#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:40:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179454 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/51/4335158.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_4335158
loop_
_publ_author_name
'Maria V. Ivanova'
'Tobias Köchner'
'Hélène P. A. Mercier'
'Gary J. Schrobilgen'
_publ_section_title
;
 Synthesis and Lewis Acid Properties of (ReO3F)∞ and the X-ray
 Crystal Structures of (HF)2ReO3F.HF and
 [N(CH3)4]2-[{ReO3(μ-F)}3(μ3-O)].CH3CN
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6806
_journal_page_last               6819
_journal_paper_doi               10.1021/ic302221y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'KF 4(HF)'
_chemical_formula_sum            'F5 K'
_chemical_formula_weight         134.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                   6.287(5)
_cell_length_b                   6.287(5)
_cell_length_c                   12.937(5)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68
_cell_measurement_theta_min      0
_cell_volume                     511.4(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'SHELXTL V6.10 2001  Bruker-AXS'
_computing_publication_material  'SHELXTL V6.10 2001  Bruker-AXS'
_computing_structure_refinement  'SHELXTL V6.10 2001 Bruker-AXS'
_computing_structure_solution    'SHELXTL V6.10 2001  Bruker-AXS'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4237
_diffrn_reflns_theta_full        33.87
_diffrn_reflns_theta_max         33.87
_diffrn_reflns_theta_min         7.43
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       plates
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0298
_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)+(0.0451P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                411
_reflns_number_total             494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302221y_si_002_3.cif
_cod_data_source_block           KF.4HF
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4335158
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'
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
K001 K 2.0000 1.2500 0.6250 0.01335(17) Uani 1 4 d S
F002 F 1.5000 0.7500 0.6250 0.0153(3) Uani 1 4 d S
F003 F 1.76832(12) 1.05601(14) 0.47378(6) 0.0220(2) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
F003 K001 F003 120.97(4) . 15_686
F003 K001 F003 120.97(4) . 16_846
F003 K001 F003 88.32(6) 15_686 16_846
F003 K001 F003 88.32(6) . 2_975
F003 K001 F003 120.97(4) 15_686 2_975
F003 K001 F003 120.97(4) 16_846 2_975
F003 K001 F003 161.93(3) . 4_685
F003 K001 F003 72.21(3) 15_686 4_685
F003 K001 F003 68.53(3) 16_846 4_685
F003 K001 F003 73.79(5) 2_975 4_685
F003 K001 F003 73.79(5) . 3_745
F003 K001 F003 68.53(3) 15_686 3_745
F003 K001 F003 72.21(3) 16_846 3_745
F003 K001 F003 161.93(3) 2_975 3_745
F003 K001 F003 124.19(6) 4_685 3_745
F003 K001 F003 68.53(3) . 9_976
F003 K001 F003 161.93(3) 15_686 9_976
F003 K001 F003 73.79(5) 16_846 9_976
F003 K001 F003 72.21(3) 2_975 9_976
F003 K001 F003 102.65(2) 4_685 9_976
F003 K001 F003 102.65(2) 3_745 9_976
F003 K001 F003 72.21(3) . 10_566
F003 K001 F003 73.79(5) 15_686 10_566
F003 K001 F003 161.93(3) 16_846 10_566
F003 K001 F003 68.53(3) 2_975 10_566
F003 K001 F003 102.65(2) 4_685 10_566
F003 K001 F003 102.65(2) 3_745 10_566
F003 K001 F003 124.19(6) 9_976 10_566
F003 K001 K001 152.47(2) . 13_976
F003 K001 K001 78.30(5) 15_686 13_976
F003 K001 K001 34.29(2) 16_846 13_976
F003 K001 K001 98.17(5) 2_975 13_976
F003 K001 K001 34.241(18) 4_685 13_976
F003 K001 K001 98.94(4) 3_745 13_976
F003 K001 K001 87.93(4) 9_976 13_976
F003 K001 K001 135.02(2) 10_566 13_976
F003 K001 K001 34.29(2) . 9_976
F003 K001 K001 152.46(2) 15_686 9_976
F003 K001 K001 98.17(5) 16_846 9_976
F003 K001 K001 78.30(5) 2_975 9_976
F003 K001 K001 135.02(2) 4_685 9_976
F003 K001 K001 87.93(4) 3_745 9_976
F003 K001 K001 34.241(18) 9_976 9_976
F003 K001 K001 98.94(4) 10_566 9_976
K001 K001 K001 120.95(3) 13_976 9_976
F003 K001 K001 78.30(5) . 9_986
F003 K001 K001 98.17(5) 15_686 9_986
F003 K001 K001 152.47(2) 16_846 9_986
F003 K001 K001 34.29(2) 2_975 9_986
F003 K001 K001 87.93(4) 4_685 9_986
F003 K001 K001 135.02(2) 3_745 9_986
F003 K001 K001 98.94(4) 9_976 9_986
F003 K001 K001 34.241(18) 10_566 9_986
K001 K001 K001 120.95(3) 13_976 9_986
K001 K001 K001 88.37(5) 9_976 9_986
F003 K001 K001 98.17(5) . 13_876
F003 K001 K001 34.29(2) 15_686 13_876
F003 K001 K001 78.30(5) 16_846 13_876
F003 K001 K001 152.47(2) 2_975 13_876
F003 K001 K001 98.94(4) 4_685 13_876
F003 K001 K001 34.241(17) 3_745 13_876
F003 K001 K001 135.02(2) 9_976 13_876
F003 K001 K001 87.93(4) 10_566 13_876
K001 K001 K001 88.37(5) 13_976 13_876
K001 K001 K001 120.95(3) 9_976 13_876
K001 K001 K001 120.95(3) 9_986 13_876
K001 F003 K001 111.47(3) . 9_976
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K001 F003 2.7269(14) .
K001 F003 2.7269(14) 15_686
K001 F003 2.7269(14) 16_846
K001 F003 2.7269(14) 2_975
K001 F003 2.7306(19) 4_685
K001 F003 2.7306(19) 3_745
K001 F003 2.7306(19) 9_976
K001 F003 2.7306(19) 10_566
K001 K001 4.510(2) 13_976
K001 K001 4.510(2) 9_976
K001 K001 4.510(2) 9_986
K001 K001 4.510(2) 13_876
F003 K001 2.7306(19) 9_976
