# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_20210620e
_database_code_depnum_ccdc_archive 'CCDC 2091528'
loop_
_audit_author_name
_audit_author_address
'Xizhu Zhang'
;University of Jinan
China
;
_audit_update_record             
;
2021-06-22 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
_audit_creation_date             2021-06-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'O31 P W9, C8 H13 N2, 0.5(O)'
_chemical_formula_sum            'C8 H13 N2 O31.50 P W9'
_chemical_formula_weight         2326.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         PWCON
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   12.2103(3)
_cell_length_b                   22.9104(4)
_cell_length_c                   27.6227(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7727.2(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7660
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.2900
_cell_measurement_theta_min      3.1750
_shelx_estimated_absorpt_T_max   0.084
_shelx_estimated_absorpt_T_min   0.084
_exptl_absorpt_coefficient_mu    49.304
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45987
_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            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             8064
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23740
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.200
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     28.00  74.00   1.00    0.56    --   48.45 -83.00  24.00   46
  2  ω    -27.00  27.00   1.00    0.56    --  -48.45  19.00  60.00   54
  3  ω   -120.00 -75.00   1.00    0.56    --  -48.45-125.00 150.00   45
  4  ω    -44.00 -13.00   1.00    1.30    --  -86.25  39.00  -5.00   31
  5  ω    -43.00 -16.00   1.00    1.30    --  -86.25  38.00  90.00   27
  6  ω    114.00 174.00   1.00    1.30    --  106.49  83.00 145.00   60
  7  ω     34.00  64.00   1.00    1.30    --  106.49 -57.00  60.00   30
  8  ω     34.00  66.00   1.00    1.30    --  106.49 -57.00 -90.00   32
  9  ω     35.00  87.00   1.00    1.30    --  106.49 -77.00-180.00   52
 10  ω     52.00 106.00   1.00    1.30    --  106.49 -83.00  24.00   54
 11  ω     54.00 116.00   1.00    1.30    --  106.49-149.00 -25.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0090456000
_diffrn_orient_matrix_UB_12      -0.0041507000
_diffrn_orient_matrix_UB_13      0.0555319000
_diffrn_orient_matrix_UB_21      0.1102437000
_diffrn_orient_matrix_UB_22      0.0326852000
_diffrn_orient_matrix_UB_23      -0.0017654000
_diffrn_orient_matrix_UB_31      -0.0607252000
_diffrn_orient_matrix_UB_32      0.0585953000
_diffrn_orient_matrix_UB_33      0.0049540000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5812
_reflns_number_total             6821
_reflns_odcompleteness_completeness 98.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.664
_refine_diff_density_min         -1.972
_refine_diff_density_rms         0.322
_refine_ls_extinction_coef       0.0000068(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6821
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0396
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0404P)²+148.1687P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0956
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C43) \\sim Ueq, Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O24) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O28) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) = Uanis(O1) = Uanis(O2)
3. Rigid body (RIGU) restrains
 W9, O24, C43, C51, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Others
 1*[Sof(O1)]+1*[Sof(O2)]+1*[Sof(O3)]=1 with esd of 0.0001
5.a Secondary CH2 refined with riding coordinates:
 C48(H48a,H48b), C47(H47a,H47b), C46(H46a,H46b)
5.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C44(H44), C50(H50), C42(H42)
5.c Idealised Me refined as rotating group:
 N49(H49a,H49b,H49c)
;
_atom_sites_solution_hydrogens   geom
_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 0.43981(5) 0.60966(2) 0.60222(2) 0.01488(14) Uani 1 1 d . . . . .
W2 W 0.67888(5) 0.82040(2) 0.91811(2) 0.01624(14) Uani 1 1 d . . . . .
W3 W 0.26531(5) 0.70699(2) 0.83334(2) 0.01584(14) Uani 1 1 d . . . . .
W4 W 0.76299(5) 0.70028(2) 0.83618(2) 0.01602(14) Uani 1 1 d . . . . .
W5 W 0.26563(5) 0.65315(2) 0.70537(2) 0.01649(14) Uani 1 1 d . . . . .
W6 W 0.52566(5) 0.63133(2) 0.85664(2) 0.01640(14) Uani 1 1 d . . . . .
W7 W 0.76471(5) 0.64815(2) 0.70786(2) 0.01652(14) Uani 1 1 d . . . . .
W8 W 0.52751(5) 0.57837(2) 0.72812(2) 0.01700(14) Uani 1 1 d . . . . .
W9 W 0.43713(5) 0.74891(2) 0.56224(2) 0.01808(14) Uani 1 1 d . . . . .
P10 P 0.5183(2) 0.77804(11) 0.81786(10) 0.0107(6) Uani 1 1 d . . . . .
O15 O 0.5811(7) 0.7751(3) 0.9582(3) 0.0176(18) Uani 1 1 d . . . . .
O16 O 0.5055(6) 0.5800(3) 0.6587(3) 0.0134(17) Uani 1 1 d . . . . .
O17 O 0.3215(7) 0.6331(3) 0.6427(3) 0.0160(18) Uani 1 1 d . . . . .
O18 O 0.2460(7) 0.6866(4) 0.7682(3) 0.0195(18) Uani 1 1 d . . . . .
O19 O 0.7309(7) 0.8552(3) 0.8600(3) 0.0160(18) Uani 1 1 d . . . . .
O20 O 0.5810(7) 0.8861(3) 0.9279(3) 0.0175(18) Uani 1 1 d . . . . .
O21 O 0.3948(7) 0.6693(4) 0.5575(3) 0.0172(18) Uani 1 1 d . . . . .
O22 O 0.7606(7) 0.6619(3) 0.7753(3) 0.0178(18) Uani 1 1 d . . . . .
O23 O 0.3825(7) 0.6534(4) 0.8370(3) 0.0185(18) Uani 1 1 d . . . . .
O24 O 0.3225(7) 0.7620(3) 0.6058(3) 0.0164(17) Uani 1 1 d . U . . .
O12 O 0.5778(6) 0.8241(3) 0.7872(3) 0.0117(16) Uani 1 1 d . . . . .
O25 O 0.5474(7) 0.6000(3) 0.7932(3) 0.0159(18) Uani 1 1 d . . . . .
O26 O 0.7283(6) 0.7490(3) 0.8915(3) 0.0157(17) Uani 1 1 d . . . . .
O27 O 0.1959(7) 0.7808(4) 0.8223(3) 0.0185(18) Uani 1 1 d . . . . .
O28 O 0.6808(7) 0.6381(3) 0.8640(3) 0.0167(18) Uani 1 1 d . U . . .
O29 O 0.3838(7) 0.6093(3) 0.7306(3) 0.0173(18) Uani 1 1 d . . . . .
O30 O 0.8929(7) 0.6799(4) 0.8542(3) 0.024(2) Uani 1 1 d . . . . .
O31 O 0.5041(7) 0.6834(4) 0.9091(3) 0.0207(19) Uani 1 1 d . . . . .
O32 O 0.7883(7) 0.7712(3) 0.8032(3) 0.0180(18) Uani 1 1 d . . . . .
O11 O 0.3999(7) 0.7708(3) 0.8022(3) 0.0150(17) Uani 1 1 d . . . . .
O33 O 0.1582(7) 0.6691(4) 0.8580(3) 0.024(2) Uani 1 1 d . . . . .
O34 O 0.6812(7) 0.5779(3) 0.7174(3) 0.0186(18) Uani 1 1 d . . . . .
O35 O 0.3876(8) 0.7765(4) 0.5079(3) 0.0222(19) Uani 1 1 d . . . . .
O36 O 0.1579(8) 0.6053(4) 0.7048(3) 0.025(2) Uani 1 1 d . . . . .
O37 O 0.7812(8) 0.8370(4) 0.9583(3) 0.024(2) Uani 1 1 d . . . . .
O13 O 0.5791(7) 0.7194(3) 0.8180(3) 0.0151(17) Uani 1 1 d . . . . .
O38 O 0.3899(8) 0.5483(3) 0.5742(3) 0.0207(19) Uani 1 1 d . . . . .
O39 O 0.5031(8) 0.5680(4) 0.8875(3) 0.023(2) Uani 1 1 d . . . . .
O40 O 0.8942(8) 0.6208(4) 0.7040(3) 0.027(2) Uani 1 1 d . . . . .
O41 O 0.5073(8) 0.5045(4) 0.7351(4) 0.026(2) Uani 1 1 d . . . . .
N45 N 0.4942(9) 0.4317(5) 0.5805(4) 0.020(2) Uani 1 1 d . . . . .
O14 O 0.5179(6) 0.7998(3) 0.8721(3) 0.0137(17) Uani 1 1 d . . . . .
N49 N 0.4838(11) 0.2415(5) 0.5775(4) 0.030(3) Uani 1 1 d . . . . .
H49A H 0.513131 0.240907 0.547985 0.045 Uiso 1 1 calc R U . . .
H49B H 0.416704 0.226415 0.576392 0.045 Uiso 1 1 calc R U . . .
H49C H 0.525135 0.220631 0.597557 0.045 Uiso 1 1 calc R U . . .
C48 C 0.4777(10) 0.3034(6) 0.5952(5) 0.024(3) Uani 1 1 d . . . . .
H48A H 0.549960 0.320960 0.593974 0.029 Uiso 1 1 calc R U . . .
H48B H 0.452871 0.303902 0.628510 0.029 Uiso 1 1 calc R U . . .
C47 C 0.3982(11) 0.3388(6) 0.5635(5) 0.024(3) Uani 1 1 d . . . . .
H47A H 0.424845 0.339161 0.530394 0.029 Uiso 1 1 calc R U . . .
H47B H 0.327064 0.319871 0.563556 0.029 Uiso 1 1 calc R U . . .
C51 C 0.6463(12) 0.4668(6) 0.5370(5) 0.025(3) Uani 1 1 d . . . . .
H51 H 0.681731 0.472266 0.507505 0.030 Uiso 1 1 calc R U . . .
C46 C 0.3856(12) 0.4010(6) 0.5811(5) 0.030(3) Uani 1 1 d . . . . .
H46A H 0.334285 0.421612 0.560511 0.036 Uiso 1 1 calc R U . . .
H46B H 0.356539 0.400886 0.613811 0.036 Uiso 1 1 calc R U . . .
C43 C 0.6966(10) 0.4858(5) 0.5803(4) 0.014(2) Uani 1 1 d . U . . .
C44 C 0.5476(12) 0.4408(5) 0.5381(4) 0.022(3) Uani 1 1 d . . . . .
H44 H 0.515279 0.428808 0.509305 0.026 Uiso 1 1 calc R U . . .
C50 C 0.5382(10) 0.4507(5) 0.6227(4) 0.017(3) Uani 1 1 d . U . . .
H50 H 0.500047 0.445768 0.651529 0.021 Uiso 1 1 calc R U . . .
C42 C 0.6384(12) 0.4770(5) 0.6229(5) 0.020(3) Uani 1 1 d . . . . .
H42 H 0.668421 0.489290 0.652150 0.024 Uiso 1 1 calc R U . . .
O1 O 0.250000 0.500000 0.792(5) 0.059(8) Uani 0.135(3) 2 d S T P A 1
O2 O 0.250000 0.500000 0.8114(16) 0.059(8) Uani 0.423(3) 2 d S T P B 2
O3 O 0.250000 0.500000 0.8557(15) 0.059(8) Uani 0.443(3) 2 d S T P C 3


_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 O16 1.881(8) . ?
W1 O17 1.904(8) . ?
W1 O20 1.917(9) 4_566 ?
W1 O21 1.923(8) . ?
W1 O38 1.716(8) . ?
W1 O14 2.390(8) 4_566 ?
W2 O15 1.931(8) . ?
W2 O19 1.903(8) . ?
W2 O20 1.940(8) . ?
W2 O26 1.892(8) . ?
W2 O37 1.713(9) . ?
W2 O14 2.387(8) . ?
W3 O18 1.874(8) . ?
W3 O23 1.889(8) . ?
W3 O24 1.955(8) 4_566 ?
W3 O27 1.915(8) . ?
W3 O11 2.361(8) . ?
W3 O33 1.710(9) . ?
W4 O22 1.897(8) . ?
W4 O26 1.939(8) . ?
W4 O28 1.903(8) . ?
W4 O30 1.726(9) . ?
W4 O32 1.888(8) . ?
W4 O13 2.343(8) . ?
W5 O17 1.917(9) . ?
W5 O18 1.912(8) . ?
W5 O27 1.898(8) 4_566 ?
W5 O29 1.891(9) . ?
W5 O11 2.402(8) 4_566 ?
W5 O36 1.712(9) . ?
W6 O23 1.899(8) . ?
W6 O25 1.912(8) . ?
W6 O28 1.912(8) . ?
W6 O31 1.895(8) . ?
W6 O13 2.374(8) . ?
W6 O39 1.705(8) . ?
W7 O19 1.920(8) 4_566 ?
W7 O22 1.891(9) . ?
W7 O12 2.374(8) 4_566 ?
W7 O32 1.895(8) 4_566 ?
W7 O34 1.923(9) . ?
W7 O40 1.703(9) . ?
W8 O16 1.937(8) . ?
W8 O12 2.356(8) 4_566 ?
W8 O25 1.880(8) . ?
W8 O29 1.894(9) . ?
W8 O34 1.900(9) . ?
W8 O41 1.721(8) . ?
W9 O15 1.928(9) 4_566 ?
W9 O21 1.900(8) . ?
W9 O24 1.869(8) . ?
W9 O31 1.924(8) 4_566 ?
W9 O35 1.737(8) . ?
W9 O14 2.347(8) 4_566 ?
P10 O12 1.536(8) . ?
P10 O11 1.518(9) . ?
P10 O13 1.536(8) . ?
P10 O14 1.580(8) . ?
N45 C46 1.502(18) . ?
N45 C44 1.355(17) . ?
N45 C50 1.355(16) . ?
N49 H49A 0.8900 . ?
N49 H49B 0.8900 . ?
N49 H49C 0.8900 . ?
N49 C48 1.500(18) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 C47 1.539(19) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C47 C46 1.51(2) . ?
C51 H51 0.9300 . ?
C51 C43 1.414(17) . ?
C51 C44 1.35(2) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C43 C43 1.46(2) 2_665 ?
C43 C42 1.390(17) . ?
C44 H44 0.9300 . ?
C50 H50 0.9300 . ?
C50 C42 1.364(19) . ?
C42 H42 0.9300 . ?

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
O16 W1 O17 86.5(3) . . ?
O16 W1 O20 89.7(3) . 4_566 ?
O16 W1 O21 155.8(3) . . ?
O16 W1 O14 84.1(3) . 4_566 ?
O17 W1 O20 157.4(3) . 4_566 ?
O17 W1 O21 87.7(3) . . ?
O17 W1 O14 83.4(3) . 4_566 ?
O20 W1 O21 86.6(3) 4_566 . ?
O20 W1 O14 74.1(3) 4_566 4_566 ?
O21 W1 O14 71.8(3) . 4_566 ?
O38 W1 O16 103.3(4) . . ?
O38 W1 O17 103.1(4) . . ?
O38 W1 O20 99.5(4) . 4_566 ?
O38 W1 O21 100.9(4) . . ?
O38 W1 O14 170.4(3) . 4_566 ?
O15 W2 O20 87.5(4) . . ?
O15 W2 O14 72.0(3) . . ?
O19 W2 O15 156.4(3) . . ?
O19 W2 O20 89.9(3) . . ?
O19 W2 O14 84.7(3) . . ?
O20 W2 O14 73.8(3) . . ?
O26 W2 O15 87.5(3) . . ?
O26 W2 O19 85.9(3) . . ?
O26 W2 O20 157.1(4) . . ?
O26 W2 O14 83.4(3) . . ?
O37 W2 O15 101.4(4) . . ?
O37 W2 O19 102.1(4) . . ?
O37 W2 O20 100.7(4) . . ?
O37 W2 O26 102.2(4) . . ?
O37 W2 O14 171.3(4) . . ?
O18 W3 O23 89.1(4) . . ?
O18 W3 O24 164.1(4) . 4_566 ?
O18 W3 O27 90.7(4) . . ?
O18 W3 O11 83.8(3) . . ?
O23 W3 O24 85.4(3) . 4_566 ?
O23 W3 O27 156.6(4) . . ?
O23 W3 O11 83.9(3) . . ?
O24 W3 O11 80.8(3) 4_566 . ?
O27 W3 O24 88.5(3) . 4_566 ?
O27 W3 O11 72.8(3) . . ?
O33 W3 O18 99.2(4) . . ?
O33 W3 O23 103.2(4) . . ?
O33 W3 O24 96.6(4) . 4_566 ?
O33 W3 O27 99.9(4) . . ?
O33 W3 O11 172.2(3) . . ?
O22 W4 O26 164.1(4) . . ?
O22 W4 O28 90.2(3) . . ?
O22 W4 O13 83.2(3) . . ?
O26 W4 O13 81.5(3) . . ?
O28 W4 O26 89.9(3) . . ?
O28 W4 O13 73.8(3) . . ?
O30 W4 O22 98.2(4) . . ?
O30 W4 O26 97.5(4) . . ?
O30 W4 O28 99.5(4) . . ?
O30 W4 O32 102.8(4) . . ?
O30 W4 O13 173.2(4) . . ?
O32 W4 O22 88.5(3) . . ?
O32 W4 O26 85.4(3) . . ?
O32 W4 O28 157.6(4) . . ?
O32 W4 O13 83.9(3) . . ?
O17 W5 O11 81.5(3) . 4_566 ?
O18 W5 O17 163.9(4) . . ?
O18 W5 O11 82.8(3) . 4_566 ?
O27 W5 O17 89.2(3) 4_566 . ?
O27 W5 O18 89.5(4) 4_566 . ?
O27 W5 O11 72.1(3) 4_566 4_566 ?
O29 W5 O17 86.2(3) . . ?
O29 W5 O18 88.5(4) . . ?
O29 W5 O27 156.2(4) . 4_566 ?
O29 W5 O11 84.1(3) . 4_566 ?
O36 W5 O17 96.4(4) . . ?
O36 W5 O18 99.7(4) . . ?
O36 W5 O27 99.3(4) . 4_566 ?
O36 W5 O29 104.4(4) . . ?
O36 W5 O11 171.1(4) . 4_566 ?
O23 W6 O25 88.0(4) . . ?
O23 W6 O28 157.1(3) . . ?
O23 W6 O13 84.2(3) . . ?
O25 W6 O13 82.4(3) . . ?
O28 W6 O25 89.4(4) . . ?
O28 W6 O13 72.9(3) . . ?
O31 W6 O23 85.6(4) . . ?
O31 W6 O25 163.0(4) . . ?
O31 W6 O28 90.3(4) . . ?
O31 W6 O13 81.3(3) . . ?
O39 W6 O23 102.7(4) . . ?
O39 W6 O25 99.3(4) . . ?
O39 W6 O28 100.2(4) . . ?
O39 W6 O31 97.5(4) . . ?
O39 W6 O13 172.9(4) . . ?
O19 W7 O12 82.0(3) 4_566 4_566 ?
O19 W7 O34 89.2(3) 4_566 . ?
O22 W7 O19 164.3(4) . 4_566 ?
O22 W7 O12 82.7(3) . 4_566 ?
O22 W7 O32 90.0(3) . 4_566 ?
O22 W7 O34 89.5(3) . . ?
O32 W7 O19 85.1(3) 4_566 4_566 ?
O32 W7 O12 83.9(3) 4_566 4_566 ?
O32 W7 O34 156.7(4) 4_566 . ?
O34 W7 O12 73.0(3) . 4_566 ?
O40 W7 O19 97.1(4) . 4_566 ?
O40 W7 O22 98.5(4) . . ?
O40 W7 O12 174.0(4) . 4_566 ?
O40 W7 O32 101.9(4) . 4_566 ?
O40 W7 O34 101.1(4) . . ?
O16 W8 O12 80.8(3) . 4_566 ?
O25 W8 O16 163.6(3) . . ?
O25 W8 O12 83.5(3) . 4_566 ?
O25 W8 O29 89.2(3) . . ?
O25 W8 O34 91.3(4) . . ?
O29 W8 O16 84.2(3) . . ?
O29 W8 O12 83.9(3) . 4_566 ?
O29 W8 O34 157.4(3) . . ?
O34 W8 O16 89.0(3) . . ?
O34 W8 O12 73.8(3) . 4_566 ?
O41 W8 O16 96.3(4) . . ?
O41 W8 O12 172.0(4) . 4_566 ?
O41 W8 O25 99.9(4) . . ?
O41 W8 O29 103.4(4) . . ?
O41 W8 O34 98.8(4) . . ?
O15 W9 O14 73.0(3) 4_566 4_566 ?
O21 W9 O15 87.3(3) . 4_566 ?
O21 W9 O31 156.7(4) . 4_566 ?
O21 W9 O14 73.2(3) . 4_566 ?
O24 W9 O15 156.6(4) . 4_566 ?
O24 W9 O21 89.7(3) . . ?
O24 W9 O31 85.7(4) . 4_566 ?
O24 W9 O14 83.9(3) . 4_566 ?
O31 W9 O15 87.9(4) 4_566 4_566 ?
O31 W9 O14 83.5(3) 4_566 4_566 ?
O35 W9 O15 99.7(4) . 4_566 ?
O35 W9 O21 101.2(4) . . ?
O35 W9 O24 103.7(4) . . ?
O35 W9 O31 102.1(4) . 4_566 ?
O35 W9 O14 170.7(4) . 4_566 ?
O12 P10 O14 107.9(4) . . ?
O11 P10 O12 111.7(5) . . ?
O11 P10 O13 111.4(4) . . ?
O11 P10 O14 107.6(5) . . ?
O13 P10 O12 111.9(5) . . ?
O13 P10 O14 106.0(4) . . ?
W9 O15 W2 123.3(4) 4_566 . ?
W1 O16 W8 152.5(4) . . ?
W1 O17 W5 150.2(5) . . ?
W3 O18 W5 162.9(5) . . ?
W2 O19 W7 151.5(4) . 4_566 ?
W1 O20 W2 122.2(4) 4_566 . ?
W9 O21 W1 124.0(4) . . ?
W7 O22 W4 161.8(5) . . ?
W3 O23 W6 152.3(5) . . ?
W9 O24 W3 151.6(5) . 4_566 ?
W8 O12 W7 90.4(3) 4_566 4_566 ?
P10 O12 W7 127.4(4) . 4_566 ?
P10 O12 W8 128.8(4) . 4_566 ?
W8 O25 W6 163.2(5) . . ?
W2 O26 W4 150.9(5) . . ?
W5 O27 W3 124.7(5) 4_566 . ?
W4 O28 W6 122.7(4) . . ?
W5 O29 W8 153.2(5) . . ?
W6 O31 W9 151.7(5) . 4_566 ?
W4 O32 W7 153.1(5) . 4_566 ?
W3 O11 W5 90.3(3) . 4_566 ?
P10 O11 W3 128.8(5) . . ?
P10 O11 W5 126.5(4) . 4_566 ?
W8 O34 W7 122.7(4) . . ?
W4 O13 W6 90.5(3) . . ?
P10 O13 W4 128.9(5) . . ?
P10 O13 W6 127.7(5) . . ?
C44 N45 C46 120.4(11) . . ?
C50 N45 C46 119.4(11) . . ?
C50 N45 C44 120.2(11) . . ?
W2 O14 W1 90.0(3) . 4_566 ?
W9 O14 W1 90.9(3) 4_566 4_566 ?
W9 O14 W2 91.6(3) 4_566 . ?
P10 O14 W1 123.8(4) . 4_566 ?
P10 O14 W2 124.4(4) . . ?
P10 O14 W9 125.7(4) . 4_566 ?
H49A N49 H49B 109.5 . . ?
H49A N49 H49C 109.5 . . ?
H49B N49 H49C 109.5 . . ?
C48 N49 H49A 109.5 . . ?
C48 N49 H49B 109.5 . . ?
C48 N49 H49C 109.5 . . ?
N49 C48 H48A 109.6 . . ?
N49 C48 H48B 109.6 . . ?
N49 C48 C47 110.1(12) . . ?
H48A C48 H48B 108.2 . . ?
C47 C48 H48A 109.6 . . ?
C47 C48 H48B 109.6 . . ?
C48 C47 H47A 109.2 . . ?
C48 C47 H47B 109.2 . . ?
H47A C47 H47B 107.9 . . ?
C46 C47 C48 112.1(12) . . ?
C46 C47 H47A 109.2 . . ?
C46 C47 H47B 109.2 . . ?
C43 C51 H51 119.8 . . ?
C44 C51 H51 119.8 . . ?
C44 C51 C43 120.3(12) . . ?
N45 C46 C47 110.4(11) . . ?
N45 C46 H46A 109.6 . . ?
N45 C46 H46B 109.6 . . ?
C47 C46 H46A 109.6 . . ?
C47 C46 H46B 109.6 . . ?
H46A C46 H46B 108.1 . . ?
C51 C43 C43 121.7(8) . 2_665 ?
C42 C43 C51 116.8(12) . . ?
C42 C43 C43 121.5(8) . 2_665 ?
N45 C44 H44 119.4 . . ?
C51 C44 N45 121.3(12) . . ?
C51 C44 H44 119.4 . . ?
N45 C50 H50 119.9 . . ?
N45 C50 C42 120.1(11) . . ?
C42 C50 H50 119.9 . . ?
C43 C42 H42 119.4 . . ?
C50 C42 C43 121.2(12) . . ?
C50 C42 H42 119.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O15 W2 O26 W4 130.6(9) . . . . ?
O15 W9 O21 W1 72.5(5) 4_566 . . . ?
O15 W9 O24 W3 48.8(15) 4_566 . . 4_566 ?
O16 W8 O25 W6 63(2) . . . . ?
O16 W8 O29 W5 -29.4(10) . . . . ?
O16 W8 O34 W7 85.3(5) . . . . ?
O17 W1 O16 W8 -25.5(10) . . . . ?
O17 W5 O29 W8 29.3(10) . . . . ?
O18 W3 O23 W6 136.8(11) . . . . ?
O18 W5 O29 W8 -135.5(10) . . . . ?
O19 W2 O26 W4 -26.7(9) . . . . ?
O19 W7 O22 W4 -70(2) 4_566 . . . ?
O20 W1 O16 W8 132.2(10) 4_566 . . . ?
O20 W2 O26 W4 53.2(15) . . . . ?
O21 W1 O16 W8 51.0(15) . . . . ?
O21 W9 O24 W3 131.5(10) . . . 4_566 ?
O22 W4 O32 W7 136.9(11) . . . 4_566 ?
O23 W3 O18 W5 -7.3(18) . . . . ?
O23 W6 O31 W9 -27.0(11) . . . 4_566 ?
O24 W3 O18 W5 62(2) 4_566 . . . ?
O24 W3 O23 W6 -28.3(11) 4_566 . . . ?
O24 W9 O21 W1 -84.3(5) . . . . ?
O12 W7 O22 W4 -82.5(16) 4_566 . . . ?
O12 W8 O25 W6 80.6(16) 4_566 . . . ?
O12 W8 O29 W5 52.0(10) 4_566 . . . ?
O12 W8 O34 W7 4.6(4) 4_566 . . . ?
O12 P10 O11 W3 179.1(5) . . . . ?
O12 P10 O11 W5 -53.6(7) . . . 4_566 ?
O12 P10 O13 W4 52.4(7) . . . . ?
O12 P10 O13 W6 -178.1(5) . . . . ?
O12 P10 O14 W1 58.4(6) . . . 4_566 ?
O12 P10 O14 W2 -58.9(6) . . . . ?
O12 P10 O14 W9 178.7(5) . . . 4_566 ?
O25 W6 O23 W3 -135.5(11) . . . . ?
O25 W6 O31 W9 41(2) . . . 4_566 ?
O25 W8 O29 W5 135.6(10) . . . . ?
O25 W8 O34 W7 -78.3(5) . . . . ?
O26 W4 O22 W7 66(2) . . . . ?
O26 W4 O32 W7 -28.4(11) . . . 4_566 ?
O27 W3 O18 W5 149.3(18) . . . . ?
O27 W3 O23 W6 47.1(17) . . . . ?
O27 W5 O29 W8 -50.2(15) 4_566 . . . ?
O28 W4 O22 W7 155.7(17) . . . . ?
O28 W4 O32 W7 50.1(17) . . . 4_566 ?
O28 W6 O23 W3 -51.7(17) . . . . ?
O28 W6 O31 W9 130.4(11) . . . 4_566 ?
O29 W8 O25 W6 -3.3(16) . . . . ?
O29 W8 O34 W7 12.9(12) . . . . ?
O30 W4 O22 W7 -104.7(17) . . . . ?
O30 W4 O32 W7 -125.0(11) . . . 4_566 ?
O31 W6 O23 W3 28.7(11) . . . . ?
O31 W9 O21 W1 -5.9(12) 4_566 . . . ?
O31 W9 O24 W3 -25.7(10) 4_566 . . 4_566 ?
O32 W4 O22 W7 -2.0(17) . . . . ?
O32 W7 O22 W4 1.4(17) 4_566 . . . ?
O11 W3 O18 W5 76.7(18) . . . . ?
O11 W3 O23 W6 52.9(11) . . . . ?
O11 W5 O29 W8 -52.6(10) 4_566 . . . ?
O11 P10 O12 W7 -177.4(5) . . . 4_566 ?
O11 P10 O12 W8 53.9(7) . . . 4_566 ?
O11 P10 O13 W4 178.2(5) . . . . ?
O11 P10 O13 W6 -52.3(7) . . . . ?
O11 P10 O14 W1 -62.2(6) . . . 4_566 ?
O11 P10 O14 W2 -179.5(4) . . . . ?
O11 P10 O14 W9 58.1(6) . . . 4_566 ?
O33 W3 O18 W5 -110.5(18) . . . . ?
O33 W3 O23 W6 -124.0(11) . . . . ?
O34 W7 O22 W4 -155.4(17) . . . . ?
O34 W8 O25 W6 154.1(16) . . . . ?
O34 W8 O29 W5 44.0(15) . . . . ?
O35 W9 O21 W1 171.9(5) . . . . ?
O35 W9 O24 W3 -127.1(10) . . . 4_566 ?
O36 W5 O29 W8 124.9(10) . . . . ?
O37 W2 O26 W4 -128.3(9) . . . . ?
O13 W4 O22 W7 82.0(16) . . . . ?
O13 W4 O32 W7 53.6(11) . . . 4_566 ?
O13 W6 O23 W3 -52.9(11) . . . . ?
O13 W6 O31 W9 57.8(11) . . . 4_566 ?
O13 P10 O12 W7 -51.7(6) . . . 4_566 ?
O13 P10 O12 W8 179.6(5) . . . 4_566 ?
O13 P10 O11 W3 53.1(7) . . . . ?
O13 P10 O11 W5 -179.5(5) . . . 4_566 ?
O13 P10 O14 W1 178.4(5) . . . 4_566 ?
O13 P10 O14 W2 61.2(6) . . . . ?
O13 P10 O14 W9 -61.2(6) . . . 4_566 ?
O38 W1 O16 W8 -128.1(10) . . . . ?
O39 W6 O23 W3 125.4(11) . . . . ?
O39 W6 O31 W9 -129.3(11) . . . 4_566 ?
O40 W7 O22 W4 103.5(17) . . . . ?
O41 W8 O25 W6 -106.8(16) . . . . ?
O41 W8 O29 W5 -124.4(10) . . . . ?
O41 W8 O34 W7 -178.5(5) . . . . ?
N45 C50 C42 C43 1.1(17) . . . . ?
O14 W1 O16 W8 58.2(10) 4_566 . . . ?
O14 W2 O26 W4 58.5(9) . . . . ?
O14 W9 O21 W1 -0.5(4) 4_566 . . . ?
O14 W9 O24 W3 58.3(9) 4_566 . . 4_566 ?
O14 P10 O12 W7 64.6(6) . . . 4_566 ?
O14 P10 O12 W8 -64.1(6) . . . 4_566 ?
O14 P10 O11 W3 -62.7(6) . . . . ?
O14 P10 O11 W5 64.6(6) . . . 4_566 ?
O14 P10 O13 W4 -65.1(7) . . . . ?
O14 P10 O13 W6 64.4(6) . . . . ?
N49 C48 C47 C46 177.7(11) . . . . ?
C48 C47 C46 N45 59.9(15) . . . . ?
C51 C43 C42 C50 0.6(17) . . . . ?
C46 N45 C44 C51 -178.1(12) . . . . ?
C46 N45 C50 C42 177.9(11) . . . . ?
C43 C51 C44 N45 -0.6(19) . . . . ?
C43 C43 C42 C50 179.7(13) 2_665 . . . ?
C44 N45 C46 C47 63.6(15) . . . . ?
C44 N45 C50 C42 -2.6(17) . . . . ?
C44 C51 C43 C43 -180.0(14) . . . 2_665 ?
C44 C51 C43 C42 -0.9(18) . . . . ?
C50 N45 C46 C47 -116.8(12) . . . . ?
C50 N45 C44 C51 2.3(18) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.807 -0.153 0.865 1766.8 608.1 ?
2 0.250 0.000 0.834 24.9 0.0 ?
3 0.250 0.500 0.666 24.9 0.0 ?
4 0.750 0.000 0.166 24.9 0.0 ?
5 0.750 0.500 0.334 24.9 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.954
_oxdiff_exptl_absorpt_empirical_full_min 0.599
