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_4331155
_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 H57 N4 Ni O2, F6 Sb'
_chemical_formula_sum            'C40 H57 F6 N4 Ni O2 Sb'
_chemical_formula_weight         920.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-07-24 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.3800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5147(3)
_cell_length_b                   9.0739(2)
_cell_length_c                   32.0739(6)
_cell_measurement_reflns_used    9008
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      67.88
_cell_measurement_theta_min      2.96
_cell_volume                     4204.60(15)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0871
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            56704
_diffrn_reflns_theta_full        68.31
_diffrn_reflns_theta_max         68.31
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    6.201
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       rod
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.072
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7678
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.8620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                6590
_reflns_number_total             7678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301684h_si_002_1.cif
_cod_data_source_block           cu_david4b_0m
_cod_original_cell_volume        4204.59(15)
_cod_database_code               4331155