# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Shih-Sheng Sun' _publ_contact_author_email SSSUN@CHEM.SINICA.EDU.TW _publ_section_title ; Colorimetric and luminescent sensing of F- anion through strong anion-? interaction inside the ?-acidic cavity of a pyridyl-triazine bridged trinuclear Re(I)-tricarbonyl diimine complex ; loop_ _publ_author_name 'Shih-Sheng Sun' 'Chi-We Chen' 'Chen-Yen Hung' 'Ashutosh S Singh' ; Yuh-Sheng Wen ; # Attachment 'i9674.cif' data_i9674 _database_code_depnum_ccdc_archive 'CCDC 698789' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H60 F18 N12 O11 P3 Re3' _chemical_formula_sum 'C69 H60 F18 N12 O11 P3 Re3' _chemical_formula_weight 2226.80 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 P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 22.8100(5) _cell_length_b 25.0562(5) _cell_length_c 14.1649(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.4580(10) _cell_angle_gamma 90.00 _cell_volume 7985.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 9816 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.86 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.852 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4312 _exptl_absorpt_coefficient_mu 4.702 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS, 1996' _exptl_absorpt_correction_T_min 0.2204 _exptl_absorpt_correction_T_max 0.2679 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52621 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13979 _reflns_number_gt 11081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0641P)^2^+60.5789P] 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 13979 _refine_ls_number_parameters 982 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.894057(15) 0.980599(14) 0.23756(2) 0.03313(10) Uani 1 1 d . . . Re2 Re 0.489924(13) 1.170187(13) 0.52327(2) 0.03042(10) Uani 1 1 d . . . Re3 Re 0.723495(14) 0.791288(12) 0.87115(2) 0.02767(10) Uani 1 1 d . . . O30 O 0.8836(3) 1.0314(3) 0.0384(5) 0.0535(17) Uani 1 1 d . . . O31 O 1.0195(3) 0.9453(3) 0.2121(5) 0.0603(19) Uani 1 1 d . . . O32 O 0.8354(3) 0.8784(3) 0.1447(5) 0.0524(17) Uani 1 1 d . . . O33 O 0.4314(3) 1.1442(3) 0.3183(4) 0.0436(15) Uani 1 1 d . . . O34 O 0.4494(3) 1.2857(3) 0.4765(6) 0.064(2) Uani 1 1 d . . . O35 O 0.3660(2) 1.1589(2) 0.5787(4) 0.0388(14) Uani 1 1 d . . . O36 O 0.6034(3) 0.7490(3) 0.7703(5) 0.065(2) Uani 1 1 d . . . O37 O 0.7734(3) 0.6791(2) 0.8455(5) 0.0515(17) Uani 1 1 d . . . O38 O 0.6886(3) 0.7598(3) 1.0641(4) 0.0472(16) Uani 1 1 d . . . N1 N 0.7268(3) 0.9419(3) 0.4722(4) 0.0257(14) Uani 1 1 d . . . N3 N 0.6506(3) 1.0075(3) 0.4543(4) 0.0272(14) Uani 1 1 d . . . N5 N 0.6560(3) 0.9422(3) 0.5787(4) 0.0271(14) Uani 1 1 d . . . N9 N 0.8041(3) 1.0075(3) 0.2593(5) 0.0361(16) Uani 1 1 d . . . N15 N 0.5165(3) 1.0863(3) 0.5641(4) 0.0263(14) Uani 1 1 d . . . N21 N 0.7474(3) 0.8179(2) 0.7339(4) 0.0266(14) Uani 1 1 d . . . N40 N 0.9090(3) 0.9550(3) 0.3864(5) 0.0319(15) Uani 1 1 d . . . N47 N 0.9177(3) 1.0527(3) 0.3202(5) 0.0363(16) Uani 1 1 d . . . N54 N 0.5439(3) 1.1834(3) 0.6628(5) 0.0347(16) Uani 1 1 d . . . N61 N 0.5806(3) 1.1780(3) 0.4971(5) 0.0341(16) Uani 1 1 d . . . N68 N 0.8074(3) 0.8317(3) 0.9229(5) 0.0311(15) Uani 1 1 d . . . N75 N 0.7005(3) 0.8744(3) 0.8883(4) 0.0290(15) Uani 1 1 d . . . C2 C 0.6984(3) 0.9837(3) 0.4290(5) 0.0273(17) Uani 1 1 d . . . C4 C 0.6320(3) 0.9856(3) 0.5308(5) 0.0226(15) Uani 1 1 d . . . C6 C 0.7041(3) 0.9232(3) 0.5459(5) 0.0268(16) Uani 1 1 d . . . C7 C 0.7229(3) 1.0061(3) 0.3471(5) 0.0312(18) Uani 1 1 d . . . C8 C 0.7774(3) 0.9873(3) 0.3292(5) 0.0294(17) Uani 1 1 d . . . H8 H 0.7961 0.9599 0.3671 0.035 Uiso 1 1 calc R . . C10 C 0.7767(5) 1.0473(4) 0.2060(7) 0.057(3) Uani 1 1 d . . . H10 H 0.7951 1.0621 0.1582 0.069 Uiso 1 1 calc R . . C11 C 0.7225(5) 1.0671(5) 0.2192(8) 0.062(3) Uani 1 1 d . . . H11 H 0.7044 1.0940 0.1793 0.074 Uiso 1 1 calc R . . C12 C 0.6949(4) 1.0473(4) 0.2914(7) 0.049(3) Uani 1 1 d . . . H12 H 0.6588 1.0611 0.3024 0.059 Uiso 1 1 calc R . . C13 C 0.5817(3) 1.0111(3) 0.5670(5) 0.0261(16) Uani 1 1 d . . . C14 C 0.5597(3) 1.0594(3) 0.5303(5) 0.0262(16) Uani 1 1 d . . . H14 H 0.5755 1.0740 0.4796 0.031 Uiso 1 1 calc R . . C16 C 0.4926(3) 1.0628(3) 0.6334(6) 0.0309(18) Uani 1 1 d . . . H16 H 0.4618 1.0805 0.6560 0.037 Uiso 1 1 calc R . . C17 C 0.5104(4) 1.0141(3) 0.6737(6) 0.0354(19) Uani 1 1 d . . . H17 H 0.4916 0.9990 0.7207 0.042 Uiso 1 1 calc R . . C18 C 0.5575(4) 0.9886(3) 0.6414(6) 0.0329(18) Uani 1 1 d . . . H18 H 0.5725 0.9568 0.6693 0.039 Uiso 1 1 calc R . . C19 C 0.7356(3) 0.8770(3) 0.5986(5) 0.0249(16) Uani 1 1 d . . . C20 C 0.7180(3) 0.8574(3) 0.6820(5) 0.0233(15) Uani 1 1 d . . . H20 H 0.6848 0.8723 0.7024 0.028 Uiso 1 1 calc R . . C22 C 0.7941(3) 0.7956(3) 0.7004(5) 0.0287(17) Uani 1 1 d . . . H22 H 0.8143 0.7677 0.7349 0.034 Uiso 1 1 calc R . . C23 C 0.8128(3) 0.8120(3) 0.6186(6) 0.0291(17) Uani 1 1 d . . . H23 H 0.8450 0.7955 0.5981 0.035 Uiso 1 1 calc R . . C24 C 0.7835(3) 0.8532(3) 0.5668(5) 0.0275(17) Uani 1 1 d . . . H24 H 0.7957 0.8650 0.5109 0.033 Uiso 1 1 calc R . . C30 C 0.8868(4) 1.0119(4) 0.1134(6) 0.038(2) Uani 1 1 d . . . C31 C 0.9727(4) 0.9576(4) 0.2228(6) 0.043(2) Uani 1 1 d . . . C32 C 0.8597(4) 0.9153(4) 0.1786(6) 0.042(2) Uani 1 1 d . . . C33 C 0.4532(3) 1.1538(3) 0.3959(7) 0.0332(18) Uani 1 1 d . . . C34 C 0.4671(4) 1.2433(3) 0.4956(8) 0.044(2) Uani 1 1 d . . . C35 C 0.4126(4) 1.1624(3) 0.5595(6) 0.0320(18) Uani 1 1 d . . . C36 C 0.6475(4) 0.7646(4) 0.8093(7) 0.042(2) Uani 1 1 d . . . C37 C 0.7544(4) 0.7206(4) 0.8565(6) 0.0362(19) Uani 1 1 d . . . C38 C 0.7028(4) 0.7714(3) 0.9928(6) 0.0350(19) Uani 1 1 d . . . C41 C 0.9156(3) 0.9939(3) 0.4539(6) 0.0300(18) Uani 1 1 d . . . C42 C 0.9210(3) 0.9818(4) 0.5499(6) 0.0363(19) Uani 1 1 d . . . H42 H 0.9241 1.0094 0.5943 0.044 Uiso 1 1 calc R . . C43 C 0.9218(4) 0.9302(4) 0.5811(6) 0.040(2) Uani 1 1 d . . . C44 C 0.9193(4) 0.8904(4) 0.5119(6) 0.040(2) Uani 1 1 d . . . H44 H 0.9224 0.8547 0.5302 0.048 Uiso 1 1 calc R . . C45 C 0.9121(3) 0.9039(4) 0.4164(6) 0.0364(19) Uani 1 1 d . . . H45 H 0.9093 0.8768 0.3710 0.044 Uiso 1 1 calc R . . C46 C 0.9244(5) 0.9165(4) 0.6860(6) 0.050(2) Uani 1 1 d . . . H46A H 0.9243 0.8785 0.6936 0.075 Uiso 1 1 calc R . . H46B H 0.8904 0.9314 0.7085 0.075 Uiso 1 1 calc R . . H46C H 0.9600 0.9311 0.7224 0.075 Uiso 1 1 calc R . . C48 C 0.9175(3) 1.0492(3) 0.4159(6) 0.0340(19) Uani 1 1 d . . . C49 C 0.9206(4) 1.0939(4) 0.4733(6) 0.038(2) Uani 1 1 d . . . H49 H 0.9196 1.0902 0.5384 0.045 Uiso 1 1 calc R . . C50 C 0.9253(4) 1.1445(4) 0.4345(7) 0.041(2) Uani 1 1 d . . . C51 C 0.9257(4) 1.1478(4) 0.3366(7) 0.046(2) Uani 1 1 d . . . H51 H 0.9287 1.1807 0.3074 0.055 Uiso 1 1 calc R . . C52 C 0.9214(4) 1.1014(4) 0.2834(7) 0.047(2) Uani 1 1 d . . . H52 H 0.9211 1.1042 0.2178 0.056 Uiso 1 1 calc R . . C53 C 0.9292(5) 1.1942(4) 0.4942(8) 0.055(3) Uani 1 1 d . . . H53A H 0.9316 1.1847 0.5604 0.082 Uiso 1 1 calc R . . H53B H 0.8945 1.2157 0.4746 0.082 Uiso 1 1 calc R . . H53C H 0.9640 1.2140 0.4858 0.082 Uiso 1 1 calc R . . C55 C 0.6036(4) 1.1808(3) 0.6671(7) 0.037(2) Uani 1 1 d . . . C56 C 0.6419(4) 1.1804(3) 0.7552(7) 0.042(2) Uani 1 1 d . . . H56 H 0.6826 1.1775 0.7562 0.050 Uiso 1 1 calc R . . C57 C 0.6205(4) 1.1844(3) 0.8401(7) 0.042(2) Uani 1 1 d . . . C58 C 0.5595(4) 1.1871(4) 0.8349(7) 0.046(2) Uani 1 1 d . . . H58 H 0.5430 1.1895 0.8906 0.056 Uiso 1 1 calc R . . C59 C 0.5228(4) 1.1864(4) 0.7463(7) 0.044(2) Uani 1 1 d . . . H59 H 0.4819 1.1881 0.7444 0.053 Uiso 1 1 calc R . . C60 C 0.6610(5) 1.1834(4) 0.9355(8) 0.056(3) Uani 1 1 d . . . H60A H 0.6505 1.2119 0.9748 0.083 Uiso 1 1 calc R . . H60B H 0.7014 1.1879 0.9259 0.083 Uiso 1 1 calc R . . H60C H 0.6570 1.1499 0.9665 0.083 Uiso 1 1 calc R . . C62 C 0.6238(4) 1.1774(3) 0.5741(7) 0.037(2) Uani 1 1 d . . . C63 C 0.6833(4) 1.1731(4) 0.5635(8) 0.048(2) Uani 1 1 d . . . H63 H 0.7124 1.1714 0.6178 0.057 Uiso 1 1 calc R . . C64 C 0.7001(4) 1.1713(4) 0.4738(8) 0.050(2) Uani 1 1 d . . . C65 C 0.6544(4) 1.1744(4) 0.3967(8) 0.049(2) Uani 1 1 d . . . H65 H 0.6636 1.1746 0.3350 0.058 Uiso 1 1 calc R . . C66 C 0.5961(4) 1.1772(3) 0.4085(7) 0.041(2) Uani 1 1 d . . . H66 H 0.5665 1.1786 0.3549 0.049 Uiso 1 1 calc R . . C67 C 0.7637(4) 1.1658(6) 0.4618(9) 0.075(4) Uani 1 1 d . . . H67A H 0.7798 1.1335 0.4920 0.113 Uiso 1 1 calc R . . H67B H 0.7859 1.1958 0.4908 0.113 Uiso 1 1 calc R . . H67C H 0.7663 1.1647 0.3949 0.113 Uiso 1 1 calc R . . C69 C 0.8059(4) 0.8855(4) 0.9170(6) 0.0357(19) Uani 1 1 d . . . C70 C 0.8579(4) 0.9152(4) 0.9244(6) 0.039(2) Uani 1 1 d . . . H70 H 0.8560 0.9520 0.9169 0.046 Uiso 1 1 calc R . . C71 C 0.9130(4) 0.8894(5) 0.9432(6) 0.046(2) Uani 1 1 d . . . C72 C 0.9137(4) 0.8357(4) 0.9542(7) 0.049(2) Uani 1 1 d . . . H72 H 0.9497 0.8177 0.9697 0.058 Uiso 1 1 calc R . . C73 C 0.8604(4) 0.8075(4) 0.9423(6) 0.040(2) Uani 1 1 d . . . H73 H 0.8616 0.7705 0.9480 0.049 Uiso 1 1 calc R . . C74 C 0.9696(5) 0.9226(5) 0.9514(8) 0.068(3) Uani 1 1 d . . . H74A H 0.9601 0.9575 0.9254 0.101 Uiso 1 1 calc R . . H74B H 0.9970 0.9055 0.9166 0.101 Uiso 1 1 calc R . . H74C H 0.9872 0.9257 1.0176 0.101 Uiso 1 1 calc R . . C76 C 0.7458(4) 0.9096(3) 0.9039(5) 0.0305(18) Uani 1 1 d . . . C77 C 0.7358(5) 0.9636(4) 0.9105(7) 0.048(2) Uani 1 1 d . . . H77 H 0.7678 0.9870 0.9224 0.058 Uiso 1 1 calc R . . C78 C 0.6785(5) 0.9830(4) 0.8994(7) 0.055(3) Uani 1 1 d . . . C79 C 0.6332(5) 0.9463(4) 0.8856(7) 0.053(3) Uani 1 1 d . . . H79 H 0.5940 0.9578 0.8801 0.064 Uiso 1 1 calc R . . C80 C 0.6448(4) 0.8933(4) 0.8799(6) 0.037(2) Uani 1 1 d . . . H80 H 0.6132 0.8694 0.8698 0.044 Uiso 1 1 calc R . . C81 C 0.6670(7) 1.0435(4) 0.9056(10) 0.087(4) Uani 1 1 d . . . H81A H 0.7041 1.0617 0.9254 0.131 Uiso 1 1 calc R . . H81B H 0.6410 1.0500 0.9512 0.131 Uiso 1 1 calc R . . H81C H 0.6489 1.0565 0.8439 0.131 Uiso 1 1 calc R . . P1 P 0.55353(13) 0.3798(3) 0.6407(2) 0.113(2) Uani 1 1 d . . . F1 F 0.5199(5) 0.3321(6) 0.6764(9) 0.195(8) Uani 1 1 d . . . F2 F 0.5498(4) 0.3616(9) 0.5365(7) 0.279(12) Uani 1 1 d . . . F3 F 0.6137(4) 0.3518(4) 0.6721(6) 0.109(3) Uani 1 1 d . . . F4 F 0.5903(5) 0.4309(6) 0.6108(7) 0.167(6) Uani 1 1 d . . . F5 F 0.5597(3) 0.4062(3) 0.7442(5) 0.0778(19) Uani 1 1 d . . . F6 F 0.4951(5) 0.4134(11) 0.6135(8) 0.286(13) Uani 1 1 d . . . P2 P 0.78889(10) 0.45348(10) 0.19434(17) 0.0414(5) Uani 1 1 d . . . F7 F 0.7633(6) 0.4461(4) 0.0855(6) 0.146(5) Uani 1 1 d . . . F8 F 0.7264(4) 0.4722(6) 0.2076(8) 0.174(6) Uani 1 1 d . . . F9 F 0.8146(5) 0.4600(4) 0.2998(6) 0.141(4) Uani 1 1 d . . . F10 F 0.7750(4) 0.3944(3) 0.2167(7) 0.128(4) Uani 1 1 d . . . F11 F 0.8508(4) 0.4329(4) 0.1744(7) 0.121(4) Uani 1 1 d . . . F12 F 0.8020(5) 0.5119(3) 0.1685(10) 0.161(5) Uani 1 1 d . . . P3 P 0.96425(7) 0.73230(7) 0.74848(13) 0.0179(4) Uani 1 1 d . . . F13 F 0.9841(6) 0.7441(4) 0.6526(7) 0.157(5) Uani 1 1 d . . . F14 F 1.0223(3) 0.7574(4) 0.8099(6) 0.111(3) Uani 1 1 d . . . F15 F 0.9357(5) 0.7232(4) 0.8434(9) 0.144(5) Uani 1 1 d . . . F16 F 0.9014(5) 0.7142(4) 0.6901(9) 0.140(4) Uani 1 1 d . . . F17 F 0.9381(4) 0.7918(3) 0.7463(7) 0.110(3) Uani 1 1 d . . . F18 F 0.9884(4) 0.6740(3) 0.7578(8) 0.125(4) Uani 1 1 d . . . O91 O 0.6195 0.9270 0.2644 0.078 Uani 1 1 d . . . C90 C 0.6210 0.9185 0.1815 0.053 Uani 1 1 d . . . C92 C 0.5690 0.9255 0.1092 0.111 Uani 1 1 d . . . H92A H 0.5344 0.9283 0.1393 0.167 Uiso 1 1 calc R . . H92B H 0.5649 0.8954 0.0667 0.167 Uiso 1 1 calc R . . H92C H 0.5732 0.9574 0.0734 0.167 Uiso 1 1 calc R . . C93 C 0.6773 0.9004 0.1498 0.099 Uani 1 1 d . . . H93A H 0.7066 0.8928 0.2049 0.149 Uiso 1 1 calc R . . H93B H 0.6917 0.9281 0.1126 0.149 Uiso 1 1 calc R . . H93C H 0.6696 0.8688 0.1115 0.149 Uiso 1 1 calc R . . O95 O 0.8082 0.2954 0.4018 0.173 Uiso 1 1 d . . . C94 C 0.8403 0.3127 0.3574 0.135 Uiso 1 1 d . . . C96 C 0.8898 0.3468 0.3823 0.117 Uiso 1 1 d . . . H96A H 0.8912 0.3593 0.4466 0.175 Uiso 1 1 calc R . . H96B H 0.8864 0.3767 0.3393 0.175 Uiso 1 1 calc R . . H96C H 0.9257 0.3275 0.3778 0.175 Uiso 1 1 calc R . . C97 C 0.8510 0.2887 0.2434 0.149 Uiso 1 1 d . . . H97A H 0.8206 0.2631 0.2206 0.224 Uiso 1 1 calc R . . H97B H 0.8893 0.2720 0.2488 0.224 Uiso 1 1 calc R . . H97C H 0.8488 0.3180 0.1992 0.224 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 0.03458(19) 0.0373(2) 0.03077(18) -0.00269(14) 0.01512(14) -0.00088(14) Re2 0.02245(17) 0.02575(18) 0.0435(2) 0.00065(14) 0.00664(14) 0.00269(12) Re3 0.02676(17) 0.02706(18) 0.02886(17) 0.00434(13) 0.00357(13) -0.00127(13) O30 0.069(5) 0.054(4) 0.043(4) 0.005(3) 0.023(3) -0.008(4) O31 0.036(4) 0.075(5) 0.075(5) -0.014(4) 0.027(4) 0.002(4) O32 0.060(4) 0.048(4) 0.049(4) -0.009(3) 0.011(3) -0.012(3) O33 0.040(4) 0.047(4) 0.042(4) 0.010(3) 0.005(3) -0.002(3) O34 0.039(4) 0.028(4) 0.123(7) 0.011(4) 0.007(4) 0.003(3) O35 0.025(3) 0.039(3) 0.054(4) -0.009(3) 0.010(3) 0.000(3) O36 0.047(4) 0.058(5) 0.080(5) 0.028(4) -0.022(4) -0.030(4) O37 0.085(5) 0.027(4) 0.046(4) 0.007(3) 0.019(4) 0.015(3) O38 0.048(4) 0.056(4) 0.043(4) 0.013(3) 0.020(3) 0.014(3) N1 0.025(3) 0.030(4) 0.023(3) -0.001(3) 0.007(3) 0.001(3) N3 0.023(3) 0.031(4) 0.027(3) 0.003(3) 0.003(3) 0.003(3) N5 0.024(3) 0.030(4) 0.028(3) -0.002(3) 0.007(3) -0.003(3) N9 0.034(4) 0.048(4) 0.030(4) 0.005(3) 0.017(3) 0.004(3) N15 0.018(3) 0.029(4) 0.032(3) -0.002(3) 0.005(3) 0.001(3) N21 0.028(3) 0.027(4) 0.025(3) 0.004(3) 0.004(3) -0.001(3) N40 0.024(3) 0.040(4) 0.034(4) 0.000(3) 0.011(3) 0.000(3) N47 0.040(4) 0.036(4) 0.036(4) -0.001(3) 0.015(3) -0.002(3) N54 0.024(3) 0.026(4) 0.054(4) -0.006(3) 0.004(3) 0.001(3) N61 0.028(4) 0.029(4) 0.046(4) 0.000(3) 0.010(3) -0.002(3) N68 0.027(4) 0.037(4) 0.029(3) -0.005(3) 0.005(3) -0.001(3) N75 0.039(4) 0.027(4) 0.023(3) 0.003(3) 0.009(3) -0.001(3) C2 0.026(4) 0.030(4) 0.026(4) 0.002(3) 0.003(3) 0.002(3) C4 0.019(4) 0.022(4) 0.026(4) 0.001(3) 0.001(3) -0.003(3) C6 0.028(4) 0.025(4) 0.026(4) 0.000(3) 0.003(3) -0.002(3) C7 0.031(4) 0.037(5) 0.028(4) 0.002(3) 0.010(3) 0.001(4) C8 0.029(4) 0.031(4) 0.029(4) 0.004(3) 0.006(3) 0.002(3) C10 0.059(6) 0.070(7) 0.048(6) 0.032(5) 0.026(5) 0.020(6) C11 0.060(7) 0.073(8) 0.058(6) 0.038(6) 0.026(5) 0.030(6) C12 0.042(5) 0.063(7) 0.047(5) 0.025(5) 0.017(4) 0.025(5) C13 0.026(4) 0.024(4) 0.028(4) 0.000(3) 0.003(3) -0.005(3) C14 0.027(4) 0.027(4) 0.024(4) -0.004(3) 0.004(3) 0.001(3) C16 0.023(4) 0.037(5) 0.034(4) -0.006(4) 0.011(3) 0.001(3) C17 0.030(4) 0.039(5) 0.041(5) 0.003(4) 0.017(4) 0.000(4) C18 0.033(4) 0.029(4) 0.036(4) 0.003(4) 0.007(4) 0.001(3) C19 0.024(4) 0.029(4) 0.022(4) -0.001(3) 0.004(3) -0.003(3) C20 0.020(4) 0.023(4) 0.026(4) 0.000(3) 0.000(3) 0.002(3) C22 0.028(4) 0.024(4) 0.032(4) 0.005(3) 0.002(3) 0.006(3) C23 0.026(4) 0.029(4) 0.033(4) 0.000(3) 0.007(3) 0.008(3) C24 0.027(4) 0.027(4) 0.030(4) -0.003(3) 0.009(3) 0.000(3) C30 0.043(5) 0.040(5) 0.037(5) 0.000(4) 0.019(4) -0.001(4) C31 0.047(6) 0.044(5) 0.042(5) -0.008(4) 0.019(4) -0.003(4) C32 0.049(5) 0.046(6) 0.036(5) -0.004(4) 0.020(4) 0.001(5) C33 0.025(4) 0.029(4) 0.046(5) 0.009(4) 0.008(4) 0.001(3) C34 0.034(5) 0.023(5) 0.079(7) 0.008(4) 0.018(5) 0.001(4) C35 0.034(5) 0.020(4) 0.042(5) -0.006(3) 0.005(4) 0.006(3) C36 0.042(5) 0.034(5) 0.049(5) 0.014(4) 0.002(4) -0.010(4) C37 0.041(5) 0.036(5) 0.032(4) 0.005(4) 0.007(4) 0.001(4) C38 0.029(4) 0.034(5) 0.042(5) 0.006(4) 0.007(4) 0.008(4) C41 0.019(4) 0.033(4) 0.038(4) -0.005(4) 0.005(3) 0.001(3) C42 0.027(4) 0.041(5) 0.040(5) -0.002(4) 0.002(4) -0.004(4) C43 0.024(4) 0.055(6) 0.039(5) 0.004(4) 0.001(4) 0.001(4) C44 0.028(4) 0.046(5) 0.046(5) 0.004(4) 0.008(4) 0.000(4) C45 0.027(4) 0.041(5) 0.044(5) -0.003(4) 0.011(4) 0.004(4) C46 0.057(6) 0.051(6) 0.040(5) 0.008(4) 0.003(5) -0.006(5) C48 0.023(4) 0.040(5) 0.041(5) -0.010(4) 0.011(3) -0.005(3) C49 0.028(4) 0.047(6) 0.039(5) -0.008(4) 0.009(4) -0.003(4) C50 0.034(5) 0.035(5) 0.058(6) -0.018(4) 0.014(4) -0.005(4) C51 0.058(6) 0.030(5) 0.054(6) 0.004(4) 0.023(5) -0.005(4) C52 0.059(6) 0.043(6) 0.044(5) 0.005(4) 0.023(5) -0.004(5) C53 0.065(7) 0.034(5) 0.066(7) -0.012(5) 0.014(5) -0.007(5) C55 0.027(4) 0.027(4) 0.055(6) -0.005(4) 0.006(4) -0.001(3) C56 0.027(4) 0.035(5) 0.062(6) -0.005(4) 0.003(4) 0.001(4) C57 0.039(5) 0.029(5) 0.053(6) -0.009(4) -0.004(4) -0.009(4) C58 0.045(6) 0.047(6) 0.047(5) -0.016(4) 0.009(4) -0.001(4) C59 0.039(5) 0.048(6) 0.047(5) -0.015(4) 0.012(4) 0.003(4) C60 0.050(6) 0.048(6) 0.065(7) -0.009(5) -0.002(5) -0.009(5) C62 0.027(4) 0.023(4) 0.061(6) 0.003(4) 0.008(4) -0.001(3) C63 0.027(5) 0.047(6) 0.069(7) 0.004(5) 0.008(4) -0.001(4) C64 0.032(5) 0.057(6) 0.066(7) 0.006(5) 0.019(5) 0.001(4) C65 0.042(5) 0.037(5) 0.072(7) 0.009(5) 0.025(5) -0.003(4) C66 0.036(5) 0.030(5) 0.058(6) 0.004(4) 0.015(4) -0.003(4) C67 0.030(5) 0.118(11) 0.080(8) 0.003(8) 0.018(5) -0.004(6) C69 0.043(5) 0.042(5) 0.023(4) -0.005(4) 0.008(4) -0.007(4) C70 0.046(5) 0.040(5) 0.031(4) -0.005(4) 0.011(4) -0.018(4) C71 0.029(5) 0.080(8) 0.032(5) -0.014(5) 0.010(4) -0.016(5) C72 0.038(5) 0.062(7) 0.046(6) -0.009(5) 0.005(4) 0.003(5) C73 0.035(5) 0.049(6) 0.037(5) 0.005(4) 0.007(4) 0.009(4) C74 0.051(6) 0.103(10) 0.049(6) -0.019(6) 0.011(5) -0.037(6) C76 0.041(5) 0.027(4) 0.026(4) 0.000(3) 0.012(3) -0.004(4) C77 0.059(6) 0.036(5) 0.056(6) 0.002(4) 0.026(5) -0.005(5) C78 0.087(8) 0.035(5) 0.049(6) 0.008(4) 0.030(6) 0.017(5) C79 0.054(6) 0.066(7) 0.045(6) 0.015(5) 0.026(5) 0.030(6) C80 0.032(5) 0.045(5) 0.037(5) 0.004(4) 0.014(4) 0.010(4) C81 0.126(12) 0.037(6) 0.110(11) -0.012(7) 0.053(9) 0.022(7) P1 0.0299(15) 0.269(6) 0.0395(16) -0.028(3) 0.0038(13) -0.011(3) F1 0.113(8) 0.307(18) 0.180(11) -0.176(12) 0.074(8) -0.126(10) F2 0.077(6) 0.68(4) 0.087(7) -0.177(13) 0.032(5) -0.093(12) F3 0.087(6) 0.137(8) 0.105(6) -0.042(6) 0.023(5) -0.023(5) F4 0.116(8) 0.275(15) 0.115(8) 0.109(9) 0.039(6) 0.038(9) F5 0.074(4) 0.095(5) 0.066(4) -0.005(4) 0.014(3) -0.002(4) F6 0.066(6) 0.68(4) 0.107(8) 0.060(15) 0.007(6) 0.112(13) P2 0.0354(12) 0.0415(14) 0.0451(13) 0.0071(11) 0.0002(10) 0.0033(10) F7 0.237(12) 0.117(8) 0.064(5) 0.001(5) -0.038(6) 0.085(8) F8 0.083(6) 0.281(15) 0.165(10) 0.109(10) 0.044(6) 0.103(8) F9 0.177(10) 0.153(9) 0.076(5) -0.041(6) -0.035(6) 0.101(8) F10 0.116(7) 0.086(6) 0.155(8) 0.058(6) -0.059(6) -0.035(5) F11 0.082(5) 0.160(9) 0.131(7) 0.074(7) 0.050(5) 0.052(6) F12 0.142(9) 0.059(5) 0.241(13) 0.043(6) -0.091(9) -0.011(5) P3 0.0104(8) 0.0102(8) 0.0337(10) 0.0097(7) 0.0050(7) 0.0040(6) F13 0.262(14) 0.125(8) 0.101(7) -0.017(6) 0.081(8) -0.073(9) F14 0.078(5) 0.134(8) 0.109(6) 0.052(6) -0.020(5) -0.027(5) F15 0.192(11) 0.081(6) 0.195(11) 0.019(6) 0.139(9) -0.001(6) F16 0.115(8) 0.083(6) 0.210(12) -0.016(7) -0.004(8) -0.006(5) F17 0.105(6) 0.061(5) 0.155(8) 0.002(5) -0.006(6) 0.011(4) F18 0.131(8) 0.047(4) 0.211(11) 0.026(5) 0.075(7) 0.040(5) O91 0.062 0.126 0.050 -0.010 0.024 -0.013 C90 0.055 0.069 0.038 -0.011 0.019 -0.007 C92 0.082 0.185 0.064 -0.037 0.003 0.012 C93 0.100 0.139 0.063 -0.026 0.027 0.026 _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 C30 1.908(9) . ? Re1 C31 1.928(10) . ? Re1 C32 1.944(10) . ? Re1 N47 2.173(7) . ? Re1 N40 2.176(7) . ? Re1 N9 2.228(7) . ? Re2 C33 1.906(9) . ? Re2 C35 1.926(9) . ? Re2 C34 1.927(9) . ? Re2 N61 2.170(7) . ? Re2 N54 2.175(7) . ? Re2 N15 2.236(6) . ? Re3 C38 1.926(9) . ? Re3 C36 1.929(9) . ? Re3 C37 1.931(9) . ? Re3 N75 2.170(6) . ? Re3 N68 2.184(7) . ? Re3 N21 2.207(6) . ? O30 C30 1.160(10) . ? O31 C31 1.146(11) . ? O32 C32 1.141(11) . ? O33 C33 1.154(10) . ? O34 C34 1.152(10) . ? O35 C35 1.142(10) . ? O36 C36 1.134(10) . ? O37 C37 1.147(10) . ? O38 C38 1.147(10) . ? N1 C6 1.325(9) . ? N1 C2 1.327(10) . ? N3 C2 1.343(10) . ? N3 C4 1.345(9) . ? N5 C6 1.345(10) . ? N5 C4 1.350(9) . ? N9 C10 1.344(12) . ? N9 C8 1.344(10) . ? N15 C16 1.336(10) . ? N15 C14 1.346(9) . ? N21 C20 1.346(9) . ? N21 C22 1.355(10) . ? N40 C45 1.347(11) . ? N40 C41 1.356(10) . ? N47 C52 1.335(11) . ? N47 C48 1.359(10) . ? N54 C59 1.351(11) . ? N54 C55 1.354(10) . ? N61 C62 1.345(11) . ? N61 C66 1.357(11) . ? N68 C73 1.340(11) . ? N68 C69 1.350(11) . ? N75 C80 1.344(10) . ? N75 C76 1.348(10) . ? C2 C7 1.478(11) . ? C4 C13 1.476(10) . ? C6 C19 1.496(10) . ? C7 C8 1.390(11) . ? C7 C12 1.391(12) . ? C8 H8 0.9300 . ? C10 C11 1.371(14) . ? C10 H10 0.9300 . ? C11 C12 1.379(13) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.379(11) . ? C13 C18 1.387(11) . ? C14 H14 0.9300 . ? C16 C17 1.379(12) . ? C16 H16 0.9300 . ? C17 C18 1.390(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.382(10) . ? C19 C20 1.399(10) . ? C20 H20 0.9300 . ? C22 C23 1.362(11) . ? C22 H22 0.9300 . ? C23 C24 1.376(11) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C41 C42 1.379(12) . ? C41 C48 1.491(12) . ? C42 C43 1.367(12) . ? C42 H42 0.9300 . ? C43 C44 1.392(13) . ? C43 C46 1.516(12) . ? C44 C45 1.379(12) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C48 C49 1.378(12) . ? C49 C50 1.394(13) . ? C49 H49 0.9300 . ? C50 C51 1.392(13) . ? C50 C53 1.498(12) . ? C51 C52 1.380(13) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C55 C56 1.401(12) . ? C55 C62 1.468(13) . ? C56 C57 1.373(13) . ? C56 H56 0.9300 . ? C57 C58 1.384(13) . ? C57 C60 1.506(13) . ? C58 C59 1.389(13) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C62 C63 1.395(12) . ? C63 C64 1.386(14) . ? C63 H63 0.9300 . ? C64 C65 1.383(14) . ? C64 C67 1.495(13) . ? C65 C66 1.370(12) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C69 C70 1.389(12) . ? C69 C76 1.481(12) . ? C70 C71 1.399(13) . ? C70 H70 0.9300 . ? C71 C72 1.356(14) . ? C71 C74 1.524(13) . ? C72 C73 1.392(13) . ? C72 H72 0.9300 . ? C73 H73 0.9300 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C76 C77 1.377(12) . ? C77 C78 1.381(15) . ? C77 H77 0.9300 . ? C78 C79 1.374(15) . ? C78 C81 1.543(14) . ? C79 C80 1.359(13) . ? C79 H79 0.9300 . ? C80 H80 0.9300 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? P1 F2 1.534(9) . ? P1 F3 1.540(10) . ? P1 F1 1.549(15) . ? P1 F6 1.569(14) . ? P1 F5 1.594(7) . ? P1 F4 1.625(13) . ? P2 F9 1.522(8) . ? P2 F8 1.541(9) . ? P2 F12 1.550(9) . ? P2 F10 1.557(8) . ? P2 F7 1.567(8) . ? P2 F11 1.573(8) . ? P3 F13 1.529(9) . ? P3 F18 1.558(7) . ? P3 F14 1.590(8) . ? P3 F16 1.600(10) . ? P3 F17 1.604(8) . ? P3 F15 1.605(9) . ? O91 C90 1.1995 . ? C90 C92 1.4457 . ? C90 C93 1.4970 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? O95 C94 1.1274 . ? C94 C96 1.4133 . ? C94 C97 1.7776 . ? C96 H96A 0.9600 . ? C96 H96B 0.9600 . ? C96 H96C 0.9600 . ? C97 H97A 0.9600 . ? C97 H97B 0.9600 . ? C97 H97C 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 C30 Re1 C31 87.9(4) . . ? C30 Re1 C32 89.0(4) . . ? C31 Re1 C32 91.0(4) . . ? C30 Re1 N47 97.5(3) . . ? C31 Re1 N47 98.9(3) . . ? C32 Re1 N47 168.3(3) . . ? C30 Re1 N40 172.0(3) . . ? C31 Re1 N40 90.9(3) . . ? C32 Re1 N40 99.0(3) . . ? N47 Re1 N40 74.8(3) . . ? C30 Re1 N9 93.5(3) . . ? C31 Re1 N9 178.3(3) . . ? C32 Re1 N9 89.9(3) . . ? N47 Re1 N9 80.0(3) . . ? N40 Re1 N9 87.5(2) . . ? C33 Re2 C35 87.2(3) . . ? C33 Re2 C34 87.2(4) . . ? C35 Re2 C34 85.5(3) . . ? C33 Re2 N61 98.1(3) . . ? C35 Re2 N61 174.4(3) . . ? C34 Re2 N61 96.5(3) . . ? C33 Re2 N54 171.3(3) . . ? C35 Re2 N54 100.3(3) . . ? C34 Re2 N54 97.7(4) . . ? N61 Re2 N54 74.2(3) . . ? C33 Re2 N15 95.7(3) . . ? C35 Re2 N15 93.3(3) . . ? C34 Re2 N15 176.8(3) . . ? N61 Re2 N15 84.5(2) . . ? N54 Re2 N15 79.6(2) . . ? C38 Re3 C36 89.0(4) . . ? C38 Re3 C37 90.4(3) . . ? C36 Re3 C37 87.1(4) . . ? C38 Re3 N75 92.8(3) . . ? C36 Re3 N75 99.7(3) . . ? C37 Re3 N75 172.5(3) . . ? C38 Re3 N68 98.6(3) . . ? C36 Re3 N68 170.5(3) . . ? C37 Re3 N68 98.4(3) . . ? N75 Re3 N68 74.5(2) . . ? C38 Re3 N21 177.4(3) . . ? C36 Re3 N21 92.2(3) . . ? C37 Re3 N21 92.0(3) . . ? N75 Re3 N21 84.7(2) . . ? N68 Re3 N21 79.9(2) . . ? C6 N1 C2 114.7(6) . . ? C2 N3 C4 114.3(6) . . ? C6 N5 C4 113.5(6) . . ? C10 N9 C8 117.8(7) . . ? C10 N9 Re1 120.1(6) . . ? C8 N9 Re1 121.9(5) . . ? C16 N15 C14 116.8(7) . . ? C16 N15 Re2 118.6(5) . . ? C14 N15 Re2 124.2(5) . . ? C20 N21 C22 117.6(6) . . ? C20 N21 Re3 122.0(5) . . ? C22 N21 Re3 120.4(5) . . ? C45 N40 C41 117.8(7) . . ? C45 N40 Re1 125.2(6) . . ? C41 N40 Re1 116.9(5) . . ? C52 N47 C48 117.4(7) . . ? C52 N47 Re1 125.1(6) . . ? C48 N47 Re1 116.3(5) . . ? C59 N54 C55 117.6(8) . . ? C59 N54 Re2 125.0(6) . . ? C55 N54 Re2 116.7(6) . . ? C62 N61 C66 118.8(7) . . ? C62 N61 Re2 116.9(6) . . ? C66 N61 Re2 123.8(6) . . ? C73 N68 C69 118.6(8) . . ? C73 N68 Re3 124.8(6) . . ? C69 N68 Re3 115.4(5) . . ? C80 N75 C76 118.1(7) . . ? C80 N75 Re3 124.8(6) . . ? C76 N75 Re3 117.0(5) . . ? N1 C2 N3 125.7(7) . . ? N1 C2 C7 116.3(7) . . ? N3 C2 C7 118.0(7) . . ? N3 C4 N5 125.3(7) . . ? N3 C4 C13 118.0(6) . . ? N5 C4 C13 116.7(6) . . ? N1 C6 N5 126.4(7) . . ? N1 C6 C19 116.6(7) . . ? N5 C6 C19 117.0(6) . . ? C8 C7 C12 119.2(7) . . ? C8 C7 C2 118.7(7) . . ? C12 C7 C2 122.0(7) . . ? N9 C8 C7 122.3(7) . . ? N9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? N9 C10 C11 122.7(8) . . ? N9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C10 C11 C12 120.1(9) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 117.7(8) . . ? C11 C12 H12 121.1 . . ? C7 C12 H12 121.1 . . ? C14 C13 C18 118.5(7) . . ? C14 C13 C4 120.3(7) . . ? C18 C13 C4 121.2(7) . . ? N15 C14 C13 123.3(7) . . ? N15 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? N15 C16 C17 124.5(7) . . ? N15 C16 H16 117.8 . . ? C17 C16 H16 117.8 . . ? C16 C17 C18 117.5(7) . . ? C16 C17 H17 121.3 . . ? C18 C17 H17 121.3 . . ? C13 C18 C17 119.3(8) . . ? C13 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C24 C19 C20 118.5(7) . . ? C24 C19 C6 120.8(7) . . ? C20 C19 C6 120.7(7) . . ? N21 C20 C19 122.1(7) . . ? N21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? N21 C22 C23 123.2(7) . . ? N21 C22 H22 118.4 . . ? C23 C22 H22 118.4 . . ? C22 C23 C24 119.2(7) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C23 C24 C19 119.4(7) . . ? C23 C24 H24 120.3 . . ? C19 C24 H24 120.3 . . ? O30 C30 Re1 178.6(9) . . ? O31 C31 Re1 177.8(9) . . ? O32 C32 Re1 174.8(8) . . ? O33 C33 Re2 179.2(8) . . ? O34 C34 Re2 175.1(8) . . ? O35 C35 Re2 177.8(8) . . ? O36 C36 Re3 177.9(9) . . ? O37 C37 Re3 178.0(8) . . ? O38 C38 Re3 177.9(7) . . ? N40 C41 C42 121.3(8) . . ? N40 C41 C48 114.9(7) . . ? C42 C41 C48 123.8(7) . . ? C43 C42 C41 121.4(8) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C42 C43 C44 116.9(8) . . ? C42 C43 C46 121.8(9) . . ? C44 C43 C46 121.2(9) . . ? C45 C44 C43 120.0(9) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? N40 C45 C44 122.3(8) . . ? N40 C45 H45 118.9 . . ? C44 C45 H45 118.9 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N47 C48 C49 121.9(8) . . ? N47 C48 C41 115.1(7) . . ? C49 C48 C41 122.9(8) . . ? C48 C49 C50 120.4(8) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C51 C50 C49 117.4(8) . . ? C51 C50 C53 120.3(9) . . ? C49 C50 C53 122.4(9) . . ? C52 C51 C50 118.9(8) . . ? C52 C51 H51 120.5 . . ? C50 C51 H51 120.5 . . ? N47 C52 C51 124.0(9) . . ? N47 C52 H52 118.0 . . ? C51 C52 H52 118.0 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N54 C55 C56 121.1(8) . . ? N54 C55 C62 115.1(8) . . ? C56 C55 C62 123.9(8) . . ? C57 C56 C55 121.4(8) . . ? C57 C56 H56 119.3 . . ? C55 C56 H56 119.3 . . ? C56 C57 C58 117.1(8) . . ? C56 C57 C60 122.1(9) . . ? C58 C57 C60 120.8(9) . . ? C57 C58 C59 120.0(9) . . ? C57 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? N54 C59 C58 122.9(8) . . ? N54 C59 H59 118.6 . . ? C58 C59 H59 118.6 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N61 C62 C63 120.7(9) . . ? N61 C62 C55 115.6(7) . . ? C63 C62 C55 123.8(8) . . ? C64 C63 C62 121.4(9) . . ? C64 C63 H63 119.3 . . ? C62 C63 H63 119.3 . . ? C65 C64 C63 115.9(9) . . ? C65 C64 C67 122.3(10) . . ? C63 C64 C67 121.8(10) . . ? C66 C65 C64 121.8(10) . . ? C66 C65 H65 119.1 . . ? C64 C65 H65 119.1 . . ? N61 C66 C65 121.3(9) . . ? N61 C66 H66 119.4 . . ? C65 C66 H66 119.4 . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N68 C69 C70 121.0(8) . . ? N68 C69 C76 115.4(7) . . ? C70 C69 C76 123.5(8) . . ? C69 C70 C71 119.8(9) . . ? C69 C70 H70 120.1 . . ? C71 C70 H70 120.1 . . ? C72 C71 C70 118.3(8) . . ? C72 C71 C74 122.6(10) . . ? C70 C71 C74 119.1(10) . . ? C71 C72 C73 119.8(9) . . ? C71 C72 H72 120.1 . . ? C73 C72 H72 120.1 . . ? N68 C73 C72 122.3(9) . . ? N68 C73 H73 118.8 . . ? C72 C73 H73 118.8 . . ? C71 C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C71 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N75 C76 C77 121.6(8) . . ? N75 C76 C69 114.9(7) . . ? C77 C76 C69 123.4(8) . . ? C76 C77 C78 120.1(9) . . ? C76 C77 H77 119.9 . . ? C78 C77 H77 119.9 . . ? C79 C78 C77 117.1(9) . . ? C79 C78 C81 122.5(11) . . ? C77 C78 C81 120.4(11) . . ? C80 C79 C78 120.9(9) . . ? C80 C79 H79 119.5 . . ? C78 C79 H79 119.5 . . ? N75 C80 C79 122.0(9) . . ? N75 C80 H80 119.0 . . ? C79 C80 H80 119.0 . . ? C78 C81 H81A 109.5 . . ? C78 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C78 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? F2 P1 F3 92.8(7) . . ? F2 P1 F1 97.6(9) . . ? F3 P1 F1 91.1(8) . . ? F2 P1 F6 90.8(8) . . ? F3 P1 F6 174.4(10) . . ? F1 P1 F6 92.8(9) . . ? F2 P1 F5 172.5(10) . . ? F3 P1 F5 89.0(4) . . ? F1 P1 F5 89.7(5) . . ? F6 P1 F5 86.9(7) . . ? F2 P1 F4 86.2(9) . . ? F3 P1 F4 87.8(5) . . ? F1 P1 F4 176.1(6) . . ? F6 P1 F4 88.1(10) . . ? F5 P1 F4 86.6(6) . . ? F9 P2 F8 93.6(6) . . ? F9 P2 F12 94.2(7) . . ? F8 P2 F12 87.8(7) . . ? F9 P2 F10 87.8(6) . . ? F8 P2 F10 92.3(7) . . ? F12 P2 F10 178.1(6) . . ? F9 P2 F7 179.0(5) . . ? F8 P2 F7 87.3(6) . . ? F12 P2 F7 86.2(6) . . ? F10 P2 F7 91.9(6) . . ? F9 P2 F11 89.9(5) . . ? F8 P2 F11 176.3(7) . . ? F12 P2 F11 93.1(6) . . ? F10 P2 F11 86.8(6) . . ? F7 P2 F11 89.1(6) . . ? F13 P3 F18 96.0(6) . . ? F13 P3 F14 93.9(6) . . ? F18 P3 F14 94.2(6) . . ? F13 P3 F16 88.1(7) . . ? F18 P3 F16 93.0(6) . . ? F14 P3 F16 172.3(5) . . ? F13 P3 F17 88.0(6) . . ? F18 P3 F17 175.9(6) . . ? F14 P3 F17 85.2(5) . . ? F16 P3 F17 87.4(5) . . ? F13 P3 F15 172.8(7) . . ? F18 P3 F15 89.0(5) . . ? F14 P3 F15 90.8(6) . . ? F16 P3 F15 86.6(7) . . ? F17 P3 F15 87.0(5) . . ? O91 C90 C92 121.338(1) . . ? O91 C90 C93 120.765(2) . . ? C92 C90 C93 117.896(1) . . ? C90 C92 H92A 109.5 . . ? C90 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C90 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C90 C93 H93A 109.5 . . ? C90 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C90 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? O95 C94 C96 131.280(1) . . ? O95 C94 C97 125.041(1) . . ? C96 C94 C97 102.002(1) . . ? C94 C96 H96A 109.5 . . ? C94 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C94 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C94 C97 H97A 109.5 . . ? C94 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C94 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.952 _refine_diff_density_min -1.283 _refine_diff_density_rms 0.172