Oxidative damage of proline residues by nitrate radicals (NO<sub>3</sub>˙): a kinetic and product study.
Nathanael, Joses G.; White, Jonathan M.; Richter, Annika; Nuske, Madison R.; Wille, Uta; Organic & biomolecular chemistry 18 (2020) 6949–6957; doi:10.1039/d0ob01337d

data_7157682
_publ_section_title
;
 Oxidative damage of proline residues by nitrate radicals
 (NO<sub>3</sub>&#x02D9;): a kinetic and product study.
;
_journal_issue                   35
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6949
_journal_page_last               6957
_journal_paper_doi               10.1039/d0ob01337d
_journal_volume                  18
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_sum            'C15 H18 N4 O7'
_chemical_formula_weight         366.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-03-21 deposited with the CCDC.	2020-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.126(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.7625(2)
_cell_length_b                   13.0451(8)
_cell_length_c                   13.8262(10)
_cell_measurement_reflns_used    1313
_cell_measurement_temperature    130.0(1)
_cell_measurement_theta_max      74.2030
_cell_measurement_theta_min      4.6330
_cell_volume                     855.55(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4959
_diffrn_reflns_point_group_measured_fraction_full 0.814
_diffrn_reflns_point_group_measured_fraction_max 0.776
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.735
_diffrn_reflns_theta_min         4.669
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       needle
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.508
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 705 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2723
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0542P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.537
_reflns_Friedel_fraction_full    0.614
_reflns_Friedel_fraction_max     0.567
_reflns_number_gt                2335
_reflns_number_total             2723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob01337d2.cif
_cod_data_source_block           prophe
_cod_depositor_comments          'Adding full bibliography for 7157682.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7157682
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     'Joses (UW) JN_3-2PFI_A1-1-F33'
_oxdiff_exptl_absorpt_empirical_full_min 0.752
_oxdiff_exptl_absorpt_empirical_full_max 1.424
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              41849