Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Riou, Didier' 'Barthelet, K.' 'Ferey, Gerard' _publ_contact_author_name 'Prof Didier Riou' _publ_contact_author_address ; Institut Lavoisier UMR CNRS8637 Universite de Versailles St Quentin en Yvelines 45 Avenue des Etats-Unis Versailles 78035 FRANCE ; _publ_contact_author_email 'RIOU@CHIMIE.UVSQ.FR' _publ_section_title ; (VIII(H2O))3O{O2C-C6H4-CO2}3.(Cl, 9H2O) (MIL-59) : a scarce example of vanadocarboxylate with a frustrated three-dimensional hybrid framework. ; data_MIL-59 _database_code_CSD 182284 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H4 Cl0.33 O8.33 V' _chemical_formula_weight 296.20 _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' 'V' 'V' 0.3005 0.5294 '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' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 19.29070(10) _cell_length_b 19.29070(10) _cell_length_c 19.29070(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7178.67(6) _cell_formula_units_Z 24 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 47867 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cubic _exptl_crystal_colour dark green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 1.670(4) _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'pycnometry' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 0.933 _exptl_absorpt_correction_type Semi empirical (SADABS) _exptl_absorpt_correction_T_min 0.784810 _exptl_absorpt_correction_T_max 0.880739 _exptl_special_details ; ? ; _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47867 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 29.87 _reflns_number_total 3345 _reflns_number_observed 2750 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Diamnod Brandenburg' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0555P)^2^+11.2419P] 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 SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3345 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_obs 0.0513 _refine_ls_wR_factor_all 0.1331 _refine_ls_wR_factor_obs 0.1238 _refine_ls_goodness_of_fit_all 1.140 _refine_ls_goodness_of_fit_obs 1.175 _refine_ls_restrained_S_all 1.140 _refine_ls_restrained_S_obs 1.175 _refine_ls_shift/esd_max -0.001 _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 V1 V 0.75509(2) 0.39102(2) 0.14242(2) 0.01682(14) Uani 1 d . . O1 O 0.80451(10) 0.48174(9) 0.15148(10) 0.0256(4) Uani 1 d . . O2 O 0.83494(9) 0.33494(9) 0.16506(9) 0.0176(6) Uani 1 d S . O3 O 0.69107(10) 0.30864(10) 0.13710(12) 0.0310(5) Uani 1 d . . O4 O 0.72206(10) 0.39737(11) 0.24087(10) 0.0277(4) Uani 1 d . . O5 O 0.77398(11) 0.39115(10) 0.04025(9) 0.0276(4) Uani 1 d . . O6 O 0.66938(11) 0.45057(11) 0.11735(11) 0.0320(5) Uani 1 d . . C1 C 0.74479(13) 0.36925(14) 0.29530(13) 0.0225(5) Uani 1 d . . C2 C 0.85500(13) 0.50048(13) 0.18967(14) 0.0223(5) Uani 1 d . . C3 C 0.69392(13) 0.33926(15) 0.34526(13) 0.0238(5) Uani 1 d . . C4 C 0.62343(13) 0.34303(14) 0.33040(14) 0.0232(5) Uani 1 d . . H4 H 0.60811(13) 0.36856(14) 0.29249(14) 0.028 Uiso 1 calc R . C5 C 0.80861(15) 0.37225(14) -0.07596(13) 0.0245(5) Uani 1 d . . C6 C 0.7699(2) 0.4287(2) -0.09915(14) 0.0336(7) Uani 1 d . . H6 H 0.7459(2) 0.4560(2) -0.06754(14) 0.040 Uiso 1 calc R . C7 C 0.71669(14) 0.3023(2) 0.4030(2) 0.0327(7) Uani 1 d . . H7 H 0.76362(14) 0.3012(2) 0.4140(2) 0.039 Uiso 1 calc R . C8 C 0.6693(2) 0.2672(2) 0.4441(2) 0.0413(8) Uani 1 d . . H8 H 0.6845(2) 0.2418(2) 0.4822(2) 0.050 Uiso 1 calc R . Cl Cl 0.5638(2) 0.4837(3) 0.2146(2) 0.0484(9) Uani 0.33 d P . OW1 O 0.5634(7) 0.4788(8) 0.2189(8) 0.141(5) Uani 0.67 d P . OW2 O 0.8677(2) 0.5525(2) -0.0074(2) 0.0682(9) Uani 1 d . . OW3 O 0.5756(2) 0.3989(3) 0.0212(3) 0.127(2) Uani 1 d . . OW4 O 0.9419(2) 0.4419(2) 0.0581(2) 0.0598(13) Uani 1 d S . 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 V1 0.0173(2) 0.0149(2) 0.0183(2) 0.00015(14) 0.00001(15) -0.00022(14) O1 0.0277(10) 0.0184(9) 0.0308(10) 0.0002(7) -0.0056(8) -0.0036(7) O2 0.0176(6) 0.0176(6) 0.0176(6) -0.0013(6) -0.0013(6) 0.0013(6) O3 0.0236(10) 0.0184(9) 0.0511(13) 0.0011(8) -0.0014(9) -0.0025(7) O4 0.0258(9) 0.0354(11) 0.0221(9) 0.0048(8) 0.0061(7) 0.0055(8) O5 0.0359(11) 0.0289(10) 0.0181(9) -0.0005(7) 0.0007(8) 0.0067(8) O6 0.0274(10) 0.0286(10) 0.0402(12) -0.0008(9) -0.0064(9) 0.0070(8) C1 0.0211(12) 0.0267(12) 0.0196(11) -0.0029(10) 0.0038(9) 0.0013(9) C2 0.0233(12) 0.0180(11) 0.0255(12) -0.0021(9) 0.0022(10) 0.0005(9) C3 0.0189(12) 0.0314(13) 0.0210(12) 0.0018(10) 0.0022(9) 0.0013(10) C4 0.0200(12) 0.0287(13) 0.0210(12) 0.0029(10) 0.0000(9) 0.0019(10) C5 0.0320(14) 0.0243(12) 0.0172(11) 0.0007(9) -0.0032(10) 0.0025(10) C6 0.050(2) 0.0310(14) 0.0202(13) -0.0026(11) -0.0004(12) 0.0150(13) C7 0.0168(12) 0.052(2) 0.0294(14) 0.0087(13) -0.0030(10) 0.0052(12) C8 0.0238(14) 0.068(2) 0.032(2) 0.024(2) -0.0029(12) 0.0057(14) Cl 0.0298(15) 0.061(2) 0.055(2) -0.005(2) 0.0121(15) 0.0021(15) OW1 0.137(9) 0.138(11) 0.148(11) 0.021(8) -0.002(8) 0.019(8) OW2 0.079(2) 0.064(2) 0.061(2) 0.003(2) 0.000(2) -0.005(2) OW3 0.105(3) 0.158(5) 0.118(4) -0.046(3) 0.001(3) -0.089(3) OW4 0.0598(13) 0.0598(13) 0.0598(13) 0.0015(14) 0.0015(14) -0.0015(14) _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 V1 O2 1.9322(4) . ? V1 O1 2.000(2) . ? V1 O5 2.004(2) . ? V1 O4 2.007(2) . ? V1 O3 2.015(2) . ? V1 O6 2.071(2) . ? O1 C2 1.274(3) . ? O2 V1 1.9323(4) 11_556 ? O2 V1 1.9323(4) 8_645 ? O3 C1 1.265(3) 8_645 ? O4 C1 1.260(3) . ? O5 C2 1.263(3) 8_645 ? C1 O3 1.265(3) 11_556 ? C1 C3 1.492(4) . ? C2 O5 1.263(3) 11_556 ? C2 C5 1.494(4) 11_556 ? C3 C4 1.391(4) . ? C3 C7 1.394(4) . ? C4 C5 1.390(4) 18_655 ? C4 H4 0.93 . ? C5 C4 1.390(4) 24_656 ? C5 C6 1.394(4) . ? C5 C2 1.494(4) 8_645 ? C6 C8 1.386(4) 24_656 ? C6 H6 0.93 . ? C7 C8 1.387(4) . ? C7 H7 0.93 . ? C8 C6 1.386(4) 18_655 ? C8 H8 0.93 . ? 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 V1 O1 95.17(9) . . ? O2 V1 O5 94.47(8) . . ? O1 V1 O5 89.90(8) . . ? O2 V1 O4 94.21(8) . . ? O1 V1 O4 90.87(8) . . ? O5 V1 O4 171.18(8) . . ? O2 V1 O3 93.36(9) . . ? O1 V1 O3 170.52(8) . . ? O5 V1 O3 93.57(9) . . ? O4 V1 O3 84.36(9) . . ? O2 V1 O6 179.47(6) . . ? O1 V1 O6 85.16(8) . . ? O5 V1 O6 85.11(8) . . ? O4 V1 O6 86.19(8) . . ? O3 V1 O6 86.34(8) . . ? C2 O1 V1 131.6(2) . . ? V1 O2 V1 119.995(2) . 11_556 ? V1 O2 V1 119.996(2) . 8_645 ? V1 O2 V1 119.996(2) 11_556 8_645 ? C1 O3 V1 130.2(2) 8_645 . ? C1 O4 V1 130.7(2) . . ? C2 O5 V1 135.4(2) 8_645 . ? O4 C1 O3 123.6(2) . 11_556 ? O4 C1 C3 118.4(2) . . ? O3 C1 C3 117.9(2) 11_556 . ? O5 C2 O1 124.5(2) 11_556 . ? O5 C2 C5 118.1(2) 11_556 11_556 ? O1 C2 C5 117.4(2) . 11_556 ? C4 C3 C7 120.0(2) . . ? C4 C3 C1 119.3(2) . . ? C7 C3 C1 120.5(2) . . ? C5 C4 C3 120.0(2) 18_655 . ? C5 C4 H4 120.02(15) 18_655 . ? C3 C4 H4 120.0(2) . . ? C4 C5 C6 119.9(2) 24_656 . ? C4 C5 C2 120.1(2) 24_656 8_645 ? C6 C5 C2 119.9(2) . 8_645 ? C8 C6 C5 120.1(3) 24_656 . ? C8 C6 H6 120.0(2) 24_656 . ? C5 C6 H6 120.0(2) . . ? C8 C7 C3 119.9(3) . . ? C8 C7 H7 120.0(2) . . ? C3 C7 H7 120.0(2) . . ? C6 C8 C7 120.2(3) 18_655 . ? C6 C8 H8 119.9(2) 18_655 . ? C7 C8 H8 119.9(2) . . ? _refine_diff_density_max 0.817 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.086