Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof John Nelson' _publ_contact_author_address ; Department of Chemistry University of Nevada - Reno Reno Nevada 89557-0020 USA ; _publ_contact_author_email JHNELSON@UNR.EDU _publ_section_title ; Phosphaallyl Complexes of Ru(II) Derived from Dicyclohexylvinylphosphine (DCVP) ; loop_ _publ_author_name 'John Nelson' 'Dorota Duraczynska' data_jhn562a _database_code_depnum_ccdc_archive 'CCDC 248575' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H55 F6 P3 Ru' _chemical_formula_weight 759.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.6206(4) _cell_length_b 23.1706(10) _cell_length_c 15.5767(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.2030(10) _cell_angle_gamma 90.00 _cell_volume 3458.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7683 _exptl_absorpt_correction_T_max 0.7819 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28448 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 29.99 _reflns_number_total 9568 _reflns_number_gt 8181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1350P)^2^+0.0000P] 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 9568 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1732 _refine_ls_wR_factor_gt 0.1595 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.913270(19) 0.106319(7) 0.797967(11) 0.01255(9) Uani 1 1 d . . . P1 P 0.75571(6) 0.15036(2) 0.87901(4) 0.01431(14) Uani 1 1 d . . . P2 P 0.78784(7) 0.11075(2) 0.66184(4) 0.01319(14) Uani 1 1 d . . . C1 C 1.0210(3) 0.02792(10) 0.75447(17) 0.0212(5) Uani 1 1 d . . . H1A H 1.0071 0.0111 0.6952 0.025 Uiso 1 1 calc R . . C2 C 0.9448(3) 0.01222(10) 0.82395(19) 0.0252(6) Uani 1 1 d . . . H2A H 0.8702 -0.0179 0.8232 0.030 Uiso 1 1 calc R . . C3 C 1.0004(3) 0.04504(11) 0.89750(17) 0.0218(5) Uani 1 1 d . . . H3A H 0.9719 0.0416 0.9574 0.026 Uiso 1 1 calc R . . C4 C 1.1111(3) 0.07948(11) 0.87161(17) 0.0209(5) Uani 1 1 d . . . H4A H 1.1728 0.1050 0.9103 0.025 Uiso 1 1 calc R . . C5 C 1.1254(3) 0.06924(11) 0.78217(17) 0.0197(5) Uani 1 1 d . . . H5A H 1.1981 0.0857 0.7472 0.024 Uiso 1 1 calc R . . C6 C 0.9148(3) 0.18713(9) 0.86863(16) 0.0168(5) Uani 1 1 d . . . H6A H 0.9833 0.1942 0.9197 0.020 Uiso 1 1 calc R . . C7 C 0.9455(3) 0.20213(10) 0.78493(16) 0.0180(5) Uani 1 1 d . . . H7A H 1.0418 0.2153 0.7782 0.022 Uiso 1 1 calc R . . H7B H 0.8728 0.2237 0.7490 0.022 Uiso 1 1 calc R . . C8 C 0.7572(3) 0.12893(11) 0.99268(15) 0.0193(5) Uani 1 1 d . . . H8A H 0.8555 0.1168 1.0100 0.023 Uiso 1 1 calc R . . C9 C 0.7278(3) 0.17745(11) 1.05480(17) 0.0249(6) Uani 1 1 d . . . H9A H 0.7880 0.2111 1.0452 0.030 Uiso 1 1 calc R . . H9B H 0.6292 0.1898 1.0443 0.030 Uiso 1 1 calc R . . C10 C 0.7567(3) 0.15618(12) 1.14741(17) 0.0240(5) Uani 1 1 d . . . H10A H 0.7343 0.1872 1.1876 0.029 Uiso 1 1 calc R . . H10B H 0.8571 0.1469 1.1589 0.029 Uiso 1 1 calc R . . C11 C 0.6700(4) 0.10267(12) 1.1635(2) 0.0292(7) Uani 1 1 d . . . H11A H 0.6954 0.0885 1.2228 0.035 Uiso 1 1 calc R . . H11B H 0.5698 0.1131 1.1586 0.035 Uiso 1 1 calc R . . C12 C 0.6935(3) 0.05504(12) 1.09975(18) 0.0279(6) Uani 1 1 d . . . H12A H 0.6302 0.0224 1.1093 0.033 Uiso 1 1 calc R . . H12B H 0.7906 0.0409 1.1104 0.033 Uiso 1 1 calc R . . C13 C 0.6680(3) 0.07505(11) 1.00565(16) 0.0202(5) Uani 1 1 d . . . H13A H 0.5680 0.0843 0.9919 0.024 Uiso 1 1 calc R . . H13B H 0.6934 0.0439 0.9666 0.024 Uiso 1 1 calc R . . C14 C 0.6031(3) 0.19352(10) 0.84114(15) 0.0156(4) Uani 1 1 d . . . H14A H 0.5998 0.1943 0.7768 0.019 Uiso 1 1 calc R . . C15 C 0.6130(3) 0.25682(10) 0.87129(17) 0.0205(5) Uani 1 1 d . . . H15A H 0.6148 0.2584 0.9349 0.025 Uiso 1 1 calc R . . H15B H 0.7006 0.2742 0.8544 0.025 Uiso 1 1 calc R . . C16 C 0.4879(3) 0.29108(11) 0.8306(2) 0.0267(6) Uani 1 1 d . . . H16A H 0.4921 0.3309 0.8539 0.032 Uiso 1 1 calc R . . H16B H 0.4937 0.2935 0.7676 0.032 Uiso 1 1 calc R . . C17 C 0.3508(3) 0.26426(12) 0.8477(2) 0.0280(6) Uani 1 1 d . . . H17A H 0.2737 0.2861 0.8163 0.034 Uiso 1 1 calc R . . H17B H 0.3389 0.2667 0.9101 0.034 Uiso 1 1 calc R . . C18 C 0.3428(3) 0.20126(12) 0.8193(2) 0.0265(6) Uani 1 1 d . . . H18A H 0.3450 0.1990 0.7560 0.032 Uiso 1 1 calc R . . H18B H 0.2536 0.1843 0.8342 0.032 Uiso 1 1 calc R . . C19 C 0.4648(3) 0.16666(10) 0.86335(18) 0.0207(5) Uani 1 1 d . . . H19A H 0.4592 0.1261 0.8435 0.025 Uiso 1 1 calc R . . H19B H 0.4602 0.1670 0.9266 0.025 Uiso 1 1 calc R . . C20 C 0.6847(3) 0.17458(10) 0.62864(15) 0.0177(5) Uani 1 1 d . . . H20A H 0.7320 0.2105 0.6355 0.021 Uiso 1 1 calc R . . C21 C 0.5520(3) 0.17732(11) 0.59607(18) 0.0241(5) Uani 1 1 d . . . H21A H 0.4987 0.1429 0.5875 0.029 Uiso 1 1 calc R . . H21B H 0.5106 0.2136 0.5814 0.029 Uiso 1 1 calc R . . C22 C 0.9039(3) 0.10735(9) 0.57271(17) 0.0172(5) Uani 1 1 d . . . H22A H 0.9591 0.0709 0.5813 0.021 Uiso 1 1 calc R . . C23 C 1.0102(3) 0.15706(11) 0.57692(17) 0.0228(5) Uani 1 1 d . . . H23A H 0.9602 0.1943 0.5683 0.027 Uiso 1 1 calc R . . H23B H 1.0626 0.1578 0.6346 0.027 Uiso 1 1 calc R . . C24 C 1.1121(3) 0.14997(14) 0.5080(2) 0.0301(6) Uani 1 1 d . . . H24A H 1.1683 0.1146 0.5200 0.036 Uiso 1 1 calc R . . H24B H 1.1766 0.1833 0.5103 0.036 Uiso 1 1 calc R . . C25 C 1.0356(3) 0.14579(14) 0.41748(19) 0.0305(6) Uani 1 1 d . . . H25A H 0.9882 0.1828 0.4026 0.037 Uiso 1 1 calc R . . H25B H 1.1040 0.1386 0.3749 0.037 Uiso 1 1 calc R . . C26 C 0.9283(3) 0.09725(13) 0.41300(18) 0.0262(6) Uani 1 1 d . . . H26A H 0.9772 0.0597 0.4206 0.031 Uiso 1 1 calc R . . H26B H 0.8756 0.0973 0.3554 0.031 Uiso 1 1 calc R . . C27 C 0.8263(3) 0.10368(11) 0.48215(17) 0.0210(5) Uani 1 1 d . . . H27A H 0.7621 0.0702 0.4794 0.025 Uiso 1 1 calc R . . H27B H 0.7698 0.1390 0.4708 0.025 Uiso 1 1 calc R . . C28 C 0.6590(2) 0.05256(10) 0.63666(15) 0.0150(4) Uani 1 1 d . . . H28A H 0.6061 0.0628 0.5805 0.018 Uiso 1 1 calc R . . C29 C 0.5527(3) 0.05009(11) 0.70401(16) 0.0188(5) Uani 1 1 d . . . H29A H 0.5123 0.0889 0.7110 0.023 Uiso 1 1 calc R . . H29B H 0.6000 0.0381 0.7603 0.023 Uiso 1 1 calc R . . C30 C 0.4358(3) 0.00723(10) 0.67620(17) 0.0195(5) Uani 1 1 d . . . H30A H 0.3700 0.0048 0.7214 0.023 Uiso 1 1 calc R . . H30B H 0.3835 0.0209 0.6224 0.023 Uiso 1 1 calc R . . C31 C 0.4967(3) -0.05245(10) 0.66144(17) 0.0203(5) Uani 1 1 d . . . H31A H 0.5392 -0.0679 0.7170 0.024 Uiso 1 1 calc R . . H31B H 0.4205 -0.0789 0.6399 0.024 Uiso 1 1 calc R . . C32 C 0.6065(3) -0.05082(10) 0.59717(17) 0.0186(5) Uani 1 1 d . . . H32A H 0.5620 -0.0398 0.5397 0.022 Uiso 1 1 calc R . . H32B H 0.6475 -0.0897 0.5923 0.022 Uiso 1 1 calc R . . C33 C 0.7223(3) -0.00762(10) 0.62523(16) 0.0181(5) Uani 1 1 d . . . H33A H 0.7902 -0.0059 0.5812 0.022 Uiso 1 1 calc R . . H33B H 0.7724 -0.0204 0.6803 0.022 Uiso 1 1 calc R . . P3 P 0.22398(8) 0.15897(3) 0.10264(5) 0.02370(17) Uani 1 1 d . . . F1 F 0.1300(3) 0.20282(10) 0.14894(16) 0.0557(6) Uani 1 1 d . . . F2 F 0.3562(3) 0.19974(11) 0.12279(15) 0.0571(7) Uani 1 1 d . . . F3 F 0.3180(3) 0.11424(11) 0.05351(16) 0.0553(7) Uani 1 1 d . . . F4 F 0.0924(2) 0.11733(9) 0.07988(14) 0.0392(5) Uani 1 1 d . . . F5 F 0.2614(3) 0.12582(10) 0.19065(13) 0.0467(5) Uani 1 1 d . . . F6 F 0.1874(3) 0.19159(10) 0.01257(13) 0.0481(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01061(14) 0.01538(12) 0.01087(13) -0.00022(5) -0.00340(9) 0.00144(5) P1 0.0140(3) 0.0178(3) 0.0107(3) -0.0011(2) -0.0017(2) 0.0016(2) P2 0.0118(3) 0.0162(3) 0.0110(3) -0.00064(18) -0.0019(2) 0.00069(19) C1 0.0214(13) 0.0192(10) 0.0213(12) -0.0041(9) -0.0070(10) 0.0074(9) C2 0.0219(13) 0.0163(10) 0.0357(15) 0.0053(10) -0.0076(12) 0.0037(9) C3 0.0219(13) 0.0281(11) 0.0154(11) 0.0070(9) 0.0019(10) 0.0102(10) C4 0.0131(11) 0.0293(12) 0.0190(12) -0.0033(9) -0.0062(9) 0.0068(9) C5 0.0136(11) 0.0237(10) 0.0217(12) -0.0016(9) 0.0008(9) 0.0066(9) C6 0.0132(11) 0.0169(9) 0.0192(11) -0.0030(8) -0.0047(9) -0.0003(8) C7 0.0150(11) 0.0177(10) 0.0201(11) -0.0008(9) -0.0041(9) -0.0017(8) C8 0.0190(12) 0.0256(11) 0.0131(10) 0.0014(9) 0.0003(9) 0.0015(9) C9 0.0326(15) 0.0258(12) 0.0155(11) -0.0004(9) -0.0018(11) -0.0016(11) C10 0.0273(14) 0.0335(13) 0.0111(11) -0.0016(9) 0.0009(10) -0.0010(11) C11 0.0316(17) 0.0372(15) 0.0181(13) 0.0065(10) -0.0012(12) 0.0012(11) C12 0.0335(16) 0.0276(12) 0.0223(13) 0.0089(10) 0.0017(12) 0.0029(11) C13 0.0202(12) 0.0225(10) 0.0176(11) 0.0016(9) 0.0004(10) 0.0015(9) C14 0.0145(11) 0.0191(9) 0.0129(10) -0.0012(8) -0.0008(8) 0.0014(8) C15 0.0218(13) 0.0186(10) 0.0200(12) -0.0011(9) -0.0040(10) 0.0022(9) C16 0.0254(14) 0.0216(11) 0.0323(14) 0.0055(10) -0.0023(12) 0.0052(10) C17 0.0226(14) 0.0279(12) 0.0338(15) 0.0047(11) 0.0041(12) 0.0111(11) C18 0.0132(12) 0.0297(12) 0.0358(15) 0.0022(11) -0.0014(11) 0.0028(10) C19 0.0139(11) 0.0218(10) 0.0264(13) -0.0010(9) 0.0013(10) 0.0007(9) C20 0.0204(12) 0.0187(9) 0.0132(10) 0.0016(8) -0.0020(9) 0.0021(9) C21 0.0212(13) 0.0262(11) 0.0241(13) 0.0045(10) -0.0018(11) 0.0049(10) C22 0.0170(13) 0.0192(10) 0.0146(12) 0.0000(7) -0.0024(10) -0.0002(8) C23 0.0221(13) 0.0290(12) 0.0180(12) -0.0027(9) 0.0058(10) -0.0080(10) C24 0.0259(15) 0.0384(15) 0.0271(14) -0.0016(12) 0.0075(12) -0.0088(12) C25 0.0313(16) 0.0409(15) 0.0209(13) 0.0035(11) 0.0115(12) -0.0017(12) C26 0.0255(15) 0.0387(13) 0.0148(12) -0.0034(10) 0.0041(11) 0.0008(12) C27 0.0180(13) 0.0323(13) 0.0125(12) -0.0010(9) 0.0008(10) -0.0001(9) C28 0.0126(11) 0.0185(9) 0.0132(10) -0.0009(8) -0.0029(8) -0.0013(8) C29 0.0171(11) 0.0215(10) 0.0175(11) -0.0021(8) 0.0005(9) -0.0014(9) C30 0.0131(11) 0.0234(10) 0.0219(12) 0.0012(9) 0.0014(9) -0.0008(9) C31 0.0152(12) 0.0214(10) 0.0234(12) -0.0003(9) -0.0026(10) -0.0017(9) C32 0.0150(11) 0.0204(10) 0.0202(11) -0.0046(9) 0.0007(9) -0.0023(8) C33 0.0141(11) 0.0187(10) 0.0213(11) -0.0032(9) -0.0003(9) -0.0010(8) P3 0.0180(3) 0.0329(3) 0.0185(3) 0.0004(3) -0.0077(3) -0.0031(3) F1 0.0540(15) 0.0576(13) 0.0542(14) -0.0202(11) -0.0025(12) 0.0214(11) F2 0.0485(14) 0.0724(15) 0.0455(13) 0.0042(11) -0.0226(11) -0.0341(12) F3 0.0338(13) 0.0820(16) 0.0491(14) -0.0203(12) -0.0014(11) 0.0151(11) F4 0.0244(10) 0.0509(10) 0.0406(11) -0.0017(9) -0.0056(9) -0.0143(8) F5 0.0584(14) 0.0499(11) 0.0280(10) 0.0104(9) -0.0165(10) -0.0008(10) F6 0.0573(14) 0.0542(12) 0.0284(10) 0.0129(9) -0.0196(10) -0.0151(11) _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 C6 2.171(2) . ? Ru1 C3 2.211(2) . ? Ru1 C4 2.220(2) . ? Ru1 C1 2.227(2) . ? Ru1 C2 2.233(2) . ? Ru1 C5 2.248(3) . ? Ru1 C7 2.253(2) . ? Ru1 P1 2.2977(7) . ? Ru1 P2 2.3450(6) . ? P1 C6 1.772(3) . ? P1 C14 1.830(2) . ? P1 C8 1.838(3) . ? P2 C20 1.829(2) . ? P2 C28 1.849(2) . ? P2 C22 1.860(3) . ? C1 C2 1.409(4) . ? C1 C5 1.426(4) . ? C2 C3 1.437(4) . ? C3 C4 1.418(4) . ? C4 C5 1.432(4) . ? C6 C7 1.406(4) . ? C8 C9 1.527(4) . ? C8 C13 1.539(4) . ? C9 C10 1.526(4) . ? C10 C11 1.528(4) . ? C11 C12 1.515(4) . ? C12 C13 1.536(4) . ? C14 C19 1.536(4) . ? C14 C15 1.540(3) . ? C15 C16 1.530(4) . ? C16 C17 1.504(4) . ? C17 C18 1.525(4) . ? C18 C19 1.532(4) . ? C20 C21 1.332(4) . ? C22 C23 1.538(3) . ? C22 C27 1.537(4) . ? C23 C24 1.527(4) . ? C24 C25 1.533(4) . ? C25 C26 1.524(4) . ? C26 C27 1.529(4) . ? C28 C29 1.531(4) . ? C28 C33 1.538(3) . ? C29 C30 1.533(3) . ? C30 C31 1.527(3) . ? C31 C32 1.520(4) . ? C32 C33 1.532(3) . ? P3 F1 1.577(2) . ? P3 F5 1.584(2) . ? P3 F2 1.593(2) . ? P3 F6 1.604(2) . ? P3 F4 1.606(2) . ? P3 F3 1.613(2) . ? 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 C6 Ru1 C3 102.34(9) . . ? C6 Ru1 C4 90.77(9) . . ? C3 Ru1 C4 37.34(10) . . ? C6 Ru1 C1 151.12(9) . . ? C3 Ru1 C1 62.10(10) . . ? C4 Ru1 C1 61.84(9) . . ? C6 Ru1 C2 139.06(10) . . ? C3 Ru1 C2 37.74(10) . . ? C4 Ru1 C2 62.42(10) . . ? C1 Ru1 C2 36.83(11) . . ? C6 Ru1 C5 114.86(9) . . ? C3 Ru1 C5 62.68(10) . . ? C4 Ru1 C5 37.38(9) . . ? C1 Ru1 C5 37.16(9) . . ? C2 Ru1 C5 62.43(10) . . ? C6 Ru1 C7 37.01(9) . . ? C3 Ru1 C7 130.50(9) . . ? C4 Ru1 C7 101.77(9) . . ? C1 Ru1 C7 134.79(10) . . ? C2 Ru1 C7 163.88(10) . . ? C5 Ru1 C7 103.47(10) . . ? C6 Ru1 P1 46.61(7) . . ? C3 Ru1 P1 97.30(7) . . ? C4 Ru1 P1 114.70(7) . . ? C1 Ru1 P1 151.36(8) . . ? C2 Ru1 P1 114.80(8) . . ? C5 Ru1 P1 151.69(7) . . ? C7 Ru1 P1 73.45(8) . . ? C6 Ru1 P2 113.57(6) . . ? C3 Ru1 P2 142.53(7) . . ? C4 Ru1 P2 145.71(7) . . ? C1 Ru1 P2 88.63(6) . . ? C2 Ru1 P2 104.89(7) . . ? C5 Ru1 P2 108.39(7) . . ? C7 Ru1 P2 86.51(6) . . ? P1 Ru1 P2 99.58(2) . . ? C6 P1 C14 112.48(11) . . ? C6 P1 C8 106.65(12) . . ? C14 P1 C8 113.22(12) . . ? C6 P1 Ru1 62.94(8) . . ? C14 P1 Ru1 128.01(8) . . ? C8 P1 Ru1 117.48(9) . . ? C20 P2 C28 101.15(11) . . ? C20 P2 C22 99.80(11) . . ? C28 P2 C22 104.29(11) . . ? C20 P2 Ru1 120.84(8) . . ? C28 P2 Ru1 116.09(8) . . ? C22 P2 Ru1 112.25(8) . . ? C2 C1 C5 110.0(2) . . ? C2 C1 Ru1 71.83(15) . . ? C5 C1 Ru1 72.24(14) . . ? C1 C2 C3 107.1(2) . . ? C1 C2 Ru1 71.34(14) . . ? C3 C2 Ru1 70.28(13) . . ? C4 C3 C2 107.8(2) . . ? C4 C3 Ru1 71.69(14) . . ? C2 C3 Ru1 71.99(13) . . ? C3 C4 C5 108.9(2) . . ? C3 C4 Ru1 70.97(14) . . ? C5 C4 Ru1 72.39(13) . . ? C1 C5 C4 106.2(2) . . ? C1 C5 Ru1 70.60(14) . . ? C4 C5 Ru1 70.24(14) . . ? C7 C6 P1 117.33(17) . . ? C7 C6 Ru1 74.66(14) . . ? P1 C6 Ru1 70.45(8) . . ? C6 C7 Ru1 68.33(13) . . ? C9 C8 C13 112.1(2) . . ? C9 C8 P1 115.22(17) . . ? C13 C8 P1 112.96(17) . . ? C10 C9 C8 109.4(2) . . ? C9 C10 C11 111.2(2) . . ? C12 C11 C10 111.6(3) . . ? C11 C12 C13 112.7(2) . . ? C12 C13 C8 109.1(2) . . ? C19 C14 C15 110.4(2) . . ? C19 C14 P1 113.06(16) . . ? C15 C14 P1 113.34(16) . . ? C16 C15 C14 110.1(2) . . ? C17 C16 C15 112.5(2) . . ? C16 C17 C18 111.5(2) . . ? C17 C18 C19 110.8(2) . . ? C18 C19 C14 109.3(2) . . ? C21 C20 P2 128.5(2) . . ? C23 C22 C27 110.3(2) . . ? C23 C22 P2 112.23(17) . . ? C27 C22 P2 114.4(2) . . ? C24 C23 C22 110.9(2) . . ? C23 C24 C25 111.6(3) . . ? C26 C25 C24 110.8(2) . . ? C25 C26 C27 111.8(2) . . ? C26 C27 C22 111.3(2) . . ? C29 C28 C33 109.9(2) . . ? C29 C28 P2 111.01(16) . . ? C33 C28 P2 114.90(16) . . ? C28 C29 C30 110.4(2) . . ? C31 C30 C29 110.3(2) . . ? C32 C31 C30 112.0(2) . . ? C31 C32 C33 111.0(2) . . ? C32 C33 C28 109.9(2) . . ? F1 P3 F5 90.64(13) . . ? F1 P3 F2 90.47(15) . . ? F5 P3 F2 90.14(12) . . ? F1 P3 F6 90.40(14) . . ? F5 P3 F6 178.94(14) . . ? F2 P3 F6 90.06(12) . . ? F1 P3 F4 90.86(14) . . ? F5 P3 F4 90.70(12) . . ? F2 P3 F4 178.42(14) . . ? F6 P3 F4 89.08(11) . . ? F1 P3 F3 178.84(13) . . ? F5 P3 F3 90.34(14) . . ? F2 P3 F3 90.15(15) . . ? F6 P3 F3 88.62(14) . . ? F4 P3 F3 88.50(13) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 2.379 _refine_diff_density_min -4.128 _refine_diff_density_rms 0.163 #===END data_jhn521a _database_code_depnum_ccdc_archive 'CCDC 248576' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H59 Cl2 F6 P3 Ru' _chemical_formula_weight 858.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1094(14) _cell_length_b 12.8338(14) _cell_length_c 17.610(2) _cell_angle_alpha 101.606(11) _cell_angle_beta 100.011(14) _cell_angle_gamma 113.171(11) _cell_volume 1974.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 12.46 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .46 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9179 _exptl_absorpt_correction_T_max 0.9463 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7905 _diffrn_reflns_av_R_equivalents 0.1361 _diffrn_reflns_av_sigmaI/netI 0.1356 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6763 _reflns_number_gt 4136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0000P] 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 6763 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1354 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.1825 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.72790(7) 0.83627(5) 0.65484(4) 0.0325(2) Uani 1 1 d . . . P1 P 0.8686(2) 1.01647(17) 0.75454(12) 0.0381(5) Uani 1 1 d . . . P2 P 0.4853(2) 0.81718(16) 0.65250(11) 0.0340(5) Uani 1 1 d . . . C1 C 0.8320(9) 0.7429(7) 0.5850(5) 0.048(2) Uani 1 1 d . . . C2 C 0.8811(10) 0.7535(8) 0.6682(6) 0.055(2) Uani 1 1 d . . . H2A H 0.9855 0.7933 0.7017 0.066 Uiso 1 1 calc R . . C3 C 0.7574(10) 0.6885(7) 0.6917(5) 0.052(2) Uani 1 1 d . . . H3A H 0.7587 0.6750 0.7446 0.062 Uiso 1 1 calc R . . C4 C 0.6313(9) 0.6395(6) 0.6240(5) 0.046(2) Uani 1 1 d . . . H4A H 0.5289 0.5864 0.6221 0.055 Uiso 1 1 calc R . . C5 C 0.6776(9) 0.6733(7) 0.5582(5) 0.0437(19) Uani 1 1 d . . . H5A H 0.6140 0.6473 0.5027 0.052 Uiso 1 1 calc R . . C6 C 0.9359(13) 0.7925(10) 0.5358(7) 0.095(4) Uani 1 1 d . . . H6A H 0.9660 0.7343 0.5122 0.143 Uiso 1 1 calc R . . H6B H 1.0229 0.8626 0.5701 0.143 Uiso 1 1 calc R . . H6C H 0.8850 0.8122 0.4938 0.143 Uiso 1 1 calc R . . C7 C 0.7544(9) 0.9771(6) 0.5954(5) 0.0446(19) Uani 1 1 d . . . H7A H 0.7572 0.9585 0.5397 0.054 Uiso 1 1 calc R . . H7B H 0.6981 1.0218 0.6064 0.054 Uiso 1 1 calc R . . C8 C 0.8869(9) 1.0094(6) 0.6549(5) 0.0435(19) Uani 1 1 d . . . H8A H 0.9817 1.0227 0.6421 0.052 Uiso 1 1 calc R . . C9 C 0.8211(8) 1.1369(6) 0.7928(5) 0.0401(18) Uani 1 1 d . . . H9A H 0.7281 1.1220 0.7545 0.048 Uiso 1 1 calc R . . C10 C 0.9415(9) 1.2601(7) 0.7966(6) 0.053(2) Uani 1 1 d . . . H10A H 1.0373 1.2751 0.8307 0.063 Uiso 1 1 calc R . . H10B H 0.9517 1.2600 0.7428 0.063 Uiso 1 1 calc R . . C11 C 0.9007(11) 1.3587(8) 0.8298(6) 0.066(3) Uani 1 1 d . . . H11A H 0.9816 1.4349 0.8350 0.080 Uiso 1 1 calc R . . H11B H 0.8114 1.3493 0.7923 0.080 Uiso 1 1 calc R . . C12 C 0.8728(11) 1.3569(8) 0.9115(6) 0.073(3) Uani 1 1 d . . . H12A H 0.9641 1.3717 0.9500 0.087 Uiso 1 1 calc R . . H12B H 0.8451 1.4195 0.9307 0.087 Uiso 1 1 calc R . . C13 C 0.7491(12) 1.2384(9) 0.9061(6) 0.075(3) Uani 1 1 d . . . H13A H 0.6562 1.2253 0.8699 0.090 Uiso 1 1 calc R . . H13B H 0.7341 1.2384 0.9590 0.090 Uiso 1 1 calc R . . C14 C 0.7901(10) 1.1390(7) 0.8748(5) 0.052(2) Uani 1 1 d . . . H14A H 0.7086 1.0635 0.8701 0.063 Uiso 1 1 calc R . . H14B H 0.8784 1.1490 0.9135 0.063 Uiso 1 1 calc R . . C15 C 1.0441(9) 1.0484(8) 0.8290(5) 0.053(2) Uani 1 1 d . . . H15A H 1.0670 1.1227 0.8691 0.064 Uiso 1 1 calc R . . C16 C 1.1774(11) 1.0757(12) 0.7999(8) 0.104(5) Uani 1 1 d . . . H16A H 1.1900 1.1380 0.7744 0.124 Uiso 1 1 calc R . . H16B H 1.1638 1.0057 0.7596 0.124 Uiso 1 1 calc R . . C17 C 1.3184(10) 1.1158(11) 0.8691(8) 0.094(4) Uani 1 1 d . . . H17A H 1.4031 1.1266 0.8474 0.112 Uiso 1 1 calc R . . H17B H 1.3397 1.1915 0.9056 0.112 Uiso 1 1 calc R . . C18 C 1.2995(14) 1.0273(11) 0.9147(8) 0.103(4) Uani 1 1 d . . . H18A H 1.2942 0.9556 0.8803 0.123 Uiso 1 1 calc R . . H18B H 1.3865 1.0590 0.9610 0.123 Uiso 1 1 calc R . . C19 C 1.1670(14) 0.9977(13) 0.9418(7) 0.099(4) Uani 1 1 d . . . H19A H 1.1820 1.0657 0.9845 0.119 Uiso 1 1 calc R . . H19B H 1.1543 0.9331 0.9650 0.119 Uiso 1 1 calc R . . C20 C 1.0216(10) 0.9611(8) 0.8759(5) 0.058(2) Uani 1 1 d . . . H20A H 0.9919 0.8829 0.8398 0.069 Uiso 1 1 calc R . . H20B H 0.9420 0.9569 0.9008 0.069 Uiso 1 1 calc R . . C21 C 0.4634(8) 0.9513(6) 0.6889(5) 0.0389(18) Uani 1 1 d . . . H21A H 0.5010 0.9883 0.7443 0.047 Uiso 1 1 calc R . . C22 C 0.4016(10) 1.0022(8) 0.6471(6) 0.062(2) Uani 1 1 d . . . H22A H 0.3619 0.9696 0.5914 0.074 Uiso 1 1 calc R . . H22B H 0.3975 1.0710 0.6732 0.074 Uiso 1 1 calc R . . C23 C 0.3979(8) 0.7314(6) 0.7197(4) 0.0347(17) Uani 1 1 d . . . H23A H 0.3870 0.6507 0.6994 0.042 Uiso 1 1 calc R . . C24 C 0.4974(9) 0.7826(7) 0.8074(5) 0.047(2) Uani 1 1 d . . . H24A H 0.5960 0.7877 0.8083 0.056 Uiso 1 1 calc R . . H24B H 0.5090 0.8622 0.8298 0.056 Uiso 1 1 calc R . . C25 C 0.4297(10) 0.7055(8) 0.8589(5) 0.058(2) Uani 1 1 d . . . H25A H 0.4268 0.6282 0.8393 0.069 Uiso 1 1 calc R . . H25B H 0.4929 0.7416 0.9142 0.069 Uiso 1 1 calc R . . C26 C 0.2727(10) 0.6902(8) 0.8571(5) 0.057(2) Uani 1 1 d . . . H26A H 0.2769 0.7658 0.8835 0.069 Uiso 1 1 calc R . . H26B H 0.2300 0.6349 0.8864 0.069 Uiso 1 1 calc R . . C27 C 0.1724(9) 0.6433(8) 0.7698(5) 0.056(2) Uani 1 1 d . . . H27A H 0.1569 0.5629 0.7458 0.067 Uiso 1 1 calc R . . H27B H 0.0754 0.6409 0.7700 0.067 Uiso 1 1 calc R . . C28 C 0.2420(8) 0.7210(7) 0.7192(5) 0.045(2) Uani 1 1 d . . . H28A H 0.2491 0.7995 0.7403 0.054 Uiso 1 1 calc R . . H28B H 0.1780 0.6874 0.6641 0.054 Uiso 1 1 calc R . . C29 C 0.3402(8) 0.7415(6) 0.5517(4) 0.0357(17) Uani 1 1 d . . . H29A H 0.2559 0.7593 0.5572 0.043 Uiso 1 1 calc R . . C30 C 0.3978(9) 0.7931(7) 0.4850(5) 0.0446(19) Uani 1 1 d . . . H30A H 0.4360 0.8788 0.5024 0.054 Uiso 1 1 calc R . . H30B H 0.4790 0.7747 0.4756 0.054 Uiso 1 1 calc R . . C31 C 0.2706(9) 0.7403(7) 0.4069(5) 0.056(2) Uani 1 1 d . . . H31A H 0.3095 0.7692 0.3648 0.067 Uiso 1 1 calc R . . H31B H 0.1951 0.7668 0.4151 0.067 Uiso 1 1 calc R . . C32 C 0.1477(9) 0.5549(7) 0.4456(5) 0.052(2) Uani 1 1 d . . . H32A H 0.1084 0.4691 0.4278 0.063 Uiso 1 1 calc R . . H32B H 0.0673 0.5735 0.4564 0.063 Uiso 1 1 calc R . . C33 C 0.1971(10) 0.6035(7) 0.3793(5) 0.054(2) Uani 1 1 d . . . H33A H 0.1112 0.5736 0.3326 0.065 Uiso 1 1 calc R . . H33B H 0.2683 0.5765 0.3635 0.065 Uiso 1 1 calc R . . C34 C 0.2771(9) 0.6061(6) 0.5249(5) 0.0437(19) Uani 1 1 d . . . H34A H 0.2399 0.5746 0.5666 0.052 Uiso 1 1 calc R . . H34B H 0.3554 0.5835 0.5159 0.052 Uiso 1 1 calc R . . P3 P 0.3687(3) 0.3542(2) 0.70252(16) 0.0649(7) Uani 1 1 d . . . F1 F 0.2887(9) 0.4117(6) 0.6525(5) 0.132(3) Uani 1 1 d . . . F2 F 0.5080(8) 0.4811(6) 0.7426(4) 0.122(3) Uani 1 1 d . . . F3 F 0.4306(10) 0.3290(9) 0.6302(5) 0.154(3) Uani 1 1 d . . . F4 F 0.4522(9) 0.2978(7) 0.7510(5) 0.132(3) Uani 1 1 d . . . F5 F 0.2293(9) 0.2315(6) 0.6644(5) 0.137(3) Uani 1 1 d . . . F6 F 0.3058(10) 0.3810(7) 0.7748(5) 0.145(3) Uani 1 1 d . . . C35 C 0.6675(14) 0.5547(12) 0.9294(8) 0.110(5) Uani 1 1 d . . . H35A H 0.5792 0.5678 0.9164 0.132 Uiso 1 1 calc R . . H35B H 0.6482 0.4805 0.8917 0.132 Uiso 1 1 calc R . . Cl1 Cl 0.8171(5) 0.6681(4) 0.9176(3) 0.1555(19) Uani 1 1 d . . . Cl2 Cl 0.6967(4) 0.5427(4) 1.0250(2) 0.1358(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0329(3) 0.0299(3) 0.0346(4) 0.0091(3) 0.0083(3) 0.0146(3) P1 0.0344(11) 0.0336(11) 0.0400(12) 0.0105(9) 0.0057(9) 0.0111(9) P2 0.0375(11) 0.0304(10) 0.0324(11) 0.0091(9) 0.0079(9) 0.0144(9) C1 0.043(5) 0.044(5) 0.062(6) 0.009(4) 0.025(4) 0.025(4) C2 0.045(5) 0.052(5) 0.065(6) -0.001(5) 0.000(5) 0.031(5) C3 0.071(6) 0.043(5) 0.050(5) 0.012(4) 0.011(5) 0.037(5) C4 0.047(5) 0.027(4) 0.062(6) 0.011(4) 0.012(4) 0.019(4) C5 0.057(5) 0.044(5) 0.036(5) 0.006(4) 0.012(4) 0.032(4) C6 0.099(9) 0.088(8) 0.092(9) 0.001(7) 0.042(8) 0.041(7) C7 0.057(5) 0.036(4) 0.037(5) 0.009(4) 0.010(4) 0.019(4) C8 0.043(5) 0.033(4) 0.053(5) 0.017(4) 0.016(4) 0.011(4) C9 0.037(4) 0.030(4) 0.040(5) 0.005(3) 0.001(4) 0.008(3) C10 0.044(5) 0.034(4) 0.065(6) 0.009(4) 0.006(4) 0.009(4) C11 0.082(7) 0.038(5) 0.069(7) 0.012(5) 0.008(5) 0.024(5) C12 0.071(7) 0.048(6) 0.081(8) -0.009(5) 0.000(6) 0.030(5) C13 0.071(7) 0.084(8) 0.056(6) -0.001(6) 0.014(5) 0.032(6) C14 0.055(5) 0.039(5) 0.046(5) 0.005(4) 0.009(4) 0.011(4) C15 0.054(5) 0.057(6) 0.052(5) 0.022(5) 0.007(4) 0.027(5) C16 0.050(7) 0.145(12) 0.139(12) 0.100(10) 0.030(7) 0.037(7) C17 0.031(5) 0.113(10) 0.123(11) 0.042(9) 0.004(6) 0.023(6) C18 0.098(10) 0.102(10) 0.097(10) 0.019(8) -0.022(8) 0.058(8) C19 0.107(10) 0.147(12) 0.070(8) 0.052(8) 0.021(7) 0.074(10) C20 0.055(6) 0.065(6) 0.056(6) 0.028(5) 0.013(5) 0.025(5) C21 0.038(4) 0.031(4) 0.042(5) 0.007(4) 0.007(4) 0.013(3) C22 0.077(7) 0.051(5) 0.066(6) 0.019(5) 0.017(5) 0.037(5) C23 0.036(4) 0.025(4) 0.038(4) 0.007(3) 0.005(3) 0.012(3) C24 0.048(5) 0.045(5) 0.038(5) 0.011(4) 0.007(4) 0.015(4) C25 0.083(7) 0.054(6) 0.038(5) 0.019(4) 0.011(5) 0.031(5) C26 0.070(6) 0.059(6) 0.061(6) 0.030(5) 0.036(5) 0.034(5) C27 0.041(5) 0.062(6) 0.055(6) 0.023(5) 0.017(4) 0.010(4) C28 0.043(5) 0.058(5) 0.036(5) 0.019(4) 0.013(4) 0.021(4) C29 0.029(4) 0.039(4) 0.037(4) 0.014(3) 0.005(3) 0.013(3) C30 0.049(5) 0.035(4) 0.044(5) 0.013(4) 0.012(4) 0.013(4) C31 0.051(5) 0.054(5) 0.045(5) 0.018(4) -0.005(4) 0.011(4) C32 0.053(5) 0.035(5) 0.054(6) 0.012(4) 0.008(4) 0.008(4) C33 0.052(5) 0.048(5) 0.044(5) 0.008(4) 0.000(4) 0.012(4) C34 0.045(5) 0.034(4) 0.044(5) 0.011(4) 0.010(4) 0.011(4) P3 0.0812(19) 0.0509(15) 0.0598(17) 0.0187(13) 0.0293(14) 0.0215(14) F1 0.142(7) 0.096(5) 0.153(7) 0.056(5) 0.001(5) 0.054(5) F2 0.126(6) 0.081(5) 0.096(5) 0.031(4) 0.013(4) -0.012(4) F3 0.169(8) 0.218(10) 0.094(6) 0.028(6) 0.071(6) 0.100(8) F4 0.165(8) 0.109(6) 0.118(6) 0.046(5) -0.005(5) 0.069(6) F5 0.127(6) 0.068(4) 0.139(7) 0.037(5) -0.015(5) -0.013(4) F6 0.155(7) 0.141(7) 0.132(7) 0.026(6) 0.093(6) 0.044(6) C35 0.101(10) 0.112(10) 0.128(12) 0.056(9) 0.003(8) 0.059(9) Cl1 0.163(4) 0.130(3) 0.123(3) 0.074(3) -0.006(3) 0.016(3) Cl2 0.084(2) 0.223(5) 0.097(3) 0.065(3) 0.015(2) 0.060(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 C8 2.170(7) . ? Ru1 C2 2.203(7) . ? Ru1 C1 2.215(7) . ? Ru1 C7 2.216(7) . ? Ru1 C4 2.225(7) . ? Ru1 C5 2.227(7) . ? Ru1 C3 2.232(8) . ? Ru1 P1 2.316(2) . ? Ru1 P2 2.359(2) . ? P1 C8 1.785(8) . ? P1 C9 1.830(7) . ? P1 C15 1.854(8) . ? P2 C21 1.825(7) . ? P2 C23 1.875(7) . ? P2 C29 1.878(7) . ? C1 C5 1.391(11) . ? C1 C2 1.424(12) . ? C1 C6 1.506(13) . ? C2 C3 1.388(12) . ? C3 C4 1.408(11) . ? C4 C5 1.407(11) . ? C7 C8 1.402(11) . ? C9 C14 1.528(11) . ? C9 C10 1.549(10) . ? C10 C11 1.519(11) . ? C11 C12 1.517(13) . ? C12 C13 1.513(14) . ? C13 C14 1.521(12) . ? C15 C16 1.464(13) . ? C15 C20 1.492(10) . ? C16 C17 1.533(14) . ? C17 C18 1.490(15) . ? C18 C19 1.436(16) . ? C19 C20 1.540(13) . ? C21 C22 1.308(10) . ? C23 C28 1.527(10) . ? C23 C24 1.536(10) . ? C24 C25 1.521(10) . ? C25 C26 1.514(11) . ? C26 C27 1.536(12) . ? C27 C28 1.519(10) . ? C29 C34 1.531(10) . ? C29 C30 1.550(10) . ? C30 C31 1.526(11) . ? C31 C33 1.541(11) . ? C32 C33 1.502(11) . ? C32 C34 1.553(11) . ? P3 F3 1.545(7) . ? P3 F5 1.554(7) . ? P3 F6 1.556(7) . ? P3 F4 1.563(7) . ? P3 F1 1.567(7) . ? P3 F2 1.588(7) . ? C35 Cl2 1.706(13) . ? C35 Cl1 1.717(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 C8 Ru1 C2 98.7(3) . . ? C8 Ru1 C1 92.8(3) . . ? C2 Ru1 C1 37.6(3) . . ? C8 Ru1 C7 37.3(3) . . ? C2 Ru1 C7 124.7(3) . . ? C1 Ru1 C7 99.1(3) . . ? C8 Ru1 C4 153.9(3) . . ? C2 Ru1 C4 61.2(3) . . ? C1 Ru1 C4 61.0(3) . . ? C7 Ru1 C4 140.1(3) . . ? C8 Ru1 C5 120.6(3) . . ? C2 Ru1 C5 61.9(3) . . ? C1 Ru1 C5 36.5(3) . . ? C7 Ru1 C5 106.3(3) . . ? C4 Ru1 C5 36.8(3) . . ? C8 Ru1 C3 132.4(3) . . ? C2 Ru1 C3 36.5(3) . . ? C1 Ru1 C3 61.7(3) . . ? C7 Ru1 C3 160.1(3) . . ? C4 Ru1 C3 36.8(3) . . ? C5 Ru1 C3 61.8(3) . . ? C8 Ru1 P1 46.8(2) . . ? C2 Ru1 P1 100.4(2) . . ? C1 Ru1 P1 122.3(2) . . ? C7 Ru1 P1 73.1(2) . . ? C4 Ru1 P1 146.7(2) . . ? C5 Ru1 P1 158.8(2) . . ? C3 Ru1 P1 111.8(2) . . ? C8 Ru1 P2 114.9(2) . . ? C2 Ru1 P2 146.0(3) . . ? C1 Ru1 P2 137.9(2) . . ? C7 Ru1 P2 87.4(2) . . ? C4 Ru1 P2 87.6(2) . . ? C5 Ru1 P2 101.7(2) . . ? C3 Ru1 P2 110.0(3) . . ? P1 Ru1 P2 99.41(7) . . ? C8 P1 C9 110.6(3) . . ? C8 P1 C15 113.3(4) . . ? C9 P1 C15 105.4(4) . . ? C8 P1 Ru1 62.3(2) . . ? C9 P1 Ru1 130.7(3) . . ? C15 P1 Ru1 122.5(3) . . ? C21 P2 C23 99.5(3) . . ? C21 P2 C29 102.5(3) . . ? C23 P2 C29 103.9(3) . . ? C21 P2 Ru1 118.5(2) . . ? C23 P2 Ru1 113.8(2) . . ? C29 P2 Ru1 116.4(2) . . ? C5 C1 C2 108.1(7) . . ? C5 C1 C6 127.8(9) . . ? C2 C1 C6 124.0(9) . . ? C5 C1 Ru1 72.2(4) . . ? C2 C1 Ru1 70.7(4) . . ? C6 C1 Ru1 126.2(6) . . ? C3 C2 C1 108.3(8) . . ? C3 C2 Ru1 72.9(4) . . ? C1 C2 Ru1 71.7(4) . . ? C2 C3 C4 107.4(8) . . ? C2 C3 Ru1 70.6(5) . . ? C4 C3 Ru1 71.3(4) . . ? C5 C4 C3 108.9(8) . . ? C5 C4 Ru1 71.7(4) . . ? C3 C4 Ru1 71.9(4) . . ? C1 C5 C4 107.4(7) . . ? C1 C5 Ru1 71.3(5) . . ? C4 C5 Ru1 71.5(4) . . ? C8 C7 Ru1 69.6(4) . . ? C7 C8 P1 115.3(6) . . ? C7 C8 Ru1 73.1(4) . . ? P1 C8 Ru1 70.9(3) . . ? C14 C9 C10 110.3(7) . . ? C14 C9 P1 112.4(5) . . ? C10 C9 P1 112.7(5) . . ? C11 C10 C9 111.6(7) . . ? C12 C11 C10 111.2(7) . . ? C13 C12 C11 110.9(8) . . ? C12 C13 C14 110.0(8) . . ? C13 C14 C9 112.3(7) . . ? C16 C15 C20 113.9(7) . . ? C16 C15 P1 116.2(7) . . ? C20 C15 P1 112.7(6) . . ? C15 C16 C17 111.3(10) . . ? C18 C17 C16 111.4(9) . . ? C19 C18 C17 112.4(10) . . ? C18 C19 C20 115.0(9) . . ? C15 C20 C19 110.6(8) . . ? C22 C21 P2 128.4(7) . . ? C28 C23 C24 108.9(6) . . ? C28 C23 P2 113.7(5) . . ? C24 C23 P2 112.4(5) . . ? C25 C24 C23 111.2(7) . . ? C26 C25 C24 111.8(7) . . ? C25 C26 C27 110.9(7) . . ? C28 C27 C26 111.4(7) . . ? C27 C28 C23 111.3(6) . . ? C34 C29 C30 110.6(6) . . ? C34 C29 P2 114.3(5) . . ? C30 C29 P2 111.8(5) . . ? C31 C30 C29 110.0(6) . . ? C30 C31 C33 112.2(7) . . ? C33 C32 C34 112.5(7) . . ? C32 C33 C31 111.0(7) . . ? C29 C34 C32 108.7(6) . . ? F3 P3 F5 89.9(5) . . ? F3 P3 F6 179.1(5) . . ? F5 P3 F6 90.4(5) . . ? F3 P3 F4 91.8(5) . . ? F5 P3 F4 90.5(4) . . ? F6 P3 F4 89.1(5) . . ? F3 P3 F1 86.6(5) . . ? F5 P3 F1 90.3(4) . . ? F6 P3 F1 92.5(5) . . ? F4 P3 F1 178.2(5) . . ? F3 P3 F2 91.6(5) . . ? F5 P3 F2 178.3(5) . . ? F6 P3 F2 88.1(5) . . ? F4 P3 F2 90.4(4) . . ? F1 P3 F2 88.9(4) . . ? Cl2 C35 Cl1 112.8(7) . . ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.862 _refine_diff_density_max 1.510 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.101 #===END data_jhn566fm _database_code_depnum_ccdc_archive 'CCDC 248577' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H36 F6 O P2' _chemical_formula_weight 576.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 9.6199(6) _cell_length_b 12.0564(8) _cell_length_c 13.1906(8) _cell_angle_alpha 72.1230(10) _cell_angle_beta 75.2560(10) _cell_angle_gamma 69.1020(10) _cell_volume 1342.01(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5336 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max .17 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .003 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 0.226 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24172 _diffrn_reflns_av_R_equivalents 0.0748 _diffrn_reflns_av_sigmaI/netI 0.1517 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 32.39 _reflns_number_total 9488 _reflns_number_gt 4901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] 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 9488 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1265 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.2033 _refine_ls_wR_factor_gt 0.1885 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 P1 P 0.76134(9) 0.10945(7) 0.22140(6) 0.01257(17) Uani 1 1 d . . . C1 C 0.7533(3) 0.1968(3) 0.3134(2) 0.0144(6) Uani 1 1 d . . . H1A H 0.8125 0.1418 0.3697 0.017 Uiso 1 1 calc R . . C2 C 0.5893(4) 0.2441(3) 0.3678(3) 0.0207(7) Uani 1 1 d . . . H2A H 0.5512 0.1755 0.4067 0.025 Uiso 1 1 calc R . . H2B H 0.5270 0.2951 0.3133 0.025 Uiso 1 1 calc R . . C3 C 0.5806(4) 0.3185(3) 0.4466(3) 0.0246(8) Uani 1 1 d . . . H3A H 0.4759 0.3517 0.4771 0.030 Uiso 1 1 calc R . . H3B H 0.6340 0.2648 0.5054 0.030 Uiso 1 1 calc R . . C4 C 0.6483(4) 0.4224(3) 0.3912(3) 0.0254(8) Uani 1 1 d . . . H4A H 0.6469 0.4636 0.4443 0.030 Uiso 1 1 calc R . . H4B H 0.5875 0.4814 0.3384 0.030 Uiso 1 1 calc R . . C5 C 0.8108(4) 0.3758(3) 0.3350(3) 0.0254(8) Uani 1 1 d . . . H5A H 0.8479 0.4449 0.2960 0.030 Uiso 1 1 calc R . . H5B H 0.8743 0.3252 0.3890 0.030 Uiso 1 1 calc R . . C6 C 0.8211(4) 0.3021(3) 0.2569(3) 0.0182(7) Uani 1 1 d . . . H6A H 0.9260 0.2691 0.2268 0.022 Uiso 1 1 calc R . . H6B H 0.7678 0.3553 0.1980 0.022 Uiso 1 1 calc R . . C7 C 0.7391(3) -0.0385(3) 0.2958(2) 0.0145(6) Uani 1 1 d . . . H7A H 0.6516 -0.0258 0.3532 0.017 Uiso 1 1 calc R . . C8 C 0.7102(4) -0.1035(3) 0.2221(3) 0.0157(6) Uani 1 1 d . . . H8A H 0.6186 -0.0541 0.1926 0.019 Uiso 1 1 calc R . . H8B H 0.7932 -0.1131 0.1624 0.019 Uiso 1 1 calc R . . C9 C 0.6950(4) -0.2290(3) 0.2867(3) 0.0189(7) Uani 1 1 d . . . H9A H 0.6063 -0.2184 0.3422 0.023 Uiso 1 1 calc R . . H9B H 0.6814 -0.2703 0.2391 0.023 Uiso 1 1 calc R . . C10 C 0.8330(4) -0.3075(3) 0.3393(3) 0.0202(7) Uani 1 1 d . . . H10A H 0.9205 -0.3242 0.2837 0.024 Uiso 1 1 calc R . . H10B H 0.8181 -0.3850 0.3818 0.024 Uiso 1 1 calc R . . C11 C 0.8615(4) -0.2432(3) 0.4119(3) 0.0195(7) Uani 1 1 d . . . H11A H 0.9522 -0.2936 0.4423 0.023 Uiso 1 1 calc R . . H11B H 0.7778 -0.2330 0.4710 0.023 Uiso 1 1 calc R . . C12 C 0.8795(4) -0.1178(3) 0.3489(3) 0.0165(6) Uani 1 1 d . . . H12A H 0.9685 -0.1281 0.2938 0.020 Uiso 1 1 calc R . . H12B H 0.8925 -0.0773 0.3976 0.020 Uiso 1 1 calc R . . C13 C 0.9245(4) 0.0935(3) 0.1194(2) 0.0152(6) Uani 1 1 d . . . H13A H 1.0239 0.0571 0.1312 0.018 Uiso 1 1 calc R . . C14 C 0.8788(4) 0.1434(3) 0.0217(3) 0.0166(6) Uani 1 1 d . . . H14A H 0.9461 0.1444 -0.0429 0.020 Uiso 1 1 calc R . . C15 C 0.6329(3) 0.1904(3) 0.1264(2) 0.0138(6) Uani 1 1 d . . . H15A H 0.5290 0.2227 0.1439 0.017 Uiso 1 1 calc R . . C16 C 0.7118(4) 0.1966(3) 0.0259(2) 0.0147(6) Uani 1 1 d . . . C17 C 0.6512(4) 0.2408(3) -0.0805(2) 0.0146(6) Uani 1 1 d . . . C18 C 0.4800(4) 0.2675(3) -0.0607(2) 0.0147(6) Uani 1 1 d . . . C19 C 0.3796(4) 0.3837(3) -0.0899(3) 0.0174(6) Uani 1 1 d . . . H19A H 0.4162 0.4501 -0.1235 0.021 Uiso 1 1 calc R . . C20 C 0.2244(4) 0.4015(3) -0.0690(3) 0.0215(7) Uani 1 1 d . . . H20A H 0.1584 0.4794 -0.0894 0.026 Uiso 1 1 calc R . . C21 C 0.1684(4) 0.3040(3) -0.0183(3) 0.0211(7) Uani 1 1 d . . . H21A H 0.0650 0.3161 -0.0046 0.025 Uiso 1 1 calc R . . C22 C 0.2670(4) 0.1883(3) 0.0121(3) 0.0205(7) Uani 1 1 d . . . H22A H 0.2299 0.1224 0.0467 0.025 Uiso 1 1 calc R . . C23 C 0.4203(4) 0.1706(3) -0.0089(3) 0.0206(7) Uani 1 1 d . . . H23A H 0.4855 0.0923 0.0119 0.025 Uiso 1 1 calc R . . C24 C 0.7015(3) 0.3496(3) -0.1535(3) 0.0158(6) Uani 1 1 d . . . C25 C 0.7309(4) 0.3667(3) -0.2651(3) 0.0208(7) Uani 1 1 d . . . H25A H 0.7237 0.3092 -0.2954 0.025 Uiso 1 1 calc R . . C26 C 0.7710(4) 0.4685(3) -0.3322(3) 0.0235(7) Uani 1 1 d . . . H26A H 0.7902 0.4783 -0.4066 0.028 Uiso 1 1 calc R . . C27 C 0.7824(4) 0.5553(3) -0.2885(3) 0.0270(8) Uani 1 1 d . . . H27A H 0.8087 0.6235 -0.3336 0.032 Uiso 1 1 calc R . . C28 C 0.7543(4) 0.5399(3) -0.1773(3) 0.0260(8) Uani 1 1 d . . . H28A H 0.7623 0.5974 -0.1473 0.031 Uiso 1 1 calc R . . C29 C 0.7140(4) 0.4380(3) -0.1110(3) 0.0221(7) Uani 1 1 d . . . H29A H 0.6948 0.4284 -0.0366 0.026 Uiso 1 1 calc R . . O1 O 0.7245(3) 0.1344(2) -0.1243(2) 0.0205(5) Uani 1 1 d . . . P2 P 0.75285(10) 0.96617(8) -0.34565(7) 0.01762(19) Uani 1 1 d . . . F1 F 0.6558(3) 0.8892(2) -0.25471(18) 0.0417(6) Uani 1 1 d . . . F2 F 0.6524(2) 1.0867(2) -0.30113(18) 0.0329(5) Uani 1 1 d . . . F3 F 0.8464(2) 1.0458(2) -0.43644(17) 0.0334(5) Uani 1 1 d . . . F4 F 0.8529(3) 0.84711(19) -0.38801(18) 0.0337(5) Uani 1 1 d . . . F5 F 0.6353(2) 0.9985(2) -0.42520(17) 0.0304(5) Uani 1 1 d . . . F6 F 0.8682(2) 0.93607(19) -0.26506(16) 0.0276(5) Uani 1 1 d . . . H1B H 0.679(6) 0.141(5) -0.179(4) 0.067(17) 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 P1 0.0135(4) 0.0124(4) 0.0126(4) -0.0030(3) -0.0032(3) -0.0041(3) C1 0.0168(15) 0.0108(14) 0.0147(15) -0.0015(11) -0.0043(12) -0.0033(12) C2 0.0199(17) 0.0183(16) 0.0229(17) -0.0071(13) 0.0014(13) -0.0059(13) C3 0.032(2) 0.0173(16) 0.0214(18) -0.0078(14) -0.0021(15) -0.0020(15) C4 0.0271(19) 0.0193(17) 0.034(2) -0.0146(15) -0.0076(16) -0.0027(15) C5 0.0272(19) 0.0223(18) 0.032(2) -0.0109(15) -0.0045(16) -0.0100(15) C6 0.0176(16) 0.0151(15) 0.0219(17) -0.0039(13) -0.0001(13) -0.0077(13) C7 0.0160(15) 0.0128(14) 0.0134(14) -0.0016(11) -0.0027(12) -0.0041(12) C8 0.0161(15) 0.0155(15) 0.0180(15) -0.0048(12) -0.0058(12) -0.0048(12) C9 0.0204(17) 0.0162(15) 0.0222(17) -0.0036(13) -0.0052(13) -0.0076(13) C10 0.0272(18) 0.0130(15) 0.0213(17) -0.0024(13) -0.0085(14) -0.0056(13) C11 0.0247(18) 0.0141(15) 0.0201(17) -0.0008(12) -0.0100(14) -0.0046(13) C12 0.0199(16) 0.0135(14) 0.0193(16) -0.0048(12) -0.0080(13) -0.0045(12) C13 0.0134(15) 0.0188(15) 0.0132(14) -0.0027(12) -0.0026(11) -0.0053(12) C14 0.0157(15) 0.0182(15) 0.0159(15) -0.0035(12) -0.0012(12) -0.0066(13) C15 0.0136(15) 0.0123(14) 0.0149(15) -0.0035(11) -0.0047(11) -0.0014(11) C16 0.0189(16) 0.0127(14) 0.0141(14) -0.0027(11) -0.0037(12) -0.0064(12) C17 0.0167(15) 0.0134(14) 0.0132(14) -0.0024(11) -0.0017(12) -0.0052(12) C18 0.0189(16) 0.0149(14) 0.0132(14) -0.0033(12) -0.0056(12) -0.0064(12) C19 0.0202(16) 0.0145(15) 0.0185(16) -0.0029(12) -0.0020(13) -0.0078(13) C20 0.0183(17) 0.0159(15) 0.0271(18) -0.0032(13) -0.0039(14) -0.0030(13) C21 0.0186(17) 0.0255(18) 0.0224(17) -0.0082(14) -0.0021(13) -0.0093(14) C22 0.0267(18) 0.0228(17) 0.0167(16) -0.0004(13) -0.0039(13) -0.0163(15) C23 0.0272(18) 0.0145(15) 0.0219(17) -0.0005(13) -0.0096(14) -0.0078(14) C24 0.0138(15) 0.0159(15) 0.0157(15) -0.0004(12) -0.0028(12) -0.0049(12) C25 0.0181(17) 0.0222(17) 0.0183(16) -0.0033(13) -0.0025(13) -0.0033(14) C26 0.0208(18) 0.0261(18) 0.0166(16) 0.0018(14) -0.0015(13) -0.0060(14) C27 0.0205(18) 0.0228(18) 0.030(2) 0.0055(15) -0.0040(15) -0.0072(14) C28 0.031(2) 0.0214(18) 0.0273(19) 0.0001(15) -0.0081(16) -0.0128(15) C29 0.0270(19) 0.0205(17) 0.0175(16) -0.0007(13) -0.0030(14) -0.0095(14) O1 0.0258(13) 0.0162(11) 0.0199(12) -0.0081(10) -0.0071(10) -0.0013(10) P2 0.0157(4) 0.0233(4) 0.0150(4) -0.0056(3) -0.0036(3) -0.0057(3) F1 0.0439(15) 0.0563(16) 0.0277(13) 0.0038(11) -0.0021(11) -0.0329(13) F2 0.0231(11) 0.0385(13) 0.0360(13) -0.0193(10) -0.0095(10) 0.0039(10) F3 0.0298(12) 0.0406(13) 0.0264(12) 0.0014(10) -0.0014(10) -0.0167(11) F4 0.0390(13) 0.0278(12) 0.0349(13) -0.0153(10) -0.0134(11) 0.0010(10) F5 0.0265(12) 0.0429(13) 0.0274(11) -0.0101(10) -0.0147(9) -0.0083(10) F6 0.0253(11) 0.0354(12) 0.0244(11) -0.0113(9) -0.0136(9) -0.0020(9) _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 P1 C13 1.783(3) . ? P1 C15 1.796(3) . ? P1 C1 1.807(3) . ? P1 C7 1.811(3) . ? C1 C6 1.535(4) . ? C1 C2 1.536(4) . ? C2 C3 1.538(5) . ? C3 C4 1.519(5) . ? C4 C5 1.533(5) . ? C5 C6 1.520(5) . ? C7 C12 1.542(4) . ? C7 C8 1.549(4) . ? C8 C9 1.530(4) . ? C9 C10 1.520(4) . ? C10 C11 1.527(4) . ? C11 C12 1.532(4) . ? C13 C14 1.357(4) . ? C14 C16 1.495(4) . ? C15 C16 1.344(4) . ? C16 C17 1.526(4) . ? C17 O1 1.442(4) . ? C17 C24 1.524(4) . ? C17 C18 1.529(4) . ? C18 C19 1.391(4) . ? C18 C23 1.396(4) . ? C19 C20 1.396(5) . ? C20 C21 1.380(5) . ? C21 C22 1.383(5) . ? C22 C23 1.379(5) . ? C24 C25 1.389(4) . ? C24 C29 1.399(4) . ? C25 C26 1.391(5) . ? C26 C27 1.387(5) . ? C27 C28 1.388(5) . ? C28 C29 1.389(5) . ? P2 F3 1.590(2) . ? P2 F4 1.591(2) . ? P2 F1 1.593(2) . ? P2 F6 1.603(2) . ? P2 F5 1.603(2) . ? P2 F2 1.620(2) . ? 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 C13 P1 C15 93.89(15) . . ? C13 P1 C1 114.92(15) . . ? C15 P1 C1 113.34(14) . . ? C13 P1 C7 110.90(15) . . ? C15 P1 C7 112.71(14) . . ? C1 P1 C7 110.26(14) . . ? C6 C1 C2 111.3(3) . . ? C6 C1 P1 112.0(2) . . ? C2 C1 P1 109.5(2) . . ? C1 C2 C3 110.2(3) . . ? C4 C3 C2 111.8(3) . . ? C3 C4 C5 111.5(3) . . ? C6 C5 C4 111.5(3) . . ? C5 C6 C1 111.3(3) . . ? C12 C7 C8 111.0(2) . . ? C12 C7 P1 109.8(2) . . ? C8 C7 P1 111.3(2) . . ? C9 C8 C7 110.0(3) . . ? C10 C9 C8 111.6(3) . . ? C9 C10 C11 110.9(3) . . ? C10 C11 C12 111.3(3) . . ? C11 C12 C7 110.0(3) . . ? C14 C13 P1 108.2(2) . . ? C13 C14 C16 114.9(3) . . ? C16 C15 P1 108.8(2) . . ? C15 C16 C14 114.1(3) . . ? C15 C16 C17 128.0(3) . . ? C14 C16 C17 117.7(3) . . ? O1 C17 C24 110.6(2) . . ? O1 C17 C16 100.7(2) . . ? C24 C17 C16 111.1(2) . . ? O1 C17 C18 110.2(2) . . ? C24 C17 C18 112.6(2) . . ? C16 C17 C18 111.1(3) . . ? C19 C18 C23 117.9(3) . . ? C19 C18 C17 123.6(3) . . ? C23 C18 C17 118.4(3) . . ? C18 C19 C20 120.5(3) . . ? C21 C20 C19 120.4(3) . . ? C20 C21 C22 119.6(3) . . ? C23 C22 C21 120.1(3) . . ? C22 C23 C18 121.5(3) . . ? C25 C24 C29 117.7(3) . . ? C25 C24 C17 121.0(3) . . ? C29 C24 C17 121.2(3) . . ? C24 C25 C26 121.1(3) . . ? C27 C26 C25 120.3(3) . . ? C26 C27 C28 119.6(3) . . ? C27 C28 C29 119.6(3) . . ? C28 C29 C24 121.6(3) . . ? F3 P2 F4 90.72(13) . . ? F3 P2 F1 178.68(14) . . ? F4 P2 F1 90.44(14) . . ? F3 P2 F6 90.15(12) . . ? F4 P2 F6 90.04(11) . . ? F1 P2 F6 90.49(12) . . ? F3 P2 F5 89.94(12) . . ? F4 P2 F5 91.12(12) . . ? F1 P2 F5 89.40(12) . . ? F6 P2 F5 178.84(13) . . ? F3 P2 F2 89.43(13) . . ? F4 P2 F2 179.18(12) . . ? F1 P2 F2 89.42(13) . . ? F6 P2 F2 89.15(11) . . ? F5 P2 F2 89.69(12) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 32.39 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.781 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.096 data_552abs _database_code_depnum_ccdc_archive 'CCDC 248578' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 9 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H52 F12 P4' _chemical_formula_weight 740.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 7.934(7) _cell_length_b 12.17(2) _cell_length_c 17.83(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.60(14) _cell_angle_gamma 90.00 _cell_volume 1692(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max .25 _exptl_crystal_size_mid .21 _exptl_crystal_size_min .09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.309 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8097 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.1107 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2937 _reflns_number_gt 2250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+0.0000P] 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 2937 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1455 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 P1 P 0.92101(9) 0.60934(5) 0.44316(4) 0.0153(2) Uani 1 1 d . . . C1 C 0.9960(4) 0.5838(2) 0.35484(16) 0.0193(6) Uani 1 1 d . . . H1A H 1.0870 0.5262 0.3662 0.023 Uiso 1 1 calc R . . C2 C 0.8578(4) 0.5380(3) 0.29089(17) 0.0281(7) Uani 1 1 d . . . H2A H 0.8058 0.4714 0.3091 0.034 Uiso 1 1 calc R . . H2B H 0.7663 0.5933 0.2762 0.034 Uiso 1 1 calc R . . C3 C 0.9375(5) 0.5094(3) 0.22237(19) 0.0339(8) Uani 1 1 d . . . H3A H 0.8468 0.4834 0.1804 0.041 Uiso 1 1 calc R . . H3B H 1.0208 0.4489 0.2361 0.041 Uiso 1 1 calc R . . C4 C 1.0287(5) 0.6083(3) 0.19505(18) 0.0304(8) Uani 1 1 d . . . H4A H 1.0851 0.5854 0.1525 0.036 Uiso 1 1 calc R . . H4B H 0.9430 0.6655 0.1756 0.036 Uiso 1 1 calc R . . C5 C 1.1618(4) 0.6561(3) 0.25865(19) 0.0309(8) Uani 1 1 d . . . H5A H 1.2126 0.7227 0.2400 0.037 Uiso 1 1 calc R . . H5B H 1.2548 0.6019 0.2741 0.037 Uiso 1 1 calc R . . C6 C 1.0814(5) 0.6855(2) 0.32709(18) 0.0274(7) Uani 1 1 d . . . H6A H 0.9947 0.7440 0.3128 0.033 Uiso 1 1 calc R . . H6B H 1.1708 0.7138 0.3688 0.033 Uiso 1 1 calc R . . C7 C 0.7895(4) 0.7310(2) 0.44711(16) 0.0172(6) Uani 1 1 d . . . H7A H 0.7449 0.7243 0.4958 0.021 Uiso 1 1 calc R . . C8 C 0.8893(4) 0.8403(2) 0.4536(2) 0.0283(8) Uani 1 1 d . . . H8A H 0.9889 0.8361 0.4960 0.034 Uiso 1 1 calc R . . H8B H 0.9323 0.8546 0.4058 0.034 Uiso 1 1 calc R . . C9 C 0.7696(4) 0.9339(2) 0.4684(2) 0.0308(8) Uani 1 1 d . . . H9A H 0.7325 0.9213 0.5177 0.037 Uiso 1 1 calc R . . H9B H 0.8328 1.0045 0.4718 0.037 Uiso 1 1 calc R . . C10 C 0.6140(4) 0.9412(2) 0.40571(19) 0.0287(8) Uani 1 1 d . . . H10A H 0.6503 0.9595 0.3570 0.034 Uiso 1 1 calc R . . H10B H 0.5379 1.0007 0.4175 0.034 Uiso 1 1 calc R . . C11 C 0.5156(4) 0.8326(2) 0.3972(2) 0.0298(8) Uani 1 1 d . . . H11A H 0.4188 0.8379 0.3535 0.036 Uiso 1 1 calc R . . H11B H 0.4674 0.8191 0.4438 0.036 Uiso 1 1 calc R . . C12 C 0.6308(4) 0.7358(2) 0.38435(17) 0.0249(7) Uani 1 1 d . . . H12A H 0.5658 0.6663 0.3838 0.030 Uiso 1 1 calc R . . H12B H 0.6662 0.7439 0.3342 0.030 Uiso 1 1 calc R . . C13 C 0.7959(4) 0.4933(2) 0.46555(16) 0.0171(6) Uani 1 1 d . . . H13A H 0.7479 0.5115 0.5115 0.020 Uiso 1 1 calc R . . H13B H 0.6982 0.4824 0.4229 0.020 Uiso 1 1 calc R . . C14 C 0.8957(4) 0.3836(2) 0.48003(16) 0.0164(6) Uani 1 1 d . . . H14A H 0.9352 0.3616 0.4327 0.020 Uiso 1 1 calc R . . H14B H 0.8168 0.3258 0.4920 0.020 Uiso 1 1 calc R . . P2 P 0.59708(10) 0.66637(6) 0.64215(4) 0.0207(3) Uani 1 1 d . . . F1 F 0.5119(3) 0.67527(18) 0.55493(11) 0.0437(6) Uani 1 1 d . . . F2 F 0.4116(3) 0.66863(17) 0.66398(12) 0.0453(6) Uani 1 1 d . . . F3 F 0.6863(3) 0.6529(2) 0.72835(11) 0.0576(7) Uani 1 1 d . . . F4 F 0.7847(2) 0.66023(14) 0.61995(10) 0.0279(5) Uani 1 1 d . . . F5 F 0.6116(3) 0.79503(17) 0.64855(17) 0.0723(9) Uani 1 1 d . . . F6 F 0.5843(3) 0.53523(15) 0.63434(12) 0.0405(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0063(5) 0.0170(4) 0.0226(4) 0.0014(3) 0.0022(3) -0.0013(3) C1 0.0112(17) 0.0208(13) 0.0270(16) 0.0016(11) 0.0064(13) 0.0000(11) C2 0.027(2) 0.0325(16) 0.0255(16) -0.0041(13) 0.0061(14) -0.0053(13) C3 0.033(2) 0.0401(18) 0.0282(17) -0.0053(14) 0.0049(15) 0.0031(15) C4 0.022(2) 0.0420(18) 0.0286(17) 0.0076(14) 0.0094(14) 0.0149(14) C5 0.018(2) 0.0433(18) 0.0340(19) 0.0114(14) 0.0111(15) -0.0013(14) C6 0.028(2) 0.0268(15) 0.0291(17) 0.0024(12) 0.0101(15) -0.0079(13) C7 0.0097(17) 0.0190(13) 0.0232(14) -0.0010(11) 0.0037(12) -0.0001(11) C8 0.0137(19) 0.0219(15) 0.049(2) -0.0058(13) 0.0034(15) -0.0003(12) C9 0.023(2) 0.0213(14) 0.049(2) -0.0058(13) 0.0070(16) 0.0003(13) C10 0.023(2) 0.0206(14) 0.044(2) 0.0040(13) 0.0086(15) 0.0049(13) C11 0.013(2) 0.0259(15) 0.049(2) 0.0057(13) 0.0027(15) 0.0033(12) C12 0.0164(18) 0.0211(14) 0.0348(17) 0.0035(12) -0.0018(14) 0.0005(12) C13 0.0068(16) 0.0207(13) 0.0234(15) 0.0002(11) 0.0020(12) -0.0018(11) C14 0.0082(16) 0.0182(13) 0.0224(15) 0.0020(11) 0.0013(12) -0.0027(11) P2 0.0085(5) 0.0248(4) 0.0296(5) -0.0058(3) 0.0054(3) -0.0025(3) F1 0.0131(12) 0.0774(15) 0.0387(12) 0.0232(10) -0.0005(9) -0.0077(10) F2 0.0137(12) 0.0662(14) 0.0608(14) -0.0289(10) 0.0198(10) -0.0081(10) F3 0.0306(15) 0.116(2) 0.0257(12) -0.0159(11) 0.0038(10) -0.0202(13) F4 0.0062(10) 0.0444(10) 0.0336(10) -0.0029(8) 0.0048(8) -0.0021(7) F5 0.0143(13) 0.0259(11) 0.170(3) -0.0217(13) -0.0002(15) -0.0023(9) F6 0.0203(12) 0.0262(10) 0.0700(15) 0.0030(8) -0.0048(10) -0.0031(8) _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 P1 C14 1.807(4) 3_766 ? P1 C1 1.810(4) . ? P1 C13 1.813(4) . ? P1 C7 1.820(4) . ? C1 C2 1.534(5) . ? C1 C6 1.535(4) . ? C2 C3 1.516(5) . ? C3 C4 1.529(5) . ? C4 C5 1.516(5) . ? C5 C6 1.520(5) . ? C7 C12 1.524(5) . ? C7 C8 1.542(4) . ? C8 C9 1.536(5) . ? C9 C10 1.507(5) . ? C10 C11 1.528(5) . ? C11 C12 1.535(5) . ? C13 C14 1.550(4) . ? C14 P1 1.807(4) 3_766 ? P2 F5 1.573(4) . ? P2 F3 1.578(4) . ? P2 F1 1.581(4) . ? P2 F2 1.590(3) . ? P2 F6 1.603(4) . ? P2 F4 1.611(2) . ? 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 C14 P1 C1 108.68(19) 3_766 . ? C14 P1 C13 105.50(14) 3_766 . ? C1 P1 C13 109.82(15) . . ? C14 P1 C7 108.59(14) 3_766 . ? C1 P1 C7 117.11(14) . . ? C13 P1 C7 106.51(18) . . ? C2 C1 C6 110.5(3) . . ? C2 C1 P1 113.9(2) . . ? C6 C1 P1 112.2(2) . . ? C3 C2 C1 109.6(3) . . ? C2 C3 C4 111.6(3) . . ? C5 C4 C3 111.7(3) . . ? C4 C5 C6 110.7(3) . . ? C5 C6 C1 110.2(3) . . ? C12 C7 C8 111.5(2) . . ? C12 C7 P1 113.9(2) . . ? C8 C7 P1 114.5(2) . . ? C9 C8 C7 109.1(3) . . ? C10 C9 C8 111.4(3) . . ? C9 C10 C11 110.9(3) . . ? C10 C11 C12 111.8(3) . . ? C7 C12 C11 110.7(3) . . ? C14 C13 P1 115.1(2) . . ? C13 C14 P1 113.61(19) . 3_766 ? F5 P2 F3 91.10(15) . . ? F5 P2 F1 90.89(14) . . ? F3 P2 F1 177.51(14) . . ? F5 P2 F2 91.36(12) . . ? F3 P2 F2 91.88(19) . . ? F1 P2 F2 89.57(19) . . ? F5 P2 F6 178.91(14) . . ? F3 P2 F6 89.49(13) . . ? F1 P2 F6 88.51(11) . . ? F2 P2 F6 89.53(11) . . ? F5 P2 F4 90.30(12) . . ? F3 P2 F4 88.02(18) . . ? F1 P2 F4 90.47(18) . . ? F2 P2 F4 178.34(11) . . ? F6 P2 F4 88.80(10) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.867 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.116 #===END data_jhn524a _database_code_depnum_ccdc_archive 'CCDC 248579' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 10 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H32 Br O P Ru' _chemical_formula_weight 511.41 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' 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' Br Br -0.2901 2.4595 '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 P2(1)/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 7.3591(13) _cell_length_b 17.738(3) _cell_length_c 16.924(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.011(15) _cell_angle_gamma 90.00 _cell_volume 2207.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 5.33 _cell_measurement_theta_max 12.51 _exptl_crystal_description shard _exptl_crystal_colour red _exptl_crystal_size_max .40 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 2.599 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8423 _exptl_absorpt_correction_T_max 0.9569 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3953 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.1250 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 22.52 _reflns_number_total 2879 _reflns_number_gt 1458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1836P)^2^+1.5003P] 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 2879 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1956 _refine_ls_R_factor_gt 0.1034 _refine_ls_wR_factor_ref 0.3276 _refine_ls_wR_factor_gt 0.2604 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 1.050 _refine_ls_shift/su_mean 0.005 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 0.1899(2) 0.11909(9) 0.10475(10) 0.0667(7) Uani 1 1 d . . . P1 P 0.2667(7) 0.2064(4) 0.2015(4) 0.091(2) Uani 1 1 d . . . Br1 Br -0.0641(4) 0.2010(2) 0.0430(3) 0.1565(16) Uani 1 1 d . . . C1 C 0.272(4) 0.089(2) -0.018(2) 0.131(12) Uani 1 1 d . . . C2 C 0.252(3) 0.0229(19) 0.025(2) 0.111(11) Uani 1 1 d . . . H2A H 0.1647 -0.0168 0.0099 0.133 Uiso 1 1 calc R . . C3 C 0.372(5) 0.020(2) 0.094(2) 0.134(12) Uani 1 1 d . . . C4 C 0.475(3) 0.088(2) 0.0882(16) 0.093(9) Uani 1 1 d . . . H4A H 0.5812 0.1036 0.1212 0.111 Uiso 1 1 calc R . . C5 C 0.414(4) 0.1209(18) 0.021(2) 0.124(11) Uani 1 1 d . . . H5A H 0.4647 0.1688 0.0026 0.149 Uiso 1 1 calc R . . C6 C 0.174(9) 0.104(3) -0.094(3) 0.14(2) Uani 0.50 1 d P . . H6A H 0.2419 0.0840 -0.1370 0.203 Uiso 0.50 1 calc PR . . H6B H 0.1606 0.1578 -0.1014 0.203 Uiso 0.50 1 calc PR . . H6C H 0.0563 0.0811 -0.0944 0.203 Uiso 0.50 1 calc PR . . C6A C 0.440(18) 0.013(8) 0.170(7) 0.33(7) Uiso 0.50 1 d P . . H6AA H 0.5219 -0.0288 0.1731 0.488 Uiso 0.50 1 calc PR . . H6AB H 0.3422 0.0056 0.2048 0.488 Uiso 0.50 1 calc PR . . H6AC H 0.5044 0.0586 0.1843 0.488 Uiso 0.50 1 calc PR . . C7 C 0.076(4) 0.262(3) 0.225(3) 0.25(3) Uani 1 1 d . . . H7A H -0.0046 0.2758 0.1843 0.299 Uiso 1 1 calc R . . C8 C 0.040(5) 0.285(3) 0.294(3) 0.27(3) Uani 1 1 d . . . H8A H 0.1174 0.2728 0.3367 0.322 Uiso 1 1 calc R . . H8B H -0.0627 0.3142 0.3014 0.322 Uiso 1 1 calc R . . C9 C 0.434(5) 0.2836(11) 0.1615(17) 0.139(13) Uani 1 1 d . . . H9A H 0.5330 0.2597 0.1334 0.167 Uiso 1 1 calc R . . C10 C 0.313(6) 0.3269(15) 0.105(3) 0.28(3) Uani 1 1 d . . . H10A H 0.3266 0.3088 0.0515 0.335 Uiso 1 1 calc R . . H10B H 0.1864 0.3206 0.1186 0.335 Uiso 1 1 calc R . . C11 C 0.364(19) 0.405(5) 0.111(10) 1.05(14) Uani 1 1 d . . . H11A H 0.2761 0.4358 0.0813 1.261 Uiso 1 1 calc R . . H11B H 0.3656 0.4209 0.1656 1.261 Uiso 1 1 calc R . . C12 C 0.544(7) 0.414(4) 0.079(4) 0.32(5) Uani 1 1 d . . . H12A H 0.5695 0.4653 0.0622 0.388 Uiso 1 1 calc R . . H12B H 0.5700 0.3784 0.0373 0.388 Uiso 1 1 calc R . . C13 C 0.632(5) 0.393(2) 0.162(3) 0.23(3) Uani 1 1 d . . . H13A H 0.6602 0.4390 0.1907 0.271 Uiso 1 1 calc R . . H13B H 0.7463 0.3670 0.1538 0.271 Uiso 1 1 calc R . . C14 C 0.505(6) 0.340(2) 0.215(3) 0.22(2) Uani 1 1 d . . . H14A H 0.5759 0.3170 0.2583 0.269 Uiso 1 1 calc R . . H14B H 0.4073 0.3691 0.2373 0.269 Uiso 1 1 calc R . . C15 C 0.381(4) 0.175(2) 0.2927(15) 0.139(12) Uani 1 1 d . . . H15A H 0.3826 0.2177 0.3294 0.167 Uiso 1 1 calc R . . C16 C 0.271(7) 0.111(4) 0.331(2) 0.33(4) Uani 1 1 d . . . H16A H 0.2747 0.0653 0.3003 0.399 Uiso 1 1 calc R . . H16B H 0.1460 0.1260 0.3380 0.399 Uiso 1 1 calc R . . C17 C 0.381(16) 0.102(3) 0.415(2) 0.44(8) Uani 1 1 d . . . H17A H 0.4110 0.1517 0.4368 0.533 Uiso 1 1 calc R . . H17B H 0.3062 0.0761 0.4524 0.533 Uiso 1 1 calc R . . C18 C 0.550(6) 0.059(3) 0.403(4) 0.29(4) Uani 1 1 d . . . H18A H 0.5377 0.0210 0.3619 0.344 Uiso 1 1 calc R . . H18B H 0.6035 0.0377 0.4512 0.344 Uiso 1 1 calc R . . C19 C 0.650(4) 0.138(2) 0.3741(17) 0.180(18) Uani 1 1 d . . . H19A H 0.7803 0.1305 0.3697 0.215 Uiso 1 1 calc R . . H19B H 0.6288 0.1789 0.4102 0.215 Uiso 1 1 calc R . . C20 C 0.549(4) 0.153(2) 0.286(2) 0.163(15) Uani 1 1 d . . . H20A H 0.6163 0.1908 0.2581 0.196 Uiso 1 1 calc R . . H20B H 0.5510 0.1066 0.2553 0.196 Uiso 1 1 calc R . . C21 C -0.034(3) 0.0683(13) 0.1732(13) 0.062(7) Uiso 1 1 d . . . O1 O -0.0662(17) 0.0518(7) 0.1945(8) 0.049(4) 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 0.0401(9) 0.0784(12) 0.0818(12) -0.0292(10) 0.0039(7) -0.0034(9) P1 0.037(3) 0.116(5) 0.118(5) -0.068(4) 0.000(3) 0.007(3) Br1 0.094(2) 0.150(3) 0.223(4) -0.023(3) -0.031(2) -0.004(2) C1 0.10(2) 0.13(3) 0.16(3) -0.08(3) 0.03(2) -0.03(2) C2 0.075(17) 0.09(2) 0.17(3) -0.11(2) 0.03(2) -0.022(16) C3 0.12(3) 0.13(3) 0.15(3) -0.05(2) 0.07(3) 0.04(2) C4 0.058(14) 0.15(3) 0.069(16) -0.043(17) -0.003(12) 0.026(17) C5 0.089(19) 0.15(3) 0.14(3) -0.05(2) 0.06(2) -0.05(2) C6 0.17(6) 0.13(5) 0.10(4) 0.04(4) -0.01(4) -0.05(4) C7 0.08(2) 0.34(6) 0.32(5) -0.28(5) -0.02(3) 0.01(3) C8 0.11(3) 0.30(5) 0.39(7) -0.26(5) -0.05(4) 0.05(3) C9 0.22(3) 0.033(13) 0.16(2) -0.013(14) -0.11(2) 0.011(17) C10 0.30(5) 0.050(18) 0.47(7) 0.08(3) -0.29(5) -0.06(2) C11 0.92(14) 0.35(6) 1.8(4) 0.69(13) -1.0(2) -0.500 C12 0.18(5) 0.47(10) 0.32(7) 0.29(7) 0.02(5) 0.13(6) C13 0.16(4) 0.17(4) 0.36(7) -0.12(4) 0.08(4) -0.11(3) C14 0.17(4) 0.17(4) 0.32(5) -0.05(4) -0.15(4) 0.02(3) C15 0.075(18) 0.25(4) 0.097(19) -0.02(2) -0.006(15) -0.05(2) C16 0.27(6) 0.57(10) 0.16(4) 0.06(5) -0.01(3) -0.34(7) C17 1.0(2) 0.23(6) 0.08(3) 0.00(3) 0.04(7) -0.16(10) C18 0.18(4) 0.33(8) 0.36(8) 0.24(7) 0.12(5) 0.11(5) C19 0.083(19) 0.34(6) 0.11(2) 0.08(3) 0.028(17) -0.02(3) C20 0.09(2) 0.21(4) 0.19(3) 0.10(3) -0.01(2) -0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C4 2.20(2) . ? Ru1 C3 2.22(3) . ? Ru1 C5 2.22(2) . ? Ru1 C2 2.238(19) . ? Ru1 C21 2.23(2) . ? Ru1 C1 2.26(3) . ? Ru1 P1 2.310(5) . ? Ru1 Br1 2.562(4) . ? P1 C7 1.78(3) . ? P1 C15 1.82(3) . ? P1 C9 1.98(3) . ? C1 C5 1.34(4) . ? C1 C2 1.39(4) . ? C1 C6 1.48(6) . ? C2 C3 1.45(4) . ? C3 C6A 1.36(12) . ? C3 C4 1.44(4) . ? C4 C5 1.35(4) . ? C7 C8 1.26(5) . ? C9 C14 1.44(4) . ? C9 C10 1.50(3) . ? C10 C11 1.44(7) . ? C11 C12 1.46(17) . ? C12 C13 1.58(6) . ? C13 C14 1.63(6) . ? C15 C20 1.31(4) . ? C15 C16 1.54(5) . ? C16 C17 1.62(8) . ? C17 C18 1.48(11) . ? C18 C19 1.66(6) . ? C19 C20 1.66(4) . ? C21 O1 0.53(3) . ? 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 C4 Ru1 C3 38.1(10) . . ? C4 Ru1 C5 35.5(10) . . ? C3 Ru1 C5 59.8(12) . . ? C4 Ru1 C2 61.1(9) . . ? C3 Ru1 C2 37.8(11) . . ? C5 Ru1 C2 56.5(10) . . ? C4 Ru1 C21 133.7(12) . . ? C3 Ru1 C21 100.3(12) . . ? C5 Ru1 C21 156.5(10) . . ? C2 Ru1 C21 100.2(11) . . ? C4 Ru1 C1 62.3(10) . . ? C3 Ru1 C1 63.6(13) . . ? C5 Ru1 C1 34.9(10) . . ? C2 Ru1 C1 36.0(11) . . ? C21 Ru1 C1 127.6(11) . . ? C4 Ru1 P1 92.6(7) . . ? C3 Ru1 P1 117.1(13) . . ? C5 Ru1 P1 106.1(9) . . ? C2 Ru1 P1 153.0(8) . . ? C21 Ru1 P1 93.9(6) . . ? C1 Ru1 P1 138.4(10) . . ? C4 Ru1 Br1 140.9(9) . . ? C3 Ru1 Br1 148.1(12) . . ? C5 Ru1 Br1 106.1(11) . . ? C2 Ru1 Br1 110.3(11) . . ? C21 Ru1 Br1 84.3(6) . . ? C1 Ru1 Br1 88.4(11) . . ? P1 Ru1 Br1 93.79(18) . . ? C7 P1 C15 109(2) . . ? C7 P1 C9 101.5(19) . . ? C15 P1 C9 103.2(11) . . ? C7 P1 Ru1 111.1(10) . . ? C15 P1 Ru1 119.4(12) . . ? C9 P1 Ru1 111.2(8) . . ? C5 C1 C2 101(3) . . ? C5 C1 C6 134(5) . . ? C2 C1 C6 124(4) . . ? C5 C1 Ru1 70.9(16) . . ? C2 C1 Ru1 71.3(17) . . ? C6 C1 Ru1 129(3) . . ? C1 C2 C3 113(3) . . ? C1 C2 Ru1 72.7(15) . . ? C3 C2 Ru1 70.5(13) . . ? C6A C3 C4 88(7) . . ? C6A C3 C2 164(7) . . ? C4 C3 C2 103(3) . . ? C6A C3 Ru1 101(6) . . ? C4 C3 Ru1 70.0(15) . . ? C2 C3 Ru1 71.7(15) . . ? C5 C4 C3 105(3) . . ? C5 C4 Ru1 73.0(14) . . ? C3 C4 Ru1 71.9(14) . . ? C1 C5 C4 118(3) . . ? C1 C5 Ru1 74.2(16) . . ? C4 C5 Ru1 71.5(14) . . ? C8 C7 P1 125(4) . . ? C14 C9 C10 104(2) . . ? C14 C9 P1 119(3) . . ? C10 C9 P1 102(2) . . ? C11 C10 C9 108(4) . . ? C12 C11 C10 109(10) . . ? C11 C12 C13 90(6) . . ? C12 C13 C14 114(3) . . ? C9 C14 C13 105(4) . . ? C20 C15 C16 109(4) . . ? C20 C15 P1 115(2) . . ? C16 C15 P1 110(2) . . ? C15 C16 C17 101(3) . . ? C18 C17 C16 109(5) . . ? C17 C18 C19 89(4) . . ? C18 C19 C20 102(3) . . ? C15 C20 C19 112(3) . . ? O1 C21 Ru1 160(4) . . ? _diffrn_measured_fraction_theta_max 0.855 _diffrn_reflns_theta_full 22.52 _diffrn_measured_fraction_theta_full 0.855 _refine_diff_density_max 1.253 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.158 #===END data_jhn512a _database_code_depnum_ccdc_archive 'CCDC 248580' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 11 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H31 F6 N O P2 Ru' _chemical_formula_weight 614.50 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.281(3) _cell_length_b 11.664(2) _cell_length_c 16.326(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.389(13) _cell_angle_gamma 90.00 _cell_volume 2696.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 5.36 _cell_measurement_theta_max 12.57 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max .40 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9234 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5928 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0847 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4743 _reflns_number_gt 2385 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+0.0000P] 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 0.0004(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4743 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1253 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.89771(4) 0.61482(6) 0.19901(3) 0.0651(3) Uani 1 1 d . . . P1 P 0.96697(12) 0.45678(17) 0.27132(10) 0.0537(5) Uani 1 1 d . . . N1 N 0.8997(4) 0.7032(6) 0.3076(4) 0.0642(17) Uani 1 1 d . . . C1 C 0.9957(16) 0.742(2) 0.1494(9) 0.191(11) Uani 1 1 d . . . C2 C 0.9021(18) 0.7677(12) 0.1200(9) 0.186(10) Uani 1 1 d . . . C3 C 0.8599(8) 0.6819(12) 0.0734(5) 0.115(4) Uani 1 1 d . . . H3A H 0.7962 0.6840 0.0427 0.138 Uiso 1 1 calc R . . C4 C 0.9262(8) 0.5923(8) 0.0716(4) 0.088(3) Uani 1 1 d . . . H4A H 0.9186 0.5220 0.0386 0.105 Uiso 1 1 calc R . . C5 C 1.0087(8) 0.6328(14) 0.1166(6) 0.116(4) Uani 1 1 d . . . H5A H 1.0687 0.5909 0.1238 0.139 Uiso 1 1 calc R . . C6 C 1.0300(14) 0.8499(19) 0.1902(11) 0.104(7) Uani 0.50 1 d P . . C6A C 0.912(3) 0.890(2) 0.1487(17) 0.195(15) Uani 0.50 1 d P . . C7 C 0.9106(5) 0.4270(7) 0.3632(4) 0.070(2) Uani 1 1 d . . . H7A H 0.8951 0.4909 0.3929 0.084 Uiso 1 1 calc R . . C8 C 0.8896(6) 0.3297(9) 0.3921(5) 0.098(3) Uani 1 1 d . . . H8A H 0.9033 0.2625 0.3653 0.117 Uiso 1 1 calc R . . H8B H 0.8607 0.3260 0.4400 0.117 Uiso 1 1 calc R . . C9 C 1.0917(4) 0.4772(6) 0.3126(4) 0.0529(17) Uani 1 1 d . . . H9A H 1.1265 0.4844 0.2648 0.063 Uiso 1 1 calc R . . C10 C 1.1085(4) 0.5891(6) 0.3622(4) 0.062(2) Uani 1 1 d . . . H10A H 1.0750 0.5858 0.4102 0.075 Uiso 1 1 calc R . . H10B H 1.0837 0.6532 0.3283 0.075 Uiso 1 1 calc R . . C11 C 1.2153(5) 0.6079(6) 0.3906(4) 0.068(2) Uani 1 1 d . . . H11A H 1.2478 0.6196 0.3426 0.082 Uiso 1 1 calc R . . H11B H 1.2237 0.6763 0.4246 0.082 Uiso 1 1 calc R . . C12 C 1.2578(5) 0.5062(7) 0.4391(5) 0.079(2) Uani 1 1 d . . . H12A H 1.2303 0.5000 0.4903 0.095 Uiso 1 1 calc R . . H12B H 1.3252 0.5179 0.4530 0.095 Uiso 1 1 calc R . . C13 C 1.2404(5) 0.3955(7) 0.3903(5) 0.082(2) Uani 1 1 d . . . H13A H 1.2654 0.3314 0.4241 0.098 Uiso 1 1 calc R . . H13B H 1.2733 0.3985 0.3419 0.098 Uiso 1 1 calc R . . C14 C 1.1351(5) 0.3769(7) 0.3633(4) 0.073(2) Uani 1 1 d . . . H14A H 1.1262 0.3073 0.3307 0.087 Uiso 1 1 calc R . . H14B H 1.1031 0.3674 0.4118 0.087 Uiso 1 1 calc R . . C15 C 0.9643(4) 0.3184(6) 0.2165(4) 0.0543(18) Uani 1 1 d . . . H15A H 0.9810 0.2582 0.2576 0.065 Uiso 1 1 calc R . . C16 C 1.0351(5) 0.3130(7) 0.1532(4) 0.066(2) Uani 1 1 d . . . H16A H 1.0197 0.3720 0.1118 0.079 Uiso 1 1 calc R . . H16B H 1.0980 0.3285 0.1810 0.079 Uiso 1 1 calc R . . C17 C 1.0344(5) 0.1967(7) 0.1110(4) 0.075(2) Uani 1 1 d . . . H17A H 1.0532 0.1377 0.1517 0.090 Uiso 1 1 calc R . . H17B H 1.0792 0.1967 0.0711 0.090 Uiso 1 1 calc R . . C18 C 0.9358(5) 0.1712(8) 0.0677(5) 0.094(3) Uani 1 1 d . . . H18A H 0.9349 0.0959 0.0424 0.112 Uiso 1 1 calc R . . H18B H 0.9189 0.2272 0.0244 0.112 Uiso 1 1 calc R . . C19 C 0.8635(5) 0.1751(8) 0.1297(5) 0.093(3) Uani 1 1 d . . . H19A H 0.8008 0.1603 0.1011 0.111 Uiso 1 1 calc R . . H19B H 0.8781 0.1158 0.1710 0.111 Uiso 1 1 calc R . . C20 C 0.8646(5) 0.2919(7) 0.1721(4) 0.075(2) Uani 1 1 d . . . H20A H 0.8196 0.2921 0.2119 0.090 Uiso 1 1 calc R . . H20B H 0.8459 0.3509 0.1313 0.090 Uiso 1 1 calc R . . C21 C 0.7795(6) 0.5531(8) 0.2043(5) 0.081(2) Uani 1 1 d . . . C22 C 0.9074(5) 0.7624(7) 0.3631(5) 0.067(2) Uani 1 1 d . . . C23 C 0.9185(6) 0.8381(8) 0.4353(5) 0.101(4) Uani 1 1 d . . . H23A H 0.870(2) 0.8299(9) 0.4626(15) 0.151 Uiso 1 1 calc R . . H23B H 0.9216(6) 0.909(4) 0.4192(9) 0.151 Uiso 1 1 calc R . . H23C H 0.970(3) 0.8203(12) 0.4673(17) 0.151 Uiso 1 1 calc R . . O1 O 0.7048(4) 0.5152(7) 0.2010(4) 0.123(3) Uani 1 1 d . . . P2 P 1.1843(3) 0.0029(3) 0.38288(19) 0.1180(10) Uani 1 1 d . . . F1 F 1.2656(8) -0.0699(11) 0.3702(9) 0.311(7) Uani 1 1 d . . . F2 F 1.2398(6) 0.0838(8) 0.4484(5) 0.213(4) Uani 1 1 d . . . F3 F 1.0909(5) 0.0693(7) 0.3786(5) 0.184(3) Uani 1 1 d . . . F4 F 1.1264(13) -0.0906(13) 0.3296(10) 0.373(9) Uani 1 1 d . . . F5 F 1.2111(10) 0.0734(9) 0.3104(6) 0.305(7) Uani 1 1 d . . . F6 F 1.1553(6) -0.0701(7) 0.4558(5) 0.194(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0720(4) 0.0763(5) 0.0464(3) -0.0011(3) 0.0051(3) -0.0005(4) P1 0.0499(10) 0.0712(13) 0.0408(9) -0.0042(9) 0.0089(8) -0.0099(10) N1 0.056(4) 0.076(5) 0.061(4) -0.001(3) 0.009(3) 0.014(3) C1 0.29(2) 0.22(2) 0.070(9) -0.019(11) 0.071(12) -0.17(2) C2 0.44(3) 0.063(8) 0.076(9) 0.001(7) 0.097(15) -0.022(16) C3 0.145(9) 0.151(10) 0.049(5) 0.037(6) 0.012(5) 0.070(9) C4 0.123(8) 0.100(7) 0.042(4) 0.008(4) 0.017(5) 0.018(6) C5 0.096(7) 0.204(14) 0.053(5) 0.045(7) 0.026(5) 0.000(9) C6 0.106(14) 0.107(16) 0.094(13) 0.006(12) -0.008(11) -0.064(13) C6A 0.38(5) 0.076(16) 0.15(2) 0.012(15) 0.09(3) 0.10(2) C7 0.066(5) 0.093(6) 0.054(4) -0.002(4) 0.016(4) -0.011(5) C8 0.113(7) 0.120(8) 0.065(5) -0.007(6) 0.034(5) -0.034(7) C9 0.054(4) 0.052(4) 0.051(4) 0.000(3) 0.001(3) -0.006(4) C10 0.043(4) 0.080(6) 0.061(4) -0.007(4) -0.002(3) -0.001(4) C11 0.069(5) 0.064(5) 0.069(4) -0.002(4) -0.002(4) -0.013(4) C12 0.063(5) 0.086(6) 0.081(5) 0.003(5) -0.019(4) -0.011(5) C13 0.074(5) 0.080(6) 0.085(5) 0.017(5) -0.015(4) 0.010(5) C14 0.073(5) 0.065(5) 0.075(5) 0.011(4) -0.011(4) -0.005(4) C15 0.048(4) 0.067(5) 0.050(4) -0.002(4) 0.012(3) -0.017(4) C16 0.047(4) 0.085(6) 0.067(4) -0.017(4) 0.012(3) -0.009(4) C17 0.069(5) 0.079(6) 0.079(5) -0.018(5) 0.017(4) -0.004(5) C18 0.085(6) 0.117(7) 0.082(5) -0.050(5) 0.025(5) -0.034(6) C19 0.067(5) 0.127(8) 0.086(6) -0.030(6) 0.017(4) -0.042(5) C20 0.052(4) 0.105(7) 0.068(4) -0.026(5) 0.012(4) -0.020(5) C21 0.066(5) 0.094(7) 0.079(5) -0.028(5) -0.008(4) -0.002(5) C22 0.055(5) 0.076(6) 0.071(5) 0.007(5) 0.012(4) 0.015(4) C23 0.118(8) 0.108(8) 0.074(5) -0.031(6) 0.005(5) 0.015(6) O1 0.065(4) 0.165(7) 0.135(6) -0.049(5) 0.001(4) -0.016(4) P2 0.147(3) 0.117(2) 0.100(2) -0.004(2) 0.050(2) 0.033(2) F1 0.253(11) 0.296(12) 0.433(17) 0.067(12) 0.237(12) 0.159(10) F2 0.217(8) 0.229(9) 0.198(8) -0.088(7) 0.043(6) -0.062(7) F3 0.143(6) 0.187(7) 0.218(8) -0.006(6) 0.008(5) 0.072(5) F4 0.49(3) 0.269(16) 0.357(19) -0.133(14) 0.057(17) 0.015(16) F5 0.517(19) 0.246(11) 0.196(8) 0.100(8) 0.212(11) 0.112(12) F6 0.222(8) 0.196(7) 0.180(7) 0.068(6) 0.091(6) 0.027(6) _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 C21 1.848(9) . ? Ru1 N1 2.048(6) . ? Ru1 C4 2.186(7) . ? Ru1 C3 2.196(7) . ? Ru1 C2 2.207(12) . ? Ru1 C5 2.216(8) . ? Ru1 C1 2.261(15) . ? Ru1 P1 2.339(2) . ? P1 C7 1.825(7) . ? P1 C9 1.837(6) . ? P1 C15 1.844(7) . ? N1 C22 1.134(8) . ? C1 C2 1.39(3) . ? C1 C5 1.41(2) . ? C1 C6 1.48(3) . ? C2 C3 1.351(18) . ? C2 C6A 1.51(3) . ? C3 C4 1.414(12) . ? C4 C5 1.388(13) . ? C6 C6A 1.80(4) . ? C7 C8 1.280(11) . ? C9 C14 1.519(9) . ? C9 C10 1.538(8) . ? C10 C11 1.552(9) . ? C11 C12 1.510(9) . ? C12 C13 1.522(10) . ? C13 C14 1.527(10) . ? C15 C16 1.537(8) . ? C15 C20 1.543(8) . ? C16 C17 1.521(9) . ? C17 C18 1.523(10) . ? C18 C19 1.537(9) . ? C19 C20 1.527(11) . ? C21 O1 1.150(9) . ? C22 C23 1.465(10) . ? P2 F1 1.474(8) . ? P2 F5 1.530(8) . ? P2 F3 1.537(7) . ? P2 F6 1.562(7) . ? P2 F2 1.563(8) . ? P2 F4 1.563(15) . ? 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 C21 Ru1 N1 93.8(3) . . ? C21 Ru1 C4 106.3(4) . . ? N1 Ru1 C4 154.2(3) . . ? C21 Ru1 C3 93.8(4) . . ? N1 Ru1 C3 127.1(4) . . ? C4 Ru1 C3 37.6(3) . . ? C21 Ru1 C2 115.9(7) . . ? N1 Ru1 C2 95.8(4) . . ? C4 Ru1 C2 61.2(4) . . ? C3 Ru1 C2 35.7(5) . . ? C21 Ru1 C5 142.6(5) . . ? N1 Ru1 C5 123.1(4) . . ? C4 Ru1 C5 36.7(3) . . ? C3 Ru1 C5 60.6(4) . . ? C2 Ru1 C5 59.5(6) . . ? C21 Ru1 C1 152.1(7) . . ? N1 Ru1 C1 92.2(5) . . ? C4 Ru1 C1 62.5(5) . . ? C3 Ru1 C1 61.4(5) . . ? C2 Ru1 C1 36.3(7) . . ? C5 Ru1 C1 36.6(5) . . ? C21 Ru1 P1 90.0(3) . . ? N1 Ru1 P1 90.11(17) . . ? C4 Ru1 P1 105.5(3) . . ? C3 Ru1 P1 142.1(3) . . ? C2 Ru1 P1 152.9(6) . . ? C5 Ru1 P1 95.3(3) . . ? C1 Ru1 P1 117.2(7) . . ? C7 P1 C9 103.5(3) . . ? C7 P1 C15 104.4(3) . . ? C9 P1 C15 104.5(3) . . ? C7 P1 Ru1 111.2(3) . . ? C9 P1 Ru1 114.2(2) . . ? C15 P1 Ru1 117.6(2) . . ? C22 N1 Ru1 171.1(6) . . ? C2 C1 C5 103.3(15) . . ? C2 C1 C6 103(3) . . ? C5 C1 C6 153(2) . . ? C2 C1 Ru1 69.7(9) . . ? C5 C1 Ru1 70.0(8) . . ? C6 C1 Ru1 125.7(12) . . ? C3 C2 C1 112.0(18) . . ? C3 C2 C6A 154(2) . . ? C1 C2 C6A 93(3) . . ? C3 C2 Ru1 71.7(7) . . ? C1 C2 Ru1 74.0(10) . . ? C6A C2 Ru1 126.4(13) . . ? C2 C3 C4 107.9(13) . . ? C2 C3 Ru1 72.6(6) . . ? C4 C3 Ru1 70.8(4) . . ? C5 C4 C3 105.3(10) . . ? C5 C4 Ru1 72.8(5) . . ? C3 C4 Ru1 71.6(4) . . ? C4 C5 C1 111.5(13) . . ? C4 C5 Ru1 70.4(5) . . ? C1 C5 Ru1 73.5(7) . . ? C1 C6 C6A 79.2(14) . . ? C2 C6A C6 85.1(16) . . ? C8 C7 P1 128.4(7) . . ? C14 C9 C10 109.9(5) . . ? C14 C9 P1 114.1(5) . . ? C10 C9 P1 112.4(4) . . ? C9 C10 C11 111.0(5) . . ? C12 C11 C10 111.0(6) . . ? C11 C12 C13 111.4(6) . . ? C12 C13 C14 111.1(7) . . ? C9 C14 C13 111.5(6) . . ? C16 C15 C20 108.9(5) . . ? C16 C15 P1 112.8(5) . . ? C20 C15 P1 111.3(5) . . ? C17 C16 C15 112.0(6) . . ? C16 C17 C18 109.7(6) . . ? C17 C18 C19 110.4(6) . . ? C20 C19 C18 110.9(7) . . ? C19 C20 C15 110.3(6) . . ? O1 C21 Ru1 174.8(8) . . ? N1 C22 C23 179.3(9) . . ? F1 P2 F5 85.5(6) . . ? F1 P2 F3 168.2(8) . . ? F5 P2 F3 89.8(6) . . ? F1 P2 F6 94.8(6) . . ? F5 P2 F6 178.9(8) . . ? F3 P2 F6 89.7(5) . . ? F1 P2 F2 96.0(8) . . ? F5 P2 F2 92.8(7) . . ? F3 P2 F2 95.1(5) . . ? F6 P2 F2 88.2(5) . . ? F1 P2 F4 83.7(7) . . ? F5 P2 F4 96.4(8) . . ? F3 P2 F4 86.1(7) . . ? F6 P2 F4 82.5(7) . . ? F2 P2 F4 170.7(8) . . ? _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.883 _refine_diff_density_max 0.499 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.080 #===END data_jhn413a _database_code_depnum_ccdc_archive 'CCDC 248581' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 12 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H31 F6 N O P2 Ru' _chemical_formula_weight 662.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 P2(1)/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 13.309(4) _cell_length_b 14.461(4) _cell_length_c 15.945(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.71(4) _cell_angle_gamma 90.00 _cell_volume 2906.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 8.62 _exptl_crystal_description shard _exptl_crystal_colour pale_yellow _exptl_crystal_size_max .42 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8128 _exptl_absorpt_correction_T_max 0.9848 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6334 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.1553 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5121 _reflns_number_gt 2617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.0000P] 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 5121 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1710 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.1965 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.807 _refine_ls_shift/su_mean 0.052 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 1.48414(6) 0.13403(6) 1.35055(5) 0.0380(3) Uani 1 1 d . . . P1 P 1.4705(2) 0.0643(2) 1.21453(16) 0.0427(7) Uani 1 1 d . . . N1 N 1.6366(7) 0.0805(6) 1.4004(5) 0.047(2) Uani 1 1 d . . . O1 O 1.3685(7) -0.0262(6) 1.3968(6) 0.079(3) Uani 1 1 d . . . C1 C 1.3636(8) 0.2412(8) 1.3415(8) 0.054(3) Uani 1 1 d . . . C2 C 1.4343(9) 0.2795(8) 1.3020(7) 0.058(3) Uani 1 1 d . . . C3 C 1.5370(9) 0.2840(7) 1.3670(7) 0.050(3) Uani 1 1 d . . . C4 C 1.5270(10) 0.2491(8) 1.4473(7) 0.063(3) Uani 1 1 d . . . C5 C 1.4202(10) 0.2258(8) 1.4338(8) 0.058(3) Uani 1 1 d . . . C6 C 1.2453(9) 0.2415(10) 1.3011(10) 0.099(5) Uani 1 1 d . . . H6A H 1.2180 0.3006 1.3106 0.148 Uiso 1 1 calc R . . H6B H 1.2155 0.1942 1.3282 0.148 Uiso 1 1 calc R . . H6C H 1.2265 0.2298 1.2387 0.148 Uiso 1 1 calc R . . C7 C 1.4044(11) 0.3216(8) 1.2104(7) 0.082(4) Uani 1 1 d . . . H7A H 1.3873 0.3857 1.2133 0.123 Uiso 1 1 calc R . . H7B H 1.3441 0.2896 1.1717 0.123 Uiso 1 1 calc R . . H7C H 1.4630 0.3161 1.1879 0.123 Uiso 1 1 calc R . . C8 C 1.6364(9) 0.3248(9) 1.3560(10) 0.091(5) Uani 1 1 d . . . H8A H 1.6382 0.3901 1.3671 0.137 Uiso 1 1 calc R . . H8B H 1.6368 0.3141 1.2967 0.137 Uiso 1 1 calc R . . H8C H 1.6975 0.2961 1.3972 0.137 Uiso 1 1 calc R . . C9 C 1.6131(12) 0.2497(10) 1.5359(8) 0.118(6) Uani 1 1 d . . . H9A H 1.6138 0.3085 1.5640 0.178 Uiso 1 1 calc R . . H9B H 1.6805 0.2393 1.5276 0.178 Uiso 1 1 calc R . . H9C H 1.5998 0.2016 1.5725 0.178 Uiso 1 1 calc R . . C10 C 1.3705(12) 0.1953(10) 1.5026(9) 0.105(5) Uani 1 1 d . . . H10A H 1.3496 0.2487 1.5287 0.158 Uiso 1 1 calc R . . H10B H 1.4211 0.1600 1.5478 0.158 Uiso 1 1 calc R . . H10C H 1.3093 0.1578 1.4749 0.158 Uiso 1 1 calc R . . C11 C 1.5513(9) -0.0417(11) 1.2270(8) 0.076(4) Uani 1 1 d . . . H11A H 1.5303 -0.0887 1.2575 0.091 Uiso 1 1 calc R . . C12 C 1.6250(15) -0.0616(15) 1.2039(12) 0.157(8) Uani 1 1 d . . . H12A H 1.6518 -0.0190 1.1729 0.188 Uiso 1 1 calc R . . H12B H 1.6557 -0.1198 1.2167 0.188 Uiso 1 1 calc R . . C13 C 1.3417(8) 0.0187(6) 1.1459(6) 0.039(2) Uani 1 1 d . . . C14 C 1.2517(8) 0.0313(7) 1.1684(6) 0.047(3) Uani 1 1 d . . . H14A H 1.2555 0.0626 1.2202 0.056 Uiso 1 1 calc R . . C15 C 1.1534(8) -0.0027(8) 1.1136(8) 0.060(3) Uani 1 1 d . . . H15A H 1.0920 0.0049 1.1287 0.072 Uiso 1 1 calc R . . C16 C 1.1514(10) -0.0479(8) 1.0367(7) 0.061(3) Uani 1 1 d . . . H16A H 1.0868 -0.0693 0.9989 0.074 Uiso 1 1 calc R . . C17 C 1.2404(10) -0.0621(8) 1.0143(7) 0.066(3) Uani 1 1 d . . . H17A H 1.2367 -0.0928 0.9622 0.079 Uiso 1 1 calc R . . C18 C 1.3347(9) -0.0308(8) 1.0691(7) 0.059(3) Uani 1 1 d . . . H18A H 1.3962 -0.0426 1.0551 0.071 Uiso 1 1 calc R . . C19 C 1.5134(8) 0.1383(8) 1.1401(6) 0.052(2) Uani 1 1 d . . . C20 C 1.4492(8) 0.1631(7) 1.0557(7) 0.053(3) Uani 1 1 d . . . H20A H 1.3812 0.1384 1.0340 0.064 Uiso 1 1 calc R . . C21 C 1.4825(11) 0.2226(9) 1.0035(8) 0.073(4) Uani 1 1 d . . . H21A H 1.4370 0.2403 0.9483 0.087 Uiso 1 1 calc R . . C22 C 1.5840(13) 0.2555(10) 1.0341(10) 0.084(4) Uani 1 1 d . . . H22A H 1.6081 0.2948 0.9985 0.100 Uiso 1 1 calc R . . C23 C 1.6501(10) 0.2322(11) 1.1151(9) 0.085(4) Uani 1 1 d . . . H23A H 1.7188 0.2555 1.1346 0.102 Uiso 1 1 calc R . . C24 C 1.6155(9) 0.1732(9) 1.1697(8) 0.064(3) Uani 1 1 d . . . H24A H 1.6608 0.1575 1.2255 0.077 Uiso 1 1 calc R . . C25 C 1.4180(9) 0.0312(8) 1.3782(6) 0.051(3) Uani 1 1 d . . . C26 C 1.7212(9) 0.0576(8) 1.4342(7) 0.056(3) Uani 1 1 d . . . C27 C 1.8283(9) 0.0295(10) 1.4806(9) 0.094(5) Uani 1 1 d . . . H27A H 1.8739 0.0827 1.4921 0.141 Uiso 1 1 calc R . . H27B H 1.8515 -0.0138 1.4450 0.141 Uiso 1 1 calc R . . H27C H 1.8312 0.0009 1.5357 0.141 Uiso 1 1 calc R . . P2 P 1.4498(3) 0.3928(4) 0.7760(3) 0.0919(14) Uani 1 1 d . . . F1 F 1.3980(19) 0.365(2) 0.6907(8) 0.381(16) Uani 1 1 d . . . F2 F 1.3619(7) 0.3461(8) 0.8083(7) 0.151(4) Uani 1 1 d . . . F3 F 1.5378(12) 0.4401(11) 0.7510(11) 0.238(7) Uani 1 1 d . . . F4 F 1.5020(15) 0.4168(19) 0.8643(8) 0.321(13) Uani 1 1 d . . . F5 F 1.385(2) 0.4741(13) 0.758(2) 0.393(19) Uani 1 1 d . . . F6 F 1.5089(14) 0.3048(12) 0.7929(18) 0.292(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0402(4) 0.0382(4) 0.0309(4) 0.0030(4) 0.0048(3) 0.0022(5) P1 0.0448(16) 0.0466(17) 0.0350(13) 0.0004(12) 0.0106(12) 0.0020(14) N1 0.046(5) 0.048(6) 0.043(5) 0.002(4) 0.007(4) 0.008(5) O1 0.103(7) 0.062(6) 0.082(6) 0.013(5) 0.042(6) -0.016(5) C1 0.045(7) 0.046(7) 0.068(8) -0.010(6) 0.013(6) 0.004(6) C2 0.063(8) 0.049(7) 0.050(7) -0.008(6) 0.003(6) 0.024(6) C3 0.051(7) 0.029(6) 0.063(7) -0.003(5) 0.007(6) 0.006(5) C4 0.071(8) 0.048(7) 0.044(6) -0.006(6) -0.018(6) 0.008(7) C5 0.079(9) 0.044(7) 0.061(7) -0.015(6) 0.035(7) 0.011(7) C6 0.055(8) 0.084(11) 0.151(14) -0.030(10) 0.025(9) 0.013(8) C7 0.119(11) 0.064(8) 0.049(7) 0.021(6) 0.007(7) 0.032(8) C8 0.065(9) 0.054(8) 0.155(14) 0.011(9) 0.036(9) -0.015(7) C9 0.148(14) 0.072(10) 0.074(9) -0.032(8) -0.050(9) 0.012(10) C10 0.172(15) 0.087(11) 0.107(11) 0.014(9) 0.116(11) 0.016(11) C11 0.048(8) 0.119(12) 0.059(7) -0.017(8) 0.015(6) 0.031(8) C12 0.140(18) 0.17(2) 0.135(17) -0.015(15) 0.003(14) 0.059(16) C13 0.056(6) 0.030(6) 0.027(5) -0.001(4) 0.008(5) -0.006(5) C14 0.056(7) 0.037(6) 0.042(6) -0.001(5) 0.009(5) 0.006(5) C15 0.045(7) 0.061(8) 0.071(8) -0.004(7) 0.014(6) -0.010(6) C16 0.062(8) 0.059(8) 0.046(7) 0.002(6) -0.007(6) -0.016(7) C17 0.091(10) 0.056(8) 0.045(6) -0.015(6) 0.011(7) -0.012(8) C18 0.060(7) 0.060(8) 0.057(7) -0.018(6) 0.019(6) -0.020(6) C19 0.059(6) 0.057(6) 0.040(5) -0.009(6) 0.017(5) 0.003(7) C20 0.057(7) 0.057(8) 0.046(6) 0.009(5) 0.018(5) -0.005(6) C21 0.088(10) 0.084(10) 0.049(7) 0.012(7) 0.025(7) 0.000(9) C22 0.111(12) 0.078(10) 0.083(10) 0.021(8) 0.062(10) 0.006(10) C23 0.069(9) 0.115(13) 0.077(9) -0.006(9) 0.033(8) -0.029(9) C24 0.052(7) 0.078(9) 0.057(7) 0.000(7) 0.008(6) 0.001(7) C25 0.069(8) 0.061(8) 0.026(5) 0.010(5) 0.022(5) 0.012(7) C26 0.051(7) 0.064(8) 0.054(7) 0.008(6) 0.017(6) 0.010(7) C27 0.053(8) 0.113(12) 0.102(11) 0.035(9) 0.004(7) 0.021(8) P2 0.071(3) 0.130(4) 0.069(2) 0.030(3) 0.015(2) 0.002(3) F1 0.35(2) 0.67(5) 0.063(7) 0.037(16) -0.015(11) -0.14(3) F2 0.095(6) 0.207(12) 0.156(9) 0.048(8) 0.049(6) -0.005(8) F3 0.236(14) 0.249(16) 0.310(18) 0.022(14) 0.201(15) -0.082(13) F4 0.257(18) 0.54(4) 0.124(10) -0.090(16) 0.006(11) -0.25(2) F5 0.39(3) 0.195(16) 0.75(5) 0.27(3) 0.39(4) 0.19(2) F6 0.200(16) 0.213(17) 0.54(4) 0.03(2) 0.22(2) 0.064(14) _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 C25 1.852(12) . ? Ru1 N1 2.077(9) . ? Ru1 C1 2.201(10) . ? Ru1 C4 2.216(11) . ? Ru1 C5 2.230(10) . ? Ru1 C2 2.266(11) . ? Ru1 C3 2.269(10) . ? Ru1 P1 2.345(3) . ? P1 C19 1.820(11) . ? P1 C13 1.835(10) . ? P1 C11 1.846(14) . ? N1 C26 1.130(12) . ? O1 C25 1.156(12) . ? C1 C2 1.404(15) . ? C1 C5 1.439(15) . ? C1 C6 1.499(14) . ? C2 C3 1.428(14) . ? C2 C7 1.513(14) . ? C3 C4 1.421(15) . ? C3 C8 1.510(15) . ? C4 C5 1.409(15) . ? C4 C9 1.507(14) . ? C5 C10 1.518(14) . ? C11 C12 1.188(18) . ? C13 C14 1.368(13) . ? C13 C18 1.396(13) . ? C14 C15 1.408(13) . ? C15 C16 1.383(14) . ? C16 C17 1.357(15) . ? C17 C18 1.357(14) . ? C19 C24 1.383(14) . ? C19 C20 1.390(13) . ? C20 C21 1.365(14) . ? C21 C22 1.367(16) . ? C22 C23 1.351(17) . ? C23 C24 1.398(16) . ? C26 C27 1.438(15) . ? P2 F1 1.374(15) . ? P2 F4 1.399(12) . ? P2 F5 1.433(14) . ? P2 F6 1.475(16) . ? P2 F3 1.516(11) . ? P2 F2 1.574(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 C25 Ru1 N1 95.2(4) . . ? C25 Ru1 C1 100.9(5) . . ? N1 Ru1 C1 152.8(4) . . ? C25 Ru1 C4 118.2(5) . . ? N1 Ru1 C4 90.7(4) . . ? C1 Ru1 C4 62.4(4) . . ? C25 Ru1 C5 92.0(4) . . ? N1 Ru1 C5 120.4(4) . . ? C1 Ru1 C5 37.9(4) . . ? C4 Ru1 C5 37.0(4) . . ? C25 Ru1 C2 135.8(5) . . ? N1 Ru1 C2 128.3(4) . . ? C1 Ru1 C2 36.6(4) . . ? C4 Ru1 C2 61.5(4) . . ? C5 Ru1 C2 61.7(4) . . ? C25 Ru1 C3 153.3(4) . . ? N1 Ru1 C3 94.8(4) . . ? C1 Ru1 C3 61.8(4) . . ? C4 Ru1 C3 36.9(4) . . ? C5 Ru1 C3 61.7(4) . . ? C2 Ru1 C3 36.7(4) . . ? C25 Ru1 P1 88.5(3) . . ? N1 Ru1 P1 88.3(2) . . ? C1 Ru1 P1 113.8(3) . . ? C4 Ru1 P1 153.2(4) . . ? C5 Ru1 P1 151.1(3) . . ? C2 Ru1 P1 99.0(3) . . ? C3 Ru1 P1 116.5(3) . . ? C19 P1 C13 104.5(4) . . ? C19 P1 C11 105.4(5) . . ? C13 P1 C11 99.6(5) . . ? C19 P1 Ru1 113.8(3) . . ? C13 P1 Ru1 119.1(3) . . ? C11 P1 Ru1 112.8(4) . . ? C26 N1 Ru1 173.1(9) . . ? C2 C1 C5 108.3(10) . . ? C2 C1 C6 124.7(11) . . ? C5 C1 C6 125.0(12) . . ? C2 C1 Ru1 74.2(6) . . ? C5 C1 Ru1 72.1(6) . . ? C6 C1 Ru1 132.3(8) . . ? C1 C2 C3 108.3(10) . . ? C1 C2 C7 125.9(11) . . ? C3 C2 C7 125.2(12) . . ? C1 C2 Ru1 69.2(6) . . ? C3 C2 Ru1 71.8(6) . . ? C7 C2 Ru1 131.3(8) . . ? C4 C3 C2 107.1(10) . . ? C4 C3 C8 125.6(11) . . ? C2 C3 C8 127.1(11) . . ? C4 C3 Ru1 69.5(6) . . ? C2 C3 Ru1 71.5(6) . . ? C8 C3 Ru1 127.6(8) . . ? C5 C4 C3 109.2(9) . . ? C5 C4 C9 124.8(13) . . ? C3 C4 C9 125.5(13) . . ? C5 C4 Ru1 72.1(6) . . ? C3 C4 Ru1 73.6(6) . . ? C9 C4 Ru1 127.2(8) . . ? C4 C5 C1 106.9(10) . . ? C4 C5 C10 127.7(12) . . ? C1 C5 C10 125.3(12) . . ? C4 C5 Ru1 71.0(6) . . ? C1 C5 Ru1 70.0(6) . . ? C10 C5 Ru1 126.6(8) . . ? C12 C11 P1 132.7(17) . . ? C14 C13 C18 118.7(9) . . ? C14 C13 P1 121.7(7) . . ? C18 C13 P1 119.6(8) . . ? C13 C14 C15 120.6(10) . . ? C16 C15 C14 117.7(10) . . ? C17 C16 C15 122.3(11) . . ? C18 C17 C16 119.1(11) . . ? C17 C18 C13 121.5(11) . . ? C24 C19 C20 117.9(10) . . ? C24 C19 P1 118.1(8) . . ? C20 C19 P1 124.0(9) . . ? C21 C20 C19 122.2(11) . . ? C20 C21 C22 118.6(12) . . ? C23 C22 C21 121.4(13) . . ? C22 C23 C24 120.2(12) . . ? C19 C24 C23 119.7(11) . . ? O1 C25 Ru1 172.4(10) . . ? N1 C26 C27 177.7(12) . . ? F1 P2 F4 177.0(15) . . ? F1 P2 F5 88.0(15) . . ? F4 P2 F5 94.1(16) . . ? F1 P2 F6 89.7(15) . . ? F4 P2 F6 88.1(13) . . ? F5 P2 F6 175.4(13) . . ? F1 P2 F3 93.3(10) . . ? F4 P2 F3 88.6(9) . . ? F5 P2 F3 92.6(10) . . ? F6 P2 F3 91.5(9) . . ? F1 P2 F2 90.4(10) . . ? F4 P2 F2 87.6(7) . . ? F5 P2 F2 87.3(8) . . ? F6 P2 F2 88.8(8) . . ? F3 P2 F2 176.2(8) . . ? _diffrn_measured_fraction_theta_max 0.840 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.840 _refine_diff_density_max 0.868 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.108 #===END data_jhn469a _database_code_depnum_ccdc_archive 'CCDC 248582' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 13A _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.50 H33 F6 O1.50 P3 Ru' _chemical_formula_weight 791.60 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.8398(18) _cell_length_b 19.6539(18) _cell_length_c 16.9986(15) _cell_angle_alpha 90.00 _cell_angle_beta 104.883(9) _cell_angle_gamma 90.00 _cell_volume 3500.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 3.88 _cell_measurement_theta_max 12.51 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .44 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1604 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8516 _exptl_absorpt_correction_T_max 0.9673 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7676 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0865 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6169 _reflns_number_gt 3652 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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 6169 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1895 _refine_ls_wR_factor_gt 0.1565 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.86855(6) 0.83299(3) 0.61994(4) 0.0481(2) Uani 1 1 d . . . P1 P 0.70713(18) 0.89891(9) 0.54047(11) 0.0458(5) Uani 1 1 d . . . P2 P 0.87188(19) 0.92081(9) 0.70766(11) 0.0460(5) Uani 1 1 d . . . C1 C 0.9693(9) 0.7316(4) 0.6412(6) 0.072(2) Uani 1 1 d . . . C2 C 0.9365(14) 0.7501(4) 0.7120(6) 0.094(4) Uani 1 1 d . . . H2A H 0.9945 0.7552 0.7663 0.113 Uiso 1 1 calc R . . C3 C 0.8009(14) 0.7536(5) 0.6915(8) 0.091(4) Uani 1 1 d . . . H3A H 0.7493 0.7620 0.7302 0.109 Uiso 1 1 calc R . . C4 C 0.7534(11) 0.7371(4) 0.6107(9) 0.099(4) Uani 1 1 d . . . H4A H 0.6629 0.7322 0.5823 0.119 Uiso 1 1 calc R . . C5 C 0.8569(12) 0.7245(4) 0.5772(6) 0.085(3) Uani 1 1 d . . . H5A H 0.8519 0.7089 0.5217 0.102 Uiso 1 1 calc R . . C6 C 1.0998(11) 0.7158(6) 0.6345(9) 0.139(5) Uani 1 1 d . . . H6A H 1.1184 0.6688 0.6473 0.209 Uiso 1 1 calc R . . H6B H 1.1604 0.7438 0.6718 0.209 Uiso 1 1 calc R . . H6C H 1.1052 0.7247 0.5799 0.209 Uiso 1 1 calc R . . C7 C 0.7177(7) 0.9654(4) 0.6882(4) 0.0482(18) Uani 1 1 d . . . H7A H 0.6472 0.9385 0.6982 0.058 Uiso 1 1 calc R . . C8 C 0.7086(7) 0.9808(3) 0.5964(4) 0.0479(17) Uani 1 1 d . . . H8A H 0.6348 1.0094 0.5716 0.057 Uiso 1 1 calc R . . C9 C 0.8376(7) 1.0164(3) 0.5971(4) 0.0497(18) Uani 1 1 d . . . H9A H 0.8758 0.9959 0.5571 0.060 Uiso 1 1 calc R . . H9B H 0.8242 1.0645 0.5848 0.060 Uiso 1 1 calc R . . C10 C 0.9247(7) 1.0063(4) 0.6842(4) 0.0500(18) Uani 1 1 d . . . H10A H 1.0165 1.0119 0.6904 0.060 Uiso 1 1 calc R . . C11 C 0.8666(8) 1.0500(3) 0.7390(4) 0.0532(19) Uani 1 1 d . . . C12 C 0.9397(9) 1.1116(4) 0.7811(5) 0.076(3) Uani 1 1 d . . . H12A H 0.8909 1.1338 0.8135 0.114 Uiso 1 1 calc R . . H12B H 0.9541 1.1428 0.7409 0.114 Uiso 1 1 calc R . . H12C H 1.0202 1.0972 0.8155 0.114 Uiso 1 1 calc R . . C13 C 0.7503(7) 1.0286(4) 0.7388(4) 0.0489(18) Uani 1 1 d . . . C14 C 0.6584(8) 1.0589(4) 0.7818(5) 0.072(2) Uani 1 1 d . . . H14A H 0.6952 1.0990 0.8107 0.108 Uiso 1 1 calc R . . H14B H 0.6408 1.0263 0.8197 0.108 Uiso 1 1 calc R . . H14C H 0.5804 1.0706 0.7427 0.108 Uiso 1 1 calc R . . C15 C 0.9341(8) 0.9083(4) 0.8158(5) 0.059(2) Uani 1 1 d . . . C16 C 0.8561(10) 0.8970(5) 0.8655(5) 0.085(3) Uani 1 1 d . . . H16A H 0.7681 0.8950 0.8440 0.102 Uiso 1 1 calc R . . C17 C 0.9089(16) 0.8883(7) 0.9495(8) 0.133(5) Uani 1 1 d . . . H17A H 0.8555 0.8824 0.9839 0.159 Uiso 1 1 calc R . . C18 C 1.0365(19) 0.8885(8) 0.9802(8) 0.147(6) Uani 1 1 d . . . H18A H 1.0708 0.8813 1.0356 0.177 Uiso 1 1 calc R . . C19 C 1.1168(14) 0.8993(8) 0.9303(8) 0.140(5) Uani 1 1 d . . . H19A H 1.2047 0.9017 0.9518 0.168 Uiso 1 1 calc R . . C20 C 1.0638(10) 0.9066(6) 0.8475(6) 0.097(3) Uani 1 1 d . . . H20A H 1.1172 0.9104 0.8127 0.116 Uiso 1 1 calc R . . C21 C 0.5469(7) 0.8628(4) 0.5207(5) 0.0515(18) Uani 1 1 d . . . C22 C 0.4966(8) 0.8423(4) 0.5836(5) 0.067(2) Uani 1 1 d . . . H22A H 0.5436 0.8481 0.6373 0.081 Uiso 1 1 calc R . . C23 C 0.3756(9) 0.8128(5) 0.5672(6) 0.077(3) Uani 1 1 d . . . H23A H 0.3420 0.8004 0.6103 0.092 Uiso 1 1 calc R . . C24 C 0.3052(9) 0.8016(5) 0.4889(6) 0.079(3) Uani 1 1 d . . . H24A H 0.2253 0.7811 0.4788 0.094 Uiso 1 1 calc R . . C25 C 0.3537(9) 0.8209(5) 0.4269(6) 0.078(3) Uani 1 1 d . . . H25A H 0.3065 0.8136 0.3736 0.094 Uiso 1 1 calc R . . C26 C 0.4735(8) 0.8517(4) 0.4412(5) 0.065(2) Uani 1 1 d . . . H26A H 0.5047 0.8650 0.3975 0.077 Uiso 1 1 calc R . . C27 C 0.7174(7) 0.9242(4) 0.4389(4) 0.0511(18) Uani 1 1 d . . . C28 C 0.6740(8) 0.9857(5) 0.4052(5) 0.068(2) Uani 1 1 d . . . H28A H 0.6419 1.0177 0.4351 0.081 Uiso 1 1 calc R . . C29 C 0.6780(8) 1.0001(6) 0.3255(5) 0.079(3) Uani 1 1 d . . . H29A H 0.6485 1.0419 0.3027 0.095 Uiso 1 1 calc R . . C30 C 0.7241(9) 0.9542(6) 0.2810(5) 0.078(3) Uani 1 1 d . . . H30A H 0.7257 0.9645 0.2278 0.094 Uiso 1 1 calc R . . C31 C 0.7682(9) 0.8930(6) 0.3143(5) 0.080(3) Uani 1 1 d . . . H31A H 0.7989 0.8610 0.2837 0.096 Uiso 1 1 calc R . . C32 C 0.7672(7) 0.8790(4) 0.3930(5) 0.062(2) Uani 1 1 d . . . H32A H 0.8008 0.8379 0.4161 0.074 Uiso 1 1 calc R . . C33 C 0.9922(9) 0.8739(4) 0.5768(5) 0.066(2) Uani 1 1 d . . . O1 O 1.0680(6) 0.8964(4) 0.5499(4) 0.093(2) Uani 1 1 d . . . P3 P 0.4709(3) 0.81153(18) 0.83584(19) 0.0992(10) Uani 1 1 d . . . F1 F 0.5752(13) 0.7810(7) 0.8018(8) 0.257(6) Uani 1 1 d . . . F2 F 0.4744(15) 0.7437(7) 0.8800(7) 0.269(7) Uani 1 1 d . . . F3 F 0.5746(10) 0.8344(5) 0.9119(5) 0.191(4) Uani 1 1 d . . . F4 F 0.3756(11) 0.8374(10) 0.8737(8) 0.327(10) Uani 1 1 d . . . F5 F 0.4946(13) 0.8741(5) 0.7936(6) 0.245(6) Uani 1 1 d . . . F6 F 0.3750(11) 0.7860(10) 0.7635(5) 0.318(10) Uani 1 1 d . . . O2 O 0.5000 1.0000 1.0000 0.49(4) Uani 1 2 d S . . C35 C 0.438(5) 1.040(3) 0.936(2) 0.120(16) Uani 0.50 1 d P . . C36 C 0.362(8) 1.023(3) 0.993(4) 0.18(3) Uani 0.50 1 d P . . C35A C 0.516(6) 1.047(2) 0.947(2) 0.102(10) Uani 0.50 1 d P . . C36A C 0.342(5) 1.032(2) 0.9470(18) 0.229(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0577(4) 0.0347(3) 0.0563(4) 0.0037(3) 0.0227(3) 0.0026(3) P1 0.0514(11) 0.0422(10) 0.0466(11) 0.0006(8) 0.0178(9) 0.0006(9) P2 0.0511(11) 0.0389(10) 0.0504(11) 0.0012(8) 0.0171(9) -0.0012(9) C1 0.074(6) 0.047(5) 0.094(7) 0.012(5) 0.018(6) 0.004(5) C2 0.169(13) 0.046(5) 0.068(6) 0.019(5) 0.032(7) 0.007(7) C3 0.144(11) 0.042(5) 0.114(9) -0.002(5) 0.082(9) -0.004(6) C4 0.091(8) 0.030(4) 0.177(13) 0.010(6) 0.035(8) -0.020(5) C5 0.130(9) 0.034(4) 0.090(7) -0.005(4) 0.027(7) -0.004(5) C6 0.092(9) 0.094(9) 0.234(16) 0.042(10) 0.046(9) 0.032(7) C7 0.044(4) 0.049(4) 0.054(4) 0.000(3) 0.019(4) -0.004(3) C8 0.061(5) 0.036(4) 0.052(4) 0.001(3) 0.026(4) 0.008(3) C9 0.064(5) 0.031(4) 0.059(5) 0.005(3) 0.024(4) -0.004(3) C10 0.047(4) 0.044(4) 0.064(5) -0.005(4) 0.021(4) -0.007(3) C11 0.065(5) 0.036(4) 0.059(5) -0.003(3) 0.018(4) -0.005(4) C12 0.088(7) 0.055(5) 0.088(6) -0.023(5) 0.030(5) -0.008(5) C13 0.058(5) 0.042(4) 0.050(4) -0.001(3) 0.020(4) 0.005(4) C14 0.071(6) 0.069(6) 0.082(6) -0.027(5) 0.031(5) -0.002(5) C15 0.062(5) 0.062(5) 0.052(5) 0.007(4) 0.016(4) 0.007(4) C16 0.095(7) 0.097(7) 0.063(6) 0.020(5) 0.023(5) 0.005(6) C17 0.162(13) 0.152(13) 0.096(10) 0.053(9) 0.057(9) 0.064(11) C18 0.187(17) 0.185(16) 0.061(8) 0.025(9) 0.016(10) 0.065(14) C19 0.121(11) 0.187(15) 0.083(9) 0.013(9) -0.027(8) 0.027(10) C20 0.081(7) 0.129(10) 0.077(7) 0.023(6) 0.013(6) 0.010(7) C21 0.052(5) 0.044(4) 0.061(5) -0.012(4) 0.019(4) -0.001(4) C22 0.068(5) 0.078(6) 0.059(5) -0.012(4) 0.022(4) -0.018(5) C23 0.073(6) 0.088(7) 0.081(6) -0.015(5) 0.041(5) -0.020(5) C24 0.070(6) 0.068(6) 0.102(8) -0.019(6) 0.031(6) -0.013(5) C25 0.062(6) 0.085(7) 0.080(6) -0.011(5) 0.003(5) -0.009(5) C26 0.071(6) 0.063(5) 0.064(5) -0.004(4) 0.025(5) -0.003(4) C27 0.061(5) 0.053(4) 0.045(4) 0.003(3) 0.025(4) -0.004(4) C28 0.069(6) 0.073(6) 0.059(5) 0.012(4) 0.012(4) -0.005(5) C29 0.064(6) 0.099(7) 0.069(6) 0.032(6) 0.004(5) -0.014(5) C30 0.065(6) 0.125(9) 0.045(5) 0.012(6) 0.013(4) -0.017(6) C31 0.070(6) 0.115(9) 0.059(6) -0.009(6) 0.025(5) -0.007(6) C32 0.058(5) 0.077(6) 0.055(5) 0.004(4) 0.023(4) 0.004(4) C33 0.066(6) 0.054(5) 0.082(6) -0.005(4) 0.028(5) 0.006(4) O1 0.069(4) 0.101(5) 0.124(6) 0.014(4) 0.052(4) -0.002(4) P3 0.115(3) 0.115(3) 0.0772(19) 0.0057(17) 0.0426(19) -0.011(2) F1 0.296(14) 0.246(14) 0.286(13) -0.070(11) 0.180(12) 0.019(11) F2 0.345(17) 0.241(13) 0.206(10) 0.061(10) 0.045(11) -0.153(13) F3 0.213(9) 0.230(11) 0.121(6) -0.021(6) 0.026(7) -0.027(8) F4 0.166(10) 0.59(3) 0.249(13) -0.043(15) 0.093(9) 0.169(14) F5 0.319(15) 0.148(8) 0.229(11) 0.112(8) 0.002(10) -0.005(9) F6 0.197(10) 0.62(3) 0.108(7) -0.012(11) -0.009(7) -0.192(15) O2 0.36(8) 0.41(9) 0.69(12) -0.01(8) 0.09(11) 0.08(7) C35 0.07(2) 0.18(4) 0.10(2) 0.01(2) 0.00(2) 0.03(3) C36 0.22(6) 0.16(4) 0.20(6) -0.14(5) 0.10(6) -0.07(4) C35A 0.11(3) 0.12(2) 0.08(2) 0.005(16) 0.04(2) -0.02(3) C36A 0.24(4) 0.32(4) 0.12(2) -0.11(2) 0.02(2) 0.01(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 C33 1.867(9) . ? Ru1 C3 2.216(9) . ? Ru1 C4 2.243(9) . ? Ru1 C5 2.245(8) . ? Ru1 C2 2.248(9) . ? Ru1 C1 2.256(9) . ? Ru1 P2 2.2752(19) . ? Ru1 P1 2.313(2) . ? P1 C21 1.826(8) . ? P1 C27 1.827(7) . ? P1 C8 1.867(7) . ? P2 C15 1.805(8) . ? P2 C7 1.840(7) . ? P2 C10 1.851(7) . ? C1 C2 1.388(12) . ? C1 C5 1.417(13) . ? C1 C6 1.482(13) . ? C2 C3 1.422(15) . ? C3 C4 1.377(14) . ? C4 C5 1.404(14) . ? C7 C13 1.501(9) . ? C7 C8 1.567(9) . ? C8 C9 1.562(10) . ? C9 C10 1.551(10) . ? C10 C11 1.517(10) . ? C11 C13 1.328(10) . ? C11 C12 1.523(10) . ? C13 C14 1.502(10) . ? C15 C16 1.358(11) . ? C15 C20 1.371(12) . ? C16 C17 1.406(14) . ? C17 C18 1.348(19) . ? C18 C19 1.380(18) . ? C19 C20 1.384(14) . ? C21 C22 1.380(10) . ? C21 C26 1.397(10) . ? C22 C23 1.394(12) . ? C23 C24 1.372(12) . ? C24 C25 1.347(12) . ? C25 C26 1.397(12) . ? C27 C28 1.368(11) . ? C27 C32 1.382(10) . ? C28 C29 1.395(11) . ? C29 C30 1.353(13) . ? C30 C31 1.362(13) . ? C31 C32 1.369(11) . ? C33 O1 1.128(9) . ? P3 F4 1.442(10) . ? P3 F6 1.478(10) . ? P3 F5 1.480(9) . ? P3 F1 1.520(10) . ? P3 F2 1.525(11) . ? P3 F3 1.547(9) . ? O2 C35A 1.34(3) . ? O2 C35A 1.34(3) 3_677 ? O2 C35 1.36(4) . ? O2 C35 1.36(4) 3_677 ? O2 C36 1.53(8) . ? O2 C36 1.53(8) 3_677 ? O2 C36A 1.83(5) 3_677 ? O2 C36A 1.83(5) . ? C35 C35A 0.83(4) . ? C35 C36A 1.12(7) . ? C35 C36 1.46(9) . ? C36 C36A 0.78(8) . ? C36 C35A 1.99(10) 3_677 ? C35A C36A 1.92(7) . ? C35A C36 1.99(10) 3_677 ? 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 C33 Ru1 C3 153.0(4) . . ? C33 Ru1 C4 141.0(4) . . ? C3 Ru1 C4 36.0(4) . . ? C33 Ru1 C5 105.6(4) . . ? C3 Ru1 C5 60.7(4) . . ? C4 Ru1 C5 36.5(4) . . ? C33 Ru1 C2 116.5(5) . . ? C3 Ru1 C2 37.1(4) . . ? C4 Ru1 C2 61.1(4) . . ? C5 Ru1 C2 61.2(4) . . ? C33 Ru1 C1 94.4(3) . . ? C3 Ru1 C1 60.3(4) . . ? C4 Ru1 C1 60.5(4) . . ? C5 Ru1 C1 36.7(3) . . ? C2 Ru1 C1 35.9(3) . . ? C33 Ru1 P2 92.2(3) . . ? C3 Ru1 P2 97.2(3) . . ? C4 Ru1 P2 126.7(4) . . ? C5 Ru1 P2 157.3(3) . . ? C2 Ru1 P2 98.4(3) . . ? C1 Ru1 P2 129.7(3) . . ? C33 Ru1 P1 92.4(3) . . ? C3 Ru1 P1 114.1(4) . . ? C4 Ru1 P1 96.1(3) . . ? C5 Ru1 P1 111.8(3) . . ? C2 Ru1 P1 151.1(4) . . ? C1 Ru1 P1 148.3(3) . . ? P2 Ru1 P1 80.80(7) . . ? C21 P1 C27 102.6(4) . . ? C21 P1 C8 108.2(3) . . ? C27 P1 C8 104.6(3) . . ? C21 P1 Ru1 115.5(3) . . ? C27 P1 Ru1 118.9(3) . . ? C8 P1 Ru1 106.2(2) . . ? C15 P2 C7 109.4(3) . . ? C15 P2 C10 106.7(4) . . ? C7 P2 C10 81.1(3) . . ? C15 P2 Ru1 120.2(3) . . ? C7 P2 Ru1 112.5(2) . . ? C10 P2 Ru1 120.1(2) . . ? C2 C1 C5 109.3(10) . . ? C2 C1 C6 125.8(12) . . ? C5 C1 C6 124.7(11) . . ? C2 C1 Ru1 71.7(5) . . ? C5 C1 Ru1 71.3(5) . . ? C6 C1 Ru1 127.2(7) . . ? C1 C2 C3 106.2(10) . . ? C1 C2 Ru1 72.4(5) . . ? C3 C2 Ru1 70.2(6) . . ? C4 C3 C2 109.3(10) . . ? C4 C3 Ru1 73.1(6) . . ? C2 C3 Ru1 72.7(5) . . ? C3 C4 C5 108.2(11) . . ? C3 C4 Ru1 70.9(6) . . ? C5 C4 Ru1 71.9(5) . . ? C4 C5 C1 106.9(9) . . ? C4 C5 Ru1 71.7(5) . . ? C1 C5 Ru1 72.0(5) . . ? C13 C7 C8 110.9(6) . . ? C13 C7 P2 102.8(5) . . ? C8 C7 P2 95.4(4) . . ? C9 C8 C7 104.6(6) . . ? C9 C8 P1 106.3(4) . . ? C7 C8 P1 109.3(4) . . ? C10 C9 C8 105.9(5) . . ? C11 C10 C9 105.5(6) . . ? C11 C10 P2 100.5(5) . . ? C9 C10 P2 100.1(4) . . ? C13 C11 C10 111.3(6) . . ? C13 C11 C12 129.2(7) . . ? C10 C11 C12 119.4(7) . . ? C11 C13 C7 110.3(6) . . ? C11 C13 C14 128.4(7) . . ? C7 C13 C14 121.3(7) . . ? C16 C15 C20 119.5(8) . . ? C16 C15 P2 121.7(7) . . ? C20 C15 P2 118.7(7) . . ? C15 C16 C17 119.7(11) . . ? C18 C17 C16 120.2(12) . . ? C17 C18 C19 120.6(12) . . ? C18 C19 C20 118.6(13) . . ? C15 C20 C19 121.2(11) . . ? C22 C21 C26 117.6(7) . . ? C22 C21 P1 121.2(6) . . ? C26 C21 P1 121.1(6) . . ? C21 C22 C23 120.3(8) . . ? C24 C23 C22 121.4(8) . . ? C25 C24 C23 118.9(9) . . ? C24 C25 C26 121.2(9) . . ? C25 C26 C21 120.6(8) . . ? C28 C27 C32 118.3(7) . . ? C28 C27 P1 122.6(6) . . ? C32 C27 P1 119.1(6) . . ? C27 C28 C29 119.5(9) . . ? C30 C29 C28 121.2(9) . . ? C29 C30 C31 119.7(8) . . ? C30 C31 C32 119.6(9) . . ? C31 C32 C27 121.7(9) . . ? O1 C33 Ru1 177.6(8) . . ? F4 P3 F6 93.4(8) . . ? F4 P3 F5 99.0(10) . . ? F6 P3 F5 93.0(7) . . ? F4 P3 F1 175.6(9) . . ? F6 P3 F1 89.0(8) . . ? F5 P3 F1 84.5(7) . . ? F4 P3 F2 91.1(9) . . ? F6 P3 F2 92.1(8) . . ? F5 P3 F2 168.4(9) . . ? F1 P3 F2 85.2(8) . . ? F4 P3 F3 88.6(7) . . ? F6 P3 F3 176.9(9) . . ? F5 P3 F3 89.1(6) . . ? F1 P3 F3 88.9(7) . . ? F2 P3 F3 85.5(6) . . ? C35A O2 C35A 180.00(3) . 3_677 ? C35A O2 C35 35.9(18) . . ? C35A O2 C35 144.1(18) 3_677 . ? C35A O2 C35 144.1(18) . 3_677 ? C35A O2 C35 35.9(18) 3_677 3_677 ? C35 O2 C35 180(5) . 3_677 ? C35A O2 C36 92(4) . . ? C35A O2 C36 88(4) 3_677 . ? C35 O2 C36 60(3) . . ? C35 O2 C36 120(3) 3_677 . ? C35A O2 C36 88(4) . 3_677 ? C35A O2 C36 92(4) 3_677 3_677 ? C35 O2 C36 120(3) . 3_677 ? C35 O2 C36 60(3) 3_677 3_677 ? C36 O2 C36 180.00(3) . 3_677 ? C35A O2 C36A 107(3) . 3_677 ? C35A O2 C36A 73(3) 3_677 3_677 ? C35 O2 C36A 143(3) . 3_677 ? C35 O2 C36A 37(3) 3_677 3_677 ? C36 O2 C36A 155(3) . 3_677 ? C36 O2 C36A 25(3) 3_677 3_677 ? C35A O2 C36A 73(3) . . ? C35A O2 C36A 107(3) 3_677 . ? C35 O2 C36A 37(3) . . ? C35 O2 C36A 143(3) 3_677 . ? C36 O2 C36A 25(3) . . ? C36 O2 C36A 155(3) 3_677 . ? C36A O2 C36A 180.00(2) 3_677 . ? C35A C35 C36A 159(6) . . ? C35A C35 O2 70(4) . . ? C36A C35 O2 94(5) . . ? C35A C35 C36 128(6) . . ? C36A C35 C36 32(5) . . ? O2 C35 C36 66(4) . . ? C36A C36 C35 49(7) . . ? C36A C36 O2 100(9) . . ? C35 C36 O2 54(3) . . ? C36A C36 C35A 131(8) . 3_677 ? C35 C36 C35A 95(5) . 3_677 ? O2 C36 C35A 42(2) . 3_677 ? C35 C35A O2 74(4) . . ? C35 C35A C36A 12(4) . . ? O2 C35A C36A 66(2) . . ? C35 C35A C36 120(7) . 3_677 ? O2 C35A C36 50(3) . 3_677 ? C36A C35A C36 114(3) . 3_677 ? C36 C36A C35 99(10) . . ? C36 C36A O2 56(8) . . ? C35 C36A O2 48(3) . . ? C36 C36A C35A 90(9) . . ? C35 C36A C35A 9(3) . . ? O2 C36A C35A 41.6(17) . . ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 0.696 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.085 #===END data_jhn492a _database_code_depnum_ccdc_archive 'CCDC 248583' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 14A _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H41 F6 O P3 Ru' _chemical_formula_weight 809.68 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.119(2) _cell_length_b 27.564(5) _cell_length_c 12.1072(19) _cell_angle_alpha 90.00 _cell_angle_beta 94.171(15) _cell_angle_gamma 90.00 _cell_volume 3700.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 4.78 _cell_measurement_theta_max 12.52 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max .48 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8982 _exptl_absorpt_correction_T_max 0.9611 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7946 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.1288 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6514 _reflns_number_gt 3668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+0.0000P] 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 6514 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1451 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1325 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.82618(5) 0.86297(2) 0.57251(5) 0.03322(19) Uani 1 1 d . . . P1 P 0.81118(17) 0.90946(7) 0.72888(16) 0.0353(5) Uani 1 1 d . . . P2 P 0.68855(17) 0.92065(7) 0.50283(16) 0.0344(5) Uani 1 1 d . . . C1 C 0.7545(10) 0.7977(3) 0.4755(10) 0.077(4) Uani 1 1 d . . . C2 C 0.8793(9) 0.7992(3) 0.4740(7) 0.054(2) Uani 1 1 d . . . C3 C 0.9321(8) 0.7933(3) 0.5811(8) 0.054(2) Uani 1 1 d . . . C4 C 0.8415(12) 0.7880(3) 0.6506(7) 0.069(3) Uani 1 1 d . . . C5 C 0.7305(9) 0.7916(3) 0.5908(12) 0.077(4) Uani 1 1 d . . . C6 C 0.6661(14) 0.7961(4) 0.3761(13) 0.223(11) Uani 1 1 d . . . H6A H 0.6517 0.7630 0.3545 0.334 Uiso 1 1 calc R . . H6B H 0.6983 0.8135 0.3162 0.334 Uiso 1 1 calc R . . H6C H 0.5916 0.8108 0.3939 0.334 Uiso 1 1 calc R . . C7 C 0.9506(14) 0.8006(4) 0.3704(10) 0.149(7) Uani 1 1 d . . . H7A H 0.9604 0.7682 0.3434 0.223 Uiso 1 1 calc R . . H7B H 1.0284 0.8147 0.3886 0.223 Uiso 1 1 calc R . . H7C H 0.9076 0.8197 0.3142 0.223 Uiso 1 1 calc R . . C8 C 1.0646(9) 0.7871(4) 0.6140(12) 0.135(6) Uani 1 1 d . . . H8A H 1.0853 0.7534 0.6112 0.203 Uiso 1 1 calc R . . H8B H 1.0819 0.7991 0.6879 0.203 Uiso 1 1 calc R . . H8C H 1.1109 0.8050 0.5638 0.203 Uiso 1 1 calc R . . C9 C 0.8557(16) 0.7709(4) 0.7705(9) 0.174(8) Uani 1 1 d . . . H9A H 0.8589 0.7361 0.7724 0.261 Uiso 1 1 calc R . . H9B H 0.7882 0.7819 0.8089 0.261 Uiso 1 1 calc R . . H9C H 0.9289 0.7839 0.8057 0.261 Uiso 1 1 calc R . . C10 C 0.6077(12) 0.7789(4) 0.6322(19) 0.245(12) Uani 1 1 d . . . H10A H 0.5976 0.7443 0.6321 0.368 Uiso 1 1 calc R . . H10B H 0.5451 0.7935 0.5844 0.368 Uiso 1 1 calc R . . H10C H 0.6034 0.7911 0.7061 0.368 Uiso 1 1 calc R . . C11 C 0.6687(6) 0.9441(3) 0.7264(6) 0.0362(18) Uani 1 1 d . . . H11A H 0.5956 0.9247 0.7320 0.043 Uiso 1 1 calc R . . C12 C 0.6832(6) 0.9681(3) 0.6109(6) 0.0375(18) Uani 1 1 d . . . H12A H 0.6190 0.9917 0.5922 0.045 Uiso 1 1 calc R . . C13 C 0.8100(6) 0.9929(2) 0.6209(6) 0.0377(18) Uani 1 1 d . . . H13A H 0.8554 0.9847 0.5581 0.045 Uiso 1 1 calc R . . H13B H 0.8023 1.0279 0.6249 0.045 Uiso 1 1 calc R . . C14 C 0.8724(6) 0.9724(2) 0.7295(6) 0.0362(18) Uani 1 1 d . . . H14A H 0.9605 0.9749 0.7360 0.043 Uiso 1 1 calc R . . C15 C 0.8091(7) 0.9962(3) 0.8220(6) 0.044(2) Uani 1 1 d . . . C16 C 0.8681(8) 1.0360(3) 0.8894(7) 0.057(2) Uani 1 1 d . . . H16A H 0.8151 1.0467 0.9436 0.086 Uiso 1 1 calc R . . H16B H 0.8853 1.0626 0.8420 0.086 Uiso 1 1 calc R . . H16C H 0.9418 1.0243 0.9261 0.086 Uiso 1 1 calc R . . C17 C 0.6942(7) 0.9817(3) 0.8176(6) 0.0409(19) Uani 1 1 d . . . C18 C 0.5948(7) 0.9975(3) 0.8862(7) 0.058(2) Uani 1 1 d . . . H18A H 0.6250 1.0211 0.9394 0.087 Uiso 1 1 calc R . . H18B H 0.5648 0.9699 0.9242 0.087 Uiso 1 1 calc R . . H18C H 0.5307 1.0115 0.8392 0.087 Uiso 1 1 calc R . . C19 C 0.8455(7) 0.8838(3) 0.8643(6) 0.0382(18) Uani 1 1 d . . . C20 C 0.9647(8) 0.8760(3) 0.9021(7) 0.056(2) Uani 1 1 d . . . H20A H 1.0260 0.8871 0.8602 0.067 Uiso 1 1 calc R . . C21 C 0.9942(9) 0.8523(3) 0.9995(8) 0.069(3) Uani 1 1 d . . . H21A H 1.0745 0.8480 1.0247 0.083 Uiso 1 1 calc R . . C22 C 0.9047(11) 0.8353(4) 1.0587(8) 0.076(3) Uani 1 1 d . . . H22A H 0.9249 0.8177 1.1229 0.092 Uiso 1 1 calc R . . C23 C 0.7856(10) 0.8430(4) 1.0276(8) 0.073(3) Uani 1 1 d . . . H23A H 0.7265 0.8319 1.0719 0.088 Uiso 1 1 calc R . . C24 C 0.7528(7) 0.8676(3) 0.9288(6) 0.049(2) Uani 1 1 d . . . H24A H 0.6722 0.8732 0.9064 0.059 Uiso 1 1 calc R . . C25 C 0.7268(7) 0.9550(3) 0.3799(6) 0.0421(19) Uani 1 1 d . . . C26 C 0.7864(7) 0.9319(3) 0.2990(6) 0.053(2) Uani 1 1 d . . . H26A H 0.8111 0.8999 0.3092 0.064 Uiso 1 1 calc R . . C27 C 0.8098(8) 0.9561(4) 0.2025(7) 0.067(3) Uani 1 1 d . . . H27A H 0.8488 0.9403 0.1474 0.080 Uiso 1 1 calc R . . C28 C 0.7749(8) 1.0034(4) 0.1889(7) 0.063(3) Uani 1 1 d . . . H28A H 0.7904 1.0198 0.1244 0.076 Uiso 1 1 calc R . . C29 C 0.7176(8) 1.0267(3) 0.2695(8) 0.064(3) Uani 1 1 d . . . H29A H 0.6961 1.0592 0.2607 0.077 Uiso 1 1 calc R . . C30 C 0.6915(7) 1.0019(3) 0.3647(7) 0.055(2) Uani 1 1 d . . . H30A H 0.6498 1.0175 0.4184 0.066 Uiso 1 1 calc R . . C31 C 0.5319(7) 0.9025(3) 0.4627(7) 0.0418(19) Uani 1 1 d . . . C32 C 0.4876(8) 0.9035(3) 0.3544(8) 0.059(2) Uani 1 1 d . . . H32A H 0.5351 0.9158 0.3008 0.071 Uiso 1 1 calc R . . C33 C 0.3727(9) 0.8864(4) 0.3235(9) 0.078(3) Uani 1 1 d . . . H33A H 0.3447 0.8860 0.2492 0.094 Uiso 1 1 calc R . . C34 C 0.3004(9) 0.8701(4) 0.4027(11) 0.089(4) Uani 1 1 d . . . H34A H 0.2226 0.8595 0.3823 0.107 Uiso 1 1 calc R . . C35 C 0.3421(8) 0.8695(4) 0.5109(10) 0.083(3) Uani 1 1 d . . . H35A H 0.2920 0.8591 0.5644 0.100 Uiso 1 1 calc R . . C36 C 0.4594(8) 0.8844(3) 0.5426(8) 0.063(3) Uani 1 1 d . . . H36A H 0.4891 0.8823 0.6163 0.075 Uiso 1 1 calc R . . C37 C 0.9560(7) 0.9006(3) 0.5335(6) 0.0417(19) Uani 1 1 d . . . O1 O 1.0398(5) 0.9200(2) 0.5077(6) 0.076(2) Uani 1 1 d . . . P3 P 0.3729(3) 0.84820(9) 0.9270(3) 0.0790(9) Uani 1 1 d . . . F1 F 0.3127(10) 0.8157(4) 0.8430(10) 0.228(5) Uani 1 1 d . . . F2 F 0.3054(8) 0.8204(3) 1.0141(10) 0.204(5) Uani 1 1 d . . . F3 F 0.4428(11) 0.8819(4) 1.0123(9) 0.223(5) Uani 1 1 d . . . F4 F 0.4428(6) 0.8753(3) 0.8375(6) 0.135(3) Uani 1 1 d . . . F5 F 0.2716(7) 0.8855(3) 0.9145(9) 0.179(4) Uani 1 1 d . . . F6 F 0.4778(6) 0.8125(2) 0.9475(8) 0.152(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0340(3) 0.0263(3) 0.0403(3) 0.0011(3) 0.0094(2) -0.0012(3) P1 0.0360(11) 0.0308(10) 0.0396(11) 0.0001(9) 0.0068(9) -0.0015(9) P2 0.0333(11) 0.0322(11) 0.0384(11) 0.0027(9) 0.0081(9) -0.0010(9) C1 0.086(8) 0.024(5) 0.111(9) -0.024(5) -0.058(8) 0.019(5) C2 0.084(7) 0.028(4) 0.052(6) -0.003(4) 0.024(5) 0.009(5) C3 0.058(6) 0.031(4) 0.071(6) -0.004(5) 0.003(5) 0.007(4) C4 0.131(10) 0.026(5) 0.050(6) 0.006(4) 0.016(7) -0.002(6) C5 0.057(6) 0.023(5) 0.157(12) -0.020(6) 0.055(8) -0.011(5) C6 0.28(2) 0.062(8) 0.28(2) -0.083(11) -0.248(18) 0.070(11) C7 0.284(19) 0.062(7) 0.120(10) 0.005(7) 0.143(12) 0.036(10) C8 0.061(7) 0.063(7) 0.272(17) -0.035(9) -0.060(9) 0.030(6) C9 0.40(3) 0.051(7) 0.071(8) 0.018(6) 0.038(12) 0.065(11) C10 0.135(13) 0.058(8) 0.57(4) -0.024(14) 0.225(19) -0.033(8) C11 0.037(4) 0.037(4) 0.035(4) 0.001(4) 0.008(4) -0.003(4) C12 0.037(4) 0.036(4) 0.040(4) 0.001(4) 0.010(4) 0.001(4) C13 0.049(5) 0.024(4) 0.042(4) 0.001(3) 0.013(4) 0.003(4) C14 0.030(4) 0.032(4) 0.047(5) -0.002(4) 0.010(4) -0.009(3) C15 0.048(5) 0.036(4) 0.050(5) -0.002(4) 0.017(4) 0.002(4) C16 0.061(6) 0.054(5) 0.058(6) -0.020(5) 0.008(5) -0.005(5) C17 0.052(5) 0.031(4) 0.041(5) 0.000(4) 0.015(4) 0.003(4) C18 0.058(6) 0.070(6) 0.048(5) -0.013(5) 0.016(5) 0.007(5) C19 0.041(5) 0.039(4) 0.034(4) 0.000(4) 0.003(4) -0.004(4) C20 0.053(6) 0.067(6) 0.045(5) 0.017(4) -0.009(4) -0.002(5) C21 0.069(7) 0.078(7) 0.058(6) 0.013(5) -0.010(5) 0.011(6) C22 0.100(9) 0.082(8) 0.046(6) 0.014(5) -0.006(6) 0.020(7) C23 0.088(8) 0.078(7) 0.056(6) 0.015(5) 0.023(6) 0.010(6) C24 0.058(5) 0.045(5) 0.044(5) 0.001(4) 0.007(4) 0.009(5) C25 0.046(5) 0.044(5) 0.036(4) 0.004(4) 0.001(4) -0.002(4) C26 0.066(6) 0.048(5) 0.046(5) 0.005(4) 0.010(5) -0.001(5) C27 0.073(7) 0.085(7) 0.046(6) 0.002(5) 0.021(5) 0.006(6) C28 0.062(6) 0.083(7) 0.045(5) 0.029(5) 0.010(5) -0.003(6) C29 0.074(7) 0.051(6) 0.066(6) 0.020(5) 0.006(6) 0.003(5) C30 0.056(6) 0.053(5) 0.058(6) 0.014(5) 0.021(5) 0.015(5) C31 0.035(4) 0.034(4) 0.057(5) -0.004(4) 0.005(4) 0.002(4) C32 0.050(6) 0.063(6) 0.063(6) 0.012(5) -0.006(5) -0.006(5) C33 0.058(7) 0.083(8) 0.090(8) 0.010(6) -0.018(6) -0.017(6) C34 0.044(6) 0.089(9) 0.132(11) -0.022(8) -0.002(7) -0.011(6) C35 0.054(6) 0.093(8) 0.108(9) -0.036(7) 0.034(6) -0.038(6) C36 0.049(6) 0.068(6) 0.073(6) -0.017(5) 0.016(5) -0.009(5) C37 0.044(5) 0.034(4) 0.048(5) 0.002(4) 0.012(4) 0.005(4) O1 0.052(4) 0.064(4) 0.117(6) 0.002(4) 0.044(4) -0.012(3) P3 0.074(2) 0.0434(15) 0.123(3) 0.0167(16) 0.0347(19) 0.0005(14) F1 0.239(12) 0.212(11) 0.220(11) -0.068(9) -0.081(9) -0.066(9) F2 0.160(8) 0.164(8) 0.303(13) 0.137(9) 0.115(8) 0.031(7) F3 0.305(15) 0.151(9) 0.214(11) -0.072(8) 0.021(10) -0.048(9) F4 0.100(5) 0.155(7) 0.159(6) 0.087(6) 0.058(5) 0.019(5) F5 0.112(6) 0.094(5) 0.344(13) 0.100(7) 0.112(7) 0.047(5) F6 0.099(5) 0.086(5) 0.270(10) 0.052(6) 0.016(6) 0.024(4) _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 C37 1.865(8) . ? Ru1 C2 2.229(8) . ? Ru1 C3 2.250(8) . ? Ru1 C5 2.256(8) . ? Ru1 C1 2.262(8) . ? Ru1 C4 2.273(8) . ? Ru1 P1 2.302(2) . ? Ru1 P2 2.322(2) . ? P1 C19 1.801(7) . ? P1 C11 1.848(7) . ? P1 C14 1.864(7) . ? P2 C25 1.840(8) . ? P2 C31 1.844(8) . ? P2 C12 1.854(7) . ? C1 C2 1.390(13) . ? C1 C5 1.449(14) . ? C1 C6 1.498(13) . ? C2 C3 1.393(12) . ? C2 C7 1.532(12) . ? C3 C4 1.367(12) . ? C3 C8 1.508(12) . ? C4 C5 1.388(14) . ? C4 C9 1.524(12) . ? C5 C10 1.528(13) . ? C11 C17 1.526(10) . ? C11 C12 1.567(9) . ? C12 C13 1.563(9) . ? C13 C14 1.548(9) . ? C14 C15 1.514(10) . ? C15 C17 1.336(10) . ? C15 C16 1.490(10) . ? C17 C18 1.495(10) . ? C19 C20 1.387(10) . ? C19 C24 1.411(10) . ? C20 C21 1.367(11) . ? C21 C22 1.352(13) . ? C22 C23 1.367(13) . ? C23 C24 1.400(11) . ? C25 C30 1.360(10) . ? C25 C26 1.377(10) . ? C26 C27 1.387(11) . ? C27 C28 1.366(12) . ? C28 C29 1.364(11) . ? C29 C30 1.389(11) . ? C31 C32 1.366(11) . ? C31 C36 1.395(11) . ? C32 C33 1.388(11) . ? C33 C34 1.371(13) . ? C34 C35 1.357(14) . ? C35 C36 1.394(12) . ? C37 O1 1.137(8) . ? P3 F1 1.478(9) . ? P3 F5 1.524(7) . ? P3 F6 1.533(7) . ? P3 F2 1.541(8) . ? P3 F3 1.555(10) . ? P3 F4 1.568(6) . ? 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 C37 Ru1 C2 93.6(3) . . ? C37 Ru1 C3 94.2(3) . . ? C2 Ru1 C3 36.2(3) . . ? C37 Ru1 C5 152.7(3) . . ? C2 Ru1 C5 60.6(3) . . ? C3 Ru1 C5 60.0(3) . . ? C37 Ru1 C1 124.1(4) . . ? C2 Ru1 C1 36.1(3) . . ? C3 Ru1 C1 60.6(3) . . ? C5 Ru1 C1 37.4(4) . . ? C37 Ru1 C4 125.1(4) . . ? C2 Ru1 C4 59.4(3) . . ? C3 Ru1 C4 35.2(3) . . ? C5 Ru1 C4 35.7(4) . . ? C1 Ru1 C4 60.4(3) . . ? C37 Ru1 P1 90.1(2) . . ? C2 Ru1 P1 156.5(2) . . ? C3 Ru1 P1 120.4(3) . . ? C5 Ru1 P1 110.0(3) . . ? C1 Ru1 P1 145.7(4) . . ? C4 Ru1 P1 99.9(2) . . ? C37 Ru1 P2 91.7(2) . . ? C2 Ru1 P2 122.6(3) . . ? C3 Ru1 P2 158.3(2) . . ? C5 Ru1 P2 109.3(3) . . ? C1 Ru1 P2 99.1(2) . . ? C4 Ru1 P2 143.2(3) . . ? P1 Ru1 P2 80.35(7) . . ? C19 P1 C11 110.0(3) . . ? C19 P1 C14 108.0(3) . . ? C11 P1 C14 80.3(3) . . ? C19 P1 Ru1 120.5(3) . . ? C11 P1 Ru1 112.8(2) . . ? C14 P1 Ru1 118.3(2) . . ? C25 P2 C31 101.3(4) . . ? C25 P2 C12 103.2(3) . . ? C31 P2 C12 107.4(3) . . ? C25 P2 Ru1 117.5(3) . . ? C31 P2 Ru1 119.6(2) . . ? C12 P2 Ru1 106.3(2) . . ? C2 C1 C5 105.6(8) . . ? C2 C1 C6 126.0(14) . . ? C5 C1 C6 127.9(14) . . ? C2 C1 Ru1 70.7(5) . . ? C5 C1 Ru1 71.1(5) . . ? C6 C1 Ru1 128.8(6) . . ? C1 C2 C3 109.7(8) . . ? C1 C2 C7 126.0(11) . . ? C3 C2 C7 123.9(10) . . ? C1 C2 Ru1 73.3(5) . . ? C3 C2 Ru1 72.7(5) . . ? C7 C2 Ru1 126.2(6) . . ? C4 C3 C2 107.8(8) . . ? C4 C3 C8 125.1(11) . . ? C2 C3 C8 126.6(10) . . ? C4 C3 Ru1 73.3(5) . . ? C2 C3 Ru1 71.1(5) . . ? C8 C3 Ru1 127.4(6) . . ? C3 C4 C5 109.7(8) . . ? C3 C4 C9 126.2(12) . . ? C5 C4 C9 123.1(13) . . ? C3 C4 Ru1 71.5(5) . . ? C5 C4 Ru1 71.5(5) . . ? C9 C4 Ru1 132.6(7) . . ? C4 C5 C1 107.0(8) . . ? C4 C5 C10 126.4(14) . . ? C1 C5 C10 125.0(15) . . ? C4 C5 Ru1 72.8(5) . . ? C1 C5 Ru1 71.5(5) . . ? C10 C5 Ru1 132.0(7) . . ? C17 C11 C12 109.4(6) . . ? C17 C11 P1 103.1(5) . . ? C12 C11 P1 95.1(4) . . ? C13 C12 C11 105.4(6) . . ? C13 C12 P2 106.7(5) . . ? C11 C12 P2 110.0(5) . . ? C14 C13 C12 104.7(5) . . ? C15 C14 C13 105.5(6) . . ? C15 C14 P1 102.5(5) . . ? C13 C14 P1 101.2(5) . . ? C17 C15 C16 128.6(7) . . ? C17 C15 C14 109.6(7) . . ? C16 C15 C14 120.9(7) . . ? C15 C17 C18 129.4(7) . . ? C15 C17 C11 111.0(7) . . ? C18 C17 C11 119.6(7) . . ? C20 C19 C24 119.2(7) . . ? C20 C19 P1 119.7(6) . . ? C24 C19 P1 120.9(6) . . ? C21 C20 C19 121.5(8) . . ? C22 C21 C20 118.9(9) . . ? C21 C22 C23 122.4(9) . . ? C22 C23 C24 119.9(9) . . ? C23 C24 C19 118.1(8) . . ? C30 C25 C26 119.5(8) . . ? C30 C25 P2 121.2(6) . . ? C26 C25 P2 119.3(6) . . ? C25 C26 C27 120.5(8) . . ? C28 C27 C26 119.4(9) . . ? C29 C28 C27 120.5(8) . . ? C28 C29 C30 119.9(9) . . ? C25 C30 C29 120.3(8) . . ? C32 C31 C36 119.1(8) . . ? C32 C31 P2 120.9(6) . . ? C36 C31 P2 119.8(7) . . ? C31 C32 C33 120.8(9) . . ? C34 C33 C32 119.8(10) . . ? C35 C34 C33 120.2(10) . . ? C34 C35 C36 120.6(10) . . ? C35 C36 C31 119.4(9) . . ? O1 C37 Ru1 174.2(7) . . ? F1 P3 F5 92.6(6) . . ? F1 P3 F6 91.3(6) . . ? F5 P3 F6 175.9(6) . . ? F1 P3 F2 87.2(6) . . ? F5 P3 F2 90.6(4) . . ? F6 P3 F2 88.4(5) . . ? F1 P3 F3 176.8(7) . . ? F5 P3 F3 89.6(6) . . ? F6 P3 F3 86.5(6) . . ? F2 P3 F3 95.0(7) . . ? F1 P3 F4 92.0(6) . . ? F5 P3 F4 90.6(4) . . ? F6 P3 F4 90.5(4) . . ? F2 P3 F4 178.6(5) . . ? F3 P3 F4 85.7(5) . . ? _diffrn_measured_fraction_theta_max 0.861 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.861 _refine_diff_density_max 0.725 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.095 #===END