Synthesis and characterization of semiaromatic polyamides comprising benzofurobenzofuran repeating units
Cretenoud, Julien; Özen, Bilal; Schmaltz, Thomas; Görl, Daniel; Fabrizio, Alberto; Corminboeuf, Clémence; Fadaei Tirani, Farzaneh; Scopelliti, Rosario; Frauenrath, Holger; Polym. Chem. 8 (2017) 2197–; doi:10.1039/C7PY00129K

data_1545522
_publ_section_title
;
 Synthesis and characterization of semiaromatic polyamides comprising
 benzofurobenzofuran repeating units
;
_journal_issue                   14
_journal_name_full               'Polym. Chem.'
_journal_page_first              2197
_journal_paper_doi               10.1039/C7PY00129K
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C22 H24 N2 O5, 1.5(C2 H6 O)'
_chemical_formula_sum            'C25 H33 N2 O6.5'
_chemical_formula_weight         465.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-01-18 deposited with the CCDC.
2017-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.789(2)
_cell_angle_beta                 103.313(3)
_cell_angle_gamma                109.953(2)
_cell_formula_units_Z            4
_cell_length_a                   10.1910(3)
_cell_length_b                   13.7072(3)
_cell_length_c                   19.0724(5)
_cell_measurement_reflns_used    10960
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.5850
_cell_measurement_theta_min      3.9640
_cell_volume                     2424.55(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -57.00  31.00   1.00    1.00    --  -42.26  57.00 -90.00   88
  2  \w     30.00  83.00   1.00    1.00    --   42.26-125.00-180.00   53
  3  \w     37.00 122.00   1.00    1.00    --  110.51-125.00-180.00   85
  4  \w     76.00 122.00   1.00    1.00    --  110.51-125.00 -30.00   46
  5  \w     54.00  80.00   1.00    1.00    --  110.51 -94.00   0.00   26
  6  \w     45.00  78.00   1.00    1.00    --  110.51 -61.00  60.00   33
  7  \w     42.00 108.00   1.00    1.00    --  110.51 -94.00  30.00   66
  8  \w     35.00 136.00   1.00    1.00    --  110.51 -30.00 -30.00  101
  9  \w    117.00 178.00   1.00    1.00    --  110.51  45.00 -30.00   61
 10  \w    122.00 178.00   1.00    1.00    --  110.51 125.00 -30.00   56
 11  \w    117.00 159.00   1.00    1.00    --  110.51 117.00 -65.00   42
 12  \w     38.00 136.00   1.00    1.00    --  110.51 -45.00-120.00   98
 13  \w     32.00  83.00   1.00    1.00    --   42.26-125.00  30.00   51
 14  \w     23.00  50.00   1.00    1.00    --   42.26-125.00 120.00   27
 15  \w     34.00 159.00   1.00    1.00    --  110.51 -15.00 150.00  125
 16  \w     29.00  78.00   1.00    1.00    --  110.51 -94.00 -90.00   49
 17  \w   -130.00  42.00   1.00    1.00    --  -42.26   0.00 -90.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17613
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.154
_diffrn_reflns_theta_min         3.448
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       irregular
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.545
_exptl_crystal_size_mid          0.445
_exptl_crystal_size_min          0.360
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         9787
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.4636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8567
_reflns_number_total             9787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7py00129k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
Adding full bibliography for 1545521--1545522.cif.

2019-07-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2424.57(12)
_cod_original_formula_moiety     '2(C22 H24 N2 O5), 3(C2 H6 O)'
_cod_original_formula_sum        'C50 H66 N4 O13'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     931.06
_cod_database_code               1545522
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              92675