data_global # # Reactivity of the Chiral Metallic Bronsted Acid # [(n6-p-MeC6H4iPr)Ru(K3 P,O,O-POH)][SbF6]2 # (POH=(SC1,RC2)-Ph2PC(Ph)HC(OH)(HCH2OMe) # toward Aldimines # # # by Pilar Pardo, Daniel Carmona, Pilar Lamata, Ricardo Rodriguez, # Fernando J. Lahoz, Pilar Garcia-Ordu\~a, Luis A. Oro # # # Submitted to Organometallics # Manuscript number ........... # ----------------------------------------------------------- # # Person for contact _publ_contact_author_name 'Dr. Fernando J. Lahoz' _publ_contact_author_address ; Dr. Fernando J. Lahoz Departamento de Qu\'imica Inorg\'anica Instituto de S\'intesis Qu\'imica y Cat\'alisis Homog\'enea - ISQCH Universidad de Zaragoza - C.S.I.C. C/ Pedro Cerbuna, 12 50009 Zaragoza, Spain ; _publ_contact_author_phone '+34 976 761147' _publ_contact_author_fax '+34 976 761187' _publ_contact_author_email lahoz@unizar.es # ------------------------------------------------------------ # Publication details loop_ _publ_author_name 'Pardo, P.' 'Carmona,D.' 'Lamata, P.' 'Rodriguez, R.' 'Lahoz, F.J.' 'Garcia-Ordu\~a,P.' 'Oro,L.A.' _publ_requested_journal 'Organometallics' _journal_name_full ' Organometallics' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '2014' # ---------------------------------------------------------- # Data for cmpnd_3 (local labelling as fjl250as; PPA-568) data_cmpnd_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H41 N O2 P Ru, F6 Sb, C H2 Cl2, H2 O' _chemical_formula_sum 'C39 H45 Cl2 F6 N O3 P Ru Sb' _chemical_formula_weight 1014.45 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' 'F' 'F' 0.0171 0.0103 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.2729(5) _cell_length_b 16.6169(8) _cell_length_c 25.1147(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.749(5) _cell_angle_gamma 90.00 _cell_volume 4225.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9145 _cell_measurement_theta_min 2.355 _cell_measurement_theta_max 27.823 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.217 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.158 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7782 _exptl_absorpt_correction_T_max 0.8461 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX CCD system' _diffrn_measurement_method 'narrow \w frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 72100 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.89 _reflns_number_total 9971 _reflns_number_gt 9301 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, PLATON(Spek, 1998)' _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. Asymmetric unit contains a Ru complex, a SbF6 counterion, and a dichloromethane and a water solvent molecules. Two phenyl rings of the Ru-complex molecules have been found to be disordered. Carbon atoms have been included in the model in two sets of positions, with complementary occupancy factors: refined 0.57/0.43 for C11-C16 phenyl ring and fixed 0.5/0.5 for three carbon atoms of C27-C32 phenyl ring (the refinement of their ocuppancy factors leads to 0.5/0.5 values, so they have been fixed). Disordered atoms have been isotropically refined. Dichloromethane molecule has also been found to be disordered in two parts. Carbon atom of the majoritary part and one chlorine atom of the minoritary one share the positions. They have been refined with EXYZ and EADP commands. Most of the hydrogen atoms have been included in the model in calculated positions and refined with a riding model. Those of water molecule have been observed in Fourier difference map, and refined with geometrical restraints and their parameter related to that of the oxygen atom. At the end of the refinement, residual density peaks are located around Sb atom and in the region of disordered dichloromethane molecule. Attempts to include these peaks in the model (even like highly disordered hexane molecule) leads to unrealistic parameters. ; _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^)+(0.0411P)^2^+16.9932P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9971 _refine_ls_number_parameters 475 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl250as in P 1 21/c 1 CELL 0.71073 10.2729 16.6169 25.1147 90.000 99.749 90.000 ZERR 4.00 0.0005 0.0008 0.0012 0.000 0.005 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H F N O P RU SB CL UNIT 156 180 24 4 12 4 4 4 8 MERG 2 OMIT 0 1 1 OMIT -1 4 1 EXYZ C50A CL1B EADP C50A CL1B DFIX 0.96 0.010 O3 H1W O3 H2W FMAP 2 PLAN 20 ACTA BOND $H CONF WPDB -2 L.S. 4 TEMP -173.00 WGHT 0.041100 16.993200 FVAR 0.21533 0.56911 MOLE 1 RU 7 0.062037 0.858826 0.181685 11.00000 0.01658 0.01763 = 0.01558 0.00142 0.00477 0.00033 P1 6 -0.106829 0.764652 0.161226 11.00000 0.03006 0.02112 = 0.01593 0.00062 0.00649 -0.00739 O1 5 0.172564 0.763183 0.161512 11.00000 0.03374 0.02273 = 0.03325 0.00282 0.01715 0.00639 O2 5 0.283360 0.649331 0.096246 11.00000 0.09341 0.04061 = 0.07757 0.01662 0.06254 0.02699 N1 4 0.032103 0.879894 0.094527 11.00000 0.02412 0.02337 = 0.01608 0.00034 0.00589 -0.00315 H1N 2 0.062402 0.838337 0.080742 11.00000 0.02111 H2N 2 -0.048587 0.879194 0.082541 11.00000 0.03250 C1 1 0.249072 0.912434 0.231980 11.00000 0.01674 0.02910 = 0.01962 -0.00016 0.00076 -0.00005 C2 1 0.175622 0.974508 0.203612 11.00000 0.01985 0.02281 = 0.01963 -0.00226 0.00426 -0.00492 AFIX 43 H2 2 0.217546 1.010207 0.182282 11.00000 -1.20000 AFIX 0 C3 1 0.037566 0.985311 0.206141 11.00000 0.02020 0.01902 = 0.01903 -0.00281 0.00140 0.00014 AFIX 43 H3 2 -0.011398 1.025614 0.184581 11.00000 -1.20000 AFIX 0 C4 1 -0.025983 0.936864 0.240198 11.00000 0.01826 0.02779 = 0.01793 -0.00670 0.00393 -0.00255 C5 1 0.047476 0.871893 0.268091 11.00000 0.02317 0.02822 = 0.01629 -0.00004 0.00509 -0.00473 AFIX 43 H5 2 0.006500 0.837435 0.290516 11.00000 -1.20000 AFIX 0 C6 1 0.179822 0.858537 0.262632 11.00000 0.02301 0.02850 = 0.01893 0.00463 0.00028 0.00251 AFIX 43 H6 2 0.224791 0.812896 0.279541 11.00000 -1.20000 AFIX 0 C7 1 0.394052 0.896170 0.230042 11.00000 0.01727 0.04706 = 0.02752 0.00298 0.00355 0.00509 AFIX 2 H7 2 0.400099 0.837595 0.219149 11.00000 -1.20000 AFIX 0 C8 1 0.451619 0.948056 0.189729 11.00000 0.01992 0.10121 = 0.03786 0.02199 0.00921 0.00575 AFIX 137 H8A 2 0.402024 0.938933 0.153332 11.00000 -1.50000 H8B 2 0.544476 0.933689 0.190593 11.00000 -1.50000 H8C 2 0.445388 1.004924 0.199328 11.00000 -1.50000 AFIX 0 C9 1 0.475120 0.905334 0.286846 11.00000 0.02042 0.07341 = 0.03155 0.00464 -0.00062 -0.00235 AFIX 137 H9A 2 0.471126 0.961326 0.298718 11.00000 -1.50000 H9B 2 0.567188 0.890550 0.286194 11.00000 -1.50000 H9C 2 0.438877 0.869985 0.311943 11.00000 -1.50000 AFIX 0 C10 1 -0.165893 0.952762 0.248657 11.00000 0.02121 0.03980 = 0.02914 -0.00670 0.00931 -0.00049 AFIX 137 H10A 2 -0.164327 0.981374 0.282881 11.00000 -1.50000 H10B 2 -0.212582 0.901509 0.249711 11.00000 -1.50000 H10C 2 -0.211491 0.985713 0.218864 11.00000 -1.50000 PART 1 AFIX 66 C11A 1 -0.252965 0.804253 0.108474 21.00000 0.01890 C12A 1 -0.285025 0.885377 0.110147 21.00000 0.01880 AFIX 43 H12A 2 -0.233849 0.919954 0.135643 21.00000 -1.20000 AFIX 65 C13A 1 -0.391962 0.915910 0.074516 21.00000 0.02011 AFIX 43 H13A 2 -0.413873 0.971354 0.075660 21.00000 -1.20000 AFIX 65 C14A 1 -0.466841 0.865319 0.037212 21.00000 0.02115 AFIX 43 H14A 2 -0.539928 0.886187 0.012860 21.00000 -1.20000 AFIX 65 C15A 1 -0.434782 0.784195 0.035539 21.00000 0.02379 AFIX 43 H15A 2 -0.485959 0.749619 0.010043 21.00000 -1.20000 AFIX 65 C16A 1 -0.327845 0.753662 0.071169 21.00000 0.02547 AFIX 43 H16A 2 -0.305935 0.698217 0.070025 21.00000 -1.20000 PART 2 AFIX 66 C11B 1 -0.228917 0.788474 0.106570 -21.00000 0.01645 C12B 1 -0.278714 0.866042 0.108237 -21.00000 0.02100 AFIX 43 H12B 2 -0.238454 0.902853 0.134989 -21.00000 -1.20000 AFIX 65 C13B 1 -0.387416 0.889752 0.070762 -21.00000 0.02609 AFIX 43 H13B 2 -0.421450 0.942767 0.071902 -21.00000 -1.20000 AFIX 65 C14B 1 -0.446323 0.835893 0.031620 -21.00000 0.02581 AFIX 43 H14B 2 -0.520616 0.852098 0.006007 -21.00000 -1.20000 AFIX 65 C15B 1 -0.396527 0.758324 0.029952 -21.00000 0.03101 AFIX 43 H15B 2 -0.436788 0.721514 0.003200 -21.00000 -1.20000 AFIX 65 C16B 1 -0.287825 0.734614 0.067427 -21.00000 0.02481 AFIX 43 H16B 2 -0.253792 0.681599 0.066287 -21.00000 -1.20000 AFIX 0 PART 0 C17 1 -0.195887 0.730785 0.214644 11.00000 0.02983 0.01957 = 0.01994 0.00070 0.00873 -0.00545 C18 1 -0.333687 0.735251 0.210484 11.00000 0.02934 0.03084 = 0.02745 0.00739 0.00558 -0.00407 AFIX 43 H18 2 -0.385797 0.755984 0.178567 11.00000 -1.20000 AFIX 0 C19 1 -0.394447 0.709223 0.253263 11.00000 0.03017 0.03720 = 0.03967 0.00946 0.01450 -0.00020 AFIX 43 H19 2 -0.487872 0.711312 0.250028 11.00000 -1.20000 AFIX 0 C20 1 -0.318353 0.680263 0.300568 11.00000 0.04250 0.02613 = 0.02910 0.00586 0.02032 -0.00007 AFIX 43 H20 2 -0.359624 0.663620 0.329847 11.00000 -1.20000 AFIX 0 C21 1 -0.182066 0.675778 0.304828 11.00000 0.04154 0.02008 = 0.01947 0.00286 0.01006 0.00054 AFIX 43 H21 2 -0.130205 0.656255 0.337176 11.00000 -1.20000 AFIX 0 C22 1 -0.120690 0.699752 0.261919 11.00000 0.02977 0.02105 = 0.02254 0.00141 0.00880 -0.00087 AFIX 43 H22 2 -0.027606 0.695007 0.264785 11.00000 -1.20000 AFIX 0 C23 1 -0.018881 0.680199 0.140187 11.00000 0.06341 0.01873 = 0.02953 -0.00272 0.02557 -0.00777 C24 1 0.114284 0.694389 0.145924 11.00000 0.05840 0.01992 = 0.03441 0.00438 0.02809 0.00469 C25 1 0.214970 0.628885 0.138952 11.00000 0.09347 0.02776 = 0.06927 0.01065 0.05711 0.01967 AFIX 23 H25A 2 0.278849 0.622825 0.172951 11.00000 -1.20000 H25B 2 0.168921 0.576842 0.130909 11.00000 -1.20000 AFIX 0 C26 1 0.396724 0.597122 0.094033 11.00000 0.12938 0.06383 = 0.13004 0.01598 0.08736 0.03876 AFIX 137 H26A 2 0.459508 0.601617 0.127931 11.00000 -1.50000 H26B 2 0.439952 0.613483 0.063835 11.00000 -1.50000 H26C 2 0.366762 0.541239 0.088849 11.00000 -1.50000 AFIX 0 C27 1 -0.085949 0.605280 0.116562 11.00000 0.09851 0.02280 = 0.03850 -0.00809 0.03468 -0.02250 PART 1 C28A 1 -0.104398 0.589391 0.058649 10.50000 0.02676 AFIX 43 H28A 2 -0.069078 0.626756 0.036257 10.50000 -1.20000 AFIX 0 C29A 1 -0.171542 0.521848 0.034292 10.50000 0.03374 AFIX 43 H29A 2 -0.168478 0.509269 -0.002374 10.50000 -1.20000 AFIX 0 C30A 1 -0.243182 0.473080 0.064503 10.50000 0.03522 AFIX 43 H30A 2 -0.300766 0.432077 0.048026 10.50000 -1.20000 AFIX 0 PART 2 C28B 1 -0.036973 0.573476 0.070155 10.50000 0.04004 AFIX 43 H28B 2 0.030490 0.600446 0.055521 10.50000 -1.20000 AFIX 0 C29B 1 -0.091678 0.502219 0.047630 10.50000 0.05469 AFIX 43 H29B 2 -0.070540 0.483548 0.014372 10.50000 -1.20000 AFIX 0 C30B 1 -0.178467 0.457614 0.074053 10.50000 0.04388 AFIX 43 H30B 2 -0.206605 0.405962 0.060518 10.50000 -1.20000 AFIX 0 PART 0 C31 1 -0.225580 0.487879 0.120773 11.00000 0.08928 0.03036 = 0.04684 0.00065 0.02258 -0.02524 AFIX 2 H31 2 -0.276291 0.456438 0.140099 11.00000 -1.20000 AFIX 0 C32 1 -0.163632 0.557104 0.144490 11.00000 0.06139 0.02519 = 0.02889 0.00196 0.01374 -0.01042 AFIX 2 H32 2 -0.176188 0.572265 0.178340 11.00000 -1.20000 AFIX 0 C33 1 0.085277 0.953347 0.075617 11.00000 0.02022 0.02317 = 0.01412 0.00106 0.00263 -0.00312 C34 1 0.009890 1.023149 0.070066 11.00000 0.02474 0.02813 = 0.01636 0.00069 0.00343 0.00324 AFIX 43 H34 2 -0.077391 1.022782 0.077903 11.00000 -1.20000 AFIX 0 C35 1 0.063435 1.094023 0.052843 11.00000 0.04753 0.02074 = 0.01950 0.00064 0.00282 0.00068 AFIX 43 H35 2 0.012542 1.142053 0.049051 11.00000 -1.20000 AFIX 0 C36 1 0.191569 1.094212 0.041229 11.00000 0.04569 0.03299 = 0.02426 0.00667 0.00023 -0.01778 AFIX 43 H36 2 0.228119 1.142458 0.029806 11.00000 -1.20000 AFIX 0 C37 1 0.265184 1.024307 0.046340 11.00000 0.02310 0.05099 = 0.02742 0.01243 0.00300 -0.01118 AFIX 43 H37 2 0.352279 1.024601 0.038300 11.00000 -1.20000 AFIX 0 C38 1 0.212520 0.953243 0.063231 11.00000 0.01972 0.03533 = 0.02378 0.00766 0.00464 0.00345 AFIX 43 H38 2 0.263039 0.905070 0.066276 11.00000 -1.20000 AFIX 0 MOLE 2 SB 8 0.302481 0.672929 0.376394 11.00000 0.01969 0.03426 = 0.02114 0.00678 0.00013 -0.00555 F1 3 0.128474 0.705509 0.352992 11.00000 0.02459 0.23993 = 0.05133 0.05595 0.00162 0.02762 F2 3 0.474836 0.639498 0.400243 11.00000 0.03375 0.12054 = 0.03700 0.01640 0.00610 0.03246 F3 3 0.336147 0.682376 0.305632 11.00000 0.04505 0.10287 = 0.03030 0.02482 0.01425 0.00568 F4 3 0.264755 0.664132 0.447017 11.00000 0.03650 0.07353 = 0.02102 0.00151 0.00373 0.01111 F5 3 0.247938 0.567405 0.363777 11.00000 0.15426 0.06239 = 0.08308 -0.03522 0.06315 -0.06659 F6 3 0.350443 0.779527 0.389601 11.00000 0.13832 0.03369 = 0.15001 -0.00687 0.07101 -0.01574 MOLE 3 PART 3 C50A 1 0.314311 0.331934 0.084683 10.50000 0.15424 AFIX 23 H50A 2 0.362406 0.303326 0.116644 10.50000 -1.20000 H50B 2 0.283283 0.289964 0.057507 10.50000 -1.20000 AFIX 0 CL1A 9 0.424683 0.382823 0.060329 10.50000 0.06822 CL2A 9 0.179489 0.368998 0.103614 10.50000 0.08802 PART 4 C50B 1 0.144014 0.314717 0.079018 10.50000 0.06900 AFIX 23 H50C 2 0.108929 0.301964 0.040774 10.50000 -1.20000 H50D 2 0.131542 0.266259 0.100529 10.50000 -1.20000 AFIX 0 CL1B 9 0.314311 0.331934 0.084683 10.50000 0.15424 CL2B 9 0.058133 0.383706 0.097025 10.50000 0.14951 MOLE 4 PART 0 O3 5 0.133293 0.756651 0.025971 11.00000 0.10671 0.04618 = 0.05527 0.01269 0.04917 0.02039 H1W 2 0.199397 0.718827 0.042527 11.00000 -1.20000 H2W 2 0.186129 0.780337 0.001975 11.00000 -1.20000 HKLF 4 REM fjl250as in P 1 21/c 1 REM R1 = 0.0417 for 9301 Fo > 4sig(Fo) and 0.0445 for all 9971 data REM 475 parameters refined using 2 restraints END ; 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 Ru Ru 0.06204(2) 0.858826(14) 0.181685(9) 0.01636(7) Uani 1 1 d . A . P1 P -0.10683(9) 0.76465(5) 0.16123(3) 0.02207(17) Uani 1 1 d . . . O1 O 0.1726(3) 0.76318(14) 0.16151(10) 0.0286(5) Uani 1 1 d . . . O2 O 0.2834(4) 0.6493(2) 0.09625(17) 0.0649(12) Uani 1 1 d . A . N1 N 0.0321(3) 0.87989(17) 0.09453(11) 0.0209(5) Uani 1 1 d . . . H1N H 0.062(4) 0.838(2) 0.0807(16) 0.021(10) Uiso 1 1 d . . . H2N H -0.049(5) 0.879(3) 0.0825(18) 0.033(11) Uiso 1 1 d . . . C1 C 0.2491(3) 0.9124(2) 0.23198(13) 0.0221(6) Uani 1 1 d . . . C2 C 0.1756(3) 0.97451(19) 0.20361(12) 0.0207(6) Uani 1 1 d . A . H2 H 0.2175 1.0102 0.1823 0.025 Uiso 1 1 calc R . . C3 C 0.0376(3) 0.98531(19) 0.20614(12) 0.0196(6) Uani 1 1 d . . . H3 H -0.0114 1.0256 0.1846 0.024 Uiso 1 1 calc R A . C4 C -0.0260(3) 0.9369(2) 0.24020(12) 0.0212(6) Uani 1 1 d . A . C5 C 0.0475(3) 0.8719(2) 0.26809(12) 0.0224(6) Uani 1 1 d . . . H5 H 0.0065 0.8374 0.2905 0.027 Uiso 1 1 calc R A . C6 C 0.1798(3) 0.8585(2) 0.26263(13) 0.0239(6) Uani 1 1 d . A . H6 H 0.2248 0.8129 0.2795 0.029 Uiso 1 1 calc R . . C7 C 0.3941(3) 0.8962(3) 0.23004(15) 0.0306(8) Uani 1 1 d . A . H7 H 0.400(4) 0.838(3) 0.2191(19) 0.037 Uiso 1 1 d . . . C8 C 0.4516(4) 0.9481(4) 0.18973(18) 0.0525(13) Uani 1 1 d . . . H8A H 0.4020 0.9389 0.1533 0.079 Uiso 1 1 calc R A . H8B H 0.5445 0.9337 0.1906 0.079 Uiso 1 1 calc R . . H8C H 0.4454 1.0049 0.1993 0.079 Uiso 1 1 calc R . . C9 C 0.4751(4) 0.9053(3) 0.28685(16) 0.0424(10) Uani 1 1 d . . . H9A H 0.4711 0.9613 0.2987 0.064 Uiso 1 1 calc R A . H9B H 0.5672 0.8905 0.2862 0.064 Uiso 1 1 calc R . . H9C H 0.4389 0.8700 0.3119 0.064 Uiso 1 1 calc R . . C10 C -0.1659(3) 0.9528(2) 0.24866(15) 0.0295(7) Uani 1 1 d . . . H10A H -0.1643 0.9814 0.2829 0.044 Uiso 1 1 calc R A . H10B H -0.2126 0.9015 0.2497 0.044 Uiso 1 1 calc R . . H10C H -0.2115 0.9857 0.2189 0.044 Uiso 1 1 calc R . . C11A C -0.2530(4) 0.8043(3) 0.10847(15) 0.0189(13) Uiso 0.569(14) 1 d PG A 1 C12A C -0.2850(4) 0.8854(3) 0.11015(15) 0.0188(13) Uiso 0.569(14) 1 d PG A 1 H12A H -0.2338 0.9200 0.1356 0.023 Uiso 0.569(14) 1 calc PR A 1 C13A C -0.3920(4) 0.9159(3) 0.07452(16) 0.0201(13) Uiso 0.569(14) 1 d PG A 1 H13A H -0.4139 0.9714 0.0757 0.024 Uiso 0.569(14) 1 calc PR A 1 C14A C -0.4668(4) 0.8653(3) 0.03721(15) 0.0212(14) Uiso 0.569(14) 1 d PG A 1 H14A H -0.5399 0.8862 0.0129 0.025 Uiso 0.569(14) 1 calc PR A 1 C15A C -0.4348(5) 0.7842(3) 0.03554(15) 0.0238(15) Uiso 0.569(14) 1 d PG A 1 H15A H -0.4860 0.7496 0.0100 0.029 Uiso 0.569(14) 1 calc PR A 1 C16A C -0.3278(5) 0.7537(3) 0.07117(17) 0.0255(15) Uiso 0.569(14) 1 d PG A 1 H16A H -0.3059 0.6982 0.0700 0.031 Uiso 0.569(14) 1 calc PR A 1 C11B C -0.2289(5) 0.7885(4) 0.10657(19) 0.0165(16) Uiso 0.431(14) 1 d PG A 2 C12B C -0.2787(5) 0.8660(4) 0.1082(2) 0.0210(19) Uiso 0.431(14) 1 d PG A 2 H12B H -0.2385 0.9029 0.1350 0.025 Uiso 0.431(14) 1 calc PR A 2 C13B C -0.3874(5) 0.8898(4) 0.0708(2) 0.0261(19) Uiso 0.431(14) 1 d PG A 2 H13B H -0.4214 0.9428 0.0719 0.031 Uiso 0.431(14) 1 calc PR A 2 C14B C -0.4463(5) 0.8359(5) 0.0316(2) 0.026(2) Uiso 0.431(14) 1 d PG A 2 H14B H -0.5206 0.8521 0.0060 0.031 Uiso 0.431(14) 1 calc PR A 2 C15B C -0.3965(7) 0.7583(4) 0.0300(2) 0.031(2) Uiso 0.431(14) 1 d PG A 2 H15B H -0.4368 0.7215 0.0032 0.037 Uiso 0.431(14) 1 calc PR A 2 C16B C -0.2878(7) 0.7346(3) 0.0674(2) 0.0248(19) Uiso 0.431(14) 1 d PG A 2 H16B H -0.2538 0.6816 0.0663 0.030 Uiso 0.431(14) 1 calc PR A 2 C17 C -0.1959(3) 0.73078(19) 0.21464(13) 0.0226(6) Uani 1 1 d . A . C18 C -0.3337(4) 0.7353(2) 0.21048(15) 0.0291(7) Uani 1 1 d . . . H18 H -0.3858 0.7560 0.1786 0.035 Uiso 1 1 calc R A . C19 C -0.3944(4) 0.7092(2) 0.25326(16) 0.0347(8) Uani 1 1 d . A . H19 H -0.4879 0.7113 0.2500 0.042 Uiso 1 1 calc R . . C20 C -0.3184(4) 0.6803(2) 0.30057(15) 0.0309(8) Uani 1 1 d . . . H20 H -0.3596 0.6636 0.3298 0.037 Uiso 1 1 calc R A . C21 C -0.1821(4) 0.6758(2) 0.30483(13) 0.0265(7) Uani 1 1 d . A . H21 H -0.1302 0.6563 0.3372 0.032 Uiso 1 1 calc R . . C22 C -0.1207(3) 0.6998(2) 0.26192(13) 0.0239(6) Uani 1 1 d . . . H22 H -0.0276 0.6950 0.2648 0.029 Uiso 1 1 calc R A . C23 C -0.0189(5) 0.6802(2) 0.14019(15) 0.0352(9) Uani 1 1 d . A . C24 C 0.1143(4) 0.6944(2) 0.14592(16) 0.0352(9) Uani 1 1 d . A . C25 C 0.2150(6) 0.6289(3) 0.1390(2) 0.0585(15) Uani 1 1 d . . . H25A H 0.2788 0.6228 0.1730 0.070 Uiso 1 1 calc R A . H25B H 0.1689 0.5768 0.1309 0.070 Uiso 1 1 calc R . . C26 C 0.3967(8) 0.5971(4) 0.0940(4) 0.100(3) Uani 1 1 d . . . H26A H 0.4595 0.6016 0.1279 0.150 Uiso 1 1 calc R A . H26B H 0.4400 0.6135 0.0638 0.150 Uiso 1 1 calc R . . H26C H 0.3668 0.5412 0.0888 0.150 Uiso 1 1 calc R . . C27 C -0.0859(6) 0.6053(2) 0.11656(18) 0.0506(13) Uani 1 1 d . . . C28A C -0.1044(7) 0.5894(4) 0.0586(3) 0.0268(13) Uiso 0.50 1 d P A 1 H28A H -0.0691 0.6268 0.0363 0.032 Uiso 0.50 1 calc PR A 1 C29A C -0.1715(8) 0.5218(5) 0.0343(3) 0.0337(16) Uiso 0.50 1 d P A 1 H29A H -0.1685 0.5093 -0.0024 0.040 Uiso 0.50 1 calc PR A 1 C30A C -0.2432(9) 0.4731(5) 0.0645(3) 0.0352(16) Uiso 0.50 1 d P A 1 H30A H -0.3008 0.4321 0.0480 0.042 Uiso 0.50 1 calc PR A 1 C28B C -0.0370(9) 0.5735(5) 0.0702(4) 0.0400(18) Uiso 0.50 1 d P A 2 H28B H 0.0305 0.6004 0.0555 0.048 Uiso 0.50 1 calc PR A 2 C29B C -0.0917(11) 0.5022(7) 0.0476(4) 0.055(2) Uiso 0.50 1 d P A 2 H29B H -0.0705 0.4835 0.0144 0.066 Uiso 0.50 1 calc PR A 2 C30B C -0.1785(10) 0.4576(6) 0.0741(4) 0.044(2) Uiso 0.50 1 d P A 2 H30B H -0.2066 0.4060 0.0605 0.053 Uiso 0.50 1 calc PR A 2 C31 C -0.2256(6) 0.4879(3) 0.1208(2) 0.0542(13) Uani 1 1 d . . . H31 H -0.276(6) 0.456(4) 0.140(2) 0.065 Uiso 1 1 d . . . C32 C -0.1636(5) 0.5571(2) 0.14449(16) 0.0378(9) Uani 1 1 d . A . H32 H -0.176(5) 0.572(3) 0.178(2) 0.045 Uiso 1 1 d . . . C33 C 0.0853(3) 0.95335(19) 0.07562(12) 0.0192(6) Uani 1 1 d . A . C34 C 0.0099(3) 1.0231(2) 0.07007(12) 0.0231(6) Uani 1 1 d . . . H34 H -0.0774 1.0228 0.0779 0.028 Uiso 1 1 calc R A . C35 C 0.0634(4) 1.0940(2) 0.05284(13) 0.0296(7) Uani 1 1 d . A . H35 H 0.0125 1.1421 0.0491 0.036 Uiso 1 1 calc R . . C36 C 0.1916(4) 1.0942(2) 0.04123(15) 0.0350(8) Uani 1 1 d . . . H36 H 0.2281 1.1425 0.0298 0.042 Uiso 1 1 calc R A . C37 C 0.2652(4) 1.0243(3) 0.04634(15) 0.0340(8) Uani 1 1 d . A . H37 H 0.3523 1.0246 0.0383 0.041 Uiso 1 1 calc R . . C38 C 0.2125(3) 0.9532(2) 0.06323(13) 0.0262(7) Uani 1 1 d . . . H38 H 0.2630 0.9051 0.0663 0.031 Uiso 1 1 calc R A . Sb Sb 0.30248(2) 0.672929(15) 0.376394(9) 0.02542(7) Uani 1 1 d . . . F1 F 0.1285(3) 0.7055(4) 0.35299(13) 0.1058(18) Uani 1 1 d . . . F2 F 0.4748(3) 0.6395(2) 0.40024(11) 0.0638(9) Uani 1 1 d . . . F3 F 0.3361(3) 0.6824(2) 0.30563(10) 0.0585(8) Uani 1 1 d . . . F4 F 0.2648(2) 0.66413(17) 0.44702(9) 0.0438(6) Uani 1 1 d . . . F5 F 0.2479(5) 0.5674(2) 0.36378(16) 0.0949(15) Uani 1 1 d . . . F6 F 0.3504(5) 0.7795(2) 0.3896(2) 0.1019(15) Uani 1 1 d . . . C50A C 0.3143(6) 0.3319(3) 0.0847(2) 0.1542(19) Uiso 0.50 1 d P B 3 H50A H 0.3624 0.3033 0.1166 0.185 Uiso 0.50 1 calc PR B 3 H50B H 0.2833 0.2900 0.0575 0.185 Uiso 0.50 1 calc PR B 3 Cl1A Cl 0.4247(3) 0.3828(2) 0.06033(13) 0.0682(7) Uiso 0.50 1 d P B 3 Cl2A Cl 0.1795(4) 0.3690(3) 0.10361(17) 0.0880(10) Uiso 0.50 1 d P B 3 C50B C 0.1440(13) 0.3147(8) 0.0790(5) 0.069(3) Uiso 0.50 1 d P C 4 H50C H 0.1089 0.3020 0.0408 0.083 Uiso 0.50 1 calc PR C 4 H50D H 0.1315 0.2663 0.1005 0.083 Uiso 0.50 1 calc PR C 4 Cl1B Cl 0.3143(6) 0.3319(3) 0.0847(2) 0.1542(19) Uiso 0.50 1 d P C 4 Cl2B Cl 0.0581(7) 0.3837(4) 0.0970(3) 0.150(2) Uiso 0.50 1 d P C 4 O3 O 0.1333(5) 0.7567(2) 0.02597(15) 0.0653(11) Uani 1 1 d D . . H1W H 0.199(5) 0.719(3) 0.043(2) 0.078 Uiso 1 1 d D . . H2W H 0.186(5) 0.780(4) 0.002(2) 0.078 Uiso 1 1 d 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 Ru 0.01658(12) 0.01763(12) 0.01558(12) 0.00142(8) 0.00477(8) 0.00033(8) P1 0.0301(4) 0.0211(4) 0.0159(3) 0.0006(3) 0.0065(3) -0.0074(3) O1 0.0337(13) 0.0227(11) 0.0333(13) 0.0028(10) 0.0171(11) 0.0064(10) O2 0.093(3) 0.0406(18) 0.078(3) 0.0166(17) 0.063(2) 0.0270(18) N1 0.0241(14) 0.0234(14) 0.0161(12) 0.0003(10) 0.0059(10) -0.0031(11) C1 0.0167(14) 0.0291(16) 0.0196(14) -0.0002(12) 0.0008(11) -0.0001(12) C2 0.0198(14) 0.0228(15) 0.0196(14) -0.0023(12) 0.0043(11) -0.0049(12) C3 0.0202(14) 0.0190(14) 0.0190(14) -0.0028(11) 0.0014(11) 0.0001(11) C4 0.0183(14) 0.0278(16) 0.0179(14) -0.0067(12) 0.0039(11) -0.0026(12) C5 0.0232(15) 0.0282(16) 0.0163(14) 0.0000(12) 0.0051(11) -0.0047(12) C6 0.0230(15) 0.0285(16) 0.0189(14) 0.0046(12) 0.0003(12) 0.0025(12) C7 0.0173(15) 0.047(2) 0.0275(17) 0.0030(15) 0.0035(13) 0.0051(14) C8 0.0199(17) 0.101(4) 0.038(2) 0.022(2) 0.0092(16) 0.006(2) C9 0.0204(17) 0.073(3) 0.0316(19) 0.005(2) -0.0006(14) -0.0024(18) C10 0.0212(15) 0.040(2) 0.0291(17) -0.0067(15) 0.0093(13) -0.0005(14) C17 0.0298(16) 0.0196(14) 0.0199(14) 0.0007(12) 0.0087(12) -0.0054(12) C18 0.0293(17) 0.0308(18) 0.0274(17) 0.0074(14) 0.0056(14) -0.0041(14) C19 0.0302(18) 0.037(2) 0.040(2) 0.0095(16) 0.0145(16) -0.0002(15) C20 0.042(2) 0.0261(17) 0.0291(17) 0.0059(14) 0.0203(15) -0.0001(15) C21 0.0415(19) 0.0201(15) 0.0195(15) 0.0029(12) 0.0101(14) 0.0005(13) C22 0.0298(16) 0.0211(15) 0.0225(15) 0.0014(12) 0.0088(13) -0.0009(13) C23 0.063(3) 0.0187(16) 0.0295(18) -0.0027(13) 0.0256(18) -0.0078(16) C24 0.058(2) 0.0199(16) 0.0344(19) 0.0044(14) 0.0281(18) 0.0047(16) C25 0.093(4) 0.028(2) 0.069(3) 0.011(2) 0.057(3) 0.020(2) C26 0.129(7) 0.064(4) 0.130(7) 0.016(4) 0.087(6) 0.039(4) C27 0.099(4) 0.0228(18) 0.038(2) -0.0081(16) 0.035(2) -0.022(2) C31 0.089(4) 0.030(2) 0.047(3) 0.0006(19) 0.023(3) -0.025(2) C32 0.061(3) 0.0252(18) 0.0289(19) 0.0020(15) 0.0137(18) -0.0104(17) C33 0.0202(14) 0.0232(15) 0.0141(13) 0.0011(11) 0.0026(11) -0.0031(11) C34 0.0247(15) 0.0281(16) 0.0164(14) 0.0007(12) 0.0034(11) 0.0032(13) C35 0.048(2) 0.0207(15) 0.0195(15) 0.0006(12) 0.0028(14) 0.0007(14) C36 0.046(2) 0.0330(19) 0.0243(17) 0.0067(14) 0.0002(15) -0.0178(17) C37 0.0231(16) 0.051(2) 0.0274(17) 0.0124(16) 0.0030(13) -0.0112(16) C38 0.0197(15) 0.0353(18) 0.0238(15) 0.0077(13) 0.0046(12) 0.0034(13) Sb 0.01969(11) 0.03426(13) 0.02114(11) 0.00678(9) 0.00013(8) -0.00555(8) F1 0.0246(13) 0.240(6) 0.0513(18) 0.056(3) 0.0016(12) 0.028(2) F2 0.0337(13) 0.121(3) 0.0370(14) 0.0164(16) 0.0061(11) 0.0325(16) F3 0.0451(15) 0.103(2) 0.0303(13) 0.0248(14) 0.0142(11) 0.0057(15) F4 0.0365(12) 0.0735(18) 0.0210(10) 0.0015(11) 0.0037(9) 0.0111(12) F5 0.154(4) 0.062(2) 0.083(2) -0.0352(19) 0.063(3) -0.067(2) F6 0.138(4) 0.0337(17) 0.150(4) -0.007(2) 0.071(3) -0.016(2) O3 0.107(3) 0.046(2) 0.055(2) 0.0127(16) 0.049(2) 0.020(2) _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 Ru O1 2.066(2) . ? Ru C6 2.183(3) . ? Ru N1 2.186(3) . ? Ru C5 2.211(3) . ? Ru C3 2.216(3) . ? Ru C4 2.260(3) . ? Ru C2 2.268(3) . ? Ru C1 2.293(3) . ? Ru P1 2.3282(9) . ? P1 C11B 1.741(4) . ? P1 C23 1.796(4) . ? P1 C17 1.836(3) . ? P1 C11A 1.941(3) . ? O1 C24 1.319(5) . ? O2 C25 1.419(5) . ? O2 C26 1.461(7) . ? N1 C33 1.450(4) . ? N1 H1N 0.85(4) . ? N1 H2N 0.83(5) . ? C1 C2 1.400(4) . ? C1 C6 1.444(5) . ? C1 C7 1.523(4) . ? C2 C3 1.442(4) . ? C2 H2 0.9500 . ? C3 C4 1.412(4) . ? C3 H3 0.9500 . ? C4 C5 1.431(5) . ? C4 C10 1.511(4) . ? C5 C6 1.407(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.523(6) . ? C7 C9 1.533(5) . ? C7 H7 1.02(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11A C12A 1.3900 . ? C11A C16A 1.3900 . ? C12A C13A 1.3900 . ? C12A H12A 0.9500 . ? C13A C14A 1.3900 . ? C13A H13A 0.9500 . ? C14A C15A 1.3900 . ? C14A H14A 0.9500 . ? C15A C16A 1.3900 . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C11B C12B 1.3900 . ? C11B C16B 1.3900 . ? C12B C13B 1.3900 . ? C12B H12B 0.9500 . ? C13B C14B 1.3900 . ? C13B H13B 0.9500 . ? C14B C15B 1.3900 . ? C14B H14B 0.9500 . ? C15B C16B 1.3900 . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? C17 C22 1.401(5) . ? C17 C18 1.404(5) . ? C18 C19 1.399(5) . ? C18 H18 0.9500 . ? C19 C20 1.393(5) . ? C19 H19 0.9500 . ? C20 C21 1.388(5) . ? C20 H20 0.9500 . ? C21 C22 1.396(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.371(6) . ? C23 C27 1.496(5) . ? C24 C25 1.532(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C32 1.400(5) . ? C27 C28B 1.445(10) . ? C27 C28A 1.459(8) . ? C28A C29A 1.402(10) . ? C28A H28A 0.9500 . ? C29A C30A 1.401(11) . ? C29A H29A 0.9500 . ? C30A C31 1.416(9) . ? C30A H30A 0.9500 . ? C28B C29B 1.389(14) . ? C28B H28B 0.9500 . ? C29B C30B 1.409(14) . ? C29B H29B 0.9500 . ? C30B C31 1.434(10) . ? C30B H30B 0.9500 . ? C31 C32 1.398(6) . ? C31 H31 0.93(6) . ? C32 H32 0.92(5) . ? C33 C34 1.389(4) . ? C33 C38 1.394(4) . ? C34 C35 1.399(5) . ? C34 H34 0.9500 . ? C35 C36 1.396(6) . ? C35 H35 0.9500 . ? C36 C37 1.380(6) . ? C36 H36 0.9500 . ? C37 C38 1.395(5) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? Sb F5 1.852(3) . ? Sb F6 1.853(3) . ? Sb F2 1.856(2) . ? Sb F1 1.865(3) . ? Sb F3 1.874(2) . ? Sb F4 1.884(2) . ? C50A Cl1A 1.615(6) . ? C50A Cl2A 1.657(7) . ? C50A H50A 0.9900 . ? C50A H50B 0.9900 . ? C50B Cl2B 1.560(14) . ? C50B H50C 0.9900 . ? C50B H50D 0.9900 . ? O3 H1W 0.966(10) . ? O3 H2W 0.961(10) . ? 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 O1 Ru C6 89.18(12) . . ? O1 Ru N1 82.39(11) . . ? C6 Ru N1 153.46(12) . . ? O1 Ru C5 116.59(11) . . ? C6 Ru C5 37.35(12) . . ? N1 Ru C5 160.99(12) . . ? O1 Ru C3 152.96(11) . . ? C6 Ru C3 79.33(12) . . ? N1 Ru C3 97.03(11) . . ? C5 Ru C3 66.74(12) . . ? O1 Ru C4 153.89(11) . . ? C6 Ru C4 67.38(12) . . ? N1 Ru C4 123.72(12) . . ? C5 Ru C4 37.30(12) . . ? C3 Ru C4 36.77(11) . . ? O1 Ru C2 115.48(11) . . ? C6 Ru C2 66.07(12) . . ? N1 Ru C2 94.98(11) . . ? C5 Ru C2 78.23(12) . . ? C3 Ru C2 37.49(11) . . ? C4 Ru C2 66.54(11) . . ? O1 Ru C1 89.42(11) . . ? C6 Ru C1 37.55(12) . . ? N1 Ru C1 116.87(11) . . ? C5 Ru C1 67.10(11) . . ? C3 Ru C1 66.59(11) . . ? C4 Ru C1 79.00(11) . . ? C2 Ru C1 35.74(11) . . ? O1 Ru P1 81.30(8) . . ? C6 Ru P1 118.61(9) . . ? N1 Ru P1 85.04(8) . . ? C5 Ru P1 96.37(9) . . ? C3 Ru P1 125.69(8) . . ? C4 Ru P1 99.44(8) . . ? C2 Ru P1 163.12(8) . . ? C1 Ru P1 154.98(9) . . ? C11B P1 C23 106.1(3) . . ? C11B P1 C17 105.3(2) . . ? C23 P1 C17 108.25(15) . . ? C23 P1 C11A 115.7(2) . . ? C17 P1 C11A 100.32(18) . . ? C11B P1 Ru 115.57(19) . . ? C23 P1 Ru 101.36(14) . . ? C17 P1 Ru 119.32(11) . . ? C11A P1 Ru 112.58(13) . . ? C24 O1 Ru 119.9(2) . . ? C25 O2 C26 112.7(4) . . ? C33 N1 Ru 117.8(2) . . ? C33 N1 H1N 111(3) . . ? Ru N1 H1N 106(3) . . ? C33 N1 H2N 107(3) . . ? Ru N1 H2N 109(3) . . ? H1N N1 H2N 105(4) . . ? C2 C1 C6 117.2(3) . . ? C2 C1 C7 124.1(3) . . ? C6 C1 C7 118.7(3) . . ? C2 C1 Ru 71.14(17) . . ? C6 C1 Ru 67.07(17) . . ? C7 C1 Ru 130.3(2) . . ? C1 C2 C3 121.3(3) . . ? C1 C2 Ru 73.13(18) . . ? C3 C2 Ru 69.31(17) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? Ru C2 H2 131.0 . . ? C4 C3 C2 121.0(3) . . ? C4 C3 Ru 73.32(18) . . ? C2 C3 Ru 73.20(18) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? Ru C3 H3 125.8 . . ? C3 C4 C5 117.8(3) . . ? C3 C4 C10 122.2(3) . . ? C5 C4 C10 119.9(3) . . ? C3 C4 Ru 69.91(17) . . ? C5 C4 Ru 69.48(17) . . ? C10 C4 Ru 133.3(2) . . ? C6 C5 C4 120.6(3) . . ? C6 C5 Ru 70.23(18) . . ? C4 C5 Ru 73.22(17) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? Ru C5 H5 129.3 . . ? C5 C6 C1 121.7(3) . . ? C5 C6 Ru 72.42(18) . . ? C1 C6 Ru 75.38(18) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? Ru C6 H6 124.7 . . ? C1 C7 C8 114.4(3) . . ? C1 C7 C9 109.4(3) . . ? C8 C7 C9 110.6(3) . . ? C1 C7 H7 106(3) . . ? C8 C7 H7 108(3) . . ? C9 C7 H7 107(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12A C11A C16A 120.0 . . ? C12A C11A P1 117.9(2) . . ? C16A C11A P1 122.1(2) . . ? C11A C12A C13A 120.0 . . ? C11A C12A H12A 120.0 . . ? C13A C12A H12A 120.0 . . ? C12A C13A C14A 120.0 . . ? C12A C13A H13A 120.0 . . ? C14A C13A H13A 120.0 . . ? C15A C14A C13A 120.0 . . ? C15A C14A H14A 120.0 . . ? C13A C14A H14A 120.0 . . ? C14A C15A C16A 120.0 . . ? C14A C15A H15A 120.0 . . ? C16A C15A H15A 120.0 . . ? C15A C16A C11A 120.0 . . ? C15A C16A H16A 120.0 . . ? C11A C16A H16A 120.0 . . ? C12B C11B C16B 120.0 . . ? C12B C11B P1 114.0(3) . . ? C16B C11B P1 125.5(3) . . ? C11B C12B C13B 120.0 . . ? C11B C12B H12B 120.0 . . ? C13B C12B H12B 120.0 . . ? C14B C13B C12B 120.0 . . ? C14B C13B H13B 120.0 . . ? C12B C13B H13B 120.0 . . ? C15B C14B C13B 120.0 . . ? C15B C14B H14B 120.0 . . ? C13B C14B H14B 120.0 . . ? C14B C15B C16B 120.0 . . ? C14B C15B H15B 120.0 . . ? C16B C15B H15B 120.0 . . ? C15B C16B C11B 120.0 . . ? C15B C16B H16B 120.0 . . ? C11B C16B H16B 120.0 . . ? C22 C17 C18 119.1(3) . . ? C22 C17 P1 117.4(2) . . ? C18 C17 P1 123.4(3) . . ? C19 C18 C17 120.1(3) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 120.2(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 120.2(3) . . ? C21 C22 H22 119.9 . . ? C17 C22 H22 119.9 . . ? C24 C23 C27 124.7(4) . . ? C24 C23 P1 112.2(3) . . ? C27 C23 P1 123.1(4) . . ? O1 C24 C23 125.1(3) . . ? O1 C24 C25 111.6(4) . . ? C23 C24 C25 123.1(4) . . ? O2 C25 C24 110.3(3) . . ? O2 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? O2 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? O2 C26 H26A 109.5 . . ? O2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28B 120.0(5) . . ? C32 C27 C28A 114.0(5) . . ? C32 C27 C23 122.7(4) . . ? C28B C27 C23 115.1(5) . . ? C28A C27 C23 121.3(4) . . ? C29A C28A C27 123.4(6) . . ? C29A C28A H28A 118.3 . . ? C27 C28A H28A 118.3 . . ? C30A C29A C28A 119.4(7) . . ? C30A C29A H29A 120.3 . . ? C28A C29A H29A 120.3 . . ? C29A C30A C31 116.8(7) . . ? C29A C30A H30A 121.6 . . ? C31 C30A H30A 121.6 . . ? C29B C28B C27 117.9(8) . . ? C29B C28B H28B 121.1 . . ? C27 C28B H28B 121.1 . . ? C28B C29B C30B 120.1(10) . . ? C28B C29B H29B 120.0 . . ? C30B C29B H29B 120.0 . . ? C29B C30B C31 121.9(8) . . ? C29B C30B H30B 119.0 . . ? C31 C30B H30B 119.0 . . ? C32 C31 C30A 122.7(5) . . ? C32 C31 C30B 116.4(6) . . ? C32 C31 H31 120(4) . . ? C30A C31 H31 116(4) . . ? C30B C31 H31 122(4) . . ? C31 C32 C27 120.9(4) . . ? C31 C32 H32 120(3) . . ? C27 C32 H32 119(3) . . ? C34 C33 C38 120.4(3) . . ? C34 C33 N1 120.1(3) . . ? C38 C33 N1 119.5(3) . . ? C33 C34 C35 119.5(3) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 120.0(3) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C37 C36 C35 120.0(3) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 120.4(3) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C33 C38 C37 119.6(3) . . ? C33 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? F5 Sb F6 177.7(2) . . ? F5 Sb F2 90.9(2) . . ? F6 Sb F2 91.0(2) . . ? F5 Sb F1 88.6(2) . . ? F6 Sb F1 89.5(2) . . ? F2 Sb F1 179.25(17) . . ? F5 Sb F3 90.92(15) . . ? F6 Sb F3 90.20(18) . . ? F2 Sb F3 90.69(12) . . ? F1 Sb F3 89.87(13) . . ? F5 Sb F4 89.03(14) . . ? F6 Sb F4 89.80(17) . . ? F2 Sb F4 90.58(11) . . ? F1 Sb F4 88.87(12) . . ? F3 Sb F4 178.74(11) . . ? Cl1A C50A Cl2A 126.0(4) . . ? Cl1A C50A H50A 105.8 . . ? Cl2A C50A H50A 105.8 . . ? Cl1A C50A H50B 105.8 . . ? Cl2A C50A H50B 105.8 . . ? H50A C50A H50B 106.2 . . ? Cl2B C50B H50C 107.9 . . ? Cl2B C50B H50D 107.9 . . ? H50C C50B H50D 107.2 . . ? H1W O3 H2W 96(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ru P1 C11B -116.6(3) . . . . ? C6 Ru P1 C11B 159.1(3) . . . . ? N1 Ru P1 C11B -33.6(3) . . . . ? C5 Ru P1 C11B 127.4(3) . . . . ? C3 Ru P1 C11B 61.5(3) . . . . ? C4 Ru P1 C11B 89.8(3) . . . . ? C2 Ru P1 C11B 57.2(4) . . . . ? C1 Ru P1 C11B 174.0(3) . . . . ? O1 Ru P1 C23 -2.46(15) . . . . ? C6 Ru P1 C23 -86.72(16) . . . . ? N1 Ru P1 C23 80.58(15) . . . . ? C5 Ru P1 C23 -118.48(16) . . . . ? C3 Ru P1 C23 175.67(16) . . . . ? C4 Ru P1 C23 -156.03(15) . . . . ? C2 Ru P1 C23 171.4(3) . . . . ? C1 Ru P1 C23 -71.8(2) . . . . ? O1 Ru P1 C17 116.18(15) . . . . ? C6 Ru P1 C17 31.92(17) . . . . ? N1 Ru P1 C17 -160.78(15) . . . . ? C5 Ru P1 C17 0.16(16) . . . . ? C3 Ru P1 C17 -65.69(16) . . . . ? C4 Ru P1 C17 -37.39(15) . . . . ? C2 Ru P1 C17 -70.0(3) . . . . ? C1 Ru P1 C17 46.8(2) . . . . ? O1 Ru P1 C11A -126.68(18) . . . . ? C6 Ru P1 C11A 149.1(2) . . . . ? N1 Ru P1 C11A -43.64(19) . . . . ? C5 Ru P1 C11A 117.30(19) . . . . ? C3 Ru P1 C11A 51.5(2) . . . . ? C4 Ru P1 C11A 79.76(19) . . . . ? C2 Ru P1 C11A 47.1(3) . . . . ? C1 Ru P1 C11A 163.9(3) . . . . ? C6 Ru O1 C24 120.1(3) . . . . ? N1 Ru O1 C24 -85.2(3) . . . . ? C5 Ru O1 C24 93.7(3) . . . . ? C3 Ru O1 C24 -175.7(3) . . . . ? C4 Ru O1 C24 94.6(3) . . . . ? C2 Ru O1 C24 -177.1(2) . . . . ? C1 Ru O1 C24 157.6(3) . . . . ? P1 Ru O1 C24 0.9(2) . . . . ? O1 Ru N1 C33 -115.4(2) . . . . ? C6 Ru N1 C33 -42.8(4) . . . . ? C5 Ru N1 C33 67.6(4) . . . . ? C3 Ru N1 C33 37.4(2) . . . . ? C4 Ru N1 C33 64.7(3) . . . . ? C2 Ru N1 C33 -0.3(2) . . . . ? C1 Ru N1 C33 -29.9(3) . . . . ? P1 Ru N1 C33 162.8(2) . . . . ? O1 Ru C1 C2 138.65(19) . . . . ? C6 Ru C1 C2 -131.9(3) . . . . ? N1 Ru C1 C2 57.5(2) . . . . ? C5 Ru C1 C2 -102.0(2) . . . . ? C3 Ru C1 C2 -28.51(18) . . . . ? C4 Ru C1 C2 -64.89(19) . . . . ? P1 Ru C1 C2 -153.65(17) . . . . ? O1 Ru C1 C6 -89.41(19) . . . . ? N1 Ru C1 C6 -170.58(19) . . . . ? C5 Ru C1 C6 29.95(19) . . . . ? C3 Ru C1 C6 103.4(2) . . . . ? C4 Ru C1 C6 67.0(2) . . . . ? C2 Ru C1 C6 131.9(3) . . . . ? P1 Ru C1 C6 -21.7(3) . . . . ? O1 Ru C1 C7 19.5(3) . . . . ? C6 Ru C1 C7 108.9(4) . . . . ? N1 Ru C1 C7 -61.7(3) . . . . ? C5 Ru C1 C7 138.9(3) . . . . ? C3 Ru C1 C7 -147.6(3) . . . . ? C4 Ru C1 C7 176.0(3) . . . . ? C2 Ru C1 C7 -119.1(4) . . . . ? P1 Ru C1 C7 87.2(4) . . . . ? C6 C1 C2 C3 1.6(5) . . . . ? C7 C1 C2 C3 178.4(3) . . . . ? Ru C1 C2 C3 52.0(3) . . . . ? C6 C1 C2 Ru -50.3(3) . . . . ? C7 C1 C2 Ru 126.4(3) . . . . ? O1 Ru C2 C1 -47.0(2) . . . . ? C6 Ru C2 C1 29.73(18) . . . . ? N1 Ru C2 C1 -130.97(19) . . . . ? C5 Ru C2 C1 66.99(19) . . . . ? C3 Ru C2 C1 134.0(3) . . . . ? C4 Ru C2 C1 104.3(2) . . . . ? P1 Ru C2 C1 139.7(2) . . . . ? O1 Ru C2 C3 178.99(17) . . . . ? C6 Ru C2 C3 -104.2(2) . . . . ? N1 Ru C2 C3 95.06(19) . . . . ? C5 Ru C2 C3 -66.98(19) . . . . ? C4 Ru C2 C3 -29.67(17) . . . . ? C1 Ru C2 C3 -134.0(3) . . . . ? P1 Ru C2 C3 5.8(4) . . . . ? C1 C2 C3 C4 4.3(5) . . . . ? Ru C2 C3 C4 57.9(3) . . . . ? C1 C2 C3 Ru -53.7(3) . . . . ? O1 Ru C3 C4 -132.7(2) . . . . ? C6 Ru C3 C4 -66.31(19) . . . . ? N1 Ru C3 C4 140.30(18) . . . . ? C5 Ru C3 C4 -29.40(18) . . . . ? C2 Ru C3 C4 -130.7(3) . . . . ? C1 Ru C3 C4 -103.4(2) . . . . ? P1 Ru C3 C4 51.4(2) . . . . ? O1 Ru C3 C2 -2.0(3) . . . . ? C6 Ru C3 C2 64.36(19) . . . . ? N1 Ru C3 C2 -89.02(18) . . . . ? C5 Ru C3 C2 101.3(2) . . . . ? C4 Ru C3 C2 130.7(3) . . . . ? C1 Ru C3 C2 27.26(17) . . . . ? P1 Ru C3 C2 -177.94(14) . . . . ? C2 C3 C4 C5 -5.9(4) . . . . ? Ru C3 C4 C5 52.0(3) . . . . ? C2 C3 C4 C10 172.8(3) . . . . ? Ru C3 C4 C10 -129.3(3) . . . . ? C2 C3 C4 Ru -57.9(3) . . . . ? O1 Ru C4 C3 130.6(2) . . . . ? C6 Ru C4 C3 102.9(2) . . . . ? N1 Ru C4 C3 -49.7(2) . . . . ? C5 Ru C4 C3 131.9(3) . . . . ? C2 Ru C4 C3 30.21(18) . . . . ? C1 Ru C4 C3 65.42(18) . . . . ? P1 Ru C4 C3 -139.96(16) . . . . ? O1 Ru C4 C5 -1.3(3) . . . . ? C6 Ru C4 C5 -29.04(18) . . . . ? N1 Ru C4 C5 178.44(17) . . . . ? C3 Ru C4 C5 -131.9(3) . . . . ? C2 Ru C4 C5 -101.7(2) . . . . ? C1 Ru C4 C5 -66.49(19) . . . . ? P1 Ru C4 C5 88.13(17) . . . . ? O1 Ru C4 C10 -113.6(4) . . . . ? C6 Ru C4 C10 -141.3(4) . . . . ? N1 Ru C4 C10 66.2(4) . . . . ? C5 Ru C4 C10 -112.2(4) . . . . ? C3 Ru C4 C10 115.8(4) . . . . ? C2 Ru C4 C10 146.1(4) . . . . ? C1 Ru C4 C10 -178.7(4) . . . . ? P1 Ru C4 C10 -24.1(3) . . . . ? C3 C4 C5 C6 1.7(5) . . . . ? C10 C4 C5 C6 -177.0(3) . . . . ? Ru C4 C5 C6 53.9(3) . . . . ? C3 C4 C5 Ru -52.2(2) . . . . ? C10 C4 C5 Ru 129.1(3) . . . . ? O1 Ru C5 C6 47.0(2) . . . . ? N1 Ru C5 C6 -136.4(3) . . . . ? C3 Ru C5 C6 -103.4(2) . . . . ? C4 Ru C5 C6 -132.4(3) . . . . ? C2 Ru C5 C6 -65.8(2) . . . . ? C1 Ru C5 C6 -30.10(19) . . . . ? P1 Ru C5 C6 130.40(19) . . . . ? O1 Ru C5 C4 179.35(17) . . . . ? C6 Ru C5 C4 132.4(3) . . . . ? N1 Ru C5 C4 -4.0(4) . . . . ? C3 Ru C5 C4 29.01(17) . . . . ? C2 Ru C5 C4 66.57(18) . . . . ? C1 Ru C5 C4 102.3(2) . . . . ? P1 Ru C5 C4 -97.22(17) . . . . ? C4 C5 C6 C1 4.3(5) . . . . ? Ru C5 C6 C1 59.6(3) . . . . ? C4 C5 C6 Ru -55.3(3) . . . . ? C2 C1 C6 C5 -5.8(5) . . . . ? C7 C1 C6 C5 177.2(3) . . . . ? Ru C1 C6 C5 -58.1(3) . . . . ? C2 C1 C6 Ru 52.3(3) . . . . ? C7 C1 C6 Ru -124.6(3) . . . . ? O1 Ru C6 C5 -139.2(2) . . . . ? N1 Ru C6 C5 149.8(2) . . . . ? C3 Ru C6 C5 65.4(2) . . . . ? C4 Ru C6 C5 29.01(19) . . . . ? C2 Ru C6 C5 102.3(2) . . . . ? C1 Ru C6 C5 130.7(3) . . . . ? P1 Ru C6 C5 -59.6(2) . . . . ? O1 Ru C6 C1 90.12(19) . . . . ? N1 Ru C6 C1 19.1(4) . . . . ? C5 Ru C6 C1 -130.7(3) . . . . ? C3 Ru C6 C1 -65.27(19) . . . . ? C4 Ru C6 C1 -101.7(2) . . . . ? C2 Ru C6 C1 -28.38(18) . . . . ? P1 Ru C6 C1 169.73(15) . . . . ? C2 C1 C7 C8 -6.0(5) . . . . ? C6 C1 C7 C8 170.7(4) . . . . ? Ru C1 C7 C8 87.6(4) . . . . ? C2 C1 C7 C9 118.7(4) . . . . ? C6 C1 C7 C9 -64.6(4) . . . . ? Ru C1 C7 C9 -147.8(3) . . . . ? C11B P1 C11A C12A -145.2(17) . . . . ? C23 P1 C11A C12A -151.1(2) . . . . ? C17 P1 C11A C12A 92.7(2) . . . . ? Ru P1 C11A C12A -35.2(3) . . . . ? C11B P1 C11A C16A 37.2(15) . . . . ? C23 P1 C11A C16A 31.3(3) . . . . ? C17 P1 C11A C16A -84.8(2) . . . . ? Ru P1 C11A C16A 147.2(2) . . . . ? C16A C11A C12A C13A 0.0 . . . . ? P1 C11A C12A C13A -177.6(3) . . . . ? C11A C12A C13A C14A 0.0 . . . . ? C12A C13A C14A C15A 0.0 . . . . ? C13A C14A C15A C16A 0.0 . . . . ? C14A C15A C16A C11A 0.0 . . . . ? C12A C11A C16A C15A 0.0 . . . . ? P1 C11A C16A C15A 177.5(3) . . . . ? C23 P1 C11B C12B -160.4(3) . . . . ? C17 P1 C11B C12B 85.0(3) . . . . ? C11A P1 C11B C12B 25.2(15) . . . . ? Ru P1 C11B C12B -48.9(4) . . . . ? C23 P1 C11B C16B 27.9(4) . . . . ? C17 P1 C11B C16B -86.7(4) . . . . ? C11A P1 C11B C16B -146.5(18) . . . . ? Ru P1 C11B C16B 139.3(3) . . . . ? C16B C11B C12B C13B 0.0 . . . . ? P1 C11B C12B C13B -172.2(4) . . . . ? C11B C12B C13B C14B 0.0 . . . . ? C12B C13B C14B C15B 0.0 . . . . ? C13B C14B C15B C16B 0.0 . . . . ? C14B C15B C16B C11B 0.0 . . . . ? C12B C11B C16B C15B 0.0 . . . . ? P1 C11B C16B C15B 171.3(5) . . . . ? C11B P1 C17 C22 173.6(3) . . . . ? C23 P1 C17 C22 60.5(3) . . . . ? C11A P1 C17 C22 -177.9(3) . . . . ? Ru P1 C17 C22 -54.6(3) . . . . ? C11B P1 C17 C18 -7.0(4) . . . . ? C23 P1 C17 C18 -120.1(3) . . . . ? C11A P1 C17 C18 1.5(3) . . . . ? Ru P1 C17 C18 124.8(3) . . . . ? C22 C17 C18 C19 0.3(5) . . . . ? P1 C17 C18 C19 -179.1(3) . . . . ? C17 C18 C19 C20 1.3(6) . . . . ? C18 C19 C20 C21 -1.3(6) . . . . ? C19 C20 C21 C22 -0.3(5) . . . . ? C20 C21 C22 C17 1.8(5) . . . . ? C18 C17 C22 C21 -1.8(5) . . . . ? P1 C17 C22 C21 177.6(3) . . . . ? C11B P1 C23 C24 125.1(3) . . . . ? C17 P1 C23 C24 -122.3(3) . . . . ? C11A P1 C23 C24 126.1(3) . . . . ? Ru P1 C23 C24 4.1(3) . . . . ? C11B P1 C23 C27 -51.9(4) . . . . ? C17 P1 C23 C27 60.7(4) . . . . ? C11A P1 C23 C27 -50.9(4) . . . . ? Ru P1 C23 C27 -173.0(3) . . . . ? Ru O1 C24 C23 1.9(5) . . . . ? Ru O1 C24 C25 -173.7(3) . . . . ? C27 C23 C24 O1 172.7(4) . . . . ? P1 C23 C24 O1 -4.3(5) . . . . ? C27 C23 C24 C25 -12.2(6) . . . . ? P1 C23 C24 C25 170.8(3) . . . . ? C26 O2 C25 C24 169.4(6) . . . . ? O1 C24 C25 O2 -65.0(6) . . . . ? C23 C24 C25 O2 119.3(5) . . . . ? C24 C23 C27 C32 123.4(5) . . . . ? P1 C23 C27 C32 -59.9(6) . . . . ? C24 C23 C27 C28B -39.9(7) . . . . ? P1 C23 C27 C28B 136.7(5) . . . . ? C24 C23 C27 C28A -73.4(7) . . . . ? P1 C23 C27 C28A 103.3(6) . . . . ? C32 C27 C28A C29A -12.7(10) . . . . ? C28B C27 C28A C29A 96.3(12) . . . . ? C23 C27 C28A C29A -177.2(6) . . . . ? C27 C28A C29A C30A 10.5(12) . . . . ? C28A C29A C30A C31 -10.0(12) . . . . ? C32 C27 C28B C29B 13.7(12) . . . . ? C28A C27 C28B C29B -72.8(11) . . . . ? C23 C27 C28B C29B 177.5(8) . . . . ? C27 C28B C29B C30B -8.5(14) . . . . ? C28B C29B C30B C31 7.5(16) . . . . ? C29A C30A C31 C32 13.3(11) . . . . ? C29A C30A C31 C30B -72.9(12) . . . . ? C29B C30B C31 C32 -10.9(12) . . . . ? C29B C30B C31 C30A 99.4(15) . . . . ? C30A C31 C32 C27 -16.7(9) . . . . ? C30B C31 C32 C27 16.1(9) . . . . ? C28B C27 C32 C31 -18.0(9) . . . . ? C28A C27 C32 C31 15.2(8) . . . . ? C23 C27 C32 C31 179.4(5) . . . . ? Ru N1 C33 C34 -88.7(3) . . . . ? Ru N1 C33 C38 91.2(3) . . . . ? C38 C33 C34 C35 -1.2(5) . . . . ? N1 C33 C34 C35 178.7(3) . . . . ? C33 C34 C35 C36 0.2(5) . . . . ? C34 C35 C36 C37 0.5(5) . . . . ? C35 C36 C37 C38 -0.2(6) . . . . ? C34 C33 C38 C37 1.5(5) . . . . ? N1 C33 C38 C37 -178.4(3) . . . . ? C36 C37 C38 C33 -0.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.860 _refine_diff_density_min -1.485 _refine_diff_density_rms 0.113 #===END # # # ---------------------------------------------------------- # Data for compound 4 (local labelling as fjl221as) data_cmpnd_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 O2 P Ru, 2(F6 Sb), C6 H8 N' _chemical_formula_sum 'C38 H44 F12 N O2 P Ru Sb2' _chemical_formula_weight 1150.28 _chemical_absolute_configuration rmad 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_space_group_name_Hall 'C 2y' 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' _cell_length_a 29.518(3) _cell_length_b 10.8722(11) _cell_length_c 12.9904(14) _cell_angle_alpha 90.00 _cell_angle_beta 94.993(2) _cell_angle_gamma 90.00 _cell_volume 4153.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19174 _cell_measurement_theta_min 2.505 _cell_measurement_theta_max 23.300 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.059 _exptl_crystal_size_min 0.035 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 1.778 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.682 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX CCD system' _diffrn_measurement_method 'narrow \w frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19172 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0896 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.56 _reflns_number_total 9403 _reflns_number_gt 7270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, PLATON(Spek, 1998)' _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. Hydrogen atoms have been included in the model in calculated positions and refined with a riding model, except hydrogen atom bounded to N1 atom. This later has been observed at difference Fourier maps, and refined with a restraint in NH distance. Asymmetric unit contains a ruthenium complex, two SbF6 counterions and a C6 H8 N molecule. One of the SbF6 molecules has found to be disordered. It has been included in the model with fluorine atoms in two set of positions, with complementary ocupancy factors (0.74 / 0.26). They have been refined isotropically. At the end of the refinement, two residual density peaks of 1.60 e/A^3 are observed at 0.87 A from the Sb atoms. They have no chemical sence. Six other residual density peaks of 0.9 e/A^3 are located in the proximity of disordered fluorine atoms. ; _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^)+(0.0394P)^2^+25.5146P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 9403 _refine_ls_number_parameters 518 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl221as in C2 CELL 0.71073 29.5180 10.8722 12.9904 90.000 94.993 90.000 ZERR 4.00 0.0030 0.0011 0.0014 0.000 0.002 0.000 LATT -7 SYMM - X, Y, - Z SFAC C H N O F P RU SB UNIT 152 176 4 8 48 4 4 8 MERG 2 OMIT 11 -9 10 OMIT -27 9 2 DFIX 0.87 0.02 N1 H1 FMAP 2 PLAN 20 ACTA 55.00 BOND $H CONF WPDB -2 L.S. 4 TEMP -173.00 WGHT 0.039400 25.514601 FVAR 0.13373 0.73969 RU 7 0.898994 0.473834 0.671327 11.00000 0.01604 0.01609 = 0.01890 -0.00079 -0.00082 0.00003 P1 6 0.869012 0.449536 0.830412 11.00000 0.01927 0.01655 = 0.01772 -0.00116 -0.00232 -0.00034 O1 4 0.839697 0.378319 0.630916 11.00000 0.01791 0.01784 = 0.02812 -0.00425 0.00398 -0.00496 O2 4 0.848753 0.619999 0.665175 11.00000 0.02720 0.01429 = 0.02316 0.00424 0.00079 -0.00140 N1 3 0.836673 0.182070 0.515430 11.00000 0.02664 0.02180 = 0.02969 -0.00816 0.00934 -0.00013 C1 1 0.931244 0.439174 0.522415 11.00000 0.00661 0.03687 = 0.02463 -0.00515 0.00568 -0.00353 C2 1 0.944309 0.554173 0.559557 11.00000 0.01970 0.01781 = 0.02733 -0.00131 0.00282 -0.00204 AFIX 43 H2 2 0.940514 0.622545 0.514086 11.00000 -1.20000 AFIX 0 C3 1 0.963167 0.574951 0.662660 11.00000 0.02108 0.02848 = 0.03247 -0.00352 0.00919 -0.00458 AFIX 43 H3 2 0.970002 0.656466 0.685326 11.00000 -1.20000 AFIX 0 C4 1 0.971673 0.477382 0.730407 11.00000 0.01232 0.03221 = 0.03232 -0.00005 0.00178 0.00937 C5 1 0.957649 0.358065 0.696177 11.00000 0.01783 0.02284 = 0.03163 0.00049 -0.00256 0.01294 AFIX 43 H5 2 0.961860 0.289717 0.741563 11.00000 -1.20000 AFIX 0 C6 1 0.937686 0.341510 0.595796 11.00000 0.01619 0.02270 = 0.02678 -0.00290 0.00317 0.00927 AFIX 43 H6 2 0.927887 0.261283 0.575212 11.00000 -1.20000 AFIX 0 C7 1 0.906931 0.415349 0.416339 11.00000 0.01594 0.03106 = 0.02523 -0.00442 0.00142 -0.00037 AFIX 13 H7 2 0.874589 0.395245 0.426759 11.00000 -1.20000 AFIX 0 C8 1 0.926831 0.304069 0.363521 11.00000 0.04133 0.03270 = 0.02923 -0.01004 0.00840 -0.00572 AFIX 137 H8A 2 0.959222 0.318075 0.356605 11.00000 -1.50000 H8B 2 0.910817 0.292723 0.294880 11.00000 -1.50000 H8C 2 0.923176 0.230266 0.405312 11.00000 -1.50000 AFIX 0 C9 1 0.906433 0.530329 0.347814 11.00000 0.03840 0.04096 = 0.02535 0.00710 0.00496 0.00015 AFIX 137 H9A 2 0.892997 0.599129 0.383244 11.00000 -1.50000 H9B 2 0.888351 0.514044 0.282350 11.00000 -1.50000 H9C 2 0.937631 0.551269 0.334071 11.00000 -1.50000 AFIX 0 C10 1 0.995679 0.494651 0.837585 11.00000 0.01567 0.05024 = 0.03606 0.00471 -0.00312 0.00037 AFIX 137 H10A 2 1.028651 0.490556 0.833681 11.00000 -1.50000 H10B 2 0.986286 0.429554 0.883381 11.00000 -1.50000 H10C 2 0.987598 0.574991 0.864891 11.00000 -1.50000 AFIX 0 C11 1 0.887903 0.312364 0.901305 11.00000 0.01652 0.02320 = 0.01945 -0.00290 0.00370 -0.00134 C12 1 0.914360 0.317424 0.993320 11.00000 0.02959 0.02199 = 0.03242 -0.00397 -0.00835 0.00033 AFIX 43 H12 2 0.921209 0.394975 1.024592 11.00000 -1.20000 AFIX 0 C13 1 0.931308 0.210884 1.041535 11.00000 0.05081 0.02396 = 0.03678 0.00157 -0.02070 0.00397 AFIX 43 H13 2 0.949644 0.214849 1.105281 11.00000 -1.20000 AFIX 0 C14 1 0.920907 0.098806 0.994710 11.00000 0.05612 0.01777 = 0.03624 0.00538 -0.01714 0.00764 AFIX 43 H14 2 0.932089 0.025025 1.026828 11.00000 -1.20000 AFIX 0 C15 1 0.894997 0.093291 0.903731 11.00000 0.03227 0.01697 = 0.03851 -0.00109 -0.00983 -0.00003 AFIX 43 H15 2 0.888415 0.015375 0.872873 11.00000 -1.20000 AFIX 0 C16 1 0.878001 0.197322 0.854948 11.00000 0.02854 0.02653 = 0.01579 0.00271 -0.00099 0.00298 AFIX 43 H16 2 0.859865 0.191921 0.791010 11.00000 -1.20000 AFIX 0 C17 1 0.877092 0.573584 0.922151 11.00000 0.01941 0.02193 = 0.01499 0.00157 -0.00482 0.00380 C18 1 0.858065 0.572242 1.016353 11.00000 0.02906 0.01846 = 0.01955 -0.00426 -0.00346 -0.00090 AFIX 43 H18 2 0.838314 0.506993 1.031602 11.00000 -1.20000 AFIX 0 C19 1 0.867495 0.664387 1.087910 11.00000 0.04177 0.03155 = 0.01471 -0.00367 0.00018 0.01233 AFIX 43 H19 2 0.853441 0.664197 1.150980 11.00000 -1.20000 AFIX 0 C20 1 0.897369 0.756687 1.067560 11.00000 0.03764 0.02146 = 0.02654 -0.01202 -0.00862 -0.00241 AFIX 43 H20 2 0.904433 0.818587 1.118033 11.00000 -1.20000 AFIX 0 C21 1 0.917170 0.761131 0.975806 11.00000 0.02828 0.02255 = 0.02988 -0.00287 0.00301 -0.00366 AFIX 43 H21 2 0.937870 0.824983 0.962676 11.00000 -1.20000 AFIX 0 C22 1 0.906133 0.668952 0.901513 11.00000 0.02629 0.01699 = 0.02068 -0.00387 0.00186 0.00069 AFIX 43 H22 2 0.918714 0.672215 0.836699 11.00000 -1.20000 AFIX 0 C23 1 0.807339 0.427945 0.788544 11.00000 0.01322 0.01571 = 0.02161 -0.00480 0.00293 -0.00159 AFIX 13 H23 2 0.801257 0.339113 0.801790 11.00000 -1.20000 AFIX 0 C24 1 0.803194 0.440374 0.668601 11.00000 0.01723 0.02439 = 0.01865 -0.00840 0.00337 -0.00274 AFIX 13 H24 2 0.774287 0.400126 0.640316 11.00000 -1.20000 AFIX 0 C25 1 0.803761 0.569838 0.629093 11.00000 0.02169 0.02716 = 0.01299 0.00330 -0.00205 0.00803 AFIX 23 H25A 2 0.799332 0.570996 0.552676 11.00000 -1.20000 H25B 2 0.779296 0.618854 0.656783 11.00000 -1.20000 AFIX 0 C26 1 0.856167 0.736349 0.620806 11.00000 0.03219 0.01962 = 0.04183 0.00780 -0.00475 -0.00015 AFIX 137 H26A 2 0.855442 0.728059 0.545560 11.00000 -1.50000 H26B 2 0.885900 0.768097 0.648021 11.00000 -1.50000 H26C 2 0.832294 0.793473 0.638108 11.00000 -1.50000 AFIX 0 C27 1 0.774147 0.496207 0.847516 11.00000 0.02379 0.02236 = 0.01566 -0.00269 0.00480 0.00377 C28 1 0.773602 0.625443 0.853015 11.00000 0.01890 0.03177 = 0.02638 0.00089 -0.00408 0.00554 AFIX 43 H28 2 0.796150 0.671556 0.822072 11.00000 -1.20000 AFIX 0 C29 1 0.740912 0.685637 0.902505 11.00000 0.02483 0.03417 = 0.02604 0.00026 0.00130 0.01424 AFIX 43 H29 2 0.740765 0.772978 0.904606 11.00000 -1.20000 AFIX 0 C30 1 0.708348 0.620685 0.949111 11.00000 0.03467 0.05118 = 0.02215 -0.01383 -0.00572 0.02206 AFIX 43 H30 2 0.685832 0.662761 0.983518 11.00000 -1.20000 AFIX 0 C31 1 0.708659 0.494013 0.945474 11.00000 0.02191 0.05393 = 0.03133 0.00609 0.01457 -0.00476 AFIX 43 H31 2 0.686469 0.448281 0.977963 11.00000 -1.20000 AFIX 0 C32 1 0.741346 0.433564 0.894422 11.00000 0.02573 0.02514 = 0.02097 0.00156 -0.00461 -0.00117 AFIX 43 H32 2 0.741028 0.346241 0.891838 11.00000 -1.20000 AFIX 0 C33 1 0.815736 0.185687 0.420359 11.00000 0.01680 0.03230 = 0.03211 -0.00080 -0.00090 0.00040 AFIX 43 H33 2 0.796392 0.253062 0.400689 11.00000 -1.20000 AFIX 0 C34 1 0.821620 0.094049 0.350608 11.00000 0.02408 0.02975 = 0.02854 0.00054 -0.00147 -0.00036 AFIX 43 H34 2 0.806904 0.099015 0.282728 11.00000 -1.20000 AFIX 0 C35 1 0.848473 -0.004038 0.378263 11.00000 0.01783 0.03053 = 0.02413 -0.00330 -0.00462 -0.00203 C36 1 0.870447 -0.006412 0.478093 11.00000 0.01539 0.01512 = 0.04560 0.00681 0.00865 0.00046 AFIX 43 H36 2 0.890167 -0.072473 0.499274 11.00000 -1.20000 AFIX 0 C37 1 0.863272 0.086894 0.544510 11.00000 0.03304 0.02425 = 0.02599 -0.00336 -0.00300 -0.00816 AFIX 43 H37 2 0.877489 0.084206 0.612952 11.00000 -1.20000 AFIX 0 C38 1 0.853695 -0.108758 0.305703 11.00000 0.04074 0.04478 = 0.04005 -0.01823 0.00706 -0.00336 AFIX 137 H38A 2 0.827823 -0.164911 0.307835 11.00000 -1.50000 H38B 2 0.881957 -0.153006 0.326361 11.00000 -1.50000 H38C 2 0.854731 -0.077021 0.235337 11.00000 -1.50000 AFIX 0 SB1 8 0.996526 0.943127 0.692313 11.00000 0.03568 0.02886 = 0.04207 0.00776 -0.00232 -0.00232 SB2 8 0.755835 0.528917 0.292177 11.00000 0.02524 0.02474 = 0.02814 0.00164 -0.00544 0.00341 PART 1 F1A 5 1.035977 0.804528 0.701595 21.00000 0.07103 F2A 5 0.955329 1.067591 0.679591 21.00000 0.05325 F3A 5 0.962071 0.855767 0.584814 21.00000 0.02882 F4A 5 1.028020 1.015275 0.798765 21.00000 0.07584 F5A 5 1.030756 1.018393 0.599181 21.00000 0.06387 F6A 5 0.961488 0.858586 0.779988 21.00000 0.06403 PART 2 F1B 5 1.035950 0.831590 0.639025 -21.00000 0.07004 F2B 5 0.987095 1.070330 0.802697 -21.00000 0.10300 F3B 5 0.936841 0.909047 0.710277 -21.00000 0.11350 F4B 5 1.053557 1.009685 0.748702 -21.00000 0.07518 F5B 5 0.981549 1.074701 0.599362 -21.00000 0.10488 F6B 5 0.995796 0.843564 0.802792 -21.00000 0.06943 PART 0 F7 5 0.800012 0.411551 0.269074 11.00000 0.05333 0.05006 = 0.08542 -0.01097 0.00769 0.02339 F8 5 0.713272 0.647532 0.312715 11.00000 0.06738 0.06223 = 0.05256 0.01659 0.02743 0.03374 F9 5 0.711772 0.433820 0.218118 11.00000 0.05869 0.06452 = 0.06230 -0.01491 -0.01144 -0.02570 F10 5 0.800271 0.619415 0.367811 11.00000 0.04498 0.08145 = 0.03830 -0.00112 -0.00794 -0.02073 F11 5 0.769271 0.608232 0.173432 11.00000 0.05512 0.06004 = 0.03631 0.01267 0.00881 -0.00307 F12 5 0.743243 0.448590 0.413749 11.00000 0.05244 0.05044 = 0.04383 0.01806 -0.00807 -0.00754 H1 2 0.829621 0.227751 0.567362 11.00000 0.02573 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM fjl221as in C2 REM R1 = 0.0556 for 7270 Fo > 4sig(Fo) and 0.0803 for all 9403 data REM 518 parameters refined using 2 restraints END ; 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 Ru Ru 0.898994(19) 0.47383(5) 0.67133(5) 0.01715(14) Uani 1 1 d . . . P1 P 0.86901(6) 0.4495(2) 0.83041(14) 0.0181(4) Uani 1 1 d . . . O1 O 0.83970(18) 0.3783(5) 0.6309(4) 0.0212(13) Uani 1 1 d . . . O2 O 0.84875(19) 0.6200(5) 0.6652(4) 0.0216(12) Uani 1 1 d . . . N1 N 0.8367(2) 0.1821(6) 0.5154(6) 0.0256(16) Uani 1 1 d D . . C1 C 0.9312(2) 0.4392(8) 0.5224(6) 0.0225(17) Uani 1 1 d . . . C2 C 0.9443(3) 0.5542(7) 0.5596(6) 0.0216(18) Uani 1 1 d . . . H2 H 0.9405 0.6225 0.5141 0.026 Uiso 1 1 calc R . . C3 C 0.9632(3) 0.5750(8) 0.6627(7) 0.027(2) Uani 1 1 d . . . H3 H 0.9700 0.6565 0.6853 0.032 Uiso 1 1 calc R . . C4 C 0.9717(2) 0.4774(8) 0.7304(6) 0.0256(18) Uani 1 1 d . . . C5 C 0.9576(3) 0.3581(8) 0.6962(7) 0.0244(19) Uani 1 1 d . . . H5 H 0.9619 0.2897 0.7416 0.029 Uiso 1 1 calc R . . C6 C 0.9377(3) 0.3415(8) 0.5958(6) 0.0218(18) Uani 1 1 d . . . H6 H 0.9279 0.2613 0.5752 0.026 Uiso 1 1 calc R . . C7 C 0.9069(3) 0.4153(8) 0.4163(6) 0.0241(19) Uani 1 1 d . . . H7 H 0.8746 0.3952 0.4268 0.029 Uiso 1 1 calc R . . C8 C 0.9268(3) 0.3041(9) 0.3635(7) 0.034(2) Uani 1 1 d . . . H8A H 0.9592 0.3181 0.3566 0.051 Uiso 1 1 calc R . . H8B H 0.9108 0.2927 0.2949 0.051 Uiso 1 1 calc R . . H8C H 0.9232 0.2303 0.4053 0.051 Uiso 1 1 calc R . . C9 C 0.9064(3) 0.5303(10) 0.3478(6) 0.035(2) Uani 1 1 d . . . H9A H 0.8930 0.5991 0.3832 0.052 Uiso 1 1 calc R . . H9B H 0.8884 0.5140 0.2823 0.052 Uiso 1 1 calc R . . H9C H 0.9376 0.5513 0.3341 0.052 Uiso 1 1 calc R . . C10 C 0.9957(3) 0.4947(9) 0.8376(6) 0.034(2) Uani 1 1 d . . . H10A H 1.0287 0.4906 0.8337 0.051 Uiso 1 1 calc R . . H10B H 0.9863 0.4296 0.8834 0.051 Uiso 1 1 calc R . . H10C H 0.9876 0.5750 0.8649 0.051 Uiso 1 1 calc R . . C11 C 0.8879(3) 0.3124(8) 0.9013(6) 0.0196(17) Uani 1 1 d . . . C12 C 0.9144(3) 0.3174(9) 0.9933(7) 0.029(2) Uani 1 1 d . . . H12 H 0.9212 0.3950 1.0246 0.034 Uiso 1 1 calc R . . C13 C 0.9313(3) 0.2109(9) 1.0415(8) 0.039(3) Uani 1 1 d . . . H13 H 0.9496 0.2148 1.1053 0.046 Uiso 1 1 calc R . . C14 C 0.9209(3) 0.0988(8) 0.9947(7) 0.038(2) Uani 1 1 d . . . H14 H 0.9321 0.0250 1.0268 0.046 Uiso 1 1 calc R . . C15 C 0.8950(3) 0.0933(8) 0.9037(7) 0.030(2) Uani 1 1 d . . . H15 H 0.8884 0.0154 0.8729 0.036 Uiso 1 1 calc R . . C16 C 0.8780(3) 0.1973(8) 0.8549(6) 0.0238(18) Uani 1 1 d . . . H16 H 0.8599 0.1919 0.7910 0.029 Uiso 1 1 calc R . . C17 C 0.8771(3) 0.5736(7) 0.9222(6) 0.0191(17) Uani 1 1 d . . . C18 C 0.8581(3) 0.5722(7) 1.0164(6) 0.0227(18) Uani 1 1 d . . . H18 H 0.8383 0.5070 1.0316 0.027 Uiso 1 1 calc R . . C19 C 0.8675(3) 0.6644(8) 1.0879(6) 0.029(2) Uani 1 1 d . . . H19 H 0.8534 0.6642 1.1510 0.035 Uiso 1 1 calc R . . C20 C 0.8974(3) 0.7567(8) 1.0676(7) 0.029(2) Uani 1 1 d . . . H20 H 0.9044 0.8186 1.1180 0.035 Uiso 1 1 calc R . . C21 C 0.9172(3) 0.7611(8) 0.9758(7) 0.027(2) Uani 1 1 d . . . H21 H 0.9379 0.8250 0.9627 0.032 Uiso 1 1 calc R . . C22 C 0.9061(3) 0.6690(7) 0.9015(6) 0.0213(17) Uani 1 1 d . . . H22 H 0.9187 0.6722 0.8367 0.026 Uiso 1 1 calc R . . C23 C 0.8073(2) 0.4279(7) 0.7885(5) 0.0168(16) Uani 1 1 d . . . H23 H 0.8013 0.3391 0.8018 0.020 Uiso 1 1 calc R . . C24 C 0.8032(2) 0.4404(8) 0.6686(5) 0.0200(16) Uani 1 1 d . . . H24 H 0.7743 0.4001 0.6403 0.024 Uiso 1 1 calc R . . C25 C 0.8038(3) 0.5698(7) 0.6291(6) 0.0208(17) Uani 1 1 d . . . H25A H 0.7993 0.5710 0.5527 0.025 Uiso 1 1 calc R . . H25B H 0.7793 0.6189 0.6568 0.025 Uiso 1 1 calc R . . C26 C 0.8562(3) 0.7363(8) 0.6208(7) 0.032(2) Uani 1 1 d . . . H26A H 0.8554 0.7281 0.5456 0.048 Uiso 1 1 calc R . . H26B H 0.8859 0.7681 0.6480 0.048 Uiso 1 1 calc R . . H26C H 0.8323 0.7935 0.6381 0.048 Uiso 1 1 calc R . . C27 C 0.7741(2) 0.4962(7) 0.8475(5) 0.0204(18) Uani 1 1 d . . . C28 C 0.7736(3) 0.6254(8) 0.8530(6) 0.0260(19) Uani 1 1 d . . . H28 H 0.7962 0.6716 0.8221 0.031 Uiso 1 1 calc R . . C29 C 0.7409(3) 0.6856(9) 0.9025(7) 0.028(2) Uani 1 1 d . . . H29 H 0.7408 0.7730 0.9046 0.034 Uiso 1 1 calc R . . C30 C 0.7083(3) 0.6207(9) 0.9491(7) 0.036(2) Uani 1 1 d . . . H30 H 0.6858 0.6628 0.9835 0.044 Uiso 1 1 calc R . . C31 C 0.7087(3) 0.4940(9) 0.9455(6) 0.035(2) Uani 1 1 d . . . H31 H 0.6865 0.4483 0.9780 0.042 Uiso 1 1 calc R . . C32 C 0.7413(3) 0.4336(8) 0.8944(6) 0.0243(18) Uani 1 1 d . . . H32 H 0.7410 0.3462 0.8918 0.029 Uiso 1 1 calc R . . C33 C 0.8157(3) 0.1857(9) 0.4204(7) 0.027(2) Uani 1 1 d . . . H33 H 0.7964 0.2531 0.4007 0.033 Uiso 1 1 calc R . . C34 C 0.8216(3) 0.0940(8) 0.3506(7) 0.028(2) Uani 1 1 d . . . H34 H 0.8069 0.0990 0.2827 0.033 Uiso 1 1 calc R . . C35 C 0.8485(2) -0.0040(8) 0.3783(6) 0.0245(19) Uani 1 1 d . . . C36 C 0.8704(2) -0.0064(7) 0.4781(6) 0.0250(19) Uani 1 1 d . . . H36 H 0.8902 -0.0725 0.4993 0.030 Uiso 1 1 calc R . . C37 C 0.8633(3) 0.0869(8) 0.5445(7) 0.028(2) Uani 1 1 d . . . H37 H 0.8775 0.0842 0.6130 0.034 Uiso 1 1 calc R . . C38 C 0.8537(3) -0.1088(9) 0.3057(8) 0.042(2) Uani 1 1 d . . . H38A H 0.8278 -0.1649 0.3078 0.062 Uiso 1 1 calc R . . H38B H 0.8820 -0.1530 0.3264 0.062 Uiso 1 1 calc R . . H38C H 0.8547 -0.0770 0.2353 0.062 Uiso 1 1 calc R . . Sb1 Sb 0.99653(2) 0.94313(5) 0.69231(5) 0.03587(17) Uani 1 1 d . . . Sb2 Sb 0.755835(19) 0.52892(5) 0.29218(4) 0.02650(14) Uani 1 1 d . . . F1A F 1.0360(3) 0.8045(10) 0.7016(9) 0.071(3) Uiso 0.740(8) 1 d P A 1 F2A F 0.9553(3) 1.0676(8) 0.6796(6) 0.053(2) Uiso 0.740(8) 1 d P A 1 F3A F 0.9621(2) 0.8558(6) 0.5848(5) 0.0288(18) Uiso 0.740(8) 1 d P A 1 F4A F 1.0280(3) 1.0153(10) 0.7988(8) 0.076(3) Uiso 0.740(8) 1 d P A 1 F5A F 1.0308(3) 1.0184(9) 0.5992(7) 0.064(3) Uiso 0.740(8) 1 d P A 1 F6A F 0.9615(4) 0.8586(9) 0.7800(8) 0.064(3) Uiso 0.740(8) 1 d P A 1 F1B F 1.0360(10) 0.832(3) 0.639(2) 0.070(8) Uiso 0.260(8) 1 d P A 2 F2B F 0.9871(12) 1.070(3) 0.803(3) 0.103(12) Uiso 0.260(8) 1 d P A 2 F3B F 0.9368(13) 0.909(4) 0.710(3) 0.114(13) Uiso 0.260(8) 1 d P A 2 F4B F 1.0536(10) 1.010(3) 0.749(2) 0.075(9) Uiso 0.260(8) 1 d P A 2 F5B F 0.9815(12) 1.075(3) 0.599(3) 0.105(12) Uiso 0.260(8) 1 d P A 2 F6B F 0.9958(10) 0.844(3) 0.803(2) 0.069(9) Uiso 0.260(8) 1 d P A 2 F7 F 0.8000(2) 0.4116(6) 0.2691(5) 0.0628(19) Uani 1 1 d . . . F8 F 0.7133(2) 0.6475(6) 0.3127(5) 0.0594(19) Uani 1 1 d . . . F9 F 0.7118(2) 0.4338(6) 0.2181(5) 0.0628(18) Uani 1 1 d . . . F10 F 0.8003(2) 0.6194(6) 0.3678(5) 0.0556(18) Uani 1 1 d . . . F11 F 0.7693(2) 0.6082(6) 0.1734(4) 0.0502(16) Uani 1 1 d . . . F12 F 0.74324(18) 0.4486(6) 0.4137(4) 0.0496(15) Uani 1 1 d . . . H1 H 0.830(3) 0.228(7) 0.567(4) 0.03(2) Uiso 1 1 d 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 Ru 0.0160(3) 0.0161(3) 0.0189(3) -0.0008(3) -0.0008(2) 0.0000(3) P1 0.0193(9) 0.0165(11) 0.0177(9) -0.0012(8) -0.0023(7) -0.0003(8) O1 0.018(3) 0.018(3) 0.028(3) -0.004(2) 0.004(2) -0.005(2) O2 0.027(3) 0.014(3) 0.023(3) 0.004(2) 0.001(2) -0.001(2) N1 0.027(4) 0.022(4) 0.030(4) -0.008(3) 0.009(3) 0.000(3) C1 0.007(3) 0.037(5) 0.025(4) -0.005(4) 0.006(3) -0.004(3) C2 0.020(4) 0.018(5) 0.027(4) -0.001(3) 0.003(3) -0.002(3) C3 0.021(4) 0.028(5) 0.032(5) -0.004(4) 0.009(4) -0.005(4) C4 0.012(3) 0.032(5) 0.032(4) 0.000(4) 0.002(3) 0.009(4) C5 0.018(4) 0.023(5) 0.032(5) 0.000(4) -0.003(4) 0.013(3) C6 0.016(4) 0.023(5) 0.027(4) -0.003(4) 0.003(3) 0.009(3) C7 0.016(4) 0.031(5) 0.025(4) -0.004(4) 0.001(3) 0.000(3) C8 0.041(5) 0.033(5) 0.029(5) -0.010(4) 0.008(4) -0.006(4) C9 0.038(5) 0.041(5) 0.025(4) 0.007(5) 0.005(4) 0.000(5) C10 0.016(4) 0.050(7) 0.036(5) 0.005(4) -0.003(3) 0.000(4) C11 0.017(4) 0.023(5) 0.019(4) -0.003(3) 0.004(3) -0.001(3) C12 0.030(5) 0.022(5) 0.032(5) -0.004(4) -0.008(4) 0.000(4) C13 0.051(6) 0.024(5) 0.037(5) 0.002(4) -0.021(5) 0.004(5) C14 0.056(6) 0.018(5) 0.036(5) 0.005(4) -0.017(5) 0.008(4) C15 0.032(5) 0.017(5) 0.039(5) -0.001(4) -0.010(4) 0.000(4) C16 0.029(4) 0.027(5) 0.016(4) 0.003(3) -0.001(3) 0.003(4) C17 0.019(4) 0.022(4) 0.015(4) 0.002(3) -0.005(3) 0.004(3) C18 0.029(4) 0.018(4) 0.020(4) -0.004(3) -0.003(3) -0.001(3) C19 0.042(5) 0.032(5) 0.015(4) -0.004(4) 0.000(4) 0.012(4) C20 0.038(5) 0.021(5) 0.027(5) -0.012(4) -0.009(4) -0.002(4) C21 0.028(5) 0.023(5) 0.030(5) -0.003(4) 0.003(4) -0.004(4) C22 0.026(4) 0.017(4) 0.021(4) -0.004(3) 0.002(3) 0.001(3) C23 0.013(3) 0.016(4) 0.022(4) -0.005(3) 0.003(3) -0.002(3) C24 0.017(4) 0.024(4) 0.019(4) -0.008(3) 0.003(3) -0.003(3) C25 0.022(4) 0.027(5) 0.013(4) 0.003(3) -0.002(3) 0.008(3) C26 0.032(5) 0.020(5) 0.042(6) 0.008(4) -0.005(4) 0.000(4) C27 0.024(4) 0.022(5) 0.016(3) -0.003(3) 0.005(3) 0.004(3) C28 0.019(4) 0.032(5) 0.026(4) 0.001(4) -0.004(3) 0.006(4) C29 0.025(5) 0.034(5) 0.026(4) 0.000(4) 0.001(4) 0.014(4) C30 0.035(5) 0.051(7) 0.022(4) -0.014(4) -0.006(4) 0.022(5) C31 0.022(4) 0.054(7) 0.031(5) 0.006(4) 0.015(4) -0.005(4) C32 0.026(4) 0.025(5) 0.021(4) 0.002(4) -0.005(3) -0.001(4) C33 0.017(4) 0.032(5) 0.032(5) -0.001(4) -0.001(4) 0.000(4) C34 0.024(4) 0.030(5) 0.029(5) 0.001(4) -0.001(4) 0.000(4) C35 0.018(4) 0.031(5) 0.024(4) -0.003(3) -0.005(3) -0.002(3) C36 0.015(4) 0.015(4) 0.046(5) 0.007(4) 0.009(4) 0.000(3) C37 0.033(5) 0.024(5) 0.026(4) -0.003(4) -0.003(4) -0.008(4) C38 0.041(6) 0.045(6) 0.040(6) -0.018(5) 0.007(5) -0.003(5) Sb1 0.0357(3) 0.0289(4) 0.0421(4) 0.0078(3) -0.0023(3) -0.0023(3) Sb2 0.0252(3) 0.0247(3) 0.0281(3) 0.0016(3) -0.0054(2) 0.0034(3) F7 0.053(4) 0.050(4) 0.085(5) -0.011(4) 0.008(4) 0.023(3) F8 0.067(4) 0.062(4) 0.053(4) 0.017(3) 0.027(3) 0.034(4) F9 0.059(4) 0.065(5) 0.062(4) -0.015(4) -0.011(3) -0.026(4) F10 0.045(4) 0.081(5) 0.038(3) -0.001(3) -0.008(3) -0.021(3) F11 0.055(4) 0.060(4) 0.036(3) 0.013(3) 0.009(3) -0.003(3) F12 0.052(3) 0.050(4) 0.044(3) 0.018(3) -0.008(3) -0.008(3) _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 Ru O1 2.063(5) . ? Ru C6 2.129(8) . ? Ru C5 2.142(8) . ? Ru O2 2.170(5) . ? Ru C3 2.202(8) . ? Ru C4 2.215(7) . ? Ru C2 2.236(8) . ? Ru C1 2.261(7) . ? Ru P1 2.3328(19) . ? P1 C17 1.802(8) . ? P1 C11 1.815(9) . ? P1 C23 1.869(7) . ? O1 C24 1.396(9) . ? O2 C26 1.415(10) . ? O2 C25 1.474(9) . ? N1 C33 1.333(11) . ? N1 C37 1.334(11) . ? N1 H1 0.88(2) . ? C1 C2 1.383(11) . ? C1 C6 1.429(12) . ? C1 C7 1.519(10) . ? C2 C3 1.423(11) . ? C2 H2 0.9500 . ? C3 C4 1.387(12) . ? C3 H3 0.9500 . ? C4 C5 1.421(12) . ? C4 C10 1.518(11) . ? C5 C6 1.395(11) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.533(12) . ? C7 C9 1.534(12) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.371(11) . ? C11 C16 1.408(11) . ? C12 C13 1.389(12) . ? C12 H12 0.9500 . ? C13 C14 1.384(13) . ? C13 H13 0.9500 . ? C14 C15 1.352(12) . ? C14 H14 0.9500 . ? C15 C16 1.370(11) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.386(11) . ? C17 C18 1.390(10) . ? C18 C19 1.378(11) . ? C18 H18 0.9500 . ? C19 C20 1.377(12) . ? C19 H19 0.9500 . ? C20 C21 1.373(12) . ? C20 H20 0.9500 . ? C21 C22 1.410(11) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C27 1.493(10) . ? C23 C24 1.558(10) . ? C23 H23 1.0000 . ? C24 C25 1.499(12) . ? C24 H24 1.0000 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C32 1.369(11) . ? C27 C28 1.407(12) . ? C28 C29 1.371(11) . ? C28 H28 0.9500 . ? C29 C30 1.375(13) . ? C29 H29 0.9500 . ? C30 C31 1.378(13) . ? C30 H30 0.9500 . ? C31 C32 1.384(11) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.368(12) . ? C33 H33 0.9500 . ? C34 C35 1.358(11) . ? C34 H34 0.9500 . ? C35 C36 1.399(11) . ? C35 C38 1.495(12) . ? C36 C37 1.360(11) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? Sb1 F4A 1.780(10) . ? Sb1 F6B 1.80(3) . ? Sb1 F2A 1.817(8) . ? Sb1 F5A 1.835(9) . ? Sb1 F3B 1.83(4) . ? Sb1 F6A 1.848(10) . ? Sb1 F1B 1.86(3) . ? Sb1 F5B 1.90(4) . ? Sb1 F1A 1.902(11) . ? Sb1 F3A 1.908(6) . ? Sb1 F4B 1.92(3) . ? Sb1 F2B 2.03(4) . ? Sb2 F8 1.836(6) . ? Sb2 F11 1.840(5) . ? Sb2 F10 1.852(6) . ? Sb2 F9 1.862(6) . ? Sb2 F7 1.867(6) . ? Sb2 F12 1.870(5) . ? 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 O1 Ru C6 91.1(3) . . ? O1 Ru C5 113.5(3) . . ? C6 Ru C5 38.1(3) . . ? O1 Ru O2 78.3(2) . . ? C6 Ru O2 150.5(3) . . ? C5 Ru O2 167.6(3) . . ? O1 Ru C3 162.3(3) . . ? C6 Ru C3 79.4(3) . . ? C5 Ru C3 67.3(3) . . ? O2 Ru C3 102.8(3) . . ? O1 Ru C4 150.6(3) . . ? C6 Ru C4 68.2(3) . . ? C5 Ru C4 38.0(3) . . ? O2 Ru C4 129.7(3) . . ? C3 Ru C4 36.6(3) . . ? O1 Ru C2 125.0(3) . . ? C6 Ru C2 65.8(3) . . ? C5 Ru C2 78.8(3) . . ? O2 Ru C2 97.8(2) . . ? C3 Ru C2 37.4(3) . . ? C4 Ru C2 66.5(3) . . ? O1 Ru C1 96.3(2) . . ? C6 Ru C1 37.8(3) . . ? C5 Ru C1 68.7(3) . . ? O2 Ru C1 115.3(3) . . ? C3 Ru C1 67.1(3) . . ? C4 Ru C1 80.3(3) . . ? C2 Ru C1 35.8(3) . . ? O1 Ru P1 77.85(16) . . ? C6 Ru P1 126.3(2) . . ? C5 Ru P1 99.4(2) . . ? O2 Ru P1 78.75(15) . . ? C3 Ru P1 119.8(2) . . ? C4 Ru P1 97.2(2) . . ? C2 Ru P1 156.1(2) . . ? C1 Ru P1 163.7(2) . . ? C17 P1 C11 105.2(3) . . ? C17 P1 C23 110.9(3) . . ? C11 P1 C23 107.0(4) . . ? C17 P1 Ru 117.6(3) . . ? C11 P1 Ru 114.8(3) . . ? C23 P1 Ru 101.0(2) . . ? C24 O1 Ru 109.3(4) . . ? C26 O2 C25 111.6(6) . . ? C26 O2 Ru 122.7(5) . . ? C25 O2 Ru 109.6(4) . . ? C33 N1 C37 120.0(7) . . ? C33 N1 H1 125(6) . . ? C37 N1 H1 113(6) . . ? C2 C1 C6 115.0(7) . . ? C2 C1 C7 124.5(8) . . ? C6 C1 C7 120.2(8) . . ? C2 C1 Ru 71.1(4) . . ? C6 C1 Ru 66.1(4) . . ? C7 C1 Ru 127.1(5) . . ? C1 C2 C3 123.1(8) . . ? C1 C2 Ru 73.1(4) . . ? C3 C2 Ru 70.0(4) . . ? C1 C2 H2 118.4 . . ? C3 C2 H2 118.4 . . ? Ru C2 H2 131.7 . . ? C4 C3 C2 120.7(8) . . ? C4 C3 Ru 72.2(5) . . ? C2 C3 Ru 72.6(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? Ru C3 H3 127.6 . . ? C3 C4 C5 117.9(7) . . ? C3 C4 C10 122.1(8) . . ? C5 C4 C10 120.0(8) . . ? C3 C4 Ru 71.2(5) . . ? C5 C4 Ru 68.2(4) . . ? C10 C4 Ru 132.9(5) . . ? C6 C5 C4 119.9(8) . . ? C6 C5 Ru 70.4(4) . . ? C4 C5 Ru 73.8(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? Ru C5 H5 127.8 . . ? C5 C6 C1 123.3(8) . . ? C5 C6 Ru 71.5(5) . . ? C1 C6 Ru 76.1(5) . . ? C5 C6 H6 118.4 . . ? C1 C6 H6 118.4 . . ? Ru C6 H6 126.0 . . ? C1 C7 C8 111.8(7) . . ? C1 C7 C9 111.5(7) . . ? C8 C7 C9 111.6(7) . . ? C1 C7 H7 107.2 . . ? C8 C7 H7 107.2 . . ? C9 C7 H7 107.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 119.3(8) . . ? C12 C11 P1 122.4(7) . . ? C16 C11 P1 118.0(6) . . ? C11 C12 C13 121.0(8) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 118.6(8) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C15 C14 C13 120.7(8) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 121.6(8) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C11 118.8(8) . . ? C15 C16 H16 120.6 . . ? C11 C16 H16 120.6 . . ? C22 C17 C18 118.8(7) . . ? C22 C17 P1 118.7(6) . . ? C18 C17 P1 122.3(6) . . ? C19 C18 C17 120.8(8) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 119.7(8) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 121.4(8) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 118.6(8) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C17 C22 C21 120.6(8) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C27 C23 C24 118.2(6) . . ? C27 C23 P1 117.0(5) . . ? C24 C23 P1 105.7(5) . . ? C27 C23 H23 104.8 . . ? C24 C23 H23 104.8 . . ? P1 C23 H23 104.8 . . ? O1 C24 C25 107.6(6) . . ? O1 C24 C23 108.2(6) . . ? C25 C24 C23 114.9(6) . . ? O1 C24 H24 108.6 . . ? C25 C24 H24 108.6 . . ? C23 C24 H24 108.6 . . ? O2 C25 C24 106.0(6) . . ? O2 C25 H25A 110.5 . . ? C24 C25 H25A 110.5 . . ? O2 C25 H25B 110.5 . . ? C24 C25 H25B 110.5 . . ? H25A C25 H25B 108.7 . . ? O2 C26 H26A 109.5 . . ? O2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 117.5(8) . . ? C32 C27 C23 120.1(7) . . ? C28 C27 C23 122.2(7) . . ? C29 C28 C27 120.8(8) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.6(9) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C31 119.4(8) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C30 C31 C32 119.9(8) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C27 C32 C31 121.8(8) . . ? C27 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? N1 C33 C34 121.1(8) . . ? N1 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C35 C34 C33 120.1(8) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 118.2(8) . . ? C34 C35 C38 121.4(8) . . ? C36 C35 C38 120.4(8) . . ? C37 C36 C35 119.3(8) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? N1 C37 C36 121.3(8) . . ? N1 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? F4A Sb1 F6B 71.8(10) . . ? F4A Sb1 F2A 92.4(4) . . ? F6B Sb1 F2A 117.8(10) . . ? F4A Sb1 F5A 92.0(4) . . ? F6B Sb1 F5A 147.1(10) . . ? F2A Sb1 F5A 90.6(4) . . ? F4A Sb1 F3B 115.6(12) . . ? F6B Sb1 F3B 72.5(15) . . ? F2A Sb1 F3B 61.3(13) . . ? F5A Sb1 F3B 139.8(13) . . ? F4A Sb1 F6A 91.3(5) . . ? F6B Sb1 F6A 33.2(9) . . ? F2A Sb1 F6A 91.2(4) . . ? F5A Sb1 F6A 176.2(4) . . ? F3B Sb1 F6A 39.3(12) . . ? F4A Sb1 F1B 106.0(10) . . ? F6B Sb1 F1B 87.5(14) . . ? F2A Sb1 F1B 152.8(10) . . ? F5A Sb1 F1B 69.3(10) . . ? F3B Sb1 F1B 123.8(15) . . ? F6A Sb1 F1B 107.9(10) . . ? F4A Sb1 F5B 103.8(11) . . ? F6B Sb1 F5B 160.4(14) . . ? F2A Sb1 F5B 42.6(11) . . ? F5A Sb1 F5B 49.9(11) . . ? F3B Sb1 F5B 93.4(17) . . ? F6A Sb1 F5B 130.9(11) . . ? F1B Sb1 F5B 112.0(15) . . ? F4A Sb1 F1A 91.4(5) . . ? F6B Sb1 F1A 61.5(10) . . ? F2A Sb1 F1A 175.6(4) . . ? F5A Sb1 F1A 91.5(4) . . ? F3B Sb1 F1A 114.9(13) . . ? F6A Sb1 F1A 86.5(5) . . ? F1B Sb1 F1A 26.6(9) . . ? F5B Sb1 F1A 138.1(12) . . ? F4A Sb1 F3A 175.8(4) . . ? F6B Sb1 F3A 104.0(10) . . ? F2A Sb1 F3A 89.7(3) . . ? F5A Sb1 F3A 91.6(3) . . ? F3B Sb1 F3A 62.4(12) . . ? F6A Sb1 F3A 85.0(4) . . ? F1B Sb1 F3A 73.3(10) . . ? F5B Sb1 F3A 80.2(11) . . ? F1A Sb1 F3A 86.4(4) . . ? F4A Sb1 F4B 32.4(8) . . ? F6B Sb1 F4B 89.6(13) . . ? F2A Sb1 F4B 108.2(9) . . ? F5A Sb1 F4B 64.4(9) . . ? F3B Sb1 F4B 148.0(15) . . ? F6A Sb1 F4B 118.2(9) . . ? F1B Sb1 F4B 80.3(13) . . ? F5B Sb1 F4B 96.1(14) . . ? F1A Sb1 F4B 76.3(10) . . ? F3A Sb1 F4B 149.5(9) . . ? F4A Sb1 F2B 41.0(10) . . ? F6B Sb1 F2B 80.5(13) . . ? F2A Sb1 F2B 54.9(11) . . ? F5A Sb1 F2B 106.2(10) . . ? F3B Sb1 F2B 81.7(15) . . ? F6A Sb1 F2B 77.6(10) . . ? F1B Sb1 F2B 146.9(14) . . ? F5B Sb1 F2B 84.1(15) . . ? F1A Sb1 F2B 128.0(11) . . ? F3A Sb1 F2B 139.4(11) . . ? F4B Sb1 F2B 69.1(13) . . ? F8 Sb2 F11 89.6(3) . . ? F8 Sb2 F10 90.7(3) . . ? F11 Sb2 F10 90.1(3) . . ? F8 Sb2 F9 90.5(3) . . ? F11 Sb2 F9 91.1(3) . . ? F10 Sb2 F9 178.3(3) . . ? F8 Sb2 F7 178.3(3) . . ? F11 Sb2 F7 88.9(3) . . ? F10 Sb2 F7 88.6(3) . . ? F9 Sb2 F7 90.2(3) . . ? F8 Sb2 F12 90.9(3) . . ? F11 Sb2 F12 179.0(3) . . ? F10 Sb2 F12 89.1(3) . . ? F9 Sb2 F12 89.8(3) . . ? F7 Sb2 F12 90.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ru P1 C17 -144.2(3) . . . . ? C6 Ru P1 C17 133.4(4) . . . . ? C5 Ru P1 C17 103.6(4) . . . . ? O2 Ru P1 C17 -63.9(3) . . . . ? C3 Ru P1 C17 34.5(4) . . . . ? C4 Ru P1 C17 65.2(4) . . . . ? C2 Ru P1 C17 19.9(6) . . . . ? C1 Ru P1 C17 145.5(7) . . . . ? O1 Ru P1 C11 91.3(3) . . . . ? C6 Ru P1 C11 8.9(4) . . . . ? C5 Ru P1 C11 -20.9(4) . . . . ? O2 Ru P1 C11 171.6(3) . . . . ? C3 Ru P1 C11 -90.0(4) . . . . ? C4 Ru P1 C11 -59.3(4) . . . . ? C2 Ru P1 C11 -104.6(6) . . . . ? C1 Ru P1 C11 20.9(7) . . . . ? O1 Ru P1 C23 -23.5(3) . . . . ? C6 Ru P1 C23 -105.8(4) . . . . ? C5 Ru P1 C23 -135.7(3) . . . . ? O2 Ru P1 C23 56.8(3) . . . . ? C3 Ru P1 C23 155.2(4) . . . . ? C4 Ru P1 C23 -174.1(3) . . . . ? C2 Ru P1 C23 140.7(6) . . . . ? C1 Ru P1 C23 -93.8(7) . . . . ? C6 Ru O1 C24 -179.7(5) . . . . ? C5 Ru O1 C24 148.5(5) . . . . ? O2 Ru O1 C24 -27.5(5) . . . . ? C3 Ru O1 C24 -122.8(9) . . . . ? C4 Ru O1 C24 136.5(6) . . . . ? C2 Ru O1 C24 -118.8(5) . . . . ? C1 Ru O1 C24 -142.1(5) . . . . ? P1 Ru O1 C24 53.4(4) . . . . ? O1 Ru O2 C26 -138.1(6) . . . . ? C6 Ru O2 C26 -67.0(8) . . . . ? C5 Ru O2 C26 59.4(15) . . . . ? C3 Ru O2 C26 23.8(6) . . . . ? C4 Ru O2 C26 52.0(7) . . . . ? C2 Ru O2 C26 -13.9(6) . . . . ? C1 Ru O2 C26 -46.6(7) . . . . ? P1 Ru O2 C26 142.1(6) . . . . ? O1 Ru O2 C25 -4.3(4) . . . . ? C6 Ru O2 C25 66.8(7) . . . . ? C5 Ru O2 C25 -166.8(12) . . . . ? C3 Ru O2 C25 157.7(5) . . . . ? C4 Ru O2 C25 -174.1(4) . . . . ? C2 Ru O2 C25 120.0(4) . . . . ? C1 Ru O2 C25 87.2(5) . . . . ? P1 Ru O2 C25 -84.1(4) . . . . ? O1 Ru C1 C2 146.5(5) . . . . ? C6 Ru C1 C2 -129.8(6) . . . . ? C5 Ru C1 C2 -100.7(5) . . . . ? O2 Ru C1 C2 66.4(5) . . . . ? C3 Ru C1 C2 -27.3(5) . . . . ? C4 Ru C1 C2 -63.0(5) . . . . ? P1 Ru C1 C2 -145.7(6) . . . . ? O1 Ru C1 C6 -83.7(5) . . . . ? C5 Ru C1 C6 29.1(5) . . . . ? O2 Ru C1 C6 -163.7(4) . . . . ? C3 Ru C1 C6 102.5(5) . . . . ? C4 Ru C1 C6 66.8(5) . . . . ? C2 Ru C1 C6 129.8(6) . . . . ? P1 Ru C1 C6 -15.9(9) . . . . ? O1 Ru C1 C7 27.1(8) . . . . ? C6 Ru C1 C7 110.8(9) . . . . ? C5 Ru C1 C7 139.9(8) . . . . ? O2 Ru C1 C7 -53.0(8) . . . . ? C3 Ru C1 C7 -146.7(8) . . . . ? C4 Ru C1 C7 177.6(8) . . . . ? C2 Ru C1 C7 -119.4(10) . . . . ? P1 Ru C1 C7 94.9(9) . . . . ? C6 C1 C2 C3 0.5(11) . . . . ? C7 C1 C2 C3 173.9(7) . . . . ? Ru C1 C2 C3 51.3(7) . . . . ? C6 C1 C2 Ru -50.8(6) . . . . ? C7 C1 C2 Ru 122.6(7) . . . . ? O1 Ru C2 C1 -42.1(5) . . . . ? C6 Ru C2 C1 31.1(4) . . . . ? C5 Ru C2 C1 68.9(5) . . . . ? O2 Ru C2 C1 -123.2(4) . . . . ? C3 Ru C2 C1 135.9(7) . . . . ? C4 Ru C2 C1 106.8(5) . . . . ? P1 Ru C2 C1 157.0(4) . . . . ? O1 Ru C2 C3 -178.0(4) . . . . ? C6 Ru C2 C3 -104.8(5) . . . . ? C5 Ru C2 C3 -67.0(5) . . . . ? O2 Ru C2 C3 100.8(5) . . . . ? C4 Ru C2 C3 -29.2(5) . . . . ? C1 Ru C2 C3 -135.9(7) . . . . ? P1 Ru C2 C3 21.0(8) . . . . ? C1 C2 C3 C4 3.5(12) . . . . ? Ru C2 C3 C4 56.1(7) . . . . ? C1 C2 C3 Ru -52.6(7) . . . . ? O1 Ru C3 C4 -126.1(9) . . . . ? C6 Ru C3 C4 -67.7(5) . . . . ? C5 Ru C3 C4 -29.8(5) . . . . ? O2 Ru C3 C4 142.4(5) . . . . ? C2 Ru C3 C4 -131.4(7) . . . . ? C1 Ru C3 C4 -105.2(5) . . . . ? P1 Ru C3 C4 58.2(5) . . . . ? O1 Ru C3 C2 5.3(12) . . . . ? C6 Ru C3 C2 63.8(5) . . . . ? C5 Ru C3 C2 101.7(5) . . . . ? O2 Ru C3 C2 -86.1(5) . . . . ? C4 Ru C3 C2 131.4(7) . . . . ? C1 Ru C3 C2 26.2(5) . . . . ? P1 Ru C3 C2 -170.3(4) . . . . ? C2 C3 C4 C5 -4.9(11) . . . . ? Ru C3 C4 C5 51.4(6) . . . . ? C2 C3 C4 C10 174.3(7) . . . . ? Ru C3 C4 C10 -129.4(7) . . . . ? C2 C3 C4 Ru -56.3(7) . . . . ? O1 Ru C4 C3 150.0(5) . . . . ? C6 Ru C4 C3 101.8(5) . . . . ? C5 Ru C4 C3 132.0(7) . . . . ? O2 Ru C4 C3 -50.6(6) . . . . ? C2 Ru C4 C3 29.8(5) . . . . ? C1 Ru C4 C3 64.4(5) . . . . ? P1 Ru C4 C3 -131.9(5) . . . . ? O1 Ru C4 C5 18.1(8) . . . . ? C6 Ru C4 C5 -30.2(5) . . . . ? O2 Ru C4 C5 177.4(4) . . . . ? C3 Ru C4 C5 -132.0(7) . . . . ? C2 Ru C4 C5 -102.2(5) . . . . ? C1 Ru C4 C5 -67.6(5) . . . . ? P1 Ru C4 C5 96.1(5) . . . . ? O1 Ru C4 C10 -93.2(10) . . . . ? C6 Ru C4 C10 -141.5(10) . . . . ? C5 Ru C4 C10 -111.3(11) . . . . ? O2 Ru C4 C10 66.1(10) . . . . ? C3 Ru C4 C10 116.7(11) . . . . ? C2 Ru C4 C10 146.5(10) . . . . ? C1 Ru C4 C10 -178.9(9) . . . . ? P1 Ru C4 C10 -15.2(9) . . . . ? C3 C4 C5 C6 2.5(11) . . . . ? C10 C4 C5 C6 -176.7(7) . . . . ? Ru C4 C5 C6 55.3(7) . . . . ? C3 C4 C5 Ru -52.8(7) . . . . ? C10 C4 C5 Ru 128.0(6) . . . . ? O1 Ru C5 C6 58.7(6) . . . . ? O2 Ru C5 C6 -140.0(12) . . . . ? C3 Ru C5 C6 -102.1(6) . . . . ? C4 Ru C5 C6 -130.9(8) . . . . ? C2 Ru C5 C6 -64.8(5) . . . . ? C1 Ru C5 C6 -28.9(5) . . . . ? P1 Ru C5 C6 139.5(5) . . . . ? O1 Ru C5 C4 -170.5(4) . . . . ? C6 Ru C5 C4 130.9(8) . . . . ? O2 Ru C5 C4 -9.2(16) . . . . ? C3 Ru C5 C4 28.7(5) . . . . ? C2 Ru C5 C4 66.1(5) . . . . ? C1 Ru C5 C4 102.0(5) . . . . ? P1 Ru C5 C4 -89.7(5) . . . . ? C4 C5 C6 C1 1.6(12) . . . . ? Ru C5 C6 C1 58.4(7) . . . . ? C4 C5 C6 Ru -56.9(7) . . . . ? C2 C1 C6 C5 -3.0(11) . . . . ? C7 C1 C6 C5 -176.7(7) . . . . ? Ru C1 C6 C5 -56.3(7) . . . . ? C2 C1 C6 Ru 53.3(6) . . . . ? C7 C1 C6 Ru -120.4(6) . . . . ? O1 Ru C6 C5 -128.4(5) . . . . ? O2 Ru C6 C5 163.7(5) . . . . ? C3 Ru C6 C5 66.6(5) . . . . ? C4 Ru C6 C5 30.1(5) . . . . ? C2 Ru C6 C5 103.2(6) . . . . ? C1 Ru C6 C5 132.8(7) . . . . ? P1 Ru C6 C5 -52.7(6) . . . . ? O1 Ru C6 C1 98.8(4) . . . . ? C5 Ru C6 C1 -132.8(7) . . . . ? O2 Ru C6 C1 30.9(8) . . . . ? C3 Ru C6 C1 -66.2(5) . . . . ? C4 Ru C6 C1 -102.7(5) . . . . ? C2 Ru C6 C1 -29.5(4) . . . . ? P1 Ru C6 C1 174.5(3) . . . . ? C2 C1 C7 C8 136.3(8) . . . . ? C6 C1 C7 C8 -50.6(9) . . . . ? Ru C1 C7 C8 -132.1(7) . . . . ? C2 C1 C7 C9 10.6(10) . . . . ? C6 C1 C7 C9 -176.4(7) . . . . ? Ru C1 C7 C9 102.1(8) . . . . ? C17 P1 C11 C12 -16.8(8) . . . . ? C23 P1 C11 C12 -134.8(7) . . . . ? Ru P1 C11 C12 114.0(7) . . . . ? C17 P1 C11 C16 168.7(6) . . . . ? C23 P1 C11 C16 50.7(7) . . . . ? Ru P1 C11 C16 -60.5(7) . . . . ? C16 C11 C12 C13 -0.3(13) . . . . ? P1 C11 C12 C13 -174.8(7) . . . . ? C11 C12 C13 C14 0.0(15) . . . . ? C12 C13 C14 C15 0.3(16) . . . . ? C13 C14 C15 C16 -0.3(16) . . . . ? C14 C15 C16 C11 -0.1(14) . . . . ? C12 C11 C16 C15 0.3(12) . . . . ? P1 C11 C16 C15 175.0(6) . . . . ? C11 P1 C17 C22 119.7(7) . . . . ? C23 P1 C17 C22 -125.0(6) . . . . ? Ru P1 C17 C22 -9.5(7) . . . . ? C11 P1 C17 C18 -55.2(7) . . . . ? C23 P1 C17 C18 60.2(7) . . . . ? Ru P1 C17 C18 175.6(5) . . . . ? C22 C17 C18 C19 0.5(12) . . . . ? P1 C17 C18 C19 175.4(6) . . . . ? C17 C18 C19 C20 -2.3(12) . . . . ? C18 C19 C20 C21 1.9(13) . . . . ? C19 C20 C21 C22 0.3(13) . . . . ? C18 C17 C22 C21 1.7(12) . . . . ? P1 C17 C22 C21 -173.3(6) . . . . ? C20 C21 C22 C17 -2.1(13) . . . . ? C17 P1 C23 C27 -10.5(7) . . . . ? C11 P1 C23 C27 103.7(6) . . . . ? Ru P1 C23 C27 -135.9(5) . . . . ? C17 P1 C23 C24 123.4(5) . . . . ? C11 P1 C23 C24 -122.4(5) . . . . ? Ru P1 C23 C24 -2.0(5) . . . . ? Ru O1 C24 C25 54.7(6) . . . . ? Ru O1 C24 C23 -70.1(6) . . . . ? C27 C23 C24 O1 174.9(6) . . . . ? P1 C23 C24 O1 41.6(7) . . . . ? C27 C23 C24 C25 54.6(9) . . . . ? P1 C23 C24 C25 -78.7(7) . . . . ? C26 O2 C25 C24 171.7(6) . . . . ? Ru O2 C25 C24 32.5(6) . . . . ? O1 C24 C25 O2 -57.4(7) . . . . ? C23 C24 C25 O2 63.3(8) . . . . ? C24 C23 C27 C32 109.5(8) . . . . ? P1 C23 C27 C32 -122.4(7) . . . . ? C24 C23 C27 C28 -67.3(10) . . . . ? P1 C23 C27 C28 60.8(9) . . . . ? C32 C27 C28 C29 -0.9(12) . . . . ? C23 C27 C28 C29 176.0(7) . . . . ? C27 C28 C29 C30 0.9(13) . . . . ? C28 C29 C30 C31 -0.2(13) . . . . ? C29 C30 C31 C32 -0.6(14) . . . . ? C28 C27 C32 C31 0.1(11) . . . . ? C23 C27 C32 C31 -176.8(7) . . . . ? C30 C31 C32 C27 0.6(13) . . . . ? C37 N1 C33 C34 -1.2(13) . . . . ? N1 C33 C34 C35 1.3(13) . . . . ? C33 C34 C35 C36 -1.6(12) . . . . ? C33 C34 C35 C38 176.8(8) . . . . ? C34 C35 C36 C37 1.8(11) . . . . ? C38 C35 C36 C37 -176.6(8) . . . . ? C33 N1 C37 C36 1.5(12) . . . . ? C35 C36 C37 N1 -1.8(12) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.614 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.157