Direct Amination of Arenes with Azodicarboxylates Catalyzed by Bisulfate Salt/HFIP Association.
Tang, Ren-Jin; Retailleau, Pascal; Milcent, Thierry; Crousse, Benoit; ACS omega 4 (2019) 8960–8966; doi:10.1021/acsomega.9b00781

data_4515018
_publ_section_title
;
 Direct Amination of Arenes with Azodicarboxylates Catalyzed by Bisulfate
 Salt/HFIP Association.
;
_journal_issue                   5
_journal_name_full               'ACS omega'
_journal_page_first              8960
_journal_page_last               8966
_journal_paper_doi               10.1021/acsomega.9b00781
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C17 H20 N2 O4'
_chemical_formula_sum            'C17 H20 N2 O4'
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_cell_angle_beta                 102.033(5)
_cell_angle_gamma                90
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_diffrn_ambient_environment      air
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_diffrn_detector                 'Dectris PILATUS3R 200K HPAD'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device       'four-circle XtaLabPro diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.996
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_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41415
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.654
_diffrn_reflns_theta_min         3.658
_diffrn_source                   'micro-focus sealed X-ray tube'
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_exptl_absorpt_coefficient_mu    0.090
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_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.14
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_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         8603
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0579P)^2^+1.0831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5729
_reflns_number_total             8604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00781_si_002.cif
_cod_data_source_block           exp_2
_cod_database_code               4515018
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              96542
_shelx_hkl_checksum              2149