#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:02:51 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179500 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/97/4339756.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_4339756
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         TcO3F
_chemical_formula_sum            'F O3 Tc'
_chemical_formula_weight         165.00
_chemical_name_common            technetiumfluoridetrioxide
_chemical_name_systematic
; 
 technetiumfluoridetrioxide 
;
_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                 93.212(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.689(3)
_cell_length_b                   5.069(3)
_cell_length_c                   9.305(5)
_cell_measurement_temperature    158(2)
_cell_volume                     267.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      20
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1787
_diffrn_reflns_theta_full        28.92
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         4.39
_exptl_absorpt_coefficient_mu    5.179
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.424602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.930
_refine_diff_density_min         -3.067
_refine_diff_density_rms         0.491
_refine_ls_extinction_coef       0.003(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   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0613
_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)+(0.0535P)²+21.2095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1578
_reflns_number_gt                547
_reflns_number_total             660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070333y-file003.cif
_cod_data_source_block           tco3f
_cod_original_cell_volume        267.9(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4339756
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
Tc Tc 0.67408(18) 0.0798(2) 0.36186(11) 0.0073(4) Uani 1 1 d
F F 0.3434(13) 0.1374(14) 0.4546(8) 0.0065(14) Uani 1 1 d
O1 O 0.9037(17) -0.093(2) 0.3081(11) 0.0133(19) Uani 1 1 d
O2 O 0.5445(15) 0.2189(17) 0.2062(9) 0.0067(16) Uani 1 1 d
O3 O 0.7938(17) 0.3402(18) 0.4496(11) 0.0112(19) 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
Tc 0.0083(6) 0.0041(5) 0.0094(6) -0.0005(4) 0.0003(3) 0.0000(4)
F 0.010(3) 0.007(3) 0.002(3) 0.002(2) -0.001(3) 0.004(3)
O1 0.012(4) 0.009(4) 0.018(5) -0.001(4) -0.004(3) 0.005(4)
O2 0.009(4) 0.004(4) 0.007(4) 0.002(3) 0.002(3) 0.000(3)
O3 0.011(4) 0.006(4) 0.017(5) 0.002(3) 0.002(4) 0.002(3)
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'
Tc Tc -1.4390 0.7593 '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
O1 Tc O3 104.8(5) . .
O1 Tc O2 105.4(5) . .
O3 Tc O2 103.2(4) . .
O1 Tc F 92.5(4) . 3_656
O3 Tc F 93.1(4) . 3_656
O2 Tc F 151.5(4) . 3_656
O1 Tc F 156.0(4) . .
O3 Tc F 92.2(4) . .
O2 Tc F 86.5(3) . .
F Tc F 69.5(3) 3_656 .
O1 Tc O2 85.3(4) . 2_645
O3 Tc O2 165.2(4) . 2_645
O2 Tc O2 84.0(2) . 2_645
F Tc O2 75.4(3) 3_656 2_645
F Tc O2 75.1(3) . 2_645
Tc F Tc 110.5(3) 3_656 .
Tc O2 Tc 139.1(5) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tc O1 1.674(10) .
Tc O3 1.677(10) .
Tc O2 1.738(9) .
Tc F 2.039(7) 3_656
Tc F 2.133(7) .
Tc O2 2.282(9) 2_645
F Tc 2.039(7) 3_656
O2 Tc 2.282(9) 2_655
