data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'P C McGowan' _publ_contact_author_email P.C.MCGOWAN@CHEM.LEEDS.AC.UK _publ_section_title ; Controlling the Binding of Dihydrogen Using Ruthenium Complexes Containing N-mono-Functionalised 1,4,7-Triazacyclononane Ligand Systems ; loop_ _publ_author_name 'P C McGowan' 'Andrew L Gott' 'Thomas J Podesta' # Attachment 'RuH170408.cif' data_tjp17 _database_code_depnum_ccdc_archive 'CCDC 685068' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'in paper 1' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 B Cl2 F4 N4 O P Ru' _chemical_formula_weight 784.41 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' 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' B B 0.0013 0.0007 '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' 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 P21/c 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 8.9651(2) _cell_length_b 18.4207(4) _cell_length_c 21.1509(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.6010(10) _cell_angle_gamma 90.00 _cell_volume 3469.78(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8717 _exptl_absorpt_correction_T_max 0.8717 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35264 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6791 _reflns_number_gt 5827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+3.9224P] 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 SHELXL _refine_ls_extinction_coef 0.0026(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6791 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.45712(2) 0.519262(11) 0.201327(9) 0.02243(9) Uani 1 1 d . . . Cl1 Cl 0.76088(12) 0.59810(6) 0.46356(5) 0.0594(2) Uani 1 1 d . . . Cl2 Cl 0.56456(19) 0.66185(8) 0.54911(6) 0.0983(5) Uani 1 1 d . . . P1 P 0.55869(8) 0.40675(3) 0.20764(3) 0.02320(15) Uani 1 1 d . . . F1 F 0.9084(2) 0.70659(10) 0.07096(10) 0.0537(5) Uani 1 1 d . . . F2 F 0.7135(2) 0.65237(10) 0.01082(8) 0.0432(4) Uani 1 1 d . . . F3 F 0.9235(2) 0.58819(10) 0.04501(8) 0.0443(4) Uani 1 1 d . . . F4 F 0.7663(2) 0.62336(12) 0.11524(9) 0.0506(5) Uani 1 1 d . . . O1 O 0.7475(3) 0.57456(12) 0.26811(12) 0.0478(6) Uani 1 1 d . . . N1 N 0.3336(3) 0.62271(12) 0.20030(10) 0.0257(5) Uani 1 1 d . . . N2 N 0.2383(2) 0.48478(12) 0.15704(10) 0.0263(5) Uani 1 1 d . . . H2 H 0.2227 0.4371 0.1692 0.032 Uiso 1 1 calc R . . N3 N 0.4661(3) 0.55386(12) 0.10125(10) 0.0273(5) Uani 1 1 d . . . H3 H 0.5653 0.5524 0.0923 0.033 Uiso 1 1 calc R . . N4 N 0.1447(3) 0.62676(15) 0.31850(12) 0.0399(6) Uani 1 1 d . . . C1 C 0.1695(3) 0.61066(15) 0.17847(13) 0.0289(6) Uani 1 1 d . . . H1A H 0.1475 0.6260 0.1335 0.035 Uiso 1 1 calc R . . H1B H 0.1083 0.6409 0.2044 0.035 Uiso 1 1 calc R . . C2 C 0.1269(3) 0.53201(15) 0.18449(13) 0.0289(6) Uani 1 1 d . . . H2A H 0.1242 0.5197 0.2299 0.035 Uiso 1 1 calc R . . H2B H 0.0256 0.5236 0.1617 0.035 Uiso 1 1 calc R . . C3 C 0.2259(3) 0.48747(15) 0.08573(12) 0.0292(6) Uani 1 1 d . . . H3A H 0.1578 0.5276 0.0702 0.035 Uiso 1 1 calc R . . H3B H 0.1814 0.4415 0.0681 0.035 Uiso 1 1 calc R . . C4 C 0.3781(3) 0.49876(16) 0.06179(13) 0.0296(6) Uani 1 1 d . . . H4A H 0.4338 0.4523 0.0637 0.036 Uiso 1 1 calc R . . H4B H 0.3635 0.5150 0.0169 0.036 Uiso 1 1 calc R . . C5 C 0.4069(3) 0.62909(15) 0.09022(13) 0.0311(6) Uani 1 1 d . . . H5A H 0.3041 0.6270 0.0674 0.037 Uiso 1 1 calc R . . H5B H 0.4713 0.6560 0.0633 0.037 Uiso 1 1 calc R . . C6 C 0.4036(3) 0.66863(15) 0.15298(13) 0.0306(6) Uani 1 1 d . . . H6A H 0.5074 0.6815 0.1705 0.037 Uiso 1 1 calc R . . H6B H 0.3457 0.7142 0.1456 0.037 Uiso 1 1 calc R . . C7 C 0.3536(3) 0.66314(15) 0.26243(13) 0.0311(6) Uani 1 1 d . . . H7A H 0.3033 0.7109 0.2562 0.037 Uiso 1 1 calc R . . H7B H 0.4621 0.6723 0.2741 0.037 Uiso 1 1 calc R . . C8 C 0.2930(3) 0.62504(15) 0.31726(13) 0.0310(6) Uani 1 1 d . . . C9 C 0.3893(4) 0.59223(17) 0.36505(14) 0.0377(7) Uani 1 1 d . . . H9 H 0.4949 0.5935 0.3638 0.045 Uiso 1 1 calc R . . C10 C 0.3293(4) 0.55758(19) 0.41467(15) 0.0464(8) Uani 1 1 d . . . H10 H 0.3926 0.5345 0.4478 0.056 Uiso 1 1 calc R . . C11 C 0.1754(4) 0.5575(2) 0.41464(16) 0.0514(9) Uani 1 1 d . . . H11 H 0.1307 0.5339 0.4476 0.062 Uiso 1 1 calc R . . C12 C 0.0876(4) 0.5922(2) 0.36615(15) 0.0490(8) Uani 1 1 d . . . H12 H -0.0183 0.5917 0.3664 0.059 Uiso 1 1 calc R . . C13 C 0.6362(3) 0.55348(15) 0.24129(13) 0.0318(6) Uani 1 1 d . . . C14 C 0.6886(3) 0.38823(15) 0.27974(12) 0.0280(6) Uani 1 1 d . . . C15 C 0.6564(4) 0.41528(16) 0.33844(13) 0.0345(6) Uani 1 1 d . . . H15 H 0.5687 0.4437 0.3406 0.041 Uiso 1 1 calc R . . C16 C 0.7513(4) 0.40105(19) 0.39367(14) 0.0436(8) Uani 1 1 d . . . H16 H 0.7280 0.4198 0.4332 0.052 Uiso 1 1 calc R . . C17 C 0.8786(4) 0.3601(2) 0.39159(16) 0.0506(9) Uani 1 1 d . . . H17 H 0.9429 0.3503 0.4295 0.061 Uiso 1 1 calc R . . C18 C 0.9126(4) 0.3333(2) 0.33411(16) 0.0489(9) Uani 1 1 d . . . H18 H 1.0002 0.3047 0.3326 0.059 Uiso 1 1 calc R . . C19 C 0.8194(3) 0.34775(17) 0.27824(14) 0.0356(7) Uani 1 1 d . . . H19 H 0.8453 0.3299 0.2388 0.043 Uiso 1 1 calc R . . C20 C 0.4126(3) 0.33715(14) 0.20854(12) 0.0256(5) Uani 1 1 d . . . C21 C 0.3716(3) 0.30986(15) 0.26537(14) 0.0306(6) Uani 1 1 d . . . H21 H 0.4271 0.3237 0.3045 0.037 Uiso 1 1 calc R . . C22 C 0.2506(3) 0.26259(16) 0.26583(15) 0.0370(7) Uani 1 1 d . . . H22 H 0.2261 0.2432 0.3050 0.044 Uiso 1 1 calc R . . C23 C 0.1659(4) 0.24376(16) 0.20938(17) 0.0408(7) Uani 1 1 d . . . H23 H 0.0823 0.2121 0.2097 0.049 Uiso 1 1 calc R . . C24 C 0.2036(3) 0.27125(16) 0.15223(16) 0.0386(7) Uani 1 1 d . . . H24 H 0.1450 0.2587 0.1135 0.046 Uiso 1 1 calc R . . C25 C 0.3267(3) 0.31704(15) 0.15141(13) 0.0307(6) Uani 1 1 d . . . H25 H 0.3529 0.3348 0.1120 0.037 Uiso 1 1 calc R . . C26 C 0.6679(3) 0.37595(14) 0.14452(12) 0.0262(5) Uani 1 1 d . . . C27 C 0.7600(3) 0.42659(15) 0.11865(13) 0.0280(6) Uani 1 1 d . . . H27 H 0.7608 0.4756 0.1327 0.034 Uiso 1 1 calc R . . C28 C 0.8501(3) 0.40599(17) 0.07269(13) 0.0325(6) Uani 1 1 d . . . H28 H 0.9121 0.4410 0.0555 0.039 Uiso 1 1 calc R . . C29 C 0.8504(3) 0.33464(17) 0.05172(13) 0.0349(7) Uani 1 1 d . . . H29 H 0.9128 0.3206 0.0204 0.042 Uiso 1 1 calc R . . C30 C 0.7589(3) 0.28391(16) 0.07683(13) 0.0349(6) Uani 1 1 d . . . H30 H 0.7583 0.2350 0.0625 0.042 Uiso 1 1 calc R . . C31 C 0.6684(3) 0.30438(15) 0.12265(13) 0.0300(6) Uani 1 1 d . . . H31 H 0.6060 0.2693 0.1394 0.036 Uiso 1 1 calc R . . C32 C 0.6850(6) 0.6780(2) 0.4922(2) 0.0708(13) Uani 1 1 d . . . H32A H 0.7681 0.7096 0.5109 0.085 Uiso 1 1 calc R . . H32B H 0.6298 0.7045 0.4561 0.085 Uiso 1 1 calc R . . B1 B 0.8281(4) 0.64303(17) 0.06064(14) 0.0289(6) Uani 1 1 d . . . H33 H 0.407(4) 0.5029(18) 0.2634(15) 0.036(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02383(13) 0.02014(13) 0.02289(12) -0.00093(7) 0.00082(8) -0.00001(8) Cl1 0.0597(6) 0.0585(6) 0.0603(6) -0.0012(4) 0.0077(4) 0.0065(4) Cl2 0.1379(13) 0.0883(9) 0.0806(8) -0.0200(7) 0.0637(9) -0.0279(9) P1 0.0253(3) 0.0209(3) 0.0232(3) 0.0005(2) 0.0023(3) 0.0004(3) F1 0.0571(13) 0.0366(10) 0.0647(13) -0.0009(9) -0.0046(10) -0.0158(9) F2 0.0404(10) 0.0480(11) 0.0389(10) -0.0065(8) -0.0064(8) 0.0101(8) F3 0.0445(11) 0.0471(11) 0.0405(10) -0.0059(8) 0.0012(8) 0.0170(8) F4 0.0474(11) 0.0700(14) 0.0366(10) 0.0024(9) 0.0144(8) -0.0068(10) O1 0.0389(13) 0.0388(12) 0.0600(15) -0.0003(11) -0.0187(11) -0.0085(10) N1 0.0280(12) 0.0220(11) 0.0269(11) -0.0008(9) 0.0015(9) 0.0014(9) N2 0.0251(12) 0.0255(12) 0.0281(11) -0.0040(9) 0.0025(9) 0.0001(9) N3 0.0256(12) 0.0306(12) 0.0257(11) 0.0014(9) 0.0030(9) 0.0017(9) N4 0.0405(15) 0.0467(16) 0.0325(13) -0.0016(11) 0.0044(11) 0.0063(12) C1 0.0268(14) 0.0308(14) 0.0287(13) -0.0029(11) 0.0009(11) 0.0060(11) C2 0.0237(14) 0.0322(14) 0.0309(14) -0.0040(11) 0.0041(10) 0.0004(11) C3 0.0277(14) 0.0330(15) 0.0258(13) -0.0054(11) -0.0015(10) 0.0009(11) C4 0.0295(15) 0.0344(14) 0.0245(13) -0.0031(11) 0.0008(11) 0.0022(12) C5 0.0333(15) 0.0298(14) 0.0301(14) 0.0051(11) 0.0025(11) 0.0020(12) C6 0.0316(15) 0.0264(14) 0.0336(14) 0.0029(11) 0.0028(11) 0.0002(11) C7 0.0372(16) 0.0241(14) 0.0314(14) -0.0044(11) 0.0011(12) 0.0027(11) C8 0.0382(16) 0.0256(14) 0.0286(14) -0.0068(11) 0.0007(11) 0.0044(12) C9 0.0429(18) 0.0379(17) 0.0311(15) -0.0043(12) -0.0011(13) 0.0061(13) C10 0.060(2) 0.048(2) 0.0305(16) 0.0016(14) -0.0004(14) 0.0112(16) C11 0.064(2) 0.059(2) 0.0323(16) 0.0037(15) 0.0087(15) -0.0084(18) C12 0.0434(19) 0.071(2) 0.0335(17) 0.0001(16) 0.0075(14) 0.0007(17) C13 0.0371(16) 0.0242(14) 0.0333(14) 0.0024(11) 0.0004(12) 0.0024(12) C14 0.0300(14) 0.0268(14) 0.0267(13) 0.0026(10) 0.0007(11) -0.0001(11) C15 0.0388(17) 0.0350(15) 0.0293(14) 0.0005(11) 0.0017(12) 0.0068(13) C16 0.049(2) 0.053(2) 0.0273(15) -0.0019(13) -0.0017(13) 0.0059(16) C17 0.046(2) 0.066(2) 0.0360(17) 0.0013(16) -0.0113(14) 0.0103(17) C18 0.0355(18) 0.066(2) 0.0435(18) 0.0003(16) -0.0050(14) 0.0200(16) C19 0.0353(16) 0.0397(17) 0.0312(15) -0.0015(12) 0.0009(12) 0.0054(13) C20 0.0268(13) 0.0206(13) 0.0300(13) 0.0003(10) 0.0050(10) 0.0024(10) C21 0.0309(15) 0.0278(14) 0.0336(14) 0.0030(11) 0.0066(11) 0.0032(11) C22 0.0353(16) 0.0309(15) 0.0473(17) 0.0088(13) 0.0151(13) 0.0015(12) C23 0.0304(16) 0.0281(15) 0.065(2) 0.0011(14) 0.0115(14) -0.0020(12) C24 0.0354(17) 0.0304(15) 0.0487(18) -0.0073(13) -0.0005(13) -0.0008(12) C25 0.0344(15) 0.0245(13) 0.0336(14) -0.0018(11) 0.0056(12) -0.0013(11) C26 0.0278(14) 0.0265(13) 0.0239(12) 0.0027(10) 0.0013(10) 0.0020(11) C27 0.0249(14) 0.0268(14) 0.0318(14) 0.0031(11) 0.0011(11) -0.0003(11) C28 0.0251(14) 0.0396(16) 0.0327(14) 0.0070(12) 0.0038(11) 0.0000(12) C29 0.0308(15) 0.0468(18) 0.0279(14) 0.0013(12) 0.0064(11) 0.0094(13) C30 0.0417(17) 0.0314(15) 0.0320(15) -0.0011(12) 0.0065(12) 0.0084(13) C31 0.0367(16) 0.0253(14) 0.0287(14) 0.0015(11) 0.0068(11) 0.0031(11) C32 0.094(3) 0.052(2) 0.072(3) -0.014(2) 0.036(2) -0.016(2) B1 0.0296(16) 0.0294(16) 0.0276(15) -0.0029(12) 0.0027(12) -0.0018(13) _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 Ru1 H33 1.47(3) . ? Ru1 C13 1.837(3) . ? Ru1 N2 2.170(2) . ? Ru1 N1 2.203(2) . ? Ru1 N3 2.221(2) . ? Ru1 P1 2.2615(7) . ? Cl1 C32 1.759(4) . ? Cl2 C32 1.732(4) . ? P1 C26 1.834(3) . ? P1 C20 1.835(3) . ? P1 C14 1.841(3) . ? F1 B1 1.378(4) . ? F2 B1 1.395(4) . ? F3 B1 1.388(4) . ? F4 B1 1.385(4) . ? O1 C13 1.157(4) . ? N1 C6 1.502(3) . ? N1 C7 1.503(3) . ? N1 C1 1.507(3) . ? N2 C2 1.491(3) . ? N2 C3 1.500(3) . ? N3 C4 1.483(3) . ? N3 C5 1.493(3) . ? N4 C8 1.333(4) . ? N4 C12 1.342(4) . ? C1 C2 1.507(4) . ? C3 C4 1.523(4) . ? C5 C6 1.517(4) . ? C7 C8 1.509(4) . ? C8 C9 1.390(4) . ? C9 C10 1.389(5) . ? C10 C11 1.379(5) . ? C11 C12 1.376(5) . ? C14 C19 1.393(4) . ? C14 C15 1.398(4) . ? C15 C16 1.389(4) . ? C16 C17 1.373(5) . ? C17 C18 1.378(5) . ? C18 C19 1.392(4) . ? C20 C21 1.390(4) . ? C20 C25 1.406(4) . ? C21 C22 1.393(4) . ? C22 C23 1.383(5) . ? C23 C24 1.388(5) . ? C24 C25 1.391(4) . ? C26 C31 1.397(4) . ? C26 C27 1.398(4) . ? C27 C28 1.387(4) . ? C28 C29 1.387(4) . ? C29 C30 1.389(4) . ? C30 C31 1.386(4) . ? 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 H33 Ru1 C13 89.9(13) . . ? H33 Ru1 N2 88.5(13) . . ? C13 Ru1 N2 176.17(11) . . ? H33 Ru1 N1 89.0(13) . . ? C13 Ru1 N1 96.86(10) . . ? N2 Ru1 N1 79.65(8) . . ? H33 Ru1 N3 163.9(13) . . ? C13 Ru1 N3 102.38(11) . . ? N2 Ru1 N3 78.62(8) . . ? N1 Ru1 N3 79.37(8) . . ? H33 Ru1 P1 85.5(13) . . ? C13 Ru1 P1 87.86(9) . . ? N2 Ru1 P1 95.46(6) . . ? N1 Ru1 P1 172.70(6) . . ? N3 Ru1 P1 105.12(6) . . ? C26 P1 C20 103.46(12) . . ? C26 P1 C14 101.88(12) . . ? C20 P1 C14 104.26(12) . . ? C26 P1 Ru1 119.05(9) . . ? C20 P1 Ru1 110.97(9) . . ? C14 P1 Ru1 115.52(9) . . ? C6 N1 C7 106.7(2) . . ? C6 N1 C1 110.3(2) . . ? C7 N1 C1 110.8(2) . . ? C6 N1 Ru1 104.23(16) . . ? C7 N1 Ru1 114.25(16) . . ? C1 N1 Ru1 110.34(15) . . ? C2 N2 C3 113.4(2) . . ? C2 N2 Ru1 105.89(15) . . ? C3 N2 Ru1 112.54(16) . . ? C4 N3 C5 113.0(2) . . ? C4 N3 Ru1 105.35(16) . . ? C5 N3 Ru1 111.36(16) . . ? C8 N4 C12 118.1(3) . . ? N1 C1 C2 111.3(2) . . ? N2 C2 C1 109.9(2) . . ? N2 C3 C4 111.9(2) . . ? N3 C4 C3 110.2(2) . . ? N3 C5 C6 110.6(2) . . ? N1 C6 C5 111.4(2) . . ? N1 C7 C8 115.1(2) . . ? N4 C8 C9 122.2(3) . . ? N4 C8 C7 116.9(2) . . ? C9 C8 C7 120.9(3) . . ? C10 C9 C8 119.2(3) . . ? C11 C10 C9 118.3(3) . . ? C12 C11 C10 119.1(3) . . ? N4 C12 C11 123.0(3) . . ? O1 C13 Ru1 178.0(3) . . ? C19 C14 C15 118.1(3) . . ? C19 C14 P1 122.3(2) . . ? C15 C14 P1 119.6(2) . . ? C16 C15 C14 120.7(3) . . ? C17 C16 C15 120.5(3) . . ? C16 C17 C18 119.6(3) . . ? C17 C18 C19 120.6(3) . . ? C18 C19 C14 120.5(3) . . ? C21 C20 C25 118.4(3) . . ? C21 C20 P1 121.4(2) . . ? C25 C20 P1 119.8(2) . . ? C20 C21 C22 121.0(3) . . ? C23 C22 C21 120.1(3) . . ? C22 C23 C24 119.7(3) . . ? C23 C24 C25 120.3(3) . . ? C24 C25 C20 120.4(3) . . ? C31 C26 C27 118.4(3) . . ? C31 C26 P1 123.7(2) . . ? C27 C26 P1 117.8(2) . . ? C28 C27 C26 120.7(3) . . ? C27 C28 C29 120.4(3) . . ? C28 C29 C30 119.5(3) . . ? C31 C30 C29 120.2(3) . . ? C30 C31 C26 120.9(3) . . ? Cl2 C32 Cl1 113.1(2) . . ? F1 B1 F4 110.0(2) . . ? F1 B1 F3 109.3(3) . . ? F4 B1 F3 108.9(2) . . ? F1 B1 F2 109.9(2) . . ? F4 B1 F2 109.4(2) . . ? F3 B1 F2 109.3(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.175 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.075 #===END data_c:\x-rays~1\finish~1\andrew~1\alg3\alg3 _database_code_depnum_ccdc_archive 'CCDC 685069' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'in paper 2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50.50 H56 B Cl5 F4 N4 P2 Ru' _chemical_formula_weight 1146.06 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Ru Ru -1.2594 0.8363 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.3337(4) _cell_length_b 17.2454(5) _cell_length_c 21.8269(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.428(2) _cell_angle_gamma 90.00 _cell_volume 5247.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2348 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8403 _exptl_absorpt_correction_T_max 0.9302 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 ; 'Nonius KappaCCD area detector diffractometer' ; _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28511 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.11 _reflns_number_total 9076 _reflns_number_gt 7505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+23.7411P] 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 SHELXL _refine_ls_extinction_coef 0.0121(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9076 _refine_ls_number_parameters 680 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.1875 _refine_ls_wR_factor_gt 0.1797 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.76153(3) 0.32653(3) -0.00086(2) 0.0304(2) Uani 1 1 d . . . H1 H 0.866(4) 0.321(3) 0.014(3) 0.030(15) Uiso 1 1 d . . . N1 N 0.7848(3) 0.4498(3) -0.0342(2) 0.0303(10) Uani 1 1 d . . . C2 C 0.6925(4) 0.4722(3) -0.0780(3) 0.0369(13) Uani 1 1 d . . . H2A H 0.6861 0.4440 -0.1183 0.044 Uiso 1 1 calc R . . H2B H 0.6937 0.5284 -0.0870 0.044 Uiso 1 1 calc R . . C3 C 0.6061(4) 0.4545(3) -0.0512(3) 0.0378(14) Uani 1 1 d . . . H3A H 0.6004 0.4951 -0.0203 0.045 Uiso 1 1 calc R . . H3B H 0.5475 0.4564 -0.0857 0.045 Uiso 1 1 calc R . . N4 N 0.6119(3) 0.3764(3) -0.0196(3) 0.0369(11) Uani 1 1 d . . . H4 H 0.5693 0.3424 -0.0448 0.044 Uiso 1 1 calc R . . C5 C 0.5897(5) 0.3817(4) 0.0433(3) 0.0445(15) Uani 1 1 d . . . H5A H 0.5807 0.3289 0.0588 0.053 Uiso 1 1 calc R . . H5B H 0.5292 0.4108 0.0398 0.053 Uiso 1 1 calc R . . C6 C 0.6707(5) 0.4224(4) 0.0898(3) 0.0424(15) Uani 1 1 d . . . H6A H 0.6657 0.4791 0.0826 0.051 Uiso 1 1 calc R . . H6B H 0.6644 0.4122 0.1333 0.051 Uiso 1 1 calc R . . N7 N 0.7660(4) 0.3949(3) 0.0828(3) 0.0382(12) Uani 1 1 d . . . H7 H 0.7917 0.3637 0.1174 0.046 Uiso 1 1 calc R . . C8 C 0.8347(5) 0.4593(4) 0.0824(3) 0.0377(13) Uani 1 1 d . . . H8A H 0.9001 0.4382 0.0864 0.045 Uiso 1 1 calc R . . H8B H 0.8358 0.4943 0.1185 0.045 Uiso 1 1 calc R . . C9 C 0.8044(5) 0.5035(3) 0.0218(3) 0.0371(13) Uani 1 1 d . . . H9A H 0.8556 0.5404 0.0180 0.045 Uiso 1 1 calc R . . H9B H 0.7458 0.5336 0.0222 0.045 Uiso 1 1 calc R . . C10 C 0.8653(4) 0.4557(3) -0.0675(3) 0.0338(12) Uani 1 1 d . . . H10A H 0.8597 0.4125 -0.0980 0.041 Uiso 1 1 calc R . . H10B H 0.9270 0.4494 -0.0361 0.041 Uiso 1 1 calc R . . C11 C 0.8672(4) 0.5325(3) -0.1025(3) 0.0359(13) Uani 1 1 d . . . N12 N 0.9095(4) 0.5927(3) -0.0691(3) 0.0406(12) Uani 1 1 d . . . C13 C 0.9099(5) 0.6601(4) -0.0996(3) 0.0455(15) Uani 1 1 d . . . H13 H 0.9392 0.7035 -0.0760 0.055 Uiso 1 1 calc R . . C14 C 0.8712(5) 0.6709(4) -0.1624(3) 0.0454(16) Uani 1 1 d . . . H14 H 0.8737 0.7201 -0.1816 0.055 Uiso 1 1 calc R . . C15 C 0.8284(5) 0.6081(4) -0.1970(3) 0.0513(17) Uani 1 1 d . . . H15 H 0.8006 0.6129 -0.2408 0.062 Uiso 1 1 calc R . . C16 C 0.8268(6) 0.5375(4) -0.1663(3) 0.0518(17) Uani 1 1 d . . . H16 H 0.7982 0.4932 -0.1890 0.062 Uiso 1 1 calc R . . P1 P 0.74687(12) 0.21682(9) 0.05287(8) 0.0371(4) Uani 1 1 d . . . C111 C 0.7694(5) 0.2359(4) 0.1385(3) 0.0472(17) Uani 1 1 d . . . C112 C 0.6951(6) 0.2531(4) 0.1690(3) 0.0511(17) Uani 1 1 d . . . H112 H 0.6303 0.2489 0.1461 0.061 Uiso 1 1 calc R . . C113 C 0.7142(7) 0.2756(4) 0.2309(4) 0.060(2) Uani 1 1 d . . . H113 H 0.6629 0.2857 0.2506 0.072 Uiso 1 1 calc R . . C114 C 0.8096(7) 0.2837(5) 0.2653(4) 0.068(2) Uani 1 1 d . . . H114 H 0.8238 0.2997 0.3082 0.081 Uiso 1 1 calc R . . C115 C 0.8806(6) 0.2682(5) 0.2358(4) 0.064(2) Uani 1 1 d . . . H115 H 0.9452 0.2733 0.2588 0.076 Uiso 1 1 calc R . . C116 C 0.8633(5) 0.2457(4) 0.1742(3) 0.0500(17) Uani 1 1 d . . . H116 H 0.9157 0.2365 0.1554 0.060 Uiso 1 1 calc R . . C121 C 0.6307(5) 0.1664(3) 0.0391(4) 0.0467(17) Uani 1 1 d . . . C122 C 0.5621(5) 0.1814(4) -0.0154(4) 0.0494(18) Uani 1 1 d . . . H122 H 0.5754 0.2178 -0.0449 0.059 Uiso 1 1 calc R . . C123 C 0.4749(6) 0.1442(4) -0.0276(5) 0.071(3) Uani 1 1 d . . . H123 H 0.4271 0.1541 -0.0649 0.085 Uiso 1 1 calc R . . C124 C 0.4592(9) 0.0888(4) 0.0198(7) 0.086(4) Uani 1 1 d . . . H124 H 0.4003 0.0613 0.0126 0.103 Uiso 1 1 calc R . . C125 C 0.5255(8) 0.0756(5) 0.0732(6) 0.073(3) Uani 1 1 d . . . H125 H 0.5129 0.0397 0.1033 0.088 Uiso 1 1 calc R . . C126 C 0.6100(6) 0.1135(4) 0.0840(4) 0.061(2) Uani 1 1 d . . . H126 H 0.6564 0.1046 0.1222 0.073 Uiso 1 1 calc R . . C131 C 0.8327(5) 0.1366(4) 0.0556(3) 0.0423(15) Uani 1 1 d . . . C132 C 0.9264(5) 0.1534(4) 0.0532(3) 0.0445(16) Uani 1 1 d . . . H132 H 0.9430 0.2057 0.0471 0.053 Uiso 1 1 calc R . . C133 C 0.9974(6) 0.0967(4) 0.0594(3) 0.0510(18) Uani 1 1 d . . . H133 H 1.0609 0.1100 0.0572 0.061 Uiso 1 1 calc R . . C134 C 0.9731(6) 0.0205(5) 0.0686(3) 0.058(2) Uani 1 1 d . . . H134 H 1.0205 -0.0189 0.0735 0.070 Uiso 1 1 calc R . . C135 C 0.8815(7) 0.0018(4) 0.0708(4) 0.057(2) Uani 1 1 d . . . H135 H 0.8654 -0.0507 0.0766 0.069 Uiso 1 1 calc R . . C136 C 0.8116(6) 0.0587(4) 0.0646(3) 0.0506(17) Uani 1 1 d . . . H136 H 0.7483 0.0445 0.0665 0.061 Uiso 1 1 calc R . . P2 P 0.77420(10) 0.26128(8) -0.09067(7) 0.0311(3) Uani 1 1 d . . . C211 C 0.7245(4) 0.1622(3) -0.1099(3) 0.0347(13) Uani 1 1 d . . . C212 C 0.7805(5) 0.0966(3) -0.0886(3) 0.0381(13) Uani 1 1 d . . . H212 H 0.8438 0.1032 -0.0637 0.046 Uiso 1 1 calc R . . C213 C 0.7451(5) 0.0224(3) -0.1031(3) 0.0444(15) Uani 1 1 d . . . H213 H 0.7846 -0.0212 -0.0885 0.053 Uiso 1 1 calc R . . C214 C 0.6538(5) 0.0111(4) -0.1383(4) 0.0471(16) Uani 1 1 d . . . H214 H 0.6300 -0.0399 -0.1482 0.057 Uiso 1 1 calc R . . C215 C 0.5963(5) 0.0747(4) -0.1593(4) 0.0522(18) Uani 1 1 d . . . H215 H 0.5326 0.0673 -0.1832 0.063 Uiso 1 1 calc R . . C216 C 0.6313(4) 0.1491(4) -0.1456(3) 0.0429(15) Uani 1 1 d . . . H216 H 0.5913 0.1922 -0.1608 0.051 Uiso 1 1 calc R . . C221 C 0.8957(4) 0.2438(3) -0.1031(3) 0.0359(13) Uani 1 1 d . . . C222 C 0.9115(5) 0.1937(4) -0.1507(3) 0.0437(15) Uani 1 1 d . . . H222 H 0.8582 0.1678 -0.1767 0.052 Uiso 1 1 calc R . . C223 C 1.0018(5) 0.1811(4) -0.1607(3) 0.0479(16) Uani 1 1 d . . . H223 H 1.0099 0.1472 -0.1934 0.058 Uiso 1 1 calc R . . C224 C 1.0811(5) 0.2178(4) -0.1229(3) 0.0441(15) Uani 1 1 d . . . H224 H 1.1435 0.2091 -0.1294 0.053 Uiso 1 1 calc R . . C225 C 1.0676(5) 0.2674(4) -0.0758(3) 0.0398(14) Uani 1 1 d . . . H225 H 1.1211 0.2932 -0.0500 0.048 Uiso 1 1 calc R . . C226 C 0.9771(4) 0.2795(3) -0.0662(3) 0.0328(12) Uani 1 1 d . . . H226 H 0.9697 0.3134 -0.0333 0.039 Uiso 1 1 calc R . . C231 C 0.7181(4) 0.3096(3) -0.1659(3) 0.0365(13) Uani 1 1 d . . . C232 C 0.6207(5) 0.3299(3) -0.1768(3) 0.0466(16) Uani 1 1 d . . . H232 H 0.5854 0.3167 -0.1465 0.056 Uiso 1 1 calc R . . C233 C 0.5753(6) 0.3688(4) -0.2307(4) 0.063(2) Uani 1 1 d . . . H233 H 0.5093 0.3817 -0.2370 0.076 Uiso 1 1 calc R . . C234 C 0.6243(8) 0.3891(4) -0.2754(4) 0.072(3) Uani 1 1 d . . . H234 H 0.5928 0.4166 -0.3122 0.087 Uiso 1 1 calc R . . C235 C 0.7200(7) 0.3692(4) -0.2664(4) 0.063(2) Uani 1 1 d . . . H235 H 0.7539 0.3825 -0.2975 0.076 Uiso 1 1 calc R . . C236 C 0.7672(5) 0.3301(4) -0.2124(3) 0.0467(16) Uani 1 1 d . . . H236 H 0.8330 0.3170 -0.2069 0.056 Uiso 1 1 calc R . . B1 B 0.6474(6) 0.6596(5) 0.0968(4) 0.0487(19) Uani 1 1 d . . . F1 F 0.6188(3) 0.6204(2) 0.0390(2) 0.0577(11) Uani 1 1 d . . . F2 F 0.5664(3) 0.6842(3) 0.1150(3) 0.0762(15) Uani 1 1 d . . . F3 F 0.6991(3) 0.7252(3) 0.0878(2) 0.0669(13) Uani 1 1 d . . . F4 F 0.7056(4) 0.6130(3) 0.1393(3) 0.0828(15) Uani 1 1 d . . . C1S C 0.8795(9) 0.5929(7) 0.2373(7) 0.059(3) Uani 0.50 1 d PDU A 1 H1SA H 0.8343 0.6139 0.1997 0.071 Uiso 0.50 1 calc PR A 1 H1SB H 0.8824 0.6297 0.2725 0.071 Uiso 0.50 1 calc PR A 1 Cl1 Cl 0.9935(4) 0.5842(4) 0.2219(3) 0.0804(15) Uani 0.50 1 d PDU A 1 Cl2 Cl 0.8378(3) 0.5025(2) 0.25703(18) 0.0571(9) Uani 0.50 1 d PDU A 1 C2S C 0.9377(12) 0.6220(10) 0.2287(9) 0.082(5) Uani 0.50 1 d PDU B 2 H2SA H 0.8964 0.6544 0.1958 0.099 Uiso 0.50 1 calc PR B 2 H2SB H 0.8955 0.5927 0.2504 0.099 Uiso 0.50 1 calc PR B 2 Cl3 Cl 1.0022(5) 0.5569(4) 0.1931(4) 0.0879(18) Uani 0.50 1 d PDU B 2 Cl4 Cl 1.0119(3) 0.6812(3) 0.2821(2) 0.0781(12) Uani 0.50 1 d PDU B 2 C3S C 0.3493(9) 0.2614(6) 0.0676(5) 0.098(3) Uani 1 1 d DU . . H3S1 H 0.3187 0.2921 0.0300 0.118 Uiso 0.503(15) 1 calc PR C 3 H3S2 H 0.4037 0.2333 0.0570 0.118 Uiso 0.503(15) 1 calc PR C 3 H3S3 H 0.333(16) 0.267(14) -0.007(11) 0.118 Uiso 0.497(15) 1 d P C 4 H3S4 H 0.291(18) 0.296(16) 0.065(12) 0.118 Uiso 0.497(15) 1 d P C 4 Cl5A Cl 0.3967(5) 0.3257(4) 0.1260(3) 0.084(2) Uani 0.503(15) 1 d PDU C 3 Cl6A Cl 0.2680(15) 0.1935(13) 0.0782(8) 0.071(3) Uani 0.503(15) 1 d PDU C 3 Cl5B Cl 0.4085(4) 0.2678(9) 0.1495(4) 0.124(6) Uani 0.497(15) 1 d PDU C 4 Cl6B Cl 0.2586(15) 0.1876(11) 0.0611(8) 0.061(3) Uani 0.497(15) 1 d PDU C 4 C4S C 0.6761(9) 0.5323(9) 0.2659(8) 0.095(4) Uani 0.50 1 d PDU D 5 H4SA H 0.6825 0.5710 0.2336 0.113 Uiso 0.50 1 calc PR D 5 H4SB H 0.6622 0.5605 0.3023 0.113 Uiso 0.50 1 calc PR D 5 Cl7 Cl 0.7831(5) 0.4814(3) 0.2900(4) 0.116(2) Uani 0.50 1 d PDU D 5 Cl8 Cl 0.5803(5) 0.4691(3) 0.2345(3) 0.0997(19) Uani 0.50 1 d PDU D 5 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 0.0291(3) 0.0235(3) 0.0403(3) 0.00534(19) 0.01140(18) 0.00295(18) N1 0.029(2) 0.025(2) 0.036(3) 0.0047(19) 0.0063(19) 0.0012(18) C2 0.034(3) 0.023(3) 0.050(4) 0.006(3) 0.004(3) 0.000(2) C3 0.033(3) 0.020(3) 0.058(4) 0.005(3) 0.005(3) 0.005(2) N4 0.031(3) 0.024(2) 0.057(3) 0.001(2) 0.011(2) 0.0000(19) C5 0.041(3) 0.029(3) 0.071(5) 0.006(3) 0.026(3) 0.002(3) C6 0.043(4) 0.036(3) 0.054(4) 0.004(3) 0.022(3) 0.007(3) N7 0.038(3) 0.027(2) 0.053(3) 0.006(2) 0.019(2) 0.007(2) C8 0.043(3) 0.032(3) 0.038(3) -0.001(3) 0.011(3) 0.000(3) C9 0.044(3) 0.026(3) 0.040(3) -0.004(2) 0.008(3) 0.001(2) C10 0.035(3) 0.024(3) 0.044(3) 0.002(2) 0.012(2) -0.005(2) C11 0.037(3) 0.027(3) 0.046(3) 0.002(3) 0.015(3) -0.002(2) N12 0.041(3) 0.028(3) 0.052(3) 0.005(2) 0.008(2) -0.004(2) C13 0.047(4) 0.030(3) 0.059(4) 0.002(3) 0.011(3) -0.008(3) C14 0.046(4) 0.032(3) 0.061(4) 0.019(3) 0.019(3) -0.002(3) C15 0.060(4) 0.048(4) 0.043(4) 0.009(3) 0.006(3) -0.010(3) C16 0.069(5) 0.042(4) 0.044(4) 0.003(3) 0.011(3) -0.014(3) P1 0.0402(9) 0.0252(7) 0.0517(10) 0.0079(7) 0.0223(7) 0.0070(6) C111 0.059(4) 0.027(3) 0.064(4) 0.020(3) 0.032(3) 0.011(3) C112 0.066(5) 0.040(4) 0.057(4) 0.014(3) 0.033(4) 0.014(3) C113 0.088(6) 0.044(4) 0.057(5) 0.013(3) 0.037(4) 0.019(4) C114 0.102(7) 0.057(5) 0.045(4) 0.013(4) 0.017(4) 0.031(5) C115 0.065(5) 0.071(5) 0.050(4) 0.013(4) 0.003(4) 0.029(4) C116 0.049(4) 0.047(4) 0.053(4) 0.016(3) 0.010(3) 0.025(3) C121 0.054(4) 0.022(3) 0.075(5) 0.007(3) 0.037(4) 0.003(3) C122 0.043(4) 0.023(3) 0.092(6) -0.004(3) 0.035(4) -0.002(3) C123 0.043(4) 0.040(4) 0.138(8) -0.019(5) 0.037(5) -0.003(3) C124 0.093(7) 0.029(4) 0.169(11) -0.035(5) 0.097(8) -0.029(4) C125 0.082(7) 0.046(5) 0.111(8) -0.003(5) 0.061(6) -0.012(4) C126 0.082(6) 0.029(3) 0.090(6) -0.002(4) 0.058(5) -0.001(3) C131 0.051(4) 0.034(3) 0.049(4) 0.011(3) 0.025(3) 0.011(3) C132 0.048(4) 0.046(4) 0.043(4) 0.014(3) 0.020(3) 0.020(3) C133 0.057(4) 0.058(4) 0.039(4) 0.007(3) 0.012(3) 0.028(3) C134 0.081(6) 0.051(4) 0.045(4) 0.001(3) 0.018(4) 0.037(4) C135 0.089(6) 0.034(4) 0.054(4) 0.008(3) 0.026(4) 0.020(4) C136 0.077(5) 0.028(3) 0.051(4) 0.008(3) 0.025(4) 0.013(3) P2 0.0281(7) 0.0245(7) 0.0411(8) 0.0035(6) 0.0091(6) 0.0002(5) C211 0.034(3) 0.027(3) 0.047(3) 0.002(3) 0.016(2) -0.001(2) C212 0.041(3) 0.028(3) 0.046(3) 0.006(3) 0.011(3) 0.006(2) C213 0.050(4) 0.022(3) 0.067(4) 0.005(3) 0.025(3) 0.006(3) C214 0.047(4) 0.024(3) 0.077(5) -0.001(3) 0.029(3) -0.005(3) C215 0.041(4) 0.034(3) 0.082(5) 0.000(3) 0.015(3) -0.009(3) C216 0.033(3) 0.027(3) 0.069(4) 0.000(3) 0.013(3) 0.003(2) C221 0.038(3) 0.028(3) 0.045(3) 0.006(3) 0.017(3) 0.002(2) C222 0.045(4) 0.040(3) 0.048(4) -0.003(3) 0.015(3) -0.007(3) C223 0.049(4) 0.044(4) 0.054(4) -0.011(3) 0.020(3) -0.003(3) C224 0.034(3) 0.043(4) 0.061(4) 0.000(3) 0.021(3) 0.005(3) C225 0.039(3) 0.034(3) 0.047(4) 0.002(3) 0.012(3) -0.004(3) C226 0.030(3) 0.029(3) 0.041(3) 0.006(2) 0.010(2) -0.002(2) C231 0.042(3) 0.023(3) 0.040(3) -0.001(2) 0.001(3) -0.008(2) C232 0.047(4) 0.024(3) 0.059(4) -0.002(3) -0.007(3) -0.003(3) C233 0.064(5) 0.032(4) 0.073(5) -0.001(4) -0.025(4) -0.001(3) C234 0.101(7) 0.037(4) 0.054(5) 0.008(4) -0.034(5) -0.020(4) C235 0.098(7) 0.042(4) 0.043(4) 0.007(3) 0.003(4) -0.021(4) C236 0.063(4) 0.033(3) 0.042(4) 0.000(3) 0.008(3) -0.013(3) B1 0.040(4) 0.046(4) 0.060(5) -0.016(4) 0.012(3) 0.000(3) F1 0.044(2) 0.051(2) 0.079(3) -0.030(2) 0.017(2) -0.0029(18) F2 0.047(2) 0.091(4) 0.100(4) -0.054(3) 0.035(2) -0.023(2) F3 0.050(2) 0.057(3) 0.100(4) -0.024(2) 0.030(2) -0.021(2) F4 0.100(4) 0.055(3) 0.087(4) -0.008(3) 0.010(3) 0.001(3) C1S 0.078(9) 0.049(7) 0.049(8) 0.002(7) 0.011(7) 0.013(7) Cl1 0.068(3) 0.083(4) 0.088(4) 0.003(3) 0.014(3) -0.001(3) Cl2 0.059(2) 0.058(2) 0.051(2) -0.0006(17) 0.0063(16) -0.0009(17) C2S 0.075(12) 0.057(10) 0.138(16) -0.003(9) 0.071(10) -0.013(8) Cl3 0.064(3) 0.070(4) 0.121(6) -0.008(3) 0.004(3) 0.000(3) Cl4 0.075(3) 0.100(4) 0.062(2) 0.004(2) 0.020(2) 0.002(2) C3S 0.144(10) 0.052(6) 0.102(7) -0.009(5) 0.035(7) -0.027(5) Cl5A 0.122(5) 0.053(4) 0.083(4) -0.005(3) 0.038(3) 0.001(3) Cl6A 0.077(6) 0.062(5) 0.085(9) 0.018(6) 0.041(7) 0.014(3) Cl5B 0.063(3) 0.208(15) 0.103(5) -0.044(7) 0.021(3) -0.007(4) Cl6B 0.076(4) 0.047(4) 0.065(6) 0.014(4) 0.025(4) 0.012(2) C4S 0.182(13) 0.054(10) 0.056(11) 0.000(8) 0.045(11) 0.013(7) Cl7 0.171(6) 0.054(3) 0.139(5) -0.023(3) 0.069(5) 0.002(3) Cl8 0.160(5) 0.043(2) 0.131(4) -0.001(3) 0.107(4) 0.000(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 Ru1 H1 1.46(6) . ? Ru1 N7 2.162(5) . ? Ru1 N4 2.258(5) . ? Ru1 P1 2.2614(16) . ? Ru1 N1 2.296(4) . ? Ru1 P2 2.3037(16) . ? N1 C2 1.492(7) . ? N1 C10 1.503(7) . ? N1 C9 1.506(7) . ? C2 C3 1.519(9) . ? C3 N4 1.507(7) . ? N4 C5 1.481(9) . ? C5 C6 1.525(10) . ? C6 N7 1.489(8) . ? N7 C8 1.486(8) . ? C8 C9 1.501(9) . ? C10 C11 1.533(8) . ? C11 N12 1.332(8) . ? C11 C16 1.381(9) . ? N12 C13 1.341(8) . ? C13 C14 1.365(10) . ? C14 C15 1.381(10) . ? C15 C16 1.393(10) . ? P1 C121 1.840(7) . ? P1 C131 1.842(6) . ? P1 C111 1.850(8) . ? C111 C116 1.401(10) . ? C111 C112 1.413(9) . ? C112 C113 1.372(11) . ? C113 C114 1.406(13) . ? C114 C115 1.352(12) . ? C115 C116 1.364(11) . ? C121 C122 1.381(11) . ? C121 C126 1.419(10) . ? C122 C123 1.375(10) . ? C123 C124 1.463(15) . ? C124 C125 1.341(16) . ? C125 C126 1.348(13) . ? C131 C132 1.388(9) . ? C131 C136 1.402(9) . ? C132 C133 1.394(9) . ? C133 C134 1.387(11) . ? C134 C135 1.363(12) . ? C135 C136 1.386(10) . ? P2 C221 1.848(6) . ? P2 C231 1.850(6) . ? P2 C211 1.861(6) . ? C211 C216 1.399(9) . ? C211 C212 1.403(8) . ? C212 C213 1.387(9) . ? C213 C214 1.368(10) . ? C214 C215 1.385(10) . ? C215 C216 1.385(9) . ? C221 C226 1.397(8) . ? C221 C222 1.410(9) . ? C222 C223 1.379(9) . ? C223 C224 1.393(10) . ? C224 C225 1.385(9) . ? C225 C226 1.378(8) . ? C231 C232 1.404(9) . ? C231 C236 1.410(9) . ? C232 C233 1.380(10) . ? C233 C234 1.373(14) . ? C234 C235 1.384(14) . ? C235 C236 1.389(10) . ? B1 F4 1.358(10) . ? B1 F2 1.379(9) . ? B1 F3 1.391(9) . ? B1 F1 1.405(9) . ? C1S Cl1 1.750(12) . ? C1S Cl2 1.759(12) . ? C2S Cl4 1.718(13) . ? C2S Cl3 1.748(13) . ? C3S Cl6A 1.706(13) . ? C3S Cl5A 1.705(9) . ? C3S Cl5B 1.795(12) . ? C3S Cl6B 1.802(12) . ? C4S Cl7 1.741(13) . ? C4S Cl8 1.762(13) . ? 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 H1 Ru1 N7 91(2) . . ? H1 Ru1 N4 161(2) . . ? N7 Ru1 N4 77.64(19) . . ? H1 Ru1 P1 93(2) . . ? N7 Ru1 P1 90.37(14) . . ? N4 Ru1 P1 102.35(13) . . ? H1 Ru1 N1 85(2) . . ? N7 Ru1 N1 77.58(18) . . ? N4 Ru1 N1 77.99(17) . . ? P1 Ru1 N1 167.64(13) . . ? H1 Ru1 P2 83(2) . . ? N7 Ru1 P2 172.88(14) . . ? N4 Ru1 P2 106.95(14) . . ? P1 Ru1 P2 93.88(6) . . ? N1 Ru1 P2 97.84(12) . . ? C2 N1 C10 109.8(4) . . ? C2 N1 C9 109.3(4) . . ? C10 N1 C9 109.3(4) . . ? C2 N1 Ru1 105.7(3) . . ? C10 N1 Ru1 113.6(3) . . ? C9 N1 Ru1 109.0(3) . . ? N1 C2 C3 112.4(5) . . ? N4 C3 C2 113.2(5) . . ? C5 N4 C3 111.6(5) . . ? C5 N4 Ru1 104.8(4) . . ? C3 N4 Ru1 111.9(3) . . ? N4 C5 C6 110.5(5) . . ? N7 C6 C5 111.1(5) . . ? C8 N7 C6 112.8(5) . . ? C8 N7 Ru1 107.0(4) . . ? C6 N7 Ru1 114.4(4) . . ? N7 C8 C9 109.2(5) . . ? C8 C9 N1 111.4(5) . . ? N1 C10 C11 113.8(5) . . ? N12 C11 C16 122.3(6) . . ? N12 C11 C10 117.4(5) . . ? C16 C11 C10 120.3(5) . . ? C11 N12 C13 117.2(6) . . ? N12 C13 C14 124.7(6) . . ? C13 C14 C15 117.9(6) . . ? C14 C15 C16 118.5(6) . . ? C11 C16 C15 119.4(6) . . ? C121 P1 C131 102.9(3) . . ? C121 P1 C111 100.8(3) . . ? C131 P1 C111 98.2(3) . . ? C121 P1 Ru1 120.0(2) . . ? C131 P1 Ru1 120.2(2) . . ? C111 P1 Ru1 111.0(2) . . ? C116 C111 C112 116.4(7) . . ? C116 C111 P1 120.3(5) . . ? C112 C111 P1 122.7(6) . . ? C113 C112 C111 121.6(8) . . ? C112 C113 C114 120.1(7) . . ? C115 C114 C113 118.1(8) . . ? C114 C115 C116 122.8(8) . . ? C115 C116 C111 121.0(7) . . ? C122 C121 C126 119.6(7) . . ? C122 C121 P1 119.2(5) . . ? C126 C121 P1 121.2(7) . . ? C123 C122 C121 120.9(8) . . ? C122 C123 C124 116.7(10) . . ? C125 C124 C123 122.1(8) . . ? C124 C125 C126 119.7(9) . . ? C125 C126 C121 121.0(10) . . ? C132 C131 C136 116.5(6) . . ? C132 C131 P1 119.2(5) . . ? C136 C131 P1 124.1(5) . . ? C131 C132 C133 122.8(7) . . ? C134 C133 C132 118.4(7) . . ? C135 C134 C133 120.4(6) . . ? C134 C135 C136 120.6(7) . . ? C135 C136 C131 121.2(7) . . ? C221 P2 C231 100.0(3) . . ? C221 P2 C211 98.1(3) . . ? C231 P2 C211 98.5(3) . . ? C221 P2 Ru1 117.9(2) . . ? C231 P2 Ru1 115.5(2) . . ? C211 P2 Ru1 122.6(2) . . ? C216 C211 C212 117.0(5) . . ? C216 C211 P2 122.7(4) . . ? C212 C211 P2 120.4(5) . . ? C213 C212 C211 121.2(6) . . ? C214 C213 C212 120.7(6) . . ? C213 C214 C215 119.4(6) . . ? C214 C215 C216 120.3(7) . . ? C215 C216 C211 121.4(6) . . ? C226 C221 C222 116.1(5) . . ? C226 C221 P2 122.2(5) . . ? C222 C221 P2 121.7(5) . . ? C223 C222 C221 122.1(6) . . ? C222 C223 C224 120.1(6) . . ? C225 C224 C223 119.0(6) . . ? C226 C225 C224 120.4(6) . . ? C225 C226 C221 122.3(6) . . ? C232 C231 C236 117.3(6) . . ? C232 C231 P2 118.3(5) . . ? C236 C231 P2 124.4(5) . . ? C233 C232 C231 121.3(8) . . ? C234 C233 C232 120.9(8) . . ? C233 C234 C235 119.3(7) . . ? C234 C235 C236 120.9(8) . . ? C235 C236 C231 120.4(7) . . ? F4 B1 F2 114.1(7) . . ? F4 B1 F3 108.4(6) . . ? F2 B1 F3 107.6(6) . . ? F4 B1 F1 109.5(6) . . ? F2 B1 F1 108.5(6) . . ? F3 B1 F1 108.6(7) . . ? Cl1 C1S Cl2 110.9(8) . . ? Cl4 C2S Cl3 112.0(10) . . ? Cl6A C3S Cl5A 120.7(9) . . ? Cl6A C3S Cl5B 95.0(8) . . ? Cl5A C3S Cl5B 37.1(4) . . ? Cl6A C3S Cl6B 12.0(10) . . ? Cl5A C3S Cl6B 132.3(10) . . ? Cl5B C3S Cl6B 106.7(8) . . ? Cl7 C4S Cl8 111.0(9) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.822 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.105 #===END data_c:\x-rays~1\finish~1\andrew~1\alg12\alg12 _database_code_depnum_ccdc_archive 'CCDC 685070' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'in paper 4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H110 B2 Cl0 F8 N6 O4 P4 Ru2' _chemical_formula_weight 1863.50 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' P P 0.1023 0.0942 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.88850(10) _cell_length_b 18.62980(10) _cell_length_c 19.9116(2) _cell_angle_alpha 91.74 _cell_angle_beta 111.43 _cell_angle_gamma 108.2990(10) _cell_volume 4814.85(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1932 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8490 _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 ; 'Nonius KappaCCD area detector diffractometer' ; _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 100011 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.46 _reflns_number_total 21956 _reflns_number_gt 17437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+9.1024P] 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 SHELXL _refine_ls_extinction_coef 0.0014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 21956 _refine_ls_number_parameters 1122 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1950 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.84913(2) 0.604937(17) 0.699538(16) 0.02477(10) Uani 1 1 d . . . Ru2 Ru 0.63595(2) 0.911824(16) 0.330463(15) 0.02361(10) Uani 1 1 d . . . P1 P 1.01163(7) 0.62586(6) 0.70293(5) 0.0270(2) Uiso 1 1 d . . . P2 P 0.90233(7) 0.62176(6) 0.82270(5) 0.0266(2) Uani 1 1 d . . . P3 P 0.54687(7) 0.81263(6) 0.23308(5) 0.0261(2) Uani 1 1 d . . . P4 P 0.51418(8) 0.96661(6) 0.29476(5) 0.0272(2) Uani 1 1 d . . . F11 F 0.4877(2) 0.35427(16) 0.52393(16) 0.0469(6) Uani 1 1 d . . . F12 F 0.4507(2) 0.24269(18) 0.45375(19) 0.0583(8) Uani 1 1 d . . . F13 F 0.6071(2) 0.33633(16) 0.48603(19) 0.0547(8) Uani 1 1 d . . . F14 F 0.5655(2) 0.2692(2) 0.57041(19) 0.0593(8) Uani 1 1 d . . . F21 F 1.0491(3) 1.1063(3) 0.3955(2) 0.0824(12) Uani 1 1 d . A . F22A F 0.9332(4) 1.0457(4) 0.2802(3) 0.0572(16) Uani 0.50 1 d PDU A 2 F23A F 1.0974(6) 1.1166(5) 0.2968(5) 0.061(2) Uani 0.50 1 d PDU A 2 F24A F 1.0683(7) 1.0122(5) 0.3519(6) 0.064(3) Uani 0.50 1 d PDU A 2 F22B F 1.0201(14) 1.1214(6) 0.2868(5) 0.133(5) Uani 0.50 1 d PDU A 1 F23B F 1.1543(9) 1.1049(5) 0.3385(9) 0.114(4) Uani 0.50 1 d PDU A 1 F24B F 1.0263(10) 1.0003(5) 0.3149(7) 0.081(3) Uani 0.50 1 d PDU A 1 O1 O 0.6536(3) 0.46567(19) 0.41930(17) 0.0469(8) Uani 1 1 d . . . H1C H 0.6269 0.4194 0.4217 0.056 Uiso 1 1 calc R . . O2 O 1.0020(3) 0.8732(2) 0.3925(2) 0.0516(9) Uani 1 1 d . . . H2C H 1.0209 0.9157 0.3791 0.062 Uiso 1 1 calc R . . O1S O 0.6134(6) 0.7675(6) 0.8184(5) 0.0701(14) Uani 0.50 1 d PD . . O2S O 0.9218(6) 0.8226(4) 0.1229(4) 0.0509(17) Uani 0.50 1 d P B 1 O1W O 0.9355(8) 0.9393(6) 0.0805(6) 0.084(3) Uiso 0.50 1 d P C 2 O2W O 0.5000 0.5000 1.0000 0.085(2) Uani 1 2 d S . . N1 N 0.7586(2) 0.5667(2) 0.57610(18) 0.0303(7) Uani 1 1 d . . . N2 N 0.8212(3) 0.7116(2) 0.66482(19) 0.0322(7) Uani 1 1 d . . . H2 H 0.8830 0.7529 0.6843 0.039 Uiso 1 1 calc R . . N3 N 0.6919(2) 0.5809(2) 0.68819(19) 0.0318(7) Uani 1 1 d . . . H3 H 0.6869 0.5639 0.7306 0.038 Uiso 1 1 calc R . . N4 N 0.7851(2) 0.88519(18) 0.37902(18) 0.0274(6) Uani 1 1 d . . . N5 N 0.6206(2) 0.85970(19) 0.42762(17) 0.0289(7) Uani 1 1 d . . . H5 H 0.5561 0.8217 0.4132 0.035 Uiso 1 1 calc R . . N6 N 0.7339(3) 1.00655(19) 0.41975(18) 0.0302(7) Uani 1 1 d . . . H6 H 0.7152 1.0489 0.4065 0.036 Uiso 1 1 calc R . . C1 C 0.7816(3) 0.6371(2) 0.5425(2) 0.0346(9) Uani 1 1 d . . . H1A H 0.7318 0.6264 0.4910 0.042 Uiso 1 1 calc R . . H1B H 0.8514 0.6502 0.5424 0.042 Uiso 1 1 calc R . . C2 C 0.7761(3) 0.7052(2) 0.5828(2) 0.0338(9) Uani 1 1 d . . . H2A H 0.8132 0.7528 0.5692 0.041 Uiso 1 1 calc R . . H2B H 0.7032 0.7011 0.5664 0.041 Uiso 1 1 calc R . . C3 C 0.7498(3) 0.7229(2) 0.6967(3) 0.0357(9) Uani 1 1 d . . . H3A H 0.7253 0.7644 0.6766 0.043 Uiso 1 1 calc R . . H3B H 0.7865 0.7383 0.7504 0.043 Uiso 1 1 calc R . . C4 C 0.6583(3) 0.6492(3) 0.6792(2) 0.0359(9) Uani 1 1 d . . . H4A H 0.6227 0.6520 0.7121 0.043 Uiso 1 1 calc R . . H4B H 0.6089 0.6433 0.6282 0.043 Uiso 1 1 calc R . . C5 C 0.6247(3) 0.5166(2) 0.6264(2) 0.0348(9) Uani 1 1 d . . . H5A H 0.5515 0.5072 0.6167 0.042 Uiso 1 1 calc R . . H5B H 0.6392 0.4693 0.6393 0.042 Uiso 1 1 calc R . . C6 C 0.6447(3) 0.5362(3) 0.5594(2) 0.0351(9) Uani 1 1 d . . . H6A H 0.6143 0.5752 0.5398 0.042 Uiso 1 1 calc R . . H6B H 0.6109 0.4898 0.5214 0.042 Uiso 1 1 calc R . . C7 C 0.7884(3) 0.5074(2) 0.5462(2) 0.0340(9) Uani 1 1 d . . . H7A H 0.7579 0.4584 0.5610 0.041 Uiso 1 1 calc R . . H7B H 0.8641 0.5222 0.5707 0.041 Uiso 1 1 calc R . . C8 C 0.7593(4) 0.4918(3) 0.4638(2) 0.0418(10) Uani 1 1 d . . . H8A H 0.7931 0.5397 0.4489 0.050 Uiso 1 1 calc R . . H8B H 0.7880 0.4533 0.4540 0.050 Uiso 1 1 calc R . . C9 C 1.0431(4) 0.7189(3) 0.4947(3) 0.0472(12) Uani 1 1 d . . . H9 H 1.0468 0.7376 0.4515 0.057 Uiso 1 1 calc R . . C10 C 1.1285(3) 0.6929(2) 0.7790(2) 0.0324(8) Uani 1 1 d . . . C11 C 1.1562(4) 0.5531(3) 0.7128(3) 0.0439(11) Uani 1 1 d . . . H11 H 1.2045 0.6036 0.7223 0.053 Uiso 1 1 calc R . . C12 C 0.9739(3) 0.4982(2) 0.8486(2) 0.0320(8) Uani 1 1 d . . . H12 H 0.9235 0.4755 0.8007 0.038 Uiso 1 1 calc R . . C13 C 0.9975(3) 0.7802(3) 0.8439(3) 0.0395(10) Uani 1 1 d . . . H13 H 0.9954 0.7707 0.7961 0.047 Uiso 1 1 calc R . . C14 C 0.7487(3) 0.5022(3) 0.8449(2) 0.0345(9) Uani 1 1 d . . . H14 H 0.7820 0.4699 0.8347 0.041 Uiso 1 1 calc R . . C15 C 1.0174(4) 0.4058(3) 0.6859(3) 0.0472(11) Uani 1 1 d . . . H15 H 0.9699 0.3551 0.6773 0.057 Uiso 1 1 calc R . . C16 C 1.1679(4) 0.7712(3) 0.7785(3) 0.0416(10) Uani 1 1 d . . . H16 H 1.1377 0.7915 0.7362 0.050 Uiso 1 1 calc R . . C17 C 1.1756(3) 0.6651(3) 0.8425(2) 0.0393(10) Uani 1 1 d . . . H17 H 1.1507 0.6119 0.8446 0.047 Uiso 1 1 calc R . . C18 C 0.6091(4) 0.5157(3) 0.8717(3) 0.0451(11) Uani 1 1 d . . . H18 H 0.5486 0.4936 0.8807 0.054 Uiso 1 1 calc R . . C19 C 1.0521(4) 0.6484(3) 0.5074(3) 0.0455(11) Uani 1 1 d . . . H19 H 1.0614 0.6183 0.4728 0.055 Uiso 1 1 calc R . . C20 C 0.9854(3) 0.5712(2) 0.8776(2) 0.0296(8) Uani 1 1 d . . . C21 C 1.0607(3) 0.6029(3) 0.9484(2) 0.0356(9) Uani 1 1 d . . . H21 H 1.0700 0.6523 0.9698 0.043 Uiso 1 1 calc R . . C22 C 1.1216(4) 0.5631(3) 0.9875(2) 0.0417(10) Uani 1 1 d . . . H22 H 1.1726 0.5857 1.0352 0.050 Uiso 1 1 calc R . . C23 C 1.0039(4) 0.8092(3) 0.9836(3) 0.0503(12) Uani 1 1 d . . . H23 H 1.0066 0.8192 1.0315 0.060 Uiso 1 1 calc R . . C24 C 1.0382(4) 0.8554(3) 0.8810(3) 0.0514(12) Uani 1 1 d . . . H24 H 1.0642 0.8968 0.8586 0.062 Uiso 1 1 calc R . . C25 C 1.2969(4) 0.7924(3) 0.9008(3) 0.0553(14) Uani 1 1 d . . . H25 H 1.3539 0.8258 0.9417 0.066 Uiso 1 1 calc R . . C26 C 0.6487(4) 0.5946(3) 0.8736(3) 0.0487(12) Uani 1 1 d . . . H26 H 0.6144 0.6264 0.8832 0.058 Uiso 1 1 calc R . . C27 C 0.4881(5) 1.0076(3) 0.0879(3) 0.0530(13) Uani 1 1 d . . . H27 H 0.5334 1.0205 0.0632 0.064 Uiso 1 1 calc R . . C28 C 0.7907(3) 0.5819(2) 0.8480(2) 0.0311(8) Uani 1 1 d . . . C29 C 1.1191(5) 0.4179(3) 0.6968(3) 0.0560(14) Uani 1 1 d . . . H29 H 1.1412 0.3754 0.6955 0.067 Uiso 1 1 calc R . . C30 C 1.1879(4) 0.4913(3) 0.7096(3) 0.0525(13) Uani 1 1 d . . . H30 H 1.2571 0.4995 0.7161 0.063 Uiso 1 1 calc R . . C31 C 1.0542(3) 0.5426(2) 0.7022(2) 0.0334(8) Uani 1 1 d . . . C32 C 0.6915(5) 0.8857(3) 0.0929(3) 0.0528(13) Uani 1 1 d . . . H32 H 0.7509 0.9261 0.0950 0.063 Uiso 1 1 calc R . . C33 C 0.5489(5) 0.7726(3) 0.0276(3) 0.0531(13) Uani 1 1 d . . . H33 H 0.5087 0.7352 -0.0153 0.064 Uiso 1 1 calc R . . C34 C 1.0287(3) 0.7618(3) 0.5441(3) 0.0411(10) Uani 1 1 d . . . H34 H 1.0226 0.8102 0.5353 0.049 Uiso 1 1 calc R . . C35 C 0.6586(4) 0.4702(3) 0.8567(2) 0.0417(10) Uani 1 1 d . . . H35 H 0.6312 0.4163 0.8543 0.050 Uiso 1 1 calc R . . C36 C 0.9852(4) 0.4676(3) 0.6877(2) 0.0372(9) Uani 1 1 d . . . H36 H 0.9152 0.4589 0.6789 0.045 Uiso 1 1 calc R . . C37 C 1.0406(4) 0.8694(3) 0.9500(3) 0.0591(15) Uani 1 1 d . . . H37 H 1.0675 0.9206 0.9748 0.071 Uiso 1 1 calc R . . C38 C 1.0329(3) 0.6637(2) 0.6224(2) 0.0312(8) Uani 1 1 d . . . C39 C 0.3862(5) 0.9993(4) 0.0520(3) 0.0639(17) Uani 1 1 d . . . H39 H 0.3611 1.0065 0.0024 0.077 Uiso 1 1 calc R . . C40 C 0.9598(3) 0.7186(2) 0.8767(2) 0.0344(9) Uani 1 1 d . . . C41 C 1.0473(3) 0.6215(3) 0.5716(2) 0.0370(9) Uani 1 1 d . . . H41 H 1.0542 0.5732 0.5802 0.044 Uiso 1 1 calc R . . C42 C 0.7385(3) 0.6271(3) 0.8613(3) 0.0400(10) Uani 1 1 d . . . H42 H 0.7642 0.6808 0.8622 0.048 Uiso 1 1 calc R . . C43 C 1.0231(3) 0.7347(2) 0.6073(2) 0.0347(9) Uani 1 1 d . . . H43 H 1.0123 0.7648 0.6410 0.042 Uiso 1 1 calc R . . C44 C 1.0341(4) 0.4577(3) 0.8877(2) 0.0385(9) Uani 1 1 d . . . H44 H 1.0245 0.4079 0.8668 0.046 Uiso 1 1 calc R . . C45 C 0.7221(3) 0.9925(2) 0.4902(2) 0.0351(9) Uani 1 1 d . . . H45A H 0.7159 1.0382 0.5122 0.042 Uiso 1 1 calc R . . H45B H 0.7842 0.9845 0.5248 0.042 Uiso 1 1 calc R . . C46 C 0.6285(3) 0.9235(3) 0.4786(2) 0.0349(9) Uani 1 1 d . . . H46A H 0.6332 0.9068 0.5261 0.042 Uiso 1 1 calc R . . H46B H 0.5659 0.9373 0.4582 0.042 Uiso 1 1 calc R . . C47 C 0.7027(3) 0.8261(2) 0.4630(2) 0.0326(8) Uani 1 1 d . . . H47A H 0.6702 0.7749 0.4733 0.039 Uiso 1 1 calc R . . H47B H 0.7518 0.8590 0.5104 0.039 Uiso 1 1 calc R . . C48 C 0.7619(3) 0.8182(2) 0.4170(2) 0.0312(8) Uani 1 1 d . . . H48A H 0.8273 0.8126 0.4489 0.037 Uiso 1 1 calc R . . H48B H 0.7211 0.7711 0.3801 0.037 Uiso 1 1 calc R . . C49 C 0.8408(3) 1.0244(2) 0.4255(2) 0.0327(8) Uani 1 1 d . . . H49A H 0.8887 1.0650 0.4680 0.039 Uiso 1 1 calc R . . H49B H 0.8470 1.0432 0.3809 0.039 Uiso 1 1 calc R . . C50 C 0.8688(3) 0.9529(2) 0.4345(2) 0.0319(8) Uani 1 1 d . . . H50A H 0.8791 0.9415 0.4845 0.038 Uiso 1 1 calc R . . H50B H 0.9343 0.9618 0.4284 0.038 Uiso 1 1 calc R . . C51 C 0.8201(3) 0.8657(2) 0.3216(2) 0.0327(8) Uani 1 1 d . . . H51A H 0.8465 0.9135 0.3035 0.039 Uiso 1 1 calc R . . H51B H 0.7588 0.8310 0.2801 0.039 Uiso 1 1 calc R . . C52 C 0.9025(3) 0.8284(3) 0.3423(3) 0.0412(10) Uani 1 1 d . . . H52A H 0.8779 0.7819 0.3628 0.049 Uiso 1 1 calc R . . H52B H 0.9079 0.8113 0.2969 0.049 Uiso 1 1 calc R . . C53 C 0.5684(3) 0.7212(2) 0.2540(2) 0.0280(8) Uani 1 1 d . . . C54 C 0.6135(3) 0.6855(2) 0.2199(2) 0.0328(8) Uani 1 1 d . . . H54 H 0.6291 0.7054 0.1805 0.039 Uiso 1 1 calc R . . C55 C 0.6362(3) 0.6209(3) 0.2428(3) 0.0376(9) Uani 1 1 d . . . H55 H 0.6680 0.5978 0.2193 0.045 Uiso 1 1 calc R . . C56 C 0.6129(4) 0.5902(3) 0.2992(3) 0.0404(10) Uani 1 1 d . . . H56 H 0.6275 0.5458 0.3141 0.048 Uiso 1 1 calc R . . C57 C 0.5681(3) 0.6250(2) 0.3337(2) 0.0342(9) Uani 1 1 d . . . H57 H 0.5522 0.6045 0.3728 0.041 Uiso 1 1 calc R . . C58 C 0.5464(3) 0.6896(2) 0.3116(2) 0.0296(8) Uani 1 1 d . . . H58 H 0.5160 0.7130 0.3360 0.036 Uiso 1 1 calc R . . C59 C 0.5784(3) 0.8219(2) 0.1511(2) 0.0335(9) Uani 1 1 d . . . C60 C 0.6634(4) 0.8815(3) 0.1520(3) 0.0393(10) Uani 1 1 d . . . H60 H 0.7029 0.9202 0.1940 0.047 Uiso 1 1 calc R . . C61 C 0.9634(4) 0.7346(3) 0.9469(2) 0.0392(10) Uani 1 1 d . . . H61 H 0.9377 0.6936 0.9698 0.047 Uiso 1 1 calc R . . C62 C 0.6321(5) 0.8300(4) 0.0299(3) 0.0608(15) Uani 1 1 d . . . H62 H 0.6506 0.8329 -0.0111 0.073 Uiso 1 1 calc R . . C63 C 1.1086(4) 0.4904(3) 0.9576(3) 0.0423(10) Uani 1 1 d . . . H63 H 1.1503 0.4632 0.9848 0.051 Uiso 1 1 calc R . . C64 C 0.5205(4) 0.7671(3) 0.0876(2) 0.0415(10) Uani 1 1 d . . . H64 H 0.4616 0.7260 0.0851 0.050 Uiso 1 1 calc R . . C65 C 0.4033(3) 0.7766(2) 0.1874(2) 0.0305(8) Uani 1 1 d . . . C66 C 0.3423(3) 0.7246(3) 0.2162(2) 0.0371(9) Uani 1 1 d . . . H66 H 0.3742 0.7043 0.2580 0.045 Uiso 1 1 calc R . . C67 C 0.2353(4) 0.7020(3) 0.1844(3) 0.0435(10) Uani 1 1 d . . . H67 H 0.1950 0.6674 0.2052 0.052 Uiso 1 1 calc R . . C68 C 0.1875(4) 0.7297(3) 0.1226(3) 0.0466(11) Uani 1 1 d . . . H68 H 0.1145 0.7143 0.1011 0.056 Uiso 1 1 calc R . . C69 C 0.2462(4) 0.7797(3) 0.0925(3) 0.0453(11) Uani 1 1 d . . . H69 H 0.2137 0.7984 0.0498 0.054 Uiso 1 1 calc R . . C70 C 0.3537(3) 0.8030(3) 0.1246(2) 0.0371(9) Uani 1 1 d . . . H70 H 0.3934 0.8374 0.1034 0.044 Uiso 1 1 calc R . . C71 C 0.4601(3) 0.9791(2) 0.1982(2) 0.0334(9) Uani 1 1 d . . . C72 C 0.5247(4) 0.9968(2) 0.1610(2) 0.0379(9) Uani 1 1 d . . . H72 H 0.5949 1.0018 0.1854 0.045 Uiso 1 1 calc R . . C73 C 1.2583(4) 0.7146(3) 0.9023(3) 0.0515(12) Uani 1 1 d . . . H73 H 1.2889 0.6948 0.9448 0.062 Uiso 1 1 calc R . . C74 C 1.2511(4) 0.8206(3) 0.8388(3) 0.0503(12) Uani 1 1 d . . . H74 H 1.2763 0.8738 0.8373 0.060 Uiso 1 1 calc R . . C75 C 0.3212(5) 0.9807(4) 0.0874(3) 0.0616(16) Uani 1 1 d . . . H75 H 0.2506 0.9741 0.0618 0.074 Uiso 1 1 calc R . . C76 C 0.3564(4) 0.9711(3) 0.1602(3) 0.0452(11) Uani 1 1 d . . . H76 H 0.3103 0.9592 0.1843 0.054 Uiso 1 1 calc R . . C77 C 0.3983(3) 0.9329(2) 0.3161(2) 0.0326(8) Uani 1 1 d . . . C78 C 0.3714(3) 0.8611(2) 0.3351(2) 0.0338(9) Uani 1 1 d . . . H78 H 0.4130 0.8308 0.3375 0.041 Uiso 1 1 calc R . . C79 C 0.2839(3) 0.8319(3) 0.3509(3) 0.0440(11) Uani 1 1 d . . . H79 H 0.2662 0.7822 0.3638 0.053 Uiso 1 1 calc R . . C80 C 0.2232(4) 0.8762(3) 0.3477(3) 0.0487(12) Uani 1 1 d . . . H80 H 0.1635 0.8566 0.3581 0.058 Uiso 1 1 calc R . . C81 C 0.2497(4) 0.9486(3) 0.3295(3) 0.0474(12) Uani 1 1 d . . . H81 H 0.2081 0.9787 0.3276 0.057 Uiso 1 1 calc R . . C82 C 0.3374(3) 0.9779(3) 0.3137(3) 0.0401(10) Uani 1 1 d . . . H82 H 0.3555 1.0279 0.3015 0.048 Uiso 1 1 calc R . . C83 C 0.5699(3) 1.0680(2) 0.3393(2) 0.0318(8) Uani 1 1 d . . . C84 C 0.5621(4) 1.0905(3) 0.4036(2) 0.0378(9) Uani 1 1 d . . . H84 H 0.5197 1.0540 0.4217 0.045 Uiso 1 1 calc R . . C85 C 0.6144(4) 1.1648(3) 0.4421(3) 0.0490(12) Uani 1 1 d . . . H85 H 0.6065 1.1791 0.4852 0.059 Uiso 1 1 calc R . . C86 C 0.6785(4) 1.2180(3) 0.4168(3) 0.0528(13) Uani 1 1 d . . . H86 H 0.7150 1.2688 0.4431 0.063 Uiso 1 1 calc R . . C87 C 0.6893(4) 1.1972(3) 0.3534(3) 0.0458(11) Uani 1 1 d . . . H87 H 0.7333 1.2337 0.3364 0.055 Uiso 1 1 calc R . . C88 C 0.6357(3) 1.1231(2) 0.3149(3) 0.0378(9) Uani 1 1 d . . . H88 H 0.6434 1.1092 0.2715 0.045 Uiso 1 1 calc R . . C1S C 0.4515(10) 0.7163(8) 0.8073(8) 0.0701(14) Uani 0.50 1 d PD . . H1S1 H 0.4998 0.7192 0.8573 0.105 Uiso 0.50 1 calc PR . . H1S2 H 0.4083 0.6627 0.7864 0.105 Uiso 0.50 1 calc PR . . H1S3 H 0.4079 0.7460 0.8080 0.105 Uiso 0.50 1 calc PR . . C2S C 0.5079(8) 0.7470(8) 0.7637(7) 0.0701(14) Uani 0.50 1 d PD . . H2S1 H 0.4935 0.7925 0.7447 0.084 Uiso 0.50 1 calc PR . . H2S2 H 0.4933 0.7082 0.7224 0.084 Uiso 0.50 1 calc PR . . C3S C 0.6725(9) 0.8289(7) 0.8309(8) 0.0701(14) Uani 0.50 1 d PD . . H3S1 H 0.6408 0.8622 0.8463 0.084 Uiso 0.50 1 calc PR . . H3S2 H 0.6727 0.8411 0.7829 0.084 Uiso 0.50 1 calc PR . . C4S C 0.7766(9) 0.8570(8) 0.8795(8) 0.0701(14) Uani 0.50 1 d PD . . H4S1 H 0.7813 0.8637 0.9299 0.105 Uiso 0.50 1 calc PR . . H4S2 H 0.8115 0.9065 0.8686 0.105 Uiso 0.50 1 calc PR . . H4S3 H 0.8096 0.8205 0.8741 0.105 Uiso 0.50 1 calc PR . . C5S C 0.7990(10) 0.6971(7) 0.0682(9) 0.080(4) Uani 0.50 1 d P B 1 H5S1 H 0.7730 0.7216 0.0260 0.121 Uiso 0.50 1 calc PR B 1 H5S2 H 0.7411 0.6580 0.0734 0.121 Uiso 0.50 1 calc PR B 1 H5S3 H 0.8452 0.6730 0.0608 0.121 Uiso 0.50 1 calc PR B 1 C6S C 0.8585(13) 0.7581(7) 0.1382(6) 0.071(4) Uani 0.50 1 d P B 1 H6S1 H 0.8095 0.7720 0.1540 0.086 Uiso 0.50 1 calc PR B 1 H6S2 H 0.9007 0.7374 0.1781 0.086 Uiso 0.50 1 calc PR B 1 C7S C 0.9787(10) 0.8876(7) 0.1776(6) 0.061(3) Uani 0.50 1 d P B 1 H7S1 H 1.0289 0.8748 0.2195 0.073 Uiso 0.50 1 calc PR B 1 H7S2 H 0.9314 0.9020 0.1950 0.073 Uiso 0.50 1 calc PR B 1 C8S C 1.0352(10) 0.9546(7) 0.1511(7) 0.065(3) Uani 0.50 1 d P B 1 H8S1 H 1.0985 0.9486 0.1514 0.097 Uiso 0.50 1 calc PR B 1 H8S2 H 1.0528 1.0020 0.1834 0.097 Uiso 0.50 1 calc PR B 1 H8S3 H 0.9914 0.9568 0.1012 0.097 Uiso 0.50 1 calc PR B 1 B1 B 0.5288(4) 0.3009(3) 0.5090(3) 0.0395(11) Uani 1 1 d . . . B2 B 1.0430(5) 1.0744(3) 0.3301(3) 0.0508(14) Uani 1 1 d D . . H1 H 0.841(4) 0.517(3) 0.715(3) 0.047(14) Uiso 1 1 d . . . H2D H 0.673(4) 0.956(3) 0.274(3) 0.046(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02347(16) 0.02640(16) 0.02250(16) 0.00748(11) 0.00676(12) 0.00862(12) Ru2 0.02410(16) 0.02387(16) 0.02228(16) 0.00632(11) 0.00730(12) 0.00960(12) P2 0.0268(5) 0.0284(5) 0.0239(5) 0.0057(4) 0.0081(4) 0.0108(4) P3 0.0278(5) 0.0269(5) 0.0238(5) 0.0054(4) 0.0086(4) 0.0115(4) P4 0.0288(5) 0.0285(5) 0.0246(5) 0.0052(4) 0.0075(4) 0.0138(4) F11 0.0475(15) 0.0443(15) 0.0517(16) 0.0038(12) 0.0153(13) 0.0253(13) F12 0.0518(17) 0.0483(17) 0.069(2) -0.0034(15) 0.0235(15) 0.0110(14) F13 0.0608(18) 0.0400(15) 0.077(2) 0.0146(14) 0.0459(17) 0.0121(14) F14 0.0547(18) 0.067(2) 0.068(2) 0.0350(17) 0.0262(16) 0.0320(16) F21 0.069(2) 0.099(3) 0.068(2) -0.019(2) 0.0302(19) 0.015(2) F22A 0.037(3) 0.064(4) 0.045(3) 0.017(3) -0.003(2) 0.006(3) F23A 0.050(4) 0.055(4) 0.067(5) 0.032(4) 0.022(4) 0.004(4) F24A 0.052(5) 0.042(5) 0.101(8) 0.020(5) 0.027(4) 0.022(4) F22B 0.222(15) 0.067(6) 0.070(6) 0.025(5) 0.009(8) 0.054(8) F23B 0.114(9) 0.060(5) 0.195(13) 0.005(7) 0.111(9) 0.007(6) F24B 0.101(9) 0.031(4) 0.118(10) 0.002(5) 0.069(7) 0.002(5) O1 0.0497(19) 0.0412(17) 0.0289(15) 0.0061(13) 0.0018(14) 0.0049(15) O2 0.0359(17) 0.061(2) 0.058(2) 0.0093(18) 0.0136(16) 0.0227(16) O1S 0.063(3) 0.086(4) 0.081(4) 0.029(3) 0.025(3) 0.053(3) O2S 0.058(4) 0.057(4) 0.042(4) -0.004(3) 0.024(3) 0.022(4) O2W 0.123(6) 0.066(4) 0.096(5) 0.019(4) 0.079(5) 0.032(4) N1 0.0252(15) 0.0331(17) 0.0264(16) 0.0093(13) 0.0061(13) 0.0065(13) N2 0.0276(16) 0.0326(17) 0.0329(18) 0.0092(14) 0.0074(14) 0.0110(14) N3 0.0271(16) 0.0373(18) 0.0301(17) 0.0116(14) 0.0106(13) 0.0104(14) N4 0.0233(15) 0.0241(15) 0.0322(17) 0.0063(13) 0.0084(13) 0.0077(12) N5 0.0256(15) 0.0330(17) 0.0257(16) 0.0086(13) 0.0064(13) 0.0112(13) N6 0.0298(16) 0.0279(16) 0.0271(16) 0.0040(13) 0.0048(13) 0.0102(13) C1 0.0298(19) 0.037(2) 0.0273(19) 0.0147(16) 0.0061(16) 0.0048(17) C2 0.0278(19) 0.035(2) 0.034(2) 0.0181(17) 0.0064(16) 0.0105(16) C3 0.033(2) 0.036(2) 0.041(2) 0.0124(18) 0.0126(18) 0.0177(18) C4 0.0269(19) 0.042(2) 0.040(2) 0.0129(18) 0.0122(17) 0.0133(17) C5 0.0284(19) 0.036(2) 0.035(2) 0.0127(17) 0.0091(16) 0.0073(17) C6 0.0263(19) 0.037(2) 0.032(2) 0.0101(17) 0.0058(16) 0.0039(17) C7 0.034(2) 0.035(2) 0.0263(19) 0.0043(16) 0.0081(16) 0.0079(17) C8 0.048(3) 0.041(2) 0.028(2) 0.0041(18) 0.0126(19) 0.007(2) C9 0.046(3) 0.060(3) 0.035(2) 0.022(2) 0.018(2) 0.014(2) C10 0.0256(18) 0.041(2) 0.0295(19) 0.0056(16) 0.0113(16) 0.0097(17) C11 0.043(2) 0.054(3) 0.044(3) 0.013(2) 0.018(2) 0.027(2) C12 0.034(2) 0.036(2) 0.0272(19) 0.0086(16) 0.0110(16) 0.0139(17) C13 0.039(2) 0.034(2) 0.043(2) 0.0042(18) 0.0140(19) 0.0117(18) C14 0.035(2) 0.041(2) 0.0280(19) 0.0092(17) 0.0113(16) 0.0140(18) C15 0.065(3) 0.038(2) 0.039(2) 0.0048(19) 0.016(2) 0.026(2) C16 0.037(2) 0.043(2) 0.035(2) 0.0041(19) 0.0109(18) 0.0054(19) C17 0.028(2) 0.050(3) 0.033(2) 0.0082(19) 0.0076(17) 0.0090(19) C18 0.035(2) 0.063(3) 0.037(2) 0.009(2) 0.0188(19) 0.012(2) C19 0.052(3) 0.056(3) 0.033(2) 0.012(2) 0.021(2) 0.018(2) C20 0.0289(18) 0.035(2) 0.0259(18) 0.0083(15) 0.0099(15) 0.0133(16) C21 0.034(2) 0.042(2) 0.028(2) 0.0050(17) 0.0076(17) 0.0162(18) C22 0.040(2) 0.055(3) 0.025(2) 0.0065(19) 0.0035(17) 0.023(2) C23 0.059(3) 0.051(3) 0.036(2) -0.003(2) 0.011(2) 0.023(2) C24 0.048(3) 0.034(2) 0.058(3) -0.001(2) 0.012(2) 0.006(2) C25 0.038(3) 0.063(3) 0.039(3) 0.003(2) 0.006(2) -0.003(2) C26 0.040(2) 0.066(3) 0.046(3) 0.006(2) 0.021(2) 0.022(2) C27 0.071(4) 0.053(3) 0.031(2) 0.017(2) 0.015(2) 0.021(3) C28 0.033(2) 0.039(2) 0.0224(18) 0.0091(15) 0.0102(15) 0.0144(17) C29 0.070(4) 0.061(3) 0.046(3) 0.003(2) 0.012(3) 0.047(3) C30 0.051(3) 0.066(3) 0.054(3) 0.012(3) 0.020(2) 0.039(3) C31 0.040(2) 0.038(2) 0.029(2) 0.0094(16) 0.0142(17) 0.0205(18) C32 0.064(3) 0.063(3) 0.049(3) 0.026(3) 0.035(3) 0.029(3) C33 0.078(4) 0.064(3) 0.028(2) 0.009(2) 0.022(2) 0.037(3) C34 0.033(2) 0.041(2) 0.041(2) 0.0185(19) 0.0100(18) 0.0066(18) C35 0.037(2) 0.047(3) 0.034(2) 0.0104(19) 0.0131(18) 0.008(2) C36 0.046(2) 0.043(2) 0.027(2) 0.0082(17) 0.0141(18) 0.021(2) C37 0.057(3) 0.044(3) 0.059(3) -0.015(2) 0.004(3) 0.019(2) C38 0.0248(18) 0.036(2) 0.031(2) 0.0089(16) 0.0101(15) 0.0093(16) C39 0.087(4) 0.065(4) 0.027(2) 0.012(2) 0.001(3) 0.036(3) C40 0.031(2) 0.035(2) 0.034(2) 0.0008(17) 0.0064(16) 0.0139(17) C41 0.038(2) 0.041(2) 0.033(2) 0.0102(18) 0.0146(18) 0.0137(19) C42 0.038(2) 0.048(3) 0.040(2) 0.0091(19) 0.0181(19) 0.020(2) C43 0.0266(19) 0.036(2) 0.035(2) 0.0081(17) 0.0074(16) 0.0080(17) C44 0.044(2) 0.041(2) 0.037(2) 0.0111(18) 0.0160(19) 0.022(2) C45 0.036(2) 0.036(2) 0.0259(19) 0.0010(16) 0.0064(16) 0.0101(18) C46 0.037(2) 0.044(2) 0.0249(19) 0.0063(17) 0.0106(16) 0.0177(19) C47 0.0297(19) 0.036(2) 0.032(2) 0.0160(17) 0.0096(16) 0.0129(17) C48 0.0270(18) 0.0281(19) 0.035(2) 0.0129(16) 0.0075(16) 0.0105(15) C49 0.0284(19) 0.0255(18) 0.035(2) 0.0054(15) 0.0059(16) 0.0056(15) C50 0.0238(18) 0.0286(19) 0.034(2) 0.0030(16) 0.0048(15) 0.0052(15) C51 0.0286(19) 0.032(2) 0.039(2) 0.0080(17) 0.0141(17) 0.0115(16) C52 0.032(2) 0.044(2) 0.054(3) 0.013(2) 0.019(2) 0.0192(19) C53 0.0279(18) 0.0250(18) 0.0282(18) 0.0047(14) 0.0073(15) 0.0099(15) C54 0.032(2) 0.034(2) 0.033(2) 0.0062(16) 0.0114(16) 0.0147(17) C55 0.039(2) 0.037(2) 0.041(2) 0.0059(18) 0.0152(19) 0.0206(19) C56 0.045(2) 0.030(2) 0.046(3) 0.0125(18) 0.013(2) 0.0180(19) C57 0.030(2) 0.030(2) 0.035(2) 0.0084(16) 0.0095(17) 0.0055(16) C58 0.0266(18) 0.0303(19) 0.0276(19) 0.0037(15) 0.0082(15) 0.0074(15) C59 0.042(2) 0.039(2) 0.0252(19) 0.0106(16) 0.0132(17) 0.0210(19) C60 0.048(3) 0.045(2) 0.035(2) 0.0164(19) 0.020(2) 0.025(2) C61 0.040(2) 0.046(2) 0.032(2) 0.0025(18) 0.0106(18) 0.019(2) C62 0.086(4) 0.080(4) 0.042(3) 0.024(3) 0.041(3) 0.044(4) C63 0.044(2) 0.052(3) 0.036(2) 0.016(2) 0.0105(19) 0.029(2) C64 0.051(3) 0.047(3) 0.030(2) 0.0054(19) 0.015(2) 0.024(2) C65 0.0291(19) 0.0296(19) 0.0289(19) -0.0005(15) 0.0057(15) 0.0126(16) C66 0.033(2) 0.037(2) 0.036(2) 0.0052(17) 0.0094(17) 0.0104(18) C67 0.035(2) 0.042(2) 0.047(3) 0.000(2) 0.013(2) 0.0092(19) C68 0.030(2) 0.047(3) 0.049(3) -0.008(2) 0.0032(19) 0.011(2) C69 0.040(2) 0.046(3) 0.038(2) 0.000(2) -0.0003(19) 0.019(2) C70 0.036(2) 0.035(2) 0.036(2) 0.0036(17) 0.0089(18) 0.0139(18) C71 0.042(2) 0.0291(19) 0.0279(19) 0.0050(15) 0.0064(17) 0.0188(17) C72 0.046(2) 0.036(2) 0.027(2) 0.0087(16) 0.0093(18) 0.0136(19) C73 0.036(2) 0.066(3) 0.036(2) 0.010(2) 0.004(2) 0.009(2) C74 0.043(3) 0.047(3) 0.045(3) 0.001(2) 0.013(2) 0.000(2) C75 0.065(4) 0.073(4) 0.040(3) 0.002(3) -0.004(3) 0.046(3) C76 0.047(3) 0.051(3) 0.034(2) 0.003(2) 0.0020(19) 0.031(2) C77 0.0287(19) 0.041(2) 0.0267(19) 0.0018(16) 0.0079(15) 0.0142(17) C78 0.0296(19) 0.039(2) 0.0286(19) 0.0026(16) 0.0080(16) 0.0110(17) C79 0.035(2) 0.050(3) 0.039(2) 0.004(2) 0.0116(19) 0.007(2) C80 0.034(2) 0.067(3) 0.041(3) -0.002(2) 0.015(2) 0.013(2) C81 0.035(2) 0.067(3) 0.043(3) -0.005(2) 0.012(2) 0.025(2) C82 0.035(2) 0.045(2) 0.041(2) 0.0036(19) 0.0112(19) 0.020(2) C83 0.0311(19) 0.033(2) 0.0300(19) 0.0040(16) 0.0053(16) 0.0173(17) C84 0.041(2) 0.039(2) 0.035(2) 0.0021(18) 0.0118(18) 0.0207(19) C85 0.046(3) 0.049(3) 0.049(3) -0.008(2) 0.010(2) 0.025(2) C86 0.043(3) 0.040(3) 0.063(3) -0.009(2) 0.006(2) 0.017(2) C87 0.042(2) 0.033(2) 0.060(3) 0.001(2) 0.017(2) 0.014(2) C88 0.037(2) 0.034(2) 0.041(2) 0.0036(18) 0.0124(18) 0.0159(18) C1S 0.063(3) 0.086(4) 0.081(4) 0.029(3) 0.025(3) 0.053(3) C2S 0.063(3) 0.086(4) 0.081(4) 0.029(3) 0.025(3) 0.053(3) C3S 0.063(3) 0.086(4) 0.081(4) 0.029(3) 0.025(3) 0.053(3) C4S 0.063(3) 0.086(4) 0.081(4) 0.029(3) 0.025(3) 0.053(3) C5S 0.060(7) 0.046(6) 0.114(12) -0.035(7) 0.022(7) 0.009(6) C6S 0.120(11) 0.066(8) 0.044(6) 0.003(5) 0.048(7) 0.036(8) C7S 0.074(8) 0.067(7) 0.039(5) -0.002(5) 0.021(5) 0.024(6) C8S 0.073(8) 0.060(7) 0.054(7) -0.002(5) 0.026(6) 0.013(6) B1 0.043(3) 0.034(2) 0.050(3) 0.013(2) 0.025(2) 0.016(2) B2 0.072(4) 0.037(3) 0.051(3) 0.013(2) 0.029(3) 0.023(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 Ru1 H1 1.66(5) . ? Ru1 N3 2.164(3) . ? Ru1 N2 2.235(3) . ? Ru1 P2 2.2622(10) . ? Ru1 N1 2.288(3) . ? Ru1 P1 2.3014(10) . ? Ru2 H2D 1.56(5) . ? Ru2 N6 2.168(3) . ? Ru2 N5 2.244(3) . ? Ru2 P4 2.2579(10) . ? Ru2 N4 2.294(3) . ? Ru2 P3 2.3018(10) . ? P1 C31 1.853(4) . ? P1 C38 1.863(4) . ? P1 C10 1.864(4) . ? P2 C40 1.840(4) . ? P2 C20 1.849(4) . ? P2 C28 1.852(4) . ? P3 C59 1.855(4) . ? P3 C53 1.862(4) . ? P3 C65 1.867(4) . ? P4 C71 1.848(4) . ? P4 C83 1.849(4) . ? P4 C77 1.850(4) . ? F11 B1 1.396(6) . ? F12 B1 1.392(6) . ? F13 B1 1.389(6) . ? F14 B1 1.378(6) . ? F21 B2 1.374(7) . ? F22A B2 1.476(8) . ? F23A B2 1.318(8) . ? F24A B2 1.364(10) . ? F22B B2 1.283(9) . ? F23B B2 1.515(11) . ? F24B B2 1.328(10) . ? O1 C8 1.404(6) . ? O2 C52 1.408(6) . ? O1S C3S 1.156(12) . ? O1S C2S 1.465(12) . ? O2S C6S 1.394(15) . ? O2S C7S 1.403(13) . ? N1 C1 1.492(5) . ? N1 C7 1.493(6) . ? N1 C6 1.511(5) . ? N2 C3 1.484(6) . ? N2 C2 1.507(5) . ? N3 C5 1.486(6) . ? N3 C4 1.500(5) . ? N4 C48 1.492(5) . ? N4 C51 1.496(5) . ? N4 C50 1.513(5) . ? N5 C46 1.487(5) . ? N5 C47 1.504(5) . ? N6 C49 1.481(5) . ? N6 C45 1.497(5) . ? C1 C2 1.521(6) . ? C3 C4 1.520(6) . ? C5 C6 1.502(6) . ? C7 C8 1.529(6) . ? C9 C34 1.365(7) . ? C9 C19 1.384(7) . ? C10 C16 1.394(6) . ? C10 C17 1.407(6) . ? C11 C30 1.382(7) . ? C11 C31 1.402(6) . ? C12 C44 1.389(6) . ? C12 C20 1.395(6) . ? C13 C24 1.396(6) . ? C13 C40 1.403(6) . ? C14 C35 1.394(6) . ? C14 C28 1.409(6) . ? C15 C36 1.381(6) . ? C15 C29 1.392(8) . ? C16 C74 1.398(7) . ? C17 C73 1.390(7) . ? C18 C35 1.374(7) . ? C18 C26 1.395(8) . ? C19 C41 1.404(6) . ? C20 C21 1.405(6) . ? C21 C22 1.385(6) . ? C22 C63 1.388(7) . ? C23 C61 1.387(7) . ? C23 C37 1.390(9) . ? C24 C37 1.376(8) . ? C25 C74 1.383(8) . ? C25 C73 1.387(8) . ? C26 C42 1.397(7) . ? C27 C39 1.375(9) . ? C27 C72 1.400(6) . ? C28 C42 1.390(6) . ? C29 C30 1.377(9) . ? C31 C36 1.396(6) . ? C32 C60 1.382(7) . ? C32 C62 1.402(9) . ? C33 C62 1.343(9) . ? C33 C64 1.401(7) . ? C34 C43 1.391(6) . ? C38 C41 1.380(6) . ? C38 C43 1.405(6) . ? C39 C75 1.363(10) . ? C40 C61 1.397(6) . ? C44 C63 1.392(7) . ? C45 C46 1.506(6) . ? C47 C48 1.516(6) . ? C49 C50 1.512(6) . ? C51 C52 1.530(6) . ? C53 C54 1.393(6) . ? C53 C58 1.401(5) . ? C54 C55 1.394(6) . ? C55 C56 1.382(7) . ? C56 C57 1.384(6) . ? C57 C58 1.385(6) . ? C59 C60 1.392(7) . ? C59 C64 1.399(6) . ? C65 C70 1.393(6) . ? C65 C66 1.399(6) . ? C66 C67 1.393(6) . ? C67 C68 1.384(7) . ? C68 C69 1.378(8) . ? C69 C70 1.398(6) . ? C71 C72 1.385(6) . ? C71 C76 1.405(6) . ? C75 C76 1.388(7) . ? C77 C78 1.379(6) . ? C77 C82 1.405(6) . ? C78 C79 1.398(6) . ? C79 C80 1.389(7) . ? C80 C81 1.381(8) . ? C81 C82 1.401(7) . ? C83 C84 1.391(6) . ? C83 C88 1.413(6) . ? C84 C85 1.390(7) . ? C85 C86 1.390(8) . ? C86 C87 1.389(8) . ? C87 C88 1.389(6) . ? C1S C2S 1.431(14) . ? C3S C4S 1.406(13) . ? C5S C6S 1.545(17) . ? C7S C8S 1.500(17) . ? 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 H1 Ru1 N3 90.4(18) . . ? H1 Ru1 N2 166.8(18) . . ? N3 Ru1 N2 77.80(13) . . ? H1 Ru1 P2 79.1(18) . . ? N3 Ru1 P2 90.10(9) . . ? N2 Ru1 P2 106.35(9) . . ? H1 Ru1 N1 93.3(19) . . ? N3 Ru1 N1 77.59(13) . . ? N2 Ru1 N1 78.62(13) . . ? P2 Ru1 N1 165.59(9) . . ? H1 Ru1 P1 88.8(18) . . ? N3 Ru1 P1 175.78(10) . . ? N2 Ru1 P1 102.50(9) . . ? P2 Ru1 P1 93.83(4) . . ? N1 Ru1 P1 98.31(9) . . ? H2D Ru2 N6 92.9(19) . . ? H2D Ru2 N5 167.1(19) . . ? N6 Ru2 N5 77.77(12) . . ? H2D Ru2 P4 84.0(19) . . ? N6 Ru2 P4 90.34(9) . . ? N5 Ru2 P4 104.75(9) . . ? H2D Ru2 N4 91.2(19) . . ? N6 Ru2 N4 77.29(12) . . ? N5 Ru2 N4 78.18(12) . . ? P4 Ru2 N4 166.49(9) . . ? H2D Ru2 P3 83.2(19) . . ? N6 Ru2 P3 174.05(10) . . ? N5 Ru2 P3 105.31(9) . . ? P4 Ru2 P3 93.74(4) . . ? N4 Ru2 P3 98.21(9) . . ? C31 P1 C38 99.31(19) . . ? C31 P1 C10 98.8(2) . . ? C38 P1 C10 100.55(18) . . ? C31 P1 Ru1 118.43(15) . . ? C38 P1 Ru1 114.61(13) . . ? C10 P1 Ru1 121.36(13) . . ? C40 P2 C20 103.09(19) . . ? C40 P2 C28 99.9(2) . . ? C20 P2 C28 98.95(18) . . ? C40 P2 Ru1 120.73(15) . . ? C20 P2 Ru1 120.33(13) . . ? C28 P2 Ru1 109.93(13) . . ? C59 P3 C53 99.26(18) . . ? C59 P3 C65 99.39(19) . . ? C53 P3 C65 100.01(18) . . ? C59 P3 Ru2 118.37(15) . . ? C53 P3 Ru2 114.01(13) . . ? C65 P3 Ru2 121.95(13) . . ? C71 P4 C83 99.57(18) . . ? C71 P4 C77 102.37(19) . . ? C83 P4 C77 100.62(19) . . ? C71 P4 Ru2 119.23(14) . . ? C83 P4 Ru2 109.86(13) . . ? C77 P4 Ru2 121.60(14) . . ? C3S O1S C2S 121.6(10) . . ? C6S O2S C7S 118.6(8) . . ? C1 N1 C7 110.4(3) . . ? C1 N1 C6 108.5(3) . . ? C7 N1 C6 110.0(3) . . ? C1 N1 Ru1 106.0(2) . . ? C7 N1 Ru1 112.3(2) . . ? C6 N1 Ru1 109.5(2) . . ? C3 N2 C2 111.3(3) . . ? C3 N2 Ru1 105.8(2) . . ? C2 N2 Ru1 111.8(2) . . ? C5 N3 C4 112.2(3) . . ? C5 N3 Ru1 107.6(3) . . ? C4 N3 Ru1 114.0(2) . . ? C48 N4 C51 109.7(3) . . ? C48 N4 C50 109.0(3) . . ? C51 N4 C50 109.9(3) . . ? C48 N4 Ru2 106.2(2) . . ? C51 N4 Ru2 112.3(2) . . ? C50 N4 Ru2 109.7(2) . . ? C46 N5 C47 111.2(3) . . ? C46 N5 Ru2 105.0(2) . . ? C47 N5 Ru2 112.2(2) . . ? C49 N6 C45 113.4(3) . . ? C49 N6 Ru2 107.3(2) . . ? C45 N6 Ru2 113.6(2) . . ? N1 C1 C2 112.6(3) . . ? N2 C2 C1 113.9(3) . . ? N2 C3 C4 110.2(4) . . ? N3 C4 C3 111.1(3) . . ? N3 C5 C6 109.5(3) . . ? C5 C6 N1 111.5(3) . . ? N1 C7 C8 119.0(4) . . ? O1 C8 C7 116.3(4) . . ? C34 C9 C19 120.1(4) . . ? C16 C10 C17 117.6(4) . . ? C16 C10 P1 123.0(3) . . ? C17 C10 P1 119.2(3) . . ? C30 C11 C31 121.2(5) . . ? C44 C12 C20 121.8(4) . . ? C24 C13 C40 120.5(5) . . ? C35 C14 C28 120.6(4) . . ? C36 C15 C29 120.0(5) . . ? C10 C16 C74 121.3(5) . . ? C73 C17 C10 120.7(5) . . ? C35 C18 C26 119.3(4) . . ? C9 C19 C41 119.7(5) . . ? C12 C20 C21 117.6(4) . . ? C12 C20 P2 119.6(3) . . ? C21 C20 P2 122.8(3) . . ? C22 C21 C20 120.9(4) . . ? C21 C22 C63 120.5(4) . . ? C61 C23 C37 119.7(5) . . ? C37 C24 C13 119.9(5) . . ? C74 C25 C73 118.9(5) . . ? C18 C26 C42 120.3(5) . . ? C39 C27 C72 119.7(5) . . ? C42 C28 C14 118.1(4) . . ? C42 C28 P2 121.8(3) . . ? C14 C28 P2 119.7(3) . . ? C30 C29 C15 120.0(5) . . ? C29 C30 C11 120.0(5) . . ? C36 C31 C11 117.9(4) . . ? C36 C31 P1 121.4(3) . . ? C11 C31 P1 120.7(3) . . ? C60 C32 C62 119.7(5) . . ? C62 C33 C64 121.0(5) . . ? C9 C34 C43 120.1(4) . . ? C18 C35 C14 120.8(5) . . ? C15 C36 C31 120.9(5) . . ? C24 C37 C23 120.5(5) . . ? C41 C38 C43 117.3(4) . . ? C41 C38 P1 122.8(3) . . ? C43 C38 P1 119.5(3) . . ? C75 C39 C27 120.1(5) . . ? C61 C40 C13 118.3(4) . . ? C61 C40 P2 123.8(4) . . ? C13 C40 P2 117.8(3) . . ? C38 C41 C19 121.4(4) . . ? C28 C42 C26 120.9(5) . . ? C34 C43 C38 121.4(4) . . ? C12 C44 C63 119.7(4) . . ? N6 C45 C46 111.4(3) . . ? N5 C46 C45 110.5(3) . . ? N5 C47 C48 113.8(3) . . ? N4 C48 C47 112.8(3) . . ? N6 C49 C50 109.4(3) . . ? C49 C50 N4 110.9(3) . . ? N4 C51 C52 118.4(4) . . ? O2 C52 C51 117.4(4) . . ? C54 C53 C58 117.6(4) . . ? C54 C53 P3 123.8(3) . . ? C58 C53 P3 118.4(3) . . ? C53 C54 C55 121.0(4) . . ? C56 C55 C54 120.5(4) . . ? C55 C56 C57 119.3(4) . . ? C56 C57 C58 120.3(4) . . ? C57 C58 C53 121.4(4) . . ? C60 C59 C64 117.8(4) . . ? C60 C59 P3 121.0(3) . . ? C64 C59 P3 121.1(3) . . ? C32 C60 C59 121.3(5) . . ? C23 C61 C40 121.1(5) . . ? C33 C62 C32 119.9(5) . . ? C22 C63 C44 119.5(4) . . ? C59 C64 C33 120.3(5) . . ? C70 C65 C66 117.9(4) . . ? C70 C65 P3 120.7(3) . . ? C66 C65 P3 121.4(3) . . ? C67 C66 C65 120.9(4) . . ? C68 C67 C66 120.3(5) . . ? C69 C68 C67 119.7(4) . . ? C68 C69 C70 120.2(5) . . ? C65 C70 C69 121.1(4) . . ? C72 C71 C76 118.1(4) . . ? C72 C71 P4 118.5(3) . . ? C76 C71 P4 123.4(4) . . ? C71 C72 C27 121.0(5) . . ? C25 C73 C17 121.1(5) . . ? C25 C74 C16 120.5(5) . . ? C39 C75 C76 121.1(5) . . ? C75 C76 C71 120.1(5) . . ? C78 C77 C82 119.2(4) . . ? C78 C77 P4 118.4(3) . . ? C82 C77 P4 122.4(3) . . ? C77 C78 C79 121.2(4) . . ? C80 C79 C78 119.5(5) . . ? C81 C80 C79 120.1(4) . . ? C80 C81 C82 120.5(4) . . ? C81 C82 C77 119.6(5) . . ? C84 C83 C88 117.6(4) . . ? C84 C83 P4 121.8(3) . . ? C88 C83 P4 119.9(3) . . ? C83 C84 C85 122.0(5) . . ? C86 C85 C84 119.3(5) . . ? C87 C86 C85 120.3(5) . . ? C86 C87 C88 119.9(5) . . ? C87 C88 C83 120.9(4) . . ? C1S C2S O1S 100.0(10) . . ? O1S C3S C4S 128.6(12) . . ? O2S C6S C5S 108.5(10) . . ? O2S C7S C8S 112.5(9) . . ? F14 B1 F13 110.5(4) . . ? F14 B1 F12 108.6(4) . . ? F13 B1 F12 109.6(4) . . ? F14 B1 F11 110.0(4) . . ? F13 B1 F11 109.6(4) . . ? F12 B1 F11 108.5(4) . . ? F22B B2 F23A 51.3(8) . . ? F22B B2 F24B 129.6(9) . . ? F23A B2 F24B 112.3(8) . . ? F22B B2 F24A 157.3(10) . . ? F23A B2 F24A 115.1(8) . . ? F24B B2 F24A 31.9(5) . . ? F22B B2 F21 103.9(7) . . ? F23A B2 F21 119.0(6) . . ? F24B B2 F21 121.8(7) . . ? F24A B2 F21 98.7(7) . . ? F22B B2 F22A 67.9(8) . . ? F23A B2 F22A 109.0(6) . . ? F24B B2 F22A 78.9(7) . . ? F24A B2 F22A 107.1(6) . . ? F21 B2 F22A 106.9(5) . . ? F22B B2 F23B 91.5(10) . . ? F23A B2 F23B 42.0(6) . . ? F24B B2 F23B 97.8(8) . . ? F24A B2 F23B 82.0(7) . . ? F21 B2 F23B 102.2(6) . . ? F22A B2 F23B 147.5(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.912 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.142 #===END data_alg22 _database_code_depnum_ccdc_archive 'CCDC 685071' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'in paper 3' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46.25 H52.50 Cl1.75 N3 P2 Ru' _chemical_formula_weight 875.46 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' 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' 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 P21/c 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 19.3240(4) _cell_length_b 10.2040(2) _cell_length_c 21.5530(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.6230(10) _cell_angle_gamma 90.00 _cell_volume 4241.37(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1819 _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8426 _exptl_absorpt_correction_T_max 0.9883 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 ; 'Nonius KappaCCD area detector diffractometer' ; _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31788 _diffrn_reflns_av_R_equivalents 0.1416 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.53 _reflns_number_total 9600 _reflns_number_gt 7152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1220P)^2^+16.5570P] 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 SHELXL _refine_ls_extinction_coef 0.0046(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9600 _refine_ls_number_parameters 501 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.2397 _refine_ls_wR_factor_gt 0.2007 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.79322(2) 0.06996(4) 0.708532(19) 0.02463(18) Uani 1 1 d . . . Cl1 Cl 0.91801(5) 0.50383(11) 0.68753(5) 0.0200(3) Uani 1 1 d . . . Cl2 Cl 0.5394(4) 0.4981(16) 0.4840(4) 0.119(5) Uani 0.25 1 d P . 1 Cl3 Cl 0.5396(3) 0.3732(6) 0.4264(4) 0.097(2) Uani 0.50 1 d P A 2 P1 P 0.70890(7) 0.15009(15) 0.76636(6) 0.0258(3) Uani 1 1 d . . . P2 P 0.74702(7) 0.16254(15) 0.61729(6) 0.0276(3) Uani 1 1 d . . . N1 N 0.8790(2) -0.0520(5) 0.6691(2) 0.0283(10) Uani 1 1 d . . . N4 N 0.8876(2) 0.1951(5) 0.7301(2) 0.0300(10) Uani 1 1 d . . . H4 H 0.8784 0.2805 0.7170 0.036 Uiso 1 1 calc R . . N7 N 0.8399(2) -0.0254(5) 0.7899(2) 0.0289(10) Uani 1 1 d . . . H7 H 0.8052 -0.0375 0.8174 0.035 Uiso 1 1 calc R . . C2 C 0.9327(3) 0.0430(6) 0.6497(3) 0.0289(11) Uani 1 1 d . . . H2A H 0.9154 0.0875 0.6110 0.035 Uiso 1 1 calc R . . H2B H 0.9753 -0.0055 0.6409 0.035 Uiso 1 1 calc R . . C3 C 0.9500(3) 0.1453(6) 0.6997(3) 0.0307(12) Uani 1 1 d . . . H3A H 0.9827 0.1065 0.7319 0.037 Uiso 1 1 calc R . . H3B H 0.9737 0.2200 0.6808 0.037 Uiso 1 1 calc R . . C5 C 0.8984(3) 0.1926(6) 0.7994(3) 0.0312(12) Uani 1 1 d . . . H5A H 0.8615 0.2442 0.8178 0.037 Uiso 1 1 calc R . . H5B H 0.9436 0.2335 0.8121 0.037 Uiso 1 1 calc R . . C6 C 0.8972(3) 0.0525(6) 0.8235(3) 0.0319(12) Uani 1 1 d . . . H6A H 0.9423 0.0101 0.8175 0.038 Uiso 1 1 calc R . . H6B H 0.8901 0.0534 0.8686 0.038 Uiso 1 1 calc R . . C8 C 0.8625(3) -0.1554(6) 0.7709(3) 0.0327(12) Uani 1 1 d . . . H8A H 0.8219 -0.2088 0.7565 0.039 Uiso 1 1 calc R . . H8B H 0.8868 -0.2007 0.8066 0.039 Uiso 1 1 calc R . . C9 C 0.9111(3) -0.1395(6) 0.7187(3) 0.0309(12) Uani 1 1 d . . . H9A H 0.9556 -0.1013 0.7353 0.037 Uiso 1 1 calc R . . H9B H 0.9209 -0.2264 0.7007 0.037 Uiso 1 1 calc R . . C10 C 0.8532(3) -0.1331(6) 0.6148(3) 0.0322(12) Uani 1 1 d . . . H10A H 0.8239 -0.0769 0.5864 0.039 Uiso 1 1 calc R . . H10B H 0.8231 -0.2031 0.6301 0.039 Uiso 1 1 calc R . . C11 C 0.9092(3) -0.1977(6) 0.5770(3) 0.0371(13) Uani 1 1 d . . . H11A H 0.9365 -0.1288 0.5574 0.044 Uiso 1 1 calc R . . H11B H 0.9411 -0.2491 0.6053 0.044 Uiso 1 1 calc R . . C12 C 0.8771(4) -0.2855(9) 0.5279(3) 0.0533(19) Uani 1 1 d . . . H12 H 0.8526 -0.3600 0.5413 0.064 Uiso 1 1 calc R . . C13 C 0.8798(5) -0.2686(10) 0.4682(4) 0.068(2) Uani 1 1 d . . . H13A H 0.9038 -0.1953 0.4528 0.082 Uiso 1 1 calc R . . H13B H 0.8578 -0.3295 0.4400 0.082 Uiso 1 1 calc R . . C14 C 0.7026(3) 0.3234(6) 0.6212(3) 0.0323(12) Uani 1 1 d . . . C15 C 0.6305(3) 0.3268(7) 0.6308(3) 0.0406(15) Uani 1 1 d . . . H15 H 0.6049 0.2473 0.6297 0.049 Uiso 1 1 calc R . . C16 C 0.5967(4) 0.4440(8) 0.6418(4) 0.055(2) Uani 1 1 d . . . H16 H 0.5486 0.4440 0.6486 0.066 Uiso 1 1 calc R . . C17 C 0.6331(4) 0.5605(8) 0.6428(4) 0.055(2) Uani 1 1 d . . . H17 H 0.6100 0.6403 0.6507 0.066 Uiso 1 1 calc R . . C18 C 0.7031(4) 0.5620(7) 0.6323(3) 0.0488(17) Uani 1 1 d . . . H18 H 0.7279 0.6424 0.6323 0.059 Uiso 1 1 calc R . . C19 C 0.7370(3) 0.4429(7) 0.6215(3) 0.0409(15) Uani 1 1 d . . . H19 H 0.7849 0.4442 0.6142 0.049 Uiso 1 1 calc R . . C20 C 0.8091(3) 0.1950(6) 0.5570(3) 0.0304(12) Uani 1 1 d . . . C21 C 0.8631(3) 0.2843(7) 0.5686(3) 0.0378(14) Uani 1 1 d . . . H21 H 0.8662 0.3316 0.6067 0.045 Uiso 1 1 calc R . . C22 C 0.9128(3) 0.3051(8) 0.5254(3) 0.0439(16) Uani 1 1 d . . . H22 H 0.9486 0.3674 0.5337 0.053 Uiso 1 1 calc R . . C23 C 0.9097(3) 0.2351(8) 0.4707(3) 0.0494(18) Uani 1 1 d . . . H23 H 0.9435 0.2499 0.4413 0.059 Uiso 1 1 calc R . . C24 C 0.8582(3) 0.1440(7) 0.4582(3) 0.0417(15) Uani 1 1 d . . . H24 H 0.8572 0.0945 0.4208 0.050 Uiso 1 1 calc R . . C25 C 0.8075(3) 0.1242(7) 0.5005(3) 0.0371(14) Uani 1 1 d . . . H25 H 0.7715 0.0625 0.4913 0.044 Uiso 1 1 calc R . . C26 C 0.6807(3) 0.0705(6) 0.5685(3) 0.0317(13) Uani 1 1 d . . . C27 C 0.6402(3) 0.1315(7) 0.5215(3) 0.0383(14) Uani 1 1 d . . . H27 H 0.6464 0.2223 0.5137 0.046 Uiso 1 1 calc R . . C28 C 0.5909(3) 0.0619(8) 0.4857(3) 0.0465(18) Uani 1 1 d . . . H28 H 0.5625 0.1055 0.4546 0.056 Uiso 1 1 calc R . . C29 C 0.5828(3) -0.0728(8) 0.4953(3) 0.0466(18) Uani 1 1 d . . . H29 H 0.5490 -0.1208 0.4707 0.056 Uiso 1 1 calc R . . C30 C 0.6238(3) -0.1345(8) 0.5402(3) 0.0420(15) Uani 1 1 d . . . H30 H 0.6191 -0.2262 0.5464 0.050 Uiso 1 1 calc R . . C31 C 0.6723(3) -0.0642(6) 0.5767(3) 0.0348(13) Uani 1 1 d . . . H31 H 0.7004 -0.1083 0.6079 0.042 Uiso 1 1 calc R . . C32 C 0.6163(3) 0.1344(6) 0.7396(2) 0.0294(12) Uani 1 1 d . . . C33 C 0.5961(3) 0.0272(6) 0.7034(3) 0.0334(13) Uani 1 1 d . . . H33 H 0.6296 -0.0359 0.6930 0.040 Uiso 1 1 calc R . . C34 C 0.5269(3) 0.0111(7) 0.6820(3) 0.0412(15) Uani 1 1 d . . . H34 H 0.5139 -0.0620 0.6566 0.049 Uiso 1 1 calc R . . C35 C 0.4772(3) 0.1010(8) 0.6977(3) 0.0467(16) Uani 1 1 d . . . H35 H 0.4301 0.0896 0.6832 0.056 Uiso 1 1 calc R . . C36 C 0.4966(3) 0.2067(8) 0.7343(3) 0.0496(17) Uani 1 1 d . . . H36 H 0.4628 0.2688 0.7452 0.060 Uiso 1 1 calc R . . C37 C 0.5654(3) 0.2232(7) 0.7554(3) 0.0366(13) Uani 1 1 d . . . H37 H 0.5780 0.2960 0.7812 0.044 Uiso 1 1 calc R . . C38 C 0.7049(3) 0.0598(6) 0.8407(3) 0.0288(12) Uani 1 1 d . . . C39 C 0.6675(3) -0.0580(6) 0.8437(3) 0.0366(14) Uani 1 1 d . . . H39 H 0.6416 -0.0890 0.8077 0.044 Uiso 1 1 calc R . . C40 C 0.6678(3) -0.1293(7) 0.8983(3) 0.0417(15) Uani 1 1 d . . . H40 H 0.6426 -0.2091 0.8992 0.050 Uiso 1 1 calc R . . C41 C 0.7043(4) -0.0862(7) 0.9513(3) 0.0431(16) Uani 1 1 d . . . H41 H 0.7035 -0.1346 0.9889 0.052 Uiso 1 1 calc R . . C42 C 0.7426(3) 0.0301(7) 0.9489(3) 0.0375(14) Uani 1 1 d . . . H42 H 0.7686 0.0605 0.9850 0.045 Uiso 1 1 calc R . . C43 C 0.7427(3) 0.0997(7) 0.8949(3) 0.0338(13) Uani 1 1 d . . . H43 H 0.7692 0.1780 0.8941 0.041 Uiso 1 1 calc R . . C44 C 0.7167(3) 0.3205(6) 0.7956(2) 0.0301(12) Uani 1 1 d . . . C45 C 0.6855(3) 0.3704(6) 0.8481(3) 0.0306(12) Uani 1 1 d . . . H45 H 0.6547 0.3170 0.8697 0.037 Uiso 1 1 calc R . . C46 C 0.6996(3) 0.4957(6) 0.8681(3) 0.0380(14) Uani 1 1 d . . . H46 H 0.6770 0.5294 0.9026 0.046 Uiso 1 1 calc R . . C47 C 0.7458(4) 0.5735(7) 0.8390(3) 0.0430(15) Uani 1 1 d . . . H47 H 0.7559 0.6594 0.8540 0.052 Uiso 1 1 calc R . . C48 C 0.7775(4) 0.5259(7) 0.7880(3) 0.0419(15) Uani 1 1 d . . . H48 H 0.8091 0.5793 0.7673 0.050 Uiso 1 1 calc R . . C49 C 0.7630(3) 0.4002(6) 0.7669(3) 0.0326(12) Uani 1 1 d . . . H49 H 0.7854 0.3679 0.7320 0.039 Uiso 1 1 calc R . . C2A C 0.5394(4) 0.4981(16) 0.4840(4) 0.119(5) Uani 0.25 1 d P . 2 H2A1 H 0.5765 0.4808 0.5168 0.143 Uiso 0.25 1 calc PR . 2 H2A2 H 0.5487 0.5841 0.4649 0.143 Uiso 0.25 1 calc PR . 2 H1 H 0.733(4) -0.046(8) 0.701(3) 0.05(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0198(2) 0.0284(3) 0.0258(3) 0.00063(17) 0.00189(16) -0.00012(16) Cl1 0.0125(5) 0.0178(5) 0.0294(6) -0.0019(5) -0.0007(4) -0.0048(4) Cl2 0.057(5) 0.245(15) 0.056(4) 0.036(7) 0.003(4) -0.037(7) Cl3 0.053(3) 0.071(3) 0.165(6) 0.027(4) -0.012(3) 0.006(2) P1 0.0210(6) 0.0303(8) 0.0261(7) 0.0007(6) 0.0022(5) -0.0011(5) P2 0.0229(6) 0.0335(8) 0.0265(7) 0.0007(6) 0.0018(5) 0.0014(5) N1 0.031(2) 0.022(2) 0.032(2) -0.0002(19) 0.0048(19) 0.0006(18) N4 0.022(2) 0.038(3) 0.030(2) 0.001(2) 0.0005(17) -0.0003(19) N7 0.027(2) 0.029(2) 0.031(2) 0.002(2) 0.0026(18) -0.0029(19) C2 0.022(2) 0.030(3) 0.034(3) 0.001(2) 0.001(2) 0.002(2) C3 0.022(2) 0.032(3) 0.039(3) 0.006(2) 0.004(2) -0.001(2) C5 0.026(3) 0.037(3) 0.031(3) -0.001(2) -0.002(2) -0.004(2) C6 0.026(3) 0.040(3) 0.029(3) 0.008(2) -0.002(2) 0.005(2) C8 0.030(3) 0.039(3) 0.029(3) 0.003(2) -0.001(2) 0.005(2) C9 0.025(3) 0.030(3) 0.038(3) 0.004(2) 0.003(2) 0.003(2) C10 0.026(3) 0.034(3) 0.037(3) -0.004(3) 0.004(2) 0.002(2) C11 0.038(3) 0.035(3) 0.039(3) -0.004(3) 0.009(3) 0.002(3) C12 0.049(4) 0.062(5) 0.050(4) -0.016(4) 0.017(3) -0.003(4) C13 0.073(6) 0.080(6) 0.053(5) -0.022(4) 0.011(4) -0.014(5) C14 0.035(3) 0.036(3) 0.026(3) 0.003(2) 0.003(2) 0.009(2) C15 0.038(3) 0.046(4) 0.039(3) 0.007(3) 0.009(3) 0.006(3) C16 0.044(4) 0.066(5) 0.056(4) 0.012(4) 0.019(3) 0.022(4) C17 0.065(5) 0.049(5) 0.053(4) 0.013(4) 0.017(4) 0.020(4) C18 0.060(4) 0.039(4) 0.049(4) 0.008(3) 0.011(3) 0.002(3) C19 0.036(3) 0.046(4) 0.040(3) 0.004(3) 0.002(3) 0.003(3) C20 0.028(3) 0.036(3) 0.027(3) 0.006(2) 0.003(2) 0.004(2) C21 0.029(3) 0.045(4) 0.039(3) 0.012(3) -0.002(2) 0.006(3) C22 0.028(3) 0.056(4) 0.049(4) 0.015(3) 0.005(3) -0.002(3) C23 0.033(3) 0.074(5) 0.043(4) 0.015(4) 0.014(3) 0.009(3) C24 0.041(3) 0.053(4) 0.032(3) -0.001(3) 0.008(3) 0.011(3) C25 0.029(3) 0.046(4) 0.036(3) 0.001(3) 0.004(2) 0.006(3) C26 0.024(3) 0.040(3) 0.031(3) 0.002(2) 0.004(2) 0.003(2) C27 0.029(3) 0.056(4) 0.030(3) 0.006(3) 0.005(2) -0.001(3) C28 0.024(3) 0.083(6) 0.032(3) 0.002(3) 0.000(2) 0.002(3) C29 0.027(3) 0.075(6) 0.038(3) -0.015(3) 0.002(3) -0.011(3) C30 0.028(3) 0.056(4) 0.043(3) -0.013(3) 0.007(3) -0.005(3) C31 0.027(3) 0.040(4) 0.037(3) -0.004(3) 0.003(2) -0.002(2) C32 0.023(3) 0.040(3) 0.025(3) 0.004(2) 0.005(2) -0.001(2) C33 0.028(3) 0.041(3) 0.031(3) 0.003(3) 0.002(2) -0.005(2) C34 0.032(3) 0.047(4) 0.044(3) -0.003(3) -0.003(3) -0.013(3) C35 0.024(3) 0.059(4) 0.056(4) -0.004(4) -0.006(3) -0.002(3) C36 0.029(3) 0.062(5) 0.058(4) 0.001(4) 0.003(3) 0.007(3) C37 0.026(3) 0.044(4) 0.040(3) 0.000(3) 0.003(2) 0.004(3) C38 0.024(3) 0.034(3) 0.029(3) -0.002(2) 0.004(2) 0.000(2) C39 0.034(3) 0.042(4) 0.033(3) -0.004(3) 0.000(2) -0.007(3) C40 0.044(4) 0.041(4) 0.041(3) 0.010(3) 0.007(3) -0.008(3) C41 0.052(4) 0.043(4) 0.035(3) 0.011(3) 0.008(3) 0.003(3) C42 0.038(3) 0.045(4) 0.030(3) 0.003(3) -0.002(2) 0.000(3) C43 0.029(3) 0.038(3) 0.034(3) 0.003(3) 0.003(2) -0.005(2) C44 0.027(3) 0.035(3) 0.028(3) -0.002(2) 0.002(2) 0.001(2) C45 0.026(3) 0.035(3) 0.031(3) 0.002(2) 0.007(2) 0.002(2) C46 0.039(3) 0.041(4) 0.035(3) -0.007(3) 0.007(3) 0.008(3) C47 0.045(4) 0.036(4) 0.049(4) -0.004(3) 0.004(3) -0.001(3) C48 0.045(4) 0.035(3) 0.047(4) 0.001(3) 0.014(3) -0.004(3) C49 0.033(3) 0.032(3) 0.033(3) -0.002(3) 0.005(2) 0.003(2) C2A 0.057(5) 0.245(15) 0.056(4) 0.036(7) 0.003(4) -0.037(7) _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 Ru1 H1 1.66(8) . ? Ru1 N7 2.152(5) . ? Ru1 N4 2.251(5) . ? Ru1 P1 2.2658(14) . ? Ru1 N1 2.279(5) . ? Ru1 P2 2.3098(15) . ? Cl2 Cl2 1.712(17) 3_666 ? P1 C32 1.852(6) . ? P1 C44 1.853(6) . ? P1 C38 1.854(6) . ? P2 C20 1.852(6) . ? P2 C14 1.857(6) . ? P2 C26 1.861(6) . ? N1 C10 1.492(7) . ? N1 C9 1.497(7) . ? N1 C2 1.498(7) . ? N4 C5 1.495(7) . ? N4 C3 1.497(7) . ? N7 C8 1.463(8) . ? N7 C6 1.511(7) . ? C2 C3 1.522(8) . ? C5 C6 1.522(8) . ? C8 C9 1.520(8) . ? C10 C11 1.542(8) . ? C11 C12 1.492(10) . ? C12 C13 1.303(11) . ? C14 C19 1.388(9) . ? C14 C15 1.421(8) . ? C15 C16 1.390(10) . ? C16 C17 1.380(12) . ? C17 C18 1.386(11) . ? C18 C19 1.406(10) . ? C20 C21 1.397(9) . ? C20 C25 1.414(9) . ? C21 C22 1.395(9) . ? C22 C23 1.377(11) . ? C23 C24 1.377(11) . ? C24 C25 1.395(8) . ? C26 C27 1.388(8) . ? C26 C31 1.396(9) . ? C27 C28 1.383(9) . ? C28 C29 1.400(11) . ? C29 C30 1.366(10) . ? C30 C31 1.387(9) . ? C32 C33 1.385(9) . ? C32 C37 1.396(8) . ? C33 C34 1.395(8) . ? C34 C35 1.386(10) . ? C35 C36 1.375(11) . ? C36 C37 1.388(9) . ? C38 C43 1.399(8) . ? C38 C39 1.407(8) . ? C39 C40 1.384(9) . ? C40 C41 1.376(10) . ? C41 C42 1.402(10) . ? C42 C43 1.364(9) . ? C44 C49 1.383(8) . ? C44 C45 1.411(8) . ? C45 C46 1.372(9) . ? C46 C47 1.375(9) . ? C47 C48 1.381(9) . ? C48 C49 1.383(9) . ? 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 H1 Ru1 N7 91(3) . . ? H1 Ru1 N4 168(3) . . ? N7 Ru1 N4 78.25(18) . . ? H1 Ru1 P1 78(3) . . ? N7 Ru1 P1 89.64(13) . . ? N4 Ru1 P1 106.47(13) . . ? H1 Ru1 N1 95(3) . . ? N7 Ru1 N1 77.30(18) . . ? N4 Ru1 N1 77.75(17) . . ? P1 Ru1 N1 165.29(13) . . ? H1 Ru1 P2 88(3) . . ? N7 Ru1 P2 176.20(14) . . ? N4 Ru1 P2 102.02(13) . . ? P1 Ru1 P2 93.90(5) . . ? N1 Ru1 P2 99.02(13) . . ? C32 P1 C44 104.1(3) . . ? C32 P1 C38 97.7(2) . . ? C44 P1 C38 100.4(3) . . ? C32 P1 Ru1 120.75(18) . . ? C44 P1 Ru1 118.65(18) . . ? C38 P1 Ru1 111.53(18) . . ? C20 P2 C14 101.3(3) . . ? C20 P2 C26 98.4(3) . . ? C14 P2 C26 99.7(3) . . ? C20 P2 Ru1 115.96(18) . . ? C14 P2 Ru1 118.54(18) . . ? C26 P2 Ru1 119.4(2) . . ? C10 N1 C9 109.4(4) . . ? C10 N1 C2 110.1(4) . . ? C9 N1 C2 108.7(4) . . ? C10 N1 Ru1 112.4(3) . . ? C9 N1 Ru1 109.7(3) . . ? C2 N1 Ru1 106.4(3) . . ? C5 N4 C3 111.4(4) . . ? C5 N4 Ru1 104.9(3) . . ? C3 N4 Ru1 112.5(4) . . ? C8 N7 C6 112.8(4) . . ? C8 N7 Ru1 107.4(3) . . ? C6 N7 Ru1 114.1(3) . . ? N1 C2 C3 111.9(4) . . ? N4 C3 C2 113.2(4) . . ? N4 C5 C6 110.6(5) . . ? N7 C6 C5 111.0(4) . . ? N7 C8 C9 108.7(5) . . ? N1 C9 C8 110.2(4) . . ? N1 C10 C11 116.1(5) . . ? C12 C11 C10 110.9(5) . . ? C13 C12 C11 125.5(8) . . ? C19 C14 C15 116.8(6) . . ? C19 C14 P2 123.6(5) . . ? C15 C14 P2 119.2(5) . . ? C16 C15 C14 121.4(7) . . ? C17 C16 C15 119.9(7) . . ? C16 C17 C18 120.6(7) . . ? C17 C18 C19 119.1(7) . . ? C14 C19 C18 122.1(6) . . ? C21 C20 C25 117.6(5) . . ? C21 C20 P2 120.0(4) . . ? C25 C20 P2 122.2(5) . . ? C22 C21 C20 121.2(6) . . ? C23 C22 C21 120.0(7) . . ? C24 C23 C22 120.6(6) . . ? C23 C24 C25 120.0(6) . . ? C24 C25 C20 120.7(6) . . ? C27 C26 C31 118.1(6) . . ? C27 C26 P2 121.5(5) . . ? C31 C26 P2 120.4(5) . . ? C28 C27 C26 120.9(7) . . ? C27 C28 C29 120.1(6) . . ? C30 C29 C28 119.4(6) . . ? C29 C30 C31 120.4(7) . . ? C30 C31 C26 121.1(6) . . ? C33 C32 C37 118.2(5) . . ? C33 C32 P1 118.5(4) . . ? C37 C32 P1 123.3(5) . . ? C32 C33 C34 120.6(6) . . ? C35 C34 C33 120.4(6) . . ? C36 C35 C34 119.4(6) . . ? C35 C36 C37 120.3(7) . . ? C36 C37 C32 121.1(6) . . ? C43 C38 C39 117.0(5) . . ? C43 C38 P1 122.0(4) . . ? C39 C38 P1 120.9(4) . . ? C40 C39 C38 120.9(6) . . ? C41 C40 C39 120.9(6) . . ? C40 C41 C42 119.0(6) . . ? C43 C42 C41 120.1(6) . . ? C42 C43 C38 122.2(6) . . ? C49 C44 C45 117.9(6) . . ? C49 C44 P1 116.2(4) . . ? C45 C44 P1 125.5(5) . . ? C46 C45 C44 120.1(5) . . ? C45 C46 C47 121.1(6) . . ? C46 C47 C48 119.6(6) . . ? C47 C48 C49 119.8(6) . . ? C48 C49 C44 121.4(6) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 3.040 _refine_diff_density_min -2.159 _refine_diff_density_rms 0.208 #===END data_alg5 _database_code_depnum_ccdc_archive 'CCDC 685072' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'in paper 5' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H41 B2 F8 N4 O2 P Ru' _chemical_formula_weight 843.37 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' P P 0.1023 0.0942 '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' B B 0.0013 0.0007 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3690(2) _cell_length_b 12.4991(2) _cell_length_c 23.0691(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.0030(10) _cell_angle_gamma 90.00 _cell_volume 3552.93(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8951 _exptl_absorpt_correction_T_max 0.8951 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36076 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6976 _reflns_number_gt 5993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+2.6835P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6976 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0779 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru -0.190264(14) 0.177225(13) 0.088525(7) 0.01869(7) Uani 1 1 d . . . C1 C -0.10728(19) 0.21090(17) 0.02824(10) 0.0233(5) Uani 1 1 d . . . O1 O -0.05587(14) 0.22645(14) -0.01035(7) 0.0330(4) Uani 1 1 d . . . N1 N -0.07885(16) 0.06191(14) 0.12592(8) 0.0231(4) Uani 1 1 d . . . C2 C -0.0716(2) -0.02087(18) 0.07942(10) 0.0261(5) Uani 1 1 d . . . H2A H -0.0312 -0.0840 0.0957 0.031 Uiso 1 1 calc R . . H2B H -0.0321 0.0087 0.0475 0.031 Uiso 1 1 calc R . . C3 C -0.1856(2) -0.05400(17) 0.05598(10) 0.0269(5) Uani 1 1 d . . . H3A H -0.1818 -0.0931 0.0189 0.032 Uiso 1 1 calc R . . H3B H -0.2159 -0.1032 0.0840 0.032 Uiso 1 1 calc R . . N4 N -0.26058(15) 0.04161(14) 0.04576(8) 0.0226(4) Uani 1 1 d . . . H4 H -0.2705 0.0554 0.0060 0.027 Uiso 1 1 calc R . . C5 C -0.36821(19) 0.02328(18) 0.06805(10) 0.0256(5) Uani 1 1 d . . . H5A H -0.3969 -0.0472 0.0546 0.031 Uiso 1 1 calc R . . H5B H -0.4198 0.0790 0.0526 0.031 Uiso 1 1 calc R . . C6 C -0.35776(19) 0.02668(18) 0.13422(10) 0.0261(5) Uani 1 1 d . . . H6A H -0.4304 0.0368 0.1483 0.031 Uiso 1 1 calc R . . H6B H -0.3284 -0.0424 0.1496 0.031 Uiso 1 1 calc R . . N7 N -0.28378(15) 0.11645(15) 0.15673(8) 0.0232(4) Uani 1 1 d . . . H7 H -0.3254 0.1716 0.1702 0.028 Uiso 1 1 calc R . . C8 C -0.20334(19) 0.08004(19) 0.20498(10) 0.0261(5) Uani 1 1 d . . . H8A H -0.2407 0.0377 0.2335 0.031 Uiso 1 1 calc R . . H8B H -0.1692 0.1429 0.2253 0.031 Uiso 1 1 calc R . . C9 C -0.1172(2) 0.01221(18) 0.17999(10) 0.0257(5) Uani 1 1 d . . . H9A H -0.0547 0.0037 0.2095 0.031 Uiso 1 1 calc R . . H9B H -0.1471 -0.0598 0.1705 0.031 Uiso 1 1 calc R . . C10 C 0.02384(19) 0.12264(18) 0.13927(11) 0.0268(5) Uani 1 1 d . . . H10A H 0.0590 0.1354 0.1030 0.032 Uiso 1 1 calc R . . H10B H 0.0743 0.0804 0.1660 0.032 Uiso 1 1 calc R . . C11 C -0.00012(19) 0.22784(19) 0.16711(10) 0.0255(5) Uani 1 1 d . . . N12 N -0.09834(15) 0.27304(15) 0.14997(8) 0.0219(4) Uani 1 1 d . . . C13 C -0.1243(2) 0.36607(18) 0.17498(10) 0.0253(5) Uani 1 1 d . . . H13 H -0.1941 0.3959 0.1650 0.030 Uiso 1 1 calc R . . C14 C -0.0533(2) 0.4197(2) 0.21451(10) 0.0302(5) Uani 1 1 d . . . H14 H -0.0736 0.4858 0.2307 0.036 Uiso 1 1 calc R . . C15 C 0.0478(2) 0.3758(2) 0.23010(11) 0.0346(6) Uani 1 1 d . . . H15 H 0.0986 0.4123 0.2563 0.041 Uiso 1 1 calc R . . C16 C 0.0736(2) 0.2778(2) 0.20695(11) 0.0329(6) Uani 1 1 d . . . H16 H 0.1415 0.2450 0.2183 0.039 Uiso 1 1 calc R . . P1 P -0.31547(5) 0.30503(4) 0.05008(2) 0.01982(13) Uani 1 1 d . . . C111 C -0.25730(18) 0.42797(17) 0.02188(9) 0.0219(5) Uani 1 1 d . . . C112 C -0.1541(2) 0.46296(19) 0.04211(10) 0.0275(5) Uani 1 1 d . . . H112 H -0.1109 0.4208 0.0695 0.033 Uiso 1 1 calc R . . C113 C -0.1134(2) 0.55899(19) 0.02264(11) 0.0335(6) Uani 1 1 d . . . H113 H -0.0438 0.5832 0.0378 0.040 Uiso 1 1 calc R . . C114 C -0.1740(2) 0.61940(19) -0.01871(11) 0.0303(5) Uani 1 1 d . . . H114 H -0.1464 0.6850 -0.0320 0.036 Uiso 1 1 calc R . . C115 C -0.2749(2) 0.58338(19) -0.04041(11) 0.0299(5) Uani 1 1 d . . . H115 H -0.3157 0.6235 -0.0697 0.036 Uiso 1 1 calc R . . C116 C -0.3175(2) 0.48938(19) -0.02013(10) 0.0272(5) Uani 1 1 d . . . H116 H -0.3879 0.4665 -0.0348 0.033 Uiso 1 1 calc R . . C121 C -0.40903(18) 0.35256(18) 0.10141(9) 0.0218(5) Uani 1 1 d . . . C122 C -0.40815(19) 0.45821(18) 0.12068(10) 0.0259(5) Uani 1 1 d . . . H122 H -0.3588 0.5080 0.1064 0.031 Uiso 1 1 calc R . . C123 C -0.4792(2) 0.49119(19) 0.16077(10) 0.0305(5) Uani 1 1 d . . . H123 H -0.4783 0.5635 0.1735 0.037 Uiso 1 1 calc R . . C124 C -0.5513(2) 0.4196(2) 0.18230(10) 0.0298(5) Uani 1 1 d . . . H124 H -0.5998 0.4428 0.2094 0.036 Uiso 1 1 calc R . . C125 C -0.5522(2) 0.31379(19) 0.16404(10) 0.0277(5) Uani 1 1 d . . . H125 H -0.6006 0.2641 0.1791 0.033 Uiso 1 1 calc R . . C126 C -0.48208(18) 0.28066(18) 0.12357(10) 0.0242(5) Uani 1 1 d . . . H126 H -0.4837 0.2084 0.1108 0.029 Uiso 1 1 calc R . . C131 C -0.40299(19) 0.26337(17) -0.01404(10) 0.0225(5) Uani 1 1 d . . . C132 C -0.3536(2) 0.22113(18) -0.06113(10) 0.0274(5) Uani 1 1 d . . . H132 H -0.2782 0.2050 -0.0572 0.033 Uiso 1 1 calc R . . C133 C -0.4139(2) 0.2026(2) -0.11356(10) 0.0322(6) Uani 1 1 d . . . H133 H -0.3797 0.1734 -0.1453 0.039 Uiso 1 1 calc R . . C134 C -0.5233(2) 0.22616(19) -0.12013(10) 0.0313(6) Uani 1 1 d . . . H134 H -0.5637 0.2152 -0.1566 0.038 Uiso 1 1 calc R . . C135 C -0.5741(2) 0.26587(19) -0.07332(11) 0.0301(5) Uani 1 1 d . . . H135 H -0.6497 0.2806 -0.0775 0.036 Uiso 1 1 calc R . . C136 C -0.51435(19) 0.28407(18) -0.02035(10) 0.0264(5) Uani 1 1 d . . . H136 H -0.5495 0.3107 0.0117 0.032 Uiso 1 1 calc R . . B1 B -0.2953(2) -0.0664(2) -0.09940(13) 0.0326(6) Uani 1 1 d . . . F11 F -0.37643(13) -0.06126(15) -0.06148(8) 0.0530(5) Uani 1 1 d . . . F12 F -0.33802(18) -0.04262(15) -0.15480(7) 0.0668(6) Uani 1 1 d . . . F13 F -0.24967(13) -0.16729(11) -0.09789(8) 0.0459(4) Uani 1 1 d . . . F14 F -0.21496(12) 0.00869(11) -0.08050(7) 0.0386(4) Uani 1 1 d . . . B2 B -0.1706(2) -0.2897(2) 0.18887(12) 0.0289(6) Uani 1 1 d . . . F21 F -0.11176(13) -0.24518(12) 0.14647(7) 0.0407(4) Uani 1 1 d . . . F22 F -0.10137(12) -0.31890(12) 0.23712(6) 0.0376(4) Uani 1 1 d . . . F23 F -0.24502(13) -0.21463(13) 0.20595(8) 0.0494(4) Uani 1 1 d . . . F24 F -0.22554(14) -0.38013(12) 0.16729(6) 0.0429(4) Uani 1 1 d . . . O1S O 0.2393(2) 0.1229(2) 0.28377(11) 0.0698(7) Uani 1 1 d . . . C1S C 0.3111(2) 0.1620(3) 0.31721(13) 0.0477(8) Uani 1 1 d . . . C2S C 0.3444(3) 0.2758(3) 0.31367(15) 0.0549(8) Uani 1 1 d . . . H2S1 H 0.2966 0.3125 0.2839 0.082 Uiso 1 1 calc R . . H2S2 H 0.4195 0.2796 0.3034 0.082 Uiso 1 1 calc R . . H2S3 H 0.3390 0.3104 0.3514 0.082 Uiso 1 1 calc R . . C3S C 0.3696(3) 0.0964(3) 0.36365(13) 0.0558(9) Uani 1 1 d . . . H3S1 H 0.3477 0.0214 0.3588 0.084 Uiso 1 1 calc R . . H3S2 H 0.3517 0.1220 0.4018 0.084 Uiso 1 1 calc R . . H3S3 H 0.4480 0.1026 0.3610 0.084 Uiso 1 1 calc 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 0.01934(10) 0.01744(10) 0.01930(10) 0.00126(7) 0.00180(7) 0.00105(7) C1 0.0239(12) 0.0196(11) 0.0262(12) 0.0011(9) 0.0003(10) -0.0003(9) O1 0.0316(10) 0.0362(10) 0.0326(9) 0.0030(8) 0.0103(8) -0.0027(8) N1 0.0251(10) 0.0205(9) 0.0241(9) 0.0017(8) 0.0036(8) 0.0030(8) C2 0.0308(13) 0.0234(11) 0.0246(11) -0.0007(9) 0.0054(10) 0.0063(10) C3 0.0346(14) 0.0187(11) 0.0277(12) -0.0011(9) 0.0035(10) 0.0047(10) N4 0.0264(10) 0.0192(9) 0.0223(9) 0.0011(8) 0.0023(8) 0.0015(8) C5 0.0261(12) 0.0219(11) 0.0285(12) 0.0001(10) 0.0010(10) -0.0010(9) C6 0.0257(12) 0.0219(11) 0.0311(12) 0.0040(10) 0.0050(10) -0.0028(9) N7 0.0245(10) 0.0215(9) 0.0238(9) 0.0009(8) 0.0040(8) 0.0029(8) C8 0.0291(13) 0.0273(12) 0.0220(11) 0.0052(9) 0.0028(10) 0.0026(10) C9 0.0300(13) 0.0246(11) 0.0225(11) 0.0055(9) 0.0018(10) 0.0048(10) C10 0.0211(12) 0.0278(12) 0.0312(12) 0.0025(10) 0.0009(10) 0.0037(9) C11 0.0231(12) 0.0262(12) 0.0269(11) 0.0037(10) 0.0010(9) 0.0007(10) N12 0.0201(10) 0.0232(9) 0.0224(9) 0.0025(8) 0.0014(8) 0.0021(8) C13 0.0283(13) 0.0214(11) 0.0261(11) 0.0015(9) 0.0009(10) 0.0010(9) C14 0.0367(14) 0.0273(12) 0.0260(12) -0.0016(10) -0.0003(10) -0.0020(10) C15 0.0379(15) 0.0349(14) 0.0288(13) -0.0011(11) -0.0085(11) -0.0056(11) C16 0.0274(13) 0.0344(13) 0.0354(13) 0.0031(11) -0.0064(11) 0.0013(11) P1 0.0194(3) 0.0184(3) 0.0214(3) 0.0012(2) 0.0005(2) 0.0005(2) C111 0.0242(12) 0.0186(10) 0.0232(11) 0.0005(9) 0.0035(9) 0.0014(9) C112 0.0282(13) 0.0263(12) 0.0272(12) 0.0040(10) -0.0024(10) -0.0007(10) C113 0.0330(14) 0.0292(13) 0.0373(14) 0.0039(11) -0.0025(11) -0.0081(11) C114 0.0355(14) 0.0216(11) 0.0344(13) 0.0058(10) 0.0072(11) -0.0016(10) C115 0.0295(13) 0.0279(12) 0.0325(13) 0.0090(10) 0.0041(10) 0.0056(10) C116 0.0232(12) 0.0284(12) 0.0295(12) 0.0054(10) 0.0003(10) 0.0014(10) C121 0.0196(11) 0.0238(11) 0.0214(11) 0.0018(9) -0.0013(9) 0.0031(9) C122 0.0291(13) 0.0237(11) 0.0244(11) 0.0007(9) -0.0006(10) -0.0014(10) C123 0.0391(15) 0.0256(12) 0.0270(12) -0.0046(10) 0.0044(11) 0.0023(10) C124 0.0284(13) 0.0370(14) 0.0243(12) -0.0022(10) 0.0049(10) 0.0039(11) C125 0.0257(13) 0.0310(13) 0.0263(12) 0.0026(10) 0.0015(10) -0.0010(10) C126 0.0235(12) 0.0211(11) 0.0276(12) 0.0011(9) 0.0002(9) 0.0014(9) C131 0.0263(12) 0.0171(10) 0.0235(11) 0.0013(9) -0.0016(9) -0.0028(9) C132 0.0283(13) 0.0248(12) 0.0285(12) 0.0009(10) -0.0007(10) 0.0016(10) C133 0.0412(15) 0.0308(13) 0.0242(12) -0.0020(10) 0.0010(11) -0.0018(11) C134 0.0398(15) 0.0255(12) 0.0267(12) 0.0029(10) -0.0075(11) -0.0079(11) C135 0.0264(13) 0.0253(12) 0.0368(13) 0.0040(10) -0.0067(11) -0.0037(10) C136 0.0270(13) 0.0232(11) 0.0283(12) -0.0002(10) -0.0009(10) 0.0014(10) B1 0.0308(16) 0.0350(15) 0.0320(15) -0.0035(12) 0.0027(12) 0.0023(12) F11 0.0318(9) 0.0703(12) 0.0585(11) -0.0221(9) 0.0133(8) -0.0097(8) F12 0.0998(16) 0.0589(11) 0.0372(9) -0.0052(9) -0.0189(10) 0.0164(11) F13 0.0375(9) 0.0283(8) 0.0716(12) 0.0016(8) 0.0035(8) 0.0003(7) F14 0.0375(9) 0.0330(8) 0.0463(9) -0.0053(7) 0.0100(7) -0.0049(6) B2 0.0285(15) 0.0246(13) 0.0330(14) 0.0048(12) 0.0005(12) -0.0010(11) F21 0.0468(10) 0.0339(8) 0.0431(9) 0.0103(7) 0.0129(7) -0.0027(7) F22 0.0373(9) 0.0398(8) 0.0339(8) 0.0037(6) -0.0066(7) -0.0058(7) F23 0.0380(9) 0.0374(9) 0.0746(12) 0.0049(8) 0.0163(8) 0.0068(7) F24 0.0543(10) 0.0366(8) 0.0357(8) 0.0001(7) -0.0074(7) -0.0174(7) O1S 0.0654(17) 0.0767(17) 0.0630(15) 0.0062(13) -0.0188(13) 0.0021(14) C1S 0.0359(16) 0.073(2) 0.0347(15) 0.0040(15) 0.0069(13) 0.0146(15) C2S 0.0392(18) 0.074(2) 0.0530(19) 0.0130(17) 0.0109(14) 0.0061(16) C3S 0.053(2) 0.076(2) 0.0386(16) 0.0074(16) 0.0050(15) 0.0153(17) _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 Ru1 C1 1.848(2) . ? Ru1 N4 2.1103(18) . ? Ru1 N12 2.1107(18) . ? Ru1 N1 2.1244(18) . ? Ru1 N7 2.1699(19) . ? Ru1 P1 2.3445(6) . ? C1 O1 1.155(3) . ? N1 C10 1.489(3) . ? N1 C2 1.499(3) . ? N1 C9 1.507(3) . ? C2 C3 1.523(3) . ? C3 N4 1.519(3) . ? N4 C5 1.486(3) . ? C5 C6 1.521(3) . ? C6 N7 1.511(3) . ? N7 C8 1.498(3) . ? C8 C9 1.515(3) . ? C10 C11 1.504(3) . ? C11 N12 1.367(3) . ? C11 C16 1.386(3) . ? N12 C13 1.349(3) . ? C13 C14 1.383(3) . ? C14 C15 1.384(4) . ? C15 C16 1.385(4) . ? P1 C121 1.826(2) . ? P1 C131 1.831(2) . ? P1 C111 1.840(2) . ? C111 C112 1.391(3) . ? C111 C116 1.399(3) . ? C112 C113 1.391(3) . ? C113 C114 1.385(3) . ? C114 C115 1.379(3) . ? C115 C116 1.386(3) . ? C121 C122 1.393(3) . ? C121 C126 1.402(3) . ? C122 C123 1.393(3) . ? C123 C124 1.385(4) . ? C124 C125 1.388(3) . ? C125 C126 1.391(3) . ? C131 C132 1.396(3) . ? C131 C136 1.397(3) . ? C132 C133 1.384(3) . ? C133 C134 1.380(4) . ? C134 C135 1.388(4) . ? C135 C136 1.391(3) . ? B1 F12 1.372(3) . ? B1 F13 1.381(3) . ? B1 F11 1.389(3) . ? B1 F14 1.408(3) . ? B2 F21 1.386(3) . ? B2 F24 1.388(3) . ? B2 F22 1.392(3) . ? B2 F23 1.395(3) . ? O1S C1S 1.226(4) . ? C1S C2S 1.485(5) . ? C1S C3S 1.487(4) . ? 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 C1 Ru1 N4 93.69(9) . . ? C1 Ru1 N12 94.26(8) . . ? N4 Ru1 N12 161.02(7) . . ? C1 Ru1 N1 94.41(9) . . ? N4 Ru1 N1 82.60(7) . . ? N12 Ru1 N1 79.62(7) . . ? C1 Ru1 N7 172.67(8) . . ? N4 Ru1 N7 80.43(7) . . ? N12 Ru1 N7 90.09(7) . . ? N1 Ru1 N7 80.56(7) . . ? C1 Ru1 P1 87.25(7) . . ? N4 Ru1 P1 97.97(5) . . ? N12 Ru1 P1 99.60(5) . . ? N1 Ru1 P1 178.20(5) . . ? N7 Ru1 P1 97.85(5) . . ? O1 C1 Ru1 176.4(2) . . ? C10 N1 C2 113.38(18) . . ? C10 N1 C9 111.31(17) . . ? C2 N1 C9 110.53(17) . . ? C10 N1 Ru1 104.46(13) . . ? C2 N1 Ru1 104.76(13) . . ? C9 N1 Ru1 112.09(14) . . ? N1 C2 C3 109.31(19) . . ? N4 C3 C2 112.03(18) . . ? C5 N4 C3 112.23(17) . . ? C5 N4 Ru1 107.89(13) . . ? C3 N4 Ru1 109.77(13) . . ? N4 C5 C6 110.04(18) . . ? N7 C6 C5 111.20(18) . . ? C8 N7 C6 111.90(17) . . ? C8 N7 Ru1 106.48(14) . . ? C6 N7 Ru1 110.84(13) . . ? N7 C8 C9 109.34(18) . . ? N1 C9 C8 111.53(18) . . ? N1 C10 C11 109.74(19) . . ? N12 C11 C16 121.5(2) . . ? N12 C11 C10 116.2(2) . . ? C16 C11 C10 122.3(2) . . ? C13 N12 C11 118.12(19) . . ? C13 N12 Ru1 129.93(15) . . ? C11 N12 Ru1 111.89(15) . . ? N12 C13 C14 122.6(2) . . ? C13 C14 C15 119.1(2) . . ? C14 C15 C16 119.0(2) . . ? C15 C16 C11 119.6(2) . . ? C121 P1 C131 104.65(10) . . ? C121 P1 C111 104.31(10) . . ? C131 P1 C111 100.01(10) . . ? C121 P1 Ru1 114.30(7) . . ? C131 P1 Ru1 115.87(7) . . ? C111 P1 Ru1 115.92(7) . . ? C112 C111 C116 118.5(2) . . ? C112 C111 P1 121.32(17) . . ? C116 C111 P1 120.16(17) . . ? C111 C112 C113 120.7(2) . . ? C114 C113 C112 120.2(2) . . ? C115 C114 C113 119.4(2) . . ? C114 C115 C116 120.9(2) . . ? C115 C116 C111 120.3(2) . . ? C122 C121 C126 118.6(2) . . ? C122 C121 P1 121.85(18) . . ? C126 C121 P1 119.54(17) . . ? C123 C122 C121 120.3(2) . . ? C124 C123 C122 120.7(2) . . ? C123 C124 C125 119.7(2) . . ? C124 C125 C126 119.9(2) . . ? C125 C126 C121 120.9(2) . . ? C132 C131 C136 118.9(2) . . ? C132 C131 P1 117.91(18) . . ? C136 C131 P1 122.68(18) . . ? C133 C132 C131 120.3(2) . . ? C134 C133 C132 120.6(2) . . ? C133 C134 C135 119.8(2) . . ? C134 C135 C136 120.0(2) . . ? C135 C136 C131 120.3(2) . . ? F12 B1 F13 110.2(2) . . ? F12 B1 F11 109.6(2) . . ? F13 B1 F11 110.0(2) . . ? F12 B1 F14 110.4(2) . . ? F13 B1 F14 109.0(2) . . ? F11 B1 F14 107.7(2) . . ? F21 B2 F24 110.2(2) . . ? F21 B2 F22 110.2(2) . . ? F24 B2 F22 108.7(2) . . ? F21 B2 F23 109.2(2) . . ? F24 B2 F23 109.5(2) . . ? F22 B2 F23 109.0(2) . . ? O1S C1S C2S 122.4(3) . . ? O1S C1S C3S 120.9(3) . . ? C2S C1S C3S 116.6(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.612 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.065 #===END data_alg6 _database_code_depnum_ccdc_archive 'CCDC 685073' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'in paper 9' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H39 B2 F8 N4 O2 P Ru' _chemical_formula_weight 793.31 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' 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.59150(10) _cell_length_b 10.23540(10) _cell_length_c 18.2375(3) _cell_angle_alpha 90.3360(10) _cell_angle_beta 96.8480(11) _cell_angle_gamma 113.4930(10) _cell_volume 1627.50(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.613 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9191 _exptl_absorpt_correction_T_max 0.9301 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 ; 'Nonius KappaCCD area detector diffractometer' ; _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29394 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6362 _reflns_number_gt 5773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+1.0155P] 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 6362 _refine_ls_number_parameters 486 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.277 _refine_ls_shift/su_mean 0.013 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 Ru1 Ru 0.110009(18) 0.141084(17) 0.235398(9) 0.02355(7) Uani 1 1 d . . . N1 N 0.2447(2) 0.35276(19) 0.20953(10) 0.0302(4) Uani 1 1 d . . . C1 C 0.1478(3) 0.4379(3) 0.19963(14) 0.0364(5) Uani 1 1 d . . . H1A H 0.1247 0.4490 0.1462 0.044 Uiso 1 1 calc R . . H1B H 0.2061 0.5343 0.2240 0.044 Uiso 1 1 calc R . . C2 C -0.0016(3) 0.3668(2) 0.23203(14) 0.0346(5) Uani 1 1 d . . . H2A H 0.0175 0.3848 0.2864 0.041 Uiso 1 1 calc R . . H2B H -0.0752 0.4075 0.2119 0.041 Uiso 1 1 calc R . . N2 N -0.0683(2) 0.2092(2) 0.21300(10) 0.0303(4) Uani 1 1 d . . . H2 H -0.1429 0.1639 0.2433 0.036 Uiso 1 1 calc R . . C3 C -0.1403(3) 0.1749(3) 0.13341(13) 0.0370(5) Uani 1 1 d . . . H3A H -0.1101 0.2641 0.1068 0.044 Uiso 1 1 calc R . . H3B H -0.2533 0.1334 0.1312 0.044 Uiso 1 1 calc R . . C4 C -0.0916(3) 0.0701(3) 0.09493(13) 0.0367(5) Uani 1 1 d . . . H4A H -0.1535 -0.0283 0.1076 0.044 Uiso 1 1 calc R . . H4B H -0.1097 0.0751 0.0406 0.044 Uiso 1 1 calc R . . N3 N 0.0745(2) 0.1061(2) 0.11891(10) 0.0319(4) Uani 1 1 d . . . H3 H 0.0974 0.0294 0.1063 0.038 Uiso 1 1 calc R . . C5 C 0.1757(3) 0.2374(3) 0.08413(13) 0.0393(6) Uani 1 1 d . . . H5A H 0.1133 0.2884 0.0626 0.047 Uiso 1 1 calc R . . H5B H 0.2193 0.2086 0.0435 0.047 Uiso 1 1 calc R . . C6 C 0.3059(3) 0.3376(3) 0.14024(14) 0.0376(5) Uani 1 1 d . . . H6A H 0.3853 0.2989 0.1510 0.045 Uiso 1 1 calc R . . H6B H 0.3539 0.4322 0.1197 0.045 Uiso 1 1 calc R . . C7 C 0.3670(3) 0.4104(2) 0.27382(14) 0.0352(5) Uani 1 1 d . . . H7A H 0.4181 0.5155 0.2729 0.042 Uiso 1 1 calc R . . H7B H 0.4450 0.3706 0.2711 0.042 Uiso 1 1 calc R . . C8 C 0.2968(3) 0.3706(2) 0.34432(13) 0.0317(5) Uani 1 1 d . . . N9 N 0.1729(2) 0.24283(19) 0.34034(10) 0.0281(4) Uani 1 1 d . . . C10 C 0.0981(3) 0.2079(3) 0.40034(12) 0.0310(5) Uani 1 1 d . . . H10 H 0.0088 0.1217 0.3976 0.037 Uiso 1 1 calc R . . C11 C 0.1460(3) 0.2922(3) 0.46529(13) 0.0383(5) Uani 1 1 d . . . H11 H 0.0897 0.2644 0.5061 0.046 Uiso 1 1 calc R . . C12 C 0.2764(3) 0.4176(3) 0.47051(14) 0.0435(6) Uani 1 1 d . . . H12 H 0.3141 0.4749 0.5155 0.052 Uiso 1 1 calc R . . C13 C 0.3507(3) 0.4574(3) 0.40863(15) 0.0410(6) Uani 1 1 d . . . H13 H 0.4389 0.5445 0.4104 0.049 Uiso 1 1 calc R . . P1 P -0.03221(6) -0.08846(6) 0.26497(3) 0.02422(12) Uani 1 1 d . . . C111 C -0.0782(2) -0.2274(2) 0.19052(12) 0.0279(4) Uani 1 1 d . . . C112 C 0.0435(3) -0.2262(2) 0.15507(13) 0.0321(5) Uani 1 1 d . . . H112 H 0.1438 -0.1557 0.1701 0.039 Uiso 1 1 calc R . . C113 C 0.0204(3) -0.3264(3) 0.09805(13) 0.0375(5) Uani 1 1 d . . . H113 H 0.1044 -0.3240 0.0745 0.045 Uiso 1 1 calc R . . C114 C -0.1250(3) -0.4295(3) 0.07575(13) 0.0395(6) Uani 1 1 d . . . H114 H -0.1412 -0.4977 0.0366 0.047 Uiso 1 1 calc R . . C115 C -0.2463(3) -0.4332(3) 0.11054(16) 0.0491(7) Uani 1 1 d . . . H115 H -0.3460 -0.5045 0.0955 0.059 Uiso 1 1 calc R . . C116 C -0.2236(3) -0.3331(3) 0.16756(15) 0.0428(6) Uani 1 1 d . . . H116 H -0.3081 -0.3369 0.1911 0.051 Uiso 1 1 calc R . . C121 C 0.0548(2) -0.1639(2) 0.33996(11) 0.0270(4) Uani 1 1 d . . . C122 C -0.0030(3) -0.3117(2) 0.34710(12) 0.0315(5) Uani 1 1 d . . . H122 H -0.0860 -0.3732 0.3126 0.038 Uiso 1 1 calc R . . C123 C 0.0595(3) -0.3691(3) 0.40399(13) 0.0359(5) Uani 1 1 d . . . H123 H 0.0211 -0.4697 0.4073 0.043 Uiso 1 1 calc R . . C124 C 0.1777(3) -0.2807(3) 0.45604(13) 0.0360(5) Uani 1 1 d . . . H124 H 0.2186 -0.3201 0.4957 0.043 Uiso 1 1 calc R . . C125 C 0.2356(3) -0.1346(3) 0.44978(13) 0.0344(5) Uani 1 1 d . . . H125 H 0.3164 -0.0735 0.4854 0.041 Uiso 1 1 calc R . . C126 C 0.1759(2) -0.0763(2) 0.39151(12) 0.0292(4) Uani 1 1 d . . . H126 H 0.2184 0.0240 0.3870 0.035 Uiso 1 1 calc R . . C131 C -0.2202(2) -0.1208(2) 0.29328(12) 0.0285(4) Uani 1 1 d . . . C132 C -0.3361(3) -0.1155(3) 0.24091(14) 0.0356(5) Uani 1 1 d . . . H132 H -0.3166 -0.0959 0.1914 0.043 Uiso 1 1 calc R . . C133 C -0.4796(3) -0.1384(3) 0.25999(15) 0.0417(6) Uani 1 1 d . . . H133 H -0.5584 -0.1376 0.2233 0.050 Uiso 1 1 calc R . . C134 C -0.5077(3) -0.1623(3) 0.33211(16) 0.0434(6) Uani 1 1 d . . . H134 H -0.6057 -0.1778 0.3453 0.052 Uiso 1 1 calc R . . C135 C -0.3932(3) -0.1637(3) 0.38514(14) 0.0397(6) Uani 1 1 d . . . H135 H -0.4120 -0.1778 0.4351 0.048 Uiso 1 1 calc R . . C136 C -0.2502(3) -0.1446(2) 0.36597(13) 0.0328(5) Uani 1 1 d . . . H136 H -0.1728 -0.1478 0.4027 0.039 Uiso 1 1 calc R . . O1 O 0.30555(19) 0.08232(18) 0.24493(12) 0.0301(3) Uani 1 1 d . . . H1A H 0.365(3) 0.107(3) 0.2761(16) 0.031(8) Uiso 1 1 d . . . H1B H 0.339(4) 0.081(3) 0.2087(18) 0.046(9) Uiso 1 1 d . . . O2 O 0.3651(3) 0.0445(3) 0.10693(13) 0.0576(6) Uani 1 1 d . . . H2A H 0.416(5) 0.111(5) 0.084(2) 0.085(14) Uiso 1 1 d . . . H2B H 0.384(5) -0.013(5) 0.094(2) 0.075(13) Uiso 1 1 d . . . B1 B 0.6673(3) 0.2687(3) 0.33631(16) 0.0374(6) Uani 1 1 d . . . F1 F 0.7039(2) 0.40446(18) 0.36579(11) 0.0649(5) Uani 1 1 d . . . F2 F 0.64196(17) 0.2652(2) 0.25982(8) 0.0549(4) Uani 1 1 d . . . F3 F 0.53078(16) 0.17798(16) 0.36177(8) 0.0445(3) Uani 1 1 d . . . F4 F 0.78331(18) 0.2243(2) 0.35784(10) 0.0579(4) Uani 1 1 d . . . B2 B 0.5520(3) 0.2424(3) -0.03595(16) 0.0396(6) Uani 1 1 d DU . . F5A F 0.4543(7) 0.1137(4) -0.0706(4) 0.0713(15) Uani 0.777(7) 1 d PDU A 1 F6A F 0.6812(3) 0.2182(3) -0.0105(2) 0.0801(12) Uani 0.777(7) 1 d PDU A 1 F7A F 0.4944(5) 0.2770(3) 0.0192(3) 0.113(2) Uani 0.777(7) 1 d PDU A 1 F8A F 0.5979(5) 0.3467(4) -0.0836(3) 0.0853(13) Uani 0.777(7) 1 d PDU A 1 F5B F 0.5934(14) 0.2437(8) 0.0381(5) 0.083(6) Uani 0.223(7) 1 d PDU A 2 F6B F 0.488(3) 0.3459(19) -0.0375(9) 0.156(8) Uani 0.223(7) 1 d PDU A 2 F7B F 0.423(2) 0.130(2) -0.0602(14) 0.109(8) Uani 0.223(7) 1 d PDU A 2 F8B F 0.638(2) 0.308(3) -0.0832(11) 0.203(12) Uani 0.223(7) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02273(10) 0.02338(10) 0.02560(10) 0.00360(7) 0.00455(7) 0.00998(7) N1 0.0303(10) 0.0265(9) 0.0370(10) 0.0074(8) 0.0094(8) 0.0133(8) C1 0.0383(13) 0.0285(12) 0.0460(14) 0.0086(10) 0.0079(10) 0.0165(10) C2 0.0359(12) 0.0302(12) 0.0441(13) 0.0054(10) 0.0058(10) 0.0199(10) N2 0.0287(9) 0.0307(10) 0.0332(10) 0.0059(8) 0.0048(8) 0.0134(8) C3 0.0339(12) 0.0414(14) 0.0379(13) 0.0077(10) -0.0012(10) 0.0192(11) C4 0.0378(13) 0.0427(14) 0.0280(11) 0.0043(10) -0.0021(9) 0.0164(11) N3 0.0339(10) 0.0345(10) 0.0304(10) 0.0075(8) 0.0064(8) 0.0162(8) C5 0.0454(14) 0.0429(14) 0.0347(13) 0.0148(10) 0.0146(11) 0.0203(12) C6 0.0373(13) 0.0342(13) 0.0437(14) 0.0137(10) 0.0164(10) 0.0136(10) C7 0.0275(11) 0.0246(11) 0.0504(14) 0.0034(10) 0.0052(10) 0.0072(9) C8 0.0292(11) 0.0257(11) 0.0411(13) 0.0010(9) 0.0006(9) 0.0130(9) N9 0.0271(9) 0.0268(9) 0.0334(10) 0.0017(7) 0.0033(7) 0.0141(8) C10 0.0326(12) 0.0350(12) 0.0315(11) 0.0031(9) 0.0048(9) 0.0197(10) C11 0.0468(14) 0.0495(15) 0.0305(12) -0.0003(10) 0.0012(10) 0.0330(13) C12 0.0542(16) 0.0449(15) 0.0383(14) -0.0109(11) -0.0109(12) 0.0320(13) C13 0.0396(13) 0.0306(13) 0.0513(15) -0.0074(11) -0.0090(11) 0.0168(11) P1 0.0233(3) 0.0234(3) 0.0262(3) 0.0026(2) 0.0043(2) 0.0093(2) C111 0.0300(11) 0.0258(11) 0.0281(11) 0.0019(8) 0.0022(8) 0.0118(9) C112 0.0318(12) 0.0293(11) 0.0363(12) 0.0014(9) 0.0047(9) 0.0134(9) C113 0.0480(14) 0.0348(13) 0.0373(13) 0.0036(10) 0.0106(11) 0.0231(11) C114 0.0536(15) 0.0323(13) 0.0322(12) -0.0028(10) 0.0006(11) 0.0183(11) C115 0.0418(15) 0.0417(15) 0.0518(16) -0.0148(12) 0.0000(12) 0.0061(12) C116 0.0329(13) 0.0405(14) 0.0488(15) -0.0080(11) 0.0094(11) 0.0075(11) C121 0.0277(11) 0.0293(11) 0.0275(11) 0.0025(8) 0.0060(8) 0.0146(9) C122 0.0361(12) 0.0293(11) 0.0308(11) 0.0029(9) 0.0053(9) 0.0146(10) C123 0.0465(14) 0.0304(12) 0.0377(13) 0.0076(10) 0.0116(10) 0.0210(11) C124 0.0462(14) 0.0419(14) 0.0312(12) 0.0077(10) 0.0084(10) 0.0288(12) C125 0.0359(12) 0.0414(13) 0.0302(12) -0.0004(10) 0.0015(9) 0.0209(11) C126 0.0306(11) 0.0276(11) 0.0326(11) 0.0017(9) 0.0049(9) 0.0148(9) C131 0.0271(11) 0.0239(11) 0.0357(12) 0.0042(9) 0.0077(9) 0.0104(9) C132 0.0306(12) 0.0376(13) 0.0409(13) 0.0089(10) 0.0081(10) 0.0150(10) C133 0.0288(12) 0.0425(14) 0.0575(16) 0.0081(12) 0.0079(11) 0.0177(11) C134 0.0338(13) 0.0343(13) 0.0677(18) 0.0045(12) 0.0213(12) 0.0156(11) C135 0.0452(14) 0.0307(12) 0.0463(14) 0.0047(10) 0.0230(12) 0.0140(11) C136 0.0379(12) 0.0275(11) 0.0346(12) 0.0026(9) 0.0095(10) 0.0135(10) O1 0.0265(9) 0.0342(9) 0.0319(9) 0.0020(7) 0.0049(8) 0.0143(7) O2 0.0764(16) 0.0575(14) 0.0544(13) 0.0075(11) 0.0313(11) 0.0368(13) B1 0.0282(13) 0.0417(16) 0.0389(15) 0.0015(12) 0.0027(11) 0.0111(12) F1 0.0624(11) 0.0407(9) 0.0800(13) -0.0100(8) 0.0081(9) 0.0090(8) F2 0.0390(8) 0.0815(12) 0.0403(8) 0.0074(8) 0.0061(7) 0.0198(8) F3 0.0319(7) 0.0499(9) 0.0457(8) 0.0048(7) 0.0063(6) 0.0097(6) F4 0.0407(9) 0.0811(12) 0.0605(10) 0.0120(9) 0.0056(7) 0.0338(9) B2 0.0361(14) 0.0356(15) 0.0424(15) 0.0003(12) 0.0036(12) 0.0102(12) F5A 0.085(3) 0.0374(15) 0.069(3) -0.0090(16) -0.026(2) 0.0120(18) F6A 0.0400(13) 0.095(2) 0.105(3) 0.0369(17) 0.0042(13) 0.0272(13) F7A 0.132(3) 0.0515(17) 0.154(5) -0.017(2) 0.111(4) 0.0087(19) F8A 0.111(3) 0.0462(16) 0.106(3) 0.0427(17) 0.031(2) 0.0337(17) F5B 0.105(10) 0.027(4) 0.066(6) 0.004(4) -0.069(7) -0.005(5) F6B 0.27(2) 0.175(13) 0.112(11) 0.015(10) 0.001(12) 0.186(15) F7B 0.063(9) 0.108(10) 0.069(10) 0.028(10) -0.039(8) -0.043(8) F8B 0.103(13) 0.28(3) 0.126(12) -0.045(13) 0.097(12) -0.048(12) _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 Ru1 N9 2.0764(18) . ? Ru1 N2 2.0897(18) . ? Ru1 N3 2.1163(19) . ? Ru1 N1 2.1240(18) . ? Ru1 O1 2.1754(16) . ? Ru1 P1 2.3036(5) . ? N1 C7 1.487(3) . ? N1 C6 1.488(3) . ? N1 C1 1.505(3) . ? C1 C2 1.519(3) . ? C2 N2 1.500(3) . ? N2 C3 1.506(3) . ? C3 C4 1.526(3) . ? C4 N3 1.492(3) . ? N3 C5 1.506(3) . ? C5 C6 1.523(4) . ? C7 C8 1.505(3) . ? C8 N9 1.367(3) . ? C8 C13 1.382(3) . ? N9 C10 1.352(3) . ? C10 C11 1.379(3) . ? C11 C12 1.382(4) . ? C12 C13 1.383(4) . ? P1 C131 1.837(2) . ? P1 C111 1.843(2) . ? P1 C121 1.849(2) . ? C111 C116 1.394(3) . ? C111 C112 1.396(3) . ? C112 C113 1.391(3) . ? C113 C114 1.382(4) . ? C114 C115 1.378(4) . ? C115 C116 1.391(4) . ? C121 C126 1.392(3) . ? C121 C122 1.401(3) . ? C122 C123 1.386(3) . ? C123 C124 1.386(4) . ? C124 C125 1.383(3) . ? C125 C126 1.395(3) . ? C131 C136 1.393(3) . ? C131 C132 1.395(3) . ? C132 C133 1.388(3) . ? C133 C134 1.378(4) . ? C134 C135 1.378(4) . ? C135 C136 1.394(3) . ? B1 F4 1.378(3) . ? B1 F1 1.379(3) . ? B1 F2 1.385(3) . ? B1 F3 1.404(3) . ? B2 F8B 1.267(12) . ? B2 F7A 1.314(4) . ? B2 F7B 1.336(14) . ? B2 F8A 1.347(4) . ? B2 F5B 1.360(8) . ? B2 F5A 1.370(5) . ? B2 F6A 1.387(4) . ? B2 F6B 1.421(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 N9 Ru1 N2 91.73(7) . . ? N9 Ru1 N3 161.58(7) . . ? N2 Ru1 N3 82.07(7) . . ? N9 Ru1 N1 79.64(7) . . ? N2 Ru1 N1 82.41(7) . . ? N3 Ru1 N1 82.35(7) . . ? N9 Ru1 O1 92.93(7) . . ? N2 Ru1 O1 172.34(7) . . ? N3 Ru1 O1 91.65(8) . . ? N1 Ru1 O1 92.45(7) . . ? N9 Ru1 P1 99.76(5) . . ? N2 Ru1 P1 98.52(5) . . ? N3 Ru1 P1 98.31(5) . . ? N1 Ru1 P1 178.92(5) . . ? O1 Ru1 P1 86.68(5) . . ? C7 N1 C6 112.61(18) . . ? C7 N1 C1 111.69(18) . . ? C6 N1 C1 111.91(18) . . ? C7 N1 Ru1 104.59(13) . . ? C6 N1 Ru1 105.32(13) . . ? C1 N1 Ru1 110.26(13) . . ? N1 C1 C2 111.84(18) . . ? N2 C2 C1 109.70(18) . . ? C2 N2 C3 111.41(17) . . ? C2 N2 Ru1 107.00(13) . . ? C3 N2 Ru1 111.55(14) . . ? N2 C3 C4 111.86(18) . . ? N3 C4 C3 109.69(19) . . ? C4 N3 C5 111.84(18) . . ? C4 N3 Ru1 106.56(14) . . ? C5 N3 Ru1 110.03(15) . . ? N3 C5 C6 111.70(18) . . ? N1 C6 C5 109.52(19) . . ? N1 C7 C8 109.29(18) . . ? N9 C8 C13 121.7(2) . . ? N9 C8 C7 115.36(19) . . ? C13 C8 C7 123.0(2) . . ? C10 N9 C8 117.54(19) . . ? C10 N9 Ru1 128.71(15) . . ? C8 N9 Ru1 113.22(14) . . ? N9 C10 C11 122.8(2) . . ? C10 C11 C12 119.5(2) . . ? C11 C12 C13 118.4(2) . . ? C8 C13 C12 120.0(2) . . ? C131 P1 C111 103.29(10) . . ? C131 P1 C121 102.60(10) . . ? C111 P1 C121 99.74(10) . . ? C131 P1 Ru1 115.99(7) . . ? C111 P1 Ru1 115.36(7) . . ? C121 P1 Ru1 117.49(7) . . ? C116 C111 C112 118.0(2) . . ? C116 C111 P1 125.25(17) . . ? C112 C111 P1 116.75(17) . . ? C113 C112 C111 121.1(2) . . ? C114 C113 C112 120.0(2) . . ? C115 C114 C113 119.8(2) . . ? C114 C115 C116 120.4(2) . . ? C115 C116 C111 120.7(2) . . ? C126 C121 C122 118.4(2) . . ? C126 C121 P1 121.27(16) . . ? C122 C121 P1 120.28(16) . . ? C123 C122 C121 120.7(2) . . ? C122 C123 C124 120.4(2) . . ? C125 C124 C123 119.5(2) . . ? C124 C125 C126 120.4(2) . . ? C121 C126 C125 120.5(2) . . ? C136 C131 C132 118.2(2) . . ? C136 C131 P1 122.58(17) . . ? C132 C131 P1 119.12(17) . . ? C133 C132 C131 121.0(2) . . ? C134 C133 C132 120.0(2) . . ? C133 C134 C135 119.9(2) . . ? C134 C135 C136 120.4(2) . . ? C131 C136 C135 120.4(2) . . ? F4 B1 F1 110.7(2) . . ? F4 B1 F2 109.5(2) . . ? F1 B1 F2 110.2(2) . . ? F4 B1 F3 110.4(2) . . ? F1 B1 F3 107.5(2) . . ? F2 B1 F3 108.5(2) . . ? F8B B2 F7A 136.7(13) . . ? F8B B2 F7B 117.8(16) . . ? F7A B2 F7B 93.9(13) . . ? F8B B2 F8A 28.6(14) . . ? F7A B2 F8A 112.7(3) . . ? F7B B2 F8A 115.3(12) . . ? F8B B2 F5B 126.9(12) . . ? F7A B2 F5B 50.8(6) . . ? F7B B2 F5B 112.2(12) . . ? F8A B2 F5B 130.7(4) . . ? F8B B2 F5A 105.5(12) . . ? F7A B2 F5A 111.6(4) . . ? F7B B2 F5A 19.4(14) . . ? F8A B2 F5A 112.5(4) . . ? F5B B2 F5A 116.7(5) . . ? F8B B2 F6A 80.7(14) . . ? F7A B2 F6A 110.9(4) . . ? F7B B2 F6A 118.2(12) . . ? F8A B2 F6A 105.7(3) . . ? F5B B2 F6A 60.4(6) . . ? F5A B2 F6A 102.8(3) . . ? F8B B2 F6B 90.4(14) . . ? F7A B2 F6B 55.0(7) . . ? F7B B2 F6B 97.1(13) . . ? F8A B2 F6B 61.9(9) . . ? F5B B2 F6B 100.2(8) . . ? F5A B2 F6B 113.4(9) . . ? F6A B2 F6B 143.7(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 F4 0.93 2.44 3.177(3) 136.7 1_455 N3 H3 O2 0.93 2.51 3.125(3) 123.9 . O1 H1A F3 0.72(3) 1.99(3) 2.712(2) 179(3) . O1 H1A F2 0.72(3) 2.56(3) 2.993(2) 121(3) . O1 H1B O2 0.77(3) 1.96(3) 2.705(3) 164(3) . O2 H2A F5B 0.81(4) 1.99(5) 2.767(12) 159(4) . O2 H2A F7A 0.81(4) 2.02(5) 2.815(5) 167(4) . O2 H2B F5A 0.73(4) 2.25(4) 2.925(6) 154(4) 2_655 O2 H2B F6A 0.73(4) 2.40(4) 3.054(5) 149(4) 2_655 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.393 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.062