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_7054924
_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 H31 N, 0.0833(H3 C2 N)'
_chemical_formula_sum            'C29.166 H31.25 N1.08'
_chemical_formula_weight         396.94
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   46.312(3)
_cell_length_b                   46.312(3)
_cell_length_c                   5.6266(5)
_cell_measurement_reflns_used    1100
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.8531
_cell_measurement_theta_min      4.1448
_cell_volume                     10451.1(13)
_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
;
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 0.967
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_details
;
  1 omega  -19.00   33.50   0.7500   75.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6287 -101.0000   30.0000 70

  2 omega  -39.00   28.50   0.7500   75.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6287  -88.0000 -118.0000 90

  3 omega  -12.00   22.50   0.7500   75.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6287   77.0000 -180.0000 46

  4 omega  -12.00   87.00   0.7500   75.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6287   77.0000  -30.0000 132

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0029066000
_diffrn_orient_matrix_UB_12      0.0119414000
_diffrn_orient_matrix_UB_13      0.0576378000
_diffrn_orient_matrix_UB_21      -0.0172069000
_diffrn_orient_matrix_UB_22      -0.0096424000
_diffrn_orient_matrix_UB_23      -0.0275566000
_diffrn_orient_matrix_UB_31      -0.0028175000
_diffrn_orient_matrix_UB_32      -0.0087756000
_diffrn_orient_matrix_UB_33      0.1086810000
_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  0.132
_diffrn_reflns_av_unetI/netI     0.4091
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            18106
_diffrn_reflns_theta_full        25.158
_diffrn_reflns_theta_max         28.917
_diffrn_reflns_theta_min         4.153
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34134
_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    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             3848.508
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1478
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         2119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2244
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.0058815
_refine_ls_shift/su_mean         0.0001963
_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: 
 1.74 -9.13 -1.29 -2.61 -1.97 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0893
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0424
_reflns_limit_h_max              28
_reflns_limit_h_min              -58
_reflns_limit_k_max              61
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                2119
_reflns_number_total             5450
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.34
_oxford_diffrn_Wilson_scale      29.76
_oxford_refine_ls_r_factor_ref   0.0713
_oxford_refine_ls_scale          0.4137(9)
_oxford_reflns_number_all        5442
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c5nj01052g1.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7054919--7054928.cif.'
_cod_original_cell_volume        10451.3(14)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_database_code               7054924
_cell_oxdiff_length_a            46.301(3)
_cell_oxdiff_length_b            46.293(4)
_cell_oxdiff_length_c            5.6263(5)
_cell_oxdiff_angle_alpha         90.001(7)
_cell_oxdiff_angle_beta          90.009(6)
_cell_oxdiff_angle_gamma         119.930(8)
_cell_oxdiff_volume              10451(1)
_montpellier_reflns_maxres       1.04
_montpellier_reflns_completeness_maxres 99.09
_montpellier_reflns_redundancy_maxres 4.44