Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Elisa Barea' _publ_contact_author_address ; Dipartimento di Chimica Inorganica, Metallorganica e Analitica Universita degli Studi di Milano Via Venezian 21 Milano 20133 ITALY ; _publ_contact_author_email EBAREAM@UGR.ES _publ_section_title ; [Re2(mu-1,2,4-triazolate)2(mu-OH)(CO)6]-: a novel metalloligand for the construction of flexible porous coordination networks ; loop_ _publ_author_name 'Elisa Barea' "Giuseppe D'Alfonso" 'Jorge Navarro' 'Antonio Rodriguez-Dieguez' 'A. Sironi' #========================================================================== data_[Et4N][Re2(mu-1,2,4-triazolate-kN1:kN2)2(mu-OH)(CO)6].CH3OH _database_code_depnum_ccdc_archive 'CCDC 668220' _audit_creation_method SHELXL-97 #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H29 N7 O8 Re2' _chemical_formula_weight 855.89 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 12.152(2) _cell_length_b 12.204(2) _cell_length_c 19.056(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.72(3) _cell_angle_gamma 90.00 _cell_volume 2745.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 8.863 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.321 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 ? _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 32200 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 29.41 _reflns_number_total 7155 _reflns_number_gt 5885 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0430P)^2^+2.7588P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7155 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1A O 0.0972(3) 0.3886(4) 0.9120(2) 0.0709(13) Uani 1 1 d . . . C1A C 0.1472(4) 0.3823(7) 0.8550(3) 0.073(2) Uani 1 1 d . . . H1A1 H 0.1072 0.4285 0.8166 0.110 Uiso 1 1 calc R . . H1A2 H 0.1449 0.3079 0.8383 0.110 Uiso 1 1 calc R . . H1A3 H 0.2245 0.4060 0.8701 0.110 Uiso 1 1 calc R . . H7 H 0.387(3) 0.903(4) 0.170(2) 0.029(11) Uiso 1 1 d . . . Re1 Re 0.467690(12) 0.764796(12) 0.091875(7) 0.02255(6) Uani 1 1 d . . . Re2 Re 0.255281(13) 0.763170(12) 0.199069(8) 0.02531(6) Uani 1 1 d . . . C1 C 0.5481(3) 0.6687(3) 0.0434(2) 0.0336(8) Uani 1 1 d . . . O1 O 0.5953(3) 0.6097(3) 0.01260(18) 0.0514(8) Uani 1 1 d . . . C2 C 0.4402(4) 0.8545(3) 0.0072(2) 0.0333(8) Uani 1 1 d . . . O2 O 0.4242(3) 0.9046(3) -0.04527(16) 0.0546(9) Uani 1 1 d . . . C3 C 0.6078(3) 0.8401(3) 0.1298(2) 0.0315(8) Uani 1 1 d . . . O3 O 0.6930(3) 0.8830(3) 0.15290(19) 0.0519(8) Uani 1 1 d . . . C4 C 0.1661(4) 0.6679(3) 0.2427(2) 0.0365(9) Uani 1 1 d . . . O4 O 0.1133(3) 0.6114(3) 0.27051(18) 0.0533(9) Uani 1 1 d . . . C5 C 0.1226(4) 0.8506(4) 0.1662(2) 0.0422(10) Uani 1 1 d . . . O5 O 0.0418(3) 0.9020(3) 0.1461(2) 0.0721(12) Uani 1 1 d . . . C6 C 0.2919(5) 0.8402(4) 0.2880(2) 0.0491(12) Uani 1 1 d . . . O6 O 0.3143(5) 0.8843(3) 0.34309(19) 0.0905(17) Uani 1 1 d . . . O7 O 0.3622(2) 0.8526(2) 0.14634(12) 0.0252(5) Uani 1 1 d . . . N11 N 0.4846(3) 0.6608(2) 0.18631(15) 0.0253(6) Uani 1 1 d . . . N12 N 0.4059(3) 0.6616(3) 0.22747(15) 0.0266(6) Uani 1 1 d . . . C13 C 0.4410(3) 0.5869(3) 0.27887(19) 0.0319(8) Uani 1 1 d . . . H13 H 0.4024 0.5708 0.3143 0.038 Uiso 1 1 calc R . . N14 N 0.5365(3) 0.5376(3) 0.27441(18) 0.0366(8) Uani 1 1 d . . . C15 C 0.5595(3) 0.5860(3) 0.2159(2) 0.0319(8) Uani 1 1 d . . . H15 H 0.6223 0.5683 0.1981 0.038 Uiso 1 1 calc R . . N21 N 0.3104(2) 0.6765(2) 0.05801(14) 0.0243(6) Uani 1 1 d . . . N22 N 0.2311(3) 0.6737(2) 0.09827(15) 0.0250(6) Uani 1 1 d . . . C23 C 0.1495(3) 0.6089(3) 0.0631(2) 0.0306(8) Uani 1 1 d . . . H23 H 0.0846 0.5931 0.0790 0.037 Uiso 1 1 calc R . . N24 N 0.1698(3) 0.5680(3) 0.00213(17) 0.0357(8) Uani 1 1 d . . . C25 C 0.2700(3) 0.6121(3) 0.00194(19) 0.0317(8) Uani 1 1 d . . . H25 H 0.3080 0.5989 -0.0342 0.038 Uiso 1 1 calc R . . N30 N 0.1575(3) 0.2291(3) 0.10613(19) 0.0359(8) Uani 1 1 d . . . C31 C 0.2129(4) 0.1192(4) 0.1008(3) 0.0535(12) Uani 1 1 d . . . H31A H 0.1611 0.0621 0.1078 0.064 Uiso 1 1 calc R . . H31B H 0.2801 0.1138 0.1401 0.064 Uiso 1 1 calc R . . C32 C 0.2466(6) 0.0974(6) 0.0305(4) 0.083(2) Uani 1 1 d . . . H32A H 0.2809 0.0263 0.0323 0.124 Uiso 1 1 calc R . . H32B H 0.2997 0.1521 0.0234 0.124 Uiso 1 1 calc R . . H32C H 0.1805 0.0999 -0.0088 0.124 Uiso 1 1 calc R . . C33 C 0.2353(5) 0.3213(4) 0.0956(3) 0.0511(12) Uani 1 1 d . . . H33A H 0.1970 0.3903 0.0987 0.061 Uiso 1 1 calc R . . H33B H 0.2472 0.3159 0.0472 0.061 Uiso 1 1 calc R . . C34 C 0.3499(5) 0.3248(6) 0.1485(3) 0.0720(19) Uani 1 1 d . . . H34A H 0.3925 0.3859 0.1373 0.108 Uiso 1 1 calc R . . H34B H 0.3901 0.2581 0.1451 0.108 Uiso 1 1 calc R . . H34C H 0.3398 0.3327 0.1967 0.108 Uiso 1 1 calc R . . C35 C 0.1336(5) 0.2346(4) 0.1796(3) 0.0549(13) Uani 1 1 d . . . H35A H 0.2047 0.2266 0.2155 0.066 Uiso 1 1 calc R . . H35B H 0.0861 0.1728 0.1850 0.066 Uiso 1 1 calc R . . C36 C 0.0767(6) 0.3380(6) 0.1957(3) 0.087(2) Uani 1 1 d . . . H36A H 0.0645 0.3341 0.2436 0.130 Uiso 1 1 calc R . . H36B H 0.0052 0.3461 0.1615 0.130 Uiso 1 1 calc R . . H36C H 0.1240 0.3998 0.1923 0.130 Uiso 1 1 calc R . . C37 C 0.0497(5) 0.2411(4) 0.0475(3) 0.0485(12) Uani 1 1 d . . . H37A H 0.0688 0.2365 0.0010 0.058 Uiso 1 1 calc R . . H37B H 0.0189 0.3136 0.0513 0.058 Uiso 1 1 calc R . . C38 C -0.0419(4) 0.1569(5) 0.0494(3) 0.0601(14) Uani 1 1 d . . . H38A H -0.1067 0.1708 0.0105 0.090 Uiso 1 1 calc R . . H38B H -0.0634 0.1619 0.0946 0.090 Uiso 1 1 calc R . . H38C H -0.0133 0.0847 0.0442 0.090 Uiso 1 1 calc R . . H1A H 0.1028 0.4483 0.9225 0.12(3) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1A 0.079(3) 0.086(3) 0.061(2) -0.037(2) 0.041(2) -0.050(2) C1A 0.055(3) 0.119(6) 0.052(3) -0.027(3) 0.026(3) -0.012(3) Re1 0.02756(9) 0.02313(9) 0.01921(8) 0.00104(4) 0.01002(6) 0.00147(5) Re2 0.03291(10) 0.02501(9) 0.02190(9) -0.00018(5) 0.01422(7) 0.00326(5) C1 0.037(2) 0.0333(19) 0.036(2) 0.0002(16) 0.0208(17) 0.0009(17) O1 0.053(2) 0.0496(19) 0.061(2) -0.0100(16) 0.0321(17) 0.0087(16) C2 0.042(2) 0.035(2) 0.0263(18) 0.0017(15) 0.0147(16) 0.0008(17) O2 0.081(3) 0.053(2) 0.0321(16) 0.0166(14) 0.0194(16) 0.0048(18) C3 0.033(2) 0.0324(19) 0.0314(19) -0.0020(15) 0.0126(16) -0.0010(16) O3 0.0408(18) 0.050(2) 0.065(2) -0.0096(17) 0.0130(16) -0.0095(15) C4 0.046(2) 0.034(2) 0.037(2) 0.0025(17) 0.0233(18) 0.0043(18) O4 0.059(2) 0.053(2) 0.057(2) 0.0117(16) 0.0311(17) -0.0067(17) C5 0.047(3) 0.036(2) 0.053(3) 0.0128(19) 0.030(2) 0.011(2) O5 0.061(2) 0.069(3) 0.100(3) 0.038(2) 0.046(2) 0.036(2) C6 0.083(4) 0.040(2) 0.036(2) -0.0043(18) 0.036(2) -0.010(2) O6 0.184(5) 0.065(3) 0.040(2) -0.0271(18) 0.061(3) -0.044(3) O7 0.0309(14) 0.0229(13) 0.0243(12) -0.0048(9) 0.0115(11) -0.0014(10) N11 0.0280(15) 0.0280(15) 0.0204(13) 0.0029(11) 0.0064(11) 0.0001(12) N12 0.0328(17) 0.0290(15) 0.0188(13) 0.0041(11) 0.0079(12) 0.0002(13) C13 0.040(2) 0.0324(19) 0.0232(17) 0.0056(14) 0.0073(15) -0.0035(16) N14 0.0389(19) 0.0365(18) 0.0325(16) 0.0118(14) 0.0045(14) 0.0039(15) C15 0.030(2) 0.0325(19) 0.0328(19) 0.0060(15) 0.0077(15) 0.0035(16) N21 0.0268(15) 0.0274(15) 0.0196(13) -0.0017(11) 0.0071(11) 0.0031(12) N22 0.0287(15) 0.0271(14) 0.0204(13) 0.0006(11) 0.0080(11) 0.0031(12) C23 0.0282(19) 0.0311(19) 0.0312(18) 0.0019(15) 0.0044(15) 0.0021(15) N24 0.041(2) 0.0360(18) 0.0271(16) -0.0047(13) 0.0030(14) -0.0013(15) C25 0.040(2) 0.0328(19) 0.0219(16) -0.0043(14) 0.0075(15) 0.0016(16) N30 0.0363(19) 0.0369(18) 0.035(2) 0.0137(14) 0.0086(15) 0.0030(14) C31 0.047(3) 0.045(3) 0.066(3) 0.007(2) 0.008(2) 0.012(2) C32 0.075(4) 0.084(5) 0.095(5) -0.029(4) 0.032(4) 0.009(4) C33 0.061(3) 0.046(3) 0.047(3) 0.013(2) 0.012(2) -0.006(2) C34 0.072(4) 0.081(5) 0.053(3) 0.006(3) -0.003(3) -0.029(3) C35 0.062(4) 0.067(3) 0.038(3) 0.010(2) 0.014(2) 0.004(3) C36 0.105(6) 0.095(5) 0.068(4) -0.018(4) 0.036(4) 0.019(4) C37 0.056(3) 0.053(3) 0.032(2) 0.0134(18) -0.001(2) 0.009(2) C38 0.048(3) 0.070(4) 0.058(3) 0.013(3) 0.001(2) -0.002(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 O1A C1A 1.367(5) . ? Re1 C1 1.900(4) . ? Re1 C2 1.913(4) . ? Re1 C3 1.919(4) . ? Re1 O7 2.122(2) . ? Re1 N21 2.156(3) . ? Re1 N11 2.172(3) . ? Re2 C6 1.897(4) . ? Re2 C4 1.909(4) . ? Re2 C5 1.911(4) . ? Re2 O7 2.123(2) . ? Re2 N22 2.168(3) . ? Re2 N12 2.170(3) . ? C1 O1 1.162(5) . ? C2 O2 1.148(4) . ? C3 O3 1.151(5) . ? C4 O4 1.153(5) . ? C5 O5 1.152(5) . ? C6 O6 1.153(5) . ? N11 C15 1.318(5) . ? N11 N12 1.374(4) . ? N12 C13 1.332(4) . ? C13 N14 1.328(5) . ? N14 C15 1.349(5) . ? N21 C25 1.323(4) . ? N21 N22 1.367(4) . ? N22 C23 1.321(5) . ? C23 N24 1.340(5) . ? N24 C25 1.331(5) . ? N30 C35 1.498(6) . ? N30 C33 1.513(6) . ? N30 C37 1.513(6) . ? N30 C31 1.514(6) . ? C31 C32 1.515(7) . ? C33 C34 1.514(7) . ? C35 C36 1.506(8) . ? C37 C38 1.522(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 C2 87.13(17) . . ? C1 Re1 C3 88.08(17) . . ? C2 Re1 C3 90.31(17) . . ? C1 Re1 O7 171.73(14) . . ? C2 Re1 O7 96.82(14) . . ? C3 Re1 O7 99.13(13) . . ? C1 Re1 N21 93.86(15) . . ? C2 Re1 N21 93.94(15) . . ? C3 Re1 N21 175.40(13) . . ? O7 Re1 N21 78.65(10) . . ? C1 Re1 N11 94.80(15) . . ? C2 Re1 N11 175.49(15) . . ? C3 Re1 N11 93.82(14) . . ? O7 Re1 N11 80.76(11) . . ? N21 Re1 N11 81.87(11) . . ? C6 Re2 C4 87.12(19) . . ? C6 Re2 C5 91.0(2) . . ? C4 Re2 C5 87.78(18) . . ? C6 Re2 O7 97.35(15) . . ? C4 Re2 O7 173.42(14) . . ? C5 Re2 O7 96.94(14) . . ? C6 Re2 N22 174.38(18) . . ? C4 Re2 N22 96.17(15) . . ? C5 Re2 N22 93.66(17) . . ? O7 Re2 N22 79.00(10) . . ? C6 Re2 N12 93.14(19) . . ? C4 Re2 N12 94.32(15) . . ? C5 Re2 N12 175.44(15) . . ? O7 Re2 N12 80.65(10) . . ? N22 Re2 N12 82.10(11) . . ? O1 C1 Re1 178.6(4) . . ? O2 C2 Re1 177.2(4) . . ? O3 C3 Re1 178.4(4) . . ? O4 C4 Re2 178.5(4) . . ? O5 C5 Re2 179.1(5) . . ? O6 C6 Re2 178.1(4) . . ? Re1 O7 Re2 118.69(13) . . ? C15 N11 N12 105.4(3) . . ? C15 N11 Re1 132.8(3) . . ? N12 N11 Re1 121.8(2) . . ? C13 N12 N11 105.7(3) . . ? C13 N12 Re2 132.7(3) . . ? N11 N12 Re2 121.5(2) . . ? N14 C13 N12 113.3(3) . . ? C13 N14 C15 102.2(3) . . ? N11 C15 N14 113.5(3) . . ? C25 N21 N22 105.2(3) . . ? C25 N21 Re1 132.2(3) . . ? N22 N21 Re1 122.5(2) . . ? C23 N22 N21 105.9(3) . . ? C23 N22 Re2 132.8(2) . . ? N21 N22 Re2 121.3(2) . . ? N22 C23 N24 113.1(3) . . ? C25 N24 C23 102.1(3) . . ? N21 C25 N24 113.7(3) . . ? C35 N30 C33 110.9(4) . . ? C35 N30 C37 111.1(4) . . ? C33 N30 C37 106.8(3) . . ? C35 N30 C31 106.8(3) . . ? C33 N30 C31 110.4(4) . . ? C37 N30 C31 110.9(4) . . ? N30 C31 C32 115.6(4) . . ? N30 C33 C34 115.9(4) . . ? N30 C35 C36 115.4(4) . . ? N30 C37 C38 115.3(4) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 29.41 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.695 _refine_diff_density_min -1.416 _refine_diff_density_rms 0.175 #========================================================================== data_[Ag{Re2(mu3-trz-kN1:kN2:kN4)2(mu3-OH)(CO)6}]n.4nCH3OH _database_code_depnum_ccdc_archive 'CCDC 668221' _audit_creation_method SHELXL-97 #========================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H17 Ag N6 O11 Re2' _chemical_formula_weight 925.61 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' Ag Ag -0.8971 1.1015 '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 ? _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 9.0741(18) _cell_length_b 15.264(3) _cell_length_c 17.667(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.18(3) _cell_angle_gamma 90.00 _cell_volume 2415.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 10.864 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.218 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 ? _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 22911 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 22.07 _reflns_number_total 2957 _reflns_number_gt 2551 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0525P)^2^+34.1557P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2957 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _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 0.00271(5) 0.02867(4) 0.22730(3) 0.0236(2) Uani 1 1 d . . . Re2 Re 0.36694(5) -0.00167(3) 0.16793(3) 0.0224(2) Uani 1 1 d . . . Ag Ag -0.07302(11) 0.17464(7) -0.10905(6) 0.0322(3) Uani 1 1 d . . . C1 C -0.1472(14) -0.0535(9) 0.1888(8) 0.026(3) Uani 1 1 d . . . O1 O -0.2334(10) -0.1064(7) 0.1620(6) 0.041(3) Uani 1 1 d . . . C2 C -0.0178(16) -0.0043(11) 0.3313(10) 0.040(4) Uani 1 1 d . . . O2 O -0.0357(13) -0.0235(9) 0.3915(7) 0.059(3) Uani 1 1 d . . . C3 C -0.1453(15) 0.1137(9) 0.2331(8) 0.029(3) Uani 1 1 d . . . O3 O -0.2348(11) 0.1682(7) 0.2376(6) 0.047(3) Uani 1 1 d . . . C4 C 0.5190(16) -0.0400(9) 0.2494(8) 0.029(3) Uani 1 1 d . . . O4 O 0.6116(11) -0.0621(8) 0.2971(7) 0.052(3) Uani 1 1 d . . . C5 C 0.3982(14) -0.1051(11) 0.1093(8) 0.029(3) Uani 1 1 d . . . O5 O 0.4265(11) -0.1644(7) 0.0760(6) 0.042(3) Uani 1 1 d . . . C6 C 0.5135(14) 0.0523(9) 0.1187(8) 0.026(3) Uani 1 1 d . . . O6 O 0.6019(11) 0.0827(7) 0.0856(6) 0.041(3) Uani 1 1 d . . . O7 O 0.1852(9) -0.0565(6) 0.2150(5) 0.025(2) Uani 1 1 d . . . N11 N 0.0446(10) 0.0655(7) 0.1136(6) 0.019(2) Uani 1 1 d . . . N12 N 0.1798(12) 0.0524(7) 0.0894(6) 0.027(3) Uani 1 1 d . . . C13 C 0.1640(14) 0.0818(8) 0.0191(8) 0.024(3) Uani 1 1 d . . . H13 H 0.2404 0.0818 -0.0103 0.029 Uiso 1 1 calc R . . N14 N 0.0253(10) 0.1119(7) -0.0065(6) 0.024(3) Uani 1 1 d . . . C15 C -0.0432(13) 0.1015(8) 0.0561(8) 0.024(3) Uani 1 1 d . . . H15 H -0.1413 0.1181 0.0578 0.029 Uiso 1 1 calc R . . N21 N 0.1864(11) 0.1171(8) 0.2644(6) 0.025(3) Uani 1 1 d . . . N22 N 0.3202(11) 0.1084(7) 0.2379(6) 0.023(3) Uani 1 1 d . . . C23 C 0.4044(14) 0.1731(9) 0.2700(8) 0.029(3) Uani 1 1 d . . . H23 H 0.5015 0.1830 0.2614 0.035 Uiso 1 1 calc R . . N24 N 0.3372(11) 0.2226(7) 0.3158(6) 0.026(3) Uani 1 1 d . . . C25 C 0.2015(15) 0.1852(9) 0.3106(8) 0.029(3) Uani 1 1 d . . . H25 H 0.1269 0.2053 0.3367 0.035 Uiso 1 1 calc R . . O10 O 0.2671(17) 0.8676(9) 0.3574(8) 0.086(5) Uani 1 1 d . . . C10 C 0.363(2) 0.7957(13) 0.3719(11) 0.066(5) Uani 1 1 d . . . H10A H 0.4047 0.7822 0.3267 0.099 Uiso 1 1 calc R . . H10B H 0.3076 0.7461 0.3856 0.099 Uiso 1 1 calc R . . H10C H 0.4414 0.8093 0.4133 0.099 Uiso 1 1 calc R . . O20 O 0.317(3) -0.001(4) 0.500(2) 0.33(3) Uani 1 1 d . . . C20 C 0.394(4) 0.024(2) 0.432(2) 0.157(16) Uani 1 1 d . . . H20A H 0.3236 0.0217 0.3857 0.236 Uiso 1 1 calc R . . H20B H 0.4745 -0.0160 0.4289 0.236 Uiso 1 1 calc R . . H20C H 0.4336 0.0825 0.4395 0.236 Uiso 1 1 calc R . . O30 O 0.854(3) 0.876(2) 0.5162(13) 0.160(10) Uani 1 1 d . . . C30 C 0.784(4) 0.818(2) 0.458(2) 0.20(2) Uani 1 1 d . . . H30A H 0.7299 0.8514 0.4163 0.304 Uiso 1 1 calc R . . H30B H 0.7163 0.7800 0.4785 0.304 Uiso 1 1 calc R . . H30C H 0.8590 0.7835 0.4389 0.304 Uiso 1 1 calc R . . O40 O 0.155(3) 0.862(2) 0.4965(15) 0.184(12) Uani 1 1 d . . . C40 C 0.234(4) 0.824(3) 0.5617(16) 0.157(16) Uani 1 1 d . . . H40A H 0.3330 0.8488 0.5712 0.235 Uiso 1 1 calc R . . H40B H 0.2406 0.7622 0.5547 0.235 Uiso 1 1 calc R . . H40C H 0.1843 0.8363 0.6045 0.235 Uiso 1 1 calc R . . H7 H 0.225(17) -0.083(11) 0.271(10) 0.06(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0199(3) 0.0240(4) 0.0260(4) -0.0014(2) 0.0006(2) -0.0031(2) Re2 0.0195(3) 0.0218(4) 0.0244(4) 0.0003(2) -0.0011(2) 0.0013(2) Ag 0.0308(6) 0.0298(7) 0.0341(7) 0.0095(5) -0.0005(5) 0.0074(5) C1 0.016(7) 0.023(8) 0.039(9) 0.002(7) 0.002(6) -0.001(6) O1 0.034(5) 0.038(6) 0.051(7) -0.015(6) 0.009(5) -0.011(5) C2 0.031(9) 0.047(10) 0.039(11) -0.015(9) -0.001(7) -0.008(7) O2 0.054(7) 0.088(10) 0.035(8) 0.013(7) 0.008(6) -0.006(6) C3 0.026(7) 0.023(8) 0.036(9) -0.001(7) 0.002(6) -0.012(7) O3 0.036(6) 0.041(7) 0.063(8) -0.017(6) 0.003(5) 0.005(6) C4 0.038(9) 0.021(8) 0.029(9) 0.000(7) 0.008(7) 0.010(7) O4 0.029(6) 0.075(9) 0.050(7) 0.020(7) 0.002(5) 0.004(6) C5 0.020(7) 0.036(10) 0.032(9) 0.009(8) 0.004(6) 0.005(6) O5 0.045(6) 0.027(6) 0.054(7) -0.013(6) 0.007(5) 0.008(5) C6 0.026(8) 0.028(8) 0.023(8) 0.008(7) -0.002(6) 0.006(6) O6 0.034(6) 0.050(7) 0.038(6) 0.012(5) 0.008(5) -0.003(5) O7 0.019(5) 0.025(5) 0.031(6) 0.002(5) 0.002(4) -0.002(4) N11 0.013(5) 0.016(6) 0.026(6) -0.006(5) 0.000(5) 0.005(4) N12 0.038(7) 0.012(6) 0.029(7) -0.003(5) 0.004(5) 0.001(5) C13 0.029(8) 0.012(7) 0.030(9) 0.000(6) 0.002(6) 0.002(6) N14 0.013(5) 0.023(6) 0.033(7) -0.003(5) -0.001(5) 0.002(5) C15 0.014(6) 0.019(7) 0.036(9) -0.002(7) -0.005(6) 0.000(5) N21 0.023(6) 0.032(7) 0.020(6) 0.002(6) 0.003(5) -0.005(5) N22 0.027(6) 0.020(6) 0.022(6) -0.001(5) 0.002(5) -0.001(5) C23 0.023(7) 0.031(9) 0.029(8) -0.004(7) -0.006(6) -0.004(6) N24 0.022(6) 0.030(7) 0.025(7) -0.010(6) 0.002(5) -0.007(5) C25 0.031(8) 0.030(9) 0.024(8) -0.005(7) -0.005(6) 0.003(6) O10 0.123(12) 0.073(10) 0.064(9) 0.030(8) 0.016(8) 0.070(9) C10 0.095(14) 0.057(13) 0.049(12) 0.009(10) 0.022(10) 0.009(11) O20 0.14(3) 0.69(11) 0.14(3) 0.03(4) 0.00(2) -0.10(4) C20 0.17(3) 0.09(2) 0.18(4) -0.03(2) -0.06(3) 0.02(2) O30 0.137(17) 0.21(3) 0.127(18) 0.048(18) -0.009(14) -0.047(18) C30 0.15(3) 0.16(4) 0.25(5) 0.13(4) -0.11(3) -0.08(3) O40 0.137(18) 0.26(4) 0.15(2) 0.04(2) 0.009(15) 0.07(2) C40 0.17(3) 0.23(4) 0.07(2) 0.01(2) 0.024(19) 0.10(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 C3 1.883(15) . ? Re1 C1 1.895(14) . ? Re1 C2 1.942(19) . ? Re1 O7 2.143(8) . ? Re1 N21 2.164(10) . ? Re1 N11 2.177(10) . ? Re2 C6 1.890(15) . ? Re2 C4 1.919(15) . ? Re2 C5 1.934(17) . ? Re2 O7 2.132(8) . ? Re2 N22 2.167(11) . ? Re2 N12 2.177(11) . ? Ag N14 2.117(11) . ? Ag N24 2.132(10) 4_565 ? C1 O1 1.170(16) . ? C2 O2 1.140(19) . ? C3 O3 1.173(17) . ? C4 O4 1.141(16) . ? C5 O5 1.132(17) . ? C6 O6 1.162(16) . ? N11 C15 1.307(16) . ? N11 N12 1.376(14) . ? N12 C13 1.307(17) . ? C13 N14 1.348(16) . ? N14 C15 1.362(16) . ? N21 C25 1.316(17) . ? N21 N22 1.376(14) . ? N22 C23 1.320(17) . ? C23 N24 1.324(17) . ? N24 C25 1.347(16) . ? N24 Ag 2.132(10) 4_666 ? O10 C10 1.40(2) . ? O20 C20 1.53(5) . ? O30 C30 1.43(4) . ? O40 C40 1.38(3) . ? 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 Re1 C1 89.9(5) . . ? C3 Re1 C2 87.2(6) . . ? C1 Re1 C2 89.8(6) . . ? C3 Re1 O7 173.3(5) . . ? C1 Re1 O7 94.8(5) . . ? C2 Re1 O7 97.5(5) . . ? C3 Re1 N21 94.3(5) . . ? C1 Re1 N21 174.8(5) . . ? C2 Re1 N21 93.5(5) . . ? O7 Re1 N21 80.7(4) . . ? C3 Re1 N11 95.9(5) . . ? C1 Re1 N11 93.4(5) . . ? C2 Re1 N11 175.5(5) . . ? O7 Re1 N11 79.1(3) . . ? N21 Re1 N11 83.1(4) . . ? C6 Re2 C4 90.2(6) . . ? C6 Re2 C5 86.3(6) . . ? C4 Re2 C5 90.2(5) . . ? C6 Re2 O7 174.2(4) . . ? C4 Re2 O7 95.5(5) . . ? C5 Re2 O7 94.4(5) . . ? C6 Re2 N22 98.1(5) . . ? C4 Re2 N22 89.5(5) . . ? C5 Re2 N22 175.6(5) . . ? O7 Re2 N22 81.3(4) . . ? C6 Re2 N12 94.4(5) . . ? C4 Re2 N12 171.1(5) . . ? C5 Re2 N12 97.7(5) . . ? O7 Re2 N12 79.8(4) . . ? N22 Re2 N12 82.3(4) . . ? N14 Ag N24 158.9(4) . 4_565 ? O1 C1 Re1 175.6(12) . . ? O2 C2 Re1 177.3(13) . . ? O3 C3 Re1 178.3(12) . . ? O4 C4 Re2 178.7(13) . . ? O5 C5 Re2 175.4(12) . . ? O6 C6 Re2 176.8(13) . . ? Re2 O7 Re1 117.4(4) . . ? C15 N11 N12 106.5(10) . . ? C15 N11 Re1 130.6(8) . . ? N12 N11 Re1 123.0(7) . . ? C13 N12 N11 106.1(10) . . ? C13 N12 Re2 133.8(9) . . ? N11 N12 Re2 120.1(8) . . ? N12 C13 N14 112.9(12) . . ? C13 N14 C15 102.2(11) . . ? C13 N14 Ag 133.2(9) . . ? C15 N14 Ag 124.3(8) . . ? N11 C15 N14 112.2(11) . . ? C25 N21 N22 106.1(10) . . ? C25 N21 Re1 132.9(9) . . ? N22 N21 Re1 121.0(8) . . ? C23 N22 N21 105.2(11) . . ? C23 N22 Re2 132.3(9) . . ? N21 N22 Re2 122.2(8) . . ? N22 C23 N24 113.4(12) . . ? C23 N24 C25 102.9(11) . . ? C23 N24 Ag 129.2(8) . 4_666 ? C25 N24 Ag 127.5(9) . 4_666 ? N21 C25 N24 112.4(12) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 22.07 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.058 _refine_diff_density_min -2.383 _refine_diff_density_rms 0.252