New Schiff base salts as sources of blue and green light in the solid state: the role of the anion and protonation
Sobczak, Paulina; Sierański, Tomasz; Świątkowski, Marcin; Trzęsowska-Kruszyńska, Agata; CrystEngComm 25 (2023) 6185–6193; doi:10.1039/D3CE00758H

data_7247581
_publ_section_title
;
 New Schiff base salts as sources of blue and green light in the solid
 state: the role of the anion and protonation
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              6185
_journal_page_last               6193
_journal_paper_doi               10.1039/D3CE00758H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C15 H14 N O3, H O4 S'
_chemical_formula_sum            'C15 H15 N O7 S'
_chemical_formula_weight         353.34
_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             2023-07-28
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-07-28 deposited with the CCDC.	2023-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.109(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.47140(10)
_cell_length_b                   9.3275(2)
_cell_length_c                   17.7797(5)
_cell_measurement_reflns_used    12883
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      78.7550
_cell_measurement_theta_min      4.7330
_cell_volume                     741.54(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.976
_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   -120.00 -33.00   0.50    6.00    --  -48.87 -57.00 -30.00  174
  2  \w   -120.00 -41.00   0.50    6.00    --  -48.87-178.00-180.00  158
  3  \w    -41.00  27.00   0.50    6.00    --  -48.87  38.00 120.00  136
  4  \w    -20.00  27.00   0.50    6.00    --  -48.87  19.00-150.00   94
  5  \w     25.00 114.00   0.50    6.00    --   48.87  77.00  30.00  178
  6  \w    -27.00  20.00   0.50    6.00    --   48.87 -19.00   0.00   94
  7  \w    -41.00 -13.00   0.50   16.00    --  -88.50  38.00-180.00   56
  8  \w    -41.00 -13.00   0.50   16.00    --  -88.50  38.00 150.00   56
  9  \w    -87.00 -19.00   0.50   16.00    --  -88.50 125.00  90.00  136
 10  \w   -164.00 -75.00   0.50   16.00    --  -88.50 -38.00-150.00  178
 11  \w    -41.00 -13.00   0.50   16.00    --  -88.50  38.00  90.00   56
 12  \w    -87.00 -19.00   0.50   16.00    --  -88.50 125.00-150.00  136
 13  \w   -160.00 -16.00   0.50   16.00    --  -88.50   0.00-150.00  288
 14  \w   -157.00 -85.00   0.50   16.00    --  -88.50 -99.00-150.00  144
 15  \w    -41.00 -13.00   0.50   16.00    --  -88.50  38.00 120.00   56
 16  \w    -41.00 -13.00   0.50   16.00    --  -88.50  38.00 -60.00   56
 17  \w    -87.00 -19.00   0.50   16.00    --  -88.50 125.00 150.00  136
 18  \w     86.00 176.00   0.50   16.00    --  110.00  77.00  30.00  180
 19  \w     38.00  66.00   0.50   16.00    --  110.00 -57.00 120.00   56
 20  \w     41.00 113.00   0.50   16.00    --  110.00-125.00  60.00  144
 21  \w     41.00 106.00   0.50   16.00    --  110.00 -99.00   0.00  130
 22  \w     41.00 106.00   0.50   16.00    --  110.00 -99.00-120.00  130
 23  \w     94.00 178.00   0.50   16.00    --  110.00 125.00  60.00  168
 24  \w     45.00 134.00   0.50   16.00    --  110.00 -77.00  60.00  178
 25  \w     41.00 106.00   0.50   16.00    --  110.00 -99.00  90.00  130
 26  \w     41.00 106.00   0.50   16.00    --  110.00 -99.00-180.00  130
 27  \w     38.00  66.00   0.50   16.00    --  110.00 -57.00 -90.00   56
 28  \w     25.00 114.00   0.50    6.00    --   48.87  77.00-120.00  178
 29  \w     25.00 114.00   0.50    6.00    --   48.87  77.00   0.00  178
 30  \w     25.00 114.00   0.50    6.00    --   48.87  77.00 120.00  178
 31  \w     25.00 114.00   0.50    6.00    --   48.87  77.00 -90.00  178
 32  \w     33.00 121.00   0.50    6.00    --   48.87  57.00  90.00  176
 33  \w     25.00 114.00   0.50    6.00    --   48.87  77.00 150.00  178
 34  \w   -154.00 -65.00   0.50   16.00    --  -88.50 -77.00  30.00  178
 35  \w   -154.00 -65.00   0.50   16.00    --  -88.50 -77.00-180.00  178
 36  \w   -154.00 -65.00   0.50   16.00    --  -88.50 -77.00 120.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0331452000
_diffrn_orient_matrix_UB_12      -0.0456742000
_diffrn_orient_matrix_UB_13      0.0828592000
_diffrn_orient_matrix_UB_21      0.3417892000
_diffrn_orient_matrix_UB_22      -0.0083829000
_diffrn_orient_matrix_UB_23      -0.0097371000
_diffrn_orient_matrix_UB_31      0.0276038000
_diffrn_orient_matrix_UB_32      0.1585269000
_diffrn_orient_matrix_UB_33      0.0233726000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24898
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.665
_diffrn_reflns_theta_min         4.741
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.327
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.86a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       prism
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.393(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2993
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0432P)^2^+0.2527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.874
_reflns_number_gt                2972
_reflns_number_total             2993
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 55.3443\% 
around [-1.00 0.00 0.01] (reciprocal) or [-1.00 0.00 -0.00] (direct)
;
_cod_data_source_file            d3ce00758h2.cif
_cod_data_source_block           ps10_s04_2_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7247579--7247585.cif.'
_cod_database_code               7247581
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H15 N1 O7 S1'
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.617
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.607(18)
 0.393(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C10(H10), C13(H13), C8(H8), C14(H14), C11(H11), C3(H3), C7(H7),
 C6(H6), C4(H4)
3.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O7(H7A)
;
_shelx_res_checksum              91624
_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 1.877
_oxdiff_exptl_absorpt_empirical_full_min 0.526
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2