Photoactivatable Fluorescent Tags for Dual-Modality Positron Emission Tomography Optical Imaging.
Guillou, Amaury; Nisli, Eda; Klingler, Simon; Linden, Anthony; Holland, Jason P.; Journal of medicinal chemistry 65 (2022) 811–823; doi:10.1021/acs.jmedchem.1c01899

data_1566281
_publ_section_title
;
 Photoactivatable Fluorescent Tags for Dual-Modality Positron Emission
 Tomography Optical Imaging.
;
_journal_issue                   1
_journal_name_full               'Journal of medicinal chemistry'
_journal_page_first              811
_journal_page_last               823
_journal_paper_doi               10.1021/acs.jmedchem.1c01899
_journal_volume                  65
_journal_year                    2022
_chemical_formula_moiety         'C37 H47 F6 N4 O4 P, 1.5(C4 H10 O)'
_chemical_formula_sum            'C43 H62 F6 N4 O5.5 P'
_chemical_formula_weight         867.93
_chemical_name_systematic
;
N-(9-(2-(4-(tert-butoxycarbonyl)piperazine-1-carbonyl)phenyl)-6-
(diethylamino)-3H-xanthen-3-ylidene)-N-ethylethanaminium 
hexafluorophosphate 1.5 diethyl ether solvate
;
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                103.6966(18)
_cell_angle_beta                 99.4485(18)
_cell_angle_gamma                117.548(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1015(3)
_cell_length_b                   13.9905(3)
_cell_length_c                   14.3129(3)
_cell_measurement_reflns_used    28928
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      79.0120
_cell_measurement_theta_min      3.8010
_cell_volume                     2142.83(10)
_computing_cell_refinement
'CrysAlisPro, Version 1.171.40.84a (Rigaku Oxford Diffraction, 2020)'
_computing_data_collection
'CrysAlisPro, Version 1.171.40.84a (Rigaku Oxford Diffraction, 2020)'
_computing_data_reduction
'CrysAlisPro, Version 1.171.40.84a (Rigaku Oxford Diffraction, 2020)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-2018 and PLATON (Spek, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(2)
_diffrn_detector                 'hybrid pixel area detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type
'Pilatus 200K hybrid pixel area detector on \k goniostat'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'four-circle \k-geometry diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction XtaLAB Synergy, dual radiation diffractometer'
_diffrn_measurement_method       '\w scans'
_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  0.0353
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            46395
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.445
_diffrn_reflns_theta_min         3.352
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray source'
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model 
plus an empirical absorption correction using spherical harmonics, 
implemented in the SCALE3 ABSPACK scaling algorithm.
CrysAlisPro, Version 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       needle
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_platon_squeeze_details          'see _refine_special_details'
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.00116(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018 (Sheldrick, 2015b)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+0.7245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8239
_reflns_number_total             9146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jm1c01899_si_001.cif
_cod_data_source_block           7
_cod_original_cell_volume        2142.82(9)
_cod_original_formula_sum        'C43 H62 F6 N4 O5.50 P'
_cod_database_code               1566281
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.828
_oxdiff_exptl_absorpt_empirical_full_max 1.247
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              98973
_shelx_hkl_checksum              78148
_shelx_fab_checksum              14068