Vinylpyrroles: solid-state structures and aggregation-induced emission properties
Okawara, Toru; Matsufuji, Yurina; Mizuno, Kouhei; Takehara, Kenji; Nagamura, Toshihiko; Iwasa, Seiji; RSC Advances 9 (2019) 22817–; doi:10.1039/C9RA04088A

data_7233259
_publ_section_title
;
 Vinylpyrroles: solid-state structures and aggregation-induced emission
 properties
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              22817
_journal_paper_doi               10.1039/C9RA04088A
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C20 H25 N3 O7'
_chemical_formula_sum            'C20 H25 N3 O7'
_chemical_formula_weight         419.44
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-24 deposited with the CCDC.    2019-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.833(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.799(2)
_cell_length_b                   5.2201(7)
_cell_length_c                   21.974(3)
_cell_measurement_reflns_used    1884
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.2350
_cell_measurement_theta_min      3.2960
_cell_volume                     1998.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9988
_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    -74.00 119.00   1.00  100.00    --   30.00  54.00-180.00  193
  2  \w    -74.00 119.00   1.00  100.00    --   30.00  54.00  60.00  193
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0007436000
_diffrn_orient_matrix_UB_12      -0.0105357000
_diffrn_orient_matrix_UB_13      0.0320643000
_diffrn_orient_matrix_UB_21      -0.0169279000
_diffrn_orient_matrix_UB_22      0.1232493000
_diffrn_orient_matrix_UB_23      -0.0007292000
_diffrn_orient_matrix_UB_31      -0.0370130000
_diffrn_orient_matrix_UB_32      -0.0561452000
_diffrn_orient_matrix_UB_33      -0.0077396000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.0957
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12866
_diffrn_reflns_theta_full        26.3696
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.69
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34a (Rigaku Oxford Diffraction, 2017)
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    1.3941
_exptl_crystal_description       plate
_exptl_crystal_F_000             888.5297
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.6459
_refine_diff_density_min         -0.5536
_refine_diff_density_rms         0.1388
_refine_ls_d_res_high            0.8001
_refine_ls_d_res_low             7.5702
_refine_ls_goodness_of_fit_ref   1.1119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    36
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1119
_refine_ls_R_factor_all          0.1443
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+2.3620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2756
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              6
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                2400
_reflns_number_total             4094
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9ra04088a2.cif
_cod_data_source_block           yano070
_cod_database_code               7233259
_chemical_oxdiff_formula         C
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C19(H19a,H19b), C13(H13a,H13b), C17(H17a,H17b)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C5(H5)
2.c Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C20(H20a,H20b,H20c), C16(H16a,H16b,H16c), C18(H18a,H18b,
 H18c), C14(H14a,H14b,H14c)
;
_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 1.342
_oxdiff_exptl_absorpt_empirical_full_min 0.812