# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mei-Jin Li' _publ_contact_author_email meijinli@gmail.com loop_ _publ_author_name 'Mei-Jin Li' 'Xing Liu' 'Yun-Qin Shi' 'Rui-jia Xie' 'Qiao-hua Wei' ; Guo Nan Chen ; # Attachment '- 1.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 862689' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H26 F12 N4 O3 P2 Re' _chemical_formula_weight 882.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2420(16) _cell_length_b 14.566(3) _cell_length_c 25.304(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.72(3) _cell_angle_gamma 90.00 _cell_volume 3034.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8378 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.932 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 4.218 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'spherical harmonics expansion of the absorption surface ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.75000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mar CCD 165 nm' _diffrn_measurement_method oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8378 _diffrn_reflns_av_R_equivalents 0.0124 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4330 _reflns_number_gt 4033 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Mar CCD' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.The bond distances of P3-F were fixated as 1.58A using the oder of dfix. ; _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^)+(0.0146P)^2^+2.5261P] 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 4330 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0166 _refine_ls_R_factor_gt 0.0149 _refine_ls_wR_factor_ref 0.0376 _refine_ls_wR_factor_gt 0.0371 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 -1.359058(12) 0.284874(7) 0.042142(4) 0.00653(5) Uani 1 1 d . . . P1 P -0.32315(9) 0.42993(5) 0.33748(3) 0.01386(16) Uani 1 1 d . . . P2 P -0.15292(9) 1.03102(5) 0.36252(3) 0.01583(17) Uani 1 1 d . . . F11 F -0.1852(2) 0.38592(13) 0.37621(8) 0.0303(5) Uani 1 1 d . . . F12 F -0.4599(2) 0.39395(13) 0.37533(7) 0.0274(4) Uani 1 1 d . . . F13 F -0.3088(2) 0.52449(12) 0.37017(7) 0.0256(4) Uani 1 1 d . . . F14 F -0.4596(2) 0.47544(12) 0.29877(7) 0.0215(4) Uani 1 1 d . . . F15 F -0.1840(2) 0.46702(11) 0.29941(7) 0.0189(4) Uani 1 1 d . . . F16 F -0.3356(2) 0.33691(12) 0.30423(7) 0.0286(4) Uani 1 1 d . . . F21 F -0.2819(3) 0.94994(14) 0.35401(8) 0.0406(5) Uani 1 1 d . . . F22 F -0.0312(2) 0.96268(13) 0.39473(7) 0.0329(5) Uani 1 1 d . . . F23 F -0.2315(2) 1.05875(13) 0.41684(7) 0.0294(4) Uani 1 1 d . . . F24 F -0.0215(2) 1.11211(11) 0.37130(7) 0.0221(4) Uani 1 1 d . . . F25 F -0.0691(2) 1.00186(12) 0.30853(6) 0.0228(4) Uani 1 1 d . . . F26 F -0.2697(2) 1.09962(14) 0.33004(8) 0.0383(5) Uani 1 1 d . . . O1 O -1.6950(2) 0.23434(14) 0.08209(8) 0.0184(5) Uani 1 1 d . . . O2 O -1.5243(3) 0.29338(13) -0.06992(8) 0.0170(5) Uani 1 1 d . . . O3 O -1.4358(2) 0.49016(13) 0.05756(8) 0.0162(4) Uani 1 1 d . . . N1 N -1.2773(3) 0.14349(15) 0.03815(8) 0.0091(5) Uani 1 1 d . . . N2 N -1.2225(3) 0.26107(15) 0.11650(9) 0.0071(5) Uani 1 1 d . . . N3 N -1.1251(3) 0.32246(15) 0.01572(9) 0.0106(5) Uani 1 1 d . . . N4 N -0.7622(3) 0.22684(15) 0.26186(9) 0.0078(5) Uani 1 1 d . . . C1 C -1.5674(4) 0.25237(19) 0.06807(11) 0.0121(6) Uani 1 1 d . . . C2 C -1.4600(3) 0.29199(17) -0.02817(13) 0.0111(6) Uani 1 1 d . . . C3 C -1.4101(3) 0.4133(2) 0.05187(10) 0.0098(6) Uani 1 1 d . . . C4 C -1.0054(4) 0.35401(18) 0.00381(11) 0.0124(6) Uani 1 1 d . . . C5 C -0.8537(4) 0.3969(2) -0.01140(12) 0.0190(7) Uani 1 1 d . . . C10 C -1.3130(3) 0.08616(19) -0.00251(11) 0.0121(6) Uani 1 1 d . . . H10A H -1.3741 0.1085 -0.0316 0.015 Uiso 1 1 calc R . . C11 C -1.2633(3) -0.00362(19) -0.00298(11) 0.0125(6) Uani 1 1 d . . . H11A H -1.2922 -0.0409 -0.0318 0.015 Uiso 1 1 calc R . . C12 C -1.1701(3) -0.03916(18) 0.03936(11) 0.0119(6) Uani 1 1 d . . . C13 C -1.1282(3) 0.02073(18) 0.08094(11) 0.0095(6) Uani 1 1 d . . . H13A H -1.0627 0.0002 0.1095 0.011 Uiso 1 1 calc R . . C14 C -1.1837(3) 0.11045(18) 0.07996(10) 0.0074(6) Uani 1 1 d . . . C15 C -1.1507(3) 0.17714(18) 0.12363(10) 0.0067(6) Uani 1 1 d . . . C16 C -1.0582(3) 0.15668(17) 0.16920(10) 0.0075(6) Uani 1 1 d . . . H16A H -1.0112 0.0989 0.1733 0.009 Uiso 1 1 calc R . . C17 C -1.1088(3) 0.30742(18) 0.20155(11) 0.0093(6) Uani 1 1 d . . . H17A H -1.0977 0.3525 0.2275 0.011 Uiso 1 1 calc R . . C18 C -1.0350(3) 0.22227(17) 0.20915(10) 0.0067(5) Uani 1 1 d . . . C19 C -1.1990(3) 0.32440(18) 0.15504(10) 0.0080(6) Uani 1 1 d . . . H19A H -1.2455 0.3821 0.1501 0.010 Uiso 1 1 calc R . . C20 C -1.1184(4) -0.13829(19) 0.04037(12) 0.0198(7) Uani 1 1 d . . . H20A H -1.1579 -0.1680 0.0084 0.030 Uiso 1 1 calc R . . H20B H -1.1624 -0.1683 0.0703 0.030 Uiso 1 1 calc R . . H20C H -1.0020 -0.1418 0.0430 0.030 Uiso 1 1 calc R . . C21 C -0.9403(3) 0.19831(18) 0.25990(10) 0.0085(6) Uani 1 1 d . . . H21A H -0.9460 0.1324 0.2651 0.010 Uiso 1 1 calc R . . H21B H -0.9925 0.2273 0.2891 0.010 Uiso 1 1 calc R . . C22 C -0.7438(3) 0.33084(18) 0.25875(11) 0.0119(6) Uani 1 1 d . . . H22A H -0.6292 0.3452 0.2570 0.014 Uiso 1 1 calc R . . H22B H -0.7977 0.3520 0.2261 0.014 Uiso 1 1 calc R . . C23 C -0.8114(4) 0.3841(2) 0.30453(12) 0.0176(6) Uani 1 1 d . . . H23A H -0.7945 0.4486 0.2993 0.026 Uiso 1 1 calc R . . H23B H -0.7568 0.3652 0.3371 0.026 Uiso 1 1 calc R . . H23C H -0.9256 0.3721 0.3061 0.026 Uiso 1 1 calc R . . C24 C -0.6823(3) 0.19191(19) 0.31382(10) 0.0114(6) Uani 1 1 d . . . H24A H -0.5755 0.2196 0.3184 0.014 Uiso 1 1 calc R . . H24B H -0.7462 0.2128 0.3427 0.014 Uiso 1 1 calc R . . C25 C -0.6637(3) 0.08860(19) 0.31796(11) 0.0147(6) Uani 1 1 d . . . H25A H -0.6131 0.0731 0.3517 0.022 Uiso 1 1 calc R . . H25B H -0.5974 0.0671 0.2903 0.022 Uiso 1 1 calc R . . H25C H -0.7688 0.0602 0.3144 0.022 Uiso 1 1 calc R . . C26 C -0.6828(3) 0.18482(19) 0.21439(11) 0.0099(6) Uani 1 1 d . . . H26A H -0.7071 0.1197 0.2134 0.012 Uiso 1 1 calc R . . H26B H -0.7317 0.2119 0.1824 0.012 Uiso 1 1 calc R . . C27 C -0.5001(3) 0.1968(2) 0.21369(12) 0.0180(7) Uani 1 1 d . . . H27A H -0.4608 0.1683 0.1826 0.027 Uiso 1 1 calc R . . H27B H -0.4497 0.1687 0.2446 0.027 Uiso 1 1 calc R . . H27C H -0.4743 0.2611 0.2134 0.027 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 0.00800(7) 0.00637(6) 0.00490(7) 0.00069(4) -0.00290(4) 0.00079(4) P1 0.0146(4) 0.0151(4) 0.0112(4) 0.0022(3) -0.0054(3) -0.0062(3) P2 0.0166(4) 0.0154(4) 0.0157(4) -0.0025(3) 0.0029(3) -0.0025(3) F11 0.0232(10) 0.0301(11) 0.0359(12) 0.0162(8) -0.0170(9) -0.0069(8) F12 0.0239(10) 0.0391(11) 0.0188(10) 0.0136(8) -0.0026(8) -0.0120(8) F13 0.0404(11) 0.0222(10) 0.0140(9) -0.0062(7) -0.0014(8) -0.0068(8) F14 0.0168(9) 0.0276(10) 0.0193(9) 0.0103(7) -0.0064(8) -0.0052(7) F15 0.0165(9) 0.0170(9) 0.0236(10) 0.0018(7) 0.0038(8) -0.0038(7) F16 0.0396(11) 0.0162(9) 0.0294(11) -0.0037(8) -0.0035(9) -0.0107(8) F21 0.0432(12) 0.0379(12) 0.0423(12) -0.0199(10) 0.0196(10) -0.0272(10) F22 0.0477(12) 0.0270(11) 0.0245(11) 0.0089(8) 0.0057(10) 0.0138(9) F23 0.0285(10) 0.0332(11) 0.0275(11) -0.0128(8) 0.0138(9) -0.0054(8) F24 0.0251(10) 0.0216(9) 0.0195(10) -0.0029(7) -0.0001(8) -0.0083(7) F25 0.0307(10) 0.0220(9) 0.0164(9) -0.0045(7) 0.0081(8) -0.0067(8) F26 0.0320(11) 0.0423(12) 0.0388(13) -0.0046(9) -0.0159(10) 0.0130(9) O1 0.0125(11) 0.0261(12) 0.0167(12) 0.0035(9) 0.0004(9) -0.0049(9) O2 0.0238(11) 0.0164(11) 0.0100(12) -0.0010(8) -0.0079(10) 0.0034(8) O3 0.0209(11) 0.0104(11) 0.0170(11) -0.0005(8) -0.0016(9) 0.0034(8) N1 0.0128(11) 0.0100(12) 0.0041(12) -0.0011(9) -0.0033(10) -0.0008(9) N2 0.0061(11) 0.0071(11) 0.0080(12) 0.0008(9) -0.0003(9) -0.0013(9) N3 0.0132(13) 0.0093(11) 0.0091(12) 0.0005(9) -0.0021(10) 0.0027(10) N4 0.0084(11) 0.0097(12) 0.0050(12) 0.0000(9) -0.0030(10) -0.0014(9) C1 0.0201(17) 0.0102(14) 0.0053(14) -0.0008(11) -0.0078(13) 0.0023(12) C2 0.0103(14) 0.0051(14) 0.0181(19) 0.0006(11) 0.0030(14) 0.0029(10) C3 0.0072(13) 0.0185(17) 0.0034(14) 0.0028(11) -0.0028(11) -0.0019(11) C4 0.0170(16) 0.0087(14) 0.0111(15) -0.0011(11) -0.0021(12) 0.0057(12) C5 0.0122(15) 0.0210(16) 0.0244(17) 0.0014(13) 0.0064(13) -0.0025(12) C10 0.0138(14) 0.0141(15) 0.0080(15) 0.0011(11) -0.0052(12) -0.0013(11) C11 0.0150(14) 0.0123(15) 0.0095(15) -0.0057(11) -0.0045(12) -0.0022(11) C12 0.0116(14) 0.0096(14) 0.0145(16) -0.0020(11) 0.0006(12) -0.0013(11) C13 0.0088(13) 0.0112(14) 0.0079(14) 0.0011(11) -0.0040(11) 0.0007(11) C14 0.0070(13) 0.0089(13) 0.0063(14) -0.0003(10) -0.0010(11) -0.0018(10) C15 0.0058(13) 0.0065(13) 0.0078(14) 0.0013(10) 0.0011(11) -0.0025(10) C16 0.0076(13) 0.0061(13) 0.0086(14) 0.0031(10) -0.0012(11) -0.0007(10) C17 0.0091(13) 0.0102(14) 0.0084(15) -0.0026(11) -0.0014(12) -0.0038(10) C18 0.0040(13) 0.0096(13) 0.0064(14) 0.0015(10) -0.0002(11) -0.0043(10) C19 0.0082(13) 0.0055(13) 0.0102(15) 0.0005(11) -0.0012(12) 0.0008(10) C20 0.0250(17) 0.0115(15) 0.0223(17) -0.0061(12) -0.0063(14) 0.0042(13) C21 0.0074(13) 0.0098(14) 0.0082(14) 0.0013(10) -0.0014(12) -0.0025(10) C22 0.0119(14) 0.0076(14) 0.0158(15) 0.0016(11) -0.0040(12) -0.0039(11) C23 0.0160(15) 0.0146(15) 0.0214(17) -0.0061(12) -0.0061(13) 0.0013(12) C24 0.0096(14) 0.0186(15) 0.0054(14) 0.0021(11) -0.0059(12) -0.0010(11) C25 0.0146(15) 0.0174(15) 0.0114(15) 0.0031(12) -0.0053(12) 0.0003(12) C26 0.0119(14) 0.0121(14) 0.0055(14) -0.0025(11) -0.0019(12) -0.0010(11) C27 0.0133(15) 0.0258(17) 0.0152(16) -0.0027(12) 0.0037(13) -0.0026(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.926(3) . ? Re1 C2 1.931(3) . ? Re1 C3 1.935(3) . ? Re1 N3 2.142(2) . ? Re1 N1 2.171(2) . ? Re1 N2 2.174(2) . ? P1 F16 1.5957(18) . ? P1 F11 1.5997(19) . ? P1 F14 1.5999(18) . ? P1 F12 1.6013(18) . ? P1 F13 1.6081(18) . ? P1 F15 1.6247(18) . ? P2 F26 1.589(2) . ? P2 F21 1.5968(19) . ? P2 F23 1.5988(18) . ? P2 F22 1.608(2) . ? P2 F24 1.6109(18) . ? P2 F25 1.6166(18) . ? O1 C1 1.156(3) . ? O2 C2 1.159(4) . ? O3 C3 1.150(3) . ? N1 C10 1.347(4) . ? N1 C14 1.367(3) . ? N2 C19 1.350(3) . ? N2 C15 1.366(3) . ? N3 C4 1.142(4) . ? N4 C26 1.523(3) . ? N4 C21 1.524(3) . ? N4 C22 1.525(3) . ? N4 C24 1.529(3) . ? C4 C5 1.465(4) . ? C10 C11 1.371(4) . ? C10 H10A 0.9300 . ? C11 C12 1.389(4) . ? C11 H11A 0.9300 . ? C12 C13 1.397(4) . ? C12 C20 1.505(4) . ? C13 C14 1.384(4) . ? C13 H13A 0.9300 . ? C14 C15 1.487(4) . ? C15 C16 1.385(4) . ? C16 C18 1.398(4) . ? C16 H16A 0.9300 . ? C17 C19 1.384(4) . ? C17 C18 1.391(4) . ? C17 H17A 0.9300 . ? C18 C21 1.511(4) . ? C19 H19A 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.522(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.516(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.517(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 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 88.56(11) . . ? C1 Re1 C3 89.52(11) . . ? C2 Re1 C3 88.77(11) . . ? C1 Re1 N3 178.23(10) . . ? C2 Re1 N3 93.07(10) . . ? C3 Re1 N3 89.82(10) . . ? C1 Re1 N1 93.80(10) . . ? C2 Re1 N1 97.42(9) . . ? C3 Re1 N1 173.03(10) . . ? N3 Re1 N1 86.68(8) . . ? C1 Re1 N2 95.70(10) . . ? C2 Re1 N2 171.43(9) . . ? C3 Re1 N2 98.67(9) . . ? N3 Re1 N2 82.77(8) . . ? N1 Re1 N2 74.92(8) . . ? F16 P1 F11 90.50(11) . . ? F16 P1 F14 90.18(10) . . ? F11 P1 F14 179.10(10) . . ? F16 P1 F12 90.46(10) . . ? F11 P1 F12 90.15(10) . . ? F14 P1 F12 90.42(10) . . ? F16 P1 F13 178.97(11) . . ? F11 P1 F13 89.72(11) . . ? F14 P1 F13 89.58(10) . . ? F12 P1 F13 90.55(10) . . ? F16 P1 F15 89.95(10) . . ? F11 P1 F15 89.72(10) . . ? F14 P1 F15 89.70(9) . . ? F12 P1 F15 179.58(11) . . ? F13 P1 F15 89.05(9) . . ? F26 P2 F21 90.70(13) . . ? F26 P2 F23 91.46(11) . . ? F21 P2 F23 90.49(10) . . ? F26 P2 F22 178.65(13) . . ? F21 P2 F22 90.35(12) . . ? F23 P2 F22 89.39(11) . . ? F26 P2 F24 89.83(11) . . ? F21 P2 F24 179.45(13) . . ? F23 P2 F24 89.63(10) . . ? F22 P2 F24 89.12(11) . . ? F26 P2 F25 90.05(11) . . ? F21 P2 F25 90.00(10) . . ? F23 P2 F25 178.41(12) . . ? F22 P2 F25 89.10(10) . . ? F24 P2 F25 89.86(9) . . ? C10 N1 C14 117.9(2) . . ? C10 N1 Re1 124.53(18) . . ? C14 N1 Re1 117.58(17) . . ? C19 N2 C15 118.0(2) . . ? C19 N2 Re1 124.54(17) . . ? C15 N2 Re1 117.40(17) . . ? C4 N3 Re1 170.9(2) . . ? C26 N4 C21 108.3(2) . . ? C26 N4 C22 108.1(2) . . ? C21 N4 C22 111.6(2) . . ? C26 N4 C24 111.1(2) . . ? C21 N4 C24 108.2(2) . . ? C22 N4 C24 109.6(2) . . ? O1 C1 Re1 177.6(2) . . ? O2 C2 Re1 177.4(2) . . ? O3 C3 Re1 178.1(2) . . ? N3 C4 C5 178.5(3) . . ? N1 C10 C11 122.9(3) . . ? N1 C10 H10A 118.5 . . ? C11 C10 H10A 118.5 . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C11 C12 C13 117.1(2) . . ? C11 C12 C20 121.1(2) . . ? C13 C12 C20 121.8(2) . . ? C14 C13 C12 120.4(2) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? N1 C14 C13 121.3(2) . . ? N1 C14 C15 114.9(2) . . ? C13 C14 C15 123.7(2) . . ? N2 C15 C16 121.4(2) . . ? N2 C15 C14 115.1(2) . . ? C16 C15 C14 123.5(2) . . ? C15 C16 C18 120.4(2) . . ? C15 C16 H16A 119.8 . . ? C18 C16 H16A 119.8 . . ? C19 C17 C18 119.4(2) . . ? C19 C17 H17A 120.3 . . ? C18 C17 H17A 120.3 . . ? C17 C18 C16 117.7(2) . . ? C17 C18 C21 121.9(2) . . ? C16 C18 C21 120.3(2) . . ? N2 C19 C17 123.0(2) . . ? N2 C19 H19A 118.5 . . ? C17 C19 H19A 118.5 . . ? C12 C20 H20A 109.5 . . ? C12 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C12 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 N4 115.0(2) . . ? C18 C21 H21A 108.5 . . ? N4 C21 H21A 108.5 . . ? C18 C21 H21B 108.5 . . ? N4 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 N4 115.2(2) . . ? C23 C22 H22A 108.5 . . ? N4 C22 H22A 108.5 . . ? C23 C22 H22B 108.5 . . ? N4 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 N4 115.3(2) . . ? C25 C24 H24A 108.4 . . ? N4 C24 H24A 108.4 . . ? C25 C24 H24B 108.4 . . ? N4 C24 H24B 108.4 . . ? H24A C24 H24B 107.5 . . ? 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 . . ? C27 C26 N4 115.3(2) . . ? C27 C26 H26A 108.5 . . ? N4 C26 H26A 108.5 . . ? C27 C26 H26B 108.5 . . ? N4 C26 H26B 108.5 . . ? H26A C26 H26B 107.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.663 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.066 # Attachment '- 2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 862690' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H43 F18 N6 O3 P3 Re' _chemical_formula_weight 1168.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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 14.420(3) _cell_length_b 23.520(5) _cell_length_c 14.260(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4836.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16140 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 30.88 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2308 _exptl_absorpt_coefficient_mu 2.717 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.75000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mar CCD 165 nm' _diffrn_measurement_method oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 16140 _diffrn_reflns_av_R_equivalents 0.1131 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.69 _reflns_number_total 5464 _reflns_number_gt 4894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Mar CCD' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1138P)^2^+17.6915P] 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 SHELXL _refine_ls_extinction_coef 0.0048(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 5464 _refine_ls_number_parameters 554 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1934 _refine_ls_wR_factor_gt 0.1865 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re -0.70271(5) 0.43246(2) 2.59562(18) 0.0282(2) Uiso 0.80 1 d P A 1 Re1' Re -0.6770(2) 0.43517(9) 2.5844(3) 0.0292(7) Uiso 0.20 1 d P A 2 O1 O -0.5589(12) 0.5009(6) 2.7131(13) 0.084(5) Uani 1 1 d . A . O2 O -0.6436(10) 0.3241(5) 2.6990(10) 0.064(3) Uani 1 1 d . A . O3 O -0.8409(10) 0.4554(7) 2.7507(8) 0.061(3) Uani 1 1 d . A . P1 P -1.4437(3) 0.29039(18) 2.1205(3) 0.0483(9) Uani 1 1 d . . . P2 P 0.0380(2) 0.48944(14) 1.0944(4) 0.0456(7) Uani 1 1 d . . . P3 P -0.6439(3) 0.67461(16) 1.11162(16) 0.0506(10) Uani 1 1 d D . . F11 F -1.3813(8) 0.2744(5) 2.2079(9) 0.075(3) Uani 1 1 d . . . F12 F -1.4249(9) 0.3561(5) 2.1351(9) 0.082(4) Uani 1 1 d . . . F13 F -1.5071(11) 0.3052(6) 2.0332(11) 0.090(4) Uani 1 1 d . . . F14 F -1.5307(8) 0.2919(5) 2.1879(9) 0.066(3) Uani 1 1 d . . . F15 F -1.4610(8) 0.2235(4) 2.1024(9) 0.066(2) Uani 1 1 d . . . F16 F -1.3564(14) 0.2848(5) 2.0544(10) 0.116(7) Uani 1 1 d . . . F21 F 0.0851(14) 0.4309(5) 1.1170(14) 0.113(7) Uani 1 1 d . . . F22 F -0.0166(10) 0.5475(5) 1.0728(7) 0.079(3) Uani 1 1 d . . . F23 F 0.1311(8) 0.5225(6) 1.1098(12) 0.098(4) Uani 1 1 d . . . F24 F 0.0153(9) 0.4982(6) 1.2048(8) 0.071(3) Uani 1 1 d . . . F25 F -0.0576(9) 0.4582(6) 1.0841(11) 0.094(4) Uani 1 1 d . . . F26 F 0.0568(11) 0.4817(5) 0.9870(8) 0.081(4) Uani 1 1 d . . . F31 F -0.6351(11) 0.6631(8) 1.2203(3) 0.103(5) Uani 1 1 d D . . F32 F -0.6583(9) 0.6898(7) 1.0046(3) 0.097(5) Uani 1 1 d D . . F33 F -0.5875(17) 0.6191(5) 1.0864(18) 0.190(12) Uani 1 1 d D . . F34 F -0.7363(11) 0.6386(11) 1.1136(11) 0.171(11) Uani 1 1 d D . . F35 F -0.5477(9) 0.7064(9) 1.1045(16) 0.149(8) Uani 1 1 d D . . F36 F -0.696(2) 0.7318(7) 1.1369(15) 0.223(18) Uani 1 1 d D . . N1 N -0.7419(8) 0.5030(4) 2.5045(8) 0.036(2) Uani 1 1 d . . . N2 N -0.7992(6) 0.3960(5) 2.4981(8) 0.031(2) Uani 1 1 d . . . N3 N -0.9185(11) 0.6656(5) 2.3369(9) 0.046(3) Uani 1 1 d . A . N4 N -1.1055(8) 0.3454(5) 2.3418(8) 0.033(2) Uani 1 1 d . A . N5 N -0.6030(8) 0.4163(5) 2.4838(9) 0.042(2) Uani 1 1 d . . . C1 C -0.6104(16) 0.4736(8) 2.6659(14) 0.067(5) Uani 1 1 d . . . C2 C -0.6638(11) 0.3651(7) 2.6605(11) 0.050(3) Uani 1 1 d . . . C3 C -0.7904(12) 0.4464(8) 2.6910(13) 0.053(4) Uani 1 1 d . . . C4 C -0.5539(10) 0.4044(7) 2.4297(13) 0.052(4) Uani 1 1 d . A . C5 C -0.4893(12) 0.3902(8) 2.3491(12) 0.057(4) Uani 1 1 d . . . C11 C -0.7112(10) 0.5559(6) 2.5084(12) 0.041(3) Uani 1 1 d . A . H11A H -0.6684 0.5652 2.5548 0.049 Uiso 1 1 calc R . . C12 C -0.7385(11) 0.5966(6) 2.4492(11) 0.046(3) Uani 1 1 d . . . H12A H -0.7143 0.6331 2.4547 0.055 Uiso 1 1 calc R A . C13 C -0.8032(10) 0.5847(7) 2.3791(12) 0.043(3) Uani 1 1 d . A . C14 C -0.8343(10) 0.5301(6) 2.3723(11) 0.041(3) Uani 1 1 d . . . H14A H -0.8752 0.5201 2.3246 0.049 Uiso 1 1 calc R A . C15 C -0.8045(8) 0.4892(5) 2.4373(10) 0.032(3) Uani 1 1 d . A . C16 C -0.8360(10) 0.4307(5) 2.4326(10) 0.030(3) Uani 1 1 d . A . C17 C -0.9030(9) 0.4101(5) 2.3714(9) 0.033(2) Uani 1 1 d . . . H17A H -0.9279 0.4343 2.3263 0.040 Uiso 1 1 calc R A . C18 C -0.9326(9) 0.3557(5) 2.3760(9) 0.035(3) Uani 1 1 d . A . C19 C -0.8928(9) 0.3190(5) 2.4410(10) 0.035(3) Uani 1 1 d . . . H19A H -0.9099 0.2809 2.4436 0.042 Uiso 1 1 calc R A . C20 C -0.8275(10) 0.3408(5) 2.5013(10) 0.038(3) Uani 1 1 d . A . H20A H -0.8016 0.3169 2.5461 0.046 Uiso 1 1 calc R . . C31 C -0.8382(10) 0.6280(5) 2.3062(10) 0.042(3) Uani 1 1 d . . . H31A H -0.7867 0.6524 2.2887 0.050 Uiso 1 1 calc R A . H31B H -0.8570 0.6074 2.2505 0.050 Uiso 1 1 calc R . . C32 C -0.8906(14) 0.7011(7) 2.4199(10) 0.055(4) Uani 1 1 d . . . H32A H -0.8705 0.6758 2.4696 0.066 Uiso 1 1 calc R A . H32B H -0.9450 0.7212 2.4424 0.066 Uiso 1 1 calc R . . C33 C -0.8141(18) 0.7445(8) 2.4029(18) 0.088(8) Uani 1 1 d . A . H33A H -0.8017 0.7648 2.4599 0.131 Uiso 1 1 calc R . . H33B H -0.8335 0.7708 2.3553 0.131 Uiso 1 1 calc R . . H33C H -0.7589 0.7253 2.3827 0.131 Uiso 1 1 calc R . . C34 C -0.9959(11) 0.6262(6) 2.3655(10) 0.045(3) Uani 1 1 d . . . H34A H -0.9766 0.6057 2.4211 0.054 Uiso 1 1 calc R A . H34B H -1.0051 0.5986 2.3159 0.054 Uiso 1 1 calc R . . C35 C -1.0904(15) 0.6555(8) 2.3863(14) 0.066(5) Uani 1 1 d . A . H35A H -1.1351 0.6272 2.4041 0.099 Uiso 1 1 calc R . . H35B H -1.1116 0.6749 2.3312 0.099 Uiso 1 1 calc R . . H35C H -1.0829 0.6823 2.4365 0.099 Uiso 1 1 calc R . . C36 C -0.9444(11) 0.7012(6) 2.2561(10) 0.044(3) Uani 1 1 d . . . H36A H -0.8895 0.7213 2.2348 0.052 Uiso 1 1 calc R A . H36B H -0.9887 0.7295 2.2771 0.052 Uiso 1 1 calc R . . C37 C -0.9857(15) 0.6698(7) 2.1736(11) 0.062(5) Uani 1 1 d . A . H37A H -1.0003 0.6964 2.1247 0.092 Uiso 1 1 calc R . . H37B H -1.0412 0.6506 2.1930 0.092 Uiso 1 1 calc R . . H37C H -0.9418 0.6425 2.1506 0.092 Uiso 1 1 calc R . . C41 C -1.0080(8) 0.3356(6) 2.3085(9) 0.035(2) Uani 1 1 d . . . H41A H -0.9998 0.3549 2.2490 0.042 Uiso 1 1 calc R A . H41B H -0.9997 0.2952 2.2974 0.042 Uiso 1 1 calc R . . C42 C -1.1705(11) 0.3185(8) 2.2702(11) 0.048(4) Uani 1 1 d . . . H42A H -1.1543 0.2787 2.2639 0.058 Uiso 1 1 calc R A . H42B H -1.2332 0.3203 2.2947 0.058 Uiso 1 1 calc R . . C43 C -1.1703(14) 0.3444(11) 2.1756(13) 0.075(6) Uani 1 1 d . A . H43A H -1.2136 0.3247 2.1362 0.112 Uiso 1 1 calc R . . H43B H -1.1093 0.3417 2.1491 0.112 Uiso 1 1 calc R . . H43C H -1.1879 0.3837 2.1802 0.112 Uiso 1 1 calc R . . C44 C -1.1244(10) 0.3166(6) 2.4369(10) 0.043(3) Uani 1 1 d . . . H44A H -1.0829 0.3331 2.4830 0.051 Uiso 1 1 calc R A . H44B H -1.1872 0.3259 2.4558 0.051 Uiso 1 1 calc R . . C45 C -1.1138(14) 0.2535(9) 2.4402(14) 0.068(5) Uani 1 1 d . A . H45A H -1.1271 0.2402 2.5024 0.102 Uiso 1 1 calc R . . H45B H -1.0514 0.2435 2.4237 0.102 Uiso 1 1 calc R . . H45C H -1.1561 0.2363 2.3966 0.102 Uiso 1 1 calc R . . C46 C -1.1211(10) 0.4091(7) 2.3523(12) 0.047(3) Uani 1 1 d . . . H46A H -1.1017 0.4277 2.2948 0.056 Uiso 1 1 calc R A . H46B H -1.0817 0.4230 2.4023 0.056 Uiso 1 1 calc R . . C47 C -1.2228(12) 0.4271(8) 2.3737(17) 0.061(5) Uani 1 1 d . A . H47A H -1.2262 0.4677 2.3788 0.092 Uiso 1 1 calc R . . H47B H -1.2424 0.4101 2.4316 0.092 Uiso 1 1 calc R . . H47C H -1.2625 0.4145 2.3238 0.092 Uiso 1 1 calc R . . C01 C -0.742(2) 0.3447(14) 2.1142(19) 0.108(10) Uani 1 1 d . B . H01A H -0.8073 0.3438 2.0991 0.162 Uiso 1 1 calc R . . H01B H -0.7131 0.3108 2.0912 0.162 Uiso 1 1 calc R . . H01C H -0.7143 0.3774 2.0853 0.162 Uiso 1 1 calc R . . C02 C -0.732(2) 0.3479(14) 2.2089(17) 0.093(8) Uani 1 1 d . . . N01 N -0.7131(16) 0.3488(12) 2.288(2) 0.104(7) Uiso 1 1 d . B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.112(11) 0.045(7) 0.093(11) -0.006(7) -0.048(10) -0.019(7) O2 0.095(9) 0.031(5) 0.066(8) 0.024(5) -0.014(7) 0.004(6) O3 0.080(9) 0.071(9) 0.030(5) -0.002(6) 0.013(6) 0.023(8) P1 0.058(2) 0.0426(19) 0.044(2) 0.0003(15) 0.0063(15) -0.0153(16) P2 0.0618(18) 0.0359(15) 0.0391(14) -0.002(2) -0.007(2) 0.0017(13) P3 0.0543(18) 0.0413(17) 0.056(3) 0.0045(17) -0.0053(18) -0.0030(14) F11 0.076(7) 0.078(8) 0.070(7) -0.008(6) -0.014(6) -0.021(6) F12 0.112(9) 0.063(7) 0.071(7) -0.011(6) 0.035(7) -0.038(6) F13 0.110(11) 0.079(9) 0.082(9) 0.020(7) -0.040(8) -0.013(7) F14 0.065(6) 0.054(6) 0.079(8) -0.006(6) 0.018(6) -0.010(5) F15 0.102(7) 0.050(5) 0.046(5) 0.000(5) 0.013(6) -0.025(5) F16 0.206(16) 0.059(7) 0.083(9) -0.031(6) 0.096(10) -0.066(9) F21 0.174(16) 0.055(7) 0.111(17) 0.001(7) 0.024(12) 0.045(8) F22 0.125(9) 0.061(6) 0.049(7) -0.001(5) -0.021(6) 0.024(6) F23 0.077(7) 0.122(11) 0.094(11) -0.012(9) 0.008(8) -0.027(7) F24 0.086(8) 0.088(8) 0.039(5) 0.002(5) -0.014(5) 0.022(6) F25 0.092(7) 0.123(10) 0.067(8) -0.007(9) -0.010(8) -0.056(7) F26 0.139(12) 0.056(7) 0.047(6) -0.007(5) 0.031(7) -0.014(7) F31 0.103(10) 0.146(15) 0.060(7) 0.022(8) -0.027(7) -0.035(10) F32 0.077(8) 0.163(15) 0.051(6) 0.014(8) -0.009(6) -0.045(9) F33 0.27(3) 0.115(12) 0.18(2) 0.080(15) 0.15(2) 0.109(15) F34 0.105(10) 0.35(3) 0.062(10) 0.014(13) -0.004(8) -0.130(16) F35 0.129(12) 0.21(2) 0.109(13) -0.013(16) -0.024(13) -0.109(13) F36 0.39(4) 0.16(2) 0.118(16) 0.065(14) 0.11(2) 0.19(3) N1 0.056(6) 0.014(4) 0.037(5) 0.002(4) -0.005(5) 0.001(4) N2 0.040(5) 0.023(5) 0.028(5) -0.005(4) -0.016(4) -0.001(4) N3 0.085(10) 0.019(5) 0.034(6) -0.006(4) -0.004(6) 0.020(5) N4 0.043(6) 0.028(5) 0.029(5) 0.004(4) 0.006(4) 0.001(4) N5 0.038(5) 0.043(6) 0.045(6) -0.001(6) 0.006(5) 0.003(5) C1 0.106(15) 0.044(9) 0.053(9) 0.014(8) -0.016(10) 0.007(9) C2 0.056(8) 0.056(9) 0.039(7) 0.002(7) -0.008(6) 0.007(7) C3 0.065(10) 0.045(8) 0.048(9) 0.007(8) -0.027(8) 0.007(7) C4 0.043(7) 0.051(9) 0.062(9) 0.004(8) -0.006(7) -0.018(6) C5 0.066(10) 0.051(9) 0.054(9) -0.006(7) 0.024(8) 0.005(8) C11 0.054(8) 0.022(5) 0.048(8) -0.008(6) -0.005(6) -0.004(5) C12 0.053(8) 0.031(6) 0.054(8) 0.005(6) -0.001(7) -0.001(6) C13 0.053(8) 0.027(7) 0.048(8) -0.008(6) 0.004(6) -0.003(5) C14 0.049(7) 0.028(6) 0.045(7) -0.011(5) -0.002(6) 0.006(5) C15 0.047(7) 0.011(5) 0.037(6) -0.002(5) -0.006(5) -0.002(4) C16 0.036(6) 0.025(6) 0.029(6) -0.003(4) -0.011(5) 0.002(5) C17 0.043(6) 0.027(6) 0.029(5) -0.001(4) 0.000(5) 0.008(5) C18 0.041(6) 0.031(6) 0.034(6) -0.005(5) 0.008(5) -0.001(5) C19 0.037(6) 0.023(5) 0.045(7) -0.010(5) -0.002(5) -0.002(4) C20 0.050(7) 0.029(6) 0.036(6) 0.006(5) 0.001(6) 0.005(5) C31 0.057(8) 0.023(6) 0.045(7) 0.001(5) 0.005(6) -0.004(5) C32 0.099(13) 0.037(7) 0.028(6) -0.011(6) -0.005(7) 0.013(8) C33 0.14(2) 0.038(9) 0.084(15) -0.007(10) -0.057(15) 0.015(10) C34 0.075(9) 0.028(6) 0.034(6) 0.001(5) 0.009(6) 0.016(6) C35 0.092(13) 0.054(10) 0.052(9) -0.006(8) 0.016(9) 0.008(9) C36 0.064(9) 0.036(7) 0.031(6) 0.004(5) -0.004(6) -0.005(6) C37 0.106(14) 0.042(8) 0.036(8) -0.004(6) -0.018(9) 0.010(9) C41 0.037(6) 0.038(7) 0.029(5) -0.004(5) -0.002(5) 0.011(5) C42 0.045(7) 0.055(9) 0.044(8) -0.016(7) 0.009(6) -0.018(7) C43 0.061(10) 0.121(19) 0.042(9) -0.019(11) -0.016(8) -0.007(11) C44 0.044(7) 0.047(8) 0.038(7) 0.009(6) 0.003(5) -0.010(6) C45 0.069(10) 0.081(13) 0.055(9) 0.011(10) -0.005(8) -0.029(10) C46 0.040(7) 0.046(8) 0.054(8) -0.009(7) -0.001(6) 0.016(6) C47 0.032(7) 0.067(11) 0.085(14) 0.009(10) 0.012(9) 0.008(7) C01 0.105(17) 0.14(2) 0.075(18) -0.010(16) 0.012(14) 0.051(17) C02 0.108(17) 0.12(2) 0.053(11) 0.006(13) 0.012(12) 0.036(16) _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 1.89(2) . ? Re1 C2 1.919(16) . ? Re1 C1 1.93(2) . ? Re1 N2 2.146(9) . ? Re1 N5 2.180(12) . ? Re1 N1 2.183(10) . ? Re1' C1 1.76(2) . ? Re1' N5 1.843(13) . ? Re1' C2 1.983(17) . ? Re1' N1 2.173(10) . ? Re1' C3 2.25(2) . ? Re1' N2 2.338(9) . ? O1 C1 1.19(2) . ? O2 C2 1.147(19) . ? O3 C3 1.14(2) . ? P1 F16 1.577(14) . ? P1 F11 1.582(13) . ? P1 F14 1.582(12) . ? P1 F12 1.583(12) . ? P1 F13 1.583(13) . ? P1 F15 1.615(10) . ? P2 F23 1.566(12) . ? P2 F26 1.567(12) . ? P2 F21 1.568(12) . ? P2 F25 1.570(11) . ? P2 F22 1.607(12) . ? P2 F24 1.620(12) . ? P3 F34 1.579(2) . ? P3 F31 1.579(2) . ? P3 F35 1.579(2) . ? P3 F33 1.579(2) . ? P3 F36 1.580(2) . ? P3 F32 1.580(2) . ? N1 C11 1.321(17) . ? N1 C15 1.356(17) . ? N2 C16 1.350(16) . ? N2 C20 1.360(17) . ? N3 C36 1.472(18) . ? N3 C32 1.504(19) . ? N3 C34 1.51(2) . ? N3 C31 1.521(18) . ? N4 C41 1.502(16) . ? N4 C46 1.523(18) . ? N4 C42 1.524(19) . ? N4 C44 1.539(17) . ? N5 C4 1.08(2) . ? C4 C5 1.52(2) . ? C11 C12 1.34(2) . ? C11 H11A 0.9300 . ? C12 C13 1.39(2) . ? C12 H12A 0.9300 . ? C13 C14 1.363(19) . ? C13 C31 1.54(2) . ? C14 C15 1.404(19) . ? C14 H14A 0.9300 . ? C15 C16 1.451(15) . ? C16 C17 1.389(18) . ? C17 C18 1.350(17) . ? C17 H17A 0.9300 . ? C18 C19 1.391(19) . ? C18 C41 1.528(18) . ? C19 C20 1.375(19) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.52(3) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.55(2) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.51(2) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.48(3) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C45 1.49(3) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.56(2) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C01 C02 1.36(4) . ? C01 H01A 0.9600 . ? C01 H01B 0.9600 . ? C01 H01C 0.9600 . ? C02 N01 1.16(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Re1 C2 89.6(7) . . ? C3 Re1 C1 90.0(9) . . ? C2 Re1 C1 87.8(7) . . ? C3 Re1 N2 95.9(6) . . ? C2 Re1 N2 99.9(6) . . ? C1 Re1 N2 170.3(6) . . ? C3 Re1 N5 179.1(6) . . ? C2 Re1 N5 90.9(6) . . ? C1 Re1 N5 90.7(8) . . ? N2 Re1 N5 83.3(5) . . ? C3 Re1 N1 97.1(6) . . ? C2 Re1 N1 172.2(6) . . ? C1 Re1 N1 96.1(6) . . ? N2 Re1 N1 75.5(4) . . ? N5 Re1 N1 82.4(5) . . ? C1 Re1' N5 108.8(9) . . ? C1 Re1' C2 90.8(7) . . ? N5 Re1' C2 99.8(6) . . ? C1 Re1' N1 101.8(6) . . ? N5 Re1' N1 91.0(5) . . ? C2 Re1' N1 159.9(6) . . ? C1 Re1' C3 83.7(9) . . ? N5 Re1' C3 167.5(6) . . ? C2 Re1' C3 78.4(7) . . ? N1 Re1' C3 87.4(5) . . ? C1 Re1' N2 164.2(8) . . ? N5 Re1' N2 86.1(5) . . ? C2 Re1' N2 91.9(6) . . ? N1 Re1' N2 71.9(4) . . ? C3 Re1' N2 81.6(5) . . ? F16 P1 F11 89.9(9) . . ? F16 P1 F14 176.4(7) . . ? F11 P1 F14 88.7(7) . . ? F16 P1 F12 91.3(6) . . ? F11 P1 F12 91.7(7) . . ? F14 P1 F12 91.9(6) . . ? F16 P1 F13 90.5(10) . . ? F11 P1 F13 178.9(7) . . ? F14 P1 F13 90.9(8) . . ? F12 P1 F13 89.3(8) . . ? F16 P1 F15 87.0(6) . . ? F11 P1 F15 89.0(7) . . ? F14 P1 F15 89.8(6) . . ? F12 P1 F15 178.2(7) . . ? F13 P1 F15 90.0(7) . . ? F23 P2 F26 92.6(9) . . ? F23 P2 F21 92.0(10) . . ? F26 P2 F21 91.4(9) . . ? F23 P2 F25 176.7(9) . . ? F26 P2 F25 90.3(8) . . ? F21 P2 F25 89.4(10) . . ? F23 P2 F22 91.4(8) . . ? F26 P2 F22 89.8(7) . . ? F21 P2 F22 176.3(9) . . ? F25 P2 F22 87.1(8) . . ? F23 P2 F24 88.6(8) . . ? F26 P2 F24 178.2(8) . . ? F21 P2 F24 90.0(9) . . ? F25 P2 F24 88.5(8) . . ? F22 P2 F24 88.8(6) . . ? F34 P3 F31 87.6(8) . . ? F34 P3 F35 175.1(13) . . ? F31 P3 F35 94.2(11) . . ? F34 P3 F33 89.7(15) . . ? F31 P3 F33 92.3(13) . . ? F35 P3 F33 85.6(13) . . ? F34 P3 F36 93.1(17) . . ? F31 P3 F36 87.7(10) . . ? F35 P3 F36 91.5(16) . . ? F33 P3 F36 177.2(17) . . ? F34 P3 F32 91.6(8) . . ? F31 P3 F32 175.7(11) . . ? F35 P3 F32 87.0(10) . . ? F33 P3 F32 91.9(12) . . ? F36 P3 F32 88.0(11) . . ? C11 N1 C15 118.6(11) . . ? C11 N1 Re1' 121.6(10) . . ? C15 N1 Re1' 118.8(8) . . ? C11 N1 Re1 127.1(10) . . ? C15 N1 Re1 114.3(8) . . ? Re1' N1 Re1 10.75(10) . . ? C16 N2 C20 118.8(10) . . ? C16 N2 Re1 117.5(8) . . ? C20 N2 Re1 123.6(9) . . ? C16 N2 Re1' 115.0(8) . . ? C20 N2 Re1' 125.7(9) . . ? Re1 N2 Re1' 9.21(9) . . ? C36 N3 C32 111.6(11) . . ? C36 N3 C34 112.0(13) . . ? C32 N3 C34 109.1(13) . . ? C36 N3 C31 107.4(12) . . ? C32 N3 C31 110.2(13) . . ? C34 N3 C31 106.5(10) . . ? C41 N4 C46 108.7(11) . . ? C41 N4 C42 107.5(11) . . ? C46 N4 C42 112.5(12) . . ? C41 N4 C44 112.1(11) . . ? C46 N4 C44 108.7(11) . . ? C42 N4 C44 107.4(11) . . ? C4 N5 Re1' 174.2(14) . . ? C4 N5 Re1 175.0(13) . . ? Re1' N5 Re1 6.56(11) . . ? O1 C1 Re1' 173(2) . . ? O1 C1 Re1 175(2) . . ? Re1' C1 Re1 11.59(19) . . ? O2 C2 Re1 177.6(15) . . ? O2 C2 Re1' 170.1(16) . . ? Re1 C2 Re1' 11.86(13) . . ? O3 C3 Re1 177.6(16) . . ? O3 C3 Re1' 172.4(16) . . ? Re1 C3 Re1' 5.27(12) . . ? N5 C4 C5 175.9(19) . . ? N1 C11 C12 123.3(14) . . ? N1 C11 H11A 118.4 . . ? C12 C11 H11A 118.4 . . ? C11 C12 C13 120.4(14) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C14 C13 C12 117.4(15) . . ? C14 C13 C31 117.8(13) . . ? C12 C13 C31 124.8(13) . . ? C13 C14 C15 119.8(14) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? N1 C15 C14 120.4(11) . . ? N1 C15 C16 117.9(11) . . ? C14 C15 C16 121.6(12) . . ? N2 C16 C17 119.9(11) . . ? N2 C16 C15 114.7(11) . . ? C17 C16 C15 125.3(12) . . ? C18 C17 C16 121.3(12) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C19 119.4(12) . . ? C17 C18 C41 119.2(12) . . ? C19 C18 C41 121.3(11) . . ? C20 C19 C18 117.8(11) . . ? C20 C19 H19A 121.1 . . ? C18 C19 H19A 121.1 . . ? N2 C20 C19 122.8(12) . . ? N2 C20 H20A 118.6 . . ? C19 C20 H20A 118.6 . . ? N3 C31 C13 116.1(12) . . ? N3 C31 H31A 108.3 . . ? C13 C31 H31A 108.3 . . ? N3 C31 H31B 108.3 . . ? C13 C31 H31B 108.3 . . ? H31A C31 H31B 107.4 . . ? N3 C32 C33 116.1(16) . . ? N3 C32 H32A 108.3 . . ? C33 C32 H32A 108.3 . . ? N3 C32 H32B 108.3 . . ? C33 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 C35 115.4(12) . . ? N3 C34 H34A 108.4 . . ? C35 C34 H34A 108.4 . . ? N3 C34 H34B 108.4 . . ? C35 C34 H34B 108.4 . . ? H34A C34 H34B 107.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 C37 115.5(12) . . ? N3 C36 H36A 108.4 . . ? C37 C36 H36A 108.4 . . ? N3 C36 H36B 108.4 . . ? C37 C36 H36B 108.4 . . ? H36A C36 H36B 107.5 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C41 C18 114.8(10) . . ? N4 C41 H41A 108.6 . . ? C18 C41 H41A 108.6 . . ? N4 C41 H41B 108.6 . . ? C18 C41 H41B 108.6 . . ? H41A C41 H41B 107.5 . . ? C43 C42 N4 116.1(13) . . ? C43 C42 H42A 108.3 . . ? N4 C42 H42A 108.3 . . ? C43 C42 H42B 108.3 . . ? N4 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 N4 116.5(13) . . ? C45 C44 H44A 108.2 . . ? N4 C44 H44A 108.2 . . ? C45 C44 H44B 108.2 . . ? N4 C44 H44B 108.2 . . ? H44A C44 H44B 107.3 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N4 C46 C47 115.2(14) . . ? N4 C46 H46A 108.5 . . ? C47 C46 H46A 108.5 . . ? N4 C46 H46B 108.5 . . ? C47 C46 H46B 108.5 . . ? H46A C46 H46B 107.5 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C02 C01 H01A 109.5 . . ? C02 C01 H01B 109.5 . . ? H01A C01 H01B 109.5 . . ? C02 C01 H01C 109.5 . . ? H01A C01 H01C 109.5 . . ? H01B C01 H01C 109.5 . . ? N01 C02 C01 173(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.69 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.864 _refine_diff_density_min -2.208 _refine_diff_density_rms 0.212