data_publication_text _publ_contact_author_name 'Daniel Lundberg' _publ_contact_author_address ;Department of Chemistry Uppsala Biocenter P.O. Box 7015 Swedish University of Agricultural Sciences SE-750 07 Uppsala SWEDEN ; _publ_contact_author_email daniel.lundberg@kemi.slu.se _publ_contact_author_phone +46-18-671549 loop_ _publ_author_name _publ_author_address 'Lundberg, Daniel' ;Department of Chemistry Uppsala Biocenter P.O. Box 7015 Swedish University of Agricultural Sciences SE-750 07 Uppsala SWEDEN ; 'Persson, Ingmar' ;Department of Chemistry Uppsala Biocenter P.O. Box 7015 Swedish University of Agricultural Sciences SE-750 07 Uppsala SWEDEN ; 'Krakowiak, Joanna' ;Department of Chemistry P.O. Box 7015 Swedish University of Agricultural Sciences SE-750 07 Uppsala SWEDEN permanent address: Department of Physical Chemistry Chemical Faculty Gdansk University of Technology Narutowicza 11/12 PL-80952 Gdansk POLAND ; data_voaqm _audit_creation_method SHELXL-97 _chemical_name_systematic 'pentaaquaoxovanadium(IV) trifluoromethanesulfonate' _chemical_name_common 'pentaaquaoxovanadium(IV) triflate' _chemical_formula_moiety '2(C F3 O3 S), H10 O6 V' _chemical_formula_sum 'C2 H10 F6 O12 S2 V' _chemical_compound_source synthesized _chemical_properties_physical hygroscopic _exptl_crystal_recrystallization_method 'from saturated aqueous solution' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour blue _diffrn_ambient_temperature 295(2) _chemical_formula_weight 455.16 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_int_tables_number 11 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.7598(11) _cell_length_b 7.8650(9) _cell_length_c 10.2154(11) _cell_angle_alpha 90.00 _cell_angle_beta 102.555(2) _cell_angle_gamma 90.00 _cell_volume 765.39(15) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4904 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 29.7 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 454 _exptl_absorpt_coefficient_mu 1.043 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.610 _exptl_absorpt_correction_T_max 0.728 _exptl_absorpt_process_details 'SADABS, Bruker (2004)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker APEX-II' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4087 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.67 _reflns_number_total 1561 _reflns_number_gt 1275 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 2.0' _computing_publication_material 'Diamond 2.0' _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^)+(0.0985P)^2^] 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 refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.086(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1561 _refine_ls_number_parameters 143 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_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 0.18123(6) 0.7500 0.04998(6) 0.0377(3) Uani 1 2 d S . . O1 O 0.0241(3) 0.7500 -0.0287(3) 0.0614(8) Uani 1 2 d S . . O11 O 0.1698(2) 0.5699(2) 0.1896(2) 0.0523(5) Uani 1 1 d D . . H11A H 0.202(4) 0.471(3) 0.190(4) 0.123(17) Uiso 1 1 d D . . H11B H 0.094(3) 0.560(4) 0.217(4) 0.098(14) Uiso 1 1 d D . . O12 O 0.2485(2) 0.5654(3) -0.0589(2) 0.0529(5) Uani 1 1 d D . . H12A H 0.196(3) 0.519(4) -0.125(3) 0.093(15) Uiso 1 1 d D . . H12B H 0.331(2) 0.564(5) -0.076(4) 0.105(15) Uiso 1 1 d D . . O13 O 0.4049(3) 0.7500 0.1429(3) 0.0479(7) Uani 1 2 d SD . . H13A H 0.458(2) 0.8357(19) 0.165(3) 0.077(11) Uiso 1 1 d D . . S2 S 0.45248(10) 0.2500 0.19077(11) 0.0456(3) Uani 1 2 d S . . O21 O 0.4993(2) 0.0974(2) 0.1375(3) 0.0669(7) Uani 1 1 d . . . O22 O 0.3063(3) 0.2500 0.1959(4) 0.0625(8) Uani 1 2 d S . . C2 C 0.5470(9) 0.2500 0.3642(8) 0.116(2) Uani 1 2 d S . . F21 F 0.5163(5) 0.1203(6) 0.4233(4) 0.235(2) Uani 1 1 d . . . F22 F 0.6827(5) 0.2500 0.3692(5) 0.163(2) Uani 1 2 d S . . S3 S 0.14706(9) 0.2500 0.69964(9) 0.0378(3) Uani 1 2 d S . . O31 O 0.07727(19) 0.0968(2) 0.72893(19) 0.0497(5) Uani 1 1 d . . . O32 O 0.2950(3) 0.2500 0.7475(3) 0.0597(8) Uani 1 2 d S . . C3 C 0.1169(5) 0.2500 0.5166(5) 0.0587(11) Uani 1 2 d S . . F31 F 0.1745(3) 0.1148(3) 0.4757(2) 0.0947(7) Uani 1 1 d . . . F32 F -0.0169(4) 0.2500 0.4626(3) 0.0945(10) Uani 1 2 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 0.0281(4) 0.0322(4) 0.0544(4) 0.000 0.0122(3) 0.000 O1 0.0335(15) 0.0664(18) 0.082(2) 0.000 0.0081(14) 0.000 O11 0.0494(12) 0.0348(10) 0.0808(15) 0.0079(9) 0.0319(11) 0.0032(9) O12 0.0390(11) 0.0545(12) 0.0678(14) -0.0209(10) 0.0173(10) -0.0087(10) O13 0.0329(13) 0.0364(14) 0.0720(19) 0.000 0.0059(13) 0.000 S2 0.0381(5) 0.0296(5) 0.0740(7) 0.000 0.0225(5) 0.000 O21 0.0536(13) 0.0380(10) 0.1183(19) -0.0113(11) 0.0385(13) -0.0009(9) O22 0.0439(16) 0.0432(15) 0.110(2) 0.000 0.0383(16) 0.000 C2 0.102(6) 0.151(7) 0.093(5) 0.000 0.018(5) 0.000 F21 0.198(4) 0.349(6) 0.150(3) 0.146(3) 0.019(3) -0.029(4) F22 0.079(3) 0.246(6) 0.141(4) 0.000 -0.026(3) 0.000 S3 0.0309(5) 0.0411(5) 0.0417(5) 0.000 0.0083(4) 0.000 O31 0.0438(11) 0.0480(10) 0.0599(12) 0.0051(9) 0.0169(9) -0.0046(9) O32 0.0327(15) 0.0635(17) 0.078(2) 0.000 0.0015(14) 0.000 C3 0.071(3) 0.059(3) 0.051(2) 0.000 0.021(2) 0.000 F31 0.135(2) 0.0867(14) 0.0730(14) -0.0184(11) 0.0463(14) 0.0146(15) F32 0.080(2) 0.122(2) 0.0650(18) 0.000 -0.0209(16) 0.000 _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 O1 1.569(3) . ? V1 O12 2.023(2) 4_575 ? V1 O12 2.023(2) . ? V1 O11 2.030(2) 4_575 ? V1 O11 2.030(2) . ? V1 O13 2.183(3) . ? S2 O21 1.434(2) . ? S2 O21 1.434(2) 4_565 ? S2 O22 1.439(3) . ? S2 C2 1.811(7) . ? C2 F21 1.255(5) . ? C2 F21 1.255(5) 4_565 ? C2 F22 1.315(9) . ? S3 O32 1.420(3) . ? S3 O31 1.4473(18) 4_565 ? S3 O31 1.4473(18) . ? S3 C3 1.828(5) . ? C3 F32 1.302(5) . ? C3 F31 1.313(3) . ? C3 F31 1.313(3) 4_565 ? 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 O1 V1 O12 96.68(11) . 4_575 ? O1 V1 O12 96.68(11) . . ? O12 V1 O12 91.71(13) 4_575 . ? O1 V1 O11 99.38(11) . 4_575 ? O12 V1 O11 87.67(9) 4_575 4_575 ? O12 V1 O11 163.89(9) . 4_575 ? O1 V1 O11 99.38(11) . . ? O12 V1 O11 163.89(9) 4_575 . ? O12 V1 O11 87.67(9) . . ? O11 V1 O11 88.49(13) 4_575 . ? O1 V1 O13 175.10(14) . . ? O12 V1 O13 79.95(8) 4_575 . ? O12 V1 O13 79.95(8) . . ? O11 V1 O13 84.10(8) 4_575 . ? O11 V1 O13 84.10(8) . . ? O21 S2 O21 113.74(18) . 4_565 ? O21 S2 O22 114.48(11) . . ? O21 S2 O22 114.48(11) 4_565 . ? O21 S2 C2 103.59(18) . . ? O21 S2 C2 103.59(18) 4_565 . ? O22 S2 C2 105.2(3) . . ? F21 C2 F21 108.8(8) . 4_565 ? F21 C2 F22 109.0(5) . . ? F21 C2 F22 109.0(5) 4_565 . ? F21 C2 S2 110.3(4) . . ? F21 C2 S2 110.3(4) 4_565 . ? F22 C2 S2 109.5(6) . . ? O32 S3 O31 114.69(10) . 4_565 ? O32 S3 O31 114.69(10) . . ? O31 S3 O31 112.77(15) 4_565 . ? O32 S3 C3 106.1(2) . . ? O31 S3 C3 103.47(12) 4_565 . ? O31 S3 C3 103.47(12) . . ? F32 C3 F31 108.9(3) . . ? F32 C3 F31 108.9(3) . 4_565 ? F31 C3 F31 108.1(4) . 4_565 ? F32 C3 S3 110.9(3) . . ? F31 C3 S3 109.9(2) . . ? F31 C3 S3 109.9(2) 4_565 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.486 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.069 #===END data_voclo4m _audit_creation_method SHELXL-97 _chemical_name_systematic 'pentakis(dimethylsulfoxide)oxovanadium(IV) perchlorate' _chemical_name_common 'pentakis(dmso)oxovanadium(IV) perchlorate' _chemical_formula_moiety 'C10 H30 O6 S5 V, 2 (Cl O4)' _chemical_formula_sum 'C10 H30 Cl2 O14 S5 V' _chemical_compound_source synthesized _chemical_properties_physical hygroscopic _exptl_crystal_recrystallization_method 'from saturated solution' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour blue _diffrn_ambient_temperature 295(2) _chemical_formula_weight 656.48 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' Cl Cl 0.1484 0.1585 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.0482(15) _cell_length_b 10.8796(15) _cell_length_c 24.928(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.297(5) _cell_angle_gamma 90.00 _cell_volume 2828.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1520 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 21.80 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 0.962 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7023 _exptl_absorpt_correction_T_max 0.8770 _exptl_absorpt_process_details 'SADABS, Bruker (2004)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13771 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4950 _reflns_number_gt 2477 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1357P)^2^] 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_extinction_coef ? _refine_ls_number_reflns 4950 _refine_ls_number_parameters 337 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.1324 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2255 _refine_ls_wR_factor_gt 0.1948 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_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 0.12116(10) 0.26322(9) 0.32771(4) 0.0547(3) Uani 1 1 d . A . O1 O 0.0891(5) 0.4063(5) 0.3715(2) 0.0829(14) Uani 1 1 d . . . S1 S -0.03336(18) 0.48066(17) 0.35499(8) 0.0783(6) Uani 1 1 d . . . C11 C -0.0546(10) 0.5082(10) 0.4217(4) 0.119(3) Uani 1 1 d . . . H11A H -0.0798 0.4333 0.4354 0.179 Uiso 1 1 calc R . . H11B H -0.1199 0.5693 0.4172 0.179 Uiso 1 1 calc R . . H11C H 0.0246 0.5368 0.4484 0.179 Uiso 1 1 calc R . . C12 C 0.0142(10) 0.6266(8) 0.3404(4) 0.117(3) Uani 1 1 d . . . H12A H 0.0287 0.6252 0.3045 0.176 Uiso 1 1 calc R . . H12B H 0.0920 0.6497 0.3698 0.176 Uiso 1 1 calc R . . H12C H -0.0518 0.6851 0.3389 0.176 Uiso 1 1 calc R . . O2 O 0.3091(4) 0.3036(4) 0.3586(2) 0.0811(14) Uani 1 1 d . . . S2 S 0.36629(18) 0.42805(18) 0.35159(9) 0.0824(6) Uani 1 1 d . . . C21 C 0.4245(10) 0.4872(10) 0.4198(4) 0.122(3) Uani 1 1 d . . . H21A H 0.3542 0.5151 0.4311 0.182 Uiso 1 1 calc R . . H21B H 0.4808 0.5548 0.4206 0.182 Uiso 1 1 calc R . . H21C H 0.4708 0.4244 0.4454 0.182 Uiso 1 1 calc R . . C22 C 0.5103(8) 0.3865(8) 0.3416(4) 0.108(3) Uani 1 1 d . . . H22A H 0.4924 0.3518 0.3043 0.162 Uiso 1 1 calc R . . H22B H 0.5541 0.3269 0.3697 0.162 Uiso 1 1 calc R . . H22C H 0.5634 0.4579 0.3452 0.162 Uiso 1 1 calc R . . O3 O -0.0565(5) 0.2000(5) 0.3163(2) 0.0921(16) Uani 1 1 d . . . S3A S -0.1110(3) 0.1385(4) 0.3519(2) 0.0693(16) Uani 0.496(8) 1 d P A 1 S3B S -0.1174(4) 0.0876(4) 0.3112(3) 0.092(2) Uani 0.504(8) 1 d P A 2 C31 C -0.2776(8) 0.1241(11) 0.3111(6) 0.162(5) Uani 1 1 d . . . H31A H -0.3138 0.2043 0.3004 0.243 Uiso 1 1 calc R A 1 H31B H -0.3217 0.0836 0.3335 0.243 Uiso 1 1 calc R A 1 H31C H -0.2866 0.0766 0.2776 0.243 Uiso 1 1 calc R A 1 C32 C -0.0759(10) -0.0148(9) 0.3614(5) 0.144(4) Uani 1 1 d . . . H32A H 0.0127 -0.0250 0.3838 0.217 Uiso 1 1 calc R A 1 H32B H -0.0918 -0.0533 0.3250 0.217 Uiso 1 1 calc R A 1 H32C H -0.1289 -0.0522 0.3805 0.217 Uiso 1 1 calc R A 1 O4 O 0.1646(5) 0.0962(4) 0.3036(2) 0.0889(15) Uani 1 1 d . . . S4 S 0.2847(2) 0.0259(2) 0.32914(11) 0.0954(7) Uani 1 1 d . A . C41 C 0.2369(10) -0.1235(9) 0.3311(5) 0.144(4) Uani 1 1 d . . . H41A H 0.1976 -0.1320 0.3600 0.216 Uiso 1 1 calc R A . H41B H 0.3102 -0.1767 0.3396 0.216 Uiso 1 1 calc R . . H41C H 0.1763 -0.1453 0.2949 0.216 Uiso 1 1 calc R . . C42 C 0.3494(12) 0.0068(15) 0.2749(5) 0.198(7) Uani 1 1 d . . . H42A H 0.3843 0.0835 0.2678 0.298 Uiso 1 1 calc R A . H42B H 0.2835 -0.0198 0.2410 0.298 Uiso 1 1 calc R . . H42C H 0.4162 -0.0539 0.2860 0.298 Uiso 1 1 calc R . . O5 O 0.1680(5) 0.1688(5) 0.40851(19) 0.0793(14) Uani 1 1 d . . . S5 S 0.2344(2) 0.2154(2) 0.46709(9) 0.0907(7) Uani 1 1 d . A . C51 C 0.3771(8) 0.1276(10) 0.4950(4) 0.118(3) Uani 1 1 d . . . H51A H 0.4370 0.1509 0.4764 0.177 Uiso 1 1 calc R A . H51B H 0.3572 0.0418 0.4887 0.177 Uiso 1 1 calc R . . H51C H 0.4141 0.1428 0.5351 0.177 Uiso 1 1 calc R . . C52 C 0.1456(9) 0.1534(11) 0.5086(4) 0.124(4) Uani 1 1 d . . . H52A H 0.0639 0.1938 0.4988 0.185 Uiso 1 1 calc R A . H52B H 0.1920 0.1660 0.5482 0.185 Uiso 1 1 calc R . . H52C H 0.1328 0.0670 0.5011 0.185 Uiso 1 1 calc R . . O6 O 0.0890(5) 0.3284(5) 0.2682(2) 0.0831(14) Uani 1 1 d . . . Cl1 Cl 0.3944(2) 0.2458(2) 0.16539(10) 0.0923(7) Uani 1 1 d DU . . O11 O 0.430(4) 0.199(3) 0.1233(13) 0.246(13) Uani 0.496(8) 1 d PDU A 1 O12 O 0.387(3) 0.3657(13) 0.1561(15) 0.27(2) Uani 0.496(8) 1 d PDU A 1 O13 O 0.2823(17) 0.202(3) 0.1617(16) 0.259(17) Uani 0.496(8) 1 d PDU A 1 O14 O 0.482(3) 0.218(3) 0.2128(11) 0.233(19) Uani 0.496(8) 1 d PDU A 1 O11B O 0.5088(12) 0.1988(19) 0.1867(11) 0.140(10) Uani 0.504(8) 1 d PDU A 2 O12B O 0.403(3) 0.3448(17) 0.1330(7) 0.181(14) Uani 0.504(8) 1 d PDU A 2 O13B O 0.3164(19) 0.1653(14) 0.1305(10) 0.155(10) Uani 0.504(8) 1 d PDU A 2 O14B O 0.349(3) 0.287(2) 0.2038(11) 0.205(10) Uani 0.504(8) 1 d PDU A 2 Cl2 Cl 0.2457(2) 0.7372(2) 0.00414(11) 0.0920(6) Uani 1 1 d D . . O21 O 0.1457(10) 0.6738(11) -0.0304(5) 0.256(6) Uani 1 1 d D . . O22 O 0.3210(13) 0.6706(10) 0.0473(4) 0.252(7) Uani 1 1 d D . . O23 O 0.2069(14) 0.8337(13) 0.0200(6) 0.398(14) Uani 1 1 d D . . O24 O 0.3138(16) 0.7584(18) -0.0269(7) 0.375(11) Uani 1 1 d D . . 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 0.0542(6) 0.0456(6) 0.0614(7) 0.0028(5) 0.0151(5) 0.0004(5) O1 0.081(3) 0.072(3) 0.086(3) -0.023(3) 0.015(3) 0.013(3) S1 0.0756(12) 0.0612(11) 0.0890(13) -0.0023(9) 0.0149(10) 0.0091(9) C11 0.132(8) 0.129(8) 0.122(8) 0.002(6) 0.077(7) 0.027(6) C12 0.146(9) 0.085(6) 0.123(8) 0.036(5) 0.047(7) 0.006(6) O2 0.061(3) 0.067(3) 0.109(4) 0.006(3) 0.018(3) -0.010(2) S2 0.0704(12) 0.0687(13) 0.1041(15) 0.0010(11) 0.0233(11) -0.0123(9) C21 0.131(8) 0.113(8) 0.139(9) -0.049(6) 0.069(7) -0.034(6) C22 0.101(7) 0.096(7) 0.146(8) -0.009(6) 0.066(6) -0.020(5) O3 0.058(3) 0.081(4) 0.130(5) 0.021(3) 0.021(3) -0.009(3) S3A 0.062(2) 0.079(3) 0.069(3) -0.008(2) 0.0250(19) -0.0068(19) S3B 0.084(3) 0.067(3) 0.129(5) -0.005(3) 0.038(3) -0.013(2) C31 0.064(6) 0.156(10) 0.276(15) 0.057(10) 0.068(8) 0.001(6) C32 0.121(8) 0.104(8) 0.177(11) 0.055(7) 0.008(7) -0.009(6) O4 0.081(3) 0.063(3) 0.111(4) -0.012(3) 0.016(3) 0.012(3) S4 0.0827(14) 0.0707(14) 0.1205(18) -0.0036(12) 0.0171(12) 0.0156(11) C41 0.116(8) 0.089(7) 0.232(13) 0.033(8) 0.064(8) 0.011(6) C42 0.165(12) 0.288(19) 0.177(12) 0.077(13) 0.104(11) 0.115(13) O5 0.084(3) 0.088(4) 0.062(3) 0.014(3) 0.018(3) 0.000(3) S5 0.0870(14) 0.0966(16) 0.0797(14) 0.0119(11) 0.0159(11) 0.0010(12) C51 0.071(5) 0.153(9) 0.117(7) 0.043(6) 0.014(5) 0.014(5) C52 0.096(6) 0.212(12) 0.076(6) 0.008(6) 0.047(5) -0.012(7) O6 0.087(3) 0.086(3) 0.074(3) 0.013(3) 0.023(3) 0.003(3) Cl1 0.0790(15) 0.0886(17) 0.1005(17) -0.0072(14) 0.0176(12) -0.0011(12) O11 0.32(4) 0.23(3) 0.26(3) 0.05(2) 0.19(3) 0.11(3) O12 0.20(3) 0.073(15) 0.44(5) -0.08(2) -0.02(3) 0.040(15) O13 0.095(14) 0.37(5) 0.31(4) 0.04(3) 0.06(2) -0.06(2) O14 0.21(3) 0.25(3) 0.141(19) 0.07(2) -0.06(2) -0.02(3) O11B 0.052(8) 0.124(13) 0.22(3) -0.007(16) 0.016(12) 0.018(8) O12B 0.25(3) 0.16(2) 0.095(11) 0.055(13) -0.004(12) -0.05(2) O13B 0.100(14) 0.110(12) 0.19(2) -0.053(13) -0.038(13) 0.007(10) O14B 0.26(3) 0.17(2) 0.21(2) 0.035(18) 0.10(2) 0.01(2) Cl2 0.0736(13) 0.0919(16) 0.1067(16) -0.0066(13) 0.0247(12) 0.0029(12) O21 0.164(9) 0.228(12) 0.300(14) 0.022(11) -0.024(9) -0.071(9) O22 0.331(16) 0.167(9) 0.175(9) 0.003(8) -0.029(10) 0.040(10) O23 0.291(17) 0.39(2) 0.40(2) -0.248(18) -0.039(15) 0.205(17) O24 0.31(2) 0.47(3) 0.40(2) 0.11(2) 0.193(19) -0.047(19) _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 O6 1.574(5) . ? V1 O1 1.998(5) . ? V1 O3 2.010(5) . ? V1 O2 2.010(5) . ? V1 O4 2.022(5) . ? V1 O5 2.166(4) . ? O1 S1 1.513(5) . ? S1 C12 1.748(9) . ? S1 C11 1.779(8) . ? O2 S2 1.528(5) . ? S2 C21 1.730(8) . ? S2 C22 1.750(8) . ? O3 S3B 1.381(7) . ? O3 S3A 1.396(6) . ? S3A C32 1.711(11) . ? S3A C31 1.792(11) . ? S3B C32 1.624(10) . ? S3B C31 1.813(10) . ? O4 S4 1.481(5) . ? S4 C41 1.715(10) . ? S4 C42 1.737(10) . ? O5 S5 1.490(5) . ? S5 C51 1.776(8) . ? S5 C52 1.778(8) . ? Cl1 O14 1.293(14) . ? Cl1 O13 1.301(14) . ? Cl1 O14B 1.301(13) . ? Cl1 O11B 1.302(12) . ? Cl1 O12 1.323(14) . ? Cl1 O13B 1.331(11) . ? Cl1 O11 1.339(14) . ? Cl1 O12B 1.368(12) . ? Cl2 O23 1.246(9) . ? Cl2 O24 1.266(11) . ? Cl2 O22 1.336(9) . ? Cl2 O21 1.345(9) . ? 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 O6 V1 O1 97.9(2) . . ? O6 V1 O3 96.6(2) . . ? O1 V1 O3 90.2(2) . . ? O6 V1 O2 98.4(2) . . ? O1 V1 O2 88.1(2) . . ? O3 V1 O2 165.0(2) . . ? O6 V1 O4 97.3(2) . . ? O1 V1 O4 164.8(2) . . ? O3 V1 O4 88.1(2) . . ? O2 V1 O4 89.6(2) . . ? O6 V1 O5 178.2(2) . . ? O1 V1 O5 83.8(2) . . ? O3 V1 O5 83.7(2) . . ? O2 V1 O5 81.3(2) . . ? O4 V1 O5 81.0(2) . . ? S1 O1 V1 124.9(3) . . ? O1 S1 C12 103.8(4) . . ? O1 S1 C11 102.6(4) . . ? C12 S1 C11 100.5(5) . . ? S2 O2 V1 124.3(3) . . ? O2 S2 C21 104.5(4) . . ? O2 S2 C22 102.5(4) . . ? C21 S2 C22 100.1(5) . . ? S3B O3 S3A 48.4(3) . . ? S3B O3 V1 137.7(4) . . ? S3A O3 V1 132.8(4) . . ? O3 S3A C32 115.4(6) . . ? O3 S3A C31 105.0(5) . . ? C32 S3A C31 97.8(6) . . ? O3 S3B C32 122.1(6) . . ? O3 S3B C31 104.6(5) . . ? C32 S3B C31 100.3(6) . . ? S3A C31 S3B 36.8(2) . . ? S3B C32 S3A 39.8(3) . . ? S4 O4 V1 127.1(3) . . ? O4 S4 C41 105.1(4) . . ? O4 S4 C42 105.5(5) . . ? C41 S4 C42 96.8(7) . . ? S5 O5 V1 129.7(3) . . ? O5 S5 C51 106.7(4) . . ? O5 S5 C52 104.6(4) . . ? C51 S5 C52 99.0(5) . . ? O14 Cl1 O13 112.9(14) . . ? O14 Cl1 O14B 76.2(16) . . ? O13 Cl1 O14B 65.5(15) . . ? O14 Cl1 O11B 37.1(16) . . ? O13 Cl1 O11B 131.2(19) . . ? O14B Cl1 O11B 113.2(12) . . ? O14 Cl1 O12 111.9(14) . . ? O13 Cl1 O12 110.2(14) . . ? O14B Cl1 O12 76.9(16) . . ? O11B Cl1 O12 117.0(18) . . ? O14 Cl1 O13B 125.0(18) . . ? O13 Cl1 O13B 47.0(14) . . ? O14B Cl1 O13B 112.5(13) . . ? O11B Cl1 O13B 109.9(10) . . ? O12 Cl1 O13B 123.1(17) . . ? O14 Cl1 O11 107.6(13) . . ? O13 Cl1 O11 108.9(14) . . ? O14B Cl1 O11 174.3(16) . . ? O11B Cl1 O11 70.9(15) . . ? O12 Cl1 O11 105.1(13) . . ? O13B Cl1 O11 61.9(14) . . ? O14 Cl1 O12B 123.0(18) . . ? O13 Cl1 O12B 119.7(19) . . ? O14B Cl1 O12B 106.5(11) . . ? O11B Cl1 O12B 107.6(11) . . ? O12 Cl1 O12B 29.9(17) . . ? O13B Cl1 O12B 106.7(11) . . ? O11 Cl1 O12B 75.2(14) . . ? O23 Cl2 O24 112.2(11) . . ? O23 Cl2 O22 112.9(8) . . ? O24 Cl2 O22 104.7(10) . . ? O23 Cl2 O21 109.9(8) . . ? O24 Cl2 O21 103.3(9) . . ? O22 Cl2 O21 113.5(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.677 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.085 #===END data_vo2cf1m _audit_creation_method SHELXL-97 _chemical_name_systematic 'tetrakis(dimethylsulfoxide)dioxovanadium(V) triflate' _chemical_name_common 'tetrakis(dmso)dioxovanadium triflate' _chemical_formula_moiety 'C8 H24 O6 S4 V, C F3 O3 S' _chemical_formula_sum 'C9 H24 F3 O9 S5 V' _chemical_compound_source synthesized _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour yellow _diffrn_ambient_temperature 295(2) _chemical_formula_weight 544.52 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.756(3) _cell_length_b 6.4360(12) _cell_length_c 24.660(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.291(4) _cell_angle_gamma 90.00 _cell_volume 2181.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1820 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 21.80 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.420 _exptl_absorpt_correction_T_max 0.448 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11340 _diffrn_reflns_av_R_equivalents 0.1607 _diffrn_reflns_av_sigmaI/netI 0.2018 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4116 _reflns_number_gt 1717 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0379P)^2^] 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_extinction_coef ? _refine_ls_number_reflns 4116 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2107 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1114 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_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 0.13569(9) 0.4449(2) 0.37340(5) 0.0392(4) Uani 1 1 d . . . O11 O 0.0547(4) 0.3279(9) 0.4067(2) 0.079(2) Uani 1 1 d . A . O12 O 0.1350(5) 0.3251(10) 0.3170(2) 0.090(2) Uani 1 1 d . A . O13 O 0.0641(8) 0.6707(17) 0.3285(5) 0.049(3) Uani 0.548(6) 1 d P A 1 S13 S -0.0323(3) 0.7452(7) 0.3491(2) 0.0486(15) Uani 0.548(6) 1 d P A 1 O13B O 0.0356(9) 0.6785(17) 0.3681(5) 0.039(3) Uani 0.452(6) 1 d P A 2 S13B S -0.0032(4) 0.7442(7) 0.3112(2) 0.0390(16) Uani 0.452(6) 1 d P A 2 C131 C -0.0543(6) 0.9888(11) 0.3204(3) 0.062(3) Uani 1 1 d . . . H13A H -0.0029 1.0823 0.3316 0.093 Uiso 1 1 calc R A 1 H13B H -0.1152 1.0414 0.3322 0.093 Uiso 1 1 calc R A 1 H13C H -0.0568 0.9772 0.2816 0.093 Uiso 1 1 calc R A 1 C132 C -0.1156(5) 0.5964(12) 0.3060(4) 0.070(3) Uani 1 1 d . . . H13D H -0.1266 0.6677 0.2721 0.104 Uiso 1 1 calc R A 1 H13E H -0.1762 0.5805 0.3235 0.104 Uiso 1 1 calc R A 1 H13F H -0.0882 0.4619 0.2994 0.104 Uiso 1 1 calc R A 1 O14 O 0.1653(4) 0.6680(9) 0.4399(2) 0.077(2) Uani 1 1 d . A . S14 S 0.09804(15) 0.6849(3) 0.48559(8) 0.0435(6) Uani 1 1 d . . . C141 C 0.1233(6) 0.9370(11) 0.5125(3) 0.056(2) Uani 1 1 d . A . H14A H 0.1902 0.9440 0.5251 0.084 Uiso 1 1 calc R . . H14B H 0.0821 0.9633 0.5423 0.084 Uiso 1 1 calc R . . H14C H 0.1112 1.0394 0.4848 0.084 Uiso 1 1 calc R . . C142 C 0.1514(6) 0.5381(13) 0.5377(4) 0.075(3) Uani 1 1 d . A . H14D H 0.1394 0.3934 0.5309 0.112 Uiso 1 1 calc R . . H14E H 0.1241 0.5768 0.5715 0.112 Uiso 1 1 calc R . . H14F H 0.2203 0.5630 0.5396 0.112 Uiso 1 1 calc R . . O15 O 0.2521(4) 0.6530(9) 0.3475(2) 0.080(2) Uani 1 1 d . A . S15 S 0.27896(17) 0.6661(4) 0.28923(8) 0.0608(7) Uani 1 1 d . . . C151 C 0.3217(7) 0.9196(13) 0.2813(3) 0.078(3) Uani 1 1 d . A . H15A H 0.2697 1.0161 0.2866 0.118 Uiso 1 1 calc R . . H15B H 0.3451 0.9361 0.2454 0.118 Uiso 1 1 calc R . . H15C H 0.3736 0.9458 0.3075 0.118 Uiso 1 1 calc R . . C152 C 0.3926(7) 0.5413(16) 0.2873(4) 0.105(4) Uani 1 1 d . A . H15D H 0.4359 0.5984 0.3149 0.157 Uiso 1 1 calc R . . H15E H 0.4193 0.5623 0.2523 0.157 Uiso 1 1 calc R . . H15F H 0.3844 0.3953 0.2935 0.157 Uiso 1 1 calc R . . O16 O 0.2316(8) 0.2946(16) 0.4215(5) 0.042(3) Uani 0.548(6) 1 d P A 1 S16 S 0.3352(3) 0.2467(6) 0.40563(16) 0.0413(14) Uani 0.548(6) 1 d P A 1 O16B O 0.2633(10) 0.3082(19) 0.3898(5) 0.036(3) Uani 0.452(6) 1 d P A 2 S16B S 0.2951(4) 0.2432(7) 0.44802(19) 0.0369(16) Uani 0.452(6) 1 d P A 2 C161 C 0.3579(5) 0.0070(11) 0.4380(3) 0.051(2) Uani 1 1 d . . . H16A H 0.3870 0.0310 0.4735 0.077 Uiso 1 1 calc R A 1 H16B H 0.4014 -0.0739 0.4170 0.077 Uiso 1 1 calc R A 1 H16C H 0.2978 -0.0668 0.4412 0.077 Uiso 1 1 calc R A 1 C162 C 0.4045(6) 0.4064(13) 0.4541(4) 0.086(3) Uani 1 1 d . . . H16D H 0.3922 0.5505 0.4464 0.128 Uiso 1 1 calc R A 1 H16E H 0.4726 0.3781 0.4513 0.128 Uiso 1 1 calc R A 1 H16F H 0.3851 0.3752 0.4902 0.128 Uiso 1 1 calc R A 1 S3 S 0.37082(18) 0.6297(4) 0.12400(9) 0.0565(6) Uani 1 1 d . . . O31 O 0.4600(4) 0.6644(9) 0.1536(2) 0.0783(19) Uani 1 1 d . . . O32 O 0.2876(5) 0.6921(10) 0.1503(2) 0.091(2) Uani 1 1 d . . . O33 O 0.3734(4) 0.6782(10) 0.0679(2) 0.0772(19) Uani 1 1 d . . . C3 C 0.3579(8) 0.3515(16) 0.1233(4) 0.075(3) Uani 1 1 d . . . F31 F 0.2804(5) 0.2895(10) 0.0971(3) 0.119(2) Uani 1 1 d . . . F32 F 0.4334(5) 0.2632(9) 0.0999(3) 0.128(2) Uani 1 1 d . . . F33 F 0.3592(5) 0.2716(9) 0.1725(3) 0.119(2) Uani 1 1 d . . . 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 0.0367(8) 0.0426(8) 0.0379(8) -0.0019(7) -0.0024(6) -0.0004(7) O11 0.086(5) 0.078(4) 0.076(4) -0.023(4) 0.038(4) -0.044(4) O12 0.104(5) 0.116(6) 0.051(4) -0.033(4) 0.024(4) -0.059(4) O13 0.037(7) 0.067(8) 0.044(7) -0.003(6) 0.011(6) 0.008(6) S13 0.047(3) 0.057(3) 0.042(3) -0.002(2) 0.007(3) 0.005(2) O13B 0.025(7) 0.046(7) 0.045(8) 0.010(7) -0.006(7) 0.024(6) S13B 0.038(3) 0.044(3) 0.035(4) 0.003(2) 0.001(3) 0.004(2) C131 0.060(6) 0.046(6) 0.079(6) -0.002(5) -0.006(5) 0.007(4) C132 0.046(5) 0.051(6) 0.110(8) 0.012(6) -0.025(5) -0.008(4) O14 0.087(5) 0.078(4) 0.069(4) -0.036(3) 0.039(4) -0.042(4) S14 0.0446(12) 0.0483(14) 0.0375(11) -0.0067(10) 0.0019(10) -0.0048(10) C141 0.067(6) 0.046(5) 0.054(5) -0.003(5) 0.005(5) -0.003(5) C142 0.050(6) 0.061(6) 0.111(8) 0.018(6) -0.016(6) -0.001(5) O15 0.090(5) 0.110(5) 0.042(3) -0.017(4) 0.017(3) -0.058(4) S15 0.0682(16) 0.0768(17) 0.0376(12) -0.0018(12) 0.0038(12) -0.0279(14) C151 0.109(8) 0.068(7) 0.058(6) 0.017(5) 0.005(6) -0.006(6) C152 0.119(9) 0.115(9) 0.081(7) 0.002(7) 0.018(7) 0.052(8) O16 0.038(8) 0.042(7) 0.046(8) 0.012(6) 0.007(7) 0.007(5) S16 0.040(3) 0.042(2) 0.042(3) 0.0019(19) -0.001(2) 0.005(2) O16B 0.024(8) 0.051(8) 0.032(8) 0.012(7) -0.005(7) 0.005(6) S16B 0.031(3) 0.047(3) 0.032(3) 0.003(2) 0.002(2) 0.004(2) C161 0.046(5) 0.049(6) 0.059(6) 0.006(4) 0.002(5) 0.010(4) C162 0.067(6) 0.044(6) 0.142(9) -0.002(6) -0.040(7) -0.002(5) S3 0.0474(14) 0.0762(18) 0.0457(13) -0.0037(13) 0.0009(12) -0.0050(13) O31 0.068(4) 0.094(5) 0.071(4) 0.001(4) -0.022(4) -0.029(4) O32 0.066(4) 0.127(6) 0.082(4) -0.002(4) 0.026(4) 0.024(4) O33 0.080(5) 0.111(5) 0.041(3) 0.013(3) 0.010(3) -0.012(4) C3 0.062(7) 0.093(8) 0.069(7) 0.004(7) 0.005(6) -0.005(7) F31 0.107(5) 0.120(5) 0.125(5) 0.001(4) -0.055(4) -0.049(4) F32 0.133(6) 0.075(4) 0.179(7) -0.023(4) 0.033(5) 0.009(4) F33 0.138(6) 0.108(5) 0.108(5) 0.042(4) -0.024(4) -0.037(4) _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 O12 1.590(5) . ? V1 O11 1.598(5) . ? V1 O16 1.990(12) . ? V1 O16B 1.990(14) . ? V1 O13B 2.039(12) . ? V1 O13 2.055(13) . ? V1 O15 2.202(5) . ? V1 O14 2.206(5) . ? O13 S13 1.516(12) . ? S13 C131 1.742(9) . ? S13 C132 1.807(9) . ? O13B S13B 1.542(14) . ? C131 H13A 0.9600 . ? C131 H13B 0.9600 . ? C131 H13C 0.9600 . ? C132 H13D 0.9600 . ? C132 H13E 0.9600 . ? C132 H13F 0.9600 . ? O14 S14 1.490(5) . ? S14 C142 1.735(8) . ? S14 C141 1.782(7) . ? C141 H14A 0.9600 . ? C141 H14B 0.9600 . ? C141 H14C 0.9600 . ? C142 H14D 0.9600 . ? C142 H14E 0.9600 . ? C142 H14F 0.9600 . ? O15 S15 1.500(5) . ? S15 C151 1.747(8) . ? S15 C152 1.759(9) . ? C151 H15A 0.9600 . ? C151 H15B 0.9600 . ? C151 H15C 0.9600 . ? C152 H15D 0.9600 . ? C152 H15E 0.9600 . ? C152 H15F 0.9600 . ? O16 S16 1.524(12) . ? S16 C161 1.759(8) . ? S16 C162 1.817(9) . ? O16B S16B 1.543(13) . ? C161 H16A 0.9600 . ? C161 H16B 0.9600 . ? C161 H16C 0.9600 . ? C162 H16D 0.9600 . ? C162 H16E 0.9600 . ? C162 H16F 0.9600 . ? S3 O32 1.397(6) . ? S3 O33 1.420(5) . ? S3 O31 1.420(6) . ? S3 C3 1.799(11) . ? C3 F31 1.288(10) . ? C3 F33 1.317(10) . ? C3 F32 1.334(10) . ? 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 O12 V1 O11 103.9(3) . . ? O12 V1 O16 105.4(4) . . ? O11 V1 O16 85.7(4) . . ? O12 V1 O16B 86.4(4) . . ? O11 V1 O16B 108.3(4) . . ? O16 V1 O16B 26.6(3) . . ? O12 V1 O13B 108.8(4) . . ? O11 V1 O13B 84.1(4) . . ? O16 V1 O13B 145.7(5) . . ? O16B V1 O13B 157.9(5) . . ? O12 V1 O13 83.5(4) . . ? O11 V1 O13 106.3(4) . . ? O16 V1 O13 163.2(4) . . ? O16B V1 O13 145.3(5) . . ? O13B V1 O13 30.3(3) . . ? O12 V1 O15 91.1(2) . . ? O11 V1 O15 164.9(2) . . ? O16 V1 O15 89.8(3) . . ? O16B V1 O15 71.5(4) . . ? O13B V1 O15 91.7(4) . . ? O13 V1 O15 75.6(3) . . ? O12 V1 O14 163.9(3) . . ? O11 V1 O14 92.1(2) . . ? O16 V1 O14 77.0(4) . . ? O16B V1 O14 90.1(4) . . ? O13B V1 O14 70.8(4) . . ? O13 V1 O14 90.6(4) . . ? O15 V1 O14 72.86(19) . . ? S13 O13 V1 116.7(8) . . ? O13 S13 C131 106.8(7) . . ? O13 S13 C132 100.2(6) . . ? C131 S13 C132 98.2(5) . . ? S13B O13B V1 117.9(8) . . ? S13 C131 H13A 109.5 . . ? S13 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? S13 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? S13 C132 H13D 109.5 . . ? S13 C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? S13 C132 H13F 109.5 . . ? H13D C132 H13F 109.5 . . ? H13E C132 H13F 109.5 . . ? S14 O14 V1 120.5(3) . . ? O14 S14 C142 105.2(4) . . ? O14 S14 C141 103.3(3) . . ? C142 S14 C141 98.6(4) . . ? S14 C141 H14A 109.5 . . ? S14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? S14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? S14 C142 H14D 109.5 . . ? S14 C142 H14E 109.5 . . ? H14D C142 H14E 109.5 . . ? S14 C142 H14F 109.5 . . ? H14D C142 H14F 109.5 . . ? H14E C142 H14F 109.5 . . ? S15 O15 V1 121.5(3) . . ? O15 S15 C151 104.9(4) . . ? O15 S15 C152 104.7(4) . . ? C151 S15 C152 96.9(5) . . ? S15 C151 H15A 109.5 . . ? S15 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? S15 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? S15 C152 H15D 109.5 . . ? S15 C152 H15E 109.5 . . ? H15D C152 H15E 109.5 . . ? S15 C152 H15F 109.5 . . ? H15D C152 H15F 109.5 . . ? H15E C152 H15F 109.5 . . ? S16 O16 V1 123.4(7) . . ? O16 S16 C161 102.2(5) . . ? O16 S16 C162 100.8(6) . . ? C161 S16 C162 96.8(4) . . ? S16B O16B V1 121.6(8) . . ? S16 C161 H16A 109.5 . . ? S16 C161 H16B 109.5 . . ? H16A C161 H16B 109.5 . . ? S16 C161 H16C 109.5 . . ? H16A C161 H16C 109.5 . . ? H16B C161 H16C 109.5 . . ? S16 C162 H16D 109.5 . . ? S16 C162 H16E 109.5 . . ? H16D C162 H16E 109.5 . . ? S16 C162 H16F 109.5 . . ? H16D C162 H16F 109.5 . . ? H16E C162 H16F 109.5 . . ? O32 S3 O33 116.2(4) . . ? O32 S3 O31 115.0(4) . . ? O33 S3 O31 114.4(4) . . ? O32 S3 C3 102.0(5) . . ? O33 S3 C3 102.4(5) . . ? O31 S3 C3 104.2(5) . . ? F31 C3 F33 108.7(9) . . ? F31 C3 F32 107.1(9) . . ? F33 C3 F32 104.4(9) . . ? F31 C3 S3 113.1(8) . . ? F33 C3 S3 112.4(7) . . ? F32 C3 S3 110.5(7) . . ? 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 O12 V1 O13 S13 126.1(7) . . . . ? O11 V1 O13 S13 23.5(8) . . . . ? O16 V1 O13 S13 -110.8(14) . . . . ? O16B V1 O13 S13 -160.0(7) . . . . ? O13B V1 O13 S13 -20.9(7) . . . . ? O15 V1 O13 S13 -141.0(7) . . . . ? O14 V1 O13 S13 -68.9(7) . . . . ? V1 O13 S13 C131 158.9(5) . . . . ? V1 O13 S13 C132 -99.3(7) . . . . ? O12 V1 O13B S13B -16.0(9) . . . . ? O11 V1 O13B S13B -118.7(8) . . . . ? O16 V1 O13B S13B 167.9(6) . . . . ? O16B V1 O13B S13B 115.4(12) . . . . ? O13 V1 O13B S13B 18.8(7) . . . . ? O15 V1 O13B S13B 75.8(8) . . . . ? O14 V1 O13B S13B 147.0(9) . . . . ? O12 V1 O14 S14 161.5(10) . . . . ? O11 V1 O14 S14 -13.0(5) . . . . ? O16 V1 O14 S14 -98.0(5) . . . . ? O16B V1 O14 S14 -121.3(5) . . . . ? O13B V1 O14 S14 70.1(6) . . . . ? O13 V1 O14 S14 93.4(5) . . . . ? O15 V1 O14 S14 168.2(5) . . . . ? V1 O14 S14 C142 98.5(5) . . . . ? V1 O14 S14 C141 -158.6(4) . . . . ? O12 V1 O15 S15 13.9(5) . . . . ? O11 V1 O15 S15 -168.6(10) . . . . ? O16 V1 O15 S15 119.3(5) . . . . ? O16B V1 O15 S15 99.7(6) . . . . ? O13B V1 O15 S15 -94.9(5) . . . . ? O13 V1 O15 S15 -69.0(5) . . . . ? O14 V1 O15 S15 -164.2(5) . . . . ? V1 O15 S15 C151 150.6(5) . . . . ? V1 O15 S15 C152 -108.0(5) . . . . ? O12 V1 O16 S16 52.0(8) . . . . ? O11 V1 O16 S16 155.2(7) . . . . ? O16B V1 O16 S16 6.2(8) . . . . ? O13B V1 O16 S16 -131.9(8) . . . . ? O13 V1 O16 S16 -68.4(18) . . . . ? O15 V1 O16 S16 -39.2(7) . . . . ? O14 V1 O16 S16 -111.6(7) . . . . ? V1 O16 S16 C161 -146.7(6) . . . . ? V1 O16 S16 C162 113.8(7) . . . . ? O12 V1 O16B S16B -146.3(8) . . . . ? O11 V1 O16B S16B -42.8(9) . . . . ? O16 V1 O16B S16B -10.1(7) . . . . ? O13B V1 O16B S16B 79.1(16) . . . . ? O13 V1 O16B S16B 140.6(8) . . . . ? O15 V1 O16B S16B 121.3(8) . . . . ? O14 V1 O16B S16B 49.4(8) . . . . ? O32 S3 C3 F31 60.9(8) . . . . ? O33 S3 C3 F31 -59.7(8) . . . . ? O31 S3 C3 F31 -179.1(7) . . . . ? O32 S3 C3 F33 -62.8(9) . . . . ? O33 S3 C3 F33 176.6(7) . . . . ? O31 S3 C3 F33 57.2(8) . . . . ? O32 S3 C3 F32 -179.0(8) . . . . ? O33 S3 C3 F32 60.4(8) . . . . ? O31 S3 C3 F32 -59.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.308 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.083 #===END data_vodmpu3m _audit_creation_method SHELXL-97 _chemical_name_systematic ;'tetrakis(N,N-dimethylpropyleneurea)oxovanadium(IV) trifluoromethanesulfonate' ; _chemical_name_common ;'tetrakis(dmpu)oxovanadium(IV) triflate' ; _chemical_formula_moiety ? _chemical_formula_sum 'C26 H48 F6 N8 O11 S2 V' _chemical_compound_source synthesized _chemical_properties_physical hygroscopic _exptl_crystal_recrystallization_method 'from dmpu solvent' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour blue _diffrn_ambient_temperature 295(2) _chemical_formula_weight 877.78 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.590(4) _cell_length_b 27.137(6) _cell_length_c 18.215(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.667(5) _cell_angle_gamma 90.00 _cell_volume 8107(3) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3656 _exptl_absorpt_coefficient_mu 0.436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.791 _exptl_absorpt_correction_T_max 0.840 _exptl_absorpt_process_details 'SADABS, Bruker (2004)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42469 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.1059 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.68 _reflns_number_total 15320 _reflns_number_gt 6205 _reflns_threshold_expression I>2\s(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 'Diamond 2.0' _computing_publication_material 'Diamond 2.0' _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^)+(0.1638P)^2^] 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_extinction_coef ? _refine_ls_number_reflns 15320 _refine_ls_number_parameters 1012 _refine_ls_number_restraints 99 _refine_ls_R_factor_all 0.2013 _refine_ls_R_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.2948 _refine_ls_wR_factor_gt 0.2299 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_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 0.17169(7) 0.39992(4) 0.36112(6) 0.0519(3) Uani 1 1 d . . . O10 O 0.2395(3) 0.44104(16) 0.3667(3) 0.0665(13) Uani 1 1 d . . . O1 O 0.2183(3) 0.33943(16) 0.4085(2) 0.0599(12) Uani 1 1 d . . . C1 C 0.2501(5) 0.2996(3) 0.3877(4) 0.0571(17) Uani 1 1 d . . . N11 N 0.2079(4) 0.2577(2) 0.3862(3) 0.0688(16) Uani 1 1 d . . . N12 N 0.3242(4) 0.3003(2) 0.3691(3) 0.0673(16) Uani 1 1 d . . . C11 C 0.1319(6) 0.2559(3) 0.4168(5) 0.100(3) Uani 1 1 d . . . H11A H 0.1397 0.2708 0.4652 0.150 Uiso 1 1 calc R . . H11B H 0.1154 0.2222 0.4207 0.150 Uiso 1 1 calc R . . H11C H 0.0905 0.2735 0.3848 0.150 Uiso 1 1 calc R . . C12 C 0.3723(5) 0.3452(4) 0.3785(6) 0.103(3) Uani 1 1 d . . . H12A H 0.3746 0.3569 0.4285 0.155 Uiso 1 1 calc R . . H12B H 0.3475 0.3698 0.3445 0.155 Uiso 1 1 calc R . . H12C H 0.4265 0.3385 0.3688 0.155 Uiso 1 1 calc R . . C13 C 0.2434(6) 0.2110(3) 0.3684(5) 0.087(3) Uani 1 1 d . . . H13A H 0.2006 0.1890 0.3457 0.104 Uiso 1 1 calc R . . H13B H 0.2703 0.1956 0.4136 0.104 Uiso 1 1 calc R . . C14 C 0.3029(6) 0.2189(3) 0.3170(5) 0.082(2) Uani 1 1 d . . . H14A H 0.3295 0.1880 0.3089 0.098 Uiso 1 1 calc R . . H14B H 0.2747 0.2304 0.2695 0.098 Uiso 1 1 calc R . . C15 C 0.3647(5) 0.2555(3) 0.3475(5) 0.084(2) Uani 1 1 d . . . H15A H 0.3991 0.2418 0.3905 0.101 Uiso 1 1 calc R . . H15B H 0.3990 0.2636 0.3105 0.101 Uiso 1 1 calc R . . O2 O 0.1767(3) 0.36638(15) 0.2664(2) 0.0560(11) Uani 1 1 d . . . C2 C 0.1420(4) 0.3707(3) 0.1992(4) 0.0576(17) Uani 1 1 d . . . N21 N 0.0974(4) 0.3341(2) 0.1683(3) 0.0680(16) Uani 1 1 d . . . N22 N 0.1545(4) 0.4099(2) 0.1594(3) 0.0742(18) Uani 1 1 d . . . C21 C 0.0897(6) 0.2885(3) 0.2093(5) 0.091(3) Uani 1 1 d . . . H21A H 0.1143 0.2928 0.2601 0.137 Uiso 1 1 calc R . . H21B H 0.1167 0.2623 0.1873 0.137 Uiso 1 1 calc R . . H21C H 0.0330 0.2805 0.2074 0.137 Uiso 1 1 calc R . . C22 C 0.2118(7) 0.4483(3) 0.1893(5) 0.107(3) Uani 1 1 d . . . H22A H 0.1822 0.4760 0.2042 0.160 Uiso 1 1 calc R . . H22B H 0.2435 0.4584 0.1520 0.160 Uiso 1 1 calc R . . H22C H 0.2475 0.4357 0.2316 0.160 Uiso 1 1 calc R . . C23 C 0.0636(7) 0.3340(4) 0.0890(5) 0.114(4) Uani 1 1 d . . . H23A H 0.1025 0.3192 0.0609 0.137 Uiso 1 1 calc R . . H23B H 0.0141 0.3145 0.0811 0.137 Uiso 1 1 calc R . . C24 C 0.1169(7) 0.4161(4) 0.0812(4) 0.101(3) Uani 1 1 d . . . H24A H 0.1002 0.4501 0.0726 0.122 Uiso 1 1 calc R . . H24B H 0.1567 0.4084 0.0490 0.122 Uiso 1 1 calc R . . C25 C 0.0458(7) 0.3837(5) 0.0628(6) 0.130(4) Uani 1 1 d . . . H25A H 0.0007 0.3967 0.0853 0.156 Uiso 1 1 calc R . . H25B H 0.0293 0.3833 0.0094 0.156 Uiso 1 1 calc R . . O3 O 0.0685(3) 0.42826(15) 0.3104(2) 0.0568(11) Uani 1 1 d . . . C3 C 0.0033(5) 0.4456(3) 0.3295(3) 0.0585(18) Uani 1 1 d . . . N31 N -0.0650(4) 0.4202(2) 0.3134(3) 0.0725(17) Uani 1 1 d . . . N32 N 0.0044(4) 0.4890(2) 0.3644(3) 0.0774(19) Uani 1 1 d . . . C31 C -0.0682(5) 0.3749(3) 0.2698(5) 0.089(3) Uani 1 1 d . . . H31A H -0.1002 0.3804 0.2220 0.134 Uiso 1 1 calc R . . H31B H -0.0927 0.3492 0.2951 0.134 Uiso 1 1 calc R . . H31C H -0.0140 0.3654 0.2635 0.134 Uiso 1 1 calc R . . C32 C 0.0761(6) 0.5198(3) 0.3725(5) 0.103(3) Uani 1 1 d . . . H32A H 0.1169 0.5064 0.4101 0.154 Uiso 1 1 calc R . . H32B H 0.0621 0.5525 0.3866 0.154 Uiso 1 1 calc R . . H32C H 0.0970 0.5212 0.3261 0.154 Uiso 1 1 calc R . . C33 C -0.1429(6) 0.4403(4) 0.3268(6) 0.109(3) Uani 1 1 d . . . H33A H -0.1793 0.4135 0.3349 0.131 Uiso 1 1 calc R . . H33B H -0.1677 0.4586 0.2835 0.131 Uiso 1 1 calc R . . C34 C -0.1319(8) 0.4726(5) 0.3912(7) 0.131(4) Uani 1 1 d . . . H34A H -0.1171 0.4529 0.4356 0.157 Uiso 1 1 calc R . . H34B H -0.1832 0.4888 0.3950 0.157 Uiso 1 1 calc R . . C35 C -0.0683(7) 0.5106(4) 0.3878(6) 0.111(3) Uani 1 1 d . . . H35A H -0.0896 0.5362 0.3530 0.134 Uiso 1 1 calc R . . H35B H -0.0538 0.5256 0.4363 0.134 Uiso 1 1 calc R . . O4 O 0.1227(3) 0.40813(15) 0.4532(2) 0.0518(11) Uani 1 1 d . . . C4 C 0.1341(4) 0.3890(2) 0.5176(4) 0.0584(18) Uani 1 1 d . . . N41 N 0.0734(4) 0.3609(2) 0.5381(3) 0.0696(17) Uani 1 1 d . . . N42 N 0.2003(4) 0.3964(2) 0.5647(3) 0.0726(17) Uani 1 1 d . . . C41 C -0.0020(5) 0.3536(3) 0.4877(5) 0.090(3) Uani 1 1 d . . . H41A H -0.0469 0.3654 0.5104 0.135 Uiso 1 1 calc R . . H41B H -0.0093 0.3191 0.4768 0.135 Uiso 1 1 calc R . . H41C H 0.0002 0.3714 0.4425 0.135 Uiso 1 1 calc R . . C42 C 0.2642(5) 0.4264(3) 0.5448(5) 0.088(3) Uani 1 1 d . . . H42A H 0.3027 0.4060 0.5246 0.133 Uiso 1 1 calc R . . H42B H 0.2911 0.4432 0.5880 0.133 Uiso 1 1 calc R . . H42C H 0.2417 0.4502 0.5083 0.133 Uiso 1 1 calc R . . C43 C 0.0794(7) 0.3418(4) 0.6133(6) 0.119(4) Uani 1 1 d . . . H43A H 0.0510 0.3641 0.6423 0.143 Uiso 1 1 calc R . . H43B H 0.0518 0.3102 0.6117 0.143 Uiso 1 1 calc R . . C44 C 0.2173(6) 0.3727(3) 0.6404(4) 0.090(3) Uani 1 1 d . . . H44A H 0.2712 0.3580 0.6470 0.108 Uiso 1 1 calc R . . H44B H 0.2166 0.3977 0.6783 0.108 Uiso 1 1 calc R . . C45 C 0.1587(7) 0.3359(4) 0.6490(6) 0.125(4) Uani 1 1 d . . . H45A H 0.1789 0.3049 0.6324 0.150 Uiso 1 1 calc R . . H45B H 0.1567 0.3325 0.7017 0.150 Uiso 1 1 calc R . . V2 V 0.66359(7) 0.40087(4) 0.87628(6) 0.0488(3) Uani 1 1 d . . . O20 O 0.7304(3) 0.44230(17) 0.8871(2) 0.0677(13) Uani 1 1 d . . . O5 O 0.5882(3) 0.41674(15) 0.7858(2) 0.0570(12) Uani 1 1 d . . . C5 C 0.5806(5) 0.4048(2) 0.7173(3) 0.0563(17) Uani 1 1 d . . . N51 N 0.5178(4) 0.3774(2) 0.6887(3) 0.0662(16) Uani 1 1 d . . . N52 N 0.6358(4) 0.4190(2) 0.6753(3) 0.0706(17) Uani 1 1 d . . . C51 C 0.4544(5) 0.3664(3) 0.7320(4) 0.086(3) Uani 1 1 d . . . H51A H 0.4777 0.3629 0.7832 0.129 Uiso 1 1 calc R . . H51B H 0.4278 0.3362 0.7146 0.129 Uiso 1 1 calc R . . H51C H 0.4152 0.3927 0.7270 0.129 Uiso 1 1 calc R . . C52 C 0.6986(7) 0.4532(4) 0.7023(5) 0.113(4) Uani 1 1 d . . . H52A H 0.7500 0.4364 0.7115 0.169 Uiso 1 1 calc R . . H52B H 0.6870 0.4677 0.7477 0.169 Uiso 1 1 calc R . . H52C H 0.7010 0.4786 0.6660 0.169 Uiso 1 1 calc R . . C53 C 0.5020(6) 0.3660(4) 0.6089(4) 0.100(3) Uani 1 1 d . . . H53A H 0.4671 0.3912 0.5831 0.120 Uiso 1 1 calc R . . H53B H 0.4738 0.3346 0.6014 0.120 Uiso 1 1 calc R . . C54 C 0.5790(8) 0.3635(4) 0.5776(5) 0.117(4) Uani 1 1 d . . . H54A H 0.6099 0.3349 0.5975 0.141 Uiso 1 1 calc R . . H54B H 0.5668 0.3598 0.5241 0.141 Uiso 1 1 calc R . . C55 C 0.6274(6) 0.4072(4) 0.5950(4) 0.097(3) Uani 1 1 d . . . H55A H 0.6019 0.4347 0.5665 0.116 Uiso 1 1 calc R . . H55B H 0.6810 0.4023 0.5812 0.116 Uiso 1 1 calc R . . O6 O 0.5754(3) 0.42496(16) 0.9305(2) 0.0566(11) Uani 1 1 d . . . C6 C 0.5070(5) 0.4458(3) 0.9120(3) 0.0568(17) Uani 1 1 d . . . N61 N 0.4392(4) 0.4211(2) 0.9169(3) 0.0632(15) Uani 1 1 d . . . N62 N 0.5030(4) 0.4928(2) 0.8890(3) 0.0698(17) Uani 1 1 d . . . C61 C 0.4453(5) 0.3717(3) 0.9487(4) 0.080(2) Uani 1 1 d . . . H61A H 0.5012 0.3646 0.9679 0.120 Uiso 1 1 calc R . . H61B H 0.4256 0.3481 0.9109 0.120 Uiso 1 1 calc R . . H61C H 0.4130 0.3698 0.9881 0.120 Uiso 1 1 calc R . . C62 C 0.5736(6) 0.5221(3) 0.8853(5) 0.099(3) Uani 1 1 d . . . H62A H 0.6212 0.5047 0.9081 0.149 Uiso 1 1 calc R . . H62B H 0.5691 0.5527 0.9109 0.149 Uiso 1 1 calc R . . H62C H 0.5779 0.5287 0.8342 0.149 Uiso 1 1 calc R . . C63 C 0.3579(5) 0.4420(4) 0.8960(6) 0.102(3) Uani 1 1 d . . . H63A H 0.3387 0.4554 0.9396 0.122 Uiso 1 1 calc R . . H63B H 0.3204 0.4163 0.8756 0.122 Uiso 1 1 calc R . . C64 C 0.3596(6) 0.4810(4) 0.8409(6) 0.113(3) Uani 1 1 d . . . H64A H 0.3072 0.4977 0.8324 0.136 Uiso 1 1 calc R . . H64B H 0.3696 0.4668 0.7942 0.136 Uiso 1 1 calc R . . C65 C 0.4246(6) 0.5170(3) 0.8674(5) 0.096(3) Uani 1 1 d . . . H65A H 0.4292 0.5406 0.8284 0.116 Uiso 1 1 calc R . . H65B H 0.4099 0.5348 0.9097 0.116 Uiso 1 1 calc R . . O7 O 0.6889(3) 0.35354(15) 0.9575(2) 0.0588(12) Uani 1 1 d . . . C7 C 0.6746(4) 0.3482(2) 1.0239(4) 0.0518(16) Uani 1 1 d . . . N71 N 0.6234(3) 0.3127(2) 1.0378(3) 0.0571(14) Uani 1 1 d . . . N72 N 0.7081(3) 0.3782(2) 1.0774(3) 0.0597(14) Uani 1 1 d . . . C71 C 0.5963(5) 0.2750(3) 0.9830(4) 0.070(2) Uani 1 1 d . . . H71A H 0.5949 0.2883 0.9340 0.106 Uiso 1 1 calc R . . H71B H 0.5427 0.2641 0.9892 0.106 Uiso 1 1 calc R . . H71C H 0.6333 0.2476 0.9896 0.106 Uiso 1 1 calc R . . C72 C 0.7743(5) 0.4105(3) 1.0647(4) 0.089(3) Uani 1 1 d . . . H72A H 0.7988 0.3983 1.0238 0.133 Uiso 1 1 calc R . . H72B H 0.8145 0.4115 1.1085 0.133 Uiso 1 1 calc R . . H72C H 0.7535 0.4431 1.0535 0.133 Uiso 1 1 calc R . . C73 C 0.6102(5) 0.3009(3) 1.1131(3) 0.0648(19) Uani 1 1 d . . . H73A H 0.6510 0.2776 1.1352 0.078 Uiso 1 1 calc R . . H73B H 0.5568 0.2860 1.1121 0.078 Uiso 1 1 calc R . . C74 C 0.6156(5) 0.3475(3) 1.1586(4) 0.070(2) Uani 1 1 d . . . H74A H 0.6104 0.3399 1.2097 0.084 Uiso 1 1 calc R . . H74B H 0.5721 0.3699 1.1390 0.084 Uiso 1 1 calc R . . C75 C 0.6975(5) 0.3708(3) 1.1548(4) 0.068(2) Uani 1 1 d . . . H75A H 0.7010 0.4023 1.1804 0.081 Uiso 1 1 calc R . . H75B H 0.7406 0.3498 1.1792 0.081 Uiso 1 1 calc R . . O8 O 0.7042(3) 0.34938(17) 0.8163(2) 0.0625(12) Uani 1 1 d . . . C8 C 0.7400(6) 0.3081(3) 0.8341(4) 0.073(2) Uani 1 1 d . . . N81 N 0.8183(5) 0.3068(3) 0.8606(4) 0.092(2) Uani 1 1 d . . . N82 N 0.6963(5) 0.2663(2) 0.8203(3) 0.0779(19) Uani 1 1 d . . . C81 C 0.6136(6) 0.2684(3) 0.7848(5) 0.093(3) Uani 1 1 d . . . H81A H 0.5888 0.2982 0.7989 0.139 Uiso 1 1 calc R . . H81B H 0.5843 0.2405 0.7997 0.139 Uiso 1 1 calc R . . H81C H 0.6120 0.2678 0.7319 0.139 Uiso 1 1 calc R . . C82 C 0.8652(6) 0.3509(4) 0.8690(6) 0.123(4) Uani 1 1 d . . . H82A H 0.9187 0.3445 0.8572 0.185 Uiso 1 1 calc R . . H82B H 0.8694 0.3623 0.9193 0.185 Uiso 1 1 calc R . . H82C H 0.8390 0.3756 0.8360 0.185 Uiso 1 1 calc R . . C83 C 0.7381(7) 0.2179(3) 0.8318(6) 0.114(4) Uani 1 1 d . . . H83A H 0.6999 0.1929 0.8429 0.136 Uiso 1 1 calc R . . H83B H 0.7592 0.2082 0.7871 0.136 Uiso 1 1 calc R . . C84 C 0.8049(9) 0.2224(4) 0.8936(6) 0.129(4) Uani 1 1 d . . . H84A H 0.8329 0.1910 0.9010 0.154 Uiso 1 1 calc R . . H84B H 0.7825 0.2300 0.9386 0.154 Uiso 1 1 calc R . . C85 C 0.8630(7) 0.2601(5) 0.8818(6) 0.121(4) Uani 1 1 d . . . H85A H 0.8931 0.2500 0.8426 0.146 Uiso 1 1 calc R . . H85B H 0.9015 0.2650 0.9268 0.146 Uiso 1 1 calc R . . S10 S 0.85493(16) 0.24824(10) 0.11665(15) 0.0963(8) Uani 1 1 d D . . O11 O 0.8659(7) 0.2729(4) 0.1834(5) 0.209(5) Uani 1 1 d D . . O12 O 0.7838(6) 0.2650(5) 0.0711(6) 0.225(6) Uani 1 1 d D . . O13 O 0.9211(4) 0.2442(2) 0.0765(3) 0.0957(18) Uani 1 1 d D . . C10 C 0.8343(11) 0.1879(7) 0.1417(10) 0.181(7) Uani 1 1 d D . . F11 F 0.8148(8) 0.1629(4) 0.0774(7) 0.258(7) Uani 1 1 d D . . F12 F 0.8943(8) 0.1661(5) 0.1756(9) 0.315(11) Uani 1 1 d D . . F13 F 0.7726(6) 0.1845(4) 0.1779(5) 0.212(4) Uani 1 1 d D . . S20 S 0.35675(19) 0.23716(9) 0.59215(15) 0.0971(8) Uani 1 1 d D . . O21 O 0.4038(4) 0.2303(2) 0.5369(3) 0.112(2) Uani 1 1 d D . . O22 O 0.2794(9) 0.2545(6) 0.5700(9) 0.315(10) Uani 1 1 d D . . O23 O 0.3977(9) 0.2600(4) 0.6541(5) 0.256(8) Uani 1 1 d D . . C20 C 0.3433(9) 0.1756(7) 0.6284(8) 0.158(6) Uani 1 1 d D . . F21 F 0.3027(5) 0.1790(3) 0.6861(4) 0.164(3) Uani 1 1 d D . . F22 F 0.4076(8) 0.1544(4) 0.6452(7) 0.250(6) Uani 1 1 d D . . F23 F 0.2966(8) 0.1531(4) 0.5739(6) 0.253(6) Uani 1 1 d D . . S30 S 0.6186(2) 0.42193(13) 0.36395(16) 0.1175(10) Uani 1 1 d D . . O31 O 0.6530(5) 0.4309(4) 0.3035(4) 0.169(4) Uani 1 1 d D . . O32 O 0.6717(6) 0.4380(5) 0.4323(4) 0.207(5) Uani 1 1 d D . . O33 O 0.5893(7) 0.3750(3) 0.3792(7) 0.217(5) Uani 1 1 d D . . C30 C 0.5344(10) 0.4610(6) 0.3694(10) 0.152(5) Uani 1 1 d D . . F31 F 0.4943(6) 0.4512(4) 0.4191(5) 0.205(4) Uani 1 1 d D . . F32 F 0.4822(7) 0.4493(6) 0.3071(7) 0.292(8) Uani 1 1 d D . . F33 F 0.5486(7) 0.5056(3) 0.3532(8) 0.259(6) Uani 1 1 d D . . S40 S 0.1108(3) 0.42528(19) 0.8403(2) 0.1532(16) Uani 1 1 d D . . O41 O 0.1602(7) 0.4392(7) 0.7982(7) 0.266(7) Uani 1 1 d D . . O42 O 0.0967(10) 0.3843(5) 0.8806(9) 0.257(7) Uani 1 1 d D . . O43 O 0.1706(11) 0.4321(16) 0.9087(11) 0.33(3) Uani 0.50 1 d PD . . O44 O 0.0526(16) 0.4094(7) 0.7740(8) 0.212(12) Uani 0.50 1 d PD . . C40 C 0.0489(13) 0.4710(6) 0.8666(8) 0.192(7) Uani 1 1 d DU . . F41 F 0.0450(9) 0.5091(3) 0.8309(6) 0.252(5) Uani 1 1 d DU . . F42 F 0.0016(7) 0.4589(4) 0.9074(6) 0.223(5) Uani 1 1 d DU . . F43 F 0.099(2) 0.4912(8) 0.9272(9) 0.298(15) Uani 0.50 1 d PDU . . F44 F -0.0201(14) 0.4613(11) 0.8052(12) 0.261(9) Uani 0.50 1 d PDU . . 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 0.0522(7) 0.0456(6) 0.0581(7) 0.0007(5) 0.0085(5) -0.0016(5) O10 0.062(3) 0.060(3) 0.077(3) -0.008(2) 0.009(2) -0.023(2) O1 0.065(3) 0.050(3) 0.065(3) 0.001(2) 0.010(2) 0.013(2) C1 0.059(5) 0.052(4) 0.058(4) 0.002(3) 0.005(3) 0.008(4) N11 0.085(5) 0.046(4) 0.078(4) 0.009(3) 0.021(3) 0.009(3) N12 0.063(4) 0.067(4) 0.071(4) 0.000(3) 0.004(3) 0.011(3) C11 0.097(7) 0.087(6) 0.125(7) 0.009(6) 0.048(6) -0.007(5) C12 0.057(6) 0.111(8) 0.139(8) -0.021(6) 0.008(5) -0.001(5) C13 0.117(8) 0.045(4) 0.099(6) 0.006(4) 0.019(6) 0.013(4) C14 0.095(7) 0.063(5) 0.087(6) -0.011(4) 0.011(5) 0.018(5) C15 0.079(6) 0.085(6) 0.090(6) -0.001(5) 0.018(5) 0.029(5) O2 0.063(3) 0.055(3) 0.051(3) -0.010(2) 0.010(2) -0.001(2) C2 0.065(5) 0.056(4) 0.053(4) -0.010(4) 0.013(3) 0.000(4) N21 0.086(5) 0.062(4) 0.052(3) -0.007(3) 0.000(3) -0.015(3) N22 0.097(5) 0.069(4) 0.058(4) 0.004(3) 0.014(3) -0.016(4) C21 0.119(8) 0.061(5) 0.087(6) -0.001(4) -0.008(5) -0.016(5) C22 0.148(9) 0.082(6) 0.090(6) 0.008(5) 0.017(6) -0.051(6) C23 0.151(10) 0.120(9) 0.065(5) -0.015(6) -0.002(6) -0.058(7) C24 0.131(9) 0.108(7) 0.061(5) 0.015(5) 0.000(5) -0.015(6) C25 0.142(10) 0.149(11) 0.088(7) 0.026(7) -0.016(7) -0.045(9) O3 0.063(3) 0.058(3) 0.048(2) 0.005(2) 0.004(2) 0.013(2) C3 0.067(5) 0.061(5) 0.045(4) 0.007(3) 0.000(3) 0.014(4) N31 0.056(4) 0.087(5) 0.074(4) 0.003(4) 0.009(3) 0.011(4) N32 0.098(6) 0.054(4) 0.078(4) -0.004(3) 0.004(4) 0.021(4) C31 0.085(6) 0.085(6) 0.096(6) -0.021(5) 0.008(5) -0.010(5) C32 0.127(9) 0.059(5) 0.116(7) -0.012(5) -0.001(6) -0.001(6) C33 0.075(7) 0.130(9) 0.127(8) -0.001(7) 0.030(6) 0.020(6) C34 0.123(10) 0.135(10) 0.143(10) -0.019(9) 0.051(8) 0.041(8) C35 0.126(9) 0.094(7) 0.118(8) -0.015(6) 0.032(7) 0.047(7) O4 0.058(3) 0.053(3) 0.045(2) 0.002(2) 0.006(2) 0.003(2) C4 0.064(5) 0.053(4) 0.058(4) -0.011(3) 0.007(4) 0.010(4) N41 0.072(4) 0.082(4) 0.056(3) 0.022(3) 0.010(3) -0.004(3) N42 0.059(4) 0.085(5) 0.070(4) -0.002(3) -0.002(3) 0.005(4) C41 0.056(5) 0.120(7) 0.092(6) 0.030(5) 0.005(4) -0.011(5) C42 0.067(6) 0.101(7) 0.095(6) -0.025(5) 0.005(5) -0.008(5) C43 0.121(9) 0.125(9) 0.106(7) 0.052(7) 0.003(7) -0.011(7) C44 0.103(7) 0.089(6) 0.069(5) 0.012(5) -0.019(5) 0.023(6) C45 0.115(9) 0.145(10) 0.108(8) 0.057(7) -0.010(7) -0.025(8) V2 0.0544(7) 0.0442(6) 0.0471(6) -0.0009(5) 0.0057(5) -0.0096(5) O20 0.068(3) 0.069(3) 0.064(3) 0.002(2) 0.005(2) -0.023(3) O5 0.071(3) 0.051(3) 0.047(3) 0.000(2) 0.001(2) -0.004(2) C5 0.078(5) 0.045(4) 0.044(4) 0.008(3) 0.005(3) -0.010(4) N51 0.069(4) 0.073(4) 0.055(3) -0.006(3) 0.004(3) -0.019(3) N52 0.084(5) 0.073(4) 0.053(3) 0.000(3) 0.003(3) -0.030(3) C51 0.055(5) 0.114(7) 0.089(6) -0.014(5) 0.010(4) -0.022(5) C52 0.149(10) 0.108(7) 0.083(6) 0.015(5) 0.022(6) -0.054(7) C53 0.107(8) 0.126(8) 0.063(5) -0.023(5) -0.001(5) -0.025(6) C54 0.181(12) 0.114(8) 0.060(5) -0.022(5) 0.029(6) -0.030(8) C55 0.110(7) 0.121(8) 0.063(5) -0.016(5) 0.028(5) -0.022(6) O6 0.062(3) 0.056(3) 0.052(3) 0.006(2) 0.009(2) 0.006(2) C6 0.074(5) 0.056(4) 0.041(4) -0.002(3) 0.011(3) 0.011(4) N61 0.054(4) 0.057(4) 0.080(4) 0.020(3) 0.013(3) 0.006(3) N62 0.080(5) 0.045(4) 0.086(4) 0.004(3) 0.018(3) 0.004(3) C61 0.088(6) 0.067(5) 0.086(5) 0.021(4) 0.016(4) -0.005(4) C62 0.131(9) 0.046(5) 0.117(7) 0.007(5) 0.007(6) -0.006(5) C63 0.073(6) 0.114(8) 0.118(7) 0.024(6) 0.010(5) 0.013(5) C64 0.093(8) 0.103(8) 0.137(9) 0.026(7) -0.004(6) 0.025(6) C65 0.107(8) 0.075(6) 0.106(7) 0.007(5) 0.011(6) 0.028(6) O7 0.071(3) 0.055(3) 0.051(3) 0.009(2) 0.011(2) 0.002(2) C7 0.049(4) 0.053(4) 0.052(4) 0.014(3) 0.003(3) 0.013(3) N71 0.067(4) 0.053(3) 0.050(3) 0.005(3) 0.005(3) 0.004(3) N72 0.058(4) 0.064(4) 0.055(3) 0.003(3) 0.004(3) -0.001(3) C71 0.083(6) 0.060(5) 0.068(4) 0.004(4) 0.013(4) -0.002(4) C72 0.082(6) 0.109(7) 0.068(5) -0.006(5) -0.011(4) -0.025(5) C73 0.076(5) 0.068(5) 0.054(4) 0.010(4) 0.021(4) 0.002(4) C74 0.075(5) 0.082(5) 0.056(4) 0.009(4) 0.019(4) 0.010(4) C75 0.081(6) 0.070(5) 0.048(4) -0.002(4) 0.000(4) 0.006(4) O8 0.070(3) 0.060(3) 0.058(3) -0.006(2) 0.012(2) 0.012(3) C8 0.087(7) 0.090(6) 0.044(4) -0.011(4) 0.011(4) 0.011(5) N81 0.075(5) 0.106(6) 0.092(5) -0.024(4) 0.006(4) 0.012(5) N82 0.106(6) 0.061(4) 0.066(4) -0.009(3) 0.014(4) 0.013(4) C81 0.098(7) 0.088(6) 0.088(6) -0.023(5) 0.001(5) -0.002(5) C82 0.065(6) 0.156(10) 0.149(9) -0.042(8) 0.019(6) -0.005(7) C83 0.166(11) 0.071(6) 0.099(7) -0.002(5) 0.005(7) 0.034(6) C84 0.172(13) 0.111(9) 0.098(8) 0.006(7) 0.004(8) 0.071(9) C85 0.116(10) 0.133(10) 0.110(8) 0.006(8) 0.001(7) 0.049(8) S10 0.0852(17) 0.0994(19) 0.1056(18) -0.0164(15) 0.0190(14) 0.0200(14) O11 0.248(12) 0.219(10) 0.175(8) -0.111(8) 0.087(8) -0.072(9) O12 0.129(8) 0.368(16) 0.181(9) 0.061(10) 0.031(6) 0.118(9) O13 0.093(4) 0.090(4) 0.108(4) -0.006(3) 0.028(4) -0.009(3) C10 0.162(16) 0.24(2) 0.170(14) -0.050(15) 0.106(13) -0.050(14) F11 0.395(18) 0.173(8) 0.252(11) -0.081(9) 0.192(12) -0.141(10) F12 0.239(14) 0.330(16) 0.41(2) 0.274(17) 0.166(13) 0.148(12) F13 0.220(9) 0.255(10) 0.193(7) -0.018(7) 0.140(7) -0.079(8) S20 0.129(2) 0.0744(15) 0.0950(17) -0.0094(13) 0.0394(16) 0.0146(15) O21 0.134(6) 0.122(5) 0.092(4) 0.008(4) 0.050(4) -0.004(4) O22 0.265(15) 0.38(2) 0.329(17) 0.135(16) 0.143(13) 0.231(16) O23 0.44(2) 0.198(10) 0.155(8) -0.107(8) 0.136(11) -0.188(12) C20 0.113(11) 0.25(2) 0.119(10) -0.015(12) 0.052(9) -0.076(12) F21 0.173(7) 0.191(7) 0.150(5) -0.018(5) 0.096(5) -0.068(5) F22 0.218(11) 0.236(11) 0.322(14) 0.168(10) 0.125(11) 0.070(9) F23 0.286(13) 0.259(11) 0.241(10) -0.111(9) 0.131(10) -0.170(10) S30 0.126(2) 0.142(3) 0.0923(19) 0.0002(18) 0.0419(17) 0.017(2) O31 0.129(7) 0.288(12) 0.101(5) 0.029(6) 0.052(5) 0.036(7) O32 0.155(8) 0.365(16) 0.093(6) -0.001(7) -0.005(5) -0.022(9) O33 0.249(13) 0.101(6) 0.322(15) 0.044(8) 0.108(11) 0.021(7) C30 0.160(14) 0.134(12) 0.171(14) 0.044(11) 0.059(12) 0.043(10) F31 0.176(8) 0.291(11) 0.171(7) 0.023(7) 0.098(6) 0.053(8) F32 0.182(10) 0.46(2) 0.212(11) 0.110(12) -0.035(8) -0.012(12) F33 0.246(12) 0.095(6) 0.434(18) 0.015(9) 0.053(11) 0.037(7) S40 0.147(3) 0.193(4) 0.132(3) 0.032(3) 0.061(3) 0.054(3) O41 0.152(10) 0.47(2) 0.184(10) 0.030(13) 0.069(9) -0.021(13) O42 0.316(19) 0.187(11) 0.286(16) 0.072(11) 0.104(15) 0.119(12) O43 0.075(12) 0.79(8) 0.119(16) 0.14(3) 0.018(11) 0.02(2) O44 0.38(4) 0.168(17) 0.081(10) -0.062(11) 0.007(15) -0.066(19) C40 0.31(2) 0.169(13) 0.104(10) 0.080(10) 0.067(12) 0.044(14) F41 0.430(17) 0.138(7) 0.193(9) 0.067(7) 0.060(10) 0.056(9) F42 0.237(11) 0.258(11) 0.202(9) 0.093(9) 0.123(8) 0.104(9) F43 0.56(4) 0.25(2) 0.081(10) -0.016(12) 0.033(18) -0.21(3) F44 0.26(2) 0.31(2) 0.194(17) 0.081(18) -0.023(15) 0.036(19) _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 O10 1.577(4) . ? V1 O1 1.959(4) . ? V1 O2 1.963(4) . ? V1 O3 1.975(4) . ? V1 O4 1.983(4) . ? O1 C1 1.286(7) . ? C1 N12 1.323(9) . ? C1 N11 1.334(9) . ? N11 C11 1.453(10) . ? N11 C13 1.455(9) . ? N12 C12 1.452(10) . ? N12 C15 1.471(9) . ? C13 C14 1.475(12) . ? C14 C15 1.475(11) . ? O2 C2 1.277(7) . ? C2 N21 1.313(8) . ? C2 N22 1.323(8) . ? N21 C21 1.460(9) . ? N21 C23 1.469(9) . ? N22 C22 1.459(10) . ? N22 C24 1.476(9) . ? C23 C25 1.446(13) . ? C24 C25 1.468(13) . ? O3 C3 1.275(8) . ? C3 N31 1.320(9) . ? C3 N32 1.337(9) . ? N31 C33 1.457(10) . ? N31 C31 1.460(9) . ? N32 C32 1.445(11) . ? N32 C35 1.461(11) . ? C33 C34 1.453(13) . ? C34 C35 1.484(15) . ? O4 C4 1.272(7) . ? C4 N42 1.303(9) . ? C4 N41 1.360(9) . ? N41 C41 1.449(9) . ? N41 C43 1.455(10) . ? N42 C42 1.426(10) . ? N42 C44 1.508(9) . ? C43 C45 1.387(13) . ? C44 C45 1.419(12) . ? V2 O20 1.570(4) . ? V2 O8 1.955(5) . ? V2 O7 1.956(4) . ? V2 O5 1.961(4) . ? V2 O6 1.995(5) . ? O5 C5 1.277(7) . ? C5 N51 1.322(8) . ? C5 N52 1.336(9) . ? N51 C51 1.438(9) . ? N51 C53 1.470(9) . ? N52 C52 1.425(10) . ? N52 C55 1.482(9) . ? C53 C54 1.475(13) . ? C54 C55 1.440(12) . ? O6 C6 1.267(8) . ? C6 N61 1.324(9) . ? C6 N62 1.341(8) . ? N61 C63 1.460(10) . ? N61 C61 1.459(8) . ? N62 C62 1.426(10) . ? N62 C65 1.456(10) . ? C63 C64 1.462(12) . ? C64 C65 1.480(13) . ? O7 C7 1.275(7) . ? C7 N72 1.327(8) . ? C7 N71 1.334(8) . ? N71 C71 1.452(8) . ? N71 C73 1.458(8) . ? N72 C72 1.450(9) . ? N72 C75 1.461(8) . ? C73 C74 1.505(10) . ? C74 C75 1.510(10) . ? O8 C8 1.286(9) . ? C8 N81 1.317(10) . ? C8 N82 1.349(10) . ? N81 C82 1.423(12) . ? N81 C85 1.489(12) . ? N82 C81 1.428(10) . ? N82 C83 1.485(10) . ? C83 C84 1.461(14) . ? C84 C85 1.443(15) . ? S10 O11 1.376(8) . ? S10 O13 1.411(6) . ? S10 O12 1.411(8) . ? S10 C10 1.749(19) . ? C10 F12 1.24(2) . ? C10 F13 1.301(13) . ? C10 F11 1.350(16) . ? S20 O23 1.374(9) . ? S20 O21 1.376(6) . ? S20 O22 1.369(12) . ? S20 C20 1.822(17) . ? C20 F22 1.211(16) . ? C20 F23 1.314(14) . ? C20 F21 1.335(13) . ? S30 O31 1.336(7) . ? S30 O33 1.405(9) . ? S30 O32 1.478(8) . ? S30 C30 1.769(14) . ? C30 F31 1.229(14) . ? C30 F33 1.278(15) . ? C30 F32 1.358(18) . ? S40 O41 1.261(11) . ? S40 O42 1.371(13) . ? S40 O43 1.48(2) . ? S40 O44 1.491(17) . ? S40 C40 1.724(18) . ? O42 O43 1.81(3) . ? C40 F42 1.205(17) . ? C40 F41 1.217(14) . ? C40 F43 1.39(2) . ? C40 F44 1.50(3) . ? F41 F44 1.71(2) . ? 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 O10 V1 O1 109.5(2) . . ? O10 V1 O2 105.1(2) . . ? O1 V1 O2 86.12(19) . . ? O10 V1 O3 108.3(2) . . ? O1 V1 O3 142.1(2) . . ? O2 V1 O3 85.30(18) . . ? O10 V1 O4 104.2(2) . . ? O1 V1 O4 84.62(18) . . ? O2 V1 O4 150.71(19) . . ? O3 V1 O4 85.13(18) . . ? C1 O1 V1 136.6(4) . . ? O1 C1 N12 120.1(7) . . ? O1 C1 N11 119.0(7) . . ? N12 C1 N11 120.9(6) . . ? C1 N11 C11 120.3(6) . . ? C1 N11 C13 121.2(7) . . ? C11 N11 C13 117.4(6) . . ? C1 N12 C12 119.8(6) . . ? C1 N12 C15 122.4(7) . . ? C12 N12 C15 117.4(7) . . ? N11 C13 C14 110.3(6) . . ? C15 C14 C13 110.7(7) . . ? N12 C15 C14 109.7(7) . . ? C2 O2 V1 136.7(4) . . ? O2 C2 N21 119.1(7) . . ? O2 C2 N22 120.9(6) . . ? N21 C2 N22 119.9(6) . . ? C2 N21 C21 120.6(6) . . ? C2 N21 C23 121.9(7) . . ? C21 N21 C23 116.9(6) . . ? C2 N22 C22 121.1(6) . . ? C2 N22 C24 122.8(7) . . ? C22 N22 C24 116.0(7) . . ? C25 C23 N21 110.6(8) . . ? C25 C24 N22 111.2(8) . . ? C23 C25 C24 111.4(10) . . ? C3 O3 V1 136.6(4) . . ? O3 C3 N31 118.8(7) . . ? O3 C3 N32 120.2(7) . . ? N31 C3 N32 121.0(7) . . ? C3 N31 C33 121.4(8) . . ? C3 N31 C31 121.3(7) . . ? C33 N31 C31 116.4(7) . . ? C3 N32 C32 120.8(7) . . ? C3 N32 C35 122.7(8) . . ? C32 N32 C35 116.1(8) . . ? N31 C33 C34 110.7(8) . . ? C33 C34 C35 112.9(10) . . ? N32 C35 C34 110.9(8) . . ? C4 O4 V1 135.4(4) . . ? O4 C4 N42 122.6(7) . . ? O4 C4 N41 117.9(6) . . ? N42 C4 N41 119.5(7) . . ? C4 N41 C41 120.5(6) . . ? C4 N41 C43 120.6(7) . . ? C41 N41 C43 118.6(7) . . ? C4 N42 C42 120.3(7) . . ? C4 N42 C44 123.9(7) . . ? C42 N42 C44 115.6(7) . . ? C45 C43 N41 114.1(9) . . ? C45 C44 N42 111.4(7) . . ? C43 C45 C44 118.9(9) . . ? O20 V2 O8 106.6(2) . . ? O20 V2 O7 108.0(2) . . ? O8 V2 O7 84.27(19) . . ? O20 V2 O5 107.3(2) . . ? O8 V2 O5 85.23(19) . . ? O7 V2 O5 144.76(19) . . ? O20 V2 O6 105.1(2) . . ? O8 V2 O6 148.3(2) . . ? O7 V2 O6 86.02(18) . . ? O5 V2 O6 85.54(19) . . ? C5 O5 V2 136.2(5) . . ? O5 C5 N51 119.0(6) . . ? O5 C5 N52 120.6(6) . . ? N51 C5 N52 120.4(6) . . ? C5 N51 C51 119.9(6) . . ? C5 N51 C53 121.3(7) . . ? C51 N51 C53 117.6(6) . . ? C5 N52 C52 121.3(6) . . ? C5 N52 C55 122.0(6) . . ? C52 N52 C55 115.9(7) . . ? N51 C53 C54 110.8(7) . . ? C55 C54 C53 111.4(9) . . ? C54 C55 N52 111.2(7) . . ? C6 O6 V2 135.1(4) . . ? O6 C6 N61 119.4(6) . . ? O6 C6 N62 120.6(7) . . ? N61 C6 N62 119.9(7) . . ? C6 N61 C63 123.2(6) . . ? C6 N61 C61 119.0(6) . . ? C63 N61 C61 117.8(7) . . ? C6 N62 C62 122.8(7) . . ? C6 N62 C65 120.9(7) . . ? C62 N62 C65 116.3(7) . . ? N61 C63 C64 110.4(8) . . ? C63 C64 C65 109.9(9) . . ? N62 C65 C64 111.7(7) . . ? C7 O7 V2 137.9(4) . . ? O7 C7 N72 120.6(6) . . ? O7 C7 N71 118.5(6) . . ? N72 C7 N71 120.9(6) . . ? C7 N71 C71 121.2(6) . . ? C7 N71 C73 121.8(6) . . ? C71 N71 C73 114.7(6) . . ? C7 N72 C72 119.9(6) . . ? C7 N72 C75 121.7(6) . . ? C72 N72 C75 116.1(6) . . ? N71 C73 C74 109.2(6) . . ? C73 C74 C75 107.9(6) . . ? N72 C75 C74 110.0(6) . . ? C8 O8 V2 131.8(4) . . ? O8 C8 N81 120.6(9) . . ? O8 C8 N82 118.1(8) . . ? N81 C8 N82 121.2(8) . . ? C8 N81 C82 120.6(8) . . ? C8 N81 C85 122.9(9) . . ? C82 N81 C85 116.5(9) . . ? C8 N82 C81 120.3(7) . . ? C8 N82 C83 119.4(8) . . ? C81 N82 C83 119.7(8) . . ? C84 C83 N82 108.6(8) . . ? C83 C84 C85 112.9(10) . . ? C84 C85 N81 108.9(10) . . ? O11 S10 O13 119.1(5) . . ? O11 S10 O12 110.5(7) . . ? O13 S10 O12 111.5(5) . . ? O11 S10 C10 103.3(8) . . ? O13 S10 C10 105.2(6) . . ? O12 S10 C10 106.0(9) . . ? F12 C10 F13 110.4(17) . . ? F12 C10 F11 105.2(17) . . ? F13 C10 F11 107.5(14) . . ? F12 C10 S10 113.7(14) . . ? F13 C10 S10 113.5(14) . . ? F11 C10 S10 105.8(12) . . ? O23 S20 O21 113.4(6) . . ? O23 S20 O22 114.4(9) . . ? O21 S20 O22 116.1(7) . . ? O23 S20 C20 100.8(7) . . ? O21 S20 C20 104.8(6) . . ? O22 S20 C20 105.2(9) . . ? F22 C20 F23 111.5(17) . . ? F22 C20 F21 111.3(14) . . ? F23 C20 F21 108.5(11) . . ? F22 C20 S20 112.2(10) . . ? F23 C20 S20 104.1(11) . . ? F21 C20 S20 109.0(12) . . ? O31 S30 O33 122.1(7) . . ? O31 S30 O32 111.5(6) . . ? O33 S30 O32 106.3(7) . . ? O31 S30 C30 112.1(7) . . ? O33 S30 C30 103.3(7) . . ? O32 S30 C30 98.7(8) . . ? F31 C30 F33 120.9(16) . . ? F31 C30 F32 102.6(15) . . ? F33 C30 F32 98.3(13) . . ? F31 C30 S30 115.6(11) . . ? F33 C30 S30 112.3(12) . . ? F32 C30 S30 102.9(12) . . ? O41 S40 O42 138.3(10) . . ? O41 S40 O43 93.5(11) . . ? O42 S40 O43 78.4(13) . . ? O41 S40 O44 89.6(10) . . ? O42 S40 O44 93.3(11) . . ? O43 S40 O44 170.4(18) . . ? O41 S40 C40 115.0(10) . . ? O42 S40 C40 106.1(8) . . ? O43 S40 C40 91.6(15) . . ? O44 S40 C40 95.3(12) . . ? S40 O42 O43 53.6(9) . . ? S40 O43 O42 48.1(10) . . ? F42 C40 F41 125.1(18) . . ? F42 C40 F43 89.0(14) . . ? F41 C40 F43 93.8(18) . . ? F42 C40 F44 85.2(19) . . ? F41 C40 F44 77.2(13) . . ? F43 C40 F44 164(2) . . ? F42 C40 S40 116.4(12) . . ? F41 C40 S40 116.6(13) . . ? F43 C40 S40 101.3(19) . . ? F44 C40 S40 94.9(15) . . ? C40 F41 F44 58.8(11) . . ? C40 F44 F41 44.0(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.724 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.080 #===END