Iodonitrene in Action: Direct Transformation of Amino Acids into Terminal Diazirines and <sup>15</sup>N<sub>2</sub>-Diazirines and Their Application as Hyperpolarized Markers.
Glachet, Thomas; Marzag, Hamid; Saraiva Rosa, Nathalie; Colell, Johannes F. P.; Zhang, Guannan; Warren, Warren S.; Franck, Xavier; Theis, Thomas; Reboul, Vincent; Journal of the American Chemical Society 141 (2019) 13689–13696; doi:10.1021/jacs.9b07035

data_4128890
_publ_section_title
;
 Iodonitrene in Action: Direct Transformation of Amino Acids into Terminal
 Diazirines and <sup>15</sup>N<sub>2</sub>-Diazirines and Their
 Application as Hyperpolarized Markers.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13689
_journal_page_last               13696
_journal_paper_doi               10.1021/jacs.9b07035
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C15 H20 N4 O3'
_chemical_formula_sum            'C15 H20 N4 O3'
_chemical_formula_weight         304.35
_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-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 99.557(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1878(16)
_cell_length_b                   7.9625(15)
_cell_length_c                   19.590(3)
_cell_measurement_reflns_used    4918
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.77
_cell_volume                     1567.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_av_unetI/netI     0.1372
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32808
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.691
_diffrn_reflns_theta_min         2.435
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2016/2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.3847
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1477 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.9(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         9636
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0778
_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^)+(0.0555P)^2^+0.2407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1944
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                5510
_reflns_number_total             9636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b07035_si_004.cif
_cod_data_source_block           glachet6_0m_a
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4128890
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              41966
_shelx_hkl_checksum              88692