# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Maria Arriortua' _publ_contact_author_email MARIBEL.ARRIORTUA@EHU.ES _publ_section_title ; Catalytic Performance of the High and Low Temperature Polimorphs of (C6N2H16)0.5[(VO)(HAsO4)F]: Structural, Thermal, Spectroscopic and Magnetic Studies ; _publ_requested_category FM loop_ _publ_author_name 'Maria Arriortua' 'Begona Bazan' 'Teresa Berrocal' 'M. Iglesias' 'Jose Mesa' 'Jose L Pizarro' ; T.Rojo ; 'J.L. Vilas' # Attachment 'DchVAs_HT.cif' data_vasfdch _database_code_depnum_ccdc_archive 'CCDC 711728' _audit_creation_date 2008-04-15T12:42:27-00:00 _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_formula_sum 'C3 H9 As F N O5 V ' _chemical_formula_weight 283.97 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.0251(18) _cell_length_b 7.3224(6) _cell_length_c 10.3442(7) _cell_angle_alpha 90 _cell_angle_beta 109.250(6) _cell_angle_gamma 90 _cell_volume 1646.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2368 _cell_measurement_theta_min 2.7734 _cell_measurement_theta_max 32.3707 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_absorpt_correction_T_min 0.81216 _exptl_absorpt_correction_T_max 1.00000 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_orient_matrix_UB_11 0.0239118026 _diffrn_orient_matrix_UB_12 -0.0734657354 _diffrn_orient_matrix_UB_13 -0.0164836686 _diffrn_orient_matrix_UB_21 -0.0464351653 _diffrn_orient_matrix_UB_22 0.0206314408 _diffrn_orient_matrix_UB_23 -0.0257870886 _diffrn_orient_matrix_UB_31 0.0453494841 _diffrn_orient_matrix_UB_32 0.0597791039 _diffrn_orient_matrix_UB_33 -0.0114353072 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_unetI/netI 0.1144 _diffrn_reflns_number 7607 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 32.46 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.913 _reflns_number_total 2710 _reflns_number_gt 1474 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _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^)+(0.0415P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 2710 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.859 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.779 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.169 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 As As 0.195843(16) 0.18776(6) 0.21986(4) 0.01274(11) Uani 1 1 d . . . V V 0.18415(3) 0.18390(10) 0.52009(6) 0.01235(14) Uani 1 1 d . . . F F 0.28081(9) 0.1037(3) 0.5410(2) 0.0176(5) Uani 1 1 d . . . O1 O 0.16564(11) 0.0912(4) 0.3283(2) 0.0175(6) Uani 1 1 d . . . O2 O 0.15935(12) 0.3927(4) 0.1646(3) 0.0208(6) Uani 1 1 d . . . H2 H 0.1733 0.4391 0.1089 0.031 Uiso 1 1 calc R . . O3 O 0.17873(12) 0.0714(4) 0.0744(3) 0.0180(6) Uani 1 1 d . . . O4 O 0.27169(11) 0.2252(4) 0.2851(3) 0.0185(6) Uani 1 1 d . . . O5 O 0.11831(12) 0.2580(4) 0.5157(3) 0.0252(7) Uani 1 1 d . . . N1 N 0.13165(14) 0.3021(5) -0.1583(4) 0.0244(8) Uani 1 1 d . . . H1A H 0.137 0.2823 -0.2386 0.037 Uiso 1 1 calc R . . H1B H 0.1501 0.2141 -0.0999 0.037 Uiso 1 1 calc R . . H1C H 0.1479 0.4096 -0.1252 0.037 Uiso 1 1 calc R . . C1 C 0.06462(19) 0.3025(7) -0.1773(6) 0.0417(13) Uani 1 1 d . . . H1 H 0.0612 0.305 -0.0853 0.063 Uiso 1 1 calc R . . C2 C 0.0344(2) 0.1341(8) -0.2422(8) 0.073(3) Uani 1 1 d . . . H2A H 0.0543 0.0302 -0.1871 0.109 Uiso 1 1 calc R . . H2B H 0.039 0.1218 -0.3317 0.109 Uiso 1 1 calc R . . C3 C 0.0343(2) 0.4709(8) -0.2472(7) 0.062(2) Uani 1 1 d . . . H3A H 0.0364 0.4754 -0.3393 0.092 Uiso 1 1 calc R . . H3B H 0.0552 0.5775 -0.1978 0.092 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 As 0.01633(19) 0.0112(2) 0.00983(18) -0.00031(18) 0.00317(13) 0.00097(18) V 0.0150(3) 0.0110(3) 0.0109(3) -0.0007(3) 0.0039(2) -0.0001(3) F 0.0215(12) 0.0151(13) 0.0160(11) 0.0033(9) 0.0058(9) 0.0005(10) O1 0.0178(13) 0.0273(17) 0.0058(12) -0.0023(12) 0.0017(10) -0.0062(13) O2 0.0286(16) 0.0134(15) 0.0184(15) 0.0050(12) 0.0050(12) 0.0049(12) O3 0.0272(15) 0.0154(15) 0.0098(13) -0.0030(12) 0.0039(11) 0.0048(13) O4 0.0160(13) 0.0264(18) 0.0125(13) -0.0024(12) 0.0038(10) -0.0020(12) O5 0.0214(15) 0.0288(18) 0.0252(17) -0.0033(13) 0.0072(13) 0.0066(12) N1 0.0195(16) 0.023(2) 0.0302(19) 0.0065(18) 0.0073(14) 0.0007(17) C1 0.018(2) 0.034(3) 0.065(4) 0.013(3) 0.003(2) -0.001(2) C2 0.022(3) 0.027(3) 0.154(8) -0.014(4) 0.008(4) -0.001(2) C3 0.022(3) 0.039(4) 0.102(5) 0.005(3) -0.009(3) -0.004(2) #----------------------------------------------------------------------------# # 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 As O3 1.659(3) . ? As O1 1.660(3) . ? As O4 1.674(3) . ? As O2 1.723(3) . ? V O5 1.597(3) . ? V F 1.951(2) 7_556 ? V O3 1.968(3) 6_556 ? V O1 2.005(2) . ? V O4 2.046(3) 7_556 ? V F 2.242(2) . ? F V 1.951(2) 7_556 ? O2 H2 0.82 . ? O3 V 1.968(3) 6 ? O4 V 2.046(3) 7_556 ? N1 C1 1.490(5) . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? C1 C2 1.465(7) . ? C1 C3 1.482(8) . ? C1 H1 0.98 . ? C2 C2 1.540(10) 2_554 ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C3 1.562(10) 2_554 ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? 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 O3 As O1 111.52(13) . . ? O3 As O4 110.73(13) . . ? O1 As O4 114.26(13) . . ? O3 As O2 101.69(13) . . ? O1 As O2 109.13(13) . . ? O4 As O2 108.72(13) . . ? O5 V F 102.13(13) . 7_556 ? O5 V O3 100.47(14) . 6_556 ? F V O3 157.21(10) 7_556 6_556 ? O5 V O1 101.36(13) . . ? F V O1 85.71(10) 7_556 . ? O3 V O1 87.04(11) 6_556 . ? O5 V O4 94.37(13) . 7_556 ? F V O4 86.29(10) 7_556 7_556 ? O3 V O4 94.90(11) 6_556 7_556 ? O1 V O4 163.55(11) . 7_556 ? O5 V F 174.10(13) . . ? F V F 74.74(10) 7_556 . ? O3 V F 82.99(10) 6_556 . ? O1 V F 83.52(9) . . ? O4 V F 80.52(9) 7_556 . ? V F V 105.26(10) 7_556 . ? As O1 V 121.64(15) . . ? As O2 H2 109.5 . . ? As O3 V 136.74(16) . 6 ? As O4 V 124.32(15) . 7_556 ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C2 C1 C3 113.6(5) . . ? C2 C1 N1 111.9(4) . . ? C3 C1 N1 111.5(4) . . ? C2 C1 H1 106.4 . . ? C3 C1 H1 106.4 . . ? N1 C1 H1 106.4 . . ? C1 C2 C2 111.4(4) . 2_554 ? C1 C2 H2A 109.3 . . ? C2 C2 H2A 109.3 2_554 . ? C1 C2 H2B 109.3 . . ? C2 C2 H2B 109.3 2_554 . ? H2A C2 H2B 108 . . ? C1 C3 C3 109.0(4) . 2_554 ? C1 C3 H3A 109.9 . . ? C3 C3 H3A 109.9 2_554 . ? C1 C3 H3B 109.9 . . ? C3 C3 H3B 109.9 2_554 . ? H3A C3 H3B 108.3 . . ? # Attachment 'DchVAs_LT.cif' data_vasdch _database_code_depnum_ccdc_archive 'CCDC 711729' _audit_creation_date 2008-04-15T12:49:31-00:00 _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_formula_sum 'C3 H9 As F N O5 V' _chemical_formula_weight 283.97 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.065(2) _cell_length_b 7.2717(4) _cell_length_c 10.3959(10) _cell_angle_alpha 90 _cell_angle_beta 104.290(8) _cell_angle_gamma 90 _cell_volume 1543.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7049 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 27.92 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.168 _exptl_crystal_size_min 0.023 _exptl_crystal_density_diffrn 2.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.544 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_absorpt_correction_T_min 0.4148 _exptl_absorpt_correction_T_max 0.8796 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_probe x-ray _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_area_resol_mean 6.67 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_unetI/netI 0.0694 _diffrn_reflns_number 1698 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 27.58 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.966 _diffrn_measured_fraction_theta_max 0.945 _reflns_number_total 1698 _reflns_number_gt 1220 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'DIRDIF99 (Beurkens et al, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _publ_section_references ; P.T. Beurskens, G. Beurskens, R. de Gelder, S. Garcia-Granda, R.O. Gould, and J.M.M. Smits (2008). The DIRDIF2008 program system, Crystallography Laboratory, University of Nijmegen, The Netherlands. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838 Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. Stoe & Cie (2002). Program name(s). Stoe & Cie GmbH, Darmstadt, Germany ; #----------------------------------------------------------------------------# # 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^)+(0.0465P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 1698 _refine_ls_number_parameters 111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.064 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.266 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.184 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 As As 0.19163(3) 0.18772(10) 0.23053(6) 0.01519(17) Uani 1 1 d . . . V V 0.18059(5) 0.18478(19) 0.53353(10) 0.0160(3) Uani 1 1 d . . . F F 0.28195(16) 0.1015(5) 0.5358(4) 0.0213(9) Uani 1 1 d . . . O1 O 0.1596(2) 0.0920(8) 0.3451(4) 0.0201(11) Uani 1 1 d . . . O2 O 0.1528(2) 0.3951(6) 0.1865(5) 0.0254(11) Uani 1 1 d . . . H2 H 0.1672 0.4433 0.1283 0.038 Uiso 1 1 calc R . . O3 O 0.1727(2) 0.0720(7) 0.0889(4) 0.0204(11) Uani 1 1 d . . . O4 O 0.2725(2) 0.2240(6) 0.2811(4) 0.0205(10) Uani 1 1 d . . . O5 O 0.1112(2) 0.2650(8) 0.5409(5) 0.0255(13) Uani 1 1 d . . . N1 N 0.1167(3) 0.2913(10) -0.1463(7) 0.0301(15) Uani 1 1 d . . . H1A H 0.1134 0.2752 -0.2325 0.045 Uiso 1 1 calc R . . H1B H 0.1407 0.2011 -0.1006 0.045 Uiso 1 1 calc R . . H1C H 0.1358 0.3989 -0.1208 0.045 Uiso 1 1 calc R . . C1 C 0.0478(3) 0.2891(11) -0.1201(8) 0.0297(17) Uani 1 1 d . . . H1 H 0.0532 0.2915 -0.0237 0.036 Uiso 1 1 calc R . . C2 C 0.0114(4) 0.1156(11) -0.1724(9) 0.033(2) Uani 1 1 d . . . H2A H -0.0266 0.1037 -0.136 0.04 Uiso 1 1 calc R . . H2B H 0.0396 0.0104 -0.1433 0.04 Uiso 1 1 calc R . . C3 C 0.0116(4) 0.4596(11) -0.1764(8) 0.035(2) Uani 1 1 d . . . H3A H -0.026 0.4741 -0.1389 0.042 Uiso 1 1 calc R . . H3B H 0.04 0.5649 -0.1492 0.042 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 As 0.0201(3) 0.0142(3) 0.0113(3) -0.0007(4) 0.0040(2) 0.0005(3) V 0.0202(6) 0.0151(6) 0.0123(5) 0.0002(6) 0.0033(4) -0.0005(5) F 0.0228(19) 0.020(2) 0.022(2) -0.0003(18) 0.0083(15) -0.0018(15) O1 0.022(2) 0.028(3) 0.011(2) -0.007(2) 0.0041(18) -0.004(2) O2 0.031(2) 0.022(3) 0.023(3) 0.002(3) 0.005(2) 0.0026(19) O3 0.030(3) 0.016(3) 0.014(2) -0.002(2) 0.0026(18) 0.006(2) O4 0.025(2) 0.024(3) 0.013(2) 0.000(2) 0.0051(18) 0.0004(18) O5 0.024(2) 0.026(3) 0.028(3) 0.000(2) 0.010(2) 0.002(2) N1 0.029(3) 0.027(4) 0.033(3) 0.019(4) 0.007(3) 0.004(3) C1 0.026(3) 0.042(5) 0.025(4) 0.007(4) 0.012(3) 0.005(3) C2 0.032(4) 0.025(4) 0.044(5) 0.013(4) 0.012(3) 0.001(3) C3 0.026(4) 0.030(5) 0.044(6) -0.013(4) -0.001(3) 0.001(3) #----------------------------------------------------------------------------# # 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 As O3 1.657(5) . ? As O1 1.660(5) . ? As O4 1.674(4) . ? As O2 1.722(5) . ? V O5 1.593(5) . ? V F 1.959(4) 7_556 ? V O3 1.973(5) 6_556 ? V O1 2.015(5) . ? V O4 2.047(5) 7_556 ? V F 2.214(4) . ? F V 1.959(4) 7_556 ? O2 H2 0.82 . ? O3 V 1.973(5) 6 ? O4 V 2.047(5) 7_556 ? N1 C1 1.540(9) . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? C1 C3 1.497(11) . ? C1 C2 1.507(11) . ? C1 H1 0.98 . ? C2 C2 1.565(17) 2_554 ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C3 1.488(17) 2_554 ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? 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 O3 As O1 111.9(2) . . ? O3 As O4 111.3(2) . . ? O1 As O4 113.8(2) . . ? O3 As O2 102.4(2) . . ? O1 As O2 107.9(3) . . ? O4 As O2 108.9(2) . . ? O5 V F 100.6(2) . 7_556 ? O5 V O3 100.8(3) . 6_556 ? F V O3 158.24(19) 7_556 6_556 ? O5 V O1 100.7(2) . . ? F V O1 85.4(2) 7_556 . ? O3 V O1 87.3(2) 6_556 . ? O5 V O4 94.1(2) . 7_556 ? F V O4 86.82(18) 7_556 7_556 ? O3 V O4 95.06(19) 6_556 7_556 ? O1 V O4 164.32(18) . 7_556 ? O5 V F 173.5(2) . . ? F V F 75.27(17) 7_556 . ? O3 V F 83.63(18) 6_556 . ? O1 V F 84.20(18) . . ? O4 V F 80.67(16) 7_556 . ? V F V 104.73(17) 7_556 . ? As O1 V 121.8(3) . . ? As O2 H2 109.5 . . ? As O3 V 136.1(3) . 6 ? As O4 V 124.4(2) . 7_556 ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C3 C1 C2 112.7(6) . . ? C3 C1 N1 109.5(6) . . ? C2 C1 N1 111.3(7) . . ? C3 C1 H1 107.7 . . ? C2 C1 H1 107.7 . . ? N1 C1 H1 107.7 . . ? C1 C2 C2 111.8(6) . 2_554 ? C1 C2 H2A 109.3 . . ? C2 C2 H2A 109.3 2_554 . ? C1 C2 H2B 109.3 . . ? C2 C2 H2B 109.3 2_554 . ? H2A C2 H2B 107.9 . . ? C3 C3 C1 114.1(6) 2_554 . ? C3 C3 H3A 108.7 2_554 . ? C1 C3 H3A 108.7 . . ? C3 C3 H3B 108.7 2_554 . ? C1 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 V F V -52(2) . . . 7_556 ? F V F V 0 7_556 . . 7_556 ? O3 V F V 174.6(2) 6_556 . . 7_556 ? O1 V F V 86.7(2) . . . 7_556 ? O4 V F V -89.1(2) 7_556 . . 7_556 ? O3 As O1 V 174.0(3) . . . . ? O4 As O1 V 46.8(4) . . . . ? O2 As O1 V -74.2(3) . . . . ? O5 V O1 As 112.8(4) . . . . ? F V O1 As 12.8(3) 7_556 . . . ? O3 V O1 As -146.7(3) 6_556 . . . ? O4 V O1 As -47.5(10) 7_556 . . . ? F V O1 As -62.8(3) . . . . ? O1 As O3 V -54.1(5) . . . 6 ? O4 As O3 V 74.4(4) . . . 6 ? O2 As O3 V -169.3(4) . . . 6 ? O3 As O4 V -167.4(3) . . . 7_556 ? O1 As O4 V -40.0(4) . . . 7_556 ? O2 As O4 V 80.4(4) . . . 7_556 ? C3 C1 C2 C2 50.6(10) . . . 2_554 ? N1 C1 C2 C2 -72.9(9) . . . 2_554 ? C2 C1 C3 C3 -50.3(11) . . . 2_554 ? N1 C1 C3 C3 74.1(10) . . . 2_554 ?