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_1556534
_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         '0.5(C H2 Cl2), F6 P, C34 H28 N'
_chemical_formula_sum            'C34.5 H29 Cl F6 N P'
_chemical_formula_weight         638.01
_chemical_name_common            TPE-Py
_chemical_name_systematic        TPE-EP-G
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-07
_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                 93.8053(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.2525(2)
_cell_length_b                   9.21940(13)
_cell_length_c                   59.1397(9)
_cell_measurement_reflns_used    11185
_cell_measurement_temperature    100.03(11)
_cell_measurement_theta_max      73.0670
_cell_measurement_theta_min      4.0480
_cell_volume                     6121.70(17)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.03(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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     29.00 105.50   0.75   25.00    --  106.99 -77.00 -90.00  102
  2  \w   -117.00 -15.00   0.75   10.00    --  -40.57 -37.00   0.00  136
  3  \w    -69.00  32.25   0.75   10.00    --  -40.57  57.00 150.00  135
  4  \w    -92.00  -2.00   0.75   10.00    --  -40.57 125.00-150.00  120
  5  \w     65.00 116.00   0.75   25.00    --  106.99-125.00 -90.00   68
  6  \w     38.00 115.25   0.75   25.00    --  106.99-125.00  60.00  103
  7  \w     46.00 164.50   0.75   25.00    --  106.99  15.00  30.00  158
  8  \w     33.00 134.25   0.75   25.00    --  106.99 -45.00   0.00  135
  9  \w     32.00 116.00   0.75   25.00    --  106.99-125.00-180.00  112
 10  \w     32.00 130.25   0.75   25.00    --  106.99 -45.00 120.00  131
 11  \w    109.00 178.00   0.75   25.00    --  106.99  45.00  60.00   92
;
_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      -0.1136970000
_diffrn_orient_matrix_UB_12      0.0206380000
_diffrn_orient_matrix_UB_13      -0.0156822000
_diffrn_orient_matrix_UB_21      0.0009888000
_diffrn_orient_matrix_UB_22      -0.1626067000
_diffrn_orient_matrix_UB_23      -0.0059458000
_diffrn_orient_matrix_UB_31      -0.0768846000
_diffrn_orient_matrix_UB_32      -0.0322975000
_diffrn_orient_matrix_UB_33      0.0200047000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            32777
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.498
_diffrn_reflns_theta_min         3.959
_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    2.143
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72507
_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    1.384
_exptl_crystal_description       needle
_exptl_crystal_F_000             2632
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         10976
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0660P)^2^+8.2250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9143
_reflns_number_total             10976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04239c2.cif
_cod_data_source_block           khor3cult
_cod_depositor_comments
;

 Adding full bibliography for 1556534--1556535.cif.

2022-11-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        6121.68(17)
_cod_original_formula_moiety     'C H2 Cl2, 2(F6 P), 2(C34 H28 N)'
_cod_original_formula_sum        'C69 H58 Cl2 F12 N2 P2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1276.01
_cod_database_code               1556534
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.674
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3B-C2B \\sim C4B-C3B \\sim C5B-C4B \\sim C6B-C5B
 with sigma of 0.02
 C3A-C2A \\sim C4A-C3A \\sim C5A-C4A \\sim C6A-C5A
 with sigma of 0.02
 N1A-C2B \\sim N1A-C6B
 with sigma of 0.02
 N1A-C6A \\sim N1A-C2A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N1A, C2B, C3B, C4B, C5B, C6B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1A, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: C2A(0.75) H2A(0.75) C2B(0.25) H2B(0.25) C3A(0.75) H3A(0.75)
 C3B(0.25) H3B(0.25) C4A(0.75) C4B(0.25) C5A(0.75) H5A(0.75) C5B(0.25)
 H5B(0.25) C6A(0.75) H6A(0.75) C6B(0.25) H6B(0.25) C7A(0.75) H7A(0.75)
 C7B(0.25) H7B(0.25) C8A(0.75) H8A(0.75) C8B(0.25) H8B(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
5.b 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), C2A(H2A), C2B(H2B), C3A(H3A), C3B(H3B), C5A(H5A), C5B(H5B), C6A(H6A),
  C6B(H6B), C7A(H7A), C7B(H7B), C8A(H8A), C8B(H8B), C12A(H12A), C13A(H13A),
 C15A(H15A), C16A(H16A), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A),
 C26A(H26A), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A),
 C42A(H42A), C43A(H43A), C44A(H44A), C45A(H45A), C46A(H46A)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              38288
_olex2_date_sample_data_collection 2018-11-06
_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 1.558
_oxdiff_exptl_absorpt_empirical_full_min 0.671