Macroscopic crystalline deformation in an organic dye during reversible phase transition caused by alkyl disorder
Minami, Takaya; Sato, Hiroyasu; Matsumoto, Shinya; CrystEngComm 20 (2018) 2644–; doi:10.1039/C8CE00465J

data_7230495
_publ_section_title
;
 Macroscopic crystalline deformation in an organic dye during reversible
 phase transition caused by alkyl disorder
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              2644
_journal_paper_doi               10.1039/C8CE00465J
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C26 H30 N6'
_chemical_formula_sum            'C26 H30 N6'
_chemical_formula_weight         426.56
_chemical_melting_point          551
_chemical_name_common            DE2
_chemical_name_systematic
'N, N'-bis [(4-diethylaminophenyl) methylidene] diaminomaleonitrile'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-12-13 deposited with the CCDC.
2018-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                80.038(5)
_cell_angle_beta                 76.141(5)
_cell_angle_gamma                89.607(5)
_cell_formula_units_Z            3
_cell_length_a                   9.2410(5)
_cell_length_b                   11.3265(6)
_cell_length_c                   18.1906(10)
_cell_measurement_reflns_used    1949
_cell_measurement_temperature    343
_cell_measurement_theta_max      20.73
_cell_measurement_theta_min      1.98
_cell_volume                     1819.49(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      343
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11703
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.790
_diffrn_reflns_theta_max         24.790
_diffrn_reflns_theta_min         2.272
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             684.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform and diethyl ether'
_exptl_crystal_size_max          0.481
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.20
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6186
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.2086
_refine_ls_R_factor_gt           0.0841
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1059P)^2^+0.0528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2404
_reflns_number_total             6186
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c8ce00465j9.cif
_cod_data_source_block           DE2_343K
_cod_depositor_comments
'Adding full bibliography for 7230490--7230496.cif.'
_cod_database_code               7230495
_shelx_res_checksum              770