Molecular amorphous glasses toward large azomethine crystals with aggregation-induced emission
Marin, Luminita; van der Lee, Arie; Shova, Sergiu; Arvinte, Adina; Barboiu, Mihail; New J. Chem. 39 (2015) 6404–; doi:10.1039/C5NJ01052G

data_7054926
_publ_section_title
;
 Molecular amorphous glasses toward large azomethine crystals with
 aggregation-induced emission
;
_journal_issue                   8
_journal_name_full               'New J. Chem.'
_journal_page_first              6404
_journal_paper_doi               10.1039/C5NJ01052G
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C29 H29 N O5'
_chemical_formula_sum            'C29 H29 N O5'
_chemical_formula_weight         471.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_update_record
;
2015-06-05 deposited with the CCDC.
2015-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.793(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8394(7)
_cell_length_b                   8.7672(3)
_cell_length_c                   13.8699(6)
_cell_measurement_reflns_used    2469
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.9107
_cell_measurement_theta_min      4.1890
_cell_volume                     2361.55(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      175
_diffrn_detector_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_details
;
  1 omega  -46.00   16.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7849  -61.0000  155.0000 62

  2 omega   37.00   74.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7849  179.0000  120.0000 37

  3 omega   47.00   84.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7849  179.0000  -60.0000 37

  4 omega  -52.00   50.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7849    0.0000    0.0000 102

  5 omega   34.00   59.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7849  179.0000   30.0000 25

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0183651000
_diffrn_orient_matrix_UB_12      -0.0608107000
_diffrn_orient_matrix_UB_13      -0.0164774000
_diffrn_orient_matrix_UB_21      0.0184821000
_diffrn_orient_matrix_UB_22      -0.0117852000
_diffrn_orient_matrix_UB_23      0.0488825000
_diffrn_orient_matrix_UB_31      -0.0256037000
_diffrn_orient_matrix_UB_32      -0.0520636000
_diffrn_orient_matrix_UB_33      0.0082099000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_unetI/netI     0.1100
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13155
_diffrn_reflns_theta_full        25.234
_diffrn_reflns_theta_max         29.005
_diffrn_reflns_theta_min         4.197
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.0003196
_refine_ls_shift/su_mean         0.0000423
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 19.1 16.6 17.5 7.09 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0770
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_refine_ls_wR_factor_ref         0.0600
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                3524
_reflns_number_total             5448
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.21
_oxford_diffrn_Wilson_scale      0.13
_oxford_refine_ls_r_factor_ref   0.0714
_oxford_refine_ls_scale          3.173(8)
_oxford_reflns_number_all        5448
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c5nj01052g1.cif
_cod_data_source_block           14
_cod_depositor_comments
'Adding full bibliography for 7054919--7054928.cif.'
_cod_original_cell_volume        2361.57(15)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               7054926
_cell_oxdiff_length_a            19.8373(11)
_cell_oxdiff_length_b            8.7658(5)
_cell_oxdiff_length_c            13.8731(8)
_cell_oxdiff_angle_alpha         89.985(4)
_cell_oxdiff_angle_beta          101.813(5)
_cell_oxdiff_angle_gamma         89.973(4)
_cell_oxdiff_volume              2361.3(2)
_montpellier_reflns_maxres       0.79
_montpellier_reflns_completeness_maxres 99.18
_montpellier_reflns_redundancy_maxres 2.49