Site-Selective Conversion of Azido Groups at Carbonyl α-Positions to Diazo Groups in Diazido and Triazido Compounds.
Yokoi, Taiki; Tanimoto, Hiroki; Ueda, Tomomi; Morimoto, Tsumoru; Kakiuchi, Kiyomi; The Journal of organic chemistry 83 (2018) 12103–12121; doi:10.1021/acs.joc.8b02074

data_4035186
_publ_section_title
;
 Site-Selective Conversion of Azido Groups at Carbonyl \a-Positions to
 Diazo Groups in Diazido and Triazido Compounds.
;
_journal_issue                   19
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12103
_journal_page_last               12121
_journal_paper_doi               10.1021/acs.joc.8b02074
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C22 H21 N3 O3 S'
_chemical_formula_sum            'C22 H21 N3 O3 S'
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_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.126(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
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_cell_length_b                   9.68067(18)
_cell_length_c                   20.4861(4)
_cell_measurement_reflns_used    26483
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_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.02
_cell_volume                     2037.49(8)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
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_computing_molecular_graphics    'CrystalStructure 4.2.4'
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_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_k_min       -12
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_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33730
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.016
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
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_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.020
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_refine_diff_density_min         -0.35
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_refine_ls_number_reflns         4683
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0442P)^2^+1.0946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0948
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