# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# 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_2111
_database_code_depnum_ccdc_archive 'CCDC 1985463'
loop_
_audit_author_name
_audit_author_address
'ruiqi Wang'
;Peking University
China
;
_audit_update_record             
;
2020-02-21 deposited with the CCDC.	2022-05-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ca2 O2 S3 Sb2'
_chemical_formula_weight         451.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.8616(7)
_cell_length_b                   4.0014(2)
_cell_length_c                   12.7811(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.313(4)
_cell_angle_gamma                90
_cell_volume                     747.78(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    2826
_cell_measurement_theta_min      5.2720
_cell_measurement_theta_max      30.5630

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.013
_exptl_crystal_F_000             824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    9.351
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3893
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.878
_diffrn_reflns_theta_max         30.498
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             995
_reflns_number_gt                969
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0114P)²+0.0699P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         995
_refine_ls_number_parameters     42
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0117
_refine_ls_R_factor_gt           0.0111
_refine_ls_wR_factor_ref         0.0259
_refine_ls_wR_factor_gt          0.0257
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.004
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.56554(2) 0.35092(3) 0.62702(2) 0.00626(5) Uani 1 1 d . . . . .
Ca1 Ca 0.69871(2) 0.90271(8) 0.83792(2) 0.00616(7) Uani 1 1 d . . . . .
S1 S 0.5000 -0.06966(14) 0.7500 0.00681(10) Uani 1 2 d S T P . .
S2 S 0.65424(3) -0.05856(10) 0.54120(3) 0.00824(8) Uani 1 1 d . . . . .
O1 O 0.67046(7) 0.4068(3) 0.74341(9) 0.0062(2) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.00540(7) 0.00704(7) 0.00583(7) -0.00033(3) -0.00033(4) 0.00060(3)
Ca1 0.00629(14) 0.00585(14) 0.00662(15) 0.00002(11) 0.00193(11) 0.00048(11)
S1 0.0059(2) 0.0063(2) 0.0086(2) 0.000 0.00242(18) 0.000
S2 0.01015(18) 0.00818(18) 0.00683(17) -0.00059(13) 0.00270(13) 0.00070(15)
O1 0.0051(5) 0.0070(5) 0.0058(5) 0.0002(4) -0.0006(4) 0.0003(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 O1 1.9657(11) . ?
Sb1 S2 2.4785(4) . ?
Sb1 S1 2.6076(4) . ?
Sb1 Ca1 3.4580(4) 4_646 ?
Sb1 Ca1 3.5340(4) 1_545 ?
Sb1 Ca1 3.7613(4) . ?
Ca1 O1 2.3220(12) . ?
Ca1 O1 2.3499(12) 1_565 ?
Ca1 O1 2.3632(11) 4_656 ?
Ca1 S2 2.8620(5) 6_566 ?
Ca1 S1 2.9678(4) 1_565 ?
Ca1 S2 3.0596(5) 4_656 ?
Ca1 S2 3.2560(5) 4_666 ?
Ca1 Sb1 3.4580(4) 4_656 ?
Ca1 Sb1 3.5340(4) 1_565 ?
Ca1 Ca1 3.5502(5) 4_646 ?
Ca1 Ca1 3.5502(5) 4_656 ?
S1 Sb1 2.6076(4) 2_656 ?
S1 Ca1 2.9678(4) 2_646 ?
S1 Ca1 2.9678(4) 1_545 ?
S2 Ca1 2.8621(5) 6_565 ?
S2 Ca1 3.0596(5) 4_646 ?
S2 Ca1 3.2560(5) 4_636 ?
O1 Ca1 2.3499(11) 1_545 ?
O1 Ca1 2.3632(11) 4_646 ?

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
O1 Sb1 S2 89.85(3) . . ?
O1 Sb1 S1 87.05(3) . . ?
S2 Sb1 S1 97.225(15) . . ?
O1 Sb1 Ca1 41.15(3) . 4_646 ?
S2 Sb1 Ca1 59.346(11) . 4_646 ?
S1 Sb1 Ca1 116.084(7) . 4_646 ?
O1 Sb1 Ca1 38.78(3) . 1_545 ?
S2 Sb1 Ca1 74.481(11) . 1_545 ?
S1 Sb1 Ca1 55.342(6) . 1_545 ?
Ca1 Sb1 Ca1 61.018(8) 4_646 1_545 ?
O1 Sb1 Ca1 31.41(3) . . ?
S2 Sb1 Ca1 116.864(11) . . ?
S1 Sb1 Ca1 98.758(9) . . ?
Ca1 Sb1 Ca1 58.734(7) 4_646 . ?
Ca1 Sb1 Ca1 66.442(7) 1_545 . ?
O1 Ca1 O1 117.85(5) . 1_565 ?
O1 Ca1 O1 82.15(4) . 4_656 ?
O1 Ca1 O1 81.57(4) 1_565 4_656 ?
O1 Ca1 S2 127.51(3) . 6_566 ?
O1 Ca1 S2 103.33(3) 1_565 6_566 ?
O1 Ca1 S2 137.70(3) 4_656 6_566 ?
O1 Ca1 S1 76.11(3) . 1_565 ?
O1 Ca1 S1 72.50(3) 1_565 1_565 ?
O1 Ca1 S1 132.41(3) 4_656 1_565 ?
S2 Ca1 S1 87.693(12) 6_566 1_565 ?
O1 Ca1 S2 78.08(3) . 4_656 ?
O1 Ca1 S2 145.40(3) 1_565 4_656 ?
O1 Ca1 S2 69.92(3) 4_656 4_656 ?
S2 Ca1 S2 86.169(14) 6_566 4_656 ?
S1 Ca1 S2 141.820(17) 1_565 4_656 ?
O1 Ca1 S2 148.89(3) . 4_666 ?
O1 Ca1 S2 73.66(3) 1_565 4_666 ?
O1 Ca1 S2 70.67(3) 4_656 4_666 ?
S2 Ca1 S2 70.697(14) 6_566 4_666 ?
S1 Ca1 S2 133.858(17) 1_565 4_666 ?
S2 Ca1 S2 78.561(12) 4_656 4_666 ?
O1 Ca1 Sb1 95.79(3) . 4_656 ?
O1 Ca1 Sb1 101.63(3) 1_565 4_656 ?
O1 Ca1 Sb1 33.18(3) 4_656 4_656 ?
S2 Ca1 Sb1 106.781(13) 6_566 4_656 ?
S1 Ca1 Sb1 165.412(11) 1_565 4_656 ?
S2 Ca1 Sb1 44.178(9) 4_656 4_656 ?
S2 Ca1 Sb1 53.111(9) 4_666 4_656 ?
O1 Ca1 Sb1 90.72(3) . 1_565 ?
O1 Ca1 Sb1 31.59(3) 1_565 1_565 ?
O1 Ca1 Sb1 93.07(3) 4_656 1_565 ?
S2 Ca1 Sb1 113.142(13) 6_566 1_565 ?
S1 Ca1 Sb1 46.280(9) 1_565 1_565 ?
S2 Ca1 Sb1 160.593(12) 4_656 1_565 ?
S2 Ca1 Sb1 105.226(12) 4_666 1_565 ?
Sb1 Ca1 Sb1 123.049(9) 4_656 1_565 ?
O1 Ca1 Ca1 41.17(3) . 4_646 ?
O1 Ca1 Ca1 102.46(3) 1_565 4_646 ?
O1 Ca1 Ca1 40.98(3) 4_656 4_646 ?
S2 Ca1 Ca1 153.198(15) 6_566 4_646 ?
S1 Ca1 Ca1 106.995(15) 1_565 4_646 ?
S2 Ca1 Ca1 68.336(11) 4_656 4_646 ?
S2 Ca1 Ca1 110.222(14) 4_666 4_646 ?
Sb1 Ca1 Ca1 60.547(10) 4_656 4_646 ?
Sb1 Ca1 Ca1 92.780(12) 1_565 4_646 ?
O1 Ca1 Ca1 102.15(3) . 4_656 ?
O1 Ca1 Ca1 41.27(3) 1_565 4_656 ?
O1 Ca1 Ca1 40.30(3) 4_656 4_656 ?
S2 Ca1 Ca1 130.314(12) 6_566 4_656 ?
S1 Ca1 Ca1 104.495(15) 1_565 4_656 ?
S2 Ca1 Ca1 108.105(15) 4_656 4_656 ?
S2 Ca1 Ca1 66.387(10) 4_666 4_656 ?
Sb1 Ca1 Ca1 64.903(10) 4_656 4_656 ?
Sb1 Ca1 Ca1 58.434(8) 1_565 4_656 ?
Ca1 Ca1 Ca1 68.602(11) 4_646 4_656 ?
O1 Ca1 Sb1 26.18(3) . . ?
O1 Ca1 Sb1 96.48(3) 1_565 . ?
O1 Ca1 Sb1 93.30(3) 4_656 . ?
S2 Ca1 Sb1 126.947(13) 6_566 . ?
S1 Ca1 Sb1 52.431(10) 1_565 . ?
S2 Ca1 Sb1 104.147(12) 4_656 . ?
S2 Ca1 Sb1 162.003(11) 4_666 . ?
Sb1 Ca1 Sb1 116.656(9) 4_656 . ?
Sb1 Ca1 Sb1 66.442(7) 1_565 . ?
Ca1 Ca1 Sb1 56.362(8) 4_646 . ?
Ca1 Ca1 Sb1 96.181(12) 4_656 . ?
Sb1 S1 Sb1 99.61(2) 2_656 . ?
Sb1 S1 Ca1 78.377(8) 2_656 2_646 ?
Sb1 S1 Ca1 104.451(11) . 2_646 ?
Sb1 S1 Ca1 104.452(11) 2_656 1_545 ?
Sb1 S1 Ca1 78.377(9) . 1_545 ?
Ca1 S1 Ca1 175.73(2) 2_646 1_545 ?
Sb1 S2 Ca1 119.029(17) . 6_565 ?
Sb1 S2 Ca1 76.476(12) . 4_646 ?
Ca1 S2 Ca1 93.832(14) 6_565 4_646 ?
Sb1 S2 Ca1 126.347(15) . 4_636 ?
Ca1 S2 Ca1 109.304(14) 6_565 4_636 ?
Ca1 S2 Ca1 78.562(12) 4_646 4_636 ?
Sb1 O1 Ca1 122.41(5) . . ?
Sb1 O1 Ca1 109.63(5) . 1_545 ?
Ca1 O1 Ca1 117.85(5) . 1_545 ?
Sb1 O1 Ca1 105.67(5) . 4_646 ?
Ca1 O1 Ca1 98.53(4) . 4_646 ?
Ca1 O1 Ca1 97.75(4) 1_545 4_646 ?


_refine_diff_density_max         0.390
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.120

_shelx_res_file                  
;

    2111.res created by SHELXL-2014/7


TITL 2111_a.res in C2/c
CELL 0.71073 14.8616 4.0014 12.7811 90 100.313 90
ZERR 4 0.0007 0.0002 0.0006 0 0.004 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC Ca O  S  Sb
UNIT 8  8  12  8
LIST 6
L.S. 30
ACTA 52
BOND $H
FMAP 2
PLAN 5
MORE -1
CONF
WGHT    0.011400    0.069900
FVAR       0.20752
SB1   4    0.565536    0.350915    0.627019    11.00000    0.00540    0.00704 =
         0.00583   -0.00033   -0.00033    0.00060
CA1   1    0.698709    0.902709    0.837916    11.00000    0.00629    0.00585 =
         0.00662    0.00002    0.00193    0.00048
S1    3    0.500000   -0.069657    0.750000    10.50000    0.00594    0.00633 =
         0.00856    0.00000    0.00242    0.00000
S2    3    0.654238   -0.058563    0.541202    11.00000    0.01015    0.00818 =
         0.00683   -0.00059    0.00270    0.00070
O1    2    0.670463    0.406786    0.743406    11.00000    0.00515    0.00700 =
         0.00583    0.00017   -0.00056    0.00034
HKLF 4

REM  2111_a.res in C2/c
REM R1 =  0.0111 for     969 Fo > 4sig(Fo)  and  0.0117 for all     995 data
REM     42 parameters refined using      0 restraints

END

WGHT      0.0114      0.0699

REM Highest difference peak  0.390,  deepest hole -0.507,  1-sigma level  0.120
Q1    1   0.6086  0.3666  0.7583  11.00000  0.05    0.39
Q2    1   0.6377  0.4608  0.7153  11.00000  0.05    0.37
Q3    1   0.4809  0.1863  0.5999  11.00000  0.05    0.36
Q4    1   0.6773  0.4569  0.6246  11.00000  0.05    0.34
Q5    1   0.5935  0.0762  0.4226  11.00000  0.05    0.34
;
_shelx_res_checksum              21065
####################################################################### 
# 
# 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_1602
_database_code_depnum_ccdc_archive 'CCDC 1985461'
loop_
_audit_author_name
_audit_author_address
'ruiqi Wang'
;Peking University
China
;
_audit_update_record             
;
2020-02-21 deposited with the CCDC.	2022-05-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ba4 O4 S6 Sb4'
_chemical_formula_weight         1292.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.0862(9)
_cell_length_b                   7.8909(5)
_cell_length_c                   7.1929(5)
_cell_angle_alpha                90
_cell_angle_beta                 113.867(5)
_cell_angle_gamma                90
_cell_volume                     834.95(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    1758
_cell_measurement_theta_min      4.7990
_cell_measurement_theta_max      30.3270

_exptl_crystal_description       bulk
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.142
_exptl_crystal_F_000             1112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    16.385
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2789
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.835
_diffrn_reflns_theta_max         30.326
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1052
_reflns_number_gt                989
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0135P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1052
_refine_ls_number_parameters     42
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0161
_refine_ls_R_factor_gt           0.0144
_refine_ls_wR_factor_ref         0.0328
_refine_ls_wR_factor_gt          0.0324
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 0.17774(2) 0.34732(2) 0.21999(3) 0.00649(6) Uani 1 1 d . . . . .
Sb1 Sb 0.06426(2) 0.79591(3) 0.07709(3) 0.00669(6) Uani 1 1 d . . . . .
S1 S 0.0000 0.57037(14) 0.2500 0.0078(2) Uani 1 2 d S T P . .
S2 S 0.35316(5) 0.45050(10) 0.11276(12) 0.00823(15) Uani 1 1 d . . . . .
O1 O 0.16854(15) 0.6668(3) 0.0901(3) 0.0077(4) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ba1 0.00709(10) 0.00600(10) 0.00675(10) 0.00065(7) 0.00320(8) 0.00047(6)
Sb1 0.00570(10) 0.00710(12) 0.00692(11) -0.00043(8) 0.00218(8) 0.00109(7)
S1 0.0091(5) 0.0065(5) 0.0096(5) 0.000 0.0056(4) 0.000
S2 0.0103(3) 0.0077(3) 0.0078(3) 0.0022(3) 0.0047(3) 0.0010(3)
O1 0.0071(10) 0.0066(11) 0.0095(11) -0.0003(9) 0.0037(9) 0.0011(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
Ba1 O1 2.672(2) . ?
Ba1 O1 2.697(2) 4_545 ?
Ba1 O1 2.727(2) 6_566 ?
Ba1 S2 3.2458(8) 7 ?
Ba1 S2 3.3139(7) . ?
Ba1 S1 3.4379(6) . ?
Ba1 S2 3.4617(8) 4_545 ?
Ba1 S2 3.4696(8) 6_566 ?
Ba1 S1 3.4934(4) 5_565 ?
Ba1 Sb1 3.7772(4) 5_565 ?
Ba1 Sb1 3.8232(4) 4_545 ?
Ba1 Sb1 3.8732(3) 6_566 ?
Sb1 O1 1.932(2) . ?
Sb1 S2 2.4148(8) 4 ?
Sb1 S1 2.6122(8) . ?
Sb1 Ba1 3.7771(4) 5_565 ?
Sb1 Ba1 3.8232(4) 4 ?
Sb1 Ba1 3.8732(3) 6_565 ?
S1 Sb1 2.6122(8) 2 ?
S1 Ba1 3.4379(6) 2 ?
S1 Ba1 3.4933(4) 6_566 ?
S1 Ba1 3.4933(4) 5_565 ?
S2 Sb1 2.4148(8) 4_545 ?
S2 Ba1 3.2458(8) 7 ?
S2 Ba1 3.4617(8) 4 ?
S2 Ba1 3.4696(8) 6_565 ?
O1 Ba1 2.697(2) 4 ?
O1 Ba1 2.727(2) 6_565 ?

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
O1 Ba1 O1 125.81(5) . 4_545 ?
O1 Ba1 O1 111.27(6) . 6_566 ?
O1 Ba1 O1 83.38(7) 4_545 6_566 ?
O1 Ba1 S2 117.06(5) . 7 ?
O1 Ba1 S2 80.02(5) 4_545 7 ?
O1 Ba1 S2 129.60(5) 6_566 7 ?
O1 Ba1 S2 67.58(5) . . ?
O1 Ba1 S2 63.59(5) 4_545 . ?
O1 Ba1 S2 128.67(5) 6_566 . ?
S2 Ba1 S2 84.09(2) 7 . ?
O1 Ba1 S1 66.99(5) . . ?
O1 Ba1 S1 148.62(5) 4_545 . ?
O1 Ba1 S1 65.46(5) 6_566 . ?
S2 Ba1 S1 122.264(18) 7 . ?
S2 Ba1 S1 134.19(2) . . ?
O1 Ba1 S2 168.41(5) . 4_545 ?
O1 Ba1 S2 65.00(5) 4_545 4_545 ?
O1 Ba1 S2 63.37(5) 6_566 4_545 ?
S2 Ba1 S2 66.463(7) 7 4_545 ?
S2 Ba1 S2 123.966(19) . 4_545 ?
S1 Ba1 S2 101.61(2) . 4_545 ?
O1 Ba1 S2 76.27(5) . 6_566 ?
O1 Ba1 S2 63.48(5) 4_545 6_566 ?
O1 Ba1 S2 64.63(5) 6_566 6_566 ?
S2 Ba1 S2 139.889(13) 7 6_566 ?
S2 Ba1 S2 65.667(14) . 6_566 ?
S1 Ba1 S2 97.848(17) . 6_566 ?
S2 Ba1 S2 108.470(16) 4_545 6_566 ?
O1 Ba1 S1 65.06(5) . 5_565 ?
O1 Ba1 S1 144.29(5) 4_545 5_565 ?
O1 Ba1 S1 127.28(5) 6_566 5_565 ?
S2 Ba1 S1 66.41(2) 7 5_565 ?
S2 Ba1 S1 99.769(16) . 5_565 ?
S1 Ba1 S1 65.778(11) . 5_565 ?
S2 Ba1 S1 109.15(2) 4_545 5_565 ?
S2 Ba1 S1 141.26(2) 6_566 5_565 ?
O1 Ba1 Sb1 100.71(5) . 5_565 ?
O1 Ba1 Sb1 130.71(5) 4_545 5_565 ?
O1 Ba1 Sb1 95.13(5) 6_566 5_565 ?
S2 Ba1 Sb1 63.313(14) 7 5_565 ?
S2 Ba1 Sb1 136.187(15) . 5_565 ?
S1 Ba1 Sb1 59.717(14) . 5_565 ?
S2 Ba1 Sb1 70.479(14) 4_545 5_565 ?
S2 Ba1 Sb1 155.609(13) 6_566 5_565 ?
S1 Ba1 Sb1 41.885(13) 5_565 5_565 ?
O1 Ba1 Sb1 97.56(5) . 4_545 ?
O1 Ba1 Sb1 28.31(5) 4_545 4_545 ?
O1 Ba1 Sb1 95.87(5) 6_566 4_545 ?
S2 Ba1 Sb1 91.343(15) 7 4_545 ?
S2 Ba1 Sb1 38.730(14) . 4_545 ?
S1 Ba1 Sb1 146.332(13) . 4_545 ?
S2 Ba1 Sb1 93.309(14) 4_545 4_545 ?
S2 Ba1 Sb1 48.573(13) 6_566 4_545 ?
S1 Ba1 Sb1 136.567(7) 5_565 4_545 ?
Sb1 Ba1 Sb1 153.553(6) 5_565 4_545 ?
O1 Ba1 Sb1 122.21(4) . 6_566 ?
O1 Ba1 Sb1 95.24(5) 4_545 6_566 ?
O1 Ba1 Sb1 27.70(5) 6_566 6_566 ?
S2 Ba1 Sb1 107.761(15) 7 6_566 ?
S2 Ba1 Sb1 154.191(15) . 6_566 ?
S1 Ba1 Sb1 58.710(14) . 6_566 ?
S2 Ba1 Sb1 48.169(13) 4_545 6_566 ?
S2 Ba1 Sb1 92.319(14) 6_566 6_566 ?
S1 Ba1 Sb1 105.973(8) 5_565 6_566 ?
Sb1 Ba1 Sb1 68.496(8) 5_565 6_566 ?
Sb1 Ba1 Sb1 116.484(7) 4_545 6_566 ?
O1 Sb1 S2 94.56(7) . 4 ?
O1 Sb1 S1 96.94(7) . . ?
S2 Sb1 S1 94.59(2) 4 . ?
O1 Sb1 Ba1 123.05(7) . 5_565 ?
S2 Sb1 Ba1 136.848(19) 4 5_565 ?
S1 Sb1 Ba1 63.233(6) . 5_565 ?
O1 Sb1 Ba1 41.45(7) . 4 ?
S2 Sb1 Ba1 59.159(18) 4 4 ?
S1 Sb1 Ba1 117.911(10) . 4 ?
Ba1 Sb1 Ba1 163.505(7) 5_565 4 ?
O1 Sb1 Ba1 41.00(7) . 6_565 ?
S2 Sb1 Ba1 121.966(19) 4 6_565 ?
S1 Sb1 Ba1 120.029(19) . 6_565 ?
Ba1 Sb1 Ba1 101.065(8) 5_565 6_565 ?
Ba1 Sb1 Ba1 63.517(7) 4 6_565 ?
O1 Sb1 Ba1 37.73(7) . . ?
S2 Sb1 Ba1 100.95(2) 4 . ?
S1 Sb1 Ba1 59.502(17) . . ?
Ba1 Sb1 Ba1 98.163(7) 5_565 . ?
Ba1 Sb1 Ba1 71.196(5) 4 . ?
Ba1 Sb1 Ba1 67.442(5) 6_565 . ?
Sb1 S1 Sb1 94.10(4) . 2 ?
Sb1 S1 Ba1 151.417(15) . 2 ?
Sb1 S1 Ba1 79.602(7) 2 2 ?
Sb1 S1 Ba1 79.601(6) . . ?
Sb1 S1 Ba1 151.416(15) 2 . ?
Ba1 S1 Ba1 118.41(3) 2 . ?
Sb1 S1 Ba1 90.427(18) . 6_566 ?
Sb1 S1 Ba1 74.881(14) 2 6_566 ?
Ba1 S1 Ba1 114.222(11) 2 6_566 ?
Ba1 S1 Ba1 77.297(8) . 6_566 ?
Sb1 S1 Ba1 74.882(14) . 5_565 ?
Sb1 S1 Ba1 90.427(18) 2 5_565 ?
Ba1 S1 Ba1 77.297(8) 2 5_565 ?
Ba1 S1 Ba1 114.222(11) . 5_565 ?
Ba1 S1 Ba1 158.57(4) 6_566 5_565 ?
Sb1 S2 Ba1 100.28(3) 4_545 7 ?
Sb1 S2 Ba1 82.11(2) 4_545 . ?
Ba1 S2 Ba1 95.91(2) 7 . ?
Sb1 S2 Ba1 103.80(3) 4_545 4 ?
Ba1 S2 Ba1 155.57(3) 7 4 ?
Ba1 S2 Ba1 83.442(17) . 4 ?
Sb1 S2 Ba1 161.20(3) 4_545 6_565 ?
Ba1 S2 Ba1 84.322(19) 7 6_565 ?
Ba1 S2 Ba1 79.276(17) . 6_565 ?
Ba1 S2 Ba1 71.531(16) 4 6_565 ?
Sb1 O1 Ba1 116.01(9) . . ?
Sb1 O1 Ba1 110.24(10) . 4 ?
Ba1 O1 Ba1 114.29(8) . 4 ?
Sb1 O1 Ba1 111.30(10) . 6_565 ?
Ba1 O1 Ba1 106.60(8) . 6_565 ?
Ba1 O1 Ba1 96.62(7) 4 6_565 ?

_refine_diff_density_max         0.730
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.196

_shelx_res_file                  
;

    1602.res created by SHELXL-2014/7


TITL 1 in C2/c
CELL 0.71073  16.08618   7.89089   7.19294  90.0000 113.8673  90.0000
ZERR    2.00   0.00089   0.00046   0.00045   0.0000   0.0053   0.0000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC O  S  Sb Ba
UNIT 8  12  8  8
LIST 4
L.S. 30
ACTA
BOND
FMAP 2
PLAN 20
WGHT    0.013500
FVAR       0.09486
MOLE 1
BA1   4    0.177744    0.347320    0.219990    11.00000    0.00709    0.00600 =
         0.00675    0.00065    0.00320    0.00047
SB1   3    0.064264    0.795910    0.077090    11.00000    0.00570    0.00710 =
         0.00692   -0.00043    0.00218    0.00109
S1    2    0.000000    0.570367    0.250000    10.50000    0.00914    0.00653 =
         0.00961    0.00000    0.00558    0.00000
S2    2    0.353161    0.450498    0.112755    11.00000    0.01026    0.00767 =
         0.00776    0.00219    0.00469    0.00097
O1    1    0.168543    0.666802    0.090059    11.00000    0.00710    0.00665 =
         0.00951   -0.00026    0.00368    0.00107
HKLF 4

REM  1 in C2/c
REM R1 =  0.0144 for     989 Fo > 4sig(Fo)  and  0.0161 for all    1052 data
REM     42 parameters refined using      0 restraints

END

WGHT      0.0135      0.0000

REM Highest difference peak  0.730,  deepest hole -0.963,  1-sigma level  0.196
Q1    1   0.1878  0.7210 -0.0425  11.00000  0.05    0.73
Q2    1   0.1519  0.7936  0.0831  11.00000  0.05    0.67
Q3    1   0.0645  0.8021  0.2016  11.00000  0.05    0.58
Q4    1   0.3183  0.2542  0.0683  11.00000  0.05    0.57
Q5    1  -0.0434  0.6112  0.0695  11.00000  0.05    0.57
Q6    1   0.0543  0.4032  0.0942  11.00000  0.05    0.56
Q7    1   0.1362  0.6472 -0.0585  11.00000  0.05    0.55
Q8    1  -0.0599  0.6650  0.1274  11.00000  0.05    0.54
Q9    1   0.2268  0.5786  0.2133  11.00000  0.05    0.53
Q10   1   0.0545  0.3420  0.0434  11.00000  0.05    0.53
Q11   1   0.0911  0.3204  0.1879  11.00000  0.05    0.52
Q12   1   0.0570  0.6853  0.2299  11.00000  0.05    0.52
Q13   1   0.2989  0.6416  0.0899  11.00000  0.05    0.51
Q14   1   0.2779  0.4538  0.1459  11.00000  0.05    0.51
Q15   1   0.3199  0.3535  0.2350  11.00000  0.05    0.51
Q16   1   0.1334  0.4399  0.2753  11.00000  0.05    0.50
Q17   1   0.1979  0.8087  0.1628  11.00000  0.05    0.49
Q18   1   0.2809  0.3206 -0.0662  11.00000  0.05    0.47
Q19   1   0.1946  0.5322  0.2976  11.00000  0.05    0.46
Q20   1   0.1161  0.3427 -0.0065  11.00000  0.05    0.46
;
_shelx_res_checksum              27952
