622 0.3000 Uiso R . . . . . H921 H 0.5690 0.4949 0.0440 0.2250 0.5000 Uiso R . . . . . H922 H 0.5986 0.5322 -0.0190 0.2250 0.5000 Uiso R . . . . . H923 H 0.5279 0.5597 0.0225 0.2250 0.5000 Uiso R . . . . . H931 H 0.6526 0.5707 0.2507 0.1228 0.5000 Uiso R . . . . . H932 H 0.5643 0.5806 0.2281 0.1228 0.5000 Uiso R . . . . . H933 H 0.6228 0.5419 0.1829 0.1228 0.5000 Uiso R . . . . . H961 H 0.7108 0.6720 0.2172 0.1690 0.3000 Uiso R . . . . . H962 H 0.7261 0.5994 0.2361 0.1690 0.3000 Uiso R . . . . . H963 H 0.6395 0.6269 0.2354 0.1690 0.3000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02762(7) 0.02291(7) 0.02776(7) 0.00111(6) -0.00251(5) -0.00072(6) N1 0.0317(8) 0.0298(8) 0.0284(7) 0.0004(6) -0.0031(6) 0.0049(7) N2 0.0412(9) 0.0253(8) 0.0335(8) 0.0045(7) -0.0114(7) -0.0024(7) N3 0.0313(8) 0.0433(10) 0.0302(8) 0.0051(7) -0.0062(7) -0.0067(7) N4 0.0310(8) 0.0305(8) 0.0287(8) 0.0011(6) -0.0012(6) 0.0008(6) N5 0.0253(7) 0.0260(7) 0.0294(8) 0.0002(6) 0.0003(6) 0.0005(6) N6 0.0283(8) 0.0269(7) 0.0296(8) 0.0004(6) -0.0025(6) 0.0003(6) C1 0.0363(10) 0.0357(10) 0.0348(10) 0.0028(8) 0.0003(8) 0.0063(8) C2 0.0390(11) 0.0531(13) 0.0423(11) 0.0041(10) 0.0056(9) 0.0098(10) C3 0.0450(13) 0.0590(15) 0.0376(11) -0.0047(10) -0.0022(10) 0.0215(11) C4 0.0520(13) 0.0413(12) 0.0384(11) -0.0102(9) -0.0125(10) 0.0198(10) C5 0.0423(11) 0.0301(10) 0.0309(10) -0.0027(8) -0.0121(8) 0.0077(8) C6 0.0492(12) 0.0272(10) 0.0371(11) -0.0028(8) -0.0166(9) 0.0039(8) C7 0.0696(16) 0.0299(11) 0.0537(14) -0.0079(10) -0.0241(12) 0.0008(11) C8 0.0827(19) 0.0264(11) 0.0683(17) 0.0031(11) -0.0375(15) -0.0109(12) C9 0.0677(16) 0.0385(12) 0.0583(16) 0.0150(11) -0.0284(13) -0.0213(12) C10 0.0452(12) 0.0372(11) 0.0396(11) 0.0124(9) -0.0177(9) -0.0127(9) C11 0.0372(11) 0.0465(12) 0.0385(11) 0.0131(9) -0.0117(9) -0.0100(9) C12 0.0432(13) 0.0705(18) 0.0646(17) 0.0299(14) -0.0049(12) -0.0169(13) C13 0.0378(13) 0.104(3) 0.074(2) 0.0345(18) 0.0150(13) -0.0046(15) C14 0.0379(13) 0.091(2) 0.0574(16) 0.0101(15) 0.0129(11) 0.0051(13) C15 0.0361(11) 0.0597(14) 0.0384(12) 0.0022(10) 0.0025(9) 0.0011(10) C16 0.0399(11) 0.0334(11) 0.0369(10) 0.0038(8) -0.0062(8) 0.0037(8) C17 0.0415(11) 0.0455(13) 0.0449(12) 0.0052(10) -0.0120(9) 0.0099(9) C18 0.0384(11) 0.0497(13) 0.0461(12) 0.0010(10) -0.0139(10) 0.0001(10) C19 0.0365(10) 0.0370(11) 0.0382(11) -0.0014(8) -0.0065(9) -0.0013(8) C20 0.0282(9) 0.0315(9) 0.0298(9) 0.0016(7) 0.0000(7) -0.0011(7) C21 0.0254(9) 0.0285(9) 0.0312(9) -0.0005(7) 0.0020(7) -0.0024(7) C22 0.0299(9) 0.0310(10) 0.0369(10) -0.0023(8) 0.0001(8) -0.0036(7) C23 0.0281(9) 0.0250(9) 0.0454(11) -0.0017(8) 0.0038(8) -0.0009(7) C24 0.0280(9) 0.0270(9) 0.0424(11) 0.0011(8) 0.0001(8) 0.0022(7) C25 0.0247(8) 0.0267(9) 0.0334(9) 0.0002(7) 0.0013(7) 0.0014(7) C26 0.0273(9) 0.0293(9) 0.0314(9) -0.0005(7) -0.0001(7) 0.0001(7) C27 0.0310(10) 0.0307(10) 0.0458(12) 0.0028(8) -0.0059(9) 0.0023(8) C28 0.0323(10) 0.0437(12) 0.0478(12) 0.0026(10) -0.0109(9) 0.0011(9) C29 0.0392(11) 0.0389(11) 0.0467(12) -0.0033(9) -0.0137(9) -0.0043(9) C30 0.0390(10) 0.0303(10) 0.0376(10) -0.0010(8) -0.0078(8) -0.0032(8) B1 0.0242(9) 0.0211(9) 0.0307(10) 0.0016(7) -0.0011(8) -0.0007(7) B2 0.0346(11) 0.0288(10) 0.0317(11) -0.0004(8) -0.0043(9) 0.0054(8) C31 0.0213(8) 0.0291(9) 0.0310(9) -0.0025(7) -0.0002(7) 0.0039(7) C32 0.0316(10) 0.0345(10) 0.0380(10) -0.0007(8) -0.0035(8) -0.0014(8) C33 0.0367(11) 0.0407(11) 0.0472(12) -0.0108(9) -0.0101(9) -0.0013(9) C34 0.0383(11) 0.0586(14) 0.0333(11) -0.0112(10) -0.0101(9) 0.0111(10) C35 0.0490(13) 0.0582(15) 0.0333(11) 0.0051(10) -0.0021(9) 0.0053(11) C36 0.0354(10) 0.0416(11) 0.0350(11) 0.0052(9) -0.0008(8) -0.0027(8) C37 0.0269(8) 0.0184(8) 0.0324(9) 0.0037(7) -0.0017(7) 0.0002(6) C38 0.0284(9) 0.0249(9) 0.0360(10) 0.0022(7) -0.0026(7) 0.0031(7) C39 0.0275(9) 0.0328(10) 0.0484(12) 0.0036(9) 0.0029(8) 0.0042(8) C40 0.0423(12) 0.0387(11) 0.0450(12) -0.0021(9) 0.0105(9) 0.0068(9) C41 0.0464(12) 0.0409(12) 0.0391(11) -0.0094(9) 0.0027(9) 0.0002(9) C42 0.0311(10) 0.0334(10) 0.0378(10) -0.0040(8) -0.0024(8) -0.0023(8) C43 0.0274(9) 0.0245(8) 0.0308(9) 0.0002(7) 0.0004(7) -0.0011(7) C44 0.0260(9) 0.0264(9) 0.0540(13) 0.0013(8) 0.0029(8) 0.0004(7) C45 0.0366(11) 0.0239(9) 0.0592(14) 0.0024(9) 0.0074(10) -0.0032(8) C46 0.0331(10) 0.0363(11) 0.0537(13) -0.0012(9) 0.0060(9) -0.0126(8) C47 0.0244(9) 0.0418(11) 0.0556(13) 0.0010(10) -0.0012(9) -0.0034(8) C48 0.0270(9) 0.0308(9) 0.0453(12) 0.0030(8) -0.0029(8) 0.0000(7) C49 0.0226(8) 0.0216(8) 0.0336(9) 0.0011(7) -0.0025(7) -0.0023(6) C50 0.0323(9) 0.0247(9) 0.0343(10) -0.0013(7) -0.0013(8) 0.0012(7) C51 0.0391(11) 0.0288(9) 0.0344(10) 0.0039(8) -0.0031(8) 0.0011(8) C52 0.0365(10) 0.0256(9) 0.0432(11) 0.0054(8) -0.0023(8) 0.0034(8) C53 0.0346(10) 0.0252(9) 0.0417(11) -0.0008(8) 0.0028(8) 0.0058(7) C54 0.0306(9) 0.0270(9) 0.0346(10) 0.0003(7) 0.0009(8) -0.0011(7) C55 0.0359(10) 0.0308(10) 0.0311(9) 0.0002(7) 0.0016(8) 0.0027(8) C56 0.0440(12) 0.0334(10) 0.0410(11) 0.0003(8) -0.0022(9) 0.0073(9) C57 0.0617(15) 0.0294(10) 0.0454(12) 0.0035(9) 0.0026(11) 0.0035(10) C58 0.0543(14) 0.0351(11) 0.0433(12) -0.0030(9) 0.0029(10) -0.0101(10) C59 0.0414(12) 0.0409(12) 0.0475(13) -0.0020(10) -0.0053(10) -0.0053(9) C60 0.0410(11) 0.0308(10) 0.0392(11) 0.0000(8) -0.0046(9) 0.0004(8) C61 0.0345(10) 0.0301(9) 0.0341(10) -0.0044(8) -0.0072(8) 0.0026(8) C62 0.0377(11) 0.0337(10) 0.0399(11) -0.0013(8) -0.0049(9) 0.0011(8) C63 0.0358(11) 0.0442(12) 0.0441(12) -0.0086(10) -0.0033(9) 0.0036(9) C64 0.0448(13) 0.0422(12) 0.0539(14) -0.0105(10) -0.0065(11) 0.0149(10) C65 0.0614(15) 0.0290(10) 0.0534(14) -0.0009(9) -0.0024(11) 0.0109(10) C66 0.0473(12) 0.0322(10) 0.0423(12) -0.0031(9) 0.0006(9) 0.0018(9) C67 0.0360(10) 0.0378(11) 0.0337(10) -0.0038(8) -0.0034(8) 0.0112(8) C68 0.0455(13) 0.0532(14) 0.0386(12) -0.0060(10) -0.0072(10) 0.0056(10) C69 0.0542(15) 0.0781(19) 0.0428(13) -0.0129(13) -0.0156(11) 0.0093(13) C70 0.0616(16) 0.087(2) 0.0345(12) -0.0031(13) -0.0073(11) 0.0253(15) C71 0.0713(18) 0.0697(18) 0.0372(12) 0.0114(12) 0.0051(12) 0.0230(15) C72 0.0500(13) 0.0470(13) 0.0362(11) 0.0008(9) 0.0005(9) 0.0100(10) C73 0.0350(10) 0.0311(9) 0.0323(9) -0.0047(8) -0.0063(8) -0.0009(8) C74 0.0369(11) 0.0415(12) 0.0383(11) 0.0018(9) -0.0007(9) -0.0003(9) C75 0.0367(11) 0.0539(14) 0.0460(13) -0.0033(10) 0.0003(10) 0.0018(10) C76 0.0464(13) 0.0552(14) 0.0409(12) -0.0058(10) 0.0066(10) -0.0074(11) C77 0.0636(15) 0.0459(13) 0.0306(11) -0.0001(9) -0.0050(10) -0.0071(11) C78 0.0435(12) 0.0401(11) 0.0339(10) -0.0024(8) -0.0094(9) 0.0027(9) Br1 0.0926(3) 0.03342(19) 0.0915(3) 0.01665(19) 0.0135(3) 0.02522(19) Br2 0.0754(7) 0.0500(5) 0.0983(8) -0.0310(6) -0.0018(6) 0.0050(5) C79 0.0266(17) 0.0240(15) 0.036(2) 0.0053(15) -0.006(2) 0.0029(11) C81 0.065(2) 0.0306(17) 0.044(2) -0.0048(15) -0.0012(18) 0.0074(15) C82 0.053(2) 0.0220(14) 0.049(2) 0.0117(17) 0.005(3) 0.0123(13) C85 0.035(4) 0.032(4) 0.031(4) -0.008(3) -0.014(4) -0.002(3) C87 0.056(4) 0.031(3) 0.068(5) 0.017(4) -0.019(5) -0.001(3) C88 0.063(4) 0.037(4) 0.049(5) -0.009(4) -0.019(5) 0.011(4) S1 0.0480(4) 0.0288(3) 0.0448(4) 0.0062(3) -0.0088(3) 0.0038(3) S2 0.0552(8) 0.0483(7) 0.0438(7) -0.0034(5) -0.0046(6) -0.0004(6) C86 0.0480(4) 0.0288(3) 0.0448(4) 0.0062(3) -0.0088(3) 0.0038(3) C80 0.0552(8) 0.0483(7) 0.0438(7) -0.0034(5) -0.0046(6) -0.0004(6) N90 0.158(4) 0.180(5) 0.199(4) -0.070(4) 0.112(4) -0.059(4) C91 0.136(4) 0.177(6) 0.233(6) -0.102(5) 0.143(4) -0.057(4) C92 0.144(5) 0.207(7) 0.209(6) -0.106(5) 0.136(4) -0.058(5) C93 0.102(4) 0.088(4) 0.118(5) -0.001(4) 0.011(4) 0.010(4) C94 0.068(3) 0.084(4) 0.111(5) 0.006(3) 0.007(4) 0.014(3) N94 0.086(4) 0.114(5) 0.202(6) 0.084(5) 0.007(4) 0.032(4) C95 0.139(5) 0.121(6) 0.188(5) -0.061(6) 0.116(5) -0.007(6) C96 0.137(6) 0.105(7) 0.180(6) -0.041(6) 0.085(6) 0.019(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2286(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . N1 . 2.0739(17) yes Ru1 . N2 . 1.9833(17) yes Ru1 . N3 . 2.0709(18) yes Ru1 . N4 . 2.0857(16) yes Ru1 . N5 . 1.9772(16) yes Ru1 . N6 . 2.0703(16) yes N1 . C1 . 1.344(3) yes N1 . C5 . 1.366(3) yes N2 . C6 . 1.351(3) yes N2 . C10 . 1.351(3) yes N3 . C11 . 1.367(3) yes N3 . C15 . 1.347(3) yes N4 . C16 . 1.344(3) yes N4 . C20 . 1.365(3) yes N5 . C21 . 1.352(2) yes N5 . C25 . 1.355(2) yes N6 . C26 . 1.369(3) yes N6 . C30 . 1.340(3) yes C1 . C2 . 1.386(3) yes C1 . H11 . 0.960 no C2 . C3 . 1.383(4) yes C2 . H21 . 0.960 no C3 . C4 . 1.370(4) yes C3 . H31 . 0.960 no C4 . C5 . 1.391(3) yes C4 . H41 . 0.960 no C5 . C6 . 1.471(3) yes C6 . C7 . 1.387(3) yes C7 . C8 . 1.390(4) yes C7 . H71 . 0.960 no C8 . C9 . 1.376(5) yes C8 . H81 . 0.960 no C9 . C10 . 1.395(3) yes C9 . H91 . 0.960 no C10 . C11 . 1.463(4) yes C11 . C12 . 1.391(4) yes C12 . C13 . 1.381(5) yes C12 . H121 . 0.960 no C13 . C14 . 1.368(5) yes C13 . H131 . 0.960 no C14 . C15 . 1.395(4) yes C14 . H141 . 0.960 no C15 . H151 . 0.960 no C16 . C17 . 1.387(3) yes C16 . H161 . 0.960 no C17 . C18 . 1.380(4) yes C17 . H171 . 0.960 no C18 . C19 . 1.384(3) yes C18 . H181 . 0.960 no C19 . C20 . 1.391(3) yes C19 . H191 . 0.960 no C20 . C21 . 1.475(3) yes C21 . C22 . 1.384(3) yes C22 . C23 . 1.399(3) yes C22 . H221 . 0.960 no C23 . C24 . 1.399(3) yes C23 . C79 . 1.465(5) yes C23 . C85 . 1.527(9) yes C24 . C25 . 1.385(3) yes C24 . H241 . 0.960 no C25 . C26 . 1.473(3) yes C26 . C27 . 1.386(3) yes C27 . C28 . 1.386(3) yes C27 . H271 . 0.960 no C28 . C29 . 1.380(3) yes C28 . H281 . 0.960 no C29 . C30 . 1.386(3) yes C29 . H291 . 0.960 no C30 . H301 . 0.960 no B1 . C31 . 1.645(3) yes B1 . C37 . 1.650(3) yes B1 . C43 . 1.644(3) yes B1 . C49 . 1.641(3) yes B2 . C55 . 1.637(3) yes B2 . C61 . 1.652(3) yes B2 . C67 . 1.646(3) yes B2 . C73 . 1.639(3) yes C31 . C32 . 1.396(3) yes C31 . C36 . 1.399(3) yes C32 . C33 . 1.392(3) yes C32 . H321 . 0.960 no C33 . C34 . 1.378(4) yes C33 . H331 . 0.960 no C34 . C35 . 1.381(4) yes C34 . H341 . 0.960 no C35 . C36 . 1.391(3) yes C35 . H351 . 0.960 no C36 . H361 . 0.960 no C37 . C38 . 1.398(3) yes C37 . C42 . 1.408(3) yes C38 . C39 . 1.396(3) yes C38 . H381 . 0.960 no C39 . C40 . 1.373(3) yes C39 . H391 . 0.960 no C40 . C41 . 1.391(3) yes C40 . H401 . 0.960 no C41 . C42 . 1.388(3) yes C41 . H411 . 0.960 no C42 . H421 . 0.960 no C43 . C44 . 1.400(3) yes C43 . C48 . 1.392(3) yes C44 . C45 . 1.383(3) yes C44 . H441 . 0.960 no C45 . C46 . 1.372(3) yes C45 . H451 . 0.960 no C46 . C47 . 1.373(3) yes C46 . H461 . 0.960 no C47 . C48 . 1.396(3) yes C47 . H471 . 0.960 no C48 . H481 . 0.960 no C49 . C50 . 1.402(3) yes C49 . C54 . 1.405(3) yes C50 . C51 . 1.395(3) yes C50 . H501 . 0.960 no C51 . C52 . 1.383(3) yes C51 . H511 . 0.960 no C52 . C53 . 1.386(3) yes C52 . H521 . 0.960 no C53 . C54 . 1.390(3) yes C53 . H531 . 0.960 no C54 . H541 . 0.960 no C55 . C56 . 1.406(3) yes C55 . C60 . 1.393(3) yes C56 . C57 . 1.391(3) yes C56 . H561 . 0.960 no C57 . C58 . 1.382(4) yes C57 . H571 . 0.960 no C58 . C59 . 1.381(4) yes C58 . H581 . 0.960 no C59 . C60 . 1.388(3) yes C59 . H591 . 0.960 no C60 . H601 . 0.960 no C61 . C62 . 1.400(3) yes C61 . C66 . 1.392(3) yes C62 . C63 . 1.386(3) yes C62 . H621 . 0.960 no C63 . C64 . 1.377(4) yes C63 . H631 . 0.960 no C64 . C65 . 1.388(4) yes C64 . H641 . 0.960 no C65 . C66 . 1.396(3) yes C65 . H651 . 0.960 no C66 . H661 . 0.960 no C67 . C68 . 1.405(3) yes C67 . C72 . 1.393(3) yes C68 . C69 . 1.394(4) yes C68 . H681 . 0.960 no C69 . C70 . 1.372(5) yes C69 . H691 . 0.960 no C70 . C71 . 1.375(5) yes C70 . H701 . 0.960 no C71 . C72 . 1.400(4) yes C71 . H711 . 0.960 no C72 . H721 . 0.960 no C73 . C74 . 1.399(3) yes C73 . C78 . 1.405(3) yes C74 . C75 . 1.389(3) yes C74 . H741 . 0.960 no C75 . C76 . 1.380(4) yes C75 . H751 . 0.960 no C76 . C77 . 1.386(4) yes C76 . H761 . 0.960 no C77 . C78 . 1.388(4) yes C77 . H771 . 0.960 no C78 . H781 . 0.960 no Br1 . C82 . 1.879(3) yes Br2 . C88 . 1.871(7) yes C79 . S1 . 1.734(4) yes C79 . C80 . 1.408(4) yes C81 . C82 . 1.341(5) yes C81 . C80 . 1.297(4) yes C81 . H811 . 0.960 no C82 . S1 . 1.740(4) yes C85 . S2 . 1.723(7) yes C85 . C86 . 1.373(8) yes C87 . C88 . 1.353(8) yes C87 . S1 . 1.372(7) yes C87 . C86 . 1.372(7) yes C87 . H871 . 0.960 no C88 . S2 . 1.736(7) yes S1 . H861 . 0.960 no S2 . H801 . 0.960 no C86 . H861 . 0.960 no C80 . H801 . 0.960 no N90 . C91 . 1.370(16) yes N90 . C95 . 1.40(3) yes C91 . C92 . 1.30(2) yes C92 . H921 . 0.960 no C92 . H922 . 0.960 no C92 . H923 . 0.960 no C93 . C94 . 1.143(12) yes C93 . H931 . 0.960 no C93 . H932 . 0.960 no C93 . H933 . 0.960 no C94 . N94 . 1.272(12) yes C95 . C96 . 1.14(3) yes C96 . H961 . 0.960 no C96 . H962 . 0.960 no C96 . H963 . 0.960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 78.66(7) yes N1 . Ru1 . N3 . 157.62(7) yes N2 . Ru1 . N3 . 78.96(8) yes N1 . Ru1 . N4 . 86.27(6) yes N2 . Ru1 . N4 . 102.53(7) yes N3 . Ru1 . N4 . 98.22(6) yes N1 . Ru1 . N5 . 104.53(7) yes N2 . Ru1 . N5 . 176.74(7) yes N3 . Ru1 . N5 . 97.85(7) yes N4 . Ru1 . N5 . 78.47(6) yes N1 . Ru1 . N6 . 97.79(6) yes N2 . Ru1 . N6 . 100.01(7) yes N3 . Ru1 . N6 . 86.46(6) yes N4 . Ru1 . N6 . 157.45(7) yes N5 . Ru1 . N6 . 79.04(6) yes Ru1 . N1 . C1 . 127.08(14) yes Ru1 . N1 . C5 . 114.20(14) yes C1 . N1 . C5 . 118.27(18) yes Ru1 . N2 . C6 . 119.16(15) yes Ru1 . N2 . C10 . 118.79(16) yes C6 . N2 . C10 . 122.02(19) yes Ru1 . N3 . C11 . 113.76(16) yes Ru1 . N3 . C15 . 127.29(16) yes C11 . N3 . C15 . 118.8(2) yes Ru1 . N4 . C16 . 127.22(14) yes Ru1 . N4 . C20 . 114.06(13) yes C16 . N4 . C20 . 118.24(18) yes Ru1 . N5 . C21 . 119.53(13) yes Ru1 . N5 . C25 . 118.95(13) yes C21 . N5 . C25 . 121.04(16) yes Ru1 . N6 . C26 . 113.93(12) yes Ru1 . N6 . C30 . 127.36(14) yes C26 . N6 . C30 . 118.52(17) yes N1 . C1 . C2 . 122.3(2) yes N1 . C1 . H11 . 118.8 no C2 . C1 . H11 . 118.8 no C1 . C2 . C3 . 119.4(2) yes C1 . C2 . H21 . 120.3 no C3 . C2 . H21 . 120.3 no C2 . C3 . C4 . 118.8(2) yes C2 . C3 . H31 . 120.6 no C4 . C3 . H31 . 120.6 no C3 . C4 . C5 . 120.1(2) yes C3 . C4 . H41 . 120.0 no C5 . C4 . H41 . 120.0 no C4 . C5 . N1 . 121.2(2) yes C4 . C5 . C6 . 123.9(2) yes N1 . C5 . C6 . 114.86(18) yes C5 . C6 . N2 . 112.83(18) yes C5 . C6 . C7 . 127.1(2) yes N2 . C6 . C7 . 120.1(2) yes C6 . C7 . C8 . 118.3(3) yes C6 . C7 . H71 . 120.8 no C8 . C7 . H71 . 120.8 no C7 . C8 . C9 . 121.2(2) yes C7 . C8 . H81 . 119.4 no C9 . C8 . H81 . 119.4 no C8 . C9 . C10 . 118.6(3) yes C8 . C9 . H91 . 120.7 no C10 . C9 . H91 . 120.7 no C9 . C10 . N2 . 119.8(3) yes C9 . C10 . C11 . 127.2(2) yes N2 . C10 . C11 . 112.99(19) yes C10 . C11 . N3 . 115.5(2) yes C10 . C11 . C12 . 123.4(2) yes N3 . C11 . C12 . 121.1(3) yes C11 . C12 . C13 . 119.0(3) yes C11 . C12 . H121 . 120.5 no C13 . C12 . H121 . 120.5 no C12 . C13 . C14 . 120.2(3) yes C12 . C13 . H131 . 119.9 no C14 . C13 . H131 . 119.9 no C13 . C14 . C15 . 118.8(3) yes C13 . C14 . H141 . 120.6 no C15 . C14 . H141 . 120.6 no C14 . C15 . N3 . 121.9(3) yes C14 . C15 . H151 . 119.0 no N3 . C15 . H151 . 119.0 no N4 . C16 . C17 . 122.3(2) yes N4 . C16 . H161 . 118.8 no C17 . C16 . H161 . 118.8 no C16 . C17 . C18 . 119.3(2) yes C16 . C17 . H171 . 120.4 no C18 . C17 . H171 . 120.4 no C17 . C18 . C19 . 119.4(2) yes C17 . C18 . H181 . 120.3 no C19 . C18 . H181 . 120.3 no C18 . C19 . C20 . 118.8(2) yes C18 . C19 . H191 . 120.6 no C20 . C19 . H191 . 120.6 no C19 . C20 . N4 . 121.94(18) yes C19 . C20 . C21 . 123.20(18) yes N4 . C20 . C21 . 114.82(17) yes C20 . C21 . N5 . 112.48(16) yes C20 . C21 . C22 . 126.77(18) yes N5 . C21 . C22 . 120.75(18) yes C21 . C22 . C23 . 119.37(18) yes C21 . C22 . H221 . 120.3 no C23 . C22 . H221 . 120.3 no C22 . C23 . C24 . 118.78(18) yes C22 . C23 . C79 . 117.1(2) yes C24 . C23 . C79 . 123.8(3) yes C22 . C23 . C85 . 130.6(5) yes C24 . C23 . C85 . 110.5(4) yes C23 . C24 . C25 . 119.68(18) yes C23 . C24 . H241 . 120.2 no C25 . C24 . H241 . 120.2 no C24 . C25 . N5 . 120.33(18) yes C24 . C25 . C26 . 126.77(18) yes N5 . C25 . C26 . 112.78(16) yes C25 . C26 . N6 . 115.06(16) yes C25 . C26 . C27 . 123.64(18) yes N6 . C26 . C27 . 121.28(18) yes C26 . C27 . C28 . 119.4(2) yes C26 . C27 . H271 . 120.3 no C28 . C27 . H271 . 120.3 no C27 . C28 . C29 . 119.2(2) yes C27 . C28 . H281 . 120.4 no C29 . C28 . H281 . 120.4 no C28 . C29 . C30 . 119.0(2) yes C28 . C29 . H291 . 120.5 no C30 . C29 . H291 . 120.5 no C29 . C30 . N6 . 122.6(2) yes C29 . C30 . H301 . 118.7 no N6 . C30 . H301 . 118.7 no C31 . B1 . C37 . 109.64(14) yes C31 . B1 . C43 . 109.95(15) yes C37 . B1 . C43 . 107.94(14) yes C31 . B1 . C49 . 109.86(15) yes C37 . B1 . C49 . 110.23(15) yes C43 . B1 . C49 . 109.19(14) yes C55 . B2 . C61 . 108.33(16) yes C55 . B2 . C67 . 112.78(17) yes C61 . B2 . C67 . 104.54(16) yes C55 . B2 . C73 . 103.25(16) yes C61 . B2 . C73 . 116.85(17) yes C67 . B2 . C73 . 111.33(17) yes B1 . C31 . C32 . 121.22(17) yes B1 . C31 . C36 . 123.75(17) yes C32 . C31 . C36 . 115.00(18) yes C31 . C32 . C33 . 123.2(2) yes C31 . C32 . H321 . 118.4 no C33 . C32 . H321 . 118.4 no C32 . C33 . C34 . 119.9(2) yes C32 . C33 . H331 . 120.0 no C34 . C33 . H331 . 120.0 no C33 . C34 . C35 . 118.8(2) yes C33 . C34 . H341 . 120.6 no C35 . C34 . H341 . 120.6 no C34 . C35 . C36 . 120.6(2) yes C34 . C35 . H351 . 119.7 no C36 . C35 . H351 . 119.7 no C31 . C36 . C35 . 122.5(2) yes C31 . C36 . H361 . 118.8 no C35 . C36 . H361 . 118.8 no B1 . C37 . C38 . 124.62(16) yes B1 . C37 . C42 . 120.67(16) yes C38 . C37 . C42 . 114.71(17) yes C37 . C38 . C39 . 123.02(19) yes C37 . C38 . H381 . 118.5 no C39 . C38 . H381 . 118.5 no C38 . C39 . C40 . 120.2(2) yes C38 . C39 . H391 . 119.9 no C40 . C39 . H391 . 119.9 no C39 . C40 . C41 . 119.0(2) yes C39 . C40 . H401 . 120.5 no C41 . C40 . H401 . 120.5 no C40 . C41 . C42 . 119.9(2) yes C40 . C41 . H411 . 120.1 no C42 . C41 . H411 . 120.1 no C37 . C42 . C41 . 123.07(19) yes C37 . C42 . H421 . 118.5 no C41 . C42 . H421 . 118.5 no B1 . C43 . C44 . 120.41(16) yes B1 . C43 . C48 . 124.86(17) yes C44 . C43 . C48 . 114.73(17) yes C43 . C44 . C45 . 123.48(19) yes C43 . C44 . H441 . 118.3 no C45 . C44 . H441 . 118.3 no C44 . C45 . C46 . 119.9(2) yes C44 . C45 . H451 . 120.1 no C46 . C45 . H451 . 120.1 no C45 . C46 . C47 . 119.01(19) yes C45 . C46 . H461 . 120.5 no C47 . C46 . H461 . 120.5 no C46 . C47 . C48 . 120.5(2) yes C46 . C47 . H471 . 119.7 no C48 . C47 . H471 . 119.7 no C47 . C48 . C43 . 122.36(19) yes C47 . C48 . H481 . 118.8 no C43 . C48 . H481 . 118.8 no B1 . C49 . C50 . 123.21(16) yes B1 . C49 . C54 . 121.35(17) yes C50 . C49 . C54 . 115.25(17) yes C49 . C50 . C51 . 122.51(18) yes C49 . C50 . H501 . 118.7 no C51 . C50 . H501 . 118.7 no C50 . C51 . C52 . 120.46(19) yes C50 . C51 . H511 . 119.8 no C52 . C51 . H511 . 119.8 no C51 . C52 . C53 . 118.73(18) yes C51 . C52 . H521 . 120.6 no C53 . C52 . H521 . 120.6 no C52 . C53 . C54 . 120.33(19) yes C52 . C53 . H531 . 119.8 no C54 . C53 . H531 . 119.8 no C49 . C54 . C53 . 122.71(19) yes C49 . C54 . H541 . 118.6 no C53 . C54 . H541 . 118.7 no B2 . C55 . C56 . 122.57(19) yes B2 . C55 . C60 . 121.96(18) yes C56 . C55 . C60 . 115.3(2) yes C55 . C56 . C57 . 122.4(2) yes C55 . C56 . H561 . 118.8 no C57 . C56 . H561 . 118.8 no C56 . C57 . C58 . 120.3(2) yes C56 . C57 . H571 . 119.9 no C58 . C57 . H571 . 119.9 no C57 . C58 . C59 . 118.8(2) yes C57 . C58 . H581 . 120.6 no C59 . C58 . H581 . 120.6 no C58 . C59 . C60 . 120.3(2) yes C58 . C59 . H591 . 119.9 no C60 . C59 . H591 . 119.9 no C55 . C60 . C59 . 122.9(2) yes C55 . C60 . H601 . 118.5 no C59 . C60 . H601 . 118.5 no B2 . C61 . C62 . 118.03(18) yes B2 . C61 . C66 . 127.0(2) yes C62 . C61 . C66 . 115.00(19) yes C61 . C62 . C63 . 123.7(2) yes C61 . C62 . H621 . 118.2 no C63 . C62 . H621 . 118.2 no C62 . C63 . C64 . 119.7(2) yes C62 . C63 . H631 . 120.1 no C64 . C63 . H631 . 120.1 no C63 . C64 . C65 . 118.7(2) yes C63 . C64 . H641 . 120.6 no C65 . C64 . H641 . 120.6 no C64 . C65 . C66 . 120.5(2) yes C64 . C65 . H651 . 119.7 no C66 . C65 . H651 . 119.7 no C65 . C66 . C61 . 122.3(2) yes C65 . C66 . H661 . 118.9 no C61 . C66 . H661 . 118.9 no B2 . C67 . C68 . 120.0(2) yes B2 . C67 . C72 . 124.6(2) yes C68 . C67 . C72 . 115.1(2) yes C67 . C68 . C69 . 122.9(3) yes C67 . C68 . H681 . 118.6 no C69 . C68 . H681 . 118.6 no C68 . C69 . C70 . 120.0(3) yes C68 . C69 . H691 . 120.0 no C70 . C69 . H691 . 120.0 no C69 . C70 . C71 . 119.2(2) yes C69 . C70 . H701 . 120.4 no C71 . C70 . H701 . 120.4 no C70 . C71 . C72 . 120.4(3) yes C70 . C71 . H711 . 119.8 no C72 . C71 . H711 . 119.8 no C71 . C72 . C67 . 122.4(3) yes C71 . C72 . H721 . 118.8 no C67 . C72 . H721 . 118.8 no B2 . C73 . C74 . 120.35(18) yes B2 . C73 . C78 . 124.25(19) yes C74 . C73 . C78 . 114.9(2) yes C73 . C74 . C75 . 123.0(2) yes C73 . C74 . H741 . 118.5 no C75 . C74 . H741 . 118.5 no C74 . C75 . C76 . 120.5(2) yes C74 . C75 . H751 . 119.8 no C76 . C75 . H751 . 119.8 no C75 . C76 . C77 . 118.4(2) yes C75 . C76 . H761 . 120.8 no C77 . C76 . H761 . 120.8 no C76 . C77 . C78 . 120.6(2) yes C76 . C77 . H771 . 119.7 no C78 . C77 . H771 . 119.7 no C73 . C78 . C77 . 122.6(2) yes C73 . C78 . H781 . 118.7 no C77 . C78 . H781 . 118.7 no C23 . C79 . S1 . 116.6(3) yes S1 . C79 . S2 . 106.7(2) yes C23 . C79 . C80 . 136.3(3) yes S1 . C79 . C80 . 106.7(2) yes C82 . C81 . C80 . 110.0(3) yes C82 . C81 . H811 . 125.0 no C80 . C81 . H811 . 125.0 no Br1 . C82 . C81 . 127.6(3) yes Br1 . C82 . S1 . 118.1(3) yes C81 . C82 . S1 . 114.3(3) yes C23 . C85 . S2 . 110.1(4) yes C23 . C85 . C86 . 140.0(6) yes S2 . C85 . C86 . 109.0(6) yes C88 . C87 . C86 . 108.2(6) yes C88 . C87 . H871 . 126.9 no C86 . C87 . H871 . 124.2 no Br2 . C88 . C87 . 121.3(6) yes Br2 . C88 . S2 . 124.0(5) yes C87 . C88 . S2 . 114.7(6) yes C82 . S1 . C79 . 89.55(19) yes C88 . S2 . C85 . 89.8(4) yes C85 . C86 . C87 . 117.6(5) yes C85 . C86 . H861 . 121.2 no C87 . C86 . H861 . 121.2 no C79 . C80 . C81 . 119.4(3) yes C79 . C80 . H801 . 120.3 no C81 . C80 . H801 . 120.3 no N90 . C91 . C92 . 168(2) yes C91 . C92 . H921 . 109.7 no C91 . C92 . H922 . 109.4 no H921 . C92 . H922 . 109.5 no C91 . C92 . H923 . 109.3 no H921 . C92 . H923 . 109.5 no H922 . C92 . H923 . 109.5 no C94 . C93 . H931 . 109.6 no C94 . C93 . H932 . 109.4 no H931 . C93 . H932 . 109.5 no C94 . C93 . H933 . 109.5 no H931 . C93 . H933 . 109.5 no H932 . C93 . H933 . 109.5 no C93 . C94 . N94 . 176.5(12) yes N90 . C95 . C96 . 166(2) yes C95 . C96 . H961 . 108.9 no C95 . C96 . H962 . 109.9 no H961 . C96 . H962 . 109.5 no C95 . C96 . H963 . 109.5 no H961 . C96 . H963 . 109.5 no H962 . C96 . H963 . 109.5 no # start Validation Reply Form _vrf_PLAT432_em94_173k ; PROBLEM: Short Inter X...Y Contact C93 .. C96 .. 2.13 Ang. RESPONSE: Short contacts arise from fractional occupancies ; # end Validation Reply Form # Attachment '[Ru_2_2][PF6]2.cif' data_em148 _database_code_depnum_ccdc_archive 'CCDC 694387' _audit_creation_date 07-10-16 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '10161333 em148_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 21.9200(5) _cell_length_b 16.6540(3) _cell_length_c 27.7472(6) _cell_angle_alpha 90 _cell_angle_beta 111.2193(8) _cell_angle_gamma 90 _cell_volume 9442.5(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C76 H48 Br4 F24 N12 P4 Ru2 S4 # Dc = 1.66 Fooo = 5064.00 Mu = 22.63 M = 2359.17 # Found Formula = C86 H63 Br4 F24 N17 P4 Ru2 S4 # Dc = 1.80 FOOO = 5064.00 Mu = 22.73 M = 2564.43 _chemical_formula_sum 'C86 H63 Br4 F24 N17 P4 Ru2 S4' _chemical_formula_moiety '2(C38 H24 Br2 N6 Ru S2), 4(F6 P), 5(C2 H3 N)' _chemical_compound_source ? _chemical_formula_weight 2564.43 _cell_measurement_reflns_used 35873 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 5064 _exptl_absorpt_coefficient_mu 2.273 # Sheldrick geometric approximatio 0.58 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.96 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 73683 _reflns_number_total 21466 _diffrn_reflns_av_R_equivalents 0.060 # Number of reflections with Friedels Law is 21466 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 21489 _diffrn_reflns_theta_min 0.996 _diffrn_reflns_theta_max 27.415 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.415 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _reflns_limit_h_min -28 _reflns_limit_h_max 26 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 35 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.94 _refine_diff_density_max 1.53 _refine_ls_number_reflns 13157 _refine_ls_number_restraints 208 _refine_ls_number_parameters 1270 #_refine_ls_R_factor_ref 0.0468 _refine_ls_wR_factor_ref 0.0493 _refine_ls_goodness_of_fit_ref 1.1311 #_reflns_number_all 21242 _refine_ls_R_factor_all 0.0855 _refine_ls_wR_factor_all 0.0612 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>1.5\s(I) _reflns_number_gt 13157 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_gt 0.0493 _refine_ls_shift/su_max 0.001381 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.44 1.38 1.08 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ru1 Ru 0.019274(14) 0.260394(16) 0.200554(12) 0.0239 1.0000 Uani . . . . . . Ru2 Ru 0.521729(14) 0.276834(16) 0.698437(12) 0.0234 1.0000 Uani . . . . . . N1 N -0.01345(14) 0.17941(17) 0.24198(12) 0.0234 1.0000 Uani . . . . . . N2 N -0.07628(14) 0.26725(17) 0.16282(12) 0.0228 1.0000 Uani . . . . . . N3 N 0.01428(15) 0.34503(18) 0.14485(13) 0.0268 1.0000 Uani . . . . . . N4 N 0.03254(15) 0.34699(18) 0.25655(13) 0.0269 1.0000 Uani . . . . . . N5 N 0.11445(15) 0.25162(18) 0.23933(13) 0.0261 1.0000 Uani . . . . . . N6 N 0.04376(15) 0.17014(18) 0.15956(12) 0.0248 1.0000 Uani . . . . . . N7 N 0.49315(15) 0.19852(18) 0.74365(13) 0.0277 1.0000 Uani . . . . . . N8 N 0.42554(15) 0.27837(17) 0.66177(13) 0.0253 1.0000 Uani . . . . . . N9 N 0.51197(15) 0.35840(18) 0.63929(12) 0.0256 1.0000 Uani . . . . . . N10 N 0.53334(15) 0.36879(18) 0.75121(12) 0.0254 1.0000 Uani . . . . . . N11 N 0.61713(15) 0.27222(17) 0.73707(12) 0.0252 1.0000 Uani . . . . . . N12 N 0.54821(15) 0.18237(18) 0.66112(13) 0.0263 1.0000 Uani . . . . . . C1 C 0.0225(2) 0.1354(2) 0.28281(16) 0.0329 1.0000 Uani . . . . . . C2 C -0.0053(2) 0.0851(3) 0.30871(17) 0.0369 1.0000 Uani . . . . . . C3 C -0.0723(2) 0.0796(3) 0.29238(18) 0.0386 1.0000 Uani . . . . . . C4 C -0.1101(2) 0.1248(2) 0.25064(16) 0.0324 1.0000 Uani . . . . . . C5 C -0.08044(18) 0.1736(2) 0.22554(15) 0.0265 1.0000 Uani . . . . . . C6 C -0.11658(18) 0.2230(2) 0.17944(15) 0.0248 1.0000 Uani . . . . . . C7 C -0.18385(17) 0.2272(2) 0.15410(15) 0.0255 1.0000 Uani . . . . . . C8 C -0.21002(19) 0.2772(2) 0.11101(15) 0.0270 1.0000 Uani . . . . . . C9 C -0.16674(19) 0.3213(2) 0.09433(15) 0.0277 1.0000 Uani . . . . . . C10 C -0.10037(19) 0.3157(2) 0.12123(15) 0.0271 1.0000 Uani . . . . . . C11 C -0.04776(19) 0.3598(2) 0.11078(15) 0.0284 1.0000 Uani . . . . . . C12 C -0.0602(2) 0.4127(2) 0.06969(18) 0.0372 1.0000 Uani . . . . . . C13 C -0.0070(3) 0.4513(3) 0.06375(18) 0.0433 1.0000 Uani . . . . . . C14 C 0.0551(2) 0.4377(2) 0.09811(19) 0.0397 1.0000 Uani . . . . . . C15 C 0.0638(2) 0.3849(2) 0.13821(18) 0.0357 1.0000 Uani . . . . . . C16 C -0.0123(2) 0.3971(2) 0.26247(17) 0.0328 1.0000 Uani . . . . . . C17 C 0.0013(2) 0.4512(2) 0.30238(18) 0.0354 1.0000 Uani . . . . . . C18 C 0.0638(2) 0.4534(3) 0.33881(18) 0.0403 1.0000 Uani . . . . . . C19 C 0.1117(2) 0.4030(3) 0.33365(17) 0.0351 1.0000 Uani . . . . . . C20 C 0.09525(18) 0.3507(2) 0.29194(15) 0.0263 1.0000 Uani . . . . . . C21 C 0.14314(18) 0.2968(2) 0.28189(16) 0.0271 1.0000 Uani . . . . . . C22 C 0.20896(19) 0.2904(2) 0.30954(16) 0.0318 1.0000 Uani . . . . . . C23 C 0.24722(18) 0.2372(2) 0.29323(17) 0.0294 1.0000 Uani . . . . . . C24 C 0.21633(18) 0.1904(2) 0.24937(16) 0.0280 1.0000 Uani . . . . . . C25 C 0.14976(18) 0.1977(2) 0.22309(15) 0.0266 1.0000 Uani . . . . . . C26 C 0.10885(19) 0.1511(2) 0.17788(16) 0.0280 1.0000 Uani . . . . . . C27 C 0.1331(2) 0.0902(2) 0.15574(17) 0.0326 1.0000 Uani . . . . . . C28 C 0.0905(2) 0.0487(3) 0.11374(18) 0.0389 1.0000 Uani . . . . . . C29 C 0.0250(2) 0.0693(2) 0.09463(18) 0.0366 1.0000 Uani . . . . . . C30 C 0.0032(2) 0.1295(2) 0.11846(16) 0.0304 1.0000 Uani . . . . . . C31 C -0.28080(18) 0.2856(2) 0.08377(15) 0.0283 1.0000 Uani . . . . . . C32 C -0.31345(19) 0.3416(2) 0.04741(16) 0.0310 1.0000 Uani . . . . . . C33 C -0.3821(2) 0.3300(2) 0.02961(16) 0.0323 1.0000 Uani . . . . . . C34 C -0.4020(2) 0.2677(2) 0.05211(17) 0.0350 1.0000 Uani . . . . . . C35 C 0.31789(19) 0.2315(2) 0.32225(16) 0.0314 1.0000 Uani . . . . . . C36 C 0.3556(2) 0.2778(3) 0.36245(18) 0.0369 1.0000 Uani . . . . . . C37 C 0.4220(2) 0.2558(3) 0.37942(18) 0.0388 1.0000 Uani . . . . . . C38 C 0.4350(2) 0.1941(3) 0.35391(19) 0.0440 1.0000 Uani . . . . . . C41 C 0.53162(19) 0.1592(2) 0.78588(16) 0.0318 1.0000 Uani . . . . . . C42 C 0.5067(2) 0.1100(3) 0.81458(18) 0.0379 1.0000 Uani . . . . . . C43 C 0.4404(2) 0.1004(2) 0.79918(17) 0.0362 1.0000 Uani . . . . . . C44 C 0.3990(2) 0.1394(2) 0.75488(17) 0.0341 1.0000 Uani . . . . . . C45 C 0.42626(18) 0.1883(2) 0.72745(15) 0.0282 1.0000 Uani . . . . . . C46 C 0.38768(18) 0.2331(2) 0.68076(15) 0.0268 1.0000 Uani . . . . . . C47 C 0.31988(18) 0.2331(2) 0.65563(15) 0.0279 1.0000 Uani . . . . . . C48 C 0.29158(18) 0.2804(2) 0.61213(15) 0.0256 1.0000 Uani . . . . . . C49 C 0.33245(19) 0.3257(2) 0.59374(16) 0.0296 1.0000 Uani . . . . . . C50 C 0.39893(19) 0.3245(2) 0.61951(15) 0.0271 1.0000 Uani . . . . . . C51 C 0.44843(18) 0.3720(2) 0.60720(15) 0.0279 1.0000 Uani . . . . . . C52 C 0.4330(2) 0.4274(3) 0.56782(17) 0.0374 1.0000 Uani . . . . . . C53 C 0.4827(2) 0.4702(3) 0.55983(18) 0.0404 1.0000 Uani . . . . . . C54 C 0.5464(2) 0.4559(2) 0.59169(18) 0.0379 1.0000 Uani . . . . . . C55 C 0.5600(2) 0.4005(2) 0.63139(17) 0.0323 1.0000 Uani . . . . . . C56 C 0.48689(19) 0.4180(2) 0.75526(16) 0.0309 1.0000 Uani . . . . . . C57 C 0.5003(2) 0.4771(3) 0.79270(18) 0.0373 1.0000 Uani . . . . . . C58 C 0.5644(2) 0.4858(3) 0.82764(19) 0.0413 1.0000 Uani . . . . . . C59 C 0.6125(2) 0.4360(3) 0.82306(17) 0.0380 1.0000 Uani . . . . . . C60 C 0.59624(19) 0.3783(2) 0.78477(15) 0.0275 1.0000 Uani . . . . . . C61 C 0.64461(18) 0.3221(2) 0.77734(15) 0.0264 1.0000 Uani . . . . . . C62 C 0.71051(18) 0.3179(2) 0.80671(15) 0.0267 1.0000 Uani . . . . . . C63 C 0.74959(18) 0.2606(2) 0.79411(15) 0.0268 1.0000 Uani . . . . . . C64 C 0.71952(17) 0.2084(2) 0.75265(15) 0.0256 1.0000 Uani . . . . . . C65 C 0.65337(19) 0.2151(2) 0.72512(15) 0.0269 1.0000 Uani . . . . . . C66 C 0.61357(19) 0.1631(2) 0.68219(15) 0.0260 1.0000 Uani . . . . . . C67 C 0.6387(2) 0.0985(2) 0.66388(17) 0.0332 1.0000 Uani . . . . . . C68 C 0.5971(2) 0.0533(3) 0.62343(19) 0.0395 1.0000 Uani . . . . . . C69 C 0.5320(2) 0.0740(3) 0.60192(19) 0.0392 1.0000 Uani . . . . . . C70 C 0.5088(2) 0.1387(2) 0.62187(15) 0.0300 1.0000 Uani . . . . . . C71 C 0.22041(18) 0.2847(2) 0.58435(15) 0.0274 1.0000 Uani . . . . . . C72 C 0.18526(19) 0.3374(2) 0.54684(16) 0.0308 1.0000 Uani . . . . . . C73 C 0.11799(19) 0.3220(2) 0.52940(16) 0.0319 1.0000 Uani . . . . . . C74 C 0.10004(19) 0.2599(2) 0.55330(17) 0.0342 1.0000 Uani . . . . . . C75 C 0.82008(19) 0.2564(2) 0.82430(16) 0.0291 1.0000 Uani . . . . . . C76 C 0.8565(2) 0.3047(2) 0.86394(17) 0.0336 1.0000 Uani . . . . . . C77 C 0.9233(2) 0.2829(3) 0.88225(18) 0.0364 1.0000 Uani . . . . . . C78 C 0.9379(2) 0.2197(3) 0.85777(18) 0.0374 1.0000 Uani . . . . . . S1 S -0.33533(5) 0.22046(6) 0.09561(4) 0.0312 1.0000 Uani . . . . . . S2 S 0.36525(5) 0.16036(7) 0.30647(5) 0.0421 1.0000 Uani . . . . . . S3 S 0.16839(5) 0.21730(6) 0.59805(4) 0.0330 1.0000 Uani . . . . . . S4 S 0.86847(5) 0.18425(7) 0.81063(5) 0.0383 1.0000 Uani . . . . . . Br1 Br -0.44077(2) 0.39813(3) -0.01996(2) 0.0482 1.0000 Uani . . . . . . Br2 Br 0.48746(2) 0.31187(3) 0.43228(2) 0.0549 1.0000 Uani . . . . . . Br3 Br 0.05698(2) 0.38315(3) 0.47655(2) 0.0476 1.0000 Uani . . . . . . Br4 Br 0.98744(2) 0.33812(3) 0.93642(2) 0.0540 1.0000 Uani . . . . . . P1 P 0.26104(6) 0.49643(7) 0.26985(6) 0.0450 1.0000 Uani . . . . . . P2 P 0.18904(5) 0.00734(6) 0.32554(4) 0.0324 1.0000 Uani . . . . . . P3 P 0.30491(5) 0.52052(6) 0.66696(5) 0.0340 1.0000 Uani . . . . . . P4 P 0.77254(8) 0.01140(11) 0.45229(6) 0.0623 1.0000 Uani D U . . . . F1 F 0.19895(15) 0.47860(18) 0.28517(15) 0.0619 1.0000 Uani . . . . . . F2 F 0.32348(14) 0.51444(16) 0.25522(14) 0.0549 1.0000 Uani . . . . . . F3 F 0.30757(17) 0.4550(2) 0.32234(16) 0.0713 1.0000 Uani . . . . . . F4 F 0.21476(14) 0.53769(17) 0.21777(12) 0.0517 1.0000 Uani . . . . . . F5 F 0.27049(14) 0.58194(17) 0.29903(13) 0.0549 1.0000 Uani . . . . . . F6 F 0.25166(16) 0.41171(17) 0.24138(17) 0.0684 1.0000 Uani . . . . . . F11 F 0.24027(16) -0.01438(18) 0.38113(12) 0.0604 1.0000 Uani . . . . . . F12 F 0.13715(14) 0.02880(17) 0.26949(11) 0.0502 1.0000 Uani . . . . . . F13 F 0.12993(14) -0.01601(17) 0.34364(13) 0.0527 1.0000 Uani . . . . . . F14 F 0.24690(14) 0.03116(16) 0.30660(14) 0.0574 1.0000 Uani . . . . . . F15 F 0.18505(14) 0.09834(15) 0.34299(12) 0.0484 1.0000 Uani . . . . . . F16 F 0.19163(15) -0.08327(15) 0.30717(12) 0.0510 1.0000 Uani . . . . . . F21 F 0.24525(15) 0.54564(17) 0.68321(17) 0.0686 1.0000 Uani . . . . . . F22 F 0.36541(15) 0.49509(18) 0.65132(13) 0.0562 1.0000 Uani . . . . . . F23 F 0.35489(15) 0.54185(18) 0.72378(11) 0.0529 1.0000 Uani . . . . . . F24 F 0.25591(17) 0.4986(2) 0.61053(13) 0.0682 1.0000 Uani . . . . . . F25 F 0.31036(15) 0.61110(15) 0.64959(13) 0.0536 1.0000 Uani . . . . . . F26 F 0.30003(15) 0.43007(15) 0.68489(13) 0.0527 1.0000 Uani . . . . . . F31 F 0.78099(19) 0.0153(2) 0.51143(13) 0.0756 1.0000 Uani D U . . . . F32 F 0.7668(2) 0.0150(4) 0.39408(15) 0.1323 1.0000 Uani D U . . . . F33 F 0.7007(2) 0.0434(4) 0.43793(19) 0.1353 1.0000 Uani D U . . . . F34 F 0.84506(17) -0.0191(3) 0.46782(15) 0.0860 1.0000 Uani D U . . . . F35 F 0.7996(3) 0.1024(3) 0.4595(2) 0.1330 1.0000 Uani D U . . . . F36 F 0.7479(3) -0.0760(3) 0.4477(2) 0.1267 1.0000 Uani D U . . . . N13 N 0.4092(4) 0.2213(4) 0.5185(2) 0.0945 1.0000 Uani D U . . . . N14 N 0.8368(4) 0.4248(7) 0.5617(5) 0.1545 1.0000 Uani D U . . . . N15 N 0.2394(4) 0.3102(4) 0.4405(3) 0.0867 1.0000 Uani D U . . . . N16 N 0.6454(3) 0.3825(4) 0.4703(2) 0.0857 1.0000 Uani D U . . . . N17 N 0.9225(5) 0.2679(5) 0.5162(4) 0.1271 1.0000 Uani D U . . . . C81 C 0.3771(3) 0.1743(4) 0.4898(2) 0.0682 1.0000 Uani D U . . . . C82 C 0.3373(4) 0.1146(4) 0.4538(3) 0.0803 1.0000 Uani D U . . . . C83 C 0.7898(4) 0.4528(6) 0.5670(4) 0.1172 1.0000 Uani D U . . . . C84 C 0.7319(5) 0.4856(6) 0.5731(5) 0.1175 1.0000 Uani D U . . . . C85 C 0.2071(3) 0.2569(4) 0.4421(3) 0.0707 1.0000 Uani D U . . . . C86 C 0.1659(5) 0.1902(5) 0.4439(4) 0.1031 1.0000 Uani D U . . . . C87 C 0.6559(4) 0.3258(4) 0.4507(3) 0.0800 1.0000 Uani D U . . . . C88 C 0.6622(6) 0.2550(5) 0.4231(4) 0.1090 1.0000 Uani D U . . . . C89 C 0.8823(4) 0.3075(5) 0.4871(3) 0.0879 1.0000 Uani D U . . . . C90 C 0.8392(6) 0.3612(8) 0.4493(5) 0.1498 1.0000 Uani D U . . . . H11 H 0.0678 0.1392 0.2936 0.0360 1.0000 Uiso R . . . . . H21 H 0.0211 0.0554 0.3372 0.0429 1.0000 Uiso R . . . . . H31 H -0.0919 0.0468 0.3097 0.0481 1.0000 Uiso R . . . . . H41 H -0.1554 0.1221 0.2394 0.0372 1.0000 Uiso R . . . . . H71 H -0.2115 0.1969 0.1658 0.0329 1.0000 Uiso R . . . . . H91 H -0.1824 0.3534 0.0651 0.0340 1.0000 Uiso R . . . . . H121 H -0.1028 0.4209 0.0461 0.0449 1.0000 Uiso R . . . . . H131 H -0.0134 0.4856 0.0359 0.0560 1.0000 Uiso R . . . . . H141 H 0.0910 0.4636 0.0947 0.0549 1.0000 Uiso R . . . . . H151 H 0.1059 0.3752 0.1619 0.0459 1.0000 Uiso R . . . . . H161 H -0.0543 0.3947 0.2379 0.0378 1.0000 Uiso R . . . . . H171 H -0.0311 0.4853 0.3050 0.0431 1.0000 Uiso R . . . . . H181 H 0.0743 0.4888 0.3665 0.0450 1.0000 Uiso R . . . . . H191 H 0.1537 0.4039 0.3580 0.0401 1.0000 Uiso R . . . . . H221 H 0.2282 0.3203 0.3392 0.0339 1.0000 Uiso R . . . . . H241 H 0.2405 0.1542 0.2381 0.0320 1.0000 Uiso R . . . . . H271 H 0.1770 0.0771 0.1685 0.0410 1.0000 Uiso R . . . . . H281 H 0.1062 0.0079 0.0989 0.0469 1.0000 Uiso R . . . . . H291 H -0.0042 0.0433 0.0660 0.0450 1.0000 Uiso R . . . . . H301 H -0.0411 0.1432 0.1057 0.0360 1.0000 Uiso R . . . . . H321 H -0.2930 0.3826 0.0366 0.0347 1.0000 Uiso R . . . . . H341 H -0.4450 0.2527 0.0449 0.0401 1.0000 Uiso R . . . . . H361 H 0.3395 0.3191 0.3767 0.0389 1.0000 Uiso R . . . . . H381 H 0.4766 0.1722 0.3604 0.0479 1.0000 Uiso R . . . . . H411 H 0.5770 0.1662 0.7959 0.0379 1.0000 Uiso R . . . . . H421 H 0.5349 0.0832 0.8438 0.0448 1.0000 Uiso R . . . . . H431 H 0.4224 0.0689 0.8184 0.0450 1.0000 Uiso R . . . . . H441 H 0.3540 0.1339 0.7444 0.0420 1.0000 Uiso R . . . . . H471 H 0.2941 0.2018 0.6683 0.0330 1.0000 Uiso R . . . . . H491 H 0.3146 0.3556 0.5639 0.0340 1.0000 Uiso R . . . . . H521 H 0.3898 0.4358 0.5462 0.0430 1.0000 Uiso R . . . . . H531 H 0.4732 0.5067 0.5328 0.0490 1.0000 Uiso R . . . . . H541 H 0.5802 0.4836 0.5864 0.0510 1.0000 Uiso R . . . . . H551 H 0.6028 0.3918 0.6534 0.0409 1.0000 Uiso R . . . . . H561 H 0.4444 0.4119 0.7316 0.0348 1.0000 Uiso R . . . . . H571 H 0.4672 0.5109 0.7944 0.0459 1.0000 Uiso R . . . . . H581 H 0.5746 0.5250 0.8529 0.0500 1.0000 Uiso R . . . . . H591 H 0.6554 0.4420 0.8455 0.0441 1.0000 Uiso R . . . . . H621 H 0.7291 0.3520 0.8343 0.0340 1.0000 Uiso R . . . . . H641 H 0.7441 0.1696 0.7441 0.0319 1.0000 Uiso R . . . . . H671 H 0.6827 0.0863 0.6780 0.0390 1.0000 Uiso R . . . . . H681 H 0.6129 0.0092 0.6114 0.0489 1.0000 Uiso R . . . . . H691 H 0.5035 0.0456 0.5738 0.0459 1.0000 Uiso R . . . . . H701 H 0.4648 0.1525 0.6077 0.0349 1.0000 Uiso R . . . . . H721 H 0.2037 0.3786 0.5343 0.0378 1.0000 Uiso R . . . . . H741 H 0.0573 0.2430 0.5464 0.0370 1.0000 Uiso R . . . . . H761 H 0.8398 0.3469 0.8769 0.0417 1.0000 Uiso R . . . . . H821 H 0.3154 0.1393 0.4207 0.1201 1.0000 Uiso R . . . . . H822 H 0.3662 0.0730 0.4512 0.1200 1.0000 Uiso R . . . . . H823 H 0.3061 0.0931 0.4674 0.1201 1.0000 Uiso R . . . . . H841 H 0.7274 0.5425 0.5658 0.1910 1.0000 Uiso R . . . . . H842 H 0.7377 0.4758 0.6090 0.1911 1.0000 Uiso R . . . . . H843 H 0.6934 0.4575 0.5508 0.1910 1.0000 Uiso R . . . . . H861 H 0.1634 0.1876 0.4780 0.1630 1.0000 Uiso R . . . . . H862 H 0.1844 0.1407 0.4374 0.1630 1.0000 Uiso R . . . . . H863 H 0.1226 0.1966 0.4187 0.1631 1.0000 Uiso R . . . . . H881 H 0.6976 0.2224 0.4455 0.1801 1.0000 Uiso R . . . . . H882 H 0.6724 0.2700 0.3930 0.1801 1.0000 Uiso R . . . . . H883 H 0.6222 0.2236 0.4119 0.1801 1.0000 Uiso R . . . . . H901 H 0.8030 0.3309 0.4254 0.2221 1.0000 Uiso R . . . . . H902 H 0.8243 0.4003 0.4685 0.2221 1.0000 Uiso R . . . . . H903 H 0.8648 0.3863 0.4315 0.2222 1.0000 Uiso R . . . . . H781 H 0.9797 0.1980 0.8650 0.0439 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01910(14) 0.02395(14) 0.02979(17) -0.00082(11) 0.01037(12) -0.00103(10) Ru2 0.01853(14) 0.02322(14) 0.02915(16) 0.00024(11) 0.00931(12) 0.00047(10) N1 0.0207(15) 0.0231(14) 0.0263(16) 0.0007(11) 0.0082(13) 0.0005(11) N2 0.0226(15) 0.0224(13) 0.0226(15) 0.0009(11) 0.0071(12) -0.0012(11) N3 0.0265(16) 0.0236(14) 0.0360(18) -0.0047(13) 0.0183(14) -0.0031(12) N4 0.0221(15) 0.0276(15) 0.0334(17) -0.0008(12) 0.0131(13) -0.0002(12) N5 0.0208(15) 0.0287(15) 0.0308(17) -0.0001(12) 0.0118(13) -0.0038(11) N6 0.0202(15) 0.0255(14) 0.0296(17) 0.0014(12) 0.0100(13) -0.0018(11) N7 0.0222(15) 0.0261(15) 0.0374(19) 0.0021(13) 0.0139(14) 0.0031(11) N8 0.0218(15) 0.0223(14) 0.0315(17) -0.0004(12) 0.0091(13) 0.0019(11) N9 0.0256(16) 0.0239(14) 0.0303(17) -0.0004(12) 0.0138(13) 0.0004(11) N10 0.0212(15) 0.0253(14) 0.0291(17) -0.0010(12) 0.0083(13) 0.0015(11) N11 0.0241(16) 0.0226(14) 0.0292(17) 0.0016(12) 0.0101(13) 0.0009(11) N12 0.0243(16) 0.0244(14) 0.0321(18) -0.0015(12) 0.0123(14) -0.0032(11) C1 0.0257(19) 0.036(2) 0.037(2) -0.0002(16) 0.0111(17) 0.0044(15) C2 0.034(2) 0.041(2) 0.035(2) 0.0134(17) 0.0116(18) 0.0074(17) C3 0.039(2) 0.037(2) 0.043(3) 0.0169(18) 0.019(2) 0.0012(17) C4 0.0236(19) 0.0356(19) 0.037(2) 0.0097(16) 0.0089(16) 0.0017(15) C5 0.0241(19) 0.0250(17) 0.030(2) -0.0023(14) 0.0089(16) 0.0004(13) C6 0.0223(18) 0.0240(16) 0.031(2) 0.0012(14) 0.0125(15) 0.0007(13) C7 0.0200(17) 0.0266(17) 0.031(2) 0.0006(14) 0.0112(15) -0.0037(13) C8 0.0286(19) 0.0235(17) 0.028(2) -0.0007(14) 0.0098(16) 0.0007(13) C9 0.031(2) 0.0235(16) 0.026(2) 0.0044(13) 0.0079(16) 0.0015(13) C10 0.0271(19) 0.0245(17) 0.032(2) -0.0012(14) 0.0129(16) -0.0055(13) C11 0.033(2) 0.0237(17) 0.031(2) -0.0020(14) 0.0146(17) -0.0019(14) C12 0.043(2) 0.035(2) 0.036(2) 0.0037(17) 0.0175(19) -0.0020(17) C13 0.062(3) 0.038(2) 0.039(2) 0.0002(18) 0.030(2) -0.012(2) C14 0.050(3) 0.034(2) 0.050(3) -0.0050(18) 0.036(2) -0.0122(18) C15 0.037(2) 0.0293(19) 0.049(3) -0.0066(17) 0.025(2) -0.0065(15) C16 0.026(2) 0.0307(19) 0.042(2) 0.0009(16) 0.0126(17) 0.0037(14) C17 0.031(2) 0.035(2) 0.044(2) -0.0044(17) 0.0177(18) 0.0075(16) C18 0.043(2) 0.040(2) 0.038(2) -0.0133(18) 0.015(2) -0.0006(18) C19 0.025(2) 0.041(2) 0.036(2) -0.0085(17) 0.0065(17) -0.0017(16) C20 0.0210(18) 0.0309(18) 0.0275(19) -0.0032(14) 0.0094(15) -0.0004(13) C21 0.0203(17) 0.0284(17) 0.035(2) -0.0041(15) 0.0123(15) -0.0037(13) C22 0.027(2) 0.0316(19) 0.034(2) -0.0009(15) 0.0083(16) -0.0019(15) C23 0.0203(17) 0.0260(17) 0.044(2) 0.0022(15) 0.0140(17) 0.0002(13) C24 0.0258(19) 0.0204(16) 0.039(2) 0.0030(14) 0.0136(16) 0.0031(13) C25 0.0258(18) 0.0247(16) 0.032(2) 0.0028(14) 0.0139(15) 0.0006(13) C26 0.0271(19) 0.0229(16) 0.037(2) 0.0012(15) 0.0155(17) -0.0019(13) C27 0.034(2) 0.0322(19) 0.033(2) -0.0027(15) 0.0139(17) 0.0018(15) C28 0.047(3) 0.032(2) 0.041(2) -0.0068(17) 0.020(2) -0.0008(18) C29 0.038(2) 0.032(2) 0.038(2) -0.0052(17) 0.0116(19) -0.0069(16) C30 0.033(2) 0.0271(17) 0.030(2) 0.0004(14) 0.0105(16) -0.0060(14) C31 0.0240(18) 0.0294(18) 0.029(2) 0.0000(15) 0.0068(15) 0.0014(14) C32 0.029(2) 0.0282(18) 0.031(2) 0.0002(15) 0.0051(16) 0.0060(14) C33 0.031(2) 0.0305(18) 0.029(2) -0.0003(15) 0.0025(17) 0.0062(14) C34 0.028(2) 0.035(2) 0.035(2) -0.0031(16) 0.0036(17) 0.0048(15) C35 0.025(2) 0.0305(18) 0.037(2) 0.0030(15) 0.0096(17) -0.0003(14) C36 0.029(2) 0.035(2) 0.042(2) 0.0025(18) 0.0074(18) 0.0029(16) C37 0.024(2) 0.037(2) 0.045(3) 0.0048(18) -0.0001(18) -0.0020(16) C38 0.021(2) 0.044(2) 0.054(3) -0.002(2) -0.0023(19) 0.0037(16) C41 0.0235(19) 0.0339(19) 0.037(2) 0.0052(16) 0.0090(17) 0.0008(15) C42 0.032(2) 0.037(2) 0.041(3) 0.0065(18) 0.0098(19) 0.0084(16) C43 0.038(2) 0.035(2) 0.037(2) 0.0101(17) 0.0154(19) 0.0013(16) C44 0.028(2) 0.034(2) 0.042(2) 0.0101(17) 0.0154(18) 0.0009(15) C45 0.0230(18) 0.0321(18) 0.029(2) 0.0053(15) 0.0088(15) 0.0024(14) C46 0.0226(18) 0.0273(17) 0.031(2) 0.0023(14) 0.0098(15) 0.0010(13) C47 0.0242(18) 0.0264(17) 0.033(2) 0.0030(14) 0.0107(16) -0.0022(13) C48 0.0228(18) 0.0240(16) 0.030(2) -0.0051(14) 0.0091(15) -0.0009(13) C49 0.0250(19) 0.0327(19) 0.030(2) 0.0049(15) 0.0089(16) -0.0005(14) C50 0.028(2) 0.0241(17) 0.029(2) 0.0005(14) 0.0100(16) 0.0013(13) C51 0.0238(18) 0.0320(18) 0.028(2) -0.0033(15) 0.0093(15) -0.0013(14) C52 0.037(2) 0.041(2) 0.034(2) 0.0075(17) 0.0120(18) -0.0023(17) C53 0.047(3) 0.039(2) 0.039(2) 0.0062(18) 0.020(2) -0.0059(18) C54 0.040(2) 0.033(2) 0.048(3) 0.0015(18) 0.025(2) -0.0092(17) C55 0.029(2) 0.0305(19) 0.042(2) -0.0037(16) 0.0193(18) -0.0033(15) C56 0.0251(19) 0.036(2) 0.034(2) 0.0015(16) 0.0128(16) 0.0067(15) C57 0.034(2) 0.035(2) 0.044(2) -0.0025(17) 0.0161(19) 0.0094(16) C58 0.040(2) 0.039(2) 0.045(3) -0.0159(19) 0.016(2) 0.0023(18) C59 0.030(2) 0.043(2) 0.037(2) -0.0077(18) 0.0074(18) 0.0053(17) C60 0.030(2) 0.0268(17) 0.030(2) -0.0002(14) 0.0161(16) 0.0007(14) C61 0.0210(18) 0.0291(18) 0.029(2) 0.0010(14) 0.0087(15) -0.0018(13) C62 0.0241(19) 0.0306(18) 0.0253(19) -0.0030(14) 0.0089(15) 0.0011(13) C63 0.0194(17) 0.0277(17) 0.033(2) 0.0039(14) 0.0095(15) -0.0006(13) C64 0.0202(17) 0.0283(17) 0.0302(19) 0.0051(14) 0.0114(15) 0.0078(13) C65 0.0278(19) 0.0256(17) 0.029(2) 0.0031(14) 0.0129(16) 0.0003(14) C66 0.0269(19) 0.0238(16) 0.0283(19) 0.0016(14) 0.0113(15) 0.0006(13) C67 0.030(2) 0.0307(19) 0.040(2) 0.0003(16) 0.0146(18) 0.0030(15) C68 0.044(2) 0.032(2) 0.046(3) -0.0056(18) 0.021(2) 0.0038(17) C69 0.045(3) 0.032(2) 0.042(3) -0.0087(17) 0.018(2) -0.0078(17) C70 0.0280(19) 0.0297(18) 0.031(2) 0.0021(15) 0.0089(16) -0.0067(14) C71 0.0229(18) 0.0307(18) 0.0265(19) -0.0032(14) 0.0065(15) -0.0005(14) C72 0.0257(19) 0.0312(18) 0.035(2) -0.0012(15) 0.0107(17) -0.0030(14) C73 0.0207(18) 0.0355(19) 0.033(2) 0.0021(16) 0.0018(16) 0.0049(14) C74 0.0194(18) 0.039(2) 0.040(2) -0.0045(17) 0.0060(17) -0.0002(15) C75 0.0242(19) 0.0288(18) 0.035(2) -0.0016(15) 0.0122(17) 0.0012(14) C76 0.029(2) 0.0295(19) 0.040(2) -0.0034(16) 0.0103(17) 0.0001(15) C77 0.025(2) 0.039(2) 0.041(2) 0.0011(17) 0.0062(17) 0.0004(16) C78 0.0190(19) 0.042(2) 0.041(2) -0.0012(18) -0.0005(17) 0.0042(15) S1 0.0237(5) 0.0329(5) 0.0349(5) 0.0044(4) 0.0082(4) 0.0012(3) S2 0.0231(5) 0.0431(6) 0.0541(7) -0.0100(5) 0.0069(5) 0.0056(4) S3 0.0222(5) 0.0354(5) 0.0395(6) 0.0059(4) 0.0087(4) -0.0006(4) S4 0.0221(5) 0.0409(5) 0.0470(6) -0.0094(4) 0.0065(4) 0.0061(4) Br1 0.0387(3) 0.0441(2) 0.0482(3) 0.0105(2) -0.0005(2) 0.01140(18) Br2 0.0379(3) 0.0496(3) 0.0563(3) -0.0023(2) -0.0079(2) -0.0049(2) Br3 0.0351(2) 0.0498(3) 0.0459(3) 0.0110(2) 0.0004(2) 0.00771(18) Br4 0.0378(3) 0.0464(3) 0.0580(3) -0.0100(2) -0.0066(2) -0.00015(19) P1 0.0366(6) 0.0351(6) 0.0736(8) 0.0131(5) 0.0324(6) 0.0086(4) P2 0.0289(5) 0.0268(5) 0.0408(6) 0.0043(4) 0.0119(4) 0.0039(4) P3 0.0279(5) 0.0279(5) 0.0461(6) -0.0037(4) 0.0133(5) -0.0026(4) P4 0.0659(10) 0.0796(10) 0.0415(7) 0.0021(7) 0.0195(7) 0.0275(8) F1 0.0518(18) 0.0492(16) 0.106(3) 0.0174(16) 0.0536(19) 0.0074(13) F2 0.0426(16) 0.0444(15) 0.092(2) 0.0157(15) 0.0412(16) 0.0081(12) F3 0.059(2) 0.070(2) 0.096(3) 0.0375(19) 0.041(2) 0.0251(16) F4 0.0438(16) 0.0496(15) 0.067(2) 0.0038(14) 0.0268(15) 0.0060(12) F5 0.0450(16) 0.0469(15) 0.077(2) 0.0031(14) 0.0276(16) 0.0086(12) F6 0.0568(19) 0.0361(14) 0.131(3) -0.0007(17) 0.056(2) 0.0040(13) F11 0.062(2) 0.0503(16) 0.0498(17) 0.0083(13) -0.0026(14) 0.0063(14) F12 0.0489(16) 0.0483(15) 0.0462(16) 0.0097(12) 0.0083(13) 0.0042(12) F13 0.0477(16) 0.0489(15) 0.074(2) 0.0164(14) 0.0371(15) 0.0066(12) F14 0.0455(16) 0.0437(15) 0.098(3) 0.0217(15) 0.0445(17) 0.0102(12) F15 0.0533(17) 0.0292(12) 0.0605(18) -0.0053(11) 0.0179(14) 0.0039(11) F16 0.0655(19) 0.0310(13) 0.0604(18) 0.0005(12) 0.0275(15) 0.0053(12) F21 0.0456(17) 0.0422(15) 0.133(3) -0.0218(18) 0.050(2) -0.0083(13) F22 0.0523(17) 0.0528(16) 0.078(2) -0.0149(15) 0.0404(16) -0.0060(13) F23 0.0562(18) 0.0514(16) 0.0443(16) -0.0074(12) 0.0102(14) -0.0076(13) F24 0.063(2) 0.0565(18) 0.060(2) -0.0075(15) -0.0090(16) -0.0061(15) F25 0.0584(18) 0.0310(13) 0.0655(19) 0.0075(12) 0.0154(15) -0.0048(11) F26 0.0632(19) 0.0316(13) 0.070(2) 0.0013(12) 0.0326(16) -0.0033(12) F31 0.076(2) 0.101(3) 0.056(2) -0.0165(18) 0.0305(18) 0.008(2) F32 0.108(3) 0.227(5) 0.058(2) 0.006(3) 0.027(2) 0.057(4) F33 0.094(3) 0.218(5) 0.083(3) -0.014(3) 0.018(3) 0.080(3) F34 0.070(2) 0.119(3) 0.072(2) -0.012(2) 0.0294(19) 0.027(2) F35 0.171(5) 0.092(3) 0.143(4) 0.023(3) 0.067(4) 0.013(3) F36 0.115(4) 0.122(3) 0.147(4) -0.063(3) 0.052(3) -0.025(3) N13 0.107(5) 0.101(5) 0.053(3) -0.008(3) 0.002(3) 0.012(4) N14 0.067(5) 0.173(9) 0.182(9) 0.005(7) -0.006(6) -0.008(5) N15 0.107(5) 0.087(4) 0.078(4) 0.024(3) 0.047(4) 0.018(3) N16 0.076(4) 0.096(4) 0.072(4) -0.001(3) 0.011(3) -0.022(3) N17 0.154(8) 0.102(6) 0.108(6) 0.009(4) 0.028(5) 0.025(5) C81 0.074(4) 0.077(4) 0.044(3) -0.005(3) 0.010(3) 0.021(3) C82 0.083(5) 0.078(4) 0.071(4) -0.017(3) 0.019(4) 0.009(3) C83 0.072(5) 0.098(6) 0.142(7) -0.038(5) -0.008(5) -0.016(4) C84 0.103(6) 0.097(6) 0.146(8) -0.024(6) 0.036(6) -0.024(5) C85 0.083(5) 0.085(4) 0.057(4) 0.010(3) 0.039(3) 0.028(3) C86 0.106(6) 0.115(6) 0.111(6) -0.027(5) 0.067(5) -0.005(5) C87 0.078(5) 0.084(4) 0.081(5) 0.020(3) 0.032(4) -0.009(4) C88 0.154(8) 0.089(5) 0.113(7) 0.025(5) 0.083(6) 0.015(5) C89 0.101(6) 0.089(5) 0.075(5) 0.004(4) 0.032(4) 0.008(4) C90 0.157(10) 0.143(9) 0.130(9) 0.025(7) 0.028(7) 0.049(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.08494(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . N1 . 2.062(3) yes Ru1 . N2 . 1.977(3) yes Ru1 . N3 . 2.065(3) yes Ru1 . N4 . 2.062(3) yes Ru1 . N5 . 1.976(3) yes Ru1 . N6 . 2.070(3) yes Ru2 . N7 . 2.058(3) yes Ru2 . N8 . 1.982(3) yes Ru2 . N9 . 2.081(3) yes Ru2 . N10 . 2.070(3) yes Ru2 . N11 . 1.976(3) yes Ru2 . N12 . 2.078(3) yes N1 . C1 . 1.340(5) yes N1 . C5 . 1.375(5) yes N2 . C6 . 1.353(4) yes N2 . C10 . 1.349(5) yes N3 . C11 . 1.369(5) yes N3 . C15 . 1.342(5) yes N4 . C16 . 1.345(5) yes N4 . C20 . 1.371(5) yes N5 . C21 . 1.348(5) yes N5 . C25 . 1.365(5) yes N6 . C26 . 1.367(5) yes N6 . C30 . 1.347(5) yes N7 . C41 . 1.341(5) yes N7 . C45 . 1.380(5) yes N8 . C46 . 1.361(5) yes N8 . C50 . 1.346(5) yes N9 . C51 . 1.374(5) yes N9 . C55 . 1.347(5) yes N10 . C56 . 1.343(5) yes N10 . C60 . 1.365(5) yes N11 . C61 . 1.348(5) yes N11 . C65 . 1.355(5) yes N12 . C66 . 1.375(5) yes N12 . C70 . 1.334(5) yes C1 . C2 . 1.381(6) yes C1 . H11 . 0.930 no C2 . C3 . 1.374(6) yes C2 . H21 . 0.935 no C3 . C4 . 1.378(6) yes C3 . H31 . 0.930 no C4 . C5 . 1.376(5) yes C4 . H41 . 0.929 no C5 . C6 . 1.486(5) yes C6 . C7 . 1.387(5) yes C7 . C8 . 1.399(5) yes C7 . H71 . 0.932 no C8 . C9 . 1.404(5) yes C8 . C31 . 1.466(5) yes C9 . C10 . 1.377(5) yes C9 . H91 . 0.927 no C10 . C11 . 1.482(5) yes C11 . C12 . 1.387(6) yes C12 . C13 . 1.393(6) yes C12 . H121 . 0.935 no C13 . C14 . 1.370(7) yes C13 . H131 . 0.931 no C14 . C15 . 1.376(6) yes C14 . H141 . 0.931 no C15 . H151 . 0.932 no C16 . C17 . 1.374(6) yes C16 . H161 . 0.926 no C17 . C18 . 1.378(6) yes C17 . H171 . 0.933 no C18 . C19 . 1.391(6) yes C18 . H181 . 0.930 no C19 . C20 . 1.387(5) yes C19 . H191 . 0.926 no C20 . C21 . 1.483(5) yes C21 . C22 . 1.371(5) yes C22 . C23 . 1.403(5) yes C22 . H221 . 0.922 no C23 . C24 . 1.397(6) yes C23 . C35 . 1.468(5) yes C24 . C25 . 1.380(5) yes C24 . H241 . 0.927 no C25 . C26 . 1.471(5) yes C26 . C27 . 1.388(5) yes C27 . C28 . 1.385(6) yes C27 . H271 . 0.923 no C28 . C29 . 1.382(6) yes C28 . H281 . 0.923 no C29 . C30 . 1.379(6) yes C29 . H291 . 0.929 no C30 . H301 . 0.933 no C31 . C32 . 1.371(5) yes C31 . S1 . 1.731(4) yes C32 . C33 . 1.416(6) yes C32 . H321 . 0.926 no C33 . C34 . 1.361(6) yes C33 . Br1 . 1.885(4) yes C34 . S1 . 1.713(4) yes C34 . H341 . 0.926 no C35 . C36 . 1.362(6) yes C35 . S2 . 1.733(4) yes C36 . C37 . 1.407(6) yes C36 . H361 . 0.924 no C37 . C38 . 1.335(7) yes C37 . Br2 . 1.886(4) yes C38 . S2 . 1.712(4) yes C38 . H381 . 0.937 no C41 . C42 . 1.385(6) yes C41 . H411 . 0.938 no C42 . C43 . 1.368(6) yes C42 . H421 . 0.937 no C43 . C44 . 1.396(6) yes C43 . H431 . 0.930 no C44 . C45 . 1.388(5) yes C44 . H441 . 0.928 no C45 . C46 . 1.469(5) yes C46 . C47 . 1.394(5) yes C47 . C48 . 1.386(5) yes C47 . H471 . 0.926 no C48 . C49 . 1.401(5) yes C48 . C71 . 1.471(5) yes C49 . C50 . 1.371(5) yes C49 . H491 . 0.923 no C50 . C51 . 1.479(5) yes C51 . C52 . 1.375(6) yes C52 . C53 . 1.385(6) yes C52 . H521 . 0.931 no C53 . C54 . 1.376(7) yes C53 . H531 . 0.928 no C54 . C55 . 1.384(6) yes C54 . H541 . 0.928 no C55 . H551 . 0.928 no C56 . C57 . 1.382(6) yes C56 . H561 . 0.931 no C57 . C58 . 1.396(6) yes C57 . H571 . 0.933 no C58 . C59 . 1.382(6) yes C58 . H581 . 0.925 no C59 . C60 . 1.381(6) yes C59 . H591 . 0.927 no C60 . C61 . 1.483(5) yes C61 . C62 . 1.380(5) yes C62 . C63 . 1.407(5) yes C62 . H621 . 0.921 no C63 . C64 . 1.402(5) yes C63 . C75 . 1.469(5) yes C64 . C65 . 1.377(5) yes C64 . H641 . 0.924 no C65 . C66 . 1.476(5) yes C66 . C67 . 1.386(5) yes C67 . C68 . 1.385(6) yes C67 . H671 . 0.924 no C68 . C69 . 1.376(7) yes C68 . H681 . 0.924 no C69 . C70 . 1.389(6) yes C69 . H691 . 0.932 no C70 . H701 . 0.930 no C71 . C72 . 1.366(5) yes C71 . S3 . 1.737(4) yes C72 . C73 . 1.399(5) yes C72 . H721 . 0.925 no C73 . C74 . 1.361(6) yes C73 . Br3 . 1.886(4) yes C74 . S3 . 1.716(4) yes C74 . H741 . 0.929 no C75 . C76 . 1.363(6) yes C75 . S4 . 1.733(4) yes C76 . C77 . 1.412(6) yes C76 . H761 . 0.923 no C77 . C78 . 1.353(6) yes C77 . Br4 . 1.885(4) yes C78 . S4 . 1.713(4) yes C78 . H781 . 0.936 no P1 . F1 . 1.594(3) yes P1 . F2 . 1.591(3) yes P1 . F3 . 1.601(4) yes P1 . F4 . 1.590(3) yes P1 . F5 . 1.614(3) yes P1 . F6 . 1.594(3) yes P2 . F11 . 1.587(3) yes P2 . F12 . 1.600(3) yes P2 . F13 . 1.598(3) yes P2 . F14 . 1.589(3) yes P2 . F15 . 1.603(3) yes P2 . F16 . 1.600(3) yes P3 . F21 . 1.586(3) yes P3 . F22 . 1.595(3) yes P3 . F23 . 1.601(3) yes P3 . F24 . 1.588(3) yes P3 . F25 . 1.601(3) yes P3 . F26 . 1.602(3) yes P4 . F31 . 1.585(3) yes P4 . F32 . 1.575(4) yes P4 . F33 . 1.571(4) yes P4 . F34 . 1.573(4) yes P4 . F35 . 1.612(5) yes P4 . F36 . 1.542(4) yes N13 . C81 . 1.156(7) yes N14 . C83 . 1.188(8) yes N15 . C85 . 1.146(7) yes N16 . C87 . 1.155(7) yes N17 . C89 . 1.161(7) yes C81 . C82 . 1.454(7) yes C82 . H821 . 0.962 no C82 . H822 . 0.960 no C82 . H823 . 0.963 no C83 . C84 . 1.446(8) yes C84 . H841 . 0.968 no C84 . H842 . 0.971 no C84 . H843 . 0.968 no C85 . C86 . 1.443(8) yes C86 . H861 . 0.969 no C86 . H862 . 0.964 no C86 . H863 . 0.961 no C87 . C88 . 1.439(8) yes C88 . H881 . 0.967 no C88 . H882 . 0.971 no C88 . H883 . 0.971 no C89 . C90 . 1.440(8) yes C90 . H901 . 0.970 no C90 . H902 . 0.969 no C90 . H903 . 0.966 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 79.48(12) yes N1 . Ru1 . N3 . 158.24(12) yes N2 . Ru1 . N3 . 78.77(12) yes N1 . Ru1 . N4 . 91.15(12) yes N2 . Ru1 . N4 . 101.07(12) yes N3 . Ru1 . N4 . 92.37(12) yes N1 . Ru1 . N5 . 99.19(12) yes N2 . Ru1 . N5 . 178.67(12) yes N3 . Ru1 . N5 . 102.56(13) yes N4 . Ru1 . N5 . 78.95(13) yes N1 . Ru1 . N6 . 92.47(12) yes N2 . Ru1 . N6 . 100.76(12) yes N3 . Ru1 . N6 . 92.21(12) yes N4 . Ru1 . N6 . 158.17(12) yes N5 . Ru1 . N6 . 79.22(13) yes N7 . Ru2 . N8 . 79.58(13) yes N7 . Ru2 . N9 . 158.02(12) yes N8 . Ru2 . N9 . 78.47(12) yes N7 . Ru2 . N10 . 91.39(12) yes N8 . Ru2 . N10 . 100.91(12) yes N9 . Ru2 . N10 . 91.50(12) yes N7 . Ru2 . N11 . 98.08(13) yes N8 . Ru2 . N11 . 177.66(12) yes N9 . Ru2 . N11 . 103.87(12) yes N10 . Ru2 . N11 . 79.05(12) yes N7 . Ru2 . N12 . 91.47(12) yes N8 . Ru2 . N12 . 101.02(12) yes N9 . Ru2 . N12 . 93.94(12) yes N10 . Ru2 . N12 . 158.05(12) yes N11 . Ru2 . N12 . 79.00(12) yes Ru1 . N1 . C1 . 127.8(3) yes Ru1 . N1 . C5 . 114.0(2) yes C1 . N1 . C5 . 118.2(3) yes Ru1 . N2 . C6 . 119.0(2) yes Ru1 . N2 . C10 . 119.9(2) yes C6 . N2 . C10 . 121.0(3) yes Ru1 . N3 . C11 . 114.2(2) yes Ru1 . N3 . C15 . 127.9(3) yes C11 . N3 . C15 . 117.9(4) yes Ru1 . N4 . C16 . 128.1(3) yes Ru1 . N4 . C20 . 113.7(2) yes C16 . N4 . C20 . 118.2(3) yes Ru1 . N5 . C21 . 120.1(2) yes Ru1 . N5 . C25 . 118.8(3) yes C21 . N5 . C25 . 121.0(3) yes Ru1 . N6 . C26 . 114.0(2) yes Ru1 . N6 . C30 . 127.3(3) yes C26 . N6 . C30 . 118.6(3) yes Ru2 . N7 . C41 . 127.5(3) yes Ru2 . N7 . C45 . 113.7(2) yes C41 . N7 . C45 . 118.8(3) yes Ru2 . N8 . C46 . 118.6(2) yes Ru2 . N8 . C50 . 120.0(3) yes C46 . N8 . C50 . 121.4(3) yes Ru2 . N9 . C51 . 114.2(2) yes Ru2 . N9 . C55 . 127.2(3) yes C51 . N9 . C55 . 118.5(3) yes Ru2 . N10 . C56 . 127.4(3) yes Ru2 . N10 . C60 . 113.8(2) yes C56 . N10 . C60 . 118.7(3) yes Ru2 . N11 . C61 . 119.6(2) yes Ru2 . N11 . C65 . 119.6(3) yes C61 . N11 . C65 . 120.7(3) yes Ru2 . N12 . C66 . 113.6(2) yes Ru2 . N12 . C70 . 127.2(3) yes C66 . N12 . C70 . 119.1(3) yes N1 . C1 . C2 . 122.4(4) yes N1 . C1 . H11 . 117.9 no C2 . C1 . H11 . 119.7 no C1 . C2 . C3 . 119.3(4) yes C1 . C2 . H21 . 120.4 no C3 . C2 . H21 . 120.3 no C2 . C3 . C4 . 119.1(4) yes C2 . C3 . H31 . 120.5 no C4 . C3 . H31 . 120.4 no C3 . C4 . C5 . 119.8(4) yes C3 . C4 . H41 . 120.0 no C5 . C4 . H41 . 120.1 no C4 . C5 . N1 . 121.1(3) yes C4 . C5 . C6 . 124.1(3) yes N1 . C5 . C6 . 114.8(3) yes C5 . C6 . N2 . 112.6(3) yes C5 . C6 . C7 . 127.0(3) yes N2 . C6 . C7 . 120.4(3) yes C6 . C7 . C8 . 119.7(3) yes C6 . C7 . H71 . 120.1 no C8 . C7 . H71 . 120.2 no C7 . C8 . C9 . 118.5(3) yes C7 . C8 . C31 . 121.8(3) yes C9 . C8 . C31 . 119.7(3) yes C8 . C9 . C10 . 119.5(3) yes C8 . C9 . H91 . 120.6 no C10 . C9 . H91 . 119.9 no C9 . C10 . N2 . 121.0(3) yes C9 . C10 . C11 . 127.2(4) yes N2 . C10 . C11 . 111.9(3) yes C10 . C11 . N3 . 115.1(3) yes C10 . C11 . C12 . 122.7(4) yes N3 . C11 . C12 . 122.2(4) yes C11 . C12 . C13 . 117.8(4) yes C11 . C12 . H121 . 121.1 no C13 . C12 . H121 . 121.0 no C12 . C13 . C14 . 120.3(4) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 119.5 no C13 . C14 . C15 . 118.7(4) yes C13 . C14 . H141 . 121.1 no C15 . C14 . H141 . 120.2 no C14 . C15 . N3 . 123.0(4) yes C14 . C15 . H151 . 119.5 no N3 . C15 . H151 . 117.5 no N4 . C16 . C17 . 123.4(4) yes N4 . C16 . H161 . 117.2 no C17 . C16 . H161 . 119.4 no C16 . C17 . C18 . 118.5(4) yes C16 . C17 . H171 . 120.9 no C18 . C17 . H171 . 120.7 no C17 . C18 . C19 . 119.7(4) yes C17 . C18 . H181 . 120.4 no C19 . C18 . H181 . 119.9 no C18 . C19 . C20 . 119.1(4) yes C18 . C19 . H191 . 120.2 no C20 . C19 . H191 . 120.7 no C19 . C20 . N4 . 121.1(3) yes C19 . C20 . C21 . 123.3(3) yes N4 . C20 . C21 . 115.6(3) yes C20 . C21 . N5 . 111.4(3) yes C20 . C21 . C22 . 127.9(4) yes N5 . C21 . C22 . 120.7(3) yes C21 . C22 . C23 . 119.9(4) yes C21 . C22 . H221 . 120.4 no C23 . C22 . H221 . 119.6 no C22 . C23 . C24 . 118.4(3) yes C22 . C23 . C35 . 119.9(4) yes C24 . C23 . C35 . 121.7(3) yes C23 . C24 . C25 . 119.8(3) yes C23 . C24 . H241 . 119.9 no C25 . C24 . H241 . 120.2 no C24 . C25 . N5 . 120.1(3) yes C24 . C25 . C26 . 127.3(3) yes N5 . C25 . C26 . 112.6(3) yes C25 . C26 . N6 . 115.3(3) yes C25 . C26 . C27 . 123.3(4) yes N6 . C26 . C27 . 121.4(4) yes C26 . C27 . C28 . 119.2(4) yes C26 . C27 . H271 . 121.0 no C28 . C27 . H271 . 119.8 no C27 . C28 . C29 . 119.3(4) yes C27 . C28 . H281 . 119.8 no C29 . C28 . H281 . 120.9 no C28 . C29 . C30 . 119.3(4) yes C28 . C29 . H291 . 120.8 no C30 . C29 . H291 . 119.9 no C29 . C30 . N6 . 122.2(4) yes C29 . C30 . H301 . 119.4 no N6 . C30 . H301 . 118.4 no C8 . C31 . C32 . 128.1(4) yes C8 . C31 . S1 . 121.2(3) yes C32 . C31 . S1 . 110.7(3) yes C31 . C32 . C33 . 111.7(4) yes C31 . C32 . H321 . 123.8 no C33 . C32 . H321 . 124.5 no C32 . C33 . C34 . 114.8(4) yes C32 . C33 . Br1 . 122.1(3) yes C34 . C33 . Br1 . 123.1(3) yes C33 . C34 . S1 . 109.9(3) yes C33 . C34 . H341 . 125.2 no S1 . C34 . H341 . 124.9 no C23 . C35 . C36 . 128.3(4) yes C23 . C35 . S2 . 121.0(3) yes C36 . C35 . S2 . 110.7(3) yes C35 . C36 . C37 . 111.9(4) yes C35 . C36 . H361 . 124.0 no C37 . C36 . H361 . 124.0 no C36 . C37 . C38 . 114.6(4) yes C36 . C37 . Br2 . 122.4(3) yes C38 . C37 . Br2 . 123.0(3) yes C37 . C38 . S2 . 111.0(3) yes C37 . C38 . H381 . 125.3 no S2 . C38 . H381 . 123.7 no N7 . C41 . C42 . 122.5(4) yes N7 . C41 . H411 . 117.6 no C42 . C41 . H411 . 119.9 no C41 . C42 . C43 . 119.1(4) yes C41 . C42 . H421 . 120.4 no C43 . C42 . H421 . 120.6 no C42 . C43 . C44 . 119.9(4) yes C42 . C43 . H431 . 120.6 no C44 . C43 . H431 . 119.5 no C43 . C44 . C45 . 119.0(4) yes C43 . C44 . H441 . 120.5 no C45 . C44 . H441 . 120.5 no C44 . C45 . N7 . 120.7(3) yes C44 . C45 . C46 . 123.8(3) yes N7 . C45 . C46 . 115.4(3) yes C45 . C46 . N8 . 112.7(3) yes C45 . C46 . C47 . 127.6(3) yes N8 . C46 . C47 . 119.7(3) yes C46 . C47 . C48 . 119.7(3) yes C46 . C47 . H471 . 119.7 no C48 . C47 . H471 . 120.6 no C47 . C48 . C49 . 118.7(3) yes C47 . C48 . C71 . 122.7(3) yes C49 . C48 . C71 . 118.7(3) yes C48 . C49 . C50 . 120.1(4) yes C48 . C49 . H491 . 119.9 no C50 . C49 . H491 . 120.0 no C49 . C50 . N8 . 120.4(3) yes C49 . C50 . C51 . 127.0(4) yes N8 . C50 . C51 . 112.6(3) yes C50 . C51 . N9 . 114.7(3) yes C50 . C51 . C52 . 123.5(4) yes N9 . C51 . C52 . 121.7(4) yes C51 . C52 . C53 . 119.4(4) yes C51 . C52 . H521 . 121.0 no C53 . C52 . H521 . 119.6 no C52 . C53 . C54 . 118.8(4) yes C52 . C53 . H531 . 120.4 no C54 . C53 . H531 . 120.7 no C53 . C54 . C55 . 120.1(4) yes C53 . C54 . H541 . 119.7 no C55 . C54 . H541 . 120.1 no C54 . C55 . N9 . 121.4(4) yes C54 . C55 . H551 . 120.2 no N9 . C55 . H551 . 118.4 no N10 . C56 . C57 . 122.4(4) yes N10 . C56 . H561 . 118.0 no C57 . C56 . H561 . 119.6 no C56 . C57 . C58 . 118.8(4) yes C56 . C57 . H571 . 120.6 no C58 . C57 . H571 . 120.5 no C57 . C58 . C59 . 118.9(4) yes C57 . C58 . H581 . 120.4 no C59 . C58 . H581 . 120.7 no C58 . C59 . C60 . 119.7(4) yes C58 . C59 . H591 . 119.8 no C60 . C59 . H591 . 120.6 no C59 . C60 . N10 . 121.4(3) yes C59 . C60 . C61 . 123.2(4) yes N10 . C60 . C61 . 115.3(3) yes C60 . C61 . N11 . 112.2(3) yes C60 . C61 . C62 . 126.8(4) yes N11 . C61 . C62 . 121.1(3) yes C61 . C62 . C63 . 119.3(3) yes C61 . C62 . H621 . 120.8 no C63 . C62 . H621 . 119.9 no C62 . C63 . C64 . 118.4(3) yes C62 . C63 . C75 . 120.0(3) yes C64 . C63 . C75 . 121.5(3) yes C63 . C64 . C65 . 119.5(3) yes C63 . C64 . H641 . 119.9 no C65 . C64 . H641 . 120.6 no C64 . C65 . N11 . 120.9(3) yes C64 . C65 . C66 . 126.6(3) yes N11 . C65 . C66 . 112.4(3) yes C65 . C66 . N12 . 115.3(3) yes C65 . C66 . C67 . 123.7(4) yes N12 . C66 . C67 . 121.1(4) yes C66 . C67 . C68 . 119.1(4) yes C66 . C67 . H671 . 120.6 no C68 . C67 . H671 . 120.3 no C67 . C68 . C69 . 119.3(4) yes C67 . C68 . H681 . 120.0 no C69 . C68 . H681 . 120.6 no C68 . C69 . C70 . 119.6(4) yes C68 . C69 . H691 . 120.7 no C70 . C69 . H691 . 119.8 no C69 . C70 . N12 . 121.7(4) yes C69 . C70 . H701 . 119.8 no N12 . C70 . H701 . 118.5 no C48 . C71 . C72 . 129.0(4) yes C48 . C71 . S3 . 120.6(3) yes C72 . C71 . S3 . 110.3(3) yes C71 . C72 . C73 . 112.3(4) yes C71 . C72 . H721 . 124.1 no C73 . C72 . H721 . 123.6 no C72 . C73 . C74 . 115.1(4) yes C72 . C73 . Br3 . 122.2(3) yes C74 . C73 . Br3 . 122.7(3) yes C73 . C74 . S3 . 109.7(3) yes C73 . C74 . H741 . 125.3 no S3 . C74 . H741 . 125.1 no C63 . C75 . C76 . 128.3(4) yes C63 . C75 . S4 . 120.6(3) yes C76 . C75 . S4 . 111.1(3) yes C75 . C76 . C77 . 111.5(4) yes C75 . C76 . H761 . 124.4 no C77 . C76 . H761 . 124.1 no C76 . C77 . C78 . 115.0(4) yes C76 . C77 . Br4 . 122.6(3) yes C78 . C77 . Br4 . 122.4(3) yes C77 . C78 . S4 . 110.2(3) yes C77 . C78 . H781 . 125.7 no S4 . C78 . H781 . 124.1 no C31 . S1 . C34 . 92.8(2) yes C35 . S2 . C38 . 91.8(2) yes C71 . S3 . C74 . 92.6(2) yes C75 . S4 . C78 . 92.2(2) yes F1 . P1 . F2 . 179.4(2) yes F1 . P1 . F3 . 90.08(19) yes F2 . P1 . F3 . 89.41(18) yes F1 . P1 . F4 . 89.85(18) yes F2 . P1 . F4 . 90.66(17) yes F3 . P1 . F4 . 179.88(19) yes F1 . P1 . F5 . 89.86(17) yes F2 . P1 . F5 . 89.74(16) yes F3 . P1 . F5 . 90.0(2) yes F4 . P1 . F5 . 89.91(17) yes F1 . P1 . F6 . 89.88(17) yes F2 . P1 . F6 . 90.52(17) yes F3 . P1 . F6 . 89.7(2) yes F4 . P1 . F6 . 90.4(2) yes F5 . P1 . F6 . 179.6(2) yes F11 . P2 . F12 . 179.68(17) yes F11 . P2 . F13 . 90.47(19) yes F12 . P2 . F13 . 89.30(17) yes F11 . P2 . F14 . 90.55(19) yes F12 . P2 . F14 . 89.68(18) yes F13 . P2 . F14 . 178.97(18) yes F11 . P2 . F15 . 91.07(17) yes F12 . P2 . F15 . 89.14(16) yes F13 . P2 . F15 . 89.78(16) yes F14 . P2 . F15 . 90.06(16) yes F11 . P2 . F16 . 90.03(17) yes F12 . P2 . F16 . 89.76(16) yes F13 . P2 . F16 . 89.83(16) yes F14 . P2 . F16 . 90.31(16) yes F15 . P2 . F16 . 178.84(18) yes F21 . P3 . F22 . 179.3(2) yes F21 . P3 . F23 . 90.1(2) yes F22 . P3 . F23 . 89.24(18) yes F21 . P3 . F24 . 90.5(2) yes F22 . P3 . F24 . 90.2(2) yes F23 . P3 . F24 . 179.35(19) yes F21 . P3 . F25 . 89.77(17) yes F22 . P3 . F25 . 90.47(17) yes F23 . P3 . F25 . 89.32(16) yes F24 . P3 . F25 . 90.97(18) yes F21 . P3 . F26 . 90.30(17) yes F22 . P3 . F26 . 89.45(16) yes F23 . P3 . F26 . 90.09(17) yes F24 . P3 . F26 . 89.61(18) yes F25 . P3 . F26 . 179.42(18) yes F31 . P4 . F32 . 175.1(3) yes F31 . P4 . F33 . 88.8(2) yes F32 . P4 . F33 . 91.5(2) yes F31 . P4 . F34 . 90.1(2) yes F32 . P4 . F34 . 89.5(2) yes F33 . P4 . F34 . 178.6(3) yes F31 . P4 . F35 . 86.2(2) yes F32 . P4 . F35 . 88.9(3) yes F33 . P4 . F35 . 90.1(3) yes F34 . P4 . F35 . 88.9(3) yes F31 . P4 . F36 . 91.7(3) yes F32 . P4 . F36 . 93.2(3) yes F33 . P4 . F36 . 90.6(3) yes F34 . P4 . F36 . 90.4(3) yes F35 . P4 . F36 . 177.7(3) yes N13 . C81 . C82 . 179.4(8) yes C81 . C82 . H821 . 109.4 no C81 . C82 . H822 . 107.4 no H821 . C82 . H822 . 110.6 no C81 . C82 . H823 . 108.6 no H821 . C82 . H823 . 110.7 no H822 . C82 . H823 . 110.1 no N14 . C83 . C84 . 179.0(11) yes C83 . C84 . H841 . 111.9 no C83 . C84 . H842 . 105.3 no H841 . C84 . H842 . 110.1 no C83 . C84 . H843 . 109.9 no H841 . C84 . H843 . 109.8 no H842 . C84 . H843 . 109.7 no N15 . C85 . C86 . 179.4(8) yes C85 . C86 . H861 . 109.0 no C85 . C86 . H862 . 110.0 no H861 . C86 . H862 . 108.7 no C85 . C86 . H863 . 110.9 no H861 . C86 . H863 . 109.0 no H862 . C86 . H863 . 109.2 no N16 . C87 . C88 . 174.3(10) yes C87 . C88 . H881 . 109.1 no C87 . C88 . H882 . 110.1 no H881 . C88 . H882 . 108.4 no C87 . C88 . H883 . 111.2 no H881 . C88 . H883 . 108.9 no H882 . C88 . H883 . 109.1 no N17 . C89 . C90 . 172.5(12) yes C89 . C90 . H901 . 109.5 no C89 . C90 . H902 . 106.2 no H901 . C90 . H902 . 111.7 no C89 . C90 . H903 . 106.9 no H901 . C90 . H903 . 111.0 no H902 . C90 . H903 . 111.3 no # Attachment '[Ru_3_2][PF6]2.cif' data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 694388' _audit_creation_date 07-08-03 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '8031319 em97_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.2501(2) _cell_length_b 15.8647(3) _cell_length_c 18.8399(3) _cell_angle_alpha 86.6850(12) _cell_angle_beta 86.9732(12) _cell_angle_gamma 77.8687(10) _cell_volume 3279.10(10) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C50 H42 F12 N6 P2 Ru1 S2 Si2 # Dc = 1.25 Fooo = 1420.00 Mu = 4.56 M = 1238.22 # Found Formula = C60 H66 F12 N6 P2 Ru1 S2 Si2 # Dc = 1.40 FOOO = 1420.00 Mu = 4.64 M = 1382.52 _chemical_formula_sum 'C60 H66 F12 N6 P2 Ru1 S2 Si2' _chemical_formula_moiety 'C60 H66 N6 Ru S2 Si2, 2(F6 P)' _chemical_compound_source ? _chemical_formula_weight 1382.52 _cell_measurement_reflns_used 14875 _cell_measurement_theta_min 1 _cell_measurement_theta_max 32 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.21 _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 0.464 # Sheldrick geometric approximatio 0.92 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.98 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 29010 _reflns_number_total 15425 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections with Friedels Law is 15425 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 18978 _diffrn_reflns_theta_min 1.853 _diffrn_reflns_theta_max 30.156 _diffrn_measured_fraction_theta_max 0.795 _diffrn_reflns_theta_full 27.141 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -14 _reflns_limit_h_max 15 _reflns_limit_k_min -20 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.83 _refine_diff_density_max 1.28 _refine_ls_number_reflns 9861 _refine_ls_number_restraints 1192 _refine_ls_number_parameters 802 #_refine_ls_R_factor_ref 0.0447 _refine_ls_wR_factor_ref 0.0494 _refine_ls_goodness_of_fit_ref 1.1118 #_reflns_number_all 15341 _refine_ls_R_factor_all 0.0771 _refine_ls_wR_factor_all 0.0580 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 9861 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_gt 0.0494 _refine_ls_shift/su_max 0.038687 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.78 1.62 1.40 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ru1 Ru 0.187575(19) 0.519960(14) 0.269389(11) 0.0270 1.0000 Uani . . . . . . N1 N 0.12322(19) 0.55243(14) 0.37147(11) 0.0259 1.0000 Uani . . . . . . N2 N 0.33125(19) 0.46777(14) 0.32451(11) 0.0262 1.0000 Uani . . . . . . N3 N 0.3098(2) 0.47110(15) 0.18939(12) 0.0321 1.0000 Uani . . . . . . N4 N 0.1057(2) 0.41464(15) 0.27330(12) 0.0313 1.0000 Uani . . . . . . N5 N 0.04366(19) 0.56597(14) 0.21211(11) 0.0271 1.0000 Uani . . . . . . N6 N 0.2147(2) 0.64224(15) 0.24068(12) 0.0314 1.0000 Uani . . . . . . C1 C 0.0146(2) 0.59975(17) 0.39240(15) 0.0306 1.0000 Uani . . . . . . C2 C -0.0165(2) 0.61802(18) 0.46242(15) 0.0328 1.0000 Uani . . . . . . C3 C 0.0668(2) 0.58728(17) 0.51423(15) 0.0315 1.0000 Uani . . . . . . C4 C 0.1793(2) 0.53822(17) 0.49375(14) 0.0290 1.0000 Uani . . . . . . C5 C 0.2062(2) 0.52147(16) 0.42321(14) 0.0268 1.0000 Uani . . . . . . C6 C 0.3237(2) 0.46975(16) 0.39639(13) 0.0259 1.0000 Uani . . . . . . C7 C 0.4169(2) 0.42505(16) 0.43685(14) 0.0271 1.0000 Uani . . . . . . C8 C 0.5217(2) 0.37731(16) 0.40286(14) 0.0276 1.0000 Uani . . . . . . C9 C 0.5287(2) 0.37772(17) 0.32846(14) 0.0290 1.0000 Uani . . . . . . C10 C 0.4320(2) 0.42411(17) 0.29026(14) 0.0280 1.0000 Uani . . . . . . C11 C 0.4226(2) 0.43029(18) 0.21148(14) 0.0308 1.0000 Uani . . . . . . C12 C 0.5165(3) 0.3991(2) 0.16429(15) 0.0379 1.0000 Uani . . . . . . C13 C 0.4968(3) 0.4084(2) 0.09156(17) 0.0476 1.0000 Uani . . . . . . C14 C 0.3833(3) 0.4495(3) 0.06964(16) 0.0479 1.0000 Uani . . . . . . C15 C 0.2932(3) 0.4805(2) 0.11839(15) 0.0397 1.0000 Uani . . . . . . C16 C 0.1445(3) 0.3367(2) 0.30610(16) 0.0400 1.0000 Uani . . . . . . C17 C 0.0837(3) 0.2698(2) 0.30323(19) 0.0462 1.0000 Uani . . . . . . C18 C -0.0203(3) 0.2826(2) 0.26543(18) 0.0454 1.0000 Uani . . . . . . C19 C -0.0629(3) 0.3623(2) 0.23184(16) 0.0400 1.0000 Uani . . . . . . C20 C 0.0010(2) 0.42777(19) 0.23605(14) 0.0314 1.0000 Uani . . . . . . C21 C -0.0347(2) 0.51427(18) 0.20098(14) 0.0307 1.0000 Uani . . . . . . C22 C -0.1342(2) 0.5442(2) 0.15939(15) 0.0344 1.0000 Uani . . . . . . C23 C -0.1542(2) 0.6285(2) 0.13011(15) 0.0345 1.0000 Uani . . . . . . C24 C -0.0705(3) 0.67963(19) 0.14123(15) 0.0341 1.0000 Uani . . . . . . C25 C 0.0291(2) 0.64639(18) 0.18190(14) 0.0307 1.0000 Uani . . . . . . C26 C 0.1288(2) 0.68987(18) 0.19656(14) 0.0316 1.0000 Uani . . . . . . C27 C 0.1392(3) 0.7698(2) 0.16794(17) 0.0409 1.0000 Uani . . . . . . C28 C 0.2370(3) 0.8040(2) 0.1847(2) 0.0517 1.0000 Uani . . . . . . C29 C 0.3222(3) 0.7572(2) 0.2294(2) 0.0511 1.0000 Uani . . . . . . C30 C 0.3098(3) 0.6773(2) 0.25558(17) 0.0397 1.0000 Uani . . . . . . C31 C 0.6201(2) 0.32788(17) 0.44567(14) 0.0286 1.0000 Uani . . . . . . C32 C 0.6186(2) 0.31069(19) 0.51812(15) 0.0329 1.0000 Uani . . . . . . C33 C 0.7285(3) 0.26044(19) 0.54231(16) 0.0363 1.0000 Uani . . . . . . C34 C 0.8146(2) 0.23939(17) 0.48869(15) 0.0305 1.0000 Uani . . . . . . C35 C 0.9368(3) 0.19110(18) 0.49565(15) 0.0337 1.0000 Uani . . . . . . C36 C 1.0359(3) 0.1515(2) 0.50829(17) 0.0372 1.0000 Uani . . . . . . C37 C 1.2813(3) 0.1728(2) 0.54690(19) 0.0436 1.0000 Uani . . . . . . C38 C 1.3104(4) 0.2076(3) 0.4722(2) 0.0618 1.0000 Uani . . . . . . C39 C 1.3974(4) 0.1389(3) 0.5885(3) 0.0645 1.0000 Uani . . . . . . C40 C 1.2361(3) -0.0098(2) 0.5059(2) 0.0482 1.0000 Uani . . . . . . C41 C 1.2745(4) 0.0006(3) 0.4273(3) 0.0671 1.0000 Uani . . . . . . C42 C 1.3366(3) -0.0690(2) 0.5496(3) 0.0606 1.0000 Uani . . . . . . C43 C 1.1252(4) 0.0742(3) 0.6451(2) 0.0568 1.0000 Uani . . . . . . C44 C 1.0362(5) 0.0122(4) 0.6495(3) 0.0932 1.0000 Uani . . . . . . C45 C 1.0752(5) 0.1589(3) 0.6825(2) 0.0787 1.0000 Uani . . . . . . C46 C -0.2648(3) 0.6633(2) 0.09059(15) 0.0368 1.0000 Uani . . . . . . C47 C -0.3791(3) 0.6474(2) 0.10451(16) 0.0406 1.0000 Uani . . . . . . C48 C -0.4667(3) 0.6975(2) 0.06067(17) 0.0442 1.0000 Uani . . . . . . C49 C -0.4196(3) 0.7512(2) 0.01334(16) 0.0432 1.0000 Uani . . . . . . C50 C -0.4817(3) 0.8127(2) -0.0391(2) 0.0491 1.0000 Uani . . . . . . C51 C -0.5360(4) 0.8640(3) -0.0793(2) 0.0544 1.0000 Uani . . . . . . C52 C -0.5825(4) 1.0530(3) -0.1246(2) 0.0638 1.0000 Uani . . . . . . C53 C -0.4457(5) 1.0429(4) -0.1144(3) 0.0879 1.0000 Uani . . . . . . C54 C -0.6231(6) 1.1201(3) -0.1856(3) 0.0834 1.0000 Uani . . . . . . C55 C -0.6157(5) 0.9127(3) -0.2287(2) 0.0688 1.0000 Uani . . . . . . C56 C -0.4853(7) 0.8899(6) -0.2553(3) 0.1285 1.0000 Uani . . . . . . C57 C -0.6789(8) 0.8382(4) -0.2363(3) 0.1108 1.0000 Uani . . . . . . C58 C -0.7938(4) 0.9563(3) -0.0958(3) 0.0668 1.0000 Uani . . . . . . C59 C -0.8041(5) 0.9660(5) -0.0169(3) 0.1004 1.0000 Uani . . . . . . C60 C -0.8859(5) 1.0261(5) -0.1352(4) 0.1097 1.0000 Uani . . . . . . S1 S 0.75960(6) 0.28186(5) 0.40733(4) 0.0322 1.0000 Uani . . . . . . S2 S -0.26421(7) 0.73937(6) 0.02166(4) 0.0455 1.0000 Uani . . . . . . Si1 Si 1.17809(7) 0.09481(5) 0.54940(5) 0.0347 1.0000 Uani . . . . . . Si2 Si -0.63279(9) 0.94859(6) -0.13399(6) 0.0498 1.0000 Uani . . . . . . P1 P 0.33268(6) 0.39871(5) 0.66656(4) 0.0329 1.0000 Uani . . . . . . P2 P 0.86062(9) 0.31119(8) 0.03899(5) 0.0605 1.0000 Uani D U . . . . F1 F 0.2230(2) 0.48043(14) 0.65928(11) 0.0559 1.0000 Uani . . . . . . F2 F 0.44271(17) 0.31711(14) 0.67271(12) 0.0527 1.0000 Uani . . . . . . F3 F 0.29339(17) 0.36246(12) 0.59545(9) 0.0419 1.0000 Uani . . . . . . F4 F 0.3729(2) 0.43659(15) 0.73605(10) 0.0550 1.0000 Uani . . . . . . F5 F 0.24658(19) 0.34727(14) 0.71285(11) 0.0536 1.0000 Uani . . . . . . F6 F 0.4183(2) 0.44980(14) 0.61757(11) 0.0545 1.0000 Uani . . . . . . F11 F 0.7479(4) 0.3066(5) -0.0041(4) 0.1092 0.5000 Uani D U . . . . F12 F 0.9742(5) 0.3305(4) 0.0778(3) 0.0698 0.5000 Uani D U . . . . F13 F 0.8324(7) 0.2520(4) 0.1015(3) 0.1144 0.5000 Uani D U . . . . F14 F 0.8947(6) 0.3799(4) -0.0236(3) 0.0923 0.5000 Uani D U . . . . F15 F 0.7785(2) 0.3893(2) 0.08085(15) 0.0892 1.0000 Uani D U . . . . F16 F 0.9426(3) 0.23444(19) -0.00252(15) 0.0917 1.0000 Uani D U . . . . F21 F 0.7459(4) 0.2643(4) 0.0362(4) 0.0830 0.5000 Uani D U . . . . F22 F 0.9748(5) 0.3483(4) 0.0490(4) 0.0855 0.5000 Uani D U . . . . F23 F 0.8925(5) 0.2514(3) 0.1111(2) 0.0745 0.5000 Uani D U . . . . F24 F 0.8248(7) 0.3601(4) -0.0318(3) 0.1027 0.5000 Uani D U . . . . H11 H -0.0417 0.6207 0.3570 0.0361 1.0000 Uiso R . . . . . H21 H -0.0941 0.6509 0.4743 0.0391 1.0000 Uiso R . . . . . H31 H 0.0480 0.5996 0.5624 0.0389 1.0000 Uiso R . . . . . H41 H 0.2375 0.5171 0.5277 0.0353 1.0000 Uiso R . . . . . H71 H 0.4106 0.4264 0.4869 0.0321 1.0000 Uiso R . . . . . H91 H 0.5984 0.3473 0.3047 0.0349 1.0000 Uiso R . . . . . H121 H 0.5932 0.3717 0.1807 0.0444 1.0000 Uiso R . . . . . H131 H 0.5599 0.3873 0.0589 0.0544 1.0000 Uiso R . . . . . H141 H 0.3679 0.4564 0.0212 0.0564 1.0000 Uiso R . . . . . H151 H 0.2155 0.5087 0.1036 0.0472 1.0000 Uiso R . . . . . H161 H 0.2156 0.3285 0.3316 0.0482 1.0000 Uiso R . . . . . H171 H 0.1133 0.2165 0.3268 0.0572 1.0000 Uiso R . . . . . H181 H -0.0623 0.2380 0.2619 0.0563 1.0000 Uiso R . . . . . H191 H -0.1346 0.3721 0.2061 0.0481 1.0000 Uiso R . . . . . H221 H -0.1870 0.5074 0.1513 0.0412 1.0000 Uiso R . . . . . H241 H -0.0814 0.7359 0.1210 0.0404 1.0000 Uiso R . . . . . H271 H 0.0807 0.8008 0.1372 0.0500 1.0000 Uiso R . . . . . H281 H 0.2443 0.8588 0.1656 0.0632 1.0000 Uiso R . . . . . H291 H 0.3896 0.7791 0.2416 0.0612 1.0000 Uiso R . . . . . H301 H 0.3687 0.6444 0.2855 0.0484 1.0000 Uiso R . . . . . H321 H 0.5497 0.3306 0.5482 0.0391 1.0000 Uiso R . . . . . H331 H 0.7428 0.2429 0.5899 0.0433 1.0000 Uiso R . . . . . H371 H 1.2336 0.2227 0.5734 0.0543 1.0000 Uiso R . . . . . H381 H 1.2353 0.2308 0.4485 0.0999 1.0000 Uiso R . . . . . H382 H 1.3561 0.2526 0.4760 0.1002 1.0000 Uiso R . . . . . H383 H 1.3572 0.1605 0.4456 0.1001 1.0000 Uiso R . . . . . H391 H 1.3725 0.1215 0.6370 0.1047 1.0000 Uiso R . . . . . H392 H 1.4429 0.1845 0.5897 0.1051 1.0000 Uiso R . . . . . H393 H 1.4464 0.0898 0.5651 0.1049 1.0000 Uiso R . . . . . H401 H 1.1664 -0.0396 0.5078 0.0602 1.0000 Uiso R . . . . . H411 H 1.2101 0.0399 0.4018 0.1048 1.0000 Uiso R . . . . . H412 H 1.3459 0.0267 0.4243 0.1050 1.0000 Uiso R . . . . . H413 H 1.2933 -0.0549 0.4051 0.1052 1.0000 Uiso R . . . . . H421 H 1.3059 -0.0761 0.5984 0.0921 1.0000 Uiso R . . . . . H422 H 1.4070 -0.0424 0.5487 0.0922 1.0000 Uiso R . . . . . H423 H 1.3590 -0.1248 0.5282 0.0919 1.0000 Uiso R . . . . . H431 H 1.1991 0.0441 0.6696 0.0702 1.0000 Uiso R . . . . . H441 H 1.0794 -0.0408 0.6279 0.1468 1.0000 Uiso R . . . . . H442 H 1.0148 0.0014 0.6987 0.1469 1.0000 Uiso R . . . . . H443 H 0.9642 0.0386 0.6238 0.1470 1.0000 Uiso R . . . . . H451 H 1.1417 0.1900 0.6822 0.1111 1.0000 Uiso R . . . . . H452 H 1.0487 0.1457 0.7309 0.1109 1.0000 Uiso R . . . . . H453 H 1.0070 0.1919 0.6567 0.1110 1.0000 Uiso R . . . . . H471 H -0.3959 0.6072 0.1395 0.0482 1.0000 Uiso R . . . . . H481 H -0.5496 0.6953 0.0635 0.0522 1.0000 Uiso R . . . . . H521 H -0.6252 1.0760 -0.0795 0.0803 1.0000 Uiso R . . . . . H531 H -0.4225 1.0032 -0.0735 0.1501 1.0000 Uiso R . . . . . H532 H -0.4261 1.0988 -0.1073 0.1500 1.0000 Uiso R . . . . . H533 H -0.4032 1.0188 -0.1580 0.1500 1.0000 Uiso R . . . . . H541 H -0.7098 1.1257 -0.1905 0.1340 1.0000 Uiso R . . . . . H542 H -0.6055 1.1754 -0.1748 0.1341 1.0000 Uiso R . . . . . H543 H -0.5790 1.0991 -0.2289 0.1341 1.0000 Uiso R . . . . . H551 H -0.6577 0.9620 -0.2589 0.0833 1.0000 Uiso R . . . . . H561 H -0.4524 0.9417 -0.2593 0.1843 1.0000 Uiso R . . . . . H562 H -0.4817 0.8642 -0.3008 0.1840 1.0000 Uiso R . . . . . H563 H -0.4414 0.8481 -0.2220 0.1842 1.0000 Uiso R . . . . . H571 H -0.7649 0.8588 -0.2253 0.1724 1.0000 Uiso R . . . . . H572 H -0.6656 0.8191 -0.2843 0.1720 1.0000 Uiso R . . . . . H573 H -0.6460 0.7918 -0.2029 0.1720 1.0000 Uiso R . . . . . H581 H -0.8156 0.9003 -0.1042 0.0824 1.0000 Uiso R . . . . . H591 H -0.7449 0.9205 0.0069 0.1562 1.0000 Uiso R . . . . . H592 H -0.7865 1.0220 -0.0088 0.1562 1.0000 Uiso R . . . . . H593 H -0.8864 0.9630 0.0002 0.1561 1.0000 Uiso R . . . . . H601 H -0.8786 1.0161 -0.1860 0.1582 1.0000 Uiso R . . . . . H602 H -0.8672 1.0818 -0.1265 0.1582 1.0000 Uiso R . . . . . H603 H -0.9675 1.0232 -0.1163 0.1580 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02182(10) 0.03159(12) 0.02533(11) 0.00039(7) -0.00710(7) 0.00089(7) N1 0.0219(9) 0.0266(10) 0.0284(10) 0.0009(8) -0.0064(8) -0.0029(8) N2 0.0230(10) 0.0295(11) 0.0246(10) 0.0018(8) -0.0052(8) -0.0019(8) N3 0.0274(11) 0.0360(12) 0.0302(11) 0.0009(9) -0.0073(9) 0.0007(9) N4 0.0316(11) 0.0329(12) 0.0280(10) 0.0002(9) -0.0067(9) -0.0025(9) N5 0.0244(10) 0.0312(11) 0.0235(10) 0.0009(8) -0.0055(8) -0.0002(8) N6 0.0278(10) 0.0351(12) 0.0304(11) 0.0019(9) -0.0056(9) -0.0039(9) C1 0.0237(11) 0.0307(13) 0.0358(13) 0.0023(10) -0.0079(10) -0.0016(10) C2 0.0242(12) 0.0310(13) 0.0413(14) -0.0019(11) -0.0025(10) -0.0007(10) C3 0.0309(13) 0.0318(13) 0.0312(12) -0.0053(10) -0.0005(10) -0.0044(10) C4 0.0254(11) 0.0308(13) 0.0301(12) 0.0017(10) -0.0053(9) -0.0042(10) C5 0.0214(11) 0.0241(11) 0.0345(12) 0.0015(10) -0.0080(9) -0.0030(9) C6 0.0227(11) 0.0273(12) 0.0273(11) 0.0003(9) -0.0048(9) -0.0035(9) C7 0.0245(11) 0.0278(12) 0.0290(12) 0.0017(10) -0.0060(9) -0.0048(9) C8 0.0233(11) 0.0278(12) 0.0307(12) 0.0019(10) -0.0074(9) -0.0023(9) C9 0.0209(11) 0.0303(13) 0.0331(12) 0.0010(10) -0.0055(9) 0.0015(9) C10 0.0237(11) 0.0285(12) 0.0312(12) -0.0002(10) -0.0053(9) -0.0032(9) C11 0.0289(12) 0.0315(13) 0.0299(12) -0.0006(10) -0.0080(10) -0.0005(10) C12 0.0330(14) 0.0450(16) 0.0311(13) -0.0011(12) -0.0031(11) 0.0027(12) C13 0.0391(16) 0.064(2) 0.0323(14) -0.0025(14) 0.0011(12) 0.0047(15) C14 0.0440(16) 0.067(2) 0.0267(13) -0.0019(13) -0.0070(12) 0.0039(15) C15 0.0362(14) 0.0496(17) 0.0285(13) 0.0000(12) -0.0092(11) 0.0033(12) C16 0.0405(15) 0.0390(15) 0.0373(14) 0.0050(12) -0.0101(12) -0.0007(12) C17 0.0531(18) 0.0347(15) 0.0489(17) 0.0050(13) -0.0106(14) -0.0041(13) C18 0.0515(18) 0.0444(17) 0.0441(16) -0.0034(13) -0.0038(14) -0.0178(14) C19 0.0407(15) 0.0427(16) 0.0383(15) -0.0002(12) -0.0089(12) -0.0109(12) C20 0.0270(12) 0.0384(14) 0.0274(12) -0.0017(10) -0.0049(9) -0.0031(10) C21 0.0263(12) 0.0387(14) 0.0265(11) -0.0025(10) -0.0038(9) -0.0044(10) C22 0.0289(13) 0.0421(15) 0.0318(13) -0.0020(11) -0.0087(10) -0.0045(11) C23 0.0263(12) 0.0440(15) 0.0295(12) 0.0009(11) -0.0086(10) 0.0025(11) C24 0.0300(13) 0.0357(14) 0.0333(13) 0.0020(11) -0.0089(10) 0.0017(11) C25 0.0260(12) 0.0374(14) 0.0273(12) -0.0029(10) -0.0050(10) -0.0021(10) C26 0.0272(12) 0.0338(13) 0.0318(12) 0.0010(10) -0.0047(10) -0.0016(10) C27 0.0383(15) 0.0398(15) 0.0426(15) 0.0094(12) -0.0097(12) -0.0046(12) C28 0.0513(18) 0.0414(17) 0.064(2) 0.0122(15) -0.0107(16) -0.0143(14) C29 0.0437(17) 0.0510(19) 0.063(2) 0.0094(16) -0.0144(15) -0.0199(15) C30 0.0283(13) 0.0477(17) 0.0425(15) 0.0024(13) -0.0113(11) -0.0055(12) C31 0.0197(11) 0.0297(12) 0.0348(13) 0.0013(10) -0.0042(9) -0.0014(9) C32 0.0269(12) 0.0362(14) 0.0317(13) 0.0042(11) -0.0037(10) 0.0015(10) C33 0.0302(13) 0.0390(15) 0.0362(14) 0.0065(11) -0.0111(11) 0.0007(11) C34 0.0250(12) 0.0282(12) 0.0370(13) 0.0008(10) -0.0104(10) -0.0007(10) C35 0.0328(13) 0.0318(13) 0.0375(14) 0.0009(11) -0.0117(11) -0.0069(11) C36 0.0301(13) 0.0377(15) 0.0425(15) 0.0010(12) -0.0087(11) -0.0033(11) C37 0.0383(15) 0.0380(15) 0.0532(18) -0.0029(13) -0.0095(13) -0.0032(12) C38 0.064(2) 0.055(2) 0.069(2) 0.0065(18) -0.0055(19) -0.0210(18) C39 0.0455(18) 0.050(2) 0.100(3) 0.000(2) -0.032(2) -0.0067(16) C40 0.0351(15) 0.0378(16) 0.070(2) -0.0048(15) -0.0111(15) -0.0010(12) C41 0.062(2) 0.064(2) 0.073(3) -0.021(2) -0.005(2) -0.0013(19) C42 0.0442(18) 0.0333(16) 0.102(3) -0.0031(18) -0.0242(19) 0.0023(14) C43 0.0482(19) 0.066(2) 0.0518(19) 0.0112(17) -0.0120(15) -0.0020(17) C44 0.082(3) 0.132(4) 0.076(3) 0.031(3) -0.004(3) -0.056(3) C45 0.086(3) 0.088(3) 0.048(2) -0.004(2) 0.000(2) 0.015(3) C46 0.0315(13) 0.0456(16) 0.0300(13) 0.0033(11) -0.0099(10) -0.0001(12) C47 0.0320(13) 0.0527(17) 0.0333(14) 0.0033(12) -0.0085(11) -0.0002(12) C48 0.0289(13) 0.061(2) 0.0405(15) -0.0008(14) -0.0134(12) -0.0023(13) C49 0.0384(15) 0.0514(17) 0.0347(14) -0.0018(13) -0.0143(12) 0.0052(13) C50 0.0394(16) 0.0539(19) 0.0522(19) -0.0050(15) -0.0159(14) -0.0013(14) C51 0.0514(19) 0.057(2) 0.0530(19) 0.0052(16) -0.0218(16) -0.0053(16) C52 0.072(2) 0.063(2) 0.061(2) -0.0020(19) -0.0102(19) -0.022(2) C53 0.073(3) 0.102(4) 0.100(4) -0.011(3) -0.014(3) -0.039(3) C54 0.121(4) 0.055(2) 0.077(3) 0.002(2) -0.015(3) -0.024(3) C55 0.096(3) 0.052(2) 0.054(2) 0.0015(17) -0.035(2) 0.000(2) C56 0.115(4) 0.191(6) 0.063(3) -0.028(4) -0.004(3) 0.012(5) C57 0.202(5) 0.069(3) 0.074(3) -0.005(2) -0.049(4) -0.047(4) C58 0.057(2) 0.068(3) 0.073(3) 0.011(2) -0.022(2) -0.0064(19) C59 0.062(3) 0.150(5) 0.080(3) 0.000(3) 0.003(3) -0.003(3) C60 0.059(3) 0.127(5) 0.127(5) 0.046(4) -0.023(3) 0.010(3) S1 0.0219(3) 0.0393(3) 0.0319(3) -0.0006(3) -0.0060(2) 0.0026(2) S2 0.0351(4) 0.0557(5) 0.0434(4) 0.0122(3) -0.0165(3) -0.0047(3) Si1 0.0250(3) 0.0317(4) 0.0450(4) 0.0027(3) -0.0120(3) 0.0010(3) Si2 0.0507(5) 0.0463(5) 0.0511(5) 0.0038(4) -0.0232(4) -0.0036(4) P1 0.0314(3) 0.0398(4) 0.0278(3) 0.0000(3) -0.0040(3) -0.0077(3) P2 0.0437(5) 0.0934(8) 0.0422(5) -0.0119(5) -0.0015(4) -0.0069(5) F1 0.0599(12) 0.0517(11) 0.0469(11) -0.0041(9) -0.0057(9) 0.0107(9) F2 0.0384(10) 0.0558(11) 0.0592(12) 0.0006(9) -0.0176(9) 0.0041(8) F3 0.0449(10) 0.0443(9) 0.0376(9) -0.0051(7) -0.0104(7) -0.0091(8) F4 0.0672(13) 0.0705(13) 0.0333(9) -0.0084(9) -0.0115(9) -0.0241(11) F5 0.0506(11) 0.0635(13) 0.0496(11) 0.0046(9) 0.0076(9) -0.0225(10) F6 0.0679(13) 0.0587(12) 0.0451(10) -0.0092(9) 0.0121(9) -0.0337(10) F11 0.052(3) 0.179(5) 0.099(4) -0.085(4) -0.014(3) -0.008(4) F12 0.051(2) 0.104(4) 0.051(3) 0.000(3) -0.014(2) -0.008(3) F13 0.141(4) 0.130(5) 0.090(4) -0.002(3) 0.034(4) -0.080(4) F14 0.089(3) 0.116(4) 0.050(3) 0.014(3) 0.004(3) 0.021(3) F15 0.0496(13) 0.131(2) 0.0896(18) -0.0614(18) 0.0006(13) -0.0105(14) F16 0.0878(19) 0.097(2) 0.0744(17) -0.0111(15) 0.0036(15) 0.0178(16) F21 0.063(3) 0.092(4) 0.099(4) -0.021(3) -0.015(3) -0.020(3) F22 0.051(3) 0.075(3) 0.129(5) 0.026(4) 0.003(3) -0.021(2) F23 0.093(3) 0.089(3) 0.047(2) -0.006(2) -0.023(3) -0.026(3) F24 0.136(4) 0.093(4) 0.053(3) 0.008(3) -0.017(4) 0.035(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2252(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . N1 . 2.073(2) yes Ru1 . N2 . 1.973(2) yes Ru1 . N3 . 2.057(2) yes Ru1 . N4 . 2.067(2) yes Ru1 . N5 . 1.979(2) yes Ru1 . N6 . 2.064(2) yes N1 . C1 . 1.346(3) yes N1 . C5 . 1.382(3) yes N2 . C6 . 1.354(3) yes N2 . C10 . 1.351(3) yes N3 . C11 . 1.372(3) yes N3 . C15 . 1.356(4) yes N4 . C16 . 1.347(4) yes N4 . C20 . 1.375(3) yes N5 . C21 . 1.356(4) yes N5 . C25 . 1.348(4) yes N6 . C26 . 1.379(3) yes N6 . C30 . 1.354(4) yes C1 . C2 . 1.378(4) yes C1 . H11 . 0.942 no C2 . C3 . 1.385(4) yes C2 . H21 . 0.941 no C3 . C4 . 1.388(4) yes C3 . H31 . 0.943 no C4 . C5 . 1.376(4) yes C4 . H41 . 0.936 no C5 . C6 . 1.482(3) yes C6 . C7 . 1.376(3) yes C7 . C8 . 1.405(4) yes C7 . H71 . 0.944 no C8 . C9 . 1.400(4) yes C8 . C31 . 1.465(3) yes C9 . C10 . 1.389(3) yes C9 . H91 . 0.936 no C10 . C11 . 1.490(4) yes C11 . C12 . 1.372(4) yes C12 . C13 . 1.394(4) yes C12 . H121 . 0.941 no C13 . C14 . 1.378(5) yes C13 . H131 . 0.935 no C14 . C15 . 1.363(5) yes C14 . H141 . 0.934 no C15 . H151 . 0.943 no C16 . C17 . 1.384(5) yes C16 . H161 . 0.937 no C17 . C18 . 1.375(5) yes C17 . H171 . 0.936 no C18 . C19 . 1.382(5) yes C18 . H181 . 0.937 no C19 . C20 . 1.390(4) yes C19 . H191 . 0.944 no C20 . C21 . 1.474(4) yes C21 . C22 . 1.385(4) yes C22 . C23 . 1.396(4) yes C22 . H221 . 0.939 no C23 . C24 . 1.396(4) yes C23 . C46 . 1.473(3) yes C24 . C25 . 1.384(3) yes C24 . H241 . 0.936 no C25 . C26 . 1.480(4) yes C26 . C27 . 1.374(4) yes C27 . C28 . 1.382(5) yes C27 . H271 . 0.940 no C28 . C29 . 1.376(5) yes C28 . H281 . 0.941 no C29 . C30 . 1.365(5) yes C29 . H291 . 0.943 no C30 . H301 . 0.942 no C31 . C32 . 1.376(4) yes C31 . S1 . 1.725(3) yes C32 . C33 . 1.405(4) yes C32 . H321 . 0.945 no C33 . C34 . 1.368(4) yes C33 . H331 . 0.935 no C34 . C35 . 1.434(4) yes C34 . S1 . 1.730(3) yes C35 . C36 . 1.188(4) yes C36 . Si1 . 1.848(3) yes C37 . C38 . 1.526(6) yes C37 . C39 . 1.540(5) yes C37 . Si1 . 1.863(3) yes C37 . H371 . 1.002 no C38 . H381 . 0.969 no C38 . H382 . 0.971 no C38 . H383 . 0.969 no C39 . H391 . 0.983 no C39 . H392 . 0.972 no C39 . H393 . 0.969 no C40 . C41 . 1.530(6) yes C40 . C42 . 1.549(5) yes C40 . Si1 . 1.871(4) yes C40 . H401 . 0.995 no C41 . H411 . 0.978 no C41 . H412 . 0.976 no C41 . H413 . 0.975 no C42 . H421 . 0.973 no C42 . H422 . 0.971 no C42 . H423 . 0.973 no C43 . C44 . 1.540(7) yes C43 . C45 . 1.539(6) yes C43 . Si1 . 1.900(4) yes C43 . H431 . 0.990 no C44 . H441 . 0.977 no C44 . H442 . 0.962 no C44 . H443 . 0.971 no C45 . H451 . 0.978 no C45 . H452 . 0.970 no C45 . H453 . 0.969 no C46 . C47 . 1.370(4) yes C46 . S2 . 1.721(3) yes C47 . C48 . 1.402(4) yes C47 . H471 . 0.932 no C48 . C49 . 1.362(5) yes C48 . H481 . 0.939 no C49 . C50 . 1.447(4) yes C49 . S2 . 1.733(3) yes C50 . C51 . 1.174(5) yes C51 . Si2 . 1.842(4) yes C52 . C53 . 1.534(7) yes C52 . C54 . 1.541(7) yes C52 . Si2 . 1.880(4) yes C52 . H521 . 1.002 no C53 . H531 . 0.977 no C53 . H532 . 0.976 no C53 . H533 . 0.984 no C54 . H541 . 0.969 no C54 . H542 . 0.973 no C54 . H543 . 0.971 no C55 . C56 . 1.502(9) yes C55 . C57 . 1.519(7) yes C55 . Si2 . 1.892(4) yes C55 . H551 . 0.989 no C56 . H561 . 0.967 no C56 . H562 . 0.965 no C56 . H563 . 0.962 no C57 . H571 . 0.969 no C57 . H572 . 0.964 no C57 . H573 . 0.966 no C58 . C59 . 1.500(8) yes C58 . C60 . 1.534(6) yes C58 . Si2 . 1.895(5) yes C58 . H581 . 0.992 no C59 . H591 . 0.979 no C59 . H592 . 0.973 no C59 . H593 . 0.974 no C60 . H601 . 0.976 no C60 . H602 . 0.976 no C60 . H603 . 0.976 no P1 . F1 . 1.596(2) yes P1 . F2 . 1.595(2) yes P1 . F3 . 1.6060(18) yes P1 . F4 . 1.5962(19) yes P1 . F5 . 1.589(2) yes P1 . F6 . 1.607(2) yes P2 . F11 . 1.558(4) yes P2 . F12 . 1.596(4) yes P2 . F13 . 1.526(5) yes P2 . F14 . 1.645(5) yes P2 . F15 . 1.602(3) yes P2 . F16 . 1.583(3) yes P2 . F21 . 1.624(5) yes P2 . F22 . 1.546(5) yes P2 . F23 . 1.623(4) yes P2 . F24 . 1.533(4) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 79.22(8) yes N1 . Ru1 . N3 . 158.22(8) yes N2 . Ru1 . N3 . 79.08(9) yes N1 . Ru1 . N4 . 92.37(9) yes N2 . Ru1 . N4 . 98.25(9) yes N3 . Ru1 . N4 . 92.62(9) yes N1 . Ru1 . N5 . 102.50(8) yes N2 . Ru1 . N5 . 176.85(9) yes N3 . Ru1 . N5 . 99.26(9) yes N4 . Ru1 . N5 . 79.10(9) yes N1 . Ru1 . N6 . 93.66(9) yes N2 . Ru1 . N6 . 103.56(9) yes N3 . Ru1 . N6 . 89.54(9) yes N4 . Ru1 . N6 . 158.10(9) yes N5 . Ru1 . N6 . 79.04(9) yes Ru1 . N1 . C1 . 128.56(17) yes Ru1 . N1 . C5 . 113.73(17) yes C1 . N1 . C5 . 117.7(2) yes Ru1 . N2 . C6 . 119.51(17) yes Ru1 . N2 . C10 . 119.16(17) yes C6 . N2 . C10 . 121.1(2) yes Ru1 . N3 . C11 . 115.00(18) yes Ru1 . N3 . C15 . 127.12(19) yes C11 . N3 . C15 . 117.7(2) yes Ru1 . N4 . C16 . 127.7(2) yes Ru1 . N4 . C20 . 114.02(18) yes C16 . N4 . C20 . 118.3(3) yes Ru1 . N5 . C21 . 119.22(18) yes Ru1 . N5 . C25 . 119.32(17) yes C21 . N5 . C25 . 121.4(2) yes Ru1 . N6 . C26 . 114.30(18) yes Ru1 . N6 . C30 . 127.84(19) yes C26 . N6 . C30 . 117.7(2) yes N1 . C1 . C2 . 122.9(2) yes N1 . C1 . H11 . 117.4 no C2 . C1 . H11 . 119.7 no C1 . C2 . C3 . 119.4(2) yes C1 . C2 . H21 . 119.6 no C3 . C2 . H21 . 121.0 no C2 . C3 . C4 . 118.6(3) yes C2 . C3 . H31 . 121.0 no C4 . C3 . H31 . 120.4 no C3 . C4 . C5 . 119.9(2) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 119.8 no N1 . C5 . C4 . 121.5(2) yes N1 . C5 . C6 . 114.8(2) yes C4 . C5 . C6 . 123.8(2) yes C5 . C6 . N2 . 112.5(2) yes C5 . C6 . C7 . 126.6(2) yes N2 . C6 . C7 . 120.9(2) yes C6 . C7 . C8 . 119.4(2) yes C6 . C7 . H71 . 120.4 no C8 . C7 . H71 . 120.3 no C7 . C8 . C9 . 118.7(2) yes C7 . C8 . C31 . 119.7(2) yes C9 . C8 . C31 . 121.6(2) yes C8 . C9 . C10 . 119.5(2) yes C8 . C9 . H91 . 120.1 no C10 . C9 . H91 . 120.4 no C9 . C10 . N2 . 120.4(2) yes C9 . C10 . C11 . 126.8(2) yes N2 . C10 . C11 . 112.8(2) yes C10 . C11 . N3 . 113.6(2) yes C10 . C11 . C12 . 124.3(2) yes N3 . C11 . C12 . 122.1(2) yes C11 . C12 . C13 . 119.2(3) yes C11 . C12 . H121 . 120.5 no C13 . C12 . H121 . 120.3 no C12 . C13 . C14 . 118.5(3) yes C12 . C13 . H131 . 120.0 no C14 . C13 . H131 . 121.5 no C13 . C14 . C15 . 120.3(3) yes C13 . C14 . H141 . 120.0 no C15 . C14 . H141 . 119.7 no C14 . C15 . N3 . 122.2(3) yes C14 . C15 . H151 . 120.6 no N3 . C15 . H151 . 117.2 no N4 . C16 . C17 . 122.6(3) yes N4 . C16 . H161 . 117.7 no C17 . C16 . H161 . 119.7 no C16 . C17 . C18 . 119.1(3) yes C16 . C17 . H171 . 120.2 no C18 . C17 . H171 . 120.7 no C17 . C18 . C19 . 119.5(3) yes C17 . C18 . H181 . 120.8 no C19 . C18 . H181 . 119.7 no C18 . C19 . C20 . 119.5(3) yes C18 . C19 . H191 . 120.3 no C20 . C19 . H191 . 120.2 no C19 . C20 . N4 . 121.0(3) yes C19 . C20 . C21 . 124.0(2) yes N4 . C20 . C21 . 115.0(2) yes C20 . C21 . N5 . 112.6(2) yes C20 . C21 . C22 . 127.1(3) yes N5 . C21 . C22 . 120.3(3) yes C21 . C22 . C23 . 119.4(3) yes C21 . C22 . H221 . 119.6 no C23 . C22 . H221 . 121.0 no C22 . C23 . C24 . 119.0(2) yes C22 . C23 . C46 . 119.8(3) yes C24 . C23 . C46 . 121.1(3) yes C23 . C24 . C25 . 119.6(3) yes C23 . C24 . H241 . 120.1 no C25 . C24 . H241 . 120.3 no C24 . C25 . N5 . 120.3(2) yes C24 . C25 . C26 . 126.8(3) yes N5 . C25 . C26 . 112.9(2) yes C25 . C26 . N6 . 114.3(2) yes C25 . C26 . C27 . 124.1(2) yes N6 . C26 . C27 . 121.6(3) yes C26 . C27 . C28 . 119.3(3) yes C26 . C27 . H271 . 120.4 no C28 . C27 . H271 . 120.4 no C27 . C28 . C29 . 119.4(3) yes C27 . C28 . H281 . 119.7 no C29 . C28 . H281 . 120.9 no C28 . C29 . C30 . 119.5(3) yes C28 . C29 . H291 . 120.9 no C30 . C29 . H291 . 119.5 no C29 . C30 . N6 . 122.6(3) yes C29 . C30 . H301 . 120.0 no N6 . C30 . H301 . 117.4 no C8 . C31 . C32 . 127.9(2) yes C8 . C31 . S1 . 121.5(2) yes C32 . C31 . S1 . 110.56(19) yes C31 . C32 . C33 . 113.4(3) yes C31 . C32 . H321 . 122.8 no C33 . C32 . H321 . 123.8 no C32 . C33 . C34 . 113.0(2) yes C32 . C33 . H331 . 124.5 no C34 . C33 . H331 . 122.6 no C33 . C34 . C35 . 126.9(3) yes C33 . C34 . S1 . 111.04(19) yes C35 . C34 . S1 . 122.0(2) yes C34 . C35 . C36 . 173.7(3) yes C35 . C36 . Si1 . 166.8(3) yes C38 . C37 . C39 . 111.8(3) yes C38 . C37 . Si1 . 114.1(2) yes C39 . C37 . Si1 . 113.1(2) yes C38 . C37 . H371 . 107.0 no C39 . C37 . H371 . 106.0 no Si1 . C37 . H371 . 104.0 no C37 . C38 . H381 . 109.6 no C37 . C38 . H382 . 108.8 no H381 . C38 . H382 . 110.1 no C37 . C38 . H383 . 108.6 no H381 . C38 . H383 . 108.8 no H382 . C38 . H383 . 110.9 no C37 . C39 . H391 . 107.9 no C37 . C39 . H392 . 109.3 no H391 . C39 . H392 . 110.3 no C37 . C39 . H393 . 109.2 no H391 . C39 . H393 . 110.1 no H392 . C39 . H393 . 110.1 no C41 . C40 . C42 . 112.7(3) yes C41 . C40 . Si1 . 113.8(3) yes C42 . C40 . Si1 . 111.1(3) yes C41 . C40 . H401 . 106.7 no C42 . C40 . H401 . 106.1 no Si1 . C40 . H401 . 105.8 no C40 . C41 . H411 . 110.4 no C40 . C41 . H412 . 108.2 no H411 . C41 . H412 . 107.5 no C40 . C41 . H413 . 111.2 no H411 . C41 . H413 . 109.5 no H412 . C41 . H413 . 110.0 no C40 . C42 . H421 . 109.3 no C40 . C42 . H422 . 108.7 no H421 . C42 . H422 . 110.1 no C40 . C42 . H423 . 109.0 no H421 . C42 . H423 . 110.0 no H422 . C42 . H423 . 109.7 no C44 . C43 . C45 . 113.4(4) yes C44 . C43 . Si1 . 111.2(3) yes C45 . C43 . Si1 . 111.8(3) yes C44 . C43 . H431 . 106.9 no C45 . C43 . H431 . 107.5 no Si1 . C43 . H431 . 105.5 no C43 . C44 . H441 . 106.5 no C43 . C44 . H442 . 108.5 no H441 . C44 . H442 . 111.0 no C43 . C44 . H443 . 109.1 no H441 . C44 . H443 . 111.3 no H442 . C44 . H443 . 110.3 no C43 . C45 . H451 . 107.0 no C43 . C45 . H452 . 109.2 no H451 . C45 . H452 . 110.6 no C43 . C45 . H453 . 108.8 no H451 . C45 . H453 . 111.3 no H452 . C45 . H453 . 109.8 no C23 . C46 . C47 . 127.7(3) yes C23 . C46 . S2 . 120.9(2) yes C47 . C46 . S2 . 111.2(2) yes C46 . C47 . C48 . 113.1(3) yes C46 . C47 . H471 . 122.9 no C48 . C47 . H471 . 124.0 no C47 . C48 . C49 . 112.9(3) yes C47 . C48 . H481 . 124.3 no C49 . C48 . H481 . 122.8 no C48 . C49 . C50 . 128.7(3) yes C48 . C49 . S2 . 111.3(2) yes C50 . C49 . S2 . 120.0(3) yes C49 . C50 . C51 . 177.0(4) yes C50 . C51 . Si2 . 173.6(4) yes C53 . C52 . C54 . 110.1(4) yes C53 . C52 . Si2 . 114.4(4) yes C54 . C52 . Si2 . 113.0(3) yes C53 . C52 . H521 . 106.7 no C54 . C52 . H521 . 107.9 no Si2 . C52 . H521 . 104.3 no C52 . C53 . H531 . 109.0 no C52 . C53 . H532 . 110.5 no H531 . C53 . H532 . 110.4 no C52 . C53 . H533 . 107.0 no H531 . C53 . H533 . 110.1 no H532 . C53 . H533 . 109.8 no C52 . C54 . H541 . 108.4 no C52 . C54 . H542 . 109.8 no H541 . C54 . H542 . 110.2 no C52 . C54 . H543 . 107.9 no H541 . C54 . H543 . 110.1 no H542 . C54 . H543 . 110.5 no C56 . C55 . C57 . 110.8(6) yes C56 . C55 . Si2 . 112.8(4) yes C57 . C55 . Si2 . 110.8(4) yes C56 . C55 . H551 . 107.9 no C57 . C55 . H551 . 107.3 no Si2 . C55 . H551 . 106.9 no C55 . C56 . H561 . 108.9 no C55 . C56 . H562 . 108.9 no H561 . C56 . H562 . 111.2 no C55 . C56 . H563 . 108.1 no H561 . C56 . H563 . 110.9 no H562 . C56 . H563 . 108.7 no C55 . C57 . H571 . 107.6 no C55 . C57 . H572 . 109.4 no H571 . C57 . H572 . 111.0 no C55 . C57 . H573 . 108.8 no H571 . C57 . H573 . 109.8 no H572 . C57 . H573 . 110.2 no C59 . C58 . C60 . 112.0(5) yes C59 . C58 . Si2 . 112.9(3) yes C60 . C58 . Si2 . 112.3(4) yes C59 . C58 . H581 . 106.5 no C60 . C58 . H581 . 106.4 no Si2 . C58 . H581 . 106.1 no C58 . C59 . H591 . 110.3 no C58 . C59 . H592 . 106.7 no H591 . C59 . H592 . 109.6 no C58 . C59 . H593 . 109.0 no H591 . C59 . H593 . 110.2 no H592 . C59 . H593 . 110.9 no C58 . C60 . H601 . 109.4 no C58 . C60 . H602 . 107.5 no H601 . C60 . H602 . 110.4 no C58 . C60 . H603 . 108.4 no H601 . C60 . H603 . 110.5 no H602 . C60 . H603 . 110.5 no C34 . S1 . C31 . 92.02(13) yes C49 . S2 . C46 . 91.35(15) yes C43 . Si1 . C40 . 110.24(18) yes C43 . Si1 . C37 . 109.35(17) yes C40 . Si1 . C37 . 117.28(16) yes C43 . Si1 . C36 . 102.50(15) yes C40 . Si1 . C36 . 109.39(15) yes C37 . Si1 . C36 . 107.01(14) yes C58 . Si2 . C55 . 111.9(2) yes C58 . Si2 . C52 . 110.3(2) yes C55 . Si2 . C52 . 112.8(2) yes C58 . Si2 . C51 . 106.02(19) yes C55 . Si2 . C51 . 107.29(19) yes C52 . Si2 . C51 . 108.17(19) yes F1 . P1 . F2 . 179.22(12) yes F1 . P1 . F3 . 89.84(11) yes F2 . P1 . F3 . 89.58(11) yes F1 . P1 . F4 . 89.71(12) yes F2 . P1 . F4 . 90.86(12) yes F3 . P1 . F4 . 178.55(12) yes F1 . P1 . F5 . 90.29(13) yes F2 . P1 . F5 . 90.23(12) yes F3 . P1 . F5 . 89.90(11) yes F4 . P1 . F5 . 91.47(12) yes F1 . P1 . F6 . 89.57(13) yes F2 . P1 . F6 . 89.90(12) yes F3 . P1 . F6 . 88.35(11) yes F4 . P1 . F6 . 90.28(11) yes F5 . P1 . F6 . 178.24(12) yes F11 . P2 . F12 . 171.3(4) yes F11 . P2 . F13 . 96.2(4) yes F12 . P2 . F13 . 91.3(3) yes F11 . P2 . F14 . 87.5(3) yes F12 . P2 . F14 . 84.8(3) yes F13 . P2 . F14 . 175.3(4) yes F11 . P2 . F15 . 88.9(2) yes F12 . P2 . F15 . 87.0(2) yes F13 . P2 . F15 . 87.0(3) yes F14 . P2 . F15 . 90.1(2) yes F11 . P2 . F16 . 91.4(2) yes F12 . P2 . F16 . 92.6(2) yes F13 . P2 . F16 . 93.3(3) yes F14 . P2 . F16 . 89.5(2) yes F15 . P2 . F16 . 179.55(18) yes F15 . P2 . F21 . 91.1(2) yes F15 . P2 . F22 . 90.1(3) yes F15 . P2 . F23 . 93.4(2) yes F15 . P2 . F24 . 89.7(3) yes F16 . P2 . F21 . 89.3(2) yes F16 . P2 . F22 . 89.5(3) yes F21 . P2 . F22 . 173.3(3) yes F16 . P2 . F23 . 86.8(2) yes F21 . P2 . F23 . 85.1(3) yes F22 . P2 . F23 . 88.2(3) yes F16 . P2 . F24 . 90.2(2) yes F21 . P2 . F24 . 89.7(3) yes F22 . P2 . F24 . 96.9(4) yes F23 . P2 . F24 . 174.0(4) yes # start Validation Reply Form _vrf_PLAT220_CRYSTALS_cif ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.98 Ratio RESPONSE: This is not surprising, considering the length of the terminal substituent. ; _vrf_PLAT222_CRYSTALS_cif ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.74 Ratio RESPONSE: This is not surprising, considering the length of the terminal substituent. ; _vrf_PLAT366_CRYSTALS_cif ; PROBLEM: Short? C(sp?)-C(sp?) Bond C35 - C36 ... 1.19 Ang. RESPONSE: The C35-C36 bond is an alkyne triple bond. ; # end Validation Reply Form # Attachment '[Ru_5_2][PF6]2.cif' data_CRYSTALS_cifa _database_code_depnum_ccdc_archive 'CCDC 694389' _audit_creation_date 07-07-18 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '6211343 em100_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.0690(2) _cell_length_b 12.8574(2) _cell_length_c 19.4249(4) _cell_angle_alpha 98.4604(13) _cell_angle_beta 97.6830(10) _cell_angle_gamma 92.2028(13) _cell_volume 2216.35(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C42 H26 F6 N6 P1 Ru1 S2 # Dc = 1.39 Fooo = 1112.00 Mu = 5.45 M = 924.87 # Found Formula = C44 H29 F12 N7 P2 Ru1 S2 # Dc = 1.66 FOOO = 1112.00 Mu = 6.14 M = 1110.89 _chemical_formula_sum 'C44 H29 F12 N7 P2 Ru1 S2' _chemical_formula_moiety 'C42 H26 N6 Ru S2, 2(F6 P), C2 H3 N' _chemical_compound_source ? _chemical_formula_weight 1110.89 _cell_measurement_reflns_used 9732 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.24 _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.614 # Sheldrick geometric approximatio 0.93 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.96 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 18876 _reflns_number_total 10151 _diffrn_reflns_av_R_equivalents 0.028 # Number of reflections with Friedels Law is 10151 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10185 _diffrn_reflns_theta_min 1.070 _diffrn_reflns_theta_max 27.502 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.502 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.50 _refine_diff_density_max 0.61 _refine_ls_number_reflns 7292 _refine_ls_number_restraints 2107 _refine_ls_number_parameters 715 #_refine_ls_R_factor_ref 0.0425 _refine_ls_wR_factor_ref 0.0324 _refine_ls_goodness_of_fit_ref 1.0455 #_reflns_number_all 10046 _refine_ls_R_factor_all 0.0671 _refine_ls_wR_factor_all 0.0431 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>1.8\s(I) _reflns_number_gt 7292 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_gt 0.0324 _refine_ls_shift/su_max 0.035833 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.837E-01 -0.545 -0.207 -0.244 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ru1 Ru 0.22029(2) 0.242961(18) 0.265602(12) 0.0365 1.0000 Uani . . . . . . N1 N 0.1233(2) 0.38005(18) 0.24654(13) 0.0415 1.0000 Uani . . . . . . N2 N 0.1782(2) 0.21769(17) 0.16192(12) 0.0376 1.0000 Uani . . . . . . N3 N 0.3064(2) 0.09674(18) 0.24325(12) 0.0383 1.0000 Uani . . . . . . N4 N 0.4307(2) 0.31740(17) 0.28081(11) 0.0373 1.0000 Uani . . . . . . N5 N 0.2650(2) 0.26434(18) 0.36917(12) 0.0390 1.0000 Uani . . . . . . N6 N 0.0222(2) 0.18651(18) 0.29219(12) 0.0407 1.0000 Uani . . . . . . N7 N 0.8033(4) -0.4905(3) -0.0108(2) 0.0803 1.0000 Uani . . . . . . C1 C 0.1042(3) 0.4638(2) 0.29439(17) 0.0475 1.0000 Uani . . . . . . C2 C 0.0350(4) 0.5519(3) 0.2752(2) 0.0562 1.0000 Uani . . . . . . C3 C -0.0151(4) 0.5537(3) 0.2047(2) 0.0557 1.0000 Uani . . . . . . C4 C 0.0048(3) 0.4687(2) 0.15515(18) 0.0502 1.0000 Uani . . . . . . C5 C 0.0742(3) 0.3830(2) 0.17673(16) 0.0428 1.0000 Uani . . . . . . C6 C 0.1062(3) 0.2895(2) 0.12775(15) 0.0407 1.0000 Uani . . . . . . C7 C 0.0739(3) 0.2730(2) 0.05548(16) 0.0457 1.0000 Uani . . . . . . C8 C 0.1208(3) 0.1822(2) 0.01738(16) 0.0475 1.0000 Uani . . . . . . C9 C 0.1938(3) 0.1091(2) 0.05354(15) 0.0449 1.0000 Uani . . . . . . C10 C 0.2219(3) 0.1285(2) 0.12605(14) 0.0388 1.0000 Uani . . . . . . C11 C 0.2987(3) 0.0610(2) 0.17269(14) 0.0389 1.0000 Uani . . . . . . C12 C 0.3622(3) -0.0314(2) 0.14851(16) 0.0474 1.0000 Uani . . . . . . C13 C 0.4318(4) -0.0901(2) 0.19627(17) 0.0508 1.0000 Uani . . . . . . C14 C 0.4363(3) -0.0552(2) 0.26676(17) 0.0491 1.0000 Uani . . . . . . C15 C 0.3734(3) 0.0383(2) 0.28871(15) 0.0422 1.0000 Uani . . . . . . C16 C 0.5082(3) 0.3450(2) 0.23173(15) 0.0433 1.0000 Uani . . . . . . C17 C 0.6466(3) 0.3991(3) 0.24851(17) 0.0487 1.0000 Uani . . . . . . C18 C 0.7065(3) 0.4261(3) 0.31802(17) 0.0513 1.0000 Uani . . . . . . C19 C 0.6285(3) 0.3979(2) 0.36944(16) 0.0467 1.0000 Uani . . . . . . C20 C 0.4907(3) 0.3435(2) 0.35067(14) 0.0383 1.0000 Uani . . . . . . C21 C 0.3984(3) 0.3112(2) 0.40078(14) 0.0382 1.0000 Uani . . . . . . C22 C 0.4336(3) 0.3243(2) 0.47326(14) 0.0423 1.0000 Uani . . . . . . C23 C 0.3321(3) 0.2882(2) 0.51393(15) 0.0443 1.0000 Uani . . . . . . C24 C 0.1959(3) 0.2391(3) 0.47947(15) 0.0479 1.0000 Uani . . . . . . C25 C 0.1639(3) 0.2299(2) 0.40729(15) 0.0439 1.0000 Uani . . . . . . C26 C 0.0229(3) 0.1880(2) 0.36281(16) 0.0482 1.0000 Uani . . . . . . C27 C -0.1041(4) 0.1586(3) 0.38961(19) 0.0640 1.0000 Uani . . . . . . C28 C -0.2348(4) 0.1301(3) 0.3444(2) 0.0658 1.0000 Uani . . . . . . C29 C -0.2371(3) 0.1313(3) 0.27433(19) 0.0566 1.0000 Uani . . . . . . C30 C -0.1071(3) 0.1586(2) 0.24890(17) 0.0471 1.0000 Uani . . . . . . C31 C 0.0970(4) 0.1650(3) -0.05835(15) 0.0578 1.0000 Uani D U . . . . S1 S -0.03963(11) 0.20837(8) -0.11120(5) 0.0510 0.8000 Uani D U . . . . C32 C 0.1777(3) 0.1171(2) -0.10217(12) 0.0689 0.8000 Uani D U . . . . C33 C 0.1552(5) 0.1065(4) -0.1743(2) 0.0606 0.8000 Uani D U . . . . C34 C 0.0280(5) 0.1564(3) -0.1870(2) 0.0420 0.8000 Uani D U . . . . C35 C -0.0547(5) 0.1636(3) -0.2570(2) 0.0523 0.8000 Uani . U . . . . C36 C -0.1184(6) 0.1675(4) -0.3110(3) 0.0760 0.8000 Uani . U . . . . C37 C 0.3650(4) 0.2996(3) 0.59069(16) 0.0499 1.0000 Uani . . . . . . C38 C 0.2731(3) 0.2762(3) 0.63896(15) 0.0491 1.0000 Uani . . . . . . C39 C 0.3398(4) 0.2966(3) 0.70774(18) 0.0585 1.0000 Uani . . . . . . C40 C 0.4816(4) 0.3369(3) 0.71513(16) 0.0509 1.0000 Uani . . . . . . C41 C 0.5848(4) 0.3686(3) 0.78027(18) 0.0562 1.0000 Uani . . . . . . C42 C 0.6592(4) 0.3904(3) 0.8301(2) 0.0684 1.0000 Uani . . . . . . C43 C 0.6314(6) -0.4096(5) 0.0743(3) 0.1021 1.0000 Uani . . . . . . C44 C 0.7264(5) -0.4539(4) 0.0263(2) 0.0720 1.0000 Uani . . . . . . S2 S 0.53584(9) 0.34792(7) 0.63465(4) 0.0524 1.0000 Uani . . . . . . P1 P 0.62961(10) 0.21129(7) 0.04969(4) 0.0514 1.0000 Uani D U . . . . P2 P 0.0000 0.5000 0.5000 0.0687 1.0000 Uani DS U . . . . P3 P 0.5000 0.0000 0.5000 0.0775 0.5000 Uani DS U . . . . P4 P 0.6059(10) 0.0266(5) 0.5059(3) 0.1039 0.2500 Uani D U . . . . F1 F 0.5176(3) 0.1245(3) 0.00206(15) 0.1209 1.0000 Uani D U . . . . F2 F 0.7414(3) 0.2947(2) 0.09938(14) 0.0989 1.0000 Uani D U . . . . F3 F 0.7597(3) 0.13461(18) 0.03802(13) 0.0808 1.0000 Uani D U . . . . F4 F 0.4974(3) 0.2870(2) 0.06095(12) 0.0900 1.0000 Uani D U . . . . F5 F 0.5954(3) 0.1627(2) 0.11662(13) 0.0888 1.0000 Uani D U . . . . F6 F 0.6609(4) 0.2584(2) -0.01700(14) 0.1166 1.0000 Uani D U . . . . F11 F -0.0478(2) 0.39812(19) 0.44367(12) 0.0838 1.0000 Uani D U . . . . F13 F 0.1646(2) 0.4991(2) 0.47839(12) 0.0857 1.0000 Uani D U . . . . F15 F 0.0489(3) 0.4284(2) 0.55868(12) 0.0840 1.0000 Uani D U . . . . F21 F 0.4820(10) -0.1008(5) 0.5361(4) 0.1123 0.5000 Uani D U . . . . F23 F 0.4144(12) 0.0547(6) 0.5600(4) 0.1240 0.5000 Uani D U . . . . F25 F 0.3442(14) -0.0152(12) 0.4537(6) 0.1083 0.2500 Uani D U . . . . F31 F 0.5149(18) -0.0796(10) 0.5055(7) 0.1322 0.2500 Uani D U . . . . F32 F 0.6853(16) 0.1341(7) 0.5060(6) 0.1255 0.2500 Uani D U . . . . F33 F 0.5329(12) 0.0821(5) 0.5688(3) 0.1338 0.5000 Uani D U . . . . F34 F 0.6926(19) -0.0223(10) 0.4464(6) 0.1378 0.2500 Uani D U . . . . F35 F 0.7244(15) -0.0093(8) 0.5600(5) 0.1094 0.2500 Uani D U . . . . F36 F 0.4717(18) 0.0579(10) 0.4533(6) 0.1354 0.2500 Uani D U . . . . C52 C -0.02362(11) 0.20115(8) -0.09341(5) 0.0526 0.2000 Uani D U . . . . S10 S 0.1820(3) 0.1019(2) -0.11290(12) 0.0665 0.2000 Uani D U . . . . C53 C -0.0599(17) 0.1916(13) -0.1662(4) 0.0663 0.2000 Uani D U . . . . C54 C 0.055(2) 0.131(2) -0.1806(6) 0.0734 0.2000 Uani D U . . . . C55 C 0.082(2) 0.1088(13) -0.2552(7) 0.0746 0.2000 Uani D U . . . . C56 C 0.121(2) 0.0890(14) -0.3115(8) 0.0830 0.2000 Uani D U . . . . H11 H 0.1384 0.4625 0.3420 0.0539 1.0000 Uiso R . . . . . H21 H 0.0238 0.6094 0.3093 0.0673 1.0000 Uiso R . . . . . H31 H -0.0621 0.6120 0.1908 0.0661 1.0000 Uiso R . . . . . H41 H -0.0278 0.4700 0.1075 0.0604 1.0000 Uiso R . . . . . H71 H 0.0225 0.3219 0.0323 0.0514 1.0000 Uiso R . . . . . H91 H 0.2251 0.0469 0.0292 0.0522 1.0000 Uiso R . . . . . H121 H 0.3570 -0.0532 0.0997 0.0542 1.0000 Uiso R . . . . . H131 H 0.4760 -0.1531 0.1807 0.0602 1.0000 Uiso R . . . . . H141 H 0.4800 -0.0938 0.3002 0.0584 1.0000 Uiso R . . . . . H151 H 0.3777 0.0621 0.3368 0.0503 1.0000 Uiso R . . . . . H161 H 0.4663 0.3257 0.1848 0.0480 1.0000 Uiso R . . . . . H171 H 0.6983 0.4176 0.2126 0.0554 1.0000 Uiso R . . . . . H181 H 0.7994 0.4636 0.3308 0.0582 1.0000 Uiso R . . . . . H191 H 0.6683 0.4148 0.4170 0.0532 1.0000 Uiso R . . . . . H221 H 0.5266 0.3568 0.4947 0.0480 1.0000 Uiso R . . . . . H241 H 0.1262 0.2130 0.5052 0.0553 1.0000 Uiso R . . . . . H271 H -0.0997 0.1584 0.4376 0.0714 1.0000 Uiso R . . . . . H281 H -0.3213 0.1104 0.3623 0.0730 1.0000 Uiso R . . . . . H291 H -0.3248 0.1126 0.2423 0.0652 1.0000 Uiso R . . . . . H301 H -0.1081 0.1578 0.1999 0.0561 1.0000 Uiso R . . . . . H381 H 0.1753 0.2493 0.6255 0.0551 1.0000 Uiso R . . . . . H391 H 0.2923 0.2835 0.7465 0.0694 1.0000 Uiso R . . . . . H421 H 0.7137 0.4123 0.8762 0.0837 1.0000 Uiso R . . . . . H431 H 0.5468 -0.3802 0.0499 0.1582 1.0000 Uiso R . . . . . H432 H 0.5944 -0.4630 0.0995 0.1583 1.0000 Uiso R . . . . . H433 H 0.6875 -0.3545 0.1090 0.1583 1.0000 Uiso R . . . . . H321 H 0.2631 0.0856 -0.0819 0.0801 0.8000 Uiso . . . . . . H331 H 0.2149 0.0721 -0.2070 0.0739 0.8000 Uiso R . . . . . H361 H -0.1720 0.1709 -0.3567 0.0894 0.8000 Uiso R . . . . . H521 H -0.0926 0.2361 -0.0658 0.0616 0.2000 Uiso . . . . . . H531 H -0.1373 0.2193 -0.1958 0.0894 0.2000 Uiso R . . . . . H561 H 0.1536 0.0721 -0.3567 0.1092 0.2000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03304(10) 0.03861(11) 0.03395(11) -0.00213(8) -0.00030(8) 0.00085(8) N1 0.0337(11) 0.0387(12) 0.0483(13) -0.0010(10) 0.0011(10) 0.0000(9) N2 0.0316(11) 0.0394(12) 0.0379(11) 0.0017(9) -0.0034(9) -0.0015(9) N3 0.0358(11) 0.0399(12) 0.0366(11) 0.0003(9) 0.0031(9) -0.0009(9) N4 0.0328(11) 0.0387(11) 0.0363(11) -0.0028(9) -0.0008(9) 0.0043(9) N5 0.0337(11) 0.0425(12) 0.0369(12) -0.0041(9) 0.0019(9) 0.0039(9) N6 0.0343(11) 0.0426(12) 0.0407(12) -0.0015(10) -0.0009(9) -0.0009(9) N7 0.077(2) 0.094(2) 0.068(2) 0.0124(18) 0.0067(18) -0.0074(19) C1 0.0386(14) 0.0469(16) 0.0517(17) -0.0060(13) 0.0036(12) 0.0006(12) C2 0.0483(16) 0.0433(16) 0.075(2) -0.0033(15) 0.0157(15) 0.0023(13) C3 0.0479(16) 0.0458(16) 0.076(2) 0.0142(15) 0.0111(15) 0.0095(13) C4 0.0425(15) 0.0492(16) 0.0591(18) 0.0127(14) 0.0030(13) 0.0041(13) C5 0.0348(13) 0.0426(14) 0.0484(15) 0.0050(12) 0.0005(11) -0.0024(11) C6 0.0362(13) 0.0418(14) 0.0404(14) 0.0035(11) -0.0032(11) -0.0029(11) C7 0.0423(14) 0.0490(16) 0.0424(15) 0.0085(12) -0.0064(12) -0.0024(12) C8 0.0501(16) 0.0484(16) 0.0400(15) 0.0043(12) -0.0021(12) -0.0091(13) C9 0.0507(15) 0.0432(15) 0.0378(14) 0.0007(11) 0.0035(12) -0.0054(12) C10 0.0405(13) 0.0372(13) 0.0352(13) -0.0020(10) 0.0018(11) -0.0025(11) C11 0.0398(13) 0.0400(14) 0.0340(13) -0.0004(10) 0.0033(11) -0.0048(11) C12 0.0521(16) 0.0421(15) 0.0449(15) -0.0040(12) 0.0079(13) -0.0011(13) C13 0.0549(17) 0.0398(15) 0.0565(18) 0.0008(13) 0.0097(14) 0.0052(13) C14 0.0459(15) 0.0449(15) 0.0568(18) 0.0125(13) 0.0036(13) 0.0040(13) C15 0.0397(14) 0.0470(15) 0.0392(14) 0.0051(12) 0.0055(11) 0.0001(12) C16 0.0403(14) 0.0461(15) 0.0406(14) -0.0010(12) 0.0034(11) 0.0020(12) C17 0.0427(15) 0.0553(17) 0.0453(16) 0.0005(13) 0.0050(12) -0.0025(13) C18 0.0389(14) 0.0559(17) 0.0545(17) -0.0016(14) 0.0032(13) -0.0064(13) C19 0.0379(14) 0.0535(16) 0.0435(15) -0.0033(13) -0.0003(12) 0.0019(12) C20 0.0354(13) 0.0394(13) 0.0360(13) -0.0040(10) -0.0003(10) 0.0067(10) C21 0.0345(13) 0.0406(14) 0.0354(13) -0.0020(10) -0.0021(10) 0.0067(11) C22 0.0362(13) 0.0487(15) 0.0375(14) -0.0031(12) -0.0009(11) 0.0067(11) C23 0.0425(14) 0.0536(16) 0.0349(14) -0.0014(12) 0.0047(11) 0.0119(12) C24 0.0422(14) 0.0585(17) 0.0403(15) -0.0032(13) 0.0084(12) 0.0027(13) C25 0.0403(14) 0.0486(15) 0.0400(14) -0.0038(12) 0.0065(12) 0.0048(12) C26 0.0411(14) 0.0527(16) 0.0467(16) -0.0059(13) 0.0078(12) -0.0007(12) C27 0.0476(17) 0.090(2) 0.0489(18) -0.0104(17) 0.0137(14) -0.0097(17) C28 0.0433(16) 0.084(2) 0.064(2) -0.0103(18) 0.0137(15) -0.0128(16) C29 0.0377(15) 0.0593(19) 0.066(2) -0.0035(15) -0.0008(14) -0.0080(13) C30 0.0411(14) 0.0451(15) 0.0500(16) -0.0008(13) -0.0018(12) -0.0018(12) C31 0.077(2) 0.0540(17) 0.0368(15) 0.0027(13) -0.0019(14) -0.0163(15) S1 0.0457(5) 0.0676(6) 0.0360(5) 0.0052(4) -0.0040(4) 0.0019(4) C32 0.1067(17) 0.0566(14) 0.0383(12) -0.0062(10) 0.0057(12) 0.0097(13) C33 0.076(2) 0.062(2) 0.044(2) 0.0001(18) 0.0158(19) 0.013(2) C34 0.0484(19) 0.040(2) 0.0356(17) 0.0054(15) 0.0012(15) -0.0096(15) C35 0.057(2) 0.056(2) 0.0399(19) 0.0039(16) 0.0017(16) -0.0139(18) C36 0.081(3) 0.090(3) 0.052(2) 0.006(2) -0.001(2) -0.012(3) C37 0.0492(16) 0.0564(17) 0.0408(15) 0.0001(13) 0.0005(13) 0.0101(14) C38 0.0374(14) 0.0687(19) 0.0406(15) 0.0035(13) 0.0076(12) 0.0056(13) C39 0.0585(18) 0.073(2) 0.0467(17) 0.0094(15) 0.0127(15) 0.0132(16) C40 0.0585(17) 0.0554(17) 0.0356(14) 0.0005(12) 0.0005(13) 0.0105(14) C41 0.0595(18) 0.069(2) 0.0451(17) 0.0146(15) 0.0162(15) 0.0141(16) C42 0.0582(19) 0.082(2) 0.063(2) -0.0013(19) 0.0173(17) -0.0038(18) C43 0.086(3) 0.153(4) 0.070(3) 0.021(3) 0.012(2) 0.031(3) C44 0.064(2) 0.092(3) 0.058(2) 0.0151(19) -0.0020(18) -0.008(2) S2 0.0486(4) 0.0676(5) 0.0377(4) 0.0005(3) 0.0026(3) 0.0022(4) P1 0.0512(4) 0.0556(5) 0.0429(4) -0.0049(3) 0.0043(3) 0.0015(4) P2 0.0540(7) 0.0833(9) 0.0535(7) -0.0257(6) -0.0149(6) 0.0291(7) P3 0.144(3) 0.055(2) 0.0441(16) 0.0164(15) 0.031(2) 0.049(2) P4 0.213(4) 0.065(3) 0.035(2) 0.0145(19) 0.015(3) 0.005(3) F1 0.0717(15) 0.163(3) 0.0978(19) -0.0680(18) 0.0099(14) -0.0298(16) F2 0.0776(15) 0.0972(17) 0.1027(18) -0.0454(14) 0.0204(13) -0.0295(13) F3 0.0698(13) 0.0729(14) 0.0990(17) -0.0012(12) 0.0213(12) 0.0175(11) F4 0.0930(16) 0.1181(19) 0.0622(13) 0.0106(13) 0.0143(12) 0.0513(15) F5 0.1111(18) 0.0831(16) 0.0816(15) 0.0203(12) 0.0380(14) 0.0112(14) F6 0.178(3) 0.115(2) 0.0813(17) 0.0400(15) 0.0688(17) 0.0516(19) F11 0.0695(13) 0.0906(15) 0.0697(13) -0.0358(11) -0.0224(10) 0.0298(11) F13 0.0579(12) 0.1106(18) 0.0718(14) -0.0291(13) -0.0115(10) 0.0287(12) F15 0.0777(14) 0.0993(17) 0.0628(13) -0.0135(11) -0.0137(11) 0.0356(12) F21 0.202(4) 0.059(3) 0.094(4) 0.027(3) 0.057(4) 0.045(3) F23 0.188(4) 0.086(4) 0.113(4) 0.008(3) 0.070(4) 0.039(4) F25 0.138(4) 0.122(5) 0.070(5) 0.028(5) 0.018(5) 0.026(5) F31 0.234(4) 0.075(5) 0.095(5) 0.032(5) 0.027(5) 0.023(5) F32 0.221(4) 0.061(4) 0.106(5) 0.012(4) 0.067(5) 0.018(5) F33 0.236(4) 0.093(4) 0.072(3) 0.013(3) 0.018(4) 0.014(4) F34 0.237(4) 0.091(5) 0.089(5) 0.005(5) 0.043(5) 0.012(5) F35 0.192(4) 0.072(4) 0.071(4) 0.009(4) 0.033(4) 0.058(4) F36 0.286(4) 0.058(5) 0.045(4) 0.003(4) -0.042(5) 0.037(5) C52 0.0473(5) 0.0692(6) 0.0376(5) 0.0055(4) -0.0038(4) 0.0020(4) S10 0.1079(17) 0.0579(14) 0.0395(12) -0.0045(10) 0.0392(12) 0.0228(13) C53 0.075(4) 0.078(5) 0.038(4) 0.014(5) -0.017(5) -0.015(5) C54 0.134(4) 0.045(5) 0.043(4) 0.005(4) 0.019(4) 0.000(5) C55 0.143(4) 0.043(4) 0.043(4) 0.020(4) 0.019(4) 0.007(4) C56 0.152(4) 0.052(5) 0.047(4) 0.012(4) 0.016(5) 0.011(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2730(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . N1 . 2.060(2) yes Ru1 . N2 . 1.975(2) yes Ru1 . N3 . 2.073(2) yes Ru1 . N4 . 2.067(2) yes Ru1 . N5 . 1.974(2) yes Ru1 . N6 . 2.069(2) yes N1 . C1 . 1.348(4) yes N1 . C5 . 1.376(4) yes N2 . C6 . 1.353(3) yes N2 . C10 . 1.353(3) yes N3 . C11 . 1.372(3) yes N3 . C15 . 1.342(4) yes N4 . C16 . 1.337(4) yes N4 . C20 . 1.380(3) yes N5 . C21 . 1.356(3) yes N5 . C25 . 1.353(4) yes N6 . C26 . 1.368(4) yes N6 . C30 . 1.351(3) yes N7 . C44 . 1.133(5) yes C1 . C2 . 1.389(4) yes C1 . H11 . 0.938 no C2 . C3 . 1.388(5) yes C2 . H21 . 0.935 no C3 . C4 . 1.381(5) yes C3 . H31 . 0.933 no C4 . C5 . 1.380(4) yes C4 . H41 . 0.935 no C5 . C6 . 1.483(4) yes C6 . C7 . 1.378(4) yes C7 . C8 . 1.400(4) yes C7 . H71 . 0.930 no C8 . C9 . 1.390(4) yes C8 . C31 . 1.441(4) yes C9 . C10 . 1.381(4) yes C9 . H91 . 0.941 no C10 . C11 . 1.473(4) yes C11 . C12 . 1.387(4) yes C12 . C13 . 1.384(4) yes C12 . H121 . 0.943 no C13 . C14 . 1.372(4) yes C13 . H131 . 0.945 no C14 . C15 . 1.385(4) yes C14 . H141 . 0.931 no C15 . H151 . 0.934 no C16 . C17 . 1.386(4) yes C16 . H161 . 0.934 no C17 . C18 . 1.375(4) yes C17 . H171 . 0.944 no C18 . C19 . 1.380(4) yes C18 . H181 . 0.939 no C19 . C20 . 1.386(4) yes C19 . H191 . 0.936 no C20 . C21 . 1.460(4) yes C21 . C22 . 1.385(4) yes C22 . C23 . 1.399(4) yes C22 . H221 . 0.942 no C23 . C24 . 1.403(4) yes C23 . C37 . 1.465(4) yes C24 . C25 . 1.380(4) yes C24 . H241 . 0.938 no C25 . C26 . 1.479(4) yes C26 . C27 . 1.388(4) yes C27 . C28 . 1.380(5) yes C27 . H271 . 0.927 no C28 . C29 . 1.360(5) yes C28 . H281 . 0.940 no C29 . C30 . 1.390(4) yes C29 . H291 . 0.941 no C30 . H301 . 0.950 no C31 . S1 . 1.668(3) yes C31 . C32 . 1.299(4) yes C31 . C52 . 1.345(3) yes C31 . S10 . 1.546(3) yes S1 . C34 . 1.725(4) yes C32 . C33 . 1.374(4) yes C32 . H321 . 0.952 no C33 . C34 . 1.353(5) yes C33 . H331 . 0.960 no C34 . C35 . 1.480(5) yes C35 . C36 . 1.137(6) yes C36 . H361 . 0.960 no C37 . C38 . 1.392(4) yes C37 . S2 . 1.712(3) yes C38 . C39 . 1.374(4) yes C38 . H381 . 0.929 no C39 . C40 . 1.350(5) yes C39 . H391 . 0.948 no C40 . C41 . 1.465(5) yes C40 . S2 . 1.724(3) yes C41 . C42 . 1.097(5) yes C42 . H421 . 0.960 no C43 . C44 . 1.426(6) yes C43 . H431 . 0.967 no C43 . H432 . 0.974 no C43 . H433 . 0.978 no P1 . F1 . 1.578(2) yes P1 . F2 . 1.568(2) yes P1 . F3 . 1.585(2) yes P1 . F4 . 1.591(2) yes P1 . F5 . 1.584(2) yes P1 . F6 . 1.562(3) yes P2 . F13 2_566 1.604(2) yes P2 . F15 2_566 1.597(2) yes P2 . F11 2_566 1.5839(19) yes P2 . F11 . 1.5839(19) yes P2 . F13 . 1.604(2) yes P2 . F15 . 1.597(2) yes P3 . F23 2_656 1.581(6) yes P3 . F21 2_656 1.574(6) yes P3 . F33 2_656 1.564(7) yes P3 . F25 2_656 1.559(11) yes P3 . F21 . 1.574(6) yes P3 . F23 . 1.581(6) yes P3 . F25 . 1.559(11) yes P3 . F33 . 1.564(7) yes P4 . P4 2_656 1.986(17) yes P4 . F31 . 1.567(12) yes P4 . F32 . 1.533(10) yes P4 . F33 . 1.562(9) yes P4 . F34 . 1.554(11) yes P4 . F35 . 1.534(11) yes P4 . F36 . 1.586(11) yes C52 . C53 . 1.394(8) yes C52 . H521 . 0.960 no S10 . C54 . 1.724(9) yes C53 . C54 . 1.359(9) yes C53 . H531 . 0.960 no C54 . C55 . 1.489(9) yes C55 . C56 . 1.193(9) yes C56 . H561 . 0.960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 79.05(9) yes N1 . Ru1 . N3 . 158.02(9) yes N2 . Ru1 . N3 . 79.01(9) yes N1 . Ru1 . N4 . 91.26(9) yes N2 . Ru1 . N4 . 100.87(9) yes N3 . Ru1 . N4 . 91.40(8) yes N1 . Ru1 . N5 . 102.57(9) yes N2 . Ru1 . N5 . 178.37(10) yes N3 . Ru1 . N5 . 99.36(9) yes N4 . Ru1 . N5 . 79.11(9) yes N1 . Ru1 . N6 . 89.93(9) yes N2 . Ru1 . N6 . 101.29(9) yes N3 . Ru1 . N6 . 95.80(9) yes N4 . Ru1 . N6 . 157.63(9) yes N5 . Ru1 . N6 . 78.83(9) yes Ru1 . N1 . C1 . 127.1(2) yes Ru1 . N1 . C5 . 114.25(18) yes C1 . N1 . C5 . 118.7(3) yes Ru1 . N2 . C6 . 119.70(18) yes Ru1 . N2 . C10 . 119.38(18) yes C6 . N2 . C10 . 120.9(2) yes Ru1 . N3 . C11 . 113.75(18) yes Ru1 . N3 . C15 . 127.92(18) yes C11 . N3 . C15 . 118.2(2) yes Ru1 . N4 . C16 . 127.48(18) yes Ru1 . N4 . C20 . 113.61(18) yes C16 . N4 . C20 . 118.9(2) yes Ru1 . N5 . C21 . 119.22(19) yes Ru1 . N5 . C25 . 119.62(18) yes C21 . N5 . C25 . 121.1(2) yes Ru1 . N6 . C26 . 114.17(17) yes Ru1 . N6 . C30 . 127.2(2) yes C26 . N6 . C30 . 118.3(3) yes N1 . C1 . C2 . 121.9(3) yes N1 . C1 . H11 . 119.0 no C2 . C1 . H11 . 119.1 no C1 . C2 . C3 . 118.9(3) yes C1 . C2 . H21 . 120.5 no C3 . C2 . H21 . 120.6 no C2 . C3 . C4 . 119.7(3) yes C2 . C3 . H31 . 120.3 no C4 . C3 . H31 . 120.0 no C3 . C4 . C5 . 119.2(3) yes C3 . C4 . H41 . 120.0 no C5 . C4 . H41 . 120.8 no C4 . C5 . N1 . 121.5(3) yes C4 . C5 . C6 . 123.6(3) yes N1 . C5 . C6 . 114.8(2) yes C5 . C6 . N2 . 112.1(2) yes C5 . C6 . C7 . 127.1(3) yes N2 . C6 . C7 . 120.8(3) yes C6 . C7 . C8 . 119.1(3) yes C6 . C7 . H71 . 120.5 no C8 . C7 . H71 . 120.4 no C7 . C8 . C9 . 119.1(3) yes C7 . C8 . C31 . 120.9(3) yes C9 . C8 . C31 . 120.0(3) yes C8 . C9 . C10 . 119.5(3) yes C8 . C9 . H91 . 120.9 no C10 . C9 . H91 . 119.6 no C9 . C10 . N2 . 120.4(3) yes C9 . C10 . C11 . 127.0(3) yes N2 . C10 . C11 . 112.6(2) yes C10 . C11 . N3 . 115.1(2) yes C10 . C11 . C12 . 123.6(2) yes N3 . C11 . C12 . 121.2(3) yes C11 . C12 . C13 . 119.6(3) yes C11 . C12 . H121 . 119.3 no C13 . C12 . H121 . 121.1 no C12 . C13 . C14 . 118.9(3) yes C12 . C13 . H131 . 120.7 no C14 . C13 . H131 . 120.4 no C13 . C14 . C15 . 119.7(3) yes C13 . C14 . H141 . 121.0 no C15 . C14 . H141 . 119.3 no C14 . C15 . N3 . 122.3(3) yes C14 . C15 . H151 . 119.3 no N3 . C15 . H151 . 118.4 no N4 . C16 . C17 . 122.4(3) yes N4 . C16 . H161 . 117.4 no C17 . C16 . H161 . 120.2 no C16 . C17 . C18 . 119.1(3) yes C16 . C17 . H171 . 120.2 no C18 . C17 . H171 . 120.7 no C17 . C18 . C19 . 119.4(3) yes C17 . C18 . H181 . 120.8 no C19 . C18 . H181 . 119.8 no C18 . C19 . C20 . 119.9(3) yes C18 . C19 . H191 . 120.5 no C20 . C19 . H191 . 119.6 no C19 . C20 . N4 . 120.4(3) yes C19 . C20 . C21 . 124.3(2) yes N4 . C20 . C21 . 115.3(2) yes C20 . C21 . N5 . 112.7(2) yes C20 . C21 . C22 . 127.1(2) yes N5 . C21 . C22 . 120.2(3) yes C21 . C22 . C23 . 120.0(3) yes C21 . C22 . H221 . 119.5 no C23 . C22 . H221 . 120.5 no C22 . C23 . C24 . 118.4(3) yes C22 . C23 . C37 . 121.9(3) yes C24 . C23 . C37 . 119.7(3) yes C23 . C24 . C25 . 119.7(3) yes C23 . C24 . H241 . 120.4 no C25 . C24 . H241 . 119.9 no C24 . C25 . N5 . 120.6(3) yes C24 . C25 . C26 . 127.3(3) yes N5 . C25 . C26 . 112.1(2) yes C25 . C26 . N6 . 115.0(3) yes C25 . C26 . C27 . 123.5(3) yes N6 . C26 . C27 . 121.3(3) yes C26 . C27 . C28 . 119.4(3) yes C26 . C27 . H271 . 119.5 no C28 . C27 . H271 . 121.2 no C27 . C28 . C29 . 119.5(3) yes C27 . C28 . H281 . 119.7 no C29 . C28 . H281 . 120.7 no C28 . C29 . C30 . 119.7(3) yes C28 . C29 . H291 . 121.4 no C30 . C29 . H291 . 118.9 no C29 . C30 . N6 . 121.8(3) yes C29 . C30 . H301 . 119.8 no N6 . C30 . H301 . 118.5 no C8 . C31 . S1 . 127.5(3) yes C8 . C31 . C32 . 129.5(3) yes S1 . C31 . C32 . 103.0(2) yes C8 . C31 . C52 . 120.2(3) yes C32 . C31 . C52 . 110.4(2) yes C8 . C31 . S10 . 131.7(3) yes C52 . C31 . S10 . 107.9(2) yes C31 . S1 . C34 . 93.87(18) yes C31 . C32 . C33 . 127.9(3) yes C31 . C32 . H321 . 116.2 no C33 . C32 . H321 . 116.0 no C32 . C33 . C34 . 102.4(3) yes C32 . C33 . H331 . 128.5 no C34 . C33 . H331 . 129.1 no S1 . C34 . C33 . 112.9(3) yes S1 . C34 . C35 . 120.8(3) yes C33 . C34 . C35 . 126.2(4) yes C34 . C35 . C36 . 178.9(5) yes C35 . C36 . H361 . 179.9 no C23 . C37 . C38 . 129.2(3) yes C23 . C37 . S2 . 121.6(2) yes C38 . C37 . S2 . 109.3(2) yes C37 . C38 . C39 . 114.1(3) yes C37 . C38 . H381 . 122.5 no C39 . C38 . H381 . 123.4 no C38 . C39 . C40 . 113.2(3) yes C38 . C39 . H391 . 124.0 no C40 . C39 . H391 . 122.7 no C39 . C40 . C41 . 128.0(3) yes C39 . C40 . S2 . 111.2(2) yes C41 . C40 . S2 . 120.8(3) yes C40 . C41 . C42 . 177.7(4) yes C41 . C42 . H421 . 173.0 no C44 . C43 . H431 . 110.9 no C44 . C43 . H432 . 110.7 no H431 . C43 . H432 . 108.3 no C44 . C43 . H433 . 109.5 no H431 . C43 . H433 . 109.5 no H432 . C43 . H433 . 107.8 no C43 . C44 . N7 . 178.5(5) yes C40 . S2 . C37 . 92.19(16) yes F1 . P1 . F2 . 177.7(2) yes F1 . P1 . F3 . 88.46(15) yes F2 . P1 . F3 . 90.84(14) yes F1 . P1 . F4 . 90.77(16) yes F2 . P1 . F4 . 89.92(15) yes F3 . P1 . F4 . 179.22(15) yes F1 . P1 . F5 . 89.15(17) yes F2 . P1 . F5 . 88.73(16) yes F3 . P1 . F5 . 91.72(14) yes F4 . P1 . F5 . 88.12(14) yes F1 . P1 . F6 . 90.0(2) yes F2 . P1 . F6 . 92.15(18) yes F3 . P1 . F6 . 88.61(15) yes F4 . P1 . F6 . 91.54(15) yes F5 . P1 . F6 . 179.06(19) yes F13 2_566 P2 . F15 2_566 90.22(13) yes F13 2_566 P2 . F11 2_566 89.70(12) yes F15 2_566 P2 . F11 2_566 90.54(12) yes F13 2_566 P2 . F11 . 90.30(12) yes F15 2_566 P2 . F11 . 89.46(12) yes F11 2_566 P2 . F11 . 179.993 yes F13 2_566 P2 . F13 . 179.993 yes F15 2_566 P2 . F13 . 89.78(13) yes F11 2_566 P2 . F13 . 90.30(12) yes F11 . P2 . F13 . 89.70(12) yes F13 2_566 P2 . F15 . 89.78(13) yes F15 2_566 P2 . F15 . 179.993 yes F11 2_566 P2 . F15 . 89.46(12) yes F11 . P2 . F15 . 90.54(12) yes F13 . P2 . F15 . 90.22(13) yes F23 2_656 P3 . F21 2_656 84.3(4) yes F21 2_656 P3 . F33 2_656 97.3(4) yes F23 2_656 P3 . F25 2_656 85.4(6) yes F21 2_656 P3 . F25 2_656 96.0(6) yes F33 2_656 P3 . F25 2_656 122.3(6) yes F23 2_656 P3 . F21 . 95.7(4) yes F21 2_656 P3 . F21 . 179.993 yes F33 2_656 P3 . F21 . 82.7(4) yes F25 2_656 P3 . F21 . 84.0(6) yes F31 2_656 P3 . F21 . 154.0(8) yes F23 2_656 P3 . F23 . 179.993 yes F21 2_656 P3 . F23 . 95.7(4) yes F25 2_656 P3 . F23 . 94.6(6) yes F23 2_656 P3 . F25 . 94.6(6) yes F21 2_656 P3 . F25 . 84.0(6) yes F25 2_656 P3 . F25 . 179.993 yes F31 2_656 P3 . F25 . 81.7(10) yes F21 . P3 . F23 . 84.3(4) yes F21 . P3 . F25 . 96.0(6) yes F23 . P3 . F25 . 85.4(6) yes F31 . P4 . F32 . 176.3(10) yes F31 . P4 . F33 . 91.6(7) yes F31 . P4 . F34 . 92.8(8) yes F31 . P4 . F35 . 87.5(8) yes F31 . P4 . F36 . 87.9(8) yes F32 . P4 . F33 . 86.2(6) yes F32 . P4 . F34 . 89.6(7) yes F33 . P4 . F34 . 174.5(8) yes F32 . P4 . F35 . 95.4(8) yes F33 . P4 . F35 . 87.8(6) yes F34 . P4 . F35 . 89.1(8) yes F32 . P4 . F36 . 89.1(8) yes F33 . P4 . F36 . 89.3(7) yes F34 . P4 . F36 . 94.1(8) yes F35 . P4 . F36 . 174.5(9) yes C31 . C52 . C53 . 126.4(6) yes C31 . C52 . H521 . 117.1 no C53 . C52 . H521 . 116.5 no C31 . S10 . C54 . 90.6(5) yes C52 . C53 . C54 . 94.9(10) yes C52 . C53 . H531 . 132.7 no C54 . C53 . H531 . 132.4 no S10 . C54 . C53 . 119.9(9) yes S10 . C54 . C55 . 121.6(11) yes C53 . C54 . C55 . 117.5(10) yes C54 . C55 . C56 . 171.7(17) yes C55 . C56 . H561 . 179.2 no