Dithioacetalisation of PEEK: a general technique for the solubilisation and characterisation of semi-crystalline aromatic polyketones
Colquhoun, Howard M.; Paoloni, Francois P. V.; Drew, Michael G. B.; Hodge, Philip; Chemical Communications (Cambridge, United Kingdom)  (2007) 3365–3367; doi:10.1039/b708116b

data_7102083
_publ_section_title
;
 Dithioacetalisation of PEEK: a general technique for the solubilisation
 and characterisation of semi-crystalline aromatic polyketones
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   32
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              3365
_journal_page_last               3367
_journal_paper_doi               10.1039/b708116b
_journal_year                    2007
_chemical_formula_sum            'C42 H32 O4 S4'
_chemical_formula_weight         728.92
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.218(6)
_cell_length_b                   11.2574(19)
_cell_length_c                   8.8953(15)
_cell_measurement_reflns_used    22559
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.25
_cell_measurement_theta_min      2.98
_cell_volume                     3426.5(10)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2085
_diffrn_reflns_av_sigmaI/netI    0.2347
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22559
_diffrn_reflns_theta_full        30.25
_diffrn_reflns_theta_max         30.25
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        'not applicable'
_diffrn_standards_interval_count 'not applicable'
_diffrn_standards_interval_time  10s
_diffrn_standards_number         'not applicable'
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.792
_refine_ls_R_factor_all          0.2002
_refine_ls_R_factor_gt           0.0931
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.1858P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2383
_refine_ls_wR_factor_ref         0.2881
_reflns_number_gt                2168
_reflns_number_total             5074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708116b.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7102083