# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010
data_global
_journal_name_full 'New J.Chem.'
_journal_coden_cambridge 0440
#TrackingRef '- InF3_3SbF5.cif'
#------------------ AUDIT DETAILS -------------------------------------------#
_audit_creation_date 2008-03-20
_audit_creation_method 'WinGX routine CIF_UPDATE'
_audit_conform_dict_name cif_core.dic
_audit_conform_dict_version 2.3
_audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record ?
#------------------ SUBMISSION DETAILS --------------------------------------#
# Name and address of author for correspondence
_publ_contact_author_name 'Goreshnik, Evgeny'
_publ_contact_author_address
;
Department of Inorganic Chemistry and Technology
Jozef Stefan Institute
Jamova 39 1000 Ljubljana
SLOVENIA
;
_publ_contact_author_email evgeny.goreshnik@ijs.si
_publ_contact_author_fax 386(1)4773645
_publ_contact_author_phone 386(1)4773155
_publ_requested_coeditor_name ?
_publ_contact_letter # Include date of submission
;
Date of submission ?
Please consider this CIF submission for publication as a
Regular Structural Paper in Acta Crystallographica C.
;
_publ_requested_category ?
#------------------ PROCESSING SUMMARY (JOURNAL OFFICE ONLY) ----------------#
_journal_date_recd_electronic ?
_journal_date_to_coeditor ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_date_printers_first ?
_journal_date_printers_final ?
_journal_date_proofs_out ?
_journal_date_proofs_in ?
_journal_coeditor_name ?
_journal_coeditor_code ?
_journal_coeditor_notes ?
_journal_techeditor_code ?
_journal_techeditor_notes ?
_journal_coden_ASTM ?
_journal_year ?
_journal_volume ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
#------------------ TITLE AND AUTHOR LIST------------------------------------#
_publ_section_title
;
?
;
_publ_section_title_footnote
;
?
;
loop_
_publ_author_name
_publ_author_address
Z.Mazej
;
Department of Inorganic Chemistry and Technology
Jozef Stefan Institute
Jamova 39 1000 Ljubljana
SLOVENIA
;
E.Goreshnik
;
Department of Inorganic Chemistry and Technology
Jozef Stefan Institute
Jamova 39 1000 Ljubljana
SLOVENIA
;
#------------------ TEXT ----------------------------------------------------#
_publ_section_synopsis
;
# Insert blank lines between paragraphs
?
;
_publ_section_abstract
;
# Insert blank lines between paragraphs
?
;
_publ_section_comment
;
# Insert blank lines between paragraphs
?
;
_publ_section_exptl_prep
;
?
;
_publ_section_exptl_refinement
;
?
;
# Insert blank lines between references
_publ_section_references
;
Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004).
J. Appl. Cryst. 37, 335--338.
Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J.
Appl. Cryst. 26, 343--350.
Blessing, R. H. (1995). Acta Cryst. A51, 33--38.
Farrugia, L. J. (1999) J. Appl. Cryst. 32, 837-838.
Molecular Structure Corporation. (1997--1999). TEXSAN for Windows.
Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails
Drive, The Woodlands, TX 77381, USA.
Pennington, W. T. (1999). J. Appl. Cryst. 32, 1028--1029.
Rigaku Corporation (1999). CrystalClear.
Sheldrick, G. M. (1997). SHELXL97. Program for crystal structure
refinement. University of G\"ottingen, Germany.
;
_publ_section_figure_captions
;
Figure 1. View of (I) (50% probability displacement ellipsoids)
;
_publ_section_acknowledgements
;
?
;
_publ_section_table_legends
;
Table 1. Fractional atomic coordinates and equivalent
isotropic displacement parameters (\%A^2^)
Table 2. Selected geometric parameters (\%A ,\% )
;
#------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------#
data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 783217'
#TrackingRef '- InF3_3SbF5.cif'
_audit_creation_date 2008-03-20T10:08:56-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
#------------------ CHEMICAL INFORMATION ------------------------------------#
_chemical_formula_moiety 'F18 In Sb3'
_chemical_formula_sum 'F18 In Sb3'
_chemical_formula_weight 822.07
#------------------ UNIT CELL INFORMATION -----------------------------------#
_symmetry_cell_setting trigonal
_symmetry_space_group_name_H-M 'P -3 c 1'
_symmetry_space_group_name_Hall '-P 3 2"c'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'x, x-y, z+1/2'
'-x+y, y, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, -z-1/2'
'-x, -x+y, -z-1/2'
'x-y, -y, -z-1/2'
_cell_length_a 8.7190(6)
_cell_length_b 8.7190(6)
_cell_length_c 9.5219(9)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 626.88(9)
_cell_formula_units_Z 2
_cell_measurement_temperature 200
_cell_measurement_reflns_used 1552
_cell_measurement_theta_min 2.1387
_cell_measurement_theta_max 28.6944
#------------------ CRYSTAL INFORMATION -------------------------------------#
_exptl_crystal_description Chunk
_exptl_crystal_colour Colorless
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.06
_exptl_crystal_density_diffrn 4.355
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 728
_exptl_absorpt_coefficient_mu 8.428
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.445
_exptl_absorpt_correction_T_max 0.611
_exptl_absorpt_process_details 'Blessing R.H., 1995'
#------------------ DATA COLLECTION INFORMATION -----------------------------#
_diffrn_ambient_temperature 200
_diffrn_radiation_wavelength 0.71069
_diffrn_radiation_type MoK\a
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_method dtprofit.ref
_diffrn_reflns_number 2501
_diffrn_reflns_av_R_equivalents 0.0331
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_theta_min 2.7
_diffrn_reflns_theta_max 28.69
_diffrn_reflns_theta_full 25
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measured_fraction_theta_full 0.987
_reflns_number_total 504
_reflns_number_gt 485
_reflns_threshold_expression I>2\s(I)
#------------------ COMPUTER PROGRAMS USED ----------------------------------#
_computing_data_collection 'CrystalClear (Rigaku Corporation, 1999)'
_computing_cell_refinement 'CrystalClear (Rigaku Corporation, 1999)'
_computing_data_reduction 'CrystalClear (Rigaku Corporation, 1999)'
_computing_structure_solution
;
SIR92 (Altomare et al., 1993),
TeXsan (Molecular Structure Corporation, 1997--1999).
;
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Diamond (Pennington, 1999)'
_computing_publication_material
;
WinGX 1.70 (Farrugia, L. J., 1997-2005), enCIFer v.1.2 (Allen et al., 2004)
;
#------------------ REFINEMENT INFORMATION ----------------------------------#
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+5.6520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_coef 0.0041(7)
_refine_ls_number_reflns 504
_refine_ls_number_parameters 36
_refine_ls_number_restraints 0
_refine_ls_R_factor_gt 0.0398
_refine_ls_wR_factor_ref 0.0913
_refine_ls_goodness_of_fit_ref 1.269
_refine_ls_restrained_S_all 1.269
_refine_ls_shift/su_max 0
_refine_diff_density_max 2.415
_refine_diff_density_min -2.041
#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.31 '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'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Sb1 Sb 0.65078(7) 0 0.25 0.0158(3) Uani 1 d S . .
In2 In 1 0 0 0.0160(3) Uani 1 d S . .
F1 F 0.5649(6) 0.1009(5) 0.1263(4) 0.0234(9) Uani 1 d . . .
F2 F 0.8685(5) 0.0866(5) 0.1308(4) 0.0188(8) Uani 1 d . . .
F3 F 0.5773(5) -0.2051(5) 0.1473(4) 0.0236(9) Uani 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
Sb1 0.0161(3) 0.0175(4) 0.0144(4) -0.0011(2) -0.00054(10) 0.00874(18)
In2 0.0170(4) 0.0170(4) 0.0138(6) 0 0 0.0085(2)
F1 0.026(2) 0.029(2) 0.021(2) 0.0032(16) -0.0013(17) 0.0178(18)
F2 0.0186(18) 0.023(2) 0.0163(19) 0.0022(15) 0.0056(15) 0.0115(16)
F3 0.028(2) 0.019(2) 0.023(2) -0.0056(16) -0.0032(16) 0.0108(18)
#------------------ MOLECULAR GEOMETRY --------------------------------------#
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Sb1 F1 1.839(4) . ?
Sb1 F1 1.839(4) 12_556 ?
Sb1 F3 1.849(4) . ?
Sb1 F3 1.849(4) 12_556 ?
Sb1 F2 2.007(4) 12_556 ?
Sb1 F2 2.007(4) . ?
In2 F2 2.075(4) 9_545 ?
In2 F2 2.075(4) 3_765 ?
In2 F2 2.075(4) 7_755 ?
In2 F2 2.075(4) 8_665 ?
In2 F2 2.075(4) . ?
In2 F2 2.075(4) 2_645 ?
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
F1 Sb1 F1 99.5(3) . 12_556 ?
F1 Sb1 F3 95.56(19) . . ?
F1 Sb1 F3 94.62(19) 12_556 . ?
F1 Sb1 F3 94.62(19) . 12_556 ?
F1 Sb1 F3 95.56(19) 12_556 12_556 ?
F3 Sb1 F3 164.2(3) . 12_556 ?
F1 Sb1 F2 170.78(17) . 12_556 ?
F1 Sb1 F2 89.56(18) 12_556 12_556 ?
F3 Sb1 F2 85.54(19) . 12_556 ?
F3 Sb1 F2 82.52(17) 12_556 12_556 ?
F1 Sb1 F2 89.56(18) . . ?
F1 Sb1 F2 170.78(17) 12_556 . ?
F3 Sb1 F2 82.52(17) . . ?
F3 Sb1 F2 85.54(19) 12_556 . ?
F2 Sb1 F2 81.5(2) 12_556 . ?
F2 In2 F2 180.00(17) 9_545 3_765 ?
F2 In2 F2 87.67(16) 9_545 7_755 ?
F2 In2 F2 92.33(16) 3_765 7_755 ?
F2 In2 F2 87.67(15) 9_545 8_665 ?
F2 In2 F2 92.33(15) 3_765 8_665 ?
F2 In2 F2 87.67(16) 7_755 8_665 ?
F2 In2 F2 92.33(16) 9_545 . ?
F2 In2 F2 87.67(16) 3_765 . ?
F2 In2 F2 180.0(2) 7_755 . ?
F2 In2 F2 92.33(16) 8_665 . ?
F2 In2 F2 92.33(15) 9_545 2_645 ?
F2 In2 F2 87.67(15) 3_765 2_645 ?
F2 In2 F2 92.33(16) 7_755 2_645 ?
F2 In2 F2 180.0(3) 8_665 2_645 ?
F2 In2 F2 87.67(16) . 2_645 ?
Sb1 F2 In2 142.5(2) . . ?
# Attachment '- TlF3_3SbF5.CIF'
data_TlF3_3SbF5
_database_code_depnum_ccdc_archive 'CCDC 783218'
#TrackingRef '- TlF3_3SbF5.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'F18 Sb3 Tl'
_chemical_formula_sum 'F18 Sb3 Tl'
_chemical_formula_weight 911.62
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'
_symmetry_cell_setting trigonal
_symmetry_space_group_name_H-M P-3
_symmetry_Int_Tables_number 147
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
_cell_length_a 9.408(16)
_cell_length_b 9.408(16)
_cell_length_c 8.597(14)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_volume 659.0(19)
_cell_formula_units_Z 2
_cell_measurement_temperature 200(2)
_cell_measurement_reflns_used 77
_cell_measurement_theta_min 2.3681
_cell_measurement_theta_max 28.6986
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 4.594
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 792
_exptl_absorpt_coefficient_mu 18.480
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.0445
_exptl_absorpt_correction_T_max 0.1600
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 200.0
_diffrn_radiation_wavelength 0.7107
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator 'Graphite Monochromator'
_diffrn_radiation_detector CCD
_diffrn_source_power 1.5000
_diffrn_source_voltage 50.0000
_diffrn_source_current 30.0000
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measurement_method dtprofit.ref
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_measurement_details
;
scan:
Number of images: 133
Slice: 0.1000 - 40.0000
Image width: 0.3000
Exp time: 15.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 0.0000
XTD: 50.1258
2theta: 20.0995
scan:
Number of images: 600
Slice: -90.0000 - 90.0000
Image width: 0.3000
Exp time: 15.0000
Rotation axis: Phi
Omega: 0.0000
Chi: 0.0000
Phi: 0.0000
XTD: 50.1258
2theta: 20.0995
;
_diffrn_measurement_device_details
;
AFC7: Eulerian 3-circle
;
_diffrn_reflns_number 2936
_diffrn_reflns_av_R_equivalents 0.03330
_diffrn_reflns_av_sigmaI/netI 0.073
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_theta_min 2.37
_diffrn_reflns_theta_max 27.66
_diffrn_measured_fraction_theta_max 0.98
_diffrn_reflns_theta_full 28.73
_diffrn_measured_fraction_theta_full 0.923
_reflns_number_total 1058
_reflns_number_gt 957
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+1.3977P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1058
_refine_ls_number_parameters 67
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0450
_refine_ls_R_factor_gt 0.0407
_refine_ls_wR_factor_ref 0.0972
_refine_ls_wR_factor_gt 0.0938
_refine_ls_goodness_of_fit_ref 1.137
_refine_ls_restrained_S_all 1.137
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 4.963
_refine_diff_density_min -2.878
_refine_diff_density_rms 0.412
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
Tl1 Tl 0.6667 0.3333 0.42734(7) 0.01656(19) Uani 1 3 d S . .
Sb2 Sb 0.34432(7) 0.36364(7) 0.24005(7) 0.01747(19) Uani 1 1 d . . .
F3 F 0.8612(6) 0.3899(6) 0.5964(6) 0.0208(11) Uani 1 1 d . . .
F4 F 0.3200(7) 0.2109(6) 0.0943(7) 0.0265(12) Uani 1 1 d . . .
F5 F 0.3899(7) 0.5278(7) 0.1002(7) 0.0271(12) Uani 1 1 d . . .
F6 F 0.8798(7) 0.6435(7) 0.4046(7) 0.0287(13) Uani 1 1 d . . .
F7 F 0.1250(6) 0.2904(7) 0.2668(7) 0.0302(13) Uani 1 1 d . . .
F8 F 0.5823(6) 0.4482(6) 0.2544(6) 0.0204(11) 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
Tl1 0.0158(2) 0.0158(2) 0.0181(3) 0.000 0.000 0.00790(11)
Sb2 0.0178(3) 0.0174(3) 0.0188(3) -0.0018(2) -0.0022(2) 0.0100(2)
F3 0.015(2) 0.020(2) 0.025(3) 0.002(2) -0.002(2) 0.007(2)
F4 0.037(3) 0.020(3) 0.025(3) -0.008(2) -0.003(3) 0.016(2)
F5 0.029(3) 0.026(3) 0.031(3) 0.006(2) 0.000(3) 0.017(3)
F6 0.028(3) 0.040(3) 0.028(3) -0.004(3) 0.004(2) 0.025(3)
F7 0.017(3) 0.035(3) 0.030(3) -0.006(3) -0.001(2) 0.007(2)
F8 0.014(2) 0.023(3) 0.028(3) 0.001(2) -0.001(2) 0.011(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Tl1 F3 2.184(6) . ?
Tl1 F3 2.184(6) 3_665 ?
Tl1 F3 2.184(6) 2_655 ?
Tl1 F8 2.205(6) 3_665 ?
Tl1 F8 2.205(6) 2_655 ?
Tl1 F8 2.205(6) . ?
Tl1 F6 2.593(8) 3_665 ?
Tl1 F6 2.593(8) . ?
Tl1 F6 2.593(8) 2_655 ?
Sb2 F5 1.831(6) . ?
Sb2 F4 1.833(6) . ?
Sb2 F7 1.834(6) . ?
Sb2 F6 1.894(6) 2_655 ?
Sb2 F8 1.970(6) . ?
Sb2 F3 1.977(6) 5_566 ?
F3 Sb2 1.977(6) 6_656 ?
F6 Sb2 1.894(6) 3_665 ?
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 Tl1 F3 80.6(2) . 3_665 ?
F3 Tl1 F3 80.6(2) . 2_655 ?
F3 Tl1 F3 80.6(2) 3_665 2_655 ?
F3 Tl1 F8 84.4(2) . 3_665 ?
F3 Tl1 F8 142.38(19) 3_665 3_665 ?
F3 Tl1 F8 130.6(2) 2_655 3_665 ?
F3 Tl1 F8 130.6(2) . 2_655 ?
F3 Tl1 F8 84.4(2) 3_665 2_655 ?
F3 Tl1 F8 142.38(19) 2_655 2_655 ?
F8 Tl1 F8 79.6(2) 3_665 2_655 ?
F3 Tl1 F8 142.38(19) . . ?
F3 Tl1 F8 130.6(2) 3_665 . ?
F3 Tl1 F8 84.4(2) 2_655 . ?
F8 Tl1 F8 79.6(2) 3_665 . ?
F8 Tl1 F8 79.6(2) 2_655 . ?
F3 Tl1 F6 70.27(18) . 3_665 ?
F3 Tl1 F6 72.15(18) 3_665 3_665 ?
F3 Tl1 F6 142.6(2) 2_655 3_665 ?
F8 Tl1 F6 70.32(18) 3_665 3_665 ?
F8 Tl1 F6 60.29(17) 2_655 3_665 ?
F8 Tl1 F6 132.9(2) . 3_665 ?
F3 Tl1 F6 72.15(18) . . ?
F3 Tl1 F6 142.6(2) 3_665 . ?
F3 Tl1 F6 70.27(19) 2_655 . ?
F8 Tl1 F6 60.29(17) 3_665 . ?
F8 Tl1 F6 132.9(2) 2_655 . ?
F8 Tl1 F6 70.32(18) . . ?
F6 Tl1 F6 119.44(4) 3_665 . ?
F3 Tl1 F6 142.6(2) . 2_655 ?
F3 Tl1 F6 70.27(19) 3_665 2_655 ?
F3 Tl1 F6 72.15(18) 2_655 2_655 ?
F8 Tl1 F6 132.9(2) 3_665 2_655 ?
F8 Tl1 F6 70.32(18) 2_655 2_655 ?
F8 Tl1 F6 60.29(17) . 2_655 ?
F6 Tl1 F6 119.44(4) 3_665 2_655 ?
F6 Tl1 F6 119.44(4) . 2_655 ?
F5 Sb2 F4 95.6(3) . . ?
F5 Sb2 F7 98.3(3) . . ?
F4 Sb2 F7 96.6(3) . . ?
F5 Sb2 F6 164.0(3) . 2_655 ?
F4 Sb2 F6 92.2(3) . 2_655 ?
F7 Sb2 F6 94.7(3) . 2_655 ?
F5 Sb2 F8 87.8(2) . . ?
F4 Sb2 F8 91.8(2) . . ?
F7 Sb2 F8 169.1(2) . . ?
F6 Sb2 F8 78.0(2) 2_655 . ?
F5 Sb2 F3 86.4(3) . 5_566 ?
F4 Sb2 F3 174.5(2) . 5_566 ?
F7 Sb2 F3 88.1(2) . 5_566 ?
F6 Sb2 F3 84.7(3) 2_655 5_566 ?
F8 Sb2 F3 83.2(2) . 5_566 ?
Sb2 F3 Tl1 156.7(3) 6_656 . ?
Sb2 F6 Tl1 104.3(2) 3_665 . ?
Sb2 F8 Tl1 117.3(2) . . ?
# Attachment '- TlF3_AsF5_2HF.cif'
#\#CIF_1.1
# CIF produced by WinGX routine CIF_UPDATE
# Created on 2010-03-17 at 15:50:59
# Using CIFtbx version 2.6.2 16 Jun 1998
# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\cifdoc.dat
# CIF files read : shelxl cs3 _Cs3
#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------#
data_TlF3_AsF5_2HF
_database_code_depnum_ccdc_archive 'CCDC 783219'
#TrackingRef '- TlF3_AsF5_2HF.cif'
_audit_creation_date 2010-03-17T15:50:59-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
#------------------ CHEMICAL INFORMATION ------------------------------------#
_chemical_formula_moiety 'As F9 H Tl, F H'
_chemical_formula_sum 'As F10 H2 Tl'
_chemical_formula_weight 471.31
#------------------ UNIT CELL INFORMATION -----------------------------------#
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P21/c
_symmetry_space_group_name_Hall '-P 2ybc'
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'
_cell_length_a 5.5533(4)
_cell_length_b 5.7652(5)
_cell_length_c 21.9287(19)
_cell_angle_alpha 90
_cell_angle_beta 93.279(4)
_cell_angle_gamma 90
_cell_volume 700.92(10)
_cell_formula_units_Z 4
_cell_measurement_temperature 200
_cell_measurement_reflns_used 2786
_cell_measurement_theta_min 1.8603
_cell_measurement_theta_max 29.0464
#------------------ CRYSTAL INFORMATION -------------------------------------#
_exptl_crystal_description Chunk
_exptl_crystal_colour Colorless
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.03
_exptl_crystal_density_diffrn 4.466
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 824
_exptl_absorpt_coefficient_mu 27.87
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.11
_exptl_absorpt_correction_T_max 0.375
_exptl_absorpt_process_details 'Blessing R.H., 1995'
#------------------ DATA COLLECTION INFORMATION -----------------------------#
_diffrn_ambient_temperature 200
_diffrn_radiation_wavelength 0.71069
_diffrn_radiation_type MoK\a
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_method dtprofit.ref
_diffrn_reflns_number 5364
_diffrn_reflns_av_R_equivalents 0.0717
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 1.86
_diffrn_reflns_theta_max 29.09
_diffrn_reflns_theta_full 25
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measured_fraction_theta_full 0.994
_reflns_number_total 1626
_reflns_number_gt 1444
_reflns_threshold_expression I>2\s(I)
#------------------ COMPUTER PROGRAMS USED ----------------------------------#
_computing_data_collection 'CrystalClear (Rigaku Corporation, 1999)'
_computing_cell_refinement 'CrystalClear (Rigaku Corporation, 1999)'
_computing_data_reduction 'CrystalClear (Rigaku Corporation, 1999)'
_computing_structure_solution
;
SIR92 (Altomare et al., 1993), TeXsan (Molecular Structure Corporation,
1997--1999).
;
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, K. & Berndt, M., 1999)
;
_computing_publication_material
;
WinGX 1.70 (Farrugia, L. J., 1999), enCIFer v.1.3 (Allen et al., 2004)
;
#------------------ REFINEMENT INFORMATION ----------------------------------#
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+28.8441P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.00052(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 1626
_refine_ls_number_parameters 110
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0693
_refine_ls_R_factor_gt 0.0593
_refine_ls_wR_factor_ref 0.1258
_refine_ls_wR_factor_gt 0.1177
_refine_ls_goodness_of_fit_ref 1.216
_refine_ls_restrained_S_all 1.216
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 4.386
_refine_diff_density_min -1.978
_refine_diff_density_rms 0.491
#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl1 Tl 0.75321(6) 0.10948(7) 0.771062(18) 0.01464(10) Uani 1 1 d . . .
As1 As 0.48925(19) 0.2252(2) 0.60286(5) 0.0203(3) Uani 1 1 d . . .
F1 F 0.7121(10) 0.1542(12) 0.6614(3) 0.0237(16) Uani 1 1 d . . .
F2 F 0.2764(13) 0.1018(15) 0.6459(4) 0.038(2) Uani 1 1 d . . .
F3 F 0.2671(13) 0.3119(16) 0.5507(3) 0.043(2) Uani 1 1 d . . .
F4 F 0.6995(12) 0.3668(12) 0.5650(3) 0.0285(17) Uani 1 1 d . . .
F5 F 0.5417(15) -0.0261(14) 0.5673(4) 0.041(2) Uani 1 1 d . . .
F6 F 0.4377(12) 0.4868(13) 0.6440(3) 0.0300(17) Uani 1 1 d . . .
F7 F 0.5555(10) -0.1886(11) 0.7349(3) 0.0204(15) Uani 1 1 d . . .
F8 F 0.9431(10) 0.4190(11) 0.7481(3) 0.0234(16) Uani 1 1 d . . .
F9 F 1.0124(11) 0.1788(13) 0.8537(3) 0.0265(17) Uani 1 1 d . . .
H1 H 0.9339 0.1955 0.8911 0.032 Uiso 1 1 d . . .
F10 F -0.0252(14) 0.2023(17) 0.4582(4) 0.046(2) Uani 1 1 d . . .
H2 H 0.0697 0.3017 0.4852 0.055 Uiso 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
Tl1 0.01375(17) 0.0141(2) 0.01596(18) 0.00033(15) 0.00002(13) 0.00017(14)
As1 0.0208(5) 0.0279(6) 0.0119(5) -0.0019(4) -0.0017(4) -0.0016(5)
F1 0.013(3) 0.033(4) 0.026(3) -0.013(3) 0.010(2) -0.008(3)
F2 0.027(3) 0.061(5) 0.026(4) 0.003(4) -0.004(3) -0.017(4)
F3 0.034(4) 0.070(6) 0.022(4) 0.002(4) -0.016(3) 0.012(4)
F4 0.033(3) 0.028(4) 0.025(3) 0.005(3) 0.011(3) 0.001(3)
F5 0.059(5) 0.029(4) 0.034(4) -0.013(4) -0.011(4) 0.001(4)
F6 0.037(3) 0.029(4) 0.025(3) -0.001(3) 0.016(3) 0.005(3)
F7 0.010(2) 0.025(3) 0.026(3) -0.008(3) 0.003(2) -0.012(2)
F8 0.016(3) 0.020(3) 0.035(4) 0.008(3) 0.012(3) -0.005(2)
F9 0.015(3) 0.042(4) 0.023(3) -0.008(3) -0.001(3) -0.002(3)
F10 0.043(4) 0.063(6) 0.030(4) -0.006(4) -0.015(4) -0.006(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Tl1 F7 2.070(6) 2_656 ?
Tl1 F8 2.075(6) 2_746 ?
Tl1 F8 2.147(6) . ?
Tl1 F7 2.165(6) . ?
Tl1 F9 2.284(6) . ?
Tl1 F6 2.307(7) 2_646 ?
Tl1 F1 2.416(7) . ?
As1 F5 1.679(8) . ?
As1 F4 1.683(7) . ?
As1 F3 1.708(7) . ?
As1 F2 1.709(8) . ?
As1 F1 1.780(7) . ?
As1 F6 1.788(7) . ?
F6 Tl1 2.307(7) 2_656 ?
F7 Tl1 2.070(6) 2_646 ?
F8 Tl1 2.075(6) 2_756 ?
F9 H1 0.960 . ?
F10 H2 0.960 . ?
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
F7 Tl1 F8 164.7(3) 2_656 2_746 ?
F7 Tl1 F8 86.2(2) 2_656 . ?
F8 Tl1 F8 88.66(7) 2_746 . ?
F7 Tl1 F7 91.28(8) 2_656 . ?
F8 Tl1 F7 84.7(2) 2_746 . ?
F8 Tl1 F7 145.0(3) . . ?
F7 Tl1 F9 115.7(3) 2_656 . ?
F8 Tl1 F9 76.7(3) 2_746 . ?
F8 Tl1 F9 75.2(3) . . ?
F7 Tl1 F9 135.5(3) . . ?
F7 Tl1 F6 78.8(3) 2_656 2_646 ?
F8 Tl1 F6 114.7(3) 2_746 2_646 ?
F8 Tl1 F6 134.3(3) . 2_646 ?
F7 Tl1 F6 78.8(2) . 2_646 ?
F9 Tl1 F6 73.2(2) . 2_646 ?
F7 Tl1 F1 81.2(2) 2_656 . ?
F8 Tl1 F1 83.5(2) 2_746 . ?
F8 Tl1 F1 72.4(2) . . ?
F7 Tl1 F1 72.7(2) . . ?
F9 Tl1 F1 142.2(2) . . ?
F6 Tl1 F1 144.6(2) 2_646 . ?
F5 As1 F4 92.6(4) . . ?
F5 As1 F3 94.6(4) . . ?
F4 As1 F3 91.3(4) . . ?
F5 As1 F2 92.4(4) . . ?
F4 As1 F2 174.8(4) . . ?
F3 As1 F2 89.7(4) . . ?
F5 As1 F1 90.3(4) . . ?
F4 As1 F1 89.7(3) . . ?
F3 As1 F1 175.0(4) . . ?
F2 As1 F1 88.9(3) . . ?
F5 As1 F6 177.4(4) . . ?
F4 As1 F6 88.6(3) . . ?
F3 As1 F6 87.7(4) . . ?
F2 As1 F6 86.4(4) . . ?
F1 As1 F6 87.4(3) . . ?
As1 F1 Tl1 139.9(3) . . ?
As1 F6 Tl1 139.4(4) . 2_656 ?
Tl1 F7 Tl1 150.5(3) 2_646 . ?
Tl1 F8 Tl1 154.5(3) 2_756 . ?
Tl1 F9 H1 114.0 . . ?