Molecular motions of a tetraphenylethylene-derived AIEgen directly monitored through in situ variable temperature single crystal X-ray diffraction
Zhou, Lian; Meng, Wei; Sun, Lin; Du, Lin; Xuan, Xiaopeng; Zhang, Jun; CrystEngComm 24 (2022) 231–234; doi:10.1039/D1CE01441B

data_7243918
_publ_section_title
;
 Molecular motions of a tetraphenylethylene-derived AIEgen directly
 monitored through in situ variable temperature single crystal X-ray
 diffraction
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              231
_journal_page_last               234
_journal_paper_doi               10.1039/D1CE01441B
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C31 H29 N O2'
_chemical_formula_sum            'C31 H29 N O2'
_chemical_formula_weight         447.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-09 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8024(4)
_cell_length_b                   9.8815(2)
_cell_length_c                   30.6532(8)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.42
_cell_volume                     5089.4(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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_temperature      180.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            39666
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         2.424
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.4915
_exptl_absorpt_correction_T_min  0.4448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5818
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0704
_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^)+(0.0382P)^2^+5.7125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4413
_reflns_number_total             5818
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01441b2.cif
_cod_data_source_block           220192404180k_0m
_cod_depositor_comments
'Adding full bibliography for 7243909--7243918.cif.'
_cod_database_code               7243918
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26A-C19 \\sim C26-C19
 with sigma of 0.01
 C27-C19 \\sim C19-C31
 with sigma of 0.01
 C18-C26 \\sim C26-C20
 with sigma of 0.01
3. Restrained planarity
 C27, C28, C29, C30, C31, C26, C19
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C26A \\sim C27A
\\sim C28A \\sim C29A \\sim C30A \\sim C31A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C26A) \\sim Ueq,
Uanis(C27A) \\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C29A) \\sim Ueq,
Uanis(C30A) \\sim Ueq, Uanis(C31A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C26, C27, C28, C29, C30, C31, C26A, C27A, C28A, C29A, C30A, C31A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=
 Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=1-FVAR(1)
 Sof(C26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=
 Sof(H30)=Sof(C31)=Sof(H31)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C27A(H27A), C28A(H28A), C29A(H29A),
 C30A(H30A), C31A(H31A)
7.b Fitted hexagon refined as free rotating group:
 C26(C27,C28,C29,C30,C31), C26A(C27A,C28A,C29A,C30A,C31A)
7.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              21482
_shelx_hkl_checksum              39459
_olex2_submission_special_instructions 'No special instructions were received'