# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004



data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Dr Stephane Cordier'
_publ_contact_author_address     
;
Institut de Chimie de Rennes
UMR 6511 CNRS-Universite de Rennes 1
Laboratoire de Chimie du Solide et
Avenue du General Leclerc
Rennes
35042
FRANCE
;

_publ_contact_author_email       STEPHANE.CORDIER@UNIV-RENNES1.FR

_publ_section_title              
;
Soluble muFi bridged niobium clusters: synthesis
and crystal structures of (Et4N)6[Nb6Fi6Bri6(NCS)a6]Br2 and
Cs1.6K2.4[Nb6Fi6Ii6(NCS)a6]
;
loop_
_publ_author_name
'Stephane Cordier'
'Nikolai G. Naumov'
'Christiane Perrin'

data_compound_1
_database_code_depnum_ccdc_archive 'CCDC 225283'

_audit_creation_date             2003-11-18T09:40:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_name_common            (Et4N)6(Nb6F6Br6(NCS)6).2Br
_chemical_formula_moiety         'C54 H120 Br8 F6 N12 Nb6 S6'
_chemical_formula_sum            'C54 H120 Br8 F6 N12 Nb6 S6'
_chemical_formula_weight         2440.68
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R_-3
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_Int_Tables_number      148
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   18.149(5)
_cell_length_b                   18.149(5)
_cell_length_c                   25.435(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                120.000
_cell_volume                     7256(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    23544
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      30.034
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3612
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 -1 0.01
-1 1 1 0.01
0 1 -1 0.045
0 -1 1 0.045
1 0 1 0.04
-1 0 -1 0.04
3 -5 -1 0.031
-3 5 1 0.029

_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.168
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_T_max  0.9333
_exptl_absorpt_correction_T_ave  0.8431

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.86563E-2
_diffrn_orient_matrix_ub_12      0.117389E-1
_diffrn_orient_matrix_ub_13      -0.372246E-1
_diffrn_orient_matrix_ub_21      0.590192E-1
_diffrn_orient_matrix_ub_22      0.130885E-1
_diffrn_orient_matrix_ub_23      -0.88495E-2
_diffrn_orient_matrix_ub_31      -0.221289E-1
_diffrn_orient_matrix_ub_32      -0.611455E-1
_diffrn_orient_matrix_ub_33      -0.90407E-2
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_number            30088
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_full        30.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             4703
_reflns_number_gt                3187
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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^)+(0.0597P)^2^+20.0632P] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_coef       0.00043(7)
_refine_ls_number_reflns         4703
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.048
_refine_ls_wR_factor_ref         0.1301
_refine_ls_wR_factor_gt          0.1139
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.56
_refine_diff_density_rms         0.107

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.25172(2) -0.31389(2) 0.211147(14) 0.04068(14) Uani 1 d . . .
Br1 Br 0.35757(3) -0.20524(3) 0.279684(18) 0.05343(16) Uani 1 d . . .
F1 F 0.26981(16) -0.20982(16) 0.16669(9) 0.0510(6) Uani 1 d . . .
N1 N 0.1533(3) -0.2883(3) 0.24992(15) 0.0535(9) Uani 1 d . . .
C1 C 0.1066(4) -0.2750(3) 0.25795(17) 0.0548(11) Uani 1 d . . .
S1 S 0.02915(10) -0.25177(11) 0.27201(7) 0.0791(4) Uani 1 d . . .
N2 N 0.2716(3) 0.0248(3) 0.23592(17) 0.0641(11) Uani 1 d . . .
C21 C 0.2603(4) 0.0281(4) 0.1777(2) 0.0752(15) Uani 1 d . . .
H21A H 0.3161 0.0569 0.1614 0.09 Uiso 1 calc R . .
H21B H 0.2338 0.0623 0.1711 0.09 Uiso 1 calc R . .
C211 C 0.2068(5) -0.0585(5) 0.1507(3) 0.101(2) Uani 1 d . . .
H21C H 0.2031 -0.0501 0.1137 0.151 Uiso 1 calc R . .
H21D H 0.1507 -0.0872 0.1656 0.151 Uiso 1 calc R . .
H21E H 0.2332 -0.0925 0.1558 0.151 Uiso 1 calc R . .
C22 C 0.3224(4) 0.1151(3) 0.2549(2) 0.0749(15) Uani 1 d . . .
H22A H 0.3765 0.1422 0.2365 0.09 Uiso 1 calc R . .
H22B H 0.2925 0.1447 0.245 0.09 Uiso 1 calc R . .
C221 C 0.3399(5) 0.1268(5) 0.3122(3) 0.101(2) Uani 1 d . . .
H22C H 0.3723 0.1865 0.32 0.151 Uiso 1 calc R . .
H22D H 0.3716 0.0998 0.3224 0.151 Uiso 1 calc R . .
H22E H 0.287 0.1018 0.3311 0.151 Uiso 1 calc R . .
C23 C 0.3169(4) -0.0263(4) 0.2476(3) 0.0791(17) Uani 1 d . . .
H23A H 0.3214 -0.0301 0.2853 0.095 Uiso 1 calc R . .
H23B H 0.282 -0.0837 0.2342 0.095 Uiso 1 calc R . .
C231 C 0.4046(4) 0.0113(5) 0.2239(3) 0.0900(19) Uani 1 d . . .
H23C H 0.4285 -0.0238 0.2326 0.135 Uiso 1 calc R . .
H23D H 0.4403 0.0675 0.2376 0.135 Uiso 1 calc R . .
H23E H 0.4008 0.0142 0.1864 0.135 Uiso 1 calc R . .
C24 C 0.1867(4) -0.0206(4) 0.2638(3) 0.0835(17) Uani 1 d . . .
H24A H 0.1576 -0.0798 0.2532 0.1 Uiso 1 calc R . .
H24B H 0.1972 -0.0188 0.3013 0.1 Uiso 1 calc R . .
C241 C 0.1290(5) 0.0140(5) 0.2542(3) 0.103(2) Uani 1 d . . .
H24C H 0.077 -0.019 0.2734 0.155 Uiso 1 calc R . .
H24D H 0.1168 0.0113 0.2173 0.155 Uiso 1 calc R . .
H24E H 0.1561 0.0721 0.2657 0.155 Uiso 1 calc R . .
Br2 Br -0.0313(2) -0.1075(2) 0.10835(17) 0.1402(12) Uani 0.33 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 0.0389(2) 0.0416(2) 0.0435(2) -0.00053(14) 0.00166(14) 0.02156(16)
Br1 0.0574(3) 0.0536(3) 0.0504(3) -0.01151(19) -0.00340(19) 0.0286(2)
F1 0.0572(15) 0.0501(13) 0.0556(15) 0.0020(11) 0.0040(12) 0.0342(12)
N1 0.048(2) 0.059(2) 0.050(2) 0.0040(17) 0.0013(17) 0.0236(19)
C1 0.069(3) 0.042(2) 0.040(2) 0.0038(18) 0.000(2) 0.018(2)
S1 0.0705(9) 0.0942(11) 0.0937(11) 0.0038(9) 0.0124(8) 0.0569(9)
N2 0.073(3) 0.051(2) 0.067(3) 0.012(2) 0.015(2) 0.030(2)
C21 0.093(4) 0.077(4) 0.069(3) 0.011(3) 0.010(3) 0.053(3)
C211 0.119(6) 0.108(5) 0.093(5) -0.015(4) -0.008(4) 0.070(5)
C22 0.088(4) 0.053(3) 0.088(4) 0.008(3) 0.015(3) 0.038(3)
C221 0.106(5) 0.098(5) 0.094(5) -0.012(4) 0.013(4) 0.048(4)
C23 0.102(5) 0.063(3) 0.082(4) 0.010(3) 0.000(3) 0.049(3)
C231 0.092(5) 0.096(5) 0.102(5) 0.012(4) 0.007(4) 0.062(4)
C24 0.082(4) 0.072(4) 0.085(4) 0.012(3) 0.022(3) 0.030(3)
C241 0.089(5) 0.121(6) 0.105(6) -0.012(5) 0.017(4) 0.056(5)
Br2 0.120(2) 0.110(2) 0.195(3) 0.036(2) 0.038(2) 0.0608(18)

#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 F1 2.081(2) 15_445 ?
Nb1 F1 2.082(2) . ?
Nb1 N1 2.282(5) . ?
Nb1 Br1 2.6134(7) . ?
Nb1 Br1 2.6212(7) 2_545 ?
Nb1 Nb1 2.8214(8) 15_445 ?
Nb1 Nb1 2.8214(8) 14 ?
Nb1 Nb1 2.9195(10) 3_655 ?
Nb1 Nb1 2.9195(10) 2_545 ?
Br1 Nb1 2.6212(7) 3_655 ?
F1 Nb1 2.080(2) 14 ?
N1 C1 1.010(6) . ?
C1 S1 1.697(6) . ?
N2 C21 1.500(7) . ?
N2 C22 1.502(7) . ?
N2 C24 1.512(7) . ?
N2 C23 1.546(7) . ?
C21 C211 1.537(9) . ?
C22 C221 1.483(9) . ?
C23 C231 1.509(9) . ?
C24 C241 1.485(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Nb1 F1 91.83(2) 15_445 . ?
F1 Nb1 N1 81.51(12) 15_445 . ?
F1 Nb1 N1 80.46(12) . . ?
F1 Nb1 Br1 166.43(7) 15_445 . ?
F1 Nb1 Br1 87.41(7) . . ?
N1 Nb1 Br1 85.00(10) . . ?
F1 Nb1 Br1 87.53(7) 15_445 2_545 ?
F1 Nb1 Br1 166.72(7) . 2_545 ?
N1 Nb1 Br1 86.33(10) . 2_545 ?
Br1 Nb1 Br1 90.11(3) . 2_545 ?
F1 Nb1 Nb1 47.34(7) 15_445 15_445 ?
F1 Nb1 Nb1 93.78(7) . 15_445 ?
N1 Nb1 Nb1 128.51(10) . 15_445 ?
Br1 Nb1 Nb1 146.231(16) . 15_445 ?
Br1 Nb1 Nb1 95.52(2) 2_545 15_445 ?
F1 Nb1 Nb1 93.72(7) 15_445 14 ?
F1 Nb1 Nb1 47.30(7) . 14 ?
N1 Nb1 Nb1 127.52(10) . 14 ?
Br1 Nb1 Nb1 95.69(2) . 14 ?
Br1 Nb1 Nb1 145.975(16) 2_545 14 ?
Nb1 Nb1 Nb1 62.31(2) 15_445 14 ?
F1 Nb1 Nb1 137.34(7) 15_445 3_655 ?
F1 Nb1 Nb1 90.91(7) . 3_655 ?
N1 Nb1 Nb1 140.74(10) . 3_655 ?
Br1 Nb1 Nb1 56.230(16) . 3_655 ?
Br1 Nb1 Nb1 98.540(14) 2_545 3_655 ?
Nb1 Nb1 Nb1 90 15_445 3_655 ?
Nb1 Nb1 Nb1 58.845(12) 14 3_655 ?
F1 Nb1 Nb1 91.03(7) 15_445 2_545 ?
F1 Nb1 Nb1 137.31(7) . 2_545 ?
N1 Nb1 Nb1 141.95(10) . 2_545 ?
Br1 Nb1 Nb1 98.722(14) . 2_545 ?
Br1 Nb1 Nb1 55.973(16) 2_545 2_545 ?
Nb1 Nb1 Nb1 58.846(12) 15_445 2_545 ?
Nb1 Nb1 Nb1 90 14 2_545 ?
Nb1 Nb1 Nb1 60 3_655 2_545 ?
Nb1 Br1 Nb1 67.80(2) . 3_655 ?
Nb1 F1 Nb1 85.35(9) 14 . ?
C1 N1 Nb1 166.0(4) . . ?
N1 C1 S1 179.2(6) . . ?
C21 N2 C22 107.2(4) . . ?
C21 N2 C24 111.3(5) . . ?
C22 N2 C24 110.3(4) . . ?
C21 N2 C23 109.7(4) . . ?
C22 N2 C23 111.8(5) . . ?
C24 N2 C23 106.6(4) . . ?
N2 C21 C211 115.4(5) . . ?
C221 C22 N2 116.3(5) . . ?
C231 C23 N2 114.2(5) . . ?
C241 C24 N2 115.7(5) . . ?

data_analytic
_database_code_depnum_ccdc_archive 'CCDC 225284'

_audit_creation_date             2003-11-26T17:27:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_name_common            Cs1.6K2.4(Nb6F6I6(NCS)6)
_chemical_formula_moiety         'C6 Cs1.6 K2.4 N6 Nb6 F6 I6 S6'
_chemical_formula_sum            'C6 Cs1.6 K2.4 N6 Nb6 F6 I6 S6'
_chemical_formula_weight         2087.84
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.406(5)
_cell_length_b                   12.237(5)
_cell_length_c                   23.155(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.307(5)
_cell_angle_gamma                90.000
_cell_volume                     4800(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    84105
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      25.028
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    2.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7248
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -1 6 0.062
-1 1 -5 0.057
-4 1 12 0.058
1 -2 -18 0.064
-10 -15 1 0.039
-7 -18 -17 0.038
10 16 1 0.035
0 1 2 0.044
4 1 -7 0.081
-3 4 -8 0.049
6 -1 3 0.03
-9 12 10 0.024
-12 1 -4 0.02
12 -1 4 0.025
7 -8 -3 0.044
-5 9 4 0.019

_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    6.945
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_absorpt_correction_T_min  0.3246
_exptl_absorpt_correction_T_max  0.5897
_exptl_absorpt_correction_T_ave  0.4881

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.42145E-2
_diffrn_orient_matrix_ub_12      0.658144E-1
_diffrn_orient_matrix_ub_13      -0.246837E-1
_diffrn_orient_matrix_ub_21      0.523235E-1
_diffrn_orient_matrix_ub_22      -0.263014E-1
_diffrn_orient_matrix_ub_23      -0.53289E-2
_diffrn_orient_matrix_ub_31      -0.270145E-1
_diffrn_orient_matrix_ub_32      -0.406746E-1
_diffrn_orient_matrix_ub_33      -0.364941E-1
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.044
_diffrn_reflns_number            23177
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             4251
_reflns_number_gt                3186
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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.

Direct methods yielded to a first partial structural solution in
C2/c space group including niobium cluster, inner fluorine and inner
iodine and six thiocyanate groups as well as cesium cations.
A first set of refinements rapidly revealed that the cesium sites
were partially occupied and, once the unit refined, that the the carbon
and sulfur atoms belonging to the NCS groups  bonded  to Nb1 and Nb2 had
large unrealistic atomic displacement parameters  related to neighboring
cations disordered  over several close positions.
Consequently, Each S(1), C(1) and  S(2), C(2)atomic positions was split
over two positions namely S11, S12, C11, C12 and S21, S22, C21, C22
respectively. The atomic displacement parameter of split atomic positions
were refined isotropically and restricted to the same value (i.e. same EADP
for (S11, S12), (C11, C12), (S21,S21),(C21,C22)).After some cycles of
refinements, it turned out that their occupation factors converged to 0.5
within the s.u.'s. It means that the NCS goups bonded to Nb1 and Nb2 are
equally distributed over two orientations.
At this stage, the units and the cesium atoms had been located but many
electronic density peaks remained close to the cesium position leading
to high R values. A first attempt to refine them as ceasium failed leading
to unrealistic thermal factor and an increase of R values. Then, after a
carefull study these peaks were attributed unambigously to potassium
cations as follows:
Indeed, K11 was added close to Cs1 (1 Angtroem). The sum of the occupancies
of Cs1/K11 site was restricted to the value corresponding to a fully
occupied position (it corresponds to one cation per formula). Seven
other peaks were located between Cs2 and Cs3 and were attributed to
K31 K32 K33 K4 K5 K7 K8. Then the sum of the occupancies of
Cs2, Cs3, K31, K32, K33, K4, K5, K7 and K8 was resticted to a value
corresponding to three cations per formula. Due to these close positions,
the atomic displacement parameters of Cs2 and Cs3 were restricted to the
same value and separately, the atomic displacement parameters of K31,
K32, K33, K4, K5, K7 and K8 were also restricted to another same value.
These atoms were then refined anisotopically.
The final structural refinements led to the refined formula
K2.4(2)Cs1.6(2)[Nb6F6I6(NCS)6] in agreement with the EDS analysis. This
stoechiometry is corroborated by electronic (16e/Nb6) and structural
considerations.
;
_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^)+(0.1086P)^2^+90.2389P] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_coef       0.00042(5)
_refine_ls_number_reflns         4251
_refine_ls_number_parameters     211
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0648
_refine_ls_wR_factor_ref         0.1976
_refine_ls_wR_factor_gt          0.1772
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.835
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.309

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
K K 0.2009 0.2494 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.368 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb -0.05293(6) 0.14998(8) -0.51277(4) 0.0521(2) Uani 1 1 d . . .
Nb2 Nb -0.08120(6) -0.05674(8) -0.45608(4) 0.0495(2) Uani 1 1 d . . .
Nb3 Nb 0.06386(6) 0.05660(8) -0.42084(4) 0.0512(2) Uani 1 1 d . . .
I1 I -0.18007(5) 0.12547(7) -0.45787(4) 0.0694(2) Uani 1 1 d . . .
I2 I -0.19289(5) -0.15651(7) -0.54729(3) 0.0648(2) Uani 1 1 d . . .
I3 I -0.15672(5) 0.12700(8) -0.62512(4) 0.0769(3) Uani 1 1 d . . .
F1 F 0.0109(4) 0.2108(5) -0.4311(3) 0.0669(18) Uani 1 1 d . . .
F2 F 0.0275(4) 0.2111(5) -0.5586(3) 0.0632(17) Uani 1 1 d . . .
F3 F -0.0174(4) 0.0004(5) -0.3737(3) 0.0609(17) Uani 1 1 d . . .
N1 N -0.0900(6) 0.3183(9) -0.5206(6) 0.080(3) Uani 1 1 d . . .
N2 N -0.1492(6) -0.1242(9) -0.3953(4) 0.066(3) Uani 1 1 d . . .
N3 N 0.1132(7) 0.1240(11) -0.3312(5) 0.085(4) Uani 1 1 d . . .
C11 C -0.1009(18) 0.410(3) -0.5109(14) 0.077(5) Uiso 0.480(12) 1 d P . .
C12 C -0.1022(17) 0.411(3) -0.5380(13) 0.077(5) Uiso 0.52 1 d P . .
C22 C -0.1674(17) -0.163(2) -0.3590(14) 0.064(4) Uiso 0.465(9) 1 d P . .
C21 C -0.1807(16) -0.138(2) -0.3560(12) 0.064(4) Uiso 0.535(9) 1 d P . .
C3 C 0.1313(9) 0.1473(13) -0.2826(6) 0.081(4) Uani 1 1 d . . .
S11 S -0.1140(7) 0.5438(10) -0.5036(6) 0.120(3) Uiso 0.480(12) 1 d P . .
S12 S -0.1223(7) 0.5439(9) -0.5477(6) 0.120(3) Uiso 0.52 1 d P . .
S21 S -0.2189(4) -0.1687(6) -0.3003(3) 0.0766(15) Uiso 0.535(9) 1 d P . .
S22 S -0.1937(5) -0.2096(7) -0.2965(4) 0.0766(15) Uiso 0.46 1 d P . .
S3 S 0.1527(5) 0.1696(6) -0.2119(2) 0.163(3) Uani 1 1 d . . .
Cs1 Cs 0 0.06905(15) -0.75 0.0869(5) Uani 0.947(4) 2 d SP . .
K11 K 0 -0.013(10) -0.75 0.0869(5) Uani 0.05 2 d SP . .
Cs2 Cs -0.0881(7) 0.5718(8) -0.4086(6) 0.174(4) Uani 0.179(4) 1 d P . .
Cs3 Cs 0.0853(9) 0.4002(11) -0.3679(8) 0.174(4) Uani 0.151(4) 1 d P . .
K31 K -0.044(2) 0.382(2) -0.3648(18) 0.144(4) Uani 0.160(8) 1 d P . .
K32 K -0.1086(19) 0.415(2) -0.3896(16) 0.144(4) Uani 0.175(8) 1 d P . .
K33 K 0.0414(15) 0.3947(16) -0.3563(12) 0.144(4) Uani 0.244(10) 1 d P . .
K4 K 0.3221(16) 0.071(2) -0.2038(15) 0.144(4) Uani 0.190(8) 1 d P . .
K5 K -0.1800(15) -0.4709(19) -0.2469(14) 0.144(4) Uani 0.203(9) 1 d P . .
K7 K 0 -0.363(2) -0.25 0.144(4) Uani 0.215(13) 2 d SP . .
K8 K -0.156(3) -0.560(3) -0.205(2) 0.144(4) Uani 0.121(9) 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 0.0585(5) 0.0468(5) 0.0509(5) 0.0029(4) 0.0122(4) -0.0020(4)
Nb2 0.0563(5) 0.0521(6) 0.0411(5) 0.0016(4) 0.0131(4) -0.0075(4)
Nb3 0.0580(5) 0.0558(6) 0.0389(5) -0.0016(4) 0.0090(4) -0.0097(4)
I1 0.0659(4) 0.0724(5) 0.0750(5) -0.0006(4) 0.0265(4) 0.0049(4)
I2 0.0633(4) 0.0726(5) 0.0577(4) -0.0041(4) 0.0123(3) -0.0202(4)
I3 0.0753(5) 0.0851(6) 0.0619(5) 0.0184(4) -0.0012(4) 0.0029(4)
F1 0.082(4) 0.057(4) 0.061(4) -0.017(3) 0.016(3) -0.007(3)
F2 0.072(4) 0.056(4) 0.064(4) 0.013(3) 0.021(3) -0.004(3)
F3 0.071(4) 0.070(4) 0.044(3) -0.003(3) 0.018(3) -0.008(3)
N1 0.066(6) 0.052(6) 0.124(10) 0.000(6) 0.023(6) -0.003(5)
N2 0.071(6) 0.080(7) 0.054(5) 0.010(5) 0.029(4) -0.010(5)
N3 0.084(7) 0.116(10) 0.054(6) -0.011(6) 0.013(5) -0.018(7)
C3 0.092(9) 0.104(10) 0.048(7) -0.010(7) 0.014(6) -0.033(8)
S3 0.226(6) 0.203(6) 0.056(2) -0.040(3) 0.025(3) -0.075(5)
Cs1 0.0987(10) 0.1157(13) 0.0459(7) 0 0.0159(6) 0
K11 0.0987(10) 0.1157(13) 0.0459(7) 0 0.0159(6) 0
Cs2 0.165(7) 0.126(6) 0.230(10) 0.003(5) 0.040(6) -0.002(5)
Cs3 0.165(7) 0.126(6) 0.230(10) 0.003(5) 0.040(6) -0.002(5)
K31 0.134(8) 0.095(6) 0.208(11) -0.069(6) 0.048(8) -0.023(6)
K32 0.134(8) 0.095(6) 0.208(11) -0.069(6) 0.048(8) -0.023(6)
K33 0.134(8) 0.095(6) 0.208(11) -0.069(6) 0.048(8) -0.023(6)
K4 0.134(8) 0.095(6) 0.208(11) -0.069(6) 0.048(8) -0.023(6)
K5 0.134(8) 0.095(6) 0.208(11) -0.069(6) 0.048(8) -0.023(6)
K7 0.134(8) 0.095(6) 0.208(11) -0.069(6) 0.048(8) -0.023(6)
K8 0.134(8) 0.095(6) 0.208(11) -0.069(6) 0.048(8) -0.023(6)

#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 F2 2.081(6) . ?
Nb1 F1 2.096(6) . ?
Nb1 N1 2.153(11) . ?
Nb1 I1 2.8105(15) . ?
Nb1 I3 2.8191(14) . ?
Nb1 Nb3 2.8243(14) . ?
Nb1 Nb2 2.8368(16) 5_554 ?
Nb1 Nb3 2.9420(17) 5_554 ?
Nb1 Nb2 2.9430(16) . ?
Nb2 F3 2.094(6) . ?
Nb2 F2 2.100(7) 5_554 ?
Nb2 N2 2.198(9) . ?
Nb2 I2 2.8001(13) . ?
Nb2 I1 2.8111(15) . ?
Nb2 Nb3 2.8313(15) . ?
Nb2 Nb1 2.8368(16) 5_554 ?
Nb2 Nb3 2.9339(15) 5_554 ?
Nb3 F1 2.089(7) . ?
Nb3 F3 2.091(6) . ?
Nb3 N3 2.215(11) . ?
Nb3 I2 2.8010(14) 5_554 ?
Nb3 I3 2.8286(15) 5_554 ?
Nb3 Nb2 2.9339(15) 5_554 ?
Nb3 Nb1 2.9420(17) 5_554 ?
Nb3 Cs3 4.372(14) . ?
I1 K32 3.96(2) . ?
I2 Nb3 2.8010(14) 5_554 ?
I2 Cs2 3.855(12) 7_454 ?
I2 Cs3 4.237(16) 5_554 ?
I3 Nb3 2.8286(16) 5_554 ?
I3 K5 4.08(3) 7_444 ?
I3 Cs1 4.4651(13) . ?
F1 K33 2.82(2) . ?
F1 Cs3 2.885(16) . ?
F1 K31 2.89(3) . ?
F2 Nb2 2.100(7) 5_554 ?
F2 Cs2 3.019(13) 5_564 ?
F3 K11 2.815(9) 5_554 ?
F3 Cs1 2.936(6) 5_554 ?
N1 C11 1.17(3) . ?
N1 C12 1.20(3) . ?
N1 K32 3.34(4) . ?
N2 C22 1.07(3) . ?
N2 C21 1.18(3) . ?
N2 Cs1 3.807(10) 5_554 ?
N3 C3 1.133(16) . ?
N3 K11 3.31(5) 5_554 ?
N3 Cs3 3.492(19) . ?
N3 Cs1 3.835(12) 5_554 ?
C11 C12 0.62(4) . ?
C11 S11 1.66(3) . ?
C11 S12 1.84(3) . ?
C11 K32 2.84(5) . ?
C11 Cs2 3.05(3) . ?
C11 K31 3.32(5) . ?
C11 Cs3 3.70(4) 5_564 ?
C12 S12 1.67(3) . ?
C12 S11 1.85(3) . ?
C12 Cs3 3.24(3) 5_564 ?
C12 K32 3.46(5) . ?
C12 Cs2 3.55(3) . ?
C12 Cs2 3.80(3) 5_564 ?
C22 S22 1.71(3) . ?
C22 S21 1.80(3) . ?
C22 Cs1 3.58(3) 5_554 ?
C22 Cs2 3.81(3) 1_545 ?
C21 S21 1.63(3) . ?
C21 S22 1.69(3) . ?
C21 Cs1 3.62(3) 5_554 ?
C3 S3 1.617(13) . ?
C3 K11 3.05(7) 5_554 ?
C3 K5 3.51(3) 3 ?
C3 K4 3.53(3) . ?
C3 Cs3 3.66(2) . ?
C3 Cs1 3.687(14) 5_554 ?
S11 S12 0.996(15) . ?
S11 Cs2 2.170(19) . ?
S11 K32 3.06(4) . ?
S11 Cs3 3.20(2) 5_564 ?
S11 K31 3.73(4) . ?
S12 Cs3 2.30(2) 5_564 ?
S12 K33 2.99(3) 5_564 ?
S12 Cs2 3.156(19) . ?
S12 K8 3.56(5) 6 ?
S12 K4 3.79(4) 8_455 ?
S21 S22 0.658(10) . ?
S21 K8 2.58(4) 4_454 ?
S21 K5 3.32(3) 4_454 ?
S21 K4 3.45(3) 2_554 ?
S21 Cs3 3.510(17) 3_445 ?
S21 Cs1 3.914(7) 5_554 ?
S22 K8 3.20(4) 4_454 ?
S22 K5 3.39(3) . ?
S22 K4 3.41(3) 3_445 ?
S22 Cs1 3.716(8) 5_554 ?
S22 K7 3.793(17) . ?
S22 Cs3 4.051(18) 3_445 ?
S3 K4 3.15(3) . ?
S3 K11 3.23(7) 5_554 ?
S3 K5 3.63(3) 3 ?
S3 Cs1 3.911(7) 5_554 ?
Cs1 K11 1.00(12) . ?
Cs1 F3 2.936(6) 6 ?
Cs1 F3 2.936(6) 5_554 ?
Cs1 C22 3.58(3) 5_554 ?
Cs1 C22 3.58(3) 6 ?
Cs1 K7 3.60(3) 5_554 ?
Cs1 C21 3.62(3) 5_554 ?
Cs1 C21 3.62(3) 6 ?
Cs1 C3 3.687(14) 5_554 ?
Cs1 C3 3.687(14) 6 ?
Cs1 S22 3.716(9) 5_554 ?
Cs1 S22 3.716(8) 6 ?
K11 F3 2.815(9) 5_554 ?
K11 F3 2.815(9) 6 ?
K11 C3 3.05(7) 5_554 ?
K11 C3 3.05(7) 6 ?
K11 S3 3.23(7) 5_554 ?
K11 S3 3.23(7) 6 ?
K11 N3 3.31(5) 5_554 ?
K11 N3 3.31(5) 6 ?
K11 K7 4.60(13) 5_554 ?
Cs2 K32 2.02(3) . ?
Cs2 K31 2.57(4) . ?
Cs2 F2 3.019(13) 5_564 ?
Cs2 K33 3.16(3) . ?
Cs2 Cs3 3.619(19) . ?
Cs2 K7 3.724(14) 1_565 ?
Cs2 C12 3.80(3) 5_564 ?
Cs2 C22 3.81(3) 1_565 ?
Cs3 K33 0.87(3) . ?
Cs3 K8 1.91(5) 2_564 ?
Cs3 K31 2.28(4) . ?
Cs3 S12 2.30(2) 5_564 ?
Cs3 K4 2.91(3) 4_554 ?
Cs3 S11 3.20(2) 5_564 ?
Cs3 K5 3.20(4) 2_564 ?
Cs3 C12 3.24(3) 5_564 ?
Cs3 K32 3.30(4) . ?
Cs3 S21 3.510(17) 3 ?
K31 K32 1.20(4) . ?
K31 K33 1.46(4) . ?
K31 K8 3.56(6) 2_564 ?
K31 K7 4.05(4) 1_565 ?
K31 K5 4.39(4) 1_565 ?
K31 K4 4.46(4) 4_554 ?
K31 K5 4.53(4) 2_564 ?
K32 K33 2.56(4) . ?
K32 K5 4.04(4) 1_565 ?
K32 K7 4.31(3) 1_565 ?
K32 K8 4.55(6) 1_565 ?
K33 K8 2.23(5) 2_564 ?
K33 S12 2.99(3) 5_564 ?
K33 K4 3.27(4) 4_554 ?
K33 K5 3.40(4) 2_564 ?
K33 K7 4.02(3) 1_565 ?
K4 K5 1.11(4) 3 ?
K4 K8 1.64(4) 3 ?
K4 Cs3 2.91(3) 4_544 ?
K4 K33 3.27(4) 4_544 ?
K4 S22 3.41(3) 3 ?
K4 S21 3.45(3) 2_554 ?
K4 K7 3.59(3) 3 ?
K4 S12 3.79(4) 8_556 ?
K4 K31 4.46(4) 4_544 ?
K4 Cs2 4.76(3) 4_544 ?
K5 K4 1.11(4) 3_445 ?
K5 K8 1.45(5) . ?
K5 Cs3 3.20(4) 2_544 ?
K5 S21 3.32(3) 4_444 ?
K5 K33 3.40(4) 2_544 ?
K5 K7 3.41(3) . ?
K5 C3 3.51(3) 3_445 ?
K5 S3 3.63(3) 3_445 ?
K5 K32 4.04(4) 1_545 ?
K5 I3 4.08(2) 7_444 ?
K5 K31 4.39(4) 1_545 ?
K7 K5 3.41(3) 2_554 ?
K7 K4 3.59(3) 3_445 ?
K7 K4 3.59(3) 4_544 ?
K7 Cs1 3.60(3) 5_554 ?
K7 Cs2 3.724(14) 2_544 ?
K7 Cs2 3.724(14) 1_545 ?
K7 S22 3.793(17) 2_554 ?
K7 K8 3.94(5) . ?
K7 K8 3.94(5) 2_554 ?
K7 K33 4.02(3) 1_545 ?
K8 K4 1.64(4) 3_445 ?
K8 Cs3 1.91(5) 2_544 ?
K8 K33 2.23(5) 2_544 ?
K8 S21 2.58(4) 4_444 ?
K8 S22 3.20(4) 4_444 ?
K8 K31 3.56(6) 2_544 ?
K8 S12 3.56(5) 6_556 ?
K8 K32 4.55(6) 1_545 ?
K8 K31 4.62(6) 1_545 ?
K8 K32 4.63(5) 2_544 ?

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
F2 Nb1 F1 93.1(3) . . ?
F2 Nb1 N1 80.6(4) . . ?
F1 Nb1 N1 79.8(4) . . ?
F2 Nb1 I1 164.01(18) . . ?
F1 Nb1 I1 86.5(2) . . ?
N1 Nb1 I1 83.6(3) . . ?
F2 Nb1 I3 85.91(18) . . ?
F1 Nb1 I3 164.07(19) . . ?
N1 Nb1 I3 84.4(3) . . ?
I1 Nb1 I3 90.15(4) . . ?
F2 Nb1 Nb3 94.46(18) . . ?
F1 Nb1 Nb3 47.46(19) . . ?
N1 Nb1 Nb3 126.9(3) . . ?
I1 Nb1 Nb3 96.95(4) . . ?
I3 Nb1 Nb3 148.46(5) . . ?
F2 Nb1 Nb2 47.57(18) . 5_554 ?
F1 Nb1 Nb2 94.36(19) . 5_554 ?
N1 Nb1 Nb2 127.7(3) . 5_554 ?
I1 Nb1 Nb2 148.41(5) . 5_554 ?
I3 Nb1 Nb2 96.62(4) . 5_554 ?
Nb3 Nb1 Nb2 62.43(4) . 5_554 ?
F2 Nb1 Nb3 90.72(19) . 5_554 ?
F1 Nb1 Nb3 137.16(19) . 5_554 ?
N1 Nb1 Nb3 142.7(3) . 5_554 ?
I1 Nb1 Nb3 100.46(4) . 5_554 ?
I3 Nb1 Nb3 58.76(3) . 5_554 ?
Nb3 Nb1 Nb3 89.71(4) . 5_554 ?
Nb2 Nb1 Nb3 58.64(4) 5_554 5_554 ?
F2 Nb1 Nb2 137.53(18) . . ?
F1 Nb1 Nb2 90.63(19) . . ?
N1 Nb1 Nb2 141.4(3) . . ?
I1 Nb1 Nb2 58.44(3) . . ?
I3 Nb1 Nb2 100.86(4) . . ?
Nb3 Nb1 Nb2 58.76(4) . . ?
Nb2 Nb1 Nb2 89.97(4) 5_554 . ?
Nb3 Nb1 Nb2 59.81(4) 5_554 . ?
F3 Nb2 F2 91.7(3) . 5_554 ?
F3 Nb2 N2 78.1(3) . . ?
F2 Nb2 N2 81.0(3) 5_554 . ?
F3 Nb2 I2 164.42(18) . . ?
F2 Nb2 I2 86.31(18) 5_554 . ?
N2 Nb2 I2 86.4(3) . . ?
F3 Nb2 I1 86.75(19) . . ?
F2 Nb2 I1 164.53(18) 5_554 . ?
N2 Nb2 I1 83.7(3) . . ?
I2 Nb2 I1 91.05(4) . . ?
F3 Nb2 Nb3 47.38(18) . . ?
F2 Nb2 Nb3 93.45(18) 5_554 . ?
N2 Nb2 Nb3 125.1(3) . . ?
I2 Nb2 Nb3 148.13(4) . . ?
I1 Nb2 Nb3 96.78(5) . . ?
F3 Nb2 Nb1 94.05(19) . 5_554 ?
F2 Nb2 Nb1 47.01(18) 5_554 5_554 ?
N2 Nb2 Nb1 127.4(3) . 5_554 ?
I2 Nb2 Nb1 95.86(4) . 5_554 ?
I1 Nb2 Nb1 148.45(5) . 5_554 ?
Nb3 Nb2 Nb1 62.54(4) . 5_554 ?
F3 Nb2 Nb3 137.11(18) . 5_554 ?
F2 Nb2 Nb3 90.95(18) 5_554 5_554 ?
N2 Nb2 Nb3 144.4(3) . 5_554 ?
I2 Nb2 Nb3 58.43(3) . 5_554 ?
I1 Nb2 Nb3 100.65(4) . 5_554 ?
Nb3 Nb2 Nb3 89.74(4) . 5_554 ?
Nb1 Nb2 Nb3 58.58(3) 5_554 5_554 ?
F3 Nb2 Nb1 90.63(18) . . ?
F2 Nb2 Nb1 137.03(18) 5_554 . ?
N2 Nb2 Nb1 141.1(3) . . ?
I2 Nb2 Nb1 101.35(4) . . ?
I1 Nb2 Nb1 58.42(4) . . ?
Nb3 Nb2 Nb1 58.53(3) . . ?
Nb1 Nb2 Nb1 90.03(4) 5_554 . ?
Nb3 Nb2 Nb1 60.08(4) 5_554 . ?
F1 Nb3 F3 91.3(3) . . ?
F1 Nb3 N3 80.6(4) . . ?
F3 Nb3 N3 78.3(4) . . ?
F1 Nb3 I2 86.3(2) . 5_554 ?
F3 Nb3 I2 163.82(17) . 5_554 ?
N3 Nb3 I2 85.6(3) . 5_554 ?
F1 Nb3 Nb1 47.67(17) . . ?
F3 Nb3 Nb1 94.04(18) . . ?
N3 Nb3 Nb1 127.8(3) . . ?
I2 Nb3 Nb1 96.12(4) 5_554 . ?
F1 Nb3 I3 163.55(18) . 5_554 ?
F3 Nb3 I3 86.50(19) . 5_554 ?
N3 Nb3 I3 83.0(3) . 5_554 ?
I2 Nb3 I3 91.28(5) 5_554 5_554 ?
Nb1 Nb3 I3 148.73(5) . 5_554 ?
F1 Nb3 Nb2 93.92(19) . . ?
F3 Nb3 Nb2 47.47(16) . . ?
N3 Nb3 Nb2 125.5(3) . . ?
I2 Nb3 Nb2 148.63(4) 5_554 . ?
Nb1 Nb3 Nb2 62.71(4) . . ?
I3 Nb3 Nb2 96.53(5) 5_554 . ?
F1 Nb3 Nb2 91.74(19) . 5_554 ?
F3 Nb3 Nb2 137.74(17) . 5_554 ?
N3 Nb3 Nb2 143.7(3) . 5_554 ?
I2 Nb3 Nb2 58.40(3) 5_554 5_554 ?
Nb1 Nb3 Nb2 58.99(4) . 5_554 ?
I3 Nb3 Nb2 100.85(4) 5_554 5_554 ?
Nb2 Nb3 Nb2 90.26(4) . 5_554 ?
F1 Nb3 Nb1 137.96(18) . 5_554 ?
F3 Nb3 Nb1 91.14(18) . 5_554 ?
N3 Nb3 Nb1 140.7(4) . 5_554 ?
I2 Nb3 Nb1 101.35(4) 5_554 5_554 ?
Nb1 Nb3 Nb1 90.29(4) . 5_554 ?
I3 Nb3 Nb1 58.45(4) 5_554 5_554 ?
Nb2 Nb3 Nb1 58.82(4) . 5_554 ?
Nb2 Nb3 Nb1 60.11(4) 5_554 5_554 ?
F1 Nb3 Cs3 34.0(3) . . ?
F3 Nb3 Cs3 101.2(3) . . ?
N3 Nb3 Cs3 52.4(4) . . ?
I2 Nb3 Cs3 68.4(2) 5_554 . ?
Nb1 Nb3 Cs3 79.8(2) . . ?
I3 Nb3 Cs3 130.8(2) 5_554 . ?
Nb2 Nb3 Cs3 124.4(2) . . ?
Nb2 Nb3 Cs3 104.5(2) 5_554 . ?
Nb1 Nb3 Cs3 164.6(2) 5_554 . ?
Nb1 I1 Nb2 63.14(4) . . ?
Nb1 I1 K32 83.0(5) . . ?
Nb2 I1 K32 124.6(5) . . ?
Nb2 I2 Nb3 63.17(4) . 5_554 ?
Nb2 I2 Cs2 123.73(18) . 7_454 ?
Nb3 I2 Cs2 128.08(18) 5_554 7_454 ?
Nb2 I2 Cs3 110.6(2) . 5_554 ?
Nb3 I2 Cs3 73.6(2) 5_554 5_554 ?
Cs2 I2 Cs3 125.6(3) 7_454 5_554 ?
Nb1 I3 Nb3 62.79(4) . 5_554 ?
Nb1 I3 K5 155.3(4) . 7_444 ?
Nb3 I3 K5 98.3(4) 5_554 7_444 ?
Nb1 I3 Cs1 104.84(4) . . ?
Nb3 I3 Cs1 74.70(4) 5_554 . ?
K5 I3 Cs1 83.2(4) 7_444 . ?
Nb3 F1 Nb1 84.9(2) . . ?
Nb3 F1 K33 129.5(6) . . ?
Nb1 F1 K33 145.5(6) . . ?
Nb3 F1 Cs3 122.2(4) . . ?
Nb1 F1 Cs3 145.6(4) . . ?
K33 F1 Cs3 17.5(5) . . ?
Nb3 F1 K31 141.9(9) . . ?
Nb1 F1 K31 124.4(8) . . ?
K33 F1 K31 29.7(8) . . ?
Cs3 F1 K31 46.5(7) . . ?
Nb1 F2 Nb2 85.4(2) . 5_554 ?
Nb1 F2 Cs2 139.4(4) . 5_564 ?
Nb2 F2 Cs2 131.6(4) 5_554 5_564 ?
Nb3 F3 Nb2 85.1(2) . . ?
Nb3 F3 K11 125.9(12) . 5_554 ?
Nb2 F3 K11 148.8(14) . 5_554 ?
Nb3 F3 Cs1 132.4(3) . 5_554 ?
Nb2 F3 Cs1 134.9(3) . 5_554 ?
K11 F3 Cs1 20(2) 5_554 5_554 ?
C11 N1 C12 30(2) . . ?
C11 N1 Nb1 164.0(18) . . ?
C12 N1 Nb1 162.5(18) . . ?
C11 N1 K32 55.4(17) . . ?
C12 N1 K32 85.7(17) . . ?
Nb1 N1 K32 110.6(7) . . ?
C22 N2 C21 20(2) . . ?
C22 N2 Nb2 165.1(17) . . ?
C21 N2 Nb2 164.5(15) . . ?
C22 N2 Cs1 69.6(16) . 5_554 ?
C21 N2 Cs1 71.8(14) . 5_554 ?
Nb2 N2 Cs1 98.1(3) . 5_554 ?
C3 N3 Nb3 169.6(12) . . ?
C3 N3 K11 66.7(13) . 5_554 ?
Nb3 N3 K11 103.1(11) . 5_554 ?
C3 N3 Cs3 89.4(11) . . ?
Nb3 N3 Cs3 97.5(5) . . ?
K11 N3 Cs3 117.9(19) 5_554 . ?
C3 N3 Cs1 74.0(9) . 5_554 ?
Nb3 N3 Cs1 95.6(4) . 5_554 ?
K11 N3 Cs1 13.8(19) 5_554 5_554 ?
Cs3 N3 Cs1 131.1(5) . 5_554 ?
C12 C11 N1 77(5) . . ?
C12 C11 S11 97(5) . . ?
N1 C11 S11 174(3) . . ?
C12 C11 S12 65(4) . . ?
N1 C11 S12 142(3) . . ?
S11 C11 S12 32.5(8) . . ?
C12 C11 K32 175(5) . . ?
N1 C11 K32 105(2) . . ?
S11 C11 K32 80.9(14) . . ?
S12 C11 K32 112.9(16) . . ?
C12 C11 Cs2 139(5) . . ?
N1 C11 Cs2 142(2) . . ?
S11 C11 Cs2 43.4(9) . . ?
S12 C11 Cs2 75.9(11) . . ?
K32 C11 Cs2 39.9(7) . . ?
C12 C11 K31 164(5) . . ?
N1 C11 K31 94.2(19) . . ?
S11 C11 K31 90.8(14) . . ?
S12 C11 K31 123.0(15) . . ?
K32 C11 K31 20.8(8) . . ?
Cs2 C11 K31 47.4(7) . . ?
C12 C11 Cs3 39(4) . 5_564 ?
N1 C11 Cs3 114(2) . 5_564 ?
S11 C11 Cs3 59.8(11) . 5_564 ?
S12 C11 Cs3 30.1(8) . 5_564 ?
K32 C11 Cs3 140.0(13) . 5_564 ?
Cs2 C11 Cs3 100.3(9) . 5_564 ?
K31 C11 Cs3 141.5(11) . 5_564 ?
C11 C12 N1 72(5) . . ?
C11 C12 S12 95(5) . . ?
N1 C12 S12 168(3) . . ?
C11 C12 S11 63(4) . . ?
N1 C12 S11 136(2) . . ?
S12 C12 S11 32.4(8) . . ?
C11 C12 Cs3 134(5) . 5_564 ?
N1 C12 Cs3 149(2) . 5_564 ?
S12 C12 Cs3 42.4(9) . 5_564 ?
S11 C12 Cs3 72.2(11) . 5_564 ?
C11 C12 K32 4(4) . . ?
N1 C12 K32 74.1(16) . . ?
S12 C12 K32 93.7(13) . . ?
S11 C12 K32 61.8(10) . . ?
Cs3 C12 K32 133.2(11) 5_564 . ?
C11 C12 Cs2 34(4) . . ?
N1 C12 Cs2 105.5(17) . . ?
S12 C12 Cs2 62.8(10) . . ?
S11 C12 Cs2 30.5(7) . . ?
Cs3 C12 Cs2 99.9(9) 5_564 . ?
K32 C12 Cs2 33.4(5) . . ?
C11 C12 Cs2 120(4) . 5_564 ?
N1 C12 Cs2 93.6(16) . 5_564 ?
S12 C12 Cs2 94.1(12) . 5_564 ?
S11 C12 Cs2 106.4(12) . 5_564 ?
Cs3 C12 Cs2 61.3(6) 5_564 5_564 ?
K32 C12 Cs2 123.5(10) . 5_564 ?
Cs2 C12 Cs2 110.3(8) . 5_564 ?
N2 C22 S22 173(3) . . ?
N2 C22 S21 154(3) . . ?
S22 C22 S21 21.4(5) . . ?
N2 C22 Cs1 94.1(18) . 5_554 ?
S22 C22 Cs1 81.0(11) . 5_554 ?
S21 C22 Cs1 86.9(11) . 5_554 ?
N2 C22 Cs2 87.0(18) . 1_545 ?
S22 C22 Cs2 99.0(12) . 1_545 ?
S21 C22 Cs2 118.3(13) . 1_545 ?
Cs1 C22 Cs2 101.2(7) 5_554 1_545 ?
N2 C21 S21 174(2) . . ?
N2 C21 S22 151(2) . . ?
S21 C21 S22 22.8(5) . . ?
N2 C21 Cs1 90.2(14) . 5_554 ?
S21 C21 Cs1 88.1(11) . 5_554 ?
S22 C21 Cs1 80.0(10) . 5_554 ?
N3 C3 S3 174.3(14) . . ?
N3 C3 K11 93.3(12) . 5_554 ?
S3 C3 K11 81.5(8) . 5_554 ?
N3 C3 K5 99.3(12) . 3 ?
S3 C3 K5 81.1(8) . 3 ?
K11 C3 K5 115.7(18) 5_554 3 ?
N3 C3 K4 117.4(13) . . ?
S3 C3 K4 63.3(8) . . ?
K11 C3 K4 113.5(14) 5_554 . ?
K5 C3 K4 18.2(6) 3 . ?
N3 C3 Cs3 72.6(10) . . ?
S3 C3 Cs3 112.0(8) . . ?
K11 C3 Cs3 120.4(16) 5_554 . ?
K5 C3 Cs3 123.5(7) 3 . ?
K4 C3 Cs3 124.5(7) . . ?
N3 C3 Cs1 88.8(10) . 5_554 ?
S3 C3 Cs1 85.6(6) . 5_554 ?
K11 C3 Cs1 13.3(19) 5_554 5_554 ?
K5 C3 Cs1 104.3(6) 3 5_554 ?
K4 C3 Cs1 104.9(6) . 5_554 ?
Cs3 C3 Cs1 130.4(5) . 5_554 ?
S12 S11 C11 83.6(15) . . ?
S12 S11 C12 64.2(13) . . ?
C11 S11 C12 19.5(14) . . ?
S12 S11 Cs2 170.1(13) . . ?
C11 S11 Cs2 104.9(13) . . ?
C12 S11 Cs2 124.0(12) . . ?
S12 S11 K32 148.5(13) . . ?
C11 S11 K32 66.6(13) . . ?
C12 S11 K32 86.1(11) . . ?
Cs2 S11 K32 41.2(6) . . ?
S12 S11 Cs3 20.9(9) . 5_564 ?
C11 S11 Cs3 93.6(13) . 5_564 ?
C12 S11 Cs3 74.5(11) . 5_564 ?
Cs2 S11 Cs3 150.2(7) . 5_564 ?
K32 S11 Cs3 158.8(7) . 5_564 ?
S12 S11 K31 145.5(13) . . ?
C11 S11 K31 62.7(12) . . ?
C12 S11 K31 81.8(11) . . ?
Cs2 S11 K31 42.2(6) . . ?
K32 S11 K31 17.0(7) . . ?
Cs3 S11 K31 145.5(7) 5_564 . ?
S11 S12 C12 83.4(15) . . ?
S11 S12 C11 63.8(14) . . ?
C12 S12 C11 19.7(13) . . ?
S11 S12 Cs3 150.3(13) . 5_564 ?
C12 S12 Cs3 108.3(12) . 5_564 ?
C11 S12 Cs3 126.3(12) . 5_564 ?
S11 S12 K33 141.3(12) . 5_564 ?
C12 S12 K33 103.0(12) . 5_564 ?
C11 S12 K33 119.2(12) . 5_564 ?
Cs3 S12 K33 11.6(6) 5_564 5_564 ?
S11 S12 Cs2 6.8(9) . . ?
C12 S12 Cs2 89.1(11) . . ?
C11 S12 Cs2 69.7(11) . . ?
Cs3 S12 Cs2 144.3(6) 5_564 . ?
K33 S12 Cs2 136.2(6) 5_564 . ?
S11 S12 K8 176.7(13) . 6 ?
C12 S12 K8 99.8(13) . 6 ?
C11 S12 K8 119.4(13) . 6 ?
Cs3 S12 K8 29.0(8) 5_564 6 ?
K33 S12 K8 38.7(9) 5_564 6 ?
Cs2 S12 K8 170.6(8) . 6 ?
S11 S12 K4 157.0(12) . 8_455 ?
C12 S12 K4 76.5(11) . 8_455 ?
C11 S12 K4 95.3(11) . 8_455 ?
Cs3 S12 K4 50.1(6) 5_564 8_455 ?
K33 S12 K4 56.2(6) 5_564 8_455 ?
Cs2 S12 K4 163.8(6) . 8_455 ?
K8 S12 K4 25.6(7) 6 8_455 ?
S22 S21 C21 84.3(14) . . ?
S22 S21 C22 72.4(14) . . ?
C21 S21 C22 12.2(15) . . ?
S22 S21 K8 158.6(15) . 4_454 ?
C21 S21 K8 114.9(14) . 4_454 ?
C22 S21 K8 126.2(14) . 4_454 ?
S22 S21 K5 153.8(12) . 4_454 ?
C21 S21 K5 115.9(11) . 4_454 ?
C22 S21 K5 128.0(11) . 4_454 ?
K8 S21 K5 24.7(12) 4_454 4_454 ?
S22 S21 K4 167.9(13) . 2_554 ?
C21 S21 K4 97.8(11) . 2_554 ?
C22 S21 K4 110.0(11) . 2_554 ?
K8 S21 K4 27.1(10) 4_454 2_554 ?
K5 S21 K4 18.8(7) 4_454 2_554 ?
S22 S21 Cs3 142.4(12) . 3_445 ?
C21 S21 Cs3 97.1(10) . 3_445 ?
C22 S21 Cs3 104.8(10) . 3_445 ?
K8 S21 Cs3 32.2(12) 4_454 3_445 ?
K5 S21 Cs3 55.8(6) 4_454 3_445 ?
K4 S21 Cs3 49.4(6) 2_554 3_445 ?
S22 S21 Cs1 67.8(10) . 5_554 ?
C21 S21 Cs1 67.4(10) . 5_554 ?
C22 S21 Cs1 65.9(10) . 5_554 ?
K8 S21 Cs1 126.8(10) 4_454 5_554 ?
K5 S21 Cs1 103.2(5) 4_454 5_554 ?
K4 S21 Cs1 101.8(5) 2_554 5_554 ?
Cs3 S21 Cs1 146.8(3) 3_445 5_554 ?
S21 S22 C21 73.0(14) . . ?
S21 S22 C22 86.2(15) . . ?
C21 S22 C22 13.5(14) . . ?
S21 S22 K8 17.1(12) . 4_454 ?
C21 S22 K8 88.5(12) . 4_454 ?
C22 S22 K8 101.3(13) . 4_454 ?
S21 S22 K5 139.1(13) . . ?
C21 S22 K5 138.9(11) . . ?
C22 S22 K5 126.1(12) . . ?
K8 S22 K5 122.0(9) 4_454 . ?
S21 S22 K4 129.6(13) . 3_445 ?
C21 S22 K4 156.1(11) . 3_445 ?
C22 S22 K4 142.7(12) . 3_445 ?
K8 S22 K4 113.1(9) 4_454 3_445 ?
K5 S22 K4 18.9(6) . 3_445 ?
S21 S22 Cs1 102.7(11) . 5_554 ?
C21 S22 Cs1 73.4(9) . 5_554 ?
C22 S22 Cs1 71.9(10) . 5_554 ?
K8 S22 Cs1 114.9(8) 4_454 5_554 ?
K5 S22 Cs1 110.5(5) . 5_554 ?
K4 S22 Cs1 104.3(5) 3_445 5_554 ?
S21 S22 K7 159.6(12) . . ?
C21 S22 K7 102.2(10) . . ?
C22 S22 K7 90.7(10) . . ?
K8 S22 K7 163.0(10) 4_454 . ?
K5 S22 K7 56.4(6) . . ?
K4 S22 K7 59.6(6) 3_445 . ?
Cs1 S22 K7 57.3(4) 5_554 . ?
S21 S22 Cs3 31.9(10) . 3_445 ?
C21 S22 Cs3 77.7(10) . 3_445 ?
C22 S22 Cs3 87.6(10) . 3_445 ?
K8 S22 Cs3 27.5(10) 4_454 3_445 ?
K5 S22 Cs3 115.9(5) . 3_445 ?
K4 S22 Cs3 116.7(6) 3_445 3_445 ?
Cs1 S22 Cs3 132.7(3) 5_554 3_445 ?
K7 S22 Cs3 168.1(5) . 3_445 ?
C3 S3 K4 89.4(9) . . ?
C3 S3 K11 68.9(6) . 5_554 ?
K4 S3 K11 119.2(17) . 5_554 ?
C3 S3 K5 72.8(8) . 3 ?
K4 S3 K5 17.1(7) . 3 ?
K11 S3 K5 108.0(16) 5_554 3 ?
C3 S3 Cs1 70.1(5) . 5_554 ?
K4 S3 Cs1 107.7(5) . 5_554 ?
K11 S3 Cs1 11.9(18) 5_554 5_554 ?
K5 S3 Cs1 97.7(4) 3 5_554 ?
K11 Cs1 F3 73.17(13) . 6 ?
K11 Cs1 F3 73.17(13) . 5_554 ?
F3 Cs1 F3 146.3(3) 6 5_554 ?
K11 Cs1 C22 108.7(5) . 5_554 ?
F3 Cs1 C22 131.7(5) 6 5_554 ?
F3 Cs1 C22 61.3(5) 5_554 5_554 ?
K11 Cs1 C22 108.7(5) . 6 ?
F3 Cs1 C22 61.3(5) 6 6 ?
F3 Cs1 C22 131.7(5) 5_554 6 ?
C22 Cs1 C22 142.5(10) 5_554 6 ?
K11 Cs1 K7 180.00(4) . 5_554 ?
F3 Cs1 K7 106.83(13) 6 5_554 ?
F3 Cs1 K7 106.83(13) 5_554 5_554 ?
C22 Cs1 K7 71.3(5) 5_554 5_554 ?
C22 Cs1 K7 71.3(5) 6 5_554 ?
K11 Cs1 C21 103.5(4) . 5_554 ?
F3 Cs1 C21 127.4(5) 6 5_554 ?
F3 Cs1 C21 61.8(5) 5_554 5_554 ?
C22 Cs1 C21 6.4(7) 5_554 5_554 ?
C22 Cs1 C21 147.6(5) 6 5_554 ?
K7 Cs1 C21 76.5(4) 5_554 5_554 ?
K11 Cs1 C21 103.5(4) . 6 ?
F3 Cs1 C21 61.8(5) 6 6 ?
F3 Cs1 C21 127.4(5) 5_554 6 ?
C22 Cs1 C21 147.6(5) 5_554 6 ?
C22 Cs1 C21 6.4(7) 6 6 ?
K7 Cs1 C21 76.5(4) 5_554 6 ?
C21 Cs1 C21 153.0(8) 5_554 6 ?
K11 Cs1 C3 44.1(3) . 5_554 ?
F3 Cs1 C3 93.6(2) 6 5_554 ?
F3 Cs1 C3 61.4(2) 5_554 5_554 ?
C22 Cs1 C3 121.9(6) 5_554 5_554 ?
C22 Cs1 C3 86.1(5) 6 5_554 ?
K7 Cs1 C3 135.9(3) 5_554 5_554 ?
C21 Cs1 C3 120.8(5) 5_554 5_554 ?
C21 Cs1 C3 79.8(5) 6 5_554 ?
K11 Cs1 C3 44.1(3) . 6 ?
F3 Cs1 C3 61.4(2) 6 6 ?
F3 Cs1 C3 93.6(2) 5_554 6 ?
C22 Cs1 C3 86.1(5) 5_554 6 ?
C22 Cs1 C3 121.9(6) 6 6 ?
K7 Cs1 C3 135.9(3) 5_554 6 ?
C21 Cs1 C3 79.8(5) 5_554 6 ?
C21 Cs1 C3 120.8(5) 6 6 ?
C3 Cs1 C3 88.2(5) 5_554 6 ?
K11 Cs1 S22 117.57(15) . 5_554 ?
F3 Cs1 S22 107.41(19) 6 5_554 ?
F3 Cs1 S22 88.20(18) 5_554 5_554 ?
C22 Cs1 S22 27.1(5) 5_554 5_554 ?
C22 Cs1 S22 126.4(5) 6 5_554 ?
K7 Cs1 S22 62.43(15) 5_554 5_554 ?
C21 Cs1 S22 26.6(5) 5_554 5_554 ?
C21 Cs1 S22 132.7(4) 6 5_554 ?
C3 Cs1 S22 146.8(3) 5_554 5_554 ?
C3 Cs1 S22 80.1(3) 6 5_554 ?
K11 Cs1 S22 117.57(16) . 6 ?
F3 Cs1 S22 88.20(18) 6 6 ?
F3 Cs1 S22 107.41(19) 5_554 6 ?
C22 Cs1 S22 126.4(5) 5_554 6 ?
C22 Cs1 S22 27.1(5) 6 6 ?
K7 Cs1 S22 62.43(15) 5_554 6 ?
C21 Cs1 S22 132.7(4) 5_554 6 ?
C21 Cs1 S22 26.6(5) 6 6 ?
C3 Cs1 S22 80.1(3) 5_554 6 ?
C3 Cs1 S22 146.8(3) 6 6 ?
S22 Cs1 S22 124.9(3) 5_554 6 ?
Cs1 K11 F3 87(3) . 5_554 ?
Cs1 K11 F3 87(3) . 6 ?
F3 K11 F3 174(5) 5_554 6 ?
Cs1 K11 C3 123(2) . 5_554 ?
F3 K11 C3 71.8(10) 5_554 5_554 ?
F3 K11 C3 111.8(18) 6 5_554 ?
Cs1 K11 C3 123(2) . 6 ?
F3 K11 C3 111.8(18) 5_554 6 ?
F3 K11 C3 71.8(10) 6 6 ?
C3 K11 C3 115(4) 5_554 6 ?
Cs1 K11 S3 126.4(18) . 5_554 ?
F3 K11 S3 101.5(16) 5_554 5_554 ?
F3 K11 S3 82.3(12) 6 5_554 ?
C3 K11 S3 29.7(7) 5_554 5_554 ?
C3 K11 S3 103(3) 6 5_554 ?
Cs1 K11 S3 126.4(18) . 6 ?
F3 K11 S3 82.3(12) 5_554 6 ?
F3 K11 S3 101.5(16) 6 6 ?
C3 K11 S3 103(3) 5_554 6 ?
C3 K11 S3 29.7(7) 6 6 ?
S3 K11 S3 107(4) 5_554 6 ?
Cs1 K11 N3 114(2) . 5_554 ?
F3 K11 N3 51.9(6) 5_554 5_554 ?
F3 K11 N3 131.4(19) 6 5_554 ?
C3 K11 N3 20.0(4) 5_554 5_554 ?
C3 K11 N3 120(4) 6 5_554 ?
S3 K11 N3 49.6(10) 5_554 5_554 ?
S3 K11 N3 99(3) 6 5_554 ?
Cs1 K11 N3 114(2) . 6 ?
F3 K11 N3 131.4(19) 5_554 6 ?
F3 K11 N3 51.9(6) 6 6 ?
C3 K11 N3 120(4) 5_554 6 ?
C3 K11 N3 20.0(4) 6 6 ?
S3 K11 N3 99(3) 5_554 6 ?
S3 K11 N3 49.6(10) 6 6 ?
N3 K11 N3 132(4) 5_554 6 ?
Cs1 K11 K7 0.000(8) . 5_554 ?
F3 K11 K7 87(3) 5_554 5_554 ?
F3 K11 K7 87(3) 6 5_554 ?
C3 K11 K7 123(2) 5_554 5_554 ?
C3 K11 K7 123(2) 6 5_554 ?
S3 K11 K7 126.4(18) 5_554 5_554 ?
S3 K11 K7 126.4(18) 6 5_554 ?
N3 K11 K7 114(2) 5_554 5_554 ?
N3 K11 K7 114(2) 6 5_554 ?
K32 Cs2 S11 93.7(11) . . ?
K32 Cs2 K31 27.1(10) . . ?
S11 Cs2 K31 103.3(10) . . ?
K32 Cs2 F2 168.7(11) . 5_564 ?
S11 Cs2 F2 83.5(5) . 5_564 ?
K31 Cs2 F2 143.3(9) . 5_564 ?
K32 Cs2 C11 64.5(12) . . ?
S11 Cs2 C11 31.7(7) . . ?
K31 Cs2 C11 71.6(10) . . ?
F2 Cs2 C11 110.0(8) 5_564 . ?
K32 Cs2 S12 96.8(11) . . ?
S11 Cs2 S12 3.1(4) . . ?
K31 Cs2 S12 105.9(9) . . ?
F2 Cs2 S12 80.4(4) 5_564 . ?
C11 Cs2 S12 34.4(7) . . ?
K32 Cs2 K33 53.9(10) . . ?
S11 Cs2 K33 104.1(7) . . ?
K31 Cs2 K33 27.2(9) . . ?
F2 Cs2 K33 116.1(6) 5_564 . ?
C11 Cs2 K33 76.8(8) . . ?
S12 Cs2 K33 105.5(6) . . ?
K32 Cs2 C12 71.0(11) . . ?
S11 Cs2 C12 25.6(6) . . ?
K31 Cs2 C12 77.8(10) . . ?
F2 Cs2 C12 103.7(6) 5_564 . ?
C11 Cs2 C12 6.5(8) . . ?
S12 Cs2 C12 28.1(5) . . ?
K33 Cs2 C12 81.2(7) . . ?
K32 Cs2 Cs3 64.5(10) . . ?
S11 Cs2 Cs3 98.0(6) . . ?
K31 Cs2 Cs3 38.8(8) . . ?
F2 Cs2 Cs3 104.9(4) 5_564 . ?
C11 Cs2 Cs3 74.6(7) . . ?
S12 Cs2 Cs3 98.8(5) . . ?
K33 Cs2 Cs3 12.5(5) . . ?
C12 Cs2 Cs3 77.8(6) . . ?
K32 Cs2 K7 92.3(12) . 1_565 ?
S11 Cs2 K7 167.4(6) . 1_565 ?
K31 Cs2 K7 77.7(9) . 1_565 ?
F2 Cs2 K7 88.4(5) 5_564 1_565 ?
C11 Cs2 K7 147.5(8) . 1_565 ?
S12 Cs2 K7 165.3(5) . 1_565 ?
K33 Cs2 K7 70.9(6) . 1_565 ?
C12 Cs2 K7 152.1(7) . 1_565 ?
Cs3 Cs2 K7 74.8(5) . 1_565 ?
K32 Cs2 C12 109.6(11) . 5_564 ?
S11 Cs2 C12 70.9(6) . 5_564 ?
K31 Cs2 C12 88.7(10) . 5_564 ?
F2 Cs2 C12 59.1(5) 5_564 5_564 ?
C11 Cs2 C12 72.4(7) . 5_564 ?
S12 Cs2 C12 69.4(5) . 5_564 ?
K33 Cs2 C12 64.3(7) . 5_564 ?
C12 Cs2 C12 69.7(8) . 5_564 ?
Cs3 Cs2 C12 51.7(5) . 5_564 ?
K7 Cs2 C12 96.7(5) 1_565 5_564 ?
K32 Cs2 C22 130.6(12) . 1_565 ?
S11 Cs2 C22 115.8(7) . 1_565 ?
K31 Cs2 C22 138.2(11) . 1_565 ?
F2 Cs2 C22 59.8(5) 5_564 1_565 ?
C11 Cs2 C22 145.0(8) . 1_565 ?
S12 Cs2 C22 113.8(6) . 1_565 ?
K33 Cs2 C22 138.2(7) . 1_565 ?
C12 Cs2 C22 140.3(7) . 1_565 ?
Cs3 Cs2 C22 139.0(6) . 1_565 ?
K7 Cs2 C22 67.5(6) 1_565 1_565 ?
C12 Cs2 C22 117.0(7) 5_564 1_565 ?
K33 Cs3 K8 100(3) . 2_564 ?
K33 Cs3 K31 16(2) . . ?
K8 Cs3 K31 115.9(19) 2_564 . ?
K33 Cs3 S12 136(2) . 5_564 ?
K8 Cs3 S12 115.2(15) 2_564 5_564 ?
K31 Cs3 S12 121.8(13) . 5_564 ?
K33 Cs3 F1 76.7(17) . . ?
K8 Cs3 F1 141.0(13) 2_564 . ?
K31 Cs3 F1 66.9(8) . . ?
S12 Cs3 F1 89.3(6) 5_564 . ?
K33 Cs3 K4 107(2) . 4_554 ?
K8 Cs3 K4 32.1(12) 2_564 4_554 ?
K31 Cs3 K4 118.2(11) . 4_554 ?
S12 Cs3 K4 92.6(8) 5_564 4_554 ?
F1 Cs3 K4 172.0(8) . 4_554 ?
K33 Cs3 S11 130(2) . 5_564 ?
K8 Cs3 S11 124.0(15) 2_564 5_564 ?
K31 Cs3 S11 114.6(12) . 5_564 ?
S12 Cs3 S11 8.9(4) 5_564 5_564 ?
F1 Cs3 S11 81.3(5) . 5_564 ?
K4 Cs3 S11 101.0(8) 4_554 5_564 ?
K33 Cs3 K5 96(2) . 2_564 ?
K8 Cs3 K5 15.4(12) 2_564 2_564 ?
K31 Cs3 K5 110.2(12) . 2_564 ?
S12 Cs3 K5 111.6(8) 5_564 2_564 ?
F1 Cs3 K5 154.5(7) . 2_564 ?
K4 Cs3 K5 20.3(7) 4_554 2_564 ?
S11 Cs3 K5 120.3(7) 5_564 2_564 ?
K33 Cs3 C12 119(2) . 5_564 ?
K8 Cs3 C12 105.8(14) 2_564 5_564 ?
K31 Cs3 C12 109.4(12) . 5_564 ?
S12 Cs3 C12 29.4(6) 5_564 5_564 ?
F1 Cs3 C12 109.4(8) . 5_564 ?
K4 Cs3 C12 75.3(8) 4_554 5_564 ?
S11 Cs3 C12 33.3(6) 5_564 5_564 ?
K5 Cs3 C12 95.6(8) 2_564 5_564 ?
K33 Cs3 K32 27(2) . . ?
K8 Cs3 K32 123.3(17) 2_564 . ?
K31 Cs3 K32 13.4(12) . . ?
S12 Cs3 K32 109.3(9) 5_564 . ?
F1 Cs3 K32 69.0(6) . . ?
K4 Cs3 K32 117.4(9) 4_554 . ?
S11 Cs3 K32 102.7(8) 5_564 . ?
K5 Cs3 K32 114.4(9) 2_564 . ?
C12 Cs3 K32 96.1(9) 5_564 . ?
K33 Cs3 N3 86.1(19) . . ?
K8 Cs3 N3 90.5(12) 2_564 . ?
K31 Cs3 N3 89.1(9) . . ?
S12 Cs3 N3 116.4(7) 5_564 . ?
F1 Cs3 N3 50.7(3) . . ?
K4 Cs3 N3 121.8(7) 4_554 . ?
S11 Cs3 N3 113.0(6) 5_564 . ?
K5 Cs3 N3 105.0(6) 2_564 . ?
C12 Cs3 N3 145.7(8) 5_564 . ?
K32 Cs3 N3 99.8(7) . . ?
K33 Cs3 S21 133(2) . 3 ?
K8 Cs3 S21 46.0(14) 2_564 3 ?
K31 Cs3 S21 145.9(12) . 3 ?
S12 Cs3 S21 91.0(6) 5_564 3 ?
F1 Cs3 S21 108.0(5) . 3 ?
K4 Cs3 S21 64.2(6) 4_554 3 ?
S11 Cs3 S21 97.0(5) 5_564 3 ?
K5 Cs3 S21 59.1(5) 2_564 3 ?
C12 Cs3 S21 104.1(7) 5_564 3 ?
K32 Cs3 S21 159.2(9) . 3 ?
N3 Cs3 S21 65.9(3) . 3 ?
K32 K31 K33 147(4) . . ?
K32 K31 Cs3 141(3) . . ?
K33 K31 Cs3 9.3(14) . . ?
K32 K31 Cs2 49.9(19) . . ?
K33 K31 Cs2 99.4(18) . . ?
Cs3 K31 Cs2 96.2(13) . . ?
K32 K31 F1 112(2) . . ?
K33 K31 F1 72.3(15) . . ?
Cs3 K31 F1 66.6(9) . . ?
Cs2 K31 F1 123.4(15) . . ?
K32 K31 C11 57(2) . . ?
K33 K31 C11 101(2) . . ?
Cs3 K31 C11 91.4(14) . . ?
Cs2 K31 C11 60.9(10) . . ?
F1 K31 C11 65.9(9) . . ?
K32 K31 K8 149(2) . 2_564 ?
K33 K31 K8 19.8(16) . 2_564 ?
Cs3 K31 K8 28.9(11) . 2_564 ?
Cs2 K31 K8 99.9(11) . 2_564 ?
F1 K31 K8 88.7(12) . 2_564 ?
C11 K31 K8 118.3(14) . 2_564 ?
K32 K31 S11 48(2) . . ?
K33 K31 S11 101(2) . . ?
Cs3 K31 S11 93.0(13) . . ?
Cs2 K31 S11 34.5(6) . . ?
F1 K31 S11 90.5(10) . . ?
C11 K31 S11 26.5(7) . . ?
K8 K31 S11 112.2(12) 2_564 . ?
K32 K31 K7 94.2(19) . 1_565 ?
K33 K31 K7 78.4(14) . 1_565 ?
Cs3 K31 K7 84.7(9) . 1_565 ?
Cs2 K31 K7 64.0(7) . 1_565 ?
F1 K31 K7 150.6(11) . 1_565 ?
C11 K31 K7 123.9(11) . 1_565 ?
K8 K31 K7 62.0(9) 2_564 1_565 ?
S11 K31 K7 97.7(7) . 1_565 ?
K32 K31 K5 65(2) . 1_565 ?
K33 K31 K5 123.5(18) . 1_565 ?
Cs3 K31 K5 131.2(12) . 1_565 ?
Cs2 K31 K5 73.9(9) . 1_565 ?
F1 K31 K5 156.8(11) . 1_565 ?
C11 K31 K5 121.0(11) . 1_565 ?
K8 K31 K5 104.3(12) 2_564 1_565 ?
S11 K31 K5 101.8(9) . 1_565 ?
K7 K31 K5 47.5(5) 1_565 1_565 ?
K32 K31 K4 129(2) . 4_554 ?
K33 K31 K4 29.4(12) . 4_554 ?
Cs3 K31 K4 35.1(7) . 4_554 ?
Cs2 K31 K4 80.2(8) . 4_554 ?
F1 K31 K4 101.5(10) . 4_554 ?
C11 K31 K4 109.9(11) . 4_554 ?
K8 K31 K4 19.8(7) 2_564 4_554 ?
S11 K31 K4 96.8(8) . 4_554 ?
K7 K31 K4 49.6(5) 1_565 4_554 ?
K5 K31 K4 96.6(8) 1_565 4_554 ?
K32 K31 K5 137(2) . 2_564 ?
K33 K31 K5 33.5(14) . 2_564 ?
Cs3 K31 K5 41.6(8) . 2_564 ?
Cs2 K31 K5 90.4(8) . 2_564 ?
F1 K31 K5 104.2(10) . 2_564 ?
C11 K31 K5 123.9(12) . 2_564 ?
K8 K31 K5 15.5(8) 2_564 2_564 ?
S11 K31 K5 110.5(8) . 2_564 ?
K7 K31 K5 46.5(5) 1_565 2_564 ?
K5 K31 K5 90.0(8) 1_565 2_564 ?
K4 K31 K5 14.2(5) 4_554 2_564 ?
K31 K32 Cs2 103(2) . . ?
K31 K32 K33 18(2) . . ?
Cs2 K32 K33 86.5(12) . . ?
K31 K32 C11 102(3) . . ?
Cs2 K32 C11 75.7(14) . . ?
K33 K32 C11 91.1(14) . . ?
K31 K32 S11 115(3) . . ?
Cs2 K32 S11 45.1(9) . . ?
K33 K32 S11 97.9(13) . . ?
C11 K32 S11 32.4(8) . . ?
K31 K32 Cs3 26(2) . . ?
Cs2 K32 Cs3 81.9(10) . . ?
K33 K32 Cs3 8.9(8) . . ?
C11 K32 Cs3 82.6(11) . . ?
S11 K32 Cs3 89.2(9) . . ?
K31 K32 N1 92(2) . . ?
Cs2 K32 N1 94.6(14) . . ?
K33 K32 N1 86.2(11) . . ?
C11 K32 N1 19.9(7) . . ?
S11 K32 N1 52.3(7) . . ?
Cs3 K32 N1 79.0(8) . . ?
K31 K32 C12 103(3) . . ?
Cs2 K32 C12 75.6(13) . . ?
K33 K32 C12 92.0(12) . . ?
C11 K32 C12 0.9(9) . . ?
S11 K32 C12 32.1(7) . . ?
Cs3 K32 C12 83.4(10) . . ?
N1 K32 C12 20.2(6) . . ?
K31 K32 I1 93.9(19) . . ?
Cs2 K32 I1 144.9(15) . . ?
K33 K32 I1 103.8(9) . . ?
C11 K32 I1 70.7(9) . . ?
S11 K32 I1 99.9(9) . . ?
Cs3 K32 I1 103.2(7) . . ?
N1 K32 I1 53.7(4) . . ?
C12 K32 I1 70.7(7) . . ?
K31 K32 K5 99(3) . 1_565 ?
Cs2 K32 K5 87.3(10) . 1_565 ?
K33 K32 K5 105.8(12) . 1_565 ?
C11 K32 K5 155.3(13) . 1_565 ?
S11 K32 K5 125.0(9) . 1_565 ?
Cs3 K32 K5 113.0(10) . 1_565 ?
N1 K32 K5 168.0(11) . 1_565 ?
C12 K32 K5 154.6(11) . 1_565 ?
I1 K32 K5 120.6(9) . 1_565 ?
K31 K32 K7 69.6(19) . 1_565 ?
Cs2 K32 K7 59.7(8) . 1_565 ?
K33 K32 K7 66.0(8) . 1_565 ?
C11 K32 K7 129.9(11) . 1_565 ?
S11 K32 K7 104.1(8) . 1_565 ?
Cs3 K32 K7 70.4(6) . 1_565 ?
N1 K32 K7 141.9(9) . 1_565 ?
C12 K32 K7 130.2(10) . 1_565 ?
I1 K32 K7 154.9(10) . 1_565 ?
K5 K32 K7 48.2(5) 1_565 1_565 ?
K31 K32 K8 86(3) . 1_565 ?
Cs2 K32 K8 102.7(12) . 1_565 ?
K33 K32 K8 96.7(13) . 1_565 ?
C11 K32 K8 171.9(14) . 1_565 ?
S11 K32 K8 143.2(10) . 1_565 ?
Cs3 K32 K8 105.1(10) . 1_565 ?
N1 K32 K8 162.6(10) . 1_565 ?
C12 K32 K8 171.1(12) . 1_565 ?
I1 K32 K8 109.1(9) . 1_565 ?
K5 K32 K8 18.3(6) 1_565 1_565 ?
K7 K32 K8 52.8(6) 1_565 1_565 ?
Cs3 K33 K31 155(4) . . ?
Cs3 K33 K8 57(2) . 2_564 ?
K31 K33 K8 147(3) . 2_564 ?
Cs3 K33 K32 144(3) . . ?
K31 K33 K32 14.8(18) . . ?
K8 K33 K32 150.1(17) 2_564 . ?
Cs3 K33 F1 85.8(19) . . ?
K31 K33 F1 78.0(14) . . ?
K8 K33 F1 127.2(15) 2_564 . ?
K32 K33 F1 81.8(9) . . ?
Cs3 K33 S12 32(2) . 5_564 ?
K31 K33 S12 124(2) . 5_564 ?
K8 K33 S12 84.6(15) 2_564 5_564 ?
K32 K33 S12 112.0(13) . 5_564 ?
F1 K33 S12 78.3(7) . 5_564 ?
Cs3 K33 Cs2 115(2) . . ?
K31 K33 Cs2 53.5(15) . . ?
K8 K33 Cs2 121.7(12) 2_564 . ?
K32 K33 Cs2 39.6(8) . . ?
F1 K33 Cs2 107.2(8) . . ?
S12 K33 Cs2 87.6(8) 5_564 . ?
Cs3 K33 K4 58.4(18) . 4_554 ?
K31 K33 K4 137.9(16) . 4_554 ?
K8 K33 K4 27.3(10) 2_564 4_554 ?
K32 K33 K4 131.0(10) . 4_554 ?
F1 K33 K4 143.5(11) . 4_554 ?
S12 K33 K4 74.3(8) 5_564 4_554 ?
Cs2 K33 K4 95.5(7) . 4_554 ?
Cs3 K33 K5 69(2) . 2_564 ?
K31 K33 K5 132.8(18) . 2_564 ?
K8 K33 K5 18.1(12) 2_564 2_564 ?
K32 K33 K5 132.4(11) . 2_564 ?
F1 K33 K5 145.2(10) . 2_564 ?
S12 K33 K5 91.2(8) 5_564 2_564 ?
Cs2 K33 K5 105.4(7) . 2_564 ?
K4 K33 K5 19.1(6) 4_554 2_564 ?
Cs3 K33 K7 115.2(19) . 1_565 ?
K31 K33 K7 80.7(15) . 1_565 ?
K8 K33 K7 71.8(13) 2_564 1_565 ?
K32 K33 K7 78.4(8) . 1_565 ?
F1 K33 K7 158.5(9) . 1_565 ?
S12 K33 K7 116.9(7) 5_564 1_565 ?
Cs2 K33 K7 61.1(5) . 1_565 ?
K4 K33 K7 58.0(6) 4_554 1_565 ?
K5 K33 K7 54.0(5) 2_564 1_565 ?
K5 K4 K8 60(2) 3 3 ?
K5 K4 Cs3 95(2) 3 4_544 ?
K8 K4 Cs3 38.1(19) 3 4_544 ?
K5 K4 S3 107(2) 3 . ?
K8 K4 S3 126(2) 3 . ?
Cs3 K4 S3 134.2(12) 4_544 . ?
K5 K4 K33 87(2) 3 4_544 ?
K8 K4 K33 38.6(18) 3 4_544 ?
Cs3 K4 K33 14.7(5) 4_544 4_544 ?
S3 K4 K33 148.9(12) . 4_544 ?
K5 K4 S22 79(2) 3 3 ?
K8 K4 S22 138(2) 3 3 ?
Cs3 K4 S22 151.3(11) 4_544 3 ?
S3 K4 S22 73.8(6) . 3 ?
K33 K4 S22 137.0(10) 4_544 3 ?
K5 K4 S21 74.1(19) 3 2_554 ?
K8 K4 S21 45.6(17) 3 2_554 ?
Cs3 K4 S21 66.4(6) 4_544 2_554 ?
S3 K4 S21 80.9(6) . 2_554 ?
K33 K4 S21 76.2(7) 4_544 2_554 ?
S22 K4 S21 136.0(9) 3 2_554 ?
K5 K4 C3 80(2) 3 . ?
K8 K4 C3 116.4(19) 3 . ?
Cs3 K4 C3 144.8(10) 4_544 . ?
S3 K4 C3 27.3(3) . . ?
K33 K4 C3 154.2(9) 4_544 . ?
S22 K4 C3 62.3(6) 3 . ?
S21 K4 C3 78.8(6) 2_554 . ?
K5 K4 K7 72(2) 3 3 ?
K8 K4 K7 90(2) 3 3 ?
Cs3 K4 K7 85.9(8) 4_544 3 ?
S3 K4 K7 138.9(10) . 3 ?
K33 K4 K7 71.5(8) 4_544 3 ?
S22 K4 K7 65.5(7) 3 3 ?
S21 K4 K7 133.5(9) 2_554 3 ?
C3 K4 K7 124.0(10) . 3 ?
K5 K4 S12 129(2) 3 8_556 ?
K8 K4 S12 69(2) 3 8_556 ?
Cs3 K4 S12 37.3(6) 4_544 8_556 ?
S3 K4 S12 103.3(9) . 8_556 ?
K33 K4 S12 49.4(7) 4_544 8_556 ?
S22 K4 S12 149.1(8) 3 8_556 ?
S21 K4 S12 71.3(6) 2_554 8_556 ?
C3 K4 S12 126.5(9) . 8_556 ?
K7 K4 S12 108.6(8) 3 8_556 ?
K5 K4 K31 86(2) 3 4_544 ?
K8 K4 K31 47.1(18) 3 4_544 ?
Cs3 K4 K31 26.8(6) 4_544 4_544 ?
S3 K4 K31 160.1(12) . 4_544 ?
K33 K4 K31 12.7(6) 4_544 4_544 ?
S22 K4 K31 124.6(9) 3 4_544 ?
S21 K4 K31 88.0(7) 2_554 4_544 ?
C3 K4 K31 162.9(9) . 4_544 ?
K7 K4 K31 59.2(7) 3 4_544 ?
S12 K4 K31 57.3(7) 8_556 4_544 ?
K5 K4 Cs2 109(2) 3 4_544 ?
K8 K4 Cs2 79.1(18) 3 4_544 ?
Cs3 K4 Cs2 49.4(5) 4_544 4_544 ?
S3 K4 Cs2 144.1(8) . 4_544 ?
K33 K4 Cs2 41.4(5) 4_544 4_544 ?
S22 K4 Cs2 105.6(6) 3 4_544 ?
S21 K4 Cs2 115.8(8) 2_554 4_544 ?
C3 K4 Cs2 164.4(7) . 4_544 ?
K7 K4 Cs2 50.6(4) 3 4_544 ?
S12 K4 Cs2 58.5(5) 8_556 4_544 ?
K31 K4 Cs2 32.2(5) 4_544 4_544 ?
K4 K5 K8 78(3) 3_445 . ?
K4 K5 Cs3 65(2) 3_445 2_544 ?
K8 K5 Cs3 20.5(17) . 2_544 ?
K4 K5 S21 87(2) 3_445 4_444 ?
K8 K5 S21 47.8(19) . 4_444 ?
Cs3 K5 S21 65.1(7) 2_544 4_444 ?
K4 K5 S22 82(2) 3_445 . ?
K8 K5 S22 157(2) . . ?
Cs3 K5 S22 136.8(8) 2_544 . ?
S21 K5 S22 143.0(9) 4_444 . ?
K4 K5 K33 74(2) 3_445 2_544 ?
K8 K5 K33 28.5(18) . 2_544 ?
Cs3 K5 K33 14.7(5) 2_544 2_544 ?
S21 K5 K33 76.1(8) 4_444 2_544 ?
S22 K5 K33 132.6(8) . 2_544 ?
K4 K5 K7 90(2) 3_445 . ?
K8 K5 K7 100(2) . . ?
Cs3 K5 K7 84.7(7) 2_544 . ?
S21 K5 K7 147.8(10) 4_444 . ?
S22 K5 K7 67.8(7) . . ?
K33 K5 K7 72.3(7) 2_544 . ?
K4 K5 C3 82(2) 3_445 3_445 ?
K8 K5 C3 125(2) . 3_445 ?
Cs3 K5 C3 132.4(10) 2_544 3_445 ?
S21 K5 C3 80.8(6) 4_444 3_445 ?
S22 K5 C3 62.7(5) . 3_445 ?
K33 K5 C3 147.0(11) 2_544 3_445 ?
K7 K5 C3 130.5(9) . 3_445 ?
K4 K5 S3 56.3(19) 3_445 3_445 ?
K8 K5 S3 109(2) . 3_445 ?
Cs3 K5 S3 109.5(9) 2_544 3_445 ?
S21 K5 S3 76.1(6) 4_444 3_445 ?
S22 K5 S3 68.3(5) . 3_445 ?
K33 K5 S3 123.2(10) 2_544 3_445 ?
K7 K5 S3 127.5(8) . 3_445 ?
C3 K5 S3 26.1(3) 3_445 3_445 ?
K4 K5 K32 160(2) 3_445 1_545 ?
K8 K5 K32 101(2) . 1_545 ?
Cs3 K5 K32 108.2(9) 2_544 1_545 ?
S21 K5 K32 107.6(7) 4_444 1_545 ?
S22 K5 K32 93.4(9) . 1_545 ?
K33 K5 K32 96.0(9) 2_544 1_545 ?
K7 K5 K32 70.1(7) . 1_545 ?
C3 K5 K32 113.4(9) 3_445 1_545 ?
S3 K5 K32 139.5(10) 3_445 1_545 ?
K4 K5 I3 138(2) 3_445 7_444 ?
K8 K5 I3 100.4(18) . 7_444 ?
Cs3 K5 I3 120.8(7) 2_544 7_444 ?
S21 K5 I3 64.2(4) 4_444 7_444 ?
S22 K5 I3 102.3(8) . 7_444 ?
K33 K5 I3 123.1(7) 2_544 7_444 ?
K7 K5 I3 130.9(9) . 7_444 ?
C3 K5 I3 64.1(5) 3_445 7_444 ?
S3 K5 I3 85.6(5) 3_445 7_444 ?
K32 K5 I3 62.5(6) 1_545 7_444 ?
K4 K5 K31 147(2) 3_445 1_545 ?
K8 K5 K31 90(2) . 1_545 ?
Cs3 K5 K31 93.8(8) 2_544 1_545 ?
S21 K5 K31 108.0(7) 4_444 1_545 ?
S22 K5 K31 100.4(9) . 1_545 ?
K33 K5 K31 80.9(9) 2_544 1_545 ?
K7 K5 K31 61.0(7) . 1_545 ?
C3 K5 K31 129.2(10) 3_445 1_545 ?
S3 K5 K31 155.2(10) 3_445 1_545 ?
K32 K5 K31 15.7(6) 1_545 1_545 ?
I3 K5 K31 75.0(6) 7_444 1_545 ?
K5 K7 K5 134.6(12) . 2_554 ?
K5 K7 K4 18.1(6) . 3_445 ?
K5 K7 K4 141.0(10) 2_554 3_445 ?
K5 K7 K4 141.0(10) . 4_544 ?
K5 K7 K4 18.1(6) 2_554 4_544 ?
K4 K7 K4 154.0(12) 3_445 4_544 ?
K5 K7 Cs1 112.7(6) . 5_554 ?
K5 K7 Cs1 112.7(6) 2_554 5_554 ?
K4 K7 Cs1 103.0(6) 3_445 5_554 ?
K4 K7 Cs1 103.0(6) 4_544 5_554 ?
K5 K7 Cs2 93.9(6) . 2_544 ?
K5 K7 Cs2 76.5(6) 2_554 2_544 ?
K4 K7 Cs2 81.1(6) 3_445 2_544 ?
K4 K7 Cs2 93.3(6) 4_544 2_544 ?
Cs1 K7 Cs2 102.3(5) 5_554 2_544 ?
K5 K7 Cs2 76.5(6) . 1_545 ?
K5 K7 Cs2 93.9(6) 2_554 1_545 ?
K4 K7 Cs2 93.3(6) 3_445 1_545 ?
K4 K7 Cs2 81.1(6) 4_544 1_545 ?
Cs1 K7 Cs2 102.3(5) 5_554 1_545 ?
Cs2 K7 Cs2 155.4(9) 2_544 1_545 ?
K5 K7 S22 160.9(6) . 2_554 ?
K5 K7 S22 55.8(5) 2_554 2_554 ?
K4 K7 S22 142.9(6) 3_445 2_554 ?
K4 K7 S22 54.9(5) 4_544 2_554 ?
Cs1 K7 S22 60.3(4) 5_554 2_554 ?
Cs2 K7 S22 71.9(2) 2_544 2_554 ?
Cs2 K7 S22 121.5(3) 1_545 2_554 ?
K5 K7 S22 55.8(5) . . ?
K5 K7 S22 160.9(6) 2_554 . ?
K4 K7 S22 54.9(5) 3_445 . ?
K4 K7 S22 142.9(6) 4_544 . ?
Cs1 K7 S22 60.3(4) 5_554 . ?
Cs2 K7 S22 121.5(3) 2_544 . ?
Cs2 K7 S22 71.9(2) 1_545 . ?
S22 K7 S22 120.5(8) 2_554 . ?
K5 K7 K8 21.3(8) . . ?
K5 K7 K8 117.5(11) 2_554 . ?
K4 K7 K8 24.6(7) 3_445 . ?
K4 K7 K8 129.4(10) 4_544 . ?
Cs1 K7 K8 127.6(7) 5_554 . ?
Cs2 K7 K8 76.2(8) 2_544 . ?
Cs2 K7 K8 88.8(8) 1_545 . ?
S22 K7 K8 148.0(8) 2_554 . ?
S22 K7 K8 75.9(7) . . ?
K5 K7 K8 117.5(11) . 2_554 ?
K5 K7 K8 21.3(8) 2_554 2_554 ?
K4 K7 K8 129.4(10) 3_445 2_554 ?
K4 K7 K8 24.6(7) 4_544 2_554 ?
Cs1 K7 K8 127.6(7) 5_554 2_554 ?
Cs2 K7 K8 88.8(8) 2_544 2_554 ?
Cs2 K7 K8 76.2(8) 1_545 2_554 ?
S22 K7 K8 75.9(7) 2_554 2_554 ?
S22 K7 K8 148.0(8) . 2_554 ?
K8 K7 K8 104.8(13) . 2_554 ?
K5 K7 K33 91.3(8) . 1_545 ?
K5 K7 K33 53.7(7) 2_554 1_545 ?
K4 K7 K33 107.8(8) 3_445 1_545 ?
K4 K7 K33 50.5(6) 4_544 1_545 ?
Cs1 K7 K33 137.5(5) 5_554 1_545 ?
Cs2 K7 K33 110.8(7) 2_544 1_545 ?
Cs2 K7 K33 48.0(5) 1_545 1_545 ?
S22 K7 K33 105.4(4) 2_554 1_545 ?
S22 K7 K33 117.7(4) . 1_545 ?
K8 K7 K33 86.8(9) . 1_545 ?
K8 K7 K33 32.6(8) 2_554 1_545 ?
K5 K8 K4 41.6(18) . 3_445 ?
K5 K8 Cs3 144(3) . 2_544 ?
K4 K8 Cs3 110(2) 3_445 2_544 ?
K5 K8 K33 133(3) . 2_544 ?
K4 K8 K33 114(2) 3_445 2_544 ?
Cs3 K8 K33 22.5(10) 2_544 2_544 ?
K5 K8 S21 108(2) . 4_444 ?
K4 K8 S21 107(2) 3_445 4_444 ?
Cs3 K8 S21 102(2) 2_544 4_444 ?
K33 K8 S21 119(2) 2_544 4_444 ?
K5 K8 S22 109(2) . 4_444 ?
K4 K8 S22 111(2) 3_445 4_444 ?
Cs3 K8 S22 101.9(19) 2_544 4_444 ?
K33 K8 S22 117.6(19) 2_544 4_444 ?
S21 K8 S22 4.3(3) 4_444 4_444 ?
K5 K8 K31 124(2) . 2_544 ?
K4 K8 K31 113(2) 3_445 2_544 ?
Cs3 K8 K31 35.2(12) 2_544 2_544 ?
K33 K8 K31 12.8(10) 2_544 2_544 ?
S21 K8 K31 128.7(17) 4_444 2_544 ?
S22 K8 K31 126.8(15) 4_444 2_544 ?
K5 K8 S12 127(2) . 6_556 ?
K4 K8 S12 85(2) 3_445 6_556 ?
Cs3 K8 S12 35.8(11) 2_544 6_556 ?
K33 K8 S12 56.7(14) 2_544 6_556 ?
S21 K8 S12 85.5(14) 4_444 6_556 ?
S22 K8 S12 87.9(12) 4_444 6_556 ?
K31 K8 S12 68.4(11) 2_544 6_556 ?
K5 K8 K7 58.5(18) . . ?
K4 K8 K7 65.7(18) 3_445 . ?
Cs3 K8 K7 92.7(15) 2_544 . ?
K33 K8 K7 75.6(13) 2_544 . ?
S21 K8 K7 165.4(19) 4_444 . ?
S22 K8 K7 165.1(17) 4_444 . ?
K31 K8 K7 65.1(9) 2_544 . ?
S12 K8 K7 106.0(10) 6_556 . ?
K5 K8 K32 61(2) . 1_545 ?
K4 K8 K32 100(2) 3_445 1_545 ?
Cs3 K8 K32 126.5(19) 2_544 1_545 ?
K33 K8 K32 104.5(17) 2_544 1_545 ?
S21 K8 K32 110.3(13) 4_444 1_545 ?
S22 K8 K32 107.3(11) 4_444 1_545 ?
K31 K8 K32 92.5(13) 2_544 1_545 ?
S12 K8 K32 160.6(13) 6_556 1_545 ?
K7 K8 K32 60.5(8) . 1_545 ?
K5 K8 K31 72(2) . 1_545 ?
K4 K8 K31 108(2) 3_445 1_545 ?
Cs3 K8 K31 111.4(18) 2_544 1_545 ?
K33 K8 K31 89.5(15) 2_544 1_545 ?
S21 K8 K31 118.4(13) 4_444 1_545 ?
S22 K8 K31 114.7(11) 4_444 1_545 ?
K31 K8 K31 77.6(12) 2_544 1_545 ?
S12 K8 K31 146.0(13) 6_556 1_545 ?
K7 K8 K31 55.8(8) . 1_545 ?
K32 K8 K31 15.1(6) 1_545 1_545 ?
K5 K8 K32 118(2) . 2_544 ?
K4 K8 K32 105.5(19) 3_445 2_544 ?
Cs3 K8 K32 36.6(12) 2_544 2_544 ?
K33 K8 K32 16.0(10) 2_544 2_544 ?
S21 K8 K32 134.5(16) 4_444 2_544 ?
S22 K8 K32 133.1(14) 4_444 2_544 ?
K31 K8 K32 7.7(6) 2_544 2_544 ?
S12 K8 K32 66.9(9) 6_556 2_544 ?
K7 K8 K32 59.7(7) . 2_544 ?
K32 K8 K32 93.7(10) 1_545 2_544 ?
K31 K8 K32 79.2(9) 1_545 2_544 ?