# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_257_0119p
_database_code_depnum_ccdc_archive 'CCDC 1968360'
loop_
_audit_author_name
_audit_author_address
'Hiromi Ota'
;Okayama University
Japan
;
_audit_update_record             
;
2019-11-27 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'O39 S W11'
_chemical_formula_moiety         'O39 S W11'
_chemical_formula_weight         2678.39
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      cubic
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'
_space_group_IT_number           229
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'x, z, y'
'y, x, z'
'z, y, x'
'x, -y, -z'
'z, -x, -y'
'y, -z, -x'
'x, -z, -y'
'y, -x, -z'
'z, -y, -x'
'-x, y, -z'
'-z, x, -y'
'-y, z, -x'
'-x, z, -y'
'-y, x, -z'
'-z, y, -x'
'-x, -y, z'
'-z, -x, y'
'-y, -z, x'
'-x, -z, y'
'-y, -x, z'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'x+1/2, z+1/2, y+1/2'
'y+1/2, x+1/2, z+1/2'
'z+1/2, y+1/2, x+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, -x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'x+1/2, -z+1/2, -y+1/2'
'y+1/2, -x+1/2, -z+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x+1/2, -z+1/2, y+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'-x, -z, -y'
'-y, -x, -z'
'-z, -y, -x'
'-x, y, z'
'-z, x, y'
'-y, z, x'
'-x, z, y'
'-y, x, z'
'-z, y, x'
'x, -y, z'
'z, -x, y'
'y, -z, x'
'x, -z, y'
'y, -x, z'
'z, -y, x'
'x, y, -z'
'z, x, -y'
'y, z, -x'
'x, z, -y'
'y, x, -z'
'z, y, -x'
'-x+1/2, -y+1/2, -z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, x+1/2, y+1/2'
'-y+1/2, z+1/2, x+1/2'
'-x+1/2, z+1/2, y+1/2'
'-y+1/2, x+1/2, z+1/2'
'-z+1/2, y+1/2, x+1/2'
'x+1/2, -y+1/2, z+1/2'
'z+1/2, -x+1/2, y+1/2'
'y+1/2, -z+1/2, x+1/2'
'x+1/2, -z+1/2, y+1/2'
'y+1/2, -x+1/2, z+1/2'
'z+1/2, -y+1/2, x+1/2'
'x+1/2, y+1/2, -z+1/2'
'z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, -x+1/2'
'x+1/2, z+1/2, -y+1/2'
'y+1/2, x+1/2, -z+1/2'
'z+1/2, y+1/2, -x+1/2'
#------------------------------------------------------------------------------
_cell_length_a                   17.565(10)
_cell_length_b                   17.565(10)
_cell_length_c                   17.565(10)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     5419(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6466
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      31.20
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2284.00
_exptl_absorpt_coefficient_mu    11.690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.203
_exptl_absorpt_correction_T_max  0.311

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.626
_diffrn_reflns_number            42711
_diffrn_reflns_av_R_equivalents  0.0931
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         3.281
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             649
_reflns_number_gt                645
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0931
_refine_ls_wR_factor_ref         0.2189
_refine_ls_wR_factor_gt          0.2188
_refine_ls_number_restraints     4
_refine_ls_number_reflns         649
_refine_ls_number_parameters     19
_refine_ls_goodness_of_fit_ref   1.282
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0631P)²+120.4308P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.64
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
W W -0.8490 6.8722
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
W1 W 0.64452(5) 0.64452(5) 0.500000 0.1118(9) Uani 0.9167 4 d S TU P . .
S1 S 0.500000 0.500000 0.500000 0.038(3) Uani 1 48 d S TU P . .
O1 O 0.7130(9) 0.7130(9) 0.500000 0.207(13) Uani 0.9167 4 d S TU P . .
O2 O 0.6823(9) 0.5699(8) 0.5699(8) 0.137(6) Uani 1 2 d S TU P . .
O3 O 0.5466(10) 0.5466(10) 0.5466(10) 0.057(8) Uani 0.5 6 d S TU P . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1 1.70(2) . ?
W1 O2 1.915(6) . ?
W1 O2 1.915(6) 67_556 ?
W1 O2 1.915(6) 68_556 ?
W1 O2 1.915(6) 2 ?
S1 O3 1.42(3) 49_666 ?
S1 O3 1.42(3) . ?
S1 O3 1.42(3) 67_556 ?
S1 O3 1.42(3) 7_566 ?
S1 O3 1.42(3) 55_655 ?
S1 O3 1.42(3) 13_656 ?
S1 O3 1.42(3) 61_565 ?
S1 O3 1.42(3) 19_665 ?
O3 O3 1.64(3) 67_556 ?
O3 O3 1.64(3) 55_655 ?
O3 O3 1.64(3) 61_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 W1 O2 103.8(5) . . ?
O1 W1 O2 103.8(5) . 67_556 ?
O2 W1 O2 79.8(11) . 67_556 ?
O1 W1 O2 103.8(5) . 68_556 ?
O2 W1 O2 152.4(10) . 68_556 ?
O2 W1 O2 93.7(11) 67_556 68_556 ?
O1 W1 O2 103.8(5) . 2 ?
O2 W1 O2 93.7(11) . 2 ?
O2 W1 O2 152.4(10) 67_556 2 ?
O2 W1 O2 79.8(11) 68_556 2 ?
O3 S1 O3 180.0(11) 49_666 . ?
O3 S1 O3 109.471(4) 49_666 67_556 ?
O3 S1 O3 70.529(1) . 67_556 ?
O3 S1 O3 70.529(2) 49_666 7_566 ?
O3 S1 O3 109.471(11) . 7_566 ?
O3 S1 O3 70.529(1) 67_556 7_566 ?
O3 S1 O3 109.471(1) 49_666 55_655 ?
O3 S1 O3 70.529(3) . 55_655 ?
O3 S1 O3 109.471(4) 67_556 55_655 ?
O3 S1 O3 180.0 7_566 55_655 ?
O3 S1 O3 70.529(5) 49_666 13_656 ?
O3 S1 O3 109.471(5) . 13_656 ?
O3 S1 O3 70.529(2) 67_556 13_656 ?
O3 S1 O3 109.5 7_566 13_656 ?
O3 S1 O3 70.529(5) 55_655 13_656 ?
O3 S1 O3 109.471(1) 49_666 61_565 ?
O3 S1 O3 70.529(1) . 61_565 ?
O3 S1 O3 109.471(10) 67_556 61_565 ?
O3 S1 O3 70.529(3) 7_566 61_565 ?
O3 S1 O3 109.471(1) 55_655 61_565 ?
O3 S1 O3 180.0(11) 13_656 61_565 ?
O3 S1 O3 70.529(9) 49_666 19_665 ?
O3 S1 O3 109.471(1) . 19_665 ?
O3 S1 O3 180.0(11) 67_556 19_665 ?
O3 S1 O3 109.5 7_566 19_665 ?
O3 S1 O3 70.529(9) 55_655 19_665 ?
O3 S1 O3 109.471(2) 13_656 19_665 ?
O3 S1 O3 70.529(8) 61_565 19_665 ?
W1 O2 W1 139.2(9) 3 . ?
S1 O3 O3 54.736(1) . 67_556 ?
S1 O3 O3 54.7 . 55_655 ?
O3 O3 O3 90.000(3) 67_556 55_655 ?
S1 O3 O3 54.7 . 61_565 ?
O3 O3 O3 90.0 67_556 61_565 ?
O3 O3 O3 90.000(3) 55_655 61_565 ?

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
O3 S1 O3 O3 60.000(3) 7_566 . . 67_556 ?
O3 S1 O3 O3 -120.000(3) 55_655 . . 67_556 ?
O3 S1 O3 O3 -60.000(3) 13_656 . . 67_556 ?
O3 S1 O3 O3 120.000(2) 61_565 . . 67_556 ?
O3 S1 O3 O3 180.000(0) 19_665 . . 67_556 ?
O3 S1 O3 O3 120.000(1) 67_556 . . 55_655 ?
O3 S1 O3 O3 180.000(0) 7_566 . . 55_655 ?
O3 S1 O3 O3 60.000(2) 13_656 . . 55_655 ?
O3 S1 O3 O3 -120.000(2) 61_565 . . 55_655 ?
O3 S1 O3 O3 -60.000(1) 19_665 . . 55_655 ?
O3 S1 O3 O3 -120.000(2) 67_556 . . 61_565 ?
O3 S1 O3 O3 -60.000(3) 7_566 . . 61_565 ?
O3 S1 O3 O3 120.000(4) 55_655 . . 61_565 ?
O3 S1 O3 O3 180.000(2) 13_656 . . 61_565 ?
O3 S1 O3 O3 60.000(2) 19_665 . . 61_565 ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_1209a
_database_code_depnum_ccdc_archive 'CCDC 1968361'
loop_
_audit_author_name
_audit_author_address
'Hiromi Ota'
;Okayama University
Japan
;
_audit_update_record             
;
2019-11-27 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'Ni O39 S W11'
_chemical_formula_moiety         'Ni O39 S W11'
_chemical_formula_weight         2737.09
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      cubic
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'
_space_group_IT_number           229
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'x, z, y'
'y, x, z'
'z, y, x'
'x, -y, -z'
'z, -x, -y'
'y, -z, -x'
'x, -z, -y'
'y, -x, -z'
'z, -y, -x'
'-x, y, -z'
'-z, x, -y'
'-y, z, -x'
'-x, z, -y'
'-y, x, -z'
'-z, y, -x'
'-x, -y, z'
'-z, -x, y'
'-y, -z, x'
'-x, -z, y'
'-y, -x, z'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'x+1/2, z+1/2, y+1/2'
'y+1/2, x+1/2, z+1/2'
'z+1/2, y+1/2, x+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, -x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'x+1/2, -z+1/2, -y+1/2'
'y+1/2, -x+1/2, -z+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x+1/2, -z+1/2, y+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'-x, -z, -y'
'-y, -x, -z'
'-z, -y, -x'
'-x, y, z'
'-z, x, y'
'-y, z, x'
'-x, z, y'
'-y, x, z'
'-z, y, x'
'x, -y, z'
'z, -x, y'
'y, -z, x'
'x, -z, y'
'y, -x, z'
'z, -y, x'
'x, y, -z'
'z, x, -y'
'y, z, -x'
'x, z, -y'
'y, x, -z'
'z, y, -x'
'-x+1/2, -y+1/2, -z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, x+1/2, y+1/2'
'-y+1/2, z+1/2, x+1/2'
'-x+1/2, z+1/2, y+1/2'
'-y+1/2, x+1/2, z+1/2'
'-z+1/2, y+1/2, x+1/2'
'x+1/2, -y+1/2, z+1/2'
'z+1/2, -x+1/2, y+1/2'
'y+1/2, -z+1/2, x+1/2'
'x+1/2, -z+1/2, y+1/2'
'y+1/2, -x+1/2, z+1/2'
'z+1/2, -y+1/2, x+1/2'
'x+1/2, y+1/2, -z+1/2'
'z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, -x+1/2'
'x+1/2, z+1/2, -y+1/2'
'y+1/2, x+1/2, -z+1/2'
'z+1/2, y+1/2, -x+1/2'
#------------------------------------------------------------------------------
_cell_length_a                   17.747(14)
_cell_length_b                   17.747(14)
_cell_length_c                   17.747(14)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     5590(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7694
_cell_measurement_theta_min      3.20
_cell_measurement_theta_max      27.50
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2340.00
_exptl_absorpt_coefficient_mu    11.498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.265
_exptl_absorpt_correction_T_max  0.317

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.111
_diffrn_reflns_number            43725
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         3.247
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             668
_reflns_number_gt                661
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1151
_refine_ls_wR_factor_gt          0.1147
_refine_ls_number_restraints     0
_refine_ls_number_reflns         668
_refine_ls_number_parameters     19
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0412P)²+86.4902P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.85
_refine_diff_density_min         -1.18
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
W W -0.8490 6.8722
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
W1 W 0.64401(2) 0.64401(2) 0.500000 0.0631(3) Uani 0.9165 4 d S T P . .
Ni1 Ni 0.64401(2) 0.64401(2) 0.500000 0.0631(3) Uani 0.0833 4 d S T P . .
S1 S 0.500000 0.500000 0.500000 0.0303(18) Uani 1 48 d S T P . .
O1 O 0.7118(5) 0.7118(5) 0.500000 0.105(5) Uani 0.9167 4 d S T P . .
O2 O 0.6789(6) 0.5733(4) 0.5733(4) 0.093(3) Uani 1 2 d S T P . .
O3 O 0.5488(6) 0.5488(6) 0.5488(6) 0.033(4) Uani 0.5 6 d S T P . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1 1.702(12) . ?
W1 O2 1.911(4) . ?
W1 O2 1.911(4) 68_556 ?
W1 O2 1.911(4) 67_556 ?
W1 O2 1.911(4) 2 ?
S1 O3 1.500(19) . ?
S1 O3 1.500(19) 49_666 ?
S1 O3 1.500(19) 67_556 ?
S1 O3 1.500(19) 7_566 ?
S1 O3 1.500(19) 55_655 ?
S1 O3 1.500(19) 13_656 ?
S1 O3 1.500(19) 61_565 ?
S1 O3 1.500(19) 19_665 ?
O3 O3 1.73(2) 67_556 ?
O3 O3 1.73(2) 55_655 ?
O3 O3 1.73(2) 61_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 W1 O2 103.6(3) . . ?
O1 W1 O2 103.6(3) . 68_556 ?
O2 W1 O2 152.8(6) . 68_556 ?
O1 W1 O2 103.6(3) . 67_556 ?
O2 W1 O2 85.8(6) . 67_556 ?
O2 W1 O2 87.9(5) 68_556 67_556 ?
O1 W1 O2 103.6(3) . 2 ?
O2 W1 O2 87.9(5) . 2 ?
O2 W1 O2 85.8(6) 68_556 2 ?
O2 W1 O2 152.8(6) 67_556 2 ?
O3 S1 O3 180.0(7) . 49_666 ?
O3 S1 O3 70.5 . 67_556 ?
O3 S1 O3 109.471(3) 49_666 67_556 ?
O3 S1 O3 109.471(6) . 7_566 ?
O3 S1 O3 70.529(2) 49_666 7_566 ?
O3 S1 O3 70.529(1) 67_556 7_566 ?
O3 S1 O3 70.529(2) . 55_655 ?
O3 S1 O3 109.5 49_666 55_655 ?
O3 S1 O3 109.471(2) 67_556 55_655 ?
O3 S1 O3 180.0 7_566 55_655 ?
O3 S1 O3 109.471(3) . 13_656 ?
O3 S1 O3 70.529(3) 49_666 13_656 ?
O3 S1 O3 70.529(2) 67_556 13_656 ?
O3 S1 O3 109.471(1) 7_566 13_656 ?
O3 S1 O3 70.529(2) 55_655 13_656 ?
O3 S1 O3 70.5 . 61_565 ?
O3 S1 O3 109.471(1) 49_666 61_565 ?
O3 S1 O3 109.471(6) 67_556 61_565 ?
O3 S1 O3 70.529(1) 7_566 61_565 ?
O3 S1 O3 109.471(1) 55_655 61_565 ?
O3 S1 O3 180.0(7) 13_656 61_565 ?
O3 S1 O3 109.5 . 19_665 ?
O3 S1 O3 70.529(6) 49_666 19_665 ?
O3 S1 O3 180.0(7) 67_556 19_665 ?
O3 S1 O3 109.5 7_566 19_665 ?
O3 S1 O3 70.529(5) 55_655 19_665 ?
O3 S1 O3 109.471(2) 13_656 19_665 ?
O3 S1 O3 70.529(4) 61_565 19_665 ?
W1 O2 W1 142.1(6) . 3 ?
S1 O3 O3 54.738(1) . 67_556 ?
S1 O3 O3 54.7 . 55_655 ?
O3 O3 O3 90.003(2) 67_556 55_655 ?
S1 O3 O3 54.7 . 61_565 ?
O3 O3 O3 90.003(2) 67_556 61_565 ?
O3 O3 O3 90.0 55_655 61_565 ?

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
O3 S1 O3 O3 60.000(2) 7_566 . . 67_556 ?
O3 S1 O3 O3 -120.000(2) 55_655 . . 67_556 ?
O3 S1 O3 O3 -60.000(1) 13_656 . . 67_556 ?
O3 S1 O3 O3 120.000(2) 61_565 . . 67_556 ?
O3 S1 O3 O3 180.000(1) 19_665 . . 67_556 ?
O3 S1 O3 O3 120.000(1) 67_556 . . 55_655 ?
O3 S1 O3 O3 180.000(1) 7_566 . . 55_655 ?
O3 S1 O3 O3 60.000(1) 13_656 . . 55_655 ?
O3 S1 O3 O3 -120.000(1) 61_565 . . 55_655 ?
O3 S1 O3 O3 -60.000(0) 19_665 . . 55_655 ?
O3 S1 O3 O3 -120.000(1) 67_556 . . 61_565 ?
O3 S1 O3 O3 -60.000(2) 7_566 . . 61_565 ?
O3 S1 O3 O3 120.000(2) 55_655 . . 61_565 ?
O3 S1 O3 O3 180.000(1) 13_656 . . 61_565 ?
O3 S1 O3 O3 60.000(1) 19_665 . . 61_565 ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_1210a
_database_code_depnum_ccdc_archive 'CCDC 1968486'
loop_
_audit_author_name
_audit_author_address
'Hiromi Ota'
;Okayama University
Japan
;
_audit_update_record             
;
2019-11-27 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'Cu O39 S W11'
_chemical_formula_moiety         'Cu O39 S W11'
_chemical_formula_weight         2741.93
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      cubic
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'
_space_group_IT_number           229
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'x, z, y'
'y, x, z'
'z, y, x'
'x, -y, -z'
'z, -x, -y'
'y, -z, -x'
'x, -z, -y'
'y, -x, -z'
'z, -y, -x'
'-x, y, -z'
'-z, x, -y'
'-y, z, -x'
'-x, z, -y'
'-y, x, -z'
'-z, y, -x'
'-x, -y, z'
'-z, -x, y'
'-y, -z, x'
'-x, -z, y'
'-y, -x, z'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'x+1/2, z+1/2, y+1/2'
'y+1/2, x+1/2, z+1/2'
'z+1/2, y+1/2, x+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, -x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'x+1/2, -z+1/2, -y+1/2'
'y+1/2, -x+1/2, -z+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x+1/2, -z+1/2, y+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'-x, -z, -y'
'-y, -x, -z'
'-z, -y, -x'
'-x, y, z'
'-z, x, y'
'-y, z, x'
'-x, z, y'
'-y, x, z'
'-z, y, x'
'x, -y, z'
'z, -x, y'
'y, -z, x'
'x, -z, y'
'y, -x, z'
'z, -y, x'
'x, y, -z'
'z, x, -y'
'y, z, -x'
'x, z, -y'
'y, x, -z'
'z, y, -x'
'-x+1/2, -y+1/2, -z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, x+1/2, y+1/2'
'-y+1/2, z+1/2, x+1/2'
'-x+1/2, z+1/2, y+1/2'
'-y+1/2, x+1/2, z+1/2'
'-z+1/2, y+1/2, x+1/2'
'x+1/2, -y+1/2, z+1/2'
'z+1/2, -x+1/2, y+1/2'
'y+1/2, -z+1/2, x+1/2'
'x+1/2, -z+1/2, y+1/2'
'y+1/2, -x+1/2, z+1/2'
'z+1/2, -y+1/2, x+1/2'
'x+1/2, y+1/2, -z+1/2'
'z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, -x+1/2'
'x+1/2, z+1/2, -y+1/2'
'y+1/2, x+1/2, -z+1/2'
'z+1/2, y+1/2, -x+1/2'
#------------------------------------------------------------------------------
_cell_length_a                   17.805(14)
_cell_length_b                   17.805(14)
_cell_length_c                   17.805(14)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     5645(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7681
_cell_measurement_theta_min      3.20
_cell_measurement_theta_max      27.50
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2342.00
_exptl_absorpt_coefficient_mu    11.408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.261
_exptl_absorpt_correction_T_max  0.320

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.111
_diffrn_reflns_number            42660
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_min         3.236
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             675
_reflns_number_gt                659
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0866
_refine_ls_wR_factor_gt          0.0859
_refine_ls_number_restraints     0
_refine_ls_number_reflns         675
_refine_ls_number_parameters     19
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0378P)²+48.5844P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.96
_refine_diff_density_min         -0.75
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
W W -0.8490 6.8722
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
W1 W 0.64375(2) 0.64375(2) 0.500000 0.0603(2) Uani 0.9165 4 d S T P . .
Cu1 Cu 0.64375(2) 0.64375(2) 0.500000 0.0603(2) Uani 0.0833 4 d S T P . .
S1 S 0.500000 0.500000 0.500000 0.0229(12) Uani 1 48 d S T P . .
O1 O 0.7125(4) 0.7125(4) 0.500000 0.109(4) Uani 0.9167 4 d S T P . .
O2 O 0.6792(4) 0.5737(3) 0.5737(3) 0.092(2) Uani 1 2 d S T P . .
O3 O 0.5491(4) 0.5491(4) 0.5491(4) 0.040(3) Uani 0.5 6 d S T P . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1 1.730(10) . ?
W1 O2 1.917(3) . ?
W1 O2 1.917(3) 68_556 ?
W1 O2 1.917(3) 67_556 ?
W1 O2 1.917(3) 2 ?
S1 O3 1.514(13) 49_666 ?
S1 O3 1.514(13) 67_556 ?
S1 O3 1.514(13) 19_665 ?
S1 O3 1.514(13) 7_566 ?
S1 O3 1.514(13) 55_655 ?
S1 O3 1.514(13) 13_656 ?
S1 O3 1.514(13) 61_565 ?
S1 O3 1.514(13) . ?
O3 O3 1.748(15) 67_556 ?
O3 O3 1.748(15) 55_655 ?
O3 O3 1.748(15) 61_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 W1 O2 103.1(2) . . ?
O1 W1 O2 103.1(2) . 68_556 ?
O2 W1 O2 153.7(4) . 68_556 ?
O1 W1 O2 103.1(2) . 67_556 ?
O2 W1 O2 86.4(4) . 67_556 ?
O2 W1 O2 87.7(4) 68_556 67_556 ?
O1 W1 O2 103.1(2) . 2 ?
O2 W1 O2 87.7(4) . 2 ?
O2 W1 O2 86.4(4) 68_556 2 ?
O2 W1 O2 153.7(4) 67_556 2 ?
O3 S1 O3 109.471(2) 49_666 67_556 ?
O3 S1 O3 70.529(4) 49_666 19_665 ?
O3 S1 O3 180.0(5) 67_556 19_665 ?
O3 S1 O3 70.529(1) 49_666 7_566 ?
O3 S1 O3 70.5 67_556 7_566 ?
O3 S1 O3 109.5 19_665 7_566 ?
O3 S1 O3 109.5 49_666 55_655 ?
O3 S1 O3 109.471(1) 67_556 55_655 ?
O3 S1 O3 70.529(1) 19_665 55_655 ?
O3 S1 O3 180.0 7_566 55_655 ?
O3 S1 O3 70.529(2) 49_666 13_656 ?
O3 S1 O3 70.529(1) 67_556 13_656 ?
O3 S1 O3 109.5 19_665 13_656 ?
O3 S1 O3 109.5 7_566 13_656 ?
O3 S1 O3 70.529(2) 55_655 13_656 ?
O3 S1 O3 109.5 49_666 61_565 ?
O3 S1 O3 109.471(4) 67_556 61_565 ?
O3 S1 O3 70.529(1) 19_665 61_565 ?
O3 S1 O3 70.529(1) 7_566 61_565 ?
O3 S1 O3 109.5 55_655 61_565 ?
O3 S1 O3 180.0(5) 13_656 61_565 ?
O3 S1 O3 180.0(5) 49_666 . ?
O3 S1 O3 70.5 67_556 . ?
O3 S1 O3 109.471(1) 19_665 . ?
O3 S1 O3 109.471(4) 7_566 . ?
O3 S1 O3 70.5 55_655 . ?
O3 S1 O3 109.471(3) 13_656 . ?
O3 S1 O3 70.5 61_565 . ?
W1 O2 W1 141.5(4) 3 . ?
S1 O3 O3 54.734(1) . 67_556 ?
S1 O3 O3 54.7 . 55_655 ?
O3 O3 O3 89.998(1) 67_556 55_655 ?
S1 O3 O3 54.7 . 61_565 ?
O3 O3 O3 90.0 67_556 61_565 ?
O3 O3 O3 89.998(1) 55_655 61_565 ?

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
O3 S1 O3 O3 180.000(0) 19_665 . . 67_556 ?
O3 S1 O3 O3 60.000(1) 7_566 . . 67_556 ?
O3 S1 O3 O3 -120.000(1) 55_655 . . 67_556 ?
O3 S1 O3 O3 -60.000(1) 13_656 . . 67_556 ?
O3 S1 O3 O3 120.000(1) 61_565 . . 67_556 ?
O3 S1 O3 O3 120.000(0) 67_556 . . 55_655 ?
O3 S1 O3 O3 -60.000(0) 19_665 . . 55_655 ?
O3 S1 O3 O3 180.000(0) 7_566 . . 55_655 ?
O3 S1 O3 O3 60.000(1) 13_656 . . 55_655 ?
O3 S1 O3 O3 -120.000(1) 61_565 . . 55_655 ?
O3 S1 O3 O3 -120.000(1) 67_556 . . 61_565 ?
O3 S1 O3 O3 60.000(1) 19_665 . . 61_565 ?
O3 S1 O3 O3 -60.000(1) 7_566 . . 61_565 ?
O3 S1 O3 O3 120.000(1) 55_655 . . 61_565 ?
O3 S1 O3 O3 180.000(1) 13_656 . . 61_565 ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_1210a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1968484'
loop_
_audit_author_name
_audit_author_address
'Hiromi Ota'
;Okayama University
Japan
;
_audit_update_record             
;
2019-11-27 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'Co O39 S W11'
_chemical_formula_moiety         'Co O39 S W11'
_chemical_formula_weight         2737.32
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      cubic
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'
_space_group_IT_number           229
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'x, z, y'
'y, x, z'
'z, y, x'
'x, -y, -z'
'z, -x, -y'
'y, -z, -x'
'x, -z, -y'
'y, -x, -z'
'z, -y, -x'
'-x, y, -z'
'-z, x, -y'
'-y, z, -x'
'-x, z, -y'
'-y, x, -z'
'-z, y, -x'
'-x, -y, z'
'-z, -x, y'
'-y, -z, x'
'-x, -z, y'
'-y, -x, z'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'x+1/2, z+1/2, y+1/2'
'y+1/2, x+1/2, z+1/2'
'z+1/2, y+1/2, x+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, -x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'x+1/2, -z+1/2, -y+1/2'
'y+1/2, -x+1/2, -z+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x+1/2, -z+1/2, y+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'-x, -z, -y'
'-y, -x, -z'
'-z, -y, -x'
'-x, y, z'
'-z, x, y'
'-y, z, x'
'-x, z, y'
'-y, x, z'
'-z, y, x'
'x, -y, z'
'z, -x, y'
'y, -z, x'
'x, -z, y'
'y, -x, z'
'z, -y, x'
'x, y, -z'
'z, x, -y'
'y, z, -x'
'x, z, -y'
'y, x, -z'
'z, y, -x'
'-x+1/2, -y+1/2, -z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, x+1/2, y+1/2'
'-y+1/2, z+1/2, x+1/2'
'-x+1/2, z+1/2, y+1/2'
'-y+1/2, x+1/2, z+1/2'
'-z+1/2, y+1/2, x+1/2'
'x+1/2, -y+1/2, z+1/2'
'z+1/2, -x+1/2, y+1/2'
'y+1/2, -z+1/2, x+1/2'
'x+1/2, -z+1/2, y+1/2'
'y+1/2, -x+1/2, z+1/2'
'z+1/2, -y+1/2, x+1/2'
'x+1/2, y+1/2, -z+1/2'
'z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, -x+1/2'
'x+1/2, z+1/2, -y+1/2'
'y+1/2, x+1/2, -z+1/2'
'z+1/2, y+1/2, -x+1/2'
#------------------------------------------------------------------------------
_cell_length_a                   17.854(14)
_cell_length_b                   17.854(14)
_cell_length_c                   17.854(14)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     5691(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8277
_cell_measurement_theta_min      3.20
_cell_measurement_theta_max      27.40
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2338.00
_exptl_absorpt_coefficient_mu    11.273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.363
_exptl_absorpt_correction_T_max  0.508

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.111
_diffrn_reflns_number            43956
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_theta_max         27.329
_diffrn_reflns_theta_min         3.227
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             669
_reflns_number_gt                665
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1056
_refine_ls_wR_factor_gt          0.1054
_refine_ls_number_restraints     0
_refine_ls_number_reflns         669
_refine_ls_number_parameters     19
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0471P)²+57.4389P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.69
_refine_diff_density_min         -1.23
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Co 0.3494 0.9721
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
W W -0.8490 6.8722
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
W1 W 0.64381(2) 0.64381(2) 0.500000 0.0600(3) Uani 0.9165 4 d S T P . .
Co1 Co 0.64381(2) 0.64381(2) 0.500000 0.0600(3) Uani 0.0833 4 d S T P . .
S1 S 0.500000 0.500000 0.500000 0.0287(15) Uani 1 48 d S T P . .
O1 O 0.7117(4) 0.7117(4) 0.500000 0.101(4) Uani 0.9167 4 d S T P . .
O2 O 0.6782(5) 0.5736(3) 0.5736(3) 0.091(3) Uani 1 2 d S T P . .
O3 O 0.5489(5) 0.5489(5) 0.5489(5) 0.031(3) Uani 0.5 6 d S T P . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1 1.714(11) . ?
W1 O2 1.917(3) . ?
W1 O2 1.917(3) 68_556 ?
W1 O2 1.917(3) 67_556 ?
W1 O2 1.917(3) 2 ?
S1 O3 1.513(16) 49_666 ?
S1 O3 1.513(16) 67_556 ?
S1 O3 1.513(16) 19_665 ?
S1 O3 1.513(16) 7_566 ?
S1 O3 1.513(16) 55_655 ?
S1 O3 1.513(16) 13_656 ?
S1 O3 1.513(16) 61_565 ?
S1 O3 1.513(16) . ?
O3 O3 1.747(19) 67_556 ?
O3 O3 1.747(19) 55_655 ?
O3 O3 1.747(19) 61_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 W1 O2 103.6(3) . . ?
O1 W1 O2 103.6(3) . 68_556 ?
O2 W1 O2 152.8(6) . 68_556 ?
O1 W1 O2 103.6(3) . 67_556 ?
O2 W1 O2 86.6(5) . 67_556 ?
O2 W1 O2 87.1(5) 68_556 67_556 ?
O1 W1 O2 103.6(3) . 2 ?
O2 W1 O2 87.1(5) . 2 ?
O2 W1 O2 86.6(5) 68_556 2 ?
O2 W1 O2 152.8(6) 67_556 2 ?
O3 S1 O3 109.471(2) 49_666 67_556 ?
O3 S1 O3 70.529(5) 49_666 19_665 ?
O3 S1 O3 180.0(6) 67_556 19_665 ?
O3 S1 O3 70.529(1) 49_666 7_566 ?
O3 S1 O3 70.5 67_556 7_566 ?
O3 S1 O3 109.5 19_665 7_566 ?
O3 S1 O3 109.5 49_666 55_655 ?
O3 S1 O3 109.471(2) 67_556 55_655 ?
O3 S1 O3 70.529(2) 19_665 55_655 ?
O3 S1 O3 180.0(6) 7_566 55_655 ?
O3 S1 O3 70.529(3) 49_666 13_656 ?
O3 S1 O3 70.529(1) 67_556 13_656 ?
O3 S1 O3 109.471(1) 19_665 13_656 ?
O3 S1 O3 109.471(1) 7_566 13_656 ?
O3 S1 O3 70.529(2) 55_655 13_656 ?
O3 S1 O3 109.5 49_666 61_565 ?
O3 S1 O3 109.471(5) 67_556 61_565 ?
O3 S1 O3 70.529(1) 19_665 61_565 ?
O3 S1 O3 70.529(2) 7_566 61_565 ?
O3 S1 O3 109.471(1) 55_655 61_565 ?
O3 S1 O3 180.0(6) 13_656 61_565 ?
O3 S1 O3 180.0(6) 49_666 . ?
O3 S1 O3 70.5 67_556 . ?
O3 S1 O3 109.471(2) 19_665 . ?
O3 S1 O3 109.471(6) 7_566 . ?
O3 S1 O3 70.529(1) 55_655 . ?
O3 S1 O3 109.471(4) 13_656 . ?
O3 S1 O3 70.5 61_565 . ?
W1 O2 W1 142.5(5) 3 . ?
S1 O3 O3 54.735(1) . 67_556 ?
S1 O3 O3 54.735(1) . 55_655 ?
O3 O3 O3 89.999(2) 67_556 55_655 ?
S1 O3 O3 54.735(1) . 61_565 ?
O3 O3 O3 89.999(1) 67_556 61_565 ?
O3 O3 O3 89.999(2) 55_655 61_565 ?

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
O3 S1 O3 O3 180.000(0) 19_665 . . 67_556 ?
O3 S1 O3 O3 60.000(2) 7_566 . . 67_556 ?
O3 S1 O3 O3 -120.000(2) 55_655 . . 67_556 ?
O3 S1 O3 O3 -60.000(1) 13_656 . . 67_556 ?
O3 S1 O3 O3 120.000(1) 61_565 . . 67_556 ?
O3 S1 O3 O3 120.000(1) 67_556 . . 55_655 ?
O3 S1 O3 O3 -60.000(1) 19_665 . . 55_655 ?
O3 S1 O3 O3 180.000(0) 7_566 . . 55_655 ?
O3 S1 O3 O3 60.000(1) 13_656 . . 55_655 ?
O3 S1 O3 O3 -120.000(1) 61_565 . . 55_655 ?
O3 S1 O3 O3 -120.000(1) 67_556 . . 61_565 ?
O3 S1 O3 O3 60.000(1) 19_665 . . 61_565 ?
O3 S1 O3 O3 -60.000(2) 7_566 . . 61_565 ?
O3 S1 O3 O3 120.000(2) 55_655 . . 61_565 ?
O3 S1 O3 O3 180.000(1) 13_656 . . 61_565 ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_1209a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1968488'
loop_
_audit_author_name
_audit_author_address
'Hiromi Ota'
;Okayama University
Japan
;
_audit_update_record             
;
2019-11-27 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'Mn O39 S W11'
_chemical_formula_moiety         'Mn O39 S W11'
_chemical_formula_weight         2733.32
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      cubic
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'
_space_group_IT_number           229
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'x, z, y'
'y, x, z'
'z, y, x'
'x, -y, -z'
'z, -x, -y'
'y, -z, -x'
'x, -z, -y'
'y, -x, -z'
'z, -y, -x'
'-x, y, -z'
'-z, x, -y'
'-y, z, -x'
'-x, z, -y'
'-y, x, -z'
'-z, y, -x'
'-x, -y, z'
'-z, -x, y'
'-y, -z, x'
'-x, -z, y'
'-y, -x, z'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'x+1/2, z+1/2, y+1/2'
'y+1/2, x+1/2, z+1/2'
'z+1/2, y+1/2, x+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, -x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'x+1/2, -z+1/2, -y+1/2'
'y+1/2, -x+1/2, -z+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x+1/2, -z+1/2, y+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'-x, -z, -y'
'-y, -x, -z'
'-z, -y, -x'
'-x, y, z'
'-z, x, y'
'-y, z, x'
'-x, z, y'
'-y, x, z'
'-z, y, x'
'x, -y, z'
'z, -x, y'
'y, -z, x'
'x, -z, y'
'y, -x, z'
'z, -y, x'
'x, y, -z'
'z, x, -y'
'y, z, -x'
'x, z, -y'
'y, x, -z'
'z, y, -x'
'-x+1/2, -y+1/2, -z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, x+1/2, y+1/2'
'-y+1/2, z+1/2, x+1/2'
'-x+1/2, z+1/2, y+1/2'
'-y+1/2, x+1/2, z+1/2'
'-z+1/2, y+1/2, x+1/2'
'x+1/2, -y+1/2, z+1/2'
'z+1/2, -x+1/2, y+1/2'
'y+1/2, -z+1/2, x+1/2'
'x+1/2, -z+1/2, y+1/2'
'y+1/2, -x+1/2, z+1/2'
'z+1/2, -y+1/2, x+1/2'
'x+1/2, y+1/2, -z+1/2'
'z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, -x+1/2'
'x+1/2, z+1/2, -y+1/2'
'y+1/2, x+1/2, -z+1/2'
'z+1/2, y+1/2, -x+1/2'
#------------------------------------------------------------------------------
_cell_length_a                   17.864(16)
_cell_length_b                   17.864(16)
_cell_length_c                   17.864(16)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     5701(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7503
_cell_measurement_theta_min      3.20
_cell_measurement_theta_max      27.40
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2334.00
_exptl_absorpt_coefficient_mu    11.219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_T_max  0.291

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.111
_diffrn_reflns_number            43310
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_theta_max         27.257
_diffrn_reflns_theta_min         3.226
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             668
_reflns_number_gt                639
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0726
_refine_ls_wR_factor_ref         0.1755
_refine_ls_wR_factor_gt          0.1739
_refine_ls_number_restraints     6
_refine_ls_number_reflns         668
_refine_ls_number_parameters     19
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0654P)²+93.3820P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn Mn 0.3368 0.7283
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
W W -0.8490 6.8722
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
W1 W 0.64415(3) 0.64415(3) 0.500000 0.0812(5) Uani 0.9165 4 d S TU P . .
Mn1 Mn 0.64415(3) 0.64415(3) 0.500000 0.0812(5) Uani 0.0833 4 d S TU P . .
S1 S 0.500000 0.500000 0.500000 0.033(2) Uani 1 48 d S TU P . .
O1 O 0.7138(6) 0.7138(6) 0.500000 0.143(8) Uani 0.9167 4 d S TU P . .
O2 O 0.6799(8) 0.5736(6) 0.5736(6) 0.110(4) Uani 1 2 d S TU P . .
O3 O 0.5481(8) 0.5481(8) 0.5481(8) 0.053(7) Uani 0.5 6 d S TU P . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1 1.759(17) . ?
W1 O2 1.930(5) . ?
W1 O2 1.930(5) 68_556 ?
W1 O2 1.930(5) 67_556 ?
W1 O2 1.930(5) 2 ?
S1 O3 1.49(2) . ?
S1 O3 1.49(2) 49_666 ?
S1 O3 1.49(2) 67_556 ?
S1 O3 1.49(2) 7_566 ?
S1 O3 1.49(2) 55_655 ?
S1 O3 1.49(2) 13_656 ?
S1 O3 1.49(2) 61_565 ?
S1 O3 1.49(2) 19_665 ?
O3 O3 1.72(3) 67_556 ?
O3 O3 1.72(3) 55_655 ?
O3 O3 1.72(3) 61_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 W1 O2 103.2(4) . . ?
O1 W1 O2 103.2(4) . 68_556 ?
O2 W1 O2 153.6(8) . 68_556 ?
O1 W1 O2 103.2(4) . 67_556 ?
O2 W1 O2 85.9(8) . 67_556 ?
O2 W1 O2 88.2(8) 68_556 67_556 ?
O1 W1 O2 103.2(4) . 2 ?
O2 W1 O2 88.2(8) . 2 ?
O2 W1 O2 85.9(8) 68_556 2 ?
O2 W1 O2 153.6(8) 67_556 2 ?
O3 S1 O3 180.0(8) . 49_666 ?
O3 S1 O3 70.5 . 67_556 ?
O3 S1 O3 109.471(3) 49_666 67_556 ?
O3 S1 O3 109.471(8) . 7_566 ?
O3 S1 O3 70.529(2) 49_666 7_566 ?
O3 S1 O3 70.5 67_556 7_566 ?
O3 S1 O3 70.529(2) . 55_655 ?
O3 S1 O3 109.471(1) 49_666 55_655 ?
O3 S1 O3 109.471(3) 67_556 55_655 ?
O3 S1 O3 180.0 7_566 55_655 ?
O3 S1 O3 109.471(4) . 13_656 ?
O3 S1 O3 70.529(4) 49_666 13_656 ?
O3 S1 O3 70.529(2) 67_556 13_656 ?
O3 S1 O3 109.471(1) 7_566 13_656 ?
O3 S1 O3 70.529(4) 55_655 13_656 ?
O3 S1 O3 70.5 . 61_565 ?
O3 S1 O3 109.5 49_666 61_565 ?
O3 S1 O3 109.471(8) 67_556 61_565 ?
O3 S1 O3 70.529(2) 7_566 61_565 ?
O3 S1 O3 109.471(1) 55_655 61_565 ?
O3 S1 O3 180.0(8) 13_656 61_565 ?
O3 S1 O3 109.5 . 19_665 ?
O3 S1 O3 70.529(6) 49_666 19_665 ?
O3 S1 O3 180.0(8) 67_556 19_665 ?
O3 S1 O3 109.5 7_566 19_665 ?
O3 S1 O3 70.529(6) 55_655 19_665 ?
O3 S1 O3 109.471(1) 13_656 19_665 ?
O3 S1 O3 70.529(6) 61_565 19_665 ?
W1 O2 W1 141.3(8) . 3 ?
S1 O3 O3 54.738(2) . 67_556 ?
S1 O3 O3 54.738(1) . 55_655 ?
O3 O3 O3 90.003(2) 67_556 55_655 ?
S1 O3 O3 54.738(1) . 61_565 ?
O3 O3 O3 90.003(1) 67_556 61_565 ?
O3 O3 O3 90.003(3) 55_655 61_565 ?

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
O3 S1 O3 O3 60.000(2) 7_566 . . 67_556 ?
O3 S1 O3 O3 -120.000(2) 55_655 . . 67_556 ?
O3 S1 O3 O3 -60.000(2) 13_656 . . 67_556 ?
O3 S1 O3 O3 120.000(2) 61_565 . . 67_556 ?
O3 S1 O3 O3 180.000(0) 19_665 . . 67_556 ?
O3 S1 O3 O3 120.000(1) 67_556 . . 55_655 ?
O3 S1 O3 O3 180.000(0) 7_566 . . 55_655 ?
O3 S1 O3 O3 60.000(2) 13_656 . . 55_655 ?
O3 S1 O3 O3 -120.000(2) 61_565 . . 55_655 ?
O3 S1 O3 O3 -60.000(1) 19_665 . . 55_655 ?
O3 S1 O3 O3 -120.000(2) 67_556 . . 61_565 ?
O3 S1 O3 O3 -60.000(2) 7_566 . . 61_565 ?
O3 S1 O3 O3 120.000(2) 55_655 . . 61_565 ?
O3 S1 O3 O3 180.000(2) 13_656 . . 61_565 ?
O3 S1 O3 O3 60.000(2) 19_665 . . 61_565 ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================
#     End of CIF
#==============================================================================
