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_7244956
_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         'C12 H10 O5, H2 O'
_chemical_formula_sum            'C12 H12 O6'
_chemical_formula_weight         252.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_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                103.594(3)
_cell_angle_beta                 96.171(3)
_cell_angle_gamma                98.824(4)
_cell_formula_units_Z            2
_cell_length_a                   6.6514(3)
_cell_length_b                   7.1118(3)
_cell_length_c                   12.5709(3)
_cell_measurement_reflns_used    9367
_cell_measurement_temperature    139(20)
_cell_measurement_theta_max      40.2340
_cell_measurement_theta_min      3.0200
_cell_volume                     564.73(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139(20)
_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 1.000
_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    -72.00  28.20   0.30    7.50    --    1.09 -57.00-180.00  334
  2  \w    -11.00  91.00   0.30    7.50    --   18.00  60.00  13.45  340
  3  \w     -3.00  99.00   0.30    7.50    --   26.00  59.00 119.13  340
  4  \w      2.00 102.20   0.30    7.50    --   30.00  58.00 -88.60  334
  5  \w    -34.00  66.20   0.30   30.00    --   38.00 -59.00 -41.19  334
  6  \w   -135.00 -34.80   0.30   30.00    --  -62.64 -59.00-156.86  334
  7  \w    -92.00  10.00   0.30   30.00    --  -62.64  60.00-179.79  340
  8  \w   -135.00 -34.80   0.30   30.00    --  -62.64 -58.00-126.98  334
  9  \w   -135.00 -34.80   0.30   30.00    --  -62.64 -57.00 -90.00  334
 10  \w    -92.00  10.00   0.30   30.00    --  -62.64  60.00 -37.36  340
;
_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      0.0224651000
_diffrn_orient_matrix_UB_12      0.0915057000
_diffrn_orient_matrix_UB_13      0.0405010000
_diffrn_orient_matrix_UB_21      0.0093786000
_diffrn_orient_matrix_UB_22      -0.0500422000
_diffrn_orient_matrix_UB_23      0.0423758000
_diffrn_orient_matrix_UB_31      0.1063921000
_diffrn_orient_matrix_UB_32      0.0048929000
_diffrn_orient_matrix_UB_33      -0.0032862000
_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  0.0243
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12124
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.999
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       plate
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.551
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0639P)^2^+0.1208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2461
_reflns_number_total             2799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp01235a2.cif
_cod_data_source_block           21bh011_cd_c
_cod_database_code               7244956
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
;
_shelx_res_checksum              67287
_olex2_submission_original_sample_id EN09-hydrate
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.541
_oxdiff_exptl_absorpt_empirical_full_min 0.726