# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Elon Ison' _publ_contact_author_email eaison@ncsu.edu loop_ _publ_author_name E.Ison C.Lilly P.Boyle data_x1 _database_code_depnum_ccdc_archive 'CCDC 831035' #TrackingRef '- CIF[1].txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H47 N3 O2 P Re' _chemical_formula_weight 867.02 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5052(2) _cell_length_b 14.6432(4) _cell_length_c 16.3909(4) _cell_angle_alpha 111.4709(14) _cell_angle_beta 94.3130(14) _cell_angle_gamma 90.4943(13) _cell_volume 1892.89(8) _cell_formula_units_Z 2 _cell_measurement_temperature 110 _cell_measurement_reflns_used 9799 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 36.68 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 3.293 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4284 _exptl_absorpt_correction_T_max 0.8022 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Kappa Axis X8 Apex2' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 77022 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 39.40 _reflns_number_total 20705 _reflns_number_gt 17519 _reflns_threshold_expression >2sigma(I) _computing_data_collection Apex2 _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution XS _computing_structure_refinement XL _computing_molecular_graphics NRCVAX _computing_publication_material cif2tables.py _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^)+(0.0333P)^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 20705 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.015 _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 0.404534(7) 0.330420(4) 1.101130(4) 0.01469(2) Uani 1 1 d . . . O1 O 0.60268(14) 0.32778(10) 1.11940(8) 0.0216(2) Uani 1 1 d . . . C1 C 0.3127(2) 0.22106(13) 1.14343(12) 0.0204(3) Uani 1 1 d . . . H1A H 0.3338 0.1558 1.1013 0.031 Uiso 1 1 calc R . . H1B H 0.1986 0.2276 1.1469 0.031 Uiso 1 1 calc R . . H1C H 0.3635 0.2294 1.2015 0.031 Uiso 1 1 calc R . . N1 N 0.31336(16) 0.43088(10) 1.20146(9) 0.0164(2) Uani 1 1 d . . . N2 N 0.31824(16) 0.43098(10) 1.04943(9) 0.0166(2) Uani 1 1 d . . . N3 N 0.32980(17) 0.24889(10) 0.97889(9) 0.0176(2) Uani 1 1 d . . . C2 C 0.26483(18) 0.42268(11) 1.28013(10) 0.0157(3) Uani 1 1 d . . . C3 C 0.10443(19) 0.41416(12) 1.29205(11) 0.0186(3) Uani 1 1 d . . . C4 C 0.0619(2) 0.39983(13) 1.36714(11) 0.0209(3) Uani 1 1 d . . . H4 H -0.0467 0.3923 1.3742 0.025 Uiso 1 1 calc R . . C5 C 0.1744(2) 0.39620(13) 1.43216(11) 0.0201(3) Uani 1 1 d . . . C6 C 0.3322(2) 0.40897(12) 1.42063(11) 0.0196(3) Uani 1 1 d . . . H6 H 0.4102 0.4090 1.4653 0.024 Uiso 1 1 calc R . . C7 C 0.38025(18) 0.42174(12) 1.34611(11) 0.0171(3) Uani 1 1 d . . . C8 C -0.0213(2) 0.41765(15) 1.22346(13) 0.0259(4) Uani 1 1 d . . . H8A H -0.1191 0.3857 1.2296 0.039 Uiso 1 1 calc R . . H8B H 0.0137 0.3833 1.1647 0.039 Uiso 1 1 calc R . . H8C H -0.0403 0.4862 1.2315 0.039 Uiso 1 1 calc R . . C9 C 0.1289(2) 0.37659(15) 1.51153(12) 0.0268(4) Uani 1 1 d . . . H9A H 0.1330 0.3061 1.4998 0.040 Uiso 1 1 calc R . . H9B H 0.0217 0.3982 1.5240 0.040 Uiso 1 1 calc R . . H9C H 0.2026 0.4127 1.5624 0.040 Uiso 1 1 calc R . . C10 C 0.5528(2) 0.43286(15) 1.33506(12) 0.0241(3) Uani 1 1 d . . . H10A H 0.6146 0.4445 1.3911 0.036 Uiso 1 1 calc R . . H10B H 0.5695 0.4886 1.3167 0.036 Uiso 1 1 calc R . . H10C H 0.5865 0.3727 1.2902 0.036 Uiso 1 1 calc R . . C11 C 0.2977(2) 0.52991(12) 1.19906(11) 0.0191(3) Uani 1 1 d . . . H11A H 0.3903 0.5724 1.2320 0.023 Uiso 1 1 calc R . . H11B H 0.2017 0.5596 1.2268 0.023 Uiso 1 1 calc R . . C12 C 0.28695(19) 0.52166(12) 1.10490(11) 0.0178(3) Uani 1 1 d . . . C13 C 0.2434(2) 0.59352(13) 1.07213(12) 0.0215(3) Uani 1 1 d . . . H13 H 0.2232 0.6580 1.1106 0.026 Uiso 1 1 calc R . . C14 C 0.2300(2) 0.56850(14) 0.98142(12) 0.0238(3) Uani 1 1 d . . . H14 H 0.2020 0.6169 0.9576 0.029 Uiso 1 1 calc R . . C15 C 0.2569(2) 0.47395(14) 0.92539(12) 0.0235(3) Uani 1 1 d . . . H15 H 0.2465 0.4570 0.8634 0.028 Uiso 1 1 calc R . . C16 C 0.2991(2) 0.40458(12) 0.96102(11) 0.0187(3) Uani 1 1 d . . . C17 C 0.3202(2) 0.29687(13) 0.91398(11) 0.0217(3) Uani 1 1 d . . . H17A H 0.2299 0.2680 0.8697 0.026 Uiso 1 1 calc R . . H17B H 0.4179 0.2867 0.8831 0.026 Uiso 1 1 calc R . . C18 C 0.28468(18) 0.14672(12) 0.94109(10) 0.0165(3) Uani 1 1 d . . . C19 C 0.40018(19) 0.07669(12) 0.91514(11) 0.0194(3) Uani 1 1 d . . . C20 C 0.3538(2) -0.02249(13) 0.87900(12) 0.0229(3) Uani 1 1 d . . . H20 H 0.4321 -0.0699 0.8601 0.027 Uiso 1 1 calc R . . C21 C 0.1961(2) -0.05434(13) 0.86966(12) 0.0222(3) Uani 1 1 d . . . C22 C 0.0839(2) 0.01680(13) 0.89671(11) 0.0211(3) Uani 1 1 d . . . H22 H -0.0240 -0.0035 0.8916 0.025 Uiso 1 1 calc R . . C23 C 0.12479(19) 0.11690(13) 0.93105(11) 0.0194(3) Uani 1 1 d . . . C24 C 0.5722(2) 0.10792(15) 0.92558(14) 0.0274(4) Uani 1 1 d . . . H24A H 0.6362 0.0496 0.9073 0.041 Uiso 1 1 calc R . . H24B H 0.6027 0.1481 0.9873 0.041 Uiso 1 1 calc R . . H24C H 0.5896 0.1463 0.8889 0.041 Uiso 1 1 calc R . . C25 C 0.1501(3) -0.16220(14) 0.83226(14) 0.0311(4) Uani 1 1 d . . . H25A H 0.0867 -0.1782 0.8731 0.047 Uiso 1 1 calc R . . H25B H 0.2454 -0.2006 0.8238 0.047 Uiso 1 1 calc R . . H25C H 0.0883 -0.1780 0.7756 0.047 Uiso 1 1 calc R . . C26 C -0.0003(2) 0.19203(15) 0.95714(14) 0.0294(4) Uani 1 1 d . . . H26A H -0.0164 0.2219 0.9127 0.044 Uiso 1 1 calc R . . H26B H 0.0335 0.2430 1.0142 0.044 Uiso 1 1 calc R . . H26C H -0.0993 0.1600 0.9615 0.044 Uiso 1 1 calc R . . P1 P -0.11537(5) 0.17263(3) 0.66366(3) 0.01579(7) Uani 1 1 d . . . O2 O -0.17582(15) 0.24820(9) 0.74240(8) 0.0221(2) Uani 1 1 d . . . C27 C 0.09741(18) 0.17145(12) 0.67220(10) 0.0175(3) Uani 1 1 d . . . C28 C 0.1771(2) 0.25418(14) 0.66968(12) 0.0235(3) Uani 1 1 d . . . H28 H 0.1191 0.3051 0.6602 0.028 Uiso 1 1 calc R . . C29 C 0.3411(2) 0.26218(17) 0.68102(13) 0.0289(4) Uani 1 1 d . . . H29 H 0.3948 0.3184 0.6790 0.035 Uiso 1 1 calc R . . C30 C 0.4266(2) 0.18801(17) 0.69529(12) 0.0296(4) Uani 1 1 d . . . H30 H 0.5385 0.1936 0.7030 0.035 Uiso 1 1 calc R . . C31 C 0.3487(2) 0.10626(16) 0.69819(13) 0.0288(4) Uani 1 1 d . . . H31 H 0.4073 0.0556 0.7078 0.035 Uiso 1 1 calc R . . C32 C 0.1839(2) 0.09784(14) 0.68699(12) 0.0231(3) Uani 1 1 d . . . H32 H 0.1308 0.0417 0.6895 0.028 Uiso 1 1 calc R . . C33 C -0.16602(18) 0.19714(12) 0.56481(11) 0.0177(3) Uani 1 1 d . . . C34 C -0.2642(2) 0.27475(14) 0.57184(13) 0.0262(4) Uani 1 1 d . . . H34 H -0.3025 0.3117 0.6269 0.031 Uiso 1 1 calc R . . C35 C -0.3063(3) 0.29827(17) 0.49835(15) 0.0359(5) Uani 1 1 d . . . H35 H -0.3715 0.3521 0.5036 0.043 Uiso 1 1 calc R . . C36 C -0.2531(2) 0.24319(16) 0.41760(14) 0.0316(4) Uani 1 1 d . . . H36 H -0.2854 0.2576 0.3670 0.038 Uiso 1 1 calc R . . C37 C -0.1527(3) 0.16690(15) 0.41059(13) 0.0281(4) Uani 1 1 d . . . H37 H -0.1144 0.1300 0.3555 0.034 Uiso 1 1 calc R . . C38 C -0.1083(2) 0.14467(13) 0.48440(12) 0.0241(3) Uani 1 1 d . . . H38 H -0.0380 0.0933 0.4798 0.029 Uiso 1 1 calc R . . C39 C -0.19433(19) 0.05093(12) 0.64541(11) 0.0184(3) Uani 1 1 d . . . C40 C -0.1821(2) 0.01917(14) 0.71532(13) 0.0249(3) Uani 1 1 d . . . H40 H -0.1286 0.0606 0.7695 0.030 Uiso 1 1 calc R . . C41 C -0.2446(3) -0.07024(15) 0.70914(14) 0.0308(4) Uani 1 1 d . . . H41 H -0.2319 -0.0907 0.7579 0.037 Uiso 1 1 calc R . . C42 C -0.3258(3) -0.12989(15) 0.63160(14) 0.0305(4) Uani 1 1 d . . . H42 H -0.3691 -0.1920 0.6265 0.037 Uiso 1 1 calc R . . C43 C -0.3444(2) -0.09889(15) 0.56071(13) 0.0302(4) Uani 1 1 d . . . H43 H -0.4023 -0.1394 0.5077 0.036 Uiso 1 1 calc R . . C44 C -0.2784(2) -0.00901(13) 0.56709(12) 0.0233(3) Uani 1 1 d . . . H44 H -0.2905 0.0116 0.5184 0.028 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 0.01570(3) 0.01395(3) 0.01489(3) 0.00631(2) -0.00095(2) 0.00041(2) O1 0.0180(5) 0.0249(6) 0.0241(6) 0.0118(5) -0.0001(4) 0.0006(4) C1 0.0222(7) 0.0175(7) 0.0221(8) 0.0084(6) 0.0010(6) 0.0003(6) N1 0.0206(6) 0.0141(6) 0.0153(6) 0.0068(5) -0.0015(5) 0.0004(5) N2 0.0198(6) 0.0156(6) 0.0150(6) 0.0065(5) 0.0006(4) 0.0004(5) N3 0.0219(6) 0.0149(6) 0.0154(6) 0.0055(5) -0.0008(5) 0.0011(5) C2 0.0188(6) 0.0128(6) 0.0150(6) 0.0049(5) -0.0017(5) 0.0002(5) C3 0.0189(7) 0.0167(7) 0.0183(7) 0.0050(6) -0.0022(5) 0.0006(5) C4 0.0188(7) 0.0216(8) 0.0213(8) 0.0068(6) 0.0019(6) -0.0006(6) C5 0.0250(8) 0.0180(7) 0.0178(7) 0.0070(6) 0.0021(6) 0.0005(6) C6 0.0229(7) 0.0195(7) 0.0164(7) 0.0074(6) -0.0029(5) 0.0001(6) C7 0.0177(6) 0.0164(7) 0.0172(7) 0.0066(6) -0.0012(5) 0.0005(5) C8 0.0191(7) 0.0315(10) 0.0270(9) 0.0119(8) -0.0047(6) 0.0009(6) C9 0.0333(9) 0.0275(9) 0.0218(8) 0.0114(7) 0.0046(7) -0.0048(7) C10 0.0190(7) 0.0331(10) 0.0215(8) 0.0125(7) -0.0032(6) -0.0027(6) C11 0.0263(8) 0.0141(7) 0.0159(7) 0.0051(6) -0.0015(6) -0.0004(6) C12 0.0211(7) 0.0147(7) 0.0181(7) 0.0070(6) 0.0003(5) -0.0012(5) C13 0.0265(8) 0.0166(7) 0.0247(8) 0.0113(6) 0.0034(6) 0.0034(6) C14 0.0309(9) 0.0235(8) 0.0235(8) 0.0154(7) 0.0058(7) 0.0062(7) C15 0.0316(9) 0.0247(8) 0.0187(8) 0.0129(7) 0.0036(6) 0.0044(7) C16 0.0221(7) 0.0196(7) 0.0156(7) 0.0080(6) 0.0009(5) 0.0009(6) C17 0.0301(8) 0.0195(8) 0.0152(7) 0.0063(6) 0.0011(6) 0.0025(6) C18 0.0180(6) 0.0167(7) 0.0135(6) 0.0042(5) -0.0002(5) 0.0004(5) C19 0.0172(6) 0.0183(7) 0.0211(7) 0.0053(6) 0.0015(5) 0.0014(5) C20 0.0227(7) 0.0177(7) 0.0263(8) 0.0062(6) -0.0001(6) 0.0042(6) C21 0.0263(8) 0.0188(8) 0.0219(8) 0.0088(6) -0.0032(6) -0.0016(6) C22 0.0178(7) 0.0241(8) 0.0209(8) 0.0084(6) -0.0025(6) -0.0037(6) C23 0.0162(6) 0.0223(8) 0.0177(7) 0.0055(6) -0.0008(5) 0.0018(5) C24 0.0181(7) 0.0254(9) 0.0353(10) 0.0065(8) 0.0054(7) 0.0013(6) C25 0.0365(10) 0.0196(8) 0.0357(11) 0.0105(8) -0.0079(8) -0.0061(7) C26 0.0189(7) 0.0306(10) 0.0309(10) 0.0026(8) -0.0014(7) 0.0054(7) P1 0.01495(16) 0.01500(18) 0.01645(18) 0.00465(14) 0.00121(13) 0.00043(13) O2 0.0233(6) 0.0198(6) 0.0201(6) 0.0026(5) 0.0056(4) 0.0019(4) C27 0.0162(6) 0.0202(7) 0.0145(7) 0.0044(6) 0.0005(5) 0.0000(5) C28 0.0207(7) 0.0291(9) 0.0220(8) 0.0116(7) -0.0012(6) -0.0031(6) C29 0.0225(8) 0.0392(11) 0.0250(9) 0.0126(8) -0.0006(7) -0.0088(7) C30 0.0157(7) 0.0470(12) 0.0205(8) 0.0062(8) 0.0005(6) 0.0002(7) C31 0.0217(8) 0.0343(10) 0.0251(9) 0.0051(8) 0.0002(6) 0.0094(7) C32 0.0201(7) 0.0214(8) 0.0251(8) 0.0057(7) 0.0004(6) 0.0031(6) C33 0.0156(6) 0.0171(7) 0.0212(7) 0.0082(6) -0.0001(5) 0.0000(5) C34 0.0239(8) 0.0280(9) 0.0306(9) 0.0145(8) 0.0047(7) 0.0088(7) C35 0.0306(10) 0.0409(12) 0.0439(12) 0.0250(10) 0.0000(9) 0.0125(9) C36 0.0327(10) 0.0358(11) 0.0321(10) 0.0216(9) -0.0077(8) -0.0037(8) C37 0.0397(10) 0.0237(9) 0.0222(9) 0.0104(7) 0.0008(7) -0.0014(8) C38 0.0314(9) 0.0189(8) 0.0232(8) 0.0090(7) 0.0031(7) 0.0043(6) C39 0.0164(6) 0.0168(7) 0.0210(7) 0.0058(6) 0.0017(5) -0.0003(5) C40 0.0338(9) 0.0194(8) 0.0259(9) 0.0129(7) 0.0055(7) -0.0019(7) C41 0.0383(11) 0.0260(9) 0.0320(10) 0.0165(8) -0.0018(8) -0.0066(8) C42 0.0354(10) 0.0193(8) 0.0353(11) 0.0081(8) 0.0042(8) -0.0055(7) C43 0.0357(10) 0.0234(9) 0.0254(9) 0.0025(7) 0.0006(7) -0.0101(7) C44 0.0275(8) 0.0212(8) 0.0183(8) 0.0043(6) 0.0003(6) -0.0040(6) _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 O1 1.6926(12) . ? Re1 N3 1.9718(14) . ? Re1 N1 1.9774(14) . ? Re1 N2 2.0648(13) . ? Re1 C1 2.1278(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? N1 C2 1.428(2) . ? N1 C11 1.472(2) . ? N2 C12 1.349(2) . ? N2 C16 1.352(2) . ? N3 C18 1.430(2) . ? N3 C17 1.472(2) . ? C2 C3 1.404(2) . ? C2 C7 1.409(2) . ? C3 C4 1.394(2) . ? C3 C8 1.508(2) . ? C4 C5 1.394(2) . ? C4 H4 0.9500 . ? C5 C6 1.390(2) . ? C5 C9 1.507(2) . ? C6 C7 1.391(2) . ? C6 H6 0.9500 . ? C7 C10 1.507(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.499(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.387(2) . ? C13 C14 1.390(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.382(2) . ? C15 H15 0.9500 . ? C16 C17 1.500(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.399(2) . ? C18 C23 1.404(2) . ? C19 C20 1.393(2) . ? C19 C24 1.508(2) . ? C20 C21 1.395(3) . ? C20 H20 0.9500 . ? C21 C22 1.391(3) . ? C21 C25 1.506(3) . ? C22 C23 1.394(2) . ? C22 H22 0.9500 . ? C23 C26 1.506(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? P1 O2 1.4895(13) . ? P1 C27 1.8053(16) . ? P1 C33 1.8063(17) . ? P1 C39 1.8097(17) . ? C27 C32 1.393(2) . ? C27 C28 1.398(3) . ? C28 C29 1.391(3) . ? C28 H28 0.9500 . ? C29 C30 1.392(3) . ? C29 H29 0.9500 . ? C30 C31 1.381(3) . ? C30 H30 0.9500 . ? C31 C32 1.398(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.390(2) . ? C33 C34 1.392(2) . ? C34 C35 1.392(3) . ? C34 H34 0.9500 . ? C35 C36 1.386(3) . ? C35 H35 0.9500 . ? C36 C37 1.389(3) . ? C36 H36 0.9500 . ? C37 C38 1.391(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.383(2) . ? C39 C44 1.399(2) . ? C40 C41 1.375(3) . ? C40 H40 0.9500 . ? C41 C42 1.379(3) . ? C41 H41 0.9500 . ? C42 C43 1.393(3) . ? C42 H42 0.9500 . ? C43 C44 1.391(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? 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 O1 Re1 N3 111.76(6) . . ? O1 Re1 N1 111.41(6) . . ? N3 Re1 N1 135.88(6) . . ? O1 Re1 N2 117.59(6) . . ? N3 Re1 N2 76.29(5) . . ? N1 Re1 N2 76.23(5) . . ? O1 Re1 C1 104.61(6) . . ? N3 Re1 C1 89.37(6) . . ? N1 Re1 C1 88.41(6) . . ? N2 Re1 C1 137.79(6) . . ? Re1 C1 H1A 109.5 . . ? Re1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Re1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 N1 C11 113.53(13) . . ? C2 N1 Re1 128.88(10) . . ? C11 N1 Re1 117.54(10) . . ? C12 N2 C16 122.17(14) . . ? C12 N2 Re1 118.92(11) . . ? C16 N2 Re1 118.88(11) . . ? C18 N3 C17 112.83(13) . . ? C18 N3 Re1 129.78(11) . . ? C17 N3 Re1 117.38(11) . . ? C3 C2 C7 119.65(15) . . ? C3 C2 N1 121.06(13) . . ? C7 C2 N1 119.29(14) . . ? C4 C3 C2 119.37(14) . . ? C4 C3 C8 119.99(15) . . ? C2 C3 C8 120.62(15) . . ? C5 C4 C3 121.84(16) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C6 C5 C4 117.72(16) . . ? C6 C5 C9 120.40(15) . . ? C4 C5 C9 121.87(16) . . ? C5 C6 C7 122.42(15) . . ? C5 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C6 C7 C2 118.92(15) . . ? C6 C7 C10 120.81(14) . . ? C2 C7 C10 120.27(15) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 108.51(13) . . ? N1 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? N1 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N2 C12 C13 120.15(15) . . ? N2 C12 C11 112.47(14) . . ? C13 C12 C11 127.31(15) . . ? C12 C13 C14 118.16(16) . . ? C12 C13 H13 120.9 . . ? C14 C13 H13 120.9 . . ? C15 C14 C13 120.83(16) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 118.97(16) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? N2 C16 C15 119.57(16) . . ? N2 C16 C17 112.02(14) . . ? C15 C16 C17 128.33(15) . . ? N3 C17 C16 108.78(13) . . ? N3 C17 H17A 109.9 . . ? C16 C17 H17A 109.9 . . ? N3 C17 H17B 109.9 . . ? C16 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C19 C18 C23 120.18(15) . . ? C19 C18 N3 119.91(14) . . ? C23 C18 N3 119.91(14) . . ? C20 C19 C18 119.01(15) . . ? C20 C19 C24 120.37(15) . . ? C18 C19 C24 120.61(15) . . ? C19 C20 C21 122.06(16) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C22 C21 C20 117.71(16) . . ? C22 C21 C25 121.49(17) . . ? C20 C21 C25 120.80(17) . . ? C21 C22 C23 122.07(15) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C22 C23 C18 118.94(15) . . ? C22 C23 C26 120.66(15) . . ? C18 C23 C26 120.40(16) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 P1 C27 111.95(7) . . ? O2 P1 C33 111.84(8) . . ? C27 P1 C33 104.60(8) . . ? O2 P1 C39 111.72(8) . . ? C27 P1 C39 108.96(8) . . ? C33 P1 C39 107.43(8) . . ? C32 C27 C28 119.27(16) . . ? C32 C27 P1 124.30(14) . . ? C28 C27 P1 116.27(13) . . ? C29 C28 C27 120.20(18) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.12(19) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C31 C30 C29 120.04(17) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.14(18) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C27 C32 C31 120.24(18) . . ? C27 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C38 C33 C34 119.48(16) . . ? C38 C33 P1 123.30(13) . . ? C34 C33 P1 117.19(14) . . ? C33 C34 C35 120.09(19) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.09(19) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.03(18) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C36 C37 C38 119.81(19) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C33 C38 C37 120.44(17) . . ? C33 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C40 C39 C44 118.33(16) . . ? C40 C39 P1 117.91(13) . . ? C44 C39 P1 123.53(13) . . ? C41 C40 C39 122.27(19) . . ? C41 C40 H40 118.9 . . ? C39 C40 H40 118.9 . . ? C40 C41 C42 119.39(19) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C41 C42 C43 119.82(18) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C44 C43 C42 120.37(18) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C39 119.78(17) . . ? C43 C44 H44 120.1 . . ? C39 C44 H44 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Re1 N1 C2 -85.81(14) . . . . ? N3 Re1 N1 C2 106.71(13) . . . . ? N2 Re1 N1 C2 159.60(14) . . . . ? C1 Re1 N1 C2 19.27(13) . . . . ? O1 Re1 N1 C11 91.24(12) . . . . ? N3 Re1 N1 C11 -76.23(14) . . . . ? N2 Re1 N1 C11 -23.35(11) . . . . ? C1 Re1 N1 C11 -163.68(12) . . . . ? O1 Re1 N2 C12 -89.27(13) . . . . ? N3 Re1 N2 C12 163.09(13) . . . . ? N1 Re1 N2 C12 17.94(12) . . . . ? C1 Re1 N2 C12 89.71(15) . . . . ? O1 Re1 N2 C16 88.93(13) . . . . ? N3 Re1 N2 C16 -18.70(12) . . . . ? N1 Re1 N2 C16 -163.85(14) . . . . ? C1 Re1 N2 C16 -92.08(15) . . . . ? O1 Re1 N3 C18 87.89(14) . . . . ? N1 Re1 N3 C18 -104.66(14) . . . . ? N2 Re1 N3 C18 -157.53(15) . . . . ? C1 Re1 N3 C18 -17.61(14) . . . . ? O1 Re1 N3 C17 -90.68(13) . . . . ? N1 Re1 N3 C17 76.76(15) . . . . ? N2 Re1 N3 C17 23.89(12) . . . . ? C1 Re1 N3 C17 163.82(13) . . . . ? C11 N1 C2 C3 78.35(19) . . . . ? Re1 N1 C2 C3 -104.50(16) . . . . ? C11 N1 C2 C7 -102.58(17) . . . . ? Re1 N1 C2 C7 74.57(18) . . . . ? C7 C2 C3 C4 -3.3(2) . . . . ? N1 C2 C3 C4 175.81(15) . . . . ? C7 C2 C3 C8 178.39(16) . . . . ? N1 C2 C3 C8 -2.5(2) . . . . ? C2 C3 C4 C5 1.7(3) . . . . ? C8 C3 C4 C5 -179.96(17) . . . . ? C3 C4 C5 C6 1.0(3) . . . . ? C3 C4 C5 C9 -177.45(17) . . . . ? C4 C5 C6 C7 -2.2(3) . . . . ? C9 C5 C6 C7 176.32(16) . . . . ? C5 C6 C7 C2 0.6(3) . . . . ? C5 C6 C7 C10 -178.48(17) . . . . ? C3 C2 C7 C6 2.2(2) . . . . ? N1 C2 C7 C6 -176.93(15) . . . . ? C3 C2 C7 C10 -178.77(16) . . . . ? N1 C2 C7 C10 2.1(2) . . . . ? C2 N1 C11 C12 -157.27(13) . . . . ? Re1 N1 C11 C12 25.23(17) . . . . ? C16 N2 C12 C13 -4.3(3) . . . . ? Re1 N2 C12 C13 173.82(13) . . . . ? C16 N2 C12 C11 172.91(15) . . . . ? Re1 N2 C12 C11 -8.94(19) . . . . ? N1 C11 C12 N2 -9.5(2) . . . . ? N1 C11 C12 C13 167.50(17) . . . . ? N2 C12 C13 C14 1.4(3) . . . . ? C11 C12 C13 C14 -175.43(17) . . . . ? C12 C13 C14 C15 1.1(3) . . . . ? C13 C14 C15 C16 -0.7(3) . . . . ? C12 N2 C16 C15 4.7(3) . . . . ? Re1 N2 C16 C15 -173.42(13) . . . . ? C12 N2 C16 C17 -172.22(15) . . . . ? Re1 N2 C16 C17 9.64(19) . . . . ? C14 C15 C16 N2 -2.2(3) . . . . ? C14 C15 C16 C17 174.22(18) . . . . ? C18 N3 C17 C16 155.55(14) . . . . ? Re1 N3 C17 C16 -25.64(18) . . . . ? N2 C16 C17 N3 9.3(2) . . . . ? C15 C16 C17 N3 -167.33(18) . . . . ? C17 N3 C18 C19 95.94(18) . . . . ? Re1 N3 C18 C19 -82.69(19) . . . . ? C17 N3 C18 C23 -84.80(19) . . . . ? Re1 N3 C18 C23 96.57(17) . . . . ? C23 C18 C19 C20 0.3(3) . . . . ? N3 C18 C19 C20 179.57(15) . . . . ? C23 C18 C19 C24 179.97(16) . . . . ? N3 C18 C19 C24 -0.8(2) . . . . ? C18 C19 C20 C21 -1.5(3) . . . . ? C24 C19 C20 C21 178.88(17) . . . . ? C19 C20 C21 C22 0.9(3) . . . . ? C19 C20 C21 C25 -178.58(18) . . . . ? C20 C21 C22 C23 0.9(3) . . . . ? C25 C21 C22 C23 -179.69(17) . . . . ? C21 C22 C23 C18 -2.0(3) . . . . ? C21 C22 C23 C26 178.12(17) . . . . ? C19 C18 C23 C22 1.3(2) . . . . ? N3 C18 C23 C22 -177.91(15) . . . . ? C19 C18 C23 C26 -178.73(16) . . . . ? N3 C18 C23 C26 2.0(2) . . . . ? O2 P1 C27 C32 107.73(15) . . . . ? C33 P1 C27 C32 -130.98(15) . . . . ? C39 P1 C27 C32 -16.36(17) . . . . ? O2 P1 C27 C28 -67.63(15) . . . . ? C33 P1 C27 C28 53.66(15) . . . . ? C39 P1 C27 C28 168.29(13) . . . . ? C32 C27 C28 C29 0.6(3) . . . . ? P1 C27 C28 C29 176.21(14) . . . . ? C27 C28 C29 C30 -0.3(3) . . . . ? C28 C29 C30 C31 0.0(3) . . . . ? C29 C30 C31 C32 -0.1(3) . . . . ? C28 C27 C32 C31 -0.7(3) . . . . ? P1 C27 C32 C31 -175.94(14) . . . . ? C30 C31 C32 C27 0.5(3) . . . . ? O2 P1 C33 C38 172.17(14) . . . . ? C27 P1 C33 C38 50.80(17) . . . . ? C39 P1 C33 C38 -64.90(16) . . . . ? O2 P1 C33 C34 -5.82(16) . . . . ? C27 P1 C33 C34 -127.19(14) . . . . ? C39 P1 C33 C34 117.11(14) . . . . ? C38 C33 C34 C35 1.2(3) . . . . ? P1 C33 C34 C35 179.25(16) . . . . ? C33 C34 C35 C36 1.3(3) . . . . ? C34 C35 C36 C37 -2.6(3) . . . . ? C35 C36 C37 C38 1.3(3) . . . . ? C34 C33 C38 C37 -2.4(3) . . . . ? P1 C33 C38 C37 179.62(15) . . . . ? C36 C37 C38 C33 1.2(3) . . . . ? O2 P1 C39 C40 -51.45(16) . . . . ? C27 P1 C39 C40 72.77(16) . . . . ? C33 P1 C39 C40 -174.46(14) . . . . ? O2 P1 C39 C44 122.93(15) . . . . ? C27 P1 C39 C44 -112.86(15) . . . . ? C33 P1 C39 C44 -0.08(17) . . . . ? C44 C39 C40 C41 2.4(3) . . . . ? P1 C39 C40 C41 177.05(16) . . . . ? C39 C40 C41 C42 -1.6(3) . . . . ? C40 C41 C42 C43 -0.3(3) . . . . ? C41 C42 C43 C44 1.4(3) . . . . ? C42 C43 C44 C39 -0.6(3) . . . . ? C40 C39 C44 C43 -1.2(3) . . . . ? P1 C39 C44 C43 -175.60(15) . . . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 34.53 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.498 _refine_diff_density_min -1.231 _refine_diff_density_rms 0.141 #===END data_x2 _database_code_depnum_ccdc_archive 'CCDC 831036' #TrackingRef '- CIF[1].txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25.50 H30 Cl2 N3 O Re' _chemical_formula_weight 651.62 #formula should be (C25 H29 Cl N3 O Re) 0.5(CH2Cl2) 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6153(5) _cell_length_b 11.9246(6) _cell_length_c 12.6634(6) _cell_angle_alpha 63.761(2) _cell_angle_beta 73.053(2) _cell_angle_gamma 81.327(2) _cell_volume 1245.39(11) _cell_formula_units_Z 2 _cell_measurement_temperature 110 _cell_measurement_reflns_used 9996 _cell_measurement_theta_min 3.23 _cell_measurement_theta_max 41.47 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 642 _exptl_absorpt_coefficient_mu 5.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2533 _exptl_absorpt_correction_T_max 0.6340 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Kappa Axis X8 Apex2' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 76499 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 42.80 _reflns_number_total 16306 _reflns_number_gt 14661 _reflns_threshold_expression >2sigma(I) _computing_data_collection Apex2 _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution XS _computing_structure_refinement XL _computing_molecular_graphics NRCVAX _computing_publication_material cif2tables.py _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^)+(0.0302P)^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 16306 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.006 _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 0.889966(5) 0.629989(5) 0.621741(4) 0.00991(1) Uani 1 1 d . . . Cl1 Cl 0.65311(3) 0.70595(3) 0.67505(3) 0.01520(5) Uani 1 1 d . . . O1 O 0.87387(12) 0.49047(10) 0.62246(10) 0.01591(18) Uani 1 1 d . . . N1 N 0.92263(12) 0.60743(12) 0.77678(10) 0.01315(19) Uani 1 1 d . . . N2 N 1.10527(12) 0.66670(11) 0.57567(10) 0.01149(17) Uani 1 1 d . . . N3 N 0.91788(12) 0.76431(11) 0.45584(10) 0.01184(18) Uani 1 1 d . . . C2 C 0.82038(14) 0.61216(13) 0.88249(11) 0.0124(2) Uani 1 1 d . . . C3 C 0.80340(16) 0.72227(14) 0.90014(12) 0.0145(2) Uani 1 1 d . . . C4 C 0.69936(16) 0.72677(15) 1.00161(13) 0.0162(2) Uani 1 1 d . . . H4 H 0.6897 0.8001 1.0152 0.019 Uiso 1 1 calc R . . C5 C 0.60952(15) 0.62689(15) 1.08336(12) 0.0155(2) Uani 1 1 d . . . C6 C 0.62953(16) 0.51825(15) 1.06437(12) 0.0155(2) Uani 1 1 d . . . H6 H 0.5687 0.4494 1.1192 0.019 Uiso 1 1 calc R . . C7 C 0.73667(15) 0.50790(14) 0.96692(12) 0.0139(2) Uani 1 1 d . . . C8 C 0.8898(2) 0.83578(16) 0.80850(15) 0.0231(3) Uani 1 1 d . . . H8A H 0.8581 0.9052 0.8323 0.035 Uiso 1 1 calc R . . H8B H 0.8742 0.8592 0.7282 0.035 Uiso 1 1 calc R . . H8C H 0.9933 0.8170 0.8052 0.035 Uiso 1 1 calc R . . C9 C 0.49360(18) 0.63586(18) 1.18974(14) 0.0213(3) Uani 1 1 d . . . H9A H 0.5396 0.6340 1.2501 0.032 Uiso 1 1 calc R . . H9B H 0.4286 0.5651 1.2269 0.032 Uiso 1 1 calc R . . H9C H 0.4374 0.7143 1.1611 0.032 Uiso 1 1 calc R . . C10 C 0.76210(19) 0.38595(15) 0.95539(14) 0.0200(3) Uani 1 1 d . . . H10A H 0.6815 0.3303 1.0111 0.030 Uiso 1 1 calc R . . H10B H 0.8535 0.3467 0.9760 0.030 Uiso 1 1 calc R . . H10C H 0.7679 0.4012 0.8716 0.030 Uiso 1 1 calc R . . C11 C 1.07302(15) 0.57973(15) 0.78957(12) 0.0154(2) Uani 1 1 d . . . H11A H 1.0885 0.4884 0.8328 0.018 Uiso 1 1 calc R . . H11B H 1.0913 0.6204 0.8374 0.018 Uiso 1 1 calc R . . C12 C 1.17505(14) 0.62830(13) 0.66480(12) 0.0130(2) Uani 1 1 d . . . C13 C 1.32329(15) 0.64440(15) 0.63505(13) 0.0159(2) Uani 1 1 d . . . H13 H 1.3742 0.6158 0.6967 0.019 Uiso 1 1 calc R . . C14 C 1.39649(16) 0.70388(16) 0.51194(14) 0.0180(2) Uani 1 1 d . . . H14 H 1.4987 0.7135 0.4894 0.022 Uiso 1 1 calc R . . C15 C 1.32016(15) 0.74892(15) 0.42255(13) 0.0158(2) Uani 1 1 d . . . H15 H 1.3690 0.7912 0.3391 0.019 Uiso 1 1 calc R . . C16 C 1.17180(14) 0.73114(13) 0.45724(12) 0.0124(2) Uani 1 1 d . . . C17 C 1.06797(15) 0.78474(14) 0.37818(12) 0.0133(2) Uani 1 1 d . . . H17A H 1.0838 0.8754 0.3285 0.016 Uiso 1 1 calc R . . H17B H 1.0843 0.7438 0.3224 0.016 Uiso 1 1 calc R . . C18 C 0.81391(14) 0.83893(13) 0.39018(11) 0.0120(2) Uani 1 1 d . . . C19 C 0.76657(15) 0.79748(14) 0.31825(12) 0.0139(2) Uani 1 1 d . . . C20 C 0.67026(16) 0.87276(14) 0.25022(13) 0.0162(2) Uani 1 1 d . . . H20 H 0.6406 0.8456 0.2002 0.019 Uiso 1 1 calc R . . C21 C 0.61580(17) 0.98699(15) 0.25323(14) 0.0181(2) Uani 1 1 d . . . C22 C 0.66289(17) 1.02561(15) 0.32599(14) 0.0182(2) Uani 1 1 d . . . H22 H 0.6266 1.1028 0.3297 0.022 Uiso 1 1 calc R . . C23 C 0.76190(16) 0.95401(14) 0.39358(13) 0.0148(2) Uani 1 1 d . . . C24 C 0.81724(19) 0.67283(16) 0.31545(16) 0.0211(3) Uani 1 1 d . . . H24A H 0.7766 0.6615 0.2583 0.032 Uiso 1 1 calc R . . H24B H 0.7844 0.6059 0.3970 0.032 Uiso 1 1 calc R . . H24C H 0.9237 0.6699 0.2892 0.032 Uiso 1 1 calc R . . C25 C 0.5105(2) 1.06644(18) 0.17955(18) 0.0281(4) Uani 1 1 d . . . H25A H 0.4391 1.0128 0.1841 0.042 Uiso 1 1 calc R . . H25B H 0.5637 1.1115 0.0945 0.042 Uiso 1 1 calc R . . H25C H 0.4602 1.1267 0.2121 0.042 Uiso 1 1 calc R . . C26 C 0.80958(15) 1.00045(8) 0.47037(8) 0.0215(3) Uani 1 1 d . . . H26A H 0.8151 1.0918 0.4296 0.032 Uiso 1 1 calc R . . H26B H 0.9055 0.9639 0.4815 0.032 Uiso 1 1 calc R . . H26C H 0.7392 0.9758 0.5499 0.032 Uiso 1 1 calc R . . C1Y C 1.03012(11) 0.95389(8) 0.96843(7) 0.0373(9) Uani 0.50 1 d PR A -1 H1Y1 H 1.0826 0.9644 0.8849 0.045 Uiso 0.50 1 calc PR B -1 H1Y2 H 0.9648 0.8824 1.0046 0.045 Uiso 0.50 1 calc PR C -1 Cl1Y Cl 1.15888(10) 0.91927(9) 1.05647(8) 0.0410(3) Uani 0.50 1 d PR A -1 Cl2Y Cl 0.92713(10) 1.08697(11) 0.96096(8) 0.0617(4) Uani 0.50 1 d PR A -1 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 0.00896(2) 0.01063(2) 0.00983(2) -0.00382(2) -0.00252(2) -0.00064(1) Cl1 0.00981(11) 0.01916(14) 0.01492(12) -0.00648(11) -0.00229(10) 0.00060(10) O1 0.0158(4) 0.0136(4) 0.0185(4) -0.0065(4) -0.0045(4) -0.0014(3) N1 0.0105(4) 0.0179(5) 0.0110(4) -0.0062(4) -0.0028(4) -0.0001(4) N2 0.0106(4) 0.0122(4) 0.0114(4) -0.0049(4) -0.0025(4) -0.0002(3) N3 0.0104(4) 0.0130(5) 0.0107(4) -0.0036(4) -0.0029(4) -0.0002(3) C2 0.0112(5) 0.0149(5) 0.0098(4) -0.0043(4) -0.0023(4) -0.0007(4) C3 0.0164(5) 0.0140(5) 0.0117(5) -0.0044(4) -0.0028(4) -0.0016(4) C4 0.0172(6) 0.0177(6) 0.0141(5) -0.0075(5) -0.0037(5) 0.0008(5) C5 0.0130(5) 0.0211(6) 0.0127(5) -0.0074(5) -0.0036(4) 0.0003(5) C6 0.0144(5) 0.0186(6) 0.0113(5) -0.0039(4) -0.0025(4) -0.0034(5) C7 0.0139(5) 0.0153(6) 0.0109(4) -0.0034(4) -0.0033(4) -0.0025(4) C8 0.0299(8) 0.0178(7) 0.0185(6) -0.0067(5) 0.0005(6) -0.0081(6) C9 0.0168(6) 0.0299(8) 0.0177(6) -0.0126(6) -0.0009(5) -0.0010(6) C10 0.0263(7) 0.0155(6) 0.0172(6) -0.0061(5) -0.0042(6) -0.0027(5) C11 0.0123(5) 0.0202(6) 0.0125(5) -0.0056(5) -0.0037(4) 0.0001(4) C12 0.0113(5) 0.0151(5) 0.0132(5) -0.0061(4) -0.0038(4) 0.0004(4) C13 0.0112(5) 0.0204(6) 0.0163(5) -0.0075(5) -0.0048(4) 0.0010(4) C14 0.0105(5) 0.0244(7) 0.0182(6) -0.0093(5) -0.0020(5) -0.0006(5) C15 0.0119(5) 0.0209(6) 0.0137(5) -0.0074(5) -0.0011(4) -0.0016(5) C16 0.0121(5) 0.0136(5) 0.0118(4) -0.0062(4) -0.0021(4) -0.0007(4) C17 0.0125(5) 0.0150(5) 0.0109(4) -0.0041(4) -0.0026(4) -0.0009(4) C18 0.0122(5) 0.0120(5) 0.0112(4) -0.0042(4) -0.0037(4) 0.0006(4) C19 0.0143(5) 0.0144(5) 0.0140(5) -0.0064(4) -0.0050(4) 0.0007(4) C20 0.0171(6) 0.0169(6) 0.0159(5) -0.0061(5) -0.0076(5) 0.0002(5) C21 0.0176(6) 0.0179(6) 0.0179(6) -0.0050(5) -0.0088(5) 0.0029(5) C22 0.0206(6) 0.0144(6) 0.0201(6) -0.0072(5) -0.0084(5) 0.0039(5) C23 0.0169(5) 0.0136(5) 0.0151(5) -0.0067(4) -0.0053(5) 0.0010(4) C24 0.0268(7) 0.0177(6) 0.0271(7) -0.0137(6) -0.0145(6) 0.0051(6) C25 0.0310(9) 0.0234(8) 0.0327(8) -0.0088(7) -0.0219(8) 0.0088(7) C26 0.0294(8) 0.0176(7) 0.0229(6) -0.0106(6) -0.0119(6) 0.0015(6) C1Y 0.045(2) 0.036(2) 0.0294(18) -0.0153(17) -0.0017(18) -0.0088(19) Cl1Y 0.0667(8) 0.0342(5) 0.0218(4) -0.0107(4) -0.0126(5) -0.0014(6) Cl2Y 0.0605(9) 0.0593(9) 0.0367(6) -0.0103(6) 0.0029(7) 0.0176(8) _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 O1 1.6898(11) . ? Re1 N3 1.9690(11) . ? Re1 N1 1.9730(11) . ? Re1 N2 2.0399(11) . ? Re1 Cl1 2.3420(3) . ? N1 C2 1.4299(17) . ? N1 C11 1.4736(18) . ? N2 C16 1.3486(17) . ? N2 C12 1.3512(17) . ? N3 C18 1.4299(17) . ? N3 C17 1.4751(17) . ? C2 C7 1.4005(19) . ? C2 C3 1.405(2) . ? C3 C4 1.396(2) . ? C3 C8 1.502(2) . ? C4 C5 1.391(2) . ? C4 H4 0.9500 . ? C5 C6 1.395(2) . ? C5 C9 1.511(2) . ? C6 C7 1.398(2) . ? C6 H6 0.9500 . ? C7 C10 1.502(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.5010(19) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.3842(19) . ? C13 C14 1.401(2) . ? C13 H13 0.9500 . ? C14 C15 1.392(2) . ? C14 H14 0.9500 . ? C15 C16 1.3843(19) . ? C15 H15 0.9500 . ? C16 C17 1.4940(19) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.403(2) . ? C18 C19 1.4102(18) . ? C19 C20 1.391(2) . ? C19 C24 1.505(2) . ? C20 C21 1.396(2) . ? C20 H20 0.9500 . ? C21 C22 1.396(2) . ? C21 C25 1.508(2) . ? C22 C23 1.397(2) . ? C22 H22 0.9500 . ? C23 C26 1.5083(16) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C1Y Cl2Y 1.7192 . ? C1Y Cl1Y 1.7861 . ? C1Y H1Y1 0.9900 . ? C1Y H1Y2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 N3 110.83(5) . . ? O1 Re1 N1 110.89(5) . . ? N3 Re1 N1 136.22(5) . . ? O1 Re1 N2 108.98(5) . . ? N3 Re1 N2 77.53(5) . . ? N1 Re1 N2 77.01(5) . . ? O1 Re1 Cl1 106.56(4) . . ? N3 Re1 Cl1 90.10(4) . . ? N1 Re1 Cl1 90.42(4) . . ? N2 Re1 Cl1 144.47(3) . . ? C2 N1 C11 113.37(11) . . ? C2 N1 Re1 129.55(9) . . ? C11 N1 Re1 117.07(8) . . ? C16 N2 C12 122.45(12) . . ? C16 N2 Re1 118.57(9) . . ? C12 N2 Re1 118.97(9) . . ? C18 N3 C17 112.03(10) . . ? C18 N3 Re1 130.55(9) . . ? C17 N3 Re1 117.00(9) . . ? C7 C2 C3 120.41(12) . . ? C7 C2 N1 119.97(13) . . ? C3 C2 N1 119.61(12) . . ? C4 C3 C2 118.84(13) . . ? C4 C3 C8 120.22(14) . . ? C2 C3 C8 120.86(13) . . ? C5 C4 C3 121.87(14) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 118.10(13) . . ? C4 C5 C9 120.92(14) . . ? C6 C5 C9 120.98(14) . . ? C5 C6 C7 121.83(13) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C6 C7 C2 118.79(13) . . ? C6 C7 C10 120.03(13) . . ? C2 C7 C10 121.18(13) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 108.49(11) . . ? N1 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? N1 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N2 C12 C13 119.87(12) . . ? N2 C12 C11 112.52(11) . . ? C13 C12 C11 127.44(12) . . ? C12 C13 C14 118.47(13) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 120.31(13) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 118.90(13) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? N2 C16 C15 119.69(12) . . ? N2 C16 C17 112.95(11) . . ? C15 C16 C17 127.17(12) . . ? N3 C17 C16 109.04(10) . . ? N3 C17 H17A 109.9 . . ? C16 C17 H17A 109.9 . . ? N3 C17 H17B 109.9 . . ? C16 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C23 C18 C19 119.75(12) . . ? C23 C18 N3 120.97(12) . . ? C19 C18 N3 119.25(12) . . ? C20 C19 C18 119.19(13) . . ? C20 C19 C24 119.84(13) . . ? C18 C19 C24 120.97(13) . . ? C19 C20 C21 122.05(13) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C22 C21 C20 117.80(14) . . ? C22 C21 C25 121.09(15) . . ? C20 C21 C25 121.10(14) . . ? C21 C22 C23 121.87(14) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C22 C23 C18 119.31(13) . . ? C22 C23 C26 119.67(12) . . ? C18 C23 C26 121.01(12) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Cl2Y C1Y Cl1Y 112.7 . . ? Cl2Y C1Y H1Y1 109.1 . . ? Cl1Y C1Y H1Y1 109.1 . . ? Cl2Y C1Y H1Y2 109.1 . . ? Cl1Y C1Y H1Y2 109.1 . . ? H1Y1 C1Y H1Y2 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Re1 N1 C2 -96.04(13) . . . . ? N3 Re1 N1 C2 102.47(13) . . . . ? N2 Re1 N1 C2 158.35(13) . . . . ? Cl1 Re1 N1 C2 11.89(12) . . . . ? O1 Re1 N1 C11 83.01(11) . . . . ? N3 Re1 N1 C11 -78.49(13) . . . . ? N2 Re1 N1 C11 -22.61(10) . . . . ? Cl1 Re1 N1 C11 -169.06(10) . . . . ? O1 Re1 N2 C16 91.20(11) . . . . ? N3 Re1 N2 C16 -16.80(10) . . . . ? N1 Re1 N2 C16 -160.89(11) . . . . ? Cl1 Re1 N2 C16 -88.95(11) . . . . ? O1 Re1 N2 C12 -90.33(11) . . . . ? N3 Re1 N2 C12 161.67(11) . . . . ? N1 Re1 N2 C12 17.58(10) . . . . ? Cl1 Re1 N2 C12 89.52(12) . . . . ? O1 Re1 N3 C18 86.48(12) . . . . ? N1 Re1 N3 C18 -112.02(12) . . . . ? N2 Re1 N3 C18 -167.72(13) . . . . ? Cl1 Re1 N3 C18 -21.31(12) . . . . ? O1 Re1 N3 C17 -85.32(10) . . . . ? N1 Re1 N3 C17 76.19(12) . . . . ? N2 Re1 N3 C17 20.48(9) . . . . ? Cl1 Re1 N3 C17 166.89(9) . . . . ? C11 N1 C2 C7 -98.22(15) . . . . ? Re1 N1 C2 C7 80.86(16) . . . . ? C11 N1 C2 C3 82.53(16) . . . . ? Re1 N1 C2 C3 -98.39(15) . . . . ? C7 C2 C3 C4 -1.5(2) . . . . ? N1 C2 C3 C4 177.72(13) . . . . ? C7 C2 C3 C8 -178.37(14) . . . . ? N1 C2 C3 C8 0.9(2) . . . . ? C2 C3 C4 C5 -1.9(2) . . . . ? C8 C3 C4 C5 174.94(15) . . . . ? C3 C4 C5 C6 2.5(2) . . . . ? C3 C4 C5 C9 -177.51(14) . . . . ? C4 C5 C6 C7 0.3(2) . . . . ? C9 C5 C6 C7 -179.63(14) . . . . ? C5 C6 C7 C2 -3.7(2) . . . . ? C5 C6 C7 C10 175.27(14) . . . . ? C3 C2 C7 C6 4.2(2) . . . . ? N1 C2 C7 C6 -175.01(12) . . . . ? C3 C2 C7 C10 -174.70(13) . . . . ? N1 C2 C7 C10 6.1(2) . . . . ? C2 N1 C11 C12 -156.66(12) . . . . ? Re1 N1 C11 C12 24.14(15) . . . . ? C16 N2 C12 C13 -6.1(2) . . . . ? Re1 N2 C12 C13 175.45(11) . . . . ? C16 N2 C12 C11 169.48(13) . . . . ? Re1 N2 C12 C11 -8.93(16) . . . . ? N1 C11 C12 N2 -9.03(17) . . . . ? N1 C11 C12 C13 166.19(15) . . . . ? N2 C12 C13 C14 1.7(2) . . . . ? C11 C12 C13 C14 -173.15(15) . . . . ? C12 C13 C14 C15 2.0(2) . . . . ? C13 C14 C15 C16 -1.6(2) . . . . ? C12 N2 C16 C15 6.6(2) . . . . ? Re1 N2 C16 C15 -175.02(11) . . . . ? C12 N2 C16 C17 -168.89(13) . . . . ? Re1 N2 C16 C17 9.53(15) . . . . ? C14 C15 C16 N2 -2.6(2) . . . . ? C14 C15 C16 C17 172.15(14) . . . . ? C18 N3 C17 C16 165.51(11) . . . . ? Re1 N3 C17 C16 -21.20(14) . . . . ? N2 C16 C17 N3 6.90(16) . . . . ? C15 C16 C17 N3 -168.13(14) . . . . ? C17 N3 C18 C23 -96.31(15) . . . . ? Re1 N3 C18 C23 91.58(15) . . . . ? C17 N3 C18 C19 81.82(15) . . . . ? Re1 N3 C18 C19 -90.30(15) . . . . ? C23 C18 C19 C20 0.9(2) . . . . ? N3 C18 C19 C20 -177.21(12) . . . . ? C23 C18 C19 C24 -178.30(14) . . . . ? N3 C18 C19 C24 3.5(2) . . . . ? C18 C19 C20 C21 -1.7(2) . . . . ? C24 C19 C20 C21 177.57(15) . . . . ? C19 C20 C21 C22 1.0(2) . . . . ? C19 C20 C21 C25 -179.45(15) . . . . ? C20 C21 C22 C23 0.4(2) . . . . ? C25 C21 C22 C23 -179.13(16) . . . . ? C21 C22 C23 C18 -1.1(2) . . . . ? C21 C22 C23 C26 179.76(14) . . . . ? C19 C18 C23 C22 0.4(2) . . . . ? N3 C18 C23 C22 178.53(13) . . . . ? C19 C18 C23 C26 179.53(12) . . . . ? N3 C18 C23 C26 -2.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 37.04 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.558 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.177 #===END data_x8 _database_code_depnum_ccdc_archive 'CCDC 831037' #TrackingRef '- CIF[1].txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H28 N3 O3 Re' _chemical_formula_weight 604.70 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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9434(13) _cell_length_b 13.1771(10) _cell_length_c 11.4807(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.956(4) _cell_angle_gamma 90.00 _cell_volume 2408.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110 _cell_measurement_reflns_used 9904 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 24.42 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 5.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3287 _exptl_absorpt_correction_T_max 0.9510 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Kappa Axis X8 Apex2' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 74284 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 32.56 _reflns_number_total 8715 _reflns_number_gt 5750 _reflns_threshold_expression >2sigma(I) _computing_data_collection Apex2 _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution SIR92 _computing_structure_refinement XL _computing_molecular_graphics NRCVAX _computing_publication_material cif2tables.py _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^)+(0.0414P)^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 8715 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 1.001309(10) 0.266369(12) 0.077842(13) 0.01878(6) Uani 1 1 d . . . O1 O 1.08522(18) 0.3233(2) 0.0155(2) 0.0267(7) Uani 1 1 d . . . O2 O 0.93907(19) 0.2184(2) -0.0355(2) 0.0273(7) Uani 1 1 d . . . O3 O 0.95118(18) 0.3642(2) 0.1457(2) 0.0263(7) Uani 1 1 d . . . N1 N 1.0768(2) 0.1713(2) 0.1606(3) 0.0185(7) Uani 1 1 d . . . N2 N 0.9189(2) 0.1717(2) 0.1962(3) 0.0184(7) Uani 1 1 d . . . N3 N 0.7097(2) 0.2654(3) 0.1283(3) 0.0286(8) Uani 1 1 d . . . C2 C 1.1649(2) 0.1638(3) 0.1370(3) 0.0187(8) Uani 1 1 d . . . C3 C 1.1908(3) 0.0908(3) 0.0572(3) 0.0221(9) Uani 1 1 d . . . C4 C 1.2754(3) 0.0867(3) 0.0351(3) 0.0267(10) Uani 1 1 d . . . H4 H 1.2936 0.0361 -0.0169 0.032 Uiso 1 1 calc R . . C5 C 1.3341(3) 0.1519(4) 0.0845(4) 0.0321(10) Uani 1 1 d . . . C6 C 1.3061(3) 0.2228(3) 0.1644(4) 0.0299(10) Uani 1 1 d . . . H6 H 1.3458 0.2680 0.2008 0.036 Uiso 1 1 calc R . . C7 C 1.2226(3) 0.2299(3) 0.1925(3) 0.0219(8) Uani 1 1 d . . . C8 C 1.1288(3) 0.0206(3) -0.0048(4) 0.0318(10) Uani 1 1 d . . . H8A H 1.1152 -0.0353 0.0473 0.048 Uiso 1 1 calc R . . H8B H 1.1533 -0.0069 -0.0747 0.048 Uiso 1 1 calc R . . H8C H 1.0775 0.0582 -0.0275 0.048 Uiso 1 1 calc R . . C9 C 1.4251(3) 0.1496(4) 0.0515(4) 0.0437(13) Uani 1 1 d . . . H9A H 1.4429 0.0791 0.0416 0.066 Uiso 1 1 calc R . . H9B H 1.4606 0.1816 0.1134 0.066 Uiso 1 1 calc R . . H9C H 1.4307 0.1867 -0.0217 0.066 Uiso 1 1 calc R . . C10 C 1.1954(3) 0.3060(4) 0.2811(4) 0.0326(10) Uani 1 1 d . . . H10A H 1.1758 0.2701 0.3493 0.049 Uiso 1 1 calc R . . H10B H 1.1497 0.3477 0.2465 0.049 Uiso 1 1 calc R . . H10C H 1.2430 0.3496 0.3050 0.049 Uiso 1 1 calc R . . C11 C 1.0524(2) 0.0980(3) 0.2495(3) 0.0206(8) Uani 1 1 d . . . H11A H 1.0839 0.1124 0.3243 0.025 Uiso 1 1 calc R . . H11B H 1.0666 0.0284 0.2248 0.025 Uiso 1 1 calc R . . C12 C 0.9605(2) 0.1053(3) 0.2659(3) 0.0190(8) Uani 1 1 d . . . C13 C 0.9208(3) 0.0472(3) 0.3486(3) 0.0217(8) Uani 1 1 d . . . H13 H 0.9520 0.0015 0.3980 0.026 Uiso 1 1 calc R . . C14 C 0.8351(3) 0.0577(3) 0.3569(4) 0.0249(9) Uani 1 1 d . . . H14 H 0.8063 0.0189 0.4121 0.030 Uiso 1 1 calc R . . C15 C 0.7915(3) 0.1256(3) 0.2839(3) 0.0246(9) Uani 1 1 d . . . H15 H 0.7325 0.1335 0.2885 0.029 Uiso 1 1 calc R . . C16 C 0.8346(2) 0.1819(3) 0.2039(3) 0.0193(8) Uani 1 1 d . . . C17 C 0.7884(3) 0.2520(3) 0.1220(4) 0.0232(9) Uani 1 1 d . . . H17 H 0.8179 0.2870 0.0644 0.028 Uiso 1 1 calc R . . C18 C 0.6682(2) 0.3322(3) 0.0461(3) 0.0221(9) Uani 1 1 d . . . C19 C 0.6729(3) 0.4371(3) 0.0609(4) 0.0244(9) Uani 1 1 d . . . C20 C 0.6268(3) 0.4973(3) -0.0179(4) 0.0299(10) Uani 1 1 d . . . H20 H 0.6296 0.5689 -0.0088 0.036 Uiso 1 1 calc R . . C21 C 0.5767(3) 0.4579(3) -0.1092(4) 0.0291(10) Uani 1 1 d . . . C22 C 0.5737(3) 0.3526(3) -0.1216(4) 0.0279(10) Uani 1 1 d . . . H22 H 0.5399 0.3237 -0.1836 0.033 Uiso 1 1 calc R . . C23 C 0.6192(3) 0.2892(3) -0.0450(4) 0.0236(9) Uani 1 1 d . . . C24 C 0.7269(3) 0.4840(4) 0.1587(4) 0.0367(11) Uani 1 1 d . . . H24A H 0.7191 0.5577 0.1581 0.055 Uiso 1 1 calc R . . H24B H 0.7860 0.4681 0.1479 0.055 Uiso 1 1 calc R . . H24C H 0.7106 0.4564 0.2335 0.055 Uiso 1 1 calc R . . C25 C 0.5280(3) 0.5263(4) -0.1936(4) 0.0400(12) Uani 1 1 d . . . H25A H 0.5107 0.5876 -0.1529 0.060 Uiso 1 1 calc R . . H25B H 0.4781 0.4905 -0.2256 0.060 Uiso 1 1 calc R . . H25C H 0.5636 0.5453 -0.2572 0.060 Uiso 1 1 calc R . . C26 C 0.6202(3) 0.1755(4) -0.0637(4) 0.0366(11) Uani 1 1 d . . . H26A H 0.5805 0.1577 -0.1285 0.055 Uiso 1 1 calc R . . H26B H 0.6040 0.1412 0.0074 0.055 Uiso 1 1 calc R . . H26C H 0.6769 0.1540 -0.0822 0.055 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 0.02321(9) 0.01653(8) 0.01688(8) 0.00174(6) 0.00366(6) 0.00089(7) O1 0.0326(17) 0.0256(17) 0.0224(14) 0.0040(12) 0.0043(12) 0.0044(13) O2 0.0322(17) 0.0276(17) 0.0223(15) 0.0033(12) 0.0026(12) 0.0000(13) O3 0.0309(17) 0.0197(15) 0.0288(16) 0.0033(12) 0.0065(13) -0.0001(12) N1 0.0213(18) 0.0185(17) 0.0163(15) 0.0005(13) 0.0050(13) -0.0018(13) N2 0.0234(18) 0.0193(17) 0.0129(15) -0.0002(12) 0.0034(13) 0.0014(14) N3 0.0226(19) 0.033(2) 0.030(2) 0.0076(16) 0.0031(15) 0.0048(16) C2 0.022(2) 0.019(2) 0.0151(17) 0.0025(15) 0.0039(15) -0.0012(16) C3 0.027(2) 0.019(2) 0.0205(19) 0.0030(16) 0.0062(16) 0.0048(17) C4 0.035(3) 0.024(2) 0.022(2) 0.0039(17) 0.0101(18) 0.0096(19) C5 0.025(2) 0.043(3) 0.028(2) 0.012(2) 0.0033(19) 0.001(2) C6 0.027(2) 0.036(3) 0.026(2) 0.0065(19) -0.0036(18) -0.0068(19) C7 0.025(2) 0.021(2) 0.0192(19) 0.0038(16) 0.0013(16) 0.0004(17) C8 0.040(3) 0.025(2) 0.031(2) -0.0093(19) 0.008(2) -0.002(2) C9 0.024(3) 0.064(4) 0.044(3) 0.011(3) 0.007(2) 0.001(2) C10 0.041(3) 0.031(2) 0.026(2) -0.010(2) 0.0018(19) -0.007(2) C11 0.023(2) 0.023(2) 0.0169(18) 0.0028(15) 0.0042(15) 0.0001(16) C12 0.022(2) 0.017(2) 0.0184(18) -0.0026(15) 0.0031(15) -0.0001(15) C13 0.028(2) 0.019(2) 0.0178(19) 0.0011(15) 0.0049(16) -0.0004(17) C14 0.033(3) 0.018(2) 0.025(2) -0.0016(16) 0.0098(18) -0.0024(17) C15 0.024(2) 0.023(2) 0.027(2) -0.0016(17) 0.0079(17) -0.0006(17) C16 0.021(2) 0.018(2) 0.0191(18) -0.0041(15) 0.0008(15) -0.0004(15) C17 0.028(2) 0.020(2) 0.022(2) -0.0014(15) 0.0039(17) -0.0009(16) C18 0.016(2) 0.032(2) 0.0184(19) 0.0026(17) 0.0049(15) 0.0029(17) C19 0.021(2) 0.027(2) 0.025(2) -0.0033(17) 0.0024(17) -0.0002(17) C20 0.032(3) 0.024(2) 0.035(3) -0.0028(19) 0.009(2) 0.0015(19) C21 0.026(2) 0.034(3) 0.028(2) 0.0080(19) 0.0067(18) 0.0024(19) C22 0.021(2) 0.038(3) 0.024(2) -0.0016(18) 0.0000(17) -0.0022(19) C23 0.021(2) 0.023(2) 0.028(2) 0.0021(17) 0.0076(17) 0.0005(16) C24 0.042(3) 0.035(3) 0.033(3) -0.007(2) -0.001(2) 0.002(2) C25 0.034(3) 0.050(3) 0.036(3) 0.014(2) 0.001(2) 0.006(2) C26 0.030(3) 0.033(3) 0.046(3) -0.005(2) 0.002(2) -0.004(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 O2 1.716(3) . ? Re1 O1 1.722(3) . ? Re1 O3 1.724(3) . ? Re1 N1 1.950(3) . ? Re1 N2 2.305(3) . ? N1 C2 1.449(5) . ? N1 C11 1.472(5) . ? N2 C12 1.338(5) . ? N2 C16 1.359(5) . ? N3 C17 1.273(6) . ? N3 C18 1.428(5) . ? C2 C7 1.396(6) . ? C2 C3 1.405(5) . ? C3 C4 1.386(6) . ? C3 C8 1.507(6) . ? C4 C5 1.372(6) . ? C4 H4 0.9500 . ? C5 C6 1.398(6) . ? C5 C9 1.519(6) . ? C6 C7 1.390(6) . ? C6 H6 0.9500 . ? C7 C10 1.507(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.490(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.397(5) . ? C13 C14 1.382(6) . ? C13 H13 0.9500 . ? C14 C15 1.389(6) . ? C14 H14 0.9500 . ? C15 C16 1.390(5) . ? C15 H15 0.9500 . ? C16 C17 1.485(6) . ? C17 H17 0.9500 . ? C18 C23 1.393(6) . ? C18 C19 1.395(6) . ? C19 C20 1.386(6) . ? C19 C24 1.511(6) . ? C20 C21 1.385(6) . ? C20 H20 0.9500 . ? C21 C22 1.395(6) . ? C21 C25 1.509(6) . ? C22 C23 1.390(6) . ? C22 H22 0.9500 . ? C23 C26 1.514(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 O2 Re1 O1 106.05(13) . . ? O2 Re1 O3 110.78(14) . . ? O1 Re1 O3 104.50(13) . . ? O2 Re1 N1 116.79(13) . . ? O1 Re1 N1 90.54(13) . . ? O3 Re1 N1 123.32(13) . . ? O2 Re1 N2 85.58(12) . . ? O1 Re1 N2 163.68(12) . . ? O3 Re1 N2 81.20(12) . . ? N1 Re1 N2 73.79(12) . . ? C2 N1 C11 112.2(3) . . ? C2 N1 Re1 122.2(2) . . ? C11 N1 Re1 125.5(3) . . ? C12 N2 C16 119.2(3) . . ? C12 N2 Re1 115.2(2) . . ? C16 N2 Re1 125.5(2) . . ? C17 N3 C18 118.2(4) . . ? C7 C2 C3 121.1(4) . . ? C7 C2 N1 119.6(3) . . ? C3 C2 N1 119.3(3) . . ? C4 C3 C2 117.9(4) . . ? C4 C3 C8 120.7(4) . . ? C2 C3 C8 121.4(4) . . ? C5 C4 C3 123.3(4) . . ? C5 C4 H4 118.4 . . ? C3 C4 H4 118.4 . . ? C4 C5 C6 117.2(4) . . ? C4 C5 C9 121.6(4) . . ? C6 C5 C9 121.2(4) . . ? C7 C6 C5 122.6(4) . . ? C7 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? C6 C7 C2 117.9(4) . . ? C6 C7 C10 120.9(4) . . ? C2 C7 C10 121.1(4) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 110.0(3) . . ? N1 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? N1 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N2 C12 C13 122.4(4) . . ? N2 C12 C11 115.3(3) . . ? C13 C12 C11 122.3(4) . . ? C14 C13 C12 118.5(4) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C15 119.3(4) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C16 119.6(4) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? N2 C16 C15 120.9(4) . . ? N2 C16 C17 118.7(3) . . ? C15 C16 C17 120.3(4) . . ? N3 C17 C16 120.5(4) . . ? N3 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C23 C18 C19 121.3(4) . . ? C23 C18 N3 118.0(4) . . ? C19 C18 N3 120.7(4) . . ? C20 C19 C18 117.7(4) . . ? C20 C19 C24 120.9(4) . . ? C18 C19 C24 121.4(4) . . ? C21 C20 C19 123.0(4) . . ? C21 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? C20 C21 C22 117.7(4) . . ? C20 C21 C25 121.3(4) . . ? C22 C21 C25 121.0(4) . . ? C23 C22 C21 121.3(4) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C18 119.0(4) . . ? C22 C23 C26 121.0(4) . . ? C18 C23 C26 119.9(4) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Re1 N1 C2 99.3(3) . . . . ? O1 Re1 N1 C2 -9.1(3) . . . . ? O3 Re1 N1 C2 -116.9(3) . . . . ? N2 Re1 N1 C2 175.6(3) . . . . ? O2 Re1 N1 C11 -78.9(3) . . . . ? O1 Re1 N1 C11 172.8(3) . . . . ? O3 Re1 N1 C11 65.0(3) . . . . ? N2 Re1 N1 C11 -2.6(3) . . . . ? O2 Re1 N2 C12 123.3(3) . . . . ? O1 Re1 N2 C12 -13.0(6) . . . . ? O3 Re1 N2 C12 -124.9(3) . . . . ? N1 Re1 N2 C12 3.7(2) . . . . ? O2 Re1 N2 C16 -60.1(3) . . . . ? O1 Re1 N2 C16 163.7(4) . . . . ? O3 Re1 N2 C16 51.8(3) . . . . ? N1 Re1 N2 C16 -179.6(3) . . . . ? C11 N1 C2 C7 -96.8(4) . . . . ? Re1 N1 C2 C7 84.8(4) . . . . ? C11 N1 C2 C3 84.0(4) . . . . ? Re1 N1 C2 C3 -94.4(4) . . . . ? C7 C2 C3 C4 -0.2(6) . . . . ? N1 C2 C3 C4 179.0(3) . . . . ? C7 C2 C3 C8 -178.8(4) . . . . ? N1 C2 C3 C8 0.4(5) . . . . ? C2 C3 C4 C5 -2.0(6) . . . . ? C8 C3 C4 C5 176.7(4) . . . . ? C3 C4 C5 C6 2.6(6) . . . . ? C3 C4 C5 C9 -175.6(4) . . . . ? C4 C5 C6 C7 -1.2(6) . . . . ? C9 C5 C6 C7 177.1(4) . . . . ? C5 C6 C7 C2 -0.8(6) . . . . ? C5 C6 C7 C10 178.7(4) . . . . ? C3 C2 C7 C6 1.5(6) . . . . ? N1 C2 C7 C6 -177.7(3) . . . . ? C3 C2 C7 C10 -178.0(4) . . . . ? N1 C2 C7 C10 2.8(6) . . . . ? C2 N1 C11 C12 -177.1(3) . . . . ? Re1 N1 C11 C12 1.2(4) . . . . ? C16 N2 C12 C13 -1.5(5) . . . . ? Re1 N2 C12 C13 175.4(3) . . . . ? C16 N2 C12 C11 178.9(3) . . . . ? Re1 N2 C12 C11 -4.2(4) . . . . ? N1 C11 C12 N2 2.3(5) . . . . ? N1 C11 C12 C13 -177.4(3) . . . . ? N2 C12 C13 C14 1.2(6) . . . . ? C11 C12 C13 C14 -179.2(4) . . . . ? C12 C13 C14 C15 -0.4(6) . . . . ? C13 C14 C15 C16 -0.1(6) . . . . ? C12 N2 C16 C15 0.9(5) . . . . ? Re1 N2 C16 C15 -175.6(3) . . . . ? C12 N2 C16 C17 -176.9(3) . . . . ? Re1 N2 C16 C17 6.5(5) . . . . ? C14 C15 C16 N2 -0.1(6) . . . . ? C14 C15 C16 C17 177.7(4) . . . . ? C18 N3 C17 C16 -178.9(4) . . . . ? N2 C16 C17 N3 -178.3(4) . . . . ? C15 C16 C17 N3 3.9(6) . . . . ? C17 N3 C18 C23 104.5(5) . . . . ? C17 N3 C18 C19 -79.1(5) . . . . ? C23 C18 C19 C20 0.4(6) . . . . ? N3 C18 C19 C20 -175.9(4) . . . . ? C23 C18 C19 C24 -179.2(4) . . . . ? N3 C18 C19 C24 4.5(6) . . . . ? C18 C19 C20 C21 0.1(6) . . . . ? C24 C19 C20 C21 179.7(4) . . . . ? C19 C20 C21 C22 -0.4(6) . . . . ? C19 C20 C21 C25 -179.5(4) . . . . ? C20 C21 C22 C23 0.1(6) . . . . ? C25 C21 C22 C23 179.2(4) . . . . ? C21 C22 C23 C18 0.4(6) . . . . ? C21 C22 C23 C26 -175.9(4) . . . . ? C19 C18 C23 C22 -0.7(6) . . . . ? N3 C18 C23 C22 175.8(4) . . . . ? C19 C18 C23 C26 175.7(4) . . . . ? N3 C18 C23 C26 -7.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 32.56 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 4.222 _refine_diff_density_min -2.412 _refine_diff_density_rms 0.210