# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2005


data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177

_publ_contact_author_name        'Dr Romute Yu Garlyauskayte'
_publ_contact_author_address     
;
Institute of Organic Chemistry
National Academy of Sciences of Ukraine
Murmanskaya str 5
Kiev
02094
UKRAINE
;

_publ_contact_author_email       ROMA@BPCI.KIEV.UA

_publ_section_title              
;
Synthesis of new organic super acids - N-
(trifluoromethylsulfonyl)imino derivatives of trifluoromethanesulfonic
acid and trifluoromethylsulfonyl imide
;
loop_
_publ_author_name
'Romute Yu. Garlyauskayte'
'Michel Armand'
'Alexander N. Chernega'
'Christophe Michot'
;
Y.L.Yagupolskii
;
'Lev M. Yagupolskii'

data_CRYSTALS_cif2
_database_code_depnum_ccdc_archive 'CCDC 257232'
_audit_creation_date             2005-18-04
_audit_creation_method           CRYSTALS_ver_12-03-99

#****************************************************************************

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

_chemical_name_systematic        # IUPAC name, in full
;
potassium salt of bis [N-(trifluoromethylsulfonylimino)]trifluoro-
methanesulfonic acid

;

_chemical_melting_point          '98-101 C'

_refine_ls_matrix_type           full

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   'no H atoms'

_refine_ls_hydrogen_treatment    noref

#****************************************************************************
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al 2001)
;
_computing_molecular_graphics    
;
CAMERON (Watkin et al 1996)
;
#=============================================================

_cell_length_a                   22.385(6)
_cell_angle_alpha                90
_cell_length_b                   16.653(4)
_cell_angle_beta                 90
_cell_length_c                   7.093(4)
_cell_angle_gamma                90
_cell_volume                     2644.1(18)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P b c n '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y,z+1/2
-x,y,-z+1/2
-x+1/2,-y+1/2,z+1/2
x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 International_Tables_Vol_IV_Table_2.2B
'K ' 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 International_Tables_Vol_IV_Table_2.2B

_cell_formula_units_Z            8
_chemical_formula_sum            ' C3 F9 K1 N2 O5 S3 '
_chemical_formula_moiety         ' C3 F9 K1 N2 O5 S3 '
_chemical_compound_source        
;
?
;
_chemical_formula_weight         450.32

_cell_measurement_reflns_used    22
_cell_measurement_theta_min      12
_cell_measurement_theta_max      13
_cell_measurement_temperature    293

_exptl_crystal_description       ' block '
_exptl_crystal_colour            ' colourless '
_exptl_crystal_size_min          0.14
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_max          0.37

_exptl_crystal_density_diffrn    2.262
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             1760.000
_exptl_absorpt_coefficient_mu    1.012
# Sheldrick geometric definitions 0.78 0.87

_diffrn_measurement_device_type  
;
Enraf Nonius CAD-4
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
CAD-4 software
;
_computing_data_reduction        
;
RC93
;
_computing_cell_refinement       
;
CAD-4 software
;
_computing_structure_solution    
;
SIR92
;
_diffrn_measurement_method       \w/2\q
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   
;
DIFABS (Walker & Stuart, 1983)
;
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_T_max  0.87

_diffrn_standards_interval_time  '3600 s'
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_diffrn_standards_decay_%        3.86

_diffrn_ambient_temperature      293
_diffrn_reflns_number            2332
_reflns_number_total             2332
_diffrn_reflns_av_R_equivalents  0.00
# Number of reflections with Friedels Law is 2332
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 2324

_diffrn_reflns_theta_min         1.524
_diffrn_reflns_theta_max         24.980
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        24.980
_diffrn_measured_fraction_theta_full 0.999

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              0
_reflns_limit_h_max              26
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_refine_diff_density_min         -0.73
_refine_diff_density_max         0.71

_refine_ls_number_reflns         1087
_refine_ls_number_parameters     209

#_refine_ls_R_factor_ref 0.0674
_refine_ls_wR_factor_ref         0.0649
_refine_ls_goodness_of_fit_ref   1.1658

#_reflns_number_all 2332
_refine_ls_R_factor_all          0.1687
_refine_ls_wR_factor_all         0.0831

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>2.50u(I)
_reflns_number_gt                1087
_refine_ls_R_factor_gt           0.0674
_refine_ls_wR_factor_gt          0.0649

_refine_ls_shift/su_max          0.000659
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2

0.910 -0.161 0.657 -0.198 0.167
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

## -------------------REFERENCES ----------------------##
_publ_section_references         
;
Walker, N., and Stuart, D. Acta Cryst, (1983) A39, 158-166

Watkin D.J. (1994),
Acta Cryst, A50, 411-437
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.

Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper
R.I. (2001) CRYSTALS
Issue 11. Chemical Crystallography Laboratory, OXFORD, UK.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical
Crystallography Laboratory, OXFORD, UK.
;

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

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_occupancy
_atom_site_adp_type
_atom_site_attached_hydrogens
K1 K 0.5000 0.41998(18) 0.2500 0.0469 1.0000 Uani .
K2 K 0.5000 0.10766(16) 0.2500 0.0413 1.0000 Uani .
S1 S 0.4050(1) 0.38533(12) 0.7562(5) 0.0408 1.0000 Uani .
S2 S 0.41039(11) 0.24778(14) 0.5329(3) 0.0376 1.0000 Uani .
S3 S 0.4111(1) 0.10505(12) 0.7499(5) 0.0382 1.0000 Uani .
F1 F 0.3268(3) 0.4946(4) 0.8216(15) 0.0977 1.0000 Uani .
F2 F 0.3054(4) 0.3822(5) 0.9468(12) 0.0937 1.0000 Uani .
F3 F 0.2932(3) 0.4004(4) 0.6534(11) 0.0692 1.0000 Uani .
F4 F 0.3418(4) 0.3342(4) 0.320(1) 0.0905 1.0000 Uani .
F5 F 0.2961(3) 0.2368(5) 0.4606(16) 0.0995 1.0000 Uani .
F6 F 0.3547(5) 0.2127(6) 0.2248(13) 0.1403 1.0000 Uani .
F7 F 0.3099(3) 0.1698(4) 0.8571(12) 0.0770 1.0000 Uani .
F8 F 0.3265(4) 0.0535(7) 0.961(2) 0.1690 1.0000 Uani .
F9 F 0.3006(3) 0.0706(5) 0.6783(16) 0.1105 1.0000 Uani .
O1 O 0.4258(3) 0.4305(4) 0.5978(14) 0.0653 1.0000 Uani .
O2 O 0.4331(4) 0.3956(5) 0.9323(15) 0.0719 1.0000 Uani .
O3 O 0.4594(4) 0.2735(4) 0.4198(13) 0.0712 1.0000 Uani .
O4 O 0.4400(3) 0.1425(4) 0.9049(11) 0.0502 1.0000 Uani .
O5 O 0.4279(3) 0.0256(4) 0.7005(12) 0.0576 1.0000 Uani .
N1 N 0.3954(4) 0.2925(4) 0.716(1) 0.0351 1.0000 Uani .
N2 N 0.4105(3) 0.1546(4) 0.5606(11) 0.0379 1.0000 Uani .
C1 C 0.3265(5) 0.4156(6) 0.797(2) 0.0477 1.0000 Uani .
C2 C 0.3455(7) 0.2571(7) 0.3723(17) 0.0667 1.0000 Uani .
C3 C 0.3320(5) 0.0987(7) 0.8202(19) 0.0504 1.0000 Uani .
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
K1 0.0561(19) 0.0518(16) 0.0328(19) 0.0000 -0.010(2) 0.0000
K2 0.0448(17) 0.0383(13) 0.041(2) 0.0000 -0.001(2) 0.0000
S1 0.0354(13) 0.0343(11) 0.0528(18) -0.0031(16) -0.0049(18) 0.001(1)
S2 0.0439(12) 0.0397(11) 0.0291(11) -0.0003(12) -0.0005(13) 0.0036(12)
S3 0.0313(11) 0.036(1) 0.0469(16) 0.0018(15) -0.0076(17) 0.003(1)
F1 0.081(5) 0.057(4) 0.156(9) -0.021(5) -0.017(6) 0.032(4)
F2 0.084(6) 0.126(6) 0.071(6) 0.021(5) 0.040(6) 0.018(5)
F3 0.037(4) 0.101(5) 0.069(5) -0.017(4) -0.019(4) 0.018(4)
F4 0.149(8) 0.075(5) 0.047(5) 0.016(4) -0.026(5) 0.021(5)
F5 0.060(4) 0.092(5) 0.147(9) 0.010(6) -0.037(6) 0.003(4)
F6 0.205(11) 0.139(8) 0.077(7) -0.072(6) -0.075(7) 0.065(8)
F7 0.055(4) 0.082(5) 0.095(6) -0.002(4) 0.009(4) 0.015(4)
F8 0.076(6) 0.19(1) 0.238(15) 0.155(11) 0.065(8) 0.029(6)
F9 0.046(4) 0.115(6) 0.170(11) -0.071(7) -0.006(6) -0.005(4)
O1 0.045(4) 0.042(4) 0.108(8) 0.018(5) 0.017(5) 0.002(3)
O2 0.059(5) 0.061(4) 0.096(7) -0.026(5) -0.044(5) 0.017(4)
O3 0.078(6) 0.064(5) 0.071(6) -0.004(4) 0.035(5) -0.003(4)
O4 0.056(5) 0.061(4) 0.034(4) -0.005(4) -0.015(4) -0.001(4)
O5 0.055(4) 0.040(4) 0.078(6) -0.003(4) -0.007(5) 0.017(3)
N1 0.051(5) 0.032(4) 0.022(5) -0.005(3) 0.001(4) -0.001(3)
N2 0.042(4) 0.040(4) 0.031(4) -0.014(4) -0.003(5) 0.004(4)
C1 0.036(6) 0.046(6) 0.061(9) -0.005(6) 0.000(6) 0.014(5)
C2 0.110(12) 0.054(7) 0.036(7) 0.002(7) -0.026(7) 0.019(8)
C3 0.042(7) 0.050(6) 0.059(9) 0.011(6) -0.009(6) -0.005(5)
_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 . O1 . 1.430(9) yes
S1 . O2 . 1.41(1) yes
S1 . N1 . 1.588(7) yes
S1 . C1 . 1.85(1) yes
S2 . O3 . 1.426(8) yes
S2 . N1 . 1.531(7) yes
S2 . N2 . 1.564(8) yes
S2 . C2 . 1.852(13) yes
S3 . O4 . 1.419(8) yes
S3 . O5 . 1.419(6) yes
S3 . N2 . 1.576(9) yes
S3 . C3 . 1.844(12) yes
F1 . C1 . 1.326(12) yes
F2 . C1 . 1.291(14) yes
F3 . C1 . 1.284(13) yes
F4 . C2 . 1.340(13) yes
F5 . C2 . 1.316(16) yes
F6 . C2 . 1.297(14) yes
F7 . C3 . 1.309(12) yes
F8 . C3 . 1.257(14) yes
F9 . C3 . 1.313(14) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . S1 . O2 . 119.2(5) yes
O1 . S1 . N1 . 114.4(5) yes
O2 . S1 . N1 . 109.8(5) yes
O1 . S1 . C1 . 106.7(5) yes
O2 . S1 . C1 . 104.7(6) yes
N1 . S1 . C1 . 99.5(5) yes
O3 . S2 . N1 . 119.9(5) yes
O3 . S2 . N2 . 111.6(4) yes
N1 . S2 . N2 . 112.1(4) yes
O3 . S2 . C2 . 103.4(6) yes
N1 . S2 . C2 . 108.0(5) yes
N2 . S2 . C2 . 99.3(5) yes
O4 . S3 . O5 . 118.7(5) yes
O4 . S3 . N2 . 115.7(4) yes
O5 . S3 . N2 . 106.3(5) yes
O4 . S3 . C3 . 104.7(5) yes
O5 . S3 . C3 . 105.5(5) yes
N2 . S3 . C3 . 104.6(5) yes
S1 . N1 . S2 . 126.7(5) yes
S2 . N2 . S3 . 128.8(5) yes
S1 . C1 . F1 . 106.6(8) yes
S1 . C1 . F2 . 110.9(8) yes
F1 . C1 . F2 . 108.6(11) yes
S1 . C1 . F3 . 112.0(8) yes
F1 . C1 . F3 . 107.7(10) yes
F2 . C1 . F3 . 110.9(10) yes
S2 . C2 . F4 . 107.5(10) yes
S2 . C2 . F5 . 110.2(8) yes
F4 . C2 . F5 . 109.0(12) yes
S2 . C2 . F6 . 108.9(10) yes
F4 . C2 . F6 . 109.4(11) yes
F5 . C2 . F6 . 111.8(13) yes
S3 . C3 . F7 . 111.3(8) yes
S3 . C3 . F8 . 110.1(9) yes
F7 . C3 . F8 . 110.2(13) yes
S3 . C3 . F9 . 109.1(9) yes
F7 . C3 . F9 . 105.9(10) yes
F8 . C3 . F9 . 110.2(12) yes
_chemical_name_common            
;
potassium salt of bis (N-
(trifluoromethylsulfonylimino))trifluoro-methanesulfonic acid
;

data_CRYSTALS_cif1
_database_code_depnum_ccdc_archive 'CCDC 257233'
_audit_creation_date             2005-18-04
_audit_creation_method           CRYSTALS_ver_12-03-99

#****************************************************************************

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

_chemical_name_systematic        # IUPAC name, in full
;
potassium solt of N-bis[N-(trifluoromethylsulfonylimido)]trifluoromethane-
sulfoximidoyl imide
;

_chemical_melting_point          120-124

_refine_ls_matrix_type           full

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   'no H atoms'

_refine_ls_hydrogen_treatment    noref

#****************************************************************************
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al 2001)
;
_computing_molecular_graphics    
;
CAMERON (Watkin et al 1996)
;
#=============================================================

_cell_length_a                   13.479(7)
_cell_angle_alpha                90
_cell_length_b                   11.203(4)
_cell_angle_beta                 90
_cell_length_c                   24.545(8)
_cell_angle_gamma                90
_cell_volume                     3706.3(26)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P b c a '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 International_Tables_Vol_IV_Table_2.2B
'K ' 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 International_Tables_Vol_IV_Table_2.2B

_cell_formula_units_Z            8
_chemical_formula_sum            ' C4 F12 K1 N3 O6 S4 '
_chemical_formula_moiety         ' C4 F12 K1 N3 O6 S4 '
_chemical_compound_source        
;
?
;
_chemical_formula_weight         581.40

_cell_measurement_reflns_used    22
_cell_measurement_theta_min      10
_cell_measurement_theta_max      11
_cell_measurement_temperature    293

_exptl_crystal_description       ' plate '
_exptl_crystal_colour            ' colourless '
_exptl_crystal_size_min          0.12
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_max          0.46

_exptl_crystal_density_diffrn    2.084
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             2272.000
_exptl_absorpt_coefficient_mu    0.884
# Sheldrick geometric definitions 0.74 0.90

_diffrn_measurement_device_type  
;
CAD4 Enraf Nonius
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
CAD4 software
;
_computing_data_reduction        
;
RC93
;
_computing_cell_refinement       
;
CAD4 software
;
_computing_structure_solution    
;
SIR92
;
_diffrn_measurement_method       \w/2\q
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   
;
Azimutal absorption correction (North et al, 1968)
;
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.90

_diffrn_standards_interval_time  '3600 s'
_diffrn_standards_interval_count 147
_diffrn_standards_number         2
_diffrn_standards_decay_%        5.31

_diffrn_ambient_temperature      293
_diffrn_reflns_number            3584
_reflns_number_total             3584
_diffrn_reflns_av_R_equivalents  2.01
# Number of reflections with Friedels Law is 3584
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 4028

_diffrn_reflns_theta_min         1.659
_diffrn_reflns_theta_max         26.956
_diffrn_measured_fraction_theta_max 0.888

_diffrn_reflns_theta_full        24.934
_diffrn_measured_fraction_theta_full 0.998

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       31
_reflns_limit_h_min              0
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              31

_refine_diff_density_min         -0.36
_refine_diff_density_max         0.45

_refine_ls_number_reflns         1645
_refine_ls_number_parameters     271

#_refine_ls_R_factor_ref 0.0401
_refine_ls_wR_factor_ref         0.0443
_refine_ls_goodness_of_fit_ref   1.1501

#_reflns_number_all 3584
_refine_ls_R_factor_all          0.1409
_refine_ls_wR_factor_all         0.0833

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                1645
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_gt          0.0443

_refine_ls_shift/su_max          0.000276
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2

0.806 0.381 0.558
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

## -------------------REFERENCES ----------------------##

_publ_section_references         
;
North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968),
Acta Cryst, A24, 351-359

Watkin D.J. (1994),
Acta Cryst, A50, 411-437
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.

Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper
R.I. (2001) CRYSTALS
Issue 11. Chemical Crystallography Laboratory, OXFORD, UK.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical
Crystallography Laboratory, OXFORD, UK.
;

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

# Replace trailing . with the number of unfound
# hydrogen atoms attaced to relavent atom

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_occupancy
_atom_site_adp_type
_atom_site_attached_hydrogens
K1 K 0.25256(9) -0.28843(11) 0.29422(5) 0.0509 1.0000 Uani .
S1 S -0.00167(12) 0.02728(14) 0.24587(7) 0.0520 1.0000 Uani .
S2 S -0.1042(1) -0.09745(14) 0.32652(6) 0.0496 1.0000 Uani .
S3 S 0.0328(1) -0.19238(13) 0.39913(5) 0.0447 1.0000 Uani .
S4 S 0.1785(1) -0.01657(13) 0.39171(6) 0.0452 1.0000 Uani .
F1 F 0.0417(3) -0.0319(4) 0.14694(17) 0.0979 1.0000 Uani .
F2 F -0.0526(3) -0.1566(4) 0.18696(18) 0.0941 1.0000 Uani .
F3 F 0.1011(3) -0.1489(4) 0.2072(2) 0.1075 1.0000 Uani .
F4 F -0.2129(4) 0.0977(5) 0.3272(2) 0.1128 1.0000 Uani .
F5 F -0.2359(5) -0.0137(6) 0.3932(2) 0.1379 1.0000 Uani .
F6 F -0.1066(5) 0.0887(6) 0.3902(3) 0.1863 1.0000 Uani .
F7 F -0.0500(4) -0.3551(4) 0.45953(18) 0.0953 1.0000 Uani .
F8 F -0.0636(4) -0.1779(4) 0.49136(18) 0.1013 1.0000 Uani .
F9 F 0.0752(4) -0.2686(5) 0.49530(17) 0.1014 1.0000 Uani .
F11 F 0.3551(3) -0.0144(5) 0.4334(2) 0.1005 1.0000 Uani .
F12 F 0.2666(3) -0.1610(4) 0.4581(2) 0.1067 1.0000 Uani .
F13 F 0.2411(4) 0.0090(6) 0.49090(17) 0.1227 1.0000 Uani .
O1 O -0.0942(3) 0.0795(4) 0.23106(19) 0.0754 1.0000 Uani .
O2 O 0.0847(3) 0.0977(4) 0.24763(19) 0.0790 1.0000 Uani .
O3 O -0.1795(3) -0.1471(4) 0.29298(18) 0.0626 1.0000 Uani .
O4 O 0.0933(3) -0.2801(4) 0.37430(17) 0.0602 1.0000 Uani .
O5 O 0.1711(3) 0.1099(4) 0.38920(19) 0.0665 1.0000 Uani .
O6 O 0.2189(3) -0.0768(4) 0.34610(17) 0.0600 1.0000 Uani .
N1 N -0.0073(3) -0.0490(5) 0.3008(2) 0.0583 1.0000 Uani .
N2 N -0.0744(3) -0.1810(5) 0.3738(2) 0.0571 1.0000 Uani .
N3 N 0.0773(3) -0.0697(4) 0.41447(18) 0.0457 1.0000 Uani .
C1 C 0.0241(4) -0.0843(6) 0.1941(3) 0.0607 1.0000 Uani .
C2 C -0.1653(6) 0.0303(8) 0.3609(4) 0.0796 1.0000 Uani .
C3 C -0.0055(5) -0.2528(7) 0.4666(3) 0.0672 1.0000 Uani .
C4 C 0.2647(5) -0.0470(7) 0.4475(3) 0.0645 1.0000 Uani .
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
K1 0.0411(6) 0.0558(8) 0.0559(7) -0.0024(7) 0.0046(7) -0.0046(6)
S1 0.0488(8) 0.0539(8) 0.0532(8) 0.0119(8) -0.0097(6) -0.0062(8)
S2 0.0342(7) 0.0586(9) 0.0559(9) 0.0045(8) -0.0051(7) -0.0046(7)
S3 0.0400(7) 0.0537(9) 0.0405(7) 0.0053(7) 0.0060(6) 0.0009(6)
S4 0.0429(7) 0.0506(9) 0.0422(7) 0.0015(7) -0.0028(7) -0.0024(7)
F1 0.110(3) 0.119(4) 0.065(3) 0.004(3) 0.022(3) -0.014(3)
F2 0.076(3) 0.102(3) 0.104(3) -0.035(3) 0.014(2) -0.032(2)
F3 0.074(3) 0.104(3) 0.145(4) -0.002(3) 0.010(3) 0.034(3)
F4 0.106(3) 0.129(4) 0.103(4) 0.006(3) 0.005(3) 0.068(3)
F5 0.141(5) 0.180(6) 0.093(3) -0.005(4) 0.051(4) 0.041(4)
F6 0.136(5) 0.147(5) 0.276(9) -0.148(6) -0.098(6) 0.060(4)
F7 0.113(4) 0.082(3) 0.091(3) 0.028(3) 0.029(3) -0.019(3)
F8 0.116(4) 0.109(4) 0.079(3) 0.008(3) 0.055(3) 0.021(3)
F9 0.097(3) 0.143(4) 0.065(3) 0.038(3) -0.011(2) -0.001(3)
F11 0.054(2) 0.136(4) 0.112(3) 0.022(3) -0.031(2) -0.024(3)
F12 0.094(3) 0.089(3) 0.138(4) 0.042(3) -0.055(3) -0.002(3)
F13 0.124(4) 0.191(6) 0.053(2) -0.033(3) -0.027(3) 0.023(4)
O1 0.072(3) 0.087(3) 0.067(3) 0.017(3) -0.004(2) 0.031(3)
O2 0.084(3) 0.079(3) 0.074(3) 0.019(3) -0.014(3) -0.042(3)
O3 0.041(2) 0.081(3) 0.065(3) -0.003(2) -0.011(2) -0.009(2)
O4 0.057(2) 0.060(3) 0.063(3) -0.008(2) 0.018(2) 0.001(2)
O5 0.070(3) 0.050(3) 0.080(3) 0.014(2) -0.006(3) -0.005(2)
O6 0.053(2) 0.078(3) 0.050(2) -0.009(2) 0.0104(19) -0.012(2)
N1 0.038(3) 0.073(3) 0.064(3) 0.016(3) -0.011(2) -0.014(2)
N2 0.043(3) 0.064(3) 0.064(3) 0.022(3) 0.002(2) -0.011(2)
N3 0.042(2) 0.053(3) 0.043(2) -0.007(2) 0.008(2) 0.000(2)
C1 0.039(4) 0.074(4) 0.068(4) -0.001(4) -0.001(3) -0.010(3)
C2 0.060(4) 0.092(6) 0.087(5) -0.027(5) -0.011(4) 0.018(4)
C3 0.068(4) 0.081(5) 0.053(4) 0.016(4) 0.014(4) 0.004(5)
C4 0.054(4) 0.078(5) 0.061(4) 0.005(4) -0.017(3) -0.005(4)
_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 . O1 . 1.425(5) yes
S1 . O2 . 1.408(4) yes
S1 . N1 . 1.598(5) yes
S1 . C1 . 1.816(7) yes
S2 . O3 . 1.419(4) yes
S2 . N1 . 1.550(5) yes
S2 . N2 . 1.544(5) yes
S2 . C2 . 1.854(8) yes
S3 . O4 . 1.415(4) yes
S3 . N2 . 1.578(5) yes
S3 . N3 . 1.546(5) yes
S3 . C3 . 1.862(7) yes
S4 . O5 . 1.421(4) yes
S4 . O6 . 1.416(4) yes
S4 . N3 . 1.590(4) yes
S4 . C4 . 1.828(6) yes
F1 . C1 . 1.319(8) yes
F2 . C1 . 1.326(7) yes
F3 . C1 . 1.306(7) yes
F4 . C2 . 1.292(9) yes
F5 . C2 . 1.333(9) yes
F6 . C2 . 1.253(8) yes
F7 . C3 . 1.306(8) yes
F8 . C3 . 1.298(8) yes
F9 . C3 . 1.308(8) yes
F11 . C4 . 1.319(8) yes
F12 . C4 . 1.304(8) yes
F13 . C4 . 1.276(8) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . S1 . O2 . 120.1(3) yes
O1 . S1 . N1 . 113.2(3) yes
O2 . S1 . N1 . 108.3(3) yes
O1 . S1 . C1 . 105.8(3) yes
O2 . S1 . C1 . 104.4(3) yes
N1 . S1 . C1 . 103.3(3) yes
O3 . S2 . N1 . 120.2(3) yes
O3 . S2 . N2 . 112.6(3) yes
N1 . S2 . N2 . 107.4(3) yes
O3 . S2 . C2 . 104.5(3) yes
N1 . S2 . C2 . 106.8(4) yes
N2 . S2 . C2 . 103.9(4) yes
O4 . S3 . N2 . 114.5(3) yes
O4 . S3 . N3 . 119.9(2) yes
N2 . S3 . N3 . 112.3(3) yes
O4 . S3 . C3 . 106.9(3) yes
N2 . S3 . C3 . 97.2(3) yes
N3 . S3 . C3 . 102.3(3) yes
O5 . S4 . O6 . 117.9(3) yes
O5 . S4 . N3 . 109.2(3) yes
O6 . S4 . N3 . 115.4(2) yes
O5 . S4 . C4 . 105.2(3) yes
O6 . S4 . C4 . 105.0(3) yes
N3 . S4 . C4 . 102.2(3) yes
S1 . N1 . S2 . 124.8(3) yes
S2 . N2 . S3 . 125.7(3) yes
S3 . N3 . S4 . 125.5(3) yes
S1 . C1 . F1 . 110.0(5) yes
S1 . C1 . F2 . 111.3(4) yes
F1 . C1 . F2 . 107.2(6) yes
S1 . C1 . F3 . 111.2(5) yes
F1 . C1 . F3 . 108.7(6) yes
F2 . C1 . F3 . 108.3(6) yes
S2 . C2 . F4 . 112.3(6) yes
S2 . C2 . F5 . 107.6(6) yes
F4 . C2 . F5 . 104.0(6) yes
S2 . C2 . F6 . 112.6(5) yes
F4 . C2 . F6 . 112.1(8) yes
F5 . C2 . F6 . 107.6(8) yes
S3 . C3 . F7 . 109.1(5) yes
S3 . C3 . F8 . 110.4(5) yes
F7 . C3 . F8 . 110.6(6) yes
S3 . C3 . F9 . 107.3(5) yes
F7 . C3 . F9 . 109.5(6) yes
F8 . C3 . F9 . 109.7(7) yes
S4 . C4 . F11 . 109.8(5) yes
S4 . C4 . F12 . 110.2(5) yes
F11 . C4 . F12 . 107.8(6) yes
S4 . C4 . F13 . 112.1(5) yes
F11 . C4 . F13 . 108.3(6) yes
F12 . C4 . F13 . 108.6(7) yes
_chemical_name_common            
;
potassium solt of N-bis(N-
(trifluoromethylsulfonylimido))trifluoromethane-sulfoximidoyl imide
;