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_7054921
_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         'C21 H26 N2 O3'
_chemical_formula_sum            'C21 H26 N2 O3'
_chemical_formula_weight         354.44
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                95.744(13)
_cell_angle_beta                 91.859(12)
_cell_angle_gamma                101.739(15)
_cell_formula_units_Z            2
_cell_length_a                   4.6306(8)
_cell_length_b                   8.8802(17)
_cell_length_c                   23.893(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    175
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     955.7(3)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_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 16.1593
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_details
;
  1 omega  -23.00   25.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0127  -99.0000   30.0000 48

  2 omega   36.00   88.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5908 -178.0000   60.0000 52

  3 omega   -6.00   87.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5908   38.0000 -150.0000 93

  4 omega   -2.00   43.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5908   57.0000  -60.0000 45

  5 omega  -36.00   64.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5908  -19.0000    0.0000 100

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.0728331000
_diffrn_orient_matrix_UB_12      0.0560836000
_diffrn_orient_matrix_UB_13      -0.0097944000
_diffrn_orient_matrix_UB_21      0.0476894000
_diffrn_orient_matrix_UB_22      -0.0160152000
_diffrn_orient_matrix_UB_23      -0.0274646000
_diffrn_orient_matrix_UB_31      -0.1302676000
_diffrn_orient_matrix_UB_32      -0.0577369000
_diffrn_orient_matrix_UB_33      -0.0065263000
_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  0.084
_diffrn_reflns_av_unetI/netI     0.078
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7017
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         29.184
_diffrn_reflns_theta_min         1.716
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         1866
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.2757
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0.0000773
_refine_ls_shift/su_mean         0.0000100
_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: 
 16.9 -6.25 14.3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1788
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0897
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              29
_reflns_limit_l_min              -30
_reflns_number_gt                1686
_reflns_number_total             4096
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0836
_oxford_refine_ls_scale          2.728(14)
_oxford_reflns_number_all        7017
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c5nj01052g1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7054919--7054928.cif.'
_cod_original_cell_volume        955.71(11)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7054921
_montpellier_reflns_maxres       1.08
_montpellier_reflns_completeness_maxres 90.89
_montpellier_reflns_redundancy_maxres 1.67