Polymorph selectivity of an AIE luminogen under nano-confinement to visualize polymer microstructures
Khorloo, Michidmaa; Cheng, Yanhua; Zhang, Haoke; Chen, Ming; Sung, Herman H. Y.; Williams, Ian D.; Lam, Jacky W. Y.; Tang, Ben Zhong; Chemical Science 11 (2020) 997–1005; doi:10.1039/C9SC04239C

data_1556535
_publ_section_title
;
 Polymorph selectivity of an AIE luminogen under nano-confinement to
 visualize polymer microstructures
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              997
_journal_page_last               1005
_journal_paper_doi               10.1039/C9SC04239C
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'F6 P, C34 H28 N'
_chemical_formula_sum            'C34 H28 F6 N P'
_chemical_formula_weight         595.54
_chemical_name_common            TPE-Py
_chemical_name_systematic        TPE-EP-Y
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-05-22 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.168(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8939(7)
_cell_length_b                   9.1783(2)
_cell_length_c                   12.5794(3)
_cell_measurement_reflns_used    6010
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.6250
_cell_measurement_theta_min      5.1320
_cell_volume                     2845.03(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.915
_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     82.00 138.00   1.00   20.00    --  106.99 -30.00 -60.00   56
  2  \w   -109.00 -14.00   1.00    8.00    --  -40.57 -37.00   0.00   95
  3  \w    -91.00  -2.00   1.00    8.00    --  -40.57 125.00-120.00   89
  4  \w    -67.00  36.00   1.00    8.00    --  -40.57  37.00-180.00  103
  5  \w     78.00 158.00   1.00   20.00    --  106.99  61.00 -90.00   80
  6  \w     48.00 117.00   1.00   20.00    --  106.99-125.00 -30.00   69
  7  \w     31.00 138.00   1.00   20.00    --  106.99 -30.00  90.00  107
  8  \w     32.00 117.00   1.00   20.00    --  106.99-125.00 120.00   85
  9  \w     94.00 173.00   1.00   20.00    --  106.99 125.00  90.00   79
 10  \w     29.00  67.00   1.00   20.00    --  106.99 -30.00 -60.00   38
 11  \w     96.00 171.00   1.00   20.00    --  106.99 125.00 150.00   75
 12  \w     28.00 141.00   1.00   20.00    --  106.99 -77.00 120.00  113
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0309900000
_diffrn_orient_matrix_UB_12      -0.1428328000
_diffrn_orient_matrix_UB_13      -0.0298507000
_diffrn_orient_matrix_UB_21      -0.0530776000
_diffrn_orient_matrix_UB_22      0.0726909000
_diffrn_orient_matrix_UB_23      0.0221994000
_diffrn_orient_matrix_UB_31      -0.0114693000
_diffrn_orient_matrix_UB_32      0.0498615000
_diffrn_orient_matrix_UB_33      -0.1179998000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14173
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.499
_diffrn_reflns_theta_min         5.386
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         4687
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0869
_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^)+(0.0980P)^2^+11.2920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2128
_refine_ls_wR_factor_ref         0.2163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4216
_reflns_number_total             4687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04239c2.cif
_cod_data_source_block           khor2a
_cod_depositor_comments
;Adding full bibliography for 1556534--1556535.cif.

 Adding full bibliography for 1556534--1556535.cif.
;
_cod_original_cell_volume        2845.01(13)
_cod_database_code               1556535
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.764
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(P1A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.003
3. Others
 Fixed Sof: P1(0.9) P1A(0.1)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15),
 C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              14968
_olex2_date_sample_data_collection 2018-10-25
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.164
_oxdiff_exptl_absorpt_empirical_full_min 0.773