Utilizing the aggregation-induced emission phenomenon to visualize spontaneous molecular directed motion in the solid state
Liu, Jianxun; Xing, Chang; Wei, Donghui; Deng, Qianqian; Yang, Cuiping; Peng, Qiuchen; Hou, Hongwei; Li, Yuanyuan; Li, Kai; Materials Chemistry Frontiers 3 (2019) 2746–; doi:10.1039/C9QM00586B

data_1554693
_publ_section_title
;
 Utilizing the aggregation-induced emission phenomenon to visualize
 spontaneous molecular directed motion in the solid state
;
_journal_issue                   12
_journal_name_full               'Materials Chemistry Frontiers'
_journal_page_first              2746
_journal_paper_doi               10.1039/C9QM00586B
_journal_volume                  3
_journal_year                    2019
_chemical_formula_moiety         'C17 H19 N O2'
_chemical_formula_sum            'C17 H19 N O2'
_chemical_formula_weight         269.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc235s7b
_audit_creation_date             2019-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-21 deposited with the CCDC.	2019-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                86.545(2)
_cell_angle_beta                 84.929(2)
_cell_angle_gamma                89.992(2)
_cell_formula_units_Z            4
_cell_length_a                   6.1745(2)
_cell_length_b                   7.0411(2)
_cell_length_c                   33.2296(10)
_cell_measurement_reflns_used    6672
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      72.9700
_cell_measurement_theta_min      2.7020
_cell_volume                     1436.38(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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     56.00  87.00   0.50    0.50    --    0.00  57.00 -30.00   62
  2  \w    -28.00  43.00   0.50    0.50    --    0.00  57.00 -30.00  142
  3  \w    -15.00  18.00   0.50    0.50    --    0.00  57.00  90.00   66
  4  \w     -8.00  28.00   0.50    0.50    --    0.00 -38.00  90.00   72
  5  \w    -88.00 -15.00   0.50    0.50    --    0.00 -38.00  90.00  146
  6  \w    -29.00  88.00   0.50    0.50    --    0.00  57.00-180.00  234
  7  \w     14.00  72.00   0.50    3.00    --   97.60 -82.00 120.00  116
  8  \w     29.00 148.00   0.50    3.00    --   97.60 -15.00 150.00  238
  9  \w    139.00 186.00   0.50    3.00    --   97.60  82.00 120.00   94
 10  \w     64.00 130.00   0.50    3.00    --   97.60 -82.00 -30.00  132
 11  \w     57.00 134.00   0.50    3.00    --   97.60 -82.00 150.00  154
 12  \w     55.00 126.00   0.50    3.00    --   97.60 -82.00 -90.00  142
 13  \w     65.00 186.00   0.50    3.00    --   97.60  30.00 120.00  242
 14  \w     79.00 134.00   0.50    3.00    --   97.60 -82.00  30.00  110
 15  \w     60.00 132.00   0.50    3.00    --   97.60 -82.00  60.00  144
 16  \w     48.00 134.00   0.50    3.00    --   97.60 -82.00-180.00  172
 17  \w     64.00 142.00   0.50    3.00    --   97.60  30.00   0.00  156
 18  \w     72.00 185.00   0.50    3.00    --   97.60  45.00-180.00  226
 19  \w     78.00 122.00   0.50    3.00    --   97.60 -82.00 120.00   88
 20  \w     80.00 107.00   0.50    3.00    --   97.60  45.00   0.00   54
 21  \w     45.00  71.00   0.50    3.00    --   97.60 -82.00-150.00   52
 22  \w     95.00 120.00   0.50    3.00    --   97.60 -82.00-150.00   50
 23  \w     12.00  38.00   0.50    3.00    --   97.60 -82.00-180.00   52
 24  \w      8.00 123.00   0.50    3.00    --   97.60 -30.00 150.00  230
 25  \w     89.00 116.00   0.50    3.00    --   97.60  82.00 120.00   54
 26  \w     12.00 117.00   0.50    3.00    --   97.60 -45.00   0.00  210
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0798765000
_diffrn_orient_matrix_UB_12      0.0322991000
_diffrn_orient_matrix_UB_13      0.0416870000
_diffrn_orient_matrix_UB_21      -0.1438976000
_diffrn_orient_matrix_UB_22      -0.1664303000
_diffrn_orient_matrix_UB_23      0.0190200000
_diffrn_orient_matrix_UB_31      0.1888596000
_diffrn_orient_matrix_UB_32      -0.1389565000
_diffrn_orient_matrix_UB_33      -0.0086436000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            14654
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        65.999
_diffrn_reflns_theta_max         65.999
_diffrn_reflns_theta_min         2.675
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0396P)^2^+1.2218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4268
_reflns_number_total             4957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qm00586b3.cif
_cod_data_source_block           20190110c6_1
_cod_depositor_comments
;

2022-03-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C17 H19 N O2)'
_cod_original_formula_sum        'C34 H38 N2 O4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     538.66
_cod_database_code               1554693
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.887
_reflns_odcompleteness_completeness 98.93
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C32(H32A,H32B), C20(H20A,H20B), C28(H28A,
 H28B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4A), C13(H13), C15(H15), C17(H17), C18(H18), C19(H19), C22(H22), C24(H24),
  C30(H30), C6(H6), C7(H7), C11(H11), C14(H14), C16(H16), C25(H25), C26(H26),
 C27(H27), C29(H29)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O3(H3)
;
_shelx_res_checksum              51496
_shelx_hkl_checksum              79512
_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 1.303
_oxdiff_exptl_absorpt_empirical_full_min 0.775