Biradical o-iminobenzosemiquinonato(1−) complexes of nickel(ii): catalytic activity in three-component coupling of aldehydes, amines and alkynes
Nasibipour, Mina; Safaei, Elham; Moaddeli, Ali; Masoumpour, Marziyeh Sadat; Wojtczak, Andrzej; RSC Advances 11 (2021) 12845–12859; doi:10.1039/D0RA10248B

data_7242613
_publ_section_title
;
 Biradical o-iminobenzosemiquinonato(1&#x2212;) complexes of nickel(ii):
 catalytic activity in three-component coupling of aldehydes, amines and
 alkynes
;
_journal_issue                   21
_journal_name_full               'RSC Advances'
_journal_page_first              12845
_journal_page_last               12859
_journal_paper_doi               10.1039/D0RA10248B
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C70 H88 N4 Ni O4'
_chemical_formula_sum            'C70 H88 N4 Ni O4'
_chemical_formula_weight         1108.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-10-07 deposited with the CCDC.	2021-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.001(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1423(6)
_cell_length_b                   17.5195(5)
_cell_length_c                   23.9371(9)
_cell_measurement_reflns_used    13911
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6120
_cell_measurement_theta_min      2.3000
_cell_volume                     7313.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_publication_material  'CIFTAB-2017 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2564
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Oxford Sapphire CCD'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            52213
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.366
_diffrn_reflns_theta_min         2.325
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2384
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH--CH2Cl2'
_exptl_crystal_size_max          0.793
_exptl_crystal_size_mid          0.564
_exptl_crystal_size_min          0.517
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         16548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+4.4837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10626
_reflns_number_total             16548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra10248b2.cif
_cod_data_source_block           e1464a_sq
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7242613
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.792
_shelx_estimated_absorpt_t_max   0.857
_exptl_absorpt_special_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_shelx_res_checksum              51691
_shelx_fab_checksum              71679