Cyclic oligomers of poly(ether ketone) (PEK): synthesis, extraction from polymer, fractionation, and characterisation of the cyclic trimer, tetramer and pentamer
Ben-Haida, Abderrazak; Colquhoun, Howard M.; Hodge, Philip; Williams, David J.; Journal of Materials Chemistry 10 (2000) 2011–; doi:10.1039/b000738m

data_7203966
_publ_section_title
;
 Cyclic oligomers of poly(ether ketone) (PEK): synthesis, extraction
 from polymer, fractionation, and characterisation of the cyclic
 trimer, tetramer and pentamer
;
_journal_issue                   9
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2011
_journal_paper_doi               10.1039/b000738m
_journal_volume                  10
_journal_year                    2000
_chemical_formula_sum            'C53.5 H35 Cl3 O8'
_chemical_formula_weight         912.17
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                75.262(4)
_cell_angle_beta                 73.004(5)
_cell_angle_gamma                80.202(4)
_cell_formula_units_Z            1
_cell_length_a                   8.7603(5)
_cell_length_b                   10.1072(5)
_cell_length_c                   14.0404(8)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.94
_cell_measurement_theta_min      11.05
_cell_volume                     1143.57(11)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3938
_diffrn_reflns_theta_max         62.49
_diffrn_reflns_theta_min         3.37
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.272
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       needles
_exptl_crystal_F_000             471
_exptl_crystal_size_max          .93
_exptl_crystal_size_mid          .33
_exptl_crystal_size_min          .05
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0028(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.070
_refine_ls_goodness_of_fit_obs   1.124
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         3389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_restrained_S_obs      1.124
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_obs          0.0609
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1060P)^2^+0.3610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2084
_refine_ls_wR_factor_obs         0.1741
_reflns_number_observed          2816
_reflns_number_total             3635
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000738m.txt
_cod_data_source_block           hmc9814
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1060P)^2^+0.3610P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1060P)^2^+0.3610P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C53.50 H35 Cl3 O8'
_cod_database_code               7203966