Synthesis, photophysics and photosensitizing hydrogen evolution of a near-infrared heavy-atom-free sensitizer
Lin, Ming-Sui; Nie, Qing-Bin; Chen, Jia-Nan; Liu, Ze-Yu; Wu, Qiao-Yu; Liu, Xiao-Feng; Liu, Chao; Pan, Zhong-Hua; Xiao, Wang-Chuan; Luo, Geng-Geng; New Journal of Chemistry 49 (2025) 7647–7654; doi:10.1039/D5NJ00537J

data_7063738
_publ_section_title
;
 Synthesis, photophysics and photosensitizing hydrogen evolution of a
 near-infrared heavy-atom-free sensitizer
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7647
_journal_page_last               7654
_journal_paper_doi               10.1039/D5NJ00537J
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C16 H10 B F2 N3'
_chemical_formula_sum            'C16 H10 B F2 N3'
_chemical_formula_weight         293.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-03-24
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-03-25 deposited with the CCDC.	2025-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.741(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9084(13)
_cell_length_b                   19.068(3)
_cell_length_c                   10.7534(18)
_cell_measurement_reflns_used    888
_cell_measurement_temperature    393.15
_cell_measurement_theta_max      28.6210
_cell_measurement_theta_min      3.3690
_cell_volume                     1411.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      393.15
_diffrn_detector_area_resol_mean 16.1213
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.839
_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    -56.00  54.00   1.00   13.50    --   16.81 -19.00 -60.00  110
  2  \w    -17.00  14.00   1.00   13.50    --  -17.59 -99.00 -30.00   31
  3  \w    -25.00  14.00   1.00   13.50    --  -17.59 -99.00 -90.00   39
  4  \w     60.00  88.00   1.00   13.50    --   16.81 178.00 -60.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2950
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.085
_diffrn_reflns_theta_min         3.146
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.049(4)
_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   1.054
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1595
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0614P)^2^+0.1987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                933
_reflns_number_total             1595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00537j2.cif
_cod_data_source_block           exp_3019
_cod_depositor_comments
'Adding full bibliography for 7063738--7063739.cif.'
_cod_database_code               7063738
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 F1A-B1 = F1-B1
 1.39 with sigma of 0.0001
 B1-F1 \\sim B1-F1A
 with sigma of 0.02
 F1A-B1 \\sim F1-B1
 with sigma of 0.02
 F1-B1 \\sim F1A-B1
 with sigma of 0.001
2. Uiso/Uaniso restraints and constraints
F1A \\sim F1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
F1 \\sim F1A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
3. Rigid body (RIGU) restrains
 F1A, F1, B1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: F1(0.5) F1A(0.5)
;
_shelx_res_checksum              3541
_shelx_hkl_checksum              4230
_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 2.037
_oxdiff_exptl_absorpt_empirical_full_min 0.439