Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bala Manimaran' 'T. Rajendran' 'Yi-Long Lu' 'Gene-Hsiang Lee' 'Shie-Ming Peng' 'Kuang-Lieh Lu' _publ_contact_author_name 'Prof Kuang-Lieh Lu' _publ_contact_author_address ; Prof Kuang-Lieh Lu Institute of Chemistry Academia Sinica Taipei 115 TAIWAN ; _publ_contact_author_email 'lu@chem.sinica.edu.tw' data_ic7187 _database_code_CSD 156620 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C68 H68 N4 O16 Re4' _chemical_formula_weight 1942.06 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.2304(1) _cell_length_b 23.5898(1) _cell_length_c 15.9339(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.796(1) _cell_angle_gamma 90.00 _cell_volume 3428.69(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method ? _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 7.106 _exptl_absorpt_correction_type ' empirical used sadabs' _exptl_absorpt_correction_T_min 0.3533 _exptl_absorpt_correction_T_max 0.4921 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24951 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7796 _reflns_number_observed 6802 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+2.5488P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00083(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7796 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_obs 0.0379 _refine_ls_wR_factor_all 0.0699 _refine_ls_wR_factor_obs 0.0658 _refine_ls_goodness_of_fit_all 1.206 _refine_ls_goodness_of_fit_obs 1.221 _refine_ls_restrained_S_all 1.206 _refine_ls_restrained_S_obs 1.221 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re -0.04881(2) 0.723100(8) 0.435956(12) 0.01792(6) Uani 1 d . . Re2 Re 0.31647(2) 0.733692(8) 0.506839(13) 0.01855(6) Uani 1 d . . O1 O -0.1068(4) 0.8008(2) 0.5824(2) 0.0368(10) Uani 1 d . . O2 O -0.2809(5) 0.7894(2) 0.3161(3) 0.0389(10) Uani 1 d . . O3 O -0.2968(4) 0.6477(2) 0.4816(3) 0.0356(10) Uani 1 d . . O4 O 0.2526(4) 0.8056(2) 0.6574(2) 0.0327(9) Uani 1 d . . O5 O 0.5677(4) 0.8151(2) 0.4871(3) 0.0404(10) Uani 1 d . . O6 O 0.5473(5) 0.6806(2) 0.6433(3) 0.0457(11) Uani 1 d . . O7 O 0.1464(4) 0.76559(13) 0.4105(2) 0.0192(7) Uani 1 d . . O8 O 0.1311(4) 0.67775(14) 0.5091(2) 0.0199(7) Uani 1 d . . N1 N -0.0006(4) 0.6671(2) 0.3318(3) 0.0196(9) Uani 1 d . . N2 N 0.3692(4) 0.6762(2) 0.4047(3) 0.0190(9) Uani 1 d . . C1 C -0.0841(6) 0.7716(2) 0.5277(3) 0.0227(11) Uani 1 d . . C2 C -0.1925(6) 0.7644(2) 0.3613(3) 0.0252(12) Uani 1 d . . C3 C -0.2043(6) 0.6764(2) 0.4634(3) 0.0242(11) Uani 1 d . . C4 C 0.2730(6) 0.7795(2) 0.5988(3) 0.0224(11) Uani 1 d . . C5 C 0.4718(6) 0.7846(2) 0.4930(4) 0.0287(12) Uani 1 d . . C6 C 0.4587(6) 0.6985(2) 0.5905(3) 0.0272(12) Uani 1 d . . C7 C -0.0389(6) 0.6118(2) 0.3275(3) 0.0250(12) Uani 1 d . . H7A H -0.0913(6) 0.5969(2) 0.3694(3) 0.030 Uiso 1 calc R . C8 C -0.0048(6) 0.5761(2) 0.2646(3) 0.0266(12) Uani 1 d . . H8A H -0.0346(6) 0.5375(2) 0.2640(3) 0.032 Uiso 1 calc R . C9 C 0.0727(5) 0.5959(2) 0.2019(3) 0.0208(11) Uani 1 d . . C10 C 0.1073(5) 0.6534(2) 0.2051(3) 0.0209(11) Uani 1 d . . H10A H 0.1569(5) 0.6696(2) 0.1629(3) 0.025 Uiso 1 calc R . C11 C 0.0697(5) 0.6870(2) 0.2694(3) 0.0217(11) Uani 1 d . . H11A H 0.0946(5) 0.7261(2) 0.2699(3) 0.026 Uiso 1 calc R . C12 C 0.1132(6) 0.5573(2) 0.1368(3) 0.0239(11) Uani 1 d . . H12A H 0.0770(6) 0.5195(2) 0.1355(3) 0.029 Uiso 1 calc R . C13 C 0.1978(6) 0.5719(2) 0.0793(3) 0.0228(11) Uani 1 d . . H13A H 0.2323(6) 0.6099(2) 0.0816(3) 0.027 Uiso 1 calc R . C14 C 0.2434(6) 0.5360(2) 0.0131(3) 0.0225(11) Uani 1 d . . C15 C 0.1991(6) 0.4795(2) 0.0006(3) 0.0249(12) Uani 1 d . . H15A H 0.1343(6) 0.4633(2) 0.0350(3) 0.030 Uiso 1 calc R . C16 C 0.2486(6) 0.4470(2) -0.0613(3) 0.0255(12) Uani 1 d . . H16A H 0.2166(6) 0.4088(2) -0.0690(3) 0.031 Uiso 1 calc R . C17 C 0.3445(6) 0.4689(2) -0.1129(3) 0.0264(12) Uani 1 d . . C18 C 0.3862(7) 0.5259(2) -0.1021(4) 0.0341(14) Uani 1 d . . H18A H 0.4488(7) 0.5424(2) -0.1375(4) 0.041 Uiso 1 calc R . C19 C 0.3357(6) 0.5583(2) -0.0392(4) 0.0339(14) Uani 1 d . . H19A H 0.3656(6) 0.5968(2) -0.0322(4) 0.041 Uiso 1 calc R . C20 C 0.3967(6) 0.4307(2) -0.1746(3) 0.0294(13) Uani 1 d . . H20A H 0.3616(6) 0.3928(2) -0.1751(3) 0.035 Uiso 1 calc R . C21 C 0.5136(6) 0.5577(2) 0.2296(3) 0.0279(12) Uani 1 d . . H21A H 0.4781(6) 0.5200(2) 0.2312(3) 0.034 Uiso 1 calc R . C22 C 0.4648(5) 0.5993(2) 0.2885(3) 0.0229(11) Uani 1 d . . C23 C 0.3889(6) 0.5818(2) 0.3530(3) 0.0260(12) Uani 1 d . . H23A H 0.3673(6) 0.5427(2) 0.3586(3) 0.031 Uiso 1 calc R . C24 C 0.3445(6) 0.6203(2) 0.4090(3) 0.0244(11) Uani 1 d . . H24A H 0.2941(6) 0.6067(2) 0.4526(3) 0.029 Uiso 1 calc R . C25 C 0.4894(6) 0.6577(2) 0.2840(3) 0.0247(12) Uani 1 d . . H25A H 0.5396(6) 0.6724(2) 0.2410(3) 0.030 Uiso 1 calc R . C26 C 0.4407(5) 0.6939(2) 0.3419(3) 0.0233(11) Uani 1 d . . H26A H 0.4586(5) 0.7334(2) 0.3371(3) 0.028 Uiso 1 calc R . C27 C 0.1347(6) 0.8245(2) 0.3851(3) 0.0257(12) Uani 1 d . . H27A H 0.1458(6) 0.8487(2) 0.4365(3) 0.031 Uiso 1 calc R . H27B H 0.0359(6) 0.8314(2) 0.3528(3) 0.031 Uiso 1 calc R . C28 C 0.2494(6) 0.8415(2) 0.3307(4) 0.0291(12) Uani 1 d . . H28A H 0.2506(6) 0.8131(2) 0.2851(4) 0.035 Uiso 1 calc R . H28B H 0.3473(6) 0.8414(2) 0.3662(4) 0.035 Uiso 1 calc R . C29 C 0.2196(7) 0.8999(2) 0.2911(4) 0.0331(13) Uani 1 d . . H29A H 0.2220(7) 0.9284(2) 0.3369(4) 0.040 Uiso 1 calc R . H29B H 0.1201(7) 0.9003(2) 0.2574(4) 0.040 Uiso 1 calc R . C30 C 0.3314(8) 0.9163(3) 0.2336(5) 0.054(2) Uani 1 d . . H30A H 0.3078(8) 0.9541(3) 0.2096(5) 0.081 Uiso 1 calc R . H30B H 0.3280(8) 0.8887(3) 0.1874(5) 0.081 Uiso 1 calc R . H30C H 0.4299(8) 0.9168(3) 0.2668(5) 0.081 Uiso 1 calc R . C31 C 0.1067(6) 0.6548(2) 0.5903(4) 0.0309(13) Uani 1 d . . H31A H 0.0013(6) 0.6459(2) 0.5876(4) 0.037 Uiso 1 calc R . H31B H 0.1324(6) 0.6840(2) 0.6348(4) 0.037 Uiso 1 calc R . C32 C 0.1966(7) 0.6014(2) 0.6150(4) 0.0374(14) Uani 1 d . . H32A H 0.2999(7) 0.6085(2) 0.6083(4) 0.045 Uiso 1 calc R . H32B H 0.1941(7) 0.5929(2) 0.6757(4) 0.045 Uiso 1 calc R . C33 C 0.1403(7) 0.5502(2) 0.5618(4) 0.040(2) Uani 1 d . . H33A H 0.1164(7) 0.5618(2) 0.5016(4) 0.048 Uiso 1 calc R . H33B H 0.0489(7) 0.5365(2) 0.5803(4) 0.048 Uiso 1 calc R . C34 C 0.2529(8) 0.5014(3) 0.5692(5) 0.061(2) Uani 1 d . . H34A H 0.2119(8) 0.4695(3) 0.5339(5) 0.091 Uiso 1 calc R . H34B H 0.2754(8) 0.4892(3) 0.6285(5) 0.091 Uiso 1 calc R . H34C H 0.3429(8) 0.5145(3) 0.5497(5) 0.091 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01714(11) 0.02233(11) 0.01501(11) -0.00289(7) 0.00474(8) 0.00208(8) Re2 0.01764(11) 0.02361(11) 0.01477(11) -0.00338(8) 0.00365(8) 0.00266(8) O1 0.039(2) 0.043(2) 0.028(2) -0.015(2) 0.004(2) 0.013(2) O2 0.032(2) 0.047(3) 0.036(3) 0.010(2) 0.000(2) 0.010(2) O3 0.024(2) 0.045(2) 0.040(3) 0.002(2) 0.010(2) -0.004(2) O4 0.033(2) 0.038(2) 0.028(2) -0.013(2) 0.008(2) 0.003(2) O5 0.032(2) 0.056(3) 0.033(2) -0.004(2) 0.006(2) -0.015(2) O6 0.043(3) 0.054(3) 0.036(3) 0.003(2) -0.006(2) 0.015(2) O7 0.020(2) 0.021(2) 0.017(2) -0.0016(13) 0.0037(15) 0.0021(14) O8 0.018(2) 0.026(2) 0.017(2) -0.0017(14) 0.0069(15) 0.0025(14) N1 0.018(2) 0.024(2) 0.016(2) -0.001(2) 0.000(2) 0.003(2) N2 0.015(2) 0.027(2) 0.015(2) -0.003(2) 0.003(2) 0.002(2) C1 0.021(3) 0.028(3) 0.018(3) -0.002(2) 0.001(2) 0.003(2) C2 0.025(3) 0.031(3) 0.020(3) 0.000(2) 0.006(2) -0.001(2) C3 0.021(3) 0.033(3) 0.018(3) -0.006(2) 0.001(2) 0.004(2) C4 0.015(3) 0.027(3) 0.024(3) -0.002(2) 0.001(2) 0.002(2) C5 0.028(3) 0.039(3) 0.021(3) -0.005(2) 0.007(2) 0.000(2) C6 0.027(3) 0.033(3) 0.023(3) -0.005(2) 0.007(2) 0.008(2) C7 0.022(3) 0.028(3) 0.028(3) -0.002(2) 0.012(2) -0.001(2) C8 0.033(3) 0.023(3) 0.026(3) -0.004(2) 0.010(2) -0.002(2) C9 0.017(3) 0.026(3) 0.019(3) -0.004(2) 0.002(2) 0.000(2) C10 0.021(3) 0.028(3) 0.013(3) 0.002(2) 0.002(2) 0.003(2) C11 0.019(3) 0.024(3) 0.022(3) -0.002(2) 0.002(2) 0.001(2) C12 0.028(3) 0.022(3) 0.023(3) -0.008(2) 0.005(2) 0.001(2) C13 0.023(3) 0.025(3) 0.022(3) -0.008(2) 0.006(2) 0.001(2) C14 0.025(3) 0.025(3) 0.019(3) -0.006(2) 0.007(2) 0.003(2) C15 0.024(3) 0.031(3) 0.022(3) -0.001(2) 0.008(2) 0.001(2) C16 0.026(3) 0.026(3) 0.027(3) -0.004(2) 0.008(2) 0.004(2) C17 0.031(3) 0.028(3) 0.022(3) -0.007(2) 0.008(2) 0.002(2) C18 0.039(4) 0.037(3) 0.033(3) -0.005(3) 0.025(3) -0.004(3) C19 0.039(4) 0.031(3) 0.036(3) -0.007(3) 0.020(3) -0.005(3) C20 0.032(3) 0.031(3) 0.027(3) -0.004(2) 0.011(3) -0.003(2) C21 0.028(3) 0.032(3) 0.025(3) -0.004(2) 0.008(2) 0.003(2) C22 0.017(3) 0.029(3) 0.023(3) -0.004(2) 0.004(2) 0.002(2) C23 0.027(3) 0.023(3) 0.029(3) -0.004(2) 0.008(2) 0.002(2) C24 0.027(3) 0.028(3) 0.020(3) 0.001(2) 0.010(2) 0.002(2) C25 0.022(3) 0.038(3) 0.015(3) -0.001(2) 0.007(2) 0.003(2) C26 0.023(3) 0.027(3) 0.021(3) -0.003(2) 0.004(2) 0.001(2) C27 0.029(3) 0.025(3) 0.024(3) -0.001(2) 0.006(2) 0.003(2) C28 0.030(3) 0.029(3) 0.029(3) 0.000(2) 0.007(3) -0.003(2) C29 0.046(4) 0.027(3) 0.027(3) 0.000(2) 0.007(3) -0.005(3) C30 0.076(5) 0.039(4) 0.053(5) 0.007(3) 0.030(4) -0.006(4) C31 0.033(3) 0.034(3) 0.028(3) 0.002(2) 0.014(3) -0.002(2) C32 0.035(4) 0.042(4) 0.035(4) 0.009(3) 0.006(3) -0.002(3) C33 0.038(4) 0.037(3) 0.047(4) 0.012(3) 0.009(3) -0.003(3) C34 0.061(5) 0.040(4) 0.082(6) 0.016(4) 0.013(5) 0.006(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 Re1 C2 1.907(6) . ? Re1 C3 1.912(6) . ? Re1 C1 1.923(5) . ? Re1 O7 2.154(3) . ? Re1 O8 2.161(3) . ? Re1 N1 2.219(4) . ? Re2 C5 1.909(6) . ? Re2 C6 1.912(6) . ? Re2 C4 1.912(5) . ? Re2 O7 2.156(3) . ? Re2 O8 2.166(3) . ? Re2 N2 2.229(4) . ? O1 C1 1.154(6) . ? O2 C2 1.164(6) . ? O3 C3 1.160(6) . ? O4 C4 1.158(6) . ? O5 C5 1.155(7) . ? O6 C6 1.160(6) . ? O7 C27 1.447(6) . ? O8 C31 1.451(6) . ? N1 C7 1.350(6) . ? N1 C11 1.351(6) . ? N2 C24 1.340(6) . ? N2 C26 1.347(6) . ? C7 C8 1.383(7) . ? C8 C9 1.395(7) . ? C9 C10 1.393(7) . ? C9 C12 1.472(7) . ? C10 C11 1.380(7) . ? C12 C13 1.337(7) . ? C13 C14 1.463(6) . ? C14 C19 1.384(7) . ? C14 C15 1.400(7) . ? C15 C16 1.381(7) . ? C16 C17 1.395(7) . ? C17 C18 1.402(7) . ? C17 C20 1.468(7) . ? C18 C19 1.396(7) . ? C20 C21 1.323(7) 3_665 ? C21 C20 1.322(7) 3_665 ? C21 C22 1.475(7) . ? C22 C23 1.392(7) . ? C22 C25 1.400(7) . ? C23 C24 1.378(7) . ? C25 C26 1.382(7) . ? C27 C28 1.520(7) . ? C28 C29 1.523(7) . ? C29 C30 1.531(8) . ? C31 C32 1.528(8) . ? C32 C33 1.520(8) . ? C33 C34 1.544(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 C2 Re1 C3 87.8(2) . . ? C2 Re1 C1 89.3(2) . . ? C3 Re1 C1 87.0(2) . . ? C2 Re1 O7 99.6(2) . . ? C3 Re1 O7 171.9(2) . . ? C1 Re1 O7 96.3(2) . . ? C2 Re1 O8 173.1(2) . . ? C3 Re1 O8 97.7(2) . . ? C1 Re1 O8 95.2(2) . . ? O7 Re1 O8 74.68(13) . . ? C2 Re1 N1 92.1(2) . . ? C3 Re1 N1 94.1(2) . . ? C1 Re1 N1 178.2(2) . . ? O7 Re1 N1 82.36(14) . . ? O8 Re1 N1 83.29(13) . . ? C5 Re2 C6 84.6(2) . . ? C5 Re2 C4 89.0(2) . . ? C6 Re2 C4 85.0(2) . . ? C5 Re2 O7 100.2(2) . . ? C6 Re2 O7 174.6(2) . . ? C4 Re2 O7 97.6(2) . . ? C5 Re2 O8 174.1(2) . . ? C6 Re2 O8 100.6(2) . . ? C4 Re2 O8 94.2(2) . . ? O7 Re2 O8 74.53(13) . . ? C5 Re2 N2 92.7(2) . . ? C6 Re2 N2 92.4(2) . . ? C4 Re2 N2 176.8(2) . . ? O7 Re2 N2 84.80(13) . . ? O8 Re2 N2 84.41(13) . . ? C27 O7 Re1 118.1(3) . . ? C27 O7 Re2 123.3(3) . . ? Re1 O7 Re2 104.06(14) . . ? C31 O8 Re1 117.0(3) . . ? C31 O8 Re2 118.2(3) . . ? Re1 O8 Re2 103.49(14) . . ? C7 N1 C11 116.8(4) . . ? C7 N1 Re1 122.1(3) . . ? C11 N1 Re1 121.1(3) . . ? C24 N2 C26 116.7(4) . . ? C24 N2 Re2 120.2(3) . . ? C26 N2 Re2 122.7(3) . . ? O1 C1 Re1 179.3(5) . . ? O2 C2 Re1 179.5(5) . . ? O3 C3 Re1 178.5(5) . . ? O4 C4 Re2 176.2(5) . . ? O5 C5 Re2 178.0(5) . . ? O6 C6 Re2 175.7(5) . . ? N1 C7 C8 122.5(5) . . ? C7 C8 C9 120.9(5) . . ? C10 C9 C8 116.1(4) . . ? C10 C9 C12 123.2(5) . . ? C8 C9 C12 120.7(5) . . ? C11 C10 C9 120.2(5) . . ? N1 C11 C10 123.4(5) . . ? C13 C12 C9 124.2(5) . . ? C12 C13 C14 127.3(5) . . ? C19 C14 C15 118.0(5) . . ? C19 C14 C13 119.0(5) . . ? C15 C14 C13 123.0(5) . . ? C16 C15 C14 120.6(5) . . ? C15 C16 C17 121.7(5) . . ? C16 C17 C18 118.0(5) . . ? C16 C17 C20 118.0(5) . . ? C18 C17 C20 124.0(5) . . ? C19 C18 C17 119.9(5) . . ? C14 C19 C18 121.8(5) . . ? C21 C20 C17 128.3(5) 3_665 . ? C20 C21 C22 124.6(5) 3_665 . ? C23 C22 C25 115.7(5) . . ? C23 C22 C21 120.7(5) . . ? C25 C22 C21 123.6(5) . . ? C24 C23 C22 121.0(5) . . ? N2 C24 C23 123.1(5) . . ? C26 C25 C22 120.2(5) . . ? N2 C26 C25 123.3(5) . . ? O7 C27 C28 112.6(4) . . ? C27 C28 C29 112.2(5) . . ? C28 C29 C30 112.5(5) . . ? O8 C31 C32 112.7(4) . . ? C33 C32 C31 112.6(5) . . ? C32 C33 C34 112.4(6) . . ? _refine_diff_density_max 1.187 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.232 Complex [{(CO)3Re((-OC4H9)2Re(CO)3}2((-pz)2] 1a data_ic7056 _database_code_CSD 156621 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H44 N4 O16 Re4' _chemical_formula_weight 1533.55 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7043(1) _cell_length_b 16.5541(1) _cell_length_c 14.5020(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.974(1) _cell_angle_gamma 90.00 _cell_volume 2328.30(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 6502 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 2.187 _exptl_crystal_density_method ? _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 10.432 _exptl_absorpt_correction_type ' empirical used sadabs' _exptl_absorpt_correction_T_min 0.3237 _exptl_absorpt_correction_T_max 0.4920 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14671 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5288 _reflns_number_observed 4729 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+1.3674P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00048(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5287 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_obs 0.0232 _refine_ls_wR_factor_all 0.0454 _refine_ls_wR_factor_obs 0.0437 _refine_ls_goodness_of_fit_all 1.144 _refine_ls_goodness_of_fit_obs 1.167 _refine_ls_restrained_S_all 1.144 _refine_ls_restrained_S_obs 1.167 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 1.47684(2) 0.184377(9) 0.327733(10) 0.02177(5) Uani 1 d . . Re2 Re 1.232632(15) 0.041643(9) 0.289891(10) 0.02009(5) Uani 1 d . . O1 O 1.3468(4) 0.2917(2) 0.1759(2) 0.0516(9) Uani 1 d . . O2 O 1.5088(4) 0.3386(2) 0.4437(3) 0.0522(9) Uani 1 d . . O3 O 1.7610(4) 0.2219(2) 0.2519(2) 0.0528(10) Uani 1 d . . O4 O 0.9385(3) 0.0012(2) 0.3447(2) 0.0451(8) Uani 1 d . . O5 O 1.1156(4) 0.1436(2) 0.1293(2) 0.0562(10) Uani 1 d . . O6 O 1.2057(4) -0.1050(2) 0.1619(2) 0.0485(9) Uani 1 d . . O7 O 1.2840(3) 0.14230(15) 0.3791(2) 0.0214(5) Uani 1 d . . O8 O 1.4455(3) 0.0685(2) 0.2659(2) 0.0220(6) Uani 1 d . . N1 N 1.5639(3) 0.1122(2) 0.4434(2) 0.0201(6) Uani 1 d . . N2 N 1.3220(3) -0.0270(2) 0.4068(2) 0.0193(6) Uani 1 d . . C1 C 1.3953(5) 0.2490(3) 0.2319(3) 0.0344(10) Uani 1 d . . C2 C 1.4956(4) 0.2808(3) 0.3992(3) 0.0337(10) Uani 1 d . . C3 C 1.6539(5) 0.2081(3) 0.2798(3) 0.0338(10) Uani 1 d . . C4 C 1.0494(4) 0.0183(3) 0.3241(3) 0.0296(9) Uani 1 d . . C5 C 1.1599(4) 0.1063(3) 0.1896(3) 0.0331(10) Uani 1 d . . C6 C 1.2157(4) -0.0499(3) 0.2102(3) 0.0289(9) Uani 1 d . . C7 C 1.6672(4) 0.0594(2) 0.4330(3) 0.0235(8) Uani 1 d . . H7A H 1.7029(4) 0.0512(2) 0.3736(3) 0.028 Uiso 1 calc R . C8 C 1.5197(4) 0.1227(2) 0.5291(3) 0.0243(8) Uani 1 d . . H8A H 1.4476(4) 0.1602(2) 0.5391(3) 0.029 Uiso 1 calc R . C9 C 1.4239(4) -0.0808(2) 0.3970(3) 0.0230(8) Uani 1 d . . H9A H 1.4580(4) -0.0902(2) 0.3373(3) 0.028 Uiso 1 calc R . C10 C 1.2776(4) -0.0168(2) 0.4927(3) 0.0244(8) Uani 1 d . . H10A H 1.2059(4) 0.0209(2) 0.5027(3) 0.029 Uiso 1 calc R . C11 C 1.1808(4) 0.2040(3) 0.3936(3) 0.0336(10) Uani 1 d . . H11A H 1.1287(4) 0.2137(3) 0.3347(3) 0.040 Uiso 1 calc R . H11B H 1.2279(4) 0.2550(3) 0.4114(3) 0.040 Uiso 1 calc R . C12 C 1.0801(4) 0.1822(3) 0.4671(3) 0.0332(10) Uani 1 d . . H12A H 1.1291(4) 0.1804(3) 0.5281(3) 0.040 Uiso 1 calc R . H12B H 1.0413(4) 0.1279(3) 0.4542(3) 0.040 Uiso 1 calc R . C13 C 0.9637(4) 0.2438(3) 0.4695(3) 0.0391(11) Uani 1 d . . H13A H 1.0037(4) 0.2986(3) 0.4754(3) 0.047 Uiso 1 calc R . H13B H 0.9094(4) 0.2414(3) 0.4104(3) 0.047 Uiso 1 calc R . C14 C 0.8680(5) 0.2291(3) 0.5489(4) 0.058(2) Uani 1 d . . H14A H 0.7950(5) 0.2700(3) 0.5476(4) 0.087 Uiso 1 calc R . H14B H 0.9208(5) 0.2325(3) 0.6076(4) 0.087 Uiso 1 calc R . H14C H 0.8266(5) 0.1753(3) 0.5426(4) 0.087 Uiso 1 calc R . C15 C 1.4975(4) 0.0525(3) 0.1739(3) 0.0302(9) Uani 1 d . . H15A H 1.4930(4) 0.1028(3) 0.1369(3) 0.036 Uiso 1 calc R . H15B H 1.4380(4) 0.0118(3) 0.1423(3) 0.036 Uiso 1 calc R . C16 C 1.6448(4) 0.0220(3) 0.1789(3) 0.0295(9) Uani 1 d . . H16A H 1.6486(4) -0.0299(3) 0.2128(3) 0.035 Uiso 1 calc R . H16B H 1.7037(4) 0.0613(3) 0.2133(3) 0.035 Uiso 1 calc R . C17 C 1.7004(4) 0.0098(3) 0.0825(3) 0.0353(10) Uani 1 d . . H17A H 1.7031(4) 0.0624(3) 0.0502(3) 0.042 Uiso 1 calc R . H17B H 1.6378(4) -0.0264(3) 0.0465(3) 0.042 Uiso 1 calc R . C18 C 1.8454(5) -0.0268(4) 0.0875(4) 0.065(2) Uani 1 d . . H18A H 1.8784(5) -0.0340(4) 0.0249(4) 0.097 Uiso 1 calc R . H18B H 1.8426(5) -0.0793(4) 0.1186(4) 0.097 Uiso 1 calc R . H18C H 1.9079(5) 0.0094(4) 0.1222(4) 0.097 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02492(9) 0.02379(8) 0.01677(8) 0.00412(6) 0.00314(6) -0.00069(6) Re2 0.01797(8) 0.02606(8) 0.01623(8) 0.00116(6) 0.00056(5) 0.00310(6) O1 0.056(2) 0.057(2) 0.041(2) 0.030(2) 0.002(2) 0.000(2) O2 0.068(2) 0.032(2) 0.056(2) -0.012(2) 0.003(2) -0.004(2) O3 0.046(2) 0.070(2) 0.043(2) -0.013(2) 0.021(2) -0.029(2) O4 0.021(2) 0.069(2) 0.046(2) -0.008(2) 0.0086(14) -0.005(2) O5 0.072(3) 0.057(2) 0.037(2) 0.015(2) -0.021(2) 0.016(2) O6 0.057(2) 0.041(2) 0.048(2) -0.018(2) -0.003(2) -0.001(2) O7 0.0217(13) 0.0230(13) 0.0196(14) 0.0010(10) 0.0030(11) 0.0053(10) O8 0.0213(13) 0.0309(14) 0.0139(13) -0.0003(10) 0.0026(11) 0.0001(11) N1 0.021(2) 0.023(2) 0.017(2) 0.0021(12) 0.0011(13) -0.0026(12) N2 0.0174(15) 0.023(2) 0.018(2) 0.0013(12) 0.0027(12) -0.0017(12) C1 0.037(2) 0.038(2) 0.029(2) 0.011(2) 0.004(2) -0.007(2) C2 0.038(2) 0.030(2) 0.034(2) 0.006(2) 0.002(2) -0.003(2) C3 0.042(3) 0.036(2) 0.023(2) -0.003(2) 0.002(2) -0.010(2) C4 0.026(2) 0.038(2) 0.024(2) -0.005(2) -0.003(2) 0.006(2) C5 0.034(2) 0.033(2) 0.031(2) -0.002(2) -0.004(2) 0.005(2) C6 0.026(2) 0.035(2) 0.026(2) 0.002(2) -0.002(2) 0.000(2) C7 0.024(2) 0.029(2) 0.018(2) 0.000(2) 0.004(2) 0.002(2) C8 0.022(2) 0.031(2) 0.020(2) -0.001(2) 0.006(2) 0.005(2) C9 0.024(2) 0.030(2) 0.015(2) 0.0003(15) 0.006(2) 0.003(2) C10 0.022(2) 0.029(2) 0.023(2) 0.000(2) 0.005(2) 0.005(2) C11 0.033(2) 0.031(2) 0.037(3) 0.000(2) 0.007(2) 0.010(2) C12 0.031(2) 0.038(2) 0.031(2) -0.005(2) 0.005(2) 0.003(2) C13 0.029(2) 0.043(3) 0.044(3) -0.018(2) -0.005(2) 0.012(2) C14 0.037(3) 0.054(3) 0.085(4) -0.040(3) 0.025(3) -0.009(2) C15 0.030(2) 0.044(2) 0.017(2) -0.001(2) 0.009(2) -0.001(2) C16 0.031(2) 0.035(2) 0.023(2) -0.001(2) 0.007(2) 0.003(2) C17 0.033(2) 0.046(3) 0.028(2) -0.008(2) 0.012(2) -0.002(2) C18 0.040(3) 0.102(5) 0.053(4) -0.025(3) 0.016(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.905(4) . ? Re1 C2 1.908(4) . ? Re1 C3 1.916(4) . ? Re1 O8 2.135(3) . ? Re1 O7 2.154(2) . ? Re1 N1 2.204(3) . ? Re2 C4 1.902(4) . ? Re2 C6 1.909(4) . ? Re2 C5 1.921(4) . ? Re2 O8 2.153(2) . ? Re2 O7 2.157(3) . ? Re2 N2 2.194(3) . ? O1 C1 1.163(5) . ? O2 C2 1.159(5) . ? O3 C3 1.151(5) . ? O4 C4 1.162(5) . ? O5 C5 1.143(5) . ? O6 C6 1.152(5) . ? O7 C11 1.451(5) . ? O8 C15 1.468(4) . ? N1 C8 1.340(5) . ? N1 C7 1.343(5) . ? N2 C9 1.342(5) . ? N2 C10 1.343(5) . ? C7 C10 1.379(5) 3_856 ? C8 C9 1.375(5) 3_856 ? C9 C8 1.375(5) 3_856 ? C10 C7 1.379(5) 3_856 ? C11 C12 1.514(6) . ? C12 C13 1.523(6) . ? C13 C14 1.524(7) . ? C15 C16 1.515(6) . ? C16 C17 1.529(5) . ? C17 C18 1.531(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 87.5(2) . . ? C1 Re1 C3 88.6(2) . . ? C2 Re1 C3 87.5(2) . . ? C1 Re1 O8 98.6(2) . . ? C2 Re1 O8 171.55(14) . . ? C3 Re1 O8 98.51(14) . . ? C1 Re1 O7 95.16(14) . . ? C2 Re1 O7 98.65(14) . . ? C3 Re1 O7 172.93(15) . . ? O8 Re1 O7 75.03(9) . . ? C1 Re1 N1 177.1(2) . . ? C2 Re1 N1 90.74(15) . . ? C3 Re1 N1 93.6(2) . . ? O8 Re1 N1 82.98(10) . . ? O7 Re1 N1 82.89(10) . . ? C4 Re2 C6 86.2(2) . . ? C4 Re2 C5 89.3(2) . . ? C6 Re2 C5 87.8(2) . . ? C4 Re2 O8 174.19(14) . . ? C6 Re2 O8 97.42(14) . . ? C5 Re2 O8 95.32(15) . . ? C4 Re2 O7 101.51(14) . . ? C6 Re2 O7 171.58(14) . . ? C5 Re2 O7 95.48(14) . . ? O8 Re2 O7 74.58(9) . . ? C4 Re2 N2 92.37(15) . . ? C6 Re2 N2 94.58(14) . . ? C5 Re2 N2 177.16(15) . . ? O8 Re2 N2 82.87(10) . . ? O7 Re2 N2 81.95(10) . . ? C11 O7 Re1 115.8(2) . . ? C11 O7 Re2 119.0(2) . . ? Re1 O7 Re2 103.17(10) . . ? C15 O8 Re1 119.7(2) . . ? C15 O8 Re2 118.1(2) . . ? Re1 O8 Re2 103.97(10) . . ? C8 N1 C7 116.9(3) . . ? C8 N1 Re1 120.6(2) . . ? C7 N1 Re1 122.4(2) . . ? C9 N2 C10 116.3(3) . . ? C9 N2 Re2 122.3(2) . . ? C10 N2 Re2 121.4(2) . . ? O1 C1 Re1 176.8(4) . . ? O2 C2 Re1 178.8(4) . . ? O3 C3 Re1 179.1(4) . . ? O4 C4 Re2 177.7(4) . . ? O5 C5 Re2 178.9(4) . . ? O6 C6 Re2 179.8(3) . . ? N1 C7 C10 121.1(3) . 3_856 ? N1 C8 C9 121.7(3) . 3_856 ? N2 C9 C8 121.9(3) . 3_856 ? N2 C10 C7 122.1(3) . 3_856 ? O7 C11 C12 113.5(3) . . ? C11 C12 C13 110.7(4) . . ? C14 C13 C12 112.5(4) . . ? O8 C15 C16 111.7(3) . . ? C15 C16 C17 111.2(3) . . ? C16 C17 C18 111.2(4) . . ? _refine_diff_density_max 0.956 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.125 Complex [{(CO)3Re((-OC7H7)2Re(CO)3}2((-bpe)2] data_ic7344 _database_code_CSD 156622 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C64 H48 N4 O16 Re4' _chemical_formula_weight 1873.86 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.9987(2) _cell_length_b 15.8020(2) _cell_length_c 20.9551(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5959.95(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 2.088 _exptl_crystal_density_method ? _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 8.172 _exptl_absorpt_correction_type ' empirical used sadabs' _exptl_absorpt_correction_T_min 0.3171 _exptl_absorpt_correction_T_max 0.4921 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 41657 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6828 _reflns_number_observed 6267 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+17.1596P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000079(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6828 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_obs 0.0316 _refine_ls_wR_factor_all 0.0644 _refine_ls_wR_factor_obs 0.0619 _refine_ls_goodness_of_fit_all 1.109 _refine_ls_goodness_of_fit_obs 1.114 _refine_ls_restrained_S_all 1.109 _refine_ls_restrained_S_obs 1.114 _refine_ls_shift/esd_max -0.009 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.092996(9) 0.330720(11) 0.278855(9) 0.02406(6) Uani 1 d . . Re2 Re 0.191048(9) 0.375029(11) 0.414337(8) 0.02251(6) Uani 1 d . . O1 O 0.1516(2) 0.4912(2) 0.2131(2) 0.0437(9) Uani 1 d . . O2 O -0.0601(2) 0.3766(2) 0.2253(2) 0.0460(10) Uani 1 d . . O3 O 0.1103(2) 0.2422(3) 0.1498(2) 0.0483(10) Uani 1 d . . O4 O 0.3540(2) 0.3618(2) 0.4555(2) 0.0379(8) Uani 1 d . . O5 O 0.1737(2) 0.4670(3) 0.5425(2) 0.0474(10) Uani 1 d . . O6 O 0.2373(2) 0.5445(2) 0.3542(2) 0.0385(8) Uani 1 d . . O7 O 0.1962(2) 0.3024(2) 0.32744(14) 0.0250(7) Uani 1 d . . O8 O 0.0814(2) 0.3751(2) 0.3754(2) 0.0264(7) Uani 1 d . . N1 N 0.0541(2) 0.2119(2) 0.3240(2) 0.0239(8) Uani 1 d . . N2 N 0.1538(2) 0.2549(2) 0.4581(2) 0.0232(8) Uani 1 d . . C1 C 0.1297(2) 0.4323(3) 0.2393(2) 0.0296(10) Uani 1 d . . C2 C -0.0026(3) 0.3588(3) 0.2466(3) 0.0313(11) Uani 1 d . . C3 C 0.1065(2) 0.2754(3) 0.1987(3) 0.0323(11) Uani 1 d . . C4 C 0.2919(3) 0.3646(3) 0.4397(2) 0.0283(10) Uani 1 d . . C5 C 0.1780(3) 0.4328(3) 0.4939(2) 0.0312(10) Uani 1 d . . C6 C 0.2186(3) 0.4808(3) 0.3761(2) 0.0290(10) Uani 1 d . . C7 C 0.2688(3) 0.3062(6) 0.2980(3) 0.064(2) Uani 1 d . . H7A H 0.3035(3) 0.2718(6) 0.3240(3) 0.076 Uiso 1 calc R . H7B H 0.2864(3) 0.3655(6) 0.2997(3) 0.076 Uiso 1 calc R . C8 C 0.2735(3) 0.2762(4) 0.2300(2) 0.0357(12) Uani 1 d . . C9 C 0.2700(3) 0.1910(4) 0.2149(3) 0.0436(13) Uani 1 d . . H9A H 0.2663(3) 0.1505(4) 0.2483(3) 0.052 Uiso 1 calc R . C10 C 0.2717(3) 0.1639(4) 0.1529(3) 0.052(2) Uani 1 d . . H10A H 0.2673(3) 0.1055(4) 0.1429(3) 0.063 Uiso 1 calc R . C11 C 0.2801(4) 0.2242(5) 0.1045(3) 0.059(2) Uani 1 d . . H11A H 0.2802(4) 0.2063(5) 0.0612(3) 0.071 Uiso 1 calc R . C12 C 0.2880(4) 0.3078(5) 0.1182(3) 0.057(2) Uani 1 d . . H12A H 0.2963(4) 0.3475(5) 0.0849(3) 0.069 Uiso 1 calc R . C13 C 0.2839(3) 0.3342(4) 0.1807(3) 0.0472(14) Uani 1 d . . H13A H 0.2883(3) 0.3927(4) 0.1903(3) 0.057 Uiso 1 calc R . C13' C 0.0231(3) 0.4314(3) 0.3956(3) 0.0360(11) Uani 1 d . . H13B H 0.0124(3) 0.4207(3) 0.4413(3) 0.043 Uiso 1 calc R . H13C H -0.0225(3) 0.4179(3) 0.3712(3) 0.043 Uiso 1 calc R . C15 C 0.0403(3) 0.5247(3) 0.3871(3) 0.0317(11) Uani 1 d . . C16 C 0.0332(3) 0.5634(3) 0.3280(3) 0.0380(12) Uani 1 d . . H16A H 0.0160(3) 0.5318(3) 0.2923(3) 0.046 Uiso 1 calc R . C17 C 0.0513(3) 0.6489(3) 0.3210(3) 0.0414(13) Uani 1 d . . H17A H 0.0479(3) 0.6750(3) 0.2803(3) 0.050 Uiso 1 calc R . C18 C 0.0740(3) 0.6953(3) 0.3729(3) 0.0405(13) Uani 1 d . . H18A H 0.0857(3) 0.7536(3) 0.3680(3) 0.049 Uiso 1 calc R . C19 C 0.0798(3) 0.6577(4) 0.4322(3) 0.0397(12) Uani 1 d . . H19A H 0.0948(3) 0.6900(4) 0.4681(3) 0.048 Uiso 1 calc R . C20 C 0.0637(3) 0.5730(3) 0.4388(3) 0.0367(12) Uani 1 d . . H20A H 0.0687(3) 0.5471(3) 0.4794(3) 0.044 Uiso 1 calc R . C21 C -0.0115(3) 0.2078(3) 0.3547(2) 0.0335(11) Uani 1 d . . H21A H -0.0408(3) 0.2577(3) 0.3572(2) 0.040 Uiso 1 calc R . C22 C -0.0386(3) 0.1348(3) 0.3826(3) 0.0320(11) Uani 1 d . . H22A H -0.0853(3) 0.1356(3) 0.4038(3) 0.038 Uiso 1 calc R . C23 C 0.0023(2) 0.0599(3) 0.3799(2) 0.0237(9) Uani 1 d . . C24 C 0.0696(3) 0.0643(3) 0.3476(3) 0.0324(11) Uani 1 d . . H24A H 0.0998(3) 0.0152(3) 0.3439(3) 0.039 Uiso 1 calc R . C25 C 0.0931(3) 0.1399(3) 0.3207(3) 0.0310(10) Uani 1 d . . H25A H 0.1393(3) 0.1406(3) 0.2987(3) 0.037 Uiso 1 calc R . C26 C -0.0216(2) -0.0193(3) 0.4104(2) 0.0260(9) Uani 1 d . . H26A H 0.0102(2) -0.0669(3) 0.4062(2) 0.031 Uiso 1 calc R . C27 C -0.0845(2) -0.0298(3) 0.4436(2) 0.0256(9) Uani 1 d . . H27A H -0.1173(2) 0.0171(3) 0.4460(2) 0.031 Uiso 1 calc R . C28 C 0.1939(3) 0.1830(3) 0.4565(2) 0.0302(10) Uani 1 d . . H28A H 0.2388(3) 0.1824(3) 0.4327(2) 0.036 Uiso 1 calc R . C29 C 0.1727(3) 0.1102(3) 0.4880(3) 0.0328(11) Uani 1 d . . H29A H 0.2031(3) 0.0611(3) 0.4855(3) 0.039 Uiso 1 calc R . C30 C 0.1071(2) 0.1078(3) 0.5233(2) 0.0227(9) Uani 1 d . . C31 C 0.0650(3) 0.1817(3) 0.5234(2) 0.0306(11) Uani 1 d . . H31A H 0.0190(3) 0.1833(3) 0.5455(2) 0.037 Uiso 1 calc R . C32 C 0.0898(3) 0.2523(3) 0.4916(3) 0.0349(11) Uani 1 d . . H32A H 0.0602(3) 0.3020(3) 0.4933(3) 0.042 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02037(9) 0.02542(10) 0.02638(10) 0.00626(7) -0.00260(7) -0.00292(7) Re2 0.02436(9) 0.02065(9) 0.02252(10) 0.00193(7) 0.00055(7) -0.00293(6) O1 0.048(2) 0.041(2) 0.043(2) 0.017(2) -0.002(2) -0.011(2) O2 0.031(2) 0.042(2) 0.066(3) 0.012(2) -0.019(2) -0.001(2) O3 0.038(2) 0.075(3) 0.033(2) -0.008(2) -0.003(2) -0.003(2) O4 0.032(2) 0.040(2) 0.042(2) -0.002(2) -0.009(2) -0.0041(15) O5 0.064(3) 0.040(2) 0.038(2) -0.009(2) 0.002(2) 0.000(2) O6 0.043(2) 0.031(2) 0.041(2) 0.010(2) -0.005(2) -0.012(2) O7 0.0202(14) 0.033(2) 0.022(2) -0.0002(13) -0.0005(12) -0.0006(12) O8 0.0230(15) 0.025(2) 0.032(2) 0.0041(14) 0.0011(13) 0.0011(12) N1 0.023(2) 0.021(2) 0.027(2) 0.002(2) -0.0029(15) -0.0012(15) N2 0.023(2) 0.023(2) 0.024(2) 0.001(2) 0.0007(14) -0.0007(14) C1 0.025(2) 0.033(3) 0.030(3) 0.008(2) -0.006(2) -0.002(2) C2 0.026(2) 0.025(2) 0.043(3) 0.008(2) -0.005(2) -0.002(2) C3 0.023(2) 0.042(3) 0.032(3) 0.008(2) -0.003(2) -0.004(2) C4 0.031(2) 0.026(2) 0.028(2) -0.001(2) 0.001(2) -0.004(2) C5 0.037(3) 0.025(2) 0.031(3) 0.002(2) 0.002(2) -0.003(2) C6 0.029(2) 0.030(2) 0.029(2) 0.002(2) -0.006(2) -0.002(2) C7 0.024(3) 0.122(6) 0.044(4) -0.023(4) 0.003(2) -0.006(3) C8 0.025(2) 0.056(3) 0.027(3) 0.000(2) -0.001(2) 0.001(2) C9 0.042(3) 0.047(3) 0.042(3) 0.005(3) -0.004(2) 0.007(2) C10 0.049(3) 0.058(4) 0.049(4) -0.016(3) -0.007(3) 0.019(3) C11 0.056(4) 0.091(6) 0.031(3) -0.008(3) -0.003(3) 0.030(4) C12 0.049(3) 0.089(5) 0.033(3) 0.017(3) 0.002(3) 0.017(3) C13 0.036(3) 0.052(4) 0.054(4) 0.002(3) 0.002(3) 0.005(3) C13 0.033(2) 0.030(3) 0.045(3) 0.005(2) 0.012(2) 0.000(2) C15 0.027(2) 0.027(2) 0.041(3) 0.002(2) 0.007(2) 0.003(2) C16 0.038(3) 0.032(3) 0.045(3) -0.001(2) -0.007(2) 0.008(2) C17 0.043(3) 0.036(3) 0.045(3) 0.011(3) 0.001(2) 0.004(2) C18 0.031(2) 0.027(3) 0.064(4) 0.008(3) 0.009(2) 0.003(2) C19 0.034(3) 0.036(3) 0.049(3) -0.006(3) 0.001(2) 0.008(2) C20 0.039(3) 0.037(3) 0.034(3) 0.001(2) 0.008(2) 0.011(2) C21 0.029(2) 0.027(2) 0.045(3) 0.008(2) 0.009(2) 0.004(2) C22 0.027(2) 0.026(2) 0.043(3) 0.010(2) 0.010(2) 0.002(2) C23 0.023(2) 0.026(2) 0.022(2) 0.001(2) -0.005(2) -0.003(2) C24 0.028(2) 0.026(2) 0.044(3) -0.002(2) 0.004(2) 0.001(2) C25 0.023(2) 0.028(2) 0.042(3) 0.004(2) 0.005(2) 0.000(2) C26 0.025(2) 0.022(2) 0.031(2) 0.002(2) -0.003(2) -0.001(2) C27 0.030(2) 0.019(2) 0.027(2) 0.000(2) 0.000(2) 0.001(2) C28 0.030(2) 0.025(2) 0.036(3) -0.001(2) 0.007(2) 0.001(2) C29 0.035(2) 0.022(2) 0.042(3) 0.001(2) 0.010(2) 0.004(2) C30 0.028(2) 0.022(2) 0.019(2) -0.001(2) -0.001(2) -0.003(2) C31 0.027(2) 0.026(2) 0.038(3) 0.007(2) 0.011(2) 0.006(2) C32 0.034(2) 0.029(2) 0.041(3) 0.011(2) 0.009(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C2 1.901(5) . ? Re1 C3 1.910(6) . ? Re1 C1 1.924(5) . ? Re1 O8 2.151(3) . ? Re1 O7 2.165(3) . ? Re1 N1 2.216(4) . ? Re2 C4 1.899(5) . ? Re2 C5 1.915(5) . ? Re2 C6 1.919(5) . ? Re2 O8 2.135(3) . ? Re2 O7 2.154(3) . ? Re2 N2 2.212(4) . ? O1 C1 1.150(6) . ? O2 C2 1.163(6) . ? O3 C3 1.152(6) . ? O4 C4 1.166(6) . ? O5 C5 1.155(6) . ? O6 C6 1.156(6) . ? O7 C7 1.447(6) . ? O8 C13 1.441(6) . ? N1 C25 1.339(6) . ? N1 C21 1.347(6) . ? N2 C28 1.346(6) . ? N2 C32 1.351(6) . ? C7 C8 1.504(8) . ? C8 C9 1.384(8) . ? C8 C13 1.394(8) . ? C9 C10 1.368(8) . ? C10 C11 1.399(10) . ? C11 C12 1.359(10) . ? C12 C13 1.377(9) . ? C13 C15 1.518(7) . ? C15 C20 1.389(7) . ? C15 C16 1.388(7) . ? C16 C17 1.397(8) . ? C17 C18 1.374(8) . ? C18 C19 1.381(8) . ? C19 C20 1.376(8) . ? C21 C22 1.383(6) . ? C22 C23 1.394(6) . ? C23 C24 1.390(6) . ? C23 C26 1.469(6) . ? C24 C25 1.386(7) . ? C26 C27 1.338(6) . ? C27 C30 1.472(6) 5_556 ? C28 C29 1.379(7) . ? C29 C30 1.394(6) . ? C30 C31 1.392(6) . ? C30 C27 1.472(6) 5_556 ? C31 C32 1.373(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C3 84.8(2) . . ? C2 Re1 C1 87.9(2) . . ? C3 Re1 C1 87.6(2) . . ? C2 Re1 O8 99.8(2) . . ? C3 Re1 O8 171.5(2) . . ? C1 Re1 O8 99.6(2) . . ? C2 Re1 O7 172.7(2) . . ? C3 Re1 O7 102.1(2) . . ? C1 Re1 O7 94.6(2) . . ? O8 Re1 O7 73.02(11) . . ? C2 Re1 N1 93.7(2) . . ? C3 Re1 N1 91.6(2) . . ? C1 Re1 N1 178.2(2) . . ? O8 Re1 N1 81.00(13) . . ? O7 Re1 N1 83.97(12) . . ? C4 Re2 C5 85.1(2) . . ? C4 Re2 C6 86.9(2) . . ? C5 Re2 C6 88.8(2) . . ? C4 Re2 O8 172.1(2) . . ? C5 Re2 O8 102.6(2) . . ? C6 Re2 O8 94.5(2) . . ? C4 Re2 O7 98.6(2) . . ? C5 Re2 O7 174.2(2) . . ? C6 Re2 O7 95.7(2) . . ? O8 Re2 O7 73.54(11) . . ? C4 Re2 N2 95.7(2) . . ? C5 Re2 N2 90.6(2) . . ? C6 Re2 N2 177.4(2) . . ? O8 Re2 N2 83.04(12) . . ? O7 Re2 N2 84.63(13) . . ? C7 O7 Re2 112.1(3) . . ? C7 O7 Re1 124.5(3) . . ? Re2 O7 Re1 104.52(13) . . ? C13 O8 Re2 124.2(3) . . ? C13 O8 Re1 123.3(3) . . ? Re2 O8 Re1 105.66(13) . . ? C25 N1 C21 116.4(4) . . ? C25 N1 Re1 122.2(3) . . ? C21 N1 Re1 121.4(3) . . ? C28 N2 C32 116.4(4) . . ? C28 N2 Re2 123.5(3) . . ? C32 N2 Re2 120.0(3) . . ? O1 C1 Re1 177.1(5) . . ? O2 C2 Re1 178.1(5) . . ? O3 C3 Re1 176.2(4) . . ? O4 C4 Re2 177.2(4) . . ? O5 C5 Re2 176.7(5) . . ? O6 C6 Re2 177.8(4) . . ? O7 C7 C8 116.1(4) . . ? C9 C8 C13 118.4(5) . . ? C9 C8 C7 121.4(6) . . ? C13 C8 C7 120.2(6) . . ? C10 C9 C8 121.4(6) . . ? C9 C10 C11 118.5(6) . . ? C12 C11 C10 121.3(6) . . ? C11 C12 C13 119.3(6) . . ? C12 C13 C8 120.9(6) . . ? O8 C13 C15 114.6(4) . . ? C20 C15 C16 118.8(5) . . ? C20 C15 C13 120.3(5) . . ? C16 C15 C13 120.9(5) . . ? C15 C16 C17 119.8(5) . . ? C18 C17 C16 120.2(5) . . ? C17 C18 C19 120.3(5) . . ? C18 C19 C20 119.5(5) . . ? C15 C20 C19 121.3(5) . . ? N1 C21 C22 123.4(4) . . ? C21 C22 C23 120.4(4) . . ? C24 C23 C22 115.9(4) . . ? C24 C23 C26 120.7(4) . . ? C22 C23 C26 123.4(4) . . ? C25 C24 C23 120.5(4) . . ? N1 C25 C24 123.4(4) . . ? C27 C26 C23 125.4(4) . . ? C26 C27 C30 125.7(4) . 5_556 ? N2 C28 C29 123.0(4) . . ? C28 C29 C30 120.6(4) . . ? C29 C30 C31 116.0(4) . . ? C29 C30 C27 120.5(4) . 5_556 ? C31 C30 C27 123.5(4) . 5_556 ? C32 C31 C30 120.3(4) . . ? N2 C32 C31 123.6(4) . . ? _refine_diff_density_max 1.318 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.115