Exploring the excited-state charge transfer fluorescence profile of 7-hydroxycoumarin and 2-methylimidazole – a combined X-ray diffraction and theoretical approach
Hawkins, Bryson A.; Najib, Elias; Du, Jonathan J.; Lai, Felcia; Platts, James A.; Groundwater, Paul W.; Hibbs, David E.; Physical Chemistry Chemical Physics  (2022) –; doi:10.1039/D2CP01235A

data_7244957
_publ_section_title
;
 Exploring the excited-state charge transfer fluorescence profile of
 7-hydroxycoumarin and 2-methylimidazole -- a combined X-ray diffraction
 and theoretical approach
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D2CP01235A
_journal_year                    2022
_chemical_formula_moiety         'C4 N2 H6'
_chemical_formula_sum            'C4 H6 N2'
_chemical_formula_weight         82.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-02-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-28 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.0180(2)
_cell_length_b                   8.1483(4)
_cell_length_c                   9.6871(3)
_cell_measurement_reflns_used    14451
_cell_measurement_temperature    120.1(3)
_cell_measurement_theta_max      51.4350
_cell_measurement_theta_min      3.9710
_cell_volume                     475.02(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.1(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2474
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -10.00  91.00   1.00   10.00    --   18.00  57.00 -17.36  101
  2  \w    -11.00  91.00   1.00   10.00    --   18.00  60.00  87.62  102
  3  \w     -6.00  95.00   1.00   10.00    --   22.00  56.00 170.81  101
  4  \w     -3.00  99.00   1.00   10.00    --   26.00  60.00 -98.85  102
  5  \w    -30.00  71.00   1.00   92.50    --   42.00 -60.00 101.93  101
  6  \w   -135.00 -34.00   1.00   92.50    --  -62.64 -57.00  90.00  101
  7  \w   -135.00 -34.00   1.00   92.50    --  -62.64 -60.00-177.13  101
  8  \w   -135.00 -34.00   1.00   92.50    --  -62.64 -57.00  60.00  101
  9  \w   -135.00 -34.00   1.00   92.50    --  -62.64 -60.00 123.13  101
 10  \w     37.00 138.00   1.00   92.50    --   64.83  57.00-180.00  101
 11  \w     36.00 138.00   1.00   92.50    --   64.83  59.00-106.48  102
 12  \w     36.00 138.00   1.00   92.50    --   64.83  60.00  20.88  102
 13  \w     37.00 138.00   1.00   92.50    --   64.83  57.00 120.00  101
 14  \w     -8.00  94.00   1.00   92.50    --   64.83 -60.00 -89.96  102
 15  \w     -8.00  94.00   1.00   92.50    --   64.83 -60.00  85.89  102
 16  \w     -8.00  93.00   1.00   92.50    --   64.83 -59.00 122.96  101
 17  \w     -8.00  94.00   1.00   92.50    --   64.83 -60.00 172.87  102
 18  \w     37.00 138.00   1.00   92.50    --   64.83  57.00 -30.00  101
 19  \w     37.00 138.00   1.00   92.50    --   64.83  57.00  60.00  101
 20  \w     37.00 138.00   1.00   92.50    --   64.83  57.00 -60.00  101
 21  \w     -8.00  42.00   1.00   92.50    --   64.83 -60.00  49.06   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0695656000
_diffrn_orient_matrix_UB_12      -0.0003442000
_diffrn_orient_matrix_UB_13      0.0591167000
_diffrn_orient_matrix_UB_21      -0.0767032000
_diffrn_orient_matrix_UB_22      0.0514046000
_diffrn_orient_matrix_UB_23      0.0349818000
_diffrn_orient_matrix_UB_31      -0.0563737000
_diffrn_orient_matrix_UB_32      -0.0702294000
_diffrn_orient_matrix_UB_33      0.0253285000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_number            2246
_diffrn_reflns_point_group_measured_fraction_full 0.614
_diffrn_reflns_point_group_measured_fraction_max 0.566
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         45.276
_diffrn_reflns_theta_min         3.267
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       block
_exptl_crystal_F_000             176
_exptl_crystal_preparation       'Used as purchased'
_exptl_crystal_recrystallization_method n/a
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   3(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         2246
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1027P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                1947
_reflns_number_total             2246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp01235a2.cif
_cod_data_source_block           21bh009_cd
_cod_original_formula_sum        'C4 N2 H6'
_cod_database_code               7244957
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     52.01
_olex2_refinement_description
;
1. Restrained distances
 C4'-H4'B
 1.059 with sigma of 0.02
 C4'-H4'C
 1.059 with sigma of 0.02
 C4'-H4'A
 1.059 with sigma of 0.02
 C2'-H2'
 1.083 with sigma of 0.02
 C1'-H1'
 1.083 with sigma of 0.02
 N1'-H1'A
 1.009 with sigma of 0.02
;
_shelx_res_checksum              80519
_olex2_exptl_crystal_mounting_method Paratone-N
_olex2_submission_original_sample_id 2mim
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 6.154
_oxdiff_exptl_absorpt_empirical_full_min 0.249