#------------------------------------------------------------------------------ #$Date: 2016-03-25 13:43:39 +0200 (Fri, 25 Mar 2016) $ #$Revision: 179860 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/56/7015600.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_7015600 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_paper_doi 10.1039/c0dt01765e _journal_volume 40 _journal_year 2011 _chemical_formula_moiety 'F5 V, 2(C H6 N)' _chemical_formula_sum 'C2 H12 F5 N2 V' _chemical_formula_weight 210.08 _chemical_name_systematic ; ? ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _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 4 _cell_length_a 10.256(3) _cell_length_b 7.899(4) _cell_length_c 9.157(5) _cell_measurement_reflns_used 2937 _cell_measurement_temperature 125(2) _cell_measurement_theta_max 26.3661 _cell_measurement_theta_min 1.9857 _cell_volume 741.8(6) _computing_cell_refinement 'CrystalClear (rigaku Corp., 2008)' _computing_data_collection 'CrystalClear (rigaku Corp., 2008)' _computing_data_reduction 'CrystalClear (rigaku Corp., 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 125(2) _diffrn_measured_fraction_theta_full 0.968 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1625 _diffrn_reflns_av_sigmaI/netI 0.0893 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 3576 _diffrn_reflns_theta_full 26.33 _diffrn_reflns_theta_max 26.33 _diffrn_reflns_theta_min 3.41 _exptl_absorpt_coefficient_mu 1.363 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.28261 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 424 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.966 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.273 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 59 _refine_ls_number_reflns 784 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.168 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.1164 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1705P)^2^+9.0991P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3419 _refine_ls_wR_factor_ref 0.3474 _reflns_number_gt 734 _reflns_number_total 784 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c0dt01765e.txt _cod_data_source_block 6 _cod_database_code 7015600 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' 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 0.5000 0.0218(9) Uani 1 2 d S . . F1 F -0.0101(7) 0.7500 0.4688(8) 0.0266(19) Uani 1 2 d S . . F2 F 0.1916(6) 0.4952(6) 0.4251(5) 0.0346(16) Uani 1 1 d . . . F3 F -0.0793(6) 0.4626(7) 0.3284(4) 0.0332(15) Uani 1 1 d . . . N2 N 0.2627(10) 0.7500 0.2442(9) 0.030(3) Uani 1 2 d S . . H2A H 0.2949 0.8545 0.2489 0.045 Uiso 0.50 1 calc PR . . H2B H 0.3218 0.6810 0.2052 0.045 Uiso 0.50 1 calc PR . . H2C H 0.2427 0.7145 0.3337 0.045 Uiso 0.50 1 calc PR . . C2 C 0.1401(11) 0.7500 0.1495(11) 0.027(3) Uani 1 2 d S . . H2D H 0.0791 0.8311 0.1871 0.040 Uiso 0.50 1 calc PR . . H2E H 0.1014 0.6394 0.1508 0.040 Uiso 0.50 1 calc PR . . H2F H 0.1629 0.7795 0.0510 0.040 Uiso 0.50 1 calc PR . . N1 N 0.1803(10) 0.2500 0.2283(10) 0.030(2) Uani 1 2 d S . . H1A H 0.1857 0.3544 0.2645 0.045 Uiso 0.50 1 calc PR . . H1B H 0.2593 0.2150 0.2017 0.045 Uiso 0.50 1 calc PR . . H1C H 0.1486 0.1806 0.2961 0.045 Uiso 0.50 1 calc PR . . C1 C 0.0974(14) 0.2500 0.1063(12) 0.042(4) Uani 1 2 d S . . H1D H 0.0163 0.1969 0.1315 0.063 Uiso 0.50 1 calc PR . . H1E H 0.1378 0.1887 0.0279 0.063 Uiso 0.50 1 calc PR . . H1F H 0.0814 0.3645 0.0760 0.063 Uiso 0.50 1 calc PR . . 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 0.0309(15) 0.0315(16) 0.0032(12) 0.0011(7) 0.0003(6) -0.0011(8) F1 0.057(5) 0.018(4) 0.005(3) 0.000 -0.007(3) 0.000 F2 0.035(3) 0.053(4) 0.016(2) 0.005(2) 0.010(2) 0.004(2) F3 0.058(4) 0.038(3) 0.003(2) 0.0003(19) -0.009(2) -0.002(3) N2 0.028(6) 0.051(7) 0.010(4) 0.000 0.005(4) 0.000 C2 0.024(6) 0.048(8) 0.009(5) 0.000 -0.006(4) 0.000 N1 0.026(6) 0.050(7) 0.013(4) 0.000 0.003(4) 0.000 C1 0.033(7) 0.083(12) 0.009(5) 0.000 -0.002(5) 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' 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' V V 0.3005 0.5294 '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' 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 F3 V1 F3 180.000(1) . 5_566 ? F3 V1 F1 89.2(3) . 5_566 ? F3 V1 F1 90.8(3) 5_566 5_566 ? F3 V1 F1 90.8(3) . . ? F3 V1 F1 89.2(3) 5_566 . ? F1 V1 F1 180.0(4) 5_566 . ? F3 V1 F2 97.9(2) . . ? F3 V1 F2 82.1(2) 5_566 . ? F1 V1 F2 88.9(2) 5_566 . ? F1 V1 F2 91.1(3) . . ? F3 V1 F2 82.1(2) . 5_566 ? F3 V1 F2 97.9(2) 5_566 5_566 ? F1 V1 F2 91.1(3) 5_566 5_566 ? F1 V1 F2 88.9(3) . 5_566 ? F2 V1 F2 180.0 . 5_566 ? V1 F1 V1 162.5(4) 4_556 . ? C2 N2 H2A 109.5 . . ? C2 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C2 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? N2 C2 H2D 109.5 . . ? N2 C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? N2 C2 H2F 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? N1 C1 H1F 109.5 . . ? H1D C1 H1F 109.5 . . ? H1E C1 H1F 109.5 . . ? 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 F3 1.794(5) . ? V1 F3 1.794(5) 5_566 ? V1 F1 1.998(2) 5_566 ? V1 F1 1.998(2) . ? V1 F2 2.082(6) . ? V1 F2 2.082(6) 5_566 ? F1 V1 1.998(2) 4_556 ? N2 C2 1.527(14) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? C2 H2D 0.9600 . ? C2 H2E 0.9600 . ? C2 H2F 0.9600 . ? N1 C1 1.405(15) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C1 H1F 0.9600 . ? 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 N2 H2A F3 0.89 2.06 2.867(9) 149.9 3_565 N2 H2A F2 0.89 2.27 2.707(8) 110.3 8_575 N2 H2B F3 0.89 2.02 2.867(9) 157.5 6_656 N2 H2B F1 0.89 2.41 3.039(12) 127.9 6_656 N2 H2C F2 0.89 1.99 2.707(8) 136.1 . N1 H1A F2 0.89 1.85 2.648(8) 149.0 . N1 H1B F3 0.89 2.19 3.027(11) 157.3 3 N1 H1B F3 0.89 2.58 3.027(11) 112.2 6_656 N1 H1C F2 0.89 1.88 2.648(8) 144.0 8_565 N1 H1C F3 0.89 2.61 3.279(11) 132.3 8_565 N1 H1C F1 0.89 2.64 3.277(12) 129.7 5_566