Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_mor570i _database_code_CSD 188871 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common MIL-62 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C2.50 H0.50 Fe0.50 O2' _chemical_formula_weight 90.45 _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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 6.2378(7) _cell_length_b 17.589(2) _cell_length_c 4.6039(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.863(2) _cell_angle_gamma 90.00 _cell_volume 454.54(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas 2.66(1) _exptl_crystal_density_diffrn 2.644 _exptl_crystal_density_method 'He pycnometer' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 3.237 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.61 _exptl_absorpt_correction_T_max 0.80 _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 'SMART CCD diffractometer' _diffrn_measurement_method 'scan omega' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1585 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 29.53 _reflns_number_total 612 _reflns_number_observed 560 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'DIAMOND (Version 2.1)' _computing_publication_material ? _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^)+(0.0515P)^2^+0.8172P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 612 _refine_ls_number_parameters 48 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_obs 0.0291 _refine_ls_wR_factor_all 0.0804 _refine_ls_wR_factor_obs 0.0768 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.040 _refine_ls_restrained_S_all 1.037 _refine_ls_restrained_S_obs 1.040 _refine_ls_shift/esd_max 0.000 _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 Fe1 Fe 0.0000 0.20939(2) 0.0000 0.0122(2) Uani 1 d S . O1 O 0.2377(3) 0.30146(9) 0.2076(4) 0.0138(4) Uani 1 d . . O2 O 0.2073(3) 0.13349(10) 0.3486(4) 0.0163(4) Uani 1 d . . C1 C 0.3250(6) 0.0000 0.6880(8) 0.0130(6) Uani 1 d S . H1 H 0.2076(6) 0.0000 0.4760(8) 0.016 Uiso 1 calc SR . C2 C 0.2882(4) 0.13913(12) 0.6488(5) 0.0113(4) Uani 1 d . . C3 C 0.4095(4) 0.06982(12) 0.8406(5) 0.0112(4) Uani 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 Fe1 0.0128(3) 0.0104(3) 0.0106(3) 0.000 0.0026(2) 0.000 O1 0.0163(8) 0.0099(7) 0.0145(8) -0.0012(6) 0.0060(7) 0.0008(6) O2 0.0212(9) 0.0147(8) 0.0104(8) 0.0016(6) 0.0046(7) 0.0043(7) C1 0.0145(14) 0.0125(14) 0.0088(13) 0.000 0.0020(11) 0.000 C2 0.0097(9) 0.0106(9) 0.0124(10) 0.0010(7) 0.0037(8) 0.0003(8) C3 0.0134(9) 0.0088(9) 0.0109(10) 0.0004(8) 0.0049(9) 0.0000(8) _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 O2 2.054(2) 2 ? Fe1 O2 2.054(2) . ? Fe1 O1 2.121(2) . ? Fe1 O1 2.121(2) 2 ? Fe1 O1 2.234(2) 8_455 ? Fe1 O1 2.234(2) 7 ? O1 C2 1.284(3) 7_556 ? O1 Fe1 2.234(2) 7 ? O2 C2 1.252(3) . ? C1 C3 1.399(3) 6 ? C1 C3 1.399(3) . ? C1 H1 0.93 . ? C2 O1 1.284(3) 7_556 ? C2 C3 1.502(3) . ? C3 C3 1.408(4) 2_657 ? 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 O2 Fe1 O2 98.93(10) 2 . ? O2 Fe1 O1 157.89(7) 2 . ? O2 Fe1 O1 93.79(7) . . ? O2 Fe1 O1 93.79(7) 2 2 ? O2 Fe1 O1 157.89(7) . 2 ? O1 Fe1 O1 80.43(9) . 2 ? O2 Fe1 O1 87.11(6) 2 8_455 ? O2 Fe1 O1 86.52(6) . 8_455 ? O1 Fe1 O1 111.77(6) . 8_455 ? O1 Fe1 O1 76.09(7) 2 8_455 ? O2 Fe1 O1 86.52(6) 2 7 ? O2 Fe1 O1 87.11(6) . 7 ? O1 Fe1 O1 76.09(7) . 7 ? O1 Fe1 O1 111.77(6) 2 7 ? O1 Fe1 O1 170.20(8) 8_455 7 ? C2 O1 Fe1 129.31(15) 7_556 . ? C2 O1 Fe1 124.74(14) 7_556 7 ? Fe1 O1 Fe1 103.91(7) . 7 ? C2 O2 Fe1 128.6(2) . . ? C3 C1 C3 122.8(3) 6 . ? C3 C1 H1 118.61(14) 6 . ? C3 C1 H1 118.61(14) . . ? O2 C2 O1 123.5(2) . 7_556 ? O2 C2 C3 116.2(2) . . ? O1 C2 C3 120.2(2) 7_556 . ? C1 C3 C3 118.60(14) . 2_657 ? C1 C3 C2 115.7(2) . . ? C3 C3 C2 125.59(11) 2_657 . ? _refine_diff_density_max 0.622 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.114