Modulating the photolysis of aryl azides in a supramolecular host to develop photoactivatable fluorophores.
Qiu, Xujun; Pohl, Eric; Jung, André; Cai, Qianyu; Su, Haopu; Fuhr, Olaf; Schepers, Ute; Bräse, Stefan; Chemical communications (Cambridge, England) 60 (2024) 12856–12859; doi:10.1039/d4cc03907f

data_7133812
_publ_section_title
;
 Modulating the photolysis of aryl azides in a supramolecular host to
 develop photoactivatable fluorophores.
;
_journal_issue                   88
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12856
_journal_page_last               12859
_journal_paper_doi               10.1039/d4cc03907f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'Cl, 2.5(H2 O), C24 H20 N5'
_chemical_formula_sum            'C24 H25 Cl N5 O2.5'
_chemical_formula_weight         458.94
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-23
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-25 deposited with the CCDC.	2024-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                101.497(2)
_cell_angle_beta                 93.876(2)
_cell_angle_gamma                103.476(2)
_cell_formula_units_Z            4
_cell_length_a                   9.5693(2)
_cell_length_b                   10.1473(2)
_cell_length_c                   24.8566(6)
_cell_measurement_reflns_used    35790
_cell_measurement_temperature    180
_cell_measurement_theta_max      64.52
_cell_measurement_theta_min      3.18
_cell_volume                     2283.56(9)
_computing_cell_refinement
;
X-Area Recipe 2.0.1 (STOE, 2023)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.192.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.15.0 (STOE, 2023)
X-Area LANA 2.7.12 (STOE, 2023)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.3, Darmstadt 2023
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      180
_diffrn_detector                 'Eiger R 4M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
 2047 frames, detector distance = 80 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37773
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         62.499
_diffrn_reflns_theta_min         3.180
_diffrn_source                   'Metal Jet D2+'
_diffrn_source_current           3.57
_diffrn_source_power             0.250
_diffrn_source_target            Ga
_diffrn_source_type              'Metal Jet D2+'
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  0.9678
_exptl_absorpt_correction_T_min  0.8774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          1.490
_refine_ls_shift/su_mean         0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1465P)^2^+1.0542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8429
_reflns_number_total             10827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03907f2.cif
_cod_data_source_block           xqr271s-2
_cod_depositor_comments
'Adding full bibliography for 7133811--7133812.cif.'
_cod_original_formula_sum        'C24 H25 Cl N5 O2.50'
_cod_database_code               7133812
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.874
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B), O5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C41(H41), C42(H42), C45(H45),
  C46(H46), C47(H47)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              72841
_shelx_hkl_checksum              1277
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '80.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '15.5 cm'
_stoe_detector_size_y            '16.2 cm'
_stoe_evaluation_integration_a   18.0
_stoe_evaluation_integration_b   0.4
_stoe_evaluation_integration_ems 0.014
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 97.8
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 128.2
_stoe_evaluation_lana_max_2theta_desired 125.0
_stoe_evaluation_lana_mean_redundancy 3.5
_stoe_evaluation_lana_number_refls_after_or 37777
_stoe_evaluation_lana_number_refls_outliers 6932
_stoe_evaluation_lana_number_refls_total 44709
_stoe_evaluation_lana_number_refls_unique 10830
_stoe_evaluation_lana_number_refls_written 37777
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
2Theta          12.0   25.4   38.8   52.2   65.6   79.0   92.4  105.8  119.2
<Resolution>    5.55   2.91   1.94   1.51   1.24   1.06   0.93   0.84   0.78
N(total)          92    380   1607   6113   8138   7794   8323   7405   4857
<Redundancy>     1.4    1.5    2.3    4.9    4.7    3.8    3.7    3.2    2.4
Complet. [%%]    86.6   92.7   98.5  100.0   99.9   97.2   99.2   99.2   93.6
<I/sigma>      219.3  216.0   78.7   39.5   26.3   15.3    7.9    5.1    4.6
R(int)         0.013  0.019  0.019  0.021  0.022  0.030  0.048  0.070  0.078
;
_stoe_measurement_identifier     XQR271S-2
_stoe_measurement_max_exposure_per_frame '1.0 s'
_stoe_measurement_mean_exposure_per_frame '1.0 s'
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '34 min'
_stoe_measurement_total_frame_number 2047
_stoe_measurement_total_run_number 24
_stoe_measurement_tube_power     '250 W'