Synthesis, characterization and study on the dissimilar reactivity of a Ni(II)-bis(iminosemiquinone) complex core to ligand-appended hemilabile –CH2OH and –CH2NH2 units
Sarkar, Prasenjit; Ghorai, Samir; Chandra Paul, Ganesh; Khannam, Mahmuda; Barman, Surajit; Mukherjee, Chandan; Inorganica Chimica Acta 502 (2020) 119340–; doi:10.1016/j.ica.2019.119340

data_1565498
_publ_section_title
;
 Synthesis, characterization and study on the dissimilar reactivity of a
 Ni(II)-bis(iminosemiquinone) complex core to ligand-appended hemilabile
 --CH2OH and --CH2NH2 units
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119340
_journal_paper_doi               10.1016/j.ica.2019.119340
_journal_volume                  502
_journal_year                    2020
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C42 H54 N2 Ni O4'
_chemical_formula_sum            'C21 H27 N Ni0.5 O2'
_chemical_formula_weight         354.79
_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
_cell_angle_alpha                71.193(8)
_cell_angle_beta                 80.081(10)
_cell_angle_gamma                81.402(8)
_cell_formula_units_Z            2
_cell_length_a                   5.7899(8)
_cell_length_b                   12.5127(9)
_cell_length_c                   13.9208(14)
_cell_measurement_reflns_used    6216
_cell_measurement_temperature    102(3)
_cell_measurement_theta_max      24.994
_cell_measurement_theta_min      2.657
_cell_volume                     935.62(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      102(3)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5759
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.657
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_recrystallization_method 'dichloromethane and methanol'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0823
_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^)+(0.0957P)^2^+2.9213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2278
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2334
_reflns_number_total             3293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            exp_6565.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C21 H27 N Ni0.50 O2'
_cod_database_code               1565498
_shelxl_version_number           2013-4
_shelx_res_checksum              82249
_shelx_hkl_checksum              88820