Microcrystal Electron Diffraction Elucidates Water-Specific Polymorphism-Induced Emission Enhancement of Bis-arylacylhydrazone.
Cho, Hye Jin; Kim, Kyung-Su; Kim, Hyunwoo; Kim, Taewoo; Malyutin, Andrey G.; Rees, Douglas C.; Yoo, Byung-Kuk; Song, Changsik; ACS applied materials & interfaces 13 (2021) 7546–7555; doi:10.1021/acsami.0c21248

data_4518489
_publ_section_title
;
 Microcrystal Electron Diffraction Elucidates Water-Specific
 Polymorphism-Induced Emission Enhancement of Bis-arylacylhydrazone.
;
_journal_issue                   6
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              7546
_journal_page_last               7555
_journal_paper_doi               10.1021/acsami.0c21248
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C22 H18 N4 O2'
_chemical_formula_sum            'C22 H18 N4 O2'
_chemical_formula_weight         370.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.80(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.420(4)
_cell_length_b                   5.1900(10)
_cell_length_c                   16.740(3)
_cell_measurement_reflns_used    5272
_cell_measurement_temperature    100
_cell_measurement_theta_max      0.898
_cell_measurement_theta_min      0.138
_cell_volume                     1781.6(6)
_computing_cell_refinement       XDS
_computing_data_collection       manual
_computing_data_reduction        XDSCONV
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.751
_diffrn_measured_fraction_theta_max 0.753
_diffrn_measurement_device_type  'thermo fisher talos arctica'
_diffrn_measurement_method       'single axis continous rotation'
_diffrn_radiation_type           '200 keV electrons'
_diffrn_radiation_wavelength     0.02508
_diffrn_reflns_av_R_equivalents  0.1320
_diffrn_reflns_av_unetI/netI     0.1785
_diffrn_reflns_Laue_measured_fraction_full 0.751
_diffrn_reflns_Laue_measured_fraction_max 0.753
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11995
_diffrn_reflns_point_group_measured_fraction_full 0.718
_diffrn_reflns_point_group_measured_fraction_max 0.721
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         0.898
_diffrn_reflns_theta_min         0.138
_diffrn_source                   'field emission gun'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       'micro crystal'
_exptl_crystal_F_000             309
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_coef       2521(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.379
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         5272
_refine_ls_number_restraints     446
_refine_ls_restrained_S_all      1.347
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.1492
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3564
_refine_ls_wR_factor_ref         0.3641
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_full    0.686
_reflns_Friedel_fraction_max     0.689
_reflns_number_gt                4568
_reflns_number_total             5272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c21248_si_002.cif
_cod_data_source_block           merged_01
_cod_depositor_comments
'Adding full bibliography for 4518489--4518490.cif.'
_cod_original_cell_volume        1781.6(7)
_cod_database_code               4518489
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
'electron diffraction, unknown absorption effects'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12A) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C4A)
\\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C14A) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N3A(H3A), C1A(H1AA), C2A(H2A), C3A(H3AA), C4A(H4A), C5A(H5A),
 C7A(H7A), C10A(H10A), C11A(H11A), C13A(H13A), C14A(H14A), C16A(H16A),
 C18A(H18A), C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A), N1B(H1B), N3B(H3B),
  C1B(H1BA), C2B(H2B), C3B(H3BA), C4B(H4B), C5B(H5B), C7B(H7B), C10B(H10B),
 C11B(H11B), C13B(H13B), C14B(H14B), C16B(H16B), C18B(H18B), C19B(H19B),
 C20B(H20B), C21B(H21B), C22B(H22B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              85037
_shelx_hkl_checksum              26635
_olex2_submission_special_instructions 'No special instructions were received'