Synthesis of perfectly alternating copolymers for polymers of intrinsic microporosity
Zhang, Jian; Jin, Jianyong; Cooney, Ralph; Fu, Qiang; Qiao, Greg G.; Thomas, Sylvie; Merkel, Tim C.; Polym. Chem. 6 (2015) 5003–; doi:10.1039/C5PY00570A

data_1520502
_publ_section_title
;
 Synthesis of perfectly alternating copolymers for polymers of intrinsic
 microporosity
;
_journal_issue                   28
_journal_name_full               'Polym. Chem.'
_journal_page_first              5003
_journal_paper_doi               10.1039/C5PY00570A
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C37 H20 F4 N4 O4'
_chemical_formula_sum            'C37 H20 F4 N4 O4'
_chemical_formula_weight         660.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-12-18
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_audit_update_record
;
2015-03-27 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.514(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.674(3)
_cell_length_b                   10.0584(12)
_cell_length_c                   13.4593(16)
_cell_measurement_temperature    372(2)
_cell_volume                     3027.4(7)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      372(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2020
_diffrn_reflns_av_unetI/netI     0.1246
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58522
_diffrn_reflns_theta_full        28.15
_diffrn_reflns_theta_max         28.15
_diffrn_reflns_theta_min         0.91
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1490 before and 0.1141 after correction.
The Ratio of minimum to maximum transmission is 0.5341.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.0079(13)
_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_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0953P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.2117
_reflns_number_gt                3538
_reflns_number_total             7260
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5py00570a2.cif
_cod_data_source_block           abam1
_cod_depositor_comments          'Adding full bibliography for 1520502.cif.'
_cod_original_cell_volume        3027.4(6)
_cod_database_code               1520502
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H16A(0.055) H16B(0.055) H16C(0.055) H17A(0.055) H17B(0.055)
 H17C(0.055) H18A(0.038) H18B(0.038) H20A(0.037) H20B(0.037) H22A(0.057)
 H22B(0.057) H22C(0.057) H23A(0.056) H23B(0.056) H23C(0.056)
 Fixed X: H16A(0.2308) H16B(0.2531) H16C(0.185) H17A(0.1589) H17B(0.2267)
 H17C(0.1882) H18A(0.2929) H18B(0.2899) H20A(0.2404) H20B(0.2067) H22A(0.3835)
 H22B(0.3351) H22C(0.3581) H23A(0.257) H23B(0.2693) H23C(0.3217)
 Fixed Y: H16A(0.1254) H16B(-0.0213) H16C(0.0122) H17A(-0.1572) H17B(-0.1931)
 H17C(-0.1541) H18A(-0.0274) H18B(0.1165) H20A(-0.0881) H20B(0.0168) H22A(-
 0.0626) H22B(-0.1671) H22C(-0.0618) H23A(0.0636) H23B(-0.0891) H23C(0.0077)
 Fixed Z: H16A(1.2725) H16B(1.2919) H16C(1.2848) H17A(1.1522) H17B(1.1582)
 H17C(1.0546) H18A(1.0965) H18B(1.1413) H20A(0.9306) H20B(0.855) H22A(0.8718)
 H22B(0.89) H22C(0.9733) H23A(0.7122) H23B(0.7272) H23C(0.7141)
;