Reversible Double Oxidation and Protonation of the Non-Innocent Bridge in a Nickel(II) Salophen Complex
David de Bellefeuille; Mohammad S. Askari; Benedikt Lassalle-Kaiser; Yves Journaux; Ally Aukauloo; Maylis Orio; Fabrice Thomas; Xavier Ottenwaelder; Inorganic Chemistry 51 (2012) 12796–12804; doi:10.1021/ic301684h

data_4331156
_publ_contact_author_address
;
Concordia University
Department of Chemistry and Biochemistry
7141 Sherbrooke Street West
Montr\'eal, Qu\'ebec
Canada H4B 1R6
;
_publ_contact_author_email       dr.x@concordia.ca
_publ_contact_author_fax         '+1 514 848 2868'
_publ_contact_author_name        'Ottenwaelder, Xavier'
_publ_contact_author_phone       '+1 514 848 2424 ext 8934'
_publ_section_title
;
 Reversible Double Oxidation and Protonation of the Non-Innocent Bridge in
 a Nickel(II) Salophen Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12796
_journal_page_last               12804
_journal_paper_doi               10.1021/ic301684h
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C40 H56 N4 Ni O2'
_chemical_formula_sum            'C40 H56 N4 Ni O2'
_chemical_formula_weight         683.60
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.883(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.9521(7)
_cell_length_b                   15.1711(4)
_cell_length_c                   10.3912(3)
_cell_measurement_reflns_used    6275
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      67.11
_cell_measurement_theta_min      3.47
_cell_volume                     3695.03(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16344
_diffrn_reflns_theta_full        68.04
_diffrn_reflns_theta_max         68.04
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  0.9682
_exptl_absorpt_correction_T_min  0.5931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       needle
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0539P)^2^+2.8636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                2528
_reflns_number_total             3334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301684h_si_002_2.cif
_cod_data_source_block           cu_david1_0m
_cod_database_code               4331156