# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_coden_Cambridge 440 _publ_requested_journal NJC loop_ _publ_author_name _publ_author_address _publ_author_footnote J.P.Majoral ; Departamento de Qu\'imica Org\'anica e Inorg\'anica, Instituto Universitario de Qu\'imica Organomet\'alica ?Enrique Moles? (Unidad Asociada al CSIC), Facultad de Qu\'imica, Universidad de Oviedo, E-33071 Oviedo, Spain ; ; ? # Footnote for author 1 ; 'Victorio Cadierno' ; Departamento de Qu\'imica Org\'anica e Inorg\'anica, Instituto Universitario de Qu\'imica Organomet\'alica "Enrique Moles" (Unidad Asociada al CSIC), Facultad de Qu\'imica, Universidad de Oviedo, E-33071 Oviedo, Spain ; ; ? # Footnote 2 ; 'Pascale Crochet' ; Centre of Molecular and Macromolecular Studies, The Polish Academy of Sciences, Sienkiewicza 112, 90363 \/L\'od\'z, Poland ; ; ? # Footnote 2 ; 'Alba E. Diaz-Alvarez' ; Departamento de Qu\'imica Org\'anica e Inorg\'anica, Instituto Universitario de Qu\'imica Organomet\'alica "Enrique Moles" (Unidad Asociada al CSIC), Facultad de Qu\'imica, Universidad de Oviedo, E-33071 Oviedo, Spain ; ; ? # Footnote 2 ; 'Carine Duhayon' ; Laboratoire de Chimie de Coordination CNRS, UPR 8241, 205 route de Narbonne, 31077 Toulouse cedex 4, France ; ; ? # Footnote 2 ; J.Gimeno ; Departamento de Qu\'imica Org\'anica e Inorg\'anica, Instituto Universitario de Qu\'imica Organomet\'alica "Enrique Moles" (Unidad Asociada al CSIC), Facultad de Qu\'imica, Universidad de Oviedo, E-33071 Oviedo, Spain ; ; ? # Footnote 2 ; 'Maria Zablocka' ; Laboratoire de Chimie de Coordination CNRS, UPR 8241, 205 route de Narbonne, 31077 Toulouse cedex 4, France ; ; ? # Footnote 2 ; _publ_contact_author_name J.P.Majoral _publ_contact_author_address ; Laboratoire de Chimie de Coodination du CNRS 205,route de Narbonne, 31077 Toulouse Cedex France ; _publ_contact_author_email MAJORAL@LCC-TOULOUSE.FR _publ_section_title ; Imination reactions of free and coordinated 2-diphenylphosphino-1-phenyl-phospholane: Access to regioisomeric ruthenium(II) complexes containing novel iminophosphorane-phosphine ligands ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_name_full ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? _publ_contact_author_fax '+(33) 561553003' _publ_contact_author_phone '+(33) 561333123' _publ_requested_category CO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name ? # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; ; # Attachment 'B606781F_CIFs.doc' data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 612113' _audit_creation_date 04-11-04 _audit_creation_method CRYSTALS_ver_12.24 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 22.247(4) _cell_length_b 10.040(2) _cell_length_c 20.632(4) _cell_angle_alpha 90 _cell_angle_beta 95.89(3) _cell_angle_gamma 90 _cell_volume 4584.0(16) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? 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' 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' 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' 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' _cell_formula_units_Z 4 _chemical_formula_sum 'C45 H47 Cl5 N1 O3 P3 Ru1' _chemical_formula_moiety 'C44 H46 Cl2 N O3 P3 Ru, C H Cl3 ' _chemical_compound_source ? _chemical_formula_weight 1021.07 _cell_measurement_reflns_used 5837 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 26.6 _cell_measurement_temperature 180 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2088.001 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.93 # Sheldrick geometric definitions 0.86 0.93 _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'Xcalibur, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _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 180 _diffrn_reflns_number 34425 _reflns_number_total 9554 _diffrn_reflns_av_R_equivalents 0.036 # Number of reflections with Friedels Law is 9554 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9566 _diffrn_reflns_theta_min 2.739 _diffrn_reflns_theta_max 26.578 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.578 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -27 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.57 _refine_diff_density_max 0.70 _refine_ls_number_reflns 4376 _refine_ls_number_restraints 6 _refine_ls_number_parameters 404 #_refine_ls_R_factor_ref 0.0417 _refine_ls_wR_factor_ref 0.0493 _refine_ls_goodness_of_fit_ref 1.1191 #_reflns_number_all 9532 _refine_ls_R_factor_all 0.0884 _refine_ls_wR_factor_all 0.0519 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.50u(I) _reflns_number_gt 4376 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_gt 0.0493 _refine_ls_shift/su_max 0.018222 # 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 refU # 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: 1.77 -0.138 1.28 ; _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen ; H atoms placed geometrically after each cycle 3 disordered phenyl rings ; _publ_section_exptl_prep ; ? ; # 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) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Oxford Diffraction, (2002) CrysAlis RED. Oxford Diffraction, (2002) Xcalibur User Manual 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 atoms attached 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 0.375695(19) 0.49468(5) 0.45160(2) 0.0225 1.0000 Uani . . . . . . P1 P 0.27035(6) 0.51809(15) 0.45172(7) 0.0240 1.0000 Uani . . . . . . P2 P 0.17683(8) 0.5515(2) 0.56331(8) 0.0436 1.0000 Uani D . . . . . P3 P 0.14837(9) 0.3727(2) 0.66247(8) 0.0455 1.0000 Uani . . . . . . N1 N 0.1893(3) 0.4299(6) 0.6112(3) 0.0410 1.0000 Uani . . . . . . O1 O 0.1040(2) 0.4539(6) 0.6912(2) 0.0619 1.0000 Uani . . . . . . O2 O 0.1213(3) 0.2428(6) 0.6264(2) 0.0626 1.0000 Uani D . . . . . O3 O 0.1927(2) 0.3155(5) 0.7207(2) 0.0496 1.0000 Uani D . . . . . C1 C 0.2336(3) 0.6199(6) 0.3853(3) 0.0274 1.0000 Uani . . . . . . C2 C 0.2654(3) 0.7293(6) 0.3653(3) 0.0339 1.0000 Uani . . . . . . C3 C 0.2378(3) 0.8201(6) 0.3205(3) 0.0383 1.0000 Uani . . . . . . C4 C 0.1786(3) 0.8016(7) 0.2955(3) 0.0450 1.0000 Uani . . . . . . C5 C 0.1467(3) 0.6930(8) 0.3145(3) 0.0485 1.0000 Uani . . . . . . C6 C 0.1732(3) 0.6024(7) 0.3598(3) 0.0374 1.0000 Uani . . . . . . C7 C 0.2363(3) 0.3534(6) 0.4450(3) 0.0289 1.0000 Uani . . . . . . C8 C 0.2112(3) 0.2994(7) 0.3859(3) 0.0355 1.0000 Uani . . . . . . C9 C 0.1905(4) 0.1695(7) 0.3825(4) 0.0485 1.0000 Uani . . . . . . C10 C 0.1961(4) 0.0905(8) 0.4383(4) 0.0598 1.0000 Uani . . . . . . C11 C 0.2210(4) 0.1407(7) 0.4961(4) 0.0524 1.0000 Uani . . . . . . C12 C 0.2421(3) 0.2714(6) 0.5006(3) 0.0350 1.0000 Uani . . . . . . C13 C 0.2452(3) 0.5983(6) 0.5264(3) 0.0320 1.0000 Uani . . . . . . C14 C 0.2388(3) 0.7508(7) 0.5204(4) 0.0468 1.0000 Uani . . . . . . C15 C 0.2162(4) 0.8014(8) 0.5817(4) 0.0625 1.0000 Uani . . . . . . C16 C 0.1680(5) 0.7099(9) 0.6028(5) 0.0845 1.0000 Uani . . . . . . C35 C 0.3949(3) 0.2982(6) 0.4089(3) 0.0319 1.0000 Uani . . . . . . C36 C 0.4509(3) 0.3534(6) 0.4361(3) 0.0301 1.0000 Uani . . . . . . C37 C 0.4695(3) 0.4808(6) 0.4203(3) 0.0316 1.0000 Uani . . . . . . C38 C 0.4333(3) 0.5619(6) 0.3755(3) 0.0322 1.0000 Uani . . . . . . C39 C 0.3791(3) 0.5094(8) 0.3457(2) 0.0360 1.0000 Uani . . . . . . C40 C 0.3600(3) 0.3792(6) 0.3626(3) 0.0338 1.0000 Uani . . . . . . C41 C 0.3744(3) 0.1592(7) 0.4232(4) 0.0487 1.0000 Uani . . . . . . C42 C 0.3832(5) 0.0678(9) 0.3661(5) 0.0764 1.0000 Uani . . . . . . C43 C 0.4047(7) 0.1015(9) 0.4845(5) 0.0985 1.0000 Uani . . . . . . C44 C 0.4534(4) 0.7004(7) 0.3610(3) 0.0491 1.0000 Uani . . . . . . C45 C 0.4207(3) 0.6588(7) 0.6742(3) 0.0410 1.0000 Uani . . . . . . Cl1 Cl 0.38992(7) 0.71192(14) 0.50097(7) 0.0316 1.0000 Uani . . . . . . Cl2 Cl 0.37492(7) 0.41488(14) 0.56159(7) 0.0300 1.0000 Uani . . . . . . Cl3 Cl 0.45638(10) 0.8134(2) 0.67126(11) 0.0668 1.0000 Uani . . . . . . Cl4 Cl 0.34932(9) 0.6751(2) 0.70307(11) 0.0574 1.0000 Uani . . . . . . Cl5 Cl 0.46527(11) 0.5498(3) 0.72483(10) 0.0758 1.0000 Uani . . . . . . C17 C 0.1136(3) 0.5552(9) 0.5046(4) 0.0437(14) 0.5000 Uiso DG . . . . . C18 C 0.0840(4) 0.6675(7) 0.4780(4) 0.0437(14) 0.5000 Uiso G . . . . . C19 C 0.0361(4) 0.6539(7) 0.4296(4) 0.0437(14) 0.5000 Uiso G . . . . . C20 C 0.0177(3) 0.5278(9) 0.4079(4) 0.0437(14) 0.5000 Uiso G . . . . . C21 C 0.0473(4) 0.4154(7) 0.4345(4) 0.0437(14) 0.5000 Uiso G . . . . . C22 C 0.0952(4) 0.4291(8) 0.4828(4) 0.0437(14) 0.5000 Uiso G . . . . . C23 C 0.0794(5) 0.1471(11) 0.6406(6) 0.089(2) 0.6000 Uiso DG . . . . . C24 C 0.0588(5) 0.0587(12) 0.5914(5) 0.089(2) 0.6000 Uiso G . . . . . C25 C 0.0125(5) -0.0299(11) 0.6009(5) 0.089(2) 0.6000 Uiso G . . . . . C26 C -0.0133(4) -0.0300(11) 0.6595(6) 0.089(2) 0.6000 Uiso G . . . . . C27 C 0.0073(5) 0.0584(13) 0.7087(5) 0.089(2) 0.6000 Uiso G . . . . . C28 C 0.0537(6) 0.1470(11) 0.6992(6) 0.089(2) 0.6000 Uiso G . . . . . C29 C 0.2381(3) 0.2288(6) 0.7092(4) 0.0543(11) 0.7000 Uiso DG . . . . . C30 C 0.2928(3) 0.2729(5) 0.6900(4) 0.0543(11) 0.7000 Uiso G . . . . . C31 C 0.3377(2) 0.1815(7) 0.6793(4) 0.0543(11) 0.7000 Uiso G . . . . . C32 C 0.3278(3) 0.0462(6) 0.6876(4) 0.0543(11) 0.7000 Uiso G . . . . . C33 C 0.2731(3) 0.0022(5) 0.7067(4) 0.0543(11) 0.7000 Uiso G . . . . . C34 C 0.2282(2) 0.0935(7) 0.7175(4) 0.0543(11) 0.7000 Uiso G . . . . . C171 C 0.1143(4) 0.5043(10) 0.5022(4) 0.0532(17) 0.5000 Uiso DG . . . . . C181 C 0.0804(4) 0.6043(8) 0.4694(5) 0.0532(17) 0.5000 Uiso G . . . . . C191 C 0.0340(4) 0.5716(9) 0.4217(5) 0.0532(17) 0.5000 Uiso G . . . . . C201 C 0.0216(4) 0.4388(11) 0.4067(4) 0.0532(17) 0.5000 Uiso G . . . . . C211 C 0.0556(5) 0.3387(8) 0.4395(5) 0.0532(17) 0.5000 Uiso G . . . . . C221 C 0.1020(4) 0.3714(9) 0.4872(5) 0.0532(17) 0.5000 Uiso G . . . . . C231 C 0.0788(7) 0.1671(16) 0.6573(9) 0.088(3) 0.4000 Uiso DG . . . . . C241 C 0.0751(8) 0.0375(18) 0.6334(8) 0.088(3) 0.4000 Uiso G . . . . . C251 C 0.0383(8) -0.0550(13) 0.6602(9) 0.088(3) 0.4000 Uiso G . . . . . C261 C 0.0051(7) -0.0180(15) 0.7109(9) 0.088(3) 0.4000 Uiso G . . . . . C271 C 0.0088(7) 0.1116(17) 0.7347(8) 0.088(3) 0.4000 Uiso G . . . . . C281 C 0.0456(8) 0.2041(13) 0.7079(9) 0.088(3) 0.4000 Uiso G . . . . . C291 C 0.2455(5) 0.2425(15) 0.7088(10) 0.052(3) 0.3000 Uiso DG . . . . . C301 C 0.2982(7) 0.3176(11) 0.7118(9) 0.052(3) 0.3000 Uiso G . . . . . C311 C 0.3528(5) 0.2567(15) 0.7027(9) 0.052(3) 0.3000 Uiso G . . . . . C321 C 0.3547(4) 0.1206(15) 0.6906(9) 0.052(3) 0.3000 Uiso G . . . . . C331 C 0.3020(6) 0.0455(11) 0.6876(9) 0.052(3) 0.3000 Uiso G . . . . . C341 C 0.2474(5) 0.1064(15) 0.6967(9) 0.052(3) 0.3000 Uiso G . . . . . H21 H 0.3085 0.7429 0.3833 0.080(4) 1.0000 Uiso . . . . . . H31 H 0.2610 0.8985 0.3065 0.080(4) 1.0000 Uiso . . . . . . H41 H 0.1587 0.8668 0.2635 0.080(4) 1.0000 Uiso . . . . . . H51 H 0.1039 0.6793 0.2955 0.080(4) 1.0000 Uiso . . . . . . H61 H 0.1493 0.5253 0.3742 0.080(4) 1.0000 Uiso . . . . . . H81 H 0.2081 0.3556 0.3456 0.080(4) 1.0000 Uiso . . . . . . H91 H 0.1717 0.1325 0.3401 0.080(4) 1.0000 Uiso . . . . . . H101 H 0.1814 -0.0038 0.4358 0.080(4) 1.0000 Uiso . . . . . . H111 H 0.2244 0.0831 0.5359 0.080(4) 1.0000 Uiso . . . . . . H121 H 0.2611 0.3069 0.5432 0.080(4) 1.0000 Uiso . . . . . . H131 H 0.2792 0.5836 0.5613 0.080(4) 1.0000 Uiso . . . . . . H141 H 0.2790 0.7915 0.5149 0.080(4) 1.0000 Uiso . . . . . . H142 H 0.2095 0.7738 0.4821 0.080(4) 1.0000 Uiso . . . . . . H151 H 0.2506 0.8060 0.6169 0.080(4) 1.0000 Uiso . . . . . . H152 H 0.1989 0.8926 0.5737 0.080(4) 1.0000 Uiso . . . . . . H161 H 0.1732 0.6988 0.6512 0.080(4) 1.0000 Uiso . . . . . . H162 H 0.1270 0.7476 0.5892 0.080(4) 1.0000 Uiso . . . . . . H181 H 0.0970 0.7582 0.4935 0.080(4) 0.5000 Uiso . . . . . . H191 H 0.0147 0.7346 0.4103 0.080(4) 0.5000 Uiso . . . . . . H201 H -0.0169 0.5178 0.3729 0.080(4) 0.5000 Uiso . . . . . . H211 H 0.0340 0.3247 0.4186 0.080(4) 0.5000 Uiso . . . . . . H221 H 0.1163 0.3482 0.5018 0.080(4) 0.5000 Uiso . . . . . . H241 H 0.0773 0.0587 0.5492 0.080(4) 0.6000 Uiso . . . . . . H251 H -0.0024 -0.0935 0.5655 0.080(4) 0.6000 Uiso . . . . . . H261 H -0.0466 -0.0937 0.6663 0.080(4) 0.6000 Uiso . . . . . . H271 H -0.0111 0.0582 0.7509 0.080(4) 0.6000 Uiso . . . . . . H281 H 0.0686 0.2104 0.7346 0.080(4) 0.6000 Uiso . . . . . . H301 H 0.3000 0.3703 0.6843 0.080(4) 0.7000 Uiso . . . . . . H311 H 0.3771 0.2133 0.6658 0.080(4) 0.7000 Uiso . . . . . . H321 H 0.3601 -0.0194 0.6800 0.080(4) 0.7000 Uiso . . . . . . H331 H 0.2659 -0.0952 0.7126 0.080(4) 0.7000 Uiso . . . . . . H341 H 0.1888 0.0618 0.7311 0.080(4) 0.7000 Uiso . . . . . . H361 H 0.4778 0.2987 0.4676 0.080(4) 1.0000 Uiso . . . . . . H371 H 0.5090 0.5157 0.4408 0.080(4) 1.0000 Uiso . . . . . . H391 H 0.3537 0.5632 0.3125 0.080(4) 1.0000 Uiso . . . . . . H401 H 0.3209 0.3437 0.3412 0.080(4) 1.0000 Uiso . . . . . . H411 H 0.3300 0.1632 0.4276 0.080(4) 1.0000 Uiso . . . . . . H421 H 0.3694 -0.0241 0.3760 0.080(4) 1.0000 Uiso . . . . . . H422 H 0.4269 0.0658 0.3589 0.080(4) 1.0000 Uiso . . . . . . H423 H 0.3589 0.1019 0.3260 0.080(4) 1.0000 Uiso . . . . . . H431 H 0.3987 0.1619 0.5218 0.080(4) 1.0000 Uiso . . . . . . H432 H 0.4488 0.0913 0.4805 0.080(4) 1.0000 Uiso . . . . . . H433 H 0.3868 0.0121 0.4923 0.080(4) 1.0000 Uiso . . . . . . H441 H 0.4227 0.7430 0.3286 0.080(4) 1.0000 Uiso . . . . . . H442 H 0.4576 0.7540 0.4020 0.080(4) 1.0000 Uiso . . . . . . H443 H 0.4932 0.6965 0.3425 0.080(4) 1.0000 Uiso . . . . . . H451 H 0.4152 0.6206 0.6293 0.080(4) 1.0000 Uiso . . . . . . H1811 H 0.0891 0.6997 0.4801 0.080(4) 0.5000 Uiso . . . . . . H1911 H 0.0094 0.6434 0.3980 0.080(4) 0.5000 Uiso . . . . . . H2011 H -0.0118 0.4150 0.3723 0.080(4) 0.5000 Uiso . . . . . . H2111 H 0.0466 0.2429 0.4286 0.080(4) 0.5000 Uiso . . . . . . H2211 H 0.1263 0.2992 0.5106 0.080(4) 0.5000 Uiso . . . . . . H2411 H 0.0985 0.0097 0.5975 0.080(4) 0.4000 Uiso . . . . . . H2511 H 0.0354 -0.1494 0.6439 0.080(4) 0.4000 Uiso . . . . . . H2611 H -0.0217 -0.0854 0.7308 0.080(4) 0.4000 Uiso . . . . . . H2711 H -0.0157 0.1377 0.7714 0.080(4) 0.4000 Uiso . . . . . . H2811 H 0.0474 0.2968 0.7250 0.080(4) 0.4000 Uiso . . . . . . H3011 H 0.2967 0.4152 0.7200 0.080(4) 0.3000 Uiso . . . . . . H3111 H 0.3909 0.3107 0.7049 0.080(4) 0.3000 Uiso . . . . . . H3211 H 0.3944 0.0769 0.6839 0.080(4) 0.3000 Uiso . . . . . . H3311 H 0.3039 -0.0527 0.6785 0.080(4) 0.3000 Uiso . . . . . . H3411 H 0.2116 0.0463 0.6927 0.080(4) 0.3000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02333(19) 0.0232(2) 0.02108(18) 0.0015(2) 0.00351(13) 0.0025(2) P1 0.0237(7) 0.0255(8) 0.0235(6) 0.0031(6) 0.0049(5) 0.0011(6) P2 0.0451(10) 0.0523(10) 0.0366(10) 0.0122(8) 0.0200(8) 0.0154(8) P3 0.0503(11) 0.0568(12) 0.0300(9) 0.0006(8) 0.0076(8) -0.0116(9) N1 0.048(3) 0.045(3) 0.031(3) 0.008(3) 0.010(2) 0.004(3) O1 0.049(3) 0.094(4) 0.046(3) -0.004(3) 0.020(2) -0.001(3) O2 0.077(4) 0.065(4) 0.044(3) 0.003(3) 0.001(3) -0.032(3) O3 0.062(3) 0.064(3) 0.023(2) 0.001(2) 0.005(2) -0.011(3) C1 0.028(3) 0.031(3) 0.024(3) 0.004(2) 0.006(2) 0.007(2) C2 0.034(3) 0.031(3) 0.038(3) 0.006(3) 0.009(3) 0.007(3) C3 0.051(4) 0.032(3) 0.034(3) 0.010(3) 0.014(3) 0.009(3) C4 0.053(4) 0.047(4) 0.036(4) 0.015(3) 0.007(3) 0.020(3) C5 0.036(4) 0.068(5) 0.040(4) 0.010(4) -0.006(3) 0.017(4) C6 0.031(3) 0.050(4) 0.032(3) 0.004(3) 0.009(3) 0.005(3) C7 0.029(3) 0.024(3) 0.035(3) 0.000(2) 0.011(3) -0.002(2) C8 0.034(3) 0.038(4) 0.035(3) -0.001(3) 0.004(3) -0.009(3) C9 0.059(5) 0.043(4) 0.045(4) -0.012(3) 0.012(3) -0.019(4) C10 0.084(6) 0.041(4) 0.057(5) -0.004(4) 0.017(4) -0.023(4) C11 0.071(5) 0.040(4) 0.048(4) 0.010(3) 0.012(4) -0.013(4) C12 0.041(4) 0.032(3) 0.033(3) 0.002(3) 0.005(3) -0.007(3) C13 0.039(3) 0.027(3) 0.030(3) 0.003(3) 0.006(3) 0.005(3) C14 0.048(4) 0.037(4) 0.059(5) -0.003(3) 0.020(4) 0.003(3) C15 0.081(6) 0.049(5) 0.059(5) -0.015(4) 0.017(4) 0.024(4) C16 0.132(9) 0.056(5) 0.077(6) 0.019(5) 0.066(6) 0.044(6) C35 0.035(3) 0.028(3) 0.035(3) -0.012(3) 0.016(3) 0.000(3) C36 0.027(3) 0.037(3) 0.026(3) 0.000(3) 0.003(2) 0.010(3) C37 0.026(3) 0.035(4) 0.036(3) -0.001(3) 0.012(2) 0.003(3) C38 0.039(4) 0.037(3) 0.023(3) 0.002(3) 0.012(3) 0.006(3) C39 0.036(3) 0.058(4) 0.015(2) 0.001(3) 0.005(2) 0.015(4) C40 0.027(3) 0.042(4) 0.032(3) -0.015(3) 0.004(2) 0.005(3) C41 0.052(4) 0.030(4) 0.067(5) -0.005(3) 0.023(4) 0.001(3) C42 0.092(7) 0.043(5) 0.098(7) -0.032(5) 0.031(6) -0.017(5) C43 0.189(13) 0.027(4) 0.080(7) 0.004(5) 0.018(7) 0.000(6) C44 0.072(5) 0.042(4) 0.038(4) 0.012(3) 0.027(4) -0.005(4) C45 0.046(4) 0.043(4) 0.034(3) -0.001(3) 0.005(3) 0.010(3) Cl1 0.0354(8) 0.0251(7) 0.0345(8) -0.0026(6) 0.0052(6) -0.0028(6) Cl2 0.0341(8) 0.0310(8) 0.0249(7) 0.0041(6) 0.0034(5) 0.0009(6) Cl3 0.0688(14) 0.0606(13) 0.0736(14) -0.0221(11) 0.0199(11) -0.0201(11) Cl4 0.0496(11) 0.0548(11) 0.0694(13) -0.0036(10) 0.0136(9) 0.0061(9) Cl5 0.0919(16) 0.0965(17) 0.0414(10) 0.0098(10) 0.0182(10) 0.0546(14) _refine_ls_extinction_method None 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 . P1 . 2.3556(15) yes Ru1 . C35 . 2.219(6) yes Ru1 . C36 . 2.242(6) yes Ru1 . C37 . 2.251(5) yes Ru1 . C38 . 2.231(6) yes Ru1 . C39 . 2.199(5) yes Ru1 . C40 . 2.170(6) yes Ru1 . Cl1 . 2.4142(16) yes Ru1 . Cl2 . 2.4083(15) yes P1 . C1 . 1.833(6) yes P1 . C7 . 1.818(6) yes P1 . C13 . 1.875(6) yes P2 . N1 . 1.577(6) yes P2 . C13 . 1.830(6) yes P2 . C16 . 1.808(9) yes P2 . C17 . 1.761(4) yes P2 . C171 . 1.841(4) yes P3 . N1 . 1.573(5) yes P3 . O1 . 1.452(6) yes P3 . O2 . 1.589(5) yes P3 . O3 . 1.582(5) yes O2 . C23 . 1.391(5) yes O2 . C231 . 1.415(5) yes O3 . C29 . 1.372(4) yes O3 . C291 . 1.427(5) yes C1 . C2 . 1.392(8) yes C1 . C6 . 1.403(8) yes C2 . C3 . 1.395(9) yes C2 . H21 . 1.001 no C3 . C4 . 1.377(10) yes C3 . H31 . 1.001 no C4 . C5 . 1.379(11) yes C4 . H41 . 1.000 no C5 . C6 . 1.392(9) yes C5 . H51 . 1.000 no C6 . H61 . 1.000 no C7 . C8 . 1.397(9) yes C7 . C12 . 1.407(9) yes C8 . C9 . 1.382(9) yes C8 . H81 . 1.001 no C9 . C10 . 1.393(11) yes C9 . H91 . 1.001 no C10 . C11 . 1.360(11) yes C10 . H101 . 1.001 no C11 . C12 . 1.392(9) yes C11 . H111 . 1.001 no C12 . H121 . 1.001 no C13 . C14 . 1.541(9) yes C13 . H131 . 1.001 no C14 . C15 . 1.497(10) yes C14 . H141 . 1.000 no C14 . H142 . 1.000 no C15 . C16 . 1.509(14) yes C15 . H151 . 1.001 no C15 . H152 . 1.000 no C16 . H161 . 1.000 no C16 . H162 . 1.001 no C35 . C36 . 1.424(8) yes C35 . C40 . 1.423(9) yes C35 . C41 . 1.508(9) yes C36 . C37 . 1.394(9) yes C36 . H361 . 1.001 no C37 . C38 . 1.418(8) yes C37 . H371 . 1.000 no C38 . C39 . 1.400(9) yes C38 . C44 . 1.501(9) yes C39 . C40 . 1.429(10) yes C39 . H391 . 1.001 no C40 . H401 . 1.000 no C41 . C42 . 1.521(11) yes C41 . C43 . 1.489(13) yes C41 . H411 . 1.001 no C42 . H421 . 1.000 no C42 . H422 . 0.999 no C42 . H423 . 1.001 no C43 . H431 . 0.999 no C43 . H432 . 0.998 no C43 . H433 . 1.001 no C44 . H441 . 1.001 no C44 . H442 . 1.000 no C44 . H443 . 1.000 no C45 . Cl3 . 1.748(8) yes C45 . Cl4 . 1.759(7) yes C45 . Cl5 . 1.749(7) yes C45 . H451 . 1.000 no C17 . C18 . 1.3900(2) yes C17 . C22 . 1.3900(2) yes C18 . C19 . 1.3900(4) yes C18 . H181 . 0.997 no C19 . C20 . 1.3900(2) yes C19 . H191 . 1.002 no C20 . C21 . 1.3900(2) yes C20 . H201 . 1.005 no C21 . C22 . 1.3900(4) yes C21 . H211 . 1.003 no C22 . H221 . 0.998 no C23 . C24 . 1.3900(3) yes C23 . C28 . 1.3900(3) yes C24 . C25 . 1.3900(2) yes C24 . H241 . 1.001 no C25 . C26 . 1.3900(3) yes C25 . H251 . 1.000 no C26 . C27 . 1.3900(3) yes C26 . H261 . 0.999 no C27 . C28 . 1.3900(2) yes C27 . H271 . 0.999 no C28 . H281 . 1.000 no C29 . C30 . 1.3900(3) yes C29 . C34 . 1.3900(3) yes C30 . C31 . 1.3900(2) yes C30 . H301 . 1.001 no C31 . C32 . 1.3900(3) yes C31 . H311 . 1.000 no C32 . C33 . 1.3900(3) yes C32 . H321 . 0.999 no C33 . C34 . 1.3900(2) yes C33 . H331 . 0.999 no C34 . H341 . 1.000 no C171 . C181 . 1.3900(3) yes C171 . C221 . 1.3900(3) yes C181 . C191 . 1.3900(4) yes C181 . H1811 . 0.997 no C191 . C201 . 1.3900(3) yes C191 . H1911 . 1.001 no C201 . C211 . 1.3900(3) yes C201 . H2011 . 1.004 no C211 . C221 . 1.3900(4) yes C211 . H2111 . 1.003 no C221 . H2211 . 0.999 no C231 . C241 . 1.3900(2) yes C231 . C281 . 1.3900(3) yes C241 . C251 . 1.3900(2) yes C241 . H2411 . 0.989 no C251 . C261 . 1.3900(3) yes C251 . H2511 . 1.006 no C261 . C271 . 1.3900(2) yes C261 . H2611 . 1.017 no C271 . C281 . 1.3900(2) yes C271 . H2711 . 1.011 no C281 . H2811 . 0.994 no C291 . C301 . 1.3900(2) yes C291 . C341 . 1.3900(3) yes C301 . C311 . 1.3900(2) yes C301 . H3011 . 0.995 no C311 . C321 . 1.3900(3) yes C311 . H3111 . 1.004 no C321 . C331 . 1.3900(2) yes C321 . H3211 . 1.009 no C331 . C341 . 1.3900(2) yes C331 . H3311 . 1.005 no C341 . H3411 . 0.997 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 P1 . Ru1 . C35 . 108.74(16) yes P1 . Ru1 . C36 . 145.14(17) yes C35 . Ru1 . C36 . 37.2(2) yes P1 . Ru1 . C37 . 163.34(15) yes C35 . Ru1 . C37 . 67.0(2) yes C36 . Ru1 . C37 . 36.1(2) yes P1 . Ru1 . C38 . 127.90(16) yes C35 . Ru1 . C38 . 80.9(2) yes C36 . Ru1 . C38 . 66.4(2) yes C37 . Ru1 . C38 . 36.9(2) yes P1 . Ru1 . C39 . 97.48(15) yes C35 . Ru1 . C39 . 68.8(3) yes C36 . Ru1 . C39 . 78.3(2) yes C37 . Ru1 . C39 . 65.9(2) yes C38 . Ru1 . C39 . 36.8(2) yes P1 . Ru1 . C40 . 88.90(16) yes C35 . Ru1 . C40 . 37.8(2) yes C36 . Ru1 . C40 . 66.3(2) yes C37 . Ru1 . C40 . 78.3(2) yes C38 . Ru1 . C40 . 67.7(2) yes P1 . Ru1 . Cl1 . 89.81(6) yes C35 . Ru1 . Cl1 . 161.45(16) yes C36 . Ru1 . Cl1 . 124.39(17) yes C37 . Ru1 . Cl1 . 95.27(17) yes C38 . Ru1 . Cl1 . 87.92(17) yes P1 . Ru1 . Cl2 . 85.91(6) yes C35 . Ru1 . Cl2 . 95.66(17) yes C36 . Ru1 . Cl2 . 90.11(15) yes C37 . Ru1 . Cl2 . 110.28(16) yes C38 . Ru1 . Cl2 . 145.48(17) yes C39 . Ru1 . C40 . 38.2(3) yes C39 . Ru1 . Cl1 . 110.0(2) yes C40 . Ru1 . Cl1 . 147.42(18) yes C39 . Ru1 . Cl2 . 164.3(2) yes C40 . Ru1 . Cl2 . 127.14(19) yes Cl1 . Ru1 . Cl2 . 85.20(6) yes Ru1 . P1 . C1 . 114.98(19) yes Ru1 . P1 . C7 . 108.41(19) yes C1 . P1 . C7 . 107.4(3) yes Ru1 . P1 . C13 . 115.2(2) yes C1 . P1 . C13 . 103.1(3) yes C7 . P1 . C13 . 107.2(3) yes N1 . P2 . C13 . 111.1(3) yes N1 . P2 . C16 . 114.8(4) yes C13 . P2 . C16 . 95.4(4) yes N1 . P2 . C17 . 121.6(4) yes C13 . P2 . C17 . 110.4(4) yes C16 . P2 . C17 . 100.1(5) yes N1 . P2 . C171 . 107.6(4) yes C13 . P2 . C171 . 112.5(4) yes C16 . P2 . C171 . 115.2(5) yes N1 . P3 . O1 . 122.3(3) yes N1 . P3 . O2 . 101.7(3) yes O1 . P3 . O2 . 114.3(3) yes N1 . P3 . O3 . 106.5(3) yes O1 . P3 . O3 . 106.9(3) yes O2 . P3 . O3 . 103.6(3) yes P2 . N1 . P3 . 128.8(4) yes P3 . O2 . C23 . 134.2(7) yes P3 . O2 . C231 . 117.9(9) yes P3 . O3 . C29 . 120.7(5) yes P3 . O3 . C291 . 121.0(9) yes P1 . C1 . C2 . 117.4(5) yes P1 . C1 . C6 . 123.2(5) yes C2 . C1 . C6 . 119.0(5) yes C1 . C2 . C3 . 120.6(6) yes C1 . C2 . H21 . 119.630 no C3 . C2 . H21 . 119.721 no C2 . C3 . C4 . 119.9(6) yes C2 . C3 . H31 . 120.018 no C4 . C3 . H31 . 120.037 no C3 . C4 . C5 . 120.0(6) yes C3 . C4 . H41 . 120.019 no C5 . C4 . H41 . 119.940 no C4 . C5 . C6 . 120.8(7) yes C4 . C5 . H51 . 119.612 no C6 . C5 . H51 . 119.570 no C1 . C6 . C5 . 119.6(6) yes C1 . C6 . H61 . 120.198 no C5 . C6 . H61 . 120.225 no P1 . C7 . C8 . 123.0(5) yes P1 . C7 . C12 . 117.9(5) yes C8 . C7 . C12 . 118.7(6) yes C7 . C8 . C9 . 120.7(6) yes C7 . C8 . H81 . 119.583 no C9 . C8 . H81 . 119.671 no C8 . C9 . C10 . 119.6(7) yes C8 . C9 . H91 . 120.115 no C10 . C9 . H91 . 120.271 no C9 . C10 . C11 . 120.5(7) yes C9 . C10 . H101 . 119.711 no C11 . C10 . H101 . 119.794 no C10 . C11 . C12 . 120.8(7) yes C10 . C11 . H111 . 119.654 no C12 . C11 . H111 . 119.587 no C7 . C12 . C11 . 119.7(6) yes C7 . C12 . H121 . 120.131 no C11 . C12 . H121 . 120.174 no P1 . C13 . P2 . 124.2(4) yes P1 . C13 . C14 . 113.2(4) yes P2 . C13 . C14 . 102.5(4) yes P1 . C13 . H131 . 105.084 no P2 . C13 . H131 . 105.199 no C14 . C13 . H131 . 105.090 no C13 . C14 . C15 . 107.8(6) yes C13 . C14 . H141 . 109.899 no C15 . C14 . H141 . 109.923 no C13 . C14 . H142 . 109.868 no C15 . C14 . H142 . 109.860 no H141 . C14 . H142 . 109.470 no C14 . C15 . C16 . 110.4(7) yes C14 . C15 . H151 . 109.170 no C16 . C15 . H151 . 109.329 no C14 . C15 . H152 . 109.177 no C16 . C15 . H152 . 109.420 no H151 . C15 . H152 . 109.356 no C15 . C16 . P2 . 107.0(5) yes C15 . C16 . H161 . 110.123 no P2 . C16 . H161 . 110.189 no C15 . C16 . H162 . 110.033 no P2 . C16 . H162 . 110.096 no H161 . C16 . H162 . 109.389 no Ru1 . C35 . C36 . 72.2(3) yes Ru1 . C35 . C40 . 69.2(3) yes C36 . C35 . C40 . 115.9(5) yes Ru1 . C35 . C41 . 132.1(4) yes C36 . C35 . C41 . 123.6(6) yes C40 . C35 . C41 . 120.3(6) yes Ru1 . C36 . C35 . 70.5(3) yes Ru1 . C36 . C37 . 72.3(3) yes C35 . C36 . C37 . 122.2(5) yes Ru1 . C36 . H361 . 131.229 no C35 . C36 . H361 . 118.880 no C37 . C36 . H361 . 118.877 no Ru1 . C37 . C36 . 71.5(3) yes Ru1 . C37 . C38 . 70.8(3) yes C36 . C37 . C38 . 121.2(6) yes Ru1 . C37 . H371 . 131.112 no C36 . C37 . H371 . 119.423 no C38 . C37 . H371 . 119.426 no Ru1 . C38 . C37 . 72.4(3) yes Ru1 . C38 . C39 . 70.4(3) yes C37 . C38 . C39 . 118.4(6) yes Ru1 . C38 . C44 . 128.7(4) yes C37 . C38 . C44 . 120.1(6) yes C39 . C38 . C44 . 121.5(6) yes Ru1 . C39 . C38 . 72.8(3) yes Ru1 . C39 . C40 . 69.8(3) yes C38 . C39 . C40 . 120.1(5) yes Ru1 . C39 . H391 . 129.898 no C38 . C39 . H391 . 119.912 no C40 . C39 . H391 . 119.957 no Ru1 . C40 . C39 . 72.0(3) yes Ru1 . C40 . C35 . 73.0(3) yes C39 . C40 . C35 . 122.1(5) yes Ru1 . C40 . H401 . 128.346 no C39 . C40 . H401 . 119.020 no C35 . C40 . H401 . 118.916 no C35 . C41 . C42 . 109.9(6) yes C35 . C41 . C43 . 114.0(7) yes C42 . C41 . C43 . 109.9(7) yes C35 . C41 . H411 . 107.548 no C42 . C41 . H411 . 107.567 no C43 . C41 . H411 . 107.672 no C41 . C42 . H421 . 109.442 no C41 . C42 . H422 . 109.483 no H421 . C42 . H422 . 109.569 no C41 . C42 . H423 . 109.424 no H421 . C42 . H423 . 109.412 no H422 . C42 . H423 . 109.498 no C41 . C43 . H431 . 109.427 no C41 . C43 . H432 . 109.452 no H431 . C43 . H432 . 109.684 no C41 . C43 . H433 . 109.311 no H431 . C43 . H433 . 109.457 no H432 . C43 . H433 . 109.496 no C38 . C44 . H441 . 109.439 no C38 . C44 . H442 . 109.482 no H441 . C44 . H442 . 109.465 no C38 . C44 . H443 . 109.449 no H441 . C44 . H443 . 109.455 no H442 . C44 . H443 . 109.536 no Cl3 . C45 . Cl4 . 111.0(4) yes Cl3 . C45 . Cl5 . 110.1(4) yes Cl4 . C45 . Cl5 . 109.4(4) yes Cl3 . C45 . H451 . 108.699 no Cl4 . C45 . H451 . 108.729 no Cl5 . C45 . H451 . 108.749 no P2 . C17 . C18 . 126.9(5) yes P2 . C17 . C22 . 113.0(5) yes C18 . C17 . C22 . 120.00(2) yes C17 . C18 . C19 . 120.00(2) yes C17 . C18 . H181 . 120.256 no C19 . C18 . H181 . 119.744 no C18 . C19 . C20 . 120.000(4) yes C18 . C19 . H191 . 120.276 no C20 . C19 . H191 . 119.724 no C19 . C20 . C21 . 120.000(16) yes C19 . C20 . H201 . 120.057 no C21 . C20 . H201 . 119.943 no C20 . C21 . C22 . 120.00(2) yes C20 . C21 . H211 . 119.818 no C22 . C21 . H211 . 120.183 no C17 . C22 . C21 . 120.000(16) yes C17 . C22 . H221 . 120.205 no C21 . C22 . H221 . 119.795 no O2 . C23 . C24 . 117.7(9) yes O2 . C23 . C28 . 122.0(9) yes C24 . C23 . C28 . 120.000(15) yes C23 . C24 . C25 . 120.000(15) yes C23 . C24 . H241 . 120.032 no C25 . C24 . H241 . 119.968 no C24 . C25 . C26 . 120.00(2) yes C24 . C25 . H251 . 120.002 no C26 . C25 . H251 . 119.998 no C25 . C26 . C27 . 120.000(15) yes C25 . C26 . H261 . 120.016 no C27 . C26 . H261 . 119.983 no C26 . C27 . C28 . 120.000(15) yes C26 . C27 . H271 . 120.061 no C28 . C27 . H271 . 119.939 no C23 . C28 . C27 . 120.000(15) yes C23 . C28 . H281 . 119.909 no C27 . C28 . H281 . 120.090 no O3 . C29 . C30 . 121.9(5) yes O3 . C29 . C34 . 118.1(5) yes C30 . C29 . C34 . 120.000(10) yes C29 . C30 . C31 . 120.000(10) yes C29 . C30 . H301 . 119.968 no C31 . C30 . H301 . 120.031 no C30 . C31 . C32 . 120.000(17) yes C30 . C31 . H311 . 119.952 no C32 . C31 . H311 . 120.047 no C31 . C32 . C33 . 120.000(7) yes C31 . C32 . H321 . 119.976 no C33 . C32 . H321 . 120.024 no C32 . C33 . C34 . 120.000(10) yes C32 . C33 . H331 . 120.015 no C34 . C33 . H331 . 119.985 no C29 . C34 . C33 . 120.000(7) yes C29 . C34 . H341 . 119.970 no C33 . C34 . H341 . 120.030 no P2 . C171 . C181 . 118.8(6) yes P2 . C171 . C221 . 121.2(6) yes C181 . C171 . C221 . 120.00(2) yes C171 . C181 . C191 . 120.00(2) yes C171 . C181 . H1811 . 120.200 no C191 . C181 . H1811 . 119.801 no C181 . C191 . C201 . 120.000(10) yes C181 . C191 . H1911 . 120.279 no C201 . C191 . H1911 . 119.721 no C191 . C201 . C211 . 120.000(12) yes C191 . C201 . H2011 . 120.109 no C211 . C201 . H2011 . 119.891 no C201 . C211 . C221 . 120.00(2) yes C201 . C211 . H2111 . 119.859 no C221 . C211 . H2111 . 120.141 no C171 . C221 . C211 . 120.000(12) yes C171 . C221 . H2211 . 120.223 no C211 . C221 . H2211 . 119.777 no O2 . C231 . C241 . 111.2(13) yes O2 . C231 . C281 . 128.7(13) yes C241 . C231 . C281 . 120.000(9) yes C231 . C241 . C251 . 120.000(9) yes C231 . C241 . H2411 . 120.918 no C251 . C241 . H2411 . 119.081 no C241 . C251 . C261 . 119.999(19) yes C241 . C251 . H2511 . 121.066 no C261 . C251 . H2511 . 118.932 no C251 . C261 . C271 . 120.000(12) yes C251 . C261 . H2611 . 120.300 no C271 . C261 . H2611 . 119.698 no C261 . C271 . C281 . 120.000(9) yes C261 . C271 . H2711 . 119.377 no C281 . C271 . H2711 . 120.621 no C231 . C281 . C271 . 120.000(12) yes C231 . C281 . H2811 . 120.796 no C271 . C281 . H2811 . 119.199 no O3 . C291 . C301 . 114.7(11) yes O3 . C291 . C341 . 125.2(11) yes C301 . C291 . C341 . 120.000(15) yes C29 . C301 . C311 . 119.2(4) yes C291 . C301 . C311 . 120.000(15) yes C291 . C301 . H3011 . 119.932 no C311 . C301 . H3011 . 120.065 no C301 . C311 . C321 . 120.001(13) yes C301 . C311 . H3111 . 120.157 no C321 . C311 . H3111 . 119.842 no C311 . C321 . C331 . 120.000(6) yes C311 . C321 . H3211 . 119.721 no C331 . C321 . H3211 . 120.279 no C321 . C331 . C341 . 120.000(15) yes C321 . C331 . H3311 . 119.252 no C341 . C331 . H3311 . 120.747 no C291 . C341 . C331 . 120.001(6) yes C291 . C341 . H3411 . 124.807 no C331 . C341 . H3411 . 115.175 no #===END data_CRYSTALS_cif_2 _database_code_depnum_ccdc_archive 'CCDC 612114' _audit_creation_date 06-04-10 _audit_creation_method CRYSTALS_ver_12.51 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.2949(18) _cell_length_b 12.576(3) _cell_length_c 18.412(3) _cell_angle_alpha 101.298(17) _cell_angle_beta 90.983(15) _cell_angle_gamma 95.652(17) _cell_volume 2098.8(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' 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' 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' 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' Sb -0.5866 1.5461 19.6418 5.3034 19.0455 0.4607 5.0371 27.9074 2.6827 75.2825 4.5909 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C78 H72 Cl2 F20 N4 P4 Ru2 Sb2 # Dc = 1.65 Fooo = 1032.00 Mu = 12.18 M = 1042.93 # Found Formula = C78 H72 Cl2 F20 N4 P4 Ru2 Sb2 # Dc = 1.65 FOOO = 1032.00 Mu = 12.18 M = 1042.93 _chemical_formula_sum 'C78 H72 Cl2 F20 N4 P4 Ru2 Sb2' _chemical_formula_moiety 'C78 H72 Cl2 F8 N4 P4 Ru2, 2(F6 Sb)' _chemical_compound_source ? _chemical_formula_weight 2085.86 _cell_measurement_reflns_used 3000 _cell_measurement_theta_min 3 _cell_measurement_theta_max 24 _cell_measurement_temperature 180 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.218 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.97 _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _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 'Xcalibur, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _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 180 _diffrn_reflns_number 12150 _reflns_number_total 6010 _diffrn_reflns_av_R_equivalents 0.117 # Number of reflections with Friedels Law is 6010 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 14749 _diffrn_reflns_theta_min 2.888 _diffrn_reflns_theta_max 32.069 _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 26.617 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -18 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.89 _refine_diff_density_max 2.09 _refine_ls_number_reflns 2720 _refine_ls_number_restraints 0 _refine_ls_number_parameters 264 #_refine_ls_R_factor_ref 0.0831 _refine_ls_wR_factor_ref 0.0848 _refine_ls_goodness_of_fit_ref 1.1210 #_reflns_number_all 13348 _refine_ls_R_factor_all 0.3028 _refine_ls_wR_factor_all 0.1228 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2720 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_gt 0.0848 _refine_ls_shift/su_max 0.000295 # 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 refu # 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: 6.86 -3.27 4.75 0.945 ; _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # Some potentially useful phrases are: ; Hydrogen atoms were placed geometrically after each cycle. Small and bad quality crystal, only Ru Sb P and Cl atoms were anisotropically refined ; _publ_section_exptl_prep ; ? ; # 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), 435-435 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 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. Oxford Diffraction, (2002) CrysAlis RED. Oxford Diffraction, (2002) Xcalibur User Manual 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 0.84018(16) 0.63220(12) 0.69834(8) 0.0253 1.0000 Uani . . . . . . P1 P 0.7352(4) 0.4521(4) 0.6984(2) 0.0214 1.0000 Uani . . . . . . P2 P 0.7976(5) 0.2445(3) 0.7740(2) 0.0232 1.0000 Uani . . . . . . Sb1 Sb 0.0000 0.0000 0.5000 0.0372 1.0000 Uani S . . . . . Sb2 Sb 0.8741(4) -0.0312(3) 0.07142(19) 0.0653 0.5000 Uani . . . . . . Cl1 Cl 1.0647(5) 0.5693(4) 0.6567(2) 0.0355 1.0000 Uani . . . . . . C1 C 0.9715(19) 0.6444(14) 0.8616(10) 0.029(4) 1.0000 Uiso . . . . . . C2 C 1.0414(18) 0.6614(14) 0.9323(9) 0.030(4) 1.0000 Uiso . . . . . . C3 C 1.1806(17) 0.7071(13) 0.9460(9) 0.021(4) 1.0000 Uiso . . . . . . C4 C 1.2455(18) 0.7309(13) 1.0123(9) 0.023(4) 1.0000 Uiso . . . . . . C5 C 1.1747(17) 0.7077(13) 1.0751(8) 0.022(4) 1.0000 Uiso . . . . . . C6 C 1.0369(18) 0.6546(13) 1.0614(9) 0.025(4) 1.0000 Uiso . . . . . . C7 C 0.9714(18) 0.6328(13) 0.9946(9) 0.026(4) 1.0000 Uiso . . . . . . C8 C 0.796(2) 0.6872(15) 0.5917(10) 0.036(4) 1.0000 Uiso . . . . . . C9 C 0.669(2) 0.6594(16) 0.6239(11) 0.039(5) 1.0000 Uiso . . . . . . C10 C 0.636(2) 0.7038(15) 0.6968(10) 0.038(5) 1.0000 Uiso . . . . . . C11 C 0.733(2) 0.7812(15) 0.7436(10) 0.036(4) 1.0000 Uiso . . . . . . C12 C 0.866(2) 0.8142(15) 0.7126(10) 0.039(5) 1.0000 Uiso . . . . . . C13 C 0.898(2) 0.7743(16) 0.6426(11) 0.043(5) 1.0000 Uiso . . . . . . C14 C 0.839(2) 0.6457(16) 0.5138(11) 0.043(5) 1.0000 Uiso . . . . . . C15 C 0.701(2) 0.8339(15) 0.8222(11) 0.039(5) 1.0000 Uiso . . . . . . C16 C 0.595(2) 0.7671(19) 0.8597(13) 0.057(6) 1.0000 Uiso . . . . . . C17 C 0.656(3) 0.946(2) 0.8219(15) 0.076(8) 1.0000 Uiso . . . . . . C18 C 0.6646(17) 0.3741(13) 0.6074(8) 0.022(4) 1.0000 Uiso . . . . . . C19 C 0.7469(19) 0.3864(15) 0.5485(10) 0.034(4) 1.0000 Uiso . . . . . . C20 C 0.705(2) 0.3254(15) 0.4750(10) 0.038(5) 1.0000 Uiso . . . . . . C21 C 0.583(2) 0.2511(15) 0.4689(10) 0.035(4) 1.0000 Uiso . . . . . . C22 C 0.499(2) 0.2432(15) 0.5267(10) 0.036(4) 1.0000 Uiso . . . . . . C23 C 0.5412(19) 0.3030(14) 0.5957(9) 0.031(4) 1.0000 Uiso . . . . . . C24 C 0.5854(19) 0.4604(14) 0.7608(10) 0.032(4) 1.0000 Uiso . . . . . . C25 C 0.446(2) 0.4742(16) 0.7388(10) 0.040(5) 1.0000 Uiso . . . . . . C26 C 0.336(2) 0.4882(16) 0.7897(11) 0.041(5) 1.0000 Uiso . . . . . . C27 C 0.366(2) 0.4871(15) 0.8635(10) 0.036(4) 1.0000 Uiso . . . . . . C28 C 0.505(2) 0.4750(18) 0.8855(12) 0.050(5) 1.0000 Uiso . . . . . . C29 C 0.6179(17) 0.4635(13) 0.8376(9) 0.024(4) 1.0000 Uiso . . . . . . C30 C 0.6426(17) 0.1660(13) 0.7225(9) 0.025(4) 1.0000 Uiso . . . . . . C31 C 0.507(2) 0.1684(15) 0.7545(10) 0.038(5) 1.0000 Uiso . . . . . . C32 C 0.386(2) 0.1046(18) 0.7157(12) 0.052(6) 1.0000 Uiso . . . . . . C33 C 0.406(2) 0.0375(18) 0.6482(12) 0.049(5) 1.0000 Uiso . . . . . . C34 C 0.536(2) 0.0346(17) 0.6184(11) 0.045(5) 1.0000 Uiso . . . . . . C35 C 0.6583(17) 0.0981(13) 0.6546(9) 0.025(4) 1.0000 Uiso . . . . . . C36 C 0.9584(18) 0.1716(13) 0.7527(9) 0.027(4) 1.0000 Uiso . . . . . . C37 C 1.055(2) 0.2438(15) 0.7075(10) 0.038(5) 1.0000 Uiso . . . . . . C38 C 0.9578(17) 0.3124(13) 0.6704(9) 0.023(4) 1.0000 Uiso . . . . . . C39 C 0.8613(17) 0.3632(13) 0.7316(8) 0.022(4) 1.0000 Uiso . . . . . . N1 N 0.9161(15) 0.6332(11) 0.8033(8) 0.027(4) 1.0000 Uiso . . . . . . N2 N 1.2491(15) 0.7358(11) 1.1432(8) 0.030(3) 1.0000 Uiso . . . . . . F3 F 1.2529(11) 0.7357(8) 0.8876(6) 0.042(3) 1.0000 Uiso . . . . . . F4 F 1.3845(12) 0.7804(9) 1.0228(6) 0.048(3) 1.0000 Uiso . . . . . . F6 F 0.9615(12) 0.6306(9) 1.1202(6) 0.043(3) 1.0000 Uiso . . . . . . F7 F 0.8302(11) 0.5838(9) 0.9832(6) 0.042(3) 1.0000 Uiso . . . . . . F8 F 0.900(3) -0.118(2) -0.0217(15) 0.068(3) 0.5000 Uiso . . . . . . F9 F 0.971(3) 0.091(2) 0.0443(15) 0.068(3) 0.5000 Uiso . . . . . . F10 F 1.056(3) -0.060(2) 0.0976(15) 0.068(3) 0.5000 Uiso . . . . . . F11 F 0.843(3) 0.041(2) 0.1614(15) 0.068(3) 0.5000 Uiso . . . . . . F12 F 0.699(3) 0.002(2) 0.0464(14) 0.068(3) 0.5000 Uiso . . . . . . F13 F 0.754(3) -0.176(2) 0.0883(14) 0.068(3) 0.5000 Uiso . . . . . . F14 F -0.1722(16) -0.0883(12) 0.4927(9) 0.085(4) 1.0000 Uiso . . . . . . F15 F 0.0952(15) -0.1220(12) 0.4873(8) 0.076(4) 1.0000 Uiso . . . . . . F16 F 0.0035(14) 0.0009(10) 0.6000(7) 0.061(3) 1.0000 Uiso . . . . . . H91 H 0.5955 0.6044 0.5934 0.044(9) 1.0000 Uiso . . . . . . H101 H 0.5409 0.6797 0.7161 0.044(9) 1.0000 Uiso . . . . . . H121 H 0.9379 0.8690 0.7444 0.044(9) 1.0000 Uiso . . . . . . H131 H 0.9911 0.8022 0.6231 0.044(9) 1.0000 Uiso . . . . . . H141 H 0.9373 0.6803 0.5061 0.044(9) 1.0000 Uiso . . . . . . H142 H 0.8394 0.5648 0.5052 0.044(9) 1.0000 Uiso . . . . . . H143 H 0.7674 0.6645 0.4782 0.044(9) 1.0000 Uiso . . . . . . H151 H 0.7943 0.8445 0.8519 0.044(9) 1.0000 Uiso . . . . . . H171 H 0.6348 0.9815 0.8735 0.044(9) 1.0000 Uiso . . . . . . H172 H 0.7361 0.9907 0.8030 0.044(9) 1.0000 Uiso . . . . . . H173 H 0.5674 0.9390 0.7891 0.044(9) 1.0000 Uiso . . . . . . H191 H 0.8372 0.4381 0.5563 0.044(9) 1.0000 Uiso . . . . . . H201 H 0.7612 0.3362 0.4308 0.044(9) 1.0000 Uiso . . . . . . H211 H 0.5558 0.2020 0.4199 0.044(9) 1.0000 Uiso . . . . . . H221 H 0.4065 0.1940 0.5195 0.044(9) 1.0000 Uiso . . . . . . H231 H 0.4801 0.2943 0.6388 0.044(9) 1.0000 Uiso . . . . . . H251 H 0.4236 0.4741 0.6854 0.044(9) 1.0000 Uiso . . . . . . H261 H 0.2360 0.4989 0.7730 0.044(9) 1.0000 Uiso . . . . . . H271 H 0.2881 0.4950 0.9004 0.044(9) 1.0000 Uiso . . . . . . H281 H 0.5248 0.4744 0.9389 0.044(9) 1.0000 Uiso . . . . . . H291 H 0.7182 0.4577 0.8559 0.044(9) 1.0000 Uiso . . . . . . H311 H 0.4958 0.2149 0.8044 0.044(9) 1.0000 Uiso . . . . . . H321 H 0.2878 0.1076 0.7364 0.044(9) 1.0000 Uiso . . . . . . H331 H 0.3218 -0.0098 0.6212 0.044(9) 1.0000 Uiso . . . . . . H341 H 0.5464 -0.0141 0.5692 0.044(9) 1.0000 Uiso . . . . . . H351 H 0.7552 0.0948 0.6319 0.044(9) 1.0000 Uiso . . . . . . H361 H 1.0108 0.1652 0.7993 0.044(9) 1.0000 Uiso . . . . . . H362 H 0.9307 0.0971 0.7221 0.044(9) 1.0000 Uiso . . . . . . H371 H 1.1287 0.2935 0.7418 0.044(9) 1.0000 Uiso . . . . . . H372 H 1.1060 0.1956 0.6685 0.044(9) 1.0000 Uiso . . . . . . H381 H 1.0179 0.3705 0.6512 0.044(9) 1.0000 Uiso . . . . . . H382 H 0.8976 0.2648 0.6287 0.044(9) 1.0000 Uiso . . . . . . H391 H 0.9280 0.4127 0.7697 0.044(9) 1.0000 Uiso . . . . . . H161 H 0.6290 0.6939 0.8586 0.044(9) 1.0000 Uiso . . . . . . H162 H 0.5863 0.8049 0.9123 0.044(9) 1.0000 Uiso . . . . . . H163 H 0.4982 0.7579 0.8333 0.044(9) 1.0000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0278(10) 0.0294(10) 0.0187(8) 0.0067(7) -0.0027(7) -0.0005(7) P1 0.022(2) 0.028(2) 0.013(2) 0.0017(18) -0.0018(17) 0.0037(19) P2 0.029(3) 0.022(2) 0.020(2) 0.0071(18) -0.0007(18) 0.0028(19) Sb1 0.0396(14) 0.0349(13) 0.0337(12) 0.0014(10) 0.0065(10) -0.0025(10) Sb2 0.089(3) 0.049(2) 0.056(2) 0.0009(16) -0.0137(18) 0.0187(19) Cl1 0.026(2) 0.039(3) 0.040(3) 0.006(2) 0.005(2) 0.000(2) _refine_ls_extinction_method None 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 . P1 . 2.376(5) yes Ru1 . Cl1 . 2.390(5) yes Ru1 . C8 . 2.250(18) yes Ru1 . C9 . 2.18(2) yes Ru1 . C10 . 2.182(19) yes Ru1 . C11 . 2.234(19) yes Ru1 . C12 . 2.241(19) yes Ru1 . C13 . 2.26(2) yes Ru1 . N1 . 2.043(14) yes P1 . C18 . 1.841(16) yes P1 . C24 . 1.818(18) yes P1 . C39 . 1.872(16) yes P2 . N2 2_767 1.570(15) yes P2 . C30 . 1.804(16) yes P2 . C36 . 1.838(17) yes P2 . C39 . 1.867(16) yes Sb1 . F14 2_556 1.843(15) yes Sb1 . F16 2_556 1.839(12) yes Sb1 . F15 2_556 1.823(15) yes Sb1 . F14 . 1.843(15) yes Sb1 . F15 . 1.823(15) yes Sb1 . F16 . 1.839(12) yes Sb2 . F9 2_755 2.62(3) yes Sb2 . Sb2 2_755 3.697(8) yes Sb2 . F8 . 1.88(3) yes Sb2 . F9 . 1.86(3) yes Sb2 . F10 . 1.84(3) yes Sb2 . F11 . 1.77(3) yes Sb2 . F12 . 1.79(3) yes Sb2 . F13 . 2.11(3) yes C1 . C2 . 1.41(2) yes C1 . N1 . 1.16(2) yes C2 . C3 . 1.36(2) yes C2 . C7 . 1.42(2) yes C3 . C4 . 1.32(2) yes C3 . F3 . 1.366(18) yes C4 . C5 . 1.41(2) yes C4 . F4 . 1.371(19) yes C5 . C6 . 1.38(2) yes C5 . N2 . 1.39(2) yes C6 . C7 . 1.33(2) yes C6 . F6 . 1.365(18) yes C7 . F7 . 1.388(19) yes C8 . C9 . 1.38(3) yes C8 . C13 . 1.53(3) yes C8 . C14 . 1.50(3) yes C9 . C10 . 1.40(3) yes C9 . H91 . 1.000 no C10 . C11 . 1.40(3) yes C10 . H101 . 1.000 no C11 . C12 . 1.43(3) yes C11 . C15 . 1.52(3) yes C12 . C13 . 1.34(3) yes C12 . H121 . 1.000 no C13 . H131 . 1.000 no C14 . H141 . 1.000 no C14 . H142 . 1.000 no C14 . H143 . 1.000 no C15 . C16 . 1.50(3) yes C15 . C17 . 1.51(3) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C16 . H162 . 1.000 no C16 . H163 . 1.000 no C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no C18 . C19 . 1.36(2) yes C18 . C23 . 1.37(2) yes C19 . C20 . 1.45(3) yes C19 . H191 . 1.000 no C20 . C21 . 1.39(2) yes C20 . H201 . 1.000 no C21 . C22 . 1.34(2) yes C21 . H211 . 1.000 no C22 . C23 . 1.37(2) yes C22 . H221 . 1.000 no C23 . H231 . 1.000 no C24 . C25 . 1.39(3) yes C24 . C29 . 1.43(2) yes C25 . C26 . 1.40(3) yes C25 . H251 . 1.000 no C26 . C27 . 1.39(3) yes C26 . H261 . 1.000 no C27 . C28 . 1.38(3) yes C27 . H271 . 1.000 no C28 . C29 . 1.38(3) yes C28 . H281 . 1.000 no C29 . H291 . 1.000 no C30 . C31 . 1.40(2) yes C30 . C35 . 1.39(2) yes C31 . C32 . 1.41(3) yes C31 . H311 . 1.000 no C32 . C33 . 1.38(3) yes C32 . H321 . 1.000 no C33 . C34 . 1.33(3) yes C33 . H331 . 1.000 no C34 . C35 . 1.40(3) yes C34 . H341 . 1.000 no C35 . H351 . 1.000 no C36 . C37 . 1.58(2) yes C36 . H361 . 1.000 no C36 . H362 . 1.000 no C37 . C38 . 1.55(2) yes C37 . H371 . 1.000 no C37 . H372 . 1.000 no C38 . C39 . 1.53(2) yes C38 . H381 . 1.000 no C38 . H382 . 1.000 no C39 . H391 . 1.000 no F8 . F9 2_755 1.31(3) 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 P1 . Ru1 . Cl1 . 92.11(16) yes P1 . Ru1 . C8 . 113.1(5) yes Cl1 . Ru1 . C8 . 92.2(5) yes P1 . Ru1 . C9 . 91.9(5) yes Cl1 . Ru1 . C9 . 123.5(5) yes C8 . Ru1 . C9 . 36.2(7) yes P1 . Ru1 . C10 . 95.9(5) yes Cl1 . Ru1 . C10 . 159.3(5) yes C8 . Ru1 . C10 . 67.1(7) yes C9 . Ru1 . C10 . 37.4(7) yes P1 . Ru1 . C11 . 123.5(5) yes Cl1 . Ru1 . C11 . 143.7(5) yes C8 . Ru1 . C11 . 80.9(7) yes C9 . Ru1 . C11 . 67.5(7) yes C10 . Ru1 . C11 . 37.1(7) yes P1 . Ru1 . C12 . 160.7(5) yes Cl1 . Ru1 . C12 . 107.2(5) yes C8 . Ru1 . C12 . 67.8(7) yes C9 . Ru1 . C12 . 78.2(7) yes C10 . Ru1 . C12 . 66.1(7) yes P1 . Ru1 . C13 . 152.5(5) yes Cl1 . Ru1 . C13 . 86.5(5) yes C8 . Ru1 . C13 . 39.7(7) yes C9 . Ru1 . C13 . 66.5(7) yes C10 . Ru1 . C13 . 77.5(7) yes P1 . Ru1 . N1 . 86.1(4) yes Cl1 . Ru1 . N1 . 86.8(4) yes C8 . Ru1 . N1 . 160.8(6) yes C9 . Ru1 . N1 . 149.7(6) yes C10 . Ru1 . N1 . 112.7(6) yes C11 . Ru1 . C12 . 37.3(7) yes C11 . Ru1 . C13 . 65.5(7) yes C12 . Ru1 . C13 . 34.6(7) yes C11 . Ru1 . N1 . 88.6(6) yes C12 . Ru1 . N1 . 94.1(6) yes C13 . Ru1 . N1 . 121.2(6) yes Ru1 . P1 . C18 . 115.0(5) yes Ru1 . P1 . C24 . 108.2(6) yes C18 . P1 . C24 . 107.6(8) yes Ru1 . P1 . C39 . 114.2(5) yes C18 . P1 . C39 . 104.5(7) yes C24 . P1 . C39 . 106.7(8) yes N2 2_767 P2 . C30 . 104.3(7) yes N2 2_767 P2 . C36 . 116.8(8) yes C30 . P2 . C36 . 109.2(8) yes N2 2_767 P2 . C39 . 119.8(7) yes C30 . P2 . C39 . 110.8(7) yes C36 . P2 . C39 . 95.8(7) yes F14 2_556 Sb1 . F16 2_556 87.5(6) yes F14 2_556 Sb1 . F15 2_556 88.7(6) yes F16 2_556 Sb1 . F15 2_556 88.1(6) yes F14 2_556 Sb1 . F14 . 179.994 yes F16 2_556 Sb1 . F14 . 92.5(6) yes F15 2_556 Sb1 . F14 . 91.3(6) yes F14 2_556 Sb1 . F15 . 91.3(6) yes F16 2_556 Sb1 . F15 . 91.9(6) yes F15 2_556 Sb1 . F15 . 179.994 yes F14 . Sb1 . F15 . 88.7(6) yes F14 2_556 Sb1 . F16 . 92.5(6) yes F16 2_556 Sb1 . F16 . 179.994 yes F15 2_556 Sb1 . F16 . 91.9(6) yes F14 . Sb1 . F16 . 87.5(6) yes F15 . Sb1 . F16 . 88.1(6) yes F9 2_755 Sb2 . Sb2 2_755 28.1(6) yes F9 2_755 Sb2 . F8 . 28.2(9) yes Sb2 2_755 Sb2 . F8 . 52.4(8) yes F9 2_755 Sb2 . F9 . 69.8(12) yes Sb2 2_755 Sb2 . F9 . 41.7(8) yes F8 . Sb2 . F9 . 91.6(11) yes F9 2_755 Sb2 . F10 . 67.7(10) yes Sb2 2_755 Sb2 . F10 . 71.5(8) yes F8 . Sb2 . F10 . 86.8(12) yes F9 . Sb2 . F10 . 84.5(12) yes F9 2_755 Sb2 . F11 . 154.8(11) yes Sb2 2_755 Sb2 . F11 . 131.8(9) yes F8 . Sb2 . F11 . 175.6(12) yes F9 . Sb2 . F11 . 92.8(12) yes F10 . Sb2 . F11 . 93.3(12) yes F9 2_755 Sb2 . F12 . 112.5(10) yes Sb2 2_755 Sb2 . F12 . 107.7(8) yes F8 . Sb2 . F12 . 94.2(12) yes F9 . Sb2 . F12 . 93.7(12) yes F10 . Sb2 . F12 . 178.0(12) yes F9 2_755 Sb2 . F13 . 105.7(9) yes Sb2 2_755 Sb2 . F13 . 133.6(7) yes F8 . Sb2 . F13 . 82.4(11) yes F9 . Sb2 . F13 . 172.8(11) yes F10 . Sb2 . F13 . 99.2(11) yes F11 . Sb2 . F12 . 85.9(12) yes F11 . Sb2 . F13 . 93.2(11) yes F12 . Sb2 . F13 . 82.7(11) yes C2 . C1 . N1 . 178.0(19) yes C1 . C2 . C3 . 122.7(16) yes C1 . C2 . C7 . 122.5(15) yes C3 . C2 . C7 . 114.8(15) yes C2 . C3 . C4 . 124.1(16) yes C2 . C3 . F3 . 117.0(14) yes C4 . C3 . F3 . 118.7(14) yes C3 . C4 . C5 . 121.5(15) yes C3 . C4 . F4 . 121.2(15) yes C5 . C4 . F4 . 117.3(14) yes C4 . C5 . C6 . 115.2(14) yes C4 . C5 . N2 . 118.4(14) yes C6 . C5 . N2 . 126.4(14) yes C5 . C6 . C7 . 122.8(15) yes C5 . C6 . F6 . 118.2(14) yes C7 . C6 . F6 . 118.8(14) yes C2 . C7 . C6 . 121.4(15) yes C2 . C7 . F7 . 117.1(14) yes C6 . C7 . F7 . 121.5(14) yes Ru1 . C8 . C9 . 69.1(11) yes Ru1 . C8 . C13 . 70.4(10) yes C9 . C8 . C13 . 113.6(17) yes Ru1 . C8 . C14 . 131.6(13) yes C9 . C8 . C14 . 127.3(17) yes C13 . C8 . C14 . 119.1(16) yes Ru1 . C9 . C8 . 74.6(11) yes Ru1 . C9 . C10 . 71.4(11) yes C8 . C9 . C10 . 123.8(17) yes Ru1 . C9 . H91 . 128.4 no C8 . C9 . H91 . 118.1 no C10 . C9 . H91 . 118.1 no Ru1 . C10 . C9 . 71.2(11) yes Ru1 . C10 . C11 . 73.5(11) yes C9 . C10 . C11 . 122.0(17) yes Ru1 . C10 . H101 . 128.7 no C9 . C10 . H101 . 119.0 no C11 . C10 . H101 . 119.0 no Ru1 . C11 . C10 . 69.4(11) yes Ru1 . C11 . C12 . 71.6(11) yes C10 . C11 . C12 . 116.6(17) yes Ru1 . C11 . C15 . 131.7(13) yes C10 . C11 . C15 . 124.1(16) yes C12 . C11 . C15 . 119.3(16) yes Ru1 . C12 . C11 . 71.1(11) yes Ru1 . C12 . C13 . 73.3(12) yes C11 . C12 . C13 . 122.3(18) yes Ru1 . C12 . H121 . 129.4 no C11 . C12 . H121 . 118.8 no C13 . C12 . H121 . 118.8 no Ru1 . C13 . C8 . 70.0(10) yes Ru1 . C13 . C12 . 72.1(12) yes C8 . C13 . C12 . 121.7(17) yes Ru1 . C13 . H131 . 131.9 no C8 . C13 . H131 . 119.1 no C12 . C13 . H131 . 119.1 no C8 . C14 . H141 . 109.5 no C8 . C14 . H142 . 109.5 no H141 . C14 . H142 . 109.5 no C8 . C14 . H143 . 109.5 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no C11 . C15 . C16 . 114.7(17) yes C11 . C15 . C17 . 108.6(17) yes C16 . C15 . C17 . 112.3(18) yes C11 . C15 . H151 . 106.9 no C16 . C15 . H151 . 106.9 no C17 . C15 . H151 . 106.9 no C15 . C16 . H161 . 109.5 no C15 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 109.5 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no C15 . C17 . H171 . 109.5 no C15 . C17 . H172 . 109.5 no H171 . C17 . H172 . 109.5 no C15 . C17 . H173 . 109.5 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no P1 . C18 . C19 . 116.0(12) yes P1 . C18 . C23 . 125.1(12) yes C19 . C18 . C23 . 118.8(15) yes C18 . C19 . C20 . 120.6(16) yes C18 . C19 . H191 . 119.7 no C20 . C19 . H191 . 119.7 no C19 . C20 . C21 . 116.7(16) yes C19 . C20 . H201 . 121.7 no C21 . C20 . H201 . 121.7 no C20 . C21 . C22 . 122.0(17) yes C20 . C21 . H211 . 119.0 no C22 . C21 . H211 . 119.0 no C21 . C22 . C23 . 119.7(17) yes C21 . C22 . H221 . 120.2 no C23 . C22 . H221 . 120.2 no C22 . C23 . C18 . 122.0(16) yes C22 . C23 . H231 . 119.0 no C18 . C23 . H231 . 119.0 no P1 . C24 . C25 . 123.1(14) yes P1 . C24 . C29 . 117.4(13) yes C25 . C24 . C29 . 119.2(16) yes C24 . C25 . C26 . 121.4(17) yes C24 . C25 . H251 . 119.3 no C26 . C25 . H251 . 119.3 no C25 . C26 . C27 . 119.3(18) yes C25 . C26 . H261 . 120.4 no C27 . C26 . H261 . 120.4 no C26 . C27 . C28 . 119.3(18) yes C26 . C27 . H271 . 120.4 no C28 . C27 . H271 . 120.3 no C27 . C28 . C29 . 123.5(19) yes C27 . C28 . H281 . 118.2 no C29 . C28 . H281 . 118.2 no C24 . C29 . C28 . 117.3(16) yes C24 . C29 . H291 . 121.4 no C28 . C29 . H291 . 121.4 no P2 . C30 . C31 . 119.0(12) yes P2 . C30 . C35 . 120.8(12) yes C31 . C30 . C35 . 120.1(15) yes C30 . C31 . C32 . 119.2(17) yes C30 . C31 . H311 . 120.4 no C32 . C31 . H311 . 120.4 no C31 . C32 . C33 . 119.0(20) yes C31 . C32 . H321 . 120.5 no C33 . C32 . H321 . 120.5 no C32 . C33 . C34 . 122(2) yes C32 . C33 . H331 . 119.2 no C34 . C33 . H331 . 119.2 no C33 . C34 . C35 . 121.3(19) yes C33 . C34 . H341 . 119.3 no C35 . C34 . H341 . 119.3 no C34 . C35 . C30 . 118.8(16) yes C34 . C35 . H351 . 120.6 no C30 . C35 . H351 . 120.6 no P2 . C36 . C37 . 104.7(11) yes P2 . C36 . H361 . 110.6 no C37 . C36 . H361 . 110.6 no P2 . C36 . H362 . 110.6 no C37 . C36 . H362 . 110.6 no H361 . C36 . H362 . 109.5 no C36 . C37 . C38 . 109.1(14) yes C36 . C37 . H371 . 109.6 no C38 . C37 . H371 . 109.6 no C36 . C37 . H372 . 109.6 no C38 . C37 . H372 . 109.6 no H371 . C37 . H372 . 109.5 no C37 . C38 . C39 . 105.4(13) yes C37 . C38 . H381 . 110.5 no C39 . C38 . H381 . 110.5 no C37 . C38 . H382 . 110.5 no C39 . C38 . H382 . 110.5 no H381 . C38 . H382 . 109.5 no C38 . C39 . P1 . 112.4(11) yes C38 . C39 . P2 . 102.5(10) yes P1 . C39 . P2 . 123.0(8) yes C38 . C39 . H391 . 105.9 no P1 . C39 . H391 . 105.9 no P2 . C39 . H391 . 105.9 no Ru1 . N1 . C1 . 171.5(14) yes C5 . N2 . P2 2_767 134.2(12) yes #===END data_CRYSTALS_cif_3 _database_code_depnum_ccdc_archive 'CCDC 612115' _audit_creation_date 06-06-09 _audit_creation_method CRYSTALS_ver_12.51 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 15.4570(10) _cell_length_b 14.6930(8) _cell_length_c 20.1840(11) _cell_angle_alpha 90 _cell_angle_beta 99.750(5) _cell_angle_gamma 90 _cell_volume 4517.8(5) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? 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' 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' 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' Sb -0.5866 1.5461 19.6418 5.3034 19.0455 0.4607 5.0371 27.9074 2.6827 75.2825 4.5909 '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' 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 2 # Given Formula = C86 H92 Cl2 F20 N4 O2 P4 Ru2 Sb2 # Dc = 1.64 Fooo = 2232.00 Mu = 11.39 M = 1117.05 # Found Formula = C86 H92 Cl2 F20 N4 O2 P4 Ru2 Sb2 # Dc = 1.64 FOOO = 2232.00 Mu = 11.39 M = 1117.05 _chemical_formula_sum 'C86 H92 Cl2 F20 N4 O2 P4 Ru2 Sb2' _chemical_formula_moiety 'C78 H72 Cl2 F8 N4 P4 Ru2, 2(C4 H10 O), 2(F6 Sb) ' _chemical_compound_source ? _chemical_formula_weight 2234.10 _cell_measurement_reflns_used 6792 _cell_measurement_theta_min 4 _cell_measurement_theta_max 28 _cell_measurement_temperature 180 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.97 _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _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 'Xcalibur, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _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 180 _diffrn_reflns_number 39404 _reflns_number_total 12075 _diffrn_reflns_av_R_equivalents 0.113 # Number of reflections with Friedels Law is 12075 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 12082 _diffrn_reflns_theta_min 2.950 _diffrn_reflns_theta_max 29.014 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.014 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -21 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.91 _refine_diff_density_max 1.93 _refine_ls_number_reflns 4864 _refine_ls_number_restraints 0 _refine_ls_number_parameters 466 #_refine_ls_R_factor_ref 0.0637 _refine_ls_wR_factor_ref 0.0675 _refine_ls_goodness_of_fit_ref 1.1485 #_reflns_number_all 12054 _refine_ls_R_factor_all 0.1657 _refine_ls_wR_factor_all 0.0828 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4864 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_gt 0.0675 _refine_ls_shift/su_max 0.000550 # 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: 10.9 1.77 8.89 3.38 ; _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # Some potentially useful phrases are: ; Hydrogen were now refined using a riding model with C-H distances restrained to 1.0 \%A and with Uiso=1.2 Uequiv C Small and bad quality crystal, ; _publ_section_exptl_prep ; ? ; # 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), 435-435 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 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. Oxford Diffraction, (2002) CrysAlis RED. Oxford Diffraction, (2002) Xcalibur User Manual 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 0.81529(4) 0.23807(5) 0.61444(3) 0.0220 1.0000 Uani . . . . . . Sb1 Sb 0.15833(5) 0.48322(6) 0.59084(4) 0.0454 1.0000 Uani . . . . . . P1 P 0.71341(14) 0.22087(14) 0.68720(10) 0.0225 1.0000 Uani . . . . . . P2 P 0.50587(14) 0.26189(15) 0.64444(9) 0.0202 1.0000 Uani . . . . . . Cl1 Cl 0.74024(16) 0.11384(16) 0.55268(11) 0.0330 1.0000 Uani . . . . . . N1 N 0.5307(4) 0.3567(5) 0.6160(3) 0.0209 1.0000 Uani . . . . . . N2 N 0.2712(5) 0.6789(5) 0.4428(3) 0.0215 1.0000 Uani . . . . . . C1 C 0.7323(6) 0.1188(7) 0.7372(4) 0.0319 1.0000 Uani . . . . . . C2 C 0.6432(7) 0.0852(7) 0.7468(5) 0.0420 1.0000 Uani . . . . . . C3 C 0.5838(7) 0.0927(6) 0.6769(5) 0.0356 1.0000 Uani . . . . . . C4 C 0.5993(5) 0.1874(6) 0.6475(4) 0.0241 1.0000 Uani . . . . . . C5 C 0.7117(6) 0.3141(6) 0.7467(4) 0.0255 1.0000 Uani . . . . . . C6 C 0.7179(6) 0.3001(8) 0.8146(4) 0.0357 1.0000 Uani . . . . . . C7 C 0.7200(7) 0.3735(9) 0.8580(5) 0.0483 1.0000 Uani . . . . . . C8 C 0.7188(7) 0.4618(9) 0.8340(5) 0.0468 1.0000 Uani . . . . . . C9 C 0.7114(7) 0.4767(7) 0.7652(5) 0.0381 1.0000 Uani . . . . . . C10 C 0.7084(6) 0.4030(6) 0.7219(4) 0.0300 1.0000 Uani . . . . . . C11 C 0.4733(5) 0.4189(5) 0.5830(4) 0.0203 1.0000 Uani . . . . . . C12 C 0.4263(5) 0.4079(5) 0.5171(4) 0.0176 1.0000 Uani . . . . . . C13 C 0.3771(5) 0.4726(6) 0.4841(4) 0.0223 1.0000 Uani . . . . . . C14 C 0.3693(5) 0.5586(6) 0.5110(4) 0.0189 1.0000 Uani . . . . . . C15 C 0.4162(5) 0.5736(5) 0.5759(4) 0.0188 1.0000 Uani . . . . . . C16 C 0.4656(5) 0.5072(6) 0.6102(3) 0.0188 1.0000 Uani . . . . . . C17 C 0.3164(6) 0.6272(6) 0.4753(4) 0.0278 1.0000 Uani . . . . . . C18 C 0.4162(5) 0.2028(6) 0.5948(4) 0.0217 1.0000 Uani . . . . . . C19 C 0.4267(7) 0.1309(6) 0.5498(4) 0.0320 1.0000 Uani . . . . . . C20 C 0.3538(8) 0.0959(8) 0.5093(5) 0.0441 1.0000 Uani . . . . . . C21 C 0.2728(9) 0.1269(8) 0.5102(5) 0.0561 1.0000 Uani . . . . . . C22 C 0.2590(8) 0.1998(9) 0.5529(5) 0.0516 1.0000 Uani . . . . . . C23 C 0.3317(6) 0.2363(7) 0.5944(5) 0.0344 1.0000 Uani . . . . . . C24 C 0.4749(6) 0.2717(6) 0.7267(4) 0.0243 1.0000 Uani . . . . . . C25 C 0.4230(6) 0.2057(6) 0.7523(4) 0.0279 1.0000 Uani . . . . . . C26 C 0.4009(7) 0.2168(7) 0.8152(5) 0.0408 1.0000 Uani . . . . . . C27 C 0.4284(7) 0.2913(7) 0.8528(5) 0.0365 1.0000 Uani . . . . . . C28 C 0.4792(7) 0.3577(6) 0.8298(5) 0.0356 1.0000 Uani . . . . . . C29 C 0.5021(6) 0.3474(6) 0.7662(4) 0.0238 1.0000 Uani . . . . . . C30 C 0.8999(8) 0.4467(8) 0.6508(6) 0.0513 1.0000 Uani . . . . . . C31 C 0.9537(8) 0.0554(8) 0.6144(6) 0.0513 1.0000 Uani . . . . . . C32 C 0.9261(8) -0.0061(8) 0.6634(6) 0.0513 1.0000 Uani . . . . . . C33 C 1.0506(8) 0.0413(8) 0.6141(6) 0.0513 1.0000 Uani . . . . . . C34 C 0.9405(8) 0.1572(8) 0.6270(6) 0.0513 1.0000 Uani . . . . . . C35 C 0.9279(8) 0.1922(9) 0.6893(6) 0.0513 1.0000 Uani . . . . . . C36 C 0.9125(8) 0.2847(8) 0.6973(6) 0.0513 1.0000 Uani . . . . . . C37 C 0.9135(8) 0.3482(9) 0.6433(6) 0.0513 1.0000 Uani . . . . . . C38 C 0.9258(8) 0.3117(9) 0.5805(6) 0.0513 1.0000 Uani . . . . . . C39 C 0.9387(8) 0.2189(8) 0.5724(6) 0.0513 1.0000 Uani . . . . . . F1 F 0.4361(4) 0.3280(3) 0.4852(2) 0.0303 1.0000 Uani . . . . . . F2 F 0.3342(3) 0.4571(3) 0.4202(2) 0.0311 1.0000 Uani . . . . . . F3 F 0.4088(3) 0.6554(3) 0.6041(2) 0.0298 1.0000 Uani . . . . . . F4 F 0.5090(3) 0.5249(4) 0.6719(2) 0.0288 1.0000 Uani . . . . . . F5 F 0.1042(6) 0.3704(6) 0.5854(5) 0.0846 1.0000 Uani . . . . . . F6 F 0.2139(5) 0.5968(5) 0.5963(3) 0.0606 1.0000 Uani . . . . . . F7 F 0.0547(5) 0.5402(7) 0.5501(5) 0.0937 1.0000 Uani . . . . . . F8 F 0.2641(5) 0.4343(5) 0.6339(5) 0.0763 1.0000 Uani . . . . . . F9 F 0.1234(5) 0.5027(6) 0.6741(3) 0.0742 1.0000 Uani . . . . . . F10 F 0.1910(6) 0.4648(7) 0.5067(4) 0.0908 1.0000 Uani . . . . . . O1 O 0.9229(9) 0.7525(8) 0.1774(7) 0.098(4) 1.0000 Uiso . . . . . . C40 C 0.8308(18) 0.7276(17) 0.2581(13) 0.141(9) 1.0000 Uiso . . . . . . C41 C 0.8433(18) 0.7686(19) 0.1937(14) 0.147(9) 1.0000 Uiso . . . . . . C42 C 0.9397(16) 0.7878(17) 0.1137(13) 0.124(7) 1.0000 Uiso . . . . . . C43 C 1.0262(18) 0.7625(18) 0.1064(14) 0.151(10) 1.0000 Uiso . . . . . . H11 H 0.7691 0.1328 0.7817 0.0379 1.0000 Uiso R . . . . . H12 H 0.7626 0.0720 0.7134 0.0379 1.0000 Uiso R . . . . . H21 H 0.6195 0.1237 0.7805 0.0513 1.0000 Uiso R . . . . . H22 H 0.6470 0.0205 0.7623 0.0513 1.0000 Uiso R . . . . . H31 H 0.5208 0.0864 0.6819 0.0450 1.0000 Uiso R . . . . . H32 H 0.5993 0.0439 0.6465 0.0450 1.0000 Uiso R . . . . . H41 H 0.6032 0.1753 0.5993 0.0308 1.0000 Uiso R . . . . . H61 H 0.7208 0.2367 0.8329 0.0434 1.0000 Uiso R . . . . . H71 H 0.7226 0.3625 0.9072 0.0578 1.0000 Uiso R . . . . . H81 H 0.7231 0.5144 0.8659 0.0559 1.0000 Uiso R . . . . . H91 H 0.7082 0.5402 0.7470 0.0459 1.0000 Uiso R . . . . . H101 H 0.7038 0.4137 0.6725 0.0348 1.0000 Uiso R . . . . . H191 H 0.4863 0.1060 0.5476 0.0378 1.0000 Uiso R . . . . . H201 H 0.3618 0.0452 0.4778 0.0513 1.0000 Uiso R . . . . . H211 H 0.2216 0.0984 0.4805 0.0636 1.0000 Uiso R . . . . . H221 H 0.1987 0.2244 0.5533 0.0599 1.0000 Uiso R . . . . . H231 H 0.3232 0.2880 0.6248 0.0398 1.0000 Uiso R . . . . . H251 H 0.4019 0.1510 0.7248 0.0352 1.0000 Uiso R . . . . . H261 H 0.3646 0.1696 0.8333 0.0499 1.0000 Uiso R . . . . . H271 H 0.4114 0.2983 0.8982 0.0447 1.0000 Uiso R . . . . . H281 H 0.4992 0.4120 0.8582 0.0440 1.0000 Uiso R . . . . . H291 H 0.5385 0.3952 0.7489 0.0293 1.0000 Uiso R . . . . . H311 H 0.9207 0.0395 0.5688 0.0615 1.0000 Uiso R . . . . . H321 H 0.8621 0.0028 0.6638 0.0615 1.0000 Uiso R . . . . . H322 H 0.9602 0.0073 0.7090 0.0615 1.0000 Uiso R . . . . . H323 H 0.9369 -0.0705 0.6509 0.0615 1.0000 Uiso R . . . . . H331 H 1.0703 0.0832 0.5806 0.0615 1.0000 Uiso R . . . . . H332 H 1.0843 0.0546 0.6598 0.0615 1.0000 Uiso R . . . . . H333 H 1.0611 -0.0232 0.6018 0.0615 1.0000 Uiso R . . . . . H351 H 0.9301 0.1505 0.7287 0.0615 1.0000 Uiso R . . . . . H361 H 0.9004 0.3075 0.7415 0.0615 1.0000 Uiso R . . . . . H301 H 0.9032 0.4781 0.6074 0.0617 1.0000 Uiso R . . . . . H302 H 0.9465 0.4713 0.6868 0.0617 1.0000 Uiso R . . . . . H303 H 0.8409 0.4574 0.6634 0.0617 1.0000 Uiso R . . . . . H421 H 0.9340 0.8557 0.1132 0.1484 1.0000 Uiso R . . . . . H422 H 0.8964 0.7615 0.0761 0.1484 1.0000 Uiso R . . . . . H431 H 1.0388 0.7864 0.0626 0.1834 1.0000 Uiso R . . . . . H432 H 1.0691 0.7889 0.1442 0.1834 1.0000 Uiso R . . . . . H433 H 1.0314 0.6947 0.1071 0.1834 1.0000 Uiso R . . . . . H411 H 0.8353 0.8359 0.1970 0.1770 1.0000 Uiso R . . . . . H412 H 0.7975 0.7434 0.1574 0.1770 1.0000 Uiso R . . . . . H401 H 0.7707 0.7418 0.2675 0.1697 1.0000 Uiso R . . . . . H402 H 0.8758 0.7526 0.2951 0.1697 1.0000 Uiso R . . . . . H403 H 0.8380 0.6601 0.2555 0.1697 1.0000 Uiso R . . . . . H381 H 0.9253 0.3535 0.5413 0.0617 1.0000 Uiso R . . . . . H391 H 0.9468 0.1951 0.5274 0.0617 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 0.0230(3) 0.0252(4) 0.0179(3) -0.0001(3) 0.0035(2) 0.0041(3) Sb1 0.0341(4) 0.0691(5) 0.0353(4) -0.0162(4) 0.0129(3) -0.0224(4) P1 0.0281(11) 0.0211(12) 0.0185(9) 0.0034(8) 0.0045(8) 0.0055(9) P2 0.0257(10) 0.0182(10) 0.0168(9) 0.0028(8) 0.0042(7) -0.0025(9) Cl1 0.0411(13) 0.0305(12) 0.0287(11) -0.0081(9) 0.0094(9) 0.0009(10) N1 0.020(3) 0.021(4) 0.022(3) 0.005(3) 0.005(3) 0.001(3) N2 0.029(4) 0.016(4) 0.020(3) -0.006(3) 0.005(3) 0.003(3) C1 0.039(5) 0.035(6) 0.020(4) 0.011(4) 0.001(4) 0.005(4) C2 0.053(7) 0.030(6) 0.045(6) 0.013(5) 0.017(5) 0.006(5) C3 0.038(5) 0.021(5) 0.052(6) 0.013(4) 0.020(5) 0.000(4) C4 0.021(4) 0.029(5) 0.026(4) 0.005(4) 0.016(3) 0.008(4) C5 0.030(5) 0.027(5) 0.018(4) 0.001(3) -0.001(3) 0.010(4) C6 0.034(5) 0.057(6) 0.018(4) 0.001(4) 0.007(4) 0.001(5) C7 0.042(6) 0.081(9) 0.022(5) -0.015(5) 0.007(4) 0.000(6) C8 0.038(6) 0.066(8) 0.036(5) -0.021(5) 0.005(4) 0.001(5) C9 0.041(6) 0.027(5) 0.048(6) -0.016(4) 0.010(4) -0.004(4) C10 0.026(5) 0.037(5) 0.024(4) -0.004(4) -0.005(3) 0.000(4) C11 0.028(4) 0.019(4) 0.016(4) -0.002(3) 0.012(3) -0.004(3) C12 0.020(4) 0.014(4) 0.018(4) 0.002(3) 0.002(3) -0.003(3) C13 0.019(4) 0.027(5) 0.022(4) -0.006(3) 0.005(3) -0.004(3) C14 0.019(4) 0.022(4) 0.015(3) 0.004(3) 0.002(3) -0.002(3) C15 0.018(4) 0.012(4) 0.028(4) -0.002(3) 0.011(3) 0.000(3) C16 0.013(3) 0.030(5) 0.012(3) -0.003(3) -0.001(3) -0.002(3) C17 0.031(5) 0.034(5) 0.019(4) -0.007(4) 0.007(3) -0.003(4) C18 0.028(4) 0.018(4) 0.017(3) 0.002(3) -0.002(3) -0.010(3) C19 0.049(6) 0.023(5) 0.023(4) -0.009(4) 0.003(4) -0.015(4) C20 0.056(7) 0.044(6) 0.028(5) -0.006(4) -0.006(5) -0.024(5) C21 0.072(9) 0.052(8) 0.035(6) -0.002(5) -0.017(6) -0.042(7) C22 0.039(6) 0.072(8) 0.039(6) 0.015(6) -0.007(5) -0.009(6) C23 0.035(5) 0.030(5) 0.034(4) 0.004(4) -0.006(4) -0.003(4) C24 0.033(4) 0.025(4) 0.016(3) 0.004(3) 0.006(3) 0.008(4) C25 0.036(5) 0.027(5) 0.025(4) 0.007(3) 0.017(4) 0.004(4) C26 0.054(7) 0.038(6) 0.035(5) 0.008(4) 0.020(5) 0.008(5) C27 0.044(6) 0.044(6) 0.023(4) 0.009(4) 0.012(4) 0.017(5) C28 0.058(6) 0.026(5) 0.026(4) -0.003(4) 0.017(4) 0.006(5) C29 0.032(5) 0.022(4) 0.019(4) 0.007(3) 0.009(3) 0.000(3) C30 0.0514(7) 0.0514(7) 0.0514(7) 0.0014(7) 0.0099(7) 0.0014(7) C31 0.0514(7) 0.0514(7) 0.0514(7) 0.0014(7) 0.0099(7) 0.0014(7) C32 0.0514(7) 0.0514(7) 0.0514(7) 0.0014(7) 0.0099(7) 0.0014(7) C33 0.0514(7) 0.0514(7) 0.0514(7) 0.0014(7) 0.0099(7) 0.0014(7) C34 0.0514(7) 0.0514(7) 0.0514(7) 0.0014(7) 0.0099(7) 0.0014(7) C35 0.0514(7) 0.0514(7) 0.0514(7) 0.0014(7) 0.0099(7) 0.0014(7) C36 0.0514(7) 0.0514(7) 0.0514(7) 0.0014(7) 0.0099(7) 0.0014(7) C37 0.0514(7) 0.0514(7) 0.0514(7) 0.0014(7) 0.0099(7) 0.0014(7) C38 0.0514(7) 0.0514(7) 0.0514(7) 0.0014(7) 0.0099(7) 0.0014(7) C39 0.0514(7) 0.0514(7) 0.0514(7) 0.0014(7) 0.0099(7) 0.0014(7) F1 0.052(3) 0.022(3) 0.015(2) -0.0025(19) 0.000(2) 0.003(2) F2 0.044(3) 0.037(3) 0.011(2) -0.0018(19) 0.001(2) -0.001(2) F3 0.040(3) 0.019(3) 0.030(3) -0.009(2) 0.003(2) 0.000(2) F4 0.033(3) 0.033(3) 0.018(2) -0.005(2) -0.002(2) -0.001(2) F5 0.087(6) 0.085(6) 0.090(6) -0.023(5) 0.038(5) -0.047(5) F6 0.077(5) 0.061(4) 0.049(4) -0.011(3) 0.024(3) -0.021(4) F7 0.051(5) 0.142(9) 0.082(6) -0.027(6) -0.009(4) 0.003(5) F8 0.061(5) 0.059(5) 0.104(7) -0.021(4) -0.001(4) -0.016(4) F9 0.058(4) 0.128(7) 0.043(3) -0.028(4) 0.025(3) -0.041(5) F10 0.080(6) 0.137(8) 0.068(5) -0.058(5) 0.047(4) -0.061(6) _refine_ls_extinction_method None 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 . N2 2_666 2.022(7) yes Ru1 . P1 . 2.342(2) yes Ru1 . Cl1 . 2.396(2) yes Ru1 . C34 . 2.248(12) yes Ru1 . C35 . 2.208(12) yes Ru1 . C36 . 2.161(12) yes Ru1 . C37 . 2.227(12) yes Ru1 . C38 . 2.226(12) yes Ru1 . C39 . 2.233(12) yes Sb1 . F5 . 1.852(8) yes Sb1 . F6 . 1.871(7) yes Sb1 . F7 . 1.869(9) yes Sb1 . F8 . 1.861(8) yes Sb1 . F9 . 1.872(6) yes Sb1 . F10 . 1.872(7) yes P1 . C1 . 1.804(9) yes P1 . C4 . 1.876(9) yes P1 . C5 . 1.825(9) yes P2 . N1 . 1.579(7) yes P2 . C4 . 1.805(8) yes P2 . C18 . 1.791(8) yes P2 . C24 . 1.811(8) yes N1 . C11 . 1.366(11) yes N2 . C17 . 1.157(11) yes C1 . C2 . 1.505(14) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . C3 . 1.551(15) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . C4 . 1.547(12) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . H41 . 1.000 no C5 . C6 . 1.375(11) yes C5 . C10 . 1.397(13) yes C6 . C7 . 1.386(15) yes C6 . H61 . 1.000 no C7 . C8 . 1.383(17) yes C7 . H71 . 1.000 no C8 . C9 . 1.392(15) yes C8 . H81 . 1.000 no C9 . C10 . 1.387(13) yes C9 . H91 . 1.000 no C10 . H101 . 1.000 no C11 . C12 . 1.412(11) yes C11 . C16 . 1.422(11) yes C12 . C13 . 1.324(12) yes C12 . F1 . 1.361(9) yes C13 . C14 . 1.389(12) yes C13 . F2 . 1.366(9) yes C14 . C15 . 1.403(11) yes C14 . C17 . 1.416(12) yes C15 . C16 . 1.355(11) yes C15 . F3 . 1.343(9) yes C16 . F4 . 1.335(8) yes C18 . C19 . 1.420(12) yes C18 . C23 . 1.394(13) yes C19 . C20 . 1.375(13) yes C19 . H191 . 1.000 no C20 . C21 . 1.336(18) yes C20 . H201 . 1.000 no C21 . C22 . 1.414(18) yes C21 . H211 . 1.000 no C22 . C23 . 1.390(14) yes C22 . H221 . 1.000 no C23 . H231 . 1.000 no C24 . C25 . 1.411(12) yes C24 . C29 . 1.392(12) yes C25 . C26 . 1.378(12) yes C25 . H251 . 1.000 no C26 . C27 . 1.360(15) yes C26 . H261 . 1.000 no C27 . C28 . 1.381(14) yes C27 . H271 . 1.000 no C28 . C29 . 1.395(11) yes C28 . H281 . 1.000 no C29 . H291 . 1.000 no C30 . C37 . 1.474(17) yes C30 . H301 . 1.000 no C30 . H302 . 1.000 no C30 . H303 . 1.000 no C31 . C32 . 1.456(16) yes C31 . C33 . 1.513(16) yes C31 . C34 . 1.536(17) yes C31 . H311 . 1.000 no C32 . H321 . 1.000 no C32 . H322 . 1.000 no C32 . H323 . 1.000 no C33 . H331 . 1.000 no C33 . H332 . 1.000 no C33 . H333 . 1.000 no C34 . C35 . 1.403(16) yes C34 . C39 . 1.423(16) yes C35 . C36 . 1.393(17) yes C35 . H351 . 1.000 no C36 . C37 . 1.437(17) yes C36 . H361 . 1.000 no C37 . C38 . 1.418(16) yes C38 . C39 . 1.392(17) yes C38 . H381 . 1.000 no C39 . H391 . 1.000 no O1 . C41 . 1.35(3) yes O1 . C42 . 1.45(3) yes C40 . C41 . 1.47(3) yes C40 . H401 . 1.000 no C40 . H402 . 1.000 no C40 . H403 . 1.000 no C41 . H411 . 1.000 no C41 . H412 . 1.000 no C42 . C43 . 1.42(3) yes C42 . H421 . 1.000 no C42 . H422 . 1.000 no C43 . H431 . 1.000 no C43 . H432 . 1.000 no C43 . H433 . 1.000 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 N2 2_666 Ru1 . P1 . 88.5(2) yes N2 2_666 Ru1 . Cl1 . 87.0(2) yes P1 . Ru1 . Cl1 . 85.77(8) yes N2 2_666 Ru1 . C34 . 148.9(4) yes P1 . Ru1 . C34 . 122.0(3) yes Cl1 . Ru1 . C34 . 89.3(3) yes N2 2_666 Ru1 . C35 . 160.6(4) yes P1 . Ru1 . C35 . 94.2(3) yes Cl1 . Ru1 . C35 . 112.3(3) yes C34 . Ru1 . C35 . 36.7(4) yes N2 2_666 Ru1 . C36 . 123.8(4) yes P1 . Ru1 . C36 . 90.1(3) yes Cl1 . Ru1 . C36 . 148.8(3) yes C34 . Ru1 . C36 . 66.9(5) yes C35 . Ru1 . C36 . 37.2(4) yes N2 2_666 Ru1 . C37 . 93.8(4) yes P1 . Ru1 . C37 . 114.5(3) yes Cl1 . Ru1 . C37 . 159.7(3) yes C34 . Ru1 . C37 . 79.5(5) yes C35 . Ru1 . C37 . 67.6(5) yes N2 2_666 Ru1 . C38 . 89.9(4) yes P1 . Ru1 . C38 . 151.4(3) yes Cl1 . Ru1 . C38 . 122.6(3) yes C34 . Ru1 . C38 . 66.5(4) yes C35 . Ru1 . C38 . 78.6(4) yes N2 2_666 Ru1 . C39 . 112.6(4) yes P1 . Ru1 . C39 . 158.9(3) yes Cl1 . Ru1 . C39 . 94.3(3) yes C34 . Ru1 . C39 . 37.0(4) yes C35 . Ru1 . C39 . 66.2(4) yes C36 . Ru1 . C37 . 38.2(4) yes C36 . Ru1 . C38 . 67.4(4) yes C37 . Ru1 . C38 . 37.1(4) yes C36 . Ru1 . C39 . 78.9(5) yes C37 . Ru1 . C39 . 66.6(4) yes C38 . Ru1 . C39 . 36.4(4) yes F5 . Sb1 . F6 . 179.5(4) yes F5 . Sb1 . F7 . 91.7(4) yes F6 . Sb1 . F7 . 88.7(4) yes F5 . Sb1 . F8 . 92.0(4) yes F6 . Sb1 . F8 . 87.6(3) yes F7 . Sb1 . F8 . 176.0(4) yes F5 . Sb1 . F9 . 89.6(4) yes F6 . Sb1 . F9 . 90.6(3) yes F7 . Sb1 . F9 . 88.3(4) yes F8 . Sb1 . F9 . 90.2(4) yes F5 . Sb1 . F10 . 90.3(4) yes F6 . Sb1 . F10 . 89.5(3) yes F7 . Sb1 . F10 . 90.5(4) yes F8 . Sb1 . F10 . 91.0(4) yes F9 . Sb1 . F10 . 178.8(4) yes Ru1 . P1 . C1 . 112.2(3) yes Ru1 . P1 . C4 . 116.3(3) yes C1 . P1 . C4 . 94.2(4) yes Ru1 . P1 . C5 . 114.7(3) yes C1 . P1 . C5 . 106.0(4) yes C4 . P1 . C5 . 111.2(4) yes N1 . P2 . C4 . 107.7(4) yes N1 . P2 . C18 . 115.9(4) yes C4 . P2 . C18 . 105.3(4) yes N1 . P2 . C24 . 112.5(4) yes C4 . P2 . C24 . 110.6(4) yes C18 . P2 . C24 . 104.6(4) yes P2 . N1 . C11 . 126.1(6) yes Ru1 2_666 N2 . C17 . 175.5(7) yes P1 . C1 . C2 . 106.2(7) yes P1 . C1 . H11 . 110.2 no C2 . C1 . H11 . 110.2 no P1 . C1 . H12 . 110.3 no C2 . C1 . H12 . 110.4 no H11 . C1 . H12 . 109.5 no C1 . C2 . C3 . 105.9(8) yes C1 . C2 . H21 . 110.5 no C3 . C2 . H21 . 110.5 no C1 . C2 . H22 . 110.2 no C3 . C2 . H22 . 110.2 no H21 . C2 . H22 . 109.5 no C2 . C3 . C4 . 107.9(8) yes C2 . C3 . H31 . 109.8 no C4 . C3 . H31 . 109.8 no C2 . C3 . H32 . 109.9 no C4 . C3 . H32 . 109.9 no H31 . C3 . H32 . 109.5 no C3 . C4 . P1 . 105.5(6) yes C3 . C4 . P2 . 112.6(6) yes P1 . C4 . P2 . 123.0(5) yes C3 . C4 . H41 . 104.7 no P1 . C4 . H41 . 104.8 no P2 . C4 . H41 . 104.7 no P1 . C5 . C6 . 122.5(7) yes P1 . C5 . C10 . 118.1(6) yes C6 . C5 . C10 . 119.3(8) yes C5 . C6 . C7 . 120.2(10) yes C5 . C6 . H61 . 119.9 no C7 . C6 . H61 . 119.9 no C6 . C7 . C8 . 120.8(9) yes C6 . C7 . H71 . 119.5 no C8 . C7 . H71 . 119.6 no C7 . C8 . C9 . 119.4(10) yes C7 . C8 . H81 . 120.3 no C9 . C8 . H81 . 120.3 no C8 . C9 . C10 . 119.6(10) yes C8 . C9 . H91 . 120.2 no C10 . C9 . H91 . 120.2 no C5 . C10 . C9 . 120.7(9) yes C5 . C10 . H101 . 119.7 no C9 . C10 . H101 . 119.7 no N1 . C11 . C12 . 124.8(7) yes N1 . C11 . C16 . 120.8(7) yes C12 . C11 . C16 . 113.8(7) yes C11 . C12 . C13 . 123.5(7) yes C11 . C12 . F1 . 117.6(7) yes C13 . C12 . F1 . 118.8(7) yes C12 . C13 . C14 . 122.4(7) yes C12 . C13 . F2 . 120.1(7) yes C14 . C13 . F2 . 117.5(7) yes C13 . C14 . C15 . 116.3(7) yes C13 . C14 . C17 . 121.9(7) yes C15 . C14 . C17 . 121.8(7) yes C14 . C15 . C16 . 121.4(7) yes C14 . C15 . F3 . 117.9(7) yes C16 . C15 . F3 . 120.6(7) yes C11 . C16 . C15 . 122.5(7) yes C11 . C16 . F4 . 118.4(7) yes C15 . C16 . F4 . 119.1(7) yes C14 . C17 . N2 . 175.4(9) yes P2 . C18 . C19 . 123.9(7) yes P2 . C18 . C23 . 117.9(7) yes C19 . C18 . C23 . 117.8(8) yes C18 . C19 . C20 . 119.3(10) yes C18 . C19 . H191 . 120.4 no C20 . C19 . H191 . 120.3 no C19 . C20 . C21 . 122.6(11) yes C19 . C20 . H201 . 118.7 no C21 . C20 . H201 . 118.7 no C20 . C21 . C22 . 120.4(10) yes C20 . C21 . H211 . 119.8 no C22 . C21 . H211 . 119.8 no C21 . C22 . C23 . 117.9(11) yes C21 . C22 . H221 . 121.0 no C23 . C22 . H221 . 121.0 no C18 . C23 . C22 . 122.0(10) yes C18 . C23 . H231 . 119.1 no C22 . C23 . H231 . 119.0 no P2 . C24 . C25 . 122.4(7) yes P2 . C24 . C29 . 119.2(6) yes C25 . C24 . C29 . 118.3(7) yes C24 . C25 . C26 . 120.1(9) yes C24 . C25 . H251 . 120.0 no C26 . C25 . H251 . 119.9 no C25 . C26 . C27 . 120.5(9) yes C25 . C26 . H261 . 119.8 no C27 . C26 . H261 . 119.7 no C26 . C27 . C28 . 121.5(9) yes C26 . C27 . H271 . 119.3 no C28 . C27 . H271 . 119.3 no C27 . C28 . C29 . 118.7(9) yes C27 . C28 . H281 . 120.6 no C29 . C28 . H281 . 120.7 no C28 . C29 . C24 . 120.9(8) yes C28 . C29 . H291 . 119.5 no C24 . C29 . H291 . 119.6 no C37 . C30 . H301 . 109.5 no C37 . C30 . H302 . 109.5 no H301 . C30 . H302 . 109.5 no C37 . C30 . H303 . 109.5 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no C32 . C31 . C33 . 108.7(10) yes C32 . C31 . C34 . 115.4(10) yes C33 . C31 . C34 . 107.0(10) yes C32 . C31 . H311 . 108.5 no C33 . C31 . H311 . 108.4 no C34 . C31 . H311 . 108.6 no C31 . C32 . H321 . 109.2 no C31 . C32 . H322 . 109.6 no H321 . C32 . H322 . 109.5 no C31 . C32 . H323 . 109.7 no H321 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no C31 . C33 . H331 . 109.5 no C31 . C33 . H332 . 109.4 no H331 . C33 . H332 . 109.5 no C31 . C33 . H333 . 109.5 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.5 no C31 . C34 . Ru1 . 129.1(9) yes C31 . C34 . C35 . 123.2(11) yes Ru1 . C34 . C35 . 70.1(7) yes C31 . C34 . C39 . 118.5(11) yes Ru1 . C34 . C39 . 70.9(7) yes C35 . C34 . C39 . 118.3(11) yes Ru1 . C35 . C34 . 73.2(7) yes Ru1 . C35 . C36 . 69.6(7) yes C34 . C35 . C36 . 120.9(12) yes Ru1 . C35 . H351 . 130.4 no C34 . C35 . H351 . 119.8 no C36 . C35 . H351 . 119.4 no Ru1 . C36 . C35 . 73.3(7) yes Ru1 . C36 . C37 . 73.4(7) yes C35 . C36 . C37 . 121.4(11) yes Ru1 . C36 . H361 . 125.9 no C35 . C36 . H361 . 119.5 no C37 . C36 . H361 . 119.1 no Ru1 . C37 . C30 . 129.6(9) yes Ru1 . C37 . C36 . 68.4(7) yes C30 . C37 . C36 . 122.6(11) yes Ru1 . C37 . C38 . 71.4(7) yes C30 . C37 . C38 . 120.4(11) yes C36 . C37 . C38 . 117.0(11) yes Ru1 . C38 . C37 . 71.5(7) yes Ru1 . C38 . C39 . 72.1(7) yes C37 . C38 . C39 . 121.2(11) yes Ru1 . C38 . H381 . 129.6 no C37 . C38 . H381 . 119.4 no C39 . C38 . H381 . 119.4 no Ru1 . C39 . C34 . 72.1(7) yes Ru1 . C39 . C38 . 71.5(7) yes C34 . C39 . C38 . 121.1(11) yes Ru1 . C39 . H391 . 129.5 no C34 . C39 . H391 . 119.4 no C38 . C39 . H391 . 119.4 no C41 . O1 . C42 . 117.5(19) yes C41 . C40 . H401 . 110.3 no C41 . C40 . H402 . 109.2 no H401 . C40 . H402 . 109.5 no C41 . C40 . H403 . 109.0 no H401 . C40 . H403 . 109.5 no H402 . C40 . H403 . 109.5 no C40 . C41 . O1 . 114(2) yes C40 . C41 . H411 . 108.1 no O1 . C41 . H411 . 108.5 no C40 . C41 . H412 . 108.3 no O1 . C41 . H412 . 108.5 no H411 . C41 . H412 . 109.5 no O1 . C42 . C43 . 108(2) yes O1 . C42 . H421 . 109.6 no C43 . C42 . H421 . 110.0 no O1 . C42 . H422 . 109.6 no C43 . C42 . H422 . 110.0 no H421 . C42 . H422 . 109.5 no C42 . C43 . H431 . 109.2 no C42 . C43 . H432 . 109.6 no H431 . C43 . H432 . 109.5 no C42 . C43 . H433 . 109.6 no H431 . C43 . H433 . 109.5 no H432 . C43 . H433 . 109.5 no