# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TSF3_Mo6Br14_Br_25K
_database_code_depnum_ccdc_archive 'CCDC 999363'
_audit_update_record             
;
2014-04-25 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            
; 
(TSF)3[(Mo6Br14)Br] 
;
_chemical_melting_point          ?
_chemical_formula_moiety         '(C6 Se4 H4 +)3, Mo6 Br14 2-, Br -'
_chemical_formula_sum            'C18 H12 Br15 Mo6 Se12'
_chemical_formula_weight         2950.09

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_H-M   R-3
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'

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                   17.2701(18)
_cell_length_b                   17.2701(18)
_cell_length_c                   14.6308(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3779.1(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    25(2)
_cell_measurement_reflns_used    5396
_cell_measurement_theta_min      3.8641
_cell_measurement_theta_max      30.2806

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3915
_exptl_absorpt_coefficient_mu    22.032
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.3894
_exptl_absorpt_correction_T_min  0.2451
_exptl_absorpt_process_details   
;
Higashi, T. (2000). 
A numerical absorption correction program NUMABS
Rigaku Corporation, Tokyo, Japan
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      25(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Mercury (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 14.7059
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13558
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.86
_diffrn_reflns_theta_max         27.50
_reflns_number_total             1931
_reflns_number_gt                1777
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0288P)²+34.1916P] where P=(Fo²+2Fc²)/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         1931
_refine_ls_number_parameters     78
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0691
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_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
C1 C 0.3641(3) 0.2115(3) 0.1669(4) 0.0121(10) Uani 1 1 d . . .
C2 C 0.5133(4) 0.3736(4) 0.1915(4) 0.0164(11) Uani 1 1 d . . .
H2 H 0.5738 0.4230 0.2099 0.020 Uiso 1 1 calc R . .
C3 C 0.4603(4) 0.3907(4) 0.1380(4) 0.0147(11) Uani 1 1 d . . .
H3 H 0.4811 0.4528 0.1157 0.018 Uiso 1 1 calc R . .
Se1 Se 0.47241(3) 0.25628(3) 0.23100(3) 0.01214(14) Uani 1 1 d . . .
Se2 Se 0.34666(3) 0.29655(3) 0.10565(3) 0.01159(13) Uani 1 1 d . . .
Br1 Br -0.00273(3) 0.17281(3) 0.42764(3) 0.00973(13) Uani 1 1 d . . .
Br2 Br 0.0000 0.0000 0.28203(5) 0.00917(18) Uani 1 3 d S . .
Br3 Br 0.20877(3) 0.21329(3) 0.32408(3) 0.01142(13) Uani 1 1 d . . .
Mo1 Mo 0.08737(3) 0.08890(3) 0.42639(3) 0.00819(12) Uani 1 1 d . . .
Br4 Br 0.0000 0.0000 0.0000 0.0117(2) Uani 1 6 d S . .

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
C1 0.009(2) 0.012(3) 0.016(3) 0.001(2) 0.002(2) 0.005(2)
C2 0.012(2) 0.013(3) 0.020(3) -0.002(2) -0.001(2) 0.003(2)
C3 0.017(3) 0.015(3) 0.011(3) -0.001(2) 0.004(2) 0.007(2)
Se1 0.0110(3) 0.0123(3) 0.0129(3) 0.00077(19) -0.00120(19) 0.0057(2)
Se2 0.0107(3) 0.0118(3) 0.0123(3) 0.00111(19) 0.00015(19) 0.0056(2)
Br1 0.0118(3) 0.0100(2) 0.0080(3) 0.00042(17) 0.00000(17) 0.0059(2)
Br2 0.0102(3) 0.0102(3) 0.0071(4) 0.000 0.000 0.00510(13)
Br3 0.0108(2) 0.0118(3) 0.0098(3) 0.00058(18) 0.00084(18) 0.0042(2)
Mo1 0.0086(2) 0.0088(2) 0.0067(2) 0.00039(15) 0.00035(15) 0.00402(17)
Br4 0.0107(4) 0.0107(4) 0.0138(6) 0.000 0.000 0.00533(18)

_geom_special_details            
; 
  The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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
C1 C1 1.372(10) 13 ?
C1 Se2 1.869(5) . ?
C1 Se1 1.878(5) . ?
C2 C3 1.345(8) . ?
C2 Se1 1.873(5) . ?
C2 H2 1.0000 . ?
C3 Se2 1.878(5) . ?
C3 H3 1.0000 . ?
Br1 Mo1 2.6017(6) 12_556 ?
Br1 Mo1 2.6031(7) . ?
Br1 Mo1 2.6075(7) 2 ?
Br2 Mo1 2.6036(8) 3 ?
Br2 Mo1 2.6036(8) 2 ?
Br2 Mo1 2.6036(8) . ?
Br3 Mo1 2.5975(7) . ?
Mo1 Br1 2.6018(7) 11_556 ?
Mo1 Br1 2.6074(7) 3 ?
Mo1 Mo1 2.6367(8) 3 ?
Mo1 Mo1 2.6368(8) 2 ?
Mo1 Mo1 2.6376(7) 12_556 ?
Mo1 Mo1 2.6376(7) 11_556 ?

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
C1 C1 Se2 123.1(5) 13 . ?
C1 C1 Se1 121.2(5) 13 . ?
Se2 C1 Se1 115.8(3) . . ?
C3 C2 Se1 119.1(4) . . ?
C3 C2 H2 120.4 . . ?
Se1 C2 H2 120.4 . . ?
C2 C3 Se2 119.2(4) . . ?
C2 C3 H3 120.4 . . ?
Se2 C3 H3 120.4 . . ?
C2 Se1 C1 92.9(2) . . ?
C1 Se2 C3 92.9(2) . . ?
Mo1 Br1 Mo1 60.896(19) 12_556 . ?
Mo1 Br1 Mo1 60.838(19) 12_556 2 ?
Mo1 Br1 Mo1 60.80(2) . 2 ?
Mo1 Br2 Mo1 60.84(2) 3 2 ?
Mo1 Br2 Mo1 60.84(2) 3 . ?
Mo1 Br2 Mo1 60.84(2) 2 . ?
Br3 Mo1 Br1 90.36(2) . 11_556 ?
Br3 Mo1 Br1 90.20(2) . . ?
Br1 Mo1 Br1 89.948(16) 11_556 . ?
Br3 Mo1 Br2 90.59(2) . . ?
Br1 Mo1 Br2 179.04(2) 11_556 . ?
Br1 Mo1 Br2 90.140(16) . . ?
Br3 Mo1 Br1 90.91(2) . 3 ?
Br1 Mo1 Br1 89.852(16) 11_556 3 ?
Br1 Mo1 Br1 178.87(2) . 3 ?
Br2 Mo1 Br1 90.042(16) . 3 ?
Br3 Mo1 Mo1 135.26(2) . 3 ?
Br1 Mo1 Mo1 119.589(16) 11_556 3 ?
Br1 Mo1 Mo1 119.68(2) . 3 ?
Br2 Mo1 Mo1 59.578(12) . 3 ?
Br1 Mo1 Mo1 59.52(2) 3 3 ?
Br3 Mo1 Mo1 134.85(2) . 2 ?
Br1 Mo1 Mo1 119.699(16) 11_556 2 ?
Br1 Mo1 Mo1 59.68(2) . 2 ?
Br2 Mo1 Mo1 59.578(12) . 2 ?
Br1 Mo1 Mo1 119.52(2) 3 2 ?
Mo1 Mo1 Mo1 60.0 3 2 ?
Br3 Mo1 Mo1 134.74(2) . 12_556 ?
Br1 Mo1 Mo1 59.69(2) 11_556 12_556 ?
Br1 Mo1 Mo1 59.526(15) . 12_556 ?
Br2 Mo1 Mo1 119.586(17) . 12_556 ?
Br1 Mo1 Mo1 119.45(2) 3 12_556 ?
Mo1 Mo1 Mo1 90.0 3 12_556 ?
Mo1 Mo1 Mo1 60.009(11) 2 12_556 ?
Br3 Mo1 Mo1 135.15(2) . 11_556 ?
Br1 Mo1 Mo1 59.58(2) 11_556 11_556 ?
Br1 Mo1 Mo1 119.51(2) . 11_556 ?
Br2 Mo1 Mo1 119.587(17) . 11_556 ?
Br1 Mo1 Mo1 59.473(15) 3 11_556 ?
Mo1 Mo1 Mo1 60.010(11) 3 11_556 ?
Mo1 Mo1 Mo1 90.0 2 11_556 ?
Mo1 Mo1 Mo1 59.98(2) 12_556 11_556 ?

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
Se1 C2 C3 Se2 0.5(6) . . . . ?
C3 C2 Se1 C1 1.5(5) . . . . ?
C1 C1 Se1 C2 177.3(6) 13 . . . ?
Se2 C1 Se1 C2 -3.1(3) . . . . ?
C1 C1 Se2 C3 -177.1(6) 13 . . . ?
Se1 C1 Se2 C3 3.2(3) . . . . ?
C2 C3 Se2 C1 -2.3(5) . . . . ?
Mo1 Br1 Mo1 Br3 -144.56(2) 12_556 . . . ?
Mo1 Br1 Mo1 Br3 144.576(14) 2 . . . ?
Mo1 Br1 Mo1 Br1 -54.20(2) 12_556 . . 11_556 ?
Mo1 Br1 Mo1 Br1 -125.062(16) 2 . . 11_556 ?
Mo1 Br1 Mo1 Br2 124.851(18) 12_556 . . . ?
Mo1 Br1 Mo1 Br2 53.984(18) 2 . . . ?
Mo1 Br1 Mo1 Br1 25.6(13) 12_556 . . 3 ?
Mo1 Br1 Mo1 Br1 -45.2(13) 2 . . 3 ?
Mo1 Br1 Mo1 Mo1 70.403(13) 12_556 . . 3 ?
Mo1 Br1 Mo1 Mo1 -0.464(15) 2 . . 3 ?
Mo1 Br1 Mo1 Mo1 70.867(15) 12_556 . . 2 ?
Mo1 Br1 Mo1 Mo1 -70.867(15) 2 . . 12_556 ?
Mo1 Br1 Mo1 Mo1 0.19(2) 12_556 . . 11_556 ?
Mo1 Br1 Mo1 Mo1 -70.68(2) 2 . . 11_556 ?
Mo1 Br2 Mo1 Br3 144.85(2) 3 . . . ?
Mo1 Br2 Mo1 Br3 -144.27(2) 2 . . . ?
Mo1 Br2 Mo1 Br1 -29.7(13) 3 . . 11_556 ?
Mo1 Br2 Mo1 Br1 41.2(13) 2 . . 11_556 ?
Mo1 Br2 Mo1 Br1 -124.946(17) 3 . . . ?
Mo1 Br2 Mo1 Br1 -54.07(2) 2 . . . ?
Mo1 Br2 Mo1 Br1 53.94(2) 3 . . 3 ?
Mo1 Br2 Mo1 Br1 124.814(17) 2 . . 3 ?
Mo1 Br2 Mo1 Mo1 70.878(10) 2 . . 3 ?
Mo1 Br2 Mo1 Mo1 -70.878(10) 3 . . 2 ?
Mo1 Br2 Mo1 Mo1 -70.523(9) 3 . . 12_556 ?
Mo1 Br2 Mo1 Mo1 0.355(12) 2 . . 12_556 ?
Mo1 Br2 Mo1 Mo1 -0.354(12) 3 . . 11_556 ?
Mo1 Br2 Mo1 Mo1 70.524(9) 2 . . 11_556 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.530
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.271
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TSF3_Mo6Br14_Br_100K
_database_code_depnum_ccdc_archive 'CCDC 999364'
_audit_update_record             
;
2014-04-25 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            
; 
(TSF)3[(Mo6Br14)Br]
;
_chemical_formula_moiety         
;
(C6 H4 Se4 1+) 3,Br1 1-,Br14 Mo6 2-
;
_chemical_formula_sum            'C18 H12 Br15 Mo6 Se12'
_chemical_formula_weight         2950.09

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'
Se Se -0.0929 2.2259 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_Int_Tables_number      148

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

_cell_length_a                   11.0988(9)
_cell_length_b                   11.0988(9)
_cell_length_c                   11.0988(9)
_cell_angle_alpha                102.0577(4)
_cell_angle_beta                 102.0577(4)
_cell_angle_gamma                102.0577(4)
_cell_volume                     1261.12(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3486
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      28.12

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1305
_exptl_absorpt_coefficient_mu    22.007
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2589
_exptl_absorpt_correction_T_max  0.3830
_exptl_absorpt_process_details   
;
 APEX2 Software
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7072
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         27.45
_reflns_number_total             1903
_reflns_number_gt                1707
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 '
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0213P)²+1.4033P] where P=(Fo²+2Fc²)/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         1903
_refine_ls_number_parameters     78
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0203
_refine_ls_wR_factor_ref         0.0409
_refine_ls_wR_factor_gt          0.0395
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.001
_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
C1 C 0.5145(3) 0.4558(3) 0.0315(3) 0.0147(7) Uani 1 1 d . . .
C2 C 0.5517(4) 0.3177(4) 0.2035(4) 0.0213(8) Uani 1 1 d . . .
H2 H 0.5585 0.2863 0.2821 0.026 Uiso 1 1 calc R . .
C3 C 0.5688(3) 0.2484(4) 0.0982(4) 0.0196(8) Uani 1 1 d . . .
H3 H 0.5886 0.1644 0.0970 0.024 Uiso 1 1 calc R . .
Se1 Se 0.51501(4) 0.47456(3) 0.20300(3) 0.01796(9) Uani 1 1 d . . .
Se2 Se 0.55529(3) 0.30947(3) -0.04760(3) 0.01693(9) Uani 1 1 d . . .
Br1 Br -0.10309(3) 0.24499(3) 0.07423(3) 0.01361(8) Uani 1 1 d . . .
Br2 Br 0.21713(4) 0.21713(4) 0.21713(4) 0.01229(12) Uani 1 3 d S . .
Br3 Br -0.03353(3) 0.17135(3) 0.38805(3) 0.01661(9) Uani 1 1 d . . .
Mo1 Mo -0.01414(3) 0.07207(3) 0.16205(3) 0.01035(7) Uani 1 1 d . . .
Br4 Br 0.5000 0.5000 0.5000 0.01580(17) Uani 1 6 d S . .

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
C1 0.0129(17) 0.0142(17) 0.0145(17) 0.0019(13) 0.0043(13) -0.0006(13)
C2 0.023(2) 0.0197(19) 0.025(2) 0.0129(16) 0.0052(16) 0.0059(15)
C3 0.0182(18) 0.0220(19) 0.0195(19) 0.0097(15) 0.0043(15) 0.0035(15)
Se1 0.02232(19) 0.01913(19) 0.01505(18) 0.00556(14) 0.00747(14) 0.00744(15)
Se2 0.01985(19) 0.01467(18) 0.01803(18) 0.00436(14) 0.00786(14) 0.00536(14)
Br1 0.01338(17) 0.01106(16) 0.01529(17) 0.00131(13) 0.00277(13) 0.00406(12)
Br2 0.01139(13) 0.01139(13) 0.01139(13) 0.00109(15) 0.00109(15) 0.00109(15)
Br3 0.01709(18) 0.01718(18) 0.01348(17) 0.00006(13) 0.00580(13) 0.00228(14)
Mo1 0.00999(14) 0.01030(14) 0.00961(14) 0.00139(10) 0.00231(10) 0.00175(11)
Br4 0.0171(2) 0.0171(2) 0.0171(2) 0.0073(2) 0.0073(2) 0.0073(2)

_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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
C1 C1 1.370(7) 4_665 ?
C1 Se2 1.868(4) . ?
C1 Se1 1.870(3) . ?
C2 C3 1.331(5) . ?
C2 Se1 1.870(4) . ?
C2 H2 1.0000 . ?
C3 Se2 1.871(4) . ?
C3 H3 1.0000 . ?
Br1 Mo1 2.5975(5) 5 ?
Br1 Mo1 2.5992(5) 3 ?
Br1 Mo1 2.6037(5) . ?
Br2 Mo1 2.6002(6) 2 ?
Br2 Mo1 2.6002(6) . ?
Br2 Mo1 2.6002(6) 3 ?
Br3 Mo1 2.5927(5) . ?
Mo1 Br1 2.5974(5) 6 ?
Mo1 Br1 2.5992(5) 2 ?
Mo1 Mo1 2.6335(5) 2 ?
Mo1 Mo1 2.6336(5) 3 ?
Mo1 Mo1 2.6342(5) 6 ?
Mo1 Mo1 2.6343(5) 5 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C1 Se2 122.6(4) 4_665 . ?
C1 C1 Se1 121.7(4) 4_665 . ?
Se2 C1 Se1 115.76(18) . . ?
C3 C2 Se1 119.3(3) . . ?
C3 C2 H2 120.3 . . ?
Se1 C2 H2 120.3 . . ?
C2 C3 Se2 119.4(3) . . ?
C2 C3 H3 120.3 . . ?
Se2 C3 H3 120.3 . . ?
C2 Se1 C1 92.71(16) . . ?
C1 Se2 C3 92.67(16) . . ?
Mo1 Br1 Mo1 60.916(13) 5 3 ?
Mo1 Br1 Mo1 60.859(13) 5 . ?
Mo1 Br1 Mo1 60.819(14) 3 . ?
Mo1 Br2 Mo1 60.850(15) 2 . ?
Mo1 Br2 Mo1 60.850(15) 2 3 ?
Mo1 Br2 Mo1 60.851(15) . 3 ?
Br3 Mo1 Br1 90.408(13) . 6 ?
Br3 Mo1 Br1 90.196(14) . 2 ?
Br1 Mo1 Br1 89.941(11) 6 2 ?
Br3 Mo1 Br2 90.556(13) . . ?
Br1 Mo1 Br2 179.032(16) 6 . ?
Br1 Mo1 Br2 90.147(11) 2 . ?
Br3 Mo1 Br1 90.952(14) . . ?
Br1 Mo1 Br1 89.845(11) 6 . ?
Br1 Mo1 Br1 178.834(16) 2 . ?
Br2 Mo1 Br1 90.048(11) . . ?
Br3 Mo1 Mo1 134.805(14) . 2 ?
Br1 Mo1 Mo1 119.695(11) 6 2 ?
Br1 Mo1 Mo1 59.676(14) 2 2 ?
Br2 Mo1 Mo1 59.574(8) . 2 ?
Br1 Mo1 Mo1 119.505(14) . 2 ?
Br3 Mo1 Mo1 135.243(14) . 3 ?
Br1 Mo1 Mo1 119.583(11) 6 3 ?
Br1 Mo1 Mo1 119.674(14) 2 3 ?
Br2 Mo1 Mo1 59.575(8) . 3 ?
Br1 Mo1 Mo1 59.507(14) . 3 ?
Mo1 Mo1 Mo1 60.0 2 3 ?
Br3 Mo1 Mo1 134.756(14) . 6 ?
Br1 Mo1 Mo1 59.685(13) 6 6 ?
Br1 Mo1 Mo1 59.509(10) 2 6 ?
Br2 Mo1 Mo1 119.584(10) . 6 ?
Br1 Mo1 Mo1 119.435(14) . 6 ?
Mo1 Mo1 Mo1 60.011(7) 2 6 ?
Mo1 Mo1 Mo1 90.0 3 6 ?
Br3 Mo1 Mo1 135.194(14) . 5 ?
Br1 Mo1 Mo1 59.575(13) 6 5 ?
Br1 Mo1 Mo1 119.491(14) 2 5 ?
Br2 Mo1 Mo1 119.582(10) . 5 ?
Br1 Mo1 Mo1 59.454(10) . 5 ?
Mo1 Mo1 Mo1 90.000(1) 2 5 ?
Mo1 Mo1 Mo1 60.008(7) 3 5 ?
Mo1 Mo1 Mo1 59.982(14) 6 5 ?

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
Se1 C2 C3 Se2 -0.1(4) . . . . ?
C3 C2 Se1 C1 1.8(3) . . . . ?
C1 C1 Se1 C2 176.9(4) 4_665 . . . ?
Se2 C1 Se1 C2 -2.9(2) . . . . ?
C1 C1 Se2 C3 -176.9(4) 4_665 . . . ?
Se1 C1 Se2 C3 2.9(2) . . . . ?
C2 C3 Se2 C1 -1.7(3) . . . . ?
Mo1 Br2 Mo1 Br3 144.251(18) 2 . . . ?
Mo1 Br2 Mo1 Br3 -144.869(18) 3 . . . ?
Mo1 Br2 Mo1 Br1 -41.2(9) 2 . . 6 ?
Mo1 Br2 Mo1 Br1 29.7(9) 3 . . 6 ?
Mo1 Br2 Mo1 Br1 54.053(14) 2 . . 2 ?
Mo1 Br2 Mo1 Br1 124.933(12) 3 . . 2 ?
Mo1 Br2 Mo1 Br1 -124.797(12) 2 . . . ?
Mo1 Br2 Mo1 Br1 -53.917(14) 3 . . . ?
Mo1 Br2 Mo1 Mo1 70.880(6) 3 . . 2 ?
Mo1 Br2 Mo1 Mo1 -70.880(6) 2 . . 3 ?
Mo1 Br2 Mo1 Mo1 -0.355(8) 2 . . 6 ?
Mo1 Br2 Mo1 Mo1 70.525(6) 3 . . 6 ?
Mo1 Br2 Mo1 Mo1 -70.525(6) 2 . . 5 ?
Mo1 Br2 Mo1 Mo1 0.355(8) 3 . . 5 ?
Mo1 Br1 Mo1 Br3 -144.503(14) 5 . . . ?
Mo1 Br1 Mo1 Br3 144.529(9) 3 . . . ?
Mo1 Br1 Mo1 Br1 -54.097(14) 5 . . 6 ?
Mo1 Br1 Mo1 Br1 -125.066(11) 3 . . 6 ?
Mo1 Br1 Mo1 Br1 25.3(8) 5 . . 2 ?
Mo1 Br1 Mo1 Br1 -45.6(8) 3 . . 2 ?
Mo1 Br1 Mo1 Br2 124.941(11) 5 . . . ?
Mo1 Br1 Mo1 Br2 53.972(12) 3 . . . ?
Mo1 Br1 Mo1 Mo1 70.491(9) 5 . . 2 ?
Mo1 Br1 Mo1 Mo1 -0.478(10) 3 . . 2 ?
Mo1 Br1 Mo1 Mo1 70.969(10) 5 . . 3 ?
Mo1 Br1 Mo1 Mo1 0.375(16) 5 . . 6 ?
Mo1 Br1 Mo1 Mo1 -70.593(14) 3 . . 6 ?
Mo1 Br1 Mo1 Mo1 -70.969(10) 3 . . 5 ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.116
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TSF3_Mo6Br14_Br_298K
_database_code_depnum_ccdc_archive 'CCDC 999365'
_audit_update_record             
;
2014-04-25 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            
; 
(TSF)3[(Mo6Br14)Br]
;
_chemical_formula_moiety         
;
3(C6 H4 Se4 1+),Br1 1-,Br14 Mo6 2-
;
_chemical_formula_sum            'C18 H12 Br15 Mo6 Se12'
_chemical_formula_weight         2950.09

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'
Se Se -0.0929 2.2259 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_Int_Tables_number      148

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

_cell_length_a                   11.1579(5)
_cell_length_b                   11.1579(5)
_cell_length_c                   11.1579(5)
_cell_angle_alpha                101.8000(10)
_cell_angle_beta                 101.8000(10)
_cell_angle_gamma                101.8000(10)
_cell_volume                     1286.32(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2726
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      28.21

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.808
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1305
_exptl_absorpt_coefficient_mu    21.576
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2682
_exptl_absorpt_correction_T_max  0.3887
_exptl_absorpt_process_details   
;
 APEX2 Software
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7248
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1939
_reflns_number_gt                1594
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 '
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0213P)²+1.4033P] where P=(Fo²+2Fc²)/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         1939
_refine_ls_number_parameters     78
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0488
_refine_ls_wR_factor_gt          0.0454
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
C1 C 0.5144(4) 0.4554(4) 0.0312(4) 0.0330(10) Uani 1 1 d . . .
C2 C 0.5518(5) 0.3191(5) 0.2019(5) 0.0472(13) Uani 1 1 d . . .
H2 H 0.5591 0.2878 0.2803 0.057 Uiso 1 1 calc R . .
C3 C 0.5685(5) 0.2503(5) 0.0979(5) 0.0450(12) Uani 1 1 d . . .
H3 H 0.5885 0.1668 0.0972 0.054 Uiso 1 1 calc R . .
Se1 Se 0.51479(5) 0.47407(5) 0.20146(5) 0.04403(14) Uani 1 1 d . . .
Se2 Se 0.55455(5) 0.31041(5) -0.04693(5) 0.04150(13) Uani 1 1 d . . .
Br1 Br -0.10255(4) 0.24459(4) 0.07170(4) 0.03236(11) Uani 1 1 d . . .
Br2 Br 0.21449(4) 0.21449(4) 0.21449(4) 0.02890(16) Uani 1 3 d S . .
Br3 Br -0.03563(5) 0.17134(5) 0.38444(4) 0.04034(13) Uani 1 1 d . . .
Mo1 Mo -0.01515(3) 0.07208(3) 0.16049(3) 0.02380(9) Uani 1 1 d . . .
Br4 Br 0.5000 0.5000 0.5000 0.0384(3) Uani 1 6 d S . .

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
C1 0.026(2) 0.038(3) 0.035(2) 0.0077(19) 0.0120(19) 0.0041(19)
C2 0.050(3) 0.049(3) 0.048(3) 0.024(3) 0.012(3) 0.014(2)
C3 0.049(3) 0.041(3) 0.051(3) 0.020(2) 0.013(2) 0.016(2)
Se1 0.0560(3) 0.0468(3) 0.0357(3) 0.0128(2) 0.0183(2) 0.0184(2)
Se2 0.0496(3) 0.0359(3) 0.0441(3) 0.0101(2) 0.0202(2) 0.0142(2)
Br1 0.0323(2) 0.0256(2) 0.0367(2) 0.00240(18) 0.00627(19) 0.01031(18)
Br2 0.02670(17) 0.02670(17) 0.02670(17) 0.0021(2) 0.0021(2) 0.0021(2)
Br3 0.0430(3) 0.0411(3) 0.0318(3) -0.0015(2) 0.0155(2) 0.0048(2)
Mo1 0.02346(19) 0.02373(18) 0.02179(18) 0.00309(13) 0.00538(14) 0.00395(14)
Br4 0.0420(3) 0.0420(3) 0.0420(3) 0.0186(4) 0.0186(4) 0.0186(4)

_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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
C1 C1 1.378(9) 4_665 ?
C1 Se2 1.860(5) . ?
C1 Se1 1.867(4) . ?
C2 C3 1.324(7) . ?
C2 Se1 1.859(5) . ?
C2 H2 1.0000 . ?
C3 Se2 1.862(5) . ?
C3 H3 1.0000 . ?
Br1 Mo1 2.6008(5) 5 ?
Br1 Mo1 2.6008(6) 3 ?
Br1 Mo1 2.6058(6) . ?
Br2 Mo1 2.6010(6) 3 ?
Br2 Mo1 2.6010(6) . ?
Br2 Mo1 2.6010(6) 2 ?
Br3 Mo1 2.5938(6) . ?
Mo1 Br1 2.6008(5) 6 ?
Mo1 Br1 2.6008(6) 2 ?
Mo1 Mo1 2.6343(6) 3 ?
Mo1 Mo1 2.6343(6) 2 ?
Mo1 Mo1 2.6364(6) 5 ?
Mo1 Mo1 2.6364(6) 6 ?

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
C1 C1 Se2 122.8(5) 4_665 . ?
C1 C1 Se1 121.3(5) 4_665 . ?
Se2 C1 Se1 115.9(2) . . ?
C3 C2 Se1 119.6(4) . . ?
C3 C2 H2 120.2 . . ?
Se1 C2 H2 120.2 . . ?
C2 C3 Se2 119.4(4) . . ?
C2 C3 H3 120.3 . . ?
Se2 C3 H3 120.3 . . ?
C2 Se1 C1 92.4(2) . . ?
C1 Se2 C3 92.5(2) . . ?
Mo1 Br1 Mo1 60.908(16) 5 3 ?
Mo1 Br1 Mo1 60.843(17) 5 . ?
Mo1 Br1 Mo1 60.789(18) 3 . ?
Mo1 Br2 Mo1 60.850(19) 3 . ?
Mo1 Br2 Mo1 60.849(19) 3 2 ?
Mo1 Br2 Mo1 60.850(19) . 2 ?
Br3 Mo1 Br1 90.496(18) . 6 ?
Br3 Mo1 Br1 90.112(19) . 2 ?
Br1 Mo1 Br1 89.950(14) 6 2 ?
Br3 Mo1 Br2 90.474(17) . . ?
Br1 Mo1 Br2 179.02(2) 6 . ?
Br1 Mo1 Br2 90.150(14) 2 . ?
Br3 Mo1 Br1 90.996(19) . . ?
Br1 Mo1 Br1 89.843(14) 6 . ?
Br1 Mo1 Br1 178.87(2) 2 . ?
Br2 Mo1 Br1 90.039(14) . . ?
Br3 Mo1 Mo1 135.225(18) . 3 ?
Br1 Mo1 Mo1 119.572(14) 6 3 ?
Br1 Mo1 Mo1 119.697(18) 2 3 ?
Br2 Mo1 Mo1 59.575(9) . 3 ?
Br1 Mo1 Mo1 59.513(18) . 3 ?
Br3 Mo1 Mo1 134.708(18) . 2 ?
Br1 Mo1 Mo1 119.695(15) 6 2 ?
Br1 Mo1 Mo1 59.700(18) 2 2 ?
Br2 Mo1 Mo1 59.576(9) . 2 ?
Br1 Mo1 Mo1 119.510(18) . 2 ?
Mo1 Mo1 Mo1 60.0 3 2 ?
Br3 Mo1 Mo1 135.290(18) . 5 ?
Br1 Mo1 Mo1 59.545(17) 6 5 ?
Br1 Mo1 Mo1 119.495(17) 2 5 ?
Br2 Mo1 Mo1 119.601(13) . 5 ?
Br1 Mo1 Mo1 59.485(13) . 5 ?
Mo1 Mo1 Mo1 60.027(8) 3 5 ?
Mo1 Mo1 Mo1 90.0 2 5 ?
Br3 Mo1 Mo1 134.775(18) . 6 ?
Br1 Mo1 Mo1 59.671(17) 6 6 ?
Br1 Mo1 Mo1 59.547(13) 2 6 ?
Br2 Mo1 Mo1 119.600(13) . 6 ?
Br1 Mo1 Mo1 119.432(17) . 6 ?
Mo1 Mo1 Mo1 90.0 3 6 ?
Mo1 Mo1 Mo1 60.025(8) 2 6 ?
Mo1 Mo1 Mo1 59.948(17) 5 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
Se1 C2 C3 Se2 0.0(6) . . . . ?
C3 C2 Se1 C1 1.6(5) . . . . ?
C1 C1 Se1 C2 177.2(5) 4_665 . . . ?
Se2 C1 Se1 C2 -2.6(3) . . . . ?
C1 C1 Se2 C3 -177.2(5) 4_665 . . . ?
Se1 C1 Se2 C3 2.6(3) . . . . ?
C2 C3 Se2 C1 -1.6(5) . . . . ?
Mo1 Br2 Mo1 Br3 -144.93(2) 3 . . . ?
Mo1 Br2 Mo1 Br3 144.19(2) 2 . . . ?
Mo1 Br2 Mo1 Br1 29.1(11) 3 . . 6 ?
Mo1 Br2 Mo1 Br1 -41.8(11) 2 . . 6 ?
Mo1 Br2 Mo1 Br1 124.959(16) 3 . . 2 ?
Mo1 Br2 Mo1 Br1 54.081(18) 2 . . 2 ?
Mo1 Br2 Mo1 Br1 -53.930(18) 3 . . . ?
Mo1 Br2 Mo1 Br1 -124.809(15) 2 . . . ?
Mo1 Br2 Mo1 Mo1 -70.878(8) 2 . . 3 ?
Mo1 Br2 Mo1 Mo1 70.878(8) 3 . . 2 ?
Mo1 Br2 Mo1 Mo1 0.366(10) 3 . . 5 ?
Mo1 Br2 Mo1 Mo1 -70.512(7) 2 . . 5 ?
Mo1 Br2 Mo1 Mo1 70.509(7) 3 . . 6 ?
Mo1 Br2 Mo1 Mo1 -0.369(10) 2 . . 6 ?
Mo1 Br1 Mo1 Br3 -144.568(18) 5 . . . ?
Mo1 Br1 Mo1 Br3 144.455(13) 3 . . . ?
Mo1 Br1 Mo1 Br1 -54.074(18) 5 . . 6 ?
Mo1 Br1 Mo1 Br1 -125.052(15) 3 . . 6 ?
Mo1 Br1 Mo1 Br1 25.3(11) 5 . . 2 ?
Mo1 Br1 Mo1 Br1 -45.7(11) 3 . . 2 ?
Mo1 Br1 Mo1 Br2 124.957(14) 5 . . . ?
Mo1 Br1 Mo1 Br2 53.980(15) 3 . . . ?
Mo1 Br1 Mo1 Mo1 70.977(13) 5 . . 3 ?
Mo1 Br1 Mo1 Mo1 70.514(12) 5 . . 2 ?
Mo1 Br1 Mo1 Mo1 -0.464(13) 3 . . 2 ?
Mo1 Br1 Mo1 Mo1 -70.977(13) 3 . . 5 ?
Mo1 Br1 Mo1 Mo1 0.38(2) 5 . . 6 ?
Mo1 Br1 Mo1 Mo1 -70.597(18) 3 . . 6 ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.107
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TSF3_Mo6Cl14_Cl_25K
_database_code_depnum_ccdc_archive 'CCDC 999366'
_audit_update_record             
;
2014-04-25 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            
; 
(TSF)3[(Mo6Cl14)Cl] 
;
_chemical_melting_point          ?
_chemical_formula_moiety         '(C6 Se4 H4 +)3, Mo6 Cl14 2-, Cl -'
_chemical_formula_sum            'C18 H12 Cl15 Mo6 Se12'
_chemical_formula_weight         2283.19

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   R-3
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'

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                   16.9464(13)
_cell_length_b                   16.9464(13)
_cell_length_c                   14.0495(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3494.2(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    25(2)
_cell_measurement_reflns_used    5847
_cell_measurement_theta_min      3.9493
_cell_measurement_theta_max      30.1912

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3105
_exptl_absorpt_coefficient_mu    11.823
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.4853
_exptl_absorpt_correction_T_min  0.2585
_exptl_absorpt_process_details   
;
Higashi, T. (2000). 
A numerical absorption correction program NUMABS
Rigaku Corporation, Tokyo, Japan
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      25(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Mercury (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 14.7059
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12352
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.95
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1779
_reflns_number_gt                1588
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0095P)²+0.0000P] where P=(Fo²+2Fc²)/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         1779
_refine_ls_number_parameters     78
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0168
_refine_ls_R_factor_gt           0.0151
_refine_ls_wR_factor_ref         0.0325
_refine_ls_wR_factor_gt          0.0322
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_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
C1 C 0.30196(15) 0.18153(15) 0.16686(15) 0.0071(5) Uani 1 1 d . . .
C2 C 0.20668(15) 0.26745(15) 0.19962(16) 0.0086(5) Uani 1 1 d . . .
H2 H 0.1866 0.3104 0.2229 0.010 Uiso 1 1 calc R . .
C3 C 0.15089(15) 0.19570(15) 0.14654(16) 0.0091(5) Uani 1 1 d . . .
H3 H 0.0885 0.1840 0.1303 0.011 Uiso 1 1 calc R . .
Se1 Se 0.322704(15) 0.287263(15) 0.230230(16) 0.00665(6) Uani 1 1 d . . .
Se2 Se 0.190676(15) 0.117197(15) 0.102880(16) 0.00666(6) Uani 1 1 d . . .
Cl1 Cl 0.16908(4) 0.16845(4) 0.42836(4) 0.00651(12) Uani 1 1 d . . .
Cl2 Cl 0.0000 0.0000 0.28442(6) 0.00578(19) Uani 1 3 d S . .
Cl3 Cl 0.20607(4) -0.00203(4) 0.32587(4) 0.00777(12) Uani 1 1 d . . .
Mo1 Mo 0.088685(13) -0.000443(12) 0.424219(13) 0.00424(6) Uani 1 1 d . . .
Cl4 Cl 0.0000 0.0000 0.0000 0.0075(3) Uani 1 6 d S . .

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
C1 0.0074(11) 0.0066(11) 0.0041(12) 0.0005(9) 0.0009(9) 0.0011(9)
C2 0.0066(12) 0.0110(12) 0.0099(12) 0.0018(9) 0.0028(9) 0.0057(10)
C3 0.0103(12) 0.0118(12) 0.0076(12) 0.0026(9) 0.0008(9) 0.0074(10)
Se1 0.00612(12) 0.00650(12) 0.00700(13) -0.00130(9) -0.00030(9) 0.00291(10)
Se2 0.00605(12) 0.00654(12) 0.00691(12) -0.00105(9) -0.00099(9) 0.00278(10)
Cl1 0.0066(3) 0.0065(3) 0.0054(3) 0.0008(2) 0.0004(2) 0.0024(2)
Cl2 0.0068(3) 0.0068(3) 0.0038(5) 0.000 0.000 0.00338(14)
Cl3 0.0075(3) 0.0107(3) 0.0061(3) 0.0004(2) 0.0013(2) 0.0053(2)
Mo1 0.00491(10) 0.00515(10) 0.00277(11) 0.00004(7) 0.00024(7) 0.00260(8)
Cl4 0.0070(4) 0.0070(4) 0.0085(7) 0.000 0.000 0.0035(2)

_geom_special_details            
; 
  The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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
C1 C1 1.386(4) 13 ?
C1 Se1 1.870(2) . ?
C1 Se2 1.870(2) . ?
C2 C3 1.334(3) . ?
C2 Se1 1.872(2) . ?
C2 H2 1.0000 . ?
C3 Se2 1.870(2) . ?
C3 H3 1.0000 . ?
Cl1 Mo1 2.4741(6) 12_556 ?
Cl1 Mo1 2.4771(6) 2 ?
Cl1 Mo1 2.4803(6) . ?
Cl2 Mo1 2.4754(7) 3 ?
Cl2 Mo1 2.4754(7) 2 ?
Cl2 Mo1 2.4755(7) . ?
Cl3 Mo1 2.4332(6) . ?
Mo1 Cl1 2.4742(6) 11_556 ?
Mo1 Cl1 2.4771(6) 3 ?
Mo1 Mo1 2.6085(4) 11_556 ?
Mo1 Mo1 2.6085(4) 12_556 ?
Mo1 Mo1 2.6096(4) 3 ?
Mo1 Mo1 2.6096(4) 2 ?

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
C1 C1 Se1 122.6(2) 13 . ?
C1 C1 Se2 121.3(2) 13 . ?
Se1 C1 Se2 116.05(12) . . ?
C3 C2 Se1 119.62(17) . . ?
C3 C2 H2 120.2 . . ?
Se1 C2 H2 120.2 . . ?
C2 C3 Se2 119.24(17) . . ?
C2 C3 H3 120.4 . . ?
Se2 C3 H3 120.4 . . ?
C1 Se1 C2 92.37(10) . . ?
C1 Se2 C3 92.57(10) . . ?
Mo1 Cl1 Mo1 63.585(15) 12_556 2 ?
Mo1 Cl1 Mo1 63.540(15) 12_556 . ?
Mo1 Cl1 Mo1 63.527(15) 2 . ?
Mo1 Cl2 Mo1 63.62(2) 3 2 ?
Mo1 Cl2 Mo1 63.62(2) 3 . ?
Mo1 Cl2 Mo1 63.62(2) 2 . ?
Cl3 Mo1 Cl1 91.443(19) . 11_556 ?
Cl3 Mo1 Cl2 92.89(2) . . ?
Cl1 Mo1 Cl2 175.671(19) 11_556 . ?
Cl3 Mo1 Cl1 91.830(19) . 3 ?
Cl1 Mo1 Cl1 89.879(13) 11_556 3 ?
Cl2 Mo1 Cl1 90.025(13) . 3 ?
Cl3 Mo1 Cl1 92.616(19) . . ?
Cl1 Mo1 Cl1 89.807(13) 11_556 . ?
Cl2 Mo1 Cl1 89.953(13) . . ?
Cl1 Mo1 Cl1 175.549(19) 3 . ?
Cl3 Mo1 Mo1 134.290(15) . 11_556 ?
Cl1 Mo1 Mo1 58.346(15) 11_556 11_556 ?
Cl2 Mo1 Mo1 118.160(13) . 11_556 ?
Cl1 Mo1 Mo1 58.154(13) 3 11_556 ?
Cl1 Mo1 Mo1 118.126(14) . 11_556 ?
Cl3 Mo1 Mo1 134.773(15) . 12_556 ?
Cl1 Mo1 Mo1 58.266(15) 11_556 12_556 ?
Cl2 Mo1 Mo1 118.160(13) . 12_556 ?
Cl1 Mo1 Mo1 118.167(14) 3 12_556 ?
Cl1 Mo1 Mo1 58.115(13) . 12_556 ?
Mo1 Mo1 Mo1 60.027(11) 11_556 12_556 ?
Cl3 Mo1 Mo1 135.218(15) . 3 ?
Cl1 Mo1 Mo1 118.316(13) 11_556 3 ?
Cl2 Mo1 Mo1 58.190(11) . 3 ?
Cl1 Mo1 Mo1 58.297(14) 3 3 ?
Cl1 Mo1 Mo1 118.159(14) . 3 ?
Mo1 Mo1 Mo1 59.987(5) 11_556 3 ?
Mo1 Mo1 Mo1 90.0 12_556 3 ?
Cl3 Mo1 Mo1 135.709(15) . 2 ?
Cl1 Mo1 Mo1 118.238(13) 11_556 2 ?
Cl2 Mo1 Mo1 58.190(11) . 2 ?
Cl1 Mo1 Mo1 118.278(14) 3 2 ?
Cl1 Mo1 Mo1 58.178(14) . 2 ?
Mo1 Mo1 Mo1 90.0 11_556 2 ?
Mo1 Mo1 Mo1 59.986(5) 12_556 2 ?
Mo1 Mo1 Mo1 60.0 3 2 ?

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
Se1 C2 C3 Se2 -0.6(3) . . . . ?
C1 C1 Se1 C2 -176.5(3) 13 . . . ?
Se2 C1 Se1 C2 3.62(13) . . . . ?
C3 C2 Se1 C1 -1.8(2) . . . . ?
C1 C1 Se2 C3 176.3(3) 13 . . . ?
Se1 C1 Se2 C3 -3.86(13) . . . . ?
C2 C3 Se2 C1 2.7(2) . . . . ?
Mo1 Cl2 Mo1 Cl3 143.614(17) 3 . . . ?
Mo1 Cl2 Mo1 Cl3 -144.304(17) 2 . . . ?
Mo1 Cl2 Mo1 Cl1 -36.95(19) 3 . . 11_556 ?
Mo1 Cl2 Mo1 Cl1 35.13(19) 2 . . 11_556 ?
Mo1 Cl2 Mo1 Cl1 51.781(15) 3 . . 3 ?
Mo1 Cl2 Mo1 Cl1 123.863(14) 2 . . 3 ?
Mo1 Cl2 Mo1 Cl1 -123.768(14) 3 . . . ?
Mo1 Cl2 Mo1 Cl1 -51.686(15) 2 . . . ?
Mo1 Cl2 Mo1 Mo1 -1.475(9) 3 . . 11_556 ?
Mo1 Cl2 Mo1 Mo1 70.607(5) 2 . . 11_556 ?
Mo1 Cl2 Mo1 Mo1 -70.608(5) 3 . . 12_556 ?
Mo1 Cl2 Mo1 Mo1 1.475(9) 2 . . 12_556 ?
Mo1 Cl2 Mo1 Mo1 72.082(10) 2 . . 3 ?
Mo1 Cl2 Mo1 Mo1 -72.082(10) 3 . . 2 ?
Mo1 Cl1 Mo1 Cl3 -143.312(16) 12_556 . . . ?
Mo1 Cl1 Mo1 Cl3 144.583(15) 2 . . . ?
Mo1 Cl1 Mo1 Cl1 -51.876(19) 12_556 . . 11_556 ?
Mo1 Cl1 Mo1 Cl1 -123.982(17) 2 . . 11_556 ?
Mo1 Cl1 Mo1 Cl2 123.801(16) 12_556 . . . ?
Mo1 Cl1 Mo1 Cl2 51.696(16) 2 . . . ?
Mo1 Cl1 Mo1 Cl1 34.1(3) 12_556 . . 3 ?
Mo1 Cl1 Mo1 Cl1 -38.0(3) 2 . . 3 ?
Mo1 Cl1 Mo1 Mo1 1.478(16) 12_556 . . 11_556 ?
Mo1 Cl1 Mo1 Mo1 -70.627(14) 2 . . 11_556 ?
Mo1 Cl1 Mo1 Mo1 -72.105(11) 2 . . 12_556 ?
Mo1 Cl1 Mo1 Mo1 70.550(12) 12_556 . . 3 ?
Mo1 Cl1 Mo1 Mo1 -1.555(14) 2 . . 3 ?
Mo1 Cl1 Mo1 Mo1 72.105(11) 12_556 . . 2 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.125
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TSF3_Mo6Cl14_Cl_100K
_database_code_depnum_ccdc_archive 'CCDC 999367'
_audit_update_record             
;
2014-04-25 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            
; 
(TSF)3[(Mo6Cl14)Cl] 
;
_chemical_melting_point          ?
_chemical_formula_moiety         '(C6 Se4 H4 +)3, Mo6 Cl14 2-, Cl -'
_chemical_formula_sum            'C18 H12 Cl15 Mo6 Se12'
_chemical_formula_weight         2283.19

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   'R-3   '
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_Int_Tables_number      148

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

_cell_length_a                   10.8505(5)
_cell_length_b                   10.8505(5)
_cell_length_c                   10.8505(5)
_cell_angle_alpha                102.6318(2)
_cell_angle_beta                 102.6318(2)
_cell_angle_gamma                102.6318(2)
_cell_volume                     1167.76(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5073
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      28.10

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1035
_exptl_absorpt_coefficient_mu    11.792
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3354
_exptl_absorpt_correction_T_max  0.4677
_exptl_absorpt_process_details   
;
 APEX2 Software
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6491
_diffrn_reflns_av_R_equivalents  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0122
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         27.50
_reflns_number_total             1762
_reflns_number_gt                1688
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 '
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0133P)²+0.9427P] where P=(Fo²+2Fc²)/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         1762
_refine_ls_number_parameters     78
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0145
_refine_ls_R_factor_gt           0.0132
_refine_ls_wR_factor_ref         0.0299
_refine_ls_wR_factor_gt          0.0295
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_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
C1 C 0.51494(18) 0.45407(18) 0.03132(18) 0.0128(4) Uani 1 1 d . . .
C2 C 0.5498(2) 0.3088(2) 0.2022(2) 0.0175(4) Uani 1 1 d . . .
H2 H 0.5552 0.2747 0.2811 0.021 Uiso 1 1 calc R . .
C3 C 0.5679(2) 0.2397(2) 0.0937(2) 0.0169(4) Uani 1 1 d . . .
H3 H 0.5873 0.1533 0.0903 0.020 Uiso 1 1 calc R . .
Se1 Se 0.51429(2) 0.470351(19) 0.206033(19) 0.01454(5) Uani 1 1 d . . .
Se2 Se 0.55679(2) 0.305461(19) -0.052754(19) 0.01443(5) Uani 1 1 d . . .
Cl1 Cl 0.90257(4) 0.23985(4) 0.07152(4) 0.01274(9) Uani 1 1 d . . .
Cl2 Cl 1.21463(5) 0.21463(5) 0.21463(5) 0.01152(14) Uani 1 3 d S . .
Cl3 Cl 0.96744(5) 0.17223(5) 0.38114(4) 0.01492(9) Uani 1 1 d . . .
Mo1 Mo 0.986702(15) 0.075277(15) 0.164405(15) 0.00923(5) Uani 1 1 d . . .
Cl4 Cl 0.5000 0.5000 0.5000 0.0139(2) Uani 1 6 d S . .

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
C1 0.0119(9) 0.0140(9) 0.0123(9) 0.0024(7) 0.0054(7) 0.0025(7)
C2 0.0180(10) 0.0172(10) 0.0182(10) 0.0084(8) 0.0042(8) 0.0042(8)
C3 0.0179(10) 0.0151(10) 0.0198(10) 0.0088(8) 0.0053(8) 0.0047(8)
Se1 0.01767(10) 0.01593(10) 0.01182(10) 0.00448(7) 0.00582(7) 0.00601(7)
Se2 0.01805(10) 0.01290(10) 0.01437(10) 0.00411(7) 0.00716(7) 0.00550(7)
Cl1 0.0127(2) 0.0102(2) 0.0140(2) 0.00138(16) 0.00258(16) 0.00377(16)
Cl2 0.01052(16) 0.01052(16) 0.01052(16) 0.00093(19) 0.00093(19) 0.00093(19)
Cl3 0.0154(2) 0.0150(2) 0.0121(2) 0.00000(17) 0.00553(17) 0.00189(17)
Mo1 0.00895(8) 0.00904(8) 0.00828(8) 0.00113(6) 0.00188(6) 0.00148(6)
Cl4 0.0150(3) 0.0150(3) 0.0150(3) 0.0065(3) 0.0065(3) 0.0065(3)

_geom_special_details            
; 
  The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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
C1 C1 1.379(4) 4_665 ?
C1 Se1 1.8668(19) . ?
C1 Se2 1.8699(19) . ?
C2 C3 1.329(3) . ?
C2 Se1 1.869(2) . ?
C2 H2 1.0000 . ?
C3 Se2 1.870(2) . ?
C3 H3 1.0000 . ?
Cl1 Mo1 2.4714(5) 5_665 ?
Cl1 Mo1 2.4748(5) 3_654 ?
Cl1 Mo1 2.4770(5) . ?
Cl2 Mo1 2.4726(6) 3_654 ?
Cl2 Mo1 2.4727(6) . ?
Cl2 Mo1 2.4727(6) 2_645 ?
Cl3 Mo1 2.4310(5) . ?
Mo1 Cl1 2.4714(5) 6_656 ?
Mo1 Cl1 2.4748(5) 2_645 ?
Mo1 Mo1 2.6061(3) 5_665 ?
Mo1 Mo1 2.6061(3) 6_656 ?
Mo1 Mo1 2.6070(3) 3_654 ?
Mo1 Mo1 2.6070(3) 2_645 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C1 Se1 121.62(19) 4_665 . ?
C1 C1 Se2 122.50(19) 4_665 . ?
Se1 C1 Se2 115.88(10) . . ?
C3 C2 Se1 119.43(16) . . ?
C3 C2 H2 120.3 . . ?
Se1 C2 H2 120.3 . . ?
C2 C3 Se2 119.45(16) . . ?
C2 C3 H3 120.3 . . ?
Se2 C3 H3 120.3 . . ?
C1 Se1 C2 92.61(9) . . ?
C3 Se2 C1 92.51(9) . . ?
Mo1 Cl1 Mo1 63.592(12) 5_665 3_654 ?
Mo1 Cl1 Mo1 63.560(12) 5_665 . ?
Mo1 Cl1 Mo1 63.534(13) 3_654 . ?
Mo1 Cl2 Mo1 63.627(17) 3_654 . ?
Mo1 Cl2 Mo1 63.627(17) 3_654 2_645 ?
Mo1 Cl2 Mo1 63.628(17) . 2_645 ?
Cl3 Mo1 Cl1 91.534(15) . 6_656 ?
Cl3 Mo1 Cl2 92.809(15) . . ?
Cl1 Mo1 Cl2 175.657(16) 6_656 . ?
Cl3 Mo1 Cl1 91.871(16) . 2_645 ?
Cl1 Mo1 Cl1 89.863(11) 6_656 2_645 ?
Cl2 Mo1 Cl1 90.018(11) . 2_645 ?
Cl3 Mo1 Cl1 92.592(16) . . ?
Cl1 Mo1 Cl1 89.813(11) 6_656 . ?
Cl2 Mo1 Cl1 89.967(11) . . ?
Cl1 Mo1 Cl1 175.532(16) 2_645 . ?
Cl3 Mo1 Mo1 134.819(13) . 5_665 ?
Cl1 Mo1 Mo1 58.267(12) 6_656 5_665 ?
Cl2 Mo1 Mo1 118.159(10) . 5_665 ?
Cl1 Mo1 Mo1 118.148(12) 2_645 5_665 ?
Cl1 Mo1 Mo1 58.116(10) . 5_665 ?
Cl3 Mo1 Mo1 134.360(13) . 6_656 ?
Cl1 Mo1 Mo1 58.323(12) 6_656 6_656 ?
Cl2 Mo1 Mo1 118.159(10) . 6_656 ?
Cl1 Mo1 Mo1 58.140(10) 2_645 6_656 ?
Cl1 Mo1 Mo1 118.122(12) . 6_656 ?
Mo1 Mo1 Mo1 60.022(8) 5_665 6_656 ?
Cl3 Mo1 Mo1 135.639(13) . 3_654 ?
Cl1 Mo1 Mo1 118.243(11) 6_656 3_654 ?
Cl2 Mo1 Mo1 58.186(9) . 3_654 ?
Cl1 Mo1 Mo1 118.255(12) 2_645 3_654 ?
Cl1 Mo1 Mo1 58.192(12) . 3_654 ?
Mo1 Mo1 Mo1 59.990(4) 5_665 3_654 ?
Mo1 Mo1 Mo1 90.0 6_656 3_654 ?
Cl3 Mo1 Mo1 135.174(13) . 2_645 ?
Cl1 Mo1 Mo1 118.297(11) 6_656 2_645 ?
Cl2 Mo1 Mo1 58.187(9) . 2_645 ?
Cl1 Mo1 Mo1 58.274(12) 2_645 2_645 ?
Cl1 Mo1 Mo1 118.173(12) . 2_645 ?
Mo1 Mo1 Mo1 90.0 5_665 2_645 ?
Mo1 Mo1 Mo1 59.989(4) 6_656 2_645 ?
Mo1 Mo1 Mo1 60.0 3_654 2_645 ?

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
Se1 C2 C3 Se2 -0.2(2) . . . . ?
C1 C1 Se1 C2 176.0(2) 4_665 . . . ?
Se2 C1 Se1 C2 -3.38(11) . . . . ?
C3 C2 Se1 C1 2.20(18) . . . . ?
C2 C3 Se2 C1 -1.87(18) . . . . ?
C1 C1 Se2 C3 -176.1(2) 4_665 . . . ?
Se1 C1 Se2 C3 3.29(11) . . . . ?
Mo1 Cl2 Mo1 Cl3 -144.284(15) 3_654 . . . ?
Mo1 Cl2 Mo1 Cl3 143.630(15) 2_645 . . . ?
Mo1 Cl2 Mo1 Cl1 35.41(16) 3_654 . . 6_656 ?
Mo1 Cl2 Mo1 Cl1 -36.68(16) 2_645 . . 6_656 ?
Mo1 Cl2 Mo1 Cl1 123.841(12) 3_654 . . 2_645 ?
Mo1 Cl2 Mo1 Cl1 51.755(13) 2_645 . . 2_645 ?
Mo1 Cl2 Mo1 Cl1 -51.691(13) 3_654 . . . ?
Mo1 Cl2 Mo1 Cl1 -123.777(12) 2_645 . . . ?
Mo1 Cl2 Mo1 Mo1 1.480(8) 3_654 . . 5_665 ?
Mo1 Cl2 Mo1 Mo1 -70.606(3) 2_645 . . 5_665 ?
Mo1 Cl2 Mo1 Mo1 70.607(3) 3_654 . . 6_656 ?
Mo1 Cl2 Mo1 Mo1 -1.479(8) 2_645 . . 6_656 ?
Mo1 Cl2 Mo1 Mo1 -72.086(8) 2_645 . . 3_654 ?
Mo1 Cl2 Mo1 Mo1 72.086(8) 3_654 . . 2_645 ?
Mo1 Cl1 Mo1 Cl3 -143.400(14) 5_665 . . . ?
Mo1 Cl1 Mo1 Cl3 144.496(12) 3_654 . . . ?
Mo1 Cl1 Mo1 Cl1 -51.873(16) 5_665 . . 6_656 ?
Mo1 Cl1 Mo1 Cl1 -123.977(15) 3_654 . . 6_656 ?
Mo1 Cl1 Mo1 Cl2 123.789(13) 5_665 . . . ?
Mo1 Cl1 Mo1 Cl2 51.686(13) 3_654 . . . ?
Mo1 Cl1 Mo1 Cl1 34.0(2) 5_665 . . 2_645 ?
Mo1 Cl1 Mo1 Cl1 -38.1(2) 3_654 . . 2_645 ?
Mo1 Cl1 Mo1 Mo1 -72.104(9) 3_654 . . 5_665 ?
Mo1 Cl1 Mo1 Mo1 1.460(14) 5_665 . . 6_656 ?
Mo1 Cl1 Mo1 Mo1 -70.644(12) 3_654 . . 6_656 ?
Mo1 Cl1 Mo1 Mo1 72.104(9) 5_665 . . 3_654 ?
Mo1 Cl1 Mo1 Mo1 70.539(10) 5_665 . . 2_645 ?
Mo1 Cl1 Mo1 Mo1 -1.565(12) 3_654 . . 2_645 ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.073
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TSF3_Mo6Cl14_Cl_300K
_database_code_depnum_ccdc_archive 'CCDC 999368'
_audit_update_record             
;
2014-04-25 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            
; 
(TSF)3[(Mo6Cl14)Cl] 
;
_chemical_melting_point          ?
_chemical_formula_moiety         '(C6 Se4 H4 +)3, Mo6 Cl14 2-, Cl -'
_chemical_formula_sum            'C18 H12 Cl15 Mo6 Se12'
_chemical_formula_weight         2283.19

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   'R-3   '
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_Int_Tables_number      148

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

_cell_length_a                   10.9080(7)
_cell_length_b                   10.9080(7)
_cell_length_c                   10.9080(7)
_cell_angle_alpha                102.3484(3)
_cell_angle_beta                 102.3484(3)
_cell_angle_gamma                102.3484(3)
_cell_volume                     1191.82(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    4073
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      28.18


_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1035
_exptl_absorpt_coefficient_mu    11.554
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3321
_exptl_absorpt_correction_T_max  0.4738
_exptl_absorpt_process_details   
;
 APEX2 Software
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6674
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0146
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1797
_reflns_number_gt                1584
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 '
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0133P)²+0.9427P] where P=(Fo²+2Fc²)/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         1797
_refine_ls_number_parameters     78
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0180
_refine_ls_wR_factor_ref         0.0363
_refine_ls_wR_factor_gt          0.0343
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.001
_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
C1 C 0.5146(3) 0.4544(3) 0.0313(3) 0.0298(6) Uani 1 1 d . . .
C2 C 0.5502(3) 0.3100(3) 0.2009(3) 0.0430(7) Uani 1 1 d . . .
H2 H 0.5561 0.2760 0.2796 0.052 Uiso 1 1 calc R . .
C3 C 0.5682(3) 0.2419(3) 0.0939(3) 0.0433(7) Uani 1 1 d . . .
H3 H 0.5882 0.1562 0.0911 0.052 Uiso 1 1 calc R . .
Se1 Se 0.51395(3) 0.46987(3) 0.20459(3) 0.03923(8) Uani 1 1 d . . .
Se2 Se 0.55617(3) 0.30648(3) -0.05195(3) 0.03897(8) Uani 1 1 d . . .
Cl1 Cl 0.90300(6) 0.23952(6) 0.06876(6) 0.03154(14) Uani 1 1 d . . .
Cl2 Cl 1.21180(7) 0.21180(7) 0.21180(7) 0.0284(2) Uani 1 3 d S . .
Cl3 Cl 0.96517(7) 0.17217(7) 0.37723(7) 0.03874(16) Uani 1 1 d . . .
Mo1 Mo 0.98548(2) 0.07522(2) 0.16273(2) 0.02308(6) Uani 1 1 d . . .
Cl4 Cl 0.5000 0.5000 0.5000 0.0358(4) Uani 1 6 d S . .

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
C1 0.0285(13) 0.0338(14) 0.0285(13) 0.0074(11) 0.0122(11) 0.0080(11)
C2 0.0461(18) 0.0449(18) 0.0427(18) 0.0223(14) 0.0117(14) 0.0121(14)
C3 0.0492(18) 0.0383(16) 0.0490(19) 0.0214(14) 0.0156(14) 0.0141(14)
Se1 0.04833(18) 0.04392(18) 0.03107(15) 0.01250(12) 0.01618(13) 0.01649(13)
Se2 0.04936(18) 0.03484(16) 0.03951(17) 0.01125(12) 0.02042(13) 0.01605(13)
Cl1 0.0319(3) 0.0249(3) 0.0354(3) 0.0031(3) 0.0069(3) 0.0100(3)
Cl2 0.0261(2) 0.0261(2) 0.0261(2) 0.0023(3) 0.0023(3) 0.0023(3)
Cl3 0.0417(4) 0.0391(4) 0.0304(3) -0.0006(3) 0.0154(3) 0.0051(3)
Mo1 0.02278(11) 0.02290(11) 0.02088(11) 0.00311(8) 0.00527(8) 0.00418(8)
Cl4 0.0391(5) 0.0391(5) 0.0391(5) 0.0174(5) 0.0174(5) 0.0174(5)

_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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
C1 C1 1.374(5) 4_665 ?
C1 Se1 1.864(3) . ?
C1 Se2 1.870(3) . ?
C2 C3 1.320(5) . ?
C2 Se1 1.863(3) . ?
C2 H2 1.0000 . ?
C3 Se2 1.864(3) . ?
C3 H3 1.0000 . ?
Cl1 Mo1 2.4742(6) 5_665 ?
Cl1 Mo1 2.4766(7) 3_654 ?
Cl1 Mo1 2.4805(7) . ?
Cl2 Mo1 2.4741(8) 2_645 ?
Cl2 Mo1 2.4741(8) 3_654 ?
Cl2 Mo1 2.4741(8) . ?
Cl3 Mo1 2.4301(7) . ?
Mo1 Cl1 2.4742(6) 6_656 ?
Mo1 Cl1 2.4766(7) 2_645 ?
Mo1 Mo1 2.6079(4) 6_656 ?
Mo1 Mo1 2.6079(4) 5_665 ?
Mo1 Mo1 2.6089(4) 2_645 ?
Mo1 Mo1 2.6089(4) 3_654 ?

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
C1 C1 Se1 122.0(3) 4_665 . ?
C1 C1 Se2 122.3(3) 4_665 . ?
Se1 C1 Se2 115.67(14) . . ?
C3 C2 Se1 119.6(2) . . ?
C3 C2 H2 120.2 . . ?
Se1 C2 H2 120.2 . . ?
C2 C3 Se2 119.6(2) . . ?
C2 C3 H3 120.2 . . ?
Se2 C3 H3 120.2 . . ?
C2 Se1 C1 92.60(13) . . ?
C3 Se2 C1 92.45(13) . . ?
Mo1 Cl1 Mo1 63.575(17) 5_665 3_654 ?
Mo1 Cl1 Mo1 63.519(17) 5_665 . ?
Mo1 Cl1 Mo1 63.511(18) 3_654 . ?
Mo1 Cl2 Mo1 63.64(2) 2_645 3_654 ?
Mo1 Cl2 Mo1 63.64(2) 2_645 . ?
Mo1 Cl2 Mo1 63.64(2) 3_654 . ?
Cl3 Mo1 Cl2 92.70(2) . . ?
Cl3 Mo1 Cl1 91.64(2) . 6_656 ?
Cl2 Mo1 Cl1 175.66(2) . 6_656 ?
Cl3 Mo1 Cl1 91.78(2) . 2_645 ?
Cl2 Mo1 Cl1 90.032(16) . 2_645 ?
Cl1 Mo1 Cl1 89.891(16) 6_656 2_645 ?
Cl3 Mo1 Cl1 92.65(2) . . ?
Cl2 Mo1 Cl1 89.942(16) . . ?
Cl1 Mo1 Cl1 89.801(16) 6_656 . ?
Cl1 Mo1 Cl1 175.57(2) 2_645 . ?
Cl3 Mo1 Mo1 134.41(2) . 6_656 ?
Cl2 Mo1 Mo1 118.153(13) . 6_656 ?
Cl1 Mo1 Mo1 58.357(17) 6_656 6_656 ?
Cl1 Mo1 Mo1 58.168(15) 2_645 6_656 ?
Cl1 Mo1 Mo1 118.131(17) . 6_656 ?
Cl3 Mo1 Mo1 134.94(2) . 5_665 ?
Cl2 Mo1 Mo1 118.152(13) . 5_665 ?
Cl1 Mo1 Mo1 58.258(17) 6_656 5_665 ?
Cl1 Mo1 Mo1 118.179(17) 2_645 5_665 ?
Cl1 Mo1 Mo1 58.123(15) . 5_665 ?
Mo1 Mo1 Mo1 60.024(10) 6_656 5_665 ?
Cl3 Mo1 Mo1 135.06(2) . 2_645 ?
Cl2 Mo1 Mo1 58.181(12) . 2_645 ?
Cl1 Mo1 Mo1 118.330(16) 6_656 2_645 ?
Cl1 Mo1 Mo1 58.318(18) 2_645 2_645 ?
Cl1 Mo1 Mo1 118.153(18) . 2_645 ?
Mo1 Mo1 Mo1 59.989(5) 6_656 2_645 ?
Mo1 Mo1 Mo1 89.999(1) 5_665 2_645 ?
Cl3 Mo1 Mo1 135.59(2) . 3_654 ?
Cl2 Mo1 Mo1 58.181(12) . 3_654 ?
Cl1 Mo1 Mo1 118.232(16) 6_656 3_654 ?
Cl1 Mo1 Mo1 118.297(18) 2_645 3_654 ?
Cl1 Mo1 Mo1 58.173(18) . 3_654 ?
Mo1 Mo1 Mo1 90.0 6_656 3_654 ?
Mo1 Mo1 Mo1 59.988(5) 5_665 3_654 ?
Mo1 Mo1 Mo1 60.0 2_645 3_654 ?

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
Se1 C2 C3 Se2 -0.3(4) . . . . ?
C3 C2 Se1 C1 2.0(3) . . . . ?
C1 C1 Se1 C2 176.5(3) 4_665 . . . ?
Se2 C1 Se1 C2 -2.99(16) . . . . ?
C2 C3 Se2 C1 -1.6(3) . . . . ?
C1 C1 Se2 C3 -176.6(3) 4_665 . . . ?
Se1 C1 Se2 C3 2.88(17) . . . . ?
Mo1 Cl2 Mo1 Cl3 143.58(2) 2_645 . . . ?
Mo1 Cl2 Mo1 Cl3 -144.33(2) 3_654 . . . ?
Mo1 Cl2 Mo1 Cl1 -37.2(2) 2_645 . . 6_656 ?
Mo1 Cl2 Mo1 Cl1 34.9(2) 3_654 . . 6_656 ?
Mo1 Cl2 Mo1 Cl1 51.797(18) 2_645 . . 2_645 ?
Mo1 Cl2 Mo1 Cl1 123.886(17) 3_654 . . 2_645 ?
Mo1 Cl2 Mo1 Cl1 -123.773(17) 2_645 . . . ?
Mo1 Cl2 Mo1 Cl1 -51.684(18) 3_654 . . . ?
Mo1 Cl2 Mo1 Mo1 -1.482(11) 2_645 . . 6_656 ?
Mo1 Cl2 Mo1 Mo1 70.607(4) 3_654 . . 6_656 ?
Mo1 Cl2 Mo1 Mo1 -70.606(4) 2_645 . . 5_665 ?
Mo1 Cl2 Mo1 Mo1 1.483(11) 3_654 . . 5_665 ?
Mo1 Cl2 Mo1 Mo1 72.089(11) 3_654 . . 2_645 ?
Mo1 Cl2 Mo1 Mo1 -72.089(11) 2_645 . . 3_654 ?
Mo1 Cl1 Mo1 Cl3 -143.50(2) 5_665 . . . ?
Mo1 Cl1 Mo1 Cl3 144.390(19) 3_654 . . . ?
Mo1 Cl1 Mo1 Cl2 123.796(18) 5_665 . . . ?
Mo1 Cl1 Mo1 Cl2 51.690(18) 3_654 . . . ?
Mo1 Cl1 Mo1 Cl1 -51.88(2) 5_665 . . 6_656 ?
Mo1 Cl1 Mo1 Cl1 -123.98(2) 3_654 . . 6_656 ?
Mo1 Cl1 Mo1 Cl1 34.1(3) 5_665 . . 2_645 ?
Mo1 Cl1 Mo1 Cl1 -38.0(3) 3_654 . . 2_645 ?
Mo1 Cl1 Mo1 Mo1 1.49(2) 5_665 . . 6_656 ?
Mo1 Cl1 Mo1 Mo1 -70.619(17) 3_654 . . 6_656 ?
Mo1 Cl1 Mo1 Mo1 -72.106(13) 3_654 . . 5_665 ?
Mo1 Cl1 Mo1 Mo1 70.561(15) 5_665 . . 2_645 ?
Mo1 Cl1 Mo1 Mo1 -1.545(17) 3_654 . . 2_645 ?
Mo1 Cl1 Mo1 Mo1 72.106(13) 5_665 . . 3_654 ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.073
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TTF3_Mo6Br14_Br_100K
_database_code_depnum_ccdc_archive 'CCDC 999369'
_audit_update_record             
;
2015-07-08 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            
; 
(TTF)3[(Mo6B14)Br] 
;
_chemical_melting_point          ?
_chemical_formula_moiety         '(C6 S4 H4 +)3, Mo6 Br14 2-, Br -'
_chemical_formula_sum            'C18 H12 Br15 Mo6 S12'
_chemical_formula_weight         2387.29

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'
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   'R -3   '
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_Int_Tables_number      148

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

_cell_length_a                   10.8797(5)
_cell_length_b                   10.8797(5)
_cell_length_c                   10.8797(5)
_cell_angle_alpha                101.1590(10)
_cell_angle_beta                 101.1590(10)
_cell_angle_gamma                101.1590(10)
_cell_volume                     1203.35(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3804
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      28.09

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1089
_exptl_absorpt_coefficient_mu    14.509
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2037
_exptl_absorpt_correction_T_max  0.2958
_exptl_absorpt_process_details   
;
 APEX2 Software
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6614
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1800
_reflns_number_gt                1629
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 '
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0167P)²+4.2907P] where P=(Fo²+2Fc²)/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         1800
_refine_ls_number_parameters     78
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0214
_refine_ls_wR_factor_ref         0.0476
_refine_ls_wR_factor_gt          0.0459
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.002
_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
Mo1 Mo 0.92749(3) 0.83627(3) 0.01709(3) 0.01008(8) Uani 1 1 d . . .
Br2 Br 0.78394(4) 0.78394(4) -0.21606(4) 0.01225(12) Uani 1 3 d S . .
Br3 Br 1.07227(3) 0.89225(3) 0.24985(3) 0.01314(9) Uani 1 1 d . . .
Br5 Br 0.82697(3) 0.60717(3) 0.03819(3) 0.01628(9) Uani 1 1 d . . .
Br4 Br 0.5000 0.5000 0.5000 0.0208(2) Uani 1 6 d S . .
S1 S 0.51550(10) 0.47518(9) 0.19508(9) 0.0199(2) Uani 1 1 d . . .
S2 S 0.54862(9) 0.31449(9) -0.03801(9) 0.01874(19) Uani 1 1 d . . .
C1 C 0.5141(4) 0.4547(4) 0.0338(4) 0.0174(7) Uani 1 1 d . . .
C3 C 0.5655(4) 0.2555(4) 0.0993(4) 0.0209(8) Uani 1 1 d . . .
H3 H 0.5858 0.1697 0.0988 0.025 Uiso 1 1 calc R . .
C2 C 0.5503(4) 0.3292(4) 0.2057(4) 0.0209(8) Uani 1 1 d . . .
H2 H 0.5588 0.3008 0.2884 0.025 Uiso 1 1 calc R . .

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
Mo1 0.01007(15) 0.00930(14) 0.01000(15) 0.00203(11) 0.00167(11) 0.00135(11)
Br2 0.01144(14) 0.01144(14) 0.01144(14) 0.00086(15) 0.00086(15) 0.00086(15)
Br3 0.01461(17) 0.01333(17) 0.01087(16) 0.00383(13) 0.00125(13) 0.00277(13)
Br5 0.01622(18) 0.01315(18) 0.01822(19) 0.00598(14) 0.00244(14) 0.00008(14)
Br4 0.0219(2) 0.0219(2) 0.0219(2) 0.0077(3) 0.0077(3) 0.0077(3)
S1 0.0234(5) 0.0200(5) 0.0176(5) 0.0037(4) 0.0071(4) 0.0068(4)
S2 0.0208(5) 0.0162(4) 0.0205(5) 0.0035(4) 0.0078(4) 0.0056(4)
C1 0.0164(18) 0.0195(19) 0.0159(18) 0.0010(15) 0.0069(15) 0.0038(15)
C3 0.0184(19) 0.020(2) 0.026(2) 0.0077(16) 0.0062(16) 0.0048(15)
C2 0.021(2) 0.021(2) 0.022(2) 0.0084(16) 0.0047(16) 0.0058(16)

_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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
Mo1 Br5 2.5933(5) . ?
Mo1 Br3 2.5986(5) . ?
Mo1 Br2 2.6002(6) . ?
Mo1 Br3 2.6012(5) 6_766 ?
Mo1 Br3 2.6049(4) 5_676 ?
Mo1 Mo1 2.6322(5) 3_564 ?
Mo1 Mo1 2.6323(5) 2_654 ?
Mo1 Mo1 2.6374(5) 5_676 ?
Mo1 Mo1 2.6374(5) 6_766 ?
Br2 Mo1 2.6002(6) 3_564 ?
Br2 Mo1 2.6003(6) 2_654 ?
Br3 Mo1 2.6012(5) 5_676 ?
Br3 Mo1 2.6049(5) 6_766 ?
S1 C1 1.722(4) . ?
S1 C2 1.723(4) . ?
S2 C1 1.718(4) . ?
S2 C3 1.728(4) . ?
C1 C1 1.386(8) 4_665 ?
C3 C2 1.333(6) . ?

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
Br5 Mo1 Br3 90.935(14) . . ?
Br5 Mo1 Br2 89.956(14) . . ?
Br3 Mo1 Br2 179.106(17) . . ?
Br5 Mo1 Br3 90.046(14) . 6_766 ?
Br3 Mo1 Br3 89.830(12) . 6_766 ?
Br2 Mo1 Br3 90.244(12) . 6_766 ?
Br5 Mo1 Br3 91.166(14) . 5_676 ?
Br3 Mo1 Br3 89.746(12) . 5_676 ?
Br2 Mo1 Br3 90.161(12) . 5_676 ?
Br3 Mo1 Br3 178.723(18) 6_766 5_676 ?
Br5 Mo1 Mo1 134.965(14) . 3_564 ?
Br3 Mo1 Mo1 119.634(12) . 3_564 ?
Br2 Mo1 Mo1 59.591(8) . 3_564 ?
Br3 Mo1 Mo1 119.696(14) 6_766 3_564 ?
Br3 Mo1 Mo1 59.557(14) 5_676 3_564 ?
Br5 Mo1 Mo1 134.259(14) . 2_654 ?
Br3 Mo1 Mo1 119.729(11) . 2_654 ?
Br2 Mo1 Mo1 59.592(8) . 2_654 ?
Br3 Mo1 Mo1 59.698(14) 6_766 2_654 ?
Br3 Mo1 Mo1 119.556(14) 5_676 2_654 ?
Mo1 Mo1 Mo1 60.0 3_564 2_654 ?
Br5 Mo1 Mo1 135.741(14) . 5_676 ?
Br3 Mo1 Mo1 59.571(13) . 5_676 ?
Br2 Mo1 Mo1 119.653(11) . 5_676 ?
Br3 Mo1 Mo1 119.347(14) 6_766 5_676 ?
Br3 Mo1 Mo1 59.427(10) 5_676 5_676 ?
Mo1 Mo1 Mo1 60.063(7) 3_564 5_676 ?
Mo1 Mo1 Mo1 90.000(1) 2_654 5_676 ?
Br5 Mo1 Mo1 135.025(14) . 6_766 ?
Br3 Mo1 Mo1 59.665(13) . 6_766 ?
Br2 Mo1 Mo1 119.656(11) . 6_766 ?
Br3 Mo1 Mo1 59.474(10) 6_766 6_766 ?
Br3 Mo1 Mo1 119.300(15) 5_676 6_766 ?
Mo1 Mo1 Mo1 90.0 3_564 6_766 ?
Mo1 Mo1 Mo1 60.064(7) 2_654 6_766 ?
Mo1 Mo1 Mo1 59.873(14) 5_676 6_766 ?
Mo1 Br2 Mo1 60.816(16) 3_564 . ?
Mo1 Br2 Mo1 60.817(16) 3_564 2_654 ?
Mo1 Br2 Mo1 60.816(16) . 2_654 ?
Mo1 Br3 Mo1 60.955(14) . 5_676 ?
Mo1 Br3 Mo1 60.907(14) . 6_766 ?
Mo1 Br3 Mo1 60.744(15) 5_676 6_766 ?
C1 S1 C2 94.78(19) . . ?
C1 S2 C3 94.71(19) . . ?
C1 C1 S2 122.2(4) 4_665 . ?
C1 C1 S1 121.9(4) 4_665 . ?
S2 C1 S1 115.9(2) . . ?
C2 C3 S2 117.3(3) . . ?
C3 C2 S1 117.3(3) . . ?

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
Br5 Mo1 Br2 Mo1 145.069(17) . . . 3_564 ?
Br3 Mo1 Br2 Mo1 -30.1(10) . . . 3_564 ?
Br3 Mo1 Br2 Mo1 -124.885(12) 6_766 . . 3_564 ?
Br3 Mo1 Br2 Mo1 53.904(14) 5_676 . . 3_564 ?
Mo1 Mo1 Br2 Mo1 -70.867(7) 2_654 . . 3_564 ?
Mo1 Mo1 Br2 Mo1 -0.386(9) 5_676 . . 3_564 ?
Mo1 Mo1 Br2 Mo1 -70.481(6) 6_766 . . 3_564 ?
Br5 Mo1 Br2 Mo1 -144.064(17) . . . 2_654 ?
Br3 Mo1 Br2 Mo1 40.8(10) . . . 2_654 ?
Br3 Mo1 Br2 Mo1 -54.018(14) 6_766 . . 2_654 ?
Br3 Mo1 Br2 Mo1 124.771(12) 5_676 . . 2_654 ?
Mo1 Mo1 Br2 Mo1 70.867(6) 3_564 . . 2_654 ?
Mo1 Mo1 Br2 Mo1 70.481(6) 5_676 . . 2_654 ?
Mo1 Mo1 Br2 Mo1 0.386(9) 6_766 . . 2_654 ?
Br5 Mo1 Br3 Mo1 -145.198(15) . . . 5_676 ?
Br2 Mo1 Br3 Mo1 30.0(10) . . . 5_676 ?
Br3 Mo1 Br3 Mo1 124.759(10) 6_766 . . 5_676 ?
Br3 Mo1 Br3 Mo1 -54.036(12) 5_676 . . 5_676 ?
Mo1 Mo1 Br3 Mo1 0.129(16) 3_564 . . 5_676 ?
Mo1 Mo1 Br3 Mo1 70.401(15) 2_654 . . 5_676 ?
Mo1 Mo1 Br3 Mo1 70.688(14) 6_766 . . 5_676 ?
Br5 Mo1 Br3 Mo1 144.115(14) . . . 6_766 ?
Br2 Mo1 Br3 Mo1 -40.7(10) . . . 6_766 ?
Br3 Mo1 Br3 Mo1 54.071(12) 6_766 . . 6_766 ?
Br3 Mo1 Br3 Mo1 -124.724(10) 5_676 . . 6_766 ?
Mo1 Mo1 Br3 Mo1 -70.559(15) 3_564 . . 6_766 ?
Mo1 Mo1 Br3 Mo1 -0.287(16) 2_654 . . 6_766 ?
Mo1 Mo1 Br3 Mo1 -70.688(13) 5_676 . . 6_766 ?
C3 S2 C1 C1 -178.0(4) . . . 4_665 ?
C3 S2 C1 S1 1.5(3) . . . . ?
C2 S1 C1 C1 178.0(5) . . . 4_665 ?
C2 S1 C1 S2 -1.5(3) . . . . ?
C1 S2 C3 C2 -0.9(4) . . . . ?
S2 C3 C2 S1 0.0(5) . . . . ?
C1 S1 C2 C3 0.9(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.569
_refine_diff_density_min         -1.971
_refine_diff_density_rms         0.123
_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TTF3_Mo6Br14_Br_300K
_database_code_depnum_ccdc_archive 'CCDC 999370'
_audit_update_record             
;
2014-04-25 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_common            
; 
(TTF)3[(Mo6B14)Br] 
;
_chemical_melting_point          ?
_chemical_formula_moiety         '(C6 S4 H4 +)3, Mo6 Br14 2-, Br -'
_chemical_formula_sum            'C18 H12 Br15 Mo6 S12'
_chemical_formula_weight         2387.29

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'
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   'R -3   '
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_Int_Tables_number      148

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

_cell_length_a                   10.9429(5)
_cell_length_b                   10.9429(5)
_cell_length_c                   10.9429(5)
_cell_angle_alpha                100.9150(10)
_cell_angle_beta                 100.9150(10)
_cell_angle_gamma                100.9150(10)
_cell_volume                     1228.45(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    3804
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      28.09

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1089
_exptl_absorpt_coefficient_mu    14.213
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2012
_exptl_absorpt_correction_T_max  0.3014
_exptl_absorpt_process_details   
;
 APEX2 Software
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6645
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         27.47
_reflns_number_total             1835
_reflns_number_gt                1519
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 '
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0171P)²+3.9942P] where P=(Fo²+2Fc²)/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         1835
_refine_ls_number_parameters     78
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0586
_refine_ls_wR_factor_gt          0.0524
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_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
Mo1 Mo 0.92759(4) 0.83793(4) 0.01802(4) 0.02365(10) Uani 1 1 d . . .
Br2 Br 0.78654(5) 0.78654(5) -0.21346(5) 0.02963(18) Uani 1 3 d S . .
Br3 Br 1.06978(5) 0.89289(5) 0.24922(4) 0.03211(13) Uani 1 1 d . . .
Br5 Br 0.82720(5) 0.61106(5) 0.04037(5) 0.04044(14) Uani 1 1 d . . .
Br4 Br 0.5000 0.5000 0.5000 0.0473(3) Uani 1 6 d S . .
S1 S 0.51537(15) 0.47504(15) 0.19348(14) 0.0485(4) Uani 1 1 d . . .
S2 S 0.54773(14) 0.31557(13) -0.03712(14) 0.0448(3) Uani 1 1 d . . .
C1 C 0.5142(5) 0.4552(5) 0.0344(5) 0.0366(11) Uani 1 1 d . . .
C3 C 0.5647(6) 0.2572(6) 0.0991(6) 0.0496(14) Uani 1 1 d . . .
H3 H 0.5845 0.1716 0.0990 0.060 Uiso 1 1 calc R . .
C2 C 0.5501(6) 0.3310(6) 0.2046(6) 0.0514(15) Uani 1 1 d . . .
H2 H 0.5592 0.3032 0.2872 0.062 Uiso 1 1 calc R . .

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
Mo1 0.0237(2) 0.0219(2) 0.0237(2) 0.00502(15) 0.00400(15) 0.00305(15)
Br2 0.02757(19) 0.02757(19) 0.02757(19) 0.0015(2) 0.0015(2) 0.0015(2)
Br3 0.0364(3) 0.0326(3) 0.0259(2) 0.00982(19) 0.0025(2) 0.0065(2)
Br5 0.0404(3) 0.0322(3) 0.0454(3) 0.0159(2) 0.0050(2) -0.0013(2)
Br4 0.0506(4) 0.0506(4) 0.0506(4) 0.0198(5) 0.0198(5) 0.0198(5)
S1 0.0593(9) 0.0480(8) 0.0424(8) 0.0093(7) 0.0188(7) 0.0171(7)
S2 0.0506(8) 0.0377(7) 0.0489(8) 0.0070(6) 0.0188(7) 0.0127(6)
C1 0.032(3) 0.039(3) 0.036(3) 0.002(2) 0.012(2) 0.005(2)
C3 0.043(3) 0.045(3) 0.064(4) 0.019(3) 0.014(3) 0.010(3)
C2 0.058(4) 0.054(4) 0.048(3) 0.017(3) 0.016(3) 0.018(3)

_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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
Mo1 Br5 2.5941(6) . ?
Mo1 Br3 2.6005(6) . ?
Mo1 Br2 2.6012(7) . ?
Mo1 Br3 2.6017(6) 6_766 ?
Mo1 Br3 2.6068(6) 5_676 ?
Mo1 Mo1 2.6321(6) 3_564 ?
Mo1 Mo1 2.6321(6) 2_654 ?
Mo1 Mo1 2.6377(6) 6_766 ?
Mo1 Mo1 2.6377(6) 5_676 ?
Br2 Mo1 2.6012(7) 2_654 ?
Br2 Mo1 2.6012(7) 3_564 ?
Br3 Mo1 2.6018(6) 5_676 ?
Br3 Mo1 2.6068(6) 6_766 ?
S1 C1 1.711(5) . ?
S1 C2 1.711(6) . ?
S2 C1 1.718(5) . ?
S2 C3 1.722(6) . ?
C1 C1 1.389(10) 4_665 ?
C3 C2 1.333(8) . ?

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
Br5 Mo1 Br3 90.94(2) . . ?
Br5 Mo1 Br2 89.920(19) . . ?
Br3 Mo1 Br2 179.13(2) . . ?
Br5 Mo1 Br3 89.99(2) . 6_766 ?
Br3 Mo1 Br3 89.848(16) . 6_766 ?
Br2 Mo1 Br3 90.254(16) . 6_766 ?
Br5 Mo1 Br3 91.18(2) . 5_676 ?
Br3 Mo1 Br3 89.737(16) . 5_676 ?
Br2 Mo1 Br3 90.143(16) . 5_676 ?
Br3 Mo1 Br3 178.77(2) 6_766 5_676 ?
Br5 Mo1 Mo1 134.963(19) . 3_564 ?
Br3 Mo1 Mo1 119.627(16) . 3_564 ?
Br2 Mo1 Mo1 59.607(10) . 3_564 ?
Br3 Mo1 Mo1 119.737(19) 6_766 3_564 ?
Br3 Mo1 Mo1 59.550(19) 5_676 3_564 ?
Br5 Mo1 Mo1 134.24(2) . 2_654 ?
Br3 Mo1 Mo1 119.755(16) . 2_654 ?
Br2 Mo1 Mo1 59.605(10) . 2_654 ?
Br3 Mo1 Mo1 59.740(19) 6_766 2_654 ?
Br3 Mo1 Mo1 119.547(19) 5_676 2_654 ?
Mo1 Mo1 Mo1 60.0 3_564 2_654 ?
Br5 Mo1 Mo1 135.030(19) . 6_766 ?
Br3 Mo1 Mo1 59.685(18) . 6_766 ?
Br2 Mo1 Mo1 119.674(14) . 6_766 ?
Br3 Mo1 Mo1 59.510(14) 6_766 6_766 ?
Br3 Mo1 Mo1 119.307(19) 5_676 6_766 ?
Mo1 Mo1 Mo1 89.999(1) 3_564 6_766 ?
Mo1 Mo1 Mo1 60.070(9) 2_654 6_766 ?
Br5 Mo1 Mo1 135.77(2) . 5_676 ?
Br3 Mo1 Mo1 59.558(18) . 5_676 ?
Br2 Mo1 Mo1 119.674(14) . 5_676 ?
Br3 Mo1 Mo1 119.369(19) 6_766 5_676 ?
Br3 Mo1 Mo1 59.448(14) 5_676 5_676 ?
Mo1 Mo1 Mo1 60.068(9) 3_564 5_676 ?
Mo1 Mo1 Mo1 90.0 2_654 5_676 ?
Mo1 Mo1 Mo1 59.859(19) 6_766 5_676 ?
Mo1 Br2 Mo1 60.79(2) 2_654 . ?
Mo1 Br2 Mo1 60.79(2) 2_654 3_564 ?
Mo1 Br2 Mo1 60.79(2) . 3_564 ?
Mo1 Br3 Mo1 60.933(18) . 5_676 ?
Mo1 Br3 Mo1 60.867(18) . 6_766 ?
Mo1 Br3 Mo1 60.707(19) 5_676 6_766 ?
C1 S1 C2 94.9(3) . . ?
C1 S2 C3 94.6(3) . . ?
C1 C1 S1 122.6(5) 4_665 . ?
C1 C1 S2 121.5(5) 4_665 . ?
S1 C1 S2 115.9(3) . . ?
C2 C3 S2 117.1(5) . . ?
C3 C2 S1 117.5(5) . . ?

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
Br5 Mo1 Br2 Mo1 -144.06(2) . . . 2_654 ?
Br3 Mo1 Br2 Mo1 42.7(13) . . . 2_654 ?
Br3 Mo1 Br2 Mo1 -54.067(19) 6_766 . . 2_654 ?
Br3 Mo1 Br2 Mo1 124.768(17) 5_676 . . 2_654 ?
Mo1 Mo1 Br2 Mo1 70.854(9) 3_564 . . 2_654 ?
Mo1 Mo1 Br2 Mo1 0.380(11) 6_766 . . 2_654 ?
Mo1 Mo1 Br2 Mo1 70.473(8) 5_676 . . 2_654 ?
Br5 Mo1 Br2 Mo1 145.09(2) . . . 3_564 ?
Br3 Mo1 Br2 Mo1 -28.2(13) . . . 3_564 ?
Br3 Mo1 Br2 Mo1 -124.921(17) 6_766 . . 3_564 ?
Br3 Mo1 Br2 Mo1 53.914(19) 5_676 . . 3_564 ?
Mo1 Mo1 Br2 Mo1 -70.854(9) 2_654 . . 3_564 ?
Mo1 Mo1 Br2 Mo1 -70.474(8) 6_766 . . 3_564 ?
Mo1 Mo1 Br2 Mo1 -0.380(11) 5_676 . . 3_564 ?
Br5 Mo1 Br3 Mo1 -145.23(2) . . . 5_676 ?
Br2 Mo1 Br3 Mo1 28.0(13) . . . 5_676 ?
Br3 Mo1 Br3 Mo1 124.779(13) 6_766 . . 5_676 ?
Br3 Mo1 Br3 Mo1 -54.063(16) 5_676 . . 5_676 ?
Mo1 Mo1 Br3 Mo1 0.09(2) 3_564 . . 5_676 ?
Mo1 Mo1 Br3 Mo1 70.37(2) 2_654 . . 5_676 ?
Mo1 Mo1 Br3 Mo1 70.667(18) 6_766 . . 5_676 ?
Br5 Mo1 Br3 Mo1 144.10(2) . . . 6_766 ?
Br2 Mo1 Br3 Mo1 -42.6(13) . . . 6_766 ?
Br3 Mo1 Br3 Mo1 54.111(16) 6_766 . . 6_766 ?
Br3 Mo1 Br3 Mo1 -124.730(13) 5_676 . . 6_766 ?
Mo1 Mo1 Br3 Mo1 -70.58(2) 3_564 . . 6_766 ?
Mo1 Mo1 Br3 Mo1 -0.30(2) 2_654 . . 6_766 ?
Mo1 Mo1 Br3 Mo1 -70.667(18) 5_676 . . 6_766 ?
C2 S1 C1 C1 177.8(6) . . . 4_665 ?
C2 S1 C1 S2 -1.0(4) . . . . ?
C3 S2 C1 C1 -177.7(6) . . . 4_665 ?
C3 S2 C1 S1 1.2(4) . . . . ?
C1 S2 C3 C2 -0.9(5) . . . . ?
S2 C3 C2 S1 0.4(7) . . . . ?
C1 S1 C2 C3 0.4(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.735
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.141
