# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_2018rwz614a
_database_code_depnum_ccdc_archive 'CCDC 1854218'
_audit_update_record             
;
2018-07-06 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H32 F4 P4 W, 2 (O W F5), C2 H3 N'
_chemical_formula_sum            'C22 H35 F14 N O2 P4 W3'
_chemical_formula_weight         1286.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

_cell_length_a                   16.7303(10)
_cell_length_b                   17.878(2)
_cell_length_c                   24.095(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7206.9(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15431
_cell_measurement_theta_min      1.8490
_cell_measurement_theta_max      29.6340

_exptl_crystal_description       fragment
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4784
_exptl_absorpt_coefficient_mu    9.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.37576
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'


_diffrn_radiation_wavelength     0.71073

_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
;
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector
;
_diffrn_detector                 'CCD plate'

_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a


_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo

_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .




_diffrn_ambient_temperature      100(2)





_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39879
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         26.00
_reflns_number_total             7082
_reflns_number_gt                5357
_reflns_threshold_expression     >2σ(I)

_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0371P)²+93.4172P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7082
_refine_ls_number_parameters     424
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0863
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      8.096
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.56185(12) 0.24091(11) 0.56495(9) 0.0214(5) Uani 1 1 d D . .
P1 P 0.6818(8) 0.2598(8) 0.6307(6) 0.026(3) Uani 1 1 d . . .
P2 P 0.5535(10) 0.1384(8) 0.6402(6) 0.030(3) Uani 1 1 d . . .
P3 P 0.4575(8) 0.3382(8) 0.5343(6) 0.024(3) Uani 1 1 d . . .
P4 P 0.5516(8) 0.2341(8) 0.4577(6) 0.026(3) Uani 1 1 d . . .
F1 F 0.6280(18) 0.3229(17) 0.5413(12) 0.029(7) Uani 1 1 d . . .
F2 F 0.4705(18) 0.1779(16) 0.5539(13) 0.028(7) Uani 1 1 d . . .
F3 F 0.6340(18) 0.1680(17) 0.5359(12) 0.031(8) Uani 1 1 d . . .
F4 F 0.5156(18) 0.2928(16) 0.6272(12) 0.026(7) Uani 1 1 d . . .
C1 C 0.773(3) 0.241(4) 0.594(3) 0.045(17) Uani 1 1 d . . .
H1A H 0.8186 0.2487 0.6186 0.067 Uiso 1 1 calc R . .
H1B H 0.7773 0.2753 0.5620 0.067 Uiso 1 1 calc R . .
H1C H 0.7727 0.1894 0.5804 0.067 Uiso 1 1 calc R . .
C2 C 0.685(4) 0.356(3) 0.653(3) 0.040(16) Uani 1 1 d . . .
H2A H 0.6366 0.3684 0.6735 0.061 Uiso 1 1 calc R . .
H2B H 0.6897 0.3889 0.6204 0.061 Uiso 1 1 calc R . .
H2C H 0.7320 0.3638 0.6770 0.061 Uiso 1 1 calc R . .
C3 C 0.681(3) 0.203(3) 0.693(2) 0.033(14) Uani 1 1 d . . .
C4 C 0.736(4) 0.214(4) 0.736(3) 0.044(17) Uani 1 1 d . . .
H4A H 0.7769 0.2505 0.7326 0.053 Uiso 1 1 calc R . .
C5 C 0.728(4) 0.172(4) 0.784(3) 0.052(19) Uani 1 1 d D . .
H5A H 0.7641 0.1802 0.8135 0.062 Uiso 1 1 calc R . .
C6 C 0.670(4) 0.118(4) 0.789(3) 0.06(2) Uani 1 1 d D . .
H6A H 0.6664 0.0884 0.8213 0.066 Uiso 1 1 calc R . .
C7 C 0.616(4) 0.106(3) 0.746(3) 0.041(16) Uani 1 1 d . . .
H7A H 0.5755 0.0692 0.7489 0.049 Uiso 1 1 calc R . .
C8 C 0.621(4) 0.149(3) 0.698(2) 0.033(14) Uani 1 1 d . . .
C9 C 0.572(5) 0.049(3) 0.609(3) 0.05(2) Uani 1 1 d . . .
H9A H 0.6281 0.0461 0.5967 0.077 Uiso 1 1 calc R . .
H9B H 0.5371 0.0424 0.5764 0.077 Uiso 1 1 calc R . .
H9C H 0.5615 0.0090 0.6357 0.077 Uiso 1 1 calc R . .
C10 C 0.455(4) 0.137(4) 0.670(3) 0.044(17) Uani 1 1 d . . .
H10A H 0.4507 0.0951 0.6963 0.066 Uiso 1 1 calc R . .
H10B H 0.4150 0.1309 0.6408 0.066 Uiso 1 1 calc R . .
H10C H 0.4452 0.1840 0.6900 0.066 Uiso 1 1 calc R . .
C11 C 0.649(3) 0.240(4) 0.428(2) 0.039(15) Uani 1 1 d . . .
H11A H 0.6450 0.2388 0.3871 0.058 Uiso 1 1 calc R . .
H11B H 0.6815 0.1972 0.4402 0.058 Uiso 1 1 calc R . .
H11C H 0.6750 0.2865 0.4393 0.058 Uiso 1 1 calc R . .
C12 C 0.509(4) 0.145(3) 0.438(2) 0.039(16) Uani 1 1 d . . .
H12A H 0.4529 0.1432 0.4490 0.058 Uiso 1 1 calc R . .
H12B H 0.5385 0.1045 0.4565 0.058 Uiso 1 1 calc R . .
H12C H 0.5134 0.1386 0.3977 0.058 Uiso 1 1 calc R . .
C13 C 0.492(3) 0.306(3) 0.426(2) 0.027(13) Uani 1 1 d . . .
C14 C 0.489(4) 0.317(3) 0.369(2) 0.036(15) Uani 1 1 d . . .
H14A H 0.5191 0.2854 0.3446 0.044 Uiso 1 1 calc R . .
C15 C 0.441(4) 0.373(3) 0.348(3) 0.043(16) Uani 1 1 d D . .
H15A H 0.4389 0.3809 0.3087 0.051 Uiso 1 1 calc R . .
C16 C 0.397(4) 0.419(3) 0.382(2) 0.039(16) Uani 1 1 d D . .
H16A H 0.3644 0.4572 0.3665 0.047 Uiso 1 1 calc R . .
C17 C 0.400(4) 0.409(3) 0.439(2) 0.033(14) Uani 1 1 d . . .
H17A H 0.3702 0.4406 0.4626 0.040 Uiso 1 1 calc R . .
C18 C 0.448(3) 0.353(3) 0.461(2) 0.024(12) Uani 1 1 d . . .
C19 C 0.362(3) 0.313(3) 0.562(3) 0.036(15) Uani 1 1 d . . .
H19A H 0.3650 0.3126 0.6024 0.054 Uiso 1 1 calc R . .
H19B H 0.3478 0.2629 0.5485 0.054 Uiso 1 1 calc R . .
H19C H 0.3222 0.3491 0.5495 0.054 Uiso 1 1 calc R . .
C20 C 0.485(4) 0.428(3) 0.562(2) 0.032(14) Uani 1 1 d . . .
H20A H 0.4424 0.4641 0.5535 0.049 Uiso 1 1 calc R . .
H20B H 0.5348 0.4444 0.5448 0.049 Uiso 1 1 calc R . .
H20C H 0.4915 0.4239 0.6021 0.049 Uiso 1 1 calc R . .
W2 W 0.94114(16) 0.36911(14) 0.74599(11) 0.0372(6) Uani 1 1 d D . .
W3 W 0.71760(15) -0.04360(13) 0.46938(11) 0.0353(6) Uani 1 1 d . . .
F5 F 0.999(3) 0.423(3) 0.6924(17) 0.069(13) Uani 1 1 d . . .
F6 F 0.855(3) 0.433(2) 0.7321(19) 0.065(13) Uani 1 1 d . . .
F7 F 0.879(2) 0.312(3) 0.7950(17) 0.062(12) Uani 1 1 d . . .
F8 F 0.898(3) 0.313(2) 0.6870(17) 0.061(12) Uani 1 1 d . . .
F9 F 1.025(3) 0.301(3) 0.750(2) 0.072(14) Uani 1 1 d . . .
F10 F 0.741(3) -0.020(3) 0.5435(18) 0.087(17) Uani 1 1 d . . .
F11 F 0.701(3) -0.065(4) 0.3961(19) 0.099(19) Uani 1 1 d . . .
F12 F 0.828(3) -0.055(3) 0.460(2) 0.076(15) Uani 1 1 d . . .
F13 F 0.610(2) -0.026(2) 0.480(2) 0.063(13) Uani 1 1 d . . .
F14 F 0.729(3) 0.058(2) 0.453(2) 0.076(15) Uani 1 1 d . . .
O1 O 0.979(4) 0.428(3) 0.7982(19) 0.070(17) Uani 1 1 d D . .
O2 O 0.706(3) -0.139(3) 0.491(3) 0.077(18) Uani 1 1 d D . .
N1 N 0.341(5) 0.483(4) 0.257(3) 0.07(2) Uani 1 1 d . . .
C21 C 0.325(4) 0.529(4) 0.226(3) 0.052(19) Uani 1 1 d . . .
C22 C 0.306(5) 0.587(5) 0.188(3) 0.07(2) Uani 1 1 d . . .
H22A H 0.2479 0.5895 0.1834 0.098 Uiso 1 1 calc R . .
H22B H 0.3313 0.5767 0.1523 0.098 Uiso 1 1 calc R . .
H22C H 0.3256 0.6349 0.2026 0.098 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 F3 1.91(3) . ?
W1 F2 1.92(3) . ?
W1 F1 1.92(3) . ?
W1 F4 1.93(3) . ?
W1 P3 2.572(14) . ?
W1 P1 2.579(14) . ?
W1 P2 2.582(14) . ?
W1 P4 2.592(14) . ?
P1 C1 1.80(6) . ?
P1 C3 1.80(6) . ?
P1 C2 1.81(6) . ?
P2 C8 1.79(6) . ?
P2 C10 1.80(6) . ?
P2 C9 1.80(6) . ?
P3 C19 1.78(6) . ?
P3 C20 1.79(5) . ?
P3 C18 1.80(5) . ?
P4 C11 1.79(6) . ?
P4 C13 1.80(5) . ?
P4 C12 1.81(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.40(9) . ?
C3 C8 1.40(8) . ?
C4 C5 1.38(9) . ?
C4 H4A 0.9500 . ?
C5 C6 1.38(9) . ?
C5 H5A 0.9500 . ?
C6 C7 1.39(10) . ?
C6 H6A 0.9500 . ?
C7 C8 1.39(8) . ?
C7 H7A 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.39(8) . ?
C13 C18 1.39(7) . ?
C14 C15 1.39(9) . ?
C14 H14A 0.9500 . ?
C15 C16 1.38(8) . ?
C15 H15A 0.9500 . ?
C16 C17 1.38(8) . ?
C16 H16A 0.9500 . ?
C17 C18 1.39(8) . ?
C17 H17A 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
W2 O1 1.76(5) . ?
W2 F9 1.85(4) . ?
W2 F6 1.87(4) . ?
W2 F7 1.87(4) . ?
W2 F5 1.88(4) . ?
W2 F8 1.89(4) . ?
W3 O2 1.79(5) . ?
W3 F11 1.83(5) . ?
W3 F13 1.86(4) . ?
W3 F14 1.87(4) . ?
W3 F12 1.87(4) . ?
W3 F10 1.88(4) . ?
N1 C21 1.13(9) . ?
C21 C22 1.43(11) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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
F3 W1 F2 93.0(13) . . ?
F3 W1 F1 92.7(13) . . ?
F2 W1 F1 150.0(13) . . ?
F3 W1 F4 150.2(13) . . ?
F2 W1 F4 94.1(13) . . ?
F1 W1 F4 95.4(13) . . ?
F3 W1 P3 141.7(10) . . ?
F2 W1 P3 79.5(9) . . ?
F1 W1 P3 77.9(10) . . ?
F4 W1 P3 68.0(9) . . ?
F3 W1 P1 79.8(10) . . ?
F2 W1 P1 141.5(10) . . ?
F1 W1 P1 68.5(9) . . ?
F4 W1 P1 76.7(9) . . ?
P3 W1 P1 128.0(4) . . ?
F3 W1 P2 78.9(10) . . ?
F2 W1 P2 68.7(10) . . ?
F1 W1 P2 141.3(9) . . ?
F4 W1 P2 76.9(9) . . ?
P3 W1 P2 130.1(5) . . ?
P1 W1 P2 72.8(5) . . ?
F3 W1 P4 69.2(9) . . ?
F2 W1 P4 77.4(10) . . ?
F1 W1 P4 77.2(9) . . ?
F4 W1 P4 140.6(9) . . ?
P3 W1 P4 72.6(4) . . ?
P1 W1 P4 132.0(4) . . ?
P2 W1 P4 131.5(5) . . ?
C1 P1 C3 108(3) . . ?
C1 P1 C2 107(3) . . ?
C3 P1 C2 107(3) . . ?
C1 P1 W1 109(2) . . ?
C3 P1 W1 115(2) . . ?
C2 P1 W1 109(2) . . ?
C8 P2 C10 105(3) . . ?
C8 P2 C9 108(3) . . ?
C10 P2 C9 108(3) . . ?
C8 P2 W1 115(2) . . ?
C10 P2 W1 110(2) . . ?
C9 P2 W1 109(2) . . ?
C19 P3 C20 108(3) . . ?
C19 P3 C18 109(3) . . ?
C20 P3 C18 105(3) . . ?
C19 P3 W1 109(2) . . ?
C20 P3 W1 109.1(19) . . ?
C18 P3 W1 116.2(18) . . ?
C11 P4 C13 107(3) . . ?
C11 P4 C12 108(3) . . ?
C13 P4 C12 108(3) . . ?
C11 P4 W1 110(2) . . ?
C13 P4 W1 115.3(19) . . ?
C12 P4 W1 109(2) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C8 120(6) . . ?
C4 C3 P1 122(5) . . ?
C8 C3 P1 117(4) . . ?
C5 C4 C3 119(6) . . ?
C5 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
C4 C5 C6 121(6) . . ?
C4 C5 H5A 119.4 . . ?
C6 C5 H5A 119.4 . . ?
C5 C6 C7 120(6) . . ?
C5 C6 H6A 120.0 . . ?
C7 C6 H6A 120.0 . . ?
C6 C7 C8 120(6) . . ?
C6 C7 H7A 120.0 . . ?
C8 C7 H7A 120.0 . . ?
C7 C8 C3 120(6) . . ?
C7 C8 P2 123(5) . . ?
C3 C8 P2 118(4) . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P4 C11 H11A 109.5 . . ?
P4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P4 C12 H12A 109.5 . . ?
P4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
P4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 120(5) . . ?
C14 C13 P4 123(4) . . ?
C18 C13 P4 118(4) . . ?
C15 C14 C13 119(6) . . ?
C15 C14 H14A 120.6 . . ?
C13 C14 H14A 120.6 . . ?
C16 C15 C14 122(6) . . ?
C16 C15 H15A 119.2 . . ?
C14 C15 H15A 119.2 . . ?
C15 C16 C17 120(6) . . ?
C15 C16 H16A 120.1 . . ?
C17 C16 H16A 120.1 . . ?
C16 C17 C18 119(5) . . ?
C16 C17 H17A 120.3 . . ?
C18 C17 H17A 120.3 . . ?
C17 C18 C13 121(5) . . ?
C17 C18 P3 122(4) . . ?
C13 C18 P3 117(4) . . ?
P3 C19 H19A 109.5 . . ?
P3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
P3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
P3 C20 H20A 109.5 . . ?
P3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
P3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1 W2 F9 94(3) . . ?
O1 W2 F6 93(2) . . ?
F9 W2 F6 172(2) . . ?
O1 W2 F7 94(2) . . ?
F9 W2 F7 91(2) . . ?
F6 W2 F7 91.1(19) . . ?
O1 W2 F5 90(2) . . ?
F9 W2 F5 89(2) . . ?
F6 W2 F5 88(2) . . ?
F7 W2 F5 175.6(18) . . ?
O1 W2 F8 176(2) . . ?
F9 W2 F8 89(2) . . ?
F6 W2 F8 84.1(19) . . ?
F7 W2 F8 88.4(19) . . ?
F5 W2 F8 87.3(19) . . ?
O2 W3 F11 94(3) . . ?
O2 W3 F13 91(2) . . ?
F11 W3 F13 92(2) . . ?
O2 W3 F14 175(3) . . ?
F11 W3 F14 91(3) . . ?
F13 W3 F14 88(2) . . ?
O2 W3 F12 93(2) . . ?
F11 W3 F12 90(2) . . ?
F13 W3 F12 176(2) . . ?
F14 W3 F12 88(2) . . ?
O2 W3 F10 88(3) . . ?
F11 W3 F10 176(2) . . ?
F13 W3 F10 92(2) . . ?
F14 W3 F10 88(2) . . ?
F12 W3 F10 86(2) . . ?
N1 C21 C22 179(9) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.825
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.208


# start Validation Reply Form
_vrf_PLAT342_2018rwz614a         
;
PROBLEM: Low Bond Precision on  C-C Bonds ..........0.08615 Ang. 
RESPONSE: The crystal sample is extremely air-sensitve. 
We have tried several times but can't get better quality data collected

;

# end Validation Reply Form

####################################################################### 
# 
# 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_2018rwz621b
_database_code_depnum_ccdc_archive 'CCDC 1854219'
_audit_update_record             
;
2018-07-06 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H32 As4 F4 W, W F8'
_chemical_formula_sum            'C20 H32 As4 F12 W2'
_chemical_formula_weight         1167.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ' orthorhombic '

_symmetry_space_group_name_H-M   'F d d d'

_space_group_name_Hall           '-F 2uv 2vw'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   13.1003(10)
_cell_length_b                   21.3132(10)
_cell_length_c                   21.3804(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5969.6(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2580
_cell_measurement_theta_min      2.0350
_cell_measurement_theta_max      27.7820

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4320
_exptl_absorpt_coefficient_mu    12.188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.25533
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;  
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  
;
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0527542000
_diffrn_orient_matrix_UB_12      0.0062650500
_diffrn_orient_matrix_UB_13      -0.0040591500
_diffrn_orient_matrix_UB_21      -0.0093586000
_diffrn_orient_matrix_UB_22      0.0091677500
_diffrn_orient_matrix_UB_23      -0.0313849500
_diffrn_orient_matrix_UB_31      -0.0079123000
_diffrn_orient_matrix_UB_32      0.0313817000
_diffrn_orient_matrix_UB_33      0.0098964000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .




_diffrn_ambient_temperature      100(2)

_diffrn_radiation_source         'fine-focus sealed tube'



_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5922
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1279
_reflns_number_gt                997
_reflns_threshold_expression     >2σ(I)




_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?



_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0551P)²+118.6874P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1279
_refine_ls_number_parameters     87
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.1115
_refine_ls_wR_factor_gt          0.1036
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_restrained_S_all      1.143
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.6250 0.6250 0.1250 0.0366(3) Uani 1 4 d S . .
W2 W 0.8750 0.8750 0.3750 0.0371(3) Uani 1 4 d SU . .
As1 As 0.69713(7) 0.68634(4) 0.22203(5) 0.0403(3) Uani 1 1 d . . .
F1 F 0.5041(4) 0.5662(3) 0.0956(3) 0.0509(15) Uani 1 1 d . . .
C3 C 0.6562(8) 0.6521(5) 0.3013(5) 0.046(3) Uani 1 1 d . . .
C5 C 0.6557(9) 0.6513(5) 0.4122(5) 0.056(3) Uani 1 1 d . . .
H5A H 0.6770 0.6690 0.4509 0.067 Uiso 1 1 calc R . .
C4 C 0.6855(10) 0.6779(5) 0.3586(5) 0.054(3) Uani 1 1 d . . .
H4A H 0.7268 0.7145 0.3595 0.065 Uiso 1 1 calc R . .
C2 C 0.8434(8) 0.6891(5) 0.2277(6) 0.056(3) Uani 1 1 d . . .
H2A H 0.8635 0.7159 0.2629 0.085 Uiso 1 1 calc R . .
H2B H 0.8716 0.7064 0.1888 0.085 Uiso 1 1 calc R . .
H2C H 0.8699 0.6466 0.2342 0.085 Uiso 1 1 calc R . .
C1 C 0.6561(9) 0.7726(5) 0.2232(7) 0.059(3) Uani 1 1 d . . .
H1A H 0.5815 0.7752 0.2206 0.088 Uiso 1 1 calc R . .
H1B H 0.6864 0.7945 0.1874 0.088 Uiso 1 1 calc R . .
H1C H 0.6793 0.7922 0.2621 0.088 Uiso 1 1 calc R . .
F2 F 0.8464(19) 0.9386(8) 0.3177(8) 0.228(8) Uani 0.90 1 d PU . .
F3 F 0.751(3) 0.9101(14) 0.3795(15) 0.228(8) Uani 0.50 1 d P . .
F4 F 0.793(3) 0.9117(13) 0.4260(13) 0.228(8) Uani 0.60 1 d P . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 2.114(6) 14 ?
W1 F1 2.114(6) . ?
W1 F1 2.114(6) 8_554 ?
W1 F1 2.114(6) 11_554 ?
W1 As1 2.6279(10) 11_554 ?
W1 As1 2.6279(10) . ?
W1 As1 2.6279(10) 8_554 ?
W1 As1 2.6279(10) 14 ?
W2 F3 1.79(4) 3_655 ?
W2 F3 1.79(4) . ?
W2 F3 1.79(4) 4_565 ?
W2 F3 1.79(4) 2_665 ?
W2 F4 1.72(3) 3_655 ?
W2 F4 1.72(3) 4_565 ?
W2 F4 1.72(3) . ?
W2 F4 1.72(3) 2_665 ?
W2 F2 1.866(12) 3_655 ?
W2 F2 1.866(12) 2_665 ?
W2 F2 1.866(12) . ?
W2 F2 1.866(12) 4_565 ?
As1 C1 1.915(10) . ?
As1 C3 1.922(12) . ?
As1 C2 1.921(10) . ?
C3 C4 1.396(15) . ?
C3 C3 1.42(2) 14 ?
C5 C4 1.337(16) . ?
C5 C5 1.38(2) 14 ?
C5 H5A 0.9500 . ?
C4 H4A 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
F2 F4 1.56(4) 3_655 ?
F3 F4 1.14(4) . ?
F3 F3 1.51(6) 4_565 ?
F4 F2 1.56(4) 3_655 ?

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
F1 W1 F1 145.4(3) 14 . ?
F1 W1 F1 107.4(3) 14 8_554 ?
F1 W1 F1 83.0(3) . 8_554 ?
F1 W1 F1 83.0(3) 14 11_554 ?
F1 W1 F1 107.4(3) . 11_554 ?
F1 W1 F1 145.4(3) 8_554 11_554 ?
F1 W1 As1 74.92(15) 14 11_554 ?
F1 W1 As1 77.91(15) . 11_554 ?
F1 W1 As1 70.78(15) 8_554 11_554 ?
F1 W1 As1 143.01(15) 11_554 11_554 ?
F1 W1 As1 70.78(15) 14 . ?
F1 W1 As1 143.01(15) . . ?
F1 W1 As1 74.92(15) 8_554 . ?
F1 W1 As1 77.91(15) 11_554 . ?
As1 W1 As1 120.33(4) 11_554 . ?
F1 W1 As1 77.91(15) 14 8_554 ?
F1 W1 As1 74.92(15) . 8_554 ?
F1 W1 As1 143.01(15) 8_554 8_554 ?
F1 W1 As1 70.78(15) 11_554 8_554 ?
As1 W1 As1 75.74(4) 11_554 8_554 ?
As1 W1 As1 137.85(4) . 8_554 ?
F1 W1 As1 143.01(15) 14 14 ?
F1 W1 As1 70.78(15) . 14 ?
F1 W1 As1 77.91(15) 8_554 14 ?
F1 W1 As1 74.92(15) 11_554 14 ?
As1 W1 As1 137.85(4) 11_554 14 ?
As1 W1 As1 75.74(4) . 14 ?
As1 W1 As1 120.33(4) 8_554 14 ?
F3 W2 F3 130(2) 3_655 . ?
F3 W2 F3 174(2) 3_655 4_565 ?
F3 W2 F3 50(2) . 4_565 ?
F3 W2 F3 50(2) 3_655 2_665 ?
F3 W2 F3 174(2) . 2_665 ?
F3 W2 F3 130(2) 4_565 2_665 ?
F3 W2 F4 37.8(15) 3_655 3_655 ?
F3 W2 F4 114.1(14) . 3_655 ?
F3 W2 F4 136.2(16) 4_565 3_655 ?
F3 W2 F4 70.1(18) 2_665 3_655 ?
F3 W2 F4 136.2(16) 3_655 4_565 ?
F3 W2 F4 70.1(18) . 4_565 ?
F3 W2 F4 37.8(15) 4_565 4_565 ?
F3 W2 F4 114.1(14) 2_665 4_565 ?
F4 W2 F4 101.2(18) 3_655 4_565 ?
F3 W2 F4 114.1(14) 3_655 . ?
F3 W2 F4 37.8(15) . . ?
F3 W2 F4 70.1(18) 4_565 . ?
F3 W2 F4 136.2(16) 2_665 . ?
F4 W2 F4 125.8(18) 3_655 . ?
F4 W2 F4 103(3) 4_565 . ?
F3 W2 F4 70.1(18) 3_655 2_665 ?
F3 W2 F4 136.2(16) . 2_665 ?
F3 W2 F4 114.1(14) 4_565 2_665 ?
F3 W2 F4 37.8(15) 2_665 2_665 ?
F4 W2 F4 103(3) 3_655 2_665 ?
F4 W2 F4 125.8(18) 4_565 2_665 ?
F4 W2 F4 101.2(18) . 2_665 ?
F3 W2 F2 63.2(10) 3_655 3_655 ?
F3 W2 F2 80.9(15) . 3_655 ?
F3 W2 F2 121.5(15) 4_565 3_655 ?
F3 W2 F2 95.0(11) 2_665 3_655 ?
F4 W2 F2 87.8(9) 3_655 3_655 ?
F4 W2 F2 150.9(18) 4_565 3_655 ?
F4 W2 F2 51.5(13) . 3_655 ?
F4 W2 F2 77.8(9) 2_665 3_655 ?
F3 W2 F2 95.0(11) 3_655 2_665 ?
F3 W2 F2 121.5(15) . 2_665 ?
F3 W2 F2 80.9(15) 4_565 2_665 ?
F3 W2 F2 63.2(10) 2_665 2_665 ?
F4 W2 F2 77.8(9) 3_655 2_665 ?
F4 W2 F2 51.5(13) 4_565 2_665 ?
F4 W2 F2 150.9(18) . 2_665 ?
F4 W2 F2 87.8(9) 2_665 2_665 ?
F2 W2 F2 156.8(15) 3_655 2_665 ?
F3 W2 F2 80.9(15) 3_655 . ?
F3 W2 F2 63.2(10) . . ?
F3 W2 F2 95.0(11) 4_565 . ?
F3 W2 F2 121.5(15) 2_665 . ?
F4 W2 F2 51.5(13) 3_655 . ?
F4 W2 F2 77.8(9) 4_565 . ?
F4 W2 F2 87.8(9) . . ?
F4 W2 F2 150.9(18) 2_665 . ?
F2 W2 F2 86.8(13) 3_655 . ?
F2 W2 F2 97.9(13) 2_665 . ?
F3 W2 F2 121.5(15) 3_655 4_565 ?
F3 W2 F2 95.0(11) . 4_565 ?
F3 W2 F2 63.2(10) 4_565 4_565 ?
F3 W2 F2 80.9(15) 2_665 4_565 ?
F4 W2 F2 150.9(18) 3_655 4_565 ?
F4 W2 F2 87.8(9) 4_565 4_565 ?
F4 W2 F2 77.8(9) . 4_565 ?
F4 W2 F2 51.5(13) 2_665 4_565 ?
F2 W2 F2 97.9(13) 3_655 4_565 ?
F2 W2 F2 86.8(13) 2_665 4_565 ?
F2 W2 F2 156.8(15) . 4_565 ?
C1 As1 C3 105.9(5) . . ?
C1 As1 C2 104.5(5) . . ?
C3 As1 C2 103.6(5) . . ?
C1 As1 W1 112.7(4) . . ?
C3 As1 W1 114.0(3) . . ?
C2 As1 W1 115.1(4) . . ?
C4 C3 C3 118.7(7) . 14 ?
C4 C3 As1 123.2(9) . . ?
C3 C3 As1 118.1(3) 14 . ?
C4 C5 C5 121.0(7) . 14 ?
C4 C5 H5A 119.5 . . ?
C5 C5 H5A 119.5 14 . ?
C5 C4 C3 120.4(11) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
As1 C2 H2A 109.5 . . ?
As1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
As1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
As1 C1 H1A 109.5 . . ?
As1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
As1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
F4 F2 W2 59.4(12) 3_655 . ?
F4 F3 F3 98(2) . 4_565 ?
F4 F3 W2 68(3) . . ?
F3 F3 W2 65.0(12) 4_565 . ?
F3 F4 F2 122(3) . 3_655 ?
F3 F4 W2 74(3) . . ?
F2 F4 W2 69.1(15) 3_655 . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         1.076
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.180

# start Validation Reply Form
_vrf_PLAT029_2018rwz621b         
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PROBLEM: diffrn_measured_fraction_theta_full value Low .
RESPONSE: The crystal sample is extremely air-sensitve. 
The reflection intensity is quite poor especially at high angle. 
We have tried several times but can't get better quality data collected


;
_vrf_PLAT244_2018rwz621b         
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PROBLEM: Low 'Solvent' Ueq as Compared to Neighbors of
RESPONSE: The crystal sample is extremely air-sensitve. 
The reflection intensity is quite poor especially at high angle. 
We have tried several times but can't get better quality data collected
The WF8 anion is badly disordered.
;

_vrf_PLAT250_2018rwz621b         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.1 Note  
RESPONSE: The crystal sample is extremely air-sensitve. 
The reflection intensity is quite poor especially at high angle. 
We have tried several times but can't get better quality data collected
The WF8 anion is badly disordered.
;
_vrf_PLAT342_2018rwz621b         
;
PROBLEM: Low Bond Precision on  C-C Bonds 
RESPONSE: The crystal sample is extremely air-sensitve. 
The reflection intensity is quite poor especially at high angle. 
We have tried several times but can't get better quality data collected

;

# end Validation Reply Form







