# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2007

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Howard Colquhoun'
_publ_contact_author_address     
;
School of Chemistry
The University of Reading
Whiteknights
Reading
RG6 6AD
UNITED KINGDOM
;

_publ_contact_author_email       H.M.COLQUHOUN@RDG.AC.UK

_publ_section_title              
;
Dithioacetalisation of PEEK: a general technique for
the solubilisation and characterisation of semi-crystalline aromatic
polyketones
;

_publ_section_references         
;
Oxford Diffraction Ltd, Crysalis Program (2005)

Oxford Diffraction Ltd, Abspack Program (2005)

Sheldrick, G.M. (1997) SHELXL program for crystallography refinement.
University of Gottingen, Germany.

Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands
;
loop_
_publ_author_name
'Howard Colquhoun'
'M. Drew'
'P. Hodge'
'Francois P. V. Paoloni'

data_1
_database_code_depnum_ccdc_archive 'CCDC 649151'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H32 O4 S4'
_chemical_formula_weight         728.92

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   34.218(6)
_cell_length_b                   11.2574(19)
_cell_length_c                   8.8953(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3426.5(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    22559
_cell_measurement_theta_min      2.98
_cell_measurement_theta_max      30.25

_exptl_crystal_description       needle
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         'not applicable'
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count 'not applicable'
_diffrn_standards_interval_time  10s
_diffrn_standards_decay_%        'not applicable'
_diffrn_reflns_number            22559
_diffrn_reflns_av_R_equivalents  0.2085
_diffrn_reflns_av_sigmaI/netI    0.2347
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         30.25
_reflns_number_total             5074
_reflns_number_gt                2168
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)

_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     
;
w=1/[\s^2^(Fo^2^)+(0.1858P)^2^+0.0000P] 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         5074
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2002
_refine_ls_R_factor_gt           0.0931
_refine_ls_wR_factor_ref         0.2881
_refine_ls_wR_factor_gt          0.2383
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_restrained_S_all      0.792
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.32517(14) 0.4541(4) 0.0017(5) 0.0245(11) Uani 1 1 d . . .
S101 S 0.28752(4) 0.42363(12) 0.14524(14) 0.0314(4) Uani 1 1 d . . .
C102 C 0.24963(18) 0.3682(7) 0.0212(7) 0.0512(17) Uani 1 1 d . . .
H10A H 0.2407 0.2913 0.0563 0.061 Uiso 1 1 calc R . .
H10B H 0.2275 0.4222 0.0222 0.061 Uiso 1 1 calc R . .
C103 C 0.26521(17) 0.3568(5) -0.1375(6) 0.0386(14) Uani 1 1 d . . .
H10C H 0.2438 0.3575 -0.2090 0.046 Uiso 1 1 calc R . .
H10D H 0.2794 0.2827 -0.1487 0.046 Uiso 1 1 calc R . .
S104 S 0.29721(4) 0.48043(12) -0.17145(15) 0.0332(4) Uani 1 1 d . . .
C11 C 0.35311(14) 0.3508(4) -0.0238(5) 0.0238(11) Uani 1 1 d . . .
C12 C 0.34866(14) 0.2373(4) 0.0366(6) 0.0261(11) Uani 1 1 d . . .
H12 H 0.3269 0.2203 0.0954 0.031 Uiso 1 1 calc R . .
C13 C 0.37628(16) 0.1492(4) 0.0102(6) 0.0298(12) Uani 1 1 d . . .
H13 H 0.3726 0.0738 0.0506 0.036 Uiso 1 1 calc R . .
C14 C 0.40886(14) 0.1723(4) -0.0748(5) 0.0226(10) Uani 1 1 d . . .
C15 C 0.41357(15) 0.2840(4) -0.1389(5) 0.0277(11) Uani 1 1 d . . .
H15 H 0.4351 0.2998 -0.1995 0.033 Uiso 1 1 calc R . .
C16 C 0.38599(14) 0.3717(4) -0.1120(5) 0.0268(11) Uani 1 1 d . . .
H16 H 0.3896 0.4465 -0.1540 0.032 Uiso 1 1 calc R . .
O17 O 0.43438(10) 0.0792(3) -0.0993(4) 0.0313(8) Uani 1 1 d . . .
C21 C 0.47363(14) 0.1060(4) -0.1285(5) 0.0239(11) Uani 1 1 d . . .
C22 C 0.49021(15) 0.0476(4) -0.2503(5) 0.0270(12) Uani 1 1 d . . .
H22 H 0.4751 -0.0013 -0.3112 0.032 Uiso 1 1 calc R . .
C23 C 0.53012(15) 0.0636(4) -0.2800(6) 0.0286(11) Uani 1 1 d . . .
H23 H 0.5417 0.0260 -0.3617 0.034 Uiso 1 1 calc R . .
C24 C 0.55197(15) 0.1354(4) -0.1870(5) 0.0265(11) Uani 1 1 d . . .
C25 C 0.53455(15) 0.1930(4) -0.0680(6) 0.0286(12) Uani 1 1 d . . .
H25 H 0.5495 0.2422 -0.0068 0.034 Uiso 1 1 calc R . .
C26 C 0.49569(15) 0.1789(4) -0.0386(5) 0.0279(11) Uani 1 1 d . . .
H26 H 0.4842 0.2184 0.0420 0.034 Uiso 1 1 calc R . .
O27 O 0.59177(10) 0.1420(3) -0.2196(4) 0.0369(9) Uani 1 1 d . . .
C31 C 0.61206(15) 0.2408(5) -0.1619(6) 0.0317(12) Uani 1 1 d . . .
C32 C 0.64126(16) 0.2244(5) -0.0630(7) 0.0360(13) Uani 1 1 d . . .
H32 H 0.6478 0.1479 -0.0325 0.043 Uiso 1 1 calc R . .
C33 C 0.66185(16) 0.3218(5) -0.0057(6) 0.0308(12) Uani 1 1 d . . .
H33 H 0.6812 0.3104 0.0662 0.037 Uiso 1 1 calc R . .
C35 C 0.62392(15) 0.4494(4) -0.1613(6) 0.0311(12) Uani 1 1 d . . .
H35 H 0.6180 0.5251 -0.1962 0.037 Uiso 1 1 calc R . .
C34 C 0.65343(14) 0.4346(5) -0.0558(6) 0.0277(11) Uani 1 1 d . . .
C36 C 0.60325(16) 0.3528(5) -0.2152(6) 0.0333(13) Uani 1 1 d . . .
H36 H 0.5836 0.3631 -0.2864 0.040 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.026(3) 0.027(3) 0.021(2) -0.0008(19) -0.004(2) 0.005(2)
S101 0.0288(7) 0.0370(8) 0.0283(7) -0.0037(6) 0.0064(5) -0.0028(6)
C102 0.031(3) 0.070(5) 0.053(4) -0.009(3) -0.001(3) -0.012(3)
C103 0.040(3) 0.032(3) 0.043(3) -0.010(3) -0.013(3) -0.004(3)
S104 0.0393(8) 0.0354(8) 0.0249(7) -0.0012(6) -0.0084(6) 0.0063(6)
C11 0.025(3) 0.025(3) 0.022(2) 0.001(2) -0.002(2) -0.003(2)
C12 0.023(3) 0.028(3) 0.027(3) 0.000(2) 0.004(2) -0.002(2)
C13 0.040(3) 0.021(3) 0.028(3) 0.001(2) 0.000(2) 0.002(2)
C14 0.024(3) 0.020(2) 0.024(2) -0.0062(19) -0.002(2) 0.001(2)
C15 0.025(3) 0.034(3) 0.024(3) 0.002(2) 0.006(2) 0.003(2)
C16 0.030(3) 0.025(2) 0.026(3) -0.002(2) 0.001(2) 0.000(2)
O17 0.0273(19) 0.0265(19) 0.040(2) -0.0070(16) 0.0005(16) 0.0044(16)
C21 0.031(3) 0.022(2) 0.019(2) 0.0059(19) 0.000(2) 0.006(2)
C22 0.039(3) 0.016(2) 0.026(3) -0.0036(19) -0.002(2) -0.001(2)
C23 0.035(3) 0.023(3) 0.027(3) 0.000(2) -0.003(2) 0.001(2)
C24 0.030(3) 0.021(2) 0.028(3) 0.003(2) 0.001(2) 0.003(2)
C25 0.036(3) 0.020(2) 0.030(3) -0.002(2) -0.009(2) 0.000(2)
C26 0.031(3) 0.031(3) 0.022(2) -0.005(2) 0.004(2) 0.003(2)
O27 0.028(2) 0.032(2) 0.051(2) -0.0179(18) 0.0055(17) -0.0065(16)
C31 0.033(3) 0.026(3) 0.036(3) -0.010(2) 0.012(2) -0.002(2)
C32 0.038(3) 0.021(3) 0.049(4) -0.002(2) 0.004(3) 0.004(2)
C33 0.036(3) 0.023(3) 0.033(3) 0.002(2) -0.003(2) 0.008(2)
C35 0.039(3) 0.022(2) 0.032(3) 0.000(2) -0.009(2) 0.003(2)
C34 0.027(3) 0.028(3) 0.028(3) -0.007(2) 0.002(2) 0.001(2)
C36 0.042(3) 0.030(3) 0.028(3) -0.010(2) -0.009(2) 0.003(2)

_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
C1 C11 1.522(7) . ?
C1 C34 1.529(7) 5_665 ?
C1 S104 1.837(5) . ?
C1 S101 1.846(5) . ?
S101 C102 1.813(6) . ?
C102 C103 1.514(8) . ?
C103 S104 1.796(6) . ?
C11 C16 1.391(7) . ?
C11 C12 1.394(7) . ?
C12 C13 1.390(7) . ?
C13 C14 1.372(7) . ?
C14 O17 1.382(6) . ?
C14 C15 1.390(7) . ?
C15 C16 1.386(7) . ?
O17 C21 1.401(6) . ?
C21 C26 1.372(7) . ?
C21 C22 1.389(7) . ?
C22 C23 1.403(7) . ?
C23 C24 1.377(7) . ?
C24 C25 1.377(7) . ?
C24 O27 1.394(6) . ?
C25 C26 1.365(7) . ?
O27 C31 1.409(6) . ?
C31 C32 1.344(8) . ?
C31 C36 1.379(7) . ?
C32 C33 1.400(7) . ?
C33 C34 1.376(7) . ?
C35 C36 1.383(7) . ?
C35 C34 1.389(7) . ?
C34 C1 1.529(7) 5_665 ?

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
C11 C1 C34 111.9(4) . 5_665 ?
C11 C1 S104 109.0(3) . . ?
C34 C1 S104 112.4(3) 5_665 . ?
C11 C1 S101 113.5(3) . . ?
C34 C1 S101 105.6(3) 5_665 . ?
S104 C1 S101 104.3(2) . . ?
C102 S101 C1 98.1(2) . . ?
C103 C102 S101 110.2(4) . . ?
C102 C103 S104 107.8(4) . . ?
C103 S104 C1 93.0(2) . . ?
C16 C11 C12 117.4(4) . . ?
C16 C11 C1 117.6(4) . . ?
C12 C11 C1 125.0(4) . . ?
C13 C12 C11 121.0(5) . . ?
C14 C13 C12 120.7(5) . . ?
O17 C14 C13 117.2(4) . . ?
O17 C14 C15 123.2(4) . . ?
C13 C14 C15 119.5(4) . . ?
C14 C15 C16 119.6(5) . . ?
C11 C16 C15 121.8(5) . . ?
C14 O17 C21 118.2(4) . . ?
C26 C21 C22 120.9(5) . . ?
C26 C21 O17 123.2(4) . . ?
C22 C21 O17 115.8(4) . . ?
C21 C22 C23 119.0(5) . . ?
C24 C23 C22 119.4(5) . . ?
C23 C24 C25 120.2(5) . . ?
C23 C24 O27 115.9(4) . . ?
C25 C24 O27 123.9(5) . . ?
C26 C25 C24 121.0(5) . . ?
C25 C26 C21 119.6(5) . . ?
C24 O27 C31 116.6(4) . . ?
C32 C31 C36 120.9(5) . . ?
C32 C31 O27 119.7(5) . . ?
C36 C31 O27 119.3(5) . . ?
C31 C32 C33 120.3(5) . . ?
C34 C33 C32 120.0(5) . . ?
C36 C35 C34 120.8(5) . . ?
C33 C34 C35 118.8(5) . . ?
C33 C34 C1 123.6(5) . 5_665 ?
C35 C34 C1 117.5(4) . 5_665 ?
C31 C36 C35 119.2(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
C11 C1 S101 C102 -92.4(4) . . . . ?
C34 C1 S101 C102 144.7(4) 5_665 . . . ?
S104 C1 S101 C102 26.0(3) . . . . ?
C1 S101 C102 C103 6.3(5) . . . . ?
S101 C102 C103 S104 -37.9(6) . . . . ?
C102 C103 S104 C1 50.9(4) . . . . ?
C11 C1 S104 C103 77.7(4) . . . . ?
C34 C1 S104 C103 -157.7(4) 5_665 . . . ?
S101 C1 S104 C103 -43.8(3) . . . . ?
C34 C1 C11 C16 -50.8(6) 5_665 . . . ?
S104 C1 C11 C16 74.1(5) . . . . ?
S101 C1 C11 C16 -170.1(3) . . . . ?
C34 C1 C11 C12 128.0(5) 5_665 . . . ?
S104 C1 C11 C12 -107.1(5) . . . . ?
S101 C1 C11 C12 8.7(6) . . . . ?
C16 C11 C12 C13 0.5(7) . . . . ?
C1 C11 C12 C13 -178.3(4) . . . . ?
C11 C12 C13 C14 0.7(8) . . . . ?
C12 C13 C14 O17 -178.2(4) . . . . ?
C12 C13 C14 C15 -2.1(7) . . . . ?
O17 C14 C15 C16 178.1(4) . . . . ?
C13 C14 C15 C16 2.2(7) . . . . ?
C12 C11 C16 C15 -0.3(7) . . . . ?
C1 C11 C16 C15 178.5(4) . . . . ?
C14 C15 C16 C11 -1.0(7) . . . . ?
C13 C14 O17 C21 -154.3(4) . . . . ?
C15 C14 O17 C21 29.7(6) . . . . ?
C14 O17 C21 C26 51.7(6) . . . . ?
C14 O17 C21 C22 -132.4(4) . . . . ?
C26 C21 C22 C23 0.4(7) . . . . ?
O17 C21 C22 C23 -175.6(4) . . . . ?
C21 C22 C23 C24 0.7(7) . . . . ?
C22 C23 C24 C25 -1.4(7) . . . . ?
C22 C23 C24 O27 176.9(4) . . . . ?
C23 C24 C25 C26 1.0(8) . . . . ?
O27 C24 C25 C26 -177.2(5) . . . . ?
C24 C25 C26 C21 0.2(8) . . . . ?
C22 C21 C26 C25 -0.9(7) . . . . ?
O17 C21 C26 C25 174.8(4) . . . . ?
C23 C24 O27 C31 159.7(5) . . . . ?
C25 C24 O27 C31 -22.0(7) . . . . ?
C24 O27 C31 C32 117.7(5) . . . . ?
C24 O27 C31 C36 -66.4(6) . . . . ?
C36 C31 C32 C33 3.6(8) . . . . ?
O27 C31 C32 C33 179.5(5) . . . . ?
C31 C32 C33 C34 -3.0(8) . . . . ?
C32 C33 C34 C35 1.1(8) . . . . ?
C32 C33 C34 C1 -178.9(5) . . . 5_665 ?
C36 C35 C34 C33 0.1(8) . . . . ?
C36 C35 C34 C1 -179.9(5) . . . 5_665 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        30.25
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.112

#===END