Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (c) The Royal Society of Chemistry 2004 data_global _publ_contact_author_email millange@chimie.uvsq.fr _publ_contact_author_name 'Dr Franck Millange' _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_address ; Institut Lavoisier Universite de Versailles 45 Avenue des Etats-Unis Versailles 78035 FRANCE ; _publ_contact_author_phone '(33) 1 39 25 43 61' _publ_contact_author_fax '(33) 1 39 25 43 58' _publ_section_references ; Sheldrick, G.M. (1993). SHELXL-93. Program for crystal structure determination. Univ. of Gottingen, Federal Republic of Germany. Sheldrick, G.M. (1997). SHELXS-86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. ; loop_ _publ_author_name _publ_author_address F.Millange ; Institut Lavoisier, IREM, UMR CNRS C 8637 Universite de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; C.Serre ; Institut Lavoisier, IREM, UMR CNRS C 8637 Universite de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; J.Marrot ; Institut Lavoisier, IREM, UMR CNRS C 8637 Universite de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; N.Gardant ; Laboratoire des Materiaux Inorganiques UMR CNRS 7574 1 place Aristide Briand 92195 Meudon cedex France ; F.Pelle ; Laboratoire des Materiaux Inorganiques UMR CNRS 7574 1 place Aristide Briand 92195 Meudon cedex France ; G.Ferey ; Institut Lavoisier, IREM, UMR CNRS C 8637 Universite de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; data_MIL83 _database_code_depnum_ccdc_archive 'CCDC 223880' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H42 Eu2 O12' _chemical_formula_weight 970.62 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)cm 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' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 16.46600(10) _cell_length_b 16.46600(10) _cell_length_c 7.73750(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1816.80(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4416 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 3.482 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2749 _exptl_absorpt_correction_T_max 0.8733 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; Blessing, Acta Cryst. (1995) A51, 33-38 ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12056 _diffrn_reflns_av_R_equivalents 0.0948 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 29.76 _reflns_number_total 1676 _reflns_number_gt 1239 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1160P)^2^+23.9998P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(2) _refine_ls_number_reflns 1676 _refine_ls_number_parameters 72 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2153 _refine_ls_wR_factor_gt 0.1919 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 Eu1 Eu -0.3333 1.3333 0.3688(2) 0.01834(2) Uani 1 3 d S . . O1 O -0.30479(7) 1.25164(7) 0.6339(3) 0.0527(4) Uani 1 1 d DU . . O2 O -0.36223(19) 1.17591(12) 0.8333(2) 0.0956(8) Uani 1 1 d U . . C1 C -0.33656(12) 1.17341(11) 0.6861(3) 0.0488(5) Uani 1 1 d DU . . C2 C -0.33568(9) 1.08777(10) 0.6151(2) 0.0439(3) Uani 1 1 d DU . . C3 C -0.24538(19) 1.0000 0.6515(3) 0.0863(5) Uani 1 2 d SDU . . H3 H -0.1918 1.0000 0.7067 0.104 Uiso 1 2 calc SR . . C4 C -0.42673(13) 1.0000 0.6214(5) 0.0924(9) Uani 1 2 d SDU . . H4A H -0.4646 1.0000 0.5253 0.111 Uiso 1 2 calc SR . . H4B H -0.4586 1.0000 0.7269 0.111 Uiso 1 2 calc SR . . C5 C -0.31835(18) 1.08403(15) 0.4359(2) 0.0759(6) Uani 1 1 d DU . . H5A H -0.2570 1.1373 0.4110 0.091 Uiso 1 1 calc R . . H5B H -0.3637 1.0938 0.3729 0.091 Uiso 1 1 calc R . . C6 C -0.32060(14) 1.0000 0.3608(5) 0.0863(5) Uani 1 2 d SDU . . H6 H -0.3151 1.0000 0.2347 0.104 Uiso 1 2 calc SR . . C7 C -0.25388(10) 1.08867(11) 0.6989(3) 0.0439(3) Uani 1 1 d DU . . H7A H -0.2596 1.0912 0.8233 0.053 Uiso 1 1 calc R . . H7B H -0.1969 1.1448 0.6637 0.053 Uiso 1 1 calc R . . C8 C -0.24137(15) 1.0000 0.4615(3) 0.0957(7) Uani 1 2 d SDU . . H8A H -0.2379 0.9453 0.4262 0.115 Uiso 0.50 1 calc PR . . H8B H -0.1832 1.0547 0.4262 0.115 Uiso 0.50 1 calc PR . . 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 Eu1 0.01663(2) 0.01663(2) 0.02178(4) 0.000 0.000 0.00831(1) O1 0.0366(4) 0.0256(3) 0.1016(10) 0.0118(7) 0.0025(8) 0.0198(2) O2 0.1530(15) 0.0385(7) 0.0507(8) -0.0167(6) 0.0158(8) 0.0142(8) C1 0.0316(6) 0.0270(5) 0.0769(10) -0.0076(6) 0.0041(7) 0.0065(4) C2 0.0272(4) 0.0221(3) 0.0710(6) 0.0091(5) -0.0016(5) 0.0038(2) C3 0.0466(6) 0.0262(8) 0.1793(11) 0.000 0.0506(8) 0.0131(4) C4 0.0166(6) 0.0178(8) 0.243(3) 0.000 -0.0073(14) 0.0089(4) C5 0.1160(10) 0.0559(7) 0.0655(8) -0.0167(7) -0.0175(8) 0.0503(5) C6 0.0466(6) 0.0262(8) 0.1793(11) 0.000 0.0506(8) 0.0131(4) C7 0.0272(4) 0.0221(3) 0.0710(6) 0.0091(5) -0.0016(5) 0.0038(2) C8 0.0545(8) 0.070(2) 0.1678(12) 0.000 0.0604(9) 0.0349(11) _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 Eu1 O2 2.406(2) 7_664 ? Eu1 O2 2.406(2) 8_354 ? Eu1 O2 2.406(2) 9_584 ? Eu1 O1 2.443(2) 7_664 ? Eu1 O1 2.443(2) 8_354 ? Eu1 O1 2.443(2) 9_584 ? Eu1 O1 2.621(2) . ? Eu1 O1 2.621(2) 2_685 ? Eu1 O1 2.621(2) 3_365 ? Eu1 C1 2.966(2) 7_664 ? Eu1 C1 2.966(2) 8_354 ? Eu1 C1 2.966(2) 9_584 ? O1 C1 1.193(2) . ? O1 Eu1 2.443(2) 7_665 ? O2 C1 1.223(3) . ? O2 Eu1 2.406(2) 7_665 ? C1 C2 1.520(3) . ? C1 Eu1 2.966(2) 7_665 ? C2 C5 1.423(3) . ? C2 C4 1.4738(16) . ? C2 C7 1.488(3) . ? C3 C8 1.471(3) . ? C3 C7 1.578(3) 11_675 ? C3 C7 1.578(3) . ? C3 H3 0.9800 . ? C4 C2 1.4738(16) 11_675 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.484(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C5 1.484(3) 11_675 ? C6 C8 1.520(4) . ? C6 H6 0.9800 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? 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 Eu1 O2 118.71(2) 7_664 8_354 ? O2 Eu1 O2 118.71(2) 7_664 9_584 ? O2 Eu1 O2 118.72(2) 8_354 9_584 ? O2 Eu1 O1 46.41(6) 7_664 7_664 ? O2 Eu1 O1 88.86(7) 8_354 7_664 ? O2 Eu1 O1 117.03(8) 9_584 7_664 ? O2 Eu1 O1 117.03(8) 7_664 8_354 ? O2 Eu1 O1 46.41(6) 8_354 8_354 ? O2 Eu1 O1 88.86(7) 9_584 8_354 ? O1 Eu1 O1 70.69(8) 7_664 8_354 ? O2 Eu1 O1 88.86(7) 7_664 9_584 ? O2 Eu1 O1 117.03(8) 8_354 9_584 ? O2 Eu1 O1 46.41(6) 9_584 9_584 ? O1 Eu1 O1 70.69(8) 7_664 9_584 ? O1 Eu1 O1 70.69(8) 8_354 9_584 ? O2 Eu1 O1 74.86(6) 7_664 . ? O2 Eu1 O1 79.82(6) 8_354 . ? O2 Eu1 O1 134.90(8) 9_584 . ? O1 Eu1 O1 103.08(5) 7_664 . ? O1 Eu1 O1 125.05(4) 8_354 . ? O1 Eu1 O1 161.17(5) 9_584 . ? O2 Eu1 O1 79.82(6) 7_664 2_685 ? O2 Eu1 O1 134.90(8) 8_354 2_685 ? O2 Eu1 O1 74.86(6) 9_584 2_685 ? O1 Eu1 O1 125.05(4) 7_664 2_685 ? O1 Eu1 O1 161.17(5) 8_354 2_685 ? O1 Eu1 O1 103.08(5) 9_584 2_685 ? O1 Eu1 O1 65.25(7) . 2_685 ? O2 Eu1 O1 134.90(8) 7_664 3_365 ? O2 Eu1 O1 74.86(6) 8_354 3_365 ? O2 Eu1 O1 79.82(6) 9_584 3_365 ? O1 Eu1 O1 161.17(5) 7_664 3_365 ? O1 Eu1 O1 103.08(5) 8_354 3_365 ? O1 Eu1 O1 125.05(4) 9_584 3_365 ? O1 Eu1 O1 65.25(7) . 3_365 ? O1 Eu1 O1 65.25(7) 2_685 3_365 ? O2 Eu1 C1 23.48(6) 7_664 7_664 ? O2 Eu1 C1 105.06(8) 8_354 7_664 ? O2 Eu1 C1 119.62(8) 9_584 7_664 ? O1 Eu1 C1 22.97(5) 7_664 7_664 ? O1 Eu1 C1 93.66(7) 8_354 7_664 ? O1 Eu1 C1 78.04(6) 9_584 7_664 ? O1 Eu1 C1 89.81(6) . 7_664 ? O1 Eu1 C1 102.53(4) 2_685 7_664 ? O1 Eu1 C1 154.87(7) 3_365 7_664 ? O2 Eu1 C1 119.62(8) 7_664 8_354 ? O2 Eu1 C1 23.48(6) 8_354 8_354 ? O2 Eu1 C1 105.06(8) 9_584 8_354 ? O1 Eu1 C1 78.04(6) 7_664 8_354 ? O1 Eu1 C1 22.97(5) 8_354 8_354 ? O1 Eu1 C1 93.66(7) 9_584 8_354 ? O1 Eu1 C1 102.53(4) . 8_354 ? O1 Eu1 C1 154.87(7) 2_685 8_354 ? O1 Eu1 C1 89.81(6) 3_365 8_354 ? C1 Eu1 C1 99.16(6) 7_664 8_354 ? O2 Eu1 C1 105.06(8) 7_664 9_584 ? O2 Eu1 C1 119.62(8) 8_354 9_584 ? O2 Eu1 C1 23.48(6) 9_584 9_584 ? O1 Eu1 C1 93.66(7) 7_664 9_584 ? O1 Eu1 C1 78.04(6) 8_354 9_584 ? O1 Eu1 C1 22.97(5) 9_584 9_584 ? O1 Eu1 C1 154.87(7) . 9_584 ? O1 Eu1 C1 89.81(6) 2_685 9_584 ? O1 Eu1 C1 102.53(4) 3_365 9_584 ? C1 Eu1 C1 99.16(6) 7_664 9_584 ? C1 Eu1 C1 99.16(6) 8_354 9_584 ? C1 O1 Eu1 103.96(16) . 7_665 ? C1 O1 Eu1 136.49(15) . . ? Eu1 O1 Eu1 99.58(5) 7_665 . ? C1 O2 Eu1 104.90(14) . 7_665 ? O1 C1 O2 104.6(2) . . ? O1 C1 C2 132.6(2) . . ? O2 C1 C2 122.13(18) . . ? O1 C1 Eu1 53.06(13) . 7_665 ? O2 C1 Eu1 51.62(12) . 7_665 ? C2 C1 Eu1 172.61(15) . 7_665 ? C5 C2 C4 96.76(18) . . ? C5 C2 C7 102.99(18) . . ? C4 C2 C7 117.85(16) . . ? C5 C2 C1 119.18(18) . . ? C4 C2 C1 114.88(15) . . ? C7 C2 C1 105.16(14) . . ? C8 C3 C7 104.89(15) . 11_675 ? C8 C3 C7 104.89(15) . . ? C7 C3 C7 106.5(2) 11_675 . ? C8 C3 H3 113.3 . . ? C7 C3 H3 113.3 11_675 . ? C7 C3 H3 113.3 . . ? C2 C4 C2 116.3(2) . 11_675 ? C2 C4 H4A 108.2 . . ? C2 C4 H4A 108.2 11_675 . ? C2 C4 H4B 108.2 . . ? C2 C4 H4B 108.2 11_675 . ? H4A C4 H4B 107.4 . . ? C2 C5 C6 120.7(2) . . ? C2 C5 H5A 107.2 . . ? C6 C5 H5A 107.2 . . ? C2 C5 H5B 107.2 . . ? C6 C5 H5B 107.2 . . ? H5A C5 H5B 106.8 . . ? C5 C6 C5 107.7(3) 11_675 . ? C5 C6 C8 100.3(2) 11_675 . ? C5 C6 C8 100.3(2) . . ? C5 C6 H6 115.5 11_675 . ? C5 C6 H6 115.5 . . ? C8 C6 H6 115.5 . . ? C2 C7 C3 112.83(16) . . ? C2 C7 H7A 109.0 . . ? C3 C7 H7A 109.0 . . ? C2 C7 H7B 109.0 . . ? C3 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C3 C8 C6 118.3(2) . . ? C3 C8 H8A 107.7 . . ? C6 C8 H8A 107.7 . . ? C3 C8 H8B 107.7 . . ? C6 C8 H8B 107.7 . . ? H8A C8 H8B 107.1 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 29.76 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 3.740 _refine_diff_density_min -1.402 _refine_diff_density_rms 0.318 #===END