# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Pope, Simon' _publ_contact_author_email popesj@cardiff.ac.uk _publ_section_title ; The development of responsive luminescent lifetime probes based upon axially functionalised fac-{Re(CO)3(di-imine)(L)}+ complexes ; loop_ _publ_author_name S.Pope L.Mullice # Attachment '- sjp0920.cif' data_sjp0920 _database_code_depnum_ccdc_archive 'CCDC 768922' #TrackingRef '- sjp0920.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H28 N4 O3 Re S2, C F3 S O3' _chemical_formula_sum 'C34 H28 F3 N4 O6 Re S3' _chemical_formula_weight 927.98 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 14.6110(4) _cell_length_b 13.6180(4) _cell_length_c 18.0200(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.6000(10) _cell_angle_gamma 90.00 _cell_volume 3484.95(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4496 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 3.734 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3166 _exptl_absorpt_correction_T_max 0.8650 _exptl_absorpt_process_details Denzo/Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14284 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.1010 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7920 _reflns_number_gt 4496 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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^)+(0.0553P)^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 7920 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1183 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1114 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 C1 C 0.4355(6) 0.1174(5) 0.1652(4) 0.046(2) Uani 1 1 d . . . H1A H 0.3958 0.1746 0.1684 0.068 Uiso 1 1 calc R . . H1B H 0.4030 0.0742 0.1239 0.068 Uiso 1 1 calc R . . H1C H 0.4951 0.1394 0.1549 0.068 Uiso 1 1 calc R . . C2 C 0.4544(5) 0.0630(5) 0.2387(4) 0.0353(17) Uani 1 1 d . . . C3 C 0.4093(5) -0.0270(5) 0.2418(4) 0.0367(18) Uani 1 1 d . . . H3 H 0.3633 -0.0490 0.1986 0.044 Uiso 1 1 calc R . . C4 C 0.4299(6) -0.0831(5) 0.3052(5) 0.043(2) Uani 1 1 d . . . H4 H 0.3981 -0.1435 0.3071 0.052 Uiso 1 1 calc R . . C5 C 0.5002(5) -0.0505(5) 0.3695(4) 0.0350(18) Uani 1 1 d . . . C6 C 0.5392(5) 0.0425(5) 0.3650(4) 0.0312(16) Uani 1 1 d . . . C7 C 0.6071(5) 0.0783(5) 0.4287(4) 0.0325(16) Uani 1 1 d . . . C8 C 0.6366(5) 0.0198(5) 0.4940(4) 0.0395(18) Uani 1 1 d . . . C9 C 0.5951(6) -0.0746(5) 0.4958(5) 0.045(2) Uani 1 1 d . . . H9 H 0.6143 -0.1145 0.5400 0.054 Uiso 1 1 calc R . . C10 C 0.5303(6) -0.1078(5) 0.4372(5) 0.049(2) Uani 1 1 d . . . H10 H 0.5034 -0.1708 0.4401 0.059 Uiso 1 1 calc R . . C11 C 0.7037(6) 0.0597(6) 0.5552(5) 0.053(2) Uani 1 1 d . . . H11 H 0.7225 0.0241 0.6017 0.063 Uiso 1 1 calc R . . C12 C 0.7414(6) 0.1477(6) 0.5484(5) 0.053(2) Uani 1 1 d . . . H12 H 0.7870 0.1743 0.5900 0.063 Uiso 1 1 calc R . . C13 C 0.7146(6) 0.2004(6) 0.4811(5) 0.0439(19) Uani 1 1 d . . . C14 C 0.7679(6) 0.2949(7) 0.4741(5) 0.063(2) Uani 1 1 d . . . H14A H 0.7818 0.2978 0.4235 0.094 Uiso 1 1 calc R . . H14B H 0.8270 0.2960 0.5135 0.094 Uiso 1 1 calc R . . H14C H 0.7293 0.3515 0.4808 0.094 Uiso 1 1 calc R . . C15 C 0.5112(5) 0.3112(5) 0.2257(5) 0.0372(18) Uani 1 1 d . . . C16 C 0.6778(5) 0.2092(5) 0.2665(4) 0.0348(17) Uani 1 1 d . . . C17 C 0.6341(5) 0.3755(5) 0.3368(5) 0.0414(19) Uani 1 1 d . . . C18 C 0.3744(5) 0.2596(4) 0.3417(4) 0.0332(16) Uani 1 1 d . . . H18 H 0.3602 0.2251 0.2946 0.040 Uiso 1 1 calc R . . C19 C 0.3018(5) 0.2865(5) 0.3734(4) 0.0332(17) Uani 1 1 d . . . H19 H 0.2389 0.2704 0.3481 0.040 Uiso 1 1 calc R . . C20 C 0.3184(5) 0.3360(4) 0.4409(4) 0.0330(17) Uani 1 1 d . . . C21 C 0.4102(5) 0.3572(5) 0.4761(4) 0.0373(18) Uani 1 1 d . . . H21 H 0.4244 0.3913 0.5234 0.045 Uiso 1 1 calc R . . C22 C 0.4828(5) 0.3285(5) 0.4423(4) 0.0368(18) Uani 1 1 d . . . H22 H 0.5460 0.3430 0.4674 0.044 Uiso 1 1 calc R . . C23 C 0.2381(5) 0.3678(5) 0.4768(5) 0.0411(19) Uani 1 1 d . . . H23A H 0.2645 0.4044 0.5245 0.049 Uiso 1 1 calc R . . H23B H 0.1955 0.4126 0.4413 0.049 Uiso 1 1 calc R . . C24 C 0.2388(5) 0.2288(5) 0.5604(5) 0.044(2) Uani 1 1 d . . . H24A H 0.2415 0.2670 0.6077 0.053 Uiso 1 1 calc R . . H24B H 0.3040 0.2196 0.5547 0.053 Uiso 1 1 calc R . . C25 C 0.1937(5) 0.1289(5) 0.5665(5) 0.046(2) Uani 1 1 d . . . C26 C 0.1377(4) 0.0727(4) 0.5082(4) 0.0308(17) Uani 1 1 d . . . H26 H 0.1173 0.0903 0.4559 0.037 Uiso 1 1 calc R . . C27 C 0.1166(6) -0.0190(6) 0.5438(6) 0.062(3) Uani 1 1 d . . . H27 H 0.0800 -0.0699 0.5152 0.074 Uiso 1 1 calc R . . C28 C 0.1523(6) -0.0262(6) 0.6190(7) 0.068(3) Uani 1 1 d . . . H28 H 0.1427 -0.0809 0.6490 0.081 Uiso 1 1 calc R . . C29 C 0.0914(5) 0.3140(6) 0.5069(5) 0.047(2) Uani 1 1 d . . . H29A H 0.1006 0.3728 0.5401 0.057 Uiso 1 1 calc R . . H29B H 0.0660 0.2610 0.5339 0.057 Uiso 1 1 calc R . . C30 C 0.0219(5) 0.3371(5) 0.4346(5) 0.051(2) Uani 1 1 d . . . C31 C -0.0456(5) 0.4128(6) 0.4198(6) 0.057(2) Uani 1 1 d . . . H31 H -0.0529 0.4625 0.4550 0.068 Uiso 1 1 calc R . . C32 C -0.1010(6) 0.4036(7) 0.3442(7) 0.073(3) Uani 1 1 d . . . H32 H -0.1503 0.4481 0.3232 0.088 Uiso 1 1 calc R . . C33 C -0.0784(6) 0.3259(8) 0.3035(6) 0.078(3) Uani 1 1 d . . . H33 H -0.1094 0.3105 0.2524 0.094 Uiso 1 1 calc R . . C34 C 0.1234(7) 0.0491(6) 0.2188(6) 0.057(2) Uani 1 1 d . . . O1 O 0.4753(4) 0.3522(4) 0.1702(3) 0.0522(15) Uani 1 1 d . . . O2 O 0.7330(4) 0.1820(4) 0.2364(3) 0.0525(15) Uani 1 1 d . . . O3 O 0.6640(4) 0.4535(4) 0.3450(3) 0.0592(17) Uani 1 1 d . . . O4 O 0.0790(5) 0.1818(5) 0.1192(5) 0.114(3) Uani 1 1 d . . . O5 O 0.1939(6) 0.0664(4) 0.1040(4) 0.104(3) Uani 1 1 d . . . O6 O 0.2297(4) 0.1918(4) 0.2002(3) 0.0697(18) Uani 1 1 d . . . S1 S 0.21647(19) 0.07334(18) 0.65452(16) 0.0727(8) Uani 1 1 d . . . S2 S 0.0129(2) 0.26058(16) 0.35739(17) 0.0697(7) Uani 1 1 d . . . S3 S 0.16131(15) 0.13048(13) 0.15301(12) 0.0473(5) Uani 1 1 d . . . Re1 Re 0.579319(18) 0.247306(19) 0.315933(15) 0.03098(11) Uani 1 1 d . . . N1 N 0.5150(4) 0.0996(4) 0.3004(3) 0.0300(13) Uani 1 1 d . . . N2 N 0.6467(4) 0.1696(4) 0.4225(3) 0.0324(14) Uani 1 1 d . . . N3 N 0.4651(4) 0.2801(4) 0.3742(3) 0.0281(13) Uani 1 1 d . . . N4 N 0.1834(4) 0.2829(4) 0.4942(4) 0.0422(16) Uani 1 1 d . . . F1 F 0.0532(4) -0.0079(4) 0.1852(3) 0.0843(18) Uani 1 1 d . . . F2 F 0.0987(6) 0.0928(5) 0.2732(4) 0.138(3) Uani 1 1 d . . . F3 F 0.1898(5) -0.0138(5) 0.2485(4) 0.122(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.058(5) 0.034(4) 0.038(5) -0.001(3) -0.001(4) -0.003(4) C2 0.041(4) 0.039(4) 0.028(4) -0.003(3) 0.012(4) 0.002(3) C3 0.042(5) 0.032(4) 0.036(5) -0.001(3) 0.009(4) -0.003(3) C4 0.060(6) 0.029(4) 0.046(5) -0.012(4) 0.022(5) 0.002(4) C5 0.037(4) 0.032(4) 0.040(5) 0.005(3) 0.018(4) 0.005(3) C6 0.033(4) 0.032(4) 0.032(4) 0.003(3) 0.013(4) 0.014(3) C7 0.038(4) 0.039(4) 0.020(4) 0.004(3) 0.005(3) 0.014(3) C8 0.037(4) 0.051(5) 0.034(5) 0.002(4) 0.013(4) 0.010(4) C9 0.053(5) 0.045(5) 0.037(5) 0.018(4) 0.014(4) 0.020(4) C10 0.068(6) 0.037(4) 0.049(6) 0.011(4) 0.028(5) 0.019(4) C11 0.044(5) 0.074(6) 0.037(5) 0.015(5) 0.003(4) 0.033(5) C12 0.046(5) 0.068(6) 0.035(5) -0.006(4) -0.012(4) 0.005(4) C13 0.043(5) 0.051(5) 0.036(5) -0.008(4) 0.006(4) 0.007(4) C14 0.054(6) 0.084(6) 0.040(6) -0.012(5) -0.006(5) -0.019(5) C15 0.029(4) 0.042(4) 0.043(5) 0.005(4) 0.013(4) 0.002(3) C16 0.031(4) 0.033(3) 0.034(5) -0.001(3) -0.005(4) 0.004(3) C17 0.029(4) 0.045(4) 0.050(5) 0.002(4) 0.008(4) 0.007(4) C18 0.035(4) 0.027(3) 0.035(4) 0.004(3) 0.003(3) 0.000(3) C19 0.030(4) 0.026(3) 0.039(5) 0.003(3) 0.000(4) 0.003(3) C20 0.038(4) 0.026(3) 0.034(5) 0.007(3) 0.007(4) 0.005(3) C21 0.046(5) 0.032(4) 0.034(5) -0.003(3) 0.011(4) 0.005(3) C22 0.038(4) 0.031(4) 0.037(5) 0.004(3) 0.002(4) 0.001(3) C23 0.037(4) 0.034(4) 0.056(5) -0.002(4) 0.018(4) 0.004(3) C24 0.038(4) 0.054(5) 0.040(5) -0.004(4) 0.008(4) 0.007(3) C25 0.047(5) 0.039(4) 0.062(6) 0.021(4) 0.031(5) 0.018(4) C26 0.021(3) 0.018(3) 0.053(5) 0.002(3) 0.007(3) -0.002(3) C27 0.045(6) 0.051(5) 0.085(8) -0.002(5) 0.006(6) 0.006(4) C28 0.051(6) 0.048(5) 0.106(9) 0.016(6) 0.023(6) 0.005(4) C29 0.040(5) 0.046(5) 0.059(6) 0.012(4) 0.019(5) 0.009(4) C30 0.038(5) 0.046(4) 0.076(7) 0.006(4) 0.028(5) -0.004(4) C31 0.034(5) 0.053(5) 0.074(7) 0.002(5) -0.007(5) 0.006(4) C32 0.040(6) 0.076(7) 0.105(10) 0.015(6) 0.018(6) 0.006(5) C33 0.043(6) 0.100(8) 0.078(8) 0.025(7) -0.011(6) -0.027(6) C34 0.062(6) 0.046(5) 0.065(7) -0.012(5) 0.023(6) 0.000(5) O1 0.052(4) 0.049(3) 0.050(4) 0.018(3) 0.002(3) 0.000(3) O2 0.049(4) 0.065(4) 0.049(4) 0.009(3) 0.023(3) 0.017(3) O3 0.057(4) 0.038(3) 0.081(5) -0.003(3) 0.011(3) -0.012(3) O4 0.084(5) 0.068(5) 0.151(8) 0.044(5) -0.052(5) -0.003(4) O5 0.181(8) 0.066(4) 0.096(6) -0.038(4) 0.093(6) -0.055(5) O6 0.067(4) 0.068(4) 0.065(5) -0.013(3) -0.003(4) -0.027(3) S1 0.0778(18) 0.0695(15) 0.075(2) 0.0193(14) 0.0255(16) 0.0116(13) S2 0.0774(17) 0.0586(15) 0.0726(18) 0.0030(13) 0.0165(15) -0.0025(12) S3 0.0583(14) 0.0346(10) 0.0407(13) -0.0024(9) -0.0050(11) -0.0075(10) Re1 0.03011(16) 0.03199(16) 0.03032(17) 0.00137(15) 0.00607(12) -0.00003(14) N1 0.031(3) 0.028(3) 0.030(3) 0.002(3) 0.007(3) 0.006(2) N2 0.028(3) 0.044(3) 0.023(4) -0.003(3) 0.003(3) 0.011(3) N3 0.027(3) 0.023(3) 0.032(4) -0.001(2) 0.003(3) -0.001(2) N4 0.043(4) 0.045(3) 0.045(4) 0.009(3) 0.023(3) 0.011(3) F1 0.092(4) 0.057(3) 0.109(5) -0.009(3) 0.035(4) -0.033(3) F2 0.226(8) 0.099(5) 0.130(6) -0.063(4) 0.124(6) -0.062(5) F3 0.126(6) 0.113(5) 0.118(6) 0.068(5) 0.013(5) 0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.486(10) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.343(8) . ? C2 C3 1.399(9) . ? C3 C4 1.348(10) . ? C3 H3 0.9500 . ? C4 C5 1.425(10) . ? C4 H4 0.9500 . ? C5 C6 1.399(9) . ? C5 C10 1.428(10) . ? C6 N1 1.375(8) . ? C6 C7 1.415(9) . ? C7 N2 1.386(8) . ? C7 C8 1.403(9) . ? C8 C11 1.402(11) . ? C8 C9 1.426(10) . ? C9 C10 1.321(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.337(11) . ? C11 H11 0.9500 . ? C12 C13 1.384(11) . ? C12 H12 0.9500 . ? C13 N2 1.335(9) . ? C13 C14 1.525(12) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 O1 1.156(8) . ? C15 Re1 1.906(8) . ? C16 O2 1.136(8) . ? C16 Re1 1.932(8) . ? C17 O3 1.145(8) . ? C17 Re1 1.920(8) . ? C18 N3 1.346(8) . ? C18 C19 1.369(9) . ? C18 H18 0.9500 . ? C19 C20 1.360(9) . ? C19 H19 0.9500 . ? C20 C21 1.374(9) . ? C20 C23 1.530(9) . ? C21 C22 1.397(9) . ? C21 H21 0.9500 . ? C22 N3 1.362(9) . ? C22 H22 0.9500 . ? C23 N4 1.481(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N4 1.473(10) . ? C24 C25 1.525(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.399(10) . ? C25 S1 1.718(8) . ? C26 C27 1.470(10) . ? C26 H26 0.9500 . ? C27 C28 1.337(12) . ? C27 H27 0.9500 . ? C28 S1 1.686(9) . ? C28 H28 0.9500 . ? C29 N4 1.478(8) . ? C29 C30 1.485(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.409(10) . ? C30 S2 1.719(9) . ? C31 C32 1.416(12) . ? C31 H31 0.9500 . ? C32 C33 1.372(13) . ? C32 H32 0.9500 . ? C33 S2 1.704(10) . ? C33 H33 0.9500 . ? C34 F2 1.271(9) . ? C34 F3 1.310(10) . ? C34 F1 1.314(10) . ? C34 S3 1.802(9) . ? O4 S3 1.400(6) . ? O5 S3 1.403(6) . ? O6 S3 1.421(5) . ? Re1 N1 2.210(5) . ? Re1 N2 2.211(6) . ? Re1 N3 2.216(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 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 . . ? N1 C2 C3 121.1(7) . . ? N1 C2 C1 120.0(6) . . ? C3 C2 C1 118.8(7) . . ? C4 C3 C2 121.1(7) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.2(7) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 117.4(7) . . ? C6 C5 C10 119.7(7) . . ? C4 C5 C10 122.8(7) . . ? N1 C6 C5 122.2(7) . . ? N1 C6 C7 118.9(6) . . ? C5 C6 C7 118.9(6) . . ? N2 C7 C8 121.6(7) . . ? N2 C7 C6 118.1(6) . . ? C8 C7 C6 120.2(7) . . ? C11 C8 C7 117.5(7) . . ? C11 C8 C9 123.6(8) . . ? C7 C8 C9 118.9(7) . . ? C10 C9 C8 121.2(7) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C5 121.0(8) . . ? C9 C10 H10 119.5 . . ? C5 C10 H10 119.5 . . ? C12 C11 C8 120.1(8) . . ? C12 C11 H11 120.0 . . ? C8 C11 H11 120.0 . . ? C11 C12 C13 120.5(8) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? N2 C13 C12 122.3(8) . . ? N2 C13 C14 119.9(7) . . ? C12 C13 C14 117.7(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C15 Re1 175.6(6) . . ? O2 C16 Re1 176.2(7) . . ? O3 C17 Re1 176.0(7) . . ? N3 C18 C19 122.9(7) . . ? N3 C18 H18 118.6 . . ? C19 C18 H18 118.6 . . ? C20 C19 C18 120.9(7) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 117.8(7) . . ? C19 C20 C23 121.7(7) . . ? C21 C20 C23 120.5(7) . . ? C20 C21 C22 119.9(7) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? N3 C22 C21 121.7(7) . . ? N3 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? N4 C23 C20 112.0(5) . . ? N4 C23 H23A 109.2 . . ? C20 C23 H23A 109.2 . . ? N4 C23 H23B 109.2 . . ? C20 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? N4 C24 C25 109.9(7) . . ? N4 C24 H24A 109.7 . . ? C25 C24 H24A 109.7 . . ? N4 C24 H24B 109.7 . . ? C25 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C26 C25 C24 128.3(7) . . ? C26 C25 S1 113.8(5) . . ? C24 C25 S1 117.8(7) . . ? C25 C26 C27 106.4(7) . . ? C25 C26 H26 126.8 . . ? C27 C26 H26 126.8 . . ? C28 C27 C26 115.6(8) . . ? C28 C27 H27 122.2 . . ? C26 C27 H27 122.2 . . ? C27 C28 S1 112.1(7) . . ? C27 C28 H28 124.0 . . ? S1 C28 H28 124.0 . . ? N4 C29 C30 112.6(7) . . ? N4 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? N4 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C31 C30 C29 128.7(8) . . ? C31 C30 S2 111.9(7) . . ? C29 C30 S2 119.2(6) . . ? C30 C31 C32 109.5(8) . . ? C30 C31 H31 125.3 . . ? C32 C31 H31 125.3 . . ? C33 C32 C31 115.3(9) . . ? C33 C32 H32 122.3 . . ? C31 C32 H32 122.3 . . ? C32 C33 S2 110.6(8) . . ? C32 C33 H33 124.7 . . ? S2 C33 H33 124.7 . . ? F2 C34 F3 108.0(10) . . ? F2 C34 F1 107.4(8) . . ? F3 C34 F1 103.0(7) . . ? F2 C34 S3 114.0(6) . . ? F3 C34 S3 111.0(7) . . ? F1 C34 S3 112.8(7) . . ? C28 S1 C25 92.0(5) . . ? C33 S2 C30 92.6(5) . . ? O4 S3 O5 114.9(6) . . ? O4 S3 O6 112.2(4) . . ? O5 S3 O6 116.6(4) . . ? O4 S3 C34 103.2(5) . . ? O5 S3 C34 103.5(4) . . ? O6 S3 C34 104.5(4) . . ? C15 Re1 C17 82.1(3) . . ? C15 Re1 C16 91.4(3) . . ? C17 Re1 C16 90.7(3) . . ? C15 Re1 N1 100.7(3) . . ? C17 Re1 N1 175.9(3) . . ? C16 Re1 N1 92.2(2) . . ? C15 Re1 N2 175.1(2) . . ? C17 Re1 N2 100.6(3) . . ? C16 Re1 N2 92.5(2) . . ? N1 Re1 N2 76.3(2) . . ? C15 Re1 N3 90.7(3) . . ? C17 Re1 N3 92.8(2) . . ? C16 Re1 N3 176.0(2) . . ? N1 Re1 N3 84.16(19) . . ? N2 Re1 N3 85.2(2) . . ? C2 N1 C6 118.6(6) . . ? C2 N1 Re1 128.4(5) . . ? C6 N1 Re1 112.9(5) . . ? C13 N2 C7 117.7(6) . . ? C13 N2 Re1 129.2(5) . . ? C7 N2 Re1 112.9(4) . . ? C18 N3 C22 116.8(6) . . ? C18 N3 Re1 121.7(5) . . ? C22 N3 Re1 121.3(5) . . ? C24 N4 C29 111.3(6) . . ? C24 N4 C23 109.9(6) . . ? C29 N4 C23 111.4(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.971 _refine_diff_density_min -1.562 _refine_diff_density_rms 0.154