Tuning the catecholase activity of bis(pyrazolyl)methane-based copper(II) complexes by substitutions of the ligand core: unraveling a dual O2/H2O2 oxidation mechanism
Jayaweera, Nuwanthaka P.; Hall, Ashley E.; Wilson, Ashton A.; Konkle, Mary E.; Wheeler, Kraig A.; Semeniuc, Radu F.; Inorganica Chimica Acta 506 (2020) 119507–; doi:10.1016/j.ica.2020.119507

data_1564967
_publ_section_title
;
 Tuning the catecholase activity of bis(pyrazolyl)methane-based copper(II)
 complexes by substitutions of the ligand core: unraveling a dual O2/H2O2
 oxidation mechanism
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119507
_journal_paper_doi               10.1016/j.ica.2020.119507
_journal_volume                  506
_journal_year                    2020
_chemical_formula_sum            'C26 H28 Cu2 N10 O5'
_chemical_formula_weight         687.68
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'direct methods, SHELXS'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   38.1953(9)
_cell_length_b                   38.1953(9)
_cell_length_c                   10.8879(3)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.61
_cell_measurement_theta_min      2.31
_cell_volume                     13756.1(6)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction
;
SADABS (Bruker, 2013) and XPREP (Bruker, 2013)
;
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            69630
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.400
_diffrn_reflns_theta_min         2.313
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_exptl_absorpt_coefficient_mu    2.165
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/7, Bruker AXS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       'transparent hexagon'
_exptl_crystal_F_000             6336
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         5595
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0470P)^2^+49.1609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5049
_reflns_number_total             5595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-506-119507.cif
_cod_data_source_block           16rfs04_squeeze
_cod_original_cell_volume        13756.1(8)
_cod_database_code               1564967
_shelx_estimated_absorpt_t_min   0.557
_shelx_estimated_absorpt_t_max   0.813