# Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               J.Mater.Chem.
_journal_coden_Cambridge         1145
loop_
_publ_author_name
_publ_author_address
'Stefanie Jakob'
;
Department Chemie und Biochemie
Ludwig - Maximilians - Universitat Munchen
Butenandtstrasse 5 - 13 (D)
D 81377 Munchen
Germany
;
'Helen Muller'
;
Department Chemie und Biochemie
Ludwig - Maximilians - Universitat Munchen
Butenandtstrasse 5 - 13 (D)
D 81377 Munchen
Germany
;
'Dirk Johrendt'
;
Department Chemie und Biochemie
Ludwig - Maximilians - Universitat Munchen
Butenandtstrasse 5 - 13 (D)
D 81377 Munchen
Germany
;
'Rainer Pottgen'
;
Institut fur Anorganische und Analytische Chemie
Westfalische Wilhelms - Universitat Munster
Wilhelm Klemm Strasse 8
D 48149 Munster
Germany
;
'Sudhindra Rayaprol'
;
Institut fur Anorganische und Analytische Chemie
Westfalische Wilhelms - Universitat Munster
Wilhelm Klemm Strasse 8
D 48149 Munster
Germany
;
;
S.Altmannshofer
;
;
Lehrstuhl fur Chemische Physik und Materialwissenschaften
Universitat Augsburg
Universitatsstrasse 1 (Gebaude Sud)
D 86159 Augsburg
Germany
;
'Wolfgang Scherer'
;
Lehrstuhl fur Chemische Physik und Materialwissenschaften
Universitat Augsburg
Universitatsstrasse 1 (Gebaude Sud)
D 86159 Augsburg
Germany
;

_publ_contact_author             
;
Dirk Johrendt
Department Chemie und Biochemie
Ludwig-Maximilians-Universitat Munchen
Butenandtstrasse 5 - 13 (D)
D 81377 Munchen
Germany
;
_publ_contact_author_email       Dirk.Johrendt@cup.uni-muenchen.de
_publ_contact_author_fax         '049 89 2180 77431'
_publ_contact_author_phone       '049 89 2180 77430'
_publ_section_title              
;
Structural and Magnetic Transitions in the Mott-Insulator GaNb4S8
;
_publ_contact_author_name        'Dirk Johrendt'

# Attachment 'GaNb4S8_50K_REV1.CIF'

data_GaNb4S8_50K
_database_code_depnum_ccdc_archive 'CCDC 642571'

# 2. Crystal data_50a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Ga Nb4 S8'
_chemical_formula_sum            'Ga Nb4 S8'
_chemical_formula_weight         697.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'F -4 3 m'
_symmetry_space_group_name_Hall  'F -4 2 3'

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

_cell_length_a                   9.9866(11)
_cell_length_b                   9.9866(11)
_cell_length_c                   9.9866(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     995.99(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    50(2)
_cell_measurement_reflns_used    1504
_cell_measurement_theta_min      5.7
_cell_measurement_theta_max      46.49

_exptl_crystal_description       cube
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour            'dark grey'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1292
_exptl_absorpt_coefficient_mu    8.746
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.117
_exptl_absorpt_correction_T_max  0.186
_exptl_absorpt_process_details   'using program MULABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      50(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode FR 591 Bruker'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'HUBER 4 circle diffractometer'
_diffrn_measurement_method       'rotating measurement'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            1504
_diffrn_reflns_av_R_equivalents  0.1296
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.53
_diffrn_reflns_theta_max         23.24
_reflns_number_total             98
_reflns_number_gt                97
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'FD345 (Weber, 2004)'
_computing_cell_refinement       'EVAL-14 (Duisenberg, 2003)'
_computing_data_reduction        'EVAL-14 (Duisenberg, 2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0041P)^2^+6.8536P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(6)
_refine_ls_number_reflns         98
_refine_ls_number_parameters     12
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0127
_refine_ls_wR_factor_ref         0.0485
_refine_ls_wR_factor_gt          0.0478
_refine_ls_goodness_of_fit_ref   1.351
_refine_ls_restrained_S_all      1.351
_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
Ga Ga 0.0000 0.0000 0.0000 0.0052(6) Uani 1 24 d S . .
Nb Nb 0.60537(6) 0.60537(6) 0.60537(6) 0.0070(4) Uani 1 6 d S . .
S1 S 0.3666(2) 0.3666(2) 0.3666(2) 0.0063(9) Uani 1 6 d S . .
S2 S 0.8675(3) 0.8675(3) 0.8675(3) 0.0084(12) 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
Ga 0.0052(6) 0.0052(6) 0.0052(6) 0.000 0.000 0.000
Nb 0.0070(4) 0.0070(4) 0.0070(4) 0.0000(3) 0.0000(3) 0.0000(3)
S1 0.0063(9) 0.0063(9) 0.0063(9) -0.0001(7) -0.0001(7) -0.0001(7)
S2 0.0084(12) 0.0084(12) 0.0084(12) -0.0022(8) -0.0022(8) -0.0022(8)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ga S2 2.292(4) 1_444 ?
Ga S2 2.292(4) 4_466 ?
Ga S2 2.292(4) 2_664 ?
Ga S2 2.292(4) 3_646 ?
Nb S1 2.417(3) 4_566 ?
Nb S1 2.417(3) 3_656 ?
Nb S1 2.417(3) 2_665 ?
Nb S2 2.646(2) 28_566 ?
Nb S2 2.646(2) 51_656 ?
Nb S2 2.646(2) 74_665 ?
Nb Nb 2.9764(17) 4_566 ?
Nb Nb 2.9764(17) 2_665 ?
Nb Nb 2.9764(17) 3_656 ?
S1 Nb 2.417(3) 4_566 ?
S1 Nb 2.417(3) 2_665 ?
S1 Nb 2.417(3) 3_656 ?
S2 Ga 2.292(4) 1_666 ?
S2 Nb 2.646(2) 28_566 ?
S2 Nb 2.646(2) 74_665 ?
S2 Nb 2.646(2) 51_656 ?

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
S2 Ga S2 109.5 1_444 4_466 ?
S2 Ga S2 109.5 1_444 2_664 ?
S2 Ga S2 109.5 4_466 2_664 ?
S2 Ga S2 109.5 1_444 3_646 ?
S2 Ga S2 109.5 4_466 3_646 ?
S2 Ga S2 109.5 2_664 3_646 ?
S1 Nb S1 102.40(9) 4_566 3_656 ?
S1 Nb S1 102.40(9) 4_566 2_665 ?
S1 Nb S1 102.40(9) 3_656 2_665 ?
S1 Nb S2 162.27(9) 4_566 28_566 ?
S1 Nb S2 88.55(10) 3_656 28_566 ?
S1 Nb S2 88.55(10) 2_665 28_566 ?
S1 Nb S2 88.55(10) 4_566 51_656 ?
S1 Nb S2 162.27(9) 3_656 51_656 ?
S1 Nb S2 88.55(10) 2_665 51_656 ?
S2 Nb S2 77.70(14) 28_566 51_656 ?
S1 Nb S2 88.55(10) 4_566 74_665 ?
S1 Nb S2 88.55(10) 3_656 74_665 ?
S1 Nb S2 162.27(9) 2_665 74_665 ?
S2 Nb S2 77.70(14) 28_566 74_665 ?
S2 Nb S2 77.70(14) 51_656 74_665 ?
S1 Nb Nb 99.41(8) 4_566 4_566 ?
S1 Nb Nb 51.99(6) 3_656 4_566 ?
S1 Nb Nb 51.99(6) 2_665 4_566 ?
S2 Nb Nb 98.32(9) 28_566 4_566 ?
S2 Nb Nb 140.54(5) 51_656 4_566 ?
S2 Nb Nb 140.54(5) 74_665 4_566 ?
S1 Nb Nb 51.99(6) 4_566 2_665 ?
S1 Nb Nb 51.99(6) 3_656 2_665 ?
S1 Nb Nb 99.41(8) 2_665 2_665 ?
S2 Nb Nb 140.54(5) 28_566 2_665 ?
S2 Nb Nb 140.54(5) 51_656 2_665 ?
S2 Nb Nb 98.32(9) 74_665 2_665 ?
Nb Nb Nb 60.0 4_566 2_665 ?
S1 Nb Nb 51.99(6) 4_566 3_656 ?
S1 Nb Nb 99.41(8) 3_656 3_656 ?
S1 Nb Nb 51.99(6) 2_665 3_656 ?
S2 Nb Nb 140.54(5) 28_566 3_656 ?
S2 Nb Nb 98.32(9) 51_656 3_656 ?
S2 Nb Nb 140.54(5) 74_665 3_656 ?
Nb Nb Nb 60.0 4_566 3_656 ?
Nb Nb Nb 60.0 2_665 3_656 ?
Nb S1 Nb 76.03(12) 4_566 2_665 ?
Nb S1 Nb 76.03(12) 4_566 3_656 ?
Nb S1 Nb 76.03(12) 2_665 3_656 ?
Ga S2 Nb 116.94(9) 1_666 28_566 ?
Ga S2 Nb 116.94(9) 1_666 74_665 ?
Nb S2 Nb 101.07(11) 28_566 74_665 ?
Ga S2 Nb 116.94(9) 1_666 51_656 ?
Nb S2 Nb 101.07(11) 28_566 51_656 ?
Nb S2 Nb 101.07(11) 74_665 51_656 ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        23.24
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.520
_refine_diff_density_rms         0.674

data_GaNb4S8_20K
_database_code_depnum_ccdc_archive 'CCDC 642572'

# 2. Crystal data_113_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Ga Nb4 S8'
_chemical_formula_sum            'Ga Nb4 S8'
_chemical_formula_weight         697.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P -4 21 m'
_symmetry_space_group_name_Hall  'P -4 2ab'

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

_cell_length_a                   9.9917(14)
_cell_length_b                   9.9917(14)
_cell_length_c                   9.978(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     996.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    20(2)
_cell_measurement_reflns_used    11656
_cell_measurement_theta_min      5.7
_cell_measurement_theta_max      66.61

_exptl_crystal_description       cube
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour            'dark grey'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1292
_exptl_absorpt_coefficient_mu    8.744
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.096
_exptl_absorpt_correction_T_max  0.167
_exptl_absorpt_process_details   'using program MULABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      20.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode FR 591 Bruker'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'HUBER 4 circle diffractometer'
_diffrn_measurement_method       'rotating measurement'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11656
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.56
_diffrn_reflns_theta_max         33.30
_reflns_number_total             2003
_reflns_number_gt                1975
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'FD345 (Weber, 2004)'
_computing_cell_refinement       'EVAL-14 (Duisenberg, 2003)'
_computing_data_reduction        'EVAL-14 (Duisenberg, 2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Pseudo-merohedral twinning and triple crystal domains; Twin law: 010 001 100;
Twin ratio:0.29:0.30:0.41.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+2.4816P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(18)
_refine_ls_number_reflns         2003
_refine_ls_number_parameters     54
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0790
_refine_ls_wR_factor_gt          0.0778
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.013

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.85775(6) 0.85268(6) 0.64574(12) 0.00368(18) Uani 1 1 d . . .
Nb2 Nb 0.85508(6) 0.64492(6) 0.85010(12) 0.00308(19) Uani 1 2 d S . .
Nb3 Nb 0.64271(7) 0.85729(7) 0.86007(12) 0.0040(2) Uani 1 2 d S . .
Ga Ga 0.75120(4) 0.74880(4) 0.24980(12) 0.00329(13) Uani 1 2 d S . .
S11 S 0.88556(19) 0.61444(19) 0.6122(2) 0.00438(19) Uani 1 2 d S . .
S12 S 0.61810(19) 0.88190(19) 0.6217(2) 0.00438(19) Uani 1 2 d S . .
S13 S 0.8821(2) 0.8846(2) 0.8823(3) 0.00438(19) Uani 1 1 d . . .
S21 S 0.88394(18) 0.88217(18) 0.3819(3) 0.00388(19) Uani 1 1 d . . .
S22 S 0.8829(2) 0.6171(2) 0.1137(3) 0.00388(19) Uani 1 2 d S . .
S23 S 0.6163(2) 0.8837(2) 0.1202(3) 0.00388(19) Uani 1 2 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
Nb1 0.0022(3) 0.0026(3) 0.0062(4) 0.0002(2) -0.0012(2) -0.0003(3)
Nb2 0.0027(3) 0.0027(3) 0.0038(3) -0.00005(19) 0.00005(19) -0.0004(3)
Nb3 0.0036(3) 0.0036(3) 0.0049(3) -0.0002(2) 0.0002(2) 0.0002(4)
Ga 0.0015(6) 0.0015(6) 0.0069(12) 0.00002(11) -0.00002(11) -0.0003(4)
S11 0.0036(5) 0.0036(5) 0.0060(9) 0.00003(14) -0.00003(14) 0.0000(6)
S12 0.0036(5) 0.0036(5) 0.0060(9) 0.00003(14) -0.00003(14) 0.0000(6)
S13 0.0036(5) 0.0036(5) 0.0060(9) 0.00003(14) -0.00003(14) 0.0000(6)
S21 0.0033(7) 0.0037(7) 0.0046(11) -0.0014(4) -0.0012(4) 0.0008(6)
S22 0.0033(7) 0.0037(7) 0.0046(11) -0.0014(4) -0.0012(4) 0.0008(6)
S23 0.0033(7) 0.0037(7) 0.0046(11) -0.0014(4) -0.0012(4) 0.0008(6)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 S13 2.394(3) . ?
Nb1 S11 2.4198(19) . ?
Nb1 S12 2.424(2) . ?
Nb1 S21 2.6318(18) 4_756 ?
Nb1 S21 2.6573(19) 3_576 ?
Nb1 S21 2.662(3) . ?
Nb1 Nb2 2.9099(10) . ?
Nb1 Nb1 2.9734(17) 7_665 ?
Nb1 Nb3 3.0319(10) . ?
Nb2 S11 2.412(2) . ?
Nb2 S13 2.431(2) . ?
Nb2 S13 2.431(2) 7_665 ?
Nb2 S23 2.643(2) 4_756 ?
Nb2 S23 2.643(2) 3_566 ?
Nb2 S22 2.660(3) 1_556 ?
Nb2 Nb1 2.9099(10) 7_665 ?
Nb2 Nb3 3.0025(19) . ?
Nb3 S12 2.404(2) . ?
Nb3 S13 2.418(2) . ?
Nb3 S13 2.418(2) 7_665 ?
Nb3 S23 2.622(3) 1_556 ?
Nb3 S22 2.621(2) 3_576 ?
Nb3 S22 2.621(2) 4_656 ?
Nb3 Nb1 3.0318(10) 7_665 ?
Ga S21 2.296(2) . ?
Ga S21 2.296(2) 7_665 ?
Ga S23 2.303(2) . ?
Ga S22 2.304(2) . ?
S11 Nb1 2.4198(19) 7_665 ?
S12 Nb1 2.424(2) 7_665 ?
S21 Nb1 2.6318(18) 3_576 ?
S21 Nb1 2.6573(18) 4_756 ?
S22 Nb3 2.621(2) 4_756 ?
S22 Nb3 2.621(2) 3_566 ?
S22 Nb2 2.660(3) 1_554 ?
S23 Nb3 2.622(3) 1_554 ?
S23 Nb2 2.643(2) 3_576 ?
S23 Nb2 2.643(2) 4_656 ?

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
S13 Nb1 S11 104.81(6) . . ?
S13 Nb1 S12 100.48(6) . . ?
S11 Nb1 S12 102.61(10) . . ?
S13 Nb1 S21 89.26(12) . 4_756 ?
S11 Nb1 S21 89.36(6) . 4_756 ?
S12 Nb1 S21 161.93(6) . 4_756 ?
S13 Nb1 S21 87.77(11) . 3_576 ?
S11 Nb1 S21 161.69(7) . 3_576 ?
S12 Nb1 S21 87.77(5) . 3_576 ?
S21 Nb1 S21 77.35(8) 4_756 3_576 ?
S13 Nb1 S21 161.86(10) . . ?
S11 Nb1 S21 87.76(9) . . ?
S12 Nb1 S21 89.20(8) . . ?
S21 Nb1 S21 77.66(8) 4_756 . ?
S21 Nb1 S21 77.22(8) 3_576 . ?
S13 Nb1 Nb2 53.49(6) . . ?
S11 Nb1 Nb2 52.86(6) . . ?
S12 Nb1 Nb2 98.40(4) . . ?
S21 Nb1 Nb2 99.62(5) 4_756 . ?
S21 Nb1 Nb2 141.26(12) 3_576 . ?
S21 Nb1 Nb2 140.61(7) . . ?
S13 Nb1 Nb1 99.56(8) . 7_665 ?
S11 Nb1 Nb1 52.09(4) . 7_665 ?
S12 Nb1 Nb1 52.17(4) . 7_665 ?
S21 Nb1 Nb1 141.46(5) 4_756 7_665 ?
S21 Nb1 Nb1 139.93(5) 3_576 7_665 ?
S21 Nb1 Nb1 98.50(6) . 7_665 ?
Nb2 Nb1 Nb1 59.28(3) . 7_665 ?
S13 Nb1 Nb3 51.29(6) . . ?
S11 Nb1 Nb3 101.18(4) . . ?
S12 Nb1 Nb3 50.79(5) . . ?
S21 Nb1 Nb3 140.51(12) 4_756 . ?
S21 Nb1 Nb3 97.07(5) 3_576 . ?
S21 Nb1 Nb3 139.96(7) . . ?
Nb2 Nb1 Nb3 60.66(6) . . ?
Nb1 Nb1 Nb3 60.64(3) 7_665 . ?
S11 Nb2 S13 103.90(9) . . ?
S11 Nb2 S13 103.90(9) . 7_665 ?
S13 Nb2 S13 101.62(12) . 7_665 ?
S11 Nb2 S23 88.40(10) . 4_756 ?
S13 Nb2 S23 88.96(7) . 4_756 ?
S13 Nb2 S23 161.11(7) 7_665 4_756 ?
S11 Nb2 S23 88.40(10) . 3_566 ?
S13 Nb2 S23 161.11(7) . 3_566 ?
S13 Nb2 S23 88.96(7) 7_665 3_566 ?
S23 Nb2 S23 76.93(10) 4_756 3_566 ?
S11 Nb2 S22 161.21(11) . 1_556 ?
S13 Nb2 S22 87.75(11) . 1_556 ?
S13 Nb2 S22 87.76(11) 7_665 1_556 ?
S23 Nb2 S22 76.96(7) 4_756 1_556 ?
S23 Nb2 S22 76.96(7) 3_566 1_556 ?
S11 Nb2 Nb1 53.09(5) . 7_665 ?
S13 Nb2 Nb1 100.42(5) . 7_665 ?
S13 Nb2 Nb1 52.33(8) 7_665 7_665 ?
S23 Nb2 Nb1 141.47(10) 4_756 7_665 ?
S23 Nb2 Nb1 98.43(4) 3_566 7_665 ?
S22 Nb2 Nb1 140.06(7) 1_556 7_665 ?
S11 Nb2 Nb1 53.09(5) . . ?
S13 Nb2 Nb1 52.33(8) . . ?
S13 Nb2 Nb1 100.42(5) 7_665 . ?
S23 Nb2 Nb1 98.43(4) 4_756 . ?
S23 Nb2 Nb1 141.47(10) 3_566 . ?
S22 Nb2 Nb1 140.06(7) 1_556 . ?
Nb1 Nb2 Nb1 61.45(6) 7_665 . ?
S11 Nb2 Nb3 102.18(7) . . ?
S13 Nb2 Nb3 51.54(5) . . ?
S13 Nb2 Nb3 51.54(5) 7_665 . ?
S23 Nb2 Nb3 140.42(6) 4_756 . ?
S23 Nb2 Nb3 140.42(6) 3_566 . ?
S22 Nb2 Nb3 96.61(7) 1_556 . ?
Nb1 Nb2 Nb3 61.68(3) 7_665 . ?
Nb1 Nb2 Nb3 61.68(3) . . ?
S12 Nb3 S13 100.39(8) . . ?
S12 Nb3 S13 100.39(8) . 7_665 ?
S13 Nb3 S13 102.40(12) . 7_665 ?
S12 Nb3 S23 163.51(11) . 1_556 ?
S13 Nb3 S23 89.85(11) . 1_556 ?
S13 Nb3 S23 89.85(11) 7_665 1_556 ?
S12 Nb3 S22 89.28(10) . 3_576 ?
S13 Nb3 S22 88.62(7) . 3_576 ?
S13 Nb3 S22 163.64(6) 7_665 3_576 ?
S23 Nb3 S22 77.99(6) 1_556 3_576 ?
S12 Nb3 S22 89.28(10) . 4_656 ?
S13 Nb3 S22 163.64(6) . 4_656 ?
S13 Nb3 S22 88.62(7) 7_665 4_656 ?
S23 Nb3 S22 77.99(6) 1_556 4_656 ?
S22 Nb3 S22 78.26(10) 3_576 4_656 ?
S12 Nb3 Nb2 96.42(8) . . ?
S13 Nb3 Nb2 51.94(5) . . ?
S13 Nb3 Nb2 51.94(5) 7_665 . ?
S23 Nb3 Nb2 100.07(7) 1_556 . ?
S22 Nb3 Nb2 140.55(6) 3_576 . ?
S22 Nb3 Nb2 140.55(6) 4_656 . ?
S12 Nb3 Nb1 51.40(5) . . ?
S13 Nb3 Nb1 50.60(7) . . ?
S13 Nb3 Nb1 97.44(5) 7_665 . ?
S23 Nb3 Nb1 140.44(7) 1_556 . ?
S22 Nb3 Nb1 98.90(5) 3_576 . ?
S22 Nb3 Nb1 140.68(10) 4_656 . ?
Nb2 Nb3 Nb1 57.66(3) . . ?
S12 Nb3 Nb1 51.40(5) . 7_665 ?
S13 Nb3 Nb1 97.44(5) . 7_665 ?
S13 Nb3 Nb1 50.60(7) 7_665 7_665 ?
S23 Nb3 Nb1 140.44(7) 1_556 7_665 ?
S22 Nb3 Nb1 140.68(10) 3_576 7_665 ?
S22 Nb3 Nb1 98.90(5) 4_656 7_665 ?
Nb2 Nb3 Nb1 57.66(3) . 7_665 ?
Nb1 Nb3 Nb1 58.73(5) . 7_665 ?
S21 Ga S21 109.95(19) . 7_665 ?
S21 Ga S23 108.71(8) . . ?
S21 Ga S23 108.70(8) 7_665 . ?
S21 Ga S22 109.86(8) . . ?
S21 Ga S22 109.87(8) 7_665 . ?
S23 Ga S22 109.73(18) . . ?
Nb2 S11 Nb1 74.05(5) . . ?
Nb2 S11 Nb1 74.05(5) . 7_665 ?
Nb1 S11 Nb1 75.81(8) . 7_665 ?
Nb3 S12 Nb1 77.81(5) . . ?
Nb3 S12 Nb1 77.81(5) . 7_665 ?
Nb1 S12 Nb1 75.65(8) . 7_665 ?
Nb1 S13 Nb3 78.11(6) . . ?
Nb1 S13 Nb2 74.18(6) . . ?
Nb3 S13 Nb2 76.52(9) . . ?
Ga S21 Nb1 116.39(9) . 3_576 ?
Ga S21 Nb1 117.34(9) . 4_756 ?
Nb1 S21 Nb1 101.38(10) 3_576 4_756 ?
Ga S21 Nb1 116.53(14) . . ?
Nb1 S21 Nb1 101.60(8) 3_576 . ?
Nb1 S21 Nb1 100.94(8) 4_756 . ?
Ga S22 Nb3 116.82(7) . 4_756 ?
Ga S22 Nb3 116.81(7) . 3_566 ?
Nb3 S22 Nb3 100.58(12) 4_756 3_566 ?
Ga S22 Nb2 117.60(15) . 1_554 ?
Nb3 S22 Nb2 101.07(6) 4_756 1_554 ?
Nb3 S22 Nb2 101.07(6) 3_566 1_554 ?
Ga S23 Nb3 115.99(15) . 1_554 ?
Ga S23 Nb2 116.85(7) . 3_576 ?
Nb3 S23 Nb2 101.51(6) 1_554 3_576 ?
Ga S23 Nb2 116.86(7) . 4_656 ?
Nb3 S23 Nb2 101.51(6) 1_554 4_656 ?
Nb2 S23 Nb2 101.59(12) 3_576 4_656 ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        33.30
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         1.054
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.172