Nano-assemblies from J‑aggregated dyes to improve the selectivity of H2S-activatable photosensitizer
Zhang, Dongsheng; Xiong, Ming-Chen; Niu, Li-Ya; Yang, Qing-Zheng; Chemical Communications  (2022) –; doi:10.1039/D2CC04191J

data_7130531
_publ_section_title
;
 Nano-assemblies from J&#x2011;aggregated dyes to improve the selectivity
 of H2S-activatable photosensitizer
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04191J
_journal_year                    2022
_chemical_formula_moiety         '1.5(C H2 Cl2), C42 H25 B F2 N6 O6'
_chemical_formula_sum            'C43.5 H28 B Cl3 F2 N6 O6'
_chemical_formula_weight         885.923
_chemical_name_systematic        B-NO2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2022-07-11
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.05.31 svn.r152b0213 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-07-22 deposited with the CCDC.	2022-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.187(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3763(3)
_cell_length_b                   9.1712(2)
_cell_length_c                   25.6188(5)
_cell_measurement_reflns_used    10740
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.8440
_cell_measurement_theta_min      3.4460
_cell_volume                     4082.63(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9492
_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     96.00 170.00   0.50    1.20    --  104.75  61.00 -60.00  148
  2  \w     98.00 168.00   0.50    1.20    --  104.75  61.00-120.00  140
  3  \w     93.00 178.00   0.50    1.20    --  104.75  17.00-140.00  170
  4  \w    105.00 177.00   0.50    1.20    --  104.75  15.00 -60.00  144
  5  \w     36.00  62.00   0.50    0.20    --   47.03  17.00-140.00   52
  6  \w   -120.00 -34.00   0.50    0.20    --  -47.03 -17.00  50.00  172
  7  \w   -124.00 -98.00   0.50    1.20    -- -102.00 -17.00  50.00   52
  8  \w    -66.00 -33.00   0.50    1.20    -- -102.00  61.00  30.00   66
  9  \w    -94.00 -30.00   0.50    1.20    -- -102.00  77.00  30.00  128
 10  \w   -103.00 -61.00   0.50    1.20    -- -102.00  77.00   0.00   84
 11  \w    -68.00 -34.00   0.50    1.20    -- -102.00  61.00   0.00   68
 12  \w   -102.00 -30.00   0.50    1.20    -- -102.00  77.00 -60.00  144
 13  \w    -68.00 -42.00   0.50    1.20    -- -102.00  61.00-150.00   52
 14  \w    -21.00   5.00   0.50    0.20    --  -47.03  17.00-140.00   52
 15  \w    -17.00  27.00   0.50    0.20    --  -47.03  19.00   0.00   88
 16  \w    -24.00   1.00   0.50    0.20    --   47.03 -17.00  50.00   50
 17  \w    -22.00  44.00   0.50    0.20    --   47.03 -37.00 -90.00  132
 18  \w     68.00  97.00   0.50    1.20    --  104.75 -94.00-120.00   58
 19  \w     36.00  62.00   0.50    1.20    --  104.75 -94.00-120.00   52
 20  \w    -25.00  28.00   0.50    0.20    --   47.03 -19.00 -30.00  106
 21  \w     80.00 105.00   0.50    1.20    --  104.75 125.00  60.00   50
 22  \w    153.00 178.00   0.50    1.20    --  104.75 125.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.9988
_diffrn_reflns_Laue_measured_fraction_max 0.9492
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28422
_diffrn_reflns_point_group_measured_fraction_full 0.9988
_diffrn_reflns_point_group_measured_fraction_max 0.9492
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.67
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    2.601
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             1822.615
_exptl_crystal_preparation       1
_exptl_crystal_recrystallization_method 1
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.3063
_refine_diff_density_min         -0.2896
_refine_diff_density_rms         0.0655
_refine_ls_d_res_high            0.7923
_refine_ls_d_res_low             12.8093
_refine_ls_extinction_coef       0.0004
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0358
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    58
_refine_ls_number_parameters     598
_refine_ls_number_reflns         8171
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.0347
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+2.3368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -21
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              -17
_reflns_number_gt                6550
_reflns_number_total             8171
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2cc04191j2.cif
_cod_data_source_block           exp_9624_auto
_cod_database_code               7130531
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl01-C22 \\sim Cl-C22A
 with sigma of 0.02
 Cl02-C22 \\sim Cl2-C22A
 with sigma of 0.02
 Cl01-Cl02 \\sim Cl-Cl2
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C22A, Cl, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl)=Sof(Cl2)=Sof(C22A)=Sof(H22c)=Sof(H22d)=1-FVAR(1)
 Sof(Cl01)=Sof(Cl02)=Sof(C22)=Sof(H22a)=Sof(H22b)=FVAR(1)
 Fixed Sof: Cl00(0.5) Cl1(0.5) C3(0.5) H3a(0.5) H3b(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C22A(H22c,H22d), C3(H3a,H3b)
5.b Aromatic/amide H refined with riding coordinates:
 C00Q(H00Q), C00S(H00S), C00V(H00V), C00W(H00W), C00Z(H00Z), C010(H010),
 C011(H011), C013(H013), C016(H016), C017(H017), C018(H018), C019(H019),
 C01B(H01B), C01D(H01D), C01F(H01F), C01H(H01H), C01I(H01I), C01J(H01J),
 C01K(H01K), C01L(H01L), C01N(H01N), C01O(H01O)
5.c Idealised Me refined as rotating group:
 C01M(H01a,H01c,H01e)
;
_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
;