Oxidation of diazenyl-protected N-heterocycles – a new entry to functionalized lactams
Petrović, Martina; Scarpi, Dina; Nieger, Martin; Jung, Nicole; Occhiato, Ernesto G.; Bräse, Stefan; RSC Adv. 7 (2017) 9461–; doi:10.1039/C6RA26546D

data_7227608
_publ_section_title
;
 Oxidation of diazenyl-protected N-heterocycles -- a new entry to
 functionalized lactams
;
_journal_issue                   16
_journal_name_full               'RSC Adv.'
_journal_page_first              9461
_journal_paper_doi               10.1039/C6RA26546D
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C18 H19 N3 O2'
_chemical_formula_sum            'C18 H19 N3 O2'
_chemical_formula_weight         309.36
_chemical_name_systematic
'4-(3,4-dihydro-1H-isoquinolin-2-ylazo)-benzoic acid ethyl ester'
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-10-17 deposited with the CCDC.
2016-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.355(2)
_cell_angle_gamma                90
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_cell_length_c                   7.7858(7)
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_computing_cell_refinement       'APEX3 v2015.9-RC2 (Bruker AXS)'
_computing_data_collection       'APEX3 v2015.9-RC2 (Bruker AXS)'
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_computing_molecular_graphics    Shelxtl
_computing_publication_material  publCIF
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE with Photon100 detector'
_diffrn_measurement_method       'rotation in \f and \w, 1\%, shutterless'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_min       -7
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_diffrn_reflns_limit_k_min       -41
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_diffrn_reflns_limit_l_min       -8
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        67.679
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_diffrn_source                   'INCOATEC microfocus sealed tube'
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_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
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_refine_diff_density_min         -0.239
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_refine_ls_extinction_coef       0.0037(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.6671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                2951
_reflns_number_total             3057
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           sb840_hy_compound_3c_5
_cod_database_code               7227608
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              61775