# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Peter Sadler' _publ_contact_author_email P.J.Sadler@warwick.ac.uk _publ_section_title ; Structure-Activity Relationships for Organometallic Osmium Arene Phenylazopyridine Complexes with Potent Anticancer Activity ; loop_ _publ_author_name Y.Fu A.Habtemariam A.Basri D.Braddick G.Clarkson P.Sadler # Attachment '- Fy16_complex18.cif' data_fy16 _database_code_depnum_ccdc_archive 'CCDC 821519' #TrackingRef '- Fy16_complex18.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H22 Br F6 I N3 Os P' _chemical_formula_weight 858.40 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 '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 7.8035(3) _cell_length_b 11.9630(5) _cell_length_c 13.6394(6) _cell_angle_alpha 100.216(4) _cell_angle_beta 102.863(4) _cell_angle_gamma 90.779(3) _cell_volume 1219.78(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7302 _cell_measurement_theta_min 3.19 _cell_measurement_theta_max 28.98 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 8.258 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 10365 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 29.07 _reflns_number_total 5620 _reflns_number_gt 4915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0320P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5620 _refine_ls_number_parameters 310 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.033 _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 Os1 Os 0.42885(2) 0.320245(12) 0.731598(12) 0.01057(5) Uani 1 1 d . . . I1 I 0.14439(3) 0.42856(2) 0.77381(2) 0.01581(7) Uani 1 1 d . . . N1 N 0.4355(4) 0.2590(3) 0.8635(3) 0.0121(7) Uani 1 1 d . . . C2 C 0.3405(5) 0.1685(3) 0.8756(3) 0.0130(8) Uani 1 1 d . . . H2A H 0.2590 0.1261 0.8183 0.016 Uiso 1 1 calc R . . Br3 Br 0.22034(6) 0.01394(3) 0.98310(3) 0.01938(10) Uani 1 1 d . . . C3 C 0.3605(5) 0.1375(3) 0.9698(3) 0.0140(8) Uani 1 1 d . . . C4 C 0.4789(5) 0.1962(3) 1.0560(3) 0.0162(9) Uani 1 1 d . . . H4A H 0.4953 0.1725 1.1201 0.019 Uiso 1 1 calc R . . C5 C 0.5718(5) 0.2907(3) 1.0445(3) 0.0152(9) Uani 1 1 d . . . H5A H 0.6533 0.3340 1.1013 0.018 Uiso 1 1 calc R . . C6 C 0.5446(5) 0.3213(3) 0.9496(3) 0.0155(9) Uani 1 1 d . . . N7 N 0.6281(4) 0.4184(3) 0.9368(3) 0.0153(7) Uani 1 1 d . . . N8 N 0.5872(4) 0.4354(3) 0.8439(3) 0.0123(7) Uani 1 1 d . . . C9 C 0.6713(5) 0.5380(3) 0.8308(3) 0.0135(8) Uani 1 1 d . . . C10 C 0.8291(5) 0.5816(3) 0.9008(4) 0.0202(10) Uani 1 1 d . . . H10A H 0.8788 0.5445 0.9558 0.024 Uiso 1 1 calc R . . C11 C 0.9107(6) 0.6804(3) 0.8876(4) 0.0241(11) Uani 1 1 d . . . H11A H 1.0170 0.7115 0.9341 0.029 Uiso 1 1 calc R . . C12 C 0.8370(6) 0.7342(3) 0.8062(4) 0.0222(11) Uani 1 1 d . . . H12A H 0.8955 0.8000 0.7963 0.027 Uiso 1 1 calc R . . C13 C 0.6800(6) 0.6919(3) 0.7403(4) 0.0204(10) Uani 1 1 d . . . H13A H 0.6289 0.7301 0.6863 0.024 Uiso 1 1 calc R . . C14 C 0.5953(6) 0.5931(3) 0.7524(3) 0.0164(9) Uani 1 1 d . . . H14A H 0.4867 0.5642 0.7072 0.020 Uiso 1 1 calc R . . C15 C 0.6308(5) 0.2759(3) 0.6426(3) 0.0147(9) Uani 1 1 d . . . H15A H 0.7570 0.2993 0.6753 0.018 Uiso 1 1 calc R . . C16 C 0.5219(6) 0.3542(3) 0.5949(3) 0.0164(9) Uani 1 1 d . . . H16A H 0.5745 0.4317 0.5980 0.020 Uiso 1 1 calc R . . C17 C 0.3376(6) 0.3370(3) 0.5652(3) 0.0159(6) Uani 1 1 d U . . C18 C 0.2620(6) 0.2313(3) 0.5811(3) 0.0153(5) Uani 1 1 d U . . H18A H 0.1318 0.2219 0.5729 0.018 Uiso 1 1 calc R . . C19 C 0.3703(5) 0.1534(3) 0.6259(3) 0.0147(5) Uani 1 1 d U . . H19A H 0.3133 0.0905 0.6490 0.018 Uiso 1 1 calc R . . C20 C 0.5573(5) 0.1736(3) 0.6602(3) 0.0145(5) Uani 1 1 d U . . C21 C 0.6672(5) 0.0880(3) 0.7116(3) 0.0148(6) Uani 1 1 d U . . H21A H 0.5951 0.0530 0.7515 0.018 Uiso 1 1 calc R . . C22 C 0.8377(6) 0.1392(4) 0.7853(4) 0.0275(11) Uani 1 1 d . . . H22A H 0.8113 0.2017 0.8357 0.041 Uiso 1 1 calc R . . H22B H 0.9156 0.1680 0.7471 0.041 Uiso 1 1 calc R . . H22C H 0.8960 0.0806 0.8206 0.041 Uiso 1 1 calc R . . C23 C 0.7037(6) -0.0061(4) 0.6284(4) 0.0234(10) Uani 1 1 d . . . H23A H 0.7794 -0.0607 0.6603 0.035 Uiso 1 1 calc R . . H23B H 0.7628 0.0273 0.5833 0.035 Uiso 1 1 calc R . . H23C H 0.5922 -0.0452 0.5884 0.035 Uiso 1 1 calc R . . C24 C 0.2221(6) 0.4223(3) 0.5185(3) 0.0213(10) Uani 1 1 d . . . H24A H 0.2829 0.4979 0.5397 0.032 Uiso 1 1 calc R . . H24B H 0.1118 0.4237 0.5416 0.032 Uiso 1 1 calc R . . H24C H 0.1965 0.4009 0.4437 0.032 Uiso 1 1 calc R . . P10 P 0.80176(15) 0.17373(9) 0.34750(10) 0.0219(3) Uani 1 1 d . . . F11 F 0.6040(4) 0.1202(3) 0.3060(4) 0.0620(12) Uani 1 1 d . . . F12 F 0.9996(3) 0.2232(2) 0.3814(2) 0.0329(7) Uani 1 1 d . . . F13 F 0.7385(6) 0.2846(3) 0.4069(4) 0.0732(14) Uani 1 1 d . . . F14 F 0.8634(4) 0.0624(3) 0.2848(3) 0.0532(10) Uani 1 1 d . . . F15 F 0.7758(4) 0.2328(3) 0.2494(3) 0.0551(10) Uani 1 1 d . . . F16 F 0.8284(5) 0.1142(3) 0.4436(3) 0.0633(11) 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 Os1 0.01206(9) 0.01036(8) 0.00842(9) 0.00000(6) 0.00195(6) -0.00101(6) I1 0.01281(14) 0.01704(13) 0.01601(16) -0.00071(10) 0.00294(11) 0.00164(10) N1 0.0134(17) 0.0123(15) 0.0097(19) -0.0006(13) 0.0025(14) -0.0004(13) C2 0.010(2) 0.0161(19) 0.011(2) -0.0018(16) 0.0014(17) 0.0022(16) Br3 0.0213(2) 0.0187(2) 0.0196(3) 0.00666(17) 0.00562(19) -0.00294(17) C3 0.014(2) 0.0125(18) 0.017(2) 0.0063(16) 0.0054(18) 0.0015(16) C4 0.018(2) 0.020(2) 0.012(2) 0.0023(16) 0.0041(18) 0.0059(17) C5 0.016(2) 0.0172(19) 0.012(2) 0.0019(16) 0.0028(18) 0.0024(17) C6 0.014(2) 0.0147(19) 0.017(2) -0.0006(16) 0.0048(18) 0.0025(16) N7 0.0156(18) 0.0142(16) 0.014(2) 0.0007(14) 0.0014(15) -0.0019(14) N8 0.0120(17) 0.0127(15) 0.012(2) -0.0017(13) 0.0051(15) 0.0006(13) C9 0.013(2) 0.0113(18) 0.016(2) -0.0022(16) 0.0063(18) -0.0009(15) C10 0.013(2) 0.018(2) 0.029(3) 0.0004(18) 0.008(2) 0.0044(17) C11 0.014(2) 0.019(2) 0.037(3) -0.004(2) 0.008(2) -0.0039(18) C12 0.023(2) 0.0119(19) 0.035(3) -0.0009(19) 0.019(2) -0.0018(18) C13 0.032(3) 0.015(2) 0.018(3) 0.0019(17) 0.014(2) 0.0034(18) C14 0.019(2) 0.0151(19) 0.014(2) -0.0012(16) 0.0042(18) 0.0006(17) C15 0.016(2) 0.020(2) 0.009(2) 0.0018(16) 0.0042(17) -0.0001(17) C16 0.029(2) 0.0118(18) 0.010(2) 0.0008(15) 0.0103(19) -0.0007(17) C17 0.0210(13) 0.0163(12) 0.0080(13) -0.0028(11) 0.0022(11) 0.0000(11) C18 0.0198(12) 0.0154(10) 0.0081(12) -0.0032(9) 0.0022(10) -0.0008(9) C19 0.0189(11) 0.0148(10) 0.0080(12) -0.0036(9) 0.0026(10) -0.0014(9) C20 0.0182(12) 0.0146(11) 0.0085(12) -0.0029(9) 0.0024(10) -0.0008(10) C21 0.0183(13) 0.0151(12) 0.0091(13) -0.0016(11) 0.0021(11) -0.0002(11) C22 0.022(2) 0.023(2) 0.036(3) 0.008(2) 0.001(2) 0.0004(19) C23 0.027(3) 0.022(2) 0.024(3) 0.0058(19) 0.012(2) 0.0093(19) C24 0.031(3) 0.021(2) 0.011(2) 0.0050(17) 0.003(2) 0.0042(19) P10 0.0206(6) 0.0164(5) 0.0282(8) 0.0057(5) 0.0036(5) -0.0025(5) F11 0.0241(17) 0.0361(17) 0.128(4) 0.028(2) 0.013(2) -0.0085(14) F12 0.0248(15) 0.0340(15) 0.0342(19) 0.0118(13) -0.0087(13) -0.0069(12) F13 0.089(3) 0.0342(18) 0.106(4) -0.010(2) 0.060(3) 0.0028(18) F14 0.050(2) 0.0393(17) 0.053(2) -0.0228(16) 0.0000(18) 0.0067(15) F15 0.0376(19) 0.070(2) 0.052(2) 0.0405(19) -0.0230(17) -0.0195(17) F16 0.100(3) 0.056(2) 0.038(2) 0.0281(17) 0.012(2) -0.024(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 Os1 N8 2.033(3) . ? Os1 N1 2.051(3) . ? Os1 C15 2.210(4) . ? Os1 C20 2.216(4) . ? Os1 C19 2.220(4) . ? Os1 C16 2.243(4) . ? Os1 C18 2.245(4) . ? Os1 C17 2.268(4) . ? Os1 I1 2.7056(3) . ? N1 C2 1.358(5) . ? N1 C6 1.373(5) . ? C2 C3 1.375(6) . ? C2 H2A 0.9500 . ? Br3 C3 1.885(4) . ? C3 C4 1.391(6) . ? C4 C5 1.385(6) . ? C4 H4A 0.9500 . ? C5 C6 1.379(6) . ? C5 H5A 0.9500 . ? C6 N7 1.380(5) . ? N7 N8 1.290(5) . ? N8 C9 1.441(5) . ? C9 C14 1.381(6) . ? C9 C10 1.408(6) . ? C10 C11 1.394(6) . ? C10 H10A 0.9500 . ? C11 C12 1.398(7) . ? C11 H11A 0.9500 . ? C12 C13 1.377(7) . ? C12 H12A 0.9500 . ? C13 C14 1.400(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.418(6) . ? C15 C20 1.426(5) . ? C15 H15A 1.0000 . ? C16 C17 1.407(6) . ? C16 H16A 1.0000 . ? C17 C18 1.459(6) . ? C17 C24 1.503(6) . ? C18 C19 1.396(6) . ? C18 H18A 1.0000 . ? C19 C20 1.433(6) . ? C19 H19A 1.0000 . ? C20 C21 1.511(6) . ? C21 C22 1.523(6) . ? C21 C23 1.528(6) . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? P10 F13 1.573(3) . ? P10 F16 1.575(3) . ? P10 F12 1.583(3) . ? P10 F14 1.591(3) . ? P10 F15 1.596(3) . ? P10 F11 1.603(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 N8 Os1 N1 75.15(13) . . ? N8 Os1 C15 95.44(14) . . ? N1 Os1 C15 120.55(14) . . ? N8 Os1 C20 116.63(14) . . ? N1 Os1 C20 94.54(14) . . ? C15 Os1 C20 37.59(14) . . ? N8 Os1 C19 153.30(14) . . ? N1 Os1 C19 96.41(14) . . ? C15 Os1 C19 66.66(14) . . ? C20 Os1 C19 37.69(15) . . ? N8 Os1 C16 100.22(14) . . ? N1 Os1 C16 157.48(15) . . ? C15 Os1 C16 37.14(15) . . ? C20 Os1 C16 67.44(15) . . ? C19 Os1 C16 77.77(14) . . ? N8 Os1 C18 163.58(14) . . ? N1 Os1 C18 121.07(14) . . ? C15 Os1 C18 78.79(15) . . ? C20 Os1 C18 67.55(15) . . ? C19 Os1 C18 36.42(15) . . ? C16 Os1 C18 65.91(15) . . ? N8 Os1 C17 125.89(14) . . ? N1 Os1 C17 158.33(14) . . ? C15 Os1 C17 67.10(15) . . ? C20 Os1 C17 80.77(15) . . ? C19 Os1 C17 67.00(15) . . ? C16 Os1 C17 36.34(16) . . ? C18 Os1 C17 37.71(14) . . ? N8 Os1 I1 89.49(9) . . ? N1 Os1 I1 84.91(9) . . ? C15 Os1 I1 154.49(11) . . ? C20 Os1 I1 152.91(10) . . ? C19 Os1 I1 115.35(11) . . ? C16 Os1 I1 117.35(11) . . ? C18 Os1 I1 89.51(10) . . ? C17 Os1 I1 89.78(10) . . ? C2 N1 C6 117.4(4) . . ? C2 N1 Os1 127.8(3) . . ? C6 N1 Os1 114.7(3) . . ? N1 C2 C3 120.9(4) . . ? N1 C2 H2A 119.5 . . ? C3 C2 H2A 119.5 . . ? C2 C3 C4 121.8(4) . . ? C2 C3 Br3 119.2(3) . . ? C4 C3 Br3 119.0(3) . . ? C5 C4 C3 117.3(4) . . ? C5 C4 H4A 121.3 . . ? C3 C4 H4A 121.3 . . ? C6 C5 C4 119.2(4) . . ? C6 C5 H5A 120.4 . . ? C4 C5 H5A 120.4 . . ? N1 C6 C5 123.1(4) . . ? N1 C6 N7 116.4(4) . . ? C5 C6 N7 120.6(4) . . ? N8 N7 C6 112.8(3) . . ? N7 N8 C9 112.9(3) . . ? N7 N8 Os1 120.8(2) . . ? C9 N8 Os1 126.2(3) . . ? C14 C9 C10 121.2(4) . . ? C14 C9 N8 120.2(4) . . ? C10 C9 N8 118.6(4) . . ? C11 C10 C9 118.4(5) . . ? C11 C10 H10A 120.8 . . ? C9 C10 H10A 120.8 . . ? C10 C11 C12 120.4(4) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 120.2(4) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 120.3(4) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C9 C14 C13 119.4(4) . . ? C9 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C16 C15 C20 120.9(4) . . ? C16 C15 Os1 72.7(2) . . ? C20 C15 Os1 71.4(2) . . ? C16 C15 H15A 119.1 . . ? C20 C15 H15A 119.1 . . ? Os1 C15 H15A 119.1 . . ? C17 C16 C15 122.4(4) . . ? C17 C16 Os1 72.8(2) . . ? C15 C16 Os1 70.2(2) . . ? C17 C16 H16A 118.0 . . ? C15 C16 H16A 118.0 . . ? Os1 C16 H16A 118.0 . . ? C16 C17 C18 116.8(4) . . ? C16 C17 C24 122.2(4) . . ? C18 C17 C24 120.9(4) . . ? C16 C17 Os1 70.8(2) . . ? C18 C17 Os1 70.3(2) . . ? C24 C17 Os1 129.8(3) . . ? C19 C18 C17 120.5(4) . . ? C19 C18 Os1 70.8(2) . . ? C17 C18 Os1 72.0(2) . . ? C19 C18 H18A 119.2 . . ? C17 C18 H18A 119.2 . . ? Os1 C18 H18A 119.2 . . ? C18 C19 C20 122.5(4) . . ? C18 C19 Os1 72.7(2) . . ? C20 C19 Os1 71.0(2) . . ? C18 C19 H19A 118.0 . . ? C20 C19 H19A 118.0 . . ? Os1 C19 H19A 118.0 . . ? C15 C20 C19 116.8(4) . . ? C15 C20 C21 123.0(4) . . ? C19 C20 C21 120.2(3) . . ? C15 C20 Os1 71.0(2) . . ? C19 C20 Os1 71.3(2) . . ? C21 C20 Os1 128.4(3) . . ? C20 C21 C22 114.1(3) . . ? C20 C21 C23 108.3(4) . . ? C22 C21 C23 111.1(4) . . ? C20 C21 H21A 107.7 . . ? C22 C21 H21A 107.7 . . ? C23 C21 H21A 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C17 C24 H24A 109.5 . . ? C17 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C17 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F13 P10 F16 92.2(2) . . ? F13 P10 F12 91.10(19) . . ? F16 P10 F12 90.77(19) . . ? F13 P10 F14 178.6(3) . . ? F16 P10 F14 89.1(2) . . ? F12 P10 F14 89.40(17) . . ? F13 P10 F15 88.5(2) . . ? F16 P10 F15 179.3(2) . . ? F12 P10 F15 89.15(16) . . ? F14 P10 F15 90.2(2) . . ? F13 P10 F11 91.9(2) . . ? F16 P10 F11 91.5(2) . . ? F12 P10 F11 176.2(2) . . ? F14 P10 F11 87.59(18) . . ? F15 P10 F11 88.56(19) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2A F14 0.95 2.49 3.338(5) 148.7 2_656 C4 H4A F15 0.95 2.49 3.060(5) 118.4 1_556 _diffrn_measured_fraction_theta_max 0.859 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.450 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.162 # Attachment '- fy12_complex16.cif' data_fy12 _database_code_depnum_ccdc_archive 'CCDC 821520' #TrackingRef '- fy12_complex16.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H22 Cl2 F6 N3 Os P' _chemical_formula_weight 722.49 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' 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' Os Os -1.2165 7.6030 '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 9.1784(2) _cell_length_b 10.6711(3) _cell_length_c 12.2921(4) _cell_angle_alpha 93.579(2) _cell_angle_beta 93.460(2) _cell_angle_gamma 96.430(2) _cell_volume 1191.28(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7708 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 29.31 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 5.706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _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 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 9986 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 29.38 _reflns_number_total 5549 _reflns_number_gt 5037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0173P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5549 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0424 _refine_ls_wR_factor_gt 0.0417 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 Os1 Os 0.441872(11) 0.268020(10) 0.276608(8) 0.00961(4) Uani 1 1 d . . . N1 N 0.5309(2) 0.1002(2) 0.28816(18) 0.0127(5) Uani 1 1 d . . . C2 C 0.6554(3) 0.0708(3) 0.2470(2) 0.0142(6) Uani 1 1 d . . . H2A H 0.7084 0.1286 0.2039 0.017 Uiso 1 1 calc R . . Cl3 Cl 0.86812(8) -0.07540(7) 0.21015(7) 0.02403(17) Uani 1 1 d . . . C3 C 0.7074(3) -0.0425(3) 0.2663(2) 0.0170(7) Uani 1 1 d . . . C4 C 0.6330(3) -0.1285(3) 0.3278(2) 0.0158(6) Uani 1 1 d . . . H4A H 0.6692 -0.2067 0.3404 0.019 Uiso 1 1 calc R . . C5 C 0.5042(3) -0.0989(3) 0.3711(2) 0.0144(6) Uani 1 1 d . . . H5A H 0.4498 -0.1562 0.4140 0.017 Uiso 1 1 calc R . . C6 C 0.4569(3) 0.0166(3) 0.3501(2) 0.0118(6) Uani 1 1 d . . . N7 N 0.3341(2) 0.0542(2) 0.39775(18) 0.0117(5) Uani 1 1 d . . . N8 N 0.3132(2) 0.1679(2) 0.37495(18) 0.0109(5) Uani 1 1 d . . . C9 C 0.1926(3) 0.2138(3) 0.4284(2) 0.0118(6) Uani 1 1 d . . . C10 C 0.0630(3) 0.1358(3) 0.4360(2) 0.0170(6) Uani 1 1 d . . . H10A H 0.0511 0.0517 0.4037 0.020 Uiso 1 1 calc R . . C11 C -0.0482(3) 0.1817(3) 0.4911(3) 0.0226(7) Uani 1 1 d . . . H11A H -0.1385 0.1296 0.4950 0.027 Uiso 1 1 calc R . . C12 C -0.0297(3) 0.3032(3) 0.5410(2) 0.0210(7) Uani 1 1 d . . . H12A H -0.1060 0.3333 0.5806 0.025 Uiso 1 1 calc R . . C13 C 0.1001(3) 0.3807(3) 0.5329(2) 0.0173(6) Uani 1 1 d . . . H13A H 0.1124 0.4639 0.5669 0.021 Uiso 1 1 calc R . . C14 C 0.2120(3) 0.3377(3) 0.4754(2) 0.0138(6) Uani 1 1 d . . . H14A H 0.3002 0.3914 0.4682 0.017 Uiso 1 1 calc R . . Cl1 Cl 0.60187(7) 0.33935(6) 0.43481(5) 0.01469(14) Uani 1 1 d . . . C15 C 0.5263(3) 0.3152(3) 0.1163(2) 0.0136(6) Uani 1 1 d . . . H15A H 0.6150 0.2776 0.0920 0.016 Uiso 1 1 calc R . . C16 C 0.3862(3) 0.2403(3) 0.1018(2) 0.0150(6) Uani 1 1 d . . . H16A H 0.3793 0.1532 0.0654 0.018 Uiso 1 1 calc R . . C17 C 0.2616(3) 0.2805(3) 0.1497(2) 0.0171(6) Uani 1 1 d . . . C18 C 0.2815(3) 0.3950(3) 0.2181(2) 0.0162(6) Uani 1 1 d . . . H18A H 0.2014 0.4149 0.2657 0.019 Uiso 1 1 calc R . . C19 C 0.4211(3) 0.4654(3) 0.2369(2) 0.0144(6) Uani 1 1 d . . . H19A H 0.4367 0.5341 0.2970 0.017 Uiso 1 1 calc R . . C20 C 0.5460(3) 0.4277(3) 0.1839(2) 0.0127(6) Uani 1 1 d . . . C21 C 0.6924(3) 0.5080(3) 0.2041(2) 0.0152(6) Uani 1 1 d . . . H21A H 0.6940 0.5548 0.2772 0.018 Uiso 1 1 calc R . . C22 C 0.8264(3) 0.4340(3) 0.2035(2) 0.0193(7) Uani 1 1 d . . . H22A H 0.8206 0.3739 0.2607 0.029 Uiso 1 1 calc R . . H22B H 0.9164 0.4929 0.2173 0.029 Uiso 1 1 calc R . . H22C H 0.8278 0.3878 0.1322 0.029 Uiso 1 1 calc R . . C23 C 0.6994(3) 0.6054(3) 0.1170(2) 0.0208(7) Uani 1 1 d . . . H23A H 0.6168 0.6557 0.1226 0.031 Uiso 1 1 calc R . . H23B H 0.6938 0.5614 0.0442 0.031 Uiso 1 1 calc R . . H23C H 0.7921 0.6613 0.1287 0.031 Uiso 1 1 calc R . . C24 C 0.1131(3) 0.2037(3) 0.1321(3) 0.0230(7) Uani 1 1 d . . . H24A H 0.1257 0.1148 0.1150 0.034 Uiso 1 1 calc R . . H24B H 0.0569 0.2351 0.0713 0.034 Uiso 1 1 calc R . . H24C H 0.0601 0.2113 0.1986 0.034 Uiso 1 1 calc R . . P10 P 0.23943(8) 0.78015(7) 0.12699(6) 0.01625(16) Uani 1 1 d . . . F11 F 0.2650(2) 0.64344(16) 0.07536(14) 0.0260(4) Uani 1 1 d . . . F12 F 0.2159(2) 0.91730(17) 0.17862(15) 0.0306(5) Uani 1 1 d . . . F13 F 0.06774(19) 0.73607(19) 0.12720(15) 0.0332(5) Uani 1 1 d . . . F14 F 0.41214(18) 0.82550(18) 0.12485(14) 0.0270(4) Uani 1 1 d . . . F15 F 0.2651(2) 0.73333(17) 0.24724(13) 0.0262(4) Uani 1 1 d . . . F16 F 0.21539(19) 0.82704(17) 0.00572(13) 0.0239(4) 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 Os1 0.00986(6) 0.00882(6) 0.01033(6) 0.00323(4) 0.00107(4) 0.00030(4) N1 0.0120(12) 0.0144(13) 0.0111(12) 0.0005(9) -0.0020(10) -0.0003(10) C2 0.0138(14) 0.0112(15) 0.0171(15) -0.0004(11) 0.0000(12) 0.0001(11) Cl3 0.0176(4) 0.0181(4) 0.0369(5) -0.0038(3) 0.0054(3) 0.0057(3) C3 0.0156(15) 0.0171(16) 0.0172(15) -0.0061(12) -0.0056(13) 0.0047(12) C4 0.0229(16) 0.0099(15) 0.0140(14) -0.0013(11) -0.0059(13) 0.0047(12) C5 0.0226(15) 0.0102(14) 0.0090(13) -0.0005(11) -0.0040(12) -0.0010(12) C6 0.0126(13) 0.0133(15) 0.0087(13) -0.0007(11) 0.0006(11) -0.0011(11) N7 0.0157(12) 0.0097(12) 0.0088(11) 0.0007(9) -0.0003(10) -0.0015(10) N8 0.0111(11) 0.0110(12) 0.0100(11) 0.0002(9) -0.0001(10) 0.0002(9) C9 0.0107(13) 0.0148(15) 0.0105(13) 0.0038(11) 0.0012(11) 0.0018(11) C10 0.0161(15) 0.0136(15) 0.0208(16) 0.0045(12) 0.0003(13) -0.0023(12) C11 0.0130(15) 0.0250(18) 0.0307(18) 0.0099(14) 0.0059(14) -0.0009(13) C12 0.0183(15) 0.0275(18) 0.0197(16) 0.0063(13) 0.0073(13) 0.0084(13) C13 0.0201(15) 0.0184(16) 0.0137(14) 0.0013(12) 0.0004(13) 0.0039(13) C14 0.0128(14) 0.0126(15) 0.0156(14) 0.0025(11) -0.0007(12) 0.0002(11) Cl1 0.0149(3) 0.0141(3) 0.0140(3) 0.0027(3) -0.0023(3) -0.0022(3) C15 0.0163(14) 0.0156(15) 0.0095(13) 0.0053(11) -0.0003(12) 0.0018(12) C16 0.0194(15) 0.0156(15) 0.0101(14) 0.0048(11) 0.0015(12) -0.0001(12) C17 0.0165(15) 0.0195(16) 0.0146(15) 0.0070(12) -0.0045(13) -0.0016(12) C18 0.0144(14) 0.0167(16) 0.0199(16) 0.0112(12) 0.0025(12) 0.0053(12) C19 0.0194(15) 0.0083(14) 0.0160(14) 0.0072(11) 0.0011(12) 0.0004(12) C20 0.0173(14) 0.0106(14) 0.0108(13) 0.0081(11) 0.0002(12) 0.0013(11) C21 0.0160(14) 0.0136(15) 0.0149(14) 0.0004(11) 0.0006(12) -0.0025(12) C22 0.0141(14) 0.0231(17) 0.0203(16) 0.0010(13) 0.0021(13) -0.0001(13) C23 0.0237(16) 0.0160(16) 0.0222(16) 0.0063(13) 0.0034(14) -0.0039(13) C24 0.0139(15) 0.0258(18) 0.0283(18) 0.0089(14) -0.0034(14) -0.0029(13) P10 0.0135(4) 0.0208(4) 0.0143(4) -0.0016(3) 0.0011(3) 0.0028(3) F11 0.0366(11) 0.0214(10) 0.0215(9) -0.0005(8) 0.0068(8) 0.0088(8) F12 0.0380(11) 0.0248(11) 0.0288(10) -0.0078(8) -0.0012(9) 0.0108(9) F13 0.0148(9) 0.0485(13) 0.0347(11) -0.0061(9) 0.0057(9) -0.0009(9) F14 0.0138(9) 0.0440(12) 0.0221(10) 0.0022(8) 0.0010(8) -0.0007(8) F15 0.0313(10) 0.0329(11) 0.0150(9) 0.0021(8) 0.0047(8) 0.0037(9) F16 0.0273(10) 0.0293(11) 0.0160(9) 0.0045(8) -0.0034(8) 0.0076(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 Os1 N8 2.012(2) . ? Os1 N1 2.059(2) . ? Os1 C16 2.173(3) . ? Os1 C19 2.218(3) . ? Os1 C17 2.226(3) . ? Os1 C15 2.227(3) . ? Os1 C18 2.227(3) . ? Os1 C20 2.263(3) . ? Os1 Cl1 2.3954(6) . ? N1 C2 1.339(4) . ? N1 C6 1.360(4) . ? C2 C3 1.377(4) . ? C2 H2A 0.9500 . ? Cl3 C3 1.727(3) . ? C3 C4 1.375(4) . ? C4 C5 1.386(4) . ? C4 H4A 0.9500 . ? C5 C6 1.386(4) . ? C5 H5A 0.9500 . ? C6 N7 1.388(4) . ? N7 N8 1.295(3) . ? N8 C9 1.437(3) . ? C9 C10 1.385(4) . ? C9 C14 1.398(4) . ? C10 C11 1.377(4) . ? C10 H10A 0.9500 . ? C11 C12 1.388(4) . ? C11 H11A 0.9500 . ? C12 C13 1.384(4) . ? C12 H12A 0.9500 . ? C13 C14 1.384(4) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.405(4) . ? C15 C16 1.432(4) . ? C15 H15A 1.0000 . ? C16 C17 1.413(4) . ? C16 H16A 1.0000 . ? C17 C18 1.427(4) . ? C17 C24 1.506(4) . ? C18 C19 1.409(4) . ? C18 H18A 1.0000 . ? C19 C20 1.435(4) . ? C19 H19A 1.0000 . ? C20 C21 1.509(4) . ? C21 C22 1.534(4) . ? C21 C23 1.538(4) . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? P10 F13 1.5935(19) . ? P10 F12 1.6008(19) . ? P10 F11 1.6016(18) . ? P10 F15 1.6020(18) . ? P10 F14 1.6070(19) . ? P10 F16 1.6123(18) . ? 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 N8 Os1 N1 74.96(9) . . ? N8 Os1 C16 117.45(10) . . ? N1 Os1 C16 95.08(10) . . ? N8 Os1 C19 125.17(10) . . ? N1 Os1 C19 159.45(10) . . ? C16 Os1 C19 79.57(10) . . ? N8 Os1 C17 94.60(10) . . ? N1 Os1 C17 119.26(10) . . ? C16 Os1 C17 37.46(11) . . ? C19 Os1 C17 67.43(10) . . ? N8 Os1 C15 154.46(9) . . ? N1 Os1 C15 97.18(10) . . ? C16 Os1 C15 37.95(10) . . ? C19 Os1 C15 66.40(11) . . ? C17 Os1 C15 67.67(11) . . ? N8 Os1 C18 98.58(10) . . ? N1 Os1 C18 156.14(10) . . ? C16 Os1 C18 67.11(11) . . ? C19 Os1 C18 36.97(10) . . ? C17 Os1 C18 37.37(11) . . ? C15 Os1 C18 78.69(10) . . ? N8 Os1 C20 162.41(10) . . ? N1 Os1 C20 122.31(10) . . ? C16 Os1 C20 67.51(10) . . ? C19 Os1 C20 37.35(10) . . ? C17 Os1 C20 79.97(10) . . ? C15 Os1 C20 36.45(10) . . ? C18 Os1 C20 66.99(10) . . ? N8 Os1 Cl1 87.82(6) . . ? N1 Os1 Cl1 84.88(6) . . ? C16 Os1 Cl1 153.90(8) . . ? C19 Os1 Cl1 91.33(7) . . ? C17 Os1 Cl1 155.55(8) . . ? C15 Os1 Cl1 116.06(7) . . ? C18 Os1 Cl1 118.20(8) . . ? C20 Os1 Cl1 90.43(7) . . ? C2 N1 C6 118.8(2) . . ? C2 N1 Os1 126.6(2) . . ? C6 N1 Os1 114.45(18) . . ? N1 C2 C3 120.7(3) . . ? N1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C4 C3 C2 121.1(3) . . ? C4 C3 Cl3 120.4(2) . . ? C2 C3 Cl3 118.5(3) . . ? C3 C4 C5 118.7(3) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? C4 C5 C6 118.0(3) . . ? C4 C5 H5A 121.0 . . ? C6 C5 H5A 121.0 . . ? N1 C6 C5 122.6(3) . . ? N1 C6 N7 117.1(2) . . ? C5 C6 N7 120.1(3) . . ? N8 N7 C6 111.2(2) . . ? N7 N8 C9 113.1(2) . . ? N7 N8 Os1 122.16(18) . . ? C9 N8 Os1 124.69(18) . . ? C10 C9 C14 121.2(3) . . ? C10 C9 N8 120.7(2) . . ? C14 C9 N8 118.1(2) . . ? C11 C10 C9 119.1(3) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 120.6(3) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C14 C13 C12 120.5(3) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C9 118.7(3) . . ? C13 C14 H14A 120.7 . . ? C9 C14 H14A 120.7 . . ? C20 C15 C16 120.8(3) . . ? C20 C15 Os1 73.17(16) . . ? C16 C15 Os1 68.98(16) . . ? C20 C15 H15A 118.9 . . ? C16 C15 H15A 118.9 . . ? Os1 C15 H15A 118.9 . . ? C17 C16 C15 121.3(3) . . ? C17 C16 Os1 73.29(16) . . ? C15 C16 Os1 73.07(15) . . ? C17 C16 H16A 119.1 . . ? C15 C16 H16A 119.1 . . ? Os1 C16 H16A 119.1 . . ? C16 C17 C18 117.9(3) . . ? C16 C17 C24 121.4(3) . . ? C18 C17 C24 120.7(3) . . ? C16 C17 Os1 69.25(15) . . ? C18 C17 Os1 71.38(15) . . ? C24 C17 Os1 129.3(2) . . ? C19 C18 C17 120.8(3) . . ? C19 C18 Os1 71.15(15) . . ? C17 C18 Os1 71.25(16) . . ? C19 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? Os1 C18 H18A 118.9 . . ? C18 C19 C20 121.2(3) . . ? C18 C19 Os1 71.88(15) . . ? C20 C19 Os1 73.03(16) . . ? C18 C19 H19A 119.0 . . ? C20 C19 H19A 119.0 . . ? Os1 C19 H19A 119.0 . . ? C15 C20 C19 117.9(3) . . ? C15 C20 C21 122.7(3) . . ? C19 C20 C21 119.4(2) . . ? C15 C20 Os1 70.38(16) . . ? C19 C20 Os1 69.62(16) . . ? C21 C20 Os1 130.69(17) . . ? C20 C21 C22 114.8(2) . . ? C20 C21 C23 107.0(2) . . ? C22 C21 C23 111.0(3) . . ? C20 C21 H21A 108.0 . . ? C22 C21 H21A 108.0 . . ? C23 C21 H21A 108.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C17 C24 H24A 109.5 . . ? C17 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C17 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F13 P10 F12 90.47(11) . . ? F13 P10 F11 90.21(11) . . ? F12 P10 F11 179.33(11) . . ? F13 P10 F15 90.53(11) . . ? F12 P10 F15 89.99(10) . . ? F11 P10 F15 89.99(10) . . ? F13 P10 F14 179.06(11) . . ? F12 P10 F14 89.48(11) . . ? F11 P10 F14 89.85(10) . . ? F15 P10 F14 90.41(10) . . ? F13 P10 F16 90.01(10) . . ? F12 P10 F16 90.27(10) . . ? F11 P10 F16 89.74(9) . . ? F15 P10 F16 179.40(11) . . ? F14 P10 F16 89.05(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C15 H15A F11 1.00 2.54 3.146(3) 119.0 2_665 C15 H15A F16 1.00 2.36 3.335(3) 165.3 2_665 C5 H5A Cl1 0.95 2.80 3.702(3) 158.3 2_656 _diffrn_measured_fraction_theta_max 0.845 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.800 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.122 # Attachment '- fy14_complex14.cif' data_fy14 _database_code_depnum_ccdc_archive 'CCDC 821521' #TrackingRef '- fy14_complex14.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H22 Cl F6 I N3 Os P' _chemical_formula_weight 813.94 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 '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 7.6626(5) _cell_length_b 11.9693(8) _cell_length_c 13.6120(6) _cell_angle_alpha 99.966(5) _cell_angle_beta 102.906(5) _cell_angle_gamma 91.374(5) _cell_volume 1195.99(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7206 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 29.20 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 6.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.23 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 5 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. The PF6 was modelled as disordered over two positions and refined to the ratio of 52:48. Restraints were used to give both components chemically sensible bond angles and distances ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 10563 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 29.21 _reflns_number_total 5555 _reflns_number_gt 4898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0467P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5555 _refine_ls_number_parameters 365 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0779 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.43064(2) 0.318209(15) 0.735337(13) 0.00900(7) Uani 1 1 d . . . I2 I 0.14292(4) 0.42674(3) 0.77612(2) 0.01378(8) Uani 1 1 d . . . N1 N 0.4328(5) 0.2549(3) 0.8674(3) 0.0119(8) Uani 1 1 d . . . C2 C 0.3367(6) 0.1630(4) 0.8768(4) 0.0117(9) Uani 1 1 d . . . H2A H 0.2554 0.1203 0.8186 0.014 Uiso 1 1 calc R . . Cl3 Cl 0.22535(16) 0.01495(11) 0.98062(10) 0.0189(3) Uani 1 1 d . . . C3 C 0.3570(6) 0.1313(4) 0.9713(4) 0.0135(10) Uani 1 1 d . . . C4 C 0.4794(6) 0.1885(4) 1.0574(4) 0.0153(10) Uani 1 1 d . . . H4A H 0.4986 0.1623 1.1208 0.018 Uiso 1 1 calc R . . C5 C 0.5719(6) 0.2842(4) 1.0480(4) 0.0153(10) Uani 1 1 d . . . H5A H 0.6541 0.3273 1.1057 0.018 Uiso 1 1 calc R . . C6 C 0.5440(6) 0.3173(4) 0.9531(3) 0.0119(9) Uani 1 1 d . . . N7 N 0.6302(5) 0.4154(3) 0.9423(3) 0.0130(8) Uani 1 1 d . . . N8 N 0.5904(5) 0.4336(3) 0.8490(3) 0.0112(8) Uani 1 1 d . . . C9 C 0.6785(6) 0.5367(4) 0.8380(4) 0.0127(10) Uani 1 1 d . . . C10 C 0.8331(6) 0.5841(4) 0.9112(4) 0.0169(10) Uani 1 1 d . . . H10A H 0.8798 0.5488 0.9681 0.020 Uiso 1 1 calc R . . C11 C 0.9169(7) 0.6833(5) 0.8994(4) 0.0199(11) Uani 1 1 d . . . H11A H 1.0222 0.7156 0.9485 0.024 Uiso 1 1 calc R . . C12 C 0.8504(7) 0.7356(5) 0.8180(4) 0.0212(11) Uani 1 1 d . . . H12A H 0.9115 0.8022 0.8100 0.025 Uiso 1 1 calc R . . C13 C 0.6922(7) 0.6906(4) 0.7468(4) 0.0170(10) Uani 1 1 d . . . H13A H 0.6442 0.7274 0.6911 0.020 Uiso 1 1 calc R . . C14 C 0.6061(7) 0.5917(4) 0.7581(4) 0.0154(10) Uani 1 1 d . . . H14A H 0.4972 0.5618 0.7110 0.018 Uiso 1 1 calc R . . C15 C 0.6389(6) 0.2740(4) 0.6484(4) 0.0132(10) Uani 1 1 d . . . H15A H 0.7679 0.2959 0.6823 0.016 Uiso 1 1 calc R . . C16 C 0.5305(7) 0.3547(4) 0.6008(3) 0.0151(10) Uani 1 1 d . . . H16A H 0.5860 0.4323 0.6047 0.018 Uiso 1 1 calc R . . C17 C 0.3422(6) 0.3368(4) 0.5694(4) 0.0158(10) Uani 1 1 d . . . C18 C 0.2629(6) 0.2323(4) 0.5830(3) 0.0128(10) Uani 1 1 d . . . H18A H 0.1297 0.2245 0.5741 0.015 Uiso 1 1 calc R . . C19 C 0.3666(6) 0.1518(4) 0.6279(3) 0.0128(10) Uani 1 1 d . . . H19A H 0.3048 0.0885 0.6489 0.015 Uiso 1 1 calc R . . C20 C 0.5575(6) 0.1710(4) 0.6632(4) 0.0116(9) Uani 1 1 d . . . C21 C 0.6665(6) 0.0842(4) 0.7143(4) 0.0162(10) Uani 1 1 d . . . H21A H 0.5879 0.0439 0.7485 0.019 Uiso 1 1 calc R . . C22 C 0.8339(7) 0.1356(5) 0.7958(5) 0.0296(13) Uani 1 1 d . . . H22A H 0.7988 0.1915 0.8483 0.044 Uiso 1 1 calc R . . H22B H 0.9156 0.1729 0.7636 0.044 Uiso 1 1 calc R . . H22C H 0.8945 0.0752 0.8276 0.044 Uiso 1 1 calc R . . C23 C 0.7159(8) -0.0029(5) 0.6308(4) 0.0238(12) Uani 1 1 d . . . H23A H 0.6063 -0.0371 0.5814 0.036 Uiso 1 1 calc R . . H23B H 0.7814 -0.0622 0.6617 0.036 Uiso 1 1 calc R . . H23C H 0.7917 0.0349 0.5954 0.036 Uiso 1 1 calc R . . C24 C 0.2310(7) 0.4236(4) 0.5227(4) 0.0204(11) Uani 1 1 d . . . H24A H 0.2921 0.4992 0.5492 0.031 Uiso 1 1 calc R . . H24B H 0.1138 0.4221 0.5402 0.031 Uiso 1 1 calc R . . H24C H 0.2142 0.4063 0.4480 0.031 Uiso 1 1 calc R . . P10 P 0.19715(19) 0.81868(12) 0.64434(12) 0.0255(3) Uani 1 1 d DU . . F11 F 0.1747(9) 0.8835(6) 0.5545(6) 0.0280(9) Uani 0.524(4) 1 d PDU A 1 F12 F 0.2243(8) 0.7602(6) 0.7492(5) 0.0286(9) Uani 0.524(4) 1 d PDU A 1 F13 F 0.1350(9) 0.9312(6) 0.7180(6) 0.0311(9) Uani 0.524(4) 1 d PDU A 1 F14 F 0.2580(9) 0.7110(5) 0.5860(6) 0.0309(8) Uani 0.524(4) 1 d PDU A 1 F15 F -0.0049(14) 0.7708(10) 0.6212(10) 0.0258(9) Uani 0.524(4) 1 d PDU A 1 F16 F 0.4011(8) 0.8729(5) 0.6925(6) 0.0291(9) Uani 0.524(4) 1 d PDU A 1 F11A F 0.1216(10) 0.9048(7) 0.5626(7) 0.0254(9) Uani 0.476(4) 1 d PDU A 2 F12A F 0.2638(9) 0.7276(6) 0.7104(6) 0.0297(8) Uani 0.476(4) 1 d PDU A 2 F13A F 0.2104(11) 0.9170(7) 0.7311(6) 0.0335(10) Uani 0.476(4) 1 d PDU A 2 F14A F 0.1835(9) 0.7175(6) 0.5387(6) 0.0285(9) Uani 0.476(4) 1 d PDU A 2 F15A F -0.0083(16) 0.7848(11) 0.6317(12) 0.0254(9) Uani 0.476(4) 1 d PDU A 2 F16A F 0.3977(8) 0.8487(6) 0.6313(6) 0.0306(9) Uani 0.476(4) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.01150(10) 0.00841(10) 0.00647(10) 0.00041(7) 0.00155(7) 0.00030(7) I2 0.01251(15) 0.01459(17) 0.01314(16) -0.00004(13) 0.00246(12) 0.00247(12) N1 0.0134(19) 0.011(2) 0.010(2) 0.0000(16) 0.0015(15) 0.0029(16) C2 0.010(2) 0.015(2) 0.008(2) 0.0004(19) -0.0005(17) 0.0002(18) Cl3 0.0238(6) 0.0158(6) 0.0198(6) 0.0084(5) 0.0069(5) -0.0007(5) C3 0.014(2) 0.013(2) 0.017(2) 0.005(2) 0.0091(19) 0.0050(19) C4 0.018(2) 0.019(3) 0.010(2) 0.005(2) 0.0033(19) 0.007(2) C5 0.018(2) 0.018(3) 0.008(2) -0.002(2) 0.0023(19) 0.006(2) C6 0.014(2) 0.015(2) 0.005(2) -0.0022(19) 0.0023(17) 0.0052(19) N7 0.015(2) 0.012(2) 0.010(2) -0.0005(16) 0.0005(15) 0.0022(16) N8 0.0108(18) 0.013(2) 0.0086(19) -0.0022(16) 0.0028(15) -0.0012(16) C9 0.016(2) 0.008(2) 0.014(2) -0.0028(19) 0.0059(19) 0.0019(19) C10 0.014(2) 0.017(3) 0.018(3) -0.001(2) 0.0027(19) 0.004(2) C11 0.012(2) 0.020(3) 0.025(3) -0.003(2) 0.005(2) 0.000(2) C12 0.024(3) 0.016(3) 0.026(3) -0.001(2) 0.015(2) 0.000(2) C13 0.026(3) 0.013(2) 0.015(3) 0.003(2) 0.010(2) 0.002(2) C14 0.020(2) 0.012(2) 0.014(2) -0.001(2) 0.007(2) -0.001(2) C15 0.020(2) 0.011(2) 0.010(2) 0.0001(19) 0.0063(19) 0.0006(19) C16 0.028(3) 0.015(2) 0.005(2) 0.0010(19) 0.0078(19) 0.001(2) C17 0.020(2) 0.019(3) 0.008(2) 0.001(2) 0.0040(19) 0.001(2) C18 0.017(2) 0.015(2) 0.005(2) 0.0022(19) -0.0006(18) 0.0012(19) C19 0.023(2) 0.009(2) 0.006(2) -0.0015(18) 0.0048(19) -0.0004(19) C20 0.015(2) 0.011(2) 0.010(2) 0.0020(19) 0.0047(18) 0.0027(19) C21 0.019(2) 0.015(3) 0.015(3) 0.004(2) 0.003(2) 0.005(2) C22 0.025(3) 0.029(3) 0.030(3) 0.008(3) -0.006(2) 0.005(3) C23 0.035(3) 0.017(3) 0.024(3) 0.005(2) 0.014(2) 0.014(2) C24 0.030(3) 0.016(3) 0.015(3) 0.003(2) 0.003(2) 0.000(2) P10 0.0222(6) 0.0191(7) 0.0337(8) 0.0093(6) 0.0004(5) 0.0000(5) F11 0.0272(17) 0.0232(16) 0.0345(16) 0.0133(15) 0.0032(16) 0.0003(15) F12 0.0263(16) 0.0234(16) 0.0336(17) 0.0108(15) -0.0029(15) 0.0026(14) F13 0.0241(17) 0.0236(16) 0.0375(16) -0.0016(15) -0.0049(16) 0.0055(16) F14 0.0279(14) 0.0247(14) 0.0373(15) 0.0044(14) 0.0022(13) 0.0044(13) F15 0.0222(14) 0.0204(17) 0.0329(17) 0.0078(15) -0.0002(14) 0.0005(14) F16 0.0237(15) 0.0235(16) 0.0381(17) 0.0073(16) 0.0019(16) -0.0034(14) F11A 0.0229(17) 0.0212(16) 0.0339(16) 0.0127(15) 0.0043(16) 0.0028(15) F12A 0.0268(14) 0.0232(14) 0.0359(15) 0.0092(13) -0.0023(13) 0.0040(13) F13A 0.0296(17) 0.0247(16) 0.0377(17) -0.0006(15) -0.0055(16) 0.0023(16) F14A 0.0252(16) 0.0236(16) 0.0344(17) 0.0046(15) 0.0026(15) 0.0045(15) F15A 0.0219(15) 0.0203(17) 0.0327(17) 0.0080(15) 0.0009(14) 0.0009(15) F16A 0.0247(15) 0.0254(16) 0.0389(17) 0.0091(16) -0.0006(16) -0.0033(15) _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 Os1 N8 2.033(4) . ? Os1 N1 2.065(4) . ? Os1 C15 2.213(5) . ? Os1 C20 2.219(5) . ? Os1 C19 2.230(5) . ? Os1 C16 2.239(5) . ? Os1 C18 2.240(5) . ? Os1 C17 2.260(5) . ? Os1 I2 2.7002(4) . ? N1 C2 1.349(6) . ? N1 C6 1.367(6) . ? C2 C3 1.380(7) . ? C2 H2A 0.9500 . ? Cl3 C3 1.739(5) . ? C3 C4 1.387(7) . ? C4 C5 1.372(7) . ? C4 H4A 0.9500 . ? C5 C6 1.389(7) . ? C5 H5A 0.9500 . ? C6 N7 1.379(6) . ? N7 N8 1.296(5) . ? N8 C9 1.439(6) . ? C9 C14 1.386(7) . ? C9 C10 1.401(7) . ? C10 C11 1.387(7) . ? C10 H10A 0.9500 . ? C11 C12 1.371(8) . ? C11 H11A 0.9500 . ? C12 C13 1.401(7) . ? C12 H12A 0.9500 . ? C13 C14 1.390(7) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.434(7) . ? C15 C16 1.434(7) . ? C15 H15A 1.0000 . ? C16 C17 1.410(7) . ? C16 H16A 1.0000 . ? C17 C18 1.436(7) . ? C17 C24 1.497(7) . ? C18 C19 1.399(7) . ? C18 H18A 1.0000 . ? C19 C20 1.434(6) . ? C19 H19A 1.0000 . ? C20 C21 1.515(7) . ? C21 C23 1.524(7) . ? C21 C22 1.531(7) . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? P10 F13A 1.500(8) . ? P10 F14 1.532(6) . ? P10 F11 1.539(7) . ? P10 F12A 1.555(7) . ? P10 F15A 1.580(12) . ? P10 F15 1.582(10) . ? P10 F16 1.625(6) . ? P10 F16A 1.625(7) . ? P10 F11A 1.665(8) . ? P10 F12 1.670(7) . ? P10 F13 1.680(7) . ? P10 F14A 1.694(7) . ? 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 N8 Os1 N1 75.47(16) . . ? N8 Os1 C15 95.73(16) . . ? N1 Os1 C15 120.19(17) . . ? N8 Os1 C20 117.80(16) . . ? N1 Os1 C20 94.52(16) . . ? C15 Os1 C20 37.75(17) . . ? N8 Os1 C19 154.39(17) . . ? N1 Os1 C19 96.31(16) . . ? C15 Os1 C19 67.07(17) . . ? C20 Os1 C19 37.61(17) . . ? N8 Os1 C16 99.81(17) . . ? N1 Os1 C16 157.49(17) . . ? C15 Os1 C16 37.58(18) . . ? C20 Os1 C16 67.83(18) . . ? C19 Os1 C16 78.40(18) . . ? N8 Os1 C18 162.69(17) . . ? N1 Os1 C18 121.55(17) . . ? C15 Os1 C18 78.74(18) . . ? C20 Os1 C18 67.17(17) . . ? C19 Os1 C18 36.46(17) . . ? C16 Os1 C18 65.80(18) . . ? N8 Os1 C17 125.53(17) . . ? N1 Os1 C17 158.32(17) . . ? C15 Os1 C17 67.40(18) . . ? C20 Os1 C17 80.55(18) . . ? C19 Os1 C17 66.95(18) . . ? C16 Os1 C17 36.52(17) . . ? C18 Os1 C17 37.21(17) . . ? N8 Os1 I2 88.76(11) . . ? N1 Os1 I2 84.98(11) . . ? C15 Os1 I2 154.78(13) . . ? C20 Os1 I2 152.51(12) . . ? C19 Os1 I2 115.02(12) . . ? C16 Os1 I2 117.20(13) . . ? C18 Os1 I2 89.66(12) . . ? C17 Os1 I2 89.81(13) . . ? C2 N1 C6 118.8(4) . . ? C2 N1 Os1 127.4(3) . . ? C6 N1 Os1 113.7(3) . . ? N1 C2 C3 119.8(4) . . ? N1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C2 C3 C4 122.0(4) . . ? C2 C3 Cl3 118.2(4) . . ? C4 C3 Cl3 119.8(4) . . ? C5 C4 C3 117.7(5) . . ? C5 C4 H4A 121.1 . . ? C3 C4 H4A 121.1 . . ? C4 C5 C6 119.2(4) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? N1 C6 N7 117.5(4) . . ? N1 C6 C5 122.1(5) . . ? N7 C6 C5 120.4(4) . . ? N8 N7 C6 112.6(4) . . ? N7 N8 C9 112.6(4) . . ? N7 N8 Os1 120.5(3) . . ? C9 N8 Os1 126.8(3) . . ? C14 C9 C10 120.1(5) . . ? C14 C9 N8 120.2(4) . . ? C10 C9 N8 119.7(4) . . ? C11 C10 C9 119.0(5) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C12 C11 C10 121.2(5) . . ? C12 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C11 C12 C13 119.9(5) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 119.5(5) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C9 C14 C13 120.2(5) . . ? C9 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C20 C15 C16 120.3(4) . . ? C20 C15 Os1 71.3(3) . . ? C16 C15 Os1 72.2(3) . . ? C20 C15 H15A 119.4 . . ? C16 C15 H15A 119.4 . . ? Os1 C15 H15A 119.4 . . ? C17 C16 C15 121.5(5) . . ? C17 C16 Os1 72.5(3) . . ? C15 C16 Os1 70.2(3) . . ? C17 C16 H16A 118.5 . . ? C15 C16 H16A 118.5 . . ? Os1 C16 H16A 118.5 . . ? C16 C17 C18 117.5(4) . . ? C16 C17 C24 120.7(5) . . ? C18 C17 C24 121.8(4) . . ? C16 C17 Os1 71.0(3) . . ? C18 C17 Os1 70.7(3) . . ? C24 C17 Os1 129.9(3) . . ? C19 C18 C17 121.8(4) . . ? C19 C18 Os1 71.4(3) . . ? C17 C18 Os1 72.1(3) . . ? C19 C18 H18A 118.5 . . ? C17 C18 H18A 118.5 . . ? Os1 C18 H18A 118.5 . . ? C18 C19 C20 121.1(4) . . ? C18 C19 Os1 72.2(3) . . ? C20 C19 Os1 70.8(3) . . ? C18 C19 H19A 118.8 . . ? C20 C19 H19A 118.8 . . ? Os1 C19 H19A 118.8 . . ? C15 C20 C19 117.7(4) . . ? C15 C20 C21 122.1(4) . . ? C19 C20 C21 120.2(4) . . ? C15 C20 Os1 70.9(3) . . ? C19 C20 Os1 71.6(3) . . ? C21 C20 Os1 128.4(3) . . ? C20 C21 C23 108.0(4) . . ? C20 C21 C22 114.0(4) . . ? C23 C21 C22 111.0(4) . . ? C20 C21 H21A 107.9 . . ? C23 C21 H21A 107.9 . . ? C22 C21 H21A 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C17 C24 H24A 109.5 . . ? C17 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C17 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F13A P10 F14 155.8(4) . . ? F13A P10 F11 99.5(5) . . ? F14 P10 F11 94.7(4) . . ? F13A P10 F12A 97.3(4) . . ? F14 P10 F12A 65.0(4) . . ? F11 P10 F12A 158.4(4) . . ? F13A P10 F15A 96.3(5) . . ? F14 P10 F15A 101.3(5) . . ? F11 P10 F15A 97.2(7) . . ? F12A P10 F15A 94.3(7) . . ? F13A P10 F15 103.7(5) . . ? F14 P10 F15 93.9(5) . . ? F11 P10 F15 96.6(6) . . ? F12A P10 F15 92.4(6) . . ? F15A P10 F15 7.5(8) . . ? F13A P10 F16 66.9(4) . . ? F14 P10 F16 93.3(4) . . ? F11 P10 F16 92.1(4) . . ? F12A P10 F16 82.1(4) . . ? F15A P10 F16 161.9(6) . . ? F15 P10 F16 168.2(6) . . ? F13A P10 F16A 92.7(4) . . ? F14 P10 F16A 72.7(4) . . ? F11 P10 F16A 73.3(4) . . ? F12A P10 F16A 92.5(4) . . ? F15A P10 F16A 168.0(6) . . ? F15 P10 F16A 162.2(6) . . ? F16 P10 F16A 29.5(3) . . ? F13A P10 F11A 88.9(4) . . ? F14 P10 F11A 109.2(4) . . ? F11 P10 F11A 17.7(4) . . ? F12A P10 F11A 173.8(4) . . ? F15A P10 F11A 84.4(6) . . ? F15 P10 F11A 85.5(6) . . ? F16 P10 F11A 100.9(4) . . ? F16A P10 F11A 87.8(4) . . ? F13A P10 F12 75.1(4) . . ? F14 P10 F12 90.2(4) . . ? F11 P10 F12 174.6(4) . . ? F12A P10 F12 25.7(3) . . ? F15A P10 F12 84.0(7) . . ? F15 P10 F12 85.3(6) . . ? F16 P10 F12 85.4(3) . . ? F16A P10 F12 106.1(3) . . ? F11A P10 F12 159.0(4) . . ? F13A P10 F13 20.9(3) . . ? F14 P10 F13 174.7(4) . . ? F11 P10 F13 90.6(4) . . ? F12A P10 F13 109.7(4) . . ? F15A P10 F13 78.7(5) . . ? F15 P10 F13 86.1(5) . . ? F16 P10 F13 85.8(3) . . ? F16A P10 F13 108.3(4) . . ? F11A P10 F13 76.1(4) . . ? F12 P10 F13 84.5(4) . . ? F13A P10 F14A 174.2(4) . . ? F14 P10 F14A 27.2(3) . . ? F11 P10 F14A 74.7(4) . . ? F12A P10 F14A 88.1(4) . . ? F15A P10 F14A 85.5(5) . . ? F15 P10 F14A 78.2(5) . . ? F16 P10 F14A 111.9(4) . . ? F16A P10 F14A 84.8(4) . . ? F11A P10 F14A 85.8(4) . . ? F12 P10 F14A 110.6(4) . . ? F13 P10 F14A 156.9(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2A F13 0.95 2.47 3.315(8) 147.8 1_545 C4 H4A F12 0.95 2.48 3.027(8) 116.5 2_667 C5 H5A F12 0.95 2.41 2.994(8) 119.5 2_667 C18 H18A F15 1.00 2.63 3.024(14) 103.6 2_566 C24 H24C F15 0.98 2.53 2.994(11) 108.5 2_566 _diffrn_measured_fraction_theta_max 0.854 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.683 _refine_diff_density_min -1.828 _refine_diff_density_rms 0.197 # Attachment '- fy17_complex13.cif' data_fy17 _database_code_depnum_ccdc_archive 'CCDC 821522' #TrackingRef '- fy17_complex13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H18 Cl F6 I N3 Os P' _chemical_formula_weight 833.92 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 '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 6.9574(2) _cell_length_b 16.7829(6) _cell_length_c 20.7297(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.182(3) _cell_angle_gamma 90.00 _cell_volume 2416.78(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9509 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 29.27 _exptl_crystal_description block _exptl_crystal_colour block _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 6.796 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 13972 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 29.33 _reflns_number_total 5709 _reflns_number_gt 5033 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0222P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5709 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0484 _refine_ls_wR_factor_gt 0.0475 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Os1 Os 0.172603(16) 0.615995(7) 0.290764(6) 0.00741(4) Uani 1 1 d . . . I1 I -0.18441(3) 0.551836(13) 0.289826(9) 0.01117(5) Uani 1 1 d . . . N1 N 0.2431(4) 0.52939(16) 0.35817(12) 0.0095(5) Uani 1 1 d . . . C2 C 0.2268(4) 0.53339(19) 0.42266(14) 0.0107(7) Uani 1 1 d . . . H2A H 0.1837 0.5813 0.4415 0.013 Uiso 1 1 calc R . . Cl3 Cl 0.24359(12) 0.47595(5) 0.54356(4) 0.01688(18) Uani 1 1 d . . . C3 C 0.2718(5) 0.4690(2) 0.46135(15) 0.0136(7) Uani 1 1 d . . . C4 C 0.3399(5) 0.3987(2) 0.43620(16) 0.0160(7) Uani 1 1 d . . . H4A H 0.3742 0.3548 0.4634 0.019 Uiso 1 1 calc R . . C5 C 0.3565(5) 0.3946(2) 0.37028(16) 0.0155(7) Uani 1 1 d . . . H5A H 0.4025 0.3475 0.3509 0.019 Uiso 1 1 calc R . . C6 C 0.3048(5) 0.46012(19) 0.33299(15) 0.0121(7) Uani 1 1 d . . . N7 N 0.3093(4) 0.45578(16) 0.26652(12) 0.0122(6) Uani 1 1 d . . . N8 N 0.2497(4) 0.52120(16) 0.23926(12) 0.0099(5) Uani 1 1 d . . . C9 C 0.2500(4) 0.51829(19) 0.16985(14) 0.0101(6) Uani 1 1 d . . . C10 C 0.1103(5) 0.56010(19) 0.13345(15) 0.0118(7) Uani 1 1 d . . . H10A H 0.0154 0.5903 0.1539 0.014 Uiso 1 1 calc R . . C11 C 0.1121(5) 0.5568(2) 0.06647(16) 0.0152(7) Uani 1 1 d . . . H11A H 0.0190 0.5857 0.0407 0.018 Uiso 1 1 calc R . . C12 C 0.2495(5) 0.5115(2) 0.03720(16) 0.0177(8) Uani 1 1 d . . . H12A H 0.2497 0.5094 -0.0086 0.021 Uiso 1 1 calc R . . C13 C 0.3861(5) 0.4693(2) 0.07420(16) 0.0169(7) Uani 1 1 d . . . H13A H 0.4784 0.4376 0.0538 0.020 Uiso 1 1 calc R . . C14 C 0.3883(5) 0.4731(2) 0.14103(15) 0.0120(7) Uani 1 1 d . . . H14A H 0.4833 0.4452 0.1667 0.014 Uiso 1 1 calc R . . C15 C 0.0600(4) 0.72834(18) 0.24672(15) 0.0098(6) Uani 1 1 d . . . H15A H -0.0644 0.7279 0.2201 0.012 Uiso 1 1 calc R . . C16 C 0.2319(5) 0.70859(19) 0.21797(16) 0.0133(7) Uani 1 1 d . . . H16A H 0.2271 0.6937 0.1712 0.016 Uiso 1 1 calc R . . C17 C 0.4021(5) 0.69327(19) 0.25672(16) 0.0141(7) Uani 1 1 d . . . H17A H 0.5153 0.6687 0.2367 0.017 Uiso 1 1 calc R . . C18 C 0.3991(4) 0.69770(18) 0.32407(16) 0.0117(7) Uani 1 1 d . . . H18A H 0.5113 0.6776 0.3516 0.014 Uiso 1 1 calc R . . C19 C 0.2280(4) 0.72446(18) 0.35376(15) 0.0095(6) Uani 1 1 d . . . H19A H 0.2205 0.7192 0.4016 0.011 Uiso 1 1 calc R . . C20 C 0.0592(4) 0.74121(18) 0.31576(15) 0.0090(6) Uani 1 1 d . . . C21 C -0.1143(4) 0.77283(19) 0.34540(15) 0.0099(6) Uani 1 1 d . . . C22 C -0.1509(4) 0.7585(2) 0.40974(15) 0.0129(7) Uani 1 1 d . . . H22A H -0.0715 0.7226 0.4345 0.016 Uiso 1 1 calc R . . C23 C -0.3026(5) 0.7964(2) 0.43792(16) 0.0156(7) Uani 1 1 d . . . H23A H -0.3262 0.7864 0.4819 0.019 Uiso 1 1 calc R . . C24 C -0.4188(5) 0.8486(2) 0.40227(16) 0.0159(7) Uani 1 1 d . . . H24A H -0.5216 0.8748 0.4218 0.019 Uiso 1 1 calc R . . C25 C -0.3859(5) 0.8628(2) 0.33766(17) 0.0155(7) Uani 1 1 d . . . H25A H -0.4668 0.8984 0.3130 0.019 Uiso 1 1 calc R . . C26 C -0.2351(5) 0.8250(2) 0.30937(16) 0.0133(7) Uani 1 1 d . . . H26A H -0.2135 0.8344 0.2652 0.016 Uiso 1 1 calc R . . P10 P 0.19784(13) 0.75673(6) 0.57821(4) 0.01621(19) Uani 1 1 d . . . F11 F 0.2159(4) 0.68815(14) 0.52492(11) 0.0363(6) Uani 1 1 d . . . F12 F 0.1836(3) 0.82520(15) 0.63096(11) 0.0364(6) Uani 1 1 d . . . F13 F -0.0309(3) 0.75000(15) 0.57104(11) 0.0348(6) Uani 1 1 d . . . F14 F 0.4298(3) 0.76306(12) 0.58558(9) 0.0224(5) Uani 1 1 d . . . F15 F 0.2062(3) 0.69106(15) 0.63394(11) 0.0396(6) Uani 1 1 d . . . F16 F 0.1952(3) 0.82162(14) 0.52236(10) 0.0303(5) 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 Os1 0.00784(6) 0.00628(7) 0.00805(6) -0.00009(5) -0.00021(4) 0.00074(5) I1 0.00904(10) 0.01217(11) 0.01225(10) 0.00052(9) -0.00001(7) -0.00083(8) N1 0.0099(13) 0.0098(14) 0.0085(12) -0.0006(12) -0.0018(10) 0.0013(11) C2 0.0098(15) 0.0103(17) 0.0120(15) -0.0001(14) 0.0006(12) 0.0009(12) Cl3 0.0176(4) 0.0231(5) 0.0099(4) 0.0025(4) 0.0008(3) 0.0001(3) C3 0.0119(16) 0.0188(19) 0.0099(15) -0.0013(15) -0.0008(12) -0.0038(13) C4 0.0193(18) 0.0112(18) 0.0168(17) 0.0046(15) -0.0048(14) -0.0017(14) C5 0.0221(18) 0.0091(17) 0.0151(16) 0.0001(15) 0.0000(14) 0.0019(14) C6 0.0135(16) 0.0096(17) 0.0131(15) -0.0035(14) -0.0007(12) 0.0020(13) N7 0.0156(14) 0.0081(14) 0.0126(13) 0.0024(12) -0.0017(11) 0.0021(11) N8 0.0082(13) 0.0091(14) 0.0123(13) -0.0006(12) 0.0006(10) -0.0020(11) C9 0.0132(16) 0.0091(16) 0.0081(14) -0.0018(14) 0.0017(12) -0.0048(13) C10 0.0131(16) 0.0061(16) 0.0160(16) -0.0025(14) 0.0002(13) -0.0020(13) C11 0.0181(17) 0.0125(18) 0.0147(16) 0.0022(15) -0.0021(13) -0.0047(14) C12 0.0223(18) 0.0195(19) 0.0116(15) -0.0023(16) 0.0025(13) -0.0088(15) C13 0.0154(17) 0.0182(19) 0.0177(17) -0.0063(16) 0.0064(13) -0.0041(14) C14 0.0116(16) 0.0108(17) 0.0134(16) -0.0026(14) -0.0010(12) -0.0004(13) C15 0.0132(15) 0.0021(15) 0.0138(15) 0.0020(14) -0.0009(12) -0.0004(12) C16 0.0187(17) 0.0056(16) 0.0160(16) -0.0007(15) 0.0038(13) 0.0001(13) C17 0.0157(16) 0.0060(16) 0.0211(17) 0.0042(15) 0.0052(13) -0.0020(13) C18 0.0093(15) 0.0059(16) 0.0194(16) -0.0019(14) -0.0027(12) -0.0013(12) C19 0.0105(15) 0.0030(15) 0.0147(15) 0.0025(14) -0.0025(12) -0.0021(12) C20 0.0098(15) 0.0032(15) 0.0143(15) -0.0013(13) 0.0022(12) -0.0005(12) C21 0.0087(15) 0.0056(16) 0.0153(15) -0.0035(14) 0.0009(12) -0.0006(12) C22 0.0122(16) 0.0133(17) 0.0130(15) -0.0030(14) -0.0021(12) 0.0044(13) C23 0.0169(17) 0.0157(18) 0.0144(15) -0.0083(15) 0.0017(13) -0.0030(14) C24 0.0134(16) 0.0131(18) 0.0213(17) -0.0073(16) 0.0017(13) -0.0011(14) C25 0.0141(16) 0.0079(17) 0.0243(18) -0.0024(15) -0.0009(14) 0.0012(13) C26 0.0137(16) 0.0095(17) 0.0164(16) -0.0009(15) -0.0008(13) -0.0038(13) P10 0.0193(5) 0.0163(5) 0.0125(4) 0.0009(4) -0.0039(3) -0.0019(4) F11 0.0500(15) 0.0249(13) 0.0324(12) -0.0150(11) -0.0115(11) 0.0047(11) F12 0.0341(13) 0.0425(15) 0.0324(12) -0.0214(12) 0.0013(10) 0.0044(11) F13 0.0188(11) 0.0483(16) 0.0367(13) 0.0064(12) -0.0053(10) -0.0087(11) F14 0.0192(10) 0.0228(12) 0.0246(11) 0.0045(10) -0.0032(8) 0.0020(9) F15 0.0420(14) 0.0436(16) 0.0318(12) 0.0257(12) -0.0098(11) -0.0139(12) F16 0.0306(12) 0.0292(13) 0.0306(12) 0.0175(11) -0.0046(10) 0.0016(10) _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 Os1 N8 2.006(3) . ? Os1 N1 2.057(3) . ? Os1 C18 2.172(3) . ? Os1 C17 2.203(3) . ? Os1 C15 2.219(3) . ? Os1 C16 2.221(3) . ? Os1 C19 2.261(3) . ? Os1 C20 2.313(3) . ? Os1 I1 2.7063(2) . ? N1 C2 1.350(4) . ? N1 C6 1.354(4) . ? C2 C3 1.372(5) . ? C2 H2A 0.9500 . ? Cl3 C3 1.730(3) . ? C3 C4 1.384(5) . ? C4 C5 1.379(5) . ? C4 H4A 0.9500 . ? C5 C6 1.381(5) . ? C5 H5A 0.9500 . ? C6 N7 1.382(4) . ? N7 N8 1.293(4) . ? N8 C9 1.440(4) . ? C9 C14 1.386(4) . ? C9 C10 1.388(4) . ? C10 C11 1.390(4) . ? C10 H10A 0.9500 . ? C11 C12 1.388(5) . ? C11 H11A 0.9500 . ? C12 C13 1.383(5) . ? C12 H12A 0.9500 . ? C13 C14 1.386(4) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.405(4) . ? C15 C20 1.448(4) . ? C15 H15A 1.0000 . ? C16 C17 1.417(5) . ? C16 H16A 1.0000 . ? C17 C18 1.399(4) . ? C17 H17A 1.0000 . ? C18 C19 1.442(4) . ? C18 H18A 1.0000 . ? C19 C20 1.406(4) . ? C19 H19A 1.0000 . ? C20 C21 1.483(4) . ? C21 C22 1.392(4) . ? C21 C26 1.400(4) . ? C22 C23 1.389(4) . ? C22 H22A 0.9500 . ? C23 C24 1.378(5) . ? C23 H23A 0.9500 . ? C24 C25 1.392(5) . ? C24 H24A 0.9500 . ? C25 C26 1.384(5) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? P10 F16 1.589(2) . ? P10 F12 1.593(2) . ? P10 F13 1.594(2) . ? P10 F15 1.595(2) . ? P10 F11 1.605(2) . ? P10 F14 1.616(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 N8 Os1 N1 74.94(10) . . ? N8 Os1 C18 117.34(11) . . ? N1 Os1 C18 95.09(11) . . ? N8 Os1 C17 94.39(11) . . ? N1 Os1 C17 118.94(11) . . ? C18 Os1 C17 37.30(12) . . ? N8 Os1 C15 123.63(11) . . ? N1 Os1 C15 161.02(11) . . ? C18 Os1 C15 80.08(12) . . ? C17 Os1 C15 67.27(12) . . ? N8 Os1 C16 97.36(11) . . ? N1 Os1 C16 155.50(11) . . ? C18 Os1 C16 67.38(12) . . ? C17 Os1 C16 37.35(12) . . ? C15 Os1 C16 36.91(11) . . ? N8 Os1 C19 154.71(11) . . ? N1 Os1 C19 98.63(11) . . ? C18 Os1 C19 37.89(11) . . ? C17 Os1 C19 66.90(12) . . ? C15 Os1 C19 66.33(11) . . ? C16 Os1 C19 78.28(11) . . ? N8 Os1 C20 160.80(11) . . ? N1 Os1 C20 124.14(10) . . ? C18 Os1 C20 66.78(11) . . ? C17 Os1 C20 78.41(11) . . ? C15 Os1 C20 37.19(11) . . ? C16 Os1 C20 66.11(11) . . ? C19 Os1 C20 35.77(11) . . ? N8 Os1 I1 87.31(7) . . ? N1 Os1 I1 84.72(7) . . ? C18 Os1 I1 154.51(8) . . ? C17 Os1 I1 155.92(9) . . ? C15 Os1 I1 91.84(8) . . ? C16 Os1 I1 118.59(9) . . ? C19 Os1 I1 116.84(8) . . ? C20 Os1 I1 92.22(7) . . ? C2 N1 C6 118.1(3) . . ? C2 N1 Os1 127.4(2) . . ? C6 N1 Os1 114.4(2) . . ? N1 C2 C3 120.7(3) . . ? N1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C2 C3 C4 121.5(3) . . ? C2 C3 Cl3 119.2(3) . . ? C4 C3 Cl3 119.2(3) . . ? C5 C4 C3 117.7(3) . . ? C5 C4 H4A 121.1 . . ? C3 C4 H4A 121.1 . . ? C4 C5 C6 118.8(3) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? N1 C6 C5 123.1(3) . . ? N1 C6 N7 117.1(3) . . ? C5 C6 N7 119.8(3) . . ? N8 N7 C6 111.5(3) . . ? N7 N8 C9 112.9(2) . . ? N7 N8 Os1 122.01(19) . . ? C9 N8 Os1 125.0(2) . . ? C14 C9 C10 121.6(3) . . ? C14 C9 N8 119.3(3) . . ? C10 C9 N8 119.1(3) . . ? C9 C10 C11 118.5(3) . . ? C9 C10 H10A 120.7 . . ? C11 C10 H10A 120.7 . . ? C12 C11 C10 120.2(3) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C13 C12 C11 120.5(3) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C14 120.0(3) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C9 C14 C13 119.1(3) . . ? C9 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C16 C15 C20 120.3(3) . . ? C16 C15 Os1 71.62(18) . . ? C20 C15 Os1 74.96(17) . . ? C16 C15 H15A 119.7 . . ? C20 C15 H15A 119.7 . . ? Os1 C15 H15A 119.7 . . ? C15 C16 C17 120.4(3) . . ? C15 C16 Os1 71.47(18) . . ? C17 C16 Os1 70.65(18) . . ? C15 C16 H16A 119.1 . . ? C17 C16 H16A 119.1 . . ? Os1 C16 H16A 119.1 . . ? C18 C17 C16 119.9(3) . . ? C18 C17 Os1 70.15(17) . . ? C16 C17 Os1 72.00(18) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? Os1 C17 H17A 119.5 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 Os1 72.55(18) . . ? C19 C18 Os1 74.39(18) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? Os1 C18 H18A 119.9 . . ? C20 C19 C18 120.5(3) . . ? C20 C19 Os1 74.16(18) . . ? C18 C19 Os1 67.72(17) . . ? C20 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? Os1 C19 H19A 119.1 . . ? C19 C20 C15 118.4(3) . . ? C19 C20 C21 120.9(3) . . ? C15 C20 C21 120.7(3) . . ? C19 C20 Os1 70.08(18) . . ? C15 C20 Os1 67.86(16) . . ? C21 C20 Os1 135.5(2) . . ? C22 C21 C26 118.8(3) . . ? C22 C21 C20 122.1(3) . . ? C26 C21 C20 118.8(3) . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C24 C23 C22 120.2(3) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C26 C25 C24 119.9(3) . . ? C26 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? C25 C26 C21 120.5(3) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? F16 P10 F12 90.41(14) . . ? F16 P10 F13 90.55(12) . . ? F12 P10 F13 90.89(13) . . ? F16 P10 F15 178.51(14) . . ? F12 P10 F15 90.13(14) . . ? F13 P10 F15 90.83(13) . . ? F16 P10 F11 89.32(13) . . ? F12 P10 F11 179.03(14) . . ? F13 P10 F11 90.05(13) . . ? F15 P10 F11 90.12(14) . . ? F16 P10 F14 89.71(11) . . ? F12 P10 F14 89.27(12) . . ? F13 P10 F14 179.70(14) . . ? F15 P10 F14 88.91(12) . . ? F11 P10 F14 89.79(12) . . ? _diffrn_measured_fraction_theta_max 0.860 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.718 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.153 # Attachment '- fy18_complex19.cif' data_fy18 _database_code_depnum_ccdc_archive 'CCDC 821523' #TrackingRef '- fy18_complex19.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H18 Br Cl F6 N3 Os P' _chemical_formula_weight 786.93 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 '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 8.8866(5) _cell_length_b 10.0428(4) _cell_length_c 14.1695(7) _cell_angle_alpha 103.452(4) _cell_angle_beta 94.374(4) _cell_angle_gamma 100.802(4) _cell_volume 1198.54(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8051 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 29.33 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 7.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.41 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 10015 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 29.35 _reflns_number_total 5466 _reflns_number_gt 4836 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0310P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5466 _refine_ls_number_parameters 325 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 1.055 _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 Os1 Os 0.781706(17) 0.133670(15) 0.246250(11) 0.01146(5) Uani 1 1 d . . . Cl1 Cl 0.87070(11) 0.21857(10) 0.11187(7) 0.0183(2) Uani 1 1 d . . . N1 N 0.5727(4) 0.1698(3) 0.1980(2) 0.0155(7) Uani 1 1 d . . . C2 C 0.5242(5) 0.2928(4) 0.2227(3) 0.0174(8) Uani 1 1 d . . . H2A H 0.5910 0.3723 0.2658 0.021 Uiso 1 1 calc R . . C3 C 0.3814(5) 0.3041(4) 0.1866(3) 0.0204(9) Uani 1 1 d . . . Br3 Br 0.32313(5) 0.47783(4) 0.22676(3) 0.02391(10) Uani 1 1 d . . . C4 C 0.2812(5) 0.1902(4) 0.1230(3) 0.0210(9) Uani 1 1 d . . . H4A H 0.1811 0.1973 0.0988 0.025 Uiso 1 1 calc R . . C5 C 0.3316(5) 0.0662(4) 0.0958(3) 0.0186(9) Uani 1 1 d . . . H5A H 0.2668 -0.0136 0.0519 0.022 Uiso 1 1 calc R . . C6 C 0.4787(5) 0.0598(4) 0.1337(3) 0.0172(8) Uani 1 1 d . . . N7 N 0.5336(4) -0.0607(3) 0.1066(2) 0.0167(7) Uani 1 1 d . . . N8 N 0.6697(4) -0.0484(3) 0.1494(2) 0.0151(7) Uani 1 1 d . . . C9 C 0.7291(5) -0.1738(4) 0.1238(3) 0.0182(9) Uani 1 1 d . . . C10 C 0.6281(5) -0.3041(4) 0.1076(3) 0.0252(10) Uani 1 1 d . . . H10A H 0.5210 -0.3101 0.1119 0.030 Uiso 1 1 calc R . . C11 C 0.6869(6) -0.4233(5) 0.0854(4) 0.0313(11) Uani 1 1 d . . . H11A H 0.6177 -0.5115 0.0740 0.038 Uiso 1 1 calc R . . C12 C 0.8471(5) -0.4210(4) 0.0786(3) 0.0175(9) Uani 1 1 d . . . H12A H 0.8873 -0.5038 0.0653 0.021 Uiso 1 1 calc R . . C13 C 0.9399(5) -0.2869(4) 0.0932(3) 0.0237(10) Uani 1 1 d . . . H13A H 1.0465 -0.2789 0.0866 0.028 Uiso 1 1 calc R . . C14 C 0.8830(5) -0.1651(4) 0.1169(3) 0.0196(9) Uani 1 1 d . . . H14A H 0.9508 -0.0762 0.1282 0.023 Uiso 1 1 calc R . . C15 C 0.9811(4) 0.2844(4) 0.3453(3) 0.0178(9) Uani 1 1 d . . . H15A H 1.0409 0.3611 0.3206 0.021 Uiso 1 1 calc R . . C16 C 1.0163(5) 0.1489(4) 0.3188(3) 0.0195(9) Uani 1 1 d . . . H16A H 1.1017 0.1338 0.2780 0.023 Uiso 1 1 calc R . . C17 C 0.9182(5) 0.0339(4) 0.3360(3) 0.0202(9) Uani 1 1 d . . . H17A H 0.9340 -0.0627 0.3077 0.024 Uiso 1 1 calc R . . C18 C 0.7801(5) 0.0515(4) 0.3776(3) 0.0174(9) Uani 1 1 d . . . H18A H 0.7004 -0.0327 0.3785 0.021 Uiso 1 1 calc R . . C19 C 0.7428(5) 0.1856(4) 0.3994(3) 0.0150(8) Uani 1 1 d . . . H19A H 0.6371 0.1944 0.4160 0.018 Uiso 1 1 calc R . . C20 C 0.8478(5) 0.3061(4) 0.3878(3) 0.0151(8) Uani 1 1 d . . . C21 C 0.8096(4) 0.4470(4) 0.4156(3) 0.0163(8) Uani 1 1 d . . . C22 C 0.7244(5) 0.4799(4) 0.4916(3) 0.0207(9) Uani 1 1 d . . . H22A H 0.6926 0.4130 0.5276 0.025 Uiso 1 1 calc R . . C23 C 0.6839(5) 0.6102(4) 0.5165(3) 0.0235(9) Uani 1 1 d . . . H23A H 0.6243 0.6307 0.5688 0.028 Uiso 1 1 calc R . . C24 C 0.7294(6) 0.7085(5) 0.4661(4) 0.0325(11) Uani 1 1 d . . . H24A H 0.7021 0.7973 0.4832 0.039 Uiso 1 1 calc R . . C25 C 0.8171(7) 0.6763(5) 0.3888(4) 0.0445(14) Uani 1 1 d . . . H25A H 0.8501 0.7440 0.3536 0.053 Uiso 1 1 calc R . . C26 C 0.8559(6) 0.5467(5) 0.3637(4) 0.0314(11) Uani 1 1 d . . . H26A H 0.9143 0.5254 0.3108 0.038 Uiso 1 1 calc R . . P10 P 0.69560(13) 0.11741(12) 0.66311(8) 0.0197(2) Uani 1 1 d . . . F11 F 0.8060(3) 0.0604(3) 0.58641(17) 0.0270(6) Uani 1 1 d . . . F12 F 0.5848(4) 0.1727(3) 0.7396(2) 0.0454(8) Uani 1 1 d . . . F13 F 0.6033(3) -0.0394(3) 0.6510(2) 0.0469(8) Uani 1 1 d . . . F14 F 0.7914(4) 0.2724(3) 0.6766(3) 0.0560(9) Uani 1 1 d U . . F15 F 0.8072(3) 0.0972(3) 0.74988(18) 0.0350(7) Uani 1 1 d . . . F16 F 0.5821(4) 0.1360(5) 0.5778(2) 0.0658(10) Uani 1 1 d U . . 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 Os1 0.01221(8) 0.01127(8) 0.01149(8) 0.00398(5) 0.00135(6) 0.00258(5) Cl1 0.0206(5) 0.0188(5) 0.0162(5) 0.0075(4) 0.0041(4) 0.0013(4) N1 0.0134(17) 0.0219(17) 0.0128(17) 0.0073(14) 0.0021(14) 0.0042(13) C2 0.018(2) 0.021(2) 0.017(2) 0.0079(17) 0.0054(17) 0.0091(16) C3 0.029(2) 0.022(2) 0.017(2) 0.0081(17) 0.0078(19) 0.0144(18) Br3 0.0246(2) 0.0225(2) 0.0294(2) 0.00986(18) 0.00609(19) 0.01165(17) C4 0.023(2) 0.030(2) 0.014(2) 0.0109(18) 0.0062(18) 0.0073(18) C5 0.018(2) 0.023(2) 0.014(2) 0.0051(17) 0.0032(17) 0.0032(17) C6 0.017(2) 0.021(2) 0.015(2) 0.0071(16) 0.0065(17) 0.0023(16) N7 0.0151(17) 0.0216(18) 0.0111(17) 0.0052(14) 0.0001(14) -0.0024(14) N8 0.0204(18) 0.0117(15) 0.0123(16) 0.0036(13) 0.0033(14) 0.0000(13) C9 0.026(2) 0.017(2) 0.013(2) 0.0045(16) 0.0034(18) 0.0067(17) C10 0.034(3) 0.016(2) 0.029(2) 0.0062(18) 0.013(2) 0.0063(18) C11 0.040(3) 0.017(2) 0.035(3) 0.0047(19) 0.011(2) 0.0019(19) C12 0.024(2) 0.0132(19) 0.0104(19) -0.0067(15) 0.0041(17) 0.0046(16) C13 0.026(2) 0.026(2) 0.022(2) 0.0052(18) 0.0033(19) 0.0111(18) C14 0.022(2) 0.019(2) 0.017(2) 0.0036(17) -0.0026(18) 0.0047(17) C15 0.014(2) 0.020(2) 0.015(2) 0.0028(17) -0.0048(17) -0.0006(16) C16 0.015(2) 0.025(2) 0.018(2) 0.0046(17) -0.0007(18) 0.0056(17) C17 0.025(2) 0.023(2) 0.013(2) 0.0045(17) -0.0043(18) 0.0103(17) C18 0.023(2) 0.019(2) 0.0099(19) 0.0073(16) -0.0065(17) 0.0016(16) C19 0.019(2) 0.019(2) 0.0074(18) 0.0051(15) -0.0018(16) 0.0022(16) C20 0.020(2) 0.0143(19) 0.0091(19) 0.0028(15) -0.0029(16) -0.0003(15) C21 0.0134(19) 0.0146(19) 0.017(2) 0.0012(16) -0.0046(17) -0.0004(15) C22 0.020(2) 0.018(2) 0.021(2) 0.0023(17) -0.0004(18) 0.0021(16) C23 0.022(2) 0.023(2) 0.021(2) -0.0024(18) -0.0028(19) 0.0057(17) C24 0.042(3) 0.017(2) 0.035(3) -0.001(2) -0.003(2) 0.010(2) C25 0.061(4) 0.024(3) 0.057(4) 0.020(2) 0.023(3) 0.011(2) C26 0.042(3) 0.019(2) 0.036(3) 0.011(2) 0.015(2) 0.002(2) P10 0.0186(6) 0.0246(6) 0.0233(6) 0.0144(5) 0.0089(5) 0.0099(4) F11 0.0334(15) 0.0337(14) 0.0209(13) 0.0103(11) 0.0104(11) 0.0171(12) F12 0.0522(19) 0.059(2) 0.0523(19) 0.0353(16) 0.0396(16) 0.0398(16) F13 0.0446(19) 0.0389(17) 0.0477(19) 0.0096(14) 0.0078(16) -0.0140(14) F14 0.067(2) 0.0253(14) 0.085(2) 0.0187(15) 0.0447(18) 0.0127(14) F15 0.0292(15) 0.0577(18) 0.0168(14) 0.0034(13) -0.0017(12) 0.0150(13) F16 0.0433(18) 0.136(3) 0.0514(19) 0.061(2) 0.0190(15) 0.0483(19) _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 Os1 N8 2.039(3) . ? Os1 N1 2.055(3) . ? Os1 C19 2.181(4) . ? Os1 C18 2.204(4) . ? Os1 C16 2.215(4) . ? Os1 C17 2.215(4) . ? Os1 C15 2.242(4) . ? Os1 C20 2.278(4) . ? Os1 Cl1 2.3896(9) . ? N1 C6 1.348(5) . ? N1 C2 1.362(5) . ? C2 C3 1.366(6) . ? C2 H2A 0.9500 . ? C3 C4 1.389(6) . ? C3 Br3 1.886(4) . ? C4 C5 1.382(6) . ? C4 H4A 0.9500 . ? C5 C6 1.393(6) . ? C5 H5A 0.9500 . ? C6 N7 1.372(5) . ? N7 N8 1.283(5) . ? N8 C9 1.436(5) . ? C9 C14 1.367(6) . ? C9 C10 1.399(6) . ? C10 C11 1.374(6) . ? C10 H10A 0.9500 . ? C11 C12 1.431(6) . ? C11 H11A 0.9500 . ? C12 C13 1.402(6) . ? C12 H12A 0.9500 . ? C13 C14 1.390(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.400(6) . ? C15 C16 1.425(6) . ? C15 H15A 1.0000 . ? C16 C17 1.393(6) . ? C16 H16A 1.0000 . ? C17 C18 1.424(6) . ? C17 H17A 1.0000 . ? C18 C19 1.417(6) . ? C18 H18A 1.0000 . ? C19 C20 1.433(5) . ? C19 H19A 1.0000 . ? C20 C21 1.487(5) . ? C21 C22 1.377(6) . ? C21 C26 1.395(6) . ? C22 C23 1.395(6) . ? C22 H22A 0.9500 . ? C23 C24 1.367(6) . ? C23 H23A 0.9500 . ? C24 C25 1.405(7) . ? C24 H24A 0.9500 . ? C25 C26 1.382(7) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? P10 F16 1.582(3) . ? P10 F14 1.589(3) . ? P10 F12 1.594(3) . ? P10 F15 1.594(3) . ? P10 F13 1.597(3) . ? P10 F11 1.598(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 N8 Os1 N1 74.32(13) . . ? N8 Os1 C19 122.50(13) . . ? N1 Os1 C19 93.31(14) . . ? N8 Os1 C18 96.66(13) . . ? N1 Os1 C18 114.20(14) . . ? C19 Os1 C18 37.69(14) . . ? N8 Os1 C16 119.71(14) . . ? N1 Os1 C16 165.96(14) . . ? C19 Os1 C16 79.58(15) . . ? C18 Os1 C16 66.91(15) . . ? N8 Os1 C17 95.66(14) . . ? N1 Os1 C17 149.97(14) . . ? C19 Os1 C17 67.88(15) . . ? C18 Os1 C17 37.60(15) . . ? C16 Os1 C17 36.66(15) . . ? N8 Os1 C15 156.54(15) . . ? N1 Os1 C15 128.72(14) . . ? C19 Os1 C15 66.42(15) . . ? C18 Os1 C15 78.56(14) . . ? C16 Os1 C15 37.27(15) . . ? C17 Os1 C15 66.45(15) . . ? N8 Os1 C20 159.76(13) . . ? N1 Os1 C20 100.46(14) . . ? C19 Os1 C20 37.42(13) . . ? C18 Os1 C20 67.20(14) . . ? C16 Os1 C20 66.58(15) . . ? C17 Os1 C20 79.07(15) . . ? C15 Os1 C20 36.07(15) . . ? N8 Os1 Cl1 88.86(9) . . ? N1 Os1 Cl1 84.69(9) . . ? C19 Os1 Cl1 146.85(10) . . ? C18 Os1 Cl1 161.09(11) . . ? C16 Os1 Cl1 94.64(11) . . ? C17 Os1 Cl1 123.99(11) . . ? C15 Os1 Cl1 89.18(11) . . ? C20 Os1 Cl1 110.38(10) . . ? C6 N1 C2 118.5(3) . . ? C6 N1 Os1 115.1(3) . . ? C2 N1 Os1 126.4(3) . . ? N1 C2 C3 121.2(4) . . ? N1 C2 H2A 119.4 . . ? C3 C2 H2A 119.4 . . ? C2 C3 C4 120.9(4) . . ? C2 C3 Br3 118.2(3) . . ? C4 C3 Br3 120.9(3) . . ? C5 C4 C3 118.0(4) . . ? C5 C4 H4A 121.0 . . ? C3 C4 H4A 121.0 . . ? C4 C5 C6 119.2(4) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? N1 C6 N7 117.2(4) . . ? N1 C6 C5 122.2(4) . . ? N7 C6 C5 120.7(4) . . ? N8 N7 C6 112.2(3) . . ? N7 N8 C9 113.5(3) . . ? N7 N8 Os1 121.2(3) . . ? C9 N8 Os1 125.3(3) . . ? C14 C9 C10 120.7(4) . . ? C14 C9 N8 120.0(3) . . ? C10 C9 N8 119.3(4) . . ? C11 C10 C9 118.8(4) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? C10 C11 C12 123.2(4) . . ? C10 C11 H11A 118.4 . . ? C12 C11 H11A 118.4 . . ? C13 C12 C11 114.6(4) . . ? C13 C12 H12A 122.7 . . ? C11 C12 H12A 122.7 . . ? C14 C13 C12 123.0(4) . . ? C14 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? C9 C14 C13 119.7(4) . . ? C9 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C20 C15 C16 121.7(4) . . ? C20 C15 Os1 73.4(2) . . ? C16 C15 Os1 70.3(2) . . ? C20 C15 H15A 118.5 . . ? C16 C15 H15A 118.5 . . ? Os1 C15 H15A 118.5 . . ? C17 C16 C15 120.2(4) . . ? C17 C16 Os1 71.7(2) . . ? C15 C16 Os1 72.4(2) . . ? C17 C16 H16A 119.5 . . ? C15 C16 H16A 119.5 . . ? Os1 C16 H16A 119.5 . . ? C16 C17 C18 119.7(4) . . ? C16 C17 Os1 71.7(2) . . ? C18 C17 Os1 70.8(2) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? Os1 C17 H17A 119.6 . . ? C19 C18 C17 119.5(4) . . ? C19 C18 Os1 70.2(2) . . ? C17 C18 Os1 71.6(2) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? Os1 C18 H18A 119.6 . . ? C18 C19 C20 121.1(4) . . ? C18 C19 Os1 72.1(2) . . ? C20 C19 Os1 75.0(2) . . ? C18 C19 H19A 119.3 . . ? C20 C19 H19A 119.3 . . ? Os1 C19 H19A 119.3 . . ? C15 C20 C19 117.5(4) . . ? C15 C20 C21 122.2(3) . . ? C19 C20 C21 120.2(4) . . ? C15 C20 Os1 70.6(2) . . ? C19 C20 Os1 67.6(2) . . ? C21 C20 Os1 130.7(3) . . ? C22 C21 C26 118.8(4) . . ? C22 C21 C20 120.4(4) . . ? C26 C21 C20 120.8(4) . . ? C21 C22 C23 120.9(4) . . ? C21 C22 H22A 119.5 . . ? C23 C22 H22A 119.5 . . ? C24 C23 C22 120.5(4) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C23 C24 C25 119.0(4) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? C26 C25 C24 120.4(5) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C25 C26 C21 120.3(5) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? F16 P10 F14 90.3(2) . . ? F16 P10 F12 89.37(17) . . ? F14 P10 F12 90.94(17) . . ? F16 P10 F15 178.92(18) . . ? F14 P10 F15 90.54(18) . . ? F12 P10 F15 89.90(16) . . ? F16 P10 F13 91.2(2) . . ? F14 P10 F13 178.4(2) . . ? F12 P10 F13 89.67(17) . . ? F15 P10 F13 88.03(17) . . ? F16 P10 F11 90.71(16) . . ? F14 P10 F11 89.59(16) . . ? F12 P10 F11 179.46(16) . . ? F15 P10 F11 90.01(14) . . ? F13 P10 F11 89.79(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4A Cl1 0.95 2.82 3.707(5) 155.2 1_455 C5 H5A Cl1 0.95 2.74 3.664(4) 163.9 2_655 C19 H19A F13 1.00 2.38 3.100(5) 128.6 2_656 C17 H17A F15 1.00 2.55 3.175(5) 120.0 2_756 C16 H16A F15 1.00 2.55 3.175(5) 120.1 2_756 _diffrn_measured_fraction_theta_max 0.829 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.113 _refine_diff_density_min -1.144 _refine_diff_density_rms 0.140 # Attachment '- fy23_complex10.cif' data_fy23 _database_code_depnum_ccdc_archive 'CCDC 821524' #TrackingRef '- fy23_complex10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H18 Cl F7 N3 Os P' _chemical_formula_weight 726.02 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' 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' Os Os -1.2165 7.6030 '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 7.4624(2) _cell_length_b 10.8856(4) _cell_length_c 14.5449(5) _cell_angle_alpha 81.182(3) _cell_angle_beta 84.223(2) _cell_angle_gamma 82.970(3) _cell_volume 1154.74(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7310 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 29.36 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 5.782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 9633 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 29.43 _reflns_number_total 5349 _reflns_number_gt 4863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0314P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5349 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.003 _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 Os1 Os 0.805561(16) 0.712932(12) 0.841013(8) 0.00897(5) Uani 1 1 d . . . Cl1 Cl 1.09066(10) 0.68746(8) 0.90454(6) 0.01570(17) Uani 1 1 d . . . N1 N 0.7969(4) 0.8892(3) 0.8762(2) 0.0106(6) Uani 1 1 d . . . C2 C 0.7380(4) 0.9241(3) 0.9600(2) 0.0134(7) Uani 1 1 d . . . H2A H 0.6803 0.8679 1.0069 0.016 Uiso 1 1 calc R . . F3 F 0.6958(3) 1.0720(2) 1.06212(15) 0.0239(5) Uani 1 1 d . . . C3 C 0.7618(5) 1.0414(3) 0.9773(2) 0.0166(7) Uani 1 1 d . . . C4 C 0.8483(5) 1.1261(3) 0.9135(3) 0.0184(8) Uani 1 1 d . . . H4A H 0.8656 1.2058 0.9279 0.022 Uiso 1 1 calc R . . C5 C 0.9091(5) 1.0900(3) 0.8277(3) 0.0180(7) Uani 1 1 d . . . H5A H 0.9696 1.1449 0.7810 0.022 Uiso 1 1 calc R . . C6 C 0.8802(5) 0.9728(3) 0.8111(2) 0.0137(7) Uani 1 1 d . . . N7 N 0.9409(4) 0.9320(3) 0.7263(2) 0.0145(6) Uani 1 1 d . . . N8 N 0.9167(4) 0.8168(3) 0.72702(19) 0.0117(6) Uani 1 1 d . . . C9 C 0.9671(4) 0.7746(3) 0.6376(2) 0.0118(7) Uani 1 1 d . . . C10 C 0.9176(5) 0.8510(3) 0.5573(2) 0.0150(7) Uani 1 1 d . . . H10A H 0.8582 0.9328 0.5605 0.018 Uiso 1 1 calc R . . C11 C 0.9556(5) 0.8072(4) 0.4722(2) 0.0191(8) Uani 1 1 d . . . H11A H 0.9193 0.8578 0.4166 0.023 Uiso 1 1 calc R . . C12 C 1.0473(5) 0.6885(4) 0.4688(3) 0.0198(8) Uani 1 1 d . . . H12A H 1.0737 0.6580 0.4106 0.024 Uiso 1 1 calc R . . C13 C 1.0999(5) 0.6152(4) 0.5493(3) 0.0182(8) Uani 1 1 d . . . H13A H 1.1642 0.5349 0.5458 0.022 Uiso 1 1 calc R . . C14 C 1.0612(4) 0.6559(3) 0.6351(2) 0.0140(7) Uani 1 1 d . . . H14A H 1.0974 0.6050 0.6906 0.017 Uiso 1 1 calc R . . P10 P 0.64862(13) 0.69703(10) 1.21615(7) 0.0194(2) Uani 1 1 d . . . F11 F 0.8231(3) 0.7155(2) 1.14250(17) 0.0315(6) Uani 1 1 d . . . F12 F 0.4743(3) 0.6786(3) 1.28781(16) 0.0407(7) Uani 1 1 d . . . F13 F 0.5223(4) 0.7578(4) 1.13731(18) 0.0747(13) Uani 1 1 d . . . F14 F 0.7807(5) 0.6317(4) 1.2930(2) 0.0746(12) Uani 1 1 d . . . F15 F 0.6626(5) 0.8259(3) 1.2485(3) 0.0710(11) Uani 1 1 d . . . F16 F 0.6445(5) 0.5638(3) 1.1845(3) 0.0749(12) Uani 1 1 d . . . C15 C 0.7428(4) 0.5496(3) 0.7787(2) 0.0122(7) Uani 1 1 d . . . H15A H 0.8210 0.5247 0.7232 0.015 Uiso 1 1 calc R . . C16 C 0.8011(4) 0.5077(3) 0.8675(2) 0.0132(7) Uani 1 1 d . . . H16A H 0.9176 0.4522 0.8740 0.016 Uiso 1 1 calc R . . C17 C 0.7105(5) 0.5576(3) 0.9474(2) 0.0162(7) Uani 1 1 d . . . H17A H 0.7651 0.5375 1.0087 0.019 Uiso 1 1 calc R . . C18 C 0.5672(4) 0.6519(3) 0.9355(2) 0.0140(7) Uani 1 1 d . . . H18A H 0.5207 0.6989 0.9885 0.017 Uiso 1 1 calc R . . C19 C 0.5141(4) 0.6994(3) 0.8439(2) 0.0139(7) Uani 1 1 d . . . H19A H 0.4296 0.7782 0.8350 0.017 Uiso 1 1 calc R . . C20 C 0.5974(4) 0.6493(3) 0.7643(2) 0.0121(7) Uani 1 1 d . . . C21 C 0.5445(4) 0.7011(3) 0.6693(2) 0.0137(7) Uani 1 1 d . . . C22 C 0.4601(5) 0.8234(4) 0.6515(3) 0.0180(8) Uani 1 1 d . . . H22A H 0.4355 0.8732 0.7005 0.022 Uiso 1 1 calc R . . C23 C 0.4124(5) 0.8718(4) 0.5624(3) 0.0224(8) Uani 1 1 d . . . H23A H 0.3539 0.9545 0.5505 0.027 Uiso 1 1 calc R . . C24 C 0.4497(5) 0.8002(4) 0.4905(3) 0.0234(9) Uani 1 1 d . . . H24A H 0.4184 0.8343 0.4294 0.028 Uiso 1 1 calc R . . C25 C 0.5317(5) 0.6802(4) 0.5074(3) 0.0210(8) Uani 1 1 d . . . H25A H 0.5569 0.6312 0.4580 0.025 Uiso 1 1 calc R . . C26 C 0.5783(5) 0.6300(4) 0.5971(2) 0.0167(7) Uani 1 1 d . . . H26A H 0.6335 0.5464 0.6087 0.020 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.00880(7) 0.00854(8) 0.00967(7) -0.00017(5) -0.00072(5) -0.00280(5) Cl1 0.0108(4) 0.0157(4) 0.0209(4) -0.0002(3) -0.0048(3) -0.0026(3) N1 0.0088(13) 0.0091(14) 0.0146(14) -0.0022(12) 0.0000(11) -0.0032(10) C2 0.0104(15) 0.0155(19) 0.0144(16) -0.0025(14) -0.0008(14) -0.0006(13) F3 0.0281(12) 0.0222(12) 0.0238(11) -0.0141(10) 0.0064(10) -0.0053(9) C3 0.0141(16) 0.020(2) 0.0182(18) -0.0089(16) -0.0018(15) -0.0020(14) C4 0.0177(17) 0.0132(19) 0.0252(19) -0.0027(16) -0.0032(16) -0.0039(14) C5 0.0229(18) 0.0117(18) 0.0196(18) -0.0009(15) -0.0004(16) -0.0061(14) C6 0.0154(16) 0.0120(18) 0.0148(16) -0.0016(14) -0.0037(14) -0.0045(13) N7 0.0186(15) 0.0129(16) 0.0123(14) -0.0006(12) -0.0005(12) -0.0052(12) N8 0.0130(13) 0.0110(15) 0.0114(13) 0.0004(12) -0.0014(12) -0.0044(11) C9 0.0114(15) 0.0139(18) 0.0114(15) -0.0030(14) 0.0005(13) -0.0067(13) C10 0.0151(16) 0.0136(18) 0.0167(17) -0.0009(15) -0.0017(14) -0.0040(13) C11 0.0193(18) 0.026(2) 0.0118(17) 0.0010(16) -0.0023(15) -0.0067(15) C12 0.0220(18) 0.025(2) 0.0142(17) -0.0074(16) 0.0037(15) -0.0073(15) C13 0.0163(17) 0.021(2) 0.0197(18) -0.0078(16) 0.0026(15) -0.0070(15) C14 0.0113(15) 0.0163(18) 0.0151(16) 0.0000(14) -0.0021(14) -0.0056(13) P10 0.0244(5) 0.0206(5) 0.0139(4) 0.0004(4) -0.0026(4) -0.0081(4) F11 0.0208(11) 0.0325(14) 0.0385(14) -0.0004(12) 0.0057(11) -0.0049(10) F12 0.0423(15) 0.0609(19) 0.0197(12) -0.0031(12) 0.0082(11) -0.0212(13) F13 0.0260(14) 0.163(4) 0.0198(14) 0.0146(18) -0.0025(12) 0.0165(19) F14 0.062(2) 0.114(3) 0.0348(17) 0.0127(18) -0.0153(16) 0.025(2) F15 0.070(2) 0.045(2) 0.107(3) -0.048(2) 0.032(2) -0.0251(16) F16 0.087(3) 0.052(2) 0.095(3) -0.042(2) 0.043(2) -0.0468(18) C15 0.0117(15) 0.0070(16) 0.0183(17) -0.0020(14) 0.0009(14) -0.0045(12) C16 0.0126(16) 0.0084(17) 0.0181(17) 0.0018(14) -0.0016(14) -0.0039(13) C17 0.0187(17) 0.0151(19) 0.0157(17) 0.0022(15) -0.0018(15) -0.0106(14) C18 0.0143(16) 0.0171(19) 0.0118(16) -0.0018(14) 0.0016(14) -0.0089(14) C19 0.0113(15) 0.0146(18) 0.0157(17) -0.0002(14) 0.0005(14) -0.0046(13) C20 0.0101(15) 0.0133(18) 0.0143(16) -0.0012(14) -0.0031(14) -0.0061(13) C21 0.0102(15) 0.0168(19) 0.0151(16) -0.0002(14) -0.0031(14) -0.0069(13) C22 0.0170(17) 0.018(2) 0.0189(18) -0.0010(15) -0.0009(15) -0.0036(14) C23 0.0196(18) 0.020(2) 0.025(2) 0.0074(17) -0.0071(16) -0.0029(15) C24 0.0203(18) 0.035(2) 0.0164(18) 0.0044(17) -0.0083(16) -0.0133(17) C25 0.0200(18) 0.031(2) 0.0151(17) -0.0044(17) -0.0017(15) -0.0125(16) C26 0.0161(17) 0.0167(19) 0.0175(17) -0.0004(15) -0.0024(15) -0.0048(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 Os1 N8 2.023(3) . ? Os1 N1 2.053(3) . ? Os1 C19 2.194(3) . ? Os1 C16 2.212(3) . ? Os1 C15 2.233(3) . ? Os1 C20 2.233(3) . ? Os1 C18 2.239(3) . ? Os1 C17 2.242(4) . ? Os1 Cl1 2.3727(8) . ? N1 C2 1.347(4) . ? N1 C6 1.366(4) . ? C2 C3 1.374(5) . ? C2 H2A 0.9500 . ? F3 C3 1.356(4) . ? C3 C4 1.374(5) . ? C4 C5 1.382(5) . ? C4 H4A 0.9500 . ? C5 C6 1.380(5) . ? C5 H5A 0.9500 . ? C6 N7 1.389(4) . ? N7 N8 1.287(4) . ? N8 C9 1.445(4) . ? C9 C10 1.380(5) . ? C9 C14 1.397(5) . ? C10 C11 1.385(5) . ? C10 H10A 0.9500 . ? C11 C12 1.392(5) . ? C11 H11A 0.9500 . ? C12 C13 1.375(5) . ? C12 H12A 0.9500 . ? C13 C14 1.379(5) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? P10 F15 1.564(3) . ? P10 F13 1.572(3) . ? P10 F14 1.592(3) . ? P10 F16 1.592(3) . ? P10 F12 1.596(3) . ? P10 F11 1.612(2) . ? C15 C16 1.396(5) . ? C15 C20 1.444(4) . ? C15 H15A 1.0000 . ? C16 C17 1.431(5) . ? C16 H16A 1.0000 . ? C17 C18 1.394(5) . ? C17 H17A 1.0000 . ? C18 C19 1.430(5) . ? C18 H18A 1.0000 . ? C19 C20 1.411(5) . ? C19 H19A 1.0000 . ? C20 C21 1.483(5) . ? C21 C26 1.383(5) . ? C21 C22 1.399(5) . ? C22 C23 1.387(5) . ? C22 H22A 0.9500 . ? C23 C24 1.384(5) . ? C23 H23A 0.9500 . ? C24 C25 1.370(6) . ? C24 H24A 0.9500 . ? C25 C26 1.396(5) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? 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 N8 Os1 N1 74.52(11) . . ? N8 Os1 C19 115.97(12) . . ? N1 Os1 C19 99.48(12) . . ? N8 Os1 C16 127.96(12) . . ? N1 Os1 C16 155.90(12) . . ? C19 Os1 C16 79.24(13) . . ? N8 Os1 C15 100.78(12) . . ? N1 Os1 C15 162.29(12) . . ? C19 Os1 C15 66.79(12) . . ? C16 Os1 C15 36.61(12) . . ? N8 Os1 C20 94.53(12) . . ? N1 Os1 C20 124.78(12) . . ? C19 Os1 C20 37.15(12) . . ? C16 Os1 C20 67.60(13) . . ? C15 Os1 C20 37.74(12) . . ? N8 Os1 C18 152.01(12) . . ? N1 Os1 C18 97.73(12) . . ? C19 Os1 C18 37.62(12) . . ? C16 Os1 C18 66.43(13) . . ? C15 Os1 C18 78.33(12) . . ? C20 Os1 C18 67.41(12) . . ? N8 Os1 C17 165.42(12) . . ? N1 Os1 C17 119.76(12) . . ? C19 Os1 C17 66.89(13) . . ? C16 Os1 C17 37.47(13) . . ? C15 Os1 C17 66.54(13) . . ? C20 Os1 C17 79.76(13) . . ? C18 Os1 C17 36.24(13) . . ? N8 Os1 Cl1 88.36(8) . . ? N1 Os1 Cl1 82.24(8) . . ? C19 Os1 Cl1 155.30(9) . . ? C16 Os1 Cl1 89.23(9) . . ? C15 Os1 Cl1 115.00(9) . . ? C20 Os1 Cl1 152.62(9) . . ? C18 Os1 Cl1 117.68(9) . . ? C17 Os1 Cl1 90.71(9) . . ? C2 N1 C6 118.2(3) . . ? C2 N1 Os1 126.2(2) . . ? C6 N1 Os1 115.1(2) . . ? N1 C2 C3 119.7(3) . . ? N1 C2 H2A 120.2 . . ? C3 C2 H2A 120.2 . . ? F3 C3 C2 116.9(3) . . ? F3 C3 C4 120.0(3) . . ? C2 C3 C4 123.2(3) . . ? C3 C4 C5 117.1(3) . . ? C3 C4 H4A 121.5 . . ? C5 C4 H4A 121.5 . . ? C6 C5 C4 118.8(3) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? N1 C6 C5 123.2(3) . . ? N1 C6 N7 116.1(3) . . ? C5 C6 N7 120.8(3) . . ? N8 N7 C6 111.7(3) . . ? N7 N8 C9 112.8(3) . . ? N7 N8 Os1 122.1(2) . . ? C9 N8 Os1 124.9(2) . . ? C10 C9 C14 121.8(3) . . ? C10 C9 N8 119.3(3) . . ? C14 C9 N8 118.8(3) . . ? C9 C10 C11 119.3(3) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C10 C11 C12 119.5(3) . . ? C10 C11 H11A 120.3 . . ? C12 C11 H11A 120.3 . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C14 121.3(3) . . ? C12 C13 H13A 119.4 . . ? C14 C13 H13A 119.4 . . ? C13 C14 C9 117.8(3) . . ? C13 C14 H14A 121.1 . . ? C9 C14 H14A 121.1 . . ? F15 P10 F13 92.8(2) . . ? F15 P10 F14 89.1(2) . . ? F13 P10 F14 177.57(19) . . ? F15 P10 F16 177.1(2) . . ? F13 P10 F16 89.6(2) . . ? F14 P10 F16 88.5(2) . . ? F15 P10 F12 89.85(16) . . ? F13 P10 F12 89.81(15) . . ? F14 P10 F12 91.73(17) . . ? F16 P10 F12 91.76(16) . . ? F15 P10 F11 90.58(16) . . ? F13 P10 F11 89.45(14) . . ? F14 P10 F11 88.99(16) . . ? F16 P10 F11 87.84(15) . . ? F12 P10 F11 179.16(14) . . ? C16 C15 C20 121.1(3) . . ? C16 C15 Os1 70.9(2) . . ? C20 C15 Os1 71.16(18) . . ? C16 C15 H15A 118.7 . . ? C20 C15 H15A 118.7 . . ? Os1 C15 H15A 118.7 . . ? C15 C16 C17 120.5(3) . . ? C15 C16 Os1 72.5(2) . . ? C17 C16 Os1 72.4(2) . . ? C15 C16 H16A 119.4 . . ? C17 C16 H16A 119.4 . . ? Os1 C16 H16A 119.4 . . ? C18 C17 C16 119.4(3) . . ? C18 C17 Os1 71.7(2) . . ? C16 C17 Os1 70.1(2) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? Os1 C17 H17A 119.8 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 Os1 72.0(2) . . ? C19 C18 Os1 69.48(19) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? Os1 C18 H18A 119.3 . . ? C20 C19 C18 121.8(3) . . ? C20 C19 Os1 72.95(18) . . ? C18 C19 Os1 72.89(19) . . ? C20 C19 H19A 118.8 . . ? C18 C19 H19A 118.8 . . ? Os1 C19 H19A 118.8 . . ? C19 C20 C15 117.2(3) . . ? C19 C20 C21 121.4(3) . . ? C15 C20 C21 121.4(3) . . ? C19 C20 Os1 69.90(19) . . ? C15 C20 Os1 71.11(18) . . ? C21 C20 Os1 127.2(2) . . ? C26 C21 C22 119.1(3) . . ? C26 C21 C20 120.8(3) . . ? C22 C21 C20 120.2(3) . . ? C23 C22 C21 119.9(3) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C22 120.3(4) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C25 C24 C23 120.1(4) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C21 C26 C25 120.5(3) . . ? C21 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2A F13 0.95 2.37 3.311(5) 170.2 . C19 H19A Cl1 1.00 2.86 3.207(3) 101.0 1_455 C19 H19A F3 1.00 2.42 3.189(4) 133.0 2_677 _diffrn_measured_fraction_theta_max 0.837 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.152 _refine_diff_density_min -1.411 _refine_diff_density_rms 0.143 # Attachment '- fy24_complex7.cif' data_fy24 _database_code_depnum_ccdc_archive 'CCDC 821525' #TrackingRef '- fy24_complex7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H18 Cl2 F6 N3 Os P' _chemical_formula_weight 742.47 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' 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' Os Os -1.2165 7.6030 '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 7.6240(5) _cell_length_b 28.9718(19) _cell_length_c 11.0421(14) _cell_angle_alpha 90.00 _cell_angle_beta 94.240(8) _cell_angle_gamma 90.00 _cell_volume 2432.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4676 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 29.27 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 5.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 12096 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 29.33 _reflns_number_total 5739 _reflns_number_gt 3906 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.1259P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5739 _refine_ls_number_parameters 325 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1996 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Os1 Os 0.26685(5) 0.568489(11) 0.79867(3) 0.03267(17) Uani 1 1 d . . . Cl1 Cl 0.5563(3) 0.53697(10) 0.8263(3) 0.0511(6) Uani 1 1 d . . . N1 N 0.3326(13) 0.5775(3) 0.6166(8) 0.045(2) Uani 1 1 d . . . Cl2 Cl 0.2276(4) 0.49533(9) 0.5398(3) 0.0545(7) Uani 1 1 d . . . C2 C 0.3232(13) 0.5481(3) 0.5232(9) 0.041(2) Uani 1 1 d . . . C3 C 0.3887(16) 0.5583(5) 0.4103(11) 0.055(3) Uani 1 1 d . . . H3A H 0.3759 0.5372 0.3467 0.066 Uiso 1 1 calc R . . C4 C 0.4706(18) 0.5991(5) 0.3959(12) 0.066(3) Uani 1 1 d . . . H4A H 0.5195 0.6061 0.3234 0.080 Uiso 1 1 calc R . . C5 C 0.4800(17) 0.6294(4) 0.4881(10) 0.056(3) Uani 1 1 d . . . H5A H 0.5327 0.6580 0.4780 0.067 Uiso 1 1 calc R . . C6 C 0.4114(12) 0.6188(4) 0.6000(9) 0.039(2) Uani 1 1 d . . . N7 N 0.4258(12) 0.6497(3) 0.6942(8) 0.046(2) Uani 1 1 d . . . N8 N 0.3704(10) 0.6320(2) 0.7900(7) 0.0363(17) Uani 1 1 d . . . C9 C 0.3800(12) 0.6646(3) 0.8896(9) 0.040(2) Uani 1 1 d . . . C10 C 0.3035(15) 0.7081(3) 0.8718(11) 0.053(3) Uani 1 1 d . . . H10A H 0.2464 0.7160 0.7973 0.063 Uiso 1 1 calc R . . C11 C 0.3142(18) 0.7392(4) 0.9667(14) 0.069(4) Uani 1 1 d . . . H11A H 0.2630 0.7682 0.9566 0.083 Uiso 1 1 calc R . . C12 C 0.3992(19) 0.7276(5) 1.0744(14) 0.072(4) Uani 1 1 d . . . H12A H 0.4067 0.7493 1.1367 0.086 Uiso 1 1 calc R . . C13 C 0.4760(17) 0.6843(4) 1.0957(11) 0.058(3) Uani 1 1 d . . . H13A H 0.5337 0.6769 1.1704 0.070 Uiso 1 1 calc R . . C14 C 0.4628(15) 0.6526(4) 1.0007(10) 0.051(3) Uani 1 1 d . . . H14A H 0.5100 0.6232 1.0121 0.061 Uiso 1 1 calc R . . C15 C -0.0104(13) 0.5547(3) 0.7530(10) 0.040(2) Uani 1 1 d . . . H15A H -0.0595 0.5580 0.6689 0.048 Uiso 1 1 calc R . . C16 C 0.0640(14) 0.5117(3) 0.7940(11) 0.050(3) Uani 1 1 d . . . H16A H 0.0721 0.4867 0.7351 0.061 Uiso 1 1 calc R . . C17 C 0.1652(14) 0.5089(4) 0.9049(10) 0.049(3) Uani 1 1 d U . . H17A H 0.2404 0.4819 0.9219 0.059 Uiso 1 1 calc R . . C18 C 0.1851(15) 0.5476(4) 0.9801(11) 0.052(3) Uani 1 1 d U . . H18A H 0.2713 0.5473 1.0505 0.063 Uiso 1 1 calc R . . C19 C 0.0962(11) 0.5900(3) 0.9438(8) 0.0330(19) Uani 1 1 d U . . H19A H 0.1247 0.6184 0.9897 0.040 Uiso 1 1 calc R . . C20 C -0.0030(13) 0.5931(3) 0.8307(9) 0.041(2) Uani 1 1 d U . . C21 C -0.0746(13) 0.6396(3) 0.7896(9) 0.042(2) Uani 1 1 d . . . C22 C -0.1408(13) 0.6700(4) 0.8720(11) 0.051(3) Uani 1 1 d . . . H22A H -0.1514 0.6614 0.9523 0.061 Uiso 1 1 calc R . . C23 C -0.1913(17) 0.7142(4) 0.8302(14) 0.067(4) Uani 1 1 d . . . H23A H -0.2348 0.7349 0.8849 0.080 Uiso 1 1 calc R . . C24 C -0.1792(17) 0.7280(5) 0.7133(15) 0.071(4) Uani 1 1 d . . . H24A H -0.2133 0.7576 0.6890 0.085 Uiso 1 1 calc R . . C25 C -0.1158(18) 0.6974(4) 0.6317(13) 0.068(3) Uani 1 1 d . . . H25A H -0.1069 0.7067 0.5518 0.082 Uiso 1 1 calc R . . C26 C -0.0647(14) 0.6528(4) 0.6665(10) 0.049(3) Uani 1 1 d . . . H26A H -0.0248 0.6322 0.6102 0.059 Uiso 1 1 calc R . . P10 P 0.0409(4) 0.37055(9) 0.7186(3) 0.0488(7) Uani 1 1 d . . . F11 F -0.1084(11) 0.4015(3) 0.7700(7) 0.081(2) Uani 1 1 d . . . F12 F 0.1930(10) 0.3394(2) 0.6678(7) 0.072(2) Uani 1 1 d . . . F13 F -0.1014(11) 0.3432(3) 0.6368(8) 0.085(2) Uani 1 1 d . . . F14 F 0.1871(12) 0.3993(3) 0.8001(8) 0.092(3) Uani 1 1 d . . . F15 F 0.0576(14) 0.4062(3) 0.6119(8) 0.098(3) Uani 1 1 d . . . F16 F 0.0240(15) 0.3359(3) 0.8276(8) 0.101(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 Os1 0.0353(2) 0.0263(2) 0.0362(3) -0.00046(14) 0.00128(16) 0.00032(13) Cl1 0.0449(14) 0.0542(15) 0.0533(16) 0.0048(13) -0.0026(12) 0.0126(12) N1 0.057(6) 0.038(4) 0.038(5) 0.004(4) -0.008(4) 0.008(4) Cl2 0.0604(16) 0.0474(14) 0.0551(16) -0.0193(13) 0.0000(13) -0.0028(13) C2 0.042(5) 0.041(5) 0.039(6) 0.002(5) -0.008(4) 0.004(4) C3 0.050(6) 0.073(8) 0.041(6) -0.008(6) 0.000(5) 0.011(6) C4 0.064(8) 0.091(10) 0.044(7) -0.003(7) 0.011(6) 0.007(8) C5 0.074(8) 0.051(6) 0.044(6) 0.011(6) 0.015(6) -0.001(6) C6 0.029(4) 0.050(6) 0.040(5) 0.007(5) 0.009(4) -0.006(4) N7 0.053(5) 0.036(4) 0.049(5) -0.002(4) 0.008(4) -0.005(4) N8 0.044(4) 0.030(4) 0.034(4) 0.003(3) -0.004(3) -0.011(3) C9 0.037(5) 0.040(5) 0.041(5) -0.006(4) 0.003(4) -0.007(4) C10 0.059(7) 0.038(5) 0.060(7) 0.000(5) -0.005(6) -0.009(5) C11 0.071(8) 0.044(6) 0.090(10) -0.030(7) -0.006(7) -0.002(6) C12 0.084(10) 0.057(7) 0.076(10) -0.023(7) 0.019(8) -0.002(7) C13 0.076(8) 0.048(6) 0.049(7) -0.017(5) -0.005(6) -0.013(6) C14 0.059(7) 0.044(6) 0.049(6) 0.001(5) 0.004(5) -0.008(5) C15 0.042(5) 0.032(4) 0.046(6) -0.005(5) 0.003(4) -0.022(4) C16 0.049(6) 0.032(5) 0.074(8) 0.000(5) 0.029(6) -0.013(5) C17 0.051(3) 0.046(3) 0.051(3) 0.005(3) 0.008(3) 0.002(3) C18 0.053(4) 0.051(4) 0.052(4) 0.006(3) 0.003(3) -0.003(3) C19 0.032(3) 0.036(3) 0.032(3) -0.004(2) 0.014(2) 0.001(2) C20 0.042(3) 0.039(3) 0.041(3) 0.000(3) 0.002(2) -0.004(3) C21 0.036(5) 0.043(5) 0.047(6) -0.003(5) -0.006(4) -0.001(4) C22 0.038(5) 0.055(6) 0.061(7) -0.011(6) 0.009(5) 0.000(5) C23 0.064(7) 0.054(7) 0.082(10) -0.035(7) 0.007(7) 0.009(6) C24 0.062(8) 0.060(8) 0.088(11) -0.003(8) -0.019(7) 0.008(6) C25 0.073(8) 0.061(8) 0.069(8) 0.008(7) -0.007(7) 0.004(7) C26 0.042(5) 0.053(6) 0.051(6) -0.005(5) -0.001(5) 0.004(5) P10 0.0608(18) 0.0393(14) 0.0457(16) -0.0006(13) 0.0002(13) 0.0014(13) F11 0.087(5) 0.092(6) 0.065(5) -0.019(4) 0.003(4) 0.024(5) F12 0.070(4) 0.060(4) 0.090(5) -0.017(4) 0.019(4) 0.010(4) F13 0.072(5) 0.085(5) 0.095(6) -0.027(5) -0.011(4) -0.006(4) F14 0.086(5) 0.078(5) 0.107(7) -0.038(5) -0.023(5) 0.007(5) F15 0.161(9) 0.057(4) 0.079(6) 0.027(4) 0.023(6) 0.015(5) F16 0.161(9) 0.074(5) 0.074(6) 0.023(5) 0.045(6) 0.019(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 Os1 N8 2.007(7) . ? Os1 N1 2.124(9) . ? Os1 C15 2.173(10) . ? Os1 C18 2.225(12) . ? Os1 C19 2.227(9) . ? Os1 C20 2.230(10) . ? Os1 C16 2.255(10) . ? Os1 C17 2.257(11) . ? Os1 Cl1 2.387(3) . ? N1 C2 1.336(14) . ? N1 C6 1.357(13) . ? Cl2 C2 1.709(11) . ? C2 C3 1.408(16) . ? C3 C4 1.353(19) . ? C3 H3A 0.9300 . ? C4 C5 1.342(17) . ? C4 H4A 0.9300 . ? C5 C6 1.411(14) . ? C5 H5A 0.9300 . ? C6 N7 1.371(13) . ? N7 N8 1.276(11) . ? N8 C9 1.447(12) . ? C9 C14 1.382(14) . ? C9 C10 1.398(14) . ? C10 C11 1.379(16) . ? C10 H10A 0.9300 . ? C11 C12 1.355(19) . ? C11 H11A 0.9300 . ? C12 C13 1.397(18) . ? C12 H12A 0.9300 . ? C13 C14 1.392(15) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C20 1.402(14) . ? C15 C16 1.429(15) . ? C15 H15A 0.9800 . ? C16 C17 1.400(16) . ? C16 H16A 0.9800 . ? C17 C18 1.398(16) . ? C17 H17A 0.9800 . ? C18 C19 1.446(15) . ? C18 H18A 0.9800 . ? C19 C20 1.414(13) . ? C19 H19A 0.9800 . ? C20 C21 1.511(14) . ? C21 C22 1.388(14) . ? C21 C26 1.420(15) . ? C22 C23 1.405(17) . ? C22 H22A 0.9300 . ? C23 C24 1.36(2) . ? C23 H23A 0.9300 . ? C24 C25 1.38(2) . ? C24 H24A 0.9300 . ? C25 C26 1.396(16) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? P10 F13 1.573(8) . ? P10 F15 1.580(8) . ? P10 F16 1.580(8) . ? P10 F11 1.587(8) . ? P10 F12 1.603(7) . ? P10 F14 1.612(8) . ? 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 N8 Os1 N1 73.8(3) . . ? N8 Os1 C15 122.4(3) . . ? N1 Os1 C15 95.5(4) . . ? N8 Os1 C18 115.4(4) . . ? N1 Os1 C18 170.8(4) . . ? C15 Os1 C18 80.0(4) . . ? N8 Os1 C19 91.7(3) . . ? N1 Os1 C19 146.9(3) . . ? C15 Os1 C19 67.0(4) . . ? C18 Os1 C19 37.9(4) . . ? N8 Os1 C20 94.9(3) . . ? N1 Os1 C20 113.3(3) . . ? C15 Os1 C20 37.1(4) . . ? C18 Os1 C20 67.7(4) . . ? C19 Os1 C20 37.0(3) . . ? N8 Os1 C16 159.8(4) . . ? N1 Os1 C16 106.1(4) . . ? C15 Os1 C16 37.6(4) . . ? C18 Os1 C16 65.5(4) . . ? C19 Os1 C16 77.6(4) . . ? C20 Os1 C16 66.3(4) . . ? N8 Os1 C17 151.3(4) . . ? N1 Os1 C17 134.5(4) . . ? C15 Os1 C17 67.3(4) . . ? C18 Os1 C17 36.3(4) . . ? C19 Os1 C17 66.4(4) . . ? C20 Os1 C17 78.8(4) . . ? C16 Os1 C17 36.2(4) . . ? N8 Os1 Cl1 89.6(2) . . ? N1 Os1 Cl1 83.5(3) . . ? C15 Os1 Cl1 146.5(3) . . ? C18 Os1 Cl1 95.7(3) . . ? C19 Os1 Cl1 126.8(2) . . ? C20 Os1 Cl1 163.1(3) . . ? C16 Os1 Cl1 110.5(3) . . ? C17 Os1 Cl1 89.5(3) . . ? C2 N1 C6 117.2(9) . . ? C2 N1 Os1 130.5(8) . . ? C6 N1 Os1 112.0(7) . . ? N1 C2 C3 123.2(10) . . ? N1 C2 Cl2 119.2(9) . . ? C3 C2 Cl2 117.6(9) . . ? C4 C3 C2 118.9(11) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C5 C4 C3 118.9(12) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? C4 C5 C6 121.2(12) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? N1 C6 N7 119.0(9) . . ? N1 C6 C5 120.4(10) . . ? N7 C6 C5 120.6(9) . . ? N8 N7 C6 110.7(8) . . ? N7 N8 C9 111.4(7) . . ? N7 N8 Os1 124.4(6) . . ? C9 N8 Os1 124.1(6) . . ? C14 C9 C10 120.7(9) . . ? C14 C9 N8 120.3(9) . . ? C10 C9 N8 119.0(9) . . ? C11 C10 C9 118.8(11) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? C12 C11 C10 120.1(12) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 122.6(12) . . ? C11 C12 H12A 118.7 . . ? C13 C12 H12A 118.7 . . ? C14 C13 C12 117.4(12) . . ? C14 C13 H13A 121.3 . . ? C12 C13 H13A 121.3 . . ? C9 C14 C13 120.3(10) . . ? C9 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C20 C15 C16 120.0(10) . . ? C20 C15 Os1 73.7(5) . . ? C16 C15 Os1 74.3(6) . . ? C20 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? Os1 C15 H15A 120.0 . . ? C17 C16 C15 120.6(10) . . ? C17 C16 Os1 72.0(6) . . ? C15 C16 Os1 68.1(5) . . ? C17 C16 H16A 118.6 . . ? C15 C16 H16A 118.6 . . ? Os1 C16 H16A 118.6 . . ? C18 C17 C16 120.0(10) . . ? C18 C17 Os1 70.6(6) . . ? C16 C17 Os1 71.8(6) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? Os1 C17 H17A 119.4 . . ? C17 C18 C19 119.4(10) . . ? C17 C18 Os1 73.1(7) . . ? C19 C18 Os1 71.1(6) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? Os1 C18 H18A 120.0 . . ? C20 C19 C18 120.4(9) . . ? C20 C19 Os1 71.6(5) . . ? C18 C19 Os1 71.0(6) . . ? C20 C19 H19A 119.2 . . ? C18 C19 H19A 119.2 . . ? Os1 C19 H19A 119.2 . . ? C15 C20 C19 119.1(9) . . ? C15 C20 C21 121.7(9) . . ? C19 C20 C21 118.6(8) . . ? C15 C20 Os1 69.2(6) . . ? C19 C20 Os1 71.4(5) . . ? C21 C20 Os1 123.7(7) . . ? C22 C21 C26 120.3(10) . . ? C22 C21 C20 120.6(10) . . ? C26 C21 C20 119.0(9) . . ? C21 C22 C23 117.8(11) . . ? C21 C22 H22A 121.1 . . ? C23 C22 H22A 121.1 . . ? C24 C23 C22 122.9(12) . . ? C24 C23 H23A 118.5 . . ? C22 C23 H23A 118.5 . . ? C23 C24 C25 118.9(13) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? C24 C25 C26 121.3(13) . . ? C24 C25 H25A 119.4 . . ? C26 C25 H25A 119.4 . . ? C25 C26 C21 118.7(11) . . ? C25 C26 H26A 120.6 . . ? C21 C26 H26A 120.6 . . ? F13 P10 F15 89.6(5) . . ? F13 P10 F16 91.5(6) . . ? F15 P10 F16 178.6(5) . . ? F13 P10 F11 90.5(5) . . ? F15 P10 F11 89.8(5) . . ? F16 P10 F11 89.2(5) . . ? F13 P10 F12 90.1(4) . . ? F15 P10 F12 90.4(5) . . ? F16 P10 F12 90.6(5) . . ? F11 P10 F12 179.4(5) . . ? F13 P10 F14 178.8(6) . . ? F15 P10 F14 89.3(6) . . ? F16 P10 F14 89.7(6) . . ? F11 P10 F14 89.6(5) . . ? F12 P10 F14 89.9(5) . . ? _diffrn_measured_fraction_theta_max 0.860 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.453 _refine_diff_density_min -4.967 _refine_diff_density_rms 0.279 # Attachment '- fy6_complex24.cif' data_fy6 _database_code_depnum_ccdc_archive 'CCDC 821526' #TrackingRef '- fy6_complex24.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H27 Cl F6 I N3 O1.50 Os P' _chemical_formula_weight 854.99 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.4975(4) _cell_length_b 14.2729(3) _cell_length_c 20.3022(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5649.82(18) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11341 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 32.69 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3256 _exptl_absorpt_coefficient_mu 5.820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 27877 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 32.76 _reflns_number_total 9445 _reflns_number_gt 6059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0343P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9445 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.140228(8) 0.909894(11) 0.268847(7) 0.01320(4) Uani 1 1 d . . . N1 N 0.12106(18) 0.8641(2) 0.17478(14) 0.0158(7) Uani 1 1 d . . . I1 I 0.060909(14) 0.761431(18) 0.300460(12) 0.01789(6) Uani 1 1 d . . . C2 C 0.0670(2) 0.8862(3) 0.13791(18) 0.0197(9) Uani 1 1 d . . . H2A H 0.0341 0.9291 0.1545 0.024 Uiso 1 1 calc R . . C3 C 0.0576(2) 0.8476(3) 0.07533(19) 0.0246(10) Uani 1 1 d . . . H3A H 0.0190 0.8644 0.0494 0.030 Uiso 1 1 calc R . . Cl4 Cl 0.09419(7) 0.73894(8) -0.02572(5) 0.0309(3) Uani 1 1 d . . . C4 C 0.1049(2) 0.7853(3) 0.05218(18) 0.0214(10) Uani 1 1 d . . . C5 C 0.1611(2) 0.7604(3) 0.08948(18) 0.0192(9) Uani 1 1 d . . . H5A H 0.1942 0.7169 0.0738 0.023 Uiso 1 1 calc R . . C6 C 0.1670(2) 0.8018(3) 0.15087(17) 0.0144(8) Uani 1 1 d . . . N7 N 0.22049(18) 0.7776(2) 0.19196(14) 0.0172(7) Uani 1 1 d . . . N8 N 0.21567(18) 0.8187(2) 0.24803(14) 0.0138(7) Uani 1 1 d . . . C9 C 0.2703(2) 0.7953(3) 0.29310(19) 0.0162(8) Uani 1 1 d . . . C10 C 0.2551(2) 0.7765(3) 0.35827(18) 0.0185(9) Uani 1 1 d . . . H10A H 0.2089 0.7784 0.3731 0.022 Uiso 1 1 calc R . . C11 C 0.3068(2) 0.7549(3) 0.40144(19) 0.0225(9) Uani 1 1 d . . . H11A H 0.2963 0.7408 0.4460 0.027 Uiso 1 1 calc R . . C12 C 0.3737(2) 0.7538(3) 0.3803(2) 0.0246(10) Uani 1 1 d . . . H12A H 0.4095 0.7397 0.4104 0.029 Uiso 1 1 calc R . . C13 C 0.3888(2) 0.7732(3) 0.3149(2) 0.0255(10) Uani 1 1 d . . . H13A H 0.4352 0.7731 0.3006 0.031 Uiso 1 1 calc R . . C14 C 0.3372(2) 0.7926(3) 0.27037(18) 0.0162(8) Uani 1 1 d . . . H14A H 0.3474 0.8038 0.2253 0.019 Uiso 1 1 calc R . . C15 C 0.1294(2) 0.9779(3) 0.36709(18) 0.0184(9) Uani 1 1 d . . . H15A H 0.1219 0.9376 0.4067 0.022 Uiso 1 1 calc R . . C16 C 0.1958(2) 0.9925(3) 0.34498(19) 0.0172(8) Uani 1 1 d . . . H16A H 0.2346 0.9623 0.3693 0.021 Uiso 1 1 calc R . . C17 C 0.2090(2) 1.0346(3) 0.2828(2) 0.0206(9) Uani 1 1 d . . . C18 C 0.1517(2) 1.0579(3) 0.2428(2) 0.0214(9) Uani 1 1 d . . . H18A H 0.1590 1.0760 0.1957 0.026 Uiso 1 1 calc R . . C19 C 0.0830(2) 1.0464(3) 0.2673(2) 0.0213(9) Uani 1 1 d . . . H19A H 0.0436 1.0541 0.2364 0.026 Uiso 1 1 calc R . . C20 C 0.0715(2) 1.0067(3) 0.32938(19) 0.0187(9) Uani 1 1 d . . . C21 C 0.0001(2) 0.9930(3) 0.3579(2) 0.0227(9) Uani 1 1 d . . . H21A H -0.0003 0.9317 0.3819 0.027 Uiso 1 1 calc R . . C22 C -0.0120(2) 1.0710(3) 0.4087(2) 0.0335(12) Uani 1 1 d . . . H22A H 0.0230 1.0673 0.4432 0.050 Uiso 1 1 calc R . . H22B H -0.0576 1.0634 0.4284 0.050 Uiso 1 1 calc R . . H22C H -0.0093 1.1321 0.3868 0.050 Uiso 1 1 calc R . . C23 C -0.0567(2) 0.9906(3) 0.3066(2) 0.0292(10) Uani 1 1 d . . . H23A H -0.0439 0.9477 0.2710 0.044 Uiso 1 1 calc R . . H23B H -0.0636 1.0536 0.2886 0.044 Uiso 1 1 calc R . . H23C H -0.0994 0.9688 0.3272 0.044 Uiso 1 1 calc R . . C24 C 0.2809(2) 1.0467(3) 0.2584(2) 0.0260(10) Uani 1 1 d . . . H24A H 0.3086 0.9929 0.2720 0.039 Uiso 1 1 calc R . . H24B H 0.3004 1.1042 0.2771 0.039 Uiso 1 1 calc R . . H24C H 0.2806 1.0511 0.2103 0.039 Uiso 1 1 calc R . . P10 P 0.27195(13) 0.98256(15) 0.04515(7) 0.0244(5) Uani 0.801(6) 1 d P A 1 F11 F 0.3431(2) 0.9622(3) 0.00823(19) 0.0494(13) Uani 0.801(6) 1 d P A 1 F12 F 0.2014(2) 1.0001(3) 0.0829(2) 0.0470(12) Uani 0.801(6) 1 d P A 1 F13 F 0.3112(2) 1.0514(3) 0.09393(17) 0.0479(13) Uani 0.801(6) 1 d P A 1 F14 F 0.2339(4) 0.9130(5) -0.0042(3) 0.0477(16) Uani 0.801(6) 1 d P A 1 F15 F 0.2575(3) 1.0676(3) -0.0034(2) 0.0454(12) Uani 0.801(6) 1 d P A 1 F16 F 0.2877(2) 0.8975(3) 0.0938(2) 0.0438(12) Uani 0.801(6) 1 d P A 1 P10A P 0.2464(4) 1.0084(5) 0.0418(3) 0.0160(17) Uiso 0.199(6) 1 d P A 2 F11A F 0.2258(10) 1.0742(14) -0.0160(9) 0.041(5) Uiso 0.199(6) 1 d P A 2 F12A F 0.2708(11) 0.9385(14) 0.1005(9) 0.042(5) Uiso 0.199(6) 1 d P A 2 F13A F 0.3258(10) 1.0276(14) 0.0271(8) 0.052(5) Uiso 0.199(6) 1 d P A 2 F14A F 0.1713(9) 0.9813(11) 0.0559(7) 0.032(4) Uiso 0.199(6) 1 d P A 2 F15A F 0.2474(10) 1.0898(12) 0.0933(8) 0.053(5) Uiso 0.199(6) 1 d P A 2 F16A F 0.2547(17) 0.922(3) -0.006(2) 0.067(13) Uiso 0.199(6) 1 d P A 2 O25 O 0.4739(4) 1.0568(6) 0.3856(4) 0.0473(19) Uiso 0.50 1 d P B -1 C26 C 0.4224(9) 1.0327(11) 0.4035(7) 0.076(4) Uiso 0.50 1 d P B -1 O27 O 0.5989(9) 1.0467(13) 0.5212(8) 0.179(7) Uiso 0.50 1 d P C -1 O28 O 0.4257(5) 0.8661(7) 0.5501(4) 0.071(3) Uiso 0.50 1 d P D -1 C29 C 0.3968(5) 0.7816(7) 0.5743(5) 0.034(2) Uiso 0.50 1 d P D -1 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 Os1 0.01576(7) 0.01252(7) 0.01132(6) -0.00037(6) 0.00020(6) 0.00027(7) N1 0.0194(18) 0.0173(19) 0.0108(14) 0.0023(13) -0.0013(13) -0.0025(15) I1 0.02127(13) 0.01714(14) 0.01526(11) 0.00080(10) -0.00065(11) -0.00346(11) C2 0.021(2) 0.022(2) 0.0163(17) 0.0029(16) 0.0017(17) -0.0009(19) C3 0.025(2) 0.033(3) 0.0154(18) 0.0017(18) -0.0047(18) -0.002(2) Cl4 0.0425(7) 0.0371(7) 0.0131(4) -0.0048(4) -0.0026(5) -0.0035(6) C4 0.030(3) 0.024(2) 0.0111(16) -0.0015(16) 0.0006(17) -0.007(2) C5 0.030(2) 0.012(2) 0.0150(17) -0.0010(15) 0.0033(17) -0.0051(19) C6 0.020(2) 0.009(2) 0.0136(17) 0.0013(14) 0.0015(16) -0.0045(17) N7 0.0238(19) 0.0155(18) 0.0123(14) -0.0005(13) 0.0031(14) -0.0006(16) N8 0.0186(17) 0.0085(16) 0.0144(13) 0.0010(12) 0.0013(14) -0.0041(14) C9 0.019(2) 0.0093(19) 0.0203(18) -0.0010(15) -0.0016(17) 0.0006(17) C10 0.018(2) 0.022(2) 0.0155(17) 0.0007(16) 0.0018(16) 0.0013(19) C11 0.024(2) 0.024(3) 0.0189(19) -0.0003(17) 0.0004(18) 0.000(2) C12 0.021(2) 0.020(2) 0.033(2) 0.0005(19) -0.0076(19) -0.0020(19) C13 0.013(2) 0.025(3) 0.038(2) -0.003(2) 0.0031(19) 0.003(2) C14 0.0179(19) 0.016(2) 0.0150(16) -0.0015(16) 0.0024(17) -0.0009(17) C15 0.024(2) 0.018(2) 0.0136(16) -0.0033(15) 0.0013(16) 0.0004(19) C16 0.016(2) 0.010(2) 0.0249(19) -0.0077(16) 0.0021(17) 0.0019(17) C17 0.020(2) 0.010(2) 0.031(2) -0.0058(16) 0.0033(18) 0.0041(17) C18 0.030(3) 0.0115(19) 0.0223(19) 0.0015(16) 0.0033(18) -0.0001(19) C19 0.025(2) 0.013(2) 0.026(2) -0.0030(18) -0.0031(19) 0.0050(18) C20 0.024(2) 0.010(2) 0.0216(19) -0.0056(16) 0.0004(18) 0.0028(18) C21 0.018(2) 0.020(2) 0.030(2) -0.0024(18) 0.0032(19) -0.0006(19) C22 0.021(2) 0.035(3) 0.045(3) -0.016(2) 0.015(2) -0.002(2) C23 0.021(2) 0.025(3) 0.041(3) 0.000(2) -0.005(2) 0.000(2) C24 0.022(2) 0.017(2) 0.039(2) -0.0008(19) 0.008(2) -0.004(2) P10 0.0302(12) 0.0242(10) 0.0187(7) 0.0028(6) 0.0060(7) -0.0074(9) F11 0.040(2) 0.064(3) 0.044(2) 0.010(2) 0.0158(19) -0.002(2) F12 0.049(3) 0.051(3) 0.041(2) 0.000(2) 0.012(2) 0.005(2) F13 0.066(3) 0.039(2) 0.039(2) 0.0043(18) -0.008(2) -0.017(2) F14 0.052(4) 0.049(3) 0.042(3) -0.022(2) -0.002(3) -0.015(3) F15 0.053(3) 0.047(3) 0.036(2) 0.0159(18) -0.005(2) 0.004(2) F16 0.047(3) 0.037(3) 0.048(2) 0.018(2) 0.007(2) -0.007(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 Os1 N8 2.009(3) . ? Os1 N1 2.053(3) . ? Os1 C18 2.190(4) . ? Os1 C16 2.226(4) . ? Os1 C15 2.228(4) . ? Os1 C19 2.245(4) . ? Os1 C17 2.247(4) . ? Os1 C20 2.284(4) . ? Os1 I1 2.7007(3) . ? N1 C2 1.330(5) . ? N1 C6 1.352(5) . ? C2 C3 1.396(5) . ? C2 H2A 0.9500 . ? C3 C4 1.364(6) . ? C3 H3A 0.9500 . ? Cl4 C4 1.727(4) . ? C4 C5 1.378(6) . ? C5 C6 1.384(5) . ? C5 H5A 0.9500 . ? C6 N7 1.379(5) . ? N7 N8 1.284(4) . ? N8 C9 1.443(5) . ? C9 C10 1.382(5) . ? C9 C14 1.385(5) . ? C10 C11 1.370(6) . ? C10 H10A 0.9500 . ? C11 C12 1.374(6) . ? C11 H11A 0.9500 . ? C12 C13 1.388(6) . ? C12 H12A 0.9500 . ? C13 C14 1.380(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.387(6) . ? C15 C20 1.424(6) . ? C15 H15A 1.0000 . ? C16 C17 1.422(6) . ? C16 H16A 1.0000 . ? C17 C18 1.421(6) . ? C17 C24 1.495(6) . ? C18 C19 1.438(6) . ? C18 H18A 1.0000 . ? C19 C20 1.400(6) . ? C19 H19A 1.0000 . ? C20 C21 1.520(6) . ? C21 C23 1.522(6) . ? C21 C22 1.535(6) . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? P10 F15 1.589(4) . ? P10 F13 1.591(4) . ? P10 F12 1.594(5) . ? P10 F14 1.594(7) . ? P10 F16 1.595(4) . ? P10 F11 1.603(4) . ? P10A F14A 1.541(17) . ? P10A F11A 1.56(2) . ? P10A F15A 1.564(17) . ? P10A F16A 1.58(4) . ? P10A F13A 1.60(2) . ? P10A F12A 1.63(2) . ? O25 C26 1.121(17) . ? O28 C29 1.420(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 N8 Os1 N1 74.41(13) . . ? N8 Os1 C18 119.97(15) . . ? N1 Os1 C18 95.81(14) . . ? N8 Os1 C16 97.63(14) . . ? N1 Os1 C16 154.60(14) . . ? C18 Os1 C16 66.84(15) . . ? N8 Os1 C15 122.70(14) . . ? N1 Os1 C15 162.57(15) . . ? C18 Os1 C15 78.78(15) . . ? C16 Os1 C15 36.29(14) . . ? N8 Os1 C19 157.36(15) . . ? N1 Os1 C19 99.97(14) . . ? C18 Os1 C19 37.80(16) . . ? C16 Os1 C19 77.97(15) . . ? C15 Os1 C19 65.60(15) . . ? N8 Os1 C17 95.88(14) . . ? N1 Os1 C17 118.56(14) . . ? C18 Os1 C17 37.34(16) . . ? C16 Os1 C17 37.07(14) . . ? C15 Os1 C17 66.36(15) . . ? C19 Os1 C17 67.10(16) . . ? N8 Os1 C20 159.20(14) . . ? N1 Os1 C20 125.90(14) . . ? C18 Os1 C20 66.81(15) . . ? C16 Os1 C20 65.91(15) . . ? C15 Os1 C20 36.77(15) . . ? C19 Os1 C20 36.00(14) . . ? C17 Os1 C20 78.68(15) . . ? N8 Os1 I1 87.76(9) . . ? N1 Os1 I1 82.36(9) . . ? C18 Os1 I1 150.81(12) . . ? C16 Os1 I1 121.97(10) . . ? C15 Os1 I1 94.29(11) . . ? C19 Os1 I1 113.57(12) . . ? C17 Os1 I1 159.00(10) . . ? C20 Os1 I1 90.61(11) . . ? C2 N1 C6 118.6(3) . . ? C2 N1 Os1 126.3(3) . . ? C6 N1 Os1 115.0(2) . . ? N1 C2 C3 121.5(4) . . ? N1 C2 H2A 119.2 . . ? C3 C2 H2A 119.2 . . ? C4 C3 C2 118.8(4) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C3 C4 C5 121.1(4) . . ? C3 C4 Cl4 118.9(3) . . ? C5 C4 Cl4 120.0(3) . . ? C4 C5 C6 116.8(4) . . ? C4 C5 H5A 121.6 . . ? C6 C5 H5A 121.6 . . ? N1 C6 N7 116.7(3) . . ? N1 C6 C5 123.3(4) . . ? N7 C6 C5 120.0(4) . . ? N8 N7 C6 111.5(3) . . ? N7 N8 C9 113.7(3) . . ? N7 N8 Os1 122.4(3) . . ? C9 N8 Os1 123.8(2) . . ? C10 C9 C14 121.0(4) . . ? C10 C9 N8 119.6(4) . . ? C14 C9 N8 119.4(3) . . ? C11 C10 C9 119.9(4) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.1(4) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C13 119.9(4) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 120.7(4) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C9 118.3(4) . . ? C13 C14 H14A 120.8 . . ? C9 C14 H14A 120.8 . . ? C16 C15 C20 121.5(4) . . ? C16 C15 Os1 71.8(2) . . ? C20 C15 Os1 73.7(2) . . ? C16 C15 H15A 118.9 . . ? C20 C15 H15A 118.9 . . ? Os1 C15 H15A 118.9 . . ? C15 C16 C17 121.3(4) . . ? C15 C16 Os1 72.0(2) . . ? C17 C16 Os1 72.3(2) . . ? C15 C16 H16A 118.8 . . ? C17 C16 H16A 118.8 . . ? Os1 C16 H16A 118.8 . . ? C18 C17 C16 117.6(4) . . ? C18 C17 C24 121.4(4) . . ? C16 C17 C24 120.8(4) . . ? C18 C17 Os1 69.1(2) . . ? C16 C17 Os1 70.7(2) . . ? C24 C17 Os1 127.6(3) . . ? C17 C18 C19 120.5(4) . . ? C17 C18 Os1 73.5(2) . . ? C19 C18 Os1 73.2(2) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? Os1 C18 H18A 119.6 . . ? C20 C19 C18 120.5(4) . . ? C20 C19 Os1 73.5(2) . . ? C18 C19 Os1 69.0(2) . . ? C20 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? Os1 C19 H19A 119.1 . . ? C19 C20 C15 118.2(4) . . ? C19 C20 C21 122.9(4) . . ? C15 C20 C21 118.9(4) . . ? C19 C20 Os1 70.5(2) . . ? C15 C20 Os1 69.5(2) . . ? C21 C20 Os1 131.7(3) . . ? C20 C21 C23 114.1(4) . . ? C20 C21 C22 107.7(3) . . ? C23 C21 C22 111.3(4) . . ? C20 C21 H21A 107.8 . . ? C23 C21 H21A 107.8 . . ? C22 C21 H21A 107.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C17 C24 H24A 109.5 . . ? C17 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C17 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F15 P10 F13 90.0(2) . . ? F15 P10 F12 91.4(3) . . ? F13 P10 F12 91.1(3) . . ? F15 P10 F14 90.2(4) . . ? F13 P10 F14 179.0(4) . . ? F12 P10 F14 89.9(3) . . ? F15 P10 F16 179.1(3) . . ? F13 P10 F16 89.5(2) . . ? F12 P10 F16 89.3(2) . . ? F14 P10 F16 90.3(3) . . ? F15 P10 F11 90.1(2) . . ? F13 P10 F11 89.2(3) . . ? F12 P10 F11 178.4(3) . . ? F14 P10 F11 89.7(4) . . ? F16 P10 F11 89.1(2) . . ? F14A P10A F11A 92.7(10) . . ? F14A P10A F15A 94.2(10) . . ? F11A P10A F15A 93.4(10) . . ? F14A P10A F16A 90.9(14) . . ? F11A P10A F16A 92.2(17) . . ? F15A P10A F16A 172.3(17) . . ? F14A P10A F13A 175.4(10) . . ? F11A P10A F13A 90.3(10) . . ? F15A P10A F13A 89.2(10) . . ? F16A P10A F13A 85.5(14) . . ? F14A P10A F12A 89.3(10) . . ? F11A P10A F12A 177.6(11) . . ? F15A P10A F12A 87.8(10) . . ? F16A P10A F12A 86.5(17) . . ? F13A P10A F12A 87.7(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C5 H5A F13 0.95 2.40 3.034(6) 123.8 8_655 C5 H5A F15A 0.95 2.18 3.020(18) 147.0 8_655 C2 H2A O25 0.95 2.32 3.076(9) 136.5 6_556 C3 H3A O28 0.95 2.72 3.629(10) 160.9 6_556 C3 H3A O27 0.95 2.69 3.577(19) 156.3 2_574 C15 H15A Cl4 1.00 2.92 3.845(4) 154.4 7_576 C16 H16A F15 1.00 2.62 3.322(6) 126.9 2_575 C16 H16A F11A 1.00 2.51 3.347(19) 141.2 2_575 _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.734 _refine_diff_density_min -1.466 _refine_diff_density_rms 0.179 # Attachment '- fy7_complex20.cif' data_fy7 _database_code_depnum_ccdc_archive 'CCDC 821527' #TrackingRef '- fy7_complex20.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H22 Br Cl F6 N3 Os P' _chemical_formula_weight 766.95 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 '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 16.6936(5) _cell_length_b 9.0505(3) _cell_length_c 16.9583(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.970(3) _cell_angle_gamma 90.00 _cell_volume 2437.19(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15235 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 32.47 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 7.108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 34168 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 32.58 _reflns_number_total 8294 _reflns_number_gt 6277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0199P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8294 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0524 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _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 Os1 Os 0.259190(6) 0.958218(13) 0.009564(6) 0.01171(3) Uani 1 1 d . . . Cl1 Cl 0.27957(4) 1.08532(9) -0.10616(4) 0.01737(15) Uani 1 1 d . . . N1 N 0.36874(14) 1.0589(3) 0.07691(14) 0.0145(5) Uani 1 1 d . . . C2 C 0.37658(17) 1.1942(4) 0.11167(16) 0.0162(6) Uani 1 1 d . . . H2A H 0.3274 1.2505 0.1073 0.019 Uiso 1 1 calc R . . Br3 Br 0.457968(19) 1.44071(4) 0.202408(18) 0.02347(7) Uani 1 1 d . . . C3 C 0.45472(18) 1.2530(3) 0.15361(17) 0.0173(6) Uani 1 1 d . . . C4 C 0.52737(18) 1.1737(4) 0.16004(17) 0.0197(7) Uani 1 1 d . . . H4A H 0.5811 1.2129 0.1892 0.024 Uiso 1 1 calc R . . C5 C 0.51994(17) 1.0357(4) 0.12289(17) 0.0189(6) Uani 1 1 d . . . H5A H 0.5686 0.9791 0.1255 0.023 Uiso 1 1 calc R . . C6 C 0.44036(16) 0.9819(3) 0.08195(16) 0.0136(6) Uani 1 1 d . . . N7 N 0.43060(14) 0.8492(3) 0.03983(14) 0.0151(5) Uani 1 1 d . . . N8 N 0.35209(13) 0.8206(3) 0.00198(13) 0.0133(5) Uani 1 1 d . . . C9 C 0.33892(17) 0.6896(3) -0.04799(17) 0.0153(6) Uani 1 1 d . . . C10 C 0.39137(18) 0.5685(4) -0.02263(19) 0.0192(7) Uani 1 1 d . . . H10A H 0.4352 0.5701 0.0288 0.023 Uiso 1 1 calc R . . C11 C 0.3790(2) 0.4444(4) -0.0736(2) 0.0269(7) Uani 1 1 d . . . H11A H 0.4132 0.3591 -0.0564 0.032 Uiso 1 1 calc R . . C12 C 0.3158(2) 0.4465(4) -0.15021(19) 0.0273(8) Uani 1 1 d . . . H12A H 0.3086 0.3636 -0.1861 0.033 Uiso 1 1 calc R . . C13 C 0.2642(2) 0.5664(4) -0.17413(19) 0.0249(8) Uani 1 1 d . . . H13A H 0.2208 0.5651 -0.2259 0.030 Uiso 1 1 calc R . . C14 C 0.27463(18) 0.6895(4) -0.12375(17) 0.0196(7) Uani 1 1 d . . . H14A H 0.2387 0.7727 -0.1404 0.023 Uiso 1 1 calc R . . C15 C 0.17122(16) 1.0704(3) 0.06680(17) 0.0153(6) Uani 1 1 d . . . H15A H 0.1876 1.1683 0.0944 0.018 Uiso 1 1 calc R . . C16 C 0.20533(16) 0.9383(4) 0.11144(17) 0.0164(6) Uani 1 1 d . . . H16A H 0.2433 0.9467 0.1698 0.020 Uiso 1 1 calc R . . C17 C 0.19545(17) 0.7990(4) 0.07164(17) 0.0169(6) Uani 1 1 d . . . C18 C 0.15398(16) 0.7959(4) -0.01556(17) 0.0169(6) Uani 1 1 d . . . H18A H 0.1574 0.7038 -0.0470 0.020 Uiso 1 1 calc R . . C19 C 0.12486(16) 0.9254(3) -0.05997(18) 0.0153(6) Uani 1 1 d . . . H19A H 0.1074 0.9223 -0.1219 0.018 Uiso 1 1 calc R . . C20 C 0.13142(16) 1.0663(3) -0.01924(17) 0.0150(6) Uani 1 1 d . . . C21 C 0.09765(16) 1.2017(3) -0.07118(18) 0.0155(6) Uani 1 1 d . . . H21A H 0.1034 1.1849 -0.1275 0.019 Uiso 1 1 calc R . . C22 C 0.14292(18) 1.3447(4) -0.03749(19) 0.0211(7) Uani 1 1 d . . . H22A H 0.2030 1.3343 -0.0311 0.032 Uiso 1 1 calc R . . H22B H 0.1357 1.3667 0.0165 0.032 Uiso 1 1 calc R . . H22C H 0.1193 1.4255 -0.0761 0.032 Uiso 1 1 calc R . . C23 C 0.00329(17) 1.2117(4) -0.08071(18) 0.0201(7) Uani 1 1 d . . . H23A H -0.0219 1.2933 -0.1182 0.030 Uiso 1 1 calc R . . H23B H -0.0041 1.2294 -0.0264 0.030 Uiso 1 1 calc R . . H23C H -0.0244 1.1188 -0.1037 0.030 Uiso 1 1 calc R . . C24 C 0.22740(18) 0.6597(4) 0.11834(19) 0.0216(7) Uani 1 1 d . . . H24A H 0.2712 0.6838 0.1703 0.032 Uiso 1 1 calc R . . H24B H 0.2511 0.5954 0.0846 0.032 Uiso 1 1 calc R . . H24C H 0.1809 0.6087 0.1307 0.032 Uiso 1 1 calc R . . P10 P 0.44033(5) 1.84349(10) 0.30259(4) 0.01686(16) Uani 1 1 d . . . F11 F 0.46757(12) 1.9006(2) 0.39621(10) 0.0305(5) Uani 1 1 d . . . F12 F 0.41232(10) 1.7857(2) 0.20868(10) 0.0230(4) Uani 1 1 d . . . F13 F 0.42832(13) 2.0103(2) 0.26984(11) 0.0315(5) Uani 1 1 d . . . F14 F 0.45021(10) 1.6754(2) 0.33485(11) 0.0239(4) Uani 1 1 d . . . F15 F 0.53648(10) 1.8455(2) 0.30354(11) 0.0315(5) Uani 1 1 d . . . F16 F 0.34313(10) 1.8404(2) 0.30156(10) 0.0251(4) 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 Os1 0.00919(5) 0.01562(6) 0.01016(5) -0.00026(5) 0.00276(3) 0.00014(5) Cl1 0.0157(3) 0.0232(4) 0.0151(3) 0.0049(3) 0.0075(3) 0.0034(3) N1 0.0133(11) 0.0187(14) 0.0127(11) 0.0005(10) 0.0058(9) -0.0016(10) C2 0.0159(14) 0.0190(17) 0.0147(14) 0.0004(12) 0.0060(12) -0.0009(12) Br3 0.02575(16) 0.02228(18) 0.01908(14) -0.00476(13) 0.00206(12) -0.00575(13) C3 0.0215(15) 0.0190(17) 0.0124(13) -0.0022(12) 0.0065(12) -0.0053(13) C4 0.0139(14) 0.0296(19) 0.0141(14) -0.0004(13) 0.0023(12) -0.0081(13) C5 0.0111(12) 0.0304(19) 0.0147(13) 0.0016(14) 0.0032(11) 0.0002(13) C6 0.0129(13) 0.0193(17) 0.0089(12) 0.0007(11) 0.0041(10) 0.0006(11) N7 0.0127(11) 0.0207(14) 0.0131(11) 0.0009(10) 0.0056(9) 0.0008(10) N8 0.0127(11) 0.0190(14) 0.0093(11) 0.0004(10) 0.0048(9) 0.0022(10) C9 0.0169(14) 0.0180(16) 0.0135(13) -0.0001(12) 0.0083(12) -0.0010(12) C10 0.0164(14) 0.0203(18) 0.0209(15) 0.0003(13) 0.0058(12) 0.0007(12) C11 0.0284(17) 0.0209(19) 0.0346(18) 0.0006(15) 0.0143(15) 0.0040(14) C12 0.0406(19) 0.023(2) 0.0239(16) -0.0079(15) 0.0186(15) -0.0060(16) C13 0.0335(18) 0.028(2) 0.0143(14) -0.0051(13) 0.0093(13) -0.0048(15) C14 0.0227(15) 0.0220(18) 0.0145(14) -0.0001(13) 0.0065(12) 0.0021(13) C15 0.0092(12) 0.0216(18) 0.0162(13) -0.0030(12) 0.0056(11) -0.0030(11) C16 0.0096(12) 0.0292(19) 0.0112(12) 0.0018(12) 0.0044(10) -0.0044(12) C17 0.0093(13) 0.0252(18) 0.0168(14) 0.0022(13) 0.0049(11) -0.0061(12) C18 0.0105(13) 0.0220(17) 0.0184(14) -0.0028(13) 0.0047(12) 0.0009(12) C19 0.0091(12) 0.0204(17) 0.0149(13) 0.0003(12) 0.0015(11) -0.0025(11) C20 0.0089(12) 0.0215(18) 0.0155(13) 0.0012(12) 0.0051(11) 0.0016(11) C21 0.0112(13) 0.0188(16) 0.0167(14) 0.0003(12) 0.0047(11) 0.0005(11) C22 0.0162(14) 0.0193(17) 0.0268(16) 0.0021(14) 0.0054(13) 0.0007(13) C23 0.0156(14) 0.0218(18) 0.0232(15) 0.0018(13) 0.0062(13) 0.0030(12) C24 0.0205(15) 0.0191(18) 0.0237(16) 0.0046(13) 0.0050(13) -0.0050(13) P10 0.0182(4) 0.0183(4) 0.0129(3) 0.0018(3) 0.0031(3) -0.0020(3) F11 0.0424(11) 0.0341(12) 0.0124(8) -0.0023(8) 0.0045(8) -0.0108(10) F12 0.0260(9) 0.0275(11) 0.0147(8) -0.0034(8) 0.0050(7) -0.0044(8) F13 0.0544(13) 0.0185(11) 0.0219(9) 0.0050(8) 0.0123(9) -0.0031(9) F14 0.0243(9) 0.0203(11) 0.0275(9) 0.0078(8) 0.0086(8) 0.0046(8) F15 0.0175(9) 0.0498(15) 0.0253(10) 0.0067(10) 0.0040(8) -0.0087(9) F16 0.0189(9) 0.0331(12) 0.0226(9) 0.0048(8) 0.0056(7) 0.0064(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 Os1 N8 2.024(2) . ? Os1 N1 2.047(2) . ? Os1 C16 2.187(3) . ? Os1 C19 2.208(3) . ? Os1 C18 2.228(3) . ? Os1 C17 2.238(3) . ? Os1 C15 2.238(3) . ? Os1 C20 2.259(3) . ? Os1 Cl1 2.3880(7) . ? N1 C2 1.347(4) . ? N1 C6 1.364(3) . ? C2 C3 1.385(4) . ? C2 H2A 0.9500 . ? Br3 C3 1.883(3) . ? C3 C4 1.384(4) . ? C4 C5 1.387(4) . ? C4 H4A 0.9500 . ? C5 C6 1.384(4) . ? C5 H5A 0.9500 . ? C6 N7 1.381(4) . ? N7 N8 1.295(3) . ? N8 C9 1.435(4) . ? C9 C10 1.386(4) . ? C9 C14 1.397(4) . ? C10 C11 1.393(4) . ? C10 H10A 0.9500 . ? C11 C12 1.399(5) . ? C11 H11A 0.9500 . ? C12 C13 1.367(5) . ? C12 H12A 0.9500 . ? C13 C14 1.382(4) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.405(4) . ? C15 C16 1.436(4) . ? C15 H15A 1.0000 . ? C16 C17 1.415(4) . ? C16 H16A 1.0000 . ? C17 C18 1.427(4) . ? C17 C24 1.497(4) . ? C18 C19 1.397(4) . ? C18 H18A 1.0000 . ? C19 C20 1.438(4) . ? C19 H19A 1.0000 . ? C20 C21 1.513(4) . ? C21 C22 1.519(4) . ? C21 C23 1.536(4) . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? P10 F11 1.5964(18) . ? P10 F13 1.600(2) . ? P10 F15 1.6003(18) . ? P10 F12 1.6026(18) . ? P10 F14 1.608(2) . ? P10 F16 1.6177(18) . ? 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 N8 Os1 N1 74.88(10) . . ? N8 Os1 C16 120.61(10) . . ? N1 Os1 C16 96.33(9) . . ? N8 Os1 C19 123.72(10) . . ? N1 Os1 C19 160.58(11) . . ? C16 Os1 C19 79.25(10) . . ? N8 Os1 C18 99.00(11) . . ? N1 Os1 C18 156.37(10) . . ? C16 Os1 C18 66.72(10) . . ? C19 Os1 C18 36.71(11) . . ? N8 Os1 C17 96.82(11) . . ? N1 Os1 C17 119.79(10) . . ? C16 Os1 C17 37.28(11) . . ? C19 Os1 C17 67.21(10) . . ? C18 Os1 C17 37.26(10) . . ? N8 Os1 C15 157.66(10) . . ? N1 Os1 C15 98.56(10) . . ? C16 Os1 C15 37.84(11) . . ? C19 Os1 C15 66.33(10) . . ? C18 Os1 C15 78.35(11) . . ? C17 Os1 C15 67.50(11) . . ? N8 Os1 C20 160.69(10) . . ? N1 Os1 C20 123.32(10) . . ? C16 Os1 C20 67.40(10) . . ? C19 Os1 C20 37.55(11) . . ? C18 Os1 C20 66.92(11) . . ? C17 Os1 C20 79.99(11) . . ? C15 Os1 C20 36.40(10) . . ? N8 Os1 Cl1 86.44(7) . . ? N1 Os1 Cl1 85.11(7) . . ? C16 Os1 Cl1 152.42(8) . . ? C19 Os1 Cl1 90.27(8) . . ? C18 Os1 Cl1 117.67(7) . . ? C17 Os1 Cl1 154.93(7) . . ? C15 Os1 Cl1 114.63(8) . . ? C20 Os1 Cl1 88.75(7) . . ? C2 N1 C6 118.2(2) . . ? C2 N1 Os1 126.72(19) . . ? C6 N1 Os1 114.99(19) . . ? N1 C2 C3 121.5(3) . . ? N1 C2 H2A 119.2 . . ? C3 C2 H2A 119.2 . . ? C4 C3 C2 120.3(3) . . ? C4 C3 Br3 121.8(2) . . ? C2 C3 Br3 117.8(2) . . ? C3 C4 C5 118.5(3) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? C6 C5 C4 118.8(3) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? N1 C6 N7 116.8(2) . . ? N1 C6 C5 122.6(3) . . ? N7 C6 C5 120.5(3) . . ? N8 N7 C6 111.7(2) . . ? N7 N8 C9 113.9(2) . . ? N7 N8 Os1 121.6(2) . . ? C9 N8 Os1 124.44(17) . . ? C10 C9 C14 121.2(3) . . ? C10 C9 N8 120.2(2) . . ? C14 C9 N8 118.5(3) . . ? C9 C10 C11 119.1(3) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C10 C11 C12 119.3(3) . . ? C10 C11 H11A 120.3 . . ? C12 C11 H11A 120.3 . . ? C13 C12 C11 120.8(3) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C12 C13 C14 120.6(3) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C13 C14 C9 118.9(3) . . ? C13 C14 H14A 120.5 . . ? C9 C14 H14A 120.5 . . ? C20 C15 C16 120.6(3) . . ? C20 C15 Os1 72.59(16) . . ? C16 C15 Os1 69.16(15) . . ? C20 C15 H15A 118.9 . . ? C16 C15 H15A 118.9 . . ? Os1 C15 H15A 118.9 . . ? C17 C16 C15 121.4(3) . . ? C17 C16 Os1 73.29(16) . . ? C15 C16 Os1 73.00(16) . . ? C17 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? Os1 C16 H16A 119.0 . . ? C16 C17 C18 117.4(3) . . ? C16 C17 C24 121.9(3) . . ? C18 C17 C24 120.7(3) . . ? C16 C17 Os1 69.43(16) . . ? C18 C17 Os1 71.00(17) . . ? C24 C17 Os1 130.4(2) . . ? C19 C18 C17 121.3(3) . . ? C19 C18 Os1 70.88(17) . . ? C17 C18 Os1 71.74(16) . . ? C19 C18 H18A 118.7 . . ? C17 C18 H18A 118.7 . . ? Os1 C18 H18A 118.7 . . ? C18 C19 C20 121.5(3) . . ? C18 C19 Os1 72.42(16) . . ? C20 C19 Os1 73.14(15) . . ? C18 C19 H19A 118.9 . . ? C20 C19 H19A 118.9 . . ? Os1 C19 H19A 118.9 . . ? C15 C20 C19 117.6(3) . . ? C15 C20 C21 123.7(3) . . ? C19 C20 C21 118.6(2) . . ? C15 C20 Os1 71.01(16) . . ? C19 C20 Os1 69.32(15) . . ? C21 C20 Os1 129.35(19) . . ? C20 C21 C22 114.7(2) . . ? C20 C21 C23 107.2(2) . . ? C22 C21 C23 111.4(3) . . ? C20 C21 H21A 107.8 . . ? C22 C21 H21A 107.8 . . ? C23 C21 H21A 107.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C17 C24 H24A 109.5 . . ? C17 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C17 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F11 P10 F13 90.38(11) . . ? F11 P10 F15 90.53(10) . . ? F13 P10 F15 90.62(12) . . ? F11 P10 F12 179.56(11) . . ? F13 P10 F12 89.76(10) . . ? F15 P10 F12 89.88(10) . . ? F11 P10 F14 90.00(11) . . ? F13 P10 F14 178.75(11) . . ? F15 P10 F14 90.57(11) . . ? F12 P10 F14 89.85(10) . . ? F11 P10 F16 89.62(10) . . ? F13 P10 F16 89.70(11) . . ? F15 P10 F16 179.64(13) . . ? F12 P10 F16 89.97(9) . . ? F14 P10 F16 89.11(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C5 H5A Cl1 0.95 2.72 3.615(3) 157.9 3_675 C16 H16A F16 1.00 2.53 3.449(3) 152.7 1_545 C15 H15A F16 1.00 2.52 3.368(3) 142.2 2_545 _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.010 _refine_diff_density_min -1.610 _refine_diff_density_rms 0.168 # Attachment '- fy8_complex26.cif' data_fy8 _database_code_depnum_ccdc_archive 'CCDC 821528' #TrackingRef '- fy8_complex26.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H22 Cl2 F6 N3 Os P' _chemical_formula_weight 722.49 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' 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' Os Os -1.2165 7.6030 '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 7.2224(2) _cell_length_b 10.6661(4) _cell_length_c 15.8327(6) _cell_angle_alpha 79.383(3) _cell_angle_beta 78.400(3) _cell_angle_gamma 85.931(3) _cell_volume 1173.57(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18133 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 32.64 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.045 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 5.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 27520 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 32.70 _reflns_number_total 7987 _reflns_number_gt 7118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0208P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7987 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0450 _refine_ls_wR_factor_gt 0.0443 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.804764(11) 0.882307(8) 0.223826(5) 0.00877(3) Uani 1 1 d . . . Cl1 Cl 1.07366(7) 0.83462(5) 0.11762(3) 0.01535(10) Uani 1 1 d . . . N1 N 0.8826(2) 1.06917(18) 0.18037(11) 0.0107(3) Uani 1 1 d . . . C2 C 0.8399(3) 1.1496(2) 0.11068(14) 0.0136(4) Uani 1 1 d . . . H2A H 0.7701 1.1193 0.0741 0.016 Uiso 1 1 calc R . . C3 C 0.8939(3) 1.2751(2) 0.09012(14) 0.0151(4) Uani 1 1 d . . . H3A H 0.8603 1.3305 0.0408 0.018 Uiso 1 1 calc R . . Cl4 Cl 1.06371(8) 1.47555(5) 0.12134(4) 0.02018(12) Uani 1 1 d . . . C4 C 0.9980(3) 1.3184(2) 0.14293(15) 0.0144(4) Uani 1 1 d . . . C5 C 1.0520(3) 1.2361(2) 0.21276(14) 0.0142(4) Uani 1 1 d . . . H5A H 1.1277 1.2635 0.2481 0.017 Uiso 1 1 calc R . . C6 C 0.9913(3) 1.1121(2) 0.22916(14) 0.0111(4) Uani 1 1 d . . . N7 N 1.0436(3) 1.02490(18) 0.29756(12) 0.0128(4) Uani 1 1 d . . . N8 N 0.9781(2) 0.91391(17) 0.30152(11) 0.0102(3) Uani 1 1 d . . . C9 C 1.0320(3) 0.8191(2) 0.37041(14) 0.0110(4) Uani 1 1 d . . . C10 C 1.0073(3) 0.8476(2) 0.45418(14) 0.0147(4) Uani 1 1 d . . . H10A H 0.9541 0.9280 0.4662 0.018 Uiso 1 1 calc R . . C11 C 1.0619(3) 0.7562(2) 0.51997(15) 0.0181(5) Uani 1 1 d . . . H11A H 1.0427 0.7730 0.5780 0.022 Uiso 1 1 calc R . . C12 C 1.1436(3) 0.6417(2) 0.50162(16) 0.0202(5) Uani 1 1 d . . . H12A H 1.1842 0.5809 0.5467 0.024 Uiso 1 1 calc R . . C13 C 1.1676(3) 0.6138(2) 0.41740(16) 0.0196(5) Uani 1 1 d . . . H13A H 1.2243 0.5343 0.4053 0.024 Uiso 1 1 calc R . . C14 C 1.1085(3) 0.7023(2) 0.35111(15) 0.0150(4) Uani 1 1 d . . . H14A H 1.1203 0.6833 0.2939 0.018 Uiso 1 1 calc R . . C15 C 0.5285(3) 0.8919(2) 0.17796(14) 0.0108(4) Uani 1 1 d . . . H15A H 0.5094 0.9573 0.1261 0.013 Uiso 1 1 calc R . . C16 C 0.5052(3) 0.9304(2) 0.26194(14) 0.0126(4) Uani 1 1 d . . . H16A H 0.4645 1.0206 0.2676 0.015 Uiso 1 1 calc R . . C17 C 0.5583(3) 0.8470(2) 0.33446(14) 0.0135(4) Uani 1 1 d . . . C18 C 0.6498(3) 0.7278(2) 0.31979(15) 0.0143(4) Uani 1 1 d . . . H18A H 0.7145 0.6770 0.3659 0.017 Uiso 1 1 calc R . . C19 C 0.6834(3) 0.6932(2) 0.23584(15) 0.0140(4) Uani 1 1 d . . . H19A H 0.7702 0.6183 0.2244 0.017 Uiso 1 1 calc R . . C20 C 0.6171(3) 0.7737(2) 0.16393(14) 0.0119(4) Uani 1 1 d . . . C21 C 0.6552(3) 0.7306(2) 0.07617(15) 0.0145(4) Uani 1 1 d . . . H21A H 0.7898 0.6986 0.0646 0.017 Uiso 1 1 calc R . . C22 C 0.6280(3) 0.8362(2) 0.00032(15) 0.0185(5) Uani 1 1 d . . . H22A H 0.7149 0.9047 -0.0040 0.028 Uiso 1 1 calc R . . H22B H 0.4973 0.8704 0.0104 0.028 Uiso 1 1 calc R . . H22C H 0.6542 0.8017 -0.0543 0.028 Uiso 1 1 calc R . . C23 C 0.5290(4) 0.6186(2) 0.08167(17) 0.0241(5) Uani 1 1 d . . . H23A H 0.5508 0.5510 0.1301 0.036 Uiso 1 1 calc R . . H23B H 0.5598 0.5853 0.0266 0.036 Uiso 1 1 calc R . . H23C H 0.3960 0.6479 0.0918 0.036 Uiso 1 1 calc R . . C24 C 0.5285(3) 0.8867(2) 0.42277(15) 0.0188(5) Uani 1 1 d . . . H24A H 0.5305 0.9800 0.4152 0.028 Uiso 1 1 calc R . . H24B H 0.6297 0.8486 0.4533 0.028 Uiso 1 1 calc R . . H24C H 0.4060 0.8576 0.4573 0.028 Uiso 1 1 calc R . . P10 P 0.50279(9) 0.69852(6) 0.68003(4) 0.01772(12) Uani 1 1 d . . . F11 F 0.3390(2) 0.60066(15) 0.72494(12) 0.0375(4) Uani 1 1 d . . . F12 F 0.66460(19) 0.79853(15) 0.63642(10) 0.0268(3) Uani 1 1 d . . . F13 F 0.4839(2) 0.75061(15) 0.77072(10) 0.0297(4) Uani 1 1 d . . . F14 F 0.5242(2) 0.64677(16) 0.59010(10) 0.0298(4) Uani 1 1 d . . . F15 F 0.6590(2) 0.59439(16) 0.71020(10) 0.0295(4) Uani 1 1 d . . . F16 F 0.34706(19) 0.80395(14) 0.65090(10) 0.0257(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 Os1 0.00899(4) 0.00803(4) 0.00934(4) -0.00150(3) -0.00158(3) -0.00123(3) Cl1 0.0128(2) 0.0187(3) 0.0146(2) -0.0066(2) 0.00083(18) -0.0012(2) N1 0.0101(8) 0.0102(9) 0.0112(8) -0.0016(7) -0.0002(6) -0.0023(7) C2 0.0137(10) 0.0138(11) 0.0133(10) -0.0011(9) -0.0036(8) -0.0015(9) C3 0.0164(10) 0.0142(11) 0.0129(10) 0.0022(9) -0.0029(8) -0.0001(9) Cl4 0.0256(3) 0.0094(2) 0.0242(3) 0.0022(2) -0.0045(2) -0.0059(2) C4 0.0144(10) 0.0095(10) 0.0172(11) -0.0020(9) 0.0020(8) -0.0024(8) C5 0.0135(10) 0.0125(11) 0.0165(11) -0.0027(9) -0.0025(8) -0.0018(9) C6 0.0110(9) 0.0110(10) 0.0111(10) -0.0018(8) -0.0012(7) -0.0017(8) N7 0.0142(9) 0.0105(9) 0.0137(9) -0.0004(7) -0.0034(7) -0.0026(7) N8 0.0098(8) 0.0093(8) 0.0113(8) -0.0019(7) -0.0016(6) 0.0002(7) C9 0.0104(9) 0.0117(10) 0.0108(10) 0.0004(8) -0.0034(7) -0.0027(8) C10 0.0154(10) 0.0146(11) 0.0150(11) -0.0035(9) -0.0031(8) -0.0030(9) C11 0.0189(11) 0.0235(13) 0.0118(10) -0.0002(10) -0.0042(8) -0.0047(10) C12 0.0187(11) 0.0186(12) 0.0212(12) 0.0075(10) -0.0082(9) -0.0034(10) C13 0.0193(11) 0.0124(11) 0.0258(13) 0.0007(10) -0.0056(9) 0.0015(9) C14 0.0163(10) 0.0124(11) 0.0167(11) -0.0032(9) -0.0038(8) 0.0007(9) C15 0.0088(9) 0.0113(10) 0.0123(10) -0.0013(8) -0.0017(7) -0.0025(8) C16 0.0092(9) 0.0112(10) 0.0167(11) -0.0035(9) 0.0002(8) -0.0007(8) C17 0.0091(9) 0.0158(11) 0.0142(10) -0.0016(9) 0.0021(8) -0.0066(9) C18 0.0118(10) 0.0143(11) 0.0159(11) 0.0025(9) -0.0028(8) -0.0075(9) C19 0.0130(10) 0.0090(10) 0.0208(11) -0.0020(9) -0.0044(8) -0.0035(8) C20 0.0094(9) 0.0120(10) 0.0144(10) -0.0012(8) -0.0029(7) -0.0036(8) C21 0.0136(10) 0.0130(11) 0.0184(11) -0.0057(9) -0.0037(8) -0.0002(9) C22 0.0206(11) 0.0197(12) 0.0166(11) -0.0074(10) -0.0042(9) 0.0027(10) C23 0.0292(13) 0.0200(13) 0.0278(14) -0.0109(11) -0.0078(11) -0.0075(11) C24 0.0164(11) 0.0239(13) 0.0149(11) -0.0037(10) 0.0016(8) -0.0051(10) P10 0.0166(3) 0.0159(3) 0.0202(3) -0.0045(3) -0.0017(2) 0.0010(2) F11 0.0321(9) 0.0183(8) 0.0561(12) 0.0000(8) 0.0034(8) -0.0101(7) F12 0.0174(7) 0.0333(9) 0.0278(8) -0.0044(7) 0.0015(6) -0.0071(7) F13 0.0382(9) 0.0281(9) 0.0216(8) -0.0111(7) 0.0022(6) 0.0024(7) F14 0.0359(9) 0.0313(9) 0.0291(8) -0.0155(7) -0.0173(7) 0.0107(7) F15 0.0346(9) 0.0302(9) 0.0264(8) -0.0092(7) -0.0138(7) 0.0155(7) F16 0.0173(7) 0.0180(8) 0.0399(9) -0.0025(7) -0.0050(6) 0.0034(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 Os1 N8 2.0067(17) . ? Os1 N1 2.0638(18) . ? Os1 C16 2.177(2) . ? Os1 C19 2.217(2) . ? Os1 C18 2.221(2) . ? Os1 C17 2.231(2) . ? Os1 C15 2.246(2) . ? Os1 C20 2.286(2) . ? Os1 Cl1 2.3915(5) . ? N1 C2 1.341(3) . ? N1 C6 1.360(3) . ? C2 C3 1.382(3) . ? C2 H2A 0.9500 . ? C3 C4 1.387(3) . ? C3 H3A 0.9500 . ? Cl4 C4 1.729(2) . ? C4 C5 1.383(3) . ? C5 C6 1.385(3) . ? C5 H5A 0.9500 . ? C6 N7 1.387(3) . ? N7 N8 1.292(2) . ? N8 C9 1.439(3) . ? C9 C14 1.387(3) . ? C9 C10 1.389(3) . ? C10 C11 1.388(3) . ? C10 H10A 0.9500 . ? C11 C12 1.373(4) . ? C11 H11A 0.9500 . ? C12 C13 1.393(3) . ? C12 H12A 0.9500 . ? C13 C14 1.390(3) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.407(3) . ? C15 C16 1.438(3) . ? C15 H15A 1.0000 . ? C16 C17 1.418(3) . ? C16 H16A 1.0000 . ? C17 C18 1.426(3) . ? C17 C24 1.505(3) . ? C18 C19 1.415(3) . ? C18 H18A 1.0000 . ? C19 C20 1.437(3) . ? C19 H19A 1.0000 . ? C20 C21 1.510(3) . ? C21 C22 1.521(3) . ? C21 C23 1.533(3) . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? P10 F14 1.5953(16) . ? P10 F11 1.5996(16) . ? P10 F12 1.6005(15) . ? P10 F15 1.6054(16) . ? P10 F16 1.6064(16) . ? P10 F13 1.6103(16) . ? 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 N8 Os1 N1 74.68(7) . . ? N8 Os1 C16 117.68(8) . . ? N1 Os1 C16 94.72(8) . . ? N8 Os1 C19 122.00(8) . . ? N1 Os1 C19 163.16(8) . . ? C16 Os1 C19 79.76(8) . . ? N8 Os1 C18 95.60(7) . . ? N1 Os1 C18 153.14(8) . . ? C16 Os1 C18 67.25(8) . . ? C19 Os1 C18 37.18(8) . . ? N8 Os1 C17 93.25(7) . . ? N1 Os1 C17 116.97(8) . . ? C16 Os1 C17 37.49(8) . . ? C19 Os1 C17 67.52(8) . . ? C18 Os1 C17 37.35(8) . . ? N8 Os1 C15 155.28(8) . . ? N1 Os1 C15 99.71(7) . . ? C16 Os1 C15 37.89(8) . . ? C19 Os1 C15 66.21(8) . . ? C18 Os1 C15 78.55(8) . . ? C17 Os1 C15 67.44(8) . . ? N8 Os1 C20 159.12(8) . . ? N1 Os1 C20 126.07(7) . . ? C16 Os1 C20 67.25(8) . . ? C19 Os1 C20 37.17(8) . . ? C18 Os1 C20 66.81(8) . . ? C17 Os1 C20 79.54(8) . . ? C15 Os1 C20 36.16(8) . . ? N8 Os1 Cl1 89.63(5) . . ? N1 Os1 Cl1 84.45(5) . . ? C16 Os1 Cl1 151.53(6) . . ? C19 Os1 Cl1 92.86(6) . . ? C18 Os1 Cl1 121.03(6) . . ? C17 Os1 Cl1 158.37(6) . . ? C15 Os1 Cl1 114.08(6) . . ? C20 Os1 Cl1 90.25(6) . . ? C2 N1 C6 117.99(18) . . ? C2 N1 Os1 127.67(14) . . ? C6 N1 Os1 114.34(14) . . ? N1 C2 C3 122.4(2) . . ? N1 C2 H2A 118.8 . . ? C3 C2 H2A 118.8 . . ? C2 C3 C4 118.6(2) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C5 C4 C3 120.4(2) . . ? C5 C4 Cl4 119.34(17) . . ? C3 C4 Cl4 120.24(18) . . ? C4 C5 C6 117.3(2) . . ? C4 C5 H5A 121.4 . . ? C6 C5 H5A 121.4 . . ? N1 C6 C5 123.2(2) . . ? N1 C6 N7 116.98(19) . . ? C5 C6 N7 119.81(19) . . ? N8 N7 C6 111.09(17) . . ? N7 N8 C9 113.26(17) . . ? N7 N8 Os1 122.58(14) . . ? C9 N8 Os1 124.04(13) . . ? C14 C9 C10 121.9(2) . . ? C14 C9 N8 119.10(19) . . ? C10 C9 N8 119.0(2) . . ? C11 C10 C9 118.6(2) . . ? C11 C10 H10A 120.7 . . ? C9 C10 H10A 120.7 . . ? C12 C11 C10 120.4(2) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C13 120.6(2) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 120.0(2) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C9 C14 C13 118.5(2) . . ? C9 C14 H14A 120.8 . . ? C13 C14 H14A 120.8 . . ? C20 C15 C16 120.8(2) . . ? C20 C15 Os1 73.45(12) . . ? C16 C15 Os1 68.45(11) . . ? C20 C15 H15A 118.9 . . ? C16 C15 H15A 118.9 . . ? Os1 C15 H15A 118.9 . . ? C17 C16 C15 121.0(2) . . ? C17 C16 Os1 73.33(12) . . ? C15 C16 Os1 73.66(12) . . ? C17 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? Os1 C16 H16A 119.3 . . ? C16 C17 C18 117.9(2) . . ? C16 C17 C24 120.7(2) . . ? C18 C17 C24 121.3(2) . . ? C16 C17 Os1 69.18(12) . . ? C18 C17 Os1 70.92(12) . . ? C24 C17 Os1 128.43(14) . . ? C19 C18 C17 121.0(2) . . ? C19 C18 Os1 71.27(12) . . ? C17 C18 Os1 71.72(12) . . ? C19 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? Os1 C18 H18A 118.9 . . ? C18 C19 C20 121.0(2) . . ? C18 C19 Os1 71.55(12) . . ? C20 C19 Os1 74.01(12) . . ? C18 C19 H19A 119.2 . . ? C20 C19 H19A 119.2 . . ? Os1 C19 H19A 119.2 . . ? C15 C20 C19 118.0(2) . . ? C15 C20 C21 123.4(2) . . ? C19 C20 C21 118.5(2) . . ? C15 C20 Os1 70.39(11) . . ? C19 C20 Os1 68.82(11) . . ? C21 C20 Os1 129.63(14) . . ? C20 C21 C22 113.82(19) . . ? C20 C21 C23 108.68(19) . . ? C22 C21 C23 110.83(19) . . ? C20 C21 H21A 107.8 . . ? C22 C21 H21A 107.8 . . ? C23 C21 H21A 107.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C17 C24 H24A 109.5 . . ? C17 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C17 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F14 P10 F11 90.48(10) . . ? F14 P10 F12 90.56(9) . . ? F11 P10 F12 178.78(10) . . ? F14 P10 F15 90.32(8) . . ? F11 P10 F15 90.35(9) . . ? F12 P10 F15 90.28(9) . . ? F14 P10 F16 90.49(9) . . ? F11 P10 F16 89.93(9) . . ? F12 P10 F16 89.43(8) . . ? F15 P10 F16 179.14(9) . . ? F14 P10 F13 179.31(9) . . ? F11 P10 F13 89.97(9) . . ? F12 P10 F13 88.99(8) . . ? F15 P10 F13 89.16(9) . . ? F16 P10 F13 90.02(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C13 H13A F15 0.95 2.47 3.290(3) 145.1 2_766 C19 H19A F11 1.00 2.46 3.090(3) 120.7 2_666 C16 H16A F13 1.00 2.44 3.350(3) 150.9 2_676 C19 H19A Cl4 1.00 2.92 3.855(2) 155.6 1_545 _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.287 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.140