# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Professor Isabel Goncalves' _publ_contact_author_address ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; _publ_contact_author_email igoncalves@dq.ua.pt _publ_contact_author_fax '+351 234 370084' _publ_contact_author_phone '+351 234 378190' loop_ _publ_author_name _publ_author_footnote _publ_author_address T.R.Amarante . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'F.A.Almeida Paz' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; N.J.O.Silva . ; Instituto de Ciencia de Materiales de Aragon CSIC - Universidad de Zaragoza 50009 Zaragoza Spain ; M.Pillinger . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; ; A.D.Lopes ; . ; Department of Chemistry and Biochemistry Faculty of Sciences and Technology University of Algarve 8005-139 Faro Portugal ; F.Palacio . ; Instituto de Ciencia de Materiales de Aragon CSIC - Universidad de Zaragoza 50009 Zaragoza Spain ; F.Kuhn . ; Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrabe 4 D-85747 Garching bei Munchen Germany ; C.C.Romao . ; Instituto de Tecnologia Quimica e Biologica Universidade Nova de Lisboa Quinta do Marques, EAN Apartado 127 2781-901 Oeiras Portugal ; I.S.Goncalves . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; data_1 _database_code_depnum_ccdc_archive 'CCDC 703470' # ======================================================================= _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '20 June 2008' # ======================================================================= _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H20 Fe5 N4 O16 Re2' _chemical_formula_sum 'C32 H20 Fe5 N4 O16 Re2' _chemical_formula_weight 1368.17 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' Fe Fe 0.3463 0.8444 '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' _symmetry_space_group_name_Hall '-P 2yn' 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 12.235(4) _cell_length_b 11.833(4) _cell_length_c 14.492(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.606(16) _cell_angle_gamma 90.00 _cell_volume 2020.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8396 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 34.95 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 7.783 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3051 _exptl_absorpt_correction_T_max 0.4088 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker X8 Kappa CCD APEX II' _diffrn_measurement_method 'omega/phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78359 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 36.32 _reflns_number_total 9700 _reflns_number_gt 7837 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 ' _computing_data_reduction 'SAINT+ (Bruker, 1997-2005)' _computing_structure_solution 'SHELXTL (Bruker 2001)' _computing_structure_refinement 'SHELXTL ' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material 'SHELXTL ' _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^)+(0.0242P)^2^+4.8353P] 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 9700 _refine_ls_number_parameters 283 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.059 _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 Fe1 Fe 0.5000 0.5000 0.0000 0.01720(9) Uani 1 2 d S . . Fe2 Fe 0.22118(3) 0.69031(3) 0.15512(3) 0.02035(7) Uani 1 1 d . . . Fe3 Fe 0.73005(3) 0.59193(3) 0.33781(2) 0.01852(7) Uani 1 1 d . . . O1 O 0.41304(17) 0.35047(18) 0.01716(17) 0.0328(4) Uani 1 1 d D . . N1 N 0.3682(2) 0.5935(2) 0.03611(19) 0.0286(5) Uani 1 1 d . . . N2 N 0.5859(2) 0.4993(3) 0.14853(18) 0.0355(6) Uani 1 1 d . . . Re1 Re 0.28949(8) 0.27328(8) 0.01993(5) 0.01917(7) Uani 0.50 1 d PD A 1 O2 O 0.2063(5) 0.3434(5) 0.0777(4) 0.0480(7) Uiso 0.50 1 d PD A 1 O3 O 0.2112(5) 0.2520(5) -0.0999(4) 0.0480(7) Uiso 0.50 1 d PD A 1 O4 O 0.3299(9) 0.1479(6) 0.0714(7) 0.043(3) Uani 0.50 1 d PD A 1 Re1' Re 0.29281(10) 0.29073(9) 0.02377(7) 0.0407(3) Uani 0.50 1 d PD A 2 O2' O 0.2444(5) 0.3447(5) 0.1128(4) 0.0480(7) Uiso 0.50 1 d PD A 2 O3' O 0.1924(5) 0.2882(5) -0.0840(4) 0.0480(7) Uiso 0.50 1 d PD A 2 O4' O 0.3223(9) 0.1419(5) 0.0533(7) 0.0337(19) Uani 0.50 1 d PD A 2 O5 O 0.3818(2) 0.5969(3) 0.3242(2) 0.0581(8) Uani 1 1 d . . . O6 O 0.3342(3) 0.9090(2) 0.1707(2) 0.0576(8) Uani 1 1 d . . . O7 O 0.59939(19) 0.4781(2) 0.45095(17) 0.0360(5) Uani 1 1 d . . . O8 O 0.5967(3) 0.7997(2) 0.3182(2) 0.0513(7) Uani 1 1 d . . . C1 C 0.3107(2) 0.6311(2) 0.0796(2) 0.0239(5) Uani 1 1 d . A . C2 C 0.3189(2) 0.6341(3) 0.2591(2) 0.0337(6) Uani 1 1 d . . . C3 C 0.2902(3) 0.8240(3) 0.1648(2) 0.0347(6) Uani 1 1 d . . . C4 C 0.0922(2) 0.5697(3) 0.1336(2) 0.0316(6) Uani 1 1 d . . . H4 H 0.1040 0.4904 0.1387 0.038 Uiso 1 1 calc R . . C5 C 0.0864(2) 0.6443(3) 0.2086(2) 0.0296(6) Uani 1 1 d . . . H5 H 0.0932 0.6232 0.2732 0.036 Uiso 1 1 calc R . . C6 C 0.0689(3) 0.7550(3) 0.1716(3) 0.0364(7) Uani 1 1 d . . . H6 H 0.0623 0.8214 0.2065 0.044 Uiso 1 1 calc R . . C7 C 0.0631(3) 0.7487(4) 0.0721(3) 0.0438(9) Uani 1 1 d . . . H7 H 0.0516 0.8106 0.0288 0.053 Uiso 1 1 calc R . . C8 C 0.0771(2) 0.6357(4) 0.0495(2) 0.0397(8) Uani 1 1 d . . . H8 H 0.0767 0.6077 -0.0120 0.048 Uiso 1 1 calc R . . C9 C 0.6377(2) 0.5331(3) 0.22162(19) 0.0276(5) Uani 1 1 d . A . C10 C 0.6508(2) 0.5209(2) 0.40689(18) 0.0228(4) Uani 1 1 d . . . C11 C 0.6487(3) 0.7182(3) 0.3259(2) 0.0312(6) Uani 1 1 d . . . C12 C 0.8710(2) 0.4862(3) 0.3584(2) 0.0322(6) Uani 1 1 d . . . H12 H 0.8678 0.4060 0.3567 0.039 Uiso 1 1 calc R . . C13 C 0.8814(2) 0.5554(3) 0.4404(2) 0.0365(7) Uani 1 1 d . . . H13 H 0.8866 0.5293 0.5034 0.044 Uiso 1 1 calc R . . C14 C 0.8824(3) 0.6678(4) 0.4128(3) 0.0437(9) Uani 1 1 d . . . H14 H 0.8891 0.7316 0.4539 0.052 Uiso 1 1 calc R . . C15 C 0.8717(3) 0.6711(3) 0.3123(3) 0.0401(7) Uani 1 1 d . . . H15 H 0.8686 0.7369 0.2741 0.048 Uiso 1 1 calc R . . C16 C 0.8665(2) 0.5584(3) 0.2804(2) 0.0337(6) Uani 1 1 d . . . H16 H 0.8609 0.5349 0.2166 0.040 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 Fe1 0.01593(18) 0.0190(2) 0.01577(18) -0.00489(16) 0.00273(15) 0.00162(15) Fe2 0.01842(14) 0.02066(17) 0.02409(15) 0.00147(12) 0.00937(12) 0.00332(12) Fe3 0.01670(13) 0.02333(17) 0.01549(13) -0.00130(12) 0.00426(11) -0.00260(12) O1 0.0272(9) 0.0231(10) 0.0480(13) -0.0015(9) 0.0101(9) -0.0018(8) N1 0.0279(10) 0.0248(12) 0.0373(12) -0.0019(9) 0.0158(9) 0.0050(9) N2 0.0276(11) 0.0532(18) 0.0226(10) -0.0069(11) 0.0017(9) -0.0016(11) Re1 0.02167(14) 0.01215(16) 0.02317(14) 0.00344(10) 0.00512(11) -0.00021(10) O4 0.072(6) 0.028(4) 0.030(5) -0.003(3) 0.012(4) -0.006(3) Re1' 0.0340(3) 0.0376(5) 0.0575(4) 0.0190(3) 0.0244(3) 0.0024(2) O4' 0.054(4) 0.021(3) 0.022(3) -0.001(2) 0.002(2) -0.009(3) O5 0.0352(13) 0.094(3) 0.0416(14) 0.0206(15) 0.0045(11) 0.0176(14) O6 0.083(2) 0.0306(14) 0.0677(19) -0.0130(13) 0.0345(17) -0.0203(14) O7 0.0317(10) 0.0397(13) 0.0417(12) 0.0134(10) 0.0187(9) 0.0029(9) O8 0.0595(17) 0.0367(14) 0.0612(17) 0.0156(13) 0.0223(14) 0.0189(12) C1 0.0233(10) 0.0197(11) 0.0308(12) -0.0001(9) 0.0108(9) 0.0019(9) C2 0.0238(11) 0.0453(18) 0.0332(14) 0.0048(13) 0.0097(10) 0.0043(11) C3 0.0430(16) 0.0270(15) 0.0400(15) -0.0057(12) 0.0213(13) -0.0015(12) C4 0.0240(11) 0.0358(16) 0.0351(14) -0.0020(12) 0.0080(10) -0.0070(11) C5 0.0224(11) 0.0387(16) 0.0314(13) 0.0069(11) 0.0135(10) 0.0033(10) C6 0.0273(12) 0.0368(16) 0.0511(18) 0.0060(14) 0.0210(13) 0.0122(11) C7 0.0268(13) 0.060(2) 0.0466(18) 0.0259(17) 0.0135(13) 0.0138(14) C8 0.0215(11) 0.069(2) 0.0270(13) 0.0011(14) 0.0034(10) -0.0047(13) C9 0.0244(11) 0.0381(15) 0.0195(10) -0.0003(10) 0.0044(9) 0.0000(10) C10 0.0204(9) 0.0250(12) 0.0229(10) 0.0018(9) 0.0057(8) 0.0015(9) C11 0.0330(13) 0.0312(15) 0.0311(13) 0.0055(11) 0.0117(11) 0.0004(11) C12 0.0202(10) 0.0367(16) 0.0394(15) -0.0024(12) 0.0074(10) 0.0033(10) C13 0.0181(10) 0.063(2) 0.0250(12) -0.0030(13) -0.0004(9) 0.0003(12) C14 0.0241(12) 0.054(2) 0.052(2) -0.0283(17) 0.0100(13) -0.0144(13) C15 0.0289(13) 0.0393(18) 0.058(2) 0.0042(15) 0.0217(14) -0.0078(12) C16 0.0236(11) 0.0517(19) 0.0293(13) -0.0058(13) 0.0132(10) -0.0019(12) _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 Fe1 O1 2.113(2) . ? Fe1 O1 2.113(2) 3_665 ? Fe1 N2 2.126(3) 3_665 ? Fe1 N2 2.126(3) . ? Fe1 N1 2.133(2) 3_665 ? Fe1 N1 2.133(2) . ? Fe2 C2 1.781(3) . ? Fe2 C3 1.781(3) . ? Fe2 C1 1.880(3) . ? Fe2 C5 2.074(3) . ? Fe2 C6 2.086(3) . ? Fe2 C4 2.087(3) . ? Fe2 C7 2.101(3) . ? Fe2 C8 2.101(3) . ? Fe3 C11 1.778(3) . ? Fe3 C10 1.781(3) . ? Fe3 C9 1.890(3) . ? Fe3 C13 2.084(3) . ? Fe3 C12 2.087(3) . ? Fe3 C15 2.088(3) . ? Fe3 C14 2.091(3) . ? Fe3 C16 2.094(3) . ? O1 Re1' 1.658(2) . ? O1 Re1 1.776(2) . ? N1 C1 1.152(3) . ? N2 C9 1.150(4) . ? Re1 O4 1.674(6) . ? Re1 O2 1.698(5) . ? Re1 O3 1.760(5) . ? Re1' O2' 1.684(5) . ? Re1' O3' 1.708(5) . ? Re1' O4' 1.826(5) . ? O5 C2 1.134(4) . ? O6 C3 1.133(4) . ? O7 C10 1.129(3) . ? O8 C11 1.144(4) . ? C4 C8 1.416(5) . ? C4 C5 1.416(4) . ? C4 H4 0.9500 . ? C5 C6 1.409(5) . ? C5 H5 0.9500 . ? C6 C7 1.426(5) . ? C6 H6 0.9500 . ? C7 C8 1.399(6) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C12 C16 1.406(5) . ? C12 C13 1.420(5) . ? C12 H12 0.9500 . ? C13 C14 1.390(6) . ? C13 H13 0.9500 . ? C14 C15 1.428(6) . ? C14 H14 0.9500 . ? C15 C16 1.407(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O1 180.00(13) . 3_665 ? O1 Fe1 N2 89.71(11) . 3_665 ? O1 Fe1 N2 90.29(11) 3_665 3_665 ? O1 Fe1 N2 90.29(11) . . ? O1 Fe1 N2 89.71(11) 3_665 . ? N2 Fe1 N2 180.00(19) 3_665 . ? O1 Fe1 N1 91.85(9) . 3_665 ? O1 Fe1 N1 88.15(9) 3_665 3_665 ? N2 Fe1 N1 87.38(11) 3_665 3_665 ? N2 Fe1 N1 92.62(11) . 3_665 ? O1 Fe1 N1 88.15(9) . . ? O1 Fe1 N1 91.85(9) 3_665 . ? N2 Fe1 N1 92.62(11) 3_665 . ? N2 Fe1 N1 87.38(11) . . ? N1 Fe1 N1 180.0 3_665 . ? C2 Fe2 C3 93.93(17) . . ? C2 Fe2 C1 89.43(13) . . ? C3 Fe2 C1 92.22(13) . . ? C2 Fe2 C5 90.34(13) . . ? C3 Fe2 C5 127.69(13) . . ? C1 Fe2 C5 139.99(13) . . ? C2 Fe2 C6 117.19(14) . . ? C3 Fe2 C6 94.84(15) . . ? C1 Fe2 C6 151.81(14) . . ? C5 Fe2 C6 39.61(13) . . ? C2 Fe2 C4 100.35(15) . . ? C3 Fe2 C4 160.44(15) . . ? C1 Fe2 C4 101.17(12) . . ? C5 Fe2 C4 39.79(12) . . ? C6 Fe2 C4 66.76(14) . . ? C2 Fe2 C7 155.81(13) . . ? C3 Fe2 C7 95.57(17) . . ? C1 Fe2 C7 112.34(14) . . ? C5 Fe2 C7 66.32(13) . . ? C6 Fe2 C7 39.81(15) . . ? C4 Fe2 C7 66.23(15) . . ? C2 Fe2 C8 137.89(16) . . ? C3 Fe2 C8 128.17(16) . . ? C1 Fe2 C8 88.11(13) . . ? C5 Fe2 C8 66.18(12) . . ? C6 Fe2 C8 66.19(15) . . ? C4 Fe2 C8 39.53(13) . . ? C7 Fe2 C8 38.89(17) . . ? C11 Fe3 C10 94.35(13) . . ? C11 Fe3 C9 92.19(14) . . ? C10 Fe3 C9 92.36(12) . . ? C11 Fe3 C13 127.60(15) . . ? C10 Fe3 C13 90.87(13) . . ? C9 Fe3 C13 139.69(14) . . ? C11 Fe3 C12 159.65(14) . . ? C10 Fe3 C12 101.00(13) . . ? C9 Fe3 C12 100.37(13) . . ? C13 Fe3 C12 39.81(13) . . ? C11 Fe3 C15 94.32(15) . . ? C10 Fe3 C15 156.15(14) . . ? C9 Fe3 C15 109.45(14) . . ? C13 Fe3 C15 66.36(15) . . ? C12 Fe3 C15 66.48(14) . . ? C11 Fe3 C14 94.98(16) . . ? C10 Fe3 C14 117.04(14) . . ? C9 Fe3 C14 148.99(13) . . ? C13 Fe3 C14 38.88(16) . . ? C12 Fe3 C14 66.18(14) . . ? C15 Fe3 C14 39.96(16) . . ? C11 Fe3 C16 127.31(14) . . ? C10 Fe3 C16 138.32(13) . . ? C9 Fe3 C16 85.76(12) . . ? C13 Fe3 C16 66.02(12) . . ? C12 Fe3 C16 39.31(13) . . ? C15 Fe3 C16 39.32(14) . . ? C14 Fe3 C16 66.01(13) . . ? Re1' O1 Fe1 147.81(13) . . ? Re1 O1 Fe1 153.10(13) . . ? C1 N1 Fe1 161.3(2) . . ? C9 N2 Fe1 158.6(3) . . ? O4 Re1 O2 111.0(4) . . ? O4 Re1 O3 109.3(4) . . ? O2 Re1 O3 108.5(3) . . ? O4 Re1 O1 108.3(4) . . ? O2 Re1 O1 112.8(2) . . ? O3 Re1 O1 107.0(2) . . ? O1 Re1' O2' 112.5(2) . . ? O1 Re1' O3' 112.7(2) . . ? O2' Re1' O3' 113.1(3) . . ? O1 Re1' O4' 107.6(3) . . ? O2' Re1' O4' 105.9(4) . . ? O3' Re1' O4' 104.2(4) . . ? N1 C1 Fe2 177.6(3) . . ? O5 C2 Fe2 178.7(3) . . ? O6 C3 Fe2 179.8(3) . . ? C8 C4 C5 107.2(3) . . ? C8 C4 Fe2 70.75(18) . . ? C5 C4 Fe2 69.60(17) . . ? C8 C4 H4 126.4 . . ? C5 C4 H4 126.4 . . ? Fe2 C4 H4 124.8 . . ? C6 C5 C4 108.7(3) . . ? C6 C5 Fe2 70.64(16) . . ? C4 C5 Fe2 70.61(16) . . ? C6 C5 H5 125.7 . . ? C4 C5 H5 125.7 . . ? Fe2 C5 H5 124.7 . . ? C5 C6 C7 107.3(3) . . ? C5 C6 Fe2 69.76(15) . . ? C7 C6 Fe2 70.67(17) . . ? C5 C6 H6 126.3 . . ? C7 C6 H6 126.3 . . ? Fe2 C6 H6 124.8 . . ? C8 C7 C6 108.1(3) . . ? C8 C7 Fe2 70.55(18) . . ? C6 C7 Fe2 69.52(18) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Fe2 C7 H7 125.5 . . ? C7 C8 C4 108.7(3) . . ? C7 C8 Fe2 70.6(2) . . ? C4 C8 Fe2 69.72(17) . . ? C7 C8 H8 125.6 . . ? C4 C8 H8 125.6 . . ? Fe2 C8 H8 125.7 . . ? N2 C9 Fe3 176.2(3) . . ? O7 C10 Fe3 178.5(3) . . ? O8 C11 Fe3 179.8(3) . . ? C16 C12 C13 107.3(3) . . ? C16 C12 Fe3 70.64(17) . . ? C13 C12 Fe3 69.99(17) . . ? C16 C12 H12 126.4 . . ? C13 C12 H12 126.4 . . ? Fe3 C12 H12 124.6 . . ? C14 C13 C12 108.5(3) . . ? C14 C13 Fe3 70.85(19) . . ? C12 C13 Fe3 70.20(16) . . ? C14 C13 H13 125.7 . . ? C12 C13 H13 125.7 . . ? Fe3 C13 H13 124.8 . . ? C13 C14 C15 108.2(3) . . ? C13 C14 Fe3 70.26(17) . . ? C15 C14 Fe3 69.91(18) . . ? C13 C14 H14 125.9 . . ? C15 C14 H14 125.9 . . ? Fe3 C14 H14 125.5 . . ? C16 C15 C14 107.0(3) . . ? C16 C15 Fe3 70.56(17) . . ? C14 C15 Fe3 70.13(18) . . ? C16 C15 H15 126.5 . . ? C14 C15 H15 126.5 . . ? Fe3 C15 H15 124.5 . . ? C12 C16 C15 108.9(3) . . ? C12 C16 Fe3 70.05(16) . . ? C15 C16 Fe3 70.12(17) . . ? C12 C16 H16 125.6 . . ? C15 C16 H16 125.6 . . ? Fe3 C16 H16 125.8 . . ? 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 N2 Fe1 O1 Re1' -74.7(3) 3_665 . . . ? N2 Fe1 O1 Re1' 105.3(3) . . . . ? N1 Fe1 O1 Re1' -162.1(3) 3_665 . . . ? N1 Fe1 O1 Re1' 17.9(3) . . . . ? N2 Fe1 O1 Re1 -68.9(3) 3_665 . . . ? N2 Fe1 O1 Re1 111.1(3) . . . . ? N1 Fe1 O1 Re1 -156.3(3) 3_665 . . . ? N1 Fe1 O1 Re1 23.7(3) . . . . ? O1 Fe1 N1 C1 69.7(7) . . . . ? O1 Fe1 N1 C1 -110.3(7) 3_665 . . . ? N2 Fe1 N1 C1 159.3(7) 3_665 . . . ? N2 Fe1 N1 C1 -20.7(7) . . . . ? O1 Fe1 N2 C9 -162.4(7) . . . . ? O1 Fe1 N2 C9 17.6(7) 3_665 . . . ? N1 Fe1 N2 C9 105.7(7) 3_665 . . . ? N1 Fe1 N2 C9 -74.3(7) . . . . ? Re1' O1 Re1 O4 -134.6(7) . . . . ? Fe1 O1 Re1 O4 -165.6(5) . . . . ? Re1' O1 Re1 O2 -11.4(6) . . . . ? Fe1 O1 Re1 O2 -42.4(4) . . . . ? Re1' O1 Re1 O3 107.7(6) . . . . ? Fe1 O1 Re1 O3 76.8(4) . . . . ? Re1 O1 Re1' O2' 147.8(7) . . . . ? Fe1 O1 Re1' O2' -58.2(4) . . . . ? Re1 O1 Re1' O3' -82.9(6) . . . . ? Fe1 O1 Re1' O3' 71.2(4) . . . . ? Re1 O1 Re1' O4' 31.5(6) . . . . ? Fe1 O1 Re1' O4' -174.5(4) . . . . ? C2 Fe2 C4 C8 -164.5(2) . . . . ? C3 Fe2 C4 C8 59.3(5) . . . . ? C1 Fe2 C4 C8 -73.0(2) . . . . ? C5 Fe2 C4 C8 117.6(3) . . . . ? C6 Fe2 C4 C8 80.2(2) . . . . ? C7 Fe2 C4 C8 36.6(2) . . . . ? C2 Fe2 C4 C5 77.9(2) . . . . ? C3 Fe2 C4 C5 -58.3(5) . . . . ? C1 Fe2 C4 C5 169.36(18) . . . . ? C6 Fe2 C4 C5 -37.39(19) . . . . ? C7 Fe2 C4 C5 -81.0(2) . . . . ? C8 Fe2 C4 C5 -117.6(3) . . . . ? C8 C4 C5 C6 -0.5(3) . . . . ? Fe2 C4 C5 C6 60.7(2) . . . . ? C8 C4 C5 Fe2 -61.1(2) . . . . ? C2 Fe2 C5 C6 135.2(2) . . . . ? C3 Fe2 C5 C6 40.0(3) . . . . ? C1 Fe2 C5 C6 -135.3(2) . . . . ? C4 Fe2 C5 C6 -118.9(3) . . . . ? C7 Fe2 C5 C6 -38.2(2) . . . . ? C8 Fe2 C5 C6 -80.9(2) . . . . ? C2 Fe2 C5 C4 -105.9(2) . . . . ? C3 Fe2 C5 C4 158.9(2) . . . . ? C1 Fe2 C5 C4 -16.4(3) . . . . ? C6 Fe2 C5 C4 118.9(3) . . . . ? C7 Fe2 C5 C4 80.7(2) . . . . ? C8 Fe2 C5 C4 38.1(2) . . . . ? C4 C5 C6 C7 0.4(3) . . . . ? Fe2 C5 C6 C7 61.0(2) . . . . ? C4 C5 C6 Fe2 -60.6(2) . . . . ? C2 Fe2 C6 C5 -52.4(3) . . . . ? C3 Fe2 C6 C5 -149.3(2) . . . . ? C1 Fe2 C6 C5 106.8(3) . . . . ? C4 Fe2 C6 C5 37.56(19) . . . . ? C7 Fe2 C6 C5 117.8(3) . . . . ? C8 Fe2 C6 C5 80.8(2) . . . . ? C2 Fe2 C6 C7 -170.2(2) . . . . ? C3 Fe2 C6 C7 92.9(3) . . . . ? C1 Fe2 C6 C7 -11.0(4) . . . . ? C5 Fe2 C6 C7 -117.8(3) . . . . ? C4 Fe2 C6 C7 -80.2(2) . . . . ? C8 Fe2 C6 C7 -36.9(2) . . . . ? C5 C6 C7 C8 -0.1(4) . . . . ? Fe2 C6 C7 C8 60.3(2) . . . . ? C5 C6 C7 Fe2 -60.4(2) . . . . ? C2 Fe2 C7 C8 -97.1(4) . . . . ? C3 Fe2 C7 C8 150.2(2) . . . . ? C1 Fe2 C7 C8 55.5(2) . . . . ? C5 Fe2 C7 C8 -80.9(2) . . . . ? C6 Fe2 C7 C8 -118.9(3) . . . . ? C4 Fe2 C7 C8 -37.22(19) . . . . ? C2 Fe2 C7 C6 21.8(5) . . . . ? C3 Fe2 C7 C6 -90.9(2) . . . . ? C1 Fe2 C7 C6 174.4(2) . . . . ? C5 Fe2 C7 C6 38.0(2) . . . . ? C4 Fe2 C7 C6 81.7(2) . . . . ? C8 Fe2 C7 C6 118.9(3) . . . . ? C6 C7 C8 C4 -0.1(4) . . . . ? Fe2 C7 C8 C4 59.5(2) . . . . ? C6 C7 C8 Fe2 -59.6(2) . . . . ? C5 C4 C8 C7 0.4(3) . . . . ? Fe2 C4 C8 C7 -60.0(2) . . . . ? C5 C4 C8 Fe2 60.38(19) . . . . ? C2 Fe2 C8 C7 142.7(2) . . . . ? C3 Fe2 C8 C7 -38.9(3) . . . . ? C1 Fe2 C8 C7 -130.3(2) . . . . ? C5 Fe2 C8 C7 81.3(2) . . . . ? C6 Fe2 C8 C7 37.8(2) . . . . ? C4 Fe2 C8 C7 119.6(3) . . . . ? C2 Fe2 C8 C4 23.1(3) . . . . ? C3 Fe2 C8 C4 -158.5(2) . . . . ? C1 Fe2 C8 C4 110.1(2) . . . . ? C5 Fe2 C8 C4 -38.31(19) . . . . ? C6 Fe2 C8 C4 -81.8(2) . . . . ? C7 Fe2 C8 C4 -119.6(3) . . . . ? C11 Fe3 C12 C16 -57.2(4) . . . . ? C10 Fe3 C12 C16 164.48(19) . . . . ? C9 Fe3 C12 C16 70.0(2) . . . . ? C13 Fe3 C12 C16 -117.6(3) . . . . ? C15 Fe3 C12 C16 -36.8(2) . . . . ? C14 Fe3 C12 C16 -80.7(2) . . . . ? C11 Fe3 C12 C13 60.4(5) . . . . ? C10 Fe3 C12 C13 -77.9(2) . . . . ? C9 Fe3 C12 C13 -172.4(2) . . . . ? C15 Fe3 C12 C13 80.7(2) . . . . ? C14 Fe3 C12 C13 36.9(2) . . . . ? C16 Fe3 C12 C13 117.6(3) . . . . ? C16 C12 C13 C14 0.4(3) . . . . ? Fe3 C12 C13 C14 -60.8(2) . . . . ? C16 C12 C13 Fe3 61.1(2) . . . . ? C11 Fe3 C13 C14 -38.7(3) . . . . ? C10 Fe3 C13 C14 -134.9(2) . . . . ? C9 Fe3 C13 C14 130.4(2) . . . . ? C12 Fe3 C13 C14 118.9(3) . . . . ? C15 Fe3 C13 C14 37.8(2) . . . . ? C16 Fe3 C13 C14 81.0(2) . . . . ? C11 Fe3 C13 C12 -157.6(2) . . . . ? C10 Fe3 C13 C12 106.3(2) . . . . ? C9 Fe3 C13 C12 11.6(3) . . . . ? C15 Fe3 C13 C12 -81.1(2) . . . . ? C14 Fe3 C13 C12 -118.9(3) . . . . ? C16 Fe3 C13 C12 -37.9(2) . . . . ? C12 C13 C14 C15 0.5(3) . . . . ? Fe3 C13 C14 C15 -59.8(2) . . . . ? C12 C13 C14 Fe3 60.4(2) . . . . ? C11 Fe3 C14 C13 150.2(2) . . . . ? C10 Fe3 C14 C13 52.7(2) . . . . ? C9 Fe3 C14 C13 -107.1(3) . . . . ? C12 Fe3 C14 C13 -37.80(19) . . . . ? C15 Fe3 C14 C13 -119.0(3) . . . . ? C16 Fe3 C14 C13 -81.0(2) . . . . ? C11 Fe3 C14 C15 -90.8(2) . . . . ? C10 Fe3 C14 C15 171.7(2) . . . . ? C9 Fe3 C14 C15 11.9(4) . . . . ? C13 Fe3 C14 C15 119.0(3) . . . . ? C12 Fe3 C14 C15 81.2(2) . . . . ? C16 Fe3 C14 C15 38.1(2) . . . . ? C13 C14 C15 C16 -1.2(4) . . . . ? Fe3 C14 C15 C16 -61.3(2) . . . . ? C13 C14 C15 Fe3 60.1(2) . . . . ? C11 Fe3 C15 C16 -150.1(2) . . . . ? C10 Fe3 C15 C16 98.8(4) . . . . ? C9 Fe3 C15 C16 -56.3(2) . . . . ? C13 Fe3 C15 C16 80.5(2) . . . . ? C12 Fe3 C15 C16 36.8(2) . . . . ? C14 Fe3 C15 C16 117.3(3) . . . . ? C11 Fe3 C15 C14 92.6(2) . . . . ? C10 Fe3 C15 C14 -18.4(5) . . . . ? C9 Fe3 C15 C14 -173.5(2) . . . . ? C13 Fe3 C15 C14 -36.8(2) . . . . ? C12 Fe3 C15 C14 -80.4(2) . . . . ? C16 Fe3 C15 C14 -117.3(3) . . . . ? C13 C12 C16 C15 -1.1(3) . . . . ? Fe3 C12 C16 C15 59.6(2) . . . . ? C13 C12 C16 Fe3 -60.71(19) . . . . ? C14 C15 C16 C12 1.4(3) . . . . ? Fe3 C15 C16 C12 -59.5(2) . . . . ? C14 C15 C16 Fe3 61.0(2) . . . . ? C11 Fe3 C16 C12 158.4(2) . . . . ? C10 Fe3 C16 C12 -23.3(3) . . . . ? C9 Fe3 C16 C12 -112.0(2) . . . . ? C13 Fe3 C16 C12 38.4(2) . . . . ? C15 Fe3 C16 C12 119.8(3) . . . . ? C14 Fe3 C16 C12 81.1(2) . . . . ? C11 Fe3 C16 C15 38.6(3) . . . . ? C10 Fe3 C16 C15 -143.1(2) . . . . ? C9 Fe3 C16 C15 128.1(2) . . . . ? C13 Fe3 C16 C15 -81.4(2) . . . . ? C12 Fe3 C16 C15 -119.8(3) . . . . ? C14 Fe3 C16 C15 -38.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 36.32 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 3.468 _refine_diff_density_min -2.166 _refine_diff_density_rms 0.143 # ===== END ===== # # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 703471' # ======================================================================= _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '23 June 2008' # ======================================================================= _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H9 Fe N3 O8 Re2' _chemical_formula_sum 'C6 H9 Fe N3 O8 Re2' _chemical_formula_weight 679.43 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1668(18) _cell_length_b 8.5307(17) _cell_length_c 11.649(2) _cell_angle_alpha 71.125(9) _cell_angle_beta 78.002(10) _cell_angle_gamma 89.368(11) _cell_volume 749.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8046 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 46.15 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 17.094 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1982 _exptl_absorpt_correction_T_max 0.2797 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker X8 Kappa CCD APEX II' _diffrn_measurement_method 'omega/phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36714 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 33.14 _reflns_number_total 5692 _reflns_number_gt 5343 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 ' _computing_data_reduction 'SAINT+ (Bruker, 1997-2005)' _computing_structure_solution 'SHELXTL (Bruker 2001)' _computing_structure_refinement 'SHELXTL ' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material 'SHELXTL ' _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^)+(0.0294P)^2^+2.3391P] 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 SHELXL _refine_ls_extinction_coef 0.0077(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5692 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.191047(19) -0.03118(2) 0.776088(13) 0.01445(5) Uani 1 1 d . . . Re2 Re 0.476207(17) 0.454227(17) 0.331422(13) 0.01083(5) Uani 1 1 d . . . Fe1 Fe 0.5000 0.0000 0.5000 0.00998(13) Uani 1 2 d S . . Fe2 Fe 0.5000 0.5000 0.0000 0.01054(13) Uani 1 2 d S . . O1 O 0.3879(4) -0.0026(4) 0.6754(3) 0.0194(6) Uani 1 1 d . . . O2 O 0.2150(5) -0.0093(5) 0.9132(3) 0.0254(7) Uani 1 1 d . . . O3 O 0.0619(5) 0.1151(6) 0.7103(4) 0.0354(9) Uani 1 1 d . . . O4 O 0.1019(6) -0.2240(5) 0.8049(4) 0.0380(9) Uani 1 1 d . . . O5 O 0.4269(4) 0.2463(4) 0.4186(3) 0.0210(6) Uani 1 1 d . . . O6 O 0.3009(4) 0.5625(4) 0.3497(3) 0.0223(6) Uani 1 1 d . . . O7 O 0.6335(5) 0.5323(5) 0.3769(3) 0.0275(7) Uani 1 1 d . . . O8 O 0.5437(4) 0.4769(4) 0.1741(3) 0.0191(6) Uani 1 1 d . . . N1 N 0.7313(5) 0.1083(5) 0.5091(3) 0.0184(7) Uani 1 1 d . . . C1 C 0.8467(6) 0.1957(5) 0.4817(4) 0.0192(8) Uani 1 1 d . . . C2 C 0.9943(7) 0.3096(7) 0.4415(5) 0.0333(12) Uani 1 1 d . . . H2A H 1.0650 0.2974 0.3661 0.050 Uiso 1 1 calc R . . H2B H 1.0579 0.2842 0.5073 0.050 Uiso 1 1 calc R . . H2C H 0.9596 0.4238 0.4238 0.050 Uiso 1 1 calc R . . N2 N 0.4149(5) 0.2422(4) 0.0696(4) 0.0196(7) Uani 1 1 d . . . C3 C 0.3811(5) 0.1024(5) 0.1140(4) 0.0158(7) Uani 1 1 d . . . C4 C 0.3434(6) -0.0747(5) 0.1697(4) 0.0201(8) Uani 1 1 d . . . H4A H 0.4060 -0.1193 0.2353 0.030 Uiso 1 1 calc R . . H4B H 0.3758 -0.1281 0.1061 0.030 Uiso 1 1 calc R . . H4C H 0.2229 -0.0968 0.2055 0.030 Uiso 1 1 calc R . . N3 N 0.2491(4) 0.5628(4) 0.0599(3) 0.0162(6) Uani 1 1 d . . . C5 C 0.1140(5) 0.5961(5) 0.0869(4) 0.0140(7) Uani 1 1 d . . . C6 C -0.0578(5) 0.6374(6) 0.1196(5) 0.0242(9) Uani 1 1 d . . . H6A H -0.1329 0.5592 0.1064 0.036 Uiso 1 1 calc R . . H6B H -0.0719 0.7504 0.0674 0.036 Uiso 1 1 calc R . . H6C H -0.0849 0.6305 0.2072 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01306(8) 0.01864(9) 0.01204(8) -0.00622(6) -0.00168(5) 0.00125(6) Re2 0.01104(8) 0.00839(7) 0.01273(8) -0.00398(5) -0.00095(5) -0.00164(5) Fe1 0.0094(3) 0.0083(3) 0.0114(3) -0.0031(2) -0.0004(2) -0.0015(2) Fe2 0.0102(3) 0.0091(3) 0.0121(3) -0.0036(2) -0.0016(2) 0.0008(2) O1 0.0146(13) 0.0269(16) 0.0184(13) -0.0129(12) 0.0020(10) -0.0035(11) O2 0.0303(18) 0.0333(18) 0.0161(14) -0.0127(13) -0.0049(12) 0.0067(14) O3 0.0272(19) 0.050(2) 0.0279(17) -0.0096(17) -0.0095(14) 0.0199(17) O4 0.047(2) 0.033(2) 0.0290(18) -0.0062(16) -0.0022(17) -0.0194(18) O5 0.0224(16) 0.0098(12) 0.0260(15) 0.0001(11) -0.0044(12) 0.0014(11) O6 0.0193(15) 0.0125(13) 0.0300(16) -0.0046(12) 0.0021(12) 0.0043(11) O7 0.0254(17) 0.0352(19) 0.0234(15) -0.0133(14) -0.0019(13) -0.0131(14) O8 0.0159(14) 0.0257(15) 0.0156(12) -0.0066(11) -0.0037(10) 0.0000(11) N1 0.0167(16) 0.0207(17) 0.0189(15) -0.0085(13) -0.0030(12) -0.0048(13) C1 0.0192(19) 0.0204(19) 0.0171(17) -0.0053(15) -0.0033(14) -0.0038(15) C2 0.024(2) 0.039(3) 0.034(3) -0.008(2) -0.0072(19) -0.018(2) N2 0.0205(17) 0.0139(15) 0.0233(17) -0.0066(13) -0.0014(13) -0.0003(13) C3 0.0139(17) 0.0153(17) 0.0192(17) -0.0073(14) -0.0030(13) 0.0005(13) C4 0.026(2) 0.0114(16) 0.0214(18) -0.0040(14) -0.0048(15) -0.0055(15) N3 0.0140(15) 0.0136(14) 0.0219(16) -0.0076(12) -0.0029(12) 0.0020(11) C5 0.0160(17) 0.0125(16) 0.0146(15) -0.0073(13) -0.0007(13) -0.0009(13) C6 0.0133(19) 0.027(2) 0.034(2) -0.0159(19) 0.0007(16) 0.0048(15) _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 O4 1.708(4) . ? Re1 O3 1.716(4) . ? Re1 O2 1.716(3) . ? Re1 O1 1.749(3) . ? Re2 O7 1.704(3) . ? Re2 O6 1.709(3) . ? Re2 O5 1.738(3) . ? Re2 O8 1.747(3) . ? Fe1 O1 2.051(3) . ? Fe1 O1 2.051(3) 2_656 ? Fe1 O5 2.142(3) . ? Fe1 O5 2.142(3) 2_656 ? Fe1 N1 2.149(4) . ? Fe1 N1 2.149(4) 2_656 ? Fe2 O8 2.079(3) 2_665 ? Fe2 O8 2.079(3) . ? Fe2 N3 2.144(3) . ? Fe2 N3 2.144(3) 2_665 ? Fe2 N2 2.150(4) 2_665 ? Fe2 N2 2.150(4) . ? N1 C1 1.133(5) . ? C1 C2 1.454(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? N2 C3 1.147(5) . ? C3 C4 1.446(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? N3 C5 1.142(5) . ? C5 C6 1.446(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Re1 O3 108.9(2) . . ? O4 Re1 O2 109.43(19) . . ? O3 Re1 O2 109.43(18) . . ? O4 Re1 O1 110.69(19) . . ? O3 Re1 O1 109.59(18) . . ? O2 Re1 O1 108.82(16) . . ? O7 Re2 O6 110.19(18) . . ? O7 Re2 O5 110.70(17) . . ? O6 Re2 O5 108.87(15) . . ? O7 Re2 O8 107.97(16) . . ? O6 Re2 O8 108.81(16) . . ? O5 Re2 O8 110.27(16) . . ? O1 Fe1 O1 180.0 . 2_656 ? O1 Fe1 O5 91.79(13) . . ? O1 Fe1 O5 88.21(13) 2_656 . ? O1 Fe1 O5 88.21(13) . 2_656 ? O1 Fe1 O5 91.79(13) 2_656 2_656 ? O5 Fe1 O5 180.00(19) . 2_656 ? O1 Fe1 N1 91.98(13) . . ? O1 Fe1 N1 88.02(13) 2_656 . ? O5 Fe1 N1 88.09(14) . . ? O5 Fe1 N1 91.91(14) 2_656 . ? O1 Fe1 N1 88.02(13) . 2_656 ? O1 Fe1 N1 91.98(13) 2_656 2_656 ? O5 Fe1 N1 91.91(14) . 2_656 ? O5 Fe1 N1 88.09(14) 2_656 2_656 ? N1 Fe1 N1 180.0(2) . 2_656 ? O8 Fe2 O8 180.0 2_665 . ? O8 Fe2 N3 91.04(13) 2_665 . ? O8 Fe2 N3 88.96(13) . . ? O8 Fe2 N3 88.96(13) 2_665 2_665 ? O8 Fe2 N3 91.04(13) . 2_665 ? N3 Fe2 N3 180.0 . 2_665 ? O8 Fe2 N2 88.78(14) 2_665 2_665 ? O8 Fe2 N2 91.22(14) . 2_665 ? N3 Fe2 N2 90.69(14) . 2_665 ? N3 Fe2 N2 89.31(14) 2_665 2_665 ? O8 Fe2 N2 91.22(14) 2_665 . ? O8 Fe2 N2 88.78(14) . . ? N3 Fe2 N2 89.31(14) . . ? N3 Fe2 N2 90.69(14) 2_665 . ? N2 Fe2 N2 180.0 2_665 . ? Re1 O1 Fe1 141.34(18) . . ? Re2 O5 Fe1 151.10(19) . . ? Re2 O8 Fe2 152.42(18) . . ? C1 N1 Fe1 160.0(4) . . ? N1 C1 C2 177.8(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 N2 Fe2 173.1(4) . . ? N2 C3 C4 178.4(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 N3 Fe2 176.9(3) . . ? N3 C5 C6 179.1(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Re1 O1 Fe1 60.0(3) . . . . ? O3 Re1 O1 Fe1 -60.1(3) . . . . ? O2 Re1 O1 Fe1 -179.7(3) . . . . ? O5 Fe1 O1 Re1 79.3(3) . . . . ? O5 Fe1 O1 Re1 -100.7(3) 2_656 . . . ? N1 Fe1 O1 Re1 167.4(3) . . . . ? N1 Fe1 O1 Re1 -12.6(3) 2_656 . . . ? O7 Re2 O5 Fe1 -46.4(4) . . . . ? O6 Re2 O5 Fe1 -167.6(4) . . . . ? O8 Re2 O5 Fe1 73.1(4) . . . . ? O1 Fe1 O5 Re2 119.9(4) . . . . ? O1 Fe1 O5 Re2 -60.1(4) 2_656 . . . ? N1 Fe1 O5 Re2 28.0(4) . . . . ? N1 Fe1 O5 Re2 -152.0(4) 2_656 . . . ? O7 Re2 O8 Fe2 -155.3(4) . . . . ? O6 Re2 O8 Fe2 -35.7(4) . . . . ? O5 Re2 O8 Fe2 83.6(4) . . . . ? N3 Fe2 O8 Re2 16.9(4) . . . . ? N3 Fe2 O8 Re2 -163.1(4) 2_665 . . . ? N2 Fe2 O8 Re2 107.6(4) 2_665 . . . ? N2 Fe2 O8 Re2 -72.4(4) . . . . ? O1 Fe1 N1 C1 -129.8(11) . . . . ? O1 Fe1 N1 C1 50.2(11) 2_656 . . . ? O5 Fe1 N1 C1 -38.0(11) . . . . ? O5 Fe1 N1 C1 142.0(11) 2_656 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.891 _refine_diff_density_min -3.633 _refine_diff_density_rms 0.277 # ===== END ===== #