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_4335344
_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         'C20 H27 N3 O3 S2'
_chemical_formula_sum            'C20 H27 N3 O3 S2'
_chemical_formula_weight         421.57
_chemical_name_systematic
; 
9-(2'-Hydroxy-3'-methylthio-5'-tert-butylphenyl)-6-methylthio-3-acetyl-
5,7,8-triazanona-3,6,8-trien-2-one 
;
_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                 99.084(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.0432(17)
_cell_length_b                   7.7185(7)
_cell_length_c                   32.514(3)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.12
_cell_measurement_theta_min      2.55
_cell_volume                     4223.5(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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0933
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            44412
_diffrn_reflns_theta_full        30.23
_diffrn_reflns_theta_max         30.23
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  0.9781
_exptl_absorpt_correction_T_min  0.9465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         6189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0484P)^2^+5.6434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                4601
_reflns_number_total             6189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4004966_si_002_2.cif
_cod_data_source_block           sopl018
_cod_database_code               4335344