# 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_ZL215F1_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 1401808'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 Pentacarbonyl-(ethoxy-thieno[2,3-b]thiophen-2-yl-methylidene)-tungsten
;
_chemical_name_common            .
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H8 O6 S2 W'
_chemical_formula_sum            'C14 H8 O6 S2 W'
_chemical_formula_weight         520.17

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      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

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

_cell_length_a                   16.3613(7)
_cell_length_b                   26.0082(11)
_cell_length_c                   7.5595(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3216.8(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9294
_cell_measurement_theta_min      2.489
_cell_measurement_theta_max      27.557

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.148
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    7.467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4411
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'

_exptl_special_details           
;
 ?
;

_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       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            128826
_diffrn_reflns_av_unetI/netI     0.0076
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.490
_diffrn_reflns_theta_max         27.482
_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             3678
_reflns_number_gt                3594
_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, 2013)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXTL, SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    
;
 ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
 Mercury (Macrae et al., 2008)
;
_computing_publication_material  'SHELXL-2013, 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)+(0.0245P)²+4.6338P] 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         3678
_refine_ls_number_parameters     228
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0207
_refine_ls_wR_factor_ref         0.0570
_refine_ls_wR_factor_gt          0.0565
_refine_ls_goodness_of_fit_ref   1.351
_refine_ls_restrained_S_all      1.348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_diff_density_max         1.712
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.136

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 0.39842(2) 0.11724(2) 0.66665(2) 0.02033(6) Uani 1 1 d . . . . .
C1 C 0.2818(2) 0.09247(12) 0.6546(4) 0.0291(7) Uani 1 1 d . . . . .
O1 O 0.21505(16) 0.07940(11) 0.6511(4) 0.0449(7) Uani 1 1 d . . . . .
C2 C 0.43201(19) 0.06897(11) 0.4681(4) 0.0268(6) Uani 1 1 d . . . . .
O2 O 0.44963(17) 0.04172(9) 0.3561(3) 0.0366(6) Uani 1 1 d . . . . .
C3 C 0.36577(17) 0.16957(11) 0.4773(4) 0.0231(6) Uani 1 1 d . . . . .
O3 O 0.34278(15) 0.19652(9) 0.3705(3) 0.0322(5) Uani 1 1 d . . . . .
C4 C 0.36201(18) 0.16603(12) 0.8639(4) 0.0245(6) Uani 1 1 d . . . . .
O4 O 0.33972(14) 0.19287(9) 0.9726(3) 0.0336(5) Uani 1 1 d . . . . .
C5 C 0.4153(2) 0.05828(13) 0.8422(4) 0.0292(7) Uani 1 1 d . . . . .
O5 O 0.41746(17) 0.02311(10) 0.9319(4) 0.0438(6) Uani 1 1 d . . . . .
C6 C 0.52308(19) 0.14978(11) 0.6870(4) 0.0257(6) Uani 1 1 d . . . . .
O6 O 0.59379(14) 0.12507(9) 0.7009(4) 0.0351(6) Uani 1 1 d . . . . .
C7 C 0.5427(5) 0.2043(4) 0.7083(16) 0.019(2) Uani 0.5300(14) 1 d D . P A 1
C8 C 0.49313(17) 0.24614(11) 0.6735(4) 0.0217(6) Uani 0.5300(14) 1 d D . P A 1
H8 H 0.4371 0.2435 0.6419 0.026 Uiso 0.5300(14) 1 calc R U P A 1
C9 C 0.5355(5) 0.2935(3) 0.6902(12) 0.0244(9) Uani 0.5300(14) 1 d D . P A 1
C10 C 0.6167(4) 0.2859(2) 0.7386(9) 0.0248(13) Uani 0.5300(14) 1 d D . P A 1
S1 S 0.64443(9) 0.22264(6) 0.7564(3) 0.0275(3) Uani 0.5300(14) 1 d D . P A 1
C11 C 0.5159(2) 0.34709(12) 0.6718(4) 0.0264(6) Uani 0.5300(14) 1 d D . P A 1
H11 H 0.4639 0.3601 0.6378 0.032 Uiso 0.5300(14) 1 calc R U P A 1
C12 C 0.5830(5) 0.3769(4) 0.7105(12) 0.025(2) Uani 0.5300(14) 1 d D . P A 1
H12 H 0.5813 0.4134 0.7117 0.030 Uiso 0.5300(14) 1 calc R U P A 1
S2 S 0.67117(10) 0.34214(6) 0.7569(3) 0.0360(4) Uani 0.5300(14) 1 d D . P A 1
C7A C 0.5436(6) 0.2039(4) 0.663(2) 0.019(2) Uani 0.4700(14) 1 d D . P A 2
C8A C 0.49313(17) 0.24614(11) 0.6735(4) 0.0217(6) Uani 0.4700(14) 1 d D . P A 2
H8A H 0.4354 0.2436 0.6834 0.026 Uiso 0.4700(14) 1 calc R U P A 2
C9A C 0.5347(6) 0.2934(3) 0.6677(14) 0.0244(9) Uani 0.4700(14) 1 d D . P A 2
C10A C 0.6185(5) 0.2858(3) 0.6562(10) 0.0248(13) Uani 0.4700(14) 1 d D . P A 2
S1A S 0.64708(11) 0.22285(7) 0.6547(3) 0.0275(3) Uani 0.4700(14) 1 d D . P A 2
C11A C 0.5159(2) 0.34709(12) 0.6718(4) 0.0264(6) Uani 0.4700(14) 1 d D . P A 2
H11A H 0.4620 0.3602 0.6858 0.032 Uiso 0.4700(14) 1 calc R U P A 2
C12A C 0.5820(6) 0.3769(4) 0.6538(15) 0.025(2) Uani 0.4700(14) 1 d D . P A 2
H12A H 0.5796 0.4133 0.6441 0.030 Uiso 0.4700(14) 1 calc R U P A 2
S2A S 0.67218(12) 0.34245(7) 0.6502(4) 0.0360(4) Uani 0.4700(14) 1 d D . P A 2
C13 C 0.5982(2) 0.06940(13) 0.7080(7) 0.0453(11) Uani 1 1 d . . . . .
H13A H 0.5724 0.0543 0.6016 0.054 Uiso 1 1 calc R U . . .
H13B H 0.5692 0.0565 0.8139 0.054 Uiso 1 1 calc R U . . .
C14 C 0.6859(2) 0.05498(14) 0.7159(7) 0.0485(10) Uani 1 1 d . . . . .
H14A H 0.7137 0.0671 0.6089 0.073 Uiso 1 1 calc R U . . .
H14B H 0.6909 0.0175 0.7240 0.073 Uiso 1 1 calc R U . . .
H14C H 0.7112 0.0708 0.8201 0.073 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 2.016(3) . ?
W1 C2 2.032(3) . ?
W1 C3 2.046(3) . ?
W1 C4 2.047(3) . ?
W1 C5 2.047(3) . ?
W1 C6 2.214(3) . ?
C1 O1 1.144(4) . ?
C2 O2 1.141(4) . ?
C3 O3 1.134(4) . ?
C4 O4 1.138(4) . ?
C5 O5 1.139(4) . ?
C6 O6 1.328(4) . ?
C6 C7A 1.457(11) . ?
C6 C7 1.463(10) . ?
O6 C13 1.450(4) . ?
C7 C8 1.382(9) . ?
C7 S1 1.769(9) . ?
C8 C9 1.418(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(9) . ?
C9 C11 1.438(8) . ?
C10 S1 1.711(6) . ?
C10 S2 1.719(6) . ?
C11 C12 1.376(9) . ?
C11 H11 0.9500 . ?
C12 S2 1.739(9) . ?
C12 H12 0.9500 . ?
C7A S1A 1.765(10) . ?
C9A C10A 1.387(10) . ?
C10A S1A 1.703(7) . ?
C10A S2A 1.716(7) . ?
C12A S2A 1.727(10) . ?
C12A H12A 0.9500 . ?
C13 C14 1.485(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 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 C2 91.45(13) . . ?
C1 W1 C3 86.21(12) . . ?
C2 W1 C3 87.99(12) . . ?
C1 W1 C4 87.45(13) . . ?
C2 W1 C4 178.69(12) . . ?
C3 W1 C4 91.22(12) . . ?
C1 W1 C5 85.26(13) . . ?
C2 W1 C5 88.83(13) . . ?
C3 W1 C5 170.82(12) . . ?
C4 W1 C5 91.79(13) . . ?
C1 W1 C6 175.88(12) . . ?
C2 W1 C6 92.20(12) . . ?
C3 W1 C6 91.99(11) . . ?
C4 W1 C6 88.88(11) . . ?
C5 W1 C6 96.74(13) . . ?
O1 C1 W1 178.2(3) . . ?
O2 C2 W1 178.9(3) . . ?
O3 C3 W1 175.1(2) . . ?
O4 C4 W1 178.2(3) . . ?
O5 C5 W1 172.6(3) . . ?
O6 C6 C7A 106.0(4) . . ?
O6 C6 C7 105.6(4) . . ?
O6 C6 W1 128.6(2) . . ?
C7A C6 W1 125.0(4) . . ?
C7 C6 W1 125.5(4) . . ?
C6 O6 C13 122.0(2) . . ?
C8 C7 C6 127.8(7) . . ?
C8 C7 S1 112.3(6) . . ?
C6 C7 S1 119.4(5) . . ?
C7 C8 C9 112.3(6) . . ?
C7 C8 H8 123.9 . . ?
C9 C8 H8 123.9 . . ?
C10 C9 C8 111.5(6) . . ?
C10 C9 C11 112.1(6) . . ?
C8 C9 C11 136.3(7) . . ?
C9 C10 S1 114.2(5) . . ?
C9 C10 S2 113.3(5) . . ?
S1 C10 S2 132.4(4) . . ?
C10 S1 C7 89.6(4) . . ?
C12 C11 C9 110.3(6) . . ?
C12 C11 H11 124.8 . . ?
C9 C11 H11 124.8 . . ?
C11 C12 S2 114.3(6) . . ?
C11 C12 H12 122.8 . . ?
S2 C12 H12 122.8 . . ?
C10 S2 C12 89.8(4) . . ?
C6 C7A S1A 119.7(6) . . ?
C9A C10A S1A 114.1(5) . . ?
C9A C10A S2A 112.7(5) . . ?
S1A C10A S2A 133.2(5) . . ?
C10A S1A C7A 90.3(4) . . ?
S2A C12A H12A 123.5 . . ?
C10A S2A C12A 90.5(4) . . ?
O6 C13 C14 107.6(3) . . ?
O6 C13 H13A 110.2 . . ?
C14 C13 H13A 110.2 . . ?
O6 C13 H13B 110.2 . . ?
C14 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
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
C7A C6 O6 C13 -173.6(7) . . . . ?
C7 C6 O6 C13 172.5(6) . . . . ?
W1 C6 O6 C13 -1.1(5) . . . . ?
O6 C6 C7 C8 167.3(9) . . . . ?
C7A C6 C7 C8 74(3) . . . . ?
W1 C6 C7 C8 -18.8(13) . . . . ?
O6 C6 C7 S1 -3.5(9) . . . . ?
C7A C6 C7 S1 -97(3) . . . . ?
W1 C6 C7 S1 170.3(4) . . . . ?
C6 C7 C8 C9 -173.2(10) . . . . ?
S1 C7 C8 C9 -1.8(8) . . . . ?
C7 C8 C9 C10 -0.3(8) . . . . ?
C7 C8 C9 C11 -179.5(11) . . . . ?
C8 C9 C10 S1 2.4(9) . . . . ?
C11 C9 C10 S1 -178.3(5) . . . . ?
C8 C9 C10 S2 179.0(5) . . . . ?
C11 C9 C10 S2 -1.7(9) . . . . ?
C9 C10 S1 C7 -2.8(8) . . . . ?
S2 C10 S1 C7 -178.6(7) . . . . ?
C8 C7 S1 C10 2.6(7) . . . . ?
C6 C7 S1 C10 174.8(8) . . . . ?
C10 C9 C11 C12 -1.1(9) . . . . ?
C8 C9 C11 C12 178.1(9) . . . . ?
C9 C11 C12 S2 3.3(8) . . . . ?
C9 C10 S2 C12 2.9(7) . . . . ?
S1 C10 S2 C12 178.7(6) . . . . ?
C11 C12 S2 C10 -3.6(6) . . . . ?
O6 C6 C7A S1A 1.2(11) . . . . ?
C7 C6 C7A S1A 91(3) . . . . ?
W1 C6 C7A S1A -171.7(5) . . . . ?
C9A C10A S1A C7A 1.6(9) . . . . ?
S2A C10A S1A C7A -179.7(8) . . . . ?
C6 C7A S1A C10A -172.7(10) . . . . ?
C9A C10A S2A C12A -2.3(7) . . . . ?
S1A C10A S2A C12A 179.0(7) . . . . ?
C6 O6 C13 C14 177.7(4) . . . . ?

_shelxl_version_number           2013-4



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane, DCM'
