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

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

data_(wscl4)2-heptane-2
_database_code_depnum_ccdc_archive 'CCDC 1949960'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton 
United Kingdom
;
_audit_update_record             
;
2019-08-28 deposited with the CCDC.	2020-01-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_(wscl4)2-heptane-2  
;
PROBLEM: Check Calcd Resid. Dens.  1.08A   From C4              5.07 eA-3
RESPONSE: Minor unresolved twinning
;
_vrf_PLAT971_(wscl4)2-heptane-2_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.82A   From W1              4.59 eA-3
RESPONSE: Residual density from tungsten - absorption correction issue.
;
_vrf_PLAT971_(wscl4)2-heptane-2_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.39A   From C2              4.56 eA-3
RESPONSE: Minor unresolved twinning
;
_vrf_PLAT971_(wscl4)2-heptane-2_4 
;
PROBLEM: Check Calcd Resid. Dens.  0.75A   From W2              4.25 eA-3
RESPONSE: Residual density from tungsten - absorption correction issue.
;
_vrf_PLAT972_(wscl4)2-heptane-2  
;
PROBLEM: Check Calcd Resid. Dens.  0.70A   From W2             -3.63 eA-3
RESPONSE: Residual density from tungsten - absorption correction issue.
;
_vrf_PLAT973_(wscl4)2-heptane-2  
;
PROBLEM: Check Calcd Positive Resid. Density on        W2       4.17 eA-3
RESPONSE: Residual density from tungsten - absorption correction issue.
;
_vrf_PLAT973_(wscl4)2-heptane-2_2 
;
PROBLEM: Check Calcd Positive Resid. Density on        W1       4.02 eA-3
RESPONSE: Residual density from tungsten - absorption correction issue.
;
# Added during the CSD deposition process: Wednesday 28 August 2019 03:01 PM
# end Validation Reply Form

_audit_creation_date             2019-08-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C5 H12 Cl8 S4 W2'
_chemical_formula_sum            'C5 H12 Cl8 S4 W2'
_chemical_formula_weight         851.69
_chemical_melting_point          ?
_chemical_oxdiff_formula         W2S4Cl8C5H12
_chemical_oxdiff_usercomment     'Red Plate'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   6.6665(2)
_cell_length_b                   11.1479(2)
_cell_length_c                   13.8916(3)
_cell_angle_alpha                101.979(2)
_cell_angle_beta                 100.011(2)
_cell_angle_gamma                95.717(2)
_cell_volume                     984.61(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9050
_cell_measurement_temperature    100.03(10)
_cell_measurement_theta_max      30.8190
_cell_measurement_theta_min      3.1940
_shelx_estimated_absorpt_T_max   0.779
_shelx_estimated_absorpt_T_min   0.559
_exptl_absorpt_coefficient_mu    13.166
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.873
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             780
_exptl_crystal_recrystallization_method 'Slow ecaporation from dcm'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15275
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         3.060
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00  24.00   1.00    1.00    --    5.00 -38.00 -60.00  108
  2  ω    -84.00   2.00   1.00    1.00    --  -12.10 -60.00 150.00   86
  3  ω   -101.00  14.00   1.00    1.00    --  -12.10 -60.00 -90.00  115
  4  ω    -88.00 -25.00   1.00    1.00    --  -12.10 -57.00  90.00   63
  5  ω    -12.00  14.00   1.00    1.00    --  -12.10 -57.00  90.00   26
  6  ω    -88.00 -17.00   1.00    1.00    --  -12.10 -38.00   0.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0202453000
_diffrn_orient_matrix_UB_12      0.0619408000
_diffrn_orient_matrix_UB_13      0.0131158000
_diffrn_orient_matrix_UB_21      -0.1067707000
_diffrn_orient_matrix_UB_22      -0.0215617000
_diffrn_orient_matrix_UB_23      -0.0086076000
_diffrn_orient_matrix_UB_31      0.0099839000
_diffrn_orient_matrix_UB_32      -0.0038273000
_diffrn_orient_matrix_UB_33      0.0509082000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4231
_reflns_number_total             5051
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         4.948
_refine_diff_density_min         -3.648
_refine_diff_density_rms         0.356
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         5051
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0495
_refine_ls_restrained_S_all      1.177
_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)+(0.0578P)²+8.7607P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1279
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_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
W2 W 0.81055(5) 0.81496(3) 0.08377(2) 0.01963(11) Uani 1 1 d . . . . .
W1 W 0.22843(5) 0.21292(3) 0.43550(2) 0.01962(11) Uani 1 1 d . . . . .
Cl1 Cl 0.3376(3) 0.02312(18) 0.39649(16) 0.0250(4) Uani 1 1 d . . . . .
Cl2 Cl 0.0425(3) 0.18249(19) 0.27395(15) 0.0240(4) Uani 1 1 d . . . . .
Cl3 Cl 0.2075(3) 0.42341(19) 0.45338(15) 0.0249(4) Uani 1 1 d . . . . .
Cl4 Cl 0.4990(3) 0.26890(19) 0.57320(15) 0.0246(4) Uani 1 1 d . . . . .
Cl8 Cl 0.7357(4) 0.86327(19) 0.24253(15) 0.0262(4) Uani 1 1 d . . . . .
S2 S 0.5582(3) 0.26375(18) 0.34127(15) 0.0197(4) Uani 1 1 d . . . . .
Cl6 Cl 0.9076(4) 0.7082(2) -0.05933(15) 0.0271(4) Uani 1 1 d . . . . .
Cl5 Cl 0.4854(3) 0.7006(2) 0.02378(17) 0.0279(4) Uani 1 1 d . . . . .
Cl7 Cl 1.1537(3) 0.86945(19) 0.15352(17) 0.0278(4) Uani 1 1 d . . . . .
S3 S 0.8741(3) 0.58885(19) 0.13485(16) 0.0227(4) Uani 1 1 d . . . . .
S4 S 0.7524(4) 0.9797(2) 0.03881(17) 0.0276(5) Uani 1 1 d . . . . .
S1 S -0.0131(4) 0.1635(2) 0.50518(19) 0.0320(5) Uani 1 1 d . . . . .
C1 C 0.5104(14) 0.1506(8) 0.2226(7) 0.0243(18) Uani 1 1 d . . . . .
H1A H 0.513912 0.069188 0.234977 0.036 Uiso 1 1 calc GR . . . .
H1B H 0.614256 0.167909 0.185522 0.036 Uiso 1 1 calc GR . . . .
H1C H 0.377549 0.154837 0.184566 0.036 Uiso 1 1 calc GR . . . .
C4 C 0.6833(14) 0.5532(8) 0.2069(7) 0.0236(17) Uani 1 1 d . . . . .
H4A H 0.689636 0.623395 0.262456 0.028 Uiso 1 1 calc R . . . .
H4B H 0.547464 0.540606 0.164529 0.028 Uiso 1 1 calc R . . . .
C3 C 0.7138(14) 0.4382(7) 0.2481(6) 0.0213(16) Uani 1 1 d . . . . .
H3A H 0.726463 0.370160 0.194278 0.026 Uiso 1 1 calc R . . . .
H3B H 0.839442 0.454646 0.298657 0.026 Uiso 1 1 calc R . . . .
C2 C 0.5313(14) 0.4029(7) 0.2941(6) 0.0214(17) Uani 1 1 d . . . . .
H2A H 0.405519 0.389134 0.243779 0.026 Uiso 1 1 calc R . . . .
H2B H 0.520929 0.470598 0.348714 0.026 Uiso 1 1 calc R . . . .
C5 C 1.1060(15) 0.6165(10) 0.2303(8) 0.036(2) Uani 1 1 d . . . . .
H5A H 1.222443 0.637712 0.201929 0.054 Uiso 1 1 calc GR . . . .
H5B H 1.122124 0.543118 0.255039 0.054 Uiso 1 1 calc GR . . . .
H5C H 1.096642 0.683523 0.284535 0.054 Uiso 1 1 calc GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W2 0.0224(2) 0.01807(17) 0.01798(18) 0.00332(13) 0.00464(13) 0.00165(13)
W1 0.0196(2) 0.02008(18) 0.01943(18) 0.00539(13) 0.00424(13) 0.00152(13)
Cl1 0.0302(11) 0.0192(9) 0.0251(10) 0.0064(8) 0.0029(8) 0.0022(8)
Cl2 0.0206(10) 0.0283(10) 0.0204(9) 0.0039(8) 0.0005(7) 0.0010(8)
Cl3 0.0276(11) 0.0231(9) 0.0246(10) 0.0035(8) 0.0070(8) 0.0075(8)
Cl4 0.0258(11) 0.0267(10) 0.0192(9) 0.0028(8) 0.0015(8) 0.0035(8)
Cl8 0.0370(12) 0.0222(9) 0.0213(9) 0.0035(8) 0.0116(9) 0.0056(8)
S2 0.0204(10) 0.0182(9) 0.0201(9) 0.0043(7) 0.0037(8) 0.0023(7)
Cl6 0.0318(12) 0.0291(10) 0.0207(9) 0.0045(8) 0.0072(8) 0.0047(9)
Cl5 0.0224(11) 0.0282(10) 0.0307(11) 0.0059(9) 0.0018(8) 0.0009(8)
Cl7 0.0261(11) 0.0227(10) 0.0310(11) 0.0036(8) 0.0027(9) -0.0033(8)
S3 0.0246(11) 0.0191(9) 0.0251(10) 0.0055(8) 0.0069(8) 0.0024(8)
S4 0.0351(13) 0.0227(10) 0.0275(11) 0.0086(9) 0.0090(9) 0.0056(9)
S1 0.0267(12) 0.0385(13) 0.0340(12) 0.0127(10) 0.0119(10) 0.0005(10)
C1 0.023(4) 0.018(4) 0.028(4) -0.003(3) 0.008(4) 0.000(3)
C4 0.024(4) 0.019(4) 0.030(4) 0.003(3) 0.015(4) 0.004(3)
C3 0.026(4) 0.016(4) 0.025(4) 0.006(3) 0.008(3) 0.007(3)
C2 0.030(5) 0.017(4) 0.020(4) 0.006(3) 0.010(3) 0.005(3)
C5 0.021(5) 0.046(6) 0.045(6) 0.024(5) 0.003(4) 0.004(4)

_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
W2 Cl8 2.312(2) . ?
W2 Cl6 2.325(2) . ?
W2 Cl5 2.323(2) . ?
W2 Cl7 2.291(2) . ?
W2 S3 2.808(2) . ?
W2 S4 2.109(2) . ?
W1 Cl1 2.295(2) . ?
W1 Cl2 2.307(2) . ?
W1 Cl3 2.329(2) . ?
W1 Cl4 2.320(2) . ?
W1 S2 2.816(2) . ?
W1 S1 2.102(2) . ?
S2 C1 1.812(8) . ?
S2 C2 1.818(8) . ?
S3 C4 1.812(8) . ?
S3 C5 1.807(10) . ?
C4 C3 1.525(11) . ?
C3 C2 1.525(11) . ?

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
Cl8 W2 Cl6 161.42(8) . . ?
Cl8 W2 Cl5 89.52(8) . . ?
Cl8 W2 S3 82.73(7) . . ?
Cl6 W2 S3 78.71(7) . . ?
Cl5 W2 Cl6 87.77(8) . . ?
Cl5 W2 S3 78.55(7) . . ?
Cl7 W2 Cl8 89.46(8) . . ?
Cl7 W2 Cl6 87.48(8) . . ?
Cl7 W2 Cl5 161.92(8) . . ?
Cl7 W2 S3 83.42(7) . . ?
S4 W2 Cl8 98.96(8) . . ?
S4 W2 Cl6 99.62(8) . . ?
S4 W2 Cl5 99.08(9) . . ?
S4 W2 Cl7 98.91(9) . . ?
S4 W2 S3 177.11(8) . . ?
Cl1 W1 Cl2 90.66(8) . . ?
Cl1 W1 Cl3 161.63(8) . . ?
Cl1 W1 Cl4 88.62(8) . . ?
Cl1 W1 S2 77.55(7) . . ?
Cl2 W1 Cl3 87.71(8) . . ?
Cl2 W1 Cl4 161.03(8) . . ?
Cl2 W1 S2 81.92(7) . . ?
Cl3 W1 S2 84.11(7) . . ?
Cl4 W1 Cl3 87.04(8) . . ?
Cl4 W1 S2 79.41(7) . . ?
S1 W1 Cl1 98.82(9) . . ?
S1 W1 Cl2 98.54(9) . . ?
S1 W1 Cl3 99.52(9) . . ?
S1 W1 Cl4 100.30(9) . . ?
S1 W1 S2 176.35(8) . . ?
C1 S2 W1 106.4(3) . . ?
C1 S2 C2 99.1(4) . . ?
C2 S2 W1 109.6(3) . . ?
C4 S3 W2 107.6(3) . . ?
C5 S3 W2 107.8(3) . . ?
C5 S3 C4 100.4(5) . . ?
C3 C4 S3 112.8(6) . . ?
C2 C3 C4 109.9(7) . . ?
C3 C2 S2 111.4(6) . . ?

_shelx_res_file                  
;
TITL (wscl4)2-heptane-2_a.res in P-1
    (wscl4)2-heptane-2.res
    created by SHELXL-2018/3 at 11:18:08 on 20-Aug-2019
REM Old TITL (WSCl4)2-Heptane-2 in P-1 #2
REM SHELXT solution in P-1: R1 0.055, Rweak 0.002, Alpha 0.048
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C5 S2 Cl10 W2
CELL 0.71073 6.6665 11.1479 13.8916 101.979 100.011 95.717
ZERR 2 0.0002 0.0002 0.0003 0.002 0.002 0.002
LATT 1
SFAC C H Cl S W
UNIT 10 24 16 8 4

L.S. 10
PLAN  20
SIZE 0.05 0.02 0.03
BOND
list 4
fmap 2
acta
OMIT -5 4 2
REM <olex2.extras>
REM <HklSrc "%.\\(WSCl4)2-Heptane-2.hkl">
REM </olex2.extras>

WGHT    0.057800    8.760700
FVAR       0.29600
W2    5    0.810553    0.814955    0.083775    11.00000    0.02242    0.01807 =
         0.01798    0.00332    0.00464    0.00165
W1    5    0.228429    0.212916    0.435505    11.00000    0.01960    0.02008 =
         0.01943    0.00539    0.00424    0.00152
CL1   3    0.337566    0.023117    0.396489    11.00000    0.03016    0.01917 =
         0.02513    0.00637    0.00294    0.00223
CL2   3    0.042505    0.182490    0.273954    11.00000    0.02056    0.02832 =
         0.02037    0.00389    0.00049    0.00097
CL3   3    0.207453    0.423408    0.453376    11.00000    0.02761    0.02313 =
         0.02458    0.00345    0.00699    0.00748
CL4   3    0.499004    0.268896    0.573205    11.00000    0.02582    0.02674 =
         0.01915    0.00285    0.00154    0.00353
CL8   3    0.735678    0.863269    0.242528    11.00000    0.03704    0.02224 =
         0.02125    0.00352    0.01161    0.00558
S2    4    0.558201    0.263751    0.341266    11.00000    0.02040    0.01817 =
         0.02011    0.00426    0.00366    0.00232
CL6   3    0.907608    0.708180   -0.059329    11.00000    0.03176    0.02908 =
         0.02067    0.00449    0.00720    0.00469
CL5   3    0.485447    0.700553    0.023775    11.00000    0.02237    0.02824 =
         0.03067    0.00585    0.00177    0.00092
CL7   3    1.153655    0.869445    0.153517    11.00000    0.02614    0.02273 =
         0.03096    0.00359    0.00267   -0.00329
S3    4    0.874083    0.588854    0.134855    11.00000    0.02462    0.01912 =
         0.02515    0.00554    0.00689    0.00235
S4    4    0.752405    0.979685    0.038810    11.00000    0.03508    0.02270 =
         0.02750    0.00862    0.00896    0.00557
S1    4   -0.013093    0.163459    0.505183    11.00000    0.02671    0.03848 =
         0.03403    0.01267    0.01185    0.00054
C1    1    0.510357    0.150626    0.222641    11.00000    0.02326    0.01843 =
         0.02793   -0.00314    0.00806    0.00018
AFIX 137
H1A   2    0.513912    0.069188    0.234977    11.00000   -1.50000
H1B   2    0.614256    0.167909    0.185522    11.00000   -1.50000
H1C   2    0.377549    0.154837    0.184566    11.00000   -1.50000
AFIX   0
C4    1    0.683274    0.553217    0.206896    11.00000    0.02399    0.01943 =
         0.02996    0.00324    0.01504    0.00388
AFIX  23
H4A   2    0.689636    0.623395    0.262456    11.00000   -1.20000
H4B   2    0.547464    0.540606    0.164529    11.00000   -1.20000
AFIX   0
C3    1    0.713757    0.438249    0.248059    11.00000    0.02602    0.01575 =
         0.02453    0.00555    0.00832    0.00665
AFIX  23
H3A   2    0.726463    0.370160    0.194278    11.00000   -1.20000
H3B   2    0.839442    0.454646    0.298657    11.00000   -1.20000
AFIX   0
C2    1    0.531252    0.402888    0.294098    11.00000    0.03028    0.01696 =
         0.01995    0.00627    0.00994    0.00500
AFIX  23
H2A   2    0.405519    0.389134    0.243779    11.00000   -1.20000
H2B   2    0.520929    0.470598    0.348714    11.00000   -1.20000
AFIX   0
C5    1    1.105999    0.616547    0.230270    11.00000    0.02099    0.04600 =
         0.04504    0.02402    0.00258    0.00445
AFIX 137
H5A   2    1.222443    0.637712    0.201929    11.00000   -1.50000
H5B   2    1.122124    0.543118    0.255039    11.00000   -1.50000
H5C   2    1.096642    0.683523    0.284535    11.00000   -1.50000
AFIX   0
HKLF 4




REM  (wscl4)2-heptane-2_a.res in P-1
REM wR2 = 0.1279, GooF = S = 1.177, Restrained GooF = 1.177 for all data
REM R1 = 0.0495 for 4231 Fo > 4sig(Fo) and 0.0580 for all 5051 data
REM 174 parameters refined using 0 restraints

END

WGHT      0.0580      8.6939

REM Highest difference peak  4.948,  deepest hole -3.648,  1-sigma level  0.356
Q1    1   0.6008  0.5796  0.2642  11.00000  0.05    4.95
Q2    1   0.1542  0.1588  0.3990  11.00000  0.05    4.94
Q3    1   0.7307  0.7534  0.0423  11.00000  0.05    4.58
Q4    1   0.3561  0.3925  0.2148  11.00000  0.05    4.39
Q5    1   0.5597  0.8173  0.2196  11.00000  0.05    1.84
Q6    1   0.7817  0.9194  0.0992  11.00000  0.05    1.77
Q7    1   0.0419  0.2623  0.5365  11.00000  0.05    1.69
Q8    1   0.3737  0.1811  0.2000  11.00000  0.05    1.61
Q9    1   0.8519  1.1377  0.0149  11.00000  0.05    1.60
Q10   1   0.2907  0.1154  0.4181  11.00000  0.05    1.60
Q11   1   0.8756  0.7226  0.0456  11.00000  0.05    1.56
Q12   1   1.0816  0.8791  0.2188  11.00000  0.05    1.55
Q13   1   0.2009  0.3161  0.4596  11.00000  0.05    1.51
Q14   1   0.6363  0.9489  0.0809  11.00000  0.05    1.49
Q15   1   0.7087  1.0026  0.1262  11.00000  0.05    1.48
Q16   1   0.3168  0.1071  0.2985  11.00000  0.05    1.41
Q17   1   0.4631  0.6951 -0.0928  11.00000  0.05    1.40
Q18   1   0.4026  0.7072  0.1396  11.00000  0.05    1.39
Q19   1  -0.0960  0.0886  0.3762  11.00000  0.05    1.37
Q20   1   0.4058  0.2161  0.4856  11.00000  0.05    1.36
;
_shelx_res_checksum              95827
_olex2_exptl_crystal_mounting_method Mounted
_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 6.112
_oxdiff_exptl_absorpt_empirical_full_min 0.471
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_wocl3(mes(ch2)2sme)
_database_code_depnum_ccdc_archive 'CCDC 1949962'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton 
United Kingdom
;
_audit_update_record             
;
2019-08-28 deposited with the CCDC.	2020-01-28 downloaded from the CCDC.
;
_audit_creation_date             2019-08-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H10 Cl3 O S2 W'
_chemical_formula_sum            'C4 H10 Cl3 O S2 W'
_chemical_formula_weight         428.44
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         S2OWCl4C4H10
_chemical_oxdiff_usercomment     'Green Block'
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'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   6.7317(3)
_cell_length_b                   6.9581(3)
_cell_length_c                   7.1904(3)
_cell_angle_alpha                108.981(4)
_cell_angle_beta                 98.845(4)
_cell_angle_gamma                114.330(4)
_cell_volume                     273.54(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4433
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.2750
_cell_measurement_theta_min      3.5910
_shelx_estimated_absorpt_T_max   0.205
_shelx_estimated_absorpt_T_min   0.205
_exptl_absorpt_coefficient_mu    11.619
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.601
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             199
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5239
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.669
_diffrn_reflns_theta_min         3.179
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -108.00  16.00   1.00    1.00    --  -19.10 -57.00 -60.00  124
  2  ω   -108.00  16.00   1.00    1.00    --  -19.10 -57.00  30.00  124
  3  ω   -108.00  16.00   1.00    1.00    --  -19.10 -57.00-120.00  124
  4  ω   -108.00  16.00   1.00    1.00    --  -19.10 -57.00 150.00  124
  5  ω    -55.00  70.00   1.00    1.00    --  -19.10  60.00  60.00  125
  6  ω    -55.00  16.00   1.00    1.00    --  -19.10  60.00 150.00   71
  7  ω    -55.00  70.00   1.00    1.00    --  -19.10  60.00-120.00  125
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0560061000
_diffrn_orient_matrix_UB_12      -0.1219409000
_diffrn_orient_matrix_UB_13      -0.0287687000
_diffrn_orient_matrix_UB_21      0.0631138000
_diffrn_orient_matrix_UB_22      0.0213866000
_diffrn_orient_matrix_UB_23      0.0998944000
_diffrn_orient_matrix_UB_31      -0.0890535000
_diffrn_orient_matrix_UB_32      0.0073677000
_diffrn_orient_matrix_UB_33      0.0379704000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.790
_reflns_number_gt                2854
_reflns_number_total             2880
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         3.758
_refine_diff_density_min         -2.629
_refine_diff_density_rms         0.290
_refine_ls_abs_structure_details 
;
 Flack x determined using 1267 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2880
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0452
_refine_ls_restrained_S_all      1.041
_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)+(0.0699P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1045
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.19193(2) 0.08236(2) 0.61482(2) 0.01412(15) Uani 1 1 d . . . . .
Cl1 Cl 0.1009(8) -0.2308(7) 0.2975(6) 0.0189(7) Uani 1 1 d . . . . .
Cl2 Cl 0.3757(7) -0.0486(7) 0.8055(6) 0.0188(7) Uani 1 1 d . . . . .
S1 S 0.5970(6) 0.2345(6) 0.5237(6) 0.0148(6) Uani 1 1 d . . . . .
S2 S 0.1316(7) 0.3090(7) 0.4220(6) 0.0152(6) Uani 1 1 d . . . . .
Cl3 Cl 0.3789(8) 0.4529(7) 0.9020(6) 0.0183(7) Uani 1 1 d . . . . .
O1 O -0.081(2) -0.016(2) 0.637(2) 0.023(2) Uani 1 1 d . . . . .
C2 C 0.550(3) 0.372(3) 0.359(3) 0.019(3) Uani 1 1 d . . . . .
H2A H 0.698505 0.483465 0.363099 0.023 Uiso 1 1 calc R . . . .
H2B H 0.465619 0.253663 0.216426 0.023 Uiso 1 1 calc R . . . .
C4 C -0.021(3) 0.122(3) 0.147(3) 0.021(3) Uani 1 1 d . . . . .
H4A H 0.063367 0.049108 0.090999 0.032 Uiso 1 1 calc GR . . . .
H4B H -0.035642 0.214064 0.076823 0.032 Uiso 1 1 calc GR . . . .
H4C H -0.172085 0.004386 0.128068 0.032 Uiso 1 1 calc GR . . . .
C3 C 0.417(3) 0.497(3) 0.425(2) 0.017(3) Uani 1 1 d . . . . .
H3A H 0.400208 0.568357 0.331901 0.021 Uiso 1 1 calc R . . . .
H3B H 0.506187 0.621722 0.564369 0.021 Uiso 1 1 calc R . . . .
C1 C 0.824(3) 0.481(3) 0.752(2) 0.021(3) Uani 1 1 d . . . . .
H1A H 0.780717 0.599895 0.797459 0.032 Uiso 1 1 calc GR . . . .
H1B H 0.963446 0.542591 0.719447 0.032 Uiso 1 1 calc GR . . . .
H1C H 0.848443 0.433934 0.860498 0.032 Uiso 1 1 calc GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.0174(2) 0.0129(2) 0.0137(2) 0.00632(16) 0.00608(16) 0.00804(17)
Cl1 0.022(2) 0.0140(16) 0.0177(17) 0.0043(14) 0.0038(15) 0.0089(15)
Cl2 0.0235(19) 0.0169(16) 0.0191(17) 0.0085(14) 0.0064(14) 0.0123(15)
S1 0.0143(16) 0.0150(15) 0.0160(16) 0.0055(13) 0.0060(13) 0.0088(13)
S2 0.0171(18) 0.0164(16) 0.0164(17) 0.0087(14) 0.0064(14) 0.0105(15)
Cl3 0.025(2) 0.0159(16) 0.0172(17) 0.0061(14) 0.0094(15) 0.0127(15)
O1 0.023(6) 0.018(5) 0.029(6) 0.012(5) 0.008(5) 0.010(4)
C2 0.021(7) 0.020(7) 0.026(8) 0.014(6) 0.014(6) 0.013(6)
C4 0.023(8) 0.022(7) 0.017(7) 0.009(6) 0.002(6) 0.010(6)
C3 0.017(7) 0.017(6) 0.020(7) 0.010(6) 0.008(6) 0.010(6)
C1 0.014(7) 0.020(7) 0.015(7) 0.001(6) 0.000(5) 0.004(6)

_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 Cl1 2.359(4) . ?
W1 Cl2 2.337(3) . ?
W1 S1 2.758(3) . ?
W1 S2 2.520(3) . ?
W1 Cl3 2.358(4) . ?
W1 O1 1.729(12) . ?
S1 C2 1.813(16) . ?
S1 C1 1.790(16) . ?
S2 C4 1.803(17) . ?
S2 C3 1.818(15) . ?
C2 C3 1.51(2) . ?

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
Cl1 W1 S1 77.13(14) . . ?
Cl1 W1 S2 90.72(13) . . ?
Cl2 W1 Cl1 91.68(13) . . ?
Cl2 W1 S1 82.17(13) . . ?
Cl2 W1 S2 160.80(12) . . ?
Cl2 W1 Cl3 89.99(13) . . ?
S2 W1 S1 79.81(12) . . ?
Cl3 W1 Cl1 162.56(11) . . ?
Cl3 W1 S1 85.91(13) . . ?
Cl3 W1 S2 82.20(13) . . ?
O1 W1 Cl1 98.4(4) . . ?
O1 W1 Cl2 105.1(4) . . ?
O1 W1 S1 171.7(4) . . ?
O1 W1 S2 93.4(4) . . ?
O1 W1 Cl3 98.0(4) . . ?
C2 S1 W1 102.2(5) . . ?
C1 S1 W1 108.6(5) . . ?
C1 S1 C2 101.5(8) . . ?
C4 S2 W1 111.2(5) . . ?
C4 S2 C3 102.2(8) . . ?
C3 S2 W1 105.4(5) . . ?
C3 C2 S1 113.1(11) . . ?
C2 C3 S2 114.0(10) . . ?

_shelx_res_file                  
;
TITL DS EX90 WOCl4(Mte)-2 in P1 #1
    wocl3(mes(ch2)2sme).res
    created by SHELXL-2018/3 at 16:04:43 on 19-Aug-2019
REM reset to P1 #1
CELL 0.71073 6.731747 6.958135 7.190426 108.9811 98.8453 114.3301
ZERR 1 0.000283 0.000296 0.000345 0.0041 0.0038 0.0042
LATT -1
SFAC C H Cl O S W
UNIT 4 10 3 1 2 1

L.S. 4
PLAN  20
SIZE 0.2 0.2 0.2
fmap 2
acta
OMIT -2 4 3
OMIT -1 -2 -7
REM <olex2.extras>
REM <HklSrc "%.\\WOCl3(MeS(CH2)2SMe).hkl">
REM </olex2.extras>

WGHT    0.069900
FVAR       7.19046
W1    6    0.191930    0.082360    0.614820    11.00000    0.01736    0.01288 =
         0.01367    0.00632    0.00608    0.00804
CL1   3    0.100926   -0.230813    0.297467    11.00000    0.02178    0.01397 =
         0.01767    0.00434    0.00380    0.00892
CL2   3    0.375719   -0.048573    0.805487    11.00000    0.02346    0.01691 =
         0.01906    0.00855    0.00637    0.01227
S1    5    0.597043    0.234520    0.523700    11.00000    0.01432    0.01502 =
         0.01602    0.00546    0.00599    0.00880
S2    5    0.131572    0.308970    0.421959    11.00000    0.01709    0.01637 =
         0.01639    0.00873    0.00640    0.01049
CL3   3    0.378948    0.452919    0.901968    11.00000    0.02477    0.01591 =
         0.01725    0.00606    0.00940    0.01272
O1    4   -0.080578   -0.016360    0.637372    11.00000    0.02339    0.01835 =
         0.02861    0.01191    0.00794    0.01010
C2    1    0.549894    0.372103    0.359270    11.00000    0.02098    0.02029 =
         0.02631    0.01441    0.01442    0.01340
AFIX  23
H2A   2    0.698505    0.483465    0.363099    11.00000   -1.20000
H2B   2    0.465619    0.253663    0.216426    11.00000   -1.20000
AFIX   0
C4    1   -0.021029    0.122322    0.147377    11.00000    0.02296    0.02214 =
         0.01699    0.00926    0.00234    0.01024
AFIX 137
H4A   2    0.063367    0.049108    0.090999    11.00000   -1.50000
H4B   2   -0.035642    0.214064    0.076823    11.00000   -1.50000
H4C   2   -0.172085    0.004386    0.128068    11.00000   -1.50000
AFIX   0
C3    1    0.416916    0.497098    0.424620    11.00000    0.01748    0.01740 =
         0.02023    0.00958    0.00789    0.00955
AFIX  23
H3A   2    0.400208    0.568357    0.331901    11.00000   -1.20000
H3B   2    0.506187    0.621722    0.564369    11.00000   -1.20000
AFIX   0
C1    1    0.823692    0.481356    0.751714    11.00000    0.01417    0.02050 =
         0.01512    0.00086   -0.00047    0.00414
AFIX 137
H1A   2    0.780717    0.599895    0.797459    11.00000   -1.50000
H1B   2    0.963446    0.542591    0.719447    11.00000   -1.50000
H1C   2    0.848443    0.433934    0.860498    11.00000   -1.50000
AFIX   0
HKLF 4




REM  DS EX90 WOCl4(Mte)-2 in P1 #1
REM wR2 = 0.1045, GooF = S = 1.041, Restrained GooF = 1.041 for all data
REM R1 = 0.0452 for 2854 Fo > 4sig(Fo) and 0.0460 for all 2880 data
REM 102 parameters refined using 3 restraints

END

WGHT      0.0699      0.0000

REM Highest difference peak  3.758,  deepest hole -2.629,  1-sigma level  0.290
Q1    1   0.2930  0.1818  0.7411  11.00000  0.05    3.76
Q2    1   0.0858 -0.0157  0.4909  11.00000  0.05    3.73
Q3    1   0.2412  0.1933  0.6020  11.00000  0.05    2.90
Q4    1   0.1364 -0.0418  0.6295  11.00000  0.05    2.89
Q5    1   0.1912  0.2262  0.7387  11.00000  0.05    2.10
Q6    1   0.3000  0.0797  0.6030  11.00000  0.05    2.01
Q7    1   0.1902 -0.0659  0.4939  11.00000  0.05    1.83
Q8    1   0.0765  0.0811  0.6337  11.00000  0.05    1.77
Q9    1   0.1385  0.0297  0.7345  11.00000  0.05    1.64
Q10   1   0.2463  0.0647  0.4866  11.00000  0.05    1.63
Q11   1   0.3823  0.3400  0.7989  11.00000  0.05    1.27
Q12   1   0.2312 -0.0969  0.4156  11.00000  0.05    1.18
Q13   1   0.0164 -0.1834  0.4358  11.00000  0.05    1.15
Q14   1   0.1388  0.2607  0.8253  11.00000  0.05    1.05
Q15   1   0.3262  0.0713  0.7762  11.00000  0.05    1.01
Q16   1  -0.0242 -0.0811  0.6818  11.00000  0.05    1.00
Q17   1   0.3954  0.2402  0.5432  11.00000  0.05    0.96
Q18   1   0.4221  0.0882  0.7943  11.00000  0.05    0.94
Q19   1   0.2219  0.3669  0.8020  11.00000  0.05    0.93
Q20   1   0.2053  0.4478  0.4204  11.00000  0.05    0.93
;
_shelx_res_checksum              86325
_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 5.417
_oxdiff_exptl_absorpt_empirical_full_min 0.145
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_(wscl4)2phs(ch2)2sph)
_database_code_depnum_ccdc_archive 'CCDC 1949961'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton 
United Kingdom
;
_audit_update_record             
;
2019-08-28 deposited with the CCDC.	2020-01-28 downloaded from the CCDC.
;
_audit_creation_date             2019-07-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H14 Cl8 S4 W2'
_chemical_formula_sum            'C14 H14 Cl8 S4 W2'
_chemical_formula_weight         961.79
_chemical_melting_point          ?
_chemical_oxdiff_formula         W2S4Cl8C8H14
_chemical_oxdiff_usercomment     'Red Plate'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.5790(2)
_cell_length_b                   13.9272(3)
_cell_length_c                   17.2182(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.368(2)
_cell_angle_gamma                90
_cell_volume                     2521.21(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7424
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.1850
_cell_measurement_theta_min      3.4920
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.300
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.534
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1784
_exptl_crystal_preparation       'Vapour Diffusion from DCM and Hexane'
_exptl_crystal_recrystallization_method 'Vapour Difrfusion from DCM and Hexane'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17788
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.262
_diffrn_reflns_theta_min         2.925
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -101.00  18.00   1.00   12.04    --  -12.10 -60.00 -60.00  119
  2  ω    -36.00  60.00   1.00   12.04    --  -12.10  38.00 -90.00   96
  3  ω   -100.00   7.00   1.00   12.04    --  -12.10 -60.00 120.00  107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0113027000
_diffrn_orient_matrix_UB_12      -0.0097979000
_diffrn_orient_matrix_UB_13      0.0405867000
_diffrn_orient_matrix_UB_21      0.0305686000
_diffrn_orient_matrix_UB_22      0.0451204000
_diffrn_orient_matrix_UB_23      0.0061471000
_diffrn_orient_matrix_UB_31      -0.0590741000
_diffrn_orient_matrix_UB_32      0.0214960000
_diffrn_orient_matrix_UB_33      0.0057143000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5333
_reflns_number_total             6811
_reflns_odcompleteness_completeness 94.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.153
_refine_diff_density_min         -2.693
_refine_diff_density_rms         0.308
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         6811
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0420
_refine_ls_restrained_S_all      0.968
_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)+(0.0191P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0816
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C1(H1), C4(H4), C14(H14), C3(H3), C10(H10), C13(H13), C11(H11),
 C2(H2), C12(H12)
;
_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
W2 W 0.74439(2) 0.72548(2) 0.47774(2) 0.01153(7) Uani 1 1 d . . . . .
W1 W -0.01076(2) 0.49484(2) 0.25901(2) 0.01132(7) Uani 1 1 d . . . . .
Cl6 Cl 0.73154(15) 0.71606(14) 0.34269(9) 0.0187(4) Uani 1 1 d . . . . .
Cl2 Cl 0.05990(15) 0.49411(13) 0.13834(9) 0.0177(4) Uani 1 1 d . . . . .
Cl7 Cl 0.71557(15) 0.88978(13) 0.46492(9) 0.0178(4) Uani 1 1 d . . . . .
Cl4 Cl -0.00667(15) 0.50357(13) 0.39390(9) 0.0184(4) Uani 1 1 d . . . . .
Cl8 Cl 0.67927(15) 0.73878(13) 0.59971(9) 0.0181(4) Uani 1 1 d . . . . .
Cl5 Cl 0.70344(15) 0.56236(12) 0.48074(10) 0.0175(3) Uani 1 1 d . . . . .
Cl1 Cl 0.04041(15) 0.33369(13) 0.27274(9) 0.0181(4) Uani 1 1 d . . . . .
S3 S 0.47793(14) 0.73872(13) 0.42685(9) 0.0121(3) Uani 1 1 d . . . . .
S2 S 0.25435(15) 0.50037(12) 0.31401(9) 0.0122(3) Uani 1 1 d . . . . .
Cl3 Cl 0.01084(14) 0.65945(13) 0.25794(9) 0.0177(4) Uani 1 1 d . . . . .
S4 S 0.94293(16) 0.71737(14) 0.50507(11) 0.0204(4) Uani 1 1 d . . . . .
S1 S -0.20780(16) 0.48411(15) 0.22747(10) 0.0213(4) Uani 1 1 d . . . . .
C5 C 0.3741(6) 0.5661(5) 0.1873(4) 0.0171(15) Uani 1 1 d . . . . .
H5 H 0.346112 0.627522 0.197818 0.020 Uiso 1 1 calc R . . . .
C8 C 0.4313(6) 0.6210(5) 0.3879(4) 0.0150(14) Uani 1 1 d . . . . .
H8A H 0.485601 0.603397 0.348278 0.018 Uiso 1 1 calc R . . . .
H8B H 0.443438 0.573823 0.429462 0.018 Uiso 1 1 calc R . . . .
C7 C 0.2932(6) 0.6192(5) 0.3522(4) 0.0142(14) Uani 1 1 d . . . . .
H7A H 0.280218 0.666178 0.310469 0.017 Uiso 1 1 calc R . . . .
H7B H 0.238087 0.635606 0.391639 0.017 Uiso 1 1 calc R . . . .
C1 C 0.3891(7) 0.3980(6) 0.2190(4) 0.0250(17) Uani 1 1 d . . . . .
H1 H 0.372768 0.346907 0.251211 0.030 Uiso 1 1 calc R . . . .
C4 C 0.4421(6) 0.5507(5) 0.1246(4) 0.0179(16) Uani 1 1 d . . . . .
H4 H 0.461397 0.602125 0.093597 0.021 Uiso 1 1 calc R . . . .
C14 C 0.3772(6) 0.6800(5) 0.5619(4) 0.0193(16) Uani 1 1 d . . . . .
H14 H 0.424755 0.623953 0.560413 0.023 Uiso 1 1 calc R . . . .
C6 C 0.3475(6) 0.4891(5) 0.2349(3) 0.0115(14) Uani 1 1 d . . . . .
C3 C 0.4815(6) 0.4598(5) 0.1078(4) 0.0175(15) Uani 1 1 d . . . . .
H3 H 0.525835 0.449748 0.064756 0.021 Uiso 1 1 calc R . . . .
C10 C 0.3148(6) 0.8350(5) 0.5093(4) 0.0167(15) Uani 1 1 d . . . . .
H10 H 0.319387 0.882238 0.471546 0.020 Uiso 1 1 calc R . . . .
C9 C 0.3816(6) 0.7501(5) 0.5046(4) 0.0135(14) Uani 1 1 d . . . . .
C13 C 0.3009(7) 0.6949(6) 0.6210(4) 0.0257(18) Uani 1 1 d . . . . .
H13 H 0.295570 0.647756 0.658680 0.031 Uiso 1 1 calc R . . . .
C11 C 0.2401(6) 0.8501(6) 0.5706(4) 0.0220(16) Uani 1 1 d . . . . .
H11 H 0.196530 0.907599 0.574319 0.026 Uiso 1 1 calc R . . . .
C2 C 0.4554(7) 0.3828(6) 0.1548(4) 0.0254(17) Uani 1 1 d . . . . .
H2 H 0.482270 0.321308 0.143406 0.031 Uiso 1 1 calc R . . . .
C12 C 0.2322(6) 0.7794(6) 0.6248(4) 0.0230(17) Uani 1 1 d . . . . .
H12 H 0.180485 0.787883 0.664508 0.028 Uiso 1 1 calc R . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W2 0.00967(12) 0.01182(15) 0.01285(14) 0.00054(10) 0.00015(10) -0.00043(11)
W1 0.00967(12) 0.01209(15) 0.01206(14) -0.00001(10) 0.00059(10) -0.00077(11)
Cl6 0.0155(7) 0.0263(10) 0.0148(8) 0.0014(7) 0.0045(7) 0.0037(7)
Cl2 0.0179(8) 0.0222(10) 0.0130(8) -0.0014(7) 0.0016(7) -0.0018(7)
Cl7 0.0163(7) 0.0133(9) 0.0229(9) 0.0027(7) -0.0015(7) -0.0010(7)
Cl4 0.0169(8) 0.0261(10) 0.0130(8) -0.0006(7) 0.0046(7) 0.0024(7)
Cl8 0.0206(8) 0.0196(10) 0.0139(8) -0.0007(7) 0.0010(7) -0.0013(7)
Cl5 0.0153(7) 0.0130(9) 0.0236(8) -0.0011(7) -0.0001(7) -0.0005(7)
Cl1 0.0183(8) 0.0123(9) 0.0227(9) -0.0005(7) -0.0023(7) -0.0010(7)
S3 0.0111(7) 0.0140(9) 0.0116(8) -0.0025(6) 0.0031(6) -0.0001(7)
S2 0.0122(7) 0.0135(9) 0.0112(8) -0.0016(7) 0.0022(6) -0.0012(7)
Cl3 0.0146(7) 0.0136(9) 0.0246(9) 0.0000(7) 0.0009(7) 0.0005(7)
S4 0.0130(8) 0.0213(11) 0.0261(9) 0.0005(8) -0.0016(7) 0.0012(8)
S1 0.0121(8) 0.0280(12) 0.0228(9) 0.0064(8) -0.0029(7) -0.0029(8)
C5 0.015(3) 0.013(4) 0.022(4) 0.002(3) -0.002(3) 0.001(3)
C8 0.011(3) 0.016(4) 0.017(3) -0.007(3) -0.001(3) -0.002(3)
C7 0.019(3) 0.013(4) 0.010(3) 0.001(3) 0.001(3) -0.001(3)
C1 0.036(4) 0.018(4) 0.024(4) 0.011(3) 0.014(4) 0.007(4)
C4 0.015(3) 0.024(4) 0.016(3) 0.013(3) 0.006(3) 0.000(3)
C14 0.018(3) 0.019(4) 0.022(4) 0.006(3) 0.004(3) -0.003(3)
C6 0.012(3) 0.018(4) 0.004(3) -0.002(3) 0.002(3) -0.002(3)
C3 0.016(3) 0.024(4) 0.015(3) 0.003(3) 0.010(3) 0.003(3)
C10 0.013(3) 0.017(4) 0.020(4) 0.002(3) 0.002(3) -0.003(3)
C9 0.015(3) 0.013(4) 0.013(3) -0.004(3) 0.001(3) -0.006(3)
C13 0.032(4) 0.034(5) 0.011(3) 0.001(3) 0.002(3) -0.010(4)
C11 0.016(3) 0.022(4) 0.027(4) -0.006(3) 0.000(3) 0.001(3)
C2 0.034(4) 0.015(4) 0.031(4) 0.001(3) 0.020(4) 0.007(3)
C12 0.018(3) 0.032(5) 0.019(4) -0.012(3) 0.004(3) -0.001(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
W2 Cl6 2.3180(16) . ?
W2 Cl7 2.3157(18) . ?
W2 Cl8 2.2891(16) . ?
W2 Cl5 2.3143(18) . ?
W2 S3 2.8635(16) . ?
W2 S4 2.1039(17) . ?
W1 Cl2 2.2849(16) . ?
W1 Cl4 2.3213(16) . ?
W1 Cl1 2.3148(18) . ?
W1 S2 2.8600(16) . ?
W1 Cl3 2.3041(18) . ?
W1 S1 2.1003(17) . ?
S3 C8 1.819(7) . ?
S3 C9 1.777(6) . ?
S2 C7 1.812(7) . ?
S2 C6 1.775(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.377(9) . ?
C5 C6 1.397(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.521(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C1 H1 0.9300 . ?
C1 C6 1.381(9) . ?
C1 C2 1.389(9) . ?
C4 H4 0.9300 . ?
C4 C3 1.374(10) . ?
C14 H14 0.9300 . ?
C14 C9 1.393(9) . ?
C14 C13 1.383(9) . ?
C3 H3 0.9300 . ?
C3 C2 1.390(10) . ?
C10 H10 0.9300 . ?
C10 C9 1.385(9) . ?
C10 C11 1.403(9) . ?
C13 H13 0.9300 . ?
C13 C12 1.388(11) . ?
C11 H11 0.9300 . ?
C11 C12 1.365(10) . ?
C2 H2 0.9300 . ?
C12 H12 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
Cl6 W2 S3 75.55(5) . . ?
Cl7 W2 Cl6 88.16(6) . . ?
Cl7 W2 S3 78.02(5) . . ?
Cl8 W2 Cl6 159.19(6) . . ?
Cl8 W2 Cl7 87.57(6) . . ?
Cl8 W2 Cl5 89.02(6) . . ?
Cl8 W2 S3 83.65(5) . . ?
Cl5 W2 Cl6 88.66(6) . . ?
Cl5 W2 Cl7 161.64(6) . . ?
Cl5 W2 S3 83.67(5) . . ?
S4 W2 Cl6 99.63(6) . . ?
S4 W2 Cl7 101.07(7) . . ?
S4 W2 Cl8 101.17(7) . . ?
S4 W2 Cl5 97.30(7) . . ?
S4 W2 S3 175.09(6) . . ?
Cl2 W1 Cl4 159.78(6) . . ?
Cl2 W1 Cl1 89.55(6) . . ?
Cl2 W1 S2 83.88(5) . . ?
Cl2 W1 Cl3 87.39(6) . . ?
Cl4 W1 S2 76.03(5) . . ?
Cl1 W1 Cl4 88.31(6) . . ?
Cl1 W1 S2 77.44(5) . . ?
Cl3 W1 Cl4 88.00(6) . . ?
Cl3 W1 Cl1 160.61(6) . . ?
Cl3 W1 S2 83.19(5) . . ?
S1 W1 Cl2 100.37(6) . . ?
S1 W1 Cl4 99.80(6) . . ?
S1 W1 Cl1 99.88(7) . . ?
S1 W1 S2 175.02(6) . . ?
S1 W1 Cl3 99.51(7) . . ?
C8 S3 W2 105.8(2) . . ?
C9 S3 W2 113.7(2) . . ?
C9 S3 C8 101.7(3) . . ?
C7 S2 W1 108.6(2) . . ?
C6 S2 W1 110.5(2) . . ?
C6 S2 C7 103.7(3) . . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 119.8(7) . . ?
C6 C5 H5 120.1 . . ?
S3 C8 H8A 109.2 . . ?
S3 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C7 C8 S3 111.9(5) . . ?
C7 C8 H8A 109.2 . . ?
C7 C8 H8B 109.2 . . ?
S2 C7 H7A 109.8 . . ?
S2 C7 H7B 109.8 . . ?
C8 C7 S2 109.3(5) . . ?
C8 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
C6 C1 H1 120.1 . . ?
C6 C1 C2 119.8(7) . . ?
C2 C1 H1 120.1 . . ?
C5 C4 H4 119.8 . . ?
C3 C4 C5 120.4(6) . . ?
C3 C4 H4 119.8 . . ?
C9 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C13 C14 C9 118.9(7) . . ?
C5 C6 S2 123.3(5) . . ?
C1 C6 S2 116.7(5) . . ?
C1 C6 C5 120.0(6) . . ?
C4 C3 H3 119.9 . . ?
C4 C3 C2 120.2(6) . . ?
C2 C3 H3 119.9 . . ?
C9 C10 H10 119.8 . . ?
C9 C10 C11 120.4(6) . . ?
C11 C10 H10 119.8 . . ?
C14 C9 S3 122.6(5) . . ?
C10 C9 S3 117.3(5) . . ?
C10 C9 C14 120.0(6) . . ?
C14 C13 H13 119.5 . . ?
C14 C13 C12 120.9(7) . . ?
C12 C13 H13 119.5 . . ?
C10 C11 H11 120.4 . . ?
C12 C11 C10 119.2(7) . . ?
C12 C11 H11 120.4 . . ?
C1 C2 C3 119.8(7) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C13 C12 H12 119.8 . . ?
C11 C12 C13 120.5(6) . . ?
C11 C12 H12 119.8 . . ?

_shelx_res_file                  
;
TITL (wscl4)2phs(ch2)2sph)_a.res in P2(1)/n
    (wscl4)2phs(ch2)2sph).res
    created by SHELXL-2018/3 at 12:35:31 on 01-Jul-2019
REM Old TITL (WSCl4)2PhS(CH2)2SPh) in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.068, Rweak 0.006, Alpha 0.034
REM <I/s> 0.668 for 208 systematic absences, Orientation as input
REM Formula found by SHELXT: C14 S2 Cl10 W2
CELL 0.71073 10.579 13.9272 17.2182 90 96.368 90
ZERR 4 0.0002 0.0003 0.0004 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cl S W
UNIT 56 56 32 16 8

L.S. 4
PLAN  20
BOND $H
list 4
fmap 2
acta
OMIT -5 4 2
OMIT -7 2 17
OMIT -3 0 19
OMIT -3 0 21
OMIT -10 5 17
OMIT -4 1 21
OMIT -2 0 20
OMIT -4 0 20
OMIT -5 1 21
OMIT -8 3 17
OMIT -3 2 23
OMIT -10 5 15
OMIT 0 1 23
OMIT -7 1 17
OMIT -3 1 23
OMIT -3 1 21
OMIT -11 5 14
REM <olex2.extras>
REM <HklSrc "%.\\(WSCl4)2PhS(CH2)2SPh).hkl">
REM </olex2.extras>

WGHT    0.019100
FVAR       0.13073
W2    5    0.744389    0.725478    0.477740    11.00000    0.00967    0.01182 =
         0.01285    0.00054    0.00015   -0.00043
W1    5   -0.010761    0.494843    0.259011    11.00000    0.00967    0.01209 =
         0.01206   -0.00001    0.00059   -0.00077
CL6   3    0.731541    0.716065    0.342686    11.00000    0.01550    0.02627 =
         0.01483    0.00143    0.00452    0.00372
CL2   3    0.059901    0.494113    0.138337    11.00000    0.01792    0.02221 =
         0.01303   -0.00144    0.00164   -0.00175
CL7   3    0.715572    0.889775    0.464921    11.00000    0.01629    0.01326 =
         0.02292    0.00268   -0.00150   -0.00099
CL4   3   -0.006671    0.503572    0.393898    11.00000    0.01686    0.02606 =
         0.01298   -0.00061    0.00457    0.00242
CL8   3    0.679269    0.738783    0.599706    11.00000    0.02063    0.01959 =
         0.01389   -0.00069    0.00099   -0.00132
CL5   3    0.703442    0.562362    0.480739    11.00000    0.01534    0.01302 =
         0.02358   -0.00111   -0.00013   -0.00049
CL1   3    0.040412    0.333688    0.272738    11.00000    0.01831    0.01227 =
         0.02272   -0.00053   -0.00227   -0.00096
S3    4    0.477934    0.738719    0.426846    11.00000    0.01114    0.01404 =
         0.01161   -0.00245    0.00312   -0.00015
S2    4    0.254353    0.500367    0.314005    11.00000    0.01223    0.01347 =
         0.01122   -0.00157    0.00219   -0.00124
CL3   3    0.010841    0.659448    0.257939    11.00000    0.01458    0.01365 =
         0.02461   -0.00003    0.00089    0.00045
S4    4    0.942929    0.717372    0.505070    11.00000    0.01297    0.02127 =
         0.02605    0.00046   -0.00161    0.00121
S1    4   -0.207800    0.484114    0.227474    11.00000    0.01208    0.02802 =
         0.02280    0.00642   -0.00295   -0.00288
C5    1    0.374147    0.566092    0.187264    11.00000    0.01496    0.01347 =
         0.02193    0.00228   -0.00181    0.00068
AFIX  43
H5    2    0.346112    0.627522    0.197818    11.00000   -1.20000
AFIX   0
C8    1    0.431317    0.620989    0.387851    11.00000    0.01097    0.01643 =
         0.01706   -0.00692   -0.00103   -0.00154
AFIX  23
H8A   2    0.485601    0.603397    0.348278    11.00000   -1.20000
H8B   2    0.443438    0.573823    0.429462    11.00000   -1.20000
AFIX   0
C7    1    0.293216    0.619235    0.352209    11.00000    0.01933    0.01279 =
         0.01024    0.00143    0.00065   -0.00130
AFIX  23
H7A   2    0.280218    0.666178    0.310469    11.00000   -1.20000
H7B   2    0.238087    0.635606    0.391639    11.00000   -1.20000
AFIX   0
C1    1    0.389103    0.397998    0.219006    11.00000    0.03567    0.01799 =
         0.02385    0.01069    0.01396    0.00703
AFIX  43
H1    2    0.372768    0.346907    0.251211    11.00000   -1.20000
AFIX   0
C4    1    0.442096    0.550690    0.124648    11.00000    0.01487    0.02351 =
         0.01632    0.01305    0.00612    0.00045
AFIX  43
H4    2    0.461397    0.602125    0.093597    11.00000   -1.20000
AFIX   0
C14   1    0.377191    0.679953    0.561871    11.00000    0.01786    0.01882 =
         0.02175    0.00636    0.00444   -0.00299
AFIX  43
H14   2    0.424755    0.623953    0.560413    11.00000   -1.20000
AFIX   0
C6    1    0.347486    0.489148    0.234859    11.00000    0.01204    0.01848 =
         0.00426   -0.00216    0.00223   -0.00241
C3    1    0.481541    0.459788    0.107780    11.00000    0.01597    0.02355 =
         0.01484    0.00259    0.00975    0.00269
AFIX  43
H3    2    0.525835    0.449748    0.064756    11.00000   -1.20000
AFIX   0
C10   1    0.314779    0.834962    0.509273    11.00000    0.01252    0.01743 =
         0.02011    0.00181    0.00183   -0.00268
AFIX  43
H10   2    0.319387    0.882238    0.471546    11.00000   -1.20000
AFIX   0
C9    1    0.381637    0.750071    0.504573    11.00000    0.01472    0.01266 =
         0.01293   -0.00372    0.00100   -0.00591
C13   1    0.300924    0.694934    0.620960    11.00000    0.03158    0.03412 =
         0.01135    0.00097    0.00169   -0.00975
AFIX  43
H13   2    0.295570    0.647756    0.658680    11.00000   -1.20000
AFIX   0
C11   1    0.240128    0.850088    0.570608    11.00000    0.01601    0.02221 =
         0.02716   -0.00587   -0.00006    0.00096
AFIX  43
H11   2    0.196530    0.907599    0.574319    11.00000   -1.20000
AFIX   0
C2    1    0.455430    0.382786    0.154840    11.00000    0.03425    0.01491 =
         0.03078    0.00090    0.01976    0.00692
AFIX  43
H2    2    0.482270    0.321308    0.143406    11.00000   -1.20000
AFIX   0
C12   1    0.232240    0.779395    0.624773    11.00000    0.01846    0.03236 =
         0.01884   -0.01198    0.00444   -0.00127
AFIX  43
H12   2    0.180485    0.787883    0.664508    11.00000   -1.20000
AFIX   0
HKLF 4




REM  (wscl4)2phs(ch2)2sph)_a.res in P2(1)/n
REM wR2 = 0.0816, GooF = S = 0.968, Restrained GooF = 0.968 for all data
REM R1 = 0.0420 for 5333 Fo > 4sig(Fo) and 0.0625 for all 6811 data
REM 253 parameters refined using 0 restraints

END

WGHT      0.0160      0.0000

REM Highest difference peak  2.153,  deepest hole -2.693,  1-sigma level  0.308
Q1    1   0.6689  0.7272  0.4771  11.00000  0.05    2.15
Q2    1   0.0652  0.4899  0.2626  11.00000  0.05    1.93
Q3    1  -0.0890  0.4967  0.2567  11.00000  0.05    1.64
Q4    1   0.8259  0.7299  0.4803  11.00000  0.05    1.58
Q5    1   0.7744  0.6766  0.5111  11.00000  0.05    1.56
Q6    1   0.7561  0.7830  0.5020  11.00000  0.05    1.52
Q7    1  -0.0266  0.4623  0.2255  11.00000  0.05    1.40
Q8    1   0.9066  0.7689  0.4876  11.00000  0.05    1.30
Q9    1   0.0441  0.4546  0.3088  11.00000  0.05    1.24
Q10   1   0.8179  0.8392  0.5203  11.00000  0.05    1.23
Q11   1  -0.0877  0.5823  0.2636  11.00000  0.05    1.23
Q12   1   0.6975  0.8214  0.4433  11.00000  0.05    1.20
Q13   1   0.6813  0.6171  0.4440  11.00000  0.05    1.17
Q14   1   0.5009  0.7826  0.3820  11.00000  0.05    1.15
Q15   1  -0.1576  0.4442  0.2587  11.00000  0.05    1.15
Q16   1   0.1259  0.3420  0.2619  11.00000  0.05    1.13
Q17   1   0.5032  0.7812  0.5669  11.00000  0.05    1.12
Q18   1   0.8250  0.6184  0.5112  11.00000  0.05    1.10
Q19   1   0.8419  0.8071  0.4888  11.00000  0.05    1.09
Q20   1  -0.1639  0.5395  0.2478  11.00000  0.05    1.08
;
_shelx_res_checksum              75435
_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 4.946
_oxdiff_exptl_absorpt_empirical_full_min 0.355
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_wocl3-mes(ch2)3sme
_database_code_depnum_ccdc_archive 'CCDC 1949966'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton 
United Kingdom
;
_audit_update_record             
;
2019-08-28 deposited with the CCDC.	2020-01-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_wocl3-mes(ch2)3sme  
;
PROBLEM: Check Calcd Resid. Dens.  0.87A   From W1              4.87 eA-3
RESPONSE: Residual density from tungsten - absorption correction issue.
;
_vrf_PLAT971_wocl3-mes(ch2)3sme_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.79A   From W1              4.86 eA-3
RESPONSE: Residual density from tungsten - absorption correction issue.
;
# Added during the CSD deposition process: Wednesday 28 August 2019 03:14 PM
# end Validation Reply Form

_audit_creation_date             2019-08-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C5 H12 Cl3 O S2 W'
_chemical_formula_sum            'C5 H12 Cl3 O S2 W'
_chemical_formula_weight         442.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         WS3Cl3C5H12
_chemical_oxdiff_usercomment     'Yellow Plate'
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'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   6.7576(4)
_cell_length_b                   7.3941(4)
_cell_length_c                   12.4200(5)
_cell_angle_alpha                78.514(4)
_cell_angle_beta                 81.724(4)
_cell_angle_gamma                72.508(5)
_cell_volume                     577.68(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6925
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.9440
_cell_measurement_theta_min      3.6040
_shelx_estimated_absorpt_T_max   0.810
_shelx_estimated_absorpt_T_min   0.734
_exptl_absorpt_coefficient_mu    11.008
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.544
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             414
_exptl_crystal_preparation       'Slow Evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow Evporation from DCM'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15495
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.368
_diffrn_reflns_theta_min         2.929
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  94.00   1.00    1.00    --    5.00  38.00  60.00  113
  2  ω   -101.00  18.00   1.00    1.00    --  -12.10 -60.00 -30.00  119
  3  ω   -101.00  17.00   1.00    1.00    --  -12.10 -57.00  90.00  118
  4  ω    -36.00  77.00   1.00    1.00    --  -12.10  38.00 -90.00  113
  5  ω   -101.00  18.00   1.00    1.00    --  -12.10 -60.00-180.00  119
  6  ω    -42.00  34.00   1.00    1.00    --  -12.10  60.00   0.00   76
  7  ω    -42.00  77.00   1.00    1.00    --  -12.10  60.00  90.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0921703000
_diffrn_orient_matrix_UB_12      0.0651523000
_diffrn_orient_matrix_UB_13      0.0197839000
_diffrn_orient_matrix_UB_21      -0.0453624000
_diffrn_orient_matrix_UB_22      -0.0768566000
_diffrn_orient_matrix_UB_23      0.0190060000
_diffrn_orient_matrix_UB_31      0.0407075000
_diffrn_orient_matrix_UB_32      -0.0157420000
_diffrn_orient_matrix_UB_33      0.0516840000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3219
_reflns_number_total             3459
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         4.933
_refine_diff_density_min         -3.100
_refine_diff_density_rms         0.380
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         3459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0500
_refine_ls_restrained_S_all      1.097
_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)+(0.0684P)²+0.0903P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1207
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.77911(4) 0.37917(4) 0.74275(2) 0.01455(11) Uani 1 1 d . . . . .
Cl3 Cl 0.8466(3) 0.1549(3) 0.62143(14) 0.0204(3) Uani 1 1 d . . . . .
Cl2 Cl 0.9637(3) 0.1502(3) 0.87774(14) 0.0209(3) Uani 1 1 d . . . . .
S1 S 0.6736(3) 0.5813(3) 0.89358(13) 0.0163(3) Uani 1 1 d . . . . .
Cl1 Cl 0.4485(3) 0.3131(2) 0.82472(13) 0.0181(3) Uani 1 1 d . . . . .
S2 S 0.5226(3) 0.5922(3) 0.60984(13) 0.0160(3) Uani 1 1 d . . . . .
O1 O 0.9550(8) 0.5055(7) 0.6844(4) 0.0189(10) Uani 1 1 d . . . . .
C4 C 0.3439(10) 0.7865(10) 0.6743(5) 0.0185(14) Uani 1 1 d . . . . .
H4A H 0.275354 0.883816 0.616244 0.022 Uiso 1 1 calc R . . . .
H4B H 0.237320 0.736122 0.720107 0.022 Uiso 1 1 calc R . . . .
C1 C 0.8741(12) 0.7001(12) 0.8833(6) 0.0248(16) Uani 1 1 d . . . . .
H1A H 1.008179 0.609671 0.872661 0.037 Uiso 1 1 calc GR . . . .
H1B H 0.865670 0.750214 0.949922 0.037 Uiso 1 1 calc GR . . . .
H1C H 0.855360 0.803546 0.821810 0.037 Uiso 1 1 calc GR . . . .
C3 C 0.4306(11) 0.8853(10) 0.7443(5) 0.0186(14) Uani 1 1 d . . . . .
H3A H 0.567517 0.892854 0.711178 0.022 Uiso 1 1 calc R . . . .
H3B H 0.341640 1.015805 0.743267 0.022 Uiso 1 1 calc R . . . .
C5 C 0.6699(11) 0.7199(11) 0.5071(6) 0.0215(15) Uani 1 1 d . . . . .
H5A H 0.725608 0.797161 0.541445 0.032 Uiso 1 1 calc GR . . . .
H5B H 0.580756 0.801295 0.452555 0.032 Uiso 1 1 calc GR . . . .
H5C H 0.782063 0.629582 0.472534 0.032 Uiso 1 1 calc GR . . . .
C2 C 0.4486(11) 0.7871(10) 0.8630(6) 0.0196(14) Uani 1 1 d . . . . .
H2A H 0.324330 0.745407 0.888382 0.024 Uiso 1 1 calc R . . . .
H2B H 0.448284 0.882540 0.906554 0.024 Uiso 1 1 calc R . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.01507(17) 0.01725(17) 0.01181(16) -0.00252(11) -0.00201(10) -0.00479(11)
Cl3 0.0214(8) 0.0215(8) 0.0194(8) -0.0074(6) -0.0022(6) -0.0051(6)
Cl2 0.0229(8) 0.0209(8) 0.0166(8) 0.0006(6) -0.0068(6) -0.0031(7)
S1 0.0176(8) 0.0200(8) 0.0131(7) -0.0030(6) -0.0022(6) -0.0072(6)
Cl1 0.0183(8) 0.0223(8) 0.0164(7) -0.0040(6) -0.0001(6) -0.0100(6)
S2 0.0182(8) 0.0178(8) 0.0113(7) -0.0015(6) -0.0030(6) -0.0039(6)
O1 0.020(2) 0.024(3) 0.012(2) -0.0033(19) -0.0051(18) -0.002(2)
C4 0.016(3) 0.019(3) 0.017(3) -0.002(3) -0.001(3) 0.000(3)
C1 0.031(4) 0.034(4) 0.017(3) -0.005(3) -0.002(3) -0.019(3)
C3 0.024(4) 0.016(3) 0.012(3) 0.001(2) 0.000(3) -0.003(3)
C5 0.023(4) 0.026(4) 0.014(3) 0.004(3) -0.002(3) -0.010(3)
C2 0.022(4) 0.018(3) 0.017(3) -0.004(3) 0.004(3) -0.004(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 Cl3 2.3605(17) . ?
W1 Cl2 2.3314(17) . ?
W1 S1 2.5184(17) . ?
W1 Cl1 2.4639(16) . ?
W1 S2 2.5216(17) . ?
W1 O1 1.720(5) . ?
S1 C1 1.801(7) . ?
S1 C2 1.821(7) . ?
S2 C4 1.816(7) . ?
S2 C5 1.797(7) . ?
C4 C3 1.513(10) . ?
C3 C2 1.513(9) . ?

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
Cl3 W1 S1 170.11(6) . . ?
Cl3 W1 Cl1 93.29(6) . . ?
Cl3 W1 S2 85.14(6) . . ?
Cl2 W1 Cl3 92.19(6) . . ?
Cl2 W1 S1 83.39(6) . . ?
Cl2 W1 Cl1 91.62(6) . . ?
Cl2 W1 S2 168.30(6) . . ?
S1 W1 S2 97.42(6) . . ?
Cl1 W1 S1 78.05(5) . . ?
Cl1 W1 S2 77.19(6) . . ?
O1 W1 Cl3 100.32(17) . . ?
O1 W1 Cl2 102.31(16) . . ?
O1 W1 S1 89.28(17) . . ?
O1 W1 Cl1 160.02(17) . . ?
O1 W1 S2 89.38(16) . . ?
C1 S1 W1 105.3(3) . . ?
C1 S1 C2 100.7(4) . . ?
C2 S1 W1 112.1(2) . . ?
C4 S2 W1 110.2(2) . . ?
C5 S2 W1 105.6(2) . . ?
C5 S2 C4 101.6(3) . . ?
C3 C4 S2 118.4(5) . . ?
C2 C3 C4 114.5(6) . . ?
C3 C2 S1 117.9(5) . . ?

_shelx_res_file                  
;
TITL wscl3-mesch2ch2sme_a.res in P-1
    wocl3-mes(ch2)3sme.res
    created by SHELXL-2018/3 at 15:58:30 on 19-Aug-2019
REM Old TITL WSCl3-MeSCH2CH2SMe in P1 #1
REM SHELXT solution in P-1: R1 0.057, Rweak 0.011, Alpha 0.034
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C6 S2 Cl3 W
CELL 0.71073 6.7576 7.3941 12.42 78.514 81.724 72.508
ZERR 2 0.0004 0.0004 0.0005 0.004 0.004 0.005
LATT 1
SFAC C H Cl O S W
UNIT 10 24 6 2 4 2

L.S. 4 0 0
PLAN  20
SIZE 0.03 0.02 0.02
BOND
list 4
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\WOCl3-MeS(CH2)3SMe.hkl">
REM </olex2.extras>

WGHT    0.068400    0.090300
FVAR       0.39369
W1    6    0.779109    0.379168    0.742750    11.00000    0.01507    0.01725 =
         0.01181   -0.00252   -0.00201   -0.00479
CL3   3    0.846557    0.154869    0.621428    11.00000    0.02139    0.02154 =
         0.01939   -0.00742   -0.00215   -0.00507
CL2   3    0.963717    0.150210    0.877738    11.00000    0.02295    0.02091 =
         0.01659    0.00065   -0.00682   -0.00311
S1    5    0.673602    0.581347    0.893576    11.00000    0.01759    0.02004 =
         0.01306   -0.00304   -0.00216   -0.00725
CL1   3    0.448451    0.313136    0.824720    11.00000    0.01830    0.02229 =
         0.01643   -0.00398   -0.00014   -0.01004
S2    5    0.522566    0.592215    0.609841    11.00000    0.01821    0.01784 =
         0.01134   -0.00146   -0.00301   -0.00394
O1    4    0.954968    0.505516    0.684444    11.00000    0.01951    0.02447 =
         0.01163   -0.00327   -0.00508   -0.00249
C4    1    0.343938    0.786506    0.674259    11.00000    0.01585    0.01896 =
         0.01685   -0.00193   -0.00090   -0.00017
AFIX  23
H4A   2    0.275354    0.883816    0.616244    11.00000   -1.20000
H4B   2    0.237320    0.736122    0.720107    11.00000   -1.20000
AFIX   0
C1    1    0.874108    0.700051    0.883292    11.00000    0.03064    0.03439 =
         0.01651   -0.00486   -0.00218   -0.01922
AFIX 137
H1A   2    1.008179    0.609671    0.872661    11.00000   -1.50000
H1B   2    0.865670    0.750214    0.949922    11.00000   -1.50000
H1C   2    0.855360    0.803546    0.821810    11.00000   -1.50000
AFIX   0
C3    1    0.430571    0.885326    0.744286    11.00000    0.02391    0.01606 =
         0.01177    0.00146    0.00018   -0.00286
AFIX  23
H3A   2    0.567517    0.892854    0.711178    11.00000   -1.20000
H3B   2    0.341640    1.015805    0.743267    11.00000   -1.20000
AFIX   0
C5    1    0.669909    0.719939    0.507131    11.00000    0.02331    0.02647 =
         0.01370    0.00386   -0.00224   -0.00969
AFIX 137
H5A   2    0.725608    0.797161    0.541445    11.00000   -1.50000
H5B   2    0.580756    0.801295    0.452555    11.00000   -1.50000
H5C   2    0.782063    0.629582    0.472534    11.00000   -1.50000
AFIX   0
C2    1    0.448640    0.787116    0.863010    11.00000    0.02229    0.01757 =
         0.01659   -0.00382    0.00396   -0.00395
AFIX  23
H2A   2    0.324330    0.745407    0.888382    11.00000   -1.20000
H2B   2    0.448284    0.882540    0.906554    11.00000   -1.20000
AFIX   0
HKLF 4




REM  wscl3-mesch2ch2sme_a.res in P-1
REM wR2 = 0.1207, GooF = S = 1.097, Restrained GooF = 1.097 for all data
REM R1 = 0.0500 for 3219 Fo > 4sig(Fo) and 0.0558 for all 3459 data
REM 111 parameters refined using 0 restraints

END

WGHT      0.0684      0.0903

REM Highest difference peak  4.933,  deepest hole -3.100,  1-sigma level  0.380
Q1    1   0.7294  0.5056  0.7430  11.00000  0.05    4.93
Q2    1   0.8386  0.2559  0.7413  11.00000  0.05    4.87
Q3    1   0.6933  0.3142  0.7758  11.00000  0.05    3.29
Q4    1   0.8640  0.4582  0.7086  11.00000  0.05    3.09
Q5    1   0.5923  0.2678  0.7968  11.00000  0.05    2.00
Q6    1   0.5159  0.3770  0.7792  11.00000  0.05    1.46
Q7    1   0.3421  0.2983  0.8578  11.00000  0.05    1.37
Q8    1   0.6562  0.8525  0.7801  11.00000  0.05    1.36
Q9    1   0.5803  0.6330  0.8986  11.00000  0.05    1.34
Q10   1   0.9940  0.4485  0.6827  11.00000  0.05    1.26
Q11   1   1.1104  0.4600  0.6598  11.00000  0.05    1.21
Q12   1   1.1577  0.2124  0.8065  11.00000  0.05    1.13
Q13   1   0.5016  0.1614  0.8398  11.00000  0.05    1.08
Q14   1   0.6581  0.4830  0.9392  11.00000  0.05    1.05
Q15   1   0.8471  0.2864  0.6068  11.00000  0.05    1.05
Q16   1   0.7326  0.6336  0.7179  11.00000  0.05    1.04
Q17   1   0.5333  0.4577  0.8378  11.00000  0.05    1.04
Q18   1   0.6616  0.1610  0.7539  11.00000  0.05    1.01
Q19   1   0.4351  0.5213  0.6382  11.00000  0.05    0.97
Q20   1   0.5952  0.7347  0.8971  11.00000  0.05    0.95
;
_shelx_res_checksum              91783
_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 1.904
_oxdiff_exptl_absorpt_empirical_full_min 0.563
####################################################################### 
# 
# 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_dsex94rdb
_database_code_depnum_ccdc_archive 'CCDC 1949963'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton 
United Kingdom
;
_audit_update_record             
;
2019-08-28 deposited with the CCDC.	2020-01-28 downloaded from the CCDC.
;
_audit_creation_date             2019-07-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H10 Cl8 S4 W2'
_chemical_formula_sum            'C4 H10 Cl8 S4 W2'
_chemical_formula_weight         837.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W2 S4 Cl8 C4 H10'
_chemical_oxdiff_usercomment     'Red Block'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.6849(2)
_cell_length_b                   10.5079(3)
_cell_length_c                   11.8240(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.882(3)
_cell_angle_gamma                90
_cell_volume                     954.30(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7344
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.1650
_cell_measurement_theta_min      3.2880
_shelx_estimated_absorpt_T_max   0.876
_shelx_estimated_absorpt_T_min   0.773
_exptl_absorpt_coefficient_mu    13.581
_exptl_absorpt_correction_T_max  0.00827
_exptl_absorpt_correction_T_min  0.00090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.915
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1412
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13938
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.981
_diffrn_reflns_theta_min         3.956
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -37.00  77.00   1.00    1.00    --  -12.30  38.00 -90.00  114
  2  ω   -102.00  17.00   1.00    1.00    --  -12.30 -57.00 -30.00  119
  3  ω   -102.00  17.00   1.00    1.00    --  -12.30 -57.00-120.00  119
  4  ω   -102.00  17.00   1.00    1.00    --  -12.30 -57.00 150.00  119
  5  ω    -43.00  28.00   1.00    1.00    --  -12.30  60.00   0.00   71
  6  ω    -42.00  77.00   1.00    1.00    --  -12.30  57.00  90.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0769411000
_diffrn_orient_matrix_UB_12      -0.0160792000
_diffrn_orient_matrix_UB_13      -0.0316001000
_diffrn_orient_matrix_UB_21      -0.0349005000
_diffrn_orient_matrix_UB_22      -0.0279082000
_diffrn_orient_matrix_UB_23      0.0489127000
_diffrn_orient_matrix_UB_31      -0.0373271000
_diffrn_orient_matrix_UB_32      0.0593180000
_diffrn_orient_matrix_UB_33      0.0145066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1697
_reflns_number_total             1864
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.356
_refine_diff_density_min         -1.347
_refine_diff_density_rms         0.431
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1864
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0572
_refine_ls_restrained_S_all      1.113
_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)+(0.0969P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1519
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_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 0.26713(4) 0.42356(3) 0.66838(3) 0.0437(3) Uani 1 1 d . . . . .
Cl4 Cl 0.5502(3) 0.42995(19) 0.7403(3) 0.0504(6) Uani 1 1 d . . . . .
Cl2 Cl -0.0323(3) 0.4269(2) 0.6588(3) 0.0549(6) Uani 1 1 d . . . . .
S2 S 0.2367(3) 0.4657(2) 0.9037(2) 0.0477(5) Uani 1 1 d . . . . .
Cl1 Cl 0.2455(3) 0.2183(2) 0.7357(2) 0.0537(6) Uani 1 1 d . . . . .
Cl3 Cl 0.2609(3) 0.6417(3) 0.6599(2) 0.0573(7) Uani 1 1 d . . . . .
S1 S 0.3228(3) 0.3828(3) 0.5000(2) 0.0549(6) Uani 1 1 d . . . . .
C2 C 0.3262(13) 0.6207(9) 0.9346(9) 0.057(2) Uani 1 1 d . . . . .
H2A H 0.440665 0.626600 0.904940 0.085 Uiso 1 1 calc GR . . . .
H2B H 0.332816 0.633257 1.015045 0.085 Uiso 1 1 calc GR . . . .
H2C H 0.252703 0.684744 0.900301 0.085 Uiso 1 1 calc GR . . . .
C1 C 0.0108(12) 0.4883(10) 0.9380(9) 0.052(2) Uani 1 1 d . . . . .
H1A H -0.035981 0.560216 0.895426 0.062 Uiso 1 1 calc R . . . .
H1B H -0.055240 0.413396 0.915305 0.062 Uiso 1 1 calc R . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.0435(3) 0.0420(4) 0.0458(4) 0.00098(12) 0.0048(2) 0.00014(11)
Cl4 0.0421(12) 0.0541(13) 0.0552(15) -0.0005(9) 0.0058(11) -0.0001(8)
Cl2 0.0440(13) 0.0656(15) 0.0551(16) -0.0017(10) 0.0022(11) 0.0021(8)
S2 0.0467(12) 0.0492(12) 0.0475(13) 0.0004(10) 0.0071(9) 0.0022(9)
Cl1 0.0621(13) 0.0441(11) 0.0548(13) 0.0021(9) 0.0011(10) -0.0048(9)
Cl3 0.0674(16) 0.0460(15) 0.0586(16) 0.0037(9) 0.0055(12) -0.0007(8)
S1 0.0577(14) 0.0585(13) 0.0487(13) -0.0014(11) 0.0068(10) -0.0009(10)
C2 0.057(5) 0.048(5) 0.066(6) -0.010(5) 0.006(4) -0.009(4)
C1 0.042(4) 0.059(5) 0.054(5) -0.001(4) 0.015(4) 0.008(4)

_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 Cl4 2.311(3) . ?
W1 Cl2 2.301(3) . ?
W1 S2 2.835(2) . ?
W1 Cl1 2.307(2) . ?
W1 Cl3 2.295(3) . ?
W1 S1 2.095(2) . ?
S2 C2 1.801(10) . ?
S2 C1 1.811(9) . ?
C1 C1 1.50(2) 3_567 ?

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
Cl4 W1 S2 75.01(9) . . ?
Cl2 W1 Cl4 161.06(12) . . ?
Cl2 W1 S2 86.05(9) . . ?
Cl2 W1 Cl1 87.02(9) . . ?
Cl1 W1 Cl4 88.73(8) . . ?
Cl1 W1 S2 78.35(8) . . ?
Cl3 W1 Cl4 90.29(8) . . ?
Cl3 W1 Cl2 87.89(8) . . ?
Cl3 W1 S2 83.38(8) . . ?
Cl3 W1 Cl1 161.32(8) . . ?
S1 W1 Cl4 97.84(10) . . ?
S1 W1 Cl2 101.05(10) . . ?
S1 W1 S2 172.33(8) . . ?
S1 W1 Cl1 98.98(10) . . ?
S1 W1 Cl3 99.64(10) . . ?
C2 S2 W1 107.3(4) . . ?
C2 S2 C1 101.4(5) . . ?
C1 S2 W1 110.5(3) . . ?
C1 C1 S2 112.2(9) 3_567 . ?

_shelx_res_file                  
;
TITL dsex94rdb_a.res in P2(1)/c
    dsex94rdb.res
    created by SHELXL-2018/3 at 14:18:29 on 01-Jul-2019
REM Old TITL DS EX94 rdb in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.073, Rweak 0.011, Alpha 0.026, Orientation as input
REM Formula found by SHELXT: C2 S Cl3 W
CELL 0.71073 7.684899 10.507902 11.824044 90 91.8823 90
ZERR 2 0.000226 0.0003 0.000413 0 0.0029 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl S W
UNIT 8 20 16 8 4

L.S. 10 0 0
PLAN  20
SIZE 0.02 0.02 0.01
LIST 6
fmap 2 53
acta
OMIT -4 52
OMIT 0 2 0
OMIT 0 2 1
OMIT 0 0 2
OMIT 1 1 0
OMIT 1 1 1
OMIT -1 1 1
REM <olex2.extras>
REM <HklSrc "%.\\DS%20EX94%20rdb.hkl">
REM </olex2.extras>

WGHT    0.096900
FVAR       2.26767
W1    5    0.267129    0.423559    0.668375    11.00000    0.04347    0.04198 =
         0.04580    0.00098    0.00483    0.00014
CL4   3    0.550206    0.429950    0.740308    11.00000    0.04212    0.05414 =
         0.05517   -0.00051    0.00576   -0.00010
CL2   3   -0.032338    0.426920    0.658791    11.00000    0.04402    0.06559 =
         0.05509   -0.00172    0.00224    0.00213
S2    4    0.236655    0.465680    0.903709    11.00000    0.04671    0.04922 =
         0.04745    0.00037    0.00711    0.00219
CL1   3    0.245500    0.218319    0.735697    11.00000    0.06210    0.04408 =
         0.05483    0.00210    0.00108   -0.00480
CL3   3    0.260916    0.641732    0.659885    11.00000    0.06737    0.04603 =
         0.05863    0.00373    0.00552   -0.00071
S1    4    0.322844    0.382772    0.499980    11.00000    0.05772    0.05855 =
         0.04872   -0.00136    0.00684   -0.00090
C2    1    0.326155    0.620657    0.934604    11.00000    0.05662    0.04779 =
         0.06576   -0.00986    0.00575   -0.00949
AFIX 137
H2A   2    0.440665    0.626600    0.904940    11.00000   -1.50000
H2B   2    0.332816    0.633257    1.015045    11.00000   -1.50000
H2C   2    0.252703    0.684744    0.900301    11.00000   -1.50000
AFIX   0
C1    1    0.010837    0.488343    0.937963    11.00000    0.04217    0.05915 =
         0.05422   -0.00101    0.01526    0.00752
AFIX  23
H1A   2   -0.035981    0.560216    0.895426    11.00000   -1.20000
H1B   2   -0.055240    0.413396    0.915305    11.00000   -1.20000
AFIX   0
HKLF 4




REM  dsex94rdb_a.res in P2(1)/c
REM wR2 = 0.1519, GooF = S = 1.113, Restrained GooF = 1.113 for all data
REM R1 = 0.0572 for 1697 Fo > 4sig(Fo) and 0.0597 for all 1864 data
REM 83 parameters refined using 0 restraints

END

WGHT      0.0969      0.0000

REM Highest difference peak  3.356,  deepest hole -1.347,  1-sigma level  0.431
Q1    1   0.1545  0.4176  0.6686  11.00000  0.05    3.36
Q2    1   0.3806  0.4172  0.6683  11.00000  0.05    3.24
Q3    1   0.3173  0.3605  0.6555  11.00000  0.05    2.77
Q4    1   0.2379  0.4975  0.6726  11.00000  0.05    2.62
Q5    1   0.2822  0.4974  0.6589  11.00000  0.05    2.59
Q6    1   0.2542  0.3469  0.6777  11.00000  0.05    2.52
Q7    1   0.2937  0.4182  0.5884  11.00000  0.05    2.50
Q8    1   0.2616  0.4267  0.7404  11.00000  0.05    1.99
Q9    1   0.2712  0.7174  0.6679  11.00000  0.05    1.36
Q10   1   0.1155  0.4715  0.9209  11.00000  0.05    0.97
Q11   1   0.2720  0.1635  0.6818  11.00000  0.05    0.95
Q12   1   0.2028  0.4360  0.9945  11.00000  0.05    0.93
Q13   1   0.5396  0.4251  0.6644  11.00000  0.05    0.93
Q14   1   0.2424  0.2158  0.6668  11.00000  0.05    0.91
Q15   1   0.1672  0.1964  0.7426  11.00000  0.05    0.91
Q16   1   0.2911  0.6623  0.5857  11.00000  0.05    0.90
Q17   1   0.1898  0.1548  0.6640  11.00000  0.05    0.86
Q18   1   0.2737  0.6662  0.9181  11.00000  0.05    0.81
Q19   1   0.2001  0.6827  0.5986  11.00000  0.05    0.81
Q20   1   0.1388  0.6560  0.6659  11.00000  0.05    0.76
;
_shelx_res_checksum              84528
_olex2_exptl_crystal_mounting_method Mounted
_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 5.229
_oxdiff_exptl_absorpt_empirical_full_min 0.088
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_exp614sphere
_database_code_depnum_ccdc_archive 'CCDC 1949964'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton 
United Kingdom
;
_audit_update_record             
;
2019-08-28 deposited with the CCDC.	2020-01-28 downloaded from the CCDC.
;
_audit_creation_date             2019-07-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H18 Cl8 S4 W2'
_chemical_formula_sum            'C8 H18 Cl8 S4 W2'
_chemical_formula_weight         893.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     'Red Plate'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.7903(2)
_cell_length_b                   8.89710(10)
_cell_length_c                   12.1898(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.732(2)
_cell_angle_gamma                90
_cell_volume                     1120.70(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8954
_cell_measurement_temperature    99.97(13)
_cell_measurement_theta_max      30.9100
_cell_measurement_theta_min      3.4410
_shelx_estimated_absorpt_T_max   0.893
_shelx_estimated_absorpt_T_min   0.723
_exptl_absorpt_coefficient_mu    11.574
_exptl_absorpt_correction_T_max  0.88652
_exptl_absorpt_correction_T_min  0.88652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.649
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             828
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evaporation from DCM'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18750
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.991
_diffrn_reflns_theta_min         3.021
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  94.00   1.00    1.66    --    5.00  38.00-180.00  113
  2  ω   -101.00  12.00   1.00    1.66    --  -12.10 -38.00 120.00  113
  3  ω   -101.00  18.00   1.00    1.66    --  -12.10 -60.00 -90.00  119
  4  ω    -88.00   9.00   1.00    1.66    --  -12.10 -60.00   0.00   97
  5  ω   -101.00  18.00   1.00    1.66    --  -12.10 -60.00 120.00  119
  6  ω     35.00  61.00   1.00    1.66    --  -12.10  38.00  90.00   26
  7  ω    -20.00  13.00   1.00    1.66    --  -12.10  38.00  90.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0492844000
_diffrn_orient_matrix_UB_12      -0.0082326000
_diffrn_orient_matrix_UB_13      -0.0275123000
_diffrn_orient_matrix_UB_21      -0.0473775000
_diffrn_orient_matrix_UB_22      0.0017393000
_diffrn_orient_matrix_UB_23      -0.0541418000
_diffrn_orient_matrix_UB_31      0.0061704000
_diffrn_orient_matrix_UB_32      0.0792731000
_diffrn_orient_matrix_UB_33      -0.0016902000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2117
_reflns_number_total             2199
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.053
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.220
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0391
_refine_ls_restrained_S_all      1.180
_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)+(0.0309P)²+10.6377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0884
_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 C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
;
_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 0.21375(2) 0.74893(3) 0.63811(2) 0.01503(13) Uani 1 1 d . . . . .
Cl2 Cl 0.08562(16) 0.7999(2) 0.45334(15) 0.0234(4) Uani 1 1 d . . . . .
S2 S 0.29908(16) 0.5239(2) 0.50828(15) 0.0191(4) Uani 1 1 d . . . . .
Cl1 Cl 0.07048(16) 0.5615(2) 0.65113(15) 0.0219(4) Uani 1 1 d . . . . .
Cl4 Cl 0.36116(16) 0.6410(2) 0.79507(15) 0.0238(4) Uani 1 1 d . . . . .
Cl3 Cl 0.38429(16) 0.8703(2) 0.59697(16) 0.0236(4) Uani 1 1 d . . . . .
S1 S 0.14578(18) 0.9220(2) 0.72232(17) 0.0251(4) Uani 1 1 d . . . . .
C2 C 0.2970(8) 0.2761(9) 0.6503(7) 0.0257(17) Uani 1 1 d . . . . .
H2A H 0.387327 0.255202 0.663165 0.039 Uiso 1 1 calc GR . . . .
H2B H 0.252813 0.185372 0.659529 0.039 Uiso 1 1 calc GR . . . .
H2C H 0.286632 0.349754 0.704513 0.039 Uiso 1 1 calc GR . . . .
C3 C 0.2404(7) 0.3358(8) 0.5299(6) 0.0199(15) Uani 1 1 d . . . . .
H3 H 0.147026 0.345454 0.518284 0.024 Uiso 1 1 calc R . . . .
C1 C 0.4752(6) 0.5037(9) 0.5531(6) 0.0214(15) Uani 1 1 d . . . . .
H1A H 0.514334 0.588554 0.600437 0.026 Uiso 1 1 calc R . . . .
H1B H 0.499388 0.412780 0.598025 0.026 Uiso 1 1 calc R . . . .
C4 C 0.2569(9) 0.2268(9) 0.4392(8) 0.0312(19) Uani 1 1 d . . . . .
H4A H 0.217984 0.268474 0.364497 0.047 Uiso 1 1 calc GR . . . .
H4B H 0.215693 0.133194 0.446293 0.047 Uiso 1 1 calc GR . . . .
H4C H 0.347379 0.210037 0.449322 0.047 Uiso 1 1 calc GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.01305(18) 0.01535(19) 0.01671(19) -0.00004(10) 0.00429(13) -0.00053(10)
Cl2 0.0214(8) 0.0256(9) 0.0207(9) 0.0039(7) 0.0022(7) 0.0025(7)
S2 0.0166(8) 0.0205(9) 0.0209(9) 0.0014(7) 0.0065(7) 0.0009(7)
Cl1 0.0173(8) 0.0232(9) 0.0261(9) 0.0000(7) 0.0077(7) -0.0033(7)
Cl4 0.0199(8) 0.0263(9) 0.0223(9) 0.0013(7) 0.0014(7) -0.0005(7)
Cl3 0.0198(8) 0.0201(9) 0.0322(10) -0.0011(7) 0.0093(7) -0.0055(7)
S1 0.0275(9) 0.0235(10) 0.0255(10) -0.0036(8) 0.0096(8) 0.0016(7)
C2 0.022(4) 0.027(4) 0.027(4) 0.004(3) 0.006(3) -0.001(3)
C3 0.019(3) 0.017(3) 0.026(4) -0.001(3) 0.010(3) -0.001(3)
C1 0.013(3) 0.027(4) 0.026(4) 0.004(3) 0.008(3) 0.004(3)
C4 0.034(5) 0.029(4) 0.034(5) -0.001(4) 0.015(4) 0.002(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 Cl2 2.3231(17) . ?
W1 S2 2.8633(18) . ?
W1 Cl1 2.3100(17) . ?
W1 Cl4 2.3155(17) . ?
W1 Cl3 2.3096(17) . ?
W1 S1 2.0967(19) . ?
S2 C3 1.836(7) . ?
S2 C1 1.829(7) . ?
C2 C3 1.514(11) . ?
C3 C4 1.519(11) . ?
C1 C1 1.537(14) 3_666 ?

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
Cl2 W1 S2 78.29(6) . . ?
Cl1 W1 Cl2 89.10(6) . . ?
Cl1 W1 S2 82.03(6) . . ?
Cl1 W1 Cl4 87.58(6) . . ?
Cl4 W1 Cl2 163.26(7) . . ?
Cl4 W1 S2 85.01(6) . . ?
Cl3 W1 Cl2 89.27(6) . . ?
Cl3 W1 S2 78.68(6) . . ?
Cl3 W1 Cl1 160.57(6) . . ?
Cl3 W1 Cl4 88.43(6) . . ?
S1 W1 Cl2 97.87(7) . . ?
S1 W1 S2 175.95(7) . . ?
S1 W1 Cl1 99.27(7) . . ?
S1 W1 Cl4 98.86(7) . . ?
S1 W1 Cl3 100.13(7) . . ?
C3 S2 W1 112.3(2) . . ?
C1 S2 W1 112.1(2) . . ?
C1 S2 C3 103.8(3) . . ?
C2 C3 S2 113.6(5) . . ?
C2 C3 C4 112.5(6) . . ?
C4 C3 S2 111.1(5) . . ?
C1 C1 S2 109.7(6) 3_666 . ?

_shelx_res_file                  
;
TITL exp614sphere_a.res in P2(1)/c
    exp614sphere.res
    created by SHELXL-2018/3 at 14:33:42 on 01-Jul-2019
REM Old TITL exp614sphere_a.res in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.059, Rweak 0.001, Alpha 0.010, Orientation as input
REM Formula found by SHELXT: W S Cl5 C4
CELL 0.71073 10.7903 8.8971 12.1898 90 106.732 90
ZERR 2 0.0002 0.0001 0.0002 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl S W
UNIT 16 36 16 8 4

L.S. 10 0 0
PLAN  20
SIZE 0.02 0.03 0.01
LIST 6
fmap 2 53
acta
OMIT -4 52
OMIT -8 6 10
REM <olex2.extras>
REM <HklSrc "%.\\exp%20614%20sphere.hkl">
REM </olex2.extras>

WGHT    0.030900   10.637700
FVAR       0.29344
W1    5    0.213746    0.748934    0.638106    11.00000    0.01305    0.01535 =
         0.01671   -0.00004    0.00429   -0.00053
CL2   3    0.085621    0.799912    0.453341    11.00000    0.02143    0.02562 =
         0.02065    0.00392    0.00222    0.00248
S2    4    0.299085    0.523932    0.508285    11.00000    0.01662    0.02050 =
         0.02086    0.00139    0.00655    0.00094
CL1   3    0.070483    0.561536    0.651129    11.00000    0.01729    0.02324 =
         0.02608    0.00003    0.00775   -0.00335
CL4   3    0.361158    0.640958    0.795074    11.00000    0.01994    0.02630 =
         0.02230    0.00128    0.00136   -0.00047
CL3   3    0.384287    0.870268    0.596967    11.00000    0.01976    0.02007 =
         0.03215   -0.00115    0.00932   -0.00549
S1    4    0.145776    0.921990    0.722323    11.00000    0.02746    0.02353 =
         0.02547   -0.00357    0.00958    0.00157
C2    1    0.296968    0.276061    0.650293    11.00000    0.02241    0.02701 =
         0.02720    0.00419    0.00638   -0.00118
AFIX 137
H2A   2    0.387327    0.255202    0.663165    11.00000   -1.50000
H2B   2    0.252813    0.185372    0.659529    11.00000   -1.50000
H2C   2    0.286632    0.349754    0.704513    11.00000   -1.50000
AFIX   0
C3    1    0.240398    0.335765    0.529909    11.00000    0.01926    0.01707 =
         0.02594   -0.00124    0.01040   -0.00057
AFIX  13
H3    2    0.147026    0.345454    0.518284    11.00000   -1.20000
AFIX   0
C1    1    0.475232    0.503726    0.553056    11.00000    0.01294    0.02680 =
         0.02576    0.00365    0.00785    0.00388
AFIX  23
H1A   2    0.514334    0.588554    0.600437    11.00000   -1.20000
H1B   2    0.499388    0.412780    0.598025    11.00000   -1.20000
AFIX   0
C4    1    0.256880    0.226845    0.439154    11.00000    0.03414    0.02851 =
         0.03412   -0.00083    0.01477    0.00171
AFIX 137
H4A   2    0.217984    0.268474    0.364497    11.00000   -1.50000
H4B   2    0.215693    0.133194    0.446293    11.00000   -1.50000
H4C   2    0.347379    0.210037    0.449322    11.00000   -1.50000
AFIX   0
HKLF 4




REM  exp614sphere_a.res in P2(1)/c
REM wR2 = 0.0884, GooF = S = 1.180, Restrained GooF = 1.180 for all data
REM R1 = 0.0391 for 2117 Fo > 4sig(Fo) and 0.0413 for all 2199 data
REM 102 parameters refined using 0 restraints

END

WGHT      0.0309     10.6229

REM Highest difference peak  3.053,  deepest hole -1.229,  1-sigma level  0.220
Q1    1   0.3570  0.7539  0.5835  11.00000  0.05    3.05
Q2    1   0.2978  0.9790  0.5050  11.00000  0.05    2.10
Q3    1   0.3846  0.6252  0.5960  11.00000  0.05    1.94
Q4    1   0.0792  0.9385  0.6518  11.00000  0.05    1.82
Q5    1   0.1460  0.5758  0.7208  11.00000  0.05    1.72
Q6    1   0.0829  0.6994  0.4581  11.00000  0.05    1.62
Q7    1   0.6384  0.3573  0.7072  11.00000  0.05    1.51
Q8    1   0.2939  0.7572  0.7264  11.00000  0.05    0.98
Q9    1   0.1435  0.7578  0.5489  11.00000  0.05    0.94
Q10   1   0.1203  0.5042  0.7742  11.00000  0.05    0.86
Q11   1   0.1634  0.8782  0.6432  11.00000  0.05    0.82
Q12   1   0.2830  0.5638  0.5574  11.00000  0.05    0.78
Q13   1   0.3260  0.7276  0.6614  11.00000  0.05    0.74
Q14   1   0.4177  0.5747  0.5015  11.00000  0.05    0.74
Q15   1   0.0456  0.8356  0.6749  11.00000  0.05    0.72
Q16   1   0.1899  0.6929  0.4946  11.00000  0.05    0.70
Q17   1   0.0657  0.8381  0.4846  11.00000  0.05    0.70
Q18   1   0.2786  0.6787  0.5724  11.00000  0.05    0.69
Q19   1   0.5153  0.3037  0.7360  11.00000  0.05    0.69
Q20   1   0.1904  0.6294  0.6364  11.00000  0.05    0.68
;
_shelx_res_checksum              54134
_olex2_exptl_crystal_mounting_method Mounted
_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 2.063
_oxdiff_exptl_absorpt_empirical_full_min 0.314
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_(wscl3)(mes(ch2)2sme)
_database_code_depnum_ccdc_archive 'CCDC 1949965'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton 
United Kingdom
;
_audit_update_record             
;
2019-08-28 deposited with the CCDC.	2020-01-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_(wscl3)(mes(ch2)2sme) 
;
PROBLEM: Check Calcd Resid. Dens.  1.19A   From Cl1             3.77 eA-3
RESPONSE: Residual density from tungsten - absorption correction issue.
;
# Added during the CSD deposition process: Wednesday 28 August 2019 03:14 PM
# end Validation Reply Form

_audit_creation_date             2019-08-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H10 Cl3 S3 W'
_chemical_formula_sum            'C4 H10 Cl3 S3 W'
_chemical_formula_weight         444.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         C4H10S3WCl4
_chemical_oxdiff_usercomment     'Red Block'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   6.87580(10)
_cell_length_b                   13.2588(2)
_cell_length_c                   12.5782(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.541(2)
_cell_angle_gamma                90
_cell_volume                     1143.09(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18262
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.8000
_cell_measurement_theta_min      2.2090
_shelx_estimated_absorpt_T_max   0.806
_shelx_estimated_absorpt_T_min   0.728
_exptl_absorpt_coefficient_mu    11.296
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.583
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_preparation       
'Slow evporation from (WSCl3)(MeS(CH2)2SMe) in DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from dcm.'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30189
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.187
_diffrn_reflns_theta_min         2.236
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -108.00  22.00   0.50    0.50    --  -18.80 -70.00 150.00  260
  2  ω    -59.00  71.00   0.50    0.50    --  -18.80  70.00  60.00  260
  3  ω   -108.00  22.00   0.50    0.50    --  -18.80 -70.00-120.00  260
  4  ω   -108.00  71.00   0.50    0.50    --  -18.80   0.00-180.00  358
  5  ω   -108.00  42.00   0.50    0.50    --  -18.80 -38.00 -90.00  300
  6  ω   -108.00  22.00   0.50    0.50    --  -18.80 -70.00  90.00  260
  7  ω    -56.00  -6.00   0.50    0.50    --  -18.80  57.00-150.00  100
  8  ω    -56.00  71.00   0.50    0.50    --  -18.80  57.00 -90.00  254
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0899380000
_diffrn_orient_matrix_UB_12      0.0152260000
_diffrn_orient_matrix_UB_13      0.0266961000
_diffrn_orient_matrix_UB_21      0.0196024000
_diffrn_orient_matrix_UB_22      -0.0506887000
_diffrn_orient_matrix_UB_23      0.0154511000
_diffrn_orient_matrix_UB_31      0.0471846000
_diffrn_orient_matrix_UB_32      -0.0079018000
_diffrn_orient_matrix_UB_33      -0.0474315000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3332
_reflns_number_total             3609
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.820
_refine_diff_density_min         -2.811
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         3609
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0391
_refine_ls_restrained_S_all      1.085
_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)+(0.0091P)²+13.7844P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0763
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(W1) = Uanis(W1A)
Uanis(Cl1A) = Uanis(S1)
Uanis(Cl1) = Uanis(S1A)
3. Others
 Fixed Sof: W1(0.75) Cl1(0.75) S1(0.75) Cl1A(0.25) S1A(0.25) W1A(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S2 S 0.15328(18) 0.33052(9) 0.31717(9) 0.0196(2) Uani 1 1 d . . . . .
S3 S 0.63382(19) 0.28679(10) 0.37384(9) 0.0245(2) Uani 1 1 d . . . . .
C3 C 0.4478(8) 0.2685(4) 0.4667(4) 0.0250(10) Uani 1 1 d . . . . .
H3A H 0.491271 0.216591 0.517528 0.030 Uiso 1 1 calc R . . . .
H3B H 0.432909 0.330512 0.506059 0.030 Uiso 1 1 calc R . . . .
C2 C 0.2509(8) 0.2383(4) 0.4132(4) 0.0249(10) Uani 1 1 d . . . . .
H2A H 0.159540 0.229261 0.467336 0.030 Uiso 1 1 calc R . . . .
H2B H 0.263790 0.174136 0.377377 0.030 Uiso 1 1 calc R . . . .
C1 C 0.0881(9) 0.4317(4) 0.4035(5) 0.0288(11) Uani 1 1 d . . . . .
H1A H 0.196328 0.446397 0.454074 0.043 Uiso 1 1 calc GR . . . .
H1B H -0.022260 0.411790 0.440787 0.043 Uiso 1 1 calc GR . . . .
H1C H 0.055527 0.490683 0.361565 0.043 Uiso 1 1 calc GR . . . .
C4 C 0.6866(11) 0.1590(5) 0.3371(5) 0.0396(15) Uani 1 1 d . . . . .
H4A H 0.746003 0.123867 0.398061 0.059 Uiso 1 1 calc GR . . . .
H4B H 0.774224 0.159352 0.281392 0.059 Uiso 1 1 calc GR . . . .
H4C H 0.567619 0.125602 0.312358 0.059 Uiso 1 1 calc GR . . . .
W1 W 0.48234(5) 0.38064(3) 0.21584(3) 0.02138(9) Uani 0.75 1 d . . P A 1
Cl2 Cl 0.38378(19) 0.22652(9) 0.13470(9) 0.0238(2) Uani 1 1 d . . . . .
Cl3 Cl 0.5067(2) 0.51691(10) 0.33554(11) 0.0349(3) Uani 1 1 d . . . . .
Cl1 Cl 0.2612(3) 0.46775(16) 0.10175(17) 0.0317(4) Uani 0.75 1 d . . P A 1
S1 S 0.7442(9) 0.4017(3) 0.1509(5) 0.0434(7) Uani 0.75 1 d . . P A 1
Cl1A Cl 0.724(3) 0.3816(12) 0.1636(16) 0.0434(7) Uani 0.25 1 d . . P A 2
S1A S 0.1833(12) 0.4643(6) 0.1147(7) 0.0317(4) Uani 0.25 1 d . . P A 2
W1A W 0.41958(19) 0.38700(13) 0.21242(13) 0.02138(9) Uani 0.25 1 d . . P A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S2 0.0234(6) 0.0176(5) 0.0183(5) -0.0016(4) 0.0035(4) -0.0010(4)
S3 0.0259(6) 0.0320(6) 0.0154(5) 0.0020(4) 0.0011(4) -0.0031(5)
C3 0.029(3) 0.031(2) 0.016(2) 0.0026(18) 0.0056(18) 0.000(2)
C2 0.031(3) 0.020(2) 0.024(2) 0.0050(18) 0.0053(19) -0.0004(19)
C1 0.033(3) 0.024(2) 0.032(3) -0.006(2) 0.011(2) 0.002(2)
C4 0.046(4) 0.043(3) 0.030(3) 0.005(3) 0.003(3) 0.022(3)
W1 0.0339(2) 0.01767(11) 0.01280(10) -0.00008(8) 0.00359(17) -0.00573(18)
Cl2 0.0308(6) 0.0197(5) 0.0202(5) -0.0046(4) -0.0015(4) -0.0008(4)
Cl3 0.0493(8) 0.0266(6) 0.0309(6) -0.0123(5) 0.0159(6) -0.0132(6)
Cl1 0.0434(14) 0.0226(6) 0.0288(9) 0.0034(6) 0.0014(10) 0.0065(10)
S1 0.0500(19) 0.037(2) 0.0457(19) -0.0060(15) 0.0185(12) -0.0106(15)
Cl1A 0.0500(19) 0.037(2) 0.0457(19) -0.0060(15) 0.0185(12) -0.0106(15)
S1A 0.0434(14) 0.0226(6) 0.0288(9) 0.0034(6) 0.0014(10) 0.0065(10)
W1A 0.0339(2) 0.01767(11) 0.01280(10) -0.00008(8) 0.00359(17) -0.00573(18)

_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
S2 C2 1.810(5) . ?
S2 C1 1.804(5) . ?
S2 W1 2.7644(13) . ?
S2 W1A 2.4560(19) . ?
S3 C3 1.815(5) . ?
S3 C4 1.801(7) . ?
S3 W1 2.5010(13) . ?
S3 W1A 2.754(2) . ?
C3 C2 1.517(8) . ?
W1 Cl2 2.3594(12) . ?
W1 Cl3 2.3494(13) . ?
W1 Cl1 2.315(2) . ?
W1 S1 2.054(5) . ?
Cl2 W1A 2.346(2) . ?
Cl3 W1A 2.361(2) . ?
Cl1A W1A 2.23(2) . ?
S1A W1A 2.209(8) . ?

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
C2 S2 W1 101.31(18) . . ?
C2 S2 W1A 108.13(19) . . ?
C1 S2 C2 101.4(3) . . ?
C1 S2 W1 110.50(19) . . ?
C1 S2 W1A 109.1(2) . . ?
C3 S3 W1 107.91(18) . . ?
C3 S3 W1A 100.14(18) . . ?
C4 S3 C3 101.9(3) . . ?
C4 S3 W1 110.1(2) . . ?
C4 S3 W1A 111.8(2) . . ?
C2 C3 S3 113.5(3) . . ?
C3 C2 S2 112.9(4) . . ?
S3 W1 S2 79.55(4) . . ?
Cl2 W1 S2 76.92(4) . . ?
Cl2 W1 S3 90.01(4) . . ?
Cl3 W1 S2 84.76(4) . . ?
Cl3 W1 S3 82.49(5) . . ?
Cl3 W1 Cl2 161.21(5) . . ?
Cl1 W1 S2 83.36(6) . . ?
Cl1 W1 S3 162.28(7) . . ?
Cl1 W1 Cl2 90.69(6) . . ?
Cl1 W1 Cl3 91.34(7) . . ?
S1 W1 S2 172.37(16) . . ?
S1 W1 S3 93.48(18) . . ?
S1 W1 Cl2 100.16(15) . . ?
S1 W1 Cl3 97.49(16) . . ?
S1 W1 Cl1 103.82(18) . . ?
S2 W1A S3 80.52(6) . . ?
Cl2 W1A S2 83.62(7) . . ?
Cl2 W1A S3 84.37(6) . . ?
Cl2 W1A Cl3 161.34(9) . . ?
Cl3 W1A S2 91.81(7) . . ?
Cl3 W1A S3 77.02(7) . . ?
Cl1A W1A S2 153.4(5) . . ?
Cl1A W1A S3 74.3(5) . . ?
Cl1A W1A Cl2 85.8(5) . . ?
Cl1A W1A Cl3 90.5(5) . . ?
S1A W1A S2 83.9(2) . . ?
S1A W1A S3 163.8(2) . . ?
S1A W1A Cl2 98.1(2) . . ?
S1A W1A Cl3 99.4(2) . . ?
S1A W1A Cl1A 121.8(6) . . ?

_shelx_res_file                  
;
TITL dsex79-2_a.res in P2(1)/n
    (wscl3)(mes(ch2)2sme).res
    created by SHELXL-2018/3 at 12:03:13 on 20-Aug-2019
REM Old TITL DS Ex79 - 2 in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.220, Rweak 0.011, Alpha 0.031
REM <I/s> 1.423 for 112 systematic absences, Orientation as input
REM Formula found by SHELXT: C4 S2 Cl1 W
CELL 0.71073 6.8758 13.2588 12.5782 90 94.541 90
ZERR 4 0.0001 0.0002 0.0002 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cl S W
UNIT 16 40 12 12 4
EADP W1 W1A
EADP Cl1A S1
EADP Cl1 S1A

L.S. 10
PLAN  20
SIZE 0.02 0.03 0.02
BOND
LIST 6
fmap 2
acta
OMIT -4 5 2
OMIT 8 0 0
OMIT 1 0 1
OMIT 2 0 0
OMIT -4 1 1
OMIT 1 2 0
OMIT 7 9 3
OMIT -3 0 5
OMIT 2 5 3
OMIT 8 6 3
OMIT 8 4 4
OMIT -4 5 3
OMIT 1 1 2
OMIT 2 1 1
OMIT -6 9 4
OMIT 0 2 1
OMIT -5 0 1
OMIT -3 1 6
OMIT -2 2 4
OMIT -4 0 6
OMIT 8 0 2
OMIT -4 1 2
OMIT 0 4 0
OMIT 2 2 1
OMIT -5 4 3
OMIT -1 5 2
OMIT -1 3 1
OMIT 6 6 3
OMIT 7 11 2
OMIT 2 2 0
OMIT -7 4 3
OMIT -9 4 7
OMIT 1 2 1
OMIT -2 1 5
OMIT -9 4 1
OMIT -5 14 6
OMIT -2 2 1
OMIT 7 13 1
OMIT 8 10 1
OMIT -1 1 4
OMIT 8 4 2
OMIT 7 0 1
OMIT -1 1 8
OMIT 0 0 2
OMIT -8 5 4
OMIT -4 0 16
OMIT 7 1 2
OMIT -2 0 6
OMIT -1 0 1
OMIT 2 3 2
OMIT -4 2 5
OMIT -7 5 4
REM <olex2.extras>
REM <HklSrc "%.\\(WSCl3)(MeS(CH2)2SMe).hkl">
REM </olex2.extras>

WGHT    0.009100   13.784399
FVAR       0.26587
S2    4    0.153279    0.330519    0.317175    11.00000    0.02339    0.01756 =
         0.01827   -0.00157    0.00346   -0.00097
S3    4    0.633816    0.286791    0.373841    11.00000    0.02590    0.03200 =
         0.01542    0.00203    0.00107   -0.00309
C3    1    0.447823    0.268455    0.466681    11.00000    0.02903    0.03108 =
         0.01559    0.00259    0.00560   -0.00006
AFIX  23
H3A   2    0.491271    0.216591    0.517528    11.00000   -1.20000
H3B   2    0.432909    0.330512    0.506059    11.00000   -1.20000
AFIX   0
C2    1    0.250885    0.238314    0.413166    11.00000    0.03095    0.02040 =
         0.02378    0.00505    0.00531   -0.00043
AFIX  23
H2A   2    0.159540    0.229261    0.467336    11.00000   -1.20000
H2B   2    0.263790    0.174136    0.377377    11.00000   -1.20000
AFIX   0
C1    1    0.088092    0.431683    0.403500    11.00000    0.03256    0.02362 =
         0.03175   -0.00585    0.01127    0.00165
AFIX 137
H1A   2    0.196328    0.446397    0.454074    11.00000   -1.50000
H1B   2   -0.022260    0.411790    0.440787    11.00000   -1.50000
H1C   2    0.055527    0.490683    0.361565    11.00000   -1.50000
AFIX   0
C4    1    0.686574    0.158985    0.337128    11.00000    0.04552    0.04317 =
         0.02997    0.00468    0.00269    0.02152
AFIX 137
H4A   2    0.746003    0.123867    0.398061    11.00000   -1.50000
H4B   2    0.774224    0.159352    0.281392    11.00000   -1.50000
H4C   2    0.567619    0.125602    0.312358    11.00000   -1.50000
AFIX   0
PART 1
W1    5    0.482341    0.380636    0.215836    10.75000    0.03394    0.01767 =
         0.01280   -0.00008    0.00359   -0.00573
PART 0
CL2   3    0.383784    0.226522    0.134701    11.00000    0.03085    0.01973 =
         0.02020   -0.00463   -0.00147   -0.00083
CL3   3    0.506652    0.516911    0.335539    11.00000    0.04931    0.02660 =
         0.03095   -0.01227    0.01591   -0.01323
PART 1
CL1   3    0.261236    0.467752    0.101752    10.75000    0.04342    0.02259 =
         0.02884    0.00344    0.00143    0.00653
S1    4    0.744203    0.401691    0.150868    10.75000    0.05005    0.03665 =
         0.04571   -0.00602    0.01851   -0.01056
PART 0
PART 2
CL1A  3    0.723771    0.381627    0.163583    10.25000    0.05005    0.03665 =
         0.04571   -0.00602    0.01851   -0.01056
S1A   4    0.183334    0.464273    0.114732    10.25000    0.04342    0.02259 =
         0.02884    0.00344    0.00143    0.00653
W1A   5    0.419581    0.387004    0.212416    10.25000    0.03394    0.01767 =
         0.01280   -0.00008    0.00359   -0.00573
HKLF 4




REM  dsex79-2_a.res in P2(1)/n
REM wR2 = 0.0763, GooF = S = 1.085, Restrained GooF = 1.085 for all data
REM R1 = 0.0391 for 3332 Fo > 4sig(Fo) and 0.0432 for all 3609 data
REM 111 parameters refined using 0 restraints

END

WGHT      0.0091     13.7844

REM Highest difference peak  3.820,  deepest hole -2.811,  1-sigma level  0.192
Q1    1   0.4142  0.4841  0.0574  11.00000  0.05    3.82
Q2    1   0.4240  0.4110  0.2315  11.00000  0.05    2.99
Q3    1   0.3906  0.3595  0.1944  11.00000  0.05    2.96
Q4    1   0.1076  0.4598  0.1306  11.00000  0.05    1.41
Q5    1   0.5115  0.3544  0.2363  11.00000  0.05    1.02
Q6    1   0.6452  0.3582  0.1932  11.00000  0.05    0.83
Q7    1   0.5642  0.4563  0.0648  11.00000  0.05    0.71
Q8    1   0.2693  0.3986  0.1702  11.00000  0.05    0.70
Q9    1   0.6112  0.4193  0.3353  11.00000  0.05    0.69
Q10   1   0.5599  0.4475  0.2435  11.00000  0.05    0.62
Q11   1   0.2975  0.4434  0.2277  11.00000  0.05    0.60
Q12   1   0.6217  0.2381  0.3842  11.00000  0.05    0.59
Q13   1   0.2526  0.4782  0.1750  11.00000  0.05    0.57
Q14   1   0.6642  0.3771  0.2241  11.00000  0.05    0.57
Q15   1   0.5935  0.3175  0.2332  11.00000  0.05    0.55
Q16   1   0.7120  0.3323  0.1397  11.00000  0.05    0.55
Q17   1   0.7278  0.4386  0.2196  11.00000  0.05    0.54
Q18   1   0.6401  0.3644  0.3795  11.00000  0.05    0.53
Q19   1   0.4400  0.4679  0.3048  11.00000  0.05    0.53
Q20   1   0.6301  0.4108  0.2038  11.00000  0.05    0.52
;
_shelx_res_checksum              30040
_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 1.815
_oxdiff_exptl_absorpt_empirical_full_min 0.701
