Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Professor Osamu Ishitani' _publ_contact_author_address ; Depatment of Chemistry, Graduate School of Science and Engineering, Tokyo Institute of Technology, 2-12-1 Ookayama, Meguro-ku Tokyo 152-8551, JAPAN ; _publ_contact_author_email ishitani@chem.titech.ac.jp _publ_contact_author_fax 81(35734)2240 _publ_contact_author_phone 81(35734)2240 _publ_section_title ; Crystal and molecular structure of [Re(bpy)(CO)3{P(n-Bu)3}]PF6 ; _publ_section_abstract ; We present the crystal and molecular structure of [Re(bpy)(CO)3{P(n-Bu)3}]PF6. ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. ; loop_ _publ_author_name 'Osamu Ishitani' 'Kazuhide Koike' 'Hideki Saitoh' 'Shigeki Tohyama' 'Hideaki Tsubaki' data_1+cif _database_code_depnum_ccdc_archive 'CCDC 239864' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1+ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H35 F6 N2 O3 P2 Re' _chemical_formula_weight 773.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.605(4) _cell_length_b 23.792(6) _cell_length_c 11.351(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.75(3) _cell_angle_gamma 90.00 _cell_volume 3066.1(16) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 15.81 _cell_measurement_theta_max 17.44 _exptl_crystal_description Cube _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 4.132 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4920 _exptl_absorpt_correction_T_max 0.6369 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science MXC18' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 11 _diffrn_reflns_number 9326 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.63 _reflns_number_total 8657 _reflns_number_gt 5120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC(MAC Science)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_reduction Crystan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0733P)^2^+22.7247P] 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 8657 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1158 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.2044 _refine_ls_wR_factor_gt 0.1365 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.07327(3) 0.189468(16) 0.88111(3) 0.05446(14) Uani 1 1 d . . . P1 P -0.0896(2) 0.12053(11) 0.8270(2) 0.0589(6) Uani 1 1 d . . . P2 P 0.3706(3) 0.09132(17) 0.6640(4) 0.0861(9) Uani 1 1 d . . . F1 F 0.3516(16) 0.0442(5) 0.7469(14) 0.199(7) Uani 1 1 d . . . F2 F 0.3940(18) 0.0465(5) 0.5797(17) 0.229(9) Uani 1 1 d . . . F3 F 0.3825(16) 0.1361(5) 0.5718(15) 0.192(6) Uani 1 1 d . . . F4 F 0.3543(13) 0.1365(5) 0.7561(15) 0.180(6) Uani 1 1 d . . . F5 F 0.4996(11) 0.0989(10) 0.7445(18) 0.263(10) Uani 1 1 d . . . F6 F 0.2410(11) 0.0874(10) 0.584(2) 0.283(11) Uani 1 1 d . . . O1 O 0.0563(8) 0.1688(4) 0.6063(8) 0.083(2) Uani 1 1 d . . . O2 O -0.1033(9) 0.2847(5) 0.7522(10) 0.107(3) Uani 1 1 d . . . O3 O 0.2877(9) 0.2653(3) 0.9296(11) 0.102(3) Uani 1 1 d . . . N1 N 0.1950(7) 0.1238(4) 0.9996(8) 0.0618(19) Uani 1 1 d . . . N2 N 0.0805(8) 0.1981(3) 1.0755(8) 0.0624(19) Uani 1 1 d . . . C1 C 0.0653(9) 0.1747(5) 0.7087(11) 0.069(3) Uani 1 1 d . . . C2 C -0.0363(11) 0.2491(5) 0.7974(11) 0.072(3) Uani 1 1 d . . . C3 C 0.2083(10) 0.2375(5) 0.9166(10) 0.071(3) Uani 1 1 d . . . C4 C 0.2571(9) 0.0909(5) 0.9575(13) 0.079(3) Uani 1 1 d . . . H4 H 0.2486 0.0955 0.8725 0.095 Uiso 1 1 calc R . . C5 C 0.3341(11) 0.0500(5) 1.0361(16) 0.093(4) Uani 1 1 d . . . H5 H 0.3786 0.0283 1.0060 0.111 Uiso 1 1 calc R . . C6 C 0.3424(12) 0.0426(6) 1.1624(15) 0.100(5) Uani 1 1 d . . . H6 H 0.3886 0.0138 1.2152 0.120 Uiso 1 1 calc R . . C7 C 0.2828(11) 0.0776(5) 1.2078(13) 0.086(4) Uani 1 1 d . . . H7 H 0.2922 0.0741 1.2934 0.103 Uiso 1 1 calc R . . C8 C 0.2078(9) 0.1186(4) 1.1259(10) 0.069(3) Uani 1 1 d . . . C9 C 0.1426(11) 0.1603(5) 1.1663(11) 0.075(3) Uani 1 1 d . . . C10 C 0.1417(13) 0.1569(5) 1.2885(11) 0.086(4) Uani 1 1 d . . . H10 H 0.1817 0.1286 1.3475 0.103 Uiso 1 1 calc R . . C11 C 0.0791(15) 0.1975(7) 1.3179(13) 0.104(5) Uani 1 1 d . . . H11 H 0.0769 0.1968 1.3987 0.125 Uiso 1 1 calc R . . C12 C 0.0205(14) 0.2385(6) 1.2299(13) 0.093(4) Uani 1 1 d . . . H12 H -0.0207 0.2661 1.2510 0.111 Uiso 1 1 calc R . . C13 C 0.0225(12) 0.2390(6) 1.1094(12) 0.085(3) Uani 1 1 d . . . H13 H -0.0162 0.2675 1.0503 0.103 Uiso 1 1 calc R . . C18 C -0.1607(11) 0.1159(5) 0.9370(11) 0.079(3) Uani 1 1 d . . . H18B H -0.2087 0.0821 0.9145 0.095 Uiso 1 1 calc R . . H18A H -0.0994 0.1108 1.0252 0.095 Uiso 1 1 calc R . . C19 C -0.2380(13) 0.1648(7) 0.9390(14) 0.097(4) Uani 1 1 d . . . H19B H -0.3064 0.1678 0.8552 0.117 Uiso 1 1 calc R . . H19A H -0.1942 0.1998 0.9551 0.117 Uiso 1 1 calc R . . C20 C -0.2783(19) 0.1541(13) 1.0515(16) 0.173(11) Uani 1 1 d . . . H20B H -0.3090 0.1161 1.0409 0.208 Uiso 1 1 calc R . . H20A H -0.2084 0.1552 1.1343 0.208 Uiso 1 1 calc R . . C21 C -0.355(2) 0.1870(17) 1.061(3) 0.27(2) Uani 1 1 d . . . H21A H -0.3637 0.2202 1.0101 0.404 Uiso 1 1 calc R . . H21B H -0.3302 0.1973 1.1513 0.404 Uiso 1 1 calc R . . H21C H -0.4299 0.1680 1.0301 0.404 Uiso 1 1 calc R . . C22 C -0.2072(9) 0.1314(5) 0.6614(9) 0.065(2) Uani 1 1 d . . . H22B H -0.2427 0.1678 0.6589 0.078 Uiso 1 1 calc R . . H22A H -0.1715 0.1328 0.6010 0.078 Uiso 1 1 calc R . . C23 C -0.3058(10) 0.0873(6) 0.6113(11) 0.087(4) Uani 1 1 d . . . H23A H -0.2722 0.0508 0.6091 0.104 Uiso 1 1 calc R . . H23B H -0.3416 0.0849 0.6715 0.104 Uiso 1 1 calc R . . C24 C -0.4009(10) 0.1015(7) 0.4743(12) 0.095(4) Uani 1 1 d . . . H24B H -0.4666 0.0759 0.4532 0.114 Uiso 1 1 calc R . . H24A H -0.4295 0.1393 0.4759 0.114 Uiso 1 1 calc R . . C25 C -0.3608(13) 0.0984(6) 0.3684(13) 0.098(4) Uani 1 1 d . . . H25A H -0.3033 0.1271 0.3818 0.147 Uiso 1 1 calc R . . H25B H -0.4270 0.1038 0.2850 0.147 Uiso 1 1 calc R . . H25C H -0.3265 0.0622 0.3703 0.147 Uiso 1 1 calc R . . C14 C -0.0443(10) 0.0478(4) 0.8303(11) 0.070(3) Uani 1 1 d . . . H14A H 0.0206 0.0405 0.9150 0.084 Uiso 1 1 calc R . . H14B H -0.1093 0.0239 0.8226 0.084 Uiso 1 1 calc R . . C15 C -0.0063(11) 0.0307(5) 0.7246(12) 0.082(3) Uani 1 1 d . . . H15B H -0.0733 0.0325 0.6394 0.099 Uiso 1 1 calc R . . H15A H 0.0532 0.0566 0.7247 0.099 Uiso 1 1 calc R . . C16 C 0.0434(13) -0.0290(5) 0.7495(14) 0.095(4) Uani 1 1 d . . . H16A H 0.1156 -0.0294 0.8300 0.114 Uiso 1 1 calc R . . H16B H -0.0125 -0.0537 0.7611 0.114 Uiso 1 1 calc R . . C17 C 0.0687(16) -0.0512(6) 0.6406(17) 0.115(5) Uani 1 1 d . . . H17C H -0.0014 -0.0492 0.5597 0.172 Uiso 1 1 calc R . . H17B H 0.0941 -0.0896 0.6584 0.172 Uiso 1 1 calc R . . H17A H 0.1296 -0.0291 0.6340 0.172 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 Re1 0.0593(2) 0.0575(2) 0.0448(2) 0.00412(14) 0.02100(16) 0.00041(14) P1 0.0615(14) 0.0666(14) 0.0459(12) 0.0065(10) 0.0208(10) 0.0010(11) P2 0.0736(19) 0.104(2) 0.091(2) 0.0092(19) 0.0450(18) 0.0048(18) F1 0.36(2) 0.131(8) 0.194(13) 0.006(9) 0.204(15) -0.015(11) F2 0.42(3) 0.128(9) 0.287(18) -0.065(10) 0.288(19) -0.071(12) F3 0.290(18) 0.133(9) 0.190(13) 0.011(9) 0.138(13) -0.024(11) F4 0.237(15) 0.155(10) 0.235(14) -0.020(10) 0.183(13) -0.019(10) F5 0.085(8) 0.43(3) 0.235(17) -0.116(19) 0.031(9) 0.001(12) F6 0.080(8) 0.41(3) 0.29(2) 0.08(2) 0.014(10) -0.021(12) O1 0.102(6) 0.097(6) 0.058(5) -0.008(4) 0.043(4) 0.001(5) O2 0.106(7) 0.113(7) 0.091(7) 0.015(6) 0.032(6) 0.033(6) O3 0.097(7) 0.061(4) 0.135(8) 0.000(5) 0.039(6) -0.024(4) N1 0.052(4) 0.078(5) 0.050(4) 0.003(4) 0.017(3) -0.005(4) N2 0.069(5) 0.062(4) 0.052(4) -0.003(4) 0.023(4) -0.006(4) C1 0.059(6) 0.085(7) 0.059(6) 0.013(5) 0.024(5) -0.004(5) C2 0.074(7) 0.071(6) 0.062(6) 0.002(5) 0.020(5) 0.002(5) C3 0.076(7) 0.076(6) 0.056(6) -0.008(5) 0.024(5) -0.015(5) C4 0.055(6) 0.093(8) 0.082(8) -0.001(6) 0.023(5) -0.006(5) C5 0.063(7) 0.073(7) 0.126(12) 0.012(7) 0.024(7) 0.020(6) C6 0.072(8) 0.101(10) 0.094(10) 0.031(8) 0.005(7) -0.007(7) C7 0.077(8) 0.084(8) 0.071(7) 0.005(6) 0.009(6) -0.009(6) C8 0.058(5) 0.072(6) 0.054(5) 0.013(5) 0.004(4) -0.012(5) C9 0.078(7) 0.088(7) 0.051(5) -0.002(5) 0.022(5) -0.016(6) C10 0.125(11) 0.077(7) 0.050(6) -0.005(5) 0.033(6) -0.023(7) C11 0.135(13) 0.122(12) 0.055(7) -0.008(7) 0.041(8) -0.039(10) C12 0.136(12) 0.081(7) 0.082(9) -0.025(7) 0.068(9) -0.018(8) C13 0.088(8) 0.105(9) 0.067(7) -0.018(6) 0.037(6) -0.016(7) C18 0.082(7) 0.092(8) 0.061(6) 0.004(6) 0.030(6) -0.004(6) C19 0.086(9) 0.125(11) 0.082(9) -0.015(8) 0.038(7) 0.008(8) C20 0.138(16) 0.32(3) 0.074(10) -0.008(15) 0.057(11) 0.092(19) C21 0.17(2) 0.55(7) 0.13(2) 0.07(3) 0.10(2) 0.09(3) C22 0.063(6) 0.076(6) 0.052(5) 0.008(5) 0.023(4) 0.002(5) C23 0.056(6) 0.134(11) 0.062(6) 0.012(7) 0.019(5) -0.019(7) C24 0.058(6) 0.145(12) 0.070(7) 0.009(8) 0.016(6) 0.009(7) C25 0.109(11) 0.113(10) 0.069(8) -0.013(7) 0.036(7) -0.027(9) C14 0.072(6) 0.057(5) 0.065(6) 0.006(4) 0.016(5) -0.010(5) C15 0.075(7) 0.087(7) 0.071(7) -0.003(6) 0.020(6) 0.013(6) C16 0.100(10) 0.077(7) 0.088(9) 0.020(7) 0.022(7) 0.018(7) C17 0.142(14) 0.068(7) 0.138(14) -0.007(8) 0.065(12) 0.028(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 Re1 C2 1.920(12) . ? Re1 C3 1.942(11) . ? Re1 C1 1.947(12) . ? Re1 N2 2.178(9) . ? Re1 N1 2.194(8) . ? Re1 P1 2.487(3) . ? P1 C14 1.817(11) . ? P1 C18 1.829(12) . ? P1 C22 1.837(10) . ? P2 F6 1.487(13) . ? P2 F5 1.491(13) . ? P2 F2 1.545(12) . ? P2 F3 1.546(12) . ? P2 F1 1.547(11) . ? P2 F4 1.574(12) . ? O1 C1 1.127(13) . ? O2 C2 1.147(13) . ? O3 C3 1.154(13) . ? N1 C4 1.333(14) . ? N1 C8 1.377(13) . ? N2 C9 1.335(14) . ? N2 C13 1.369(15) . ? C4 C5 1.390(16) . ? C4 H4 0.9300 . ? C5 C6 1.40(2) . ? C5 H5 0.9300 . ? C6 C7 1.36(2) . ? C6 H6 0.9300 . ? C7 C8 1.396(15) . ? C7 H7 0.9300 . ? C8 C9 1.481(17) . ? C9 C10 1.394(15) . ? C10 C11 1.38(2) . ? C10 H10 0.9300 . ? C11 C12 1.36(2) . ? C11 H11 0.9300 . ? C12 C13 1.379(16) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C18 C19 1.526(18) . ? C18 H18B 0.9700 . ? C18 H18A 0.9700 . ? C19 C20 1.59(2) . ? C19 H19B 0.9700 . ? C19 H19A 0.9700 . ? C20 C21 1.29(3) . ? C20 H20B 0.9700 . ? C20 H20A 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.534(15) . ? C22 H22B 0.9700 . ? C22 H22A 0.9700 . ? C23 C24 1.533(16) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.495(18) . ? C24 H24B 0.9700 . ? C24 H24A 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C14 C15 1.528(16) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.528(16) . ? C15 H15B 0.9700 . ? C15 H15A 0.9700 . ? C16 C17 1.50(2) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17C 0.9600 . ? C17 H17B 0.9600 . ? C17 H17A 0.9600 . ? 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 C2 Re1 C3 92.5(5) . . ? C2 Re1 C1 85.6(5) . . ? C3 Re1 C1 88.4(4) . . ? C2 Re1 N2 97.8(4) . . ? C3 Re1 N2 95.0(4) . . ? C1 Re1 N2 175.0(4) . . ? C2 Re1 N1 172.5(4) . . ? C3 Re1 N1 88.6(4) . . ? C1 Re1 N1 101.8(4) . . ? N2 Re1 N1 74.7(3) . . ? C2 Re1 P1 91.5(4) . . ? C3 Re1 P1 174.0(4) . . ? C1 Re1 P1 87.5(3) . . ? N2 Re1 P1 88.8(2) . . ? N1 Re1 P1 87.9(2) . . ? C14 P1 C18 99.8(6) . . ? C14 P1 C22 105.1(5) . . ? C18 P1 C22 106.9(5) . . ? C14 P1 Re1 113.9(4) . . ? C18 P1 Re1 117.9(4) . . ? C22 P1 Re1 111.9(3) . . ? F6 P2 F5 176.6(14) . . ? F6 P2 F2 91.8(13) . . ? F5 P2 F2 90.7(10) . . ? F6 P2 F3 91.8(11) . . ? F5 P2 F3 86.0(11) . . ? F2 P2 F3 87.4(7) . . ? F6 P2 F1 84.8(11) . . ? F5 P2 F1 97.5(12) . . ? F2 P2 F1 89.9(7) . . ? F3 P2 F1 175.6(9) . . ? F6 P2 F4 91.4(12) . . ? F5 P2 F4 86.1(9) . . ? F2 P2 F4 176.7(11) . . ? F3 P2 F4 93.3(7) . . ? F1 P2 F4 89.6(6) . . ? C4 N1 C8 120.0(10) . . ? C4 N1 Re1 124.1(8) . . ? C8 N1 Re1 115.8(7) . . ? C9 N2 C13 117.8(10) . . ? C9 N2 Re1 118.1(8) . . ? C13 N2 Re1 124.0(8) . . ? O1 C1 Re1 176.0(11) . . ? O2 C2 Re1 176.7(11) . . ? O3 C3 Re1 175.5(10) . . ? N1 C4 C5 122.4(13) . . ? N1 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C4 C5 C6 117.7(13) . . ? C4 C5 H5 121.1 . . ? C6 C5 H5 121.1 . . ? C7 C6 C5 120.1(13) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 120.1(13) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? N1 C8 C7 119.6(12) . . ? N1 C8 C9 115.7(9) . . ? C7 C8 C9 124.7(11) . . ? N2 C9 C10 123.5(13) . . ? N2 C9 C8 115.4(10) . . ? C10 C9 C8 121.0(12) . . ? C11 C10 C9 117.1(13) . . ? C11 C10 H10 121.5 . . ? C9 C10 H10 121.5 . . ? C12 C11 C10 120.7(13) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 119.6(14) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? N2 C13 C12 121.1(13) . . ? N2 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C19 C18 P1 118.0(9) . . ? C19 C18 H18B 107.8 . . ? P1 C18 H18B 107.8 . . ? C19 C18 H18A 107.8 . . ? P1 C18 H18A 107.8 . . ? H18B C18 H18A 107.1 . . ? C18 C19 C20 108.6(14) . . ? C18 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? C18 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? H19B C19 H19A 108.4 . . ? C21 C20 C19 119(2) . . ? C21 C20 H20B 107.5 . . ? C19 C20 H20B 107.5 . . ? C21 C20 H20A 107.5 . . ? C19 C20 H20A 107.5 . . ? H20B C20 H20A 107.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 P1 116.5(7) . . ? C23 C22 H22B 108.2 . . ? P1 C22 H22B 108.2 . . ? C23 C22 H22A 108.2 . . ? P1 C22 H22A 108.2 . . ? H22B C22 H22A 107.3 . . ? C24 C23 C22 112.0(11) . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C25 C24 C23 114.6(11) . . ? C25 C24 H24B 108.6 . . ? C23 C24 H24B 108.6 . . ? C25 C24 H24A 108.6 . . ? C23 C24 H24A 108.6 . . ? H24B C24 H24A 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C15 C14 P1 116.2(8) . . ? C15 C14 H14A 108.2 . . ? P1 C14 H14A 108.2 . . ? C15 C14 H14B 108.2 . . ? P1 C14 H14B 108.2 . . ? H14A C14 H14B 107.4 . . ? C16 C15 C14 110.3(11) . . ? C16 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? H15B C15 H15A 108.1 . . ? C17 C16 C15 113.1(11) . . ? C17 C16 H16A 109.0 . . ? C15 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 C17 H17C 109.5 . . ? C16 C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? C16 C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 3.117 _refine_diff_density_min -2.367 _refine_diff_density_rms 0.217 #===END data_2+cif _database_code_depnum_ccdc_archive 'CCDC 239865' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2+ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H23 F6 N2 O3 P2 Re' _chemical_formula_weight 689.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 16.185(3) _cell_length_b 14.044(2) _cell_length_c 10.644(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2419.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 30.00 _exptl_crystal_description Cube _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 5.224 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4214 _exptl_absorpt_correction_T_max 0.7446 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science MXC18' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10 _diffrn_reflns_number 3822 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 22.40 _diffrn_reflns_theta_max 34.84 _reflns_number_total 3702 _reflns_number_gt 2235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC(MAC Science)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_reduction Crystan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0403P)^2^+12.0085P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.16(3) _refine_ls_number_reflns 3702 _refine_ls_number_parameters 301 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re -0.24828(3) 0.87147(3) 0.1256(3) 0.04037(13) Uani 1 1 d . . . P1 P -0.1427(2) 1.0007(3) 0.1402(6) 0.0618(9) Uani 1 1 d . . . P2 P -0.4969(3) 1.1667(3) 0.2968(5) 0.0570(9) Uani 1 1 d . . . F1 F -0.4056(7) 1.1700(11) 0.2436(16) 0.118(5) Uani 1 1 d . . . F2 F -0.4668(9) 1.1196(10) 0.4241(12) 0.106(5) Uani 1 1 d . . . F3 F -0.5275(9) 1.2171(10) 0.1726(12) 0.113(4) Uani 1 1 d . . . F4 F -0.4817(8) 1.2708(8) 0.3601(14) 0.104(4) Uani 1 1 d . . . F5 F -0.5887(8) 1.1659(11) 0.3486(16) 0.115(5) Uani 1 1 d . . . F6 F -0.5106(9) 1.0648(8) 0.2411(14) 0.105(4) Uani 1 1 d . . . O1 O -0.3777(9) 1.0128(10) 0.0371(14) 0.092(4) Uani 1 1 d . . . O2 O -0.2041(11) 0.8373(13) -0.1428(13) 0.085(4) Uani 1 1 d . . . O3 O -0.3784(8) 0.7116(9) 0.1221(19) 0.089(4) Uani 1 1 d . . . N1 N -0.2707(7) 0.8883(8) 0.3339(11) 0.043(2) Uani 1 1 d . . . N2 N -0.1566(7) 0.7784(8) 0.2257(10) 0.045(2) Uani 1 1 d . . . C1 C -0.3306(11) 0.9603(11) 0.0716(15) 0.062(4) Uani 1 1 d . . . C2 C -0.2193(10) 0.8480(12) -0.0379(16) 0.055(3) Uani 1 1 d . . . C3 C -0.3292(8) 0.7700(10) 0.129(2) 0.066(4) Uani 1 1 d . . . C4 C -0.3310(8) 0.9398(11) 0.3861(14) 0.052(3) Uani 1 1 d . . . H4 H -0.3672 0.9720 0.3332 0.062 Uiso 1 1 calc R . . C5 C -0.3423(13) 0.9477(15) 0.5094(17) 0.075(5) Uani 1 1 d . . . H5 H -0.3838 0.9872 0.5400 0.090 Uiso 1 1 calc R . . C6 C -0.2941(13) 0.8988(15) 0.5912(17) 0.083(6) Uani 1 1 d . . . H6 H -0.3046 0.9008 0.6771 0.100 Uiso 1 1 calc R . . C7 C -0.2286(10) 0.8456(14) 0.5440(15) 0.061(4) Uani 1 1 d . . . H7 H -0.1925 0.8158 0.5995 0.073 Uiso 1 1 calc R . . C8 C -0.2157(14) 0.8359(13) 0.4117(16) 0.061(5) Uani 1 1 d . . . C9 C -0.1564(7) 0.7784(9) 0.3504(13) 0.044(3) Uani 1 1 d . . . C10 C -0.1003(10) 0.7259(12) 0.4192(18) 0.066(4) Uani 1 1 d . . . H10 H -0.0985 0.7304 0.5064 0.079 Uiso 1 1 calc R . . C11 C -0.0477(12) 0.6673(12) 0.355(2) 0.073(5) Uani 1 1 d . . . H11 H -0.0098 0.6297 0.3983 0.087 Uiso 1 1 calc R . . C12 C -0.0518(12) 0.6651(14) 0.2250(19) 0.073(5) Uani 1 1 d . . . H12 H -0.0183 0.6236 0.1797 0.088 Uiso 1 1 calc R . . C13 C -0.1046(10) 0.7236(11) 0.1648(18) 0.066(5) Uani 1 1 d . . . H13 H -0.1042 0.7251 0.0774 0.079 Uiso 1 1 calc R . . C16 C -0.0372(12) 0.9570(13) 0.119(4) 0.115(9) Uani 1 1 d . . . H16A H -0.0242 0.9151 0.1886 0.138 Uiso 1 1 calc R . . H16B H -0.0359 0.9188 0.0429 0.138 Uiso 1 1 calc R . . C17 C 0.0294(13) 1.0299(16) 0.110(4) 0.137(14) Uani 1 1 d . . . H17A H 0.0772 1.0023 0.0706 0.206 Uiso 1 1 calc R . . H17B H 0.0435 1.0518 0.1923 0.206 Uiso 1 1 calc R . . H17C H 0.0103 1.0826 0.0601 0.206 Uiso 1 1 calc R . . C18 C -0.153(2) 1.097(2) 0.038(3) 0.154(16) Uani 1 1 d . . . H18A H -0.2033 1.1298 0.0595 0.184 Uiso 1 1 calc R . . H18B H -0.1075 1.1404 0.0553 0.184 Uiso 1 1 calc R . . C19 C -0.154(3) 1.080(3) -0.097(3) 0.21(3) Uani 1 1 d . . . H19A H -0.1242 1.0225 -0.1156 0.320 Uiso 1 1 calc R . . H19B H -0.1280 1.1325 -0.1394 0.320 Uiso 1 1 calc R . . H19C H -0.2099 1.0740 -0.1250 0.320 Uiso 1 1 calc R . . C14 C -0.1276(16) 1.053(2) 0.305(3) 0.135(14) Uani 1 1 d . . . H14A H -0.1245 1.0018 0.3660 0.162 Uiso 1 1 calc R . . H14B H -0.0761 1.0882 0.3080 0.162 Uiso 1 1 calc R . . C15 C -0.195(2) 1.115(2) 0.337(4) 0.164(17) Uani 1 1 d . . . H15C H -0.1986 1.1656 0.2758 0.246 Uiso 1 1 calc R . . H15B H -0.1856 1.1424 0.4185 0.246 Uiso 1 1 calc R . . H15A H -0.2457 1.0800 0.3374 0.246 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 Re1 0.0503(2) 0.0379(2) 0.03290(19) -0.0001(5) -0.0025(3) 0.00326(16) P1 0.068(2) 0.0509(16) 0.067(3) 0.005(3) 0.005(3) -0.0092(15) P2 0.0552(19) 0.061(2) 0.055(2) -0.005(2) 0.0000(18) 0.0059(17) F1 0.067(7) 0.132(11) 0.155(14) -0.049(10) 0.024(8) -0.009(8) F2 0.122(11) 0.125(11) 0.072(8) 0.005(8) -0.035(8) 0.029(9) F3 0.137(11) 0.125(10) 0.077(8) 0.036(8) -0.014(8) 0.001(9) F4 0.105(9) 0.078(7) 0.127(12) -0.029(7) -0.040(9) 0.017(7) F5 0.078(7) 0.139(11) 0.129(12) 0.000(10) 0.039(8) 0.010(8) F6 0.128(10) 0.070(6) 0.118(11) -0.027(7) -0.015(9) -0.007(7) O1 0.102(10) 0.103(10) 0.070(8) 0.014(8) -0.031(8) 0.037(9) O2 0.101(11) 0.116(12) 0.038(7) -0.010(8) 0.008(7) 0.002(11) O3 0.097(8) 0.080(7) 0.091(10) -0.001(11) -0.019(11) -0.036(7) N1 0.048(6) 0.052(6) 0.030(5) 0.002(5) -0.012(5) -0.001(5) N2 0.051(6) 0.049(6) 0.037(5) 0.002(4) -0.006(5) 0.004(5) C1 0.080(10) 0.060(8) 0.047(7) -0.011(6) -0.026(7) 0.039(8) C2 0.060(8) 0.059(8) 0.046(8) 0.001(7) -0.008(7) 0.011(7) C3 0.056(7) 0.069(8) 0.074(10) -0.010(12) 0.019(12) 0.000(6) C4 0.041(6) 0.063(8) 0.050(8) -0.010(6) -0.013(6) 0.007(6) C5 0.078(12) 0.103(15) 0.045(9) -0.011(9) 0.016(9) -0.008(11) C6 0.095(14) 0.113(15) 0.042(9) -0.023(9) 0.025(9) -0.017(13) C7 0.061(9) 0.087(11) 0.034(7) 0.021(7) -0.003(6) 0.012(8) C8 0.091(13) 0.049(8) 0.042(8) 0.005(7) -0.032(9) 0.003(9) C9 0.039(5) 0.047(6) 0.047(7) 0.001(5) 0.013(5) -0.005(5) C10 0.066(10) 0.073(10) 0.059(9) 0.013(9) 0.004(8) 0.011(8) C11 0.075(11) 0.059(9) 0.083(13) 0.015(9) 0.000(10) 0.042(9) C12 0.069(11) 0.083(12) 0.069(12) 0.006(9) -0.004(9) 0.023(10) C13 0.067(9) 0.062(8) 0.068(12) 0.003(8) 0.012(8) 0.012(7) C16 0.080(12) 0.067(10) 0.20(3) 0.02(2) 0.01(2) -0.010(9) C17 0.081(13) 0.094(14) 0.24(4) -0.01(2) 0.08(2) -0.014(11) C18 0.21(4) 0.11(2) 0.15(3) 0.08(2) -0.06(3) -0.06(2) C19 0.39(7) 0.18(4) 0.068(18) 0.06(2) -0.02(3) -0.06(5) C14 0.109(18) 0.15(3) 0.14(3) -0.10(2) 0.077(18) -0.072(18) C15 0.13(3) 0.16(3) 0.20(4) -0.09(3) 0.02(3) -0.06(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 Re1 C2 1.833(17) . ? Re1 C1 1.913(13) . ? Re1 C3 1.936(14) . ? Re1 N2 2.245(11) . ? Re1 N1 2.258(12) . ? Re1 P1 2.498(4) . ? P1 C18 1.74(2) . ? P1 C16 1.83(2) . ? P1 C14 1.92(3) . ? P2 F6 1.566(12) . ? P2 F3 1.579(12) . ? P2 F1 1.583(12) . ? P2 F2 1.584(13) . ? P2 F5 1.585(12) . ? P2 F4 1.628(12) . ? O1 C1 1.123(16) . ? O2 C2 1.15(2) . ? O3 C3 1.145(16) . ? N1 C4 1.337(18) . ? N1 C8 1.42(2) . ? N2 C13 1.312(18) . ? N2 C9 1.327(17) . ? C4 C5 1.33(2) . ? C4 H4 0.9300 . ? C5 C6 1.36(3) . ? C5 H5 0.9300 . ? C6 C7 1.39(3) . ? C6 H6 0.9300 . ? C7 C8 1.43(2) . ? C7 H7 0.9300 . ? C8 C9 1.42(2) . ? C9 C10 1.38(2) . ? C10 C11 1.37(2) . ? C10 H10 0.9300 . ? C11 C12 1.39(3) . ? C11 H11 0.9300 . ? C12 C13 1.35(2) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C16 C17 1.49(2) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.46(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C14 C15 1.44(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15C 0.9600 . ? C15 H15B 0.9600 . ? C15 H15A 0.9600 . ? 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 C2 Re1 C1 90.6(7) . . ? C2 Re1 C3 93.3(9) . . ? C1 Re1 C3 90.8(8) . . ? C2 Re1 N2 100.2(6) . . ? C1 Re1 N2 169.1(6) . . ? C3 Re1 N2 90.6(6) . . ? C2 Re1 N1 172.8(6) . . ? C1 Re1 N1 96.6(6) . . ? C3 Re1 N1 87.2(8) . . ? N2 Re1 N1 72.6(4) . . ? C2 Re1 P1 90.8(6) . . ? C1 Re1 P1 91.2(6) . . ? C3 Re1 P1 175.4(8) . . ? N2 Re1 P1 86.6(3) . . ? N1 Re1 P1 88.4(3) . . ? C18 P1 C16 105.6(17) . . ? C18 P1 C14 106.6(17) . . ? C16 P1 C14 97.1(15) . . ? C18 P1 Re1 117.5(11) . . ? C16 P1 Re1 112.8(6) . . ? C14 P1 Re1 115.0(7) . . ? F6 P2 F3 92.7(8) . . ? F6 P2 F1 91.3(8) . . ? F3 P2 F1 88.8(9) . . ? F6 P2 F2 89.2(8) . . ? F3 P2 F2 178.0(8) . . ? F1 P2 F2 91.8(9) . . ? F6 P2 F5 89.5(8) . . ? F3 P2 F5 90.0(8) . . ? F1 P2 F5 178.6(9) . . ? F2 P2 F5 89.3(9) . . ? F6 P2 F4 177.7(8) . . ? F3 P2 F4 89.5(8) . . ? F1 P2 F4 89.0(7) . . ? F2 P2 F4 88.6(8) . . ? F5 P2 F4 90.2(8) . . ? C4 N1 C8 119.7(14) . . ? C4 N1 Re1 125.6(9) . . ? C8 N1 Re1 114.7(11) . . ? C13 N2 C9 119.4(13) . . ? C13 N2 Re1 122.1(11) . . ? C9 N2 Re1 118.5(10) . . ? O1 C1 Re1 178.2(17) . . ? O2 C2 Re1 176.1(16) . . ? O3 C3 Re1 175(2) . . ? C5 C4 N1 123.8(16) . . ? C5 C4 H4 118.1 . . ? N1 C4 H4 118.1 . . ? C4 C5 C6 120.8(19) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C7 118.6(15) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? C6 C7 C8 121.2(16) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 N1 116.8(15) . . ? C9 C8 C7 127.4(15) . . ? N1 C8 C7 115.7(18) . . ? N2 C9 C10 122.3(14) . . ? N2 C9 C8 117.3(14) . . ? C10 C9 C8 120.4(15) . . ? C11 C10 C9 117.9(18) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? C10 C11 C12 118.7(16) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C13 C12 C11 119.5(18) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? N2 C13 C12 122.0(18) . . ? N2 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C17 C16 P1 116.9(14) . . ? C17 C16 H16A 108.1 . . ? P1 C16 H16A 108.1 . . ? C17 C16 H16B 108.1 . . ? P1 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 P1 119(3) . . ? C19 C18 H18A 107.4 . . ? P1 C18 H18A 107.4 . . ? C19 C18 H18B 107.4 . . ? P1 C18 H18B 107.4 . . ? H18A C18 H18B 107.0 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C14 P1 111(3) . . ? C15 C14 H14A 109.5 . . ? P1 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? P1 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 H15C 109.5 . . ? C14 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C14 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.761 _refine_diff_density_min -1.796 _refine_diff_density_rms 0.186 #===END data_3+cif _database_code_depnum_ccdc_archive 'CCDC 239866' _audit_creation_method SHELXL-97 _publ_section_abstract ; We present the crystal and molecular structure of [Re(bpy)(CO)3{P(p-MeOPh)3}]CF3SO3. ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. ; _chemical_name_systematic ; ? ; _chemical_name_common 3+ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H29 F3 N2 O9 P Re S' _chemical_formula_weight 927.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 20.965(2) _cell_length_b 11.0830(10) _cell_length_c 16.156(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.109(9) _cell_angle_gamma 90.00 _cell_volume 3525.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 15.85 _cell_measurement_theta_max 17.49 _exptl_crystal_description Cube _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 3.625 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4766 _exptl_absorpt_correction_T_max 0.6501 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science MXC18' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6 _diffrn_reflns_number 10877 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10290 _reflns_number_gt 7673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC(MAC Science)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_reduction Crystan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+11.5090P] 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 10290 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1056 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.004 _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 Re1 Re 1.042417(9) 0.183445(17) 0.141496(12) 0.03124(6) Uani 1 1 d . . . S1 S 1.27727(12) -0.0913(2) 0.47378(16) 0.0787(6) Uani 1 1 d . . . P1 P 0.99939(6) 0.18071(11) 0.26896(8) 0.0322(2) Uani 1 1 d . . . F1 F 1.2496(4) -0.3102(6) 0.4153(5) 0.147(3) Uani 1 1 d . . . F2 F 1.1746(4) -0.2304(8) 0.4600(5) 0.147(3) Uani 1 1 d . . . F3 F 1.1830(4) -0.1705(9) 0.3364(4) 0.175(4) Uani 1 1 d . . . O1 O 1.0729(2) -0.0870(4) 0.1648(3) 0.0608(12) Uani 1 1 d . . . O2 O 0.8998(2) 0.1261(5) 0.0126(3) 0.0667(13) Uani 1 1 d . . . O3 O 1.0901(3) 0.1612(4) -0.0187(3) 0.0630(12) Uani 1 1 d . . . O4 O 1.1888(2) 0.4924(4) 0.5467(3) 0.0621(12) Uani 1 1 d . . . O5 O 0.7273(2) 0.3855(4) 0.2310(3) 0.0589(11) Uani 1 1 d . . . O6 O 0.9440(3) -0.3209(4) 0.3619(3) 0.0766(15) Uani 1 1 d . . . O7 O 1.3061(4) -0.1460(8) 0.5635(4) 0.129(3) Uani 1 1 d . . . O8 O 1.3227(4) -0.0853(6) 0.4259(4) 0.103(2) Uani 1 1 d . . . O9 O 1.2357(3) 0.0115(5) 0.4697(4) 0.100(2) Uani 1 1 d . . . N1 N 1.1410(2) 0.2425(5) 0.2307(3) 0.0424(10) Uani 1 1 d . . . N2 N 1.0365(2) 0.3794(4) 0.1415(3) 0.0430(10) Uani 1 1 d . . . C1 C 1.0603(3) 0.0131(5) 0.1560(4) 0.0467(12) Uani 1 1 d . . . C2 C 0.9537(3) 0.1476(5) 0.0619(4) 0.0454(12) Uani 1 1 d . . . C3 C 1.0751(3) 0.1756(5) 0.0423(4) 0.0429(11) Uani 1 1 d . . . C4 C 1.1935(3) 0.1680(7) 0.2693(4) 0.0576(16) Uani 1 1 d . . . H4 H 1.1880 0.0855 0.2586 0.069 Uiso 1 1 calc R . . C5 C 1.2554(3) 0.2110(10) 0.3245(5) 0.080(3) Uani 1 1 d . . . H5 H 1.2910 0.1579 0.3506 0.096 Uiso 1 1 calc R . . C6 C 1.2636(4) 0.3304(10) 0.3401(5) 0.086(3) Uani 1 1 d . . . H6 H 1.3053 0.3601 0.3766 0.103 Uiso 1 1 calc R . . C7 C 1.2106(4) 0.4084(8) 0.3022(4) 0.076(2) Uani 1 1 d . . . H7 H 1.2160 0.4908 0.3132 0.091 Uiso 1 1 calc R . . C8 C 1.1490(3) 0.3625(6) 0.2473(4) 0.0490(14) Uani 1 1 d . . . C9 C 1.0900(3) 0.4376(5) 0.2006(4) 0.0482(13) Uani 1 1 d . . . C10 C 1.0877(5) 0.5613(6) 0.2139(6) 0.073(2) Uani 1 1 d . . . H10 H 1.1240 0.6003 0.2554 0.088 Uiso 1 1 calc R . . C11 C 1.0304(5) 0.6258(7) 0.1644(7) 0.090(3) Uani 1 1 d . . . H11 H 1.0277 0.7082 0.1734 0.108 Uiso 1 1 calc R . . C12 C 0.9774(5) 0.5670(6) 0.1017(6) 0.077(2) Uani 1 1 d . . . H12 H 0.9391 0.6090 0.0672 0.093 Uiso 1 1 calc R . . C13 C 0.9829(3) 0.4456(5) 0.0919(4) 0.0513(14) Uani 1 1 d . . . H13 H 0.9479 0.4064 0.0486 0.062 Uiso 1 1 calc R . . C14 C 1.0545(2) 0.2629(5) 0.3636(3) 0.0364(10) Uani 1 1 d . . . C19 C 1.1194(3) 0.2202(5) 0.4139(3) 0.0383(10) Uani 1 1 d . . . H19 H 1.1319 0.1418 0.4055 0.046 Uiso 1 1 calc R . . C18 C 1.1647(3) 0.2933(5) 0.4754(3) 0.0399(11) Uani 1 1 d . . . H18 H 1.2076 0.2643 0.5081 0.048 Uiso 1 1 calc R . . C17 C 1.1464(3) 0.4104(5) 0.4889(3) 0.0442(12) Uani 1 1 d . . . C16 C 1.0830(3) 0.4544(5) 0.4407(4) 0.0529(14) Uani 1 1 d . . . H16 H 1.0709 0.5327 0.4498 0.063 Uiso 1 1 calc R . . C15 C 1.0375(3) 0.3816(5) 0.3788(4) 0.0489(13) Uani 1 1 d . . . H15 H 0.9948 0.4116 0.3465 0.059 Uiso 1 1 calc R . . C20 C 0.9162(2) 0.2451(4) 0.2533(3) 0.0338(9) Uani 1 1 d . . . C21 C 0.8890(3) 0.2346(5) 0.3213(4) 0.0464(12) Uani 1 1 d . . . H21 H 0.9134 0.1947 0.3732 0.056 Uiso 1 1 calc R . . C22 C 0.8263(3) 0.2832(6) 0.3116(4) 0.0517(14) Uani 1 1 d . . . H22 H 0.8090 0.2767 0.3572 0.062 Uiso 1 1 calc R . . C23 C 0.7887(3) 0.3420(5) 0.2342(4) 0.0438(12) Uani 1 1 d . . . C24 C 0.8145(3) 0.3535(5) 0.1664(4) 0.0428(11) Uani 1 1 d . . . H24 H 0.7900 0.3938 0.1147 0.051 Uiso 1 1 calc R . . C25 C 0.8779(3) 0.3035(5) 0.1769(3) 0.0410(11) Uani 1 1 d . . . H25 H 0.8949 0.3098 0.1310 0.049 Uiso 1 1 calc R . . C26 C 0.9886(3) 0.0265(5) 0.3020(3) 0.0380(10) Uani 1 1 d . . . C27 C 0.9447(3) -0.0462(5) 0.2361(3) 0.0418(11) Uani 1 1 d . . . H27 H 0.9258 -0.0156 0.1793 0.050 Uiso 1 1 calc R . . C28 C 0.9286(3) -0.1625(5) 0.2532(4) 0.0451(12) Uani 1 1 d . . . H28 H 0.8991 -0.2090 0.2084 0.054 Uiso 1 1 calc R . . C29 C 0.9565(3) -0.2084(5) 0.3363(4) 0.0528(14) Uani 1 1 d . . . C30 C 1.0011(4) -0.1376(6) 0.4025(4) 0.0651(19) Uani 1 1 d . . . H30 H 1.0206 -0.1695 0.4589 0.078 Uiso 1 1 calc R . . C31 C 1.0166(3) -0.0221(6) 0.3863(4) 0.0558(16) Uani 1 1 d . . . H31 H 1.0459 0.0241 0.4316 0.067 Uiso 1 1 calc R . . C32 C 1.2586(3) 0.4614(7) 0.5866(5) 0.079(2) Uani 1 1 d . . . H32A H 1.2629 0.3954 0.6266 0.118 Uiso 1 1 calc R . . H32B H 1.2833 0.5297 0.6183 0.118 Uiso 1 1 calc R . . H32C H 1.2766 0.4382 0.5418 0.118 Uiso 1 1 calc R . . C33 C 0.6906(3) 0.4567(7) 0.1556(5) 0.0673(19) Uani 1 1 d . . . H33A H 0.7186 0.5224 0.1497 0.101 Uiso 1 1 calc R . . H33C H 0.6502 0.4882 0.1631 0.101 Uiso 1 1 calc R . . H33B H 0.6783 0.4074 0.1037 0.101 Uiso 1 1 calc R . . C34 C 0.8897(4) -0.3874(6) 0.3008(5) 0.073(2) Uani 1 1 d . . . H34B H 0.8499 -0.3376 0.2802 0.110 Uiso 1 1 calc R . . H34C H 0.8803 -0.4577 0.3293 0.110 Uiso 1 1 calc R . . H34A H 0.9026 -0.4117 0.2517 0.110 Uiso 1 1 calc R . . C35 C 1.2189(6) -0.2083(11) 0.4206(7) 0.105(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 Re1 0.03116(9) 0.02832(9) 0.03302(10) -0.00037(7) 0.00944(7) -0.00047(6) S1 0.0820(13) 0.0660(12) 0.0888(14) -0.0135(11) 0.0302(11) 0.0122(10) P1 0.0331(6) 0.0290(6) 0.0336(6) 0.0007(5) 0.0101(5) 0.0016(4) F1 0.178(7) 0.076(4) 0.167(7) -0.044(4) 0.036(6) -0.001(4) F2 0.113(5) 0.172(7) 0.162(7) 0.031(6) 0.056(5) -0.029(5) F3 0.163(7) 0.234(10) 0.078(4) -0.021(5) -0.022(4) -0.005(6) O1 0.065(3) 0.032(2) 0.086(3) 0.003(2) 0.026(2) 0.0087(19) O2 0.044(2) 0.091(4) 0.053(2) -0.016(2) -0.0004(19) -0.006(2) O3 0.084(3) 0.057(3) 0.061(3) -0.007(2) 0.042(3) -0.008(2) O4 0.053(2) 0.052(3) 0.065(3) -0.023(2) 0.000(2) -0.007(2) O5 0.046(2) 0.064(3) 0.074(3) 0.009(2) 0.031(2) 0.016(2) O6 0.095(4) 0.045(3) 0.082(4) 0.018(3) 0.019(3) -0.015(3) O7 0.131(6) 0.183(8) 0.053(3) 0.018(4) 0.006(3) 0.076(6) O8 0.114(5) 0.106(5) 0.109(5) 0.005(4) 0.066(4) -0.005(4) O9 0.127(5) 0.076(4) 0.090(4) 0.001(3) 0.027(4) 0.049(4) N1 0.035(2) 0.054(3) 0.037(2) -0.002(2) 0.0101(17) -0.0036(19) N2 0.051(2) 0.032(2) 0.052(3) 0.0017(19) 0.025(2) -0.0045(19) C1 0.054(3) 0.043(3) 0.051(3) 0.004(2) 0.029(3) 0.006(2) C2 0.048(3) 0.043(3) 0.043(3) -0.002(2) 0.012(2) 0.000(2) C3 0.048(3) 0.031(2) 0.050(3) 0.001(2) 0.019(2) -0.003(2) C4 0.038(3) 0.082(5) 0.049(3) 0.005(3) 0.011(2) 0.010(3) C5 0.038(3) 0.139(9) 0.056(4) 0.002(5) 0.007(3) 0.001(4) C6 0.048(4) 0.151(9) 0.049(4) -0.003(5) 0.003(3) -0.041(5) C7 0.064(4) 0.106(6) 0.050(4) -0.014(4) 0.011(3) -0.047(4) C8 0.052(3) 0.059(4) 0.041(3) -0.013(3) 0.022(2) -0.022(3) C9 0.052(3) 0.044(3) 0.050(3) -0.009(2) 0.019(3) -0.018(2) C10 0.101(6) 0.038(3) 0.091(5) -0.017(3) 0.046(5) -0.029(4) C11 0.138(8) 0.033(4) 0.131(8) 0.005(4) 0.087(7) -0.004(5) C12 0.094(6) 0.034(3) 0.126(7) 0.026(4) 0.067(5) 0.014(4) C13 0.056(3) 0.042(3) 0.063(4) 0.021(3) 0.030(3) 0.008(3) C14 0.038(2) 0.038(3) 0.030(2) -0.0023(19) 0.0091(18) -0.001(2) C19 0.040(2) 0.032(2) 0.041(2) -0.002(2) 0.011(2) -0.001(2) C18 0.038(2) 0.040(3) 0.036(2) -0.003(2) 0.0050(19) 0.003(2) C17 0.048(3) 0.045(3) 0.034(2) -0.010(2) 0.007(2) -0.002(2) C16 0.058(3) 0.035(3) 0.056(3) -0.015(2) 0.006(3) 0.002(2) C15 0.056(3) 0.032(3) 0.057(3) -0.007(2) 0.016(3) 0.006(2) C20 0.033(2) 0.030(2) 0.037(2) -0.0022(18) 0.0097(18) -0.0012(17) C21 0.047(3) 0.049(3) 0.043(3) 0.007(2) 0.015(2) 0.008(2) C22 0.060(3) 0.053(3) 0.053(3) 0.010(3) 0.033(3) 0.008(3) C23 0.043(3) 0.036(3) 0.057(3) 0.004(2) 0.023(2) 0.006(2) C24 0.040(3) 0.042(3) 0.047(3) 0.008(2) 0.016(2) 0.009(2) C25 0.037(2) 0.048(3) 0.042(3) 0.006(2) 0.019(2) 0.005(2) C26 0.046(3) 0.032(2) 0.036(2) 0.0060(19) 0.014(2) 0.003(2) C27 0.046(3) 0.038(3) 0.038(2) -0.001(2) 0.010(2) -0.003(2) C28 0.054(3) 0.035(3) 0.051(3) -0.001(2) 0.023(3) -0.007(2) C29 0.059(4) 0.031(3) 0.065(4) 0.007(2) 0.018(3) -0.001(2) C30 0.085(5) 0.052(4) 0.042(3) 0.020(3) 0.000(3) -0.009(3) C31 0.077(4) 0.046(3) 0.034(3) 0.006(2) 0.005(3) -0.015(3) C32 0.056(4) 0.073(5) 0.085(5) -0.033(4) -0.004(4) 0.002(4) C33 0.048(3) 0.067(4) 0.092(5) 0.012(4) 0.032(3) 0.021(3) C34 0.087(5) 0.038(3) 0.094(6) -0.005(4) 0.030(4) -0.019(3) C35 0.122(9) 0.100(8) 0.093(7) -0.021(6) 0.036(7) -0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C2 1.904(6) . ? Re1 C1 1.923(6) . ? Re1 C3 1.950(6) . ? Re1 N1 2.174(4) . ? Re1 N2 2.176(4) . ? Re1 P1 2.5164(13) . ? S1 O8 1.420(6) . ? S1 O9 1.422(6) . ? S1 O7 1.494(6) . ? S1 C35 1.787(12) . ? P1 C14 1.814(5) . ? P1 C20 1.820(5) . ? P1 C26 1.828(5) . ? F1 C35 1.318(12) . ? F2 C35 1.317(12) . ? F3 C35 1.374(13) . ? O1 C1 1.138(7) . ? O2 C2 1.161(6) . ? O3 C3 1.143(7) . ? O4 C17 1.384(6) . ? O4 C32 1.424(8) . ? O5 C23 1.359(6) . ? O5 C33 1.433(8) . ? O6 C29 1.366(7) . ? O6 C34 1.428(8) . ? N1 C4 1.345(7) . ? N1 C8 1.356(8) . ? N2 C13 1.350(7) . ? N2 C9 1.360(7) . ? C4 C5 1.381(9) . ? C4 H4 0.9300 . ? C5 C6 1.347(13) . ? C5 H5 0.9300 . ? C6 C7 1.375(12) . ? C6 H6 0.9300 . ? C7 C8 1.388(8) . ? C7 H7 0.9300 . ? C8 C9 1.467(9) . ? C9 C10 1.391(9) . ? C10 C11 1.390(12) . ? C10 H10 0.9300 . ? C11 C12 1.382(13) . ? C11 H11 0.9300 . ? C12 C13 1.364(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C19 1.405(7) . ? C14 C15 1.406(7) . ? C19 C18 1.378(7) . ? C19 H19 0.9300 . ? C18 C17 1.392(7) . ? C18 H18 0.9300 . ? C17 C16 1.378(8) . ? C16 C15 1.380(8) . ? C16 H16 0.9300 . ? C15 H15 0.9300 . ? C20 C25 1.381(7) . ? C20 C21 1.407(7) . ? C21 C22 1.378(8) . ? C21 H21 0.9300 . ? C22 C23 1.389(8) . ? C22 H22 0.9300 . ? C23 C24 1.385(7) . ? C24 C25 1.395(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C31 1.392(7) . ? C26 C27 1.398(7) . ? C27 C28 1.384(7) . ? C27 H27 0.9300 . ? C28 C29 1.365(8) . ? C28 H28 0.9300 . ? C29 C30 1.396(9) . ? C30 C31 1.368(8) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33C 0.9600 . ? C33 H33B 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C34 H34A 0.9600 . ? 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 C2 Re1 C1 89.0(3) . . ? C2 Re1 C3 88.5(2) . . ? C1 Re1 C3 87.0(2) . . ? C2 Re1 N1 174.5(2) . . ? C1 Re1 N1 96.5(2) . . ? C3 Re1 N1 92.1(2) . . ? C2 Re1 N2 99.5(2) . . ? C1 Re1 N2 171.4(2) . . ? C3 Re1 N2 94.65(19) . . ? N1 Re1 N2 74.98(18) . . ? C2 Re1 P1 90.46(17) . . ? C1 Re1 P1 89.88(16) . . ? C3 Re1 P1 176.72(16) . . ? N1 Re1 P1 89.27(12) . . ? N2 Re1 P1 88.58(12) . . ? O8 S1 O9 116.9(4) . . ? O8 S1 O7 115.1(4) . . ? O9 S1 O7 114.0(4) . . ? O8 S1 C35 104.4(5) . . ? O9 S1 C35 104.6(5) . . ? O7 S1 C35 98.8(6) . . ? C14 P1 C20 102.9(2) . . ? C14 P1 C26 109.3(2) . . ? C20 P1 C26 101.4(2) . . ? C14 P1 Re1 112.34(17) . . ? C20 P1 Re1 118.54(16) . . ? C26 P1 Re1 111.46(17) . . ? C17 O4 C32 118.0(5) . . ? C23 O5 C33 117.0(5) . . ? C29 O6 C34 116.9(6) . . ? C4 N1 C8 119.0(5) . . ? C4 N1 Re1 124.2(4) . . ? C8 N1 Re1 116.8(4) . . ? C13 N2 C9 118.4(5) . . ? C13 N2 Re1 125.3(4) . . ? C9 N2 Re1 116.1(4) . . ? O1 C1 Re1 177.9(5) . . ? O2 C2 Re1 179.2(5) . . ? O3 C3 Re1 173.2(5) . . ? N1 C4 C5 121.6(8) . . ? N1 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 119.4(8) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 120.1(7) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C8 119.1(8) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? N1 C8 C7 120.7(7) . . ? N1 C8 C9 115.5(5) . . ? C7 C8 C9 123.8(7) . . ? N2 C9 C10 120.8(7) . . ? N2 C9 C8 116.0(5) . . ? C10 C9 C8 123.2(6) . . ? C11 C10 C9 119.1(7) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C12 C11 C10 119.8(7) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 118.1(8) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? N2 C13 C12 123.6(7) . . ? N2 C13 H13 118.2 . . ? C12 C13 H13 118.2 . . ? C19 C14 C15 117.9(5) . . ? C19 C14 P1 121.8(4) . . ? C15 C14 P1 119.4(4) . . ? C18 C19 C14 120.6(5) . . ? C18 C19 H19 119.7 . . ? C14 C19 H19 119.7 . . ? C19 C18 C17 120.2(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C16 C17 O4 114.8(5) . . ? C16 C17 C18 120.4(5) . . ? O4 C17 C18 124.7(5) . . ? C17 C16 C15 119.7(5) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C15 C14 121.3(5) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C25 C20 C21 118.0(5) . . ? C25 C20 P1 122.9(4) . . ? C21 C20 P1 119.1(4) . . ? C22 C21 C20 120.4(5) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.6(5) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? O5 C23 C24 124.0(5) . . ? O5 C23 C22 116.0(5) . . ? C24 C23 C22 120.0(5) . . ? C23 C24 C25 118.8(5) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C20 C25 C24 122.1(5) . . ? C20 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C31 C26 C27 117.9(5) . . ? C31 C26 P1 126.5(4) . . ? C27 C26 P1 115.6(4) . . ? C28 C27 C26 121.8(5) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C29 C28 C27 119.5(5) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C28 C29 O6 125.2(6) . . ? C28 C29 C30 119.4(5) . . ? O6 C29 C30 115.4(6) . . ? C31 C30 C29 121.3(5) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C26 120.1(6) . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? O4 C32 H32A 109.5 . . ? O4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O5 C33 H33A 109.5 . . ? O5 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? O5 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? H33C C33 H33B 109.5 . . ? O6 C34 H34B 109.5 . . ? O6 C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O6 C34 H34A 109.5 . . ? H34B C34 H34A 109.5 . . ? H34C C34 H34A 109.5 . . ? F2 C35 F1 108.3(11) . . ? F2 C35 F3 107.2(10) . . ? F1 C35 F3 108.1(9) . . ? F2 C35 S1 112.5(8) . . ? F1 C35 S1 112.6(9) . . ? F3 C35 S1 107.9(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.331 _refine_diff_density_min -1.509 _refine_diff_density_rms 0.162 #===END data_4+cif _database_code_depnum_ccdc_archive 'CCDC 239867' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 4+ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H29 F3 N2 O6 P Re S' _chemical_formula_weight 879.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 21.205(2) _cell_length_b 11.0280(10) _cell_length_c 15.438(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.220(10) _cell_angle_gamma 90.00 _cell_volume 3466.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 31.42 _cell_measurement_theta_max 35.01 _exptl_crystal_description Cube _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 3.675 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5268 _exptl_absorpt_correction_T_max 0.7101 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science MXC18' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7 _diffrn_reflns_number 10791 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10109 _reflns_number_gt 7527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC(MAC Science)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_reduction Crystan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10109 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1953 _refine_ls_wR_factor_gt 0.1775 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.434716(12) 0.16171(2) 0.332160(16) 0.03932(10) Uani 1 1 d . . . S1 S 0.30298(15) 0.7553(3) 0.0708(3) 0.1025(11) Uani 1 1 d . . . P1 P 0.51646(8) 0.24418(13) 0.25782(10) 0.0369(3) Uani 1 1 d . . . F1 F 0.4170(5) 0.6625(7) 0.1356(7) 0.144(4) Uani 1 1 d . . . F2 F 0.3913(6) 0.6863(10) -0.0052(7) 0.149(4) Uani 1 1 d . . . F3 F 0.4167(5) 0.8394(7) 0.0819(7) 0.129(3) Uani 1 1 d . . . O1 O 0.4792(3) -0.0903(5) 0.2895(4) 0.0694(15) Uani 1 1 d . . . O2 O 0.5372(4) 0.1711(6) 0.5175(5) 0.081(2) Uani 1 1 d . . . O3 O 0.3439(3) 0.0223(6) 0.4226(5) 0.086(2) Uani 1 1 d . . . O9 O 0.2839(7) 0.8394(12) 0.0027(11) 0.214(9) Uani 1 1 d . . . O7 O 0.2769(6) 0.6350(10) 0.0560(10) 0.150(5) Uani 1 1 d . . . O8 O 0.3025(5) 0.7987(9) 0.1519(8) 0.122(4) Uani 1 1 d . . . N1 N 0.3559(3) 0.1891(6) 0.2083(5) 0.0531(14) Uani 1 1 d . . . N2 N 0.3964(3) 0.3414(5) 0.3426(5) 0.0502(14) Uani 1 1 d . . . C1 C 0.4632(3) 0.0026(6) 0.3059(5) 0.0470(14) Uani 1 1 d . . . C2 C 0.4990(4) 0.1627(6) 0.4444(5) 0.0524(17) Uani 1 1 d . . . C3 C 0.3753(3) 0.0778(7) 0.3895(6) 0.0542(17) Uani 1 1 d . . . C4 C 0.3338(4) 0.1031(9) 0.1440(6) 0.065(2) Uani 1 1 d . . . H4 H 0.3494 0.0242 0.1556 0.078 Uiso 1 1 calc R . . C5 C 0.2892(5) 0.1284(14) 0.0624(8) 0.095(4) Uani 1 1 d . . . H5 H 0.2764 0.0687 0.0184 0.114 Uiso 1 1 calc R . . C6 C 0.2641(6) 0.2427(13) 0.0475(8) 0.100(4) Uani 1 1 d . . . H6 H 0.2333 0.2608 -0.0068 0.121 Uiso 1 1 calc R . . C7 C 0.2836(5) 0.3303(10) 0.1110(9) 0.087(3) Uani 1 1 d . . . H7 H 0.2670 0.4086 0.1001 0.105 Uiso 1 1 calc R . . C8 C 0.3295(4) 0.3009(8) 0.1934(6) 0.0609(19) Uani 1 1 d . . . C9 C 0.3515(4) 0.3862(7) 0.2695(6) 0.0554(17) Uani 1 1 d . . . C10 C 0.3280(5) 0.5039(8) 0.2648(9) 0.080(3) Uani 1 1 d . . . H10 H 0.2981 0.5325 0.2127 0.097 Uiso 1 1 calc R . . C11 C 0.3496(6) 0.5769(10) 0.3381(10) 0.093(4) Uani 1 1 d . . . H11 H 0.3348 0.6565 0.3363 0.111 Uiso 1 1 calc R . . C12 C 0.3930(6) 0.5331(9) 0.4141(8) 0.089(4) Uani 1 1 d . . . H12 H 0.4073 0.5813 0.4653 0.107 Uiso 1 1 calc R . . C13 C 0.4158(5) 0.4136(7) 0.4136(6) 0.065(2) Uani 1 1 d . . . H13 H 0.4457 0.3839 0.4654 0.078 Uiso 1 1 calc R . . C14 C 0.4835(3) 0.2507(6) 0.1363(4) 0.0436(13) Uani 1 1 d . . . C15 C 0.4695(5) 0.3559(7) 0.0845(5) 0.0588(19) Uani 1 1 d . . . H15 H 0.4787 0.4313 0.1121 0.071 Uiso 1 1 calc R . . C16 C 0.4415(6) 0.3485(8) -0.0092(6) 0.073(3) Uani 1 1 d . . . H16 H 0.4330 0.4195 -0.0430 0.087 Uiso 1 1 calc R . . C17 C 0.4263(5) 0.2382(10) -0.0521(5) 0.073(2) Uani 1 1 d . . . C18 C 0.4413(5) 0.1339(8) -0.0023(5) 0.064(2) Uani 1 1 d . . . H18 H 0.4334 0.0589 -0.0307 0.077 Uiso 1 1 calc R . . C19 C 0.4681(5) 0.1403(6) 0.0903(5) 0.0571(19) Uani 1 1 d . . . H19 H 0.4763 0.0685 0.1232 0.069 Uiso 1 1 calc R . . C20 C 0.5487(3) 0.3944(5) 0.2962(4) 0.0399(12) Uani 1 1 d . . . C21 C 0.6142(3) 0.4127(6) 0.3414(5) 0.0495(15) Uani 1 1 d . . . H21 H 0.6431 0.3476 0.3498 0.059 Uiso 1 1 calc R . . C22 C 0.6375(4) 0.5258(7) 0.3744(5) 0.0536(16) Uani 1 1 d . . . H22 H 0.6819 0.5356 0.4038 0.064 Uiso 1 1 calc R . . C23 C 0.5960(4) 0.6237(6) 0.3644(4) 0.0480(15) Uani 1 1 d . . . C24 C 0.5310(4) 0.6068(6) 0.3205(5) 0.0500(15) Uani 1 1 d . . . H24 H 0.5024 0.6722 0.3137 0.060 Uiso 1 1 calc R . . C26 C 0.5912(3) 0.1558(5) 0.2724(4) 0.0392(12) Uani 1 1 d . . . C25 C 0.5063(3) 0.4942(6) 0.2855(5) 0.0472(14) Uani 1 1 d . . . H25 H 0.4620 0.4855 0.2552 0.057 Uiso 1 1 calc R . . C27 C 0.6248(5) 0.1592(7) 0.2080(6) 0.0579(19) Uani 1 1 d . . . H27 H 0.6074 0.2036 0.1556 0.069 Uiso 1 1 calc R . . C28 C 0.6839(4) 0.0987(9) 0.2183(6) 0.063(2) Uani 1 1 d . . . H28 H 0.7048 0.1005 0.1728 0.076 Uiso 1 1 calc R . . C29 C 0.7117(4) 0.0344(7) 0.2987(6) 0.0585(18) Uani 1 1 d . . . C30 C 0.6789(3) 0.0313(6) 0.3641(5) 0.0490(15) Uani 1 1 d . . . H30 H 0.6971 -0.0101 0.4178 0.059 Uiso 1 1 calc R . . C31 C 0.6192(3) 0.0893(6) 0.3506(4) 0.0453(13) Uani 1 1 d . . . H31 H 0.5971 0.0840 0.3947 0.054 Uiso 1 1 calc R . . C32 C 0.3963(7) 0.2332(14) -0.1541(6) 0.112(4) Uani 1 1 d . . . H32C H 0.4091 0.1590 -0.1771 0.169 Uiso 1 1 calc R . . H32A H 0.4117 0.3009 -0.1816 0.169 Uiso 1 1 calc R . . H32B H 0.3493 0.2365 -0.1678 0.169 Uiso 1 1 calc R . . C33 C 0.6211(5) 0.7459(7) 0.4001(6) 0.070(2) Uani 1 1 d . . . H33A H 0.5849 0.7971 0.4018 0.105 Uiso 1 1 calc R . . H33B H 0.6445 0.7816 0.3614 0.105 Uiso 1 1 calc R . . H33C H 0.6502 0.7375 0.4599 0.105 Uiso 1 1 calc R . . C34 C 0.7767(5) -0.0337(10) 0.3120(9) 0.093(3) Uani 1 1 d . . . H34A H 0.8119 0.0138 0.3490 0.140 Uiso 1 1 calc R . . H34B H 0.7844 -0.0476 0.2544 0.140 Uiso 1 1 calc R . . H34C H 0.7745 -0.1101 0.3408 0.140 Uiso 1 1 calc R . . C35 C 0.3849(6) 0.7382(11) 0.0719(7) 0.091(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 Re1 0.04360(16) 0.03228(14) 0.04294(16) 0.00415(9) 0.01354(10) 0.00212(9) S1 0.0784(17) 0.0772(19) 0.138(3) 0.0357(19) 0.0078(18) -0.0052(14) P1 0.0469(8) 0.0284(6) 0.0349(7) 0.0029(5) 0.0109(6) 0.0004(6) F1 0.156(8) 0.128(8) 0.127(7) 0.048(5) 0.005(6) 0.050(5) F2 0.201(10) 0.150(8) 0.102(6) -0.014(5) 0.051(6) -0.015(7) F3 0.117(6) 0.102(7) 0.155(8) -0.001(5) 0.017(6) -0.036(4) O1 0.085(4) 0.038(3) 0.085(4) 0.009(3) 0.024(3) 0.016(3) O2 0.086(5) 0.104(6) 0.048(3) 0.003(3) 0.010(3) 0.016(4) O3 0.083(4) 0.071(4) 0.121(6) 0.021(4) 0.056(4) -0.005(3) O9 0.150(11) 0.192(14) 0.233(16) 0.144(12) -0.059(10) -0.007(8) O7 0.115(8) 0.101(7) 0.200(12) 0.050(8) -0.013(8) -0.057(6) O8 0.171(9) 0.084(5) 0.154(9) 0.018(6) 0.115(8) 0.024(6) N1 0.052(3) 0.046(3) 0.064(4) -0.004(3) 0.019(3) 0.000(3) N2 0.061(4) 0.040(3) 0.055(3) 0.001(2) 0.026(3) 0.004(2) C1 0.055(4) 0.033(3) 0.053(4) 0.009(2) 0.015(3) 0.009(3) C2 0.056(4) 0.055(4) 0.048(4) 0.010(3) 0.016(3) 0.009(3) C3 0.046(3) 0.048(4) 0.076(5) 0.009(3) 0.029(3) -0.001(3) C4 0.064(5) 0.063(5) 0.062(5) -0.003(4) 0.007(4) 0.001(4) C5 0.075(7) 0.117(10) 0.075(7) -0.018(7) -0.007(5) 0.002(7) C6 0.086(7) 0.112(10) 0.077(7) 0.007(6) -0.021(5) 0.021(7) C7 0.069(6) 0.078(7) 0.099(8) 0.026(6) -0.002(6) 0.012(5) C8 0.043(4) 0.058(4) 0.080(5) 0.016(4) 0.015(3) 0.004(3) C9 0.058(4) 0.041(3) 0.072(5) 0.007(3) 0.026(4) 0.007(3) C10 0.062(5) 0.052(5) 0.132(9) 0.013(5) 0.034(5) 0.019(4) C11 0.109(8) 0.052(5) 0.137(11) 0.004(6) 0.065(8) 0.026(5) C12 0.136(10) 0.051(5) 0.106(8) -0.025(5) 0.078(8) -0.006(6) C13 0.101(6) 0.043(4) 0.063(5) 0.002(3) 0.045(5) 0.000(4) C14 0.055(4) 0.042(3) 0.034(3) 0.003(2) 0.013(2) 0.000(3) C15 0.082(6) 0.044(4) 0.045(4) 0.008(3) 0.009(4) -0.004(3) C16 0.104(8) 0.065(5) 0.042(4) 0.012(3) 0.007(4) -0.001(5) C17 0.087(6) 0.092(7) 0.035(3) 0.003(4) 0.007(4) -0.008(5) C18 0.091(6) 0.060(4) 0.040(4) -0.012(3) 0.015(4) -0.007(4) C19 0.094(6) 0.034(3) 0.041(3) 0.000(3) 0.014(4) -0.004(3) C20 0.049(3) 0.031(3) 0.037(3) 0.003(2) 0.009(2) 0.000(2) C21 0.053(4) 0.044(3) 0.049(4) -0.003(3) 0.011(3) -0.002(3) C22 0.053(4) 0.050(4) 0.048(4) -0.004(3) -0.003(3) -0.007(3) C23 0.066(4) 0.035(3) 0.041(3) 0.000(3) 0.012(3) -0.005(3) C24 0.059(4) 0.025(3) 0.065(4) 0.001(3) 0.016(3) 0.003(3) C26 0.044(3) 0.034(3) 0.039(3) 0.000(2) 0.010(2) -0.002(2) C25 0.050(3) 0.035(3) 0.055(4) 0.005(3) 0.012(3) -0.003(3) C27 0.067(5) 0.055(5) 0.056(4) 0.011(3) 0.025(4) 0.013(3) C28 0.062(5) 0.073(5) 0.064(5) -0.001(4) 0.035(4) 0.004(4) C29 0.053(4) 0.048(4) 0.081(5) 0.006(4) 0.030(4) 0.009(3) C30 0.047(3) 0.040(3) 0.058(4) 0.011(3) 0.012(3) 0.006(3) C31 0.053(3) 0.040(3) 0.045(3) 0.006(3) 0.017(3) 0.002(3) C32 0.155(12) 0.127(11) 0.038(4) 0.004(5) -0.002(6) -0.008(9) C33 0.102(7) 0.043(4) 0.060(5) -0.007(3) 0.015(4) -0.011(4) C34 0.083(7) 0.085(7) 0.120(9) 0.020(6) 0.042(6) 0.043(6) C35 0.128(10) 0.072(7) 0.058(5) 0.003(5) 0.001(6) -0.002(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 Re1 C2 1.883(8) . ? Re1 C1 1.935(6) . ? Re1 C3 1.962(7) . ? Re1 N2 2.165(5) . ? Re1 N1 2.180(7) . ? Re1 P1 2.5021(15) . ? S1 O8 1.342(10) . ? S1 O9 1.376(10) . ? S1 O7 1.432(10) . ? S1 C35 1.742(14) . ? P1 C14 1.811(6) . ? P1 C26 1.820(6) . ? P1 C20 1.827(6) . ? F1 C35 1.325(12) . ? F2 C35 1.362(14) . ? F3 C35 1.291(13) . ? O1 C1 1.130(8) . ? O2 C2 1.195(11) . ? O3 C3 1.126(8) . ? N1 C8 1.347(10) . ? N1 C4 1.358(11) . ? N2 C13 1.324(10) . ? N2 C9 1.352(10) . ? C4 C5 1.377(13) . ? C4 H4 0.9300 . ? C5 C6 1.362(18) . ? C5 H5 0.9300 . ? C6 C7 1.355(17) . ? C6 H6 0.9300 . ? C7 C8 1.407(13) . ? C7 H7 0.9300 . ? C8 C9 1.475(13) . ? C9 C10 1.385(11) . ? C10 C11 1.359(16) . ? C10 H10 0.9300 . ? C11 C12 1.363(16) . ? C11 H11 0.9300 . ? C12 C13 1.404(12) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.393(9) . ? C14 C19 1.401(9) . ? C15 C16 1.404(11) . ? C15 H15 0.9300 . ? C16 C17 1.379(13) . ? C16 H16 0.9300 . ? C17 C18 1.371(13) . ? C17 C32 1.526(11) . ? C18 C19 1.385(10) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.383(9) . ? C20 C25 1.401(9) . ? C21 C22 1.386(10) . ? C21 H21 0.9300 . ? C22 C23 1.374(10) . ? C22 H22 0.9300 . ? C23 C24 1.368(10) . ? C23 C33 1.497(10) . ? C24 C25 1.396(9) . ? C24 H24 0.9300 . ? C26 C27 1.376(10) . ? C26 C31 1.396(8) . ? C25 H25 0.9300 . ? C27 C28 1.388(12) . ? C27 H27 0.9300 . ? C28 C29 1.407(12) . ? C28 H28 0.9300 . ? C29 C30 1.378(10) . ? C29 C34 1.533(11) . ? C30 C31 1.381(9) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? 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 C2 Re1 C1 90.5(3) . . ? C2 Re1 C3 88.8(3) . . ? C1 Re1 C3 86.8(3) . . ? C2 Re1 N2 96.7(3) . . ? C1 Re1 N2 172.4(3) . . ? C3 Re1 N2 95.6(3) . . ? C2 Re1 N1 170.9(3) . . ? C1 Re1 N1 98.6(3) . . ? C3 Re1 N1 91.7(3) . . ? N2 Re1 N1 74.2(3) . . ? C2 Re1 P1 90.2(2) . . ? C1 Re1 P1 86.4(2) . . ? C3 Re1 P1 173.1(2) . . ? N2 Re1 P1 91.35(17) . . ? N1 Re1 P1 90.38(18) . . ? O8 S1 O9 113.4(10) . . ? O8 S1 O7 112.1(8) . . ? O9 S1 O7 119.0(9) . . ? O8 S1 C35 107.2(6) . . ? O9 S1 C35 99.2(8) . . ? O7 S1 C35 103.9(7) . . ? C14 P1 C26 102.7(3) . . ? C14 P1 C20 107.5(3) . . ? C26 P1 C20 102.2(3) . . ? C14 P1 Re1 111.9(2) . . ? C26 P1 Re1 116.1(2) . . ? C20 P1 Re1 115.2(2) . . ? C8 N1 C4 118.2(8) . . ? C8 N1 Re1 117.2(6) . . ? C4 N1 Re1 124.6(6) . . ? C13 N2 C9 117.1(7) . . ? C13 N2 Re1 125.2(6) . . ? C9 N2 Re1 117.6(5) . . ? O1 C1 Re1 179.0(7) . . ? O2 C2 Re1 174.7(7) . . ? O3 C3 Re1 175.0(7) . . ? N1 C4 C5 122.4(10) . . ? N1 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C6 C5 C4 118.5(11) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C7 C6 C5 120.8(10) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 119.0(10) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? N1 C8 C7 120.9(9) . . ? N1 C8 C9 115.1(7) . . ? C7 C8 C9 123.9(9) . . ? N2 C9 C10 123.0(9) . . ? N2 C9 C8 115.1(6) . . ? C10 C9 C8 121.9(9) . . ? C11 C10 C9 118.6(10) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C12 119.8(9) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 118.6(10) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? N2 C13 C12 122.8(9) . . ? N2 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C15 C14 C19 116.8(6) . . ? C15 C14 P1 125.9(6) . . ? C19 C14 P1 117.3(5) . . ? C14 C15 C16 120.3(7) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 121.4(8) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C18 C17 C16 119.0(7) . . ? C18 C17 C32 120.8(10) . . ? C16 C17 C32 120.1(9) . . ? C17 C18 C19 120.0(8) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C14 122.5(7) . . ? C18 C19 H19 118.7 . . ? C14 C19 H19 118.7 . . ? C21 C20 C25 117.7(6) . . ? C21 C20 P1 121.8(5) . . ? C25 C20 P1 120.3(5) . . ? C20 C21 C22 121.5(7) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C21 120.9(7) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 118.3(6) . . ? C24 C23 C33 120.8(7) . . ? C22 C23 C33 120.9(7) . . ? C23 C24 C25 122.0(6) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C27 C26 C31 117.3(6) . . ? C27 C26 P1 120.4(5) . . ? C31 C26 P1 122.2(5) . . ? C24 C25 C20 119.6(6) . . ? C24 C25 H25 120.2 . . ? C20 C25 H25 120.2 . . ? C26 C27 C28 122.5(7) . . ? C26 C27 H27 118.8 . . ? C28 C27 H27 118.8 . . ? C27 C28 C29 119.1(7) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C30 C29 C28 119.0(7) . . ? C30 C29 C34 120.6(8) . . ? C28 C29 C34 120.3(8) . . ? C29 C30 C31 120.5(7) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C26 121.6(6) . . ? C30 C31 H31 119.2 . . ? C26 C31 H31 119.2 . . ? C17 C32 H32C 109.5 . . ? C17 C32 H32A 109.5 . . ? H32C C32 H32A 109.5 . . ? C17 C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C23 C33 H33A 109.5 . . ? C23 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C23 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? F3 C35 F1 108.2(10) . . ? F3 C35 F2 106.9(11) . . ? F1 C35 F2 103.1(11) . . ? F3 C35 S1 113.2(9) . . ? F1 C35 S1 112.4(10) . . ? F2 C35 S1 112.3(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.107 _refine_diff_density_min -3.617 _refine_diff_density_rms 0.220 #===END data_5+cif _database_code_depnum_ccdc_archive 'CCDC 239868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 5+ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H23 F6 N2 O3 P2 Re' _chemical_formula_weight 833.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.129(3) _cell_length_b 22.200(7) _cell_length_c 10.614(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.390(10) _cell_angle_gamma 90.00 _cell_volume 3052.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 13.37 _cell_measurement_theta_max 14.95 _exptl_crystal_description Cube _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 4.159 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4901 _exptl_absorpt_correction_T_max 0.6811 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science MXC18' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 7529 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7009 _reflns_number_gt 4565 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC(MAC Science)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_reduction Crystan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0827P)^2^+40.3124P] 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 7009 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.2174 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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 Re1 Re 0.87937(3) 0.09326(2) 0.81848(4) 0.03939(17) Uani 1 1 d . . . P1 P 0.7109(2) 0.05193(13) 0.7066(3) 0.0383(6) Uani 1 1 d . . . P2 P 0.6633(3) 0.2403(2) 0.2040(3) 0.0607(9) Uani 1 1 d . . . F1 F 0.7728(9) 0.2252(7) 0.1708(11) 0.121(5) Uani 1 1 d . . . F2 F 0.6729(10) 0.1825(7) 0.2898(15) 0.138(6) Uani 1 1 d . . . F3 F 0.5552(10) 0.2528(8) 0.2363(13) 0.142(6) Uani 1 1 d . . . F4 F 0.6140(12) 0.2022(6) 0.0828(13) 0.131(5) Uani 1 1 d . . . F5 F 0.6547(12) 0.2954(7) 0.1147(15) 0.150(6) Uani 1 1 d . . . F6 F 0.7194(13) 0.2765(8) 0.3200(13) 0.162(7) Uani 1 1 d . . . O2 O 0.9659(10) -0.0361(5) 0.8341(11) 0.084(4) Uani 1 1 d . . . O1 O 0.8020(11) 0.0819(5) 1.0768(10) 0.084(4) Uani 1 1 d . . . O3 O 1.0876(11) 0.1348(7) 0.9707(13) 0.112(5) Uani 1 1 d . . . N2 N 0.9244(8) 0.1168(5) 0.6370(9) 0.050(2) Uani 1 1 d . . . N1 N 0.8237(7) 0.1854(4) 0.7782(8) 0.042(2) Uani 1 1 d . . . C2 C 0.9342(11) 0.0120(8) 0.8291(14) 0.066(4) Uani 1 1 d . . . C1 C 0.8290(12) 0.0871(6) 0.9798(14) 0.058(3) Uani 1 1 d . . . C3 C 1.0089(11) 0.1199(5) 0.9114(13) 0.057(4) Uani 1 1 d . . . C13 C 0.9825(11) 0.0834(6) 0.5753(13) 0.054(3) Uani 1 1 d . . . H13 H 1.0081 0.0474 0.6126 0.064 Uiso 1 1 calc R . . C12 C 1.0076(11) 0.0988(6) 0.4580(15) 0.061(4) Uani 1 1 d . . . H12 H 1.0529 0.0754 0.4200 0.073 Uiso 1 1 calc R . . C11 C 0.9644(12) 0.1485(7) 0.4007(13) 0.066(4) Uani 1 1 d . . . H11 H 0.9750 0.1576 0.3183 0.080 Uiso 1 1 calc R . . C10 C 0.9049(11) 0.1864(7) 0.4609(11) 0.057(3) Uani 1 1 d . . . H10 H 0.8766 0.2213 0.4214 0.068 Uiso 1 1 calc R . . C9 C 0.8880(9) 0.1706(5) 0.5846(9) 0.041(2) Uani 1 1 d . . . C8 C 0.8317(10) 0.2065(6) 0.6654(11) 0.050(3) Uani 1 1 d . . . C7 C 0.7939(12) 0.2656(6) 0.6278(13) 0.059(3) Uani 1 1 d . . . H7 H 0.8005 0.2815 0.5485 0.070 Uiso 1 1 calc R . . C6 C 0.7485(13) 0.2970(7) 0.7116(16) 0.072(4) Uani 1 1 d . . . H6 H 0.7215 0.3347 0.6874 0.087 Uiso 1 1 calc R . . C5 C 0.7402(12) 0.2761(6) 0.8307(15) 0.065(4) Uani 1 1 d . . . H5 H 0.7122 0.2993 0.8897 0.078 Uiso 1 1 calc R . . C4 C 0.7769(11) 0.2174(5) 0.8577(13) 0.052(3) Uani 1 1 d . . . H4 H 0.7680 0.2000 0.9349 0.062 Uiso 1 1 calc R . . C14 C 0.6141(9) 0.1114(6) 0.6623(11) 0.045(3) Uani 1 1 d . . . C15 C 0.5852(11) 0.1319(7) 0.5411(14) 0.062(4) Uani 1 1 d . . . H15 H 0.6067 0.1127 0.4721 0.075 Uiso 1 1 calc R . . C16 C 0.5196(14) 0.1846(11) 0.523(2) 0.103(7) Uani 1 1 d . . . H16 H 0.5048 0.2017 0.4425 0.123 Uiso 1 1 calc R . . C17 C 0.4795(12) 0.2096(7) 0.6180(19) 0.075(5) Uani 1 1 d . . . H17 H 0.4332 0.2415 0.6023 0.089 Uiso 1 1 calc R . . C18 C 0.5077(11) 0.1876(6) 0.7382(17) 0.069(4) Uani 1 1 d . . . H18 H 0.4810 0.2047 0.8059 0.083 Uiso 1 1 calc R . . C19 C 0.5776(12) 0.1385(6) 0.7606(14) 0.064(4) Uani 1 1 d . . . H19 H 0.5986 0.1248 0.8435 0.077 Uiso 1 1 calc R . . C26 C 0.6440(10) -0.0011(5) 0.7992(11) 0.045(3) Uani 1 1 d . . . C27 C 0.5388(10) -0.0109(6) 0.7658(14) 0.058(3) Uani 1 1 d . . . H27 H 0.5005 0.0108 0.6994 0.069 Uiso 1 1 calc R . . C28 C 0.4922(14) -0.0524(7) 0.8308(17) 0.076(5) Uani 1 1 d . . . H28 H 0.4210 -0.0572 0.8114 0.091 Uiso 1 1 calc R . . C29 C 0.5479(14) -0.0882(8) 0.9256(17) 0.083(6) Uani 1 1 d . . . H29 H 0.5163 -0.1189 0.9646 0.100 Uiso 1 1 calc R . . C30 C 0.6485(13) -0.0766(6) 0.9584(13) 0.064(4) Uani 1 1 d . . . H30 H 0.6847 -0.0979 1.0268 0.077 Uiso 1 1 calc R . . C31 C 0.7018(11) -0.0358(5) 0.8987(11) 0.050(3) Uani 1 1 d . . . H31 H 0.7728 -0.0309 0.9219 0.060 Uiso 1 1 calc R . . C20 C 0.7197(8) 0.0097(5) 0.5584(10) 0.040(2) Uani 1 1 d . . . C21 C 0.6984(11) -0.0514(6) 0.5523(12) 0.058(3) Uani 1 1 d . . . H21 H 0.6828 -0.0696 0.6257 0.070 Uiso 1 1 calc R . . C23 C 0.7420(12) -0.0574(6) 0.3437(14) 0.064(4) Uani 1 1 d . . . H23 H 0.7537 -0.0799 0.2736 0.077 Uiso 1 1 calc R . . C24 C 0.7655(11) 0.0028(9) 0.3492(12) 0.074(5) Uani 1 1 d . . . H24 H 0.7889 0.0210 0.2804 0.089 Uiso 1 1 calc R . . C25 C 0.7548(9) 0.0373(6) 0.4569(11) 0.046(3) Uani 1 1 d . . . H25 H 0.7710 0.0781 0.4599 0.056 Uiso 1 1 calc R . . C22 C 0.6983(17) -0.0871(5) 0.4481(16) 0.085(4) Uani 1 1 d . . . H22 H 0.6732 -0.1264 0.4429 0.102 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 Re1 0.0400(3) 0.0482(3) 0.0286(2) 0.00752(16) 0.00154(17) -0.00011(17) P1 0.0392(14) 0.0461(14) 0.0294(12) 0.0044(11) 0.0053(10) 0.0002(11) P2 0.058(2) 0.082(2) 0.0432(17) 0.0109(17) 0.0124(15) 0.0020(18) F1 0.075(7) 0.212(14) 0.084(8) -0.006(9) 0.035(6) 0.004(8) F2 0.098(9) 0.150(11) 0.178(14) 0.097(11) 0.061(9) 0.036(8) F3 0.094(9) 0.228(16) 0.112(10) 0.061(11) 0.041(8) 0.067(10) F4 0.147(12) 0.130(10) 0.106(10) -0.021(8) -0.008(8) -0.066(9) F5 0.146(12) 0.147(12) 0.142(12) 0.079(10) -0.017(10) -0.025(10) F6 0.175(15) 0.195(15) 0.097(10) -0.062(10) -0.037(10) 0.076(12) O2 0.111(10) 0.076(7) 0.068(7) 0.029(6) 0.019(6) 0.045(7) O1 0.123(11) 0.092(7) 0.042(5) 0.013(5) 0.032(6) 0.011(7) O3 0.090(9) 0.153(13) 0.076(8) 0.022(8) -0.035(7) -0.063(9) N2 0.041(5) 0.081(7) 0.028(4) 0.013(5) 0.006(4) -0.009(5) N1 0.044(5) 0.054(5) 0.030(4) -0.004(4) 0.009(4) -0.017(4) C2 0.054(8) 0.092(11) 0.049(8) 0.027(7) 0.003(6) -0.002(8) C1 0.069(9) 0.047(6) 0.053(8) 0.009(6) -0.001(7) -0.014(6) C3 0.061(8) 0.044(6) 0.058(8) 0.025(6) -0.016(6) -0.022(6) C13 0.056(7) 0.064(7) 0.043(7) 0.005(6) 0.015(6) -0.002(6) C12 0.056(8) 0.072(9) 0.062(9) -0.008(7) 0.031(7) 0.012(7) C11 0.071(9) 0.093(10) 0.043(7) -0.002(7) 0.030(7) 0.004(8) C10 0.068(8) 0.075(8) 0.027(5) 0.014(5) 0.009(5) -0.010(7) C9 0.047(6) 0.050(6) 0.024(5) 0.005(4) 0.002(4) -0.016(5) C8 0.050(7) 0.065(7) 0.032(5) 0.010(5) -0.002(5) -0.001(6) C7 0.077(9) 0.052(7) 0.047(7) 0.010(6) 0.010(7) 0.011(7) C6 0.084(11) 0.065(8) 0.067(10) 0.022(8) 0.008(8) 0.021(8) C5 0.074(10) 0.062(8) 0.059(8) -0.009(7) 0.014(7) 0.002(7) C4 0.070(8) 0.033(5) 0.058(7) 0.011(5) 0.027(6) -0.009(5) C14 0.039(6) 0.054(6) 0.043(6) 0.005(5) 0.005(5) 0.001(5) C15 0.063(8) 0.071(8) 0.054(8) 0.024(7) 0.015(6) 0.015(7) C16 0.071(11) 0.153(19) 0.086(13) 0.062(13) 0.018(10) 0.047(12) C17 0.060(9) 0.065(8) 0.100(13) 0.017(9) 0.017(9) 0.025(7) C18 0.057(8) 0.060(8) 0.093(12) -0.020(8) 0.020(8) 0.016(7) C19 0.077(10) 0.060(7) 0.055(8) -0.007(6) 0.010(7) 0.031(7) C26 0.070(8) 0.036(5) 0.036(5) 0.002(4) 0.028(5) 0.007(5) C27 0.045(7) 0.070(8) 0.060(8) 0.015(7) 0.012(6) 0.005(6) C28 0.071(10) 0.082(10) 0.084(11) 0.016(9) 0.042(9) -0.002(8) C29 0.084(11) 0.102(12) 0.074(11) 0.007(9) 0.045(9) -0.049(10) C30 0.105(12) 0.049(6) 0.045(7) 0.002(5) 0.028(7) -0.040(7) C31 0.067(8) 0.045(6) 0.041(6) 0.008(5) 0.012(6) -0.005(6) C20 0.033(5) 0.056(6) 0.033(5) 0.007(5) 0.012(4) -0.003(5) C21 0.068(9) 0.072(8) 0.038(6) 0.000(6) 0.021(6) -0.005(7) C23 0.080(10) 0.051(7) 0.060(9) -0.024(7) 0.003(7) 0.014(7) C24 0.058(8) 0.140(15) 0.027(6) -0.015(8) 0.016(5) 0.000(9) C25 0.047(6) 0.058(6) 0.034(5) 0.007(5) 0.009(5) -0.001(5) C22 0.162 0.013 0.070(9) -0.018(5) -0.014(10) 0.026(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 Re1 C3 1.915(12) . ? Re1 C1 1.939(15) . ? Re1 C2 1.939(17) . ? Re1 N2 2.169(9) . ? Re1 N1 2.191(10) . ? Re1 P1 2.508(3) . ? P1 C14 1.839(12) . ? P1 C26 1.844(11) . ? P1 C20 1.851(11) . ? P2 F3 1.539(12) . ? P2 F5 1.541(13) . ? P2 F6 1.553(14) . ? P2 F2 1.567(12) . ? P2 F1 1.570(11) . ? P2 F4 1.586(12) . ? O2 C2 1.143(19) . ? O1 C1 1.148(18) . ? O3 C3 1.167(16) . ? N2 C13 1.313(17) . ? N2 C9 1.369(16) . ? N1 C8 1.306(14) . ? N1 C4 1.327(15) . ? C13 C12 1.382(18) . ? C13 H13 0.9300 . ? C12 C11 1.34(2) . ? C12 H12 0.9300 . ? C11 C10 1.375(19) . ? C11 H11 0.9300 . ? C10 C9 1.411(14) . ? C10 H10 0.9300 . ? C9 C8 1.458(17) . ? C8 C7 1.435(17) . ? C7 C6 1.34(2) . ? C7 H7 0.9300 . ? C6 C5 1.37(2) . ? C6 H6 0.9300 . ? C5 C4 1.404(18) . ? C5 H5 0.9300 . ? C4 H4 0.9300 . ? C14 C19 1.358(17) . ? C14 C15 1.359(17) . ? C15 C16 1.45(2) . ? C15 H15 0.9300 . ? C16 C17 1.33(3) . ? C16 H16 0.9300 . ? C17 C18 1.36(2) . ? C17 H17 0.9300 . ? C18 C19 1.419(18) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C26 C27 1.386(18) . ? C26 C31 1.423(17) . ? C27 C28 1.356(19) . ? C27 H27 0.9300 . ? C28 C29 1.39(3) . ? C28 H28 0.9300 . ? C29 C30 1.33(2) . ? C29 H29 0.9300 . ? C30 C31 1.362(15) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C20 C25 1.382(15) . ? C20 C21 1.386(18) . ? C21 C22 1.360(18) . ? C21 H21 0.9300 . ? C23 C24 1.37(2) . ? C23 C22 1.48(2) . ? C23 H23 0.9300 . ? C24 C25 1.402(18) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C22 H22 0.9300 . ? 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 C3 Re1 C1 88.3(6) . . ? C3 Re1 C2 88.2(6) . . ? C1 Re1 C2 93.5(6) . . ? C3 Re1 N2 92.0(5) . . ? C1 Re1 N2 169.4(5) . . ? C2 Re1 N2 97.1(5) . . ? C3 Re1 N1 93.0(4) . . ? C1 Re1 N1 95.0(5) . . ? C2 Re1 N1 171.5(5) . . ? N2 Re1 N1 74.5(4) . . ? C3 Re1 P1 176.0(3) . . ? C1 Re1 P1 89.4(4) . . ? C2 Re1 P1 88.7(4) . . ? N2 Re1 P1 90.9(3) . . ? N1 Re1 P1 90.5(2) . . ? C14 P1 C26 103.0(5) . . ? C14 P1 C20 106.4(5) . . ? C26 P1 C20 103.4(5) . . ? C14 P1 Re1 112.2(4) . . ? C26 P1 Re1 116.2(4) . . ? C20 P1 Re1 114.5(3) . . ? F3 P2 F5 90.9(9) . . ? F3 P2 F6 93.7(9) . . ? F5 P2 F6 93.1(10) . . ? F3 P2 F2 90.4(7) . . ? F5 P2 F2 177.5(10) . . ? F6 P2 F2 88.9(10) . . ? F3 P2 F1 178.1(10) . . ? F5 P2 F1 90.5(9) . . ? F6 P2 F1 87.4(8) . . ? F2 P2 F1 88.1(7) . . ? F3 P2 F4 90.5(9) . . ? F5 P2 F4 86.9(9) . . ? F6 P2 F4 175.8(9) . . ? F2 P2 F4 91.0(9) . . ? F1 P2 F4 88.4(8) . . ? C13 N2 C9 118.8(10) . . ? C13 N2 Re1 124.8(9) . . ? C9 N2 Re1 116.3(8) . . ? C8 N1 C4 120.4(11) . . ? C8 N1 Re1 116.1(8) . . ? C4 N1 Re1 123.3(7) . . ? O2 C2 Re1 179.3(15) . . ? O1 C1 Re1 177.4(14) . . ? O3 C3 Re1 177.9(11) . . ? N2 C13 C12 123.6(13) . . ? N2 C13 H13 118.2 . . ? C12 C13 H13 118.2 . . ? C11 C12 C13 117.8(12) . . ? C11 C12 H12 121.1 . . ? C13 C12 H12 121.1 . . ? C12 C11 C10 121.6(12) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C10 C9 117.9(13) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? N2 C9 C10 119.9(12) . . ? N2 C9 C8 114.5(9) . . ? C10 C9 C8 125.6(11) . . ? N1 C8 C7 120.4(12) . . ? N1 C8 C9 117.9(11) . . ? C7 C8 C9 121.5(11) . . ? C6 C7 C8 117.4(13) . . ? C6 C7 H7 121.3 . . ? C8 C7 H7 121.3 . . ? C7 C6 C5 123.2(14) . . ? C7 C6 H6 118.4 . . ? C5 C6 H6 118.4 . . ? C6 C5 C4 115.2(14) . . ? C6 C5 H5 122.4 . . ? C4 C5 H5 122.4 . . ? N1 C4 C5 123.1(12) . . ? N1 C4 H4 118.5 . . ? C5 C4 H4 118.5 . . ? C19 C14 C15 120.0(13) . . ? C19 C14 P1 116.0(10) . . ? C15 C14 P1 123.9(10) . . ? C14 C15 C16 117.5(15) . . ? C14 C15 H15 121.2 . . ? C16 C15 H15 121.2 . . ? C17 C16 C15 122.7(16) . . ? C17 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? C16 C17 C18 118.5(14) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? C17 C18 C19 120.2(14) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C14 C19 C18 120.8(14) . . ? C14 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C27 C26 C31 119.6(11) . . ? C27 C26 P1 120.3(9) . . ? C31 C26 P1 119.9(10) . . ? C28 C27 C26 119.3(14) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 121.9(16) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C30 C29 C28 117.4(13) . . ? C30 C29 H29 121.3 . . ? C28 C29 H29 121.3 . . ? C29 C30 C31 124.7(16) . . ? C29 C30 H30 117.7 . . ? C31 C30 H30 117.7 . . ? C30 C31 C26 116.9(14) . . ? C30 C31 H31 121.5 . . ? C26 C31 H31 121.5 . . ? C25 C20 C21 119.2(11) . . ? C25 C20 P1 120.9(9) . . ? C21 C20 P1 119.7(8) . . ? C22 C21 C20 125.6(13) . . ? C22 C21 H21 117.2 . . ? C20 C21 H21 117.2 . . ? C24 C23 C22 120.9(12) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 121.1(14) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C20 C25 C24 119.0(13) . . ? C20 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C21 C22 C23 113.5(12) . . ? C21 C22 H22 123.3 . . ? C23 C22 H22 123.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.362 _refine_diff_density_min -3.002 _refine_diff_density_rms 0.292 #===END data_7+cif _database_code_depnum_ccdc_archive 'CCDC 239869' _audit_creation_method SHELXL-97 _publ_section_abstract ; We present the crystal and molecular structure of [Re(bpy)(CO)3{P(O-i-Pr)3}]PF6. ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. ; _chemical_name_systematic ; ? ; _chemical_name_common 7+ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H29 F6 N2 O6 P2 Re' _chemical_formula_weight 779.61 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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' _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 8.793(3) _cell_length_b 11.660(10) _cell_length_c 16.127(6) _cell_angle_alpha 99.49(6) _cell_angle_beta 102.22(3) _cell_angle_gamma 106.75(5) _cell_volume 1501.7(15) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 31.47 _cell_measurement_theta_max 35.05 _exptl_crystal_description Cube _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 4.227 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4180 _exptl_absorpt_correction_T_max 0.5697 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science MXC18' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7443 _diffrn_reflns_av_R_equivalents 0.1140 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6891 _reflns_number_gt 5452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC(MAC Science)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_reduction Crystan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1525P)^2^+3.2152P] 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 6891 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_ref 0.2296 _refine_ls_wR_factor_gt 0.1979 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.588(2) 0.1584(16) 0.6256(9) 0.103(4) Uani 1 1 d . . . C2 C 0.7953(19) 0.0721(15) 0.5520(10) 0.099(4) Uani 1 1 d . . . C3 C 0.612(2) -0.0721(15) 0.6370(8) 0.106(5) Uani 1 1 d . . . C4 C 0.6627(12) 0.1749(9) 0.8364(7) 0.068(2) Uani 1 1 d . . . H4 H 0.5769 0.1855 0.7970 0.082 Uiso 1 1 calc R . . C5 C 0.6719(14) 0.2035(10) 0.9227(8) 0.077(3) Uani 1 1 d . . . H5 H 0.5948 0.2330 0.9420 0.093 Uiso 1 1 calc R . . C6 C 0.7989(15) 0.1874(10) 0.9812(7) 0.077(3) Uani 1 1 d . . . H6 H 0.8070 0.2047 1.0407 0.092 Uiso 1 1 calc R . . C7 C 0.9130(13) 0.1461(9) 0.9515(6) 0.066(2) Uani 1 1 d . . . H7 H 1.0014 0.1376 0.9903 0.080 Uiso 1 1 calc R . . C8 C 0.8934(11) 0.1167(8) 0.8608(5) 0.0553(17) Uani 1 1 d . . . C9 C 1.0021(11) 0.0644(8) 0.8198(5) 0.0566(17) Uani 1 1 d . . . C10 C 1.1332(13) 0.0356(10) 0.8692(8) 0.071(2) Uani 1 1 d . . . H10 H 1.1540 0.0490 0.9297 0.085 Uiso 1 1 calc R . . C11 C 1.2291(16) -0.0123(11) 0.8269(10) 0.089(3) Uani 1 1 d . . . H11 H 1.3170 -0.0304 0.8585 0.107 Uiso 1 1 calc R . . C12 C 1.1952(17) -0.0329(12) 0.7394(11) 0.095(4) Uani 1 1 d . . . H12 H 1.2566 -0.0682 0.7096 0.114 Uiso 1 1 calc R . . C13 C 1.0674(16) -0.0008(12) 0.6942(8) 0.084(3) Uani 1 1 d . . . H13 H 1.0476 -0.0118 0.6340 0.101 Uiso 1 1 calc R . . C14 C 0.840(5) 0.487(3) 0.7387(14) 0.210(15) Uani 1 1 d . . . H14 H 0.7462 0.4212 0.7434 0.252 Uiso 1 1 calc R . . C15 C 0.750(6) 0.533(4) 0.676(2) 0.33(3) Uani 1 1 d . . . H15A H 0.6349 0.5025 0.6734 0.498 Uiso 1 1 calc R . . H15B H 0.7643 0.5048 0.6196 0.498 Uiso 1 1 calc R . . H15C H 0.7896 0.6211 0.6924 0.498 Uiso 1 1 calc R . . C16 C 0.882(4) 0.560(3) 0.823(2) 0.25(2) Uani 1 1 d . . . H16A H 0.9589 0.5346 0.8616 0.371 Uiso 1 1 calc R . . H16B H 0.7842 0.5495 0.8429 0.371 Uiso 1 1 calc R . . H16C H 0.9313 0.6447 0.8236 0.371 Uiso 1 1 calc R . . C17 C 1.2447(13) 0.4245(10) 0.8428(8) 0.084(3) Uani 1 1 d . . . H17 H 1.2562 0.4952 0.8162 0.101 Uiso 1 1 calc R . . C18 C 1.383(2) 0.3748(18) 0.8367(12) 0.115(5) Uani 1 1 d . . . H18A H 1.3760 0.3097 0.8667 0.172 Uiso 1 1 calc R . . H18B H 1.4871 0.4398 0.8632 0.172 Uiso 1 1 calc R . . H18C H 1.3743 0.3433 0.7764 0.172 Uiso 1 1 calc R . . C19 C 1.241(2) 0.4632(15) 0.9381(9) 0.113(5) Uani 1 1 d . . . H19C H 1.1456 0.4866 0.9393 0.169 Uiso 1 1 calc R . . H19B H 1.3391 0.5318 0.9695 0.169 Uiso 1 1 calc R . . H19A H 1.2373 0.3952 0.9650 0.169 Uiso 1 1 calc R . . C20 C 1.119(3) 0.375(2) 0.5841(15) 0.146(8) Uani 1 1 d . . . H20 H 1.0121 0.3802 0.5559 0.175 Uiso 1 1 calc R . . C21 C 1.232(5) 0.492(4) 0.601(2) 0.35(3) Uani 1 1 d . . . H21A H 1.2058 0.5477 0.6425 0.521 Uiso 1 1 calc R . . H21B H 1.2273 0.5195 0.5480 0.521 Uiso 1 1 calc R . . H21C H 1.3411 0.4912 0.6252 0.521 Uiso 1 1 calc R . . C22 C 1.157(5) 0.296(3) 0.5189(19) 0.24(2) Uani 1 1 d . . . H22A H 1.2745 0.3118 0.5334 0.362 Uiso 1 1 calc R . . H22B H 1.1214 0.3115 0.4627 0.362 Uiso 1 1 calc R . . H22C H 1.1017 0.2110 0.5171 0.362 Uiso 1 1 calc R . . N1 N 0.7704(9) 0.1322(7) 0.8048(5) 0.0582(15) Uani 1 1 d . . . N2 N 0.9714(12) 0.0455(8) 0.7337(6) 0.0685(19) Uani 1 1 d . . . O1 O 0.4807(15) 0.1902(14) 0.6013(10) 0.143(5) Uani 1 1 d . . . O2 O 0.8129(17) 0.0564(15) 0.4842(7) 0.138(5) Uani 1 1 d . . . O3 O 0.5223(18) -0.1663(12) 0.6123(8) 0.147(5) Uani 1 1 d . . . O4 O 0.9093(19) 0.4206(12) 0.7068(11) 0.173(7) Uani 1 1 d . . . O5 O 1.0850(11) 0.3281(8) 0.7980(6) 0.101(3) Uani 1 1 d . . . O6 O 1.1018(17) 0.3357(13) 0.6534(9) 0.144(5) Uani 1 1 d . . . P1 P 0.9692(3) 0.3082(2) 0.70623(18) 0.0654(5) Uani 1 1 d . . . P2 P 0.5599(3) -0.2130(2) 0.86878(19) 0.0692(6) Uani 1 1 d . . . F1 F 0.5318(14) -0.1293(9) 0.8028(6) 0.119(3) Uani 1 1 d . . . F2 F 0.5403(13) -0.3235(9) 0.7956(7) 0.129(3) Uani 1 1 d . . . F3 F 0.3658(11) -0.2628(8) 0.8578(8) 0.122(3) Uani 1 1 d . . . F4 F 0.7530(11) -0.1578(9) 0.8866(8) 0.135(4) Uani 1 1 d . . . F5 F 0.5707(13) -0.0996(7) 0.9444(6) 0.118(3) Uani 1 1 d . . . F6 F 0.5838(16) -0.2890(10) 0.9390(9) 0.152(4) Uani 1 1 d . . . Re1 Re 0.76902(4) 0.10038(3) 0.66738(2) 0.06614(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.101(10) 0.124(11) 0.073(7) 0.028(7) 0.016(7) 0.026(8) C2 0.090(9) 0.114(10) 0.081(8) 0.019(7) 0.020(7) 0.020(7) C3 0.119(11) 0.114(10) 0.058(6) 0.001(6) 0.025(7) 0.010(9) C4 0.060(5) 0.073(5) 0.070(5) 0.007(4) 0.025(4) 0.020(4) C5 0.075(6) 0.071(5) 0.092(7) 0.008(5) 0.043(6) 0.025(5) C6 0.090(7) 0.078(6) 0.068(5) 0.017(5) 0.040(5) 0.023(5) C7 0.073(6) 0.071(5) 0.051(4) 0.013(4) 0.019(4) 0.016(4) C8 0.057(4) 0.059(4) 0.050(4) 0.012(3) 0.020(3) 0.018(3) C9 0.059(4) 0.059(4) 0.056(4) 0.018(3) 0.023(4) 0.019(3) C10 0.065(5) 0.075(6) 0.082(6) 0.028(5) 0.021(5) 0.031(4) C11 0.078(7) 0.083(7) 0.125(10) 0.038(7) 0.038(7) 0.041(6) C12 0.088(8) 0.091(8) 0.126(11) 0.021(7) 0.053(8) 0.046(7) C13 0.086(7) 0.093(7) 0.083(7) 0.011(6) 0.041(6) 0.036(6) C14 0.38(4) 0.27(3) 0.123(15) 0.075(17) 0.12(2) 0.27(3) C15 0.57(8) 0.47(6) 0.31(4) 0.27(5) 0.29(5) 0.46(7) C16 0.17(3) 0.26(3) 0.23(3) -0.10(3) -0.06(2) 0.13(3) C17 0.060(6) 0.062(5) 0.098(8) 0.019(5) -0.007(5) -0.006(4) C18 0.097(10) 0.143(14) 0.114(11) 0.056(11) 0.020(8) 0.048(10) C19 0.121(12) 0.110(10) 0.071(7) 0.010(7) -0.001(7) 0.012(9) C20 0.18(2) 0.154(17) 0.137(16) 0.070(14) 0.091(16) 0.050(15) C21 0.34(5) 0.35(5) 0.20(3) 0.09(3) 0.11(3) -0.15(4) C22 0.36(5) 0.18(2) 0.16(2) 0.025(19) 0.17(3) 0.01(3) N1 0.056(4) 0.064(4) 0.051(3) 0.009(3) 0.022(3) 0.014(3) N2 0.074(5) 0.066(4) 0.069(5) 0.014(4) 0.028(4) 0.024(4) O1 0.088(7) 0.169(11) 0.155(11) 0.032(9) -0.022(7) 0.061(8) O2 0.127(10) 0.194(13) 0.079(6) 0.005(7) 0.046(6) 0.035(9) O3 0.137(10) 0.126(9) 0.095(7) -0.012(6) 0.003(7) -0.037(8) O4 0.157(12) 0.112(8) 0.203(15) -0.036(8) -0.046(10) 0.084(9) O5 0.085(5) 0.083(5) 0.101(6) 0.043(5) -0.013(5) -0.005(4) O6 0.132(10) 0.166(11) 0.124(9) 0.057(8) 0.060(8) 0.005(8) P1 0.0596(12) 0.0707(13) 0.0690(13) 0.0216(11) 0.0198(11) 0.0224(11) P2 0.0678(14) 0.0598(12) 0.0830(16) 0.0205(11) 0.0235(12) 0.0218(11) F1 0.145(8) 0.134(7) 0.109(6) 0.059(6) 0.047(6) 0.070(6) F2 0.121(7) 0.110(6) 0.144(8) -0.023(5) 0.049(6) 0.042(5) F3 0.081(5) 0.092(5) 0.188(10) 0.014(5) 0.054(6) 0.021(4) F4 0.078(5) 0.115(6) 0.212(11) 0.038(7) 0.042(6) 0.030(5) F5 0.133(7) 0.090(5) 0.114(6) -0.009(4) 0.027(5) 0.035(5) F6 0.161(10) 0.133(8) 0.181(11) 0.092(8) 0.038(8) 0.054(7) Re1 0.0572(2) 0.0787(3) 0.0538(2) 0.00692(17) 0.01446(16) 0.01550(18) _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 C1 O1 1.13(2) . ? C1 Re1 1.941(18) . ? C2 O2 1.130(17) . ? C2 Re1 1.909(15) . ? C3 O3 1.101(18) . ? C3 Re1 1.994(16) . ? C4 N1 1.340(12) . ? C4 C5 1.357(15) . ? C4 H4 0.9300 . ? C5 C6 1.379(17) . ? C5 H5 0.9300 . ? C6 C7 1.369(15) . ? C6 H6 0.9300 . ? C7 C8 1.407(12) . ? C7 H7 0.9300 . ? C8 N1 1.331(12) . ? C8 C9 1.482(12) . ? C9 N2 1.324(12) . ? C9 C10 1.414(13) . ? C10 C11 1.370(16) . ? C10 H10 0.9300 . ? C11 C12 1.34(2) . ? C11 H11 0.9300 . ? C12 C13 1.39(2) . ? C12 H12 0.9300 . ? C13 N2 1.337(14) . ? C13 H13 0.9300 . ? C14 O4 1.23(2) . ? C14 C16 1.39(3) . ? C14 C15 1.42(4) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O5 1.467(11) . ? C17 C18 1.50(2) . ? C17 C19 1.537(19) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19C 0.9600 . ? C19 H19B 0.9600 . ? C19 H19A 0.9600 . ? C20 O6 1.30(2) . ? C20 C21 1.38(4) . ? C20 C22 1.44(3) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? N1 Re1 2.182(7) . ? N2 Re1 2.190(10) . ? O4 P1 1.547(11) . ? O5 P1 1.548(9) . ? O6 P1 1.575(12) . ? P1 Re1 2.437(4) . ? P2 F2 1.539(8) . ? P2 F6 1.566(10) . ? P2 F4 1.575(9) . ? P2 F1 1.586(8) . ? P2 F3 1.597(9) . ? P2 F5 1.611(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 O1 C1 Re1 178.8(16) . . ? O2 C2 Re1 179.1(16) . . ? O3 C3 Re1 173.3(13) . . ? N1 C4 C5 123.6(10) . . ? N1 C4 H4 118.2 . . ? C5 C4 H4 118.2 . . ? C4 C5 C6 118.2(9) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? C7 C6 C5 119.9(9) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 118.4(10) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? N1 C8 C7 121.3(8) . . ? N1 C8 C9 114.7(7) . . ? C7 C8 C9 123.9(8) . . ? N2 C9 C10 120.9(9) . . ? N2 C9 C8 116.8(8) . . ? C10 C9 C8 122.2(8) . . ? C11 C10 C9 119.0(11) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C12 C11 C10 119.6(12) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 119.0(11) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? N2 C13 C12 122.7(12) . . ? N2 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? O4 C14 C16 130(3) . . ? O4 C14 C15 113(2) . . ? C16 C14 C15 112(2) . . ? O4 C14 H14 97.2 . . ? C16 C14 H14 97.2 . . ? C15 C14 H14 97.2 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 C18 110.0(12) . . ? O5 C17 C19 105.8(11) . . ? C18 C17 C19 111.7(12) . . ? O5 C17 H17 109.8 . . ? C18 C17 H17 109.8 . . ? C19 C17 H17 109.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19C 109.5 . . ? C17 C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? C17 C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? O6 C20 C21 114(2) . . ? O6 C20 C22 116(2) . . ? C21 C20 C22 108(3) . . ? O6 C20 H20 105.9 . . ? C21 C20 H20 105.9 . . ? C22 C20 H20 105.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C8 N1 C4 118.5(8) . . ? C8 N1 Re1 117.4(6) . . ? C4 N1 Re1 123.9(7) . . ? C9 N2 C13 118.7(10) . . ? C9 N2 Re1 116.3(6) . . ? C13 N2 Re1 124.9(8) . . ? C14 O4 P1 149(2) . . ? C17 O5 P1 129.3(7) . . ? C20 O6 P1 138.8(17) . . ? O4 P1 O5 107.7(7) . . ? O4 P1 O6 102.0(10) . . ? O5 P1 O6 99.4(7) . . ? O4 P1 Re1 120.0(6) . . ? O5 P1 Re1 107.8(3) . . ? O6 P1 Re1 117.8(6) . . ? F2 P2 F6 90.9(7) . . ? F2 P2 F4 94.2(6) . . ? F6 P2 F4 89.8(7) . . ? F2 P2 F1 93.3(6) . . ? F6 P2 F1 175.6(7) . . ? F4 P2 F1 91.5(6) . . ? F2 P2 F3 89.9(5) . . ? F6 P2 F3 88.8(7) . . ? F4 P2 F3 175.7(6) . . ? F1 P2 F3 89.6(6) . . ? F2 P2 F5 177.2(6) . . ? F6 P2 F5 89.4(7) . . ? F4 P2 F5 88.6(6) . . ? F1 P2 F5 86.4(5) . . ? F3 P2 F5 87.3(5) . . ? C2 Re1 C1 89.3(7) . . ? C2 Re1 C3 88.5(6) . . ? C1 Re1 C3 90.3(8) . . ? C2 Re1 N1 172.8(5) . . ? C1 Re1 N1 97.5(5) . . ? C3 Re1 N1 93.8(4) . . ? C2 Re1 N2 98.9(5) . . ? C1 Re1 N2 171.6(5) . . ? C3 Re1 N2 91.5(6) . . ? N1 Re1 N2 74.2(3) . . ? C2 Re1 P1 91.4(5) . . ? C1 Re1 P1 91.9(5) . . ? C3 Re1 P1 177.8(6) . . ? N1 Re1 P1 86.1(2) . . ? N2 Re1 P1 86.4(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.201 _refine_diff_density_min -3.900 _refine_diff_density_rms 0.218 #===END data_8+cif _database_code_depnum_ccdc_archive 'CCDC 239870' _audit_creation_method SHELXL-97 _publ_section_abstract ; We present the crystal and molecular structure of [Re(bpy)(CO)3{P(OEt)3}]PF6. ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. ; _chemical_name_systematic ; ? ; _chemical_name_common 8+ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H23 F6 N2 O6 P2 Re' _chemical_formula_weight 737.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 9.931(3) _cell_length_b 11.158(2) _cell_length_c 12.489(4) _cell_angle_alpha 93.04(2) _cell_angle_beta 97.23(2) _cell_angle_gamma 104.04(2) _cell_volume 1326.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 26.86 _cell_measurement_theta_max 30.08 _exptl_crystal_description Cube _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 4.778 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4483 _exptl_absorpt_correction_T_max 0.6466 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science MXC18' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 20 _diffrn_reflns_number 6572 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6098 _reflns_number_gt 5245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC(MAC Science)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_reduction Crystan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1069P)^2^+1.5274P] 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 6098 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1783 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_restrained_S_all 1.176 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re -0.11845(3) 0.17841(2) 0.18927(2) 0.06175(15) Uani 1 1 d . . . P1 P -0.1562(3) 0.2212(2) 0.37412(18) 0.0692(5) Uani 1 1 d . . . P2 P 0.3946(3) 0.6675(3) 0.2102(2) 0.0828(6) Uani 1 1 d . . . F1 F 0.2697(10) 0.6172(10) 0.2765(7) 0.140(4) Uani 1 1 d . . . F2 F 0.5186(12) 0.7157(13) 0.1427(9) 0.158(4) Uani 1 1 d . . . F3 F 0.3538(15) 0.5377(10) 0.1399(8) 0.145(4) Uani 1 1 d . . . F4 F 0.2980(11) 0.7139(10) 0.1218(7) 0.140(3) Uani 1 1 d . . . F5 F 0.4325(12) 0.7963(9) 0.2791(8) 0.148(4) Uani 1 1 d . . . F6 F 0.4953(12) 0.6205(12) 0.2946(9) 0.168(4) Uani 1 1 d . . . O1 O 0.1974(8) 0.2565(11) 0.2640(9) 0.125(3) Uani 1 1 d . . . O2 O -0.1209(11) -0.0926(7) 0.2286(9) 0.117(3) Uani 1 1 d . . . O3 O -0.0630(10) 0.1220(8) -0.0445(7) 0.102(2) Uani 1 1 d . . . O4 O -0.2735(11) 0.2876(11) 0.3764(6) 0.126(4) Uani 1 1 d . . . O5 O -0.0258(13) 0.3164(13) 0.4425(8) 0.151(4) Uani 1 1 d . . . O6 O -0.180(2) 0.1178(11) 0.4496(10) 0.178(7) Uani 1 1 d . . . N1 N -0.1456(8) 0.3613(6) 0.1572(5) 0.0649(15) Uani 1 1 d . . . N2 N -0.3468(7) 0.1528(7) 0.1483(5) 0.0639(15) Uani 1 1 d . . . C1 C 0.0818(13) 0.2281(12) 0.2352(10) 0.093(3) Uani 1 1 d . . . C2 C -0.1185(12) 0.0085(10) 0.2138(10) 0.086(3) Uani 1 1 d . . . C3 C -0.0857(11) 0.1447(9) 0.0400(8) 0.076(2) Uani 1 1 d . . . C4 C -0.0399(11) 0.4633(9) 0.1605(9) 0.082(2) Uani 1 1 d . . . H4 H 0.0519 0.4564 0.1759 0.098 Uiso 1 1 calc R . . C5 C -0.0633(14) 0.5788(10) 0.1417(10) 0.090(3) Uani 1 1 d . . . H5 H 0.0115 0.6482 0.1439 0.108 Uiso 1 1 calc R . . C6 C -0.1965(13) 0.5882(9) 0.1202(8) 0.088(3) Uani 1 1 d . . . H6 H -0.2139 0.6652 0.1092 0.106 Uiso 1 1 calc R . . C7 C -0.3058(11) 0.4865(9) 0.1142(7) 0.081(2) Uani 1 1 d . . . H7 H -0.3977 0.4927 0.0974 0.097 Uiso 1 1 calc R . . C8 C -0.2774(8) 0.3727(7) 0.1340(6) 0.0613(15) Uani 1 1 d . . . C9 C -0.3895(9) 0.2554(8) 0.1277(6) 0.0651(17) Uani 1 1 d . . . C10 C -0.5322(10) 0.2473(10) 0.1058(8) 0.083(2) Uani 1 1 d . . . H10 H -0.5633 0.3178 0.0918 0.099 Uiso 1 1 calc R . . C11 C -0.6257(11) 0.1368(13) 0.1050(10) 0.098(3) Uani 1 1 d . . . H11 H -0.7212 0.1314 0.0902 0.117 Uiso 1 1 calc R . . C12 C -0.5815(10) 0.0351(11) 0.1253(9) 0.087(3) Uani 1 1 d . . . H12 H -0.6465 -0.0405 0.1256 0.105 Uiso 1 1 calc R . . C13 C -0.4389(11) 0.0421(10) 0.1461(8) 0.081(2) Uani 1 1 d . . . H13 H -0.4076 -0.0288 0.1582 0.097 Uiso 1 1 calc R . . C14 C -0.3326(15) 0.3284(14) 0.4666(9) 0.106(4) Uani 1 1 d . . . H14A H -0.2696 0.4027 0.5052 0.127 Uiso 1 1 calc R . . H14B H -0.3490 0.2644 0.5165 0.127 Uiso 1 1 calc R . . C15 C -0.4677(15) 0.3545(16) 0.4209(12) 0.122(5) Uani 1 1 d . . . H15A H -0.4501 0.4167 0.3706 0.182 Uiso 1 1 calc R . . H15B H -0.5103 0.3836 0.4785 0.182 Uiso 1 1 calc R . . H15C H -0.5295 0.2799 0.3841 0.182 Uiso 1 1 calc R . . C16 C 0.031(3) 0.334(2) 0.5511(17) 0.210(12) Uani 1 1 d . . . H16A H 0.0236 0.4156 0.5775 0.251 Uiso 1 1 calc R . . H16B H -0.0299 0.2743 0.5883 0.251 Uiso 1 1 calc R . . C17 C 0.157(2) 0.329(2) 0.5836(16) 0.189(10) Uani 1 1 d . . . H17A H 0.1612 0.2437 0.5803 0.284 Uiso 1 1 calc R . . H17B H 0.1847 0.3651 0.6569 0.284 Uiso 1 1 calc R . . H17C H 0.2188 0.3735 0.5379 0.284 Uiso 1 1 calc R . . C18 C -0.268(3) 0.0119(18) 0.453(2) 0.174(9) Uani 1 1 d . . . H18B H -0.2360 -0.0525 0.4163 0.209 Uiso 1 1 calc R . . H18A H -0.3588 0.0135 0.4147 0.209 Uiso 1 1 calc R . . C19 C -0.283(3) -0.018(2) 0.563(2) 0.227(15) Uani 1 1 d . . . H19A H -0.1973 -0.0314 0.5983 0.340 Uiso 1 1 calc R . . H19B H -0.3577 -0.0912 0.5623 0.340 Uiso 1 1 calc R . . H19C H -0.3052 0.0500 0.6023 0.340 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 Re1 0.0671(2) 0.0600(2) 0.0630(2) 0.00539(14) 0.01613(14) 0.02193(14) P1 0.0773(12) 0.0755(13) 0.0583(10) 0.0068(9) 0.0102(9) 0.0254(10) P2 0.0928(16) 0.0883(16) 0.0691(12) 0.0079(11) 0.0130(11) 0.0250(13) F1 0.115(6) 0.184(9) 0.102(5) -0.006(6) 0.036(4) -0.008(6) F2 0.138(7) 0.225(12) 0.136(8) 0.053(8) 0.067(6) 0.058(8) F3 0.223(11) 0.110(6) 0.108(6) -0.009(5) 0.023(6) 0.058(7) F4 0.171(8) 0.176(9) 0.093(5) 0.013(5) -0.003(5) 0.092(7) F5 0.165(9) 0.123(7) 0.136(7) -0.025(6) 0.024(6) 0.006(6) F6 0.159(9) 0.193(10) 0.141(8) 0.067(7) -0.030(6) 0.041(7) O1 0.064(4) 0.175(10) 0.137(8) 0.028(7) 0.008(4) 0.034(5) O2 0.152(8) 0.065(4) 0.159(8) 0.028(5) 0.062(7) 0.047(5) O3 0.123(6) 0.108(6) 0.085(5) 0.004(4) 0.042(4) 0.037(5) O4 0.153(8) 0.202(10) 0.066(4) 0.014(5) 0.029(4) 0.122(8) O5 0.139(9) 0.195(12) 0.090(6) -0.025(7) 0.002(6) 0.003(8) O6 0.34(2) 0.104(7) 0.123(8) 0.050(6) 0.119(11) 0.068(10) N1 0.083(4) 0.060(3) 0.056(3) 0.006(3) 0.014(3) 0.023(3) N2 0.069(4) 0.067(4) 0.052(3) -0.001(3) 0.009(3) 0.012(3) C1 0.092(7) 0.094(7) 0.094(7) 0.011(5) 0.001(5) 0.034(6) C2 0.090(6) 0.073(6) 0.103(7) 0.009(5) 0.025(5) 0.029(5) C3 0.084(5) 0.074(5) 0.074(5) 0.005(4) 0.023(4) 0.024(4) C4 0.088(6) 0.066(5) 0.089(6) 0.004(4) 0.020(5) 0.013(4) C5 0.109(8) 0.066(5) 0.096(7) 0.011(5) 0.016(6) 0.020(5) C6 0.119(8) 0.070(5) 0.082(6) 0.001(4) 0.003(5) 0.043(5) C7 0.096(6) 0.080(5) 0.067(5) 0.002(4) 0.001(4) 0.030(5) C8 0.072(4) 0.064(4) 0.050(3) 0.000(3) 0.006(3) 0.024(3) C9 0.076(4) 0.071(4) 0.052(3) 0.001(3) 0.012(3) 0.025(4) C10 0.079(5) 0.098(7) 0.076(5) -0.004(5) 0.006(4) 0.035(5) C11 0.071(5) 0.122(9) 0.100(7) -0.008(6) 0.020(5) 0.026(6) C12 0.071(5) 0.096(7) 0.083(6) -0.003(5) 0.005(4) 0.005(5) C13 0.088(6) 0.079(5) 0.069(5) 0.005(4) 0.018(4) 0.008(4) C14 0.132(10) 0.131(10) 0.077(6) 0.003(6) 0.041(6) 0.063(8) C15 0.107(9) 0.150(13) 0.122(10) -0.013(9) 0.032(8) 0.056(9) C16 0.23(2) 0.21(2) 0.143(16) -0.004(15) -0.091(17) 0.015(18) C17 0.164(18) 0.24(3) 0.125(14) 0.013(14) -0.052(13) 0.009(16) C18 0.183(19) 0.126(14) 0.21(2) 0.038(15) 0.087(18) 0.007(13) C19 0.36(4) 0.19(2) 0.19(2) 0.105(19) 0.16(3) 0.09(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 Re1 C1 1.932(12) . ? Re1 C2 1.936(11) . ? Re1 C3 1.965(9) . ? Re1 N1 2.173(7) . ? Re1 N2 2.206(7) . ? Re1 P1 2.426(2) . ? P1 O6 1.522(10) . ? P1 O4 1.527(8) . ? P1 O5 1.578(11) . ? P2 F6 1.560(9) . ? P2 F4 1.563(8) . ? P2 F5 1.573(10) . ? P2 F2 1.583(10) . ? P2 F1 1.584(8) . ? P2 F3 1.588(10) . ? O1 C1 1.121(14) . ? O2 C2 1.149(13) . ? O3 C3 1.135(11) . ? O4 C14 1.437(12) . ? O5 C16 1.39(2) . ? O6 C18 1.29(2) . ? N1 C4 1.343(12) . ? N1 C8 1.343(11) . ? N2 C9 1.340(11) . ? N2 C13 1.343(12) . ? C4 C5 1.392(15) . ? C4 H4 0.9300 . ? C5 C6 1.347(17) . ? C5 H5 0.9300 . ? C6 C7 1.358(15) . ? C6 H6 0.9300 . ? C7 C8 1.394(12) . ? C7 H7 0.9300 . ? C8 C9 1.489(12) . ? C9 C10 1.388(12) . ? C10 C11 1.350(16) . ? C10 H10 0.9300 . ? C11 C12 1.338(17) . ? C11 H11 0.9300 . ? C12 C13 1.390(15) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.491(18) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.28(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.45(3) . ? C18 H18B 0.9700 . ? C18 H18A 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 C2 89.8(5) . . ? C1 Re1 C3 89.8(5) . . ? C2 Re1 C3 88.5(5) . . ? C1 Re1 N1 97.0(4) . . ? C2 Re1 N1 173.1(4) . . ? C3 Re1 N1 92.0(3) . . ? C1 Re1 N2 170.5(4) . . ? C2 Re1 N2 98.3(4) . . ? C3 Re1 N2 95.4(3) . . ? N1 Re1 N2 74.8(3) . . ? C1 Re1 P1 89.6(4) . . ? C2 Re1 P1 91.6(4) . . ? C3 Re1 P1 179.4(3) . . ? N1 Re1 P1 87.96(18) . . ? N2 Re1 P1 85.16(18) . . ? O6 P1 O4 108.3(8) . . ? O6 P1 O5 100.4(9) . . ? O4 P1 O5 103.1(7) . . ? O6 P1 Re1 120.4(5) . . ? O4 P1 Re1 110.6(3) . . ? O5 P1 Re1 112.3(4) . . ? F6 P2 F4 177.5(6) . . ? F6 P2 F5 89.6(7) . . ? F4 P2 F5 91.4(6) . . ? F6 P2 F2 90.6(7) . . ? F4 P2 F2 87.2(6) . . ? F5 P2 F2 90.5(7) . . ? F6 P2 F1 89.5(6) . . ? F4 P2 F1 92.7(6) . . ? F5 P2 F1 90.4(6) . . ? F2 P2 F1 179.1(6) . . ? F6 P2 F3 91.2(7) . . ? F4 P2 F3 87.7(6) . . ? F5 P2 F3 179.0(6) . . ? F2 P2 F3 90.0(7) . . ? F1 P2 F3 89.1(6) . . ? C14 O4 P1 130.0(8) . . ? C16 O5 P1 134.3(15) . . ? C18 O6 P1 138.1(19) . . ? C4 N1 C8 118.2(8) . . ? C4 N1 Re1 124.5(7) . . ? C8 N1 Re1 117.4(6) . . ? C9 N2 C13 121.4(8) . . ? C9 N2 Re1 115.9(5) . . ? C13 N2 Re1 122.6(7) . . ? O1 C1 Re1 178.6(12) . . ? O2 C2 Re1 178.8(10) . . ? O3 C3 Re1 176.9(9) . . ? N1 C4 C5 122.1(10) . . ? N1 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 118.6(11) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C7 120.8(10) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C8 118.6(9) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? N1 C8 C7 121.7(8) . . ? N1 C8 C9 115.5(7) . . ? C7 C8 C9 122.8(8) . . ? N2 C9 C10 119.1(8) . . ? N2 C9 C8 116.3(7) . . ? C10 C9 C8 124.5(8) . . ? C11 C10 C9 119.9(10) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 120.3(10) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.2(10) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? N2 C13 C12 119.0(10) . . ? N2 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? O4 C14 C15 106.5(10) . . ? O4 C14 H14A 110.4 . . ? C15 C14 H14A 110.4 . . ? O4 C14 H14B 110.4 . . ? C15 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 O5 122(3) . . ? C17 C16 H16A 106.8 . . ? O5 C16 H16A 106.8 . . ? C17 C16 H16B 106.8 . . ? O5 C16 H16B 106.8 . . ? H16A C16 H16B 106.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O6 C18 C19 112(2) . . ? O6 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? O6 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? H18B C18 H18A 107.9 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.609 _refine_diff_density_min -2.824 _refine_diff_density_rms 0.217 #===END data_9+cif _database_code_depnum_ccdc_archive 'CCDC 239871' _audit_creation_method SHELXL-97 _publ_section_abstract ; We present the crystal and molecular structure of [Re(bpy)(CO)3{P(OMe)3}]CF3SO3. ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. ; _chemical_name_systematic ; ? ; _chemical_name_common 9+ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H17 F3 N2 O9 P Re S' _chemical_formula_weight 699.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.574(2) _cell_length_b 12.052(2) _cell_length_c 14.391(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.790(10) _cell_angle_gamma 90.00 _cell_volume 2346.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 31.59 _cell_measurement_theta_max 35.05 _exptl_crystal_description Cube _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 5.411 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.2936 _exptl_absorpt_correction_T_max 0.6137 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science MXC18' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6 _diffrn_reflns_number 3665 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3552 _reflns_number_gt 3237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC(MAC Science)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_reduction Crystan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0696P)^2^+6.8418P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.018(15) _refine_ls_number_reflns 3552 _refine_ls_number_parameters 310 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.238 _refine_ls_restrained_S_all 1.238 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.75098(4) -0.48352(3) 0.81198(4) 0.04467(14) Uani 1 1 d . . . S1 S 0.2497(5) -0.5228(4) 0.9150(4) 0.0773(12) Uani 1 1 d . . . P1 P 0.8577(2) -0.5633(3) 0.7022(2) 0.0459(6) Uani 1 1 d . . . N1 N 0.6339(8) -0.5826(10) 0.7434(7) 0.052(2) Uani 1 1 d . . . N2 N 0.6901(7) -0.3804(10) 0.6972(6) 0.047(2) Uani 1 1 d . . . O1 O 0.8192(10) -0.6507(13) 0.9646(9) 0.089(4) Uani 1 1 d . . . O2 O 0.9163(8) -0.3290(10) 0.8914(8) 0.070(3) Uani 1 1 d . . . O3 O 0.6078(10) -0.3784(15) 0.9438(9) 0.090(4) Uani 1 1 d . . . O4 O 0.8031(9) -0.6201(9) 0.6126(8) 0.068(3) Uani 1 1 d . . . O5 O 0.9201(8) -0.4694(8) 0.6587(8) 0.058(2) Uani 1 1 d . . . O6 O 0.9322(8) -0.6588(9) 0.7352(8) 0.069(3) Uani 1 1 d . . . O7 O 0.2313(15) -0.6345(12) 0.8860(13) 0.112(6) Uani 1 1 d . . . O8 O 0.1667(16) -0.449(2) 0.896(2) 0.158(12) Uani 1 1 d . . . O9 O 0.309(2) -0.5062(16) 0.9997(17) 0.128(9) Uani 1 1 d . . . F1 F 0.347(3) -0.3691(19) 0.841(2) 0.231(14) Uani 1 1 d . . . F2 F 0.414(3) -0.532(3) 0.840(3) 0.217(16) Uani 1 1 d . . . F3 F 0.273(6) -0.487(3) 0.7477(16) 0.31(3) Uani 1 1 d . . . C1 C 0.7971(12) -0.5909(14) 0.9089(10) 0.064(4) Uani 1 1 d . . . C2 C 0.8536(9) -0.3870(11) 0.8613(8) 0.051(3) Uani 1 1 d . . . C3 C 0.6597(11) -0.4177(14) 0.8962(9) 0.059(3) Uani 1 1 d . . . C4 C 0.6107(15) -0.6859(17) 0.7675(10) 0.079(5) Uani 1 1 d . . . H4 H 0.6477 -0.7188 0.8173 0.095 Uiso 1 1 calc R . . C5 C 0.5357(16) -0.746(2) 0.7230(14) 0.092(7) Uani 1 1 d . . . H5 H 0.5225 -0.8175 0.7419 0.111 Uiso 1 1 calc R . . C6 C 0.4806(13) -0.699(2) 0.6508(15) 0.095(8) Uani 1 1 d . . . H6 H 0.4278 -0.7374 0.6210 0.114 Uiso 1 1 calc R . . C7 C 0.5026(11) -0.5917(19) 0.6209(12) 0.075(5) Uani 1 1 d . . . H7 H 0.4671 -0.5595 0.5698 0.090 Uiso 1 1 calc R . . C8 C 0.5798(11) -0.5350(15) 0.6703(10) 0.061(4) Uani 1 1 d . . . C9 C 0.6120(9) -0.4237(13) 0.6442(9) 0.055(3) Uani 1 1 d . . . C10 C 0.5690(12) -0.3627(15) 0.5672(10) 0.068(4) Uani 1 1 d . . . H10 H 0.5153 -0.3913 0.5305 0.082 Uiso 1 1 calc R . . C11 C 0.6068(14) -0.2619(18) 0.5473(11) 0.081(6) Uani 1 1 d . . . H11 H 0.5799 -0.2230 0.4953 0.097 Uiso 1 1 calc R . . C12 C 0.6853(13) -0.2153(14) 0.6034(11) 0.068(4) Uani 1 1 d . . . H12 H 0.7103 -0.1454 0.5910 0.081 Uiso 1 1 calc R . . C13 C 0.7235(9) -0.2774(11) 0.6773(9) 0.052(3) Uani 1 1 d . . . H13 H 0.7751 -0.2476 0.7161 0.062 Uiso 1 1 calc R . . C14 C 0.7940(16) -0.7367(13) 0.5958(13) 0.080(5) Uani 1 1 d . . . H14C H 0.8575 -0.7713 0.6076 0.120 Uiso 1 1 calc R . . H14B H 0.7696 -0.7491 0.5321 0.120 Uiso 1 1 calc R . . H14A H 0.7487 -0.7679 0.6364 0.120 Uiso 1 1 calc R . . C15 C 0.9916(14) -0.4947(16) 0.5926(17) 0.076(5) Uani 1 1 d . . . H15C H 1.0538 -0.5130 0.6256 0.113 Uiso 1 1 calc R . . H15A H 0.9997 -0.4313 0.5536 0.113 Uiso 1 1 calc R . . H15B H 0.9686 -0.5565 0.5547 0.113 Uiso 1 1 calc R . . C16 C 1.0080(14) -0.641(2) 0.8099(14) 0.091(6) Uani 1 1 d . . . H16A H 1.0394 -0.5706 0.8013 0.136 Uiso 1 1 calc R . . H16B H 1.0563 -0.6990 0.8098 0.136 Uiso 1 1 calc R . . H16C H 0.9789 -0.6408 0.8685 0.136 Uiso 1 1 calc R . . C17 C 0.323(4) -0.472(3) 0.828(3) 0.135(14) 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 Re1 0.0446(2) 0.0527(2) 0.03590(18) 0.0004(4) -0.00129(13) -0.0090(3) S1 0.085(3) 0.082(3) 0.062(3) -0.005(2) -0.010(2) -0.012(2) P1 0.0433(13) 0.0456(14) 0.0472(14) -0.0042(12) -0.0056(11) -0.0007(11) N1 0.055(6) 0.060(6) 0.040(5) -0.011(4) 0.006(4) -0.021(5) N2 0.038(4) 0.068(6) 0.033(4) 0.002(4) -0.002(3) 0.002(4) O1 0.106(10) 0.099(10) 0.059(6) 0.031(7) -0.008(6) -0.020(8) O2 0.066(6) 0.076(7) 0.065(6) -0.008(5) -0.008(5) -0.021(5) O3 0.081(7) 0.128(13) 0.067(7) -0.004(8) 0.035(6) -0.001(8) O4 0.083(7) 0.055(5) 0.063(6) -0.016(5) -0.019(5) 0.004(5) O5 0.056(5) 0.056(5) 0.062(6) -0.008(4) 0.011(4) -0.003(4) O6 0.069(6) 0.059(5) 0.074(6) -0.004(5) -0.018(5) 0.018(5) O7 0.147(15) 0.065(7) 0.117(13) 0.004(8) -0.032(11) -0.022(9) O8 0.101(14) 0.125(17) 0.24(3) -0.06(2) -0.031(17) 0.021(13) O9 0.16(2) 0.136(17) 0.082(13) -0.003(10) -0.050(14) -0.016(12) F1 0.36(4) 0.116(15) 0.23(3) 0.022(18) 0.08(3) -0.10(2) F2 0.16(2) 0.28(4) 0.23(4) -0.06(3) 0.10(2) -0.02(2) F3 0.64(10) 0.24(4) 0.041(10) -0.003(11) -0.01(3) -0.14(4) C1 0.066(8) 0.074(9) 0.049(6) 0.024(6) -0.003(6) -0.004(7) C2 0.056(6) 0.059(7) 0.036(5) 0.009(5) -0.002(4) 0.000(5) C3 0.067(8) 0.069(8) 0.042(6) -0.007(5) 0.014(5) -0.022(6) C4 0.103(12) 0.090(12) 0.046(7) -0.006(7) 0.012(7) -0.043(10) C5 0.089(12) 0.109(15) 0.082(12) -0.019(11) 0.022(10) -0.054(12) C6 0.063(9) 0.122(16) 0.105(14) -0.065(13) 0.034(9) -0.053(10) C7 0.046(6) 0.117(14) 0.063(8) -0.025(9) 0.006(6) -0.016(8) C8 0.047(6) 0.093(10) 0.044(6) -0.020(7) 0.014(5) -0.010(6) C9 0.044(5) 0.070(8) 0.049(6) -0.008(6) 0.000(5) 0.008(5) C10 0.072(9) 0.081(10) 0.047(6) -0.008(7) -0.013(6) 0.023(8) C11 0.093(11) 0.102(13) 0.047(7) 0.009(8) -0.001(7) 0.054(11) C12 0.086(10) 0.060(8) 0.059(7) 0.009(6) 0.014(7) 0.029(7) C13 0.047(5) 0.057(7) 0.052(6) 0.003(5) 0.006(5) 0.005(5) C14 0.107(14) 0.053(8) 0.077(11) -0.009(7) -0.013(9) -0.014(8) C15 0.057(9) 0.091(12) 0.082(13) -0.015(9) 0.019(9) 0.003(8) C16 0.066(9) 0.124(17) 0.076(11) 0.012(11) -0.026(8) 0.018(10) C17 0.20(4) 0.13(3) 0.08(2) -0.007(16) 0.02(2) -0.02(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 Re1 C2 1.906(13) . ? Re1 C1 1.966(13) . ? Re1 C3 1.971(14) . ? Re1 N1 2.159(9) . ? Re1 N2 2.174(10) . ? Re1 P1 2.429(3) . ? P1 O5 1.575(11) . ? P1 O6 1.579(10) . ? P1 O4 1.589(10) . ? S1 O9 1.42(2) . ? S1 O7 1.425(15) . ? S1 O8 1.45(2) . ? S1 C17 1.78(4) . ? O2 C2 1.157(16) . ? N2 C9 1.357(16) . ? N2 C13 1.361(18) . ? O6 C16 1.442(19) . ? N1 C4 1.34(2) . ? N1 C8 1.36(2) . ? C8 C7 1.39(2) . ? C8 C9 1.47(2) . ? O3 C3 1.128(19) . ? C13 C12 1.367(19) . ? C13 H13 0.9300 . ? C9 C10 1.41(2) . ? C1 O1 1.101(17) . ? C4 C5 1.36(2) . ? C4 H4 0.9300 . ? C7 C6 1.40(3) . ? C7 H7 0.9300 . ? C10 C11 1.36(3) . ? C10 H10 0.9300 . ? C5 C6 1.35(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C14 O4 1.429(18) . ? C14 H14C 0.9600 . ? C14 H14B 0.9600 . ? C14 H14A 0.9600 . ? O5 C15 1.45(2) . ? C11 C12 1.40(3) . ? C11 H11 0.9300 . ? C15 H15C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C12 H12 0.9300 . ? F1 C17 1.29(4) . ? F2 C17 1.42(6) . ? F3 C17 1.30(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 C2 Re1 C1 87.6(6) . . ? C2 Re1 C3 90.1(6) . . ? C1 Re1 C3 90.4(7) . . ? C2 Re1 N1 174.2(5) . . ? C1 Re1 N1 98.0(6) . . ? C3 Re1 N1 91.6(5) . . ? C2 Re1 N2 98.9(4) . . ? C1 Re1 N2 173.4(6) . . ? C3 Re1 N2 91.1(5) . . ? N1 Re1 N2 75.5(4) . . ? C2 Re1 P1 91.5(4) . . ? C1 Re1 P1 91.7(5) . . ? C3 Re1 P1 177.4(4) . . ? N1 Re1 P1 86.6(3) . . ? N2 Re1 P1 86.7(3) . . ? O5 P1 O6 106.9(6) . . ? O5 P1 O4 102.5(7) . . ? O6 P1 O4 100.0(6) . . ? O5 P1 Re1 110.1(4) . . ? O6 P1 Re1 119.7(5) . . ? O4 P1 Re1 115.8(5) . . ? O9 S1 O7 117.3(11) . . ? O9 S1 O8 117.0(16) . . ? O7 S1 O8 114.4(12) . . ? O9 S1 C17 104.2(19) . . ? O7 S1 C17 102.3(15) . . ? O8 S1 C17 97(2) . . ? C9 N2 C13 119.4(11) . . ? C9 N2 Re1 115.9(9) . . ? C13 N2 Re1 124.7(8) . . ? O2 C2 Re1 179.6(12) . . ? C16 O6 P1 120.9(13) . . ? C4 N1 C8 118.0(13) . . ? C4 N1 Re1 125.2(11) . . ? C8 N1 Re1 116.8(9) . . ? N1 C8 C7 121.5(17) . . ? N1 C8 C9 115.5(11) . . ? C7 C8 C9 122.9(16) . . ? N2 C13 C12 123.5(14) . . ? N2 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? N2 C9 C10 119.5(14) . . ? N2 C9 C8 116.2(12) . . ? C10 C9 C8 124.3(13) . . ? O1 C1 Re1 177.1(16) . . ? O3 C3 Re1 178.8(16) . . ? N1 C4 C5 124(2) . . ? N1 C4 H4 118.2 . . ? C5 C4 H4 118.2 . . ? C8 C7 C6 117.8(19) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C11 C10 C9 119.5(15) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C6 C5 C4 119(2) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 120.2(15) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? O4 C14 H14C 109.5 . . ? O4 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? O4 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C15 O5 P1 121.5(10) . . ? C10 C11 C12 121.3(14) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? O5 C15 H15C 109.5 . . ? O5 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? O5 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 O4 P1 126.1(11) . . ? C13 C12 C11 116.8(16) . . ? C13 C12 H12 121.6 . . ? C11 C12 H12 121.6 . . ? O6 C16 H16A 109.5 . . ? O6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? F1 C17 F3 111(4) . . ? F1 C17 F2 106(4) . . ? F3 C17 F2 115(5) . . ? F1 C17 S1 112(3) . . ? F3 C17 S1 107(4) . . ? F2 C17 S1 105(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.100 _refine_diff_density_min -1.993 _refine_diff_density_rms 0.522 #===END data_10+cif _database_code_depnum_ccdc_archive 'CCDC 239872' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 10+ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H23 F6 N2 O6 P2 Re' _chemical_formula_weight 881.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.880(3) _cell_length_b 10.972(4) _cell_length_c 15.286(5) _cell_angle_alpha 71.11(2) _cell_angle_beta 76.66(3) _cell_angle_gamma 77.73(3) _cell_volume 1661.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 15.84 _cell_measurement_theta_max 17.49 _exptl_crystal_description Cube _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 3.833 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6159 _exptl_absorpt_correction_T_max 0.8026 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science MXC18' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 9 _diffrn_reflns_number 8263 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _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 1.95 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7613 _reflns_number_gt 6043 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC(MAC Science)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_reduction Crystan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0702P)^2^+8.4454P] 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 7613 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1583 _refine_ls_wR_factor_gt 0.1361 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Re1 Re 0.36927(3) 0.42314(3) 0.86436(2) 0.04470(12) Uani 1 1 d . . . P1 P 0.3678(2) 0.5228(2) 0.69922(15) 0.0481(5) Uani 1 1 d . . . P2 P -0.0720(3) 0.9164(3) 0.8385(2) 0.0729(7) Uani 1 1 d . . . F1 F 0.0183(14) 1.0046(15) 0.7667(7) 0.197(7) Uani 1 1 d . . . F2 F -0.1753(13) 0.8408(15) 0.9108(7) 0.180(6) Uani 1 1 d . . . F3 F -0.1547(17) 1.0358(18) 0.848(2) 0.309(13) Uani 1 1 d . . . F4 F -0.0119(17) 0.9314(15) 0.9134(8) 0.207(8) Uani 1 1 d . . . F5 F -0.130(2) 0.904(2) 0.7661(8) 0.302(14) Uani 1 1 d . . . F6 F 0.009(2) 0.7929(17) 0.847(2) 0.356(16) Uani 1 1 d . . . O1 O 0.6542(7) 0.4289(9) 0.8498(7) 0.092(3) Uani 1 1 d . . . O2 O 0.3029(9) 0.6976(8) 0.8866(7) 0.099(3) Uani 1 1 d . . . O3 O 0.3714(9) 0.3251(8) 1.0783(6) 0.088(2) Uani 1 1 d . . . O5 O 0.2260(6) 0.5865(7) 0.6823(4) 0.0592(15) Uani 1 1 d . . . O6 O 0.4371(6) 0.6483(6) 0.6489(4) 0.0573(14) Uani 1 1 d . . . O4 O 0.4261(6) 0.4459(6) 0.6219(5) 0.0613(15) Uani 1 1 d . . . N1 N 0.3921(6) 0.2247(7) 0.8619(5) 0.0497(15) Uani 1 1 d . . . N2 N 0.1782(6) 0.3815(6) 0.8784(5) 0.0478(15) Uani 1 1 d . . . C1 C 0.5473(12) 0.4352(10) 0.8497(8) 0.075(3) Uani 1 1 d . . . C2 C 0.3290(9) 0.5931(9) 0.8766(7) 0.058(2) Uani 1 1 d . . . C3 C 0.3657(10) 0.3572(9) 1.0005(7) 0.059(2) Uani 1 1 d . . . C4 C 0.5078(10) 0.1434(10) 0.8548(7) 0.065(2) Uani 1 1 d . . . H4 H 0.5829 0.1782 0.8426 0.078 Uiso 1 1 calc R . . C5 C 0.5154(11) 0.0118(11) 0.8654(10) 0.084(3) Uani 1 1 d . . . H5 H 0.5941 -0.0415 0.8614 0.101 Uiso 1 1 calc R . . C6 C 0.4061(12) -0.0367(11) 0.8817(11) 0.090(4) Uani 1 1 d . . . H6 H 0.4098 -0.1251 0.8899 0.108 Uiso 1 1 calc R . . C7 C 0.2901(11) 0.0402(10) 0.8864(8) 0.072(3) Uani 1 1 d . . . H7 H 0.2156 0.0053 0.8961 0.087 Uiso 1 1 calc R . . C8 C 0.2846(8) 0.1713(8) 0.8766(6) 0.0509(18) Uani 1 1 d . . . C9 C 0.1652(8) 0.2631(8) 0.8799(6) 0.0529(19) Uani 1 1 d . . . C10 C 0.0489(10) 0.2306(12) 0.8829(8) 0.075(3) Uani 1 1 d . . . H10 H 0.0426 0.1464 0.8850 0.089 Uiso 1 1 calc R . . C11 C -0.0559(10) 0.3214(13) 0.8828(10) 0.086(4) Uani 1 1 d . . . H11 H -0.1344 0.2995 0.8839 0.103 Uiso 1 1 calc R . . C12 C -0.0495(10) 0.4464(13) 0.8811(8) 0.080(3) Uani 1 1 d . . . H12 H -0.1216 0.5095 0.8810 0.097 Uiso 1 1 calc R . . C13 C 0.0721(9) 0.4734(12) 0.8794(7) 0.070(3) Uani 1 1 d . . . H13 H 0.0802 0.5563 0.8790 0.084 Uiso 1 1 calc R . . C20 C 0.1941(8) 0.6811(11) 0.6002(6) 0.064(3) Uani 1 1 d . . . C25 C 0.1703(11) 0.6416(14) 0.5293(9) 0.087(4) Uani 1 1 d . . . H25 H 0.1766 0.5537 0.5346 0.104 Uiso 1 1 calc R . . C24 C 0.1369(15) 0.738(2) 0.4502(10) 0.116(6) Uani 1 1 d . . . H24 H 0.1204 0.7142 0.4012 0.139 Uiso 1 1 calc R . . C23 C 0.1280(17) 0.865(2) 0.4438(11) 0.135(8) Uani 1 1 d . . . H23 H 0.1055 0.9285 0.3902 0.162 Uiso 1 1 calc R . . C22 C 0.1513(15) 0.9022(15) 0.5144(13) 0.120(6) Uani 1 1 d . . . H22 H 0.1439 0.9903 0.5088 0.144 Uiso 1 1 calc R . . C21 C 0.1859(12) 0.8101(11) 0.5941(9) 0.082(3) Uani 1 1 d . . . H21 H 0.2033 0.8346 0.6423 0.098 Uiso 1 1 calc R . . C26 C 0.5617(9) 0.6591(10) 0.6521(6) 0.056(2) Uani 1 1 d . . . C27 C 0.5752(13) 0.7549(12) 0.6866(8) 0.081(3) Uani 1 1 d . . . H27 H 0.5042 0.8065 0.7103 0.097 Uiso 1 1 calc R . . C28 C 0.6990(15) 0.7732(15) 0.6854(10) 0.099(4) Uani 1 1 d . . . H28 H 0.7094 0.8378 0.7091 0.119 Uiso 1 1 calc R . . C29 C 0.8037(15) 0.7006(18) 0.6512(9) 0.104(5) Uani 1 1 d . . . H29 H 0.8850 0.7147 0.6511 0.125 Uiso 1 1 calc R . . C30 C 0.7876(13) 0.6032(18) 0.6156(11) 0.111(5) Uani 1 1 d . . . H30 H 0.8586 0.5514 0.5922 0.133 Uiso 1 1 calc R . . C31 C 0.6645(10) 0.5843(12) 0.6155(8) 0.077(3) Uani 1 1 d . . . H31 H 0.6530 0.5213 0.5907 0.093 Uiso 1 1 calc R . . C14 C 0.3971(10) 0.3271(9) 0.6239(6) 0.060(2) Uani 1 1 d . . . C19 C 0.5014(13) 0.2426(11) 0.5945(9) 0.082(3) Uani 1 1 d . . . H19 H 0.5840 0.2624 0.5804 0.099 Uiso 1 1 calc R . . C18 C 0.4769(18) 0.1263(13) 0.5870(10) 0.105(5) Uani 1 1 d . . . H18 H 0.5435 0.0686 0.5653 0.126 Uiso 1 1 calc R . . C17 C 0.355(2) 0.0978(15) 0.6116(10) 0.114(6) Uani 1 1 d . . . H17 H 0.3397 0.0200 0.6069 0.137 Uiso 1 1 calc R . . C16 C 0.2543(17) 0.1807(15) 0.6428(9) 0.104(5) Uani 1 1 d . . . H16 H 0.1723 0.1590 0.6598 0.125 Uiso 1 1 calc R . . C15 C 0.2758(11) 0.2964(12) 0.6488(8) 0.074(3) Uani 1 1 d . . . H15 H 0.2081 0.3537 0.6698 0.089 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 Re1 0.04046(18) 0.04303(18) 0.0537(2) -0.01408(13) -0.01234(13) -0.00817(12) P1 0.0418(10) 0.0503(11) 0.0530(11) -0.0133(9) -0.0080(8) -0.0116(8) P2 0.0783(18) 0.0825(19) 0.0669(15) -0.0177(14) -0.0138(13) -0.0363(15) F1 0.231(14) 0.289(16) 0.114(7) -0.041(9) 0.019(8) -0.206(13) F2 0.202(12) 0.263(15) 0.094(6) -0.007(8) -0.011(7) -0.165(12) F3 0.168(15) 0.186(16) 0.57(4) -0.17(2) -0.03(2) 0.031(12) F4 0.311(19) 0.226(14) 0.124(8) 0.026(8) -0.094(10) -0.186(15) F5 0.49(3) 0.40(3) 0.103(7) 0.031(11) -0.107(12) -0.37(3) F6 0.24(2) 0.149(14) 0.65(5) -0.17(2) -0.04(3) 0.061(13) O1 0.043(4) 0.102(6) 0.135(7) -0.027(5) -0.035(4) -0.012(4) O2 0.101(7) 0.068(5) 0.142(8) -0.047(5) -0.021(6) -0.017(4) O3 0.108(7) 0.087(6) 0.072(5) -0.022(4) -0.028(4) -0.013(5) O5 0.045(3) 0.073(4) 0.054(3) -0.010(3) -0.009(3) -0.011(3) O6 0.055(3) 0.046(3) 0.067(4) -0.007(3) -0.011(3) -0.015(3) O4 0.061(4) 0.063(4) 0.064(4) -0.027(3) 0.001(3) -0.019(3) N1 0.043(3) 0.055(4) 0.052(4) -0.016(3) -0.008(3) -0.010(3) N2 0.038(3) 0.043(3) 0.060(4) -0.014(3) -0.005(3) -0.004(3) C1 0.091(8) 0.060(6) 0.073(7) -0.003(5) -0.033(6) -0.018(5) C2 0.056(5) 0.046(4) 0.074(6) -0.017(4) -0.015(4) -0.007(4) C3 0.068(6) 0.054(5) 0.059(5) -0.017(4) -0.026(4) -0.003(4) C4 0.063(6) 0.059(5) 0.078(6) -0.021(5) -0.017(5) -0.012(4) C5 0.069(7) 0.058(6) 0.127(10) -0.041(6) -0.016(7) 0.010(5) C6 0.082(8) 0.057(6) 0.139(12) -0.040(7) -0.022(8) -0.006(5) C7 0.073(7) 0.060(6) 0.097(8) -0.028(5) -0.025(6) -0.016(5) C8 0.055(5) 0.054(5) 0.047(4) -0.012(3) -0.012(3) -0.016(4) C9 0.051(5) 0.048(4) 0.064(5) -0.015(4) -0.012(4) -0.018(4) C10 0.052(5) 0.078(7) 0.093(8) -0.015(6) -0.019(5) -0.017(5) C11 0.044(5) 0.086(8) 0.128(11) -0.027(7) -0.019(6) -0.013(5) C12 0.042(5) 0.107(9) 0.080(7) -0.020(6) -0.016(5) 0.011(5) C13 0.044(5) 0.091(7) 0.069(6) -0.022(5) -0.002(4) -0.010(5) C20 0.045(5) 0.086(7) 0.041(4) 0.004(4) -0.014(3) 0.005(4) C25 0.070(7) 0.110(10) 0.081(8) -0.036(7) -0.027(6) 0.012(6) C24 0.100(10) 0.168(16) 0.068(8) -0.034(9) -0.044(7) 0.035(11) C23 0.111(13) 0.173(19) 0.074(9) 0.010(11) -0.036(9) 0.029(12) C22 0.099(11) 0.091(10) 0.122(13) 0.020(9) -0.026(9) 0.011(8) C21 0.082(8) 0.069(7) 0.078(7) -0.001(6) -0.022(6) -0.003(6) C26 0.055(5) 0.067(5) 0.050(4) -0.010(4) -0.009(4) -0.023(4) C27 0.091(8) 0.085(8) 0.076(7) -0.030(6) -0.001(6) -0.039(6) C28 0.112(11) 0.118(11) 0.092(9) -0.038(8) -0.008(8) -0.071(9) C29 0.096(10) 0.164(15) 0.075(8) -0.036(9) -0.007(7) -0.075(11) C30 0.059(7) 0.159(15) 0.123(12) -0.062(11) 0.009(7) -0.029(8) C31 0.057(6) 0.101(9) 0.087(7) -0.047(7) 0.001(5) -0.024(6) C14 0.073(6) 0.061(5) 0.053(5) -0.024(4) -0.007(4) -0.017(4) C19 0.089(8) 0.071(7) 0.088(8) -0.038(6) 0.003(6) -0.010(6) C18 0.152(15) 0.067(7) 0.097(10) -0.037(7) -0.008(9) -0.011(8) C17 0.186(19) 0.087(10) 0.083(9) -0.022(7) -0.017(10) -0.062(11) C16 0.136(13) 0.112(11) 0.082(8) -0.027(8) 0.001(8) -0.081(10) C15 0.075(7) 0.086(7) 0.069(6) -0.019(5) -0.015(5) -0.032(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 Re1 C2 1.883(9) . ? Re1 C1 1.926(12) . ? Re1 C3 1.963(9) . ? Re1 N1 2.150(7) . ? Re1 N2 2.171(7) . ? Re1 P1 2.407(2) . ? P1 O6 1.595(6) . ? P1 O5 1.595(6) . ? P1 O4 1.607(7) . ? P2 F6 1.437(15) . ? P2 F5 1.447(10) . ? P2 F3 1.452(15) . ? P2 F4 1.508(11) . ? P2 F1 1.525(9) . ? P2 F2 1.549(10) . ? O1 C1 1.151(13) . ? O2 C2 1.172(12) . ? O3 C3 1.139(11) . ? O5 C20 1.406(10) . ? O6 C26 1.399(10) . ? O4 C14 1.395(11) . ? N1 C8 1.359(10) . ? N1 C4 1.384(12) . ? N2 C9 1.329(10) . ? N2 C13 1.362(12) . ? C4 C5 1.386(14) . ? C4 H4 0.9300 . ? C5 C6 1.344(17) . ? C5 H5 0.9300 . ? C6 C7 1.362(16) . ? C6 H6 0.9300 . ? C7 C8 1.386(13) . ? C7 H7 0.9300 . ? C8 C9 1.467(12) . ? C9 C10 1.373(13) . ? C10 C11 1.346(15) . ? C10 H10 0.9300 . ? C11 C12 1.379(17) . ? C11 H11 0.9300 . ? C12 C13 1.409(15) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C20 C21 1.373(16) . ? C20 C25 1.382(16) . ? C25 C24 1.385(18) . ? C25 H25 0.9300 . ? C24 C23 1.36(3) . ? C24 H24 0.9300 . ? C23 C22 1.36(3) . ? C23 H23 0.9300 . ? C22 C21 1.378(17) . ? C22 H22 0.9300 . ? C21 H21 0.9300 . ? C26 C31 1.363(14) . ? C26 C27 1.367(14) . ? C27 C28 1.398(18) . ? C27 H27 0.9300 . ? C28 C29 1.35(2) . ? C28 H28 0.9300 . ? C29 C30 1.40(2) . ? C29 H29 0.9300 . ? C30 C31 1.399(17) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C14 C15 1.369(14) . ? C14 C19 1.391(14) . ? C19 C18 1.402(17) . ? C19 H19 0.9300 . ? C18 C17 1.37(2) . ? C18 H18 0.9300 . ? C17 C16 1.37(2) . ? C17 H17 0.9300 . ? C16 C15 1.373(17) . ? C16 H16 0.9300 . ? C15 H15 0.9300 . ? 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 C2 Re1 C1 88.6(4) . . ? C2 Re1 C3 88.3(4) . . ? C1 Re1 C3 87.9(4) . . ? C2 Re1 N1 172.7(3) . . ? C1 Re1 N1 97.8(4) . . ? C3 Re1 N1 88.3(3) . . ? C2 Re1 N2 99.8(3) . . ? C1 Re1 N2 171.7(4) . . ? C3 Re1 N2 92.4(3) . . ? N1 Re1 N2 73.9(3) . . ? C2 Re1 P1 86.7(3) . . ? C1 Re1 P1 92.3(3) . . ? C3 Re1 P1 175.0(3) . . ? N1 Re1 P1 96.67(19) . . ? N2 Re1 P1 88.13(19) . . ? O6 P1 O5 99.1(3) . . ? O6 P1 O4 98.0(3) . . ? O5 P1 O4 106.0(4) . . ? O6 P1 Re1 117.5(3) . . ? O5 P1 Re1 110.1(2) . . ? O4 P1 Re1 123.0(3) . . ? F6 P2 F5 93.7(15) . . ? F6 P2 F3 169.6(18) . . ? F5 P2 F3 95.0(15) . . ? F6 P2 F4 87.0(14) . . ? F5 P2 F4 179.1(9) . . ? F3 P2 F4 84.3(12) . . ? F6 P2 F1 99.4(13) . . ? F5 P2 F1 92.0(7) . . ? F3 P2 F1 86.0(11) . . ? F4 P2 F1 87.3(6) . . ? F6 P2 F2 87.0(12) . . ? F5 P2 F2 87.1(7) . . ? F3 P2 F2 87.7(12) . . ? F4 P2 F2 93.4(6) . . ? F1 P2 F2 173.5(10) . . ? C20 O5 P1 125.1(6) . . ? C26 O6 P1 126.4(6) . . ? C14 O4 P1 126.3(6) . . ? C8 N1 C4 117.2(8) . . ? C8 N1 Re1 117.7(6) . . ? C4 N1 Re1 124.8(6) . . ? C9 N2 C13 118.5(8) . . ? C9 N2 Re1 118.3(5) . . ? C13 N2 Re1 123.0(6) . . ? O1 C1 Re1 171.8(10) . . ? O2 C2 Re1 178.3(10) . . ? O3 C3 Re1 174.2(9) . . ? N1 C4 C5 122.2(10) . . ? N1 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 118.2(10) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C5 C6 C7 121.7(11) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C6 C7 C8 119.1(10) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? N1 C8 C7 121.5(9) . . ? N1 C8 C9 114.7(7) . . ? C7 C8 C9 123.7(8) . . ? N2 C9 C10 122.2(9) . . ? N2 C9 C8 114.9(7) . . ? C10 C9 C8 122.9(8) . . ? C11 C10 C9 119.5(11) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 121.4(10) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 116.5(10) . . ? C11 C12 H12 121.7 . . ? C13 C12 H12 121.7 . . ? N2 C13 C12 121.8(11) . . ? N2 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C21 C20 C25 122.3(10) . . ? C21 C20 O5 118.5(10) . . ? C25 C20 O5 119.2(11) . . ? C20 C25 C24 117.7(14) . . ? C20 C25 H25 121.2 . . ? C24 C25 H25 121.2 . . ? C23 C24 C25 120.4(15) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C23 C22 121.1(14) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C22 C21 120.5(17) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C20 C21 C22 118.1(14) . . ? C20 C21 H21 121.0 . . ? C22 C21 H21 121.0 . . ? C31 C26 C27 121.9(10) . . ? C31 C26 O6 121.2(9) . . ? C27 C26 O6 116.7(10) . . ? C26 C27 C28 118.0(12) . . ? C26 C27 H27 121.0 . . ? C28 C27 H27 121.0 . . ? C29 C28 C27 122.4(12) . . ? C29 C28 H28 118.8 . . ? C27 C28 H28 118.8 . . ? C28 C29 C30 118.6(12) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? C31 C30 C29 119.8(14) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C26 C31 C30 119.2(11) . . ? C26 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? C15 C14 C19 121.9(10) . . ? C15 C14 O4 123.5(9) . . ? C19 C14 O4 114.6(9) . . ? C14 C19 C18 117.3(13) . . ? C14 C19 H19 121.3 . . ? C18 C19 H19 121.3 . . ? C17 C18 C19 119.9(14) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C16 C17 C18 121.7(13) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C16 C15 119.4(14) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C14 C15 C16 119.8(13) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.435 _refine_diff_density_min -2.627 _refine_diff_density_rms 0.191 #===END