Catalytic Oxidation of 3,5-Di-tert-butylcatechol by a Series of Mononuclear Manganese Complexes: Synthesis, Structure, and Kinetic Investigation
Michael U. Triller; Daniel Pursche; Wen-Yuan Hsieh; Vincent L. Pecoraro; Annette Rompel; Bernt Krebs; Inorganic Chemistry 42 (2003) 6274–6283; doi:10.1021/ic0347788

data_4314389
_publ_section_title
;
 Catalytic Oxidation of 3,5-Di-tert-butylcatechol by a Series of
 Mononuclear Manganese Complexes: Synthesis, Structure, and Kinetic
 Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6274
_journal_page_last               6283
_journal_paper_doi               10.1021/ic0347788
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '[Mn(mimppa)(tcc)] . 2 CHCl3'
_chemical_formula_sum            'C25 H19 Cl10 Mn N4 O3'
_chemical_formula_weight         832.88
_chemical_melting_point          493
_chemical_name_common            'manganese(III)tetrachlorocatechol monomer'
_chemical_name_systematic
; 
 manganesetetrachlorocatechol((1-methylimidazol-2-yl)methyl)
((2-pyridyl)methyl)-2-hydroxyphenylamine) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.50(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.417(3)
_cell_length_b                   13.930(3)
_cell_length_c                   17.497(3)
_cell_measurement_temperature    100(2)
_cell_volume                     3204.5(12)
_computing_cell_refinement       'SMART/SAINT software package, Bruker Nonius'
_computing_data_collection       'SMART software package, Bruker Nonius'
_computing_data_reduction
'G. M. Sheldrick, Shelxltl Plus, Siemens Analytical X-ray Instruments 1990'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker AXS Smart 6000 CCD'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.1035
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18412
_diffrn_reflns_theta_full        71.63
_diffrn_reflns_theta_max         71.63
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    11.342
_exptl_absorpt_correction_type
'Program sadabs, SAINT software package, Bruker Nonius, Karlsruhe'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.831
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0298P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                3739
_reflns_number_total             5971
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0347788si20030711_042806_5.cif
_cod_data_source_block           complex6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3204.5(11)
_cod_database_code               4314389