# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_mo_ZL215F2_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1401809'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 Thienyl[2,3-b]thiophenene-2,5-di[(ethoxycarbene)pentacarbonyltungsten(0)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H12 O12 S2 W2'
_chemical_formula_sum            'C22 H12 O12 S2 W2'
_chemical_formula_weight         900.14

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_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                   13.1323(5)
_cell_length_b                   14.6364(6)
_cell_length_c                   13.8925(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.4568(11)
_cell_angle_gamma                90
_cell_volume                     2658.17(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9718
_cell_measurement_theta_min      2.469
_cell_measurement_theta_max      34.985

_exptl_crystal_description       parallelopipped
_exptl_crystal_colour            red
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.249
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.042
_exptl_absorpt_coefficient_mu    8.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1464
_exptl_absorpt_correction_T_max  0.2720
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ' I\mS  micro focus'
_diffrn_radiation_monochromator  'Focusing Montel optics'
_diffrn_measurement_device_type  'Bruker kappa Photon CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            122480
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.469
_diffrn_reflns_theta_max         35.060
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11750
_reflns_number_gt                9579
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTS (Sheldrick, 2014)'
_computing_structure_refinement  Bruker
_computing_molecular_graphics    
;
 ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
 Mercury (Macrae et al., 2008)
;
_computing_publication_material  'SHELXL-2014, PLATON (Spek, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0219P)²+4.4584P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic-phasing
_atom_sites_solution_secondary   .
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11750
_refine_ls_number_parameters     345
_refine_ls_number_restraints     315
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0556
_refine_ls_wR_factor_gt          0.0503
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

_refine_diff_density_max         2.470
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.169

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 1.07619(2) 0.49418(2) 0.30777(2) 0.01784(2) Uani 1 1 d . U . . .
C1 C 1.12028(19) 0.56534(18) 0.4289(2) 0.0222(5) Uani 1 1 d . U . . .
O1 O 1.14349(17) 0.60185(15) 0.50110(15) 0.0295(4) Uani 1 1 d . U . . .
C2 C 1.2275(2) 0.4737(2) 0.2898(2) 0.0259(5) Uani 1 1 d . U . . .
O2 O 1.31307(16) 0.4678(2) 0.28291(17) 0.0405(6) Uani 1 1 d . U . . .
C3 C 1.0752(2) 0.37997(19) 0.3938(2) 0.0256(5) Uani 1 1 d . U . . .
O3 O 1.0763(2) 0.31775(16) 0.44249(19) 0.0414(6) Uani 1 1 d . U . . .
C4 C 0.9307(2) 0.5316(2) 0.3293(2) 0.0268(5) Uani 1 1 d . U . . .
O4 O 0.85107(17) 0.55682(18) 0.3417(2) 0.0433(6) Uani 1 1 d . U . . .
C5 C 1.0756(2) 0.60439(19) 0.2177(2) 0.0260(5) Uani 1 1 d . U . . .
O5 O 1.0719(2) 0.66362(16) 0.16462(17) 0.0407(6) Uani 1 1 d . U . . .
C6 C 1.01487(18) 0.40991(17) 0.18486(18) 0.0189(4) Uani 1 1 d . U . . .
O6 O 1.04952(14) 0.39779(14) 0.09921(14) 0.0253(4) Uani 1 1 d . U . . .
W2 W 0.45622(2) 0.16447(2) 0.35752(2) 0.02049(3) Uani 1 1 d . U . . .
C7 C 0.4121(2) 0.1670(2) 0.4933(2) 0.0327(6) Uani 1 1 d . U . . .
O7 O 0.3894(2) 0.1691(2) 0.57086(19) 0.0540(8) Uani 1 1 d . U . . .
C8 C 0.4070(2) 0.0322(2) 0.3454(2) 0.0315(6) Uani 1 1 d . U . . .
O8 O 0.3789(2) -0.04148(18) 0.3433(2) 0.0531(7) Uani 1 1 d . U . . .
C9 C 0.5947(2) 0.1137(2) 0.4113(2) 0.0269(5) Uani 1 1 d . U . . .
O9 O 0.67141(18) 0.08330(18) 0.43970(18) 0.0406(5) Uani 1 1 d . U . . .
C10 C 0.4998(2) 0.2983(2) 0.3703(2) 0.0252(5) Uani 1 1 d . U . . .
O10 O 0.52340(18) 0.37295(16) 0.37551(18) 0.0374(5) Uani 1 1 d . U . . .
C11 C 0.3141(2) 0.2106(2) 0.3058(2) 0.0314(6) Uani 1 1 d . U . . .
O11 O 0.23450(18) 0.2370(2) 0.2810(2) 0.0504(7) Uani 1 1 d . U . . .
C12 C 0.51977(18) 0.16682(17) 0.21685(18) 0.0189(4) Uani 1 1 d . U . . .
O12 O 0.48215(13) 0.13319(14) 0.13293(13) 0.0229(4) Uani 1 1 d . U . . .
S1 S 0.86859(5) 0.31059(5) 0.07111(5) 0.02373(12) Uani 1 1 d . U . . .
S2 S 0.65991(5) 0.20860(5) 0.08461(5) 0.02214(12) Uani 1 1 d . U . . .
C13 C 0.91898(17) 0.35910(17) 0.18187(17) 0.0180(4) Uani 1 1 d . U . . .
C14 C 0.85839(18) 0.34210(17) 0.25456(18) 0.0200(4) Uani 1 1 d . U . . .
H14 H 0.8735 0.3629 0.3191 0.024 Uiso 1 1 calc R U . . .
C15 C 0.77074(17) 0.29003(17) 0.22309(17) 0.0175(4) Uani 1 1 d . U . . .
C16 C 0.76620(18) 0.26964(17) 0.12511(18) 0.0191(4) Uani 1 1 d . U . . .
C17 C 0.68615(18) 0.25402(18) 0.26613(18) 0.0198(4) Uani 1 1 d . U . . .
H17 H 0.6774 0.2601 0.3329 0.024 Uiso 1 1 calc R U . . .
C18 C 0.61754(18) 0.20915(17) 0.20131(17) 0.0182(4) Uani 1 1 d . U . . .
C19 C 1.1453(2) 0.4365(2) 0.0745(2) 0.0303(6) Uani 1 1 d . U . . .
H19A H 1.2037 0.4070 0.1128 0.036 Uiso 1 1 calc R U . . .
H19B H 1.1474 0.5029 0.0884 0.036 Uiso 1 1 calc R U . . .
C20 C 1.1513(2) 0.4200(2) -0.0312(2) 0.0280(6) Uani 1 1 d . U . . .
H20A H 1.0947 0.4516 -0.0684 0.042 Uiso 1 1 calc R U . . .
H20B H 1.1467 0.3543 -0.0444 0.042 Uiso 1 1 calc R U . . .
H20C H 1.2165 0.4434 -0.0499 0.042 Uiso 1 1 calc R U . . .
C21 C 0.3823(2) 0.0885(2) 0.1234(2) 0.0294(6) Uani 1 1 d . U . . .
H21A H 0.3304 0.1289 0.1484 0.035 Uiso 1 1 calc R U . . .
H21B H 0.3853 0.0310 0.1611 0.035 Uiso 1 1 calc R U . . .
C22 C 0.3539(2) 0.0686(3) 0.0189(2) 0.0368(7) Uani 1 1 d . U . . .
H22A H 0.3454 0.1262 -0.0170 0.055 Uiso 1 1 calc R U . . .
H22B H 0.2896 0.0343 0.0117 0.055 Uiso 1 1 calc R U . . .
H22C H 0.4081 0.0323 -0.0065 0.055 Uiso 1 1 calc R U . . .


_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 C1 2.017(3) . ?
W1 C4 2.036(3) . ?
W1 C5 2.041(3) . ?
W1 C2 2.049(3) . ?
W1 C3 2.055(3) . ?
W1 C6 2.196(3) . ?
C1 O1 1.151(3) . ?
C2 O2 1.140(3) . ?
C3 O3 1.134(4) . ?
C4 O4 1.138(3) . ?
C5 O5 1.136(4) . ?
C6 O6 1.326(3) . ?
C6 C13 1.460(3) . ?
O6 C19 1.451(3) . ?
W2 C7 2.026(3) . ?
W2 C9 2.040(3) . ?
W2 C10 2.043(3) . ?
W2 C8 2.043(3) . ?
W2 C11 2.050(3) . ?
W2 C12 2.197(2) . ?
C7 O7 1.145(4) . ?
C8 O8 1.139(4) . ?
C9 O9 1.137(4) . ?
C10 O10 1.136(4) . ?
C11 O11 1.137(4) . ?
C12 O12 1.318(3) . ?
C12 C18 1.460(3) . ?
O12 C21 1.460(3) . ?
S1 C16 1.709(2) . ?
S1 C13 1.765(2) . ?
S2 C16 1.707(2) . ?
S2 C18 1.763(2) . ?
C13 C14 1.367(3) . ?
C14 C15 1.415(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(3) . ?
C15 C17 1.413(3) . ?
C17 C18 1.378(3) . ?
C17 H17 0.9500 . ?
C19 C20 1.497(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.492(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W1 C4 86.40(11) . . ?
C1 W1 C5 95.02(10) . . ?
C4 W1 C5 85.92(12) . . ?
C1 W1 C2 88.43(11) . . ?
C4 W1 C2 172.63(12) . . ?
C5 W1 C2 89.31(12) . . ?
C1 W1 C3 87.25(11) . . ?
C4 W1 C3 94.33(11) . . ?
C5 W1 C3 177.72(11) . . ?
C2 W1 C3 90.66(11) . . ?
C1 W1 C6 173.59(9) . . ?
C4 W1 C6 89.18(11) . . ?
C5 W1 C6 89.28(10) . . ?
C2 W1 C6 96.38(10) . . ?
C3 W1 C6 88.46(10) . . ?
O1 C1 W1 176.1(2) . . ?
O2 C2 W1 175.4(3) . . ?
O3 C3 W1 178.5(3) . . ?
O4 C4 W1 176.7(3) . . ?
O5 C5 W1 176.7(2) . . ?
O6 C6 C13 106.0(2) . . ?
O6 C6 W1 129.88(17) . . ?
C13 C6 W1 124.04(17) . . ?
C6 O6 C19 122.7(2) . . ?
C7 W2 C9 89.37(12) . . ?
C7 W2 C10 90.25(12) . . ?
C9 W2 C10 94.87(11) . . ?
C7 W2 C8 88.70(12) . . ?
C9 W2 C8 87.08(13) . . ?
C10 W2 C8 177.78(12) . . ?
C7 W2 C11 89.39(13) . . ?
C9 W2 C11 177.51(12) . . ?
C10 W2 C11 87.30(12) . . ?
C8 W2 C11 90.73(13) . . ?
C7 W2 C12 173.99(10) . . ?
C9 W2 C12 86.04(10) . . ?
C10 W2 C12 86.29(10) . . ?
C8 W2 C12 94.92(10) . . ?
C11 W2 C12 95.34(11) . . ?
O7 C7 W2 178.4(3) . . ?
O8 C8 W2 176.8(3) . . ?
O9 C9 W2 178.1(3) . . ?
O10 C10 W2 178.6(3) . . ?
O11 C11 W2 177.1(3) . . ?
O12 C12 C18 106.8(2) . . ?
O12 C12 W2 129.72(17) . . ?
C18 C12 W2 123.50(17) . . ?
C12 O12 C21 120.4(2) . . ?
C16 S1 C13 90.22(12) . . ?
C16 S2 C18 90.82(11) . . ?
C14 C13 C6 129.3(2) . . ?
C14 C13 S1 111.99(17) . . ?
C6 C13 S1 118.73(18) . . ?
C13 C14 C15 112.5(2) . . ?
C13 C14 H14 123.7 . . ?
C15 C14 H14 123.7 . . ?
C16 C15 C17 111.9(2) . . ?
C16 C15 C14 112.1(2) . . ?
C17 C15 C14 136.0(2) . . ?
C15 C16 S2 113.14(18) . . ?
C15 C16 S1 113.10(18) . . ?
S2 C16 S1 133.76(15) . . ?
C18 C17 C15 113.1(2) . . ?
C18 C17 H17 123.4 . . ?
C15 C17 H17 123.4 . . ?
C17 C18 C12 129.4(2) . . ?
C17 C18 S2 111.04(17) . . ?
C12 C18 S2 119.53(18) . . ?
O6 C19 C20 107.3(2) . . ?
O6 C19 H19A 110.3 . . ?
C20 C19 H19A 110.3 . . ?
O6 C19 H19B 110.3 . . ?
C20 C19 H19B 110.3 . . ?
H19A C19 H19B 108.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O12 C21 C22 108.4(2) . . ?
O12 C21 H21A 110.0 . . ?
C22 C21 H21A 110.0 . . ?
O12 C21 H21B 110.0 . . ?
C22 C21 H21B 110.0 . . ?
H21A C21 H21B 108.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 C6 O6 C19 -178.7(2) . . . . ?
W1 C6 O6 C19 5.0(4) . . . . ?
C18 C12 O12 C21 -178.0(2) . . . . ?
W2 C12 O12 C21 2.0(4) . . . . ?
O6 C6 C13 C14 172.8(3) . . . . ?
W1 C6 C13 C14 -10.6(4) . . . . ?
O6 C6 C13 S1 -7.3(3) . . . . ?
W1 C6 C13 S1 169.24(13) . . . . ?
C16 S1 C13 C14 0.7(2) . . . . ?
C16 S1 C13 C6 -179.2(2) . . . . ?
C6 C13 C14 C15 179.9(2) . . . . ?
S1 C13 C14 C15 0.0(3) . . . . ?
C13 C14 C15 C16 -0.9(3) . . . . ?
C13 C14 C15 C17 179.6(3) . . . . ?
C17 C15 C16 S2 0.7(3) . . . . ?
C14 C15 C16 S2 -178.86(18) . . . . ?
C17 C15 C16 S1 -178.96(18) . . . . ?
C14 C15 C16 S1 1.4(3) . . . . ?
C18 S2 C16 C15 0.1(2) . . . . ?
C18 S2 C16 S1 179.7(2) . . . . ?
C13 S1 C16 C15 -1.2(2) . . . . ?
C13 S1 C16 S2 179.2(2) . . . . ?
C16 C15 C17 C18 -1.5(3) . . . . ?
C14 C15 C17 C18 177.9(3) . . . . ?
C15 C17 C18 C12 -177.0(2) . . . . ?
C15 C17 C18 S2 1.6(3) . . . . ?
O12 C12 C18 C17 179.6(3) . . . . ?
W2 C12 C18 C17 -0.4(4) . . . . ?
O12 C12 C18 S2 1.1(3) . . . . ?
W2 C12 C18 S2 -178.91(12) . . . . ?
C16 S2 C18 C17 -1.0(2) . . . . ?
C16 S2 C18 C12 177.8(2) . . . . ?
C6 O6 C19 C20 -172.0(2) . . . . ?
C12 O12 C21 C22 172.7(3) . . . . ?

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane, DCM'
####################################################################### 
# 
# 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_mo_ZL220F22_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1401810'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
'Thienyl[2,3-b]thiophenene-2,5-di[(ethoxycarbene)pentacarbonylchromium(0)], Thienyl[2,3-b]thiophenene-2-[(ethoxycarbene)pentacarbonylchromium(0)]-5-[(ethoxycarbene)pentacarbonyltungsten(0)] co-crystal'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'0.38(C22 H12 Cr2 O12 S2), 0.62(C22 H12 Cr O12 S2 W)'
_chemical_formula_sum            'C22 H12 Cr1.38 O12 S2 W0.62'
_chemical_formula_weight         717.85

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'
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'
Cr Cr 0.3209 0.6236 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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                   13.0556(8)
_cell_length_b                   14.5145(10)
_cell_length_c                   13.8325(9)
_cell_angle_alpha                90
_cell_angle_beta                 95.3950(18)
_cell_angle_gamma                90
_cell_volume                     2609.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9529
_cell_measurement_theta_min      2.485
_cell_measurement_theta_max      28.357

_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.057
_exptl_absorpt_coefficient_mu    3.517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5058
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ' I\mS  micro focus'
_diffrn_radiation_monochromator  'Focusing Montel optics'
_diffrn_measurement_device_type  'Bruker kappa Photon CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            98242
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.485
_diffrn_reflns_theta_max         28.363
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6523
_reflns_number_gt                5789
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTS (Sheldrick, 2014)'
_computing_structure_refinement  Bruker
_computing_molecular_graphics    
;
 ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
 Mercury (Macrae et al., 2008)
;
_computing_publication_material  'SHELXL-2014, PLATON (Spek, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0206P)²+4.0832P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic-phasing
_atom_sites_solution_secondary   .
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6523
_refine_ls_number_parameters     347
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0659
_refine_ls_wR_factor_gt          0.0626
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

_refine_diff_density_max         0.606
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.096

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
Cr1 Cr 1.07717(2) 0.49381(2) 0.30742(2) 0.01723(7) Uani 0.6799(13) 1 d . . P .
.
W1 W 1.07717(2) 0.49381(2) 0.30742(2) 0.01723(7) Uani 0.3201(13) 1 d . . P . .
C1 C 1.1186(2) 0.56209(18) 0.4227(2) 0.0254(5) Uani 1 1 d . . . . .
O1 O 1.14058(16) 0.59903(14) 0.49475(15) 0.0339(5) Uani 1 1 d . . . . .
C2 C 1.2216(2) 0.4734(2) 0.2904(2) 0.0284(6) Uani 1 1 d . . . . .
O2 O 1.30767(16) 0.46759(18) 0.28530(16) 0.0439(6) Uani 1 1 d . . . . .
C3 C 1.0747(2) 0.38253(19) 0.3888(2) 0.0270(6) Uani 1 1 d . . . . .
O3 O 1.07629(18) 0.31970(15) 0.43717(18) 0.0420(5) Uani 1 1 d . . . . .
C4 C 0.9363(2) 0.53008(19) 0.3283(2) 0.0282(6) Uani 1 1 d . . . . .
O4 O 0.85801(16) 0.55777(16) 0.34188(19) 0.0443(6) Uani 1 1 d . . . . .
C5 C 1.0757(2) 0.59874(19) 0.2198(2) 0.0278(6) Uani 1 1 d . . . . .
O5 O 1.07247(19) 0.65891(15) 0.16680(17) 0.0417(5) Uani 1 1 d . . . . .
C6 C 1.01666(18) 0.41155(17) 0.18874(18) 0.0200(5) Uani 1 1 d . . . . .
O6 O 1.05113(13) 0.39813(13) 0.10275(14) 0.0266(4) Uani 1 1 d . . . . .
Cr2 Cr 0.45611(2) 0.16382(2) 0.35822(2) 0.01916(8) Uani 0.7027(13) 1 d . . P .
.
W2 W 0.45611(2) 0.16382(2) 0.35822(2) 0.01916(8) Uani 0.2973(13) 1 d . . P . .
C7 C 0.4157(2) 0.1653(2) 0.4879(2) 0.0370(7) Uani 1 1 d . . . . .
O7 O 0.3924(2) 0.1671(2) 0.56567(18) 0.0554(7) Uani 1 1 d . . . . .
C8 C 0.4106(2) 0.0354(2) 0.3463(2) 0.0331(6) Uani 1 1 d . . . . .
O8 O 0.3829(2) -0.03872(17) 0.34573(18) 0.0531(7) Uani 1 1 d . . . . .
C9 C 0.5904(2) 0.11507(19) 0.4095(2) 0.0265(5) Uani 1 1 d . . . . .
O9 O 0.66709(17) 0.08432(16) 0.43881(16) 0.0396(5) Uani 1 1 d . . . . .
C10 C 0.4970(2) 0.2919(2) 0.3705(2) 0.0279(6) Uani 1 1 d . . . . .
O10 O 0.51820(17) 0.36795(15) 0.37693(17) 0.0399(5) Uani 1 1 d . . . . .
C11 C 0.3216(2) 0.2077(2) 0.3074(2) 0.0340(6) Uani 1 1 d . . . . .
O11 O 0.24204(18) 0.23514(19) 0.2832(2) 0.0531(7) Uani 1 1 d . . . . .
C12 C 0.51828(18) 0.16595(16) 0.22205(18) 0.0193(5) Uani 1 1 d . . . . .
S1 S 0.86850(5) 0.31202(5) 0.07415(5) 0.02501(15) Uani 1 1 d . . . . .
S2 S 0.65834(5) 0.20934(5) 0.08817(5) 0.02340(15) Uani 1 1 d . . . . .
O12 O 0.48084(13) 0.13229(13) 0.13745(13) 0.0247(4) Uani 1 1 d . . . . .
C13 C 0.91969(18) 0.36082(17) 0.18567(18) 0.0200(5) Uani 1 1 d . . . . .
C14 C 0.85840(18) 0.34353(17) 0.25847(18) 0.0201(5) Uani 1 1 d . . . . .
H14 H 0.8733 0.3644 0.3233 0.024 Uiso 1 1 calc R U . . .
C15 C 0.77027(18) 0.29107(16) 0.22660(18) 0.0191(5) Uani 1 1 d . . . . .
C16 C 0.76554(18) 0.27103(17) 0.12848(18) 0.0198(5) Uani 1 1 d . . . . .
C17 C 0.68505(18) 0.25464(17) 0.27035(18) 0.0210(5) Uani 1 1 d . . . . .
H17 H 0.6764 0.2610 0.3375 0.025 Uiso 1 1 calc R U . . .
C18 C 0.61661(18) 0.20956(16) 0.20623(18) 0.0189(5) Uani 1 1 d . . . . .
C19 C 1.1485(2) 0.4356(2) 0.0767(2) 0.0318(6) Uani 1 1 d . . . . .
H19A H 1.2069 0.4041 0.1135 0.038 Uiso 1 1 calc R U . . .
H19B H 1.1528 0.5023 0.0916 0.038 Uiso 1 1 calc R U . . .
C20 C 1.1514(2) 0.4201(2) -0.0298(2) 0.0292(6) Uani 1 1 d . . . . .
H20A H 1.2176 0.4414 -0.0497 0.044 Uiso 1 1 calc R U . . .
H20B H 1.0954 0.4545 -0.0656 0.044 Uiso 1 1 calc R U . . .
H20C H 1.1433 0.3542 -0.0441 0.044 Uiso 1 1 calc R U . . .
C21 C 0.3822(2) 0.0845(2) 0.1271(2) 0.0334(7) Uani 1 1 d . . . . .
H21A H 0.3290 0.1226 0.1544 0.040 Uiso 1 1 calc R U . . .
H21B H 0.3878 0.0253 0.1628 0.040 Uiso 1 1 calc R U . . .
C22 C 0.3531(2) 0.0673(3) 0.0222(2) 0.0429(8) Uani 1 1 d . . . . .
H22A H 0.2898 0.0306 0.0145 0.064 Uiso 1 1 calc R U . . .
H22B H 0.4086 0.0338 -0.0054 0.064 Uiso 1 1 calc R U . . .
H22C H 0.3415 0.1263 -0.0116 0.064 Uiso 1 1 calc R U . . .


_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
Cr1 C1 1.911(3) . ?
Cr1 C5 1.945(3) . ?
Cr1 C2 1.945(3) . ?
Cr1 C4 1.960(3) . ?
Cr1 C3 1.971(3) . ?
Cr1 C6 2.122(2) . ?
C1 O1 1.145(3) . ?
C2 O2 1.135(3) . ?
C3 O3 1.130(3) . ?
C4 O4 1.130(3) . ?
C5 O5 1.139(3) . ?
C6 O6 1.325(3) . ?
C6 C13 1.462(3) . ?
O6 C19 1.459(3) . ?
Cr2 C7 1.917(3) . ?
Cr2 C11 1.937(3) . ?
Cr2 C10 1.937(3) . ?
Cr2 C8 1.959(3) . ?
Cr2 C9 1.961(3) . ?
Cr2 C12 2.120(2) . ?
C7 O7 1.145(4) . ?
C8 O8 1.135(4) . ?
C9 O9 1.135(3) . ?
C10 O10 1.139(4) . ?
C11 O11 1.134(4) . ?
C12 O12 1.319(3) . ?
C12 C18 1.466(3) . ?
S1 C16 1.707(2) . ?
S1 C13 1.770(3) . ?
S2 C16 1.710(2) . ?
S2 C18 1.769(2) . ?
O12 C21 1.458(3) . ?
C13 C14 1.367(3) . ?
C14 C15 1.415(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.384(3) . ?
C15 C17 1.418(3) . ?
C17 C18 1.365(3) . ?
C17 H17 0.9500 . ?
C19 C20 1.495(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.485(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Cr1 C5 95.68(11) . . ?
C1 Cr1 C2 88.78(11) . . ?
C5 Cr1 C2 89.78(12) . . ?
C1 Cr1 C4 86.20(11) . . ?
C5 Cr1 C4 85.83(12) . . ?
C2 Cr1 C4 172.97(12) . . ?
C1 Cr1 C3 88.12(11) . . ?
C5 Cr1 C3 176.17(11) . . ?
C2 Cr1 C3 90.74(11) . . ?
C4 Cr1 C3 94.01(11) . . ?
C1 Cr1 C6 173.07(10) . . ?
C5 Cr1 C6 88.71(10) . . ?
C2 Cr1 C6 96.62(10) . . ?
C4 Cr1 C6 88.78(11) . . ?
C3 Cr1 C6 87.46(10) . . ?
O1 C1 Cr1 175.9(2) . . ?
O2 C2 Cr1 174.3(3) . . ?
O3 C3 Cr1 177.6(3) . . ?
O4 C4 Cr1 174.6(3) . . ?
O5 C5 Cr1 177.9(2) . . ?
O6 C6 C13 105.4(2) . . ?
O6 C6 Cr1 130.10(17) . . ?
C13 C6 Cr1 124.37(17) . . ?
C6 O6 C19 123.0(2) . . ?
C7 Cr2 C11 90.94(13) . . ?
C7 Cr2 C10 90.29(12) . . ?
C11 Cr2 C10 87.09(12) . . ?
C7 Cr2 C8 88.93(12) . . ?
C11 Cr2 C8 91.44(13) . . ?
C10 Cr2 C8 178.33(12) . . ?
C7 Cr2 C9 88.89(13) . . ?
C11 Cr2 C9 178.04(12) . . ?
C10 Cr2 C9 94.86(11) . . ?
C8 Cr2 C9 86.60(12) . . ?
C7 Cr2 C12 173.32(11) . . ?
C11 Cr2 C12 94.73(11) . . ?
C10 Cr2 C12 86.47(10) . . ?
C8 Cr2 C12 94.45(10) . . ?
C9 Cr2 C12 85.58(10) . . ?
O7 C7 Cr2 179.2(3) . . ?
O8 C8 Cr2 175.4(3) . . ?
O9 C9 Cr2 178.0(2) . . ?
O10 C10 Cr2 178.0(3) . . ?
O11 C11 Cr2 175.8(3) . . ?
O12 C12 C18 106.5(2) . . ?
O12 C12 Cr2 129.94(17) . . ?
C18 C12 Cr2 123.55(17) . . ?
C16 S1 C13 90.24(12) . . ?
C16 S2 C18 90.67(12) . . ?
C12 O12 C21 120.9(2) . . ?
C14 C13 C6 129.5(2) . . ?
C14 C13 S1 111.67(18) . . ?
C6 C13 S1 118.81(18) . . ?
C13 C14 C15 112.6(2) . . ?
C13 C14 H14 123.7 . . ?
C15 C14 H14 123.7 . . ?
C16 C15 C14 112.3(2) . . ?
C16 C15 C17 112.1(2) . . ?
C14 C15 C17 135.7(2) . . ?
C15 C16 S1 113.20(18) . . ?
C15 C16 S2 112.92(18) . . ?
S1 C16 S2 133.87(16) . . ?
C18 C17 C15 113.2(2) . . ?
C18 C17 H17 123.4 . . ?
C15 C17 H17 123.4 . . ?
C17 C18 C12 129.7(2) . . ?
C17 C18 S2 111.16(18) . . ?
C12 C18 S2 119.14(18) . . ?
O6 C19 C20 107.0(2) . . ?
O6 C19 H19A 110.3 . . ?
C20 C19 H19A 110.3 . . ?
O6 C19 H19B 110.3 . . ?
C20 C19 H19B 110.3 . . ?
H19A C19 H19B 108.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O12 C21 C22 108.6(2) . . ?
O12 C21 H21A 110.0 . . ?
C22 C21 H21A 110.0 . . ?
O12 C21 H21B 110.0 . . ?
C22 C21 H21B 110.0 . . ?
H21A C21 H21B 108.3 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 C6 O6 C19 -178.4(2) . . . . ?
Cr1 C6 O6 C19 5.1(4) . . . . ?
C18 C12 O12 C21 -179.5(2) . . . . ?
Cr2 C12 O12 C21 -0.3(4) . . . . ?
O6 C6 C13 C14 172.1(3) . . . . ?
Cr1 C6 C13 C14 -11.1(4) . . . . ?
O6 C6 C13 S1 -7.7(3) . . . . ?
Cr1 C6 C13 S1 169.02(12) . . . . ?
C16 S1 C13 C14 0.7(2) . . . . ?
C16 S1 C13 C6 -179.5(2) . . . . ?
C6 C13 C14 C15 -179.7(2) . . . . ?
S1 C13 C14 C15 0.2(3) . . . . ?
C13 C14 C15 C16 -1.2(3) . . . . ?
C13 C14 C15 C17 179.5(3) . . . . ?
C14 C15 C16 S1 1.8(3) . . . . ?
C17 C15 C16 S1 -178.76(18) . . . . ?
C14 C15 C16 S2 -178.94(18) . . . . ?
C17 C15 C16 S2 0.6(3) . . . . ?
C13 S1 C16 C15 -1.4(2) . . . . ?
C13 S1 C16 S2 179.5(2) . . . . ?
C18 S2 C16 C15 0.1(2) . . . . ?
C18 S2 C16 S1 179.2(2) . . . . ?
C16 C15 C17 C18 -1.1(3) . . . . ?
C14 C15 C17 C18 178.2(3) . . . . ?
C15 C17 C18 C12 -177.5(2) . . . . ?
C15 C17 C18 S2 1.1(3) . . . . ?
O12 C12 C18 C17 179.6(2) . . . . ?
Cr2 C12 C18 C17 0.3(4) . . . . ?
O12 C12 C18 S2 1.0(3) . . . . ?
Cr2 C12 C18 S2 -178.27(12) . . . . ?
C16 S2 C18 C17 -0.7(2) . . . . ?
C16 S2 C18 C12 178.1(2) . . . . ?
C6 O6 C19 C20 -170.3(2) . . . . ?
C12 O12 C21 C22 171.5(3) . . . . ?

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_mo_ZL228F5_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1401811'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/5
_chemical_name_systematic        
'2-(Ethoxy-(pentacarbonyl-tungsten)-carbene)-4,6-diethoxy-5,5,5,5-tetracarbonyl-5-tungsta-cyclopenta[b]thieno[3,2-d]thiophene hemidichloromethane'
_chemical_name_common            .
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H16 O12 S2 W2, 0.5(C1 H2 Cl2)'
_chemical_formula_sum            'C24.50 H17 Cl O12 S2 W2'
_chemical_formula_weight         970.65

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

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

_cell_length_a                   26.7813(12)
_cell_length_b                   26.7813(12)
_cell_length_c                   17.3239(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12425.4(13)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9322
_cell_measurement_theta_min      2.567
_cell_measurement_theta_max      33.054

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_F_000             7312
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.058
_exptl_absorpt_coefficient_mu    7.678
_shelx_estimated_absorpt_T_min   0.241
_shelx_estimated_absorpt_T_max   0.664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4610
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'I\ms micro focus'
_diffrn_measurement_device_type  'Bruker kappa, Photon 100 CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            270658
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.067
_diffrn_reflns_theta_max         33.240
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11904
_reflns_number_gt                10088
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXTL, SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
 ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
 Mercury (Macrae et al., 2008)
;
_computing_publication_material  'SHELXL-2014, PLATON (Spek, 2009)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0188P)²+19.9755P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic-phasing
_atom_sites_solution_secondary   .
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11904
_refine_ls_number_parameters     415
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0200
_refine_ls_wR_factor_ref         0.0446
_refine_ls_wR_factor_gt          0.0416
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000

_refine_diff_density_max         0.967
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.124

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 0.56510(2) 0.40289(2) 0.56786(2) 0.02085(2) Uani 1 1 d . . . . .
C1 C 0.50550(8) 0.44685(8) 0.58364(12) 0.0261(4) Uani 1 1 d . . . . .
O1 O 0.47029(6) 0.47061(7) 0.59419(10) 0.0366(4) Uani 1 1 d . . . . .
C2 C 0.51691(9) 0.34489(9) 0.56882(14) 0.0318(5) Uani 1 1 d . . . . .
O2 O 0.48819(7) 0.31317(7) 0.56740(13) 0.0506(5) Uani 1 1 d . . . . .
C3 C 0.55618(8) 0.40747(9) 0.44971(14) 0.0305(5) Uani 1 1 d . . . . .
O3 O 0.54974(8) 0.40998(9) 0.38521(11) 0.0500(5) Uani 1 1 d . . . . .
C4 C 0.57244(10) 0.39949(9) 0.68506(14) 0.0325(5) Uani 1 1 d . . . . .
O4 O 0.57523(10) 0.39806(8) 0.75041(12) 0.0584(6) Uani 1 1 d . . . . .
C5 C 0.63341(8) 0.36003(7) 0.55541(12) 0.0237(4) Uani 1 1 d . . . . .
O5 O 0.64695(6) 0.31283(6) 0.55873(11) 0.0345(4) Uani 1 1 d . . . . .
C6 C 0.62128(7) 0.46076(7) 0.55713(11) 0.0200(3) Uani 1 1 d . . . . .
O6 O 0.62306(5) 0.50977(5) 0.56182(8) 0.0233(3) Uani 1 1 d . . . . .
W2 W 0.78842(2) 0.63935(2) 0.46955(2) 0.01871(2) Uani 1 1 d . . . . .
C7 C 0.76256(8) 0.71029(8) 0.47804(13) 0.0267(4) Uani 1 1 d . . . . .
O7 O 0.74890(8) 0.75035(6) 0.48435(12) 0.0422(4) Uani 1 1 d . . . . .
C8 C 0.72421(8) 0.62023(8) 0.41372(12) 0.0238(4) Uani 1 1 d . . . . .
O8 O 0.68709(7) 0.61150(7) 0.38483(10) 0.0374(4) Uani 1 1 d . . . . .
C9 C 0.82129(9) 0.65769(8) 0.36699(14) 0.0297(4) Uani 1 1 d . . . . .
O9 O 0.83892(8) 0.67069(7) 0.31030(11) 0.0458(5) Uani 1 1 d . . . . .
C10 C 0.84928(9) 0.66611(9) 0.52739(15) 0.0351(5) Uani 1 1 d . . . . .
O10 O 0.88115(8) 0.68445(9) 0.55956(16) 0.0652(7) Uani 1 1 d . . . . .
C11 C 0.75624(9) 0.62292(8) 0.57371(12) 0.0256(4) Uani 1 1 d . . . . .
O11 O 0.73862(8) 0.61307(7) 0.63115(10) 0.0420(4) Uani 1 1 d . . . . .
C12 C 0.81439(7) 0.56204(7) 0.46895(10) 0.0192(3) Uani 1 1 d . . . . .
O12 O 0.85971(5) 0.54379(6) 0.45710(9) 0.0253(3) Uani 1 1 d . . . . .
S1 S 0.73739(2) 0.37137(2) 0.52229(3) 0.02322(9) Uani 1 1 d . . . . .
S2 S 0.81094(2) 0.45900(2) 0.48463(3) 0.02149(9) Uani 1 1 d . . . . .
C13 C 0.67654(7) 0.39093(7) 0.54001(11) 0.0209(4) Uani 1 1 d . . . . .
C14 C 0.67119(7) 0.44229(7) 0.53837(11) 0.0192(3) Uani 1 1 d . . . . .
C15 C 0.71688(7) 0.46685(7) 0.51952(11) 0.0183(3) Uani 1 1 d . . . . .
C16 C 0.75534(7) 0.43236(7) 0.50943(11) 0.0197(3) Uani 1 1 d . . . . .
C17 C 0.78292(7) 0.51877(7) 0.48590(11) 0.0193(3) Uani 1 1 d . . . . .
C18 C 0.73316(7) 0.51623(7) 0.50562(11) 0.0198(3) Uani 1 1 d . . . . .
H18 H 0.7121 0.5446 0.5095 0.024 Uiso 1 1 calc R U . . .
C19 C 0.60931(10) 0.27493(9) 0.5752(2) 0.0499(8) Uani 1 1 d . . . . .
H19A H 0.5848 0.2733 0.5325 0.060 Uiso 1 1 calc R U . . .
H19B H 0.5912 0.2834 0.6233 0.060 Uiso 1 1 calc R U . . .
C20 C 0.63507(12) 0.22631(12) 0.5837(3) 0.0745(13) Uani 1 1 d . . . . .
H20A H 0.6523 0.2180 0.5355 0.112 Uiso 1 1 calc R U . . .
H20B H 0.6105 0.2003 0.5956 0.112 Uiso 1 1 calc R U . . .
H20C H 0.6595 0.2285 0.6258 0.112 Uiso 1 1 calc R U . . .
C21 C 0.57789(8) 0.53746(8) 0.58029(14) 0.0283(4) Uani 1 1 d . . . . .
H21A H 0.5655 0.5281 0.6322 0.034 Uiso 1 1 calc R U . . .
H21B H 0.5514 0.5302 0.5420 0.034 Uiso 1 1 calc R U . . .
C22 C 0.59153(11) 0.59162(10) 0.5782(2) 0.0541(8) Uani 1 1 d . . . . .
H22A H 0.6199 0.5976 0.6127 0.081 Uiso 1 1 calc R U . . .
H22B H 0.5630 0.6117 0.5952 0.081 Uiso 1 1 calc R U . . .
H22C H 0.6006 0.6011 0.5254 0.081 Uiso 1 1 calc R U . . .
C23 C 0.90266(8) 0.57509(9) 0.44184(16) 0.0342(5) Uani 1 1 d . . . . .
H23A H 0.9047 0.6023 0.4804 0.041 Uiso 1 1 calc R U . . .
H23B H 0.9001 0.5902 0.3898 0.041 Uiso 1 1 calc R U . . .
C24 C 0.94785(9) 0.54227(11) 0.44683(19) 0.0431(6) Uani 1 1 d . . . . .
H24A H 0.9497 0.5273 0.4983 0.065 Uiso 1 1 calc R U . . .
H24B H 0.9779 0.5623 0.4375 0.065 Uiso 1 1 calc R U . . .
H24C H 0.9455 0.5158 0.4079 0.065 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5462(3) 0.7210(3) 0.6142(2) 0.090(4) Uani 0.388(16) 1 d . . P A 1
Cl1A Cl 0.4932(17) 0.8025(6) 0.6391(8) 0.107(19) Uani 0.112(16) 1 d . . P A 2
C25 C 0.5052(14) 0.7667(6) 0.6456(12) 0.087(8) Uani 0.25 1 d . . P . .
Cl2A Cl 0.5553(4) 0.2562(4) 0.7844(5) 0.250(6) Uani 0.35 1 d D . P B 1
Cl2B Cl 0.4891(16) 0.2669(9) 0.7539(10) 0.241(12) Uani 0.15 1 d D . P B 2
C26 C 0.5000 0.2500 0.8482(11) 0.48(5) Uani 0.5 2 d DS T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C1 2.002(2) . ?
W1 C2 2.019(2) . ?
W1 C4 2.042(2) . ?
W1 C3 2.064(2) . ?
W1 C6 2.168(2) . ?
W1 C5 2.170(2) . ?
C1 O1 1.152(3) . ?
C2 O2 1.146(3) . ?
C3 O3 1.133(3) . ?
C4 O4 1.135(3) . ?
C5 O5 1.317(2) . ?
C5 C13 1.446(3) . ?
O5 C19 1.459(3) . ?
C6 O6 1.316(2) . ?
C6 C14 1.462(3) . ?
O6 C21 1.455(2) . ?
W2 C7 2.027(2) . ?
W2 C8 2.038(2) . ?
W2 C9 2.043(2) . ?
W2 C10 2.043(2) . ?
W2 C11 2.048(2) . ?
W2 C12 2.184(2) . ?
C7 O7 1.139(3) . ?
C8 O8 1.137(3) . ?
C9 O9 1.144(3) . ?
C10 O10 1.132(3) . ?
C11 O11 1.132(3) . ?
C12 O12 1.325(2) . ?
C12 C17 1.463(3) . ?
O12 C23 1.448(3) . ?
S1 C16 1.7170(19) . ?
S1 C13 1.739(2) . ?
S2 C16 1.706(2) . ?
S2 C17 1.7681(19) . ?
C13 C14 1.383(3) . ?
C14 C15 1.427(3) . ?
C15 C16 1.394(3) . ?
C15 C18 1.413(3) . ?
C17 C18 1.377(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.481(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.496(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.498(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
Cl1 C25 1.73(2) . ?
Cl1A C25 1.77(4) 15_566 ?
Cl2A C26 1.855(12) . ?
Cl2B C26 1.720(17) . ?

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
C1 W1 C2 86.66(9) . . ?
C1 W1 C4 88.12(9) . . ?
C2 W1 C4 91.09(10) . . ?
C1 W1 C3 90.46(9) . . ?
C2 W1 C3 88.85(10) . . ?
C4 W1 C3 178.58(10) . . ?
C1 W1 C6 98.31(8) . . ?
C2 W1 C6 173.73(8) . . ?
C4 W1 C6 92.88(9) . . ?
C3 W1 C6 87.29(8) . . ?
C1 W1 C5 175.21(8) . . ?
C2 W1 C5 97.63(8) . . ?
C4 W1 C5 89.67(9) . . ?
C3 W1 C5 91.75(8) . . ?
C6 W1 C5 77.56(7) . . ?
O1 C1 W1 177.3(2) . . ?
O2 C2 W1 177.0(2) . . ?
O3 C3 W1 177.9(2) . . ?
O4 C4 W1 178.2(3) . . ?
O5 C5 C13 109.73(18) . . ?
O5 C5 W1 137.36(15) . . ?
C13 C5 W1 112.91(14) . . ?
C5 O5 C19 119.10(19) . . ?
O6 C6 C14 108.54(16) . . ?
O6 C6 W1 137.13(14) . . ?
C14 C6 W1 114.32(13) . . ?
C6 O6 C21 119.47(16) . . ?
C7 W2 C8 88.95(9) . . ?
C7 W2 C9 89.14(9) . . ?
C8 W2 C9 90.65(9) . . ?
C7 W2 C10 84.74(9) . . ?
C8 W2 C10 173.65(9) . . ?
C9 W2 C10 89.91(10) . . ?
C7 W2 C11 89.64(9) . . ?
C8 W2 C11 90.52(9) . . ?
C9 W2 C11 178.30(9) . . ?
C10 W2 C11 88.79(10) . . ?
C7 W2 C12 175.85(8) . . ?
C8 W2 C12 91.62(8) . . ?
C9 W2 C12 94.96(8) . . ?
C10 W2 C12 94.63(8) . . ?
C11 W2 C12 86.24(8) . . ?
O7 C7 W2 178.2(2) . . ?
O8 C8 W2 176.28(19) . . ?
O9 C9 W2 176.1(2) . . ?
O10 C10 W2 174.6(2) . . ?
O11 C11 W2 178.9(2) . . ?
O12 C12 C17 105.47(16) . . ?
O12 C12 W2 129.97(14) . . ?
C17 C12 W2 124.51(13) . . ?
C12 O12 C23 122.87(17) . . ?
C16 S1 C13 89.93(9) . . ?
C16 S2 C17 90.28(9) . . ?
C14 C13 C5 119.35(18) . . ?
C14 C13 S1 113.13(15) . . ?
C5 C13 S1 127.52(15) . . ?
C13 C14 C15 111.97(17) . . ?
C13 C14 C6 115.25(17) . . ?
C15 C14 C6 132.78(17) . . ?
C16 C15 C18 111.76(17) . . ?
C16 C15 C14 110.91(17) . . ?
C18 C15 C14 137.28(18) . . ?
C15 C16 S2 113.53(14) . . ?
C15 C16 S1 114.02(15) . . ?
S2 C16 S1 132.43(12) . . ?
C18 C17 C12 130.26(17) . . ?
C18 C17 S2 111.67(14) . . ?
C12 C17 S2 118.04(14) . . ?
C17 C18 C15 112.76(17) . . ?
C17 C18 H18 123.6 . . ?
C15 C18 H18 123.6 . . ?
O5 C19 C20 108.0(2) . . ?
O5 C19 H19A 110.1 . . ?
C20 C19 H19A 110.1 . . ?
O5 C19 H19B 110.1 . . ?
C20 C19 H19B 110.1 . . ?
H19A C19 H19B 108.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O6 C21 C22 106.6(2) . . ?
O6 C21 H21A 110.4 . . ?
C22 C21 H21A 110.4 . . ?
O6 C21 H21B 110.4 . . ?
C22 C21 H21B 110.4 . . ?
H21A C21 H21B 108.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O12 C23 C24 107.0(2) . . ?
O12 C23 H23A 110.3 . . ?
C24 C23 H23A 110.3 . . ?
O12 C23 H23B 110.3 . . ?
C24 C23 H23B 110.3 . . ?
H23A C23 H23B 108.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Cl1 C25 Cl1 96(2) 12_767 . ?
Cl1A C25 Cl1A 91(2) . 12_767 ?
Cl2A C26 Cl2A 106.8(11) 6_554 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 C5 O5 C19 178.9(2) . . . . ?
W1 C5 O5 C19 -0.3(4) . . . . ?
C14 C6 O6 C21 -179.76(17) . . . . ?
W1 C6 O6 C21 1.5(3) . . . . ?
C17 C12 O12 C23 -177.18(19) . . . . ?
W2 C12 O12 C23 0.4(3) . . . . ?
O5 C5 C13 C14 -176.46(19) . . . . ?
W1 C5 C13 C14 2.9(2) . . . . ?
O5 C5 C13 S1 3.6(3) . . . . ?
W1 C5 C13 S1 -177.03(12) . . . . ?
C16 S1 C13 C14 -1.90(16) . . . . ?
C16 S1 C13 C5 178.08(19) . . . . ?
C5 C13 C14 C15 -177.75(17) . . . . ?
S1 C13 C14 C15 2.2(2) . . . . ?
C5 C13 C14 C6 3.2(3) . . . . ?
S1 C13 C14 C6 -176.77(14) . . . . ?
O6 C6 C14 C13 173.05(17) . . . . ?
W1 C6 C14 C13 -7.9(2) . . . . ?
O6 C6 C14 C15 -5.7(3) . . . . ?
W1 C6 C14 C15 173.38(17) . . . . ?
C13 C14 C15 C16 -1.4(2) . . . . ?
C6 C14 C15 C16 177.4(2) . . . . ?
C13 C14 C15 C18 175.7(2) . . . . ?
C6 C14 C15 C18 -5.6(4) . . . . ?
C18 C15 C16 S2 0.8(2) . . . . ?
C14 C15 C16 S2 178.64(13) . . . . ?
C18 C15 C16 S1 -177.90(14) . . . . ?
C14 C15 C16 S1 0.0(2) . . . . ?
C17 S2 C16 C15 -0.79(16) . . . . ?
C17 S2 C16 S1 177.58(16) . . . . ?
C13 S1 C16 C15 1.08(16) . . . . ?
C13 S1 C16 S2 -177.29(16) . . . . ?
O12 C12 C17 C18 177.1(2) . . . . ?
W2 C12 C17 C18 -0.7(3) . . . . ?
O12 C12 C17 S2 -0.9(2) . . . . ?
W2 C12 C17 S2 -178.65(9) . . . . ?
C16 S2 C17 C18 0.60(15) . . . . ?
C16 S2 C17 C12 178.94(16) . . . . ?
C12 C17 C18 C15 -178.36(19) . . . . ?
S2 C17 C18 C15 -0.3(2) . . . . ?
C16 C15 C18 C17 -0.3(2) . . . . ?
C14 C15 C18 C17 -177.4(2) . . . . ?
C5 O5 C19 C20 -174.1(3) . . . . ?
C6 O6 C21 C22 -177.8(2) . . . . ?
C12 O12 C23 C24 169.4(2) . . . . ?

_shelxl_version_number           2014/5

####################################################################### 
# 
# 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_mo_ZL228F7_2_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1401812'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/5
_chemical_name_systematic        
2,2,2,2,5,5,5,5-Octacarbonyl-1,3,4,6-tetraethoxy-2,5-ditungsta-dicyclopenta[b,e]thieno[3,2-d]thiophene
_chemical_name_common            .
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H20 O12 S2 W2'
_chemical_formula_sum            'C26 H20 O12 S2 W2'
_chemical_formula_weight         956.24

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_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                   7.2013(3)
_cell_length_b                   34.2589(15)
_cell_length_c                   12.5924(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.9948(12)
_cell_angle_gamma                90
_cell_volume                     3038.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9009
_cell_measurement_theta_min      2.378
_cell_measurement_theta_max      38.750

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.090
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.086
_exptl_absorpt_coefficient_mu    7.762
_shelx_estimated_absorpt_T_min   0.207
_shelx_estimated_absorpt_T_max   0.555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4197
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'I\ms micro focus'
_diffrn_measurement_device_type  'Bruker kappa, Photon 100 CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            223788
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.036
_diffrn_reflns_theta_max         36.318
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14696
_reflns_number_gt                12986
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXTL, SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
 ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
 Mercury (Macrae et al., 2008)
;
_computing_publication_material  'SHELXL-2014, PLATON (Spek, 2009)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0195P)²+2.5989P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic-phasing
_atom_sites_solution_secondary   .
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14696
_refine_ls_number_parameters     383
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0538
_refine_ls_wR_factor_gt          0.0522
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

_refine_diff_density_max         1.843
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.137

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 0.13788(2) 0.27640(2) 0.38855(2) 0.01640(2) Uani 1 1 d . . . . .
C1 C -0.0324(3) 0.30713(8) 0.2687(2) 0.0287(5) Uani 1 1 d . . . . .
O1 O -0.1253(3) 0.32369(7) 0.19868(19) 0.0497(6) Uani 1 1 d . . . . .
C2 C 0.1028(3) 0.23115(7) 0.28333(19) 0.0236(4) Uani 1 1 d . . . . .
O2 O 0.0724(3) 0.20583(6) 0.22199(16) 0.0358(4) Uani 1 1 d . . . . .
C3 C 0.3714(3) 0.30069(7) 0.34289(18) 0.0229(4) Uani 1 1 d . . . . .
O3 O 0.5006(3) 0.31630(6) 0.32498(17) 0.0356(4) Uani 1 1 d . . . . .
C4 C -0.0888(3) 0.25777(7) 0.45036(18) 0.0228(4) Uani 1 1 d . . . . .
O4 O -0.2143(3) 0.24747(6) 0.48474(18) 0.0382(4) Uani 1 1 d . . . . .
C5 C 0.3307(3) 0.24863(6) 0.52003(17) 0.0173(3) Uani 1 1 d . . . . .
O5 O 0.3855(2) 0.21288(4) 0.55155(14) 0.0233(3) Uani 1 1 d . . . . .
C6 C 0.1926(3) 0.32105(5) 0.51176(16) 0.0157(3) Uani 1 1 d . . . . .
O6 O 0.1029(2) 0.35149(4) 0.53894(13) 0.0206(3) Uani 1 1 d . . . . .
W2 W 0.49370(2) 0.46634(2) 0.75757(2) 0.01644(2) Uani 1 1 d . . . . .
C7 C 0.3322(3) 0.50522(7) 0.65847(19) 0.0250(4) Uani 1 1 d . . . . .
O7 O 0.2427(3) 0.52896(6) 0.60698(18) 0.0414(5) Uani 1 1 d . . . . .
C8 C 0.5689(4) 0.51284(7) 0.85536(19) 0.0265(4) Uani 1 1 d . . . . .
O8 O 0.6083(3) 0.54065(6) 0.90575(18) 0.0426(5) Uani 1 1 d . . . . .
C9 C 0.7264(3) 0.47526(6) 0.69051(18) 0.0219(4) Uani 1 1 d . . . . .
O9 O 0.8577(3) 0.47999(6) 0.65467(16) 0.0355(4) Uani 1 1 d . . . . .
C10 C 0.2653(3) 0.45162(7) 0.82447(19) 0.0254(4) Uani 1 1 d . . . . .
O10 O 0.1394(3) 0.44235(7) 0.85966(18) 0.0442(5) Uani 1 1 d . . . . .
C11 C 0.6514(3) 0.42130(6) 0.85805(16) 0.0175(3) Uani 1 1 d . . . . .
O11 O 0.7683(2) 0.41860(5) 0.95364(12) 0.0217(3) Uani 1 1 d . . . . .
C12 C 0.4314(3) 0.41499(6) 0.65700(15) 0.0159(3) Uani 1 1 d . . . . .
O12 O 0.3680(2) 0.40775(4) 0.55311(11) 0.0187(3) Uani 1 1 d . . . . .
S1 S 0.60400(7) 0.26663(2) 0.71295(4) 0.02037(9) Uani 1 1 d . . . . .
S2 S 0.73034(8) 0.33957(2) 0.86130(4) 0.02161(10) Uani 1 1 d . . . . .
C13 C 0.4286(3) 0.27664(5) 0.59949(16) 0.0165(3) Uani 1 1 d . . . . .
C14 C 0.3697(2) 0.31499(5) 0.59259(15) 0.0146(3) Uani 1 1 d . . . . .
C15 C 0.4758(3) 0.33816(5) 0.67859(15) 0.0154(3) Uani 1 1 d . . . . .
C16 C 0.6026(3) 0.31482(6) 0.75074(16) 0.0186(3) Uani 1 1 d . . . . .
C17 C 0.6190(3) 0.38272(6) 0.81068(16) 0.0172(3) Uani 1 1 d . . . . .
C18 C 0.4930(3) 0.37800(6) 0.71233(15) 0.0154(3) Uani 1 1 d . . . . .
C19 C 0.2997(4) 0.18021(7) 0.4855(2) 0.0307(5) Uani 1 1 d . . . . .
H19A H 0.3415 0.1799 0.4155 0.037 Uiso 1 1 calc R U . . .
H19B H 0.1596 0.1824 0.4706 0.037 Uiso 1 1 calc R U . . .
C20 C 0.3628(6) 0.14343(8) 0.5487(3) 0.0500(8) Uani 1 1 d . . . . .
H20A H 0.5016 0.1415 0.5624 0.075 Uiso 1 1 calc R U . . .
H20B H 0.3067 0.1207 0.5066 0.075 Uiso 1 1 calc R U . . .
H20C H 0.3213 0.1442 0.6180 0.075 Uiso 1 1 calc R U . . .
C21 C -0.0869(3) 0.36020(8) 0.4781(2) 0.0326(5) Uani 1 1 d . . . . .
H21A H -0.1639 0.3361 0.4651 0.039 Uiso 1 1 calc R U . . .
H21B H -0.0811 0.3720 0.4072 0.039 Uiso 1 1 calc R U . . .
C22 C -0.1707(5) 0.38782(12) 0.5446(3) 0.0516(9) Uani 1 1 d . . . . .
H22A H -0.1693 0.3762 0.6159 0.077 Uiso 1 1 calc R U . . .
H22B H -0.3019 0.3936 0.5083 0.077 Uiso 1 1 calc R U . . .
H22C H -0.0967 0.4120 0.5537 0.077 Uiso 1 1 calc R U . . .
C23 C 0.8203(3) 0.45352(7) 1.01733(19) 0.0274(4) Uani 1 1 d . . . . .
H23A H 0.7056 0.4688 1.0217 0.033 Uiso 1 1 calc R U . . .
H23B H 0.9050 0.4700 0.9836 0.033 Uiso 1 1 calc R U . . .
C24 C 0.9205(5) 0.44091(10) 1.1285(2) 0.0487(8) Uani 1 1 d . . . . .
H24A H 0.8318 0.4266 1.1636 0.073 Uiso 1 1 calc R U . . .
H24B H 0.9677 0.4639 1.1720 0.073 Uiso 1 1 calc R U . . .
H24C H 1.0274 0.4239 1.1226 0.073 Uiso 1 1 calc R U . . .
C25 C 0.3125(3) 0.43924(6) 0.47674(17) 0.0243(4) Uani 1 1 d . . . . .
H25A H 0.4095 0.4602 0.4887 0.029 Uiso 1 1 calc R U . . .
H25B H 0.1897 0.4505 0.4850 0.029 Uiso 1 1 calc R U . . .
C26 C 0.2951(4) 0.42175(8) 0.36574(19) 0.0348(6) Uani 1 1 d . . . . .
H26A H 0.4187 0.4115 0.3580 0.052 Uiso 1 1 calc R U . . .
H26B H 0.2534 0.4419 0.3106 0.052 Uiso 1 1 calc R U . . .
H26C H 0.2020 0.4005 0.3562 0.052 Uiso 1 1 calc R U . . .


_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 C2 2.021(2) . ?
W1 C1 2.030(2) . ?
W1 C4 2.051(2) . ?
W1 C3 2.062(2) . ?
W1 C5 2.149(2) . ?
W1 C6 2.1561(19) . ?
C1 O1 1.141(3) . ?
C2 O2 1.152(3) . ?
C3 O3 1.135(3) . ?
C4 O4 1.136(3) . ?
C5 O5 1.322(2) . ?
C5 C13 1.458(3) . ?
O5 C19 1.453(3) . ?
C6 O6 1.309(2) . ?
C6 C14 1.472(3) . ?
O6 C21 1.452(3) . ?
W2 C8 2.018(2) . ?
W2 C7 2.020(2) . ?
W2 C9 2.050(2) . ?
W2 C10 2.060(2) . ?
W2 C12 2.1597(19) . ?
W2 C11 2.162(2) . ?
C7 O7 1.150(3) . ?
C8 O8 1.147(3) . ?
C9 O9 1.141(3) . ?
C10 O10 1.134(3) . ?
C11 O11 1.321(2) . ?
C11 C17 1.449(3) . ?
O11 C23 1.446(3) . ?
C12 O12 1.317(2) . ?
C12 C18 1.469(3) . ?
O12 C25 1.445(2) . ?
S1 C16 1.719(2) . ?
S1 C13 1.733(2) . ?
S2 C16 1.724(2) . ?
S2 C17 1.738(2) . ?
C13 C14 1.378(3) . ?
C14 C15 1.429(3) . ?
C15 C16 1.398(3) . ?
C15 C18 1.427(3) . ?
C17 C18 1.384(3) . ?
C19 C20 1.508(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.473(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.499(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.502(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 W1 C1 86.36(10) . . ?
C2 W1 C4 90.53(9) . . ?
C1 W1 C4 92.18(10) . . ?
C2 W1 C3 97.17(9) . . ?
C1 W1 C3 89.14(10) . . ?
C4 W1 C3 172.26(8) . . ?
C2 W1 C5 97.96(9) . . ?
C1 W1 C5 174.94(9) . . ?
C4 W1 C5 90.43(8) . . ?
C3 W1 C5 87.70(8) . . ?
C2 W1 C6 174.51(9) . . ?
C1 W1 C6 99.13(9) . . ?
C4 W1 C6 89.35(8) . . ?
C3 W1 C6 82.91(8) . . ?
C5 W1 C6 76.55(7) . . ?
O1 C1 W1 177.5(3) . . ?
O2 C2 W1 176.3(2) . . ?
O3 C3 W1 174.0(2) . . ?
O4 C4 W1 179.9(3) . . ?
O5 C5 C13 109.38(17) . . ?
O5 C5 W1 138.25(14) . . ?
C13 C5 W1 112.36(13) . . ?
C5 O5 C19 118.48(18) . . ?
O6 C6 C14 109.60(16) . . ?
O6 C6 W1 136.62(13) . . ?
C14 C6 W1 113.58(13) . . ?
C6 O6 C21 119.18(17) . . ?
C8 W2 C7 84.47(10) . . ?
C8 W2 C9 89.70(9) . . ?
C7 W2 C9 93.57(9) . . ?
C8 W2 C10 94.57(10) . . ?
C7 W2 C10 90.45(9) . . ?
C9 W2 C10 174.40(9) . . ?
C8 W2 C12 176.24(9) . . ?
C7 W2 C12 98.75(8) . . ?
C9 W2 C12 88.16(8) . . ?
C10 W2 C12 87.38(8) . . ?
C8 W2 C11 99.47(9) . . ?
C7 W2 C11 175.60(8) . . ?
C9 W2 C11 88.43(8) . . ?
C10 W2 C11 87.31(8) . . ?
C12 W2 C11 77.38(7) . . ?
O7 C7 W2 175.9(2) . . ?
O8 C8 W2 176.0(2) . . ?
O9 C9 W2 178.9(2) . . ?
O10 C10 W2 177.7(2) . . ?
O11 C11 C17 109.21(17) . . ?
O11 C11 W2 137.81(15) . . ?
C17 C11 W2 112.96(13) . . ?
C11 O11 C23 119.37(18) . . ?
O12 C12 C18 108.47(16) . . ?
O12 C12 W2 136.31(14) . . ?
C18 C12 W2 114.76(13) . . ?
C12 O12 C25 120.75(16) . . ?
C16 S1 C13 89.61(9) . . ?
C16 S2 C17 89.67(9) . . ?
C14 C13 C5 119.05(17) . . ?
C14 C13 S1 113.73(14) . . ?
C5 C13 S1 126.97(15) . . ?
C13 C14 C15 111.90(16) . . ?
C13 C14 C6 112.90(16) . . ?
C15 C14 C6 134.06(17) . . ?
C16 C15 C18 110.41(16) . . ?
C16 C15 C14 110.41(16) . . ?
C18 C15 C14 139.17(17) . . ?
C15 C16 S1 114.21(14) . . ?
C15 C16 S2 114.23(15) . . ?
S1 C16 S2 131.56(12) . . ?
C18 C17 C11 119.63(17) . . ?
C18 C17 S2 113.28(15) . . ?
C11 C17 S2 127.04(14) . . ?
C17 C18 C15 112.24(17) . . ?
C17 C18 C12 113.62(17) . . ?
C15 C18 C12 133.19(17) . . ?
O5 C19 C20 107.2(2) . . ?
O5 C19 H19A 110.3 . . ?
C20 C19 H19A 110.3 . . ?
O5 C19 H19B 110.3 . . ?
C20 C19 H19B 110.3 . . ?
H19A C19 H19B 108.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O6 C21 C22 106.5(2) . . ?
O6 C21 H21A 110.4 . . ?
C22 C21 H21A 110.4 . . ?
O6 C21 H21B 110.4 . . ?
C22 C21 H21B 110.4 . . ?
H21A C21 H21B 108.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O11 C23 C24 107.4(2) . . ?
O11 C23 H23A 110.2 . . ?
C24 C23 H23A 110.2 . . ?
O11 C23 H23B 110.2 . . ?
C24 C23 H23B 110.2 . . ?
H23A C23 H23B 108.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O12 C25 C26 106.22(18) . . ?
O12 C25 H25A 110.5 . . ?
C26 C25 H25A 110.5 . . ?
O12 C25 H25B 110.5 . . ?
C26 C25 H25B 110.5 . . ?
H25A C25 H25B 108.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 C5 O5 C19 177.87(19) . . . . ?
W1 C5 O5 C19 -0.8(3) . . . . ?
C14 C6 O6 C21 -172.5(2) . . . . ?
W1 C6 O6 C21 1.9(3) . . . . ?
C17 C11 O11 C23 -179.33(18) . . . . ?
W2 C11 O11 C23 -1.3(3) . . . . ?
C18 C12 O12 C25 -174.73(17) . . . . ?
W2 C12 O12 C25 -3.2(3) . . . . ?
O5 C5 C13 C14 -169.15(18) . . . . ?
W1 C5 C13 C14 9.9(2) . . . . ?
O5 C5 C13 S1 4.8(3) . . . . ?
W1 C5 C13 S1 -176.20(12) . . . . ?
C16 S1 C13 C14 -1.19(17) . . . . ?
C16 S1 C13 C5 -175.38(19) . . . . ?
C5 C13 C14 C15 177.88(18) . . . . ?
S1 C13 C14 C15 3.2(2) . . . . ?
C5 C13 C14 C6 8.3(3) . . . . ?
S1 C13 C14 C6 -166.42(14) . . . . ?
O6 C6 C14 C13 153.20(18) . . . . ?
W1 C6 C14 C13 -22.6(2) . . . . ?
O6 C6 C14 C15 -13.3(3) . . . . ?
W1 C6 C14 C15 170.84(18) . . . . ?
C13 C14 C15 C16 -4.0(2) . . . . ?
C6 C14 C15 C16 162.7(2) . . . . ?
C13 C14 C15 C18 175.0(2) . . . . ?
C6 C14 C15 C18 -18.4(4) . . . . ?
C18 C15 C16 S1 -176.13(14) . . . . ?
C14 C15 C16 S1 3.1(2) . . . . ?
C18 C15 C16 S2 3.6(2) . . . . ?
C14 C15 C16 S2 -177.15(14) . . . . ?
C13 S1 C16 C15 -1.18(17) . . . . ?
C13 S1 C16 S2 179.16(17) . . . . ?
C17 S2 C16 C15 -1.44(17) . . . . ?
C17 S2 C16 S1 178.23(17) . . . . ?
O11 C11 C17 C18 176.76(18) . . . . ?
W2 C11 C17 C18 -1.8(2) . . . . ?
O11 C11 C17 S2 -6.0(3) . . . . ?
W2 C11 C17 S2 175.43(12) . . . . ?
C16 S2 C17 C18 -1.20(17) . . . . ?
C16 S2 C17 C11 -178.55(19) . . . . ?
C11 C17 C18 C15 -178.96(18) . . . . ?
S2 C17 C18 C15 3.5(2) . . . . ?
C11 C17 C18 C12 10.7(3) . . . . ?
S2 C17 C18 C12 -166.86(14) . . . . ?
C16 C15 C18 C17 -4.4(2) . . . . ?
C14 C15 C18 C17 176.6(2) . . . . ?
C16 C15 C18 C12 163.4(2) . . . . ?
C14 C15 C18 C12 -15.6(4) . . . . ?
O12 C12 C18 C17 159.05(17) . . . . ?
W2 C12 C18 C17 -14.5(2) . . . . ?
O12 C12 C18 C15 -8.6(3) . . . . ?
W2 C12 C18 C15 177.77(18) . . . . ?
C5 O5 C19 C20 -170.9(2) . . . . ?
C6 O6 C21 C22 163.9(2) . . . . ?
C11 O11 C23 C24 169.1(2) . . . . ?
C12 O12 C25 C26 166.3(2) . . . . ?

_shelxl_version_number           2014/5

####################################################################### 
# 
# 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_nvj14_p21c
_database_code_depnum_ccdc_archive 'CCDC 1422363'
_audit_update_record             
;
2015-09-04 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
5,5,5,5-Tetracarbonyl-4,6-diethoxy-5-tungsta(0)cyclopentatrieno[b]thiophene
_chemical_name_common            .
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 O6 S W'
_chemical_formula_sum            'C14 H12 O6 S W'
_chemical_formula_weight         492.15

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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                   7.3338(4)
_cell_length_b                   21.4603(12)
_cell_length_c                   10.6447(6)
_cell_angle_alpha                90
_cell_angle_beta                 108.0170(10)
_cell_angle_gamma                90
_cell_volume                     1593.17(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6702
_cell_measurement_theta_min      2.766
_cell_measurement_theta_max      26.589

_exptl_crystal_description       prism
_exptl_crystal_colour            dark-blue-black
_exptl_crystal_size_min          0.11
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_max          0.38
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    7.405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.278
_exptl_absorpt_correction_T_max  0.443
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'

_exptl_special_details           ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker (Seimens) P4'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'SMART 1000 CCD'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            8550
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         2.766
_diffrn_reflns_theta_max         26.589
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3039
_reflns_number_gt                2844
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  
;
 SHELXTL and SHELXL-2014 (Sheldrick, 2015)
;
_computing_molecular_graphics    
;
 ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
 Mercury (Macrae et al., 2008)
;
_computing_publication_material  'SHELXL-2014, PLATON (Spek, 2009)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0337P)²+0.8706P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3039
_refine_ls_number_parameters     224
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0637
_refine_ls_wR_factor_gt          0.0624
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_restrained_S_all      1.144
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

_refine_diff_density_max         1.404
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.107

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 0.43483(2) 0.34548(2) 0.70073(2) 0.03871(8) Uani 1 1 d . . . . .
C1 C 0.2549(7) 0.3030(2) 0.5414(4) 0.0563(10) Uani 1 1 d . . . . .
O1 O 0.1577(6) 0.27439(18) 0.4572(3) 0.0866(11) Uani 1 1 d . . . . .
C2 C 0.4914(8) 0.25735(19) 0.7644(4) 0.0573(11) Uani 1 1 d . . . . .
O2 O 0.5135(7) 0.20542(17) 0.7930(4) 0.0884(12) Uani 1 1 d . . . . .
C3 C 0.2230(7) 0.35363(17) 0.7889(4) 0.0470(9) Uani 1 1 d . . . . .
O3 O 0.1071(6) 0.36171(19) 0.8370(4) 0.0739(9) Uani 1 1 d . . . . .
C4 C 0.6517(7) 0.34765(16) 0.6147(5) 0.0490(10) Uani 1 1 d . . . . .
O4 O 0.7701(7) 0.35121(17) 0.5672(5) 0.0794(12) Uani 1 1 d . . . . .
C5 C 0.6217(5) 0.39473(16) 0.8690(3) 0.0389(7) Uani 1 1 d . . . . .
O5 O 0.7461(4) 0.37989(12) 0.9836(2) 0.0454(6) Uani 1 1 d . . . . .
C6 C 0.3786(5) 0.44213(16) 0.6393(3) 0.0346(7) Uani 1 1 d . . . . .
O6 O 0.2734(4) 0.47156(12) 0.5347(2) 0.0434(6) Uani 1 1 d . . . . .
C7 C 0.6074(5) 0.46196(16) 0.8556(3) 0.0373(7) Uani 1 1 d D . . . .
C8 C 0.4819(5) 0.48590(15) 0.7403(4) 0.0375(7) Uani 1 1 d D . . . .
S1 S 0.7257(5) 0.51691(9) 0.9664(3) 0.0457(6) Uani 0.636(6) 1 d D . P A 1
C9 C 0.491(2) 0.5507(4) 0.7515(12) 0.061(5) Uani 0.636(6) 1 d D . P A 1
H9 H 0.4148 0.5755 0.6838 0.073 Uiso 0.636(6) 1 calc R U P A 1
C10 C 0.614(4) 0.5779(5) 0.8645(15) 0.034(3) Uani 0.636(6) 1 d D . P A 1
H10 H 0.6336 0.6202 0.8819 0.041 Uiso 0.636(6) 1 calc R U P A 1
S1A S 0.4612(10) 0.5634(2) 0.7267(6) 0.0449(13) Uani 0.364(6) 1 d D . P A 2
C9A C 0.684(3) 0.5127(6) 0.9372(15) 0.063(9) Uiso 0.364(6) 1 d D . P A 2
H9A H 0.7722 0.5080 1.0210 0.076 Uiso 0.364(6) 1 calc R U P A 2
C10A C 0.620(7) 0.5703(8) 0.884(3) 0.037(5) Uani 0.364(6) 1 d D . P A 2
H10A H 0.6578 0.6080 0.9277 0.045 Uiso 0.364(6) 1 calc R U P A 2
C11 C 0.7825(7) 0.31474(19) 1.0192(4) 0.0564(11) Uani 1 1 d . . . . .
H11A H 0.8329 0.2937 0.9563 0.068 Uiso 1 1 calc R U . . .
H11B H 0.6646 0.2942 1.0190 0.068 Uiso 1 1 calc R U . . .
C12 C 0.9243(8) 0.3125(2) 1.1535(5) 0.0753(15) Uani 1 1 d . . . . .
H12A H 1.0423 0.3312 1.1515 0.113 Uiso 1 1 calc R U . . .
H12B H 0.9471 0.2699 1.1815 0.113 Uiso 1 1 calc R U . . .
H12C H 0.8752 0.3349 1.2141 0.113 Uiso 1 1 calc R U . . .
C13 C 0.1514(6) 0.4363(2) 0.4244(4) 0.0486(9) Uani 1 1 d . . . . .
H13A H 0.0552 0.4137 0.4515 0.058 Uiso 1 1 calc R U . . .
H13B H 0.2273 0.4065 0.3936 0.058 Uiso 1 1 calc R U . . .
C14 C 0.0565(6) 0.4815(2) 0.3160(4) 0.0550(11) Uani 1 1 d . . . . .
H14A H -0.0233 0.5095 0.3460 0.083 Uiso 1 1 calc R U . . .
H14B H -0.0207 0.4590 0.2402 0.083 Uiso 1 1 calc R U . . .
H14C H 0.1528 0.5049 0.2925 0.083 Uiso 1 1 calc R U . . .


_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 C2 2.009(4) . ?
W1 C1 2.017(4) . ?
W1 C3 2.056(5) . ?
W1 C4 2.067(5) . ?
W1 C5 2.164(4) . ?
W1 C6 2.176(3) . ?
C1 O1 1.136(5) . ?
C2 O2 1.153(5) . ?
C3 O3 1.133(6) . ?
C4 O4 1.135(6) . ?
C5 O5 1.317(4) . ?
C5 C7 1.450(5) . ?
O5 C11 1.452(5) . ?
C6 O6 1.304(4) . ?
C6 C8 1.452(5) . ?
O6 C13 1.450(5) . ?
C7 C8 1.385(5) . ?
C7 C9A 1.399(10) . ?
C7 S1 1.703(4) . ?
C8 C9 1.395(9) . ?
C8 S1A 1.673(6) . ?
S1 C10 1.734(8) . ?
C9 C10 1.391(9) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
S1A C10A 1.728(10) . ?
C9A C10A 1.379(10) . ?
C9A H9A 0.9300 . ?
C10A H10A 0.9300 . ?
C11 C12 1.486(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.504(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?

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 W1 C1 82.60(18) . . ?
C2 W1 C3 91.85(18) . . ?
C1 W1 C3 91.84(18) . . ?
C2 W1 C4 93.65(18) . . ?
C1 W1 C4 91.76(18) . . ?
C3 W1 C4 173.77(15) . . ?
C2 W1 C5 99.71(16) . . ?
C1 W1 C5 177.60(16) . . ?
C3 W1 C5 87.43(15) . . ?
C4 W1 C5 88.77(15) . . ?
C2 W1 C6 177.85(15) . . ?
C1 W1 C6 99.47(15) . . ?
C3 W1 C6 87.50(13) . . ?
C4 W1 C6 86.89(13) . . ?
C5 W1 C6 78.22(13) . . ?
O1 C1 W1 174.2(4) . . ?
O2 C2 W1 175.0(4) . . ?
O3 C3 W1 176.1(4) . . ?
O4 C4 W1 177.4(3) . . ?
O5 C5 C7 109.9(3) . . ?
O5 C5 W1 136.8(2) . . ?
C7 C5 W1 113.4(2) . . ?
C5 O5 C11 119.6(3) . . ?
O6 C6 C8 110.7(3) . . ?
O6 C6 W1 136.5(2) . . ?
C8 C6 W1 112.8(2) . . ?
C6 O6 C13 119.5(3) . . ?
C8 C7 C9A 106.9(7) . . ?
C8 C7 C5 117.6(3) . . ?
C9A C7 C5 135.3(7) . . ?
C8 C7 S1 114.4(3) . . ?
C5 C7 S1 128.0(3) . . ?
C7 C8 C9 107.1(5) . . ?
C7 C8 C6 117.9(3) . . ?
C9 C8 C6 135.0(6) . . ?
C7 C8 S1A 117.6(4) . . ?
C6 C8 S1A 124.5(3) . . ?
C7 S1 C10 92.8(4) . . ?
C10 C9 C8 119.5(9) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 S1 106.2(8) . . ?
C9 C10 H10 126.9 . . ?
S1 C10 H10 126.9 . . ?
C8 S1A C10A 89.1(6) . . ?
C10A C9A C7 115.0(12) . . ?
C10A C9A H9A 122.5 . . ?
C7 C9A H9A 122.5 . . ?
C9A C10A S1A 111.3(11) . . ?
C9A C10A H10A 124.4 . . ?
S1A C10A H10A 124.4 . . ?
O5 C11 C12 107.5(4) . . ?
O5 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
O5 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O6 C13 C14 108.0(3) . . ?
O6 C13 H13A 110.1 . . ?
C14 C13 H13A 110.1 . . ?
O6 C13 H13B 110.1 . . ?
C14 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C5 O5 C11 179.4(3) . . . . ?
W1 C5 O5 C11 0.4(5) . . . . ?
C8 C6 O6 C13 -177.1(3) . . . . ?
W1 C6 O6 C13 2.0(5) . . . . ?
O5 C5 C7 C8 -179.9(3) . . . . ?
W1 C5 C7 C8 -0.6(4) . . . . ?
O5 C5 C7 C9A -4.6(15) . . . . ?
W1 C5 C7 C9A 174.6(14) . . . . ?
O5 C5 C7 S1 -0.6(5) . . . . ?
W1 C5 C7 S1 178.6(2) . . . . ?
C5 C7 C8 C9 179.0(8) . . . . ?
S1 C7 C8 C9 -0.3(8) . . . . ?
C9A C7 C8 C6 -178.6(11) . . . . ?
C5 C7 C8 C6 -2.1(5) . . . . ?
S1 C7 C8 C6 178.6(3) . . . . ?
C9A C7 C8 S1A 1.9(11) . . . . ?
C5 C7 C8 S1A 178.4(4) . . . . ?
O6 C6 C8 C7 -177.0(3) . . . . ?
W1 C6 C8 C7 3.7(4) . . . . ?
O6 C6 C8 C9 1.5(11) . . . . ?
W1 C6 C8 C9 -177.8(10) . . . . ?
O6 C6 C8 S1A 2.5(5) . . . . ?
W1 C6 C8 S1A -176.8(4) . . . . ?
C8 C7 S1 C10 -0.2(11) . . . . ?
C5 C7 S1 C10 -179.5(11) . . . . ?
C7 C8 C9 C10 1(2) . . . . ?
C6 C8 C9 C10 -177.7(16) . . . . ?
C8 C9 C10 S1 -1(3) . . . . ?
C7 S1 C10 C9 0.7(19) . . . . ?
C7 C8 S1A C10A -2(2) . . . . ?
C6 C8 S1A C10A 178(2) . . . . ?
C8 C7 C9A C10A -1(3) . . . . ?
C5 C7 C9A C10A -176(3) . . . . ?
C7 C9A C10A S1A -1(5) . . . . ?
C8 S1A C10A C9A 2(4) . . . . ?
C5 O5 C11 C12 -178.8(4) . . . . ?
C6 O6 C13 C14 -176.9(3) . . . . ?

