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_7054923
_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         'C25 H27 N O6'
_chemical_formula_sum            'C25 H27 N O6'
_chemical_formula_weight         437.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 94.550(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.04160(18)
_cell_length_b                   13.6467(5)
_cell_length_c                   31.0182(11)
_cell_measurement_reflns_used    4995
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.9480
_cell_measurement_theta_min      4.5780
_cell_volume                     2127.36(13)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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 0.978
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details
;
  1 omega  -36.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9412    0.0000  150.0000 116

  2 omega   30.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9412 -149.0000 -131.0000 56

  3 omega  -40.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.7224   38.0000   90.0000 84

  4 omega  -77.00  -49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.7224  130.0000   53.0000 28

  5 omega   -8.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9412   38.0000    0.0000 98

  6 omega   -8.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9412   38.0000 -150.0000 98

  7 omega  -12.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9412   77.0000  -90.0000 44

  8 omega  -86.00  -29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.7224  141.0000 -132.0000 57

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0194145000
_diffrn_orient_matrix_UB_12      -0.0162489000
_diffrn_orient_matrix_UB_13      -0.0217403000
_diffrn_orient_matrix_UB_21      0.0062943000
_diffrn_orient_matrix_UB_22      0.0491713000
_diffrn_orient_matrix_UB_23      -0.0072649000
_diffrn_orient_matrix_UB_31      0.1396503000
_diffrn_orient_matrix_UB_32      -0.0044750000
_diffrn_orient_matrix_UB_33      -0.0008565000
_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  0.032
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            23748
_diffrn_reflns_theta_full        25.236
_diffrn_reflns_theta_max         29.007
_diffrn_reflns_theta_min         4.321
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1293
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4041
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.0006944
_refine_ls_shift/su_mean         0.0000507
_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:
 13.5 5.73 11.2 3.79 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0620
_refine_ls_wR_factor_gt          0.0549
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_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              41
_reflns_limit_l_min              0
_reflns_number_gt                4041
_reflns_number_total             5125
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.49
_oxford_diffrn_Wilson_scale      0.04
_oxford_refine_ls_r_factor_ref   0.0520
_oxford_refine_ls_scale          4.707(10)
_oxford_reflns_number_all        5125
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c5nj01052g1.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 7054919--7054928.cif.'
_cod_original_cell_volume        2127.37(13)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7054923
_cell_oxdiff_length_a            5.04159(15)
_cell_oxdiff_length_b            13.6457(7)
_cell_oxdiff_length_c            31.0207(12)
_cell_oxdiff_angle_alpha         89.994(4)
_cell_oxdiff_angle_beta          94.550(3)
_cell_oxdiff_angle_gamma         90.001(3)
_cell_oxdiff_volume              2127.37(16)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 90.61
_montpellier_reflns_redundancy_maxres 4.58
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  32,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  52,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  62,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  82,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  92,X'S) H   (  91,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   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE N   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,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 O   (  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                                                                             
;