Marked Stabilization of Redox States and Enhanced Catalytic Activity in Galactose Oxidase Models Based on Transition Metal S-Methylisothiosemicarbazonates with -SR Group in Ortho Position to the Phenolic Oxygen
Vladimir B. Arion; Sonja Platzer; Peter Rapta; Peter Machata; Martin Breza; Daniel Vegh; Lothar Dunsch; Joshua Telser; Sergiu Shova; Tatiana C.O. Mac Leod; Armando J.L. Pombeiro; Inorganic Chemistry 52 (2013) 7524–7540; doi:10.1021/ic4004966

data_4335347
_publ_section_title
;
 Marked Stabilization of Redox States and Enhanced Catalytic Activity in
 Galactose Oxidase Models Based on Transition Metal
 S-Methylisothiosemicarbazonates with -SR Group in Ortho Position to the
 Phenolic Oxygen
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7524
_journal_page_last               7540
_journal_paper_doi               10.1021/ic4004966
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C25 H27 N3 Ni O3 S2'
_chemical_formula_sum            'C25 H27 N3 Ni O3 S2'
_chemical_formula_weight         540.33
_chemical_name_systematic
; 
[(9-(2'-oxy-3'-phenylthio-5'-tert-butylphenyl)-6-methylthio-3-acetyl-5,7,8-
triazanona-3,6,8-trienato(-)-2'-olato(-) kappaO,kappaO',kappaN^5^, kappaN^8^)
nickel(II)]   
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.593(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.402(3)
_cell_length_b                   17.236(2)
_cell_length_c                   7.4354(9)
_cell_measurement_reflns_used    6623
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.42
_cell_volume                     2470.0(6)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1573
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            48994
_diffrn_reflns_theta_full        25.52
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.7561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.496
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.115
_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     309
_refine_ls_number_reflns         4555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0651
_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^)+(0.0435P)^2^+17.2838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1688
_reflns_number_gt                3214
_reflns_number_total             4555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4004966_si_002_5.cif
_cod_data_source_block           vlar027
_cod_original_cell_volume        2470.1(5)
_cod_database_code               4335347