Redox noninnocence of the bridge in copper(II) salophen and bis(oxamato) complexes.
de Bellefeuille, David; Orio, Maylis; Barra, Anne-Laure; Aukauloo, Ally; Journaux, Yves; Philouze, Christian; Ottenwaelder, Xavier; Thomas, Fabrice; Inorganic chemistry 54 (2015) 9013–9026; doi:10.1021/acs.inorgchem.5b01285

data_4346308
_publ_section_title
;
 Redox noninnocence of the bridge in copper(II) salophen and bis(oxamato)
 complexes.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9013
_journal_page_last               9026
_journal_paper_doi               10.1021/acs.inorgchem.5b01285
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '2(C24 H20 P 1+), C14 H14 Cu N4 O6 2-'
_chemical_formula_sum            'C62 H54 Cu N4 O6 P2'
_chemical_formula_weight         1076.57
_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   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 101.1600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0795(11)
_cell_length_b                   25.948(2)
_cell_length_c                   14.5253(11)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.38
_cell_volume                     5206.3(7)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      149(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            62464
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.805
_diffrn_reflns_theta_min         1.570
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.362
_exptl_crystal_size_min          0.248
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         12834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+2.4262P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9495
_reflns_number_total             12834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01285_si_002.cif
_cod_data_source_block           mo_david11_0m
_cod_original_cell_volume        5206.2(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4346308
_shelx_estimated_absorpt_t_min   0.794
_shelx_estimated_absorpt_t_max   0.878
_shelxl_version_number           2013-2
_shelx_res_checksum              1226
_shelx_hkl_checksum              81942