#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:02:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179500 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/97/4339753.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_4339753
loop_
_publ_author_name
'Supeł, Joanna'
'Abram, Ulrich'
'Hagenbach, Adelheid'
'Seppelt, Konrad'
_publ_section_title
;
 Technetium fluoride trioxide, TcO3F, preparation and properties.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5591
_journal_page_last               5595
_journal_paper_doi               10.1021/ic070333y
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         VOF3
_chemical_formula_sum            'F3 O V'
_chemical_formula_weight         123.94
_chemical_name_common            vanadium-trifluoride-oxide
_chemical_name_systematic
; 
 vanadium-trifluoride-oxide 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 91.32(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.569(6)
_cell_length_b                   5.007(4)
_cell_length_c                   9.341(7)
_cell_measurement_temperature    183(2)
_cell_volume                     260.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      20
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  `Bruker-SMART-CCD-Diffractometer`
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2033
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    3.667
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.599443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.002(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0255
_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/[σ²(Fo²)+(0.0433P)²+0.2121P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0677
_reflns_number_gt                551
_reflns_number_total             611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070333ysi20070221_054349.cif
_cod_data_source_block           vof3
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4339753
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'
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
V V 0.66796(7) 0.92169(8) 0.37459(4) 0.01032(19) Uani 1 1 d
F1 F 0.6498(2) 1.1406(3) 0.54279(14) 0.0116(3) Uani 1 1 d
F2 F 0.9027(3) 1.1055(3) 0.31183(16) 0.0195(4) Uani 1 1 d
F3 F 0.5486(3) 0.7783(3) 0.21262(14) 0.0145(3) Uani 1 1 d
O O 0.7993(3) 0.6775(4) 0.44202(19) 0.0179(4) 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
V 0.0113(2) 0.0113(3) 0.0084(2) -0.00103(13) -0.00049(14) -0.00020(14)
F1 0.0136(6) 0.0121(7) 0.0091(6) -0.0018(5) -0.0007(5) -0.0034(5)
F2 0.0166(7) 0.0218(9) 0.0203(8) 0.0010(6) 0.0038(6) -0.0050(6)
F3 0.0198(7) 0.0136(8) 0.0098(6) -0.0025(6) -0.0014(5) -0.0023(6)
O 0.0195(9) 0.0167(10) 0.0175(9) 0.0010(7) -0.0032(7) 0.0042(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
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
O V F2 101.88(11) . .
O V F3 100.94(10) . .
F2 V F3 101.41(9) . .
O V F1 98.68(10) . .
F2 V F1 91.63(9) . .
F3 V F1 153.58(7) . .
O V F1 97.79(10) . 3_676
F2 V F1 156.60(8) . 3_676
F3 V F1 87.03(8) . 3_676
F1 V F1 72.86(8) . 3_676
O V F3 175.65(8) . 2_655
F2 V F3 81.92(9) . 2_655
F3 V F3 80.21(6) . 2_655
F1 V F3 78.99(8) . 2_655
F1 V F3 78.04(7) 3_676 2_655
V F1 V 107.14(7) . 3_676
V F3 V 142.64(8) . 2_645
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V O 1.551(2) .
V F2 1.7133(19) .
V F3 1.7888(17) .
V F1 1.9203(18) .
V F1 1.971(2) 3_676
V F3 2.294(2) 2_655
F1 V 1.972(2) 3_676
F3 V 2.294(2) 2_645
