Cobalt-catalyzed amination of aziridines and azetidines toward 1,2- and 1,3-diamines.
Cheng, Ling-Chao; Wang, Zhihua; He, Xinglei; Liang, Wangfu; Ye, Ke-Yin; Organic & biomolecular chemistry 22 (2024) 2554–2557; doi:10.1039/d4ob00168k

data_7159826
_publ_section_title
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 Cobalt-catalyzed amination of aziridines and azetidines toward 1,2- and
 1,3-diamines.
;
_journal_issue                   13
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2554
_journal_page_last               2557
_journal_paper_doi               10.1039/d4ob00168k
_journal_volume                  22
_journal_year                    2024
_chemical_formula_moiety         'C27 H26 N2 O6 S3'
_chemical_formula_sum            'C27 H26 N2 O6 S3'
_chemical_formula_weight         570.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-17 deposited with the CCDC.	2024-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                73.30(3)
_cell_angle_beta                 70.165(18)
_cell_angle_gamma                72.632(17)
_cell_formula_units_Z            2
_cell_length_a                   10.094(4)
_cell_length_b                   10.648(6)
_cell_length_c                   13.883(9)
_cell_measurement_reflns_used    9366
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.201
_cell_measurement_theta_min      2.329
_cell_volume                     1310.5(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30688
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.223
_diffrn_reflns_theta_max         25.223
_diffrn_reflns_theta_min         2.048
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6017
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       plate
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.285
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.415
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.415
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0936
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2768
_refine_ls_wR_factor_ref         0.3043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3951
_reflns_number_total             4557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob00168k2.cif
_cod_data_source_block           hxl02_0m
_cod_depositor_comments
'Adding full bibliography for 7159826--7159827.cif.'
_cod_database_code               7159826
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.962
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.063) H1B(0.063) H1C(0.063) H3(0.038) H4(0.034) H6(0.038)
 H7(0.038) H8A(0.032) H8B(0.032) H9(0.03) H11(0.044) H12(0.056) H13(0.055)
 H14(0.049) H15(0.037) H17(0.038) H18(0.051) H19(0.053) H20(0.045) H21(0.035)
 H23(0.049) H24(0.058) H25(0.053) H26(0.054) H27(0.04) H1(0.031)
 Fixed X: H1A(0.207618) H1B(0.288379) H1C(0.119668) H3(0.012517) H4(0.032992)
 H6(0.457221) H7(0.435608) H8A(0.143958) H8B(0.205347) H9(0.417564)
 H11(0.509142) H12(0.55834) H13(0.425962) H14(0.241387) H15(0.192816)
 H17(0.10296) H18(0.121114) H19(0.159314) H20(0.174157) H21(0.154894)
 H23(0.218987) H24(0.159366) H25(0.220694) H26(0.326809) H27(0.394673)
 H1(0.404486)
 Fixed Y: H1A(1.120801) H1B(1.157318) H1C(1.178874) H3(1.001111) H4(0.787441)
 H6(0.700534) H7(0.914874) H8A(0.60243) H8B(0.728738) H9(0.627085)
 H11(0.512108) H12(0.304746) H13(0.148566) H14(0.196287) H15(0.403238)
 H17(0.881166) H18(0.805747) H19(0.57926) H20(0.427132) H21(0.497407)
 H23(1.109837) H24(1.288814) H25(1.260037) H26(1.049415) H27(0.869338)
 H1(0.508439)
 Fixed Z: H1A(0.172814) H1B(0.236053) H1C(0.273682) H3(0.389984) H4(0.492592)
 H6(0.343758) H7(0.242681) H8A(0.719243) H8B(0.648977) H9(0.710651)
 H11(0.863467) H12(0.972987) H13(1.003375) H14(0.925561) H15(0.813853)
 H17(1.050536) H18(1.222488) H19(1.29459) H20(1.203434) H21(1.031824)
 H23(0.781052) H24(0.650891) H25(0.481149) H26(0.443747) H27(0.571265)
 H1(0.60426)
;
_olex2_submission_special_instructions 'No special instructions were received'