Time-resolved luminescence detection of peroxynitrite using a reactivity-based lanthanide probe
Breen, Colum; Pal, Robert; Elsegood, Mark R. J.; Teat, Simon J.; Iza, Felipe; Wende, Kristian; Buckley, Benjamin R.; Butler, Stephen J.; Chemical Science 11 (2020) 3164–3170; doi:10.1039/C9SC06053G

data_1557338
_publ_section_title
;
 Time-resolved luminescence detection of peroxynitrite using a
 reactivity-based lanthanide probe
;
_journal_issue                   12
_journal_name_full               'Chemical Science'
_journal_page_first              3164
_journal_page_last               3170
_journal_paper_doi               10.1039/C9SC06053G
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C31 H37 B Eu N5 O9, 8(H2 O)'
_chemical_formula_sum            'C31 H53 B Eu N5 O17'
_chemical_formula_weight         930.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-11-14 deposited with the CCDC.	2020-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.300(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2696(5)
_cell_length_b                   15.8873(6)
_cell_length_c                   18.2435(7)
_cell_measurement_reflns_used    9168
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.97
_cell_measurement_theta_min      3.07
_cell_volume                     3839.7(3)
_computing_cell_refinement       'Bruker SAINT v8.38a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.38a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\w/\q shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            159626
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         36.004
_diffrn_reflns_theta_min         1.744
_diffrn_source                   'Advanced Light Source station 11.3.1'
_exptl_absorpt_coefficient_mu    1.815
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2016/2, Sheldrick, G.M., (2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1912
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.889
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.00220(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         16877
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+2.9825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15100
_reflns_number_total             16877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06053g2.cif
_cod_data_source_block           Eu1
_cod_depositor_comments
;Adding full bibliography for 1557338.cif.

 Adding full bibliography for 1557338.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1557338
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.854
_shelx_res_checksum              60747
_shelx_fab_checksum              9070