# Electronic Supplementary Material (ESI) for Nanoscale.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_compound1
_database_code_depnum_ccdc_archive 'CCDC 1920703'
loop_
_audit_author_name
_audit_author_address
'Jiangwei Zhang'
;Dalian Institute of Chemical Physics, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2019-06-04 deposited with the CCDC.	2019-08-23 downloaded from the CCDC.
;
_audit_creation_date             2019-04-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Ni O44 W12, 10(O), 24(N)'
_chemical_formula_sum            'N24 Ni O54 W12'
_chemical_formula_weight         3465.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C12H10 N3 O4 W2 Ni3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'

_cell_length_a                   17.6345(7)
_cell_length_b                   17.6345(7)
_cell_length_c                   17.6345(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5483.9(7)
_cell_formula_units_Z            1.92
_cell_measurement_reflns_used    1791
_cell_measurement_temperature    119.5(6)
_cell_measurement_theta_max      66.1480
_cell_measurement_theta_min      4.9850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.308
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3528
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.793
_diffrn_reflns_theta_max         66.793
_diffrn_reflns_theta_min         3.545
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.5(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4070
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -130.00-103.00   1.00    3.28    --  -42.91-178.00-180.00   27
  2  ω     63.00 109.00   1.00    3.28    --   42.91 143.00 -59.00   46
  3  ω     22.00  51.00   1.00   13.13    --   92.50-125.00  30.00   29
  4  ω     70.00 113.00   1.00   13.13    --   92.50 -61.00-180.00   43
  5  ω     63.00  89.00   1.00   13.13    --   92.50-125.00  30.00   26
  6  ω     79.00 112.00   1.00   13.13    --   92.50 125.00-180.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0629397000
_diffrn_orient_matrix_UB_12      0.0090423000
_diffrn_orient_matrix_UB_13      -0.0601576000
_diffrn_orient_matrix_UB_21      -0.0546700000
_diffrn_orient_matrix_UB_22      -0.0457406000
_diffrn_orient_matrix_UB_23      0.0502107000
_diffrn_orient_matrix_UB_31      -0.0267698000
_diffrn_orient_matrix_UB_32      0.0738783000
_diffrn_orient_matrix_UB_33      0.0383869000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                475
_reflns_number_total             517
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.238
_refine_diff_density_min         -4.651
_refine_diff_density_rms         0.573
_refine_ls_extinction_coef       0.00042(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         517
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0649
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1645
_refine_special_details          ?
_olex2_refinement_description    
;
1. Rigid bond restraints
 O5, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(Ni1)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.64068(4) 0.500000 0.35932(4) 0.0511(10) Uani 1 4 d S T P . .
O1 O 0.5568(8) 0.5568(8) 0.4432(8) 0.076(7) Uani 1 6 d S T P . .
O3 O 0.7077(7) 0.500000 0.2923(7) 0.107(10) Uani 1 4 d S T P . .
O2 O 0.6787(15) 0.5728(11) 0.4272(11) 0.129(8) Uani 1 2 d S T P . .
Ni1 Ni 0.500000 0.500000 0.500000 0.129(8) Uani 1 48 d S T P . .
O4 O 0.750000 0.750000 0.250000 0.52(17) Uani 1 12 d S TU P . .
N1 N 0.651(2) 0.651(2) 0.214(3) 0.18(2) Uani 1 2 d S T P . .
O5 O 0.783(3) 0.500000 0.500000 0.119(14) Uani 1 8 d S TU P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.0407(10) 0.0720(12) 0.0407(10) 0.000 0.0254(4) 0.000
O1 0.076(7) 0.076(7) 0.076(7) 0.010(7) 0.010(7) -0.010(7)
O3 0.069(10) 0.18(3) 0.069(10) 0.000 0.052(12) 0.000
O2 0.135(17) 0.126(12) 0.126(12) -0.073(15) -0.067(12) 0.067(12)
Ni1 0.135(17) 0.126(12) 0.126(12) -0.073(15) -0.067(12) 0.067(12)
O4 0.52(17) 0.52(17) 0.52(17) 0.20(11) 0.20(11) -0.20(11)
N1 0.22(3) 0.22(3) 0.09(2) 0.00(2) 0.00(2) 0.05(3)
O5 0.13(4) 0.112(19) 0.112(19) 0.000 0.000 0.000

_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 2.319(13) . ?
W1 O1 2.319(13) 51_565 ?
W1 O3 1.671(18) . ?
W1 O2 1.879(10) 51_565 ?
W1 O2 1.879(10) . ?
W1 O2 1.879(10) 60_556 ?
W1 O2 1.879(10) 11_566 ?
O1 Ni1 1.74(3) . ?

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 O1 51.2(11) 51_565 . ?
O3 W1 O1 154.4(6) . . ?
O3 W1 O1 154.4(6) . 51_565 ?
O3 W1 O2 101.5(9) . 51_565 ?
O3 W1 O2 101.5(9) . 60_556 ?
O3 W1 O2 101.5(9) . 11_566 ?
O3 W1 O2 101.5(9) . . ?
O2 W1 O1 61.7(8) 51_565 51_565 ?
O2 W1 O1 96.7(11) 51_565 . ?
O2 W1 O1 96.7(11) 60_556 . ?
O2 W1 O1 61.7(8) 11_566 . ?
O2 W1 O1 96.7(11) . 51_565 ?
O2 W1 O1 61.7(8) . . ?
O2 W1 O1 61.7(8) 60_556 51_565 ?
O2 W1 O1 96.7(11) 11_566 51_565 ?
O2 W1 O2 89.3(10) 60_556 51_565 ?
O2 W1 O2 86.2(13) . 51_565 ?
O2 W1 O2 157.1(19) . 60_556 ?
O2 W1 O2 157.1(19) 11_566 51_565 ?
O2 W1 O2 89.3(10) . 11_566 ?
O2 W1 O2 86.2(13) 60_556 11_566 ?
W1 O1 W1 98.3(7) 54_655 57_666 ?
W1 O1 W1 98.3(7) 54_655 . ?
W1 O1 W1 98.3(7) 57_666 . ?
Ni1 O1 W1 119.1(6) . . ?
Ni1 O1 W1 119.1(6) . 54_655 ?
Ni1 O1 W1 119.1(6) . 57_666 ?
W1 O2 W1 138.0(16) 54_655 . ?
O1 Ni1 O1 70.5 . 50_556 ?
O1 Ni1 O1 109.471(7) 50_556 51_565 ?
O1 Ni1 O1 180.0(8) 52_655 4_566 ?
O1 Ni1 O1 109.5 . 2_665 ?
O1 Ni1 O1 180.0(8) 3_656 51_565 ?
O1 Ni1 O1 180.0(8) 50_556 2_665 ?
O1 Ni1 O1 70.529(3) 49_666 3_656 ?
O1 Ni1 O1 70.529(2) . 52_655 ?
O1 Ni1 O1 109.471(1) 52_655 51_565 ?
O1 Ni1 O1 109.471(3) 50_556 52_655 ?
O1 Ni1 O1 70.529(1) 50_556 4_566 ?
O1 Ni1 O1 70.529(3) 2_665 52_655 ?
O1 Ni1 O1 109.471(1) 3_656 4_566 ?
O1 Ni1 O1 180.0(8) . 49_666 ?
O1 Ni1 O1 70.529(1) . 51_565 ?
O1 Ni1 O1 109.5 50_556 49_666 ?
O1 Ni1 O1 70.529(1) 2_665 51_565 ?
O1 Ni1 O1 70.529(6) 2_665 49_666 ?
O1 Ni1 O1 109.471(1) 49_666 51_565 ?
O1 Ni1 O1 109.471(2) 52_655 49_666 ?
O1 Ni1 O1 109.471(7) . 4_566 ?
O1 Ni1 O1 109.471(3) . 3_656 ?
O1 Ni1 O1 109.471(1) 2_665 4_566 ?
O1 Ni1 O1 70.529(2) 50_556 3_656 ?
O1 Ni1 O1 70.529(2) 49_666 4_566 ?
O1 Ni1 O1 109.471(1) 2_665 3_656 ?
O1 Ni1 O1 70.529(1) 51_565 4_566 ?
O1 Ni1 O1 70.529(3) 52_655 3_656 ?
# SQUEEZE RESULTS (Version = 260918)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.030 -0.014 0.452 2762 -650 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL 20190404-ni      I m -3 m     R = 0.06
CELL   17.6345   17.6345   17.6345     90.00     90.00     90.00
SPGR Im-3m
# Solvent Accessible Volume =      2762
# Electrons Found in S.A.V. =         0
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
Q101 0.092 0.904 0.096 !       2.72 eA-3
Q102 0.063 0.172 0.061 !       2.68 eA-3
Q103 0.040 0.107 0.107 !       2.53 eA-3
Q104 0.087 0.910 0.194 !       2.23 eA-3
Q105 0.827 0.896 0.040 !       2.21 eA-3
Q106 0.322 0.672 0.460 !       2.15 eA-3
Q107 0.500 0.217 0.217 !       1.82 eA-3
Q108 1.000 0.998 0.141 !       1.74 eA-3
Q109 0.954 0.999 0.047 !       1.51 eA-3
Q110 1.000 0.078 0.001 !       1.39 eA-3
Q111 0.715 0.707 0.287 !       1.38 eA-3
Q112 0.541 0.509 0.375 !       1.37 eA-3
Q113 0.936 0.939 0.061 !       1.02 eA-3
C114 0.137 0.999 0.422 !       0.94 eA-3
Q115 0.515 0.847 0.462 !       0.68 eA-3
Q116 0.346 1.000 0.000 !       0.64 eA-3
Q117 0.862 0.337 0.306 !       0.57 eA-3
Q118 0.638 0.163 0.194 !       0.57 eA-3
Q119 0.362 0.837 0.806 !       0.57 eA-3
Q120 0.663 0.315 0.853 !       0.57 eA-3
Q121 0.222 0.709 0.291 !       0.56 eA-3
;
####################################################################### 
# 
# 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_compound3
_database_code_depnum_ccdc_archive 'CCDC 1920705'
loop_
_audit_author_name
_audit_author_address
'Jiangwei Zhang'
;Dalian Institute of Chemical Physics, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2019-06-04 deposited with the CCDC.	2019-08-23 downloaded from the CCDC.
;
_audit_creation_date             2019-04-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Fe0.5 O22 W6), 24(O)'
_chemical_formula_sum            'Fe O68.01 W12'
_chemical_formula_weight         3350.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C12 H10 O3 N4 Fe3 W3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'

_cell_length_a                   17.5944(6)
_cell_length_b                   17.5944(6)
_cell_length_c                   17.5944(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5446.6(6)
_cell_formula_units_Z            1.99968
_cell_measurement_reflns_used    1594
_cell_measurement_temperature    127(13)
_cell_measurement_theta_max      66.8770
_cell_measurement_theta_min      4.9910
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.392
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2916
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3539
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.100
_diffrn_reflns_theta_max         67.100
_diffrn_reflns_theta_min         3.553
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      127(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4070
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     15.00  66.00   1.00    6.65    --   42.79 -41.00  81.00   51
  2  ω     64.00  97.00   1.00   26.61    --   92.50 -15.00   0.00   33
  3  ω    113.00 138.00   1.00   26.61    --   92.50 -15.00   0.00   25
  4  ω     73.00  99.00   1.00   26.61    --   92.50 125.00 120.00   26
  5  ω     12.00  38.00   1.00   26.61    --   92.50 -15.00   0.00   26
  6  ω    128.00 164.00   1.00   26.61    --   92.50 125.00  60.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0416082000
_diffrn_orient_matrix_UB_12      -0.0680660000
_diffrn_orient_matrix_UB_13      0.0362245000
_diffrn_orient_matrix_UB_21      -0.0747577000
_diffrn_orient_matrix_UB_22      -0.0455891000
_diffrn_orient_matrix_UB_23      0.0002809000
_diffrn_orient_matrix_UB_31      0.0187446000
_diffrn_orient_matrix_UB_32      -0.0311787000
_diffrn_orient_matrix_UB_33      -0.0795813000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                459
_reflns_number_total             516
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.612
_refine_diff_density_min         -2.379
_refine_diff_density_rms         0.509
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         516
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.1002
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1696P)²+216.3055P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2670
_refine_ls_wR_factor_ref         0.2766
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(W1) = Uanis(Fe1)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.64095(5) 0.64095(5) 0.500000 0.0667(9) Uani 1 4 d S T P . .
O1 O 0.7078(10) 0.7078(10) 0.500000 0.131(15) Uani 1 4 d S T P . .
O3 O 0.5581(13) 0.5581(13) 0.4419(13) 0.104(12) Uani 1 6 d S T P . .
O2 O 0.5741(12) 0.6825(16) 0.4259(12) 0.131(11) Uani 1 2 d S T P . .
Fe1 Fe 0.500000 0.500000 0.500000 0.0667(9) Uani 1 48 d S T P . .
O0AA O 0.679(4) 0.789(7) 0.321(4) 0.48(7) Uani 1 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.0562(10) 0.0562(10) 0.0878(14) 0.000 0.000 -0.0238(6)
O1 0.074(12) 0.074(12) 0.25(5) 0.000 0.000 -0.044(16)
O3 0.104(12) 0.104(12) 0.104(12) 0.011(12) 0.011(12) -0.011(12)
O2 0.140(15) 0.113(19) 0.140(15) -0.046(13) -0.057(19) 0.046(13)
Fe1 0.0562(10) 0.0562(10) 0.0878(14) 0.000 0.000 -0.0238(6)
O0AA 0.49(8) 0.47(14) 0.49(8) 0.12(11) -0.29(11) -0.12(11)

_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 1.66(2) . ?
W1 O3 2.301(19) 50_556 ?
W1 O3 2.301(19) . ?
W1 O3 2.301(19) 13_556 ?
W1 O2 1.902(11) 11_566 ?
W1 O2 1.902(11) 58_565 ?
W1 O2 1.902(11) 50_556 ?
W1 O2 1.902(11) . ?
O3 Fe1 1.77(4) . ?

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 O3 153.6(9) . 50_556 ?
O1 W1 O3 153.6(9) . 13_556 ?
O1 W1 O3 153.6(9) . . ?
O1 W1 O2 99.5(9) . . ?
O1 W1 O2 99.5(9) . 50_556 ?
O1 W1 O2 99.5(9) . 11_566 ?
O1 W1 O2 99.5(9) . 58_565 ?
O3 W1 O3 52.8(18) . 13_556 ?
O3 W1 O3 0.006(4) 13_556 50_556 ?
O3 W1 O3 52.8(18) . 50_556 ?
O2 W1 O3 99.0(12) 58_565 . ?
O2 W1 O3 99.0(12) . 50_556 ?
O2 W1 O3 63.1(9) 58_565 50_556 ?
O2 W1 O3 63.1(9) 50_556 13_556 ?
O2 W1 O3 99.0(12) 11_566 50_556 ?
O2 W1 O3 99.0(12) . 13_556 ?
O2 W1 O3 63.1(9) 50_556 50_556 ?
O2 W1 O3 99.0(12) 50_556 . ?
O2 W1 O3 63.1(9) . . ?
O2 W1 O3 63.1(9) 11_566 . ?
O2 W1 O3 63.1(9) 58_565 13_556 ?
O2 W1 O3 99.0(12) 11_566 13_556 ?
O2 W1 O2 86.6(16) 50_556 . ?
O2 W1 O2 160.9(18) 58_565 . ?
O2 W1 O2 86.6(16) 11_566 58_565 ?
O2 W1 O2 160.9(18) 11_566 50_556 ?
O2 W1 O2 90.3(14) 58_565 50_556 ?
O2 W1 O2 90.3(14) 11_566 . ?
W1 O3 W1 99.3(11) 11_566 55_556 ?
W1 O3 W1 99.3(11) . 55_556 ?
W1 O3 W1 99.3(11) . 11_566 ?
Fe1 O3 W1 118.3(9) . 55_556 ?
Fe1 O3 W1 118.3(9) . . ?
Fe1 O3 W1 118.3(9) . 11_566 ?
W1 O2 W1 134.4(16) . 55_556 ?
O3 Fe1 O3 109.466(1) 17_556 16_655 ?
O3 Fe1 O3 70.526(3) . 16_655 ?
O3 Fe1 O3 109.466(1) 59_655 17_556 ?
O3 Fe1 O3 109.466(11) 13_556 60_556 ?
O3 Fe1 O3 0.0(11) 19_666 55_556 ?
O3 Fe1 O3 109.5 59_655 60_556 ?
O3 Fe1 O3 109.474(4) 50_556 16_655 ?
O3 Fe1 O3 109.474(1) 19_666 60_556 ?
O3 Fe1 O3 109.466(3) 59_655 55_556 ?
O3 Fe1 O3 0.0(11) 17_556 60_556 ?
O3 Fe1 O3 109.474(11) 13_556 17_556 ?
O3 Fe1 O3 109.481(10) 50_556 51_565 ?
O3 Fe1 O3 109.466(2) 19_666 17_556 ?
O3 Fe1 O3 109.466(1) 22_565 51_565 ?
O3 Fe1 O3 109.466(3) 22_565 16_655 ?
O3 Fe1 O3 70.534(1) . 51_565 ?
O3 Fe1 O3 0(2) 55_556 16_655 ?
O3 Fe1 O3 109.466(3) 55_556 51_565 ?
O3 Fe1 O3 70.526(3) . 55_556 ?
O3 Fe1 O3 109.466(3) 16_655 51_565 ?
O3 Fe1 O3 109.481(10) 50_556 17_556 ?
O3 Fe1 O3 109.466(5) 50_556 21_556 ?
O3 Fe1 O3 109.466(1) 22_565 17_556 ?
O3 Fe1 O3 109.466(2) 22_565 21_556 ?
O3 Fe1 O3 70.534(1) . 17_556 ?
O3 Fe1 O3 70.526(3) . 21_556 ?
O3 Fe1 O3 109.466(3) 55_556 17_556 ?
O3 Fe1 O3 0.0(11) 55_556 21_556 ?
O3 Fe1 O3 109.481(6) 13_556 16_655 ?
O3 Fe1 O3 0.0(11) 16_655 21_556 ?
O3 Fe1 O3 109.466(3) 59_655 16_655 ?
O3 Fe1 O3 109.474(1) 51_565 21_556 ?
O3 Fe1 O3 0.0(11) 19_666 16_655 ?
O3 Fe1 O3 109.481(6) 13_556 55_556 ?
O3 Fe1 O3 109.466(3) 22_565 55_556 ?
O3 Fe1 O3 109.474(11) 50_556 60_556 ?
O3 Fe1 O3 0.0(11) 50_556 13_556 ?
O3 Fe1 O3 109.5 22_565 60_556 ?
O3 Fe1 O3 109.5 50_556 22_565 ?
O3 Fe1 O3 70.534(1) . 60_556 ?
O3 Fe1 O3 109.5 13_556 22_565 ?
O3 Fe1 O3 109.474(1) 55_556 60_556 ?
O3 Fe1 O3 109.5 50_556 59_655 ?
O3 Fe1 O3 109.474(1) 16_655 60_556 ?
O3 Fe1 O3 109.5 13_556 59_655 ?
O3 Fe1 O3 109.474(11) 13_556 51_565 ?
O3 Fe1 O3 0(2) 22_565 59_655 ?
O3 Fe1 O3 109.466(1) 59_655 51_565 ?
O3 Fe1 O3 70.534(1) 50_556 . ?
O3 Fe1 O3 109.466(2) 19_666 51_565 ?
O3 Fe1 O3 70.534(1) 13_556 . ?
O3 Fe1 O3 0(2) 17_556 51_565 ?
O3 Fe1 O3 180.0(11) 22_565 . ?
O3 Fe1 O3 0.0(11) 60_556 51_565 ?
O3 Fe1 O3 180.0(11) 59_655 . ?
O3 Fe1 O3 109.474(4) 13_556 21_556 ?
O3 Fe1 O3 109.466(5) 50_556 19_666 ?
O3 Fe1 O3 109.466(2) 59_655 21_556 ?
O3 Fe1 O3 109.474(4) 13_556 19_666 ?
O3 Fe1 O3 0.008(5) 19_666 21_556 ?
O3 Fe1 O3 109.474(2) 22_565 19_666 ?
O3 Fe1 O3 109.474(1) 17_556 21_556 ?
O3 Fe1 O3 109.474(2) 59_655 19_666 ?
O3 Fe1 O3 109.481(2) 60_556 21_556 ?
O3 Fe1 O3 70.519(2) . 19_666 ?
O3 Fe1 O3 109.474(4) 50_556 55_556 ?
# SQUEEZE RESULTS (Version = 260918)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.035 -0.014 0.373 3106 978 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
# Solvent Accessible Volume =      3101
# Electrons Found in S.A.V. =       970
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.609 0.090 0.090 !       1.05 eA-3
C102 0.367 1.000 0.000 !       1.04 eA-3
Q103 0.158 0.151 0.393 !       0.98 eA-3
C104 0.365 0.047-0.003 !       0.94 eA-3
C105 0.410 1.000 0.000 !       0.92 eA-3
Q106 0.064 0.845 0.064 !       0.83 eA-3
Q107 0.783 0.219-0.002 !       0.83 eA-3
C108 0.104 0.375-0.008 !       0.77 eA-3
Q109 0.436 0.842 0.158 !       0.77 eA-3
Q110 0.191 0.525 0.205 !       0.76 eA-3
Q111 0.921 0.704 0.357 !       0.74 eA-3
C112 0.059 0.637 0.052 !       0.74 eA-3
Q113 0.886 0.958 0.113 !       0.71 eA-3
Q114 0.690 0.593 0.110 !       0.71 eA-3
Q115 0.500 0.494 0.219 !       0.70 eA-3
Q116 0.904 0.045 0.157 !       0.68 eA-3
Q117 0.124 0.251 0.375 !       0.67 eA-3
C118 0.151 0.494 0.109 !       0.65 eA-3
C119 0.344 0.344 0.000 !       0.63 eA-3
Q120 1.000 0.094-0.001 !       0.61 eA-3
C121 0.832 0.475 0.408 !       0.60 eA-3
Q122 0.750 0.331 0.169 !       0.59 eA-3
Q123 0.739 0.270 0.042 !       0.58 eA-3
Q124 0.213 1.000 0.000 !       0.58 eA-3
C125 0.299 0.344 0.000 !       0.54 eA-3
Q126 0.911 0.772 0.338 !       0.52 eA-3
Q127 0.405 0.688 0.612 !       0.51 eA-3
Q128 0.905 0.188 0.112 !       0.51 eA-3
Q129 0.382 0.432 0.687 !       0.50 eA-3
;
####################################################################### 
# 
# 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_compound4
_database_code_depnum_ccdc_archive 'CCDC 1920706'
loop_
_audit_author_name
_audit_author_address
'Jiangwei Zhang'
;Dalian Institute of Chemical Physics, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2019-06-04 deposited with the CCDC.	2019-08-23 downloaded from the CCDC.
;
_audit_creation_date             2019-04-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'O44 W12, 12(N)'
_chemical_formula_sum            'N12 O44 W12'
_chemical_formula_weight         3078.20
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_H-M_alt        'I -4 3 m'
_space_group_name_Hall           'I -4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   17.6345(4)
_cell_length_b                   17.6345(4)
_cell_length_c                   17.6345(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5483.9(4)
_cell_formula_units_Z            1.92
_cell_measurement_reflns_used    772
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.788
_cell_measurement_theta_min      3.544
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.015
_exptl_absorpt_correction_T_max  0.100
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3528
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        66.788
_diffrn_reflns_theta_max         66.788
_diffrn_reflns_theta_min         3.544
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.658
_reflns_Friedel_fraction_full    0.808
_reflns_Friedel_fraction_max     0.808
_reflns_number_gt                772
_reflns_number_total             857
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.347
_refine_diff_density_min         -3.232
_refine_diff_density_rms         0.513
_refine_ls_abs_structure_details 
;
 Flack x determined using 285 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.50(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         857
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0889
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1856P)²+12.1961P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2176
_refine_ls_wR_factor_ref         0.2290
_refine_special_details          ?
_olex2_refinement_description    
;
1. Rigid bond restraints
 O3, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 O3, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N1(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.64062(3) 0.5003(2) 0.35938(3) 0.0465(8) Uani 1 2 d S T P . .
O4 O 0.563(6) 0.563(6) 0.437(6) 0.1980(13) Uani 1 6 d S TU P . .
O1 O 0.5649(12) 0.4351(12) 0.3288(13) 0.045(6) Uani 1 2 d S T P . .
O3 O 0.701(2) 0.5865(13) 0.4135(13) 0.087(13) Uani 1 2 d S TU P . .
O2 O 0.7074(7) 0.492(4) 0.2926(7) 0.086(12) Uani 1 2 d S T P . .
O5 O 0.5573(12) 0.4427(12) 0.4427(12) 0.033(7) Uani 1 6 d S T P . .
N1 N 0.733(7) 0.791(6) 0.273(19) 0.31(9) Uani 0.5 1 d . U . A -1

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
W1 0.0355(8) 0.0685(10) 0.0355(8) 0.0003(9) 0.0260(4) -0.0003(9)
O4 0.1980(13) 0.1980(13) 0.1980(13) 0.0000(8) 0.0000(8) 0.0000(8)
O1 0.049(8) 0.049(8) 0.035(11) 0.012(8) -0.012(8) -0.033(12)
O3 0.09(2) 0.085(15) 0.085(15) 0.04(2) 0.036(12) -0.036(12)
O2 0.055(8) 0.15(4) 0.055(8) 0.008(18) 0.043(11) -0.008(18)
O5 0.033(7) 0.033(7) 0.033(7) -0.007(8) 0.007(8) 0.007(8)
N1 0.26(15) 0.12(7) 0.5(3) -0.08(12) -0.28(13) -0.02(10)

_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 O4 2.24(7) . ?
W1 O1 1.843(7) . ?
W1 O1 1.843(7) 7_665 ?
W1 O3 2.09(2) 11_566 ?
W1 O3 2.09(2) . ?
W1 O2 1.67(2) . ?
W1 O5 2.313(19) . ?

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
O4 W1 O5 55(4) . . ?
O1 W1 O4 92(3) 7_665 . ?
O1 W1 O4 92(3) . . ?
O1 W1 O1 92.0(14) . 7_665 ?
O1 W1 O3 88.5(12) . 11_566 ?
O1 W1 O3 88.5(12) 7_665 . ?
O1 W1 O3 163.3(16) 7_665 11_566 ?
O1 W1 O3 163.3(16) . . ?
O1 W1 O5 56.7(8) . . ?
O1 W1 O5 56.7(8) 7_665 . ?
O3 W1 O4 71(3) . . ?
O3 W1 O4 71(3) 11_566 . ?
O3 W1 O3 86(2) . 11_566 ?
O3 W1 O5 110.7(9) 11_566 . ?
O3 W1 O5 110.7(9) . . ?
O2 W1 O4 156(5) . . ?
O2 W1 O1 104.3(19) . 7_665 ?
O2 W1 O1 104.3(19) . . ?
O2 W1 O3 91.7(19) . . ?
O2 W1 O3 91.7(19) . 11_566 ?
O2 W1 O5 149(3) . . ?
W1 O4 W1 103(5) 11_566 . ?
W1 O4 W1 103(5) 8_656 11_566 ?
W1 O4 W1 103(5) 8_656 . ?
W1 O1 W1 145.0(13) 10_656 . ?
W1 O3 W1 114.0(17) . 8_656 ?
W1 O5 W1 98.9(10) 7_665 . ?
W1 O5 W1 98.9(10) 10_656 . ?
W1 O5 W1 98.9(10) 10_656 7_665 ?
# SQUEEZE RESULTS (Version = 260918)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.021 -0.011 0.384 3559 1178 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
# Solvent Accessible Volume =      3541
# Electrons Found in S.A.V. =      1174
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
Q101 1.000 1.000 0.000 !       2.83 eA-3
Q102 0.624 0.183 0.148 !       2.13 eA-3
Q103 1.000 1.001 0.141 !       1.87 eA-3
Q104 0.866 0.321 0.296 !       1.72 eA-3
Q105 0.404 0.591 0.409 !       1.72 eA-3
Q106 0.406 0.406 0.406 !       1.54 eA-3
Q107 0.236 0.392 0.232 !       1.53 eA-3
Q108 0.176 0.188 0.060 !       1.47 eA-3
C109 0.489 0.479 0.160 !       1.41 eA-3
Q110 0.175 0.933 0.188 !       1.36 eA-3
Q111 0.036 0.094 0.094 !       1.32 eA-3
Q112 0.536 0.594 0.594 !       1.32 eA-3
Q113 0.094 0.902 0.968 !       1.31 eA-3
Q114 0.935 0.175 0.063 !       1.28 eA-3
C115 0.457 0.076 0.076 !       1.26 eA-3
C116 0.466 0.385 0.075 !       1.25 eA-3
C117 0.079 0.427 0.427 !       1.25 eA-3
C118 0.953 0.041 0.376 !       1.24 eA-3
C119 0.408 0.158 0.190 !       1.22 eA-3
Q120 0.407 0.469 0.400 !       1.22 eA-3
Q121 0.549 0.616 0.384 !       1.20 eA-3
Q122 0.933 0.832 0.058 !       1.19 eA-3
Q123 0.684 0.802 0.143 !       1.16 eA-3
C124 0.388 0.421 0.027 !       1.16 eA-3
C125 0.124 0.390 0.413 !       1.15 eA-3
C126 0.641 0.099 0.824 !       1.13 eA-3
C127 0.141 0.599 0.324 !       1.13 eA-3
C128 0.333 0.137 0.594 !       1.13 eA-3
Q129 0.678 0.156 0.061 !       1.13 eA-3
C130 0.610 0.348 0.114 !       1.13 eA-3
C131 0.358 0.832 0.911 !       1.12 eA-3
C132 0.333 0.405 0.863 !       1.12 eA-3
Q133 0.377 0.434 0.414 !       1.11 eA-3
Q134 0.309 0.586 0.468 !       1.11 eA-3
C135 0.811 0.810 0.436 !       1.10 eA-3
Q136 0.909 0.904 0.191 !       1.10 eA-3
C137 0.049 0.514 0.062 !       1.10 eA-3
C138 0.549 0.014 0.562 !       1.10 eA-3
C139 0.060 0.666 0.380 !       1.07 eA-3
C140 0.108 0.519 0.411 !       1.00 eA-3
C141 0.453 0.548 0.063 !       1.00 eA-3
Q142 0.871 0.036 0.313 !       0.96 eA-3
C143 0.097 0.857 0.416 !       0.96 eA-3
C144 0.418 0.126 0.080 !       0.95 eA-3
Q145 0.817 0.091 0.091 !       0.95 eA-3
Q146 0.283 1.000 0.000 !       0.95 eA-3
Q147 0.825 0.706 0.165 !       0.94 eA-3
Q148 0.699 0.193 0.094 !       0.94 eA-3
C149 0.665 0.119 0.912 !       0.94 eA-3
Q150 0.351 0.270 0.116 !       0.94 eA-3
C151 0.767 0.513 0.029 !       0.92 eA-3
C152 0.930 0.536 0.971 !       0.92 eA-3
Q153 0.024 0.327 0.235 !       0.90 eA-3
C154 0.986 0.739 0.388 !       0.89 eA-3
Q155 0.123 0.997 0.047 !       0.89 eA-3
C156 0.940 0.614 0.103 !       0.87 eA-3
Q157 0.096 1.000 0.000 !       0.85 eA-3
Q158 0.706 0.303-0.003 !       0.83 eA-3
Q159 1.000 0.797-0.009 !       0.83 eA-3
Q160 0.781 0.512 0.363 !       0.81 eA-3
C161 0.393 0.112 0.214 !       0.80 eA-3
C162 0.049 0.730 0.354 !       0.76 eA-3
Q163 0.640 0.245 0.245 !       0.76 eA-3
Q164 0.751 0.165 0.329 !       0.72 eA-3
C165 0.699 0.092 0.412 !       0.71 eA-3
Q166 0.737 0.267 0.419 !       0.71 eA-3
Q167 0.654 0.747 0.253 !       0.69 eA-3
Q168 0.249 0.249 0.249 !       0.69 eA-3
Q169 0.214 0.886 0.216 !       0.69 eA-3
Q170 0.263 0.268 0.419 !       0.66 eA-3
Q171 0.775 0.042 0.060 !       0.66 eA-3
Q172 0.314 0.205 0.317 !       0.65 eA-3
Q173 0.336 0.798 0.202 !       0.65 eA-3
C174 0.044 0.619 0.164 !       0.64 eA-3
Q175 0.391 0.723 0.277 !       0.62 eA-3
Q176 0.232 0.952-0.003 !       0.60 eA-3
C177 0.236 1.006 0.433 !       0.60 eA-3
Q178 0.844 0.984 0.328 !       0.58 eA-3
C179 0.379 0.169-0.004 !       0.57 eA-3
C180 0.514 0.177 0.153 !       0.56 eA-3
C181 0.544 0.685 0.088 !       0.56 eA-3
C182 0.076 0.685 0.557 !       0.56 eA-3
C183 0.438 0.733 0.039 !       0.55 eA-3
Q184 0.047 0.048 0.000 !       0.55 eA-3
C185 0.199 0.415 0.978 !       0.54 eA-3
C186 0.406 0.293 0.058 !       0.53 eA-3
Q187 0.386 0.767 0.474 !       0.53 eA-3
Q188 0.139 0.139 0.139 !       0.52 eA-3
;
####################################################################### 
# 
# 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_compound2
_database_code_depnum_ccdc_archive 'CCDC 1920704'
loop_
_audit_author_name
_audit_author_address
'Jiangwei Zhang'
;Dalian Institute of Chemical Physics, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2019-06-04 deposited with the CCDC.	2019-08-23 downloaded from the CCDC.
;
_audit_creation_date             2019-04-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Co0.5 O22 W6)'
_chemical_formula_sum            'Co1 O44 W12'
_chemical_formula_weight         2969.01
_chemical_melting_point          ?
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 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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'

_cell_length_a                   17.555(2)
_cell_length_b                   17.555(2)
_cell_length_c                   17.555(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5410.1(18)
_cell_formula_units_Z            1.92
_cell_measurement_reflns_used    515
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.889
_exptl_absorpt_correction_T_max  0.276
_exptl_absorpt_correction_T_min  0.057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,Version 1.171.39.46 
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2534
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4227
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.127
_diffrn_reflns_theta_max         25.127
_diffrn_reflns_theta_min         1.640
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                468
_reflns_number_total             515
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         3.855
_refine_diff_density_min         -3.636
_refine_diff_density_rms         0.699
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         515
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0585
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1692P)²+697.4376P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1892
_refine_ls_wR_factor_ref         0.1946
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O1)
Uanis(W1) = Uanis(Co1)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.64095(6) 0.500000 0.64095(6) 0.0416(10) Uani 1 4 d S T P . .
O3 O 0.5582(14) 0.4418(14) 0.5582(14) 0.069(9) Uani 1 6 d S T P . .
O1 O 0.7078(15) 0.500000 0.7078(15) 0.069(9) Uani 1 4 d S T P . .
O2 O 0.5722(17) 0.4278(17) 0.682(2) 0.112(16) Uani 1 2 d S T P . .
Co1 Co 0.500000 0.500000 0.500000 0.0416(10) Uani 1 48 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.0308(10) 0.0633(15) 0.0308(10) 0.000 -0.0249(7) 0.000
O3 0.069(9) 0.069(9) 0.069(9) 0.020(10) -0.020(10) 0.020(10)
O1 0.069(9) 0.069(9) 0.069(9) 0.020(10) -0.020(10) 0.020(10)
O2 0.11(2) 0.11(2) 0.12(3) -0.07(2) 0.07(2) -0.06(2)
Co1 0.0308(10) 0.0633(15) 0.0308(10) 0.000 -0.0249(7) 0.000

_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 O3 2.29(2) . ?
W1 O3 2.29(2) 51_565 ?
W1 O1 1.66(4) . ?
W1 O2 1.891(16) 51_565 ?
W1 O2 1.891(16) . ?
W1 O2 1.891(16) 6_566 ?
W1 O2 1.891(16) 55_556 ?
O3 Co1 1.77(4) . ?

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
O3 W1 O3 52.9(19) 51_565 . ?
O1 W1 O3 153.5(10) . . ?
O1 W1 O3 153.5(10) . 51_565 ?
O1 W1 O2 100.6(14) . 51_565 ?
O1 W1 O2 100.6(14) . 6_566 ?
O1 W1 O2 100.6(14) . 55_556 ?
O1 W1 O2 100.6(14) . . ?
O2 W1 O3 62.4(13) 51_565 51_565 ?
O2 W1 O3 97.7(16) 51_565 . ?
O2 W1 O3 62.4(13) 6_566 . ?
O2 W1 O3 97.7(16) 55_556 . ?
O2 W1 O3 97.7(16) . 51_565 ?
O2 W1 O3 62.4(13) . . ?
O2 W1 O3 97.7(16) 6_566 51_565 ?
O2 W1 O3 62.4(13) 55_556 51_565 ?
O2 W1 O2 159(3) 6_566 51_565 ?
O2 W1 O2 84(2) . 51_565 ?
O2 W1 O2 92.0(18) . 6_566 ?
O2 W1 O2 92.0(18) 55_556 51_565 ?
O2 W1 O2 159(3) . 55_556 ?
O2 W1 O2 84(2) 6_566 55_556 ?
W1 O3 W1 99.4(12) 58_565 6_566 ?
W1 O3 W1 99.4(12) 58_565 . ?
W1 O3 W1 99.4(12) 6_566 . ?
Co1 O3 W1 118.3(10) . . ?
Co1 O3 W1 118.3(10) . 58_565 ?
Co1 O3 W1 118.3(10) . 6_566 ?
W1 O2 W1 135(2) 58_565 . ?
O3 Co1 O3 70.532(1) . 51_565 ?
O3 Co1 O3 109.468(7) 51_565 49_666 ?
O3 Co1 O3 180.0(13) 52_655 4_566 ?
O3 Co1 O3 109.468(1) . 3_656 ?
O3 Co1 O3 70.532(6) 2_665 49_666 ?
O3 Co1 O3 180.0(13) 51_565 3_656 ?
O3 Co1 O3 180.0 50_556 2_665 ?
O3 Co1 O3 70.522(8) . 52_655 ?
O3 Co1 O3 109.478(2) 52_655 49_666 ?
O3 Co1 O3 109.468(1) 51_565 52_655 ?
O3 Co1 O3 70.532(1) 51_565 4_566 ?
O3 Co1 O3 70.532(10) 3_656 52_655 ?
O3 Co1 O3 109.468(9) 2_665 4_566 ?
O3 Co1 O3 70.532(3) . 50_556 ?
O3 Co1 O3 180.0(13) . 49_666 ?
O3 Co1 O3 109.478(13) 51_565 50_556 ?
O3 Co1 O3 70.532(7) 3_656 49_666 ?
O3 Co1 O3 70.522(3) 3_656 50_556 ?
O3 Co1 O3 109.468(1) 50_556 49_666 ?
O3 Co1 O3 109.468(1) 52_655 50_556 ?
O3 Co1 O3 109.478(12) . 4_566 ?
O3 Co1 O3 109.468(1) . 2_665 ?
O3 Co1 O3 109.468(5) 3_656 4_566 ?
O3 Co1 O3 70.522(3) 51_565 2_665 ?
O3 Co1 O3 70.532(1) 50_556 4_566 ?
O3 Co1 O3 109.478(2) 3_656 2_665 ?
O3 Co1 O3 70.5 49_666 4_566 ?
O3 Co1 O3 70.532(5) 52_655 2_665 ?
# SQUEEZE RESULTS (Version = 260918)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.012 -0.007 0.390 4095 2134 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
CELL   17.5550   17.5550   17.5550     90.00     90.00     90.00
SPGR Im-3m
# Solvent Accessible Volume =      4108
# Electrons Found in S.A.V. =      2116
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
Q101 1.000 0.141 0.003 !       4.20 eA-3
Q102 0.358 0.639 0.361 !       2.27 eA-3
C103 0.822 0.710 0.173 !       2.12 eA-3
C104 0.792 0.333 0.198 !       1.96 eA-3
C105 0.376 0.826 0.174 !       1.90 eA-3
C106 0.768 0.294 0.226 !       1.86 eA-3
C107 0.500 0.503 0.141 !       1.81 eA-3
C108 0.234 0.766 0.234 !       1.80 eA-3
Q109 0.581 0.575 0.425 !       1.73 eA-3
C110 1.000 0.422-0.005 !       1.70 eA-3
C111 0.314 0.248 0.188 !       1.65 eA-3
C112 0.031 0.500 0.484 !       1.59 eA-3
Q113 0.436 0.562 0.736 !       1.46 eA-3
Q114 0.936 0.062 0.236 !       1.46 eA-3
Q115 0.767 0.061 0.939 !       1.46 eA-3
C116 0.420 0.931 0.070 !       1.42 eA-3
C117 0.374 1.003 0.109 !       1.41 eA-3
C118 0.392 0.112 0.087 !       1.34 eA-3
C119 0.404 0.268 0.143 !       1.28 eA-3
C120 0.051 0.458 0.041 !       1.27 eA-3
Q121 0.223 1.001 0.141 !       1.27 eA-3
C122 0.362 0.126 0.256 !       1.25 eA-3
Q123 0.796 0.803 0.030 !       1.19 eA-3
C124 0.035 0.378 0.036 !       1.18 eA-3
Q125 0.058 1.001 0.125 !       1.17 eA-3
C126 0.250 0.498 0.094 !       1.13 eA-3
Q127 1.000 0.858 0.281 !       1.11 eA-3
C128 0.550 0.608 0.034 !       1.11 eA-3
Q129 0.044 0.998 0.031 !       1.10 eA-3
C130 0.155 0.634 0.366 !       1.08 eA-3
C131 0.615 0.998 0.172 !       1.07 eA-3
C132 0.375 1.002 0.063 !       1.06 eA-3
C133 0.143 0.500 0.000 !       1.06 eA-3
C134 0.750 0.579 0.079 !       1.04 eA-3
Q135 0.869 0.232 0.232 !       1.04 eA-3
C136 0.306 0.108 0.420 !       1.04 eA-3
C137 0.806 0.608 0.920 !       1.04 eA-3
C138 0.694 0.892 0.580 !       1.04 eA-3
C139 0.669 0.940 0.630 !       1.01 eA-3
C140 0.169 0.440 0.130 !       1.01 eA-3
C141 0.643 0.661 0.935 !       1.01 eA-3
Q142 0.920 0.170 0.143 !       1.00 eA-3
C143 0.731 0.686 0.121 !       0.99 eA-3
C144 0.565 0.997 0.109 !       0.94 eA-3
C145 0.595 0.199 0.199 !       0.93 eA-3
C146 0.335 0.818 0.108 !       0.93 eA-3
Q147 0.203 0.500 0.203 !       0.93 eA-3
Q148 0.125 0.195 0.065 !       0.92 eA-3
C149 0.326 0.021 0.472 !       0.91 eA-3
C150 1.000 0.438 0.040 !       0.91 eA-3
Q151 0.082 0.202 0.227 !       0.89 eA-3
Q152 0.418 0.298 0.273 !       0.89 eA-3
C153 0.035 0.582 0.202 !       0.89 eA-3
Q154 0.229 0.057 0.228 !       0.84 eA-3
C155 0.986 0.503 0.078 !       0.83 eA-3
Q156 0.128 0.050 0.128 !       0.83 eA-3
Q157 0.500 0.249 0.249 !       0.83 eA-3
C158 0.416 1.009 0.406 !       0.80 eA-3
C159 0.332 0.031 0.121 !       0.79 eA-3
C160 0.120 0.526 0.132 !       0.78 eA-3
Q161 0.180 0.288 0.117 !       0.75 eA-3
C162 0.147 0.561 0.421 !       0.73 eA-3
C163 0.221 0.376 0.015 !       0.67 eA-3
C164 0.500 0.146 0.092 !       0.67 eA-3
C165 0.443 0.027 0.281 !       0.65 eA-3
Q166 0.665 0.493 0.172 !       0.64 eA-3
Q167 0.091 0.906 0.003 !       0.60 eA-3
C168 1.000 0.323 0.357 !       0.59 eA-3
Q169 0.944 0.947 0.055 !       0.51 eA-3
;
