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_4126350
_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      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.29600(10)
_cell_length_b                   16.68720(10)
_cell_length_c                   33.1607(3)
_cell_measurement_reflns_used    40252
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      78.9830
_cell_measurement_theta_min      5.2820
_cell_volume                     4590.67(7)
_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 0.993
_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   -114.00 -23.00   0.50    2.00    --  -47.76 -77.00-180.00  182
  2  \w   -114.00 -23.00   0.50    2.00    --  -47.76 -77.00 -60.00  182
  3  \w   -114.00 -23.00   0.50    2.00    --  -47.76 -77.00  90.00  182
  4  \w     58.00 122.00   0.50    2.00    --   47.76-178.00   0.00  128
  5  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00  60.00  182
  6  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00 -90.00  182
  7  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00 120.00  182
  8  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00 -30.00  182
  9  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00-150.00  182
 10  \w    -85.00   1.00   0.50    2.00    --  -70.00 102.00  57.00  172
 11  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00  30.00  182
 12  \w     87.00 177.00   0.50    2.00    --  111.75  77.00 -90.00  180
 13  \w     40.00 120.00   0.50    2.00    --  111.75-125.00-120.00  160
 14  \w     87.00 177.00   0.50    2.00    --  111.75  77.00 120.00  180
 15  \w     87.00 177.00   0.50    2.00    --  111.75  77.00 150.00  180
 16  \w     87.00 177.00   0.50    2.00    --  111.75  77.00 -60.00  180
 17  \w     87.00 177.00   0.50    2.00    --  111.75  77.00-180.00  180
 18  \w     87.00 177.00   0.50    2.00    --  111.75  77.00  90.00  180
 19  \w     87.00 177.00   0.50    2.00    --  111.75  77.00-150.00  180
 20  \w     87.00 177.00   0.50    2.00    --  111.75  77.00   0.00  180
 21  \w     87.00 177.00   0.50    2.00    --  111.75  77.00  30.00  180
 22  \w     87.00 177.00   0.50    2.00    --  111.75  77.00  60.00  180
 23  \w     42.00 109.00   0.50    2.00    --  111.75 -99.00  30.00  134
 24  \w     87.00 177.00   0.50    2.00    --  111.75  77.00 -30.00  180
 25  \w     42.00 109.00   0.50    2.00    --  111.75 -99.00 120.00  134
 26  \w     42.00 109.00   0.50    2.00    --  111.75 -99.00 -90.00  134
 27  \w   -120.00 -31.00   0.50    2.00    --  -47.76 -57.00 120.00  178
 28  \w   -114.00 -23.00   0.50    2.00    --  -47.76 -77.00-120.00  182
 29  \w   -120.00 -31.00   0.50    2.00    --  -47.76 -57.00 -30.00  178
 30  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00   0.00  182
 31  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00-180.00  182
 32  \w    -95.00  -4.00   0.50    2.00    --  -70.00  77.00-120.00  182
 33  \w   -142.00 -71.00   0.50    2.00    --  -70.00-125.00-120.00  142
 34  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00  90.00  182
 35  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00 150.00  182
 36  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00 -60.00  182
 37  \w   -136.00 -45.00   0.50    2.00    --  -70.00 -77.00-120.00  182
 38  \w     42.00 109.00   0.50    2.00    --  111.75 -99.00  90.00  134
 39  \w     42.00 109.00   0.50    2.00    --  111.75 -99.00-180.00  134
 40  \w     96.00 177.00   0.50    2.00    --  111.75  38.00 -60.00  162
 41  \w     46.00 137.00   0.50    2.00    --  111.75 -77.00 -60.00  182
 42  \w     95.00 177.00   0.50    2.00    --  111.75  57.00-120.00  164
 43  \w     95.00 177.00   0.50    2.00    --  111.75  57.00  60.00  164
 44  \w     95.00 177.00   0.50    2.00    --  111.75  57.00-180.00  164
 45  \w     95.00 177.00   0.50    2.00    --  111.75  57.00 120.00  164
 46  \w     96.00 177.00   0.50    2.00    --  111.75  38.00   0.00  162
 47  \w     87.00 177.00   0.50    2.00    --  111.75  77.00-120.00  180
 48  \w   -124.00 -32.00   0.50    2.00    --  -47.76 -38.00   0.00  184
 49  \w     32.00 124.00   0.50    2.00    --   47.76  38.00 120.00  184
 50  \w     31.00 120.00   0.50    2.00    --   47.76  57.00 150.00  178
 51  \w   -142.00 -53.00   0.50    2.00    --  -70.00 -57.00-180.00  178
 52  \w   -142.00 -53.00   0.50    2.00    --  -70.00 -57.00 -90.00  178
 53  \w     96.00 177.00   0.50    2.00    --  111.75  38.00  60.00  162
 54  \w     36.00  70.00   0.50    2.00    --  111.75 -38.00  60.00   68
 55  \w     95.00 177.00   0.50    2.00    --  111.75  57.00 150.00  164
 56  \w     42.00 109.00   0.50    2.00    --  111.75 -99.00-120.00  134
 57  \w     40.00 106.00   0.50    2.00    --  111.75 -57.00-120.00  132
 58  \w     96.00 177.00   0.50    2.00    --  111.75  38.00  30.00  162
 59  \w     96.00 177.00   0.50    2.00    --  111.75  38.00-120.00  162
 60  \w     96.00 177.00   0.50    2.00    --  111.75  38.00 120.00  162
 61  \w     96.00 177.00   0.50    2.00    --  111.75  38.00 -30.00  162
;
_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      0.0541438000
_diffrn_orient_matrix_UB_12      -0.0068341000
_diffrn_orient_matrix_UB_13      -0.0443101000
_diffrn_orient_matrix_UB_21      0.0049550000
_diffrn_orient_matrix_UB_22      0.0920735000
_diffrn_orient_matrix_UB_23      -0.0032077000
_diffrn_orient_matrix_UB_31      0.1775464000
_diffrn_orient_matrix_UB_32      -0.0004904000
_diffrn_orient_matrix_UB_33      0.0135858000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1636
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            149801
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.360
_diffrn_reflns_theta_min         5.301
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.789
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0641P)^2^+3.2761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4346
_reflns_number_total             4997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07748_si_003.cif
_cod_data_source_block           pr180517_1_1
_cod_database_code               4126350
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C29 H23 N2 O4'
_diffrn_oxdiff_ac3_digest_frames
;
01be9808e8add3be5d8f79d0138068d50610254b972
;
_diffrn_oxdiff_ac3_digest_hkl
;
01cf02a5097502c2e35a5a15d9c909d79d9c72
;
_reflns_odcompleteness_completeness 99.91
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22-C16 \\sim C22A-C16
 with sigma of 0.02
 C25-C22 \\sim C25A-C22A
 with sigma of 0.02
 O3-C25 \\sim O3A-C25A
 with sigma of 0.02
 C25-C15 \\sim C25A-C15
 with sigma of 0.02
 C27-C22 \\sim C27A-C22A
 with sigma of 0.02
 C28A-C24A \\sim C28-C24
 with sigma of 0.02
 C29-C28 \\sim C29A-C28A \\sim C29-C27 \\sim C29A-C27A
 with sigma of 0.02
3. Rigid bond restraints
 C11, C15, C16, C22A, C27A, C29A, C28A, C24A, O3, C22, C24, C25, C27, C28, C29,
  O3A, C25A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O3A) \\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C27A)
\\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C24A) \\sim Ueq,
Uanis(C16) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 C11, C15, C16, C22A, C27A, C29A, C28A, C24A, O3, C22, C24, C25, C27, C28, C29,
  O3A, C25A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C22A)=Sof(C27A)=Sof(H27A)=Sof(C29A)=Sof(H29A)=Sof(C28A)=Sof(H28A)=
 Sof(C24A)=Sof(H24A)=Sof(O3A)=Sof(C25A)=1-FVAR(1)
 Sof(O3)=Sof(C22)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(C27)=Sof(H27)=Sof(C28)=
 Sof(H28)=Sof(C29)=Sof(H29)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C23(H23A,H23B)
7.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C14(H14), C27A(H27A), C29A(H29A), C28A(H28A),
 C24A(H24A), C24(H24), C27(H27), C28(H28), C29(H29)
7.c Fitted hexagon refined as free rotating group:
 C16(C22A,C27A,C29A,C28A,C24A)
7.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
;
_shelx_res_checksum              55201
_shelx_hkl_checksum              68983
_olex2_date_sample_data_collection 2017-05-18
_olex2_date_sample_submission    2017-05-18
_olex2_submission_original_sample_id pr180517_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 5.140
_oxdiff_exptl_absorpt_empirical_full_min 0.272