A Photoactivatable Probe for Super-Resolution Imaging of Enzymatic Activity in Live Cells.
Halabi, Elias A.; Thiel, Zacharias; Trapp, Nils; Pinotsi, Dorothea; Rivera-Fuentes, Pablo; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07748

data_4126351
_publ_section_title
;
 A Photoactivatable Probe for Super-Resolution Imaging of Enzymatic
 Activity in Live Cells.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07748
_journal_year                    2017
_chemical_formula_moiety         'C29 H23 N3 O4'
_chemical_formula_sum            'C29 H23 N3 O4'
_chemical_formula_weight         477.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                66.2730(10)
_cell_angle_beta                 88.0930(10)
_cell_angle_gamma                64.5700(10)
_cell_formula_units_Z            2
_cell_length_a                   10.07610(10)
_cell_length_b                   11.03250(10)
_cell_length_c                   12.38880(10)
_cell_measurement_reflns_used    30033
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      78.7670
_cell_measurement_theta_min      3.9330
_cell_volume                     1122.30(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.8d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.8d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.8d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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   -115.00 -25.00   0.50    0.15    --  -48.56 -77.00  60.00  180
  2  \w   -115.00 -25.00   0.50    0.15    --  -48.56 -77.00-180.00  180
  3  \w   -115.00 -25.00   0.50    0.15    --  -48.56 -77.00 -90.00  180
  4  \w   -121.00 -37.00   0.50    0.15    --  -48.56 178.00 -30.00  168
  5  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00  90.00  180
  6  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00  30.00  180
  7  \w    -94.00  -4.00   0.50    0.15    --  -70.00  77.00 -90.00  180
  8  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00-150.00  180
  9  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00 -60.00  180
 10  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00   0.00  180
 11  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00 150.00  180
 12  \w     86.00 176.00   0.50    0.15    --  110.00  77.00  30.00  180
 13  \w     86.00 176.00   0.50    0.15    --  110.00  77.00  90.00  180
 14  \w     41.00 109.00   0.50    0.15    --  110.00 -99.00  30.00  136
 15  \w     86.00 176.00   0.50    0.15    --  110.00  77.00-120.00  180
 16  \w     94.00 177.00   0.50    0.15    --  110.00  57.00 -90.00  166
 17  \w     41.00 109.00   0.50    0.15    --  110.00 -99.00 -90.00  136
 18  \w     86.00 176.00   0.50    0.15    --  110.00  77.00-180.00  180
 19  \w     41.00 109.00   0.50    0.15    --  110.00 -99.00 150.00  136
 20  \w     86.00 176.00   0.50    0.15    --  110.00  77.00   0.00  180
 21  \w     86.00 176.00   0.50    0.15    --  110.00  77.00  60.00  180
 22  \w     86.00 176.00   0.50    0.15    --  110.00  77.00 -60.00  180
 23  \w     86.00 176.00   0.50    0.15    --  110.00  77.00 120.00  180
 24  \w     86.00 176.00   0.50    0.15    --  110.00  77.00-150.00  180
 25  \w     86.00 176.00   0.50    0.15    --  110.00  77.00 -30.00  180
 26  \w   -120.00 -33.00   0.50    0.15    --  -48.56 -57.00  90.00  174
 27  \w   -115.00 -25.00   0.50    0.15    --  -48.56 -77.00 -30.00  180
 28  \w     25.00 115.00   0.50    0.15    --   48.56  77.00-120.00  180
 29  \w     60.00 120.00   0.50    0.15    --   48.56 178.00  90.00  120
 30  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00 -90.00  180
 31  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00 -30.00  180
 32  \w    -95.00 -10.00   0.50    0.15    --  -70.00 125.00   0.00  170
 33  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00-180.00  180
 34  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00  60.00  180
 35  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00 120.00  180
 36  \w   -136.00 -46.00   0.50    0.15    --  -70.00 -77.00-120.00  180
 37  \w   -145.00 -56.00   0.50    0.15    --  -70.00 -38.00 -60.00  178
 38  \w     97.00 177.00   0.50    0.15    --  110.00  38.00 150.00  160
 39  \w     41.00 109.00   0.50    0.15    --  110.00 -99.00  90.00  136
 40  \w     97.00 177.00   0.50    0.15    --  110.00  38.00-150.00  160
 41  \w     97.00 177.00   0.50    0.15    --  110.00  38.00-120.00  160
 42  \w     94.00 177.00   0.50    0.15    --  110.00  57.00 -60.00  166
 43  \w     41.00 109.00   0.50    0.15    --  110.00 -99.00 -30.00  136
 44  \w     94.00 177.00   0.50    0.15    --  110.00  57.00  30.00  166
 45  \w     94.00 177.00   0.50    0.15    --  110.00  57.00 -30.00  166
 46  \w     97.00 177.00   0.50    0.15    --  110.00  38.00 -90.00  160
 47  \w     86.00 176.00   0.50    0.15    --  110.00  77.00 150.00  180
 48  \w     94.00 177.00   0.50    0.15    --  110.00  57.00 150.00  166
 49  \w     39.00 120.00   0.50    0.15    --  110.00-125.00   0.00  162
 50  \w     94.00 177.00   0.50    0.15    --  110.00  57.00  90.00  166
 51  \w     41.00 109.00   0.50    0.15    --  110.00 -99.00-180.00  136
 52  \w     39.00 106.00   0.50    0.15    --  110.00 -57.00   0.00  134
 53  \w     45.00 134.00   0.50    0.15    --  110.00 -77.00-150.00  178
 54  \w   -120.00 -33.00   0.50    0.15    --  -48.56 -57.00-180.00  174
 55  \w   -124.00 -34.00   0.50    0.15    --  -48.56 -38.00 -60.00  180
 56  \w     33.00 120.00   0.50    0.15    --   48.56  57.00 150.00  174
 57  \w     35.00 124.00   0.50    0.15    --   48.56  38.00  30.00  178
 58  \w   -145.00 -56.00   0.50    0.15    --  -70.00 -38.00-180.00  178
 59  \w   -141.00 -54.00   0.50    0.15    --  -70.00 -57.00 -90.00  174
 60  \w   -141.00 -54.00   0.50    0.15    --  -70.00 -57.00-120.00  174
 61  \w   -141.00 -54.00   0.50    0.15    --  -70.00 -57.00-180.00  174
 62  \w   -141.00 -54.00   0.50    0.15    --  -70.00 -57.00 150.00  174
 63  \w     94.00 177.00   0.50    0.15    --  110.00  57.00-150.00  166
 64  \w     97.00 177.00   0.50    0.15    --  110.00  38.00   0.00  160
 65  \w     97.00 177.00   0.50    0.15    --  110.00  38.00 -60.00  160
 66  \w     97.00 177.00   0.50    0.15    --  110.00  38.00  90.00  160
 67  \w     94.00 177.00   0.50    0.15    --  110.00  57.00   0.00  166
 68  \w     97.00 177.00   0.50    0.15    --  110.00  38.00  30.00  160
 69  \w     86.00 176.00   0.50    0.15    --  110.00  77.00 -90.00  180
 70  \w     94.00 177.00   0.50    0.15    --  110.00  57.00 120.00  166
 71  \w     94.00 177.00   0.50    0.15    --  110.00  57.00  60.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0928078000
_diffrn_orient_matrix_UB_12      0.1178510000
_diffrn_orient_matrix_UB_13      -0.1241700000
_diffrn_orient_matrix_UB_21      -0.0632415000
_diffrn_orient_matrix_UB_22      0.1180784000
_diffrn_orient_matrix_UB_23      0.0491454000
_diffrn_orient_matrix_UB_31      0.1299545000
_diffrn_orient_matrix_UB_32      0.0387078000
_diffrn_orient_matrix_UB_33      -0.0340266000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            52193
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.318
_diffrn_reflns_theta_min         3.954
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.8d (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4795
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0780P)^2^+0.6561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4262
_reflns_number_total             4795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07748_si_007.cif
_cod_data_source_block           pr090517_1_1
_cod_database_code               4126351
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C29 H23 N O4'
_diffrn_oxdiff_ac3_digest_frames
;
011e86f0e505174ce93e5d57d6b8a6a28f120206e82
;
_diffrn_oxdiff_ac3_digest_hkl
;
012e694e398b743384cbe44421f9924771e7c0
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29A-C28 \\sim C29-C28 \\sim C29A-C26 \\sim C29-C26
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C28, C29A, C29, C26, C16, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H26C)=Sof(H26D)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=1-FVAR(1)
 Sof(H26A)=Sof(H26B)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B), C24(H24A,H24B), C26(H26A,H26B), C26(H26C,
 H26D), C28(H28A,H28B), C28(H28C,H28D), C29(H29A,H29B), C29A(H29C,H29D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C12(H12), C15(H15), C17(H17), C19(H19), C22(H22), C23(H23), C25(H25)
5.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C)
;
_shelx_res_checksum              67920
_shelx_hkl_checksum              4524
_olex2_date_sample_data_collection 2017-05-12
_olex2_date_sample_submission    2017-05-11
_olex2_submission_original_sample_id pr090517_1_1
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.404
_oxdiff_exptl_absorpt_empirical_full_min 0.807