1,3-Diamine Formation from an Interrupted Hofmann–Löffler Reaction: Iodine Catalyst Turnover through Ritter-Type Amination
Duhamel, Thomas; Martínez, Mario D.; Sideri, Ioanna K.; Muñiz, Kilian; ACS Catalysis 9 (2019) 7741–; doi:10.1021/acscatal.9b01566

data_4514831
_publ_section_title
;
 1,3-Diamine Formation from an Interrupted Hofmann--L\"offler Reaction:
 Iodine Catalyst Turnover through Ritter-Type Amination
;
_journal_issue                   9
_journal_name_full               'ACS Catalysis'
_journal_page_first              7741
_journal_paper_doi               10.1021/acscatal.9b01566
_journal_volume                  9
_journal_year                    2019
_chemical_absolute_configuration ad
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_space_group_name_H-M_alt        'P 21 21 21'
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'shelXle (H&#x00FC;bschle, Sheldrick and Dittirch, 2011)'
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_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.886
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_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
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_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6662
_diffrn_reflns_point_group_measured_fraction_full 0.937
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_diffrn_reflns_theta_full        25.242
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_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       Block
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_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
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_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.043
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;
 Flack x determined using 869 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0387P)^2^+0.1697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.565
_reflns_Friedel_fraction_full    0.849
_reflns_Friedel_fraction_max     0.677
_reflns_number_gt                2472
_reflns_number_total             2631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b01566_si_003.cif
_cod_data_source_block           0918m445
_cod_database_code               4514831
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              18646
_shelx_hkl_checksum              41810