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_7054922
_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 H21 N O'
_chemical_formula_sum            'C21 H21 N O'
_chemical_formula_weight         303.39
_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                96.420(3)
_cell_angle_beta                 103.728(3)
_cell_angle_gamma                92.257(3)
_cell_formula_units_Z            4
_cell_length_a                   9.6623(3)
_cell_length_b                   13.1399(4)
_cell_length_c                   13.4402(4)
_cell_measurement_reflns_used    7153
_cell_measurement_temperature    175
_cell_measurement_theta_max      29.0795
_cell_measurement_theta_min      4.1426
_cell_volume                     1643.40(9)
_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 0.983
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_details
;
  1 omega   35.00   60.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -       17.9412  179.0000 -150.0000 25

  2 omega   -9.00   86.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -       17.9412   77.0000  150.0000 95

  3 omega  -45.00   46.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -       17.9412  -77.0000   30.0000 91

  4 omega  -12.00   84.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -       17.9412   77.0000  -60.0000 96

  5 omega   44.00   71.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -       17.9412  179.0000 -180.0000 27

  6 omega  -44.00   49.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -      -18.6443   77.0000 -120.0000 93

  7 omega  -12.00   88.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -       17.9412   77.0000   30.0000 100

  8 omega   34.00   94.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -       17.9412  179.0000   60.0000 60

  9 omega   -3.00   88.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -       17.9412   53.0000  -70.0000 91

 10 omega   34.00   94.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -       17.9412  179.0000 -180.0000 60

 11 omega  -52.00   48.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -       17.9412  -77.0000 -180.0000 100

 12 omega  -52.00   48.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -       17.9412  -77.0000  120.0000 100

 13 omega  -49.00   12.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -      -18.6443   77.0000    0.0000 61

 14 omega  -49.00   51.00   1.0000   16.9300
omega____ theta____ kappa____ phi______ frames
    -      -18.6443   77.0000  -90.0000 100

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0675041000
_diffrn_orient_matrix_UB_12      0.0276469000
_diffrn_orient_matrix_UB_13      0.0107748000
_diffrn_orient_matrix_UB_21      0.0206873000
_diffrn_orient_matrix_UB_22      -0.0209527000
_diffrn_orient_matrix_UB_23      0.0473025000
_diffrn_orient_matrix_UB_31      0.0274305000
_diffrn_orient_matrix_UB_32      -0.0419672000
_diffrn_orient_matrix_UB_33      -0.0253856000
_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  0.036
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36618
_diffrn_reflns_theta_full        25.064
_diffrn_reflns_theta_max         29.144
_diffrn_reflns_theta_min         4.151
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95452
_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    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0757
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6078
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.0013347
_refine_ls_shift/su_mean         0.0000717
_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: 
 14.2 6.84 11.9 3.65 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0752
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0662
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6078
_reflns_number_total             8018
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.78
_oxford_diffrn_Wilson_scale      0.07
_oxford_refine_ls_r_factor_ref   0.0678
_oxford_refine_ls_scale          5.568(11)
_oxford_reflns_number_all        8018
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c5nj01052g1.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7054919--7054928.cif.'
_cod_original_cell_volume        1643.42(10)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7054922
_cell_oxdiff_length_a            9.6623(3)
_cell_oxdiff_length_b            13.1399(4)
_cell_oxdiff_length_c            13.4402(4)
_cell_oxdiff_angle_alpha         96.420(3)
_cell_oxdiff_angle_beta          103.728(3)
_cell_oxdiff_angle_gamma         92.257(3)
_cell_oxdiff_volume              1643.42(9)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 90.71
_montpellier_reflns_redundancy_maxres 4.57
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV C(14,OCC) C(141,OCC) C(15,OCC) C(151,OCC) 
CONT H(131,OCC) H(132,OCC) H(133,OCC) H(134,OCC) 
CONT H(141,OCC) H(142,OCC) H(1411,OCC) H(1412,OCC) 
CONT H(151,OCC) H(152,OCC) H(153,OCC) 
CONT H(1511,OCC) H(1512,OCC) H(1513,OCC) 
WEIGHT -1 C(141,OCC) C(151,OCC) 
CONT  H(133,OCC) H(134,OCC) 
CONT  H(1411,OCC) H(1412,OCC) 
CONT H(1511,OCC) H(1512,OCC) H(1513,OCC) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE N   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE N   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 363,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C(13,X'S) H(131,X'S) H(132,X'S) H(133,X'S) H(134,X'S) 
RIDE C(14,X'S) H(141,X'S) H(142,X'S) 
RIDE C(141,X'S) H(1411,X'S) H(1412,X'S) 
RIDE C(15,X'S) H(151,X'S) H(152,X'S)  H(153,X'S) 
RIDE C(151,X'S) H(1511,X'S) H(1512,X'S) H(1513,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
DIST 1.52,0.005 = C(13) TO C(14), C(13) TO C(141) 
SAME 0.005 , 0.05 
CONT C(13)  C(14)  C(15) AND 
CONT  C(13)  C(141)  C(151) 
A-U(IJ)'S 0.0,0.05 = C(14) TO C(141), C(15) TO C(151) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;