Structure-Based Design of High-Affinity Fluorescent Probes for the Neuropeptide Y Y<sub>1</sub> Receptor.
Müller, Christoph; Gleixner, Jakob; Tahk, Maris-Johanna; Kopanchuk, Sergei; Laasfeld, Tõnis; Weinhart, Michael; Schollmeyer, Dieter; Betschart, Martin U.; Lüdeke, Steffen; Koch, Pierre; Rinken, Ago; Keller, Max; Journal of medicinal chemistry 65 (2022) 4832–4853; doi:10.1021/acs.jmedchem.1c02033

data_1566736
_publ_section_title
;
 Structure-Based Design of High-Affinity Fluorescent Probes for the
 Neuropeptide Y Y<sub>1</sub> Receptor.
;
_journal_issue                   6
_journal_name_full               'Journal of medicinal chemistry'
_journal_page_first              4832
_journal_page_last               4853
_journal_paper_doi               10.1021/acs.jmedchem.1c02033
_journal_volume                  65
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H14 O3'
_chemical_formula_sum            'C15 H14 O3'
_chemical_formula_weight         242.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   5.5437(2)
_cell_length_b                   8.4551(3)
_cell_length_c                   52.420(3)
_cell_measurement_reflns_used    58849
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.61
_cell_measurement_theta_min      3.38
_cell_volume                     2457.06(19)
_computing_cell_refinement       'X-Area Recipe 1.34.0.0 (STOE, 2019)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)'
_computing_data_reduction        'X-Area Integrate 1.77.0.0 (STOE, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      ' 6848 frames, detector distance = 40 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            35814
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.993
_diffrn_reflns_theta_max         67.993
_diffrn_reflns_theta_min         5.062
_diffrn_source                   'Primux 100 micro'
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 1506 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.19(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0597P)^2^+0.8496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.672
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                4084
_reflns_number_total             4448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jm1c02033_si_003.cif
_cod_data_source_block           (R)-16
_cod_original_cell_volume        2457.05(17)
_cod_database_code               1566736
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.897
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              31786
_shelx_hkl_checksum              25136