Expedient Ni(OTf)2/visible light photoredox-catalyzed annulation of donor-acceptor cyclopropanes with cyclic secondary amines
Karjee, Pallab; Mishra, Manmath; Debnath, Bijoy; Punniyamurthy, Tharmalingam; Chemical Communications  (2022) –; doi:10.1039/D2CC02941C

data_7130328
_publ_section_title
;
 Expedient Ni(OTf)2/visible light photoredox-catalyzed annulation of
 donor-acceptor cyclopropanes with cyclic secondary amines
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02941C
_journal_year                    2022
_chemical_formula_sum            'C26 H25 N O4'
_chemical_formula_weight         415.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-04-01 deposited with the CCDC.	2022-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.892(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1009(6)
_cell_length_b                   7.6217(3)
_cell_length_c                   19.2497(7)
_cell_measurement_reflns_used    7462
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.85
_cell_measurement_theta_min      2.44
_cell_volume                     2210.43(15)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56496
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.047
_diffrn_reflns_theta_max         25.047
_diffrn_reflns_theta_min         1.352
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0500P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2799
_reflns_number_total             3907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02941c2.cif
_cod_data_source_block           PK-233
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7130328
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              39453
_shelx_hkl_checksum              70668