# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jose Mesa' _publ_contact_author_email JOSELUIS.MESA@EHU.ES _publ_section_title ; Microporous Vanadyl-Arsenate With The Template Incorporated Exhibiting Sorption and Catalytic Properties ; _publ_requested_category FM loop_ _publ_author_name 'Jose Mesa' 'Andres T Aguayo' 'Maria I. Arriortua' 'Begona Bazan' 'Teresa Berrocal' 'Marta Iglesias' ; J.L.Pizarro ; 'Teofilo Rojo' # Attachment 'File.cif' data_fjl25atci _database_code_depnum_ccdc_archive 'CCDC 681702' _audit_creation_date 2008-06-05T09:51:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C5 H23 As3 N2 O19 V3' _chemical_formula_weight 792.83 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-x, -y, -z' '-x+y, -x, -z-1/2' 'y, -x+y, -z' 'x, y, -z-1/2' 'x-y, x, -z' '-y, x-y, -z-1/2' _cell_length_a 19.0945(16) _cell_length_b 19.0945(16) _cell_length_c 11.0133(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3477.5(5) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1248 _cell_measurement_theta_max 4.443 _cell_measurement_theta_min 45.562 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 2.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2322 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.519 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _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_detector_area_resol_mean 8.26 _diffrn_reflns_av_R_equivalents 0.1566 _diffrn_reflns_av_unetI/netI 0.0973 _diffrn_reflns_number 30908 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'BRUKER SMART APEX CCD System' _diffrn_measurement_method '\w rotations with narrow frame' _diffrn_standards_decay_% 0 _reflns_number_total 2367 _reflns_number_gt 1673 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0134P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2367 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0725 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.331 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.142 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 V1 V 0.60527(6) 0.15124(5) 0.10030(8) 0.0074(2) Uani 1 1 d . . . V2 V 0.50653(8) -0.02355(8) 0.2500 0.0083(3) Uani 1 2 d S . . As1 As 0.41373(3) 0.01341(3) 0.01242(5) 0.00815(15) Uani 1 1 d . . . As2 As 0.50366(5) 0.22713(5) 0.2500 0.0085(2) Uani 1 2 d S . . O1 O 0.4939(2) 0.0447(2) 0.1105(3) 0.0088(9) Uani 1 1 d . . . O2 O 0.3587(2) -0.0866(2) 0.0020(3) 0.0106(9) Uani 1 1 d . . . O3 O 0.4435(2) 0.0589(2) -0.1240(3) 0.0091(9) Uiso 1 1 d . . . O4 O 0.3532(2) 0.0455(2) 0.0754(3) 0.0153(9) Uani 1 1 d . . . H2 H 0.3138 0.0323 0.0317 0.018 Uiso 1 1 calc R . . O5 O 0.5758(3) 0.1984(3) 0.2500 0.0089(12) Uiso 1 2 d S . . O6 O 0.4109(3) 0.1432(3) 0.2500 0.0100(13) Uani 1 2 d S . . O7 O 0.7217(2) 0.2321(2) 0.1229(3) 0.0098(9) Uiso 1 1 d . . . O8 O 0.5794(2) 0.1931(2) -0.0018(4) 0.0151(9) Uani 1 1 d . . . O9 O 0.4139(3) -0.0936(3) 0.2500 0.0183(14) Uani 1 2 d S . . O10 O 0.6154(3) 0.0877(3) 0.2500 0.0077(13) Uani 1 2 d S . . H1 H 0.649(6) 0.074(6) 0.2500 0.050 Uiso 1 2 d S . . O11A O 0.2138(8) 0.2157(9) 0.4081(12) 0.069(4) Uani 0.50 1 d P . . O11B O 0.2429(10) 0.1936(8) 0.4786(13) 0.090(5) Uani 0.50 1 d P . . O12 O 0.3264(4) 0.2345(4) 0.2500 0.0316(17) Uani 1 2 d S . . C1 C 0.7342(5) 0.2656(6) 0.8129(7) 0.064(3) Uani 1 1 d . . . H1A H 0.7621 0.3216 0.8391 0.077 Uiso 1 1 calc R . . H1B H 0.6784 0.2422 0.8391 0.077 Uiso 1 1 calc R . . C2 C 0.8053(5) 0.1866(6) 0.8192(6) 0.056(3) Uani 1 1 d . . . H2A H 0.8576 0.2369 0.8202 0.067 Uiso 1 1 calc R . . C3 C 0.8373(11) 0.1480(10) 0.8824(18) 0.071(6) Uani 0.50 1 d P . . H1C H 0.8465 0.1667 0.9649 0.107 Uiso 0.50 1 calc PR . . H1D H 0.8875 0.1593 0.8460 0.107 Uiso 0.50 1 calc PR . . H1E H 0.8002 0.0908 0.8808 0.107 Uiso 0.50 1 calc PR . . N1 N 0.7669(5) 0.2272(4) 0.8744(5) 0.062(2) Uani 1 1 d . . . H1F H 0.7271 0.1902 0.9215 0.075 Uiso 1 1 calc R . . H1G H 0.8038 0.2643 0.9252 0.075 Uiso 1 1 calc R . . 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 0.0104(5) 0.0087(5) 0.0017(5) 0.0000(4) -0.0003(4) 0.0036(4) V2 0.0114(7) 0.0081(7) 0.0036(7) 0.000 0.000 0.0037(6) As1 0.0109(3) 0.0116(3) 0.0023(3) -0.0012(3) -0.0008(3) 0.0059(3) As2 0.0138(5) 0.0098(4) 0.0027(4) 0.000 0.000 0.0065(4) O1 0.009(2) 0.012(2) 0.005(2) -0.0011(16) -0.0026(17) 0.0045(18) O2 0.009(2) 0.017(2) 0.003(2) -0.0022(18) -0.0004(17) 0.0050(17) O4 0.013(2) 0.030(3) 0.009(2) -0.0053(19) -0.0066(18) 0.016(2) O6 0.016(3) 0.012(3) 0.007(3) 0.000 0.000 0.010(3) O8 0.020(2) 0.012(2) 0.013(2) 0.0011(18) -0.0059(19) 0.0070(18) O9 0.015(3) 0.014(3) 0.019(3) 0.000 0.000 0.002(3) O10 0.010(3) 0.011(3) 0.003(3) 0.000 0.000 0.005(3) O11A 0.072(10) 0.086(11) 0.058(10) 0.004(8) 0.020(8) 0.046(8) O11B 0.107(13) 0.062(10) 0.081(12) 0.018(9) 0.044(10) 0.027(9) O12 0.031(4) 0.026(4) 0.038(4) 0.000 0.000 0.014(3) C1 0.052(5) 0.073(6) 0.084(7) -0.055(5) -0.049(5) 0.044(5) C2 0.057(6) 0.098(7) 0.033(5) 0.016(5) 0.006(4) 0.054(6) C3 0.075(14) 0.059(13) 0.093(16) -0.019(11) -0.046(12) 0.043(12) N1 0.135(7) 0.041(4) 0.023(4) 0.023(3) 0.050(4) 0.053(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O8 1.594(4) . ? V1 O7 1.990(4) . ? V1 O2 2.028(4) 7_655 ? V1 O1 2.085(4) . ? V1 O5 2.087(3) . ? V1 O10 2.112(3) . ? V2 O9 1.597(5) . ? V2 O3 1.983(4) 4_655 ? V2 O3 1.983(4) 7_655 ? V2 O10 2.102(5) . ? V2 O1 2.106(4) 10_556 ? V2 O1 2.106(4) . ? As1 O2 1.661(4) . ? As1 O3 1.686(3) . ? As1 O4 1.703(4) . ? As1 O1 1.718(3) . ? As2 O7 1.675(4) 8_666 ? As2 O7 1.675(4) 5_665 ? As2 O6 1.693(5) . ? As2 O5 1.718(5) . ? O2 V1 2.028(4) 7_655 ? O3 V2 1.983(4) 7_655 ? O4 H2 0.8200 . ? O5 V1 2.087(3) 10_556 ? O7 As2 1.675(4) 3_655 ? O10 V1 2.112(3) 10_556 ? O10 H1 0.80(9) . ? O11A O11B 1.151(16) . ? C1 N1 1.359(9) . ? C1 C1 1.385(15) 10_557 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.359(17) . ? C2 N1 1.442(9) . ? C2 C2 1.524(14) 10_557 ? C2 H2A 0.9800 . ? C3 H1C 0.9600 . ? C3 H1D 0.9600 . ? C3 H1E 0.9600 . ? N1 H1F 0.9000 . ? N1 H1G 0.9000 . ? 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 O8 V1 O7 101.84(17) . . ? O8 V1 O2 101.34(17) . 7_655 ? O7 V1 O2 87.38(14) . 7_655 ? O8 V1 O1 96.11(16) . . ? O7 V1 O1 161.74(15) . . ? O2 V1 O1 85.81(14) 7_655 . ? O8 V1 O5 97.09(18) . . ? O7 V1 O5 90.24(17) . . ? O2 V1 O5 161.52(15) 7_655 . ? O1 V1 O5 90.87(17) . . ? O8 V1 O10 168.2(2) . . ? O7 V1 O10 87.74(18) . . ? O2 V1 O10 85.88(15) 7_655 . ? O1 V1 O10 74.89(17) . . ? O5 V1 O10 75.71(15) . . ? O9 V2 O3 103.59(18) . 4_655 ? O9 V2 O3 103.59(18) . 7_655 ? O3 V2 O3 88.8(2) 4_655 7_655 ? O9 V2 O10 165.4(3) . . ? O3 V2 O10 86.74(15) 4_655 . ? O3 V2 O10 86.74(15) 7_655 . ? O9 V2 O1 95.53(17) . 10_556 ? O3 V2 O1 85.62(14) 4_655 10_556 ? O3 V2 O1 160.84(15) 7_655 10_556 ? O10 V2 O1 74.68(14) . 10_556 ? O9 V2 O1 95.53(17) . . ? O3 V2 O1 160.84(15) 4_655 . ? O3 V2 O1 85.62(14) 7_655 . ? O10 V2 O1 74.68(14) . . ? O1 V2 O1 93.8(2) 10_556 . ? O2 As1 O3 112.78(17) . . ? O2 As1 O4 106.84(18) . . ? O3 As1 O4 106.99(17) . . ? O2 As1 O1 112.62(17) . . ? O3 As1 O1 111.65(17) . . ? O4 As1 O1 105.40(17) . . ? O7 As2 O7 113.4(2) 8_666 5_665 ? O7 As2 O6 106.90(15) 8_666 . ? O7 As2 O6 106.90(15) 5_665 . ? O7 As2 O5 110.25(15) 8_666 . ? O7 As2 O5 110.25(15) 5_665 . ? O6 As2 O5 108.9(2) . . ? As1 O1 V1 127.05(19) . . ? As1 O1 V2 126.97(19) . . ? V1 O1 V2 105.44(15) . . ? As1 O2 V1 121.77(19) . 7_655 ? As1 O3 V2 122.95(19) . 7_655 ? As1 O4 H2 109.5 . . ? As2 O5 V1 124.76(13) . 10_556 ? As2 O5 V1 124.76(13) . . ? V1 O5 V1 104.4(2) 10_556 . ? As2 O7 V1 129.8(2) 3_655 . ? V2 O10 V1 104.63(17) . 10_556 ? V2 O10 V1 104.63(17) . . ? V1 O10 V1 102.6(2) 10_556 . ? V2 O10 H1 102(7) . . ? V1 O10 H1 120(3) 10_556 . ? V1 O10 H1 120(3) . . ? N1 C1 C1 119.9(4) . 10_557 ? N1 C1 H1A 107.3 . . ? C1 C1 H1A 107.3 10_557 . ? N1 C1 H1B 107.3 . . ? C1 C1 H1B 107.3 10_557 . ? H1A C1 H1B 106.9 . . ? C3 C2 N1 124.2(11) . . ? C3 C2 C2 120.8(9) . 10_557 ? N1 C2 C2 114.9(4) . 10_557 ? C3 C2 H2A 90.7 . . ? N1 C2 H2A 90.7 . . ? C2 C2 H2A 90.7 10_557 . ? C2 C3 H1C 109.5 . . ? C2 C3 H1D 109.5 . . ? H1C C3 H1D 109.5 . . ? C2 C3 H1E 109.5 . . ? H1C C3 H1E 109.5 . . ? H1D C3 H1E 109.5 . . ? C1 N1 C2 125.1(6) . . ? C1 N1 H1F 106.0 . . ? C2 N1 H1F 106.0 . . ? C1 N1 H1G 106.0 . . ? C2 N1 H1G 106.0 . . ? H1F N1 H1G 106.3 . . ?