# 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 'James Crowley' _publ_contact_author_email jcrowley@chemistry.otago.ac.nz loop_ _publ_author_name 'James Crowley' 'Keith Gordon' 'Christopher Anderson' 'Anastasia Elliott' 'James Lewis' 'C John McAdam' # Attachment 'cba65.cif' data_cba65 _database_code_depnum_ccdc_archive 'CCDC 885824' #TrackingRef 'cba65.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H19 F6 N7 O3 P Re' _chemical_formula_weight 808.65 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)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3982(10) _cell_length_b 13.1939(10) _cell_length_c 18.7735(16) _cell_angle_alpha 90.00 _cell_angle_beta 99.246(3) _cell_angle_gamma 90.00 _cell_volume 2786.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9876 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.35 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 4.502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4817 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33919 _diffrn_reflns_av_R_equivalents 0.1076 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.38 _reflns_number_total 5694 _reflns_number_gt 4764 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DELU command was used to restrain the anisotropic displacement parameter of one of the carbonyl carbon atoms (C31) to be more similar to the rhenium (Re1) and oxygen atoms (O31) to which it is bonded. ; _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^)+(0.0404P)^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 5694 _refine_ls_number_parameters 397 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.620792(14) 0.192098(11) 0.748911(9) 0.01044(7) Uani 1 1 d U . . C1 C 0.3230(4) 0.6258(3) 0.7969(2) 0.0196(10) Uani 1 1 d . . . H1 H 0.3332 0.6128 0.8473 0.024 Uiso 1 1 calc R . . C2 C 0.2646(4) 0.7137(3) 0.7688(3) 0.0218(11) Uani 1 1 d . . . H2 H 0.2364 0.7608 0.8003 0.026 Uiso 1 1 calc R . . C3 C 0.2475(4) 0.7325(3) 0.6956(2) 0.0191(10) Uani 1 1 d . . . H3 H 0.2089 0.7929 0.6768 0.023 Uiso 1 1 calc R . . C4 C 0.2871(4) 0.6626(3) 0.6496(2) 0.0170(10) Uani 1 1 d . . . H4 H 0.2729 0.6741 0.5989 0.020 Uiso 1 1 calc R . . C5 C 0.3474(4) 0.5762(3) 0.6770(2) 0.0140(9) Uani 1 1 d . . . H5 H 0.3760 0.5295 0.6453 0.017 Uiso 1 1 calc R . . C6 C 0.3660(3) 0.5578(3) 0.7510(2) 0.0134(9) Uani 1 1 d . . . C7 C 0.4338(4) 0.4679(3) 0.7801(2) 0.0124(9) Uani 1 1 d . . . C8 C 0.4791(3) 0.4438(3) 0.8511(2) 0.0116(9) Uani 1 1 d . . . H8 H 0.4702 0.4811 0.8932 0.014 Uiso 1 1 calc R . . C9 C 0.6081(4) 0.2978(3) 0.9060(2) 0.0136(9) Uani 1 1 d . . . H9A H 0.5771 0.2277 0.9059 0.016 Uiso 1 1 calc R . . H9B H 0.6013 0.3291 0.9531 0.016 Uiso 1 1 calc R . . C10 C 0.7363(4) 0.2957(3) 0.8959(2) 0.0119(9) Uani 1 1 d . . . C11 C 0.8206(4) 0.3412(3) 0.9474(2) 0.0163(10) Uani 1 1 d . . . H11 H 0.7981 0.3689 0.9899 0.020 Uiso 1 1 calc R . . C12 C 0.9371(4) 0.3461(3) 0.9367(2) 0.0202(10) Uani 1 1 d . . . H12 H 0.9967 0.3745 0.9722 0.024 Uiso 1 1 calc R . . C13 C 0.9649(4) 0.3083(3) 0.8723(2) 0.0164(10) Uani 1 1 d . . . H13 H 1.0440 0.3127 0.8625 0.020 Uiso 1 1 calc R . . C14 C 0.8771(4) 0.2641(3) 0.8227(2) 0.0129(9) Uani 1 1 d . . . C15 C 0.9057(4) 0.2325(3) 0.7506(2) 0.0142(9) Uani 1 1 d . . . H15A H 0.9913 0.2430 0.7493 0.017 Uiso 1 1 calc R . . H15B H 0.8876 0.1596 0.7424 0.017 Uiso 1 1 calc R . . C16 C 0.8693(4) 0.3630(3) 0.6494(2) 0.0154(9) Uani 1 1 d . . . H16 H 0.9484 0.3808 0.6445 0.018 Uiso 1 1 calc R . . C17 C 0.7647(4) 0.4031(3) 0.6124(2) 0.0130(9) Uani 1 1 d . . . C18 C 0.7469(4) 0.4829(3) 0.5569(2) 0.0151(9) Uani 1 1 d . . . C19 C 0.8328(4) 0.5046(4) 0.5152(2) 0.0225(11) Uani 1 1 d . . . H19 H 0.9053 0.4676 0.5222 0.027 Uiso 1 1 calc R . . C20 C 0.8146(4) 0.5800(4) 0.4630(2) 0.0256(11) Uani 1 1 d . . . H20 H 0.8753 0.5958 0.4356 0.031 Uiso 1 1 calc R . . C21 C 0.7086(4) 0.6318(3) 0.4510(2) 0.0223(11) Uani 1 1 d . . . H21 H 0.6957 0.6830 0.4151 0.027 Uiso 1 1 calc R . . C22 C 0.6209(4) 0.6092(3) 0.4914(2) 0.0223(11) Uani 1 1 d . . . H22 H 0.5470 0.6441 0.4825 0.027 Uiso 1 1 calc R . . C23 C 0.6398(4) 0.5366(3) 0.5444(2) 0.0175(10) Uani 1 1 d . . . H23 H 0.5798 0.5227 0.5727 0.021 Uiso 1 1 calc R . . C31 C 0.5026(4) 0.1613(3) 0.6666(3) 0.0168(10) Uani 1 1 d U . . O31 O 0.4341(3) 0.1437(2) 0.61636(16) 0.0243(8) Uani 1 1 d U . . C32 C 0.5325(4) 0.1084(3) 0.8054(2) 0.0150(9) Uani 1 1 d . . . O32 O 0.4761(3) 0.0561(2) 0.83582(17) 0.0222(7) Uani 1 1 d . . . C33 C 0.7014(4) 0.0694(3) 0.7284(2) 0.0165(9) Uani 1 1 d . . . O33 O 0.7442(3) -0.0065(2) 0.71614(16) 0.0196(7) Uani 1 1 d . . . N1 N 0.4677(3) 0.3944(2) 0.73662(18) 0.0119(7) Uani 1 1 d . . . N2 N 0.5315(3) 0.3278(2) 0.77808(19) 0.0126(8) Uani 1 1 d . . . N3 N 0.5381(3) 0.3562(2) 0.84746(17) 0.0099(7) Uani 1 1 d . . . N4 N 0.7633(3) 0.2544(2) 0.83468(18) 0.0129(8) Uani 1 1 d . . . N5 N 0.8340(3) 0.2934(2) 0.69386(19) 0.0136(8) Uani 1 1 d . . . N6 N 0.7152(3) 0.2900(2) 0.68576(19) 0.0121(8) Uani 1 1 d . . . N7 N 0.6718(3) 0.3574(3) 0.63580(18) 0.0135(8) Uani 1 1 d . . . P1 P 0.79622(10) 0.11953(8) 0.51133(6) 0.0161(3) Uani 1 1 d . . . F1 F 0.8711(3) 0.1377(2) 0.58926(15) 0.0475(9) Uani 1 1 d . . . F2 F 0.7277(2) 0.22444(19) 0.51632(14) 0.0272(6) Uani 1 1 d . . . F3 F 0.8936(3) 0.17713(19) 0.47468(19) 0.0371(8) Uani 1 1 d . . . F4 F 0.6957(3) 0.0626(2) 0.54646(17) 0.0432(8) Uani 1 1 d . . . F5 F 0.8651(2) 0.01363(18) 0.50508(13) 0.0235(6) Uani 1 1 d . . . F6 F 0.7208(2) 0.0996(2) 0.43305(14) 0.0345(7) 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 0.01137(10) 0.00752(10) 0.01118(11) 0.00036(7) -0.00198(7) 0.00052(6) C1 0.020(2) 0.018(2) 0.020(2) 0.004(2) -0.0004(19) 0.0061(19) C2 0.021(3) 0.016(2) 0.028(3) -0.004(2) 0.004(2) 0.0072(19) C3 0.017(2) 0.013(2) 0.027(3) 0.006(2) 0.004(2) 0.0039(18) C4 0.019(2) 0.017(2) 0.015(2) 0.0040(19) -0.0004(19) -0.0008(18) C5 0.015(2) 0.010(2) 0.016(2) -0.0023(18) -0.0002(18) -0.0008(17) C6 0.009(2) 0.012(2) 0.019(2) -0.0003(18) 0.0013(17) -0.0017(16) C7 0.011(2) 0.011(2) 0.015(2) -0.0037(18) 0.0000(17) -0.0024(16) C8 0.011(2) 0.0070(19) 0.016(2) -0.0018(17) 0.0004(17) -0.0019(16) C9 0.014(2) 0.014(2) 0.010(2) 0.0032(18) -0.0053(17) 0.0032(17) C10 0.015(2) 0.0071(19) 0.012(2) 0.0031(17) -0.0034(17) 0.0034(16) C11 0.020(2) 0.014(2) 0.012(2) -0.0024(19) -0.0052(18) 0.0041(18) C12 0.017(2) 0.019(2) 0.021(3) -0.001(2) -0.0090(19) 0.0031(19) C13 0.010(2) 0.018(2) 0.020(2) 0.0004(19) -0.0037(18) 0.0032(17) C14 0.012(2) 0.010(2) 0.015(2) 0.0032(18) -0.0012(17) 0.0037(17) C15 0.011(2) 0.016(2) 0.015(2) -0.0004(18) -0.0009(17) 0.0012(17) C16 0.018(2) 0.012(2) 0.017(2) -0.0020(19) 0.0040(18) -0.0035(18) C17 0.018(2) 0.009(2) 0.012(2) -0.0035(17) 0.0011(17) -0.0012(17) C18 0.020(2) 0.012(2) 0.010(2) -0.0031(18) -0.0036(18) -0.0046(18) C19 0.023(3) 0.025(3) 0.019(2) 0.004(2) 0.002(2) 0.006(2) C20 0.034(3) 0.028(3) 0.015(2) 0.003(2) 0.006(2) -0.002(2) C21 0.035(3) 0.017(2) 0.012(2) -0.001(2) -0.005(2) -0.001(2) C22 0.027(3) 0.013(2) 0.024(3) -0.004(2) -0.006(2) 0.0006(19) C23 0.022(2) 0.013(2) 0.017(2) -0.0017(19) 0.0017(19) -0.0070(18) C31 0.022(2) 0.0026(19) 0.027(3) 0.0011(19) 0.006(2) 0.0040(17) O31 0.0206(17) 0.0273(19) 0.0213(18) -0.0046(15) -0.0075(14) -0.0044(14) C32 0.014(2) 0.012(2) 0.017(2) -0.0041(19) -0.0029(18) 0.0028(18) O32 0.0189(17) 0.0179(16) 0.0310(19) 0.0083(15) 0.0080(15) 0.0029(14) C33 0.018(2) 0.024(2) 0.007(2) 0.0046(19) -0.0006(18) 0.0007(19) O33 0.0278(18) 0.0107(15) 0.0203(17) 0.0003(14) 0.0036(14) 0.0060(14) N1 0.0111(17) 0.0094(17) 0.0131(18) 0.0034(15) -0.0040(14) 0.0002(14) N2 0.0165(19) 0.0109(17) 0.0087(18) 0.0001(15) -0.0030(15) 0.0029(14) N3 0.0106(17) 0.0099(17) 0.0068(17) -0.0025(15) -0.0054(13) -0.0018(14) N4 0.0121(18) 0.0108(18) 0.0141(19) 0.0043(15) -0.0035(14) 0.0022(14) N5 0.0123(18) 0.0132(18) 0.0144(19) -0.0014(15) -0.0010(15) 0.0007(14) N6 0.0134(18) 0.0116(17) 0.0103(18) -0.0039(15) -0.0006(15) -0.0021(14) N7 0.0156(19) 0.0133(18) 0.0103(18) -0.0026(16) -0.0016(15) 0.0008(15) P1 0.0206(6) 0.0135(6) 0.0139(6) 0.0012(5) 0.0018(5) 0.0033(5) F1 0.067(2) 0.044(2) 0.0225(16) -0.0136(15) -0.0205(15) 0.0259(17) F2 0.0348(17) 0.0186(13) 0.0291(16) 0.0006(12) 0.0084(13) 0.0102(12) F3 0.0309(17) 0.0242(15) 0.062(2) -0.0002(14) 0.0253(16) -0.0047(13) F4 0.049(2) 0.0276(16) 0.060(2) 0.0127(16) 0.0310(17) 0.0056(14) F5 0.0262(15) 0.0183(14) 0.0240(15) -0.0011(12) -0.0026(12) 0.0100(11) F6 0.0346(17) 0.0310(16) 0.0312(16) -0.0079(13) -0.0153(13) 0.0118(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C32 1.922(5) . ? Re1 C31 1.924(5) . ? Re1 C33 1.930(5) . ? Re1 N6 2.155(4) . ? Re1 N2 2.173(3) . ? Re1 N4 2.251(3) . ? C1 C6 1.387(6) . ? C1 C2 1.397(6) . ? C2 C3 1.379(6) . ? C3 C4 1.388(6) . ? C4 C5 1.387(6) . ? C5 C6 1.393(6) . ? C6 C7 1.472(6) . ? C7 N1 1.363(5) . ? C7 C8 1.386(6) . ? C8 N3 1.344(5) . ? C9 N3 1.469(5) . ? C9 C10 1.503(6) . ? C10 N4 1.352(5) . ? C10 C11 1.385(6) . ? C11 C12 1.376(6) . ? C12 C13 1.390(6) . ? C13 C14 1.382(6) . ? C14 N4 1.358(5) . ? C14 C15 1.502(6) . ? C15 N5 1.473(5) . ? C16 N5 1.345(5) . ? C16 C17 1.385(6) . ? C17 N7 1.352(5) . ? C17 C18 1.473(6) . ? C18 C19 1.378(6) . ? C18 C23 1.398(6) . ? C19 C20 1.388(6) . ? C20 C21 1.375(6) . ? C21 C22 1.381(7) . ? C22 C23 1.373(6) . ? C31 O31 1.147(5) . ? C32 O32 1.156(5) . ? C33 O33 1.154(5) . ? N1 N2 1.313(4) . ? N2 N3 1.346(5) . ? N5 N6 1.339(5) . ? N6 N7 1.329(5) . ? P1 F1 1.589(3) . ? P1 F3 1.590(3) . ? P1 F4 1.598(3) . ? P1 F2 1.600(3) . ? P1 F6 1.601(3) . ? P1 F5 1.616(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C32 Re1 C31 87.75(18) . . ? C32 Re1 C33 86.36(17) . . ? C31 Re1 C33 87.57(17) . . ? C32 Re1 N6 177.99(15) . . ? C31 Re1 N6 91.82(16) . . ? C33 Re1 N6 95.58(16) . . ? C32 Re1 N2 91.52(15) . . ? C31 Re1 N2 94.62(15) . . ? C33 Re1 N2 176.90(15) . . ? N6 Re1 N2 86.56(13) . . ? C32 Re1 N4 101.35(15) . . ? C31 Re1 N4 169.63(15) . . ? C33 Re1 N4 97.87(15) . . ? N6 Re1 N4 78.92(13) . . ? N2 Re1 N4 80.31(12) . . ? C6 C1 C2 119.8(4) . . ? C3 C2 C1 120.5(4) . . ? C2 C3 C4 119.5(4) . . ? C5 C4 C3 120.4(4) . . ? C4 C5 C6 120.0(4) . . ? C1 C6 C5 119.6(4) . . ? C1 C6 C7 120.6(4) . . ? C5 C6 C7 119.8(4) . . ? N1 C7 C8 108.4(3) . . ? N1 C7 C6 122.3(4) . . ? C8 C7 C6 129.3(4) . . ? N3 C8 C7 105.1(4) . . ? N3 C9 C10 109.7(3) . . ? N4 C10 C11 122.7(4) . . ? N4 C10 C9 118.2(4) . . ? C11 C10 C9 118.9(4) . . ? C12 C11 C10 119.7(4) . . ? C11 C12 C13 118.1(4) . . ? C14 C13 C12 119.7(4) . . ? N4 C14 C13 122.4(4) . . ? N4 C14 C15 118.3(4) . . ? C13 C14 C15 119.1(4) . . ? N5 C15 C14 108.9(3) . . ? N5 C16 C17 104.6(4) . . ? N7 C17 C16 108.8(4) . . ? N7 C17 C18 121.5(4) . . ? C16 C17 C18 129.6(4) . . ? C19 C18 C23 118.7(4) . . ? C19 C18 C17 121.4(4) . . ? C23 C18 C17 119.9(4) . . ? C18 C19 C20 120.7(4) . . ? C21 C20 C19 120.0(5) . . ? C20 C21 C22 119.8(4) . . ? C23 C22 C21 120.3(4) . . ? C22 C23 C18 120.4(4) . . ? O31 C31 Re1 178.2(4) . . ? O32 C32 Re1 176.3(4) . . ? O33 C33 Re1 176.5(4) . . ? N2 N1 C7 107.7(3) . . ? N1 N2 N3 109.1(3) . . ? N1 N2 Re1 129.7(3) . . ? N3 N2 Re1 121.2(2) . . ? C8 N3 N2 109.7(3) . . ? C8 N3 C9 129.0(3) . . ? N2 N3 C9 121.2(3) . . ? C10 N4 C14 117.2(3) . . ? C10 N4 Re1 121.3(3) . . ? C14 N4 Re1 121.0(3) . . ? N6 N5 C16 110.5(3) . . ? N6 N5 C15 119.8(3) . . ? C16 N5 C15 129.4(4) . . ? N7 N6 N5 108.2(3) . . ? N7 N6 Re1 128.8(3) . . ? N5 N6 Re1 122.9(3) . . ? N6 N7 C17 107.8(3) . . ? F1 P1 F3 90.98(19) . . ? F1 P1 F4 90.33(19) . . ? F3 P1 F4 178.48(19) . . ? F1 P1 F2 90.60(15) . . ? F3 P1 F2 89.60(15) . . ? F4 P1 F2 89.61(16) . . ? F1 P1 F6 179.22(17) . . ? F3 P1 F6 89.47(18) . . ? F4 P1 F6 89.23(18) . . ? F2 P1 F6 90.04(15) . . ? F1 P1 F5 90.13(15) . . ? F3 P1 F5 90.06(15) . . ? F4 P1 F5 90.70(15) . . ? F2 P1 F5 179.21(15) . . ? F6 P1 F5 89.24(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.810 _refine_diff_density_min -2.078 _refine_diff_density_rms 0.270 # Attachment 'CBA_234.cif' data_cba_234 _database_code_depnum_ccdc_archive 'CCDC 885825' #TrackingRef 'CBA_234.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H23 F6 N7 O3 P Re' _chemical_formula_weight 740.62 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)/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 22.534(5) _cell_length_b 10.528(2) _cell_length_c 22.827(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.892(10) _cell_angle_gamma 90.00 _cell_volume 5025(2) _cell_formula_units_Z 8 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 9841 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.78 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.958 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 4.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2029 _exptl_absorpt_correction_T_max 0.4209 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 128737 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 26.65 _reflns_number_total 10344 _reflns_number_gt 8904 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997), Mercury (Macrae et al., 2008)' _computing_publication_material "SHELXL-97, enCIFer (Allen et al., 2004), PLATON (Spek, 2009), PublCIF (Westrip 2010)'" _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. Two of the propyl arms (C15, C16 & C17 and C51, C52 & C53) contained anisotropic ellipsoids that suggested certain atoms (C16, C52 and C53) could be split into two separate disordered parts. In the case of one of the arms (C17, C16 & C15) the terminal and pivotal carbon atoms (C17 and C15) were ordered, with the central carbon atom (C16) disordered over two sites. In the case of the other arm (C51, C52 and C53) the terminal carbon atom (C51) was ordered with the remaining two carbon atoms each disordered over two sites. Despite modelling of this disorder resulting in more similar Ueq values for adjacent atoms, the bonding angles between the carbon atoms of the propyl arm do not form ideal tetrahedral geometries. Given the unequivocal identity of this moiety, attempts to restrain the data to give a more aesthetically pleasing model were deemed unnecessary. Although the hexafluorophosphate (PF6-) anions were identified and attempts were made to model them, NPD atoms were observed. After attempts to impose restraints failed, SQUEEZE was used to eliminate the counterions and other diffuse disordered solvent molecules. See below for full SQUEEZE details. DELU command was used to restrain the anisotropic displacement parameters of the carbonyl atoms C22 and O22 to be more similar. The largest remaining residual density peak has a value of 4.205. This is located in a void space and is presumed to be residual density from diffuse solvent molecules that were located too close to the cationic portion of the structure to be affected by SQUEEZE. As such no serious attempts to model it were undertaken. ; _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^)+(0.0502P)^2^+26.1912P] 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 10344 _refine_ls_number_parameters 586 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.200168(11) 0.23645(2) 0.555601(11) 0.01491(8) Uani 1 1 d . . . C20 C 0.2913(3) 0.2310(6) 0.5907(3) 0.0202(13) Uani 1 1 d . . . O20 O 0.3458(2) 0.2319(4) 0.6097(2) 0.0251(10) Uani 1 1 d . . . C21 C 0.1954(3) 0.1120(6) 0.6154(3) 0.0199(13) Uani 1 1 d . . . O21 O 0.1922(2) 0.0436(4) 0.6541(2) 0.0267(10) Uani 1 1 d . . . C22 C 0.2063(3) 0.3532(6) 0.6229(3) 0.0206(13) Uani 1 1 d U . . O22 O 0.2134(2) 0.4135(5) 0.6674(2) 0.0337(12) Uani 1 1 d U . . C1 C 0.2475(4) 0.3535(10) 0.3233(4) 0.053(3) Uani 1 1 d . . . H1A H 0.2724 0.2896 0.3112 0.064 Uiso 1 1 calc R . . H1B H 0.2178 0.3954 0.2853 0.064 Uiso 1 1 calc R . . H1C H 0.2233 0.3124 0.3458 0.064 Uiso 1 1 calc R . . C2 C 0.2928(4) 0.4526(8) 0.3663(4) 0.0365(17) Uani 1 1 d . . . H2A H 0.3229 0.4094 0.4043 0.044 Uiso 1 1 calc R . . H2B H 0.3183 0.4913 0.3437 0.044 Uiso 1 1 calc R . . C3 C 0.2586(3) 0.5568(7) 0.3868(3) 0.0323(16) Uani 1 1 d . . . H3A H 0.2904 0.6194 0.4126 0.039 Uiso 1 1 calc R . . H3B H 0.2290 0.6012 0.3490 0.039 Uiso 1 1 calc R . . C4 C 0.2217(3) 0.5062(6) 0.4243(3) 0.0222(13) Uani 1 1 d . . . C5 C 0.1665(3) 0.5490(6) 0.4282(3) 0.0225(13) Uani 1 1 d . . . H5 H 0.1413 0.6188 0.4063 0.027 Uiso 1 1 calc R . . C6 C 0.1056(3) 0.4791(6) 0.4959(3) 0.0196(13) Uani 1 1 d . . . H6A H 0.0781 0.5541 0.4787 0.023 Uiso 1 1 calc R . . H6B H 0.1255 0.4883 0.5424 0.023 Uiso 1 1 calc R . . C7 C 0.0658(3) 0.3602(6) 0.4795(3) 0.0177(12) Uani 1 1 d . . . C8 C 0.0006(3) 0.3705(7) 0.4461(3) 0.0219(13) Uani 1 1 d . . . H8 H -0.0189 0.4515 0.4346 0.026 Uiso 1 1 calc R . . C9 C -0.0357(3) 0.2602(6) 0.4296(3) 0.0245(15) Uani 1 1 d . . . H9 H -0.0809 0.2643 0.4092 0.029 Uiso 1 1 calc R . . C10 C -0.0044(3) 0.1434(7) 0.4438(3) 0.0227(14) Uani 1 1 d . . . H10 H -0.0278 0.0667 0.4306 0.027 Uiso 1 1 calc R . . C11 C 0.0606(3) 0.1402(6) 0.4769(3) 0.0187(13) Uani 1 1 d . . . C12 C 0.0953(3) 0.0147(6) 0.4886(3) 0.0186(13) Uani 1 1 d . A . H12A H 0.1150 -0.0014 0.5346 0.022 Uiso 1 1 calc R . . H12B H 0.0645 -0.0546 0.4692 0.022 Uiso 1 1 calc R . . C13 C 0.1492(3) -0.0562(6) 0.4153(3) 0.0190(13) Uani 1 1 d . A . H13 H 0.1210 -0.1217 0.3926 0.023 Uiso 1 1 calc R . . C14 C 0.2032(3) -0.0138(6) 0.4078(3) 0.0189(13) Uani 1 1 d . . . N1 N 0.2417(2) 0.4031(5) 0.4626(2) 0.0185(11) Uani 1 1 d . . . N2 N 0.2013(2) 0.3838(5) 0.4898(2) 0.0186(11) Uani 1 1 d . . . N3 N 0.1552(2) 0.4722(5) 0.4694(2) 0.0164(10) Uani 1 1 d . . . N4 N 0.0954(2) 0.2469(5) 0.4974(2) 0.0168(11) Uani 1 1 d . . . N5 N 0.1449(2) 0.0154(5) 0.4619(2) 0.0172(10) Uani 1 1 d . . . N6 N 0.1932(2) 0.0992(5) 0.4822(2) 0.0174(10) Uani 1 1 d . A . N7 N 0.2291(2) 0.0809(5) 0.4494(2) 0.0160(10) Uani 1 1 d . A . Re2 Re 0.527475(11) 0.16951(2) 0.725354(10) 0.01621(8) Uani 1 1 d . . . C70 C 0.5961(3) 0.1996(7) 0.6966(3) 0.0224(13) Uani 1 1 d . . . O70 O 0.6353(2) 0.2179(5) 0.6781(2) 0.0332(12) Uani 1 1 d . . . C71 C 0.5668(3) 0.0091(6) 0.7578(3) 0.0212(13) Uani 1 1 d . . . O71 O 0.5936(2) -0.0849(5) 0.7765(2) 0.0298(11) Uani 1 1 d . . . C72 C 0.5772(3) 0.2335(6) 0.8080(3) 0.0201(13) Uani 1 1 d . . . O72 O 0.6071(2) 0.2649(4) 0.8589(2) 0.0280(11) Uani 1 1 d . . . C54 C 0.4399(6) 0.4996(10) 0.6214(5) 0.076(4) Uani 1 1 d . . . C55 C 0.4236(5) 0.5159(8) 0.6732(4) 0.058(3) Uani 1 1 d . B . H55 H 0.3980 0.5816 0.6801 0.070 Uiso 1 1 calc R . . C56 C 0.4470(3) 0.3816(6) 0.7720(3) 0.0240(14) Uani 1 1 d . . . H56A H 0.4236 0.4469 0.7859 0.029 Uiso 1 1 calc R . . H56B H 0.4905 0.3732 0.8048 0.029 Uiso 1 1 calc R . . C57 C 0.4124(3) 0.2562(6) 0.7631(3) 0.0210(14) Uani 1 1 d . . . C58 C 0.3564(3) 0.2483(6) 0.7740(3) 0.0190(13) Uani 1 1 d . . . H58 H 0.3411 0.3199 0.7895 0.023 Uiso 1 1 calc R . . C59 C 0.3229(3) 0.1365(7) 0.7624(3) 0.0236(14) Uani 1 1 d . . . H59 H 0.2855 0.1281 0.7720 0.028 Uiso 1 1 calc R . . C60 C 0.3443(3) 0.0364(6) 0.7368(3) 0.0211(13) Uani 1 1 d . . . H60 H 0.3209 -0.0408 0.7269 0.025 Uiso 1 1 calc R . . C61 C 0.4001(3) 0.0497(6) 0.7257(3) 0.0177(12) Uani 1 1 d . . . C62 C 0.4196(3) -0.0555(6) 0.6915(3) 0.0194(13) Uani 1 1 d . . . H62A H 0.4609 -0.0920 0.7197 0.023 Uiso 1 1 calc R . . H62B H 0.3871 -0.1239 0.6806 0.023 Uiso 1 1 calc R . . C63 C 0.3944(3) -0.0421(6) 0.5730(3) 0.0204(13) Uani 1 1 d . . . H63 H 0.3609 -0.1028 0.5573 0.024 Uiso 1 1 calc R . . C64 C 0.4208(3) 0.0292(6) 0.5386(3) 0.0187(13) Uani 1 1 d . . . C65 C 0.4077(3) 0.0261(7) 0.4692(3) 0.0247(14) Uani 1 1 d . . . H65A H 0.3705 -0.0300 0.4482 0.030 Uiso 1 1 calc R . . H65B H 0.4451 -0.0110 0.4627 0.030 Uiso 1 1 calc R . . C66 C 0.3938(4) 0.1579(7) 0.4380(3) 0.0353(17) Uani 1 1 d . . . H66A H 0.4266 0.2190 0.4636 0.042 Uiso 1 1 calc R . . H66B H 0.3515 0.1881 0.4362 0.042 Uiso 1 1 calc R . . C67 C 0.3942(4) 0.1513(8) 0.3706(3) 0.0398(19) Uani 1 1 d . . . H67A H 0.3852 0.2357 0.3512 0.048 Uiso 1 1 calc R . . H67B H 0.3613 0.0915 0.3453 0.048 Uiso 1 1 calc R . . H67C H 0.4362 0.1225 0.3726 0.048 Uiso 1 1 calc R . . N51 N 0.4783(4) 0.3978(6) 0.6315(3) 0.0420(17) Uani 1 1 d . . . N52 N 0.4840(2) 0.3485(5) 0.6857(3) 0.0238(12) Uani 1 1 d . . . N53 N 0.4514(3) 0.4197(5) 0.7120(3) 0.0240(12) Uani 1 1 d . B . N54 N 0.4360(2) 0.1566(5) 0.7413(2) 0.0165(10) Uani 1 1 d . . . N55 N 0.4260(2) -0.0079(5) 0.6337(2) 0.0170(10) Uani 1 1 d . . . N56 N 0.4688(2) 0.0830(5) 0.6369(2) 0.0173(10) Uani 1 1 d . . . N57 N 0.4662(2) 0.1055(5) 0.5790(2) 0.0211(11) Uani 1 1 d . . . C15A C 0.2308(3) -0.0568(7) 0.3608(3) 0.0311(16) Uani 0.60 1 d P A 1 H15A H 0.2671 -0.1148 0.3819 0.037 Uiso 0.60 1 calc PR A 1 H15B H 0.2475 0.0178 0.3455 0.037 Uiso 0.60 1 calc PR A 1 C16A C 0.1816(5) -0.1249(11) 0.3045(5) 0.026(2) Uani 0.60 1 d P A 1 H16A H 0.2042 -0.1653 0.2795 0.031 Uiso 0.60 1 calc PR A 1 H16B H 0.1616 -0.1934 0.3205 0.031 Uiso 0.60 1 calc PR A 1 C17A C 0.1297(4) -0.0405(9) 0.2615(4) 0.043(2) Uani 0.60 1 d P A 1 H17A H 0.1006 -0.0910 0.2265 0.052 Uiso 0.60 1 calc PR A 1 H17B H 0.1489 0.0270 0.2448 0.052 Uiso 0.60 1 calc PR A 1 H17C H 0.1058 -0.0027 0.2853 0.052 Uiso 0.60 1 calc PR A 1 C15B C 0.2308(3) -0.0568(7) 0.3608(3) 0.0311(16) Uani 0.40 1 d P A 2 H15C H 0.2281 -0.1505 0.3569 0.037 Uiso 0.40 1 calc PR A 2 H15D H 0.2764 -0.0321 0.3753 0.037 Uiso 0.40 1 calc PR A 2 C16B C 0.1920(9) 0.0069(19) 0.2934(9) 0.038(5) Uani 0.40 1 d P A 2 H16C H 0.1891 0.0994 0.2996 0.046 Uiso 0.40 1 calc PR A 2 H16D H 0.2169 -0.0053 0.2661 0.046 Uiso 0.40 1 calc PR A 2 C17B C 0.1297(4) -0.0405(9) 0.2615(4) 0.043(2) Uani 0.40 1 d P A 2 H17D H 0.1093 0.0061 0.2219 0.052 Uiso 0.40 1 calc PR A 2 H17E H 0.1045 -0.0297 0.2881 0.052 Uiso 0.40 1 calc PR A 2 H17F H 0.1320 -0.1309 0.2523 0.052 Uiso 0.40 1 calc PR A 2 C51A C 0.4294(4) 0.6711(9) 0.4694(4) 0.051(2) Uani 0.65 1 d P B 1 H51A H 0.4614 0.7198 0.4594 0.061 Uiso 0.65 1 calc PR B 1 H51B H 0.3917 0.7243 0.4625 0.061 Uiso 0.65 1 calc PR B 1 H51C H 0.4170 0.5961 0.4421 0.061 Uiso 0.65 1 calc PR B 1 C52A C 0.4582(5) 0.6280(12) 0.5400(6) 0.034(3) Uani 0.65 1 d P B 1 H52A H 0.4962 0.5739 0.5476 0.041 Uiso 0.65 1 calc PR B 1 H52B H 0.4711 0.7029 0.5682 0.041 Uiso 0.65 1 calc PR B 1 C53A C 0.4085(5) 0.5569(11) 0.5520(6) 0.033(3) Uani 0.65 1 d P B 1 H53A H 0.3922 0.4878 0.5207 0.039 Uiso 0.65 1 calc PR B 1 H53B H 0.3724 0.6135 0.5490 0.039 Uiso 0.65 1 calc PR B 1 C51B C 0.4294(4) 0.6711(9) 0.4694(4) 0.051(2) Uani 0.35 1 d P B 2 H51D H 0.4086 0.6462 0.4251 0.061 Uiso 0.35 1 calc PR B 2 H51E H 0.4751 0.6854 0.4793 0.061 Uiso 0.35 1 calc PR B 2 H51F H 0.4098 0.7494 0.4770 0.061 Uiso 0.35 1 calc PR B 2 C52B C 0.4204(9) 0.557(2) 0.5148(9) 0.026(4) Uani 0.35 1 d P B 2 H52C H 0.3746 0.5394 0.5052 0.032 Uiso 0.35 1 calc PR B 2 H52D H 0.4419 0.4782 0.5099 0.032 Uiso 0.35 1 calc PR B 2 C53B C 0.4534(10) 0.614(2) 0.5826(9) 0.030(5) Uani 0.35 1 d P B 2 H53C H 0.4326 0.6940 0.5880 0.036 Uiso 0.35 1 calc PR B 2 H53D H 0.4997 0.6289 0.5936 0.036 Uiso 0.35 1 calc PR 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 Re1 0.01517(12) 0.01642(13) 0.01343(12) -0.00060(9) 0.00565(9) -0.00016(9) C20 0.033(4) 0.013(3) 0.015(3) 0.000(2) 0.010(3) 0.000(3) O20 0.014(2) 0.036(3) 0.023(2) 0.003(2) 0.0044(19) 0.0013(19) C21 0.021(3) 0.021(3) 0.017(3) -0.007(3) 0.007(2) 0.000(3) O21 0.033(3) 0.027(3) 0.023(2) 0.008(2) 0.014(2) -0.001(2) C22 0.016(3) 0.022(3) 0.025(3) 0.003(3) 0.010(3) -0.001(2) O22 0.045(3) 0.035(3) 0.026(2) -0.014(2) 0.018(2) -0.003(2) C1 0.044(5) 0.090(7) 0.034(4) -0.026(5) 0.024(4) -0.018(5) C2 0.032(4) 0.046(5) 0.037(4) 0.002(4) 0.019(3) -0.003(3) C3 0.029(4) 0.040(4) 0.031(4) 0.014(3) 0.015(3) 0.001(3) C4 0.025(3) 0.017(3) 0.023(3) 0.008(3) 0.008(3) -0.003(3) C5 0.024(3) 0.021(3) 0.021(3) 0.001(3) 0.006(3) -0.002(3) C6 0.022(3) 0.017(3) 0.024(3) 0.000(2) 0.013(3) 0.004(2) C7 0.021(3) 0.022(3) 0.014(3) 0.002(2) 0.011(2) 0.002(2) C8 0.023(3) 0.030(4) 0.014(3) 0.002(3) 0.009(2) 0.005(3) C9 0.018(3) 0.038(4) 0.018(3) -0.001(3) 0.007(3) 0.004(3) C10 0.020(3) 0.036(4) 0.015(3) -0.004(3) 0.011(2) -0.008(3) C11 0.019(3) 0.026(3) 0.015(3) -0.004(2) 0.010(2) -0.006(3) C12 0.023(3) 0.019(3) 0.019(3) -0.004(2) 0.014(3) -0.007(2) C13 0.020(3) 0.016(3) 0.019(3) -0.004(2) 0.005(2) -0.005(2) C14 0.021(3) 0.017(3) 0.018(3) -0.002(2) 0.007(2) 0.005(2) N1 0.014(2) 0.025(3) 0.019(3) -0.001(2) 0.009(2) -0.003(2) N2 0.015(2) 0.018(3) 0.019(3) -0.003(2) 0.003(2) 0.001(2) N3 0.012(2) 0.019(3) 0.018(2) 0.001(2) 0.006(2) 0.001(2) N4 0.017(2) 0.022(3) 0.014(2) -0.001(2) 0.009(2) -0.001(2) N5 0.017(2) 0.018(3) 0.017(2) 0.001(2) 0.006(2) -0.001(2) N6 0.016(2) 0.013(3) 0.022(3) 0.002(2) 0.006(2) -0.001(2) N7 0.015(2) 0.017(3) 0.018(2) -0.001(2) 0.009(2) 0.000(2) Re2 0.01539(12) 0.01871(14) 0.01311(12) 0.00147(9) 0.00368(9) -0.00090(9) C70 0.018(3) 0.030(4) 0.016(3) -0.002(3) 0.004(3) 0.002(3) O70 0.026(3) 0.048(3) 0.027(3) 0.008(2) 0.013(2) -0.002(2) C71 0.019(3) 0.026(4) 0.017(3) 0.001(3) 0.006(2) -0.002(3) O71 0.032(3) 0.027(3) 0.029(2) 0.007(2) 0.010(2) 0.005(2) C72 0.021(3) 0.018(3) 0.025(3) 0.005(3) 0.012(3) -0.001(2) O72 0.028(3) 0.033(3) 0.019(2) -0.0019(19) 0.004(2) -0.005(2) C54 0.131(10) 0.061(7) 0.072(7) 0.053(6) 0.077(7) 0.057(7) C55 0.098(8) 0.036(5) 0.061(6) 0.023(4) 0.052(6) 0.036(5) C56 0.037(4) 0.021(3) 0.019(3) -0.001(3) 0.015(3) -0.003(3) C57 0.022(3) 0.027(4) 0.009(3) 0.006(2) 0.000(2) 0.001(3) C58 0.027(3) 0.019(3) 0.008(3) 0.002(2) 0.004(2) 0.005(2) C59 0.019(3) 0.032(4) 0.022(3) 0.005(3) 0.009(3) 0.001(3) C60 0.020(3) 0.021(3) 0.021(3) 0.003(3) 0.006(3) -0.002(3) C61 0.019(3) 0.019(3) 0.014(3) 0.002(2) 0.005(2) 0.002(2) C62 0.023(3) 0.020(3) 0.018(3) 0.003(2) 0.012(2) 0.000(3) C63 0.017(3) 0.026(3) 0.019(3) -0.005(3) 0.008(2) -0.003(3) C64 0.014(3) 0.025(3) 0.017(3) -0.003(2) 0.005(2) 0.000(2) C65 0.024(3) 0.032(4) 0.017(3) -0.002(3) 0.006(3) 0.001(3) C66 0.047(5) 0.032(4) 0.027(4) -0.002(3) 0.014(3) 0.003(3) C67 0.047(5) 0.043(5) 0.026(4) 0.008(3) 0.009(3) 0.000(4) N51 0.070(5) 0.031(4) 0.041(4) 0.023(3) 0.039(4) 0.022(3) N52 0.020(3) 0.026(3) 0.022(3) 0.006(2) 0.006(2) 0.000(2) N53 0.032(3) 0.018(3) 0.026(3) 0.003(2) 0.015(2) 0.002(2) N54 0.017(2) 0.018(3) 0.013(2) 0.003(2) 0.004(2) 0.004(2) N55 0.020(2) 0.018(3) 0.015(2) 0.001(2) 0.009(2) 0.000(2) N56 0.017(2) 0.019(3) 0.017(2) 0.002(2) 0.008(2) 0.000(2) N57 0.022(3) 0.027(3) 0.013(2) 0.003(2) 0.006(2) -0.001(2) C15A 0.026(3) 0.039(4) 0.034(4) -0.019(3) 0.017(3) -0.004(3) C16A 0.033(6) 0.029(6) 0.020(5) -0.004(5) 0.016(5) 0.005(5) C17A 0.047(5) 0.058(5) 0.029(4) -0.007(4) 0.020(4) 0.008(4) C15B 0.026(3) 0.039(4) 0.034(4) -0.019(3) 0.017(3) -0.004(3) C16B 0.041(11) 0.043(12) 0.039(11) -0.021(9) 0.025(9) -0.002(9) C17B 0.047(5) 0.058(5) 0.029(4) -0.007(4) 0.020(4) 0.008(4) C51A 0.054(5) 0.065(6) 0.038(5) 0.027(4) 0.023(4) 0.013(5) C52A 0.030(6) 0.038(7) 0.032(7) 0.013(5) 0.009(5) 0.002(5) C53A 0.033(6) 0.033(6) 0.026(6) 0.005(5) 0.004(5) 0.002(5) C51B 0.054(5) 0.065(6) 0.038(5) 0.027(4) 0.023(4) 0.013(5) C52B 0.024(10) 0.041(12) 0.017(9) 0.004(9) 0.010(8) 0.000(9) C53B 0.034(11) 0.035(12) 0.017(10) 0.009(9) 0.005(9) -0.003(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C20 1.906(7) . ? Re1 C21 1.924(7) . ? Re1 C22 1.933(7) . ? Re1 N2 2.166(5) . ? Re1 N6 2.173(5) . ? Re1 N4 2.239(5) . ? C20 O20 1.141(8) . ? C21 O21 1.163(8) . ? C22 O22 1.157(8) . ? C1 C2 1.532(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.512(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.497(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.355(9) . ? C4 N1 1.361(8) . ? C5 N3 1.335(8) . ? C5 H5 0.9500 . ? C6 N3 1.458(7) . ? C6 C7 1.504(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N4 1.353(8) . ? C7 C8 1.384(8) . ? C8 C9 1.389(10) . ? C8 H8 0.9500 . ? C9 C10 1.394(10) . ? C9 H9 0.9500 . ? C10 C11 1.375(8) . ? C10 H10 0.9500 . ? C11 N4 1.350(8) . ? C11 C12 1.508(9) . ? C12 N5 1.459(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N5 1.336(8) . ? C13 C14 1.366(9) . ? C13 H13 0.9500 . ? C14 N7 1.350(8) . ? C14 C15A 1.497(9) . ? N1 N2 1.295(7) . ? N2 N3 1.342(7) . ? N5 N6 1.342(7) . ? N6 N7 1.305(7) . ? Re2 C70 1.918(7) . ? Re2 C72 1.921(7) . ? Re2 C71 1.923(7) . ? Re2 N56 2.160(5) . ? Re2 N52 2.161(5) . ? Re2 N54 2.228(5) . ? C70 O70 1.128(8) . ? C71 O71 1.155(8) . ? C72 O72 1.154(8) . ? C54 N51 1.342(11) . ? C54 C55 1.376(12) . ? C54 C53B 1.59(2) . ? C54 C53A 1.593(14) . ? C55 N53 1.337(10) . ? C55 H55 0.9500 . ? C56 N53 1.465(8) . ? C56 C57 1.507(9) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 N54 1.351(8) . ? C57 C58 1.378(9) . ? C58 C59 1.370(9) . ? C58 H58 0.9500 . ? C59 C60 1.376(9) . ? C59 H59 0.9500 . ? C60 C61 1.380(9) . ? C60 H60 0.9500 . ? C61 N54 1.354(8) . ? C61 C62 1.511(8) . ? C62 N55 1.468(7) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 N55 1.350(8) . ? C63 C64 1.371(9) . ? C63 H63 0.9500 . ? C64 N57 1.357(8) . ? C64 C65 1.499(8) . ? C65 C66 1.538(10) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.543(10) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? N51 N52 1.303(8) . ? N52 N53 1.338(8) . ? N55 N56 1.341(7) . ? N56 N57 1.322(7) . ? C15A C16A 1.527(13) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A C17A 1.505(14) . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? C51A C52A 1.562(13) . ? C51A H51A 0.9800 . ? C51A H51B 0.9800 . ? C51A H51C 0.9800 . ? C52A C53A 1.455(16) . ? C52A H52A 0.9900 . ? C52A H52B 0.9900 . ? C53A H53A 0.9900 . ? C53A H53B 0.9900 . ? C52B C53B 1.57(3) . ? C52B H52C 0.9900 . ? C52B H52D 0.9900 . ? C53B H53C 0.9900 . ? C53B H53D 0.9900 . ? 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 C20 Re1 C21 91.0(3) . . ? C20 Re1 C22 86.5(3) . . ? C21 Re1 C22 82.8(3) . . ? C20 Re1 N2 91.4(2) . . ? C21 Re1 N2 176.4(2) . . ? C22 Re1 N2 94.6(2) . . ? C20 Re1 N6 93.5(2) . . ? C21 Re1 N6 95.0(2) . . ? C22 Re1 N6 177.8(2) . . ? N2 Re1 N6 87.60(19) . . ? C20 Re1 N4 169.5(2) . . ? C21 Re1 N4 97.4(2) . . ? C22 Re1 N4 100.8(2) . . ? N2 Re1 N4 80.55(18) . . ? N6 Re1 N4 79.54(18) . . ? O20 C20 Re1 176.8(6) . . ? O21 C21 Re1 175.4(5) . . ? O22 C22 Re1 173.0(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 113.4(7) . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C2 112.1(6) . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 N1 108.5(5) . . ? C5 C4 C3 129.6(6) . . ? N1 C4 C3 121.9(6) . . ? N3 C5 C4 105.4(6) . . ? N3 C5 H5 127.3 . . ? C4 C5 H5 127.3 . . ? N3 C6 C7 109.5(5) . . ? N3 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? N3 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? N4 C7 C8 122.6(6) . . ? N4 C7 C6 118.5(5) . . ? C8 C7 C6 118.9(6) . . ? C7 C8 C9 118.7(6) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C8 C9 C10 118.6(6) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 119.5(6) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? N4 C11 C10 122.1(6) . . ? N4 C11 C12 118.1(5) . . ? C10 C11 C12 119.7(6) . . ? N5 C12 C11 110.4(5) . . ? N5 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? N5 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N5 C13 C14 104.3(5) . . ? N5 C13 H13 127.8 . . ? C14 C13 H13 127.8 . . ? N7 C14 C13 108.9(5) . . ? N7 C14 C15A 122.8(6) . . ? C13 C14 C15A 128.2(6) . . ? N2 N1 C4 107.9(5) . . ? N1 N2 N3 108.5(5) . . ? N1 N2 Re1 129.5(4) . . ? N3 N2 Re1 122.0(4) . . ? C5 N3 N2 109.8(5) . . ? C5 N3 C6 129.7(5) . . ? N2 N3 C6 120.3(5) . . ? C11 N4 C7 118.1(5) . . ? C11 N4 Re1 120.8(4) . . ? C7 N4 Re1 121.0(4) . . ? C13 N5 N6 110.9(5) . . ? C13 N5 C12 128.5(5) . . ? N6 N5 C12 120.5(5) . . ? N7 N6 N5 107.5(5) . . ? N7 N6 Re1 131.2(4) . . ? N5 N6 Re1 121.3(4) . . ? N6 N7 C14 108.4(5) . . ? C70 Re2 C72 91.7(3) . . ? C70 Re2 C71 87.8(3) . . ? C72 Re2 C71 85.0(3) . . ? C70 Re2 N56 92.3(2) . . ? C72 Re2 N56 174.5(2) . . ? C71 Re2 N56 91.3(2) . . ? C70 Re2 N52 90.6(2) . . ? C72 Re2 N52 96.5(2) . . ? C71 Re2 N52 177.8(2) . . ? N56 Re2 N52 87.2(2) . . ? C70 Re2 N54 168.3(2) . . ? C72 Re2 N54 95.6(2) . . ? C71 Re2 N54 101.9(2) . . ? N56 Re2 N54 81.10(18) . . ? N52 Re2 N54 79.55(19) . . ? O70 C70 Re2 178.2(6) . . ? O71 C71 Re2 175.9(6) . . ? O72 C72 Re2 176.1(5) . . ? N51 C54 C55 108.3(7) . . ? N51 C54 C53B 117.3(11) . . ? C55 C54 C53B 123.4(12) . . ? N51 C54 C53A 119.5(9) . . ? C55 C54 C53A 130.2(9) . . ? C53B C54 C53A 42.8(8) . . ? N53 C55 C54 105.3(7) . . ? N53 C55 H55 127.3 . . ? C54 C55 H55 127.3 . . ? N53 C56 C57 109.0(5) . . ? N53 C56 H56A 109.9 . . ? C57 C56 H56A 109.9 . . ? N53 C56 H56B 109.9 . . ? C57 C56 H56B 109.9 . . ? H56A C56 H56B 108.3 . . ? N54 C57 C58 122.1(6) . . ? N54 C57 C56 118.3(6) . . ? C58 C57 C56 119.4(6) . . ? C59 C58 C57 119.5(6) . . ? C59 C58 H58 120.2 . . ? C57 C58 H58 120.2 . . ? C58 C59 C60 119.0(6) . . ? C58 C59 H59 120.5 . . ? C60 C59 H59 120.5 . . ? C59 C60 C61 119.2(6) . . ? C59 C60 H60 120.4 . . ? C61 C60 H60 120.4 . . ? N54 C61 C60 122.1(6) . . ? N54 C61 C62 119.1(5) . . ? C60 C61 C62 118.8(5) . . ? N55 C62 C61 111.0(5) . . ? N55 C62 H62A 109.4 . . ? C61 C62 H62A 109.4 . . ? N55 C62 H62B 109.4 . . ? C61 C62 H62B 109.4 . . ? H62A C62 H62B 108.0 . . ? N55 C63 C64 105.4(5) . . ? N55 C63 H63 127.3 . . ? C64 C63 H63 127.3 . . ? N57 C64 C63 108.3(5) . . ? N57 C64 C65 122.2(5) . . ? C63 C64 C65 129.5(6) . . ? C64 C65 C66 113.3(6) . . ? C64 C65 H65A 108.9 . . ? C66 C65 H65A 108.9 . . ? C64 C65 H65B 108.9 . . ? C66 C65 H65B 108.9 . . ? H65A C65 H65B 107.7 . . ? C65 C66 C67 110.2(6) . . ? C65 C66 H66A 109.6 . . ? C67 C66 H66A 109.6 . . ? C65 C66 H66B 109.6 . . ? C67 C66 H66B 109.6 . . ? H66A C66 H66B 108.1 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N52 N51 C54 108.1(6) . . ? N51 N52 N53 109.1(5) . . ? N51 N52 Re2 127.8(5) . . ? N53 N52 Re2 122.7(4) . . ? C55 N53 N52 109.2(6) . . ? C55 N53 C56 130.4(6) . . ? N52 N53 C56 120.3(5) . . ? C57 N54 C61 117.7(5) . . ? C57 N54 Re2 121.8(4) . . ? C61 N54 Re2 120.4(4) . . ? N56 N55 C63 109.9(5) . . ? N56 N55 C62 120.2(5) . . ? C63 N55 C62 129.9(5) . . ? N57 N56 N55 108.1(5) . . ? N57 N56 Re2 129.9(4) . . ? N55 N56 Re2 122.0(4) . . ? N56 N57 C64 108.3(5) . . ? C14 C15A C16A 112.4(6) . . ? C14 C15A H15A 109.1 . . ? C16A C15A H15A 109.1 . . ? C14 C15A H15B 109.1 . . ? C16A C15A H15B 109.1 . . ? H15A C15A H15B 107.9 . . ? C17A C16A C15A 114.6(9) . . ? C17A C16A H16A 108.6 . . ? C15A C16A H16A 108.6 . . ? C17A C16A H16B 108.6 . . ? C15A C16A H16B 108.6 . . ? H16A C16A H16B 107.6 . . ? C16A C17A H17A 109.5 . . ? C16A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C16A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? H16C C16B H16D 107.5 . . ? C52A C51A H51A 109.5 . . ? C52A C51A H51B 109.5 . . ? H51A C51A H51B 109.5 . . ? C52A C51A H51C 109.5 . . ? H51A C51A H51C 109.5 . . ? H51B C51A H51C 109.5 . . ? C53A C52A C51A 106.9(9) . . ? C53A C52A H52A 110.3 . . ? C51A C52A H52A 110.3 . . ? C53A C52A H52B 110.3 . . ? C51A C52A H52B 110.3 . . ? H52A C52A H52B 108.6 . . ? C52A C53A C54 107.1(10) . . ? C52A C53A H53A 110.3 . . ? C54 C53A H53A 110.3 . . ? C52A C53A H53B 110.3 . . ? C54 C53A H53B 110.3 . . ? H53A C53A H53B 108.5 . . ? C53B C52B H52C 111.2 . . ? C53B C52B H52D 111.2 . . ? H52C C52B H52D 109.2 . . ? C52B C53B C54 98.0(15) . . ? C52B C53B H53C 112.2 . . ? C54 C53B H53C 112.2 . . ? C52B C53B H53D 112.2 . . ? C54 C53B H53D 112.2 . . ? H53C C53B H53D 109.8 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.65 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 4.197 _refine_diff_density_min -1.847 _refine_diff_density_rms 0.175 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.142 0.242 0.782 195.3 54.1 2 0.642 0.258 0.282 195.3 54.5 3 -0.142 0.758 0.218 195.4 55.2 4 0.358 0.742 0.718 195.4 56.1 _platon_squeeze_details ; Disordered hexafluorophosphate (PF6-) anions and disordered solvent molecules. ;