# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2022

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

data_WB4_2_8GPa
_database_code_depnum_ccdc_archive 'CCDC 2158520'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         2800000
_audit_creation_date             2021-11-17
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.9349(4)
_cell_length_b                   2.9349(4)
_cell_length_c                   10.902(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     81.32(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    220
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      17.9640
_cell_measurement_theta_min      3.2570
_shelx_estimated_absorpt_T_max   0.967
_shelx_estimated_absorpt_T_min   0.967
_exptl_absorpt_coefficient_mu    6.687
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    9.274
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.540
_diffrn_reflns_Laue_measured_fraction_max 0.399
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            394
_diffrn_reflns_point_group_measured_fraction_full 0.540
_diffrn_reflns_point_group_measured_fraction_max 0.399
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         18.006
_diffrn_reflns_theta_min         3.270
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.540
_diffrn_measured_fraction_theta_max 0.399
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -30.00  30.00   0.50    1.00   0.00   0.00   0.00    --   120
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0214822000
_diffrn_orient_matrix_UB_12      0.0159674000
_diffrn_orient_matrix_UB_13      -0.0261543000
_diffrn_orient_matrix_UB_21      0.1117688000
_diffrn_orient_matrix_UB_22      0.0499094000
_diffrn_orient_matrix_UB_23      0.0049341000
_diffrn_orient_matrix_UB_31      -0.0055130000
_diffrn_orient_matrix_UB_32      -0.1011049000
_diffrn_orient_matrix_UB_33      -0.0017654000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                69
_reflns_number_total             79
_reflns_odcompleteness_completeness 36.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     18.01
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.449
_refine_diff_density_min         -2.228
_refine_diff_density_rms         0.535
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0243
_refine_ls_restrained_S_all      1.060
_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)+(0.0368P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0572
_refine_special_details          ?
_olex2_refinement_description    
;
;
_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 0.6667 0.3333 0.2500 0.0081(5) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.546(3) 0.0064(18) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.116(3) 0.0059(17) Uiso 1 6 d S . P . .


_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 W1 2.9349(4) 3_775 ?
W1 W1 2.9349(4) 3_765 ?
W1 W1 2.9349(4) 1_565 ?
W1 W1 2.9349(4) 1_455 ?
W1 B1 2.22(3) 13_666 ?
W1 B1 2.22(3) 4_664 ?
W1 B2 2.24(2) 16_556 ?
W1 B2 2.24(2) 1_545 ?
W1 B2 2.24(2) 16_656 ?
W1 B2 2.24(2) 16_546 ?
W1 B2 2.24(2) 1_655 ?
W1 B2 2.24(2) . ?
B1 W1 2.22(3) 13_666 ?
B1 B1 1.97(3) 13_566 ?
B1 B1 1.97(3) 13_676 ?
B1 B1 1.97(3) 13_666 ?
B1 B2 1.77(5) 16_556 ?
B1 B2 1.854(18) 4_675 ?
B1 B2 1.854(18) 4_665 ?
B1 B2 1.854(18) 4_565 ?
B2 W1 2.24(2) 1_455 ?
B2 W1 2.24(2) 1_565 ?
B2 B1 1.77(5) 16_556 ?
B2 B1 1.854(18) 4_564 ?
B2 B1 1.854(18) 4_664 ?
B2 B1 1.854(18) 4_674 ?

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
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 60.0 1_565 1_455 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 60.0 3_765 3_775 ?
B1 W1 W1 90.000(1) 4_664 1_565 ?
B1 W1 W1 90.000(1) 13_666 3_765 ?
B1 W1 W1 90.000(1) 4_664 3_765 ?
B1 W1 W1 90.000(1) 13_666 1_565 ?
B1 W1 W1 90.000(1) 4_664 1_455 ?
B1 W1 W1 90.000(1) 13_666 3_775 ?
B1 W1 W1 90.000(1) 4_664 3_775 ?
B1 W1 W1 90.000(1) 13_666 1_455 ?
B1 W1 B1 180.0 4_664 13_666 ?
B1 W1 B2 130.9(6) 4_664 16_556 ?
B1 W1 B2 130.9(7) 4_664 16_546 ?
B1 W1 B2 130.9(7) 13_666 1_545 ?
B1 W1 B2 49.1(6) 13_666 16_656 ?
B1 W1 B2 130.9(7) 4_664 16_656 ?
B1 W1 B2 49.1(7) 4_664 1_545 ?
B1 W1 B2 49.1(6) 4_664 1_655 ?
B1 W1 B2 130.9(7) 13_666 . ?
B1 W1 B2 49.1(7) 13_666 16_556 ?
B1 W1 B2 49.1(7) 13_666 16_546 ?
B1 W1 B2 49.1(7) 4_664 . ?
B1 W1 B2 130.9(7) 13_666 1_655 ?
B2 W1 W1 90.000(1) 1_545 3_765 ?
B2 W1 W1 130.9(5) 16_556 3_765 ?
B2 W1 W1 49.1(5) . 1_455 ?
B2 W1 W1 49.1(5) . 1_565 ?
B2 W1 W1 130.9(5) 16_546 3_775 ?
B2 W1 W1 90.0 1_655 1_565 ?
B2 W1 W1 130.9(5) 16_656 1_455 ?
B2 W1 W1 49.1(5) 16_656 3_765 ?
B2 W1 W1 130.9(5) 1_655 1_455 ?
B2 W1 W1 90.000(2) 16_546 1_455 ?
B2 W1 W1 49.1(5) 16_556 1_565 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 130.9(5) 1_545 3_775 ?
B2 W1 W1 130.9(5) . 3_765 ?
B2 W1 W1 49.1(5) 1_655 3_775 ?
B2 W1 W1 49.1(5) 1_655 3_765 ?
B2 W1 W1 90.000(2) . 3_775 ?
B2 W1 W1 49.1(5) 16_556 1_455 ?
B2 W1 W1 90.000(2) 16_556 3_775 ?
B2 W1 W1 90.000(1) 1_545 1_455 ?
B2 W1 W1 130.9(5) 1_545 1_565 ?
B2 W1 W1 130.9(5) 16_546 1_565 ?
B2 W1 W1 49.1(5) 16_656 3_775 ?
B2 W1 W1 90.000(1) 16_546 3_765 ?
B2 W1 B2 81.8(10) 16_656 16_546 ?
B2 W1 B2 135.6(5) 16_546 . ?
B2 W1 B2 81.8(10) 16_546 16_556 ?
B2 W1 B2 81.8(10) 16_656 16_556 ?
B2 W1 B2 135.6(5) 1_545 16_556 ?
B2 W1 B2 81.7(13) 1_545 16_546 ?
B2 W1 B2 81.8(10) 1_545 1_655 ?
B2 W1 B2 135.6(5) 1_655 16_556 ?
B2 W1 B2 135.6(5) 16_656 1_545 ?
B2 W1 B2 81.7(13) . 16_556 ?
B2 W1 B2 81.8(10) 1_545 . ?
B2 W1 B2 81.7(13) 16_656 1_655 ?
B2 W1 B2 81.8(10) 1_655 . ?
B2 W1 B2 135.6(5) 16_656 . ?
B2 W1 B2 135.6(5) 16_546 1_655 ?
B1 B1 W1 120.9(16) 13_566 13_666 ?
B1 B1 W1 120.9(16) 13_676 13_666 ?
B1 B1 W1 120.9(16) 13_666 13_666 ?
B1 B1 B1 96(2) 13_566 13_676 ?
B1 B1 B1 96(2) 13_676 13_666 ?
B1 B1 B1 96(2) 13_566 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 66.0(12) 4_675 13_666 ?
B2 B1 W1 66.0(12) 4_665 13_666 ?
B2 B1 W1 66.0(12) 4_565 13_666 ?
B2 B1 B1 126.9(4) 4_565 13_666 ?
B2 B1 B1 59.1(16) 16_556 13_666 ?
B2 B1 B1 126.9(4) 4_665 13_566 ?
B2 B1 B1 59.1(16) 16_556 13_566 ?
B2 B1 B1 126.9(4) 4_675 13_666 ?
B2 B1 B1 54.8(12) 4_675 13_676 ?
B2 B1 B1 126.9(4) 4_665 13_676 ?
B2 B1 B1 59.1(16) 16_556 13_676 ?
B2 B1 B1 126.9(4) 4_565 13_676 ?
B2 B1 B1 126.9(4) 4_675 13_566 ?
B2 B1 B1 54.8(12) 4_665 13_666 ?
B2 B1 B1 54.8(12) 4_565 13_566 ?
B2 B1 B2 114.0(12) 16_556 4_565 ?
B2 B1 B2 114.0(12) 16_556 4_675 ?
B2 B1 B2 104.6(14) 4_565 4_665 ?
B2 B1 B2 104.6(14) 4_675 4_565 ?
B2 B1 B2 114.0(12) 16_556 4_665 ?
B2 B1 B2 104.6(14) 4_675 4_665 ?
W1 B2 W1 81.8(10) 1_565 1_455 ?
W1 B2 W1 81.8(10) 1_455 . ?
W1 B2 W1 81.8(10) 1_565 . ?
B1 B2 W1 127.7(7) 4_664 1_565 ?
B1 B2 W1 127.7(7) 4_674 . ?
B1 B2 W1 130.9(7) 16_556 . ?
B1 B2 W1 130.9(6) 16_556 1_565 ?
B1 B2 W1 64.8(9) 4_664 . ?
B1 B2 W1 64.8(9) 4_564 1_455 ?
B1 B2 W1 127.7(7) 4_564 . ?
B1 B2 W1 127.7(7) 4_564 1_565 ?
B1 B2 W1 64.8(9) 4_674 1_565 ?
B1 B2 W1 127.7(7) 4_674 1_455 ?
B1 B2 W1 130.9(7) 16_556 1_455 ?
B1 B2 W1 127.7(7) 4_664 1_455 ?
B1 B2 B1 66.0(12) 16_556 4_664 ?
B1 B2 B1 66.0(12) 16_556 4_674 ?
B1 B2 B1 66.0(12) 16_556 4_564 ?
B1 B2 B1 104.6(14) 4_564 4_664 ?
B1 B2 B1 104.6(14) 4_564 4_674 ?
B1 B2 B1 104.6(14) 4_674 4_664 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.461
_oxdiff_exptl_absorpt_empirical_full_min 0.510
_vrf_PLAT029_WB4_2_8GPa          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.540 Why?  
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT911_WB4_2_8GPa          
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         13 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
####################################################################### 
# 
# 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_WB4_8_6GPa
_database_code_depnum_ccdc_archive 'CCDC 2158522'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         8600000
_audit_creation_date             2021-12-13
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.9185(6)
_cell_length_b                   2.9185(6)
_cell_length_c                   10.821(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     79.82(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    109
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      16.5140
_cell_measurement_theta_min      3.2740
_shelx_estimated_absorpt_T_max   0.967
_shelx_estimated_absorpt_T_min   0.967
_exptl_absorpt_coefficient_mu    6.812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    9.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.388
_diffrn_reflns_Laue_measured_fraction_max 0.352
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            181
_diffrn_reflns_point_group_measured_fraction_full 0.388
_diffrn_reflns_point_group_measured_fraction_max 0.352
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         16.812
_diffrn_reflns_theta_min         3.289
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.388
_diffrn_measured_fraction_theta_max 0.352
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -28.00   2.00   0.50    1.00   0.00   0.00   0.00    --    60
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0269434000
_diffrn_orient_matrix_UB_12      0.0172241000
_diffrn_orient_matrix_UB_13      -0.0259476000
_diffrn_orient_matrix_UB_21      0.1115304000
_diffrn_orient_matrix_UB_22      0.0499374000
_diffrn_orient_matrix_UB_23      0.0063666000
_diffrn_orient_matrix_UB_31      -0.0054058000
_diffrn_orient_matrix_UB_32      -0.1018844000
_diffrn_orient_matrix_UB_33      -0.0014013000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                50
_reflns_number_total             57
_reflns_odcompleteness_completeness 31.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.81
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.108
_refine_diff_density_min         -2.400
_refine_diff_density_rms         0.606
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         57
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0368
_refine_ls_restrained_S_all      1.156
_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)+(0.0556P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0849
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.6667 0.3333 0.2500 0.0070(9) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.541(7) 0.008(4) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.114(7) 0.008(4) Uiso 1 6 d S . P . .


_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 W1 2.9185(6) 3_765 ?
W1 W1 2.9185(6) 1_455 ?
W1 W1 2.9185(6) 3_775 ?
W1 W1 2.9185(6) 1_565 ?
W1 B1 2.26(7) 13_666 ?
W1 B1 2.26(7) 4_664 ?
W1 B2 2.24(5) 1_545 ?
W1 B2 2.24(5) . ?
W1 B2 2.24(5) 16_556 ?
W1 B2 2.24(5) 16_546 ?
W1 B2 2.24(5) 1_655 ?
W1 B2 2.24(5) 16_656 ?
B1 W1 2.26(7) 13_666 ?
B1 B1 1.91(7) 13_676 ?
B1 B1 1.91(7) 13_566 ?
B1 B1 1.91(7) 13_666 ?
B1 B2 1.86(4) 4_565 ?
B1 B2 1.68(11) 16_556 ?
B1 B2 1.86(4) 4_675 ?
B1 B2 1.86(4) 4_665 ?
B2 W1 2.24(5) 1_455 ?
B2 W1 2.24(5) 1_565 ?
B2 B1 1.86(4) 4_674 ?
B2 B1 1.86(4) 4_664 ?
B2 B1 1.68(11) 16_556 ?
B2 B1 1.86(4) 4_564 ?

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
W1 W1 W1 60.0 3_765 3_775 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 60.0 1_565 1_455 ?
B1 W1 W1 90.000(2) 4_664 1_455 ?
B1 W1 W1 90.000(3) 4_664 3_775 ?
B1 W1 W1 90.000(2) 13_666 1_455 ?
B1 W1 W1 90.000(2) 4_664 1_565 ?
B1 W1 W1 90.000(2) 13_666 1_565 ?
B1 W1 W1 90.000(2) 13_666 3_765 ?
B1 W1 W1 90.000(2) 4_664 3_765 ?
B1 W1 W1 90.000(3) 13_666 3_775 ?
B1 W1 B1 180.0 4_664 13_666 ?
B2 W1 W1 49.3(10) . 1_565 ?
B2 W1 W1 49.3(10) 1_655 3_775 ?
B2 W1 W1 130.7(10) 16_656 1_455 ?
B2 W1 W1 90.000(5) 16_556 3_775 ?
B2 W1 W1 90.000(2) 16_546 3_765 ?
B2 W1 W1 130.7(10) 16_556 3_765 ?
B2 W1 W1 90.000(3) . 3_775 ?
B2 W1 W1 130.7(10) 16_546 3_775 ?
B2 W1 W1 49.3(10) 16_656 3_765 ?
B2 W1 W1 49.3(10) 16_556 1_455 ?
B2 W1 W1 90.000(2) 1_545 1_455 ?
B2 W1 W1 130.7(10) 16_546 1_565 ?
B2 W1 W1 130.7(10) 1_545 3_775 ?
B2 W1 W1 130.7(10) . 3_765 ?
B2 W1 W1 130.7(10) 1_545 1_565 ?
B2 W1 W1 130.7(10) 1_655 1_455 ?
B2 W1 W1 49.3(10) . 1_455 ?
B2 W1 W1 90.0 1_655 1_565 ?
B2 W1 W1 90.000(3) 1_545 3_765 ?
B2 W1 W1 90.000(3) 16_546 1_455 ?
B2 W1 W1 49.3(10) 16_656 3_775 ?
B2 W1 W1 49.3(10) 16_556 1_565 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 49.3(10) 1_655 3_765 ?
B2 W1 B1 48.8(14) 1_545 4_664 ?
B2 W1 B1 48.8(14) . 4_664 ?
B2 W1 B1 48.8(14) 1_655 4_664 ?
B2 W1 B1 131.2(14) . 13_666 ?
B2 W1 B1 131.2(14) 16_546 4_664 ?
B2 W1 B1 48.8(14) 16_656 13_666 ?
B2 W1 B1 131.2(14) 16_656 4_664 ?
B2 W1 B1 48.8(14) 16_546 13_666 ?
B2 W1 B1 48.8(14) 16_556 13_666 ?
B2 W1 B1 131.2(14) 16_556 4_664 ?
B2 W1 B1 131.2(14) 1_545 13_666 ?
B2 W1 B1 131.2(14) 1_655 13_666 ?
B2 W1 B2 81(2) 16_656 16_556 ?
B2 W1 B2 135.8(10) 16_656 . ?
B2 W1 B2 81(2) 16_546 16_556 ?
B2 W1 B2 82(3) 1_545 16_546 ?
B2 W1 B2 135.8(10) 1_655 16_556 ?
B2 W1 B2 135.8(10) 1_545 16_656 ?
B2 W1 B2 81(2) 1_655 . ?
B2 W1 B2 135.8(10) 16_546 1_655 ?
B2 W1 B2 82(3) . 16_556 ?
B2 W1 B2 81(2) 16_656 16_546 ?
B2 W1 B2 135.8(10) 16_546 . ?
B2 W1 B2 135.8(10) 1_545 16_556 ?
B2 W1 B2 82(3) 16_656 1_655 ?
B2 W1 B2 81(2) 1_545 1_655 ?
B2 W1 B2 81(2) 1_545 . ?
B1 B1 W1 118(4) 13_666 13_666 ?
B1 B1 W1 118(4) 13_566 13_666 ?
B1 B1 W1 118(4) 13_676 13_666 ?
B1 B1 B1 100(5) 13_566 13_676 ?
B1 B1 B1 100(5) 13_676 13_666 ?
B1 B1 B1 100(5) 13_566 13_666 ?
B2 B1 W1 65(3) 4_675 13_666 ?
B2 B1 W1 65(3) 4_565 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 65(3) 4_665 13_666 ?
B2 B1 B1 53(3) 4_665 13_666 ?
B2 B1 B1 53(3) 4_565 13_566 ?
B2 B1 B1 126.7(6) 4_675 13_566 ?
B2 B1 B1 126.7(7) 4_675 13_666 ?
B2 B1 B1 126.7(6) 4_565 13_676 ?
B2 B1 B1 62(4) 16_556 13_666 ?
B2 B1 B1 126.7(6) 4_565 13_666 ?
B2 B1 B1 126.7(7) 4_665 13_676 ?
B2 B1 B1 62(4) 16_556 13_566 ?
B2 B1 B1 53(3) 4_675 13_676 ?
B2 B1 B1 62(4) 16_556 13_676 ?
B2 B1 B1 126.7(7) 4_665 13_566 ?
B2 B1 B2 115(3) 16_556 4_565 ?
B2 B1 B2 104(3) 4_565 4_665 ?
B2 B1 B2 104(3) 4_675 4_565 ?
B2 B1 B2 104(3) 4_675 4_665 ?
B2 B1 B2 115(3) 16_556 4_675 ?
B2 B1 B2 115(3) 16_556 4_665 ?
W1 B2 W1 81(2) 1_565 1_455 ?
W1 B2 W1 81(2) 1_455 . ?
W1 B2 W1 81(2) 1_565 . ?
B1 B2 W1 131.2(14) 16_556 1_455 ?
B1 B2 W1 131.2(14) 16_556 . ?
B1 B2 W1 128.2(14) 4_564 . ?
B1 B2 W1 66(2) 4_664 . ?
B1 B2 W1 128.2(14) 4_664 1_565 ?
B1 B2 W1 128.2(14) 4_674 . ?
B1 B2 W1 66(2) 4_674 1_565 ?
B1 B2 W1 128.2(14) 4_564 1_565 ?
B1 B2 W1 66(2) 4_564 1_455 ?
B1 B2 W1 128.2(14) 4_674 1_455 ?
B1 B2 W1 131.2(14) 16_556 1_565 ?
B1 B2 W1 128.2(14) 4_664 1_455 ?
B1 B2 B1 65(3) 16_556 4_664 ?
B1 B2 B1 104(3) 4_674 4_664 ?
B1 B2 B1 65(3) 16_556 4_674 ?
B1 B2 B1 104(3) 4_564 4_674 ?
B1 B2 B1 65(3) 16_556 4_564 ?
B1 B2 B1 104(3) 4_564 4_664 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.760
_oxdiff_exptl_absorpt_empirical_full_min 0.371
_vrf_PLAT029_WB4_8_6GPa          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.388 Why?  
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT911_WB4_8_6GPa          
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         20 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT971_WB4_8_6GPa          
;
PROBLEM: Check Calcd Resid. Dens.  1.74A   From B1              2.67 eA-3  
RESPONSE: Due to incompleteness of the dataset.
;
####################################################################### 
# 
# 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_WB4_5_9GPa
_database_code_depnum_ccdc_archive 'CCDC 2158521'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         5900000
_audit_creation_date             2021-12-01
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.9240(3)
_cell_length_b                   2.9240(3)
_cell_length_c                   10.861(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     80.42(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    176
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      16.4550
_cell_measurement_theta_min      3.2760
_shelx_estimated_absorpt_T_max   0.967
_shelx_estimated_absorpt_T_min   0.967
_exptl_absorpt_coefficient_mu    6.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    9.379
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.571
_diffrn_reflns_Laue_measured_fraction_max 0.456
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            222
_diffrn_reflns_point_group_measured_fraction_full 0.571
_diffrn_reflns_point_group_measured_fraction_max 0.456
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         17.500
_diffrn_reflns_theta_min         3.283
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.571
_diffrn_measured_fraction_theta_max 0.456
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -10.50  20.00   0.50    1.00   0.00   0.00   0.00    --    61
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0414954000
_diffrn_orient_matrix_UB_12      0.0150914000
_diffrn_orient_matrix_UB_13      -0.0248234000
_diffrn_orient_matrix_UB_21      0.1065113000
_diffrn_orient_matrix_UB_22      0.0617579000
_diffrn_orient_matrix_UB_23      0.0095411000
_diffrn_orient_matrix_UB_31      0.0069683000
_diffrn_orient_matrix_UB_32      -0.0952284000
_diffrn_orient_matrix_UB_33      0.0021951000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                73
_reflns_number_total             82
_reflns_odcompleteness_completeness 44.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     17.50
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.529
_refine_diff_density_min         -1.562
_refine_diff_density_rms         0.403
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         82
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0212
_refine_ls_restrained_S_all      1.122
_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)+(0.0286P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0502
_refine_special_details          ?
_olex2_refinement_description    
;
;
_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 0.6667 0.3333 0.2500 0.0052(2) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.5422(16) 0.0023(15) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.1115(19) 0.0062(18) Uiso 1 6 d S . P . .


_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 W1 2.9240(3) 3_775 ?
W1 W1 2.9240(3) 1_455 ?
W1 W1 2.9240(3) 1_565 ?
W1 W1 2.9240(3) 3_765 ?
W1 B1 2.257(18) 13_666 ?
W1 B1 2.257(18) 4_664 ?
W1 B2 2.261(14) . ?
W1 B2 2.261(14) 1_655 ?
W1 B2 2.261(14) 16_546 ?
W1 B2 2.261(14) 1_545 ?
W1 B2 2.261(14) 16_556 ?
W1 B2 2.261(14) 16_656 ?
B1 W1 2.257(18) 13_666 ?
B1 B1 1.921(17) 13_566 ?
B1 B1 1.921(17) 13_676 ?
B1 B1 1.921(17) 13_666 ?
B1 B2 1.67(3) 16_556 ?
B1 B2 1.848(11) 4_675 ?
B1 B2 1.849(11) 4_665 ?
B1 B2 1.848(11) 4_565 ?
B2 W1 2.261(14) 1_455 ?
B2 W1 2.261(14) 1_565 ?
B2 B1 1.848(11) 4_674 ?
B2 B1 1.848(11) 4_564 ?
B2 B1 1.67(3) 16_556 ?
B2 B1 1.848(11) 4_664 ?

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
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 60.0 1_455 1_565 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 60.0 3_765 3_775 ?
B1 W1 W1 90.000(1) 4_664 3_775 ?
B1 W1 W1 90.0 4_664 1_565 ?
B1 W1 W1 90.0 13_666 1_455 ?
B1 W1 W1 90.0 13_666 3_765 ?
B1 W1 W1 90.000(1) 13_666 3_775 ?
B1 W1 W1 90.000(1) 4_664 3_765 ?
B1 W1 W1 90.0 13_666 1_565 ?
B1 W1 W1 90.000(1) 4_664 1_455 ?
B1 W1 B1 180.0 4_664 13_666 ?
B1 W1 B2 131.7(4) 4_664 16_546 ?
B1 W1 B2 131.7(4) 13_666 . ?
B1 W1 B2 131.7(4) 4_664 16_656 ?
B1 W1 B2 131.7(4) 13_666 1_545 ?
B1 W1 B2 48.3(4) 13_666 16_556 ?
B1 W1 B2 48.3(4) 13_666 16_656 ?
B1 W1 B2 131.7(4) 4_664 16_556 ?
B1 W1 B2 48.3(4) 4_664 1_545 ?
B1 W1 B2 48.3(4) 4_664 1_655 ?
B1 W1 B2 48.3(4) 13_666 16_546 ?
B1 W1 B2 48.3(4) 4_664 . ?
B1 W1 B2 131.7(4) 13_666 1_655 ?
B2 W1 W1 90.000(1) 1_545 3_765 ?
B2 W1 W1 49.7(3) 16_556 1_565 ?
B2 W1 W1 130.3(3) 1_545 1_565 ?
B2 W1 W1 130.3(3) 1_655 1_455 ?
B2 W1 W1 49.7(3) 16_556 1_455 ?
B2 W1 W1 90.0 1_655 1_565 ?
B2 W1 W1 130.3(3) 16_546 1_565 ?
B2 W1 W1 90.0 16_546 3_765 ?
B2 W1 W1 90.000(1) 16_546 1_455 ?
B2 W1 W1 49.7(3) 16_656 3_765 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 49.7(3) . 1_565 ?
B2 W1 W1 90.000(1) 16_556 3_775 ?
B2 W1 W1 49.7(3) . 1_455 ?
B2 W1 W1 90.000(1) . 3_775 ?
B2 W1 W1 130.3(3) 16_546 3_775 ?
B2 W1 W1 90.0 1_545 1_455 ?
B2 W1 W1 130.3(3) 16_556 3_765 ?
B2 W1 W1 49.7(3) 16_656 3_775 ?
B2 W1 W1 130.3(3) 16_656 1_455 ?
B2 W1 W1 130.3(3) 1_545 3_775 ?
B2 W1 W1 130.3(3) . 3_765 ?
B2 W1 W1 49.7(3) 1_655 3_775 ?
B2 W1 W1 49.7(3) 1_655 3_765 ?
B2 W1 B2 80.6(6) 16_656 16_546 ?
B2 W1 B2 136.2(3) 16_546 . ?
B2 W1 B2 83.4(8) 16_556 . ?
B2 W1 B2 83.4(8) 1_545 16_546 ?
B2 W1 B2 80.6(6) 1_655 . ?
B2 W1 B2 80.6(6) 16_546 16_556 ?
B2 W1 B2 136.2(3) 16_656 1_545 ?
B2 W1 B2 83.4(8) 16_656 1_655 ?
B2 W1 B2 136.2(3) 1_545 16_556 ?
B2 W1 B2 80.6(6) 16_656 16_556 ?
B2 W1 B2 136.2(3) 1_655 16_556 ?
B2 W1 B2 136.2(3) 16_656 . ?
B2 W1 B2 136.2(3) 16_546 1_655 ?
B2 W1 B2 80.6(6) 1_545 . ?
B2 W1 B2 80.6(6) 1_545 1_655 ?
B1 B1 W1 118.5(9) 13_566 13_666 ?
B1 B1 W1 118.5(9) 13_676 13_666 ?
B1 B1 W1 118.5(9) 13_666 13_666 ?
B1 B1 B1 99.1(12) 13_566 13_676 ?
B1 B1 B1 99.1(12) 13_676 13_666 ?
B1 B1 B1 99.1(12) 13_566 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 66.0(8) 4_675 13_666 ?
B2 B1 W1 66.0(8) 4_665 13_666 ?
B2 B1 W1 66.0(8) 4_565 13_666 ?
B2 B1 B1 126.56(19) 4_675 13_666 ?
B2 B1 B1 52.5(7) 4_665 13_666 ?
B2 B1 B1 61.5(9) 16_556 13_566 ?
B2 B1 B1 126.56(19) 4_565 13_676 ?
B2 B1 B1 126.56(19) 4_675 13_566 ?
B2 B1 B1 52.5(7) 4_565 13_566 ?
B2 B1 B1 52.5(7) 4_675 13_676 ?
B2 B1 B1 61.5(9) 16_556 13_666 ?
B2 B1 B1 126.56(19) 4_665 13_566 ?
B2 B1 B1 126.56(19) 4_565 13_666 ?
B2 B1 B1 61.5(9) 16_556 13_676 ?
B2 B1 B1 126.56(19) 4_665 13_676 ?
B2 B1 B2 114.0(8) 16_556 4_565 ?
B2 B1 B2 104.5(9) 4_675 4_665 ?
B2 B1 B2 114.0(8) 16_556 4_665 ?
B2 B1 B2 114.0(8) 16_556 4_675 ?
B2 B1 B2 104.5(9) 4_675 4_565 ?
B2 B1 B2 104.5(9) 4_565 4_665 ?
W1 B2 W1 80.6(6) 1_565 1_455 ?
W1 B2 W1 80.6(6) 1_455 . ?
W1 B2 W1 80.6(6) 1_565 . ?
B1 B2 W1 127.7(4) 4_664 1_565 ?
B1 B2 W1 65.7(5) 4_674 1_565 ?
B1 B2 W1 65.7(5) 4_564 1_455 ?
B1 B2 W1 131.7(4) 16_556 1_565 ?
B1 B2 W1 65.7(5) 4_664 . ?
B1 B2 W1 127.7(4) 4_564 . ?
B1 B2 W1 127.7(4) 4_674 . ?
B1 B2 W1 127.7(4) 4_664 1_455 ?
B1 B2 W1 131.7(4) 16_556 . ?
B1 B2 W1 127.7(4) 4_564 1_565 ?
B1 B2 W1 131.7(4) 16_556 1_455 ?
B1 B2 W1 127.7(4) 4_674 1_455 ?
B1 B2 B1 66.0(8) 16_556 4_664 ?
B1 B2 B1 104.5(9) 4_564 4_674 ?
B1 B2 B1 104.5(9) 4_564 4_664 ?
B1 B2 B1 66.0(8) 16_556 4_674 ?
B1 B2 B1 104.5(9) 4_674 4_664 ?
B1 B2 B1 66.0(8) 16_556 4_564 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.074
_oxdiff_exptl_absorpt_empirical_full_min 0.585
_vrf_PLAT029_WB4_5_9GPa          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.571 Why?  
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT911_WB4_5_9GPa          
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         18 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT971_WB4_5_9GPa          
;
PROBLEM: Check Calcd Resid. Dens.  1.11A   From W1              3.39 eA-3  
RESPONSE: Due to incompleteness of the dataset.
;
####################################################################### 
# 
# 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_WB4_12_0GPa
_database_code_depnum_ccdc_archive 'CCDC 2158523'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         12000000
_audit_creation_date             2021-12-01
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.9014(3)
_cell_length_b                   2.9014(3)
_cell_length_c                   10.821(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     78.89(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    190
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      16.5590
_cell_measurement_theta_min      3.2910
_shelx_estimated_absorpt_T_max   0.966
_shelx_estimated_absorpt_T_min   0.966
_exptl_absorpt_coefficient_mu    6.893
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    9.560
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.673
_diffrn_reflns_Laue_measured_fraction_max 0.544
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            353
_diffrn_reflns_point_group_measured_fraction_full 0.673
_diffrn_reflns_point_group_measured_fraction_max 0.544
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         17.623
_diffrn_reflns_theta_min         3.308
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.673
_diffrn_measured_fraction_theta_max 0.544
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -28.00  24.00   0.50    1.00   0.00   0.00   0.00    --   104
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0430798000
_diffrn_orient_matrix_UB_12      0.0164122000
_diffrn_orient_matrix_UB_13      -0.0248638000
_diffrn_orient_matrix_UB_21      0.1067500000
_diffrn_orient_matrix_UB_22      0.0624066000
_diffrn_orient_matrix_UB_23      0.0098401000
_diffrn_orient_matrix_UB_31      0.0077549000
_diffrn_orient_matrix_UB_32      -0.0954884000
_diffrn_orient_matrix_UB_33      0.0020900000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                87
_reflns_number_total             98
_reflns_odcompleteness_completeness 50.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     17.62
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.557
_refine_diff_density_min         -2.411
_refine_diff_density_rms         0.498
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0244
_refine_ls_restrained_S_all      1.170
_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)+(0.0339P)²+0.1693P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0594
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.6667 0.3333 0.2500 0.0063(2) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.546(2) 0.0079(18) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.112(2) 0.0061(16) Uiso 1 6 d S . P . .


_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 W1 2.9014(3) 3_775 ?
W1 W1 2.9014(3) 1_455 ?
W1 W1 2.9014(3) 3_765 ?
W1 W1 2.9014(3) 1_565 ?
W1 B1 2.21(2) 13_666 ?
W1 B1 2.21(2) 4_664 ?
W1 B2 2.244(14) 16_556 ?
W1 B2 2.244(14) 16_656 ?
W1 B2 2.244(14) 1_655 ?
W1 B2 2.244(14) . ?
W1 B2 2.244(14) 16_546 ?
W1 B2 2.244(14) 1_545 ?
B1 W1 2.21(2) 13_666 ?
B1 B1 1.95(2) 13_566 ?
B1 B1 1.95(2) 13_676 ?
B1 B1 1.95(2) 13_666 ?
B1 B2 1.71(3) 16_556 ?
B1 B2 1.822(13) 4_675 ?
B1 B2 1.822(13) 4_665 ?
B1 B2 1.822(13) 4_565 ?
B2 W1 2.244(14) 1_455 ?
B2 W1 2.244(14) 1_565 ?
B2 B1 1.822(13) 4_664 ?
B2 B1 1.822(13) 4_564 ?
B2 B1 1.822(13) 4_674 ?
B2 B1 1.71(3) 16_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 60.0 1_565 1_455 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 60.0 3_765 3_775 ?
B1 W1 W1 90.000(1) 13_666 1_455 ?
B1 W1 W1 90.000(1) 4_664 3_765 ?
B1 W1 W1 90.000(1) 4_664 1_455 ?
B1 W1 W1 90.000(2) 13_666 3_775 ?
B1 W1 W1 90.000(1) 13_666 1_565 ?
B1 W1 W1 90.000(1) 13_666 3_765 ?
B1 W1 W1 90.000(1) 4_664 1_565 ?
B1 W1 W1 90.000(1) 4_664 3_775 ?
B1 W1 B1 180.0 4_664 13_666 ?
B1 W1 B2 48.3(4) 4_664 1_655 ?
B1 W1 B2 48.3(4) 4_664 . ?
B1 W1 B2 48.3(4) 4_664 1_545 ?
B1 W1 B2 131.7(4) 13_666 . ?
B1 W1 B2 48.3(4) 13_666 16_656 ?
B1 W1 B2 131.7(4) 4_664 16_656 ?
B1 W1 B2 131.7(4) 4_664 16_546 ?
B1 W1 B2 131.7(4) 13_666 1_545 ?
B1 W1 B2 131.7(4) 4_664 16_556 ?
B1 W1 B2 48.3(4) 13_666 16_546 ?
B1 W1 B2 48.3(4) 13_666 16_556 ?
B1 W1 B2 131.7(4) 13_666 1_655 ?
B2 W1 W1 90.000(1) 1_545 3_765 ?
B2 W1 W1 49.7(3) 16_656 3_765 ?
B2 W1 W1 90.0 16_546 3_765 ?
B2 W1 W1 130.3(3) . 3_765 ?
B2 W1 W1 49.7(3) 16_556 1_455 ?
B2 W1 W1 49.7(3) 16_556 1_565 ?
B2 W1 W1 130.3(3) 16_546 1_565 ?
B2 W1 W1 49.7(3) . 1_455 ?
B2 W1 W1 130.3(3) 16_656 1_455 ?
B2 W1 W1 130.3(3) 16_556 3_765 ?
B2 W1 W1 130.3(3) 1_655 1_455 ?
B2 W1 W1 130.3(3) 16_546 3_775 ?
B2 W1 W1 130.3(3) 1_545 1_565 ?
B2 W1 W1 90.0 1_655 1_565 ?
B2 W1 W1 49.7(3) 16_656 3_775 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 130.3(3) 1_545 3_775 ?
B2 W1 W1 49.7(3) . 1_565 ?
B2 W1 W1 49.7(3) 1_655 3_775 ?
B2 W1 W1 49.7(3) 1_655 3_765 ?
B2 W1 W1 90.000(1) . 3_775 ?
B2 W1 W1 90.000(1) 16_546 1_455 ?
B2 W1 W1 90.000(1) 16_556 3_775 ?
B2 W1 W1 90.0 1_545 1_455 ?
B2 W1 B2 80.5(6) 16_656 16_546 ?
B2 W1 B2 136.2(3) 1_655 16_556 ?
B2 W1 B2 83.4(8) 16_656 1_655 ?
B2 W1 B2 136.2(3) 16_656 . ?
B2 W1 B2 136.2(3) 16_546 . ?
B2 W1 B2 136.2(3) 1_545 16_556 ?
B2 W1 B2 80.5(6) 1_655 . ?
B2 W1 B2 80.5(6) 16_546 16_556 ?
B2 W1 B2 136.2(3) 16_546 1_655 ?
B2 W1 B2 80.5(6) 16_656 16_556 ?
B2 W1 B2 80.5(6) 1_545 1_655 ?
B2 W1 B2 83.4(8) . 16_556 ?
B2 W1 B2 136.2(3) 16_656 1_545 ?
B2 W1 B2 83.4(8) 1_545 16_546 ?
B2 W1 B2 80.5(6) 1_545 . ?
B1 B1 W1 120.6(12) 13_566 13_666 ?
B1 B1 W1 120.6(12) 13_676 13_666 ?
B1 B1 W1 120.6(12) 13_666 13_666 ?
B1 B1 B1 96.4(15) 13_566 13_676 ?
B1 B1 B1 96.4(15) 13_676 13_666 ?
B1 B1 B1 96.4(15) 13_566 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 66.8(10) 4_675 13_666 ?
B2 B1 W1 66.8(10) 4_665 13_666 ?
B2 B1 W1 66.8(10) 4_565 13_666 ?
B2 B1 B1 126.6(3) 4_565 13_676 ?
B2 B1 B1 53.8(8) 4_565 13_566 ?
B2 B1 B1 126.6(3) 4_675 13_566 ?
B2 B1 B1 126.6(3) 4_565 13_666 ?
B2 B1 B1 126.6(3) 4_665 13_566 ?
B2 B1 B1 59.4(12) 16_556 13_666 ?
B2 B1 B1 59.4(12) 16_556 13_676 ?
B2 B1 B1 53.8(8) 4_675 13_676 ?
B2 B1 B1 126.6(3) 4_675 13_666 ?
B2 B1 B1 59.4(12) 16_556 13_566 ?
B2 B1 B1 126.6(3) 4_665 13_676 ?
B2 B1 B1 53.8(8) 4_665 13_666 ?
B2 B1 B2 113.2(10) 16_556 4_565 ?
B2 B1 B2 113.2(10) 16_556 4_665 ?
B2 B1 B2 113.2(10) 16_556 4_675 ?
B2 B1 B2 105.5(11) 4_565 4_665 ?
B2 B1 B2 105.5(11) 4_675 4_665 ?
B2 B1 B2 105.5(11) 4_675 4_565 ?
W1 B2 W1 80.5(6) 1_565 1_455 ?
W1 B2 W1 80.5(6) 1_455 . ?
W1 B2 W1 80.5(6) 1_565 . ?
B1 B2 W1 131.7(4) 16_556 1_565 ?
B1 B2 W1 64.9(7) 4_564 1_455 ?
B1 B2 W1 127.2(6) 4_674 . ?
B1 B2 W1 127.2(6) 4_664 1_565 ?
B1 B2 W1 131.7(4) 16_556 1_455 ?
B1 B2 W1 64.9(7) 4_674 1_565 ?
B1 B2 W1 131.7(4) 16_556 . ?
B1 B2 W1 127.2(6) 4_674 1_455 ?
B1 B2 W1 127.2(6) 4_564 . ?
B1 B2 W1 127.2(6) 4_664 1_455 ?
B1 B2 W1 64.9(7) 4_664 . ?
B1 B2 W1 127.2(6) 4_564 1_565 ?
B1 B2 B1 66.8(10) 16_556 4_664 ?
B1 B2 B1 66.8(10) 16_556 4_564 ?
B1 B2 B1 105.5(11) 4_564 4_674 ?
B1 B2 B1 105.5(11) 4_674 4_664 ?
B1 B2 B1 105.5(11) 4_564 4_664 ?
B1 B2 B1 66.8(10) 16_556 4_674 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.662
_oxdiff_exptl_absorpt_empirical_full_min 0.388
_vrf_PLAT029_WB4_12_0GPa         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.673 Why?  
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT911_WB4_12_0GPa         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         13 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT972_WB4_12_0GPa         
;
PROBLEM: Check Calcd Resid. Dens.  1.79A   From B2             -3.13 eA-3  
RESPONSE: Due to incompleteness of the dataset
;
####################################################################### 
# 
# 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_WB4_16_5GPa
_database_code_depnum_ccdc_archive 'CCDC 2158524'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         16500000
_audit_creation_date             2021-12-07
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.8905(3)
_cell_length_b                   2.8905(3)
_cell_length_c                   10.793(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     78.10(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    206
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      17.3220
_cell_measurement_theta_min      3.3100
_shelx_estimated_absorpt_T_max   0.966
_shelx_estimated_absorpt_T_min   0.966
_exptl_absorpt_coefficient_mu    6.963
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    9.657
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.592
_diffrn_reflns_Laue_measured_fraction_max 0.620
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            261
_diffrn_reflns_point_group_measured_fraction_full 0.592
_diffrn_reflns_point_group_measured_fraction_max 0.620
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         13.974
_diffrn_reflns_theta_min         3.321
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.592
_diffrn_measured_fraction_theta_max 0.620
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -28.00  28.00   0.50    1.00   0.00   0.00   0.00    --   112
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0432757000
_diffrn_orient_matrix_UB_12      0.0164195000
_diffrn_orient_matrix_UB_13      -0.0248425000
_diffrn_orient_matrix_UB_21      0.1072477000
_diffrn_orient_matrix_UB_22      0.0630873000
_diffrn_orient_matrix_UB_23      0.0098911000
_diffrn_orient_matrix_UB_31      0.0081172000
_diffrn_orient_matrix_UB_32      -0.0957396000
_diffrn_orient_matrix_UB_33      0.0021836000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                56
_reflns_number_total             62
_reflns_odcompleteness_completeness 51.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     17.31
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.820
_refine_diff_density_min         -2.259
_refine_diff_density_rms         0.484
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         62
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0251
_refine_ls_restrained_S_all      1.105
_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)+(0.0386P)²+0.7430P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0601
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.6667 0.3333 0.2500 0.0049(4) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.547(3) 0.005(3) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.111(3) 0.003(2) Uiso 1 6 d S . P . .


_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 W1 2.8905(3) 3_775 ?
W1 W1 2.8905(3) 1_455 ?
W1 W1 2.8905(3) 1_565 ?
W1 W1 2.8905(3) 3_765 ?
W1 B1 2.19(3) 13_666 ?
W1 B1 2.19(3) 4_664 ?
W1 B2 2.244(19) . ?
W1 B2 2.244(19) 16_546 ?
W1 B2 2.244(19) 16_556 ?
W1 B2 2.244(19) 16_656 ?
W1 B2 2.244(19) 1_545 ?
W1 B2 2.244(19) 1_655 ?
B1 W1 2.19(3) 13_666 ?
B1 B1 1.96(3) 13_566 ?
B1 B1 1.96(3) 13_676 ?
B1 B1 1.96(3) 13_666 ?
B1 B2 1.71(4) 16_556 ?
B1 B2 1.805(16) 4_665 ?
B1 B2 1.805(17) 4_675 ?
B1 B2 1.805(17) 4_565 ?
B2 W1 2.244(19) 1_455 ?
B2 W1 2.244(19) 1_565 ?
B2 B1 1.805(17) 4_674 ?
B2 B1 1.805(16) 4_564 ?
B2 B1 1.71(4) 16_556 ?
B2 B1 1.805(16) 4_664 ?

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
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 60.0 1_455 1_565 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 60.0 3_765 3_775 ?
B1 W1 W1 90.000(1) 4_664 3_775 ?
B1 W1 W1 90.000(1) 13_666 1_455 ?
B1 W1 W1 90.000(1) 13_666 3_775 ?
B1 W1 W1 90.000(1) 4_664 3_765 ?
B1 W1 W1 90.000(1) 13_666 3_765 ?
B1 W1 W1 90.000(1) 4_664 1_565 ?
B1 W1 W1 90.000(1) 13_666 1_565 ?
B1 W1 W1 90.000(1) 4_664 1_455 ?
B1 W1 B1 180.0 4_664 13_666 ?
B1 W1 B2 131.9(5) 13_666 1_545 ?
B1 W1 B2 131.9(6) 4_664 16_656 ?
B1 W1 B2 48.1(5) 4_664 1_655 ?
B1 W1 B2 131.9(5) 13_666 . ?
B1 W1 B2 131.9(5) 4_664 16_556 ?
B1 W1 B2 131.9(5) 4_664 16_546 ?
B1 W1 B2 48.1(5) 4_664 1_545 ?
B1 W1 B2 48.1(5) 4_664 . ?
B1 W1 B2 48.1(5) 13_666 16_556 ?
B1 W1 B2 131.9(6) 13_666 1_655 ?
B1 W1 B2 48.1(5) 13_666 16_656 ?
B1 W1 B2 48.1(5) 13_666 16_546 ?
B2 W1 W1 90.000(1) 1_545 3_765 ?
B2 W1 W1 49.9(4) 16_556 1_455 ?
B2 W1 W1 130.1(4) 1_655 1_455 ?
B2 W1 W1 49.9(4) 16_656 3_765 ?
B2 W1 W1 130.1(4) 16_546 1_565 ?
B2 W1 W1 90.000(1) 16_546 3_765 ?
B2 W1 W1 130.1(4) 16_656 1_455 ?
B2 W1 W1 130.1(4) 16_556 3_765 ?
B2 W1 W1 49.9(4) 1_655 3_765 ?
B2 W1 W1 49.9(4) . 1_565 ?
B2 W1 W1 130.1(4) 1_545 1_565 ?
B2 W1 W1 90.000(1) 16_546 1_455 ?
B2 W1 W1 49.9(4) 16_656 3_775 ?
B2 W1 W1 49.9(4) 16_556 1_565 ?
B2 W1 W1 130.1(4) 1_545 3_775 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 49.9(4) 1_655 3_775 ?
B2 W1 W1 130.1(4) . 3_765 ?
B2 W1 W1 90.000(2) 16_556 3_775 ?
B2 W1 W1 90.0 1_655 1_565 ?
B2 W1 W1 90.000(2) . 3_775 ?
B2 W1 W1 130.1(4) 16_546 3_775 ?
B2 W1 W1 90.000(1) 1_545 1_455 ?
B2 W1 W1 49.9(4) . 1_455 ?
B2 W1 B2 80.2(8) 16_656 16_546 ?
B2 W1 B2 136.3(4) 16_656 . ?
B2 W1 B2 83.9(11) 1_545 16_546 ?
B2 W1 B2 80.2(8) 1_655 . ?
B2 W1 B2 83.9(11) 16_556 . ?
B2 W1 B2 83.9(11) 16_656 1_655 ?
B2 W1 B2 136.3(4) 16_546 1_655 ?
B2 W1 B2 80.2(8) 16_656 16_556 ?
B2 W1 B2 80.2(8) 1_545 1_655 ?
B2 W1 B2 80.2(8) 16_546 16_556 ?
B2 W1 B2 136.3(4) 16_656 1_545 ?
B2 W1 B2 80.2(8) 1_545 . ?
B2 W1 B2 136.3(4) 1_545 16_556 ?
B2 W1 B2 136.3(4) 16_546 . ?
B2 W1 B2 136.3(4) 1_655 16_556 ?
B1 B1 W1 121.5(15) 13_566 13_666 ?
B1 B1 W1 121.5(15) 13_676 13_666 ?
B1 B1 W1 121.5(15) 13_666 13_666 ?
B1 B1 B1 95(2) 13_566 13_676 ?
B1 B1 B1 95(2) 13_566 13_666 ?
B1 B1 B1 95(2) 13_676 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 67.6(13) 4_665 13_666 ?
B2 B1 W1 67.6(13) 4_675 13_666 ?
B2 B1 W1 67.6(13) 4_565 13_666 ?
B2 B1 B1 53.9(10) 4_665 13_666 ?
B2 B1 B1 58.5(15) 16_556 13_566 ?
B2 B1 B1 53.9(10) 4_675 13_676 ?
B2 B1 B1 53.9(10) 4_565 13_566 ?
B2 B1 B1 58.5(15) 16_556 13_676 ?
B2 B1 B1 126.4(4) 4_675 13_566 ?
B2 B1 B1 126.4(4) 4_675 13_666 ?
B2 B1 B1 126.4(4) 4_665 13_566 ?
B2 B1 B1 126.4(4) 4_665 13_676 ?
B2 B1 B1 58.5(15) 16_556 13_666 ?
B2 B1 B1 126.4(4) 4_565 13_676 ?
B2 B1 B1 126.4(4) 4_565 13_666 ?
B2 B1 B2 112.4(13) 16_556 4_565 ?
B2 B1 B2 106.4(14) 4_675 4_565 ?
B2 B1 B2 106.4(14) 4_675 4_665 ?
B2 B1 B2 112.4(13) 16_556 4_665 ?
B2 B1 B2 106.4(14) 4_565 4_665 ?
B2 B1 B2 112.4(13) 16_556 4_675 ?
W1 B2 W1 80.2(8) 1_565 1_455 ?
W1 B2 W1 80.2(8) 1_455 . ?
W1 B2 W1 80.2(8) 1_565 . ?
B1 B2 W1 64.3(10) 4_664 . ?
B1 B2 W1 126.7(8) 4_564 . ?
B1 B2 W1 64.3(10) 4_674 1_565 ?
B1 B2 W1 131.9(5) 16_556 1_455 ?
B1 B2 W1 131.9(5) 16_556 1_565 ?
B1 B2 W1 131.9(5) 16_556 . ?
B1 B2 W1 64.3(10) 4_564 1_455 ?
B1 B2 W1 126.7(8) 4_664 1_455 ?
B1 B2 W1 126.7(8) 4_674 . ?
B1 B2 W1 126.7(8) 4_564 1_565 ?
B1 B2 W1 126.7(8) 4_664 1_565 ?
B1 B2 W1 126.7(8) 4_674 1_455 ?
B1 B2 B1 67.6(13) 16_556 4_664 ?
B1 B2 B1 106.4(14) 4_564 4_664 ?
B1 B2 B1 106.4(14) 4_674 4_664 ?
B1 B2 B1 67.6(13) 16_556 4_564 ?
B1 B2 B1 67.6(13) 16_556 4_674 ?
B1 B2 B1 106.4(14) 4_564 4_674 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.004
_oxdiff_exptl_absorpt_empirical_full_min 0.646
_vrf_PLAT911_WB4_16_5GPa         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         15 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT971_WB4_16_5GPa         
;
PROBLEM: Check Calcd Resid. Dens.  1.66A   From W1              3.27 eA-3  
RESPONSE: Due to incompleteness of the dataset.
;
_vrf_PLAT972_WB4_16_5GPa         
;
PROBLEM: Check Calcd Resid. Dens.  1.79A   From W1             -3.08 eA-3  
RESPONSE: Due to incompleteness of the dataset.
;
####################################################################### 
# 
# 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_WB4_21_4GPa
_database_code_depnum_ccdc_archive 'CCDC 2158525'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         21400000
_audit_creation_date             2021-12-06
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.8726(2)
_cell_length_b                   2.8726(2)
_cell_length_c                   10.730(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     76.68(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    229
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      16.7510
_cell_measurement_theta_min      3.4390
_shelx_estimated_absorpt_T_max   0.965
_shelx_estimated_absorpt_T_min   0.965
_exptl_absorpt_coefficient_mu    7.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    9.835
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.583
_diffrn_reflns_Laue_measured_fraction_max 0.603
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            242
_diffrn_reflns_point_group_measured_fraction_full 0.583
_diffrn_reflns_point_group_measured_fraction_max 0.603
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         15.246
_diffrn_reflns_theta_min         3.341
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.583
_diffrn_measured_fraction_theta_max 0.603
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -28.00  14.50   0.50    1.00   0.00   0.00   0.00    --    85
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0437747000
_diffrn_orient_matrix_UB_12      0.0167080000
_diffrn_orient_matrix_UB_13      -0.0249845000
_diffrn_orient_matrix_UB_21      0.1078241000
_diffrn_orient_matrix_UB_22      0.0634950000
_diffrn_orient_matrix_UB_23      0.0100109000
_diffrn_orient_matrix_UB_31      0.0082181000
_diffrn_orient_matrix_UB_32      -0.0962702000
_diffrn_orient_matrix_UB_33      0.0021612000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                67
_reflns_number_total             73
_reflns_odcompleteness_completeness 55.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.75
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.500
_refine_diff_density_min         -2.448
_refine_diff_density_rms         0.583
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.356
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         73
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0281
_refine_ls_restrained_S_all      1.356
_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)+(0.0381P)²+0.0545P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0694
_refine_special_details          ?
_olex2_refinement_description    
;
;
_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 0.6667 0.3333 0.2500 0.0038(3) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.545(3) 0.004(2) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.115(3) 0.006(2) Uiso 1 6 d S . P . .


_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 W1 2.8726(2) 3_765 ?
W1 W1 2.8726(2) 1_455 ?
W1 W1 2.8726(2) 3_775 ?
W1 W1 2.8726(2) 1_565 ?
W1 B1 2.20(3) 13_666 ?
W1 B1 2.20(3) 4_664 ?
W1 B2 2.20(2) 16_656 ?
W1 B2 2.20(2) . ?
W1 B2 2.20(2) 16_556 ?
W1 B2 2.20(2) 16_546 ?
W1 B2 2.20(2) 1_655 ?
W1 B2 2.20(2) 1_545 ?
B1 W1 2.20(3) 13_666 ?
B1 B1 1.92(3) 13_676 ?
B1 B1 1.92(3) 13_566 ?
B1 B1 1.92(3) 13_666 ?
B1 B2 1.822(18) 4_565 ?
B1 B2 1.71(4) 16_556 ?
B1 B2 1.822(18) 4_675 ?
B1 B2 1.822(18) 4_665 ?
B2 W1 2.20(2) 1_455 ?
B2 W1 2.20(2) 1_565 ?
B2 B1 1.822(18) 4_674 ?
B2 B1 1.822(18) 4_664 ?
B2 B1 1.71(4) 16_556 ?
B2 B1 1.822(18) 4_564 ?

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
W1 W1 W1 60.0 3_765 3_775 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 60.0 1_565 1_455 ?
B1 W1 W1 90.000(1) 4_664 1_455 ?
B1 W1 W1 90.000(1) 4_664 3_775 ?
B1 W1 W1 90.000(1) 13_666 1_455 ?
B1 W1 W1 90.000(1) 4_664 1_565 ?
B1 W1 W1 90.000(1) 13_666 1_565 ?
B1 W1 W1 90.000(1) 13_666 3_765 ?
B1 W1 W1 90.000(1) 4_664 3_765 ?
B1 W1 W1 90.000(1) 13_666 3_775 ?
B1 W1 B1 180.0 4_664 13_666 ?
B2 W1 W1 49.3(4) . 1_565 ?
B2 W1 W1 49.3(4) 1_655 3_775 ?
B2 W1 W1 90.000(1) 1_545 1_455 ?
B2 W1 W1 90.000(2) 16_556 3_775 ?
B2 W1 W1 90.000(1) 16_546 3_765 ?
B2 W1 W1 130.7(4) 16_556 3_765 ?
B2 W1 W1 90.000(2) . 3_775 ?
B2 W1 W1 130.7(4) 16_546 3_775 ?
B2 W1 W1 90.000(1) 1_545 3_765 ?
B2 W1 W1 49.3(4) 16_556 1_455 ?
B2 W1 W1 130.7(4) 16_656 1_455 ?
B2 W1 W1 130.7(4) 16_546 1_565 ?
B2 W1 W1 49.3(4) 16_656 3_775 ?
B2 W1 W1 130.7(4) . 3_765 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 130.7(4) 1_655 1_455 ?
B2 W1 W1 49.3(4) . 1_455 ?
B2 W1 W1 90.0 1_655 1_565 ?
B2 W1 W1 49.3(4) 16_656 3_765 ?
B2 W1 W1 90.000(1) 16_546 1_455 ?
B2 W1 W1 130.7(4) 1_545 3_775 ?
B2 W1 W1 49.3(5) 16_556 1_565 ?
B2 W1 W1 130.7(4) 1_545 1_565 ?
B2 W1 W1 49.3(4) 1_655 3_765 ?
B2 W1 B1 131.1(6) 16_656 4_664 ?
B2 W1 B1 48.9(6) . 4_664 ?
B2 W1 B1 48.9(6) 1_655 4_664 ?
B2 W1 B1 131.1(6) . 13_666 ?
B2 W1 B1 131.1(6) 16_546 4_664 ?
B2 W1 B1 131.1(6) 1_545 13_666 ?
B2 W1 B1 48.9(6) 1_545 4_664 ?
B2 W1 B1 48.9(6) 16_546 13_666 ?
B2 W1 B1 48.9(6) 16_556 13_666 ?
B2 W1 B1 131.1(6) 16_556 4_664 ?
B2 W1 B1 48.9(6) 16_656 13_666 ?
B2 W1 B1 131.1(6) 1_655 13_666 ?
B2 W1 B2 135.8(4) 1_545 16_556 ?
B2 W1 B2 81.4(9) 1_545 . ?
B2 W1 B2 81.4(9) 16_546 16_556 ?
B2 W1 B2 81.4(9) 16_656 16_546 ?
B2 W1 B2 135.8(4) 1_655 16_556 ?
B2 W1 B2 135.8(4) 16_656 1_545 ?
B2 W1 B2 81.4(9) 1_655 . ?
B2 W1 B2 135.8(4) 16_546 1_655 ?
B2 W1 B2 82.3(12) . 16_556 ?
B2 W1 B2 82.3(12) 1_545 16_546 ?
B2 W1 B2 135.8(4) 16_546 . ?
B2 W1 B2 81.4(9) 16_656 16_556 ?
B2 W1 B2 81.4(9) 1_545 1_655 ?
B2 W1 B2 82.3(12) 16_656 1_655 ?
B2 W1 B2 135.8(4) 16_656 . ?
B1 B1 W1 120.1(15) 13_666 13_666 ?
B1 B1 W1 120.1(15) 13_566 13_666 ?
B1 B1 W1 120.1(15) 13_676 13_666 ?
B1 B1 B1 97(2) 13_566 13_676 ?
B1 B1 B1 97(2) 13_676 13_666 ?
B1 B1 B1 97(2) 13_566 13_666 ?
B2 B1 W1 65.6(12) 4_675 13_666 ?
B2 B1 W1 65.6(12) 4_565 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 65.6(12) 4_665 13_666 ?
B2 B1 B1 54.5(11) 4_665 13_666 ?
B2 B1 B1 54.5(11) 4_565 13_566 ?
B2 B1 B1 127.0(3) 4_675 13_566 ?
B2 B1 B1 127.0(3) 4_675 13_666 ?
B2 B1 B1 127.0(3) 4_565 13_676 ?
B2 B1 B1 59.9(15) 16_556 13_666 ?
B2 B1 B1 127.0(3) 4_565 13_666 ?
B2 B1 B1 127.0(3) 4_665 13_676 ?
B2 B1 B1 59.9(15) 16_556 13_566 ?
B2 B1 B1 54.5(11) 4_675 13_676 ?
B2 B1 B1 59.9(15) 16_556 13_676 ?
B2 B1 B1 127.0(3) 4_665 13_566 ?
B2 B1 B2 114.4(12) 16_556 4_565 ?
B2 B1 B2 104.1(15) 4_565 4_665 ?
B2 B1 B2 104.1(15) 4_675 4_565 ?
B2 B1 B2 104.1(15) 4_675 4_665 ?
B2 B1 B2 114.4(13) 16_556 4_675 ?
B2 B1 B2 114.4(12) 16_556 4_665 ?
W1 B2 W1 81.4(9) 1_565 1_455 ?
W1 B2 W1 81.4(9) 1_455 . ?
W1 B2 W1 81.4(9) 1_565 . ?
B1 B2 W1 131.1(6) 16_556 1_455 ?
B1 B2 W1 131.1(6) 16_556 . ?
B1 B2 W1 128.0(7) 4_564 . ?
B1 B2 W1 65.6(9) 4_664 . ?
B1 B2 W1 128.0(7) 4_664 1_565 ?
B1 B2 W1 128.0(7) 4_674 . ?
B1 B2 W1 65.6(9) 4_674 1_565 ?
B1 B2 W1 128.0(7) 4_564 1_565 ?
B1 B2 W1 65.6(9) 4_564 1_455 ?
B1 B2 W1 128.0(7) 4_674 1_455 ?
B1 B2 W1 131.1(6) 16_556 1_565 ?
B1 B2 W1 128.0(7) 4_664 1_455 ?
B1 B2 B1 65.6(12) 16_556 4_664 ?
B1 B2 B1 104.1(15) 4_674 4_664 ?
B1 B2 B1 65.6(12) 16_556 4_674 ?
B1 B2 B1 104.1(15) 4_564 4_674 ?
B1 B2 B1 65.6(12) 16_556 4_564 ?
B1 B2 B1 104.1(15) 4_564 4_664 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.725
_oxdiff_exptl_absorpt_empirical_full_min 0.362
_vrf_PLAT911_WB4_21_4GPa         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         17 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT972_WB4_21_4GPa         
;
PROBLEM: Check Calcd Resid. Dens.  0.89A   From B1             -2.93 eA-3  
RESPONSE: Due to incompleteness of the dataset.
;
####################################################################### 
# 
# 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_WB4_25_9GPa
_database_code_depnum_ccdc_archive 'CCDC 2158526'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         25900000
_audit_creation_date             2021-12-06
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.8625(3)
_cell_length_b                   2.8625(3)
_cell_length_c                   10.713(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     76.02(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    172
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      15.6370
_cell_measurement_theta_min      3.3410
_shelx_estimated_absorpt_T_max   0.965
_shelx_estimated_absorpt_T_min   0.965
_exptl_absorpt_coefficient_mu    7.153
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    9.921
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.562
_diffrn_reflns_Laue_measured_fraction_max 0.596
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            276
_diffrn_reflns_point_group_measured_fraction_full 0.562
_diffrn_reflns_point_group_measured_fraction_max 0.596
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         13.737
_diffrn_reflns_theta_min         3.442
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.562
_diffrn_measured_fraction_theta_max 0.596
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -28.00  28.00   0.50    1.00   0.00   0.00   0.00    --   112
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0444285000
_diffrn_orient_matrix_UB_12      0.0169319000
_diffrn_orient_matrix_UB_13      -0.0249459000
_diffrn_orient_matrix_UB_21      0.1079517000
_diffrn_orient_matrix_UB_22      0.0637117000
_diffrn_orient_matrix_UB_23      0.0101735000
_diffrn_orient_matrix_UB_31      0.0082629000
_diffrn_orient_matrix_UB_32      -0.0966526000
_diffrn_orient_matrix_UB_33      0.0022451000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                51
_reflns_number_total             56
_reflns_odcompleteness_completeness 54.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.80
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.584
_refine_diff_density_min         -2.604
_refine_diff_density_rms         0.556
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0370
_refine_ls_restrained_S_all      1.129
_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)+(0.0428P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0710
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.6667 0.3333 0.2500 0.0062(6) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.550(4) 0.008(4) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.111(4) 0.007(4) Uiso 1 6 d S . P . .


_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 W1 2.8625(3) 3_775 ?
W1 W1 2.8625(3) 3_765 ?
W1 W1 2.8625(3) 1_565 ?
W1 W1 2.8625(3) 1_455 ?
W1 B1 2.15(5) 13_666 ?
W1 B1 2.15(5) 4_664 ?
W1 B2 2.22(3) 16_556 ?
W1 B2 2.22(3) . ?
W1 B2 2.22(3) 1_545 ?
W1 B2 2.22(3) 1_655 ?
W1 B2 2.22(3) 16_656 ?
W1 B2 2.22(3) 16_546 ?
B1 W1 2.15(5) 13_666 ?
B1 B1 1.97(5) 13_566 ?
B1 B1 1.97(5) 13_676 ?
B1 B1 1.97(5) 13_666 ?
B1 B2 1.73(7) 16_556 ?
B1 B2 1.78(2) 4_665 ?
B1 B2 1.78(2) 4_675 ?
B1 B2 1.78(2) 4_565 ?
B2 W1 2.22(3) 1_455 ?
B2 W1 2.22(3) 1_565 ?
B2 B1 1.73(7) 16_556 ?
B2 B1 1.78(2) 4_564 ?
B2 B1 1.78(2) 4_664 ?
B2 B1 1.78(2) 4_674 ?

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
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 60.0 1_565 1_455 ?
W1 W1 W1 60.0 3_765 3_775 ?
B1 W1 W1 90.000(1) 4_664 1_565 ?
B1 W1 W1 90.000(3) 13_666 3_775 ?
B1 W1 W1 90.000(1) 13_666 3_765 ?
B1 W1 W1 90.000(2) 4_664 1_455 ?
B1 W1 W1 90.000(2) 4_664 3_765 ?
B1 W1 W1 90.000(1) 13_666 1_565 ?
B1 W1 W1 90.000(2) 4_664 3_775 ?
B1 W1 W1 90.000(1) 13_666 1_455 ?
B1 W1 B1 180.0 4_664 13_666 ?
B1 W1 B2 48.1(9) 4_664 1_545 ?
B1 W1 B2 48.1(9) 13_666 16_656 ?
B1 W1 B2 131.9(9) 4_664 16_546 ?
B1 W1 B2 131.9(9) 4_664 16_556 ?
B1 W1 B2 48.1(9) 13_666 16_556 ?
B1 W1 B2 48.1(9) 4_664 . ?
B1 W1 B2 131.9(9) 4_664 16_656 ?
B1 W1 B2 48.1(9) 4_664 1_655 ?
B1 W1 B2 131.9(9) 13_666 1_545 ?
B1 W1 B2 131.9(9) 13_666 1_655 ?
B1 W1 B2 131.9(9) 13_666 . ?
B1 W1 B2 48.1(9) 13_666 16_546 ?
B2 W1 W1 90.000(2) 1_545 3_765 ?
B2 W1 W1 130.1(7) . 3_765 ?
B2 W1 W1 49.9(7) 16_556 1_565 ?
B2 W1 W1 49.9(7) . 1_455 ?
B2 W1 W1 130.1(7) 16_556 3_765 ?
B2 W1 W1 90.000(1) 1_545 1_455 ?
B2 W1 W1 130.1(7) 16_546 3_775 ?
B2 W1 W1 90.0 1_655 1_565 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 49.9(7) . 1_565 ?
B2 W1 W1 49.9(7) 1_655 3_765 ?
B2 W1 W1 90.000(2) 16_546 1_455 ?
B2 W1 W1 90.000(3) 16_556 3_775 ?
B2 W1 W1 90.000(1) 16_546 3_765 ?
B2 W1 W1 130.1(7) 1_545 1_565 ?
B2 W1 W1 130.1(7) 16_546 1_565 ?
B2 W1 W1 49.9(7) 16_656 3_775 ?
B2 W1 W1 49.9(7) 16_656 3_765 ?
B2 W1 W1 130.1(7) 1_545 3_775 ?
B2 W1 W1 130.1(7) 16_656 1_455 ?
B2 W1 W1 49.9(7) 1_655 3_775 ?
B2 W1 W1 49.9(7) 16_556 1_455 ?
B2 W1 W1 90.000(2) . 3_775 ?
B2 W1 W1 130.1(7) 1_655 1_455 ?
B2 W1 B2 80.2(14) 16_656 16_546 ?
B2 W1 B2 136.3(7) 16_656 . ?
B2 W1 B2 136.3(7) 1_545 16_556 ?
B2 W1 B2 80.2(14) 16_546 16_556 ?
B2 W1 B2 80.2(14) 16_656 16_556 ?
B2 W1 B2 83.9(18) . 16_556 ?
B2 W1 B2 80.2(14) 1_545 . ?
B2 W1 B2 83.9(18) 1_545 16_546 ?
B2 W1 B2 80.2(14) 1_655 . ?
B2 W1 B2 136.3(7) 1_655 16_556 ?
B2 W1 B2 136.3(7) 16_546 1_655 ?
B2 W1 B2 136.3(7) 16_546 . ?
B2 W1 B2 80.2(14) 1_545 1_655 ?
B2 W1 B2 83.9(18) 16_656 1_655 ?
B2 W1 B2 136.3(7) 16_656 1_545 ?
B1 B1 W1 123(2) 13_566 13_666 ?
B1 B1 W1 123(2) 13_676 13_666 ?
B1 B1 W1 123(2) 13_666 13_666 ?
B1 B1 B1 93(3) 13_566 13_676 ?
B1 B1 B1 93(3) 13_566 13_666 ?
B1 B1 B1 93(3) 13_676 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 68.2(19) 4_665 13_666 ?
B2 B1 W1 68.2(19) 4_675 13_666 ?
B2 B1 W1 68.2(19) 4_565 13_666 ?
B2 B1 B1 126.3(7) 4_665 13_676 ?
B2 B1 B1 126.3(7) 4_565 13_666 ?
B2 B1 B1 57(2) 16_556 13_666 ?
B2 B1 B1 54.6(17) 4_665 13_666 ?
B2 B1 B1 54.6(17) 4_675 13_676 ?
B2 B1 B1 57(2) 16_556 13_566 ?
B2 B1 B1 126.3(7) 4_665 13_566 ?
B2 B1 B1 126.3(7) 4_675 13_566 ?
B2 B1 B1 57(2) 16_556 13_676 ?
B2 B1 B1 54.6(17) 4_565 13_566 ?
B2 B1 B1 126.3(7) 4_675 13_666 ?
B2 B1 B1 126.3(7) 4_565 13_676 ?
B2 B1 B2 111.8(19) 16_556 4_565 ?
B2 B1 B2 107(2) 4_565 4_665 ?
B2 B1 B2 107(2) 4_675 4_565 ?
B2 B1 B2 107(2) 4_675 4_665 ?
B2 B1 B2 111.8(19) 16_556 4_675 ?
B2 B1 B2 111.8(19) 16_556 4_665 ?
W1 B2 W1 80.2(14) 1_565 1_455 ?
W1 B2 W1 80.2(14) 1_455 . ?
W1 B2 W1 80.2(14) 1_565 . ?
B1 B2 W1 131.9(9) 16_556 1_455 ?
B1 B2 W1 131.9(9) 16_556 . ?
B1 B2 W1 126.4(12) 4_564 . ?
B1 B2 W1 63.8(15) 4_664 . ?
B1 B2 W1 126.4(12) 4_664 1_565 ?
B1 B2 W1 126.4(12) 4_674 . ?
B1 B2 W1 63.8(15) 4_674 1_565 ?
B1 B2 W1 126.4(12) 4_564 1_565 ?
B1 B2 W1 63.8(15) 4_564 1_455 ?
B1 B2 W1 126.4(12) 4_674 1_455 ?
B1 B2 W1 131.9(9) 16_556 1_565 ?
B1 B2 W1 126.4(12) 4_664 1_455 ?
B1 B2 B1 68.2(19) 16_556 4_664 ?
B1 B2 B1 107(2) 4_674 4_664 ?
B1 B2 B1 68.2(19) 16_556 4_674 ?
B1 B2 B1 107(2) 4_564 4_674 ?
B1 B2 B1 68.2(19) 16_556 4_564 ?
B1 B2 B1 107(2) 4_564 4_664 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.215
_oxdiff_exptl_absorpt_empirical_full_min 0.597
_vrf_PLAT911_WB4_25_9GPa         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         15 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT971_WB4_25_9GPa         
;
PROBLEM: Check Calcd Resid. Dens.  1.65A   From W1              3.44 eA-3  
RESPONSE:  Due to incompleteness of the dataset.
;
_vrf_PLAT972_WB4_25_9GPa         
;
PROBLEM: Check Calcd Resid. Dens.  1.75A   From B2             -3.20 eA-3  
RESPONSE:  Due to incompleteness of the dataset.
;
####################################################################### 
# 
# 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_WB4_36_5GPa
_database_code_depnum_ccdc_archive 'CCDC 2158528'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         36500000
_audit_creation_date             2021-12-07
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.8307(4)
_cell_length_b                   2.8307(4)
_cell_length_c                   10.619(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     73.69(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    193
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      16.4500
_cell_measurement_theta_min      3.3670
_shelx_estimated_absorpt_T_max   0.964
_shelx_estimated_absorpt_T_min   0.964
_exptl_absorpt_coefficient_mu    7.379
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    10.235
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.617
_diffrn_reflns_Laue_measured_fraction_max 0.605
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            289
_diffrn_reflns_point_group_measured_fraction_full 0.617
_diffrn_reflns_point_group_measured_fraction_max 0.605
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         15.280
_diffrn_reflns_theta_min         3.480
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.617
_diffrn_measured_fraction_theta_max 0.605
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -28.00  28.00   0.50    1.00   0.00   0.00   0.00    --   112
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0461476000
_diffrn_orient_matrix_UB_12      0.0173131000
_diffrn_orient_matrix_UB_13      -0.0251309000
_diffrn_orient_matrix_UB_21      0.1085250000
_diffrn_orient_matrix_UB_22      0.0642546000
_diffrn_orient_matrix_UB_23      0.0104715000
_diffrn_orient_matrix_UB_31      0.0083543000
_diffrn_orient_matrix_UB_32      -0.0976282000
_diffrn_orient_matrix_UB_33      0.0023204000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                67
_reflns_number_total             72
_reflns_odcompleteness_completeness 57.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.73
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.040
_refine_diff_density_min         -1.830
_refine_diff_density_rms         0.491
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         72
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0217
_refine_ls_restrained_S_all      1.181
_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)+(0.0336P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0511
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.6667 0.3333 0.2500 0.0059(3) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.5457(19) 0.0031(16) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.113(2) 0.0059(18) Uiso 1 6 d S . P . .


_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 W1 2.8307(4) 3_775 ?
W1 W1 2.8307(4) 1_565 ?
W1 W1 2.8307(4) 1_455 ?
W1 W1 2.8307(4) 3_765 ?
W1 B1 2.17(2) 13_666 ?
W1 B1 2.17(2) 4_664 ?
W1 B2 2.189(16) 16_556 ?
W1 B2 2.188(16) 16_546 ?
W1 B2 2.189(16) . ?
W1 B2 2.189(16) 16_656 ?
W1 B2 2.189(16) 1_545 ?
W1 B2 2.188(16) 1_655 ?
B1 W1 2.17(2) 13_666 ?
B1 B1 1.90(2) 13_566 ?
B1 B1 1.90(2) 13_676 ?
B1 B1 1.90(2) 13_666 ?
B1 B2 1.68(3) 16_556 ?
B1 B2 1.784(12) 4_665 ?
B1 B2 1.784(12) 4_675 ?
B1 B2 1.784(12) 4_565 ?
B2 W1 2.189(16) 1_455 ?
B2 W1 2.189(16) 1_565 ?
B2 B1 1.784(12) 4_674 ?
B2 B1 1.784(12) 4_564 ?
B2 B1 1.68(3) 16_556 ?
B2 B1 1.784(12) 4_664 ?

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
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 60.0 1_565 1_455 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 60.0 3_765 3_775 ?
B1 W1 W1 90.000(1) 4_664 3_775 ?
B1 W1 W1 90.0 13_666 1_565 ?
B1 W1 W1 90.000(1) 13_666 3_775 ?
B1 W1 W1 90.0 4_664 3_765 ?
B1 W1 W1 90.0 13_666 3_765 ?
B1 W1 W1 90.000(1) 4_664 1_455 ?
B1 W1 W1 90.0 13_666 1_455 ?
B1 W1 W1 90.0 4_664 1_565 ?
B1 W1 B1 180.0 4_664 13_666 ?
B1 W1 B2 131.7(5) 13_666 1_545 ?
B1 W1 B2 131.7(5) 4_664 16_656 ?
B1 W1 B2 48.3(5) 4_664 1_655 ?
B1 W1 B2 48.3(5) 13_666 16_556 ?
B1 W1 B2 48.3(5) 4_664 . ?
B1 W1 B2 131.7(5) 4_664 16_546 ?
B1 W1 B2 48.3(5) 4_664 1_545 ?
B1 W1 B2 131.7(5) 4_664 16_556 ?
B1 W1 B2 131.7(5) 13_666 . ?
B1 W1 B2 131.7(5) 13_666 1_655 ?
B1 W1 B2 48.3(5) 13_666 16_656 ?
B1 W1 B2 48.3(5) 13_666 16_546 ?
B2 W1 W1 90.000(1) 1_545 3_765 ?
B2 W1 W1 49.7(4) . 1_565 ?
B2 W1 W1 90.0 1_655 1_565 ?
B2 W1 W1 49.7(4) 16_656 3_765 ?
B2 W1 W1 90.000(1) 16_546 1_455 ?
B2 W1 W1 90.000(1) 16_546 3_765 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 130.3(4) . 3_765 ?
B2 W1 W1 49.7(4) 1_655 3_765 ?
B2 W1 W1 49.7(4) 16_556 1_455 ?
B2 W1 W1 90.000(1) 1_545 1_455 ?
B2 W1 W1 130.3(4) 16_546 1_565 ?
B2 W1 W1 49.7(4) 16_656 3_775 ?
B2 W1 W1 49.7(4) . 1_455 ?
B2 W1 W1 130.3(4) 1_545 3_775 ?
B2 W1 W1 130.3(4) 16_656 1_455 ?
B2 W1 W1 49.7(4) 1_655 3_775 ?
B2 W1 W1 130.3(4) 16_556 3_765 ?
B2 W1 W1 90.000(1) . 3_775 ?
B2 W1 W1 130.3(4) 1_655 1_455 ?
B2 W1 W1 90.000(1) 16_556 3_775 ?
B2 W1 W1 130.3(4) 16_546 3_775 ?
B2 W1 W1 130.3(4) 1_545 1_565 ?
B2 W1 W1 49.7(4) 16_556 1_565 ?
B2 W1 B2 80.6(7) 16_656 16_546 ?
B2 W1 B2 80.6(7) 16_656 16_556 ?
B2 W1 B2 83.4(9) 1_545 16_546 ?
B2 W1 B2 136.2(3) 1_655 16_556 ?
B2 W1 B2 83.4(9) . 16_556 ?
B2 W1 B2 83.4(9) 16_656 1_655 ?
B2 W1 B2 136.2(3) 16_546 1_655 ?
B2 W1 B2 136.2(3) 16_656 . ?
B2 W1 B2 80.6(7) 1_545 1_655 ?
B2 W1 B2 136.2(3) 16_546 . ?
B2 W1 B2 136.2(3) 16_656 1_545 ?
B2 W1 B2 136.2(3) 1_545 16_556 ?
B2 W1 B2 80.6(7) 1_545 . ?
B2 W1 B2 80.6(7) 16_546 16_556 ?
B2 W1 B2 80.6(7) 1_655 . ?
B1 B1 W1 120.7(11) 13_566 13_666 ?
B1 B1 W1 120.7(11) 13_676 13_666 ?
B1 B1 W1 120.7(11) 13_666 13_666 ?
B1 B1 B1 96.3(14) 13_566 13_676 ?
B1 B1 B1 96.3(14) 13_566 13_666 ?
B1 B1 B1 96.3(14) 13_676 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 66.4(9) 4_665 13_666 ?
B2 B1 W1 66.4(9) 4_675 13_666 ?
B2 B1 W1 66.4(9) 4_565 13_666 ?
B2 B1 B1 54.3(8) 4_665 13_666 ?
B2 B1 B1 59.3(11) 16_556 13_566 ?
B2 B1 B1 54.3(9) 4_675 13_676 ?
B2 B1 B1 54.3(8) 4_565 13_566 ?
B2 B1 B1 59.3(11) 16_556 13_676 ?
B2 B1 B1 126.8(3) 4_675 13_566 ?
B2 B1 B1 126.8(3) 4_675 13_666 ?
B2 B1 B1 126.8(3) 4_665 13_566 ?
B2 B1 B1 126.8(3) 4_665 13_676 ?
B2 B1 B1 59.3(11) 16_556 13_666 ?
B2 B1 B1 126.8(3) 4_565 13_676 ?
B2 B1 B1 126.8(3) 4_565 13_666 ?
B2 B1 B2 113.6(9) 16_556 4_565 ?
B2 B1 B2 105.0(10) 4_675 4_565 ?
B2 B1 B2 105.0(10) 4_675 4_665 ?
B2 B1 B2 113.6(9) 16_556 4_665 ?
B2 B1 B2 105.0(10) 4_565 4_665 ?
B2 B1 B2 113.6(9) 16_556 4_675 ?
W1 B2 W1 80.6(7) 1_565 1_455 ?
W1 B2 W1 80.6(7) 1_455 . ?
W1 B2 W1 80.6(7) 1_565 . ?
B1 B2 W1 65.3(6) 4_664 . ?
B1 B2 W1 127.5(5) 4_564 . ?
B1 B2 W1 65.3(6) 4_674 1_565 ?
B1 B2 W1 131.7(5) 16_556 1_455 ?
B1 B2 W1 131.7(5) 16_556 1_565 ?
B1 B2 W1 131.7(5) 16_556 . ?
B1 B2 W1 65.3(6) 4_564 1_455 ?
B1 B2 W1 127.5(5) 4_664 1_455 ?
B1 B2 W1 127.5(5) 4_674 . ?
B1 B2 W1 127.5(5) 4_564 1_565 ?
B1 B2 W1 127.5(5) 4_664 1_565 ?
B1 B2 W1 127.5(5) 4_674 1_455 ?
B1 B2 B1 66.4(9) 16_556 4_664 ?
B1 B2 B1 105.0(10) 4_564 4_664 ?
B1 B2 B1 105.0(10) 4_674 4_664 ?
B1 B2 B1 66.4(9) 16_556 4_564 ?
B1 B2 B1 66.4(9) 16_556 4_674 ?
B1 B2 B1 105.0(10) 4_564 4_674 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.936
_oxdiff_exptl_absorpt_empirical_full_min 0.664
_vrf_PLAT029_WB4_36_5GPa         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.617 Why?  
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT911_WB4_36_5GPa         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         12 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
####################################################################### 
# 
# 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_WB4_31_2GPa
_database_code_depnum_ccdc_archive 'CCDC 2158527'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         31200000
_audit_creation_date             2021-12-07
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.8438(3)
_cell_length_b                   2.8438(3)
_cell_length_c                   10.664(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     74.69(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    184
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      16.3570
_cell_measurement_theta_min      3.3740
_shelx_estimated_absorpt_T_max   0.965
_shelx_estimated_absorpt_T_min   0.965
_exptl_absorpt_coefficient_mu    7.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    10.097
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.596
_diffrn_reflns_Laue_measured_fraction_max 0.597
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            288
_diffrn_reflns_point_group_measured_fraction_full 0.596
_diffrn_reflns_point_group_measured_fraction_max 0.597
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         15.208
_diffrn_reflns_theta_min         3.464
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.596
_diffrn_measured_fraction_theta_max 0.597
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -28.00  28.00   0.50    1.00   0.00   0.00   0.00    --   112
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0456430000
_diffrn_orient_matrix_UB_12      0.0172253000
_diffrn_orient_matrix_UB_13      -0.0250759000
_diffrn_orient_matrix_UB_21      0.1080703000
_diffrn_orient_matrix_UB_22      0.0639098000
_diffrn_orient_matrix_UB_23      0.0103781000
_diffrn_orient_matrix_UB_31      0.0082638000
_diffrn_orient_matrix_UB_32      -0.0971803000
_diffrn_orient_matrix_UB_33      0.0022928000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                66
_reflns_number_total             71
_reflns_odcompleteness_completeness 55.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.91
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.235
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.408
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0233
_refine_ls_restrained_S_all      1.191
_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)+(0.0309P)²+0.1142P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0506
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.6667 0.3333 0.2500 0.0061(3) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.546(2) 0.0054(18) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.113(2) 0.0047(17) Uiso 1 6 d S . P . .


_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 W1 2.8438(3) 3_775 ?
W1 W1 2.8438(4) 1_565 ?
W1 W1 2.8438(4) 1_455 ?
W1 W1 2.8438(3) 3_765 ?
W1 B1 2.17(2) 13_666 ?
W1 B1 2.17(2) 4_664 ?
W1 B2 2.195(15) 16_556 ?
W1 B2 2.195(15) 16_546 ?
W1 B2 2.195(15) . ?
W1 B2 2.195(15) 16_656 ?
W1 B2 2.195(15) 1_545 ?
W1 B2 2.195(15) 1_655 ?
B1 W1 2.17(2) 13_666 ?
B1 B1 1.91(2) 13_566 ?
B1 B1 1.91(2) 13_676 ?
B1 B1 1.91(2) 13_666 ?
B1 B2 1.70(3) 16_556 ?
B1 B2 1.792(13) 4_665 ?
B1 B2 1.792(13) 4_675 ?
B1 B2 1.792(13) 4_565 ?
B2 W1 2.195(15) 1_455 ?
B2 W1 2.195(15) 1_565 ?
B2 B1 1.792(13) 4_674 ?
B2 B1 1.792(13) 4_564 ?
B2 B1 1.70(3) 16_556 ?
B2 B1 1.792(13) 4_664 ?

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
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 60.0 1_565 1_455 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 60.0 3_765 3_775 ?
B1 W1 W1 90.000(1) 4_664 3_775 ?
B1 W1 W1 90.000(1) 13_666 1_565 ?
B1 W1 W1 90.000(1) 13_666 3_775 ?
B1 W1 W1 90.000(1) 4_664 3_765 ?
B1 W1 W1 90.000(1) 13_666 3_765 ?
B1 W1 W1 90.000(1) 4_664 1_455 ?
B1 W1 W1 90.000(1) 13_666 1_455 ?
B1 W1 W1 90.000(1) 4_664 1_565 ?
B1 W1 B1 180.0 4_664 13_666 ?
B1 W1 B2 131.6(4) 13_666 1_545 ?
B1 W1 B2 131.6(5) 4_664 16_656 ?
B1 W1 B2 48.4(4) 4_664 1_655 ?
B1 W1 B2 48.4(4) 13_666 16_556 ?
B1 W1 B2 48.4(4) 4_664 . ?
B1 W1 B2 131.6(4) 4_664 16_546 ?
B1 W1 B2 48.4(4) 4_664 1_545 ?
B1 W1 B2 131.6(4) 4_664 16_556 ?
B1 W1 B2 131.6(4) 13_666 . ?
B1 W1 B2 131.6(5) 13_666 1_655 ?
B1 W1 B2 48.4(4) 13_666 16_656 ?
B1 W1 B2 48.4(4) 13_666 16_546 ?
B2 W1 W1 90.000(1) 1_545 3_765 ?
B2 W1 W1 49.6(3) . 1_565 ?
B2 W1 W1 90.000(1) 1_655 1_565 ?
B2 W1 W1 49.6(3) 16_656 3_765 ?
B2 W1 W1 90.000(1) 16_546 1_455 ?
B2 W1 W1 90.000(1) 16_546 3_765 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 130.4(3) . 3_765 ?
B2 W1 W1 49.6(3) 1_655 3_765 ?
B2 W1 W1 49.6(3) 16_556 1_455 ?
B2 W1 W1 90.000(1) 1_545 1_455 ?
B2 W1 W1 130.4(3) 16_546 1_565 ?
B2 W1 W1 49.6(3) 16_656 3_775 ?
B2 W1 W1 49.6(3) . 1_455 ?
B2 W1 W1 130.4(3) 1_545 3_775 ?
B2 W1 W1 130.4(3) 16_656 1_455 ?
B2 W1 W1 49.6(3) 1_655 3_775 ?
B2 W1 W1 130.4(3) 16_556 3_765 ?
B2 W1 W1 90.000(1) . 3_775 ?
B2 W1 W1 130.4(3) 1_655 1_455 ?
B2 W1 W1 90.000(2) 16_556 3_775 ?
B2 W1 W1 130.4(3) 16_546 3_775 ?
B2 W1 W1 130.4(3) 1_545 1_565 ?
B2 W1 W1 49.6(3) 16_556 1_565 ?
B2 W1 B2 80.7(7) 16_656 16_546 ?
B2 W1 B2 80.7(7) 16_656 16_556 ?
B2 W1 B2 83.2(9) 1_545 16_546 ?
B2 W1 B2 136.1(3) 1_655 16_556 ?
B2 W1 B2 83.2(9) . 16_556 ?
B2 W1 B2 83.2(9) 16_656 1_655 ?
B2 W1 B2 136.1(3) 16_546 1_655 ?
B2 W1 B2 136.1(3) 16_656 . ?
B2 W1 B2 80.7(7) 1_545 1_655 ?
B2 W1 B2 136.1(3) 16_546 . ?
B2 W1 B2 136.1(3) 16_656 1_545 ?
B2 W1 B2 136.1(3) 1_545 16_556 ?
B2 W1 B2 80.7(7) 1_545 . ?
B2 W1 B2 80.7(7) 16_546 16_556 ?
B2 W1 B2 80.7(7) 1_655 . ?
B1 B1 W1 120.9(12) 13_566 13_666 ?
B1 B1 W1 120.9(12) 13_676 13_666 ?
B1 B1 W1 120.9(12) 13_666 13_666 ?
B1 B1 B1 96.0(15) 13_566 13_676 ?
B1 B1 B1 96.0(15) 13_566 13_666 ?
B1 B1 B1 96.0(15) 13_676 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 66.4(9) 4_665 13_666 ?
B2 B1 W1 66.4(9) 4_675 13_666 ?
B2 B1 W1 66.4(9) 4_565 13_666 ?
B2 B1 B1 54.5(9) 4_665 13_666 ?
B2 B1 B1 59.1(12) 16_556 13_566 ?
B2 B1 B1 54.5(9) 4_675 13_676 ?
B2 B1 B1 54.5(9) 4_565 13_566 ?
B2 B1 B1 59.1(12) 16_556 13_676 ?
B2 B1 B1 126.8(3) 4_675 13_566 ?
B2 B1 B1 126.8(3) 4_675 13_666 ?
B2 B1 B1 126.8(3) 4_665 13_566 ?
B2 B1 B1 126.8(3) 4_665 13_676 ?
B2 B1 B1 59.1(12) 16_556 13_666 ?
B2 B1 B1 126.8(3) 4_565 13_676 ?
B2 B1 B1 126.8(3) 4_565 13_666 ?
B2 B1 B2 113.6(9) 16_556 4_565 ?
B2 B1 B2 105.1(11) 4_675 4_565 ?
B2 B1 B2 105.1(11) 4_675 4_665 ?
B2 B1 B2 113.6(9) 16_556 4_665 ?
B2 B1 B2 105.1(11) 4_565 4_665 ?
B2 B1 B2 113.6(9) 16_556 4_675 ?
W1 B2 W1 80.7(7) 1_565 1_455 ?
W1 B2 W1 80.7(7) 1_455 . ?
W1 B2 W1 80.7(7) 1_565 . ?
B1 B2 W1 65.2(7) 4_664 . ?
B1 B2 W1 127.5(5) 4_564 . ?
B1 B2 W1 65.2(7) 4_674 1_565 ?
B1 B2 W1 131.6(4) 16_556 1_455 ?
B1 B2 W1 131.6(4) 16_556 1_565 ?
B1 B2 W1 131.6(4) 16_556 . ?
B1 B2 W1 65.2(7) 4_564 1_455 ?
B1 B2 W1 127.5(5) 4_664 1_455 ?
B1 B2 W1 127.5(5) 4_674 . ?
B1 B2 W1 127.5(5) 4_564 1_565 ?
B1 B2 W1 127.5(5) 4_664 1_565 ?
B1 B2 W1 127.5(5) 4_674 1_455 ?
B1 B2 B1 66.4(9) 16_556 4_664 ?
B1 B2 B1 105.1(10) 4_564 4_664 ?
B1 B2 B1 105.1(10) 4_674 4_664 ?
B1 B2 B1 66.4(9) 16_556 4_564 ?
B1 B2 B1 66.4(9) 16_556 4_674 ?
B1 B2 B1 105.1(10) 4_564 4_674 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.872
_oxdiff_exptl_absorpt_empirical_full_min 0.697
_vrf_PLAT911_WB4_31_2GPa         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         13 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
####################################################################### 
# 
# 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_WB4_42_2GPa
_database_code_depnum_ccdc_archive 'CCDC 2158529'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         42200000
_audit_creation_date             2021-12-09
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.8240(4)
_cell_length_b                   2.8240(4)
_cell_length_c                   10.589(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     73.13(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    146
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      16.1230
_cell_measurement_theta_min      3.3920
_shelx_estimated_absorpt_T_max   0.964
_shelx_estimated_absorpt_T_min   0.964
_exptl_absorpt_coefficient_mu    7.436
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    10.313
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.565
_diffrn_reflns_Laue_measured_fraction_max 0.598
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            253
_diffrn_reflns_point_group_measured_fraction_full 0.565
_diffrn_reflns_point_group_measured_fraction_max 0.598
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         15.170
_diffrn_reflns_theta_min         3.489
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.565
_diffrn_measured_fraction_theta_max 0.598
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -28.00  18.50   0.50    1.00   0.00   0.00   0.00    --    93
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0171934000
_diffrn_orient_matrix_UB_12      -0.0462589000
_diffrn_orient_matrix_UB_13      0.0250321000
_diffrn_orient_matrix_UB_21      -0.0646582000
_diffrn_orient_matrix_UB_22      -0.1090606000
_diffrn_orient_matrix_UB_23      -0.0105418000
_diffrn_orient_matrix_UB_31      0.0981374000
_diffrn_orient_matrix_UB_32      -0.0083299000
_diffrn_orient_matrix_UB_33      -0.0024496000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                64
_reflns_number_total             70
_reflns_odcompleteness_completeness 55.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.74
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.087
_refine_diff_density_min         -1.687
_refine_diff_density_rms         0.409
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         70
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0216
_refine_ls_restrained_S_all      1.139
_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)+(0.0172P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0522
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.6667 0.3333 0.2500 0.0070(3) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.550(3) 0.004(2) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.112(3) 0.006(2) Uiso 1 6 d S . P . .


_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 W1 2.8240(4) 3_775 ?
W1 W1 2.8240(4) 3_765 ?
W1 W1 2.8240(4) 1_455 ?
W1 W1 2.8240(4) 1_565 ?
W1 B1 2.11(3) 13_666 ?
W1 B1 2.11(3) 4_664 ?
W1 B2 2.19(2) . ?
W1 B2 2.19(2) 16_556 ?
W1 B2 2.19(2) 1_545 ?
W1 B2 2.19(2) 1_655 ?
W1 B2 2.19(2) 16_656 ?
W1 B2 2.19(2) 16_546 ?
B1 W1 2.11(3) 13_666 ?
B1 B1 1.95(3) 13_566 ?
B1 B1 1.95(3) 13_676 ?
B1 B1 1.95(3) 13_666 ?
B1 B2 1.72(4) 16_556 ?
B1 B2 1.758(15) 4_665 ?
B1 B2 1.758(15) 4_675 ?
B1 B2 1.758(15) 4_565 ?
B2 W1 2.19(2) 1_455 ?
B2 W1 2.19(2) 1_565 ?
B2 B1 1.72(4) 16_556 ?
B2 B1 1.758(15) 4_564 ?
B2 B1 1.758(15) 4_664 ?
B2 B1 1.758(15) 4_674 ?

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
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 60.0 1_455 1_565 ?
W1 W1 W1 60.0 3_765 3_775 ?
B1 W1 W1 90.000(1) 4_664 1_455 ?
B1 W1 W1 90.000(2) 13_666 3_775 ?
B1 W1 W1 90.000(1) 13_666 3_765 ?
B1 W1 W1 90.000(1) 4_664 1_565 ?
B1 W1 W1 90.000(1) 4_664 3_765 ?
B1 W1 W1 90.000(1) 13_666 1_455 ?
B1 W1 W1 90.000(1) 4_664 3_775 ?
B1 W1 W1 90.000(1) 13_666 1_565 ?
B1 W1 B1 180.0 4_664 13_666 ?
B1 W1 B2 48.2(6) 4_664 1_545 ?
B1 W1 B2 48.2(6) 13_666 16_656 ?
B1 W1 B2 131.8(6) 4_664 16_546 ?
B1 W1 B2 48.2(6) 4_664 . ?
B1 W1 B2 131.8(6) 13_666 . ?
B1 W1 B2 131.8(6) 4_664 16_556 ?
B1 W1 B2 131.8(6) 4_664 16_656 ?
B1 W1 B2 48.2(6) 4_664 1_655 ?
B1 W1 B2 131.8(6) 13_666 1_545 ?
B1 W1 B2 131.8(6) 13_666 1_655 ?
B1 W1 B2 48.2(6) 13_666 16_556 ?
B1 W1 B2 48.2(6) 13_666 16_546 ?
B2 W1 W1 90.000(2) 1_545 3_765 ?
B2 W1 W1 130.2(4) 16_556 3_765 ?
B2 W1 W1 49.8(4) . 1_455 ?
B2 W1 W1 49.8(4) 16_556 1_565 ?
B2 W1 W1 130.2(4) . 3_765 ?
B2 W1 W1 130.2(4) 1_545 1_565 ?
B2 W1 W1 130.2(4) 16_546 3_775 ?
B2 W1 W1 130.2(4) 1_655 1_455 ?
B2 W1 W1 130.2(4) 16_656 1_455 ?
B2 W1 W1 49.8(4) 16_556 1_455 ?
B2 W1 W1 49.8(4) 1_655 3_765 ?
B2 W1 W1 130.2(4) 16_546 1_565 ?
B2 W1 W1 90.000(2) . 3_775 ?
B2 W1 W1 90.000(1) 16_546 3_765 ?
B2 W1 W1 90.000(1) 1_545 1_455 ?
B2 W1 W1 90.000(1) 16_546 1_455 ?
B2 W1 W1 49.8(4) 16_656 3_775 ?
B2 W1 W1 49.8(4) 16_656 3_765 ?
B2 W1 W1 130.2(4) 1_545 3_775 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 49.8(4) 1_655 3_775 ?
B2 W1 W1 49.8(4) . 1_565 ?
B2 W1 W1 90.000(2) 16_556 3_775 ?
B2 W1 W1 90.000(1) 1_655 1_565 ?
B2 W1 B2 80.4(9) 16_656 16_546 ?
B2 W1 B2 80.4(9) 16_656 16_556 ?
B2 W1 B2 80.4(9) 1_545 . ?
B2 W1 B2 136.2(4) 16_546 . ?
B2 W1 B2 136.2(4) 16_656 . ?
B2 W1 B2 83.6(11) 16_556 . ?
B2 W1 B2 136.2(4) 1_545 16_556 ?
B2 W1 B2 83.6(11) 1_545 16_546 ?
B2 W1 B2 136.2(4) 1_655 16_556 ?
B2 W1 B2 80.4(9) 1_655 . ?
B2 W1 B2 136.2(4) 16_546 1_655 ?
B2 W1 B2 80.4(9) 16_546 16_556 ?
B2 W1 B2 80.4(9) 1_545 1_655 ?
B2 W1 B2 83.6(11) 16_656 1_655 ?
B2 W1 B2 136.2(4) 16_656 1_545 ?
B1 B1 W1 123.1(13) 13_566 13_666 ?
B1 B1 W1 123.1(13) 13_676 13_666 ?
B1 B1 W1 123.1(13) 13_666 13_666 ?
B1 B1 B1 93.0(18) 13_566 13_676 ?
B1 B1 B1 93.0(18) 13_566 13_666 ?
B1 B1 B1 93.0(18) 13_676 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 68.1(12) 4_665 13_666 ?
B2 B1 W1 68.1(12) 4_675 13_666 ?
B2 B1 W1 68.1(12) 4_565 13_666 ?
B2 B1 B1 126.3(5) 4_665 13_676 ?
B2 B1 B1 126.3(5) 4_565 13_666 ?
B2 B1 B1 56.9(13) 16_556 13_666 ?
B2 B1 B1 55.1(10) 4_665 13_666 ?
B2 B1 B1 55.1(10) 4_675 13_676 ?
B2 B1 B1 56.9(13) 16_556 13_566 ?
B2 B1 B1 126.3(5) 4_665 13_566 ?
B2 B1 B1 126.3(5) 4_675 13_566 ?
B2 B1 B1 56.9(13) 16_556 13_676 ?
B2 B1 B1 55.1(10) 4_565 13_566 ?
B2 B1 B1 126.3(5) 4_675 13_666 ?
B2 B1 B1 126.3(5) 4_565 13_676 ?
B2 B1 B2 111.9(12) 16_556 4_565 ?
B2 B1 B2 106.9(13) 4_565 4_665 ?
B2 B1 B2 106.9(13) 4_675 4_565 ?
B2 B1 B2 106.9(13) 4_675 4_665 ?
B2 B1 B2 111.9(12) 16_556 4_675 ?
B2 B1 B2 111.9(12) 16_556 4_665 ?
W1 B2 W1 80.4(9) 1_565 1_455 ?
W1 B2 W1 80.4(9) 1_455 . ?
W1 B2 W1 80.4(9) 1_565 . ?
B1 B2 W1 131.8(6) 16_556 1_455 ?
B1 B2 W1 131.8(6) 16_556 . ?
B1 B2 W1 126.5(7) 4_564 . ?
B1 B2 W1 63.7(9) 4_664 . ?
B1 B2 W1 126.5(7) 4_664 1_565 ?
B1 B2 W1 126.5(7) 4_674 . ?
B1 B2 W1 63.7(9) 4_674 1_565 ?
B1 B2 W1 126.5(7) 4_564 1_565 ?
B1 B2 W1 63.7(9) 4_564 1_455 ?
B1 B2 W1 126.5(7) 4_674 1_455 ?
B1 B2 W1 131.8(6) 16_556 1_565 ?
B1 B2 W1 126.5(7) 4_664 1_455 ?
B1 B2 B1 68.1(12) 16_556 4_664 ?
B1 B2 B1 106.9(13) 4_674 4_664 ?
B1 B2 B1 68.1(12) 16_556 4_674 ?
B1 B2 B1 106.9(13) 4_564 4_674 ?
B1 B2 B1 68.1(12) 16_556 4_564 ?
B1 B2 B1 106.9(13) 4_564 4_664 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.314
_oxdiff_exptl_absorpt_empirical_full_min 0.676
_vrf_PLAT911_WB4_42_2GPa         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         14 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT971_WB4_42_2GPa         
;
PROBLEM: Check Calcd Resid. Dens.  0.83A   From B1              2.99 eA-3  
RESPONSE: Due to incompleteness of the dataset.
;
####################################################################### 
# 
# 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_WB4_P_amb
_database_code_depnum_ccdc_archive 'CCDC 2158536'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_audit_creation_date             2022-03-14
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0007 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.4201 4.6430 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.9578(6)
_cell_length_b                   2.9578(6)
_cell_length_c                   10.996(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     83.31(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    365
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6320
_cell_measurement_theta_min      5.8550
_shelx_estimated_absorpt_T_max   0.709
_shelx_estimated_absorpt_T_min   0.709
_exptl_absorpt_coefficient_mu    36.860
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    9.053
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            331
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        20.500
_diffrn_reflns_theta_max         23.454
_diffrn_reflns_theta_min         5.855
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'SMART APEX CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     91.82 158.05   0.30   19.99    --   28.00  73.85 -25.78  221
  2  ω      2.22 132.58   0.30   19.99    --   28.00  73.85  64.22  435
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1307378000
_diffrn_orient_matrix_UB_12      -0.1666610000
_diffrn_orient_matrix_UB_13      0.0302616000
_diffrn_orient_matrix_UB_21      -0.0959206000
_diffrn_orient_matrix_UB_22      0.1111843000
_diffrn_orient_matrix_UB_23      0.0161052000
_diffrn_orient_matrix_UB_31      -0.1462083000
_diffrn_orient_matrix_UB_32      -0.0863428000
_diffrn_orient_matrix_UB_33      -0.0376245000
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56087
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                66
_reflns_number_total             69
_reflns_odcompleteness_completeness 96.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     20.46
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.088
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.467
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         69
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0212
_refine_ls_restrained_S_all      1.244
_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)+(0.0306P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0459
_refine_special_details          ?
_olex2_refinement_description    
;
;
_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 0.6667 0.3333 0.2500 0.0030(3) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.5466(13) 0.002(2) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.1106(13) 0.003(3) Uiso 1 6 d S . P . .


_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 W1 2.9578(6) 3_775 ?
W1 W1 2.9578(6) 1_565 ?
W1 W1 2.9578(6) 3_765 ?
W1 W1 2.9578(6) 1_455 ?
W1 B1 2.237(15) 13_666 ?
W1 B1 2.237(15) 4_664 ?
W1 B2 2.295(10) 16_556 ?
W1 B2 2.295(10) 16_656 ?
W1 B2 2.295(10) 1_545 ?
W1 B2 2.295(10) 16_546 ?
W1 B2 2.295(10) 1_655 ?
W1 B2 2.295(10) . ?
B1 W1 2.237(15) 13_666 ?
B1 B1 1.991(15) 13_566 ?
B1 B1 1.991(15) 13_676 ?
B1 B1 1.991(15) 13_666 ?
B1 B2 1.73(2) 16_556 ?
B1 B2 1.847(7) 4_665 ?
B1 B2 1.847(7) 4_675 ?
B1 B2 1.847(7) 4_565 ?
B2 W1 2.295(10) 1_455 ?
B2 W1 2.295(10) 1_565 ?
B2 B1 1.847(7) 4_664 ?
B2 B1 1.847(7) 4_564 ?
B2 B1 1.847(7) 4_674 ?
B2 B1 1.73(2) 16_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 60.0 1_455 1_565 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 60.0 3_765 3_775 ?
B1 W1 W1 90.0 13_666 1_565 ?
B1 W1 W1 90.0 13_666 3_765 ?
B1 W1 W1 90.000(1) 4_664 3_765 ?
B1 W1 W1 90.0 13_666 1_455 ?
B1 W1 W1 90.0 4_664 1_565 ?
B1 W1 W1 90.000(1) 13_666 3_775 ?
B1 W1 W1 90.000(1) 4_664 1_455 ?
B1 W1 W1 90.000(1) 4_664 3_775 ?
B1 W1 B1 180.0 4_664 13_666 ?
B1 W1 B2 48.1(3) 4_664 1_545 ?
B1 W1 B2 131.9(3) 13_666 . ?
B1 W1 B2 48.1(3) 4_664 . ?
B1 W1 B2 48.1(3) 4_664 1_655 ?
B1 W1 B2 131.9(3) 4_664 16_556 ?
B1 W1 B2 48.1(3) 13_666 16_556 ?
B1 W1 B2 131.9(3) 13_666 1_545 ?
B1 W1 B2 131.9(3) 4_664 16_546 ?
B1 W1 B2 131.9(3) 4_664 16_656 ?
B1 W1 B2 131.9(3) 13_666 1_655 ?
B1 W1 B2 48.1(3) 13_666 16_656 ?
B1 W1 B2 48.1(3) 13_666 16_546 ?
B2 W1 W1 49.9(2) 16_656 3_765 ?
B2 W1 W1 130.1(2) 1_655 1_455 ?
B2 W1 W1 90.000(1) 1_655 1_565 ?
B2 W1 W1 90.0 16_546 3_765 ?
B2 W1 W1 90.000(1) 1_545 3_765 ?
B2 W1 W1 49.9(2) 1_655 3_765 ?
B2 W1 W1 49.9(2) 16_556 1_565 ?
B2 W1 W1 49.9(2) 16_556 1_455 ?
B2 W1 W1 130.1(2) 16_546 3_775 ?
B2 W1 W1 130.1(2) . 3_765 ?
B2 W1 W1 90.0 1_545 1_455 ?
B2 W1 W1 130.1(2) 16_556 3_765 ?
B2 W1 W1 49.9(2) 1_655 3_775 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 90.000(1) . 3_775 ?
B2 W1 W1 130.1(2) 16_546 1_565 ?
B2 W1 W1 90.000(1) 16_556 3_775 ?
B2 W1 W1 49.9(2) . 1_565 ?
B2 W1 W1 130.1(2) 16_656 1_455 ?
B2 W1 W1 90.000(1) 16_546 1_455 ?
B2 W1 W1 130.1(2) 1_545 3_775 ?
B2 W1 W1 49.9(2) . 1_455 ?
B2 W1 W1 49.9(2) 16_656 3_775 ?
B2 W1 W1 130.1(2) 1_545 1_565 ?
B2 W1 B2 83.8(5) 1_545 16_546 ?
B2 W1 B2 80.2(4) 16_656 16_546 ?
B2 W1 B2 136.31(19) 16_546 . ?
B2 W1 B2 80.2(4) 1_545 1_655 ?
B2 W1 B2 80.2(4) 1_545 . ?
B2 W1 B2 136.31(19) 1_545 16_556 ?
B2 W1 B2 83.8(5) 16_656 1_655 ?
B2 W1 B2 80.2(4) 16_656 16_556 ?
B2 W1 B2 136.31(19) 1_545 16_656 ?
B2 W1 B2 80.2(4) 16_546 16_556 ?
B2 W1 B2 136.31(19) 16_656 . ?
B2 W1 B2 136.31(19) 1_655 16_556 ?
B2 W1 B2 80.2(4) 1_655 . ?
B2 W1 B2 83.8(5) . 16_556 ?
B2 W1 B2 136.31(19) 16_546 1_655 ?
B1 B1 W1 121.0(7) 13_566 13_666 ?
B1 B1 W1 121.0(7) 13_676 13_666 ?
B1 B1 W1 121.0(7) 13_666 13_666 ?
B1 B1 B1 95.9(10) 13_566 13_676 ?
B1 B1 B1 95.9(10) 13_566 13_666 ?
B1 B1 B1 95.9(10) 13_676 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 67.6(5) 4_665 13_666 ?
B2 B1 W1 67.6(5) 4_675 13_666 ?
B2 B1 W1 67.6(5) 4_565 13_666 ?
B2 B1 B1 59.0(7) 16_556 13_676 ?
B2 B1 B1 126.33(16) 4_565 13_676 ?
B2 B1 B1 53.4(6) 4_565 13_566 ?
B2 B1 B1 126.33(16) 4_665 13_676 ?
B2 B1 B1 59.0(7) 16_556 13_666 ?
B2 B1 B1 126.33(16) 4_565 13_666 ?
B2 B1 B1 126.33(16) 4_675 13_566 ?
B2 B1 B1 59.0(7) 16_556 13_566 ?
B2 B1 B1 53.4(6) 4_675 13_676 ?
B2 B1 B1 53.4(6) 4_665 13_666 ?
B2 B1 B1 126.33(16) 4_665 13_566 ?
B2 B1 B1 126.33(16) 4_675 13_666 ?
B2 B1 B2 112.4(5) 16_556 4_565 ?
B2 B1 B2 112.4(5) 16_556 4_675 ?
B2 B1 B2 106.4(6) 4_565 4_665 ?
B2 B1 B2 106.4(6) 4_675 4_565 ?
B2 B1 B2 112.4(5) 16_556 4_665 ?
B2 B1 B2 106.4(6) 4_675 4_665 ?
W1 B2 W1 80.2(4) 1_565 1_455 ?
W1 B2 W1 80.2(4) 1_455 . ?
W1 B2 W1 80.2(4) 1_565 . ?
B1 B2 W1 64.3(4) 4_664 . ?
B1 B2 W1 126.8(3) 4_674 . ?
B1 B2 W1 131.9(3) 16_556 . ?
B1 B2 W1 131.9(3) 16_556 1_455 ?
B1 B2 W1 131.9(3) 16_556 1_565 ?
B1 B2 W1 64.3(4) 4_564 1_455 ?
B1 B2 W1 126.8(3) 4_564 . ?
B1 B2 W1 126.8(3) 4_674 1_455 ?
B1 B2 W1 64.3(4) 4_674 1_565 ?
B1 B2 W1 126.8(3) 4_664 1_455 ?
B1 B2 W1 126.8(3) 4_664 1_565 ?
B1 B2 W1 126.8(3) 4_564 1_565 ?
B1 B2 B1 67.6(5) 16_556 4_664 ?
B1 B2 B1 67.6(5) 16_556 4_674 ?
B1 B2 B1 67.6(5) 16_556 4_564 ?
B1 B2 B1 106.4(6) 4_564 4_664 ?
B1 B2 B1 106.4(6) 4_564 4_674 ?
B1 B2 B1 106.4(6) 4_674 4_664 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.712
_oxdiff_exptl_absorpt_empirical_full_min 0.603
####################################################################### 
# 
# 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_WB4_53_2GPa
_database_code_depnum_ccdc_archive 'CCDC 2158531'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         53200000
_audit_creation_date             2021-12-08
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.7932(5)
_cell_length_b                   2.7932(5)
_cell_length_c                   10.528(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     71.14(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    161
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      16.2860
_cell_measurement_theta_min      3.4140
_shelx_estimated_absorpt_T_max   0.963
_shelx_estimated_absorpt_T_min   0.963
_exptl_absorpt_coefficient_mu    7.644
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    10.602
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.600
_diffrn_reflns_Laue_measured_fraction_max 0.598
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            214
_diffrn_reflns_point_group_measured_fraction_full 0.600
_diffrn_reflns_point_group_measured_fraction_max 0.598
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         15.232
_diffrn_reflns_theta_min         3.436
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.600
_diffrn_measured_fraction_theta_max 0.598
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -28.00  28.00   0.50    1.00   0.00   0.00   0.00    --   112
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0473150000
_diffrn_orient_matrix_UB_12      0.0169156000
_diffrn_orient_matrix_UB_13      -0.0252125000
_diffrn_orient_matrix_UB_21      0.1099183000
_diffrn_orient_matrix_UB_22      0.0653139000
_diffrn_orient_matrix_UB_23      0.0106728000
_diffrn_orient_matrix_UB_31      0.0082930000
_diffrn_orient_matrix_UB_32      -0.0990390000
_diffrn_orient_matrix_UB_33      0.0026039000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                62
_reflns_number_total             67
_reflns_odcompleteness_completeness 55.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     10.44
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.271
_refine_diff_density_min         -2.116
_refine_diff_density_rms         0.555
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         67
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0217
_refine_ls_restrained_S_all      1.281
_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)+(0.0380P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0545
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.6667 0.3333 0.2500 0.0064(3) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.546(2) 0.0052(18) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.113(2) 0.0060(19) Uiso 1 6 d S . P . .


_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 W1 2.7932(5) 3_775 ?
W1 W1 2.7932(5) 1_565 ?
W1 W1 2.7932(5) 1_455 ?
W1 W1 2.7932(5) 3_765 ?
W1 B1 2.15(2) 13_666 ?
W1 B1 2.15(2) 4_664 ?
W1 B2 2.163(16) 16_556 ?
W1 B2 2.163(16) 16_546 ?
W1 B2 2.163(16) . ?
W1 B2 2.163(16) 16_656 ?
W1 B2 2.163(16) 1_545 ?
W1 B2 2.163(16) 1_655 ?
B1 W1 2.15(2) 13_666 ?
B1 B1 1.88(2) 13_566 ?
B1 B1 1.88(2) 13_676 ?
B1 B1 1.88(2) 13_666 ?
B1 B2 1.67(3) 16_556 ?
B1 B2 1.762(13) 4_665 ?
B1 B2 1.762(13) 4_675 ?
B1 B2 1.762(13) 4_565 ?
B2 W1 2.163(16) 1_455 ?
B2 W1 2.163(16) 1_565 ?
B2 B1 1.762(13) 4_674 ?
B2 B1 1.762(13) 4_564 ?
B2 B1 1.67(3) 16_556 ?
B2 B1 1.762(13) 4_664 ?

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
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 60.0 1_565 1_455 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 60.0 3_765 3_775 ?
B1 W1 W1 90.000(1) 4_664 3_775 ?
B1 W1 W1 90.000(1) 13_666 1_565 ?
B1 W1 W1 90.000(1) 13_666 3_775 ?
B1 W1 W1 90.000(1) 4_664 3_765 ?
B1 W1 W1 90.000(1) 13_666 3_765 ?
B1 W1 W1 90.000(1) 4_664 1_455 ?
B1 W1 W1 90.000(1) 13_666 1_455 ?
B1 W1 W1 90.000(1) 4_664 1_565 ?
B1 W1 B1 180.0 4_664 13_666 ?
B1 W1 B2 131.8(5) 13_666 1_545 ?
B1 W1 B2 131.8(5) 4_664 16_656 ?
B1 W1 B2 48.2(5) 4_664 1_655 ?
B1 W1 B2 48.2(5) 13_666 16_556 ?
B1 W1 B2 48.2(5) 4_664 . ?
B1 W1 B2 131.8(5) 4_664 16_546 ?
B1 W1 B2 48.2(5) 4_664 1_545 ?
B1 W1 B2 131.8(5) 4_664 16_556 ?
B1 W1 B2 131.8(5) 13_666 . ?
B1 W1 B2 131.8(5) 13_666 1_655 ?
B1 W1 B2 48.2(5) 13_666 16_656 ?
B1 W1 B2 48.2(5) 13_666 16_546 ?
B2 W1 W1 90.000(1) 1_545 3_765 ?
B2 W1 W1 49.8(4) . 1_565 ?
B2 W1 W1 90.0 1_655 1_565 ?
B2 W1 W1 49.8(4) 16_656 3_765 ?
B2 W1 W1 90.000(1) 16_546 1_455 ?
B2 W1 W1 90.000(1) 16_546 3_765 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 130.2(4) . 3_765 ?
B2 W1 W1 49.8(4) 1_655 3_765 ?
B2 W1 W1 49.8(4) 16_556 1_455 ?
B2 W1 W1 90.000(1) 1_545 1_455 ?
B2 W1 W1 130.2(4) 16_546 1_565 ?
B2 W1 W1 49.8(4) 16_656 3_775 ?
B2 W1 W1 49.8(4) . 1_455 ?
B2 W1 W1 130.2(4) 1_545 3_775 ?
B2 W1 W1 130.2(4) 16_656 1_455 ?
B2 W1 W1 49.8(4) 1_655 3_775 ?
B2 W1 W1 130.2(4) 16_556 3_765 ?
B2 W1 W1 90.000(1) . 3_775 ?
B2 W1 W1 130.2(4) 1_655 1_455 ?
B2 W1 W1 90.000(2) 16_556 3_775 ?
B2 W1 W1 130.2(4) 16_546 3_775 ?
B2 W1 W1 130.2(4) 1_545 1_565 ?
B2 W1 W1 49.8(4) 16_556 1_565 ?
B2 W1 B2 80.4(7) 16_656 16_546 ?
B2 W1 B2 80.4(7) 16_656 16_556 ?
B2 W1 B2 83.6(9) 1_545 16_546 ?
B2 W1 B2 136.2(3) 1_655 16_556 ?
B2 W1 B2 83.6(9) . 16_556 ?
B2 W1 B2 83.6(9) 16_656 1_655 ?
B2 W1 B2 136.2(3) 16_546 1_655 ?
B2 W1 B2 136.2(3) 16_656 . ?
B2 W1 B2 80.4(7) 1_545 1_655 ?
B2 W1 B2 136.2(3) 16_546 . ?
B2 W1 B2 136.2(3) 16_656 1_545 ?
B2 W1 B2 136.2(3) 1_545 16_556 ?
B2 W1 B2 80.4(7) 1_545 . ?
B2 W1 B2 80.4(7) 16_546 16_556 ?
B2 W1 B2 80.4(7) 1_655 . ?
B1 B1 W1 120.7(12) 13_566 13_666 ?
B1 B1 W1 120.7(12) 13_676 13_666 ?
B1 B1 W1 120.7(12) 13_666 13_666 ?
B1 B1 B1 96.2(16) 13_566 13_676 ?
B1 B1 B1 96.2(16) 13_566 13_666 ?
B1 B1 B1 96.2(16) 13_676 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 66.2(10) 4_665 13_666 ?
B2 B1 W1 66.2(10) 4_675 13_666 ?
B2 B1 W1 66.2(10) 4_565 13_666 ?
B2 B1 B1 54.5(9) 4_665 13_666 ?
B2 B1 B1 59.3(12) 16_556 13_566 ?
B2 B1 B1 54.5(9) 4_675 13_676 ?
B2 B1 B1 54.5(9) 4_565 13_566 ?
B2 B1 B1 59.3(12) 16_556 13_676 ?
B2 B1 B1 126.8(3) 4_675 13_566 ?
B2 B1 B1 126.8(3) 4_675 13_666 ?
B2 B1 B1 126.8(3) 4_665 13_566 ?
B2 B1 B1 126.8(3) 4_665 13_676 ?
B2 B1 B1 59.3(12) 16_556 13_666 ?
B2 B1 B1 126.8(3) 4_565 13_676 ?
B2 B1 B1 126.8(3) 4_565 13_666 ?
B2 B1 B2 113.8(10) 16_556 4_565 ?
B2 B1 B2 104.8(11) 4_675 4_565 ?
B2 B1 B2 104.8(11) 4_675 4_665 ?
B2 B1 B2 113.8(10) 16_556 4_665 ?
B2 B1 B2 104.8(11) 4_565 4_665 ?
B2 B1 B2 113.8(10) 16_556 4_675 ?
W1 B2 W1 80.4(7) 1_565 1_455 ?
W1 B2 W1 80.4(7) 1_455 . ?
W1 B2 W1 80.4(7) 1_565 . ?
B1 B2 W1 65.6(7) 4_664 . ?
B1 B2 W1 127.6(6) 4_564 . ?
B1 B2 W1 65.6(7) 4_674 1_565 ?
B1 B2 W1 131.8(5) 16_556 1_455 ?
B1 B2 W1 131.8(5) 16_556 1_565 ?
B1 B2 W1 131.8(5) 16_556 . ?
B1 B2 W1 65.6(7) 4_564 1_455 ?
B1 B2 W1 127.6(6) 4_664 1_455 ?
B1 B2 W1 127.6(6) 4_674 . ?
B1 B2 W1 127.6(6) 4_564 1_565 ?
B1 B2 W1 127.6(6) 4_664 1_565 ?
B1 B2 W1 127.6(6) 4_674 1_455 ?
B1 B2 B1 66.2(10) 16_556 4_664 ?
B1 B2 B1 104.8(11) 4_564 4_664 ?
B1 B2 B1 104.8(11) 4_674 4_664 ?
B1 B2 B1 66.2(10) 16_556 4_564 ?
B1 B2 B1 66.2(10) 16_556 4_674 ?
B1 B2 B1 104.8(11) 4_564 4_674 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.080
_oxdiff_exptl_absorpt_empirical_full_min 0.607
_vrf_PLAT029_WB4_53_2GPa         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.600 Why?  
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT911_WB4_53_2GPa         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         13 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT971_WB4_53_2GPa         
;
PROBLEM: Check Calcd Resid. Dens.  0.86A   From B1              2.52 eA-3  
RESPONSE: Due to incompleteness of the dataset.
;
####################################################################### 
# 
# 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_WB4_47_9GPa
_database_code_depnum_ccdc_archive 'CCDC 2158530'
loop_
_audit_author_name
_audit_author_address
'Elena Bykova'
;Earth and Planets Laboratory, Carnegie Institution for Science
United States of America
;
_audit_update_record             
;
2022-03-14 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_diffrn_ambient_pressure         47900000
_audit_creation_date             2021-12-08
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'tungsten tetraboride'
_chemical_formula_moiety         'B4 W1'
_chemical_formula_sum            'B4 W'
_chemical_formula_weight         227.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W B4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B -0.0005 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.9882 1.5037 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   2.8068(4)
_cell_length_b                   2.8068(4)
_cell_length_c                   10.567(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     72.09(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    167
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      16.5920
_cell_measurement_theta_min      3.4010
_shelx_estimated_absorpt_T_max   0.963
_shelx_estimated_absorpt_T_min   0.963
_exptl_absorpt_coefficient_mu    7.543
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    10.461
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             188
_exptl_crystal_preparation       'high-pressure high-temperature synthesis'
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.587
_diffrn_reflns_Laue_measured_fraction_max 0.584
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            245
_diffrn_reflns_point_group_measured_fraction_full 0.587
_diffrn_reflns_point_group_measured_fraction_max 0.584
_diffrn_reflns_theta_full        10.500
_diffrn_reflns_theta_max         16.843
_diffrn_reflns_theta_min         3.420
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'Flat panel'
_diffrn_detector_area_resol_mean 5.0
_diffrn_detector_type            'Perkin Elmer XRD1621'
_diffrn_measured_fraction_theta_full 0.587
_diffrn_measured_fraction_theta_max 0.584
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -28.00  28.00   0.50    1.00   0.00   0.00   0.00    --   112
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'customized ω-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0468160000
_diffrn_orient_matrix_UB_12      0.0170904000
_diffrn_orient_matrix_UB_13      -0.0251480000
_diffrn_orient_matrix_UB_21      0.1094817000
_diffrn_orient_matrix_UB_22      0.0650125000
_diffrn_orient_matrix_UB_23      0.0106085000
_diffrn_orient_matrix_UB_31      0.0083440000
_diffrn_orient_matrix_UB_32      -0.0985689000
_diffrn_orient_matrix_UB_33      0.0025070000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.290
_diffrn_source                   synchrotron
_diffrn_source_type              'PETRAIII, Beamline P02.2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                79
_reflns_number_total             87
_reflns_odcompleteness_completeness 55.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.84
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.192
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.509
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         87
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0223
_refine_ls_restrained_S_all      1.242
_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)+(0.0344P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0518
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.6667 0.3333 0.2500 0.0055(2) Uani 1 12 d S T P . .
B1 B 0.3333 0.6667 0.5469(16) 0.0038(13) Uiso 1 6 d S . P . .
B2 B 0.3333 0.6667 0.1114(18) 0.0056(14) Uiso 1 6 d S . P . .


_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 W1 2.8068(4) 3_775 ?
W1 W1 2.8068(3) 1_455 ?
W1 W1 2.8068(4) 1_565 ?
W1 W1 2.8068(4) 3_765 ?
W1 B1 2.146(17) 13_666 ?
W1 B1 2.146(17) 4_664 ?
W1 B2 2.184(13) . ?
W1 B2 2.184(13) 16_546 ?
W1 B2 2.184(13) 16_556 ?
W1 B2 2.184(13) 1_545 ?
W1 B2 2.184(13) 16_656 ?
W1 B2 2.184(13) 1_655 ?
B1 W1 2.146(17) 13_666 ?
B1 B1 1.900(18) 13_566 ?
B1 B1 1.900(18) 13_676 ?
B1 B1 1.900(18) 13_666 ?
B1 B2 1.67(3) 16_556 ?
B1 B2 1.758(10) 4_665 ?
B1 B2 1.758(10) 4_675 ?
B1 B2 1.758(10) 4_565 ?
B2 W1 2.184(13) 1_455 ?
B2 W1 2.184(13) 1_565 ?
B2 B1 1.758(10) 4_674 ?
B2 B1 1.758(10) 4_564 ?
B2 B1 1.67(3) 16_556 ?
B2 B1 1.758(10) 4_664 ?

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
W1 W1 W1 120.0 3_765 1_565 ?
W1 W1 W1 120.0 3_775 1_455 ?
W1 W1 W1 180.0 3_765 1_455 ?
W1 W1 W1 60.0 1_455 1_565 ?
W1 W1 W1 60.0 3_775 1_565 ?
W1 W1 W1 60.0 3_765 3_775 ?
B1 W1 W1 90.000(1) 4_664 3_775 ?
B1 W1 W1 90.0 13_666 1_455 ?
B1 W1 W1 90.000(1) 13_666 3_775 ?
B1 W1 W1 90.0 4_664 3_765 ?
B1 W1 W1 90.0 13_666 3_765 ?
B1 W1 W1 90.0 4_664 1_565 ?
B1 W1 W1 90.0 13_666 1_565 ?
B1 W1 W1 90.000(1) 4_664 1_455 ?
B1 W1 B1 180.0 4_664 13_666 ?
B1 W1 B2 47.9(4) 13_666 16_656 ?
B1 W1 B2 47.9(4) 4_664 1_545 ?
B1 W1 B2 47.9(4) 4_664 1_655 ?
B1 W1 B2 132.1(4) 13_666 . ?
B1 W1 B2 132.1(4) 4_664 16_556 ?
B1 W1 B2 132.1(4) 4_664 16_546 ?
B1 W1 B2 132.1(4) 4_664 16_656 ?
B1 W1 B2 47.9(4) 4_664 . ?
B1 W1 B2 47.9(4) 13_666 16_556 ?
B1 W1 B2 132.1(4) 13_666 1_655 ?
B1 W1 B2 132.1(4) 13_666 1_545 ?
B1 W1 B2 47.9(4) 13_666 16_546 ?
B2 W1 W1 50.0(3) 16_656 3_765 ?
B2 W1 W1 50.0(3) 16_556 1_455 ?
B2 W1 W1 130.0(3) 1_655 1_455 ?
B2 W1 W1 90.000(1) 1_545 3_765 ?
B2 W1 W1 130.0(3) 16_546 1_565 ?
B2 W1 W1 90.0 16_546 3_765 ?
B2 W1 W1 90.0 1_545 1_455 ?
B2 W1 W1 130.0(3) 16_556 3_765 ?
B2 W1 W1 50.0(3) 1_655 3_765 ?
B2 W1 W1 50.0(3) . 1_565 ?
B2 W1 W1 90.0 16_656 1_565 ?
B2 W1 W1 90.000(1) 16_546 1_455 ?
B2 W1 W1 130.0(3) 1_545 3_775 ?
B2 W1 W1 50.0(3) 16_556 1_565 ?
B2 W1 W1 50.0(3) 16_656 3_775 ?
B2 W1 W1 130.0(3) 1_545 1_565 ?
B2 W1 W1 50.0(3) 1_655 3_775 ?
B2 W1 W1 130.0(3) . 3_765 ?
B2 W1 W1 90.000(1) 16_556 3_775 ?
B2 W1 W1 90.000(1) 1_655 1_565 ?
B2 W1 W1 90.000(1) . 3_775 ?
B2 W1 W1 130.0(3) 16_546 3_775 ?
B2 W1 W1 130.0(3) 16_656 1_455 ?
B2 W1 W1 50.0(3) . 1_455 ?
B2 W1 B2 84.2(7) 1_545 16_546 ?
B2 W1 B2 80.0(6) 1_545 . ?
B2 W1 B2 80.0(6) 16_656 16_546 ?
B2 W1 B2 80.0(6) 1_655 . ?
B2 W1 B2 84.2(7) 16_556 . ?
B2 W1 B2 80.0(6) 1_545 1_655 ?
B2 W1 B2 136.4(3) 16_546 1_655 ?
B2 W1 B2 136.4(3) 1_545 16_556 ?
B2 W1 B2 84.2(7) 16_656 1_655 ?
B2 W1 B2 80.0(6) 16_546 16_556 ?
B2 W1 B2 136.4(3) 1_545 16_656 ?
B2 W1 B2 136.4(3) 16_656 . ?
B2 W1 B2 80.0(6) 16_656 16_556 ?
B2 W1 B2 136.4(3) 16_546 . ?
B2 W1 B2 136.4(3) 1_655 16_556 ?
B1 B1 W1 121.5(9) 13_566 13_666 ?
B1 B1 W1 121.5(9) 13_676 13_666 ?
B1 B1 W1 121.5(9) 13_666 13_666 ?
B1 B1 B1 95.2(12) 13_566 13_676 ?
B1 B1 B1 95.2(12) 13_566 13_666 ?
B1 B1 B1 95.2(12) 13_676 13_666 ?
B2 B1 W1 180.0 16_556 13_666 ?
B2 B1 W1 67.2(8) 4_665 13_666 ?
B2 B1 W1 67.2(8) 4_675 13_666 ?
B2 B1 W1 67.2(8) 4_565 13_666 ?
B2 B1 B1 54.3(7) 4_665 13_666 ?
B2 B1 B1 58.5(9) 16_556 13_566 ?
B2 B1 B1 54.3(7) 4_675 13_676 ?
B2 B1 B1 54.3(7) 4_565 13_566 ?
B2 B1 B1 58.5(9) 16_556 13_676 ?
B2 B1 B1 126.6(2) 4_675 13_566 ?
B2 B1 B1 126.6(2) 4_675 13_666 ?
B2 B1 B1 126.5(2) 4_665 13_566 ?
B2 B1 B1 126.5(2) 4_665 13_676 ?
B2 B1 B1 58.5(9) 16_556 13_666 ?
B2 B1 B1 126.6(2) 4_565 13_676 ?
B2 B1 B1 126.6(2) 4_565 13_666 ?
B2 B1 B2 112.8(8) 16_556 4_565 ?
B2 B1 B2 105.9(9) 4_675 4_565 ?
B2 B1 B2 105.9(9) 4_675 4_665 ?
B2 B1 B2 112.8(8) 16_556 4_665 ?
B2 B1 B2 105.9(9) 4_565 4_665 ?
B2 B1 B2 112.8(8) 16_556 4_675 ?
W1 B2 W1 80.0(6) 1_565 1_455 ?
W1 B2 W1 80.0(6) 1_455 . ?
W1 B2 W1 80.0(6) 1_565 . ?
B1 B2 W1 64.9(6) 4_664 . ?
B1 B2 W1 127.0(5) 4_564 . ?
B1 B2 W1 64.9(6) 4_674 1_565 ?
B1 B2 W1 132.1(4) 16_556 1_455 ?
B1 B2 W1 132.1(4) 16_556 1_565 ?
B1 B2 W1 132.1(4) 16_556 . ?
B1 B2 W1 64.9(6) 4_564 1_455 ?
B1 B2 W1 127.0(5) 4_664 1_455 ?
B1 B2 W1 127.0(5) 4_674 . ?
B1 B2 W1 127.0(5) 4_564 1_565 ?
B1 B2 W1 127.0(5) 4_664 1_565 ?
B1 B2 W1 127.0(5) 4_674 1_455 ?
B1 B2 B1 67.2(8) 16_556 4_664 ?
B1 B2 B1 105.9(9) 4_564 4_664 ?
B1 B2 B1 105.9(9) 4_674 4_664 ?
B1 B2 B1 67.2(8) 16_556 4_564 ?
B1 B2 B1 67.2(8) 16_556 4_674 ?
B1 B2 B1 105.9(9) 4_564 4_674 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.746
_oxdiff_exptl_absorpt_empirical_full_min 0.683
_vrf_PLAT029_WB4_47_9GPa         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.587 Why?  
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
_vrf_PLAT911_WB4_47_9GPa         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         15 Report
RESPONSE: The dataset was incomplete since the data were collected in
 a diamond anvil cell metallic body of which shadows
 more than 60% of the reflections.
;
