Macrocyclic oligomers of the aromatic polyetherketone “PK99”: synthesis, fractionation, structural characterisation and ring-opening polymerisation
Baxter, Ian; Colquhoun, Howard M.; Hodge, Philip; Kohnke, Franz H.; Lewis, David F.; Williams, David J.; Journal of Materials Chemistry 10 (2000) 309–; doi:10.1039/a908414b

data_7203940
_publ_section_title
;
 Macrocyclic oligomers of the aromatic polyetherketone
 &#x201C;PK99&#x201D;: synthesis, fractionation, structural
 characterisation and ring-opening polymerisation
;
_journal_issue                   2
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              309
_journal_paper_doi               10.1039/a908414b
_journal_volume                  10
_journal_year                    2000
_chemical_formula_sum            'C66 H44 Cl4 O8'
_chemical_formula_weight         1106.81
_chemical_name_systematic
; 
 ? 
;
_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                107.851(5)
_cell_angle_beta                 100.953(5)
_cell_angle_gamma                96.477(7)
_cell_formula_units_Z            1
_cell_length_a                   10.8001(9)
_cell_length_b                   11.0160(9)
_cell_length_c                   12.4143(9)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.96
_cell_measurement_theta_min      11.02
_cell_volume                     1356.9(2)
_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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4421
_diffrn_reflns_theta_max         62.00
_diffrn_reflns_theta_min         3.85
_diffrn_standards_decay_%        5.86
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.458
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       prism
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0023(6)
_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   1.042
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3852
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_obs          0.0638
_refine_ls_shift/esd_max         -0.020
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0914P)^2^+0.4939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2081
_refine_ls_wR_factor_obs         0.1754
_reflns_number_observed          3173
_reflns_number_total             4171
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908414b.txt
_cod_data_source_block           f9701
_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^)+(0.0914P)^2^+0.4939P] 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^)+(0.0914P)^2^+0.4939P] 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_database_code               7203940