# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'W Levason'
_publ_contact_author_email       WXL@SOTON.AC.UK

_publ_section_title              
;
Isolation and structures of sulfonium salts derived
from thioethers: [{o-C6H4(CH2SMe)2}H][NbF6] and [{[9]aneS3}H][NbF6]
;
loop_
_publ_author_name
'W Levason'
'Marek Jura'
'Gillian Reid'
'Michael Webster'

# Attachment 'SH_all3_a.cif'

# Manuscript ref.:
# Title: Isolation and structures of sulfonium salts derived from
# dialkylthioethers: [{o-C6H4(CH2SMe)2}H][NbF6] and
# [{[9]aneS3}H][NbF6]
# Authors: M. Jura, W. Levason, G. Reid, M. Webster
# Journal (proposed): Chem. Commun.
# CCDC ref. no(s).:
# DOI:
#
##############################################################################
### CIF submission form for molecular structure report ###
### Version: 2.0.2 (6 July 1998). (Updated 20-Apr-2005) ###
##############################################################################

# This is an electronic "form" for submitting structural details as a
# Crystallographic Information File (CIF).
# Full details of the format of such files are given in the paper "The
# Crystallographic Information File (CIF): a New Standard Archive File for
# Crystallography" by S. R. Hall, F. H. Allen and I. D. Brown [Acta Cryst.
# (1991), A47, 655-685].
#
# The current version of the core CIF dictionary is obtainable from
# www.iucr.org
#
# CIFs can be checked for legal syntax and possible errors (ALERTS) by
# using checkcif software at:
# http://journals.iucr.org/services/cif/checkcif.html
# http://journals.iucr.org/services/cif/checking/checkstructural.html
# http://checkcif.iucr.org (produces o/p in pdf or html format).
#
#==============================================================================
data_09mj01
_database_code_depnum_ccdc_archive 'CCDC 733488'

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2009-02-11
_audit_author_name               'Webster, M.'
_audit_update_record             
'2009-05-12 Added comment about H2 in _refine_special_details'

_chemical_name_systematic        
;
methyl{2-[(methylthio)methyl]benzyl}sulfonium hexafluoroniobate(V)
;

# ACD iLab IUPAC cation name
# methyl{2-[(methylthio)methyl]benzyl}sulfonium

_chemical_name_common            
;methyl(2-((methylthio)methyl)benzyl)sulfonium
hexafluoroniobate(V)
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H15 S2 1+, F6 Nb 1-'
_chemical_formula_sum            'C10 H15 F6 Nb S2'
_chemical_formula_weight         406.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_space_group_IT_number           14
_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                   8.5866(10)
_cell_length_b                   16.986(3)
_cell_length_c                   9.8782(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.392(10)
_cell_angle_gamma                90.00
_cell_volume                     1440.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    14112
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6989 # 0.8916
_exptl_absorpt_correction_T_max  1.0000 # 0.9769
_exptl_absorpt_process_details   
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14631
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.93
_diffrn_reflns_theta_max         27.53
_reflns_number_total             3261
_reflns_number_gt                2746
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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.

The H atom bonded to the S was added in the final stages of refinement.
Of the Shelxl difference Fourier peaks only Q4 and Q9 had suitable S-H
distances (Q9 was rather short at 0.82 Ang from S1), and looking at the
C-S-Q angles it was clear that the larger Q4 peak gave much better
values. Q4 was chosen to add to the model (as H2), and supported
by the H-bonding interaction to S1.
The H atom x,y,z was refined with a fixed Uiso value.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+6.2834P] 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 # constr # H2 xyz refined, U fixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3261
_refine_ls_number_parameters     177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1012
_refine_ls_wR_factor_gt          0.0931
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Nb1 Nb 0.01238(4) 0.37659(2) 0.81889(4) 0.01949(12) Uani 1 1 d . . .
S1 S 0.40202(12) 0.25346(6) 1.03545(10) 0.0218(2) Uani 1 1 d . . .
S2 S 0.11919(11) 0.12073(6) 0.91730(10) 0.0213(2) Uani 1 1 d . . .
F1 F -0.1320(4) 0.3351(2) 0.6924(3) 0.0589(10) Uani 1 1 d . . .
F2 F 0.1759(3) 0.33370(17) 0.7173(3) 0.0356(6) Uani 1 1 d . . .
F3 F -0.0055(3) 0.28306(17) 0.9192(3) 0.0393(7) Uani 1 1 d . . .
F4 F -0.1483(4) 0.42270(19) 0.9153(4) 0.0511(9) Uani 1 1 d . . .
F5 F 0.0262(3) 0.46815(16) 0.7108(3) 0.0380(7) Uani 1 1 d . . .
F6 F 0.1617(4) 0.4138(2) 0.9424(3) 0.0424(7) Uani 1 1 d . . .
C1 C 0.5126(6) 0.3067(3) 0.9126(5) 0.0303(10) Uani 1 1 d . . .
H1A H 0.6205 0.3124 0.9457 0.046 Uiso 1 1 calc R . .
H1B H 0.4666 0.3589 0.8984 0.046 Uiso 1 1 calc R . .
H1C H 0.5108 0.2777 0.8267 0.046 Uiso 1 1 calc R . .
C2 C 0.5166(5) 0.1635(3) 1.0537(4) 0.0219(8) Uani 1 1 d . . .
H2A H 0.6215 0.1773 1.0900 0.026 Uiso 1 1 calc R . .
H2B H 0.4667 0.1290 1.1208 0.026 Uiso 1 1 calc R . .
C3 C 0.5342(5) 0.1182(2) 0.9244(4) 0.0209(8) Uani 1 1 d . . .
C4 C 0.6686(5) 0.1303(3) 0.8497(4) 0.0260(9) Uani 1 1 d . . .
H4 H 0.7460 0.1659 0.8828 0.031 Uiso 1 1 calc R . .
C5 C 0.6910(5) 0.0911(3) 0.7275(5) 0.0300(10) Uani 1 1 d . . .
H5 H 0.7816 0.1011 0.6768 0.036 Uiso 1 1 calc R . .
C6 C 0.5807(5) 0.0376(3) 0.6802(4) 0.0274(9) Uani 1 1 d . . .
H6 H 0.5964 0.0097 0.5983 0.033 Uiso 1 1 calc R . .
C7 C 0.4477(5) 0.0250(3) 0.7533(4) 0.0255(9) Uani 1 1 d . . .
H7 H 0.3720 -0.0114 0.7202 0.031 Uiso 1 1 calc R . .
C8 C 0.4218(5) 0.0645(2) 0.8745(4) 0.0208(8) Uani 1 1 d . . .
C9 C 0.2736(5) 0.0479(2) 0.9476(4) 0.0228(8) Uani 1 1 d . . .
H9A H 0.2977 0.0456 1.0461 0.027 Uiso 1 1 calc R . .
H9B H 0.2343 -0.0045 0.9194 0.027 Uiso 1 1 calc R . .
C10 C 0.1244(5) 0.1361(3) 0.7381(4) 0.0247(9) Uani 1 1 d . . .
H10A H 0.2283 0.1544 0.7138 0.037 Uiso 1 1 calc R . .
H10B H 0.0467 0.1757 0.7113 0.037 Uiso 1 1 calc R . .
H10C H 0.1011 0.0865 0.6911 0.037 Uiso 1 1 calc R . .
H2 H 0.204(7) 0.181(4) 0.959(6) 0.050 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
Nb1 0.0209(2) 0.01765(19) 0.02006(19) 0.00123(14) 0.00246(13) 0.00258(14)
S1 0.0241(5) 0.0204(5) 0.0210(5) -0.0020(4) 0.0016(4) -0.0007(4)
S2 0.0202(5) 0.0232(5) 0.0204(5) 0.0008(4) 0.0014(4) 0.0010(4)
F1 0.0433(19) 0.084(3) 0.0484(19) 0.0000(19) -0.0144(15) -0.0238(18)
F2 0.0357(15) 0.0394(16) 0.0322(14) -0.0023(12) 0.0119(11) 0.0100(12)
F3 0.0438(16) 0.0252(14) 0.0493(17) 0.0134(12) 0.0108(13) 0.0027(12)
F4 0.0515(19) 0.0372(17) 0.066(2) 0.0092(15) 0.0337(16) 0.0200(15)
F5 0.0466(16) 0.0270(14) 0.0407(16) 0.0140(12) 0.0089(13) 0.0070(12)
F6 0.0471(17) 0.056(2) 0.0240(14) -0.0032(13) -0.0019(12) -0.0166(15)
C1 0.035(2) 0.027(2) 0.029(2) 0.0022(18) 0.0076(19) 0.0005(19)
C2 0.022(2) 0.026(2) 0.0181(18) -0.0002(16) -0.0041(15) 0.0053(16)
C3 0.022(2) 0.021(2) 0.0190(18) 0.0022(16) -0.0024(15) 0.0042(16)
C4 0.020(2) 0.029(2) 0.029(2) -0.0003(18) -0.0012(16) 0.0016(17)
C5 0.023(2) 0.038(3) 0.029(2) 0.0020(19) 0.0041(17) 0.0067(19)
C6 0.031(2) 0.025(2) 0.026(2) -0.0061(18) 0.0036(17) 0.0080(18)
C7 0.029(2) 0.022(2) 0.024(2) -0.0054(17) -0.0019(17) 0.0048(17)
C8 0.022(2) 0.022(2) 0.0189(19) 0.0009(16) 0.0004(15) 0.0057(16)
C9 0.023(2) 0.021(2) 0.025(2) 0.0030(16) 0.0022(16) 0.0022(16)
C10 0.029(2) 0.026(2) 0.0191(19) 0.0068(16) 0.0001(16) -0.0014(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
Nb1 F6 1.859(3) . ?
Nb1 F4 1.867(3) . ?
Nb1 F1 1.876(3) . ?
Nb1 F3 1.881(3) . ?
Nb1 F2 1.891(2) . ?
Nb1 F5 1.892(3) . ?
S1 C1 1.803(4) . ?
S1 C2 1.824(4) . ?
S2 C10 1.791(4) . ?
S2 C9 1.833(4) . ?
S2 H2 1.32(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.501(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.401(6) . ?
C3 C8 1.408(6) . ?
C4 C5 1.396(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.395(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.505(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

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
F6 Nb1 F4 91.66(16) . . ?
F6 Nb1 F1 177.30(17) . . ?
F4 Nb1 F1 90.75(17) . . ?
F6 Nb1 F3 90.30(14) . . ?
F4 Nb1 F3 90.84(13) . . ?
F1 Nb1 F3 88.45(16) . . ?
F6 Nb1 F2 88.27(13) . . ?
F4 Nb1 F2 177.70(13) . . ?
F1 Nb1 F2 89.37(15) . . ?
F3 Nb1 F2 91.45(13) . . ?
F6 Nb1 F5 92.23(14) . . ?
F4 Nb1 F5 90.02(13) . . ?
F1 Nb1 F5 88.98(16) . . ?
F3 Nb1 F5 177.30(14) . . ?
F2 Nb1 F5 87.69(12) . . ?
C1 S1 C2 101.3(2) . . ?
C10 S2 C9 103.0(2) . . ?
C10 S2 H2 100(3) . . ?
C9 S2 H2 95(3) . . ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
S1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 S1 114.3(3) . . ?
C3 C2 H2A 108.7 . . ?
S1 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
S1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C4 C3 C8 118.5(4) . . ?
C4 C3 C2 118.3(4) . . ?
C8 C3 C2 123.2(4) . . ?
C5 C4 C3 121.2(4) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C6 C5 C4 119.8(4) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C7 C6 C5 119.5(4) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 121.7(4) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C7 C8 C3 119.3(4) . . ?
C7 C8 C9 118.4(4) . . ?
C3 C8 C9 122.3(4) . . ?
C8 C9 S2 114.3(3) . . ?
C8 C9 H9A 108.7 . . ?
S2 C9 H9A 108.7 . . ?
C8 C9 H9B 108.7 . . ?
S2 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
S2 C10 H10A 109.5 . . ?
S2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
S2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
S2 H2 S1 1.32(6) 2.22(6) 3.4936(15) 162(4) .

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.126

#===END OF CIF ==============================================================
# 09mj18d.cif

data_09mj18
_database_code_depnum_ccdc_archive 'CCDC 733489'

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2009-04-20
_audit_author_name               'Webster, M.'
_audit_update_record             
'2009-05-12 Added comment about H1 in _refine_special_details'

_chemical_name_systematic        
;
1,4,7-trithionan-1-ium hexafluoroniobate(V)
;

# S cation: 1,4,7-trithionan-1-ium (iLab name)

_chemical_name_common            '1,4,7-trithionan-1-ium hexafluoroniobate(V)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H13 S3 1+, F6 Nb 1-'
_chemical_formula_sum            'C6 H13 F6 Nb S3'
_chemical_formula_weight         388.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_space_group_IT_number           14
_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                   12.0262(15)
_cell_length_b                   9.8162(10)
_cell_length_c                   11.3884(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.929(5)
_cell_angle_gamma                90.00
_cell_volume                     1286.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9822
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6743 # 0.8673
_exptl_absorpt_correction_T_max  0.7456 # 0.9713
_exptl_absorpt_process_details   
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18517
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.11
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2948
_reflns_number_gt                2706
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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.

The H atom bonded to S1 was added in the final stages of refinement.
The Shelxl difference Fourier peak Q1 was the only plausible peak
judged by the S-H distance and the C-S-H angles, and supported
by the H-bonding interactions to adjacent ring S atoms. The H atom
x,y,z was refined with a fixed Uiso value.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+1.0913P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom # H1 from final difference map
_refine_ls_hydrogen_treatment    mixed # C H-atoms constr, H1 refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2948
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0663
_refine_ls_wR_factor_gt          0.0643
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Nb1 Nb 0.674670(16) 0.582814(19) 0.207329(16) 0.01406(8) Uani 1 1 d . . .
F1 F 0.57188(13) 0.72190(15) 0.12864(13) 0.0288(3) Uani 1 1 d . . .
F2 F 0.68550(13) 0.66466(14) 0.36066(12) 0.0272(3) Uani 1 1 d . . .
F3 F 0.55043(12) 0.47534(15) 0.22820(13) 0.0253(3) Uani 1 1 d . . .
F4 F 0.65815(13) 0.49568(15) 0.05621(12) 0.0264(3) Uani 1 1 d . . .
F5 F 0.80197(13) 0.68615(15) 0.19350(14) 0.0303(3) Uani 1 1 d . . .
F6 F 0.77876(12) 0.44605(14) 0.29037(12) 0.0239(3) Uani 1 1 d . . .
S1 S 0.66830(5) 0.15023(5) 0.27742(4) 0.01455(12) Uani 1 1 d . . .
S2 S 0.94401(5) 0.05143(7) 0.33561(5) 0.02333(14) Uani 1 1 d . . .
S3 S 0.80806(5) 0.22380(6) 0.07181(5) 0.01753(12) Uani 1 1 d . . .
C1 C 0.70979(19) -0.0281(2) 0.30073(19) 0.0162(4) Uani 1 1 d . . .
H1A H 0.6567 -0.0754 0.3393 0.019 Uiso 1 1 calc R . .
H1B H 0.7019 -0.0715 0.2203 0.019 Uiso 1 1 calc R . .
C2 C 0.83470(19) -0.0438(2) 0.38216(19) 0.0185(4) Uani 1 1 d . . .
H2A H 0.8555 -0.1415 0.3853 0.022 Uiso 1 1 calc R . .
H2B H 0.8378 -0.0155 0.4665 0.022 Uiso 1 1 calc R . .
C3 C 0.9298(2) -0.0158(3) 0.1828(2) 0.0224(5) Uani 1 1 d . . .
H3A H 0.9982 -0.0735 0.1861 0.027 Uiso 1 1 calc R . .
H3B H 0.8598 -0.0744 0.1573 0.027 Uiso 1 1 calc R . .
C4 C 0.9202(2) 0.0959(2) 0.0866(2) 0.0210(5) Uani 1 1 d . . .
H4A H 0.9072 0.0513 0.0057 0.025 Uiso 1 1 calc R . .
H4B H 0.9960 0.1432 0.1055 0.025 Uiso 1 1 calc R . .
C5 C 0.67474(19) 0.1233(2) 0.03304(18) 0.0159(4) Uani 1 1 d . . .
H5A H 0.6313 0.1388 -0.0542 0.019 Uiso 1 1 calc R . .
H5B H 0.6948 0.0254 0.0435 0.019 Uiso 1 1 calc R . .
C6 C 0.59750(19) 0.1607(2) 0.11350(18) 0.0163(4) Uani 1 1 d . . .
H6A H 0.5292 0.0993 0.0928 0.020 Uiso 1 1 calc R . .
H6B H 0.5686 0.2548 0.0934 0.020 Uiso 1 1 calc R . .
H1 H 0.759(3) 0.188(4) 0.269(3) 0.050 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
Nb1 0.01364(12) 0.01471(12) 0.01462(12) 0.00089(7) 0.00537(8) 0.00122(7)
F1 0.0272(8) 0.0262(7) 0.0294(7) 0.0042(6) 0.0025(6) 0.0087(6)
F2 0.0389(9) 0.0236(7) 0.0205(7) -0.0043(6) 0.0109(6) 0.0001(6)
F3 0.0182(7) 0.0293(7) 0.0298(7) 0.0016(6) 0.0093(6) -0.0045(6)
F4 0.0320(8) 0.0296(7) 0.0178(6) -0.0027(6) 0.0076(6) 0.0026(6)
F5 0.0253(8) 0.0279(7) 0.0422(9) 0.0014(6) 0.0169(6) -0.0056(6)
F6 0.0234(8) 0.0219(7) 0.0240(7) 0.0029(6) 0.0034(6) 0.0063(6)
S1 0.0156(3) 0.0167(3) 0.0121(2) -0.00197(19) 0.00541(19) 0.00050(19)
S2 0.0137(3) 0.0394(3) 0.0153(3) 0.0024(2) 0.0017(2) -0.0029(2)
S3 0.0180(3) 0.0196(3) 0.0166(3) 0.0012(2) 0.0077(2) -0.0001(2)
C1 0.0173(11) 0.0158(10) 0.0152(10) 0.0007(8) 0.0044(8) 0.0023(8)
C2 0.0141(11) 0.0262(12) 0.0143(10) 0.0047(9) 0.0025(8) 0.0014(9)
C3 0.0172(11) 0.0310(13) 0.0202(11) 0.0016(10) 0.0075(9) 0.0070(10)
C4 0.0155(12) 0.0308(13) 0.0188(11) 0.0003(9) 0.0082(9) 0.0030(9)
C5 0.0148(11) 0.0193(10) 0.0116(9) -0.0002(8) 0.0006(8) 0.0012(8)
C6 0.0148(10) 0.0201(10) 0.0135(10) 0.0015(8) 0.0034(8) 0.0030(8)

_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
Nb1 F4 1.8799(13) . ?
Nb1 F5 1.8809(14) . ?
Nb1 F1 1.8842(14) . ?
Nb1 F6 1.8905(13) . ?
Nb1 F2 1.8919(13) . ?
Nb1 F3 1.8996(14) . ?
S1 H1 1.19(4) . ?
S1 C6 1.815(2) . ?
S1 C1 1.818(2) . ?
S1 H1 1.19(4) . ?
S2 C2 1.813(2) . ?
S2 C3 1.822(2) . ?
S3 C4 1.814(2) . ?
S3 C5 1.824(2) . ?
C1 C2 1.526(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.530(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.527(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?

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
# H1 S1 H1 0(3) . . ?
F4 Nb1 F5 92.31(7) . . ?
F4 Nb1 F1 90.83(6) . . ?
F5 Nb1 F1 90.38(7) . . ?
F4 Nb1 F6 90.74(6) . . ?
F5 Nb1 F6 89.33(7) . . ?
F1 Nb1 F6 178.41(6) . . ?
F4 Nb1 F2 177.14(6) . . ?
F5 Nb1 F2 90.53(7) . . ?
F1 Nb1 F2 89.46(6) . . ?
F6 Nb1 F2 88.98(6) . . ?
F4 Nb1 F3 89.12(6) . . ?
F5 Nb1 F3 177.40(6) . . ?
F1 Nb1 F3 91.77(6) . . ?
F6 Nb1 F3 88.48(6) . . ?
F2 Nb1 F3 88.03(6) . . ?
H1 S1 C6 93.8(16) . . ?
H1 S1 C1 95.1(17) . . ?
C6 S1 C1 103.36(10) . . ?
C6 S1 H1 93.8(16) . . ?
C1 S1 H1 95.1(17) . . ?
C2 S2 C3 102.60(11) . . ?
C4 S3 C5 103.03(11) . . ?
C2 C1 S1 111.44(15) . . ?
C2 C1 H1A 109.3 . . ?
S1 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
S1 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 S2 116.07(15) . . ?
C1 C2 H2A 108.3 . . ?
S2 C2 H2A 108.3 . . ?
C1 C2 H2B 108.3 . . ?
S2 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?
C4 C3 S2 112.98(17) . . ?
C4 C3 H3A 109.0 . . ?
S2 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
S2 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 S3 117.50(17) . . ?
C3 C4 H4A 107.9 . . ?
S3 C4 H4A 107.9 . . ?
C3 C4 H4B 107.9 . . ?
S3 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
C6 C5 S3 111.75(15) . . ?
C6 C5 H5A 109.3 . . ?
S3 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
S3 C5 H5B 109.3 . . ?
H5A C5 H5B 107.9 . . ?
C5 C6 S1 114.74(15) . . ?
C5 C6 H6A 108.6 . . ?
S1 C6 H6A 108.6 . . ?
C5 C6 H6B 108.6 . . ?
S1 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
H1 S1 C1 C2 39.0(16) . . . . ?
C6 S1 C1 C2 134.09(16) . . . . ?
S1 C1 C2 S2 -52.6(2) . . . . ?
C3 S2 C2 C1 -59.75(19) . . . . ?
C2 S2 C3 C4 130.47(17) . . . . ?
S2 C3 C4 S3 -53.8(2) . . . . ?
C5 S3 C4 C3 -59.4(2) . . . . ?
C4 S3 C5 C6 130.88(16) . . . . ?
S3 C5 C6 S1 -54.52(19) . . . . ?
H1 S1 C6 C5 35.2(17) . . . . ?
C1 S1 C6 C5 -60.96(18) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
S1 H1 S2 1.19(4) 2.51(4) 3.3308(9) 124(2) .
S1 H1 S3 1.19(4) 2.50(4) 3.3350(8) 125(2) .
S1 H1 F6 1.19(4) 2.55(3) 3.1788(15) 111(2) .

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.094

#===END OF CIF ==============================================================
# 09mj17d.cif

data_09mj17
_database_code_depnum_ccdc_archive 'CCDC 733490'

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2008-05-11
_audit_author_name               'Webster, M.'
_audit_update_record             
'2009-05-12 Added comment about refinement in _refine_special_details'

_chemical_name_systematic        
;
catena-(tetrafluorobis(\m-1,2-bis(methylthiomethyl)benzene-S,S')niobium(V))
undecafluoro-diniobate(V) dichloromethane solvate
;

_chemical_name_common            
;
catena-(tetrafluorobis(mu-1,2-bis(methylthiomethyl)benzene-
S,S')niobium(V)) undecafluoro-diniobate(V) dichloromethane solvate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H28 F4 Nb S4 1+, F11 Nb2 1-, C H2 Cl2'
_chemical_formula_sum            'C21 H30 Cl2 F15 Nb3 S4'
_chemical_formula_structural     
'((C6 H4 (C2 H5 S)2)2 Nb F4) (Nb2 F11) (C H2 Cl2)'
_chemical_formula_weight         1045.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5263(10)
_cell_length_b                   13.3180(15)
_cell_length_c                   14.3186(15)
_cell_angle_alpha                114.254(6)
_cell_angle_beta                 109.892(6)
_cell_angle_gamma                97.279(6)
_cell_volume                     1946.5(4) # shelxl (3)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    66433
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024
_exptl_absorpt_coefficient_mu    1.306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7935 #
_exptl_absorpt_correction_T_max  1.0000 #
_exptl_absorpt_process_details   
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39177
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.64
_diffrn_reflns_theta_max         27.77
_reflns_number_total             8948
_reflns_number_gt                7883
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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.

The normalised structure factors supported a centric distribution and
solution proceeded in Pbar1 (no. 2). The Rint was low (0.038) and the
simulated photographs of key zones from the data collection showed
no odd features. The sulfur ligands together with the bonded Nb atom
and the four F atoms bonded to Nb1 readily emerged from a
TREF command in SHELXS together with other potential Nb atoms.

The required counter ions and possible solvate proved troublesome.
One [Nb2F11]- was located with the bridging F atom positioned on
a centre of symmetry. The Nb2--F(bridge) distance was, as expected,
longer than the Nb2--F terminal bonds. Refinement gave very elongated
ellipsoids to terminal F atoms indicative of disorder.

The second anion (required for charge balance) proved
more troublesome. The Nb3...Nb4 distance (4.03 \%A) was in good
agreement with the first anion value (4.02 \%A) and a difference
electron-density map showed a number of plausible F atoms. It was
quickly realized that Nb3 and Nb4 required a sof of 0.5 if we were
seeking an Nb2F11 anion on two grounds (overall charge balance, and
too close contact to a centrosymmetrically related anion).
The possibility of overlapping NbF6 and Nb2F11 ions was explored by
allowing the Nb sofs to vary (the sum remaining 1.0), but these
refined to values close to 0.5.

Introducing the required F atoms (all with sof 0.5, and isotropic
adp) gave a fairly convincing geometry, but numerous attempts at
refinement with either isotropic or anisotropic adp's for the F
atoms saw the geometry become unreasonable even with the inclusion
of an assortment of DFIX commands, and the appearance of several
new large Q peaks in the difference map near the F atoms. R1
remained stubbornly at ca. 0.12

In addition there were four large peaks forming an isolated
group some distance from the anion which were assigned
to Cl of disordered CH2Cl2 solvate molecules with two
distances close to the Cl...Cl expected for CH2Cl2 and these were
introduced into the model with a refined sof. Plausible
bonded C atoms were later identified in the e/d map.

The strategy finally adopted introduced all the potential F atoms
gradually with a fixed Uiso and refined sof. Because of the very
smeared out nature of the electron density, the maximum found in the
peak search was in some cases displaced from the expected
position although the Nb-F distances were reasonable in all cases.
The sofs were finally adjusted by hand to provide the correct number
of F atoms, the values fixed, and the Uiso and x,y,z coordinates
allowed to refine to convergence.

The solution in P1 was also examined but it soon became clear
that the same structure was emerging with the cation chain being similar
to the Pbar1 solution. This solution was not pursued.

Although the structure refinement is unsatisfactory with regards
to one of the anions the chain cation seems sound.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+28.2339P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8948
_refine_ls_number_parameters     443
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0857
_refine_ls_wR_factor_ref         0.2099
_refine_ls_wR_factor_gt          0.2026
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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
Nb1 Nb 0.47649(5) 0.18991(5) 0.29114(5) 0.02012(15) Uani 1 1 d . . .
Nb2 Nb 0.41632(9) -0.65439(8) -0.14282(11) 0.0627(3) Uani 1 1 d . . .
Nb3 Nb 1.04744(13) 0.06284(15) 0.79768(12) 0.0393(4) Uani 0.50 1 d P . .
Nb4 Nb 0.83539(15) 0.04184(14) 0.50227(13) 0.0387(3) Uani 0.50 1 d P . .
S1 S 0.33435(15) 0.33058(15) 0.30230(15) 0.0252(3) Uani 1 1 d . . .
S2 S 0.48754(15) 0.68417(15) 0.48779(14) 0.0253(3) Uani 1 1 d . . .
S3 S 0.42608(15) -0.04511(14) 0.15624(14) 0.0254(3) Uani 1 1 d . . .
S4 S 0.36507(18) -0.15322(17) -0.19611(17) 0.0312(4) Uani 1 1 d . . .
F1 F 0.5811(3) 0.3378(3) 0.3462(3) 0.0253(8) Uani 1 1 d . . .
F2 F 0.5895(3) 0.1425(3) 0.3773(3) 0.0242(8) Uani 1 1 d . . .
F3 F 0.3423(3) 0.1161(3) 0.2979(3) 0.0253(8) Uani 1 1 d . . .
F4 F 0.3957(4) 0.1666(3) 0.1422(3) 0.0259(8) Uani 1 1 d . . .
F5 F 0.3543(12) -0.7934(8) -0.2733(8) 0.126(4) Uani 1 1 d . . .
F6 F 0.5692(9) -0.6657(8) -0.1076(16) 0.189(8) Uani 1 1 d . . .
F7 F 0.4404(11) -0.5689(10) -0.2115(14) 0.159(6) Uani 1 1 d . . .
F8 F 0.2777(6) -0.6195(7) -0.1522(7) 0.074(2) Uani 1 1 d . . .
F9 F 0.4015(7) -0.7152(6) -0.0515(6) 0.0739(19) Uani 1 1 d . . .
F10 F 0.5000 -0.5000 0.0000 0.140(7) Uani 1 2 d S . .
C1 C 0.1931(7) 0.2352(8) 0.1837(8) 0.043(2) Uani 1 1 d . . .
H1A H 0.1549 0.1819 0.2023 0.064 Uiso 1 1 calc R . .
H1B H 0.2061 0.1908 0.1168 0.064 Uiso 1 1 calc R . .
H1C H 0.1414 0.2811 0.1676 0.064 Uiso 1 1 calc R . .
C2 C 0.3866(6) 0.4188(6) 0.2479(6) 0.0235(13) Uani 1 1 d . . .
H2A H 0.4648 0.4767 0.3074 0.028 Uiso 1 1 calc R . .
H2B H 0.3993 0.3684 0.1818 0.028 Uiso 1 1 calc R . .
C3 C 0.3018(6) 0.4819(6) 0.2119(6) 0.0233(13) Uani 1 1 d . . .
C4 C 0.2499(6) 0.4484(6) 0.0961(6) 0.0256(13) Uani 1 1 d . . .
H4 H 0.2645 0.3856 0.0445 0.031 Uiso 1 1 calc R . .
C5 C 0.1776(7) 0.5051(7) 0.0555(6) 0.0308(15) Uani 1 1 d . . .
H5 H 0.1444 0.4827 -0.0231 0.037 Uiso 1 1 calc R . .
C6 C 0.1538(6) 0.5950(7) 0.1300(7) 0.0317(15) Uani 1 1 d . . .
H6 H 0.1036 0.6341 0.1028 0.038 Uiso 1 1 calc R . .
C7 C 0.2038(6) 0.6275(6) 0.2448(7) 0.0286(14) Uani 1 1 d . . .
H7 H 0.1876 0.6896 0.2957 0.034 Uiso 1 1 calc R . .
C8 C 0.2768(6) 0.5714(6) 0.2870(6) 0.0229(13) Uani 1 1 d . . .
C9 C 0.3263(6) 0.6123(6) 0.4129(5) 0.0232(13) Uani 1 1 d . . .
H9A H 0.3079 0.5450 0.4245 0.028 Uiso 1 1 calc R . .
H9B H 0.2860 0.6668 0.4463 0.028 Uiso 1 1 calc R . .
C10 C 0.5007(8) 0.7927(7) 0.4440(7) 0.0384(18) Uani 1 1 d . . .
H10A H 0.5848 0.8385 0.4792 0.058 Uiso 1 1 calc R . .
H10B H 0.4543 0.8436 0.4680 0.058 Uiso 1 1 calc R . .
H10C H 0.4700 0.7547 0.3611 0.058 Uiso 1 1 calc R . .
C11 C 0.3676(9) -0.1088(7) 0.2243(7) 0.0407(19) Uani 1 1 d . . .
H11A H 0.4329 -0.0957 0.2940 0.061 Uiso 1 1 calc R . .
H11B H 0.3291 -0.1922 0.1728 0.061 Uiso 1 1 calc R . .
H11C H 0.3089 -0.0731 0.2434 0.061 Uiso 1 1 calc R . .
C12 C 0.2914(6) -0.0791(6) 0.0319(6) 0.0249(13) Uani 1 1 d . . .
H12A H 0.2361 -0.0412 0.0576 0.030 Uiso 1 1 calc R . .
H12B H 0.3130 -0.0465 -0.0124 0.030 Uiso 1 1 calc R . .
C13 C 0.2278(6) -0.2069(6) -0.0443(6) 0.0247(13) Uani 1 1 d . . .
C14 C 0.1199(7) -0.2521(7) -0.0478(6) 0.0308(15) Uani 1 1 d . . .
H14 H 0.0898 -0.2026 -0.0008 0.037 Uiso 1 1 calc R . .
C15 C 0.0543(7) -0.3700(7) -0.1198(7) 0.0373(18) Uani 1 1 d . . .
H15 H -0.0200 -0.3995 -0.1218 0.045 Uiso 1 1 calc R . .
C16 C 0.0971(8) -0.4423(7) -0.1870(7) 0.0402(19) Uani 1 1 d . . .
H16 H 0.0533 -0.5222 -0.2353 0.048 Uiso 1 1 calc R . .
C17 C 0.2059(8) -0.3978(6) -0.1842(7) 0.0354(17) Uani 1 1 d . . .
H17 H 0.2361 -0.4483 -0.2305 0.042 Uiso 1 1 calc R . .
C18 C 0.2711(6) -0.2802(6) -0.1145(5) 0.0255(13) Uani 1 1 d . . .
C19 C 0.3836(7) -0.2385(6) -0.1211(6) 0.0281(14) Uani 1 1 d . . .
H19A H 0.4069 -0.3059 -0.1615 0.034 Uiso 1 1 calc R . .
H19B H 0.4486 -0.1901 -0.0433 0.034 Uiso 1 1 calc R . .
C20 C 0.2236(7) -0.2416(10) -0.3173(8) 0.048(2) Uani 1 1 d . . .
H20A H 0.2033 -0.2048 -0.3650 0.071 Uiso 1 1 calc R . .
H20B H 0.1616 -0.2499 -0.2913 0.071 Uiso 1 1 calc R . .
H20C H 0.2287 -0.3183 -0.3614 0.071 Uiso 1 1 calc R . .
Cl1 Cl 0.9206(8) 0.5999(12) 0.6024(8) 0.094(4) Uani 0.521(8) 1 d PD A 1
Cl2 Cl 0.7340(5) 0.6076(5) 0.4251(5) 0.0699(19) Uani 0.521(8) 1 d PD A 1
C21 C 0.8902(13) 0.6351(18) 0.4965(14) 0.050 Uiso 0.521(8) 1 d PD A 1
H21A H 0.9191 0.5889 0.4417 0.060 Uiso 0.521(8) 1 calc PR A 1
H21B H 0.9325 0.7181 0.5291 0.060 Uiso 0.521(8) 1 calc PR A 1
Cl3 Cl 0.8126(6) 0.7843(6) 0.5533(6) 0.073(2) Uani 0.479(8) 1 d PD A 2
Cl4 Cl 0.8939(10) 0.5905(8) 0.5552(12) 0.095(4) Uani 0.479(8) 1 d PD A 2
C22 C 0.831(2) 0.6578(15) 0.4766(15) 0.050 Uiso 0.479(8) 1 d PD A 2
H22A H 0.8827 0.6720 0.4414 0.060 Uiso 0.479(8) 1 calc PR A 2
H22B H 0.7521 0.6038 0.4143 0.060 Uiso 0.479(8) 1 calc PR A 2
F11 F 0.9331(5) 0.1923(4) 0.5615(4) 0.0018(10) Uiso 0.50 1 d P . .
F12 F 0.7584(7) 0.0493(6) 0.5815(7) 0.0178(14) Uiso 0.50 1 d P . .
F13 F 1.0401(14) 0.1970(12) 0.8613(11) 0.038(3) Uiso 0.50 1 d P . .
F14 F 1.0818(8) -0.0301(8) 0.8398(7) 0.0325(18) Uiso 0.50 1 d P . .
F15 F 0.9289(10) 0.0794(10) 0.6678(10) 0.038(3) Uiso 0.40 1 d P . .
F16 F 0.7576(11) 0.0089(10) 0.3558(10) 0.040(3) Uiso 0.40 1 d P . .
F17 F 0.9847(11) 0.0525(11) 0.4961(11) 0.044(3) Uiso 0.40 1 d P . .
F18 F 0.8185(12) -0.1104(12) 0.4738(12) 0.049(3) Uiso 0.40 1 d P . .
F19 F 0.8828(11) 0.2003(9) 0.5584(9) 0.032(2) Uiso 0.40 1 d P . .
F20 F 0.7145(8) 0.0500(7) 0.5475(8) 0.0269(17) Uiso 0.50 1 d P . .
F21 F 0.9196(17) 0.0353(17) 0.8332(17) 0.026(4) Uiso 0.20 1 d P . .
F22 F 1.1441(19) 0.0414(18) 0.9090(18) 0.031(4) Uiso 0.20 1 d P . .
F23 F 0.988(3) -0.099(3) 0.697(3) 0.059(7) Uiso 0.20 1 d P . .
F24 F 1.081(3) 0.199(2) 0.874(2) 0.034(7) Uiso 0.20 1 d P . .
F25 F 1.013(2) 0.173(2) 0.862(2) 0.026(6) Uiso 0.20 1 d P . .

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
Nb1 0.0233(3) 0.0189(3) 0.0191(3) 0.0097(2) 0.0094(2) 0.0074(2)
Nb2 0.0536(6) 0.0422(5) 0.1108(9) 0.0393(6) 0.0522(6) 0.0174(4)
Nb3 0.0339(7) 0.0578(9) 0.0262(7) 0.0197(7) 0.0124(6) 0.0180(7)
Nb4 0.0518(9) 0.0381(8) 0.0317(7) 0.0189(6) 0.0183(7) 0.0232(7)
S1 0.0276(8) 0.0264(8) 0.0293(8) 0.0169(7) 0.0149(7) 0.0126(6)
S2 0.0239(8) 0.0266(8) 0.0211(7) 0.0085(6) 0.0093(6) 0.0073(6)
S3 0.0285(8) 0.0214(7) 0.0233(8) 0.0100(6) 0.0089(6) 0.0085(6)
S4 0.0405(10) 0.0340(9) 0.0402(10) 0.0258(8) 0.0278(8) 0.0201(8)
F1 0.0262(19) 0.0215(18) 0.029(2) 0.0121(16) 0.0128(16) 0.0058(15)
F2 0.0279(19) 0.0250(19) 0.0237(19) 0.0138(16) 0.0117(16) 0.0117(16)
F3 0.0255(19) 0.0237(19) 0.027(2) 0.0125(16) 0.0120(16) 0.0060(15)
F4 0.032(2) 0.0236(19) 0.0215(18) 0.0113(16) 0.0094(16) 0.0111(16)
F5 0.230(13) 0.076(6) 0.099(7) 0.040(5) 0.106(8) 0.043(7)
F6 0.090(6) 0.079(6) 0.45(2) 0.132(10) 0.157(11) 0.059(5)
F7 0.172(10) 0.141(9) 0.330(18) 0.179(12) 0.194(13) 0.083(8)
F8 0.047(3) 0.107(6) 0.107(6) 0.079(5) 0.039(4) 0.039(4)
F9 0.088(5) 0.073(4) 0.065(4) 0.035(4) 0.029(4) 0.044(4)
F10 0.099(9) 0.029(5) 0.174(14) 0.006(6) -0.018(9) 0.027(5)
C1 0.022(3) 0.040(4) 0.059(5) 0.028(4) 0.006(4) 0.005(3)
C2 0.023(3) 0.024(3) 0.027(3) 0.014(3) 0.012(3) 0.008(2)
C3 0.025(3) 0.024(3) 0.024(3) 0.014(3) 0.011(3) 0.006(3)
C4 0.027(3) 0.027(3) 0.018(3) 0.009(3) 0.007(3) 0.005(3)
C5 0.029(3) 0.038(4) 0.028(3) 0.022(3) 0.008(3) 0.007(3)
C6 0.027(3) 0.032(4) 0.040(4) 0.025(3) 0.009(3) 0.009(3)
C7 0.027(3) 0.029(3) 0.036(4) 0.020(3) 0.014(3) 0.011(3)
C8 0.023(3) 0.024(3) 0.022(3) 0.013(3) 0.008(2) 0.006(2)
C9 0.022(3) 0.021(3) 0.021(3) 0.007(3) 0.007(2) 0.005(2)
C10 0.047(5) 0.039(4) 0.026(4) 0.018(3) 0.016(3) -0.001(3)
C11 0.067(6) 0.026(4) 0.030(4) 0.018(3) 0.020(4) 0.009(4)
C12 0.023(3) 0.025(3) 0.027(3) 0.016(3) 0.007(3) 0.007(3)
C13 0.021(3) 0.025(3) 0.025(3) 0.012(3) 0.007(3) 0.005(3)
C14 0.029(4) 0.038(4) 0.030(4) 0.021(3) 0.012(3) 0.009(3)
C15 0.029(4) 0.039(4) 0.037(4) 0.024(4) 0.005(3) -0.002(3)
C16 0.046(5) 0.031(4) 0.030(4) 0.017(3) 0.007(3) -0.004(3)
C17 0.051(5) 0.024(3) 0.030(4) 0.013(3) 0.019(3) 0.005(3)
C18 0.035(4) 0.021(3) 0.018(3) 0.009(3) 0.011(3) 0.006(3)
C19 0.037(4) 0.029(3) 0.032(4) 0.021(3) 0.021(3) 0.015(3)
C20 0.031(4) 0.084(7) 0.058(6) 0.056(6) 0.023(4) 0.026(4)
Cl1 0.053(5) 0.165(9) 0.080(5) 0.088(6) 0.020(4) 0.005(4)
Cl2 0.055(3) 0.058(3) 0.075(4) 0.017(3) 0.026(3) 0.016(2)
Cl3 0.066(4) 0.074(4) 0.078(4) 0.035(3) 0.034(3) 0.021(3)
Cl4 0.058(5) 0.059(4) 0.145(11) 0.043(6) 0.028(7) 0.022(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
# F11 F19 0.642(11) . ?
# F12 F20 0.601(9) . ?
# F14 F22 1.00(2) . ?
Nb1 F3 1.889(4) . ?
Nb1 F4 1.891(4) . ?
Nb1 F1 1.893(4) . ?
Nb1 F2 1.897(4) . ?
Nb1 S1 2.7383(17) . ?
Nb1 S2 2.7409(18) 2_666 ?
Nb1 S4 2.7508(19) 2_655 ?
Nb1 S3 2.7620(18) . ?
Nb2 F5 1.824(9) . ?
Nb2 F8 1.829(6) . ?
Nb2 F7 1.841(9) . ?
Nb2 F9 1.844(8) . ?
Nb2 F6 1.850(8) . ?
Nb2 F10 2.0123(12) . ?
Nb3 F25 1.57(2) . ?
Nb3 F24 1.59(3) . ?
Nb3 F14 1.629(9) . ?
Nb3 F13 1.671(14) . ?
Nb3 F22 1.80(2) . ?
Nb3 F21 1.87(2) . ?
Nb3 F23 1.89(3) . ?
Nb3 F15 2.063(12) . ?
Nb4 F12 1.703(7) . ?
Nb4 F16 1.813(12) . ?
Nb4 F20 1.837(9) . ?
Nb4 F19 1.849(11) . ?
Nb4 F18 1.865(14) . ?
Nb4 F11 1.874(5) . ?
Nb4 F17 1.893(13) . ?
Nb4 F15 2.056(12) . ?
S1 C1 1.800(8) . ?
S1 C2 1.823(7) . ?
S2 C10 1.806(8) . ?
S2 C9 1.828(7) . ?
S2 Nb1 2.7409(18) 2_666 ?
S3 C11 1.792(8) . ?
S3 C12 1.822(7) . ?
S4 C20 1.799(10) . ?
S4 C19 1.842(7) . ?
S4 Nb1 2.7508(19) 2_655 ?
F10 Nb2 2.0123(12) 2_645 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.519(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C8 1.396(10) . ?
C3 C4 1.399(9) . ?
C4 C5 1.379(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.388(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.389(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.509(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.503(9) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.383(10) . ?
C13 C18 1.399(10) . ?
C14 C15 1.404(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.364(13) . ?
C15 H15 0.9500 . ?
C16 C17 1.395(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.398(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.497(10) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Cl1 C21 1.702(14) . ?
Cl2 C21 1.777(14) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
Cl3 C22 1.687(15) . ?
Cl4 C22 1.759(16) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
F14 F23 1.72(3) . ?
F17 F17 1.53(3) 2_756 ?
# F24 F25 0.80(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
_geom_angle_publ_flag
# F25 Nb3 F24 29.4(15) . . ?
# F25 Nb3 F13 15.2(10) . . ?
# F24 Nb3 F13 16.4(11) . . ?
# F14 Nb3 F22 33.6(7) . . ?
# F12 Nb4 F20 19.1(3) . . ?
F3 Nb1 F4 96.87(17) . . ?
F3 Nb1 F1 142.29(17) . . ?
F4 Nb1 F1 94.29(17) . . ?
F3 Nb1 F2 96.67(17) . . ?
F4 Nb1 F2 142.22(17) . . ?
F1 Nb1 F2 96.18(17) . . ?
F3 Nb1 S1 73.34(12) . . ?
F4 Nb1 S1 73.44(12) . . ?
F1 Nb1 S1 75.62(12) . . ?
F2 Nb1 S1 144.34(12) . . ?
F3 Nb1 S2 75.22(13) . 2_666 ?
F4 Nb1 S2 144.20(13) . 2_666 ?
F1 Nb1 S2 74.76(13) . 2_666 ?
F2 Nb1 S2 73.52(12) . 2_666 ?
S1 Nb1 S2 70.84(5) . 2_666 ?
F3 Nb1 S4 144.24(13) . 2_655 ?
F4 Nb1 S4 74.06(13) . 2_655 ?
F1 Nb1 S4 73.46(13) . 2_655 ?
F2 Nb1 S4 74.40(12) . 2_655 ?
S1 Nb1 S4 132.62(6) . 2_655 ?
S2 Nb1 S4 131.36(6) 2_666 2_655 ?
F3 Nb1 S3 73.69(13) . . ?
F4 Nb1 S3 76.82(12) . . ?
F1 Nb1 S3 144.02(13) . . ?
F2 Nb1 S3 73.48(12) . . ?
S1 Nb1 S3 131.87(6) . . ?
S2 Nb1 S3 130.92(6) 2_666 . ?
S4 Nb1 S3 70.57(6) 2_655 . ?
F5 Nb2 F8 98.7(5) . . ?
F5 Nb2 F7 94.5(6) . . ?
F8 Nb2 F7 89.1(4) . . ?
F5 Nb2 F9 95.5(4) . . ?
F8 Nb2 F9 88.8(3) . . ?
F7 Nb2 F9 170.0(5) . . ?
F5 Nb2 F6 91.7(6) . . ?
F8 Nb2 F6 169.6(6) . . ?
F7 Nb2 F6 91.1(6) . . ?
F9 Nb2 F6 89.2(6) . . ?
F5 Nb2 F10 174.4(4) . . ?
F8 Nb2 F10 86.4(3) . . ?
F7 Nb2 F10 83.3(5) . . ?
F9 Nb2 F10 86.8(2) . . ?
F6 Nb2 F10 83.2(4) . . ?
F25 Nb3 F14 126.6(10) . . ?
F24 Nb3 F14 127.6(11) . . ?
F14 Nb3 F13 134.5(6) . . ?
F25 Nb3 F22 104.5(11) . . ?
F24 Nb3 F22 95.4(12) . . ?
F13 Nb3 F22 106.1(8) . . ?
F25 Nb3 F21 64.0(12) . . ?
F24 Nb3 F21 91.7(12) . . ?
F14 Nb3 F21 81.6(7) . . ?
F13 Nb3 F21 79.2(8) . . ?
F22 Nb3 F21 91.1(9) . . ?
F25 Nb3 F23 144.4(14) . . ?
F24 Nb3 F23 172.6(14) . . ?
F14 Nb3 F23 57.8(10) . . ?
F13 Nb3 F23 156.3(11) . . ?
F22 Nb3 F23 90.7(12) . . ?
F21 Nb3 F23 84.0(11) . . ?
F25 Nb3 F15 76.3(10) . . ?
F24 Nb3 F15 86.8(11) . . ?
F14 Nb3 F15 143.6(5) . . ?
F13 Nb3 F15 75.6(6) . . ?
F22 Nb3 F15 176.7(8) . . ?
F21 Nb3 F15 86.4(7) . . ?
F23 Nb3 F15 86.9(10) . . ?
F12 Nb4 F16 120.0(5) . . ?
F16 Nb4 F20 101.4(5) . . ?
F12 Nb4 F19 93.3(4) . . ?
F16 Nb4 F19 94.1(5) . . ?
F20 Nb4 F19 91.1(5) . . ?
F12 Nb4 F18 86.4(5) . . ?
F16 Nb4 F18 97.1(6) . . ?
F20 Nb4 F18 92.6(5) . . ?
F19 Nb4 F18 167.2(6) . . ?
F12 Nb4 F11 107.4(3) . . ?
F16 Nb4 F11 98.5(4) . . ?
F20 Nb4 F11 109.1(3) . . ?
F19 Nb4 F11 19.9(3) . . ?
F18 Nb4 F11 150.1(5) . . ?
F12 Nb4 F17 147.2(5) . . ?
F16 Nb4 F17 92.8(6) . . ?
F20 Nb4 F17 165.4(5) . . ?
F19 Nb4 F17 84.0(6) . . ?
F18 Nb4 F17 89.3(6) . . ?
F11 Nb4 F17 64.6(4) . . ?
F12 Nb4 F15 61.9(4) . . ?
F16 Nb4 F15 178.1(5) . . ?
F20 Nb4 F15 80.5(5) . . ?
F19 Nb4 F15 85.7(5) . . ?
F18 Nb4 F15 82.9(5) . . ?
F11 Nb4 F15 80.7(4) . . ?
F17 Nb4 F15 85.3(5) . . ?
C1 S1 C2 101.2(4) . . ?
C1 S1 Nb1 102.8(3) . . ?
C2 S1 Nb1 102.0(2) . . ?
C10 S2 C9 101.1(4) . . ?
C10 S2 Nb1 103.2(3) . 2_666 ?
C9 S2 Nb1 102.7(2) . 2_666 ?
C11 S3 C12 101.7(4) . . ?
C11 S3 Nb1 103.8(3) . . ?
C12 S3 Nb1 102.4(2) . . ?
C20 S4 C19 101.5(4) . . ?
C20 S4 Nb1 102.3(3) . 2_655 ?
C19 S4 Nb1 103.5(2) . 2_655 ?
Nb2 F10 Nb2 180.00(12) 2_645 . ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
S1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 S1 114.1(5) . . ?
C3 C2 H2A 108.7 . . ?
S1 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
S1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C8 C3 C4 119.4(6) . . ?
C8 C3 C2 124.1(6) . . ?
C4 C3 C2 116.4(6) . . ?
C5 C4 C3 121.1(7) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 119.6(7) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C7 119.6(7) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C6 C7 C8 121.5(7) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C7 C8 C3 118.8(6) . . ?
C7 C8 C9 117.7(6) . . ?
C3 C8 C9 123.6(6) . . ?
C8 C9 S2 113.0(5) . . ?
C8 C9 H9A 109.0 . . ?
S2 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
S2 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
S2 C10 H10A 109.5 . . ?
S2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
S2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
S3 C11 H11A 109.5 . . ?
S3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
S3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 S3 113.5(5) . . ?
C13 C12 H12A 108.9 . . ?
S3 C12 H12A 108.9 . . ?
C13 C12 H12B 108.9 . . ?
S3 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C14 C13 C18 119.1(7) . . ?
C14 C13 C12 118.2(6) . . ?
C18 C13 C12 122.6(6) . . ?
C13 C14 C15 121.0(7) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C16 C15 C14 120.1(7) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 119.5(7) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C16 C17 C18 121.0(8) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C17 C18 C13 119.2(7) . . ?
C17 C18 C19 117.6(7) . . ?
C13 C18 C19 123.2(6) . . ?
C18 C19 S4 111.6(5) . . ?
C18 C19 H19A 109.3 . . ?
S4 C19 H19A 109.3 . . ?
C18 C19 H19B 109.3 . . ?
S4 C19 H19B 109.3 . . ?
H19A C19 H19B 108.0 . . ?
S4 C20 H20A 109.5 . . ?
S4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
S4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Cl1 C21 Cl2 110.3(10) . . ?
Cl1 C21 H21A 109.6 . . ?
Cl2 C21 H21A 109.6 . . ?
Cl1 C21 H21B 109.6 . . ?
Cl2 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
Cl3 C22 Cl4 114.5(11) . . ?
Cl3 C22 H22A 108.6 . . ?
Cl4 C22 H22A 108.6 . . ?
Cl3 C22 H22B 108.6 . . ?
Cl4 C22 H22B 108.6 . . ?
H22A C22 H22B 107.6 . . ?
F19 F11 Nb4 77.9(12) . . ?
F20 F12 Nb4 93.1(12) . . ?
F22 F14 Nb3 82.5(13) . . ?
F22 F14 F23 148.5(18) . . ?
Nb3 F14 F23 68.8(11) . . ?
Nb4 F15 Nb3 155.8(6) . . ?
F17 F17 Nb4 104.3(11) 2_756 . ?
F11 F19 Nb4 82.3(12) . . ?
F12 F20 Nb4 67.8(11) . . ?
F14 F22 Nb3 63.9(12) . . ?
F14 F23 Nb3 53.4(9) . . ?
F25 F24 Nb3 74(2) . . ?
F24 F25 Nb3 76(3) . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        27.77
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         2.132
_refine_diff_density_min         -3.199
_refine_diff_density_rms         0.188

#===END OF CIF ==============================================================
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#===END OF FILE =============================================================