# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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data_mo_bvdwcrthoet_0m
_database_code_depnum_ccdc_archive 'CCDC 913650'
#TrackingRef 'web_deposit_cif_file_0_DavidC.Liles_1354520600.mo_BvdWCrThOEt.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Pentacarbonyl(ethoxy-thiophenyl-methylidene)chromium
;
_chemical_name_common            .
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 Cr1 O6 S1'
_chemical_formula_sum            'C12 H8 Cr1 O6 S1'
_chemical_formula_weight         332.25
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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/m'
_symmetry_space_group_name_Hall  '-P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
_cell_length_a                   9.5803(6)
_cell_length_b                   7.6532(5)
_cell_length_c                   9.6551(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.737(3)
_cell_angle_gamma                90.00
_cell_volume                     699.70(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9987
_cell_measurement_theta_min      2.790
_cell_measurement_theta_max      26.046
_exptl_crystal_description       hexagonal-prism
_exptl_crystal_colour            dark-orange
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.118
_exptl_crystal_density_meas      .
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             336
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6769
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'I\ms micro focus'
_diffrn_radiation_monochromator  'Quazar multi-layer optics'
_diffrn_measurement_device_type  'Bruker kappa Proton CMOS'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            20399
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         26.13
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.13
_diffrn_measured_fraction_theta_full 0.998
_reflns_number_total             1497
_reflns_number_gt                1330
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
; <i>ORTEP-3 for Windows</i> (Farrugia, 1997), <i>POV-RAY</i> (Cason, 2004),
<i>Mercury</i> (Macrae <i>et al</i>., 2008)
;
_computing_publication_material  '<i>SHELXL-97</i>, <i>PLATON</i> (Spek, 2009)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0878P)^2^+3.5878P] where P=(Fo^2^+2Fc^2^)/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         1497
_refine_ls_number_parameters     122
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0787
_refine_ls_wR_factor_ref         0.2371
_refine_ls_wR_factor_gt          0.2325
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_restrained_S_all      1.199
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.122
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.28935(14) 0.2500 0.29276(14) 0.0370(5) Uani 1 2 d S . 1
C1 C 0.4424(9) 0.2500 0.4455(10) 0.049(2) Uani 1 2 d S . 1
O1 O 0.5269(9) 0.2500 0.5290(9) 0.091(3) Uani 1 2 d S . 1
C2 C 0.2046(7) 0.4261(9) 0.3884(7) 0.0495(15) Uani 1 1 d . . 1
O2 O 0.1625(6) 0.5345(8) 0.4540(7) 0.0800(18) Uani 1 1 d . . 1
C3 C 0.3841(7) 0.4298(9) 0.2069(6) 0.0492(15) Uani 1 1 d . . 1
O3 O 0.4458(7) 0.5359(8) 0.1619(7) 0.0846(19) Uani 1 1 d . . 1
C4 C 0.1217(9) 0.2500 0.1287(9) 0.0425(19) Uani 1 2 d S . 1
O4 O -0.0169(7) 0.2500 0.1321(7) 0.0545(17) Uani 1 2 d S . 1
S1 S -0.0085(4) 0.2500 -0.1454(4) 0.0434(14) Uani 0.526(8) 2 d SP . 1
C5 C 0.1360(8) 0.2500 -0.0163(8) 0.0326(16) Uani 1 2 d S . 1
C6 C 0.2616(10) 0.2500 -0.0784(9) 0.049(2) Uani 1 2 d S . 1
H6 H 0.3528 0.2500 -0.0290 0.059 Uiso 1 2 calc SR . 1
C7 C 0.2268(15) 0.2500 -0.2277(11) 0.068(3) Uani 1 2 d S . 1
H7 H 0.2945 0.2500 -0.2872 0.082 Uiso 1 2 calc SR . 1
C8 C 0.0973(19) 0.2500 -0.2708(16) 0.046(4) Uani 0.526(8) 2 d SP . 1
H8 H 0.0612 0.2500 -0.3658 0.055 Uiso 1 2 calc SR . 1
C9 C -0.0790(10) 0.2500 0.2561(11) 0.052(2) Uani 1 2 d S . 1
H9A H -0.0498 0.3529 0.3117 0.063 Uiso 0.50 1 calc PR . 1
H9B H -0.0498 0.1471 0.3117 0.063 Uiso 0.50 1 calc PR . 1
C10 C -0.2358(11) 0.2500 0.2136(15) 0.068(3) Uani 1 2 d S . 1
H10A H -0.2809 0.2500 0.2958 0.102 Uiso 1 2 calc SR . 1
H10B H -0.2635 0.1476 0.1589 0.102 Uiso 0.50 1 calc PR . 1
H10C H -0.2635 0.3524 0.1589 0.102 Uiso 0.50 1 calc PR . 1
S1A S -0.1462(7) 0.2500 -0.0095(8) 0.078(2) Uani 0.474(8) 2 d SP . 2
C8A C -0.275(3) 0.2500 0.090(3) 0.084(9) Uani 0.474(8) 2 d SP . 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cr1 0.0383(8) 0.0348(7) 0.0378(8) 0.000 0.0057(5) 0.000
C1 0.036(4) 0.061(6) 0.045(5) 0.000 -0.005(4) 0.000
O1 0.067(5) 0.129(9) 0.069(5) 0.000 -0.020(5) 0.000
C2 0.047(3) 0.046(3) 0.057(4) -0.003(3) 0.011(3) -0.003(3)
O2 0.073(4) 0.065(4) 0.107(5) -0.028(3) 0.031(3) 0.000(3)
C3 0.060(4) 0.046(3) 0.043(3) -0.004(3) 0.011(3) -0.012(3)
O3 0.112(5) 0.069(4) 0.080(4) 0.001(3) 0.034(4) -0.032(4)
C4 0.045(4) 0.039(4) 0.045(5) 0.000 0.011(4) 0.000
O4 0.045(3) 0.061(4) 0.058(4) 0.000 0.006(3) 0.000
S1 0.039(2) 0.062(3) 0.028(2) 0.000 0.0031(15) 0.000
C5 0.038(4) 0.030(4) 0.030(4) 0.000 0.004(3) 0.000
C6 0.049(5) 0.065(6) 0.036(4) 0.000 0.012(4) 0.000
C7 0.099(9) 0.068(7) 0.047(6) 0.000 0.037(6) 0.000
C8 0.053(10) 0.063(11) 0.021(7) 0.000 0.005(6) 0.000
C9 0.042(5) 0.061(6) 0.055(5) 0.000 0.012(4) 0.000
C10 0.045(5) 0.066(7) 0.097(9) 0.000 0.027(6) 0.000
S1A 0.059(4) 0.087(5) 0.084(5) 0.000 -0.007(3) 0.000
C8A 0.087(19) 0.069(17) 0.082(19) 0.000 -0.028(15) 0.000
_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 C2 1.886(7) 4_565 ?
Cr1 C2 1.886(7) . ?
Cr1 C3 1.907(7) . ?
Cr1 C3 1.907(7) 4_565 ?
Cr1 C1 1.915(9) . ?
Cr1 C4 2.077(9) . ?
C1 O1 1.052(11) . ?
C2 O2 1.153(8) . ?
C3 O3 1.129(8) . ?
C4 O4 1.333(11) . ?
C4 C5 1.428(11) . ?
O4 C9 1.415(11) . ?
S1 C8 1.693(16) . ?
S1 C5 1.716(8) . ?
C5 C6 1.423(12) . ?
C6 C7 1.429(14) . ?
C6 H6 0.9300 . ?
C7 C8 1.25(2) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.495(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
S1A C8A 1.68(4) . ?
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 Cr1 C2 91.2(4) 4_565 . ?
C2 Cr1 C3 176.2(3) 4_565 . ?
C2 Cr1 C3 88.1(3) . . ?
C2 Cr1 C3 88.1(3) 4_565 4_565 ?
C2 Cr1 C3 176.2(3) . 4_565 ?
C3 Cr1 C3 92.4(4) . 4_565 ?
C2 Cr1 C1 87.7(3) 4_565 . ?
C2 Cr1 C1 87.7(3) . . ?
C3 Cr1 C1 88.6(3) . . ?
C3 Cr1 C1 88.6(3) 4_565 . ?
C2 Cr1 C4 91.9(3) 4_565 . ?
C2 Cr1 C4 91.9(3) . . ?
C3 Cr1 C4 91.9(3) . . ?
C3 Cr1 C4 91.9(3) 4_565 . ?
C1 Cr1 C4 179.3(4) . . ?
O1 C1 Cr1 179.7(10) . . ?
O2 C2 Cr1 174.7(6) . . ?
O3 C3 Cr1 176.4(7) . . ?
O4 C4 C5 105.6(7) . . ?
O4 C4 Cr1 129.7(6) . . ?
C5 C4 Cr1 124.7(6) . . ?
C4 O4 C9 124.7(8) . . ?
C8 S1 C5 90.8(7) . . ?
C4 C5 C6 128.8(8) . . ?
C4 C5 S1 121.7(6) . . ?
C6 C5 S1 109.5(6) . . ?
C7 C6 C5 110.0(9) . . ?
C7 C6 H6 125.0 . . ?
C5 C6 H6 125.0 . . ?
C8 C7 C6 113.8(11) . . ?
C8 C7 H7 123.1 . . ?
C6 C7 H7 123.1 . . ?
C7 C8 S1 115.8(12) . . ?
C7 C8 H8 122.1 . . ?
S1 C8 H8 122.1 . . ?
O4 C9 C10 107.6(9) . . ?
O4 C9 H9A 110.2 . . ?
C10 C9 H9A 110.2 . . ?
O4 C9 H9B 110.2 . . ?
C10 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 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
C2 Cr1 C4 O4 45.6(2) 4_565 . . . ?
C2 Cr1 C4 O4 -45.6(2) . . . . ?
C3 Cr1 C4 O4 -133.8(2) . . . . ?
C3 Cr1 C4 O4 133.8(2) 4_565 . . . ?
C2 Cr1 C4 C5 -134.4(2) 4_565 . . . ?
C2 Cr1 C4 C5 134.4(2) . . . . ?
C3 Cr1 C4 C5 46.2(2) . . . . ?
C3 Cr1 C4 C5 -46.2(2) 4_565 . . . ?
C5 C4 O4 C9 180.0 . . . . ?
O4 C4 C5 C6 180.0 . . . . ?
Cr1 C4 C5 C6 0.0 . . . . ?
O4 C4 C5 S1 0.0 . . . . ?
Cr1 C4 C5 S1 180.0 . . . . ?
C8 S1 C5 C4 180.0 . . . . ?
C8 S1 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 180.0 . . . . ?
S1 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 S1 0.0 . . . . ?
C5 S1 C8 C7 0.00 . . . . ?
C4 O4 C9 C10 180.0 . . . . ?
_iucr_refine_instructions_details 
;
TITL mo_BvdWCrThOEt_0m in P2(1)/m
CELL 0.71073 9.5803 7.6532 9.6551 90.000 98.737 90.000
ZERR 2.00 0.0006 0.0005 0.0006 0.000 0.003 0.000
LATT 1
SYMM -x, y+1/2, -z
SFAC C H O S Cr
UNIT 24 16 12 2 2
L.S. 16
ACTA
BOND $H
FMAP 2
PLAN 5
HTAB
CONF
TEMP 23.000
WGHT 0.087800 3.587800
FVAR 0.89647 0.52591
PART 1
CR1 5 0.289351 0.250000 0.292758 10.50000 0.03834 0.03485 =
0.03777 0.00000 0.00565 0.00000
C1 1 0.442393 0.250000 0.445472 10.50000 0.03649 0.06147 =
0.04500 0.00000 -0.00539 0.00000
O1 3 0.526883 0.250000 0.528986 10.50000 0.06677 0.12886 =
0.06903 0.00000 -0.01952 0.00000
C2 1 0.204578 0.426065 0.388432 11.00000 0.04688 0.04577 =
0.05691 -0.00325 0.01116 -0.00310
O2 3 0.162478 0.534508 0.454008 11.00000 0.07300 0.06515 =
0.10697 -0.02750 0.03054 0.00046
C3 1 0.384126 0.429827 0.206863 11.00000 0.06001 0.04582 =
0.04281 -0.00369 0.01144 -0.01163
O3 3 0.445787 0.535873 0.161883 11.00000 0.11164 0.06854 =
0.07965 0.00078 0.03433 -0.03176
C4 1 0.121715 0.250000 0.128727 10.50000 0.04455 0.03910 =
0.04514 0.00000 0.01079 0.00000
O4 3 -0.016866 0.250000 0.132122 10.50000 0.04481 0.06057 =
0.05750 0.00000 0.00575 0.00000
S1 4 -0.008497 0.250000 -0.145393 20.50000 0.03950 0.06196 =
0.02808 0.00000 0.00315 0.00000
C5 1 0.136015 0.250000 -0.016323 10.50000 0.03812 0.02979 =
0.02955 0.00000 0.00415 0.00000
C6 1 0.261569 0.250000 -0.078373 10.50000 0.04862 0.06451 =
0.03639 0.00000 0.01164 0.00000
AFIX 43
H6 2 0.352837 0.250000 -0.029037 10.50000 -1.20000
AFIX 0
C7 1 0.226804 0.250000 -0.227671 10.50000 0.09921 0.06771 =
0.04657 0.00000 0.03742 0.00000
AFIX 43
H7 2 0.294532 0.250000 -0.287218 10.50000 -1.20000
AFIX 0
C8 1 0.097317 0.250000 -0.270752 20.50000 0.05286 0.06252 =
0.02093 0.00000 0.00479 0.00000
AFIX 43
H8 2 0.061167 0.250000 -0.365760 10.50000 -1.20000
AFIX 0
C9 1 -0.079017 0.250000 0.256053 10.50000 0.04223 0.06134 =
0.05502 0.00000 0.01246 0.00000
AFIX 23
H9A 2 -0.049791 0.352852 0.311694 10.50000 -1.20000
H9B 2 -0.049791 0.147148 0.311693 10.50000 -1.20000
AFIX 0
C10 1 -0.235760 0.250000 0.213610 10.50000 0.04467 0.06605 =
0.09739 0.00000 0.02661 0.00000
AFIX 33
H10A 2 -0.280918 0.250000 0.295824 10.50000 -1.50000
H10B 2 -0.263496 0.147580 0.158878 10.50000 -1.50000
H10C 2 -0.263496 0.352420 0.158878 10.50000 -1.50000
PART 2
AFIX 0
S1A 4 -0.146188 0.250000 -0.009502 -20.50000 0.05892 0.08654 =
0.08380 0.00000 -0.00685 0.00000
C8A 1 -0.275321 0.250000 0.089829 -20.50000 0.08670 0.06949 =
0.08215 0.00000 -0.02801 0.00000
PART
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM mo_BvdWCrThOEt_0m in P2(1)/m
REM R1 = 0.0787 for 1330 Fo > 4sig(Fo) and 0.0861 for all 1497 data
REM 122 parameters refined using 0 restraints
END
;
_iucr_refine_reflections_details 
;
-1 0 0 43.8684 2.15487 11
-2 0 0 645.393 30.7456 2
2 0 0 672.555 30.5001 3
2 0 0 710.386 30.5457 3
2 0 0 786.161 38.7620 4
2 0 0 661.230 32.8337 6
2 0 0 668.521 31.7394 7
2 0 0 774.175 33.9252 9
-2 0 0 600.916 32.8100 6
-2 0 0 651.732 31.7235 7
-2 0 0 767.394 33.9202 9
-2 0 0 738.336 30.3638 11
-2 0 0 717.446 29.9773 13
2 0 0 659.210 30.7634 2
2 0 0 732.187 30.3703 11
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;