Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name E.Alessio _publ_contact_author_address ; Dipartimento di Scienze Chimiche Universita di Trieste Via L Giorgieri 1 Trieste 34127 ITALY ; _publ_contact_author_email ALESSI@UNITS.IT _publ_section_title ; fac-[Re(CO)3(dmso-O)3](CF3SO3): a new versatile and efficient Re(I) precursor for the preparation of mono and polynuclear compounds containing fac-[Re(CO)3]+ fragments. ; loop_ _publ_author_name 'E. Alessio' 'Massimo Casanova' 'Elisabetta Iengo' 'Fabio Munini' 'Ennio Zangrando' data_1 _database_code_depnum_ccdc_archive 'CCDC 614597' _audit_creation_method SHELXL-97 _chemical_name_systematic ; fac-tricarbonyl-tris(dimethylsulfoxide,O)-rhenium(I) triflate ; _chemical_name_common 'fac-tricarbonyl-tris(dimethylsulfoxide,O)-rhenium(i) triflate' _chemical_melting_point ? _chemical_formula_moiety 'C9 H18 O6 Re S3 1+, C F3 O3 S 1-' _chemical_formula_sum 'C10 H18 F3 O9 Re S4' _chemical_formula_weight 653.68 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.171(3) _cell_length_b 11.379(4) _cell_length_c 13.922(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.40(3) _cell_angle_gamma 90.00 _cell_volume 1109.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 5.913 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.1261 _exptl_absorpt_correction_T_max 0.4267 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12091 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.10 _reflns_number_total 2306 _reflns_number_gt 1853 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.64.04 (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^)+(0.0665P)^2^+1.5326P] 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 2306 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.096 _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 Re Re 0.14877(6) 0.7500 0.14419(3) 0.0813(2) Uani 1 2 d S . . C4 C -0.0279(18) 0.6365(13) 0.0955(8) 0.119(3) Uani 1 1 d . A . O4 O -0.1444(19) 0.5619(12) 0.0671(9) 0.183(4) Uani 1 1 d . . . C5 C 0.215(2) 0.7500 0.0210(10) 0.099(4) Uani 1 2 d S A . O5 O 0.2511(18) 0.7500 -0.0551(8) 0.137(4) Uani 1 2 d S . . O1 O 0.0892(14) 0.7500 0.2904(6) 0.099(3) Uani 1 2 d S A . S1 S 0.2498(5) 0.7500 0.3832(2) 0.0846(7) Uani 1 2 d S . . C1 C 0.188(2) 0.6361(11) 0.4531(9) 0.137(4) Uani 1 1 d . A . H1A H 0.2143 0.5622 0.4256 0.205 Uiso 1 1 calc R . . H1B H 0.0539 0.6409 0.4529 0.205 Uiso 1 1 calc R . . H1C H 0.2602 0.6422 0.5194 0.205 Uiso 1 1 calc R . . O2 O 0.3263(18) 0.6139(11) 0.2149(8) 0.098(3) Uani 0.659(8) 1 d P A 1 S2 S 0.5187(6) 0.5797(3) 0.1889(3) 0.0965(14) Uani 0.659(8) 1 d P A 1 O2B O 0.415(3) 0.6579(15) 0.2068(14) 0.083(5) Uani 0.341(8) 1 d P A 2 S2B S 0.4368(12) 0.5383(6) 0.2488(5) 0.090(3) Uani 0.341(8) 1 d P A 2 C2 C 0.488(2) 0.4321(13) 0.1597(11) 0.159(6) Uani 1 1 d . . . H2A H 0.3998 0.4238 0.0977 0.238 Uiso 1 1 calc R A 1 H2B H 0.4389 0.3925 0.2099 0.238 Uiso 1 1 calc R A 1 H2C H 0.6087 0.3983 0.1554 0.238 Uiso 1 1 calc R A 1 C3 C 0.673(2) 0.5561(13) 0.3090(11) 0.159(6) Uani 1 1 d . . . H3A H 0.7125 0.6306 0.3388 0.239 Uiso 1 1 calc R A 1 H3B H 0.7829 0.5119 0.3019 0.239 Uiso 1 1 calc R A 1 H3C H 0.6042 0.5134 0.3499 0.239 Uiso 1 1 calc R A 1 S3 S 0.2834(6) 0.2500 0.4030(2) 0.0932(9) Uani 1 2 d S . . O30 O 0.435(2) 0.2500 0.3651(14) 0.258(13) Uani 1 2 d S . . O31 O 0.260(2) 0.3446(13) 0.4504(12) 0.264(9) Uani 1 1 d . . . C30 C 0.084(3) 0.2500 0.2992(14) 0.131(6) Uani 1 2 d S . . F30 F 0.076(2) 0.1478(14) 0.2474(11) 0.155(6) Uani 0.50 1 d P . . F31 F -0.098(3) 0.2500 0.3209(18) 0.121(6) Uani 0.50 2 d SP . . F30B F 0.128(4) 0.2500 0.2200(19) 0.152(8) Uani 0.50 2 d SP. . 2 F31B F -0.038(5) 0.178(2) 0.314(2) 0.221(11) Uani 0.50 1 d P. . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.0697(4) 0.1101(4) 0.0619(3) 0.000 0.00950(19) 0.000 C4 0.093(6) 0.164(8) 0.102(6) -0.017(6) 0.021(5) -0.028(6) O4 0.177(8) 0.221(8) 0.157(7) -0.035(6) 0.049(6) -0.077(7) C5 0.096(10) 0.133(11) 0.074(7) 0.000 0.032(6) 0.000 O5 0.126(10) 0.205(12) 0.087(6) 0.000 0.043(6) 0.000 O1 0.090(6) 0.139(7) 0.068(4) 0.000 0.014(4) 0.000 S1 0.0785(19) 0.107(2) 0.0653(14) 0.000 0.0082(12) 0.000 C1 0.146(11) 0.135(9) 0.118(8) 0.030(7) 0.002(7) -0.017(8) O2 0.086(6) 0.112(7) 0.105(6) 0.013(5) 0.039(5) 0.009(5) S2 0.097(3) 0.089(2) 0.111(3) 0.0162(18) 0.0383(19) 0.0082(17) O2B 0.076(9) 0.073(8) 0.094(8) 0.007(6) 0.003(7) -0.011(7) S2B 0.104(5) 0.082(4) 0.088(4) -0.002(3) 0.031(3) 0.000(3) C2 0.163(14) 0.157(12) 0.171(13) -0.061(10) 0.069(10) -0.025(10) C3 0.131(11) 0.175(13) 0.150(11) -0.027(10) -0.020(8) 0.033(9) S3 0.095(2) 0.096(2) 0.0870(19) 0.000 0.0156(16) 0.000 O30 0.060(10) 0.50(4) 0.197(18) 0.000 -0.001(9) 0.000 O31 0.237(15) 0.229(13) 0.285(17) -0.157(13) -0.037(13) 0.028(11) C30 0.124(17) 0.170(18) 0.103(11) 0.000 0.035(10) 0.000 F30 0.139(12) 0.168(13) 0.135(11) -0.095(10) -0.022(9) 0.018(9) F31 0.086(13) 0.127(16) 0.149(16) 0.000 0.021(10) 0.000 F30B 0.145(11) 0.175(11) 0.133(11) 0.000 0.021(8) 0.000 F31B 0.207(14) 0.226(14) 0.223(14) 0.007(10) 0.030(9) -0.030(10) _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 Re C4 1.834(13) . ? Re C4 1.834(13) 4_575 ? Re C5 1.876(12) . ? Re O2 2.110(12) 4_575 ? Re O2 2.110(12) . ? Re O1 2.168(8) . ? Re O2B 2.19(2) 4_575 ? Re O2B 2.19(2) . ? C4 O4 1.196(15) . ? C5 O5 1.142(15) . ? O1 S1 1.535(9) . ? S1 C1 1.736(11) . ? S1 C1 1.736(11) 4_575 ? O2 S2 1.550(12) . ? S2 C2 1.730(14) . ? S2 C3 1.816(13) . ? O2B S2B 1.477(19) . ? S2B C3 1.731(15) . ? S2B C2 1.824(13) . ? S3 O31 1.293(11) 4_565 ? S3 O31 1.293(11) . ? S3 O30 1.30(2) . ? S3 C30 1.80(2) . ? C30 F30B 1.21(3) . ? C30 F31B 1.25(3) . ? C30 F31B 1.25(3) 4_565 ? C30 F30 1.364(14) . ? C30 F30 1.364(14) 4_565 ? C30 F31 1.40(3) . ? F30 F30B 1.30(2) . ? F30 F31B 1.40(3) . ? F31 F31B 0.94(3) 4_565 ? F31 F31B 0.94(3) . ? F30B F30 1.30(2) 4_565 ? F31B F31B 1.65(5) 4_565 ? 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 C4 Re C4 89.5(9) . 4_575 ? C4 Re C5 87.3(5) . . ? C4 Re C5 87.3(5) 4_575 . ? C4 Re O2 171.6(4) . 4_575 ? C4 Re O2 87.4(7) 4_575 4_575 ? C5 Re O2 100.4(4) . 4_575 ? C4 Re O2 87.4(7) . . ? C4 Re O2 171.6(4) 4_575 . ? C5 Re O2 100.4(4) . . ? O2 Re O2 94.5(7) 4_575 . ? C4 Re O1 95.0(4) . . ? C4 Re O1 95.0(4) 4_575 . ? C5 Re O1 176.7(5) . . ? O2 Re O1 77.4(3) 4_575 . ? O2 Re O1 77.4(3) . . ? C4 Re O2B 163.5(6) . 4_575 ? C4 Re O2B 106.5(7) 4_575 4_575 ? C5 Re O2B 89.6(7) . 4_575 ? O2 Re O2B 22.3(4) 4_575 4_575 ? O2 Re O2B 77.2(7) . 4_575 ? O1 Re O2B 87.5(6) . 4_575 ? C4 Re O2B 106.5(7) . . ? C4 Re O2B 163.5(6) 4_575 . ? C5 Re O2B 89.6(7) . . ? O2 Re O2B 77.2(7) 4_575 . ? O2 Re O2B 22.3(4) . . ? O1 Re O2B 87.5(6) . . ? O2B Re O2B 57.3(9) 4_575 . ? O4 C4 Re 177.6(11) . . ? O5 C5 Re 178.3(15) . . ? S1 O1 Re 121.7(6) . . ? O1 S1 C1 103.6(5) . . ? O1 S1 C1 103.6(5) . 4_575 ? C1 S1 C1 96.6(10) . 4_575 ? S2 O2 Re 123.6(6) . . ? O2 S2 C2 103.0(8) . . ? O2 S2 C3 102.6(7) . . ? C2 S2 C3 95.4(8) . . ? S2B O2B Re 127.6(12) . . ? O2B S2B C3 95.4(10) . . ? O2B S2B C2 111.2(10) . . ? C3 S2B C2 95.1(8) . . ? S2 C2 S2B 39.8(4) . . ? S2B C3 S2 39.9(4) . . ? O31 S3 O31 112.7(19) 4_565 . ? O31 S3 O30 114.8(9) 4_565 . ? O31 S3 O30 114.8(9) . . ? O31 S3 C30 103.9(8) 4_565 . ? O31 S3 C30 103.9(8) . . ? O30 S3 C30 105.2(10) . . ? F30B C30 F31B 118(2) . . ? F30B C30 F31B 118(2) . 4_565 ? F31B C30 F31B 82(3) . 4_565 ? F30B C30 F30 60.4(12) . . ? F31B C30 F30 64.7(15) . . ? F31B C30 F30 134(2) 4_565 . ? F30B C30 F30 60.4(12) . 4_565 ? F31B C30 F30 134(2) . 4_565 ? F31B C30 F30 64.7(15) 4_565 4_565 ? F30 C30 F30 117(2) . 4_565 ? F30B C30 F31 129(2) . . ? F31B C30 F31 41.2(17) . . ? F31B C30 F31 41.2(17) 4_565 . ? F30 C30 F31 100.4(14) . . ? F30 C30 F31 100.4(14) 4_565 . ? F30B C30 S3 114(2) . . ? F31B C30 S3 109.5(18) . . ? F31B C30 S3 109.5(18) 4_565 . ? F30 C30 S3 111.1(11) . . ? F30 C30 S3 111.1(11) 4_565 . ? F31 C30 S3 116.3(15) . . ? F30B F30 C30 53.9(13) . . ? F30B F30 F31B 102.7(19) . . ? C30 F30 F31B 53.8(13) . . ? F31B F31 F31B 122(5) 4_565 . ? F31B F31 C30 61(3) 4_565 . ? F31B F31 C30 61(3) . . ? C30 F30B F30 65.7(13) . . ? C30 F30B F30 65.7(13) . 4_565 ? F30 F30B F30 127(3) . 4_565 ? F31 F31B C30 78(3) . . ? F31 F31B F30 128(4) . . ? C30 F31B F30 61.6(17) . . ? F31 F31B F31B 29(3) . 4_565 ? C30 F31B F31B 48.8(17) . 4_565 ? F30 F31B F31B 104.0(15) . 4_565 ? 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 C4 Re C4 O4 -101(34) 4_575 . . . ? C5 Re C4 O4 172(34) . . . . ? O2 Re C4 O4 -32(36) 4_575 . . . ? O2 Re C4 O4 72(34) . . . . ? O1 Re C4 O4 -6(34) . . . . ? O2B Re C4 O4 93(34) 4_575 . . . ? O2B Re C4 O4 83(34) . . . . ? C4 Re C5 O5 44.8(5) . . . . ? C4 Re C5 O5 -44.8(5) 4_575 . . . ? O2 Re C5 O5 -131.7(4) 4_575 . . . ? O2 Re C5 O5 131.7(4) . . . . ? O1 Re C5 O5 180.00(4) . . . . ? O2B Re C5 O5 -151.4(5) 4_575 . . . ? O2B Re C5 O5 151.4(5) . . . . ? C4 Re O1 S1 135.0(5) . . . . ? C4 Re O1 S1 -135.0(5) 4_575 . . . ? C5 Re O1 S1 0.000(10) . . . . ? O2 Re O1 S1 -48.8(4) 4_575 . . . ? O2 Re O1 S1 48.8(4) . . . . ? O2B Re O1 S1 -28.7(5) 4_575 . . . ? O2B Re O1 S1 28.7(5) . . . . ? Re O1 S1 C1 -129.8(5) . . . . ? Re O1 S1 C1 129.8(5) . . . 4_575 ? C4 Re O2 S2 114.2(9) . . . . ? C4 Re O2 S2 -177(3) 4_575 . . . ? C5 Re O2 S2 27.3(10) . . . . ? O2 Re O2 S2 -74.1(9) 4_575 . . . ? O1 Re O2 S2 -150.1(9) . . . . ? O2B Re O2 S2 -59.8(8) 4_575 . . . ? O2B Re O2 S2 -34.9(14) . . . . ? Re O2 S2 C2 -123.3(9) . . . . ? Re O2 S2 C3 138.1(8) . . . . ? C4 Re O2B S2B -28.3(16) . . . . ? C4 Re O2B S2B 165.5(14) 4_575 . . . ? C5 Re O2B S2B -115.4(14) . . . . ? O2 Re O2B S2B 143.9(16) 4_575 . . . ? O2 Re O2B S2B 4.1(8) . . . . ? O1 Re O2B S2B 66.2(14) . . . . ? O2B Re O2B S2B 154.9(11) 4_575 . . . ? Re O2B S2B C3 -163.7(13) . . . . ? Re O2B S2B C2 98.7(15) . . . . ? O2 S2 C2 S2B -40.7(6) . . . . ? C3 S2 C2 S2B 63.5(7) . . . . ? O2B S2B C2 S2 28.1(10) . . . . ? C3 S2B C2 S2 -69.7(7) . . . . ? O2B S2B C3 S2 -48.8(9) . . . . ? C2 S2B C3 S2 63.1(6) . . . . ? O2 S2 C3 S2B 34.4(7) . . . . ? C2 S2 C3 S2B -70.2(7) . . . . ? O31 S3 C30 F30B -121.0(10) 4_565 . . . ? O31 S3 C30 F30B 121.0(10) . . . . ? O30 S3 C30 F30B 0.000(4) . . . . ? O31 S3 C30 F31B 15(2) 4_565 . . . ? O31 S3 C30 F31B -103(2) . . . . ? O30 S3 C30 F31B 135.6(19) . . . . ? O31 S3 C30 F31B 103(2) 4_565 . . 4_565 ? O31 S3 C30 F31B -15(2) . . . 4_565 ? O30 S3 C30 F31B -135.6(19) . . . 4_565 ? O31 S3 C30 F30 -54.9(19) 4_565 . . . ? O31 S3 C30 F30 -173.0(17) . . . . ? O30 S3 C30 F30 66.1(15) . . . . ? O31 S3 C30 F30 173.0(17) 4_565 . . 4_565 ? O31 S3 C30 F30 54.9(19) . . . 4_565 ? O30 S3 C30 F30 -66.1(15) . . . 4_565 ? O31 S3 C30 F31 59.0(10) 4_565 . . . ? O31 S3 C30 F31 -59.0(10) . . . . ? O30 S3 C30 F31 180.000(3) . . . . ? F31B C30 F30 F30B 151(3) . . . . ? F31B C30 F30 F30B 102(3) 4_565 . . . ? F30 C30 F30 F30B 22(2) 4_565 . . . ? F31 C30 F30 F30B 129(2) . . . . ? S3 C30 F30 F30B -107(2) . . . . ? F30B C30 F30 F31B -151(3) . . . . ? F31B C30 F30 F31B -49(3) 4_565 . . . ? F30 C30 F30 F31B -129(3) 4_565 . . . ? F31 C30 F30 F31B -21(2) . . . . ? S3 C30 F30 F31B 102.3(19) . . . . ? F30B C30 F31 F31B -90(3) . . . 4_565 ? F31B C30 F31 F31B -180(6) . . . 4_565 ? F30 C30 F31 F31B -150(3) . . . 4_565 ? F30 C30 F31 F31B -30(3) 4_565 . . 4_565 ? S3 C30 F31 F31B 90(3) . . . 4_565 ? F30B C30 F31 F31B 90(3) . . . . ? F31B C30 F31 F31B 180(6) 4_565 . . . ? F30 C30 F31 F31B 30(3) . . . . ? F30 C30 F31 F31B 150(3) 4_565 . . . ? S3 C30 F31 F31B -90(3) . . . . ? F31B C30 F30B F30 -30(3) . . . . ? F31B C30 F30B F30 -127(3) 4_565 . . . ? F30 C30 F30B F30 -157(2) 4_565 . . . ? F31 C30 F30B F30 -78.7(12) . . . . ? S3 C30 F30B F30 101.3(12) . . . . ? F31B C30 F30B F30 127(3) . . . 4_565 ? F31B C30 F30B F30 30(3) 4_565 . . 4_565 ? F30 C30 F30B F30 157(2) . . . 4_565 ? F31 C30 F30B F30 78.7(12) . . . 4_565 ? S3 C30 F30B F30 -101.3(12) . . . 4_565 ? F31B F30 F30B C30 24(2) . . . . ? C30 F30 F30B F30 -26(2) . . . 4_565 ? F31B F30 F30B F30 -2(4) . . . 4_565 ? F31B F31 F31B C30 0(6) 4_565 . . . ? F31B F31 F31B F30 -37(8) 4_565 . . . ? C30 F31 F31B F30 -37(3) . . . . ? C30 F31 F31B F31B 0(6) . . . 4_565 ? F30B C30 F31B F31 -118(3) . . . . ? F31B C30 F31B F31 0(4) 4_565 . . . ? F30 C30 F31B F31 -147(3) . . . . ? F30 C30 F31B F31 -43(4) 4_565 . . . ? S3 C30 F31B F31 108(3) . . . . ? F30B C30 F31B F30 29(2) . . . . ? F31B C30 F31B F30 147.1(17) 4_565 . . . ? F30 C30 F31B F30 104(3) 4_565 . . . ? F31 C30 F31B F30 147(3) . . . . ? S3 C30 F31B F30 -104.8(13) . . . . ? F30B C30 F31B F31B -118(3) . . . 4_565 ? F30 C30 F31B F31B -147.1(17) . . . 4_565 ? F30 C30 F31B F31B -43(2) 4_565 . . 4_565 ? F31 C30 F31B F31B 0(4) . . . 4_565 ? S3 C30 F31B F31B 108(2) . . . 4_565 ? F30B F30 F31B F31 19(5) . . . . ? C30 F30 F31B F31 42(4) . . . . ? F30B F30 F31B C30 -24(2) . . . . ? F30B F30 F31B F31B 0.9(17) . . . 4_565 ? C30 F30 F31B F31B 24.9(13) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 1.222 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.152 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 614598' _audit_creation_method SHELXL-97 _chemical_name_systematic ; mer-tricarbonyl-(dimethylsulfoxide,O)-(2,2'-bipyridine)-rhenium(I) triflate ; _chemical_name_common ;mer-tricarbonyl-(dimethylsulfoxide,O)-(2,2'-bipyridine)- rhenium(i) triflate ; _chemical_melting_point ? _chemical_formula_moiety 'C15 H14 N2 O4 Re S 1+, C F3 O3 S 1-' _chemical_formula_sum 'C16 H14 F3 N2 O7 Re S2' _chemical_formula_weight 653.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 6.585(3) _cell_length_b 12.714(4) _cell_length_c 12.994(3) _cell_angle_alpha 79.43(2) _cell_angle_beta 80.06(3) _cell_angle_gamma 86.72(3) _cell_volume 1053.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 6.036 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.1256 _exptl_absorpt_correction_T_max 0.4457 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14864 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 30.58 _reflns_number_total 5799 _reflns_number_gt 4785 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (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^)+(0.0582P)^2^] 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 5799 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 Re Re 0.39543(3) 0.749448(15) 0.379619(14) 0.04691(8) Uani 1 1 d . . . S1 S 0.3139(2) 0.96513(11) 0.21702(11) 0.0584(3) Uani 1 1 d . . . O4 O 0.2479(6) 0.8479(3) 0.2561(3) 0.0569(9) Uani 1 1 d . . . C14 C 0.1792(13) 1.0087(5) 0.1092(5) 0.0799(19) Uani 1 1 d . . . H14A H 0.2241 0.9665 0.0549 0.120 Uiso 1 1 calc R . . H14B H 0.2068 1.0827 0.0809 0.120 Uiso 1 1 calc R . . H14C H 0.0338 1.0006 0.1335 0.120 Uiso 1 1 calc R . . C15 C 0.1688(11) 1.0387(5) 0.3116(5) 0.0717(16) Uani 1 1 d . . . H15A H 0.2612 1.0671 0.3486 0.108 Uiso 1 1 calc R . . H15B H 0.0744 0.9920 0.3615 0.108 Uiso 1 1 calc R . . H15C H 0.0931 1.0964 0.2753 0.108 Uiso 1 1 calc R . . C11 C 0.5556(10) 0.8574(5) 0.4133(5) 0.0629(14) Uani 1 1 d . . . C12 C 0.1749(10) 0.7757(5) 0.4909(5) 0.0618(13) Uani 1 1 d . . . C13 C 0.5180(9) 0.6515(5) 0.4813(5) 0.0573(12) Uani 1 1 d . . . O1 O 0.6551(9) 0.9182(4) 0.4353(4) 0.0865(15) Uani 1 1 d . . . O2 O 0.0422(8) 0.7902(5) 0.5563(4) 0.0884(15) Uani 1 1 d . . . O3 O 0.5924(7) 0.5908(4) 0.5434(3) 0.0728(12) Uani 1 1 d . . . N1 N 0.2499(6) 0.6257(3) 0.3249(3) 0.0450(8) Uani 1 1 d . . . N2 N 0.6123(6) 0.7111(3) 0.2449(3) 0.0467(8) Uani 1 1 d . . . C1 C 0.0629(8) 0.5851(4) 0.3699(4) 0.0518(11) Uani 1 1 d . . . H1 H -0.0135 0.6140 0.4257 0.062 Uiso 1 1 calc R . . C2 C -0.0170(8) 0.5033(5) 0.3360(5) 0.0595(13) Uani 1 1 d . . . H2 H -0.1455 0.4769 0.3686 0.071 Uiso 1 1 calc R . . C3 C 0.0942(9) 0.4603(5) 0.2533(5) 0.0604(13) Uani 1 1 d . . . H3 H 0.0431 0.4039 0.2297 0.072 Uiso 1 1 calc R . . C4 C 0.2825(8) 0.5022(4) 0.2061(4) 0.0552(11) Uani 1 1 d . . . H4 H 0.3597 0.4745 0.1497 0.066 Uiso 1 1 calc R . . C5 C 0.3568(7) 0.5851(4) 0.2422(4) 0.0440(9) Uani 1 1 d . . . C6 C 0.5598(7) 0.6337(4) 0.1968(4) 0.0462(9) Uani 1 1 d . . . C7 C 0.6886(8) 0.6018(5) 0.1110(4) 0.0559(12) Uani 1 1 d . . . H7 H 0.6508 0.5475 0.0795 0.067 Uiso 1 1 calc R . . C8 C 0.8747(9) 0.6525(5) 0.0731(4) 0.0640(14) Uani 1 1 d . . . H8 H 0.9623 0.6334 0.0149 0.077 Uiso 1 1 calc R . . C9 C 0.9281(9) 0.7304(5) 0.1219(5) 0.0651(14) Uani 1 1 d . . . H9 H 1.0535 0.7641 0.0979 0.078 Uiso 1 1 calc R . . C10 C 0.7954(8) 0.7588(5) 0.2067(5) 0.0581(12) Uani 1 1 d . . . H10 H 0.8326 0.8126 0.2391 0.070 Uiso 1 1 calc R . . S2 S 0.5637(2) 0.25395(12) 0.10084(12) 0.0580(3) Uani 1 1 d . . . O21 O 0.6383(9) 0.1657(5) 0.0498(5) 0.0965(17) Uani 1 1 d . . . O22 O 0.6400(7) 0.3566(4) 0.0472(4) 0.0706(11) Uani 1 1 d . . . O23 O 0.3466(6) 0.2542(4) 0.1426(4) 0.0733(12) Uani 1 1 d . . . C20 C 0.6870(10) 0.2318(6) 0.2177(6) 0.0718(16) Uani 1 1 d . . . F21 F 0.6341(8) 0.1405(5) 0.2804(4) 0.123(2) Uani 1 1 d . . . F22 F 0.8891(6) 0.2307(4) 0.1931(4) 0.0991(14) Uani 1 1 d . . . F23 F 0.6353(9) 0.3089(5) 0.2749(4) 0.1189(18) 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 Re 0.05294(12) 0.04387(11) 0.04409(11) -0.00798(7) -0.00966(7) 0.00321(7) S1 0.0685(8) 0.0487(7) 0.0579(7) -0.0070(6) -0.0130(6) -0.0006(5) O4 0.072(2) 0.0427(19) 0.059(2) -0.0066(16) -0.0242(17) 0.0029(16) C14 0.121(6) 0.057(4) 0.068(4) -0.004(3) -0.042(4) 0.001(3) C15 0.090(4) 0.055(3) 0.070(4) -0.015(3) -0.016(3) 0.015(3) C11 0.068(4) 0.064(4) 0.063(3) -0.012(3) -0.027(3) 0.001(3) C12 0.068(3) 0.062(3) 0.059(3) -0.018(3) -0.018(2) 0.014(3) C13 0.058(3) 0.056(3) 0.058(3) -0.017(2) -0.007(2) 0.005(2) O1 0.099(4) 0.071(3) 0.103(4) -0.029(3) -0.038(3) -0.009(3) O2 0.081(3) 0.109(4) 0.073(3) -0.034(3) 0.006(2) 0.018(3) O3 0.082(3) 0.074(3) 0.061(2) -0.004(2) -0.024(2) 0.021(2) N1 0.048(2) 0.043(2) 0.044(2) -0.0044(15) -0.0106(15) 0.0006(15) N2 0.046(2) 0.045(2) 0.047(2) -0.0028(16) -0.0065(15) -0.0002(15) C1 0.047(2) 0.053(3) 0.051(3) -0.002(2) -0.0037(19) -0.0010(19) C2 0.045(3) 0.066(3) 0.063(3) 0.001(3) -0.007(2) -0.014(2) C3 0.058(3) 0.056(3) 0.071(4) -0.015(3) -0.013(2) -0.010(2) C4 0.059(3) 0.050(3) 0.057(3) -0.012(2) -0.008(2) -0.002(2) C5 0.046(2) 0.043(2) 0.043(2) -0.0052(17) -0.0081(16) 0.0007(16) C6 0.046(2) 0.050(3) 0.042(2) -0.0044(18) -0.0095(17) -0.0004(18) C7 0.058(3) 0.063(3) 0.047(3) -0.010(2) -0.010(2) 0.000(2) C8 0.060(3) 0.080(4) 0.046(3) -0.009(3) 0.004(2) 0.002(3) C9 0.058(3) 0.070(4) 0.059(3) 0.000(3) 0.005(2) -0.010(3) C10 0.052(3) 0.060(3) 0.061(3) -0.007(2) -0.005(2) -0.008(2) S2 0.0578(7) 0.0610(8) 0.0550(7) -0.0140(6) -0.0036(5) -0.0048(5) O21 0.111(4) 0.079(3) 0.103(4) -0.046(3) 0.007(3) -0.009(3) O22 0.074(3) 0.063(3) 0.069(3) -0.001(2) -0.007(2) -0.0050(19) O23 0.047(2) 0.096(3) 0.073(3) -0.003(2) -0.0123(17) -0.0094(19) C20 0.067(4) 0.069(4) 0.076(4) 0.002(3) -0.017(3) -0.008(3) F21 0.109(4) 0.129(5) 0.117(4) 0.050(3) -0.049(3) -0.038(3) F22 0.059(2) 0.101(3) 0.138(4) -0.004(3) -0.039(2) 0.000(2) F23 0.130(4) 0.155(5) 0.093(3) -0.058(3) -0.049(3) 0.027(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re C13 1.897(6) . ? Re C12 1.925(6) . ? Re C11 1.932(6) . ? Re N2 2.171(4) . ? Re N1 2.172(4) . ? Re O4 2.179(4) . ? S1 O4 1.545(4) . ? S1 C14 1.773(7) . ? S1 C15 1.792(6) . ? C11 O1 1.145(8) . ? C12 O2 1.141(7) . ? C13 O3 1.163(7) . ? N1 C5 1.349(6) . ? N1 C1 1.355(6) . ? N2 C6 1.348(6) . ? N2 C10 1.355(7) . ? C1 C2 1.365(8) . ? C2 C3 1.374(8) . ? C3 C4 1.375(7) . ? C4 C5 1.375(7) . ? C5 C6 1.485(6) . ? C6 C7 1.388(7) . ? C7 C8 1.388(8) . ? C8 C9 1.361(9) . ? C9 C10 1.374(8) . ? S2 O21 1.427(5) . ? S2 O22 1.436(4) . ? S2 O23 1.439(4) . ? S2 C20 1.813(7) . ? C20 F22 1.314(8) . ? C20 F21 1.317(8) . ? C20 F23 1.331(9) . ? 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 C13 Re C12 89.0(2) . . ? C13 Re C11 86.2(3) . . ? C12 Re C11 89.9(3) . . ? C13 Re N2 94.39(19) . . ? C12 Re N2 172.2(2) . . ? C11 Re N2 97.4(2) . . ? C13 Re N1 94.1(2) . . ? C12 Re N1 97.8(2) . . ? C11 Re N1 172.3(2) . . ? N2 Re N1 74.95(15) . . ? C13 Re O4 174.19(18) . . ? C12 Re O4 93.0(2) . . ? C11 Re O4 99.3(2) . . ? N2 Re O4 82.96(16) . . ? N1 Re O4 80.22(14) . . ? O4 S1 C14 103.3(3) . . ? O4 S1 C15 105.1(3) . . ? C14 S1 C15 99.2(4) . . ? S1 O4 Re 118.7(2) . . ? O1 C11 Re 177.2(6) . . ? O2 C12 Re 178.9(6) . . ? O3 C13 Re 179.4(6) . . ? C5 N1 C1 118.3(4) . . ? C5 N1 Re 117.1(3) . . ? C1 N1 Re 124.5(3) . . ? C6 N2 C10 118.3(4) . . ? C6 N2 Re 117.1(3) . . ? C10 N2 Re 124.7(4) . . ? N1 C1 C2 122.2(5) . . ? C1 C2 C3 119.4(5) . . ? C2 C3 C4 118.7(5) . . ? C5 C4 C3 120.0(5) . . ? N1 C5 C4 121.3(5) . . ? N1 C5 C6 115.3(4) . . ? C4 C5 C6 123.4(4) . . ? N2 C6 C7 121.8(5) . . ? N2 C6 C5 115.5(4) . . ? C7 C6 C5 122.7(5) . . ? C8 C7 C6 118.7(5) . . ? C9 C8 C7 119.5(5) . . ? C8 C9 C10 119.5(5) . . ? N2 C10 C9 122.2(6) . . ? O21 S2 O22 115.5(3) . . ? O21 S2 O23 115.3(3) . . ? O22 S2 O23 114.3(3) . . ? O21 S2 C20 103.3(4) . . ? O22 S2 C20 101.8(3) . . ? O23 S2 C20 104.2(3) . . ? F22 C20 F21 107.6(6) . . ? F22 C20 F23 106.6(6) . . ? F21 C20 F23 107.1(7) . . ? F22 C20 S2 112.1(5) . . ? F21 C20 S2 111.9(5) . . ? F23 C20 S2 111.3(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 C14 S1 O4 Re 173.7(3) . . . . ? C15 S1 O4 Re -82.8(3) . . . . ? C13 Re O4 S1 -153.0(17) . . . . ? C12 Re O4 S1 96.8(3) . . . . ? C11 Re O4 S1 6.5(3) . . . . ? N2 Re O4 S1 -89.9(3) . . . . ? N1 Re O4 S1 -165.8(3) . . . . ? C13 Re C11 O1 14(13) . . . . ? C12 Re C11 O1 103(13) . . . . ? N2 Re C11 O1 -80(13) . . . . ? N1 Re C11 O1 -78(14) . . . . ? O4 Re C11 O1 -164(13) . . . . ? C13 Re C12 O2 -98(34) . . . . ? C11 Re C12 O2 176(100) . . . . ? N2 Re C12 O2 18(35) . . . . ? N1 Re C12 O2 -4(34) . . . . ? O4 Re C12 O2 77(34) . . . . ? C12 Re C13 O3 100(56) . . . . ? C11 Re C13 O3 -170(100) . . . . ? N2 Re C13 O3 -73(56) . . . . ? N1 Re C13 O3 2(56) . . . . ? O4 Re C13 O3 -11(57) . . . . ? C13 Re N1 C5 -91.8(4) . . . . ? C12 Re N1 C5 178.7(4) . . . . ? C11 Re N1 C5 0.2(16) . . . . ? N2 Re N1 C5 1.7(3) . . . . ? O4 Re N1 C5 87.0(3) . . . . ? C13 Re N1 C1 86.4(4) . . . . ? C12 Re N1 C1 -3.1(4) . . . . ? C11 Re N1 C1 178.4(14) . . . . ? N2 Re N1 C1 179.9(4) . . . . ? O4 Re N1 C1 -94.9(4) . . . . ? C13 Re N2 C6 91.9(4) . . . . ? C12 Re N2 C6 -23.8(16) . . . . ? C11 Re N2 C6 178.6(4) . . . . ? N1 Re N2 C6 -1.2(3) . . . . ? O4 Re N2 C6 -82.9(4) . . . . ? C13 Re N2 C10 -87.7(5) . . . . ? C12 Re N2 C10 156.5(14) . . . . ? C11 Re N2 C10 -1.0(5) . . . . ? N1 Re N2 C10 179.2(5) . . . . ? O4 Re N2 C10 97.5(4) . . . . ? C5 N1 C1 C2 1.8(8) . . . . ? Re N1 C1 C2 -176.4(4) . . . . ? N1 C1 C2 C3 -0.2(9) . . . . ? C1 C2 C3 C4 -0.8(9) . . . . ? C2 C3 C4 C5 0.4(9) . . . . ? C1 N1 C5 C4 -2.2(7) . . . . ? Re N1 C5 C4 176.1(4) . . . . ? C1 N1 C5 C6 179.8(4) . . . . ? Re N1 C5 C6 -1.9(5) . . . . ? C3 C4 C5 N1 1.1(8) . . . . ? C3 C4 C5 C6 179.0(5) . . . . ? C10 N2 C6 C7 0.6(7) . . . . ? Re N2 C6 C7 -179.0(4) . . . . ? C10 N2 C6 C5 -179.7(4) . . . . ? Re N2 C6 C5 0.7(5) . . . . ? N1 C5 C6 N2 0.8(6) . . . . ? C4 C5 C6 N2 -177.1(5) . . . . ? N1 C5 C6 C7 -179.5(5) . . . . ? C4 C5 C6 C7 2.5(8) . . . . ? N2 C6 C7 C8 -1.0(8) . . . . ? C5 C6 C7 C8 179.3(5) . . . . ? C6 C7 C8 C9 1.2(9) . . . . ? C7 C8 C9 C10 -1.0(10) . . . . ? C6 N2 C10 C9 -0.4(8) . . . . ? Re N2 C10 C9 179.2(5) . . . . ? C8 C9 C10 N2 0.6(10) . . . . ? O21 S2 C20 F22 60.0(6) . . . . ? O22 S2 C20 F22 -60.0(6) . . . . ? O23 S2 C20 F22 -179.2(5) . . . . ? O21 S2 C20 F21 -61.0(6) . . . . ? O22 S2 C20 F21 178.9(6) . . . . ? O23 S2 C20 F21 59.8(6) . . . . ? O21 S2 C20 F23 179.3(5) . . . . ? O22 S2 C20 F23 59.2(6) . . . . ? O23 S2 C20 F23 -59.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 30.58 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 1.761 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.166 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 614599' _audit_creation_method SHELXL-97 _chemical_name_systematic ; mer-tricarbonyl-(4,4'-bipyridine,N)-(2,2'-bipyridine,N,N')-rhenium(I) triflate dichloromethane diethylether ; _chemical_name_common ; mer-tricarbonyl-(4,4'-bipyridine,N)-(2,2'-bipyridine,N,N')- rhenium(i) triflate dichloromethane diethylether ; _chemical_melting_point ? _chemical_formula_moiety 'C23 H16 N4 O6 Re 1+, C F3 O3 S 1-, C H2 Cl2, 0.5(C4 H10 O)' _chemical_formula_sum 'C27 H23 Cl2 F3 N4 O6.50 Re S' _chemical_formula_weight 853.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 8.350(2) _cell_length_b 10.589(3) _cell_length_c 17.861(4) _cell_angle_alpha 93.86(2) _cell_angle_beta 99.75(2) _cell_angle_gamma 94.78(2) _cell_volume 1545.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 10.514 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'vertically mounted graphite crystal' _diffrn_measurement_device_type KappaCCD2000 _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 14 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16512 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 64.87 _reflns_number_total 4448 _reflns_number_gt 4248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Supergui (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (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^)+(0.0778P)^2^+3.1873P] 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 4448 _refine_ls_number_parameters 392 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.075 _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 Re Re 0.17494(3) 0.02611(2) 0.366313(14) 0.04070(15) Uani 1 1 d . . . N1 N 0.3752(6) -0.0600(5) 0.3266(3) 0.0418(11) Uani 1 1 d . . . N2 N 0.3275(6) 0.1819(5) 0.3330(3) 0.0424(11) Uani 1 1 d . . . N3 N 0.0567(6) 0.0037(5) 0.2460(3) 0.0433(11) Uani 1 1 d . . . N4 N -0.4121(14) -0.0801(9) -0.1289(4) 0.104(3) Uani 1 1 d . . . C1 C 0.3929(8) -0.1874(6) 0.3249(4) 0.0501(15) Uani 1 1 d . . . H1 H 0.3139 -0.2421 0.3415 0.060 Uiso 1 1 calc R . . C2 C 0.5217(9) -0.2377(6) 0.2999(4) 0.0555(16) Uani 1 1 d . . . H2 H 0.5296 -0.3258 0.2986 0.067 Uiso 1 1 calc R . . C3 C 0.6405(9) -0.1583(6) 0.2765(4) 0.0544(16) Uani 1 1 d . . . H3 H 0.7302 -0.1909 0.2592 0.065 Uiso 1 1 calc R . . C4 C 0.6230(8) -0.0289(6) 0.2793(4) 0.0485(14) Uani 1 1 d . . . H4 H 0.7018 0.0272 0.2636 0.058 Uiso 1 1 calc R . . C5 C 0.4908(7) 0.0180(5) 0.3049(3) 0.0406(12) Uani 1 1 d . . . C6 C 0.4637(7) 0.1537(5) 0.3084(3) 0.0422(13) Uani 1 1 d . . . C7 C 0.5685(8) 0.2477(6) 0.2875(4) 0.0505(15) Uani 1 1 d . . . H7 H 0.6652 0.2269 0.2713 0.061 Uiso 1 1 calc R . . C8 C 0.5312(9) 0.3714(7) 0.2906(5) 0.0599(18) Uani 1 1 d . . . H8 H 0.6021 0.4361 0.2769 0.072 Uiso 1 1 calc R . . C9 C 0.3895(10) 0.3990(7) 0.3137(5) 0.0634(19) Uani 1 1 d . . . H9 H 0.3603 0.4828 0.3145 0.076 Uiso 1 1 calc R . . C10 C 0.2897(9) 0.3042(6) 0.3358(4) 0.0531(16) Uani 1 1 d . . . H10 H 0.1940 0.3242 0.3532 0.064 Uiso 1 1 calc R . . C11 C -0.0038(9) 0.1013(6) 0.2102(4) 0.0537(16) Uani 1 1 d . . . H11 H 0.0155 0.1829 0.2361 0.064 Uiso 1 1 calc R . . C12 C -0.0921(10) 0.0880(6) 0.1378(4) 0.0607(18) Uani 1 1 d . . . H12 H -0.1323 0.1597 0.1156 0.073 Uiso 1 1 calc R . . C13 C -0.1231(8) -0.0298(6) 0.0966(4) 0.0495(14) Uani 1 1 d . . . C14 C -0.0591(9) -0.1299(6) 0.1337(4) 0.0565(17) Uani 1 1 d . . . H14 H -0.0768 -0.2123 0.1088 0.068 Uiso 1 1 calc R . . C15 C 0.0296(9) -0.1104(6) 0.2060(4) 0.0548(17) Uani 1 1 d . . . H15 H 0.0736 -0.1803 0.2288 0.066 Uiso 1 1 calc R . . C16 C -0.356(2) -0.1711(13) -0.0918(8) 0.133(5) Uani 1 1 d . . . H16 H -0.3853 -0.2538 -0.1153 0.160 Uiso 1 1 calc R . . C17 C -0.2567(18) -0.1608(11) -0.0207(7) 0.116(4) Uani 1 1 d . . . H17 H -0.2149 -0.2334 -0.0005 0.139 Uiso 1 1 calc R . . C18 C -0.2210(10) -0.0490(7) 0.0186(4) 0.0594(17) Uani 1 1 d . . . C19 C -0.2773(14) 0.0504(10) -0.0195(6) 0.097(3) Uani 1 1 d . . . H19 H -0.2510 0.1343 0.0025 0.116 Uiso 1 1 calc R . . C20 C -0.3744(16) 0.0258(12) -0.0917(7) 0.104(3) Uani 1 1 d . . . H20 H -0.4160 0.0963 -0.1148 0.125 Uiso 1 1 calc R . . O1 O -0.1016(7) 0.1747(6) 0.4103(3) 0.0708(14) Uani 1 1 d . . . O2 O -0.0188(7) -0.2137(5) 0.4050(3) 0.0686(14) Uani 1 1 d . . . O3 O 0.3440(7) 0.0614(6) 0.5338(3) 0.0686(14) Uani 1 1 d . . . C21 C 0.0062(9) 0.1213(7) 0.3945(4) 0.0550(17) Uani 1 1 d . . . C22 C 0.0515(9) -0.1265(7) 0.3900(4) 0.0540(16) Uani 1 1 d . . . C23 C 0.2835(9) 0.0465(6) 0.4710(4) 0.0511(16) Uani 1 1 d . . . S1 S 0.9481(2) 0.51886(17) 0.23631(16) 0.0749(6) Uani 1 1 d . . . O4 O 0.8078(8) 0.5913(5) 0.2279(5) 0.092(2) Uani 1 1 d . . . O5 O 0.9302(8) 0.4012(6) 0.2691(5) 0.103(3) Uani 1 1 d . . . O6 O 1.1010(8) 0.5936(6) 0.2600(6) 0.102(2) Uani 1 1 d . . . C24 C 0.9529(17) 0.4632(9) 0.1370(9) 0.117(4) Uani 1 1 d . . . F1 F 0.9681(15) 0.5560(7) 0.0951(5) 0.159(4) Uani 1 1 d . . . F2 F 0.8139(13) 0.3900(7) 0.1096(6) 0.163(4) Uani 1 1 d . . . F3 F 1.0773(12) 0.3920(6) 0.1361(6) 0.147(3) Uani 1 1 d . . . C25 C 0.2119(17) 0.5800(12) 0.4997(11) 0.137(6) Uani 1 1 d . . . H25A H 0.1477 0.6215 0.5336 0.164 Uiso 1 1 calc R . . H25B H 0.1455 0.5697 0.4485 0.164 Uiso 1 1 calc R . . Cl1 Cl 0.2398(5) 0.4347(3) 0.5281(2) 0.1222(11) Uani 1 1 d . . . Cl2 Cl 0.3815(4) 0.6817(3) 0.49681(19) 0.1102(10) Uani 1 1 d . . . O7 O 0.5000 0.5000 0.0000 0.120(4) Uiso 1 2 d S . 1 C26 C 0.570(4) 0.506(3) -0.0585(17) 0.132(9) Uiso 0.50 1 d PD A 1 C27 C 0.601(3) 0.394(2) -0.1049(12) 0.169(7) Uiso 1 1 d D A 1 C26A C 0.502(4) 0.396(3) -0.0445(17) 0.138(10) Uiso 0.50 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.03953(19) 0.03795(19) 0.0432(2) 0.00533(12) 0.00257(12) 0.00368(11) N1 0.046(3) 0.037(3) 0.042(3) 0.003(2) 0.006(2) 0.009(2) N2 0.042(3) 0.037(3) 0.048(3) 0.007(2) 0.007(2) -0.001(2) N3 0.043(3) 0.035(2) 0.052(3) 0.011(2) 0.003(2) 0.003(2) N4 0.146(8) 0.102(6) 0.055(4) -0.006(4) -0.022(5) 0.048(6) C1 0.053(4) 0.035(3) 0.059(4) 0.003(3) 0.001(3) 0.001(3) C2 0.063(4) 0.036(3) 0.066(4) 0.002(3) 0.004(3) 0.009(3) C3 0.055(4) 0.050(4) 0.058(4) 0.002(3) 0.006(3) 0.015(3) C4 0.052(3) 0.046(3) 0.048(4) 0.006(3) 0.007(3) 0.009(3) C5 0.040(3) 0.037(3) 0.042(3) 0.005(2) -0.001(2) 0.001(2) C6 0.044(3) 0.037(3) 0.042(3) 0.004(2) -0.001(2) 0.002(2) C7 0.049(3) 0.046(3) 0.055(4) 0.010(3) 0.008(3) -0.002(3) C8 0.055(4) 0.043(3) 0.080(5) 0.008(3) 0.010(3) -0.002(3) C9 0.067(4) 0.038(3) 0.084(5) 0.004(3) 0.010(4) 0.008(3) C10 0.055(4) 0.032(3) 0.071(5) 0.002(3) 0.008(3) 0.004(3) C11 0.070(4) 0.036(3) 0.050(4) 0.001(3) -0.005(3) 0.007(3) C12 0.081(5) 0.040(3) 0.060(4) 0.012(3) 0.000(4) 0.015(3) C13 0.050(3) 0.048(3) 0.052(4) 0.010(3) 0.009(3) 0.007(3) C14 0.074(4) 0.039(3) 0.052(4) 0.005(3) -0.004(3) 0.007(3) C15 0.068(4) 0.034(3) 0.057(4) 0.009(3) -0.006(3) 0.009(3) C16 0.171(9) 0.105(7) 0.102(7) -0.017(6) -0.045(6) 0.047(7) C17 0.158(8) 0.085(6) 0.087(6) -0.011(5) -0.038(6) 0.049(6) C18 0.066(4) 0.057(4) 0.054(4) 0.006(3) 0.002(3) 0.016(3) C19 0.118(7) 0.077(5) 0.082(6) 0.016(4) -0.028(5) 0.011(5) C20 0.121(7) 0.094(6) 0.088(6) 0.023(5) -0.019(5) 0.019(6) O1 0.060(3) 0.074(3) 0.082(4) -0.001(3) 0.017(3) 0.025(3) O2 0.068(3) 0.055(3) 0.081(4) 0.023(3) 0.010(3) -0.013(3) O3 0.069(3) 0.086(4) 0.044(3) 0.003(2) -0.004(2) 0.003(3) C21 0.052(4) 0.057(4) 0.052(4) 0.000(3) -0.001(3) 0.004(3) C22 0.055(4) 0.061(4) 0.046(4) 0.008(3) 0.005(3) 0.012(3) C23 0.051(4) 0.049(4) 0.049(4) 0.001(3) -0.002(3) 0.005(3) S1 0.0569(10) 0.0385(9) 0.1290(19) 0.0110(10) 0.0115(11) 0.0090(7) O4 0.069(4) 0.054(3) 0.153(6) 0.012(4) 0.013(4) 0.022(3) O5 0.071(4) 0.060(4) 0.183(8) 0.043(4) 0.024(4) 0.016(3) O6 0.063(4) 0.055(3) 0.181(8) -0.002(4) 0.006(4) 0.002(3) C24 0.127(10) 0.045(5) 0.176(13) 0.007(6) 0.015(9) 0.023(6) F1 0.264(11) 0.083(5) 0.149(7) 0.022(4) 0.067(7) 0.065(6) F2 0.176(8) 0.080(4) 0.203(9) -0.032(5) -0.044(7) 0.028(5) F3 0.181(8) 0.076(4) 0.207(9) 0.009(5) 0.081(7) 0.056(5) C25 0.109(9) 0.084(8) 0.226(18) 0.025(9) 0.042(10) 0.017(7) Cl1 0.145(3) 0.0873(18) 0.130(3) 0.0170(17) 0.017(2) -0.0007(18) Cl2 0.0938(18) 0.123(2) 0.109(2) 0.0401(17) 0.0046(15) -0.0119(16) _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 Re C21 1.914(8) . ? Re C23 1.925(7) . ? Re C22 1.953(8) . ? Re N1 2.168(5) . ? Re N2 2.176(5) . ? Re N3 2.196(5) . ? N1 C5 1.343(8) . ? N1 C1 1.368(8) . ? N2 C6 1.336(8) . ? N2 C10 1.358(8) . ? N3 C11 1.342(8) . ? N3 C15 1.343(8) . ? N4 C20 1.252(14) . ? N4 C16 1.282(15) . ? C1 C2 1.366(10) . ? C2 C3 1.384(11) . ? C3 C4 1.388(9) . ? C4 C5 1.381(9) . ? C5 C6 1.472(8) . ? C6 C7 1.382(9) . ? C7 C8 1.371(10) . ? C8 C9 1.365(11) . ? C9 C10 1.372(11) . ? C11 C12 1.368(10) . ? C12 C13 1.387(10) . ? C13 C14 1.384(9) . ? C13 C18 1.482(10) . ? C14 C15 1.370(10) . ? C16 C17 1.385(15) . ? C17 C18 1.320(13) . ? C18 C19 1.365(12) . ? C19 C20 1.397(14) . ? O1 C21 1.166(9) . ? O2 C22 1.125(9) . ? O3 C23 1.143(8) . ? S1 O5 1.419(7) . ? S1 O6 1.428(7) . ? S1 O4 1.446(6) . ? S1 C24 1.839(16) . ? C24 F1 1.285(15) . ? C24 F3 1.335(14) . ? C24 F2 1.339(15) . ? C25 Cl1 1.675(13) . ? C25 Cl2 1.716(14) . ? O7 C26 1.28(3) 2_665 ? O7 C26 1.28(3) . ? C26 C27 1.461(18) . ? 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 C21 Re C23 89.0(3) . . ? C21 Re C22 87.7(3) . . ? C23 Re C22 88.3(3) . . ? C21 Re N1 172.4(3) . . ? C23 Re N1 93.6(3) . . ? C22 Re N1 99.5(3) . . ? C21 Re N2 98.5(3) . . ? C23 Re N2 93.6(3) . . ? C22 Re N2 173.5(2) . . ? N1 Re N2 74.27(19) . . ? C21 Re N3 92.1(3) . . ? C23 Re N3 178.7(2) . . ? C22 Re N3 92.6(2) . . ? N1 Re N3 85.3(2) . . ? N2 Re N3 85.41(19) . . ? C5 N1 C1 118.6(5) . . ? C5 N1 Re 117.3(4) . . ? C1 N1 Re 124.0(4) . . ? C6 N2 C10 119.5(5) . . ? C6 N2 Re 117.4(4) . . ? C10 N2 Re 123.1(5) . . ? C11 N3 C15 116.2(6) . . ? C11 N3 Re 121.8(4) . . ? C15 N3 Re 121.8(4) . . ? C20 N4 C16 112.1(9) . . ? C2 C1 N1 122.1(6) . . ? C1 C2 C3 119.7(6) . . ? C2 C3 C4 118.0(6) . . ? C5 C4 C3 120.5(6) . . ? N1 C5 C4 121.1(5) . . ? N1 C5 C6 115.5(5) . . ? C4 C5 C6 123.3(6) . . ? N2 C6 C7 120.9(6) . . ? N2 C6 C5 115.3(5) . . ? C7 C6 C5 123.8(6) . . ? C8 C7 C6 119.8(7) . . ? C9 C8 C7 119.0(7) . . ? C8 C9 C10 119.9(7) . . ? N2 C10 C9 120.9(7) . . ? N3 C11 C12 123.2(6) . . ? C11 C12 C13 120.9(6) . . ? C14 C13 C12 115.6(6) . . ? C14 C13 C18 121.7(6) . . ? C12 C13 C18 122.7(6) . . ? C15 C14 C13 120.9(6) . . ? N3 C15 C14 123.2(6) . . ? N4 C16 C17 127.1(12) . . ? C18 C17 C16 120.0(10) . . ? C17 C18 C19 114.3(8) . . ? C17 C18 C13 123.8(7) . . ? C19 C18 C13 121.8(7) . . ? C18 C19 C20 119.2(10) . . ? N4 C20 C19 127.0(10) . . ? O1 C21 Re 177.0(7) . . ? O2 C22 Re 178.8(7) . . ? O3 C23 Re 177.6(6) . . ? O5 S1 O6 116.3(5) . . ? O5 S1 O4 116.4(4) . . ? O6 S1 O4 114.4(4) . . ? O5 S1 C24 100.8(5) . . ? O6 S1 C24 103.6(6) . . ? O4 S1 C24 102.1(5) . . ? F1 C24 F3 109.7(13) . . ? F1 C24 F2 109.8(13) . . ? F3 C24 F2 108.3(9) . . ? F1 C24 S1 112.0(8) . . ? F3 C24 S1 108.7(10) . . ? F2 C24 S1 108.1(11) . . ? Cl1 C25 Cl2 118.1(8) . . ? C26 O7 C26 180(3) 2_665 . ? O7 C26 C27 124(2) . . ? 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 C21 Re N1 C5 19.1(19) . . . . ? C23 Re N1 C5 -90.6(5) . . . . ? C22 Re N1 C5 -179.5(5) . . . . ? N2 Re N1 C5 2.1(4) . . . . ? N3 Re N1 C5 88.7(4) . . . . ? C21 Re N1 C1 -163.1(16) . . . . ? C23 Re N1 C1 87.2(5) . . . . ? C22 Re N1 C1 -1.7(5) . . . . ? N2 Re N1 C1 179.9(5) . . . . ? N3 Re N1 C1 -93.5(5) . . . . ? C21 Re N2 C6 -179.8(5) . . . . ? C23 Re N2 C6 90.7(5) . . . . ? C22 Re N2 C6 -16(2) . . . . ? N1 Re N2 C6 -2.0(4) . . . . ? N3 Re N2 C6 -88.4(5) . . . . ? C21 Re N2 C10 -0.2(6) . . . . ? C23 Re N2 C10 -89.7(6) . . . . ? C22 Re N2 C10 163.2(19) . . . . ? N1 Re N2 C10 177.6(6) . . . . ? N3 Re N2 C10 91.2(5) . . . . ? C21 Re N3 C11 45.1(6) . . . . ? C23 Re N3 C11 -94(9) . . . . ? C22 Re N3 C11 132.9(6) . . . . ? N1 Re N3 C11 -127.8(6) . . . . ? N2 Re N3 C11 -53.3(5) . . . . ? C21 Re N3 C15 -129.7(6) . . . . ? C23 Re N3 C15 91(9) . . . . ? C22 Re N3 C15 -41.9(6) . . . . ? N1 Re N3 C15 57.5(5) . . . . ? N2 Re N3 C15 132.0(6) . . . . ? C5 N1 C1 C2 -1.8(10) . . . . ? Re N1 C1 C2 -179.6(5) . . . . ? N1 C1 C2 C3 1.0(11) . . . . ? C1 C2 C3 C4 -0.2(10) . . . . ? C2 C3 C4 C5 0.1(10) . . . . ? C1 N1 C5 C4 1.7(9) . . . . ? Re N1 C5 C4 179.6(4) . . . . ? C1 N1 C5 C6 -179.9(5) . . . . ? Re N1 C5 C6 -1.9(7) . . . . ? C3 C4 C5 N1 -0.9(10) . . . . ? C3 C4 C5 C6 -179.2(6) . . . . ? C10 N2 C6 C7 1.6(9) . . . . ? Re N2 C6 C7 -178.8(5) . . . . ? C10 N2 C6 C5 -177.9(6) . . . . ? Re N2 C6 C5 1.7(7) . . . . ? N1 C5 C6 N2 0.1(8) . . . . ? C4 C5 C6 N2 178.5(6) . . . . ? N1 C5 C6 C7 -179.3(6) . . . . ? C4 C5 C6 C7 -0.9(9) . . . . ? N2 C6 C7 C8 -1.3(10) . . . . ? C5 C6 C7 C8 178.1(6) . . . . ? C6 C7 C8 C9 -0.5(11) . . . . ? C7 C8 C9 C10 2.1(12) . . . . ? C6 N2 C10 C9 0.0(10) . . . . ? Re N2 C10 C9 -179.6(6) . . . . ? C8 C9 C10 N2 -1.9(12) . . . . ? C15 N3 C11 C12 1.6(11) . . . . ? Re N3 C11 C12 -173.4(6) . . . . ? N3 C11 C12 C13 -0.5(12) . . . . ? C11 C12 C13 C14 -0.1(11) . . . . ? C11 C12 C13 C18 178.8(7) . . . . ? C12 C13 C14 C15 -0.5(11) . . . . ? C18 C13 C14 C15 -179.3(7) . . . . ? C11 N3 C15 C14 -2.2(11) . . . . ? Re N3 C15 C14 172.8(6) . . . . ? C13 C14 C15 N3 1.7(12) . . . . ? C20 N4 C16 C17 -4(3) . . . . ? N4 C16 C17 C18 5(3) . . . . ? C16 C17 C18 C19 -5(2) . . . . ? C16 C17 C18 C13 176.7(13) . . . . ? C14 C13 C18 C17 1.1(14) . . . . ? C12 C13 C18 C17 -177.7(11) . . . . ? C14 C13 C18 C19 -176.6(10) . . . . ? C12 C13 C18 C19 4.6(13) . . . . ? C17 C18 C19 C20 4.6(18) . . . . ? C13 C18 C19 C20 -177.4(10) . . . . ? C16 N4 C20 C19 3(2) . . . . ? C18 C19 C20 N4 -4(2) . . . . ? C23 Re C21 O1 -126(13) . . . . ? C22 Re C21 O1 -37(13) . . . . ? N1 Re C21 O1 124(13) . . . . ? N2 Re C21 O1 141(13) . . . . ? N3 Re C21 O1 55(13) . . . . ? C21 Re C22 O2 -73(31) . . . . ? C23 Re C22 O2 16(31) . . . . ? N1 Re C22 O2 110(31) . . . . ? N2 Re C22 O2 124(30) . . . . ? N3 Re C22 O2 -165(31) . . . . ? C21 Re C23 O3 -7(16) . . . . ? C22 Re C23 O3 -95(16) . . . . ? N1 Re C23 O3 166(16) . . . . ? N2 Re C23 O3 92(16) . . . . ? N3 Re C23 O3 132(14) . . . . ? O5 S1 C24 F1 179.7(10) . . . . ? O6 S1 C24 F1 -59.6(11) . . . . ? O4 S1 C24 F1 59.5(11) . . . . ? O5 S1 C24 F3 -58.9(9) . . . . ? O6 S1 C24 F3 61.8(9) . . . . ? O4 S1 C24 F3 -179.1(8) . . . . ? O5 S1 C24 F2 58.6(8) . . . . ? O6 S1 C24 F2 179.2(7) . . . . ? O4 S1 C24 F2 -61.7(8) . . . . ? C26 O7 C26 C27 0(2) 2_665 . . . ? _diffrn_measured_fraction_theta_max 0.849 _diffrn_reflns_theta_full 64.87 _diffrn_measured_fraction_theta_full 0.849 _refine_diff_density_max 1.070 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.112 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 614600' _audit_creation_method SHELXL-97 _chemical_name_systematic ; mer-tricarbonyl-(dimethylsulfoxide,O)-bis(pyridine)-rhenium(I) triflate ; _chemical_name_common ;mer-tricarbonyl-(dimethylsulfoxide,O)-bis(pyridine)- rhenium(i) triflate ; _chemical_melting_point ? _chemical_formula_moiety 'C15 H16 N2 O4 Re S 1-, C F3 O3 S 1-' _chemical_formula_sum 'C16 H16 F3 N2 O7 Re S2' _chemical_formula_weight 655.63 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.511(3) _cell_length_b 14.814(3) _cell_length_c 24.505(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4541.7(17) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 5.598 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.183 _exptl_absorpt_correction_T_max 0.440 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31630 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 26.44 _reflns_number_total 4031 _reflns_number_gt 2181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (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^)+(0.0285P)^2^] 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 4031 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 0.826 _refine_ls_restrained_S_all 0.826 _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 Re Re 0.25825(2) 0.134898(15) 0.148389(10) 0.05538(10) Uani 1 1 d . . . O1 O 0.3703(5) 0.2859(3) 0.2127(2) 0.0887(18) Uani 1 1 d . . . O2 O 0.1811(5) 0.2898(3) 0.0746(2) 0.0908(19) Uani 1 1 d . . . O3 O 0.0605(5) 0.1599(3) 0.2188(2) 0.0851(18) Uani 1 1 d . . . C1 C 0.3295(7) 0.2268(4) 0.1895(3) 0.065(2) Uani 1 1 d . . . C2 C 0.2094(6) 0.2303(5) 0.1012(3) 0.065(2) Uani 1 1 d . . . C3 C 0.1359(7) 0.1526(4) 0.1917(3) 0.066(2) Uani 1 1 d . . . N1 N 0.1807(5) 0.0264(3) 0.0995(2) 0.0596(16) Uani 1 1 d . . . N2 N 0.3158(5) 0.0248(3) 0.2024(2) 0.0604(16) Uani 1 1 d . . . C4 C 0.1092(7) -0.0290(5) 0.1216(3) 0.081(3) Uani 1 1 d . . . H4 H 0.0944 -0.0251 0.1587 0.097 Uiso 1 1 calc R . . C5 C 0.0571(7) -0.0917(5) 0.0905(4) 0.086(3) Uani 1 1 d . . . H5 H 0.0077 -0.1302 0.1067 0.104 Uiso 1 1 calc R . . C6 C 0.0770(7) -0.0982(5) 0.0360(4) 0.089(3) Uani 1 1 d . . . H6 H 0.0415 -0.1409 0.0149 0.106 Uiso 1 1 calc R . . C7 C 0.1500(7) -0.0412(5) 0.0127(3) 0.083(3) Uani 1 1 d . . . H7 H 0.1650 -0.0445 -0.0245 0.099 Uiso 1 1 calc R . . C8 C 0.2008(6) 0.0211(5) 0.0455(3) 0.070(2) Uani 1 1 d . . . H8 H 0.2501 0.0605 0.0300 0.084 Uiso 1 1 calc R . . C9 C 0.2997(7) 0.0290(5) 0.2564(3) 0.086(3) Uani 1 1 d . . . H9 H 0.2640 0.0788 0.2706 0.103 Uiso 1 1 calc R . . C10 C 0.3336(7) -0.0370(5) 0.2916(4) 0.095(3) Uani 1 1 d . . . H10 H 0.3221 -0.0320 0.3290 0.114 Uiso 1 1 calc R . . C11 C 0.3853(7) -0.1110(5) 0.2700(4) 0.091(3) Uani 1 1 d . . . H11 H 0.4073 -0.1579 0.2925 0.109 Uiso 1 1 calc R . . C12 C 0.4032(7) -0.1145(5) 0.2167(4) 0.087(3) Uani 1 1 d . . . H12 H 0.4408 -0.1630 0.2021 0.105 Uiso 1 1 calc R . . C13 C 0.3669(6) -0.0471(4) 0.1826(3) 0.071(2) Uani 1 1 d . . . H13 H 0.3782 -0.0518 0.1452 0.085 Uiso 1 1 calc R . . S1 S 0.49148(17) 0.15365(12) 0.09199(8) 0.0703(6) Uani 1 1 d . . . O4 O 0.3935(4) 0.0943(3) 0.09865(18) 0.0635(13) Uani 1 1 d . . . C14 C 0.5850(8) 0.1107(5) 0.1397(3) 0.102(3) Uani 1 1 d . . . H14A H 0.5627 0.1261 0.1760 0.152 Uiso 1 1 calc R . . H14B H 0.6541 0.1364 0.1327 0.152 Uiso 1 1 calc R . . H14C H 0.5890 0.0462 0.1362 0.152 Uiso 1 1 calc R . . C15 C 0.5562(6) 0.1145(5) 0.0335(3) 0.097(3) Uani 1 1 d . . . H15A H 0.5160 0.1316 0.0018 0.145 Uiso 1 1 calc R . . H15B H 0.5617 0.0499 0.0351 0.145 Uiso 1 1 calc R . . H15C H 0.6264 0.1403 0.0316 0.145 Uiso 1 1 calc R . . S2 S 0.2830(2) 0.17616(15) -0.07415(10) 0.0828(7) Uani 1 1 d . . . O5 O 0.1804(6) 0.1988(4) -0.0910(3) 0.147(3) Uani 1 1 d . . . O6 O 0.3084(8) 0.0868(4) -0.0852(3) 0.184(4) Uani 1 1 d . . . O7 O 0.3163(6) 0.2043(4) -0.0215(2) 0.156(3) Uani 1 1 d . . . C16 C 0.3650(12) 0.2402(9) -0.1194(5) 0.124(4) Uani 1 1 d . . . F1 F 0.3437(7) 0.2279(7) -0.1688(3) 0.229(5) Uani 1 1 d . . . F2 F 0.4632(7) 0.2269(8) -0.1111(3) 0.264(6) Uani 1 1 d . . . F3 F 0.3508(7) 0.3282(6) -0.1095(3) 0.190(3) 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 Re 0.0543(2) 0.05834(16) 0.05355(16) 0.00668(12) 0.00484(17) 0.00261(17) O1 0.104(5) 0.085(4) 0.077(4) -0.012(3) -0.005(4) -0.013(3) O2 0.091(5) 0.100(4) 0.082(4) 0.035(3) 0.000(3) 0.018(3) O3 0.080(5) 0.089(3) 0.086(5) 0.012(3) 0.032(3) 0.015(3) C1 0.060(7) 0.072(5) 0.062(6) 0.003(4) 0.011(4) 0.009(4) C2 0.047(6) 0.089(5) 0.060(5) 0.004(4) 0.006(4) -0.004(4) C3 0.093(8) 0.048(4) 0.058(5) 0.006(3) 0.001(4) 0.007(4) N1 0.053(5) 0.062(3) 0.064(5) 0.003(3) -0.003(3) -0.002(3) N2 0.065(5) 0.057(3) 0.059(4) 0.013(3) 0.004(3) 0.011(3) C4 0.085(8) 0.079(5) 0.080(6) -0.001(4) 0.023(5) -0.027(5) C5 0.080(8) 0.081(5) 0.098(8) 0.001(5) 0.013(6) -0.018(5) C6 0.078(8) 0.083(6) 0.104(8) -0.020(5) -0.020(6) -0.008(5) C7 0.083(8) 0.088(6) 0.077(7) -0.010(5) -0.009(5) -0.012(5) C8 0.070(7) 0.077(5) 0.062(6) 0.005(4) 0.000(4) -0.013(4) C9 0.099(8) 0.096(6) 0.063(6) 0.011(5) 0.008(5) 0.029(5) C10 0.107(9) 0.105(6) 0.072(7) 0.025(5) 0.001(6) 0.010(6) C11 0.101(9) 0.067(5) 0.105(8) 0.020(5) -0.023(6) 0.015(4) C12 0.094(8) 0.076(5) 0.092(7) 0.009(5) 0.018(6) 0.018(4) C13 0.084(7) 0.060(4) 0.070(6) 0.002(4) 0.014(5) 0.005(4) S1 0.0648(17) 0.0692(10) 0.0770(14) 0.0035(10) 0.0110(11) -0.0032(10) O4 0.041(4) 0.076(3) 0.074(4) 0.002(2) 0.015(3) -0.002(2) C14 0.108(9) 0.104(6) 0.092(8) 0.018(5) -0.029(6) -0.007(5) C15 0.083(8) 0.148(8) 0.060(6) -0.011(5) 0.026(5) -0.019(5) S2 0.089(2) 0.0846(14) 0.0751(16) -0.0035(11) 0.0074(13) 0.0035(12) O5 0.066(7) 0.136(5) 0.239(9) 0.055(5) 0.008(5) -0.006(4) O6 0.307(11) 0.093(5) 0.150(7) -0.021(4) -0.028(7) 0.074(6) O7 0.227(9) 0.181(6) 0.060(5) -0.021(4) 0.020(5) -0.081(6) C16 0.105(13) 0.165(11) 0.103(11) 0.017(9) 0.018(8) 0.041(10) F1 0.209(10) 0.426(14) 0.052(4) 0.016(6) 0.012(5) -0.071(8) F2 0.070(7) 0.522(17) 0.200(9) 0.138(9) 0.044(6) 0.040(9) F3 0.189(9) 0.186(6) 0.196(8) 0.044(6) -0.005(7) -0.082(7) _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 Re C3 1.881(8) . ? Re C1 1.914(8) . ? Re C2 1.926(8) . ? Re O4 2.171(4) . ? Re N2 2.220(5) . ? Re N1 2.228(5) . ? O1 C1 1.161(8) . ? O2 C2 1.152(7) . ? O3 C3 1.159(8) . ? N1 C4 1.330(8) . ? N1 C8 1.348(8) . ? N2 C13 1.334(7) . ? N2 C9 1.341(8) . ? C4 C5 1.365(10) . ? C5 C6 1.361(11) . ? C6 C7 1.369(10) . ? C7 C8 1.380(9) . ? C9 C10 1.371(9) . ? C10 C11 1.378(10) . ? C11 C12 1.327(10) . ? C12 C13 1.379(9) . ? S1 O4 1.518(4) . ? S1 C15 1.744(7) . ? S1 C14 1.772(8) . ? S2 O6 1.389(6) . ? S2 O5 1.390(7) . ? S2 O7 1.419(6) . ? S2 C16 1.784(13) . ? C16 F1 1.253(13) . ? C16 F2 1.260(13) . ? C16 F3 1.337(12) . ? 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 C3 Re C1 89.0(3) . . ? C3 Re C2 88.7(3) . . ? C1 Re C2 86.7(3) . . ? C3 Re O4 171.9(2) . . ? C1 Re O4 97.5(3) . . ? C2 Re O4 96.5(3) . . ? C3 Re N2 91.8(3) . . ? C1 Re N2 93.3(3) . . ? C2 Re N2 179.5(3) . . ? O4 Re N2 82.98(19) . . ? C3 Re N1 92.9(3) . . ? C1 Re N1 178.1(3) . . ? C2 Re N1 93.9(3) . . ? O4 Re N1 80.6(2) . . ? N2 Re N1 86.1(2) . . ? O1 C1 Re 176.4(7) . . ? O2 C2 Re 177.2(7) . . ? O3 C3 Re 177.3(6) . . ? C4 N1 C8 119.3(6) . . ? C4 N1 Re 121.3(5) . . ? C8 N1 Re 119.2(5) . . ? C13 N2 C9 117.9(6) . . ? C13 N2 Re 121.7(5) . . ? C9 N2 Re 120.4(5) . . ? N1 C4 C5 120.9(8) . . ? C6 C5 C4 120.5(8) . . ? C5 C6 C7 119.2(8) . . ? C6 C7 C8 118.4(8) . . ? N1 C8 C7 121.7(7) . . ? N2 C9 C10 122.8(7) . . ? C9 C10 C11 118.1(8) . . ? C12 C11 C10 119.3(8) . . ? C11 C12 C13 120.8(7) . . ? N2 C13 C12 121.0(7) . . ? O4 S1 C15 105.7(3) . . ? O4 S1 C14 104.7(3) . . ? C15 S1 C14 96.6(4) . . ? S1 O4 Re 122.0(2) . . ? O6 S2 O5 112.6(5) . . ? O6 S2 O7 113.0(5) . . ? O5 S2 O7 118.0(5) . . ? O6 S2 C16 104.7(6) . . ? O5 S2 C16 102.6(6) . . ? O7 S2 C16 103.9(6) . . ? F1 C16 F2 109.9(12) . . ? F1 C16 F3 106.7(11) . . ? F2 C16 F3 104.7(14) . . ? F1 C16 S2 113.6(12) . . ? F2 C16 S2 112.1(10) . . ? F3 C16 S2 109.2(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 C3 Re C1 O1 -85(12) . . . . ? C2 Re C1 O1 3(12) . . . . ? O4 Re C1 O1 100(12) . . . . ? N2 Re C1 O1 -177(100) . . . . ? N1 Re C1 O1 111(12) . . . . ? C3 Re C2 O2 71(15) . . . . ? C1 Re C2 O2 -18(15) . . . . ? O4 Re C2 O2 -116(15) . . . . ? N2 Re C2 O2 -108(33) . . . . ? N1 Re C2 O2 163(15) . . . . ? C1 Re C3 O3 -127(17) . . . . ? C2 Re C3 O3 146(17) . . . . ? O4 Re C3 O3 16(18) . . . . ? N2 Re C3 O3 -34(17) . . . . ? N1 Re C3 O3 53(17) . . . . ? C3 Re N1 C4 -32.9(6) . . . . ? C1 Re N1 C4 131(8) . . . . ? C2 Re N1 C4 -121.8(6) . . . . ? O4 Re N1 C4 142.2(6) . . . . ? N2 Re N1 C4 58.7(6) . . . . ? C3 Re N1 C8 142.2(5) . . . . ? C1 Re N1 C8 -54(8) . . . . ? C2 Re N1 C8 53.3(6) . . . . ? O4 Re N1 C8 -42.7(5) . . . . ? N2 Re N1 C8 -126.2(5) . . . . ? C3 Re N2 C13 144.3(6) . . . . ? C1 Re N2 C13 -126.6(6) . . . . ? C2 Re N2 C13 -37(33) . . . . ? O4 Re N2 C13 -29.5(6) . . . . ? N1 Re N2 C13 51.6(6) . . . . ? C3 Re N2 C9 -35.5(6) . . . . ? C1 Re N2 C9 53.5(6) . . . . ? C2 Re N2 C9 143(33) . . . . ? O4 Re N2 C9 150.7(6) . . . . ? N1 Re N2 C9 -128.3(6) . . . . ? C8 N1 C4 C5 0.8(12) . . . . ? Re N1 C4 C5 175.9(6) . . . . ? N1 C4 C5 C6 -0.4(14) . . . . ? C4 C5 C6 C7 0.0(14) . . . . ? C5 C6 C7 C8 -0.1(13) . . . . ? C4 N1 C8 C7 -0.8(11) . . . . ? Re N1 C8 C7 -176.0(6) . . . . ? C6 C7 C8 N1 0.5(12) . . . . ? C13 N2 C9 C10 0.2(12) . . . . ? Re N2 C9 C10 -180.0(7) . . . . ? N2 C9 C10 C11 -0.8(14) . . . . ? C9 C10 C11 C12 2.1(14) . . . . ? C10 C11 C12 C13 -2.8(14) . . . . ? C9 N2 C13 C12 -0.8(12) . . . . ? Re N2 C13 C12 179.3(6) . . . . ? C11 C12 C13 N2 2.2(13) . . . . ? C15 S1 O4 Re -160.9(3) . . . . ? C14 S1 O4 Re 97.7(4) . . . . ? C3 Re O4 S1 -160.3(18) . . . . ? C1 Re O4 S1 -17.9(4) . . . . ? C2 Re O4 S1 69.6(4) . . . . ? N2 Re O4 S1 -110.3(3) . . . . ? N1 Re O4 S1 162.5(3) . . . . ? O6 S2 C16 F1 64.6(12) . . . . ? O5 S2 C16 F1 -53.2(12) . . . . ? O7 S2 C16 F1 -176.7(10) . . . . ? O6 S2 C16 F2 -60.8(13) . . . . ? O5 S2 C16 F2 -178.6(11) . . . . ? O7 S2 C16 F2 57.9(13) . . . . ? O6 S2 C16 F3 -176.4(9) . . . . ? O5 S2 C16 F3 65.8(11) . . . . ? O7 S2 C16 F3 -57.7(11) . . . . ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.862 _refine_diff_density_max 0.489 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.089 #===END data_13-rev _database_code_depnum_ccdc_archive 'CCDC 614601' _audit_creation_method SHELXL-97 _chemical_name_systematic ; mer-tricarbonyl-chloro-bis[(5-(4'pyridyl)-10,15,20-triphenyl-porphyrin)]- -rhenium(I) bis(diethylether) solvate ; _chemical_name_common ; mer-tricarbonyl-chloro-bis((5-(4'pyridyl)-10,15,20-triphenyl- porphyrin))--rhenium(i) bis(diethylether) solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C93 H68 Cl N10 O4 Re, 2(C4 H10 O)' _chemical_formula_sum 'C97 H78 Cl N10 O5 Re' _chemical_formula_weight 1685.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0074 0.0035 '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 0.0136 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0227 0.0128 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -7.2020 10.7760 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.2413 0.3112 '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/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.559(4) _cell_length_b 31.546(5) _cell_length_c 18.352(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.76(3) _cell_angle_gamma 90.00 _cell_volume 8749(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3448 _exptl_absorpt_coefficient_mu 2.980 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.0000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Elettra Synchrotron, Trieste (Italy)' _diffrn_radiation_monochromator Si111 _diffrn_measurement_device_type 'CCD MarResearch' _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 47924 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 30.35 _reflns_number_total 8450 _reflns_number_gt 6610 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (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^)+(0.1030P)^2^+14.2200P] 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 8450 _refine_ls_number_parameters 965 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1694 _refine_ls_wR_factor_gt 0.1581 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.091 _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 Re Re 0.01193(2) 0.251298(9) 0.44364(2) 0.0615(2) Uani 1 1 d . . . Cl1 Cl -0.04119(14) 0.32004(6) 0.37321(13) 0.0766(6) Uani 1 1 d . . . C1X C -0.0921(6) 0.2170(2) 0.3927(5) 0.067(2) Uani 1 1 d . . . C2X C -0.0522(6) 0.2660(3) 0.5203(6) 0.074(2) Uani 1 1 d . . . C3X C 0.0638(6) 0.1978(3) 0.5024(5) 0.065(2) Uani 1 1 d . . . O1 O -0.1520(4) 0.19535(17) 0.3629(4) 0.0782(16) Uani 1 1 d . . . O2 O -0.0937(5) 0.27531(18) 0.5648(4) 0.100(2) Uani 1 1 d . . . O3 O 0.0871(4) 0.1705(2) 0.5313(4) 0.0914(19) Uani 1 1 d . . . N1 N 0.3221(4) 0.16938(19) 0.1204(4) 0.0623(17) Uani 1 1 d . . . H1A H 0.3567 0.1861 0.1016 0.075 Uiso 1 1 calc R . . N2 N 0.4464(4) 0.1573(2) 0.0225(4) 0.0672(17) Uani 1 1 d . . . N3 N 0.4923(5) 0.25189(18) 0.0342(4) 0.0644(19) Uani 1 1 d . . . H3A H 0.4510 0.2365 0.0468 0.077 Uiso 1 1 calc R . . N4 N 0.3619(4) 0.2640(2) 0.1263(4) 0.0629(17) Uani 1 1 d . . . C1 C 0.2705(5) 0.1816(2) 0.1698(5) 0.063(2) Uani 1 1 d . . . C2 C 0.2252(5) 0.1443(2) 0.1893(5) 0.067(2) Uani 1 1 d . . . H2 H 0.1870 0.1437 0.2227 0.080 Uiso 1 1 calc R . . C3 C 0.2475(6) 0.1098(3) 0.1505(5) 0.075(2) Uani 1 1 d . . . H3 H 0.2273 0.0814 0.1522 0.090 Uiso 1 1 calc R . . C4 C 0.3090(5) 0.1257(2) 0.1060(5) 0.064(2) Uani 1 1 d . . . C5 C 0.3475(6) 0.1003(2) 0.0562(5) 0.075(2) Uani 1 1 d . . . C6 C 0.4112(6) 0.1155(2) 0.0184(5) 0.070(2) Uani 1 1 d . . . C7 C 0.4547(6) 0.0899(3) -0.0325(5) 0.076(2) Uani 1 1 d . . . H7 H 0.4434 0.0610 -0.0458 0.091 Uiso 1 1 calc R . . C8 C 0.5140(6) 0.1162(3) -0.0561(5) 0.075(2) Uani 1 1 d . . . H8 H 0.5509 0.1085 -0.0884 0.090 Uiso 1 1 calc R . . C9 C 0.5097(6) 0.1586(2) -0.0218(5) 0.068(2) Uani 1 1 d . . . C10 C 0.5621(6) 0.1952(3) -0.0333(5) 0.068(2) Uani 1 1 d . . . C11 C 0.5541(6) 0.2373(3) -0.0046(5) 0.066(2) Uani 1 1 d . . . C12 C 0.6140(6) 0.2732(3) -0.0125(5) 0.071(2) Uani 1 1 d . . . H12 H 0.6625 0.2721 -0.0356 0.085 Uiso 1 1 calc R . . C13 C 0.5852(6) 0.3087(3) 0.0207(5) 0.072(2) Uani 1 1 d . . . H13 H 0.6103 0.3363 0.0241 0.086 Uiso 1 1 calc R . . C14 C 0.5074(5) 0.2952(2) 0.0498(4) 0.064(2) Uani 1 1 d . . . C15 C 0.4574(5) 0.3220(2) 0.0896(5) 0.066(2) Uani 1 1 d . . . C16 C 0.3869(5) 0.3075(2) 0.1211(5) 0.063(2) Uani 1 1 d . . . C17 C 0.3298(6) 0.3340(2) 0.1574(5) 0.070(2) Uani 1 1 d . . . H17 H 0.3311 0.3640 0.1606 0.084 Uiso 1 1 calc R . . C18 C 0.2745(6) 0.3076(2) 0.1857(5) 0.071(2) Uani 1 1 d . . . H18 H 0.2312 0.3160 0.2115 0.085 Uiso 1 1 calc R . . C19 C 0.2962(6) 0.2631(3) 0.1676(5) 0.067(2) Uani 1 1 d . . . C20 C 0.2559(5) 0.2251(2) 0.1914(4) 0.058(2) Uani 1 1 d . . . N5 N 0.5216(5) 0.38300(19) 0.6714(4) 0.0739(19) Uani 1 1 d . . . N6 N 0.6676(5) 0.44725(19) 0.7254(5) 0.086(2) Uani 1 1 d . . . H6A H 0.6115 0.4494 0.7019 0.103 Uiso 1 1 calc R . . N7 N 0.5522(4) 0.51623(19) 0.6468(4) 0.0699(18) Uani 1 1 d . . . N8 N 0.4042(4) 0.45171(19) 0.5933(4) 0.0705(18) Uani 1 1 d . . . H8A H 0.4606 0.4495 0.6159 0.085 Uiso 1 1 calc R . . C21 C 0.4440(6) 0.3584(2) 0.6414(5) 0.075(2) Uani 1 1 d . . . C22 C 0.4665(7) 0.3133(2) 0.6636(5) 0.082(3) Uani 1 1 d . . . H22 H 0.4278 0.2897 0.6512 0.099 Uiso 1 1 calc R . . C23 C 0.5525(6) 0.3119(2) 0.7047(5) 0.078(3) Uani 1 1 d . . . H23 H 0.5836 0.2872 0.7259 0.094 Uiso 1 1 calc R . . C24 C 0.5887(6) 0.3558(2) 0.7104(5) 0.078(2) Uani 1 1 d . . . C25 C 0.6775(6) 0.3675(2) 0.7474(5) 0.081(3) Uani 1 1 d . . . C26 C 0.7121(6) 0.4101(3) 0.7542(6) 0.088(3) Uani 1 1 d . . . C27 C 0.8070(6) 0.4207(3) 0.7900(6) 0.097(3) Uani 1 1 d . . . H27 H 0.8523 0.4016 0.8133 0.116 Uiso 1 1 calc R . . C28 C 0.8149(7) 0.4642(3) 0.7819(6) 0.100(3) Uani 1 1 d . . . H28 H 0.8671 0.4804 0.8000 0.120 Uiso 1 1 calc R . . C29 C 0.7304(6) 0.4809(3) 0.7415(6) 0.084(3) Uani 1 1 d . . . C30 C 0.7115(6) 0.5248(2) 0.7188(5) 0.076(2) Uani 1 1 d . . . C31 C 0.6296(6) 0.5408(2) 0.6754(5) 0.072(2) Uani 1 1 d . . . C32 C 0.6075(6) 0.5858(2) 0.6538(5) 0.072(2) Uani 1 1 d . . . H32 H 0.6467 0.6093 0.6655 0.086 Uiso 1 1 calc R . . C33 C 0.5203(6) 0.5874(2) 0.6138(5) 0.076(2) Uani 1 1 d . . . H33 H 0.4899 0.6122 0.5924 0.091 Uiso 1 1 calc R . . C34 C 0.4817(6) 0.5441(2) 0.6098(5) 0.070(2) Uani 1 1 d . . . C35 C 0.3935(5) 0.5321(2) 0.5721(5) 0.067(2) Uani 1 1 d . . . C36 C 0.3600(5) 0.4896(2) 0.5673(5) 0.069(2) Uani 1 1 d . . . C37 C 0.2635(6) 0.4791(3) 0.5333(5) 0.082(3) Uani 1 1 d . . . H37 H 0.2179 0.4985 0.5119 0.098 Uiso 1 1 calc R . . C38 C 0.2549(6) 0.4353(3) 0.5398(5) 0.081(3) Uani 1 1 d . . . H38 H 0.2021 0.4193 0.5233 0.097 Uiso 1 1 calc R . . C39 C 0.3438(6) 0.4180(2) 0.5772(5) 0.072(2) Uani 1 1 d . . . C40 C 0.3630(6) 0.3741(2) 0.5960(5) 0.070(2) Uani 1 1 d . . . N11 N 0.0870(4) 0.23865(19) 0.3527(4) 0.0606(18) Uani 1 1 d . . . N12 N 0.1364(4) 0.28904(18) 0.4974(4) 0.0643(17) Uani 1 1 d . . . C41 C 0.0577(6) 0.2527(2) 0.2797(5) 0.062(2) Uani 1 1 d . . . H41 H 0.0005 0.2651 0.2650 0.074 Uiso 1 1 calc R . . C42 C 0.1098(6) 0.2493(2) 0.2252(5) 0.061(2) Uani 1 1 d . . . H42 H 0.0871 0.2596 0.1757 0.074 Uiso 1 1 calc R . . C43 C 0.1959(5) 0.2304(2) 0.2450(5) 0.059(2) Uani 1 1 d . . . C44 C 0.2245(5) 0.2149(2) 0.3209(5) 0.066(2) Uani 1 1 d . . . H44 H 0.2805 0.2014 0.3366 0.079 Uiso 1 1 calc R . . C45 C 0.1692(5) 0.2198(2) 0.3726(5) 0.068(2) Uani 1 1 d . . . H45 H 0.1900 0.2096 0.4225 0.081 Uiso 1 1 calc R . . C46 C 0.1747(5) 0.3158(2) 0.4533(5) 0.065(2) Uani 1 1 d . . . H46 H 0.1503 0.3168 0.4006 0.079 Uiso 1 1 calc R . . C47 C 0.2499(5) 0.3421(2) 0.4852(5) 0.067(2) Uani 1 1 d . . . H47 H 0.2751 0.3592 0.4531 0.081 Uiso 1 1 calc R . . C48 C 0.2870(6) 0.3430(2) 0.5636(5) 0.069(2) Uani 1 1 d . . . C49 C 0.2488(6) 0.3136(3) 0.6087(5) 0.076(2) Uani 1 1 d . . . H49 H 0.2732 0.3116 0.6612 0.091 Uiso 1 1 calc R . . C50 C 0.1756(6) 0.2881(2) 0.5745(5) 0.074(2) Uani 1 1 d . . . H50 H 0.1517 0.2695 0.6053 0.088 Uiso 1 1 calc R . . C51 C 0.3129(6) 0.05297(19) 0.0403(5) 0.104(4) Uani 1 1 d G . . C52 C 0.2454(6) 0.0436(3) -0.0221(5) 0.127(4) Uani 1 1 d G . . H52 H 0.2202 0.0655 -0.0562 0.153 Uiso 1 1 calc R . . C53 C 0.2146(5) 0.0023(3) -0.0348(5) 0.155(5) Uani 1 1 d G . . H53 H 0.1684 -0.0041 -0.0775 0.185 Uiso 1 1 calc R . . C54 C 0.2514(7) -0.0297(2) 0.0149(7) 0.140(5) Uani 1 1 d G . . H54 H 0.2304 -0.0580 0.0063 0.168 Uiso 1 1 calc R . . C55 C 0.3189(8) -0.0204(2) 0.0774(6) 0.171(6) Uani 1 1 d G . . H55 H 0.3441 -0.0423 0.1114 0.205 Uiso 1 1 calc R . . C56 C 0.3497(6) 0.0210(3) 0.0901(5) 0.146(5) Uani 1 1 d G . . H56 H 0.3959 0.0274 0.1328 0.175 Uiso 1 1 calc R . . C57 C 0.6296(6) 0.1875(2) -0.0801(5) 0.068(2) Uani 1 1 d . . . C58 C 0.7107(7) 0.1665(4) -0.0509(6) 0.105(3) Uani 1 1 d . . . H58 H 0.7262 0.1588 0.0007 0.126 Uiso 1 1 calc R . . C59 C 0.7700(7) 0.1565(4) -0.0974(7) 0.107(3) Uani 1 1 d . . . H59 H 0.8243 0.1427 -0.0758 0.128 Uiso 1 1 calc R . . C60 C 0.7501(7) 0.1664(3) -0.1721(6) 0.086(3) Uani 1 1 d . . . H60 H 0.7885 0.1583 -0.2029 0.103 Uiso 1 1 calc R . . C61 C 0.6706(9) 0.1893(4) -0.2029(7) 0.122(4) Uani 1 1 d . . . H61 H 0.6562 0.1971 -0.2543 0.147 Uiso 1 1 calc R . . C62 C 0.6128(8) 0.2003(4) -0.1559(7) 0.114(4) Uani 1 1 d . . . H62 H 0.5616 0.2167 -0.1762 0.137 Uiso 1 1 calc R . . C63 C 0.4817(5) 0.3697(2) 0.0998(5) 0.070(2) Uani 1 1 d . . . C64 C 0.4828(6) 0.3960(3) 0.0349(6) 0.084(3) Uani 1 1 d . . . H64 H 0.4663 0.3844 -0.0142 0.101 Uiso 1 1 calc R . . C65 C 0.5092(7) 0.4402(3) 0.0459(7) 0.101(3) Uani 1 1 d . . . H65 H 0.5140 0.4570 0.0041 0.121 Uiso 1 1 calc R . . C66 C 0.5281(7) 0.4585(3) 0.1190(7) 0.098(3) Uani 1 1 d . . . H66 H 0.5433 0.4877 0.1254 0.118 Uiso 1 1 calc R . . C67 C 0.5244(6) 0.4339(3) 0.1807(6) 0.083(3) Uani 1 1 d . . . H67 H 0.5364 0.4464 0.2292 0.100 Uiso 1 1 calc R . . C68 C 0.5021(6) 0.3890(3) 0.1722(6) 0.075(2) Uani 1 1 d . . . H68 H 0.5013 0.3724 0.2152 0.090 Uiso 1 1 calc R . . C69 C 0.3288(6) 0.5668(2) 0.5379(6) 0.075(2) Uani 1 1 d . . . C70 C 0.2996(7) 0.5704(3) 0.4591(7) 0.094(3) Uani 1 1 d . . . H70 H 0.3256 0.5523 0.4290 0.113 Uiso 1 1 calc R . . C71 C 0.2343(8) 0.5992(4) 0.4226(9) 0.125(4) Uani 1 1 d . . . H71 H 0.2174 0.6018 0.3695 0.150 Uiso 1 1 calc R . . C72 C 0.1956(8) 0.6242(3) 0.4705(9) 0.116(4) Uani 1 1 d . . . H72 H 0.1504 0.6434 0.4472 0.139 Uiso 1 1 calc R . . C73 C 0.2171(8) 0.6230(3) 0.5469(9) 0.119(4) Uani 1 1 d . . . H73 H 0.1885 0.6409 0.5755 0.143 Uiso 1 1 calc R . . C74 C 0.2876(7) 0.5926(3) 0.5840(7) 0.103(3) Uani 1 1 d . . . H74 H 0.3047 0.5904 0.6371 0.123 Uiso 1 1 calc R . . C75 C 0.7875(6) 0.5572(2) 0.7435(6) 0.072(2) Uani 1 1 d . . . C76 C 0.8310(7) 0.5737(3) 0.6893(6) 0.093(3) Uani 1 1 d . . . H76 H 0.8128 0.5644 0.6387 0.112 Uiso 1 1 calc R . . C77 C 0.9014(7) 0.6039(3) 0.7093(7) 0.096(3) Uani 1 1 d . . . H77 H 0.9286 0.6148 0.6720 0.116 Uiso 1 1 calc R . . C78 C 0.9305(6) 0.6173(3) 0.7843(7) 0.085(3) Uani 1 1 d . . . H78 H 0.9777 0.6370 0.7983 0.102 Uiso 1 1 calc R . . C79 C 0.8875(6) 0.6007(3) 0.8396(7) 0.092(3) Uani 1 1 d . . . H79 H 0.9060 0.6097 0.8903 0.111 Uiso 1 1 calc R . . C80 C 0.8170(6) 0.5706(3) 0.8187(6) 0.078(2) Uani 1 1 d . . . H80 H 0.7897 0.5596 0.8558 0.094 Uiso 1 1 calc R . . C81 C 0.7421(6) 0.3309(3) 0.7789(6) 0.080(3) Uani 1 1 d . . . C82 C 0.7568(6) 0.3177(3) 0.8538(6) 0.082(3) Uani 1 1 d . . . H82 H 0.7260 0.3315 0.8860 0.098 Uiso 1 1 calc R . . C83 C 0.8171(6) 0.2838(3) 0.8833(6) 0.082(3) Uani 1 1 d . . . H83 H 0.8255 0.2751 0.9341 0.098 Uiso 1 1 calc R . . C84 C 0.8632(7) 0.2638(3) 0.8357(7) 0.091(3) Uani 1 1 d . . . H84 H 0.9031 0.2414 0.8545 0.109 Uiso 1 1 calc R . . C85 C 0.8506(7) 0.2770(3) 0.7588(7) 0.098(3) Uani 1 1 d . . . H85 H 0.8826 0.2639 0.7269 0.117 Uiso 1 1 calc R . . C86 C 0.7903(7) 0.3096(3) 0.7319(6) 0.094(3) Uani 1 1 d . . . H86 H 0.7810 0.3180 0.6808 0.113 Uiso 1 1 calc R . . C92 C 0.9644(11) 0.6059(5) 0.4958(8) 0.161(5) Uiso 1 1 d D . . C91 C 0.9511(8) 0.6229(4) 0.4134(7) 0.116(4) Uiso 1 1 d D . . O10 O 0.9176(16) 0.6066(8) 0.3399(11) 0.370(12) Uiso 1 1 d D . . C93 C 0.9840(16) 0.6110(8) 0.2958(13) 0.218(9) Uiso 1 1 d D . . C94 C 0.9695(16) 0.5702(8) 0.2606(14) 0.237(9) Uiso 1 1 d D . . C96 C 0.818(2) 0.4805(12) 0.299(2) 0.344(17) Uiso 1 1 d D . . C95 C 0.7348(12) 0.5056(6) 0.2573(10) 0.160(5) Uiso 1 1 d D . . O20 O 0.7492(16) 0.5513(7) 0.2503(15) 0.366(12) Uiso 1 1 d D . . C97 C 0.6616(17) 0.5577(9) 0.2051(18) 0.288(14) Uiso 1 1 d D . . C98 C 0.5794(11) 0.5744(5) 0.1800(9) 0.148(5) Uiso 1 1 d 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 Re 0.0569(3) 0.0463(3) 0.0844(3) -0.00500(16) 0.0231(2) -0.00301(14) Cl1 0.0669(15) 0.0617(12) 0.1056(17) -0.0058(11) 0.0291(12) -0.0053(9) C1X 0.056(6) 0.051(4) 0.096(7) 0.001(4) 0.022(5) 0.006(4) C2X 0.074(7) 0.050(5) 0.105(7) 0.008(5) 0.038(6) 0.006(4) C3X 0.070(6) 0.047(5) 0.082(6) -0.012(4) 0.027(5) -0.021(4) O1 0.068(4) 0.058(3) 0.108(5) -0.003(3) 0.019(3) -0.010(3) O2 0.133(6) 0.060(4) 0.132(6) 0.017(4) 0.077(5) 0.024(4) O3 0.082(5) 0.084(5) 0.111(6) -0.016(4) 0.027(4) 0.003(4) N1 0.054(4) 0.057(4) 0.078(5) -0.001(3) 0.021(3) 0.001(3) N2 0.065(5) 0.069(4) 0.070(5) 0.001(3) 0.021(4) 0.003(3) N3 0.056(5) 0.067(5) 0.071(4) 0.004(3) 0.015(4) -0.003(3) N4 0.061(5) 0.060(4) 0.071(5) 0.002(3) 0.023(4) 0.003(3) C1 0.059(6) 0.058(5) 0.070(6) 0.000(4) 0.012(4) 0.003(4) C2 0.060(6) 0.059(5) 0.085(6) -0.001(4) 0.024(4) 0.001(4) C3 0.070(6) 0.055(5) 0.107(7) 0.001(5) 0.034(5) 0.001(4) C4 0.060(6) 0.052(5) 0.084(6) -0.006(4) 0.023(4) -0.002(4) C5 0.070(6) 0.053(5) 0.107(7) -0.005(4) 0.029(5) -0.002(4) C6 0.069(6) 0.060(5) 0.083(6) -0.008(4) 0.024(5) -0.001(4) C7 0.069(6) 0.068(5) 0.096(7) -0.022(5) 0.028(5) -0.003(4) C8 0.070(7) 0.067(5) 0.095(7) -0.014(4) 0.033(5) 0.003(4) C9 0.067(6) 0.068(5) 0.070(6) -0.002(4) 0.017(4) -0.001(4) C10 0.067(6) 0.074(6) 0.063(5) 0.000(4) 0.015(4) 0.006(4) C11 0.057(6) 0.073(5) 0.069(6) 0.000(4) 0.014(4) -0.002(4) C12 0.058(6) 0.074(6) 0.086(6) 0.005(5) 0.029(5) -0.004(4) C13 0.067(6) 0.069(5) 0.080(6) 0.006(4) 0.018(5) -0.006(4) C14 0.059(6) 0.062(5) 0.070(6) 0.006(4) 0.014(4) -0.001(4) C15 0.059(6) 0.058(5) 0.080(6) 0.012(4) 0.015(4) 0.003(4) C16 0.055(6) 0.055(5) 0.075(6) 0.007(4) 0.010(4) 0.004(4) C17 0.069(6) 0.047(4) 0.096(7) 0.004(4) 0.024(5) 0.001(4) C18 0.069(6) 0.055(5) 0.091(6) -0.004(4) 0.025(5) 0.011(4) C19 0.069(7) 0.059(5) 0.070(6) -0.002(4) 0.008(5) 0.005(4) C20 0.048(5) 0.057(5) 0.071(5) -0.001(4) 0.018(4) 0.002(3) N5 0.069(5) 0.051(4) 0.093(5) -0.009(4) 0.003(4) -0.008(3) N6 0.070(5) 0.045(4) 0.126(7) 0.004(4) -0.010(4) -0.007(3) N7 0.070(5) 0.054(4) 0.080(5) -0.005(3) 0.007(4) -0.003(3) N8 0.055(4) 0.058(4) 0.092(5) -0.005(3) 0.004(3) -0.001(3) C21 0.077(7) 0.056(5) 0.090(6) -0.005(4) 0.015(5) -0.005(4) C22 0.094(8) 0.049(5) 0.101(7) -0.001(4) 0.015(6) -0.014(4) C23 0.077(7) 0.051(5) 0.099(7) 0.005(4) 0.005(5) -0.008(4) C24 0.079(7) 0.051(5) 0.093(7) 0.000(4) 0.000(5) -0.006(4) C25 0.082(7) 0.048(5) 0.103(7) 0.006(4) 0.000(5) -0.010(4) C26 0.072(7) 0.059(6) 0.115(8) 0.000(5) -0.010(5) -0.007(4) C27 0.075(7) 0.055(5) 0.140(9) 0.011(5) -0.017(6) -0.007(4) C28 0.085(8) 0.056(6) 0.141(10) 0.005(5) -0.008(6) -0.008(5) C29 0.074(7) 0.058(5) 0.107(7) 0.010(5) -0.003(5) -0.005(5) C30 0.079(7) 0.054(5) 0.089(7) -0.002(4) 0.011(5) -0.011(4) C31 0.072(6) 0.059(5) 0.082(6) -0.006(4) 0.009(5) -0.002(4) C32 0.081(7) 0.044(4) 0.087(6) 0.008(4) 0.012(5) -0.005(4) C33 0.078(7) 0.044(4) 0.101(7) -0.006(4) 0.010(5) -0.002(4) C34 0.076(7) 0.059(5) 0.081(6) -0.005(4) 0.032(5) -0.003(4) C35 0.058(6) 0.063(5) 0.078(6) -0.008(4) 0.013(4) -0.001(4) C36 0.063(6) 0.056(5) 0.083(6) -0.013(4) 0.006(4) -0.004(4) C37 0.082(7) 0.062(6) 0.095(7) -0.011(5) 0.010(5) -0.001(4) C38 0.078(7) 0.060(6) 0.099(7) -0.016(5) 0.012(5) -0.009(4) C39 0.070(6) 0.061(5) 0.080(6) -0.012(4) 0.007(5) -0.010(4) C40 0.073(6) 0.048(4) 0.087(6) -0.005(4) 0.014(5) -0.006(4) N11 0.048(5) 0.048(3) 0.083(5) -0.005(3) 0.011(4) -0.002(3) N12 0.061(4) 0.054(4) 0.081(5) -0.008(3) 0.021(4) -0.007(3) C41 0.046(6) 0.057(5) 0.077(6) -0.006(4) 0.004(5) 0.000(3) C42 0.053(6) 0.064(5) 0.065(5) -0.009(4) 0.009(4) 0.006(4) C43 0.065(6) 0.042(4) 0.069(6) -0.005(4) 0.012(4) -0.005(4) C44 0.043(5) 0.060(5) 0.097(7) -0.002(4) 0.023(5) 0.005(4) C45 0.057(6) 0.057(5) 0.087(6) 0.003(4) 0.013(5) 0.000(4) C46 0.060(6) 0.056(4) 0.083(6) -0.008(4) 0.022(4) -0.004(4) C47 0.062(6) 0.053(4) 0.088(7) -0.003(4) 0.022(5) -0.011(4) C48 0.073(6) 0.056(5) 0.075(7) -0.010(4) 0.013(5) 0.002(4) C49 0.080(6) 0.079(5) 0.069(6) -0.006(5) 0.016(5) -0.013(5) C50 0.083(6) 0.060(5) 0.080(7) -0.002(4) 0.025(5) -0.016(4) C51 0.130(10) 0.055(5) 0.153(11) -0.005(6) 0.086(8) 0.011(5) C52 0.113(7) 0.098(7) 0.163(9) -0.031(6) 0.018(7) -0.031(6) C53 0.149(9) 0.138(8) 0.186(9) -0.031(8) 0.059(7) -0.024(7) C54 0.157(9) 0.117(7) 0.172(9) -0.013(7) 0.088(7) -0.017(7) C55 0.212(10) 0.140(9) 0.175(10) 0.003(8) 0.074(8) 0.015(8) C56 0.196(9) 0.090(7) 0.156(9) -0.002(7) 0.051(7) 0.004(7) C57 0.066(5) 0.071(5) 0.069(5) 0.004(4) 0.017(4) 0.003(4) C58 0.090(7) 0.141(7) 0.083(6) 0.011(5) 0.022(5) 0.027(6) C59 0.088(7) 0.135(7) 0.103(7) 0.015(6) 0.035(5) 0.038(5) C60 0.085(6) 0.090(5) 0.093(6) 0.003(5) 0.040(5) 0.012(5) C61 0.124(8) 0.157(8) 0.097(7) 0.018(6) 0.048(6) 0.038(7) C62 0.100(7) 0.140(7) 0.110(7) 0.019(6) 0.042(6) 0.039(6) C63 0.060(5) 0.062(4) 0.090(6) 0.004(4) 0.018(4) 0.002(4) C64 0.080(6) 0.071(5) 0.095(6) 0.010(4) 0.009(5) -0.006(4) C65 0.102(6) 0.075(6) 0.119(7) 0.029(5) 0.014(5) -0.001(5) C66 0.094(6) 0.074(5) 0.121(7) 0.008(6) 0.016(5) -0.001(5) C67 0.071(6) 0.075(5) 0.103(6) -0.016(5) 0.020(5) 0.003(4) C68 0.071(5) 0.065(5) 0.092(6) 0.000(4) 0.022(4) 0.005(4) C69 0.068(5) 0.060(4) 0.097(6) -0.010(4) 0.020(5) -0.002(4) C70 0.082(6) 0.083(5) 0.115(7) 0.017(5) 0.019(5) 0.011(5) C71 0.105(7) 0.106(7) 0.156(8) 0.012(7) 0.016(6) 0.003(6) C72 0.102(7) 0.076(6) 0.158(9) 0.005(6) 0.008(7) -0.005(5) C73 0.101(7) 0.080(6) 0.177(9) -0.043(6) 0.033(7) -0.001(5) C74 0.085(6) 0.081(5) 0.139(7) -0.029(5) 0.018(5) 0.001(5) C75 0.069(6) 0.049(4) 0.095(7) 0.008(5) 0.010(5) -0.005(4) C76 0.097(8) 0.084(6) 0.087(7) 0.008(5) -0.001(6) -0.015(6) C77 0.093(8) 0.079(6) 0.112(9) 0.026(6) 0.014(6) -0.023(5) C78 0.063(6) 0.058(5) 0.120(9) 0.003(5) -0.003(6) -0.002(4) C79 0.083(7) 0.070(6) 0.114(8) -0.021(5) 0.003(6) -0.012(5) C80 0.072(6) 0.063(5) 0.097(7) -0.011(5) 0.014(5) -0.007(4) C81 0.072(6) 0.051(5) 0.105(8) 0.002(5) -0.003(5) -0.010(4) C82 0.083(7) 0.062(5) 0.095(8) -0.001(5) 0.013(5) -0.007(5) C83 0.074(6) 0.059(5) 0.108(7) 0.007(5) 0.014(5) 0.008(5) C84 0.076(7) 0.053(5) 0.136(10) 0.002(6) 0.009(7) 0.003(5) C85 0.105(8) 0.071(6) 0.111(9) -0.008(6) 0.015(6) 0.010(6) C86 0.119(9) 0.066(6) 0.092(7) -0.003(5) 0.016(6) -0.003(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 Re C2X 1.964(10) . ? Re C1X 1.986(9) . ? Re C3X 2.061(11) . ? Re N12 2.288(6) . ? Re N11 2.288(7) . ? Re Cl1 2.559(2) . ? C1X O1 1.180(9) . ? C2X O2 1.193(10) . ? C3X O3 1.032(9) . ? N1 C1 1.400(10) . ? N1 C4 1.410(9) . ? N2 C9 1.419(10) . ? N2 C6 1.422(10) . ? N3 C11 1.404(11) . ? N3 C14 1.404(9) . ? N4 C19 1.411(11) . ? N4 C16 1.437(10) . ? C1 C20 1.461(11) . ? C1 C2 1.462(11) . ? C2 C3 1.388(11) . ? C3 C4 1.485(11) . ? C4 C5 1.447(11) . ? C5 C6 1.423(12) . ? C5 C51 1.591(10) . ? C6 C7 1.509(12) . ? C7 C8 1.383(12) . ? C8 C9 1.488(11) . ? C9 C10 1.457(11) . ? C10 C11 1.444(12) . ? C10 C57 1.525(12) . ? C11 C12 1.495(12) . ? C12 C13 1.400(12) . ? C13 C14 1.496(11) . ? C14 C15 1.458(12) . ? C15 C16 1.431(11) . ? C15 C63 1.552(11) . ? C16 C17 1.487(11) . ? C17 C18 1.384(12) . ? C18 C19 1.499(11) . ? C19 C20 1.466(12) . ? C20 C43 1.518(11) . ? N5 C24 1.410(11) . ? N5 C21 1.429(10) . ? N6 C26 1.398(10) . ? N6 C29 1.423(11) . ? N7 C31 1.423(10) . ? N7 C34 1.444(10) . ? N8 C36 1.403(10) . ? N8 C39 1.404(10) . ? C21 C40 1.424(12) . ? C21 C22 1.498(11) . ? C22 C23 1.373(12) . ? C23 C24 1.488(11) . ? C24 C25 1.435(12) . ? C25 C26 1.444(11) . ? C25 C81 1.550(12) . ? C26 C27 1.503(12) . ? C27 C28 1.389(12) . ? C28 C29 1.446(12) . ? C29 C30 1.457(12) . ? C30 C31 1.425(12) . ? C30 C75 1.547(12) . ? C31 C32 1.494(11) . ? C32 C33 1.382(11) . ? C33 C34 1.486(11) . ? C34 C35 1.433(11) . ? C35 C36 1.433(11) . ? C35 C69 1.519(12) . ? C36 C37 1.520(12) . ? C37 C38 1.396(12) . ? C38 C39 1.494(12) . ? C39 C40 1.441(11) . ? C40 C48 1.542(11) . ? N11 C45 1.379(10) . ? N11 C41 1.381(11) . ? N12 C46 1.397(10) . ? N12 C50 1.403(10) . ? C41 C42 1.434(13) . ? C42 C43 1.430(11) . ? C43 C44 1.443(11) . ? C44 C45 1.434(11) . ? C46 C47 1.440(11) . ? C47 C48 1.417(11) . ? C48 C49 1.461(12) . ? C49 C50 1.413(11) . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C57 C62 1.411(13) . ? C57 C58 1.413(13) . ? C58 C59 1.433(15) . ? C59 C60 1.368(14) . ? C60 C61 1.427(15) . ? C61 C62 1.429(15) . ? C63 C68 1.426(12) . ? C63 C64 1.456(12) . ? C64 C65 1.453(13) . ? C65 C66 1.426(14) . ? C66 C67 1.387(14) . ? C67 C68 1.457(12) . ? C69 C70 1.412(13) . ? C69 C74 1.432(13) . ? C70 C71 1.409(15) . ? C71 C72 1.416(18) . ? C72 C73 1.363(16) . ? C73 C74 1.494(16) . ? C75 C80 1.411(12) . ? C75 C76 1.428(13) . ? C76 C77 1.432(13) . ? C77 C78 1.410(14) . ? C78 C79 1.440(14) . ? C79 C80 1.432(12) . ? C81 C82 1.402(13) . ? C81 C86 1.438(14) . ? C82 C83 1.441(12) . ? C83 C84 1.404(14) . ? C84 C85 1.439(15) . ? C85 C86 1.400(14) . ? C92 C91 1.570(14) . ? C91 O10 1.421(15) . ? O10 C93 1.463(15) . ? C93 C94 1.433(17) . ? C96 C95 1.558(19) . ? C95 O20 1.469(15) . ? O20 C97 1.431(15) . ? C97 C98 1.359(18) . ? 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 C2X Re C1X 88.2(4) . . ? C2X Re C3X 91.2(3) . . ? C1X Re C3X 88.5(3) . . ? C2X Re N12 95.2(3) . . ? C1X Re N12 176.5(3) . . ? C3X Re N12 90.8(3) . . ? C2X Re N11 176.4(3) . . ? C1X Re N11 93.6(3) . . ? C3X Re N11 92.0(3) . . ? N12 Re N11 83.0(2) . . ? C2X Re Cl1 90.2(2) . . ? C1X Re Cl1 95.4(2) . . ? C3X Re Cl1 175.8(2) . . ? N12 Re Cl1 85.14(17) . . ? N11 Re Cl1 86.50(17) . . ? O1 C1X Re 177.5(6) . . ? O2 C2X Re 177.6(8) . . ? O3 C3X Re 177.5(8) . . ? C1 N1 C4 108.2(6) . . ? C9 N2 C6 107.9(6) . . ? C11 N3 C14 108.7(7) . . ? C19 N4 C16 107.2(6) . . ? N1 C1 C20 125.9(7) . . ? N1 C1 C2 108.7(6) . . ? C20 C1 C2 125.1(7) . . ? C3 C2 C1 108.2(7) . . ? C2 C3 C4 106.9(7) . . ? N1 C4 C5 126.6(7) . . ? N1 C4 C3 108.1(6) . . ? C5 C4 C3 125.3(7) . . ? C6 C5 C4 124.3(7) . . ? C6 C5 C51 118.1(7) . . ? C4 C5 C51 117.5(7) . . ? N2 C6 C5 126.2(7) . . ? N2 C6 C7 107.7(7) . . ? C5 C6 C7 126.1(7) . . ? C8 C7 C6 107.7(7) . . ? C7 C8 C9 107.8(7) . . ? N2 C9 C10 126.5(7) . . ? N2 C9 C8 108.8(7) . . ? C10 C9 C8 124.7(8) . . ? C11 C10 C9 125.1(8) . . ? C11 C10 C57 118.8(7) . . ? C9 C10 C57 116.1(7) . . ? N3 C11 C10 128.0(7) . . ? N3 C11 C12 108.5(7) . . ? C10 C11 C12 123.5(8) . . ? C13 C12 C11 107.1(8) . . ? C12 C13 C14 107.2(7) . . ? N3 C14 C15 125.6(7) . . ? N3 C14 C13 108.4(7) . . ? C15 C14 C13 126.0(7) . . ? C16 C15 C14 124.7(7) . . ? C16 C15 C63 116.7(7) . . ? C14 C15 C63 118.6(7) . . ? C15 C16 N4 125.3(7) . . ? C15 C16 C17 126.7(7) . . ? N4 C16 C17 107.9(7) . . ? C18 C17 C16 108.7(7) . . ? C17 C18 C19 106.7(8) . . ? N4 C19 C20 126.4(7) . . ? N4 C19 C18 109.3(7) . . ? C20 C19 C18 124.3(8) . . ? C1 C20 C19 125.4(8) . . ? C1 C20 C43 116.1(6) . . ? C19 C20 C43 118.4(6) . . ? C24 N5 C21 108.7(6) . . ? C26 N6 C29 107.0(7) . . ? C31 N7 C34 108.9(6) . . ? C36 N8 C39 109.0(6) . . ? C40 C21 N5 125.9(7) . . ? C40 C21 C22 127.2(7) . . ? N5 C21 C22 106.9(7) . . ? C23 C22 C21 108.3(7) . . ? C22 C23 C24 108.2(7) . . ? N5 C24 C25 126.7(7) . . ? N5 C24 C23 108.0(7) . . ? C25 C24 C23 125.3(8) . . ? C24 C25 C26 125.3(8) . . ? C24 C25 C81 116.8(7) . . ? C26 C25 C81 117.8(8) . . ? N6 C26 C25 127.3(8) . . ? N6 C26 C27 109.0(7) . . ? C25 C26 C27 123.5(8) . . ? C28 C27 C26 106.0(8) . . ? C27 C28 C29 108.7(8) . . ? N6 C29 C28 109.3(7) . . ? N6 C29 C30 124.6(8) . . ? C28 C29 C30 126.0(8) . . ? C31 C30 C29 126.0(7) . . ? C31 C30 C75 116.7(7) . . ? C29 C30 C75 117.3(8) . . ? N7 C31 C30 125.5(7) . . ? N7 C31 C32 107.4(7) . . ? C30 C31 C32 127.1(7) . . ? C33 C32 C31 108.0(7) . . ? C32 C33 C34 109.2(7) . . ? C35 C34 N7 126.7(7) . . ? C35 C34 C33 126.7(8) . . ? N7 C34 C33 106.5(7) . . ? C34 C35 C36 124.8(7) . . ? C34 C35 C69 118.1(7) . . ? C36 C35 C69 117.0(7) . . ? N8 C36 C35 129.3(7) . . ? N8 C36 C37 108.1(6) . . ? C35 C36 C37 122.5(7) . . ? C38 C37 C36 106.6(8) . . ? C37 C38 C39 107.7(7) . . ? N8 C39 C40 126.1(7) . . ? N8 C39 C38 108.6(7) . . ? C40 C39 C38 125.3(7) . . ? C21 C40 C39 125.2(7) . . ? C21 C40 C48 119.8(7) . . ? C39 C40 C48 115.0(7) . . ? C45 N11 C41 117.8(7) . . ? C45 N11 Re 118.9(6) . . ? C41 N11 Re 122.9(5) . . ? C46 N12 C50 117.1(7) . . ? C46 N12 Re 119.9(6) . . ? C50 N12 Re 123.0(5) . . ? N11 C41 C42 122.8(7) . . ? C43 C42 C41 120.3(8) . . ? C42 C43 C44 116.2(7) . . ? C42 C43 C20 124.3(7) . . ? C44 C43 C20 119.4(7) . . ? C45 C44 C43 120.5(7) . . ? N11 C45 C44 122.4(8) . . ? N12 C46 C47 122.0(8) . . ? C48 C47 C46 121.3(8) . . ? C47 C48 C49 116.1(7) . . ? C47 C48 C40 119.6(7) . . ? C49 C48 C40 124.3(8) . . ? C50 C49 C48 120.2(8) . . ? N12 C50 C49 123.2(7) . . ? C52 C51 C56 120.0 . . ? C52 C51 C5 120.5(7) . . ? C56 C51 C5 119.5(7) . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C55 C54 C53 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C51 120.0 . . ? C62 C57 C58 116.5(8) . . ? C62 C57 C10 121.2(8) . . ? C58 C57 C10 122.2(8) . . ? C57 C58 C59 121.4(10) . . ? C60 C59 C58 121.5(9) . . ? C59 C60 C61 118.7(9) . . ? C60 C61 C62 119.6(10) . . ? C57 C62 C61 122.0(10) . . ? C68 C63 C64 118.4(8) . . ? C68 C63 C15 121.3(7) . . ? C64 C63 C15 120.3(8) . . ? C65 C64 C63 119.4(9) . . ? C66 C65 C64 120.6(10) . . ? C67 C66 C65 120.1(9) . . ? C66 C67 C68 120.8(9) . . ? C63 C68 C67 120.6(8) . . ? C70 C69 C74 118.6(9) . . ? C70 C69 C35 120.2(8) . . ? C74 C69 C35 120.7(9) . . ? C71 C70 C69 124.1(11) . . ? C70 C71 C72 115.3(13) . . ? C73 C72 C71 126.0(12) . . ? C72 C73 C74 117.4(11) . . ? C69 C74 C73 118.7(11) . . ? C80 C75 C76 118.3(8) . . ? C80 C75 C30 122.2(8) . . ? C76 C75 C30 119.5(8) . . ? C75 C76 C77 121.6(10) . . ? C78 C77 C76 119.9(10) . . ? C77 C78 C79 118.9(9) . . ? C80 C79 C78 120.4(9) . . ? C75 C80 C79 120.8(9) . . ? C82 C81 C86 117.6(8) . . ? C82 C81 C25 121.8(9) . . ? C86 C81 C25 120.5(9) . . ? C81 C82 C83 121.9(9) . . ? C84 C83 C82 118.8(10) . . ? C83 C84 C85 120.7(9) . . ? C86 C85 C84 118.9(10) . . ? C85 C86 C81 122.1(10) . . ? O10 C91 C92 136.4(16) . . ? C91 O10 C93 110.1(19) . . ? C94 C93 O10 96(2) . . ? O20 C95 C96 115(2) . . ? C97 O20 C95 92.6(18) . . ? C98 C97 O20 160(3) . . ? 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 C2X Re C1X O1 -117(17) . . . . ? C3X Re C1X O1 -25(17) . . . . ? N12 Re C1X O1 54(20) . . . . ? N11 Re C1X O1 66(17) . . . . ? Cl1 Re C1X O1 153(17) . . . . ? C1X Re C2X O2 -51(18) . . . . ? C3X Re C2X O2 -139(18) . . . . ? N12 Re C2X O2 130(18) . . . . ? N11 Re C2X O2 69(20) . . . . ? Cl1 Re C2X O2 44(18) . . . . ? C2X Re C3X O3 67(20) . . . . ? C1X Re C3X O3 -21(20) . . . . ? N12 Re C3X O3 163(20) . . . . ? N11 Re C3X O3 -114(20) . . . . ? Cl1 Re C3X O3 177(100) . . . . ? C4 N1 C1 C20 -171.6(8) . . . . ? C4 N1 C1 C2 1.8(9) . . . . ? N1 C1 C2 C3 -1.4(9) . . . . ? C20 C1 C2 C3 172.0(8) . . . . ? C1 C2 C3 C4 0.5(9) . . . . ? C1 N1 C4 C5 178.1(8) . . . . ? C1 N1 C4 C3 -1.5(9) . . . . ? C2 C3 C4 N1 0.6(9) . . . . ? C2 C3 C4 C5 -178.9(8) . . . . ? N1 C4 C5 C6 5.3(14) . . . . ? C3 C4 C5 C6 -175.2(8) . . . . ? N1 C4 C5 C51 -171.8(8) . . . . ? C3 C4 C5 C51 7.7(13) . . . . ? C9 N2 C6 C5 178.3(8) . . . . ? C9 N2 C6 C7 -0.8(9) . . . . ? C4 C5 C6 N2 -0.5(15) . . . . ? C51 C5 C6 N2 176.6(8) . . . . ? C4 C5 C6 C7 178.5(8) . . . . ? C51 C5 C6 C7 -4.4(13) . . . . ? N2 C6 C7 C8 0.7(10) . . . . ? C5 C6 C7 C8 -178.4(9) . . . . ? C6 C7 C8 C9 -0.3(10) . . . . ? C6 N2 C9 C10 -179.8(8) . . . . ? C6 N2 C9 C8 0.7(9) . . . . ? C7 C8 C9 N2 -0.2(10) . . . . ? C7 C8 C9 C10 -179.8(8) . . . . ? N2 C9 C10 C11 -4.0(13) . . . . ? C8 C9 C10 C11 175.4(8) . . . . ? N2 C9 C10 C57 176.5(7) . . . . ? C8 C9 C10 C57 -4.0(12) . . . . ? C14 N3 C11 C10 -178.5(8) . . . . ? C14 N3 C11 C12 1.7(9) . . . . ? C9 C10 C11 N3 -4.8(14) . . . . ? C57 C10 C11 N3 174.6(8) . . . . ? C9 C10 C11 C12 175.0(8) . . . . ? C57 C10 C11 C12 -5.6(12) . . . . ? N3 C11 C12 C13 -1.2(9) . . . . ? C10 C11 C12 C13 179.0(8) . . . . ? C11 C12 C13 C14 0.2(9) . . . . ? C11 N3 C14 C15 -179.7(7) . . . . ? C11 N3 C14 C13 -1.5(9) . . . . ? C12 C13 C14 N3 0.8(9) . . . . ? C12 C13 C14 C15 178.9(8) . . . . ? N3 C14 C15 C16 2.1(13) . . . . ? C13 C14 C15 C16 -175.7(7) . . . . ? N3 C14 C15 C63 -178.3(7) . . . . ? C13 C14 C15 C63 3.9(12) . . . . ? C14 C15 C16 N4 8.0(13) . . . . ? C63 C15 C16 N4 -171.6(7) . . . . ? C14 C15 C16 C17 -175.3(8) . . . . ? C63 C15 C16 C17 5.1(12) . . . . ? C19 N4 C16 C15 174.0(7) . . . . ? C19 N4 C16 C17 -3.3(8) . . . . ? C15 C16 C17 C18 -175.3(8) . . . . ? N4 C16 C17 C18 1.9(9) . . . . ? C16 C17 C18 C19 0.1(9) . . . . ? C16 N4 C19 C20 -175.2(7) . . . . ? C16 N4 C19 C18 3.4(9) . . . . ? C17 C18 C19 N4 -2.2(10) . . . . ? C17 C18 C19 C20 176.4(8) . . . . ? N1 C1 C20 C19 -2.9(13) . . . . ? C2 C1 C20 C19 -175.3(8) . . . . ? N1 C1 C20 C43 179.0(7) . . . . ? C2 C1 C20 C43 6.7(11) . . . . ? N4 C19 C20 C1 -6.7(13) . . . . ? C18 C19 C20 C1 174.9(8) . . . . ? N4 C19 C20 C43 171.3(7) . . . . ? C18 C19 C20 C43 -7.1(12) . . . . ? C24 N5 C21 C40 -177.5(9) . . . . ? C24 N5 C21 C22 -0.5(10) . . . . ? C40 C21 C22 C23 177.3(9) . . . . ? N5 C21 C22 C23 0.4(10) . . . . ? C21 C22 C23 C24 -0.2(11) . . . . ? C21 N5 C24 C25 178.5(9) . . . . ? C21 N5 C24 C23 0.4(10) . . . . ? C22 C23 C24 N5 -0.1(11) . . . . ? C22 C23 C24 C25 -178.2(9) . . . . ? N5 C24 C25 C26 3.5(16) . . . . ? C23 C24 C25 C26 -178.7(10) . . . . ? N5 C24 C25 C81 -173.3(9) . . . . ? C23 C24 C25 C81 4.5(15) . . . . ? C29 N6 C26 C25 -175.8(10) . . . . ? C29 N6 C26 C27 0.0(11) . . . . ? C24 C25 C26 N6 -1.5(18) . . . . ? C81 C25 C26 N6 175.3(10) . . . . ? C24 C25 C26 C27 -176.7(10) . . . . ? C81 C25 C26 C27 0.1(15) . . . . ? N6 C26 C27 C28 0.9(12) . . . . ? C25 C26 C27 C28 176.8(10) . . . . ? C26 C27 C28 C29 -1.4(13) . . . . ? C26 N6 C29 C28 -0.8(12) . . . . ? C26 N6 C29 C30 178.0(10) . . . . ? C27 C28 C29 N6 1.4(13) . . . . ? C27 C28 C29 C30 -177.4(10) . . . . ? N6 C29 C30 C31 -2.3(16) . . . . ? C28 C29 C30 C31 176.3(10) . . . . ? N6 C29 C30 C75 178.2(9) . . . . ? C28 C29 C30 C75 -3.2(15) . . . . ? C34 N7 C31 C30 176.6(8) . . . . ? C34 N7 C31 C32 -1.5(9) . . . . ? C29 C30 C31 N7 -0.1(15) . . . . ? C75 C30 C31 N7 179.4(8) . . . . ? C29 C30 C31 C32 177.6(9) . . . . ? C75 C30 C31 C32 -2.9(14) . . . . ? N7 C31 C32 C33 -0.1(10) . . . . ? C30 C31 C32 C33 -178.2(9) . . . . ? C31 C32 C33 C34 1.6(10) . . . . ? C31 N7 C34 C35 178.7(8) . . . . ? C31 N7 C34 C33 2.5(9) . . . . ? C32 C33 C34 C35 -178.8(8) . . . . ? C32 C33 C34 N7 -2.5(10) . . . . ? N7 C34 C35 C36 2.1(13) . . . . ? C33 C34 C35 C36 177.5(8) . . . . ? N7 C34 C35 C69 179.0(8) . . . . ? C33 C34 C35 C69 -5.6(13) . . . . ? C39 N8 C36 C35 178.8(9) . . . . ? C39 N8 C36 C37 1.1(9) . . . . ? C34 C35 C36 N8 -3.5(14) . . . . ? C69 C35 C36 N8 179.6(8) . . . . ? C34 C35 C36 C37 173.9(8) . . . . ? C69 C35 C36 C37 -3.1(12) . . . . ? N8 C36 C37 C38 -0.8(10) . . . . ? C35 C36 C37 C38 -178.6(8) . . . . ? C36 C37 C38 C39 0.1(10) . . . . ? C36 N8 C39 C40 -178.9(8) . . . . ? C36 N8 C39 C38 -1.0(10) . . . . ? C37 C38 C39 N8 0.5(10) . . . . ? C37 C38 C39 C40 178.5(9) . . . . ? N5 C21 C40 C39 -4.8(15) . . . . ? C22 C21 C40 C39 178.8(9) . . . . ? N5 C21 C40 C48 176.0(8) . . . . ? C22 C21 C40 C48 -0.3(14) . . . . ? N8 C39 C40 C21 7.6(15) . . . . ? C38 C39 C40 C21 -170.0(9) . . . . ? N8 C39 C40 C48 -173.2(8) . . . . ? C38 C39 C40 C48 9.2(13) . . . . ? C2X Re N11 C45 118(5) . . . . ? C1X Re N11 C45 -121.8(5) . . . . ? C3X Re N11 C45 -33.2(5) . . . . ? N12 Re N11 C45 57.4(5) . . . . ? Cl1 Re N11 C45 142.9(5) . . . . ? C2X Re N11 C41 -55(5) . . . . ? C1X Re N11 C41 64.6(6) . . . . ? C3X Re N11 C41 153.2(6) . . . . ? N12 Re N11 C41 -116.2(5) . . . . ? Cl1 Re N11 C41 -30.7(5) . . . . ? C2X Re N12 C46 -132.7(6) . . . . ? C1X Re N12 C46 56(5) . . . . ? C3X Re N12 C46 136.0(6) . . . . ? N11 Re N12 C46 44.1(5) . . . . ? Cl1 Re N12 C46 -42.9(5) . . . . ? C2X Re N12 C50 44.5(6) . . . . ? C1X Re N12 C50 -126(5) . . . . ? C3X Re N12 C50 -46.8(6) . . . . ? N11 Re N12 C50 -138.6(6) . . . . ? Cl1 Re N12 C50 134.3(6) . . . . ? C45 N11 C41 C42 -1.5(10) . . . . ? Re N11 C41 C42 172.1(5) . . . . ? N11 C41 C42 C43 0.6(10) . . . . ? C41 C42 C43 C44 1.0(9) . . . . ? C41 C42 C43 C20 179.6(6) . . . . ? C1 C20 C43 C42 -111.4(8) . . . . ? C19 C20 C43 C42 70.4(9) . . . . ? C1 C20 C43 C44 67.1(9) . . . . ? C19 C20 C43 C44 -111.0(8) . . . . ? C42 C43 C44 C45 -1.7(10) . . . . ? C20 C43 C44 C45 179.7(6) . . . . ? C41 N11 C45 C44 0.8(10) . . . . ? Re N11 C45 C44 -173.1(5) . . . . ? C43 C44 C45 N11 0.8(11) . . . . ? C50 N12 C46 C47 -1.2(10) . . . . ? Re N12 C46 C47 176.2(5) . . . . ? N12 C46 C47 C48 -2.0(11) . . . . ? C46 C47 C48 C49 4.3(11) . . . . ? C46 C47 C48 C40 -175.5(7) . . . . ? C21 C40 C48 C47 -125.0(9) . . . . ? C39 C40 C48 C47 55.8(10) . . . . ? C21 C40 C48 C49 55.3(12) . . . . ? C39 C40 C48 C49 -124.0(9) . . . . ? C47 C48 C49 C50 -3.6(12) . . . . ? C40 C48 C49 C50 176.1(7) . . . . ? C46 N12 C50 C49 1.9(11) . . . . ? Re N12 C50 C49 -175.5(6) . . . . ? C48 C49 C50 N12 0.6(13) . . . . ? C6 C5 C51 C52 -83.0(9) . . . . ? C4 C5 C51 C52 94.3(9) . . . . ? C6 C5 C51 C56 98.1(9) . . . . ? C4 C5 C51 C56 -84.6(9) . . . . ? C56 C51 C52 C53 0.0 . . . . ? C5 C51 C52 C53 -178.9(7) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C51 0.0 . . . . ? C52 C51 C56 C55 0.0 . . . . ? C5 C51 C56 C55 178.9(7) . . . . ? C11 C10 C57 C62 -77.3(11) . . . . ? C9 C10 C57 C62 102.1(10) . . . . ? C11 C10 C57 C58 104.3(10) . . . . ? C9 C10 C57 C58 -76.2(11) . . . . ? C62 C57 C58 C59 -3.7(15) . . . . ? C10 C57 C58 C59 174.8(9) . . . . ? C57 C58 C59 C60 -0.8(17) . . . . ? C58 C59 C60 C61 3.4(17) . . . . ? C59 C60 C61 C62 -1.6(18) . . . . ? C58 C57 C62 C61 5.5(16) . . . . ? C10 C57 C62 C61 -173.0(10) . . . . ? C60 C61 C62 C57 -3.1(19) . . . . ? C16 C15 C63 C68 53.9(10) . . . . ? C14 C15 C63 C68 -125.7(8) . . . . ? C16 C15 C63 C64 -125.3(8) . . . . ? C14 C15 C63 C64 55.1(11) . . . . ? C68 C63 C64 C65 3.4(12) . . . . ? C15 C63 C64 C65 -177.5(8) . . . . ? C63 C64 C65 C66 -4.3(14) . . . . ? C64 C65 C66 C67 2.3(15) . . . . ? C65 C66 C67 C68 0.6(14) . . . . ? C64 C63 C68 C67 -0.5(12) . . . . ? C15 C63 C68 C67 -179.7(7) . . . . ? C66 C67 C68 C63 -1.5(13) . . . . ? C34 C35 C69 C70 111.0(9) . . . . ? C36 C35 C69 C70 -71.9(11) . . . . ? C34 C35 C69 C74 -77.5(11) . . . . ? C36 C35 C69 C74 99.7(10) . . . . ? C74 C69 C70 C71 2.6(15) . . . . ? C35 C69 C70 C71 174.4(10) . . . . ? C69 C70 C71 C72 -2.4(17) . . . . ? C70 C71 C72 C73 1.3(18) . . . . ? C71 C72 C73 C74 -0.5(18) . . . . ? C70 C69 C74 C73 -1.6(14) . . . . ? C35 C69 C74 C73 -173.3(8) . . . . ? C72 C73 C74 C69 0.6(15) . . . . ? C31 C30 C75 C80 108.6(10) . . . . ? C29 C30 C75 C80 -71.9(11) . . . . ? C31 C30 C75 C76 -72.8(11) . . . . ? C29 C30 C75 C76 106.7(10) . . . . ? C80 C75 C76 C77 -1.6(13) . . . . ? C30 C75 C76 C77 179.8(8) . . . . ? C75 C76 C77 C78 1.3(15) . . . . ? C76 C77 C78 C79 -0.9(14) . . . . ? C77 C78 C79 C80 0.7(13) . . . . ? C76 C75 C80 C79 1.4(12) . . . . ? C30 C75 C80 C79 180.0(8) . . . . ? C78 C79 C80 C75 -0.9(13) . . . . ? C24 C25 C81 C82 -94.7(11) . . . . ? C26 C25 C81 C82 88.2(11) . . . . ? C24 C25 C81 C86 86.1(11) . . . . ? C26 C25 C81 C86 -91.0(11) . . . . ? C86 C81 C82 C83 -0.6(12) . . . . ? C25 C81 C82 C83 -179.8(8) . . . . ? C81 C82 C83 C84 0.8(13) . . . . ? C82 C83 C84 C85 0.1(13) . . . . ? C83 C84 C85 C86 -1.1(14) . . . . ? C84 C85 C86 C81 1.3(14) . . . . ? C82 C81 C86 C85 -0.5(13) . . . . ? C25 C81 C86 C85 178.7(8) . . . . ? C92 C91 O10 C93 -125(2) . . . . ? C91 O10 C93 C94 138(2) . . . . ? C96 C95 O20 C97 175(2) . . . . ? C95 O20 C97 C98 130(8) . . . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 30.35 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 1.008 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.072 #===END data_15 _database_code_depnum_ccdc_archive 'CCDC 614602' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[bis(tricarbonyl-rhenium(I))-(mu-hydroxo)-(4,4'-bipyridine,N,N') ]- diethylether solvate ; _chemical_name_common ; bis(bis(tricarbonyl-rhenium(i))-(mu-hydroxo)-(4,4'- bipyridine,N,N') )-diethylether solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C32 H20 N4 O16 Re4, O C4 H 10' _chemical_formula_sum 'C36 H30 N4 O17 Re4' _chemical_formula_weight 1535.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 9.234(3) _cell_length_b 18.285(4) _cell_length_c 14.514(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.38(3) _cell_angle_gamma 90.00 _cell_volume 2430.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 9.996 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.0711 _exptl_absorpt_correction_T_max 0.3662 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Linear fit to sin(theta)/lambda - 12 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23278 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.1015 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4762 _reflns_number_gt 2782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (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^)+(0.1127P)^2^] 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 4762 _refine_ls_number_parameters 279 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1148 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.2052 _refine_ls_wR_factor_gt 0.1737 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 0.55182(7) 0.22973(3) 0.30057(5) 0.0633(3) Uani 1 1 d D . . Re2 Re 0.19145(8) 0.21834(4) 0.21674(5) 0.0660(3) Uani 1 1 d D . . O7 O 0.3639(12) 0.1633(6) 0.3046(8) 0.067(3) Uani 1 1 d D . . H71 H 0.343(3) 0.156(11) 0.356(3) 0.101 Uiso 1 1 d D . . O8 O 0.3947(13) 0.2599(6) 0.1837(9) 0.067(3) Uani 1 1 d D . . H81 H 0.41(2) 0.303(2) 0.190(13) 0.081 Uiso 1 1 d D . . N1 N 0.6054(14) 0.1428(7) 0.2027(9) 0.060(3) Uani 1 1 d . . . N2 N 0.7663(14) -0.1339(7) -0.1128(10) 0.063(3) Uani 1 1 d . . . C7 C 0.584(2) 0.0719(9) 0.2178(14) 0.079(5) Uani 1 1 d . . . H7 H 0.5415 0.0588 0.2715 0.095 Uiso 1 1 calc R . . C8 C 0.6199(18) 0.0179(8) 0.1625(14) 0.072(5) Uani 1 1 d . . . H8 H 0.6016 -0.0315 0.1777 0.087 Uiso 1 1 calc R . . C9 C 0.6822(17) 0.0335(7) 0.0842(11) 0.058(4) Uani 1 1 d . . . C10 C 0.7160(19) 0.1052(9) 0.0710(13) 0.068(4) Uani 1 1 d . . . H10 H 0.7675 0.1189 0.0211 0.082 Uiso 1 1 calc R . . C11 C 0.6757(19) 0.1563(9) 0.1294(12) 0.069(5) Uani 1 1 d . . . H11 H 0.6989 0.2058 0.1177 0.083 Uiso 1 1 calc R . . C12 C 0.822(2) -0.0668(10) -0.1175(14) 0.082(6) Uani 1 1 d . . . H12 H 0.8769 -0.0550 -0.1663 0.099 Uiso 1 1 calc R . . C13 C 0.798(2) -0.0116(10) -0.0493(15) 0.085(6) Uani 1 1 d . . . H13 H 0.8411 0.0353 -0.0527 0.103 Uiso 1 1 calc R . . C14 C 0.7151(18) -0.0264(8) 0.0204(12) 0.062(4) Uani 1 1 d . . . C15 C 0.6600(19) -0.0961(9) 0.0209(12) 0.070(5) Uani 1 1 d . . . H15 H 0.6011 -0.1090 0.0675 0.085 Uiso 1 1 calc R . . C16 C 0.687(2) -0.1480(8) -0.0436(12) 0.067(4) Uani 1 1 d . . . H16 H 0.6480 -0.1957 -0.0388 0.081 Uiso 1 1 calc R . . O1 O 0.7529(16) 0.1668(7) 0.4663(11) 0.092(4) Uani 1 1 d . . . O2 O 0.8109(14) 0.3259(7) 0.2664(10) 0.082(4) Uani 1 1 d . . . O3 O 0.4757(13) 0.3505(6) 0.4345(9) 0.078(4) Uani 1 1 d . . . O4 O -0.0613(13) 0.1353(8) 0.2838(10) 0.088(4) Uani 1 1 d . . . O5 O -0.0296(18) 0.2905(8) 0.0736(11) 0.097(4) Uani 1 1 d . . . O6 O 0.1331(14) 0.3404(8) 0.3543(10) 0.092(4) Uani 1 1 d . . . C1 C 0.674(2) 0.1913(11) 0.3994(14) 0.075(5) Uani 1 1 d . . . C2 C 0.715(2) 0.2899(9) 0.2821(13) 0.069(5) Uani 1 1 d . . . C3 C 0.5048(17) 0.3073(10) 0.3820(15) 0.075(5) Uani 1 1 d . . . C4 C 0.033(2) 0.1690(9) 0.2565(14) 0.075(5) Uani 1 1 d . . . C5 C 0.060(3) 0.2634(9) 0.1300(14) 0.077(5) Uani 1 1 d . . . C6 C 0.1555(18) 0.2958(12) 0.3018(19) 0.089(6) Uani 1 1 d . . . C1S C 1.122(5) 0.134(3) 0.534(4) 0.120(16) Uiso 0.50 1 d P . . H21 H 1.1866 0.1080 0.4967 0.180 Uiso 0.50 1 calc PR . . H22 H 1.1779 0.1706 0.5728 0.180 Uiso 0.50 1 calc PR . . H23 H 1.0440 0.1582 0.4927 0.180 Uiso 0.50 1 calc PR . . C2S C 1.063(6) 0.087(3) 0.587(4) 0.121(17) Uiso 0.50 1 d P . . H24 H 1.0162 0.0495 0.5444 0.145 Uiso 0.50 1 calc PR . . H25 H 1.1476 0.0622 0.6238 0.145 Uiso 0.50 1 calc PR . . O1S O 0.973(4) 0.0986(18) 0.646(3) 0.119(10) Uiso 0.50 1 d P . . C3S C 0.878(5) 0.055(2) 0.671(3) 0.087(11) Uiso 0.50 1 d P . . H26 H 0.9225 0.0069 0.6603 0.105 Uiso 0.50 1 calc PR . . H27 H 0.8942 0.0612 0.7395 0.105 Uiso 0.50 1 calc PR . . C4S C 0.754(6) 0.041(3) 0.659(5) 0.15(2) Uiso 0.50 1 d P . . H28 H 0.7319 0.0039 0.7047 0.231 Uiso 0.50 1 calc PR . . H29 H 0.7284 0.0209 0.5963 0.231 Uiso 0.50 1 calc PR . . H30 H 0.6961 0.0847 0.6662 0.231 Uiso 0.50 1 calc PR . . 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 0.0614(4) 0.0601(4) 0.0729(5) -0.0063(3) 0.0252(3) 0.0035(3) Re2 0.0623(4) 0.0617(4) 0.0784(5) -0.0085(3) 0.0260(4) 0.0036(3) O7 0.072(7) 0.059(6) 0.077(8) -0.005(6) 0.032(6) 0.005(5) O8 0.068(7) 0.065(6) 0.074(8) -0.007(6) 0.025(6) -0.010(6) N1 0.062(8) 0.064(7) 0.056(8) -0.005(6) 0.020(6) 0.001(6) N2 0.066(8) 0.057(7) 0.071(10) 0.008(6) 0.031(7) 0.005(6) C7 0.106(14) 0.052(9) 0.091(14) -0.004(8) 0.061(11) 0.008(9) C8 0.076(11) 0.046(8) 0.102(14) -0.002(8) 0.038(10) -0.004(7) C9 0.068(10) 0.045(7) 0.065(10) -0.005(6) 0.031(8) 0.006(7) C10 0.080(11) 0.061(9) 0.068(11) -0.006(8) 0.026(9) 0.006(8) C11 0.082(12) 0.066(9) 0.066(11) 0.006(8) 0.038(9) -0.008(8) C12 0.096(14) 0.072(11) 0.089(14) -0.012(9) 0.052(11) -0.015(10) C13 0.089(14) 0.064(10) 0.113(17) -0.001(10) 0.047(13) -0.005(9) C14 0.068(10) 0.056(8) 0.062(11) -0.001(7) 0.013(8) -0.012(7) C15 0.086(12) 0.078(11) 0.055(11) 0.007(8) 0.039(9) -0.007(9) C16 0.087(12) 0.048(8) 0.071(12) -0.001(7) 0.026(9) 0.001(8) O1 0.093(10) 0.093(9) 0.094(11) -0.002(8) 0.023(9) 0.017(8) O2 0.066(7) 0.090(9) 0.095(10) -0.017(7) 0.030(7) -0.011(7) O3 0.080(8) 0.068(7) 0.093(10) -0.023(6) 0.037(7) 0.005(6) O4 0.058(7) 0.101(9) 0.113(12) -0.008(8) 0.037(8) -0.008(7) O5 0.111(11) 0.093(9) 0.092(11) -0.006(8) 0.040(9) 0.027(9) O6 0.071(8) 0.098(9) 0.107(11) -0.050(8) 0.022(8) 0.015(7) C1 0.077(12) 0.081(11) 0.069(13) -0.016(9) 0.019(10) 0.012(10) C2 0.082(13) 0.058(9) 0.070(12) -0.012(8) 0.018(10) 0.019(9) C3 0.041(8) 0.080(11) 0.106(15) -0.008(11) 0.020(9) -0.009(8) C4 0.062(11) 0.059(9) 0.104(15) -0.013(9) 0.011(10) 0.006(8) C5 0.107(15) 0.062(10) 0.069(13) 0.000(8) 0.039(11) 0.019(10) C6 0.036(8) 0.092(13) 0.14(2) 0.004(13) 0.026(11) -0.003(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.84(2) . ? Re1 C2 1.91(2) . ? Re1 C3 1.93(2) . ? Re1 O7 2.126(11) . ? Re1 O8 2.157(13) . ? Re1 N1 2.230(12) . ? Re2 C5 1.83(2) . ? Re2 C4 1.871(19) . ? Re2 C6 1.94(2) . ? Re2 O8 2.136(11) . ? Re2 O7 2.157(12) . ? Re2 N2 2.228(13) 3_655 ? N1 C7 1.33(2) . ? N1 C11 1.338(19) . ? N2 C12 1.33(2) . ? N2 C16 1.34(2) . ? N2 Re2 2.228(13) 3_655 ? C7 C8 1.34(2) . ? C8 C9 1.37(2) . ? C9 C10 1.37(2) . ? C9 C14 1.49(2) . ? C10 C11 1.34(2) . ? C12 C13 1.45(2) . ? C13 C14 1.37(2) . ? C14 C15 1.37(2) . ? C15 C16 1.38(2) . ? O1 C1 1.22(2) . ? O2 C2 1.15(2) . ? O3 C3 1.15(2) . ? O4 C4 1.18(2) . ? O5 C5 1.19(2) . ? O6 C6 1.15(2) . ? C1S C2S 1.32(6) . ? C2S O1S 1.28(6) . ? O1S C3S 1.27(5) . ? C3S C4S 1.17(6) . ? 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 C2 85.1(8) . . ? C1 Re1 C3 88.1(8) . . ? C2 Re1 C3 84.7(6) . . ? C1 Re1 O7 100.3(7) . . ? C2 Re1 O7 173.6(6) . . ? C3 Re1 O7 98.9(5) . . ? C1 Re1 O8 171.9(7) . . ? C2 Re1 O8 101.9(6) . . ? C3 Re1 O8 96.5(7) . . ? O7 Re1 O8 72.5(4) . . ? C1 Re1 N1 93.5(6) . . ? C2 Re1 N1 94.4(6) . . ? C3 Re1 N1 178.1(7) . . ? O7 Re1 N1 81.9(4) . . ? O8 Re1 N1 82.1(5) . . ? C5 Re2 C4 87.3(9) . . ? C5 Re2 C6 87.5(8) . . ? C4 Re2 C6 87.2(7) . . ? C5 Re2 O8 102.2(7) . . ? C4 Re2 O8 170.0(6) . . ? C6 Re2 O8 96.3(6) . . ? C5 Re2 O7 172.5(6) . . ? C4 Re2 O7 98.0(6) . . ? C6 Re2 O7 98.0(7) . . ? O8 Re2 O7 72.3(4) . . ? C5 Re2 N2 90.3(6) . 3_655 ? C4 Re2 N2 95.0(6) . 3_655 ? C6 Re2 N2 176.8(8) . 3_655 ? O8 Re2 N2 81.9(4) . 3_655 ? O7 Re2 N2 84.1(5) . 3_655 ? Re1 O7 Re2 105.1(5) . . ? Re2 O8 Re1 104.7(5) . . ? C7 N1 C11 114.0(14) . . ? C7 N1 Re1 122.6(11) . . ? C11 N1 Re1 123.0(11) . . ? C12 N2 C16 117.7(14) . . ? C12 N2 Re2 120.1(11) . 3_655 ? C16 N2 Re2 122.3(10) . 3_655 ? N1 C7 C8 124.5(16) . . ? C7 C8 C9 120.3(15) . . ? C10 C9 C8 116.4(14) . . ? C10 C9 C14 123.3(14) . . ? C8 C9 C14 120.2(13) . . ? C11 C10 C9 119.4(16) . . ? N1 C11 C10 125.0(16) . . ? N2 C12 C13 120.9(16) . . ? C14 C13 C12 120.9(16) . . ? C15 C14 C13 115.5(16) . . ? C15 C14 C9 125.0(15) . . ? C13 C14 C9 119.4(14) . . ? C14 C15 C16 122.4(15) . . ? N2 C16 C15 122.7(15) . . ? O1 C1 Re1 178.6(16) . . ? O2 C2 Re1 176.6(17) . . ? O3 C3 Re1 176.0(18) . . ? O4 C4 Re2 176.4(16) . . ? O5 C5 Re2 177.4(19) . . ? O6 C6 Re2 178(2) . . ? O1S C2S C1S 129(5) . . ? C3S O1S C2S 128(4) . . ? C4S C3S O1S 143(6) . . ? 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 C1 Re1 O7 Re2 165.8(6) . . . . ? C2 Re1 O7 Re2 -47(5) . . . . ? C3 Re1 O7 Re2 76.2(7) . . . . ? O8 Re1 O7 Re2 -17.8(4) . . . . ? N1 Re1 O7 Re2 -102.1(5) . . . . ? C5 Re2 O7 Re1 61(5) . . . . ? C4 Re2 O7 Re1 -164.4(6) . . . . ? C6 Re2 O7 Re1 -76.1(7) . . . . ? O8 Re2 O7 Re1 18.0(4) . . . . ? N2 Re2 O7 Re1 101.4(5) 3_655 . . . ? C5 Re2 O8 Re1 167.4(6) . . . . ? C4 Re2 O8 Re1 -32(4) . . . . ? C6 Re2 O8 Re1 78.6(8) . . . . ? O7 Re2 O8 Re1 -17.7(4) . . . . ? N2 Re2 O8 Re1 -104.1(5) 3_655 . . . ? C1 Re1 O8 Re2 44(4) . . . . ? C2 Re1 O8 Re2 -165.2(6) . . . . ? C3 Re1 O8 Re2 -79.3(6) . . . . ? O7 Re1 O8 Re2 18.0(4) . . . . ? N1 Re1 O8 Re2 101.9(5) . . . . ? C1 Re1 N1 C7 58.0(16) . . . . ? C2 Re1 N1 C7 143.4(16) . . . . ? C3 Re1 N1 C7 -156(17) . . . . ? O7 Re1 N1 C7 -41.9(15) . . . . ? O8 Re1 N1 C7 -115.2(15) . . . . ? C1 Re1 N1 C11 -114.4(15) . . . . ? C2 Re1 N1 C11 -29.0(15) . . . . ? C3 Re1 N1 C11 31(18) . . . . ? O7 Re1 N1 C11 145.7(14) . . . . ? O8 Re1 N1 C11 72.4(14) . . . . ? C11 N1 C7 C8 -4(3) . . . . ? Re1 N1 C7 C8 -177.6(16) . . . . ? N1 C7 C8 C9 0(3) . . . . ? C7 C8 C9 C10 5(3) . . . . ? C7 C8 C9 C14 -177.1(18) . . . . ? C8 C9 C10 C11 -6(3) . . . . ? C14 C9 C10 C11 176.6(17) . . . . ? C7 N1 C11 C10 4(3) . . . . ? Re1 N1 C11 C10 176.9(15) . . . . ? C9 C10 C11 N1 1(3) . . . . ? C16 N2 C12 C13 1(3) . . . . ? Re2 N2 C12 C13 -178.5(15) 3_655 . . . ? N2 C12 C13 C14 -2(3) . . . . ? C12 C13 C14 C15 1(3) . . . . ? C12 C13 C14 C9 -174.5(18) . . . . ? C10 C9 C14 C15 -167.3(17) . . . . ? C8 C9 C14 C15 15(3) . . . . ? C10 C9 C14 C13 8(3) . . . . ? C8 C9 C14 C13 -169.6(17) . . . . ? C13 C14 C15 C16 0(3) . . . . ? C9 C14 C15 C16 175.9(18) . . . . ? C12 N2 C16 C15 1(3) . . . . ? Re2 N2 C16 C15 -179.8(14) 3_655 . . . ? C14 C15 C16 N2 -2(3) . . . . ? C2 Re1 C1 O1 98(78) . . . . ? C3 Re1 C1 O1 13(78) . . . . ? O7 Re1 C1 O1 -85(78) . . . . ? O8 Re1 C1 O1 -111(77) . . . . ? N1 Re1 C1 O1 -168(78) . . . . ? C1 Re1 C2 O2 149(23) . . . . ? C3 Re1 C2 O2 -123(23) . . . . ? O7 Re1 C2 O2 1(27) . . . . ? O8 Re1 C2 O2 -27(23) . . . . ? N1 Re1 C2 O2 55(23) . . . . ? C1 Re1 C3 O3 -46(22) . . . . ? C2 Re1 C3 O3 -132(22) . . . . ? O7 Re1 C3 O3 54(22) . . . . ? O8 Re1 C3 O3 127(22) . . . . ? N1 Re1 C3 O3 168(15) . . . . ? C5 Re2 C4 O4 161(28) . . . . ? C6 Re2 C4 O4 -111(28) . . . . ? O8 Re2 C4 O4 0(31) . . . . ? O7 Re2 C4 O4 -14(28) . . . . ? N2 Re2 C4 O4 71(28) 3_655 . . . ? C4 Re2 C5 O5 -25(35) . . . . ? C6 Re2 C5 O5 -113(35) . . . . ? O8 Re2 C5 O5 151(35) . . . . ? O7 Re2 C5 O5 110(34) . . . . ? N2 Re2 C5 O5 70(35) 3_655 . . . ? C5 Re2 C6 O6 124(50) . . . . ? C4 Re2 C6 O6 36(50) . . . . ? O8 Re2 C6 O6 -134(50) . . . . ? O7 Re2 C6 O6 -61(50) . . . . ? N2 Re2 C6 O6 169(43) 3_655 . . . ? C1S C2S O1S C3S 152(6) . . . . ? C2S O1S C3S C4S -100(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.693 _refine_diff_density_min -1.587 _refine_diff_density_rms 0.285