Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kuang-Lieh Lu' _publ_contact_author_address ; Academia Sinica Institute of Chemistry, Academia Sinica Taipei 115 TAIWAN ; _publ_contact_author_email LU@CHEM.SINICA.EDU.TW _publ_section_title ; Rigidity-modulated conformation control: A strategy for incorporating flexible building motifs into metallacycles ; loop_ _publ_author_name 'Kuang-Lieh Lu.' 'Che-Hao Chang.' 'Chuan-Hung Chuang.' 'Tzuoo-Tsair Luo.' ; M.Sathiyendiran ; 'Yuh-Sheng Wen.' data_3609 _database_code_depnum_ccdc_archive 'CCDC 632400' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H26 N8 O6 Re2' _chemical_formula_sum 'C42 H26 N8 O6 Re2' _chemical_formula_weight 1111.11 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.82300(10) _cell_length_b 10.48100(10) _cell_length_c 21.4330(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.59 _cell_angle_gamma 90.00 _cell_volume 3844.94(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 54174 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 6.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2654 _exptl_absorpt_correction_T_max 0.4596 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21160 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6777 _reflns_number_gt 6063 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1' _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^)+(0.0321P)^2^+1.8845P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6777 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re -0.148472(10) 0.408577(16) 0.273143(9) 0.03597(7) Uani 1 1 d . . . Re2 Re 0.173619(10) 0.387222(16) 0.323599(9) 0.03734(7) Uani 1 1 d . . . O1 O -0.2376(2) 0.5485(4) 0.3435(2) 0.0735(11) Uani 1 1 d . . . O2 O -0.3016(2) 0.3523(4) 0.1487(2) 0.0659(10) Uani 1 1 d . . . O3 O -0.1777(2) 0.1618(3) 0.33463(18) 0.0605(10) Uani 1 1 d . . . O4 O 0.2525(2) 0.1723(4) 0.4258(2) 0.0926(15) Uani 1 1 d . . . O5 O 0.2553(3) 0.2906(5) 0.2356(2) 0.0862(14) Uani 1 1 d . . . O6 O 0.3200(2) 0.5422(4) 0.4089(2) 0.0769(12) Uani 1 1 d . . . N1 N -0.0312(2) 0.4564(3) 0.35336(18) 0.0384(8) Uani 1 1 d . . . N2 N -0.0695(2) 0.3133(3) 0.23435(17) 0.0362(8) Uani 1 1 d . . . N3 N 0.0606(2) 0.2940(3) 0.25865(18) 0.0370(8) Uani 1 1 d . . . N4 N 0.0975(2) 0.4455(3) 0.37409(17) 0.0374(8) Uani 1 1 d . . . N5 N 0.1174(2) 0.5530(3) 0.25858(18) 0.0393(8) Uani 1 1 d . . . N6 N 0.0767(2) 0.7536(3) 0.2329(2) 0.0451(9) Uani 1 1 d . . . N7 N -0.1071(2) 0.7936(3) 0.2226(2) 0.0482(10) Uani 1 1 d . . . N8 N -0.1270(2) 0.5866(3) 0.2288(2) 0.0433(9) Uani 1 1 d . . . C1 C -0.2041(3) 0.4970(5) 0.3164(3) 0.0484(12) Uani 1 1 d . . . C2 C -0.2436(3) 0.3743(4) 0.1947(3) 0.0460(12) Uani 1 1 d . . . C3 C -0.1652(3) 0.2537(5) 0.3123(2) 0.0437(11) Uani 1 1 d . . . C4 C 0.2211(3) 0.2506(5) 0.3859(3) 0.0551(13) Uani 1 1 d . . . C5 C 0.2251(3) 0.3292(5) 0.2692(3) 0.0533(13) Uani 1 1 d . . . C6 C 0.2641(3) 0.4853(5) 0.3767(2) 0.0491(12) Uani 1 1 d . . . C7 C 0.0105(3) 0.5364(4) 0.4089(2) 0.0399(10) Uani 1 1 d . . . C8 C -0.0138(3) 0.6171(4) 0.4483(3) 0.0495(12) Uani 1 1 d . . . H8 H -0.0679 0.6210 0.4401 0.059 Uiso 1 1 d R . . C9 C 0.0417(4) 0.6873(5) 0.4984(3) 0.0628(15) Uani 1 1 d . . . H9 H 0.0255 0.7442 0.5251 0.075 Uiso 1 1 d R . . C10 C 0.1205(4) 0.6786(5) 0.5116(3) 0.0631(15) Uani 1 1 d . . . H10 H 0.1579 0.7302 0.5471 0.076 Uiso 1 1 d R . . C11 C 0.1462(3) 0.5996(5) 0.4741(3) 0.0548(14) Uani 1 1 d . . . H11 H 0.2002 0.5895 0.4829 0.066 Uiso 1 1 d R . . C12 C 0.0900(3) 0.5281(4) 0.4216(2) 0.0393(10) Uani 1 1 d . . . C13 C 0.0239(3) 0.4098(4) 0.3369(2) 0.0357(10) Uani 1 1 d . . . C14 C 0.0049(2) 0.3348(4) 0.2767(2) 0.0354(9) Uani 1 1 d . . . C15 C -0.0624(3) 0.2462(4) 0.1812(2) 0.0361(10) Uani 1 1 d . . . C16 C -0.1187(3) 0.1968(4) 0.1205(2) 0.0440(11) Uani 1 1 d . . . H16 H -0.1737 0.2020 0.1090 0.053 Uiso 1 1 d R . . C17 C -0.0931(4) 0.1372(4) 0.0761(2) 0.0533(14) Uani 1 1 d . . . H17 H -0.1301 0.1028 0.0335 0.064 Uiso 1 1 d R . . C18 C -0.0137(4) 0.1242(4) 0.0914(3) 0.0515(13) Uani 1 1 d . . . H18 H 0.0026 0.0820 0.0598 0.062 Uiso 1 1 d R . . C19 C 0.0426(3) 0.1721(4) 0.1509(2) 0.0457(11) Uani 1 1 d . . . H19 H 0.0971 0.1629 0.1611 0.055 Uiso 1 1 d R . . C20 C 0.0180(3) 0.2342(4) 0.1960(2) 0.0376(10) Uani 1 1 d . . . C21 C 0.0984(3) 0.5733(4) 0.1893(2) 0.0395(10) Uani 1 1 d . . . C22 C 0.1008(3) 0.4926(5) 0.1392(2) 0.0482(12) Uani 1 1 d . . . H22 H 0.1160 0.4053 0.1509 0.058 Uiso 1 1 d R . . C23 C 0.0802(3) 0.5421(6) 0.0747(3) 0.0593(14) Uani 1 1 d . . . H23 H 0.0821 0.4902 0.0386 0.071 Uiso 1 1 d R . . C24 C 0.0573(4) 0.6688(6) 0.0597(3) 0.0677(16) Uani 1 1 d . . . H24 H 0.0428 0.6999 0.0140 0.081 Uiso 1 1 d R . . C25 C 0.0537(3) 0.7501(5) 0.1077(3) 0.0619(15) Uani 1 1 d . . . H25 H 0.0386 0.8382 0.1000 0.074 Uiso 1 1 d R . . C26 C 0.0737(3) 0.6994(4) 0.1732(2) 0.0434(11) Uani 1 1 d . . . C27 C 0.1031(3) 0.6639(4) 0.2814(2) 0.0417(11) Uani 1 1 d . . . H27 H 0.1119 0.6724 0.3287 0.050 Uiso 1 1 d R . . C28 C 0.0672(4) 0.8906(4) 0.2416(3) 0.0593(15) Uani 1 1 d . . . H28A H 0.1119 0.9356 0.2423 0.071 Uiso 1 1 d R . . H28B H 0.0210 0.9206 0.2039 0.071 Uiso 1 1 d R . . C29 C 0.0592(3) 0.9245(4) 0.3066(3) 0.0524(13) Uani 1 1 d . . . C30 C 0.1264(3) 0.9436(5) 0.3658(3) 0.0672(16) Uani 1 1 d . . . H30 H 0.1765 0.9335 0.3647 0.081 Uiso 1 1 d R . . C31 C 0.1218(4) 0.9761(6) 0.4267(3) 0.0779(18) Uani 1 1 d . . . H31 H 0.1690 0.9857 0.4677 0.093 Uiso 1 1 d R . . C32 C 0.0510(4) 0.9953(6) 0.4280(3) 0.0728(16) Uani 1 1 d . . . H32 H 0.0474 1.0199 0.4697 0.087 Uiso 1 1 d R . . C33 C -0.0162(3) 0.9779(5) 0.3696(3) 0.0639(15) Uani 1 1 d . . . H33 H -0.0660 0.9923 0.3708 0.077 Uiso 1 1 d R . . C34 C -0.0132(3) 0.9422(4) 0.3082(3) 0.0502(12) Uani 1 1 d . . . C35 C -0.0891(3) 0.9280(4) 0.2461(3) 0.0587(15) Uani 1 1 d . . . H35A H -0.1304 0.9575 0.2577 0.070 Uiso 1 1 d R . . H35B H -0.0881 0.9783 0.2090 0.070 Uiso 1 1 d R . . C36 C -0.1291(3) 0.7459(4) 0.1570(3) 0.0466(12) Uani 1 1 d . . . C37 C -0.1391(3) 0.8033(5) 0.0958(3) 0.0619(15) Uani 1 1 d . . . H37 H -0.1330 0.8933 0.0912 0.074 Uiso 1 1 d R . . C38 C -0.1593(3) 0.7250(6) 0.0394(3) 0.0681(16) Uani 1 1 d . . . H38 H -0.1651 0.7595 -0.0040 0.082 Uiso 1 1 d R . . C39 C -0.1706(3) 0.5947(5) 0.0437(3) 0.0577(14) Uani 1 1 d . . . H39 H -0.1853 0.5441 0.0029 0.069 Uiso 1 1 d R . . C40 C -0.1624(3) 0.5377(5) 0.1033(2) 0.0488(12) Uani 1 1 d . . . H40 H -0.1700 0.4478 0.1067 0.059 Uiso 1 1 d R . . C41 C -0.1411(3) 0.6155(4) 0.1616(2) 0.0402(11) Uani 1 1 d . . . C42 C -0.1071(3) 0.6957(4) 0.2629(3) 0.0471(11) Uani 1 1 d . . . H42 H -0.0958 0.6966 0.3108 0.057 Uiso 1 1 d 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 0.03122(12) 0.03259(11) 0.04615(13) -0.00137(7) 0.01812(9) -0.00286(7) Re2 0.02928(12) 0.03736(11) 0.04353(13) 0.00500(7) 0.01331(9) 0.00296(7) O1 0.060(2) 0.078(3) 0.094(3) -0.025(2) 0.043(2) 0.004(2) O2 0.042(2) 0.068(2) 0.070(3) -0.010(2) 0.006(2) -0.0070(19) O3 0.075(3) 0.0397(19) 0.073(2) 0.0061(17) 0.037(2) -0.0115(18) O4 0.065(3) 0.073(3) 0.115(4) 0.050(3) 0.012(3) 0.010(2) O5 0.061(3) 0.122(4) 0.084(3) -0.007(3) 0.039(2) 0.031(3) O6 0.051(2) 0.086(3) 0.082(3) -0.009(2) 0.015(2) -0.028(2) N1 0.036(2) 0.0383(19) 0.041(2) -0.0033(16) 0.0165(17) -0.0028(17) N2 0.0307(19) 0.0380(19) 0.039(2) -0.0027(15) 0.0142(17) -0.0029(16) N3 0.034(2) 0.0367(19) 0.041(2) -0.0007(15) 0.0159(17) 0.0012(16) N4 0.034(2) 0.0409(19) 0.036(2) -0.0011(16) 0.0137(17) -0.0037(17) N5 0.039(2) 0.038(2) 0.040(2) 0.0055(16) 0.0156(17) 0.0030(17) N6 0.047(2) 0.035(2) 0.054(2) 0.0083(17) 0.022(2) 0.0043(18) N7 0.037(2) 0.0308(19) 0.064(3) 0.0051(18) 0.009(2) -0.0032(17) N8 0.036(2) 0.034(2) 0.055(3) 0.0015(17) 0.0139(19) -0.0039(16) C1 0.042(3) 0.041(3) 0.060(3) -0.005(2) 0.020(2) -0.007(2) C2 0.041(3) 0.036(2) 0.061(3) 0.000(2) 0.021(3) -0.001(2) C3 0.039(3) 0.051(3) 0.046(3) -0.010(2) 0.022(2) -0.003(2) C4 0.037(3) 0.050(3) 0.069(3) 0.011(3) 0.012(3) -0.001(2) C5 0.039(3) 0.058(3) 0.059(3) 0.002(2) 0.016(3) 0.008(2) C6 0.048(3) 0.050(3) 0.052(3) 0.007(2) 0.023(2) 0.003(3) C7 0.049(3) 0.038(2) 0.035(2) 0.0022(19) 0.021(2) -0.003(2) C8 0.058(3) 0.047(3) 0.050(3) -0.004(2) 0.029(3) 0.000(2) C9 0.092(5) 0.050(3) 0.053(3) -0.014(2) 0.037(3) -0.008(3) C10 0.079(4) 0.063(3) 0.043(3) -0.014(2) 0.020(3) -0.022(3) C11 0.053(3) 0.065(3) 0.041(3) -0.002(2) 0.014(3) -0.015(3) C12 0.046(3) 0.040(2) 0.031(2) 0.0025(18) 0.016(2) -0.007(2) C13 0.035(3) 0.035(2) 0.038(3) 0.0025(17) 0.016(2) -0.0015(19) C14 0.036(2) 0.029(2) 0.043(2) -0.0011(18) 0.018(2) -0.0034(19) C15 0.042(3) 0.0253(19) 0.042(2) 0.0026(18) 0.018(2) -0.0012(19) C16 0.049(3) 0.033(2) 0.047(3) -0.002(2) 0.017(2) -0.007(2) C17 0.078(4) 0.037(2) 0.040(3) -0.001(2) 0.020(3) -0.010(3) C18 0.080(4) 0.033(2) 0.048(3) 0.002(2) 0.033(3) 0.002(3) C19 0.059(3) 0.032(2) 0.055(3) 0.001(2) 0.032(3) 0.002(2) C20 0.046(3) 0.028(2) 0.042(3) 0.0050(18) 0.022(2) 0.0014(19) C21 0.033(2) 0.047(2) 0.038(3) 0.005(2) 0.014(2) -0.004(2) C22 0.044(3) 0.054(3) 0.046(3) -0.001(2) 0.018(2) -0.005(2) C23 0.064(4) 0.074(4) 0.040(3) -0.002(3) 0.022(3) -0.003(3) C24 0.074(4) 0.079(4) 0.045(3) 0.014(3) 0.019(3) 0.001(3) C25 0.064(4) 0.059(3) 0.060(3) 0.023(3) 0.023(3) 0.012(3) C26 0.037(3) 0.042(2) 0.049(3) 0.010(2) 0.015(2) 0.002(2) C27 0.046(3) 0.036(2) 0.046(3) 0.002(2) 0.023(2) -0.001(2) C28 0.070(4) 0.036(3) 0.083(4) 0.014(2) 0.042(3) 0.010(2) C29 0.054(3) 0.031(2) 0.069(4) 0.000(2) 0.022(3) 0.000(2) C30 0.040(3) 0.057(3) 0.098(5) -0.009(3) 0.021(3) -0.005(3) C31 0.064(4) 0.071(4) 0.080(4) -0.011(3) 0.012(3) -0.010(3) C32 0.075(4) 0.071(4) 0.077(4) -0.019(3) 0.036(4) -0.010(3) C33 0.053(3) 0.051(3) 0.095(4) -0.012(3) 0.039(3) -0.003(3) C34 0.039(3) 0.031(2) 0.079(4) 0.000(2) 0.023(3) -0.002(2) C35 0.043(3) 0.033(2) 0.080(4) 0.000(2) 0.006(3) -0.004(2) C36 0.032(2) 0.037(2) 0.059(3) 0.009(2) 0.008(2) -0.002(2) C37 0.046(3) 0.050(3) 0.074(4) 0.019(3) 0.009(3) -0.005(3) C38 0.058(4) 0.078(4) 0.060(4) 0.029(3) 0.015(3) 0.002(3) C39 0.051(3) 0.065(3) 0.054(3) 0.006(2) 0.020(3) 0.001(3) C40 0.044(3) 0.047(3) 0.054(3) 0.002(2) 0.019(2) -0.002(2) C41 0.031(2) 0.038(2) 0.050(3) 0.007(2) 0.014(2) 0.0012(19) C42 0.039(3) 0.041(3) 0.055(3) 0.004(2) 0.014(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.904(5) . ? Re1 C3 1.913(5) . ? Re1 C2 1.912(5) . ? Re1 N8 2.206(4) . ? Re1 N1 2.218(3) . ? Re1 N2 2.220(3) . ? Re2 C5 1.900(6) . ? Re2 C6 1.908(5) . ? Re2 C4 1.908(5) . ? Re2 N5 2.203(3) . ? Re2 N4 2.211(4) . ? Re2 N3 2.226(3) . ? O1 C1 1.153(6) . ? O2 C2 1.150(6) . ? O3 C3 1.143(6) . ? O4 C4 1.154(6) . ? O5 C5 1.160(6) . ? O6 C6 1.156(6) . ? N1 C13 1.321(5) . ? N1 C7 1.399(5) . ? N2 C14 1.332(5) . ? N2 C15 1.392(5) . ? N3 C14 1.329(5) . ? N3 C20 1.394(5) . ? N4 C13 1.333(6) . ? N4 C12 1.388(5) . ? N5 C27 1.331(6) . ? N5 C21 1.391(6) . ? N6 C27 1.336(6) . ? N6 C26 1.379(6) . ? N6 C28 1.468(6) . ? N7 C42 1.341(6) . ? N7 C36 1.383(6) . ? N7 C35 1.487(6) . ? N8 C42 1.324(6) . ? N8 C41 1.385(6) . ? C7 C8 1.400(6) . ? C7 C12 1.409(6) . ? C8 C9 1.360(7) . ? C9 C10 1.393(8) . ? C10 C11 1.374(8) . ? C11 C12 1.399(6) . ? C13 C14 1.424(6) . ? C15 C16 1.391(6) . ? C15 C20 1.417(7) . ? C16 C17 1.383(7) . ? C17 C18 1.398(8) . ? C18 C19 1.371(7) . ? C19 C20 1.393(6) . ? C21 C22 1.383(6) . ? C21 C26 1.396(6) . ? C22 C23 1.371(7) . ? C23 C24 1.392(8) . ? C24 C25 1.359(8) . ? C25 C26 1.399(7) . ? C28 C29 1.504(8) . ? C29 C30 1.383(8) . ? C29 C34 1.391(8) . ? C30 C31 1.386(9) . ? C31 C32 1.361(8) . ? C32 C33 1.372(8) . ? C33 C34 1.390(8) . ? C34 C35 1.501(7) . ? C36 C37 1.382(7) . ? C36 C41 1.395(6) . ? C37 C38 1.377(8) . ? C38 C39 1.391(7) . ? C39 C40 1.360(7) . ? C40 C41 1.404(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 C3 88.58(19) . . ? C1 Re1 C2 90.9(2) . . ? C3 Re1 C2 87.77(19) . . ? C1 Re1 N8 91.98(18) . . ? C3 Re1 N8 179.04(17) . . ? C2 Re1 N8 93.00(17) . . ? C1 Re1 N1 94.81(17) . . ? C3 Re1 N1 98.31(16) . . ? C2 Re1 N1 171.72(18) . . ? N8 Re1 N1 80.86(14) . . ? C1 Re1 N2 172.49(17) . . ? C3 Re1 N2 92.34(16) . . ? C2 Re1 N2 96.55(17) . . ? N8 Re1 N2 87.01(14) . . ? N1 Re1 N2 77.68(13) . . ? C5 Re2 C6 88.9(2) . . ? C5 Re2 C4 88.9(2) . . ? C6 Re2 C4 86.8(2) . . ? C5 Re2 N5 95.60(18) . . ? C6 Re2 N5 91.55(17) . . ? C4 Re2 N5 175.24(19) . . ? C5 Re2 N4 171.50(17) . . ? C6 Re2 N4 99.11(17) . . ? C4 Re2 N4 94.27(19) . . ? N5 Re2 N4 81.56(13) . . ? C5 Re2 N3 94.31(18) . . ? C6 Re2 N3 173.41(17) . . ? C4 Re2 N3 98.94(17) . . ? N5 Re2 N3 82.43(13) . . ? N4 Re2 N3 77.41(13) . . ? C13 N1 C7 103.0(4) . . ? C13 N1 Re1 110.3(3) . . ? C7 N1 Re1 145.1(3) . . ? C14 N2 C15 102.2(4) . . ? C14 N2 Re1 110.3(3) . . ? C15 N2 Re1 147.3(3) . . ? C14 N3 C20 102.6(4) . . ? C14 N3 Re2 110.0(3) . . ? C20 N3 Re2 144.7(3) . . ? C13 N4 C12 102.5(4) . . ? C13 N4 Re2 110.7(3) . . ? C12 N4 Re2 144.7(3) . . ? C27 N5 C21 104.9(4) . . ? C27 N5 Re2 125.0(3) . . ? C21 N5 Re2 129.7(3) . . ? C27 N6 C26 106.9(4) . . ? C27 N6 C28 127.9(4) . . ? C26 N6 C28 124.2(4) . . ? C42 N7 C36 107.3(4) . . ? C42 N7 C35 124.5(4) . . ? C36 N7 C35 128.1(4) . . ? C42 N8 C41 105.8(4) . . ? C42 N8 Re1 123.6(3) . . ? C41 N8 Re1 130.0(3) . . ? O1 C1 Re1 178.6(5) . . ? O2 C2 Re1 178.2(5) . . ? O3 C3 Re1 177.9(4) . . ? O4 C4 Re2 176.6(5) . . ? O5 C5 Re2 178.0(5) . . ? O6 C6 Re2 178.3(5) . . ? N1 C7 C8 131.8(5) . . ? N1 C7 C12 107.6(4) . . ? C8 C7 C12 120.5(4) . . ? C9 C8 C7 117.8(5) . . ? C8 C9 C10 121.9(5) . . ? C11 C10 C9 121.6(5) . . ? C10 C11 C12 117.4(5) . . ? N4 C12 C11 130.6(5) . . ? N4 C12 C7 108.7(4) . . ? C11 C12 C7 120.7(4) . . ? N1 C13 N4 118.2(4) . . ? N1 C13 C14 121.2(4) . . ? N4 C13 C14 120.3(4) . . ? N3 C14 N2 118.7(4) . . ? N3 C14 C13 120.7(4) . . ? N2 C14 C13 120.4(4) . . ? N2 C15 C16 131.1(4) . . ? N2 C15 C20 108.6(4) . . ? C16 C15 C20 120.3(4) . . ? C17 C16 C15 117.6(5) . . ? C16 C17 C18 121.9(5) . . ? C19 C18 C17 121.3(5) . . ? C18 C19 C20 117.8(5) . . ? C19 C20 N3 130.9(4) . . ? C19 C20 C15 121.2(4) . . ? N3 C20 C15 107.9(4) . . ? C22 C21 C26 120.1(4) . . ? C22 C21 N5 131.2(4) . . ? C26 C21 N5 108.7(4) . . ? C23 C22 C21 117.7(5) . . ? C22 C23 C24 121.6(5) . . ? C25 C24 C23 122.1(5) . . ? C24 C25 C26 116.4(5) . . ? N6 C26 C21 106.2(4) . . ? N6 C26 C25 131.6(4) . . ? C21 C26 C25 122.1(5) . . ? N6 C27 N5 113.2(4) . . ? N6 C28 C29 114.5(4) . . ? C30 C29 C34 119.3(5) . . ? C30 C29 C28 118.6(5) . . ? C34 C29 C28 122.1(5) . . ? C29 C30 C31 120.5(6) . . ? C32 C31 C30 120.1(6) . . ? C33 C32 C31 120.0(6) . . ? C32 C33 C34 121.0(5) . . ? C29 C34 C33 119.1(5) . . ? C29 C34 C35 123.1(5) . . ? C33 C34 C35 117.8(5) . . ? N7 C35 C34 113.2(4) . . ? C37 C36 N7 132.2(4) . . ? C37 C36 C41 122.1(5) . . ? N7 C36 C41 105.7(4) . . ? C38 C37 C36 116.9(5) . . ? C37 C38 C39 121.4(5) . . ? C40 C39 C38 122.2(5) . . ? C39 C40 C41 117.4(5) . . ? N8 C41 C36 108.8(4) . . ? N8 C41 C40 131.2(4) . . ? C36 C41 C40 120.1(4) . . ? N8 C42 N7 112.4(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.164 _refine_diff_density_min -2.175 _refine_diff_density_rms 0.587 data_i6014 _database_code_depnum_ccdc_archive 'CCDC 632401' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H34 N4 O10 Re2' _chemical_formula_sum 'C53 H34 N4 O10 Re2' _chemical_formula_weight 1259.24 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3125(15) _cell_length_b 13.6261(18) _cell_length_c 15.5143(13) _cell_angle_alpha 73.052(9) _cell_angle_beta 91.069(8) _cell_angle_gamma 119.326(11) _cell_volume 2320.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 5.277 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.2267 _exptl_absorpt_correction_T_max 0.4184 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8543 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 24.97 _reflns_number_total 8153 _reflns_number_gt 4914 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0341P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8153 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0993 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.43406(3) 0.15869(3) 0.39876(2) 0.02680(10) Uani 1 1 d . . . Re2 Re -0.10475(3) 0.01205(3) 0.79696(2) 0.03266(12) Uani 1 1 d . . . C1 C 0.4797(8) 0.2187(10) 0.2712(7) 0.047(3) Uani 1 1 d . . . C2 C 0.5774(8) 0.1634(8) 0.4020(6) 0.035(2) Uani 1 1 d . . . C3 C 0.3622(8) 0.0009(8) 0.3913(6) 0.035(2) Uani 1 1 d . . . C4 C -0.1232(8) -0.0255(9) 0.9245(7) 0.043(2) Uani 1 1 d . . . C5 C -0.2297(9) 0.0416(10) 0.8041(7) 0.047(3) Uani 1 1 d . . . C6 C -0.2193(9) -0.1516(9) 0.8156(6) 0.042(2) Uani 1 1 d . . . C11 C 0.3028(7) 0.0803(7) 0.5923(6) 0.0246(19) Uani 1 1 d . . . C12 C 0.3064(7) 0.0365(7) 0.6897(6) 0.030(2) Uani 1 1 d . . . C13 C 0.3974(8) 0.0196(8) 0.7194(6) 0.037(2) Uani 1 1 d . . . H13 H 0.4569 0.0370 0.6767 0.044 Uiso 1 1 calc R . . C14 C 0.4014(9) -0.0220(10) 0.8098(7) 0.055(3) Uani 1 1 d . . . H14 H 0.4635 -0.0321 0.8284 0.066 Uiso 1 1 calc R . . C15 C 0.3131(10) -0.0492(11) 0.8736(7) 0.066(3) Uani 1 1 d . . . H15 H 0.3162 -0.0765 0.9354 0.079 Uiso 1 1 calc R . . C16 C 0.2202(8) -0.0359(8) 0.8459(6) 0.042(2) Uani 1 1 d . . . H16 H 0.1601 -0.0561 0.8893 0.050 Uiso 1 1 calc R . . C17 C 0.2153(7) 0.0076(7) 0.7531(6) 0.030(2) Uani 1 1 d . . . C18 C 0.1172(7) 0.0222(7) 0.7240(6) 0.0270(19) Uani 1 1 d . . . C19 C 0.1179(7) 0.0730(7) 0.6307(6) 0.0272(19) Uani 1 1 d . . . C20 C 0.0247(7) 0.0906(7) 0.6018(6) 0.0253(19) Uani 1 1 d . . . C21 C 0.0256(7) 0.1426(7) 0.5050(6) 0.0256(19) Uani 1 1 d . . . C22 C -0.0625(8) 0.1664(8) 0.4737(6) 0.035(2) Uani 1 1 d . . . H22 H -0.1227 0.1493 0.5155 0.042 Uiso 1 1 calc R . . C23 C -0.0608(8) 0.2143(8) 0.3828(6) 0.036(2) Uani 1 1 d . . . H23 H -0.1210 0.2272 0.3631 0.043 Uiso 1 1 calc R . . C24 C 0.0293(8) 0.2435(8) 0.3203(6) 0.036(2) Uani 1 1 d . . . H24 H 0.0310 0.2782 0.2586 0.044 Uiso 1 1 calc R . . C25 C 0.1170(8) 0.2214(8) 0.3489(6) 0.032(2) Uani 1 1 d . . . H25 H 0.1776 0.2413 0.3062 0.038 Uiso 1 1 calc R . . C26 C 0.1163(7) 0.1700(7) 0.4402(6) 0.0250(19) Uani 1 1 d . . . C27 C 0.2079(7) 0.1439(7) 0.4690(6) 0.0252(19) Uani 1 1 d . . . C28 C 0.2121(7) 0.1015(7) 0.5628(6) 0.0243(18) Uani 1 1 d . . . C31 C 0.5028(7) 0.4266(8) 0.3561(6) 0.034(2) Uani 1 1 d . . . H31 H 0.4545 0.4193 0.3114 0.041 Uiso 1 1 calc R . . C32 C 0.5843(7) 0.3829(8) 0.4707(6) 0.033(2) Uani 1 1 d . . . C33 C 0.6227(8) 0.3283(8) 0.5428(6) 0.042(2) Uani 1 1 d . . . H33 H 0.5955 0.2471 0.5608 0.050 Uiso 1 1 calc R . . C34 C 0.7032(9) 0.4004(9) 0.5865(6) 0.047(3) Uani 1 1 d . . . H34 H 0.7308 0.3671 0.6352 0.057 Uiso 1 1 calc R . . C35 C 0.7445(9) 0.5235(9) 0.5587(7) 0.055(3) Uani 1 1 d . . . H35 H 0.7977 0.5688 0.5907 0.066 Uiso 1 1 calc R . . C36 C 0.7097(8) 0.5786(8) 0.4872(7) 0.045(2) Uani 1 1 d . . . H36 H 0.7390 0.6602 0.4682 0.053 Uiso 1 1 calc R . . C37 C 0.6262(7) 0.5039(7) 0.4437(6) 0.031(2) Uani 1 1 d . . . C38 C 0.5991(9) 0.6494(8) 0.3158(6) 0.044(2) Uani 1 1 d . . . H38A H 0.6808 0.7054 0.3140 0.052 Uiso 1 1 calc R . . H38B H 0.5538 0.6707 0.3468 0.052 Uiso 1 1 calc R . . C39 C 0.5727(8) 0.6634(8) 0.2181(7) 0.040(2) Uani 1 1 d . . . C40 C 0.5019(10) 0.7090(10) 0.1916(9) 0.070(4) Uani 1 1 d . . . H40 H 0.4691 0.7260 0.2336 0.083 Uiso 1 1 calc R . . C41 C 0.4781(14) 0.7304(15) 0.1033(11) 0.105(6) Uani 1 1 d . . . H41 H 0.4280 0.7597 0.0868 0.126 Uiso 1 1 calc R . . C42 C 0.5259(14) 0.7096(16) 0.0416(10) 0.110(6) Uani 1 1 d . . . H42 H 0.5110 0.7260 -0.0181 0.132 Uiso 1 1 calc R . . C43 C 0.5983(10) 0.6631(11) 0.0670(7) 0.065(3) Uani 1 1 d . . . H43 H 0.6319 0.6487 0.0236 0.078 Uiso 1 1 calc R . . C44 C 0.6217(8) 0.6375(8) 0.1562(7) 0.041(2) Uani 1 1 d . . . C45 C 0.6990(8) 0.5845(9) 0.1763(7) 0.045(3) Uani 1 1 d . . . H45A H 0.6536 0.5040 0.2181 0.054 Uiso 1 1 calc R . . H45B H 0.7245 0.5799 0.1201 0.054 Uiso 1 1 calc R . . C51 C 0.8720(8) 0.7697(8) 0.1875(6) 0.038(2) Uani 1 1 d . . . H51 H 0.8555 0.8221 0.1451 0.046 Uiso 1 1 calc R . . C52 C 0.9599(8) 0.6993(8) 0.2834(6) 0.038(2) Uani 1 1 d . . . C53 C 1.0352(9) 0.6819(10) 0.3393(7) 0.052(3) Uani 1 1 d . . . H53 H 1.1039 0.7456 0.3452 0.063 Uiso 1 1 calc R . . C54 C 1.0049(10) 0.5680(10) 0.3853(8) 0.063(3) Uani 1 1 d . . . H54 H 1.0548 0.5536 0.4228 0.075 Uiso 1 1 calc R . . C55 C 0.9003(11) 0.4705(11) 0.3781(8) 0.065(3) Uani 1 1 d . . . H55 H 0.8827 0.3938 0.4116 0.078 Uiso 1 1 calc R . . C56 C 0.8237(9) 0.4855(9) 0.3232(7) 0.051(3) Uani 1 1 d . . . H56 H 0.7549 0.4217 0.3175 0.061 Uiso 1 1 calc R . . C57 C 0.8562(8) 0.6024(8) 0.2769(6) 0.035(2) Uani 1 1 d . . . C61 C 0.9784(17) 0.5841(17) 0.0929(13) 0.130(6) Uiso 1 1 d . . . H61 H 1.0270 0.5806 0.1361 0.156 Uiso 1 1 calc R . . C62 C 0.8894(15) 0.4878(15) 0.0799(11) 0.098(5) Uiso 1 1 d . . . C63 C 0.8102(17) 0.4744(18) 0.0196(13) 0.133(7) Uiso 1 1 d . . . H63 H 0.7491 0.4021 0.0177 0.159 Uiso 1 1 calc R . . C64 C 0.8360(16) 0.5876(17) -0.0392(12) 0.124(6) Uiso 1 1 d . . . H64 H 0.7930 0.5918 -0.0867 0.149 Uiso 1 1 calc R . . C65 C 0.9182(17) 0.6865(18) -0.0291(13) 0.133(7) Uiso 1 1 d . . . H65 H 0.9270 0.7575 -0.0679 0.159 Uiso 1 1 calc R . . C66 C 0.9912(15) 0.6935(16) 0.0333(12) 0.118(6) Uiso 1 1 d . . . H66 H 1.0479 0.7666 0.0375 0.142 Uiso 1 1 calc R . . C67 C 0.862(2) 0.373(2) 0.1445(18) 0.256(14) Uiso 1 1 d . . . H67A H 0.7974 0.3105 0.1288 0.384 Uiso 1 1 calc R . . H67B H 0.8425 0.3697 0.2049 0.384 Uiso 1 1 calc R . . H67C H 0.9287 0.3634 0.1422 0.384 Uiso 1 1 calc R . . N1 N 0.5072(6) 0.3359(6) 0.4124(5) 0.0291(16) Uani 1 1 d . . . N2 N 0.5746(6) 0.5307(6) 0.3694(5) 0.0333(17) Uani 1 1 d . . . N3 N 0.9656(6) 0.8027(7) 0.2266(5) 0.0370(18) Uani 1 1 d . . . N4 N 0.8026(6) 0.6516(6) 0.2159(5) 0.0365(18) Uani 1 1 d . . . O1 O 0.5143(7) 0.2599(8) 0.1938(5) 0.070(2) Uani 1 1 d . . . O2 O 0.6676(5) 0.1687(6) 0.4042(5) 0.0525(19) Uani 1 1 d . . . O3 O 0.3214(6) -0.0925(6) 0.3857(5) 0.0517(19) Uani 1 1 d . . . O4 O -0.1366(7) -0.0500(7) 1.0031(5) 0.066(2) Uani 1 1 d . . . O5 O -0.3030(7) 0.0602(9) 0.8153(6) 0.086(3) Uani 1 1 d . . . O6 O -0.2875(7) -0.2491(6) 0.8319(5) 0.063(2) Uani 1 1 d . . . O7 O 0.3902(5) 0.1017(5) 0.5406(4) 0.0310(14) Uani 1 1 d . . . O8 O 0.2809(5) 0.1667(5) 0.4029(4) 0.0283(13) Uani 1 1 d . . . O9 O -0.0641(5) 0.0676(5) 0.6533(4) 0.0320(14) Uani 1 1 d . . . O10 O 0.0386(5) -0.0098(5) 0.7901(4) 0.0330(15) 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 0.0236(2) 0.0304(2) 0.0274(2) -0.01109(17) 0.00043(16) 0.01324(17) Re2 0.0260(2) 0.0413(3) 0.0273(2) -0.00885(19) 0.00295(17) 0.0156(2) C1 0.037(6) 0.064(7) 0.041(6) -0.021(5) -0.003(5) 0.023(6) C2 0.032(5) 0.028(5) 0.036(5) -0.014(4) 0.000(4) 0.007(4) C3 0.030(5) 0.044(6) 0.036(5) -0.015(5) 0.001(4) 0.021(5) C4 0.036(6) 0.049(6) 0.045(6) -0.015(5) 0.004(5) 0.023(5) C5 0.040(6) 0.070(8) 0.033(6) -0.014(5) -0.001(5) 0.032(6) C6 0.048(6) 0.045(6) 0.027(5) -0.009(5) -0.002(5) 0.021(5) C11 0.024(4) 0.019(4) 0.036(5) -0.011(4) -0.002(4) 0.014(4) C12 0.029(5) 0.032(5) 0.021(5) -0.006(4) -0.002(4) 0.011(4) C13 0.030(5) 0.048(6) 0.029(5) -0.008(4) 0.002(4) 0.019(5) C14 0.052(7) 0.093(9) 0.038(6) -0.007(6) -0.005(5) 0.057(7) C15 0.063(8) 0.097(10) 0.038(7) -0.004(6) -0.007(6) 0.052(8) C16 0.040(6) 0.057(7) 0.023(5) -0.008(5) 0.003(4) 0.023(5) C17 0.027(5) 0.031(5) 0.038(5) -0.013(4) -0.005(4) 0.017(4) C18 0.027(5) 0.032(5) 0.025(5) -0.011(4) -0.004(4) 0.017(4) C19 0.022(4) 0.032(5) 0.025(5) -0.009(4) 0.003(4) 0.012(4) C20 0.025(5) 0.022(4) 0.034(5) -0.017(4) -0.005(4) 0.011(4) C21 0.028(5) 0.026(5) 0.030(5) -0.014(4) -0.007(4) 0.016(4) C22 0.036(5) 0.040(5) 0.038(6) -0.011(4) -0.005(4) 0.025(5) C23 0.038(5) 0.042(6) 0.035(6) -0.008(4) -0.010(4) 0.028(5) C24 0.047(6) 0.044(6) 0.028(5) -0.013(4) -0.011(4) 0.029(5) C25 0.037(5) 0.040(5) 0.031(5) -0.014(4) -0.004(4) 0.027(5) C26 0.021(4) 0.018(4) 0.035(5) -0.010(4) -0.005(4) 0.009(4) C27 0.021(4) 0.015(4) 0.031(5) -0.010(4) 0.001(4) 0.002(4) C28 0.026(5) 0.018(4) 0.028(5) -0.007(4) -0.004(4) 0.011(4) C31 0.033(5) 0.043(6) 0.029(5) -0.012(4) -0.005(4) 0.021(5) C32 0.032(5) 0.038(5) 0.033(5) -0.021(4) -0.003(4) 0.015(4) C33 0.049(6) 0.040(6) 0.045(6) -0.021(5) -0.014(5) 0.025(5) C34 0.063(7) 0.053(7) 0.034(6) -0.014(5) -0.023(5) 0.035(6) C35 0.059(7) 0.051(7) 0.058(7) -0.031(6) -0.029(6) 0.022(6) C36 0.053(6) 0.032(5) 0.050(6) -0.020(5) -0.010(5) 0.019(5) C37 0.037(5) 0.022(5) 0.035(5) -0.009(4) -0.005(4) 0.016(4) C38 0.053(6) 0.035(6) 0.047(6) -0.014(5) -0.008(5) 0.026(5) C39 0.034(5) 0.033(5) 0.047(6) -0.005(5) -0.009(5) 0.016(5) C40 0.064(8) 0.064(8) 0.068(9) 0.000(7) -0.002(7) 0.035(7) C41 0.095(12) 0.125(14) 0.090(12) 0.000(11) -0.036(10) 0.072(11) C42 0.092(12) 0.146(16) 0.042(9) 0.011(9) -0.029(8) 0.048(11) C43 0.054(7) 0.075(8) 0.036(6) -0.016(6) -0.007(6) 0.013(7) C44 0.029(5) 0.044(6) 0.043(6) -0.012(5) -0.004(4) 0.014(5) C45 0.042(6) 0.050(6) 0.046(6) -0.024(5) 0.000(5) 0.021(5) C51 0.035(5) 0.043(6) 0.035(5) -0.008(5) -0.005(4) 0.021(5) C52 0.032(5) 0.040(6) 0.039(6) -0.011(5) 0.006(4) 0.016(5) C53 0.052(7) 0.059(7) 0.049(7) -0.009(6) -0.013(5) 0.035(6) C54 0.066(8) 0.061(8) 0.067(8) -0.010(7) -0.016(7) 0.042(7) C55 0.074(9) 0.060(8) 0.055(8) -0.001(6) 0.014(7) 0.038(7) C56 0.055(7) 0.037(6) 0.057(7) -0.013(5) 0.002(6) 0.022(5) C57 0.044(6) 0.036(5) 0.030(5) -0.007(4) -0.003(4) 0.025(5) N1 0.028(4) 0.027(4) 0.031(4) -0.010(3) -0.003(3) 0.012(3) N2 0.038(4) 0.035(4) 0.028(4) -0.013(3) -0.004(3) 0.019(4) N3 0.038(5) 0.040(5) 0.032(4) -0.010(4) -0.003(4) 0.020(4) N4 0.026(4) 0.034(4) 0.038(4) -0.009(4) 0.006(3) 0.008(4) O1 0.067(5) 0.107(7) 0.026(4) -0.009(4) 0.009(4) 0.042(5) O2 0.030(4) 0.062(5) 0.075(5) -0.029(4) -0.003(4) 0.027(4) O3 0.055(5) 0.046(4) 0.067(5) -0.035(4) -0.013(4) 0.025(4) O4 0.077(6) 0.091(6) 0.027(4) -0.006(4) 0.009(4) 0.046(5) O5 0.065(6) 0.135(9) 0.088(7) -0.034(6) -0.003(5) 0.073(6) O6 0.064(5) 0.045(5) 0.059(5) -0.013(4) 0.010(4) 0.013(4) O7 0.027(3) 0.037(4) 0.031(3) -0.009(3) -0.005(3) 0.019(3) O8 0.028(3) 0.036(3) 0.021(3) -0.006(3) 0.003(3) 0.017(3) O9 0.024(3) 0.042(4) 0.026(3) -0.009(3) 0.001(3) 0.016(3) O10 0.028(3) 0.043(4) 0.024(3) -0.001(3) 0.007(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C2 1.878(9) . ? Re1 C1 1.890(10) . ? Re1 C3 1.918(10) . ? Re1 O7 2.096(6) . ? Re1 O8 2.097(5) . ? Re1 N1 2.194(7) . ? Re2 C4 1.882(10) . ? Re2 C5 1.905(10) . ? Re2 C6 1.922(11) . ? Re2 O10 2.079(5) . ? Re2 O9 2.120(5) . ? Re2 N3 2.201(7) 2_666 ? C1 O1 1.158(11) . ? C2 O2 1.167(10) . ? C3 O3 1.144(10) . ? C4 O4 1.158(11) . ? C5 O5 1.149(11) . ? C6 O6 1.133(11) . ? C11 O7 1.283(9) . ? C11 C28 1.413(11) . ? C11 C12 1.463(11) . ? C12 C13 1.387(11) . ? C12 C17 1.395(11) . ? C13 C14 1.361(12) . ? C13 H13 0.9300 . ? C14 C15 1.380(13) . ? C14 H14 0.9300 . ? C15 C16 1.379(13) . ? C15 H15 0.9300 . ? C16 C17 1.401(12) . ? C16 H16 0.9300 . ? C17 C18 1.460(11) . ? C18 O10 1.293(9) . ? C18 C19 1.408(11) . ? C19 C20 1.416(11) . ? C19 C28 1.472(10) . ? C20 O9 1.288(9) . ? C20 C21 1.460(11) . ? C21 C22 1.406(11) . ? C21 C26 1.411(11) . ? C22 C23 1.366(12) . ? C22 H22 0.9300 . ? C23 C24 1.374(12) . ? C23 H23 0.9300 . ? C24 C25 1.378(11) . ? C24 H24 0.9300 . ? C25 C26 1.383(11) . ? C25 H25 0.9300 . ? C26 C27 1.458(11) . ? C27 O8 1.285(9) . ? C27 C28 1.412(11) . ? C31 N1 1.316(10) . ? C31 N2 1.342(10) . ? C31 H31 0.9300 . ? C32 C37 1.382(11) . ? C32 C33 1.390(12) . ? C32 N1 1.394(10) . ? C33 C34 1.379(12) . ? C33 H33 0.9300 . ? C34 C35 1.409(13) . ? C34 H34 0.9300 . ? C35 C36 1.358(13) . ? C35 H35 0.9300 . ? C36 C37 1.412(12) . ? C36 H36 0.9300 . ? C37 N2 1.380(10) . ? C38 N2 1.457(11) . ? C38 C39 1.529(13) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.362(14) . ? C39 C44 1.384(13) . ? C40 C41 1.380(18) . ? C40 H40 0.9300 . ? C41 C42 1.32(2) . ? C41 H41 0.9300 . ? C42 C43 1.388(18) . ? C42 H42 0.9300 . ? C43 C44 1.394(13) . ? C43 H43 0.9300 . ? C44 C45 1.504(12) . ? C45 N4 1.476(11) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C51 N3 1.305(11) . ? C51 N4 1.334(11) . ? C51 H51 0.9300 . ? C52 C53 1.377(13) . ? C52 N3 1.394(11) . ? C52 C57 1.395(12) . ? C53 C54 1.354(14) . ? C53 H53 0.9300 . ? C54 C55 1.409(15) . ? C54 H54 0.9300 . ? C55 C56 1.369(15) . ? C55 H55 0.9300 . ? C56 C57 1.381(12) . ? C56 H56 0.9300 . ? C57 N4 1.388(11) . ? C61 C62 1.34(2) . ? C61 C66 1.44(2) . ? C61 H61 0.9300 . ? C62 C63 1.38(2) . ? C62 C67 1.46(3) . ? C63 C64 1.41(2) . ? C63 H63 0.9300 . ? C64 C65 1.31(2) . ? C64 H64 0.9300 . ? C65 C66 1.35(2) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? N3 Re2 2.201(7) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C1 84.0(4) . . ? C2 Re1 C3 89.3(4) . . ? C1 Re1 C3 88.6(4) . . ? C2 Re1 O7 95.2(3) . . ? C1 Re1 O7 176.8(4) . . ? C3 Re1 O7 94.6(3) . . ? C2 Re1 O8 173.8(3) . . ? C1 Re1 O8 98.9(3) . . ? C3 Re1 O8 96.2(3) . . ? O7 Re1 O8 81.6(2) . . ? C2 Re1 N1 93.3(3) . . ? C1 Re1 N1 93.7(4) . . ? C3 Re1 N1 176.7(3) . . ? O7 Re1 N1 83.2(2) . . ? O8 Re1 N1 81.1(2) . . ? C4 Re2 C5 84.7(4) . . ? C4 Re2 C6 87.4(4) . . ? C5 Re2 C6 88.0(4) . . ? C4 Re2 O10 94.6(3) . . ? C5 Re2 O10 176.4(4) . . ? C6 Re2 O10 95.5(3) . . ? C4 Re2 O9 173.6(3) . . ? C5 Re2 O9 99.1(3) . . ? C6 Re2 O9 97.9(3) . . ? O10 Re2 O9 81.3(2) . . ? C4 Re2 N3 93.6(4) . 2_666 ? C5 Re2 N3 95.4(4) . 2_666 ? C6 Re2 N3 176.6(3) . 2_666 ? O10 Re2 N3 81.2(3) . 2_666 ? O9 Re2 N3 81.0(2) . 2_666 ? O1 C1 Re1 175.9(10) . . ? O2 C2 Re1 178.5(8) . . ? O3 C3 Re1 178.6(8) . . ? O4 C4 Re2 178.8(10) . . ? O5 C5 Re2 174.4(9) . . ? O6 C6 Re2 176.0(8) . . ? O7 C11 C28 125.8(8) . . ? O7 C11 C12 114.0(7) . . ? C28 C11 C12 120.2(7) . . ? C13 C12 C17 119.7(8) . . ? C13 C12 C11 120.7(7) . . ? C17 C12 C11 119.6(8) . . ? C14 C13 C12 121.3(8) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 119.8(9) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.1(10) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.7(9) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C12 C17 C16 118.4(8) . . ? C12 C17 C18 121.0(8) . . ? C16 C17 C18 120.6(8) . . ? O10 C18 C19 126.3(7) . . ? O10 C18 C17 114.2(7) . . ? C19 C18 C17 119.5(7) . . ? C18 C19 C20 120.0(7) . . ? C18 C19 C28 119.9(7) . . ? C20 C19 C28 120.0(7) . . ? O9 C20 C19 126.6(8) . . ? O9 C20 C21 113.7(7) . . ? C19 C20 C21 119.7(7) . . ? C22 C21 C26 118.4(8) . . ? C22 C21 C20 121.5(7) . . ? C26 C21 C20 120.0(7) . . ? C23 C22 C21 120.8(8) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.5(8) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C25 120.0(8) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 121.0(8) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C25 C26 C21 119.2(7) . . ? C25 C26 C27 120.3(7) . . ? C21 C26 C27 120.5(7) . . ? O8 C27 C28 126.3(8) . . ? O8 C27 C26 114.0(7) . . ? C28 C27 C26 119.7(7) . . ? C27 C28 C11 120.6(7) . . ? C27 C28 C19 119.8(7) . . ? C11 C28 C19 119.5(7) . . ? N1 C31 N2 113.6(8) . . ? N1 C31 H31 123.2 . . ? N2 C31 H31 123.2 . . ? C37 C32 C33 121.4(8) . . ? C37 C32 N1 108.1(8) . . ? C33 C32 N1 130.5(8) . . ? C34 C33 C32 116.7(9) . . ? C34 C33 H33 121.6 . . ? C32 C33 H33 121.6 . . ? C33 C34 C35 121.3(9) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C36 C35 C34 122.6(9) . . ? C36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? C35 C36 C37 115.7(9) . . ? C35 C36 H36 122.2 . . ? C37 C36 H36 122.2 . . ? N2 C37 C32 107.3(7) . . ? N2 C37 C36 130.5(8) . . ? C32 C37 C36 122.2(8) . . ? N2 C38 C39 115.0(7) . . ? N2 C38 H38A 108.5 . . ? C39 C38 H38A 108.5 . . ? N2 C38 H38B 108.5 . . ? C39 C38 H38B 108.5 . . ? H38A C38 H38B 107.5 . . ? C40 C39 C44 120.1(10) . . ? C40 C39 C38 116.8(10) . . ? C44 C39 C38 123.1(8) . . ? C39 C40 C41 120.8(13) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 120.7(14) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C41 C42 C43 119.5(13) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C42 C43 C44 121.2(12) . . ? C42 C43 H43 119.4 . . ? C44 C43 H43 119.4 . . ? C39 C44 C43 117.6(10) . . ? C39 C44 C45 125.8(9) . . ? C43 C44 C45 116.5(10) . . ? N4 C45 C44 114.3(8) . . ? N4 C45 H45A 108.7 . . ? C44 C45 H45A 108.7 . . ? N4 C45 H45B 108.7 . . ? C44 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? N3 C51 N4 111.8(8) . . ? N3 C51 H51 124.1 . . ? N4 C51 H51 124.1 . . ? C53 C52 N3 131.6(9) . . ? C53 C52 C57 120.4(9) . . ? N3 C52 C57 108.0(8) . . ? C54 C53 C52 117.1(11) . . ? C54 C53 H53 121.4 . . ? C52 C53 H53 121.4 . . ? C53 C54 C55 122.1(11) . . ? C53 C54 H54 119.0 . . ? C55 C54 H54 119.0 . . ? C56 C55 C54 121.9(11) . . ? C56 C55 H55 119.1 . . ? C54 C55 H55 119.1 . . ? C55 C56 C57 115.1(10) . . ? C55 C56 H56 122.4 . . ? C57 C56 H56 122.4 . . ? C56 C57 N4 131.6(9) . . ? C56 C57 C52 123.4(9) . . ? N4 C57 C52 105.1(8) . . ? C62 C61 C66 113.0(18) . . ? C62 C61 H61 123.5 . . ? C66 C61 H61 123.5 . . ? C61 C62 C63 132.3(19) . . ? C61 C62 C67 116(2) . . ? C63 C62 C67 111.1(19) . . ? C62 C63 C64 109.6(18) . . ? C62 C63 H63 125.2 . . ? C64 C63 H63 125.2 . . ? C65 C64 C63 122(2) . . ? C65 C64 H64 118.9 . . ? C63 C64 H64 118.9 . . ? C64 C65 C66 125(2) . . ? C64 C65 H65 117.5 . . ? C66 C65 H65 117.5 . . ? C65 C66 C61 117.6(19) . . ? C65 C66 H66 121.2 . . ? C61 C66 H66 121.2 . . ? C62 C67 H67A 109.5 . . ? C62 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C62 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C31 N1 C32 105.2(7) . . ? C31 N1 Re1 126.1(6) . . ? C32 N1 Re1 127.8(6) . . ? C31 N2 C37 105.7(7) . . ? C31 N2 C38 128.5(8) . . ? C37 N2 C38 125.7(7) . . ? C51 N3 C52 106.9(8) . . ? C51 N3 Re2 125.3(6) . 2_666 ? C52 N3 Re2 127.8(6) . 2_666 ? C51 N4 C57 108.2(8) . . ? C51 N4 C45 125.5(8) . . ? C57 N4 C45 125.4(8) . . ? C11 O7 Re1 133.0(5) . . ? C27 O8 Re1 132.6(5) . . ? C20 O9 Re2 131.6(5) . . ? C18 O10 Re2 133.1(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.127 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.160