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_7054927
_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         'C31 H31 N'
_chemical_formula_sum            'C31 H31 N'
_chemical_formula_weight         417.57
_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                91.773(5)
_cell_angle_beta                 94.378(6)
_cell_angle_gamma                112.400(7)
_cell_formula_units_Z            2
_cell_length_a                   7.6600(6)
_cell_length_b                   8.1559(6)
_cell_length_c                   20.1223(13)
_cell_measurement_reflns_used    2360
_cell_measurement_temperature    2175
_cell_measurement_theta_max      32.4254
_cell_measurement_theta_min      4.2031
_cell_volume                     1156.42(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
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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_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 0.986
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_details
;
  1 omega   61.00   87.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1131   77.0000   60.0000 26

  2 omega    0.00   95.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1131   77.0000  -30.0000 95

  3 omega  -40.00   54.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1131  -77.0000 -150.0000 94

  4 omega    5.00   94.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1131   77.0000  120.0000 89

  5 omega    4.00   47.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1131   77.0000   60.0000 43

  6 omega  -63.00  -34.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.8944   96.0000  176.0000 29

  7 omega  -57.00    0.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.8944    0.0000  150.0000 57

;
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0721878000
_diffrn_orient_matrix_UB_12      -0.0104544000
_diffrn_orient_matrix_UB_13      -0.0176435000
_diffrn_orient_matrix_UB_21      -0.0670122000
_diffrn_orient_matrix_UB_22      -0.0397207000
_diffrn_orient_matrix_UB_23      -0.0279716000
_diffrn_orient_matrix_UB_31      0.0205303000
_diffrn_orient_matrix_UB_32      0.0848471000
_diffrn_orient_matrix_UB_33      -0.0127054000
_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  0.024
_diffrn_reflns_av_unetI/netI     0.1200
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12532
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         4.212
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99206
_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    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4850
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.0004428
_refine_ls_shift/su_mean         0.0000388
_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: 
 8.06 3.27 6.67 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0817
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_reflns_limit_h_max              10
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_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                4850
_reflns_number_total             7349
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.57
_oxford_diffrn_Wilson_scale      0.19
_oxford_refine_ls_r_factor_ref   0.0617
_oxford_refine_ls_scale          3.942(8)
_oxford_reflns_number_all        7349
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c5nj01052g1.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7054919--7054928.cif.'
_cod_original_cell_volume        1156.41(15)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7054927
_cell_oxdiff_length_a            7.6600(6)
_cell_oxdiff_length_b            8.1559(6)
_cell_oxdiff_length_c            20.1223(13)
_cell_oxdiff_angle_alpha         91.773(5)
_cell_oxdiff_angle_beta          94.378(6)
_cell_oxdiff_angle_gamma         112.400(7)
_cell_oxdiff_volume              1156.41(14)
_montpellier_reflns_maxres       0.66
_montpellier_reflns_completeness_maxres 87.59
_montpellier_reflns_redundancy_maxres 1.71
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 112,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 122,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 133,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,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   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;