# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Vacac2(CH3CN)2BF4 _database_code_depnum_ccdc_archive 'CCDC 868968' #TrackingRef '9789_web_deposit_cif_file_0_JuliaKohl_1330082360.Kohl_Vacac2(CH3CN)2BF4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic 'bis(acetonitrile)bis(acetylacetonato)vanadium(III) tetrafluoroborate' _chemical_name_common 'bis(acetonitrile)bis(acetylacetonato)vanadium(III) tetrafluoroborate' _chemical_formula_moiety 'C14 H20 N2 O4 V 1+, B F4 1-' _chemical_formula_sum 'C14 H20 B F4 N2 O4 V' _chemical_properties_physical 'air-sensitive, moisture-sensitive' _exptl_crystal_recrystallization_method 'diffusion: acetonitrile, diethyl ether, r. t., six weeks' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _diffrn_ambient_temperature 150(2) _chemical_formula_weight 418.07 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' B B 0.0013 0.0007 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.9556(10) _cell_length_b 5.7003(4) _cell_length_c 15.8568(19) _cell_angle_alpha 90.00 _cell_angle_beta 119.774(7) _cell_angle_gamma 90.00 _cell_volume 937.99(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1444 _cell_measurement_theta_min 3.4334 _cell_measurement_theta_max 32.5296 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 428 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80760 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.3031 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3866 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1832 _reflns_number_gt 1372 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _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^ > 2\s(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. The tetrafluoroborate moiety is disordered over an inversion center and has been treated with PART -1. The positional disorder was not further resolved resulting in somewhat higher displacement parameters. ; _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^)+(0.0570P)^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_extinction_coef ? _refine_ls_number_reflns 1832 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt 0.1044 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 0.0000 0.5000 1.0000 0.0194(2) Uani 1 2 d S . . O1 O -0.01892(18) 0.3144(3) 0.88997(13) 0.0239(4) Uani 1 1 d . . . O2 O -0.15923(18) 0.6633(3) 0.90824(13) 0.0233(4) Uani 1 1 d . . . N1 N 0.1132(2) 0.7468(4) 0.97843(16) 0.0245(5) Uani 1 1 d . . . C1 C -0.1174(3) 0.0650(5) 0.7532(2) 0.0347(8) Uani 1 1 d . . . H1A H -0.0508 0.1005 0.7362 0.052 Uiso 1 1 calc R . . H1B H -0.2007 0.0465 0.6937 0.052 Uiso 1 1 calc R . . H1C H -0.0953 -0.0808 0.7909 0.052 Uiso 1 1 calc R . . C2 C -0.1256(3) 0.2619(4) 0.8126(2) 0.0257(6) Uani 1 1 d . . . C3 C -0.2405(3) 0.3799(5) 0.78310(19) 0.0277(7) Uani 1 1 d . . . H3 H -0.3159 0.3212 0.7283 0.033 Uiso 1 1 calc R . . C4 C -0.2520(3) 0.5792(5) 0.8290(2) 0.0257(6) Uani 1 1 d . . . C5 C -0.3761(3) 0.7133(5) 0.7864(2) 0.0395(8) Uani 1 1 d . . . H5A H -0.4253 0.6636 0.8177 0.059 Uiso 1 1 calc R . . H5B H -0.4266 0.6825 0.7165 0.059 Uiso 1 1 calc R . . H5C H -0.3576 0.8815 0.7974 0.059 Uiso 1 1 calc R . . C6 C 0.1788(3) 0.8772(5) 0.96998(19) 0.0241(6) Uani 1 1 d . . . C7 C 0.2612(3) 1.0422(5) 0.9571(2) 0.0351(7) Uani 1 1 d . . . H7A H 0.3512 0.9915 0.9957 0.053 Uiso 1 1 calc R . . H7B H 0.2515 1.1982 0.9786 0.053 Uiso 1 1 calc R . . H7C H 0.2368 1.0484 0.8883 0.053 Uiso 1 1 calc R . . B10 B 0.5000 0.5000 1.0000 0.0438(13) Uani 1 2 d S . . F10 F 0.4753(4) 0.6858(7) 0.9319(3) 0.0587(12) Uani 0.50 1 d P A -1 F11 F 0.4021(6) 0.5341(7) 1.0233(5) 0.0804(16) Uani 0.50 1 d P A -1 F12 F 0.4579(5) 0.2984(8) 0.9372(4) 0.0738(15) Uani 0.50 1 d P A -1 F13 F 0.6120(6) 0.4981(12) 1.0647(5) 0.120(3) Uani 0.50 1 d P A -1 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 0.0183(3) 0.0209(3) 0.0192(3) -0.0006(3) 0.0094(3) -0.0030(3) O1 0.0239(11) 0.0252(10) 0.0227(10) -0.0014(7) 0.0117(9) -0.0023(8) O2 0.0194(10) 0.0239(9) 0.0241(10) 0.0015(7) 0.0090(9) -0.0005(8) N1 0.0246(13) 0.0249(12) 0.0246(13) -0.0015(9) 0.0126(11) -0.0029(10) C1 0.045(2) 0.0341(16) 0.0271(16) -0.0045(12) 0.0195(16) -0.0052(14) C2 0.0331(17) 0.0257(14) 0.0203(14) 0.0012(11) 0.0147(13) -0.0081(12) C3 0.0236(16) 0.0343(16) 0.0215(14) -0.0020(12) 0.0083(13) -0.0078(13) C4 0.0205(15) 0.0302(14) 0.0257(15) 0.0054(12) 0.0111(13) -0.0046(11) C5 0.0268(17) 0.0444(18) 0.0393(19) 0.0067(14) 0.0103(16) 0.0056(14) C6 0.0221(15) 0.0250(15) 0.0257(15) -0.0019(11) 0.0123(13) -0.0014(12) C7 0.0384(18) 0.0299(17) 0.0486(19) -0.0024(13) 0.0305(17) -0.0090(13) B10 0.029(3) 0.041(3) 0.056(3) 0.003(3) 0.016(3) -0.014(3) F10 0.033(2) 0.074(3) 0.049(3) 0.032(2) 0.005(2) -0.008(2) F11 0.125(5) 0.048(3) 0.124(5) -0.011(3) 0.104(4) -0.016(3) F12 0.102(4) 0.052(3) 0.106(4) -0.028(3) 0.080(4) -0.035(3) F13 0.066(4) 0.118(5) 0.094(4) 0.052(4) -0.023(4) -0.018(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.9551(17) . ? V1 O2 1.9638(18) . ? V1 N1 2.095(2) . ? O1 C2 1.291(3) . ? O2 C4 1.286(3) . ? N1 C6 1.136(3) . ? C1 C2 1.500(4) . ? C2 C3 1.386(4) . ? C3 C4 1.392(4) . ? C4 C5 1.500(4) . ? C6 C7 1.448(4) . ? B10 F13 1.217(5) . ? B10 F11 1.405(5) . ? B10 F10 1.434(4) . ? B10 F12 1.438(4) . ? 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 O2 87.43(7) . . ? O1 V1 N1 90.89(8) . . ? O2 V1 N1 91.59(8) . . ? C2 O1 V1 126.53(17) . . ? C6 N1 V1 177.2(2) . . ? O1 C2 C3 123.7(2) . . ? O1 C2 C1 115.4(3) . . ? C3 C2 C1 120.9(3) . . ? C2 C3 C4 123.9(3) . . ? O2 C4 C3 123.6(3) . . ? O2 C4 C5 115.5(2) . . ? N1 C6 C7 178.8(3) . . ? F13 B10 F11 119.3(4) . . ? F13 B10 F10 111.8(3) . . ? F11 B10 F10 102.0(3) . . ? F13 B10 F12 115.9(4) . . ? F11 B10 F12 104.0(3) . . ? F10 B10 F12 101.4(3) . . ? 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 O2 V1 O1 C2 -28.7(2) . . . . ? O2 V1 O1 C2 151.3(2) 3_567 . . . ? N1 V1 O1 C2 59.7(2) 3_567 . . . ? N1 V1 O1 C2 -120.3(2) . . . . ? O1 V1 O2 C4 -152.0(2) 3_567 . . . ? O1 V1 O2 C4 28.0(2) . . . . ? N1 V1 O2 C4 -61.1(2) 3_567 . . . ? N1 V1 O2 C4 118.9(2) . . . . ? V1 O1 C2 C3 18.3(4) . . . . ? V1 O1 C2 C1 -163.44(17) . . . . ? O1 C2 C3 C4 5.2(4) . . . . ? C1 C2 C3 C4 -173.0(2) . . . . ? V1 O2 C4 C3 -16.9(4) . . . . ? V1 O2 C4 C5 164.16(19) . . . . ? C2 C3 C4 O2 -5.9(4) . . . . ? C2 C3 C4 C5 173.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.529 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.066