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_4518490
_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, 2(H2 O)'
_chemical_formula_sum            'C22 H22 N4 O4'
_chemical_formula_weight         406.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.50(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.510(3)
_cell_length_b                   4.6400(9)
_cell_length_c                   33.910(7)
_cell_measurement_reflns_used    2480
_cell_measurement_temperature    100
_cell_measurement_theta_max      1.026
_cell_measurement_theta_min      0.116
_cell_volume                     1955.7(7)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.821
_diffrn_measured_fraction_theta_max 0.826
_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  0.0939
_diffrn_reflns_av_unetI/netI     0.1322
_diffrn_reflns_Laue_measured_fraction_full 0.821
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            6633
_diffrn_reflns_point_group_measured_fraction_full 0.821
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         1.026
_diffrn_reflns_theta_min         0.116
_diffrn_source                   'field emission gun'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       'micro crystal'
_exptl_crystal_F_000             334
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       21190(46)
_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   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2480
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.2178
_refine_ls_R_factor_gt           0.2128
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1614P)^2^+3.1978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5027
_refine_ls_wR_factor_ref         0.5051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2264
_reflns_number_total             2480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c21248_si_003.cif
_cod_data_source_block           15_0p7
_cod_depositor_comments
'Adding full bibliography for 4518489--4518490.cif.'
_cod_database_code               4518490
_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
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.015 and sigma for
terminal atoms of 0.035
3.a Free rotating group:
 O2(H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C5(H5), N2(H2), C4(H4), C2(H2A), C1(H1), C7(H7), C3(H3)
;
_shelx_res_checksum              70304
_shelx_hkl_checksum              57642
_olex2_submission_special_instructions 'No special instructions were received'