Observing bioorthogonal macrocyclizations in the nuclear envelope of live cells using on/on fluorescence lifetime microscopy.
Pim, Sebastian; Bourgès, Anaïs C; Wu, Dan; Durán-Sampedro, Gonzalo; Garre, Massimiliano; O'Shea, Donal F; Chemical science 15 (2024) 14913–14923; doi:10.1039/d4sc03489a

data_1572775
_publ_section_title
;
 Observing bioorthogonal macrocyclizations in the nuclear envelope of live
 cells using on/on fluorescence lifetime microscopy.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              14913
_journal_page_last               14923
_journal_paper_doi               10.1039/d4sc03489a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C H Cl3, C44 H36 B F2 N9 O2'
_chemical_formula_sum            'C45 H37 B Cl3 F2 N9 O2'
_chemical_formula_weight         890.99
_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
_audit_creation_date             2018-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2024-03-06 deposited with the CCDC.	2024-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                106.314(5)
_cell_angle_beta                 104.337(4)
_cell_angle_gamma                105.219(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0839(13)
_cell_length_b                   13.719(2)
_cell_length_c                   15.383(3)
_cell_measurement_reflns_used    9097
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.28
_cell_measurement_theta_min      2.75
_cell_volume                     2031.6(6)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT v8.38A (Bruker, 2016)'
_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_temperature      100(2)
_diffrn_detector                 'CMOS area detector'
_diffrn_detector_area_resol_mean 5.12
_diffrn_detector_type            'Bruker PHOTON 50'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST ECO'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_detector       'Bruker PHOTON 50'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16496
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.547
_diffrn_reflns_theta_min         2.892
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_T_max  0.745373
_exptl_absorpt_correction_T_min  0.708248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 108235 reflections, Rint = 0.0667
 (64601 with I > 3sig(I), Rint = 0.0570)
;
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             920
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CHCl3'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         16496
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0437P)^2^+0.9773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13715
_reflns_number_total             16496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03489a8.cif
_cod_data_source_block           tcd1068_5
_cod_database_code               1572775
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.906
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.510(2)
 0.3536(15) 0.1361(14)
2. 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
3. Restrained distances
 Cl1-C1S \\sim Cl1A-C1S \\sim Cl3A-C1S \\sim Cl3-C1S \\sim Cl2-C1S \\sim
Cl2A-C1S
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Cl1A \\sim Cl1 \\sim Cl2 \\sim Cl3 \\sim Cl2A \\sim Cl3A: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(Cl1A)=Sof(H1SA)=Sof(Cl2A)=Sof(Cl3A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(H1S)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1S(H1S), C1S(H1SA)
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C13(H13), C14(H14), C16(H16), C17(H17), C21(H21), C22(H22),
 C24(H24), C25(H25), C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C44(H44),
  C45(H45), C46(H46)
6.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              12360
_shelx_hkl_checksum              89486
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id GDS423B
_olex2_submission_special_instructions 'No special instructions were received'