Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2002

data_General
_journal_name_full               'J.Chem.Soc.,Dalton Trans.'
_journal_coden_Cambridge         0186

#==============================================================================

_audit_creation_date             2002-10-16
_audit_creation_method           'by teXsan for Windows v1.06'
_audit_update_record             
;
?
;

_publ_requested_category         FI

_publ_contact_author_name        'Adolf Jesih'

_publ_contact_author_address     
;
Jozef Stefan Institute
Department of Inorganic Chemistry and Technology
Jamova 39
1000 Ljubljana
Slovenia 
;

_publ_contact_author_phone       '(386) 1 477 34 73'
_publ_contact_author_fax         '(386) 1 423 21 25'
_publ_contact_author_email       adolf.jesih@ijs.si

#==============================================================================

# PROCESSING SUMMARY (IUCr Office Use Only)

# TITLE AND AUTHOR LIST

_publ_section_title              
;
Alkali-metal fluoroarsenates(III) revisited; the
As4F13- anion, the crystal structure of CsAs4F13 and Raman spectra of
MAs4F13 (M = Rb, Cs)
;

_publ_section_title_footnote     
;
?
;
loop_
_publ_author_name
_publ_author_address
'Peter Klampfer'
;
Jo\<zef Stefan Institute
Department of Inorganic Chemistry and Technology
Jamova 39
1000 Ljubljana
Slovenia
;
'Primoz Benkic'
;
Jo\<zef Stefan Institute
Department of Inorganic Chemistry and Technology
Jamova 39
1000 Ljubljana
Slovenia
;
'Prof.Dr. Bogdan Volavsek'
;
Faculty of Chemistry and Chemical Technology
Smetanova 17
2000 Maribor
Slovenia
;
'Dr. Adolf Jesih'
;
Jo\<zef Stefan Institute
Department of Inorganic Chemistry and Technology
Jamova 39
1000 Ljubljana
Slovenia
;

#==============================================================================

# TEXT

_publ_section_abstract           
;
Alkali metal fluoroarsenates(III), CsAs~4~F~13~ and RbAs~4~F~13~ were 
sythesised by the reaction of CsF and RbF with liquid AsF~3~ at 353K.
Single crystal structure for CsAs~4~F~13~ was determined at 200K.
;

_publ_section_exptl_refinement   
;
ENTER EXPERIMENTAL SECTION
;

_publ_section_comment            
;
ENTER TEXT
;

_publ_section_references         
;
ENTER OTHER REFERENCES

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.

Rigaku Corporation (1999). CrystalClear.

Sheldrick, G.M. (1997). SHELXL-97
Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564.

Altomare, A., Cascarano, M., 
Giacovazzo, C., Guagliardi, A. (1994). 
J. Appl. Cryst., 26, 343. 
;

_publ_section_acknowledgements   
;
ENTER ACKNOWLEDGEMENTS
;

_publ_section_table_legends      
;
ENTER TABLE LEGENDS
;

_publ_section_figure_captions    
;
ENTER FIGURE CAPTIONS
;

#============================================================================== 
data_CsAs4F13
_database_code_CSD               196171

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'As4 Cs F13'
_chemical_formula_weight         679.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 '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'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I-4

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   9.568(4)
_cell_length_b                   9.568(4)
_cell_length_c                   6.726(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     615.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(1)
_cell_measurement_reflns_used    1778
_cell_measurement_theta_min      3.0088
_cell_measurement_theta_max      30.0326

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608
_exptl_absorpt_coefficient_mu    13.814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0518
_exptl_absorpt_correction_T_max  0.252
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      200(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2336
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_sigmaI/netI    0.0868
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.0088
_diffrn_reflns_theta_max         30.0326
_diffrn_reflns_theta_full        30.26
_reflns_number_total             760
_reflns_number_gt                695
_reflns_threshold_expression     >2sigma(I)
_diffrn_measured_fraction_theta_max 30.0326
_diffrn_measured_fraction_theta_full 88.5000
_diffrn_measurement_details      
;
scan:
	Number of images: 100
	           Slice: -20.0000 - 30.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: -90.0000
	             Phi: 0.0000
	             XTD: 34.8676
	          2theta: -9.9231
scan:
	Number of images: 360
	           Slice: -90.0000 - 90.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Phi
	           Omega: 0.0000
	             Chi: 0.0000
	             Phi: 0.0000
	             XTD: 34.8676
	          2theta: -9.9231

;
_diffrn_measurement_device_details 
;
AFC7: Eulerian 3-circle
;

_computing_data_collection       'Rigaku Corporation (1999). CrystalClear.'
_computing_cell_refinement       'Rigaku Corporation (1999). CrystalClear.'
_computing_data_reduction        'Rigaku Corporation (1999). CrystalClear.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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^)+(0.0000P)^2^+0.0000P] 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     SHELXL
_refine_ls_extinction_coef       0.124(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_number_reflns         760
_refine_ls_number_parameters     42
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.0686
_refine_ls_wR_factor_gt          0.0683
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.309

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
Cs1 Cs 0.0000 0.0000 0.0000 0.0222(3) Uani 1 4 d S . .
As1 As 0.30511(6) 0.01653(6) 0.51432(12) 0.0142(2) Uani 1 1 d . . .
F1 F 0.5000 0.0000 0.7500 0.0237(18) Uani 1 4 d S . .
F11 F 0.1674(4) 0.0770(4) 0.3632(6) 0.0226(9) Uani 1 1 d . . .
F12 F 0.2406(4) 0.1138(4) 0.7102(6) 0.0279(11) Uani 1 1 d . . .
F13 F 0.4131(4) 0.1469(4) 0.4258(6) 0.0275(10) 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
Cs1 0.0285(3) 0.0285(3) 0.0097(4) 0.000 0.000 0.000
As1 0.0121(3) 0.0162(3) 0.0142(4) 0.0009(3) -0.0001(3) 0.0016(2)
F1 0.023(3) 0.023(3) 0.026(4) 0.000 0.000 0.000
F11 0.019(2) 0.027(2) 0.022(2) 0.0002(18) -0.0091(16) 0.0053(18)
F12 0.020(2) 0.043(3) 0.021(2) -0.0147(19) -0.0008(17) 0.002(2)
F13 0.022(2) 0.030(2) 0.030(2) 0.0134(18) -0.0003(17) -0.0048(18)

_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
Cs1 F11 3.013(4) . ?
Cs1 F11 3.013(4) 3 ?
Cs1 F11 3.013(4) 4 ?
Cs1 F11 3.013(4) 2 ?
Cs1 F12 3.207(4) 2_554 ?
Cs1 F12 3.207(4) 4_556 ?
Cs1 F12 3.207(4) 1_554 ?
Cs1 F12 3.207(4) 3_556 ?
Cs1 F13 3.515(5) 5_444 ?
Cs1 F13 3.515(5) 7_455 ?
Cs1 F13 3.515(5) 6_554 ?
Cs1 F13 3.515(5) 8_545 ?
As1 F13 1.726(4) . ?
As1 F12 1.727(4) . ?
As1 F11 1.762(4) . ?
F12 Cs1 3.207(4) 1_556 ?
F13 Cs1 3.515(5) 5 ?

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
F11 Cs1 F11 131.12(11) . 3 ?
F11 Cs1 F11 131.12(11) . 4 ?
F11 Cs1 F11 71.63(17) 3 4 ?
F11 Cs1 F11 71.63(17) . 2 ?
F11 Cs1 F11 131.12(11) 3 2 ?
F11 Cs1 F11 131.12(11) 4 2 ?
F11 Cs1 F12 163.24(10) . 2_554 ?
F11 Cs1 F12 60.15(10) 3 2_554 ?
F11 Cs1 F12 60.79(10) 4 2_554 ?
F11 Cs1 F12 91.62(12) 2 2_554 ?
F11 Cs1 F12 60.79(10) . 4_556 ?
F11 Cs1 F12 163.24(10) 3 4_556 ?
F11 Cs1 F12 91.62(12) 4 4_556 ?
F11 Cs1 F12 60.15(10) 2 4_556 ?
F12 Cs1 F12 111.68(8) 2_554 4_556 ?
F11 Cs1 F12 91.62(12) . 1_554 ?
F11 Cs1 F12 60.79(10) 3 1_554 ?
F11 Cs1 F12 60.15(10) 4 1_554 ?
F11 Cs1 F12 163.24(10) 2 1_554 ?
F12 Cs1 F12 105.14(15) 2_554 1_554 ?
F12 Cs1 F12 111.68(8) 4_556 1_554 ?
F11 Cs1 F12 60.15(10) . 3_556 ?
F11 Cs1 F12 91.62(12) 3 3_556 ?
F11 Cs1 F12 163.24(10) 4 3_556 ?
F11 Cs1 F12 60.79(10) 2 3_556 ?
F12 Cs1 F12 111.68(8) 2_554 3_556 ?
F12 Cs1 F12 105.14(15) 4_556 3_556 ?
F12 Cs1 F12 111.68(8) 1_554 3_556 ?
F11 Cs1 F13 118.42(10) . 5_444 ?
F11 Cs1 F13 55.38(10) 3 5_444 ?
F11 Cs1 F13 109.75(11) 4 5_444 ?
F11 Cs1 F13 75.77(11) 2 5_444 ?
F12 Cs1 F13 54.38(9) 2_554 5_444 ?
F12 Cs1 F13 134.10(11) 4_556 5_444 ?
F12 Cs1 F13 114.20(10) 1_554 5_444 ?
F12 Cs1 F13 58.44(10) 3_556 5_444 ?
F11 Cs1 F13 109.75(11) . 7_455 ?
F11 Cs1 F13 118.42(10) 3 7_455 ?
F11 Cs1 F13 75.77(11) 4 7_455 ?
F11 Cs1 F13 55.38(10) 2 7_455 ?
F12 Cs1 F13 58.44(10) 2_554 7_455 ?
F12 Cs1 F13 54.38(9) 4_556 7_455 ?
F12 Cs1 F13 134.10(11) 1_554 7_455 ?
F12 Cs1 F13 114.20(10) 3_556 7_455 ?
F13 Cs1 F13 91.155(19) 5_444 7_455 ?
F11 Cs1 F13 75.77(11) . 6_554 ?
F11 Cs1 F13 109.75(11) 3 6_554 ?
F11 Cs1 F13 55.38(10) 4 6_554 ?
F11 Cs1 F13 118.42(10) 2 6_554 ?
F12 Cs1 F13 114.20(10) 2_554 6_554 ?
F12 Cs1 F13 58.44(10) 4_556 6_554 ?
F12 Cs1 F13 54.38(9) 1_554 6_554 ?
F12 Cs1 F13 134.10(11) 3_556 6_554 ?
F13 Cs1 F13 163.68(14) 5_444 6_554 ?
F13 Cs1 F13 91.155(19) 7_455 6_554 ?
F11 Cs1 F13 55.38(10) . 8_545 ?
F11 Cs1 F13 75.77(11) 3 8_545 ?
F11 Cs1 F13 118.42(10) 4 8_545 ?
F11 Cs1 F13 109.75(11) 2 8_545 ?
F12 Cs1 F13 134.10(11) 2_554 8_545 ?
F12 Cs1 F13 114.20(10) 4_556 8_545 ?
F12 Cs1 F13 58.44(10) 1_554 8_545 ?
F12 Cs1 F13 54.38(9) 3_556 8_545 ?
F13 Cs1 F13 91.155(19) 5_444 8_545 ?
F13 Cs1 F13 163.68(14) 7_455 8_545 ?
F13 Cs1 F13 91.155(19) 6_554 8_545 ?
F13 As1 F12 95.03(19) . . ?
F13 As1 F11 90.66(19) . . ?
F12 As1 F11 89.7(2) . . ?
As1 F11 Cs1 141.70(19) . . ?
As1 F12 Cs1 122.48(19) . 1_556 ?
As1 F13 Cs1 141.9(2) . 5 ?
#==============================================================================
#     End of CIF
#==============================================================================