# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Christian Serre' _publ_contact_author_address ; Institut Lavoisier Universite de Versailles Saint Quentin en Yvelines 45 Avenue des Etats-Unis 78035 Versailles Cedex FRANCE ; _publ_contact_author_email serre@chimie.uvsq.fr _publ_section_title ; Synthesis and catalytic properties of MIL-100(Fe), an iron(III) carboxylate with large pores ; loop_ _publ_author_name 'Patricia Horcajada' 'Suzy Surble' 'Christian Serre' 'Do-Young Hong.' 'You-Kyong Seo.' ; Jong-San Chang ; 'Jean-Marc Greneche' 'Irene Margiolaki' 'Gerard Ferey' # Attachment 'MIL100(Fe)_revised.cif' data_MIL100(Fe) _database_code_depnum_ccdc_archive 'CCDC 640536' #============================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common MIL100(Fe) _chemical_formula_moiety Fe3OF(H2O)2[C6H3(CO2)3]2.12.5H2O _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum ? _chemical_formula_weight 878 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source fe 11.76950 4.76110 7.35730 0.30720 3.52220 15.35350 2.30450 76.88050 1.03690 26.37000 1.14000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 8.01000 0.07940 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 6.00000 0.02120 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'F D -3 M' _symmetry_space_group_name_Hall '-F 4vw 2vw 3' _cell_length_a 73.34019 _cell_length_b 73.34019 _cell_length_c 73.34019 _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 394480.96900 _cell_formula_units_Z ? _cell_measurement_temperature 80K _cell_special_details ; ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting 'Borosilicate Capillaries' _pd_spec_mount_mode Transmission _pd_spec_shape Cylinder _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate 360 _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location 'ID31- ESRF' _pd_calibration_special_details Si _diffrn_ambient_temperature 80K _diffrn_source 'synchrotron source from undulator device' _diffrn_radiation_type X-ray _diffrn_radiation_wavelength 0.80098(5) _diffrn_source_target ? _diffrn_radiation_monochromator 'DOUBLE SI(111)' _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector_type SCINTILLATOR # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 19017 _pd_meas_2theta_range_min 0.91500 _pd_meas_2theta_range_max 57.96300 _pd_meas_2theta_range_inc 0.003000 #============================================================================= # 8. REFINEMENT DATA _refine_special_details ; ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ; # The next three items are given as text. _pd_proc_ls_profile_function 'pearson VII' _pd_proc_ls_background_function experimental _pd_proc_ls_pref_orient_corr 'not applied' _pd_proc_ls_prof_R_factor 11.9946 _pd_proc_ls_prof_wR_factor 16.1415 _pd_proc_ls_prof_wR_expected 5.7313 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 22.6417 _pd_proc_ls_prof_cwR_factor 24.6073 _pd_proc_ls_prof_cwR_expected 8.7372 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 7.9320 _pd_proc_ls_prof_echi2 7.9951 # Items related to LS refinement _refine_ls_R_I_factor 12.9275 _refine_ls_number_reflns 16941 _refine_ls_number_parameters 229 _refine_ls_number_restraints 162 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 0.9092 _pd_proc_2theta_range_max 57.9572 _pd_proc_2theta_range_inc 0.003000 _pd_proc_wavelength 0.801682 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions none _pd_proc_info_data_reduction none # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution 'from coordinates of MIL-100(Cr)' _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol Fe1 0.16042(17) 0.08958(17) 0.0572(2) 0.00000 1.00000 Uiso Fe Fe2 0.37500 0.1552(2) 0.87500 0.00000 1.00000 Uiso Fe Fe3 0.10905(16) 0.10905(16) 0.8642(2) 0.00000 1.00000 Uiso Fe Fe4 0.06841(16) 0.18158(16) 0.9640(2) 0.00000 1.00000 Uiso Fe Fe5 0.29760(19) 0.05702(18) 0.02406(17) 0.00000 1.00000 Uiso Fe Fe6 0.07612(14) 0.25000 0.82612(14) 0.00000 1.00000 Uiso Fe Fe7 0.98657(18) 0.16078(17) 0.86708(17) 0.00000 1.00000 Uiso Fe O1 0.3300(11) 0.9200(11) 0.4200(11) 0.00000 1.00002 Uiso O O2 0.37500 0.1284(4) 0.87500 0.00000 1.00000 Uiso O O3 0.0504(3) 0.1996(3) 0.9564(12) 0.00000 1.00000 Uiso O O4 0.0945(2) 0.25000 0.8445(2) 0.00000 1.00000 Uiso O O5 0.2040(4) 0.0671(3) 0.0926(6) 0.00000 1.00000 Uiso O O6 0.8845(4) 0.9130(6) 0.8160(5) 0.00000 1.00000 Uiso O O7 0.0905(3) 0.9005(3) 0.8782(7) 0.00000 1.00000 Uiso O O8 0.1503(6) 0.8782(4) 0.8506(5) 0.00000 1.00000 Uiso O O9 0.1205(3) 0.9104(4) 0.8832(5) 0.00000 1.00000 Uiso O O10 0.1936(3) 0.9836(5) 0.0793(7) 0.00000 1.00000 Uiso O O11 0.0518(6) 0.9363(5) 0.8387(5) 0.00000 1.00000 Uiso O O12 0.2199(6) 0.9720(5) 0.0729(7) 0.00000 1.00000 Uiso O O13 0.2147(3) 0.9641(7) 0.0130(5) 0.00000 1.00000 Uiso O O14 0.0715(5) 0.9768(5) 0.7942(6) 0.00000 1.00000 Uiso O O15 0.0576(8) 0.9640(4) 0.8291(5) 0.00000 1.00000 Uiso O O16 0.1575(3) 0.9936(7) 0.8063(6) 0.00000 1.00000 Uiso O O17 0.1781(8) 0.9728(3) 0.8286(5) 0.00000 1.00000 Uiso O O18 0.1317(4) 0.0068(5) 0.8132(4) 0.00000 1.00000 Uiso O O19 0.1707(6) 0.9648(4) 0.8556(3) 0.00000 1.00000 Uiso O O20 0.1377(3) 0.9764(6) 0.8700(6) 0.00000 1.00000 Uiso O O21 0.1215(6) 0.9925(5) 0.8500(6) 0.00000 1.00000 Uiso O O22 0.1503(5) 0.0997(5) 0.0335(4) 0.00000 1.00000 Uiso O O23 0.37500 0.1823(4) 0.87500 0.00000 1.00000 Uiso O O24 0.0940(3) 0.0940(3) 0.85000 0.00000 1.00000 Uiso O O25 0.0856(3) 0.1644(3) 0.9766(5) 0.00000 1.00000 Uiso O O26 0.3010(6) 0.0665(7) 0.9993(4) 0.00000 1.00000 Uiso O O27 0.0572(3) 0.25000 0.8074(3) 0.00000 1.00000 Uiso O O28 0.9755(5) 0.1637(5) 0.8911(3) 0.00000 1.00000 Uiso O C1 0.2422(6) 0.0078(6) 0.9835(9) 0.00000 1.00000 Uiso C C2 0.2604(4) 0.0133(5) 0.9896(4) 0.00000 1.00000 Uiso C C3 0.2321(5) 0.9683(8) 0.0179(5) 0.00000 1.00000 Uiso C C4 0.3528(10) 0.8972(10) 0.3286(11) 0.00000 1.00000 Uiso C C5 0.3366(10) 0.9134(10) 0.3607(11) 0.00000 1.00000 Uiso C C6 0.3285(8) 0.9215(8) 0.3764(7) 0.00000 1.00000 Uiso C C8 0.1704(10) 0.9009(3) 0.8240(3) 0.00000 1.00000 Uiso C C9 0.1733(9) 0.9156(3) 0.8103(2) 0.00000 1.00000 Uiso C C11 0.1071(3) 0.1429(3) 0.8435(9) 0.00000 1.00000 Uiso C C7 0.0927(4) 0.1573(4) 0.8352(12) 0.00000 1.00000 Uiso C C10 0.0664(7) 0.1836(7) 0.8214(14) 0.00000 1.00000 Uiso C C12 0.1741(12) 0.9603(2) 0.8398(4) 0.00000 1.00000 Uiso C C14 0.2324(3) 0.0425(6) 0.0931(10) 0.00000 1.00000 Uiso C C15 0.2195(4) 0.0041(5) 0.0847(11) 0.00000 1.00000 Uiso C C18 0.19811(17) 0.05189(17) 0.0978(6) 0.00000 1.00000 Uiso C C13 0.2129(2) 0.0371(2) 0.0930(11) 0.00000 1.00000 Uiso C C16 0.2398(5) 0.0102(5) 0.0809(15) 0.00000 1.00000 Uiso C C17 0.2106(2) 0.9854(5) 0.0789(12) 0.00000 1.00000 Uiso C C20 0.0897(5) 0.9663(3) 0.8523(9) 0.00000 1.00000 Uiso C C22 0.1116(7) 0.9467(4) 0.8720(8) 0.00000 1.00000 Uiso C C19 0.0782(6) 0.9492(4) 0.8499(7) 0.00000 1.00000 Uiso C C23 0.0991(4) 0.9309(3) 0.8683(8) 0.00000 1.00000 Uiso C C24 0.0806(4) 0.9330(6) 0.8612(9) 0.00000 1.00000 Uiso C C21 0.1082(4) 0.9633(4) 0.8612(9) 0.00000 1.00000 Uiso C C25 0.1036(4) 0.9129(5) 0.8767(10) 0.00000 1.00000 Uiso C C26 0.1230(6) 0.9783(6) 0.8608(9) 0.00000 1.00000 Uiso C C27 0.0622(6) 0.9495(5) 0.8381(9) 0.00000 1.00000 Uiso C C28 0.0253(11) 0.2247(11) 0.8582(5) 0.00000 1.00000 Uiso C C30 0.1099(2) 0.9612(9) 0.7636(6) 0.00000 1.00000 Uiso C C29 0.1306(2) 0.9608(7) 0.7643(8) 0.00000 1.00000 Uiso C C31 0.0301(7) 0.2199(7) 0.8987(3) 0.00000 1.00000 Uiso C C32 0.0331(11) 0.2169(11) 0.9195(4) 0.00000 1.00000 Uiso C C33 0.1406(3) 0.9971(8) 0.8027(7) 0.00000 1.00000 Uiso C Ow1 0.12500 0.12500 -0.0087(14) 0.00000 1.00000 Uiso O Ow2 0.2775(8) 0.0798(10) 0.9725(8) 0.00000 1.00000 Uiso O Ow3 0.1950(16) 0.87500 0.87500 0.00000 1.00000 Uiso O Ow4 0.2388(7) 0.9692(7) 0.1154(8) 0.00000 1.00000 Uiso O Ow5 0.9751(7) 0.1927(8) 0.9133(7) 0.00000 1.00000 Uiso O Ow6 0.0578(10) 0.2815(7) 0.7815(7) 0.00000 1.00000 Uiso O Ow8 0.0518(7) 0.0888(7) 0.8535(7) 0.00000 1.00000 Uiso O Ow9 0.1947(8) 0.9755(7) 0.1332(7) 0.00000 1.00000 Uiso O Ow10 0.1081(10) 0.9277(7) 0.9277(7) 0.00000 1.00000 Uiso O Ow11 0.0754(7) 0.1049(7) 0.0287(7) 0.00000 1.00000 Uiso O Ow12 0.3081(8) 0.0789(10) 0.9419(8) 0.00000 1.00000 Uiso O Ow13 0.2250(8) 1.0250(8) 0.1706(10) 0.00000 1.00000 Uiso O Ow14 0.0268(10) 0.9438(7) 0.9440(7) 0.00000 1.00000 Uiso O Ow15 0.0668(8) 0.9603(7) 0.9068(7) 0.00000 1.00000 Uiso O Ow16 0.1016(15) 0.1484(15) 0.782(2) 0.00000 0.50000 Uiso O Ow17 0.1096(10) 1.0155(7) 0.7345(7) 0.00000 1.00000 Uiso O Ow18 0.2399(7) 1.0101(7) 0.1450(10) 0.00000 1.00000 Uiso O Ow19 0.1480(10) 1.0386(7) 0.7114(7) 0.00000 1.00000 Uiso O Ow20 0.1185(7) 0.9860(7) 0.9298(7) 0.00000 1.00000 Uiso O Ow21 0.3288(8) 0.0195(10) 0.9212(8) 0.00000 1.00000 Uiso O Ow22 0.0388(9) 0.2475(7) 0.7475(7) 0.00000 1.00000 Uiso O Ow23 0.2234(7) 0.9704(8) 0.8423(7) 0.00000 1.00000 Uiso O Ow24 0.0918(15) 0.1582(15) 0.787(2) 0.00000 0.50000 Uiso O Ow25 0.2964(8) 0.0454(12) 0.9536(8) 0.00000 1.00000 Uiso O Ow26 0.1104(4) 0.1396(4) 0.9605(9) 0.00000 1.00000 Uiso O Ow27 0.2703(8) 0.0196(7) 0.9327(7) 0.00000 1.00000 Uiso O Ow28 0.1833(10) 1.0667(10) 0.1833(10) 0.00000 1.00000 Uiso O Ow29 0.0540(7) 0.9460(7) 1.00000 0.00000 1.00000 Uiso O Ow30 0.3121(7) -0.01997 0.9379(7) 0.00000 1.00000 Uiso O # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies.