#------------------------------------------------------------------------------ #$Date: 2014-07-12 07:06:18 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/56/7015604.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7015604 loop_ _publ_author_name 'Aidoudi, Farida H.' 'Byrne, Peter J.' 'Allan, Pheobe K.' 'Teat, Simon J.' 'Lightfoot, Philip' 'Morris, Russell E.' _publ_section_title ; Ionic liquids and deep eutectic mixtures as new solvents for the synthesis of vanadium fluorides and oxyfluorides. ; _journal_issue 16 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 4324 _journal_page_last 4331 _journal_volume 40 _journal_year 2011 _chemical_formula_moiety 'F4 O V, C2 H10 N2' _chemical_formula_sum 'C2 H10 F4 N2 O V' _chemical_formula_weight 205.06 _chemical_name_systematic ; ? ; _space_group_IT_number 130 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4a 2ac' _symmetry_space_group_name_H-M 'P 4/n c c :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 12.7330(5) _cell_length_b 12.7330(5) _cell_length_c 8.0300(4) _cell_measurement_reflns_used 3243 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 29.0 _cell_measurement_theta_min 3.2 _cell_volume 1301.90(10) _computing_cell_refinement 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_data_collection 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 93(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_radiation_monochromator confocal _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 7372 _diffrn_reflns_theta_full 25.30 _diffrn_reflns_theta_max 25.30 _diffrn_reflns_theta_min 2.26 _exptl_absorpt_coefficient_mu 1.540 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 824 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.574 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.106 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.263 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 50 _refine_ls_number_reflns 595 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.263 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0541 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+7.0095P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1305 _refine_ls_wR_factor_ref 0.1354 _reflns_number_gt 491 _reflns_number_total 595 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0dt01765e.txt _[local]_cod_data_source_block vilm181 _[local]_cod_cif_authors_sg_H-M 'P 4/n c c' _cod_database_code 7015604 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z' '-x+1/2, y, z+1/2' 'y, x, z+1/2' 'x, -y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'y-1/2, -x, -z' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z' 'x-1/2, -y, -z-1/2' '-y, -x, -z-1/2' '-x, y-1/2, -z-1/2' 'y-1/2, x-1/2, -z-1/2' 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 V2 V -0.2500 0.2500 0.2879(3) 0.0114(9) Uani 0.50 2 d SP . . F2 F -0.3981(2) 0.2493(2) 0.2490(3) 0.0203(8) Uani 1 1 d . . . O2 O -0.2500 0.2500 0.0000 0.0209(18) Uani 1 4 d S . . C1 C -0.0417(4) 0.4576(4) 0.5092(6) 0.0179(12) Uani 1 1 d . . . H1A H -0.0389 0.4106 0.4142 0.021 Uiso 1 1 calc R . . H1B H -0.0282 0.4167 0.6089 0.021 Uiso 1 1 calc R . . N1 N -0.1480(3) 0.5063(3) 0.5201(5) 0.0184(10) Uani 1 1 d . . . H1C H -0.1961 0.4562 0.5322 0.028 Uiso 1 1 calc R . . H1D H -0.1610 0.5423 0.4273 0.028 Uiso 1 1 calc R . . H1E H -0.1504 0.5494 0.6072 0.028 Uiso 1 1 calc R . . V1 V 0.2500 0.2500 0.23162(19) 0.0112(5) Uani 1 4 d S . . F1 F 0.1211(2) 0.3229(2) 0.2753(3) 0.0203(7) Uani 1 1 d . . . O1 O 0.2500 0.2500 0.0290(8) 0.0148(15) Uani 1 4 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 V2 0.0121(13) 0.0120(13) 0.010(3) 0.000 0.000 -0.0004(8) F2 0.0132(15) 0.0279(18) 0.0198(15) -0.0058(13) 0.0004(11) 0.0006(14) O2 0.022(2) 0.022(2) 0.018(4) 0.000 0.000 0.000 C1 0.014(3) 0.019(3) 0.020(3) 0.000(2) 0.001(2) 0.002(2) N1 0.019(3) 0.019(3) 0.017(2) 0.0016(17) 0.0008(18) 0.0019(19) V1 0.0123(6) 0.0123(6) 0.0089(8) 0.000 0.000 0.000 F1 0.0185(16) 0.0244(17) 0.0181(15) -0.0032(13) -0.0022(12) 0.0031(12) O1 0.017(2) 0.017(2) 0.011(3) 0.000 0.000 0.000 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' 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' 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 V2 V2 O2 180.0 14_556 5_455 ? V2 V2 F2 81.07(10) 14_556 16_566 ? O2 V2 F2 98.93(10) 5_455 16_566 ? V2 V2 F2 81.07(10) 14_556 14_556 ? O2 V2 F2 98.93(10) 5_455 14_556 ? F2 V2 F2 162.1(2) 16_566 14_556 ? V2 V2 F2 80.59(10) 14_556 . ? O2 V2 F2 99.41(10) 5_455 . ? F2 V2 F2 88.03(18) 16_566 . ? F2 V2 F2 89.06(18) 14_556 . ? V2 V2 F2 80.59(10) 14_556 3_455 ? O2 V2 F2 99.41(10) 5_455 3_455 ? F2 V2 F2 89.06(18) 16_566 3_455 ? F2 V2 F2 88.03(18) 14_556 3_455 ? F2 V2 F2 161.2(2) . 3_455 ? V2 V2 O2 0.0 14_556 . ? O2 V2 O2 180.0 5_455 . ? F2 V2 O2 81.07(10) 16_566 . ? F2 V2 O2 81.07(10) 14_556 . ? F2 V2 O2 80.59(10) . . ? F2 V2 O2 80.59(10) 3_455 . ? V2 F2 V2 18.34(12) 14_556 . ? V2 O2 V2 180.0 14_556 5_454 ? V2 O2 V2 0.0 14_556 . ? V2 O2 V2 180.0 5_454 . ? V2 O2 V2 180.0 14_556 10 ? V2 O2 V2 0.0 5_454 10 ? V2 O2 V2 180.0 . 10 ? N1 C1 C1 110.1(6) . 9_566 ? N1 C1 H1A 109.6 . . ? C1 C1 H1A 109.6 9_566 . ? N1 C1 H1B 109.6 . . ? C1 C1 H1B 109.6 9_566 . ? H1A C1 H1B 108.1 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? O1 V1 F1 100.55(9) . 4 ? O1 V1 F1 100.55(9) . 3 ? F1 V1 F1 88.08(3) 4 3 ? O1 V1 F1 100.55(9) . 2 ? F1 V1 F1 158.91(18) 4 2 ? F1 V1 F1 88.08(3) 3 2 ? O1 V1 F1 100.55(9) . . ? F1 V1 F1 88.08(3) 4 . ? F1 V1 F1 158.91(18) 3 . ? F1 V1 F1 88.08(3) 2 . ? O1 V1 O1 180.000(1) . 5 ? F1 V1 O1 79.45(9) 4 5 ? F1 V1 O1 79.45(9) 3 5 ? F1 V1 O1 79.45(9) 2 5 ? F1 V1 O1 79.45(9) . 5 ? V1 O1 V1 180.0 . 5_554 ? 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 V2 V2 0.609(4) 14_556 ? V2 O2 1.703(2) 5_455 ? V2 F2 1.909(3) 16_566 ? V2 F2 1.909(3) 14_556 ? V2 F2 1.912(3) . ? V2 F2 1.912(3) 3_455 ? V2 O2 2.312(2) . ? F2 V2 1.909(3) 14_556 ? O2 V2 1.703(2) 14_556 ? O2 V2 1.703(2) 5_454 ? O2 V2 2.312(2) 10 ? C1 N1 1.491(7) . ? C1 C1 1.523(10) 9_566 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? V1 O1 1.627(6) . ? V1 F1 1.917(3) 4 ? V1 F1 1.917(3) 3 ? V1 F1 1.917(3) 2 ? V1 F1 1.917(3) . ? V1 O1 2.388(6) 5 ? O1 V1 2.388(6) 5_554 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C F2 0.89 2.03 2.654(5) 126.3 10_556 N1 H1D F1 0.89 1.92 2.811(5) 175.5 16_566 N1 H1E F1 0.89 1.92 2.748(5) 154.7 9_566 N1 H1E F1 0.89 2.56 3.130(5) 122.6 12_566 _journal_paper_doi 10.1039/c0dt01765e