Copper-catalyzed 1,3-aminoazidation of arylcyclopropanes: a facile access to 1,3-diamine derivatives
Wang, Lihong; Wang, Xiaomin; Zhang, Ge; Yang, Shengbiao; Li, Yan; Zhang, Qian; Organic Chemistry Frontiers 6 (2019) 2934–; doi:10.1039/C9QO00638A

data_1554989
_publ_section_title
;
 Copper-catalyzed 1,3-aminoazidation of arylcyclopropanes: a facile access
 to 1,3-diamine derivatives
;
_journal_issue                   16
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              2934
_journal_paper_doi               10.1039/C9QO00638A
_journal_volume                  6
_journal_year                    2019
_chemical_formula_sum            'C27 H24 N4 O4 S2'
_chemical_formula_weight         532.62
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           ??monoclinic??
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-05-13 deposited with the CCDC.	2019-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.84
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.943
_cell_length_b                   19.423
_cell_length_c                   27.408
_cell_measurement_reflns_used    4300
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.03
_cell_measurement_theta_min      5.02
_cell_volume                     5274.238
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            65925
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7928
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1548P)^2^+6.3693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.2051
_reflns_number_gt                6524
_reflns_number_total             9313
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c9qo00638a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2022-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C54 H48 N8 O8 S4'
_cod_original_formula_weight         1065.24
_cod_original_formula_units_Z            4
_cod_original_cell_volume        5274.2
_cod_original_sg_symbol_H-M      ??P21/n??
_cod_database_code               1554989