Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_clair1 _database_code_CSD 152797 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bennington, Stephen M.' 'Cannon, R.' 'Jayasooriya, U.' 'Montfrooij, Wouter' 'Powell, Annie' 'Sowrey, Frank E.' 'Tilford, Claire' 'Wocadlo, Sigrid' _publ_contact_author_name 'Dr Frank E Sowrey' _publ_contact_author_address ; Dr Frank E Sowrey School of Physical Sciences University of Kent at Canterbury Canterbury CT2 7NZ ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hexakis(O,O'-\m-benzoate)(\m3-oxo)tris(pyridine)triiron(III) perchlorate pyridine solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H50 Cl Fe3 N4 O17' _chemical_formula_weight 1326.06 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P6(3)/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 13.541(3) _cell_length_b 13.541(3) _cell_length_c 19.136(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3038.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.96 _cell_measurement_theta_max 12.34 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1362 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.8 _diffrn_reflns_number 1687 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 23.16 _reflns_number_total 1477 _reflns_number_gt 798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'AFC7R Control Software (MSC, 1994)' _computing_cell_refinement 'AFC7R Control Software (MSC, 1994)' _computing_data_reduction 'TEXSAN 1.6 (MSC, 1996)' _computing_structure_solution 'XS in SHELXTL/PC 5.03 (Siemens, 1995)' _computing_structure_refinement 'XL in SHELXTL/PC 5.03 (Siemens, 1995)' _computing_molecular_graphics 'XP in SHELXTL/PC 5.03 (Siemens, 1995)' _computing_publication_material 'XCIF in SHELXTL/PC 5.03 (Siemens, 1995)' _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^)+(0.0464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1477 _refine_ls_number_parameters 149 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.012 _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 Fe1 Fe 0.21304(8) 0.51088(8) 0.2500 0.0481(4) Uani 1 2 d S . . N1 N 0.0749(5) 0.3313(5) 0.2500 0.0536(16) Uani 1 2 d S . . O1 O 0.3333 0.6667 0.2500 0.0414(19) Uani 1 6 d S . . O2 O 0.2824(3) 0.4595(3) 0.17547(18) 0.0578(10) Uani 1 1 d . . . O3 O 0.4691(3) 0.5874(3) 0.17622(18) 0.0624(10) Uani 1 1 d . . . C1 C 0.3841(5) 0.4942(4) 0.1562(3) 0.0514(13) Uani 1 1 d . . . C2 C 0.4056(4) 0.4239(4) 0.1053(3) 0.0508(12) Uani 1 1 d . . . C3 C 0.5165(5) 0.4546(5) 0.0859(3) 0.0705(16) Uani 1 1 d . . . H3 H 0.5787 0.5196 0.1056 0.085 Uiso 1 1 calc R . . C4 C 0.5352(5) 0.3894(6) 0.0376(3) 0.082(2) Uani 1 1 d . . . H4 H 0.6100 0.4087 0.0254 0.098 Uiso 1 1 calc R . . C5 C 0.4437(6) 0.2963(5) 0.0074(3) 0.0806(18) Uani 1 1 d . . . H5 H 0.4567 0.2540 -0.0266 0.097 Uiso 1 1 calc R . . C6 C 0.3343(5) 0.2641(5) 0.0262(3) 0.0688(16) Uani 1 1 d . . . H6 H 0.2725 0.1997 0.0057 0.083 Uiso 1 1 calc R . . C7 C 0.3155(4) 0.3273(4) 0.0756(3) 0.0582(14) Uani 1 1 d . . . H7 H 0.2404 0.3045 0.0893 0.070 Uiso 1 1 calc R . . C8 C 0.0323(4) 0.2756(5) 0.1899(3) 0.0642(15) Uani 1 1 d . . . H8 H 0.0609 0.3145 0.1474 0.077 Uiso 1 1 calc R . . C9 C -0.0534(5) 0.1613(5) 0.1884(3) 0.086(2) Uani 1 1 d . . . H9 H -0.0808 0.1234 0.1456 0.103 Uiso 1 1 calc R . . C10 C -0.0973(9) 0.1049(8) 0.2500 0.096(3) Uani 1 2 d S . . H10 H -0.1567 0.0286 0.2500 0.10(3) Uiso 1 2 calc SR . . Cl1 Cl 0.0000 0.0000 0.0000 0.1040(16) Uani 1 6 d SD . . O4 O 0.0945(12) 0.056(2) -0.0528(8) 0.092(8) Uiso 0.33 1 d PD . . O5 O 0.105(3) 0.037(3) -0.040(3) 0.088(17) Uiso 0.17 1 d PD . . O6 O 0.064(4) 0.114(2) -0.023(3) 0.165(15) Uiso 0.17 1 d PD . . C11 C -0.228(3) 0.348(7) 0.2500 0.185(9) Uani 0.83 2 d SP . 1 H11 H -0.1540 0.3580 0.2500 0.222 Uiso 0.83 2 calc SPR . 1 C12 C -0.244(6) 0.436(3) 0.2500 0.215(11) Uani 0.83 2 d SP A 1 H12 H -0.1804 0.5104 0.2500 0.258 Uiso 0.83 2 calc SPR A 1 N3 N -0.228(3) 0.348(7) 0.2500 0.185(9) Uani 0.17 2 d SP . 2 N4 N -0.244(6) 0.436(3) 0.2500 0.215(11) Uani 0.17 2 d SP B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0471(7) 0.0477(7) 0.0490(6) 0.000 0.000 0.0234(6) N1 0.048(4) 0.059(4) 0.057(4) 0.000 0.000 0.030(3) O1 0.037(3) 0.037(3) 0.049(5) 0.000 0.000 0.0187(14) O2 0.050(2) 0.057(2) 0.060(2) -0.0129(18) 0.0046(18) 0.0223(19) O3 0.053(2) 0.058(2) 0.075(3) -0.017(2) -0.003(2) 0.028(2) C1 0.060(4) 0.052(3) 0.043(3) 0.003(3) -0.005(3) 0.029(3) C2 0.057(3) 0.048(3) 0.050(3) -0.005(3) 0.001(3) 0.028(3) C3 0.053(4) 0.070(4) 0.085(4) -0.015(3) 0.003(3) 0.028(3) C4 0.061(4) 0.085(4) 0.106(5) -0.018(4) 0.014(4) 0.042(4) C5 0.086(5) 0.071(4) 0.095(5) -0.023(4) -0.004(4) 0.047(4) C6 0.062(4) 0.064(4) 0.081(4) -0.019(3) -0.006(4) 0.032(3) C7 0.058(4) 0.056(3) 0.063(3) -0.002(3) 0.006(3) 0.031(3) C8 0.060(4) 0.062(4) 0.064(4) -0.008(3) -0.007(3) 0.026(3) C9 0.076(4) 0.064(4) 0.094(5) -0.024(4) -0.014(4) 0.017(4) C10 0.092(7) 0.046(6) 0.118(9) 0.000 0.000 0.009(6) Cl1 0.0738(17) 0.0738(17) 0.164(5) 0.000 0.000 0.0369(8) C11 0.15(3) 0.27(3) 0.153(15) 0.000 0.000 0.11(3) C12 0.26(5) 0.20(3) 0.187(18) 0.000 0.000 0.12(3) N3 0.15(3) 0.27(3) 0.153(15) 0.000 0.000 0.11(3) N4 0.26(5) 0.20(3) 0.187(18) 0.000 0.000 0.12(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 Fe1 O1 1.9149(10) . ? Fe1 O2 2.014(3) 10_556 ? Fe1 O2 2.014(3) . ? Fe1 O3 2.015(3) 3_565 ? Fe1 O3 2.015(3) 12_566 ? Fe1 N1 2.206(6) . ? N1 C8 1.338(5) . ? N1 C8 1.338(5) 10_556 ? O1 Fe1 1.9149(10) 3_565 ? O1 Fe1 1.9149(10) 2_665 ? O2 C1 1.267(5) . ? O3 C1 1.269(5) . ? O3 Fe1 2.015(3) 2_665 ? C1 C2 1.489(6) . ? C2 C7 1.388(6) . ? C2 C3 1.393(7) . ? C3 C4 1.387(7) . ? C4 C5 1.377(7) . ? C5 C6 1.367(8) . ? C6 C7 1.381(6) . ? C8 C9 1.395(8) . ? C9 C10 1.367(7) . ? C10 C9 1.367(7) 10_556 ? Cl1 O6 1.408(17) 8 ? Cl1 O6 1.408(17) 2 ? Cl1 O6 1.408(17) . ? Cl1 O6 1.408(17) 9 ? Cl1 O6 1.408(17) 3 ? Cl1 O6 1.408(17) 7 ? Cl1 O5 1.467(16) 3 ? Cl1 O5 1.467(16) 9 ? Cl1 O5 1.467(16) 2 ? Cl1 O5 1.467(16) . ? Cl1 O5 1.467(16) 8 ? Cl1 O5 1.467(16) 7 ? O4 O6 1.20(5) . ? O4 O6 1.48(6) 8 ? O4 O6 1.54(6) 3 ? O5 O6 1.20(4) 8 ? O5 O6 1.23(5) 3 ? O5 O6 1.45(6) . ? O6 O5 1.20(4) 9 ? O6 O5 1.23(5) 2 ? O6 O4 1.48(6) 9 ? O6 O4 1.54(6) 2 ? O6 O6 1.59(5) 8 ? O6 O6 1.59(5) 9 ? C11 C12 1.323(19) . ? C11 C12 1.33(3) 3_455 ? C12 C11 1.33(2) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 95.39(10) . 10_556 ? O1 Fe1 O2 95.39(10) . . ? O2 Fe1 O2 90.2(2) 10_556 . ? O1 Fe1 O3 95.73(10) . 3_565 ? O2 Fe1 O3 168.87(14) 10_556 3_565 ? O2 Fe1 O3 89.36(14) . 3_565 ? O1 Fe1 O3 95.73(10) . 12_566 ? O2 Fe1 O3 89.36(14) 10_556 12_566 ? O2 Fe1 O3 168.87(14) . 12_566 ? O3 Fe1 O3 89.0(2) 3_565 12_566 ? O1 Fe1 N1 179.80(15) . . ? O2 Fe1 N1 84.48(14) 10_556 . ? O2 Fe1 N1 84.48(14) . . ? O3 Fe1 N1 84.41(14) 3_565 . ? O3 Fe1 N1 84.41(14) 12_566 . ? C8 N1 C8 118.6(7) . 10_556 ? C8 N1 Fe1 120.7(3) . . ? C8 N1 Fe1 120.7(3) 10_556 . ? Fe1 O1 Fe1 120.0 3_565 . ? Fe1 O1 Fe1 120.0 3_565 2_665 ? Fe1 O1 Fe1 120.0 . 2_665 ? C1 O2 Fe1 133.3(3) . . ? C1 O3 Fe1 133.1(3) . 2_665 ? O2 C1 O3 123.9(5) . . ? O2 C1 C2 118.5(5) . . ? O3 C1 C2 117.6(5) . . ? C7 C2 C3 118.7(5) . . ? C7 C2 C1 120.7(5) . . ? C3 C2 C1 120.6(5) . . ? C4 C3 C2 120.0(5) . . ? C5 C4 C3 119.7(6) . . ? C6 C5 C4 121.2(6) . . ? C5 C6 C7 119.2(5) . . ? C6 C7 C2 121.1(5) . . ? N1 C8 C9 121.8(6) . . ? C10 C9 C8 119.4(7) . . ? C9 C10 C9 119.0(9) 10_556 . ? O6 Cl1 O6 180(4) 8 2 ? O6 Cl1 O6 69(2) 8 . ? O6 Cl1 O6 111(2) 2 . ? O6 Cl1 O6 111(2) 8 9 ? O6 Cl1 O6 69(2) 2 9 ? O6 Cl1 O6 69(2) . 9 ? O6 Cl1 O6 69(2) 8 3 ? O6 Cl1 O6 111(2) 2 3 ? O6 Cl1 O6 111(2) . 3 ? O6 Cl1 O6 180(4) 9 3 ? O6 Cl1 O6 111(2) 8 7 ? O6 Cl1 O6 69(2) 2 7 ? O6 Cl1 O6 180(4) . 7 ? O6 Cl1 O6 111(2) 9 7 ? O6 Cl1 O6 69(2) 3 7 ? O6 Cl1 O5 129(2) 8 3 ? O6 Cl1 O5 51(2) 2 3 ? O6 Cl1 O5 130.6(17) . 3 ? O6 Cl1 O5 120(3) 9 3 ? O6 Cl1 O5 60(3) 3 3 ? O6 Cl1 O5 49.4(17) 7 3 ? O6 Cl1 O5 51(2) 8 9 ? O6 Cl1 O5 129(2) 2 9 ? O6 Cl1 O5 49.4(17) . 9 ? O6 Cl1 O5 60(3) 9 9 ? O6 Cl1 O5 120(3) 3 9 ? O6 Cl1 O5 130.6(17) 7 9 ? O5 Cl1 O5 180(2) 3 9 ? O6 Cl1 O5 120(3) 8 2 ? O6 Cl1 O5 60(3) 2 2 ? O6 Cl1 O5 51(2) . 2 ? O6 Cl1 O5 49.4(17) 9 2 ? O6 Cl1 O5 130.6(17) 3 2 ? O6 Cl1 O5 129(2) 7 2 ? O5 Cl1 O5 96(3) 3 2 ? O5 Cl1 O5 84(3) 9 2 ? O6 Cl1 O5 49.4(17) 8 . ? O6 Cl1 O5 130.6(17) 2 . ? O6 Cl1 O5 60(3) . . ? O6 Cl1 O5 129(2) 9 . ? O6 Cl1 O5 51(2) 3 . ? O6 Cl1 O5 120(3) 7 . ? O5 Cl1 O5 96(3) 3 . ? O5 Cl1 O5 84(3) 9 . ? O5 Cl1 O5 96(3) 2 . ? O6 Cl1 O5 60(3) 8 8 ? O6 Cl1 O5 120(3) 2 8 ? O6 Cl1 O5 129(2) . 8 ? O6 Cl1 O5 130.6(17) 9 8 ? O6 Cl1 O5 49.4(17) 3 8 ? O6 Cl1 O5 51(2) 7 8 ? O5 Cl1 O5 84(3) 3 8 ? O5 Cl1 O5 96(3) 9 8 ? O5 Cl1 O5 180(2) 2 8 ? O5 Cl1 O5 84(3) . 8 ? O6 Cl1 O5 130.6(17) 8 7 ? O6 Cl1 O5 49.4(17) 2 7 ? O6 Cl1 O5 120(3) . 7 ? O6 Cl1 O5 51(2) 9 7 ? O6 Cl1 O5 129(2) 3 7 ? O6 Cl1 O5 60(3) 7 7 ? O5 Cl1 O5 84(3) 3 7 ? O5 Cl1 O5 96(3) 9 7 ? O5 Cl1 O5 84(3) 2 7 ? O5 Cl1 O5 180(2) . 7 ? O5 Cl1 O5 96(3) 8 7 ? O6 O4 O6 72.3(18) . 8 ? O6 O4 Cl1 61.5(12) . . ? O6 O4 Cl1 56.4(14) 8 . ? O6 O4 O6 115(3) . 3 ? O6 O4 O6 64(2) 8 3 ? Cl1 O4 O6 55.1(13) . 3 ? O6 O5 O6 82(4) 8 3 ? O6 O5 O6 73(4) 8 . ? O6 O5 O6 119.9(19) 3 . ? O6 O5 Cl1 62.7(12) 8 . ? O6 O5 Cl1 62.2(13) 3 . ? O6 O5 Cl1 57.8(15) . . ? O4 O6 O5 111(3) . 9 ? O4 O6 O5 102(5) . 2 ? O5 O6 O5 108(5) 9 2 ? O4 O6 Cl1 69.9(16) . . ? O5 O6 Cl1 67.8(14) 9 . ? O5 O6 Cl1 67.2(16) 2 . ? O4 O6 O5 16(2) . . ? O5 O6 O5 96(3) 9 . ? O5 O6 O5 108(6) 2 . ? Cl1 O6 O5 61.8(16) . . ? O4 O6 O4 119(3) . 9 ? O5 O6 O4 15(2) 9 9 ? O5 O6 O4 94(4) 2 9 ? Cl1 O6 O4 62.8(16) . 9 ? O5 O6 O4 104(4) . 9 ? O4 O6 O4 89(3) . 2 ? O5 O6 O4 113(3) 9 2 ? O5 O6 O4 13(3) 2 2 ? Cl1 O6 O4 61.2(16) . 2 ? O5 O6 O4 95(4) . 2 ? O4 O6 O4 100(2) 9 2 ? O4 O6 O6 62(2) . 8 ? O5 O6 O6 50(3) 9 8 ? O5 O6 O6 123(2) 2 8 ? Cl1 O6 O6 55.5(12) . 8 ? O5 O6 O6 46.3(15) . 8 ? O4 O6 O6 60(4) 9 8 ? O4 O6 O6 115.9(13) 2 8 ? O4 O6 O6 124.1(15) . 9 ? O5 O6 O6 60(5) 9 9 ? O5 O6 O6 48.3(18) 2 9 ? Cl1 O6 O6 55.5(12) . 9 ? O5 O6 O6 117.3(14) . 9 ? O4 O6 O6 46(3) 9 9 ? O4 O6 O6 56(2) 2 9 ? O6 O6 O6 93(5) 8 9 ? C12 C11 C12 118(4) . 3_455 ? C11 C12 C11 122(4) . 2_565 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.16 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.346 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.061